# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_1 _database_code_depnum_ccdc_archive 'CCDC 898797' #TrackingRef 'Cs4Mo5P2O22.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Cs4 Mo5 O22 P2' _chemical_formula_weight 1425.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 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' Mo Mo -1.6832 0.6857 '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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M C222(1) _symmetry_space_group_name_Hall C2c2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 6.622(5) _cell_length_b 20.485(15) _cell_length_c 17.748(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2408(3) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2270 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 27.02 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.165 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.047 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.932 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2544 _exptl_absorpt_coefficient_mu 8.715 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.3025 _exptl_absorpt_correction_T_max 0.7024 _exptl_absorpt_process_details Face-indexed _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7424 _diffrn_reflns_av_R_equivalents 0.0406 _diffrn_reflns_av_sigmaI/netI 0.0543 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 27.77 _reflns_number_total 2833 _reflns_number_gt 2505 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens ? _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.000134(17) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881, 1213 Friedel pairs' _chemical_absolute_configuration ad _refine_ls_abs_structure_Flack 0.03(2) _refine_ls_number_reflns 2833 _refine_ls_number_parameters 153 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0383 _refine_ls_R_factor_gt 0.0314 _refine_ls_wR_factor_ref 0.0503 _refine_ls_wR_factor_gt 0.0483 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _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 Cs1 Cs 0.5000 0.59109(2) 0.2500 0.02749(15) Uani 1 2 d S . . Cs2 Cs 0.01274(9) 0.73355(2) 0.09925(3) 0.03774(14) Uani 1 1 d . . . Cs3 Cs 0.52953(14) 0.5000 0.0000 0.0430(2) Uani 1 2 d S . . Mo1 Mo -0.00938(12) 0.52575(2) 0.14517(3) 0.01826(13) Uani 1 1 d . . . Mo2 Mo 0.0000 0.27314(3) 0.2500 0.01617(17) Uani 1 2 d S . . Mo3 Mo 0.05649(10) 0.36679(3) 0.09466(3) 0.02041(15) Uani 1 1 d . . . P1 P 0.2815(3) 0.41381(8) 0.26342(10) 0.0150(4) Uani 1 1 d . . . O1 O 0.5000 0.3830(2) 0.2500 0.0211(14) Uani 1 2 d S . . O2 O 0.2997(8) 0.4735(2) 0.3118(3) 0.0207(11) Uani 1 1 d . . . O3 O 0.1924(8) 0.4298(2) 0.1863(2) 0.0176(11) Uani 1 1 d . . . O4 O -0.1760(8) 0.2211(2) 0.2148(3) 0.0268(13) Uani 1 1 d . . . O5 O 0.1459(8) 0.2987(2) 0.1620(2) 0.0211(12) Uani 1 1 d . . . O6 O 0.2177(8) 0.5574(3) 0.1186(3) 0.0288(14) Uani 1 1 d . . . O7 O 0.0000 0.5457(2) 0.2500 0.0203(14) Uani 1 2 d S . . O8 O -0.1741(9) 0.5818(2) 0.1112(3) 0.0280(13) Uani 1 1 d . . . O9 O 0.2616(8) 0.3636(3) 0.0379(3) 0.0331(14) Uani 1 1 d . . . O10 O -0.0366(8) 0.45440(18) 0.0772(2) 0.0216(12) Uani 1 1 d . . . O11 O -0.1237(9) 0.3254(2) 0.0451(3) 0.0310(14) Uani 1 1 d . . . O12 O 0.1682(7) 0.3582(2) 0.3023(2) 0.0157(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 Cs1 0.0255(4) 0.0151(3) 0.0418(4) 0.000 -0.0017(4) 0.000 Cs2 0.0277(3) 0.0539(3) 0.0316(3) -0.0091(2) -0.0072(3) 0.0060(3) Cs3 0.0308(5) 0.0605(5) 0.0378(4) -0.0130(3) 0.000 0.000 Mo1 0.0203(3) 0.0174(3) 0.0171(3) 0.0025(2) 0.0003(3) -0.0008(3) Mo2 0.0176(4) 0.0118(3) 0.0191(4) 0.000 -0.0022(4) 0.000 Mo3 0.0253(4) 0.0198(3) 0.0162(3) -0.0018(2) 0.0026(3) 0.0018(3) P1 0.0116(9) 0.0142(8) 0.0192(12) 0.0019(7) -0.0011(7) -0.0005(7) O1 0.013(3) 0.013(3) 0.037(4) 0.000 0.006(4) 0.000 O2 0.024(3) 0.014(2) 0.024(3) -0.003(2) -0.004(2) -0.003(2) O3 0.021(3) 0.017(3) 0.014(3) 0.002(2) -0.002(2) -0.001(2) O4 0.030(3) 0.019(3) 0.032(3) -0.001(2) -0.009(2) -0.001(2) O5 0.024(3) 0.018(3) 0.021(3) -0.003(2) 0.005(2) 0.007(2) O6 0.029(3) 0.026(3) 0.031(3) 0.005(2) 0.007(2) -0.005(3) O7 0.029(4) 0.015(3) 0.017(3) 0.000 -0.005(4) 0.000 O8 0.033(3) 0.023(3) 0.027(3) 0.006(2) -0.007(3) 0.002(2) O9 0.037(4) 0.032(3) 0.030(3) 0.003(3) 0.013(3) 0.008(3) O10 0.029(3) 0.020(2) 0.015(2) 0.0006(18) -0.003(2) -0.001(2) O11 0.043(4) 0.026(3) 0.024(3) -0.008(2) 0.002(3) -0.002(3) O12 0.015(3) 0.015(2) 0.017(2) -0.001(2) 0.002(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 Cs1 O2 2.960(5) . ? Cs1 O2 2.960(5) 3_655 ? Cs1 O4 2.973(5) 7 ? Cs1 O4 2.973(5) 5 ? Cs1 O6 3.068(6) . ? Cs1 O6 3.068(6) 3_655 ? Cs1 O8 3.280(6) 1_655 ? Cs1 O8 3.280(6) 3 ? Cs1 O7 3.439(3) 1_655 ? Cs1 O7 3.439(3) . ? Cs2 O4 2.918(5) 5 ? Cs2 O11 2.972(5) 4_565 ? Cs2 O5 2.987(5) 5_455 ? Cs2 O11 3.203(6) 5 ? Cs2 O9 3.324(6) 5_455 ? Cs2 O8 3.353(6) . ? Cs3 O6 3.174(6) 4_565 ? Cs3 O6 3.174(6) . ? Cs3 O8 3.249(6) 1_655 ? Cs3 O8 3.249(6) 4_665 ? Cs3 O10 3.318(5) 1_655 ? Cs3 O10 3.318(5) 4_665 ? Cs3 O9 3.378(6) 4_565 ? Cs3 O9 3.378(6) . ? Mo1 O8 1.694(5) . ? Mo1 O6 1.704(6) . ? Mo1 O10 1.903(4) . ? Mo1 O7 1.9059(17) . ? Mo1 O2 2.328(5) 3 ? Mo1 O3 2.485(5) . ? Mo2 O4 1.699(5) . ? Mo2 O4 1.699(5) 3 ? Mo2 O5 1.910(5) 3 ? Mo2 O5 1.910(5) . ? Mo2 O12 2.267(5) 3 ? Mo2 O12 2.267(5) . ? Mo3 O9 1.692(5) . ? Mo3 O11 1.708(5) . ? Mo3 O10 1.923(4) . ? Mo3 O5 1.930(5) . ? Mo3 O3 2.263(5) . ? Mo3 O12 2.364(4) 3 ? P1 O2 1.500(5) . ? P1 O3 1.526(5) . ? P1 O12 1.529(5) . ? P1 O1 1.597(3) . ? O1 P1 1.597(3) 3_655 ? O2 Mo1 2.328(5) 3 ? O4 Cs2 2.918(5) 5_445 ? O4 Cs1 2.973(5) 5_445 ? O5 Cs2 2.987(5) 5_545 ? O7 Mo1 1.9059(17) 3 ? O7 Cs1 3.439(3) 1_455 ? O8 Cs3 3.249(5) 1_455 ? O8 Cs1 3.280(6) 1_455 ? O9 Cs2 3.324(6) 5_545 ? O10 Cs3 3.318(5) 1_455 ? O11 Cs2 2.972(5) 4_565 ? O11 Cs2 3.203(6) 5_445 ? O12 Mo3 2.364(4) 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 O2 Cs1 O2 71.12(19) . 3_655 ? O2 Cs1 O4 145.73(13) . 7 ? O2 Cs1 O4 129.11(14) 3_655 7 ? O2 Cs1 O4 129.11(14) . 5 ? O2 Cs1 O4 145.73(13) 3_655 5 ? O4 Cs1 O4 52.83(19) 7 5 ? O2 Cs1 O6 79.95(14) . . ? O2 Cs1 O6 78.93(14) 3_655 . ? O4 Cs1 O6 126.90(13) 7 . ? O4 Cs1 O6 78.64(14) 5 . ? O2 Cs1 O6 78.93(14) . 3_655 ? O2 Cs1 O6 79.95(14) 3_655 3_655 ? O4 Cs1 O6 78.64(14) 7 3_655 ? O4 Cs1 O6 126.90(13) 5 3_655 ? O6 Cs1 O6 154.0(2) . 3_655 ? O2 Cs1 O8 121.73(13) . 1_655 ? O2 Cs1 O8 51.65(13) 3_655 1_655 ? O4 Cs1 O8 87.24(14) 7 1_655 ? O4 Cs1 O8 98.76(13) 5 1_655 ? O6 Cs1 O8 79.46(13) . 1_655 ? O6 Cs1 O8 99.02(13) 3_655 1_655 ? O2 Cs1 O8 51.65(13) . 3 ? O2 Cs1 O8 121.73(13) 3_655 3 ? O4 Cs1 O8 98.76(13) 7 3 ? O4 Cs1 O8 87.24(14) 5 3 ? O6 Cs1 O8 99.02(13) . 3 ? O6 Cs1 O8 79.45(13) 3_655 3 ? O8 Cs1 O8 173.33(18) 1_655 3 ? O2 Cs1 O7 102.21(13) . 1_655 ? O2 Cs1 O7 49.35(12) 3_655 1_655 ? O4 Cs1 O7 82.23(13) 7 1_655 ? O4 Cs1 O7 128.29(13) 5 1_655 ? O6 Cs1 O7 121.72(11) . 1_655 ? O6 Cs1 O7 49.64(10) 3_655 1_655 ? O8 Cs1 O7 49.52(10) 1_655 1_655 ? O8 Cs1 O7 128.15(10) 3 1_655 ? O2 Cs1 O7 49.35(12) . . ? O2 Cs1 O7 102.21(13) 3_655 . ? O4 Cs1 O7 128.29(13) 7 . ? O4 Cs1 O7 82.23(13) 5 . ? O6 Cs1 O7 49.64(10) . . ? O6 Cs1 O7 121.71(11) 3_655 . ? O8 Cs1 O7 128.15(10) 1_655 . ? O8 Cs1 O7 49.52(10) 3 . ? O7 Cs1 O7 148.62(16) 1_655 . ? O2 Cs1 Mo2 144.44(10) . 5 ? O2 Cs1 Mo2 144.44(10) 3_655 5 ? O4 Cs1 Mo2 26.42(10) 7 5 ? O4 Cs1 Mo2 26.42(10) 5 5 ? O6 Cs1 Mo2 103.02(10) . 5 ? O6 Cs1 Mo2 103.02(10) 3_655 5 ? O8 Cs1 Mo2 93.33(9) 1_655 5 ? O8 Cs1 Mo2 93.33(9) 3 5 ? O7 Cs1 Mo2 105.69(8) 1_655 5 ? O7 Cs1 Mo2 105.69(8) . 5 ? O2 Cs1 P1 55.51(11) . 3_655 ? O2 Cs1 P1 19.54(9) 3_655 3_655 ? O4 Cs1 P1 134.29(11) 7 3_655 ? O4 Cs1 P1 164.27(9) 5 3_655 ? O6 Cs1 P1 88.29(11) . 3_655 ? O6 Cs1 P1 67.18(10) 3_655 3_655 ? O8 Cs1 P1 69.96(9) 1_655 3_655 ? O8 Cs1 P1 103.58(9) 3 3_655 ? O7 Cs1 P1 52.66(8) 1_655 3_655 ? O7 Cs1 P1 96.02(9) . 3_655 ? Mo2 Cs1 P1 158.01(3) 5 3_655 ? O4 Cs2 O11 141.67(14) 5 4_565 ? O4 Cs2 O5 110.58(14) 5 5_455 ? O11 Cs2 O5 104.81(14) 4_565 5_455 ? O4 Cs2 O11 74.43(14) 5 5 ? O11 Cs2 O11 102.03(11) 4_565 5 ? O5 Cs2 O11 117.45(14) 5_455 5 ? O4 Cs2 O9 130.81(14) 5 5_455 ? O11 Cs2 O9 83.77(14) 4_565 5_455 ? O5 Cs2 O9 49.99(12) 5_455 5_455 ? O11 Cs2 O9 78.87(15) 5 5_455 ? O4 Cs2 O8 97.74(13) 5 . ? O11 Cs2 O8 64.27(14) 4_565 . ? O5 Cs2 O8 95.18(14) 5_455 . ? O11 Cs2 O8 147.25(13) 5 . ? O9 Cs2 O8 125.41(15) 5_455 . ? O4 Cs2 O9 96.03(14) 5 4_565 ? O11 Cs2 O9 47.33(14) 4_565 4_565 ? O5 Cs2 O9 152.07(12) 5_455 4_565 ? O11 Cs2 O9 76.98(13) 5 4_565 ? O9 Cs2 O9 117.20(9) 5_455 4_565 ? O8 Cs2 O9 72.24(14) . 4_565 ? O4 Cs2 O12 48.22(12) 5 7 ? O11 Cs2 O12 148.23(12) 4_565 7 ? O5 Cs2 O12 88.88(13) 5_455 7 ? O11 Cs2 O12 46.84(11) 5 7 ? O9 Cs2 O12 83.60(13) 5_455 7 ? O8 Cs2 O12 144.14(11) . 7 ? O9 Cs2 O12 116.12(12) 4_565 7 ? O4 Cs2 Mo3 120.39(10) 5 4_565 ? O11 Cs2 Mo3 22.51(11) 4_565 4_565 ? O5 Cs2 Mo3 127.32(9) 5_455 4_565 ? O11 Cs2 Mo3 89.38(9) 5 4_565 ? O9 Cs2 Mo3 99.54(10) 5_455 4_565 ? O8 Cs2 Mo3 66.84(10) . 4_565 ? O9 Cs2 Mo3 24.85(8) 4_565 4_565 ? O12 Cs2 Mo3 135.01(7) 7 4_565 ? O4 Cs2 Mo3 126.63(10) 5 5_455 ? O11 Cs2 Mo3 91.70(11) 4_565 5_455 ? O5 Cs2 Mo3 26.45(9) 5_455 5_455 ? O11 Cs2 Mo3 99.09(11) 5 5_455 ? O9 Cs2 Mo3 23.80(9) 5_455 5_455 ? O8 Cs2 Mo3 110.42(11) . 5_455 ? O9 Cs2 Mo3 134.94(9) 4_565 5_455 ? O12 Cs2 Mo3 88.33(9) 7 5_455 ? Mo3 Cs2 Mo3 112.28(3) 4_565 5_455 ? O4 Cs2 Mo2 16.79(9) 5 5 ? O11 Cs2 Mo2 147.87(11) 4_565 5 ? O5 Cs2 Mo2 107.23(10) 5_455 5 ? O11 Cs2 Mo2 60.56(10) 5 5 ? O9 Cs2 Mo2 115.53(11) 5_455 5 ? O8 Cs2 Mo2 114.54(9) . 5 ? O9 Cs2 Mo2 100.69(10) 4_565 5 ? O12 Cs2 Mo2 32.01(7) 7 5 ? Mo3 Cs2 Mo2 125.40(4) 4_565 5 ? Mo3 Cs2 Mo2 116.48(4) 5_455 5 ? O4 Cs2 Mo2 97.69(11) 5 5_455 ? O11 Cs2 Mo2 111.38(12) 4_565 5_455 ? O5 Cs2 Mo2 20.44(9) 5_455 5_455 ? O11 Cs2 Mo2 130.88(9) 5 5_455 ? O9 Cs2 Mo2 70.43(9) 5_455 5_455 ? O8 Cs2 Mo2 81.23(10) . 5_455 ? O9 Cs2 Mo2 151.50(9) 4_565 5_455 ? O12 Cs2 Mo2 91.48(8) 7 5_455 ? Mo3 Cs2 Mo2 132.13(3) 4_565 5_455 ? Mo3 Cs2 Mo2 46.83(3) 5_455 5_455 ? Mo2 Cs2 Mo2 99.62(6) 5 5_455 ? O6 Cs3 O6 98.8(2) 4_565 . ? O6 Cs3 O8 170.68(13) 4_565 1_655 ? O6 Cs3 O8 78.41(14) . 1_655 ? O6 Cs3 O8 78.41(14) 4_565 4_665 ? O6 Cs3 O8 170.68(13) . 4_665 ? O8 Cs3 O8 105.7(2) 1_655 4_665 ? O6 Cs3 O10 137.15(12) 4_565 1_655 ? O6 Cs3 O10 113.18(13) . 1_655 ? O8 Cs3 O10 51.02(12) 1_655 1_655 ? O8 Cs3 O10 65.34(13) 4_665 1_655 ? O6 Cs3 O10 113.18(13) 4_565 4_665 ? O6 Cs3 O10 137.15(12) . 4_665 ? O8 Cs3 O10 65.34(13) 1_655 4_665 ? O8 Cs3 O10 51.02(12) 4_665 4_665 ? O10 Cs3 O10 60.01(15) 1_655 4_665 ? O6 Cs3 O9 80.34(13) 4_565 4_565 ? O6 Cs3 O9 58.95(13) . 4_565 ? O8 Cs3 O9 90.69(13) 1_655 4_565 ? O8 Cs3 O9 128.51(13) 4_665 4_565 ? O10 Cs3 O9 140.38(11) 1_655 4_565 ? O10 Cs3 O9 98.03(12) 4_665 4_565 ? O6 Cs3 O9 58.95(13) 4_565 . ? O6 Cs3 O9 80.34(13) . . ? O8 Cs3 O9 128.51(13) 1_655 . ? O8 Cs3 O9 90.69(13) 4_665 . ? O10 Cs3 O9 98.03(12) 1_655 . ? O10 Cs3 O9 140.38(11) 4_665 . ? O9 Cs3 O9 116.61(19) 4_565 . ? O6 Cs3 O2 140.42(12) 4_565 3_655 ? O6 Cs3 O2 69.01(13) . 3_655 ? O8 Cs3 O2 47.00(12) 1_655 3_655 ? O8 Cs3 O2 107.40(13) 4_665 3_655 ? O10 Cs3 O2 45.24(11) 1_655 3_655 ? O10 Cs3 O2 98.92(11) 4_665 3_655 ? O9 Cs3 O2 118.61(12) 4_565 3_655 ? O9 Cs3 O2 81.62(12) . 3_655 ? O6 Cs3 O2 69.01(13) 4_565 2_664 ? O6 Cs3 O2 140.42(12) . 2_664 ? O8 Cs3 O2 107.40(13) 1_655 2_664 ? O8 Cs3 O2 47.00(12) 4_665 2_664 ? O10 Cs3 O2 98.92(11) 1_655 2_664 ? O10 Cs3 O2 45.24(11) 4_665 2_664 ? O9 Cs3 O2 81.62(12) 4_565 2_664 ? O9 Cs3 O2 118.61(12) . 2_664 ? O2 Cs3 O2 143.03(17) 3_655 2_664 ? O6 Cs3 Mo1 164.87(10) 4_565 1_655 ? O6 Cs3 Mo1 91.18(12) . 1_655 ? O8 Cs3 Mo1 23.98(9) 1_655 1_655 ? O8 Cs3 Mo1 89.90(12) 4_665 1_655 ? O10 Cs3 Mo1 27.93(7) 1_655 1_655 ? O10 Cs3 Mo1 64.61(9) 4_665 1_655 ? O9 Cs3 Mo1 114.67(9) 4_565 1_655 ? O9 Cs3 Mo1 112.26(10) . 1_655 ? O2 Cs3 Mo1 35.03(8) 3_655 1_655 ? O2 Cs3 Mo1 109.78(10) 2_664 1_655 ? O6 Cs3 Mo1 91.18(12) 4_565 4_665 ? O6 Cs3 Mo1 164.87(10) . 4_665 ? O8 Cs3 Mo1 89.90(12) 1_655 4_665 ? O8 Cs3 Mo1 23.98(9) 4_665 4_665 ? O10 Cs3 Mo1 64.61(9) 1_655 4_665 ? O10 Cs3 Mo1 27.93(7) 4_665 4_665 ? O9 Cs3 Mo1 112.26(10) 4_565 4_665 ? O9 Cs3 Mo1 114.66(9) . 4_665 ? O2 Cs3 Mo1 109.78(10) 3_655 4_665 ? O2 Cs3 Mo1 35.03(8) 2_664 4_665 ? Mo1 Cs3 Mo1 81.48(6) 1_655 4_665 ? O8 Mo1 O6 102.3(3) . . ? O8 Mo1 O10 103.6(2) . . ? O6 Mo1 O10 101.5(2) . . ? O8 Mo1 O7 102.9(2) . . ? O6 Mo1 O7 99.21(19) . . ? O10 Mo1 O7 141.81(19) . . ? O8 Mo1 O2 84.0(2) . 3 ? O6 Mo1 O2 173.7(2) . 3 ? O10 Mo1 O2 77.10(19) . 3 ? O7 Mo1 O2 78.77(15) . 3 ? O8 Mo1 O3 170.4(2) . . ? O6 Mo1 O3 84.7(2) . . ? O10 Mo1 O3 68.27(17) . . ? O7 Mo1 O3 82.25(16) . . ? O2 Mo1 O3 89.11(18) 3 . ? O8 Mo1 Cs1 53.99(19) . 1_455 ? O6 Mo1 Cs1 136.28(19) . 1_455 ? O10 Mo1 Cs1 118.53(16) . 1_455 ? O7 Mo1 Cs1 59.85(5) . 1_455 ? O2 Mo1 Cs1 47.67(12) 3 1_455 ? O3 Mo1 Cs1 124.61(11) . 1_455 ? O8 Mo1 Cs3 51.22(18) . 1_455 ? O6 Mo1 Cs3 122.78(18) . 1_455 ? O10 Mo1 Cs3 54.75(15) . 1_455 ? O7 Mo1 Cs3 132.60(4) . 1_455 ? O2 Mo1 Cs3 61.58(13) 3 1_455 ? O3 Mo1 Cs3 119.45(11) . 1_455 ? Cs1 Mo1 Cs3 73.99(5) 1_455 1_455 ? O4 Mo2 O4 102.2(3) . 3 ? O4 Mo2 O5 97.2(2) . 3 ? O4 Mo2 O5 102.6(2) 3 3 ? O4 Mo2 O5 102.6(2) . . ? O4 Mo2 O5 97.2(2) 3 . ? O5 Mo2 O5 148.2(3) 3 . ? O4 Mo2 O12 89.7(2) . 3 ? O4 Mo2 O12 166.0(2) 3 3 ? O5 Mo2 O12 82.87(18) 3 3 ? O5 Mo2 O12 72.74(18) . 3 ? O4 Mo2 O12 166.0(2) . . ? O4 Mo2 O12 89.7(2) 3 . ? O5 Mo2 O12 72.74(18) 3 . ? O5 Mo2 O12 82.87(19) . . ? O12 Mo2 O12 79.5(2) 3 . ? O4 Mo2 Cs1 51.11(16) . 5_445 ? O4 Mo2 Cs1 51.11(16) 3 5_445 ? O5 Mo2 Cs1 105.89(14) 3 5_445 ? O5 Mo2 Cs1 105.89(14) . 5_445 ? O12 Mo2 Cs1 140.23(12) 3 5_445 ? O12 Mo2 Cs1 140.23(12) . 5_445 ? O4 Mo2 Cs2 129.03(16) . 7_545 ? O4 Mo2 Cs2 29.75(16) 3 7_545 ? O5 Mo2 Cs2 85.51(16) 3 7_545 ? O5 Mo2 Cs2 100.50(16) . 7_545 ? O12 Mo2 Cs2 140.73(12) 3 7_545 ? O12 Mo2 Cs2 61.18(12) . 7_545 ? Cs1 Mo2 Cs2 79.048(14) 5_445 7_545 ? O4 Mo2 Cs2 29.75(16) . 5_445 ? O4 Mo2 Cs2 129.03(16) 3 5_445 ? O5 Mo2 Cs2 100.50(16) 3 5_445 ? O5 Mo2 Cs2 85.51(16) . 5_445 ? O12 Mo2 Cs2 61.18(12) 3 5_445 ? O12 Mo2 Cs2 140.72(12) . 5_445 ? Cs1 Mo2 Cs2 79.048(14) 5_445 5_445 ? Cs2 Mo2 Cs2 158.10(3) 7_545 5_445 ? O4 Mo2 Cs2 100.96(17) . 5_545 ? O4 Mo2 Cs2 65.06(17) 3 5_545 ? O5 Mo2 Cs2 159.82(15) 3 5_545 ? O5 Mo2 Cs2 33.11(14) . 5_545 ? O12 Mo2 Cs2 105.79(11) 3 5_545 ? O12 Mo2 Cs2 90.65(12) . 5_545 ? Cs1 Mo2 Cs2 79.373(14) 5_445 5_545 ? Cs2 Mo2 Cs2 76.28(6) 7_545 5_545 ? Cs2 Mo2 Cs2 99.62(6) 5_445 5_545 ? O4 Mo2 Cs2 65.06(17) . 7_445 ? O4 Mo2 Cs2 100.96(17) 3 7_445 ? O5 Mo2 Cs2 33.11(14) 3 7_445 ? O5 Mo2 Cs2 159.82(15) . 7_445 ? O12 Mo2 Cs2 90.65(12) 3 7_445 ? O12 Mo2 Cs2 105.79(11) . 7_445 ? Cs1 Mo2 Cs2 79.373(14) 5_445 7_445 ? Cs2 Mo2 Cs2 99.62(6) 7_545 7_445 ? Cs2 Mo2 Cs2 76.28(6) 5_445 7_445 ? Cs2 Mo2 Cs2 158.75(3) 5_545 7_445 ? O9 Mo3 O11 103.6(3) . . ? O9 Mo3 O10 101.4(2) . . ? O11 Mo3 O10 99.0(2) . . ? O9 Mo3 O5 95.4(2) . . ? O11 Mo3 O5 100.0(2) . . ? O10 Mo3 O5 150.78(17) . . ? O9 Mo3 O3 97.5(2) . . ? O11 Mo3 O3 158.6(2) . . ? O10 Mo3 O3 73.15(17) . . ? O5 Mo3 O3 81.14(19) . . ? O9 Mo3 O12 164.3(2) . 3 ? O11 Mo3 O12 85.5(2) . 3 ? O10 Mo3 O12 89.55(17) . 3 ? O5 Mo3 O12 70.14(18) . 3 ? O3 Mo3 O12 74.75(17) . 3 ? O9 Mo3 Cs2 61.9(2) . 4_565 ? O11 Mo3 Cs2 41.80(17) . 4_565 ? O10 Mo3 Cs2 108.46(12) . 4_565 ? O5 Mo3 Cs2 100.51(14) . 4_565 ? O3 Mo3 Cs2 159.36(13) . 4_565 ? O12 Mo3 Cs2 125.37(11) 3 4_565 ? O9 Mo3 Cs2 52.46(19) . 5_545 ? O11 Mo3 Cs2 101.30(18) . 5_545 ? O10 Mo3 Cs2 150.08(15) . 5_545 ? O5 Mo3 Cs2 43.57(14) . 5_545 ? O3 Mo3 Cs2 94.20(13) . 5_545 ? O12 Mo3 Cs2 113.67(11) 3 5_545 ? Cs2 Mo3 Cs2 74.21(3) 4_565 5_545 ? O2 P1 O3 111.7(3) . . ? O2 P1 O12 112.9(3) . . ? O3 P1 O12 112.1(3) . . ? O2 P1 O1 109.6(3) . . ? O3 P1 O1 107.6(2) . . ? O12 P1 O1 102.5(2) . . ? P1 O1 P1 133.4(4) . 3_655 ? P1 O2 Mo1 119.7(3) . 3 ? P1 O2 Cs1 119.2(3) . . ? Mo1 O2 Cs1 96.77(16) 3 . ? P1 O2 Cs3 133.3(2) . 2_665 ? Mo1 O2 Cs3 83.39(14) 3 2_665 ? Cs1 O2 Cs3 94.66(13) . 2_665 ? P1 O3 Mo3 132.5(3) . . ? P1 O3 Mo1 129.9(3) . . ? Mo3 O3 Mo1 91.52(16) . . ? Mo2 O4 Cs2 133.5(2) . 5_445 ? Mo2 O4 Cs1 102.5(2) . 5_445 ? Cs2 O4 Cs1 120.20(16) 5_445 5_445 ? Mo2 O5 Mo3 123.3(3) . . ? Mo2 O5 Cs2 126.5(2) . 5_545 ? Mo3 O5 Cs2 109.97(19) . 5_545 ? Mo1 O6 Cs1 114.4(2) . . ? Mo1 O6 Cs3 128.1(3) . . ? Cs1 O6 Cs3 101.02(17) . . ? Mo1 O7 Mo1 155.2(3) . 3 ? Mo1 O7 Cs1 95.13(3) . . ? Mo1 O7 Cs1 91.52(3) 3 . ? Mo1 O7 Cs1 91.52(3) . 1_455 ? Mo1 O7 Cs1 95.13(3) 3 1_455 ? Cs1 O7 Cs1 148.62(16) . 1_455 ? Mo1 O8 Cs3 104.8(2) . 1_455 ? Mo1 O8 Cs1 101.3(2) . 1_455 ? Cs3 O8 Cs1 95.10(16) 1_455 1_455 ? Mo1 O8 Cs2 114.4(2) . . ? Cs3 O8 Cs2 131.49(16) 1_455 . ? Cs1 O8 Cs2 103.68(14) 1_455 . ? Mo3 O9 Cs2 103.7(2) . 5_545 ? Mo3 O9 Cs3 120.6(2) . . ? Cs2 O9 Cs3 117.74(17) 5_545 . ? Mo3 O9 Cs2 93.3(2) . 4_565 ? Cs2 O9 Cs2 90.42(14) 5_545 4_565 ? Cs3 O9 Cs2 124.81(15) . 4_565 ? Mo1 O10 Mo3 125.8(2) . . ? Mo1 O10 Cs3 97.32(17) . 1_455 ? Mo3 O10 Cs3 127.36(19) . 1_455 ? Mo3 O11 Cs2 115.7(3) . 4_565 ? Mo3 O11 Cs2 131.4(2) . 5_445 ? Cs2 O11 Cs2 104.38(15) 4_565 5_445 ? P1 O12 Mo2 129.0(3) . . ? P1 O12 Mo3 127.0(3) . 3 ? Mo2 O12 Mo3 93.71(16) . 3 ? P1 O12 Cs2 116.2(2) . 7_545 ? Mo2 O12 Cs2 86.81(14) . 7_545 ? Mo3 O12 Cs2 92.58(13) 3 7_545 ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.77 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.971 _refine_diff_density_min -0.905 _refine_diff_density_rms 0.174