Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global #=========================================================================== _journal_coden_Cambridge 186 # 1. SUBMISSION DETAILS _publ_contact_author_name 'Prof. F. Gordon A. Stone' _publ_contact_author_address ; Department of Chemistry Baylor University PO Box 97348 Waco TX, 76798-7348 ; _publ_contact_author_email Gordon_Stone@baylor.edu _publ_contact_author_fax '254 710 2403' _publ_contact_author_phone '254 710 4427' _publ_requested_journal 'J. Chem. Soc, Dalton Transactions' _publ_contact_letter ; Please consider this CIF submission as electronic supplementary material for a manuscript submitted to J. Chem. Soc, Dalton Transactions. Title: Reactivity of the molybdenacarbaborane anion [2,2,2,2-(CO)~4~-closo- 2,1-MoCB~10~H~11~]^-^: Metal oxidation versus cage substitution Date of submission: June 2001 ; #=========================================================================== # 2. TITLE AND AUTHOR LIST _publ_section_title ; Reactivity of the molybdenacarbaborane anion [2,2,2,2-(CO)~4~-closo- 2,1-MoCB~10~H~11~]^-^: Metal oxidation versus cage substitution ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. loop_ _publ_author_name _publ_author_address 'Du, Shaowu' ; Department of Chemistry and Biochemistry Baylor University Waco TX, 76798-7348 USA ; 'Kautz, Jason A.' ; Department of Chemistry and Biochemistry Baylor University Waco TX, 76798-7348 USA ; 'McGrath, Thomas D.' ; Department of Chemistry and Biochemistry Baylor University Waco TX, 76798-7348 USA ; 'Stone, F. Gordon A.' ; Department of Chemistry and Biochemistry Baylor University Waco TX, 76798-7348 USA ; #=========================================================================== # 3. TEXT _publ_section_exptl_refinement ; Diffracted intensities were collected on an Enraf-Nonius CAD-4 operating in various scan modes as indicated below, using graphite-monochromated Mo-K\a X-radiation. The final unit cell dimensions were determined from the setting angle values of 25 accurately centered reflections. The stability of the crystal during the period of the data collection was monitored by measuring the intensities of three standard reflections every two hours. Data were collected at a constant scan speed of 5.17\% min^-1^ in \w, with a scan range of 1.15 + 0.34tan\q. The data were corrected for Lorentz, polarization and X-ray absorption effects, the latter by a numerical method based on the measurments of the various crystal faces. The structures were solved by direct methods and successive difference Fourier syntheses were used to locate all non-hydrogen atoms using SHELXTL vs. 5.03. Refinements were made on all F^2^ data using SHELXL-97. Anisotropic thermal parameters were included for all non-hydrogen atoms. Cage carbon atoms were assigned by comparison of the bond lengths between adjacent boron atoms in conjunction with the magnitudes of their isotropic thermal parameters. Hydrogen atoms were constrained to idealized geometries and assigned isotropic displacement paramaters 1.2 times U~iso~ value of the parent atom, except for methyl protons where U~iso~ = 1.5 U~iso~. The methyl groups on one of the CNBu^t^ ligands in 3 were disordered over two positions rotated apporximately 45 degrees from each other about the N(30)-C(30) bond axis. The occupancies of the major and minor subunits were restrained at 80 and 20 % respectively; the anisotropic thermal parameters of the analogous carbons in each set were assigned equivalent magnitudes. Compound 3 co-crystallized with a half-molecule of dichlormethane per asymmetric unit. One of the chlorine atoms was disordered over two sites and was refined with an fixed occupancy of 25 % in each site. Compound 14 co-crystallized with one fully ordered dichloromethane molecule per formula unit which was refined without restraint. All calculations were carried out on Dell PC computers. ; # Insert blank lines between references _publ_section_references ; Enraf-Nonius (1989). CAD-4 Software. Version 5. Enraf-Nonius, Delft, The Netherlands. Harms, K. (1993). XCAD4 A Program to extract intensities from a CAD-4 file. University of Marburg, Germany. Sheldrick, G.M. (1997). SHELXL97. Program for crystal structure refinement. University of G\\"ottingen, Germany. Siemens (1995). SHELXTL-PC. Version 5.03. Bruker Analytical X-ray Instruments Inc. (1995), Madison, Wisconsin, USA. Wilson, A.J.C. (1992) Ed. International Tables for Crystallography, Volume C, Kluwer Academic Publishers, Dordrecht, The Netherlands. ; _publ_section_acknowledgements ; This work was supported by the Robert A. Welch Foundation (Grant AA-1201) ; #=========================================================================== data_3 _database_code_CSD 166146 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_formula_moiety [2,2,2,2-(CNBu^t^)~4~-2-I-closo-2,1-MoCB~10~H~11~] _chemical_formula_sum 'C21.50 H48 B10 Cl I Mo N4' _chemical_formula_weight 729.03 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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 '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' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 17.1449(14) _cell_length_b 12.0556(18) _cell_length_c 20.686(2) _cell_angle_alpha 90.00 _cell_angle_beta 114.01(8) _cell_angle_gamma 90.00 _cell_volume 3905.8(8) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 6.2 _cell_measurement_theta_max 21.5 _exptl_crystal_description prisms _exptl_crystal_colour orange _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.240 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1468 _exptl_absorpt_coefficient_mu 1.212 _exptl_absorpt_correction_type 'Numerical, SHELXTL-PC vs 5.03 1995' _exptl_absorpt_correction_T_min 0.61883 _exptl_absorpt_correction_T_max 0.88339 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Enraf-Nonius CAD4' _diffrn_measurement_method w-4/3q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 5.0 _diffrn_reflns_number 7092 _diffrn_reflns_av_R_equivalents 0.0391 _diffrn_reflns_av_sigmaI/netI 0.0774 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.60 _diffrn_reflns_theta_max 24.96 _reflns_number_total 6849 _reflns_number_gt 4440 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Enraf-Nonius CAD4 (1989)' _computing_cell_refinement 'Enraf-Nonius CAD4 (1989)' _computing_data_reduction 'XCAD4 Siemens Software (Harms, 1993)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in SHELXTL-PC (Bruker, 1995)' _computing_publication_material 'SHELXL-97 (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^)+(0.0012P)^2^+13.2881P] 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 6849 _refine_ls_number_parameters 379 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1053 _refine_ls_R_factor_gt 0.0567 _refine_ls_wR_factor_ref 0.0998 _refine_ls_wR_factor_gt 0.0874 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.070 _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 Mo Mo 0.20562(3) 0.01921(4) 0.17828(3) 0.02913(13) Uani 1 1 d . . . B5 B 0.1444(4) -0.0273(6) 0.0526(3) 0.0297(16) Uani 1 1 d . . . H5 H 0.1171 0.0508 0.0253 0.036 Uiso 1 1 calc R . . C1 C 0.0959(4) -0.0981(6) 0.0934(3) 0.0468(18) Uani 1 1 d . . . H1 H 0.0357 -0.0669 0.0936 0.056 Uiso 1 1 calc R . . B2 B 0.1680(5) -0.1726(6) 0.1642(4) 0.0389(19) Uani 1 1 d . . . H2 H 0.1561 -0.1952 0.2109 0.047 Uiso 1 1 calc R . . B3 B 0.2736(5) -0.1429(6) 0.1652(4) 0.0359(18) Uani 1 1 d . . . H3 H 0.3338 -0.1471 0.2128 0.043 Uiso 1 1 calc R . . B4 B 0.2550(5) -0.0469(7) 0.0932(4) 0.042(2) Uani 1 1 d . . . H4 H 0.3017 0.0148 0.0921 0.050 Uiso 1 1 calc R . . B7 B 0.2183(6) -0.2651(7) 0.1268(4) 0.055(2) Uani 1 1 d . . . H7 H 0.2434 -0.3453 0.1521 0.066 Uiso 1 1 calc R . . B6 B 0.1080(5) -0.2394(6) 0.0844(4) 0.044(2) Uani 1 1 d . . . H6 H 0.0601 -0.3019 0.0818 0.053 Uiso 1 1 calc R . . B10 B 0.0909(5) -0.1484(6) 0.0140(4) 0.0397(19) Uani 1 1 d . . . H10 H 0.0320 -0.1507 -0.0348 0.048 Uiso 1 1 calc R . . B9 B 0.1912(5) -0.1172(7) 0.0141(4) 0.044(2) Uani 1 1 d . . . H9 H 0.1981 -0.0984 -0.0353 0.052 Uiso 1 1 calc R . . B8 B 0.2687(5) -0.1910(8) 0.0834(4) 0.053(2) Uani 1 1 d . . . H8 H 0.3268 -0.2224 0.0792 0.064 Uiso 1 1 calc R . . B11 B 0.1688(5) -0.2519(7) 0.0342(4) 0.045(2) Uani 1 1 d . . . H11 H 0.1612 -0.3224 -0.0016 0.054 Uiso 1 1 calc R . . I I 0.23631(4) 0.19974(5) 0.28013(3) 0.0725(2) Uani 1 1 d . . . C10 C 0.0912(4) 0.0410(6) 0.1926(3) 0.0437(18) Uani 1 1 d . . . N10 N 0.0319(4) 0.0535(5) 0.2043(3) 0.0556(17) Uani 1 1 d . . . C11 C -0.0369(5) 0.0899(8) 0.2247(4) 0.071(3) Uani 1 1 d . . . C12 C -0.0631(5) 0.2055(8) 0.1919(4) 0.087(3) Uani 1 1 d . . . H12A H -0.0161 0.2558 0.2128 0.130 Uiso 1 1 calc R . . H12B H -0.1110 0.2316 0.2005 0.130 Uiso 1 1 calc R . . H12C H -0.0788 0.2013 0.1418 0.130 Uiso 1 1 calc R . . C13 C 0.0016(6) 0.0936(10) 0.3060(4) 0.125(5) Uani 1 1 d . . . H13A H 0.0155 0.0197 0.3244 0.187 Uiso 1 1 calc R . . H13B H -0.0392 0.1252 0.3217 0.187 Uiso 1 1 calc R . . H13C H 0.0523 0.1382 0.3228 0.187 Uiso 1 1 calc R . . C14 C -0.1089(5) 0.0070(9) 0.1955(5) 0.107(4) Uani 1 1 d . . . H14A H -0.0900 -0.0637 0.2178 0.160 Uiso 1 1 calc R . . H14B H -0.1261 -0.0003 0.1454 0.160 Uiso 1 1 calc R . . H14C H -0.1565 0.0322 0.2048 0.160 Uiso 1 1 calc R . . C20 C 0.2566(4) -0.0549(5) 0.2798(3) 0.0359(16) Uani 1 1 d . . . N20 N 0.2885(3) -0.0913(4) 0.3350(3) 0.0409(14) Uani 1 1 d . . . C21 C 0.3373(5) -0.1289(6) 0.4066(3) 0.0488(19) Uani 1 1 d . . . C22 C 0.4294(5) -0.1019(10) 0.4222(5) 0.121(4) Uani 1 1 d . . . H22A H 0.4354 -0.0233 0.4183 0.182 Uiso 1 1 calc R . . H22B H 0.4460 -0.1396 0.3889 0.182 Uiso 1 1 calc R . . H22C H 0.4652 -0.1256 0.4693 0.182 Uiso 1 1 calc R . . C23 C 0.3245(6) -0.2509(7) 0.4099(4) 0.090(3) Uani 1 1 d . . . H23A H 0.3447 -0.2884 0.3788 0.135 Uiso 1 1 calc R . . H23B H 0.2648 -0.2662 0.3956 0.135 Uiso 1 1 calc R . . H23C H 0.3557 -0.2765 0.4575 0.135 Uiso 1 1 calc R . . C24 C 0.3082(7) -0.0644(8) 0.4547(4) 0.113(4) Uani 1 1 d . . . H24A H 0.3161 0.0134 0.4495 0.170 Uiso 1 1 calc R . . H24B H 0.3411 -0.0862 0.5029 0.170 Uiso 1 1 calc R . . H24C H 0.2489 -0.0791 0.4426 0.170 Uiso 1 1 calc R . . C30 C 0.3330(4) 0.0687(5) 0.2092(3) 0.0397(16) Uani 1 1 d . . . N30 N 0.4024(4) 0.0966(5) 0.2284(3) 0.0501(16) Uani 1 1 d . . . C31 C 0.4873(5) 0.1472(7) 0.2569(4) 0.057(2) Uani 1 1 d . . . C32 C 0.5349(7) 0.1103(11) 0.2112(7) 0.103(4) Uani 0.80 1 d P . . H32A H 0.5091 0.1446 0.1655 0.155 Uiso 0.80 1 calc PR . . H32B H 0.5316 0.0311 0.2059 0.155 Uiso 0.80 1 calc PR . . H32C H 0.5937 0.1323 0.2339 0.155 Uiso 0.80 1 calc PR . . C33 C 0.5333(8) 0.0983(12) 0.3316(6) 0.099(5) Uani 0.80 1 d P . . H33A H 0.5404 0.0198 0.3283 0.148 Uiso 0.80 1 calc PR . . H33B H 0.4999 0.1118 0.3585 0.148 Uiso 0.80 1 calc PR . . H33C H 0.5882 0.1326 0.3548 0.148 Uiso 0.80 1 calc PR . . C34 C 0.4758(7) 0.2683(8) 0.2574(9) 0.113(6) Uani 0.80 1 d P . . H34A H 0.4160 0.2857 0.2363 0.169 Uiso 0.80 1 calc PR . . H34B H 0.5038 0.3033 0.2309 0.169 Uiso 0.80 1 calc PR . . H34C H 0.5003 0.2948 0.3053 0.169 Uiso 0.80 1 calc PR . . C32A C 0.546(4) 0.082(6) 0.293(4) 0.103(4) Uani 0.20 1 d P . . H32D H 0.5288 0.0418 0.3251 0.155 Uiso 0.20 1 calc PR . . H32E H 0.5967 0.1238 0.3194 0.155 Uiso 0.20 1 calc PR . . H32F H 0.5570 0.0311 0.2622 0.155 Uiso 0.20 1 calc PR . . C33A C 0.467(3) 0.245(5) 0.309(2) 0.099(5) Uani 0.20 1 d P . . H33D H 0.4144 0.2823 0.2816 0.148 Uiso 0.20 1 calc PR . . H33E H 0.5128 0.2978 0.3255 0.148 Uiso 0.20 1 calc PR . . H33F H 0.4625 0.2089 0.3487 0.148 Uiso 0.20 1 calc PR . . C34A C 0.478(3) 0.224(4) 0.193(3) 0.113(6) Uani 0.20 1 d P . . H34D H 0.4274 0.2687 0.1808 0.169 Uiso 0.20 1 calc PR . . H34E H 0.4728 0.1789 0.1533 0.169 Uiso 0.20 1 calc PR . . H34F H 0.5269 0.2708 0.2062 0.169 Uiso 0.20 1 calc PR . . C40 C 0.1789(4) 0.1683(5) 0.1194(3) 0.0442(18) Uani 1 1 d . . . N40 N 0.1720(4) 0.2514(5) 0.0903(3) 0.0522(16) Uani 1 1 d . . . C41 C 0.1670(5) 0.3642(6) 0.0625(4) 0.061(2) Uani 1 1 d . . . C42 C 0.1429(6) 0.3562(8) -0.0162(4) 0.099(3) Uani 1 1 d . . . H42A H 0.0868 0.3247 -0.0389 0.149 Uiso 1 1 calc R . . H42B H 0.1833 0.3098 -0.0247 0.149 Uiso 1 1 calc R . . H42C H 0.1433 0.4289 -0.0350 0.149 Uiso 1 1 calc R . . C43 C 0.0986(6) 0.4223(7) 0.0791(5) 0.101(3) Uani 1 1 d . . . H43A H 0.0443 0.3878 0.0529 0.152 Uiso 1 1 calc R . . H43B H 0.0959 0.4990 0.0660 0.152 Uiso 1 1 calc R . . H43C H 0.1123 0.4166 0.1288 0.152 Uiso 1 1 calc R . . C44 C 0.2556(5) 0.4153(6) 0.1018(4) 0.076(3) Uani 1 1 d . . . H44A H 0.2685 0.4189 0.1514 0.114 Uiso 1 1 calc R . . H44B H 0.2564 0.4887 0.0841 0.114 Uiso 1 1 calc R . . H44C H 0.2975 0.3702 0.0944 0.114 Uiso 1 1 calc R . . Cl1 Cl 0.4231(12) 0.0641(18) -0.0662(13) 0.167(8) Uani 0.25 1 d P . . Cl1A Cl 0.3680(10) 0.0463(11) -0.1007(8) 0.098(4) Uani 0.25 1 d P . . Cl2 Cl 0.3755(4) 0.2120(5) 0.0061(3) 0.120(2) Uani 0.50 1 d P . . C50 C 0.3503(14) 0.097(2) -0.0410(10) 0.132(10) Uani 0.50 1 d P . . H50A H 0.3424 0.0373 -0.0127 0.158 Uiso 0.50 1 calc PR . . H50B H 0.2969 0.1075 -0.0820 0.158 Uiso 0.50 1 calc PR . . 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 Mo 0.0260(3) 0.0268(3) 0.0271(3) -0.0038(2) 0.0031(2) 0.0000(3) B5 0.030(4) 0.024(3) 0.025(3) -0.002(3) -0.001(3) 0.000(3) C1 0.031(4) 0.057(5) 0.042(4) -0.018(3) 0.004(3) 0.006(3) B2 0.039(4) 0.040(5) 0.036(4) 0.000(3) 0.013(3) -0.016(4) B3 0.031(4) 0.042(4) 0.029(4) 0.002(3) 0.006(3) 0.009(4) B4 0.032(4) 0.056(5) 0.032(4) 0.005(4) 0.007(3) -0.010(4) B7 0.069(6) 0.032(5) 0.045(5) 0.003(4) 0.001(4) 0.017(4) B6 0.052(5) 0.030(4) 0.049(5) -0.008(4) 0.019(4) -0.021(4) B10 0.038(4) 0.039(4) 0.035(4) -0.018(3) 0.008(3) -0.009(4) B9 0.044(5) 0.059(5) 0.030(4) -0.004(4) 0.017(4) -0.007(4) B8 0.036(5) 0.079(6) 0.039(4) -0.007(5) 0.009(4) 0.024(5) B11 0.053(5) 0.040(5) 0.038(4) -0.011(4) 0.016(4) 0.010(4) I 0.0830(4) 0.0552(3) 0.0547(3) -0.0304(3) 0.0028(3) 0.0040(3) C10 0.037(4) 0.056(5) 0.034(3) -0.014(3) 0.010(3) 0.015(4) N10 0.048(4) 0.079(5) 0.038(3) -0.016(3) 0.016(3) 0.016(3) C11 0.059(5) 0.118(8) 0.041(4) 0.000(5) 0.023(4) 0.037(6) C12 0.073(6) 0.122(8) 0.063(5) -0.032(6) 0.026(5) 0.033(6) C13 0.101(8) 0.226(13) 0.047(5) -0.010(7) 0.030(5) 0.059(9) C14 0.053(5) 0.161(11) 0.105(7) 0.050(8) 0.031(5) 0.009(7) C20 0.036(4) 0.040(4) 0.032(3) -0.008(3) 0.013(3) -0.008(3) N20 0.042(3) 0.051(4) 0.031(3) 0.001(3) 0.016(3) -0.008(3) C21 0.056(5) 0.060(5) 0.025(3) 0.010(3) 0.011(3) -0.001(4) C22 0.051(6) 0.208(13) 0.077(6) 0.042(8) -0.002(5) -0.026(7) C23 0.124(8) 0.069(6) 0.064(6) 0.019(5) 0.025(6) 0.002(6) C24 0.197(12) 0.113(8) 0.050(5) 0.010(5) 0.072(7) 0.034(8) C30 0.042(4) 0.033(4) 0.034(3) 0.006(3) 0.005(3) -0.012(3) N30 0.038(3) 0.043(4) 0.054(4) 0.006(3) 0.002(3) -0.021(3) C31 0.034(4) 0.063(5) 0.061(5) 0.002(4) 0.007(4) -0.025(4) C32 0.080(8) 0.126(11) 0.122(10) -0.040(9) 0.059(8) -0.059(8) C33 0.063(8) 0.116(11) 0.078(8) 0.023(8) -0.011(6) -0.046(8) C34 0.052(7) 0.040(7) 0.223(18) -0.008(8) 0.032(10) -0.032(6) C32A 0.080(8) 0.126(11) 0.122(10) -0.040(9) 0.059(8) -0.059(8) C33A 0.063(8) 0.116(11) 0.078(8) 0.023(8) -0.011(6) -0.046(8) C34A 0.052(7) 0.040(7) 0.223(18) -0.008(8) 0.032(10) -0.032(6) C40 0.050(4) 0.032(4) 0.035(4) -0.004(3) 0.001(3) -0.005(3) N40 0.057(4) 0.030(3) 0.050(4) -0.002(3) 0.002(3) -0.001(3) C41 0.054(5) 0.035(4) 0.069(5) 0.008(4) -0.001(4) -0.002(4) C42 0.099(7) 0.103(8) 0.061(6) 0.024(5) -0.003(5) -0.034(6) C43 0.093(7) 0.043(5) 0.143(9) -0.002(6) 0.022(7) 0.024(5) C44 0.068(6) 0.038(5) 0.094(6) 0.002(4) 0.004(5) -0.010(4) Cl1 0.143(17) 0.151(16) 0.22(2) -0.012(15) 0.093(16) 0.028(14) Cl1A 0.130(13) 0.056(7) 0.114(10) 0.023(7) 0.055(9) 0.014(8) Cl2 0.136(5) 0.096(4) 0.096(4) -0.008(3) 0.016(4) -0.023(4) C50 0.14(2) 0.20(3) 0.061(12) 0.037(15) 0.039(13) -0.09(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 Mo C30 2.097(7) . y Mo C40 2.113(7) . y Mo C10 2.116(7) . y Mo C20 2.117(6) . y Mo B3 2.346(7) . y Mo B4 2.380(8) . y Mo B2 2.386(7) . y Mo C1 2.437(6) . y Mo B5 2.441(6) . y Mo I 2.9241(9) . y B5 C1 1.645(9) . ? B5 B9 1.722(10) . ? B5 B10 1.736(9) . ? B5 B4 1.749(9) . ? C1 B10 1.719(9) . ? C1 B2 1.734(10) . ? C1 B6 1.735(10) . ? B2 B6 1.747(10) . ? B2 B7 1.768(11) . ? B2 B3 1.836(10) . ? B3 B7 1.757(11) . ? B3 B8 1.760(10) . ? B3 B4 1.811(10) . ? B4 B9 1.769(10) . ? B4 B8 1.776(12) . ? B7 B8 1.729(12) . ? B7 B6 1.758(11) . ? B7 B11 1.759(10) . ? B6 B10 1.750(10) . ? B6 B11 1.751(11) . ? B10 B11 1.750(10) . ? B10 B9 1.759(10) . ? B9 B8 1.750(11) . ? B9 B11 1.757(11) . ? B8 B11 1.757(11) . ? C10 N10 1.147(7) . ? N10 C11 1.473(9) . ? C11 C14 1.511(12) . ? C11 C12 1.535(12) . ? C11 C13 1.537(10) . ? C20 N20 1.134(7) . ? N20 C21 1.446(8) . ? C21 C23 1.492(10) . ? C21 C24 1.499(10) . ? C21 C22 1.514(10) . ? C30 N30 1.142(7) . ? N30 C31 1.462(8) . ? C31 C32A 1.25(7) . ? C31 C34 1.474(13) . ? C31 C33 1.538(13) . ? C31 C32 1.545(13) . ? C31 C34A 1.56(5) . ? C31 C33A 1.72(6) . ? C40 N40 1.151(8) . ? N40 C41 1.465(8) . ? C41 C42 1.512(10) . ? C41 C43 1.520(11) . ? C41 C44 1.530(9) . ? Cl1 Cl1A 0.95(2) . ? Cl1 C50 1.59(3) . ? Cl2 C50 1.65(2) . ? 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 C30 Mo C40 83.6(3) . . y C30 Mo C10 146.2(2) . . y C40 Mo C10 88.8(3) . . y C30 Mo C20 81.9(2) . . y C40 Mo C20 146.7(2) . . y C10 Mo C20 86.9(2) . . y C30 Mo B3 76.6(3) . . y C40 Mo B3 130.1(3) . . y C10 Mo B3 130.7(3) . . y C20 Mo B3 74.9(2) . . y C30 Mo B4 71.4(3) . . y C40 Mo B4 85.3(3) . . y C10 Mo B4 140.7(2) . . y C20 Mo B4 117.7(2) . . y B3 Mo B4 45.0(2) . . ? C30 Mo B2 120.6(3) . . y C40 Mo B2 140.3(2) . . y C10 Mo B2 85.3(3) . . y C20 Mo B2 72.2(2) . . y B3 Mo B2 45.7(3) . . ? B4 Mo B2 75.2(3) . . ? C30 Mo C1 142.0(2) . . y C40 Mo C1 99.0(2) . . y C10 Mo C1 71.6(2) . . y C20 Mo C1 110.9(2) . . y B3 Mo C1 73.0(2) . . ? B4 Mo C1 71.0(2) . . ? B2 Mo C1 42.1(2) . . ? C30 Mo B5 109.5(2) . . y C40 Mo B5 71.5(2) . . y C10 Mo B5 99.0(2) . . y C20 Mo B5 141.7(2) . . y B3 Mo B5 72.8(2) . . ? B4 Mo B5 42.5(2) . . ? B2 Mo B5 70.7(2) . . ? C1 Mo B5 39.4(2) . . ? C30 Mo I 73.04(19) . . y C40 Mo I 73.46(17) . . y C10 Mo I 73.26(18) . . y C20 Mo I 73.65(16) . . y B3 Mo I 138.64(17) . . y B4 Mo I 140.21(19) . . y B2 Mo I 140.31(18) . . y C1 Mo I 144.22(16) . . y B5 Mo I 144.30(17) . . y C1 B5 B9 109.8(5) . . ? C1 B5 B10 61.1(4) . . ? B9 B5 B10 61.1(4) . . ? C1 B5 B4 111.1(5) . . ? B9 B5 B4 61.3(4) . . ? B10 B5 B4 112.0(5) . . ? C1 B5 Mo 70.2(3) . . ? B9 B5 Mo 123.9(4) . . ? B10 B5 Mo 126.9(4) . . ? B4 B5 Mo 66.9(3) . . ? B5 C1 B10 62.1(4) . . ? B5 C1 B2 111.5(5) . . ? B10 C1 B2 111.5(5) . . ? B5 C1 B6 110.3(5) . . ? B10 C1 B6 60.9(4) . . ? B2 C1 B6 60.5(4) . . ? B5 C1 Mo 70.4(3) . . ? B10 C1 Mo 128.1(4) . . ? B2 C1 Mo 67.4(3) . . ? B6 C1 Mo 123.8(4) . . ? C1 B2 B6 59.8(4) . . ? C1 B2 B7 105.3(5) . . ? B6 B2 B7 60.0(4) . . ? C1 B2 B3 105.6(5) . . ? B6 B2 B3 107.4(5) . . ? B7 B2 B3 58.3(4) . . ? C1 B2 Mo 70.5(3) . . ? B6 B2 Mo 126.0(4) . . ? B7 B2 Mo 120.6(5) . . ? B3 B2 Mo 66.0(3) . . ? B7 B3 B8 58.9(5) . . ? B7 B3 B4 106.4(5) . . ? B8 B3 B4 59.6(4) . . ? B7 B3 B2 58.9(4) . . ? B8 B3 B2 105.3(5) . . ? B4 B3 B2 105.8(5) . . ? B7 B3 Mo 123.3(5) . . ? B8 B3 Mo 123.6(4) . . ? B4 B3 Mo 68.5(3) . . ? B2 B3 Mo 68.3(3) . . ? B5 B4 B9 58.6(4) . . ? B5 B4 B8 104.2(5) . . ? B9 B4 B8 59.2(4) . . ? B5 B4 B3 105.9(5) . . ? B9 B4 B3 106.9(5) . . ? B8 B4 B3 58.8(4) . . ? B5 B4 Mo 70.6(3) . . ? B9 B4 Mo 124.8(4) . . ? B8 B4 Mo 121.0(5) . . ? B3 B4 Mo 66.5(3) . . ? B8 B7 B3 60.6(5) . . ? B8 B7 B6 108.2(5) . . ? B3 B7 B6 110.5(5) . . ? B8 B7 B11 60.5(5) . . ? B3 B7 B11 110.4(6) . . ? B6 B7 B11 59.7(4) . . ? B8 B7 B2 109.7(6) . . ? B3 B7 B2 62.8(4) . . ? B6 B7 B2 59.4(4) . . ? B11 B7 B2 108.3(5) . . ? C1 B6 B2 59.8(4) . . ? C1 B6 B10 59.1(4) . . ? B2 B6 B10 109.4(5) . . ? C1 B6 B11 105.9(5) . . ? B2 B6 B11 109.6(6) . . ? B10 B6 B11 60.0(4) . . ? C1 B6 B7 105.7(5) . . ? B2 B6 B7 60.6(4) . . ? B10 B6 B7 108.0(6) . . ? B11 B6 B7 60.1(4) . . ? C1 B10 B5 56.8(4) . . ? C1 B10 B11 106.6(5) . . ? B5 B10 B11 106.2(5) . . ? C1 B10 B6 60.0(4) . . ? B5 B10 B6 105.4(5) . . ? B11 B10 B6 60.1(4) . . ? C1 B10 B9 104.7(5) . . ? B5 B10 B9 59.0(4) . . ? B11 B10 B9 60.1(4) . . ? B6 B10 B9 107.5(6) . . ? B5 B9 B8 106.5(5) . . ? B5 B9 B11 106.6(5) . . ? B8 B9 B11 60.1(5) . . ? B5 B9 B10 59.8(4) . . ? B8 B9 B10 108.0(6) . . ? B11 B9 B10 59.7(4) . . ? B5 B9 B4 60.1(4) . . ? B8 B9 B4 60.6(4) . . ? B11 B9 B4 109.7(5) . . ? B10 B9 B4 109.9(5) . . ? B7 B8 B9 108.3(6) . . ? B7 B8 B11 60.6(5) . . ? B9 B8 B11 60.1(4) . . ? B7 B8 B3 60.5(4) . . ? B9 B8 B3 110.0(5) . . ? B11 B8 B3 110.3(6) . . ? B7 B8 B4 109.2(6) . . ? B9 B8 B4 60.2(4) . . ? B11 B8 B4 109.3(5) . . ? B3 B8 B4 61.6(4) . . ? B10 B11 B6 60.0(4) . . ? B10 B11 B9 60.2(4) . . ? B6 B11 B9 107.5(5) . . ? B10 B11 B8 108.1(5) . . ? B6 B11 B8 107.3(5) . . ? B9 B11 B8 59.7(5) . . ? B10 B11 B7 108.0(5) . . ? B6 B11 B7 60.1(5) . . ? B9 B11 B7 106.7(6) . . ? B8 B11 B7 58.9(5) . . ? N10 C10 Mo 176.2(5) . . ? C10 N10 C11 169.2(8) . . ? N10 C11 C14 107.9(7) . . ? N10 C11 C12 105.5(7) . . ? C14 C11 C12 112.3(7) . . ? N10 C11 C13 106.6(6) . . ? C14 C11 C13 112.0(8) . . ? C12 C11 C13 112.1(8) . . ? N20 C20 Mo 175.7(6) . . ? C20 N20 C21 173.4(7) . . ? N20 C21 C23 108.8(6) . . ? N20 C21 C24 107.9(6) . . ? C23 C21 C24 112.7(7) . . ? N20 C21 C22 105.6(6) . . ? C23 C21 C22 111.3(8) . . ? C24 C21 C22 110.3(8) . . ? N30 C30 Mo 177.5(6) . . ? C30 N30 C31 171.4(7) . . ? C32A C31 N30 114(3) . . ? C32A C31 C34 134(3) . . ? N30 C31 C34 107.6(7) . . ? C32A C31 C33 37(2) . . ? N30 C31 C33 105.3(6) . . ? C34 C31 C33 112.9(10) . . ? C32A C31 C32 72(3) . . ? N30 C31 C32 108.7(7) . . ? C34 C31 C32 113.2(9) . . ? C33 C31 C32 108.8(10) . . ? C32A C31 C34A 131(3) . . ? N30 C31 C34A 99.2(16) . . ? C34 C31 C34A 56.7(19) . . ? C33 C31 C34A 155.4(17) . . ? C32 C31 C34A 64(2) . . ? C32A C31 C33A 112(3) . . ? N30 C31 C33A 96.7(16) . . ? C34 C31 C33A 42.1(15) . . ? C33 C31 C33A 77.6(16) . . ? C32 C31 C33A 150.4(17) . . ? C34A C31 C33A 98(3) . . ? N40 C40 Mo 173.9(6) . . ? C40 N40 C41 172.3(7) . . ? N40 C41 C42 108.0(6) . . ? N40 C41 C43 105.5(7) . . ? C42 C41 C43 112.0(7) . . ? N40 C41 C44 106.1(6) . . ? C42 C41 C44 112.0(7) . . ? C43 C41 C44 112.7(7) . . ? Cl1A Cl1 C50 68(2) . . ? Cl1 C50 Cl2 110.6(14) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 24.96 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.630 _refine_diff_density_min -0.682 _refine_diff_density_rms 0.097 #===END data_8 _database_code_CSD 166147 _chemical_formula_moiety ; [N(PPh~3~)~2~][2,2,2-(CO)~3~-2-I-7-{O(CH~2~)~4~}-closo-2,1-MoCB~10~H~10~] ; _chemical_formula_sum 'C44 H48 B10 I Mo N O4 P2' _chemical_formula_weight 1047.71 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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mo' 'Mo' -1.6832 0.6857 '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 Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.4517(14) _cell_length_b 10.6686(15) _cell_length_c 29.866(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.233(14) _cell_angle_gamma 90.00 _cell_volume 4884.2(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10 _cell_measurement_theta_max 15 _exptl_crystal_description blocks _exptl_crystal_colour red _exptl_crystal_size_max 0.54 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.425 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2104 _exptl_absorpt_coefficient_mu 1.007 _exptl_absorpt_correction_type 'Numerical, SHELXTL-PC vs. 5.03' _exptl_absorpt_correction_T_min 0.6122 _exptl_absorpt_correction_T_max 0.7868 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf-Nonius CAD4' _diffrn_measurement_method \w-2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 3.72 _diffrn_reflns_number 6505 _diffrn_reflns_av_R_equivalents 0.0673 _diffrn_reflns_av_sigmaI/netI 0.0465 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 22.50 _reflns_number_total 6286 _reflns_number_gt 4524 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Enraf-Nonius CAD4 (1989)' _computing_cell_refinement 'Enraf-Nonius CAD4 (1989)' _computing_data_reduction 'XCAD4 Siemens Software (Harms, 1993)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in SHELXTL-PC (Bruker, 1995)' _computing_publication_material 'SHELXL-97 (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^)+(0.0167P)^2^+12.9144P] 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 6286 _refine_ls_number_parameters 568 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0803 _refine_ls_R_factor_gt 0.0499 _refine_ls_wR_factor_ref 0.0997 _refine_ls_wR_factor_gt 0.0886 _refine_ls_goodness_of_fit_ref 1.165 _refine_ls_restrained_S_all 1.165 _refine_ls_shift/su_max 0.006 _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 Mo Mo 0.29517(4) 0.19335(5) 0.096909(19) 0.04380(17) Uani 1 1 d . . . C1 C 0.2648(4) 0.0635(6) 0.1588(2) 0.0496(17) Uani 1 1 d . . . H1 H 0.3119 -0.0136 0.1583 0.060 Uiso 1 1 calc R . . B2 B 0.3018(5) 0.2060(7) 0.1772(2) 0.049(2) Uani 1 1 d . . . H2 H 0.3702 0.2280 0.1897 0.059 Uiso 1 1 calc R . . B3 B 0.2265(5) 0.3150(7) 0.1477(3) 0.048(2) Uani 1 1 d . . . B4 B 0.1511(5) 0.2332(8) 0.1101(3) 0.062(2) Uani 1 1 d . . . H4 H 0.1180 0.2743 0.0787 0.075 Uiso 1 1 calc R . . B5 B 0.1801(5) 0.0689(8) 0.1171(3) 0.056(2) Uani 1 1 d . . . H5 H 0.1676 -0.0006 0.0898 0.067 Uiso 1 1 calc R . . B6 B 0.2406(6) 0.1085(8) 0.2098(3) 0.064(3) Uani 1 1 d . . . H6 H 0.2708 0.0694 0.2421 0.077 Uiso 1 1 calc R . . B7 B 0.2137(6) 0.2696(8) 0.2040(3) 0.060(2) Uani 1 1 d . . . H7 H 0.2252 0.3349 0.2326 0.072 Uiso 1 1 calc R . . B8 B 0.1225(5) 0.2837(9) 0.1625(3) 0.068(3) Uani 1 1 d . . . H8 H 0.0737 0.3581 0.1644 0.081 Uiso 1 1 calc R . . B9 B 0.0943(6) 0.1320(9) 0.1428(4) 0.078(3) Uani 1 1 d . . . H9 H 0.0265 0.1063 0.1305 0.094 Uiso 1 1 calc R . . B10 B 0.1666(5) 0.0158(10) 0.1766(3) 0.079(3) Uani 1 1 d . . . H10 H 0.1487 -0.0788 0.1868 0.095 Uiso 1 1 calc R . . B11 B 0.1309(6) 0.1567(8) 0.2001(3) 0.074(3) Uani 1 1 d . . . H11 H 0.0861 0.1497 0.2258 0.089 Uiso 1 1 calc R . . C2 C 0.4192(5) 0.2542(7) 0.1120(2) 0.063(2) Uani 1 1 d . . . O2 O 0.4879(3) 0.2917(6) 0.1201(2) 0.0923(19) Uani 1 1 d . . . C3 C 0.2934(5) 0.3481(7) 0.0626(2) 0.067(2) Uani 1 1 d . . . O3 O 0.2897(4) 0.4427(5) 0.04411(18) 0.098(2) Uani 1 1 d . . . C4 C 0.2413(5) 0.1404(7) 0.0355(3) 0.068(2) Uani 1 1 d . . . O4 O 0.2077(4) 0.1158(5) 0.0003(2) 0.103(2) Uani 1 1 d . . . I I 0.40352(4) -0.01034(5) 0.073342(19) 0.0760(2) Uani 1 1 d . . . O5 O 0.2475(3) 0.4573(4) 0.14443(15) 0.0559(12) Uani 1 1 d . . . C5 C 0.1828(5) 0.5526(7) 0.1298(3) 0.094(3) Uani 1 1 d . . . H5A H 0.1381 0.5562 0.1498 0.113 Uiso 1 1 calc R . . H5B H 0.1553 0.5359 0.0993 0.113 Uiso 1 1 calc R . . C6 C 0.2325(7) 0.6692(8) 0.1315(4) 0.128(4) Uani 1 1 d . . . H6A H 0.2419 0.6941 0.1013 0.154 Uiso 1 1 calc R . . H6B H 0.2003 0.7353 0.1444 0.154 Uiso 1 1 calc R . . C7 C 0.3152(7) 0.6502(7) 0.1588(3) 0.103(3) Uani 1 1 d . . . H7A H 0.3165 0.6956 0.1871 0.124 Uiso 1 1 calc R . . H7B H 0.3621 0.6811 0.1431 0.124 Uiso 1 1 calc R . . C8 C 0.3265(5) 0.5138(6) 0.1679(3) 0.065(2) Uani 1 1 d . . . H8A H 0.3780 0.4823 0.1561 0.079 Uiso 1 1 calc R . . H8B H 0.3317 0.4967 0.2000 0.079 Uiso 1 1 calc R . . N N 0.7820(3) 0.4668(5) 0.15276(17) 0.0491(14) Uani 1 1 d . . . P1 P 0.76719(10) 0.35815(15) 0.18632(5) 0.0385(4) Uani 1 1 d . . . C11 C 0.7700(4) 0.2035(6) 0.1626(2) 0.0429(16) Uani 1 1 d . . . C12 C 0.8421(4) 0.1276(6) 0.1724(2) 0.0550(18) Uani 1 1 d . . . H12 H 0.8880 0.1531 0.1936 0.066 Uiso 1 1 calc R . . C13 C 0.8463(6) 0.0146(7) 0.1511(3) 0.076(2) Uani 1 1 d . . . H13 H 0.8944 -0.0373 0.1583 0.092 Uiso 1 1 calc R . . C14 C 0.7795(6) -0.0220(7) 0.1191(3) 0.079(2) Uani 1 1 d . . . H14 H 0.7834 -0.0974 0.1039 0.095 Uiso 1 1 calc R . . C15 C 0.7070(6) 0.0523(8) 0.1094(3) 0.077(2) Uani 1 1 d . . . H15 H 0.6613 0.0267 0.0881 0.092 Uiso 1 1 calc R . . C16 C 0.7024(4) 0.1641(6) 0.1313(2) 0.0565(19) Uani 1 1 d . . . H16 H 0.6532 0.2142 0.1250 0.068 Uiso 1 1 calc R . . C21 C 0.6646(4) 0.3732(6) 0.2077(2) 0.0423(16) Uani 1 1 d . . . C22 C 0.6245(4) 0.2706(7) 0.2254(2) 0.0526(18) Uani 1 1 d . . . H22 H 0.6497 0.1915 0.2251 0.063 Uiso 1 1 calc R . . C23 C 0.5473(5) 0.2871(8) 0.2431(2) 0.063(2) Uani 1 1 d . . . H23 H 0.5205 0.2186 0.2549 0.076 Uiso 1 1 calc R . . C24 C 0.5098(5) 0.4021(9) 0.2438(2) 0.071(2) Uani 1 1 d . . . H24 H 0.4580 0.4117 0.2563 0.086 Uiso 1 1 calc R . . C25 C 0.5471(5) 0.5032(8) 0.2264(2) 0.068(2) Uani 1 1 d . . . H25 H 0.5208 0.5816 0.2266 0.081 Uiso 1 1 calc R . . C26 C 0.6251(4) 0.4881(7) 0.2081(2) 0.0548(18) Uani 1 1 d . . . H26 H 0.6508 0.5571 0.1960 0.066 Uiso 1 1 calc R . . C31 C 0.8507(4) 0.3704(6) 0.2338(2) 0.0436(16) Uani 1 1 d . . . C32 C 0.9336(4) 0.4017(7) 0.2262(2) 0.063(2) Uani 1 1 d . . . H32 H 0.9455 0.4163 0.1969 0.076 Uiso 1 1 calc R . . C33 C 1.0000(5) 0.4118(8) 0.2619(4) 0.086(3) Uani 1 1 d . . . H33 H 1.0563 0.4322 0.2564 0.104 Uiso 1 1 calc R . . C34 C 0.9830(6) 0.3922(9) 0.3043(3) 0.093(3) Uani 1 1 d . . . H34 H 1.0273 0.4009 0.3283 0.112 Uiso 1 1 calc R . . C35 C 0.9015(6) 0.3598(9) 0.3126(3) 0.094(3) Uani 1 1 d . . . H35 H 0.8906 0.3451 0.3421 0.113 Uiso 1 1 calc R . . C36 C 0.8343(5) 0.3483(7) 0.2774(2) 0.067(2) Uani 1 1 d . . . H36 H 0.7787 0.3259 0.2832 0.080 Uiso 1 1 calc R . . P2 P 0.78149(11) 0.50078(16) 0.10134(6) 0.0439(4) Uani 1 1 d . . . C41 C 0.7999(4) 0.3727(6) 0.0652(2) 0.0452(17) Uani 1 1 d . . . C42 C 0.8774(5) 0.3053(7) 0.0741(2) 0.060(2) Uani 1 1 d . . . H42 H 0.9168 0.3265 0.0991 0.072 Uiso 1 1 calc R . . C43 C 0.8969(6) 0.2084(8) 0.0469(3) 0.079(2) Uani 1 1 d . . . H43 H 0.9491 0.1645 0.0530 0.095 Uiso 1 1 calc R . . C44 C 0.8381(8) 0.1780(9) 0.0107(3) 0.093(3) Uani 1 1 d . . . H44 H 0.8504 0.1121 -0.0079 0.111 Uiso 1 1 calc R . . C45 C 0.7629(7) 0.2404(9) 0.0011(3) 0.094(3) Uani 1 1 d . . . H45 H 0.7242 0.2183 -0.0241 0.113 Uiso 1 1 calc R . . C46 C 0.7427(5) 0.3371(7) 0.0283(3) 0.072(2) Uani 1 1 d . . . H46 H 0.6898 0.3789 0.0218 0.086 Uiso 1 1 calc R . . C51 C 0.6814(4) 0.5760(7) 0.0791(2) 0.0498(17) Uani 1 1 d . . . C52 C 0.6040(5) 0.5198(8) 0.0850(3) 0.092(3) Uani 1 1 d . . . H52 H 0.6042 0.4450 0.1010 0.111 Uiso 1 1 calc R . . C53 C 0.5261(5) 0.5728(10) 0.0676(4) 0.111(4) Uani 1 1 d . . . H53 H 0.4742 0.5326 0.0716 0.133 Uiso 1 1 calc R . . C54 C 0.5237(6) 0.6818(9) 0.0450(3) 0.088(3) Uani 1 1 d . . . H54 H 0.4705 0.7171 0.0333 0.106 Uiso 1 1 calc R . . C55 C 0.5996(6) 0.7395(8) 0.0392(3) 0.080(2) Uani 1 1 d . . . H55 H 0.5986 0.8147 0.0235 0.097 Uiso 1 1 calc R . . C56 C 0.6788(5) 0.6870(7) 0.0568(2) 0.0614(19) Uani 1 1 d . . . H56 H 0.7305 0.7282 0.0532 0.074 Uiso 1 1 calc R . . C61 C 0.8694(4) 0.6074(6) 0.0963(2) 0.0453(17) Uani 1 1 d . . . C62 C 0.8973(5) 0.6277(7) 0.0550(3) 0.072(2) Uani 1 1 d . . . H62 H 0.8704 0.5861 0.0296 0.086 Uiso 1 1 calc R . . C63 C 0.9648(6) 0.7095(9) 0.0510(3) 0.091(3) Uani 1 1 d . . . H63 H 0.9832 0.7229 0.0229 0.110 Uiso 1 1 calc R . . C64 C 1.0047(5) 0.7708(8) 0.0877(4) 0.085(3) Uani 1 1 d . . . H64 H 1.0496 0.8270 0.0848 0.102 Uiso 1 1 calc R . . C65 C 0.9783(5) 0.7490(7) 0.1290(3) 0.071(2) Uani 1 1 d . . . H65 H 1.0065 0.7892 0.1543 0.085 Uiso 1 1 calc R . . C66 C 0.9107(4) 0.6688(6) 0.1335(2) 0.0536(18) Uani 1 1 d . . . H66 H 0.8927 0.6559 0.1617 0.064 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 Mo 0.0464(3) 0.0365(3) 0.0482(4) 0.0023(3) 0.0051(3) -0.0052(3) C1 0.060(4) 0.040(4) 0.049(4) 0.007(3) 0.010(3) -0.002(3) B2 0.058(5) 0.042(5) 0.046(5) 0.001(4) 0.004(4) 0.001(4) B3 0.043(4) 0.039(5) 0.065(5) 0.007(4) 0.017(4) -0.001(4) B4 0.042(5) 0.052(6) 0.093(7) -0.001(5) 0.011(5) -0.013(4) B5 0.050(5) 0.050(5) 0.066(6) 0.000(4) 0.004(4) -0.014(4) B6 0.088(7) 0.048(5) 0.061(6) 0.011(4) 0.032(5) 0.003(5) B7 0.072(6) 0.047(5) 0.066(6) 0.000(4) 0.026(5) 0.002(4) B8 0.050(5) 0.060(6) 0.097(7) 0.005(5) 0.026(5) 0.006(5) B9 0.047(5) 0.071(7) 0.117(9) 0.010(6) 0.013(5) -0.018(5) B10 0.034(5) 0.083(7) 0.125(9) -0.065(7) 0.024(5) -0.019(5) B11 0.073(6) 0.061(6) 0.097(8) 0.005(6) 0.042(6) -0.004(5) C2 0.061(5) 0.059(5) 0.070(5) -0.007(4) 0.011(4) -0.013(4) O2 0.052(3) 0.095(4) 0.131(5) -0.003(4) 0.017(3) -0.025(3) C3 0.107(6) 0.049(5) 0.046(5) 0.002(4) 0.010(4) -0.011(5) O3 0.172(6) 0.051(4) 0.072(4) 0.021(3) 0.024(4) -0.004(4) C4 0.100(6) 0.046(5) 0.054(5) 0.008(4) -0.006(5) -0.019(4) O4 0.163(6) 0.071(4) 0.065(4) 0.005(3) -0.032(4) -0.027(4) I 0.0906(4) 0.0637(4) 0.0741(4) -0.0104(3) 0.0114(3) 0.0197(3) O5 0.065(3) 0.031(3) 0.070(3) 0.003(2) 0.001(3) 0.003(2) C5 0.073(6) 0.046(5) 0.158(9) 0.018(5) 0.000(6) 0.019(5) C6 0.122(9) 0.038(6) 0.214(13) 0.017(7) -0.018(9) 0.001(6) C7 0.131(9) 0.047(6) 0.128(9) 0.004(5) -0.001(7) -0.029(6) C8 0.072(5) 0.047(5) 0.076(5) -0.006(4) 0.003(4) -0.014(4) N 0.067(4) 0.037(3) 0.044(3) -0.004(3) 0.011(3) -0.006(3) P1 0.0392(9) 0.0362(10) 0.0406(10) -0.0019(8) 0.0067(8) 0.0003(8) C11 0.054(4) 0.035(4) 0.042(4) 0.000(3) 0.015(3) -0.007(3) C12 0.061(5) 0.042(4) 0.061(5) -0.002(4) 0.001(4) 0.007(4) C13 0.092(6) 0.044(5) 0.094(6) -0.012(5) 0.012(5) 0.019(5) C14 0.115(7) 0.042(5) 0.082(6) -0.021(5) 0.020(6) -0.001(5) C15 0.097(7) 0.055(6) 0.073(6) -0.014(5) -0.009(5) -0.018(5) C16 0.057(5) 0.045(5) 0.067(5) 0.000(4) 0.003(4) -0.003(4) C21 0.038(4) 0.047(4) 0.042(4) -0.009(3) 0.004(3) 0.004(3) C22 0.050(4) 0.054(5) 0.054(4) 0.000(4) 0.010(4) 0.000(4) C23 0.052(5) 0.083(6) 0.057(5) 0.003(4) 0.014(4) -0.011(4) C24 0.053(5) 0.106(8) 0.057(5) -0.009(5) 0.016(4) 0.006(5) C25 0.060(5) 0.077(6) 0.066(5) -0.016(5) 0.005(4) 0.024(5) C26 0.051(4) 0.053(5) 0.063(5) -0.010(4) 0.015(4) 0.005(4) C31 0.042(4) 0.042(4) 0.047(4) -0.011(3) 0.003(3) 0.005(3) C32 0.049(5) 0.081(6) 0.058(5) -0.011(4) 0.002(4) 0.004(4) C33 0.052(5) 0.091(7) 0.113(8) -0.030(6) -0.001(6) 0.000(5) C34 0.067(6) 0.122(8) 0.083(7) -0.046(6) -0.022(5) 0.033(6) C35 0.098(7) 0.134(9) 0.048(5) -0.024(5) 0.000(5) 0.036(7) C36 0.057(5) 0.096(6) 0.047(5) -0.005(4) 0.005(4) 0.007(4) P2 0.0449(10) 0.0420(10) 0.0443(10) 0.0022(9) 0.0038(8) -0.0107(9) C41 0.051(4) 0.049(4) 0.037(4) -0.001(3) 0.007(3) -0.018(4) C42 0.070(5) 0.063(5) 0.050(4) -0.011(4) 0.015(4) -0.013(4) C43 0.096(7) 0.070(6) 0.080(6) -0.014(5) 0.041(5) -0.002(5) C44 0.147(10) 0.065(7) 0.072(7) -0.029(5) 0.039(7) -0.034(7) C45 0.138(9) 0.078(7) 0.059(6) -0.016(5) -0.011(6) -0.043(7) C46 0.092(6) 0.061(6) 0.060(5) 0.001(4) -0.001(5) -0.027(5) C51 0.046(4) 0.054(5) 0.050(4) 0.004(4) 0.005(3) -0.009(4) C52 0.053(5) 0.096(7) 0.125(8) 0.061(6) -0.004(5) -0.006(5) C53 0.048(6) 0.114(9) 0.169(11) 0.046(8) 0.005(6) -0.009(6) C54 0.064(6) 0.089(7) 0.106(7) -0.002(6) -0.012(5) 0.021(6) C55 0.085(6) 0.055(5) 0.097(7) 0.003(5) -0.006(5) 0.009(5) C56 0.062(5) 0.049(5) 0.072(5) 0.004(4) 0.002(4) -0.003(4) C61 0.041(4) 0.038(4) 0.058(5) 0.005(4) 0.008(3) -0.007(3) C62 0.063(5) 0.085(6) 0.066(5) -0.001(5) 0.006(4) -0.034(5) C63 0.085(6) 0.102(7) 0.091(7) 0.018(6) 0.023(5) -0.042(6) C64 0.054(5) 0.059(6) 0.144(9) 0.019(6) 0.014(6) -0.021(4) C65 0.054(5) 0.048(5) 0.109(7) -0.018(5) 0.002(5) -0.011(4) C66 0.045(4) 0.041(4) 0.075(5) -0.009(4) 0.009(4) -0.010(3) _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 Mo C3 1.942(8) . y Mo C4 1.998(8) . y Mo C2 2.019(8) . y Mo B4 2.347(8) . y Mo B3 2.349(8) . y Mo B5 2.357(8) . y Mo B2 2.390(7) . y Mo C1 2.403(6) . y Mo I 2.8839(8) . y C1 B6 1.683(10) . ? C1 B5 1.689(10) . ? C1 B2 1.692(10) . ? C1 B10 1.745(10) . ? B2 B6 1.777(11) . ? B2 B3 1.795(11) . ? B2 B7 1.798(11) . ? B3 O5 1.558(8) . y B3 B4 1.747(11) . ? B3 B8 1.753(10) . ? B3 B7 1.784(11) . ? B4 B9 1.764(12) . ? B4 B8 1.765(12) . ? B4 B5 1.815(12) . ? B5 B9 1.750(12) . ? B5 B10 1.901(13) . ? B6 B10 1.727(12) . ? B6 B11 1.760(12) . ? B6 B7 1.771(11) . ? B7 B11 1.750(12) . ? B7 B8 1.762(12) . ? B8 B11 1.754(13) . ? B8 B9 1.758(13) . ? B9 B11 1.753(14) . ? B9 B10 1.876(14) . ? B10 B11 1.776(12) . ? C2 O2 1.132(7) . y C3 O3 1.149(8) . y C4 O4 1.142(8) . y O5 C5 1.455(8) . y O5 C8 1.459(7) . y C5 C6 1.459(10) . ? C6 C7 1.440(11) . ? C7 C8 1.486(10) . ? N P1 1.568(5) . ? N P2 1.577(5) . ? P1 C21 1.789(6) . ? P1 C31 1.797(6) . ? P1 C11 1.799(6) . ? C11 C16 1.376(8) . ? C11 C12 1.379(8) . ? C12 C13 1.368(9) . ? C13 C14 1.372(10) . ? C14 C15 1.373(10) . ? C15 C16 1.367(9) . ? C21 C26 1.371(8) . ? C21 C22 1.394(8) . ? C22 C23 1.375(9) . ? C23 C24 1.359(10) . ? C24 C25 1.357(10) . ? C25 C26 1.394(9) . ? C31 C32 1.370(8) . ? C31 C36 1.377(9) . ? C32 C33 1.387(10) . ? C33 C34 1.343(11) . ? C34 C35 1.359(11) . ? C35 C36 1.386(10) . ? P2 C41 1.787(7) . ? P2 C61 1.793(6) . ? P2 C51 1.794(7) . ? C41 C46 1.375(9) . ? C41 C42 1.394(9) . ? C42 C43 1.372(10) . ? C43 C44 1.361(11) . ? C44 C45 1.339(12) . ? C45 C46 1.373(11) . ? C51 C56 1.358(9) . ? C51 C52 1.368(9) . ? C52 C53 1.371(10) . ? C53 C54 1.343(11) . ? C54 C55 1.355(11) . ? C55 C56 1.387(10) . ? C61 C62 1.374(9) . ? C61 C66 1.375(8) . ? C62 C63 1.376(10) . ? C63 C64 1.356(11) . ? C64 C65 1.366(11) . ? C65 C66 1.370(9) . ? 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 Mo C4 77.3(3) . . y C3 Mo C2 78.1(3) . . y C4 Mo C2 124.7(3) . . y C3 Mo B4 89.1(3) . . y C4 Mo B4 84.9(3) . . y C2 Mo B4 142.9(3) . . y C3 Mo B3 83.9(3) . . y C4 Mo B3 125.4(3) . . y C2 Mo B3 99.9(3) . . y B4 Mo B3 43.7(3) . . ? C3 Mo B5 130.8(3) . . y C4 Mo B5 80.5(3) . . y C2 Mo B5 148.1(3) . . y B4 Mo B5 45.4(3) . . ? B3 Mo B5 74.3(3) . . ? C3 Mo B2 118.5(3) . . y C4 Mo B2 153.8(3) . . y C2 Mo B2 80.7(3) . . y B4 Mo B2 75.2(3) . . ? B3 Mo B2 44.5(3) . . ? B5 Mo B2 73.4(3) . . ? C3 Mo C1 154.8(3) . . y C4 Mo C1 116.3(3) . . y C2 Mo C1 106.6(3) . . y B4 Mo C1 72.2(3) . . ? B3 Mo C1 71.0(2) . . ? B5 Mo C1 41.6(2) . . ? B2 Mo C1 41.3(2) . . ? C3 Mo I 118.8(2) . . y C4 Mo I 75.5(2) . . y C2 Mo I 74.5(2) . . y B4 Mo I 140.3(2) . . y B3 Mo I 153.80(19) . . y B5 Mo I 96.7(2) . . y B2 Mo I 109.53(18) . . y C1 Mo I 85.93(16) . . y B6 C1 B5 114.7(6) . . ? B6 C1 B2 63.5(4) . . ? B5 C1 B2 114.1(5) . . ? B6 C1 B10 60.5(5) . . ? B5 C1 B10 67.2(5) . . ? B2 C1 B10 115.8(5) . . ? B6 C1 Mo 128.2(4) . . ? B5 C1 Mo 67.8(3) . . ? B2 C1 Mo 68.9(3) . . ? B10 C1 Mo 131.6(5) . . ? C1 B2 B6 58.0(4) . . ? C1 B2 B3 104.5(5) . . ? B6 B2 B3 106.9(6) . . ? C1 B2 B7 103.8(5) . . ? B6 B2 B7 59.4(4) . . ? B3 B2 B7 59.6(4) . . ? C1 B2 Mo 69.7(3) . . ? B6 B2 Mo 123.9(5) . . ? B3 B2 Mo 66.5(3) . . ? B7 B2 Mo 121.9(5) . . ? O5 B3 B4 125.0(6) . . y O5 B3 B8 114.0(6) . . y B4 B3 B8 60.6(5) . . ? O5 B3 B7 111.9(6) . . y B4 B3 B7 109.1(6) . . ? B8 B3 B7 59.8(5) . . ? O5 B3 B2 122.3(6) . . y B4 B3 B2 109.3(6) . . ? B8 B3 B2 108.2(6) . . ? B7 B3 B2 60.3(4) . . ? O5 B3 Mo 112.5(4) . . y B4 B3 Mo 68.1(4) . . ? B8 B3 Mo 124.1(5) . . ? B7 B3 Mo 124.8(5) . . ? B2 B3 Mo 69.0(3) . . ? B3 B4 B9 106.7(7) . . ? B3 B4 B8 59.9(5) . . ? B9 B4 B8 59.7(5) . . ? B3 B4 B5 105.9(6) . . ? B9 B4 B5 58.5(5) . . ? B8 B4 B5 106.2(6) . . ? B3 B4 Mo 68.2(4) . . ? B9 B4 Mo 122.1(5) . . ? B8 B4 Mo 123.6(5) . . ? B5 B4 Mo 67.6(4) . . ? C1 B5 B9 104.4(6) . . ? C1 B5 B4 106.0(6) . . ? B9 B5 B4 59.3(5) . . ? C1 B5 B10 57.8(4) . . ? B9 B5 B10 61.7(5) . . ? B4 B5 B10 109.9(6) . . ? C1 B5 Mo 70.7(3) . . ? B9 B5 Mo 122.2(5) . . ? B4 B5 Mo 67.0(3) . . ? B10 B5 Mo 125.6(5) . . ? C1 B6 B10 61.5(5) . . ? C1 B6 B11 104.7(7) . . ? B10 B6 B11 61.2(5) . . ? C1 B6 B7 105.3(6) . . ? B10 B6 B7 111.6(7) . . ? B11 B6 B7 59.4(5) . . ? C1 B6 B2 58.5(4) . . ? B10 B6 B2 112.3(7) . . ? B11 B6 B2 107.9(6) . . ? B7 B6 B2 60.9(4) . . ? B11 B7 B8 59.9(5) . . ? B11 B7 B6 60.0(5) . . ? B8 B7 B6 108.0(7) . . ? B11 B7 B3 106.9(6) . . ? B8 B7 B3 59.2(5) . . ? B6 B7 B3 107.6(6) . . ? B11 B7 B2 107.4(6) . . ? B8 B7 B2 107.6(6) . . ? B6 B7 B2 59.7(4) . . ? B3 B7 B2 60.2(4) . . ? B3 B8 B11 108.2(6) . . ? B3 B8 B9 106.7(6) . . ? B11 B8 B9 59.9(5) . . ? B3 B8 B7 61.0(5) . . ? B11 B8 B7 59.7(5) . . ? B9 B8 B7 107.4(6) . . ? B3 B8 B4 59.6(4) . . ? B11 B8 B4 109.0(6) . . ? B9 B8 B4 60.1(5) . . ? B7 B8 B4 109.2(6) . . ? B5 B9 B11 108.5(7) . . ? B5 B9 B8 109.4(6) . . ? B11 B9 B8 60.0(5) . . ? B5 B9 B4 62.2(5) . . ? B11 B9 B4 109.1(7) . . ? B8 B9 B4 60.2(5) . . ? B5 B9 B10 63.1(5) . . ? B11 B9 B10 58.5(5) . . ? B8 B9 B10 108.8(7) . . ? B4 B9 B10 113.4(6) . . ? B6 B10 C1 58.0(4) . . ? B6 B10 B11 60.3(5) . . ? C1 B10 B11 101.5(6) . . ? B6 B10 B9 103.7(7) . . ? C1 B10 B9 97.2(7) . . ? B11 B10 B9 57.3(5) . . ? B6 B10 B5 102.9(6) . . ? C1 B10 B5 55.0(4) . . ? B11 B10 B5 101.2(7) . . ? B9 B10 B5 55.2(5) . . ? B7 B11 B9 108.2(6) . . ? B7 B11 B8 60.4(5) . . ? B9 B11 B8 60.2(5) . . ? B7 B11 B6 60.6(5) . . ? B9 B11 B6 107.6(6) . . ? B8 B11 B6 108.9(6) . . ? B7 B11 B10 110.4(6) . . ? B9 B11 B10 64.2(6) . . ? B8 B11 B10 113.7(7) . . ? B6 B11 B10 58.5(5) . . ? O2 C2 Mo 178.0(7) . . y O3 C3 Mo 176.1(7) . . y O4 C4 Mo 176.2(7) . . y C5 O5 C8 110.9(5) . . y C5 O5 B3 124.0(5) . . y C8 O5 B3 122.8(5) . . y O5 C5 C6 104.2(6) . . y C7 C6 C5 109.0(7) . . ? C6 C7 C8 108.4(7) . . ? O5 C8 C7 104.2(6) . . ? P1 N P2 144.0(3) . . ? N P1 C21 111.7(3) . . ? N P1 C31 107.6(3) . . ? C21 P1 C31 107.0(3) . . ? N P1 C11 114.4(3) . . ? C21 P1 C11 106.8(3) . . ? C31 P1 C11 109.1(3) . . ? C16 C11 C12 119.3(6) . . ? C16 C11 P1 119.6(5) . . ? C12 C11 P1 120.9(5) . . ? C13 C12 C11 120.2(7) . . ? C12 C13 C14 120.0(8) . . ? C13 C14 C15 120.3(7) . . ? C16 C15 C14 119.5(7) . . ? C15 C16 C11 120.7(7) . . ? C26 C21 C22 118.6(6) . . ? C26 C21 P1 119.9(5) . . ? C22 C21 P1 121.4(5) . . ? C23 C22 C21 119.6(7) . . ? C24 C23 C22 120.9(7) . . ? C25 C24 C23 120.6(7) . . ? C24 C25 C26 119.3(7) . . ? C21 C26 C25 121.0(7) . . ? C32 C31 C36 119.0(6) . . ? C32 C31 P1 118.8(5) . . ? C36 C31 P1 122.3(5) . . ? C31 C32 C33 120.6(7) . . ? C34 C33 C32 119.9(8) . . ? C33 C34 C35 120.5(8) . . ? C34 C35 C36 120.5(8) . . ? C31 C36 C35 119.6(7) . . ? N P2 C41 115.6(3) . . ? N P2 C61 108.5(3) . . ? C41 P2 C61 104.7(3) . . ? N P2 C51 111.2(3) . . ? C41 P2 C51 108.3(3) . . ? C61 P2 C51 108.2(3) . . ? C46 C41 C42 117.5(7) . . ? C46 C41 P2 124.0(6) . . ? C42 C41 P2 118.5(5) . . ? C43 C42 C41 121.5(7) . . ? C44 C43 C42 118.4(9) . . ? C45 C44 C43 121.8(9) . . ? C44 C45 C46 120.2(9) . . ? C45 C46 C41 120.7(8) . . ? C56 C51 C52 118.3(7) . . ? C56 C51 P2 122.8(5) . . ? C52 C51 P2 118.9(6) . . ? C51 C52 C53 120.7(8) . . ? C54 C53 C52 121.0(8) . . ? C53 C54 C55 119.2(8) . . ? C54 C55 C56 120.4(8) . . ? C51 C56 C55 120.5(7) . . ? C62 C61 C66 119.0(6) . . ? C62 C61 P2 120.1(5) . . ? C66 C61 P2 120.9(5) . . ? C61 C62 C63 120.2(7) . . ? C64 C63 C62 120.6(8) . . ? C63 C64 C65 119.4(8) . . ? C64 C65 C66 120.8(8) . . ? C65 C66 C61 120.0(7) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.439 _refine_diff_density_min -0.538 _refine_diff_density_rms 0.074 #===END data_11a _database_code_CSD 166148 _chemical_formula_moiety ; [2,2,2-(CO)~3~-2,3-\m-I-7-{cyclo-1,4,7-S~3~(CH~2~)~6~} -closo-2,1-MoCB~10~H~9~] ; _chemical_formula_sum 'C10 H21 B10 I Mo O3 S3' _chemical_formula_weight 616.39 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' 'S' 'S' 0.1246 0.1234 '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' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.071(2) _cell_length_b 10.9453(16) _cell_length_c 16.439(3) _cell_angle_alpha 90.00 _cell_angle_beta 115.577(14) _cell_angle_gamma 90.00 _cell_volume 2283.7(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 13 _cell_measurement_theta_max 18 _exptl_crystal_description plates _exptl_crystal_colour purple _exptl_crystal_size_max 0.59 _exptl_crystal_size_mid 0.43 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.793 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1192 _exptl_absorpt_coefficient_mu 2.210 _exptl_absorpt_correction_type 'Numerical, SHELXTL-PC vs. 5.03' _exptl_absorpt_correction_T_min 0.44417 _exptl_absorpt_correction_T_max 0.89818 _exptl_absorpt_process_details ? _exptl_special_details ; Numerical absorption correction based on 6 face measurements (-1,-1, 2); ( 1, 1,-2) 0.2950 mm ( 1, 0, 0); (-1, 0, 0) 0.0245 mm ( 0, 1, 1); ( 0,-1,-1) 0.2130 mm ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf-Nonius CAD4' _diffrn_measurement_method \w-2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 3.64 _diffrn_reflns_number 4150 _diffrn_reflns_av_R_equivalents 0.0477 _diffrn_reflns_av_sigmaI/netI 0.0381 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 24.98 _reflns_number_total 3979 _reflns_number_gt 2909 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Enraf-Nonius CAD4 (1989)' _computing_cell_refinement 'Enraf-Nonius CAD4 (1989)' _computing_data_reduction 'XCAD4 Siemens Software (Harms, 1993)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in SHELXTL-PC (Bruker, 1995)' _computing_publication_material 'SHELXL-97 (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^)+(0.0222P)^2^+9.6070P] 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 0.00026(11) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3979 _refine_ls_number_parameters 254 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0728 _refine_ls_R_factor_gt 0.0476 _refine_ls_wR_factor_ref 0.0989 _refine_ls_wR_factor_gt 0.0900 _refine_ls_goodness_of_fit_ref 1.108 _refine_ls_restrained_S_all 1.108 _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 Mo Mo -0.07513(4) 0.25985(6) 0.13101(4) 0.04304(18) Uani 1 1 d . . . C1 C 0.0975(5) 0.3325(9) 0.1750(5) 0.068(2) Uani 1 1 d . . . H1 H 0.1259 0.2839 0.1312 0.082 Uiso 1 1 calc R . . B2 B 0.0774(6) 0.2634(9) 0.2585(5) 0.054(2) Uani 1 1 d . . . B3 B -0.0214(6) 0.3464(7) 0.2789(5) 0.0400(17) Uani 1 1 d . . . B4 B -0.0663(6) 0.4609(8) 0.1972(5) 0.047(2) Uani 1 1 d . . . H4 H -0.1464 0.4988 0.1715 0.056 Uiso 1 1 calc R . . B5 B 0.0115(7) 0.4458(10) 0.1296(6) 0.065(3) Uani 1 1 d . . . H5 H -0.0199 0.4733 0.0584 0.078 Uiso 1 1 calc R . . B6 B 0.1884(7) 0.3547(11) 0.2832(6) 0.076(3) Uani 1 1 d . . . H6 H 0.2692 0.3184 0.3110 0.091 Uiso 1 1 calc R . . B7 B 0.1159(6) 0.3635(9) 0.3497(5) 0.052(2) Uani 1 1 d . . . H7 H 0.1502 0.3321 0.4202 0.063 Uiso 1 1 calc R . . B8 B 0.0300(6) 0.4933(8) 0.3098(5) 0.049(2) Uani 1 1 d . . . H8 H 0.0106 0.5504 0.3556 0.059 Uiso 1 1 calc R . . B9 B 0.0462(7) 0.5569(10) 0.2175(6) 0.066(3) Uani 1 1 d . . . H9 H 0.0343 0.6549 0.2013 0.079 Uiso 1 1 calc R . . B10 B 0.1457(8) 0.4743(12) 0.2044(7) 0.085(4) Uani 1 1 d . . . H10 H 0.1998 0.5189 0.1815 0.101 Uiso 1 1 calc R . . B11 B 0.1570(7) 0.4997(10) 0.3134(6) 0.068(3) Uani 1 1 d . . . H11 H 0.2181 0.5598 0.3614 0.081 Uiso 1 1 calc R . . I I 0.04987(4) 0.06610(5) 0.23917(4) 0.0733(2) Uani 1 1 d . . . C2 C -0.1821(6) 0.3571(7) 0.0292(5) 0.0532(18) Uani 1 1 d . . . O2 O -0.2437(5) 0.4069(5) -0.0290(4) 0.0753(17) Uani 1 1 d . . . C3 C -0.0684(6) 0.1706(9) 0.0243(5) 0.071(3) Uani 1 1 d . . . O3 O -0.0589(5) 0.1240(8) -0.0329(4) 0.113(3) Uani 1 1 d . . . C4 C -0.2050(5) 0.1881(6) 0.1294(4) 0.0450(16) Uani 1 1 d . . . O4 O -0.2794(4) 0.1493(5) 0.1297(4) 0.0649(15) Uani 1 1 d . . . S1 S -0.09809(13) 0.27373(15) 0.33759(10) 0.0405(4) Uani 1 1 d . . . C5 C -0.2194(5) 0.3599(6) 0.2915(4) 0.0477(17) Uani 1 1 d . . . H5A H -0.2044 0.4436 0.3125 0.057 Uiso 1 1 calc R . . H5B H -0.2468 0.3609 0.2263 0.057 Uiso 1 1 calc R . . C6 C -0.3043(6) 0.3088(8) 0.3170(5) 0.060(2) Uani 1 1 d . . . H6A H -0.2978 0.2205 0.3209 0.072 Uiso 1 1 calc R . . H6B H -0.3729 0.3281 0.2691 0.072 Uiso 1 1 calc R . . S2 S -0.29843(18) 0.3660(2) 0.42186(15) 0.0666(6) Uani 1 1 d . . . C7 C -0.2913(7) 0.2322(8) 0.4878(5) 0.068(2) Uani 1 1 d . . . H7A H -0.3326 0.2475 0.5211 0.081 Uiso 1 1 calc R . . H7B H -0.3247 0.1654 0.4465 0.081 Uiso 1 1 calc R . . C8 C -0.1832(7) 0.1907(7) 0.5538(5) 0.063(2) Uani 1 1 d . . . H8A H -0.1904 0.1382 0.5983 0.075 Uiso 1 1 calc R . . H8B H -0.1426 0.2616 0.5851 0.075 Uiso 1 1 calc R . . S3 S -0.11020(17) 0.10838(18) 0.50232(15) 0.0623(5) Uani 1 1 d . . . C9 C -0.0060(6) 0.2114(7) 0.5162(5) 0.058(2) Uani 1 1 d . . . H9A H 0.0263 0.2390 0.5783 0.070 Uiso 1 1 calc R . . H9B H 0.0471 0.1672 0.5053 0.070 Uiso 1 1 calc R . . C10 C -0.0387(6) 0.3222(6) 0.4554(4) 0.0492(17) Uani 1 1 d . . . H10A H 0.0224 0.3729 0.4671 0.059 Uiso 1 1 calc R . . H10B H -0.0890 0.3702 0.4677 0.059 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 Mo 0.0318(3) 0.0608(4) 0.0333(3) -0.0091(3) 0.0109(2) 0.0021(3) C1 0.040(4) 0.118(7) 0.054(4) -0.032(5) 0.028(4) -0.019(5) B2 0.031(4) 0.066(6) 0.053(5) -0.017(4) 0.006(3) 0.005(4) B3 0.033(4) 0.048(5) 0.039(4) -0.003(3) 0.016(3) -0.002(3) B4 0.049(5) 0.057(5) 0.039(4) -0.004(4) 0.024(4) -0.011(4) B5 0.052(5) 0.104(8) 0.047(5) -0.008(5) 0.028(4) -0.027(6) B6 0.035(5) 0.133(10) 0.060(6) -0.043(6) 0.020(4) -0.027(6) B7 0.036(4) 0.076(6) 0.042(4) -0.017(4) 0.014(3) -0.010(4) B8 0.049(5) 0.057(5) 0.045(4) -0.007(4) 0.023(4) -0.009(4) B9 0.067(6) 0.073(6) 0.066(6) -0.012(5) 0.037(5) -0.032(5) B10 0.065(6) 0.133(10) 0.070(6) -0.025(7) 0.042(5) -0.049(7) B11 0.057(6) 0.098(8) 0.053(5) -0.022(5) 0.028(5) -0.027(6) I 0.0518(3) 0.0721(4) 0.0680(4) -0.0180(3) -0.0005(2) 0.0266(3) C2 0.052(4) 0.062(5) 0.041(4) -0.002(4) 0.016(3) 0.002(4) O2 0.081(4) 0.075(4) 0.053(3) 0.009(3) 0.013(3) 0.010(3) C3 0.040(4) 0.115(7) 0.045(4) -0.020(5) 0.006(3) 0.027(5) O3 0.090(5) 0.175(7) 0.063(4) -0.043(5) 0.023(3) 0.045(5) C4 0.039(4) 0.044(4) 0.041(4) -0.001(3) 0.006(3) 0.006(3) O4 0.045(3) 0.067(4) 0.079(4) 0.001(3) 0.022(3) -0.010(3) S1 0.0448(9) 0.0415(9) 0.0364(8) -0.0018(7) 0.0187(7) -0.0028(8) C5 0.052(4) 0.052(4) 0.046(4) 0.000(3) 0.028(3) 0.008(4) C6 0.053(4) 0.072(5) 0.062(5) -0.003(4) 0.030(4) -0.005(4) S2 0.0915(16) 0.0595(13) 0.0749(13) 0.0125(11) 0.0603(13) 0.0203(12) C7 0.085(6) 0.070(5) 0.075(5) 0.012(5) 0.060(5) 0.005(5) C8 0.093(6) 0.051(5) 0.060(5) 0.006(4) 0.047(5) -0.005(4) S3 0.0769(14) 0.0496(11) 0.0729(13) 0.0078(10) 0.0441(11) -0.0004(10) C9 0.058(5) 0.066(5) 0.045(4) 0.010(4) 0.017(3) -0.003(4) C10 0.061(5) 0.049(4) 0.043(4) -0.004(3) 0.028(3) -0.008(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo C4 1.978(8) . y Mo C2 2.006(8) . y Mo C3 2.045(8) . y Mo B2 2.262(7) . y Mo C1 2.354(7) . y Mo B5 2.377(10) . y Mo B3 2.407(7) . y Mo B4 2.433(8) . y Mo I 2.8375(9) . y C1 B5 1.666(13) . ? C1 B10 1.678(14) . ? C1 B2 1.694(12) . ? C1 B6 1.701(11) . ? B2 B7 1.744(11) . ? B2 B6 1.747(12) . ? B2 B3 1.809(11) . ? B2 I 2.193(9) . y B3 B4 1.743(11) . ? B3 B8 1.746(11) . ? B3 B7 1.783(10) . ? B3 S1 1.905(7) . ? B4 B8 1.796(11) . ? B4 B9 1.807(11) . ? B4 B5 1.873(11) . ? B5 B10 1.780(13) . ? B5 B9 1.787(13) . ? B6 B10 1.755(17) . ? B6 B11 1.774(15) . ? B6 B7 1.791(12) . ? B7 B11 1.792(14) . ? B7 B8 1.796(12) . ? B8 B11 1.764(12) . ? B8 B9 1.772(12) . ? B9 B10 1.756(15) . ? B9 B11 1.786(14) . ? B10 B11 1.750(13) . ? C2 O2 1.117(8) . y C3 O3 1.127(8) . y C4 O4 1.132(8) . y S1 C5 1.806(7) . y S1 C10 1.826(6) . y C5 C6 1.532(9) . ? C6 S2 1.802(7) . y S2 C7 1.798(8) . y C7 C8 1.507(11) . ? C8 S3 1.825(8) . y S3 C9 1.785(7) . y C9 C10 1.511(9) . ? 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 C4 Mo C2 81.0(3) . . y C4 Mo C3 100.6(3) . . y C2 Mo C3 80.4(3) . . y C4 Mo B2 121.4(3) . . y C2 Mo B2 146.5(3) . . y C3 Mo B2 115.2(3) . . y C4 Mo C1 164.3(3) . . y C2 Mo C1 112.3(3) . . y C3 Mo C1 90.1(3) . . y B2 Mo C1 43.0(3) . . ? C4 Mo B5 144.5(3) . . y C2 Mo B5 75.0(3) . . y C3 Mo B5 100.8(4) . . y B2 Mo B5 73.1(3) . . ? C1 Mo B5 41.2(3) . . y C4 Mo B3 93.2(3) . . y C2 Mo B3 115.4(3) . . y C3 Mo B3 160.7(3) . . y B2 Mo B3 45.5(3) . . ? C1 Mo B3 74.0(2) . . ? B5 Mo B3 74.6(3) . . ? C4 Mo B4 103.5(3) . . y C2 Mo B4 76.6(3) . . y C3 Mo B4 143.4(3) . . y B2 Mo B4 74.1(3) . . ? C1 Mo B4 73.1(3) . . ? B5 Mo B4 45.8(3) . . ? B3 Mo B4 42.2(3) . . ? C4 Mo I 91.76(19) . . y C2 Mo I 163.4(2) . . y C3 Mo I 86.2(2) . . y B2 Mo I 49.4(2) . . y C1 Mo I 77.4(2) . . y B5 Mo I 117.6(2) . . y B3 Mo I 79.74(18) . . y B4 Mo I 119.83(19) . . y B5 C1 B10 64.3(6) . . ? B5 C1 B2 110.6(6) . . ? B10 C1 B2 111.6(6) . . ? B5 C1 B6 115.8(7) . . ? B10 C1 B6 62.6(6) . . ? B2 C1 B6 62.0(5) . . ? B5 C1 Mo 70.1(4) . . ? B10 C1 Mo 129.5(6) . . ? B2 C1 Mo 65.6(3) . . ? B6 C1 Mo 125.4(5) . . ? C1 B2 B7 108.5(7) . . ? C1 B2 B6 59.2(5) . . ? B7 B2 B6 61.7(5) . . ? C1 B2 B3 109.6(6) . . ? B7 B2 B3 60.2(4) . . ? B6 B2 B3 110.5(6) . . ? C1 B2 I 113.8(5) . . y B7 B2 I 135.5(6) . . y B6 B2 I 132.9(6) . . y B3 B2 I 114.8(5) . . y C1 B2 Mo 71.4(4) . . ? B7 B2 Mo 128.7(5) . . ? B6 B2 Mo 128.4(6) . . ? B3 B2 Mo 71.5(3) . . ? I B2 Mo 79.1(3) . . y B4 B3 B8 61.9(4) . . ? B4 B3 B7 111.0(6) . . ? B8 B3 B7 61.2(5) . . ? B4 B3 B2 105.6(5) . . ? B8 B3 B2 105.2(5) . . ? B7 B3 B2 58.1(4) . . ? B4 B3 S1 126.5(5) . . y B8 B3 S1 119.4(5) . . y B7 B3 S1 113.8(5) . . y B2 B3 S1 122.2(5) . . y B4 B3 Mo 69.7(3) . . ? B8 B3 Mo 124.5(5) . . ? B7 B3 Mo 118.7(4) . . ? B2 B3 Mo 63.0(3) . . ? S1 B3 Mo 110.3(3) . . y B3 B4 B8 59.1(4) . . ? B3 B4 B9 106.2(6) . . ? B8 B4 B9 58.9(5) . . ? B3 B4 B5 106.5(6) . . ? B8 B4 B5 104.8(6) . . ? B9 B4 B5 58.1(5) . . ? B3 B4 Mo 68.1(4) . . ? B8 B4 Mo 120.7(5) . . ? B9 B4 Mo 118.7(5) . . ? B5 B4 Mo 65.5(4) . . ? C1 B5 B10 58.2(6) . . ? C1 B5 B9 104.6(6) . . ? B10 B5 B9 59.0(6) . . ? C1 B5 B4 107.3(6) . . ? B10 B5 B4 107.0(6) . . ? B9 B5 B4 59.1(5) . . ? C1 B5 Mo 68.6(4) . . ? B10 B5 Mo 122.6(7) . . ? B9 B5 Mo 122.5(5) . . ? B4 B5 Mo 68.7(4) . . ? C1 B6 B2 58.8(5) . . ? C1 B6 B10 58.1(6) . . ? B2 B6 B10 105.5(6) . . ? C1 B6 B11 104.7(8) . . ? B2 B6 B11 105.7(6) . . ? B10 B6 B11 59.5(6) . . ? C1 B6 B7 106.1(6) . . ? B2 B6 B7 59.0(5) . . ? B10 B6 B7 107.8(8) . . ? B11 B6 B7 60.4(5) . . ? B2 B7 B3 61.7(4) . . ? B2 B7 B6 59.2(5) . . ? B3 B7 B6 109.8(6) . . ? B2 B7 B11 105.1(6) . . ? B3 B7 B11 106.5(6) . . ? B6 B7 B11 59.4(6) . . ? B2 B7 B8 105.8(6) . . ? B3 B7 B8 58.4(4) . . ? B6 B7 B8 106.9(7) . . ? B11 B7 B8 58.9(5) . . ? B3 B8 B11 109.4(6) . . ? B3 B8 B9 107.6(6) . . ? B11 B8 B9 60.7(5) . . ? B3 B8 B4 59.0(4) . . ? B11 B8 B4 110.2(6) . . ? B9 B8 B4 60.9(4) . . ? B3 B8 B7 60.4(4) . . ? B11 B8 B7 60.4(5) . . ? B9 B8 B7 108.0(6) . . ? B4 B8 B7 108.0(6) . . ? B10 B9 B8 107.8(7) . . ? B10 B9 B11 59.2(6) . . ? B8 B9 B11 59.5(5) . . ? B10 B9 B5 60.3(5) . . ? B8 B9 B5 109.5(6) . . ? B11 B9 B5 107.7(7) . . ? B10 B9 B4 111.0(7) . . ? B8 B9 B4 60.2(4) . . ? B11 B9 B4 108.7(7) . . ? B5 B9 B4 62.8(5) . . ? C1 B10 B11 106.8(7) . . ? C1 B10 B6 59.3(6) . . ? B11 B10 B6 60.8(6) . . ? C1 B10 B9 105.5(6) . . ? B11 B10 B9 61.2(6) . . ? B6 B10 B9 109.4(7) . . ? C1 B10 B5 57.5(5) . . ? B11 B10 B5 109.6(7) . . ? B6 B10 B5 107.6(7) . . ? B9 B10 B5 60.7(6) . . ? B10 B11 B8 108.4(6) . . ? B10 B11 B6 59.7(6) . . ? B8 B11 B6 109.0(7) . . ? B10 B11 B9 59.5(6) . . ? B8 B11 B9 59.9(5) . . ? B6 B11 B9 107.2(7) . . ? B10 B11 B7 108.0(7) . . ? B8 B11 B7 60.7(5) . . ? B6 B11 B7 60.3(6) . . ? B9 B11 B7 107.5(6) . . ? B2 I Mo 51.5(2) . . y O2 C2 Mo 177.2(7) . . y O3 C3 Mo 176.0(8) . . y O4 C4 Mo 178.4(6) . . y C5 S1 C10 102.2(3) . . ? C5 S1 B3 102.1(3) . . y C10 S1 B3 108.4(3) . . y C6 C5 S1 113.7(5) . . ? C5 C6 S2 114.6(5) . . ? C7 S2 C6 105.1(4) . . ? C8 C7 S2 117.2(6) . . ? C7 C8 S3 114.2(5) . . ? C9 S3 C8 103.0(4) . . ? C10 C9 S3 115.1(5) . . ? C9 C10 S1 109.7(5) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.401 _refine_diff_density_min -1.330 _refine_diff_density_rms 0.111 #===END data_14 _database_code_CSD 166149 _chemical_formula_moiety ; [2,2,2-(CO)~3~-2-I-3,11-{cyclo-1,4-S~2~(CH~2~)~4~}~2~ -closo-2,1-MoCB~10~H~9~] ; _chemical_formula_sum 'C13 H27 B10 Cl2 I Mo O3 S4' _chemical_formula_weight 761.43 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'S' 'S' 0.1246 0.1234 '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' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 8.8257(9) _cell_length_b 10.6900(10) _cell_length_c 30.297(4) _cell_angle_alpha 90.00 _cell_angle_beta 95.612(10) _cell_angle_gamma 90.00 _cell_volume 2844.7(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 15 _cell_measurement_theta_max 20 _exptl_crystal_description needles _exptl_crystal_colour brick-red _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.778 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1488 _exptl_absorpt_coefficient_mu 2.045 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.7290 _exptl_absorpt_correction_T_max 0.8056 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Enraf-Nonius CAD4' _diffrn_measurement_method \w-2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 4.03 _diffrn_reflns_number 5372 _diffrn_reflns_av_R_equivalents 0.0345 _diffrn_reflns_av_sigmaI/netI 0.0691 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 25.04 _reflns_number_total 5021 _reflns_number_gt 3306 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Enraf-Nonius CAD4 (1989)' _computing_cell_refinement 'Enraf-Nonius CAD4 (1989)' _computing_data_reduction 'XCAD4 Siemens Software (Harms, 1993)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in SHELXTL-PC (Bruker, 1995)' _computing_publication_material 'SHELXL-97 (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 w=1/[\s^2^(Fo^2^)+(0.0237P)^2^+6.8204P] 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 5021 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1001 _refine_ls_R_factor_gt 0.0526 _refine_ls_wR_factor_ref 0.0980 _refine_ls_wR_factor_gt 0.0857 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.089 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo Mo 0.09173(7) 0.00141(5) 0.125992(19) 0.03003(15) Uani 1 d . . . C1 C -0.1774(7) 0.0019(6) 0.1010(2) 0.0354(16) Uani 1 d . . . H1 H -0.2060 0.1017 0.0971 0.042 Uiso 1 calc R . . B2 B -0.1452(9) -0.0595(7) 0.1520(3) 0.0313(18) Uani 1 d . . . B3 B -0.0181(9) -0.1857(7) 0.1501(3) 0.0322(19) Uani 1 d . . . H3 H 0.0586 -0.2178 0.1787 0.039 Uiso 1 calc R . . B4 B 0.0227(9) -0.1929(7) 0.0927(3) 0.0318(19) Uani 1 d . . . B5 B -0.0718(9) -0.0676(7) 0.0634(3) 0.0337(19) Uani 1 d . . . H5 H -0.0288 -0.0200 0.0349 0.040 Uiso 1 calc R . . B6 B -0.3163(10) -0.0890(8) 0.1187(3) 0.037(2) Uani 1 d . . . H6 H -0.4270 -0.0535 0.1270 0.044 Uiso 1 calc R . . B7 B -0.2182(9) -0.2122(7) 0.1487(3) 0.037(2) Uani 1 d . . . H7 H -0.2659 -0.2582 0.1767 0.044 Uiso 1 calc R . . B8 B -0.1141(10) -0.2968(8) 0.1120(3) 0.042(2) Uani 1 d . . . H8 H -0.0927 -0.3978 0.1157 0.051 Uiso 1 calc R . . B9 B -0.1478(9) -0.2222(7) 0.0589(3) 0.035(2) Uani 1 d . . . H9 H -0.1488 -0.2752 0.0277 0.043 Uiso 1 calc R . . B10 B -0.2722(10) -0.0966(8) 0.0637(3) 0.040(2) Uani 1 d . . . H10 H -0.3541 -0.0667 0.0360 0.048 Uiso 1 calc R . . B11 B -0.2975(9) -0.2374(8) 0.0936(3) 0.040(2) Uani 1 d . . . H11 H -0.3951 -0.3002 0.0855 0.048 Uiso 1 calc R . . I I 0.04632(7) 0.26141(4) 0.105221(19) 0.05493(18) Uani 1 d . . . C2 C 0.1583(8) 0.0925(7) 0.1826(3) 0.0428(19) Uani 1 d . . . O2 O 0.2017(7) 0.1381(6) 0.21507(19) 0.0691(19) Uani 1 d . . . C3 C 0.2679(8) -0.0927(7) 0.1545(2) 0.0380(18) Uani 1 d . . . O3 O 0.3637(6) -0.1486(5) 0.17317(19) 0.0594(16) Uani 1 d . . . C4 C 0.2504(9) 0.0472(7) 0.0844(2) 0.0414(19) Uani 1 d . . . O4 O 0.3383(6) 0.0725(5) 0.06229(18) 0.0594(16) Uani 1 d . . . S1 S 0.2013(2) -0.27057(16) 0.07227(6) 0.0342(4) Uani 1 d . . . C5 C 0.1595(8) -0.4340(6) 0.0626(2) 0.0404(18) Uani 1 d . . . H5A H 0.1539 -0.4763 0.0907 0.048 Uiso 1 calc R . . H5B H 0.0616 -0.4425 0.0453 0.048 Uiso 1 calc R . . C6 C 0.2832(9) -0.4949(7) 0.0377(2) 0.0477(19) Uani 1 d . . . H6A H 0.2690 -0.5848 0.0377 0.057 Uiso 1 calc R . . H6B H 0.3818 -0.4771 0.0535 0.057 Uiso 1 calc R . . S2 S 0.2839(3) -0.4424(2) -0.01864(7) 0.0529(6) Uani 1 d . . . C7 C 0.3247(9) -0.2802(7) -0.0074(2) 0.051(2) Uani 1 d . . . H7A H 0.4205 -0.2737 0.0112 0.061 Uiso 1 calc R . . H7B H 0.3365 -0.2374 -0.0351 0.061 Uiso 1 calc R . . C8 C 0.2007(9) -0.2154(6) 0.0157(2) 0.045(2) Uani 1 d . . . H8A H 0.1023 -0.2322 -0.0004 0.054 Uiso 1 calc R . . H8B H 0.2173 -0.1257 0.0158 0.054 Uiso 1 calc R . . S3 S -0.1687(2) 0.04025(16) 0.20351(6) 0.0362(4) Uani 1 d . . . C9 C -0.0814(8) -0.0612(7) 0.2469(2) 0.0401(18) Uani 1 d . . . H9A H -0.1307 -0.1424 0.2449 0.048 Uiso 1 calc R . . H9B H 0.0253 -0.0730 0.2428 0.048 Uiso 1 calc R . . C10 C -0.0957(9) -0.0051(8) 0.2920(2) 0.053(2) Uani 1 d . . . H10A H -0.0548 0.0792 0.2925 0.064 Uiso 1 calc R . . H10B H -0.0338 -0.0536 0.3140 0.064 Uiso 1 calc R . . S4 S -0.2857(3) 0.0010(3) 0.30735(7) 0.0707(7) Uani 1 d . . . C11 C -0.3726(10) 0.0944(8) 0.2627(2) 0.060(2) Uani 1 d . . . H11A H -0.4787 0.1077 0.2672 0.072 Uiso 1 calc R . . H11B H -0.3232 0.1755 0.2634 0.072 Uiso 1 calc R . . C12 C -0.3639(8) 0.0363(7) 0.2174(2) 0.047(2) Uani 1 d . . . H12A H -0.4287 0.0823 0.1953 0.056 Uiso 1 calc R . . H12B H -0.3994 -0.0495 0.2176 0.056 Uiso 1 calc R . . C100 C 0.6458(11) 0.4149(9) 0.1424(3) 0.079(3) Uani 1 d . . . H10C H 0.5892 0.4916 0.1360 0.095 Uiso 1 calc R . . H10D H 0.7380 0.4192 0.1274 0.095 Uiso 1 calc R . . Cl2 Cl 0.5381(3) 0.2901(3) 0.12186(8) 0.0879(8) Uani 1 d . . . Cl1 Cl 0.6948(3) 0.4042(3) 0.19942(10) 0.0996(10) Uani 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 Mo 0.0361(3) 0.0278(3) 0.0260(3) 0.0011(3) 0.0024(2) -0.0065(3) C1 0.042(4) 0.036(4) 0.027(4) 0.003(3) 0.000(3) 0.003(4) B2 0.034(5) 0.031(4) 0.029(4) 0.000(3) 0.005(4) 0.002(4) B3 0.033(5) 0.031(4) 0.032(5) 0.000(4) -0.003(4) -0.004(4) B4 0.041(5) 0.026(4) 0.028(4) -0.002(3) 0.002(4) -0.002(4) B5 0.042(5) 0.035(4) 0.024(4) 0.004(4) -0.001(4) -0.006(4) B6 0.031(5) 0.046(5) 0.035(5) 0.000(4) 0.006(4) -0.004(4) B7 0.033(5) 0.040(5) 0.039(5) 0.004(4) 0.011(4) -0.005(4) B8 0.048(6) 0.036(5) 0.043(5) -0.009(4) 0.003(4) -0.013(4) B9 0.037(5) 0.045(5) 0.022(4) -0.005(4) -0.008(4) -0.008(4) B10 0.044(6) 0.049(5) 0.028(5) -0.003(4) 0.001(4) -0.004(4) B11 0.031(5) 0.046(5) 0.041(5) -0.011(4) 0.003(4) -0.009(4) I 0.0711(4) 0.0302(3) 0.0632(4) 0.0034(3) 0.0048(3) -0.0044(3) C2 0.039(5) 0.050(5) 0.041(5) 0.002(4) 0.009(4) -0.019(4) O2 0.083(5) 0.079(4) 0.043(4) -0.019(3) -0.008(3) -0.027(4) C3 0.031(4) 0.045(4) 0.038(4) 0.003(4) 0.002(4) -0.013(4) O3 0.036(3) 0.068(4) 0.071(4) 0.023(3) -0.013(3) -0.004(3) C4 0.054(5) 0.035(4) 0.033(4) 0.000(3) -0.008(4) -0.002(4) O4 0.052(4) 0.074(4) 0.055(4) 0.016(3) 0.021(3) -0.023(3) S1 0.0399(11) 0.0345(10) 0.0281(9) -0.0015(8) 0.0034(8) -0.0022(8) C5 0.052(5) 0.026(4) 0.044(5) -0.002(3) 0.008(4) -0.002(4) C6 0.060(5) 0.036(4) 0.048(5) -0.003(4) 0.007(4) 0.012(4) S2 0.0653(15) 0.0545(12) 0.0400(12) -0.0083(10) 0.0100(11) 0.0105(11) C7 0.063(6) 0.055(5) 0.036(4) 0.005(4) 0.012(4) -0.007(4) C8 0.067(6) 0.032(4) 0.035(4) 0.003(3) 0.009(4) 0.000(4) S3 0.0427(11) 0.0382(10) 0.0283(10) -0.0007(8) 0.0067(8) -0.0036(8) C9 0.047(5) 0.043(4) 0.030(4) 0.000(3) 0.002(4) -0.003(4) C10 0.073(6) 0.061(5) 0.025(4) 0.003(4) 0.004(4) 0.001(5) S4 0.0802(17) 0.0960(18) 0.0392(12) 0.0044(13) 0.0219(12) 0.0027(16) C11 0.061(6) 0.078(6) 0.044(5) -0.010(5) 0.019(4) 0.003(5) C12 0.040(5) 0.056(5) 0.046(5) 0.000(4) 0.012(4) 0.000(4) C100 0.082(7) 0.075(7) 0.081(7) 0.001(6) 0.015(6) -0.013(6) Cl2 0.093(2) 0.099(2) 0.0720(17) -0.0106(15) 0.0079(15) -0.0243(16) Cl1 0.076(2) 0.126(2) 0.092(2) -0.0173(19) -0.0169(16) -0.0023(18) _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 Mo C3 1.978(8) . y Mo C2 2.008(8) . y Mo C4 2.033(9) . y Mo B4 2.363(7) . y Mo B3 2.370(8) . y Mo B5 2.384(8) . y Mo B2 2.396(8) . y Mo C1 2.421(6) . y Mo I 2.8693(8) . y C1 B2 1.678(9) . ? C1 B6 1.693(10) . ? C1 B10 1.704(10) . ? C1 B5 1.710(10) . ? B2 B7 1.754(11) . ? B2 B3 1.759(11) . ? B2 B6 1.761(11) . ? B2 S3 1.917(8) . y B3 B7 1.784(11) . ? B3 B8 1.809(11) . ? B3 B4 1.813(11) . ? B4 B9 1.763(11) . ? B4 B5 1.770(11) . ? B4 B8 1.780(11) . ? B4 S1 1.936(8) . y B5 B9 1.784(11) . ? B5 B10 1.797(12) . ? B6 B10 1.750(11) . ? B6 B11 1.774(12) . ? B6 B7 1.776(11) . ? B7 B8 1.760(12) . ? B7 B11 1.767(11) . ? B8 B11 1.777(12) . ? B8 B9 1.793(11) . ? B9 B10 1.750(12) . ? B9 B11 1.774(11) . ? B10 B11 1.782(12) . ? C2 O2 1.132(8) . y C3 O3 1.139(8) . y C4 O4 1.106(8) . y S1 C5 1.804(7) . ? S1 C8 1.811(7) . ? C5 C6 1.531(9) . ? C6 S2 1.796(7) . ? S2 C7 1.798(8) . ? C7 C8 1.522(10) . ? S3 C12 1.813(7) . ? S3 C9 1.816(7) . ? C9 C10 1.508(9) . ? C10 S4 1.785(8) . ? S4 C11 1.792(8) . ? C11 C12 1.515(10) . ? C100 Cl2 1.719(9) . ? C100 Cl1 1.744(9) . ? 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 Mo C2 73.9(3) . . y C3 Mo C4 80.4(3) . . y C2 Mo C4 104.5(3) . . y C3 Mo B4 84.1(3) . . y C2 Mo B4 146.3(3) . . y C4 Mo B4 96.4(3) . . y C3 Mo B3 76.3(3) . . y C2 Mo B3 103.9(3) . . y C4 Mo B3 136.2(3) . . y B4 Mo B3 45.0(3) . . ? C3 Mo B5 125.3(3) . . y C2 Mo B5 158.8(3) . . y C4 Mo B5 88.9(3) . . y B4 Mo B5 43.8(3) . . ? B3 Mo B5 75.5(3) . . ? C3 Mo B2 113.1(3) . . y C2 Mo B2 92.5(3) . . y C4 Mo B2 161.0(3) . . y B4 Mo B2 72.8(3) . . ? B3 Mo B2 43.3(3) . . ? B5 Mo B2 72.4(3) . . ? C3 Mo C1 147.4(3) . . y C2 Mo C1 117.5(3) . . y C4 Mo C1 121.3(3) . . y B4 Mo C1 70.4(3) . . ? B3 Mo C1 71.3(2) . . ? B5 Mo C1 41.7(2) . . ? B2 Mo C1 40.8(2) . . ? C3 Mo I 132.5(2) . . y C2 Mo I 75.0(2) . . y C4 Mo I 73.8(2) . . y B4 Mo I 137.17(19) . . y B3 Mo I 146.4(2) . . y B5 Mo I 93.70(19) . . y B2 Mo I 103.16(18) . . y C1 Mo I 79.48(16) . . y B2 C1 B6 63.0(4) . . ? B2 C1 B10 113.4(6) . . ? B6 C1 B10 62.0(4) . . ? B2 C1 B5 112.9(5) . . ? B6 C1 B5 114.8(5) . . ? B10 C1 B5 63.5(4) . . ? B2 C1 Mo 68.8(3) . . ? B6 C1 Mo 128.2(4) . . ? B10 C1 Mo 127.5(5) . . ? B5 C1 Mo 68.0(3) . . ? C1 B2 B7 106.4(6) . . ? C1 B2 B3 108.7(5) . . ? B7 B2 B3 61.1(4) . . ? C1 B2 B6 58.9(4) . . ? B7 B2 B6 60.7(5) . . ? B3 B2 B6 110.9(6) . . ? C1 B2 S3 120.7(5) . . y B7 B2 S3 119.7(5) . . y B3 B2 S3 125.0(5) . . y B6 B2 S3 114.3(5) . . y C1 B2 Mo 70.4(3) . . ? B7 B2 Mo 124.1(5) . . ? B3 B2 Mo 67.5(4) . . ? B6 B2 Mo 125.9(5) . . ? S3 B2 Mo 106.5(3) . . y B2 B3 B7 59.3(4) . . ? B2 B3 B8 105.3(6) . . ? B7 B3 B8 58.7(4) . . ? B2 B3 B4 104.5(5) . . ? B7 B3 B4 105.0(5) . . ? B8 B3 B4 58.9(4) . . ? B2 B3 Mo 69.2(4) . . ? B7 B3 Mo 124.1(5) . . ? B8 B3 Mo 122.5(5) . . ? B4 B3 Mo 67.3(3) . . ? B9 B4 B5 60.7(4) . . ? B9 B4 B8 60.8(5) . . ? B5 B4 B8 109.6(6) . . ? B9 B4 B3 109.1(6) . . ? B5 B4 B3 108.7(5) . . ? B8 B4 B3 60.4(4) . . ? B9 B4 S1 114.4(5) . . y B5 B4 S1 121.5(5) . . y B8 B4 S1 115.9(5) . . y B3 B4 S1 124.7(5) . . y B9 B4 Mo 125.0(5) . . ? B5 B4 Mo 68.7(3) . . ? B8 B4 Mo 124.3(5) . . ? B3 B4 Mo 67.7(3) . . ? S1 B4 Mo 109.2(4) . . y C1 B5 B4 104.8(5) . . ? C1 B5 B9 103.2(5) . . ? B4 B5 B9 59.5(4) . . ? C1 B5 B10 58.1(4) . . ? B4 B5 B10 106.4(6) . . ? B9 B5 B10 58.5(4) . . ? C1 B5 Mo 70.3(3) . . ? B4 B5 Mo 67.5(3) . . ? B9 B5 Mo 122.8(4) . . ? B10 B5 Mo 124.7(5) . . ? C1 B6 B10 59.3(4) . . ? C1 B6 B2 58.1(4) . . ? B10 B6 B2 107.2(6) . . ? C1 B6 B11 106.1(6) . . ? B10 B6 B11 60.7(5) . . ? B2 B6 B11 107.2(6) . . ? C1 B6 B7 104.8(6) . . ? B10 B6 B7 108.1(6) . . ? B2 B6 B7 59.4(4) . . ? B11 B6 B7 59.7(5) . . ? B2 B7 B8 107.6(6) . . ? B2 B7 B11 107.8(6) . . ? B8 B7 B11 60.5(5) . . ? B2 B7 B6 59.8(4) . . ? B8 B7 B6 108.4(6) . . ? B11 B7 B6 60.1(5) . . ? B2 B7 B3 59.6(4) . . ? B8 B7 B3 61.4(5) . . ? B11 B7 B3 110.3(6) . . ? B6 B7 B3 109.1(6) . . ? B7 B8 B11 59.9(5) . . ? B7 B8 B4 107.4(6) . . ? B11 B8 B4 107.5(6) . . ? B7 B8 B9 106.7(6) . . ? B11 B8 B9 59.6(5) . . ? B4 B8 B9 59.1(4) . . ? B7 B8 B3 60.0(4) . . ? B11 B8 B3 108.8(6) . . ? B4 B8 B3 60.7(4) . . ? B9 B8 B3 107.9(6) . . ? B10 B9 B4 108.8(6) . . ? B10 B9 B11 60.8(5) . . ? B4 B9 B11 108.4(5) . . ? B10 B9 B5 61.1(5) . . ? B4 B9 B5 59.9(4) . . ? B11 B9 B5 109.6(6) . . ? B10 B9 B8 108.5(6) . . ? B4 B9 B8 60.1(4) . . ? B11 B9 B8 59.8(5) . . ? B5 B9 B8 108.3(5) . . ? C1 B10 B9 104.9(6) . . ? C1 B10 B6 58.7(4) . . ? B9 B10 B6 108.3(6) . . ? C1 B10 B11 105.2(5) . . ? B9 B10 B11 60.3(5) . . ? B6 B10 B11 60.3(5) . . ? C1 B10 B5 58.4(4) . . ? B9 B10 B5 60.4(5) . . ? B6 B10 B5 107.9(6) . . ? B11 B10 B5 108.7(6) . . ? B7 B11 B6 60.2(4) . . ? B7 B11 B9 107.2(6) . . ? B6 B11 B9 106.2(6) . . ? B7 B11 B8 59.5(5) . . ? B6 B11 B8 107.7(6) . . ? B9 B11 B8 60.7(5) . . ? B7 B11 B10 107.1(6) . . ? B6 B11 B10 59.0(5) . . ? B9 B11 B10 58.9(5) . . ? B8 B11 B10 107.8(6) . . ? O2 C2 Mo 175.9(7) . . y O3 C3 Mo 175.4(6) . . y O4 C4 Mo 178.9(7) . . y C5 S1 C8 100.3(3) . . ? C5 S1 B4 107.9(3) . . y C8 S1 B4 103.6(3) . . y C6 C5 S1 110.3(5) . . ? C5 C6 S2 113.8(5) . . ? C6 S2 C7 98.0(3) . . ? C8 C7 S2 112.7(5) . . ? C7 C8 S1 110.6(5) . . ? C12 S3 C9 99.4(3) . . ? C12 S3 B2 110.9(4) . . y C9 S3 B2 100.6(3) . . y C10 C9 S3 110.5(5) . . ? C9 C10 S4 114.5(5) . . ? C10 S4 C11 99.6(4) . . ? C12 C11 S4 113.5(6) . . ? C11 C12 S3 109.6(5) . . ? Cl2 C100 Cl1 112.5(5) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.270 _refine_diff_density_min -0.589 _refine_diff_density_rms 0.116 #===END