# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2014 data_1 # start Validation Reply Form _vrf_PLAT605_I ; PROBLEM: Structure Contains Solvent Accessible VOIDS of . 291 A**3 RESPONSE: The unit cell contains a number of solvent acetone molecules, which were not located but are included in the final formula as 3 molecules per formula unit. See PLATON/SQUEEZE details below. ; _vrf_CHEMW03_I ; WARNING: The ratio of given/expected molecular weight as calculated from the _atom_site* data lies outside the range 0.95 <> 1.05 RESPONSE: See response to PLAT605_ALERT_4_G ; _vrf_PLAT041_I ; WARNING: Calc. and Reported SumFormula Strings Differ ? Check RESPONSE: See response to PLAT605_ALERT_4_G ; # end Validation Reply Form _publ_requested_journal 'Dalton Trans.' _publ_contact_author_name 'Dr. Andrew J. Sutherland' _publ_contact_author_address ;Chemical Engineering and Applied Chemistry, Aston University, Aston Triangle, Birmingham, B4 7ET, UK ; _publ_contact_author_email a.j.sutherland@aston.ac.uk _publ_contact_author_phone 44(0)1212043425 _publ_contact_author_fax 44(0)1212043696 loop_ _publ_author_name _publ_author_address 'Efremova, O. A.' ;Chemical Engineering and Applied Chemistry, Aston University, Aston Triangle, Birmingham, B4 7ET, UK ; 'Shestopalov, M. A.' ;Nikolaev Institute of Inorganic Chemistry, SB Russian Academy of Sciences, 630090, Akad. Lavrentiev prospekt 3, Novosibirsk, Russian Federation ; 'Chirtsova, N. A.' ;Novosibirsk State University, 630090, Pirogova st. 2, Novosibisrk, Russian Federation ; 'Smolentsev, A. I.' ;Nikolaev Institute of Inorganic Chemistry, SB Russian Academy of Sciences, 630090, Akad. Lavrentiev prospekt 3, Novosibirsk, Russian Federation ; 'Mironov, Y. V.' ;Nikolaev Institute of Inorganic Chemistry, SB Russian Academy of Sciences, 630090, Akad. Lavrentiev prospekt 3, Novosibirsk, Russian Federation ; 'Kitamura, N.' ;Department of Chemistry, Faculty of Science, Hokkaido University, 060-0810 Sapporo, Japan ; 'Brylev, K. A.' ;Nikolaev Institute of Inorganic Chemistry, SB Russian Academy of Sciences, 630090, Akad. Lavrentiev prospekt 3, Novosibirsk, Russian Federation Novosibirsk State University, 630090, Pirogova st. 2, Novosibisrk, Russian Federation ; 'Sutherland, A. J.' ;Chemical Engineering and Applied Chemistry, Aston University, Aston Triangle, Birmingham, B4 7ET, UK ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.000 291 139 ' ' 2 0.500 0.500 0.500 291 138 ' ' _platon_squeeze_details ; The solvent acetone molecules appeared to be highly disordered and it was difficult to model their positions reliably. Therefore, the structure was treated via PLATON/SQUEEZE (van der Sluis & Spek, 1990; Spek, 2003) procedure to remove the contribution of the electron density in the solvent regions from the intensity data, and the solvent-free model was employed from the final refinement. The total potential solvent accessible void volume was estimated to be 582 Ang**3 and the electron count per unit cell was 277, which were assigned to 6 acetone molecules per unit cell or 3 acetone molecules per formula unit. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'I8 Mo6 N6 O18, 2(C16 H36 N), 3(C3 H6 O)' _chemical_formula_sum 'C41 H90 I8 Mo6 N8 O21' _chemical_formula_weight 2622.05 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' 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 14.5949(4) _cell_length_b 11.4521(3) _cell_length_c 22.3086(5) _cell_angle_alpha 90.00 _cell_angle_beta 95.8350(10) _cell_angle_gamma 90.00 _cell_volume 3709.39(16) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4129 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 26.25 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.348 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2472 _exptl_absorpt_coefficient_mu 4.378 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3534 _exptl_absorpt_correction_T_max 0.8108 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Nonius X8Apex CCD area-detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 25 _diffrn_standards_number 0 _diffrn_reflns_number 18245 _diffrn_reflns_av_R_equivalents 0.0339 _diffrn_reflns_av_sigmaI/netI 0.0594 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 27.50 _reflns_number_total 8462 _reflns_number_gt 4994 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement 'SAINT (Bruker, 2004)' _computing_data_reduction 'SAINT (Bruker, 2004)' _computing_structure_solution 'SHELXTL (Bruker, 2004)' _computing_structure_refinement 'SHELXTL (Bruker, 2004)' _computing_molecular_graphics 'SHELXTL (Bruker, 2004)' _computing_publication_material 'SHELXTL (Bruker, 2004)' _refine_special_details ; Distances between the following atom pairs were restrained to 1.54\%A with estimated standard deviation 0.02: C13 and C14, C23 and C24, C33 and C34, C43 and C44. Anisotropic displacement parameters of C12, C13, C14 and C34 atoms were restrained using ISOR instructions. 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^)+(0.0791P)^2^] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8462 _refine_ls_number_parameters 329 _refine_ls_number_restraints 28 _refine_ls_R_factor_all 0.0849 _refine_ls_R_factor_gt 0.0469 _refine_ls_wR_factor_ref 0.1463 _refine_ls_wR_factor_gt 0.1321 _refine_ls_goodness_of_fit_ref 0.936 _refine_ls_restrained_S_all 0.939 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group I1 I 0.29599(4) 0.35665(5) -0.00204(3) 0.05593(17) Uani 1 1 d . . . Mo1 Mo 0.44967(5) 0.43919(6) 0.06840(3) 0.04199(18) Uani 1 1 d . . . N1 N 0.3268(6) 0.3723(7) 0.1710(4) 0.067(2) Uani 1 1 d . . . I2 I 0.46253(4) 0.77418(5) -0.05609(2) 0.05372(17) Uani 1 1 d . . . Mo2 Mo 0.38387(5) 0.56264(6) -0.02782(3) 0.04182(18) Uani 1 1 d . . . N2 N 0.1855(7) 0.6152(9) -0.0879(4) 0.082(3) Uani 1 1 d . . . I3 I 0.60092(4) 0.51587(5) 0.14368(2) 0.05202(17) Uani 1 1 d . . . Mo3 Mo 0.53048(5) 0.63996(6) 0.04217(3) 0.04212(18) Uani 1 1 d . . . N3 N 0.5715(9) 0.8907(8) 0.0910(4) 0.109(4) Uani 1 1 d . . . I4 I 0.35969(4) 0.64847(5) 0.08629(2) 0.05428(17) Uani 1 1 d . . . N4 N 0.4561(5) 0.0375(7) 0.2723(4) 0.068(2) Uani 1 1 d . . . O11 O 0.4062(4) 0.3653(5) 0.1494(3) 0.0612(16) Uani 1 1 d . . . C11 C 0.3586(8) 0.0408(11) 0.2395(5) 0.095(4) Uani 1 1 d . . . H11A H 0.3213 -0.0170 0.2575 0.114 Uiso 1 1 calc R . . H11B H 0.3320 0.1168 0.2458 0.114 Uiso 1 1 calc R . . O12 O 0.3184(5) 0.3334(6) 0.2210(3) 0.083(2) Uani 1 1 d . . . C12 C 0.3538(10) 0.0187(14) 0.1747(6) 0.126(5) Uani 1 1 d DU . . H12A H 0.3806 -0.0575 0.1690 0.151 Uiso 1 1 calc R . . H12B H 0.3928 0.0757 0.1575 0.151 Uiso 1 1 calc R . . O13 O 0.2616(5) 0.4199(7) 0.1409(3) 0.091(2) Uani 1 1 d . . . C13 C 0.2610(13) 0.0218(17) 0.1385(7) 0.165(7) Uani 1 1 d DU . . H13A H 0.2338 0.0981 0.1434 0.198 Uiso 1 1 calc R . . H13B H 0.2216 -0.0355 0.1550 0.198 Uiso 1 1 calc R . . C14 C 0.2618(17) -0.002(2) 0.0707(7) 0.230(10) Uani 1 1 d DU . . H14A H 0.2662 -0.0848 0.0641 0.345 Uiso 1 1 calc R . . H14B H 0.3137 0.0362 0.0562 0.345 Uiso 1 1 calc R . . H14C H 0.2060 0.0269 0.0494 0.345 Uiso 1 1 calc R . . O21 O 0.2545(5) 0.6487(6) -0.0532(3) 0.078(2) Uani 1 1 d . . . C21 C 0.5127(8) 0.1325(9) 0.2475(5) 0.081(3) Uani 1 1 d . . . H21A H 0.5156 0.1178 0.2050 0.097 Uiso 1 1 calc R . . H21B H 0.4807 0.2061 0.2510 0.097 Uiso 1 1 calc R . . O22 O 0.1846(6) 0.5160(9) -0.1096(4) 0.116(3) Uani 1 1 d . . . C22 C 0.6090(8) 0.1460(11) 0.2769(6) 0.101(4) Uani 1 1 d . . . H22A H 0.6432 0.0741 0.2732 0.121 Uiso 1 1 calc R . . H22B H 0.6082 0.1633 0.3194 0.121 Uiso 1 1 calc R . . O23 O 0.1194(6) 0.6846(9) -0.0971(4) 0.124(3) Uani 1 1 d . . . C23 C 0.6558(8) 0.2480(12) 0.2449(7) 0.132(5) Uani 1 1 d D . . H23A H 0.6551 0.2286 0.2025 0.158 Uiso 1 1 calc R . . H23B H 0.6185 0.3176 0.2476 0.158 Uiso 1 1 calc R . . C24 C 0.7537(9) 0.2773(15) 0.2689(8) 0.170(8) Uani 1 1 d D . . H24A H 0.7948 0.2205 0.2548 0.255 Uiso 1 1 calc R . . H24B H 0.7591 0.2765 0.3122 0.255 Uiso 1 1 calc R . . H24C H 0.7692 0.3535 0.2551 0.255 Uiso 1 1 calc R . . O31 O 0.5612(5) 0.7898(5) 0.0974(3) 0.080(2) Uani 1 1 d . . . C31 C 0.4500(8) 0.0541(10) 0.3404(5) 0.082(3) Uani 1 1 d . . . H31A H 0.4106 -0.0071 0.3534 0.099 Uiso 1 1 calc R . . H31B H 0.5110 0.0410 0.3608 0.099 Uiso 1 1 calc R . . O32 O 0.6115(7) 0.9078(9) 0.0422(5) 0.134(3) Uani 1 1 d . . . C32 C 0.4162(9) 0.1661(11) 0.3624(6) 0.108(4) Uani 1 1 d . . . H32A H 0.4561 0.2283 0.3510 0.130 Uiso 1 1 calc R . . H32B H 0.3550 0.1807 0.3425 0.130 Uiso 1 1 calc R . . O33 O 0.5856(6) 0.9650(6) 0.1273(3) 0.088(2) Uani 1 1 d . . . C33 C 0.4122(8) 0.1706(13) 0.4279(6) 0.111(5) Uani 1 1 d D . . H33A H 0.3768 0.1043 0.4397 0.133 Uiso 1 1 calc R . . H33B H 0.3795 0.2409 0.4375 0.133 Uiso 1 1 calc R . . C34 C 0.5052(10) 0.1698(17) 0.4649(7) 0.174(7) Uani 1 1 d DU . . H34A H 0.5414 0.1062 0.4521 0.261 Uiso 1 1 calc R . . H34B H 0.4967 0.1603 0.5067 0.261 Uiso 1 1 calc R . . H34C H 0.5363 0.2422 0.4593 0.261 Uiso 1 1 calc R . . C41 C 0.5014(7) -0.0802(9) 0.2644(5) 0.075(3) Uani 1 1 d . . . H41A H 0.5162 -0.0861 0.2231 0.090 Uiso 1 1 calc R . . H41B H 0.5590 -0.0822 0.2902 0.090 Uiso 1 1 calc R . . C42 C 0.4457(8) -0.1866(10) 0.2781(6) 0.090(3) Uani 1 1 d . . . H42A H 0.4367 -0.1873 0.3206 0.107 Uiso 1 1 calc R . . H42B H 0.3856 -0.1828 0.2553 0.107 Uiso 1 1 calc R . . C43 C 0.4926(9) -0.2943(10) 0.2628(6) 0.096(4) Uani 1 1 d . . . H43A H 0.5499 -0.3010 0.2888 0.115 Uiso 1 1 calc R . . H43B H 0.5079 -0.2886 0.2216 0.115 Uiso 1 1 calc R . . C44 C 0.4371(12) -0.4024(12) 0.2690(7) 0.145(6) Uani 1 1 d . . . H44A H 0.4392 -0.4501 0.2338 0.218 Uiso 1 1 calc R . . H44B H 0.3744 -0.3814 0.2733 0.218 Uiso 1 1 calc R . . H44C H 0.4619 -0.4451 0.3040 0.218 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 0.0478(3) 0.0531(3) 0.0661(4) 0.0015(3) 0.0020(3) -0.0062(3) Mo1 0.0436(4) 0.0373(4) 0.0449(4) 0.0023(3) 0.0033(3) 0.0026(3) N1 0.072(6) 0.055(5) 0.072(5) -0.001(4) 0.001(5) -0.001(4) I2 0.0644(4) 0.0376(3) 0.0580(3) 0.0053(2) 0.0000(3) 0.0066(3) Mo2 0.0407(4) 0.0375(4) 0.0463(4) 0.0006(3) -0.0006(3) 0.0052(3) N2 0.067(6) 0.091(7) 0.085(6) -0.008(5) -0.008(5) 0.009(6) I3 0.0578(4) 0.0511(3) 0.0453(3) -0.0006(2) -0.0038(2) 0.0040(3) Mo3 0.0452(4) 0.0351(4) 0.0452(4) -0.0008(3) 0.0001(3) 0.0023(3) N3 0.221(14) 0.054(6) 0.054(5) -0.008(5) 0.020(7) -0.027(7) I4 0.0555(4) 0.0517(3) 0.0562(3) -0.0045(3) 0.0083(3) 0.0110(3) N4 0.041(4) 0.085(6) 0.078(5) 0.003(4) 0.006(4) 0.004(4) O11 0.051(4) 0.075(4) 0.060(3) 0.013(3) 0.020(3) 0.012(3) C11 0.084(9) 0.103(9) 0.096(8) 0.002(7) 0.003(7) 0.027(7) O12 0.095(6) 0.082(5) 0.073(5) 0.022(4) 0.022(4) 0.001(4) C12 0.113(8) 0.154(9) 0.108(7) -0.001(7) -0.001(7) 0.001(7) O13 0.064(5) 0.112(6) 0.099(5) 0.031(5) 0.021(4) 0.021(4) C13 0.138(10) 0.194(11) 0.161(10) -0.007(8) 0.008(8) 0.021(8) C14 0.226(13) 0.247(13) 0.212(13) 0.015(9) 0.007(9) -0.008(9) O21 0.057(4) 0.092(5) 0.082(4) -0.006(4) -0.013(4) 0.020(4) C21 0.070(7) 0.077(7) 0.099(8) 0.017(6) 0.020(6) -0.001(6) O22 0.089(6) 0.120(8) 0.133(7) -0.038(6) -0.019(5) -0.003(6) C22 0.073(8) 0.086(9) 0.145(11) 0.031(8) 0.019(8) -0.005(7) O23 0.075(6) 0.146(8) 0.141(8) -0.010(6) -0.033(5) 0.040(6) C23 0.119(13) 0.114(11) 0.167(14) 0.055(10) 0.033(11) -0.005(10) C24 0.074(10) 0.168(16) 0.26(2) 0.062(15) -0.018(12) -0.057(11) O31 0.118(6) 0.038(4) 0.080(4) -0.003(3) -0.007(4) -0.009(4) C31 0.070(7) 0.090(8) 0.091(8) 0.014(6) 0.023(6) 0.003(6) O32 0.129(9) 0.120(8) 0.152(9) -0.015(7) 0.003(7) -0.023(6) C32 0.075(9) 0.090(9) 0.159(13) -0.015(9) 0.009(8) 0.021(7) O33 0.119(7) 0.058(4) 0.087(5) -0.016(4) 0.013(4) -0.008(4) C33 0.090(10) 0.155(13) 0.091(8) -0.042(9) 0.023(7) 0.007(9) C34 0.174(10) 0.182(11) 0.166(10) -0.023(8) 0.017(8) 0.015(9) C41 0.053(6) 0.084(7) 0.088(7) 0.002(6) 0.004(5) 0.008(6) C42 0.075(8) 0.082(8) 0.115(9) 0.003(7) 0.027(7) -0.003(6) C43 0.116(10) 0.075(8) 0.100(9) -0.001(7) 0.027(7) -0.008(7) C44 0.166(16) 0.103(11) 0.174(15) -0.007(10) 0.059(13) -0.028(11) _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 Mo1 2.7707(9) . ? I1 Mo3 2.7709(9) 3_665 ? I1 Mo2 2.7732(9) . ? Mo1 O11 2.149(6) . ? Mo1 Mo2 2.6664(9) . ? Mo1 Mo3 2.6713(9) 3_665 ? Mo1 Mo3 2.6759(9) . ? Mo1 Mo2 2.6776(9) 3_665 ? Mo1 I3 2.7769(9) . ? Mo1 I4 2.7811(8) . ? Mo1 I2 2.7857(8) 3_665 ? N1 O12 1.219(9) . ? N1 O13 1.234(10) . ? N1 O11 1.302(10) . ? I2 Mo3 2.7767(8) . ? I2 Mo2 2.7807(9) . ? I2 Mo1 2.7857(8) 3_665 ? Mo2 O21 2.154(6) . ? Mo2 Mo3 2.6686(9) . ? Mo2 Mo3 2.6701(9) 3_665 ? Mo2 Mo1 2.6776(9) 3_665 ? Mo2 I3 2.7668(8) 3_665 ? Mo2 I4 2.7846(8) . ? N2 O22 1.234(11) . ? N2 O23 1.250(11) . ? N2 O21 1.266(10) . ? I3 Mo2 2.7667(8) 3_665 ? I3 Mo3 2.7805(8) . ? Mo3 O31 2.133(6) . ? Mo3 Mo2 2.6701(9) 3_665 ? Mo3 Mo1 2.6713(9) 3_665 ? Mo3 I1 2.7709(9) 3_665 ? Mo3 I4 2.7732(9) . ? N3 O31 1.175(10) . ? N3 O33 1.178(10) . ? N3 O32 1.301(12) . ? N4 C21 1.505(12) . ? N4 C41 1.519(13) . ? N4 C11 1.532(13) . ? N4 C31 1.542(12) . ? C11 C12 1.463(15) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.505(19) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.539(9) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C21 C22 1.498(15) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.562(15) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.512(9) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C31 C32 1.476(14) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 C33 1.470(16) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C34 1.516(9) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C41 C42 1.513(14) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 C43 1.468(15) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C43 C44 1.494(16) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? 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 Mo1 I1 Mo3 57.64(2) . 3_665 ? Mo1 I1 Mo2 57.50(2) . . ? Mo3 I1 Mo2 57.58(2) 3_665 . ? O11 Mo1 Mo2 140.62(16) . . ? O11 Mo1 Mo3 135.39(17) . 3_665 ? Mo2 Mo1 Mo3 60.03(2) . 3_665 ? O11 Mo1 Mo3 134.17(17) . . ? Mo2 Mo1 Mo3 59.94(2) . . ? Mo3 Mo1 Mo3 89.89(3) 3_665 . ? O11 Mo1 Mo2 129.55(16) . 3_665 ? Mo2 Mo1 Mo2 89.82(3) . 3_665 ? Mo3 Mo1 Mo2 59.86(2) 3_665 3_665 ? Mo3 Mo1 Mo2 59.83(2) . 3_665 ? O11 Mo1 I1 92.95(17) . . ? Mo2 Mo1 I1 61.30(2) . . ? Mo3 Mo1 I1 61.18(2) 3_665 . ? Mo3 Mo1 I1 121.23(3) . . ? Mo2 Mo1 I1 121.03(3) 3_665 . ? O11 Mo1 I3 84.29(17) . . ? Mo2 Mo1 I3 121.22(3) . . ? Mo3 Mo1 I3 120.77(3) 3_665 . ? Mo3 Mo1 I3 61.28(2) . . ? Mo2 Mo1 I3 60.93(2) 3_665 . ? I1 Mo1 I3 177.22(3) . . ? O11 Mo1 I4 92.00(16) . . ? Mo2 Mo1 I4 61.44(2) . . ? Mo3 Mo1 I4 121.47(3) 3_665 . ? Mo3 Mo1 I4 61.05(2) . . ? Mo2 Mo1 I4 120.87(3) 3_665 . ? I1 Mo1 I4 90.49(3) . . ? I3 Mo1 I4 89.92(2) . . ? O11 Mo1 I2 85.14(16) . 3_665 ? Mo2 Mo1 I2 121.15(3) . 3_665 ? Mo3 Mo1 I2 61.13(2) 3_665 3_665 ? Mo3 Mo1 I2 120.98(3) . 3_665 ? Mo2 Mo1 I2 61.15(2) 3_665 3_665 ? I1 Mo1 I2 89.93(2) . 3_665 ? I3 Mo1 I2 89.52(3) . 3_665 ? I4 Mo1 I2 177.13(3) . 3_665 ? O12 N1 O13 121.0(9) . . ? O12 N1 O11 119.5(8) . . ? O13 N1 O11 119.6(8) . . ? Mo3 I2 Mo2 57.40(2) . . ? Mo3 I2 Mo1 57.40(2) . 3_665 ? Mo2 I2 Mo1 57.50(2) . 3_665 ? O21 Mo2 Mo1 133.50(19) . . ? O21 Mo2 Mo3 129.12(19) . . ? Mo1 Mo2 Mo3 60.21(2) . . ? O21 Mo2 Mo3 140.79(19) . 3_665 ? Mo1 Mo2 Mo3 60.08(2) . 3_665 ? Mo3 Mo2 Mo3 90.07(3) . 3_665 ? O21 Mo2 Mo1 135.73(19) . 3_665 ? Mo1 Mo2 Mo1 90.18(3) . 3_665 ? Mo3 Mo2 Mo1 59.96(2) . 3_665 ? Mo3 Mo2 Mo1 60.05(2) 3_665 3_665 ? O21 Mo2 I3 93.15(18) . 3_665 ? Mo1 Mo2 I3 121.55(3) . 3_665 ? Mo3 Mo2 I3 121.25(3) . 3_665 ? Mo3 Mo2 I3 61.49(2) 3_665 3_665 ? Mo1 Mo2 I3 61.31(2) 3_665 3_665 ? O21 Mo2 I1 91.8(2) . . ? Mo1 Mo2 I1 61.20(2) . . ? Mo3 Mo2 I1 121.41(3) . . ? Mo3 Mo2 I1 61.17(2) 3_665 . ? Mo1 Mo2 I1 121.21(3) 3_665 . ? I3 Mo2 I1 90.00(2) 3_665 . ? O21 Mo2 I2 85.0(2) . . ? Mo1 Mo2 I2 121.42(3) . . ? Mo3 Mo2 I2 61.23(2) . . ? Mo3 Mo2 I2 121.38(3) 3_665 . ? Mo1 Mo2 I2 61.34(2) 3_665 . ? I3 Mo2 I2 89.83(3) 3_665 . ? I1 Mo2 I2 176.82(3) . . ? O21 Mo2 I4 83.64(18) . . ? Mo1 Mo2 I4 61.31(2) . . ? Mo3 Mo2 I4 61.09(2) . . ? Mo3 Mo2 I4 121.38(3) 3_665 . ? Mo1 Mo2 I4 121.03(3) 3_665 . ? I3 Mo2 I4 176.78(3) 3_665 . ? I1 Mo2 I4 90.37(3) . . ? I2 Mo2 I4 89.62(2) . . ? O22 N2 O23 122.9(10) . . ? O22 N2 O21 119.7(10) . . ? O23 N2 O21 117.4(10) . . ? Mo2 I3 Mo1 57.76(2) 3_665 . ? Mo2 I3 Mo3 57.54(2) 3_665 . ? Mo1 I3 Mo3 57.57(2) . . ? O31 Mo3 Mo2 135.5(2) . . ? O31 Mo3 Mo2 134.0(2) . 3_665 ? Mo2 Mo3 Mo2 89.93(3) . 3_665 ? O31 Mo3 Mo1 140.4(2) . 3_665 ? Mo2 Mo3 Mo1 60.19(2) . 3_665 ? Mo2 Mo3 Mo1 59.89(2) 3_665 3_665 ? O31 Mo3 Mo1 129.52(19) . . ? Mo2 Mo3 Mo1 59.85(2) . . ? Mo2 Mo3 Mo1 60.11(2) 3_665 . ? Mo1 Mo3 Mo1 90.11(3) 3_665 . ? O31 Mo3 I1 91.7(2) . 3_665 ? Mo2 Mo3 I1 121.36(3) . 3_665 ? Mo2 Mo3 I1 61.25(2) 3_665 3_665 ? Mo1 Mo3 I1 61.18(2) 3_665 3_665 ? Mo1 Mo3 I1 121.36(3) . 3_665 ? O31 Mo3 I4 84.9(2) . . ? Mo2 Mo3 I4 61.52(2) . . ? Mo2 Mo3 I4 121.45(3) 3_665 . ? Mo1 Mo3 I4 121.70(3) 3_665 . ? Mo1 Mo3 I4 61.35(2) . . ? I1 Mo3 I4 176.58(3) 3_665 . ? O31 Mo3 I2 92.74(18) . . ? Mo2 Mo3 I2 61.38(2) . . ? Mo2 Mo3 I2 121.36(3) 3_665 . ? Mo1 Mo3 I2 61.47(2) 3_665 . ? Mo1 Mo3 I2 121.22(3) . . ? I1 Mo3 I2 90.11(3) 3_665 . ? I4 Mo3 I2 89.94(3) . . ? O31 Mo3 I3 84.39(18) . . ? Mo2 Mo3 I3 121.00(3) . . ? Mo2 Mo3 I3 60.97(2) 3_665 . ? Mo1 Mo3 I3 120.85(3) 3_665 . ? Mo1 Mo3 I3 61.15(2) . . ? I1 Mo3 I3 89.76(3) 3_665 . ? I4 Mo3 I3 90.01(2) . . ? I2 Mo3 I3 177.12(3) . . ? O31 N3 O33 130.0(10) . . ? O31 N3 O32 108.9(10) . . ? O33 N3 O32 113.8(10) . . ? Mo3 I4 Mo1 57.60(2) . . ? Mo3 I4 Mo2 57.39(2) . . ? Mo1 I4 Mo2 57.25(2) . . ? C21 N4 C41 109.7(7) . . ? C21 N4 C11 108.9(8) . . ? C41 N4 C11 111.1(8) . . ? C21 N4 C31 111.1(8) . . ? C41 N4 C31 107.1(7) . . ? C11 N4 C31 108.8(8) . . ? N1 O11 Mo1 129.5(5) . . ? C12 C11 N4 114.6(10) . . ? C12 C11 H11A 108.6 . . ? N4 C11 H11A 108.6 . . ? C12 C11 H11B 108.6 . . ? N4 C11 H11B 108.6 . . ? H11A C11 H11B 107.6 . . ? C11 C12 C13 118.4(13) . . ? C11 C12 H12A 107.7 . . ? C13 C12 H12A 107.7 . . ? C11 C12 H12B 107.7 . . ? C13 C12 H12B 107.7 . . ? H12A C12 H12B 107.1 . . ? C12 C13 C14 115.2(14) . . ? C12 C13 H13A 108.5 . . ? C14 C13 H13A 108.5 . . ? C12 C13 H13B 108.5 . . ? C14 C13 H13B 108.5 . . ? H13A C13 H13B 107.5 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N2 O21 Mo2 130.0(7) . . ? C22 C21 N4 116.1(9) . . ? C22 C21 H21A 108.3 . . ? N4 C21 H21A 108.3 . . ? C22 C21 H21B 108.3 . . ? N4 C21 H21B 108.3 . . ? H21A C21 H21B 107.4 . . ? C21 C22 C23 108.1(10) . . ? C21 C22 H22A 110.1 . . ? C23 C22 H22A 110.1 . . ? C21 C22 H22B 110.1 . . ? C23 C22 H22B 110.1 . . ? H22A C22 H22B 108.4 . . ? C24 C23 C22 116.4(11) . . ? C24 C23 H23A 108.2 . . ? C22 C23 H23A 108.2 . . ? C24 C23 H23B 108.2 . . ? C22 C23 H23B 108.2 . . ? H23A C23 H23B 107.3 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N3 O31 Mo3 138.0(7) . . ? C32 C31 N4 119.3(10) . . ? C32 C31 H31A 107.5 . . ? N4 C31 H31A 107.5 . . ? C32 C31 H31B 107.5 . . ? N4 C31 H31B 107.5 . . ? H31A C31 H31B 107.0 . . ? C33 C32 C31 114.2(11) . . ? C33 C32 H32A 108.7 . . ? C31 C32 H32A 108.7 . . ? C33 C32 H32B 108.7 . . ? C31 C32 H32B 108.7 . . ? H32A C32 H32B 107.6 . . ? C32 C33 C34 114.7(12) . . ? C32 C33 H33A 108.6 . . ? C34 C33 H33A 108.6 . . ? C32 C33 H33B 108.6 . . ? C34 C33 H33B 108.6 . . ? H33A C33 H33B 107.6 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C42 C41 N4 116.2(8) . . ? C42 C41 H41A 108.2 . . ? N4 C41 H41A 108.2 . . ? C42 C41 H41B 108.2 . . ? N4 C41 H41B 108.2 . . ? H41A C41 H41B 107.4 . . ? C43 C42 C41 110.9(9) . . ? C43 C42 H42A 109.5 . . ? C41 C42 H42A 109.5 . . ? C43 C42 H42B 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 108.1 . . ? C42 C43 C44 113.8(11) . . ? C42 C43 H43A 108.8 . . ? C44 C43 H43A 108.8 . . ? C42 C43 H43B 108.8 . . ? C44 C43 H43B 108.8 . . ? H43A C43 H43B 107.7 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.644 _refine_diff_density_min -0.826 _refine_diff_density_rms 0.189 _publ_section_references ; Bruker AXS Inc. (2004). APEX2 (Version 1.08), SAINT (Version 7.03), SADABS (Version 2.11) and SHELXTL (Version 6.12). Bruker Advanced X-ray Solutions, Madison, WI, USA. Sluis, P. van der & Spek, A. L. (1990). Acta Cryst. A46, 194-201. Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13. ; _database_code_depnum_ccdc_archive 'CCDC 949910'