Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Jean-Pascal Sutter' _publ_contact_author_address ; Laboratoire de Chimie de Coordination - CNRS 205, route de Narbonne 31077 Toulouse (France) ; _publ_contact_author_email sutter@lcc-toulouse.fr _publ_contact_author_phone (int-33)561175823 _publ_contact_author_fax (int-33)561553003 loop_ _publ_author_name _publ_author_address I.Imaz ;ICMCB-Insitut de Chimie de la Matiere Condensee-UPR 9048 CNRS. Universite Bordeaux I 87, Avenue du Dr. Schweitzer 33600 Pessac (FRANCE) ; J.-P.Sutter ;Laboratoire de Chimie de Coordination - CNRS 205, route de Narbonne 31077 Toulouse (France) ; G.Bravic ;ICMCB-Insitut de Chimie de la Matiere Condensee-UPR 9048 CNRS. Universite Bordeaux I 87, Avenue du Dr. Schweitzer 33600 Pessac (FRANCE) ; _publ_section_title ; Structural and zeolitic features of a series of heterometallic supramolecular porous architectures based on tetrahedral {M(C2O4)4}4- primary building units ; data_SPA2 _database_code_depnum_ccdc_archive 'CCDC 246086' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C8 Cd K2 O16 U, 9H2O' _chemical_formula_sum 'C8 H18 Cd K2 O25 U' _chemical_formula_weight 942.85 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' Cd Cd -0.8075 1.2024 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 11.473(1) _cell_length_b 8.968(1) _cell_length_c 11.524(1) _cell_angle_alpha 90.00 _cell_angle_beta 97.43(2) _cell_angle_gamma 90.00 _cell_volume 1175.8(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1 _cell_measurement_theta_max 20 _exptl_crystal_description prisme _exptl_crystal_colour green _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.663 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 888 _exptl_absorpt_coefficient_mu 8.249 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details scalepack _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8688 _diffrn_reflns_av_R_equivalents 0.0120 _diffrn_reflns_av_sigmaI/netI 0.0193 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _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 2.36 _diffrn_reflns_theta_max 26.37 _reflns_number_total 4670 _reflns_number_gt 4662 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^ > 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^)+(0.0421P)^2^+1.3877P] 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 SHELXL _refine_ls_extinction_coef 0.0136(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.009(4) _refine_ls_number_reflns 4670 _refine_ls_number_parameters 335 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0171 _refine_ls_R_factor_gt 0.0160 _refine_ls_wR_factor_ref 0.0642 _refine_ls_wR_factor_gt 0.0449 _refine_ls_goodness_of_fit_ref 1.207 _refine_ls_restrained_S_all 1.207 _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 C1 C 0.5059(4) 0.9789(6) 0.2441(5) 0.0167(10) Uani 1 1 d . . . C2 C 0.5469(5) 0.8211(7) 0.2119(5) 0.0157(10) Uani 1 1 d . . . C7 C 0.2348(4) 0.7234(5) 0.0008(4) 0.0155(10) Uani 1 1 d . . . C8 C 0.2484(4) 0.5625(6) 0.0466(4) 0.0146(10) Uani 1 1 d . . . C4 C 0.2308(4) 0.7212(6) 0.5498(4) 0.0133(10) Uani 1 1 d . . . C3 C 0.2455(4) 0.5582(6) 0.5056(4) 0.0158(10) Uani 1 1 d . . . C5 C 0.0504(4) 0.9725(6) 0.2538(4) 0.0144(9) Uani 1 1 d . . . C6 C 0.0024(4) 0.8116(6) 0.2479(5) 0.0150(10) Uani 1 1 d . . . Cd1 Cd 0.77567(3) 1.01888(3) 0.22669(3) 0.01319(10) Uani 1 1 d . . . K1 K 0.26594(12) 0.2706(3) 0.26966(11) 0.0289(3) Uani 1 1 d . . . K2 K 0.77800(14) 0.5190(2) 0.21922(14) 0.0282(3) Uani 1 1 d . . . O1 O 0.5746(3) 1.0836(4) 0.2384(4) 0.0226(8) Uani 1 1 d . . . O4 O 0.4024(3) 0.9861(4) 0.2725(4) 0.0192(8) Uani 1 1 d . . . O3 O 0.4681(3) 0.7202(4) 0.2047(4) 0.0211(8) Uani 1 1 d . . . O2 O 0.6505(3) 0.8026(4) 0.1974(4) 0.0226(9) Uani 1 1 d . . . O5 O 0.2406(4) 0.4556(5) 0.5754(3) 0.0242(9) Uani 1 1 d . . . O6 O 0.2154(3) 0.7410(5) 0.6515(3) 0.0215(9) Uani 1 1 d . . . O13 O 0.2400(4) 0.4597(5) -0.0262(3) 0.0249(9) Uani 1 1 d . . . O14 O 0.2191(4) 0.7434(5) -0.1060(3) 0.0241(9) Uani 1 1 d . . . O9 O -0.1048(3) 0.7939(5) 0.2407(4) 0.0262(10) Uani 1 1 d . . . O10 O -0.0218(3) 1.0758(4) 0.2498(4) 0.0221(8) Uani 1 1 d . . . O7 O 0.2621(4) 0.5462(4) 0.3992(3) 0.0198(8) Uani 1 1 d . . . O8 O 0.2380(3) 0.8220(4) 0.4725(3) 0.0184(7) Uani 1 1 d . . . O12 O 0.1613(3) 0.9853(4) 0.2651(4) 0.0170(8) Uani 1 1 d . . . O11 O 0.0809(3) 0.7103(4) 0.2542(4) 0.0212(8) Uani 1 1 d . . . O16 O 0.2398(4) 0.8235(5) 0.0790(3) 0.0219(8) Uani 1 1 d . . . O15 O 0.2696(4) 0.5491(4) 0.1567(3) 0.0172(8) Uani 1 1 d . . . O17 O 0.4655(3) 0.7425(7) 0.4392(4) 0.0322(11) Uani 1 1 d . . . O18 O 0.0802(5) 0.2350(6) 0.4454(5) 0.0524(15) Uani 1 1 d . . . O19 O 0.0531(5) 0.3156(7) 0.1162(7) 0.0564(16) Uani 1 1 d . . . O20 O 0.3836(6) 0.2294(7) 0.0681(5) 0.0513(16) Uani 1 1 d . . . O21 O 0.5058(5) 0.3473(7) 0.3378(4) 0.0408(12) Uani 1 1 d . . . O22 O 0.5532(5) 0.4768(7) 0.0837(6) 0.0522(15) Uani 1 1 d . . . O23 O 0.9772(5) 0.5115(7) 0.4026(6) 0.0508(14) Uani 1 1 d . . . O25 O 0.6876(5) 0.6165(7) 0.4368(5) 0.0477(13) Uani 1 1 d . . . O24 O 0.9034(5) 0.5570(6) 0.0256(5) 0.0477(14) Uani 1 1 d . . . U1 U 0.287012(12) 0.76387(4) 0.282797(11) 0.01041(8) Uani 1 1 d . . . H25A H 0.7026 0.7216 0.4481 0.016 Uiso 1 1 d . . . H25B H 0.7277 0.5624 0.5018 0.016 Uiso 1 1 d . . . H17A H 0.5325 0.7129 0.4030 0.016 Uiso 1 1 d . . . H17B H 0.4498 0.6691 0.4958 0.016 Uiso 1 1 d . . . H18B H 0.0032 0.2493 0.4052 0.016 Uiso 1 1 d . . . H18C H 0.0960 0.3074 0.5070 0.016 Uiso 1 1 d . . . H19A H 0.0026 0.2315 0.1191 0.016 Uiso 1 1 d . . . H19C H 0.0142 0.4040 0.1394 0.016 Uiso 1 1 d . . . H20B H 0.4515 0.2930 0.0743 0.016 Uiso 1 1 d . . . H20C H 0.3313 0.2551 -0.0007 0.016 Uiso 1 1 d . . . H21B H 0.5107 0.4388 0.3813 0.016 Uiso 1 1 d . . . H21C H 0.5448 0.3599 0.2692 0.016 Uiso 1 1 d . . . H22A H 0.5054 0.5620 0.0924 0.016 Uiso 1 1 d . . . H22C H 0.5644 0.4657 0.0026 0.016 Uiso 1 1 d . . . H23A H 0.9811 0.6036 0.4441 0.016 Uiso 1 1 d . . . H23B H 1.0477 0.4972 0.3671 0.016 Uiso 1 1 d . . . H24A H 0.9282 0.6597 0.0227 0.016 Uiso 1 1 d . . . H24B H 0.8523 0.5343 -0.0451 0.016 Uiso 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 C1 0.011(2) 0.019(2) 0.020(2) 0.002(2) 0.0025(19) -0.0015(19) C2 0.011(2) 0.022(2) 0.015(2) -0.0027(19) 0.0039(18) -0.0023(19) C7 0.017(2) 0.018(3) 0.011(2) 0.0005(17) 0.0002(18) -0.0008(17) C8 0.013(2) 0.016(2) 0.015(2) -0.0001(19) 0.0036(18) 0.0007(18) C4 0.012(2) 0.016(3) 0.011(2) 0.0006(17) -0.0003(17) 0.0007(16) C3 0.015(2) 0.019(3) 0.013(2) 0.0023(19) 0.0020(18) -0.0045(18) C5 0.013(2) 0.017(2) 0.014(2) 0.0001(19) 0.0049(18) 0.0007(19) C6 0.012(2) 0.015(2) 0.018(2) -0.0020(17) 0.0020(18) -0.0001(17) Cd1 0.01253(17) 0.01530(18) 0.01197(18) -0.00044(16) 0.00243(13) -0.00063(15) K1 0.0328(6) 0.0175(6) 0.0363(6) 0.0015(8) 0.0045(5) -0.0029(9) K2 0.0311(7) 0.0202(6) 0.0329(7) -0.0037(7) 0.0030(6) -0.0014(6) O1 0.0148(18) 0.0171(18) 0.036(2) 0.0005(17) 0.0044(16) -0.0032(15) O4 0.0134(17) 0.0163(19) 0.029(2) -0.0001(15) 0.0074(15) 0.0003(14) O3 0.0175(19) 0.017(2) 0.030(2) -0.0090(15) 0.0088(15) -0.0050(13) O2 0.0135(16) 0.026(2) 0.029(2) -0.0043(15) 0.0061(15) -0.0003(14) O5 0.040(3) 0.0200(19) 0.0129(18) 0.0015(15) 0.0025(17) -0.0060(17) O6 0.0280(18) 0.023(3) 0.0144(15) -0.0021(15) 0.0065(14) 0.0047(16) O13 0.041(2) 0.0166(18) 0.0163(18) -0.0026(15) 0.0016(17) 0.0014(17) O14 0.041(2) 0.019(2) 0.0113(15) 0.0033(17) 0.0007(15) 0.0005(19) O9 0.0133(17) 0.021(3) 0.044(2) -0.0013(18) 0.0027(16) -0.0034(15) O10 0.0150(18) 0.0149(18) 0.036(2) -0.0001(17) 0.0035(16) 0.0034(14) O7 0.031(2) 0.0157(19) 0.0129(16) -0.0010(14) 0.0035(16) -0.0005(16) O8 0.027(2) 0.0159(17) 0.0141(18) 0.0000(14) 0.0072(15) 0.0032(14) O12 0.0108(16) 0.0137(18) 0.027(2) 0.0012(15) 0.0034(14) -0.0009(14) O11 0.0119(18) 0.0140(16) 0.037(2) -0.0010(16) 0.0016(16) 0.0011(13) O16 0.032(2) 0.0175(17) 0.0154(18) -0.0001(14) 0.0006(16) 0.0044(15) O15 0.026(2) 0.0146(18) 0.0108(16) 0.0006(13) 0.0034(14) -0.0001(15) O17 0.0203(18) 0.051(3) 0.0239(19) 0.003(2) -0.0024(15) 0.004(2) O18 0.063(3) 0.029(3) 0.060(3) -0.014(2) -0.012(3) 0.002(2) O19 0.036(3) 0.048(3) 0.085(5) 0.022(3) 0.010(3) -0.009(2) O20 0.065(3) 0.049(4) 0.038(3) 0.006(2) -0.005(2) 0.021(3) O21 0.036(3) 0.052(3) 0.033(3) -0.007(2) 0.000(2) 0.006(2) O22 0.046(3) 0.044(3) 0.070(4) -0.016(3) 0.018(3) 0.004(3) O23 0.037(3) 0.040(3) 0.076(4) 0.016(3) 0.011(3) 0.000(2) O25 0.040(3) 0.045(3) 0.058(3) 0.015(3) 0.009(3) 0.009(2) O24 0.062(3) 0.044(3) 0.035(3) -0.001(2) -0.004(2) -0.019(3) U1 0.01004(10) 0.01173(10) 0.00975(10) -0.00019(7) 0.00246(6) -0.00016(7) _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 C1 O1 1.234(6) . ? C1 O4 1.273(6) . ? C1 C2 1.551(8) . ? C2 O2 1.233(7) . ? C2 O3 1.274(6) . ? C7 O14 1.234(6) . ? C7 O16 1.269(6) . ? C7 C8 1.537(7) . ? C8 O13 1.241(7) . ? C8 O15 1.266(6) . ? C4 O6 1.220(6) . ? C4 O8 1.279(6) . ? C4 C3 1.564(7) . ? C3 O5 1.228(7) . ? C3 O7 1.270(6) . ? C5 O10 1.240(6) . ? C5 O12 1.267(6) . ? C5 C6 1.543(7) . ? C6 O9 1.232(7) . ? C6 O11 1.275(6) . ? Cd1 O13 2.355(4) 2_655 ? Cd1 O10 2.361(4) 1_655 ? Cd1 O5 2.381(4) 2_656 ? Cd1 O1 2.399(4) . ? Cd1 O2 2.411(4) . ? Cd1 O6 2.431(4) 2_656 ? Cd1 O9 2.433(4) 1_655 ? Cd1 O14 2.453(5) 2_655 ? K1 O15 2.820(4) . ? K1 O12 2.824(5) 1_545 ? K1 O19 2.852(7) . ? K1 O21 2.847(5) . ? K1 O20 2.857(6) . ? K1 O7 2.891(5) . ? K1 O4 2.991(5) 1_545 ? K1 O18 3.140(7) . ? K1 U1 4.432(3) . ? K1 U1 4.552(3) 1_545 ? K2 O9 2.804(5) 1_655 ? K2 O14 2.797(5) 2_645 ? K2 O24 2.827(6) . ? K2 O22 2.862(7) . ? K2 O23 2.906(6) . ? K2 O6 2.900(5) 2_646 ? K2 O2 2.929(5) . ? K2 O25 2.966(7) . ? O4 U1 2.404(4) . ? O4 K1 2.991(5) 1_565 ? O3 U1 2.401(4) . ? O5 Cd1 2.381(4) 2_646 ? O6 Cd1 2.431(4) 2_646 ? O6 K2 2.900(5) 2_656 ? O13 Cd1 2.355(4) 2_645 ? O14 Cd1 2.453(5) 2_645 ? O14 K2 2.797(5) 2_655 ? O9 Cd1 2.433(4) 1_455 ? O9 K2 2.804(5) 1_455 ? O10 Cd1 2.361(4) 1_455 ? O7 U1 2.406(4) . ? O8 U1 2.384(4) . ? O12 U1 2.448(4) . ? O12 K1 2.824(5) 1_565 ? O11 U1 2.394(4) . ? O16 U1 2.401(4) . ? O15 U1 2.406(4) . ? O17 U1 2.554(4) . ? U1 K1 4.552(3) 1_565 ? 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 C1 O4 126.8(5) . . ? O1 C1 C2 117.8(4) . . ? O4 C1 C2 115.4(4) . . ? O2 C2 O3 125.7(5) . . ? O2 C2 C1 118.9(5) . . ? O3 C2 C1 115.4(4) . . ? O14 C7 O16 126.4(5) . . ? O14 C7 C8 118.3(5) . . ? O16 C7 C8 115.3(4) . . ? O13 C8 O15 126.5(5) . . ? O13 C8 C7 118.0(4) . . ? O15 C8 C7 115.5(4) . . ? O6 C4 O8 126.7(5) . . ? O6 C4 C3 118.9(4) . . ? O8 C4 C3 114.4(4) . . ? O5 C3 O7 126.4(5) . . ? O5 C3 C4 118.1(4) . . ? O7 C3 C4 115.4(4) . . ? O10 C5 O12 126.4(5) . . ? O10 C5 C6 117.6(4) . . ? O12 C5 C6 116.0(4) . . ? O9 C6 O11 127.1(5) . . ? O9 C6 C5 118.1(4) . . ? O11 C6 C5 114.7(4) . . ? O13 Cd1 O10 96.22(15) 2_655 1_655 ? O13 Cd1 O5 151.72(15) 2_655 2_656 ? O10 Cd1 O5 98.15(15) 1_655 2_656 ? O13 Cd1 O1 99.08(15) 2_655 . ? O10 Cd1 O1 151.76(14) 1_655 . ? O5 Cd1 O1 78.97(15) 2_656 . ? O13 Cd1 O2 73.32(14) 2_655 . ? O10 Cd1 O2 138.56(13) 1_655 . ? O5 Cd1 O2 79.81(15) 2_656 . ? O1 Cd1 O2 69.08(13) . . ? O13 Cd1 O6 138.00(14) 2_655 2_656 ? O10 Cd1 O6 77.92(13) 1_655 2_656 ? O5 Cd1 O6 69.22(14) 2_656 2_656 ? O1 Cd1 O6 74.82(14) . 2_656 ? O2 Cd1 O6 136.03(13) . 2_656 ? O13 Cd1 O9 81.34(15) 2_655 1_655 ? O10 Cd1 O9 68.50(13) 1_655 1_655 ? O5 Cd1 O9 81.48(15) 2_656 1_655 ? O1 Cd1 O9 137.28(14) . 1_655 ? O2 Cd1 O9 70.29(14) . 1_655 ? O6 Cd1 O9 131.28(14) 2_656 1_655 ? O13 Cd1 O14 68.46(14) 2_655 2_655 ? O10 Cd1 O14 77.90(14) 1_655 2_655 ? O5 Cd1 O14 138.58(14) 2_656 2_655 ? O1 Cd1 O14 85.85(14) . 2_655 ? O2 Cd1 O14 129.72(14) . 2_655 ? O6 Cd1 O14 69.66(13) 2_656 2_655 ? O9 Cd1 O14 131.57(15) 1_655 2_655 ? O15 K1 O12 145.66(12) . 1_545 ? O15 K1 O19 69.57(15) . . ? O12 K1 O19 77.81(15) 1_545 . ? O15 K1 O21 80.88(16) . . ? O12 K1 O21 128.16(16) 1_545 . ? O19 K1 O21 148.89(18) . . ? O15 K1 O20 72.68(14) . . ? O12 K1 O20 96.45(17) 1_545 . ? O19 K1 O20 88.33(19) . . ? O21 K1 O20 73.37(16) . . ? O15 K1 O7 58.87(13) . . ? O12 K1 O7 138.54(12) 1_545 . ? O19 K1 O7 97.47(17) . . ? O21 K1 O7 74.31(15) . . ? O20 K1 O7 124.79(17) . . ? O15 K1 O4 136.18(12) . 1_545 ? O12 K1 O4 56.51(13) 1_545 1_545 ? O19 K1 O4 122.17(18) . 1_545 ? O21 K1 O4 73.58(14) . 1_545 ? O20 K1 O4 66.24(14) . 1_545 ? O7 K1 O4 140.04(12) . 1_545 ? O15 K1 O18 116.08(15) . . ? O12 K1 O18 66.27(13) 1_545 . ? O19 K1 O18 79.42(17) . . ? O21 K1 O18 123.99(15) . . ? O20 K1 O18 160.48(19) . . ? O7 K1 O18 72.36(13) . . ? O4 K1 O18 107.71(14) 1_545 . ? O15 K1 U1 29.25(8) . . ? O12 K1 U1 157.84(9) 1_545 . ? O19 K1 U1 85.32(14) . . ? O21 K1 U1 72.70(13) . . ? O20 K1 U1 97.31(13) . . ? O7 K1 U1 29.92(8) . . ? O4 K1 U1 145.56(9) 1_545 . ? O18 K1 U1 96.77(11) . . ? O15 K1 U1 153.61(9) . 1_545 ? O12 K1 U1 27.97(8) 1_545 1_545 ? O19 K1 U1 101.51(14) . 1_545 ? O21 K1 U1 100.77(13) . 1_545 ? O20 K1 U1 82.50(13) . 1_545 ? O7 K1 U1 147.21(9) . 1_545 ? O4 K1 U1 28.69(8) 1_545 1_545 ? O18 K1 U1 85.11(11) . 1_545 ? U1 K1 U1 173.15(4) . 1_545 ? O9 K2 O14 141.59(14) 1_655 2_645 ? O9 K2 O24 71.12(15) 1_655 . ? O14 K2 O24 72.56(15) 2_645 . ? O9 K2 O22 123.54(17) 1_655 . ? O14 K2 O22 72.11(15) 2_645 . ? O24 K2 O22 95.74(18) . . ? O9 K2 O23 68.46(15) 1_655 . ? O14 K2 O23 105.26(17) 2_645 . ? O24 K2 O23 98.28(17) . . ? O22 K2 O23 164.20(19) . . ? O9 K2 O6 136.90(13) 1_655 2_646 ? O14 K2 O6 58.60(13) 2_645 2_646 ? O24 K2 O6 121.80(16) . 2_646 ? O22 K2 O6 97.37(17) . 2_646 ? O23 K2 O6 68.96(14) . 2_646 ? O9 K2 O2 58.16(13) 1_655 . ? O14 K2 O2 139.75(13) 2_645 . ? O24 K2 O2 97.30(16) . . ? O22 K2 O2 70.32(14) . . ? O23 K2 O2 114.81(16) . . ? O6 K2 O2 140.36(12) 2_646 . ? O9 K2 O25 83.23(16) 1_655 . ? O14 K2 O25 132.97(16) 2_645 . ? O24 K2 O25 154.23(18) . . ? O22 K2 O25 96.39(17) . . ? O23 K2 O25 73.76(17) . . ? O6 K2 O25 78.94(14) 2_646 . ? O2 K2 O25 65.85(14) . . ? C1 O1 Cd1 116.4(3) . . ? C1 O4 U1 120.6(3) . . ? C1 O4 K1 123.0(3) . 1_565 ? U1 O4 K1 114.63(14) . 1_565 ? C2 O3 U1 120.1(3) . . ? C2 O2 Cd1 116.1(4) . . ? C2 O2 K2 125.8(4) . . ? Cd1 O2 K2 113.88(14) . . ? C3 O5 Cd1 117.6(4) . 2_646 ? C4 O6 Cd1 115.8(4) . 2_646 ? C4 O6 K2 128.4(4) . 2_656 ? Cd1 O6 K2 114.30(13) 2_646 2_656 ? C8 O13 Cd1 119.0(3) . 2_645 ? C7 O14 Cd1 115.8(4) . 2_645 ? C7 O14 K2 125.8(4) . 2_655 ? Cd1 O14 K2 117.27(14) 2_645 2_655 ? C6 O9 Cd1 116.5(3) . 1_455 ? C6 O9 K2 125.6(3) . 1_455 ? Cd1 O9 K2 117.60(15) 1_455 1_455 ? C5 O10 Cd1 119.1(3) . 1_455 ? C3 O7 U1 120.9(3) . . ? C3 O7 K1 125.8(3) . . ? U1 O7 K1 113.27(14) . . ? C4 O8 U1 121.9(3) . . ? C5 O12 U1 120.5(3) . . ? C5 O12 K1 120.2(3) . 1_565 ? U1 O12 K1 119.27(14) . 1_565 ? C6 O11 U1 122.9(3) . . ? C7 O16 U1 121.4(3) . . ? C8 O15 U1 121.3(3) . . ? C8 O15 K1 122.3(3) . . ? U1 O15 K1 115.81(14) . . ? O8 U1 O11 79.86(14) . . ? O8 U1 O16 142.92(14) . . ? O11 U1 O16 79.41(14) . . ? O8 U1 O3 134.22(14) . . ? O11 U1 O3 143.44(14) . . ? O16 U1 O3 76.51(14) . . ? O8 U1 O4 93.49(14) . . ? O11 U1 O4 134.44(13) . . ? O16 U1 O4 79.80(14) . . ? O3 U1 O4 66.91(13) . . ? O8 U1 O15 135.88(13) . . ? O11 U1 O15 75.68(14) . . ? O16 U1 O15 66.24(13) . . ? O3 U1 O15 69.60(13) . . ? O4 U1 O15 129.58(14) . . ? O8 U1 O7 66.87(13) . . ? O11 U1 O7 74.18(14) . . ? O16 U1 O7 134.26(14) . . ? O3 U1 O7 104.33(14) . . ? O4 U1 O7 143.70(14) . . ? O15 U1 O7 71.37(14) . . ? O8 U1 O12 72.10(13) . . ? O11 U1 O12 65.82(13) . . ? O16 U1 O12 71.44(14) . . ? O3 U1 O12 129.08(13) . . ? O4 U1 O12 69.24(14) . . ? O15 U1 O12 126.68(13) . . ? O7 U1 O12 126.40(13) . . ? O8 U1 O17 68.41(14) . . ? O11 U1 O17 140.32(15) . . ? O16 U1 O17 139.98(14) . . ? O3 U1 O17 66.32(14) . . ? O4 U1 O17 72.58(17) . . ? O15 U1 O17 111.27(16) . . ? O7 U1 O17 71.82(16) . . ? O12 U1 O17 121.98(16) . . ? O8 U1 K1 103.36(10) . . ? O11 U1 K1 75.30(9) . . ? O16 U1 K1 100.64(10) . . ? O3 U1 K1 82.56(9) . . ? O4 U1 K1 148.62(9) . . ? O15 U1 K1 34.94(9) . . ? O7 U1 K1 36.81(9) . . ? O12 U1 K1 141.09(9) . . ? O17 U1 K1 89.11(14) . . ? O8 U1 K1 78.14(10) . 1_565 ? O11 U1 K1 98.55(9) . 1_565 ? O16 U1 K1 74.97(10) . 1_565 ? O3 U1 K1 101.25(9) . 1_565 ? O4 U1 K1 36.68(9) . 1_565 ? O15 U1 K1 141.20(9) . 1_565 ? O7 U1 K1 144.96(9) . 1_565 ? O12 U1 K1 32.76(9) . 1_565 ? O17 U1 K1 97.62(14) . 1_565 ? K1 U1 K1 173.15(4) . 1_565 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.458 _refine_diff_density_min -1.361 _refine_diff_density_rms 0.345 #===END data_SP4 _database_code_depnum_ccdc_archive 'CCDC 266741' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C8 H10 K2 Mn O21 Zr' _chemical_formula_sum 'C8 H10 K2 Mn O21 Zr' _chemical_formula_weight 666.5 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' 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' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -2.9673 0.5597 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/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 11.819(5) _cell_length_b 12.630(5) _cell_length_c 14.699(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 106.769(5) _cell_angle_gamma 90.000(5) _cell_volume 2100.9(14) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1 _cell_measurement_theta_max 20 _exptl_crystal_description prisme _exptl_crystal_colour white _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.107 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1316 _exptl_absorpt_coefficient_mu 1.594 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.8 _exptl_absorpt_correction_T_max 0.89 _exptl_absorpt_process_details ? _exptl_special_details ; The H atoms corresponding to H2O molecules have not been located and refined in the structure but have been considered for the formula, molecular mass, density, absorption coefficient, and F(000). ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6857 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0455 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 34.95 _reflns_number_total 6857 _reflns_number_gt 6857 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^ > 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^)+(0.1474P)^2^+7.0523P] 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 SHELXL _refine_ls_extinction_coef 0.0105(16) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6857 _refine_ls_number_parameters 317 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0777 _refine_ls_R_factor_gt 0.0777 _refine_ls_wR_factor_ref 0.2420 _refine_ls_wR_factor_gt 0.2420 _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_restrained_S_all 1.093 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr1 Zr 0.67327(3) 0.56069(3) 0.79184(3) 0.01921(14) Uani 1 1 d . . . K1 K 0.42759(11) 0.71203(10) 0.59627(8) 0.0329(2) Uani 1 1 d . . . K2 K 0.71766(13) 0.26285(10) 0.86489(9) 0.0389(3) Uani 1 1 d . . . O15 O 0.5995(3) 0.4584(3) 0.8855(3) 0.0274(7) Uani 1 1 d . . . O9 O 0.6415(3) 0.5843(3) 0.6369(2) 0.0270(6) Uani 1 1 d . . . O1 O 0.8406(3) 0.6135(3) 0.7756(3) 0.0280(7) Uani 1 1 d . . . O16 O 0.4795(3) 0.5748(3) 0.7472(3) 0.0322(8) Uani 1 1 d . . . O8 O 0.7030(3) 0.6485(3) 0.9238(2) 0.0287(7) Uani 1 1 d . . . O7 O 0.6360(3) 0.7310(3) 0.7584(2) 0.0281(7) Uani 1 1 d . . . O2 O 0.8153(3) 0.4640(3) 0.8832(2) 0.0258(6) Uani 1 1 d . . . O3 O 1.0370(4) 0.5992(4) 0.8190(4) 0.0432(10) Uani 1 1 d . . . O6 O 0.6038(5) 0.8889(3) 0.8138(3) 0.0461(11) Uani 1 1 d . . . O20 O 0.8261(6) 0.2189(6) 1.0601(5) 0.0737(18) Uani 1 1 d . . . C2 C 0.9241(4) 0.4754(4) 0.8822(3) 0.0237(8) Uani 1 1 d . . . C1 C 0.9406(4) 0.5714(4) 0.8213(4) 0.0273(9) Uani 1 1 d . . . O13 O 0.3070(5) 0.5092(6) 0.7574(5) 0.0710(19) Uani 1 1 d . . . C4 C 0.6340(4) 0.7963(4) 0.8251(3) 0.0259(8) Uani 1 1 d . . . O14 O 0.4368(5) 0.3875(6) 0.9075(6) 0.082(2) Uani 1 1 d . . . C6 C 0.6301(4) 0.5035(4) 0.5811(3) 0.0258(8) Uani 1 1 d . . . O22 O 0.6155(9) 0.3175(9) 0.0813(6) 0.105(3) Uani 1 1 d . . . O21 O 0.3155(8) 0.8062(10) 0.7266(6) 0.117(4) Uani 1 1 d . . . C8 C 0.4888(5) 0.4475(5) 0.8672(4) 0.0361(11) Uani 1 1 d . . . C7 C 0.4157(5) 0.5151(6) 0.7843(5) 0.0397(13) Uani 1 1 d . . . O10 O 0.6380(4) 0.4087(3) 0.7215(2) 0.0302(7) Uani 1 1 d . . . O23 O 0.6376(3) 0.8359(4) 0.1694(3) 0.0431(12) Uani 1 1 d . . . O24A O 0.5357(8) 0.8879(8) 0.0273(7) 0.0318(18) Uani 0.40 1 d P . . O4 O 1.0066(3) 0.4181(3) 0.9218(3) 0.0323(7) Uani 1 1 d . . . O12 O 0.6313(4) 0.5044(3) 0.4985(3) 0.0365(9) Uani 1 1 d . . . O5 O 0.6821(4) 0.7990(3) 0.9962(3) 0.0368(8) Uani 1 1 d . . . O11 O 0.5861(4) 0.3169(3) 0.5861(3) 0.0376(9) Uani 1 1 d . . . C5 C 0.6160(4) 0.3986(4) 0.6310(3) 0.0251(8) Uani 1 1 d . . . C3 C 0.6751(4) 0.7467(4) 0.9252(3) 0.0252(8) Uani 1 1 d . . . Mn1 Mn 0.76678(10) 0.50272(12) 1.06775(9) 0.0578(3) Uani 1 1 d . . . O24C O 0.4003(9) 0.9862(9) 0.0410(10) 0.049(3) Uani 0.40 1 d P . . O24B O 0.4097(17) 0.9106(19) 0.0782(14) 0.036(5) Uani 0.20 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zr1 0.0173(2) 0.0206(2) 0.01847(19) 0.00197(13) 0.00309(13) -0.00011(13) K1 0.0344(5) 0.0337(5) 0.0258(5) 0.0019(4) 0.0014(4) 0.0025(4) K2 0.0501(7) 0.0280(5) 0.0386(6) -0.0024(4) 0.0128(5) 0.0081(5) O15 0.0224(15) 0.0323(16) 0.0287(16) 0.0059(13) 0.0093(12) -0.0014(12) O9 0.0333(18) 0.0249(14) 0.0214(14) 0.0005(12) 0.0058(13) -0.0034(13) O1 0.0193(14) 0.0289(16) 0.0341(17) 0.0082(13) 0.0047(13) 0.0009(12) O16 0.0191(15) 0.044(2) 0.0342(18) 0.0114(15) 0.0080(13) 0.0071(14) O8 0.0331(17) 0.0274(16) 0.0235(14) 0.0036(12) 0.0048(13) 0.0039(13) O7 0.0339(18) 0.0243(15) 0.0229(14) 0.0022(12) 0.0032(13) 0.0039(13) O2 0.0190(14) 0.0292(15) 0.0270(15) 0.0055(12) 0.0032(12) 0.0010(12) O3 0.0214(17) 0.048(2) 0.059(3) 0.011(2) 0.0097(17) -0.0039(16) O6 0.069(3) 0.0263(18) 0.041(2) 0.0010(16) 0.012(2) 0.0129(19) O20 0.063(4) 0.079(4) 0.080(4) -0.013(4) 0.021(3) 0.003(3) C2 0.0198(18) 0.0245(18) 0.0246(18) -0.0026(15) 0.0027(15) 0.0025(15) C1 0.023(2) 0.028(2) 0.030(2) -0.0003(16) 0.0058(17) 0.0009(16) O13 0.027(2) 0.107(5) 0.078(4) 0.034(4) 0.012(2) 0.003(3) C4 0.0222(19) 0.0255(19) 0.028(2) 0.0010(16) 0.0049(16) 0.0009(15) O14 0.035(3) 0.104(5) 0.110(5) 0.071(4) 0.029(3) 0.001(3) C6 0.023(2) 0.032(2) 0.0228(18) 0.0004(16) 0.0074(15) 0.0023(16) O22 0.101(6) 0.136(8) 0.080(5) -0.003(6) 0.029(5) 0.007(6) O21 0.104(6) 0.186(10) 0.061(4) -0.004(5) 0.024(4) 0.080(7) C8 0.027(2) 0.043(3) 0.040(3) 0.014(2) 0.012(2) 0.001(2) C7 0.024(2) 0.055(3) 0.043(3) 0.017(3) 0.013(2) 0.005(2) O10 0.040(2) 0.0247(15) 0.0245(15) 0.0022(12) 0.0071(14) 0.0024(14) O23 0.0212(15) 0.067(3) 0.050(2) -0.048(2) 0.0248(16) -0.0229(17) O24A 0.028(4) 0.037(5) 0.034(4) -0.006(4) 0.015(4) 0.001(4) O4 0.0246(17) 0.0326(17) 0.0358(18) 0.0016(14) 0.0027(14) 0.0069(13) O12 0.049(2) 0.041(2) 0.0220(16) -0.0005(14) 0.0135(16) 0.0021(18) O5 0.047(2) 0.0358(19) 0.0297(17) -0.0070(15) 0.0136(16) -0.0004(17) O11 0.054(3) 0.0262(17) 0.0310(18) -0.0085(14) 0.0092(17) -0.0021(16) C5 0.025(2) 0.026(2) 0.0224(18) -0.0011(15) 0.0038(15) 0.0041(15) C3 0.0232(19) 0.0255(19) 0.0269(19) -0.0020(15) 0.0069(16) -0.0019(15) Mn1 0.0405(6) 0.0842(9) 0.0480(6) 0.0189(6) 0.0118(5) 0.0056(6) O24C 0.029(5) 0.036(6) 0.085(9) -0.033(6) 0.022(5) 0.004(4) O24B 0.025(8) 0.051(12) 0.036(9) -0.027(9) 0.017(7) -0.011(8) _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 Zr1 O10 2.163(4) . ? Zr1 O1 2.165(4) . ? Zr1 O8 2.173(4) . ? Zr1 O2 2.194(3) . ? Zr1 O16 2.200(4) . ? Zr1 O9 2.219(3) . ? Zr1 O7 2.222(4) . ? Zr1 O15 2.239(3) . ? Zr1 K2 3.8990(16) 2_656 ? Zr1 K2 3.9056(19) . ? Zr1 K1 3.9411(15) . ? K1 O11 2.664(4) 3_666 ? K1 O16 2.742(4) . ? K1 O4 2.751(4) 2_656 ? K1 O5 2.853(5) 4_575 ? K1 O21 2.881(8) . ? K1 O7 2.902(4) . ? K1 O9 2.912(4) . ? K1 O12 3.056(5) 3_666 ? K1 C3 3.342(5) 4_575 ? K1 C5 3.519(5) 3_666 ? K1 Mn1 4.038(2) 4_575 ? K2 O1 2.734(4) 2_646 ? K2 O10 2.753(4) . ? K2 O2 2.771(4) . ? K2 O9 2.807(4) 2_646 ? K2 O20 2.839(8) . ? K2 O7 2.871(4) 2_646 ? K2 O15 2.896(4) . ? K2 O24B 2.91(2) 3_666 ? K2 Zr1 3.8990(16) 2_646 ? K2 K1 4.115(3) 2_646 ? O15 C8 1.265(7) . ? O9 C6 1.292(6) . ? O9 K2 2.807(4) 2_656 ? O1 C1 1.293(6) . ? O1 K2 2.734(4) 2_656 ? O16 C7 1.293(7) . ? O8 C3 1.285(6) . ? O7 C4 1.286(6) . ? O7 K2 2.871(4) 2_656 ? O2 C2 1.298(6) . ? O3 C1 1.201(6) . ? O6 C4 1.220(6) . ? C2 O4 1.219(6) . ? C2 C1 1.553(7) . ? O13 C7 1.233(7) . ? C4 C3 1.544(7) . ? O14 C8 1.230(7) . ? C6 O12 1.219(6) . ? C6 C5 1.546(7) . ? C8 C7 1.533(8) . ? O10 C5 1.287(6) . ? O4 K1 2.751(4) 2_646 ? O12 K1 3.056(5) 3_666 ? O5 C3 1.217(6) . ? O5 K1 2.853(5) 4_676 ? O11 C5 1.220(6) . ? O11 K1 2.664(4) 3_666 ? C5 K1 3.519(5) 3_666 ? C3 K1 3.342(5) 4_676 ? Mn1 K1 4.038(2) 4_676 ? O24C O24B 1.09(3) . ? O24B K2 2.91(2) 3_666 ? 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 O10 Zr1 O1 106.07(15) . . ? O10 Zr1 O8 147.00(13) . . ? O1 Zr1 O8 91.37(15) . . ? O10 Zr1 O2 78.83(14) . . ? O1 Zr1 O2 71.12(13) . . ? O8 Zr1 O2 80.79(14) . . ? O10 Zr1 O16 83.61(16) . . ? O1 Zr1 O16 147.98(14) . . ? O8 Zr1 O16 96.38(15) . . ? O2 Zr1 O16 140.78(14) . . ? O10 Zr1 O9 71.13(13) . . ? O1 Zr1 O9 74.61(14) . . ? O8 Zr1 O9 141.57(13) . . ? O2 Zr1 O9 125.16(14) . . ? O16 Zr1 O9 80.20(14) . . ? O10 Zr1 O7 139.02(13) . . ? O1 Zr1 O7 78.84(14) . . ? O8 Zr1 O7 70.98(13) . . ? O2 Zr1 O7 137.90(14) . . ? O16 Zr1 O7 74.52(15) . . ? O9 Zr1 O7 71.26(13) . . ? O10 Zr1 O15 74.12(14) . . ? O1 Zr1 O15 140.85(13) . . ? O8 Zr1 O15 74.75(14) . . ? O2 Zr1 O15 70.59(13) . . ? O16 Zr1 O15 70.95(14) . . ? O9 Zr1 O15 136.71(14) . . ? O7 Zr1 O15 127.37(14) . . ? O10 Zr1 K2 110.48(10) . 2_656 ? O1 Zr1 K2 42.67(9) . 2_656 ? O8 Zr1 K2 101.38(10) . 2_656 ? O2 Zr1 K2 113.63(10) . 2_656 ? O16 Zr1 K2 105.31(10) . 2_656 ? O9 Zr1 K2 44.96(10) . 2_656 ? O7 Zr1 K2 46.65(10) . 2_656 ? O15 Zr1 K2 174.02(10) . 2_656 ? O10 Zr1 K2 43.00(10) . . ? O1 Zr1 K2 105.81(10) . . ? O8 Zr1 K2 105.77(10) . . ? O2 Zr1 K2 43.71(10) . . ? O16 Zr1 K2 101.86(11) . . ? O9 Zr1 K2 112.41(10) . . ? O7 Zr1 K2 174.58(10) . . ? O15 Zr1 K2 47.21(10) . . ? K2 Zr1 K2 138.77(2) 2_656 . ? O10 Zr1 K1 94.70(10) . . ? O1 Zr1 K1 105.93(10) . . ? O8 Zr1 K1 107.39(10) . . ? O2 Zr1 K1 171.55(10) . . ? O16 Zr1 K1 42.17(10) . . ? O9 Zr1 K1 46.78(10) . . ? O7 Zr1 K1 46.53(10) . . ? O15 Zr1 K1 113.12(10) . . ? K2 Zr1 K1 63.32(4) 2_656 . ? K2 Zr1 K1 132.84(3) . . ? O11 K1 O16 131.44(13) 3_666 . ? O11 K1 O4 88.26(13) 3_666 2_656 ? O16 K1 O4 132.27(13) . 2_656 ? O11 K1 O5 73.58(13) 3_666 4_575 ? O16 K1 O5 110.07(12) . 4_575 ? O4 K1 O5 105.68(12) 2_656 4_575 ? O11 K1 O21 145.05(19) 3_666 . ? O16 K1 O21 76.2(2) . . ? O4 K1 O21 82.6(3) 2_656 . ? O5 K1 O21 76.6(2) 4_575 . ? O11 K1 O7 128.94(13) 3_666 . ? O16 K1 O7 56.55(11) . . ? O4 K1 O7 78.72(11) 2_656 . ? O5 K1 O7 157.47(12) 4_575 . ? O21 K1 O7 82.2(2) . . ? O11 K1 O9 85.83(12) 3_666 . ? O16 K1 O9 60.36(11) . . ? O4 K1 O9 106.91(12) 2_656 . ? O5 K1 O9 140.58(12) 4_575 . ? O21 K1 O9 129.10(18) . . ? O7 K1 O9 52.84(10) . . ? O11 K1 O12 58.59(11) 3_666 3_666 ? O16 K1 O12 76.79(12) . 3_666 ? O4 K1 O12 146.72(12) 2_656 3_666 ? O5 K1 O12 69.96(12) 4_575 3_666 ? O21 K1 O12 125.7(3) . 3_666 ? O7 K1 O12 118.42(11) . 3_666 ? O9 K1 O12 70.62(11) . 3_666 ? O11 K1 C3 58.85(13) 3_666 4_575 ? O16 K1 C3 130.55(12) . 4_575 ? O4 K1 C3 89.76(12) 2_656 4_575 ? O5 K1 C3 20.80(11) 4_575 4_575 ? O21 K1 C3 87.35(19) . 4_575 ? O7 K1 C3 165.31(12) . 4_575 ? O9 K1 C3 140.79(11) . 4_575 ? O12 K1 C3 76.13(12) 3_666 4_575 ? O11 K1 C5 16.35(12) 3_666 3_666 ? O16 K1 C5 117.02(13) . 3_666 ? O4 K1 C5 104.61(12) 2_656 3_666 ? O5 K1 C5 69.07(12) 4_575 3_666 ? O21 K1 C5 145.6(2) . 3_666 ? O7 K1 C5 132.03(12) . 3_666 ? O9 K1 C5 81.69(11) . 3_666 ? O12 K1 C5 42.31(11) 3_666 3_666 ? C3 K1 C5 59.57(11) 4_575 3_666 ? O11 K1 Zr1 119.04(11) 3_666 . ? O16 K1 Zr1 32.59(8) . . ? O4 K1 Zr1 111.09(9) 2_656 . ? O5 K1 Zr1 141.09(9) 4_575 . ? O21 K1 Zr1 95.65(17) . . ? O7 K1 Zr1 33.75(7) . . ? O9 K1 Zr1 33.73(7) . . ? O12 K1 Zr1 85.50(9) 3_666 . ? C3 K1 Zr1 159.14(9) 4_575 . ? C5 K1 Zr1 112.03(8) 3_666 . ? O11 K1 Mn1 97.36(10) 3_666 4_575 ? O16 K1 Mn1 129.55(9) . 4_575 ? O4 K1 Mn1 44.25(9) 2_656 4_575 ? O5 K1 Mn1 67.15(9) 4_575 4_575 ? O21 K1 Mn1 53.7(2) . 4_575 ? O7 K1 Mn1 105.92(8) . 4_575 ? O9 K1 Mn1 150.49(8) . 4_575 ? O12 K1 Mn1 135.42(9) 3_666 4_575 ? C3 K1 Mn1 59.42(9) 4_575 4_575 ? C5 K1 Mn1 108.67(8) 3_666 4_575 ? Zr1 K1 Mn1 137.23(4) . 4_575 ? O1 K2 O10 85.85(12) 2_646 . ? O1 K2 O2 135.47(12) 2_646 . ? O10 K2 O2 60.10(11) . . ? O1 K2 O9 57.29(11) 2_646 2_646 ? O10 K2 O9 127.10(12) . 2_646 ? O2 K2 O9 120.38(12) . 2_646 ? O1 K2 O20 124.76(18) 2_646 . ? O10 K2 O20 149.26(18) . . ? O2 K2 O20 91.57(18) . . ? O9 K2 O20 75.91(16) 2_646 . ? O1 K2 O7 59.54(11) 2_646 2_646 ? O10 K2 O7 75.28(12) . 2_646 ? O2 K2 O7 83.10(11) . 2_646 ? O9 K2 O7 54.18(10) 2_646 2_646 ? O20 K2 O7 115.61(17) . 2_646 ? O1 K2 O15 130.05(12) 2_646 . ? O10 K2 O15 55.97(11) . . ? O2 K2 O15 53.69(11) . . ? O9 K2 O15 172.37(12) 2_646 . ? O20 K2 O15 98.73(16) . . ? O7 K2 O15 125.57(11) 2_646 . ? O1 K2 O24B 70.1(3) 2_646 3_666 ? O10 K2 O24B 129.2(5) . 3_666 ? O2 K2 O24B 153.7(3) . 3_666 ? O9 K2 O24B 75.9(4) 2_646 3_666 ? O20 K2 O24B 71.5(4) . 3_666 ? O7 K2 O24B 122.1(4) 2_646 3_666 ? O15 K2 O24B 107.9(4) . 3_666 ? O1 K2 Zr1 32.46(7) 2_646 2_646 ? O10 K2 Zr1 94.84(9) . 2_646 ? O2 K2 Zr1 117.26(9) . 2_646 ? O9 K2 Zr1 33.95(7) 2_646 2_646 ? O20 K2 Zr1 109.84(15) . 2_646 ? O7 K2 Zr1 34.24(7) 2_646 2_646 ? O15 K2 Zr1 150.68(8) . 2_646 ? O24B K2 Zr1 87.9(3) 3_666 2_646 ? O1 K2 Zr1 118.19(9) 2_646 . ? O10 K2 Zr1 32.40(8) . . ? O2 K2 Zr1 33.16(7) . . ? O9 K2 Zr1 143.52(9) 2_646 . ? O20 K2 Zr1 116.85(16) . . ? O7 K2 Zr1 91.10(8) 2_646 . ? O15 K2 Zr1 34.57(7) . . ? O24B K2 Zr1 139.8(4) 3_666 . ? Zr1 K2 Zr1 120.62(4) 2_646 . ? O1 K2 K1 91.25(8) 2_646 2_646 ? O10 K2 K1 108.69(10) . 2_646 ? O2 K2 K1 75.54(8) . 2_646 ? O9 K2 K1 45.00(8) 2_646 2_646 ? O20 K2 K1 71.62(14) . 2_646 ? O7 K2 K1 44.83(8) 2_646 2_646 ? O15 K2 K1 128.40(8) . 2_646 ? O24B K2 K1 115.7(4) 3_666 2_646 ? Zr1 K2 K1 58.84(3) 2_646 2_646 ? Zr1 K2 K1 103.83(4) . 2_646 ? C8 O15 Zr1 119.6(3) . . ? C8 O15 K2 112.6(4) . . ? Zr1 O15 K2 98.22(13) . . ? C6 O9 Zr1 120.1(3) . . ? C6 O9 K2 125.6(3) . 2_656 ? Zr1 O9 K2 101.10(13) . 2_656 ? C6 O9 K1 112.5(3) . . ? Zr1 O9 K1 99.49(13) . . ? K2 O9 K1 92.02(11) 2_656 . ? C1 O1 Zr1 122.9(3) . . ? C1 O1 K2 132.0(3) . 2_656 ? Zr1 O1 K2 104.87(13) . 2_656 ? C7 O16 Zr1 120.7(3) . . ? C7 O16 K1 133.5(3) . . ? Zr1 O16 K1 105.25(14) . . ? C3 O8 Zr1 122.1(3) . . ? C4 O7 Zr1 119.9(3) . . ? C4 O7 K2 122.6(3) . 2_656 ? Zr1 O7 K2 99.11(13) . 2_656 ? C4 O7 K1 118.7(3) . . ? Zr1 O7 K1 99.72(13) . . ? K2 O7 K1 90.93(11) 2_656 . ? C2 O2 Zr1 121.2(3) . . ? C2 O2 K2 119.1(3) . . ? Zr1 O2 K2 103.13(13) . . ? O4 C2 O2 126.0(5) . . ? O4 C2 C1 121.5(4) . . ? O2 C2 C1 112.5(4) . . ? O3 C1 O1 126.7(5) . . ? O3 C1 C2 121.5(5) . . ? O1 C1 C2 111.8(4) . . ? O6 C4 O7 125.5(5) . . ? O6 C4 C3 121.2(5) . . ? O7 C4 C3 113.4(4) . . ? O12 C6 O9 126.6(5) . . ? O12 C6 C5 121.0(4) . . ? O9 C6 C5 112.4(4) . . ? O14 C8 O15 126.5(6) . . ? O14 C8 C7 118.7(5) . . ? O15 C8 C7 114.8(5) . . ? O13 C7 O16 125.4(6) . . ? O13 C7 C8 121.2(6) . . ? O16 C7 C8 113.4(5) . . ? C5 O10 Zr1 122.4(3) . . ? C5 O10 K2 130.4(3) . . ? Zr1 O10 K2 104.59(14) . . ? C2 O4 K1 136.5(3) . 2_646 ? C6 O12 K1 112.3(3) . 3_666 ? C3 O5 K1 102.9(3) . 4_676 ? C5 O11 K1 125.7(3) . 3_666 ? O11 C5 O10 125.7(5) . . ? O11 C5 C6 121.5(4) . . ? O10 C5 C6 112.9(4) . . ? O11 C5 K1 37.9(3) . 3_666 ? O10 C5 K1 162.1(3) . 3_666 ? C6 C5 K1 84.0(2) . 3_666 ? O5 C3 O8 125.7(5) . . ? O5 C3 C4 121.5(5) . . ? O8 C3 C4 112.8(4) . . ? O5 C3 K1 56.3(3) . 4_676 ? O8 C3 K1 89.2(3) . 4_676 ? C4 C3 K1 128.4(3) . 4_676 ? O24C O24B K2 144.7(15) . 3_666 ? _diffrn_measured_fraction_theta_max 0.745 _diffrn_reflns_theta_full 34.95 _diffrn_measured_fraction_theta_full 0.745 _refine_diff_density_max 2.672 _refine_diff_density_min -3.164 _refine_diff_density_rms 0.268 #===END #===END data_SPA3 _database_code_depnum_ccdc_archive 'CCDC 275039' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C7 H2 K Mg O15 U), 9(H2 O)' _chemical_formula_sum 'C14 H22 K2 Mg2 O39 U2' _chemical_formula_weight 1417.20 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' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mg Mg 0.0486 0.0363 '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' U U -9.6767 9.6646 '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 20.437(3) _cell_length_b 12.841(4) _cell_length_c 14.614(4) _cell_angle_alpha 90.00 _cell_angle_beta 94.52(3) _cell_angle_gamma 90.00 _cell_volume 3823.2(17) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1 _cell_measurement_theta_max 20 _exptl_crystal_description prisme _exptl_crystal_colour green _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.462 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2656 _exptl_absorpt_coefficient_mu 8.838 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details scalepack _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9529 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0276 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 4.13 _diffrn_reflns_theta_max 36.32 _reflns_number_total 9529 _reflns_number_gt 6805 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^ > 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^)+(0.0805P)^2^+54.0236P] 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 SHELXL _refine_ls_extinction_coef 0.00208(11) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 9529 _refine_ls_number_parameters 276 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0658 _refine_ls_R_factor_gt 0.0482 _refine_ls_wR_factor_ref 0.1510 _refine_ls_wR_factor_gt 0.1362 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group U1 U 0.805291(7) 0.248908(11) 0.210959(10) 0.01530(7) Uani 1 1 d . . . K1 K 0.78768(10) 0.0000 0.43504(12) 0.0335(4) Uani 1 2 d S . . K2 K 0.93868(8) 0.0000 0.59104(13) 0.0322(3) Uani 1 2 d S . . O1 O 0.92275(19) 0.2240(4) 0.2104(3) 0.0279(7) Uani 1 1 d . . . O2 O 0.85250(19) 0.1387(4) 0.3300(3) 0.0319(9) Uani 1 1 d . . . O3 O 0.9410(3) 0.1165(7) 0.4288(4) 0.068(2) Uani 1 1 d . . . O4 O 1.0148(2) 0.1617(5) 0.2826(4) 0.0530(14) Uani 1 1 d . . . O5' O 0.71275(19) 0.2748(3) 0.2998(3) 0.0258(7) Uani 1 1 d . . . O6 O 0.8288(2) 0.3456(4) 0.3479(3) 0.0340(9) Uani 1 1 d . . . O7 O 0.6700(2) 0.3668(4) 0.4108(3) 0.0384(10) Uani 1 1 d . . . O8 O 0.8012(2) 0.3744(5) 0.4912(3) 0.0446(12) Uani 1 1 d . . . O9 O 0.8320(2) 0.0870(3) 0.1247(3) 0.0296(8) Uani 1 1 d . . . O10 O 0.73892(19) 0.0868(3) 0.2412(3) 0.0258(7) Uani 1 1 d . . . O11 O 0.87348(18) 0.4126(3) 0.1901(3) 0.0279(7) Uani 1 1 d . . . O12 O 0.74329(18) 0.4132(3) 0.1695(3) 0.0280(7) Uani 1 1 d . . . O13 O 0.71009(19) 0.2204(3) 0.0979(2) 0.0255(7) Uani 1 1 d . . . C1 C 0.9552(3) 0.1779(5) 0.2761(4) 0.0296(10) Uani 1 1 d . . . C2 C 0.9141(3) 0.1403(5) 0.3525(4) 0.0337(12) Uani 1 1 d . . . C3 C 0.7880(3) 0.3527(4) 0.4095(4) 0.0269(9) Uani 1 1 d . . . C4 C 0.7166(2) 0.3310(4) 0.3717(3) 0.0245(9) Uani 1 1 d . . . C5 C 0.8120(3) 0.0000 0.1488(5) 0.0208(11) Uani 1 2 d S . . C6 C 0.7580(3) 0.0000 0.2157(5) 0.0201(11) Uani 1 2 d S . . C7 C 0.8458(3) 0.5000 0.1863(5) 0.0203(11) Uani 1 2 d S . . C8 C 0.7708(3) 0.5000 0.1740(5) 0.0218(11) Uani 1 2 d S . . C9 C 0.7160(2) 0.2319(4) 0.0139(3) 0.0189(7) Uani 1 1 d . . . O33 O 0.9340(3) 0.1246(8) 0.0079(5) 0.076(2) Uani 1 1 d . . . O34 O 0.9589(4) 0.3637(8) 0.0598(7) 0.099(3) Uani 1 1 d . . . O35 O 0.8830 0.5000 0.9631 0.298(19) Uani 1 2 d S . . O30 O 0.88903(15) 0.1569(4) 0.8317(3) 0.0300(9) Uani 1 1 d . . . O14 O 0.67262(18) 0.2165(3) -0.0497(2) 0.0250(7) Uani 1 1 d . . . O31 O 0.8940(7) 0.3636(19) 0.759(2) 0.35(2) Uani 1 1 d . . . Mg1 Mg 0.57814(13) 0.2090(3) 0.4333(2) 0.0571(8) Uani 1 1 d . . . O32 O 0.4611(4) 0.1077(7) 0.3981(10) 0.123(5) Uani 1 1 d . . . H32A H 0.4678 0.0348 0.4071 0.184 Uiso 1 1 d . . . H32C H 0.4308 0.1319 0.4427 0.184 Uiso 1 1 d . . . H30A H 0.8669 0.1049 0.7902 0.084 Uiso 1 1 d . . . H30B H 0.9100 0.0919 0.8472 0.036 Uiso 1 1 d . . . H33A H 0.8945 0.1370 0.0370 2.000 Uiso 1 1 d . . . H33B H 0.9515 0.1316 0.0687 0.164 Uiso 1 1 d . . . H35 H 0.9094 0.4524 0.9824 0.005 Uiso 1 1 d . . . H34A H 0.9501 0.3450 0.1136 0.100 Uiso 1 1 d . . . H31A H 0.8915 0.4013 0.7140 0.000 Uiso 1 1 d . . . H31B H 0.8514 0.3417 0.7395 2.000 Uiso 1 1 d . . . H34C H 1.0009 0.3481 0.0848 0.068 Uiso 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 U1 0.01445(9) 0.01522(9) 0.01617(9) 0.00058(5) 0.00082(5) 0.00107(5) K1 0.0424(9) 0.0344(8) 0.0255(7) 0.000 0.0151(6) 0.000 K2 0.0249(7) 0.0371(9) 0.0337(8) 0.000 -0.0025(6) 0.000 O1 0.0217(16) 0.0310(17) 0.0313(19) 0.0086(16) 0.0033(13) 0.0016(14) O2 0.0246(17) 0.042(2) 0.0295(18) 0.0164(17) 0.0042(14) 0.0029(16) O3 0.040(3) 0.116(6) 0.046(3) 0.040(3) -0.005(2) 0.020(3) O4 0.0212(19) 0.081(4) 0.057(3) 0.018(3) 0.0054(19) 0.013(2) O5' 0.0216(16) 0.0298(16) 0.0264(17) -0.0067(15) 0.0048(13) -0.0030(14) O6 0.0255(18) 0.047(2) 0.0295(18) -0.0134(18) 0.0027(14) -0.0038(17) O7 0.030(2) 0.043(2) 0.044(2) -0.014(2) 0.0125(17) 0.0031(18) O8 0.035(2) 0.070(3) 0.028(2) -0.016(2) -0.0021(16) 0.003(2) O9 0.039(2) 0.0201(15) 0.0318(18) 0.0013(14) 0.0164(16) -0.0012(14) O10 0.0266(17) 0.0181(15) 0.0336(18) -0.0011(13) 0.0084(14) 0.0010(12) O11 0.0206(15) 0.0208(16) 0.042(2) 0.0004(15) 0.0013(14) 0.0025(13) O12 0.0216(16) 0.0184(15) 0.044(2) 0.0018(14) -0.0004(14) -0.0026(12) O13 0.0254(16) 0.0319(17) 0.0190(14) 0.0022(14) 0.0017(12) -0.0050(15) C1 0.0189(19) 0.035(3) 0.034(2) 0.007(2) 0.0008(17) 0.0056(19) C2 0.029(2) 0.043(3) 0.029(2) 0.013(2) 0.0005(19) 0.013(2) C3 0.025(2) 0.030(2) 0.026(2) -0.0067(18) 0.0023(17) 0.0052(18) C4 0.026(2) 0.023(2) 0.026(2) -0.0022(16) 0.0060(16) 0.0017(16) C5 0.022(3) 0.020(3) 0.020(3) 0.000 0.002(2) 0.000 C6 0.018(2) 0.021(3) 0.022(3) 0.000 0.001(2) 0.000 C7 0.022(3) 0.017(2) 0.021(3) 0.000 0.001(2) 0.000 C8 0.023(3) 0.018(3) 0.024(3) 0.000 0.000(2) 0.000 C9 0.0171(16) 0.0217(18) 0.0177(17) 0.0024(14) -0.0001(13) -0.0013(14) O33 0.041(3) 0.136(7) 0.053(3) 0.012(4) 0.024(3) 0.008(4) O34 0.080(5) 0.120(8) 0.104(7) 0.013(6) 0.062(5) 0.003(5) O35 0.28(4) 0.26(4) 0.35(5) 0.000 0.00(4) 0.000 O30 0.0064(11) 0.060(3) 0.0239(15) -0.0060(17) 0.0041(10) 0.0075(14) O14 0.0212(15) 0.0336(18) 0.0198(15) 0.0042(14) -0.0015(11) -0.0052(14) O31 0.081(8) 0.35(3) 0.63(5) -0.36(3) 0.105(16) -0.071(13) Mg1 0.0359(13) 0.0503(16) 0.081(2) 0.0128(15) -0.0217(13) -0.0168(12) O32 0.051(4) 0.055(4) 0.252(14) 0.006(6) -0.054(6) -0.004(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 U1 O6 2.372(4) . ? U1 O2 2.386(4) . ? U1 O5' 2.400(4) . ? U1 O1 2.422(4) . ? U1 O14 2.474(4) 7_655 ? U1 O13 2.478(4) . ? U1 O12 2.511(4) . ? U1 O9 2.513(4) . ? U1 O10 2.543(4) . ? U1 O11 2.553(4) . ? K1 O8 2.715(5) 7_656 ? K1 O8 2.715(5) 4_646 ? K1 O2 2.758(4) 6 ? K1 O2 2.758(4) . ? K1 O7 2.906(5) 7_656 ? K1 O7 2.906(5) 4_646 ? K1 O10 3.132(4) 6 ? K1 O10 3.132(4) . ? K1 C6 3.215(7) . ? K1 C3 3.418(5) 7_656 ? K1 C3 3.418(5) 4_646 ? K1 C2 3.444(6) 6 ? K2 O7 2.802(5) 4_646 ? K2 O7 2.802(5) 7_656 ? K2 O3 2.807(6) 6 ? K2 O3 2.807(6) . ? K2 O4 2.889(6) 2_756 ? K2 O4 2.889(6) 5_756 ? K2 O3 2.912(7) 2_756 ? K2 O3 2.912(7) 5_756 ? K2 Mg1 3.767(3) 4_646 ? K2 Mg1 3.767(3) 7_656 ? K2 K2 3.797(4) 5_756 ? O1 C1 1.270(7) . ? O2 C2 1.275(7) . ? O3 C2 1.243(7) . ? O3 K2 2.912(7) 5_756 ? O4 C1 1.232(7) . ? O4 K2 2.889(6) 5_756 ? O5' C4 1.272(6) . ? O6 C3 1.278(6) . ? O7 C4 1.237(6) . ? O7 K2 2.802(5) 7_656 ? O7 K1 2.906(5) 7_656 ? O8 C3 1.236(7) . ? O8 K1 2.715(5) 7_656 ? O9 C5 1.250(5) . ? O10 C6 1.247(5) . ? O11 C7 1.256(5) . ? O12 C8 1.247(5) . ? O13 C9 1.252(6) . ? C1 C2 1.527(8) . ? C3 C4 1.543(8) . ? C3 K1 3.418(5) 7_656 ? C5 O9 1.250(5) 6 ? C5 C6 1.531(9) . ? C6 O10 1.247(5) 6 ? C7 O11 1.256(5) 6_565 ? C7 C8 1.530(10) . ? C8 O12 1.247(5) 6_565 ? C9 O14 1.249(6) . ? C9 C9 1.549(9) 7_655 ? O14 U1 2.474(4) 7_655 ? Mg1 O32 2.736(8) . ? Mg1 K2 3.767(3) 7_656 ? 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 O6 U1 O2 69.63(18) . . ? O6 U1 O5' 65.58(14) . . ? O2 U1 O5' 88.76(14) . . ? O6 U1 O1 86.39(15) . . ? O2 U1 O1 65.19(14) . . ? O5' U1 O1 147.50(14) . . ? O6 U1 O14 132.02(15) . 7_655 ? O2 U1 O14 135.01(14) . 7_655 ? O5' U1 O14 134.51(14) . 7_655 ? O1 U1 O14 76.43(13) . 7_655 ? O6 U1 O13 137.37(14) . . ? O2 U1 O13 130.51(15) . . ? O5' U1 O13 76.73(13) . . ? O1 U1 O13 134.79(14) . . ? O14 U1 O13 65.43(12) 7_655 . ? O6 U1 O12 80.12(15) . . ? O2 U1 O12 147.31(15) . . ? O5' U1 O12 67.04(14) . . ? O1 U1 O12 126.25(13) . . ? O14 U1 O12 75.25(14) 7_655 . ? O13 U1 O12 66.94(14) . . ? O6 U1 O9 144.94(16) . . ? O2 U1 O9 77.52(15) . . ? O5' U1 O9 126.71(13) . . ? O1 U1 O9 68.57(15) . . ? O14 U1 O9 66.91(14) 7_655 . ? O13 U1 O9 74.57(14) . . ? O12 U1 O9 134.39(14) . . ? O6 U1 O10 110.92(15) . . ? O2 U1 O10 65.06(14) . . ? O5' U1 O10 64.25(13) . . ? O1 U1 O10 115.79(13) . . ? O14 U1 O10 116.93(13) 7_655 . ? O13 U1 O10 66.03(13) . . ? O12 U1 O10 117.66(12) . . ? O9 U1 O10 63.26(12) . . ? O6 U1 O11 66.03(15) . . ? O2 U1 O11 112.46(14) . . ? O5' U1 O11 114.28(13) . . ? O1 U1 O11 63.76(13) . . ? O14 U1 O11 66.17(14) 7_655 . ? O13 U1 O11 116.68(13) . . ? O12 U1 O11 63.20(12) . . ? O9 U1 O11 118.60(13) . . ? O10 U1 O11 176.84(12) . . ? O8 K1 O8 72.9(3) 7_656 4_646 ? O8 K1 O2 166.05(15) 7_656 6 ? O8 K1 O2 101.69(16) 4_646 6 ? O8 K1 O2 101.69(16) 7_656 . ? O8 K1 O2 166.05(15) 4_646 . ? O2 K1 O2 80.5(2) 6 . ? O8 K1 O7 60.64(13) 7_656 7_656 ? O8 K1 O7 102.09(15) 4_646 7_656 ? O2 K1 O7 133.27(14) 6 7_656 ? O2 K1 O7 85.69(14) . 7_656 ? O8 K1 O7 102.09(15) 7_656 4_646 ? O8 K1 O7 60.64(13) 4_646 4_646 ? O2 K1 O7 85.69(14) 6 4_646 ? O2 K1 O7 133.27(14) . 4_646 ? O7 K1 O7 72.1(2) 7_656 4_646 ? O8 K1 O10 113.28(13) 7_656 6 ? O8 K1 O10 88.42(13) 4_646 6 ? O2 K1 O10 53.09(11) 6 6 ? O2 K1 O10 81.90(12) . 6 ? O7 K1 O10 164.70(13) 7_656 6 ? O7 K1 O10 123.07(13) 4_646 6 ? O8 K1 O10 88.42(13) 7_656 . ? O8 K1 O10 113.28(13) 4_646 . ? O2 K1 O10 81.90(12) 6 . ? O2 K1 O10 53.09(11) . . ? O7 K1 O10 123.07(13) 7_656 . ? O7 K1 O10 164.70(13) 4_646 . ? O10 K1 O10 41.68(14) 6 . ? O8 K1 C6 108.43(14) 7_656 . ? O8 K1 C6 108.43(14) 4_646 . ? O2 K1 C6 60.41(13) 6 . ? O2 K1 C6 60.41(13) . . ? O7 K1 C6 142.59(11) 7_656 . ? O7 K1 C6 142.59(11) 4_646 . ? O10 K1 C6 22.62(8) 6 . ? O10 K1 C6 22.62(8) . . ? O8 K1 C3 19.20(13) 7_656 7_656 ? O8 K1 C3 73.34(16) 4_646 7_656 ? O2 K1 C3 171.77(15) 6 7_656 ? O2 K1 C3 105.95(14) . 7_656 ? O7 K1 C3 44.04(12) 7_656 7_656 ? O7 K1 C3 86.14(14) 4_646 7_656 ? O10 K1 C3 132.04(13) 6 7_656 ? O10 K1 C3 106.02(12) . 7_656 ? C6 K1 C3 127.09(13) . 7_656 ? O8 K1 C3 73.34(16) 7_656 4_646 ? O8 K1 C3 19.20(13) 4_646 4_646 ? O2 K1 C3 105.95(14) 6 4_646 ? O2 K1 C3 171.77(15) . 4_646 ? O7 K1 C3 86.14(14) 7_656 4_646 ? O7 K1 C3 44.04(12) 4_646 4_646 ? O10 K1 C3 106.02(12) 6 4_646 ? O10 K1 C3 132.04(13) . 4_646 ? C6 K1 C3 127.09(13) . 4_646 ? C3 K1 C3 67.2(2) 7_656 4_646 ? O8 K1 C2 173.41(15) 7_656 6 ? O8 K1 C2 111.81(16) 4_646 6 ? O2 K1 C2 20.08(12) 6 6 ? O2 K1 C2 74.73(15) . 6 ? O7 K1 C2 113.22(14) 7_656 6 ? O7 K1 C2 77.18(15) 4_646 6 ? O10 K1 C2 72.01(12) 6 6 ? O10 K1 C2 93.63(13) . 6 ? C6 K1 C2 74.85(14) . 6 ? C3 K1 C2 155.95(14) 7_656 6 ? C3 K1 C2 109.53(15) 4_646 6 ? O7 K2 O7 75.2(2) 4_646 7_656 ? O7 K2 O3 74.50(17) 4_646 6 ? O7 K2 O3 112.55(19) 7_656 6 ? O7 K2 O3 112.55(19) 4_646 . ? O7 K2 O3 74.50(17) 7_656 . ? O3 K2 O3 64.4(4) 6 . ? O7 K2 O4 131.71(16) 4_646 2_756 ? O7 K2 O4 77.77(15) 7_656 2_756 ? O3 K2 O4 153.67(19) 6 2_756 ? O3 K2 O4 97.5(2) . 2_756 ? O7 K2 O4 77.77(15) 4_646 5_756 ? O7 K2 O4 131.71(16) 7_656 5_756 ? O3 K2 O4 97.5(2) 6 5_756 ? O3 K2 O4 153.67(19) . 5_756 ? O4 K2 O4 91.9(3) 2_756 5_756 ? O7 K2 O3 170.96(18) 4_646 2_756 ? O7 K2 O3 111.1(2) 7_656 2_756 ? O3 K2 O3 96.83(17) 6 2_756 ? O3 K2 O3 64.6(3) . 2_756 ? O4 K2 O3 57.09(15) 2_756 2_756 ? O4 K2 O3 101.2(2) 5_756 2_756 ? O7 K2 O3 111.1(2) 4_646 5_756 ? O7 K2 O3 170.96(18) 7_656 5_756 ? O3 K2 O3 64.6(3) 6 5_756 ? O3 K2 O3 96.83(17) . 5_756 ? O4 K2 O3 101.2(2) 2_756 5_756 ? O4 K2 O3 57.09(15) 5_756 5_756 ? O3 K2 O3 61.8(3) 2_756 5_756 ? O7 K2 K1 50.97(10) 4_646 . ? O7 K2 K1 50.97(10) 7_656 . ? O3 K2 K1 63.07(14) 6 . ? O3 K2 K1 63.07(14) . . ? O4 K2 K1 127.74(12) 2_756 . ? O4 K2 K1 127.74(12) 5_756 . ? O3 K2 K1 127.60(16) 2_756 . ? O3 K2 K1 127.60(16) 5_756 . ? O7 K2 Mg1 47.72(11) 4_646 4_646 ? O7 K2 Mg1 122.57(12) 7_656 4_646 ? O3 K2 Mg1 53.06(19) 6 4_646 ? O3 K2 Mg1 117.2(2) . 4_646 ? O4 K2 Mg1 142.76(15) 2_756 4_646 ? O4 K2 Mg1 50.99(14) 5_756 4_646 ? O3 K2 Mg1 124.87(17) 2_756 4_646 ? O3 K2 Mg1 63.41(18) 5_756 4_646 ? K1 K2 Mg1 82.88(5) . 4_646 ? O7 K2 Mg1 122.57(12) 4_646 7_656 ? O7 K2 Mg1 47.72(11) 7_656 7_656 ? O3 K2 Mg1 117.2(2) 6 7_656 ? O3 K2 Mg1 53.06(19) . 7_656 ? O4 K2 Mg1 50.99(14) 2_756 7_656 ? O4 K2 Mg1 142.76(15) 5_756 7_656 ? O3 K2 Mg1 63.41(18) 2_756 7_656 ? O3 K2 Mg1 124.87(18) 5_756 7_656 ? K1 K2 Mg1 82.88(5) . 7_656 ? Mg1 K2 Mg1 165.52(10) 4_646 7_656 ? O7 K2 K2 124.06(12) 4_646 5_756 ? O7 K2 K2 124.06(12) 7_656 5_756 ? O3 K2 K2 49.61(14) 6 5_756 ? O3 K2 K2 49.61(14) . 5_756 ? O4 K2 K2 104.23(11) 2_756 5_756 ? O4 K2 K2 104.23(11) 5_756 5_756 ? O3 K2 K2 47.23(12) 2_756 5_756 ? O3 K2 K2 47.23(12) 5_756 5_756 ? K1 K2 K2 97.65(7) . 5_756 ? Mg1 K2 K2 89.67(6) 4_646 5_756 ? Mg1 K2 K2 89.67(6) 7_656 5_756 ? C1 O1 U1 121.2(3) . . ? C2 O2 U1 120.8(4) . . ? C2 O2 K1 112.0(3) . . ? U1 O2 K1 127.19(17) . . ? C2 O3 K2 148.6(6) . . ? C2 O3 K2 110.8(5) . 5_756 ? K2 O3 K2 83.17(17) . 5_756 ? C1 O4 K2 116.3(4) . 5_756 ? C4 O5' U1 121.7(3) . . ? C3 O6 U1 122.1(4) . . ? C4 O7 K2 149.5(4) . 7_656 ? C4 O7 K1 112.6(4) . 7_656 ? K2 O7 K1 80.51(12) 7_656 7_656 ? C3 O8 K1 114.6(4) . 7_656 ? C5 O9 U1 120.6(3) . . ? C6 O10 U1 119.7(3) . . ? C6 O10 K1 82.4(4) . . ? U1 O10 K1 108.21(14) . . ? C7 O11 U1 119.5(4) . . ? C8 O12 U1 121.4(4) . . ? C9 O13 U1 120.3(3) . . ? O4 C1 O1 126.2(6) . . ? O4 C1 C2 119.3(5) . . ? O1 C1 C2 114.5(4) . . ? O3 C2 O2 125.9(6) . . ? O3 C2 C1 120.2(6) . . ? O2 C2 C1 113.9(4) . . ? O3 C2 K1 81.3(4) . . ? O2 C2 K1 47.9(3) . . ? C1 C2 K1 153.1(4) . . ? O8 C3 O6 126.3(5) . . ? O8 C3 C4 121.0(5) . . ? O6 C3 C4 112.7(4) . . ? O8 C3 K1 46.2(3) . 7_656 ? O6 C3 K1 149.6(4) . 7_656 ? C4 C3 K1 82.7(3) . 7_656 ? O7 C4 O5' 126.3(5) . . ? O7 C4 C3 120.5(5) . . ? O5' C4 C3 113.2(4) . . ? O9 C5 O9 126.7(6) 6 . ? O9 C5 C6 116.6(3) 6 . ? O9 C5 C6 116.6(3) . . ? O10 C6 O10 126.6(6) 6 . ? O10 C6 C5 116.7(3) 6 . ? O10 C6 C5 116.7(3) . . ? O10 C6 K1 75.0(4) 6 . ? O10 C6 K1 75.0(4) . . ? C5 C6 K1 123.2(4) . . ? O11 C7 O11 126.7(6) 6_565 . ? O11 C7 C8 116.6(3) 6_565 . ? O11 C7 C8 116.6(3) . . ? O12 C8 O12 126.6(7) . 6_565 ? O12 C8 C7 116.7(3) . . ? O12 C8 C7 116.7(3) 6_565 . ? O14 C9 O13 126.4(5) . . ? O14 C9 C9 116.9(5) . 7_655 ? O13 C9 C9 116.7(5) . 7_655 ? C9 O14 U1 120.5(3) . 7_655 ? O32 Mg1 K2 112.5(2) . 7_656 ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 36.32 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 3.178 _refine_diff_density_min -3.210 _refine_diff_density_rms 0.325