# 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_compound1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H140 Cr Mo6 N5 O26' _chemical_formula_weight 2023.47 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' Cr Cr 0.3209 0.6236 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 2(1)/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 25.3159(8) _cell_length_b 13.4971(3) _cell_length_c 24.9443(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.20 _cell_angle_gamma 90.00 _cell_volume 8523.3(5) _cell_formula_units_Z 4 _cell_measurement_temperature 102(2) _cell_measurement_reflns_used 16748 _cell_measurement_theta_min 0.838 _cell_measurement_theta_max 0.902 _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.577 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4172 _exptl_absorpt_coefficient_mu 1.049 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8419 _exptl_absorpt_correction_T_max 0.9024 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 102(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.0971 _diffrn_reflns_number 56831 _diffrn_reflns_av_R_equivalents 0.0610 _diffrn_reflns_av_sigmaI/netI 0.0722 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 26.00 _reflns_number_total 16649 _reflns_number_gt 14924 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _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 ; XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution ; SHELXS, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0245P)^2^+3.7038P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16649 _refine_ls_number_parameters 941 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0498 _refine_ls_R_factor_gt 0.0405 _refine_ls_wR_factor_ref 0.0887 _refine_ls_wR_factor_gt 0.0806 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_restrained_S_all 1.088 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.587890(19) 1.12634(3) 0.426834(19) 0.01525(10) Uani 1 1 d . . . Mo2 Mo 0.528763(18) 0.92597(3) 0.375452(19) 0.01444(10) Uani 1 1 d . . . Mo3 Mo 0.439885(19) 0.79996(3) 0.44858(2) 0.01761(11) Uani 1 1 d . . . Cr1 Cr 0.5000 1.0000 0.5000 0.0100(2) Uani 1 2 d S . . O1 O 0.45958(12) 0.9683(2) 0.43456(14) 0.0122(7) Uani 1 1 d . . . O2 O 0.43600(12) 1.0323(2) 0.54051(14) 0.0116(7) Uani 1 1 d . . . O3 O 0.51119(14) 1.1383(2) 0.47924(15) 0.0158(8) Uani 1 1 d . . . O4 O 0.39076(15) 0.8570(3) 0.49918(15) 0.0213(9) Uani 1 1 d . . . O5 O 0.50713(14) 0.8091(2) 0.41311(14) 0.0167(8) Uani 1 1 d . . . O6 O 0.53787(14) 1.0674(2) 0.37830(15) 0.0168(8) Uani 1 1 d . . . O7 O 0.58409(16) 1.2457(2) 0.40487(15) 0.0236(9) Uani 1 1 d . . . O8 O 0.64538(15) 1.0818(3) 0.40188(16) 0.0227(9) Uani 1 1 d . . . O9 O 0.58920(15) 0.8882(2) 0.35353(15) 0.0205(9) Uani 1 1 d . . . O10 O 0.48789(15) 0.9236(2) 0.31992(16) 0.0205(9) Uani 1 1 d . . . O11 O 0.39680(16) 0.7943(3) 0.39638(16) 0.0321(11) Uani 1 1 d . . . O12 O 0.44517(17) 0.6813(3) 0.47132(16) 0.0305(10) Uani 1 1 d . . . C1 C 0.4192(2) 1.0382(4) 0.4193(2) 0.0209(12) Uani 1 1 d . . . H1A H 0.3848 1.0033 0.4175 0.025 Uiso 1 1 calc R . . H1B H 0.4272 1.0639 0.3830 0.025 Uiso 1 1 calc R . . C2 C 0.3976(2) 1.0950(4) 0.5138(2) 0.0196(12) Uani 1 1 d . . . H2A H 0.3916 1.1549 0.5358 0.024 Uiso 1 1 calc R . . H2B H 0.3636 1.0589 0.5113 0.024 Uiso 1 1 calc R . . C3 C 0.4639(2) 1.1897(4) 0.4591(2) 0.0229(13) Uani 1 1 d . . . H3A H 0.4711 1.2133 0.4222 0.028 Uiso 1 1 calc R . . H3B H 0.4574 1.2487 0.4817 0.028 Uiso 1 1 calc R . . C4 C 0.4141(2) 1.1263(4) 0.4583(2) 0.0205(12) Uani 1 1 d . . . C5 C 0.3686(2) 1.1928(4) 0.4356(2) 0.0283(14) Uani 1 1 d . . . H5A H 0.3787 1.2182 0.4003 0.042 Uiso 1 1 calc R . . H5B H 0.3624 1.2485 0.4600 0.042 Uiso 1 1 calc R . . H5C H 0.3363 1.1534 0.4324 0.042 Uiso 1 1 calc R . . Mo4 Mo -0.082491(19) 1.16138(3) 0.05788(2) 0.01870(11) Uani 1 1 d . . . Mo5 Mo 0.024777(19) 1.07958(3) 0.12477(2) 0.01717(11) Uani 1 1 d . . . Mo6 Mo 0.10545(2) 0.91533(3) 0.06811(2) 0.02086(11) Uani 1 1 d . . . Cr2 Cr 0.0000 1.0000 0.0000 0.0121(2) Uani 1 2 d S . . O13 O -0.05961(14) 0.9414(2) -0.03910(15) 0.0165(8) Uani 1 1 d . . . O14 O 0.03013(14) 0.8699(2) 0.01752(15) 0.0159(8) Uani 1 1 d . . . O15 O -0.03916(13) 1.0078(2) 0.06739(15) 0.0156(8) Uani 1 1 d . . . O16 O -0.01302(14) 1.1835(2) 0.08874(15) 0.0180(9) Uani 1 1 d . . . O17 O 0.05158(14) 0.9458(2) 0.12007(15) 0.0203(9) Uani 1 1 d . . . O18 O 0.12387(14) 0.9135(3) -0.00676(15) 0.0196(9) Uani 1 1 d . . . O19 O 0.11794(16) 0.7962(3) 0.08605(16) 0.0303(10) Uani 1 1 d . . . O20 O 0.15787(15) 0.9824(3) 0.09141(16) 0.0282(10) Uani 1 1 d . . . O21 O 0.07926(15) 1.1439(3) 0.14450(15) 0.0238(9) Uani 1 1 d . . . O22 O -0.01250(15) 1.0664(2) 0.18100(16) 0.0215(9) Uani 1 1 d . . . O23 O -0.12052(15) 1.1420(3) 0.11354(16) 0.0261(9) Uani 1 1 d . . . O24 O -0.09519(16) 1.2800(3) 0.03822(16) 0.0294(10) Uani 1 1 d . . . C6 C -0.0876(2) 0.8619(4) -0.0126(2) 0.0201(12) Uani 1 1 d . . . H6A H -0.0877 0.8029 -0.0361 0.024 Uiso 1 1 calc R . . H6B H -0.1248 0.8822 -0.0069 0.024 Uiso 1 1 calc R . . C7 C -0.0065(2) 0.7964(4) 0.0379(2) 0.0205(13) Uani 1 1 d . . . H7A H 0.0055 0.7748 0.0738 0.025 Uiso 1 1 calc R . . H7B H -0.0058 0.7379 0.0140 0.025 Uiso 1 1 calc R . . C8 C -0.0680(2) 0.9193(3) 0.0827(2) 0.0197(13) Uani 1 1 d . . . H8A H -0.1059 0.9363 0.0867 0.024 Uiso 1 1 calc R . . H8B H -0.0550 0.8965 0.1180 0.024 Uiso 1 1 calc R . . C9 C -0.0628(2) 0.8338(4) 0.0421(2) 0.0196(12) Uani 1 1 d . . . C10 C -0.0965(2) 0.7470(4) 0.0634(3) 0.0295(14) Uani 1 1 d . . . H10A H -0.0829 0.7257 0.0983 0.044 Uiso 1 1 calc R . . H10B H -0.0948 0.6915 0.0381 0.044 Uiso 1 1 calc R . . H10C H -0.1332 0.7686 0.0673 0.044 Uiso 1 1 calc R . . O25 O -0.2464(2) 0.6919(4) 0.4656(2) 0.0670(18) Uani 1 1 d . . . N4 N -0.2327(2) 0.7663(4) 0.3858(2) 0.0393(14) Uani 1 1 d . . . C59 C -0.2215(3) 0.7021(5) 0.4244(3) 0.055(2) Uani 1 1 d . . . H59 H -0.1916 0.6607 0.4195 0.065 Uiso 1 1 calc R . . C60 C -0.2794(3) 0.8299(5) 0.3872(3) 0.052(2) Uani 1 1 d . . . H60A H -0.2988 0.8185 0.4207 0.078 Uiso 1 1 calc R . . H60B H -0.3023 0.8142 0.3566 0.078 Uiso 1 1 calc R . . H60C H -0.2685 0.8994 0.3852 0.078 Uiso 1 1 calc R . . C61 C -0.1985(3) 0.7763(6) 0.3395(3) 0.064(2) Uani 1 1 d . . . H61A H -0.2191 0.7660 0.3067 0.096 Uiso 1 1 calc R . . H61B H -0.1702 0.7269 0.3414 0.096 Uiso 1 1 calc R . . H61C H -0.1831 0.8429 0.3390 0.096 Uiso 1 1 calc R . . O26 O 0.1492(2) 1.0238(4) 0.4019(2) 0.0532(14) Uani 1 1 d . . . N5 N 0.1876(2) 1.0146(4) 0.4832(2) 0.0407(14) Uani 1 1 d . . . C62 C 0.1508(3) 0.9921(4) 0.4477(3) 0.0381(17) Uani 1 1 d . . . H62 H 0.1237 0.9480 0.4586 0.046 Uiso 1 1 calc R . . C63 C 0.2325(4) 1.0734(7) 0.4679(4) 0.088(4) Uani 1 1 d . . . H63A H 0.2321 1.0840 0.4290 0.131 Uiso 1 1 calc R . . H63B H 0.2651 1.0388 0.4780 0.131 Uiso 1 1 calc R . . H63C H 0.2311 1.1375 0.4863 0.131 Uiso 1 1 calc R . . C64 C 0.1857(4) 0.9753(6) 0.5374(3) 0.071(3) Uani 1 1 d . . . H64A H 0.1773 1.0289 0.5625 0.106 Uiso 1 1 calc R . . H64B H 0.2200 0.9466 0.5466 0.106 Uiso 1 1 calc R . . H64C H 0.1584 0.9240 0.5396 0.106 Uiso 1 1 calc R . . N1 N 0.05634(19) 0.8720(3) 0.27880(19) 0.0210(11) Uani 1 1 d . . . C11 C 0.0827(2) 0.7717(4) 0.2761(2) 0.0218(13) Uani 1 1 d . . . H11A H 0.0603 0.7233 0.2953 0.026 Uiso 1 1 calc R . . H11B H 0.1168 0.7756 0.2955 0.026 Uiso 1 1 calc R . . C12 C 0.0933(2) 0.7322(4) 0.2204(2) 0.0271(14) Uani 1 1 d . . . H12A H 0.0605 0.7363 0.1989 0.032 Uiso 1 1 calc R . . H12B H 0.1204 0.7738 0.2027 0.032 Uiso 1 1 calc R . . C13 C 0.1121(3) 0.6262(5) 0.2219(3) 0.0400(17) Uani 1 1 d . . . H13A H 0.1439 0.6221 0.2448 0.048 Uiso 1 1 calc R . . H13B H 0.0843 0.5846 0.2385 0.048 Uiso 1 1 calc R . . C14 C 0.1250(3) 0.5853(4) 0.1673(3) 0.0335(16) Uani 1 1 d . . . H14A H 0.0942 0.5926 0.1438 0.050 Uiso 1 1 calc R . . H14B H 0.1341 0.5150 0.1705 0.050 Uiso 1 1 calc R . . H14C H 0.1550 0.6216 0.1522 0.050 Uiso 1 1 calc R . . C15 C 0.0474(2) 0.8941(4) 0.3380(2) 0.0265(14) Uani 1 1 d . . . H15A H 0.0260 0.8397 0.3535 0.032 Uiso 1 1 calc R . . H15B H 0.0820 0.8938 0.3563 0.032 Uiso 1 1 calc R . . C16 C 0.0202(3) 0.9909(4) 0.3503(3) 0.0348(16) Uani 1 1 d . . . H16A H -0.0125 0.9960 0.3286 0.042 Uiso 1 1 calc R . . H16B H 0.0436 1.0465 0.3401 0.042 Uiso 1 1 calc R . . C17 C 0.0063(3) 0.9994(5) 0.4092(3) 0.0404(17) Uani 1 1 d . . . H17A H -0.0069 1.0673 0.4163 0.048 Uiso 1 1 calc R . . H17B H 0.0388 0.9900 0.4307 0.048 Uiso 1 1 calc R . . C18 C -0.0353(3) 0.9251(4) 0.4280(3) 0.0389(17) Uani 1 1 d . . . H18A H -0.0666 0.9302 0.4052 0.058 Uiso 1 1 calc R . . H18B H -0.0449 0.9394 0.4652 0.058 Uiso 1 1 calc R . . H18C H -0.0208 0.8578 0.4256 0.058 Uiso 1 1 calc R . . C19 C 0.0038(2) 0.8714(4) 0.2482(2) 0.0243(13) Uani 1 1 d . . . H19A H -0.0116 0.9387 0.2497 0.029 Uiso 1 1 calc R . . H19B H 0.0112 0.8563 0.2101 0.029 Uiso 1 1 calc R . . C20 C -0.0365(2) 0.7987(4) 0.2685(3) 0.0316(15) Uani 1 1 d . . . H20A H -0.0509 0.8225 0.3031 0.038 Uiso 1 1 calc R . . H20B H -0.0193 0.7338 0.2749 0.038 Uiso 1 1 calc R . . C21 C -0.0817(3) 0.7857(4) 0.2285(3) 0.0343(16) Uani 1 1 d . . . H21A H -0.0667 0.7657 0.1935 0.041 Uiso 1 1 calc R . . H21B H -0.1047 0.7311 0.2410 0.041 Uiso 1 1 calc R . . C22 C -0.1151(2) 0.8767(4) 0.2204(3) 0.0332(15) Uani 1 1 d . . . H22A H -0.1456 0.8601 0.1979 0.050 Uiso 1 1 calc R . . H22B H -0.0940 0.9281 0.2028 0.050 Uiso 1 1 calc R . . H22C H -0.1274 0.9010 0.2552 0.050 Uiso 1 1 calc R . . C23 C 0.0904(2) 0.9501(4) 0.2521(2) 0.0268(14) Uani 1 1 d . . . H23A H 0.0730 1.0153 0.2566 0.032 Uiso 1 1 calc R . . H23B H 0.0917 0.9359 0.2132 0.032 Uiso 1 1 calc R . . C24 C 0.1470(2) 0.9581(5) 0.2729(3) 0.0326(15) Uani 1 1 d . . . H24A H 0.1465 0.9693 0.3121 0.039 Uiso 1 1 calc R . . H24B H 0.1659 0.8952 0.2660 0.039 Uiso 1 1 calc R . . C25 C 0.1757(3) 1.0416(5) 0.2461(4) 0.054(2) Uani 1 1 d . . . H25A H 0.1565 1.1043 0.2527 0.065 Uiso 1 1 calc R . . H25B H 0.1764 1.0299 0.2069 0.065 Uiso 1 1 calc R . . C26 C 0.2321(3) 1.0517(6) 0.2665(4) 0.068(3) Uani 1 1 d . . . H26A H 0.2481 1.1119 0.2517 0.102 Uiso 1 1 calc R . . H26B H 0.2528 0.9939 0.2553 0.102 Uiso 1 1 calc R . . H26C H 0.2319 1.0558 0.3057 0.102 Uiso 1 1 calc R . . N2 N 0.28082(18) 0.6157(3) 0.49158(19) 0.0197(10) Uani 1 1 d . . . C27 C 0.2471(2) 0.5330(4) 0.4674(2) 0.0223(13) Uani 1 1 d . . . H27A H 0.2380 0.4861 0.4965 0.027 Uiso 1 1 calc R . . H27B H 0.2137 0.5627 0.4545 0.027 Uiso 1 1 calc R . . C28 C 0.2711(2) 0.4746(4) 0.4219(2) 0.0305(14) Uani 1 1 d . . . H28A H 0.3035 0.4405 0.4344 0.037 Uiso 1 1 calc R . . H28B H 0.2811 0.5200 0.3924 0.037 Uiso 1 1 calc R . . C29 C 0.2316(3) 0.3989(5) 0.4016(3) 0.0332(16) Uani 1 1 d . . . H29A H 0.2014 0.4341 0.3850 0.040 Uiso 1 1 calc R . . H29B H 0.2178 0.3605 0.4324 0.040 Uiso 1 1 calc R . . C30 C 0.2551(3) 0.3274(5) 0.3607(3) 0.046(2) Uani 1 1 d . . . H30A H 0.2678 0.3647 0.3296 0.070 Uiso 1 1 calc R . . H30B H 0.2279 0.2801 0.3492 0.070 Uiso 1 1 calc R . . H30C H 0.2846 0.2914 0.3770 0.070 Uiso 1 1 calc R . . C31 C 0.3360(2) 0.5793(4) 0.5062(2) 0.0246(13) Uani 1 1 d . . . H31A H 0.3540 0.5579 0.4729 0.029 Uiso 1 1 calc R . . H31B H 0.3562 0.6357 0.5211 0.029 Uiso 1 1 calc R . . C32 C 0.3378(2) 0.4944(4) 0.5462(3) 0.0284(14) Uani 1 1 d . . . H32A H 0.3251 0.5178 0.5815 0.034 Uiso 1 1 calc R . . H32B H 0.3141 0.4405 0.5341 0.034 Uiso 1 1 calc R . . C33 C 0.3936(3) 0.4550(5) 0.5518(3) 0.0456(18) Uani 1 1 d . . . H33A H 0.4062 0.4334 0.5160 0.055 Uiso 1 1 calc R . . H33B H 0.4168 0.5095 0.5639 0.055 Uiso 1 1 calc R . . C34 C 0.3987(3) 0.3700(5) 0.5901(3) 0.049(2) Uani 1 1 d . . . H34A H 0.3742 0.3170 0.5796 0.074 Uiso 1 1 calc R . . H34B H 0.3901 0.3925 0.6264 0.074 Uiso 1 1 calc R . . H34C H 0.4350 0.3448 0.5894 0.074 Uiso 1 1 calc R . . C35 C 0.2522(2) 0.6522(4) 0.5404(2) 0.0235(13) Uani 1 1 d . . . H35A H 0.2460 0.5951 0.5645 0.028 Uiso 1 1 calc R . . H35B H 0.2173 0.6776 0.5291 0.028 Uiso 1 1 calc R . . C36 C 0.2806(2) 0.7340(4) 0.5724(2) 0.0276(14) Uani 1 1 d . . . H36A H 0.3151 0.7089 0.5852 0.033 Uiso 1 1 calc R . . H36B H 0.2873 0.7916 0.5488 0.033 Uiso 1 1 calc R . . C37 C 0.2475(2) 0.7665(4) 0.6200(2) 0.0267(13) Uani 1 1 d . . . H37A H 0.2627 0.8281 0.6350 0.032 Uiso 1 1 calc R . . H37B H 0.2114 0.7820 0.6074 0.032 Uiso 1 1 calc R . . C38 C 0.2440(3) 0.6896(5) 0.6643(3) 0.0412(18) Uani 1 1 d . . . H38A H 0.2262 0.6302 0.6506 0.062 Uiso 1 1 calc R . . H38B H 0.2239 0.7167 0.6945 0.062 Uiso 1 1 calc R . . H38C H 0.2796 0.6721 0.6763 0.062 Uiso 1 1 calc R . . C39 C 0.2883(2) 0.6991(4) 0.4510(2) 0.0261(13) Uani 1 1 d . . . H39A H 0.3032 0.6704 0.4178 0.031 Uiso 1 1 calc R . . H39B H 0.3147 0.7461 0.4655 0.031 Uiso 1 1 calc R . . C40 C 0.2378(2) 0.7580(5) 0.4361(3) 0.0348(15) Uani 1 1 d . . . H40A H 0.2082 0.7114 0.4299 0.042 Uiso 1 1 calc R . . H40B H 0.2279 0.8023 0.4661 0.042 Uiso 1 1 calc R . . C41 C 0.2473(3) 0.8191(5) 0.3858(3) 0.0400(17) Uani 1 1 d . . . H41A H 0.2197 0.8707 0.3830 0.048 Uiso 1 1 calc R . . H41B H 0.2819 0.8529 0.3888 0.048 Uiso 1 1 calc R . . C42 C 0.2468(3) 0.7567(6) 0.3361(3) 0.056(2) Uani 1 1 d . . . H42A H 0.2494 0.7995 0.3045 0.083 Uiso 1 1 calc R . . H42B H 0.2137 0.7188 0.3346 0.083 Uiso 1 1 calc R . . H42C H 0.2768 0.7109 0.3367 0.083 Uiso 1 1 calc R . . N3 N 0.43730(18) 0.6392(3) 0.26825(18) 0.0166(10) Uani 1 1 d . . . C43 C 0.3972(2) 0.5820(4) 0.2355(2) 0.0208(13) Uani 1 1 d . . . H43A H 0.4099 0.5130 0.2315 0.025 Uiso 1 1 calc R . . H43B H 0.3956 0.6116 0.1992 0.025 Uiso 1 1 calc R . . C44 C 0.3418(2) 0.5796(4) 0.2586(2) 0.0232(13) Uani 1 1 d . . . H44A H 0.3431 0.5543 0.2959 0.028 Uiso 1 1 calc R . . H44B H 0.3272 0.6476 0.2596 0.028 Uiso 1 1 calc R . . C45 C 0.3062(2) 0.5138(4) 0.2252(2) 0.0251(13) Uani 1 1 d . . . H45A H 0.3172 0.4439 0.2297 0.030 Uiso 1 1 calc R . . H45B H 0.3103 0.5313 0.1869 0.030 Uiso 1 1 calc R . . C46 C 0.2481(2) 0.5244(5) 0.2411(3) 0.0404(18) Uani 1 1 d . . . H46A H 0.2268 0.4770 0.2206 0.061 Uiso 1 1 calc R . . H46B H 0.2361 0.5919 0.2333 0.061 Uiso 1 1 calc R . . H46C H 0.2442 0.5110 0.2795 0.061 Uiso 1 1 calc R . . C47 C 0.4874(2) 0.6451(4) 0.2352(2) 0.0203(13) Uani 1 1 d . . . H47A H 0.4990 0.5766 0.2273 0.024 Uiso 1 1 calc R . . H47B H 0.4786 0.6768 0.2006 0.024 Uiso 1 1 calc R . . C48 C 0.5334(2) 0.7002(4) 0.2595(2) 0.0214(13) Uani 1 1 d . . . H48A H 0.5444 0.6676 0.2932 0.026 Uiso 1 1 calc R . . H48B H 0.5228 0.7691 0.2679 0.026 Uiso 1 1 calc R . . C49 C 0.5791(2) 0.7008(4) 0.2202(2) 0.0258(14) Uani 1 1 d . . . H49A H 0.5686 0.7380 0.1877 0.031 Uiso 1 1 calc R . . H49B H 0.5870 0.6319 0.2093 0.031 Uiso 1 1 calc R . . C50 C 0.6294(2) 0.7482(5) 0.2439(3) 0.0346(16) Uani 1 1 d . . . H50A H 0.6571 0.7502 0.2165 0.052 Uiso 1 1 calc R . . H50B H 0.6416 0.7088 0.2745 0.052 Uiso 1 1 calc R . . H50C H 0.6215 0.8158 0.2559 0.052 Uiso 1 1 calc R . . C51 C 0.4477(2) 0.5887(4) 0.3215(2) 0.0270(14) Uani 1 1 d . . . H51A H 0.4159 0.5953 0.3443 0.032 Uiso 1 1 calc R . . H51B H 0.4771 0.6234 0.3398 0.032 Uiso 1 1 calc R . . C52 C 0.4619(3) 0.4777(4) 0.3166(3) 0.0347(16) Uani 1 1 d . . . H52A H 0.4291 0.4391 0.3110 0.042 Uiso 1 1 calc R . . H52B H 0.4847 0.4679 0.2849 0.042 Uiso 1 1 calc R . . C53 C 0.4902(3) 0.4387(5) 0.3662(3) 0.0408(17) Uani 1 1 d . . . H53A H 0.4987 0.3678 0.3607 0.049 Uiso 1 1 calc R . . H53B H 0.5240 0.4749 0.3705 0.049 Uiso 1 1 calc R . . C54 C 0.4595(3) 0.4487(5) 0.4156(3) 0.053(2) Uani 1 1 d . . . H54A H 0.4236 0.4239 0.4095 0.080 Uiso 1 1 calc R . . H54B H 0.4579 0.5186 0.4260 0.080 Uiso 1 1 calc R . . H54C H 0.4763 0.4103 0.4442 0.080 Uiso 1 1 calc R . . C55 C 0.4172(2) 0.7426(4) 0.2811(2) 0.0211(12) Uani 1 1 d . . . H55A H 0.3842 0.7363 0.3021 0.025 Uiso 1 1 calc R . . H55B H 0.4435 0.7760 0.3042 0.025 Uiso 1 1 calc R . . C56 C 0.4063(3) 0.8085(4) 0.2332(2) 0.0314(16) Uani 1 1 d . . . H56A H 0.3858 0.7715 0.2060 0.038 Uiso 1 1 calc R . . H56B H 0.4400 0.8297 0.2167 0.038 Uiso 1 1 calc R . . C57 C 0.3747(3) 0.9002(4) 0.2519(3) 0.0398(19) Uani 1 1 d . . . H57A H 0.3390 0.8793 0.2634 0.048 Uiso 1 1 calc R . . H57B H 0.3927 0.9306 0.2830 0.048 Uiso 1 1 calc R . . C58 C 0.3699(3) 0.9741(5) 0.2086(4) 0.059(2) Uani 1 1 d . . . H58A H 0.3575 0.9416 0.1759 0.089 Uiso 1 1 calc R . . H58B H 0.4045 1.0046 0.2020 0.089 Uiso 1 1 calc R . . H58C H 0.3446 1.0254 0.2193 0.089 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0211(2) 0.0144(2) 0.0102(2) -0.00155(17) 0.0040(2) -0.00535(19) Mo2 0.0209(2) 0.0126(2) 0.0099(2) -0.00126(17) 0.0039(2) -0.00369(18) Mo3 0.0249(3) 0.0156(2) 0.0123(2) -0.00470(18) 0.0051(2) -0.00813(19) Cr1 0.0158(6) 0.0076(5) 0.0065(6) -0.0003(4) 0.0013(5) -0.0016(5) O1 0.0133(18) 0.0119(15) 0.011(2) 0.0012(14) -0.0018(15) 0.0010(13) O2 0.0076(17) 0.0147(16) 0.013(2) -0.0001(14) 0.0005(15) 0.0019(14) O3 0.023(2) 0.0101(16) 0.014(2) 0.0030(14) -0.0015(16) -0.0005(15) O4 0.026(2) 0.024(2) 0.014(2) -0.0005(16) 0.0066(18) -0.0109(17) O5 0.022(2) 0.0146(17) 0.014(2) -0.0019(14) 0.0033(16) -0.0034(15) O6 0.023(2) 0.0130(16) 0.014(2) 0.0008(15) 0.0007(17) -0.0028(15) O7 0.034(2) 0.0157(18) 0.022(2) 0.0003(16) 0.0063(19) -0.0077(17) O8 0.024(2) 0.023(2) 0.022(2) -0.0059(17) 0.0064(18) -0.0072(17) O9 0.022(2) 0.0175(18) 0.022(2) -0.0027(16) 0.0002(18) -0.0044(17) O10 0.022(2) 0.0201(18) 0.020(2) -0.0019(16) -0.0020(18) -0.0071(16) O11 0.027(2) 0.055(3) 0.014(2) -0.0130(19) 0.0019(19) -0.012(2) O12 0.050(3) 0.0152(18) 0.026(2) -0.0073(17) 0.018(2) -0.0139(19) C1 0.025(3) 0.021(3) 0.017(3) 0.000(2) 0.000(3) -0.003(2) C2 0.022(3) 0.018(3) 0.019(3) 0.002(2) 0.000(3) 0.004(2) C3 0.035(3) 0.015(2) 0.019(3) 0.008(2) 0.005(3) 0.003(2) C4 0.022(3) 0.022(3) 0.017(3) 0.002(2) 0.006(3) 0.000(2) C5 0.032(3) 0.031(3) 0.022(4) 0.007(3) -0.004(3) 0.008(3) Mo4 0.0216(2) 0.0154(2) 0.0191(3) -0.00189(19) 0.0026(2) 0.00613(19) Mo5 0.0206(2) 0.0156(2) 0.0153(3) -0.00175(18) 0.0030(2) 0.00300(19) Mo6 0.0217(3) 0.0226(2) 0.0183(3) -0.0024(2) 0.0001(2) 0.0091(2) Cr2 0.0127(6) 0.0100(5) 0.0135(6) 0.0006(5) 0.0019(5) 0.0029(5) O13 0.0181(19) 0.0126(16) 0.019(2) -0.0005(15) 0.0044(17) 0.0010(15) O14 0.021(2) 0.0096(16) 0.017(2) 0.0038(14) 0.0052(17) 0.0022(15) O15 0.0163(19) 0.0128(16) 0.018(2) 0.0010(15) 0.0035(17) -0.0015(14) O16 0.023(2) 0.0111(16) 0.020(2) 0.0004(15) 0.0063(17) 0.0038(15) O17 0.029(2) 0.0176(18) 0.015(2) 0.0020(16) 0.0064(18) 0.0084(16) O18 0.019(2) 0.0224(19) 0.018(2) -0.0007(16) -0.0003(17) 0.0034(16) O19 0.039(3) 0.031(2) 0.021(2) 0.0054(18) -0.002(2) 0.0178(19) O20 0.018(2) 0.042(2) 0.024(2) -0.0069(19) -0.0006(18) 0.0108(19) O21 0.019(2) 0.028(2) 0.025(2) -0.0077(17) 0.0007(18) 0.0036(17) O22 0.027(2) 0.0188(18) 0.019(2) 0.0003(16) 0.0031(18) 0.0070(16) O23 0.022(2) 0.032(2) 0.025(3) -0.0061(18) 0.0066(18) 0.0065(18) O24 0.042(3) 0.0206(19) 0.025(2) -0.0003(17) -0.004(2) 0.0097(19) C6 0.019(3) 0.014(2) 0.027(3) -0.002(2) 0.001(3) -0.007(2) C7 0.025(3) 0.013(2) 0.023(3) 0.002(2) 0.007(3) 0.001(2) C8 0.018(3) 0.018(3) 0.023(3) 0.001(2) 0.004(2) -0.005(2) C9 0.022(3) 0.020(3) 0.017(3) 0.001(2) 0.003(3) -0.007(2) C10 0.033(3) 0.022(3) 0.033(4) -0.003(3) 0.014(3) -0.005(3) O25 0.085(4) 0.067(4) 0.049(4) 0.029(3) -0.010(3) -0.030(3) N4 0.044(3) 0.044(3) 0.031(3) 0.008(3) 0.004(3) 0.006(3) C59 0.066(6) 0.045(4) 0.052(6) 0.018(4) -0.016(5) -0.005(4) C60 0.043(4) 0.060(5) 0.053(6) 0.009(4) -0.009(4) 0.012(4) C61 0.081(6) 0.064(5) 0.047(6) 0.013(4) 0.018(5) 0.019(5) O26 0.068(4) 0.051(3) 0.041(3) -0.011(3) -0.014(3) 0.017(3) N5 0.044(4) 0.035(3) 0.042(4) 0.004(3) -0.001(3) -0.005(3) C62 0.035(4) 0.021(3) 0.058(5) -0.005(3) -0.004(4) -0.001(3) C63 0.076(7) 0.112(8) 0.075(8) 0.028(6) -0.024(6) -0.060(6) C64 0.093(7) 0.077(6) 0.042(5) 0.023(5) 0.005(5) 0.022(5) N1 0.028(3) 0.019(2) 0.016(3) 0.0021(19) 0.000(2) 0.003(2) C11 0.030(3) 0.019(3) 0.016(3) 0.003(2) 0.007(3) 0.004(3) C12 0.036(4) 0.023(3) 0.022(3) 0.004(2) 0.003(3) -0.003(3) C13 0.047(4) 0.037(4) 0.036(4) -0.008(3) 0.009(4) 0.013(3) C14 0.038(4) 0.033(3) 0.029(4) -0.008(3) 0.002(3) 0.002(3) C15 0.031(4) 0.026(3) 0.022(3) 0.004(3) 0.003(3) 0.000(3) C16 0.043(4) 0.022(3) 0.039(4) -0.001(3) 0.008(3) 0.007(3) C17 0.044(4) 0.044(4) 0.033(4) -0.012(3) -0.008(3) 0.011(3) C18 0.057(5) 0.036(3) 0.024(4) 0.007(3) 0.009(4) 0.014(3) C19 0.028(3) 0.022(3) 0.023(3) 0.007(2) -0.004(3) -0.005(3) C20 0.033(4) 0.035(3) 0.026(4) 0.014(3) -0.009(3) -0.004(3) C21 0.036(4) 0.029(3) 0.037(4) 0.008(3) -0.002(3) -0.010(3) C22 0.025(3) 0.046(4) 0.029(4) 0.007(3) 0.003(3) 0.002(3) C23 0.039(4) 0.016(3) 0.025(3) 0.002(2) 0.010(3) -0.007(3) C24 0.032(4) 0.039(4) 0.027(4) -0.006(3) 0.000(3) -0.009(3) C25 0.030(4) 0.031(4) 0.102(8) 0.003(4) 0.005(4) -0.001(3) C26 0.035(5) 0.063(5) 0.105(8) -0.002(5) 0.006(5) -0.019(4) N2 0.020(3) 0.022(2) 0.017(3) 0.0008(19) 0.002(2) -0.002(2) C27 0.019(3) 0.030(3) 0.017(3) 0.000(2) 0.000(2) -0.007(2) C28 0.034(3) 0.035(3) 0.023(4) -0.005(3) 0.005(3) -0.003(3) C29 0.032(4) 0.042(4) 0.026(4) -0.014(3) -0.006(3) 0.008(3) C30 0.061(5) 0.038(4) 0.040(5) -0.016(3) -0.013(4) 0.021(4) C31 0.019(3) 0.034(3) 0.021(3) 0.000(3) 0.003(3) 0.000(3) C32 0.029(3) 0.028(3) 0.028(4) -0.001(3) 0.000(3) 0.001(3) C33 0.042(4) 0.059(4) 0.036(4) 0.007(4) 0.000(4) 0.016(4) C34 0.055(5) 0.033(4) 0.058(5) -0.002(3) -0.014(4) 0.024(4) C35 0.024(3) 0.024(3) 0.022(3) 0.000(2) 0.007(3) -0.002(2) C36 0.031(3) 0.029(3) 0.023(3) -0.003(3) 0.002(3) -0.006(3) C37 0.025(3) 0.025(3) 0.030(3) -0.006(3) 0.000(3) -0.007(2) C38 0.049(5) 0.045(4) 0.030(4) -0.006(3) 0.003(3) -0.002(3) C39 0.027(3) 0.033(3) 0.018(3) 0.005(3) 0.008(3) -0.006(3) C40 0.027(3) 0.045(4) 0.032(4) 0.010(3) 0.004(3) -0.001(3) C41 0.043(4) 0.037(4) 0.040(5) 0.014(3) -0.003(4) -0.003(3) C42 0.070(6) 0.061(5) 0.036(4) 0.006(4) 0.013(4) 0.017(4) N3 0.025(3) 0.017(2) 0.008(2) -0.0052(18) 0.001(2) -0.004(2) C43 0.026(3) 0.024(3) 0.012(3) -0.009(2) 0.003(3) -0.005(2) C44 0.027(3) 0.028(3) 0.015(3) -0.005(2) 0.006(3) -0.002(3) C45 0.031(3) 0.024(3) 0.020(3) -0.002(2) 0.000(3) -0.002(3) C46 0.041(4) 0.036(4) 0.044(5) -0.007(3) 0.001(4) -0.006(3) C47 0.027(3) 0.017(2) 0.017(3) -0.010(2) 0.004(3) -0.005(2) C48 0.019(3) 0.022(3) 0.023(3) -0.010(2) 0.001(3) 0.001(2) C49 0.031(3) 0.021(3) 0.025(3) -0.007(2) 0.005(3) -0.004(3) C50 0.025(3) 0.039(4) 0.040(4) -0.009(3) 0.012(3) -0.009(3) C51 0.029(3) 0.030(3) 0.023(4) 0.003(3) -0.001(3) -0.004(3) C52 0.040(4) 0.036(3) 0.028(4) 0.007(3) 0.001(3) 0.010(3) C53 0.040(4) 0.037(4) 0.045(5) 0.008(3) -0.007(4) -0.003(3) C54 0.088(6) 0.030(3) 0.043(5) -0.006(3) 0.003(4) 0.016(4) C55 0.024(3) 0.017(3) 0.023(3) -0.006(2) 0.007(3) -0.002(2) C56 0.045(4) 0.022(3) 0.027(4) -0.001(3) 0.015(3) -0.011(3) C57 0.033(4) 0.025(3) 0.061(5) 0.010(3) -0.025(4) 0.001(3) C58 0.055(5) 0.042(4) 0.081(7) 0.004(4) 0.007(5) -0.003(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 Mo1 O8 1.693(4) . ? Mo1 O7 1.705(3) . ? Mo1 O6 1.924(4) . ? Mo1 O4 1.936(4) 3_676 ? Mo1 O3 2.346(4) . ? Mo1 O2 2.369(3) 3_676 ? Mo2 O9 1.703(4) . ? Mo2 O10 1.729(4) . ? Mo2 O5 1.916(3) . ? Mo2 O6 1.924(3) . ? Mo2 O2 2.347(3) 3_676 ? Mo2 O1 2.360(3) . ? Mo3 O11 1.700(4) . ? Mo3 O12 1.705(4) . ? Mo3 O5 1.923(4) . ? Mo3 O4 1.932(4) . ? Mo3 O3 2.339(4) 3_676 ? Mo3 O1 2.353(3) . ? Cr1 O3 1.958(3) . ? Cr1 O3 1.958(3) 3_676 ? Cr1 O2 1.959(3) . ? Cr1 O2 1.959(3) 3_676 ? Cr1 O1 1.974(3) . ? Cr1 O1 1.974(3) 3_676 ? O1 C1 1.443(6) . ? O2 C2 1.451(6) . ? O2 Mo2 2.347(3) 3_676 ? O2 Mo1 2.369(3) 3_676 ? O3 C3 1.471(6) . ? O3 Mo3 2.339(4) 3_676 ? O4 Mo1 1.936(4) 3_676 ? C1 C4 1.541(7) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C4 1.506(7) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.524(7) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.567(7) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? Mo4 O24 1.706(4) . ? Mo4 O23 1.710(4) . ? Mo4 O18 1.935(4) 3_575 ? Mo4 O16 1.943(4) . ? Mo4 O14 2.339(4) 3_575 ? Mo4 O15 2.357(3) . ? Mo5 O22 1.700(4) . ? Mo5 O21 1.702(4) . ? Mo5 O16 1.921(3) . ? Mo5 O17 1.932(3) . ? Mo5 O13 2.329(4) 3_575 ? Mo5 O15 2.368(3) . ? Mo6 O19 1.699(4) . ? Mo6 O20 1.708(4) . ? Mo6 O18 1.925(4) . ? Mo6 O17 1.926(4) . ? Mo6 O14 2.367(4) . ? Mo6 O13 2.369(3) 3_575 ? Cr2 O15 1.954(4) 3_575 ? Cr2 O15 1.954(4) . ? Cr2 O13 1.963(4) 3_575 ? Cr2 O13 1.963(4) . ? Cr2 O14 1.964(3) 3_575 ? Cr2 O14 1.964(3) . ? O13 C6 1.446(6) . ? O13 Mo5 2.329(4) 3_575 ? O13 Mo6 2.369(3) 3_575 ? O14 C7 1.449(6) . ? O14 Mo4 2.339(4) 3_575 ? O15 C8 1.452(6) . ? O18 Mo4 1.935(4) 3_575 ? C6 C9 1.549(8) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C9 1.515(7) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.542(7) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.544(7) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? O25 C59 1.212(10) . ? N4 C59 1.327(8) . ? N4 C61 1.450(9) . ? N4 C60 1.462(8) . ? C59 H59 0.9500 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? O26 C62 1.220(8) . ? N5 C62 1.319(9) . ? N5 C63 1.439(9) . ? N5 C64 1.454(9) . ? C62 H62 0.9500 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? N1 C11 1.512(6) . ? N1 C23 1.516(7) . ? N1 C15 1.524(7) . ? N1 C19 1.533(7) . ? C11 C12 1.512(8) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.509(8) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.504(8) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.508(7) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.516(9) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.527(9) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.505(8) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.529(8) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.504(8) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.528(8) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.499(9) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.522(10) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? N2 C35 1.499(7) . ? N2 C31 1.525(7) . ? N2 C39 1.525(7) . ? N2 C27 1.528(7) . ? C27 C28 1.510(8) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.518(8) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.526(8) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.521(8) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.515(8) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.500(9) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.542(8) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C37 1.519(8) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.518(8) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 C40 1.551(8) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.521(8) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.500(9) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? N3 C43 1.513(7) . ? N3 C47 1.514(7) . ? N3 C51 1.516(7) . ? N3 C55 1.521(6) . ? C43 C44 1.517(8) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C45 1.515(7) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.530(8) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 C48 1.509(7) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 C49 1.516(8) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 C50 1.544(8) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 C52 1.545(7) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 C53 1.524(9) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 C54 1.463(10) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 C56 1.516(8) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 C57 1.545(8) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 C58 1.474(10) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 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 O8 Mo1 O7 105.41(18) . . ? O8 Mo1 O6 100.82(17) . . ? O7 Mo1 O6 98.70(16) . . ? O8 Mo1 O4 98.73(18) . 3_676 ? O7 Mo1 O4 102.24(16) . 3_676 ? O6 Mo1 O4 146.27(15) . 3_676 ? O8 Mo1 O3 160.16(15) . . ? O7 Mo1 O3 93.86(15) . . ? O6 Mo1 O3 80.46(14) . . ? O4 Mo1 O3 72.06(14) 3_676 . ? O8 Mo1 O2 91.45(14) . 3_676 ? O7 Mo1 O2 161.86(16) . 3_676 ? O6 Mo1 O2 71.03(13) . 3_676 ? O4 Mo1 O2 81.30(13) 3_676 3_676 ? O3 Mo1 O2 70.08(11) . 3_676 ? O9 Mo2 O10 105.96(18) . . ? O9 Mo2 O5 99.66(16) . . ? O10 Mo2 O5 101.93(16) . . ? O9 Mo2 O6 101.61(16) . . ? O10 Mo2 O6 96.85(16) . . ? O5 Mo2 O6 146.41(15) . . ? O9 Mo2 O2 90.99(15) . 3_676 ? O10 Mo2 O2 161.31(14) . 3_676 ? O5 Mo2 O2 82.44(13) . 3_676 ? O6 Mo2 O2 71.53(14) . 3_676 ? O9 Mo2 O1 160.06(15) . . ? O10 Mo2 O1 93.48(15) . . ? O5 Mo2 O1 71.39(13) . . ? O6 Mo2 O1 79.96(13) . . ? O2 Mo2 O1 70.48(11) 3_676 . ? O11 Mo3 O12 105.3(2) . . ? O11 Mo3 O5 102.62(18) . . ? O12 Mo3 O5 98.28(17) . . ? O11 Mo3 O4 96.04(18) . . ? O12 Mo3 O4 101.97(17) . . ? O5 Mo3 O4 147.69(14) . . ? O11 Mo3 O3 160.93(16) . 3_676 ? O12 Mo3 O3 92.14(16) . 3_676 ? O5 Mo3 O3 82.09(14) . 3_676 ? O4 Mo3 O3 72.31(15) . 3_676 ? O11 Mo3 O1 93.74(16) . . ? O12 Mo3 O1 160.15(17) . . ? O5 Mo3 O1 71.45(12) . . ? O4 Mo3 O1 81.31(13) . . ? O3 Mo3 O1 70.00(11) 3_676 . ? O3 Cr1 O3 180.0 . 3_676 ? O3 Cr1 O2 92.53(14) . . ? O3 Cr1 O2 87.47(14) 3_676 . ? O3 Cr1 O2 87.47(14) . 3_676 ? O3 Cr1 O2 92.53(14) 3_676 3_676 ? O2 Cr1 O2 179.998(1) . 3_676 ? O3 Cr1 O1 93.60(14) . . ? O3 Cr1 O1 86.40(14) 3_676 . ? O2 Cr1 O1 92.63(14) . . ? O2 Cr1 O1 87.37(14) 3_676 . ? O3 Cr1 O1 86.40(14) . 3_676 ? O3 Cr1 O1 93.60(14) 3_676 3_676 ? O2 Cr1 O1 87.37(14) . 3_676 ? O2 Cr1 O1 92.63(14) 3_676 3_676 ? O1 Cr1 O1 180.00(17) . 3_676 ? C1 O1 Cr1 116.4(3) . . ? C1 O1 Mo3 121.4(3) . . ? Cr1 O1 Mo3 101.31(13) . . ? C1 O1 Mo2 121.3(3) . . ? Cr1 O1 Mo2 100.63(13) . . ? Mo3 O1 Mo2 90.93(11) . . ? C2 O2 Cr1 116.5(3) . . ? C2 O2 Mo2 121.7(3) . 3_676 ? Cr1 O2 Mo2 101.53(13) . 3_676 ? C2 O2 Mo1 120.9(3) . 3_676 ? Cr1 O2 Mo1 100.82(13) . 3_676 ? Mo2 O2 Mo1 90.40(12) 3_676 3_676 ? C3 O3 Cr1 115.0(3) . . ? C3 O3 Mo3 121.7(3) . 3_676 ? Cr1 O3 Mo3 102.28(15) . 3_676 ? C3 O3 Mo1 121.0(3) . . ? Cr1 O3 Mo1 101.63(14) . . ? Mo3 O3 Mo1 90.86(12) 3_676 . ? Mo3 O4 Mo1 119.3(2) . 3_676 ? Mo2 O5 Mo3 122.12(18) . . ? Mo1 O6 Mo2 120.81(18) . . ? O1 C1 C4 113.4(4) . . ? O1 C1 H1A 108.9 . . ? C4 C1 H1A 108.9 . . ? O1 C1 H1B 108.9 . . ? C4 C1 H1B 108.9 . . ? H1A C1 H1B 107.7 . . ? O2 C2 C4 113.5(4) . . ? O2 C2 H2A 108.9 . . ? C4 C2 H2A 108.9 . . ? O2 C2 H2B 108.9 . . ? C4 C2 H2B 108.9 . . ? H2A C2 H2B 107.7 . . ? O3 C3 C4 114.3(4) . . ? O3 C3 H3A 108.7 . . ? C4 C3 H3A 108.7 . . ? O3 C3 H3B 108.7 . . ? C4 C3 H3B 108.7 . . ? H3A C3 H3B 107.6 . . ? C2 C4 C3 112.1(5) . . ? C2 C4 C1 112.7(4) . . ? C3 C4 C1 111.9(4) . . ? C2 C4 C5 106.7(4) . . ? C3 C4 C5 106.9(4) . . ? C1 C4 C5 106.0(5) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? O24 Mo4 O23 105.73(19) . . ? O24 Mo4 O18 101.47(17) . 3_575 ? O23 Mo4 O18 98.65(17) . 3_575 ? O24 Mo4 O16 98.07(17) . . ? O23 Mo4 O16 102.20(17) . . ? O18 Mo4 O16 146.24(14) 3_575 . ? O24 Mo4 O14 92.58(16) . 3_575 ? O23 Mo4 O14 160.80(14) . 3_575 ? O18 Mo4 O14 71.51(14) 3_575 3_575 ? O16 Mo4 O14 80.41(14) . 3_575 ? O24 Mo4 O15 160.46(16) . . ? O23 Mo4 O15 92.63(15) . . ? O18 Mo4 O15 81.90(13) 3_575 . ? O16 Mo4 O15 70.96(12) . . ? O14 Mo4 O15 70.03(12) 3_575 . ? O22 Mo5 O21 105.35(19) . . ? O22 Mo5 O16 100.71(16) . . ? O21 Mo5 O16 99.60(17) . . ? O22 Mo5 O17 98.46(16) . . ? O21 Mo5 O17 102.08(17) . . ? O16 Mo5 O17 145.97(16) . . ? O22 Mo5 O13 162.67(15) . 3_575 ? O21 Mo5 O13 91.17(16) . 3_575 ? O16 Mo5 O13 81.25(14) . 3_575 ? O17 Mo5 O13 72.43(14) . 3_575 ? O22 Mo5 O15 94.38(16) . . ? O21 Mo5 O15 159.58(16) . . ? O16 Mo5 O15 71.05(13) . . ? O17 Mo5 O15 79.70(14) . . ? O13 Mo5 O15 69.79(12) 3_575 . ? O19 Mo6 O20 105.5(2) . . ? O19 Mo6 O18 101.44(17) . . ? O20 Mo6 O18 98.54(18) . . ? O19 Mo6 O17 99.02(17) . . ? O20 Mo6 O17 102.00(17) . . ? O18 Mo6 O17 145.81(16) . . ? O19 Mo6 O14 92.59(16) . . ? O20 Mo6 O14 160.78(16) . . ? O18 Mo6 O14 71.01(14) . . ? O17 Mo6 O14 81.01(14) . . ? O19 Mo6 O13 160.83(17) . 3_575 ? O20 Mo6 O13 92.96(15) . 3_575 ? O18 Mo6 O13 80.37(13) . 3_575 ? O17 Mo6 O13 71.60(13) . 3_575 ? O14 Mo6 O13 69.76(11) . 3_575 ? O15 Cr2 O15 180.0 3_575 . ? O15 Cr2 O13 93.39(14) 3_575 3_575 ? O15 Cr2 O13 86.61(14) . 3_575 ? O15 Cr2 O13 86.61(14) 3_575 . ? O15 Cr2 O13 93.39(14) . . ? O13 Cr2 O13 180.0 3_575 . ? O15 Cr2 O14 93.10(14) 3_575 3_575 ? O15 Cr2 O14 86.90(14) . 3_575 ? O13 Cr2 O14 92.78(14) 3_575 3_575 ? O13 Cr2 O14 87.22(14) . 3_575 ? O15 Cr2 O14 86.90(14) 3_575 . ? O15 Cr2 O14 93.10(14) . . ? O13 Cr2 O14 87.22(14) 3_575 . ? O13 Cr2 O14 92.78(14) . . ? O14 Cr2 O14 180.0 3_575 . ? C6 O13 Cr2 116.7(3) . . ? C6 O13 Mo5 121.0(3) . 3_575 ? Cr2 O13 Mo5 102.34(15) . 3_575 ? C6 O13 Mo6 120.4(3) . 3_575 ? Cr2 O13 Mo6 101.48(13) . 3_575 ? Mo5 O13 Mo6 90.24(12) 3_575 3_575 ? C7 O14 Cr2 116.2(3) . . ? C7 O14 Mo4 121.4(3) . 3_575 ? Cr2 O14 Mo4 101.68(14) . 3_575 ? C7 O14 Mo6 120.3(3) . . ? Cr2 O14 Mo6 101.53(14) . . ? Mo4 O14 Mo6 91.08(12) 3_575 . ? C8 O15 Cr2 115.9(3) . . ? C8 O15 Mo4 121.1(3) . . ? Cr2 O15 Mo4 101.37(14) . . ? C8 O15 Mo5 121.4(3) . . ? Cr2 O15 Mo5 101.26(14) . . ? Mo4 O15 Mo5 91.11(11) . . ? Mo5 O16 Mo4 121.62(17) . . ? Mo6 O17 Mo5 119.27(18) . . ? Mo6 O18 Mo4 120.98(19) . 3_575 ? O13 C6 C9 112.7(4) . . ? O13 C6 H6A 109.1 . . ? C9 C6 H6A 109.1 . . ? O13 C6 H6B 109.1 . . ? C9 C6 H6B 109.1 . . ? H6A C6 H6B 107.8 . . ? O14 C7 C9 113.4(4) . . ? O14 C7 H7A 108.9 . . ? C9 C7 H7A 108.9 . . ? O14 C7 H7B 108.9 . . ? C9 C7 H7B 108.9 . . ? H7A C7 H7B 107.7 . . ? O15 C8 C9 113.6(4) . . ? O15 C8 H8A 108.8 . . ? C9 C8 H8A 108.8 . . ? O15 C8 H8B 108.8 . . ? C9 C8 H8B 108.8 . . ? H8A C8 H8B 107.7 . . ? C7 C9 C8 112.1(5) . . ? C7 C9 C10 106.9(4) . . ? C8 C9 C10 107.1(4) . . ? C7 C9 C6 113.8(5) . . ? C8 C9 C6 111.1(4) . . ? C10 C9 C6 105.3(4) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C59 N4 C61 120.8(7) . . ? C59 N4 C60 122.6(7) . . ? C61 N4 C60 116.6(6) . . ? O25 C59 N4 125.3(8) . . ? O25 C59 H59 117.4 . . ? N4 C59 H59 117.4 . . ? N4 C60 H60A 109.5 . . ? N4 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? N4 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? N4 C61 H61A 109.5 . . ? N4 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? N4 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C62 N5 C63 120.5(7) . . ? C62 N5 C64 121.1(7) . . ? C63 N5 C64 118.3(7) . . ? O26 C62 N5 124.8(7) . . ? O26 C62 H62 117.6 . . ? N5 C62 H62 117.6 . . ? N5 C63 H63A 109.5 . . ? N5 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? N5 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? N5 C64 H64A 109.5 . . ? N5 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? N5 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C11 N1 C23 110.6(4) . . ? C11 N1 C15 106.5(4) . . ? C23 N1 C15 112.0(4) . . ? C11 N1 C19 110.8(4) . . ? C23 N1 C19 106.2(4) . . ? C15 N1 C19 110.8(5) . . ? N1 C11 C12 115.8(4) . . ? N1 C11 H11A 108.3 . . ? C12 C11 H11A 108.3 . . ? N1 C11 H11B 108.3 . . ? C12 C11 H11B 108.3 . . ? H11A C11 H11B 107.4 . . ? C13 C12 C11 111.5(5) . . ? C13 C12 H12A 109.3 . . ? C11 C12 H12A 109.3 . . ? C13 C12 H12B 109.3 . . ? C11 C12 H12B 109.3 . . ? H12A C12 H12B 108.0 . . ? C14 C13 C12 113.2(6) . . ? C14 C13 H13A 108.9 . . ? C12 C13 H13A 108.9 . . ? C14 C13 H13B 108.9 . . ? C12 C13 H13B 108.9 . . ? H13A C13 H13B 107.7 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 N1 115.8(5) . . ? C16 C15 H15A 108.3 . . ? N1 C15 H15A 108.3 . . ? C16 C15 H15B 108.3 . . ? N1 C15 H15B 108.3 . . ? H15A C15 H15B 107.4 . . ? C15 C16 C17 111.7(5) . . ? C15 C16 H16A 109.3 . . ? C17 C16 H16A 109.3 . . ? C15 C16 H16B 109.3 . . ? C17 C16 H16B 109.3 . . ? H16A C16 H16B 107.9 . . ? C16 C17 C18 114.0(5) . . ? C16 C17 H17A 108.8 . . ? C18 C17 H17A 108.8 . . ? C16 C17 H17B 108.8 . . ? C18 C17 H17B 108.8 . . ? H17A C17 H17B 107.6 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 N1 115.1(5) . . ? C20 C19 H19A 108.5 . . ? N1 C19 H19A 108.5 . . ? C20 C19 H19B 108.5 . . ? N1 C19 H19B 108.5 . . ? H19A C19 H19B 107.5 . . ? C19 C20 C21 111.2(5) . . ? C19 C20 H20A 109.4 . . ? C21 C20 H20A 109.4 . . ? C19 C20 H20B 109.4 . . ? C21 C20 H20B 109.4 . . ? H20A C20 H20B 108.0 . . ? C22 C21 C20 114.5(5) . . ? C22 C21 H21A 108.6 . . ? C20 C21 H21A 108.6 . . ? C22 C21 H21B 108.6 . . ? C20 C21 H21B 108.6 . . ? H21A C21 H21B 107.6 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N1 C23 C24 115.7(5) . . ? N1 C23 H23A 108.4 . . ? C24 C23 H23A 108.4 . . ? N1 C23 H23B 108.4 . . ? C24 C23 H23B 108.4 . . ? H23A C23 H23B 107.4 . . ? C25 C24 C23 110.9(5) . . ? C25 C24 H24A 109.5 . . ? C23 C24 H24A 109.5 . . ? C25 C24 H24B 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 108.0 . . ? C24 C25 C26 111.9(7) . . ? C24 C25 H25A 109.2 . . ? C26 C25 H25A 109.2 . . ? C24 C25 H25B 109.2 . . ? C26 C25 H25B 109.2 . . ? H25A C25 H25B 107.9 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C35 N2 C31 110.7(4) . . ? C35 N2 C39 110.9(4) . . ? C31 N2 C39 106.4(4) . . ? C35 N2 C27 106.9(4) . . ? C31 N2 C27 111.7(4) . . ? C39 N2 C27 110.3(4) . . ? C28 C27 N2 117.0(4) . . ? C28 C27 H27A 108.1 . . ? N2 C27 H27A 108.1 . . ? C28 C27 H27B 108.1 . . ? N2 C27 H27B 108.1 . . ? H27A C27 H27B 107.3 . . ? C27 C28 C29 109.7(5) . . ? C27 C28 H28A 109.7 . . ? C29 C28 H28A 109.7 . . ? C27 C28 H28B 109.7 . . ? C29 C28 H28B 109.7 . . ? H28A C28 H28B 108.2 . . ? C28 C29 C30 113.0(6) . . ? C28 C29 H29A 109.0 . . ? C30 C29 H29A 109.0 . . ? C28 C29 H29B 109.0 . . ? C30 C29 H29B 109.0 . . ? H29A C29 H29B 107.8 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C32 C31 N2 115.3(5) . . ? C32 C31 H31A 108.4 . . ? N2 C31 H31A 108.4 . . ? C32 C31 H31B 108.4 . . ? N2 C31 H31B 108.4 . . ? H31A C31 H31B 107.5 . . ? C33 C32 C31 110.7(5) . . ? C33 C32 H32A 109.5 . . ? C31 C32 H32A 109.5 . . ? C33 C32 H32B 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 108.1 . . ? C34 C33 C32 114.0(6) . . ? C34 C33 H33A 108.8 . . ? C32 C33 H33A 108.8 . . ? C34 C33 H33B 108.8 . . ? C32 C33 H33B 108.8 . . ? H33A C33 H33B 107.6 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N2 C35 C36 115.5(4) . . ? N2 C35 H35A 108.4 . . ? C36 C35 H35A 108.4 . . ? N2 C35 H35B 108.4 . . ? C36 C35 H35B 108.4 . . ? H35A C35 H35B 107.5 . . ? C37 C36 C35 110.8(4) . . ? C37 C36 H36A 109.5 . . ? C35 C36 H36A 109.5 . . ? C37 C36 H36B 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 108.1 . . ? C38 C37 C36 113.8(5) . . ? C38 C37 H37A 108.8 . . ? C36 C37 H37A 108.8 . . ? C38 C37 H37B 108.8 . . ? C36 C37 H37B 108.8 . . ? H37A C37 H37B 107.7 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N2 C39 C40 115.8(4) . . ? N2 C39 H39A 108.3 . . ? C40 C39 H39A 108.3 . . ? N2 C39 H39B 108.3 . . ? C40 C39 H39B 108.3 . . ? H39A C39 H39B 107.4 . . ? C41 C40 C39 110.1(5) . . ? C41 C40 H40A 109.6 . . ? C39 C40 H40A 109.6 . . ? C41 C40 H40B 109.6 . . ? C39 C40 H40B 109.6 . . ? H40A C40 H40B 108.1 . . ? C42 C41 C40 112.1(6) . . ? C42 C41 H41A 109.2 . . ? C40 C41 H41A 109.2 . . ? C42 C41 H41B 109.2 . . ? C40 C41 H41B 109.2 . . ? H41A C41 H41B 107.9 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C43 N3 C47 107.1(4) . . ? C43 N3 C51 111.1(4) . . ? C47 N3 C51 110.7(4) . . ? C43 N3 C55 111.0(4) . . ? C47 N3 C55 110.3(4) . . ? C51 N3 C55 106.6(4) . . ? N3 C43 C44 115.2(4) . . ? N3 C43 H43A 108.5 . . ? C44 C43 H43A 108.5 . . ? N3 C43 H43B 108.5 . . ? C44 C43 H43B 108.5 . . ? H43A C43 H43B 107.5 . . ? C45 C44 C43 110.7(5) . . ? C45 C44 H44A 109.5 . . ? C43 C44 H44A 109.5 . . ? C45 C44 H44B 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 108.1 . . ? C44 C45 C46 112.0(5) . . ? C44 C45 H45A 109.2 . . ? C46 C45 H45A 109.2 . . ? C44 C45 H45B 109.2 . . ? C46 C45 H45B 109.2 . . ? H45A C45 H45B 107.9 . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C48 C47 N3 117.1(4) . . ? C48 C47 H47A 108.0 . . ? N3 C47 H47A 108.0 . . ? C48 C47 H47B 108.0 . . ? N3 C47 H47B 108.0 . . ? H47A C47 H47B 107.3 . . ? C47 C48 C49 109.5(5) . . ? C47 C48 H48A 109.8 . . ? C49 C48 H48A 109.8 . . ? C47 C48 H48B 109.8 . . ? C49 C48 H48B 109.8 . . ? H48A C48 H48B 108.2 . . ? C48 C49 C50 112.6(5) . . ? C48 C49 H49A 109.1 . . ? C50 C49 H49A 109.1 . . ? C48 C49 H49B 109.1 . . ? C50 C49 H49B 109.1 . . ? H49A C49 H49B 107.8 . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? N3 C51 C52 114.0(5) . . ? N3 C51 H51A 108.7 . . ? C52 C51 H51A 108.7 . . ? N3 C51 H51B 108.7 . . ? C52 C51 H51B 108.7 . . ? H51A C51 H51B 107.6 . . ? C53 C52 C51 112.4(5) . . ? C53 C52 H52A 109.1 . . ? C51 C52 H52A 109.1 . . ? C53 C52 H52B 109.1 . . ? C51 C52 H52B 109.1 . . ? H52A C52 H52B 107.9 . . ? C54 C53 C52 113.6(6) . . ? C54 C53 H53A 108.8 . . ? C52 C53 H53A 108.8 . . ? C54 C53 H53B 108.8 . . ? C52 C53 H53B 108.8 . . ? H53A C53 H53B 107.7 . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C56 C55 N3 115.7(4) . . ? C56 C55 H55A 108.4 . . ? N3 C55 H55A 108.4 . . ? C56 C55 H55B 108.4 . . ? N3 C55 H55B 108.4 . . ? H55A C55 H55B 107.4 . . ? C55 C56 C57 109.0(5) . . ? C55 C56 H56A 109.9 . . ? C57 C56 H56A 109.9 . . ? C55 C56 H56B 109.9 . . ? C57 C56 H56B 109.9 . . ? H56A C56 H56B 108.3 . . ? C58 C57 C56 111.3(7) . . ? C58 C57 H57A 109.4 . . ? C56 C57 H57A 109.4 . . ? C58 C57 H57B 109.4 . . ? C56 C57 H57B 109.4 . . ? H57A C57 H57B 108.0 . . ? C57 C58 H58A 109.5 . . ? C57 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C57 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.847 _refine_diff_density_min -0.894 _refine_diff_density_rms 0.128 _database_code_depnum_ccdc_archive 'CCDC 963534' ####################################################################### # # 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_compound2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C61 H129 Cr Mo6 N4 O27' _chemical_formula_weight 1978.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr 0.3209 0.6236 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 31.4877(18) _cell_length_b 14.4928(5) _cell_length_c 21.0381(11) _cell_angle_alpha 90.00 _cell_angle_beta 122.954(8) _cell_angle_gamma 90.00 _cell_volume 8056.0(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 11106 _cell_measurement_theta_min 3.21 _cell_measurement_theta_max 29.41 _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.653 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4096 _exptl_absorpt_coefficient_mu 1.11 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.842 _exptl_absorpt_correction_T_max 0.866 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.0971 _diffrn_reflns_number 22331 _diffrn_reflns_av_R_equivalents 0.0335 _diffrn_reflns_av_sigmaI/netI 0.0473 _diffrn_reflns_limit_h_min -42 _diffrn_reflns_limit_h_max 42 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.21 _diffrn_reflns_theta_max 29.41 _reflns_number_total 9396 _reflns_number_gt 7670 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _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 ; XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution ; SHELXS, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0178P)^2^+27.2227P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9396 _refine_ls_number_parameters 479 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0542 _refine_ls_R_factor_gt 0.0382 _refine_ls_wR_factor_ref 0.0791 _refine_ls_wR_factor_gt 0.0725 _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_restrained_S_all 1.115 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.212665(11) 0.53198(2) 0.939584(16) 0.01580(7) Uani 1 1 d . . . Mo2 Mo 0.317468(11) 0.56813(2) 1.111766(16) 0.01615(7) Uani 1 1 d . . . Mo3 Mo 0.142563(10) 0.71075(2) 0.826902(15) 0.01665(7) Uani 1 1 d . . . Cr Cr 0.2500 0.7500 1.0000 0.00855(14) Uani 1 2 d S . . O1 O 0.27452(8) 0.71350(15) 1.10490(11) 0.0121(4) Uani 1 1 d . . . O2 O 0.18808(8) 0.67829(16) 0.96246(12) 0.0140(5) Uani 1 1 d . A . O7 O 0.13750(8) 0.82880(17) 0.86356(12) 0.0176(5) Uani 1 1 d . . . O9 O 0.18839(8) 0.61004(16) 0.85234(12) 0.0162(5) Uani 1 1 d . . . O3 O 0.21913(8) 0.86185(15) 1.00897(11) 0.0124(4) Uani 1 1 d . . . O4 O 0.24816(8) 0.53035(16) 1.04904(12) 0.0172(5) Uani 1 1 d . . . O8 O 0.12886(9) 0.73682(19) 0.73883(13) 0.0269(6) Uani 1 1 d . . . O12 O 0.32904(10) 0.53910(18) 1.19825(13) 0.0265(6) Uani 1 1 d . . . O5 O 0.15883(9) 0.47687(18) 0.91865(14) 0.0272(6) Uani 1 1 d . . . O10 O 0.24616(9) 0.45358(17) 0.92372(13) 0.0226(5) Uani 1 1 d . . . O11 O 0.34863(9) 0.48872(18) 1.09238(14) 0.0268(6) Uani 1 1 d . . . O6 O 0.08948(9) 0.6604(2) 0.81299(14) 0.0297(6) Uani 1 1 d . . . N13 N 0.0000 0.9648(3) 0.7500 0.0191(9) Uani 1 2 d S . . N14 N 0.17581(11) 0.3215(2) 1.10195(16) 0.0206(6) Uani 1 1 d . . . C3 C 0.15650(12) 0.7574(3) 1.10359(19) 0.0202(7) Uani 1 1 d . . . H3A H 0.1707 0.8012 1.1443 0.030 Uiso 1 1 calc R . . H3B H 0.1561 0.6974 1.1226 0.030 Uiso 1 1 calc R . . H3C H 0.1226 0.7753 1.0654 0.030 Uiso 1 1 calc R . . C1 C 0.18875(11) 0.7544(2) 1.06902(17) 0.0140(6) Uani 1 1 d . A . O13 O 0.25610(13) 0.7105(3) 1.19430(19) 0.0259(8) Uani 0.707(4) 1 d P A 1 C2 C 0.18886(12) 0.8517(2) 1.04078(18) 0.0158(7) Uani 1 1 d . . . H2A H 0.1543 0.8689 1.0027 0.019 Uiso 1 1 calc R . . H2B H 0.2012 0.8944 1.0827 0.019 Uiso 1 1 calc R . . C15 C 0.26669(13) 0.2618(3) 1.16256(19) 0.0233(8) Uani 1 1 d . . . H15A H 0.2606 0.1963 1.1521 0.028 Uiso 1 1 calc R . . H15B H 0.2689 0.2743 1.2096 0.028 Uiso 1 1 calc R . . C4 C 0.16510(12) 0.6827(2) 1.00418(18) 0.0170(7) Uani 1 1 d . . . H4A H 0.1672 0.6222 1.0255 0.020 Uiso 0.707(4) 1 calc PR A 1 H4B H 0.1295 0.6972 0.9697 0.020 Uiso 0.707(4) 1 calc PR A 1 C5 C 0.24239(11) 0.7235(2) 1.13016(17) 0.0135(6) Uani 1 1 d . . . H5 H 0.2525 0.7124 1.1800 0.016 Uiso 0.293(4) 1 calc PR A 2 C14 C 0.22291(12) 0.3160(3) 1.09865(19) 0.0206(7) Uani 1 1 d . . . H14A H 0.2136 0.2879 1.0509 0.025 Uiso 1 1 calc R . . H14B H 0.2344 0.3782 1.0991 0.025 Uiso 1 1 calc R . . C6 C 0.02850(12) 0.9048(3) 0.82061(19) 0.0224(8) Uani 1 1 d . . . H6A H 0.0537 0.8692 0.8183 0.027 Uiso 1 1 calc R . . H6B H 0.0463 0.9447 0.8646 0.027 Uiso 1 1 calc R . . C18 C 0.18595(14) 0.3782(2) 1.16983(19) 0.0214(8) Uani 1 1 d . . . H18A H 0.1556 0.3779 1.1710 0.026 Uiso 1 1 calc R . . H18B H 0.2124 0.3478 1.2156 0.026 Uiso 1 1 calc R . . C10 C 0.03879(12) 1.0243(3) 0.7476(2) 0.0237(8) Uani 1 1 d . . . H10A H 0.0659 0.9847 0.7547 0.028 Uiso 1 1 calc R . . H10B H 0.0533 1.0668 0.7900 0.028 Uiso 1 1 calc R . . C20 C 0.20221(14) 0.5295(3) 1.2360(2) 0.0251(8) Uani 1 1 d . . . H20A H 0.2222 0.4945 1.2825 0.030 Uiso 1 1 calc R . . H20B H 0.2188 0.5885 1.2434 0.030 Uiso 1 1 calc R . . C26 C 0.13511(13) 0.3659(3) 1.02808(19) 0.0249(8) Uani 1 1 d . . . H26A H 0.1292 0.3268 0.9866 0.030 Uiso 1 1 calc R . . H26B H 0.1478 0.4246 1.0230 0.030 Uiso 1 1 calc R . . C22 C 0.15968(15) 0.2264(3) 1.1118(2) 0.0263(8) Uani 1 1 d . . . H22A H 0.1875 0.1995 1.1581 0.032 Uiso 1 1 calc R . . H22B H 0.1316 0.2338 1.1181 0.032 Uiso 1 1 calc R . . C16 C 0.31656(13) 0.2880(3) 1.1713(2) 0.0255(8) Uani 1 1 d . . . H16A H 0.3223 0.3535 1.1821 0.031 Uiso 1 1 calc R . . H16B H 0.3438 0.2552 1.2146 0.031 Uiso 1 1 calc R . . C7 C -0.00458(14) 0.8391(3) 0.8312(2) 0.0279(9) Uani 1 1 d . . . H7A H -0.0306 0.8736 0.8323 0.034 Uiso 1 1 calc R . . H7B H -0.0211 0.7963 0.7891 0.034 Uiso 1 1 calc R . . C11 C 0.01885(13) 1.0795(3) 0.6753(2) 0.0267(8) Uani 1 1 d . . . H11A H -0.0103 1.1156 0.6648 0.032 Uiso 1 1 calc R . . H11B H 0.0082 1.0379 0.6331 0.032 Uiso 1 1 calc R . . C17 C 0.31875(15) 0.2669(3) 1.1021(2) 0.0312(9) Uani 1 1 d . . . H17A H 0.2937 0.3029 1.0599 0.047 Uiso 1 1 calc R . . H17B H 0.3122 0.2024 1.0900 0.047 Uiso 1 1 calc R . . H17C H 0.3517 0.2820 1.1129 0.047 Uiso 1 1 calc R . . C19 C 0.20153(15) 0.4774(3) 1.1717(2) 0.0257(8) Uani 1 1 d . . . H19A H 0.1779 0.5068 1.1236 0.031 Uiso 1 1 calc R . . H19B H 0.2349 0.4793 1.1797 0.031 Uiso 1 1 calc R . . C21 C 0.15004(15) 0.5465(3) 1.2219(2) 0.0298(9) Uani 1 1 d . . . H21A H 0.1296 0.5800 1.1754 0.045 Uiso 1 1 calc R . . H21B H 0.1534 0.5817 1.2630 0.045 Uiso 1 1 calc R . . H21C H 0.1342 0.4884 1.2184 0.045 Uiso 1 1 calc R . . C23 C 0.14398(15) 0.1588(3) 1.0474(2) 0.0315(9) Uani 1 1 d . . . H23A H 0.1707 0.1541 1.0376 0.038 Uiso 1 1 calc R . . H23B H 0.1137 0.1812 1.0017 0.038 Uiso 1 1 calc R . . C12 C 0.06018(15) 1.1435(3) 0.6842(2) 0.0318(9) Uani 1 1 d . . . H12A H 0.0713 1.1838 0.7274 0.038 Uiso 1 1 calc R . . H12B H 0.0890 1.1069 0.6942 0.038 Uiso 1 1 calc R . . C8 C 0.02715(17) 0.7864(3) 0.9044(2) 0.0420(11) Uani 1 1 d . . . H8A H 0.0532 0.7525 0.9030 0.050 Uiso 1 1 calc R . . H8B H 0.0438 0.8298 0.9462 0.050 Uiso 1 1 calc R . . C13 C 0.04202(17) 1.2016(3) 0.6143(3) 0.0468(12) Uani 1 1 d . . . H13A H 0.0321 1.1620 0.5718 0.070 Uiso 1 1 calc R . . H13B H 0.0688 1.2415 0.6223 0.070 Uiso 1 1 calc R . . H13C H 0.0136 1.2380 0.6043 0.070 Uiso 1 1 calc R . . C27 C 0.08478(14) 0.3825(3) 1.0201(2) 0.0391(11) Uani 1 1 d . B . H27A H 0.0713 0.3243 1.0242 0.047 Uiso 1 1 calc R . . H27B H 0.0899 0.4224 1.0608 0.047 Uiso 1 1 calc R . . C24 C 0.13373(18) 0.0641(3) 1.0675(3) 0.0465(12) Uani 1 1 d . . . H24A H 0.1251 0.0221 1.0262 0.056 Uiso 1 1 calc R . . H24B H 0.1648 0.0418 1.1120 0.056 Uiso 1 1 calc R . . C28 C 0.04735(16) 0.4268(4) 0.9448(3) 0.0496(13) Uani 1 1 d . . . H28A H 0.0640 0.4797 0.9395 0.059 Uiso 0.570(7) 1 calc PR B 1 H28B H 0.0412 0.3831 0.9057 0.059 Uiso 0.570(7) 1 calc PR B 1 H28C H 0.0485 0.3966 0.9046 0.059 Uiso 0.430(7) 1 d PR B 2 H28D H 0.0133 0.4212 0.9339 0.059 Uiso 0.430(7) 1 d PR B 2 C25 C 0.0925(2) 0.0598(4) 1.0830(3) 0.0586(15) Uani 1 1 d . . . H25A H 0.0618 0.0841 1.0403 0.088 Uiso 1 1 calc R . . H25B H 0.1022 0.0956 1.1272 0.088 Uiso 1 1 calc R . . H25C H 0.0873 -0.0032 1.0913 0.088 Uiso 1 1 calc R . . C9 C -0.0038(2) 0.7201(4) 0.9180(3) 0.0686(18) Uani 1 1 d . . . H9A H -0.0218 0.6791 0.8756 0.103 Uiso 1 1 calc R . . H9B H -0.0275 0.7538 0.9243 0.103 Uiso 1 1 calc R . . H9C H 0.0182 0.6849 0.9630 0.103 Uiso 1 1 calc R . . C29 C -0.0018(3) 0.4579(6) 0.9273(5) 0.0421(16) Uani 0.570(7) 1 d P B 1 H29A H -0.0206 0.4061 0.9281 0.063 Uiso 0.570(7) 1 calc PR B 1 H29B H -0.0201 0.4857 0.8779 0.063 Uiso 0.570(7) 1 calc PR B 1 H29C H 0.0027 0.5023 0.9644 0.063 Uiso 0.570(7) 1 calc PR B 1 C30 C 0.0601(4) 0.5169(8) 0.9492(6) 0.0421(16) Uani 0.430(7) 1 d P B 2 H30A H 0.0722 0.5397 0.9991 0.063 Uiso 0.430(7) 1 calc PR B 2 H30B H 0.0309 0.5516 0.9126 0.063 Uiso 0.430(7) 1 calc PR B 2 H30C H 0.0861 0.5231 0.9389 0.063 Uiso 0.430(7) 1 calc PR B 2 O14 O 0.1349(3) 0.6240(6) 0.9982(4) 0.0259(8) Uani 0.293(4) 1 d P A 2 N1A N 0.0000 0.4147(4) 0.7500 0.0352(12) Uani 1 2 d S . . O15 O 0.0000 0.2602(4) 0.7500 0.186(6) Uani 1 2 d S . . C1B C 0.0282(4) 0.3478(7) 0.7719(6) 0.052(3) Uani 0.50 1 d PD . . C1A C -0.0520(3) 0.3962(9) 0.7327(6) 0.054(3) Uani 0.50 1 d PD . . C1C C 0.0181(4) 0.5046(6) 0.7612(7) 0.071(5) Uani 0.50 1 d PD . . 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 0.02192(15) 0.01324(15) 0.01545(14) -0.00200(11) 0.01225(12) -0.00278(12) Mo2 0.01971(15) 0.01590(16) 0.01356(14) 0.00375(11) 0.00951(11) 0.00548(12) Mo3 0.01530(14) 0.02234(17) 0.01176(13) -0.00096(11) 0.00701(11) 0.00128(12) Cr 0.0098(3) 0.0097(4) 0.0071(3) -0.0006(3) 0.0052(3) 0.0004(3) O1 0.0148(10) 0.0131(12) 0.0112(10) -0.0012(9) 0.0089(9) -0.0010(9) O2 0.0131(10) 0.0152(12) 0.0147(11) -0.0028(9) 0.0083(9) -0.0011(9) O7 0.0146(11) 0.0234(14) 0.0133(11) 0.0012(10) 0.0066(9) 0.0029(10) O9 0.0181(11) 0.0170(13) 0.0150(11) -0.0029(9) 0.0099(9) -0.0025(10) O3 0.0128(10) 0.0139(12) 0.0131(11) 0.0012(9) 0.0088(9) 0.0035(9) O4 0.0248(12) 0.0142(13) 0.0171(11) 0.0011(9) 0.0142(10) 0.0009(10) O8 0.0308(14) 0.0339(16) 0.0157(12) 0.0030(11) 0.0125(10) 0.0088(12) O12 0.0365(15) 0.0262(15) 0.0178(12) 0.0076(11) 0.0153(11) 0.0070(12) O5 0.0311(14) 0.0269(16) 0.0258(14) -0.0003(11) 0.0170(11) -0.0093(12) O10 0.0325(14) 0.0157(14) 0.0231(13) -0.0005(10) 0.0174(11) 0.0018(11) O11 0.0267(13) 0.0267(16) 0.0250(13) 0.0021(11) 0.0129(11) 0.0100(11) O6 0.0196(13) 0.0400(18) 0.0256(14) -0.0033(12) 0.0099(11) -0.0040(12) N13 0.0144(19) 0.024(2) 0.018(2) 0.000 0.0080(16) 0.000 N14 0.0282(16) 0.0207(17) 0.0181(14) -0.0014(12) 0.0159(13) -0.0033(13) C3 0.0190(16) 0.028(2) 0.0197(17) 0.0018(15) 0.0144(14) 0.0030(15) C1 0.0139(15) 0.0184(18) 0.0127(15) 0.0005(13) 0.0091(12) 0.0009(13) O13 0.0244(17) 0.035(2) 0.0185(16) 0.0010(14) 0.0121(14) 0.0022(15) C2 0.0159(15) 0.0185(19) 0.0160(16) -0.0021(13) 0.0107(13) 0.0009(13) C15 0.0310(19) 0.021(2) 0.0180(17) 0.0029(14) 0.0134(15) 0.0008(16) C4 0.0137(15) 0.0223(19) 0.0170(16) -0.0010(14) 0.0097(13) -0.0025(14) C5 0.0166(15) 0.0145(17) 0.0134(15) -0.0006(12) 0.0107(13) -0.0003(13) C14 0.0250(18) 0.022(2) 0.0203(17) 0.0019(14) 0.0159(15) -0.0003(15) C6 0.0149(16) 0.030(2) 0.0179(17) 0.0033(15) 0.0064(13) 0.0061(15) C18 0.035(2) 0.019(2) 0.0175(17) -0.0021(14) 0.0184(15) -0.0030(15) C10 0.0157(16) 0.030(2) 0.0229(18) -0.0056(15) 0.0092(14) -0.0069(15) C20 0.040(2) 0.019(2) 0.0193(17) -0.0031(15) 0.0179(16) -0.0074(16) C26 0.0269(19) 0.032(2) 0.0189(18) -0.0036(15) 0.0145(15) 0.0003(16) C22 0.037(2) 0.021(2) 0.032(2) -0.0028(16) 0.0258(17) -0.0055(17) C16 0.0285(19) 0.017(2) 0.0244(19) 0.0007(15) 0.0103(15) 0.0013(16) C7 0.029(2) 0.032(2) 0.0235(19) 0.0023(16) 0.0144(16) -0.0005(17) C11 0.0207(18) 0.028(2) 0.0275(19) 0.0018(16) 0.0109(15) -0.0024(16) C17 0.036(2) 0.025(2) 0.039(2) -0.0003(18) 0.0250(18) -0.0006(18) C19 0.040(2) 0.022(2) 0.0228(18) -0.0018(15) 0.0220(17) -0.0077(17) C21 0.045(2) 0.021(2) 0.026(2) 0.0044(16) 0.0211(18) 0.0052(18) C23 0.039(2) 0.028(2) 0.038(2) -0.0121(18) 0.0276(19) -0.0091(18) C12 0.032(2) 0.032(2) 0.039(2) -0.0066(18) 0.0246(19) -0.0057(18) C8 0.049(3) 0.046(3) 0.033(2) 0.014(2) 0.023(2) 0.008(2) C13 0.045(3) 0.038(3) 0.074(3) 0.014(2) 0.043(3) 0.001(2) C27 0.029(2) 0.061(3) 0.030(2) -0.014(2) 0.0177(18) -0.001(2) C24 0.053(3) 0.027(3) 0.063(3) -0.017(2) 0.034(3) -0.005(2) C28 0.029(2) 0.063(4) 0.047(3) -0.004(2) 0.014(2) 0.009(2) C25 0.073(4) 0.035(3) 0.082(4) -0.008(3) 0.050(3) -0.020(3) C9 0.107(5) 0.045(3) 0.037(3) 0.008(2) 0.029(3) -0.027(3) C29 0.033(3) 0.042(4) 0.053(4) 0.013(3) 0.024(3) 0.008(3) C30 0.033(3) 0.042(4) 0.053(4) 0.013(3) 0.024(3) 0.008(3) O14 0.0244(17) 0.035(2) 0.0185(16) 0.0010(14) 0.0121(14) 0.0022(15) N1A 0.037(3) 0.024(3) 0.031(3) 0.000 0.010(2) 0.000 O15 0.410(15) 0.029(4) 0.360(14) 0.000 0.365(14) 0.000 C1B 0.049(6) 0.076(8) 0.048(6) -0.004(5) 0.038(5) -0.002(6) C1A 0.027(5) 0.092(9) 0.042(5) 0.017(6) 0.019(4) 0.002(5) C1C 0.111(13) 0.031(5) 0.046(8) -0.001(5) 0.027(9) -0.035(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 O5 1.701(2) . ? Mo1 O10 1.702(2) . ? Mo1 O9 1.925(2) . ? Mo1 O4 1.937(2) . ? Mo1 O3 2.371(2) 7_567 ? Mo1 O2 2.394(2) . ? Mo2 O11 1.700(2) . ? Mo2 O12 1.703(2) . ? Mo2 O4 1.916(2) . ? Mo2 O7 1.926(2) 7_567 ? Mo2 O3 2.372(2) 7_567 ? Mo2 O1 2.465(2) . ? Mo3 O6 1.697(3) . ? Mo3 O8 1.701(2) . ? Mo3 O9 1.913(2) . ? Mo3 O7 1.919(2) . ? Mo3 O2 2.442(2) . ? Mo3 O1 2.450(2) 7_567 ? Cr O3 1.951(2) 7_567 ? Cr O3 1.951(2) . ? Cr O2 1.957(2) . ? Cr O2 1.957(2) 7_567 ? Cr O1 1.973(2) . ? Cr O1 1.973(2) 7_567 ? O1 C5 1.383(3) . ? O1 Mo3 2.451(2) 7_567 ? O2 C4 1.410(4) . ? O7 Mo2 1.926(2) 7_567 ? O3 C2 1.439(3) . ? O3 Mo1 2.371(2) 7_567 ? O3 Mo2 2.372(2) 7_567 ? N13 C10 1.518(4) 2_556 ? N13 C10 1.518(4) . ? N13 C6 1.522(4) 2_556 ? N13 C6 1.522(4) . ? N14 C26 1.518(4) . ? N14 C22 1.522(5) . ? N14 C18 1.523(4) . ? N14 C14 1.524(4) . ? C3 C1 1.538(4) . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C1 C5 1.531(4) . ? C1 C2 1.531(5) . ? C1 C4 1.546(4) . ? O13 C5 1.187(4) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C15 C14 1.519(5) . ? C15 C16 1.526(5) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C4 O14 1.229(9) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 H5 0.9300 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C6 C7 1.515(5) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C18 C19 1.513(5) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C10 C11 1.520(5) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C20 C21 1.522(5) . ? C20 C19 1.540(5) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C26 C27 1.519(5) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C22 C23 1.521(5) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C16 C17 1.525(5) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C7 C8 1.509(5) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C11 C12 1.525(5) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C23 C24 1.522(6) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C12 C13 1.512(6) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C8 C9 1.504(6) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C27 C28 1.510(6) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C24 C25 1.500(6) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C28 C30 1.354(11) . ? C28 C29 1.455(8) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C28 H28C 0.9701 . ? C28 H28D 0.9699 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C29 H28D 0.6767 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? N1A C1B 1.224(10) 2_556 ? N1A C1B 1.224(10) . ? N1A C1C 1.391(10) 2_556 ? N1A C1C 1.391(10) . ? N1A C1A 1.495(9) 2_556 ? N1A C1A 1.495(9) . ? O15 C1B 1.472(11) . ? O15 C1B 1.472(11) 2_556 ? C1B C1A 1.067(13) 2_556 ? C1B C1B 1.493(18) 2_556 ? C1A C1B 1.067(13) 2_556 ? C1A C1C 1.864(16) 2_556 ? C1C C1C 0.97(2) 2_556 ? C1C C1A 1.863(16) 2_556 ? 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 O5 Mo1 O10 105.80(12) . . ? O5 Mo1 O9 101.89(11) . . ? O10 Mo1 O9 99.93(10) . . ? O5 Mo1 O4 98.71(11) . . ? O10 Mo1 O4 101.92(11) . . ? O9 Mo1 O4 144.45(10) . . ? O5 Mo1 O3 161.90(10) . 7_567 ? O10 Mo1 O3 91.08(10) . 7_567 ? O9 Mo1 O3 81.09(8) . 7_567 ? O4 Mo1 O3 70.83(8) . 7_567 ? O5 Mo1 O2 94.72(11) . . ? O10 Mo1 O2 158.93(10) . . ? O9 Mo1 O2 70.55(8) . . ? O4 Mo1 O2 79.19(8) . . ? O3 Mo1 O2 69.21(7) 7_567 . ? O11 Mo2 O12 105.85(12) . . ? O11 Mo2 O4 103.37(11) . . ? O12 Mo2 O4 99.61(11) . . ? O11 Mo2 O7 98.82(11) . 7_567 ? O12 Mo2 O7 101.85(11) . 7_567 ? O4 Mo2 O7 143.41(10) . 7_567 ? O11 Mo2 O3 92.31(10) . 7_567 ? O12 Mo2 O3 161.27(10) . 7_567 ? O4 Mo2 O3 71.14(8) . 7_567 ? O7 Mo2 O3 79.30(8) 7_567 7_567 ? O11 Mo2 O1 159.16(10) . . ? O12 Mo2 O1 93.76(10) . . ? O4 Mo2 O1 79.68(8) . . ? O7 Mo2 O1 69.69(8) 7_567 . ? O3 Mo2 O1 68.90(7) 7_567 . ? O6 Mo3 O8 105.38(12) . . ? O6 Mo3 O9 104.03(12) . . ? O8 Mo3 O9 100.38(11) . . ? O6 Mo3 O7 99.40(12) . . ? O8 Mo3 O7 102.27(11) . . ? O9 Mo3 O7 141.53(9) . . ? O6 Mo3 O2 90.91(10) . . ? O8 Mo3 O2 162.78(10) . . ? O9 Mo3 O2 69.64(8) . . ? O7 Mo3 O2 80.01(8) . . ? O6 Mo3 O1 158.34(10) . 7_567 ? O8 Mo3 O1 95.54(10) . 7_567 ? O9 Mo3 O1 77.10(8) . 7_567 ? O7 Mo3 O1 70.13(8) . 7_567 ? O2 Mo3 O1 68.96(7) . 7_567 ? O3 Cr O3 180.00(14) 7_567 . ? O3 Cr O2 87.66(9) 7_567 . ? O3 Cr O2 92.34(9) . . ? O3 Cr O2 92.34(9) 7_567 7_567 ? O3 Cr O2 87.66(9) . 7_567 ? O2 Cr O2 179.999(1) . 7_567 ? O3 Cr O1 88.45(9) 7_567 . ? O3 Cr O1 91.55(9) . . ? O2 Cr O1 90.39(9) . . ? O2 Cr O1 89.61(9) 7_567 . ? O3 Cr O1 91.55(9) 7_567 7_567 ? O3 Cr O1 88.45(9) . 7_567 ? O2 Cr O1 89.61(9) . 7_567 ? O2 Cr O1 90.39(9) 7_567 7_567 ? O1 Cr O1 180.00(13) . 7_567 ? C5 O1 Cr 118.61(18) . . ? C5 O1 Mo3 119.82(18) . 7_567 ? Cr O1 Mo3 100.30(8) . 7_567 ? C5 O1 Mo2 124.04(19) . . ? Cr O1 Mo2 99.40(8) . . ? Mo3 O1 Mo2 88.44(7) 7_567 . ? C4 O2 Cr 117.44(19) . . ? C4 O2 Mo1 119.8(2) . . ? Cr O2 Mo1 101.03(8) . . ? C4 O2 Mo3 122.98(18) . . ? Cr O2 Mo3 101.07(9) . . ? Mo1 O2 Mo3 89.10(7) . . ? Mo3 O7 Mo2 126.14(11) . 7_567 ? Mo3 O9 Mo1 124.27(11) . . ? C2 O3 Cr 116.78(19) . . ? C2 O3 Mo1 121.24(18) . 7_567 ? Cr O3 Mo1 102.01(8) . 7_567 ? C2 O3 Mo2 118.87(17) . 7_567 ? Cr O3 Mo2 103.25(9) . 7_567 ? Mo1 O3 Mo2 90.17(7) 7_567 7_567 ? Mo2 O4 Mo1 121.32(11) . . ? C10 N13 C10 110.8(4) 2_556 . ? C10 N13 C6 107.38(19) 2_556 2_556 ? C10 N13 C6 110.47(19) . 2_556 ? C10 N13 C6 110.47(19) 2_556 . ? C10 N13 C6 107.38(19) . . ? C6 N13 C6 110.4(4) 2_556 . ? C26 N14 C22 111.4(3) . . ? C26 N14 C18 111.2(3) . . ? C22 N14 C18 106.0(3) . . ? C26 N14 C14 106.0(2) . . ? C22 N14 C14 111.3(3) . . ? C18 N14 C14 111.0(3) . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C5 C1 C2 111.1(3) . . ? C5 C1 C3 108.8(2) . . ? C2 C1 C3 107.4(3) . . ? C5 C1 C4 109.1(3) . . ? C2 C1 C4 112.2(3) . . ? C3 C1 C4 108.1(3) . . ? O3 C2 C1 114.6(3) . . ? O3 C2 H2A 108.6 . . ? C1 C2 H2A 108.6 . . ? O3 C2 H2B 108.6 . . ? C1 C2 H2B 108.6 . . ? H2A C2 H2B 107.6 . . ? C14 C15 C16 110.9(3) . . ? C14 C15 H15A 109.5 . . ? C16 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? C16 C15 H15B 109.5 . . ? H15A C15 H15B 108.0 . . ? O14 C4 O2 122.3(5) . . ? O14 C4 C1 122.0(5) . . ? O2 C4 C1 114.5(3) . . ? O14 C4 H4A 43.7 . . ? O2 C4 H4A 108.6 . . ? C1 C4 H4A 108.6 . . ? O14 C4 H4B 63.9 . . ? O2 C4 H4B 108.6 . . ? C1 C4 H4B 108.6 . . ? H4A C4 H4B 107.6 . . ? O13 C5 O1 122.0(3) . . ? O13 C5 C1 123.7(3) . . ? O1 C5 C1 114.3(2) . . ? O13 C5 H5 1.3 . . ? O1 C5 H5 122.9 . . ? C1 C5 H5 122.9 . . ? C15 C14 N14 115.1(3) . . ? C15 C14 H14A 108.5 . . ? N14 C14 H14A 108.5 . . ? C15 C14 H14B 108.5 . . ? N14 C14 H14B 108.5 . . ? H14A C14 H14B 107.5 . . ? C7 C6 N13 114.5(3) . . ? C7 C6 H6A 108.6 . . ? N13 C6 H6A 108.6 . . ? C7 C6 H6B 108.6 . . ? N13 C6 H6B 108.6 . . ? H6A C6 H6B 107.6 . . ? C19 C18 N14 115.9(3) . . ? C19 C18 H18A 108.3 . . ? N14 C18 H18A 108.3 . . ? C19 C18 H18B 108.3 . . ? N14 C18 H18B 108.3 . . ? H18A C18 H18B 107.4 . . ? N13 C10 C11 115.5(3) . . ? N13 C10 H10A 108.4 . . ? C11 C10 H10A 108.4 . . ? N13 C10 H10B 108.4 . . ? C11 C10 H10B 108.4 . . ? H10A C10 H10B 107.5 . . ? C21 C20 C19 114.2(3) . . ? C21 C20 H20A 108.7 . . ? C19 C20 H20A 108.7 . . ? C21 C20 H20B 108.7 . . ? C19 C20 H20B 108.7 . . ? H20A C20 H20B 107.6 . . ? N14 C26 C27 115.4(3) . . ? N14 C26 H26A 108.4 . . ? C27 C26 H26A 108.4 . . ? N14 C26 H26B 108.4 . . ? C27 C26 H26B 108.4 . . ? H26A C26 H26B 107.5 . . ? C23 C22 N14 115.7(3) . . ? C23 C22 H22A 108.4 . . ? N14 C22 H22A 108.4 . . ? C23 C22 H22B 108.4 . . ? N14 C22 H22B 108.4 . . ? H22A C22 H22B 107.4 . . ? C17 C16 C15 114.4(3) . . ? C17 C16 H16A 108.7 . . ? C15 C16 H16A 108.7 . . ? C17 C16 H16B 108.7 . . ? C15 C16 H16B 108.7 . . ? H16A C16 H16B 107.6 . . ? C8 C7 C6 110.0(3) . . ? C8 C7 H7A 109.7 . . ? C6 C7 H7A 109.7 . . ? C8 C7 H7B 109.7 . . ? C6 C7 H7B 109.7 . . ? H7A C7 H7B 108.2 . . ? C10 C11 C12 109.7(3) . . ? C10 C11 H11A 109.7 . . ? C12 C11 H11A 109.7 . . ? C10 C11 H11B 109.7 . . ? C12 C11 H11B 109.7 . . ? H11A C11 H11B 108.2 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C18 C19 C20 109.8(3) . . ? C18 C19 H19A 109.7 . . ? C20 C19 H19A 109.7 . . ? C18 C19 H19B 109.7 . . ? C20 C19 H19B 109.7 . . ? H19A C19 H19B 108.2 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C22 C23 C24 110.4(3) . . ? C22 C23 H23A 109.6 . . ? C24 C23 H23A 109.6 . . ? C22 C23 H23B 109.6 . . ? C24 C23 H23B 109.6 . . ? H23A C23 H23B 108.1 . . ? C13 C12 C11 111.9(3) . . ? C13 C12 H12A 109.2 . . ? C11 C12 H12A 109.2 . . ? C13 C12 H12B 109.2 . . ? C11 C12 H12B 109.2 . . ? H12A C12 H12B 107.9 . . ? C9 C8 C7 112.4(4) . . ? C9 C8 H8A 109.1 . . ? C7 C8 H8A 109.1 . . ? C9 C8 H8B 109.1 . . ? C7 C8 H8B 109.1 . . ? H8A C8 H8B 107.9 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C28 C27 C26 110.8(4) . . ? C28 C27 H27A 109.5 . . ? C26 C27 H27A 109.5 . . ? C28 C27 H27B 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 108.1 . . ? C25 C24 C23 115.9(4) . . ? C25 C24 H24A 108.3 . . ? C23 C24 H24A 108.3 . . ? C25 C24 H24B 108.3 . . ? C23 C24 H24B 108.3 . . ? H24A C24 H24B 107.4 . . ? C30 C28 C29 87.3(6) . . ? C30 C28 C27 107.8(6) . . ? C29 C28 C27 120.8(5) . . ? C30 C28 H28A 24.0 . . ? C29 C28 H28A 107.1 . . ? C27 C28 H28A 107.1 . . ? C30 C28 H28B 127.0 . . ? C29 C28 H28B 107.1 . . ? C27 C28 H28B 107.1 . . ? H28A C28 H28B 106.8 . . ? C30 C28 H28C 110.1 . . ? C29 C28 H28C 117.4 . . ? C27 C28 H28C 110.1 . . ? H28A C28 H28C 88.7 . . ? H28B C28 H28C 18.5 . . ? C30 C28 H28D 110.2 . . ? C29 C28 H28D 22.9 . . ? C27 C28 H28D 110.2 . . ? H28A C28 H28D 129.5 . . ? H28B C28 H28D 93.4 . . ? H28C C28 H28D 108.5 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C28 C29 H28D 33.9 . . ? C28 C29 H29A 109.5 . . ? H28D C29 H29A 75.8 . . ? C28 C29 H29B 109.5 . . ? H28D C29 H29B 119.5 . . ? C28 C29 H29C 109.5 . . ? H28D C29 H29C 125.7 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C1B N1A C1B 75.2(10) 2_556 . ? C1B N1A C1C 122.1(7) 2_556 2_556 ? C1B N1A C1C 162.5(8) . 2_556 ? C1B N1A C1C 162.5(7) 2_556 . ? C1B N1A C1C 122.1(7) . . ? C1C N1A C1C 40.8(10) 2_556 . ? C1B N1A C1A 115.1(8) 2_556 2_556 ? C1B N1A C1A 44.9(6) . 2_556 ? C1C N1A C1A 120.2(8) 2_556 2_556 ? C1C N1A C1A 80.3(7) . 2_556 ? C1B N1A C1A 44.8(6) 2_556 . ? C1B N1A C1A 115.1(8) . . ? C1C N1A C1A 80.4(7) 2_556 . ? C1C N1A C1A 120.2(8) . . ? C1A N1A C1A 159.3(11) 2_556 . ? C1B O15 C1B 60.9(8) . 2_556 ? C1A C1B N1A 81.2(9) 2_556 . ? C1A C1B O15 150.7(10) 2_556 . ? N1A C1B O15 111.9(7) . . ? C1A C1B C1B 127.1(10) 2_556 2_556 ? N1A C1B C1B 52.4(5) . 2_556 ? O15 C1B C1B 59.5(4) . 2_556 ? C1B C1A N1A 54.0(7) 2_556 . ? C1B C1A C1C 99.1(9) 2_556 2_556 ? N1A C1A C1C 47.4(5) . 2_556 ? C1C C1C N1A 69.6(5) 2_556 . ? C1C C1C C1A 120.8(5) 2_556 2_556 ? N1A C1C C1A 52.3(5) . 2_556 ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 29.41 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.912 _refine_diff_density_min -0.692 _refine_diff_density_rms 0.106 _database_code_depnum_ccdc_archive 'CCDC 963535' ####################################################################### # # 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_compound3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'H24 Cr Mo6 N3 O27' _chemical_formula_weight 1125.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Cr Cr 0.3209 0.6236 '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' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 2(1)/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.3563(6) _cell_length_b 10.9306(5) _cell_length_c 11.7567(5) _cell_angle_alpha 90.00 _cell_angle_beta 100.137(4) _cell_angle_gamma 90.00 _cell_volume 1436.60(12) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3882 _cell_measurement_theta_min 2.96 _cell_measurement_theta_max 29.18 _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.820 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1172 _exptl_absorpt_coefficient_mu 3.020 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.704 _exptl_absorpt_correction_T_max 0.810 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.0971 _diffrn_reflns_number 6274 _diffrn_reflns_av_R_equivalents 0.0345 _diffrn_reflns_av_sigmaI/netI 0.0524 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 29.18 _reflns_number_total 3297 _reflns_number_gt 2864 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _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 ; XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution ; SHELXS, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3297 _refine_ls_number_parameters 239 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0597 _refine_ls_R_factor_gt 0.0513 _refine_ls_wR_factor_ref 0.1096 _refine_ls_wR_factor_gt 0.1017 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.83952(5) 0.23465(5) 0.07057(5) 0.00962(19) Uani 1 1 d . . . Mo2 Mo 0.70176(5) -0.01658(5) -0.04734(5) 0.01060(19) Uani 1 1 d . . . Cr Cr 1.0000 0.0000 0.0000 0.0063(3) Uani 1 2 d S . . Mo3 Mo 0.86268(5) -0.24763(5) -0.12160(5) 0.00926(19) Uani 1 1 d . . . O3 O 1.1361(4) -0.1020(4) 0.0746(4) 0.0093(9) Uani 1 1 d . . . O2 O 0.8748(4) -0.1150(4) 0.0304(4) 0.0093(9) Uani 1 1 d . . . O7 O 0.8388(4) 0.2948(5) 0.2060(4) 0.0143(10) Uani 1 1 d . . . O8 O 0.7429(5) 0.3214(5) -0.0237(4) 0.0167(10) Uani 1 1 d . . . O10 O 0.6029(4) 0.0705(5) -0.1393(4) 0.0171(11) Uani 1 1 d . . . O12 O 0.8677(4) -0.3047(5) -0.2567(4) 0.0147(10) Uani 1 1 d . . . O6 O 1.0147(4) -0.3086(4) -0.0362(4) 0.0108(9) Uani 1 1 d . . . O1 O 0.9950(4) 0.1065(4) 0.1344(4) 0.0087(9) Uani 1 1 d . . . O5 O 0.7540(4) -0.1153(4) -0.1672(4) 0.0127(10) Uani 1 1 d . . . O11 O 0.7747(5) -0.3466(5) -0.0622(4) 0.0177(11) Uani 1 1 d . . . O4 O 0.7438(4) 0.0899(4) 0.0846(4) 0.0118(9) Uani 1 1 d . . . O9 O 0.6172(5) -0.1184(5) 0.0132(4) 0.0188(11) Uani 1 1 d . . . N2 N 0.6666(7) -0.0396(7) -0.3886(6) 0.0228(15) Uani 1 1 d D . . O14 O 1.0268(9) 0.0449(6) 0.3525(6) 0.044(2) Uani 1 1 d D . . N1 N 0.6417(7) 0.0135(7) 0.2667(7) 0.0284(16) Uani 1 1 d D . . O13 O 0.4967(8) 0.2920(8) -0.2040(13) 0.082(4) Uani 1 1 d G . . H13A H 0.4885 0.2185 -0.2328 0.123 Uiso 1 1 d G . . H13B H 0.5704 0.3158 -0.2000 0.123 Uiso 1 1 d G . . N3 N 0.4940(11) -0.3392(16) -0.094(2) 0.107(9) Uani 1 1 d . . . H1 H 0.979(9) 0.060(9) 0.209(9) 0.04(3) Uiso 1 1 d . . . H1A H 0.618(6) 0.092(3) 0.276(6) 0.000(16) Uiso 1 1 d D . . H1B H 0.692(8) 0.000(7) 0.221(7) 0.01(2) Uiso 1 1 d . . . H2A H 0.687(7) -0.046(7) -0.327(7) 0.000(17) Uiso 1 1 d . . . H1C H 0.592(9) -0.030(10) 0.213(8) 0.06(4) Uiso 1 1 d D . . H3A H 0.480(9) -0.332(9) -0.049(8) 0.00(2) Uiso 1 1 d . . . H14A H 0.983(6) -0.024(4) 0.352(6) 0.006(19) Uiso 1 1 d D . . H3B H 0.522(8) -0.327(9) -0.136(8) 0.00(2) Uiso 1 1 d . . . H2B H 0.680(13) -0.082(12) -0.451(8) 0.10(5) Uiso 1 1 d D . . H14B H 0.956(7) 0.046(8) 0.339(7) 0.00(2) Uiso 1 1 d . . . O15 O 1.695(10) -0.031(13) -0.523(12) 2.2(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0130(3) 0.0084(3) 0.0075(3) -0.0015(2) 0.0020(2) 0.0021(2) Mo2 0.0089(3) 0.0137(3) 0.0089(3) -0.0016(2) 0.0006(2) -0.0004(2) Cr 0.0088(7) 0.0054(7) 0.0043(6) 0.0000(5) 0.0006(5) 0.0008(5) Mo3 0.0129(3) 0.0081(3) 0.0067(3) -0.0021(2) 0.0016(2) -0.0027(2) O3 0.010(2) 0.009(2) 0.008(2) 0.0004(18) 0.0005(16) 0.0034(18) O2 0.008(2) 0.008(2) 0.012(2) -0.0010(18) -0.0004(16) -0.0033(17) O7 0.016(3) 0.017(2) 0.010(2) -0.001(2) 0.0042(18) 0.003(2) O8 0.023(3) 0.017(2) 0.011(2) 0.002(2) 0.0044(19) 0.006(2) O10 0.011(2) 0.022(3) 0.017(2) -0.003(2) 0.0020(19) 0.004(2) O12 0.018(3) 0.019(3) 0.008(2) -0.006(2) 0.0028(18) -0.001(2) O6 0.020(3) 0.003(2) 0.009(2) 0.0024(17) 0.0014(18) 0.0018(18) O1 0.015(2) 0.008(2) 0.0019(19) -0.0021(17) -0.0012(16) 0.0025(18) O5 0.010(2) 0.016(2) 0.010(2) -0.0025(19) -0.0032(17) 0.0006(19) O11 0.022(3) 0.016(3) 0.017(2) -0.001(2) 0.007(2) -0.004(2) O4 0.015(2) 0.011(2) 0.010(2) -0.0027(19) 0.0044(17) -0.0015(19) O9 0.019(3) 0.023(3) 0.017(2) -0.003(2) 0.011(2) -0.006(2) N2 0.027(4) 0.036(4) 0.005(3) 0.003(3) 0.001(3) 0.008(3) O14 0.094(8) 0.020(3) 0.019(3) 0.003(3) 0.015(4) -0.001(4) N1 0.025(4) 0.037(4) 0.026(4) 0.005(3) 0.010(3) 0.002(3) O13 0.035(5) 0.037(4) 0.176(11) 0.038(6) 0.024(6) 0.012(4) N3 0.021(6) 0.085(11) 0.21(2) -0.106(14) 0.011(10) -0.010(6) O15 2.0(4) 2.0(4) 2.0(4) 2.0(4) -1.0(3) -1.0(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 O8 1.705(5) . ? Mo1 O7 1.724(5) . ? Mo1 O4 1.942(5) . ? Mo1 O6 1.947(5) 3_755 ? Mo1 O1 2.275(5) . ? Mo1 O3 2.293(4) 3_755 ? Mo2 O9 1.705(5) . ? Mo2 O10 1.706(5) . ? Mo2 O4 1.931(4) . ? Mo2 O5 1.949(4) . ? Mo2 O2 2.285(5) . ? Mo2 O3 2.319(4) 3_755 ? Cr O1 1.971(4) . ? Cr O1 1.971(4) 3_755 ? Cr O2 1.977(4) 3_755 ? Cr O2 1.977(4) . ? Cr O3 1.981(4) . ? Cr O3 1.981(4) 3_755 ? Mo3 O11 1.704(5) . ? Mo3 O12 1.717(4) . ? Mo3 O5 1.915(5) . ? Mo3 O6 1.955(5) . ? Mo3 O1 2.258(5) 3_755 ? Mo3 O2 2.287(4) . ? O3 Mo1 2.293(4) 3_755 ? O3 Mo2 2.319(4) 3_755 ? O6 Mo1 1.947(5) 3_755 ? O1 Mo3 2.258(5) 3_755 ? O1 H1 1.06(11) . ? O11 O15 1.7(2) 4_456 ? N2 H2A 0.72(8) . ? N2 H2B 0.90(2) . ? O14 H14A 0.90(2) . ? O14 H14B 0.79(7) . ? N1 H1A 0.91(2) . ? N1 H1B 0.86(8) . ? N1 H1C 0.903(15) . ? O13 H13A 0.8699 . ? O13 H13B 0.8700 . ? N3 H3A 0.59(8) . ? N3 H3B 0.65(8) . ? O15 O11 1.7(2) 4_655 ? 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 O8 Mo1 O7 106.3(2) . . ? O8 Mo1 O4 101.7(2) . . ? O7 Mo1 O4 98.0(2) . . ? O8 Mo1 O6 96.2(2) . 3_755 ? O7 Mo1 O6 100.1(2) . 3_755 ? O4 Mo1 O6 149.81(19) . 3_755 ? O8 Mo1 O1 158.53(18) . . ? O7 Mo1 O1 93.4(2) . . ? O4 Mo1 O1 83.34(19) . . ? O6 Mo1 O1 71.65(17) 3_755 . ? O8 Mo1 O3 90.91(19) . 3_755 ? O7 Mo1 O3 161.7(2) . 3_755 ? O4 Mo1 O3 71.98(17) . 3_755 ? O6 Mo1 O3 83.69(17) 3_755 3_755 ? O1 Mo1 O3 70.60(15) . 3_755 ? O9 Mo2 O10 105.8(3) . . ? O9 Mo2 O4 97.8(2) . . ? O10 Mo2 O4 102.4(2) . . ? O9 Mo2 O5 101.9(2) . . ? O10 Mo2 O5 95.8(2) . . ? O4 Mo2 O5 148.3(2) . . ? O9 Mo2 O2 91.9(2) . . ? O10 Mo2 O2 160.09(19) . . ? O4 Mo2 O2 83.61(18) . . ? O5 Mo2 O2 71.24(17) . . ? O9 Mo2 O3 160.3(2) . 3_755 ? O10 Mo2 O3 92.9(2) . 3_755 ? O4 Mo2 O3 71.58(17) . 3_755 ? O5 Mo2 O3 81.91(17) . 3_755 ? O2 Mo2 O3 70.77(16) . 3_755 ? O1 Cr O1 180.0 . 3_755 ? O1 Cr O2 83.83(18) . 3_755 ? O1 Cr O2 96.17(18) 3_755 3_755 ? O1 Cr O2 96.17(18) . . ? O1 Cr O2 83.83(18) 3_755 . ? O2 Cr O2 180.0 3_755 . ? O1 Cr O3 96.17(18) . . ? O1 Cr O3 83.83(18) 3_755 . ? O2 Cr O3 84.69(19) 3_755 . ? O2 Cr O3 95.31(19) . . ? O1 Cr O3 83.83(18) . 3_755 ? O1 Cr O3 96.17(18) 3_755 3_755 ? O2 Cr O3 95.31(19) 3_755 3_755 ? O2 Cr O3 84.69(19) . 3_755 ? O3 Cr O3 180.0 . 3_755 ? O11 Mo3 O12 105.4(2) . . ? O11 Mo3 O5 101.5(2) . . ? O12 Mo3 O5 98.1(2) . . ? O11 Mo3 O6 95.8(2) . . ? O12 Mo3 O6 100.4(2) . . ? O5 Mo3 O6 150.25(19) . . ? O11 Mo3 O1 160.0(2) . 3_755 ? O12 Mo3 O1 92.7(2) . 3_755 ? O5 Mo3 O1 84.19(19) . 3_755 ? O6 Mo3 O1 71.91(17) . 3_755 ? O11 Mo3 O2 92.4(2) . . ? O12 Mo3 O2 161.2(2) . . ? O5 Mo3 O2 71.76(17) . . ? O6 Mo3 O2 83.62(17) . . ? O1 Mo3 O2 70.95(15) 3_755 . ? Cr O3 Mo1 102.31(18) . 3_755 ? Cr O3 Mo2 101.60(18) . 3_755 ? Mo1 O3 Mo2 92.75(15) 3_755 3_755 ? Cr O2 Mo2 102.92(19) . . ? Cr O2 Mo3 102.00(18) . . ? Mo2 O2 Mo3 93.25(16) . . ? Mo1 O6 Mo3 117.3(2) 3_755 . ? Cr O1 Mo3 103.20(18) . 3_755 ? Cr O1 Mo1 103.26(19) . . ? Mo3 O1 Mo1 94.61(18) 3_755 . ? Cr O1 H1 114(5) . . ? Mo3 O1 H1 128(6) 3_755 . ? Mo1 O1 H1 110(6) . . ? Mo3 O5 Mo2 118.6(2) . . ? O15 O11 Mo3 168(3) 4_456 . ? Mo2 O4 Mo1 119.1(2) . . ? H2A N2 H2B 134(10) . . ? H14A O14 H14B 58(7) . . ? H1A N1 H1B 118(7) . . ? H1A N1 H1C 114(9) . . ? H1B N1 H1C 83(9) . . ? H13A O13 H13B 109.5 . . ? H3A N3 H3B 156(10) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 29.18 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 2.596 _refine_diff_density_min -1.331 _refine_diff_density_rms 0.273 _database_code_depnum_ccdc_archive 'CCDC 963536'