Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2010 data_added_by_encifer _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _data_manuscript_title ; 'Mo2O42+ Organometallic clusters from allylmolybdenum(II) complexes' ; _audit_creation_method SHELXL _pub_requested_journal 'Dalton Trans.' _publ_contact_author ; FERNANDO VILLAFA\~NE IU CINQUIMA/Quimica Inorganica Facultad de Ciencias Universidad de Valladolid C/ Prado de la Magdalena s/n 47005 Valladolid SPAIN ; _publ_contact_author_phone +34-983-184620 _publ_contact_author_fax +34-983-423013 _publ_contact_author_email fervilla@qi.uva.es loop_ _publ_author_name _publ_author_address 'Paloma Paredes' ; IU CINQUIMA/Quimica Inorganica Facultad de Ciencias Universidad de Valladolid C/ Prado de la Magdalena s/n 47005 Valladolid SPAIN ; 'Angel Lopez-Calzada' ; IU CINQUIMA/Quimica Inorganica Facultad de Ciencias Universidad de Valladolid C/ Prado de la Magdalena s/n 47005 Valladolid SPAIN ; 'Daniel Miguel' ; IU CINQUIMA/Quimica Inorganica Facultad de Ciencias Universidad de Valladolid C/ Prado de la Magdalena s/n 47005 Valladolid SPAIN ; F.Villafane ; IU CINQUIMA/Quimica Inorganica Facultad de Ciencias Universidad de Valladolid C/ Prado de la Magdalena s/n 47005 Valladolid SPAIN ; _publ_contact_author_name 'FERNANDO VILLAFANE' #-------------------------- data section of block --------------------------- data_Compound_1b_pp60bm _database_code_depnum_ccdc_archive 'CCDC 791636' #TrackingRef 'dt-art-05-2010-000570-File002_v1_0.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H24 Mo N4 O4' _chemical_formula_weight 444.34 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 Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 8.6642(6) _cell_length_b 19.3916(13) _cell_length_c 24.0284(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4037.1(5) _cell_formula_units_Z 8 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 867 _cell_measurement_theta_min 2.265 _cell_measurement_theta_max 23.262 _exptl_crystal_description PLATE _exptl_crystal_colour YELLOW _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.462 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1824 _exptl_absorpt_coefficient_mu 0.677 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.832586 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17090 _diffrn_reflns_av_R_equivalents 0.0507 _diffrn_reflns_av_sigmaI/netI 0.0355 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 23.27 _reflns_number_total 2910 _reflns_number_gt 2170 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0440P)^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_number_reflns 2910 _refine_ls_number_parameters 240 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0523 _refine_ls_R_factor_gt 0.0330 _refine_ls_wR_factor_ref 0.0786 _refine_ls_wR_factor_gt 0.0730 _refine_ls_goodness_of_fit_ref 0.970 _refine_ls_restrained_S_all 0.970 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 1.05893(3) 0.651875(15) 0.087379(13) 0.03070(13) Uani 1 1 d . . . N1 N 0.9483(3) 0.75486(15) 0.10855(13) 0.0359(8) Uani 1 1 d . . . N2 N 0.7933(3) 0.75501(14) 0.12006(13) 0.0332(8) Uani 1 1 d . . . H2 H 0.7361 0.7188 0.1190 0.040 Uiso 1 1 calc R . . N3 N 1.0373(4) 0.63527(16) 0.17966(14) 0.0420(8) Uani 1 1 d . . . N4 N 0.9602(4) 0.57844(18) 0.19722(15) 0.0524(9) Uani 1 1 d . . . H4 H 0.9100 0.5512 0.1756 0.063 Uiso 1 1 calc R . . C1 C 1.1528(5) 0.5609(2) 0.08597(17) 0.0398(10) Uani 1 1 d . . . O1 O 1.2151(4) 0.50818(15) 0.08549(14) 0.0670(9) Uani 1 1 d . . . C2 C 1.2752(5) 0.6751(2) 0.09361(17) 0.0433(10) Uani 1 1 d . . . O2 O 1.4073(3) 0.68519(17) 0.09679(14) 0.0636(9) Uani 1 1 d . . . C3 C 1.1359(5) 0.7137(2) 0.00887(17) 0.0527(12) Uani 1 1 d . . . H3A H 1.1177 0.7631 0.0092 0.063 Uiso 1 1 calc R . . H3B H 1.2328 0.7004 -0.0083 0.063 Uiso 1 1 calc R . . C4 C 1.0087(5) 0.6713(2) -0.00096(17) 0.0443(10) Uani 1 1 d . . . H4A H 0.9092 0.6899 -0.0133 0.053 Uiso 1 1 calc R . . C5 C 1.0382(5) 0.5999(2) 0.00070(17) 0.0513(11) Uani 1 1 d . . . H5A H 1.1331 0.5840 -0.0165 0.062 Uiso 1 1 calc R . . H5B H 0.9509 0.5694 -0.0051 0.062 Uiso 1 1 calc R . . O6 O 0.8107(3) 0.62195(13) 0.08841(11) 0.0410(6) Uani 1 1 d . . . C6 C 0.7513(4) 0.5614(2) 0.0882(2) 0.0488(11) Uani 1 1 d . . . O7 O 0.8035(4) 0.51253(16) 0.11565(16) 0.0787(11) Uani 1 1 d . . . C7 C 0.6134(5) 0.5507(2) 0.0519(2) 0.0686(15) Uani 1 1 d . . . H7A H 0.6457 0.5475 0.0138 0.103 Uiso 1 1 calc R . . H7B H 0.5439 0.5890 0.0561 0.103 Uiso 1 1 calc R . . H7C H 0.5619 0.5089 0.0625 0.103 Uiso 1 1 calc R . . C11 C 0.7408(4) 0.8183(2) 0.13321(16) 0.0376(10) Uani 1 1 d . . . C12 C 0.8643(5) 0.8609(2) 0.13107(18) 0.0486(11) Uani 1 1 d . . . H12 H 0.8646 0.9081 0.1382 0.058 Uiso 1 1 calc R . . C13 C 0.9915(5) 0.8205(2) 0.11612(19) 0.0440(11) Uani 1 1 d . . . C14 C 0.5747(4) 0.8322(2) 0.14628(19) 0.0555(12) Uani 1 1 d . . . H14A H 0.5633 0.8399 0.1855 0.083 Uiso 1 1 calc R . . H14B H 0.5133 0.7933 0.1353 0.083 Uiso 1 1 calc R . . H14C H 0.5411 0.8724 0.1263 0.083 Uiso 1 1 calc R . . C15 C 1.1547(5) 0.8442(2) 0.1079(2) 0.0679(15) Uani 1 1 d . . . H15A H 1.2179 0.8057 0.0975 0.102 Uiso 1 1 calc R . . H15B H 1.1928 0.8637 0.1420 0.102 Uiso 1 1 calc R . . H15C H 1.1579 0.8784 0.0791 0.102 Uiso 1 1 calc R . . C21 C 1.1005(5) 0.6623(2) 0.22585(18) 0.0528(12) Uani 1 1 d . . . C22 C 1.0601(6) 0.6225(3) 0.2715(2) 0.0709(15) Uani 1 1 d . . . H22 H 1.0883 0.6305 0.3082 0.085 Uiso 1 1 calc R . . C23 C 0.9718(5) 0.5698(3) 0.2525(2) 0.0638(14) Uani 1 1 d . . . C24 C 1.1957(6) 0.7263(2) 0.2246(2) 0.0745(15) Uani 1 1 d . . . H24A H 1.2646 0.7246 0.1933 0.112 Uiso 1 1 calc R . . H24B H 1.2545 0.7296 0.2583 0.112 Uiso 1 1 calc R . . H24C H 1.1294 0.7657 0.2213 0.112 Uiso 1 1 calc R . . C25 C 0.8933(7) 0.5097(3) 0.2800(3) 0.105(2) Uani 1 1 d . . . H25A H 0.8357 0.4843 0.2528 0.158 Uiso 1 1 calc R . . H25B H 0.8245 0.5262 0.3084 0.158 Uiso 1 1 calc R . . H25C H 0.9695 0.4801 0.2965 0.158 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 0.03468(19) 0.02678(19) 0.0307(2) -0.00180(15) 0.00101(16) 0.00098(15) N1 0.0319(17) 0.0308(18) 0.045(2) -0.0015(14) 0.0017(15) 0.0001(14) N2 0.0325(18) 0.0296(18) 0.037(2) -0.0039(14) 0.0013(15) -0.0021(14) N3 0.043(2) 0.047(2) 0.036(2) 0.0020(16) 0.0011(17) 0.0042(16) N4 0.051(2) 0.061(2) 0.045(2) 0.0124(18) 0.0020(19) 0.0020(19) C1 0.044(2) 0.034(2) 0.042(3) -0.003(2) -0.003(2) -0.0003(19) O1 0.078(2) 0.0421(18) 0.081(3) -0.0045(17) -0.0070(19) 0.0203(17) C2 0.052(3) 0.037(2) 0.041(3) -0.0078(19) 0.004(2) 0.0077(19) O2 0.0327(18) 0.069(2) 0.089(3) -0.0106(18) 0.0005(16) -0.0027(15) C3 0.067(3) 0.052(3) 0.039(3) 0.007(2) 0.017(2) -0.003(2) C4 0.051(2) 0.050(3) 0.032(3) 0.0073(19) -0.003(2) 0.005(2) C5 0.062(3) 0.053(3) 0.039(3) -0.013(2) 0.003(2) -0.001(2) O6 0.0344(14) 0.0317(14) 0.0568(19) -0.0036(13) 0.0017(13) -0.0069(12) C6 0.039(2) 0.048(3) 0.059(3) -0.010(3) 0.006(2) -0.007(2) O7 0.098(3) 0.041(2) 0.097(3) 0.0117(19) -0.023(2) -0.0214(19) C7 0.051(3) 0.068(3) 0.087(4) -0.024(3) 0.001(3) -0.013(2) C11 0.041(2) 0.037(2) 0.034(3) -0.0015(18) -0.0038(19) 0.0074(19) C12 0.049(2) 0.030(2) 0.067(3) -0.007(2) -0.007(2) 0.0058(19) C13 0.043(2) 0.028(2) 0.061(3) -0.003(2) 0.002(2) -0.0014(19) C14 0.047(2) 0.061(3) 0.059(3) -0.010(2) 0.005(2) 0.012(2) C15 0.051(3) 0.041(3) 0.112(4) -0.012(3) 0.008(3) -0.012(2) C21 0.054(3) 0.069(3) 0.035(3) -0.007(2) -0.002(2) 0.020(2) C22 0.075(3) 0.103(4) 0.035(3) -0.003(3) -0.007(3) 0.023(3) C23 0.058(3) 0.091(4) 0.042(3) 0.029(3) 0.014(3) 0.026(3) C24 0.084(4) 0.079(4) 0.060(4) -0.027(3) -0.017(3) 0.003(3) C25 0.103(5) 0.125(5) 0.088(5) 0.066(4) 0.025(4) 0.012(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 C2 1.933(4) . ? Mo1 C1 1.943(4) . ? Mo1 C4 2.199(4) . ? Mo1 O6 2.228(2) . ? Mo1 N3 2.248(3) . ? Mo1 N1 2.273(3) . ? Mo1 C5 2.321(4) . ? Mo1 C3 2.333(4) . ? N1 C13 1.340(5) . ? N1 N2 1.371(4) . ? N2 C11 1.346(4) . ? N3 C21 1.344(5) . ? N3 N4 1.356(4) . ? N4 C23 1.343(5) . ? C1 O1 1.156(4) . ? C2 O2 1.164(4) . ? C3 C4 1.396(5) . ? C4 C5 1.409(6) . ? O6 C6 1.282(5) . ? C6 O7 1.240(5) . ? C6 C7 1.495(6) . ? C11 C12 1.353(5) . ? C11 C14 1.497(5) . ? C12 C13 1.399(6) . ? C13 C15 1.500(6) . ? C21 C22 1.385(6) . ? C21 C24 1.490(6) . ? C22 C23 1.355(7) . ? C23 C25 1.504(7) . ? 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 C2 Mo1 C1 78.88(16) . . ? C2 Mo1 C4 103.10(16) . . ? C1 Mo1 C4 102.80(16) . . ? C2 Mo1 O6 174.68(14) . . ? C1 Mo1 O6 99.66(13) . . ? C4 Mo1 O6 82.20(13) . . ? C2 Mo1 N3 92.17(15) . . ? C1 Mo1 N3 85.53(14) . . ? C4 Mo1 N3 163.70(14) . . ? O6 Mo1 N3 82.60(11) . . ? C2 Mo1 N1 100.76(13) . . ? C1 Mo1 N1 168.03(14) . . ? C4 Mo1 N1 88.98(13) . . ? O6 Mo1 N1 79.59(9) . . ? N3 Mo1 N1 82.52(11) . . ? C2 Mo1 C5 104.23(16) . . ? C1 Mo1 C5 67.81(16) . . ? C4 Mo1 C5 36.20(14) . . ? O6 Mo1 C5 79.75(13) . . ? N3 Mo1 C5 144.71(14) . . ? N1 Mo1 C5 123.37(13) . . ? C2 Mo1 C3 70.47(17) . . ? C1 Mo1 C3 109.45(16) . . ? C4 Mo1 C3 35.72(14) . . ? O6 Mo1 C3 114.77(13) . . ? N3 Mo1 C3 153.50(14) . . ? N1 Mo1 C3 81.37(13) . . ? C5 Mo1 C3 61.31(15) . . ? C13 N1 N2 104.1(3) . . ? C13 N1 Mo1 138.4(3) . . ? N2 N1 Mo1 117.4(2) . . ? C11 N2 N1 112.3(3) . . ? C21 N3 N4 105.1(4) . . ? C21 N3 Mo1 136.4(3) . . ? N4 N3 Mo1 117.7(3) . . ? C23 N4 N3 111.8(4) . . ? O1 C1 Mo1 176.9(3) . . ? O2 C2 Mo1 176.1(4) . . ? C4 C3 Mo1 66.9(2) . . ? C3 C4 C5 115.6(4) . . ? C3 C4 Mo1 77.4(2) . . ? C5 C4 Mo1 76.6(2) . . ? C4 C5 Mo1 67.2(2) . . ? C6 O6 Mo1 128.8(2) . . ? O7 C6 O6 123.5(4) . . ? O7 C6 C7 119.8(4) . . ? O6 C6 C7 116.7(4) . . ? N2 C11 C12 106.3(3) . . ? N2 C11 C14 122.6(4) . . ? C12 C11 C14 131.1(4) . . ? C11 C12 C13 106.9(3) . . ? N1 C13 C12 110.3(4) . . ? N1 C13 C15 122.5(4) . . ? C12 C13 C15 127.2(4) . . ? N3 C21 C22 109.5(4) . . ? N3 C21 C24 122.2(4) . . ? C22 C21 C24 128.3(4) . . ? C23 C22 C21 107.3(5) . . ? N4 C23 C22 106.3(4) . . ? N4 C23 C25 119.8(5) . . ? C22 C23 C25 133.9(5) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 23.27 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.661 _refine_diff_density_min -0.230 _refine_diff_density_rms 0.058 #===END data_Compound_2a_an101rm _database_code_depnum_ccdc_archive 'CCDC 791637' #TrackingRef 'dt-art-05-2010-000570-File002_v1_0.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H34 Mo4 N8 O12.50' _chemical_formula_weight 1066.39 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.790(3) _cell_length_b 18.862(5) _cell_length_c 16.649(4) _cell_angle_alpha 90.00 _cell_angle_beta 94.793(5) _cell_angle_gamma 90.00 _cell_volume 4002.7(17) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 805 _cell_measurement_theta_min 2.46 _cell_measurement_theta_max 18.34 _exptl_crystal_description BLOCK _exptl_crystal_colour BROWN _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.770 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2104 _exptl_absorpt_coefficient_mu 1.290 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.581379 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18100 _diffrn_reflns_av_R_equivalents 0.1110 _diffrn_reflns_av_sigmaI/netI 0.1224 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 23.28 _reflns_number_total 5758 _reflns_number_gt 3122 _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 '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^)+(0.0696P)^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_number_reflns 5758 _refine_ls_number_parameters 460 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1321 _refine_ls_R_factor_gt 0.0584 _refine_ls_wR_factor_ref 0.1561 _refine_ls_wR_factor_gt 0.1259 _refine_ls_goodness_of_fit_ref 0.971 _refine_ls_restrained_S_all 0.971 _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 0.42947(8) 0.79219(6) 0.81477(7) 0.0513(3) Uani 1 1 d . . . Mo2 Mo 0.70570(8) 0.75515(5) 0.75913(6) 0.0428(3) Uani 1 1 d . . . Mo3 Mo 0.64573(8) 0.63786(5) 0.82256(6) 0.0420(3) Uani 1 1 d . . . Mo4 Mo 0.93644(8) 0.61438(6) 0.81092(7) 0.0503(3) Uani 1 1 d . . . N1 N 0.5026(10) 0.8353(6) 0.9303(7) 0.070(3) Uani 1 1 d . . . N2 N 0.6032(10) 0.8440(6) 0.9546(8) 0.077(4) Uani 1 1 d . . . H2 H 0.6533 0.8284 0.9280 0.092 Uiso 1 1 calc R . . N3 N 0.5367(7) 0.8708(5) 0.7642(6) 0.050(3) Uani 1 1 d . . . N4 N 0.6397(7) 0.8570(5) 0.7500(6) 0.053(3) Uani 1 1 d . . . N5 N 0.9580(7) 0.6638(5) 0.9332(6) 0.047(3) Uani 1 1 d . . . N6 N 0.8865(8) 0.6703(6) 0.9857(7) 0.059(3) Uani 1 1 d . . . H6 H 0.8211 0.6608 0.9745 0.071 Uiso 1 1 calc R . . N7 N 0.8348(8) 0.5422(5) 0.8750(6) 0.056(3) Uani 1 1 d . . . N8 N 0.7283(8) 0.5521(5) 0.8784(6) 0.052(3) Uani 1 1 d . . . O1 O 0.2908(8) 0.7042(7) 0.9229(8) 0.116(5) Uani 1 1 d . . . O2 O 0.2360(8) 0.8878(7) 0.8313(7) 0.117(5) Uani 1 1 d . . . O3 O 0.5816(5) 0.7332(4) 0.8120(4) 0.044(2) Uani 1 1 d . . . O4 O 0.6900(6) 0.7382(4) 0.6612(5) 0.062(2) Uani 1 1 d . . . O5 O 0.7834(5) 0.6722(4) 0.8066(4) 0.0416(19) Uani 1 1 d . . . O6 O 0.5958(6) 0.5933(4) 0.7420(5) 0.057(2) Uani 1 1 d . . . O7 O 1.0914(8) 0.7257(6) 0.7519(6) 0.087(3) Uani 1 1 d . . . O8 O 1.1542(9) 0.5415(7) 0.8428(8) 0.130(5) Uani 1 1 d . . . O21 O 0.8545(6) 0.8052(5) 0.7578(6) 0.063(2) Uani 1 1 d . . . O22 O 0.7905(6) 0.8051(4) 0.8746(5) 0.056(2) Uani 1 1 d . . . O23 O 0.5285(6) 0.6145(4) 0.9019(5) 0.053(2) Uani 1 1 d . . . O24 O 0.6600(6) 0.6748(4) 0.9561(4) 0.051(2) Uani 1 1 d . . . C1 C 0.3455(11) 0.7322(9) 0.8835(9) 0.077(5) Uani 1 1 d . . . C2 C 0.3090(11) 0.8536(8) 0.8249(9) 0.075(4) Uani 1 1 d . . . C3 C 0.3334(10) 0.8063(8) 0.6884(8) 0.072(4) Uani 1 1 d . . . H3A H 0.2752 0.8095 0.7182 0.086 Uiso 1 1 calc R . . H3B H 0.3501 0.8437 0.6554 0.086 Uiso 1 1 calc R . . C4 C 0.3953(11) 0.7458(9) 0.6933(8) 0.068(4) Uani 1 1 d . . . H4 H 0.4538 0.7413 0.6641 0.081 Uiso 1 1 calc R . . C5 C 0.3661(11) 0.6928(7) 0.7431(9) 0.072(4) Uani 1 1 d . . . H5A H 0.3072 0.6984 0.7717 0.086 Uiso 1 1 calc R . . H5B H 0.4051 0.6512 0.7484 0.086 Uiso 1 1 calc R . . C6 C 0.9468(13) 0.5138(8) 0.7295(9) 0.087(5) Uani 1 1 d . . . H6A H 1.0178 0.5244 0.7296 0.104 Uiso 1 1 calc R . . H6B H 0.9257 0.4704 0.7492 0.104 Uiso 1 1 calc R . . C7 C 1.0311(11) 0.6856(7) 0.7734(8) 0.062(4) Uani 1 1 d . . . C8 C 1.0726(12) 0.5665(8) 0.8320(9) 0.077(4) Uani 1 1 d . . . C9 C 0.8723(13) 0.5627(10) 0.6998(9) 0.085(5) Uani 1 1 d . . . H9 H 0.8010 0.5528 0.6994 0.102 Uiso 1 1 calc R . . C10 C 0.9070(12) 0.6277(8) 0.6705(8) 0.078(4) Uani 1 1 d . . . H10A H 0.9785 0.6370 0.6713 0.094 Uiso 1 1 calc R . . H10B H 0.8586 0.6613 0.6503 0.094 Uiso 1 1 calc R . . C11 C 0.8644(10) 0.8202(6) 0.8327(10) 0.054(4) Uani 1 1 d . . . C12 C 0.9648(11) 0.8526(8) 0.8700(10) 0.097(6) Uani 1 1 d . . . H12A H 0.9862 0.8285 0.9194 0.145 Uiso 1 1 calc R . . H12B H 0.9534 0.9018 0.8808 0.145 Uiso 1 1 calc R . . H12C H 1.0185 0.8480 0.8334 0.145 Uiso 1 1 calc R . . C13 C 0.5722(10) 0.6472(7) 0.9636(8) 0.052(3) Uani 1 1 d . . . C14 C 0.5183(10) 0.6495(8) 1.0382(8) 0.078(4) Uani 1 1 d . . . H14A H 0.5234 0.6965 1.0606 0.117 Uiso 1 1 calc R . . H14B H 0.5506 0.6164 1.0764 0.117 Uiso 1 1 calc R . . H14C H 0.4458 0.6373 1.0265 0.117 Uiso 1 1 calc R . . C21 C 0.6194(14) 0.8791(9) 1.0240(9) 0.087(5) Uani 1 1 d . . . H21 H 0.6834 0.8921 1.0507 0.105 Uiso 1 1 calc R . . C22 C 0.5274(18) 0.8911(11) 1.0459(11) 0.127(8) Uani 1 1 d . . . H22 H 0.5122 0.9130 1.0935 0.153 Uiso 1 1 calc R . . C23 C 0.4563(14) 0.8666(12) 0.9881(11) 0.127(8) Uani 1 1 d . . . H23 H 0.3840 0.8712 0.9891 0.152 Uiso 1 1 calc R . . C24 C 0.9251(13) 0.6924(8) 1.0554(9) 0.079(5) Uani 1 1 d . . . H24 H 0.8889 0.6993 1.1009 0.095 Uiso 1 1 calc R . . C25 C 1.0287(13) 0.7035(8) 1.0490(10) 0.084(5) Uani 1 1 d . . . H25 H 1.0779 0.7201 1.0890 0.101 Uiso 1 1 calc R . . C26 C 1.0458(10) 0.6857(7) 0.9732(9) 0.061(4) Uani 1 1 d . . . H26 H 1.1105 0.6884 0.9517 0.073 Uiso 1 1 calc R . . C31 C 0.6836(11) 0.9181(7) 0.7241(9) 0.071(4) Uani 1 1 d . . . H31A H 0.7523 0.9238 0.7106 0.086 Uiso 1 1 calc R . . C32 C 0.6069(11) 0.9701(7) 0.7214(9) 0.078(5) Uani 1 1 d . . . H32A H 0.6139 1.0172 0.7064 0.094 Uiso 1 1 calc R . . C33 C 0.5195(11) 0.9383(7) 0.7452(8) 0.069(4) Uani 1 1 d . . . H33A H 0.4554 0.9611 0.7479 0.083 Uiso 1 1 calc R . . C34 C 0.6933(10) 0.5012(7) 0.9251(8) 0.061(4) Uani 1 1 d . . . H34 H 0.6248 0.4977 0.9397 0.074 Uiso 1 1 calc R . . C35 C 0.7732(12) 0.4543(7) 0.9487(9) 0.076(4) Uani 1 1 d . . . H35 H 0.7696 0.4128 0.9786 0.091 Uiso 1 1 calc R . . C36 C 0.8586(13) 0.4835(8) 0.9177(10) 0.086(5) Uani 1 1 d . . . H36 H 0.9259 0.4647 0.9255 0.104 Uiso 1 1 calc R . . O91 O 0.8207(18) 0.1301(9) 0.9376(14) 0.133(6) Uiso 0.50 1 d PG . . C92 C 0.7589(19) 0.0825(14) 0.8822(13) 0.133(6) Uiso 0.50 1 d PG . . H92A H 0.6850 0.0942 0.8812 0.160 Uiso 0.50 1 calc PR . . H92B H 0.7806 0.0875 0.8281 0.160 Uiso 0.50 1 calc PR . . C93 C 0.777(2) 0.0094(11) 0.9109(17) 0.133(6) Uiso 0.50 1 d PG . . H93A H 0.8065 -0.0187 0.8697 0.160 Uiso 0.50 1 calc PR . . H93B H 0.7109 -0.0120 0.9229 0.160 Uiso 0.50 1 calc PR . . C94 C 0.850(2) 0.0119(11) 0.9840(16) 0.133(6) Uiso 0.50 1 d PG . . H94A H 0.8167 -0.0084 1.0291 0.160 Uiso 0.50 1 calc PR . . H94B H 0.9123 -0.0151 0.9760 0.160 Uiso 0.50 1 calc PR . . C95 C 0.8767(19) 0.0865(14) 1.0005(13) 0.133(6) Uiso 0.50 1 d PG . . H95A H 0.9518 0.0933 1.0000 0.160 Uiso 0.50 1 calc PR . . H95B H 0.8561 0.1001 1.0532 0.160 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0331(6) 0.0609(8) 0.0610(8) 0.0121(6) 0.0107(5) 0.0095(5) Mo2 0.0326(6) 0.0434(7) 0.0533(7) 0.0100(5) 0.0099(5) 0.0022(5) Mo3 0.0351(6) 0.0392(6) 0.0517(7) 0.0064(5) 0.0038(5) -0.0021(5) Mo4 0.0408(7) 0.0526(7) 0.0585(7) -0.0036(6) 0.0104(5) 0.0130(5) N1 0.056(8) 0.085(9) 0.070(8) -0.005(7) 0.016(7) 0.009(7) N2 0.063(9) 0.081(9) 0.087(10) -0.027(8) 0.011(7) 0.013(7) N3 0.043(6) 0.046(7) 0.062(7) 0.019(5) 0.009(5) 0.016(5) N4 0.039(6) 0.052(7) 0.068(7) 0.007(6) 0.010(5) -0.004(5) N5 0.027(6) 0.062(7) 0.051(6) -0.007(5) 0.003(5) 0.005(5) N6 0.046(7) 0.076(8) 0.055(8) -0.014(6) 0.005(6) -0.008(6) N7 0.053(7) 0.044(7) 0.069(8) 0.012(6) -0.002(6) 0.013(5) N8 0.053(7) 0.038(6) 0.064(7) 0.014(5) 0.005(5) -0.005(5) O1 0.046(7) 0.161(12) 0.145(11) 0.069(9) 0.032(7) -0.011(7) O2 0.062(7) 0.145(11) 0.146(11) -0.004(8) 0.020(7) 0.061(8) O3 0.031(4) 0.040(5) 0.063(5) 0.009(4) 0.009(4) 0.000(3) O4 0.055(6) 0.071(6) 0.059(6) 0.021(5) 0.010(4) 0.012(5) O5 0.030(4) 0.037(4) 0.057(5) 0.005(4) 0.002(4) 0.004(3) O6 0.062(6) 0.045(5) 0.064(6) 0.002(4) -0.003(4) -0.010(4) O7 0.057(7) 0.106(9) 0.104(9) 0.009(7) 0.030(6) -0.012(6) O8 0.081(9) 0.152(12) 0.157(12) -0.002(9) 0.011(8) 0.087(9) O21 0.040(5) 0.071(7) 0.079(7) 0.019(6) 0.011(5) 0.000(4) O22 0.045(5) 0.045(5) 0.079(6) 0.002(5) 0.008(5) -0.007(4) O23 0.042(5) 0.056(6) 0.060(6) 0.012(5) 0.005(4) -0.010(4) O24 0.051(5) 0.057(5) 0.047(5) -0.006(4) 0.010(4) -0.008(4) C1 0.038(9) 0.107(13) 0.086(11) 0.023(10) 0.002(8) 0.013(8) C2 0.047(9) 0.091(12) 0.085(11) 0.000(9) 0.000(8) 0.013(8) C3 0.060(9) 0.098(12) 0.058(10) 0.025(8) 0.011(7) 0.020(9) C4 0.061(9) 0.093(12) 0.049(9) -0.009(9) 0.001(7) -0.012(9) C5 0.055(9) 0.069(10) 0.091(12) 0.002(9) 0.000(8) 0.012(8) C6 0.092(12) 0.064(11) 0.104(13) -0.034(9) 0.006(10) 0.008(9) C7 0.046(9) 0.067(10) 0.073(10) -0.007(8) 0.008(7) 0.012(7) C8 0.078(11) 0.084(11) 0.071(10) 0.000(8) 0.022(8) 0.023(9) C9 0.076(12) 0.114(15) 0.064(11) -0.035(10) -0.012(9) 0.018(11) C10 0.081(11) 0.079(12) 0.074(11) -0.014(9) 0.009(8) 0.022(9) C11 0.042(9) 0.036(8) 0.084(11) 0.017(8) 0.006(8) -0.004(6) C12 0.062(10) 0.080(11) 0.142(16) 0.016(11) -0.023(10) -0.022(9) C13 0.050(9) 0.046(8) 0.061(9) 0.007(7) 0.006(7) -0.005(7) C14 0.059(9) 0.123(13) 0.053(9) 0.006(9) 0.020(7) -0.005(9) C21 0.100(15) 0.104(14) 0.056(11) -0.018(10) -0.007(10) 0.017(11) C22 0.124(18) 0.18(2) 0.079(14) -0.060(14) 0.011(13) 0.046(16) C23 0.071(13) 0.23(2) 0.081(13) -0.056(15) 0.024(11) 0.024(14) C24 0.073(12) 0.100(13) 0.065(11) -0.009(9) 0.005(9) 0.018(9) C25 0.064(12) 0.108(14) 0.078(13) -0.014(10) -0.013(9) -0.002(10) C26 0.044(9) 0.066(10) 0.072(11) -0.001(8) 0.006(8) -0.004(7) C31 0.047(9) 0.064(10) 0.103(12) 0.035(9) 0.006(8) -0.005(8) C32 0.058(10) 0.039(8) 0.138(15) 0.014(9) 0.014(9) -0.001(8) C33 0.061(10) 0.063(10) 0.083(11) 0.015(8) 0.007(8) 0.029(8) C34 0.052(9) 0.055(9) 0.077(10) 0.010(8) 0.012(7) 0.007(7) C35 0.077(11) 0.054(9) 0.095(12) 0.018(8) -0.004(9) -0.004(9) C36 0.070(11) 0.060(10) 0.125(15) 0.019(10) -0.013(10) 0.019(9) _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 C2 1.947(15) . ? Mo1 C1 1.988(17) . ? Mo1 C4 2.214(12) . ? Mo1 N1 2.222(12) . ? Mo1 N3 2.232(10) . ? Mo1 O3 2.245(7) . ? Mo1 C5 2.331(13) . ? Mo1 C3 2.361(12) . ? Mo2 O4 1.658(8) . ? Mo2 O3 1.924(7) . ? Mo2 O5 1.983(7) . ? Mo2 N4 2.099(10) . ? Mo2 O21 2.126(8) . ? Mo2 O22 2.327(8) . ? Mo2 Mo3 2.5950(15) . ? Mo3 O6 1.665(8) . ? Mo3 O5 1.915(7) . ? Mo3 O3 1.978(7) . ? Mo3 N8 2.106(9) . ? Mo3 O23 2.126(8) . ? Mo3 O24 2.322(7) . ? Mo4 C7 1.946(16) . ? Mo4 C8 1.968(15) . ? Mo4 C9 2.188(13) . ? Mo4 N7 2.216(10) . ? Mo4 N5 2.235(10) . ? Mo4 O5 2.237(7) . ? Mo4 C6 2.342(13) . ? Mo4 C10 2.350(14) . ? N1 C23 1.311(18) . ? N1 N2 1.326(14) . ? N2 C21 1.334(16) . ? N3 C33 1.327(14) . ? N3 N4 1.381(12) . ? N4 C31 1.368(15) . ? N5 N6 1.322(13) . ? N5 C26 1.324(14) . ? N6 C24 1.292(15) . ? N7 C36 1.338(15) . ? N7 N8 1.381(13) . ? N8 C34 1.337(14) . ? O1 C1 1.129(16) . ? O2 C2 1.147(15) . ? O7 C7 1.158(15) . ? O8 C8 1.145(15) . ? O21 C11 1.274(15) . ? O22 C11 1.254(15) . ? O23 C13 1.285(14) . ? O24 C13 1.253(13) . ? C3 C4 1.388(18) . ? C4 C5 1.371(17) . ? C6 C9 1.387(19) . ? C9 C10 1.40(2) . ? C11 C12 1.508(17) . ? C13 C14 1.471(16) . ? C21 C22 1.28(2) . ? C22 C23 1.35(2) . ? C24 C25 1.355(19) . ? C25 C26 1.342(18) . ? C31 C32 1.385(17) . ? C32 C33 1.357(17) . ? C34 C35 1.384(17) . ? C35 C36 1.363(19) . ? O91 C92 1.4697 . ? O91 C95 1.4698 . ? C92 C93 1.4697 . ? C93 C94 1.4697 . ? C94 C95 1.4697 . ? 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 C2 Mo1 C1 79.6(6) . . ? C2 Mo1 C4 102.5(6) . . ? C1 Mo1 C4 103.1(6) . . ? C2 Mo1 N1 89.2(5) . . ? C1 Mo1 N1 85.3(5) . . ? C4 Mo1 N1 166.5(5) . . ? C2 Mo1 N3 98.8(5) . . ? C1 Mo1 N3 167.0(5) . . ? C4 Mo1 N3 89.9(5) . . ? N1 Mo1 N3 81.7(4) . . ? C2 Mo1 O3 172.1(5) . . ? C1 Mo1 O3 103.9(4) . . ? C4 Mo1 O3 83.7(4) . . ? N1 Mo1 O3 84.1(4) . . ? N3 Mo1 O3 76.1(3) . . ? C2 Mo1 C5 106.2(5) . . ? C1 Mo1 C5 69.8(6) . . ? C4 Mo1 C5 35.0(4) . . ? N1 Mo1 C5 147.2(5) . . ? N3 Mo1 C5 122.7(5) . . ? O3 Mo1 C5 81.7(4) . . ? C2 Mo1 C3 69.7(5) . . ? C1 Mo1 C3 108.1(5) . . ? C4 Mo1 C3 35.1(5) . . ? N1 Mo1 C3 151.7(5) . . ? N3 Mo1 C3 83.1(4) . . ? O3 Mo1 C3 115.1(4) . . ? C5 Mo1 C3 60.1(5) . . ? O4 Mo2 O3 111.8(4) . . ? O4 Mo2 O5 104.8(3) . . ? O3 Mo2 O5 93.0(3) . . ? O4 Mo2 N4 95.2(4) . . ? O3 Mo2 N4 83.6(3) . . ? O5 Mo2 N4 159.5(3) . . ? O4 Mo2 O21 96.3(4) . . ? O3 Mo2 O21 151.0(4) . . ? O5 Mo2 O21 86.3(3) . . ? N4 Mo2 O21 87.0(3) . . ? O4 Mo2 O22 154.3(4) . . ? O3 Mo2 O22 93.1(3) . . ? O5 Mo2 O22 78.9(3) . . ? N4 Mo2 O22 81.1(3) . . ? O21 Mo2 O22 58.2(3) . . ? O4 Mo2 Mo3 102.7(3) . . ? O3 Mo2 Mo3 49.2(2) . . ? O5 Mo2 Mo3 47.1(2) . . ? N4 Mo2 Mo3 132.8(3) . . ? O21 Mo2 Mo3 132.7(2) . . ? O22 Mo2 Mo3 98.2(2) . . ? O6 Mo3 O5 110.8(4) . . ? O6 Mo3 O3 105.0(3) . . ? O5 Mo3 O3 93.4(3) . . ? O6 Mo3 N8 96.4(4) . . ? O5 Mo3 N8 83.6(3) . . ? O3 Mo3 N8 158.0(3) . . ? O6 Mo3 O23 98.8(4) . . ? O5 Mo3 O23 149.4(3) . . ? O3 Mo3 O23 86.3(3) . . ? N8 Mo3 O23 85.4(4) . . ? O6 Mo3 O24 156.5(4) . . ? O5 Mo3 O24 91.8(3) . . ? O3 Mo3 O24 79.1(3) . . ? N8 Mo3 O24 79.2(3) . . ? O23 Mo3 O24 58.0(3) . . ? O6 Mo3 Mo2 102.1(3) . . ? O5 Mo3 Mo2 49.4(2) . . ? O3 Mo3 Mo2 47.4(2) . . ? N8 Mo3 Mo2 132.9(3) . . ? O23 Mo3 Mo2 132.7(2) . . ? O24 Mo3 Mo2 97.5(2) . . ? C7 Mo4 C8 79.0(6) . . ? C7 Mo4 C9 103.6(6) . . ? C8 Mo4 C9 102.1(6) . . ? C7 Mo4 N7 169.8(5) . . ? C8 Mo4 N7 100.3(5) . . ? C9 Mo4 N7 86.5(6) . . ? C7 Mo4 N5 88.4(5) . . ? C8 Mo4 N5 89.4(5) . . ? C9 Mo4 N5 164.7(5) . . ? N7 Mo4 N5 81.4(4) . . ? C7 Mo4 O5 102.7(4) . . ? C8 Mo4 O5 171.5(5) . . ? C9 Mo4 O5 85.7(5) . . ? N7 Mo4 O5 76.6(3) . . ? N5 Mo4 O5 82.3(3) . . ? C7 Mo4 C6 107.8(6) . . ? C8 Mo4 C6 68.8(6) . . ? C9 Mo4 C6 35.5(5) . . ? N7 Mo4 C6 81.1(5) . . ? N5 Mo4 C6 148.9(5) . . ? O5 Mo4 C6 117.9(4) . . ? C7 Mo4 C10 70.1(6) . . ? C8 Mo4 C10 107.0(5) . . ? C9 Mo4 C10 35.8(5) . . ? N7 Mo4 C10 119.5(5) . . ? N5 Mo4 C10 149.2(5) . . ? O5 Mo4 C10 81.3(4) . . ? C6 Mo4 C10 61.5(5) . . ? C23 N1 N2 102.0(13) . . ? C23 N1 Mo1 128.0(12) . . ? N2 N1 Mo1 129.6(9) . . ? N1 N2 C21 113.7(13) . . ? C33 N3 N4 106.4(10) . . ? C33 N3 Mo1 129.2(9) . . ? N4 N3 Mo1 124.4(7) . . ? C31 N4 N3 108.6(10) . . ? C31 N4 Mo2 128.4(9) . . ? N3 N4 Mo2 122.9(7) . . ? N6 N5 C26 104.1(11) . . ? N6 N5 Mo4 127.0(8) . . ? C26 N5 Mo4 128.6(9) . . ? C24 N6 N5 113.0(11) . . ? C36 N7 N8 105.7(11) . . ? C36 N7 Mo4 130.4(10) . . ? N8 N7 Mo4 123.9(7) . . ? C34 N8 N7 107.9(9) . . ? C34 N8 Mo3 129.0(9) . . ? N7 N8 Mo3 123.1(7) . . ? Mo2 O3 Mo3 83.4(3) . . ? Mo2 O3 Mo1 130.7(3) . . ? Mo3 O3 Mo1 143.4(4) . . ? Mo3 O5 Mo2 83.5(3) . . ? Mo3 O5 Mo4 130.0(3) . . ? Mo2 O5 Mo4 143.7(4) . . ? C11 O21 Mo2 96.0(7) . . ? C11 O22 Mo2 87.3(8) . . ? C13 O23 Mo3 96.6(7) . . ? C13 O24 Mo3 88.4(7) . . ? O1 C1 Mo1 172.6(14) . . ? O2 C2 Mo1 177.7(15) . . ? C4 C3 Mo1 66.6(7) . . ? C5 C4 C3 116.9(14) . . ? C5 C4 Mo1 77.2(8) . . ? C3 C4 Mo1 78.2(8) . . ? C4 C5 Mo1 67.8(8) . . ? C9 C6 Mo4 66.2(8) . . ? O7 C7 Mo4 176.7(12) . . ? O8 C8 Mo4 176.6(15) . . ? C6 C9 C10 118.4(16) . . ? C6 C9 Mo4 78.3(8) . . ? C10 C9 Mo4 78.4(9) . . ? C9 C10 Mo4 65.8(8) . . ? O22 C11 O21 118.5(12) . . ? O22 C11 C12 121.2(15) . . ? O21 C11 C12 120.3(14) . . ? O24 C13 O23 117.0(11) . . ? O24 C13 C14 124.0(13) . . ? O23 C13 C14 119.1(12) . . ? C22 C21 N2 104.7(16) . . ? C21 C22 C23 108.6(16) . . ? N1 C23 C22 111.0(16) . . ? N6 C24 C25 106.4(14) . . ? C26 C25 C24 105.8(13) . . ? N5 C26 C25 110.7(13) . . ? N4 C31 C32 107.3(12) . . ? C33 C32 C31 106.1(12) . . ? N3 C33 C32 111.6(12) . . ? N8 C34 C35 110.4(12) . . ? C36 C35 C34 103.3(13) . . ? N7 C36 C35 112.5(13) . . ? C92 O91 C95 108.0 . . ? C93 C92 O91 108.0 . . ? C92 C93 C94 108.0 . . ? C95 C94 C93 108.0 . . ? C94 C95 O91 108.0 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 23.28 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.022 _refine_diff_density_min -0.915 _refine_diff_density_rms 0.133 #===END data_Compound_2b_pp65am _database_code_depnum_ccdc_archive 'CCDC 791638' #TrackingRef 'dt-art-05-2010-000570-File002_v1_0.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H52 Mo4 N8 O13' _chemical_formula_weight 1200.63 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' 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 22.107(15) _cell_length_b 10.393(7) _cell_length_c 22.682(15) _cell_angle_alpha 90.00 _cell_angle_beta 105.404(12) _cell_angle_gamma 90.00 _cell_volume 5024(6) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 989 _cell_measurement_theta_min 2.2647 _cell_measurement_theta_max 23.2547 _exptl_crystal_description PLATE _exptl_crystal_colour ORANGE _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.587 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2408 _exptl_absorpt_coefficient_mu 1.038 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.811125 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10703 _diffrn_reflns_av_R_equivalents 0.0296 _diffrn_reflns_av_sigmaI/netI 0.0311 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 23.32 _reflns_number_total 3632 _reflns_number_gt 3084 _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 '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^)+(0.0401P)^2^+47.2755P] 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 3632 _refine_ls_number_parameters 277 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0548 _refine_ls_R_factor_gt 0.0437 _refine_ls_wR_factor_ref 0.1152 _refine_ls_wR_factor_gt 0.1078 _refine_ls_goodness_of_fit_ref 1.117 _refine_ls_restrained_S_all 1.117 _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 0.14961(3) 0.56922(5) 0.36325(2) 0.03947(19) Uani 1 1 d . . . Mo2 Mo 0.03334(3) 0.62727(5) 0.21063(2) 0.03486(18) Uani 1 1 d . . . N1 N 0.1261(3) 0.3592(5) 0.3565(3) 0.0484(14) Uani 1 1 d . . . N2 N 0.1050(3) 0.3043(5) 0.3008(3) 0.0544(16) Uani 1 1 d . . . H2 H 0.0943 0.3469 0.2671 0.065 Uiso 1 1 calc R . . N3 N 0.1665(3) 0.5286(5) 0.2701(2) 0.0453(14) Uani 1 1 d . . . N4 N 0.1308(3) 0.5920(5) 0.2185(2) 0.0407(13) Uani 1 1 d . . . C1 C 0.1283(4) 0.5856(7) 0.4413(3) 0.0526(18) Uani 1 1 d . . . O1 O 0.1202(3) 0.5969(6) 0.4895(2) 0.0794(18) Uani 1 1 d . . . C2 C 0.2278(4) 0.5287(8) 0.4225(4) 0.062(2) Uani 1 1 d . . . O2 O 0.2726(3) 0.5080(7) 0.4610(3) 0.096(2) Uani 1 1 d . . . O3 O 0.0563(2) 0.5905(4) 0.29706(18) 0.0381(10) Uani 1 1 d . . . O4 O 0.0370(2) 0.7848(4) 0.1968(2) 0.0467(11) Uani 1 1 d . . . O21 O 0.0132(2) 0.5615(5) 0.1191(2) 0.0485(12) Uani 1 1 d . . . O22 O 0.0333(2) 0.4087(4) 0.1864(2) 0.0503(12) Uani 1 1 d . . . C3 C 0.2256(4) 0.7247(8) 0.3636(4) 0.065(2) Uani 1 1 d . . . H3A H 0.2490 0.7573 0.4031 0.079 Uiso 1 1 calc R . . H3B H 0.2506 0.7132 0.3348 0.079 Uiso 1 1 calc R . . C4 C 0.1647(4) 0.7719(6) 0.3402(3) 0.0524(19) Uani 1 1 d . . . H4 H 0.1500 0.8047 0.2983 0.063 Uiso 1 1 calc R . . C5 C 0.1282(4) 0.7820(7) 0.3820(4) 0.059(2) Uani 1 1 d . . . H5A H 0.0853 0.8109 0.3661 0.071 Uiso 1 1 calc R . . H5B H 0.1488 0.8161 0.4222 0.071 Uiso 1 1 calc R . . C11 C 0.0203(3) 0.4424(7) 0.1313(3) 0.0510(18) Uani 1 1 d . . . C12 C 0.0152(5) 0.3488(9) 0.0802(4) 0.081(3) Uani 1 1 d . . . H12A H 0.0563 0.3284 0.0765 0.122 Uiso 1 1 calc R . . H12B H -0.0092 0.3861 0.0427 0.122 Uiso 1 1 calc R . . H12C H -0.0049 0.2716 0.0887 0.122 Uiso 1 1 calc R . . C21 C 0.1364(4) 0.2598(7) 0.3961(4) 0.063(2) Uani 1 1 d . . . C22 C 0.1218(5) 0.1465(8) 0.3646(5) 0.084(3) Uani 1 1 d . . . H22 H 0.1244 0.0644 0.3814 0.100 Uiso 1 1 calc R . . C23 C 0.1028(5) 0.1763(8) 0.3043(4) 0.073(2) Uani 1 1 d . . . C24 C 0.1581(5) 0.2778(9) 0.4634(4) 0.084(3) Uani 1 1 d . . . H24A H 0.1996 0.3139 0.4740 0.126 Uiso 1 1 calc R . . H24B H 0.1588 0.1961 0.4833 0.126 Uiso 1 1 calc R . . H24C H 0.1301 0.3349 0.4764 0.126 Uiso 1 1 calc R . . C25 C 0.0832(6) 0.0960(9) 0.2477(5) 0.110(4) Uani 1 1 d . . . H25A H 0.0452 0.1302 0.2214 0.164 Uiso 1 1 calc R . . H25B H 0.0762 0.0091 0.2586 0.164 Uiso 1 1 calc R . . H25C H 0.1156 0.0973 0.2267 0.164 Uiso 1 1 calc R . . C31 C 0.2173(4) 0.4817(7) 0.2561(4) 0.0568(19) Uani 1 1 d . . . C32 C 0.2161(4) 0.5162(8) 0.1969(4) 0.063(2) Uani 1 1 d . . . H32 H 0.2461 0.4968 0.1763 0.075 Uiso 1 1 calc R . . C33 C 0.1621(4) 0.5844(7) 0.1748(3) 0.0487(17) Uani 1 1 d . . . C34 C 0.2648(4) 0.4024(9) 0.2999(4) 0.083(3) Uani 1 1 d . . . H34A H 0.2938 0.4579 0.3275 0.125 Uiso 1 1 calc R . . H34B H 0.2872 0.3505 0.2777 0.125 Uiso 1 1 calc R . . H34C H 0.2442 0.3478 0.3226 0.125 Uiso 1 1 calc R . . C35 C 0.1400(4) 0.6477(8) 0.1132(3) 0.064(2) Uani 1 1 d . . . H35A H 0.1159 0.5873 0.0843 0.097 Uiso 1 1 calc R . . H35B H 0.1755 0.6756 0.0998 0.097 Uiso 1 1 calc R . . H35C H 0.1143 0.7206 0.1162 0.097 Uiso 1 1 calc R . . O90 O 0.9147(6) 0.0014(17) 0.4190(6) 0.155(7) Uiso 0.50 1 d PG A 1 C92 C 1.0097(6) -0.0697(15) 0.4561(8) 0.078(5) Uiso 0.50 1 d PG . 1 H92A H 1.0023 -0.1045 0.4156 0.117 Uiso 0.50 1 d PG A 1 H92B H 1.0468 -0.0174 0.4650 0.117 Uiso 0.50 1 d PG A 1 H92C H 1.0153 -0.1388 0.4852 0.117 Uiso 0.50 1 d PG A 1 C91 C 0.9585(5) 0.0052(9) 0.4598(4) 0.068(4) Uiso 0.50 1 d PG . 1 C93 C 0.9462(8) 0.0733(16) 0.5058(6) 0.093(6) Uiso 0.50 1 d PG . 1 H93A H 0.9058 0.1134 0.4917 0.140 Uiso 0.50 1 d PG A 1 H93B H 0.9462 0.0168 0.5392 0.140 Uiso 0.50 1 d PG A 1 H93C H 0.9778 0.1382 0.5191 0.140 Uiso 0.50 1 d PG A 1 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 0.0485(4) 0.0332(3) 0.0365(3) 0.0046(2) 0.0110(3) 0.0040(3) Mo2 0.0469(4) 0.0272(3) 0.0318(3) 0.0011(2) 0.0128(2) -0.0009(2) N1 0.065(4) 0.029(3) 0.050(3) 0.007(3) 0.013(3) 0.008(3) N2 0.079(4) 0.031(3) 0.054(4) 0.002(3) 0.018(3) 0.007(3) N3 0.046(3) 0.044(3) 0.049(3) 0.005(3) 0.017(3) 0.010(3) N4 0.049(3) 0.037(3) 0.037(3) 0.002(2) 0.014(3) 0.000(3) C1 0.060(5) 0.047(4) 0.049(4) 0.006(3) 0.011(4) 0.007(4) O1 0.111(5) 0.094(5) 0.040(3) 0.001(3) 0.031(3) 0.008(4) C2 0.061(5) 0.063(5) 0.060(5) 0.014(4) 0.016(4) 0.008(4) O2 0.068(4) 0.114(6) 0.086(4) 0.029(4) -0.015(4) 0.013(4) O3 0.049(3) 0.033(2) 0.032(2) 0.0019(18) 0.0115(19) -0.0004(19) O4 0.063(3) 0.030(2) 0.047(3) 0.006(2) 0.015(2) -0.005(2) O21 0.059(3) 0.049(3) 0.039(2) -0.004(2) 0.015(2) -0.002(2) O22 0.065(3) 0.034(3) 0.053(3) -0.007(2) 0.020(2) 0.001(2) C3 0.070(6) 0.057(5) 0.072(5) -0.001(4) 0.024(4) -0.014(4) C4 0.071(5) 0.028(4) 0.055(4) 0.003(3) 0.013(4) -0.004(3) C5 0.075(5) 0.037(4) 0.063(5) -0.007(4) 0.014(4) 0.000(4) C11 0.051(4) 0.052(5) 0.052(5) -0.010(4) 0.018(3) -0.005(4) C12 0.107(7) 0.074(6) 0.070(6) -0.040(5) 0.035(5) -0.012(5) C21 0.085(6) 0.039(4) 0.066(5) 0.019(4) 0.022(4) 0.008(4) C22 0.130(9) 0.030(5) 0.097(7) 0.016(5) 0.041(6) -0.001(5) C23 0.102(7) 0.038(5) 0.085(6) -0.003(4) 0.035(5) 0.001(4) C24 0.115(8) 0.068(6) 0.064(6) 0.028(5) 0.015(5) 0.010(5) C25 0.170(12) 0.050(6) 0.107(8) -0.031(6) 0.033(8) -0.004(6) C31 0.059(5) 0.053(5) 0.063(5) 0.001(4) 0.023(4) 0.014(4) C32 0.067(5) 0.071(6) 0.060(5) -0.006(4) 0.033(4) 0.008(4) C33 0.060(5) 0.048(4) 0.045(4) -0.006(3) 0.025(3) -0.007(4) C34 0.080(6) 0.091(7) 0.083(6) 0.011(5) 0.030(5) 0.040(5) C35 0.073(5) 0.080(6) 0.046(4) 0.002(4) 0.027(4) -0.012(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 C2 1.932(8) . ? Mo1 C1 1.957(8) . ? Mo1 C4 2.217(7) . ? Mo1 O3 2.216(4) . ? Mo1 N1 2.239(6) . ? Mo1 N3 2.281(6) . ? Mo1 C5 2.324(7) . ? Mo1 C3 2.329(8) . ? Mo2 O4 1.674(4) . ? Mo2 O3 1.928(4) . ? Mo2 O3 1.980(5) 2 ? Mo2 O21 2.117(4) . ? Mo2 N4 2.145(6) . ? Mo2 O22 2.337(5) . ? Mo2 Mo2 2.6002(16) 2 ? N1 C21 1.347(9) . ? N1 N2 1.351(8) . ? N2 C23 1.334(10) . ? N3 C31 1.337(9) . ? N3 N4 1.392(7) . ? N4 C33 1.354(8) . ? C1 O1 1.159(9) . ? C2 O2 1.155(9) . ? O3 Mo2 1.980(5) 2 ? O21 C11 1.268(9) . ? O22 C11 1.254(9) . ? C3 C4 1.398(11) . ? C4 C5 1.402(11) . ? C11 C12 1.495(10) . ? C21 C22 1.371(12) . ? C21 C24 1.486(11) . ? C22 C23 1.355(12) . ? C23 C25 1.496(12) . ? C31 C32 1.383(11) . ? C31 C34 1.489(11) . ? C32 C33 1.362(11) . ? C33 C35 1.504(10) . ? O90 C91 1.1498 . ? C92 C93 1.12(3) 5_756 ? C92 C91 1.3960 . ? C92 C91 1.97(3) 5_756 ? C91 C93 1.3452 . ? C91 C92 1.97(2) 5_756 ? C93 C92 1.12(3) 5_756 ? 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 C2 Mo1 C1 77.1(3) . . ? C2 Mo1 C4 102.0(3) . . ? C1 Mo1 C4 102.6(3) . . ? C2 Mo1 O3 172.8(3) . . ? C1 Mo1 O3 101.5(2) . . ? C4 Mo1 O3 85.2(2) . . ? C2 Mo1 N1 89.1(3) . . ? C1 Mo1 N1 92.3(3) . . ? C4 Mo1 N1 163.1(2) . . ? O3 Mo1 N1 83.91(18) . . ? C2 Mo1 N3 105.5(3) . . ? C1 Mo1 N3 172.9(3) . . ? C4 Mo1 N3 83.4(2) . . ? O3 Mo1 N3 75.09(17) . . ? N1 Mo1 N3 81.3(2) . . ? C2 Mo1 C5 105.5(3) . . ? C1 Mo1 C5 69.0(3) . . ? C4 Mo1 C5 35.9(3) . . ? O3 Mo1 C5 80.3(2) . . ? N1 Mo1 C5 152.3(3) . . ? N3 Mo1 C5 115.9(2) . . ? C2 Mo1 C3 68.8(3) . . ? C1 Mo1 C3 106.5(3) . . ? C4 Mo1 C3 35.7(3) . . ? O3 Mo1 C3 118.2(2) . . ? N1 Mo1 C3 146.2(3) . . ? N3 Mo1 C3 80.6(3) . . ? C5 Mo1 C3 61.4(3) . . ? O4 Mo2 O3 111.84(19) . . ? O4 Mo2 O3 105.6(2) . 2 ? O3 Mo2 O3 92.21(18) . 2 ? O4 Mo2 O21 98.0(2) . . ? O3 Mo2 O21 149.64(19) . . ? O3 Mo2 O21 84.64(17) 2 . ? O4 Mo2 N4 94.9(2) . . ? O3 Mo2 N4 83.94(19) . . ? O3 Mo2 N4 159.04(19) 2 . ? O21 Mo2 N4 88.34(19) . . ? O4 Mo2 O22 154.6(2) . . ? O3 Mo2 O22 91.75(17) . . ? O3 Mo2 O22 81.64(17) 2 . ? O21 Mo2 O22 57.90(18) . . ? N4 Mo2 O22 77.91(18) . . ? O4 Mo2 Mo2 101.17(16) . 2 ? O3 Mo2 Mo2 49.15(13) . 2 ? O3 Mo2 Mo2 47.45(12) 2 2 ? O21 Mo2 Mo2 131.57(14) . 2 ? N4 Mo2 Mo2 133.07(14) . 2 ? O22 Mo2 Mo2 101.37(12) . 2 ? C21 N1 N2 104.7(6) . . ? C21 N1 Mo1 135.0(5) . . ? N2 N1 Mo1 119.4(4) . . ? C23 N2 N1 112.0(6) . . ? C31 N3 N4 107.3(5) . . ? C31 N3 Mo1 129.9(5) . . ? N4 N3 Mo1 119.7(4) . . ? C33 N4 N3 107.5(5) . . ? C33 N4 Mo2 130.4(5) . . ? N3 N4 Mo2 118.9(4) . . ? O1 C1 Mo1 175.1(7) . . ? O2 C2 Mo1 175.1(8) . . ? Mo2 O3 Mo2 83.41(16) . 2 ? Mo2 O3 Mo1 130.9(2) . . ? Mo2 O3 Mo1 144.0(2) 2 . ? C11 O21 Mo2 96.8(4) . . ? C11 O22 Mo2 87.0(4) . . ? C4 C3 Mo1 67.7(4) . . ? C3 C4 C5 116.0(7) . . ? C3 C4 Mo1 76.5(4) . . ? C5 C4 Mo1 76.2(4) . . ? C4 C5 Mo1 67.9(4) . . ? O22 C11 O21 118.2(6) . . ? O22 C11 C12 122.7(7) . . ? O21 C11 C12 119.1(7) . . ? N1 C21 C22 109.7(7) . . ? N1 C21 C24 122.6(7) . . ? C22 C21 C24 127.6(7) . . ? C23 C22 C21 107.2(7) . . ? N2 C23 C22 106.4(8) . . ? N2 C23 C25 120.8(8) . . ? C22 C23 C25 132.8(8) . . ? N3 C31 C32 109.6(7) . . ? N3 C31 C34 122.2(7) . . ? C32 C31 C34 128.2(7) . . ? C33 C32 C31 106.3(7) . . ? N4 C33 C32 109.2(6) . . ? N4 C33 C35 123.4(7) . . ? C32 C33 C35 127.4(7) . . ? C93 C92 C91 122(2) 5_756 . ? C93 C92 C91 41.2(11) 5_756 5_756 ? C91 C92 C91 80.7(12) . 5_756 ? O90 C91 C93 110.0 . . ? O90 C91 C92 117.1 . . ? C93 C91 C92 132.4 . . ? O90 C91 C92 143.2(13) . 5_756 ? C93 C91 C92 33.2(13) . 5_756 ? C92 C91 C92 99.3(13) . 5_756 ? C92 C93 C91 105.5(19) 5_756 . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 23.32 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.397 _refine_diff_density_min -0.805 _refine_diff_density_rms 0.113 #===END