# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2008 data_global _journal_coden_Cambridge 440 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Fabrizia Grepioni' 'Dario Braga' 'Enrico Modena' 'Marco Polito' 'Katia Rubini' _publ_contact_author_name 'Fabrizia Grepioni' _publ_contact_author_email FABRIZIA.GREPIONI@UNIBO.IT _publ_section_title ; Crystal forms of highly "dynamical" 18-Crown[6] complexes with M[HSO4] and M[H2PO4] (M+ = NH4+, Rb+, Cs+): thermal behaviour and solid-state preparation ; # Attachment '1_rev.CIF' data_1 _database_code_depnum_ccdc_archive 'CCDC 688380' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H31.50 N O11 P0.50 S0.50' _chemical_formula_weight 397.40 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M F2dd loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/4, y+1/4, -z+1/4' 'x, -y, -z' 'x+1/4, -y+1/4, z+1/4' 'x, y+1/2, z+1/2' 'x+1/4, y+3/4, -z+3/4' 'x, -y+1/2, -z+1/2' 'x+1/4, -y+3/4, z+3/4' 'x+1/2, y, z+1/2' 'x+3/4, y+1/4, -z+3/4' 'x+1/2, -y, -z+1/2' 'x+3/4, -y+1/4, z+3/4' 'x+1/2, y+1/2, z' 'x+3/4, y+3/4, -z+1/4' 'x+1/2, -y+1/2, -z' 'x+3/4, -y+3/4, z+1/4' _cell_length_a 8.710(5) _cell_length_b 28.868(7) _cell_length_c 31.206(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7846(5) _cell_formula_units_Z 16 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.346 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3424 _exptl_absorpt_coefficient_mu 0.205 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 1830 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0321 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 3.22 _diffrn_reflns_theta_max 24.94 _reflns_number_total 1830 _reflns_number_gt 1285 _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^)+(0.1282P)^2^+6.7307P] 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 none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.3(2) _refine_ls_number_reflns 1830 _refine_ls_number_parameters 227 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0912 _refine_ls_R_factor_gt 0.0598 _refine_ls_wR_factor_ref 0.1875 _refine_ls_wR_factor_gt 0.1613 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _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 P1 P 0.11166(19) 0.45449(5) 0.04934(5) 0.0498(5) Uani 0.50 1 d P . . S1 S 0.11166(19) 0.45449(5) 0.04934(5) 0.0498(5) Uani 0.50 1 d P . . O7 O 0.1623(8) 0.50354(18) 0.05471(16) 0.0818(18) Uani 1 1 d . . . O8 O 0.1307(11) 0.43899(19) 0.00475(18) 0.096(2) Uani 1 1 d . . . O9 O -0.0599(8) 0.4564(3) 0.0588(3) 0.107(2) Uani 1 1 d . . . O10 O 0.1847(9) 0.42355(18) 0.08004(18) 0.0859(18) Uani 1 1 d . . . O11 O -0.0156(15) 0.0000 0.0000 0.270(15) Uani 1 2 d S . . O12 O 0.2802(11) 0.0000 0.0000 0.142(5) Uani 1 2 d S . . O1 O 0.0634(6) 0.29565(16) 0.00447(16) 0.0664(14) Uani 1 1 d . . . C1 C 0.0592(11) 0.2911(3) -0.0399(3) 0.074(2) Uani 1 1 d . . . H1A H -0.0463 0.2879 -0.0494 0.089 Uiso 1 1 calc R . . H1B H 0.1150 0.2636 -0.0485 0.089 Uiso 1 1 calc R . . C2 C 0.1288(10) 0.3323(3) -0.0599(2) 0.073(2) Uani 1 1 d . . . H2A H 0.1147 0.3311 -0.0907 0.088 Uiso 1 1 calc R . . H2B H 0.0794 0.3601 -0.0493 0.088 Uiso 1 1 calc R . . O2 O 0.2914(7) 0.33347(16) -0.04987(15) 0.0654(13) Uani 1 1 d . . . C3 C 0.3674(14) 0.3721(3) -0.0674(3) 0.081(2) Uani 1 1 d . . . H3A H 0.3262 0.4004 -0.0552 0.098 Uiso 1 1 calc R . . H3B H 0.3515 0.3730 -0.0982 0.098 Uiso 1 1 calc R . . C4 C 0.5349(14) 0.3686(3) -0.0579(3) 0.091(3) Uani 1 1 d . . . H4A H 0.5747 0.3393 -0.0682 0.109 Uiso 1 1 calc R . . H4B H 0.5899 0.3934 -0.0722 0.109 Uiso 1 1 calc R . . O3 O 0.5566(7) 0.37198(19) -0.0126(2) 0.0823(18) Uani 1 1 d . . . C5 C 0.7104(12) 0.3677(3) 0.0002(5) 0.103(4) Uani 1 1 d . . . H5A H 0.7710 0.3916 -0.0137 0.124 Uiso 1 1 calc R . . H5B H 0.7496 0.3379 -0.0090 0.124 Uiso 1 1 calc R . . C6 C 0.7275(12) 0.3719(3) 0.0468(5) 0.107(4) Uani 1 1 d . . . H6A H 0.8356 0.3727 0.0542 0.128 Uiso 1 1 calc R . . H6B H 0.6809 0.4005 0.0565 0.128 Uiso 1 1 calc R . . O4 O 0.6550(6) 0.33325(18) 0.0677(2) 0.0763(16) Uani 1 1 d . . . C7 C 0.6580(10) 0.3375(3) 0.1125(3) 0.087(3) Uani 1 1 d . . . H7A H 0.6004 0.3647 0.1211 0.104 Uiso 1 1 calc R . . H7B H 0.7631 0.3412 0.1222 0.104 Uiso 1 1 calc R . . C8 C 0.5907(10) 0.2962(4) 0.1318(3) 0.083(3) Uani 1 1 d . . . H8A H 0.6431 0.2688 0.1215 0.099 Uiso 1 1 calc R . . H8B H 0.6018 0.2975 0.1627 0.099 Uiso 1 1 calc R . . O5 O 0.4318(7) 0.29423(16) 0.12065(15) 0.0643(13) Uani 1 1 d . . . C9 C 0.3601(12) 0.2544(3) 0.1379(2) 0.072(2) Uani 1 1 d . . . H9A H 0.3738 0.2534 0.1687 0.087 Uiso 1 1 calc R . . H9B H 0.4045 0.2266 0.1256 0.087 Uiso 1 1 calc R . . C10 C 0.1977(12) 0.2574(3) 0.1272(2) 0.071(2) Uani 1 1 d . . . H10A H 0.1437 0.2319 0.1408 0.085 Uiso 1 1 calc R . . H10B H 0.1565 0.2861 0.1387 0.085 Uiso 1 1 calc R . . O6 O 0.1705(6) 0.25600(17) 0.08202(16) 0.0627(13) Uani 1 1 d . . . C11 C 0.0146(9) 0.2611(3) 0.0715(3) 0.071(2) Uani 1 1 d . . . H11A H -0.0219 0.2911 0.0811 0.086 Uiso 1 1 calc R . . H11B H -0.0453 0.2374 0.0859 0.086 Uiso 1 1 calc R . . C12 C -0.0043(9) 0.2570(3) 0.0257(3) 0.071(2) Uani 1 1 d . . . H12A H 0.0437 0.2286 0.0158 0.085 Uiso 1 1 calc R . . H12B H -0.1128 0.2555 0.0188 0.085 Uiso 1 1 calc R . . N1 N 0.3149(6) 0.34398(17) 0.04559(17) 0.0509(13) 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 P1 0.0434(8) 0.0439(7) 0.0621(9) -0.0017(7) -0.0035(8) 0.0027(7) S1 0.0434(8) 0.0439(7) 0.0621(9) -0.0017(7) -0.0035(8) 0.0027(7) O7 0.101(5) 0.065(3) 0.079(3) 0.001(2) -0.040(3) -0.018(3) O8 0.138(6) 0.068(3) 0.082(4) -0.003(3) 0.012(4) 0.019(4) O9 0.048(4) 0.124(6) 0.149(6) -0.001(4) 0.013(4) -0.005(4) O10 0.114(5) 0.065(3) 0.078(3) 0.009(3) -0.009(3) 0.020(3) O11 0.039(6) 0.66(5) 0.111(9) -0.017(16) 0.000 0.000 O12 0.037(5) 0.257(15) 0.131(8) 0.063(9) 0.000 0.000 O1 0.054(3) 0.064(3) 0.081(3) -0.018(2) -0.012(3) 0.001(2) C1 0.056(4) 0.085(5) 0.082(5) -0.009(4) -0.016(4) 0.016(4) C2 0.070(5) 0.089(5) 0.061(4) 0.001(4) -0.020(4) 0.029(5) O2 0.075(3) 0.062(3) 0.059(3) 0.012(2) 0.008(3) 0.017(3) C3 0.099(7) 0.068(4) 0.076(5) 0.015(4) 0.025(5) 0.016(5) C4 0.115(8) 0.064(5) 0.095(6) 0.020(4) 0.063(6) 0.003(5) O3 0.063(4) 0.070(3) 0.114(5) 0.009(3) 0.039(3) -0.010(3) C5 0.069(7) 0.077(6) 0.163(11) 0.013(6) 0.040(7) -0.020(5) C6 0.053(5) 0.079(6) 0.189(12) 0.003(6) -0.006(6) -0.031(5) O4 0.047(3) 0.071(3) 0.111(4) -0.024(3) -0.006(3) -0.008(2) C7 0.056(5) 0.096(6) 0.107(7) -0.045(5) -0.015(5) 0.010(5) C8 0.064(5) 0.113(7) 0.071(5) -0.026(5) -0.028(4) 0.030(5) O5 0.066(3) 0.068(3) 0.059(3) -0.003(2) -0.004(2) 0.007(3) C9 0.082(6) 0.083(5) 0.052(4) 0.009(3) 0.010(4) 0.012(5) C10 0.096(7) 0.071(5) 0.047(4) 0.000(3) 0.030(4) -0.008(5) O6 0.053(3) 0.066(3) 0.070(3) -0.002(2) 0.017(2) -0.004(2) C11 0.045(4) 0.076(5) 0.093(6) -0.007(4) 0.016(4) -0.015(3) C12 0.043(4) 0.059(4) 0.111(6) 0.002(4) -0.003(4) -0.015(3) N1 0.042(3) 0.050(3) 0.060(3) 0.004(2) 0.001(2) -0.003(2) _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 P1 O10 1.456(6) . ? P1 O8 1.471(6) . ? P1 O7 1.493(5) . ? P1 O9 1.524(7) . ? O1 C1 1.393(9) . ? O1 C12 1.425(9) . ? C1 C2 1.472(12) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 O2 1.451(11) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? O2 C3 1.408(10) . ? C3 C4 1.492(17) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 O3 1.430(12) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? O3 C5 1.403(13) . ? C5 C6 1.466(16) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 O4 1.438(12) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? O4 C7 1.402(11) . ? C7 C8 1.459(14) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 O5 1.429(10) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? O5 C9 1.415(10) . ? C9 C10 1.456(13) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 O6 1.432(9) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? O6 C11 1.404(10) . ? C11 C12 1.445(11) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? 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 P1 O8 112.7(3) . . ? O10 P1 O7 112.3(3) . . ? O8 P1 O7 111.2(4) . . ? O10 P1 O9 108.9(5) . . ? O8 P1 O9 107.7(5) . . ? O7 P1 O9 103.5(4) . . ? C1 O1 C12 112.2(6) . . ? O1 C1 C2 109.6(7) . . ? O1 C1 H1A 109.8 . . ? C2 C1 H1A 109.8 . . ? O1 C1 H1B 109.8 . . ? C2 C1 H1B 109.8 . . ? H1A C1 H1B 108.2 . . ? O2 C2 C1 109.2(6) . . ? O2 C2 H2A 109.8 . . ? C1 C2 H2A 109.8 . . ? O2 C2 H2B 109.8 . . ? C1 C2 H2B 109.8 . . ? H2A C2 H2B 108.3 . . ? C3 O2 C2 113.2(7) . . ? O2 C3 C4 109.2(7) . . ? O2 C3 H3A 109.8 . . ? C4 C3 H3A 109.8 . . ? O2 C3 H3B 109.8 . . ? C4 C3 H3B 109.8 . . ? H3A C3 H3B 108.3 . . ? O3 C4 C3 108.8(7) . . ? 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 . . ? C5 O3 C4 113.6(8) . . ? O3 C5 C6 111.8(9) . . ? O3 C5 H5A 109.3 . . ? C6 C5 H5A 109.3 . . ? O3 C5 H5B 109.3 . . ? C6 C5 H5B 109.3 . . ? H5A C5 H5B 107.9 . . ? O4 C6 C5 110.1(8) . . ? O4 C6 H6A 109.6 . . ? C5 C6 H6A 109.6 . . ? O4 C6 H6B 109.6 . . ? C5 C6 H6B 109.6 . . ? H6A C6 H6B 108.2 . . ? C7 O4 C6 112.1(8) . . ? O4 C7 C8 109.5(7) . . ? O4 C7 H7A 109.8 . . ? C8 C7 H7A 109.8 . . ? O4 C7 H7B 109.8 . . ? C8 C7 H7B 109.8 . . ? H7A C7 H7B 108.2 . . ? O5 C8 C7 108.7(7) . . ? O5 C8 H8A 110.0 . . ? C7 C8 H8A 110.0 . . ? O5 C8 H8B 110.0 . . ? C7 C8 H8B 110.0 . . ? H8A C8 H8B 108.3 . . ? C9 O5 C8 111.5(7) . . ? O5 C9 C10 107.0(6) . . ? O5 C9 H9A 110.3 . . ? C10 C9 H9A 110.3 . . ? O5 C9 H9B 110.3 . . ? C10 C9 H9B 110.3 . . ? H9A C9 H9B 108.6 . . ? O6 C10 C9 112.6(6) . . ? O6 C10 H10A 109.1 . . ? C9 C10 H10A 109.1 . . ? O6 C10 H10B 109.1 . . ? C9 C10 H10B 109.1 . . ? H10A C10 H10B 107.8 . . ? C11 O6 C10 112.8(6) . . ? O6 C11 C12 109.4(6) . . ? O6 C11 H11A 109.8 . . ? C12 C11 H11A 109.8 . . ? O6 C11 H11B 109.8 . . ? C12 C11 H11B 109.8 . . ? H11A C11 H11B 108.2 . . ? O1 C12 C11 110.5(6) . . ? O1 C12 H12A 109.6 . . ? C11 C12 H12A 109.6 . . ? O1 C12 H12B 109.6 . . ? C11 C12 H12B 109.6 . . ? H12A C12 H12B 108.1 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 24.94 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.399 _refine_diff_density_min -0.254 _refine_diff_density_rms 0.071 # Attachment '2.CIF' data_2 _database_code_depnum_ccdc_archive 'CCDC 688381' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H31.50 O13 P0.50 Rb S0.50' _chemical_formula_weight 500.86 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' S S 0.1246 0.1234 '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 19.802(4) _cell_length_b 8.447(4) _cell_length_c 25.777(7) _cell_angle_alpha 90.00 _cell_angle_beta 101.00(2) _cell_angle_gamma 90.00 _cell_volume 4232(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 ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.572 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2080 _exptl_absorpt_coefficient_mu 2.486 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 2583 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0503 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.19 _diffrn_reflns_theta_max 21.98 _reflns_number_total 2583 _reflns_number_gt 1807 _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^)+(0.0647P)^2^+8.0516P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2583 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0744 _refine_ls_R_factor_gt 0.0390 _refine_ls_wR_factor_ref 0.1124 _refine_ls_wR_factor_gt 0.1008 _refine_ls_goodness_of_fit_ref 0.998 _refine_ls_restrained_S_all 0.998 _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 P1 P 0.08068(8) -0.1456(2) 0.49213(7) 0.0457(4) Uani 0.50 1 d P . . S1 S 0.08068(8) -0.1456(2) 0.49213(7) 0.0457(4) Uani 0.50 1 d P . . O1A O 0.0763(4) -0.0587(10) 0.5447(3) 0.048(2) Uani 0.60 1 d P A 1 O2A O 0.1496(5) -0.1437(17) 0.4837(4) 0.056(3) Uani 0.60 1 d P A 1 O3A O 0.0499(5) -0.3039(9) 0.4917(4) 0.062(2) Uani 0.60 1 d P A 1 O1B O 0.0443(11) -0.163(3) 0.5337(8) 0.156(11) Uani 0.40 1 d P A 2 O2B O 0.1529(13) -0.105(3) 0.5107(11) 0.140(12) Uani 0.40 1 d P A 2 O3B O 0.0897(8) -0.3154(15) 0.4708(7) 0.092(5) Uani 0.40 1 d P A 2 O4 O 0.0400(2) -0.0467(6) 0.44891(17) 0.0682(14) Uani 1 1 d . A . O5 O 0.2800(3) -0.1019(6) 0.55390(19) 0.0808(16) Uani 1 1 d . A . O6 O 0.1801(3) 0.2107(6) 0.50339(18) 0.0735(14) Uani 1 1 d . A . O7 O 0.0596(3) -0.6235(6) 0.46514(19) 0.0787(15) Uani 1 1 d . . . Rb1 Rb 0.20199(3) 0.09138(7) 0.61984(2) 0.0425(2) Uani 1 1 d . . . C1 C 0.0320(3) 0.1285(7) 0.6759(3) 0.0473(17) Uani 1 1 d . . . H1A H -0.0158 0.1394 0.6586 0.057 Uiso 1 1 calc R A . H1B H 0.0369 0.1712 0.7114 0.057 Uiso 1 1 calc R . . C2 C 0.0517(3) -0.0402(7) 0.6785(2) 0.0466(16) Uani 1 1 d . A . H2A H 0.0221 -0.0990 0.6976 0.056 Uiso 1 1 calc R . . H2B H 0.0459 -0.0834 0.6431 0.056 Uiso 1 1 calc R . . C3 C 0.1440(3) -0.2156(7) 0.7064(3) 0.0474(16) Uani 1 1 d . . . H3A H 0.1391 -0.2565 0.6707 0.057 Uiso 1 1 calc R A . H3B H 0.1157 -0.2792 0.7251 0.057 Uiso 1 1 calc R . . C4 C 0.2166(3) -0.2257(7) 0.7332(2) 0.0464(16) Uani 1 1 d . A . H4A H 0.2226 -0.1736 0.7673 0.056 Uiso 1 1 calc R . . H4B H 0.2299 -0.3358 0.7390 0.056 Uiso 1 1 calc R . . C5 C 0.3289(3) -0.1561(7) 0.7255(2) 0.0428(15) Uani 1 1 d . . . H5A H 0.3432 -0.2647 0.7332 0.051 Uiso 1 1 calc R A . H5B H 0.3361 -0.0977 0.7585 0.051 Uiso 1 1 calc R . . C6 C 0.3701(3) -0.0846(7) 0.6893(2) 0.0457(15) Uani 1 1 d . A . H6A H 0.4187 -0.0975 0.7037 0.055 Uiso 1 1 calc R . . H6B H 0.3599 -0.1373 0.6552 0.055 Uiso 1 1 calc R . . C7 C 0.3878(3) 0.1543(8) 0.6462(2) 0.0503(17) Uani 1 1 d . A . H7A H 0.3724 0.1096 0.6113 0.060 Uiso 1 1 calc R . . H7B H 0.4371 0.1382 0.6562 0.060 Uiso 1 1 calc R . . C8 C 0.3719(3) 0.3272(7) 0.6454(3) 0.0491(17) Uani 1 1 d . . . H8A H 0.3840 0.3706 0.6808 0.059 Uiso 1 1 calc R A . H8B H 0.3984 0.3824 0.6229 0.059 Uiso 1 1 calc R . . C9 C 0.2810(3) 0.5094(7) 0.6246(3) 0.0520(18) Uani 1 1 d . . . H9A H 0.3097 0.5710 0.6056 0.062 Uiso 1 1 calc R A . H9B H 0.2870 0.5501 0.6604 0.062 Uiso 1 1 calc R . . C10 C 0.2087(3) 0.5243(8) 0.5986(3) 0.0519(17) Uani 1 1 d . A . H10A H 0.1964 0.6353 0.5943 0.062 Uiso 1 1 calc R . . H10B H 0.2020 0.4764 0.5638 0.062 Uiso 1 1 calc R . . C11 C 0.0961(3) 0.4465(8) 0.6038(2) 0.0518(17) Uani 1 1 d . A . H11A H 0.0913 0.3876 0.5710 0.062 Uiso 1 1 calc R . . H11B H 0.0804 0.5539 0.5954 0.062 Uiso 1 1 calc R . . C12 C 0.0542(3) 0.3729(7) 0.6381(2) 0.0479(17) Uani 1 1 d . . . H12A H 0.0600 0.4298 0.6713 0.058 Uiso 1 1 calc R A . H12B H 0.0060 0.3777 0.6214 0.058 Uiso 1 1 calc R . . O8 O 0.07429(18) 0.2133(4) 0.64758(15) 0.0419(10) Uani 1 1 d . A . O9 O 0.12199(19) -0.0562(4) 0.70477(15) 0.0422(10) Uani 1 1 d . A . O10 O 0.25857(18) -0.1519(4) 0.70155(14) 0.0389(9) Uani 1 1 d . A . O11 O 0.35392(18) 0.0780(4) 0.68303(15) 0.0425(10) Uani 1 1 d . A . O12 O 0.30091(19) 0.3473(5) 0.62572(16) 0.0440(10) Uani 1 1 d . A . O13 O 0.16589(19) 0.4485(4) 0.62916(15) 0.0431(10) Uani 1 1 d . A . 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 P1 0.0380(9) 0.0519(11) 0.0455(10) 0.0021(8) 0.0034(8) 0.0021(8) S1 0.0380(9) 0.0519(11) 0.0455(10) 0.0021(8) 0.0034(8) 0.0021(8) O1A 0.042(5) 0.064(6) 0.032(5) -0.010(4) -0.009(3) -0.005(4) O2A 0.024(5) 0.088(9) 0.056(6) -0.014(5) 0.008(5) -0.007(5) O3A 0.074(6) 0.040(5) 0.078(6) -0.009(4) 0.027(5) -0.002(5) O1B 0.16(2) 0.24(3) 0.095(17) 0.124(19) 0.084(15) 0.132(18) O2B 0.085(14) 0.087(15) 0.21(3) 0.006(19) -0.073(18) -0.029(11) O3B 0.083(10) 0.043(8) 0.149(15) -0.032(9) 0.017(10) 0.001(8) O4 0.081(3) 0.077(3) 0.048(3) 0.018(3) 0.013(2) 0.025(3) O5 0.083(3) 0.086(4) 0.068(3) -0.029(3) 0.001(3) 0.019(3) O6 0.097(4) 0.066(3) 0.061(3) -0.005(3) 0.023(3) -0.017(3) O7 0.097(4) 0.080(4) 0.058(3) 0.003(3) 0.014(3) -0.001(3) Rb1 0.0434(4) 0.0417(4) 0.0431(4) 0.0003(3) 0.0097(3) 0.0009(3) C1 0.031(3) 0.060(5) 0.052(4) -0.006(3) 0.010(3) -0.001(3) C2 0.038(3) 0.055(4) 0.045(4) 0.002(3) 0.002(3) -0.013(3) C3 0.060(4) 0.036(4) 0.048(4) 0.001(3) 0.012(3) -0.007(3) C4 0.056(4) 0.040(4) 0.041(4) 0.012(3) 0.007(3) 0.009(3) C5 0.049(4) 0.037(3) 0.040(4) 0.003(3) 0.000(3) 0.006(3) C6 0.044(3) 0.040(4) 0.051(4) -0.001(3) 0.003(3) 0.007(3) C7 0.037(3) 0.068(5) 0.049(4) 0.000(4) 0.016(3) -0.002(3) C8 0.042(4) 0.045(4) 0.061(5) 0.006(3) 0.011(3) -0.009(3) C9 0.059(5) 0.044(4) 0.056(5) -0.009(3) 0.019(4) -0.019(3) C10 0.076(5) 0.037(4) 0.045(4) 0.007(3) 0.018(4) 0.005(3) C11 0.058(4) 0.053(4) 0.041(4) 0.004(3) 0.000(3) 0.014(3) C12 0.042(4) 0.050(4) 0.046(4) -0.006(3) -0.006(3) 0.010(3) O8 0.041(2) 0.040(2) 0.046(3) 0.003(2) 0.0087(19) 0.0065(19) O9 0.041(2) 0.039(3) 0.043(2) -0.0013(19) -0.0014(18) -0.0038(18) O10 0.041(2) 0.042(2) 0.032(2) 0.0089(19) 0.0027(18) 0.0004(18) O11 0.042(2) 0.042(2) 0.046(2) -0.001(2) 0.0173(19) 0.0050(19) O12 0.039(2) 0.039(2) 0.053(3) 0.003(2) 0.0087(19) -0.0055(19) O13 0.046(2) 0.045(3) 0.036(2) 0.010(2) 0.0025(19) -0.0012(19) _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 P1 O1B 1.409(16) . ? P1 O2A 1.422(10) . ? P1 O3A 1.469(8) . ? P1 O2B 1.46(2) . ? P1 O4 1.498(5) . ? P1 O1A 1.558(9) . ? P1 O3B 1.558(13) . ? O1A Rb1 3.116(7) . ? O2B Rb1 3.25(2) . ? O5 Rb1 2.991(5) . ? O6 Rb1 3.117(5) . ? Rb1 O12 2.902(4) . ? Rb1 O8 2.942(4) . ? Rb1 O10 3.002(4) . ? Rb1 O13 3.120(4) . ? Rb1 O11 3.138(4) . ? Rb1 O9 3.191(4) . ? Rb1 C7 3.650(6) . ? Rb1 C11 3.638(6) . ? C1 O8 1.407(7) . ? C1 C2 1.476(8) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 O9 1.434(7) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 O9 1.413(7) . ? C3 C4 1.474(8) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 O10 1.416(6) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 O10 1.412(6) . ? C5 C6 1.480(8) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 O11 1.412(7) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 O11 1.417(7) . ? C7 C8 1.493(8) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 O12 1.411(7) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 O12 1.424(7) . ? C9 C10 1.466(8) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 O13 1.416(7) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 O13 1.412(7) . ? C11 C12 1.463(8) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 O8 1.413(7) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? 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 O1B P1 O2A 139.6(10) . . ? O1B P1 O3A 68.7(13) . . ? O2A P1 O3A 114.7(7) . . ? O1B P1 O2B 112.8(16) . . ? O2A P1 O2B 30.6(11) . . ? O3A P1 O2B 126.7(12) . . ? O1B P1 O4 110.2(7) . . ? O2A P1 O4 106.0(6) . . ? O3A P1 O4 109.8(4) . . ? O2B P1 O4 117.7(12) . . ? O1B P1 O1A 42.9(12) . . ? O2A P1 O1A 109.9(5) . . ? O3A P1 O1A 110.1(5) . . ? O2B P1 O1A 79.4(12) . . ? O4 P1 O1A 105.9(4) . . ? O1B P1 O3B 106.2(14) . . ? O2A P1 O3B 77.2(8) . . ? O3A P1 O3B 40.1(6) . . ? O2B P1 O3B 99.3(12) . . ? O4 P1 O3B 109.4(7) . . ? O1A P1 O3B 140.3(8) . . ? P1 O1A Rb1 124.2(4) . . ? P1 O2B Rb1 121.1(15) . . ? O12 Rb1 O8 109.24(11) . . ? O12 Rb1 O10 108.39(11) . . ? O8 Rb1 O10 106.98(10) . . ? O12 Rb1 O5 91.11(13) . . ? O8 Rb1 O5 152.93(13) . . ? O10 Rb1 O5 82.01(13) . . ? O12 Rb1 O6 77.16(12) . . ? O8 Rb1 O6 98.80(12) . . ? O10 Rb1 O6 149.48(11) . . ? O5 Rb1 O6 67.73(14) . . ? O12 Rb1 O13 55.80(10) . . ? O8 Rb1 O13 54.74(10) . . ? O10 Rb1 O13 131.92(10) . . ? O5 Rb1 O13 136.25(13) . . ? O6 Rb1 O13 76.70(11) . . ? O12 Rb1 O1A 141.86(19) . . ? O8 Rb1 O1A 70.85(19) . . ? O10 Rb1 O1A 107.73(19) . . ? O5 Rb1 O1A 82.1(2) . . ? O6 Rb1 O1A 65.5(2) . . ? O13 Rb1 O1A 105.88(19) . . ? O12 Rb1 O11 55.18(11) . . ? O8 Rb1 O11 132.05(10) . . ? O10 Rb1 O11 54.46(10) . . ? O5 Rb1 O11 74.17(12) . . ? O6 Rb1 O11 117.05(11) . . ? O13 Rb1 O11 101.89(10) . . ? O1A Rb1 O11 151.73(18) . . ? O12 Rb1 O9 132.37(11) . . ? O8 Rb1 O9 53.68(10) . . ? O10 Rb1 O9 54.47(10) . . ? O5 Rb1 O9 123.69(13) . . ? O6 Rb1 O9 142.29(11) . . ? O13 Rb1 O9 100.02(10) . . ? O1A Rb1 O9 79.94(19) . . ? O11 Rb1 O9 100.49(10) . . ? O12 Rb1 O2B 120.8(5) . . ? O8 Rb1 O2B 105.0(5) . . ? O10 Rb1 O2B 105.6(5) . . ? O5 Rb1 O2B 48.1(5) . . ? O6 Rb1 O2B 50.7(5) . . ? O13 Rb1 O2B 121.6(5) . . ? O1A Rb1 O2B 35.2(5) . . ? O11 Rb1 O2B 122.0(5) . . ? O9 Rb1 O2B 106.8(5) . . ? O12 Rb1 C7 40.13(13) . . ? O8 Rb1 C7 141.83(13) . . ? O10 Rb1 C7 75.00(12) . . ? O5 Rb1 C7 64.76(14) . . ? O6 Rb1 C7 94.71(13) . . ? O13 Rb1 C7 94.73(13) . . ? O1A Rb1 C7 146.3(2) . . ? O11 Rb1 C7 22.52(12) . . ? O9 Rb1 C7 122.95(12) . . ? O2B Rb1 C7 111.1(5) . . ? O12 Rb1 C11 76.13(13) . . ? O8 Rb1 C11 40.15(12) . . ? O10 Rb1 C11 140.72(12) . . ? O5 Rb1 C11 137.26(14) . . ? O6 Rb1 C11 69.68(13) . . ? O13 Rb1 C11 22.48(12) . . ? O1A Rb1 C11 83.7(2) . . ? O11 Rb1 C11 124.30(12) . . ? O9 Rb1 C11 92.84(12) . . ? O2B Rb1 C11 104.5(5) . . ? C7 Rb1 C11 116.08(15) . . ? O8 C1 C2 109.7(5) . . ? O8 C1 H1A 109.7 . . ? C2 C1 H1A 109.7 . . ? O8 C1 H1B 109.7 . . ? C2 C1 H1B 109.7 . . ? H1A C1 H1B 108.2 . . ? O9 C2 C1 109.7(5) . . ? O9 C2 H2A 109.7 . . ? C1 C2 H2A 109.7 . . ? O9 C2 H2B 109.7 . . ? C1 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? O9 C3 C4 109.7(5) . . ? O9 C3 H3A 109.7 . . ? C4 C3 H3A 109.7 . . ? O9 C3 H3B 109.7 . . ? C4 C3 H3B 109.7 . . ? H3A C3 H3B 108.2 . . ? O10 C4 C3 109.3(5) . . ? O10 C4 H4A 109.8 . . ? C3 C4 H4A 109.8 . . ? O10 C4 H4B 109.8 . . ? C3 C4 H4B 109.8 . . ? H4A C4 H4B 108.3 . . ? O10 C5 C6 109.3(5) . . ? O10 C5 H5A 109.8 . . ? C6 C5 H5A 109.8 . . ? O10 C5 H5B 109.8 . . ? C6 C5 H5B 109.8 . . ? H5A C5 H5B 108.3 . . ? O11 C6 C5 109.2(5) . . ? O11 C6 H6A 109.8 . . ? C5 C6 H6A 109.8 . . ? O11 C6 H6B 109.8 . . ? C5 C6 H6B 109.8 . . ? H6A C6 H6B 108.3 . . ? O11 C7 C8 109.2(5) . . ? O11 C7 Rb1 58.0(3) . . ? C8 C7 Rb1 86.4(3) . . ? O11 C7 H7A 109.8 . . ? C8 C7 H7A 109.8 . . ? Rb1 C7 H7A 69.1 . . ? O11 C7 H7B 109.8 . . ? C8 C7 H7B 109.8 . . ? Rb1 C7 H7B 162.9 . . ? H7A C7 H7B 108.3 . . ? O12 C8 C7 108.4(5) . . ? O12 C8 H8A 110.0 . . ? C7 C8 H8A 110.0 . . ? O12 C8 H8B 110.0 . . ? C7 C8 H8B 110.0 . . ? H8A C8 H8B 108.4 . . ? O12 C9 C10 109.5(5) . . ? O12 C9 H9A 109.8 . . ? C10 C9 H9A 109.8 . . ? O12 C9 H9B 109.8 . . ? C10 C9 H9B 109.8 . . ? H9A C9 H9B 108.2 . . ? O13 C10 C9 110.0(5) . . ? O13 C10 Rb1 55.2(3) . . ? C9 C10 Rb1 84.7(4) . . ? O13 C10 H10A 109.7 . . ? C9 C10 H10A 109.7 . . ? Rb1 C10 H10A 163.0 . . ? O13 C10 H10B 109.7 . . ? C9 C10 H10B 109.7 . . ? Rb1 C10 H10B 73.9 . . ? H10A C10 H10B 108.2 . . ? O13 C11 C12 110.1(5) . . ? O13 C11 Rb1 57.7(3) . . ? C12 C11 Rb1 87.8(3) . . ? O13 C11 H11A 109.6 . . ? C12 C11 H11A 109.6 . . ? Rb1 C11 H11A 68.6 . . ? O13 C11 H11B 109.6 . . ? C12 C11 H11B 109.6 . . ? Rb1 C11 H11B 161.9 . . ? H11A C11 H11B 108.2 . . ? O8 C12 C11 109.6(5) . . ? O8 C12 H12A 109.7 . . ? C11 C12 H12A 109.7 . . ? O8 C12 H12B 109.7 . . ? C11 C12 H12B 109.7 . . ? H12A C12 H12B 108.2 . . ? C1 O8 C12 113.5(4) . . ? C1 O8 Rb1 124.9(3) . . ? C12 O8 Rb1 121.3(3) . . ? C3 O9 C2 111.7(4) . . ? C3 O9 Rb1 101.6(3) . . ? C2 O9 Rb1 101.8(3) . . ? C5 O10 C4 112.1(4) . . ? C5 O10 Rb1 121.9(3) . . ? C4 O10 Rb1 121.6(3) . . ? C6 O11 C7 113.1(4) . . ? C6 O11 Rb1 105.5(3) . . ? C7 O11 Rb1 99.5(3) . . ? C8 O12 C9 112.1(4) . . ? C8 O12 Rb1 123.1(3) . . ? C9 O12 Rb1 122.2(3) . . ? C11 O13 C10 112.6(4) . . ? C11 O13 Rb1 99.8(3) . . ? C10 O13 Rb1 102.9(3) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 21.98 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.403 _refine_diff_density_min -0.282 _refine_diff_density_rms 0.070 # Attachment '3_rev.CIF' data_3 _database_code_depnum_ccdc_archive 'CCDC 688382' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H31.50 Cs O13 P0.50 S0.50' _chemical_formula_weight 548.30 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' S S 0.1246 0.1234 '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 19.840(7) _cell_length_b 8.460(4) _cell_length_c 26.190(18) _cell_angle_alpha 90.00 _cell_angle_beta 101.14(6) _cell_angle_gamma 90.00 _cell_volume 4313(4) _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 ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.689 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2224 _exptl_absorpt_coefficient_mu 1.861 _exptl_absorpt_correction_type Psi-scan _exptl_absorpt_correction_T_min 0.648 _exptl_absorpt_correction_T_max 0.803 _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 3288 _diffrn_reflns_av_R_equivalents 0.0411 _diffrn_reflns_av_sigmaI/netI 0.0195 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.17 _diffrn_reflns_theta_max 24.99 _reflns_number_total 3196 _reflns_number_gt 2702 _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^)+(0.1636P)^2^+31.6815P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3196 _refine_ls_number_parameters 244 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0765 _refine_ls_R_factor_gt 0.0661 _refine_ls_wR_factor_ref 0.2168 _refine_ls_wR_factor_gt 0.2049 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _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 P1 P 0.91945(13) 1.1436(3) 0.50951(11) 0.0499(7) Uani 0.50 1 d P . . S1 S 0.91945(13) 1.1436(3) 0.50951(11) 0.0499(7) Uani 0.50 1 d P . . O1 O 0.9313(5) 1.0834(14) 0.4577(4) 0.093(3) Uani 1 1 d . . . O2 O 0.8490(5) 1.1256(16) 0.5096(5) 0.111(4) Uani 1 1 d . . . O3 O 0.9600(5) 1.0398(11) 0.5514(3) 0.080(2) Uani 1 1 d . . . O4 O 0.9436(9) 1.3042(12) 0.5155(6) 0.165(7) Uani 1 1 d . . . O5 O 0.8218(5) 0.7801(11) 0.5026(3) 0.088(3) Uani 1 1 d . . . O6 O 0.7143(5) 1.0936(11) 0.4506(4) 0.094(3) Uani 1 1 d . . . O7 O 0.9447(6) 1.6214(12) 0.5341(5) 0.100(3) Uani 1 1 d . . . Cs1 Cs 0.80162(3) 0.90032(6) 0.38562(2) 0.0400(3) Uani 1 1 d . . . O8 O 0.8785(3) 1.0324(7) 0.2929(2) 0.0419(14) Uani 1 1 d . . . C1 C 0.9470(5) 1.0165(12) 0.3202(4) 0.051(2) Uani 1 1 d . . . H1A H 0.9506 1.0565 0.3554 0.061 Uiso 1 1 calc R . . H1B H 0.9772 1.0786 0.3031 0.061 Uiso 1 1 calc R . . C2 C 0.9687(5) 0.8466(13) 0.3221(4) 0.052(2) Uani 1 1 d . . . H2A H 0.9633 0.8043 0.2871 0.062 Uiso 1 1 calc R . . H2B H 1.0166 0.8372 0.3388 0.062 Uiso 1 1 calc R . . O9 O 0.9270(3) 0.7625(7) 0.3506(3) 0.0451(15) Uani 1 1 d . . . C3 C 0.9475(5) 0.6035(10) 0.3591(4) 0.047(2) Uani 1 1 d . . . H3A H 0.9957 0.5981 0.3754 0.056 Uiso 1 1 calc R . . H3B H 0.9410 0.5471 0.3263 0.056 Uiso 1 1 calc R . . C4 C 0.9042(5) 0.5298(13) 0.3942(4) 0.055(3) Uani 1 1 d . . . H4A H 0.9200 0.4230 0.4031 0.067 Uiso 1 1 calc R . . H4B H 0.9089 0.5903 0.4262 0.067 Uiso 1 1 calc R . . O10 O 0.8343(3) 0.5267(7) 0.3688(2) 0.0423(14) Uani 1 1 d . . . C5 C 0.7932(5) 0.4559(11) 0.4010(4) 0.047(2) Uani 1 1 d . . . H5A H 0.8005 0.5085 0.4345 0.057 Uiso 1 1 calc R . . H5B H 0.8054 0.3454 0.4066 0.057 Uiso 1 1 calc R . . C6 C 0.7192(5) 0.4705(11) 0.3745(5) 0.054(3) Uani 1 1 d . . . H6A H 0.7135 0.4319 0.3391 0.064 Uiso 1 1 calc R . . H6B H 0.6907 0.4070 0.3927 0.064 Uiso 1 1 calc R . . O11 O 0.6986(3) 0.6315(8) 0.3743(3) 0.0504(17) Uani 1 1 d . . . C7 C 0.6286(5) 0.6517(12) 0.3544(4) 0.051(2) Uani 1 1 d . . . H7A H 0.6017 0.5981 0.3764 0.061 Uiso 1 1 calc R . . H7B H 0.6169 0.6071 0.3197 0.061 Uiso 1 1 calc R . . C8 C 0.6132(5) 0.8241(12) 0.3526(4) 0.051(2) Uani 1 1 d . . . H8A H 0.5639 0.8404 0.3430 0.061 Uiso 1 1 calc R . . H8B H 0.6290 0.8702 0.3868 0.061 Uiso 1 1 calc R . . O12 O 0.6460(3) 0.8981(6) 0.3162(3) 0.0431(15) Uani 1 1 d . . . C9 C 0.6308(5) 1.0640(11) 0.3105(4) 0.049(2) Uani 1 1 d . . . H9A H 0.6429 1.1161 0.3440 0.059 Uiso 1 1 calc R . . H9B H 0.5820 1.0790 0.2975 0.059 Uiso 1 1 calc R . . C10 C 0.6707(4) 1.1338(11) 0.2733(4) 0.043(2) Uani 1 1 d . . . H10A H 0.6634 1.0730 0.2414 0.051 Uiso 1 1 calc R . . H10B H 0.6559 1.2417 0.2650 0.051 Uiso 1 1 calc R . . O13 O 0.7410(3) 1.1310(7) 0.2974(2) 0.0425(15) Uani 1 1 d . . . C11 C 0.7840(5) 1.2009(11) 0.2648(4) 0.045(2) Uani 1 1 d . . . H11A H 0.7711 1.3106 0.2579 0.054 Uiso 1 1 calc R . . H11B H 0.7778 1.1454 0.2319 0.054 Uiso 1 1 calc R . . C12 C 0.8562(5) 1.1915(11) 0.2913(4) 0.048(2) Uani 1 1 d . . . H12A H 0.8843 1.2553 0.2728 0.057 Uiso 1 1 calc R . . H12B H 0.8610 1.2323 0.3264 0.057 Uiso 1 1 calc R . . 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 P1 0.0419(13) 0.0484(13) 0.0571(17) -0.0004(12) 0.0034(12) 0.0003(10) S1 0.0419(13) 0.0484(13) 0.0571(17) -0.0004(12) 0.0034(12) 0.0003(10) O1 0.074(6) 0.150(10) 0.053(6) 0.011(5) 0.012(5) 0.027(5) O2 0.046(5) 0.152(11) 0.137(11) 0.005(8) 0.022(6) 0.018(5) O3 0.090(6) 0.085(6) 0.068(5) 0.015(5) 0.022(5) 0.030(5) O4 0.243(17) 0.052(6) 0.160(12) -0.013(7) -0.056(11) -0.021(8) O5 0.115(7) 0.083(6) 0.066(6) 0.002(5) 0.020(5) -0.018(5) O6 0.082(6) 0.104(8) 0.094(8) -0.046(6) 0.009(6) 0.019(5) O7 0.115(9) 0.073(6) 0.106(9) 0.013(5) 0.012(7) -0.009(5) Cs1 0.0380(4) 0.0380(4) 0.0441(5) -0.0017(2) 0.0079(3) 0.00071(19) O8 0.036(3) 0.042(3) 0.047(4) -0.002(3) 0.006(3) -0.006(3) C1 0.036(4) 0.057(6) 0.060(6) -0.004(5) 0.009(4) -0.013(4) C2 0.032(4) 0.065(6) 0.058(6) -0.005(5) 0.008(4) -0.003(4) O9 0.037(3) 0.040(3) 0.060(4) 0.002(3) 0.014(3) 0.005(2) C3 0.038(5) 0.050(5) 0.051(6) 0.001(4) 0.005(5) 0.016(4) C4 0.052(5) 0.050(6) 0.059(7) 0.006(5) -0.003(5) 0.009(5) O10 0.047(3) 0.039(3) 0.038(3) 0.007(3) 0.003(3) 0.006(3) C5 0.059(6) 0.039(5) 0.044(6) 0.015(5) 0.009(5) 0.008(4) C6 0.063(6) 0.032(4) 0.075(7) -0.002(5) 0.036(5) -0.023(4) O11 0.044(4) 0.040(3) 0.068(5) -0.009(3) 0.013(3) -0.007(3) C7 0.037(5) 0.056(5) 0.065(7) 0.000(5) 0.021(5) -0.018(4) C8 0.035(4) 0.060(6) 0.060(6) -0.009(5) 0.017(5) -0.001(4) O12 0.039(3) 0.042(3) 0.052(4) -0.002(3) 0.017(3) 0.002(2) C9 0.039(5) 0.041(4) 0.065(7) -0.010(5) 0.003(5) 0.009(4) C10 0.036(4) 0.042(4) 0.047(6) 0.004(4) 0.001(4) 0.008(4) O13 0.044(3) 0.043(3) 0.039(4) 0.007(3) 0.007(3) 0.001(3) C11 0.054(5) 0.044(5) 0.039(5) 0.012(4) 0.012(4) -0.002(4) C12 0.050(5) 0.037(5) 0.056(6) 0.010(4) 0.011(5) -0.008(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 P1 O2 1.407(10) . ? P1 O4 1.439(11) . ? P1 O3 1.511(9) . ? P1 O1 1.511(10) . ? P1 Cs1 4.159(4) . ? O1 Cs1 3.272(11) . ? O2 Cs1 3.725(14) . ? O5 Cs1 3.179(9) . ? O6 Cs1 3.117(9) . ? Cs1 O11 3.033(6) . ? Cs1 O9 3.046(6) . ? Cs1 O13 3.086(6) . ? Cs1 O12 3.266(7) . ? Cs1 O10 3.273(6) . ? Cs1 O8 3.303(6) . ? Cs1 C4 3.720(10) . ? Cs1 C8 3.728(9) . ? O8 C1 1.414(11) . ? O8 C12 1.415(11) . ? C1 C2 1.499(15) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 O9 1.408(12) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? O9 C3 1.411(10) . ? C3 C4 1.507(15) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 O10 1.418(12) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? O10 C5 1.415(12) . ? C5 C6 1.501(15) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 O11 1.422(11) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? O11 C7 1.396(12) . ? C7 C8 1.489(14) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 O12 1.402(12) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? O12 C9 1.438(11) . ? C9 C10 1.490(15) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 O13 1.416(11) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? O13 C11 1.443(11) . ? C11 C12 1.467(13) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? 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 O2 P1 O4 114.4(9) . . ? O2 P1 O3 109.0(7) . . ? O4 P1 O3 110.5(7) . . ? O2 P1 O1 107.0(7) . . ? O4 P1 O1 108.0(9) . . ? O3 P1 O1 107.7(5) . . ? O2 P1 Cs1 62.5(6) . . ? O4 P1 Cs1 132.6(6) . . ? O3 P1 Cs1 114.8(4) . . ? O1 P1 Cs1 45.1(4) . . ? P1 O1 Cs1 115.9(5) . . ? P1 O2 Cs1 97.9(6) . . ? O11 Cs1 O9 104.94(17) . . ? O11 Cs1 O13 104.07(19) . . ? O9 Cs1 O13 103.83(18) . . ? O11 Cs1 O6 90.7(2) . . ? O9 Cs1 O6 159.8(2) . . ? O13 Cs1 O6 84.3(3) . . ? O11 Cs1 O5 79.1(2) . . ? O9 Cs1 O5 102.1(2) . . ? O13 Cs1 O5 151.9(2) . . ? O6 Cs1 O5 67.7(3) . . ? O11 Cs1 O12 52.74(17) . . ? O9 Cs1 O12 124.71(18) . . ? O13 Cs1 O12 52.93(16) . . ? O6 Cs1 O12 75.0(2) . . ? O5 Cs1 O12 117.6(2) . . ? O11 Cs1 O10 53.87(16) . . ? O9 Cs1 O10 52.78(15) . . ? O13 Cs1 O10 124.64(16) . . ? O6 Cs1 O10 136.5(2) . . ? O5 Cs1 O10 80.2(2) . . ? O12 Cs1 O10 96.32(14) . . ? O11 Cs1 O1 148.4(2) . . ? O9 Cs1 O1 76.0(2) . . ? O13 Cs1 O1 106.4(2) . . ? O6 Cs1 O1 84.0(3) . . ? O5 Cs1 O1 70.0(3) . . ? O12 Cs1 O1 151.3(2) . . ? O10 Cs1 O1 112.4(2) . . ? O11 Cs1 O8 125.44(18) . . ? O9 Cs1 O8 52.24(16) . . ? O13 Cs1 O8 53.38(16) . . ? O6 Cs1 O8 127.5(2) . . ? O5 Cs1 O8 145.8(2) . . ? O12 Cs1 O8 96.54(16) . . ? O10 Cs1 O8 95.51(15) . . ? O1 Cs1 O8 80.8(2) . . ? O11 Cs1 C4 74.0(2) . . ? O9 Cs1 C4 39.3(2) . . ? O13 Cs1 C4 135.0(2) . . ? O6 Cs1 C4 139.9(3) . . ? O5 Cs1 C4 73.0(3) . . ? O12 Cs1 C4 118.42(19) . . ? O10 Cs1 C4 22.23(19) . . ? O1 Cs1 C4 90.2(2) . . ? O8 Cs1 C4 90.3(2) . . ? O11 Cs1 O2 121.4(2) . . ? O9 Cs1 O2 112.0(2) . . ? O13 Cs1 O2 109.0(2) . . ? O6 Cs1 O2 47.8(2) . . ? O5 Cs1 O2 50.2(3) . . ? O12 Cs1 O2 122.70(19) . . ? O10 Cs1 O2 126.0(2) . . ? O1 Cs1 O2 38.5(2) . . ? O8 Cs1 O2 113.2(2) . . ? C4 Cs1 O2 109.6(2) . . ? O11 Cs1 C8 38.8(2) . . ? O9 Cs1 C8 134.9(2) . . ? O13 Cs1 C8 73.0(2) . . ? O6 Cs1 C8 65.1(2) . . ? O5 Cs1 C8 95.8(3) . . ? O12 Cs1 C8 21.9(2) . . ? O10 Cs1 C8 91.02(19) . . ? O1 Cs1 C8 149.0(2) . . ? O8 Cs1 C8 118.2(2) . . ? C4 Cs1 C8 112.4(2) . . ? O2 Cs1 C8 111.3(2) . . ? C1 O8 C12 111.7(7) . . ? C1 O8 Cs1 97.5(5) . . ? C12 O8 Cs1 99.0(5) . . ? O8 C1 C2 110.5(7) . . ? O8 C1 Cs1 60.6(4) . . ? C2 C1 Cs1 88.6(5) . . ? O8 C1 H1A 109.6 . . ? C2 C1 H1A 109.6 . . ? Cs1 C1 H1A 65.2 . . ? O8 C1 H1B 109.6 . . ? C2 C1 H1B 109.6 . . ? Cs1 C1 H1B 161.8 . . ? H1A C1 H1B 108.1 . . ? O9 C2 C1 107.9(7) . . ? O9 C2 H2A 110.1 . . ? C1 C2 H2A 110.1 . . ? O9 C2 H2B 110.1 . . ? C1 C2 H2B 110.1 . . ? H2A C2 H2B 108.4 . . ? C2 O9 C3 112.7(7) . . ? C2 O9 Cs1 124.3(5) . . ? C3 O9 Cs1 122.9(5) . . ? O9 C3 C4 108.1(8) . . ? O9 C3 H3A 110.1 . . ? C4 C3 H3A 110.1 . . ? O9 C3 H3B 110.1 . . ? C4 C3 H3B 110.1 . . ? H3A C3 H3B 108.4 . . ? O10 C4 C3 110.0(8) . . ? O10 C4 Cs1 60.9(4) . . ? C3 C4 Cs1 89.1(5) . . ? O10 C4 H4A 109.7 . . ? C3 C4 H4A 109.7 . . ? Cs1 C4 H4A 161.2 . . ? O10 C4 H4B 109.7 . . ? C3 C4 H4B 109.7 . . ? Cs1 C4 H4B 64.4 . . ? H4A C4 H4B 108.2 . . ? C5 O10 C4 110.7(7) . . ? C5 O10 Cs1 100.2(5) . . ? C4 O10 Cs1 96.9(5) . . ? O10 C5 C6 108.3(7) . . ? O10 C5 Cs1 58.3(4) . . ? C6 C5 Cs1 85.9(5) . . ? O10 C5 H5A 110.0 . . ? C6 C5 H5A 110.0 . . ? Cs1 C5 H5A 68.8 . . ? O10 C5 H5B 110.0 . . ? C6 C5 H3B 110.0 . . ? Cs1 C5 H5B 163.3 . . ? H5A C5 H5B 108.4 . . ? O11 C6 C5 109.6(7) . . ? O11 C6 H6A 109.7 . . ? C5 C6 H6A 109.7 . . ? O11 C6 H6B 109.7 . . ? C5 C6 H6B 109.7 . . ? H6A C6 H6B 108.2 . . ? C7 O11 C6 112.6(7) . . ? C7 O11 Cs1 123.2(5) . . ? C6 O11 Cs1 122.0(5) . . ? O11 C7 C8 108.4(7) . . ? O11 C7 H7A 110.0 . . ? C8 C7 H7A 110.0 . . ? O11 C7 H7B 110.0 . . ? C8 C7 H7B 110.0 . . ? H7A C7 H7B 108.4 . . ? O12 C8 C7 109.7(8) . . ? O12 C8 Cs1 60.2(4) . . ? C7 C8 Cs1 88.3(5) . . ? O12 C8 H8A 109.7 . . ? C7 C8 H8A 109.7 . . ? Cs1 C8 H8A 161.8 . . ? O12 C8 H8B 109.7 . . ? C7 C8 H8B 109.7 . . ? Cs1 C8 H8B 65.5 . . ? H8A C8 H8B 108.2 . . ? C8 O12 C9 113.0(7) . . ? C8 O12 Cs1 97.9(5) . . ? C9 O12 Cs1 102.1(5) . . ? O12 C9 C10 109.1(8) . . ? O12 C9 Cs1 56.4(4) . . ? C10 C9 Cs1 87.1(5) . . ? O12 C9 H9A 109.9 . . ? C10 C9 H9A 109.9 . . ? Cs1 C9 H9A 70.1 . . ? O12 C9 H9B 109.9 . . ? C10 C9 H9B 109.9 . . ? Cs1 C9 H9B 161.8 . . ? H9A C9 H9B 108.3 . . ? O13 C10 C9 107.8(8) . . ? O13 C10 H10A 110.1 . . ? C9 C10 H10A 110.1 . . ? O13 C10 H10B 110.1 . . ? C9 C10 H10B 110.1 . . ? H10A C10 H10B 108.5 . . ? C10 O13 C11 112.0(7) . . ? C10 O13 Cs1 123.5(5) . . ? C11 O13 Cs1 120.8(5) . . ? O13 C11 C12 109.5(7) . . ? O13 C11 H11A 109.8 . . ? C12 C11 H11A 109.8 . . ? O13 C11 H11B 109.8 . . ? C12 C11 H11B 109.8 . . ? H11A C11 H11B 108.2 . . ? O8 C12 C11 109.7(7) . . ? O8 C12 Cs1 59.3(4) . . ? C11 C12 Cs1 88.1(5) . . ? O8 C12 H12A 109.7 . . ? C11 C12 H12A 109.7 . . ? Cs1 C12 H12A 161.9 . . ? O8 C12 H12B 109.7 . . ? C11 C12 H12B 109.7 . . ? Cs1 C12 H12B 66.6 . . ? H12A C12 H12B 108.2 . . ? _diffrn_measured_fraction_theta_max 0.843 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.843 _refine_diff_density_max 2.274 _refine_diff_density_min -2.850 _refine_diff_density_rms 0.213 # Attachment '4_rev.CIF' data_4 _database_code_depnum_ccdc_archive 'CCDC 688383' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H58 Cs2 O24 S2' _chemical_formula_weight 1060.64 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.064(4) _cell_length_b 8.655(3) _cell_length_c 22.644(8) _cell_angle_alpha 90.00 _cell_angle_beta 100.907(6) _cell_angle_gamma 90.00 _cell_volume 2129.1(13) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.654 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1072 _exptl_absorpt_coefficient_mu 1.890 _exptl_absorpt_correction_type Psi-scan _exptl_absorpt_correction_T_min 0.598 _exptl_absorpt_correction_T_max 0.783 _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 16927 _diffrn_reflns_av_R_equivalents 0.0427 _diffrn_reflns_av_sigmaI/netI 0.0494 _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 -28 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 27.95 _reflns_number_total 4733 _reflns_number_gt 3460 _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^)+(0.0320P)^2^+2.6374P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4733 _refine_ls_number_parameters 262 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0524 _refine_ls_R_factor_gt 0.0333 _refine_ls_wR_factor_ref 0.0835 _refine_ls_wR_factor_gt 0.0762 _refine_ls_goodness_of_fit_ref 0.871 _refine_ls_restrained_S_all 0.871 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.001 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 S1 S 0.65541(9) -0.18609(13) 0.07504(5) 0.0611(3) Uani 1 1 d . . . O7 O 0.7481(3) -0.2986(4) 0.10040(18) 0.0966(11) Uani 1 1 d . . . O8A O 0.7074(6) -0.0958(7) 0.0331(3) 0.0922(17) Uani 0.70 1 d P . 1 O9A O 0.5661(6) -0.2871(11) 0.0298(5) 0.151(3) Uani 0.70 1 d P . 1 O10A O 0.5936(8) -0.1220(13) 0.1139(3) 0.140(4) Uani 0.70 1 d P . 1 O8B O 0.610(3) -0.178(2) 0.0134(6) 0.139(8) Uani 0.30 1 d P . 2 O9B O 0.5353(17) -0.209(2) 0.0856(13) 0.146(9) Uani 0.30 1 d P . 2 O10B O 0.7056(18) -0.0291(14) 0.0950(12) 0.167(9) Uani 0.30 1 d P . 2 O11 O 0.3339(3) -0.1981(4) -0.00527(15) 0.0895(10) Uani 1 1 d . . . O12 O 0.7211(3) 0.3884(4) 0.10296(16) 0.0894(10) Uani 1 1 d . . . Cs Cs 0.35772(2) 0.06103(3) 0.112957(10) 0.05116(9) Uani 1 1 d . . . O1 O 0.1054(2) -0.0811(3) 0.14869(11) 0.0548(6) Uani 1 1 d . . . C1 C 0.0202(4) -0.0656(5) 0.09344(19) 0.0690(11) Uani 1 1 d . . . H1A H -0.0535 -0.1249 0.0951 0.083 Uiso 1 1 calc R . . H1B H 0.0564 -0.1053 0.0607 0.083 Uiso 1 1 calc R . . C2 C -0.0120(3) 0.1000(5) 0.08287(19) 0.0675(11) Uani 1 1 d . . . H2A H -0.0758 0.1103 0.0473 0.081 Uiso 1 1 calc R . . H2B H -0.0433 0.1412 0.1169 0.081 Uiso 1 1 calc R . . O2 O 0.0931(2) 0.1834(3) 0.07515(13) 0.0661(7) Uani 1 1 d . . . C3 C 0.0710(4) 0.3419(5) 0.06105(19) 0.0687(11) Uani 1 1 d . . . H3A H 0.0375 0.3918 0.0928 0.082 Uiso 1 1 calc R . . H3B H 0.0113 0.3514 0.0239 0.082 Uiso 1 1 calc R . . C4 C 0.1872(4) 0.4180(5) 0.05452(19) 0.0668(11) Uani 1 1 d . . . H4A H 0.2231 0.3642 0.0244 0.080 Uiso 1 1 calc R . . H4B H 0.1707 0.5237 0.0412 0.080 Uiso 1 1 calc R . . O3 O 0.2712(2) 0.4168(3) 0.11031(12) 0.0577(6) Uani 1 1 d . . . C5 C 0.3831(4) 0.4990(5) 0.1073(2) 0.0662(11) Uani 1 1 d . . . H5A H 0.3645 0.6062 0.0968 0.079 Uiso 1 1 calc R . . H5B H 0.4223 0.4537 0.0766 0.079 Uiso 1 1 calc R . . C6 C 0.4676(4) 0.4905(5) 0.1667(2) 0.0663(11) Uani 1 1 d . . . H6A H 0.5334 0.5653 0.1683 0.080 Uiso 1 1 calc R . . H6B H 0.4229 0.5146 0.1985 0.080 Uiso 1 1 calc R . . O4 O 0.5181(2) 0.3381(3) 0.17529(12) 0.0568(6) Uani 1 1 d . . . C7 C 0.5918(3) 0.3163(5) 0.23377(18) 0.0604(10) Uani 1 1 d . . . H7A H 0.5465 0.3496 0.2642 0.073 Uiso 1 1 calc R . . H7B H 0.6660 0.3782 0.2378 0.073 Uiso 1 1 calc R . . C8 C 0.6253(3) 0.1494(5) 0.24284(18) 0.0583(10) Uani 1 1 d . . . H8A H 0.6615 0.1123 0.2097 0.070 Uiso 1 1 calc R . . H8B H 0.6852 0.1364 0.2798 0.070 Uiso 1 1 calc R . . O5 O 0.5168(2) 0.0638(3) 0.24594(11) 0.0516(6) Uani 1 1 d . . . C9 C 0.5409(4) -0.0961(4) 0.25955(18) 0.0588(10) Uani 1 1 d . . . H9A H 0.6035 -0.1057 0.2956 0.071 Uiso 1 1 calc R . . H9B H 0.5711 -0.1455 0.2267 0.071 Uiso 1 1 calc R . . C10 C 0.4264(4) -0.1726(5) 0.26867(17) 0.0592(9) Uani 1 1 d . . . H10A H 0.4446 -0.2767 0.2835 0.071 Uiso 1 1 calc R . . H10B H 0.3914 -0.1161 0.2984 0.071 Uiso 1 1 calc R . . O6 O 0.3402(2) -0.1776(3) 0.21342(11) 0.0522(6) Uani 1 1 d . . . C11 C 0.2256(3) -0.2458(4) 0.22018(19) 0.0586(10) Uani 1 1 d . . . H11A H 0.1919 -0.1909 0.2507 0.070 Uiso 1 1 calc R . . H11B H 0.2383 -0.3527 0.2326 0.070 Uiso 1 1 calc R . . C12 C 0.1387(4) -0.2371(4) 0.16153(19) 0.0591(10) Uani 1 1 d . . . H12A H 0.1773 -0.2790 0.1300 0.071 Uiso 1 1 calc R . . H12B H 0.0657 -0.2978 0.1633 0.071 Uiso 1 1 calc R . . 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 S1 0.0567(5) 0.0658(6) 0.0627(6) 0.0132(5) 0.0162(4) 0.0011(5) O7 0.086(2) 0.086(2) 0.109(3) 0.028(2) -0.0038(19) 0.0094(19) O8A 0.114(4) 0.081(4) 0.094(4) 0.025(3) 0.051(3) 0.003(3) O9A 0.087(4) 0.155(7) 0.194(9) -0.063(7) -0.019(5) 0.014(5) O10A 0.138(7) 0.206(10) 0.086(4) -0.031(5) 0.048(4) 0.067(7) O8B 0.26(3) 0.111(14) 0.049(7) 0.023(9) 0.033(11) 0.048(15) O9B 0.118(14) 0.109(14) 0.25(3) 0.055(15) 0.123(17) 0.016(10) O10B 0.151(14) 0.048(8) 0.26(2) -0.015(10) -0.070(15) -0.026(8) O11 0.099(2) 0.080(2) 0.083(2) 0.0067(18) 0.0025(18) -0.0013(19) O12 0.090(2) 0.087(2) 0.088(2) -0.0072(19) 0.0088(18) -0.0007(18) Cs 0.05688(14) 0.04978(14) 0.04639(14) 0.00166(10) 0.00869(9) 0.00374(10) O1 0.0562(14) 0.0538(16) 0.0528(15) -0.0040(12) 0.0063(11) -0.0013(11) C1 0.063(2) 0.083(3) 0.056(2) -0.009(2) -0.0017(18) -0.013(2) C2 0.050(2) 0.092(3) 0.055(2) 0.001(2) -0.0046(17) 0.005(2) O2 0.0565(14) 0.0664(17) 0.0724(18) 0.0139(15) 0.0047(13) 0.0105(13) C3 0.073(3) 0.072(3) 0.054(2) 0.004(2) -0.0078(19) 0.021(2) C4 0.088(3) 0.051(2) 0.059(2) 0.0144(19) 0.009(2) 0.019(2) O3 0.0623(15) 0.0545(15) 0.0563(15) 0.0130(12) 0.0109(12) 0.0051(12) C5 0.077(3) 0.046(2) 0.083(3) 0.019(2) 0.032(2) 0.0070(19) C6 0.068(2) 0.041(2) 0.093(3) 0.001(2) 0.024(2) -0.0017(18) O4 0.0628(14) 0.0463(14) 0.0614(16) -0.0049(12) 0.0118(12) -0.0011(11) C7 0.0494(19) 0.066(2) 0.066(2) -0.010(2) 0.0094(17) -0.0129(18) C8 0.0427(18) 0.070(3) 0.059(2) -0.0008(19) 0.0026(16) 0.0008(17) O5 0.0450(12) 0.0502(14) 0.0574(15) -0.0023(12) 0.0041(10) 0.0036(11) C9 0.062(2) 0.055(2) 0.054(2) 0.0045(17) -0.0038(17) 0.0155(17) C10 0.076(2) 0.055(2) 0.045(2) 0.0058(17) 0.0084(18) 0.0084(19) O6 0.0582(13) 0.0529(14) 0.0461(13) 0.0071(11) 0.0112(11) -0.0004(12) C11 0.064(2) 0.047(2) 0.070(3) 0.0097(18) 0.027(2) -0.0007(17) C12 0.061(2) 0.050(2) 0.070(3) -0.0070(18) 0.0207(19) -0.0063(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 S1 O10A 1.333(6) . ? S1 O8B 1.393(15) . ? S1 O9B 1.408(15) . ? S1 O8A 1.433(5) . ? S1 O7 1.452(3) . ? S1 O10B 1.505(12) . ? S1 O9A 1.551(7) . ? S1 Cs 4.1508(15) . ? O8A Cs 3.262(7) 3_655 ? O10A Cs 3.049(7) . ? O8B Cs 3.117(15) 3_655 ? O9B Cs 3.189(18) . ? O11 Cs 3.464(4) . ? Cs O2 3.079(3) . ? Cs O8B 3.117(15) 3_655 ? Cs O6 3.106(2) . ? Cs O4 3.153(3) . ? Cs O5 3.188(3) . ? Cs O3 3.222(3) . ? Cs O8A 3.262(7) 3_655 ? Cs O1 3.289(3) . ? Cs C4 3.729(4) . ? O1 C12 1.415(4) . ? O1 C1 1.423(5) . ? C1 C2 1.485(6) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 O2 1.407(5) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? O2 C3 1.419(5) . ? C3 C4 1.477(6) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 O3 1.420(5) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? O3 C5 1.440(5) . ? C5 C6 1.486(6) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 O4 1.431(5) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? O4 C7 1.430(4) . ? C7 C8 1.496(6) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 O5 1.424(4) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? O5 C9 1.432(4) . ? C9 C10 1.478(6) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 O6 1.423(4) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? O6 C11 1.432(4) . ? C11 C12 1.487(6) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? 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 O10A S1 O8B 120.6(10) . . ? O10A S1 O9B 47.8(10) . . ? O8B S1 O9B 90.3(16) . . ? O10A S1 O8A 122.1(6) . . ? O8B S1 O8A 54.6(11) . . ? O9B S1 O8A 134.4(9) . . ? O10A S1 O7 115.5(4) . . ? O8B S1 O7 121.6(8) . . ? O9B S1 O7 117.2(8) . . ? O8A S1 O7 106.6(3) . . ? O10A S1 O10B 68.4(11) . . ? O8B S1 O10B 107.3(13) . . ? O9B S1 O10B 112.6(13) . . ? O8A S1 O10B 62.3(11) . . ? O7 S1 O10B 107.1(6) . . ? O10A S1 O9A 109.2(5) . . ? O8B S1 O9A 45.9(10) . . ? O9B S1 O9A 61.9(11) . . ? O8A S1 O9A 98.9(5) . . ? O7 S1 O9A 101.3(4) . . ? O10B S1 O9A 149.3(8) . . ? O10A S1 Cs 28.7(4) . . ? O8B S1 Cs 91.9(9) . . ? O9B S1 Cs 39.3(8) . . ? O8A S1 Cs 106.9(2) . . ? O7 S1 Cs 142.45(17) . . ? O10B S1 Cs 74.6(9) . . ? O9A S1 Cs 89.8(3) . . ? S1 O8A Cs 133.1(4) . 3_655 ? S1 O10A Cs 139.2(5) . . ? S1 O8B Cs 148.7(18) . 3_655 ? S1 O9B Cs 124.4(11) . . ? O10A Cs O2 161.49(17) . . ? O10A Cs O8B 85.9(4) . 3_655 ? O2 Cs O8B 84.3(5) . 3_655 ? O10A Cs O6 79.7(2) . . ? O2 Cs O6 104.15(7) . . ? O8B Cs O6 157.2(4) 3_655 . ? O10A Cs O4 89.1(2) . . ? O2 Cs O4 106.73(7) . . ? O8B Cs O4 90.7(5) 3_655 . ? O6 Cs O4 106.60(7) . . ? O10A Cs O5 71.25(14) . . ? O2 Cs O5 125.88(7) . . ? O8B Cs O5 136.6(6) 3_655 . ? O6 Cs O5 54.05(6) . . ? O4 Cs O5 53.70(6) . . ? O10A Cs O9B 20.4(4) . . ? O2 Cs O9B 141.9(5) . . ? O8B Cs O9B 83.0(5) 3_655 . ? O6 Cs O9B 77.3(3) . . ? O4 Cs O9B 109.2(4) . . ? O5 Cs O9B 86.5(5) . . ? O10A Cs O3 138.4(2) . . ? O2 Cs O3 53.30(7) . . ? O8B Cs O3 76.0(3) 3_655 . ? O6 Cs O3 126.13(7) . . ? O4 Cs O3 54.66(7) . . ? O5 Cs O3 96.85(6) . . ? O9B Cs O3 152.7(3) . . ? O10A Cs O8A 94.57(17) . 3_655 ? O2 Cs O8A 70.75(11) . 3_655 ? O8B Cs O8A 23.3(5) 3_655 3_655 ? O6 Cs O8A 140.48(13) . 3_655 ? O4 Cs O8A 112.41(13) . 3_655 ? O5 Cs O8A 158.98(12) . 3_655 ? O9B Cs O8A 84.1(5) . 3_655 ? O3 Cs O8A 83.41(12) . 3_655 ? O10A Cs O1 124.7(2) . . ? O2 Cs O1 52.43(7) . . ? O8B Cs O1 126.6(6) 3_655 . ? O6 Cs O1 52.94(6) . . ? O4 Cs O1 127.33(7) . . ? O5 Cs O1 96.49(6) . . ? O9B Cs O1 110.9(3) . . ? O3 Cs O1 95.69(7) . . ? O8A Cs O1 104.41(12) 3_655 . ? O10A Cs O11 66.98(17) . . ? O2 Cs O11 94.51(8) . . ? O8B Cs O11 60.4(4) 3_655 . ? O6 Cs O11 97.43(8) . . ? O4 Cs O11 142.41(8) . . ? O5 Cs O11 133.05(7) . . ? O9B Cs O11 48.3(5) . . ? O3 Cs O11 128.73(7) . . ? O8A Cs O11 46.09(13) 3_655 . ? O1 Cs O11 90.22(7) . . ? O10A Cs C4 143.9(2) . . ? O2 Cs C4 39.26(9) . . ? O8B Cs C4 62.8(3) 3_655 . ? O6 Cs C4 135.49(9) . . ? O4 Cs C4 74.52(9) . . ? O5 Cs C4 118.73(8) . . ? O9B Cs C4 145.8(4) . . ? O3 Cs C4 22.05(8) . . ? O8A Cs C4 64.16(13) 3_655 . ? O1 Cs C4 90.07(9) . . ? O11 Cs C4 107.62(9) . . ? C12 O1 C1 112.0(3) . . ? C12 O1 Cs 102.0(2) . . ? C1 O1 Cs 101.6(2) . . ? O1 C1 C2 109.3(3) . . ? O1 C1 Cs 57.13(19) . . ? C2 C1 Cs 86.6(2) . . ? O1 C1 H1A 109.8 . . ? C2 C1 H1A 109.8 . . ? Cs C1 H1A 162.5 . . ? O1 C1 H1B 109.8 . . ? C2 C1 H1B 109.8 . . ? Cs C1 H1B 69.9 . . ? H1A C1 H1B 108.3 . . ? O2 C2 C1 109.7(3) . . ? O2 C2 H2A 109.7 . . ? C1 C2 H2A 109.7 . . ? O2 C2 H2B 109.7 . . ? C1 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? C2 O2 C3 114.4(3) . . ? C2 O2 Cs 123.6(2) . . ? C3 O2 Cs 120.6(2) . . ? O2 C3 C4 109.7(3) . . ? O2 C3 H3A 109.7 . . ? C4 C3 H3A 109.7 . . ? O2 C3 H3B 109.7 . . ? C4 C3 H3B 109.7 . . ? H3A C3 H3B 108.2 . . ? O3 C4 C3 110.1(3) . . ? O3 C4 Cs 58.44(17) . . ? C3 C4 Cs 89.2(2) . . ? O3 C4 H4A 109.6 . . ? C3 C4 H4A 109.6 . . ? Cs C4 H4A 66.8 . . ? O3 C4 H4B 109.6 . . ? C3 C4 H4B 109.6 . . ? Cs C4 H4B 160.8 . . ? H4A C4 H4B 108.2 . . ? C4 O3 C5 112.3(3) . . ? C4 O3 Cs 99.5(2) . . ? C5 O3 Cs 102.6(2) . . ? O3 C5 C6 109.4(3) . . ? O3 C5 Cs 55.74(18) . . ? C6 C5 Cs 87.6(2) . . ? O3 C5 H5A 109.8 . . ? C6 C5 H5A 109.8 . . ? Cs C5 H5A 161.2 . . ? O3 C5 H5B 109.8 . . ? C6 C5 H5B 109.8 . . ? Cs C5 H5B 70.5 . . ? H5A C5 H5B 108.2 . . ? O4 C6 C5 109.3(4) . . ? 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 . . ? C6 O4 C7 112.8(3) . . ? C6 O4 Cs 117.9(2) . . ? C7 O4 Cs 119.2(2) . . ? O4 C7 C8 109.7(3) . . ? O4 C7 H7A 109.7 . . ? C8 C7 H7A 109.7 . . ? O4 C7 H7B 109.7 . . ? C8 C7 H7B 109.7 . . ? H7A C7 H7B 108.2 . . ? O5 C8 C7 108.6(3) . . ? O5 C8 Cs 53.00(16) . . ? C7 C8 Cs 87.3(2) . . ? O5 C8 H8A 110.0 . . ? C7 C8 H8A 110.0 . . ? Cs C8 H8A 73.3 . . ? O5 C8 H8B 110.0 . . ? C7 C8 H8B 110.0 . . ? Cs C8 H8B 160.1 . . ? H8A C8 H8B 108.3 . . ? C8 O5 C9 112.9(3) . . ? C8 O5 Cs 106.1(2) . . ? C9 O5 Cs 104.05(19) . . ? O5 C9 C10 109.5(3) . . ? O5 C9 Cs 54.50(16) . . ? C10 C9 Cs 87.3(2) . . ? O5 C9 H9A 109.8 . . ? C10 C9 H9A 109.8 . . ? Cs C9 H9A 160.9 . . ? O5 C9 H9B 109.8 . . ? C10 C9 H9B 109.8 . . ? Cs C9 H9B 72.1 . . ? H9A C9 H9B 108.2 . . ? O6 C10 C9 109.9(3) . . ? O6 C10 H10A 109.7 . . ? C9 C10 H10A 109.7 . . ? O6 C10 H10B 109.7 . . ? C9 C10 H10B 109.7 . . ? H10A C10 H10B 108.2 . . ? C10 O6 C11 112.2(3) . . ? C10 O6 Cs 120.0(2) . . ? C11 O6 Cs 122.1(2) . . ? O6 C11 C12 108.6(3) . . ? O6 C11 H11A 110.0 . . ? C12 C11 H11A 110.0 . . ? O6 C11 H11B 110.0 . . ? C12 C11 H11B 110.0 . . ? H11A C11 H11B 108.3 . . ? O1 C12 C11 109.3(3) . . ? O1 C12 Cs 56.89(17) . . ? C11 C12 Cs 87.3(2) . . ? O1 C12 H12A 109.8 . . ? C11 C12 H12A 109.8 . . ? Cs C12 H12A 69.5 . . ? O1 C12 H12B 109.8 . . ? C11 C12 H12B 109.8 . . ? Cs C12 H12B 161.9 . . ? H12A C12 H12B 108.3 . . ? _diffrn_measured_fraction_theta_max 0.924 _diffrn_reflns_theta_full 27.95 _diffrn_measured_fraction_theta_full 0.924 _refine_diff_density_max 0.775 _refine_diff_density_min -0.499 _refine_diff_density_rms 0.074