# Electronic Supplementary Material (ESI) for CrystEngComm # 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_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C8 H12 Mo8 N4 O26, 4(C4 H7 N2), 2(C4 H6 N2)' _chemical_formula_sum 'C32 H52 Mo8 N16 O26' _chemical_formula_weight 1844.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 12.025(5) _cell_length_b 19.464(8) _cell_length_c 15.323(5) _cell_angle_alpha 90.00 _cell_angle_beta 126.97(2) _cell_angle_gamma 90.00 _cell_volume 2865.4(19) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9219 _cell_measurement_theta_min 2.72 _cell_measurement_theta_max 28.14 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.138 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1800 _exptl_absorpt_coefficient_mu 1.784 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.591 _exptl_absorpt_correction_T_max 0.700 _exptl_absorpt_process_details SADABS,Bruker(2005) _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method ; _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 12955 _diffrn_reflns_av_R_equivalents 0.0183 _diffrn_reflns_av_sigmaI/netI 0.0208 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 25.20 _reflns_number_total ; _reflns_number_gt 4712 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0212P)^2^+4.7316P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5097 _refine_ls_number_parameters 374 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0250 _refine_ls_R_factor_gt 0.0223 _refine_ls_wR_factor_ref 0.0568 _refine_ls_wR_factor_gt 0.0557 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 0.004 _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 C1 C 0.2269(4) 0.88798(17) 0.1213(3) 0.0363(8) Uani 1 1 d . . . H1 H 0.1784 0.9249 0.1220 0.044 Uiso 1 1 calc R . . C2 C 0.3488(4) 0.79426(18) 0.1654(3) 0.0384(8) Uani 1 1 d . . . H2 H 0.3988 0.7547 0.2025 0.046 Uiso 1 1 calc R . . C3 C 0.3231(4) 0.81766(19) 0.0713(3) 0.0438(9) Uani 1 1 d . . . H3 H 0.3524 0.7978 0.0331 0.053 Uiso 1 1 calc R . . C4 C 0.1885(5) 0.9205(2) -0.0535(4) 0.0609(12) Uani 1 1 d . . . H4A H 0.1214 0.9520 -0.0614 0.091 Uiso 1 1 calc R . . H4B H 0.1446 0.8921 -0.1174 0.091 Uiso 1 1 calc R . . H4C H 0.2631 0.9459 -0.0447 0.091 Uiso 1 1 calc R . . C5 C 0.7492(4) 0.78199(17) 0.3695(3) 0.0374(8) Uani 1 1 d . . . H5 H 0.6857 0.7929 0.2959 0.045 Uiso 1 1 calc R . . C6 C 0.8473(4) 0.7697(2) 0.5451(3) 0.0508(10) Uani 1 1 d . . . H6 H 0.8613 0.7710 0.6117 0.061 Uiso 1 1 calc R . . C7 C 0.9380(4) 0.7455(2) 0.5272(3) 0.0466(9) Uani 1 1 d . . . H7 H 1.0257 0.7269 0.5791 0.056 Uiso 1 1 calc R . . C8 C 0.9350(4) 0.7340(2) 0.3599(4) 0.0572(11) Uani 1 1 d . . . H8A H 0.9174 0.6862 0.3408 0.086 Uiso 1 1 calc R . . H8B H 1.0336 0.7420 0.4074 0.086 Uiso 1 1 calc R . . H8C H 0.8935 0.7611 0.2948 0.086 Uiso 1 1 calc R . . C9 C 0.8013(4) 0.9019(2) 0.1400(4) 0.0543(10) Uani 1 1 d . . . H9 H 0.8900 0.8944 0.1595 0.065 Uiso 1 1 calc R . . C10 C 0.6324(5) 0.9203(2) 0.1488(4) 0.0570(11) Uani 1 1 d . . . H10 H 0.5828 0.9282 0.1765 0.068 Uiso 1 1 calc R . . C11 C 0.5767(5) 0.9157(2) 0.0422(4) 0.0603(12) Uani 1 1 d . . . H11 H 0.4830 0.9194 -0.0165 0.072 Uiso 1 1 calc R . . C12 C 0.6736(7) 0.8948(3) -0.0633(4) 0.0864(18) Uani 1 1 d . . . H12A H 0.7650 0.8919 -0.0453 0.130 Uiso 1 1 calc R . . H12B H 0.6248 0.9331 -0.1112 0.130 Uiso 1 1 calc R . . H12C H 0.6234 0.8532 -0.0989 0.130 Uiso 1 1 calc R . . C13 C 0.1162(5) 0.8999(2) 0.4929(4) 0.0595(12) Uani 1 1 d . . . H13 H 0.1690 0.8901 0.4685 0.071 Uiso 1 1 calc R . . C14 C -0.0501(6) 0.9236(2) 0.5051(5) 0.0644(13) Uani 1 1 d . . . H14 H -0.1382 0.9331 0.4857 0.077 Uiso 1 1 calc R . . C15 C 0.0617(7) 0.9203(3) 0.6050(5) 0.0743(15) Uani 1 1 d . . . H15 H 0.0681 0.9270 0.6679 0.089 Uiso 1 1 calc R . . C16 C 0.3122(6) 0.8988(3) 0.6965(5) 0.0921(18) Uani 1 1 d . . . H16A H 0.3456 0.9419 0.7342 0.138 Uiso 1 1 calc R . . H16B H 0.3665 0.8853 0.6724 0.138 Uiso 1 1 calc R . . H16C H 0.3202 0.8644 0.7450 0.138 Uiso 1 1 calc R . . Mo1 Mo 0.52201(3) 0.961244(12) 0.40696(2) 0.02225(7) Uani 1 1 d . . . Mo2 Mo 0.57960(3) 0.837937(13) 0.60362(2) 0.02738(7) Uani 1 1 d . . . Mo3 Mo 0.21283(3) 1.027389(13) 0.30448(2) 0.02561(7) Uani 1 1 d . . . Mo4 Mo 0.30125(3) 0.828169(13) 0.34981(2) 0.02840(8) Uani 1 1 d . . . N1 N 0.2887(3) 0.83864(13) 0.1977(2) 0.0330(6) Uani 1 1 d . . . N2 N 0.2444(3) 0.87694(15) 0.0434(2) 0.0373(7) Uani 1 1 d . . . N3 N 0.7301(3) 0.79206(15) 0.4455(3) 0.0421(7) Uani 1 1 d . . . H3A H 0.6570 0.8096 0.4346 0.051 Uiso 1 1 calc R . . N4 N 0.8746(3) 0.75366(15) 0.4161(2) 0.0369(7) Uani 1 1 d . . . N5 N 0.7734(4) 0.91151(19) 0.2102(3) 0.0588(9) Uani 1 1 d . . . H5A H 0.8320 0.9121 0.2803 0.071 Uiso 1 1 calc R . . N6 N 0.6855(4) 0.90435(17) 0.0372(3) 0.0475(8) Uani 1 1 d . . . N7 N -0.0228(4) 0.91147(16) 0.4310(3) 0.0469(8) Uani 1 1 d . . . N8 N 0.1628(4) 0.90591(18) 0.5998(3) 0.0584(9) Uani 1 1 d . . . O1 O 0.5225(2) 0.86346(10) 0.43118(17) 0.0263(4) Uani 1 1 d . . . O2 O 0.3074(2) 0.93865(10) 0.33904(17) 0.0269(4) Uani 1 1 d . . . O3 O 0.4470(2) 1.04704(10) 0.41516(17) 0.0254(4) Uani 1 1 d . . . O4 O 0.3721(2) 0.83651(11) 0.49823(18) 0.0313(5) Uani 1 1 d . . . O5 O 0.7607(2) 0.87591(10) 0.65567(18) 0.0302(5) Uani 1 1 d . . . O6 O 0.1680(3) 1.03749(12) 0.17510(19) 0.0392(6) Uani 1 1 d . . . O7 O 0.5021(3) 0.96523(12) 0.28660(19) 0.0371(5) Uani 1 1 d . . . O8 O 0.5896(3) 0.83762(13) 0.7204(2) 0.0434(6) Uani 1 1 d . . . O9 O 0.6999(2) 0.97873(11) 0.50726(19) 0.0305(5) Uani 1 1 d . . . O10 O 0.6168(3) 0.75466(11) 0.5921(2) 0.0409(6) Uani 1 1 d . . . O11 O 0.0573(2) 1.00752(12) 0.2810(2) 0.0389(6) Uani 1 1 d . . . O12 O 0.1232(3) 0.82935(13) 0.2819(2) 0.0478(6) Uani 1 1 d . . . O13 O 0.3410(3) 0.74368(12) 0.3456(2) 0.0444(6) 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 C1 0.0377(19) 0.0300(17) 0.0388(19) -0.0039(14) 0.0216(16) 0.0037(14) C2 0.041(2) 0.0303(18) 0.042(2) -0.0027(15) 0.0243(17) 0.0055(15) C3 0.049(2) 0.041(2) 0.046(2) -0.0062(17) 0.0315(19) 0.0047(17) C4 0.070(3) 0.060(3) 0.048(2) 0.014(2) 0.034(2) 0.009(2) C5 0.0336(18) 0.0298(17) 0.044(2) -0.0011(15) 0.0207(17) 0.0005(14) C6 0.060(3) 0.052(2) 0.044(2) 0.0057(18) 0.034(2) 0.011(2) C7 0.045(2) 0.045(2) 0.043(2) 0.0044(17) 0.0222(19) 0.0127(17) C8 0.050(2) 0.069(3) 0.058(3) -0.021(2) 0.036(2) 0.002(2) C9 0.044(2) 0.060(3) 0.054(3) -0.003(2) 0.027(2) -0.005(2) C10 0.068(3) 0.056(3) 0.065(3) -0.004(2) 0.050(3) 0.002(2) C11 0.047(2) 0.068(3) 0.060(3) 0.006(2) 0.029(2) 0.015(2) C12 0.116(5) 0.100(4) 0.062(3) 0.009(3) 0.063(3) 0.031(4) C13 0.077(3) 0.037(2) 0.107(4) -0.008(2) 0.078(3) -0.006(2) C14 0.083(3) 0.043(2) 0.108(4) -0.014(3) 0.078(4) -0.011(2) C15 0.108(5) 0.064(3) 0.086(4) -0.011(3) 0.076(4) -0.021(3) C16 0.085(4) 0.067(4) 0.088(4) 0.013(3) 0.033(3) -0.002(3) Mo1 0.02722(14) 0.01699(13) 0.02870(14) -0.00047(10) 0.02008(12) 0.00104(10) Mo2 0.03582(16) 0.01847(13) 0.03072(15) 0.00207(10) 0.02154(13) 0.00108(11) Mo3 0.02487(14) 0.02136(13) 0.02936(14) -0.00051(10) 0.01565(12) 0.00240(10) Mo4 0.03140(15) 0.02039(14) 0.03427(15) -0.00364(11) 0.02021(13) -0.00386(11) N1 0.0367(16) 0.0251(14) 0.0350(15) -0.0063(11) 0.0204(13) -0.0022(11) N2 0.0400(17) 0.0361(16) 0.0334(15) -0.0013(12) 0.0208(14) 0.0009(13) N3 0.0413(17) 0.0346(16) 0.058(2) -0.0006(14) 0.0340(16) 0.0069(13) N4 0.0330(15) 0.0351(16) 0.0429(17) -0.0063(13) 0.0229(14) 0.0021(12) N5 0.060(2) 0.065(2) 0.0402(19) -0.0096(17) 0.0242(18) -0.0138(18) N6 0.059(2) 0.0432(18) 0.0463(19) 0.0009(14) 0.0350(18) 0.0063(15) N7 0.053(2) 0.0377(17) 0.055(2) -0.0077(15) 0.0350(18) -0.0045(15) N8 0.070(3) 0.0388(19) 0.050(2) 0.0026(15) 0.028(2) -0.0044(17) O1 0.0317(11) 0.0179(10) 0.0339(12) -0.0012(8) 0.0222(10) 0.0006(8) O2 0.0286(11) 0.0188(10) 0.0349(12) -0.0033(9) 0.0199(10) -0.0014(8) O3 0.0309(11) 0.0177(10) 0.0307(11) 0.0002(8) 0.0201(10) 0.0005(8) O4 0.0366(12) 0.0283(12) 0.0372(12) -0.0002(9) 0.0265(11) -0.0028(9) O5 0.0338(12) 0.0208(11) 0.0363(12) 0.0009(9) 0.0211(11) 0.0051(9) O6 0.0465(14) 0.0361(13) 0.0328(13) 0.0026(10) 0.0226(12) 0.0070(11) O7 0.0496(15) 0.0356(13) 0.0377(13) -0.0014(10) 0.0324(12) 0.0001(11) O8 0.0603(17) 0.0398(14) 0.0376(14) 0.0026(11) 0.0335(13) -0.0006(12) O9 0.0284(11) 0.0278(11) 0.0403(13) -0.0022(9) 0.0233(11) -0.0002(9) O10 0.0486(15) 0.0223(12) 0.0523(15) 0.0006(10) 0.0305(13) 0.0028(10) O11 0.0299(12) 0.0396(14) 0.0467(14) -0.0039(11) 0.0227(12) -0.0007(10) O12 0.0352(14) 0.0470(16) 0.0568(17) -0.0063(13) 0.0253(13) -0.0093(11) O13 0.0614(17) 0.0237(12) 0.0485(15) -0.0052(11) 0.0332(14) -0.0019(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.341(4) . ? C1 N2 1.347(4) . ? C1 H1 0.9300 . ? C2 C3 1.357(5) . ? C2 N1 1.394(4) . ? C2 H2 0.9300 . ? C3 N2 1.387(5) . ? C3 H3 0.9300 . ? C4 N2 1.475(5) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 N3 1.331(5) . ? C5 N4 1.338(4) . ? C5 H5 0.9300 . ? C6 C7 1.360(5) . ? C6 N3 1.384(5) . ? C6 H6 0.9300 . ? C7 N4 1.393(5) . ? C7 H7 0.9300 . ? C8 N4 1.473(5) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 N5 1.318(5) . ? C9 N6 1.336(5) . ? C9 H9 0.9300 . ? C10 C11 1.345(6) . ? C10 N5 1.368(6) . ? C10 H10 0.9300 . ? C11 N6 1.374(5) . ? C11 H11 0.9300 . ? C12 N6 1.470(5) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 N7 1.355(6) . ? C13 N8 1.382(6) . ? C13 H13 0.9300 . ? C14 C15 1.296(7) . ? C14 N7 1.379(5) . ? C14 H14 0.9300 . ? C15 N8 1.296(6) . ? C15 H15 0.9300 . ? C16 N8 1.496(6) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? Mo1 O7 1.713(2) . ? Mo1 O9 1.761(2) . ? Mo1 O3 1.937(2) . ? Mo1 O1 1.939(2) . ? Mo1 O2 2.169(2) . ? Mo2 O10 1.719(2) . ? Mo2 O8 1.720(2) . ? Mo2 O5 1.958(2) . ? Mo2 O4 1.997(2) . ? Mo2 O3 2.255(2) 3_676 ? Mo2 O1 2.349(2) . ? Mo3 O11 1.723(2) . ? Mo3 O6 1.725(2) . ? Mo3 O5 1.945(2) 3_676 ? Mo3 O2 1.958(2) . ? Mo3 O3 2.283(2) . ? Mo3 O9 2.408(2) 3_676 ? Mo4 O13 1.725(2) . ? Mo4 O12 1.728(3) . ? Mo4 O4 1.896(2) . ? Mo4 O2 2.161(2) . ? Mo4 N1 2.252(3) . ? Mo4 O1 2.261(2) . ? N3 H3A 0.8600 . ? N5 H5A 0.8600 . ? O3 Mo2 2.255(2) 3_676 ? O5 Mo3 1.945(2) 3_676 ? O9 Mo3 2.408(2) 3_676 ? 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 N1 C1 N2 111.1(3) . . ? N1 C1 H1 124.5 . . ? N2 C1 H1 124.5 . . ? C3 C2 N1 109.5(3) . . ? C3 C2 H2 125.3 . . ? N1 C2 H2 125.3 . . ? C2 C3 N2 106.5(3) . . ? C2 C3 H3 126.8 . . ? N2 C3 H3 126.8 . . ? N2 C4 H4A 109.5 . . ? N2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N3 C5 N4 109.0(3) . . ? N3 C5 H5 125.5 . . ? N4 C5 H5 125.5 . . ? C7 C6 N3 107.2(3) . . ? C7 C6 H6 126.4 . . ? N3 C6 H6 126.4 . . ? C6 C7 N4 106.9(3) . . ? C6 C7 H7 126.6 . . ? N4 C7 H7 126.6 . . ? N4 C8 H8A 109.5 . . ? N4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N5 C9 N6 111.1(4) . . ? N5 C9 H9 124.4 . . ? N6 C9 H9 124.4 . . ? C11 C10 N5 109.4(4) . . ? C11 C10 H10 125.3 . . ? N5 C10 H10 125.3 . . ? C10 C11 N6 106.5(4) . . ? C10 C11 H11 126.8 . . ? N6 C11 H11 126.8 . . ? N6 C12 H12A 109.5 . . ? N6 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N6 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N7 C13 N8 105.4(3) . . ? N7 C13 H13 127.3 . . ? N8 C13 H13 127.3 . . ? C15 C14 N7 111.8(4) . . ? C15 C14 H14 124.1 . . ? N7 C14 H14 124.1 . . ? C14 C15 N8 106.5(5) . . ? C14 C15 H15 126.7 . . ? N8 C15 H15 126.7 . . ? N8 C16 H16A 109.5 . . ? N8 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N8 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O7 Mo1 O9 103.92(11) . . ? O7 Mo1 O3 105.17(10) . . ? O9 Mo1 O3 98.36(9) . . ? O7 Mo1 O1 103.47(10) . . ? O9 Mo1 O1 99.24(9) . . ? O3 Mo1 O1 141.43(9) . . ? O7 Mo1 O2 97.88(10) . . ? O9 Mo1 O2 158.18(9) . . ? O3 Mo1 O2 74.94(8) . . ? O1 Mo1 O2 76.02(8) . . ? O10 Mo2 O8 104.10(12) . . ? O10 Mo2 O5 95.93(11) . . ? O8 Mo2 O5 102.28(11) . . ? O10 Mo2 O4 100.36(11) . . ? O8 Mo2 O4 96.48(12) . . ? O5 Mo2 O4 151.30(9) . . ? O10 Mo2 O3 161.61(10) . 3_676 ? O8 Mo2 O3 92.98(10) . 3_676 ? O5 Mo2 O3 73.45(8) . 3_676 ? O4 Mo2 O3 84.15(8) . 3_676 ? O10 Mo2 O1 90.12(10) . . ? O8 Mo2 O1 164.03(10) . . ? O5 Mo2 O1 83.08(9) . . ? O4 Mo2 O1 73.48(8) . . ? O3 Mo2 O1 73.95(7) 3_676 . ? O11 Mo3 O6 103.65(12) . . ? O11 Mo3 O5 103.60(10) . 3_676 ? O6 Mo3 O5 97.44(10) . 3_676 ? O11 Mo3 O2 103.87(10) . . ? O6 Mo3 O2 98.08(10) . . ? O5 Mo3 O2 144.09(9) 3_676 . ? O11 Mo3 O3 153.18(10) . . ? O6 Mo3 O3 103.17(10) . . ? O5 Mo3 O3 73.06(8) 3_676 . ? O2 Mo3 O3 71.95(8) . . ? O11 Mo3 O9 82.85(10) . 3_676 ? O6 Mo3 O9 173.08(10) . 3_676 ? O5 Mo3 O9 78.49(8) 3_676 3_676 ? O2 Mo3 O9 82.45(8) . 3_676 ? O3 Mo3 O9 70.38(7) . 3_676 ? O13 Mo4 O12 105.12(13) . . ? O13 Mo4 O4 101.07(11) . . ? O12 Mo4 O4 102.76(12) . . ? O13 Mo4 O2 157.34(11) . . ? O12 Mo4 O2 91.60(10) . . ? O4 Mo4 O2 89.72(9) . . ? O13 Mo4 N1 83.97(11) . . ? O12 Mo4 N1 95.06(12) . . ? O4 Mo4 N1 159.35(10) . . ? O2 Mo4 N1 79.34(9) . . ? O13 Mo4 O1 92.85(11) . . ? O12 Mo4 O1 161.52(10) . . ? O4 Mo4 O1 77.40(9) . . ? O2 Mo4 O1 69.93(7) . . ? N1 Mo4 O1 82.38(9) . . ? C1 N1 C2 105.5(3) . . ? C1 N1 Mo4 128.7(2) . . ? C2 N1 Mo4 125.8(2) . . ? C1 N2 C3 107.5(3) . . ? C1 N2 C4 125.5(3) . . ? C3 N2 C4 127.0(3) . . ? C5 N3 C6 108.7(3) . . ? C5 N3 H3A 125.6 . . ? C6 N3 H3A 125.6 . . ? C5 N4 C7 108.2(3) . . ? C5 N4 C8 126.0(3) . . ? C7 N4 C8 125.7(3) . . ? C9 N5 C10 106.0(4) . . ? C9 N5 H5A 127.0 . . ? C10 N5 H5A 127.0 . . ? C9 N6 C11 107.0(4) . . ? C9 N6 C12 127.3(4) . . ? C11 N6 C12 125.7(4) . . ? C13 N7 C14 104.9(4) . . ? C15 N8 C13 111.4(4) . . ? C15 N8 C16 124.9(5) . . ? C13 N8 C16 123.8(5) . . ? Mo1 O1 Mo4 109.00(9) . . ? Mo1 O1 Mo2 112.84(9) . . ? Mo4 O1 Mo2 90.41(8) . . ? Mo3 O2 Mo4 149.01(11) . . ? Mo3 O2 Mo1 106.32(9) . . ? Mo4 O2 Mo1 104.52(8) . . ? Mo1 O3 Mo2 152.04(11) . 3_676 ? Mo1 O3 Mo3 102.81(9) . . ? Mo2 O3 Mo3 93.12(8) 3_676 . ? Mo4 O4 Mo2 114.36(11) . . ? Mo3 O5 Mo2 115.16(10) 3_676 . ? Mo1 O9 Mo3 117.48(10) . 3_676 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N5 H5A N7 0.86 1.88 2.736(5) 172.8 1_655 N3 H3A O1 0.86 1.90 2.748(4) 167.6 . _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.20 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.077 _refine_diff_density_min -0.506 _refine_diff_density_rms 0.084 _database_code_depnum_ccdc_archive 'CCDC 939800' ####################################################################### # # 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_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C8 H12 Mo8 N4 O26, 4(C4 H6 N2), 4(C4 H7 N2)' _chemical_formula_sum 'C40 H64 Mo8 N20 O26' _chemical_formula_weight 2008.63 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.379(3) _cell_length_b 10.932(2) _cell_length_c 24.384(4) _cell_angle_alpha 90.00 _cell_angle_beta 134.332(8) _cell_angle_gamma 90.00 _cell_volume 3313.8(11) _cell_formula_units_Z 2 _cell_measurement_tempera ture _cell_measurement_reflns_used 8901 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 28.20 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.013 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 ; _exptl_absorpt_coefficient_mu 1.553 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.696 _exptl_absorpt_correction_T_max 0.792 _exptl_absorpt_process_details SADABS,Bruker(2005) _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans ' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15774 _diffrn_reflns_av_R_equivalents 0.0262 _diffrn_reflns_av_sigmaI/netI 0.0319 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 25.20 _reflns_number_total 5970 _reflns_number_gt 5499 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Br uker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0403P)^2^+422.3990P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5858 _refine_ls_number_parameters 429 _refine_ls_number_restraints 870 _refine_ls_R_factor_all 0.1302 _refine_ls_R_factor_gt 0.1255 _refine_ls_wR_factor_ref 0.3351 _refine_ls_wR_ factor_gt _refine_ls_goodness_of_fit_ref 1.183 _refine_ls_restrained_S_all 1.104 _refine_ls_shift/su_max 0.016 _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 0.57218(15) 0.66914(17) 0.12198(10) 0.0259(4) Uani 1 1 d . . . Mo2 Mo 0.76637(14) 0.55412(17) 0.14351(10) 0.0255(4) Uani 1 1 d . . . Mo3 Mo 0.28027(15) 0.55250(17) 0.00279(11) 0.0267(5) Uani 1 1 d . . . Mo4 Mo 0.48249(13) 0.39437(15) 0.04284(10) 0.0207(4) Uani 1 1 d . . . O1 O 0.4454(11) 0.5687(12) 0.0630(8) 0.025(3) Uani 1 1 d U . . O2 O 0.5305(13) 0.8131(15) 0.1183(10) 0.040(4) Uani 1 1 d U . . O3 O 0.5914(11) 0.5084(12) 0.0733(8) 0.023(3) Uani 1 1 d U . . O4 O 0.6333(14) 0.6185(18) 0.2112(10) 0.046(4) Uani 1 1 d U . . O5 O 0.5378(13) 0.3281(15) 0.1257(9) 0.039(4) Uani 1 1 d U . . O6 O 0.6659(11) 0.6129(13) 0.0192(8) 0.028(3) Uani 1 1 d U . . O7 O 0.2785(15) 0.6934(16) 0.0339(11) 0.047(4) Uani 1 1 d U . . O8 O 0.8767(13) 0.6243(15) 0.1710(10) 0.038(4) Uani 1 1 d U . . O9 O 0.4995(11) 0.7172(12) -0.0011(9) 0.025(3) Uani 1 1 d U . . O10 O 0.8081(14) 0.4732(17) 0.2208(10) 0.049(4) Uani 1 1 d U . . O11 O 0.1660(13) 0.4805(15) -0.0305(10) 0.037(4) Uani 1 1 d U . . O12 O 0.7045(11) 0.6974(13) 0.1473(8) 0.027(3) Uani 1 1 d U . . O13 O 0.7579(11) 0.4111(13) 0.0904(8) 0.027(3) Uani 1 1 d U . . N1 N 0.3538(17) 0.4543(18) 0.1123(12) 0.038(4) Uani 1 1 d U . . N2 N 0.4654(17) 0.3683(19) 0.2260(11) 0.039(4) Uani 1 1 d U . . C1 C 0.4536(19) 0.454(2) 0.1785(13) 0.033(4) Uani 1 1 d U . . H1 H 0.5082 0.5026 0.1917 0.040 Uiso 1 1 calc R . . C2 C 0.301(2) 0.367(2) 0.1185(14) 0.035(4) Uani 1 1 d U . . H2 H 0.2293 0.3446 0.0798 0.042 Uiso 1 1 calc R . . C3 C 0.371(2) 0.321(2) 0.1882(15) 0.040(4) Uani 1 1 d U . . H3 H 0.3552 0.2643 0.2076 0.048 Uiso 1 1 calc R . . C4 C 0.569(2) 0.342(3) 0.3053(16) 0.052(6) Uani 1 1 d U . . H4A H 0.5785 0.3979 0.3401 0.078 Uiso 1 1 calc R . . H4B H 0.6268 0.3516 0.3085 0.078 Uiso 1 1 calc R . . H4C H 0.5682 0.2597 0.3187 0.078 Uiso 1 1 calc R . . N7 N 0.2217(19) 0.676(2) 0.3660(14) 0.052(5) Uani 1 1 d U . . H7A H 0.2268 0.7520 0.3781 0.062 Uiso 1 1 d R . . N8 N 0.1560(19) 0.503(2) 0.3089(14) 0.048(4) Uani 1 1 d U . . C9 C 0.134(3) 0.618(3) 0.3152(18) 0.055(6) Uani 1 1 d U . . H9 H 0.0651 0.6487 0.2871 0.066 Uiso 1 1 calc R . . C10 C 0.316(2) 0.593(3) 0.4016(17) 0.050(5) Uani 1 1 d U . . H10 H 0.3888 0.6116 0.4386 0.060 Uiso 1 1 calc R . . C11 C 0.267(3) 0.480(3) 0.3653(19) 0.063(6) Uani 1 1 d U . . H11 H 0.3005 0.4050 0.3765 0.076 Uiso 1 1 calc R . . C12 C 0.067(3) 0.405(3) 0.261(2) 0.080(10) Uani 1 1 d U . . H12A H 0.0002 0.4385 0.2403 0.120 Uiso 1 1 calc R . . H12B H 0.0865 0.3362 0.2933 0.120 Uiso 1 1 calc R . . H12C H 0.0596 0.3784 0.2199 0.120 Uiso 1 1 calc R . . N3 N 0.950(2) 0.785(3) 0.3821(16) 0.070(6) Uani 1 1 d U . . N4 N 0.883(2) 0.642(3) 0.4016(15) 0.059(5) Uani 1 1 d U . . C17 C 0.882(2) 0.702(3) 0.3534(17) 0.048(5) Uani 1 1 d U . . H17 H 0.8331 0.6832 0.3014 0.058 Uiso 1 1 calc R . . C18 C 1.009(3) 0.794(3) 0.458(2) 0.077(8) Uani 1 1 d U . . H18 H 1.0630 0.8493 0.4937 0.093 Uiso 1 1 calc R . . C19 C 0.969(3) 0.701(3) 0.469(2) 0.067(7) Uani 1 1 d U . . H19 H 0.9955 0.6791 0.5169 0.080 Uiso 1 1 calc R . . C20 C 0.818(3) 0.544(3) 0.389(2) 0.072(8) Uani 1 1 d U . . H20A H 0.7432 0.5617 0.3445 0.108 Uiso 1 1 calc R . . H20B H 0.8282 0.5340 0.4327 0.108 Uiso 1 1 calc R . . H20C H 0.8371 0.4695 0.3799 0.108 Uiso 1 1 calc R . . N5 N 0.8929(19) 1.223(2) 0.3274(13) 0.053(5) Uani 1 1 d U . . N6 N 0.7496(17) 1.123(2) 0.2785(12) 0.044(4) Uani 1 1 d U . . C13 C 0.787(2) 1.230(3) 0.2775(17) 0.053(6) Uani 1 1 d U . . H13 H 0.7456 1.2979 0.2471 0.064 Uiso 1 1 calc R . . C14 C 0.925(3) 1.112(3) 0.3604(19) 0.069(7) Uani 1 1 d U . . H14 H 0.9948 1.0820 0.3962 0.083 Uiso 1 1 calc R . . C15 C 0.836(2) 1.054(3) 0.3311(17) 0.055(5) Uani 1 1 d U . . H15 H 0.8335 0.9763 0.3453 0.066 Uiso 1 1 calc R . . C16 C 0.636(2) 1.089(3) 0.228(2) 0.068(8) Uani 1 1 d U . . H16A H 0.6245 1.0111 0.2045 0.103 Uiso 1 1 calc R . . H16B H 0.5917 1.1495 0.1885 0.103 Uiso 1 1 calc R . . H16C H 0.6183 1.0827 0.2570 0.103 Uiso 1 1 calc R . . N9 N 0.2359(18) 0.421(2) 0.4868(14) 0.048(4) Uani 1 1 d U . . N10 N 0.0621(19) 0.373(2) 0.3951(14) 0.049(4) Uani 1 1 d U . . H10A H 0.0039 0.3318 0.3624 0.059 Uiso 1 1 calc R . . C5 C 0.169(2) 0.331(3) 0.4485(17) 0.052(5) Uani 1 1 d U . . H5 H 0.1888 0.2492 0.4553 0.062 Uiso 1 1 calc R . . C6 C 0.073(2) 0.498(3) 0.4078(17) 0.049(5) Uani 1 1 d U . . H6 H 0.0174 0.5545 0.3822 0.059 Uiso 1 1 calc R . . C7 C 0.185(2) 0.525(3) 0.4665(18) 0.052(5) Uani 1 1 d U . . H7 H 0.2155 0.6019 0.4868 0.062 Uiso 1 1 calc R . . C8 C 0.356(3) 0.404(3) 0.544(2) 0.070(8) Uani 1 1 d U . . H8A H 0.3769 0.3316 0.5732 0.105 Uiso 1 1 calc R . . H8B H 0.3914 0.4738 0.5770 0.105 Uiso 1 1 calc R . . H8C H 0.3775 0.3967 0.5163 0.105 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 0.0276(9) 0.0228(9) 0.0270(9) -0.0046(7) 0.0190(8) -0.0042(7) Mo2 0.0209(9) 0.0222(9) 0.0242(9) 0.0011(7) 0.0124(8) -0.0014(7) Mo3 0.0266(9) 0.0223(9) 0.0315(10) 0.0022(7) 0.0205(9) 0.0012(7) Mo4 0.0211(8) 0.0145(8) 0.0223(8) 0.0031(6) 0.0136(7) -0.0001(6) O1 0.034(5) 0.018(5) 0.028(5) 0.002(4) 0.024(4) -0.006(4) O2 0.037(7) 0.032(8) 0.057(8) -0.006(7) 0.035(7) -0.005(6) O3 0.028(5) 0.019(5) 0.028(5) 0.001(4) 0.022(4) 0.001(4) O4 0.046(7) 0.049(8) 0.041(7) -0.005(7) 0.030(6) -0.008(7) O5 0.042(8) 0.033(8) 0.031(7) 0.011(6) 0.022(6) 0.003(6) O6 0.030(6) 0.016(6) 0.033(6) 0.005(5) 0.020(5) 0.003(5) O7 0.049(9) 0.030(8) 0.058(9) -0.002(7) 0.036(7) -0.003(7) O8 0.032(7) 0.028(8) 0.056(9) -0.002(7) 0.032(7) -0.006(6) O9 0.026(5) 0.020(6) 0.038(6) 0.005(5) 0.025(5) 0.006(5) O10 0.036(8) 0.039(8) 0.040(8) 0.004(7) 0.015(7) -0.006(7) O11 0.031(7) 0.030(8) 0.046(8) 0.009(7) 0.026(7) 0.005(6) O12 0.027(5) 0.024(5) 0.035(5) -0.002(5) 0.023(4) 0.000(4) O13 0.017(5) 0.021(6) 0.038(6) 0.005(5) 0.018(5) 0.004(5) N1 0.043(6) 0.030(7) 0.044(6) 0.003(6) 0.031(5) -0.003(6) N2 0.055(7) 0.034(7) 0.036(7) -0.002(6) 0.035(6) 0.000(6) C1 0.043(7) 0.031(7) 0.038(7) 0.001(6) 0.032(5) -0.006(6) C2 0.047(7) 0.036(8) 0.044(7) -0.004(7) 0.040(6) -0.011(7) C3 0.047(8) 0.039(8) 0.046(8) 0.001(7) 0.037(6) -0.004(7) C4 0.054(11) 0.055(12) 0.051(11) 0.000(10) 0.038(9) 0.009(10) N7 0.056(8) 0.034(7) 0.065(8) -0.003(7) 0.042(7) -0.004(7) N8 0.055(7) 0.035(6) 0.062(7) -0.006(6) 0.044(6) -0.003(6) C9 0.060(8) 0.037(8) 0.063(8) -0.007(7) 0.041(7) 0.001(7) C10 0.058(8) 0.039(7) 0.062(8) -0.002(7) 0.045(7) -0.006(7) C11 0.065(8) 0.041(8) 0.065(8) -0.007(7) 0.039(7) 0.000(7) C12 0.068(12) 0.045(11) 0.071(12) -0.005(10) 0.028(10) 0.003(10) N3 0.049(8) 0.065(8) 0.060(8) 0.004(7) 0.026(7) 0.002(7) N4 0.049(8) 0.063(9) 0.055(8) 0.006(8) 0.033(7) 0.003(8) C17 0.044(7) 0.058(8) 0.048(7) 0.007(7) 0.034(6) 0.000(7) C18 0.054(9) 0.065(9) 0.061(9) 0.003(8) 0.022(8) 0.000(8) C19 0.051(9) 0.068(10) 0.059(9) 0.006(9) 0.030(8) 0.003(8) C20 0.051(11) 0.063(13) 0.074(13) 0.010(12) 0.034(10) -0.005(11) N5 0.048(8) 0.053(9) 0.048(8) -0.003(7) 0.029(7) -0.003(7) N6 0.041(7) 0.052(9) 0.047(8) 0.003(7) 0.034(6) -0.009(7) C13 0.044(8) 0.051(9) 0.052(9) 0.005(8) 0.029(7) -0.005(8) C14 0.049(8) 0.057(9) 0.058(9) 0.004(8) 0.021(7) -0.005(8) C15 0.045(7) 0.059(8) 0.054(8) 0.007(7) 0.032(6) -0.005(7) C16 0.044(11) 0.053(12) 0.069(12) 0.012(11) 0.025(10) -0.004(10) N9 0.048(7) 0.039(7) 0.063(7) -0.004(6) 0.040(6) 0.003(6) N10 0.049(7) 0.042(7) 0.070(8) -0.002(7) 0.046(6) 0.000(6) C5 0.053(8) 0.032(8) 0.067(8) -0.006(7) 0.040(7) 0.003(7) C6 0.053(7) 0.037(7) 0.066(8) -0.001(7) 0.045(6) 0.005(7) C7 0.059(7) 0.035(7) 0.064(7) -0.006(6) 0.044(6) -0.002(6) C8 0.055(11) 0.048(12) 0.075(12) -0.007(11) 0.033(10) -0.002(10) _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 O2 1.708(16) . ? Mo1 O4 1.713(18) . ? Mo1 O1 1.923(14) . ? Mo1 O12 1.944(14) . ? Mo1 O3 2.273(14) . ? Mo1 O9 2.363(15) . ? Mo2 O8 1.708(15) . ? Mo2 O10 1.718(18) . ? Mo2 O12 1.939(14) . ? Mo2 O13 1.970(15) . ? Mo2 O3 2.270(14) . ? Mo2 O6 2.293(14) . ? Mo3 O11 1.722(16) . ? Mo3 O7 1.727(18) . ? Mo3 O13 1.912(15) 3_665 ? Mo3 O1 2.130(14) . ? Mo3 O6 2.266(15) 3_665 ? Mo3 N1 2.27(2) . ? Mo4 O5 1.678(15) . ? Mo4 O9 1.751(14) 3_665 ? Mo4 O6 1.869(14) 3_665 ? Mo4 O3 1.929(14) . ? Mo4 O1 2.176(14) . ? Mo4 O3 2.391(13) 3_665 ? O3 Mo4 2.391(13) 3_665 ? O6 Mo4 1.869(14) 3_665 ? O6 Mo3 2.266(14) 3_665 ? O9 Mo4 1.751(14) 3_665 ? O13 Mo3 1.912(15) 3_665 ? N1 C1 1.30(3) . ? N1 C2 1.40(3) . ? N2 C3 1.30(3) . ? N2 C1 1.39(3) . ? N2 C4 1.48(3) . ? C1 H1 0.9300 . ? C2 C3 1.31(3) . ? C2 H2 0.9300 . ? C3 H3 0.9300 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? N7 C9 1.28(4) . ? N7 C10 1.51(4) . ? N7 H7A 0.8601 . ? N8 C9 1.35(4) . ? N8 C11 1.40(4) . ? N8 C12 1.55(4) . ? C9 H9 0.9300 . ? C10 C11 1.41(4) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? N3 C17 1.24(4) . ? N3 C18 1.36(4) . ? N4 C17 1.33(4) . ? N4 C19 1.38(4) . ? N4 C20 1.43(4) . ? C17 H17 0.9300 . ? C18 C19 1.37(5) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? N5 C14 1.34(4) . ? N5 C13 1.32(4) . ? N6 C15 1.33(4) . ? N6 C13 1.34(3) . ? N6 C16 1.47(3) . ? C13 H13 0.9300 . ? C14 C15 1.33(4) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? N9 C5 1.29(3) . ? N9 C7 1.32(4) . ? N9 C8 1.51(4) . ? N10 C6 1.38(3) . ? N10 C5 1.41(4) . ? N10 H10A 0.8600 . ? C5 H5 0.9300 . ? C6 C7 1.42(4) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Mo1 O4 103.2(9) . . ? O2 Mo1 O1 105.4(7) . . ? O4 Mo1 O1 97.7(7) . . ? O2 Mo1 O12 103.5(7) . . ? O4 Mo1 O12 95.8(8) . . ? O1 Mo1 O12 144.2(6) . . ? O2 Mo1 O3 153.7(7) . . ? O4 Mo1 O3 103.1(7) . . ? O1 Mo1 O3 71.2(5) . . ? O12 Mo1 O3 73.5(5) . . ? O2 Mo1 O9 84.1(7) . . ? O4 Mo1 O9 172.4(7) . . ? O1 Mo1 O9 82.0(5) . . ? O12 Mo1 O9 80.4(6) . . ? O3 Mo1 O9 69.6(5) . . ? O8 Mo2 O10 107.6(8) . . ? O8 Mo2 O12 97.3(7) . . ? O10 Mo2 O12 100.8(8) . . ? O8 Mo2 O13 99.3(7) . . ? O10 Mo2 O13 95.3(8) . . ? O12 Mo2 O13 152.2(6) . . ? O8 Mo2 O3 160.0(7) . . ? O10 Mo2 O3 91.7(7) . . ? O12 Mo2 O3 73.7(5) . . ? O13 Mo2 O3 83.3(5) . . ? O8 Mo2 O6 90.1(7) . . ? O10 Mo2 O6 160.6(7) . . ? O12 Mo2 O6 84.4(6) . . ? O13 Mo2 O6 73.4(5) . . ? O3 Mo2 O6 71.6(5) . . ? O11 Mo3 O7 104.3(8) . . ? O11 Mo3 O13 101.9(7) . 3_665 ? O7 Mo3 O13 103.8(8) . 3_665 ? O11 Mo3 O1 156.5(6) . . ? O7 Mo3 O1 93.0(7) . . ? O13 Mo3 O1 89.1(5) 3_665 . ? O11 Mo3 O6 93.1(7) . 3_665 ? O7 Mo3 O6 162.4(7) . 3_665 ? O13 Mo3 O6 75.1(5) 3_665 3_665 ? O1 Mo3 O6 69.5(5) . 3_665 ? O11 Mo3 N1 81.6(7) . . ? O7 Mo3 N1 94.2(8) . . ? O13 Mo3 N1 160.0(7) 3_665 . ? O1 Mo3 N1 81.3(6) . . ? O6 Mo3 N1 85.1(6) 3_665 . ? O5 Mo4 O9 102.4(8) . 3_665 ? O5 Mo4 O6 105.1(7) . 3_665 ? O9 Mo4 O6 101.9(7) 3_665 3_665 ? O5 Mo4 O3 103.5(7) . . ? O9 Mo4 O3 98.5(6) 3_665 . ? O6 Mo4 O3 140.1(6) 3_665 . ? O5 Mo4 O1 96.7(7) . . ? O9 Mo4 O1 160.6(6) 3_665 . ? O6 Mo4 O1 76.2(6) 3_665 . ? O3 Mo4 O1 73.3(5) . . ? O5 Mo4 O3 178.3(7) . 3_665 ? O9 Mo4 O3 77.7(6) 3_665 3_665 ? O6 Mo4 O3 76.4(5) 3_665 3_665 ? O3 Mo4 O3 74.9(6) . 3_665 ? O1 Mo4 O3 83.1(5) . 3_665 ? Mo1 O1 Mo3 148.3(8) . . ? Mo1 O1 Mo4 107.7(7) . . ? Mo3 O1 Mo4 103.9(6) . . ? Mo4 O3 Mo2 150.4(7) . . ? Mo4 O3 Mo1 103.8(6) . . ? Mo2 O3 Mo1 92.5(5) . . ? Mo4 O3 Mo4 105.1(6) . 3_665 ? Mo2 O3 Mo4 97.1(5) . 3_665 ? Mo1 O3 Mo4 97.0(5) . 3_665 ? Mo4 O6 Mo3 109.8(7) 3_665 3_665 ? Mo4 O6 Mo2 113.8(7) 3_665 . ? Mo3 O6 Mo2 91.7(5) 3_665 . ? Mo4 O9 Mo1 115.4(7) 3_665 . ? Mo2 O12 Mo1 115.4(7) . . ? Mo3 O13 Mo2 114.9(7) 3_665 . ? C1 N1 C2 105(2) . . ? C1 N1 Mo3 128.9(16) . . ? C2 N1 Mo3 125.2(16) . . ? C3 N2 C1 107(2) . . ? C3 N2 C4 129(2) . . ? C1 N2 C4 124(2) . . ? N1 C1 N2 109(2) . . ? N1 C1 H1 125.3 . . ? N2 C1 H1 125.3 . . ? C3 C2 N1 109(2) . . ? C3 C2 H2 125.7 . . ? N1 C2 H2 125.7 . . ? C2 C3 N2 109(2) . . ? C2 C3 H3 125.3 . . ? N2 C3 H3 125.3 . . ? N2 C4 H4A 109.5 . . ? N2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C9 N7 C10 110(2) . . ? C9 N7 H7A 125.5 . . ? C10 N7 H7A 125.0 . . ? C9 N8 C11 111(2) . . ? C9 N8 C12 121(3) . . ? C11 N8 C12 125(2) . . ? N7 C9 N8 109(3) . . ? N7 C9 H9 125.3 . . ? N8 C9 H9 125.3 . . ? C11 C10 N7 103(3) . . ? C11 C10 H10 128.3 . . ? N7 C10 H10 128.3 . . ? C10 C11 N8 106(3) . . ? C10 C11 H11 127.2 . . ? N8 C11 H11 127.2 . . ? N8 C12 H12A 109.5 . . ? N8 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N8 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C17 N3 C18 110(3) . . ? C17 N4 C19 100(3) . . ? C17 N4 C20 131(3) . . ? C19 N4 C20 130(3) . . ? N3 C17 N4 116(3) . . ? N3 C17 H17 122.1 . . ? N4 C17 H17 122.1 . . ? N3 C18 C19 102(3) . . ? N3 C18 H18 128.9 . . ? C19 C18 H18 128.9 . . ? C18 C19 N4 112(3) . . ? C18 C19 H19 123.8 . . ? N4 C19 H19 123.8 . . ? N4 C20 H20A 109.5 . . ? N4 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? N4 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C14 N5 C13 110(3) . . ? C15 N6 C13 106(2) . . ? C15 N6 C16 127(2) . . ? C13 N6 C16 126(2) . . ? N5 C13 N6 108(3) . . ? N5 C13 H13 126.1 . . ? N6 C13 H13 126.1 . . ? N5 C14 C15 106(3) . . ? N5 C14 H14 127.2 . . ? C15 C14 H14 127.2 . . ? N6 C15 C14 110(3) . . ? N6 C15 H15 124.8 . . ? C14 C15 H15 124.8 . . ? N6 C16 H16A 109.5 . . ? N6 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N6 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C5 N9 C7 111(2) . . ? C5 N9 C8 123(2) . . ? C7 N9 C8 126(3) . . ? C6 N10 C5 103(2) . . ? C6 N10 H10A 128.3 . . ? C5 N10 H10A 128.3 . . ? N9 C5 N10 111(2) . . ? N9 C5 H5 124.5 . . ? N10 C5 H5 124.5 . . ? N10 C6 C7 108(2) . . ? N10 C6 H6 125.9 . . ? C7 C6 H6 125.9 . . ? N9 C7 C6 107(2) . . ? N9 C7 H7 126.7 . . ? C6 C7 H7 126.7 . . ? N9 C8 H8A 109.5 . . ? N9 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N9 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 25.20 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 1.930 _refine_diff_density_min -1.850 _refine_diff_density_rms 0.395 _database_code_depnum_ccdc_archive 'CCDC 939801' ####################################################################### # # 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_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H16 Mo8 N4 O26, 4(C5 H9 N2)' _chemical_formula_sum 'C30 H52 Mo8 N12 O26' _chemical_formula_weight 1764.36 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' 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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.3366(13) _cell_length_b 11.3529(13) _cell_length_c 11.3639(14) _cell_angle_alpha 72.391(2) _cell_angle_beta 71.058(2) _cell_angle_gamma 80.060(2) _cell_volume 1314.1(3) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_ measurement_reflns_used _cell_measurement_theta_min 2.79 _cell_measurement_theta_max 28.38 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.230 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 860 _exptl_absorpt_coefficient_mu 1.937 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.634 _exptl_absorpt_correction_T_max 0.748 _exptl_absorpt_process_details SADABS,Bruker(2005) _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 6255 _diffrn_reflns_av_R_equivalents 0.0147 _diffrn_reflns_av_sigmaI/netI 0.0266 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 25.20 _reflns_number_total 4733 _reflns_number_gt &n _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0292P)^2^+1.5524P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4531 _refine_ls_number_parameters 346 _refine_ls_number_restraints 198 _refine_ls_R_factor_all 0.0276 _refine_ls_R_factor_gt 0.0234 _refine_ls_wR_factor_ref 0.0604 _refine_ls_wR_factor_gt 0.0576 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.4462(3) 0.1275(3) 0.7038(4) 0.0322(8) Uani 1 1 d U . . H1 H 0.4529 0.0942 0.7871 0.039 Uiso 1 1 calc R . . C2 C 0.4885(4) 0.1706(4) 0.4945(4) 0.0391(9) Uani 1 1 d U . . H2 H 0.5281 0.1728 0.4083 0.047 Uiso 1 1 calc R . . C3 C 0.3772(4) 0.2286(4) 0.5420(4) 0.0367(9) Uani 1 1 d U . . H3 H 0.3264 0.2791 0.4936 0.044 Uiso 1 1 calc R . . C4 C 0.6561(3) 0.0411(4) 0.5901(4) 0.0387(9) Uani 1 1 d U . . H4A H 0.6763 -0.0061 0.5268 0.046 Uiso 1 1 calc R . . H4B H 0.6543 -0.0170 0.6731 0.046 Uiso 1 1 calc R . . C6 C 0.9896(4) 0.3564(4) 0.4084(4) 0.0392(9) Uani 1 1 d U . . H6 H 0.9465 0.4340 0.4082 0.047 Uiso 1 1 calc R . . C7 C 1.0846(4) 0.1904(4) 0.3490(4) 0.0378(9) Uani 1 1 d U . . H7 H 1.1186 0.1338 0.2998 0.045 Uiso 1 1 calc R . . C8 C 1.0858(4) 0.1758(4) 0.4703(4) 0.0440(10) Uani 1 1 d U . . H8 H 1.1204 0.1073 0.5214 0.053 Uiso 1 1 calc R . . C9 C 0.8649(4) 0.3591(4) 0.1945(4) 0.0488(11) Uani 1 1 d U . . H9A H 0.8429 0.2752 0.2198 0.073 Uiso 1 1 calc R . . H9B H 0.8516 0.4009 0.1122 0.073 Uiso 1 1 calc R . . H9C H 0.8136 0.4012 0.2576 0.073 Uiso 1 1 calc R . . C10 C 0.9997(4) 0.3589(4) 0.1851(4) 0.0448(10) Uani 1 1 d U . . H10A H 1.0509 0.3123 0.1248 0.054 Uiso 1 1 calc R . . H10B H 1.0237 0.4434 0.1519 0.054 Uiso 1 1 calc R . . C11 C 0.3375(4) 0.4104(4) 0.1986(4) 0.0396(9) Uani 1 1 d U . . H11 H 0.2539 0.4383 0.2283 0.048 Uiso 1 1 calc R . . C12 C 0.3806(5) 0.3082(4) 0.1557(4) 0.0478(11) Uani 1 1 d U . . H12 H 0.3331 0.2530 0.1487 0.057 Uiso 1 1 calc R . . C13 C 0.5404(4) 0.3982(5) 0.1448(4) 0.0534(12) Uani 1 1 d U . . H13 H 0.6220 0.4158 0.1294 0.064 Uiso 1 1 calc R . . C14 C 0.7559(4) 0.1271(4) 0.5541(5) 0.0519(11) Uani 1 1 d U . . H14A H 0.7571 0.1858 0.4727 0.078 Uiso 1 1 calc R . . H14B H 0.8358 0.0802 0.5472 0.078 Uiso 1 1 calc R . . H14C H 0.7390 0.1704 0.6192 0.078 Uiso 1 1 calc R . . C15 C 0.4366(4) 0.5804(4) 0.2272(5) 0.0499(11) Uani 1 1 d U . . H15A H 0.5138 0.6193 0.1776 0.060 Uiso 1 1 calc R . . H15B H 0.3679 0.6377 0.2057 0.060 Uiso 1 1 calc R . . C16 C 0.4222(8) 0.5569(6) 0.3650(5) 0.098(2) Uani 1 1 d U . . H16A H 0.3414 0.5277 0.4143 0.148 Uiso 1 1 calc R . . H16B H 0.4296 0.6323 0.3829 0.148 Uiso 1 1 calc R . . H16C H 0.4861 0.4953 0.3882 0.148 Uiso 1 1 calc R . . Mo1 Mo 0.08966(3) 0.00850(2) 0.84005(2) 0.01866(8) Uani 1 1 d . . . Mo2 Mo -0.10820(3) 0.28001(2) 0.85494(3) 0.02062(8) Uani 1 1 d . . . Mo3 Mo 0.18775(3) 0.28497(3) 0.80470(3) 0.02361(8) Uani 1 1 d . . . Mo4 Mo -0.23971(3) 0.02438(3) 0.94700(3) 0.02147(8) Uani 1 1 d . . . N1 N 0.3507(3) 0.2009(3) 0.6743(3) 0.0288(6) Uani 1 1 d . . . N2 N 0.5324(3) 0.1075(3) 0.5971(3) 0.0313(7) Uani 1 1 d . . . N3 N 1.0238(3) 0.3039(3) 0.3113(3) 0.0303(7) Uani 1 1 d . . . N4 N 1.0267(3) 0.2810(3) 0.5039(3) 0.0409(8) Uani 1 1 d . . . H4 H 1.0155 0.2954 0.5770 0.049 Uiso 1 1 calc R . . N5 N 0.5080(4) 0.3019(4) 0.1245(3) 0.0533(10) Uani 1 1 d . . . H5 H 0.5588 0.2443 0.0962 0.064 Uiso 1 1 calc R . . N6 N 0.4388(3) 0.4655(3) 0.1904(3) 0.0379(8) Uani 1 1 d . . . O1 O 0.0247(2) 0.3165(2) 0.9080(2) 0.0247(5) Uani 1 1 d . . . O2 O -0.0926(2) 0.3944(2) 0.7122(2) 0.0290(5) Uani 1 1 d . . . O3 O -0.2312(2) 0.3358(2) 0.9619(2) 0.0289(5) Uani 1 1 d . . . O4 O 0.2129(2) -0.0486(2) 0.7355(2) 0.0308(6) Uani 1 1 d . . . O5 O -0.3706(2) 0.0920(2) 1.0375(2) 0.0331(6) Uani 1 1 d . . . O6 O 0.1933(2) 0.0998(2) 0.9129(2) 0.0232(5) Uani 1 1 d . . . O7 O -0.0920(2) 0.09701(19) 0.9913(2) 0.0199(5) Uani 1 1 d . . . O8 O 0.0701(2) 0.1773(2) 0.7538(2) 0.0222(5) Uani 1 1 d . . . O9 O -0.1899(2) 0.1704(2) 0.8111(2) 0.0253(5) Uani 1 1 d . . . O10 O -0.0401(2) -0.0460(2) 0.8293(2) 0.0250(5) Uani 1 1 d . . . O11 O 0.2765(2) 0.3304(2) 0.8751(3) 0.0388(6) Uani 1 1 d . . . O12 O -0.2936(2) -0.0597(2) 0.8777(2) 0.0348(6) Uani 1 1 d . . . O13 O 0.1897(2) 0.3996(2) 0.6656(2) 0.0371(6) 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 C1 0.0268(19) 0.0316(19) 0.0283(18) -0.0026(15) -0.0014(15) 0.0002(15) C2 0.037(2) 0.050(2) 0.0284(19) -0.0133(17) -0.0060(17) -0.0008(18) C3 0.031(2) 0.041(2) 0.034(2) -0.0074(17) -0.0080(17) -0.0009(17) C4 0.0258(19) 0.040(2) 0.044(2) -0.0141(18) -0.0037(17) 0.0058(16) C6 0.048(2) 0.031(2) 0.035(2) -0.0141(17) -0.0012(18) -0.0061(17) C7 0.043(2) 0.037(2) 0.034(2) -0.0149(16) -0.0124(18) 0.0086(17) C8 0.042(2) 0.050(2) 0.035(2) -0.0083(18) -0.0134(19) 0.0097(19) C9 0.064(3) 0.041(2) 0.052(3) -0.016(2) -0.032(2) 0.004(2) C10 0.058(3) 0.043(2) 0.031(2) 0.0010(17) -0.019(2) -0.010(2) C11 0.0253(19) 0.035(2) 0.054(2) -0.0129(18) -0.0049(18) -0.0023(16) C12 0.055(3) 0.038(2) 0.048(2) -0.0124(19) -0.009(2) -0.007(2) C13 0.032(2) 0.077(3) 0.047(2) -0.023(2) -0.005(2) 0.005(2) C14 0.037(2) 0.060(3) 0.060(3) -0.019(2) -0.012(2) -0.004(2) C15 0.042(2) 0.045(2) 0.067(3) -0.012(2) -0.019(2) -0.0108(19) C16 0.178(7) 0.059(3) 0.061(4) -0.023(3) -0.022(4) -0.029(4) Mo1 0.02156(15) 0.01674(14) 0.01617(14) -0.00483(10) -0.00348(11) -0.00065(11) Mo2 0.01948(15) 0.01830(14) 0.02101(15) -0.00476(11) -0.00334(11) 0.00070(11) Mo3 0.02018(15) 0.01823(15) 0.02875(16) -0.00484(11) -0.00292(12) -0.00270(11) Mo4 0.02012(15) 0.02123(15) 0.02344(15) -0.00557(11) -0.00723(12) -0.00153(11) N1 0.0244(15) 0.0272(15) 0.0287(15) -0.0045(12) -0.0019(13) -0.0032(12) N2 0.0241(16) 0.0323(16) 0.0310(16) -0.0083(13) -0.0011(13) 0.0011(13) N3 0.0348(17) 0.0296(16) 0.0263(15) -0.0079(13) -0.0079(14) -0.0034(13) N4 0.046(2) 0.055(2) 0.0258(16) -0.0190(16) -0.0044(15) -0.0107(17) N5 0.050(2) 0.058(2) 0.041(2) -0.0203(18) -0.0054(18) 0.0210(19) N6 0.0259(17) 0.0436(19) 0.0393(18) -0.0107(15) -0.0041(14) -0.0010(14) O1 0.0241(12) 0.0211(11) 0.0276(12) -0.0099(10) -0.0047(10) 0.0018(9) O2 0.0336(14) 0.0217(12) 0.0259(12) -0.0022(10) -0.0063(11) 0.0003(10) O3 0.0232(12) 0.0313(13) 0.0304(13) -0.0126(10) -0.0025(11) 0.0005(10) O4 0.0301(13) 0.0293(13) 0.0289(13) -0.0130(11) 0.0008(11) 0.0001(11) O5 0.0240(13) 0.0313(13) 0.0364(14) -0.0076(11) -0.0005(11) -0.0009(10) O6 0.0236(12) 0.0203(11) 0.0238(11) -0.0039(9) -0.0050(10) -0.0039(9) O7 0.0199(11) 0.0180(11) 0.0198(11) -0.0036(9) -0.0046(9) -0.0014(9) O8 0.0234(12) 0.0208(11) 0.0203(11) -0.0054(9) -0.0043(9) -0.0009(9) O9 0.0282(13) 0.0238(12) 0.0231(11) -0.0022(9) -0.0111(10) 0.0000(10) O10 0.0277(13) 0.0262(12) 0.0251(12) -0.0103(10) -0.0098(10) -0.0024(10) O11 0.0298(14) 0.0367(15) 0.0538(17) -0.0162(13) -0.0096(13) -0.0104(12) O12 0.0373(15) 0.0350(14) 0.0394(14) -0.0121(12) -0.0168(12) -0.0061(11) O13 0.0353(15) 0.0242(13) 0.0364(14) 0.0007(11) 0.0007(12) -0.0004(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are de fined 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 C1 N1 1.316(5) . ? C1 N2 1.341(4) . ? C1 H1 0.9300 . ? C2 C3 1.343(5) . ? C2 N2 1.367(5) . ? C2 H2 0.9300 . ? C3 N1 1.380(5) . ? C3 H3 0.9300 . ? C4 N2 1.463(5) . ? C4 C14 1.497(6) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C6 N4 1.303(5) . ? C6 N3 1.328(5) . ? C6 H6 0.9300 . ? C7 C8 1.342(6) . ? C7 N3 1.367(5) . ? C7 H7 0.9300 . ? C8 N4 1.361(5) . ? C8 H8 0.9300 . ? C9 C10 1.497(6) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 N3 1.474(5) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.347(6) . ? C11 N6 1.365(5) . ? C11 H11 0.9300 . ? C12 N5 1.365(6) . ? C12 H12 0.9300 . ? C13 N6 1.314(5) . ? C13 N5 1.315(7) . ? C13 H13 0.9300 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C16 1.466(7) . ? C15 N6 1.479(5) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? Mo1 O4 1.691(2) . ? Mo1 O10 1.743(2) . ? Mo1 O8 1.882(2) . ? Mo1 O7 1.934(2) 2_557 ? Mo1 O6 2.171(2) . ? Mo1 O7 2.497(2) . ? Mo2 O3 1.698(2) . ? Mo2 O2 1.723(2) . ? Mo2 O9 1.930(2) . ? Mo2 O1 1.939(2) . ? Mo2 O7 2.204(2) . ? Mo2 O8 2.293(2) . ? Mo3 O11 1.694(3) . ? Mo3 O13 1.713(2) . ? Mo3 O1 1.882(2) . ? Mo3 O6 2.091(2) . ? Mo3 N1 2.234(3) . ? Mo3 O8 2.258(2) . ? Mo4 O12 1.695(2) . ? Mo4 O5 1.716(2) . ? Mo4 O9 1.913(2) . ? Mo4 O6 1.931(2) 2_557 ? Mo4 O7 2.239(2) . ? Mo4 O10 2.368(2) . ? N4 H4 0.8600 . ? N5 H5 0.8600 . ? O6 Mo4 1.931(2) 2_557 ? O7 Mo1 1.934(2) 2_557 ? 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 N1 C1 N2 110.6(3) . . ? N1 C1 H1 124.7 . . ? N2 C1 H1 124.7 . . ? C3 C2 N2 106.9(3) . . ? C3 C2 H2 126.6 . . ? N2 C2 H2 126.6 . . ? C2 C3 N1 108.8(4) . . ? C2 C3 H3 125.6 . . ? N1 C3 H3 125.6 . . ? N2 C4 C14 112.2(3) . . ? N2 C4 H4A 109.2 . . ? C14 C4 H4A 109.2 . . ? N2 C4 H4B 109.2 . . ? C14 C4 H4B 109.2 . . ? H4A C4 H4B 107.9 . . ? N4 C6 N3 108.5(3) . . ? N4 C6 H6 125.8 . . ? N3 C6 H6 125.8 . . ? C8 C7 N3 107.2(3) . . ? C8 C7 H7 126.4 . . ? N3 C7 H7 126.4 . . ? C7 C8 N4 106.6(4) . . ? C7 C8 H8 126.7 . . ? N4 C8 H8 126.7 . . ? C10 C9 H9A 109.5 . . ? C10 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C10 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N3 C10 C9 111.8(3) . . ? N3 C10 H10A 109.3 . . ? C9 C10 H10A 109.3 . . ? N3 C10 H10B 109.3 . . ? C9 C10 H10B 109.3 . . ? H10A C10 H10B 107.9 . . ? C12 C11 N6 107.5(4) . . ? C12 C11 H11 126.3 . . ? N6 C11 H11 126.3 . . ? C11 C12 N5 106.4(4) . . ? C11 C12 H12 126.8 . . ? N5 C12 H12 126.8 . . ? N6 C13 N5 109.1(4) . . ? N6 C13 H13 125.5 . . ? N5 C13 H13 125.5 . . ? C4 C14 H14A 109.5 . . ? C4 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C4 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 N6 112.3(4) . . ? C16 C15 H15A 109.1 . . ? N6 C15 H15A 109.1 . . ? C16 C15 H15B 109.1 . . ? N6 C15 H15B 109.1 . . ? H15A C15 H15B 107.9 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O4 Mo1 O10 104.44(11) . . ? O4 Mo1 O8 103.73(11) . . ? O10 Mo1 O8 100.80(10) . . ? O4 Mo1 O7 104.93(11) . 2_557 ? O10 Mo1 O7 97.85(10) . 2_557 ? O8 Mo1 O7 140.42(9) . 2_557 ? O4 Mo1 O6 97.96(11) . . ? O10 Mo1 O6 157.47(9) . . ? O8 Mo1 O6 75.77(9) . . ? O7 Mo1 O6 73.73(9) 2_557 . ? O4 Mo1 O7 178.84(10) . . ? O10 Mo1 O7 75.86(9) . . ? O8 Mo1 O7 75.11(8) . . ? O7 Mo1 O7 76.10(9) 2_557 . ? O6 Mo1 O7 81.79(8) . . ? O3 Mo2 O2 104.24(11) . . ? O3 Mo2 O9 100.51(11) . . ? O2 Mo2 O9 95.92(11) . . ? O3 Mo2 O1 97.85(11) . . ? O2 Mo2 O1 99.47(11) . . ? O9 Mo2 O1 152.30(9) . . ? O3 Mo2 O7 94.05(10) . . ? O2 Mo2 O7 160.59(10) . . ? O9 Mo2 O7 74.03(9) . . ? O1 Mo2 O7 84.17(9) . . ? O3 Mo2 O8 166.38(10) . . ? O2 Mo2 O8 88.31(9) . . ? O9 Mo2 O8 83.12(9) . . ? O1 Mo2 O8 74.50(8) . . ? O7 Mo2 O8 74.20(8) . . ? O11 Mo3 O13 105.68(14) . . ? O11 Mo3 O1 102.05(12) . . ? O13 Mo3 O1 100.67(11) . . ? O11 Mo3 O6 94.79(11) . . ? O13 Mo3 O6 153.48(11) . . ? O1 Mo3 O6 91.12(9) . . ? O11 Mo3 N1 94.33(12) . . ? O13 Mo3 N1 83.01(11) . . ? O1 Mo3 N1 161.42(11) . . ? O6 Mo3 N1 78.72(9) . . ? O11 Mo3 O8 164.58(11) . . ? O13 Mo3 O8 89.62(11) . . ? O1 Mo3 O8 76.40(9) . . ? O6 Mo3 O8 70.02(9) . . ? N1 Mo3 O8 85.47(10) . . ? O12 Mo4 O5 105.50(13) . . ? O12 Mo4 O9 103.67(11) . . ? O5 Mo4 O9 97.23(11) . . ? O12 Mo4 O6 103.09(11) . 2_557 ? O5 Mo4 O6 97.90(11) . 2_557 ? O9 Mo4 O6 144.31(10) . 2_557 ? O12 Mo4 O7 154.99(11) . . ? O5 Mo4 O7 99.49(11) . . ? O9 Mo4 O7 73.51(9) . . ? O6 Mo4 O7 72.22(9) 2_557 . ? O12 Mo4 O10 84.17(11) . . ? O5 Mo4 O10 170.17(11) . . ? O9 Mo4 O10 78.40(9) . . ? O6 Mo4 O10 81.30(9) 2_557 . ? O7 Mo4 O10 70.88(8) . . ? C1 N1 C3 106.3(3) . . ? C1 N1 Mo3 128.0(2) . . ? C3 N1 Mo3 125.3(2) . . ? C1 N2 C2 107.4(3) . . ? C1 N2 C4 126.3(3) . . ? C2 N2 C4 126.0(3) . . ? C6 N3 C7 108.1(3) . . ? C6 N3 C10 125.6(3) . . ? C7 N3 C10 126.2(3) . . ? C6 N4 C8 109.6(3) . . ? C6 N4 H4 125.2 . . ? C8 N4 H4 125.2 . . ? C13 N5 C12 108.9(4) . . ? C13 N5 H5 125.6 . . ? C12 N5 H5 125.6 . . ? C13 N6 C11 108.2(4) . . ? C13 N6 C15 125.2(4) . . ? C11 N6 C15 126.6(3) . . ? Mo3 O1 Mo2 115.02(11) . . ? Mo4 O6 Mo3 148.79(13) 2_557 . ? Mo4 O6 Mo1 106.30(10) 2_557 . ? Mo3 O6 Mo1 104.77(10) . . ? Mo1 O7 Mo2 152.39(11) 2_557 . ? Mo1 O7 Mo4 103.63(9) 2_557 . ? Mo2 O7 Mo4 92.98(8) . . ? Mo1 O7 Mo1 103.90(9) 2_557 . ? Mo2 O7 Mo1 96.00(8) . . ? Mo4 O7 Mo1 95.93(8) . . ? Mo1 O8 Mo3 108.98(10) . . ? Mo1 O8 Mo2 113.55(10) . . ? Mo3 O8 Mo2 90.18(8) . . ? Mo4 O9 Mo2 113.96(11) . . ? Mo1 O10 Mo4 117.11(11) . . ? _diffrn_measured_fraction_theta_max 0.957 _diffrn_reflns_theta_full 25.20 _diffrn_measured_fraction_theta_full 0.957 _refine_diff_density_max 0.427 _refine_diff_density_min -0.844 _refine_diff_density_rms 0.089 _database_code_depnum_ccdc_archive 'CCDC 939802' ####################################################################### # # 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_4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H16 Mo8 N4 O26, 2(C5 H8 N2), 4(C5 H9 N2)' _chemical_formula_sum 'C40 H68 Mo8 N16 O26' _chemical_formula_weight 1956.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 12.1992(4) _cell_length_b 23.5887(6) _cell_length_c 11.8092(4) _cell_angle_alpha 90.00 _cell_angle_beta 109.758(3) _cell_angle_gamma 90.00 _cell_volume 3198.20(18) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6542 _cell_measurement_theta_min 2.9446 _cell_measurement_theta_max 29.3984 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.015 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1896 _exptl_absorpt_coefficient_mu 1.604 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.698 _exptl_absorpt_correction_T_max 0.726 _exptl_absorpt_process_details 'Global rigid bond restraints (SIMU) were applied to keep thermalparameters reasonable.Constraint (DFIX 0.02 1.45 c12 c21 c17 c22) was necessary for sensible chemical distance.Such severe restraints were necessary due to the weak diffraction.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 16270 _diffrn_reflns_av_R_equivalents 0.0351 _diffrn_reflns_av_sigmaI/netI 0.0433 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 25.02 _reflns_number_total 5655 _reflns_number_gt 4623 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0518P)^2^+15.1044P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5646 _refine_ls_number_parameters 410 _refine_ls_number_restraints 260 _refine_ls_R_factor_all 0.0530 _refine_ls_R_factor_gt 0.0402 _refine_ls_wR_factor_ref 0.1104 _refine_ls_wR_factor_gt 0.1025 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 0.021 _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 C1 C 0.6902(7) 0.2736(3) 0.6966(7) 0.0431(17) Uani 1 1 d U . . H1 H 0.7656 0.2752 0.7516 0.052 Uiso 1 1 calc R . . C2 C 0.5375(7) 0.2918(3) 0.5447(7) 0.0403(16) Uani 1 1 d U . . H2 H 0.4868 0.3082 0.4749 0.048 Uiso 1 1 calc R . . C3 C 0.5095(6) 0.2492(3) 0.6022(7) 0.0319(15) Uani 1 1 d U . . C4 C 0.1212(8) 0.4068(4) 0.7977(8) 0.0549(18) Uani 1 1 d U . . H4 H 0.0439 0.3962 0.7603 0.066 Uiso 1 1 calc R . . C5 C 0.1749(7) 0.4059(3) 0.9127(6) 0.0406(15) Uani 1 1 d U . . H5 H 0.1431 0.3946 0.9705 0.049 Uiso 1 1 calc R . . C6 C 0.2974(8) 0.4366(4) 0.8264(7) 0.0558(17) Uani 1 1 d U . . H6 H 0.3634 0.4504 0.8130 0.067 Uiso 1 1 calc R . . N8 N 0.9470(6) 0.6397(3) 0.9606(6) 0.0451(16) Uani 1 1 d . . . C8 C 0.9108(8) 0.6614(4) 0.8520(8) 0.056(2) Uani 1 1 d U . . H8 H 0.8401 0.6523 0.7934 0.067 Uiso 1 1 calc R . . C9 C 0.1785(8) 0.5472(4) 0.9588(8) 0.0569(17) Uani 1 1 d U . . H9 H 0.1743 0.5338 1.0313 0.068 Uiso 1 1 calc R . . C10 C 0.0972(7) 0.5452(4) 0.8604(8) 0.0485(16) Uani 1 1 d U . . H10 H 0.0243 0.5296 0.8490 0.058 Uiso 1 1 calc R . . C12 C 0.9734(11) 0.7361(6) 0.7298(10) 0.086(3) Uani 1 1 d DU . . C13 C 1.0788(9) 0.6985(5) 0.9409(9) 0.075(2) Uani 1 1 d U . . H13 H 1.1465 0.7199 0.9573 0.090 Uiso 1 1 calc R . . C14 C 0.4025(10) 0.6391(5) 1.0805(9) 0.078(3) Uani 1 1 d U . . H14A H 0.3830 0.6640 1.0121 0.093 Uiso 1 1 calc R . . H14B H 0.4825 0.6448 1.1293 0.093 Uiso 1 1 calc R . . H14C H 0.3533 0.6473 1.1269 0.093 Uiso 1 1 calc R . . C15 C 0.3854(8) 0.5803(4) 1.0394(8) 0.065(2) Uani 1 1 d U . . H15A H 0.3910 0.5559 1.1073 0.078 Uiso 1 1 calc R . . H15B H 0.4469 0.5696 1.0088 0.078 Uiso 1 1 calc R . . C16 C 0.2463(8) 0.5861(4) 0.8269(7) 0.0541(19) Uani 1 1 d U . . H16 H 0.2939 0.6034 0.7900 0.065 Uiso 1 1 calc R . . C17 C 0.1694(9) 0.4311(5) 0.6106(8) 0.074(2) Uani 1 1 d DU . . C19 C 0.3933(8) 0.2249(4) 0.5757(9) 0.062(2) Uani 1 1 d U . . H19 H 0.3666 0.1931 0.5278 0.074 Uiso 1 1 calc R . . C20 C 0.3244(11) 0.2568(5) 0.6339(13) 0.102(4) Uani 1 1 d U . . H20A H 0.3713 0.2650 0.7155 0.122 Uiso 1 1 calc R . . H20B H 0.2579 0.2348 0.6330 0.122 Uiso 1 1 calc R . . H20C H 0.2987 0.2917 0.5912 0.122 Uiso 1 1 calc R . . C21 C 0.9696(18) 0.7078(8) 0.6432(17) 0.172(6) Uani 1 1 d DU . . H21A H 1.0469 0.6960 0.6500 0.207 Uiso 1 1 calc R . . H21B H 0.9370 0.7299 0.5713 0.207 Uiso 1 1 calc R . . H21C H 0.9219 0.6750 0.6394 0.207 Uiso 1 1 calc R . . C22 C 0.0558(13) 0.4328(8) 0.5516(13) 0.142(5) Uani 1 1 d DU . . H22A H 0.0168 0.4484 0.6028 0.171 Uiso 1 1 calc R . . H22B H 0.0276 0.3951 0.5280 0.171 Uiso 1 1 calc R . . H22C H 0.0407 0.4561 0.4813 0.171 Uiso 1 1 calc R . . Mo1 Mo 0.50197(4) 0.44460(2) 0.59630(4) 0.01822(14) Uani 1 1 d . . . Mo2 Mo 0.73939(5) 0.38325(2) 0.55739(5) 0.02427(15) Uani 1 1 d . . . Mo3 Mo 0.44030(5) 0.41592(2) 0.30850(5) 0.02168(15) Uani 1 1 d . . . Mo4 Mo 0.77839(5) 0.50565(2) 0.68985(5) 0.02265(15) Uani 1 1 d . . . N1 N 0.6462(5) 0.3084(2) 0.5983(5) 0.0323(13) Uani 1 1 d . . . N2 N 0.6068(8) 0.2368(3) 0.7011(8) 0.070(2) Uani 1 1 d . . . N3 N 0.1912(6) 0.4247(3) 0.7401(6) 0.0486(17) Uani 1 1 d . . . N4 N 0.9868(7) 0.6977(3) 0.8356(7) 0.059(2) Uani 1 1 d . . . N5 N 0.2722(6) 0.5713(3) 0.9451(5) 0.0445(16) Uani 1 1 d . . . N6 N 0.1290(10) 0.5684(4) 0.7749(10) 0.110(4) Uani 1 1 d . . . N7 N 0.2869(8) 0.4244(4) 0.9351(7) 0.078(3) Uani 1 1 d . . . C7 C 1.0534(9) 0.6631(5) 1.0149(8) 0.066(2) Uani 1 1 d U . . H7 H 1.1015 0.6554 1.0932 0.079 Uiso 1 1 calc R . . O1 O 0.4707(4) 0.49583(18) 0.6888(4) 0.0240(9) Uani 1 1 d . . . O2 O 0.3076(4) 0.46107(18) 0.2167(4) 0.0251(10) Uani 1 1 d . . . O3 O 0.3990(3) 0.47162(16) 0.4406(3) 0.0195(9) Uani 1 1 d . . . O4 O 0.4319(4) 0.38650(18) 0.6216(4) 0.0316(11) Uani 1 1 d . . . O5 O 0.3633(4) 0.35620(19) 0.3174(4) 0.0341(11) Uani 1 1 d . . . O6 O 0.5020(4) 0.3989(2) 0.2024(4) 0.0340(11) Uani 1 1 d . . . O7 O 0.5644(4) 0.40627(17) 0.4607(4) 0.0225(9) Uani 1 1 d . . . O8 O 0.7573(4) 0.3553(2) 0.4313(4) 0.0379(12) Uani 1 1 d . . . O9 O 0.8538(4) 0.3567(2) 0.6751(4) 0.0385(12) Uani 1 1 d . . . O10 O 0.7894(4) 0.45893(19) 0.5567(4) 0.0276(10) Uani 1 1 d . . . O11 O 0.6612(4) 0.42962(17) 0.6797(4) 0.0220(9) Uani 1 1 d . . . O12 O 0.8411(4) 0.5645(2) 0.6544(4) 0.0345(11) Uani 1 1 d . . . O13 O 0.8900(4) 0.4770(2) 0.8088(4) 0.0339(11) 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 C1 0.039(4) 0.033(3) 0.052(4) 0.008(3) 0.009(3) 0.002(3) C2 0.035(4) 0.027(3) 0.053(4) 0.006(3) 0.007(3) 0.002(3) C3 0.026(3) 0.017(3) 0.050(4) 0.014(3) 0.009(3) -0.001(2) C4 0.038(3) 0.080(4) 0.050(3) 0.006(3) 0.020(3) 0.000(3) C5 0.030(3) 0.068(4) 0.032(3) 0.011(3) 0.021(3) 0.000(3) C6 0.040(3) 0.088(4) 0.044(3) 0.011(3) 0.020(3) 0.000(3) N8 0.036(4) 0.056(4) 0.044(4) -0.005(3) 0.016(3) -0.004(3) C8 0.046(4) 0.076(5) 0.047(4) -0.012(4) 0.018(3) -0.020(4) C9 0.047(3) 0.081(4) 0.051(3) 0.004(3) 0.027(3) -0.007(3) C10 0.029(3) 0.073(4) 0.050(3) 0.000(3) 0.020(3) -0.004(3) C12 0.085(5) 0.111(6) 0.062(5) -0.006(5) 0.026(4) -0.032(5) C13 0.054(5) 0.104(6) 0.061(5) -0.011(4) 0.013(4) -0.033(4) C14 0.064(6) 0.093(7) 0.057(5) 0.008(5) -0.004(5) -0.018(5) C15 0.047(4) 0.087(5) 0.047(4) 0.006(4) -0.003(4) -0.004(4) C16 0.043(4) 0.076(4) 0.041(4) 0.008(3) 0.012(3) -0.007(3) C17 0.050(4) 0.126(5) 0.044(4) 0.014(4) 0.012(4) 0.008(4) C19 0.046(4) 0.042(4) 0.091(5) 0.012(4) 0.013(4) -0.010(3) C20 0.073(7) 0.076(7) 0.156(9) 0.020(7) 0.039(7) -0.011(6) C21 0.162(10) 0.161(10) 0.153(10) 0.015(10) 0.000(10) -0.050(9) C22 0.100(9) 0.237(11) 0.086(8) 0.016(8) 0.026(7) -0.011(9) Mo1 0.0139(3) 0.0238(3) 0.0164(3) 0.0033(2) 0.0044(2) -0.0011(2) Mo2 0.0169(3) 0.0291(3) 0.0253(3) -0.0005(2) 0.0051(2) 0.0029(2) Mo3 0.0182(3) 0.0266(3) 0.0181(3) -0.0031(2) 0.0033(2) -0.0001(2) Mo4 0.0140(3) 0.0311(3) 0.0213(3) -0.0013(2) 0.0039(2) -0.0026(2) N1 0.033(3) 0.027(3) 0.033(3) 0.001(2) 0.006(3) 0.004(2) N2 0.074(6) 0.058(5) 0.074(6) 0.010(4) 0.023(5) 0.010(4) N3 0.036(4) 0.076(5) 0.034(3) 0.012(3) 0.013(3) 0.012(3) N4 0.049(5) 0.080(5) 0.053(4) 0.003(4) 0.021(4) -0.017(4) N5 0.032(4) 0.066(4) 0.033(3) 0.007(3) 0.007(3) -0.006(3) N6 0.088(8) 0.096(7) 0.094(8) -0.033(6) -0.039(6) 0.019(6) N7 0.080(7) 0.097(7) 0.059(5) 0.014(5) 0.027(5) 0.015(5) C7 0.052(5) 0.098(5) 0.045(4) -0.010(4) 0.012(4) -0.020(4) O1 0.021(2) 0.032(2) 0.020(2) 0.0011(18) 0.0076(18) -0.0017(18) O2 0.022(2) 0.033(2) 0.018(2) -0.0022(18) 0.0034(18) -0.0014(19) O3 0.014(2) 0.026(2) 0.017(2) 0.0028(17) 0.0038(16) 0.0005(17) O4 0.034(3) 0.030(2) 0.034(3) 0.004(2) 0.014(2) -0.006(2) O5 0.025(3) 0.033(2) 0.037(3) 0.000(2) 0.000(2) -0.007(2) O6 0.030(3) 0.044(3) 0.029(3) -0.007(2) 0.011(2) 0.004(2) O7 0.018(2) 0.027(2) 0.020(2) -0.0009(18) 0.0038(18) -0.0013(18) O8 0.032(3) 0.046(3) 0.035(3) -0.006(2) 0.011(2) 0.004(2) O9 0.023(3) 0.043(3) 0.041(3) 0.005(2) 0.000(2) 0.004(2) O10 0.022(2) 0.034(2) 0.029(2) -0.002(2) 0.012(2) -0.0012(19) O11 0.017(2) 0.028(2) 0.021(2) 0.0014(18) 0.0055(18) 0.0014(17) O12 0.029(3) 0.041(3) 0.035(3) -0.006(2) 0.013(2) -0.012(2) O13 0.019(2) 0.049(3) 0.030(2) 0.002(2) 0.003(2) 0.005(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N2 1.352(11) . ? C1 N1 1.375(9) . ? C2 N1 1.321(9) . ? C2 C3 1.321(10) . ? C3 N2 1.387(10) . ? C3 C19 1.462(11) . ? C4 C5 1.294(11) . ? C4 N3 1.328(10) . ? C5 N7 1.372(12) . ? C6 N7 1.363(11) . ? C6 N3 1.379(11) . ? N8 C8 1.311(11) . ? N8 C7 1.357(11) . ? C8 N4 1.325(11) . ? C9 C10 1.248(12) . ? C9 N5 1.336(10) . ? C10 N6 1.316(15) . ? C12 C21 1.21(2) . ? C12 N4 1.508(13) . ? C13 C7 1.320(13) . ? C13 N4 1.364(12) . ? C14 C15 1.463(14) . ? C15 N5 1.467(10) . ? C16 N5 1.367(10) . ? C16 N6 1.416(13) . ? C17 C22 1.325(16) . ? C17 N3 1.469(11) . ? C19 C20 1.462(15) . ? Mo1 O4 1.694(4) . ? Mo1 O1 1.756(4) . ? Mo1 O11 1.891(4) . ? Mo1 O3 1.950(4) . ? Mo1 O7 2.187(4) . ? Mo1 O3 2.431(4) 3_666 ? Mo2 O8 1.708(5) . ? Mo2 O9 1.721(5) . ? Mo2 O10 1.888(4) . ? Mo2 O7 2.123(4) . ? Mo2 N1 2.238(6) . ? Mo2 O11 2.264(4) . ? Mo3 O6 1.714(4) . ? Mo3 O5 1.716(4) . ? Mo3 O7 1.933(4) . ? Mo3 O2 1.935(4) . ? Mo3 O3 2.223(4) . ? Mo3 O1 2.343(4) 3_666 ? Mo4 O12 1.704(5) . ? Mo4 O13 1.730(4) . ? Mo4 O2 1.928(4) 3_666 ? Mo4 O10 1.962(4) . ? Mo4 O3 2.256(4) 3_666 ? Mo4 O11 2.271(4) . ? O1 Mo3 2.343(4) 3_666 ? O2 Mo4 1.928(4) 3_666 ? O3 Mo4 2.256(4) 3_666 ? O3 Mo1 2.431(4) 3_666 ? 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 N2 C1 N1 109.5(7) . . ? N1 C2 C3 111.8(7) . . ? C2 C3 N2 107.3(7) . . ? C2 C3 C19 126.1(7) . . ? N2 C3 C19 126.2(7) . . ? C5 C4 N3 111.0(8) . . ? C4 C5 N7 108.3(7) . . ? N7 C6 N3 106.8(8) . . ? C8 N8 C7 104.8(7) . . ? N8 C8 N4 112.0(8) . . ? C10 C9 N5 110.2(8) . . ? C9 C10 N6 110.6(9) . . ? C21 C12 N4 109.4(14) . . ? C7 C13 N4 106.8(9) . . ? C14 C15 N5 112.3(8) . . ? N5 C16 N6 102.6(8) . . ? C22 C17 N3 109.8(10) . . ? C3 C19 C20 111.5(9) . . ? O4 Mo1 O1 102.6(2) . . ? O4 Mo1 O11 104.3(2) . . ? O1 Mo1 O11 101.86(19) . . ? O4 Mo1 O3 103.2(2) . . ? O1 Mo1 O3 98.96(18) . . ? O11 Mo1 O3 140.61(17) . . ? O4 Mo1 O7 96.64(19) . . ? O1 Mo1 O7 160.53(17) . . ? O11 Mo1 O7 75.74(16) . . ? O3 Mo1 O7 73.58(16) . . ? O4 Mo1 O3 179.53(19) . 3_666 ? O1 Mo1 O3 77.15(16) . 3_666 ? O11 Mo1 O3 76.12(15) . 3_666 ? O3 Mo1 O3 76.46(16) . 3_666 ? O7 Mo1 O3 83.57(14) . 3_666 ? O8 Mo2 O9 104.8(2) . . ? O8 Mo2 O10 103.0(2) . . ? O9 Mo2 O10 99.9(2) . . ? O8 Mo2 O7 91.8(2) . . ? O9 Mo2 O7 157.1(2) . . ? O10 Mo2 O7 91.35(17) . . ? O8 Mo2 N1 96.2(2) . . ? O9 Mo2 N1 82.6(2) . . ? O10 Mo2 N1 159.2(2) . . ? O7 Mo2 N1 79.97(18) . . ? O8 Mo2 O11 161.47(19) . . ? O9 Mo2 O11 93.5(2) . . ? O10 Mo2 O11 75.66(16) . . ? O7 Mo2 O11 69.86(15) . . ? N1 Mo2 O11 83.64(18) . . ? O6 Mo3 O5 103.7(2) . . ? O6 Mo3 O7 104.7(2) . . ? O5 Mo3 O7 96.84(19) . . ? O6 Mo3 O2 102.2(2) . . ? O5 Mo3 O2 96.6(2) . . ? O7 Mo3 O2 146.09(17) . . ? O6 Mo3 O3 155.66(19) . . ? O5 Mo3 O3 100.58(19) . . ? O7 Mo3 O3 73.08(16) . . ? O2 Mo3 O3 73.90(15) . . ? O6 Mo3 O1 84.36(19) . 3_666 ? O5 Mo3 O1 171.6(2) . 3_666 ? O7 Mo3 O1 83.01(16) . 3_666 ? O2 Mo3 O1 79.33(16) . 3_666 ? O3 Mo3 O1 71.30(14) . 3_666 ? O12 Mo4 O13 102.9(2) . . ? O12 Mo4 O2 100.7(2) . 3_666 ? O13 Mo4 O2 97.2(2) . 3_666 ? O12 Mo4 O10 95.9(2) . . ? O13 Mo4 O10 100.5(2) . . ? O2 Mo4 O10 152.33(18) 3_666 . ? O12 Mo4 O3 92.61(19) . 3_666 ? O13 Mo4 O3 163.24(19) . 3_666 ? O2 Mo4 O3 73.26(16) 3_666 3_666 ? O10 Mo4 O3 84.05(16) . 3_666 ? O12 Mo4 O11 163.17(19) . . ? O13 Mo4 O11 92.44(19) . . ? O2 Mo4 O11 84.09(16) 3_666 . ? O10 Mo4 O11 74.14(16) . . ? O3 Mo4 O11 73.16(14) 3_666 . ? C2 N1 C1 105.6(6) . . ? C2 N1 Mo2 129.1(5) . . ? C1 N1 Mo2 124.9(5) . . ? C1 N2 C3 105.8(7) . . ? C4 N3 C6 107.0(7) . . ? C4 N3 C17 130.2(8) . . ? C6 N3 C17 122.8(7) . . ? C8 N4 C13 106.1(8) . . ? C8 N4 C12 128.7(8) . . ? C13 N4 C12 124.9(8) . . ? C9 N5 C16 108.7(7) . . ? C9 N5 C15 126.4(7) . . ? C16 N5 C15 124.9(7) . . ? C10 N6 C16 107.8(8) . . ? C6 N7 C5 106.9(8) . . ? C13 C7 N8 110.3(9) . . ? Mo1 O1 Mo3 115.0(2) . 3_666 ? Mo4 O2 Mo3 114.7(2) 3_666 . ? Mo1 O3 Mo3 104.01(17) . . ? Mo1 O3 Mo4 152.2(2) . 3_666 ? Mo3 O3 Mo4 93.10(14) . 3_666 ? Mo1 O3 Mo1 103.54(16) . 3_666 ? Mo3 O3 Mo1 96.36(14) . 3_666 ? Mo4 O3 Mo1 96.01(14) 3_666 3_666 ? Mo3 O7 Mo2 149.2(2) . . ? Mo3 O7 Mo1 105.97(19) . . ? Mo2 O7 Mo1 104.34(17) . . ? Mo2 O10 Mo4 114.7(2) . . ? Mo1 O11 Mo2 109.75(18) . . ? Mo1 O11 Mo4 113.41(19) . . ? Mo2 O11 Mo4 91.25(15) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.781 _refine_diff_density_min -1.371 _refine_diff_density_rms 0.142 _database_code_depnum_ccdc_archive 'CCDC 939803' ####################################################################### # # 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_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H20 Mo8 N4 O26, 4(C6 H11 N2)' _chemical_formula_sum 'C36 H64 Mo8 N12 O26' _chemical_formula_weight 1848.51 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.1921(4) _cell_length_b 21.5036(9) _cell_length_c 15.3277(5) _cell_angle_alpha 90.00 _cell_angle_beta 120.334(2) _cell_angle_gamma 90.00 _cell_volume 2899.42(19) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) __cell_measurement_reflns_used 9975 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 28.39 _exptl_crystal_description rodlike _exptl_crystal_colour colorless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.117 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1816 _exptl_absorpt_coefficient_mu 1.761 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.596 _exptl_absorpt_correction_T_max 0.768 _exptl_absorpt_process_details SADABS,Bruker(2005) _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14316 _diffrn_reflns_av_R_equivalents 0.0197 _diffrn_reflns_av_sigmaI/netI 0.0228 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 25.20 _reflns_number_total 5221 _reflns_number_gt 4737 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0657P)^2^+1.9889P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5154 _refine_ls_number_parameters 376 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0270 _refine_ls_R_factor_gt 0.0219 _refine_ls_wR_factor_ref 0.1049 _refine_ls_wR_factor_gt 0.0728 _refine_ls_goodness_of_fit_ref 1.232 _refine_ls_restrained_S_all 1.232 _refine_ls_shift/su_max 0.003 _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 C1 C -0.0610(5) 0.79077(18) 0.1175(3) 0.0123(8) Uani 1 1 d . . . H1 H -0.0669 0.8034 0.0575 0.015 Uiso 1 1 calc R . . C2 C -0.0038(5) 0.78599(19) 0.2740(3) 0.0141(9) Uani 1 1 d . . . H2 H 0.0380 0.7953 0.3422 0.017 Uiso 1 1 calc R . . C3 C -0.0932(5) 0.73644(19) 0.2267(3) 0.0136(8) Uani 1 1 d . . . H3 H -0.1245 0.7060 0.2554 0.016 Uiso 1 1 calc R . . C4 C -0.2356(5) 0.6990(2) 0.0435(3) 0.0199(10) Uani 1 1 d . . . H4 H -0.2574 0.6625 0.0724 0.024 Uiso 1 1 calc R . . C5 C -0.1624(6) 0.6772(2) -0.0166(4) 0.0266(11) Uani 1 1 d . . . H5A H -0.2289 0.6484 -0.0678 0.040 Uiso 1 1 calc R . . H5B H -0.0675 0.6571 0.0280 0.040 Uiso 1 1 calc R . . H5C H -0.1446 0.7123 -0.0478 0.040 Uiso 1 1 calc R . . C6 C -0.3828(5) 0.7339(3) -0.0216(3) 0.0297(12) Uani 1 1 d . . . H6A H -0.3637 0.7688 -0.0527 0.045 Uiso 1 1 calc R . . H6B H -0.4226 0.7484 0.0197 0.045 Uiso 1 1 calc R . . H6C H -0.4552 0.7067 -0.0731 0.045 Uiso 1 1 calc R . . N1 N 0.0161(4) 0.82081(16) 0.2057(2) 0.0108(7) Uani 1 1 d . . . N2 N -0.1284(4) 0.74008(16) 0.1275(2) 0.0134(7) Uani 1 1 d . . . O1 O 0.1038(3) 1.04568(13) 0.3431(2) 0.0128(6) Uani 1 1 d . . . O2 O 0.2414(3) 1.10212(13) 0.0022(2) 0.0115(6) Uani 1 1 d . . . O3 O 0.0601(3) 1.04512(12) 0.0735(2) 0.0082(6) Uani 1 1 d . . . O4 O 0.0318(3) 1.03449(13) -0.1690(2) 0.0103(6) Uani 1 1 d . . . O5 O 0.2384(3) 0.97645(13) 0.0177(2) 0.0103(6) Uani 1 1 d . . . O6 O 0.2567(3) 0.98180(13) 0.25777(19) 0.0094(6) Uani 1 1 d . . . O7 O 0.1571(3) 0.90080(13) 0.3546(2) 0.0134(6) Uani 1 1 d . . . O8 O -0.2935(3) 1.14636(13) -0.0299(2) 0.0132(6) Uani 1 1 d . . . O9 O -0.0006(3) 1.18612(13) 0.0588(2) 0.0131(6) Uani 1 1 d . . . O10 O -0.0861(3) 1.09979(12) -0.0910(2) 0.0089(6) Uani 1 1 d . . . O11 O 0.2480(3) 1.10850(13) 0.2628(2) 0.0126(6) Uani 1 1 d . . . O12 O -0.0713(3) 1.09608(13) 0.1553(2) 0.0112(6) Uani 1 1 d . . . O13 O 0.3273(3) 0.85630(14) 0.2756(2) 0.0151(6) Uani 1 1 d . . . Mo1 Mo 0.11946(4) 1.041489(15) -0.02873(2) 0.00691(12) Uani 1 1 d . . . Mo2 Mo -0.10874(4) 1.120207(16) 0.02259(2) 0.00801(12) Uani 1 1 d . . . Mo3 Mo 0.12007(4) 1.050120(15) 0.23753(2) 0.00749(12) Uani 1 1 d . . . Mo4 Mo 0.17267(4) 0.901314(15) 0.24821(2) 0.00806(12) Uani 1 1 d . . . C7 C 0.2588(5) 0.8191(2) 0.7466(3) 0.0183(9) Uani 1 1 d . . . H7 H 0.1749 0.7928 0.7195 0.022 Uiso 1 1 calc R . . C8 C 0.4162(5) 0.8941(2) 0.8306(3) 0.0174(9) Uani 1 1 d . . . H8 H 0.4597 0.9286 0.8717 0.021 Uiso 1 1 calc R . . C9 C 0.4771(5) 0.8610(2) 0.7846(3) 0.0155(9) Uani 1 1 d . . . H9 H 0.5694 0.8686 0.7880 0.019 Uiso 1 1 calc R . . C10 C 0.3837(5) 0.7678(2) 0.6627(3) 0.0173(9) Uani 1 1 d . . . H10 H 0.3177 0.7328 0.6559 0.021 Uiso 1 1 calc R . . C11 C 0.5440(5) 0.7435(2) 0.7066(3) 0.0233(10) Uani 1 1 d . . . H11A H 0.5455 0.7110 0.6641 0.035 Uiso 1 1 calc R . . H11B H 0.5787 0.7273 0.7731 0.035 Uiso 1 1 calc R . . H11C H 0.6097 0.7767 0.7105 0.035 Uiso 1 1 calc R . . C12 C 0.3222(6) 0.7973(2) 0.5588(3) 0.0284(12) Uani 1 1 d . . . H12A H 0.3907 0.8292 0.5625 0.043 Uiso 1 1 calc R . . H12B H 0.2242 0.8152 0.5373 0.043 Uiso 1 1 calc R . . H12C H 0.3129 0.7661 0.5112 0.043 Uiso 1 1 calc R . . N3 N 0.2797(4) 0.86782(18) 0.8060(3) 0.0186(8) Uani 1 1 d . . . N4 N 0.3761(4) 0.81398(16) 0.7318(3) 0.0145(7) Uani 1 1 d . . . C13 C 0.7815(5) 0.9445(2) 0.2800(3) 0.0177(9) Uani 1 1 d . . . H13 H 0.8868 0.9475 0.3117 0.021 Uiso 1 1 calc R . . C14 C 0.6859(5) 0.9199(2) 0.1879(3) 0.0208(10) Uani 1 1 d . . . H14 H 0.7141 0.9023 0.1444 0.025 Uiso 1 1 calc R . . C15 C 0.5454(5) 0.95242(19) 0.2498(3) 0.0145(9) Uani 1 1 d . . . H15 H 0.4619 0.9614 0.2568 0.017 Uiso 1 1 calc R . . C16 C 0.7467(5) 0.9924(2) 0.4195(3) 0.0148(9) Uani 1 1 d . . . H16 H 0.8154 0.9625 0.4702 0.018 Uiso 1 1 calc R . . C17 C 0.6173(5) 1.0053(2) 0.4389(3) 0.0228(10) Uani 1 1 d . . . H17A H 0.6577 1.0212 0.5062 0.034 Uiso 1 1 calc R . . H17B H 0.5628 0.9675 0.4317 0.034 Uiso 1 1 calc R . . H17C H 0.5497 1.0354 0.3911 0.034 Uiso 1 1 calc R . . C18 C 0.8376(5) 1.0508(2) 0.4293(3) 0.0176(9) Uani 1 1 d . . . H18A H 0.7692 1.0843 0.3934 0.026 Uiso 1 1 calc R . . H18B H 0.9017 1.0432 0.4013 0.026 Uiso 1 1 calc R . . H18C H 0.8992 1.0617 0.4994 0.026 Uiso 1 1 calc R . . N5 N 0.5414(4) 0.92542(18) 0.1700(3) 0.0181(8) Uani 1 1 d . . . N6 N 0.6896(4) 0.96422(16) 0.3174(3) 0.0125(7) 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 C1 0.014(2) 0.0092(19) 0.0117(19) 0.0004(15) 0.0054(16) -0.0013(16) C2 0.017(2) 0.015(2) 0.0104(19) 0.0023(16) 0.0068(17) 0.0002(17) C3 0.017(2) 0.014(2) 0.011(2) 0.0038(16) 0.0082(17) 0.0012(17) C4 0.022(2) 0.015(2) 0.016(2) -0.0024(18) 0.0044(18) -0.0127(18) C5 0.033(3) 0.017(2) 0.022(2) -0.0092(19) 0.008(2) 0.002(2) C6 0.021(3) 0.046(3) 0.018(2) -0.009(2) 0.006(2) -0.009(2) N1 0.0114(17) 0.0114(17) 0.0095(16) 0.0025(13) 0.0050(14) 0.0010(14) N2 0.0167(18) 0.0108(18) 0.0107(17) 0.0008(13) 0.0054(15) -0.0022(14) O1 0.0122(15) 0.0182(16) 0.0091(14) 0.0004(11) 0.0061(12) 0.0029(11) O2 0.0102(14) 0.0133(15) 0.0097(14) -0.0010(11) 0.0042(12) -0.0008(11) O3 0.0091(14) 0.0107(14) 0.0065(14) 0.0001(10) 0.0052(12) -0.0002(10) O4 0.0121(14) 0.0102(14) 0.0064(14) -0.0009(11) 0.0032(12) -0.0010(11) O5 0.0091(13) 0.0119(14) 0.0099(14) 0.0003(11) 0.0047(11) 0.0010(11) O6 0.0077(13) 0.0101(14) 0.0099(14) -0.0010(11) 0.0042(11) 0.0002(11) O7 0.0143(15) 0.0158(15) 0.0103(14) -0.0013(11) 0.0063(12) -0.0041(11) O8 0.0142(14) 0.0132(15) 0.0104(14) 0.0004(11) 0.0049(12) 0.0019(12) O9 0.0181(15) 0.0119(14) 0.0107(14) -0.0012(11) 0.0083(12) 0.0001(12) O10 0.0106(14) 0.0095(14) 0.0057(13) 0.0006(10) 0.0033(11) 0.0007(11) O11 0.0117(15) 0.0107(14) 0.0149(14) -0.0023(11) 0.0063(12) 0.0004(11) O12 0.0144(15) 0.0110(15) 0.0063(13) 0.0002(11) 0.0038(12) 0.0003(11) O13 0.0146(15) 0.0146(15) 0.0152(14) 0.0005(12) 0.0069(12) 0.0028(12) Mo1 0.0071(2) 0.0084(2) 0.0053(2) -0.00020(12) 0.00318(15) -0.00061(12) Mo2 0.0097(2) 0.0082(2) 0.00629(19) -0.00004(12) 0.00415(15) 0.00090(12) Mo3 0.0082(2) 0.0082(2) 0.00582(19) -0.00093(12) 0.00336(15) -0.00009(12) Mo4 0.0093(2) 0.0081(2) 0.00590(19) 0.00025(12) 0.00325(15) -0.00023(12) C7 0.015(2) 0.023(2) 0.017(2) 0.0014(18) 0.0088(18) -0.0022(18) C8 0.010(2) 0.026(2) 0.016(2) -0.0016(18) 0.0067(17) 0.0005(17) C9 0.012(2) 0.018(2) 0.015(2) -0.0024(17) 0.0062(17) 0.0007(17) C10 0.018(2) 0.017(2) 0.019(2) -0.0036(18) 0.0107(18) -0.0005(17) C11 0.022(2) 0.028(3) 0.021(2) -0.001(2) 0.011(2) 0.007(2) C12 0.040(3) 0.026(3) 0.016(2) 0.000(2) 0.012(2) 0.013(2) N3 0.0177(19) 0.026(2) 0.0129(17) 0.0002(16) 0.0082(15) 0.0007(16) N4 0.0140(18) 0.0155(18) 0.0136(17) 0.0001(14) 0.0068(14) -0.0001(14) C13 0.012(2) 0.024(2) 0.018(2) -0.0008(18) 0.0079(18) -0.0013(18) C14 0.027(3) 0.022(2) 0.017(2) -0.0045(19) 0.014(2) -0.005(2) C15 0.011(2) 0.019(2) 0.014(2) -0.0010(16) 0.0068(18) 0.0006(16) C16 0.017(2) 0.021(2) 0.0059(18) -0.0021(16) 0.0056(16) -0.0009(17) C17 0.023(2) 0.033(3) 0.017(2) -0.009(2) 0.0143(19) -0.005(2) C18 0.018(2) 0.021(2) 0.011(2) -0.0024(17) 0.0057(18) 0.0013(17) N5 0.0198(19) 0.022(2) 0.0142(18) -0.0052(15) 0.0098(15) -0.0046(16) N6 0.0102(17) 0.0164(18) 0.0119(18) 0.0013(14) 0.0063(14) 0.0023(14) _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 C1 N1 1.338(5) . ? C1 N2 1.338(5) . ? C1 H1 0.9300 . ? C2 C3 1.350(6) . ? C2 N1 1.383(5) . ? C2 H2 0.9300 . ? C3 N2 1.377(5) . ? C3 H3 0.9300 . ? C4 N2 1.487(5) . ? C4 C6 1.517(7) . ? C4 C5 1.523(7) . ? C4 H4 0.9800 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? N1 Mo4 2.217(3) . ? O1 Mo3 1.710(3) . ? O2 Mo1 1.696(3) . ? O3 Mo1 1.946(3) . ? O3 Mo2 2.196(3) . ? O3 Mo3 2.270(3) . ? O3 Mo1 2.453(3) 3_575 ? O4 Mo1 1.871(3) . ? O4 Mo4 2.273(3) 3_575 ? O4 Mo3 2.273(3) 3_575 ? O5 Mo1 1.749(3) . ? O5 Mo2 2.372(3) 3_575 ? O6 Mo4 1.903(3) . ? O6 Mo3 1.938(3) . ? O7 Mo4 1.716(3) . ? O8 Mo2 1.726(3) . ? O9 Mo2 1.707(3) . ? O10 Mo2 1.919(3) . ? O10 Mo4 2.107(3) 3_575 ? O10 Mo1 2.203(3) . ? O11 Mo3 1.708(3) . ? O12 Mo2 1.941(3) . ? O12 Mo3 1.971(3) . ? O13 Mo4 1.711(3) . ? Mo1 O3 2.453(3) 3_575 ? Mo2 O5 2.371(3) 3_575 ? Mo3 O4 2.273(3) 3_575 ? Mo4 O10 2.107(3) 3_575 ? Mo4 O4 2.273(3) 3_575 ? C7 N4 1.330(6) . ? C7 N3 1.333(6) . ? C7 H7 0.9300 . ? C8 C9 1.352(6) . ? C8 N3 1.367(6) . ? C8 H8 0.9300 . ? C9 N4 1.377(5) . ? C9 H9 0.9300 . ? C10 N4 1.481(5) . ? C10 C11 1.512(6) . ? C10 C12 1.524(6) . ? C10 H10 0.9800 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C14 1.354(6) . ? C13 N6 1.388(5) . ? C13 H13 0.9300 . ? C14 N5 1.360(6) . ? C14 H14 0.9300 . ? C15 N6 1.326(6) . ? C15 N5 1.336(5) . ? C15 H15 0.9300 . ? C16 N6 1.495(5) . ? C16 C17 1.516(6) . ? C16 C18 1.522(6) . ? C16 H16 0.9800 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 N2 110.5(3) . . ? N1 C1 H1 124.7 . . ? N2 C1 H1 124.7 . . ? C3 C2 N1 109.8(4) . . ? C3 C2 H2 125.1 . . ? N1 C2 H2 125.1 . . ? C2 C3 N2 106.1(4) . . ? C2 C3 H3 127.0 . . ? N2 C3 H3 127.0 . . ? N2 C4 C6 109.0(4) . . ? N2 C4 C5 109.7(4) . . ? C6 C4 C5 112.2(4) . . ? N2 C4 H4 108.6 . . ? C6 C4 H4 108.6 . . ? C5 C4 H4 108.6 . . ? 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 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C1 N1 C2 105.5(3) . . ? C1 N1 Mo4 130.0(3) . . ? C2 N1 Mo4 124.0(3) . . ? C1 N2 C3 108.1(3) . . ? C1 N2 C4 125.4(3) . . ? C3 N2 C4 126.2(3) . . ? Mo1 O3 Mo2 104.46(12) . . ? Mo1 O3 Mo3 150.98(15) . . ? Mo2 O3 Mo3 94.78(10) . . ? Mo1 O3 Mo1 103.62(11) . 3_575 ? Mo2 O3 Mo1 96.83(11) . 3_575 ? Mo3 O3 Mo1 95.26(10) . 3_575 ? Mo1 O4 Mo4 110.01(13) . 3_575 ? Mo1 O4 Mo3 114.46(13) . 3_575 ? Mo4 O4 Mo3 90.73(10) 3_575 3_575 ? Mo1 O5 Mo2 114.47(13) . 3_575 ? Mo4 O6 Mo3 114.71(13) . . ? Mo2 O10 Mo4 150.19(16) . 3_575 ? Mo2 O10 Mo1 105.12(12) . . ? Mo4 O10 Mo1 104.26(11) 3_575 . ? Mo2 O12 Mo3 114.32(14) . . ? O2 Mo1 O5 103.97(14) . . ? O2 Mo1 O4 103.89(13) . . ? O5 Mo1 O4 103.51(13) . . ? O2 Mo1 O3 103.10(12) . . ? O5 Mo1 O3 97.95(12) . . ? O4 Mo1 O3 139.99(13) . . ? O2 Mo1 O10 94.94(12) . . ? O5 Mo1 O10 160.61(12) . . ? O4 Mo1 O10 75.52(11) . . ? O3 Mo1 O10 73.23(11) . . ? O2 Mo1 O3 179.09(12) . 3_575 ? O5 Mo1 O3 76.86(11) . 3_575 ? O4 Mo1 O3 76.19(11) . 3_575 ? O3 Mo1 O3 76.38(11) . 3_575 ? O10 Mo1 O3 84.20(9) . 3_575 ? O9 Mo2 O8 104.74(14) . . ? O9 Mo2 O10 97.55(12) . . ? O8 Mo2 O10 104.75(12) . . ? O9 Mo2 O12 97.36(12) . . ? O8 Mo2 O12 99.56(13) . . ? O10 Mo2 O12 147.07(12) . . ? O9 Mo2 O3 103.50(12) . . ? O8 Mo2 O3 151.63(12) . . ? O10 Mo2 O3 73.91(11) . . ? O12 Mo2 O3 74.13(11) . . ? O9 Mo2 O5 174.75(12) . 3_575 ? O8 Mo2 O5 80.26(12) . 3_575 ? O10 Mo2 O5 82.52(10) . 3_575 ? O12 Mo2 O5 80.05(11) . 3_575 ? O3 Mo2 O5 71.43(9) . 3_575 ? O11 Mo3 O1 104.71(14) . . ? O11 Mo3 O6 96.68(13) . . ? O1 Mo3 O6 102.20(12) . . ? O11 Mo3 O12 99.91(12) . . ? O1 Mo3 O12 95.50(13) . . ? O6 Mo3 O12 151.76(11) . . ? O11 Mo3 O3 91.95(12) . . ? O1 Mo3 O3 160.80(13) . . ? O6 Mo3 O3 84.91(11) . . ? O12 Mo3 O3 71.90(11) . . ? O11 Mo3 O4 163.13(12) . 3_575 ? O1 Mo3 O4 91.37(12) . 3_575 ? O6 Mo3 O4 74.55(11) . 3_575 ? O12 Mo3 O4 83.28(11) . 3_575 ? O3 Mo3 O4 73.17(9) . 3_575 ? O13 Mo4 O7 106.20(13) . . ? O13 Mo4 O6 99.94(13) . . ? O7 Mo4 O6 100.75(12) . . ? O13 Mo4 O10 94.36(12) . 3_575 ? O7 Mo4 O10 154.21(13) . 3_575 ? O6 Mo4 O10 90.60(11) . 3_575 ? O13 Mo4 N1 93.87(13) . . ? O7 Mo4 N1 82.89(13) . . ? O6 Mo4 N1 164.02(12) . . ? O10 Mo4 N1 80.30(11) 3_575 . ? O13 Mo4 O4 163.09(12) . 3_575 ? O7 Mo4 O4 90.68(12) . 3_575 ? O6 Mo4 O4 75.18(10) . 3_575 ? O10 Mo4 O4 69.78(10) 3_575 3_575 ? N1 Mo4 O4 89.29(11) . 3_575 ? N4 C7 N3 109.6(4) . . ? N4 C7 H7 125.2 . . ? N3 C7 H7 125.2 . . ? C9 C8 N3 108.1(4) . . ? C9 C8 H8 125.9 . . ? N3 C8 H8 125.9 . . ? C8 C9 N4 106.8(4) . . ? C8 C9 H9 126.6 . . ? N4 C9 H9 126.6 . . ? N4 C10 C11 110.4(3) . . ? N4 C10 C12 109.0(4) . . ? C11 C10 C12 113.0(4) . . ? N4 C10 H10 108.1 . . ? C11 C10 H10 108.1 . . ? C12 C10 H10 108.1 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C7 N3 C8 107.6(4) . . ? C7 N4 C9 107.9(4) . . ? C7 N4 C10 123.6(4) . . ? C9 N4 C10 128.3(4) . . ? C14 C13 N6 105.6(4) . . ? C14 C13 H13 127.2 . . ? N6 C13 H13 127.2 . . ? C13 C14 N5 108.2(4) . . ? C13 C14 H14 125.9 . . ? N5 C14 H14 125.9 . . ? N6 C15 N5 107.9(4) . . ? N6 C15 H15 126.1 . . ? N5 C15 H15 126.1 . . ? N6 C16 C17 111.3(3) . . ? N6 C16 C18 109.5(3) . . ? C17 C16 C18 112.1(4) . . ? N6 C16 H16 107.9 . . ? C17 C16 H16 107.9 . . ? C18 C16 H16 107.9 . . ? 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 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C15 N5 C14 108.9(4) . . ? C15 N6 C13 109.4(4) . . ? C15 N6 C16 125.9(4) . . ? C13 N6 C16 124.7(3) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.20 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.191 _refine_diff_density_min -1.133 _refine_diff_density_rms 0.230 _database_code_depnum_ccdc_archive 'CCDC 939804' ####################################################################### # # 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_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H20 Mo8 N4 O26, 4(C6 H11 N2), 2(C6 H10 N2), 2(H2 O)' _chemical_formula_sum 'C48 H88 Mo8 N16 O28' _chemical_formula_weight 2104.64 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n _symmetry_space_group_name_HALL -P2yn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.5903(18) _cell_length_b 11.8542(16) _cell_length_c 24.806(3) _cell_angle_alpha 90.00 _cell_angle_beta 100.449(2) _cell_angle_gamma 90.00 _cell_volume 3640.9(8) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2497 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 25.16 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.894 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2040 _exptl_absorpt_coefficient_mu 1.418 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.788 _exptl_absorpt_correction_T_max 0.844 _exptl_absorpt_process_details SADABS,Bruker(2005) _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21001 _diffrn_reflns_av_R_equivalents 0.1035 _diffrn_reflns_av_sigmaI/netI 0.1409 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 27.59 _reflns_number_total 8458 _reflns_number_gt 4804 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1407P)^2^+10.1857P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment Constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8179 _refine_ls_number_parameters 449 _refine_ls_number_restraints 53 _refine_ls_R_factor_all 0.1500 _refine_ls_R_factor_gt 0.0850 _refine_ls_wR_factor_ref 0.2680 _refine_ls_wR_factor_gt 0.2152 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.34205(8) 0.58603(10) 1.08846(4) 0.0289(3) Uani 1 1 d . . . Mo2 Mo 0.53673(8) 0.63932(9) 1.00803(4) 0.0300(3) Uani 1 1 d . . . Mo3 Mo 0.27839(8) 0.73295(10) 0.97747(4) 0.0309(3) Uani 1 1 d . . . Mo4 Mo 0.56770(10) 0.44717(12) 1.11540(4) 0.0455(4) Uani 1 1 d . . . O1 O 0.4301(5) 0.7111(6) 1.0395(3) 0.0245(17) Uani 1 1 d . . . O2 O 0.3983(6) 0.6439(8) 0.9432(3) 0.034(2) Uani 1 1 d . . . O3 O 0.6295(7) 0.5930(9) 1.0654(4) 0.046(2) Uani 1 1 d . . . O4 O 0.4461(5) 0.4849(7) 1.0419(3) 0.0266(18) Uani 1 1 d . . . O5 O 0.4823(7) 0.5708(8) 1.1343(3) 0.044(2) Uani 1 1 d . . . O6 O 0.2521(6) 0.6036(7) 1.0164(3) 0.0296(18) Uani 1 1 d . . . O7 O 0.2968(7) 0.6973(8) 1.1224(3) 0.038(2) Uani 1 1 d . . . O8 O 0.2775(8) 0.4702(9) 1.1069(4) 0.052(3) Uani 1 1 d . . . O9 O 0.2268(7) 0.8350(8) 1.0138(4) 0.046(2) Uani 1 1 d . . . O10 O 0.1804(8) 0.7193(10) 0.9188(3) 0.052(3) Uani 1 1 d U . . O11 O 0.6903(8) 0.4713(11) 1.1581(4) 0.067(3) Uani 1 1 d U . . O12 O 0.5074(10) 0.3380(9) 1.1470(4) 0.064(3) Uani 1 1 d U . . O13 O 0.6067(8) 0.7442(9) 0.9860(5) 0.058(3) Uani 1 1 d . . . C1 C 0.4405(14) 0.8755(14) 0.9170(7) 0.062(4) Uani 1 1 d U . . H1A H 0.4656 0.8101 0.9028 0.075 Uiso 1 1 calc R . . C2 C 0.3615(12) 0.9863(13) 0.9608(6) 0.048(4) Uani 1 1 d . . . H2A H 0.3168 1.0141 0.9838 0.058 Uiso 1 1 calc R . . C3 C 0.4291(14) 1.0507(15) 0.9368(6) 0.057(4) Uani 1 1 d . . . H3A H 0.4399 1.1282 0.9396 0.068 Uiso 1 1 calc R . . C4 C 0.5658(16) 1.0051(18) 0.8794(10) 0.100(7) Uani 1 1 d DU . . H4 H 0.5991 1.0670 0.9026 0.120 Uiso 1 1 calc R . . C5 C 0.6493(12) 0.9333(18) 0.8852(6) 0.074(6) Uani 1 1 d D . . H5A H 0.6639 0.9053 0.9222 0.112 Uiso 1 1 calc R . . H5B H 0.7119 0.9718 0.8775 0.112 Uiso 1 1 calc R . . H5C H 0.6320 0.8714 0.8603 0.112 Uiso 1 1 calc R . . C6 C 0.5214(15) 1.0700(18) 0.8280(8) 0.085(7) Uani 1 1 d . . . H6A H 0.5793 1.0898 0.8094 0.128 Uiso 1 1 calc R . . H6B H 0.4867 1.1374 0.8375 0.128 Uiso 1 1 calc R . . H6C H 0.4699 1.0242 0.8044 0.128 Uiso 1 1 calc R . . C7 C 0.8683(10) 0.6019(12) 0.0520(6) 0.041(3) Uani 1 1 d . . . H7A H 0.7932 0.5989 0.0450 0.049 Uiso 1 1 calc R . . C8 C 1.0318(12) 0.5682(19) 0.0824(7) 0.074(6) Uani 1 1 d . . . H8A H 1.0944 0.5338 0.1009 0.089 Uiso 1 1 calc R . . C9 C 1.0269(14) 0.6614(15) 0.0530(7) 0.059(4) Uani 1 1 d . . . H9A H 1.0849 0.7058 0.0475 0.070 Uiso 1 1 calc R . . C10 C 0.8791(12) 0.7693(15) -0.0024(10) 0.079(6) Uani 1 1 d . . . H10A H 0.8003 0.7674 -0.0060 0.094 Uiso 1 1 calc R . . C11 C 0.9199(19) 0.8818(15) 0.0207(11) 0.096(7) Uani 1 1 d . . . H11A H 0.9006 0.8919 0.0561 0.144 Uiso 1 1 calc R . . H11B H 0.8880 0.9408 -0.0034 0.144 Uiso 1 1 calc R . . H11C H 0.9970 0.8845 0.0242 0.144 Uiso 1 1 calc R . . C12 C 0.9089(18) 0.755(2) -0.0592(8) 0.096(7) Uani 1 1 d . . . H12A H 0.8815 0.6839 -0.0746 0.143 Uiso 1 1 calc R . . H12B H 0.9861 0.7560 -0.0559 0.143 Uiso 1 1 calc R . . H12C H 0.8779 0.8151 -0.0827 0.143 Uiso 1 1 calc R . . C13 C 0.4028(16) 0.4343(14) 0.2472(8) 0.068(6) Uani 1 1 d . . . H13A H 0.4110 0.4391 0.2108 0.082 Uiso 1 1 calc R . . C14 C 0.4177(11) 0.4634(13) 0.3318(6) 0.046(3) Uani 1 1 d . . . H14A H 0.4410 0.4930 0.3666 0.056 Uiso 1 1 calc R . . C15 C 0.3466(12) 0.3756(12) 0.3190(7) 0.053(4) Uani 1 1 d . . . H15A H 0.3101 0.3379 0.3430 0.064 Uiso 1 1 calc R . . C16 C 0.2806(17) 0.2643(18) 0.2314(9) 0.083(6) Uani 1 1 d . . . H16A H 0.3112 0.2646 0.1978 0.099 Uiso 1 1 calc R . . C17 C 0.3045(13) 0.1551(12) 0.2545(6) 0.051(4) Uani 1 1 d . . . H17A H 0.2652 0.0992 0.2308 0.076 Uiso 1 1 calc R . . H17B H 0.2838 0.1516 0.2898 0.076 Uiso 1 1 calc R . . H17C H 0.3806 0.1409 0.2583 0.076 Uiso 1 1 calc R . . C18 C 0.1708(16) 0.2957(17) 0.2143(8) 0.084(6) Uani 1 1 d U . . H18A H 0.1337 0.2377 0.1912 0.126 Uiso 1 1 calc R . . H18B H 0.1671 0.3653 0.1943 0.126 Uiso 1 1 calc R . . H18C H 0.1375 0.3053 0.2459 0.126 Uiso 1 1 calc R . . N1 N 0.3680(12) 0.8753(10) 0.9467(5) 0.057(4) Uani 1 1 d . . . N2 N 0.4765(10) 0.9764(12) 0.9083(6) 0.065(4) Uani 1 1 d . . . N3 N 0.9249(8) 0.6793(10) 0.0331(5) 0.041(3) Uani 1 1 d . . . N4 N 0.9288(11) 0.5314(14) 0.0811(7) 0.085(6) Uani 1 1 d . . . N5 N 0.3397(11) 0.3547(10) 0.2661(5) 0.049(3) Uani 1 1 d . . . N6 N 0.4486(11) 0.5004(11) 0.2841(7) 0.070(5) Uani 1 1 d . . . C19 C 0.6342(11) 0.6743(10) 0.2232(6) 0.041(3) Uani 1 1 d D A 1 C22 C 0.790(2) 0.772(2) 0.1929(11) 0.097(7) Uani 1 1 d U A 1 N9 N 0.7305(12) 0.7240(13) 0.2345(6) 0.078(5) Uani 1 1 d D A 1 N8 N 0.627(2) 0.627(2) 0.2750(13) 0.075(6) Uani 0.58(2) 1 d PD A 1 C20 C 0.728(3) 0.644(3) 0.3175(14) 0.075(6) Uani 0.58(2) 1 d PD A 1 C21 C 0.799(3) 0.697(3) 0.2931(14) 0.075(6) Uani 0.58(2) 1 d PD A 1 C23 C 0.752(3) 0.830(3) 0.1512(15) 0.075(6) Uani 0.58(2) 1 d P A 1 C24 C 0.905(3) 0.711(3) 0.2072(15) 0.075(6) Uani 0.58(2) 1 d P A 1 N8' N 0.577(2) 0.667(3) 0.2560(14) 0.062(6) Uani 0.42(2) 1 d PD A 2 C20' C 0.640(3) 0.713(4) 0.3019(17) 0.062(6) Uani 0.42(2) 1 d PD A 2 C21' C 0.708(3) 0.770(3) 0.2836(17) 0.062(6) Uani 0.42(2) 1 d PD A 2 C23' C 0.795(3) 0.895(4) 0.2000(17) 0.062(6) Uani 0.42(2) 1 d P A 2 C24' C 0.883(3) 0.712(4) 0.1798(18) 0.062(6) Uani 0.42(2) 1 d P A 2 O1W O 0.8880(15) 0.3974(15) 0.1668(8) 0.125(6) Uani 1 1 d U . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0211(5) 0.0455(6) 0.0225(5) 0.0056(4) 0.0106(4) 0.0093(4) Mo2 0.0171(5) 0.0373(6) 0.0386(6) -0.0036(5) 0.0135(4) -0.0027(4) Mo3 0.0254(5) 0.0445(6) 0.0257(5) 0.0079(5) 0.0119(4) 0.0114(5) Mo4 0.0366(6) 0.0819(10) 0.0187(5) 0.0051(5) 0.0070(4) 0.0328(6) O1 0.011(3) 0.037(5) 0.027(4) -0.002(3) 0.008(3) -0.008(3) O2 0.027(4) 0.054(5) 0.025(4) 0.018(4) 0.017(3) 0.015(4) O3 0.031(5) 0.064(6) 0.050(6) -0.019(5) 0.025(4) -0.008(5) O4 0.011(3) 0.047(5) 0.024(4) 0.003(4) 0.008(3) 0.008(3) O5 0.038(5) 0.065(7) 0.028(4) -0.008(4) 0.004(4) 0.022(5) O6 0.014(4) 0.043(5) 0.032(4) 0.008(4) 0.005(3) 0.006(3) O7 0.030(5) 0.053(6) 0.035(5) 0.000(4) 0.013(4) 0.022(4) O8 0.047(6) 0.054(6) 0.068(7) 0.032(5) 0.041(5) 0.017(5) O9 0.040(5) 0.048(6) 0.061(6) 0.017(5) 0.039(5) 0.013(4) O10 0.032(5) 0.093(7) 0.028(4) 0.007(4) 0.000(4) 0.022(5) O11 0.048(5) 0.107(7) 0.039(5) -0.019(5) -0.012(4) 0.043(5) O12 0.078(7) 0.070(6) 0.052(5) 0.031(5) 0.035(5) 0.047(5) O13 0.041(6) 0.052(6) 0.091(8) 0.000(6) 0.036(6) -0.010(5) C1 0.062(8) 0.057(8) 0.075(8) 0.015(6) 0.033(7) 0.026(6) C2 0.059(9) 0.047(9) 0.043(8) 0.004(7) 0.022(7) -0.001(7) C3 0.066(11) 0.063(11) 0.043(8) 0.018(8) 0.015(8) -0.004(9) C4 0.097(10) 0.106(10) 0.105(10) 0.045(8) 0.036(8) -0.002(8) C5 0.036(9) 0.146(19) 0.046(9) 0.043(11) 0.020(7) 0.021(10) C6 0.065(12) 0.119(17) 0.080(13) 0.056(12) 0.035(10) 0.001(11) C7 0.020(6) 0.042(8) 0.060(9) 0.006(7) 0.007(6) 0.002(6) C8 0.024(7) 0.128(18) 0.071(12) 0.026(11) 0.011(8) 0.020(9) C9 0.050(10) 0.064(11) 0.069(11) -0.006(9) 0.029(9) 0.002(8) C10 0.023(7) 0.057(11) 0.16(2) 0.035(12) 0.025(10) 0.013(7) C11 0.100(18) 0.039(11) 0.15(2) 0.025(12) 0.032(16) 0.011(10) C12 0.088(16) 0.127(19) 0.065(12) 0.041(13) -0.004(12) 0.018(14) C13 0.096(15) 0.047(10) 0.079(13) 0.031(9) 0.065(12) 0.026(10) C14 0.040(8) 0.054(9) 0.046(8) -0.008(7) 0.011(6) 0.004(7) C15 0.047(9) 0.037(8) 0.089(12) 0.018(8) 0.049(9) 0.012(7) C16 0.072(14) 0.089(15) 0.083(14) -0.028(12) 0.003(11) -0.002(12) C17 0.049(9) 0.041(9) 0.065(10) 0.002(7) 0.016(8) -0.011(7) C18 0.079(9) 0.085(9) 0.074(8) -0.015(7) -0.026(7) -0.005(8) N1 0.080(10) 0.042(7) 0.066(8) 0.026(6) 0.058(8) 0.020(6) N2 0.045(7) 0.069(9) 0.089(10) 0.060(8) 0.034(7) 0.028(7) N3 0.014(5) 0.056(7) 0.051(7) 0.002(6) 0.001(5) -0.004(5) N4 0.038(8) 0.095(12) 0.135(15) 0.054(11) 0.049(9) 0.017(8) N5 0.058(8) 0.043(7) 0.049(7) 0.001(6) 0.017(6) 0.016(6) N6 0.059(9) 0.042(8) 0.130(14) -0.008(9) 0.070(9) -0.004(7) C19 0.033(7) 0.034(7) 0.059(9) -0.009(6) 0.014(6) -0.009(6) C22 0.089(10) 0.103(11) 0.107(10) 0.018(8) 0.043(8) 0.002(8) N9 0.066(10) 0.113(13) 0.061(9) -0.028(9) 0.030(8) -0.065(9) N8 0.075(11) 0.070(10) 0.092(12) -0.034(9) 0.046(9) -0.028(8) C20 0.075(11) 0.070(10) 0.092(12) -0.034(9) 0.046(9) -0.028(8) C21 0.075(11) 0.070(10) 0.092(12) -0.034(9) 0.046(9) -0.028(8) C23 0.075(11) 0.070(10) 0.092(12) -0.034(9) 0.046(9) -0.028(8) C24 0.075(11) 0.070(10) 0.092(12) -0.034(9) 0.046(9) -0.028(8) N8' 0.029(8) 0.083(14) 0.069(12) -0.011(10) -0.003(8) -0.009(8) C20' 0.029(8) 0.083(14) 0.069(12) -0.011(10) -0.003(8) -0.009(8) C21' 0.029(8) 0.083(14) 0.069(12) -0.011(10) -0.003(8) -0.009(8) C23' 0.029(8) 0.083(14) 0.069(12) -0.011(10) -0.003(8) -0.009(8) C24' 0.029(8) 0.083(14) 0.069(12) -0.011(10) -0.003(8) -0.009(8) O1W 0.113(9) 0.125(9) 0.130(9) 0.011(8) 0.006(8) -0.007(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 O8 1.700(10) . ? Mo1 O7 1.717(8) . ? Mo1 O5 1.927(9) . ? Mo1 O6 1.946(8) . ? Mo1 O4 2.243(7) . ? Mo1 O1 2.321(7) . ? Mo2 O13 1.671(10) . ? Mo2 O3 1.757(10) . ? Mo2 O1 1.875(7) . ? Mo2 O4 1.962(8) 3_667 ? Mo2 O2 2.146(8) . ? Mo2 O4 2.389(8) . ? Mo3 O9 1.705(9) . ? Mo3 O10 1.737(9) . ? Mo3 O6 1.873(8) . ? Mo3 O2 2.140(8) . ? Mo3 N1 2.239(12) . ? Mo3 O1 2.240(7) . ? Mo4 O11 1.730(10) . ? Mo4 O12 1.755(11) . ? Mo4 O2 1.921(8) 3_667 ? Mo4 O5 1.925(9) . ? Mo4 O4 2.203(7) . ? Mo4 O3 2.342(10) . ? O2 Mo4 1.921(8) 3_667 ? O4 Mo2 1.962(8) 3_667 ? C1 N1 1.273(18) . ? C1 N2 1.31(2) . ? C2 C3 1.36(2) . ? C2 N1 1.369(19) . ? C3 N2 1.34(2) . ? C4 C5 1.340(10) . ? C4 N2 1.48(2) . ? C4 C6 1.51(2) . ? C7 N4 1.266(19) . ? C7 N3 1.300(16) . ? C8 C9 1.32(2) . ? C8 N4 1.36(2) . ? C9 N3 1.307(19) . ? C10 N3 1.44(2) . ? C10 C11 1.50(3) . ? C10 C12 1.53(3) . ? C13 N6 1.26(2) . ? C13 N5 1.37(2) . ? C14 C15 1.37(2) . ? C14 N6 1.383(19) . ? C15 N5 1.323(19) . ? C16 C18 1.42(3) . ? C16 C17 1.43(2) . ? C16 N5 1.49(2) . ? C19 N9 1.332(17) . ? C19 N8 1.42(3) . ? C22 C23 1.26(4) . ? C22 N9 1.49(2) . ? C22 C24 1.60(5) . ? N9 C21 1.58(4) . ? N8 C20 1.51(4) . ? C20 C21 1.32(4) . ? N8' C20' 1.38(5) . ? C20' C21' 1.24(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O8 Mo1 O7 105.8(5) . . ? O8 Mo1 O5 101.4(5) . . ? O7 Mo1 O5 97.6(4) . . ? O8 Mo1 O6 96.1(4) . . ? O7 Mo1 O6 100.3(4) . . ? O5 Mo1 O6 150.4(3) . . ? O8 Mo1 O4 93.3(4) . . ? O7 Mo1 O4 160.0(4) . . ? O5 Mo1 O4 72.3(3) . . ? O6 Mo1 O4 83.2(3) . . ? O8 Mo1 O1 162.4(4) . . ? O7 Mo1 O1 89.9(4) . . ? O5 Mo1 O1 84.0(4) . . ? O6 Mo1 O1 72.8(3) . . ? O4 Mo1 O1 72.1(3) . . ? O13 Mo2 O3 100.6(5) . . ? O13 Mo2 O1 104.9(4) . . ? O3 Mo2 O1 103.1(4) . . ? O13 Mo2 O4 103.1(4) . 3_667 ? O3 Mo2 O4 98.2(4) . 3_667 ? O1 Mo2 O4 140.6(3) . 3_667 ? O13 Mo2 O2 98.1(5) . . ? O3 Mo2 O2 160.8(4) . . ? O1 Mo2 O2 75.8(3) . . ? O4 Mo2 O2 73.3(3) 3_667 . ? O13 Mo2 O4 176.8(4) . . ? O3 Mo2 O4 76.4(4) . . ? O1 Mo2 O4 77.1(3) . . ? O4 Mo2 O4 76.2(3) 3_667 . ? O2 Mo2 O4 84.7(3) . . ? O9 Mo3 O10 103.2(5) . . ? O9 Mo3 O6 100.9(4) . . ? O10 Mo3 O6 101.0(4) . . ? O9 Mo3 O2 157.4(4) . . ? O10 Mo3 O2 93.8(4) . . ? O6 Mo3 O2 90.2(3) . . ? O9 Mo3 N1 84.8(4) . . ? O10 Mo3 N1 96.3(5) . . ? O6 Mo3 N1 160.0(4) . . ? O2 Mo3 N1 78.5(4) . . ? O9 Mo3 O1 94.5(4) . . ? O10 Mo3 O1 162.3(4) . . ? O6 Mo3 O1 76.1(3) . . ? O2 Mo3 O1 68.9(3) . . ? N1 Mo3 O1 84.4(4) . . ? O11 Mo4 O12 105.0(6) . . ? O11 Mo4 O2 105.1(4) . 3_667 ? O12 Mo4 O2 95.6(4) . 3_667 ? O11 Mo4 O5 101.6(5) . . ? O12 Mo4 O5 98.4(4) . . ? O2 Mo4 O5 145.4(3) 3_667 . ? O11 Mo4 O4 151.9(5) . . ? O12 Mo4 O4 103.1(4) . . ? O2 Mo4 O4 72.8(3) 3_667 . ? O5 Mo4 O4 73.2(3) . . ? O11 Mo4 O3 81.8(5) . . ? O12 Mo4 O3 173.2(5) . . ? O2 Mo4 O3 82.7(3) 3_667 . ? O5 Mo4 O3 79.7(4) . . ? O4 Mo4 O3 70.1(3) . . ? Mo2 O1 Mo3 110.6(3) . . ? Mo2 O1 Mo1 112.0(4) . . ? Mo3 O1 Mo1 90.3(2) . . ? Mo4 O2 Mo3 148.0(5) 3_667 . ? Mo4 O2 Mo2 106.9(4) 3_667 . ? Mo3 O2 Mo2 104.5(3) . . ? Mo2 O3 Mo4 115.1(4) . . ? Mo2 O4 Mo4 103.3(3) 3_667 . ? Mo2 O4 Mo1 150.2(4) 3_667 . ? Mo4 O4 Mo1 93.8(3) . . ? Mo2 O4 Mo2 103.8(3) 3_667 . ? Mo4 O4 Mo2 98.2(3) . . ? Mo1 O4 Mo2 97.6(3) . . ? Mo4 O5 Mo1 114.8(4) . . ? Mo3 O6 Mo1 115.7(4) . . ? N1 C1 N2 113.8(15) . . ? C3 C2 N1 110.9(14) . . ? N2 C3 C2 103.8(15) . . ? C5 C4 N2 116.9(15) . . ? C5 C4 C6 125.4(18) . . ? N2 C4 C6 109.3(15) . . ? N4 C7 N3 111.0(12) . . ? C9 C8 N4 107.8(15) . . ? N3 C9 C8 106.8(15) . . ? N3 C10 C11 110.7(17) . . ? N3 C10 C12 110.0(15) . . ? C11 C10 C12 109.1(17) . . ? N6 C13 N5 113.5(15) . . ? C15 C14 N6 108.4(14) . . ? N5 C15 C14 107.1(13) . . ? C18 C16 C17 118.7(19) . . ? C18 C16 N5 110.0(16) . . ? C17 C16 N5 112.0(16) . . ? C1 N1 C2 103.2(13) . . ? C1 N1 Mo3 131.1(11) . . ? C2 N1 Mo3 125.5(9) . . ? C1 N2 C3 108.2(13) . . ? C1 N2 C4 127.3(16) . . ? C3 N2 C4 123.9(16) . . ? C7 N3 C9 108.3(13) . . ? C7 N3 C10 124.0(11) . . ? C9 N3 C10 127.6(13) . . ? C7 N4 C8 105.9(15) . . ? C15 N5 C13 105.8(14) . . ? C15 N5 C16 130.2(15) . . ? C13 N5 C16 124.0(15) . . ? C13 N6 C14 105.1(13) . . ? N9 C19 N8 101.0(16) . . ? C23 C22 N9 128(3) . . ? C23 C22 C24 128(3) . . ? N9 C22 C24 103(2) . . ? C19 N9 C22 125.0(16) . . ? C19 N9 C21 115.1(16) . . ? C22 N9 C21 117.2(17) . . ? C19 N8 C20 113(2) . . ? C21 C20 N8 107(3) . . ? C20 C21 N9 103(3) . . ? C21' C20' N8' 104(4) . . ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 27.59 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 1.285 _refine_diff_density_min -2.356 _refine_diff_density_rms 0.295 _database_code_depnum_ccdc_archive 'CCDC 939805' ####################################################################### # # 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_8 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C64 H96 Mo9 N32 O32 S3' _chemical_formula_sum 'C64 H96 Mo9 N32 O32 S3' _chemical_formula_weight 2785.14 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc ' 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 15.878(3) _cell_length_b 10.1503(19) _cell_length_c 16.704(3) _cell_angle_alpha 90.00 _cell_angle_beta 115.779(3) _cell_angle_gamma 90.00 _cell_volume 2424.1(8) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4007 _cell_measurement_theta_min 3.09 _cell_measurement_theta_max 27.90 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.908 _exptl_crystal_density_method &nb _exptl_crystal_F_000 1385.9 _exptl_absorpt_coefficient_mu 1.281 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.719 _exptl_absorpt_correction_T_max 0.743 _exptl_absorpt_process_details SADABS,Bruker(2005) _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bru ker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11828 _diffrn_reflns_av_R_equivalents 0.0338 _diffrn_reflns_av_sigmaI/netI 0.0408 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min &n _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4266 _reflns_number_gt 3439 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_grap hics _computing_publication_material 'Bruker SHELXTL' _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^)+(0.2000P)^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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.030(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4232 _refine_ls_number_parameters 322 _refine_ls_number_restraints 408 _refine_ls_R_factor_all 0.1150 _refine_ls_R_factor_gt 0.0734 _refine_ls_wR_factor_ref 0.2803 _refine_ls_wR_factor_gt 0.1772 _refine_ls_goodness_of_fit_ref 1.231 _refine_ls_restrained_S_all 1.197 _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 0.22980(5) 0.52691(7) 0.42969(5) 0.0247(4) Uani 1 1 d . A . Mo3 Mo 0.18344(10) 0.61546(15) 0.60153(9) 0.0274(6) Uani 0.249(6) 1 d P A 1 S1 S 0.18344(10) 0.61546(15) 0.60153(9) 0.0274(6) Uani 0.751(6) 1 d P A 2 N1 N 0.2915(5) 0.7214(8) 0.4252(5) 0.0337(15) Uani 1 1 d U . . O1 O 0.0906(5) 0.6249(9) 0.6028(6) 0.061(2) Uani 1 1 d . . . C1 C 0.3271(6) 0.7556(10) 0.3727(7) 0.0388(18) Uani 1 1 d U . . H1 H 0.3296 0.7015 0.3289 0.047 Uiso 1 1 calc R . . Mo2 Mo 0.26949(5) 0.34210(7) 0.54410(5) 0.0268(4) Uani 1 1 d . A . O2 O 0.2560(6) 0.7053(9) 0.6698(6) 0.069(2) Uani 1 1 d . . . N2 N 0.3606(6) 0.8803(9) 0.3888(6) 0.0482(19) Uani 1 1 d U . . C2 C 0.2999(7) 0.8297(10) 0.4763(7) 0.0422(19) Uani 1 1 d U . . H2 H 0.2799 0.8335 0.5210 0.051 Uiso 1 1 calc R . . O3 O 0.1746(5) 0.6455(7) 0.5054(4) 0.0386(16) Uani 1 1 d . . . N3 N 0.3803(5) 0.3030(8) 0.6822(5) 0.0401(16) Uani 1 1 d U . . C3 C 0.3395(8) 0.9279(11) 0.4546(8) 0.051(2) Uani 1 1 d U . . H3 H 0.3509 1.0122 0.4788 0.061 Uiso 1 1 calc R . . O4 O 0.2182(5) 0.4640(6) 0.6238(5) 0.0358(16) Uani 1 1 d . . . N4 N 0.4544(6) 0.2253(9) 0.8158(6) 0.0418(17) Uani 1 1 d U . . C4 C 0.4087(9) 0.9496(13) 0.3410(9) 0.065(3) Uani 1 1 d U . . H4A H 0.4750 0.9367 0.3726 0.098 Uiso 1 1 calc R . . H4B H 0.3948 1.0421 0.3376 0.098 Uiso 1 1 calc R . . H4C H 0.3869 0.9143 0.2820 0.098 Uiso 1 1 calc R . . O5 O 0.3180(5) 0.2250(6) 0.5050(5) 0.0398(16) Uani 1 1 d . . . N5 N 0.1809(6) 0.1956(8) 0.5709(5) 0.0390(16) Uani 1 1 d U . . C5 C 0.5213(8) 0.2728(13) 0.7949(8) 0.057(2) Uani 1 1 d U . . H5 H 0.5858 0.2723 0.8290 0.068 Uiso 1 1 calc R . . O6 O 0.1545(4) 0.3900(6) 0.4448(4) 0.0300(13) Uani 1 1 d . . . N6 N 0.0683(6) 0.1094(8) 0.5925(6) 0.0397(16) Uani 1 1 d U . . C6 C 0.4695(8) 0.3238(13) 0.7081(8) 0.055(2) Uani 1 1 d U . . H6 H 0.4952 0.3659 0.6745 0.066 Uiso 1 1 calc R . . O7 O 0.3362(4) 0.5024(6) 0.5454(4) 0.0288(14) Uani 1 1 d . . . N7 N 0.0982(5) 0.6036(7) 0.3247(5) 0.0325(15) Uani 1 1 d U . . C7 C 0.3721(7) 0.2443(10) 0.7504(7) 0.0393(18) Uani 1 1 d U . . H7 H 0.3158 0.2206 0.7509 0.047 Uiso 1 1 calc R . . O8 O 0.2659(5) 0.4711(6) 0.3542(4) 0.0385(17) Uani 1 1 d . . . N8 N -0.0508(6) 0.6399(8) 0.2468(5) 0.0399(18) Uani 1 1 d U . . C8 C 0.4766(8) 0.1690(12) 0.9054(8) 0.054(3) Uani 1 1 d U . . H8A H 0.4238 0.1200 0.9029 0.082 Uiso 1 1 calc R . . H8B H 0.4906 0.2392 0.9478 0.082 Uiso 1 1 calc R . . H8C H 0.5298 0.1117 0.9231 0.082 Uiso 1 1 calc R . . C9 C 0.1309(7) 0.0161(10) 0.6142(7) 0.042(2) Uani 1 1 d U A . H9 H 0.1260 -0.0687 0.6329 0.050 Uiso 1 1 calc R . . C10 C 0.2065(8) 0.0688(10) 0.6036(7) 0.0433(19) Uani 1 1 d U A . H10 H 0.2630 0.0272 0.6160 0.052 Uiso 1 1 calc R . . C11 C 0.0989(7) 0.2146(10) 0.5660(7) 0.0375(18) Uani 1 1 d U A . H11 H 0.0652 0.2924 0.5463 0.045 Uiso 1 1 calc R . . C12 C -0.0194(7) 0.0997(11) 0.5987(7) 0.047(2) Uani 1 1 d U A . H12A H -0.0477 0.0158 0.5762 0.070 Uiso 1 1 calc R . . H12B H -0.0605 0.1688 0.5643 0.070 Uiso 1 1 calc R . . H12C H -0.0084 0.1081 0.6597 0.070 Uiso 1 1 calc R . . C13 C 0.0135(6) 0.5760(10) 0.3154(6) 0.0341(18) Uani 1 1 d U A . H13 H 0.0003 0.5191 0.3521 0.041 Uiso 1 1 calc R . . C14 C 0.0875(6) 0.6907(9) 0.2558(6) 0.0322(16) Uani 1 1 d U A . H14 H 0.1349 0.7264 0.2442 0.039 Uiso 1 1 calc R . . C15 C -0.0059(6) 0.7128(10) 0.2093(6) 0.0330(17) Uani 1 1 d U A . H15 H -0.0339 0.7681 0.1604 0.040 Uiso 1 1 calc R . . C16 C -0.1556(8) 0.6321(13) 0.2129(8) 0.059(3) Uani 1 1 d U A . H16A H -0.1823 0.5916 0.1553 0.089 Uiso 1 1 calc R . . H16B H -0.1806 0.7193 0.2087 0.089 Uiso 1 1 calc R . . H16C H -0.1705 0.5805 0.2532 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 0.0263(5) 0.0222(6) 0.0250(6) -0.0010(3) 0.0106(4) 0.0021(3) Mo3 0.0300(9) 0.0306(10) 0.0227(9) 0.0007(6) 0.0125(7) 0.0065(6) S1 0.0300(9) 0.0306(10) 0.0227(9) 0.0007(6) 0.0125(7) 0.0065(6) N1 0.028(3) 0.030(3) 0.038(3) -0.001(3) 0.010(3) -0.003(3) O1 0.045(4) 0.084(6) 0.058(5) 0.018(5) 0.024(4) 0.007(4) C1 0.034(3) 0.033(3) 0.040(3) 0.001(3) 0.007(3) -0.008(3) Mo2 0.0286(6) 0.0222(6) 0.0272(6) 0.0000(3) 0.0099(4) 0.0029(3) O2 0.083(6) 0.059(6) 0.043(5) 0.008(4) 0.008(4) 0.010(5) N2 0.051(4) 0.030(3) 0.050(4) 0.005(3) 0.010(3) -0.013(3) C2 0.037(4) 0.037(4) 0.050(4) -0.009(3) 0.017(3) -0.001(3) O3 0.041(4) 0.041(4) 0.029(4) -0.007(3) 0.011(3) 0.011(3) N3 0.041(3) 0.039(3) 0.037(3) 0.001(3) 0.015(3) 0.008(3) C3 0.049(4) 0.032(4) 0.056(4) -0.006(4) 0.009(4) -0.003(3) O4 0.048(4) 0.028(4) 0.035(4) 0.001(3) 0.022(3) 0.007(3) N4 0.040(3) 0.044(4) 0.037(3) 0.000(3) 0.012(3) 0.009(3) C4 0.061(6) 0.052(6) 0.064(6) 0.010(5) 0.010(5) -0.023(5) O5 0.039(4) 0.032(4) 0.054(4) 0.003(3) 0.026(3) 0.010(3) N5 0.047(3) 0.027(3) 0.039(3) 0.001(3) 0.016(3) 0.000(3) C5 0.049(4) 0.061(4) 0.044(4) 0.004(4) 0.005(4) 0.003(4) O6 0.031(3) 0.026(3) 0.029(3) -0.002(3) 0.010(3) 0.000(3) N6 0.054(4) 0.032(3) 0.045(3) -0.002(3) 0.032(3) -0.002(3) C6 0.047(4) 0.061(4) 0.044(4) 0.006(4) 0.008(4) 0.000(4) O7 0.019(3) 0.032(3) 0.027(3) 0.001(3) 0.002(3) -0.001(2) N7 0.033(3) 0.030(3) 0.028(3) 0.003(3) 0.007(2) 0.002(3) C7 0.038(3) 0.040(4) 0.036(3) -0.001(3) 0.012(3) 0.006(3) O8 0.056(4) 0.034(4) 0.035(4) -0.001(3) 0.029(4) 0.004(3) N8 0.040(3) 0.032(3) 0.033(3) 0.006(3) 0.002(3) 0.004(3) C8 0.056(5) 0.052(6) 0.045(5) 0.008(4) 0.012(5) 0.009(5) C9 0.046(4) 0.030(4) 0.041(4) 0.003(3) 0.012(3) 0.000(3) C10 0.050(3) 0.031(3) 0.045(3) 0.001(3) 0.017(3) 0.003(3) C11 0.044(4) 0.030(4) 0.042(4) 0.001(3) 0.022(3) -0.003(3) C12 0.037(5) 0.048(5) 0.056(5) -0.005(5) 0.021(4) -0.003(4) C13 0.028(3) 0.032(4) 0.036(4) 0.004(3) 0.009(3) 0.000(3) C14 0.028(3) 0.035(3) 0.034(3) 0.005(3) 0.014(3) 0.003(3) C15 0.029(3) 0.034(4) 0.032(3) 0.004(3) 0.009(3) 0.003(3) C16 0.058(5) 0.061(6) 0.046(5) 0.005(5) 0.010(5) 0.000(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 O8 1.693(6) . ? Mo1 O6 1.920(6) . ? Mo1 O7 1.952(6) . ? Mo1 O3 2.186(6) . ? Mo1 N7 2.204(7) . ? Mo1 N1 2.220(8) . ? Mo1 Mo2 2.5536(11) . ? Mo3 O1 1.486(8) . ? Mo3 O2 1.521(9) . ? Mo3 O3 1.580(7) . ? Mo3 O4 1.621(6) . ? N1 C1 1.280(12) . ? N1 C2 1.363(13) . ? C1 N2 1.354(13) . ? Mo2 O5 1.694(6) . ? Mo2 O6 1.920(6) . ? Mo2 O7 1.936(6) . ? Mo2 O4 2.215(6) . ? Mo2 N5 2.222(8) . ? Mo2 N3 2.246(8) . ? N2 C3 1.368(16) . ? N2 C4 1.499(15) . ? C2 C3 1.311(16) . ? N3 C6 1.305(14) . ? N3 C7 1.340(13) . ? N4 C7 1.302(12) . ? N4 C5 1.344(15) . ? N4 C8 1.494(14) . ? N5 C11 1.283(13) . ? N5 C10 1.388(13) . ? C5 C6 1.418(16) . ? N6 C9 1.305(13) . ? N6 C11 1.327(12) . ? N6 C12 1.443(12) . ? N7 C13 1.316(12) . ? N7 C14 1.401(12) . ? N8 C13 1.325(12) . ? N8 C15 1.355(13) . ? N8 C16 1.508(15) . ? C9 C10 1.394(15) . ? C14 C15 1.360(12) . ? 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 O6 106.7(3) . . ? O8 Mo1 O7 105.5(3) . . ? O6 Mo1 O7 95.6(3) . . ? O8 Mo1 O3 164.9(3) . . ? O6 Mo1 O3 83.9(3) . . ? O7 Mo1 O3 83.6(3) . . ? O8 Mo1 N7 92.1(3) . . ? O6 Mo1 N7 86.1(3) . . ? O7 Mo1 N7 160.9(3) . . ? O3 Mo1 N7 77.6(3) . . ? O8 Mo1 N1 88.6(3) . . ? O6 Mo1 N1 163.2(3) . . ? O7 Mo1 N1 86.7(3) . . ? O3 Mo1 N1 79.8(3) . . ? N7 Mo1 N1 86.5(3) . . ? O8 Mo1 Mo2 105.0(2) . . ? O6 Mo1 Mo2 48.30(17) . . ? O7 Mo1 Mo2 48.67(18) . . ? O3 Mo1 Mo2 90.12(19) . . ? N7 Mo1 Mo2 134.0(2) . . ? N1 Mo1 Mo2 135.21(19) . . ? O1 Mo3 O2 112.5(5) . . ? O1 Mo3 O3 110.6(4) . . ? O2 Mo3 O3 110.4(5) . . ? O1 Mo3 O4 107.4(4) . . ? O2 Mo3 O4 109.0(4) . . ? O3 Mo3 O4 106.7(3) . . ? C1 N1 C2 105.0(9) . . ? C1 N1 Mo1 126.7(7) . . ? C2 N1 Mo1 128.3(7) . . ? N1 C1 N2 111.7(9) . . ? O5 Mo2 O6 105.4(3) . . ? O5 Mo2 O7 104.8(3) . . ? O6 Mo2 O7 96.1(3) . . ? O5 Mo2 O4 166.2(3) . . ? O6 Mo2 O4 85.3(3) . . ? O7 Mo2 O4 82.3(3) . . ? O5 Mo2 N5 92.4(3) . . ? O6 Mo2 N5 84.0(3) . . ? O7 Mo2 N5 162.0(3) . . ? O4 Mo2 N5 79.7(3) . . ? O5 Mo2 N3 89.3(3) . . ? O6 Mo2 N3 163.3(3) . . ? O7 Mo2 N3 87.5(3) . . ? O4 Mo2 N3 79.0(3) . . ? N5 Mo2 N3 87.5(3) . . ? O5 Mo2 Mo1 103.4(2) . . ? O6 Mo2 Mo1 48.31(18) . . ? O7 Mo2 Mo1 49.23(17) . . ? O4 Mo2 Mo1 90.22(17) . . ? N5 Mo2 Mo1 132.1(2) . . ? N3 Mo2 Mo1 136.6(2) . . ? C1 N2 C3 106.1(9) . . ? C1 N2 C4 125.4(10) . . ? C3 N2 C4 128.5(10) . . ? C3 C2 N1 111.6(10) . . ? Mo3 O3 Mo1 127.0(4) . . ? C6 N3 C7 106.4(9) . . ? C6 N3 Mo2 124.3(8) . . ? C7 N3 Mo2 129.0(7) . . ? C2 C3 N2 105.5(10) . . ? Mo3 O4 Mo2 124.7(4) . . ? C7 N4 C5 110.3(9) . . ? C7 N4 C8 127.7(9) . . ? C5 N4 C8 121.9(9) . . ? C11 N5 C10 106.3(9) . . ? C11 N5 Mo2 126.9(7) . . ? C10 N5 Mo2 126.6(7) . . ? N4 C5 C6 102.9(9) . . ? Mo2 O6 Mo1 83.4(2) . . ? C9 N6 C11 109.3(9) . . ? C9 N6 C12 124.9(9) . . ? C11 N6 C12 125.7(9) . . ? N3 C6 C5 110.1(11) . . ? Mo2 O7 Mo1 82.1(2) . . ? C13 N7 C14 106.5(7) . . ? C13 N7 Mo1 125.9(6) . . ? C14 N7 Mo1 127.7(6) . . ? N4 C7 N3 110.2(9) . . ? C13 N8 C15 107.7(8) . . ? C13 N8 C16 127.4(9) . . ? C15 N8 C16 124.8(8) . . ? N6 C9 C10 106.3(9) . . ? N5 C10 C9 106.5(9) . . ? N5 C11 N6 111.5(9) . . ? N7 C13 N8 111.2(8) . . ? C15 C14 N7 106.7(8) . . ? N8 C15 C14 107.9(8) . . ? _diffrn_me asured_fraction_theta_max _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 2.875 _refine_diff_density_min -4.596 _refine_diff_density_rms 0.842 _database_code_depnum_ccdc_archive 'CCDC 939887' ####################################################################### # # 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_9 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H18 Mo N6 O3' _chemical_formula_sum 'C12 H18 Mo N6 O3' _chemical_formula_weight 390.26 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting rhombohedral _symmetry_space_group_name_H-M 'R -3' _symmetry_space_group_name_Hall '-R 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 11.6102(9) _cell_length_b 11.6102(9) _cell_length_c 19.4306(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2268.3(3) _cell_formula_units_Z 6 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2033 _cell_measurement_theta_min 2.92 _cell_measurement_theta_max 27.88 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.714 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1188.0 _exptl_absorpt_coefficient_mu 0.890 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.808 _exptl_absorpt_correction_T_max 0.875 _exptl_absorpt_process_details SADABS,Bruker(2005) _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3952 _diffrn_reflns_av_R_equivalents 0.1244 _diffrn_reflns_av_sigmaI/netI 0.0656 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 25.20 _reflns_number_total 912 _reflns_number_gt 823 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0346P)^2^+1.0914P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 912 _refine_ls_number_parameters 68 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0442 _refine_ls_R_factor_gt 0.0380 _refine_ls_wR_factor_ref 0.0706 _refine_ls_wR_factor_gt 0.0663 _refine_ls_goodness_of_fit_ref 1.119 _refine_ls_restrained_S_all 1.119 _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 0.0000 0.0000 0.215097(19) 0.02734(18) Uani 1 3 d S . . O1 O 0.1578(2) 0.0729(2) 0.25037(11) 0.0420(5) Uani 1 1 d . . . N1 N 0.0972(2) 0.1700(2) 0.13199(11) 0.0286(5) Uani 1 1 d . . . N2 N 0.2522(2) 0.3580(2) 0.08615(13) 0.0331(6) Uani 1 1 d . . . C3 C 0.2241(3) 0.2633(3) 0.13328(15) 0.0345(7) Uani 1 1 d . . . H3 H 0.2864 0.2632 0.1633 0.041 Uiso 1 1 calc R . . C1 C 0.0424(3) 0.2091(3) 0.08081(15) 0.0343(6) Uani 1 1 d . . . H1 H -0.0465 0.1629 0.0678 0.041 Uiso 1 1 calc R . . C2 C 0.1360(3) 0.3238(3) 0.05223(14) 0.0349(7) Uani 1 1 d . . . H2 H 0.1240 0.3705 0.0167 0.042 Uiso 1 1 calc R . . C4 C 0.3804(3) 0.4761(4) 0.07318(19) 0.0530(9) Uani 1 1 d . . . H4A H 0.3944 0.5441 0.1058 0.079 Uiso 1 1 calc R . . H4B H 0.3816 0.5078 0.0274 0.079 Uiso 1 1 calc R . . H4C H 0.4498 0.4546 0.0778 0.079 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 0.0310(2) 0.0310(2) 0.0200(2) 0.000 0.000 0.01550(10) O1 0.0415(12) 0.0499(13) 0.0322(11) -0.0016(10) -0.0100(9) 0.0211(11) N1 0.0314(13) 0.0289(12) 0.0260(11) 0.0009(10) -0.0011(10) 0.0156(10) N2 0.0323(13) 0.0293(12) 0.0340(13) 0.0025(10) 0.0023(10) 0.0125(11) C3 0.0344(16) 0.0368(16) 0.0338(15) 0.0004(13) -0.0061(12) 0.0188(14) C1 0.0321(15) 0.0389(16) 0.0315(15) 0.0011(12) -0.0040(12) 0.0173(13) C2 0.0407(17) 0.0372(16) 0.0303(15) 0.0027(12) -0.0006(13) 0.0221(14) C4 0.0392(18) 0.0422(19) 0.064(2) 0.0081(17) 0.0028(16) 0.0099(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 O1 1.729(2) . ? Mo1 O1 1.729(2) 2 ? Mo1 O1 1.729(2) 3 ? Mo1 N1 2.356(2) 2 ? Mo1 N1 2.356(2) . ? Mo1 N1 2.356(2) 3 ? N1 C3 1.322(4) . ? N1 C1 1.374(4) . ? N2 C3 1.340(4) . ? N2 C2 1.371(4) . ? N2 C4 1.455(4) . ? C3 H3 0.9300 . ? C1 C2 1.348(4) . ? C1 H1 0.9300 . ? C2 H2 0.9300 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mo1 O1 105.33(8) . 2 ? O1 Mo1 O1 105.33(8) . 3 ? O1 Mo1 O1 105.33(8) 2 3 ? O1 Mo1 N1 159.99(9) . 2 ? O1 Mo1 N1 85.13(9) 2 2 ? O1 Mo1 N1 87.72(9) 3 2 ? O1 Mo1 N1 85.13(9) . . ? O1 Mo1 N1 87.72(9) 2 . ? O1 Mo1 N1 159.99(9) 3 . ? N1 Mo1 N1 78.19(8) 2 . ? O1 Mo1 N1 87.72(9) . 3 ? O1 Mo1 N1 159.99(9) 2 3 ? O1 Mo1 N1 85.13(9) 3 3 ? N1 Mo1 N1 78.19(8) 2 3 ? N1 Mo1 N1 78.19(8) . 3 ? C3 N1 C1 104.7(2) . . ? C3 N1 Mo1 122.96(18) . . ? C1 N1 Mo1 131.72(19) . . ? C3 N2 C2 106.9(2) . . ? C3 N2 C4 127.4(3) . . ? C2 N2 C4 125.7(3) . . ? N1 C3 N2 111.9(2) . . ? N1 C3 H3 124.0 . . ? N2 C3 H3 124.0 . . ? C2 C1 N1 110.3(3) . . ? C2 C1 H1 124.8 . . ? N1 C1 H1 124.8 . . ? C1 C2 N2 106.1(2) . . ? C1 C2 H2 126.9 . . ? N2 C2 H2 126.9 . . ? N2 C4 H4A 109.5 . . ? N2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.20 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.439 _refine_diff_density_min -1.857 _refine_diff_density_rms 0.171 _database_code_depnum_ccdc_archive 'CCDC 939888' ####################################################################### # # 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_7 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H36 Mo3 N12 O9' _chemical_formula_sum 'C30 H36 Mo3 N12 O9' _chemical_formula_weight 996.53 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' _symmetry_space_group_name_Hall 'P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.6874(7) _cell_length_b 18.8238(14) _cell_length_c 10.3652(6) _cell_angle_alpha 90.00 _cell_angle_beta 102.994(7) _cell_angle_gamma 90.00 _cell_volume 1841.7(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1398 _cell_measurement_theta_min 2.8117 _cell_measurement_theta_max 29.5084 _exptl_crystal_description brock _exptl_crystal_colour brown _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.797 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 996 _exptl_absorpt_coefficient_mu 1.075 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7387 _exptl_absorpt_correction_T_max 0.8138 _exptl_absorpt_process_details sadabs,bruker(2005) _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 9178 _diffrn_reflns_av_R_equivalents 0.0758 _diffrn_reflns_av_sigmaI/netI 0.1353 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.82 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5070 _reflns_number_gt 3686 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is &nb sp;not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.06(5) _refine_ls_number_reflns 5070 _refine_ls_number_parameters 487 _refine_ls_number_restraints 866 _refine_ls_R_factor_all 0.0973 _refine_ls_R_factor_gt 0.0599 _refine_ls_wR_factor_ref 0.0867 _refine_ls_wR_factor_gt 0.0780 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 0.940 _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 0.78266(10) 0.39288(5) 0.22375(8) 0.0249(2) Uani 1 1 d . . . Mo2 Mo 0.70904(10) 0.20960(5) 0.33810(8) 0.0270(3) Uani 1 1 d . . . Mo3 Mo 0.88584(10) 0.34818(6) 0.58419(8) 0.0288(3) Uani 1 1 d . . . O1 O 0.5296(7) 0.2260(4) 0.3135(6) 0.035(2) Uani 1 1 d . . . O2 O 0.8229(7) 0.3969(4) 0.4345(5) 0.0278(18) Uani 1 1 d . . . O3 O 0.9605(7) 0.3974(5) 0.2206(6) 0.038(2) Uani 1 1 d . . . O4 O 1.0523(7) 0.3213(4) 0.5741(6) 0.036(2) Uani 1 1 d . . . O5 O 0.7229(8) 0.1209(4) 0.3822(7) 0.040(2) Uani 1 1 d . . . O6 O 0.9203(8) 0.4119(4) 0.7064(6) 0.043(2) Uani 1 1 d . . . O7 O 0.6997(8) 0.4161(4) 0.0660(5) 0.039(2) Uani 1 1 d . . . O8 O 0.7491(8) 0.2986(4) 0.2283(7) 0.0298(18) Uani 1 1 d . . . O9 O 0.7848(7) 0.2577(4) 0.4890(6) 0.0271(18) Uani 1 1 d . . . N1 N 0.9034(10) 0.2688(6) 0.7565(9) 0.0424(18) Uani 1 1 d U . . N2 N 0.9236(11) 0.1628(7) 0.8600(10) 0.053(2) Uani 1 1 d U . . N3 N 0.6518(8) 0.3508(6) 0.6324(7) 0.0299(15) Uani 1 1 d U . . N4 N 0.4827(9) 0.3741(5) 0.7377(7) 0.0296(17) Uani 1 1 d U . . N5 N 0.5510(9) 0.4121(5) 0.2694(8) 0.0317(16) Uani 1 1 d U . . N6 N 0.3800(9) 0.4512(5) 0.3578(8) 0.0308(16) Uani 1 1 d U . . N7 N 0.9497(9) 0.1877(5) 0.3152(8) 0.0298(17) Uani 1 1 d U . . N8 N 1.1436(10) 0.1278(5) 0.3014(8) 0.0309(18) Uani 1 1 d U . . N9 N 0.6655(9) 0.1660(5) 0.1283(8) 0.0330(17) Uani 1 1 d U . . N11 N 0.7852(9) 0.5124(5) 0.2629(8) 0.0301(17) Uani 1 1 d U . . N12 N 0.7729(10) 0.6269(5) 0.2255(9) 0.0367(18) Uani 1 1 d U . . C1 C 0.6192(11) 0.3800(7) 0.7382(9) 0.0371(18) Uani 1 1 d U . . H1A H 0.6850 0.4021 0.8054 0.045 Uiso 1 1 calc R . . C2 C 0.4166(11) 0.3993(7) 0.8386(9) 0.035(2) Uani 1 1 d U . . H2 H 0.4743 0.4148 0.9177 0.042 Uiso 1 1 calc R . . C3 C 0.4181(11) 0.3392(7) 0.6226(8) 0.0313(17) Uani 1 1 d U . . H3A H 0.3234 0.3265 0.5941 0.038 Uiso 1 1 calc R . . C4 C 0.5252(11) 0.3278(6) 0.5613(9) 0.0316(16) Uani 1 1 d U . . H4A H 0.5131 0.3064 0.4787 0.038 Uiso 1 1 calc R . . C5 C 0.8385(12) 0.5487(7) 0.3815(11) 0.0366(19) Uani 1 1 d U . . H5A H 0.8742 0.5276 0.4633 0.044 Uiso 1 1 calc R . . C6 C 1.0020(12) 0.1255(7) 0.3033(9) 0.0327(18) Uani 1 1 d U . . H6A H 0.9496 0.0837 0.2967 0.039 Uiso 1 1 calc R . . C8 C 1.0592(11) 0.2345(6) 0.3175(9) 0.031(2) Uani 1 1 d U . . H8A H 1.0534 0.2836 0.3250 0.037 Uiso 1 1 calc R . . C9 C 1.1761(12) 0.1984(7) 0.3073(8) 0.032(2) Uani 1 1 d U . . H9A H 1.2634 0.2181 0.3047 0.039 Uiso 1 1 calc R . . C11 C 0.5213(11) 0.4527(6) 0.3622(10) 0.0312(16) Uani 1 1 d U . . H11A H 0.5876 0.4789 0.4226 0.037 Uiso 1 1 calc R . . C13 C 0.4274(11) 0.3855(7) 0.2013(9) 0.0333(19) Uani 1 1 d U . . H13A H 0.4177 0.3555 0.1285 0.040 Uiso 1 1 calc R . . C14 C 0.3211(12) 0.4078(7) 0.2520(9) 0.0350(19) Uani 1 1 d U . . H14A H 0.2258 0.3965 0.2224 0.042 Uiso 1 1 calc R . . C15 C 0.5783(11) 0.1817(6) -0.2240(10) 0.035(2) Uani 1 1 d U . . H15 H 0.5944 0.2295 -0.2384 0.041 Uiso 1 1 calc R . . C16 C 0.8999(12) 0.1990(8) 0.7424(11) 0.048(2) Uani 1 1 d U . . H16A H 0.8829 0.1765 0.6605 0.058 Uiso 1 1 calc R . . C17 C 0.6409(11) 0.0965(6) 0.0894(10) 0.0323(18) Uani 1 1 d U . . H17A H 0.6482 0.0580 0.1468 0.039 Uiso 1 1 calc R . . C20 C 0.6428(10) 0.2020(7) 0.0166(9) 0.0310(18) Uani 1 1 d U . . H20A H 0.6518 0.2510 0.0118 0.037 Uiso 1 1 calc R . . C21 C 0.9321(13) 0.0798(8) 0.8633(12) 0.054(2) Uani 1 1 d U . . H21 H 0.9084 0.0546 0.7842 0.064 Uiso 1 1 calc R . . C22 C 0.6057(11) 0.0919(6) -0.0403(10) 0.034(2) Uani 1 1 d U . . H22A H 0.5850 0.0502 -0.0888 0.041 Uiso 1 1 calc R . . C24 C 0.9688(15) 0.0474(10) 0.9669(14) 0.085(4) Uani 1 1 d U . . H24A H 0.9927 0.0720 1.0467 0.102 Uiso 1 1 calc R . . H24B H 0.9730 -0.0020 0.9664 0.102 Uiso 1 1 calc R . . N10 N 0.6045(10) 0.1586(5) -0.0918(8) 0.0334(18) Uani 1 1 d U . . C26 C 0.9332(13) 0.2810(8) 0.8921(11) 0.051(2) Uani 1 1 d U . . H26A H 0.9433 0.3243 0.9364 0.061 Uiso 1 1 calc R . . C27 C 0.7513(11) 0.6935(7) 0.1594(11) 0.044(2) Uani 1 1 d U . . H27 H 0.7686 0.7344 0.2107 0.053 Uiso 1 1 calc R . . C28 C 0.9443(12) 0.2128(9) 0.9459(11) 0.052(2) Uani 1 1 d U . . H28A H 0.9649 0.2043 1.0366 0.062 Uiso 1 1 calc R . . C29 C 0.5342(13) 0.1429(7) -0.3260(11) 0.051(3) Uani 1 1 d U . . H29A H 0.5168 0.0949 -0.3161 0.061 Uiso 1 1 calc R . . H29B H 0.5197 0.1627 -0.4102 0.061 Uiso 1 1 calc R . . C30 C 1.2276(13) 0.0700(7) 0.2881(10) 0.038(2) Uani 1 1 d U . . H30 H 1.1843 0.0256 0.2783 0.045 Uiso 1 1 calc R . . C7 C 1.3617(13) 0.0725(7) 0.2882(10) 0.050(3) Uani 1 1 d U . . H7A H 1.4090 0.1158 0.2977 0.060 Uiso 1 1 calc R . . H7B H 1.4103 0.0309 0.2786 0.060 Uiso 1 1 calc R . . C32 C 0.7104(12) 0.7006(8) 0.0363(11) 0.052(3) Uani 1 1 d U . . H32A H 0.6922 0.6607 -0.0178 0.062 Uiso 1 1 calc R . . H32B H 0.6983 0.7458 -0.0008 0.062 Uiso 1 1 calc R . . C23 C 0.3134(11) 0.4880(6) 0.4485(9) 0.0321(17) Uani 1 1 d U . . H23 H 0.3641 0.5241 0.4995 0.039 Uiso 1 1 calc R . . C19 C 0.7470(11) 0.5621(6) 0.1704(11) 0.0346(19) Uani 1 1 d U . . H19A H 0.7083 0.5533 0.0813 0.042 Uiso 1 1 calc R . . C18 C 0.8298(12) 0.6190(7) 0.3580(11) 0.037(2) Uani 1 1 d U . . H18A H 0.8570 0.6551 0.4197 0.045 Uiso 1 1 calc R . . C12 C 0.1884(12) 0.4745(7) 0.4638(11) 0.043(3) Uani 1 1 d U . . H12A H 0.1350 0.4387 0.4143 0.051 Uiso 1 1 calc R . . H12B H 0.1512 0.5004 0.5244 0.051 Uiso 1 1 calc R . . C10 C 0.2791(12) 0.4018(7) 0.8261(10) 0.047(3) Uani 1 1 d U . . H10A H 0.2189 0.3866 0.7480 0.056 Uiso 1 1 calc R . . H10B H 0.2417 0.4188 0.8953 0.056 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 0.0242(6) 0.0253(6) 0.0245(5) 0.0005(5) 0.0039(4) -0.0020(6) Mo2 0.0266(6) 0.0266(6) 0.0286(5) -0.0006(5) 0.0078(4) -0.0016(6) Mo3 0.0228(6) 0.0381(7) 0.0242(4) -0.0020(5) 0.0026(4) 0.0009(6) O1 0.024(4) 0.040(6) 0.043(4) -0.006(4) 0.010(3) -0.001(4) O2 0.027(4) 0.031(5) 0.024(4) 0.003(4) 0.003(3) -0.010(5) O3 0.024(4) 0.044(6) 0.049(4) 0.002(4) 0.015(4) -0.002(5) O4 0.024(4) 0.045(6) 0.037(4) -0.008(4) 0.001(3) 0.006(4) O5 0.049(5) 0.031(5) 0.043(4) 0.011(4) 0.017(4) 0.002(5) O6 0.043(5) 0.051(7) 0.031(4) -0.020(4) 0.000(4) 0.004(5) O7 0.035(5) 0.066(7) 0.014(3) -0.009(4) -0.001(3) -0.004(5) O8 0.027(4) 0.028(5) 0.036(4) 0.002(3) 0.011(3) 0.001(4) O9 0.024(4) 0.031(5) 0.028(4) -0.003(3) 0.011(3) -0.001(4) N1 0.028(3) 0.060(4) 0.040(3) 0.008(3) 0.009(3) 0.004(4) N2 0.036(4) 0.072(5) 0.053(4) 0.015(4) 0.013(4) 0.006(4) N3 0.025(3) 0.036(3) 0.030(3) 0.003(3) 0.008(3) 0.000(3) N4 0.027(3) 0.034(4) 0.027(3) 0.001(3) 0.005(3) 0.006(3) N5 0.027(3) 0.031(3) 0.035(3) -0.001(3) 0.003(3) 0.002(3) N6 0.026(3) 0.030(3) 0.037(3) 0.000(3) 0.008(3) 0.003(3) N7 0.031(3) 0.028(4) 0.031(3) -0.003(3) 0.009(3) 0.000(3) N8 0.033(4) 0.027(4) 0.035(3) 0.007(3) 0.012(3) 0.000(4) N9 0.030(3) 0.034(4) 0.035(3) -0.004(3) 0.007(3) -0.002(3) N11 0.025(3) 0.027(3) 0.039(3) 0.004(3) 0.008(3) -0.005(3) N12 0.028(4) 0.033(4) 0.050(4) 0.005(4) 0.010(3) -0.002(4) C1 0.031(3) 0.042(4) 0.036(3) 0.004(3) 0.004(3) 0.004(4) C2 0.029(4) 0.039(4) 0.036(3) -0.001(4) 0.002(3) 0.004(4) C3 0.026(3) 0.035(3) 0.031(3) 0.001(3) 0.003(3) 0.001(3) C4 0.029(3) 0.034(3) 0.031(3) -0.001(3) 0.003(3) 0.004(3) C5 0.027(4) 0.036(4) 0.046(3) 0.000(3) 0.006(3) -0.006(4) C6 0.033(4) 0.034(4) 0.033(3) 0.002(3) 0.010(3) -0.001(4) C8 0.037(4) 0.026(4) 0.029(3) -0.001(4) 0.009(4) 0.004(4) C9 0.037(4) 0.032(4) 0.032(3) 0.003(4) 0.014(3) -0.003(4) C11 0.027(3) 0.031(3) 0.036(3) -0.002(3) 0.007(3) -0.003(3) C13 0.028(4) 0.035(4) 0.035(3) -0.002(3) 0.004(3) 0.001(4) C14 0.031(4) 0.033(4) 0.039(3) -0.001(3) 0.004(3) -0.001(4) C15 0.034(4) 0.036(4) 0.035(4) 0.000(4) 0.009(4) -0.005(4) C16 0.036(4) 0.067(5) 0.043(4) 0.012(4) 0.009(3) 0.002(4) C17 0.030(4) 0.032(4) 0.036(3) -0.003(3) 0.010(3) -0.004(4) C20 0.030(4) 0.032(4) 0.034(3) -0.001(4) 0.013(3) -0.002(4) C21 0.038(4) 0.069(5) 0.053(4) 0.012(4) 0.010(4) 0.002(4) C22 0.033(4) 0.033(4) 0.035(4) -0.008(4) 0.005(3) -0.001(4) C24 0.072(7) 0.099(9) 0.083(7) 0.009(7) 0.017(7) 0.011(8) N10 0.033(4) 0.034(4) 0.033(3) -0.002(3) 0.008(3) -0.004(4) C26 0.036(4) 0.066(4) 0.050(4) 0.007(4) 0.010(3) 0.006(4) C27 0.034(4) 0.039(4) 0.060(4) 0.004(4) 0.010(4) -0.003(4) C28 0.036(4) 0.073(5) 0.048(4) 0.016(4) 0.013(4) 0.004(5) C29 0.058(7) 0.041(7) 0.050(6) -0.009(6) 0.006(6) -0.005(6) C30 0.038(4) 0.033(4) 0.044(4) 0.001(4) 0.012(4) -0.002(4) C7 0.045(7) 0.041(7) 0.065(6) -0.003(6) 0.014(6) -0.003(6) C32 0.050(5) 0.039(6) 0.064(5) 0.011(5) 0.007(5) 0.005(5) C23 0.027(3) 0.032(4) 0.036(3) -0.003(3) 0.004(3) 0.002(3) C19 0.025(4) 0.034(4) 0.047(4) 0.001(4) 0.012(3) -0.003(4) C18 0.027(4) 0.035(4) 0.048(4) -0.001(4) 0.007(4) -0.003(4) C12 0.037(6) 0.036(6) 0.056(6) -0.014(5) 0.012(5) -0.008(6) C10 0.036(6) 0.052(7) 0.050(5) 0.002(6) 0.005(5) -0.001(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 O7 1.709(6) . ? Mo1 O3 1.733(7) . ? Mo1 O8 1.807(8) . ? Mo1 O2 2.133(5) . ? Mo1 N11 2.285(10) . ? Mo1 N5 2.422(9) . ? Mo2 O1 1.727(7) . ? Mo2 O5 1.727(8) . ? Mo2 O9 1.814(6) . ? Mo2 O8 2.109(8) . ? Mo2 N9 2.273(8) . ? Mo2 N7 2.431(9) . ? Mo3 O4 1.715(7) . ? Mo3 O6 1.722(7) . ? Mo3 O2 1.787(6) . ? Mo3 O9 2.097(7) . ? Mo3 N1 2.305(10) . ? Mo3 N3 2.429(8) . ? N1 C16 1.322(16) . ? N1 C26 1.389(14) . ? N2 C28 1.279(17) . ? N2 C16 1.369(13) . ? N2 C21 1.566(18) . ? N3 C1 1.326(12) . ? N3 C4 1.352(12) . ? N4 C1 1.326(13) . ? N4 C3 1.383(12) . ? N4 C2 1.424(12) . ? N5 C11 1.310(12) . ? N5 C13 1.344(12) . ? N6 C11 1.360(13) . ? N6 C14 1.384(13) . ? N6 C23 1.432(12) . ? N7 C6 1.293(13) . ? N7 C8 1.375(13) . ? N8 C9 1.365(14) . ? N8 C6 1.378(13) . ? N8 C30 1.383(14) . ? N9 C20 1.316(13) . ? N9 C17 1.376(14) . ? N11 C19 1.331(13) . ? N11 C5 1.400(13) . ? N12 C19 1.347(14) . ? N12 C18 1.368(13) . ? N12 C27 1.420(14) . ? C1 H1A 0.9300 . ? C2 C10 1.310(14) . ? C2 H2 0.9300 . ? C3 C4 1.349(13) . ? C3 H3A 0.9300 . ? C4 H4A 0.9300 . ? C5 C18 1.344(16) . ? C5 H5A 0.9300 . ? C6 H6A 0.9300 . ? C8 C9 1.345(14) . ? C8 H8A 0.9300 . ? C9 H9A 0.9300 . ? C11 H11A 0.9300 . ? C13 C14 1.325(14) . ? C13 H13A 0.9300 . ? C14 H14A 0.9300 . ? C15 C29 1.278(14) . ? C15 N10 1.405(12) . ? C15 H15 0.9300 . ? C16 H16A 0.9300 . ? C17 C22 1.313(12) . ? C17 H17A 0.9300 . ? C20 N10 1.370(13) . ? C20 H20A 0.9300 . ? C21 C24 1.217(16) . ? C21 H21 0.9300 . ? C22 N10 1.364(14) . ? C22 H22A 0.9300 . ? C24 H24A 0.9300 . ? C24 H24B 0.9300 . ? C26 C28 1.394(19) . ? C26 H26A 0.9300 . ? C27 C32 1.256(13) . ? C27 H27 0.9300 . ? C28 H28A 0.9300 . ? C29 H29A 0.9300 . ? C29 H29B 0.9300 . ? C30 C7 1.300(14) . ? C30 H30 0.9300 . ? C7 H7A 0.9300 . ? C7 H7B 0.9300 . ? C32 H32A 0.9300 . ? C32 H32B 0.9300 . ? C23 C12 1.282(14) . ? C23 H23 0.9300 . ? C19 H19A 0.9300 . ? C18 H18A 0.9300 . ? C12 H12A 0.9300 . ? C12 H12B 0.9300 . ? C10 H10A 0.9300 . ? C10 H10B 0.9300 . ? 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 O7 Mo1 O3 103.0(3) . . ? O7 Mo1 O8 103.2(4) . . ? O3 Mo1 O8 103.5(4) . . ? O7 Mo1 O2 155.4(3) . . ? O3 Mo1 O2 93.7(3) . . ? O8 Mo1 O2 90.0(3) . . ? O7 Mo1 N11 84.4(3) . . ? O3 Mo1 N11 89.1(4) . . ? O8 Mo1 N11 163.2(3) . . ? O2 Mo1 N11 77.9(3) . . ? O7 Mo1 N5 83.8(3) . . ? O3 Mo1 N5 164.8(3) . . ? O8 Mo1 N5 87.8(3) . . ? O2 Mo1 N5 76.0(3) . . ? N11 Mo1 N5 78.0(3) . . ? O1 Mo2 O5 103.1(4) . . ? O1 Mo2 O9 103.7(3) . . ? O5 Mo2 O9 105.2(3) . . ? O1 Mo2 O8 94.6(3) . . ? O5 Mo2 O8 153.8(3) . . ? O9 Mo2 O8 88.9(3) . . ? O1 Mo2 N9 87.7(3) . . ? O5 Mo2 N9 83.8(4) . . ? O9 Mo2 N9 163.2(3) . . ? O8 Mo2 N9 77.7(3) . . ? O1 Mo2 N7 166.3(3) . . ? O5 Mo2 N7 81.0(3) . . ? O9 Mo2 N7 87.6(3) . . ? O8 Mo2 N7 77.6(3) . . ? N9 Mo2 N7 79.7(3) . . ? O4 Mo3 O6 102.7(4) . . ? O4 Mo3 O2 103.9(3) . . ? O6 Mo3 O2 104.6(4) . . ? O4 Mo3 O9 94.5(3) . . ? O6 Mo3 O9 154.8(3) . . ? O2 Mo3 O9 88.6(3) . . ? O4 Mo3 N1 87.1(3) . . ? O6 Mo3 N1 85.0(4) . . ? O2 Mo3 N1 163.0(3) . . ? O9 Mo3 N1 77.5(3) . . ? O4 Mo3 N3 162.2(4) . . ? O6 Mo3 N3 82.5(3) . . ? O2 Mo3 N3 90.9(3) . . ? O9 Mo3 N3 75.8(3) . . ? N1 Mo3 N3 76.3(3) . . ? Mo3 O2 Mo1 145.0(5) . . ? Mo1 O8 Mo2 148.2(4) . . ? Mo2 O9 Mo3 150.1(4) . . ? C16 N1 C26 105.6(10) . . ? C16 N1 Mo3 124.3(8) . . ? C26 N1 Mo3 129.7(9) . . ? C28 N2 C16 102.9(13) . . ? C28 N2 C21 136.0(11) . . ? C16 N2 C21 120.9(12) . . ? C1 N3 C4 103.2(8) . . ? C1 N3 Mo3 125.8(7) . . ? C4 N3 Mo3 130.9(6) . . ? C1 N4 C3 107.5(8) . . ? C1 N4 C2 125.6(9) . . ? C3 N4 C2 126.9(8) . . ? C11 N5 C13 106.7(9) . . ? C11 N5 Mo1 126.6(7) . . ? C13 N5 Mo1 126.7(7) . . ? C11 N6 C14 105.7(9) . . ? C11 N6 C23 124.5(9) . . ? C14 N6 C23 129.7(9) . . ? C6 N7 C8 105.4(9) . . ? C6 N7 Mo2 124.6(8) . . ? C8 N7 Mo2 130.0(7) . . ? C9 N8 C6 104.5(10) . . ? C9 N8 C30 129.5(10) . . ? C6 N8 C30 125.9(11) . . ? C20 N9 C17 104.3(9) . . ? C20 N9 Mo2 127.9(9) . . ? C17 N9 Mo2 127.4(7) . . ? C19 N11 C5 106.1(10) . . ? C19 N11 Mo1 125.0(7) . . ? C5 N11 Mo1 128.6(7) . . ? C19 N12 C18 108.7(10) . . ? C19 N12 C27 127.0(10) . . ? C18 N12 C27 124.3(10) . . ? N4 C1 N3 112.7(10) . . ? N4 C1 H1A 123.7 . . ? N3 C1 H1A 123.7 . . ? C10 C2 N4 123.7(10) . . ? C10 C2 H2 118.2 . . ? N4 C2 H2 118.2 . . ? C4 C3 N4 103.6(9) . . ? C4 C3 H3A 128.2 . . ? N4 C3 H3A 128.2 . . ? C3 C4 N3 113.1(9) . . ? C3 C4 H4A 123.5 . . ? N3 C4 H4A 123.5 . . ? C18 C5 N11 109.0(10) . . ? C18 C5 H5A 125.5 . . ? N11 C5 H5A 125.5 . . ? N7 C6 N8 112.7(11) . . ? N7 C6 H6A 123.7 . . ? N8 C6 H6A 123.7 . . ? C9 C8 N7 109.5(10) . . ? C9 C8 H8A 125.2 . . ? N7 C8 H8A 125.2 . . ? C8 C9 N8 107.9(10) . . ? C8 C9 H9A 126.1 . . ? N8 C9 H9A 126.1 . . ? N5 C11 N6 110.4(10) . . ? N5 C11 H11A 124.8 . . ? N6 C11 H11A 124.8 . . ? C14 C13 N5 110.7(10) . . ? C14 C13 H13A 124.7 . . ? N5 C13 H13A 124.7 . . ? C13 C14 N6 106.5(10) . . ? C13 C14 H14A 126.8 . . ? N6 C14 H14A 126.8 . . ? C29 C15 N10 125.7(12) . . ? C29 C15 H15 117.1 . . ? N10 C15 H15 117.1 . . ? N1 C16 N2 113.6(12) . . ? N1 C16 H16A 123.2 . . ? N2 C16 H16A 123.2 . . ? C22 C17 N9 110.5(10) . . ? C22 C17 H17A 124.7 . . ? N9 C17 H17A 124.7 . . ? N9 C20 N10 112.1(12) . . ? N9 C20 H20A 123.9 . . ? N10 C20 H20A 123.9 . . ? C24 C21 N2 121.5(15) . . ? C24 C21 H21 119.2 . . ? N2 C21 H21 119.2 . . ? C17 C22 N10 108.6(10) . . ? C17 C22 H22A 125.7 . . ? N10 C22 H22A 125.7 . . ? C21 C24 H24A 120.0 . . ? C21 C24 H24B 120.0 . . ? H24A C24 H24B 120.0 . . ? C22 N10 C20 104.5(9) . . ? C22 N10 C15 130.6(10) . . ? C20 N10 C15 124.9(11) . . ? N1 C26 C28 103.5(12) . . ? N1 C26 H26A 128.3 . . ? C28 C26 H26A 128.3 . . ? C32 C27 N12 124.3(13) . . ? C32 C27 H27 117.9 . . ? N12 C27 H27 117.9 . . ? N2 C28 C26 114.3(11) . . ? N2 C28 H28A 122.8 . . ? C26 C28 H28A 122.8 . . ? C15 C29 H29A 120.0 . . ? C15 C29 H29B 120.0 . . ? H29A C29 H29B 120.0 . . ? C7 C30 N8 125.6(13) . . ? C7 C30 H30 117.2 . . ? N8 C30 H30 117.2 . . ? C30 C7 H7A 120.0 . . ? C30 C7 H7B 120.0 . . ? H7A C7 H7B 120.0 . . ? C27 C32 H32A 120.0 . . ? C27 C32 H32B 120.0 . . ? H32A C32 H32B 120.0 . . ? C12 C23 N6 124.2(11) . . ? C12 C23 H23 117.9 . . ? N6 C23 H23 117.9 . . ? N11 C19 N12 109.7(10) . . ? N11 C19 H19A 125.2 . . ? N12 C19 H19A 125.2 . . ? C5 C18 N12 106.5(11) . . ? C5 C18 H18A 126.7 . . ? N12 C18 H18A 126.7 . . ? C23 C12 H12A 120.0 . . ? C23 C12 H12B 120.0 . . ? H12A C12 H12B 120.0 . . ? C2 C10 H10A 120.0 . . ? C2 C10 H10B 120.0 . . ? H10A C10 H10B 120.0 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C30 H30 O6 0.93 2.39 3.309(15) 170.1 2_746 C23 H23 O5 0.93 2.45 3.121(13) 129.1 2_656 C14 H14A O3 0.93 2.57 3.440(13) 156.9 1_455 C12 H12A O3 0.93 2.44 3.291(13) 151.7 1_455 C10 H10A O4 0.93 2.46 3.371(14) 166.1 1_455 C9 H9A O1 0.93 2.56 3.450(13) 159.5 1_655 C7 H7A O1 0.93 2.37 3.298(16) 177.9 1_655 C3 H3A O4 0.93 2.59 3.482(13) 161.1 1_455 C2 H2 O7 0.93 2.37 3.205(12) 149.1 1_556 C20 H20A O8 0.93 2.40 2.858(13) 110.0 . C19 H19A O7 0.93 2.59 2.951(14) 103.7 . C16 H16A O9 0.93 2.37 2.837(13) 110.5 . C8 H8A O3 0.93 2.48 3.300(14) 147.7 . C5 H5A O2 0.93 2.51 2.920(14) 106.6 . C4 H4A O1 0.93 2.32 3.213(12) 161.6 . _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.712 _refine_diff_density_min -0.650 _refine_diff_density_rms 0.140 _database_code_depnum_ccdc_archive 'CCDC 940197'