# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? #TrackingRef '- Global_Cif_with_all_2_New_structures_in_one.cif' _publ_section_title ; New insights into the mechanism of oxodiperoxomolybdenum catalysed olefin epoxidation and the crystal structures of several oxo peroxo molybdenum complexes ; # # by Matthew Herbert, Francisco Montilla, Eleuterio \'Alvarez and # Agust\'in Galindo # # To be submitted to Dalton Transactions. # Manuscript number ........... #=============================================================================80 # # Person for contact _publ_contact_author_name 'Prof. Agustin Galindo' _publ_contact_author_address ; Departamento de Qu\'imica Inorg\'anica, Universidad de Sevilla, Aptdo 1203, 41071 Sevilla, Spain ; _publ_contact_author_phone '+34 954 557160 (202)' _publ_contact_author_fax '+34 954 557153' _publ_contact_author_email galindo@us.es #=============================================================================80 # Publication details loop_ _publ_author_name _publ_author_address 'Matthew Herbert' ; Departamento de Qu\'imica Inorg\'anica, Universidad de Sevilla, Aptdo 1203, 41071 Sevilla, Spain ; 'Francisco Montilla' ; Departamento de Qu\'imica Inorg\'anica, Universidad de Sevilla, Aptdo 1203, 41071 Sevilla, Spain ; E.Alvarez ; Instituto de Investigaciones Qu\'imicas, C.S.I.C-Universidad de Sevilla, Avd. Am\'erico Vespucio, 49, Isla de la Cartuja, E-41092 Sevilla, Spain ; "Agust\'in Galindo" ; Departamento de Qu\'imica Inorg\'anica, Universidad de Sevilla, Aptdo 1203, 41071 Sevilla, Spain ; _journal_volume ? _journal_page_first ? _journal_page_last ? #========================================================================= # Three crystal structures follow, separated/terminaed by #===END. # The CIF has been tested by program checkCIF #========================================================================= #========================================================================= # Data for compound Mo(O)(O2)2(H2O)(pz) (local labelling as ea12209a) #========================================================================= data_Mo(O)(O2)2(H2O)(pz) _database_code_depnum_ccdc_archive 'CCDC 852985' #TrackingRef '- Global_Cif_with_all_2_New_structures_in_one.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C3 H6 Mo N2 O6' _chemical_formula_sum 'C3 H6 Mo N2 O6' _chemical_formula_weight 262.04 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 P2(1)/m _symmetry_space_group_name_Hall '-P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 7.3757(15) _cell_length_b 6.7764(14) _cell_length_c 8.5456(17) _cell_angle_alpha 90.00 _cell_angle_beta 114.26(3) _cell_angle_gamma 90.00 _cell_volume 389.39(16) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5913 _cell_measurement_theta_min 3.04 _cell_measurement_theta_max 30.56 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.235 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 256 _exptl_absorpt_coefficient_mu 1.681 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5953 _exptl_absorpt_correction_T_max 0.7698 _exptl_absorpt_process_details ; SADABS, Bruker (2006). APEX 2. Version 2.1. Bruker Analytical X-ray Solutions, Madison, Wisconsin, USA. ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Bruker-Nonius X8kappa APEX II CCD area detector' ; _diffrn_measurement_method 'phi and omega scans with narrow frames' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_decay_% 0 _diffrn_reflns_number 13950 _diffrn_reflns_av_R_equivalents 0.0217 _diffrn_reflns_av_sigmaI/netI 0.0091 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -6 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.99 _diffrn_reflns_theta_max 30.50 _reflns_number_total 1266 _reflns_number_gt 1243 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker (2006). APEX 2. Version 2.1.' _computing_cell_refinement 'Bruker (2006). APEX 2. Version 2.1.' _computing_data_reduction 'Bruker (2006). APEX 2. Version 2.1.' _computing_structure_solution 'Bruker (2006). APEX 2. Version 2.1.' _computing_structure_refinement 'XL, SHELXTL v. 6.14 (Bruker, 2003)' _computing_molecular_graphics 'XP, SHELXTL v. 6.14 (Bruker, 2003)' _computing_publication_material 'XCIF, SHELXTL v. 6.14 (Bruker, 2003)' _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. The asymmetric unit of the structure is formed by one molecule of Mo(O)(O2)2(H2O)(pz). All non-hydrogen atoms were refined with anisotropic displacement parameters. The hydrogen atoms were included from calculated positions and refined riding on their respective carbon atoms with isotropic displacement parameters, except the hydrogen atoms bonded to the nitrogen atoms in pyrazole rings and those bonded to an oxygen atom in water, which were detected from a difference Fourier map and refined isotropically with both N-H and O-H distances retrained (DFIX commands) to 0.90(2) \%A. The highest residual peaks, those with 0.19 e/ \%A^3^ and 0.28 e/ \%A^3^, were located close to the molybdenum metal center and have no chemical sense. ; _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^)+(0.0202P)^2^+0.1693P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1266 _refine_ls_number_parameters 72 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0147 _refine_ls_R_factor_gt 0.0143 _refine_ls_wR_factor_ref 0.0398 _refine_ls_wR_factor_gt 0.0393 _refine_ls_goodness_of_fit_ref 1.227 _refine_ls_restrained_S_all 1.233 _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 0.19778(2) 0.2500 0.239224(17) 0.01400(5) Uani 1 2 d S . . O1 O -0.0474(2) 0.2500 0.11337(18) 0.0213(3) Uani 1 2 d S . . O2 O 0.26275(15) -0.03017(15) 0.26107(12) 0.02072(18) Uani 1 1 d . . . O3 O 0.22525(15) 0.04576(15) 0.40741(12) 0.02185(19) Uani 1 1 d . . . O4 O 0.5431(2) 0.2500 0.36465(18) 0.0202(3) Uani 1 2 d SD . . H1O H 0.599(3) 0.155(2) 0.429(2) 0.024 Uiso 1 1 d D . . N1 N 0.2600(2) 0.2500 0.01244(19) 0.0177(3) Uani 1 2 d S . . N2 N 0.1092(2) 0.2500 -0.1455(2) 0.0238(3) Uani 1 2 d SD . . H1N H -0.013(3) 0.2500 -0.158(4) 0.029 Uiso 1 2 d SD . . C1 C 0.1782(3) 0.2500 -0.2679(3) 0.0278(4) Uani 1 2 d S . . H1 H 0.1001 0.2500 -0.3882 0.033 Uiso 1 2 calc SR . . C2 C 0.3832(3) 0.2500 -0.1879(3) 0.0261(4) Uani 1 2 d S . . H2 H 0.4740 0.2500 -0.2409 0.031 Uiso 1 2 calc SR . . C3 C 0.4285(3) 0.2500 -0.0128(3) 0.0244(4) Uani 1 2 d S . . H3 H 0.5591 0.2500 0.0759 0.029 Uiso 1 2 calc SR . . 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 0.01324(8) 0.01510(8) 0.01221(8) 0.000 0.00377(5) 0.000 O1 0.0153(6) 0.0287(7) 0.0181(6) 0.000 0.0051(5) 0.000 O2 0.0235(4) 0.0165(4) 0.0226(4) -0.0015(3) 0.0098(4) 0.0003(4) O3 0.0266(4) 0.0216(5) 0.0173(4) 0.0028(4) 0.0090(4) 0.0005(4) O4 0.0161(6) 0.0186(6) 0.0199(6) 0.000 0.0015(5) 0.000 N1 0.0150(6) 0.0223(7) 0.0148(6) 0.000 0.0053(5) 0.000 N2 0.0160(7) 0.0397(10) 0.0144(7) 0.000 0.0051(6) 0.000 C1 0.0264(10) 0.0409(13) 0.0184(9) 0.000 0.0116(8) 0.000 C2 0.0239(9) 0.0331(11) 0.0263(9) 0.000 0.0154(8) 0.000 C3 0.0170(8) 0.0335(10) 0.0237(9) 0.000 0.0091(7) 0.000 _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 1.6819(15) . ? Mo1 O3 1.9450(10) 4_565 ? Mo1 O3 1.9450(10) . ? Mo1 O2 1.9482(11) 4_565 ? Mo1 O2 1.9482(11) . ? Mo1 N1 2.1673(16) . ? Mo1 O4 2.3224(15) . ? O2 O3 1.4796(13) . ? O4 H1O 0.834(14) . ? N1 C3 1.346(2) . ? N1 N2 1.351(2) . ? N2 C1 1.338(2) . ? N2 H1N 0.863(17) . ? C1 C2 1.380(3) . ? C1 H1 0.9500 . ? C2 C3 1.393(3) . ? C2 H2 0.9500 . ? C3 H3 0.9500 . ? 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 O3 103.34(5) . 4_565 ? O1 Mo1 O3 103.34(5) . . ? O3 Mo1 O3 90.73(6) 4_565 . ? O1 Mo1 O2 102.64(3) . 4_565 ? O3 Mo1 O2 44.67(4) 4_565 4_565 ? O3 Mo1 O2 132.52(4) . 4_565 ? O1 Mo1 O2 102.64(3) . . ? O3 Mo1 O2 132.52(4) 4_565 . ? O3 Mo1 O2 44.67(4) . . ? O2 Mo1 O2 154.07(6) 4_565 . ? O1 Mo1 N1 89.73(7) . . ? O3 Mo1 N1 131.66(3) 4_565 . ? O3 Mo1 N1 131.66(3) . . ? O2 Mo1 N1 87.22(3) 4_565 . ? O2 Mo1 N1 87.22(3) . . ? O1 Mo1 O4 169.23(6) . . ? O3 Mo1 O4 84.12(5) 4_565 . ? O3 Mo1 O4 84.12(5) . . ? O2 Mo1 O4 77.04(3) 4_565 . ? O2 Mo1 O4 77.04(3) . . ? N1 Mo1 O4 79.49(6) . . ? O3 O2 Mo1 67.55(6) . . ? O2 O3 Mo1 67.78(5) . . ? Mo1 O4 H1O 117.1(14) . . ? C3 N1 N2 105.97(15) . . ? C3 N1 Mo1 133.78(13) . . ? N2 N1 Mo1 120.25(12) . . ? C1 N2 N1 111.09(16) . . ? C1 N2 H1N 128.1(19) . . ? N1 N2 H1N 120.8(19) . . ? N2 C1 C2 107.70(19) . . ? N2 C1 H1 126.2 . . ? C2 C1 H1 126.2 . . ? C1 C2 C3 105.21(17) . . ? C1 C2 H2 127.4 . . ? C3 C2 H2 127.4 . . ? N1 C3 C2 110.03(18) . . ? N1 C3 H3 125.0 . . ? C2 C3 H3 125.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Mo1 O2 O3 -96.28(8) . . . . ? O3 Mo1 O2 O3 25.48(6) 4_565 . . . ? O2 Mo1 O2 O3 96.77(14) 4_565 . . . ? N1 Mo1 O2 O3 174.62(7) . . . . ? O4 Mo1 O2 O3 94.76(7) . . . . ? O1 Mo1 O3 O2 94.59(7) . . . . ? O3 Mo1 O3 O2 -161.51(4) 4_565 . . . ? O2 Mo1 O3 O2 -143.91(9) 4_565 . . . ? N1 Mo1 O3 O2 -7.21(9) . . . . ? O4 Mo1 O3 O2 -77.51(6) . . . . ? O1 Mo1 N1 C3 180.0 . . . . ? O3 Mo1 N1 C3 72.27(5) 4_565 . . . ? O3 Mo1 N1 C3 -72.27(5) . . . . ? O2 Mo1 N1 C3 77.33(3) 4_565 . . . ? O2 Mo1 N1 C3 -77.33(3) . . . . ? O4 Mo1 N1 C3 0.0 . . . . ? O1 Mo1 N1 N2 0.0 . . . . ? O3 Mo1 N1 N2 -107.73(5) 4_565 . . . ? O3 Mo1 N1 N2 107.73(5) . . . . ? O2 Mo1 N1 N2 -102.67(3) 4_565 . . . ? O2 Mo1 N1 N2 102.67(3) . . . . ? O4 Mo1 N1 N2 180.0 . . . . ? C3 N1 N2 C1 0.0 . . . . ? Mo1 N1 N2 C1 180.0 . . . . ? N1 N2 C1 C2 0.0 . . . . ? N2 C1 C2 C3 0.0 . . . . ? N2 N1 C3 C2 0.0 . . . . ? Mo1 N1 C3 C2 180.0 . . . . ? C1 C2 C3 N1 0.0 . . . . ? 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 N2 H1N O2 0.863(17) 2.249(15) 2.9146(19) 134.0(10) 2 N2 H1N O2 0.863(17) 2.249(15) 2.9146(19) 134.0(10) 3 O4 H1O O2 0.834(14) 2.564(16) 3.2765(18) 144.2(17) 3_656 O4 H1O O3 0.834(14) 2.002(14) 2.8274(15) 170.4(19) 3_656 _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 30.50 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.278 _refine_diff_density_min -0.985 _refine_diff_density_rms 0.100 ###END #========================================================================= # Data for compound [Hdmpz]4[Mo8O22(O2)4(dmpz)2].2H2O # (local labelling as ea09709a) #========================================================================= data_[Hdmpz]4[Mo8O22(O2)4(dmpz)2].2H2O _database_code_depnum_ccdc_archive 'CCDC 852986' #TrackingRef '- Global_Cif_with_all_2_New_structures_in_one.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H16 Mo8 N4 O30, C10 H18 N4, 2(C5 H9 N2), 2(H2 O)' _chemical_formula_sum 'C30 H56 Mo8 N12 O32' _chemical_formula_weight 1864.39 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 C2/c _symmetry_space_group_name_Hall '-C 2yc' 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 21.4186(10) _cell_length_b 11.9572(6) _cell_length_c 23.9117(11) _cell_angle_alpha 90.00 _cell_angle_beta 101.8640(10) _cell_angle_gamma 90.00 _cell_volume 5993.1(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6039 _cell_measurement_theta_min 2.49 _cell_measurement_theta_max 24.77 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.066 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3648 _exptl_absorpt_coefficient_mu 1.712 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8456 _exptl_absorpt_correction_T_max 0.8895 _exptl_absorpt_process_details ; program SADABS, Bruker (2001). ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Bruker-Nonius X8kappa APEX II CCD area detector ; _diffrn_measurement_method 'phi and omega scans with narrow frames' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_decay_% 0 _diffrn_reflns_number 54187 _diffrn_reflns_av_R_equivalents 0.0737 _diffrn_reflns_av_sigmaI/netI 0.0559 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 30.53 _reflns_number_total 8816 _reflns_number_gt 5255 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 Software Suite (Bruker, 2007)' _computing_cell_refinement 'APEX2 Software Suite (Bruker, 2007)' _computing_data_reduction 'APEX2 Software Suite (Bruker, 2007)' _computing_structure_solution 'SIR2002 (Burla et al., 2003)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL and publCIF (Westrip, 2010)' _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. The asymmetric unit of the structure is formed by the compounds [Hdmpz]4[Mo8O22(O2)4(dmpz)2].2H2O. All non-hydrogen atoms were refined with anisotropic displacement parameters. The hydrogen atoms were included from calculated positions and refined riding on their respective carbon atoms with isotropic displacement parameters. Some geometric restrains (DFIX commands) were needed to maintain reasonable O-H bond and H-O-H angles for the water molecules. The highest residual peaks, those with 1.09 e/ \%A^3^ and 2.77 e/ \%A^3^, were located close to the molybdenum metal center and have no chemical sense. ; _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^)+(0.1380P)^2^+6.9649P] 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 8816 _refine_ls_number_parameters 428 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1241 _refine_ls_R_factor_gt 0.0595 _refine_ls_wR_factor_ref 0.2055 _refine_ls_wR_factor_gt 0.1517 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.019 _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 Mo1 Mo 0.19416(5) 0.82065(7) 0.14062(4) 0.0380(2) Uani 1 1 d U . . Mo2 Mo 0.33399(4) 0.88754(7) 0.11677(3) 0.0320(2) Uani 1 1 d U . . Mo3 Mo 0.24353(3) 0.64911(6) 0.05245(3) 0.02301(18) Uani 1 1 d U . . Mo4 Mo 0.38573(3) 0.73915(6) 0.02072(4) 0.02885(19) Uani 1 1 d U . . O1 O 0.2247(5) 0.8326(8) 0.2104(3) 0.067(2) Uani 1 1 d U . . O2 O 0.1328(5) 0.9393(8) 0.1224(5) 0.071(2) Uani 1 1 d U . . O3 O 0.1040(5) 0.8461(9) 0.1346(5) 0.075(3) Uani 1 1 d U . . O4 O 0.1704(3) 0.7628(5) 0.0551(3) 0.0280(12) Uani 1 1 d U . . O5 O 0.2709(3) 0.7253(5) 0.1233(3) 0.0322(12) Uani 1 1 d U . . O6 O 0.2482(3) 0.9347(5) 0.1123(3) 0.0349(13) Uani 1 1 d U . . O7 O 0.3002(3) 0.8228(5) 0.0269(2) 0.0227(11) Uani 1 1 d U . . O8 O 0.3925(3) 0.7727(6) 0.1027(3) 0.0350(13) Uani 1 1 d U . . O9 O 0.3646(3) 1.0071(6) 0.0938(3) 0.0435(17) Uani 1 1 d U . . O10 O 0.3616(4) 0.8854(6) 0.1897(3) 0.0501(19) Uani 1 1 d U . . O11 O 0.2096(3) 0.5295(5) 0.0686(3) 0.0309(13) Uani 1 1 d U . . O12 O 0.3163(3) 0.6051(5) 0.0390(3) 0.0309(12) Uani 1 1 d U . . O13 O 0.4239(5) 0.6119(7) -0.0079(5) 0.068(2) Uani 1 1 d U . . O14 O 0.4472(4) 0.6305(8) 0.0491(5) 0.069(2) Uani 1 1 d U . . O15 O 0.4312(3) 0.8455(6) 0.0055(3) 0.0403(16) Uani 1 1 d U . . N1 N 0.1591(5) 0.6539(8) 0.1568(4) 0.0434(18) Uani 1 1 d U . . N2 N 0.1053(4) 0.6137(8) 0.1193(4) 0.0427(19) Uani 1 1 d U . . H2N H 0.0827 0.6524 0.0909 0.051 Uiso 1 1 calc R . . C1 C 0.1783(7) 0.5705(10) 0.1928(5) 0.054(3) Uani 1 1 d U . . C2 C 0.1395(7) 0.4798(11) 0.1802(5) 0.058(3) Uani 1 1 d U . . H2 H 0.1435 0.4105 0.2001 0.070 Uiso 1 1 calc R . . C3 C 0.0925(6) 0.5082(10) 0.1323(5) 0.050(3) Uani 1 1 d U . . C4 C 0.2359(8) 0.5844(12) 0.2401(6) 0.078(5) Uani 1 1 d U . . H4A H 0.2704 0.6190 0.2249 0.117 Uiso 1 1 calc R . . H4B H 0.2498 0.5110 0.2562 0.117 Uiso 1 1 calc R . . H4C H 0.2251 0.6322 0.2700 0.117 Uiso 1 1 calc R . . C5 C 0.0377(6) 0.4468(12) 0.0964(6) 0.064(3) Uani 1 1 d U . . H5A H 0.0139 0.4974 0.0675 0.096 Uiso 1 1 calc R . . H5B H 0.0094 0.4191 0.1208 0.096 Uiso 1 1 calc R . . H5C H 0.0539 0.3835 0.0775 0.096 Uiso 1 1 calc R . . N3 N 0.1881(5) 0.1089(8) 0.0555(5) 0.053(2) Uani 1 1 d U . . H3N H 0.2100 0.0537 0.0745 0.063 Uiso 1 1 calc R . . N4 N 0.1333(4) 0.0966(7) 0.0184(5) 0.048(2) Uani 1 1 d U . . H4 H 0.1135 0.0327 0.0088 0.058 Uiso 1 1 calc R . . C6 C 0.2056(6) 0.2169(10) 0.0603(6) 0.053(3) Uani 1 1 d U . . C7 C 0.1571(6) 0.2737(10) 0.0250(6) 0.053(3) Uani 1 1 d U . . H7 H 0.1547 0.3526 0.0204 0.064 Uiso 1 1 calc R . . C8 C 0.1127(5) 0.1981(9) -0.0025(6) 0.050(2) Uani 1 1 d U . . C9 C 0.2657(8) 0.2529(12) 0.0999(7) 0.076(4) Uani 1 1 d U . . H9A H 0.2557 0.2797 0.1357 0.114 Uiso 1 1 calc R . . H9B H 0.2857 0.3132 0.0820 0.114 Uiso 1 1 calc R . . H9C H 0.2951 0.1893 0.1077 0.114 Uiso 1 1 calc R . . C10 C 0.0522(6) 0.2147(14) -0.0434(8) 0.079(4) Uani 1 1 d U . . H10A H 0.0235 0.2605 -0.0258 0.118 Uiso 1 1 calc R . . H10B H 0.0322 0.1420 -0.0543 0.118 Uiso 1 1 calc R . . H10C H 0.0603 0.2528 -0.0775 0.118 Uiso 1 1 calc R . . N5A N 0.4146(8) 0.6493(13) 0.1965(5) 0.042(4) Uani 0.50 1 d PGU A 1 H5A1 H 0.4155 0.6781 0.1628 0.050 Uiso 0.50 1 calc PR A 1 N6A N 0.4358(7) 0.7026(10) 0.2501(6) 0.041(4) Uani 0.50 1 d PGU A 1 H6A H 0.4522 0.7702 0.2555 0.049 Uiso 0.50 1 calc PR A 1 C13A C 0.4259(9) 0.6277(14) 0.2936(5) 0.050(5) Uani 0.50 1 d PGU A 1 C14A C 0.3986(8) 0.5281(13) 0.2668(6) 0.044(5) Uani 0.50 1 d PGU A 1 H14A H 0.3871 0.4638 0.2857 0.053 Uiso 0.50 1 calc PR A 1 C15A C 0.3916(8) 0.5414(12) 0.2068(6) 0.039(4) Uani 0.50 1 d PGU A 1 C16A C 0.444(2) 0.668(4) 0.3528(12) 0.070(10) Uani 0.50 1 d PU A 1 H16A H 0.4652 0.7404 0.3535 0.104 Uiso 0.50 1 calc PR A 1 H16B H 0.4724 0.6139 0.3758 0.104 Uiso 0.50 1 calc PR A 1 H16C H 0.4051 0.6764 0.3686 0.104 Uiso 0.50 1 calc PR A 1 C17A C 0.3666(17) 0.470(3) 0.1580(11) 0.080(9) Uani 0.50 1 d PU A 1 H17A H 0.3912 0.4000 0.1613 0.120 Uiso 0.50 1 calc PR A 1 H17B H 0.3702 0.5082 0.1226 0.120 Uiso 0.50 1 calc PR A 1 H17C H 0.3217 0.4526 0.1573 0.120 Uiso 0.50 1 calc PR A 1 N5B N 0.4052(8) 0.6224(14) 0.1816(5) 0.050(5) Uani 0.50 1 d PGU B 2 H5B1 H 0.3978 0.6495 0.1467 0.060 Uiso 0.50 1 calc PR B 2 N6B N 0.4035(8) 0.6837(11) 0.2322(7) 0.050(4) Uani 0.50 1 d PGU B 2 H6B H 0.3948 0.7554 0.2340 0.059 Uiso 0.50 1 calc PR B 2 C13B C 0.4182(9) 0.6089(14) 0.2792(5) 0.044(5) Uani 0.50 1 d PGU B 2 C14B C 0.4290(8) 0.5015(12) 0.2577(7) 0.045(4) Uani 0.50 1 d PGU B 2 H14B H 0.4397 0.4356 0.2798 0.054 Uiso 0.50 1 calc PR B 2 C15B C 0.4210(9) 0.5098(12) 0.1974(6) 0.046(4) Uani 0.50 1 d PGU B 2 C16B C 0.425(2) 0.655(3) 0.3361(12) 0.062(9) Uani 0.50 1 d PU B 2 H16D H 0.4565 0.7152 0.3414 0.093 Uiso 0.50 1 calc PR B 2 H16E H 0.4391 0.5958 0.3644 0.093 Uiso 0.50 1 calc PR B 2 H16F H 0.3837 0.6842 0.3411 0.093 Uiso 0.50 1 calc PR B 2 C17B C 0.4302(15) 0.435(3) 0.1504(12) 0.065(7) Uani 0.50 1 d PU B 2 H17D H 0.4734 0.4446 0.1436 0.098 Uiso 0.50 1 calc PR B 2 H17E H 0.3990 0.4535 0.1156 0.098 Uiso 0.50 1 calc PR B 2 H17F H 0.4243 0.3570 0.1610 0.098 Uiso 0.50 1 calc PR B 2 O16 O 0.5000 0.8903(13) 0.2500 0.085(5) Uani 1 2 d SD . . H16X H 0.4661 0.9387 0.2500 0.103 Uiso 0.50 1 d PRD . . H16Y H 0.5353 0.9346 0.2679 0.103 Uiso 0.50 1 d PRD . . O17 O 0.5299(8) 0.0747(17) 0.3092(10) 0.078(6) Uani 0.50 1 d PD . . H17X H 0.5134 0.1335 0.2735 0.093 Uiso 0.50 1 d PRD . . H17Y H 0.5475 0.1373 0.3356 0.093 Uiso 0.50 1 d PRD . . 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 0.0573(5) 0.0314(4) 0.0309(4) -0.0109(3) 0.0222(4) -0.0104(4) Mo2 0.0394(4) 0.0251(4) 0.0268(4) -0.0027(3) -0.0037(3) -0.0046(3) Mo3 0.0299(3) 0.0182(3) 0.0199(3) -0.0013(2) 0.0028(3) -0.0024(3) Mo4 0.0259(3) 0.0239(4) 0.0360(4) 0.0021(3) 0.0047(3) -0.0004(3) O1 0.125(7) 0.051(5) 0.033(3) -0.019(3) 0.032(4) -0.030(5) O2 0.074(5) 0.058(5) 0.094(7) -0.020(5) 0.046(5) 0.010(4) O3 0.082(5) 0.071(6) 0.087(7) -0.013(5) 0.054(5) 0.013(4) O4 0.037(3) 0.024(3) 0.025(3) -0.004(2) 0.011(2) -0.004(2) O5 0.043(3) 0.030(3) 0.022(3) -0.003(2) 0.004(2) -0.008(2) O6 0.053(3) 0.022(3) 0.030(3) -0.005(2) 0.010(3) -0.006(3) O7 0.028(2) 0.018(3) 0.021(2) 0.001(2) 0.002(2) 0.001(2) O8 0.034(3) 0.031(3) 0.034(3) 0.008(2) -0.010(2) -0.002(2) O9 0.042(4) 0.030(3) 0.053(4) 0.000(3) 0.000(3) -0.010(3) O10 0.077(5) 0.035(4) 0.030(3) -0.008(3) -0.010(3) -0.009(4) O11 0.043(3) 0.020(3) 0.031(3) -0.001(2) 0.010(3) -0.007(2) O12 0.046(3) 0.016(3) 0.030(3) 0.002(2) 0.008(3) -0.003(2) O13 0.070(6) 0.031(4) 0.117(7) 0.009(5) 0.051(5) 0.011(4) O14 0.056(4) 0.041(5) 0.116(7) 0.021(5) 0.031(5) 0.015(4) O15 0.034(3) 0.031(3) 0.055(4) 0.003(3) 0.008(3) -0.005(3) N1 0.064(5) 0.044(4) 0.029(4) -0.003(3) 0.026(4) -0.020(4) N2 0.056(5) 0.039(4) 0.037(4) -0.005(3) 0.019(4) -0.012(4) C1 0.083(7) 0.047(6) 0.034(5) 0.004(4) 0.015(4) -0.023(5) C2 0.093(8) 0.049(6) 0.035(5) 0.008(4) 0.019(5) -0.026(6) C3 0.068(6) 0.046(6) 0.042(6) -0.004(4) 0.026(4) -0.021(5) C4 0.119(11) 0.053(8) 0.051(8) 0.015(6) -0.009(7) -0.028(8) C5 0.075(8) 0.053(8) 0.065(8) -0.004(6) 0.018(6) -0.029(6) N3 0.066(5) 0.031(4) 0.069(7) 0.005(4) 0.033(4) 0.007(4) N4 0.047(4) 0.025(4) 0.082(7) 0.002(4) 0.034(4) 0.000(3) C6 0.067(6) 0.035(5) 0.065(7) -0.003(5) 0.031(5) -0.001(4) C7 0.063(6) 0.026(4) 0.078(8) 0.003(5) 0.030(5) 0.004(4) C8 0.050(5) 0.027(5) 0.083(8) 0.003(5) 0.035(4) 0.006(4) C9 0.103(10) 0.046(7) 0.070(9) -0.001(6) -0.002(7) -0.010(7) C10 0.050(6) 0.073(10) 0.116(13) 0.015(8) 0.024(6) 0.017(6) N5A 0.047(9) 0.045(9) 0.028(7) 0.009(7) -0.004(7) -0.005(8) N6A 0.040(8) 0.044(8) 0.034(8) 0.012(6) -0.006(7) 0.002(7) C13A 0.060(12) 0.048(11) 0.034(7) 0.012(7) -0.007(9) -0.014(10) C14A 0.056(12) 0.042(10) 0.027(7) 0.011(7) -0.010(8) -0.007(9) C15A 0.045(10) 0.040(9) 0.027(7) 0.015(6) -0.004(7) 0.002(7) C16A 0.10(3) 0.08(2) 0.026(9) 0.006(10) -0.003(14) -0.028(18) C17A 0.12(2) 0.062(14) 0.034(10) 0.007(9) -0.027(14) -0.026(16) N5B 0.055(11) 0.054(10) 0.039(8) 0.002(7) 0.006(9) -0.001(9) N6B 0.066(11) 0.047(8) 0.033(8) 0.013(6) 0.006(9) 0.006(9) C13B 0.055(11) 0.050(10) 0.028(7) 0.016(6) 0.010(9) 0.005(10) C14B 0.044(10) 0.049(8) 0.037(7) 0.005(6) -0.003(8) -0.004(9) C15B 0.049(11) 0.048(9) 0.037(8) 0.002(7) -0.001(8) -0.011(9) C16B 0.10(3) 0.058(16) 0.036(10) 0.006(10) 0.026(16) -0.001(17) C17B 0.081(17) 0.064(14) 0.054(12) -0.005(11) 0.022(13) -0.002(14) O16 0.051(7) 0.072(10) 0.115(13) 0.000 -0.026(8) 0.000 O17 0.060(11) 0.053(12) 0.105(17) -0.001(11) -0.019(11) 0.015(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 O1 1.668(8) . ? Mo1 O2 1.922(10) . ? Mo1 O3 1.930(10) . ? Mo1 O6 1.995(7) . ? Mo1 O5 2.110(7) . ? Mo1 O4 2.118(6) . ? Mo1 N1 2.193(9) . ? Mo2 O9 1.710(7) . ? Mo2 O10 1.722(7) . ? Mo2 O6 1.904(7) . ? Mo2 O8 1.935(7) . ? Mo2 O7 2.258(5) . ? Mo2 O5 2.387(6) . ? Mo3 O11 1.684(6) . ? Mo3 O12 1.737(7) . ? Mo3 O5 1.907(6) . ? Mo3 O7 1.965(5) 7_565 ? Mo3 O4 2.085(6) . ? Mo4 O15 1.687(7) . ? Mo4 O14 1.874(9) . ? Mo4 O13 1.919(9) . ? Mo4 O4 1.960(6) 7_565 ? Mo4 O8 1.976(7) . ? Mo4 O7 2.119(6) . ? Mo4 O12 2.289(6) . ? O2 O3 1.336(14) . ? O4 Mo4 1.960(6) 7_565 ? O7 Mo3 1.965(5) 7_565 ? O13 O14 1.370(15) . ? N1 C1 1.326(15) . ? N1 N2 1.392(12) . ? N2 C3 1.341(14) . ? N2 H2N 0.8800 . ? C1 C2 1.362(16) . ? C1 C4 1.502(18) . ? C2 C3 1.403(17) . ? C2 H2 0.9500 . ? C3 C5 1.496(16) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? N3 N4 1.327(15) . ? N3 C6 1.343(15) . ? N3 H3N 0.8800 . ? N4 C8 1.352(14) . ? N4 H4 0.8800 . ? C6 C7 1.375(18) . ? C6 C9 1.495(19) . ? C7 C8 1.378(17) . ? C7 H7 0.9500 . ? C8 C10 1.468(19) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? N5A C15A 1.4200 . ? N5A N6A 1.4200 . ? N5A H5A1 0.8800 . ? N6A C13A 1.4200 . ? N6A H6A 0.8800 . ? C13A C14A 1.4200 . ? C13A C16A 1.47(3) . ? C14A C15A 1.4200 . ? C14A H14A 0.9500 . ? C15A C17A 1.46(3) . ? C16A H16A 0.9800 . ? C16A H16B 0.9800 . ? C16A H16C 0.9800 . ? C17A H17A 0.9800 . ? C17A H17B 0.9800 . ? C17A H17C 0.9800 . ? N5B N6B 1.4200 . ? N5B C15B 1.4200 . ? N5B H5B1 0.8800 . ? N6B C13B 1.4200 . ? N6B H6B 0.8800 . ? C13B C14B 1.4200 . ? C13B C16B 1.45(3) . ? C14B C15B 1.4200 . ? C14B H14B 0.9500 . ? C15B C17B 1.48(3) . ? C16B H16D 0.9800 . ? C16B H16E 0.9800 . ? C16B H16F 0.9800 . ? C17B H17D 0.9800 . ? C17B H17E 0.9800 . ? C17B H17F 0.9800 . ? O16 H16X 0.9285 . ? O16 H16Y 0.9501 . ? O17 H17X 1.1079 . ? O17 H17Y 1.0012 . ? 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 O2 105.9(5) . . ? O1 Mo1 O3 104.0(5) . . ? O2 Mo1 O3 40.6(4) . . ? O1 Mo1 O6 98.4(4) . . ? O2 Mo1 O6 80.5(4) . . ? O3 Mo1 O6 120.6(4) . . ? O1 Mo1 O5 94.6(4) . . ? O2 Mo1 O5 151.4(4) . . ? O3 Mo1 O5 151.4(4) . . ? O6 Mo1 O5 76.8(3) . . ? O1 Mo1 O4 163.7(4) . . ? O2 Mo1 O4 90.3(4) . . ? O3 Mo1 O4 86.6(4) . . ? O6 Mo1 O4 86.3(2) . . ? O5 Mo1 O4 71.1(2) . . ? O1 Mo1 N1 88.8(4) . . ? O2 Mo1 N1 117.9(4) . . ? O3 Mo1 N1 77.4(4) . . ? O6 Mo1 N1 157.7(3) . . ? O5 Mo1 N1 81.5(3) . . ? O4 Mo1 N1 81.4(3) . . ? O9 Mo2 O10 105.3(4) . . ? O9 Mo2 O6 99.5(3) . . ? O10 Mo2 O6 100.9(4) . . ? O9 Mo2 O8 103.4(3) . . ? O10 Mo2 O8 93.8(3) . . ? O6 Mo2 O8 148.5(3) . . ? O9 Mo2 O7 92.8(3) . . ? O10 Mo2 O7 159.1(3) . . ? O6 Mo2 O7 86.0(2) . . ? O8 Mo2 O7 71.6(2) . . ? O9 Mo2 O5 163.7(3) . . ? O10 Mo2 O5 90.2(3) . . ? O6 Mo2 O5 72.0(2) . . ? O8 Mo2 O5 80.2(3) . . ? O7 Mo2 O5 73.1(2) . . ? O11 Mo3 O12 103.4(3) . . ? O11 Mo3 O5 105.7(3) . . ? O12 Mo3 O5 100.7(3) . . ? O11 Mo3 O7 102.9(3) . 7_565 ? O12 Mo3 O7 98.1(3) . 7_565 ? O5 Mo3 O7 140.8(3) . 7_565 ? O11 Mo3 O4 100.6(3) . . ? O12 Mo3 O4 155.8(3) . . ? O5 Mo3 O4 75.9(3) . . ? O7 Mo3 O4 72.9(2) 7_565 . ? O15 Mo4 O14 101.9(4) . . ? O15 Mo4 O13 102.3(4) . . ? O14 Mo4 O13 42.3(4) . . ? O15 Mo4 O4 94.6(3) . 7_565 ? O14 Mo4 O4 125.3(4) . 7_565 ? O13 Mo4 O4 83.4(4) . 7_565 ? O15 Mo4 O8 97.7(3) . . ? O14 Mo4 O8 83.0(4) . . ? O13 Mo4 O8 124.4(4) . . ? O4 Mo4 O8 145.7(3) 7_565 . ? O15 Mo4 O7 101.8(3) . . ? O14 Mo4 O7 148.7(4) . . ? O13 Mo4 O7 146.8(4) . . ? O4 Mo4 O7 72.3(2) 7_565 . ? O8 Mo4 O7 73.9(2) . . ? O15 Mo4 O12 174.9(3) . . ? O14 Mo4 O12 83.2(3) . . ? O13 Mo4 O12 81.6(3) . . ? O4 Mo4 O12 82.5(2) 7_565 . ? O8 Mo4 O12 82.5(2) . . ? O7 Mo4 O12 73.3(2) . . ? O3 O2 Mo1 70.1(6) . . ? O2 O3 Mo1 69.4(6) . . ? Mo4 O4 Mo3 106.6(3) 7_565 . ? Mo4 O4 Mo1 151.3(3) 7_565 . ? Mo3 O4 Mo1 102.1(3) . . ? Mo3 O5 Mo1 108.8(3) . . ? Mo3 O5 Mo2 113.9(3) . . ? Mo1 O5 Mo2 92.8(2) . . ? Mo2 O6 Mo1 113.5(3) . . ? Mo3 O7 Mo4 105.1(3) 7_565 . ? Mo3 O7 Mo2 148.9(3) 7_565 . ? Mo4 O7 Mo2 96.7(2) . . ? Mo2 O8 Mo4 113.5(3) . . ? Mo3 O12 Mo4 117.8(3) . . ? O14 O13 Mo4 67.1(5) . . ? O13 O14 Mo4 70.6(6) . . ? C1 N1 N2 105.3(9) . . ? C1 N1 Mo1 136.5(8) . . ? N2 N1 Mo1 117.9(7) . . ? C3 N2 N1 110.9(10) . . ? C3 N2 H2N 124.5 . . ? N1 N2 H2N 124.5 . . ? N1 C1 C2 111.2(11) . . ? N1 C1 C4 120.2(11) . . ? C2 C1 C4 128.6(12) . . ? C1 C2 C3 106.9(11) . . ? C1 C2 H2 126.6 . . ? C3 C2 H2 126.6 . . ? N2 C3 C2 105.7(10) . . ? N2 C3 C5 120.2(12) . . ? C2 C3 C5 134.1(11) . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N4 N3 C6 110.9(10) . . ? N4 N3 H3N 124.5 . . ? C6 N3 H3N 124.5 . . ? N3 N4 C8 108.9(10) . . ? N3 N4 H4 125.5 . . ? C8 N4 H4 125.5 . . ? N3 C6 C7 105.1(12) . . ? N3 C6 C9 121.3(12) . . ? C7 C6 C9 133.6(12) . . ? C6 C7 C8 109.3(11) . . ? C6 C7 H7 125.4 . . ? C8 C7 H7 125.4 . . ? N4 C8 C7 105.8(11) . . ? N4 C8 C10 122.9(12) . . ? C7 C8 C10 131.2(12) . . ? C6 C9 H9A 109.5 . . ? C6 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C6 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C15A N5A N6A 108.0 . . ? C15A N5A H5A1 126.0 . . ? N6A N5A H5A1 126.0 . . ? C13A N6A N5A 108.0 . . ? C13A N6A H6A 126.0 . . ? N5A N6A H6A 126.0 . . ? N6A C13A C14A 108.0 . . ? N6A C13A C16A 116.8(19) . . ? C14A C13A C16A 135.2(19) . . ? C15A C14A C13A 108.0 . . ? C15A C14A H14A 126.0 . . ? C13A C14A H14A 126.0 . . ? N5A C15A C14A 108.0 . . ? N5A C15A C17A 118.6(15) . . ? C14A C15A C17A 133.4(15) . . ? N6B N5B C15B 108.0 . . ? N6B N5B H5B1 126.0 . . ? C15B N5B H5B1 126.0 . . ? N5B N6B C13B 108.0 . . ? N5B N6B H6B 126.0 . . ? C13B N6B H6B 126.0 . . ? C14B C13B N6B 108.0 . . ? C14B C13B C16B 133.7(18) . . ? N6B C13B C16B 118.0(18) . . ? C13B C14B C15B 108.0 . . ? C13B C14B H14B 126.0 . . ? C15B C14B H14B 126.0 . . ? N5B C15B C14B 108.0 . . ? N5B C15B C17B 115.7(16) . . ? C14B C15B C17B 136.1(17) . . ? C13B C16B H16D 109.5 . . ? C13B C16B H16E 109.5 . . ? H16D C16B H16E 109.5 . . ? C13B C16B H16F 109.5 . . ? H16D C16B H16F 109.5 . . ? H16E C16B H16F 109.5 . . ? C15B C17B H17D 109.5 . . ? C15B C17B H17E 109.5 . . ? H17D C17B H17E 109.5 . . ? C15B C17B H17F 109.5 . . ? H17D C17B H17F 109.5 . . ? H17E C17B H17F 109.5 . . ? H16X O16 H16Y 101.6 . . ? H17X O17 H17Y 91.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Mo1 O2 O3 -93.2(7) . . . . ? O6 Mo1 O2 O3 170.8(7) . . . . ? O5 Mo1 O2 O3 132.7(7) . . . . ? O4 Mo1 O2 O3 84.5(6) . . . . ? N1 Mo1 O2 O3 4.1(8) . . . . ? O1 Mo1 O3 O2 98.2(7) . . . . ? O6 Mo1 O3 O2 -10.6(8) . . . . ? O5 Mo1 O3 O2 -132.7(8) . . . . ? O4 Mo1 O3 O2 -94.4(6) . . . . ? N1 Mo1 O3 O2 -176.3(7) . . . . ? O11 Mo3 O4 Mo4 -86.2(3) . . . 7_565 ? O12 Mo3 O4 Mo4 85.4(7) . . . 7_565 ? O5 Mo3 O4 Mo4 170.1(3) . . . 7_565 ? O7 Mo3 O4 Mo4 14.2(2) 7_565 . . 7_565 ? O11 Mo3 O4 Mo1 92.8(3) . . . . ? O12 Mo3 O4 Mo1 -95.6(7) . . . . ? O5 Mo3 O4 Mo1 -10.9(3) . . . . ? O7 Mo3 O4 Mo1 -166.8(3) 7_565 . . . ? O1 Mo1 O4 Mo4 158.0(12) . . . 7_565 ? O2 Mo1 O4 Mo4 -14.0(7) . . . 7_565 ? O3 Mo1 O4 Mo4 26.4(7) . . . 7_565 ? O6 Mo1 O4 Mo4 -94.5(7) . . . 7_565 ? O5 Mo1 O4 Mo4 -171.9(7) . . . 7_565 ? N1 Mo1 O4 Mo4 104.2(7) . . . 7_565 ? O1 Mo1 O4 Mo3 -20.1(14) . . . . ? O2 Mo1 O4 Mo3 167.9(4) . . . . ? O3 Mo1 O4 Mo3 -151.6(4) . . . . ? O6 Mo1 O4 Mo3 87.4(3) . . . . ? O5 Mo1 O4 Mo3 10.1(2) . . . . ? N1 Mo1 O4 Mo3 -73.8(3) . . . . ? O11 Mo3 O5 Mo1 -86.0(3) . . . . ? O12 Mo3 O5 Mo1 166.7(3) . . . . ? O7 Mo3 O5 Mo1 49.5(5) 7_565 . . . ? O4 Mo3 O5 Mo1 11.3(3) . . . . ? O11 Mo3 O5 Mo2 172.1(3) . . . . ? O12 Mo3 O5 Mo2 64.8(4) . . . . ? O7 Mo3 O5 Mo2 -52.5(5) 7_565 . . . ? O4 Mo3 O5 Mo2 -90.6(3) . . . . ? O1 Mo1 O5 Mo3 160.4(4) . . . . ? O2 Mo1 O5 Mo3 -63.4(8) . . . . ? O3 Mo1 O5 Mo3 29.4(9) . . . . ? O6 Mo1 O5 Mo3 -102.0(3) . . . . ? O4 Mo1 O5 Mo3 -11.4(3) . . . . ? N1 Mo1 O5 Mo3 72.3(4) . . . . ? O1 Mo1 O5 Mo2 -83.1(3) . . . . ? O2 Mo1 O5 Mo2 53.1(8) . . . . ? O3 Mo1 O5 Mo2 145.9(7) . . . . ? O6 Mo1 O5 Mo2 14.4(2) . . . . ? O4 Mo1 O5 Mo2 105.0(3) . . . . ? N1 Mo1 O5 Mo2 -171.2(3) . . . . ? O9 Mo2 O5 Mo3 36.2(12) . . . . ? O10 Mo2 O5 Mo3 -162.1(4) . . . . ? O6 Mo2 O5 Mo3 96.6(4) . . . . ? O8 Mo2 O5 Mo3 -68.3(3) . . . . ? O7 Mo2 O5 Mo3 5.3(3) . . . . ? O9 Mo2 O5 Mo1 -75.9(11) . . . . ? O10 Mo2 O5 Mo1 85.9(3) . . . . ? O6 Mo2 O5 Mo1 -15.5(2) . . . . ? O8 Mo2 O5 Mo1 179.7(3) . . . . ? O7 Mo2 O5 Mo1 -106.8(2) . . . . ? O9 Mo2 O6 Mo1 -176.4(4) . . . . ? O10 Mo2 O6 Mo1 -68.7(4) . . . . ? O8 Mo2 O6 Mo1 47.4(7) . . . . ? O7 Mo2 O6 Mo1 91.4(3) . . . . ? O5 Mo2 O6 Mo1 17.9(3) . . . . ? O1 Mo1 O6 Mo2 73.0(5) . . . . ? O2 Mo1 O6 Mo2 177.8(4) . . . . ? O3 Mo1 O6 Mo2 -175.2(4) . . . . ? O5 Mo1 O6 Mo2 -19.9(3) . . . . ? O4 Mo1 O6 Mo2 -91.3(3) . . . . ? N1 Mo1 O6 Mo2 -34.7(10) . . . . ? O15 Mo4 O7 Mo3 77.2(3) . . . 7_565 ? O14 Mo4 O7 Mo3 -144.0(7) . . . 7_565 ? O13 Mo4 O7 Mo3 -58.8(7) . . . 7_565 ? O4 Mo4 O7 Mo3 -13.9(2) 7_565 . . 7_565 ? O8 Mo4 O7 Mo3 171.9(3) . . . 7_565 ? O12 Mo4 O7 Mo3 -101.2(3) . . . 7_565 ? O15 Mo4 O7 Mo2 -80.3(3) . . . . ? O14 Mo4 O7 Mo2 58.4(8) . . . . ? O13 Mo4 O7 Mo2 143.7(6) . . . . ? O4 Mo4 O7 Mo2 -171.5(3) 7_565 . . . ? O8 Mo4 O7 Mo2 14.3(2) . . . . ? O12 Mo4 O7 Mo2 101.2(2) . . . . ? O9 Mo2 O7 Mo3 -46.1(6) . . . 7_565 ? O10 Mo2 O7 Mo3 163.5(9) . . . 7_565 ? O6 Mo2 O7 Mo3 53.2(6) . . . 7_565 ? O8 Mo2 O7 Mo3 -149.3(6) . . . 7_565 ? O5 Mo2 O7 Mo3 125.6(6) . . . 7_565 ? O9 Mo2 O7 Mo4 88.4(3) . . . . ? O10 Mo2 O7 Mo4 -62.1(10) . . . . ? O6 Mo2 O7 Mo4 -172.3(3) . . . . ? O8 Mo2 O7 Mo4 -14.8(2) . . . . ? O5 Mo2 O7 Mo4 -99.9(2) . . . . ? O9 Mo2 O8 Mo4 -71.2(4) . . . . ? O10 Mo2 O8 Mo4 -177.9(4) . . . . ? O6 Mo2 O8 Mo4 64.2(7) . . . . ? O7 Mo2 O8 Mo4 17.3(3) . . . . ? O5 Mo2 O8 Mo4 92.6(3) . . . . ? O15 Mo4 O8 Mo2 81.9(4) . . . . ? O14 Mo4 O8 Mo2 -176.9(4) . . . . ? O13 Mo4 O8 Mo2 -167.4(4) . . . . ? O4 Mo4 O8 Mo2 -28.1(7) 7_565 . . . ? O7 Mo4 O8 Mo2 -18.2(3) . . . . ? O12 Mo4 O8 Mo2 -92.9(3) . . . . ? O11 Mo3 O12 Mo4 -175.8(3) . . . . ? O5 Mo3 O12 Mo4 -66.7(4) . . . . ? O7 Mo3 O12 Mo4 78.7(3) 7_565 . . . ? O4 Mo3 O12 Mo4 12.6(9) . . . . ? O14 Mo4 O12 Mo3 154.0(5) . . . . ? O13 Mo4 O12 Mo3 -163.3(5) . . . . ? O4 Mo4 O12 Mo3 -78.9(4) 7_565 . . . ? O8 Mo4 O12 Mo3 70.1(4) . . . . ? O7 Mo4 O12 Mo3 -5.3(3) . . . . ? O15 Mo4 O13 O14 94.3(6) . . . . ? O4 Mo4 O13 O14 -172.4(6) 7_565 . . . ? O8 Mo4 O13 O14 -14.1(7) . . . . ? O7 Mo4 O13 O14 -129.8(7) . . . . ? O12 Mo4 O13 O14 -89.0(5) . . . . ? O15 Mo4 O14 O13 -95.3(6) . . . . ? O4 Mo4 O14 O13 9.3(7) 7_565 . . . ? O8 Mo4 O14 O13 168.3(6) . . . . ? O7 Mo4 O14 O13 126.0(7) . . . . ? O12 Mo4 O14 O13 85.0(5) . . . . ? O1 Mo1 N1 C1 -33.2(12) . . . . ? O2 Mo1 N1 C1 -140.6(12) . . . . ? O3 Mo1 N1 C1 -137.8(12) . . . . ? O6 Mo1 N1 C1 76.3(14) . . . . ? O5 Mo1 N1 C1 61.7(12) . . . . ? O4 Mo1 N1 C1 133.7(12) . . . . ? O1 Mo1 N1 N2 152.9(8) . . . . ? O2 Mo1 N1 N2 45.5(8) . . . . ? O3 Mo1 N1 N2 48.2(8) . . . . ? O6 Mo1 N1 N2 -97.6(11) . . . . ? O5 Mo1 N1 N2 -112.3(7) . . . . ? O4 Mo1 N1 N2 -40.2(7) . . . . ? C1 N1 N2 C3 -0.2(12) . . . . ? Mo1 N1 N2 C3 175.5(7) . . . . ? N2 N1 C1 C2 -0.2(14) . . . . ? Mo1 N1 C1 C2 -174.6(9) . . . . ? N2 N1 C1 C4 -179.7(12) . . . . ? Mo1 N1 C1 C4 6(2) . . . . ? N1 C1 C2 C3 0.5(16) . . . . ? C4 C1 C2 C3 180.0(15) . . . . ? N1 N2 C3 C2 0.5(13) . . . . ? N1 N2 C3 C5 -178.2(10) . . . . ? C1 C2 C3 N2 -0.6(14) . . . . ? C1 C2 C3 C5 177.8(14) . . . . ? C6 N3 N4 C8 -0.3(13) . . . . ? N4 N3 C6 C7 1.9(14) . . . . ? N4 N3 C6 C9 179.7(12) . . . . ? N3 C6 C7 C8 -2.9(14) . . . . ? C9 C6 C7 C8 179.8(15) . . . . ? N3 N4 C8 C7 -1.5(13) . . . . ? N3 N4 C8 C10 -178.0(12) . . . . ? C6 C7 C8 N4 2.7(14) . . . . ? C6 C7 C8 C10 178.8(14) . . . . ? C15A N5A N6A C13A 0.0 . . . . ? N5A N6A C13A C14A 0.0 . . . . ? N5A N6A C13A C16A -179(3) . . . . ? N6A C13A C14A C15A 0.0 . . . . ? C16A C13A C14A C15A 178(3) . . . . ? N6A N5A C15A C14A 0.0 . . . . ? N6A N5A C15A C17A 180(2) . . . . ? C13A C14A C15A N5A 0.0 . . . . ? C13A C14A C15A C17A -180(3) . . . . ? C15B N5B N6B C13B 0.0 . . . . ? N5B N6B C13B C14B 0.0 . . . . ? N5B N6B C13B C16B 175(3) . . . . ? N6B C13B C14B C15B 0.0 . . . . ? C16B C13B C14B C15B -173(3) . . . . ? N6B N5B C15B C14B 0.0 . . . . ? N6B N5B C15B C17B -175(2) . . . . ? C13B C14B C15B N5B 0.0 . . . . ? C13B C14B C15B C17B 174(3) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 30.53 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 2.768 _refine_diff_density_min -2.091 _refine_diff_density_rms 0.454 ###END