# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_Sample2 _audit_creation_date 2013-05-31 _audit_creation_method ; Olex2 1.2-ac2 (compiled 2012.03.27 svn.r2268, GUI svn.r4156) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C20 H44 Mo3 N2 O8 P4 S12' _chemical_formula_sum 'C20 H44 Mo3 N2 O8 P4 S12' _chemical_formula_weight 1236.99 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.8738(12) _cell_length_b 14.0031(8) _cell_length_c 14.1787(12) _cell_angle_alpha 109.182(7) _cell_angle_beta 109.922(8) _cell_angle_gamma 106.909(7) _cell_volume 2179.8(3) _cell_formula_units_Z 2 _cell_measurement_reflns_used 9820 _cell_measurement_temperature 100.00(10) _cell_measurement_theta_max 29.4108 _cell_measurement_theta_min 3.0474 _exptl_absorpt_coefficient_mu 1.613 _exptl_absorpt_correction_T_max 0.924 _exptl_absorpt_correction_T_min 0.748 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_crystal_colour 'dark brown' _exptl_crystal_density_diffrn 1.885 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 1240 _exptl_crystal_size_max 0.3091 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.0596 _exptl_special_details ; ? ; _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0253 _diffrn_reflns_av_unetI/netI 0.0341 _diffrn_reflns_Laue_measured_fraction_full 0.946 _diffrn_reflns_Laue_measured_fraction_max 0.969 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 16895 _diffrn_reflns_point_group_measured_fraction_full 0.946 _diffrn_reflns_point_group_measured_fraction_max 0.969 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.027 _diffrn_reflns_theta_min 3.047 _diffrn_ambient_temperature 100.00(10) _diffrn_detector_area_resol_mean 10.5953 _diffrn_measured_fraction_theta_full 0.9657 _diffrn_measured_fraction_theta_max 0.8159 _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0522286000 _diffrn_orient_matrix_UB_12 0.0121733000 _diffrn_orient_matrix_UB_13 -0.0023024000 _diffrn_orient_matrix_UB_21 -0.0040253000 _diffrn_orient_matrix_UB_22 0.0445027000 _diffrn_orient_matrix_UB_23 -0.0119253000 _diffrn_orient_matrix_UB_31 0.0312934000 _diffrn_orient_matrix_UB_32 0.0386362000 _diffrn_orient_matrix_UB_33 0.0592512000 _diffrn_radiation_monochromator mirror _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_source 'SuperNova (Mo) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 6664 _reflns_number_total 7478 _reflns_odcompleteness_completeness 96.57 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; SHELXL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution ; M.C.Burla, R.Caliandro, M.Camalli, B.Carrozzini, G.L.Cascarano, C.Giacovazzo, M.Mallamo, A.Mazzone, G.Polidori and R. Spagna SIR2011: a new package for crystal structure determination and refinement J. Appl. Cryst. (2012). 45, 357-361. ; _refine_diff_density_max 1.993 _refine_diff_density_min -1.259 _refine_diff_density_rms 0.126 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 450 _refine_ls_number_reflns 7478 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0448 _refine_ls_R_factor_gt 0.0389 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0375P)^2^+12.2435P] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0943 _refine_ls_wR_factor_ref 0.0986 _refine_special_details ; ? ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.05344(3) 0.25270(3) 0.10236(3) 0.01218(11) Uani 1 1 d . . . . . Mo2 Mo -0.16266(3) 0.16172(3) 0.08116(3) 0.01253(11) Uani 1 1 d . . . . . Mo3 Mo 0.01513(3) 0.15134(3) 0.23222(3) 0.01328(11) Uani 1 1 d . . . . . S1 S 0.00200(10) 0.31726(9) 0.24430(10) 0.0149(2) Uani 1 1 d . . . . . S2 S -0.11545(10) 0.13301(10) -0.06155(9) 0.0150(2) Uani 1 1 d . . . . . S3 S 0.10097(10) 0.11369(9) 0.12098(10) 0.0143(2) Uani 1 1 d . . . . . S4 S -0.16151(10) 0.00161(10) 0.09242(10) 0.0168(2) Uani 1 1 d . . . . . S11 S 0.06118(10) 0.42875(10) 0.08090(10) 0.0162(2) Uani 1 1 d . . . . . S12 S 0.14523(10) 0.24930(10) -0.02806(10) 0.0166(3) Uani 1 1 d . . . . . S21 S -0.22751(11) 0.30859(10) 0.05511(11) 0.0202(3) Uani 1 1 d . . . . . S22 S -0.37165(10) 0.03730(10) -0.08222(10) 0.0176(3) Uani 1 1 d . . . . . S31 S 0.20350(11) 0.28585(11) 0.42082(10) 0.0228(3) Uani 1 1 d . . . . . S32 S 0.06863(11) 0.01441(10) 0.30124(10) 0.0197(3) Uani 1 1 d . . . . . S41 S -0.28373(13) 0.16032(12) 0.18793(12) 0.0325(3) Uani 1 1 d . . . . . S42 S -0.05954(14) 0.16063(14) 0.38026(14) 0.0373(4) Uani 1 1 d . . . . . P11 P 0.14813(11) 0.39929(10) -0.00239(10) 0.0148(3) Uani 1 1 d . . . . . P21 P -0.37478(11) 0.17958(11) -0.07916(12) 0.0201(3) Uani 1 1 d . . . . . P31 P 0.21352(12) 0.14980(11) 0.43168(11) 0.0211(3) Uani 1 1 d . . . . . P41 P -0.17863(14) 0.21385(13) 0.35089(13) 0.0324(3) Uani 1 1 d . . . . . O11 O 0.1045(3) 0.4055(3) -0.1175(3) 0.0171(7) Uani 1 1 d . . . . . O12 O 0.2736(3) 0.5018(3) 0.0707(3) 0.0195(7) Uani 1 1 d . . . . . O21 O -0.4863(3) 0.1872(3) -0.0819(3) 0.0287(9) Uani 1 1 d . . . . . O22 O -0.3956(3) 0.1852(3) -0.1932(3) 0.0311(9) Uani 1 1 d . . . . . O31 O 0.3272(3) 0.1461(3) 0.4367(3) 0.0264(8) Uani 1 1 d . . . . . O32 O 0.2402(3) 0.1584(3) 0.5523(3) 0.0315(9) Uani 1 1 d . . . . . O41 O -0.1187(4) 0.3470(4) 0.4261(4) 0.0478(12) Uani 1 1 d . . . . . O42 O -0.2539(4) 0.1745(3) 0.4051(4) 0.0400(10) Uani 1 1 d . . . . . N1 N 0.2448(3) 0.3834(3) 0.2419(3) 0.0176(9) Uani 1 1 d . . . . . N2 N 0.3814(4) 0.5627(4) 0.4045(4) 0.0362(12) Uani 1 1 d . . . . . C1 C 0.3317(4) 0.3590(5) 0.2412(5) 0.0234(11) Uani 1 1 d . . . . . H1 H 0.3142 0.2887 0.1861 0.028 Uiso 1 1 calc R U . . . C2 C 0.4446(5) 0.4338(5) 0.3185(5) 0.0329(13) Uani 1 1 d . . . . . H2 H 0.5041 0.4166 0.3167 0.039 Uiso 1 1 calc R U . . . C3 C 0.4652(5) 0.5358(5) 0.3990(5) 0.0376(15) Uani 1 1 d . . . . . H3 H 0.5411 0.5887 0.4522 0.045 Uiso 1 1 calc R U . . . C4 C 0.2745(5) 0.4835(4) 0.3243(4) 0.0220(11) Uani 1 1 d . . . . . H4 H 0.2149 0.5004 0.3265 0.026 Uiso 1 1 calc R U . . . C11 C -0.0115(5) 0.3261(4) -0.2110(4) 0.0236(11) Uani 1 1 d . . . . . H11A H -0.0677 0.3347 -0.1874 0.028 Uiso 1 1 calc R U . . . H11B H -0.0225 0.2488 -0.2338 0.028 Uiso 1 1 calc R U . . . C12 C -0.0266(6) 0.3510(5) -0.3085(5) 0.0371(14) Uani 1 1 d . . . . . H12A H -0.1037 0.3017 -0.3701 0.056 Uiso 1 1 calc R U . . . H12B H 0.0269 0.3387 -0.3336 0.056 Uiso 1 1 calc R U . . . H12C H -0.0127 0.4285 -0.2842 0.056 Uiso 1 1 calc R U . . . C13 C 0.3566(4) 0.5051(4) 0.0290(5) 0.0242(12) Uani 1 1 d . . . . . H13A H 0.3449 0.5359 -0.0238 0.029 Uiso 1 1 calc R U . . . H13B H 0.3476 0.4293 -0.0104 0.029 Uiso 1 1 calc R U . . . C14 C 0.4747(5) 0.5794(5) 0.1306(5) 0.0333(13) Uani 1 1 d . . . . . H14A H 0.5314 0.5832 0.1058 0.050 Uiso 1 1 calc R U . . . H14B H 0.4853 0.5482 0.1822 0.050 Uiso 1 1 calc R U . . . H14C H 0.4828 0.6543 0.1686 0.050 Uiso 1 1 calc R U . . . C21 C -0.5317(6) 0.1593(5) -0.0112(6) 0.0384(15) Uani 1 1 d . . . . . H21A H -0.4917 0.1239 0.0243 0.046 Uiso 1 1 calc R U . . . H21B H -0.6126 0.1055 -0.0584 0.046 Uiso 1 1 calc R U . . . C22 C -0.5181(7) 0.2607(6) 0.0774(7) 0.058(2) Uani 1 1 d . . . . . H22A H -0.5580 0.2957 0.0424 0.087 Uiso 1 1 calc R U . . . H22B H -0.4379 0.3132 0.1255 0.087 Uiso 1 1 calc R U . . . H22C H -0.5496 0.2398 0.1224 0.087 Uiso 1 1 calc R U . . . C23 C -0.3059(5) 0.2110(6) -0.2246(5) 0.0351(14) Uani 1 1 d . . . . . H23A H -0.2978 0.1435 -0.2589 0.042 Uiso 1 1 calc R U . . . H23B H -0.2330 0.2682 -0.1577 0.042 Uiso 1 1 calc R U . . . C24 C -0.3396(6) 0.2535(6) -0.3072(5) 0.0406(15) Uani 1 1 d . . . . . H24A H -0.4129 0.1970 -0.3720 0.061 Uiso 1 1 calc R U . . . H24B H -0.2829 0.2692 -0.3315 0.061 Uiso 1 1 calc R U . . . H24C H -0.3449 0.3217 -0.2716 0.061 Uiso 1 1 calc R U . . . C31 C 0.3522(5) 0.1430(5) 0.3442(5) 0.0313(13) Uani 1 1 d . . . . . H31A H 0.3483 0.2056 0.3305 0.038 Uiso 1 1 calc R U . . . H31B H 0.2958 0.0726 0.2748 0.038 Uiso 1 1 calc R U . . . C32 C 0.4682(5) 0.1515(6) 0.3762(5) 0.0483(19) Uani 1 1 d . . . . . H32A H 0.4890 0.1580 0.3197 0.072 Uiso 1 1 calc R U . . . H32B H 0.4690 0.0847 0.3807 0.072 Uiso 1 1 calc R U . . . H32C H 0.5224 0.2172 0.4489 0.072 Uiso 1 1 calc R U . . . C33 C 0.1548(7) 0.1461(8) 0.5912(6) 0.061(2) Uani 1 1 d . . . . . H33A H 0.1005 0.0666 0.5545 0.073 Uiso 1 1 calc R U . . . H33B H 0.1126 0.1870 0.5711 0.073 Uiso 1 1 calc R U . . . C34 C 0.2130(7) 0.1911(8) 0.7147(6) 0.071(3) Uani 1 1 d . . . . . H34A H 0.2549 0.1504 0.7341 0.107 Uiso 1 1 calc R U . . . H34B H 0.1571 0.1823 0.7406 0.107 Uiso 1 1 calc R U . . . H34C H 0.2654 0.2701 0.7506 0.107 Uiso 1 1 calc R U . . . C43 C -0.3257(6) 0.0537(5) 0.3592(6) 0.0401(15) Uani 1 1 d . . . . . H43A H -0.2931 0.0097 0.3244 0.048 Uiso 1 1 calc R U . . . H43B H -0.4024 0.0306 0.3014 0.048 Uiso 1 1 calc R U . . . C44 C -0.3312(7) 0.0329(7) 0.4558(7) 0.0536(19) Uani 1 1 d . . . . . H44A H -0.3799 -0.0459 0.4265 0.080 Uiso 1 1 calc R U . . . H44B H -0.3619 0.0780 0.4909 0.080 Uiso 1 1 calc R U . . . H44C H -0.2552 0.0536 0.5113 0.080 Uiso 1 1 calc R U . . . C41 C -0.2174(14) 0.4110(7) 0.4180(9) 0.131(6) Uani 1 1 d . . . . . H41A H -0.2974 0.3576 0.3637 0.157 Uiso 1 1 d R U . . . H41B H -0.2085 0.4576 0.4913 0.157 Uiso 1 1 d R U . . . C42 C -0.1637(10) 0.4681(11) 0.3785(8) 0.121(5) Uani 1 1 d . . . . . H42A H -0.1497 0.4188 0.3251 0.181 Uiso 1 1 calc R U . . . H42B H -0.0917 0.5303 0.4406 0.181 Uiso 1 1 calc R U . . . H42C H -0.2105 0.4968 0.3410 0.181 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0125(2) 0.0106(2) 0.0120(2) 0.00479(16) 0.00583(17) 0.00436(16) Mo2 0.0128(2) 0.0118(2) 0.0119(2) 0.00499(16) 0.00596(17) 0.00497(17) Mo3 0.0126(2) 0.0128(2) 0.0130(2) 0.00571(16) 0.00616(17) 0.00449(17) S1 0.0152(6) 0.0125(5) 0.0141(6) 0.0048(5) 0.0070(5) 0.0048(5) S2 0.0145(6) 0.0142(6) 0.0130(6) 0.0042(5) 0.0066(5) 0.0052(5) S3 0.0152(6) 0.0140(5) 0.0156(6) 0.0078(5) 0.0080(5) 0.0073(5) S4 0.0139(6) 0.0131(6) 0.0202(6) 0.0075(5) 0.0062(5) 0.0051(5) S11 0.0201(6) 0.0146(6) 0.0177(6) 0.0084(5) 0.0113(5) 0.0091(5) S12 0.0209(6) 0.0153(6) 0.0194(6) 0.0096(5) 0.0133(5) 0.0097(5) S21 0.0174(6) 0.0163(6) 0.0289(7) 0.0119(5) 0.0112(5) 0.0086(5) S22 0.0147(6) 0.0168(6) 0.0179(6) 0.0083(5) 0.0062(5) 0.0050(5) S31 0.0244(7) 0.0181(6) 0.0145(6) 0.0060(5) 0.0037(5) 0.0049(5) S32 0.0223(7) 0.0178(6) 0.0195(6) 0.0107(5) 0.0103(5) 0.0075(5) S41 0.0378(8) 0.0323(8) 0.0265(7) 0.0138(6) 0.0163(7) 0.0142(7) S42 0.0331(8) 0.0462(9) 0.0406(9) 0.0232(7) 0.0223(7) 0.0197(7) P11 0.0159(6) 0.0135(6) 0.0151(6) 0.0070(5) 0.0081(5) 0.0059(5) P21 0.0151(6) 0.0225(7) 0.0264(7) 0.0170(6) 0.0093(6) 0.0077(6) P31 0.0227(7) 0.0222(7) 0.0160(6) 0.0107(5) 0.0074(6) 0.0077(6) P41 0.0319(8) 0.0323(8) 0.0287(8) 0.0135(7) 0.0137(7) 0.0114(7) O11 0.0198(18) 0.0174(17) 0.0157(17) 0.0111(14) 0.0091(15) 0.0058(15) O12 0.0163(18) 0.0180(17) 0.0231(18) 0.0089(15) 0.0120(15) 0.0046(15) O21 0.0184(19) 0.034(2) 0.048(2) 0.0301(19) 0.0183(18) 0.0146(17) O22 0.020(2) 0.043(2) 0.035(2) 0.0300(19) 0.0104(18) 0.0103(18) O31 0.0212(19) 0.032(2) 0.0228(19) 0.0156(17) 0.0068(16) 0.0099(17) O32 0.036(2) 0.039(2) 0.0199(19) 0.0176(18) 0.0129(18) 0.0142(19) O41 0.049(3) 0.037(2) 0.038(3) 0.012(2) 0.015(2) 0.011(2) O42 0.039(3) 0.033(2) 0.041(2) 0.017(2) 0.017(2) 0.011(2) N1 0.018(2) 0.017(2) 0.017(2) 0.0091(17) 0.0089(18) 0.0057(18) N2 0.032(3) 0.030(3) 0.025(3) 0.012(2) 0.003(2) 0.002(2) C1 0.018(3) 0.026(3) 0.025(3) 0.015(2) 0.010(2) 0.007(2) C2 0.020(3) 0.043(4) 0.037(3) 0.027(3) 0.011(3) 0.012(3) C3 0.018(3) 0.036(3) 0.032(3) 0.020(3) -0.003(3) -0.005(3) C4 0.023(3) 0.016(2) 0.019(3) 0.007(2) 0.009(2) 0.002(2) C11 0.025(3) 0.023(3) 0.015(2) 0.008(2) 0.006(2) 0.008(2) C12 0.050(4) 0.042(4) 0.021(3) 0.017(3) 0.016(3) 0.021(3) C13 0.022(3) 0.025(3) 0.029(3) 0.012(2) 0.017(2) 0.010(2) C14 0.023(3) 0.033(3) 0.045(4) 0.020(3) 0.017(3) 0.010(3) C21 0.036(3) 0.040(3) 0.067(4) 0.035(3) 0.039(3) 0.022(3) C22 0.076(6) 0.044(4) 0.065(5) 0.024(4) 0.045(5) 0.031(4) C23 0.031(3) 0.048(4) 0.038(3) 0.029(3) 0.021(3) 0.018(3) C24 0.039(4) 0.048(4) 0.036(3) 0.025(3) 0.018(3) 0.016(3) C31 0.030(3) 0.035(3) 0.020(3) 0.008(2) 0.010(2) 0.013(3) C32 0.026(3) 0.066(5) 0.025(3) -0.001(3) 0.008(3) 0.018(3) C33 0.068(5) 0.087(6) 0.041(4) 0.037(4) 0.038(4) 0.031(5) C34 0.055(5) 0.094(6) 0.029(4) 0.020(4) 0.022(4) -0.002(5) C43 0.043(4) 0.034(3) 0.044(4) 0.017(3) 0.025(3) 0.016(3) C44 0.057(5) 0.060(5) 0.059(5) 0.039(4) 0.032(4) 0.028(4) C41 0.230(16) 0.035(5) 0.072(7) -0.001(5) 0.089(9) 0.003(7) C42 0.079(8) 0.154(11) 0.052(6) 0.004(7) 0.042(6) 0.000(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 Mo2 2.7594(6) . ? Mo1 Mo3 2.7627(6) . ? Mo1 S1 2.3526(12) . ? Mo1 S2 2.2684(13) . ? Mo1 S3 2.2934(12) . ? Mo1 S11 2.5579(12) . ? Mo1 S12 2.5742(12) . ? Mo1 N1 2.351(4) . ? Mo2 Mo3 2.7396(7) . ? Mo2 S1 2.3467(13) . ? Mo2 S2 2.2818(12) . ? Mo2 S4 2.3036(12) . ? Mo2 S21 2.5545(13) . ? Mo2 S22 2.5770(13) . ? Mo2 S41 2.6166(15) . ? Mo3 S1 2.3381(12) . ? Mo3 S3 2.2984(12) . ? Mo3 S4 2.3023(13) . ? Mo3 S31 2.5676(14) . ? Mo3 S32 2.5983(13) . ? Mo3 S42 2.6224(16) . ? S11 P11 1.9901(16) . ? S12 P11 1.9961(17) . ? S21 P21 2.0011(19) . ? S22 P21 1.9921(18) . ? S31 P31 2.0011(19) . ? S32 P31 2.0003(18) . ? S41 P41 1.989(2) . ? S42 P41 1.977(2) . ? P11 O11 1.578(3) . ? P11 O12 1.582(3) . ? P21 O21 1.570(4) . ? P21 O22 1.576(4) . ? P31 O31 1.572(4) . ? P31 O32 1.575(4) . ? P41 O41 1.579(5) . ? P41 O42 1.574(4) . ? O11 C11 1.456(6) . ? O12 C13 1.459(6) . ? O21 C21 1.449(7) . ? O22 C23 1.448(7) . ? O31 C31 1.456(6) . ? O32 C33 1.459(8) . ? O41 C41 1.834(16) . ? O42 C43 1.460(7) . ? N1 C1 1.347(7) . ? N1 C4 1.327(6) . ? N2 C3 1.341(8) . ? N2 C4 1.337(7) . ? C1 H1 0.9300 . ? C1 C2 1.369(8) . ? C2 H2 0.9300 . ? C2 C3 1.376(9) . ? C3 H3 0.9300 . ? C4 H4 0.9300 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C11 C12 1.495(8) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C13 C14 1.502(8) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 C22 1.463(9) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 C24 1.479(8) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C31 C32 1.473(8) . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C33 C34 1.459(10) . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C43 C44 1.512(9) . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C41 H41A 0.9699 . ? C41 H41B 0.9700 . ? C41 C42 1.320(13) . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 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 Mo2 Mo1 Mo3 59.487(16) . . ? S1 Mo1 Mo2 53.94(3) . . ? S1 Mo1 Mo3 53.67(3) . . ? S1 Mo1 S11 86.80(4) . . ? S1 Mo1 S12 162.02(4) . . ? S2 Mo1 Mo2 52.89(3) . . ? S2 Mo1 Mo3 98.28(3) . . ? S2 Mo1 S1 105.34(4) . . ? S2 Mo1 S3 95.62(4) . . ? S2 Mo1 S11 93.82(4) . . ? S2 Mo1 S12 85.49(4) . . ? S2 Mo1 N1 166.06(10) . . ? S3 Mo1 Mo2 97.02(3) . . ? S3 Mo1 Mo3 53.10(3) . . ? S3 Mo1 S1 105.65(4) . . ? S3 Mo1 S11 161.72(4) . . ? S3 Mo1 S12 87.12(4) . . ? S3 Mo1 N1 86.95(10) . . ? S11 Mo1 Mo2 101.16(3) . . ? S11 Mo1 Mo3 140.42(3) . . ? S11 Mo1 S12 78.05(4) . . ? S12 Mo1 Mo2 138.36(3) . . ? S12 Mo1 Mo3 140.19(3) . . ? N1 Mo1 Mo2 140.48(10) . . ? N1 Mo1 Mo3 94.22(10) . . ? N1 Mo1 S1 87.04(10) . . ? N1 Mo1 S11 80.27(10) . . ? N1 Mo1 S12 80.95(10) . . ? Mo3 Mo2 Mo1 60.316(16) . . ? S1 Mo2 Mo1 54.14(3) . . ? S1 Mo2 Mo3 54.07(3) . . ? S1 Mo2 S21 85.49(4) . . ? S1 Mo2 S22 160.83(4) . . ? S1 Mo2 S41 92.09(4) . . ? S2 Mo2 Mo1 52.45(3) . . ? S2 Mo2 Mo3 98.60(3) . . ? S2 Mo2 S1 105.10(4) . . ? S2 Mo2 S4 95.20(4) . . ? S2 Mo2 S21 93.79(4) . . ? S2 Mo2 S22 84.78(4) . . ? S2 Mo2 S41 161.35(5) . . ? S4 Mo2 Mo1 97.43(3) . . ? S4 Mo2 Mo3 53.48(3) . . ? S4 Mo2 S1 106.61(4) . . ? S4 Mo2 S21 162.43(4) . . ? S4 Mo2 S22 88.43(4) . . ? S4 Mo2 S41 86.55(5) . . ? S21 Mo2 Mo1 100.02(3) . . ? S21 Mo2 Mo3 139.49(3) . . ? S21 Mo2 S22 77.38(4) . . ? S21 Mo2 S41 80.19(5) . . ? S22 Mo2 Mo1 137.11(3) . . ? S22 Mo2 Mo3 141.89(3) . . ? S22 Mo2 S41 76.70(4) . . ? S41 Mo2 Mo1 145.81(4) . . ? S41 Mo2 Mo3 97.34(4) . . ? Mo2 Mo3 Mo1 60.197(16) . . ? S1 Mo3 Mo1 54.16(3) . . ? S1 Mo3 Mo2 54.36(3) . . ? S1 Mo3 S31 84.67(4) . . ? S1 Mo3 S32 158.38(4) . . ? S1 Mo3 S42 88.71(5) . . ? S3 Mo3 Mo1 52.93(3) . . ? S3 Mo3 Mo2 97.45(3) . . ? S3 Mo3 S1 105.97(4) . . ? S3 Mo3 S4 93.02(4) . . ? S3 Mo3 S31 95.75(4) . . ? S3 Mo3 S32 87.05(4) . . ? S3 Mo3 S42 164.02(5) . . ? S4 Mo3 Mo1 97.37(4) . . ? S4 Mo3 Mo2 53.52(3) . . ? S4 Mo3 S1 106.94(4) . . ? S4 Mo3 S31 162.93(5) . . ? S4 Mo3 S32 89.12(4) . . ? S4 Mo3 S42 88.57(5) . . ? S31 Mo3 Mo1 99.61(3) . . ? S31 Mo3 Mo2 138.97(3) . . ? S31 Mo3 S32 76.77(4) . . ? S31 Mo3 S42 79.03(5) . . ? S32 Mo3 Mo1 139.61(3) . . ? S32 Mo3 Mo2 142.46(3) . . ? S32 Mo3 S42 77.07(5) . . ? S42 Mo3 Mo1 142.57(4) . . ? S42 Mo3 Mo2 96.27(4) . . ? Mo2 S1 Mo1 71.91(4) . . ? Mo3 S1 Mo1 72.17(3) . . ? Mo3 S1 Mo2 71.57(4) . . ? Mo1 S2 Mo2 74.66(4) . . ? Mo1 S3 Mo3 73.98(4) . . ? Mo3 S4 Mo2 73.00(4) . . ? P11 S11 Mo1 86.66(5) . . ? P11 S12 Mo1 86.09(5) . . ? P21 S21 Mo2 87.78(6) . . ? P21 S22 Mo2 87.34(6) . . ? P31 S31 Mo3 88.59(6) . . ? P31 S32 Mo3 87.75(6) . . ? P41 S41 Mo2 108.14(8) . . ? P41 S42 Mo3 109.85(8) . . ? S11 P11 S12 108.33(7) . . ? O11 P11 S11 114.40(14) . . ? O11 P11 S12 111.36(14) . . ? O11 P11 O12 101.32(18) . . ? O12 P11 S11 107.77(14) . . ? O12 P11 S12 113.61(15) . . ? S22 P21 S21 106.89(8) . . ? O21 P21 S21 114.58(17) . . ? O21 P21 S22 113.00(15) . . ? O21 P21 O22 95.5(2) . . ? O22 P21 S21 112.33(16) . . ? O22 P21 S22 114.55(17) . . ? S32 P31 S31 106.57(8) . . ? O31 P31 S31 111.74(16) . . ? O31 P31 S32 114.62(15) . . ? O31 P31 O32 95.9(2) . . ? O32 P31 S31 113.34(17) . . ? O32 P31 S32 114.70(17) . . ? S42 P41 S41 116.00(10) . . ? O41 P41 S41 113.2(2) . . ? O41 P41 S42 108.7(2) . . ? O42 P41 S41 108.08(19) . . ? O42 P41 S42 108.31(19) . . ? O42 P41 O41 101.4(2) . . ? C11 O11 P11 120.3(3) . . ? C13 O12 P11 120.2(3) . . ? C21 O21 P21 122.4(4) . . ? C23 O22 P21 122.8(4) . . ? C31 O31 P31 120.3(3) . . ? C33 O32 P31 122.7(4) . . ? P41 O41 C41 115.0(4) . . ? C43 O42 P41 119.6(4) . . ? C1 N1 Mo1 120.4(3) . . ? C4 N1 Mo1 123.5(3) . . ? C4 N1 C1 116.2(5) . . ? C3 N2 C4 115.2(5) . . ? N1 C1 H1 118.8 . . ? N1 C1 C2 122.5(5) . . ? C2 C1 H1 118.8 . . ? C1 C2 H2 121.9 . . ? C1 C2 C3 116.3(5) . . ? C3 C2 H2 121.9 . . ? N2 C3 C2 123.3(5) . . ? N2 C3 H3 118.3 . . ? C2 C3 H3 118.3 . . ? N1 C4 N2 126.5(5) . . ? N1 C4 H4 116.7 . . ? N2 C4 H4 116.7 . . ? O11 C11 H11A 110.1 . . ? O11 C11 H11B 110.1 . . ? O11 C11 C12 108.0(4) . . ? H11A C11 H11B 108.4 . . ? C12 C11 H11A 110.1 . . ? C12 C11 H11B 110.1 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O12 C13 H13A 110.2 . . ? O12 C13 H13B 110.2 . . ? O12 C13 C14 107.5(4) . . ? H13A C13 H13B 108.5 . . ? C14 C13 H13A 110.2 . . ? C14 C13 H13B 110.2 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14B 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O21 C21 H21A 109.4 . . ? O21 C21 H21B 109.4 . . ? O21 C21 C22 111.2(5) . . ? H21A C21 H21B 108.0 . . ? C22 C21 H21A 109.4 . . ? C22 C21 H21B 109.4 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22B 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O22 C23 H23A 110.2 . . ? O22 C23 H23B 110.2 . . ? O22 C23 C24 107.4(5) . . ? H23A C23 H23B 108.5 . . ? C24 C23 H23A 110.2 . . ? C24 C23 H23B 110.2 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O31 C31 H31A 109.9 . . ? O31 C31 H31B 109.9 . . ? O31 C31 C32 108.8(5) . . ? H31A C31 H31B 108.3 . . ? C32 C31 H31A 109.9 . . ? C32 C31 H31B 109.9 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32B 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? O32 C33 H33A 109.8 . . ? O32 C33 H33B 109.8 . . ? O32 C33 C34 109.2(7) . . ? H33A C33 H33B 108.3 . . ? C34 C33 H33A 109.8 . . ? C34 C33 H33B 109.8 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34B 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? O42 C43 H43A 110.0 . . ? O42 C43 H43B 110.0 . . ? O42 C43 C44 108.5(5) . . ? H43A C43 H43B 108.4 . . ? C44 C43 H43A 110.0 . . ? C44 C43 H43B 110.0 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44B 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? O41 C41 H41A 114.0 . . ? O41 C41 H41B 114.3 . . ? H41A C41 H41B 111.3 . . ? C42 C41 O41 86.4(11) . . ? C42 C41 H41A 114.3 . . ? C42 C41 H41B 114.5 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42B 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Mo1 N1 C1 C2 177.9(4) . . . . ? Mo1 N1 C4 N2 -178.3(4) . . . . ? S11 P11 O11 C11 -62.9(4) . . . . ? S11 P11 O12 C13 -178.3(3) . . . . ? S12 P11 O11 C11 60.3(4) . . . . ? S12 P11 O12 C13 61.7(4) . . . . ? S21 P21 O21 C21 -77.4(4) . . . . ? S21 P21 O22 C23 44.1(5) . . . . ? S22 P21 O21 C21 45.4(5) . . . . ? S22 P21 O22 C23 -78.1(4) . . . . ? S31 P31 O31 C31 -59.2(4) . . . . ? S31 P31 O32 C33 73.7(5) . . . . ? S32 P31 O31 C31 62.1(4) . . . . ? S32 P31 O32 C33 -49.0(6) . . . . ? S41 P41 O41 C41 53.7(5) . . . . ? S41 P41 O42 C43 60.5(5) . . . . ? S42 P41 O41 C41 -175.8(4) . . . . ? S42 P41 O42 C43 -66.0(5) . . . . ? P11 O11 C11 C12 -178.6(4) . . . . ? P11 O12 C13 C14 -156.8(4) . . . . ? P21 O21 C21 C22 110.6(6) . . . . ? P21 O22 C23 C24 -157.8(4) . . . . ? P31 O31 C31 C32 174.4(4) . . . . ? P31 O32 C33 C34 -163.2(6) . . . . ? P41 O41 C41 C42 -119.3(6) . . . . ? P41 O42 C43 C44 147.2(5) . . . . ? O11 P11 O12 C13 -57.8(4) . . . . ? O12 P11 O11 C11 -178.5(3) . . . . ? O21 P21 O22 C23 163.6(4) . . . . ? O22 P21 O21 C21 165.0(4) . . . . ? O31 P31 O32 C33 -169.6(5) . . . . ? O32 P31 O31 C31 -177.2(4) . . . . ? O41 P41 O42 C43 179.8(5) . . . . ? O42 P41 O41 C41 -61.8(5) . . . . ? N1 C1 C2 C3 0.9(8) . . . . ? C1 N1 C4 N2 1.5(8) . . . . ? C1 C2 C3 N2 0.6(9) . . . . ? C3 N2 C4 N1 -0.1(8) . . . . ? C4 N1 C1 C2 -1.8(7) . . . . ? C4 N2 C3 C2 -1.0(9) . . . . ? loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 0 1 -1 0.0298 -0.0014 0.9995 -0.9983 0.0144 0.0564 -0.0206 0 -1 1 0.0298 0.0014 -0.9995 0.9983 -0.0144 -0.0564 0.0206 0 0 1 0.0446 0.0024 -0.0006 0.9975 -0.0022 -0.0119 0.0592 0 0 -1 0.0446 -0.0024 0.0006 -0.9975 0.0022 0.0119 -0.0592 -1 0 0 0.1145 -1.0012 -0.0000 0.0015 -0.0523 0.0040 -0.0312 1 0 0 0.0814 1.0012 0.0000 -0.0015 0.0523 -0.0040 0.0312 -13 8 -9 0.0846 -13.0286 7.9958 -8.9645 -0.5625 0.5152 -0.6299 _database_code_depnum_ccdc_archive 'CCDC 920389' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_Sample4 _audit_creation_date 2013-05-31 _audit_creation_method ; Olex2 1.2-ac2 (compiled 2012.03.27 svn.r2268, GUI svn.r4156) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C18 H37 N2 O8 P3 S10 W3' _chemical_formula_sum 'C18 H37 N2 O8 P3 S10 W3' _chemical_formula_weight 1374.47 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.7100(10) _cell_length_b 13.8890(10) _cell_length_c 15.5870(10) _cell_angle_alpha 67.1580(10) _cell_angle_beta 82.4680(10) _cell_angle_gamma 81.6230(10) _cell_volume 2106.9(3) _cell_formula_units_Z 2 _cell_measurement_reflns_used ? _cell_measurement_temperature 293(2) _cell_measurement_theta_max 3.02 _cell_measurement_theta_min 25.3 _exptl_absorpt_coefficient_mu 8.817 _exptl_absorpt_correction_T_max 0.643 _exptl_absorpt_correction_T_min 0.401 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS - Bruker Nonius area detector scaling and absorption correction - V2.10 ; _exptl_crystal_colour 'dark brown' _exptl_crystal_density_diffrn 2.167 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 1300 _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.05 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0544 _diffrn_reflns_av_unetI/netI 0.0661 _diffrn_reflns_Laue_measured_fraction_full 0.983 _diffrn_reflns_Laue_measured_fraction_max 0.983 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 27847 _diffrn_reflns_point_group_measured_fraction_full 0.983 _diffrn_reflns_point_group_measured_fraction_max 0.983 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.349 _diffrn_reflns_theta_min 2.345 _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.983 _diffrn_measured_fraction_theta_max 0.983 _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source ? _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 6474 _reflns_number_total 7583 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement ? _computing_data_collection ? _computing_data_reduction ? _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; SHELXL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution ; M.C.Burla, R.Caliandro, M.Camalli, B.Carrozzini, G.L.Cascarano, C.Giacovazzo, M.Mallamo, A.Mazzone, G.Polidori and R. Spagna SIR2011: a new package for crystal structure determination and refinement J. Appl. Cryst. (2012). 45, 357-361. ; _refine_diff_density_max 1.628 _refine_diff_density_min -1.554 _refine_diff_density_rms 0.245 _refine_ls_extinction_coef 0.0070(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.221 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 410 _refine_ls_number_reflns 7583 _refine_ls_number_restraints 35 _refine_ls_R_factor_all 0.0575 _refine_ls_R_factor_gt 0.0470 _refine_ls_restrained_S_all 1.223 _refine_ls_shift/su_max 0.105 _refine_ls_shift/su_mean 0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0449P)^2^+6.8208P] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1296 _refine_ls_wR_factor_ref 0.1369 _refine_special_details ; ? ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.26775(4) 0.82197(3) 0.19680(3) 0.05372(17) Uani 1 1 d . . . . . W2 W 0.30012(3) 0.70226(3) 0.08853(3) 0.04649(16) Uani 1 1 d . . . . . S32 S 0.1930(3) 0.4533(2) 0.3313(2) 0.0788(9) Uani 1 1 d . . . . . P31 P 0.3224(5) 0.3760(3) 0.4239(3) 0.0942(12) Uani 1 1 d D . . . . S3 S 0.4309(3) 0.7333(2) 0.2916(3) 0.0743(8) Uani 1 1 d . . . . . S1 S 0.1319(2) 0.70161(18) 0.20199(19) 0.0513(6) Uani 1 1 d . . . . . S2 S 0.3907(2) 0.8534(2) 0.0585(2) 0.0622(7) Uani 1 1 d . . . . . S21 S 0.1383(2) 0.7914(2) -0.0316(2) 0.0592(6) Uani 1 1 d . . . . . S12 S 0.3351(3) 0.9870(2) 0.2040(3) 0.0856(10) Uani 1 1 d . . . . . S31 S 0.4509(4) 0.4738(3) 0.4026(3) 0.1007(12) Uani 1 1 d . . . . . S22 S 0.4246(2) 0.6994(2) -0.0630(2) 0.0664(7) Uani 1 1 d . . . . . S11 S 0.0835(2) 0.9555(2) 0.1334(2) 0.0633(7) Uani 1 1 d . . . . . S4 S 0.4578(2) 0.5794(2) 0.1666(2) 0.0618(7) Uani 1 1 d . . . . . P11 P 0.1742(3) 1.0627(2) 0.1499(2) 0.0665(8) Uani 1 1 d D . . . . P21 P 0.2704(3) 0.7739(2) -0.1289(2) 0.0673(8) Uani 1 1 d D . . . . O42 O 0.2007(9) 0.6324(6) 0.4019(6) 0.083(2) Uani 1 1 d . . . . . O21 O 0.2912(9) 0.8825(7) -0.2119(6) 0.095(3) Uani 1 1 d D . . . . O12 O 0.0924(9) 1.1213(6) 0.2101(7) 0.088(3) Uani 1 1 d D . . . . O31 O 0.2623(15) 0.3334(8) 0.5266(7) 0.129(4) Uani 1 1 d D . . . . O22 O 0.2277(11) 0.7186(8) -0.1879(8) 0.117(4) Uani 1 1 d D . . . . O11 O 0.1923(7) 1.1622(5) 0.0577(6) 0.074(2) Uani 1 1 d D . . . . N2 N 0.0334(9) 0.4676(7) 0.1044(8) 0.078(3) Uani 1 1 d . . . . . O41 O 0.1601(8) 0.8087(7) 0.3306(6) 0.078(2) Uani 1 1 d . . . . . O32 O 0.3736(14) 0.2657(8) 0.4187(9) 0.129(7) Uani 0.99(4) 1 d D . . . . N1 N 0.2155(7) 0.5555(6) 0.0869(6) 0.0526(19) Uani 1 1 d . . . . . C23 C 0.2521(15) 0.6153(11) -0.1783(13) 0.119(6) Uani 1 1 d D . . . . H23A H 0.1996 0.5728 -0.1255 0.143 Uiso 1 1 calc R U . . . H23B H 0.3400 0.5913 -0.1662 0.143 Uiso 1 1 calc R U . . . C24 C 0.2272(18) 0.6028(18) -0.2600(14) 0.149(8) Uani 1 1 d D . . . . H24A H 0.2412 0.6660 -0.3132 0.224 Uiso 1 1 calc R U . . . H24B H 0.1407 0.5888 -0.2548 0.224 Uiso 1 1 calc R U . . . H24C H 0.2825 0.5452 -0.2674 0.224 Uiso 1 1 calc R U . . . C21 C 0.3163(18) 0.9731(10) -0.1979(12) 0.125(6) Uani 1 1 d D . . . . H21A H 0.2550 0.9841 -0.1501 0.150 Uiso 1 1 calc R U . . . H21B H 0.3997 0.9605 -0.1753 0.150 Uiso 1 1 calc R U . . . C22 C 0.311(3) 1.0643(14) -0.2793(15) 0.187(11) Uani 1 1 d D . . . . H22A H 0.3730 1.0545 -0.3265 0.281 Uiso 1 1 calc R U . . . H22B H 0.3288 1.1226 -0.2659 0.281 Uiso 1 1 calc R U . . . H22C H 0.2283 1.0781 -0.3013 0.281 Uiso 1 1 calc R U . . . C31 C 0.228(4) 0.4091(18) 0.5680(15) 0.26(2) Uani 1 1 d D . . . . H31A H 0.3054 0.4313 0.5774 0.309 Uiso 1 1 calc R U . . . H31B H 0.1827 0.4700 0.5239 0.309 Uiso 1 1 calc R U . . . C32 C 0.159(3) 0.379(2) 0.647(2) 0.227(16) Uani 1 1 d D . . . . H32A H 0.0935 0.4345 0.6473 0.341 Uiso 1 1 calc R U . . . H32B H 0.2113 0.3646 0.6975 0.341 Uiso 1 1 calc R U . . . H32C H 0.1216 0.3173 0.6557 0.341 Uiso 1 1 calc R U . . . C13 C 0.045(2) 1.0644(11) 0.3045(9) 0.128(7) Uani 1 1 d D . . . . H13A H -0.0353 1.0404 0.3033 0.154 Uiso 1 1 calc R U . . . H13B H 0.1036 1.0027 0.3318 0.154 Uiso 1 1 calc R U . . . C14 C 0.027(4) 1.121(2) 0.361(2) 0.29(2) Uani 1 1 d D . . . . H14A H 0.0944 1.1653 0.3456 0.437 Uiso 1 1 calc R U . . . H14B H 0.0281 1.0738 0.4248 0.437 Uiso 1 1 calc R U . . . H14C H -0.0525 1.1635 0.3508 0.437 Uiso 1 1 calc R U . . . C11 C 0.2586(15) 1.1515(10) -0.0238(9) 0.107(5) Uani 1 1 d D . . . . H11A H 0.3444 1.1199 -0.0106 0.128 Uiso 1 1 calc R U . . . H11B H 0.2171 1.1055 -0.0420 0.128 Uiso 1 1 calc R U . . . C12 C 0.262(2) 1.2492(13) -0.0966(13) 0.140(7) Uani 1 1 d D . . . . H12A H 0.2612 1.2411 -0.1550 0.210 Uiso 1 1 calc R U . . . H12B H 0.3369 1.2790 -0.0965 0.210 Uiso 1 1 calc R U . . . H12C H 0.1885 1.2949 -0.0885 0.210 Uiso 1 1 calc R U . . . C41 C 0.1542(14) 0.7214(12) 0.4018(10) 0.087(4) Uani 1 1 d . . . . . C42 C 0.085(2) 0.7274(13) 0.4872(12) 0.129(7) Uani 1 1 d . . . . . H42A H 0.0770 0.6578 0.5325 0.193 Uiso 1 1 calc R U . . . H42B H 0.0026 0.7641 0.4734 0.193 Uiso 1 1 calc R U . . . H42C H 0.1307 0.7645 0.5117 0.27(16) Uani 1 1 calc R . . . . C4 C 0.0912(9) 0.5483(8) 0.0996(8) 0.063(3) Uani 1 1 d . . . . . H4 H 0.0396 0.6055 0.1058 0.075 Uiso 1 1 calc R U . . . C1 C 0.2869(10) 0.4725(7) 0.0778(9) 0.065(3) Uani 1 1 d . . . . . H1 H 0.3743 0.4737 0.0680 0.078 Uiso 1 1 calc R U . . . C2 C 0.2364(12) 0.3860(8) 0.0825(10) 0.081(4) Uani 1 1 d . . . . . H2 H 0.2880 0.3284 0.0772 0.097 Uiso 1 1 calc R U . . . C3 C 0.1105(13) 0.3863(9) 0.0951(11) 0.087(4) Uani 1 1 d . . . . . H3 H 0.0750 0.3280 0.0975 0.104 Uiso 1 1 calc R U . . . W3 W 0.31425(4) 0.61189(3) 0.27870(3) 0.05916(17) Uani 1 1 d . . . . . C33 C 0.435(4) 0.254(2) 0.338(2) 0.30(2) Uani 1 1 d D U . . . H33A H 0.3955 0.3048 0.2835 0.360 Uiso 1 1 calc R U . . . H33B H 0.5231 0.2652 0.3324 0.360 Uiso 1 1 calc R U . . . C34 C 0.423(5) 0.152(2) 0.346(4) 0.42(3) Uani 1 1 d D U . . . H34A H 0.4611 0.1028 0.4013 0.635 Uiso 1 1 calc R U . . . H34B H 0.4655 0.1409 0.2922 0.635 Uiso 1 1 calc R U . . . H34C H 0.3352 0.1425 0.3510 0.635 Uiso 1 1 calc R U . . . 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 W1 0.0480(2) 0.0449(2) 0.0816(3) -0.0384(2) -0.0108(2) 0.00009(16) W2 0.0355(2) 0.0402(2) 0.0714(3) -0.03093(19) -0.00476(17) 0.00106(14) S32 0.106(2) 0.0552(16) 0.078(2) -0.0246(14) -0.0095(17) -0.0166(15) P31 0.152(4) 0.0563(18) 0.074(2) -0.0251(16) -0.026(2) 0.008(2) S3 0.0724(18) 0.0627(16) 0.107(2) -0.0476(17) -0.0363(16) 0.0053(13) S1 0.0442(12) 0.0481(12) 0.0706(16) -0.0335(12) 0.0003(11) -0.0051(10) S2 0.0456(13) 0.0494(13) 0.098(2) -0.0362(14) 0.0015(13) -0.0083(10) S21 0.0451(13) 0.0562(14) 0.0761(18) -0.0271(13) -0.0103(12) 0.0067(10) S12 0.0775(19) 0.0616(17) 0.146(3) -0.064(2) -0.037(2) -0.0007(14) S31 0.132(3) 0.079(2) 0.098(3) -0.036(2) -0.058(2) 0.020(2) S22 0.0495(14) 0.0704(17) 0.085(2) -0.0423(15) 0.0072(13) 0.0031(12) S11 0.0506(13) 0.0496(13) 0.100(2) -0.0412(14) -0.0113(13) 0.0036(11) S4 0.0500(13) 0.0525(14) 0.092(2) -0.0384(14) -0.0220(13) 0.0126(11) P11 0.0699(17) 0.0483(14) 0.095(2) -0.0440(15) -0.0056(15) -0.0021(12) P21 0.0732(18) 0.0562(16) 0.075(2) -0.0330(14) -0.0027(15) 0.0068(13) O42 0.119(7) 0.055(4) 0.087(6) -0.040(4) -0.020(5) -0.002(4) O21 0.115(7) 0.076(6) 0.076(6) -0.019(5) 0.006(5) 0.007(5) O12 0.101(6) 0.067(5) 0.112(7) -0.057(5) -0.001(5) 0.005(4) O31 0.240(14) 0.073(6) 0.068(6) -0.023(5) -0.006(7) -0.012(7) O22 0.161(10) 0.092(7) 0.128(9) -0.076(6) -0.080(7) 0.053(6) O11 0.077(5) 0.049(4) 0.104(6) -0.043(4) 0.003(4) -0.002(3) N2 0.060(5) 0.062(6) 0.125(9) -0.044(6) -0.015(5) -0.013(4) O41 0.090(6) 0.072(5) 0.083(6) -0.043(5) -0.012(4) -0.002(4) O32 0.200(14) 0.073(7) 0.119(10) -0.051(6) -0.038(9) 0.035(7) N1 0.052(5) 0.045(4) 0.070(5) -0.031(4) -0.010(4) -0.002(3) C23 0.087(10) 0.125(13) 0.168(18) -0.078(13) -0.047(11) 0.015(9) C24 0.124(14) 0.23(2) 0.170(19) -0.165(19) 0.000(13) -0.018(14) C21 0.136(14) 0.082(10) 0.144(16) -0.020(10) -0.009(12) -0.043(10) C22 0.27(3) 0.085(13) 0.17(2) -0.002(13) 0.00(2) -0.036(16) C31 0.48(6) 0.19(3) 0.100(17) -0.081(18) 0.03(3) 0.03(3) C32 0.27(4) 0.18(3) 0.21(3) -0.09(2) 0.10(3) 0.00(2) C13 0.200(19) 0.088(10) 0.085(11) -0.041(9) 0.015(12) 0.019(11) C14 0.52(7) 0.23(3) 0.16(2) -0.16(3) -0.03(3) 0.09(4) C11 0.108(11) 0.077(9) 0.113(12) -0.027(9) 0.028(9) 0.001(8) C12 0.155(17) 0.115(14) 0.122(15) -0.037(12) 0.035(13) 0.007(12) C41 0.106(10) 0.092(10) 0.076(9) -0.043(8) -0.007(7) -0.014(8) C42 0.22(2) 0.095(11) 0.089(11) -0.060(9) 0.002(12) -0.012(12) H42C 0.4(3) 0.4(3) 0.2(2) -0.3(2) 0.1(2) -0.2(3) C4 0.054(6) 0.053(6) 0.092(8) -0.039(6) -0.015(5) 0.000(4) C1 0.055(6) 0.047(5) 0.105(9) -0.041(6) -0.023(6) 0.008(4) C2 0.077(8) 0.044(6) 0.136(12) -0.048(7) -0.036(7) 0.012(5) C3 0.090(9) 0.045(6) 0.143(12) -0.046(7) -0.033(8) -0.010(6) W3 0.0673(3) 0.0466(3) 0.0726(3) -0.0310(2) -0.0182(2) 0.00174(18) C33 0.38(4) 0.14(2) 0.39(4) -0.16(3) 0.21(4) -0.09(2) C34 0.49(5) 0.19(3) 0.54(6) -0.16(4) 0.30(5) -0.11(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 W1 W2 2.7550(5) . ? W1 S3 2.321(3) . ? W1 S1 2.343(2) . ? W1 S2 2.294(3) . ? W1 S12 2.547(3) . ? W1 S11 2.517(3) . ? W1 O41 2.202(9) . ? W1 W3 2.6913(6) . ? W2 S1 2.352(2) . ? W2 S2 2.297(2) . ? W2 S21 2.543(3) . ? W2 S22 2.567(3) . ? W2 S4 2.310(3) . ? W2 N1 2.359(7) . ? W2 W3 2.7492(6) . ? S32 P31 2.012(5) . ? S32 W3 2.522(3) . ? P31 S31 1.981(6) . ? P31 O31 1.559(11) . ? P31 O32 1.579(10) . ? S3 W3 2.321(3) . ? S1 W3 2.355(3) . ? S21 P21 1.995(4) . ? S12 P11 1.988(4) . ? S31 W3 2.568(4) . ? S22 P21 1.994(4) . ? S11 P11 2.002(4) . ? S4 W3 2.308(3) . ? P11 O12 1.575(8) . ? P11 O11 1.573(9) . ? P21 O21 1.583(9) . ? P21 O22 1.550(9) . ? O42 C41 1.263(15) . ? O42 W3 2.227(9) . ? O21 C21 1.425(13) . ? O12 C13 1.438(13) . ? O31 C31 1.417(15) . ? O22 C23 1.373(13) . ? O11 C11 1.421(12) . ? N2 C4 1.330(12) . ? N2 C3 1.342(15) . ? O41 C41 1.289(16) . ? O32 C33 1.391(17) . ? N1 C4 1.332(12) . ? N1 C1 1.332(12) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 C24 1.412(15) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 C22 1.403(16) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C31 C32 1.304(17) . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C13 C14 1.364(15) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C11 C12 1.393(14) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C41 C42 1.46(2) . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C4 H4 0.9300 . ? C1 H1 0.9300 . ? C1 C2 1.360(14) . ? C2 H2 0.9300 . ? C2 C3 1.336(17) . ? C3 H3 0.9300 . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C33 C34 1.394(18) . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 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 S3 W1 W2 97.12(7) . . ? S3 W1 S1 109.22(10) . . ? S3 W1 S12 85.30(11) . . ? S3 W1 S11 158.55(10) . . ? S3 W1 W3 54.57(7) . . ? S1 W1 W2 54.21(6) . . ? S1 W1 S12 158.36(10) . . ? S1 W1 S11 83.71(8) . . ? S1 W1 W3 55.25(6) . . ? S2 W1 W2 53.17(6) . . ? S2 W1 S3 95.45(12) . . ? S2 W1 S1 105.03(9) . . ? S2 W1 S12 88.91(12) . . ? S2 W1 S11 97.58(10) . . ? S2 W1 W3 100.82(6) . . ? S12 W1 W2 142.08(10) . . ? S12 W1 W3 139.19(8) . . ? S11 W1 W2 104.32(7) . . ? S11 W1 S12 78.01(9) . . ? S11 W1 W3 138.07(6) . . ? O41 W1 W2 134.1(2) . . ? O41 W1 S3 83.2(3) . . ? O41 W1 S1 82.1(2) . . ? O41 W1 S2 172.7(2) . . ? O41 W1 S12 83.8(2) . . ? O41 W1 S11 81.7(2) . . ? O41 W1 W3 84.3(2) . . ? W3 W1 W2 60.621(15) . . ? S1 W2 W1 53.93(5) . . ? S1 W2 S21 86.42(9) . . ? S1 W2 S22 161.40(9) . . ? S1 W2 N1 84.4(2) . . ? S1 W2 W3 54.30(7) . . ? S2 W2 W1 53.08(7) . . ? S2 W2 S1 104.68(9) . . ? S2 W2 S21 94.36(10) . . ? S2 W2 S22 85.94(10) . . ? S2 W2 S4 99.61(10) . . ? S2 W2 N1 168.5(2) . . ? S2 W2 W3 99.07(8) . . ? S21 W2 W1 103.88(6) . . ? S21 W2 S22 77.45(9) . . ? S21 W2 W3 140.52(6) . . ? S22 W2 W1 139.01(7) . . ? S22 W2 W3 140.15(7) . . ? S4 W2 W1 98.03(7) . . ? S4 W2 S1 106.06(10) . . ? S4 W2 S21 158.06(9) . . ? S4 W2 S22 86.71(11) . . ? S4 W2 N1 84.3(2) . . ? S4 W2 W3 53.44(8) . . ? N1 W2 W1 137.4(2) . . ? N1 W2 S21 79.0(2) . . ? N1 W2 S22 83.5(2) . . ? N1 W2 W3 91.9(2) . . ? W3 W2 W1 58.542(15) . . ? P31 S32 W3 88.13(17) . . ? S31 P31 S32 106.4(2) . . ? O31 P31 S32 112.6(6) . . ? O31 P31 S31 113.5(5) . . ? O31 P31 O32 96.8(6) . . ? O32 P31 S32 111.3(5) . . ? O32 P31 S31 116.2(6) . . ? W3 S3 W1 70.86(8) . . ? W1 S1 W2 71.85(7) . . ? W1 S1 W3 69.90(7) . . ? W2 S1 W3 71.48(7) . . ? W1 S2 W2 73.75(8) . . ? P21 S21 W2 88.31(13) . . ? P11 S12 W1 87.70(12) . . ? P31 S31 W3 87.52(18) . . ? P21 S22 W2 87.67(12) . . ? P11 S11 W1 88.25(13) . . ? W3 S4 W2 73.07(7) . . ? S12 P11 S11 106.02(16) . . ? O12 P11 S12 113.3(4) . . ? O12 P11 S11 113.1(4) . . ? O11 P11 S12 114.1(3) . . ? O11 P11 S11 113.3(3) . . ? O11 P11 O12 97.2(4) . . ? S22 P21 S21 106.54(19) . . ? O21 P21 S21 111.6(4) . . ? O21 P21 S22 114.7(4) . . ? O22 P21 S21 113.9(5) . . ? O22 P21 S22 113.2(4) . . ? O22 P21 O21 97.0(6) . . ? C41 O42 W3 122.5(9) . . ? C21 O21 P21 123.1(9) . . ? C13 O12 P11 121.1(8) . . ? C31 O31 P31 115.5(12) . . ? C23 O22 P21 129.0(9) . . ? C11 O11 P11 120.4(7) . . ? C4 N2 C3 115.2(9) . . ? C41 O41 W1 123.6(8) . . ? C33 O32 P31 123.2(14) . . ? C4 N1 W2 121.4(6) . . ? C4 N1 C1 115.3(8) . . ? C1 N1 W2 123.2(6) . . ? O22 C23 H23A 109.5 . . ? O22 C23 H23B 109.5 . . ? O22 C23 C24 110.8(15) . . ? H23A C23 H23B 108.1 . . ? C24 C23 H23A 109.5 . . ? C24 C23 H23B 109.5 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O21 C21 H21A 109.0 . . ? O21 C21 H21B 109.0 . . ? H21A C21 H21B 107.8 . . ? C22 C21 O21 113.0(16) . . ? C22 C21 H21A 109.0 . . ? C22 C21 H21B 109.0 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22B 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O31 C31 H31A 108.2 . . ? O31 C31 H31B 108.2 . . ? H31A C31 H31B 107.3 . . ? C32 C31 O31 116(2) . . ? C32 C31 H31A 108.2 . . ? C32 C31 H31B 108.2 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32B 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? O12 C13 H13A 108.7 . . ? O12 C13 H13B 108.7 . . ? H13A C13 H13B 107.6 . . ? C14 C13 O12 114.4(19) . . ? C14 C13 H13A 108.7 . . ? C14 C13 H13B 108.7 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14B 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O11 C11 H11A 109.6 . . ? O11 C11 H11B 109.6 . . ? H11A C11 H11B 108.1 . . ? C12 C11 O11 110.3(12) . . ? C12 C11 H11A 109.6 . . ? C12 C11 H11B 109.6 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O42 C41 O41 124.9(12) . . ? O42 C41 C42 118.5(14) . . ? O41 C41 C42 116.6(13) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42B 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? N2 C4 N1 126.7(9) . . ? N2 C4 H4 116.6 . . ? N1 C4 H4 116.6 . . ? N1 C1 H1 118.9 . . ? N1 C1 C2 122.3(10) . . ? C2 C1 H1 118.9 . . ? C1 C2 H2 121.0 . . ? C3 C2 C1 118.1(10) . . ? C3 C2 H2 121.0 . . ? N2 C3 H3 118.7 . . ? C2 C3 N2 122.5(10) . . ? C2 C3 H3 118.7 . . ? W1 W3 W2 60.837(14) . . ? S32 W3 W1 137.87(9) . . ? S32 W3 W2 104.75(8) . . ? S32 W3 S31 77.82(13) . . ? S3 W3 W1 54.57(8) . . ? S3 W3 W2 97.28(9) . . ? S3 W3 S32 157.96(12) . . ? S3 W3 S1 108.82(9) . . ? S3 W3 S31 85.57(12) . . ? S1 W3 W1 54.86(5) . . ? S1 W3 W2 54.21(6) . . ? S1 W3 S32 84.05(10) . . ? S1 W3 S31 159.00(13) . . ? S31 W3 W1 139.58(9) . . ? S31 W3 W2 141.18(10) . . ? S4 W3 W1 99.88(7) . . ? S4 W3 W2 53.48(7) . . ? S4 W3 S32 100.20(10) . . ? S4 W3 S3 93.44(11) . . ? S4 W3 S1 106.01(9) . . ? S4 W3 S31 87.74(13) . . ? O42 W3 W1 84.6(2) . . ? O42 W3 W2 135.1(2) . . ? O42 W3 S32 81.3(2) . . ? O42 W3 S3 82.6(2) . . ? O42 W3 S1 83.1(2) . . ? O42 W3 S31 83.7(3) . . ? O42 W3 S4 170.8(3) . . ? O32 C33 H33A 110.3 . . ? O32 C33 H33B 110.3 . . ? H33A C33 H33B 108.5 . . ? C34 C33 O32 107(2) . . ? C34 C33 H33A 110.3 . . ? C34 C33 H33B 110.3 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34B 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? _database_code_depnum_ccdc_archive 'CCDC 920390' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_Sample5 _audit_creation_date 2013-05-31 _audit_creation_method ; Olex2 1.2-ac2 (compiled 2012.03.27 svn.r2268, GUI svn.r4156) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C14 H34 Mo3 O9 P3 S10, C12 H12 N2, C2 H6 O' _chemical_formula_sum 'C28 H52 Mo3 N2 O10 P3 S10' _chemical_formula_weight 1278.04 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -0.0483 2.7339 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.8385(4) _cell_length_b 13.8201(6) _cell_length_c 14.9195(6) _cell_angle_alpha 104.542(4) _cell_angle_beta 93.902(3) _cell_angle_gamma 108.054(4) _cell_volume 2405.41(18) _cell_formula_units_Z 2 _cell_measurement_reflns_used 21934 _cell_measurement_temperature 100.00(10) _cell_measurement_theta_max 73.6655 _cell_measurement_theta_min 3.6675 _exptl_absorpt_coefficient_mu 11.730 _exptl_absorpt_correction_T_max 0.406 _exptl_absorpt_correction_T_min 0.116 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_crystal_colour 'dark brown' _exptl_crystal_density_diffrn 1.765 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 1290 _exptl_crystal_size_max 0.297 _exptl_crystal_size_mid 0.2004 _exptl_crystal_size_min 0.1197 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0373 _diffrn_reflns_av_unetI/netI 0.0233 _diffrn_reflns_Laue_measured_fraction_full 0.976 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 34841 _diffrn_reflns_point_group_measured_fraction_full 0.976 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 66.594 _diffrn_reflns_theta_min 3.667 _diffrn_ambient_temperature 100.0 _diffrn_detector_area_resol_mean 10.5953 _diffrn_measured_fraction_theta_full 0.9997 _diffrn_measured_fraction_theta_max 0.9826 _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0304238000 _diffrn_orient_matrix_UB_12 -0.0761572000 _diffrn_orient_matrix_UB_13 0.0481727000 _diffrn_orient_matrix_UB_21 0.0357858000 _diffrn_orient_matrix_UB_22 0.0881633000 _diffrn_orient_matrix_UB_23 0.0941133000 _diffrn_orient_matrix_UB_31 -0.1188824000 _diffrn_orient_matrix_UB_32 -0.0375103000 _diffrn_orient_matrix_UB_33 0.0222468000 _diffrn_radiation_monochromator mirror _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.5418 _diffrn_source 'SuperNova (Cu) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 8057 _reflns_number_total 8499 _reflns_odcompleteness_completeness 99.97 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; SHELXL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution ; M.C.Burla, R.Caliandro, M.Camalli, B.Carrozzini, G.L.Cascarano, C.Giacovazzo, M.Mallamo, A.Mazzone, G.Polidori and R. Spagna SIR2011: a new package for crystal structure determination and refinement J. Appl. Cryst. (2012). 45, 357-361. ; _refine_diff_density_max 1.113 _refine_diff_density_min -0.742 _refine_diff_density_rms 0.101 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.991 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 524 _refine_ls_number_reflns 8499 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0305 _refine_ls_R_factor_gt 0.0290 _refine_ls_restrained_S_all 0.991 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0546P)^2^+3.1970P] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0797 _refine_ls_wR_factor_ref 0.0814 _refine_special_details ; ? ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.31850(2) 0.81315(2) 0.36614(2) 0.01647(7) Uani 1 1 d . . . . . Mo2 Mo 0.39359(2) 0.85674(2) 0.20687(2) 0.01864(7) Uani 1 1 d . . . . . Mo3 Mo 0.29731(2) 0.98291(2) 0.31120(2) 0.01812(7) Uani 1 1 d . . . . . S1 S 0.20878(6) 0.80319(5) 0.23062(5) 0.01735(14) Uani 1 1 d . . . . . S2 S 0.48974(6) 0.82171(6) 0.32302(5) 0.02115(15) Uani 1 1 d . . . . . S3 S 0.36699(6) 0.98432(5) 0.45712(5) 0.02057(15) Uani 1 1 d . . . . . S4 S 0.46875(6) 1.03849(6) 0.26754(5) 0.02310(15) Uani 1 1 d . . . . . S11 S 0.37985(6) 0.77222(6) 0.51592(5) 0.02195(15) Uani 1 1 d . . . . . S12 S 0.13572(6) 0.75115(6) 0.42534(5) 0.02066(15) Uani 1 1 d . . . . . S21 S 0.56368(7) 0.87431(6) 0.12404(6) 0.02892(17) Uani 1 1 d . . . . . S22 S 0.33394(6) 0.68015(6) 0.08150(5) 0.02239(15) Uani 1 1 d . . . . . S31 S 0.32910(6) 1.18142(6) 0.37709(6) 0.02633(16) Uani 1 1 d . . . . . S32 S 0.10522(6) 0.98183(6) 0.34345(5) 0.02237(15) Uani 1 1 d . . . . . P11 P 0.22181(6) 0.73667(6) 0.53537(5) 0.02032(15) Uani 1 1 d . . . . . P21 P 0.48148(7) 0.72901(6) 0.03988(5) 0.02364(16) Uani 1 1 d . . . . . P31 P 0.16967(7) 1.14048(6) 0.39094(5) 0.02297(16) Uani 1 1 d . . . . . O1 O 0.27154(17) 0.63595(16) 0.30777(14) 0.0216(4) Uani 1 1 d . . . . . H1 H 0.2298 0.6092 0.2718 0.032 Uiso 1 1 d R U . . . O11 O 0.17290(18) 0.62461(17) 0.55372(15) 0.0260(5) Uani 1 1 d . . . . . O12 O 0.20485(18) 0.80538(17) 0.63187(14) 0.0246(4) Uani 1 1 d . . . . . O21 O 0.4756(2) 0.72506(19) -0.06715(15) 0.0317(5) Uani 1 1 d . . . . . O22 O 0.54586(19) 0.64804(18) 0.03677(15) 0.0278(5) Uani 1 1 d . . . . . O31 O 0.10441(19) 1.19807(18) 0.34236(16) 0.0290(5) Uani 1 1 d . . . . . O32 O 0.1483(2) 1.18691(17) 0.49352(15) 0.0288(5) Uani 1 1 d . . . . . O41 O 0.32167(18) 0.89905(17) 0.08831(14) 0.0248(4) Uani 1 1 d . . . . . O42 O 0.23820(18) 1.00235(16) 0.17489(14) 0.0232(4) Uani 1 1 d . . . . . C11 C 0.1639(3) 0.5283(3) 0.4811(2) 0.0297(7) Uani 1 1 d . . . . . H11A H 0.2373 0.5324 0.4624 0.036 Uiso 1 1 calc R U . . . H11B H 0.1120 0.5194 0.4251 0.036 Uiso 1 1 calc R U . . . C12 C 0.1217(3) 0.4361(3) 0.5207(3) 0.0390(8) Uani 1 1 d . . . . . H12A H 0.0492 0.4331 0.5393 0.058 Uiso 1 1 calc R U . . . H12B H 0.1742 0.4453 0.5756 0.058 Uiso 1 1 calc R U . . . H12C H 0.1141 0.3700 0.4731 0.058 Uiso 1 1 calc R U . . . C13 C 0.2387(3) 0.9206(2) 0.6477(2) 0.0281(7) Uani 1 1 d . . . . . H13A H 0.2160 0.9367 0.5898 0.034 Uiso 1 1 calc R U . . . H13B H 0.3203 0.9531 0.6650 0.034 Uiso 1 1 calc R U . . . C14 C 0.1832(3) 0.9645(3) 0.7257(2) 0.0312(7) Uani 1 1 d . . . . . H14A H 0.2009 0.9428 0.7809 0.047 Uiso 1 1 calc R U . . . H14B H 0.1027 0.9371 0.7055 0.047 Uiso 1 1 calc R U . . . H14C H 0.2099 1.0422 0.7415 0.047 Uiso 1 1 calc R U . . . C21 C 0.4400(4) 0.8029(4) -0.1011(3) 0.0500(11) Uani 1 1 d . . . . . H21A H 0.4927 0.8331 -0.1405 0.060 Uiso 1 1 calc R U . . . H21B H 0.4406 0.8618 -0.0469 0.060 Uiso 1 1 calc R U . . . C22 C 0.3277(5) 0.7529(5) -0.1562(3) 0.0724(17) Uani 1 1 d . . . . . H22A H 0.2738 0.7336 -0.1148 0.109 Uiso 1 1 calc R U . . . H22B H 0.3246 0.6888 -0.2047 0.109 Uiso 1 1 calc R U . . . H22C H 0.3102 0.8029 -0.1859 0.109 Uiso 1 1 calc R U . . . C23 C 0.5565(3) 0.6092(3) 0.1188(2) 0.0315(7) Uani 1 1 d . . . . . H23A H 0.4886 0.5493 0.1165 0.038 Uiso 1 1 calc R U . . . H23B H 0.5658 0.6667 0.1771 0.038 Uiso 1 1 calc R U . . . C24 C 0.6558(3) 0.5733(3) 0.1184(2) 0.0314(7) Uani 1 1 d . . . . . H24A H 0.7234 0.6345 0.1271 0.047 Uiso 1 1 calc R U . . . H24B H 0.6489 0.5208 0.0583 0.047 Uiso 1 1 calc R U . . . H24C H 0.6597 0.5411 0.1695 0.047 Uiso 1 1 calc R U . . . C31 C 0.0935(3) 1.1826(3) 0.2413(2) 0.0346(8) Uani 1 1 d . . . . . H31A H 0.0501 1.1077 0.2071 0.042 Uiso 1 1 calc R U . . . H31B H 0.1675 1.2007 0.2216 0.042 Uiso 1 1 calc R U . . . C32 C 0.0346(3) 1.2552(4) 0.2215(3) 0.0473(10) Uani 1 1 d . . . . . H32A H 0.0821 1.3292 0.2504 0.071 Uiso 1 1 calc R U . . . H32B H -0.0347 1.2415 0.2477 0.071 Uiso 1 1 calc R U . . . H32C H 0.0180 1.2423 0.1536 0.071 Uiso 1 1 calc R U . . . C33 C 0.1853(3) 1.1534(3) 0.5709(2) 0.0343(8) Uani 1 1 d . . . . . H33A H 0.2625 1.1539 0.5693 0.041 Uiso 1 1 calc R U . . . H33B H 0.1371 1.0805 0.5669 0.041 Uiso 1 1 calc R U . . . C34 C 0.1790(4) 1.2306(3) 0.6599(2) 0.0412(9) Uani 1 1 d . . . . . H34A H 0.1026 1.2304 0.6600 0.062 Uiso 1 1 calc R U . . . H34B H 0.2284 1.3021 0.6637 0.062 Uiso 1 1 calc R U . . . H34C H 0.2019 1.2096 0.7140 0.062 Uiso 1 1 calc R U . . . C41 C 0.2615(3) 0.9564(2) 0.0978(2) 0.0233(6) Uani 1 1 d . . . . . C42 C 0.2126(3) 0.9715(3) 0.0092(2) 0.0324(7) Uani 1 1 d . . . . . H42A H 0.2723 1.0126 -0.0179 0.049 Uiso 1 1 calc R U . . . H42B H 0.1604 1.0098 0.0242 0.049 Uiso 1 1 calc R U . . . H42C H 0.1736 0.9020 -0.0361 0.049 Uiso 1 1 calc R U . . . N51 N 0.5866(3) 0.5548(3) 0.4221(2) 0.0429(8) Uani 1 1 d . . . . . H51 H 0.6373 0.5950 0.4712 0.051 Uiso 1 1 calc R U . . . N52 N 0.0323(3) 0.2017(3) -0.0937(2) 0.0441(8) Uani 1 1 d . . . . . H52 H -0.0216 0.1625 -0.1406 0.053 Uiso 1 1 calc R U . . . C51 C 0.5115(3) 0.5933(3) 0.3853(2) 0.0278(7) Uani 1 1 d . . . . . H51A H 0.5154 0.6641 0.4146 0.033 Uiso 1 1 calc R U . . . C52 C 0.4329(2) 0.5356(2) 0.31010(19) 0.0165(5) Uani 1 1 d . . . . . H52A H 0.3823 0.5645 0.2869 0.020 Uiso 1 1 calc R U . . . C53 C 0.4285(3) 0.4356(3) 0.2689(2) 0.0251(6) Uani 1 1 d . . . . . C54 C 0.5013(3) 0.3917(3) 0.3035(2) 0.0290(7) Uani 1 1 d . . . . . H54 H 0.4961 0.3206 0.2739 0.035 Uiso 1 1 calc R U . . . C55 C 0.5803(3) 0.4519(3) 0.3802(2) 0.0322(7) Uani 1 1 d . . . . . H55 H 0.6303 0.4229 0.4043 0.039 Uiso 1 1 calc R U . . . C56 C 0.3457(3) 0.3687(3) 0.1856(2) 0.0275(7) Uani 1 1 d . . . . . H56 H 0.3404 0.2963 0.1640 0.033 Uiso 1 1 calc R U . . . C57 C 0.2779(3) 0.3997(3) 0.1379(2) 0.0269(6) Uani 1 1 d . . . . . H57 H 0.2828 0.4721 0.1578 0.032 Uiso 1 1 calc R U . . . C58 C 0.1953(3) 0.3286(3) 0.0556(2) 0.0265(7) Uani 1 1 d . . . . . C59 C 0.1122(2) 0.3614(2) 0.03348(19) 0.0186(6) Uani 1 1 d . . . . . H59 H 0.1094 0.4280 0.0686 0.022 Uiso 1 1 calc R U . . . C60 C 0.0333(3) 0.2992(3) -0.0389(2) 0.0321(7) Uani 1 1 d . . . . . H60 H -0.0258 0.3231 -0.0538 0.039 Uiso 1 1 calc R U . . . C61 C 0.2017(3) 0.2318(3) 0.0030(2) 0.0284(7) Uani 1 1 d . . . . . H61 H 0.2622 0.2101 0.0187 0.034 Uiso 1 1 calc R U . . . C62 C 0.1194(3) 0.1681(3) -0.0719(2) 0.0293(7) Uani 1 1 d . . . . . H62 H 0.1225 0.1021 -0.1080 0.035 Uiso 1 1 calc R U . . . O71 O 1.0974(2) 0.5391(2) 0.16679(19) 0.0402(6) Uani 1 1 d . . . . . H71 H 1.0945 0.4919 0.1351 0.060 Uiso 1 1 d R U . . . C71 C 0.9950(4) 0.5159(6) 0.2020(4) 0.083(2) Uani 1 1 d . . . . . H71A H 0.9868 0.5831 0.2381 0.100 Uiso 0.563(12) 1 calc R U P A 1 H71B H 0.9956 0.4721 0.2451 0.100 Uiso 0.563(12) 1 calc R U P A 1 H71C H 0.9632 0.4374 0.1816 0.100 Uiso 0.437(12) 1 calc R U P A 2 H71D H 1.0170 0.5360 0.2708 0.100 Uiso 0.437(12) 1 calc R U P A 2 C72A C 0.9008(7) 0.4595(7) 0.1269(6) 0.056(3) Uani 0.563(12) 1 d . . P A 1 H72A H 0.9015 0.5015 0.0827 0.084 Uiso 0.563(12) 1 calc R U P A 1 H72B H 0.8317 0.4486 0.1534 0.084 Uiso 0.563(12) 1 calc R U P A 1 H72C H 0.9056 0.3905 0.0940 0.084 Uiso 0.563(12) 1 calc R U P A 1 C72B C 0.9146(10) 0.5449(9) 0.1918(10) 0.065(4) Uani 0.437(12) 1 d . . P A 2 H72D H 0.9385 0.6226 0.2144 0.097 Uiso 0.437(12) 1 calc R U P A 2 H72E H 0.8587 0.5141 0.2276 0.097 Uiso 0.437(12) 1 calc R U P A 2 H72F H 0.8827 0.5212 0.1252 0.097 Uiso 0.437(12) 1 calc R U P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.01487(12) 0.01798(12) 0.01411(12) 0.00294(9) 0.00070(9) 0.00384(9) Mo2 0.01758(13) 0.02005(12) 0.01598(12) 0.00389(9) 0.00332(9) 0.00407(9) Mo3 0.01783(13) 0.01652(12) 0.01726(12) 0.00370(9) 0.00242(9) 0.00302(9) S1 0.0175(3) 0.0174(3) 0.0154(3) 0.0040(2) 0.0009(3) 0.0045(3) S2 0.0166(3) 0.0244(3) 0.0200(3) 0.0040(3) 0.0019(3) 0.0057(3) S3 0.0199(3) 0.0196(3) 0.0174(3) 0.0016(3) 0.0019(3) 0.0032(3) S4 0.0211(4) 0.0207(3) 0.0231(3) 0.0049(3) 0.0054(3) 0.0018(3) S11 0.0206(4) 0.0283(4) 0.0169(3) 0.0052(3) 0.0001(3) 0.0097(3) S12 0.0179(3) 0.0249(3) 0.0200(3) 0.0093(3) 0.0026(3) 0.0063(3) S21 0.0240(4) 0.0307(4) 0.0281(4) 0.0064(3) 0.0111(3) 0.0041(3) S22 0.0218(4) 0.0243(4) 0.0180(3) 0.0025(3) 0.0042(3) 0.0062(3) S31 0.0245(4) 0.0179(3) 0.0315(4) 0.0037(3) 0.0046(3) 0.0028(3) S32 0.0207(4) 0.0196(3) 0.0246(4) 0.0046(3) 0.0047(3) 0.0050(3) P11 0.0229(4) 0.0219(4) 0.0179(3) 0.0076(3) 0.0034(3) 0.0083(3) P21 0.0247(4) 0.0294(4) 0.0183(4) 0.0073(3) 0.0078(3) 0.0098(3) P31 0.0258(4) 0.0192(3) 0.0237(4) 0.0056(3) 0.0050(3) 0.0075(3) O1 0.0204(10) 0.0205(10) 0.0201(10) 0.0027(8) -0.0012(8) 0.0049(8) O11 0.0316(12) 0.0242(11) 0.0238(11) 0.0104(9) 0.0040(9) 0.0091(9) O12 0.0320(12) 0.0255(11) 0.0192(10) 0.0084(8) 0.0060(9) 0.0116(9) O21 0.0422(14) 0.0418(13) 0.0202(11) 0.0131(10) 0.0123(10) 0.0216(11) O22 0.0299(12) 0.0376(12) 0.0217(11) 0.0119(9) 0.0101(9) 0.0156(10) O31 0.0341(13) 0.0274(11) 0.0299(12) 0.0118(9) 0.0066(10) 0.0132(10) O32 0.0367(13) 0.0250(11) 0.0252(11) 0.0046(9) 0.0050(9) 0.0132(10) O41 0.0287(11) 0.0269(11) 0.0205(10) 0.0089(9) 0.0048(9) 0.0096(9) O42 0.0259(11) 0.0223(10) 0.0207(10) 0.0079(8) 0.0035(8) 0.0059(9) C11 0.0341(18) 0.0237(15) 0.0310(17) 0.0062(13) 0.0003(14) 0.0117(14) C12 0.0332(19) 0.0271(17) 0.060(2) 0.0167(17) 0.0131(17) 0.0106(15) C13 0.0303(17) 0.0231(15) 0.0288(16) 0.0056(13) 0.0067(13) 0.0074(13) C14 0.0344(18) 0.0305(17) 0.0285(17) 0.0065(13) 0.0096(14) 0.0113(14) C21 0.081(3) 0.065(3) 0.0315(19) 0.0271(19) 0.022(2) 0.049(3) C22 0.076(4) 0.130(5) 0.048(3) 0.043(3) 0.018(2) 0.071(4) C23 0.0324(18) 0.0438(19) 0.0273(16) 0.0186(15) 0.0113(14) 0.0172(15) C24 0.0337(18) 0.0335(17) 0.0267(16) 0.0072(14) 0.0015(14) 0.0129(15) C31 0.0353(19) 0.044(2) 0.0305(18) 0.0193(15) 0.0098(15) 0.0132(16) C32 0.041(2) 0.060(3) 0.053(2) 0.037(2) 0.0097(18) 0.0164(19) C33 0.049(2) 0.0303(17) 0.0255(17) 0.0086(14) 0.0056(15) 0.0157(16) C34 0.063(3) 0.0304(18) 0.0261(17) 0.0063(14) 0.0076(17) 0.0109(17) C41 0.0242(15) 0.0232(15) 0.0214(15) 0.0102(12) 0.0041(12) 0.0034(12) C42 0.0391(19) 0.0366(18) 0.0261(16) 0.0153(14) 0.0056(14) 0.0142(15) N51 0.0432(19) 0.0462(18) 0.0357(17) 0.0082(14) -0.0038(14) 0.0152(15) N52 0.0475(19) 0.0439(18) 0.0336(17) 0.0068(14) -0.0050(14) 0.0110(15) C51 0.0261(16) 0.0293(16) 0.0279(16) 0.0066(13) 0.0029(13) 0.0110(13) C52 0.0122(13) 0.0201(13) 0.0182(13) 0.0066(11) -0.0007(10) 0.0065(11) C53 0.0235(15) 0.0279(16) 0.0217(15) 0.0097(12) 0.0078(12) 0.0028(13) C54 0.0302(17) 0.0264(16) 0.0315(17) 0.0078(13) 0.0063(14) 0.0113(14) C55 0.0303(18) 0.0304(17) 0.0367(18) 0.0106(14) -0.0014(14) 0.0122(14) C56 0.0263(16) 0.0277(16) 0.0275(16) 0.0081(13) 0.0074(13) 0.0070(13) C57 0.0278(16) 0.0264(16) 0.0267(16) 0.0077(13) 0.0080(13) 0.0087(13) C58 0.0267(16) 0.0288(16) 0.0214(15) 0.0098(13) 0.0060(12) 0.0034(13) C59 0.0186(14) 0.0178(13) 0.0162(13) 0.0019(11) -0.0007(11) 0.0051(11) C60 0.0340(18) 0.0320(17) 0.0294(17) 0.0058(14) -0.0013(14) 0.0136(15) C61 0.0240(16) 0.0348(17) 0.0284(16) 0.0123(14) 0.0033(13) 0.0105(14) C62 0.0340(18) 0.0255(16) 0.0263(16) 0.0043(13) 0.0050(13) 0.0099(14) O71 0.0279(13) 0.0368(13) 0.0444(15) -0.0079(11) -0.0034(11) 0.0123(11) C71 0.035(3) 0.117(5) 0.067(3) -0.019(3) 0.005(2) 0.020(3) C72A 0.045(5) 0.046(5) 0.071(6) 0.015(4) -0.001(4) 0.011(4) C72B 0.067(8) 0.056(7) 0.100(10) 0.040(7) 0.040(7) 0.039(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 Mo2 2.7586(3) . ? Mo1 Mo3 2.7535(3) . ? Mo1 S1 2.3332(7) . ? Mo1 S2 2.3088(7) . ? Mo1 S3 2.2772(7) . ? Mo1 S11 2.5701(7) . ? Mo1 S12 2.5371(7) . ? Mo1 O1 2.250(2) . ? Mo2 Mo3 2.6881(3) . ? Mo2 S1 2.3368(7) . ? Mo2 S2 2.2938(7) . ? Mo2 S4 2.3014(7) . ? Mo2 S21 2.5581(8) . ? Mo2 S22 2.5289(7) . ? Mo2 O41 2.226(2) . ? Mo3 S1 2.3390(7) . ? Mo3 S3 2.2898(7) . ? Mo3 S4 2.2929(8) . ? Mo3 S31 2.5605(8) . ? Mo3 S32 2.5408(8) . ? Mo3 O42 2.230(2) . ? S11 P11 1.9941(10) . ? S12 P11 2.0029(10) . ? S21 P21 1.9907(11) . ? S22 P21 2.0018(11) . ? S31 P31 1.9876(11) . ? S32 P31 2.0024(10) . ? P11 O11 1.582(2) . ? P11 O12 1.583(2) . ? P21 O21 1.580(2) . ? P21 O22 1.578(2) . ? P31 O31 1.575(2) . ? P31 O32 1.582(2) . ? O1 H1 0.6710 . ? O11 C11 1.457(4) . ? O12 C13 1.466(4) . ? O21 C21 1.474(4) . ? O22 C23 1.469(4) . ? O31 C31 1.459(4) . ? O32 C33 1.451(4) . ? O41 C41 1.259(4) . ? O42 C41 1.270(4) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C11 C12 1.503(5) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C13 C14 1.501(4) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C21 C22 1.472(7) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C23 C24 1.505(5) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C31 C32 1.502(5) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C33 C34 1.505(5) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C41 C42 1.514(4) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? N51 H51 0.8800 . ? N51 C51 1.382(5) . ? N51 C55 1.376(5) . ? N52 H52 0.8800 . ? N52 C60 1.385(5) . ? N52 C62 1.385(5) . ? C51 H51A 0.9500 . ? C51 C52 1.346(4) . ? C52 H52A 0.9500 . ? C52 C53 1.346(4) . ? C53 C54 1.397(5) . ? C53 C56 1.471(4) . ? C54 H54 0.9500 . ? C54 C55 1.367(5) . ? C55 H55 0.9500 . ? C56 H56 0.9500 . ? C56 C57 1.322(5) . ? C57 H57 0.9500 . ? C57 C58 1.473(4) . ? C58 C59 1.335(4) . ? C58 C61 1.400(5) . ? C59 H59 0.9500 . ? C59 C60 1.333(4) . ? C60 H60 0.9500 . ? C61 H61 0.9500 . ? C61 C62 1.382(5) . ? C62 H62 0.9500 . ? O71 H71 0.6916 . ? O71 C71 1.422(6) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C71 H71C 0.9900 . ? C71 H71D 0.9900 . ? C71 C72A 1.455(10) . ? C71 C72B 1.230(12) . ? C72A H72A 0.9800 . ? C72A H72B 0.9800 . ? C72A H72C 0.9800 . ? C72B H72D 0.9800 . ? C72B H72E 0.9800 . ? C72B H72F 0.9800 . ? 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 Mo3 Mo1 Mo2 58.376(8) . . ? S1 Mo1 Mo2 53.853(18) . . ? S1 Mo1 Mo3 53.988(17) . . ? S1 Mo1 S11 160.44(3) . . ? S1 Mo1 S12 84.95(2) . . ? S2 Mo1 Mo2 52.929(19) . . ? S2 Mo1 Mo3 97.84(2) . . ? S2 Mo1 S1 104.93(3) . . ? S2 Mo1 S11 88.79(3) . . ? S2 Mo1 S12 161.60(3) . . ? S3 Mo1 Mo2 97.37(2) . . ? S3 Mo1 Mo3 53.132(19) . . ? S3 Mo1 S1 105.55(3) . . ? S3 Mo1 S2 97.58(3) . . ? S3 Mo1 S11 85.93(3) . . ? S3 Mo1 S12 94.53(3) . . ? S11 Mo1 Mo2 141.709(19) . . ? S11 Mo1 Mo3 139.004(19) . . ? S12 Mo1 Mo2 138.790(18) . . ? S12 Mo1 Mo3 100.500(18) . . ? S12 Mo1 S11 78.29(2) . . ? O1 Mo1 Mo2 94.74(5) . . ? O1 Mo1 Mo3 139.02(5) . . ? O1 Mo1 S1 85.49(5) . . ? O1 Mo1 S2 85.92(6) . . ? O1 Mo1 S3 166.98(6) . . ? O1 Mo1 S11 81.60(5) . . ? O1 Mo1 S12 79.34(6) . . ? Mo3 Mo2 Mo1 60.717(8) . . ? S1 Mo2 Mo1 53.733(17) . . ? S1 Mo2 Mo3 54.947(17) . . ? S1 Mo2 S21 160.16(3) . . ? S1 Mo2 S22 84.40(2) . . ? S2 Mo2 Mo1 53.427(19) . . ? S2 Mo2 Mo3 100.09(2) . . ? S2 Mo2 S1 105.30(3) . . ? S2 Mo2 S4 94.84(3) . . ? S2 Mo2 S21 87.44(3) . . ? S2 Mo2 S22 100.97(3) . . ? S4 Mo2 Mo1 97.42(2) . . ? S4 Mo2 Mo3 54.043(19) . . ? S4 Mo2 S1 108.34(3) . . ? S4 Mo2 S21 85.16(3) . . ? S4 Mo2 S22 156.36(3) . . ? S21 Mo2 Mo1 140.86(2) . . ? S21 Mo2 Mo3 138.82(2) . . ? S22 Mo2 Mo1 106.095(19) . . ? S22 Mo2 Mo3 137.912(19) . . ? S22 Mo2 S21 78.17(3) . . ? O41 Mo2 Mo1 133.75(6) . . ? O41 Mo2 Mo3 84.00(6) . . ? O41 Mo2 S1 82.21(6) . . ? O41 Mo2 S2 172.49(6) . . ? O41 Mo2 S4 82.42(6) . . ? O41 Mo2 S21 85.37(6) . . ? O41 Mo2 S22 79.66(6) . . ? Mo2 Mo3 Mo1 60.907(9) . . ? S1 Mo3 Mo1 53.793(17) . . ? S1 Mo3 Mo2 54.869(18) . . ? S1 Mo3 S31 160.02(3) . . ? S1 Mo3 S32 85.28(2) . . ? S3 Mo3 Mo1 52.712(18) . . ? S3 Mo3 Mo2 99.05(2) . . ? S3 Mo3 S1 104.95(2) . . ? S3 Mo3 S4 93.97(3) . . ? S3 Mo3 S31 88.33(3) . . ? S3 Mo3 S32 97.88(3) . . ? S4 Mo3 Mo1 97.77(2) . . ? S4 Mo3 Mo2 54.339(19) . . ? S4 Mo3 S1 108.55(3) . . ? S4 Mo3 S31 84.85(3) . . ? S4 Mo3 S32 158.82(3) . . ? S31 Mo3 Mo1 141.02(2) . . ? S31 Mo3 Mo2 138.77(2) . . ? S32 Mo3 Mo1 103.372(19) . . ? S32 Mo3 Mo2 139.519(19) . . ? S32 Mo3 S31 78.04(2) . . ? O42 Mo3 Mo1 133.81(5) . . ? O42 Mo3 Mo2 84.72(5) . . ? O42 Mo3 S1 81.80(6) . . ? O42 Mo3 S3 173.25(6) . . ? O42 Mo3 S4 83.66(6) . . ? O42 Mo3 S31 85.17(6) . . ? O42 Mo3 S32 82.56(6) . . ? Mo1 S1 Mo2 72.41(2) . . ? Mo1 S1 Mo3 72.22(2) . . ? Mo2 S1 Mo3 70.18(2) . . ? Mo2 S2 Mo1 73.64(2) . . ? Mo1 S3 Mo3 74.16(2) . . ? Mo3 S4 Mo2 71.62(2) . . ? P11 S11 Mo1 86.67(3) . . ? P11 S12 Mo1 87.39(3) . . ? P21 S21 Mo2 87.18(4) . . ? P21 S22 Mo2 87.75(3) . . ? P31 S31 Mo3 87.25(3) . . ? P31 S32 Mo3 87.48(3) . . ? S11 P11 S12 107.54(4) . . ? O11 P11 S11 113.18(9) . . ? O11 P11 S12 113.41(9) . . ? O11 P11 O12 96.87(12) . . ? O12 P11 S11 113.69(9) . . ? O12 P11 S12 112.06(9) . . ? S21 P21 S22 106.90(5) . . ? O21 P21 S21 112.16(10) . . ? O21 P21 S22 114.76(10) . . ? O22 P21 S21 113.90(10) . . ? O22 P21 S22 112.27(9) . . ? O22 P21 O21 96.89(12) . . ? S31 P31 S32 107.21(5) . . ? O31 P31 S31 113.32(10) . . ? O31 P31 S32 113.19(10) . . ? O31 P31 O32 95.75(12) . . ? O32 P31 S31 113.93(10) . . ? O32 P31 S32 113.37(9) . . ? Mo1 O1 H1 120.1 . . ? C11 O11 P11 119.9(2) . . ? C13 O12 P11 117.34(19) . . ? C21 O21 P21 120.3(2) . . ? C23 O22 P21 118.62(19) . . ? C31 O31 P31 121.1(2) . . ? C33 O32 P31 120.6(2) . . ? C41 O41 Mo2 123.38(19) . . ? C41 O42 Mo3 122.06(19) . . ? O11 C11 H11A 110.2 . . ? O11 C11 H11B 110.2 . . ? O11 C11 C12 107.7(3) . . ? H11A C11 H11B 108.5 . . ? C12 C11 H11A 110.2 . . ? C12 C11 H11B 110.2 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O12 C13 H13A 110.1 . . ? O12 C13 H13B 110.1 . . ? O12 C13 C14 107.9(3) . . ? H13A C13 H13B 108.4 . . ? C14 C13 H13A 110.1 . . ? C14 C13 H13B 110.1 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14B 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O21 C21 H21A 109.5 . . ? O21 C21 H21B 109.5 . . ? O21 C21 C22 110.9(4) . . ? H21A C21 H21B 108.1 . . ? C22 C21 H21A 109.5 . . ? C22 C21 H21B 109.5 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22B 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O22 C23 H23A 109.9 . . ? O22 C23 H23B 109.9 . . ? O22 C23 C24 108.7(3) . . ? H23A C23 H23B 108.3 . . ? C24 C23 H23A 109.9 . . ? C24 C23 H23B 109.9 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O31 C31 H31A 110.5 . . ? O31 C31 H31B 110.5 . . ? O31 C31 C32 106.2(3) . . ? H31A C31 H31B 108.7 . . ? C32 C31 H31A 110.5 . . ? C32 C31 H31B 110.5 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32B 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? O32 C33 H33A 110.3 . . ? O32 C33 H33B 110.3 . . ? O32 C33 C34 107.0(3) . . ? H33A C33 H33B 108.6 . . ? C34 C33 H33A 110.3 . . ? C34 C33 H33B 110.3 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34B 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? O41 C41 O42 125.7(3) . . ? O41 C41 C42 116.8(3) . . ? O42 C41 C42 117.4(3) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42B 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C51 N51 H51 120.8 . . ? C55 N51 H51 120.8 . . ? C55 N51 C51 118.3(3) . . ? C60 N52 H52 121.2 . . ? C60 N52 C62 117.6(3) . . ? C62 N52 H52 121.2 . . ? N51 C51 H51A 118.3 . . ? C52 C51 N51 123.3(3) . . ? C52 C51 H51A 118.4 . . ? C51 C52 H52A 121.1 . . ? C53 C52 C51 117.8(3) . . ? C53 C52 H52A 121.1 . . ? C52 C53 C54 121.5(3) . . ? C52 C53 C56 120.6(3) . . ? C54 C53 C56 117.9(3) . . ? C53 C54 H54 120.2 . . ? C55 C54 C53 119.5(3) . . ? C55 C54 H54 120.2 . . ? N51 C55 H55 120.3 . . ? C54 C55 N51 119.4(3) . . ? C54 C55 H55 120.3 . . ? C53 C56 H56 116.9 . . ? C57 C56 C53 126.2(3) . . ? C57 C56 H56 116.9 . . ? C56 C57 H57 118.1 . . ? C56 C57 C58 123.8(3) . . ? C58 C57 H57 118.1 . . ? C59 C58 C57 116.0(3) . . ? C59 C58 C61 121.1(3) . . ? C61 C58 C57 122.9(3) . . ? C58 C59 H59 120.6 . . ? C60 C59 C58 118.8(3) . . ? C60 C59 H59 120.6 . . ? N52 C60 H60 118.1 . . ? C59 C60 N52 123.8(3) . . ? C59 C60 H60 118.1 . . ? C58 C61 H61 120.2 . . ? C62 C61 C58 119.5(3) . . ? C62 C61 H61 120.2 . . ? N52 C62 H62 120.4 . . ? C61 C62 N52 119.1(3) . . ? C61 C62 H62 120.4 . . ? C71 O71 H71 104.9 . . ? O71 C71 H71A 109.3 . . ? O71 C71 H71B 109.3 . . ? O71 C71 H71C 104.3 . . ? O71 C71 H71D 104.3 . . ? O71 C71 C72A 111.8(5) . . ? H71A C71 H71B 107.9 . . ? H71C C71 H71D 105.6 . . ? C72A C71 H71A 109.3 . . ? C72A C71 H71B 109.3 . . ? C72B C71 O71 131.8(9) . . ? C72B C71 H71C 104.3 . . ? C72B C71 H71D 104.3 . . ? C71 C72A H72A 109.5 . . ? C71 C72A H72B 109.5 . . ? C71 C72A H72C 109.5 . . ? H72A C72A H72B 109.5 . . ? H72A C72A H72C 109.5 . . ? H72B C72A H72C 109.5 . . ? C71 C72B H72D 109.5 . . ? C71 C72B H72E 109.5 . . ? C71 C72B H72F 109.5 . . ? H72D C72B H72E 109.5 . . ? H72D C72B H72F 109.5 . . ? H72E C72B H72F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Mo2 O41 C41 O42 4.0(4) . . . . ? Mo2 O41 C41 C42 -175.9(2) . . . . ? Mo3 O42 C41 O41 -2.5(4) . . . . ? Mo3 O42 C41 C42 177.3(2) . . . . ? S11 P11 O11 C11 -63.4(2) . . . . ? S11 P11 O12 C13 61.6(2) . . . . ? S12 P11 O11 C11 59.4(2) . . . . ? S12 P11 O12 C13 -60.6(2) . . . . ? S21 P21 O21 C21 -49.5(3) . . . . ? S21 P21 O22 C23 72.3(2) . . . . ? S22 P21 O21 C21 72.8(3) . . . . ? S22 P21 O22 C23 -49.4(2) . . . . ? S31 P31 O31 C31 62.0(3) . . . . ? S31 P31 O32 C33 -65.6(3) . . . . ? S32 P31 O31 C31 -60.3(3) . . . . ? S32 P31 O32 C33 57.4(3) . . . . ? P11 O11 C11 C12 176.6(2) . . . . ? P11 O12 C13 C14 162.1(2) . . . . ? P21 O21 C21 C22 -107.1(3) . . . . ? P21 O22 C23 C24 -156.5(2) . . . . ? P31 O31 C31 C32 -175.8(2) . . . . ? P31 O32 C33 C34 165.9(2) . . . . ? O11 P11 O12 C13 -179.3(2) . . . . ? O12 P11 O11 C11 177.1(2) . . . . ? O21 P21 O22 C23 -169.7(2) . . . . ? O22 P21 O21 C21 -168.8(3) . . . . ? O31 P31 O32 C33 175.7(3) . . . . ? O32 P31 O31 C31 -178.8(2) . . . . ? N51 C51 C52 C53 -0.4(5) . . . . ? C51 N51 C55 C54 0.7(5) . . . . ? C51 C52 C53 C54 1.1(5) . . . . ? C51 C52 C53 C56 -179.1(3) . . . . ? C52 C53 C54 C55 -1.0(5) . . . . ? C52 C53 C56 C57 7.4(5) . . . . ? C53 C54 C55 N51 0.1(5) . . . . ? C53 C56 C57 C58 -179.0(3) . . . . ? C54 C53 C56 C57 -172.8(3) . . . . ? C55 N51 C51 C52 -0.5(5) . . . . ? C56 C53 C54 C55 179.3(3) . . . . ? C56 C57 C58 C59 160.0(3) . . . . ? C56 C57 C58 C61 -19.9(5) . . . . ? C57 C58 C59 C60 -178.3(3) . . . . ? C57 C58 C61 C62 178.4(3) . . . . ? C58 C59 C60 N52 -0.5(5) . . . . ? C58 C61 C62 N52 0.3(5) . . . . ? C59 C58 C61 C62 -1.4(5) . . . . ? C60 N52 C62 C61 0.7(5) . . . . ? C61 C58 C59 C60 1.5(5) . . . . ? C62 N52 C60 C59 -0.6(5) . . . . ? loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 1 -1 0 0.0599 0.9997 -0.9991 -0.0024 0.1064 -0.0525 -0.0814 -1 1 0 0.0599 -0.9997 0.9991 0.0024 -0.1064 0.0525 0.0814 0 1 0 0.1200 0.0003 0.9988 0.0031 -0.0759 0.0884 -0.0374 -1 -4 2 0.0893 -1.0007 -3.9983 1.9895 0.3699 -0.2011 0.3132 -2 1 2 0.0446 -1.9992 0.9960 2.0045 -0.0401 0.2049 0.2449 2 -1 -2 0.0916 1.9992 -0.9960 -2.0045 0.0401 -0.2049 -0.2449 -4 -5 -2 0.1159 -4.0016 -4.9892 -2.0212 0.1608 -0.7733 0.6179 1 8 -5 0.1102 1.0012 7.9987 -4.9811 -0.8186 0.2722 -0.5299 7 -6 3 0.0866 6.9986 -6.0003 2.9903 0.8139 0.0029 -0.5404 0 -8 7 0.0835 -0.0009 -8.0025 6.9845 0.9459 -0.0482 0.4557 0 8 -7 0.0874 0.0009 8.0025 -6.9845 -0.9459 0.0482 -0.4557 6 -3 6 0.1167 6.0001 -3.0088 6.0031 0.7009 0.5144 -0.4669 -5 3 -7 0.0904 -5.0003 3.0102 -7.0037 -0.7188 -0.5727 0.3257 _database_code_depnum_ccdc_archive 'CCDC 920388' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_Sample6 _audit_creation_date 2013-05-31 _audit_creation_method ; Olex2 1.2-ac2 (compiled 2012.03.27 svn.r2268, GUI svn.r4156) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C32 H70 Mo6 N2 O16 P6 S20' _chemical_formula_sum 'C32 H70 Mo6 N2 O16 P6 S20' _chemical_formula_weight 2141.56 _chemical_absolute_configuration ? _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -0.0483 2.7339 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system orthorhombic _space_group_IT_number 33 _space_group_name_H-M_alt 'P n a 21' _space_group_name_Hall 'P 2c -2n' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 14.1592(2) _cell_length_b 20.8726(4) _cell_length_c 25.0380(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 7399.7(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 13553 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 73.2040 _cell_measurement_theta_min 3.7400 _exptl_absorpt_coefficient_mu 15.050 _exptl_absorpt_correction_T_max 0.553 _exptl_absorpt_correction_T_min 0.114 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_crystal_colour 'dark brown' _exptl_crystal_density_diffrn 1.922 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 4264 _exptl_crystal_size_max 0.2834 _exptl_crystal_size_mid 0.1309 _exptl_crystal_size_min 0.0431 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0546 _diffrn_reflns_av_unetI/netI 0.0460 _diffrn_reflns_Laue_measured_fraction_full 0.975 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_number 51323 _diffrn_reflns_point_group_measured_fraction_full 0.953 _diffrn_reflns_point_group_measured_fraction_max 0.977 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 66.598 _diffrn_reflns_theta_min 3.121 _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 10.5953 _diffrn_measured_fraction_theta_full 0.9994 _diffrn_measured_fraction_theta_max 0.9542 _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 -0.0404174000 _diffrn_orient_matrix_UB_12 0.0135186000 _diffrn_orient_matrix_UB_13 -0.0560163000 _diffrn_orient_matrix_UB_21 -0.0802615000 _diffrn_orient_matrix_UB_22 0.0396528000 _diffrn_orient_matrix_UB_23 0.0251347000 _diffrn_orient_matrix_UB_31 0.0614329000 _diffrn_orient_matrix_UB_32 0.0607226000 _diffrn_orient_matrix_UB_33 -0.0040314000 _diffrn_radiation_monochromator mirror _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.5418 _diffrn_source 'SuperNova (Cu) X-ray Source' _reflns_Friedel_coverage 0.906 _reflns_Friedel_fraction_full 0.929 _reflns_Friedel_fraction_max 0.952 _reflns_number_gt 10900 _reflns_number_total 12757 _reflns_odcompleteness_completeness 99.94 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.49 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. These statistics refer to single and composite reflections containing twin component 1 only. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; SHELXL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution ; M.C.Burla, R.Caliandro, M.Camalli, B.Carrozzini, G.L.Cascarano, C.Giacovazzo, M.Mallamo, A.Mazzone, G.Polidori and R. Spagna SIR2011: a new package for crystal structure determination and refinement J. Appl. Cryst. (2012). 45, 357-361. ; _refine_diff_density_max 1.357 _refine_diff_density_min -1.156 _refine_diff_density_rms 0.221 _refine_ls_abs_structure_details ; Flack x determined using 4590 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons and Flack (2004), Acta Cryst. A60, s61). ; _refine_ls_abs_structure_Flack -0.006(9) _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.142 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 772 _refine_ls_number_reflns 12757 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0837 _refine_ls_R_factor_gt 0.0694 _refine_ls_restrained_S_all 1.141 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0989P)^2^+33.1300P] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1760 _refine_ls_wR_factor_ref 0.1907 _refine_special_details ; Refined as a 2-component twin. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary ? 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.32147(10) 0.24937(7) 0.17728(6) 0.0400(4) Uani 1 1 d . . . . . Mo2 Mo 0.24817(11) 0.18459(8) 0.09463(7) 0.0474(4) Uani 1 1 d . . . . . Mo3 Mo 0.31380(9) 0.11714(7) 0.18114(6) 0.0408(3) Uani 1 1 d . . . . . Mo4 Mo -0.07932(9) -0.25528(7) 0.10791(6) 0.0383(3) Uani 1 1 d . . . . . Mo5 Mo -0.00601(10) -0.20126(8) 0.19552(7) 0.0452(4) Uani 1 1 d . . . . . Mo6 Mo -0.07149(9) -0.12345(7) 0.11470(6) 0.0390(3) Uani 1 1 d . . . . . S1 S 0.1850(3) 0.1873(2) 0.1811(2) 0.0405(9) Uani 1 1 d . . . . . S2 S 0.3712(4) 0.2561(3) 0.0906(2) 0.0551(12) Uani 1 1 d . . . . . S3 S 0.3489(3) 0.0983(3) 0.0932(2) 0.0531(12) Uani 1 1 d . . . . . S4 S 0.4410(3) 0.1803(2) 0.2006(2) 0.0473(11) Uani 1 1 d . . . . . S5 S 0.0577(3) -0.1934(2) 0.1101(2) 0.0409(9) Uani 1 1 d . . . . . S6 S -0.1277(3) -0.2741(2) 0.1935(2) 0.0470(10) Uani 1 1 d . . . . . S7 S -0.1061(3) -0.1151(2) 0.20454(19) 0.0469(10) Uani 1 1 d . . . . . S8 S -0.1976(3) -0.1836(2) 0.0897(2) 0.0429(10) Uani 1 1 d . . . . . S11 S 0.2794(3) 0.2830(2) 0.2717(2) 0.0481(11) Uani 1 1 d . . . . . S12 S 0.4329(3) 0.3438(3) 0.1919(2) 0.0543(12) Uani 1 1 d . . . . . S21 S 0.2582(5) 0.1859(4) -0.0068(3) 0.0750(18) Uani 1 1 d . . . . . S22 S 0.0965(3) 0.1298(3) 0.0691(2) 0.0532(12) Uani 1 1 d . . . . . S31 S 0.4184(3) 0.0201(3) 0.2029(2) 0.0549(13) Uani 1 1 d . . . . . S32 S 0.2684(3) 0.0953(2) 0.2768(2) 0.0460(10) Uani 1 1 d . . . . . S41 S -0.0341(3) -0.2799(2) 0.0114(2) 0.0492(11) Uani 1 1 d . . . . . S42 S -0.1888(3) -0.3476(3) 0.0861(2) 0.0549(13) Uani 1 1 d . . . . . S51 S -0.0156(4) -0.2179(4) 0.2963(2) 0.0645(15) Uani 1 1 d . . . . . S52 S 0.1442(4) -0.1494(3) 0.2265(2) 0.0549(12) Uani 1 1 d . . . . . S61 S -0.1754(3) -0.0239(2) 0.1016(2) 0.0495(11) Uani 1 1 d . . . . . S62 S -0.0248(3) -0.0895(2) 0.02123(19) 0.0466(10) Uani 1 1 d . . . . . P1 P 0.3775(4) 0.3520(3) 0.2645(3) 0.0535(13) Uani 1 1 d . . . . . P2 P 0.1321(4) 0.1433(3) -0.0077(2) 0.0639(15) Uani 1 1 d . . . . . P3 P 0.3689(4) 0.0277(3) 0.2776(2) 0.0545(12) Uani 1 1 d . . . . . P4 P -0.1330(4) -0.3486(2) 0.0133(2) 0.0522(12) Uani 1 1 d . . . . . P5 P 0.1076(4) -0.1729(4) 0.3018(3) 0.0647(15) Uani 1 1 d . . . . . P6 P -0.1284(4) -0.0245(2) 0.0263(2) 0.0488(11) Uani 1 1 d . . . . . O1 O 0.2224(9) 0.3257(7) 0.1544(6) 0.051(3) Uani 1 1 d . . . . . O2 O 0.1612(10) 0.2718(8) 0.0843(6) 0.058(4) Uani 1 1 d . . . . . O3 O 0.0210(10) -0.3334(7) 0.1245(7) 0.054(3) Uani 1 1 d . . . . . O4 O 0.0803(9) -0.2900(7) 0.1975(7) 0.057(4) Uani 1 1 d . . . . . O11 O 0.4539(10) 0.3509(8) 0.3107(8) 0.065(4) Uani 1 1 d . . . . . O12 O 0.3381(11) 0.4210(8) 0.2771(7) 0.065(4) Uani 1 1 d . . . . . O21 O 0.0542(13) 0.1817(9) -0.0393(6) 0.068(4) Uani 1 1 d . . . . . O22 O 0.1276(12) 0.0814(9) -0.0412(6) 0.069(4) Uani 1 1 d . . . . . O31 O 0.3245(12) -0.0354(7) 0.3014(8) 0.072(5) Uani 1 1 d D . . . . O32 O 0.4478(11) 0.0437(8) 0.3199(7) 0.065(4) Uani 1 1 d . . . . . O41 O -0.2076(12) -0.3432(8) -0.0321(8) 0.067(4) Uani 1 1 d . . . . . O42 O -0.0943(10) -0.4166(7) -0.0043(7) 0.063(4) Uani 1 1 d D . . . . O51 O 0.1850(12) -0.2146(10) 0.3316(8) 0.075(5) Uani 1 1 d . . . . . O52 O 0.1037(14) -0.1149(10) 0.3420(8) 0.086(6) Uani 1 1 d . . . . . O61 O -0.0907(11) 0.0426(7) 0.0072(7) 0.064(4) Uani 1 1 d . . . . . O62 O -0.2077(13) -0.0372(9) -0.0153(9) 0.079(5) Uani 1 1 d D . . . . N1 N 0.1952(11) 0.0357(7) 0.1681(7) 0.044(4) Uani 1 1 d . . . . . N2 N 0.0471(11) -0.0443(8) 0.1355(7) 0.046(4) Uani 1 1 d . . . . . C1 C 0.1669(13) 0.3203(10) 0.1152(9) 0.050(5) Uani 1 1 d . . . . . C2 C 0.1043(17) 0.3743(13) 0.0992(15) 0.087(9) Uani 1 1 d . . . . . H2A H 0.1053 0.3788 0.0610 0.131 Uiso 1 1 calc R U . . . H2B H 0.1262 0.4132 0.1154 0.131 Uiso 1 1 calc R U . . . H2C H 0.0409 0.3657 0.1108 0.131 Uiso 1 1 calc R U . . . C3 C 0.2070(13) -0.0098(10) 0.1308(8) 0.046(4) Uani 1 1 d . . . . . H3 H 0.2663 -0.0150 0.1154 0.055 Uiso 1 1 calc R U . . . C4 C 0.1329(11) -0.0499(8) 0.1143(8) 0.040(4) Uani 1 1 d . . . . . H4 H 0.1438 -0.0807 0.0882 0.048 Uiso 1 1 calc R U . . . C5 C 0.0368(13) 0.0002(9) 0.1735(8) 0.047(4) Uani 1 1 d . . . . . H5 H -0.0216 0.0042 0.1901 0.057 Uiso 1 1 calc R U . . . C6 C 0.1083(12) 0.0403(9) 0.1889(9) 0.046(4) Uani 1 1 d . . . . . H6 H 0.0962 0.0717 0.2144 0.056 Uiso 1 1 calc R U . . . C7 C 0.0730(16) -0.3350(10) 0.1636(11) 0.059(6) Uani 1 1 d . . . . . C8 C 0.1301(16) -0.3929(10) 0.1737(11) 0.062(6) Uani 1 1 d . . . . . H8A H 0.1447 -0.4133 0.1403 0.093 Uiso 1 1 calc R U . . . H8B H 0.0951 -0.4220 0.1958 0.093 Uiso 1 1 calc R U . . . H8C H 0.1877 -0.3811 0.1914 0.093 Uiso 1 1 calc R U . . . C11 C 0.5160(14) 0.2938(11) 0.3160(9) 0.061(6) Uani 1 1 d D . . . . H11A H 0.5493 0.2857 0.2828 0.074 Uiso 1 1 calc R U . . . H11B H 0.4791 0.2562 0.3251 0.074 Uiso 1 1 calc R U . . . C12 C 0.5847(14) 0.3091(13) 0.3599(9) 0.069(7) Uani 1 1 d D . . . . H12A H 0.5509 0.3158 0.3927 0.103 Uiso 1 1 calc R U . . . H12B H 0.6191 0.3473 0.3509 0.103 Uiso 1 1 calc R U . . . H12C H 0.6280 0.2741 0.3642 0.103 Uiso 1 1 calc R U . . . C13 C 0.2604(18) 0.4455(9) 0.2440(9) 0.064(6) Uani 1 1 d D . . . . H13A H 0.2143 0.4122 0.2369 0.076 Uiso 1 1 calc R U . . . H13B H 0.2840 0.4618 0.2102 0.076 Uiso 1 1 calc R U . . . C14 C 0.218(2) 0.4984(12) 0.2765(11) 0.089(9) Uani 1 1 d D . . . . H14A H 0.2652 0.5295 0.2850 0.134 Uiso 1 1 calc R U . . . H14B H 0.1919 0.4811 0.3089 0.134 Uiso 1 1 calc R U . . . H14C H 0.1680 0.5186 0.2563 0.134 Uiso 1 1 calc R U . . . C21 C 0.033(3) 0.2461(16) -0.0248(11) 0.096(10) Uani 1 1 d D . . . . H21A H -0.0299 0.2467 -0.0101 0.115 Uiso 0.46(4) 1 calc R U P A 1 H21B H 0.0762 0.2580 0.0038 0.115 Uiso 0.46(4) 1 calc R U P A 1 H21C H 0.0100 0.2479 0.0116 0.115 Uiso 0.54(4) 1 calc R U P A 2 H21D H 0.0898 0.2723 -0.0273 0.115 Uiso 0.54(4) 1 calc R U P A 2 C22A C 0.039(6) 0.297(2) -0.0667(18) 0.09(2) Uani 0.46(4) 1 d D . P A 1 H22A H 0.0779 0.3316 -0.0541 0.134 Uiso 0.46(4) 1 calc R U P A 1 H22B H -0.0235 0.3131 -0.0740 0.134 Uiso 0.46(4) 1 calc R U P A 1 H22C H 0.0654 0.2796 -0.0988 0.134 Uiso 0.46(4) 1 calc R U P A 1 C22B C -0.040(3) 0.270(3) -0.0630(17) 0.09(2) Uani 0.54(4) 1 d D . P A 2 H22D H -0.0109 0.2817 -0.0960 0.134 Uiso 0.54(4) 1 calc R U P A 2 H22E H -0.0721 0.3058 -0.0478 0.134 Uiso 0.54(4) 1 calc R U P A 2 H22F H -0.0852 0.2360 -0.0696 0.134 Uiso 0.54(4) 1 calc R U P A 2 C23 C 0.1864(18) 0.0268(13) -0.0264(9) 0.073(7) Uani 1 1 d D . . . . H23A H 0.2459 0.0412 -0.0114 0.088 Uiso 1 1 calc R U . . . H23B H 0.1544 0.0002 -0.0003 0.088 Uiso 1 1 calc R U . . . C24 C 0.202(4) -0.009(2) -0.0771(11) 0.17(2) Uani 1 1 d D . . . . H24A H 0.2455 0.0138 -0.0994 0.249 Uiso 1 1 calc R U . . . H24B H 0.1434 -0.0148 -0.0955 0.249 Uiso 1 1 calc R U . . . H24C H 0.2285 -0.0508 -0.0690 0.249 Uiso 1 1 calc R U . . . C31 C 0.3701(17) -0.0973(9) 0.2979(13) 0.088(9) Uani 1 1 d D . . . . H31A H 0.4315 -0.0941 0.2809 0.105 Uiso 0.46(4) 1 calc R U P A 1 H31B H 0.3315 -0.1278 0.2785 0.105 Uiso 0.46(4) 1 calc R U P A 1 H31C H 0.3363 -0.1261 0.3215 0.105 Uiso 0.54(4) 1 calc R U P A 2 H31D H 0.3606 -0.1129 0.2618 0.105 Uiso 0.54(4) 1 calc R U P A 2 C32A C 0.379(3) -0.115(2) 0.3558(13) 0.060(14) Uani 0.46(4) 1 d D . P A 1 H32A H 0.4382 -0.1002 0.3693 0.090 Uiso 0.46(4) 1 calc R U P A 1 H32B H 0.3750 -0.1607 0.3594 0.090 Uiso 0.46(4) 1 calc R U P A 1 H32C H 0.3283 -0.0954 0.3755 0.090 Uiso 0.46(4) 1 calc R U P A 1 C32B C 0.4732(19) -0.104(3) 0.310(3) 0.085(17) Uani 0.54(4) 1 d D . P A 2 H32D H 0.5093 -0.0978 0.2782 0.128 Uiso 0.54(4) 1 calc R U P A 2 H32E H 0.4852 -0.1460 0.3243 0.128 Uiso 0.54(4) 1 calc R U P A 2 H32F H 0.4911 -0.0724 0.3362 0.128 Uiso 0.54(4) 1 calc R U P A 2 C33 C 0.5006(17) 0.1023(13) 0.3144(10) 0.075(8) Uani 1 1 d D . . . . H33A H 0.4581 0.1383 0.3102 0.090 Uiso 1 1 calc R U . . . H33B H 0.5415 0.1001 0.2834 0.090 Uiso 1 1 calc R U . . . C34 C 0.558(2) 0.1101(17) 0.3642(10) 0.086(9) Uani 1 1 d D . . . . H34A H 0.5748 0.0686 0.3780 0.129 Uiso 1 1 calc R U . . . H34B H 0.5224 0.1331 0.3904 0.129 Uiso 1 1 calc R U . . . H34C H 0.6149 0.1335 0.3560 0.129 Uiso 1 1 calc R U . . . C41 C -0.2710(18) -0.2855(14) -0.0309(11) 0.077(8) Uani 1 1 d D . . . . H41A H -0.3028 -0.2822 0.0033 0.093 Uiso 1 1 calc R U . . . H41B H -0.2351 -0.2466 -0.0370 0.093 Uiso 1 1 calc R U . . . C42 C -0.3408(19) -0.2963(17) -0.0750(11) 0.094(10) Uani 1 1 d D . . . . H42A H -0.3772 -0.3340 -0.0675 0.140 Uiso 1 1 calc R U . . . H42B H -0.3078 -0.3017 -0.1082 0.140 Uiso 1 1 calc R U . . . H42C H -0.3822 -0.2600 -0.0775 0.140 Uiso 1 1 calc R U . . . C43 C -0.0194(15) -0.4464(13) 0.0262(10) 0.088(9) Uani 1 1 d D . . . . H43A H -0.0410 -0.4571 0.0618 0.106 Uiso 1 1 calc R U . . . H43B H 0.0346 -0.4179 0.0290 0.106 Uiso 1 1 calc R U . . . C44 C 0.006(2) -0.5058(11) -0.0044(14) 0.107(13) Uani 1 1 d D . . . . H44A H 0.0215 -0.4946 -0.0405 0.160 Uiso 1 1 calc R U . . . H44B H -0.0464 -0.5349 -0.0042 0.160 Uiso 1 1 calc R U . . . H44C H 0.0597 -0.5260 0.0121 0.160 Uiso 1 1 calc R U . . . C51 C 0.220(2) -0.2716(16) 0.3075(11) 0.089(10) Uani 1 1 d D . . . . H51A H 0.1751 -0.2865 0.2811 0.107 Uiso 1 1 calc R U . . . H51B H 0.2788 -0.2621 0.2892 0.107 Uiso 1 1 calc R U . . . C52 C 0.237(4) -0.3237(17) 0.3475(14) 0.137(17) Uani 1 1 d D . . . . H52A H 0.2633 -0.3057 0.3795 0.205 Uiso 1 1 calc R U . . . H52B H 0.2802 -0.3545 0.3329 0.205 Uiso 1 1 calc R U . . . H52C H 0.1782 -0.3444 0.3558 0.205 Uiso 1 1 calc R U . . . C53 C 0.033(3) -0.0663(17) 0.3327(17) 0.128(15) Uani 1 1 d D . . . . H53A H 0.0276 -0.0581 0.2947 0.154 Uiso 1 1 calc R U . . . H53B H -0.0277 -0.0811 0.3456 0.154 Uiso 1 1 calc R U . . . C54 C 0.060(3) -0.0058(16) 0.3611(17) 0.119(14) Uani 1 1 d D . . . . H54A H 0.1229 -0.0099 0.3749 0.178 Uiso 1 1 calc R U . . . H54B H 0.0168 0.0017 0.3900 0.178 Uiso 1 1 calc R U . . . H54C H 0.0575 0.0295 0.3366 0.178 Uiso 1 1 calc R U . . . C61 C -0.1391(16) 0.1016(10) 0.0195(10) 0.063(6) Uani 1 1 d D . . . . H61A H -0.0934 0.1361 0.0222 0.076 Uiso 1 1 calc R U . . . H61B H -0.1705 0.0975 0.0537 0.076 Uiso 1 1 calc R U . . . C62 C -0.210(2) 0.1177(16) -0.0226(11) 0.097(10) Uani 1 1 d D . . . . H62A H -0.2576 0.0848 -0.0240 0.145 Uiso 1 1 calc R U . . . H62B H -0.1796 0.1208 -0.0567 0.145 Uiso 1 1 calc R U . . . H62C H -0.2397 0.1579 -0.0142 0.145 Uiso 1 1 calc R U . . . C63 C -0.255(2) -0.0981(11) -0.0211(12) 0.105(11) Uani 1 1 d D . . . . H63A H -0.2097 -0.1325 -0.0190 0.126 Uiso 1 1 calc R U . . . H63B H -0.3002 -0.1035 0.0080 0.126 Uiso 1 1 calc R U . . . C64 C -0.307(2) -0.1016(17) -0.0733(11) 0.091(9) Uani 1 1 d D . . . . H64A H -0.2622 -0.0978 -0.1021 0.136 Uiso 1 1 calc R U . . . H64B H -0.3518 -0.0673 -0.0755 0.136 Uiso 1 1 calc R U . . . H64C H -0.3391 -0.1419 -0.0759 0.136 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0253(7) 0.0481(8) 0.0467(8) 0.0006(6) 0.0047(6) -0.0048(6) Mo2 0.0338(8) 0.0641(10) 0.0444(7) -0.0007(7) 0.0063(6) -0.0071(7) Mo3 0.0262(6) 0.0464(7) 0.0497(8) -0.0073(6) 0.0048(6) -0.0014(5) Mo4 0.0246(7) 0.0441(7) 0.0461(8) 0.0047(6) 0.0055(6) -0.0032(5) Mo5 0.0300(7) 0.0570(8) 0.0485(8) 0.0062(7) 0.0013(6) -0.0004(6) Mo6 0.0280(7) 0.0431(7) 0.0460(7) -0.0017(6) 0.0046(6) 0.0008(5) S1 0.0262(19) 0.047(2) 0.049(2) -0.0003(18) 0.0040(18) -0.0052(16) S2 0.040(3) 0.072(3) 0.053(3) 0.006(2) 0.011(2) -0.011(2) S3 0.033(2) 0.073(3) 0.053(3) -0.010(2) 0.011(2) -0.004(2) S4 0.028(2) 0.056(3) 0.058(3) -0.006(2) 0.001(2) -0.0018(18) S5 0.030(2) 0.037(2) 0.055(3) 0.0025(18) 0.002(2) -0.0003(16) S6 0.034(2) 0.051(2) 0.056(3) 0.011(2) 0.006(2) -0.0072(19) S7 0.030(2) 0.066(3) 0.045(2) -0.002(2) 0.0036(18) 0.0021(19) S8 0.029(2) 0.047(2) 0.053(3) -0.0056(19) 0.0001(19) 0.0025(17) S11 0.036(2) 0.050(3) 0.058(3) -0.007(2) 0.005(2) -0.003(2) S12 0.035(2) 0.056(3) 0.072(3) -0.003(2) 0.007(2) -0.010(2) S21 0.066(4) 0.109(5) 0.050(3) 0.002(3) 0.015(3) -0.015(3) S22 0.036(2) 0.076(3) 0.048(2) -0.002(2) 0.002(2) -0.009(2) S31 0.033(2) 0.062(3) 0.070(3) -0.012(2) 0.001(2) 0.011(2) S32 0.037(2) 0.050(2) 0.051(2) -0.004(2) 0.0007(19) 0.0025(19) S41 0.040(2) 0.051(3) 0.057(3) -0.001(2) 0.008(2) -0.004(2) S42 0.032(2) 0.056(3) 0.077(3) -0.002(2) 0.009(2) -0.009(2) S51 0.047(3) 0.100(5) 0.047(3) 0.015(3) -0.003(2) 0.001(3) S52 0.037(3) 0.064(3) 0.063(3) 0.005(2) -0.007(2) -0.001(2) S61 0.037(2) 0.051(3) 0.061(3) -0.003(2) 0.002(2) 0.0075(19) S62 0.043(2) 0.049(2) 0.048(2) 0.0046(19) 0.0058(19) 0.003(2) P1 0.037(3) 0.048(3) 0.076(4) -0.006(2) -0.003(2) -0.004(2) P2 0.055(3) 0.091(4) 0.045(3) -0.002(3) -0.001(2) -0.001(3) P3 0.042(3) 0.056(3) 0.065(3) -0.002(2) -0.001(2) 0.010(2) P4 0.042(3) 0.045(3) 0.070(3) -0.009(2) 0.003(2) -0.001(2) P5 0.045(3) 0.089(4) 0.059(3) 0.005(3) -0.012(3) 0.004(3) P6 0.046(3) 0.047(3) 0.053(3) 0.005(2) -0.003(2) 0.006(2) O1 0.038(7) 0.048(7) 0.068(9) 0.021(6) 0.012(7) -0.014(6) O2 0.039(7) 0.072(10) 0.063(9) 0.011(8) 0.002(7) -0.012(7) O3 0.038(7) 0.046(7) 0.078(10) 0.005(7) -0.001(7) 0.009(6) O4 0.037(7) 0.059(8) 0.074(10) 0.016(8) 0.008(7) 0.003(6) O11 0.030(7) 0.069(10) 0.095(12) -0.009(8) -0.014(7) 0.002(7) O12 0.055(9) 0.061(9) 0.079(11) -0.014(8) -0.012(8) 0.007(7) O21 0.063(10) 0.091(12) 0.048(8) 0.000(8) 0.001(7) 0.005(9) O22 0.064(10) 0.090(12) 0.054(8) -0.008(8) -0.010(7) -0.002(9) O31 0.063(10) 0.052(9) 0.101(14) 0.016(9) 0.008(9) 0.004(8) O32 0.052(9) 0.072(10) 0.072(10) 0.005(8) 0.002(8) 0.010(8) O41 0.052(9) 0.066(10) 0.085(11) -0.018(8) -0.011(8) 0.004(8) O42 0.045(8) 0.046(8) 0.098(12) -0.008(8) 0.002(8) 0.010(6) O51 0.053(10) 0.099(14) 0.074(11) 0.016(10) -0.011(8) 0.010(10) O52 0.068(12) 0.114(15) 0.075(11) -0.009(11) -0.018(9) 0.014(11) O61 0.062(10) 0.046(8) 0.082(11) 0.015(7) 0.002(8) 0.005(7) O62 0.070(11) 0.072(11) 0.095(14) -0.021(10) -0.022(10) 0.013(9) N1 0.033(8) 0.037(7) 0.061(10) 0.006(7) 0.003(7) 0.001(6) N2 0.029(8) 0.050(9) 0.059(9) 0.005(7) 0.000(7) -0.001(7) C1 0.025(8) 0.072(14) 0.053(11) 0.009(10) 0.001(8) -0.004(8) C2 0.044(13) 0.089(18) 0.13(3) 0.019(18) 0.028(15) -0.002(12) C3 0.029(9) 0.057(11) 0.052(10) -0.009(9) -0.002(8) 0.009(8) C4 0.030(8) 0.034(8) 0.055(10) -0.013(8) 0.008(8) -0.015(6) C5 0.039(10) 0.049(10) 0.054(10) 0.008(8) 0.013(8) 0.007(8) C6 0.031(9) 0.045(9) 0.063(12) -0.004(9) 0.006(8) 0.009(7) C7 0.053(13) 0.045(11) 0.079(16) 0.020(11) 0.016(12) 0.006(10) C8 0.049(12) 0.053(11) 0.084(16) 0.015(11) 0.016(12) -0.001(10) C11 0.042(12) 0.065(13) 0.077(15) 0.003(11) 0.008(11) -0.004(10) C12 0.029(10) 0.12(2) 0.058(13) 0.007(13) 0.004(9) -0.007(11) C13 0.081(16) 0.045(11) 0.064(13) 0.006(10) 0.015(12) 0.020(11) C14 0.066(17) 0.10(2) 0.10(2) 0.031(17) 0.022(16) 0.023(15) C21 0.12(3) 0.11(3) 0.056(15) 0.006(15) -0.018(17) 0.02(2) C22A 0.15(6) 0.07(4) 0.05(3) 0.01(2) -0.01(3) -0.06(4) C22B 0.09(4) 0.08(4) 0.10(4) 0.03(3) 0.04(3) 0.04(3) C23 0.060(15) 0.10(2) 0.060(13) 0.006(13) -0.008(11) 0.002(13) C24 0.26(6) 0.17(4) 0.065(18) -0.01(2) 0.01(3) 0.15(4) C31 0.066(17) 0.062(15) 0.13(3) -0.018(16) -0.021(17) 0.001(13) C32A 0.06(3) 0.04(2) 0.08(3) -0.01(2) -0.02(3) 0.01(2) C32B 0.07(4) 0.08(3) 0.10(4) 0.01(3) -0.02(3) -0.02(3) C33 0.046(13) 0.081(17) 0.10(2) 0.023(15) -0.008(13) -0.010(12) C34 0.066(17) 0.12(3) 0.072(17) -0.016(16) -0.011(14) 0.004(16) C41 0.059(15) 0.088(18) 0.084(18) -0.025(15) -0.014(13) 0.026(14) C42 0.060(17) 0.13(3) 0.09(2) -0.020(19) -0.009(15) 0.039(18) C43 0.042(13) 0.12(2) 0.10(2) 0.001(19) 0.013(14) 0.025(14) C44 0.09(2) 0.078(18) 0.15(3) 0.06(2) 0.05(2) 0.045(16) C51 0.054(15) 0.14(3) 0.070(17) 0.032(18) 0.016(13) 0.026(18) C52 0.22(5) 0.11(3) 0.08(2) 0.01(2) 0.01(3) -0.01(3) C53 0.11(3) 0.17(4) 0.11(3) 0.00(3) -0.04(2) 0.02(3) C54 0.13(3) 0.10(3) 0.12(3) 0.00(2) -0.05(3) -0.02(2) C61 0.059(13) 0.039(10) 0.092(17) -0.003(10) -0.005(12) 0.010(10) C62 0.10(2) 0.10(2) 0.09(2) 0.006(17) -0.017(19) 0.047(19) C63 0.08(2) 0.10(2) 0.14(3) -0.01(2) -0.01(2) 0.027(19) C64 0.074(18) 0.12(3) 0.074(18) -0.018(17) -0.019(15) 0.008(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 Mo1 Mo2 2.681(2) . ? Mo1 Mo3 2.764(2) . ? Mo1 S1 2.328(4) . ? Mo1 S2 2.286(5) . ? Mo1 S4 2.298(5) . ? Mo1 S11 2.538(5) . ? Mo1 S12 2.550(5) . ? Mo1 O1 2.199(14) . ? Mo2 Mo3 2.746(2) . ? Mo2 S1 2.344(5) . ? Mo2 S2 2.297(5) . ? Mo2 S3 2.298(6) . ? Mo2 S21 2.543(6) . ? Mo2 S22 2.516(5) . ? Mo2 O2 2.212(16) . ? Mo3 S1 2.340(5) . ? Mo3 S3 2.291(5) . ? Mo3 S4 2.284(5) . ? Mo3 S31 2.567(5) . ? Mo3 S32 2.521(5) . ? Mo3 N1 2.412(15) . ? Mo4 Mo5 2.676(2) . ? Mo4 Mo6 2.759(2) . ? Mo4 S5 2.332(4) . ? Mo4 S6 2.285(5) . ? Mo4 S8 2.291(5) . ? Mo4 S41 2.552(5) . ? Mo4 S42 2.532(5) . ? Mo4 O3 2.202(13) . ? Mo5 Mo6 2.755(2) . ? Mo5 S5 2.328(5) . ? Mo5 S6 2.299(5) . ? Mo5 S7 2.302(5) . ? Mo5 S51 2.552(6) . ? Mo5 S52 2.509(5) . ? Mo5 O4 2.220(14) . ? Mo6 S5 2.344(4) . ? Mo6 S7 2.309(5) . ? Mo6 S8 2.272(5) . ? Mo6 S61 2.567(5) . ? Mo6 S62 2.533(5) . ? Mo6 N2 2.413(16) . ? S11 P1 2.008(7) . ? S12 P1 1.988(8) . ? S21 P2 1.996(9) . ? S22 P2 2.006(8) . ? S31 P3 2.003(8) . ? S32 P3 2.004(7) . ? S41 P4 2.004(7) . ? S42 P4 1.987(8) . ? S51 P5 1.986(9) . ? S52 P5 2.016(9) . ? S61 P6 1.999(8) . ? S62 P6 2.003(7) . ? P1 O11 1.585(17) . ? P1 O12 1.575(16) . ? P2 O21 1.576(18) . ? P2 O22 1.541(18) . ? P3 O31 1.576(17) . ? P3 O32 1.575(18) . ? P4 O41 1.555(18) . ? P4 O42 1.585(15) . ? P5 O51 1.585(17) . ? P5 O52 1.58(2) . ? P6 O61 1.573(16) . ? P6 O62 1.555(18) . ? O1 C1 1.26(3) . ? O2 C1 1.28(3) . ? O3 C7 1.23(3) . ? O4 C7 1.27(3) . ? O11 C11 1.49(3) . ? O12 C13 1.47(3) . ? O21 C21 1.42(4) . ? O22 C23 1.46(3) . ? O31 C31 1.447(7) . ? O32 C33 1.44(3) . ? O41 C41 1.50(3) . ? O42 C43 1.447(7) . ? O51 C51 1.42(4) . ? O52 C53 1.44(4) . ? O61 C61 1.44(2) . ? O62 C63 1.446(7) . ? N1 C3 1.34(3) . ? N1 C6 1.34(2) . ? N2 C4 1.33(2) . ? N2 C5 1.34(3) . ? C1 C2 1.49(3) . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 H3 0.9300 . ? C3 C4 1.40(2) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C5 C6 1.37(3) . ? C6 H6 0.9300 . ? C7 C8 1.48(3) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C11 C12 1.502(7) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C13 C14 1.499(7) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C21 H21D 0.9700 . ? C21 C22A 1.498(7) . ? C21 C22B 1.498(7) . ? C22A H22A 0.9600 . ? C22A H22B 0.9600 . ? C22A H22C 0.9600 . ? C22B H22D 0.9600 . ? C22B H22E 0.9600 . ? C22B H22F 0.9600 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 C24 1.496(7) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C31 H31C 0.9700 . ? C31 H31D 0.9700 . ? C31 C32A 1.501(7) . ? C31 C32B 1.499(7) . ? C32A H32A 0.9600 . ? C32A H32B 0.9600 . ? C32A H32C 0.9600 . ? C32B H32D 0.9600 . ? C32B H32E 0.9600 . ? C32B H32F 0.9600 . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C33 C34 1.498(7) . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C41 C42 1.499(7) . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C43 C44 1.501(7) . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C51 C52 1.497(7) . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C53 C54 1.498(7) . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? C61 H61A 0.9700 . ? C61 H61B 0.9700 . ? C61 C62 1.499(7) . ? C62 H62A 0.9600 . ? C62 H62B 0.9600 . ? C62 H62C 0.9600 . ? C63 H63A 0.9700 . ? C63 H63B 0.9700 . ? C63 C64 1.498(7) . ? C64 H64A 0.9600 . ? C64 H64B 0.9600 . ? C64 H64C 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 Mo2 Mo1 Mo3 60.54(6) . . ? S1 Mo1 Mo2 55.26(13) . . ? S1 Mo1 Mo3 53.89(11) . . ? S1 Mo1 S11 85.45(17) . . ? S1 Mo1 S12 159.58(17) . . ? S2 Mo1 Mo2 54.38(14) . . ? S2 Mo1 Mo3 96.14(15) . . ? S2 Mo1 S1 109.2(2) . . ? S2 Mo1 S4 93.0(2) . . ? S2 Mo1 S11 160.0(2) . . ? S2 Mo1 S12 84.1(2) . . ? S4 Mo1 Mo2 99.46(14) . . ? S4 Mo1 Mo3 52.67(12) . . ? S4 Mo1 S1 104.59(17) . . ? S4 Mo1 S11 96.33(19) . . ? S4 Mo1 S12 89.59(18) . . ? S11 Mo1 Mo2 140.18(12) . . ? S11 Mo1 Mo3 103.57(13) . . ? S11 Mo1 S12 78.34(18) . . ? S12 Mo1 Mo2 137.70(15) . . ? S12 Mo1 Mo3 142.26(14) . . ? O1 Mo1 Mo2 85.3(4) . . ? O1 Mo1 Mo3 135.0(4) . . ? O1 Mo1 S1 83.3(3) . . ? O1 Mo1 S2 84.5(4) . . ? O1 Mo1 S4 172.1(4) . . ? O1 Mo1 S11 83.8(4) . . ? O1 Mo1 S12 82.7(4) . . ? Mo1 Mo2 Mo3 61.22(6) . . ? S1 Mo2 Mo1 54.70(11) . . ? S1 Mo2 Mo3 54.04(12) . . ? S1 Mo2 S21 160.7(2) . . ? S1 Mo2 S22 85.42(16) . . ? S2 Mo2 Mo1 54.00(14) . . ? S2 Mo2 Mo3 96.38(15) . . ? S2 Mo2 S1 108.30(18) . . ? S2 Mo2 S3 92.2(2) . . ? S2 Mo2 S21 84.7(2) . . ? S2 Mo2 S22 158.8(2) . . ? S3 Mo2 Mo1 99.61(15) . . ? S3 Mo2 Mo3 53.15(14) . . ? S3 Mo2 S1 105.69(18) . . ? S3 Mo2 S21 87.6(2) . . ? S3 Mo2 S22 99.74(19) . . ? S21 Mo2 Mo1 138.04(17) . . ? S21 Mo2 Mo3 140.74(19) . . ? S22 Mo2 Mo1 139.11(14) . . ? S22 Mo2 Mo3 104.84(14) . . ? S22 Mo2 S21 78.4(2) . . ? O2 Mo2 Mo1 83.7(4) . . ? O2 Mo2 Mo3 134.6(4) . . ? O2 Mo2 S1 82.8(4) . . ? O2 Mo2 S2 83.2(4) . . ? O2 Mo2 S3 171.3(4) . . ? O2 Mo2 S21 84.6(5) . . ? O2 Mo2 S22 82.5(4) . . ? Mo2 Mo3 Mo1 58.24(6) . . ? S1 Mo3 Mo1 53.50(11) . . ? S1 Mo3 Mo2 54.19(13) . . ? S1 Mo3 S31 160.69(18) . . ? S1 Mo3 S32 85.10(17) . . ? S1 Mo3 N1 84.2(4) . . ? S3 Mo3 Mo1 97.42(16) . . ? S3 Mo3 Mo2 53.35(15) . . ? S3 Mo3 S1 106.0(2) . . ? S3 Mo3 S31 86.8(2) . . ? S3 Mo3 S32 159.56(19) . . ? S3 Mo3 N1 84.3(4) . . ? S4 Mo3 Mo1 53.14(13) . . ? S4 Mo3 Mo2 97.98(15) . . ? S4 Mo3 S1 104.67(17) . . ? S4 Mo3 S3 97.62(19) . . ? S4 Mo3 S31 87.43(18) . . ? S4 Mo3 S32 95.95(19) . . ? S4 Mo3 N1 169.9(4) . . ? S31 Mo3 Mo1 140.57(13) . . ? S31 Mo3 Mo2 140.12(15) . . ? S32 Mo3 Mo1 102.95(12) . . ? S32 Mo3 Mo2 139.09(12) . . ? S32 Mo3 S31 78.62(18) . . ? N1 Mo3 Mo1 136.6(4) . . ? N1 Mo3 Mo2 91.1(4) . . ? N1 Mo3 S31 82.8(4) . . ? N1 Mo3 S32 79.8(4) . . ? Mo5 Mo4 Mo6 60.90(6) . . ? S5 Mo4 Mo5 54.89(14) . . ? S5 Mo4 Mo6 54.04(11) . . ? S5 Mo4 S41 85.69(17) . . ? S5 Mo4 S42 159.37(18) . . ? S6 Mo4 Mo5 54.53(13) . . ? S6 Mo4 Mo6 97.23(14) . . ? S6 Mo4 S5 108.87(19) . . ? S6 Mo4 S8 94.60(18) . . ? S6 Mo4 S41 158.25(17) . . ? S6 Mo4 S42 83.54(18) . . ? S8 Mo4 Mo5 99.91(13) . . ? S8 Mo4 Mo6 52.47(12) . . ? S8 Mo4 S5 104.57(16) . . ? S8 Mo4 S41 97.25(18) . . ? S8 Mo4 S42 90.34(18) . . ? S41 Mo4 Mo5 139.80(12) . . ? S41 Mo4 Mo6 104.45(12) . . ? S42 Mo4 Mo5 137.28(15) . . ? S42 Mo4 Mo6 142.80(14) . . ? S42 Mo4 S41 78.23(17) . . ? O3 Mo4 Mo5 84.7(4) . . ? O3 Mo4 Mo6 134.5(4) . . ? O3 Mo4 S5 82.5(4) . . ? O3 Mo4 S6 83.7(4) . . ? O3 Mo4 S8 172.9(4) . . ? O3 Mo4 S41 82.4(5) . . ? O3 Mo4 S42 82.7(4) . . ? Mo4 Mo5 Mo6 61.04(6) . . ? S5 Mo5 Mo4 55.01(12) . . ? S5 Mo5 Mo6 54.12(11) . . ? S5 Mo5 S51 159.95(18) . . ? S5 Mo5 S52 85.71(18) . . ? S6 Mo5 Mo4 54.05(13) . . ? S6 Mo5 Mo6 97.00(14) . . ? S6 Mo5 S5 108.51(18) . . ? S6 Mo5 S7 93.30(18) . . ? S6 Mo5 S51 83.8(2) . . ? S6 Mo5 S52 158.01(19) . . ? S7 Mo5 Mo4 99.84(14) . . ? S7 Mo5 Mo6 53.42(13) . . ? S7 Mo5 S5 105.90(17) . . ? S7 Mo5 S51 88.7(2) . . ? S7 Mo5 S52 98.90(19) . . ? S51 Mo5 Mo4 137.12(17) . . ? S51 Mo5 Mo6 142.10(17) . . ? S52 Mo5 Mo4 139.81(15) . . ? S52 Mo5 Mo6 104.96(14) . . ? S52 Mo5 S51 78.3(2) . . ? O4 Mo5 Mo4 83.1(5) . . ? O4 Mo5 Mo6 133.9(5) . . ? O4 Mo5 S5 82.3(4) . . ? O4 Mo5 S6 82.0(4) . . ? O4 Mo5 S7 171.6(4) . . ? O4 Mo5 S51 83.9(5) . . ? O4 Mo5 S52 83.5(4) . . ? Mo5 Mo6 Mo4 58.06(6) . . ? S5 Mo6 Mo4 53.63(11) . . ? S5 Mo6 Mo5 53.60(13) . . ? S5 Mo6 S61 160.96(17) . . ? S5 Mo6 S62 85.66(17) . . ? S5 Mo6 N2 83.9(4) . . ? S7 Mo6 Mo4 97.31(14) . . ? S7 Mo6 Mo5 53.18(13) . . ? S7 Mo6 S5 105.15(18) . . ? S7 Mo6 S61 86.62(18) . . ? S7 Mo6 S62 159.12(18) . . ? S7 Mo6 N2 83.4(4) . . ? S8 Mo6 Mo4 53.12(12) . . ? S8 Mo6 Mo5 98.12(14) . . ? S8 Mo6 S5 104.81(16) . . ? S8 Mo6 S7 98.27(18) . . ? S8 Mo6 S61 87.83(16) . . ? S8 Mo6 S62 96.03(18) . . ? S8 Mo6 N2 170.2(4) . . ? S61 Mo6 Mo4 140.95(13) . . ? S61 Mo6 Mo5 139.78(14) . . ? S62 Mo6 Mo4 103.44(12) . . ? S62 Mo6 Mo5 139.06(12) . . ? S62 Mo6 S61 78.78(17) . . ? N2 Mo6 Mo4 136.4(4) . . ? N2 Mo6 Mo5 90.6(4) . . ? N2 Mo6 S61 82.6(4) . . ? N2 Mo6 S62 80.0(4) . . ? Mo1 S1 Mo2 70.04(14) . . ? Mo1 S1 Mo3 72.61(13) . . ? Mo3 S1 Mo2 71.77(14) . . ? Mo1 S2 Mo2 71.62(15) . . ? Mo3 S3 Mo2 73.50(16) . . ? Mo3 S4 Mo1 74.19(15) . . ? Mo4 S5 Mo6 72.32(13) . . ? Mo5 S5 Mo4 70.09(14) . . ? Mo5 S5 Mo6 72.27(14) . . ? Mo4 S6 Mo5 71.42(14) . . ? Mo5 S7 Mo6 73.40(15) . . ? Mo6 S8 Mo4 74.41(15) . . ? P1 S11 Mo1 87.2(2) . . ? P1 S12 Mo1 87.4(2) . . ? P2 S21 Mo2 87.5(3) . . ? P2 S22 Mo2 88.0(3) . . ? P3 S31 Mo3 86.2(2) . . ? P3 S32 Mo3 87.5(2) . . ? P4 S41 Mo4 86.9(2) . . ? P4 S42 Mo4 87.8(2) . . ? P5 S51 Mo5 87.5(3) . . ? P5 S52 Mo5 88.1(3) . . ? P6 S61 Mo6 85.7(2) . . ? P6 S62 Mo6 86.5(2) . . ? S12 P1 S11 107.1(3) . . ? O11 P1 S11 113.3(7) . . ? O11 P1 S12 113.4(7) . . ? O12 P1 S11 113.1(7) . . ? O12 P1 S12 113.7(8) . . ? O12 P1 O11 96.3(9) . . ? S21 P2 S22 106.1(3) . . ? O21 P2 S21 113.8(8) . . ? O21 P2 S22 112.2(7) . . ? O22 P2 S21 114.6(8) . . ? O22 P2 S22 113.2(8) . . ? O22 P2 O21 97.2(10) . . ? S31 P3 S32 107.1(3) . . ? O31 P3 S31 115.3(8) . . ? O31 P3 S32 108.0(7) . . ? O32 P3 S31 113.3(7) . . ? O32 P3 S32 111.2(7) . . ? O32 P3 O31 101.9(10) . . ? S42 P4 S41 107.0(3) . . ? O41 P4 S41 113.9(8) . . ? O41 P4 S42 113.6(7) . . ? O41 P4 O42 95.5(9) . . ? O42 P4 S41 113.1(6) . . ? O42 P4 S42 113.7(7) . . ? S51 P5 S52 106.0(4) . . ? O51 P5 S51 112.4(8) . . ? O51 P5 S52 113.3(8) . . ? O52 P5 S51 112.1(9) . . ? O52 P5 S52 114.8(9) . . ? O52 P5 O51 98.4(11) . . ? S61 P6 S62 108.0(3) . . ? O61 P6 S61 113.2(7) . . ? O61 P6 S62 109.6(7) . . ? O62 P6 S61 113.2(9) . . ? O62 P6 S62 111.7(7) . . ? O62 P6 O61 101.1(10) . . ? C1 O1 Mo1 122.4(14) . . ? C1 O2 Mo2 123.1(13) . . ? C7 O3 Mo4 123.9(15) . . ? C7 O4 Mo5 123.9(15) . . ? C11 O11 P1 118.8(13) . . ? C13 O12 P1 118.1(13) . . ? C21 O21 P2 119.9(17) . . ? C23 O22 P2 119.5(14) . . ? C31 O31 P3 122.9(17) . . ? C33 O32 P3 119.0(14) . . ? C41 O41 P4 116.7(14) . . ? C43 O42 P4 119.4(15) . . ? C51 O51 P5 120.0(17) . . ? C53 O52 P5 117.6(18) . . ? C61 O61 P6 122.3(15) . . ? C63 O62 P6 123.7(16) . . ? C3 N1 Mo3 120.4(13) . . ? C6 N1 Mo3 122.4(13) . . ? C6 N1 C3 115.8(17) . . ? C4 N2 Mo6 119.3(12) . . ? C4 N2 C5 116.4(16) . . ? C5 N2 Mo6 123.6(13) . . ? O1 C1 O2 125.5(19) . . ? O1 C1 C2 121(2) . . ? O2 C1 C2 113(2) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2B 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N1 C3 H3 118.9 . . ? N1 C3 C4 122.1(17) . . ? C4 C3 H3 118.9 . . ? N2 C4 C3 120.9(16) . . ? N2 C4 H4 119.6 . . ? C3 C4 H4 119.6 . . ? N2 C5 H5 118.5 . . ? N2 C5 C6 122.9(17) . . ? C6 C5 H5 118.5 . . ? N1 C6 C5 121.7(18) . . ? N1 C6 H6 119.1 . . ? C5 C6 H6 119.1 . . ? O3 C7 O4 124(2) . . ? O3 C7 C8 119(2) . . ? O4 C7 C8 117(2) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O11 C11 H11A 110.5 . . ? O11 C11 H11B 110.5 . . ? O11 C11 C12 106.1(19) . . ? H11A C11 H11B 108.7 . . ? C12 C11 H11A 110.5 . . ? C12 C11 H11B 110.5 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O12 C13 H13A 110.8 . . ? O12 C13 H13B 110.8 . . ? O12 C13 C14 105(2) . . ? H13A C13 H13B 108.9 . . ? C14 C13 H13A 110.8 . . ? C14 C13 H13B 110.8 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14B 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O21 C21 H21A 107.6 . . ? O21 C21 H21B 107.6 . . ? O21 C21 H21C 110.3 . . ? O21 C21 H21D 110.3 . . ? H21A C21 H21B 107.0 . . ? H21C C21 H21D 108.6 . . ? C22A C21 O21 119(4) . . ? C22A C21 H21A 107.6 . . ? C22A C21 H21B 107.6 . . ? C22B C21 O21 107(3) . . ? C22B C21 H21C 110.3 . . ? C22B C21 H21D 110.3 . . ? C21 C22A H22A 109.5 . . ? C21 C22A H22B 109.5 . . ? C21 C22A H22C 109.5 . . ? H22A C22A H22B 109.5 . . ? H22A C22A H22C 109.5 . . ? H22B C22A H22C 109.5 . . ? C21 C22B H22D 109.5 . . ? C21 C22B H22E 109.5 . . ? C21 C22B H22F 109.5 . . ? H22D C22B H22E 109.5 . . ? H22D C22B H22F 109.5 . . ? H22E C22B H22F 109.5 . . ? O22 C23 H23A 110.7 . . ? O22 C23 H23B 110.7 . . ? H23A C23 H23B 108.8 . . ? C24 C23 O22 105(2) . . ? C24 C23 H23A 110.7 . . ? C24 C23 H23B 110.7 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O31 C31 H31A 111.5 . . ? O31 C31 H31B 111.5 . . ? O31 C31 H31C 107.2 . . ? O31 C31 H31D 107.2 . . ? O31 C31 C32A 101(2) . . ? H31A C31 H31B 109.3 . . ? H31C C31 H31D 106.9 . . ? C32A C31 H31A 111.5 . . ? C32A C31 H31B 111.5 . . ? C32B C31 O31 120(3) . . ? C32B C31 H31C 107.2 . . ? C32B C31 H31D 107.2 . . ? C31 C32A H32A 109.5 . . ? C31 C32A H32B 109.5 . . ? C31 C32A H32C 109.5 . . ? H32A C32A H32B 109.5 . . ? H32A C32A H32C 109.5 . . ? H32B C32A H32C 109.5 . . ? C31 C32B H32D 109.5 . . ? C31 C32B H32E 109.5 . . ? C31 C32B H32F 109.5 . . ? H32D C32B H32E 109.5 . . ? H32D C32B H32F 109.5 . . ? H32E C32B H32F 109.5 . . ? O32 C33 H33A 110.3 . . ? O32 C33 H33B 110.3 . . ? O32 C33 C34 107(2) . . ? H33A C33 H33B 108.5 . . ? C34 C33 H33A 110.3 . . ? C34 C33 H33B 110.3 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34B 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? O41 C41 H41A 110.7 . . ? O41 C41 H41B 110.7 . . ? H41A C41 H41B 108.8 . . ? C42 C41 O41 105(2) . . ? C42 C41 H41A 110.7 . . ? C42 C41 H41B 110.7 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42B 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? O42 C43 H43A 110.7 . . ? O42 C43 H43B 110.7 . . ? O42 C43 C44 105.2(17) . . ? H43A C43 H43B 108.8 . . ? C44 C43 H43A 110.7 . . ? C44 C43 H43B 110.7 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44B 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? O51 C51 H51A 109.1 . . ? O51 C51 H51B 109.1 . . ? H51A C51 H51B 107.9 . . ? C52 C51 O51 112(3) . . ? C52 C51 H51A 109.1 . . ? C52 C51 H51B 109.1 . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52B 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? O52 C53 H53A 109.7 . . ? O52 C53 H53B 109.7 . . ? H53A C53 H53B 108.2 . . ? C54 C53 O52 110(3) . . ? C54 C53 H53A 109.7 . . ? C54 C53 H53B 109.7 . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54B 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? O61 C61 H61A 109.4 . . ? O61 C61 H61B 109.4 . . ? O61 C61 C62 111.2(19) . . ? H61A C61 H61B 108.0 . . ? C62 C61 H61A 109.4 . . ? C62 C61 H61B 109.4 . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62B 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? O62 C63 H63A 109.5 . . ? O62 C63 H63B 109.5 . . ? H63A C63 H63B 108.0 . . ? C64 C63 O62 111(2) . . ? C64 C63 H63A 109.5 . . ? C64 C63 H63B 109.5 . . ? C63 C64 H64A 109.5 . . ? C63 C64 H64B 109.5 . . ? C63 C64 H64C 109.5 . . ? H64A C64 H64B 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Mo1 O1 C1 O2 0(3) . . . . ? Mo1 O1 C1 C2 -176.8(15) . . . . ? Mo2 O2 C1 O1 1(3) . . . . ? Mo2 O2 C1 C2 177.7(13) . . . . ? Mo3 N1 C3 C4 -166.7(15) . . . . ? Mo3 N1 C6 C5 167.9(14) . . . . ? Mo4 O3 C7 O4 -5(3) . . . . ? Mo4 O3 C7 C8 173.6(14) . . . . ? Mo5 O4 C7 O3 4(3) . . . . ? Mo5 O4 C7 C8 -174.9(13) . . . . ? Mo6 N2 C4 C3 -171.6(14) . . . . ? Mo6 N2 C5 C6 172.7(15) . . . . ? S11 P1 O11 C11 63.2(17) . . . . ? S11 P1 O12 C13 -60.4(18) . . . . ? S12 P1 O11 C11 -59.1(17) . . . . ? S12 P1 O12 C13 62.0(17) . . . . ? S21 P2 O21 C21 -56(2) . . . . ? S21 P2 O22 C23 62.1(19) . . . . ? S22 P2 O21 C21 64(2) . . . . ? S22 P2 O22 C23 -59.7(19) . . . . ? S31 P3 O31 C31 47(2) . . . . ? S31 P3 O32 C33 60.5(19) . . . . ? S32 P3 O31 C31 166.8(19) . . . . ? S32 P3 O32 C33 -60.2(19) . . . . ? S41 P4 O41 C41 -66(2) . . . . ? S41 P4 O42 C43 61.2(19) . . . . ? S42 P4 O41 C41 57(2) . . . . ? S42 P4 O42 C43 -61.0(19) . . . . ? S51 P5 O51 C51 67(2) . . . . ? S51 P5 O52 C53 -56(3) . . . . ? S52 P5 O51 C51 -53(2) . . . . ? S52 P5 O52 C53 65(3) . . . . ? S61 P6 O61 C61 -42.3(18) . . . . ? S61 P6 O62 C63 -69(2) . . . . ? S62 P6 O61 C61 -162.8(14) . . . . ? S62 P6 O62 C63 53(2) . . . . ? P1 O11 C11 C12 175.7(15) . . . . ? P1 O12 C13 C14 160.6(17) . . . . ? P2 O21 C21 C22A 125(4) . . . . ? P2 O21 C21 C22B 178(3) . . . . ? P2 O22 C23 C24 -153(3) . . . . ? P3 O31 C31 C32A 122(3) . . . . ? P3 O31 C31 C32B 46(4) . . . . ? P3 O32 C33 C34 170.9(18) . . . . ? P4 O41 C41 C42 -174(2) . . . . ? P4 O42 C43 C44 -174.4(18) . . . . ? P5 O51 C51 C52 -142(3) . . . . ? P5 O52 C53 C54 -160(3) . . . . ? P6 O61 C61 C62 -89(3) . . . . ? P6 O62 C63 C64 -164(2) . . . . ? O11 P1 O12 C13 -179.0(17) . . . . ? O12 P1 O11 C11 -178.4(16) . . . . ? O21 P2 O22 C23 -177.5(18) . . . . ? O22 P2 O21 C21 -177(2) . . . . ? O31 P3 O32 C33 -175.0(18) . . . . ? O32 P3 O31 C31 -76(2) . . . . ? O41 P4 O42 C43 -179.8(19) . . . . ? O42 P4 O41 C41 176.0(19) . . . . ? O51 P5 O52 C53 -174(3) . . . . ? O52 P5 O51 C51 -175(2) . . . . ? O61 P6 O62 C63 170(2) . . . . ? O62 P6 O61 C61 79.1(18) . . . . ? N1 C3 C4 N2 0(3) . . . . ? N2 C5 C6 N1 -3(3) . . . . ? C3 N1 C6 C5 1(3) . . . . ? C4 N2 C5 C6 3(3) . . . . ? C5 N2 C4 C3 -1(3) . . . . ? C6 N1 C3 C4 0(3) . . . . ? loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 0 1 0 0.0655 -0.0000 1.0000 -0.0000 0.0135 0.0397 0.0607 -1 0 0 0.1417 -1.0000 -0.0000 0.0000 0.0404 0.0803 -0.0614 1 0 0 0.1417 1.0000 0.0000 -0.0000 -0.0404 -0.0803 0.0614 0 0 1 0.0215 0.0000 -0.0000 1.0000 -0.0560 0.0251 -0.0040 0 -1 0 0.0655 0.0000 -1.0000 0.0000 -0.0135 -0.0397 -0.0607 0 0 -1 0.0215 -0.0000 0.0000 -1.0000 0.0560 -0.0251 0.0040 _database_code_depnum_ccdc_archive 'CCDC 888490'