# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Dario Braga' _publ_contact_author_address ; Department of Chemistry Universita degli Studi de Bologna G. Ciamician, Via F. Selmi 2 Bologna I-40126 ITALY ; _publ_contact_author_email DARIO.BRAGA@UNIBO.IT _publ_section_title ; Reversible Solid-State Reaction between 18-Crown[6] and M[H2PO4] (M = K, Rb, Cs) and an Investigation of the Decomplexation Process ; loop_ _publ_author_name 'Dario Braga' 'Elena Dichiarante' 'F. Grepioni' 'Marco Polito' 'Katia Rubini' # Attachment 'Cs-rev.CIF' data_18-Crown[6].Cs[H2PO4].1.5H2O _database_code_depnum_ccdc_archive 'CCDC 633143' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H56 Cs2 O23 P2' _chemical_formula_weight 1040.45 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' Cs Cs -0.3680 2.1192 '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' P P 0.1023 0.0942 '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 25.042(5) _cell_length_b 8.248(3) _cell_length_c 20.208(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.66(2) _cell_angle_gamma 90.00 _cell_volume 4114.7(18) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.680 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2096 _exptl_absorpt_coefficient_mu 1.929 _exptl_absorpt_correction_type Psi-scan _exptl_absorpt_correction_T_min 0.574 _exptl_absorpt_correction_T_max 0.734 _exptl_absorpt_process_details ? _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 3707 _diffrn_reflns_av_R_equivalents 0.0137 _diffrn_reflns_av_sigmaI/netI 0.0169 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.22 _diffrn_reflns_theta_max 24.98 _reflns_number_total 3592 _reflns_number_gt 2996 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0621P)^2^+11.4517P] 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 0.00096(12) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3592 _refine_ls_number_parameters 341 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0462 _refine_ls_R_factor_gt 0.0354 _refine_ls_wR_factor_ref 0.1032 _refine_ls_wR_factor_gt 0.0964 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cs1 Cs 0.894832(11) 0.27959(4) 0.812112(14) 0.05475(15) Uani 1 1 d . A . C2A C 0.9225(5) -0.1466(17) 0.7960(8) 0.078(4) Uani 0.50 1 d P A 1 H2A1 H 0.9359 -0.2465 0.7796 0.094 Uiso 0.50 1 calc PR A 1 H2A2 H 0.9535 -0.0832 0.8167 0.094 Uiso 0.50 1 calc PR A 1 C4A C 0.8872(5) 0.071(3) 0.6336(8) 0.084(5) Uani 0.50 1 d P A 1 H4A1 H 0.8546 0.0206 0.6095 0.101 Uiso 0.50 1 calc PR A 1 H4A2 H 0.9113 0.0911 0.6017 0.101 Uiso 0.50 1 calc PR A 1 C6A C 0.8275(6) 0.477(2) 0.6446(7) 0.077(4) Uani 0.50 1 d P A 1 H6A1 H 0.8049 0.5355 0.6087 0.092 Uiso 0.50 1 calc PR A 1 H6A2 H 0.8572 0.5482 0.6632 0.092 Uiso 0.50 1 calc PR A 1 C8A C 0.7522(4) 0.5436(12) 0.7817(7) 0.062(3) Uani 0.50 1 d P A 1 H8A1 H 0.7226 0.4673 0.7708 0.074 Uiso 0.50 1 calc PR A 1 H8A2 H 0.7380 0.6433 0.7973 0.074 Uiso 0.50 1 calc PR A 1 C10A C 0.8097(4) 0.3668(15) 0.9431(6) 0.058(2) Uani 0.50 1 d P A 1 H10A H 0.7954 0.3641 0.9849 0.070 Uiso 0.50 1 calc PR A 1 H10B H 0.8461 0.4106 0.9524 0.070 Uiso 0.50 1 calc PR A 1 C12A C 0.8461(5) -0.055(2) 0.9286(6) 0.064(3) Uani 0.50 1 d P A 1 H12A H 0.8123 -0.1101 0.9115 0.077 Uiso 0.50 1 calc PR A 1 H12B H 0.8665 -0.1255 0.9622 0.077 Uiso 0.50 1 calc PR A 1 O5A O 0.8767(4) -0.0385(11) 0.8731(5) 0.063(2) Uani 0.50 1 d P A 1 O6A O 0.8918(4) -0.0536(11) 0.7380(4) 0.0612(19) Uani 0.50 1 d P A 1 O7A O 0.8723(3) 0.2293(13) 0.6610(5) 0.0657(19) Uani 0.50 1 d P A 1 O8A O 0.7964(3) 0.4413(13) 0.6957(4) 0.0582(18) Uani 0.50 1 d P A 1 O9A O 0.7930(4) 0.4772(12) 0.8333(6) 0.058(2) Uani 0.50 1 d P A 1 O10A O 0.8111(3) 0.2021(10) 0.9163(5) 0.0534(18) Uani 0.50 1 d P A 1 C2B C 0.9172(6) -0.125(2) 0.7381(16) 0.125(10) Uani 0.50 1 d P A 2 H2B1 H 0.9193 -0.2381 0.7256 0.151 Uiso 0.50 1 calc PR A 2 H2B2 H 0.9515 -0.0969 0.7656 0.151 Uiso 0.50 1 calc PR A 2 C4B C 0.8663(7) 0.189(3) 0.6169(10) 0.096(5) Uani 0.50 1 d P A 2 H4B1 H 0.8368 0.1243 0.5934 0.116 Uiso 0.50 1 calc PR A 2 H4B2 H 0.8949 0.1882 0.5899 0.116 Uiso 0.50 1 calc PR A 2 C6B C 0.8101(7) 0.549(2) 0.6836(10) 0.090(4) Uani 0.50 1 d P A 2 H6B1 H 0.8447 0.5967 0.7026 0.108 Uiso 0.50 1 calc PR A 2 H6B2 H 0.7969 0.6053 0.6418 0.108 Uiso 0.50 1 calc PR A 2 C8B C 0.7665(9) 0.516(2) 0.8403(9) 0.080(4) Uani 0.50 1 d P A 2 H8B1 H 0.7609 0.6318 0.8453 0.096 Uiso 0.50 1 calc PR A 2 H8B2 H 0.7313 0.4711 0.8224 0.096 Uiso 0.50 1 calc PR A 2 C10B C 0.8192(6) 0.224(3) 0.9589(10) 0.102(7) Uani 0.50 1 d P A 2 H10C H 0.7959 0.2334 0.9926 0.123 Uiso 0.50 1 calc PR A 2 H10D H 0.8511 0.2893 0.9743 0.123 Uiso 0.50 1 calc PR A 2 C12B C 0.8545(7) -0.152(2) 0.8868(10) 0.107(6) Uani 0.50 1 d P A 2 H12C H 0.8183 -0.1851 0.8664 0.129 Uiso 0.50 1 calc PR A 2 H12D H 0.8648 -0.2120 0.9283 0.129 Uiso 0.50 1 calc PR A 2 O5B O 0.8558(5) 0.0035(14) 0.8988(7) 0.086(3) Uani 0.50 1 d P A 2 O6B O 0.8796(3) -0.1102(11) 0.7740(7) 0.081(3) Uani 0.50 1 d P A 2 O7B O 0.8850(4) 0.1151(17) 0.6744(5) 0.085(3) Uani 0.50 1 d P A 2 O8B O 0.8178(5) 0.3894(12) 0.6699(6) 0.073(2) Uani 0.50 1 d P A 2 O9B O 0.7951(4) 0.5024(12) 0.7930(6) 0.076(3) Uani 0.50 1 d P A 2 O10B O 0.7940(4) 0.2890(16) 0.9042(5) 0.081(2) Uani 0.50 1 d P A 2 C1 C 0.8910(3) -0.1827(7) 0.8435(5) 0.092(2) Uani 1 1 d . . . H1A H 0.9109 -0.2528 0.8775 0.111 Uiso 1 1 calc R A 1 H1B H 0.8586 -0.2393 0.8226 0.111 Uiso 1 1 calc R A 1 C3 C 0.9109(5) -0.0310(14) 0.6796(6) 0.164(5) Uani 1 1 d . . . H3A H 0.9484 0.0027 0.6914 0.197 Uiso 1 1 calc R A 1 H3B H 0.9111 -0.1363 0.6583 0.197 Uiso 1 1 calc R A 1 C5 C 0.8482(4) 0.3445(15) 0.6183(4) 0.126(3) Uani 1 1 d . . . H5A H 0.8190 0.2931 0.5879 0.151 Uiso 1 1 calc R A 1 H5B H 0.8745 0.3814 0.5915 0.151 Uiso 1 1 calc R A 1 C7 C 0.7750(3) 0.5736(7) 0.7260(4) 0.087(2) Uani 1 1 d . . . H7A H 0.8038 0.6521 0.7381 0.105 Uiso 1 1 calc R A 1 H7B H 0.7477 0.6242 0.6926 0.105 Uiso 1 1 calc R A 1 C9 C 0.7785(4) 0.4616(9) 0.8988(5) 0.110(3) Uani 1 1 d . . . H9A H 0.7782 0.5692 0.9182 0.132 Uiso 1 1 calc R A 1 H9B H 0.7417 0.4205 0.8934 0.132 Uiso 1 1 calc R A 1 C11 C 0.8347(4) 0.0744(16) 0.9580(4) 0.139(4) Uani 1 1 d . . . H11A H 0.8677 0.1146 0.9850 0.166 Uiso 1 1 calc R A 1 H11B H 0.8101 0.0463 0.9886 0.166 Uiso 1 1 calc R A 1 P1 P 0.99636(4) 0.25363(11) 0.98111(5) 0.0397(2) Uani 1 1 d . . . O1 O 0.95082(12) 0.3716(3) 0.95526(16) 0.0563(8) Uani 1 1 d . A . O2 O 1.05009(12) 0.3470(4) 0.99072(17) 0.0581(8) Uani 1 1 d . A . O3 O 0.99802(14) 0.1284(3) 0.92432(15) 0.0563(8) Uani 1 1 d . A . H30 H 0.9934 0.0375 0.9309 0.090 Uiso 1 1 d . . . O4 O 0.98745(14) 0.1702(3) 1.04468(15) 0.0556(8) Uani 1 1 d . A . O11 O 1.0000 0.4256(10) 0.7500 0.120(3) Uani 1 2 d S . . O12 O 0.9692(3) 0.4176(6) 1.1303(2) 0.139(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 Cs1 0.0542(2) 0.0588(2) 0.0505(2) -0.00322(12) 0.00666(12) 0.00039(12) C2A 0.059(8) 0.070(8) 0.091(9) -0.026(7) -0.028(7) 0.020(6) C4A 0.050(6) 0.152(17) 0.052(7) -0.040(10) 0.010(5) 0.013(8) C6A 0.078(8) 0.080(10) 0.072(8) 0.025(9) 0.010(6) -0.026(8) C8A 0.041(6) 0.040(5) 0.099(10) -0.005(5) -0.006(5) 0.011(4) C10A 0.059(6) 0.057(7) 0.059(6) -0.018(6) 0.012(5) 0.002(5) C12A 0.063(6) 0.071(9) 0.055(7) 0.019(7) 0.002(5) -0.010(6) O5A 0.068(5) 0.050(5) 0.074(6) 0.003(4) 0.020(4) -0.005(4) O6A 0.051(4) 0.069(5) 0.063(5) -0.006(4) 0.007(4) 0.010(4) O7A 0.068(5) 0.086(7) 0.042(5) -0.007(5) 0.007(3) 0.005(4) O8A 0.068(5) 0.044(5) 0.063(5) 0.009(4) 0.015(4) -0.003(4) O9A 0.033(4) 0.065(5) 0.078(7) 0.000(5) 0.014(5) 0.015(3) O10A 0.059(4) 0.055(5) 0.041(5) -0.001(4) -0.006(3) 0.002(3) C2B 0.044(7) 0.072(10) 0.25(3) -0.068(15) -0.006(12) 0.012(7) C4B 0.077(10) 0.135(17) 0.086(13) -0.029(12) 0.041(9) -0.039(11) C6B 0.096(10) 0.068(10) 0.102(12) 0.020(9) 0.001(9) 0.009(9) C8B 0.085(11) 0.073(9) 0.085(12) -0.013(8) 0.020(10) -0.017(8) C10B 0.074(9) 0.16(2) 0.074(11) -0.022(13) 0.023(8) -0.050(12) C12B 0.101(11) 0.104(12) 0.103(13) 0.053(11) -0.026(10) -0.023(11) O5B 0.099(9) 0.072(8) 0.079(8) 0.025(6) -0.007(6) -0.027(6) O6B 0.059(5) 0.052(5) 0.124(9) -0.012(5) -0.010(6) 0.006(4) O7B 0.093(7) 0.088(7) 0.080(7) -0.025(6) 0.034(5) -0.018(6) O8B 0.080(6) 0.069(6) 0.069(6) 0.006(5) 0.006(4) -0.012(5) O9B 0.076(7) 0.061(5) 0.090(7) -0.008(5) 0.007(6) 0.007(4) O10B 0.084(7) 0.086(7) 0.071(7) -0.010(6) 0.010(5) -0.015(6) C1 0.090(5) 0.051(3) 0.119(6) 0.007(4) -0.032(5) 0.001(3) C3 0.217(12) 0.149(9) 0.157(10) 0.003(8) 0.121(9) 0.097(9) C5 0.142(7) 0.165(10) 0.084(5) 0.045(6) 0.059(5) 0.010(7) C7 0.085(4) 0.061(4) 0.101(5) 0.005(3) -0.027(4) 0.014(3) C9 0.144(7) 0.071(4) 0.135(7) -0.040(5) 0.082(6) -0.004(5) C11 0.172(9) 0.191(11) 0.063(4) 0.060(6) 0.049(5) 0.081(8) P1 0.0489(6) 0.0249(5) 0.0448(6) -0.0026(4) 0.0067(4) -0.0004(4) O1 0.0587(18) 0.0370(16) 0.0661(19) -0.0070(14) -0.0100(14) 0.0058(13) O2 0.0506(16) 0.0413(16) 0.084(2) -0.0140(16) 0.0156(15) -0.0055(13) O3 0.091(2) 0.0292(14) 0.0510(17) -0.0069(12) 0.0174(16) -0.0051(14) O4 0.090(2) 0.0300(14) 0.0505(17) -0.0022(13) 0.0235(16) 0.0021(14) O11 0.141(6) 0.101(5) 0.107(5) 0.000 -0.013(5) 0.000 O12 0.300(8) 0.060(3) 0.073(3) 0.001(2) 0.082(4) 0.012(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 Cs1 O5A 2.966(10) . ? Cs1 O7B 3.069(12) . ? Cs1 O9B 3.073(11) . ? Cs1 O7A 3.039(9) . ? Cs1 O1 3.090(3) . ? Cs1 O6A 3.124(9) . ? Cs1 O9A 3.115(10) . ? Cs1 O5B 3.128(13) . ? Cs1 O10A 3.274(9) . ? Cs1 O8B 3.308(9) . ? Cs1 O6B 3.313(8) . ? Cs1 O11 3.327(3) . ? C2A C1 1.372(19) . ? C2A O6A 1.500(17) . ? C2A H2A1 0.9700 . ? C2A H2A2 0.9700 . ? C4A C3 1.32(2) . ? C4A O7A 1.49(2) . ? C4A H4A1 0.9700 . ? C4A H4A2 0.9700 . ? C6A C5 1.36(2) . ? C6A O8A 1.427(16) . ? C6A H6A1 0.9700 . ? C6A H6A2 0.9700 . ? C8A C7 1.366(15) . ? C8A O9A 1.440(15) . ? C8A H8A1 0.9700 . ? C8A H8A2 0.9700 . ? C10A C9 1.337(15) . ? C10A O10A 1.465(14) . ? C10A H10A 0.9700 . ? C10A H10B 0.9700 . ? C12A C11 1.278(19) . ? C12A O5A 1.468(16) . ? C12A H12A 0.9700 . ? C12A H12B 0.9700 . ? O5A C1 1.405(12) . ? O6A C3 1.358(14) . ? O7A C5 1.355(15) . ? O8A C7 1.400(13) . ? O9A C9 1.438(13) . ? O10A C11 1.415(13) . ? C2B O6B 1.29(2) . ? C2B C3 1.40(3) . ? C2B H2B1 0.9700 . ? C2B H2B2 0.9700 . ? C4B O7B 1.33(2) . ? C4B C5 1.36(3) . ? C4B H4B1 0.9700 . ? C4B H4B2 0.9700 . ? C6B C7 1.34(2) . ? C6B O8B 1.367(19) . ? C6B H6B1 0.9700 . ? C6B H6B2 0.9700 . ? C8B C9 1.255(19) . ? C8B O9B 1.292(19) . ? C8B H8B1 0.9700 . ? C8B H8B2 0.9700 . ? C10B O10B 1.30(2) . ? C10B C11 1.30(2) . ? C10B H10C 0.9700 . ? C10B H10D 0.9700 . ? C12B O5B 1.31(2) . ? C12B C1 1.39(2) . ? C12B H12C 0.9700 . ? C12B H12D 0.9700 . ? O5B C11 1.505(18) . ? O6B C1 1.508(16) . ? O7B C3 1.363(18) . ? O8B C5 1.440(16) . ? O9B C7 1.484(13) . ? O10B C9 1.475(16) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? P1 O4 1.507(3) . ? P1 O1 1.523(3) . ? P1 O2 1.534(3) . ? P1 O3 1.550(3) . ? O3 H30 0.7736 . ? O11 Cs1 3.327(3) 2_756 ? 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 O5A Cs1 O7B 89.5(3) . . ? O5A Cs1 O9B 113.8(3) . . ? O7B Cs1 O9B 102.2(3) . . ? O5A Cs1 O7A 106.3(3) . . ? O7B Cs1 O7A 19.2(2) . . ? O9B Cs1 O7A 86.8(3) . . ? O5A Cs1 O1 84.5(2) . . ? O7B Cs1 O1 155.8(3) . . ? O9B Cs1 O1 101.7(2) . . ? O7A Cs1 O1 162.32(18) . . ? O5A Cs1 O6A 55.1(3) . . ? O7B Cs1 O6A 35.4(3) . . ? O9B Cs1 O6A 120.8(2) . . ? O7A Cs1 O6A 54.1(3) . . ? O1 Cs1 O6A 129.45(16) . . ? O5A Cs1 O9A 102.7(3) . . ? O7B Cs1 O9A 114.4(3) . . ? O9B Cs1 O9A 15.8(2) . . ? O7A Cs1 O9A 101.0(3) . . ? O1 Cs1 O9A 89.8(2) . . ? O6A Cs1 O9A 124.8(2) . . ? O5A Cs1 O5B 16.1(2) . . ? O7B Cs1 O5B 101.6(3) . . ? O9B Cs1 O5B 100.5(4) . . ? O7A Cs1 O5B 116.1(3) . . ? O1 Cs1 O5B 77.9(2) . . ? O6A Cs1 O5B 69.1(3) . . ? O9A Cs1 O5B 87.9(3) . . ? O5A Cs1 O10A 53.2(2) . . ? O7B Cs1 O10A 122.3(2) . . ? O9B Cs1 O10A 66.6(3) . . ? O7A Cs1 O10A 126.0(2) . . ? O1 Cs1 O10A 71.63(17) . . ? O6A Cs1 O10A 99.8(2) . . ? O9A Cs1 O10A 52.2(3) . . ? O5B Cs1 O10A 37.2(3) . . ? O5A Cs1 O8B 119.7(3) . . ? O7B Cs1 O8B 52.2(3) . . ? O9B Cs1 O8B 51.9(3) . . ? O7A Cs1 O8B 35.1(3) . . ? O1 Cs1 O8B 148.5(2) . . ? O6A Cs1 O8B 82.0(2) . . ? O9A Cs1 O8B 66.7(3) . . ? O5B Cs1 O8B 119.6(3) . . ? O10A Cs1 O8B 105.6(3) . . ? O5A Cs1 O6B 38.6(3) . . ? O7B Cs1 O6B 51.1(3) . . ? O9B Cs1 O6B 119.5(2) . . ? O7A Cs1 O6B 68.9(3) . . ? O1 Cs1 O6B 118.2(2) . . ? O6A Cs1 O6B 16.8(2) . . ? O9A Cs1 O6B 118.4(2) . . ? O5B Cs1 O6B 52.4(4) . . ? O10A Cs1 O6B 84.2(3) . . ? O8B Cs1 O6B 92.1(3) . . ? O5A Cs1 O11 131.5(2) . . ? O7B Cs1 O11 76.45(18) . . ? O9B Cs1 O11 114.5(2) . . ? O7A Cs1 O11 72.30(17) . . ? O1 Cs1 O11 90.04(8) . . ? O6A Cs1 O11 95.4(2) . . ? O9A Cs1 O11 125.5(2) . . ? O5B Cs1 O11 144.7(3) . . ? O10A Cs1 O11 161.10(16) . . ? O8B Cs1 O11 87.5(2) . . ? O6B Cs1 O11 109.3(2) . . ? C1 C2A O6A 112.2(10) . . ? C1 C2A Cs1 90.4(7) . . ? O6A C2A Cs1 59.4(6) . . ? C1 C2A H2A1 109.2 . . ? O6A C2A H2A1 109.2 . . ? Cs1 C2A H2A1 160.3 . . ? C1 C2A H2A2 109.2 . . ? O6A C2A H2A2 109.2 . . ? Cs1 C2A H2A2 65.7 . . ? H2A1 C2A H2A2 107.9 . . ? C3 C4A O7A 114.1(13) . . ? C3 C4A H4A1 108.7 . . ? O7A C4A H4A1 108.7 . . ? C3 C4A H4A2 108.7 . . ? O7A C4A H4A2 108.7 . . ? H4A1 C4A H4A2 107.6 . . ? C5 C6A O8A 114.0(16) . . ? C5 C6A Cs1 82.2(8) . . ? O8A C6A Cs1 59.4(7) . . ? C5 C6A H6A1 108.7 . . ? O8A C6A H6A1 108.7 . . ? Cs1 C6A H6A1 167.1 . . ? C5 C6A H6A2 108.7 . . ? O8A C6A H6A2 108.7 . . ? Cs1 C6A H6A2 74.0 . . ? H6A1 C6A H6A2 107.6 . . ? C7 C8A O9A 108.8(10) . . ? C7 C8A H8A1 109.9 . . ? O9A C8A H8A1 109.9 . . ? C7 C8A H8A2 109.9 . . ? O9A C8A H8A2 109.9 . . ? H8A1 C8A H8A2 108.3 . . ? C9 C10A O10A 110.0(11) . . ? C9 C10A Cs1 88.7(6) . . ? O10A C10A Cs1 60.5(5) . . ? C9 C10A H10A 109.7 . . ? O10A C10A H10A 109.7 . . ? Cs1 C10A H10A 161.6 . . ? C9 C10A H10B 109.7 . . ? O10A C10A H10B 109.7 . . ? Cs1 C10A H10B 65.1 . . ? H10A C10A H10B 108.2 . . ? C11 C12A O5A 117.6(14) . . ? C11 C12A H12A 107.9 . . ? O5A C12A H12A 107.9 . . ? C11 C12A H12B 107.9 . . ? O5A C12A H12B 107.9 . . ? H12A C12A H12B 107.2 . . ? C1 O5A C12A 116.7(10) . . ? C1 O5A Cs1 120.3(7) . . ? C12A O5A Cs1 122.4(9) . . ? C3 O6A C2A 122.7(11) . . ? C3 O6A Cs1 108.2(7) . . ? C2A O6A Cs1 96.2(6) . . ? C5 O7A C4A 119.3(13) . . ? C5 O7A Cs1 122.2(8) . . ? C4A O7A Cs1 118.5(10) . . ? C7 O8A C6A 116.8(13) . . ? C7 O8A Cs1 106.9(5) . . ? C6A O8A Cs1 99.3(8) . . ? C8A O9A C9 116.3(11) . . ? C8A O9A Cs1 126.7(9) . . ? C9 O9A Cs1 114.8(6) . . ? C11 O10A C10A 120.2(12) . . ? C11 O10A Cs1 106.3(5) . . ? C10A O10A Cs1 96.6(6) . . ? O6B C2B C3 115.6(18) . . ? O6B C2B Cs1 61.1(8) . . ? C3 C2B Cs1 80.8(8) . . ? O6B C2B H2B1 108.4 . . ? C3 C2B H2B1 108.4 . . ? Cs1 C2B H2B1 168.9 . . ? O6B C2B H2B2 108.4 . . ? C3 C2B H2B2 108.4 . . ? Cs1 C2B H2B2 74.6 . . ? H2B1 C2B H2B2 107.4 . . ? O7B C4B C5 119(2) . . ? O7B C4B H4B1 107.5 . . ? C5 C4B H4B1 107.5 . . ? O7B C4B H4B2 107.5 . . ? C5 C4B H4B2 107.5 . . ? H4B1 C4B H4B2 107.0 . . ? C7 C6B O8B 114(2) . . ? C7 C6B Cs1 90.1(9) . . ? O8B C6B Cs1 59.4(8) . . ? C7 C6B H6B1 108.8 . . ? O8B C6B H6B1 108.8 . . ? Cs1 C6B H6B1 66.6 . . ? C7 C6B H6B2 108.8 . . ? O8B C6B H6B2 108.8 . . ? Cs1 C6B H6B2 161.0 . . ? H6B1 C6B H6B2 107.7 . . ? C9 C8B O9B 126(2) . . ? C9 C8B Cs1 83.4(11) . . ? O9B C8B Cs1 43.3(11) . . ? C9 C8B H8B1 105.8 . . ? O9B C8B H8B1 105.8 . . ? Cs1 C8B H8B1 130.2 . . ? C9 C8B H8B2 105.8 . . ? O9B C8B H8B2 105.8 . . ? Cs1 C8B H8B2 118.3 . . ? H8B1 C8B H8B2 106.2 . . ? O10B C10B C11 119(2) . . ? O10B C10B Cs1 61.3(9) . . ? C11 C10B Cs1 85.1(9) . . ? O10B C10B H10C 107.5 . . ? C11 C10B H10C 107.5 . . ? Cs1 C10B H10C 166.6 . . ? O10B C10B H10D 107.5 . . ? C11 C10B H10D 107.5 . . ? Cs1 C10B H10D 72.0 . . ? H10C C10B H10D 107.0 . . ? O5B C12B C1 107.3(15) . . ? O5B C12B H12C 110.3 . . ? C1 C12B H12C 110.3 . . ? O5B C12B H12D 110.3 . . ? C1 C12B H12D 110.3 . . ? H12C C12B H12D 108.5 . . ? C12B O5B C11 121.9(18) . . ? C12B O5B Cs1 127.7(16) . . ? C11 O5B Cs1 110.3(7) . . ? C2B O6B C1 116.4(15) . . ? C2B O6B Cs1 99.1(10) . . ? C1 O6B Cs1 99.9(5) . . ? C4B O7B C3 124.7(18) . . ? C4B O7B Cs1 123.5(16) . . ? C3 O7B Cs1 110.8(8) . . ? C6B O8B C5 120.3(18) . . ? C6B O8B Cs1 99.8(9) . . ? C5 O8B Cs1 104.9(6) . . ? C8B O9B C7 119.7(13) . . ? C8B O9B Cs1 120.0(13) . . ? C7 O9B Cs1 119.7(6) . . ? C10B O10B C9 123.1(15) . . ? C10B O10B Cs1 99.1(10) . . ? C9 O10B Cs1 101.2(5) . . ? C2A C1 O5A 109.4(8) . . ? C2A C1 C12B 156.3(10) . . ? O5A C1 C12B 48.5(8) . . ? C2A C1 O6B 45.9(7) . . ? O5A C1 O6B 92.3(6) . . ? C12B C1 O6B 118.3(8) . . ? C2A C1 Cs1 68.8(6) . . ? O5A C1 Cs1 41.5(5) . . ? C12B C1 Cs1 87.8(7) . . ? O6B C1 Cs1 57.5(4) . . ? C2A C1 H1A 109.8 . . ? O5A C1 H1A 109.8 . . ? C12B C1 H1A 88.5 . . ? O6B C1 H1A 153.0 . . ? Cs1 C1 H1A 132.9 . . ? C2A C1 H1B 109.8 . . ? O5A C1 H1B 109.8 . . ? C12B C1 H1B 76.7 . . ? O6B C1 H1B 76.9 . . ? Cs1 C1 H1B 116.5 . . ? H1A C1 H1B 108.3 . . ? C4A C3 O6A 121.2(10) . . ? C4A C3 O7B 39.6(7) . . ? O6A C3 O7B 87.6(8) . . ? C4A C3 C2B 157.3(12) . . ? O6A C3 C2B 36.6(7) . . ? O7B C3 C2B 122.8(11) . . ? C4A C3 Cs1 88.8(8) . . ? O6A C3 Cs1 51.8(5) . . ? O7B C3 Cs1 49.5(6) . . ? C2B C3 Cs1 77.8(8) . . ? C4A C3 H3A 107.0 . . ? O6A C3 H3A 107.0 . . ? O7B C3 H3A 101.1 . . ? C2B C3 H3A 89.0 . . ? Cs1 C3 H3A 81.1 . . ? C4A C3 H3B 107.0 . . ? O6A C3 H3B 107.0 . . ? O7B C3 H3B 142.6 . . ? C2B C3 H3B 82.6 . . ? Cs1 C3 H3B 158.8 . . ? H3A C3 H3B 106.8 . . ? O7A C5 C6A 118.3(10) . . ? O7A C5 C4B 40.5(8) . . ? C6A C5 C4B 156.6(12) . . ? O7A C5 O8B 87.2(7) . . ? C6A C5 O8B 39.3(6) . . ? C4B C5 O8B 118.4(10) . . ? O7A C5 Cs1 40.9(6) . . ? C6A C5 Cs1 77.8(7) . . ? C4B C5 Cs1 81.3(10) . . ? O8B C5 Cs1 54.4(5) . . ? O7A C5 H5A 107.7 . . ? C6A C5 H5A 107.7 . . ? C4B C5 H5A 78.1 . . ? O8B C5 H5A 97.9 . . ? Cs1 C5 H5A 129.6 . . ? O7A C5 H5B 107.7 . . ? C6A C5 H5B 107.7 . . ? C4B C5 H5B 91.4 . . ? O8B C5 H5B 144.7 . . ? Cs1 C5 H5B 118.9 . . ? H5A C5 H5B 107.1 . . ? C6B C7 C8A 155.2(10) . . ? C6B C7 O8A 42.7(8) . . ? C8A C7 O8A 117.4(7) . . ? C6B C7 O9B 111.5(9) . . ? C8A C7 O9B 45.7(6) . . ? O8A C7 O9B 89.7(6) . . ? C6B C7 H7A 73.9 . . ? C8A C7 H7A 107.9 . . ? O8A C7 H7A 107.9 . . ? O9B C7 H7A 84.8 . . ? C6B C7 H7B 94.6 . . ? C8A C7 H7B 107.9 . . ? O8A C7 H7B 107.9 . . ? O9B C7 H7B 153.6 . . ? H7A C7 H7B 107.2 . . ? C8B C9 C10A 149.5(12) . . ? C8B C9 O9A 32.5(9) . . ? C10A C9 O9A 117.3(8) . . ? C8B C9 O10B 115.7(10) . . ? C10A C9 O10B 43.1(6) . . ? O9A C9 O10B 92.8(6) . . ? C8B C9 H9A 91.9 . . ? C10A C9 H9A 108.0 . . ? O9A C9 H9A 108.0 . . ? O10B C9 H9A 150.8 . . ? C8B C9 H9B 86.9 . . ? C10A C9 H9B 108.0 . . ? O9A C9 H9B 108.0 . . ? O10B C9 H9B 84.5 . . ? H9A C9 H9B 107.2 . . ? C12A C11 C10B 153.4(13) . . ? C12A C11 O10A 116.6(9) . . ? C10B C11 O10A 37.1(9) . . ? C12A C11 O5B 33.9(6) . . ? C10B C11 O5B 121.8(11) . . ? O10A C11 O5B 89.0(7) . . ? C12A C11 Cs1 82.3(7) . . ? C10B C11 Cs1 75.6(8) . . ? O10A C11 Cs1 53.4(4) . . ? O5B C11 Cs1 48.5(6) . . ? C12A C11 H11A 108.1 . . ? C10B C11 H11A 83.9 . . ? O10A C11 H11A 108.1 . . ? O5B C11 H11A 101.5 . . ? Cs1 C11 H11A 82.8 . . ? C12A C11 H11B 108.1 . . ? C10B C11 H11B 89.8 . . ? O10A C11 H11B 108.1 . . ? O5B C11 H11B 139.3 . . ? Cs1 C11 H11B 161.5 . . ? H11A C11 H11B 107.3 . . ? O4 P1 O1 112.00(19) . . ? O4 P1 O2 111.9(2) . . ? O1 P1 O2 108.24(18) . . ? O4 P1 O3 110.68(16) . . ? O1 P1 O3 106.46(18) . . ? O2 P1 O3 107.25(18) . . ? O4 P1 Cs1 127.06(14) . . ? O1 P1 Cs1 47.56(12) . . ? O2 P1 Cs1 120.77(14) . . ? O3 P1 Cs1 58.90(13) . . ? P1 O1 Cs1 111.11(15) . . ? P1 O3 Cs1 97.97(14) . . ? P1 O3 H30 119.7 . . ? Cs1 O3 H30 110.7 . . ? Cs1 O11 Cs1 137.6(3) . 2_756 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.926 _refine_diff_density_min -0.900 _refine_diff_density_rms 0.081 # Attachment 'K-rev.CIF' data_18-Crown[6].K[H2PO4].2H2O _database_code_depnum_ccdc_archive 'CCDC 633144' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H30 K O12 P' _chemical_formula_weight 436.43 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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 20.281(4) _cell_length_b 8.350(3) _cell_length_c 24.411(6) _cell_angle_alpha 90.00 _cell_angle_beta 92.69(2) _cell_angle_gamma 90.00 _cell_volume 4129(2) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.404 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1856 _exptl_absorpt_coefficient_mu 0.389 _exptl_absorpt_correction_type Psi-scan _exptl_absorpt_correction_T_min 0.909 _exptl_absorpt_correction_T_max 0.940 _exptl_absorpt_process_details ? _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 3676 _diffrn_reflns_av_R_equivalents 0.0202 _diffrn_reflns_av_sigmaI/netI 0.0153 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.34 _diffrn_reflns_theta_max 24.96 _reflns_number_total 3582 _reflns_number_gt 2925 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0787P)^2^+6.0505P] 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 0.0010(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3582 _refine_ls_number_parameters 242 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0617 _refine_ls_R_factor_gt 0.0487 _refine_ls_wR_factor_ref 0.1426 _refine_ls_wR_factor_gt 0.1327 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _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 0.24014(3) 0.78762(8) 0.36841(3) 0.0528(2) Uani 1 1 d . . . C1 C 0.15865(16) 0.4666(4) 0.29725(13) 0.0589(8) Uani 1 1 d . . . H1A H 0.1251 0.4009 0.2786 0.071 Uiso 1 1 calc R . . H1B H 0.1651 0.4279 0.3346 0.071 Uiso 1 1 calc R . . C2 C 0.22130(16) 0.4547(4) 0.26864(13) 0.0592(8) Uani 1 1 d . . . H2A H 0.2323 0.3430 0.2631 0.071 Uiso 1 1 calc R . . H2B H 0.2164 0.5059 0.2330 0.071 Uiso 1 1 calc R . . C3 C 0.33442(16) 0.5190(4) 0.27688(13) 0.0598(8) Uani 1 1 d . . . H3A H 0.3328 0.5736 0.2418 0.072 Uiso 1 1 calc R . . H3B H 0.3451 0.4074 0.2708 0.072 Uiso 1 1 calc R . . C4 C 0.38607(15) 0.5937(4) 0.31453(14) 0.0623(8) Uani 1 1 d . . . H4A H 0.3857 0.5439 0.3504 0.075 Uiso 1 1 calc R . . H4B H 0.4294 0.5780 0.3001 0.075 Uiso 1 1 calc R . . C5 C 0.41949(15) 0.8386(4) 0.35456(14) 0.0622(8) Uani 1 1 d . . . H5A H 0.4632 0.8280 0.3405 0.075 Uiso 1 1 calc R . . H5B H 0.4200 0.7899 0.3907 0.075 Uiso 1 1 calc R . . C6 C 0.40181(15) 1.0110(4) 0.35857(14) 0.0629(8) Uani 1 1 d . . . H6A H 0.4350 1.0668 0.3813 0.076 Uiso 1 1 calc R . . H6B H 0.4002 1.0592 0.3224 0.076 Uiso 1 1 calc R . . C7 C 0.32061(18) 1.1862(4) 0.38957(17) 0.0725(10) Uani 1 1 d . . . H7A H 0.3146 1.2391 0.3543 0.087 Uiso 1 1 calc R . . H7B H 0.3550 1.2421 0.4109 0.087 Uiso 1 1 calc R . . C8 C 0.25806(19) 1.1906(5) 0.41873(16) 0.0743(10) Uani 1 1 d . . . H8A H 0.2635 1.1325 0.4530 0.089 Uiso 1 1 calc R . . H8B H 0.2468 1.3006 0.4270 0.089 Uiso 1 1 calc R . . C9 C 0.14526(17) 1.1188(4) 0.41138(15) 0.0679(9) Uani 1 1 d . . . H9A H 0.1342 1.2267 0.4225 0.081 Uiso 1 1 calc R . . H9B H 0.1488 1.0522 0.4439 0.081 Uiso 1 1 calc R . . C10 C 0.09287(16) 1.0560(4) 0.37308(15) 0.0643(8) Uani 1 1 d . . . H10A H 0.0507 1.0586 0.3902 0.077 Uiso 1 1 calc R . . H10B H 0.0896 1.1213 0.3402 0.077 Uiso 1 1 calc R . . C11 C 0.05909(15) 0.8179(4) 0.32778(14) 0.0611(8) Uani 1 1 d . . . H11A H 0.0549 0.8656 0.2916 0.073 Uiso 1 1 calc R . . H11B H 0.0172 0.8296 0.3450 0.073 Uiso 1 1 calc R . . C12 C 0.07601(15) 0.6455(4) 0.32322(13) 0.0616(8) Uani 1 1 d . . . H12A H 0.0790 0.5975 0.3594 0.074 Uiso 1 1 calc R . . H12B H 0.0416 0.5905 0.3016 0.074 Uiso 1 1 calc R . . O1 O 0.13776(10) 0.6282(2) 0.29765(8) 0.0543(5) Uani 1 1 d . . . O2 O 0.27268(10) 0.5309(2) 0.30080(8) 0.0542(5) Uani 1 1 d . . . O3 O 0.37269(10) 0.7592(2) 0.31897(8) 0.0546(5) Uani 1 1 d . . . O4 O 0.33920(10) 1.0250(3) 0.38193(9) 0.0611(5) Uani 1 1 d . . . O5 O 0.20636(10) 1.1200(3) 0.38534(9) 0.0592(5) Uani 1 1 d . . . O6 O 0.10917(10) 0.8958(3) 0.35938(9) 0.0587(5) Uani 1 1 d . . . O7 O 0.17833(16) 0.5948(6) 0.4479(2) 0.1402(15) Uani 1 1 d . . . H700 H 0.1314 0.5967 0.4511 0.090 Uiso 1 1 d . . . O8 O 0.31083(17) 0.6568(7) 0.45525(18) 0.1484(18) Uani 1 1 d . . . H800 H 0.3636 0.6444 0.4635 0.090 Uiso 1 1 d . . . P1 P 0.01495(4) 0.75317(8) 0.49019(3) 0.0491(2) Uani 1 1 d . . . O9 O -0.03359(13) 0.8450(3) 0.45024(11) 0.0729(7) Uani 1 1 d . . . H900 H -0.043(2) 0.939(6) 0.4598(17) 0.088 Uiso 1 1 d . . . O10 O -0.02595(14) 0.6812(3) 0.53663(11) 0.0793(8) Uani 1 1 d . . . O11 O 0.04544(11) 0.6210(2) 0.45851(9) 0.0633(6) Uani 1 1 d . . . H110 H -0.0334(18) 0.581(5) 0.5365(15) 0.076 Uiso 1 1 d . . . O12 O 0.06189(11) 0.8707(3) 0.51715(10) 0.0664(6) 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 K1 0.0495(4) 0.0570(4) 0.0517(4) -0.0039(3) 0.0006(3) 0.0011(3) C1 0.0705(19) 0.0534(17) 0.0525(17) -0.0058(13) -0.0018(15) -0.0125(14) C2 0.073(2) 0.0549(17) 0.0495(16) -0.0145(13) 0.0007(15) -0.0009(15) C3 0.0679(19) 0.0590(17) 0.0539(18) -0.0036(14) 0.0154(15) 0.0088(15) C4 0.0541(17) 0.0657(19) 0.068(2) 0.0066(15) 0.0084(15) 0.0135(14) C5 0.0440(15) 0.084(2) 0.0573(18) 0.0061(16) -0.0069(13) -0.0029(15) C6 0.0494(16) 0.082(2) 0.0573(18) -0.0002(16) -0.0033(14) -0.0165(15) C7 0.070(2) 0.0596(19) 0.086(2) -0.0089(18) -0.0114(19) -0.0160(16) C8 0.082(2) 0.066(2) 0.073(2) -0.0253(18) -0.0047(19) -0.0024(18) C9 0.073(2) 0.068(2) 0.065(2) -0.0108(16) 0.0226(17) 0.0044(17) C10 0.0553(17) 0.0620(18) 0.077(2) 0.0014(16) 0.0195(16) 0.0089(14) C11 0.0422(15) 0.082(2) 0.0594(18) 0.0030(16) 0.0053(13) 0.0021(14) C12 0.0493(16) 0.083(2) 0.0532(17) -0.0039(16) 0.0066(14) -0.0168(15) O1 0.0555(11) 0.0583(12) 0.0497(11) -0.0023(9) 0.0101(9) -0.0072(9) O2 0.0581(11) 0.0586(12) 0.0461(11) -0.0113(9) 0.0040(9) 0.0018(9) O3 0.0507(11) 0.0594(12) 0.0528(11) 0.0072(9) -0.0069(9) 0.0031(9) O4 0.0555(12) 0.0603(13) 0.0673(13) -0.0024(10) -0.0007(10) -0.0090(10) O5 0.0601(12) 0.0621(13) 0.0559(12) -0.0121(10) 0.0097(10) -0.0017(10) O6 0.0485(11) 0.0582(12) 0.0694(13) -0.0033(10) 0.0044(10) 0.0040(9) O7 0.0721(19) 0.155(3) 0.196(4) 0.040(3) 0.026(2) 0.007(2) O8 0.076(2) 0.233(5) 0.133(3) 0.061(3) -0.023(2) 0.000(3) P1 0.0579(5) 0.0429(4) 0.0466(4) -0.0031(3) 0.0030(3) -0.0031(3) O9 0.0809(16) 0.0598(13) 0.0747(15) -0.0175(12) -0.0317(13) 0.0013(12) O10 0.107(2) 0.0523(12) 0.0832(17) -0.0108(12) 0.0501(15) -0.0023(13) O11 0.0762(14) 0.0533(12) 0.0630(13) -0.0032(10) 0.0299(11) -0.0035(10) O12 0.0677(13) 0.0538(12) 0.0751(15) -0.0024(10) -0.0232(11) -0.0021(10) _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 K1 O8 2.731(4) . ? K1 O2 2.803(2) . ? K1 O6 2.804(2) . ? K1 O4 2.831(2) . ? K1 O7 2.856(4) . ? K1 O5 2.893(2) . ? K1 O1 2.955(2) . ? K1 O3 3.007(2) . ? C1 O1 1.415(4) . ? C1 C2 1.482(4) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 O2 1.425(4) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 O2 1.410(4) . ? C3 C4 1.497(5) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 O3 1.414(4) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 O3 1.420(4) . ? C5 C6 1.488(5) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 O4 1.421(4) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 O4 1.412(4) . ? C7 C8 1.484(5) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 O5 1.425(4) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 O5 1.419(4) . ? C9 C10 1.478(5) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 O6 1.422(4) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 O6 1.406(4) . ? C11 C12 1.486(5) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 O1 1.433(4) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? O7 H700 0.9588 . ? O8 H800 1.0847 . ? P1 O11 1.498(2) . ? P1 O12 1.498(2) . ? P1 O10 1.556(3) . ? P1 O9 1.555(3) . ? O9 H900 0.84(5) . ? O10 H110 0.85(4) . ? 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 O8 K1 O2 91.24(13) . . ? O8 K1 O6 130.59(10) . . ? O2 K1 O6 116.64(7) . . ? O8 K1 O4 81.13(11) . . ? O2 K1 O4 114.75(7) . . ? O6 K1 O4 116.62(7) . . ? O8 K1 O7 58.55(12) . . ? O2 K1 O7 95.28(12) . . ? O6 K1 O7 77.92(9) . . ? O4 K1 O7 130.34(11) . . ? O8 K1 O5 113.09(13) . . ? O2 K1 O5 151.84(7) . . ? O6 K1 O5 58.17(6) . . ? O4 K1 O5 58.87(6) . . ? O7 K1 O5 109.23(11) . . ? O8 K1 O1 127.05(12) . . ? O2 K1 O1 59.32(6) . . ? O6 K1 O1 57.46(6) . . ? O4 K1 O1 149.21(6) . . ? O7 K1 O1 79.89(11) . . ? O5 K1 O1 110.55(6) . . ? O8 K1 O3 80.41(10) . . ? O2 K1 O3 57.57(6) . . ? O6 K1 O3 148.76(6) . . ? O4 K1 O3 57.25(6) . . ? O7 K1 O3 131.10(9) . . ? O5 K1 O3 110.79(6) . . ? O1 K1 O3 110.29(6) . . ? O1 C1 C2 109.3(2) . . ? O1 C1 H1A 109.8 . . ? C2 C1 H1A 109.8 . . ? O1 C1 H1B 109.8 . . ? C2 C1 H1B 109.8 . . ? H1A C1 H1B 108.3 . . ? O2 C2 C1 109.4(2) . . ? O2 C2 H2A 109.8 . . ? C1 C2 H2A 109.8 . . ? O2 C2 H2B 109.8 . . ? C1 C2 H2B 109.8 . . ? H2A C2 H2B 108.2 . . ? O2 C3 C4 109.0(2) . . ? O2 C3 H3A 109.9 . . ? C4 C3 H3A 109.9 . . ? O2 C3 H3B 109.9 . . ? C4 C3 H3B 109.9 . . ? H3A C3 H3B 108.3 . . ? O3 C4 C3 108.8(3) . . ? O3 C4 H4A 109.9 . . ? C3 C4 H4A 109.9 . . ? O3 C4 H4B 109.9 . . ? C3 C4 H4B 109.9 . . ? H4A C4 H4B 108.3 . . ? O3 C5 C6 109.6(3) . . ? O3 C5 H5A 109.8 . . ? C6 C5 H5A 109.8 . . ? O3 C5 H5B 109.8 . . ? C6 C5 H5B 109.8 . . ? H5A C5 H5B 108.2 . . ? O4 C6 C5 109.2(3) . . ? O4 C6 H6A 109.8 . . ? C5 C6 H6A 109.8 . . ? O4 C6 H6B 109.8 . . ? C5 C6 H6B 109.8 . . ? H6A C6 H6B 108.3 . . ? O4 C7 C8 109.1(3) . . ? O4 C7 H7A 109.9 . . ? C8 C7 H7A 109.9 . . ? O4 C7 H7B 109.9 . . ? C8 C7 H7B 109.9 . . ? H7A C7 H7B 108.3 . . ? O5 C8 C7 109.8(3) . . ? O5 C8 H8A 109.7 . . ? C7 C8 H8A 109.7 . . ? O5 C8 H8B 109.7 . . ? C7 C8 H8B 109.7 . . ? H8A C8 H8B 108.2 . . ? O5 C9 C10 109.6(3) . . ? O5 C9 H9A 109.7 . . ? C10 C9 H9A 109.7 . . ? O5 C9 H9B 109.7 . . ? C10 C9 H9B 109.7 . . ? H9A C9 H9B 108.2 . . ? O6 C10 C9 108.3(3) . . ? O6 C10 H10A 110.0 . . ? C9 C10 H10A 110.0 . . ? O6 C10 H10B 110.0 . . ? C9 C10 H10B 110.0 . . ? H10A C10 H10B 108.4 . . ? O6 C11 C12 109.0(3) . . ? O6 C11 H11A 109.9 . . ? C12 C11 H11A 109.9 . . ? O6 C11 H11B 109.9 . . ? C12 C11 H11B 109.9 . . ? H11A C11 H11B 108.3 . . ? O1 C12 C11 109.9(2) . . ? O1 C12 H12A 109.7 . . ? C11 C12 H12A 109.7 . . ? O1 C12 H12B 109.7 . . ? C11 C12 H12B 109.7 . . ? H12A C12 H12B 108.2 . . ? C1 O1 C12 111.6(2) . . ? C1 O1 K1 103.38(17) . . ? C12 O1 K1 107.73(16) . . ? C3 O2 C2 112.4(2) . . ? C3 O2 K1 122.42(17) . . ? C2 O2 K1 118.66(16) . . ? C4 O3 C5 112.2(2) . . ? C4 O3 K1 106.64(17) . . ? C5 O3 K1 107.59(17) . . ? C7 O4 C6 112.4(3) . . ? C7 O4 K1 119.36(18) . . ? C6 O4 K1 122.57(18) . . ? C9 O5 C8 112.4(3) . . ? C9 O5 K1 105.96(18) . . ? C8 O5 K1 107.80(19) . . ? C11 O6 C10 113.2(2) . . ? C11 O6 K1 123.49(17) . . ? C10 O6 K1 120.96(18) . . ? K1 O7 H700 121.0 . . ? K1 O8 H800 131.3 . . ? O11 P1 O12 116.12(14) . . ? O11 P1 O10 109.79(13) . . ? O12 P1 O10 106.40(15) . . ? O11 P1 O9 107.70(14) . . ? O12 P1 O9 108.86(13) . . ? O10 P1 O9 107.69(16) . . ? P1 O9 H900 115(3) . . ? P1 O10 H110 119(3) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 24.96 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.577 _refine_diff_density_min -0.271 _refine_diff_density_rms 0.059 # Attachment 'Rb.CIF.pdf' data_18-Crown[6].Rb[H2PO4].2H2O _database_code_depnum_ccdc_archive 'CCDC 633145' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H30 O12 P Rb' _chemical_formula_weight 482.80 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rb Rb -0.9393 2.9676 '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 25.266(6) _cell_length_b 8.590(5) _cell_length_c 19.394(6) _cell_angle_alpha 90.00 _cell_angle_beta 103.47(2) _cell_angle_gamma 90.00 _cell_volume 4093(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.567 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2000 _exptl_absorpt_coefficient_mu 2.552 _exptl_absorpt_correction_type Psi-scan _exptl_absorpt_correction_T_min 0.601 _exptl_absorpt_correction_T_max 0.665 _exptl_absorpt_process_details ? _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 3698 _diffrn_reflns_av_R_equivalents 0.0209 _diffrn_reflns_av_sigmaI/netI 0.0373 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.42 _diffrn_reflns_theta_max 24.99 _reflns_number_total 3579 _reflns_number_gt 2476 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0832P)^2^+2.5344P] 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 riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0005(1) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3579 _refine_ls_number_parameters 236 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0769 _refine_ls_R_factor_gt 0.0433 _refine_ls_wR_factor_ref 0.1283 _refine_ls_wR_factor_gt 0.1127 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _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 Rb1 Rb 0.123068(17) 0.30517(5) 0.18639(2) 0.04281(19) Uani 1 1 d . . . C1 C 0.2112(2) 0.4905(6) 0.0820(3) 0.0598(14) Uani 1 1 d . . . H1A H 0.1751 0.5343 0.0655 0.072 Uiso 1 1 calc R . . H1B H 0.2319 0.5113 0.0467 0.072 Uiso 1 1 calc R . . C2 C 0.2386(2) 0.5622(6) 0.1505(3) 0.0547(12) Uani 1 1 d . . . H2A H 0.2717 0.5057 0.1713 0.066 Uiso 1 1 calc R . . H2B H 0.2482 0.6692 0.1431 0.066 Uiso 1 1 calc R . . C3 C 0.2253(2) 0.6282(6) 0.2635(3) 0.0575(13) Uani 1 1 d . . . H3A H 0.2343 0.7360 0.2566 0.069 Uiso 1 1 calc R . . H3B H 0.2584 0.5746 0.2868 0.069 Uiso 1 1 calc R . . C4 C 0.1853(2) 0.6204(5) 0.3081(3) 0.0556(13) Uani 1 1 d . . . H4A H 0.1971 0.6863 0.3495 0.067 Uiso 1 1 calc R . . H4B H 0.1503 0.6577 0.2815 0.067 Uiso 1 1 calc R . . C5 C 0.1389(2) 0.4466(6) 0.3678(3) 0.0578(13) Uani 1 1 d . . . H5A H 0.1040 0.4763 0.3378 0.069 Uiso 1 1 calc R . . H5B H 0.1464 0.5142 0.4090 0.069 Uiso 1 1 calc R . . C6 C 0.1368(2) 0.2821(6) 0.3906(2) 0.0541(12) Uani 1 1 d . . . H6A H 0.1721 0.2498 0.4185 0.065 Uiso 1 1 calc R . . H6B H 0.1103 0.2704 0.4193 0.065 Uiso 1 1 calc R . . C7 C 0.1117(2) 0.0329(5) 0.3433(3) 0.0509(12) Uani 1 1 d . . . H7A H 0.0867 0.0268 0.3743 0.061 Uiso 1 1 calc R . . H7B H 0.1454 -0.0185 0.3664 0.061 Uiso 1 1 calc R . . C8 C 0.08751(19) -0.0437(5) 0.2739(3) 0.0520(12) Uani 1 1 d . . . H8A H 0.0781 -0.1505 0.2819 0.062 Uiso 1 1 calc R . . H8B H 0.0545 0.0104 0.2506 0.062 Uiso 1 1 calc R . . C9 C 0.1016(2) -0.1096(6) 0.1629(3) 0.0582(14) Uani 1 1 d . . . H9A H 0.0682 -0.0560 0.1408 0.070 Uiso 1 1 calc R . . H9B H 0.0929 -0.2179 0.1692 0.070 Uiso 1 1 calc R . . C10 C 0.1400(2) -0.0999(5) 0.1169(3) 0.0549(13) Uani 1 1 d . . . H10A H 0.1746 -0.1451 0.1407 0.066 Uiso 1 1 calc R . . H10B H 0.1260 -0.1580 0.0736 0.066 Uiso 1 1 calc R . . C11 C 0.1779(2) 0.0763(6) 0.0481(2) 0.0549(12) Uani 1 1 d . . . H11A H 0.1612 0.0178 0.0059 0.066 Uiso 1 1 calc R . . H11B H 0.2147 0.0377 0.0659 0.066 Uiso 1 1 calc R . . C12 C 0.1792(2) 0.2472(6) 0.0308(2) 0.0518(12) Uani 1 1 d . . . H12A H 0.1973 0.2627 -0.0076 0.062 Uiso 1 1 calc R . . H12B H 0.1423 0.2871 0.0160 0.062 Uiso 1 1 calc R . . O1 O 0.20750(13) 0.3269(3) 0.09202(17) 0.0497(8) Uani 1 1 d . . . O2 O 0.20294(12) 0.5575(4) 0.19652(17) 0.0490(8) Uani 1 1 d . . . O3 O 0.18045(13) 0.4638(3) 0.32985(17) 0.0493(8) Uani 1 1 d . . . O4 O 0.12182(13) 0.1908(4) 0.32888(16) 0.0500(8) Uani 1 1 d . . . O5 O 0.12455(12) -0.0411(3) 0.23058(16) 0.0448(7) Uani 1 1 d . . . O6 O 0.14748(13) 0.0585(3) 0.10033(16) 0.0486(8) Uani 1 1 d . . . O7 O 0.00816(16) 0.2718(7) 0.1821(2) 0.0891(14) Uani 1 1 d . . . O8 O 0.0160(4) -0.4128(10) 0.1884(3) 0.215(5) Uani 1 1 d . . . P1 P 0.00645(5) 0.25213(13) 0.00257(6) 0.0405(3) Uani 1 1 d . . . O11 O 0.05050(12) 0.3616(3) 0.04309(16) 0.0452(7) Uani 1 1 d . . . O12 O -0.03703(18) 0.3488(4) -0.0464(2) 0.0932(16) Uani 1 1 d . . . O13 O 0.03297(16) 0.1499(4) -0.04724(17) 0.0584(9) Uani 1 1 d . . . O14 O -0.01619(16) 0.1474(4) 0.0497(2) 0.0626(10) 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 Rb1 0.0486(3) 0.0342(3) 0.0460(3) -0.0025(2) 0.01171(18) -0.00534(19) C1 0.078(4) 0.042(3) 0.070(4) 0.020(3) 0.038(3) 0.008(3) C2 0.053(3) 0.032(3) 0.083(4) 0.008(2) 0.025(3) -0.003(2) C3 0.061(3) 0.035(3) 0.066(3) 0.002(2) -0.006(3) -0.015(2) C4 0.075(3) 0.032(3) 0.055(3) -0.010(2) 0.003(3) -0.002(2) C5 0.068(3) 0.054(3) 0.054(3) -0.021(2) 0.021(3) -0.003(3) C6 0.065(3) 0.059(3) 0.041(3) -0.003(2) 0.018(2) -0.006(3) C7 0.055(3) 0.042(3) 0.060(3) 0.015(2) 0.022(2) 0.003(2) C8 0.053(3) 0.033(2) 0.072(3) 0.008(2) 0.019(2) -0.006(2) C9 0.073(3) 0.034(3) 0.057(3) -0.003(2) -0.005(3) -0.017(2) C10 0.077(3) 0.031(3) 0.050(3) -0.005(2) 0.001(3) -0.006(2) C11 0.068(3) 0.054(3) 0.045(3) -0.010(2) 0.016(2) 0.004(3) C12 0.062(3) 0.057(3) 0.038(2) 0.010(2) 0.015(2) 0.005(2) O1 0.0583(19) 0.0348(18) 0.0542(19) 0.0084(15) 0.0096(15) 0.0051(14) O2 0.0461(17) 0.0378(18) 0.062(2) -0.0023(15) 0.0097(15) -0.0071(14) O3 0.0571(19) 0.0282(16) 0.061(2) -0.0003(14) 0.0094(16) -0.0017(14) O4 0.066(2) 0.0415(19) 0.0441(17) -0.0004(15) 0.0164(15) -0.0073(15) O5 0.0490(17) 0.0320(16) 0.0502(18) -0.0002(14) 0.0052(14) -0.0086(13) O6 0.067(2) 0.0300(17) 0.0489(18) -0.0024(14) 0.0140(16) 0.0019(15) O7 0.064(2) 0.156(4) 0.053(2) 0.001(3) 0.0250(19) -0.004(3) O8 0.399(12) 0.181(7) 0.084(4) -0.037(4) 0.095(6) -0.200(8) P1 0.0529(7) 0.0148(5) 0.0511(7) -0.0013(4) 0.0067(5) 0.0009(5) O11 0.0527(18) 0.0244(15) 0.0505(18) -0.0031(13) -0.0039(14) 0.0000(13) O12 0.096(3) 0.0234(17) 0.118(3) -0.014(2) -0.061(3) 0.0082(18) O13 0.100(3) 0.0281(16) 0.056(2) -0.0085(14) 0.0349(19) -0.0118(17) O14 0.096(3) 0.0239(16) 0.083(2) -0.0159(16) 0.051(2) -0.0087(17) _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 Rb1 O6 2.852(3) . ? Rb1 O7 2.899(4) . ? Rb1 O2 2.937(3) . ? Rb1 O4 2.940(3) . ? Rb1 O11 2.991(3) . ? Rb1 O5 3.093(3) . ? Rb1 O1 3.123(3) . ? Rb1 O3 3.134(3) . ? Rb1 C9 3.617(5) . ? Rb1 O8 3.638(12) 1_565 ? Rb1 C5 3.655(5) . ? Rb1 C12 3.654(5) . ? C1 O1 1.425(6) . ? C1 C2 1.481(8) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 O2 1.408(6) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 O2 1.425(6) . ? C3 C4 1.477(7) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 O3 1.424(6) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 O3 1.423(6) . ? C5 C6 1.485(7) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 O4 1.407(5) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 O4 1.420(5) . ? C7 C8 1.494(7) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 O5 1.396(6) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 O5 1.432(6) . ? C9 C10 1.464(7) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 O6 1.421(6) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 O6 1.416(5) . ? C11 C12 1.508(7) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 O1 1.412(6) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? O8 Rb1 3.638(12) 1_545 ? P1 O14 1.488(4) . ? P1 O12 1.521(4) . ? P1 O11 1.528(3) . ? P1 O13 1.567(3) . ? 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 Rb1 O7 105.13(12) . . ? O6 Rb1 O2 110.40(9) . . ? O7 Rb1 O2 137.99(13) . . ? O6 Rb1 O4 110.66(9) . . ? O7 Rb1 O4 76.37(10) . . ? O2 Rb1 O4 109.96(9) . . ? O6 Rb1 O11 75.28(9) . . ? O7 Rb1 O11 66.18(10) . . ? O2 Rb1 O11 101.86(9) . . ? O4 Rb1 O11 142.10(9) . . ? O6 Rb1 O5 57.14(9) . . ? O7 Rb1 O5 81.97(12) . . ? O2 Rb1 O5 136.67(8) . . ? O4 Rb1 O5 54.57(8) . . ? O11 Rb1 O5 112.24(8) . . ? O6 Rb1 O1 55.33(9) . . ? O7 Rb1 O1 143.61(10) . . ? O2 Rb1 O1 56.12(9) . . ? O4 Rb1 O1 136.81(9) . . ? O11 Rb1 O1 78.48(9) . . ? O5 Rb1 O1 104.71(8) . . ? O6 Rb1 O3 136.40(8) . . ? O7 Rb1 O3 108.78(10) . . ? O2 Rb1 O3 56.71(9) . . ? O4 Rb1 O3 54.18(9) . . ? O11 Rb1 O3 144.22(8) . . ? O5 Rb1 O3 101.47(8) . . ? O1 Rb1 O3 104.86(9) . . ? O6 Rb1 C9 40.61(11) . . ? O7 Rb1 C9 77.25(14) . . ? O2 Rb1 C9 144.67(11) . . ? O4 Rb1 C9 75.82(10) . . ? O11 Rb1 C9 90.07(10) . . ? O5 Rb1 C9 22.99(10) . . ? O1 Rb1 C9 95.03(11) . . ? O3 Rb1 C9 124.39(10) . . ? O6 Rb1 O8 139.78(11) . 1_565 ? O7 Rb1 O8 47.49(14) . 1_565 ? O2 Rb1 O8 90.51(12) . 1_565 ? O4 Rb1 O8 92.40(11) . 1_565 ? O11 Rb1 O8 66.77(11) . 1_565 ? O5 Rb1 O8 126.76(11) . 1_565 ? O1 Rb1 O8 125.27(10) . 1_565 ? O3 Rb1 O8 83.83(11) . 1_565 ? C9 Rb1 O8 124.58(13) . 1_565 ? O6 Rb1 C5 145.10(11) . . ? O7 Rb1 C5 86.86(12) . . ? O2 Rb1 C5 76.75(11) . . ? O4 Rb1 C5 39.56(11) . . ? O11 Rb1 C5 138.29(11) . . ? O5 Rb1 C5 93.52(11) . . ? O1 Rb1 C5 127.43(10) . . ? O3 Rb1 C5 22.57(10) . . ? C9 Rb1 C5 115.36(12) . . ? O8 Rb1 C5 71.54(13) 1_565 . ? O6 Rb1 C12 40.30(11) . . ? O7 Rb1 C12 122.75(11) . . ? O2 Rb1 C12 76.30(11) . . ? O4 Rb1 C12 145.25(10) . . ? O11 Rb1 C12 61.75(10) . . ? O5 Rb1 C12 96.65(10) . . ? O1 Rb1 C12 22.33(10) . . ? O3 Rb1 C12 127.16(10) . . ? C9 Rb1 C12 80.63(12) . . ? O8 Rb1 C12 122.13(12) 1_565 . ? C5 Rb1 C12 149.72(12) . . ? O1 C1 C2 108.7(4) . . ? O1 C1 Rb1 55.5(2) . . ? C2 C1 Rb1 84.4(3) . . ? O1 C1 H1A 110.0 . . ? C2 C1 H1A 110.0 . . ? Rb1 C1 H1A 73.0 . . ? O1 C1 H1B 110.0 . . ? C2 C1 H1B 110.0 . . ? Rb1 C1 H1B 163.2 . . ? H1A C1 H1B 108.3 . . ? O2 C2 C1 108.8(4) . . ? O2 C2 H2A 109.9 . . ? C1 C2 H2A 109.9 . . ? O2 C2 H2B 109.9 . . ? C1 C2 H2B 109.9 . . ? H2A C2 H2B 108.3 . . ? O2 C3 C4 109.5(4) . . ? O2 C3 H3A 109.8 . . ? C4 C3 H3A 109.8 . . ? O2 C3 H3B 109.8 . . ? C4 C3 H3B 109.8 . . ? H3A C3 H3B 108.2 . . ? O3 C4 C3 109.6(4) . . ? O3 C4 Rb1 56.2(2) . . ? C3 C4 Rb1 84.6(3) . . ? O3 C4 H4A 109.8 . . ? C3 C4 H4A 109.8 . . ? Rb1 C4 H4A 163.5 . . ? O3 C4 H4B 109.8 . . ? C3 C4 H4B 109.8 . . ? Rb1 C4 H4B 72.7 . . ? H4A C4 H4B 108.2 . . ? O3 C5 C6 109.5(4) . . ? O3 C5 Rb1 57.7(2) . . ? C6 C5 Rb1 88.1(3) . . ? O3 C5 H5A 109.8 . . ? C6 C5 H5A 109.8 . . ? Rb1 C5 H5A 68.2 . . ? O3 C5 H5B 109.8 . . ? C6 C5 H5B 109.8 . . ? Rb1 C5 H5B 161.5 . . ? H5A C5 H5B 108.2 . . ? O4 C6 C5 107.4(4) . . ? O4 C6 H6A 110.2 . . ? C5 C6 H6A 110.2 . . ? O4 C6 H6B 110.2 . . ? C5 C6 H6B 110.2 . . ? H6A C6 H6B 108.5 . . ? O4 C7 C8 107.3(4) . . ? O4 C7 H7A 110.3 . . ? C8 C7 H7A 110.3 . . ? O4 C7 H7B 110.3 . . ? C8 C7 H7B 110.3 . . ? H7A C7 H7B 108.5 . . ? O5 C8 C7 110.1(4) . . ? O5 C8 Rb1 55.7(2) . . ? C7 C8 Rb1 87.9(3) . . ? O5 C8 H8A 109.6 . . ? C7 C8 H8A 109.6 . . ? Rb1 C8 H8A 161.1 . . ? O5 C8 H8B 109.6 . . ? C7 C8 H8B 109.6 . . ? Rb1 C8 H8B 70.6 . . ? H8A C8 H8B 108.2 . . ? O5 C9 C10 110.6(4) . . ? O5 C9 Rb1 57.5(2) . . ? C10 C9 Rb1 85.4(3) . . ? O5 C9 H9A 109.5 . . ? C10 C9 H9A 109.5 . . ? Rb1 C9 H9A 71.1 . . ? O5 C9 H9B 109.5 . . ? C10 C9 H9B 109.5 . . ? Rb1 C9 H9B 163.8 . . ? H9A C9 H9B 108.1 . . ? O6 C10 C9 109.6(4) . . ? O6 C10 H10A 109.8 . . ? C9 C10 H10A 109.8 . . ? O6 C10 H10B 109.8 . . ? C9 C10 H10B 109.8 . . ? H10A C10 H10B 108.2 . . ? O6 C11 C12 107.9(4) . . ? O6 C11 H11A 110.1 . . ? C12 C11 H11A 110.1 . . ? O6 C11 H11B 110.1 . . ? C12 C11 H11B 110.1 . . ? H11A C11 H11B 108.4 . . ? O1 C12 C11 108.5(4) . . ? O1 C12 Rb1 57.2(2) . . ? C11 C12 Rb1 85.2(3) . . ? O1 C12 H12A 110.0 . . ? C11 C12 H12A 110.0 . . ? Rb1 C12 H12A 163.5 . . ? O1 C12 H12B 110.0 . . ? C11 C12 H12B 110.0 . . ? Rb1 C12 H12B 70.6 . . ? H12A C12 H12B 108.4 . . ? C12 O1 C1 113.6(4) . . ? C12 O1 Rb1 100.5(3) . . ? C1 O1 Rb1 102.4(3) . . ? C2 O2 C3 112.8(4) . . ? C2 O2 Rb1 120.7(3) . . ? C3 O2 Rb1 119.7(3) . . ? C4 O3 C5 112.1(4) . . ? C4 O3 Rb1 101.7(3) . . ? C5 O3 Rb1 99.8(3) . . ? C6 O4 C7 113.0(4) . . ? C6 O4 Rb1 123.6(3) . . ? C7 O4 Rb1 123.1(3) . . ? C8 O5 C9 111.1(4) . . ? C8 O5 Rb1 102.5(2) . . ? C9 O5 Rb1 99.5(2) . . ? C11 O6 C10 112.9(4) . . ? C11 O6 Rb1 124.5(3) . . ? C10 O6 Rb1 121.4(3) . . ? O14 P1 O12 112.9(3) . . ? O14 P1 O11 113.2(2) . . ? O12 P1 O11 108.60(19) . . ? O14 P1 O13 108.71(18) . . ? O12 P1 O13 105.7(2) . . ? O11 P1 O13 107.28(19) . . ? P1 O11 Rb1 126.42(16) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.855 _refine_diff_density_min -0.887 _refine_diff_density_rms 0.096