# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2001 # CCDC Number: 186/2282 data_compound1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C9 H17 B11 Mo O3' _chemical_formula_weight 388.08 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' 'Mo' 'Mo' -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y+1/2, z+1/2' '-x, -y, -z' '-x, y-1/2, -z-1/2' _cell_length_a 10.1425(19) _cell_length_b 10.4875(13) _cell_length_c 16.515(2) _cell_angle_alpha 90.00 _cell_angle_beta 93.76 _cell_angle_gamma 90.00 _cell_volume 1752.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12 _cell_measurement_theta_max 18 _exptl_crystal_description Parallelepiped _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.471 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 768 _exptl_absorpt_coefficient_mu 0.749 _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 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '4-circle diffractometer' _diffrn_measurement_method 'scintillation counter' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4157 _diffrn_reflns_av_R_equivalents 0.0150 _diffrn_reflns_av_sigmaI/netI 0.0256 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 26.96 _reflns_number_total 3801 _reflns_number_gt 3194 _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 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _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^)+(0.0509P)^2^+0.1573P] 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 3801 _refine_ls_number_parameters 232 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0369 _refine_ls_R_factor_gt 0.0289 _refine_ls_wR_factor_ref 0.0806 _refine_ls_wR_factor_gt 0.0780 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.307130(18) 0.113818(18) 0.170126(10) 0.03860(8) Uani 1 1 d . . . O1 O 0.5894(2) -0.0074(2) 0.19668(14) 0.0773(6) Uani 1 1 d . . . O2 O 0.5108(2) 0.3375(2) 0.16647(15) 0.0790(7) Uani 1 1 d . . . O3 O 0.2784(2) 0.1979(3) -0.01276(13) 0.0954(8) Uani 1 1 d . . . B2 B 0.3373(3) -0.3592(3) 0.0115(2) 0.0606(8) Uani 1 1 d . . . H2 H 0.4167 -0.4141 -0.0144 0.073 Uiso 1 1 calc R . . B3 B 0.2676(4) -0.4071(3) 0.1008(2) 0.0679(9) Uani 1 1 d . . . H3 H 0.3022 -0.4938 0.1332 0.081 Uiso 1 1 calc R . . B4 B 0.0980(4) -0.3631(3) 0.0940(2) 0.0641(9) Uani 1 1 d . . . H4 H 0.0219 -0.4202 0.1217 0.077 Uiso 1 1 calc R . . B5 B 0.0668(3) -0.2872(3) -0.0001(2) 0.0580(7) Uani 1 1 d . . . H5 H -0.0301 -0.2951 -0.0338 0.070 Uiso 1 1 calc R . . B6 B 0.2137(3) -0.2845(3) -0.05096(17) 0.0552(7) Uani 1 1 d . . . H6 H 0.2127 -0.2908 -0.1175 0.066 Uiso 1 1 calc R . . B7 B 0.2152(4) -0.2713(3) 0.15293(18) 0.0641(9) Uani 1 1 d . . . H7 H 0.2161 -0.2668 0.2195 0.077 Uiso 1 1 calc R . . B8 B 0.0897(3) -0.1960(3) 0.08973(19) 0.0553(7) Uani 1 1 d . . . H8 H 0.0093 -0.1423 0.1156 0.066 Uiso 1 1 calc R . . B9 B 0.1611(3) -0.1475(3) -0.00163(18) 0.0517(7) Uani 1 1 d . . . H9 H 0.1260 -0.0622 -0.0353 0.062 Uiso 1 1 calc R . . B10 B 0.3312(3) -0.1911(3) 0.00583(18) 0.0516(7) Uani 1 1 d . . . H10 H 0.4070 -0.1346 -0.0226 0.062 Uiso 1 1 calc R . . B11 B 0.3640(3) -0.2688(3) 0.1015(2) 0.0612(8) Uani 1 1 d . . . H11 H 0.4610 -0.2625 0.1352 0.073 Uiso 1 1 calc R . . B12 B 0.2531(3) -0.1406(3) 0.09142(17) 0.0451(6) Uani 1 1 d . . . H12 H 0.303(3) -0.043(3) 0.1119(19) 0.088(10) Uiso 1 1 d . . . C1 C 0.1781(3) -0.4065(3) 0.01132(17) 0.0571(7) Uani 1 1 d . . . H1 H 0.1520 -0.4992 -0.0164 0.069 Uiso 1 1 calc R . . C2 C 0.4870(3) 0.0338(2) 0.18661(15) 0.0508(6) Uani 1 1 d . . . C3 C 0.4357(3) 0.2589(3) 0.16727(16) 0.0529(6) Uani 1 1 d . . . C4 C 0.2885(3) 0.1654(3) 0.05228(16) 0.0617(7) Uani 1 1 d . . . C5 C 0.2436(3) 0.0861(3) 0.30292(17) 0.0674(8) Uani 1 1 d . . . H5A H 0.2963 0.0437 0.3425 0.081 Uiso 1 1 calc R . . C6 C 0.2477(3) 0.2135(3) 0.28585(17) 0.0672(8) Uani 1 1 d . . . H6 H 0.3046 0.2727 0.3114 0.081 Uiso 1 1 calc R . . C7 C 0.1504(4) 0.2400(3) 0.2225(2) 0.0759(10) Uani 1 1 d . . . H7A H 0.1309 0.3192 0.1993 0.091 Uiso 1 1 calc R . . C8 C 0.0902(3) 0.1249(4) 0.20176(19) 0.0743(10) Uani 1 1 d . . . H8 H 0.0228 0.1123 0.1616 0.089 Uiso 1 1 calc R . . C9 C 0.1486(3) 0.0321(3) 0.25185(18) 0.0702(9) Uani 1 1 d . . . H9 H 0.1264 -0.0539 0.2507 0.084 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 Mo1 0.03980(12) 0.04430(13) 0.03189(12) 0.00066(7) 0.00388(7) -0.00182(8) O1 0.0589(12) 0.0769(14) 0.0947(16) 0.0128(12) -0.0043(11) 0.0133(11) O2 0.0775(14) 0.0617(12) 0.1017(18) -0.0135(12) 0.0350(13) -0.0248(12) O3 0.0845(16) 0.156(2) 0.0460(12) 0.0364(14) 0.0061(11) 0.0093(16) B2 0.0556(18) 0.0597(19) 0.067(2) -0.0085(15) 0.0066(15) 0.0156(14) B3 0.084(2) 0.061(2) 0.0565(19) 0.0109(15) -0.0090(17) 0.0075(17) B4 0.068(2) 0.068(2) 0.0579(19) -0.0083(15) 0.0158(16) -0.0159(16) B5 0.0477(16) 0.0672(19) 0.0574(17) -0.0113(15) -0.0090(13) 0.0007(14) B6 0.0707(19) 0.0567(16) 0.0379(13) -0.0072(12) 0.0014(13) 0.0025(15) B7 0.084(2) 0.071(2) 0.0360(14) -0.0046(14) 0.0017(14) -0.0114(18) B8 0.0445(15) 0.0590(18) 0.0634(18) -0.0143(14) 0.0098(13) -0.0023(13) B9 0.0560(17) 0.0499(15) 0.0475(15) -0.0036(12) -0.0095(13) 0.0097(13) B10 0.0479(15) 0.0594(18) 0.0484(15) -0.0038(13) 0.0096(12) 0.0013(13) B11 0.0480(16) 0.073(2) 0.0608(18) -0.0010(16) -0.0133(14) 0.0106(15) B12 0.0460(14) 0.0498(15) 0.0395(13) -0.0081(11) 0.0019(11) 0.0003(11) C1 0.0679(17) 0.0498(15) 0.0536(15) -0.0088(11) 0.0034(13) -0.0025(12) C2 0.0511(14) 0.0483(14) 0.0530(14) 0.0034(11) 0.0022(11) -0.0007(11) C3 0.0541(14) 0.0491(14) 0.0574(15) -0.0012(11) 0.0176(12) -0.0003(12) C4 0.0500(14) 0.091(2) 0.0441(14) 0.0111(14) 0.0050(11) 0.0043(15) C5 0.0707(19) 0.092(2) 0.0416(14) 0.0141(14) 0.0171(13) 0.0144(17) C6 0.0682(18) 0.083(2) 0.0528(15) -0.0287(15) 0.0217(14) -0.0224(16) C7 0.092(2) 0.068(2) 0.0721(19) 0.0166(16) 0.0418(18) 0.0340(18) C8 0.0433(14) 0.130(3) 0.0502(16) -0.0109(17) 0.0084(12) -0.0064(16) C9 0.089(2) 0.0656(18) 0.0606(17) -0.0106(14) 0.0399(16) -0.0231(16) _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 Mo1 C3 2.007(3) . ? Mo1 C2 2.011(3) . ? Mo1 C4 2.017(3) . ? Mo1 C7 2.281(3) . ? Mo1 C6 2.294(3) . ? Mo1 C8 2.298(3) . ? Mo1 C9 2.329(3) . ? Mo1 C5 2.344(3) . ? O1 C2 1.127(3) . ? O2 C3 1.123(3) . ? O3 C4 1.125(3) . ? B2 C1 1.688(4) . ? B2 B3 1.750(5) . ? B2 B6 1.755(5) . ? B2 B10 1.766(5) . ? B2 B11 1.768(5) . ? B3 C1 1.683(4) . ? B3 B11 1.749(5) . ? B3 B7 1.764(5) . ? B3 B4 1.777(5) . ? B4 C1 1.697(4) . ? B4 B8 1.756(5) . ? B4 B5 1.757(5) . ? B4 B7 1.771(5) . ? B5 C1 1.687(4) . ? B5 B9 1.751(5) . ? B5 B6 1.757(4) . ? B5 B8 1.768(4) . ? B6 C1 1.694(4) . ? B6 B9 1.752(4) . ? B6 B10 1.765(4) . ? B7 B12 1.763(4) . ? B7 B8 1.778(5) . ? B7 B11 1.779(5) . ? B8 B12 1.755(4) . ? B8 B9 1.789(4) . ? B9 B12 1.746(4) . ? B9 B10 1.782(4) . ? B10 B12 1.747(4) . ? B10 B11 1.789(4) . ? B11 B12 1.753(4) . ? C5 C9 1.361(4) . ? C5 C6 1.367(4) . ? C6 C7 1.418(5) . ? C7 C8 1.386(5) . ? C8 C9 1.385(5) . ? 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 C3 Mo1 C2 74.59(10) . . ? C3 Mo1 C4 78.10(12) . . ? C2 Mo1 C4 105.62(11) . . ? C3 Mo1 C7 92.22(12) . . ? C2 Mo1 C7 147.06(12) . . ? C4 Mo1 C7 100.76(12) . . ? C3 Mo1 C6 83.13(10) . . ? C2 Mo1 C6 111.29(11) . . ? C4 Mo1 C6 131.97(13) . . ? C7 Mo1 C6 36.10(12) . . ? C3 Mo1 C8 126.90(12) . . ? C2 Mo1 C8 149.83(12) . . ? C4 Mo1 C8 100.10(11) . . ? C7 Mo1 C8 35.23(12) . . ? C6 Mo1 C8 58.64(11) . . ? C3 Mo1 C9 140.07(10) . . ? C2 Mo1 C9 115.02(12) . . ? C4 Mo1 C9 129.29(12) . . ? C7 Mo1 C9 57.95(12) . . ? C6 Mo1 C9 57.03(11) . . ? C8 Mo1 C9 34.83(12) . . ? C3 Mo1 C5 109.57(12) . . ? C2 Mo1 C5 97.15(11) . . ? C4 Mo1 C5 157.21(11) . . ? C7 Mo1 C5 58.41(11) . . ? C6 Mo1 C5 34.26(11) . . ? C8 Mo1 C5 57.81(11) . . ? C9 Mo1 C5 33.86(11) . . ? C1 B2 B3 58.57(19) . . ? C1 B2 B6 58.92(18) . . ? B3 B2 B6 108.1(2) . . ? C1 B2 B10 105.3(2) . . ? B3 B2 B10 108.5(2) . . ? B6 B2 B10 60.16(18) . . ? C1 B2 B11 104.7(2) . . ? B3 B2 B11 59.6(2) . . ? B6 B2 B11 108.6(2) . . ? B10 B2 B11 60.83(18) . . ? C1 B3 B2 58.88(19) . . ? C1 B3 B11 105.7(2) . . ? B2 B3 B11 60.7(2) . . ? C1 B3 B7 105.2(2) . . ? B2 B3 B7 109.3(2) . . ? B11 B3 B7 60.8(2) . . ? C1 B3 B4 58.65(19) . . ? B2 B3 B4 108.3(2) . . ? B11 B3 B4 108.8(2) . . ? B7 B3 B4 60.0(2) . . ? C1 B4 B8 105.0(2) . . ? C1 B4 B5 58.44(18) . . ? B8 B4 B5 60.45(19) . . ? C1 B4 B7 104.4(2) . . ? B8 B4 B7 60.54(19) . . ? B5 B4 B7 108.4(2) . . ? C1 B4 B3 57.89(19) . . ? B8 B4 B3 107.8(2) . . ? B5 B4 B3 106.9(2) . . ? B7 B4 B3 59.6(2) . . ? C1 B5 B9 105.1(2) . . ? C1 B5 B4 59.00(18) . . ? B9 B5 B4 108.9(2) . . ? C1 B5 B6 58.90(17) . . ? B9 B5 B6 59.94(18) . . ? B4 B5 B6 108.7(2) . . ? C1 B5 B8 104.9(2) . . ? B9 B5 B8 61.12(18) . . ? B4 B5 B8 59.75(18) . . ? B6 B5 B8 108.9(2) . . ? C1 B6 B9 104.7(2) . . ? C1 B6 B2 58.59(18) . . ? B9 B6 B2 108.7(2) . . ? C1 B6 B5 58.48(18) . . ? B9 B6 B5 59.84(18) . . ? B2 B6 B5 107.9(2) . . ? C1 B6 B10 105.0(2) . . ? B9 B6 B10 60.87(17) . . ? B2 B6 B10 60.22(18) . . ? B5 B6 B10 108.6(2) . . ? B12 B7 B3 105.2(2) . . ? B12 B7 B4 105.7(2) . . ? B3 B7 B4 60.4(2) . . ? B12 B7 B8 59.42(17) . . ? B3 B7 B8 107.4(2) . . ? B4 B7 B8 59.32(19) . . ? B12 B7 B11 59.32(18) . . ? B3 B7 B11 59.2(2) . . ? B4 B7 B11 107.8(2) . . ? B8 B7 B11 108.1(2) . . ? B4 B8 B12 106.7(2) . . ? B4 B8 B5 59.80(19) . . ? B12 B8 B5 105.3(2) . . ? B4 B8 B7 60.1(2) . . ? B12 B8 B7 59.87(17) . . ? B5 B8 B7 107.6(2) . . ? B4 B8 B9 107.2(2) . . ? B12 B8 B9 59.03(16) . . ? B5 B8 B9 58.95(18) . . ? B7 B8 B9 107.9(2) . . ? B12 B9 B5 106.4(2) . . ? B12 B9 B6 106.3(2) . . ? B5 B9 B6 60.22(18) . . ? B12 B9 B10 59.35(16) . . ? B5 B9 B10 108.1(2) . . ? B6 B9 B10 59.90(17) . . ? B12 B9 B8 59.50(16) . . ? B5 B9 B8 59.93(18) . . ? B6 B9 B8 108.1(2) . . ? B10 B9 B8 108.2(2) . . ? B12 B10 B6 105.8(2) . . ? B12 B10 B2 106.0(2) . . ? B6 B10 B2 59.62(18) . . ? B12 B10 B9 59.32(16) . . ? B6 B10 B9 59.22(17) . . ? B2 B10 B9 106.9(2) . . ? B12 B10 B11 59.42(17) . . ? B6 B10 B11 107.3(2) . . ? B2 B10 B11 59.66(19) . . ? B9 B10 B11 107.5(2) . . ? B3 B11 B12 106.3(2) . . ? B3 B11 B2 59.7(2) . . ? B12 B11 B2 105.6(2) . . ? B3 B11 B7 60.0(2) . . ? B12 B11 B7 59.88(18) . . ? B2 B11 B7 107.8(2) . . ? B3 B11 B10 107.5(2) . . ? B12 B11 B10 59.09(16) . . ? B2 B11 B10 59.51(18) . . ? B7 B11 B10 108.3(2) . . ? B10 B12 B9 61.33(17) . . ? B10 B12 B11 61.49(18) . . ? B9 B12 B11 110.8(2) . . ? B10 B12 B8 111.4(2) . . ? B9 B12 B8 61.47(17) . . ? B11 B12 B8 110.3(2) . . ? B10 B12 B7 111.0(2) . . ? B9 B12 B7 110.5(2) . . ? B11 B12 B7 60.80(19) . . ? B8 B12 B7 60.71(18) . . ? B3 C1 B5 114.8(2) . . ? B3 C1 B2 62.5(2) . . ? B5 C1 B2 114.5(2) . . ? B3 C1 B4 63.5(2) . . ? B5 C1 B4 62.6(2) . . ? B2 C1 B4 115.3(2) . . ? B3 C1 B6 114.4(2) . . ? B5 C1 B6 62.63(18) . . ? B2 C1 B6 62.50(19) . . ? B4 C1 B6 114.7(2) . . ? O1 C2 Mo1 177.8(2) . . ? O2 C3 Mo1 177.8(3) . . ? O3 C4 Mo1 177.9(3) . . ? C9 C5 C6 108.0(3) . . ? C9 C5 Mo1 72.45(16) . . ? C6 C5 Mo1 70.84(15) . . ? C5 C6 C7 108.3(3) . . ? C5 C6 Mo1 74.89(16) . . ? C7 C6 Mo1 71.48(15) . . ? C8 C7 C6 106.6(3) . . ? C8 C7 Mo1 73.03(17) . . ? C6 C7 Mo1 72.42(16) . . ? C9 C8 C7 107.4(3) . . ? C9 C8 Mo1 73.81(17) . . ? C7 C8 Mo1 71.74(17) . . ? C5 C9 C8 109.6(3) . . ? C5 C9 Mo1 73.69(16) . . ? C8 C9 Mo1 71.36(16) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.96 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.420 _refine_diff_density_min -0.454 _refine_diff_density_rms 0.056 #===END data_compound2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C9 H17 Ag B11 I Mo O3' _chemical_formula_weight 622.85 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 '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' 'Mo' 'Mo' -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pnna loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' 'x, -y+1/2, -z+1/2' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' '-x, y-1/2, z-1/2' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.8843(4) _cell_length_b 15.7193(4) _cell_length_c 18.1490(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3961.0(2) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.089 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2336 _exptl_absorpt_coefficient_mu 3.186 _exptl_absorpt_correction_type Scalepack _exptl_absorpt_correction_T_min 0.5683 _exptl_absorpt_correction_T_max 0.7847 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 KappaCCD _diffrn_measurement_method '2o phi + omage frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 7282 _diffrn_reflns_av_R_equivalents 0.0476 _diffrn_reflns_av_sigmaI/netI 0.0563 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.61 _diffrn_reflns_theta_max 26.00 _reflns_number_total 3870 _reflns_number_gt 3193 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSeed (Barbour, 1999)' _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^)+(0.0000P)^2^+59.8144P] 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 0.00059(8) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3870 _refine_ls_number_parameters 236 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0725 _refine_ls_R_factor_gt 0.0563 _refine_ls_wR_factor_ref 0.1145 _refine_ls_wR_factor_gt 0.1101 _refine_ls_goodness_of_fit_ref 1.229 _refine_ls_restrained_S_all 1.229 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group I1 I 0.29701(4) 0.22339(4) 0.36621(3) 0.02088(18) Uani 1 1 d . . . Ag1 Ag 0.23195(6) 0.14787(5) 0.22440(4) 0.0354(2) Uani 1 1 d . . . Mo1 Mo 0.19638(5) 0.21547(4) 0.50354(4) 0.01421(19) Uani 1 1 d . . . O1 O 0.3509(5) 0.0694(5) 0.5188(4) 0.045(2) Uani 1 1 d . . . C1 C 0.0531(6) 0.2058(6) 0.4344(5) 0.026(2) Uani 1 1 d . . . H1 H 0.0501 0.2201 0.3836 0.031 Uiso 1 1 calc R . . B1 B 0.0655(8) 0.0703(7) 0.2516(7) 0.029(2) Uani 1 1 d . . . H1A H 0.1180 0.1124 0.2809 0.035 Uiso 1 1 calc R . . O2 O 0.2673(6) 0.2413(6) 0.6652(4) 0.055(2) Uani 1 1 d . . . C2 C 0.0767(6) 0.1241(6) 0.4632(5) 0.025(2) Uani 1 1 d . . . H2 H 0.0924 0.0748 0.4354 0.030 Uiso 1 1 calc R . . B2 B -0.0256(9) 0.1121(9) 0.1962(11) 0.068(6) Uani 1 1 d . . . H2A H -0.0361 0.1819 0.1873 0.081 Uiso 1 1 calc R . . O3 O 0.2679(5) 0.4062(4) 0.4989(4) 0.0412(18) Uani 1 1 d . . . C3 C 0.0726(6) 0.1298(6) 0.5403(5) 0.026(2) Uani 1 1 d . . . H3 H 0.0844 0.0849 0.5742 0.032 Uiso 1 1 calc R . . B3 B 0.0709(8) 0.0581(8) 0.1566(6) 0.034(3) Uani 1 1 d . . . H3A H 0.1260 0.0922 0.1226 0.041 Uiso 1 1 calc R . . C4 C 0.0473(6) 0.2153(7) 0.5587(5) 0.031(2) Uani 1 1 d . . . H4 H 0.0398 0.2378 0.6069 0.037 Uiso 1 1 calc R . . B4 B 0.0999(7) -0.0291(7) 0.2145(6) 0.027(2) Uani 1 1 d . . . H4A H 0.1755 -0.0533 0.2183 0.032 Uiso 1 1 calc R . . C5 C 0.0354(6) 0.2605(6) 0.4919(6) 0.032(2) Uani 1 1 d . . . H5 H 0.0182 0.3187 0.4875 0.038 Uiso 1 1 calc R . . B5 B 0.0229(8) -0.0259(8) 0.2908(6) 0.032(3) Uani 1 1 d . . . H5A H 0.0475 -0.0482 0.3463 0.038 Uiso 1 1 calc R . . C6 C 0.2969(7) 0.1252(6) 0.5127(5) 0.030(2) Uani 1 1 d . . . B6 B -0.0549(8) 0.0624(7) 0.2818(8) 0.042(4) Uani 1 1 d . . . H6 H -0.0833 0.0985 0.3304 0.050 Uiso 1 1 calc R . . C7 C 0.2438(7) 0.2316(7) 0.6067(5) 0.031(2) Uani 1 1 d . . . C9 C -0.1161(6) 0.0421(8) 0.2036(7) 0.052(4) Uani 1 1 d . . . H9 H -0.1910 0.0683 0.2002 0.063 Uiso 1 1 calc R . . C8 C 0.2465(7) 0.3365(6) 0.5003(5) 0.0243(19) Uani 1 1 d . . . B7 B -0.0474(10) 0.0376(13) 0.1255(8) 0.067(6) Uani 1 1 d . . . H7 H -0.0723 0.0576 0.0695 0.080 Uiso 1 1 calc R . . B11 B -0.0957(7) -0.0415(7) 0.2598(6) 0.023(2) Uani 1 1 d . . . H11 H -0.1530 -0.0731 0.2934 0.028 Uiso 1 1 calc R . . B8 B 0.0295(10) -0.0488(12) 0.1367(8) 0.061(5) Uani 1 1 d . . . H8 H 0.0578 -0.0859 0.0887 0.074 Uiso 1 1 calc R . . B10 B -0.0006(8) -0.0995(7) 0.2209(8) 0.035(3) Uani 1 1 d . . . H10 H 0.0074 -0.1697 0.2297 0.042 Uiso 1 1 calc R . . B9 B -0.0902(9) -0.0567(12) 0.1648(7) 0.057(5) Uani 1 1 d . . . H9A H -0.1431 -0.0983 0.1353 0.069 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 I1 0.0172(3) 0.0274(3) 0.0180(3) -0.0012(2) 0.0038(2) 0.0008(2) Ag1 0.0321(4) 0.0320(4) 0.0420(4) 0.0069(4) 0.0028(3) -0.0042(3) Mo1 0.0134(3) 0.0146(3) 0.0147(3) -0.0003(3) 0.0005(3) 0.0005(3) O1 0.033(4) 0.035(4) 0.065(5) 0.016(4) -0.001(4) 0.017(4) C1 0.013(4) 0.039(6) 0.024(5) 0.004(4) -0.002(3) -0.002(4) B1 0.026(5) 0.022(5) 0.039(6) -0.012(5) 0.012(5) -0.016(5) O2 0.049(5) 0.097(7) 0.020(4) -0.002(4) -0.015(3) -0.009(5) C2 0.018(5) 0.026(5) 0.031(5) -0.003(4) -0.001(4) 0.002(4) B2 0.024(6) 0.033(7) 0.146(17) 0.046(10) 0.031(8) 0.004(6) O3 0.041(4) 0.022(4) 0.060(5) -0.010(4) 0.000(4) -0.007(3) C3 0.012(4) 0.030(5) 0.038(5) 0.018(5) 0.002(4) -0.010(4) B3 0.021(6) 0.045(7) 0.035(6) 0.019(6) 0.008(5) -0.003(5) C4 0.016(4) 0.048(6) 0.029(5) -0.013(5) 0.006(4) -0.005(4) B4 0.013(5) 0.028(6) 0.039(6) -0.007(5) 0.002(4) 0.001(4) C5 0.015(4) 0.031(5) 0.049(6) -0.006(5) -0.001(4) 0.003(4) B5 0.026(6) 0.042(7) 0.028(6) 0.016(5) -0.001(5) -0.007(5) C6 0.019(5) 0.040(6) 0.032(5) 0.015(5) -0.003(4) -0.007(4) B6 0.023(6) 0.025(6) 0.078(9) -0.024(7) 0.037(6) -0.017(5) C7 0.024(5) 0.043(6) 0.027(5) -0.002(5) 0.004(4) 0.010(4) C9 0.005(4) 0.058(8) 0.093(10) 0.053(7) 0.003(5) 0.002(5) C8 0.025(5) 0.025(5) 0.023(4) -0.008(4) 0.000(4) -0.004(4) B7 0.029(7) 0.121(16) 0.050(9) 0.047(10) -0.021(6) -0.025(8) B11 0.013(4) 0.021(5) 0.035(6) 0.008(5) 0.002(4) -0.008(4) B8 0.040(7) 0.108(13) 0.036(7) -0.051(9) 0.018(6) -0.029(8) B10 0.023(5) 0.015(5) 0.068(8) -0.010(6) 0.014(6) 0.002(4) B9 0.025(6) 0.118(14) 0.029(6) -0.001(8) -0.002(5) -0.034(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag I1 Ag1 2.7599(9) 3 ? I1 Mo1 2.8599(8) . ? I1 Ag1 2.9748(10) . ? Ag1 B1 2.659(10) . ? Ag1 I1 2.7599(9) 3 ? Ag1 Ag1 3.3426(16) 3 ? Mo1 C6 1.997(10) . ? Mo1 C7 2.000(10) . ? Mo1 C8 2.027(9) . ? Mo1 C3 2.284(8) . ? Mo1 C4 2.300(9) . ? Mo1 C2 2.315(9) . ? Mo1 C5 2.353(9) . ? Mo1 C1 2.357(8) . ? O1 C6 1.159(12) . ? C1 C5 1.374(13) . ? C1 C2 1.425(13) . ? B1 B3 1.735(17) . ? B1 B2 1.74(2) . ? B1 B6 1.764(14) . ? B1 B4 1.766(15) . ? B1 B5 1.773(15) . ? O2 C7 1.122(11) . ? C2 C3 1.404(13) . ? B2 C9 1.675(16) . ? B2 B3 1.741(18) . ? B2 B7 1.76(3) . ? B2 B6 1.79(2) . ? O3 C8 1.134(11) . ? C3 C4 1.429(14) . ? B3 B7 1.766(17) . ? B3 B4 1.772(16) . ? B3 B8 1.81(2) . ? C4 C5 1.415(14) . ? B4 B8 1.744(17) . ? B4 B5 1.750(16) . ? B4 B10 1.784(14) . ? B5 B10 1.748(17) . ? B5 B11 1.758(15) . ? B5 B6 1.767(18) . ? B6 C9 1.684(19) . ? B6 B11 1.774(15) . ? C9 B11 1.686(14) . ? C9 B7 1.71(2) . ? C9 B9 1.74(2) . ? B7 B8 1.74(3) . ? B7 B9 1.75(2) . ? B11 B9 1.742(17) . ? B11 B10 1.754(14) . ? B8 B9 1.742(17) . ? B8 B10 1.77(2) . ? B10 B9 1.742(19) . ? 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 Ag1 I1 Mo1 113.04(3) 3 . ? Ag1 I1 Ag1 71.19(3) 3 . ? Mo1 I1 Ag1 126.03(3) . . ? B1 Ag1 I1 137.0(3) . 3 ? B1 Ag1 I1 106.6(2) . . ? I1 Ag1 I1 97.10(3) 3 . ? B1 Ag1 Ag1 112.9(2) . 3 ? I1 Ag1 Ag1 57.40(2) 3 3 ? I1 Ag1 Ag1 51.41(2) . 3 ? C6 Mo1 C7 77.4(4) . . ? C6 Mo1 C8 115.4(4) . . ? C7 Mo1 C8 78.2(4) . . ? C6 Mo1 C3 94.7(4) . . ? C7 Mo1 C3 92.8(4) . . ? C8 Mo1 C3 145.1(4) . . ? C6 Mo1 C4 126.3(4) . . ? C7 Mo1 C4 83.6(4) . . ? C8 Mo1 C4 108.8(4) . . ? C3 Mo1 C4 36.3(4) . . ? C6 Mo1 C2 95.0(4) . . ? C7 Mo1 C2 127.6(4) . . ? C8 Mo1 C2 145.0(3) . . ? C3 Mo1 C2 35.5(3) . . ? C4 Mo1 C2 59.4(3) . . ? C6 Mo1 C5 152.2(4) . . ? C7 Mo1 C5 111.0(4) . . ? C8 Mo1 C5 92.3(4) . . ? C3 Mo1 C5 59.3(3) . . ? C4 Mo1 C5 35.4(3) . . ? C2 Mo1 C5 58.4(3) . . ? C6 Mo1 C1 126.0(4) . . ? C7 Mo1 C1 141.7(3) . . ? C8 Mo1 C1 109.5(4) . . ? C3 Mo1 C1 58.8(3) . . ? C4 Mo1 C1 58.1(3) . . ? C2 Mo1 C1 35.5(3) . . ? C5 Mo1 C1 33.9(3) . . ? C6 Mo1 I1 76.2(3) . . ? C7 Mo1 I1 130.5(3) . . ? C8 Mo1 I1 76.5(2) . . ? C3 Mo1 I1 130.4(3) . . ? C4 Mo1 I1 145.0(2) . . ? C2 Mo1 I1 95.9(2) . . ? C5 Mo1 I1 111.9(3) . . ? C1 Mo1 I1 87.2(2) . . ? C5 C1 C2 109.0(8) . . ? C5 C1 Mo1 72.9(5) . . ? C2 C1 Mo1 70.6(5) . . ? B3 B1 B2 60.0(8) . . ? B3 B1 B6 110.0(9) . . ? B2 B1 B6 61.2(8) . . ? B3 B1 B4 60.8(6) . . ? B2 B1 B4 108.0(9) . . ? B6 B1 B4 108.2(7) . . ? B3 B1 B5 108.6(8) . . ? B2 B1 B5 108.1(8) . . ? B6 B1 B5 59.9(7) . . ? B4 B1 B5 59.3(6) . . ? B3 B1 Ag1 80.2(5) . . ? B2 B1 Ag1 110.5(7) . . ? B6 B1 Ag1 156.0(7) . . ? B4 B1 Ag1 95.8(5) . . ? B5 B1 Ag1 139.1(7) . . ? C3 C2 C1 107.4(9) . . ? C3 C2 Mo1 71.0(5) . . ? C1 C2 Mo1 73.9(5) . . ? C9 B2 B3 106.9(11) . . ? C9 B2 B1 104.5(9) . . ? B3 B2 B1 59.7(7) . . ? C9 B2 B7 59.6(9) . . ? B3 B2 B7 60.5(9) . . ? B1 B2 B7 107.1(10) . . ? C9 B2 B6 58.1(7) . . ? B3 B2 B6 108.7(9) . . ? B1 B2 B6 60.0(8) . . ? B7 B2 B6 107.7(9) . . ? C2 C3 C4 107.6(9) . . ? C2 C3 Mo1 73.4(5) . . ? C4 C3 Mo1 72.4(5) . . ? B1 B3 B2 60.2(8) . . ? B1 B3 B7 107.3(9) . . ? B2 B3 B7 60.3(10) . . ? B1 B3 B4 60.5(6) . . ? B2 B3 B4 107.9(8) . . ? B7 B3 B4 105.0(9) . . ? B1 B3 B8 106.7(8) . . ? B2 B3 B8 106.8(9) . . ? B7 B3 B8 58.1(9) . . ? B4 B3 B8 58.2(7) . . ? C5 C4 C3 107.5(8) . . ? C5 C4 Mo1 74.4(5) . . ? C3 C4 Mo1 71.2(5) . . ? B8 B4 B5 107.7(8) . . ? B8 B4 B1 108.4(9) . . ? B5 B4 B1 60.6(6) . . ? B8 B4 B3 62.1(8) . . ? B5 B4 B3 108.0(8) . . ? B1 B4 B3 58.7(7) . . ? B8 B4 B10 60.3(8) . . ? B5 B4 B10 59.3(6) . . ? B1 B4 B10 108.2(7) . . ? B3 B4 B10 109.9(8) . . ? C1 C5 C4 108.5(8) . . ? C1 C5 Mo1 73.2(5) . . ? C4 C5 Mo1 70.2(5) . . ? B10 B5 B4 61.3(6) . . ? B10 B5 B11 60.0(6) . . ? B4 B5 B11 108.3(8) . . ? B10 B5 B6 109.8(8) . . ? B4 B5 B6 108.8(8) . . ? B11 B5 B6 60.4(6) . . ? B10 B5 B1 109.6(8) . . ? B4 B5 B1 60.2(6) . . ? B11 B5 B1 107.6(8) . . ? B6 B5 B1 59.8(6) . . ? O1 C6 Mo1 175.9(8) . . ? C9 B6 B1 103.3(8) . . ? C9 B6 B5 103.7(8) . . ? B1 B6 B5 60.3(6) . . ? C9 B6 B11 58.3(6) . . ? B1 B6 B11 107.3(7) . . ? B5 B6 B11 59.5(6) . . ? C9 B6 B2 57.7(8) . . ? B1 B6 B2 58.9(7) . . ? B5 B6 B2 106.6(8) . . ? B11 B6 B2 106.2(10) . . ? O2 C7 Mo1 177.6(9) . . ? B2 C9 B6 64.2(9) . . ? B2 C9 B11 115.8(9) . . ? B6 C9 B11 63.5(7) . . ? B2 C9 B7 62.7(9) . . ? B6 C9 B7 115.1(8) . . ? B11 C9 B7 112.0(10) . . ? B2 C9 B9 113.4(9) . . ? B6 C9 B9 113.9(8) . . ? B11 C9 B9 61.0(7) . . ? B7 C9 B9 60.9(9) . . ? O3 C8 Mo1 175.1(8) . . ? C9 B7 B8 106.1(10) . . ? C9 B7 B9 60.5(8) . . ? B8 B7 B9 59.9(9) . . ? C9 B7 B2 57.7(8) . . ? B8 B7 B2 109.2(9) . . ? B9 B7 B2 108.9(10) . . ? C9 B7 B3 104.3(9) . . ? B8 B7 B3 62.3(8) . . ? B9 B7 B3 109.9(10) . . ? B2 B7 B3 59.1(8) . . ? C9 B11 B9 61.1(8) . . ? C9 B11 B10 106.8(8) . . ? B9 B11 B10 59.8(8) . . ? C9 B11 B5 104.0(7) . . ? B9 B11 B5 107.1(8) . . ? B10 B11 B5 59.7(6) . . ? C9 B11 B6 58.2(8) . . ? B9 B11 B6 109.6(9) . . ? B10 B11 B6 109.2(7) . . ? B5 B11 B6 60.0(7) . . ? B7 B8 B9 60.3(9) . . ? B7 B8 B4 107.4(10) . . ? B9 B8 B4 108.1(9) . . ? B7 B8 B10 107.9(9) . . ? B9 B8 B10 59.4(7) . . ? B4 B8 B10 61.0(7) . . ? B7 B8 B3 59.6(8) . . ? B9 B8 B3 108.1(11) . . ? B4 B8 B3 59.7(7) . . ? B10 B8 B3 108.6(8) . . ? B9 B10 B5 107.6(9) . . ? B9 B10 B11 59.8(7) . . ? B5 B10 B11 60.3(6) . . ? B9 B10 B8 59.4(8) . . ? B5 B10 B8 106.5(8) . . ? B11 B10 B8 106.9(9) . . ? B9 B10 B4 106.3(9) . . ? B5 B10 B4 59.4(6) . . ? B11 B10 B4 107.0(7) . . ? B8 B10 B4 58.7(7) . . ? B11 B9 B8 108.8(9) . . ? B11 B9 B10 60.5(7) . . ? B8 B9 B10 61.2(8) . . ? B11 B9 C9 57.9(7) . . ? B8 B9 C9 104.6(10) . . ? B10 B9 C9 104.8(9) . . ? B11 B9 B7 107.5(11) . . ? B8 B9 B7 59.8(9) . . ? B10 B9 B7 108.8(9) . . ? C9 B9 B7 58.6(9) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Ag1 I1 Ag1 B1 -106.3(3) 3 . . . ? Mo1 I1 Ag1 B1 -1.0(3) . . . . ? Ag1 I1 Ag1 I1 37.44(4) 3 . . 3 ? Mo1 I1 Ag1 I1 142.71(3) . . . 3 ? Mo1 I1 Ag1 Ag1 105.28(4) . . . 3 ? Ag1 I1 Mo1 C6 -176.8(3) 3 . . . ? Ag1 I1 Mo1 C6 100.3(3) . . . . ? Ag1 I1 Mo1 C7 -117.1(4) 3 . . . ? Ag1 I1 Mo1 C7 160.0(4) . . . . ? Ag1 I1 Mo1 C8 -55.9(3) 3 . . . ? Ag1 I1 Mo1 C8 -138.7(3) . . . . ? Ag1 I1 Mo1 C3 98.8(3) 3 . . . ? Ag1 I1 Mo1 C3 15.9(3) . . . . ? Ag1 I1 Mo1 C4 47.7(5) 3 . . . ? Ag1 I1 Mo1 C4 -35.2(5) . . . . ? Ag1 I1 Mo1 C2 89.5(2) 3 . . . ? Ag1 I1 Mo1 C2 6.6(2) . . . . ? Ag1 I1 Mo1 C5 31.2(3) 3 . . . ? Ag1 I1 Mo1 C5 -51.7(3) . . . . ? Ag1 I1 Mo1 C1 55.0(2) 3 . . . ? Ag1 I1 Mo1 C1 -27.9(2) . . . . ? C6 Mo1 C1 C5 151.5(6) . . . . ? C7 Mo1 C1 C5 32.4(9) . . . . ? C8 Mo1 C1 C5 -63.2(6) . . . . ? C3 Mo1 C1 C5 80.2(6) . . . . ? C4 Mo1 C1 C5 37.3(6) . . . . ? C2 Mo1 C1 C5 118.0(8) . . . . ? I1 Mo1 C1 C5 -137.8(6) . . . . ? C6 Mo1 C1 C2 33.5(7) . . . . ? C7 Mo1 C1 C2 -85.6(8) . . . . ? C8 Mo1 C1 C2 178.7(5) . . . . ? C3 Mo1 C1 C2 -37.8(5) . . . . ? C4 Mo1 C1 C2 -80.8(6) . . . . ? C5 Mo1 C1 C2 -118.0(8) . . . . ? I1 Mo1 C1 C2 104.2(5) . . . . ? I1 Ag1 B1 B3 53.5(7) 3 . . . ? I1 Ag1 B1 B3 174.1(5) . . . . ? Ag1 Ag1 B1 B3 119.6(5) 3 . . . ? I1 Ag1 B1 B2 0.8(10) 3 . . . ? I1 Ag1 B1 B2 121.4(8) . . . . ? Ag1 Ag1 B1 B2 66.9(9) 3 . . . ? I1 Ag1 B1 B6 -64(2) 3 . . . ? I1 Ag1 B1 B6 57(2) . . . . ? Ag1 Ag1 B1 B6 2(2) 3 . . . ? I1 Ag1 B1 B4 112.5(6) 3 . . . ? I1 Ag1 B1 B4 -126.9(5) . . . . ? Ag1 Ag1 B1 B4 178.6(5) 3 . . . ? I1 Ag1 B1 B5 160.6(8) 3 . . . ? I1 Ag1 B1 B5 -78.8(10) . . . . ? Ag1 Ag1 B1 B5 -133.3(9) 3 . . . ? C5 C1 C2 C3 0.4(10) . . . . ? Mo1 C1 C2 C3 63.5(6) . . . . ? C5 C1 C2 Mo1 -63.2(6) . . . . ? C6 Mo1 C2 C3 91.2(6) . . . . ? C7 Mo1 C2 C3 13.2(8) . . . . ? C8 Mo1 C2 C3 -117.5(7) . . . . ? C4 Mo1 C2 C3 -38.5(6) . . . . ? C5 Mo1 C2 C3 -80.1(6) . . . . ? C1 Mo1 C2 C3 -115.4(8) . . . . ? I1 Mo1 C2 C3 167.8(5) . . . . ? C6 Mo1 C2 C1 -153.4(6) . . . . ? C7 Mo1 C2 C1 128.7(6) . . . . ? C8 Mo1 C2 C1 -2.1(9) . . . . ? C3 Mo1 C2 C1 115.4(8) . . . . ? C4 Mo1 C2 C1 76.9(6) . . . . ? C5 Mo1 C2 C1 35.3(5) . . . . ? I1 Mo1 C2 C1 -76.8(5) . . . . ? B3 B1 B2 C9 101.3(12) . . . . ? B6 B1 B2 C9 -38.8(9) . . . . ? B4 B1 B2 C9 62.5(12) . . . . ? B5 B1 B2 C9 -0.2(14) . . . . ? Ag1 B1 B2 C9 166.1(8) . . . . ? B6 B1 B2 B3 -140.1(9) . . . . ? B4 B1 B2 B3 -38.8(8) . . . . ? B5 B1 B2 B3 -101.5(9) . . . . ? Ag1 B1 B2 B3 64.7(7) . . . . ? B3 B1 B2 B7 39.2(9) . . . . ? B6 B1 B2 B7 -100.9(9) . . . . ? B4 B1 B2 B7 0.4(11) . . . . ? B5 B1 B2 B7 -62.3(11) . . . . ? Ag1 B1 B2 B7 103.9(8) . . . . ? B3 B1 B2 B6 140.1(9) . . . . ? B4 B1 B2 B6 101.3(8) . . . . ? B5 B1 B2 B6 38.6(9) . . . . ? Ag1 B1 B2 B6 -155.1(7) . . . . ? C1 C2 C3 C4 -0.6(10) . . . . ? Mo1 C2 C3 C4 64.9(6) . . . . ? C1 C2 C3 Mo1 -65.4(6) . . . . ? C6 Mo1 C3 C2 -92.0(6) . . . . ? C7 Mo1 C3 C2 -169.5(6) . . . . ? C8 Mo1 C3 C2 117.2(7) . . . . ? C4 Mo1 C3 C2 115.2(8) . . . . ? C5 Mo1 C3 C2 77.6(6) . . . . ? C1 Mo1 C3 C2 37.8(5) . . . . ? I1 Mo1 C3 C2 -16.0(7) . . . . ? C6 Mo1 C3 C4 152.9(6) . . . . ? C7 Mo1 C3 C4 75.3(6) . . . . ? C8 Mo1 C3 C4 2.0(9) . . . . ? C2 Mo1 C3 C4 -115.2(8) . . . . ? C5 Mo1 C3 C4 -37.6(5) . . . . ? C1 Mo1 C3 C4 -77.3(6) . . . . ? I1 Mo1 C3 C4 -131.2(5) . . . . ? B6 B1 B3 B2 36.7(9) . . . . ? B4 B1 B3 B2 136.9(8) . . . . ? B5 B1 B3 B2 100.6(9) . . . . ? Ag1 B1 B3 B2 -120.7(7) . . . . ? B2 B1 B3 B7 -39.1(10) . . . . ? B6 B1 B3 B7 -2.4(12) . . . . ? B4 B1 B3 B7 97.8(10) . . . . ? B5 B1 B3 B7 61.5(12) . . . . ? Ag1 B1 B3 B7 -159.9(9) . . . . ? B2 B1 B3 B4 -136.9(8) . . . . ? B6 B1 B3 B4 -100.2(8) . . . . ? B5 B1 B3 B4 -36.3(7) . . . . ? Ag1 B1 B3 B4 102.3(5) . . . . ? B2 B1 B3 B8 -100.2(10) . . . . ? B6 B1 B3 B8 -63.5(11) . . . . ? B4 B1 B3 B8 36.7(8) . . . . ? B5 B1 B3 B8 0.4(11) . . . . ? Ag1 B1 B3 B8 139.1(8) . . . . ? C9 B2 B3 B1 -97.2(11) . . . . ? B7 B2 B3 B1 -136.1(9) . . . . ? B6 B2 B3 B1 -35.9(9) . . . . ? C9 B2 B3 B7 38.9(10) . . . . ? B1 B2 B3 B7 136.1(9) . . . . ? B6 B2 B3 B7 100.2(11) . . . . ? C9 B2 B3 B4 -58.6(13) . . . . ? B1 B2 B3 B4 38.6(8) . . . . ? B7 B2 B3 B4 -97.5(10) . . . . ? B6 B2 B3 B4 2.7(14) . . . . ? C9 B2 B3 B8 2.7(14) . . . . ? B1 B2 B3 B8 99.9(9) . . . . ? B7 B2 B3 B8 -36.2(10) . . . . ? B6 B2 B3 B8 64.0(13) . . . . ? C2 C3 C4 C5 0.6(10) . . . . ? Mo1 C3 C4 C5 66.1(6) . . . . ? C2 C3 C4 Mo1 -65.5(6) . . . . ? C6 Mo1 C4 C5 -149.5(6) . . . . ? C7 Mo1 C4 C5 141.3(6) . . . . ? C8 Mo1 C4 C5 66.1(6) . . . . ? C3 Mo1 C4 C5 -115.1(8) . . . . ? C2 Mo1 C4 C5 -77.5(6) . . . . ? C1 Mo1 C4 C5 -35.7(5) . . . . ? I1 Mo1 C4 C5 -27.1(8) . . . . ? C6 Mo1 C4 C3 -34.3(7) . . . . ? C7 Mo1 C4 C3 -103.6(6) . . . . ? C8 Mo1 C4 C3 -178.8(5) . . . . ? C2 Mo1 C4 C3 37.7(5) . . . . ? C5 Mo1 C4 C3 115.1(8) . . . . ? C1 Mo1 C4 C3 79.4(6) . . . . ? I1 Mo1 C4 C3 88.0(7) . . . . ? B3 B1 B4 B8 -38.9(8) . . . . ? B2 B1 B4 B8 -0.4(11) . . . . ? B6 B1 B4 B8 64.3(11) . . . . ? B5 B1 B4 B8 100.4(9) . . . . ? Ag1 B1 B4 B8 -114.2(7) . . . . ? B3 B1 B4 B5 -139.2(8) . . . . ? B2 B1 B4 B5 -100.7(8) . . . . ? B6 B1 B4 B5 -36.0(8) . . . . ? Ag1 B1 B4 B5 145.5(7) . . . . ? B2 B1 B4 B3 38.5(8) . . . . ? B6 B1 B4 B3 103.2(10) . . . . ? B5 B1 B4 B3 139.2(8) . . . . ? Ag1 B1 B4 B3 -75.3(6) . . . . ? B3 B1 B4 B10 -102.7(9) . . . . ? B2 B1 B4 B10 -64.2(10) . . . . ? B6 B1 B4 B10 0.5(12) . . . . ? B5 B1 B4 B10 36.5(8) . . . . ? Ag1 B1 B4 B10 -178.1(7) . . . . ? B1 B3 B4 B8 137.6(8) . . . . ? B2 B3 B4 B8 99.1(10) . . . . ? B7 B3 B4 B8 36.0(9) . . . . ? B1 B3 B4 B5 36.7(7) . . . . ? B2 B3 B4 B5 -1.8(12) . . . . ? B7 B3 B4 B5 -64.9(11) . . . . ? B8 B3 B4 B5 -100.9(8) . . . . ? B2 B3 B4 B1 -38.5(9) . . . . ? B7 B3 B4 B1 -101.7(10) . . . . ? B8 B3 B4 B1 -137.6(8) . . . . ? B1 B3 B4 B10 99.7(8) . . . . ? B2 B3 B4 B10 61.2(12) . . . . ? B7 B3 B4 B10 -1.9(12) . . . . ? B8 B3 B4 B10 -37.9(8) . . . . ? C2 C1 C5 C4 0.0(10) . . . . ? Mo1 C1 C5 C4 -61.8(6) . . . . ? C2 C1 C5 Mo1 61.8(6) . . . . ? C3 C4 C5 C1 -0.3(10) . . . . ? Mo1 C4 C5 C1 63.6(6) . . . . ? C3 C4 C5 Mo1 -64.0(6) . . . . ? C6 Mo1 C5 C1 -55.9(11) . . . . ? C7 Mo1 C5 C1 -159.1(6) . . . . ? C8 Mo1 C5 C1 122.6(6) . . . . ? C3 Mo1 C5 C1 -78.8(6) . . . . ? C4 Mo1 C5 C1 -117.4(8) . . . . ? C2 Mo1 C5 C1 -37.0(6) . . . . ? I1 Mo1 C5 C1 46.3(6) . . . . ? C6 Mo1 C5 C4 61.4(10) . . . . ? C7 Mo1 C5 C4 -41.7(7) . . . . ? C8 Mo1 C5 C4 -120.0(6) . . . . ? C3 Mo1 C5 C4 38.6(6) . . . . ? C2 Mo1 C5 C4 80.4(6) . . . . ? C1 Mo1 C5 C4 117.4(8) . . . . ? I1 Mo1 C5 C4 163.7(5) . . . . ? B8 B4 B5 B10 37.4(10) . . . . ? B1 B4 B5 B10 138.9(8) . . . . ? B3 B4 B5 B10 103.0(9) . . . . ? B8 B4 B5 B11 -1.3(12) . . . . ? B1 B4 B5 B11 100.2(8) . . . . ? B3 B4 B5 B11 64.3(10) . . . . ? B10 B4 B5 B11 -38.7(8) . . . . ? B8 B4 B5 B6 -65.4(11) . . . . ? B1 B4 B5 B6 36.1(8) . . . . ? B3 B4 B5 B6 0.1(11) . . . . ? B10 B4 B5 B6 -102.8(9) . . . . ? B8 B4 B5 B1 -101.5(10) . . . . ? B3 B4 B5 B1 -36.0(8) . . . . ? B10 B4 B5 B1 -138.9(8) . . . . ? B3 B1 B5 B10 -0.7(11) . . . . ? B2 B1 B5 B10 62.9(11) . . . . ? B6 B1 B5 B10 102.1(9) . . . . ? B4 B1 B5 B10 -37.7(8) . . . . ? Ag1 B1 B5 B10 -97.2(11) . . . . ? B3 B1 B5 B4 37.0(7) . . . . ? B2 B1 B5 B4 100.6(10) . . . . ? B6 B1 B5 B4 139.8(9) . . . . ? Ag1 B1 B5 B4 -59.5(10) . . . . ? B3 B1 B5 B11 -64.4(10) . . . . ? B2 B1 B5 B11 -0.8(12) . . . . ? B6 B1 B5 B11 38.4(8) . . . . ? B4 B1 B5 B11 -101.4(9) . . . . ? Ag1 B1 B5 B11 -160.9(8) . . . . ? B3 B1 B5 B6 -102.8(10) . . . . ? B2 B1 B5 B6 -39.2(10) . . . . ? B4 B1 B5 B6 -139.8(9) . . . . ? Ag1 B1 B5 B6 160.7(11) . . . . ? C7 Mo1 C6 O1 100(12) . . . . ? C8 Mo1 C6 O1 170(12) . . . . ? C3 Mo1 C6 O1 8(12) . . . . ? C4 Mo1 C6 O1 27(13) . . . . ? C2 Mo1 C6 O1 -28(12) . . . . ? C5 Mo1 C6 O1 -12(13) . . . . ? C1 Mo1 C6 O1 -47(13) . . . . ? I1 Mo1 C6 O1 -123(12) . . . . ? B3 B1 B6 C9 2.1(11) . . . . ? B2 B1 B6 C9 38.3(9) . . . . ? B4 B1 B6 C9 -62.7(10) . . . . ? B5 B1 B6 C9 -98.4(8) . . . . ? Ag1 B1 B6 C9 113.7(18) . . . . ? B3 B1 B6 B5 100.5(9) . . . . ? B2 B1 B6 B5 136.7(10) . . . . ? B4 B1 B6 B5 35.7(8) . . . . ? Ag1 B1 B6 B5 -148(2) . . . . ? B3 B1 B6 B11 62.6(11) . . . . ? B2 B1 B6 B11 98.8(11) . . . . ? B4 B1 B6 B11 -2.1(12) . . . . ? B5 B1 B6 B11 -37.9(8) . . . . ? Ag1 B1 B6 B11 174.2(16) . . . . ? B3 B1 B6 B2 -36.2(10) . . . . ? B4 B1 B6 B2 -101.0(10) . . . . ? B5 B1 B6 B2 -136.7(10) . . . . ? Ag1 B1 B6 B2 75(2) . . . . ? B10 B5 B6 C9 -4.0(10) . . . . ? B4 B5 B6 C9 61.4(9) . . . . ? B11 B5 B6 C9 -39.5(6) . . . . ? B1 B5 B6 C9 97.6(8) . . . . ? B10 B5 B6 B1 -101.7(8) . . . . ? B4 B5 B6 B1 -36.3(8) . . . . ? B11 B5 B6 B1 -137.1(8) . . . . ? B10 B5 B6 B11 35.5(8) . . . . ? B4 B5 B6 B11 100.9(9) . . . . ? B1 B5 B6 B11 137.1(8) . . . . ? B10 B5 B6 B2 -63.9(11) . . . . ? B4 B5 B6 B2 1.5(12) . . . . ? B11 B5 B6 B2 -99.4(10) . . . . ? B1 B5 B6 B2 37.8(9) . . . . ? B3 B2 B6 C9 -98.7(12) . . . . ? B1 B2 B6 C9 -134.4(9) . . . . ? B7 B2 B6 C9 -34.6(9) . . . . ? C9 B2 B6 B1 134.4(9) . . . . ? B3 B2 B6 B1 35.8(9) . . . . ? B7 B2 B6 B1 99.9(10) . . . . ? C9 B2 B6 B5 96.0(9) . . . . ? B3 B2 B6 B5 -2.6(13) . . . . ? B1 B2 B6 B5 -38.4(9) . . . . ? B7 B2 B6 B5 61.5(11) . . . . ? C9 B2 B6 B11 33.7(8) . . . . ? B3 B2 B6 B11 -65.0(12) . . . . ? B1 B2 B6 B11 -100.7(9) . . . . ? B7 B2 B6 B11 -0.9(11) . . . . ? C6 Mo1 C7 O2 -144(25) . . . . ? C8 Mo1 C7 O2 96(24) . . . . ? C3 Mo1 C7 O2 -50(24) . . . . ? C4 Mo1 C7 O2 -14(24) . . . . ? C2 Mo1 C7 O2 -57(25) . . . . ? C5 Mo1 C7 O2 8(25) . . . . ? C1 Mo1 C7 O2 -10(25) . . . . ? I1 Mo1 C7 O2 157(24) . . . . ? B3 B2 C9 B6 101.9(11) . . . . ? B1 B2 C9 B6 39.7(9) . . . . ? B7 B2 C9 B6 141.2(9) . . . . ? B3 B2 C9 B11 63.4(15) . . . . ? B1 B2 C9 B11 1.2(15) . . . . ? B7 B2 C9 B11 102.7(12) . . . . ? B6 B2 C9 B11 -38.5(10) . . . . ? B3 B2 C9 B7 -39.3(10) . . . . ? B1 B2 C9 B7 -101.5(11) . . . . ? B6 B2 C9 B7 -141.2(9) . . . . ? B3 B2 C9 B9 -4.4(15) . . . . ? B1 B2 C9 B9 -66.7(14) . . . . ? B7 B2 C9 B9 34.9(10) . . . . ? B6 B2 C9 B9 -106.3(10) . . . . ? B1 B6 C9 B2 -38.9(8) . . . . ? B5 B6 C9 B2 -101.1(8) . . . . ? B11 B6 C9 B2 -141.2(9) . . . . ? B1 B6 C9 B11 102.3(8) . . . . ? B5 B6 C9 B11 40.1(7) . . . . ? B2 B6 C9 B11 141.2(9) . . . . ? B1 B6 C9 B7 -1.0(13) . . . . ? B5 B6 C9 B7 -63.1(12) . . . . ? B11 B6 C9 B7 -103.3(11) . . . . ? B2 B6 C9 B7 37.9(10) . . . . ? B1 B6 C9 B9 66.7(10) . . . . ? B5 B6 C9 B9 4.5(10) . . . . ? B11 B6 C9 B9 -35.6(8) . . . . ? B2 B6 C9 B9 105.6(10) . . . . ? C6 Mo1 C8 O3 -170(10) . . . . ? C7 Mo1 C8 O3 -100(10) . . . . ? C3 Mo1 C8 O3 -23(10) . . . . ? C4 Mo1 C8 O3 -21(10) . . . . ? C2 Mo1 C8 O3 42(10) . . . . ? C5 Mo1 C8 O3 11(10) . . . . ? C1 Mo1 C8 O3 40(10) . . . . ? I1 Mo1 C8 O3 122(10) . . . . ? B2 C9 B7 B8 102.8(10) . . . . ? B6 C9 B7 B8 64.3(13) . . . . ? B11 C9 B7 B8 -5.7(13) . . . . ? B9 C9 B7 B8 -40.2(9) . . . . ? B2 C9 B7 B9 143.1(10) . . . . ? B6 C9 B7 B9 104.6(10) . . . . ? B11 C9 B7 B9 34.5(9) . . . . ? B6 C9 B7 B2 -38.5(10) . . . . ? B11 C9 B7 B2 -108.6(10) . . . . ? B9 C9 B7 B2 -143.1(10) . . . . ? B2 C9 B7 B3 38.1(9) . . . . ? B6 C9 B7 B3 -0.5(15) . . . . ? B11 C9 B7 B3 -70.5(13) . . . . ? B9 C9 B7 B3 -105.0(11) . . . . ? B3 B2 B7 C9 135.9(10) . . . . ? B1 B2 B7 C9 97.1(9) . . . . ? B6 B2 B7 C9 33.9(8) . . . . ? C9 B2 B7 B8 -97.3(10) . . . . ? B3 B2 B7 B8 38.6(9) . . . . ? B1 B2 B7 B8 -0.2(12) . . . . ? B6 B2 B7 B8 -63.4(12) . . . . ? C9 B2 B7 B9 -33.6(9) . . . . ? B3 B2 B7 B9 102.3(11) . . . . ? B1 B2 B7 B9 63.5(12) . . . . ? B6 B2 B7 B9 0.4(13) . . . . ? C9 B2 B7 B3 -135.9(10) . . . . ? B1 B2 B7 B3 -38.8(8) . . . . ? B6 B2 B7 B3 -101.9(10) . . . . ? B1 B3 B7 C9 1.7(14) . . . . ? B2 B3 B7 C9 -37.4(10) . . . . ? B4 B3 B7 C9 64.9(12) . . . . ? B8 B3 B7 C9 101.0(11) . . . . ? B1 B3 B7 B8 -99.2(10) . . . . ? B2 B3 B7 B8 -138.3(10) . . . . ? B4 B3 B7 B8 -36.0(9) . . . . ? B1 B3 B7 B9 -61.6(14) . . . . ? B2 B3 B7 B9 -100.7(12) . . . . ? B4 B3 B7 B9 1.6(14) . . . . ? B8 B3 B7 B9 37.6(10) . . . . ? B1 B3 B7 B2 39.1(9) . . . . ? B4 B3 B7 B2 102.3(9) . . . . ? B8 B3 B7 B2 138.3(10) . . . . ? B2 C9 B11 B9 -103.7(12) . . . . ? B6 C9 B11 B9 -142.5(8) . . . . ? B7 C9 B11 B9 -34.4(9) . . . . ? B2 C9 B11 B10 -63.8(13) . . . . ? B6 C9 B11 B10 -102.5(8) . . . . ? B7 C9 B11 B10 5.5(12) . . . . ? B9 C9 B11 B10 40.0(8) . . . . ? B2 C9 B11 B5 -1.7(14) . . . . ? B6 C9 B11 B5 -40.4(7) . . . . ? B7 C9 B11 B5 67.6(11) . . . . ? B9 C9 B11 B5 102.1(8) . . . . ? B2 C9 B11 B6 38.8(11) . . . . ? B7 C9 B11 B6 108.1(9) . . . . ? B9 C9 B11 B6 142.5(8) . . . . ? B10 B5 B11 C9 -101.4(9) . . . . ? B4 B5 B11 C9 -62.1(10) . . . . ? B6 B5 B11 C9 39.5(8) . . . . ? B1 B5 B11 C9 1.4(10) . . . . ? B10 B5 B11 B9 -37.8(10) . . . . ? B4 B5 B11 B9 1.5(12) . . . . ? B6 B5 B11 B9 103.2(10) . . . . ? B1 B5 B11 B9 65.1(11) . . . . ? B4 B5 B11 B10 39.3(8) . . . . ? B6 B5 B11 B10 140.9(9) . . . . ? B1 B5 B11 B10 102.9(9) . . . . ? B10 B5 B11 B6 -140.9(9) . . . . ? B4 B5 B11 B6 -101.7(9) . . . . ? B1 B5 B11 B6 -38.1(8) . . . . ? B1 B6 B11 C9 -95.2(10) . . . . ? B5 B6 B11 C9 -133.4(8) . . . . ? B2 B6 B11 C9 -33.4(8) . . . . ? C9 B6 B11 B9 34.5(8) . . . . ? B1 B6 B11 B9 -60.7(12) . . . . ? B5 B6 B11 B9 -98.9(9) . . . . ? B2 B6 B11 B9 1.0(11) . . . . ? C9 B6 B11 B10 98.2(9) . . . . ? B1 B6 B11 B10 3.1(12) . . . . ? B5 B6 B11 B10 -35.2(8) . . . . ? B2 B6 B11 B10 64.8(11) . . . . ? C9 B6 B11 B5 133.4(8) . . . . ? B1 B6 B11 B5 38.2(8) . . . . ? B2 B6 B11 B5 100.0(8) . . . . ? C9 B7 B8 B9 40.5(9) . . . . ? B2 B7 B8 B9 101.3(10) . . . . ? B3 B7 B8 B9 138.5(9) . . . . ? C9 B7 B8 B4 -60.7(12) . . . . ? B9 B7 B8 B4 -101.3(10) . . . . ? B2 B7 B8 B4 0.0(13) . . . . ? B3 B7 B8 B4 37.2(8) . . . . ? C9 B7 B8 B10 3.6(12) . . . . ? B9 B7 B8 B10 -37.0(9) . . . . ? B2 B7 B8 B10 64.3(11) . . . . ? B3 B7 B8 B10 101.5(9) . . . . ? C9 B7 B8 B3 -97.9(10) . . . . ? B9 B7 B8 B3 -138.5(9) . . . . ? B2 B7 B8 B3 -37.2(8) . . . . ? B5 B4 B8 B7 64.3(11) . . . . ? B1 B4 B8 B7 0.2(12) . . . . ? B3 B4 B8 B7 -37.1(9) . . . . ? B10 B4 B8 B7 101.2(9) . . . . ? B5 B4 B8 B9 0.6(15) . . . . ? B1 B4 B8 B9 -63.4(14) . . . . ? B3 B4 B8 B9 -100.8(13) . . . . ? B10 B4 B8 B9 37.5(10) . . . . ? B5 B4 B8 B10 -36.9(9) . . . . ? B1 B4 B8 B10 -101.0(9) . . . . ? B3 B4 B8 B10 -138.3(8) . . . . ? B5 B4 B8 B3 101.4(8) . . . . ? B1 B4 B8 B3 37.4(7) . . . . ? B10 B4 B8 B3 138.3(8) . . . . ? B1 B3 B8 B7 100.4(10) . . . . ? B2 B3 B8 B7 37.1(10) . . . . ? B4 B3 B8 B7 138.1(9) . . . . ? B1 B3 B8 B9 63.0(12) . . . . ? B2 B3 B8 B9 -0.2(14) . . . . ? B7 B3 B8 B9 -37.3(10) . . . . ? B4 B3 B8 B9 100.8(10) . . . . ? B1 B3 B8 B4 -37.7(8) . . . . ? B2 B3 B8 B4 -100.9(10) . . . . ? B7 B3 B8 B4 -138.1(9) . . . . ? B1 B3 B8 B10 0.1(12) . . . . ? B2 B3 B8 B10 -63.1(13) . . . . ? B7 B3 B8 B10 -100.3(10) . . . . ? B4 B3 B8 B10 37.8(8) . . . . ? B4 B5 B10 B9 -98.9(9) . . . . ? B11 B5 B10 B9 37.9(7) . . . . ? B6 B5 B10 B9 2.3(11) . . . . ? B1 B5 B10 B9 -61.6(10) . . . . ? B4 B5 B10 B11 -136.8(8) . . . . ? B6 B5 B10 B11 -35.6(7) . . . . ? B1 B5 B10 B11 -99.5(8) . . . . ? B4 B5 B10 B8 -36.4(8) . . . . ? B11 B5 B10 B8 100.3(9) . . . . ? B6 B5 B10 B8 64.7(10) . . . . ? B1 B5 B10 B8 0.8(11) . . . . ? B11 B5 B10 B4 136.8(8) . . . . ? B6 B5 B10 B4 101.1(8) . . . . ? B1 B5 B10 B4 37.2(7) . . . . ? C9 B11 B10 B9 -40.6(9) . . . . ? B5 B11 B10 B9 -137.3(9) . . . . ? B6 B11 B10 B9 -102.0(10) . . . . ? C9 B11 B10 B5 96.7(8) . . . . ? B9 B11 B10 B5 137.3(9) . . . . ? B6 B11 B10 B5 35.3(9) . . . . ? C9 B11 B10 B8 -3.0(11) . . . . ? B9 B11 B10 B8 37.6(9) . . . . ? B5 B11 B10 B8 -99.7(8) . . . . ? B6 B11 B10 B8 -64.4(11) . . . . ? C9 B11 B10 B4 58.7(11) . . . . ? B9 B11 B10 B4 99.3(10) . . . . ? B5 B11 B10 B4 -38.1(8) . . . . ? B6 B11 B10 B4 -2.8(12) . . . . ? B7 B8 B10 B9 37.4(10) . . . . ? B4 B8 B10 B9 137.7(11) . . . . ? B3 B8 B10 B9 100.4(12) . . . . ? B7 B8 B10 B5 -63.6(11) . . . . ? B9 B8 B10 B5 -101.0(10) . . . . ? B4 B8 B10 B5 36.7(8) . . . . ? B3 B8 B10 B5 -0.5(12) . . . . ? B7 B8 B10 B11 -0.4(11) . . . . ? B9 B8 B10 B11 -37.8(9) . . . . ? B4 B8 B10 B11 100.0(9) . . . . ? B3 B8 B10 B11 62.7(11) . . . . ? B7 B8 B10 B4 -100.4(10) . . . . ? B9 B8 B10 B4 -137.7(11) . . . . ? B3 B8 B10 B4 -37.3(8) . . . . ? B8 B4 B10 B9 -37.1(10) . . . . ? B5 B4 B10 B9 101.1(9) . . . . ? B1 B4 B10 B9 64.1(11) . . . . ? B3 B4 B10 B9 1.5(11) . . . . ? B8 B4 B10 B5 -138.2(10) . . . . ? B1 B4 B10 B5 -37.1(8) . . . . ? B3 B4 B10 B5 -99.6(9) . . . . ? B8 B4 B10 B11 -99.8(10) . . . . ? B5 B4 B10 B11 38.5(8) . . . . ? B1 B4 B10 B11 1.4(11) . . . . ? B3 B4 B10 B11 -61.1(11) . . . . ? B5 B4 B10 B8 138.2(10) . . . . ? B1 B4 B10 B8 101.2(10) . . . . ? B3 B4 B10 B8 38.7(9) . . . . ? C9 B11 B9 B8 95.7(12) . . . . ? B10 B11 B9 B8 -38.9(11) . . . . ? B5 B11 B9 B8 -1.1(15) . . . . ? B6 B11 B9 B8 62.4(14) . . . . ? C9 B11 B9 B10 134.6(8) . . . . ? B5 B11 B9 B10 37.7(8) . . . . ? B6 B11 B9 B10 101.3(9) . . . . ? B10 B11 B9 C9 -134.6(8) . . . . ? B5 B11 B9 C9 -96.9(8) . . . . ? B6 B11 B9 C9 -33.3(7) . . . . ? C9 B11 B9 B7 32.5(9) . . . . ? B10 B11 B9 B7 -102.1(9) . . . . ? B5 B11 B9 B7 -64.4(12) . . . . ? B6 B11 B9 B7 -0.8(12) . . . . ? B7 B8 B9 B11 -99.8(13) . . . . ? B4 B8 B9 B11 0.3(17) . . . . ? B10 B8 B9 B11 38.6(10) . . . . ? B3 B8 B9 B11 -62.8(15) . . . . ? B7 B8 B9 B10 -138.4(10) . . . . ? B4 B8 B9 B10 -38.2(10) . . . . ? B3 B8 B9 B10 -101.4(10) . . . . ? B7 B8 B9 C9 -39.3(10) . . . . ? B4 B8 B9 C9 60.9(14) . . . . ? B10 B8 B9 C9 99.1(9) . . . . ? B3 B8 B9 C9 -2.3(13) . . . . ? B4 B8 B9 B7 100.1(12) . . . . ? B10 B8 B9 B7 138.4(10) . . . . ? B3 B8 B9 B7 37.0(10) . . . . ? B5 B10 B9 B11 -38.1(8) . . . . ? B8 B10 B9 B11 -137.3(10) . . . . ? B4 B10 B9 B11 -100.5(8) . . . . ? B5 B10 B9 B8 99.2(9) . . . . ? B11 B10 B9 B8 137.3(10) . . . . ? B4 B10 B9 B8 36.8(9) . . . . ? B5 B10 B9 C9 0.4(10) . . . . ? B11 B10 B9 C9 38.6(7) . . . . ? B8 B10 B9 C9 -98.7(10) . . . . ? B4 B10 B9 C9 -61.9(10) . . . . ? B5 B10 B9 B7 61.8(12) . . . . ? B11 B10 B9 B7 99.9(12) . . . . ? B8 B10 B9 B7 -37.3(10) . . . . ? B4 B10 B9 B7 -0.5(13) . . . . ? B2 C9 B9 B11 107.5(11) . . . . ? B6 C9 B9 B11 36.6(8) . . . . ? B7 C9 B9 B11 143.1(8) . . . . ? B2 C9 B9 B8 4.2(14) . . . . ? B6 C9 B9 B8 -66.7(11) . . . . ? B11 C9 B9 B8 -103.3(10) . . . . ? B7 C9 B9 B8 39.8(9) . . . . ? B2 C9 B9 B10 67.7(12) . . . . ? B6 C9 B9 B10 -3.2(11) . . . . ? B11 C9 B9 B10 -39.8(7) . . . . ? B7 C9 B9 B10 103.3(9) . . . . ? B2 C9 B9 B7 -35.6(10) . . . . ? B6 C9 B9 B7 -106.5(9) . . . . ? B11 C9 B9 B7 -143.1(8) . . . . ? C9 B7 B9 B11 -32.2(8) . . . . ? B8 B7 B9 B11 102.0(10) . . . . ? B2 B7 B9 B11 0.2(13) . . . . ? B3 B7 B9 B11 63.3(14) . . . . ? C9 B7 B9 B8 -134.2(9) . . . . ? B2 B7 B9 B8 -101.7(10) . . . . ? B3 B7 B9 B8 -38.6(10) . . . . ? C9 B7 B9 B10 -96.2(10) . . . . ? B8 B7 B9 B10 38.0(10) . . . . ? B2 B7 B9 B10 -63.8(13) . . . . ? B3 B7 B9 B10 -0.7(15) . . . . ? B8 B7 B9 C9 134.2(9) . . . . ? B2 B7 B9 C9 32.4(9) . . . . ? B3 B7 B9 C9 95.5(12) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A B1 H1A Ag1 1.12 1.97 2.659(10) 116.3 . _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.712 _refine_diff_density_min -1.697 _refine_diff_density_rms 0.179 #===END data_compound3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C9 H11 Ag B11 Br6 I Mo O3' _chemical_formula_weight 1096.26 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' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.2901 2.4595 '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' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.7200(7) _cell_length_b 11.8360(8) _cell_length_c 14.7530(15) _cell_angle_alpha 90.871(5) _cell_angle_beta 96.678(4) _cell_angle_gamma 90.355(5) _cell_volume 1338.7(2) _cell_formula_units_Z 2 _cell_measurement_temperature 170(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12 _cell_measurement_theta_max 18 _exptl_crystal_description Block _exptl_crystal_colour Red _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.720 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 992 _exptl_absorpt_coefficient_mu 11.320 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.982 _exptl_absorpt_correction_T_max 1.012 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _diffrn_ambient_temperature 170(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '4-circle diffractometer' _diffrn_measurement_method 'scintillation counter' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11052 _diffrn_reflns_av_R_equivalents 0.0967 _diffrn_reflns_av_sigmaI/netI 0.1156 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.56 _diffrn_reflns_theta_max 25.17 _reflns_number_total 4679 _reflns_number_gt 3236 _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 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _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^)+(0.1718P)^2^+29.3778P] 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 4679 _refine_ls_number_parameters 295 _refine_ls_number_restraints 115 _refine_ls_R_factor_all 0.1324 _refine_ls_R_factor_gt 0.0917 _refine_ls_wR_factor_ref 0.2844 _refine_ls_wR_factor_gt 0.2541 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 0.998 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group I1 I 0.3111(2) 0.95663(11) 0.59339(11) 0.0413(4) Uani 1 1 d . . . Ag1 Ag 0.3426(3) 0.93128(16) 0.40853(14) 0.0570(6) Uani 1 1 d . . . Mo1 Mo 0.3272(2) 0.73651(14) 0.67198(14) 0.0346(5) Uani 1 1 d . . . Br1 Br 0.4319(2) 0.75786(17) 0.29148(15) 0.0349(5) Uani 1 1 d . . . Br2 Br 0.1356(3) 1.01771(16) 0.25992(17) 0.0403(6) Uani 1 1 d . . . Br3 Br 0.0037(3) 0.76490(18) 0.39283(16) 0.0419(6) Uani 1 1 d . . . Br4 Br 0.3665(3) 0.90484(18) 0.05863(16) 0.0398(6) Uani 1 1 d . . . Br5 Br 0.3706(3) 0.58633(18) 0.06554(16) 0.0379(6) Uani 1 1 d . . . Br6 Br 0.1435(3) 0.49444(17) 0.27633(18) 0.0436(6) Uani 1 1 d . . . O1 O -0.071(3) 0.7576(16) 0.6090(13) 0.061(5) Uani 1 1 d . . . O2 O 0.570(2) 0.7043(19) 0.5155(12) 0.066(6) Uani 1 1 d . . . O3 O 0.243(4) 0.4981(19) 0.5909(19) 0.098(8) Uani 1 1 d . . . B2 B -0.149(3) 0.822(2) 0.1809(19) 0.037(4) Uani 1 1 d U . . H2 H -0.2613 0.8719 0.2018 0.044 Uiso 1 1 calc R . . B3 B -0.149(3) 0.672(2) 0.1870(19) 0.037(4) Uani 1 1 d U . . H3 H -0.2582 0.6239 0.2125 0.044 Uiso 1 1 calc R . . B4 B -0.039(3) 0.621(2) 0.0967(19) 0.037(4) Uani 1 1 d U . . H4 H -0.0767 0.5374 0.0630 0.045 Uiso 1 1 calc R . . B5 B 0.017(3) 0.737(2) 0.032(2) 0.045(4) Uani 1 1 d U . . H5 H 0.0147 0.7278 -0.0440 0.054 Uiso 1 1 calc R . . B6 B -0.042(3) 0.865(2) 0.088(2) 0.045(5) Uani 1 1 d U . . H6 H -0.0815 0.9434 0.0488 0.054 Uiso 1 1 calc R . . B7 B 0.072(3) 0.6306(19) 0.2046(18) 0.032(4) Uani 1 1 d U . . B8 B 0.180(3) 0.671(2) 0.1122(17) 0.034(4) Uani 1 1 d U . . B9 B 0.178(3) 0.824(2) 0.1044(19) 0.040(4) Uani 1 1 d U . . B10 B 0.075(3) 0.8710(18) 0.2021(18) 0.031(4) Uani 1 1 d U . . B11 B 0.009(3) 0.7557(19) 0.2601(18) 0.031(3) Uani 1 1 d U . . B12 B 0.215(3) 0.7518(17) 0.2154(16) 0.024(3) Uani 1 1 d U . . C1 C -0.157(3) 0.744(2) 0.0882(17) 0.042(6) Uani 1 1 d . . . H1 H -0.2856 0.7424 0.0441 0.051 Uiso 1 1 calc R . . C2 C 0.480(4) 0.7193(19) 0.566(2) 0.054(7) Uani 1 1 d . . . C3 C 0.295(3) 0.678(2) 0.8147(16) 0.048(6) Uani 1 1 d . . . H3 H 0.2027 0.6269 0.8234 0.058 Uiso 1 1 calc R . . C4 C 0.283(3) 0.792(2) 0.8175(16) 0.044(6) Uani 1 1 d . . . H4 H 0.1837 0.8348 0.8277 0.053 Uiso 1 1 calc R . . C5 C 0.459(4) 0.837(3) 0.8013(18) 0.064(8) Uani 1 1 d . . . H5 H 0.4919 0.9143 0.7990 0.077 Uiso 1 1 calc R . . C6 C 0.561(3) 0.745(2) 0.7905(19) 0.053(7) Uani 1 1 d . . . H6 H 0.6797 0.7464 0.7798 0.064 Uiso 1 1 calc R . . C7 C 0.455(3) 0.647(2) 0.7981(19) 0.053(7) Uani 1 1 d . . . H7 H 0.4927 0.5709 0.7922 0.063 Uiso 1 1 calc R . . C8 C 0.074(3) 0.7490(19) 0.6301(18) 0.043(6) Uani 1 1 d . . . C9 C 0.274(4) 0.578(2) 0.621(2) 0.070(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 I1 0.0466(9) 0.0307(7) 0.0486(10) 0.0039(6) 0.0140(7) -0.0024(6) Ag1 0.0756(15) 0.0469(11) 0.0486(12) -0.0027(9) 0.0077(10) 0.0007(10) Mo1 0.0298(10) 0.0293(9) 0.0474(12) 0.0039(8) 0.0153(8) -0.0002(7) Br1 0.0202(10) 0.0385(11) 0.0464(14) -0.0016(9) 0.0059(9) 0.0014(8) Br2 0.0338(11) 0.0250(10) 0.0649(16) 0.0013(9) 0.0166(11) 0.0008(8) Br3 0.0405(13) 0.0431(12) 0.0458(14) -0.0004(10) 0.0215(10) -0.0036(10) Br4 0.0281(11) 0.0429(12) 0.0513(14) 0.0119(10) 0.0160(10) -0.0031(9) Br5 0.0269(11) 0.0411(12) 0.0476(14) -0.0077(10) 0.0136(9) 0.0025(9) Br6 0.0408(13) 0.0289(11) 0.0644(16) 0.0078(10) 0.0190(11) 0.0008(9) O1 0.055(12) 0.071(12) 0.055(12) -0.004(9) -0.007(9) -0.007(9) O2 0.048(11) 0.124(17) 0.032(10) -0.007(10) 0.030(9) 0.007(11) O3 0.12(2) 0.048(13) 0.12(2) -0.038(13) 0.012(16) 0.020(13) B2 0.012(6) 0.034(8) 0.064(13) 0.001(9) 0.006(7) 0.004(6) B3 0.021(6) 0.033(8) 0.057(13) -0.004(8) 0.011(8) -0.002(6) B4 0.018(8) 0.045(8) 0.050(10) -0.002(8) 0.008(7) 0.008(7) B5 0.027(11) 0.063(13) 0.047(8) 0.009(6) 0.004(7) 0.005(9) B6 0.028(10) 0.045(9) 0.062(11) 0.016(9) 0.001(8) -0.001(8) B7 0.018(8) 0.030(6) 0.048(9) 0.001(7) 0.008(7) 0.000(6) B8 0.021(7) 0.048(9) 0.033(10) -0.005(7) 0.005(7) 0.004(7) B9 0.027(8) 0.050(9) 0.045(10) 0.010(8) 0.014(7) 0.001(7) B10 0.008(7) 0.031(6) 0.057(10) 0.007(7) 0.010(7) 0.007(5) B11 0.011(8) 0.038(10) 0.047(8) 0.001(6) 0.014(6) 0.002(7) B12 0.013(6) 0.024(8) 0.039(8) 0.000(6) 0.019(6) 0.007(5) C1 0.021(10) 0.052(13) 0.053(15) 0.012(11) 0.000(10) 0.019(10) C2 0.064(18) 0.033(12) 0.063(18) 0.001(11) -0.006(15) -0.009(12) C3 0.056(16) 0.050(14) 0.040(14) 0.011(11) 0.008(12) -0.006(12) C4 0.026(11) 0.064(16) 0.045(14) -0.015(12) 0.020(10) -0.003(10) C5 0.08(2) 0.061(17) 0.044(17) -0.006(13) 0.003(15) -0.005(15) C6 0.035(13) 0.060(16) 0.064(18) -0.004(13) 0.006(12) -0.009(12) C7 0.039(13) 0.042(13) 0.08(2) 0.015(13) 0.025(13) 0.005(11) C8 0.025(12) 0.042(12) 0.066(17) 0.012(11) 0.025(12) -0.006(9) C9 0.09(2) 0.025(13) 0.09(2) 0.005(14) 0.008(18) -0.034(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag I1 Ag1 2.778(3) . ? I1 Mo1 2.865(2) . ? I1 Ag1 2.980(3) 2_676 ? Ag1 Br2 2.771(3) . ? Ag1 Br1 2.803(3) . ? Ag1 I1 2.980(3) 2_676 ? Mo1 C8 1.99(2) . ? Mo1 C9 2.03(3) . ? Mo1 C2 2.08(3) . ? Mo1 C3 2.27(2) . ? Mo1 C7 2.28(3) . ? Mo1 C4 2.30(2) . ? Mo1 C5 2.36(3) . ? Mo1 C6 2.36(3) . ? Br1 B12 1.90(2) . ? Br2 B10 1.95(2) . ? Br3 B11 1.96(3) . ? Br4 B9 1.93(3) . ? Br5 B8 1.97(2) . ? Br6 B7 1.99(2) . ? O1 C8 1.13(3) . ? O2 C2 1.09(3) . ? O3 C9 1.05(3) . ? B2 C1 1.64(4) . ? B2 B6 1.76(4) . ? B2 B3 1.78(3) . ? B2 B11 1.78(3) . ? B2 B10 1.81(3) . ? B3 C1 1.69(4) . ? B3 B4 1.76(3) . ? B3 B7 1.77(3) . ? B3 B11 1.81(3) . ? B4 C1 1.72(3) . ? B4 B7 1.72(4) . ? B4 B5 1.76(4) . ? B4 B8 1.78(3) . ? B5 C1 1.67(3) . ? B5 B6 1.81(4) . ? B5 B8 1.81(4) . ? B5 B9 1.84(4) . ? B6 C1 1.69(4) . ? B6 B9 1.76(3) . ? B6 B10 1.82(4) . ? B7 B8 1.75(4) . ? B7 B11 1.78(3) . ? B7 B12 1.80(3) . ? B8 B12 1.78(3) . ? B8 B9 1.81(4) . ? B9 B10 1.80(4) . ? B9 B12 1.85(4) . ? B10 B11 1.73(3) . ? B10 B12 1.78(3) . ? B11 B12 1.80(3) . ? C3 C4 1.35(3) . ? C3 C7 1.34(3) . ? C4 C5 1.50(4) . ? C5 C6 1.37(4) . ? C6 C7 1.43(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 Ag1 I1 Mo1 107.87(7) . . ? Ag1 I1 Ag1 81.41(8) . 2_676 ? Mo1 I1 Ag1 114.20(7) . 2_676 ? Br2 Ag1 I1 129.21(10) . . ? Br2 Ag1 Br1 87.24(8) . . ? I1 Ag1 Br1 136.75(10) . . ? Br2 Ag1 I1 104.98(9) . 2_676 ? I1 Ag1 I1 98.59(8) . 2_676 ? Br1 Ag1 I1 91.58(8) . 2_676 ? C8 Mo1 C9 79.3(12) . . ? C8 Mo1 C2 113.6(10) . . ? C9 Mo1 C2 75.3(11) . . ? C8 Mo1 C3 96.0(10) . . ? C9 Mo1 C3 90.7(11) . . ? C2 Mo1 C3 143.5(10) . . ? C8 Mo1 C7 127.6(9) . . ? C9 Mo1 C7 84.9(11) . . ? C2 Mo1 C7 109.8(9) . . ? C3 Mo1 C7 34.3(9) . . ? C8 Mo1 C4 91.2(9) . . ? C9 Mo1 C4 123.4(11) . . ? C2 Mo1 C4 152.4(9) . . ? C3 Mo1 C4 34.5(9) . . ? C7 Mo1 C4 57.8(9) . . ? C8 Mo1 C5 121.7(10) . . ? C9 Mo1 C5 143.0(12) . . ? C2 Mo1 C5 115.1(11) . . ? C3 Mo1 C5 59.3(10) . . ? C7 Mo1 C5 58.1(10) . . ? C4 Mo1 C5 37.5(9) . . ? C8 Mo1 C6 150.0(10) . . ? C9 Mo1 C6 113.8(11) . . ? C2 Mo1 C6 96.1(10) . . ? C3 Mo1 C6 58.6(9) . . ? C7 Mo1 C6 35.9(9) . . ? C4 Mo1 C6 58.9(9) . . ? C5 Mo1 C6 33.7(9) . . ? C8 Mo1 I1 78.6(6) . . ? C9 Mo1 I1 133.7(9) . . ? C2 Mo1 I1 77.3(7) . . ? C3 Mo1 I1 131.7(6) . . ? C7 Mo1 I1 139.8(7) . . ? C4 Mo1 I1 97.2(7) . . ? C5 Mo1 I1 82.7(7) . . ? C6 Mo1 I1 105.5(6) . . ? B12 Br1 Ag1 96.8(6) . . ? B10 Br2 Ag1 95.3(7) . . ? C1 B2 B6 59.4(16) . . ? C1 B2 B3 59.2(14) . . ? B6 B2 B3 110.0(18) . . ? C1 B2 B11 104.6(15) . . ? B6 B2 B11 107.6(16) . . ? B3 B2 B11 61.0(14) . . ? C1 B2 B10 105.0(16) . . ? B6 B2 B10 61.2(15) . . ? B3 B2 B10 107.8(15) . . ? B11 B2 B10 57.5(12) . . ? C1 B3 B4 59.6(14) . . ? C1 B3 B7 102.2(17) . . ? B4 B3 B7 58.3(14) . . ? C1 B3 B2 56.3(15) . . ? B4 B3 B2 107.2(18) . . ? B7 B3 B2 106.8(16) . . ? C1 B3 B11 101.4(17) . . ? B4 B3 B11 106.4(16) . . ? B7 B3 B11 59.7(13) . . ? B2 B3 B11 59.6(13) . . ? C1 B4 B7 103.3(17) . . ? C1 B4 B3 58.1(14) . . ? B7 B4 B3 61.1(14) . . ? C1 B4 B5 57.2(14) . . ? B7 B4 B5 109.5(19) . . ? B3 B4 B5 108.5(18) . . ? C1 B4 B8 102.7(17) . . ? B7 B4 B8 59.9(14) . . ? B3 B4 B8 109.0(18) . . ? B5 B4 B8 61.4(15) . . ? C1 B5 B4 60.0(14) . . ? C1 B5 B6 57.9(15) . . ? B4 B5 B6 108.4(19) . . ? C1 B5 B8 103.6(19) . . ? B4 B5 B8 59.8(14) . . ? B6 B5 B8 105.4(19) . . ? C1 B5 B9 102(2) . . ? B4 B5 B9 107.9(19) . . ? B6 B5 B9 57.7(15) . . ? B8 B5 B9 59.5(14) . . ? C1 B6 B9 104.6(18) . . ? C1 B6 B2 56.7(14) . . ? B9 B6 B2 109.6(19) . . ? C1 B6 B5 56.7(14) . . ? B9 B6 B5 61.9(15) . . ? B2 B6 B5 105.8(19) . . ? C1 B6 B10 102.7(18) . . ? B9 B6 B10 60.5(14) . . ? B2 B6 B10 60.8(14) . . ? B5 B6 B10 108.1(17) . . ? B4 B7 B8 61.8(14) . . ? B4 B7 B3 60.6(14) . . ? B8 B7 B3 110.1(18) . . ? B4 B7 B11 109.3(16) . . ? B8 B7 B11 107.8(17) . . ? B3 B7 B11 61.1(13) . . ? B4 B7 B12 110.9(18) . . ? B8 B7 B12 60.1(13) . . ? B3 B7 B12 110.9(15) . . ? B11 B7 B12 60.3(12) . . ? B4 B7 Br6 122.0(15) . . ? B8 B7 Br6 121.4(14) . . ? B3 B7 Br6 121.1(15) . . ? B11 B7 Br6 120.5(16) . . ? B12 B7 Br6 118.3(14) . . ? B7 B8 B12 61.3(13) . . ? B7 B8 B4 58.3(14) . . ? B12 B8 B4 109.1(16) . . ? B7 B8 B5 106.1(16) . . ? B12 B8 B5 110.8(17) . . ? B4 B8 B5 58.8(14) . . ? B7 B8 B9 109.3(16) . . ? B12 B8 B9 62.2(14) . . ? B4 B8 B9 108.3(16) . . ? B5 B8 B9 61.1(15) . . ? B7 B8 Br5 124.7(16) . . ? B12 B8 Br5 121.4(14) . . ? B4 B8 Br5 121.8(15) . . ? B5 B8 Br5 119.1(16) . . ? B9 B8 Br5 119.4(15) . . ? B6 B9 B10 61.3(15) . . ? B6 B9 B8 107.5(18) . . ? B10 B9 B8 104.6(17) . . ? B6 B9 B5 60.4(15) . . ? B10 B9 B5 107.6(17) . . ? B8 B9 B5 59.5(14) . . ? B6 B9 B12 108.0(17) . . ? B10 B9 B12 58.3(12) . . ? B8 B9 B12 58.1(13) . . ? B5 B9 B12 106.3(18) . . ? B6 B9 Br4 124.2(17) . . ? B10 B9 Br4 123.1(17) . . ? B8 B9 Br4 121.0(15) . . ? B5 B9 Br4 123.6(17) . . ? B12 B9 Br4 119.8(15) . . ? B11 B10 B12 61.5(12) . . ? B11 B10 B9 109.8(16) . . ? B12 B10 B9 62.2(13) . . ? B11 B10 B2 60.3(13) . . ? B12 B10 B2 109.0(15) . . ? B9 B10 B2 105.5(17) . . ? B11 B10 B6 107.3(17) . . ? B12 B10 B6 108.6(17) . . ? B9 B10 B6 58.2(14) . . ? B2 B10 B6 58.0(14) . . ? B11 B10 Br2 123.6(17) . . ? B12 B10 Br2 123.0(14) . . ? B9 B10 Br2 120.7(15) . . ? B2 B10 Br2 121.5(13) . . ? B6 B10 Br2 119.3(14) . . ? B10 B11 B2 62.1(13) . . ? B10 B11 B7 108.3(16) . . ? B2 B11 B7 106.2(17) . . ? B10 B11 B12 60.6(12) . . ? B2 B11 B12 109.8(17) . . ? B7 B11 B12 60.3(12) . . ? B10 B11 B3 110.3(18) . . ? B2 B11 B3 59.4(13) . . ? B7 B11 B3 59.2(12) . . ? B12 B11 B3 109.4(16) . . ? B10 B11 Br3 120.2(16) . . ? B2 B11 Br3 123.0(13) . . ? B7 B11 Br3 122.0(16) . . ? B12 B11 Br3 119.2(14) . . ? B3 B11 Br3 121.8(14) . . ? B8 B12 B10 107.0(16) . . ? B8 B12 B11 106.0(16) . . ? B10 B12 B11 57.8(12) . . ? B8 B12 B7 58.6(13) . . ? B10 B12 B7 105.4(14) . . ? B11 B12 B7 59.4(12) . . ? B8 B12 B9 59.8(14) . . ? B10 B12 B9 59.5(13) . . ? B11 B12 B9 104.9(15) . . ? B7 B12 B9 105.4(17) . . ? B8 B12 Br1 123.6(12) . . ? B10 B12 Br1 121.7(14) . . ? B11 B12 Br1 122.7(15) . . ? B7 B12 Br1 124.0(14) . . ? B9 B12 Br1 123.2(14) . . ? B2 C1 B5 119(2) . . ? B2 C1 B3 64.5(15) . . ? B5 C1 B3 117.0(17) . . ? B2 C1 B6 63.9(17) . . ? B5 C1 B6 65.4(17) . . ? B3 C1 B6 118.1(19) . . ? B2 C1 B4 116.3(18) . . ? B5 C1 B4 62.8(15) . . ? B3 C1 B4 62.3(14) . . ? B6 C1 B4 116.8(17) . . ? O2 C2 Mo1 174(2) . . ? C4 C3 C7 110(2) . . ? C4 C3 Mo1 73.9(14) . . ? C7 C3 Mo1 73.5(16) . . ? C3 C4 C5 107(2) . . ? C3 C4 Mo1 71.6(13) . . ? C5 C4 Mo1 73.4(13) . . ? C6 C5 C4 106(2) . . ? C6 C5 Mo1 73.4(16) . . ? C4 C5 Mo1 69.1(14) . . ? C5 C6 C7 107(2) . . ? C5 C6 Mo1 73.0(16) . . ? C7 C6 Mo1 69.1(15) . . ? C3 C7 C6 110(2) . . ? C3 C7 Mo1 72.3(15) . . ? C6 C7 Mo1 75.0(15) . . ? O1 C8 Mo1 178(2) . . ? O3 C9 Mo1 177(3) . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 25.17 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 2.598 _refine_diff_density_min -2.947 _refine_diff_density_rms 0.369 #===END data_compound4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H27 B11 Mo O3' _chemical_formula_weight 458.21 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' 'Mo' 'Mo' -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 '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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 9.75770(10) _cell_length_b 14.1357(2) _cell_length_c 16.2310(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2238.77(5) _cell_formula_units_Z 4 _cell_measurement_temperature 170(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12 _cell_measurement_theta_max 18 _exptl_crystal_description Block _exptl_crystal_colour Orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.359 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 928 _exptl_absorpt_coefficient_mu 0.598 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_max 1.024 _exptl_absorpt_correction_T_min 0.962 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _diffrn_ambient_temperature 170(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method KappaCCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21991 _diffrn_reflns_av_R_equivalents 0.0259 _diffrn_reflns_av_sigmaI/netI 0.0220 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.56 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3939 _reflns_number_gt 3872 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction 'Denzo and Scalepack (otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _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^)+(0.0669P)^2^+1.0984P] 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 0.0068(14) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.02(4) _refine_ls_number_reflns 3939 _refine_ls_number_parameters 283 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0279 _refine_ls_R_factor_gt 0.0275 _refine_ls_wR_factor_ref 0.0835 _refine_ls_wR_factor_gt 0.0825 _refine_ls_goodness_of_fit_ref 0.988 _refine_ls_restrained_S_all 0.988 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.12169(2) 0.127041(15) 0.885626(13) 0.02362(12) Uani 1 1 d . . . O1 O 0.0481(3) 0.34248(17) 0.8983(2) 0.0515(7) Uani 1 1 d . . . O2 O 0.2363(3) 0.1806(2) 1.06160(15) 0.0500(7) Uani 1 1 d . . . O3 O -0.1893(2) 0.1377(2) 0.83014(16) 0.0475(6) Uani 1 1 d . . . B2 B -0.0479(4) -0.1017(3) 1.1473(3) 0.0408(9) Uani 1 1 d . . . H2 H -0.0102 -0.1127 1.2117 0.049 Uiso 1 1 calc R . . B3 B -0.1895(4) -0.0280(3) 1.1265(2) 0.0340(8) Uani 1 1 d . . . H3 H -0.2459 0.0098 1.1768 0.041 Uiso 1 1 calc R . . B4 B -0.2760(4) -0.0748(3) 1.0394(2) 0.0356(8) Uani 1 1 d . . . H4 H -0.3897 -0.0686 1.0318 0.043 Uiso 1 1 calc R . . B5 B -0.1836(4) -0.1732(2) 1.0090(2) 0.0353(8) Uani 1 1 d . . . H5 H -0.2390 -0.2343 0.9803 0.042 Uiso 1 1 calc R . . B6 B -0.0455(4) -0.1940(3) 1.0737(3) 0.0427(9) Uani 1 1 d . . . H6 H -0.0068 -0.2665 1.0889 0.051 Uiso 1 1 calc R . . B7 B -0.0231(4) 0.0064(3) 1.0950(2) 0.0331(8) Uani 1 1 d . . . H7 H 0.0319 0.0674 1.1240 0.040 Uiso 1 1 calc R . . B8 B -0.1664(4) 0.0238(2) 1.0279(2) 0.0317(7) Uani 1 1 d . . . H8 H -0.2062 0.0960 1.0128 0.038 Uiso 1 1 calc R . . B9 B -0.1644(4) -0.0698(3) 0.9535(2) 0.0331(7) Uani 1 1 d . . . H9 H -0.2030 -0.0596 0.8891 0.040 Uiso 1 1 calc R . . B10 B -0.0215(4) -0.1445(2) 0.9755(3) 0.0381(8) Uani 1 1 d . . . H10 H 0.0337 -0.1837 0.9256 0.046 Uiso 1 1 calc R . . B11 B 0.0666(4) -0.0967(3) 1.0621(3) 0.0404(9) Uani 1 1 d . . . H11 H 0.1804 -0.1035 1.0693 0.048 Uiso 1 1 calc R . . B12 B -0.0097(4) -0.0206(2) 0.9891(2) 0.0276(7) Uani 1 1 d . . . H12 H 0.059(5) 0.017(3) 0.950(3) 0.055(12) Uiso 1 1 d . . . C1 C -0.1989(4) -0.1498(2) 1.1123(2) 0.0452(8) Uani 1 1 d . . . H1 H -0.2633 -0.1944 1.1542 0.054 Uiso 1 1 calc R . . C2 C 0.0744(3) 0.2633(2) 0.8954(2) 0.0346(7) Uani 1 1 d . . . C3 C 0.1881(3) 0.1590(2) 1.0008(2) 0.0342(7) Uani 1 1 d . . . C4 C -0.0815(3) 0.1313(3) 0.85371(19) 0.0344(7) Uani 1 1 d . . . C5 C 0.3368(3) 0.1514(3) 0.8346(2) 0.0479(11) Uani 1 1 d . . . C6 C 0.3258(5) 0.0552(3) 0.8509(2) 0.0542(11) Uani 1 1 d . . . C7 C 0.2318(6) 0.0162(3) 0.7989(3) 0.0652(15) Uani 1 1 d . . . C8 C 0.1753(3) 0.0860(4) 0.7497(2) 0.0570(12) Uani 1 1 d . . . C9 C 0.2397(5) 0.1719(3) 0.7699(2) 0.0544(11) Uani 1 1 d . . . C10 C 0.4396(6) 0.2200(6) 0.8676(4) 0.116(3) Uani 1 1 d . . . H10A H 0.5165 0.2252 0.8290 0.174 Uiso 1 1 calc R . . H10B H 0.4733 0.1977 0.9210 0.174 Uiso 1 1 calc R . . H10C H 0.3965 0.2822 0.8743 0.174 Uiso 1 1 calc R . . C11 C 0.4209(8) 0.0026(7) 0.9080(4) 0.142(4) Uani 1 1 d . . . H11A H 0.4824 -0.0377 0.8756 0.213 Uiso 1 1 calc R . . H11B H 0.3669 -0.0369 0.9457 0.213 Uiso 1 1 calc R . . H11C H 0.4751 0.0480 0.9399 0.213 Uiso 1 1 calc R . . C12 C 0.1979(13) -0.0872(4) 0.7898(6) 0.190(6) Uani 1 1 d . . . H12A H 0.2347 -0.1222 0.8370 0.285 Uiso 1 1 calc R . . H12B H 0.2387 -0.1115 0.7389 0.285 Uiso 1 1 calc R . . H12C H 0.0982 -0.0952 0.7876 0.285 Uiso 1 1 calc R . . C13 C 0.0755(5) 0.0702(8) 0.6791(3) 0.147(5) Uani 1 1 d . . . H13A H 0.0221 0.0128 0.6895 0.220 Uiso 1 1 calc R . . H13B H 0.1266 0.0632 0.6275 0.220 Uiso 1 1 calc R . . H13C H 0.0135 0.1246 0.6749 0.220 Uiso 1 1 calc R . . C14 C 0.2260(9) 0.2647(4) 0.7245(4) 0.129(4) Uani 1 1 d . . . H14A H 0.1302 0.2741 0.7083 0.194 Uiso 1 1 calc R . . H14B H 0.2840 0.2636 0.6752 0.194 Uiso 1 1 calc R . . H14C H 0.2550 0.3165 0.7606 0.194 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 Mo1 0.02185(15) 0.02494(16) 0.02406(16) -0.00054(8) -0.00023(8) 0.00048(9) O1 0.0474(14) 0.0302(13) 0.0770(19) -0.0052(12) 0.0068(14) 0.0056(11) O2 0.0455(14) 0.0698(18) 0.0346(13) -0.0088(12) -0.0055(12) -0.0176(13) O3 0.0291(12) 0.0614(16) 0.0521(14) -0.0050(13) -0.0076(11) 0.0064(12) B2 0.044(2) 0.037(2) 0.042(2) 0.0142(16) -0.0088(17) -0.0033(16) B3 0.0386(18) 0.0360(18) 0.0273(17) 0.0037(14) 0.0034(15) -0.0031(16) B4 0.0295(18) 0.041(2) 0.0366(18) 0.0015(16) -0.0005(15) -0.0027(15) B5 0.0393(19) 0.0253(16) 0.0415(19) -0.0014(14) 0.0023(16) -0.0097(15) B6 0.043(2) 0.0263(18) 0.059(2) 0.0129(17) 0.0031(19) 0.0009(16) B7 0.0386(19) 0.0329(17) 0.0278(17) 0.0024(13) -0.0005(14) -0.0073(14) B8 0.0362(18) 0.0314(17) 0.0275(16) 0.0005(13) 0.0041(14) 0.0046(14) B9 0.0334(18) 0.0376(18) 0.0283(16) -0.0024(14) -0.0019(14) -0.0061(15) B10 0.042(2) 0.0230(16) 0.050(2) -0.0037(15) 0.0083(17) 0.0002(14) B11 0.0335(17) 0.039(2) 0.049(2) 0.0133(16) -0.0041(16) 0.0012(15) B12 0.0294(16) 0.0217(15) 0.0318(17) -0.0002(13) 0.0041(14) -0.0015(13) C1 0.052(2) 0.0334(17) 0.051(2) 0.0075(16) 0.0024(18) -0.0042(15) C2 0.0271(15) 0.0351(17) 0.0415(17) -0.0065(14) 0.0011(13) 0.0011(12) C3 0.0291(15) 0.0377(16) 0.0357(16) -0.0015(13) 0.0024(14) -0.0051(13) C4 0.0296(15) 0.0374(16) 0.0362(16) 0.0017(14) -0.0018(13) 0.0040(13) C5 0.0209(14) 0.079(3) 0.0437(19) -0.0365(19) 0.0125(14) -0.0161(15) C6 0.061(2) 0.068(3) 0.0335(18) 0.0114(19) 0.0173(18) 0.040(2) C7 0.097(4) 0.035(2) 0.064(3) -0.0126(19) 0.052(3) -0.014(2) C8 0.0236(15) 0.111(4) 0.0364(18) -0.030(2) 0.0060(14) -0.0116(19) C9 0.068(3) 0.046(2) 0.050(2) 0.0196(17) 0.036(2) 0.031(2) C10 0.067(3) 0.168(7) 0.114(5) -0.092(5) 0.044(3) -0.072(4) C11 0.124(6) 0.227(9) 0.076(4) 0.040(5) 0.026(4) 0.141(7) C12 0.314(14) 0.064(4) 0.190(9) -0.069(5) 0.195(10) -0.075(6) C13 0.042(3) 0.350(14) 0.049(3) -0.072(5) -0.004(2) -0.022(5) C14 0.196(8) 0.077(4) 0.114(5) 0.054(4) 0.109(6) 0.077(5) _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 Mo1 C2 1.986(3) . ? Mo1 C3 2.030(3) . ? Mo1 C4 2.050(3) . ? Mo1 C5 2.283(3) . ? Mo1 C9 2.293(3) . ? Mo1 C6 2.305(4) . ? Mo1 C8 2.340(3) . ? Mo1 C7 2.365(4) . ? O1 C2 1.150(4) . ? O2 C3 1.134(4) . ? O3 C4 1.123(4) . ? B2 C1 1.719(6) . ? B2 B7 1.764(5) . ? B2 B3 1.763(6) . ? B2 B6 1.768(6) . ? B2 B11 1.779(6) . ? B3 C1 1.739(5) . ? B3 B7 1.770(5) . ? B3 B8 1.774(5) . ? B3 B4 1.774(5) . ? B4 B5 1.730(5) . ? B4 C1 1.758(5) . ? B4 B8 1.766(5) . ? B4 B9 1.769(5) . ? B5 C1 1.715(6) . ? B5 B10 1.722(5) . ? B5 B9 1.728(5) . ? B5 B6 1.734(6) . ? B6 C1 1.739(6) . ? B6 B10 1.757(6) . ? B6 B11 1.768(5) . ? B7 B12 1.766(5) . ? B7 B11 1.782(5) . ? B7 B8 1.789(5) . ? B8 B12 1.769(5) . ? B8 B9 1.791(5) . ? B9 B12 1.760(5) . ? B9 B10 1.786(5) . ? B10 B12 1.769(4) . ? B10 B11 1.781(6) . ? B11 B12 1.765(5) . ? C5 C6 1.389(6) . ? C5 C9 1.444(6) . ? C5 C10 1.495(5) . ? C6 C7 1.363(7) . ? C6 C11 1.508(6) . ? C7 C8 1.384(7) . ? C7 C12 1.505(7) . ? C8 C9 1.405(6) . ? C8 C13 1.520(6) . ? C9 C14 1.510(6) . ? 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 C2 Mo1 C3 77.58(13) . . ? C2 Mo1 C4 76.53(13) . . ? C3 Mo1 C4 122.34(13) . . ? C2 Mo1 C5 95.51(14) . . ? C3 Mo1 C5 90.41(13) . . ? C4 Mo1 C5 142.48(14) . . ? C2 Mo1 C9 85.05(14) . . ? C3 Mo1 C9 122.19(17) . . ? C4 Mo1 C9 105.70(15) . . ? C5 Mo1 C9 36.79(16) . . ? C2 Mo1 C6 130.31(16) . . ? C3 Mo1 C6 92.72(15) . . ? C4 Mo1 C6 141.87(16) . . ? C5 Mo1 C6 35.25(16) . . ? C9 Mo1 C6 59.18(13) . . ? C2 Mo1 C8 111.54(17) . . ? C3 Mo1 C8 148.44(13) . . ? C4 Mo1 C8 89.16(12) . . ? C5 Mo1 C8 59.31(12) . . ? C9 Mo1 C8 35.30(16) . . ? C6 Mo1 C8 57.81(14) . . ? C2 Mo1 C7 142.68(14) . . ? C3 Mo1 C7 123.42(18) . . ? C4 Mo1 C7 107.97(18) . . ? C5 Mo1 C7 57.73(15) . . ? C9 Mo1 C7 57.81(14) . . ? C6 Mo1 C7 33.91(18) . . ? C8 Mo1 C7 34.21(17) . . ? C1 B2 B7 107.5(3) . . ? C1 B2 B3 59.9(2) . . ? B7 B2 B3 60.2(2) . . ? C1 B2 B6 59.8(2) . . ? B7 B2 B6 108.2(3) . . ? B3 B2 B6 108.5(3) . . ? C1 B2 B11 107.3(3) . . ? B7 B2 B11 60.4(2) . . ? B3 B2 B11 108.7(3) . . ? B6 B2 B11 59.8(2) . . ? C1 B3 B2 58.8(2) . . ? C1 B3 B7 106.4(3) . . ? B2 B3 B7 59.9(2) . . ? C1 B3 B8 107.2(3) . . ? B2 B3 B8 108.4(3) . . ? B7 B3 B8 60.6(2) . . ? C1 B3 B4 60.0(2) . . ? B2 B3 B4 107.7(3) . . ? B7 B3 B4 107.9(3) . . ? B8 B3 B4 59.7(2) . . ? B5 B4 C1 58.9(2) . . ? B5 B4 B8 106.8(3) . . ? C1 B4 B8 106.7(3) . . ? B5 B4 B9 59.2(2) . . ? C1 B4 B9 106.9(3) . . ? B8 B4 B9 60.9(2) . . ? B5 B4 B3 106.2(3) . . ? C1 B4 B3 59.0(2) . . ? B8 B4 B3 60.1(2) . . ? B9 B4 B3 108.7(2) . . ? C1 B5 B10 110.1(3) . . ? C1 B5 B9 110.8(3) . . ? B10 B5 B9 62.4(2) . . ? C1 B5 B4 61.4(2) . . ? B10 B5 B4 112.3(2) . . ? B9 B5 B4 61.6(2) . . ? C1 B5 B6 60.5(2) . . ? B10 B5 B6 61.1(2) . . ? B9 B5 B6 112.0(3) . . ? B4 B5 B6 111.6(3) . . ? B5 B6 C1 59.2(2) . . ? B5 B6 B10 59.1(2) . . ? C1 B6 B10 107.4(3) . . ? B5 B6 B11 106.5(3) . . ? C1 B6 B11 107.0(3) . . ? B10 B6 B11 60.7(2) . . ? B5 B6 B2 105.9(3) . . ? C1 B6 B2 58.7(2) . . ? B10 B6 B2 108.7(3) . . ? B11 B6 B2 60.4(2) . . ? B2 B7 B12 106.9(3) . . ? B2 B7 B3 59.9(2) . . ? B12 B7 B3 106.9(3) . . ? B2 B7 B11 60.2(2) . . ? B12 B7 B11 59.7(2) . . ? B3 B7 B11 108.2(3) . . ? B2 B7 B8 107.7(3) . . ? B12 B7 B8 59.7(2) . . ? B3 B7 B8 59.8(2) . . ? B11 B7 B8 108.3(3) . . ? B12 B8 B4 106.3(2) . . ? B12 B8 B3 106.6(2) . . ? B4 B8 B3 60.2(2) . . ? B12 B8 B7 59.51(19) . . ? B4 B8 B7 107.5(2) . . ? B3 B8 B7 59.6(2) . . ? B12 B8 B9 59.24(19) . . ? B4 B8 B9 59.7(2) . . ? B3 B8 B9 107.8(2) . . ? B7 B8 B9 107.5(2) . . ? B5 B9 B12 104.8(3) . . ? B5 B9 B4 59.3(2) . . ? B12 B9 B4 106.6(2) . . ? B5 B9 B10 58.7(2) . . ? B12 B9 B10 59.85(19) . . ? B4 B9 B10 107.4(3) . . ? B5 B9 B8 105.8(2) . . ? B12 B9 B8 59.75(19) . . ? B4 B9 B8 59.5(2) . . ? B10 B9 B8 108.1(2) . . ? B5 B10 B6 59.8(2) . . ? B5 B10 B12 104.7(3) . . ? B6 B10 B12 106.8(3) . . ? B5 B10 B11 106.5(3) . . ? B6 B10 B11 60.0(2) . . ? B12 B10 B11 59.6(2) . . ? B5 B10 B9 59.0(2) . . ? B6 B10 B9 108.2(3) . . ? B12 B10 B9 59.3(2) . . ? B11 B10 B9 108.1(3) . . ? B12 B11 B6 106.5(3) . . ? B12 B11 B2 106.3(3) . . ? B6 B11 B2 59.8(2) . . ? B12 B11 B7 59.70(19) . . ? B6 B11 B7 107.5(3) . . ? B2 B11 B7 59.4(2) . . ? B12 B11 B10 59.8(2) . . ? B6 B11 B10 59.3(2) . . ? B2 B11 B10 107.1(3) . . ? B7 B11 B10 108.0(3) . . ? B9 B12 B8 61.0(2) . . ? B9 B12 B7 109.9(2) . . ? B8 B12 B7 60.8(2) . . ? B9 B12 B11 110.0(2) . . ? B8 B12 B11 110.0(3) . . ? B7 B12 B11 60.6(2) . . ? B9 B12 B10 60.8(2) . . ? B8 B12 B10 109.8(3) . . ? B7 B12 B10 109.3(3) . . ? B11 B12 B10 60.5(2) . . ? B5 C1 B2 108.9(3) . . ? B5 C1 B3 108.4(3) . . ? B2 C1 B3 61.3(2) . . ? B5 C1 B6 60.3(2) . . ? B2 C1 B6 61.5(3) . . ? B3 C1 B6 111.0(3) . . ? B5 C1 B4 59.7(2) . . ? B2 C1 B4 110.5(3) . . ? B3 C1 B4 61.0(2) . . ? B6 C1 B4 110.0(3) . . ? O1 C2 Mo1 177.7(3) . . ? O2 C3 Mo1 173.3(3) . . ? O3 C4 Mo1 173.9(3) . . ? C6 C5 C9 106.5(3) . . ? C6 C5 C10 128.2(6) . . ? C9 C5 C10 124.8(5) . . ? C6 C5 Mo1 73.3(2) . . ? C9 C5 Mo1 71.99(18) . . ? C10 C5 Mo1 125.8(3) . . ? C7 C6 C5 109.3(4) . . ? C7 C6 C11 126.5(6) . . ? C5 C6 C11 123.5(6) . . ? C7 C6 Mo1 75.5(2) . . ? C5 C6 Mo1 71.49(19) . . ? C11 C6 Mo1 126.8(3) . . ? C6 C7 C8 109.6(4) . . ? C6 C7 C12 127.0(7) . . ? C8 C7 C12 123.3(7) . . ? C6 C7 Mo1 70.6(2) . . ? C8 C7 Mo1 71.9(2) . . ? C12 C7 Mo1 127.0(4) . . ? C7 C8 C9 107.7(3) . . ? C7 C8 C13 125.8(6) . . ? C9 C8 C13 126.1(6) . . ? C7 C8 Mo1 73.9(2) . . ? C9 C8 Mo1 70.5(2) . . ? C13 C8 Mo1 127.1(3) . . ? C8 C9 C5 106.8(3) . . ? C8 C9 C14 126.7(6) . . ? C5 C9 C14 125.9(6) . . ? C8 C9 Mo1 74.2(2) . . ? C5 C9 Mo1 71.22(19) . . ? C14 C9 Mo1 126.5(3) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.600 _refine_diff_density_min -0.410 _refine_diff_density_rms 0.090