Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'R.Dinda' 'P. Sengupta' 'S.Ghosh' 'H. M. Figge' 'W. S. Sheldrick' _publ_contact_author_name 'Prof Saktiprosad Ghosh' _publ_contact_author_address ; Department of Inorganic Chemistry Indian Association for the Cultivation of Science Jadavpur Calcutta-700 032 INDIA ; _publ_contact_author_email 'ICSPG@MAHENDRA.IACS.RES.IN' _publ_requested_journal 'Dalton Transactions' _publ_section_title ; A family of mononuclear molybdenum(VI), and -(IV) oxo complexes with a tridentat (ONO) ligand ; data_rd5 _database_code_CSD 182101 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H13 N3 O2' _chemical_formula_weight 255.27 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 13.181(3) _cell_length_b 6.5000(13) _cell_length_c 14.432(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.63(3) _cell_angle_gamma 90.00 _cell_volume 1225.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 15 _cell_measurement_theta_min 7.5 _cell_measurement_theta_max 15.0 _exptl_crystal_description colourless _exptl_crystal_colour prism _exptl_crystal_size_max 0.63 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.384 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 536 _exptl_absorpt_coefficient_mu 0.096 _exptl_absorpt_correction_type Semi-empirical _exptl_absorpt_correction_T_min 0.86953 _exptl_absorpt_correction_T_max 0.94383 _exptl_absorpt_process_details ? _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 'Siemens P4 4-circle-diffractometer' _diffrn_measurement_method 'Profile fitted' _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 20 _diffrn_reflns_number 1330 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0967 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max -2 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 4.42 _diffrn_reflns_theta_max 22.48 _reflns_number_total 1330 _reflns_number_gt 739 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens P4' _computing_cell_refinement 'Siemens P4' _computing_data_reduction 'XDISK' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL-PLUS (VMS)' _computing_publication_material 'SHELXL-97' _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^)+(0.0566P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1330 _refine_ls_number_parameters 209 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.1335 _refine_ls_R_factor_gt 0.0617 _refine_ls_wR_factor_ref 0.1396 _refine_ls_wR_factor_gt 0.1136 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.0749(3) 0.0089(7) 0.1183(3) 0.0408(12) Uani 1 1 d D . . H1 H 0.121(3) 0.111(6) 0.120(5) 0.09(2) Uiso 1 1 d D . . N2 N -0.0265(3) 0.0405(7) 0.1266(3) 0.0388(11) Uani 1 1 d . . . C2 C 0.1025(3) -0.1912(9) 0.1000(4) 0.0391(14) Uani 1 1 d . . . O2 O 0.0361(2) -0.3234(6) 0.0865(3) 0.0543(11) Uani 1 1 d . . . C21 C 0.2123(3) -0.2310(9) 0.0977(4) 0.0360(14) Uani 1 1 d . . . C22 C 0.2459(3) -0.4210(9) 0.0671(3) 0.0371(13) Uani 1 1 d . . . N22 N 0.1803(3) -0.5818(7) 0.0408(3) 0.0503(12) Uani 1 1 d . . . H221 H 0.2042 -0.6972 0.0241 0.071(13) Uiso 1 1 calc R . . H222 H 0.1156 -0.5668 0.0411 0.071(13) Uiso 1 1 calc R . . C23 C 0.3502(4) -0.4507(9) 0.0658(4) 0.0476(15) Uani 1 1 d D . . H23 H 0.377(3) -0.575(4) 0.047(3) 0.057 Uiso 1 1 d D . . C24 C 0.4209(3) -0.3023(10) 0.0935(4) 0.0610(18) Uani 1 1 d D . . H24 H 0.4903(14) -0.333(9) 0.095(4) 0.073 Uiso 1 1 d D . . C25 C 0.3881(3) -0.1126(11) 0.1263(5) 0.0594(18) Uani 1 1 d D . . H25 H 0.442(3) -0.020(6) 0.142(4) 0.071 Uiso 1 1 d D . . C26 C 0.2861(3) -0.0790(10) 0.1286(4) 0.0467(15) Uani 1 1 d D . . H26 H 0.261(3) 0.044(4) 0.150(4) 0.056 Uiso 1 1 d D . . C3 C -0.0568(3) 0.2208(9) 0.1448(4) 0.0372(13) Uani 1 1 d D . . H3 H -0.012(2) 0.342(4) 0.153(3) 0.031(12) Uiso 1 1 d D . . C31 C -0.1635(3) 0.2485(8) 0.1563(4) 0.0367(14) Uani 1 1 d . . . C32 C -0.1986(4) 0.4374(9) 0.1861(4) 0.0447(14) Uani 1 1 d D . . H32 H -0.152(3) 0.543(5) 0.200(4) 0.062(17) Uiso 1 1 d D . . C33 C -0.2999(4) 0.4673(10) 0.1955(4) 0.0547(16) Uani 1 1 d D . . H33 H -0.326(3) 0.589(4) 0.217(3) 0.051(14) Uiso 1 1 d D . . C34 C -0.3691(4) 0.3100(11) 0.1743(4) 0.0617(18) Uani 1 1 d D . . H34 H -0.4387(14) 0.331(9) 0.178(4) 0.074 Uiso 1 1 d D . . C35 C -0.3375(4) 0.1231(11) 0.1453(5) 0.0549(17) Uani 1 1 d D . . H35 H -0.383(3) 0.015(5) 0.128(4) 0.062(17) Uiso 1 1 d D . . C36 C -0.2356(3) 0.0897(9) 0.1375(4) 0.0384(13) Uani 1 1 d . . . O5 O -0.2077(2) -0.0991(6) 0.1090(3) 0.0615(12) Uani 1 1 d . . . H5 H -0.1573 -0.0878 0.0816 0.074 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 N1 0.039(3) 0.029(3) 0.054(3) -0.003(2) 0.005(2) 0.000(2) N2 0.040(2) 0.029(3) 0.046(3) 0.004(2) 0.0048(17) 0.0076(19) C2 0.042(3) 0.041(4) 0.034(4) -0.005(3) 0.003(2) 0.001(3) O2 0.041(2) 0.035(2) 0.086(3) -0.010(2) 0.0057(16) -0.0070(17) C21 0.035(3) 0.037(4) 0.036(4) 0.005(3) 0.002(2) 0.001(2) C22 0.042(3) 0.037(3) 0.033(3) 0.003(3) 0.004(2) 0.000(2) N22 0.057(3) 0.035(3) 0.059(3) -0.006(2) 0.008(2) 0.003(2) C23 0.046(3) 0.048(4) 0.049(4) 0.002(3) 0.006(2) 0.009(3) C24 0.034(3) 0.066(5) 0.084(5) 0.000(4) 0.009(3) 0.008(3) C25 0.036(3) 0.062(5) 0.078(5) 0.001(4) 0.000(3) -0.012(3) C26 0.043(3) 0.041(4) 0.055(4) -0.004(3) 0.002(2) 0.001(3) C3 0.041(3) 0.029(4) 0.040(4) 0.001(3) 0.000(2) -0.002(2) C31 0.043(3) 0.030(4) 0.036(4) -0.004(3) -0.001(2) 0.004(2) C32 0.060(4) 0.032(4) 0.042(4) -0.009(3) 0.003(3) 0.002(3) C33 0.065(4) 0.045(5) 0.054(4) -0.004(3) 0.010(3) 0.025(3) C34 0.054(3) 0.071(5) 0.063(4) 0.012(4) 0.017(3) 0.016(4) C35 0.044(3) 0.049(5) 0.072(5) 0.004(4) 0.010(3) 0.004(3) C36 0.051(3) 0.031(3) 0.033(3) -0.002(3) 0.006(2) 0.005(2) O5 0.059(2) 0.035(2) 0.093(3) -0.016(2) 0.0205(19) -0.0045(17) _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 N1 N2 1.374(5) . ? N1 C2 1.385(7) . ? N1 H1 0.896(11) . ? N2 C3 1.276(7) . ? C2 O2 1.223(6) . ? C2 C21 1.476(6) . ? C21 C22 1.403(7) . ? C21 C26 1.416(8) . ? C22 N22 1.377(6) . ? C22 C23 1.391(6) . ? N22 H221 0.8600 . ? N22 H222 0.8600 . ? C23 C24 1.364(8) . ? C23 H23 0.934(11) . ? C24 C25 1.409(9) . ? C24 H24 0.934(11) . ? C25 C26 1.366(6) . ? C25 H25 0.934(11) . ? C26 H26 0.935(11) . ? C3 C31 1.449(6) . ? C3 H3 0.981(11) . ? C31 C32 1.400(7) . ? C31 C36 1.405(7) . ? C32 C33 1.374(7) . ? C32 H32 0.927(11) . ? C33 C34 1.377(8) . ? C33 H33 0.931(11) . ? C34 C35 1.368(9) . ? C34 H34 0.935(11) . ? C35 C36 1.381(6) . ? C35 H35 0.933(11) . ? C36 O5 1.360(6) . ? O5 H5 0.8200 . ? 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 N1 C2 116.1(4) . . ? N2 N1 H1 123(4) . . ? C2 N1 H1 120(4) . . ? C3 N2 N1 119.3(4) . . ? O2 C2 N1 119.3(4) . . ? O2 C2 C21 123.8(5) . . ? N1 C2 C21 116.9(4) . . ? C22 C21 C26 118.8(4) . . ? C22 C21 C2 120.8(4) . . ? C26 C21 C2 120.4(5) . . ? N22 C22 C23 118.4(5) . . ? N22 C22 C21 122.9(4) . . ? C23 C22 C21 118.7(5) . . ? C22 N22 H221 120.0 . . ? C22 N22 H222 120.0 . . ? H221 N22 H222 120.0 . . ? C24 C23 C22 122.4(5) . . ? C24 C23 H23 115(3) . . ? C22 C23 H23 122(3) . . ? C23 C24 C25 119.3(5) . . ? C23 C24 H24 119(4) . . ? C25 C24 H24 122(4) . . ? C26 C25 C24 119.6(5) . . ? C26 C25 H25 127(3) . . ? C24 C25 H25 113(3) . . ? C25 C26 C21 121.2(5) . . ? C25 C26 H26 123(3) . . ? C21 C26 H26 116(3) . . ? N2 C3 C31 118.2(4) . . ? N2 C3 H3 124(2) . . ? C31 C3 H3 118(2) . . ? C32 C31 C36 117.5(4) . . ? C32 C31 C3 120.7(4) . . ? C36 C31 C3 121.9(4) . . ? C33 C32 C31 121.3(5) . . ? C33 C32 H32 120(3) . . ? C31 C32 H32 119(3) . . ? C32 C33 C34 119.8(5) . . ? C32 C33 H33 124(3) . . ? C34 C33 H33 116(3) . . ? C35 C34 C33 120.5(5) . . ? C35 C34 H34 119(4) . . ? C33 C34 H34 120(4) . . ? C34 C35 C36 120.3(6) . . ? C34 C35 H35 123(3) . . ? C36 C35 H35 117(3) . . ? O5 C36 C35 118.2(5) . . ? O5 C36 C31 121.2(4) . . ? C35 C36 C31 120.6(5) . . ? C36 O5 H5 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 N1 N2 C3 179.0(6) . . . . ? N2 N1 C2 O2 4.7(7) . . . . ? N2 N1 C2 C21 -175.6(4) . . . . ? O2 C2 C21 C22 8.7(7) . . . . ? N1 C2 C21 C22 -171.0(5) . . . . ? O2 C2 C21 C26 -169.8(6) . . . . ? N1 C2 C21 C26 10.5(7) . . . . ? C26 C21 C22 N22 176.3(5) . . . . ? C2 C21 C22 N22 -2.2(7) . . . . ? C26 C21 C22 C23 -1.8(7) . . . . ? C2 C21 C22 C23 179.7(4) . . . . ? N22 C22 C23 C24 -177.9(6) . . . . ? C21 C22 C23 C24 0.3(7) . . . . ? C22 C23 C24 C25 1.1(9) . . . . ? C23 C24 C25 C26 -0.9(9) . . . . ? C24 C25 C26 C21 -0.6(8) . . . . ? C22 C21 C26 C25 2.0(8) . . . . ? C2 C21 C26 C25 -179.5(5) . . . . ? N1 N2 C3 C31 -178.0(4) . . . . ? N2 C3 C31 C32 173.1(6) . . . . ? N2 C3 C31 C36 -7.6(7) . . . . ? C36 C31 C32 C33 -0.8(7) . . . . ? C3 C31 C32 C33 178.6(5) . . . . ? C31 C32 C33 C34 -0.7(8) . . . . ? C32 C33 C34 C35 0.9(9) . . . . ? C33 C34 C35 C36 0.4(9) . . . . ? C34 C35 C36 O5 179.5(6) . . . . ? C34 C35 C36 C31 -1.9(8) . . . . ? C32 C31 C36 O5 -179.4(5) . . . . ? C3 C31 C36 O5 1.2(7) . . . . ? C32 C31 C36 C35 2.1(7) . . . . ? C3 C31 C36 C35 -177.3(4) . . . . ? _diffrn_measured_fraction_theta_max 0.833 _diffrn_reflns_theta_full 22.48 _diffrn_measured_fraction_theta_full 0.833 _refine_diff_density_max 0.160 _refine_diff_density_min -0.156 _refine_diff_density_rms 0.035 #===END data_rd1 _database_code_CSD 182102 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H16 N3 O5 Mo' _chemical_formula_weight 426.26 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' '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)/n 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 12.019(2) _cell_length_b 9.804(2) _cell_length_c 15.004(3) _cell_angle_alpha 90.00 _cell_angle_beta 109.60(3) _cell_angle_gamma 90.00 _cell_volume 1665.4(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 15 _cell_measurement_theta_min 7.5 _cell_measurement_theta_max 15.0 _exptl_crystal_description needle _exptl_crystal_colour 'pail yellow-orange' _exptl_crystal_size_max 0.64 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.700 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 860 _exptl_absorpt_coefficient_mu 0.820 _exptl_absorpt_correction_type Semi-empirical _exptl_absorpt_correction_T_min 0.46095 _exptl_absorpt_correction_T_max 0.50254 _exptl_absorpt_process_details ? _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 'Siemens P4 4-circle-diffractometer' _diffrn_measurement_method 'Profile fitted' _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 20 _diffrn_reflns_number 3072 _diffrn_reflns_av_R_equivalents 0.0323 _diffrn_reflns_av_sigmaI/netI 0.0378 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.53 _diffrn_reflns_theta_max 24.99 _reflns_number_total 2926 _reflns_number_gt 2312 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens P4' _computing_cell_refinement 'Siemens P4' _computing_data_reduction 'XDISK' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL-PLUS (VMS)' _computing_publication_material 'SHELXL-97' _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^)+(0.0320P)^2^+0.4940P] 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 SHELXL _refine_ls_extinction_coef ?0.0000(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2926 _refine_ls_number_parameters 267 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0505 _refine_ls_R_factor_gt 0.0324 _refine_ls_wR_factor_ref 0.0719 _refine_ls_wR_factor_gt 0.0662 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.074 _refine_ls_shift/su_max 0.021 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.10340(3) 0.28532(3) 0.19880(2) 0.02966(11) Uani 1 1 d . . . O1 O 0.0301(2) 0.4272(2) 0.21434(18) 0.0402(6) Uani 1 1 d . . . O2 O 0.1999(2) 0.2458(3) 0.30694(19) 0.0527(8) Uani 1 1 d . . . O3 O 0.2140(2) 0.3579(2) 0.14335(19) 0.0403(6) Uani 1 1 d . . . O4 O -0.0205(2) 0.1476(2) 0.19514(16) 0.0323(5) Uani 1 1 d . . . O5 O -0.0211(2) 0.3046(2) 0.04124(16) 0.0356(6) Uani 1 1 d . . . N1 N 0.1404(2) 0.0957(3) 0.1307(2) 0.0299(6) Uani 1 1 d . . . N2 N 0.0615(2) -0.0124(3) 0.1234(2) 0.0330(7) Uani 1 1 d . . . C2 C 0.2278(3) 0.0705(4) 0.1018(3) 0.0357(8) Uani 1 1 d D . . H2 H 0.238(3) -0.0168(17) 0.082(2) 0.043 Uiso 1 1 d D . . C3 C -0.0189(3) 0.0252(3) 0.1591(2) 0.0289(7) Uani 1 1 d . . . C11 C -0.1277(3) 0.3877(4) 0.0084(3) 0.0361(8) Uani 1 1 d D . . H111 H -0.103(3) 0.4782(19) 0.033(3) 0.054(5) Uiso 1 1 d D . . H112 H -0.153(3) 0.392(4) -0.0606(8) 0.054(5) Uiso 1 1 d D . . C12 C -0.2227(3) 0.3294(4) 0.0406(3) 0.0506(11) Uani 1 1 d . . . H121 H -0.1968 0.3289 0.1084 0.054(5) Uiso 1 1 calc R . . H122 H -0.2396 0.2377 0.0174 0.054(5) Uiso 1 1 calc R . . H123 H -0.2927 0.3840 0.0165 0.054(5) Uiso 1 1 calc R . . C21 C 0.3163(3) 0.1699(4) 0.1018(3) 0.0359(8) Uani 1 1 d . . . C22 C 0.4151(4) 0.1272(4) 0.0790(3) 0.0460(10) Uani 1 1 d D . . H22 H 0.416(3) 0.0352(15) 0.064(3) 0.046(11) Uiso 1 1 d D . . C23 C 0.5021(4) 0.2180(6) 0.0786(3) 0.0550(11) Uani 1 1 d . . . H23 H 0.567(4) 0.186(4) 0.066(3) 0.071(15) Uiso 1 1 d . . . C24 C 0.4920(4) 0.3529(5) 0.0996(3) 0.0505(10) Uani 1 1 d D . . H24 H 0.550(3) 0.415(3) 0.100(3) 0.055(12) Uiso 1 1 d D . . C25 C 0.3959(3) 0.3993(4) 0.1218(3) 0.0398(9) Uani 1 1 d D . . H25 H 0.380(3) 0.4887(17) 0.134(3) 0.045(11) Uiso 1 1 d D . . C26 C 0.3078(3) 0.3086(3) 0.1232(2) 0.0335(8) Uani 1 1 d . . . C31 C -0.1138(3) -0.0694(3) 0.1593(2) 0.0292(7) Uani 1 1 d . . . C32 C -0.2159(3) -0.0145(4) 0.1725(3) 0.0387(9) Uani 1 1 d D . . H32 H -0.217(3) 0.0786(13) 0.183(3) 0.046 Uiso 1 1 d D . . C33 C -0.3075(3) -0.0971(4) 0.1759(3) 0.0433(9) Uani 1 1 d D . . H33 H -0.377(2) -0.058(4) 0.176(3) 0.053(12) Uiso 1 1 d D . . C34 C -0.2993(4) -0.2360(4) 0.1662(3) 0.0471(10) Uani 1 1 d D . . H34 H -0.357(3) -0.297(3) 0.170(3) 0.057 Uiso 1 1 d D . . C35 C -0.1999(4) -0.2917(4) 0.1543(3) 0.0408(9) Uani 1 1 d D . . H35 H -0.191(3) -0.3860(13) 0.151(3) 0.049 Uiso 1 1 d D . . C36 C -0.1056(3) -0.2110(4) 0.1506(2) 0.0298(7) Uani 1 1 d . . . N5 N -0.0074(3) -0.2749(3) 0.1389(2) 0.0359(7) Uani 1 1 d . . . H51 H -0.0058 -0.3622 0.1341 0.043 Uiso 1 1 calc R . . H52 H 0.0514 -0.2268 0.1365 0.043 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 0.03421(17) 0.02191(16) 0.03223(17) -0.00080(15) 0.01031(12) 0.00069(15) O1 0.0504(16) 0.0275(13) 0.0464(15) -0.0035(12) 0.0213(13) 0.0015(12) O2 0.0602(18) 0.0443(17) 0.0408(15) 0.0029(12) -0.0002(13) 0.0017(13) O3 0.0346(14) 0.0278(13) 0.0627(17) 0.0036(13) 0.0219(13) 0.0013(11) O4 0.0407(14) 0.0230(12) 0.0399(14) -0.0026(11) 0.0222(11) 0.0000(11) O5 0.0310(12) 0.0427(16) 0.0328(13) 0.0050(11) 0.0102(10) 0.0095(11) N1 0.0309(16) 0.0228(14) 0.0372(16) 0.0017(12) 0.0130(13) 0.0023(12) N2 0.0360(17) 0.0232(14) 0.0439(17) -0.0019(13) 0.0189(14) -0.0017(13) C2 0.038(2) 0.0275(18) 0.042(2) 0.0029(17) 0.0152(17) 0.0046(16) C3 0.0341(19) 0.0250(17) 0.0273(18) 0.0042(14) 0.0097(15) 0.0028(15) C11 0.035(2) 0.033(2) 0.039(2) 0.0060(17) 0.0117(17) 0.0065(17) C12 0.042(2) 0.059(3) 0.056(3) 0.009(2) 0.023(2) 0.007(2) C21 0.0299(19) 0.039(2) 0.039(2) 0.0064(17) 0.0113(16) -0.0001(16) C22 0.041(2) 0.046(3) 0.056(3) 0.003(2) 0.022(2) 0.005(2) C23 0.036(2) 0.070(3) 0.067(3) 0.003(3) 0.028(2) 0.000(2) C24 0.039(2) 0.059(3) 0.054(3) -0.002(2) 0.016(2) -0.015(2) C25 0.039(2) 0.042(2) 0.037(2) 0.0019(18) 0.0107(17) -0.0081(19) C26 0.0297(18) 0.036(2) 0.0322(18) 0.0066(15) 0.0068(15) 0.0005(15) C31 0.0347(19) 0.0276(18) 0.0270(17) 0.0033(14) 0.0125(15) 0.0011(15) C32 0.045(2) 0.0318(19) 0.043(2) 0.0013(17) 0.0191(18) 0.0058(18) C33 0.042(2) 0.045(2) 0.048(2) 0.0033(19) 0.022(2) 0.0018(19) C34 0.048(2) 0.046(2) 0.051(2) 0.003(2) 0.022(2) -0.012(2) C35 0.053(2) 0.0278(19) 0.046(2) 0.0011(19) 0.0220(18) -0.005(2) C36 0.0404(19) 0.0260(17) 0.0241(16) 0.0013(15) 0.0122(14) -0.0009(17) N5 0.0439(17) 0.0211(14) 0.0475(17) -0.0029(14) 0.0215(14) -0.0001(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 Mo1 O2 1.693(3) . ? Mo1 O1 1.704(2) . ? Mo1 O3 1.925(2) . ? Mo1 O4 1.997(2) . ? Mo1 N1 2.237(3) . ? Mo1 O5 2.343(2) . ? O3 C26 1.350(4) . ? O4 C3 1.318(4) . ? O5 C11 1.457(4) . ? N1 C2 1.288(4) . ? N1 N2 1.401(4) . ? N2 C3 1.306(4) . ? C2 C21 1.443(5) . ? C2 H2 0.927(10) . ? C3 C31 1.471(5) . ? C11 C12 1.494(5) . ? C11 H111 0.971(10) . ? C11 H112 0.978(10) . ? C12 H121 0.9600 . ? C12 H122 0.9600 . ? C12 H123 0.9600 . ? C21 C22 1.404(5) . ? C21 C26 1.409(5) . ? C22 C23 1.375(6) . ? C22 H22 0.933(10) . ? C23 C24 1.375(6) . ? C23 H23 0.92(5) . ? C24 C25 1.382(6) . ? C24 H24 0.924(10) . ? C25 C26 1.389(5) . ? C25 H25 0.928(10) . ? C31 C36 1.401(5) . ? C31 C32 1.413(5) . ? C32 C33 1.381(5) . ? C32 H32 0.928(10) . ? C33 C34 1.377(6) . ? C33 H33 0.926(10) . ? C34 C35 1.379(5) . ? C34 H34 0.931(10) . ? C35 C36 1.398(5) . ? C35 H35 0.934(10) . ? C36 N5 1.398(4) . ? N5 H51 0.8600 . ? N5 H52 0.8600 . ? 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 O1 105.97(13) . . ? O2 Mo1 O3 98.52(13) . . ? O1 Mo1 O3 102.79(11) . . ? O2 Mo1 O4 97.85(12) . . ? O1 Mo1 O4 98.09(11) . . ? O3 Mo1 O4 148.68(10) . . ? O2 Mo1 N1 94.04(12) . . ? O1 Mo1 N1 158.78(11) . . ? O3 Mo1 N1 80.67(10) . . ? O4 Mo1 N1 71.69(9) . . ? O2 Mo1 O5 170.38(11) . . ? O1 Mo1 O5 83.54(10) . . ? O3 Mo1 O5 80.45(10) . . ? O4 Mo1 O5 78.98(9) . . ? N1 Mo1 O5 76.35(9) . . ? C26 O3 Mo1 135.5(2) . . ? C3 O4 Mo1 120.9(2) . . ? C11 O5 Mo1 125.3(2) . . ? C2 N1 N2 115.8(3) . . ? C2 N1 Mo1 128.5(2) . . ? N2 N1 Mo1 115.60(19) . . ? C3 N2 N1 109.1(3) . . ? N1 C2 C21 123.7(3) . . ? N1 C2 H2 120(2) . . ? C21 C2 H2 116(2) . . ? N2 C3 O4 122.7(3) . . ? N2 C3 C31 120.2(3) . . ? O4 C3 C31 117.1(3) . . ? O5 C11 C12 110.9(3) . . ? O5 C11 H111 105(2) . . ? C12 C11 H111 113(2) . . ? O5 C11 H112 108(2) . . ? C12 C11 H112 111(2) . . ? H111 C11 H112 108(3) . . ? C11 C12 H121 109.5 . . ? C11 C12 H122 109.5 . . ? H121 C12 H122 109.5 . . ? C11 C12 H123 109.5 . . ? H121 C12 H123 109.5 . . ? H122 C12 H123 109.5 . . ? C22 C21 C26 118.4(3) . . ? C22 C21 C2 118.8(3) . . ? C26 C21 C2 122.8(3) . . ? C23 C22 C21 121.0(4) . . ? C23 C22 H22 124(2) . . ? C21 C22 H22 115(2) . . ? C24 C23 C22 119.7(4) . . ? C24 C23 H23 121(3) . . ? C22 C23 H23 119(3) . . ? C23 C24 C25 121.2(4) . . ? C23 C24 H24 121(3) . . ? C25 C24 H24 118(3) . . ? C24 C25 C26 119.7(4) . . ? C24 C25 H25 127(2) . . ? C26 C25 H25 113(2) . . ? O3 C26 C25 118.2(3) . . ? O3 C26 C21 121.8(3) . . ? C25 C26 C21 120.0(3) . . ? C36 C31 C32 118.8(3) . . ? C36 C31 C3 123.1(3) . . ? C32 C31 C3 118.1(3) . . ? C33 C32 C31 121.5(4) . . ? C33 C32 H32 121(2) . . ? C31 C32 H32 118(2) . . ? C34 C33 C32 119.4(4) . . ? C34 C33 H33 121(3) . . ? C32 C33 H33 119(3) . . ? C33 C34 C35 120.0(4) . . ? C33 C34 H34 123(3) . . ? C35 C34 H34 117(3) . . ? C34 C35 C36 122.1(4) . . ? C34 C35 H35 121(2) . . ? C36 C35 H35 117(2) . . ? C35 C36 C31 118.3(3) . . ? C35 C36 N5 118.8(3) . . ? C31 C36 N5 123.0(3) . . ? C36 N5 H51 120.0 . . ? C36 N5 H52 120.0 . . ? H51 N5 H52 120.0 . . ? 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 O2 Mo1 O3 C26 61.7(3) . . . . ? O1 Mo1 O3 C26 170.3(3) . . . . ? O4 Mo1 O3 C26 -59.1(4) . . . . ? N1 Mo1 O3 C26 -31.0(3) . . . . ? O5 Mo1 O3 C26 -108.6(3) . . . . ? O2 Mo1 O4 C3 -91.0(2) . . . . ? O1 Mo1 O4 C3 161.5(2) . . . . ? O3 Mo1 O4 C3 29.9(3) . . . . ? N1 Mo1 O4 C3 0.7(2) . . . . ? O5 Mo1 O4 C3 79.8(2) . . . . ? O2 Mo1 O5 C11 155.6(7) . . . . ? O1 Mo1 O5 C11 -15.6(3) . . . . ? O3 Mo1 O5 C11 -119.7(3) . . . . ? O4 Mo1 O5 C11 84.0(3) . . . . ? N1 Mo1 O5 C11 157.6(3) . . . . ? O2 Mo1 N1 C2 -79.7(3) . . . . ? O1 Mo1 N1 C2 119.6(4) . . . . ? O3 Mo1 N1 C2 18.2(3) . . . . ? O4 Mo1 N1 C2 -176.7(3) . . . . ? O5 Mo1 N1 C2 100.6(3) . . . . ? O2 Mo1 N1 N2 96.4(2) . . . . ? O1 Mo1 N1 N2 -64.3(4) . . . . ? O3 Mo1 N1 N2 -165.6(2) . . . . ? O4 Mo1 N1 N2 -0.6(2) . . . . ? O5 Mo1 N1 N2 -83.3(2) . . . . ? C2 N1 N2 C3 177.0(3) . . . . ? Mo1 N1 N2 C3 0.4(3) . . . . ? N2 N1 C2 C21 178.5(3) . . . . ? Mo1 N1 C2 C21 -5.4(5) . . . . ? N1 N2 C3 O4 0.2(4) . . . . ? N1 N2 C3 C31 179.3(3) . . . . ? Mo1 O4 C3 N2 -0.7(4) . . . . ? Mo1 O4 C3 C31 -179.9(2) . . . . ? Mo1 O5 C11 C12 -69.7(4) . . . . ? N1 C2 C21 C22 172.7(4) . . . . ? N1 C2 C21 C26 -7.6(6) . . . . ? C26 C21 C22 C23 0.7(6) . . . . ? C2 C21 C22 C23 -179.6(4) . . . . ? C21 C22 C23 C24 -0.7(7) . . . . ? C22 C23 C24 C25 0.3(7) . . . . ? C23 C24 C25 C26 0.1(6) . . . . ? Mo1 O3 C26 C25 -152.3(3) . . . . ? Mo1 O3 C26 C21 29.2(5) . . . . ? C24 C25 C26 O3 -178.7(3) . . . . ? C24 C25 C26 C21 -0.2(5) . . . . ? C22 C21 C26 O3 178.2(3) . . . . ? C2 C21 C26 O3 -1.5(5) . . . . ? C22 C21 C26 C25 -0.2(5) . . . . ? C2 C21 C26 C25 -179.9(3) . . . . ? N2 C3 C31 C36 20.5(5) . . . . ? O4 C3 C31 C36 -160.3(3) . . . . ? N2 C3 C31 C32 -162.0(3) . . . . ? O4 C3 C31 C32 17.1(4) . . . . ? C36 C31 C32 C33 -0.8(5) . . . . ? C3 C31 C32 C33 -178.4(3) . . . . ? C31 C32 C33 C34 0.1(6) . . . . ? C32 C33 C34 C35 0.6(6) . . . . ? C33 C34 C35 C36 -0.6(6) . . . . ? C34 C35 C36 C31 -0.1(5) . . . . ? C34 C35 C36 N5 179.6(3) . . . . ? C32 C31 C36 C35 0.8(5) . . . . ? C3 C31 C36 C35 178.2(3) . . . . ? C32 C31 C36 N5 -178.9(3) . . . . ? C3 C31 C36 N5 -1.5(5) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.606 _refine_diff_density_min -0.583 _refine_diff_density_rms 0.070 #===END data_gosh _database_code_CSD 182103 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H15 N5 O4 Mo' _chemical_formula_weight 449.28 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 11.340(3) _cell_length_b 6.7416(11) _cell_length_c 22.902(4) _cell_angle_alpha 90.00 _cell_angle_beta 99.35(2) _cell_angle_gamma 90.00 _cell_volume 1727.7(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 15 _cell_measurement_theta_min 7.5 _cell_measurement_theta_max 15 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.727 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 904 _exptl_absorpt_coefficient_mu 0.795 _exptl_absorpt_correction_type Semi-empirical _exptl_absorpt_correction_T_min 0.59780 _exptl_absorpt_correction_T_max 0.68806 _exptl_absorpt_process_details ? _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 'Siemens P4 4-circle-diffractometer' _diffrn_measurement_method 'Profile fitted' _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 20 _diffrn_reflns_number 4118 _diffrn_reflns_av_R_equivalents 0.0271 _diffrn_reflns_av_sigmaI/netI 0.0398 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 27.50 _reflns_number_total 3938 _reflns_number_gt 2961 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens P4' _computing_cell_refinement 'Siemens P4' _computing_data_reduction 'XDISK' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL-PLUS (VMS)' _computing_publication_material 'SHELXL-97' _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^)+(0.0348P)^2^+0.3372P] 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 SHELXL _refine_ls_extinction_coef 0.0008(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3938 _refine_ls_number_parameters 256 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0564 _refine_ls_R_factor_gt 0.0332 _refine_ls_wR_factor_ref 0.0747 _refine_ls_wR_factor_gt 0.0676 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.23410(2) 0.07663(3) 0.414599(11) 0.03017(8) Uani 1 1 d . . . O1 O 0.15394(19) -0.1282(3) 0.42789(10) 0.0419(5) Uani 1 1 d . . . O2 O 0.37161(19) -0.0106(3) 0.40692(12) 0.0522(6) Uani 1 1 d . . . O3 O 0.1753(2) 0.1347(3) 0.33296(9) 0.0427(5) Uani 1 1 d . . . O4 O 0.28257(18) 0.1640(3) 0.49900(9) 0.0371(5) Uani 1 1 d . . . N1 N 0.29168(19) 0.3937(3) 0.41402(10) 0.0299(5) Uani 1 1 d . . . N2 N 0.3409(2) 0.4700(3) 0.46960(11) 0.0316(5) Uani 1 1 d . . . N3 N 0.0560(2) 0.2461(4) 0.42696(10) 0.0333(5) Uani 1 1 d . . . C11 C 0.0243(3) 0.4407(5) 0.41797(17) 0.0486(8) Uani 1 1 d . . . H11 H 0.0737 0.5404 0.4076 0.059(11) Uiso 1 1 calc R . . C12 C -0.0902(3) 0.4657(6) 0.4265(2) 0.0610(11) Uani 1 1 d . . . H12 H -0.1335 0.5834 0.4229 0.092(15) Uiso 1 1 calc R . . N4 N -0.1290(2) 0.2858(4) 0.44114(12) 0.0468(7) Uani 1 1 d . . . H4 H -0.1988 0.2587 0.4490 0.056 Uiso 1 1 calc R . . C13 C -0.0398(3) 0.1584(5) 0.44113(13) 0.0378(7) Uani 1 1 d . . . H13 H -0.0441 0.0242 0.4500 0.044(9) Uiso 1 1 calc R . . C2 C 0.2913(2) 0.5112(4) 0.36983(13) 0.0321(6) Uani 1 1 d . . . H21 H 0.3316 0.6313 0.3764 0.039 Uiso 1 1 calc R . . C21 C 0.2321(3) 0.4680(4) 0.31071(13) 0.0354(7) Uani 1 1 d . . . C22 C 0.2253(3) 0.6176(5) 0.26782(15) 0.0480(8) Uani 1 1 d . . . H22 H 0.2639 0.7378 0.2774 0.059(11) Uiso 1 1 calc R . . C23 C 0.1622(4) 0.5893(6) 0.21154(16) 0.0593(10) Uani 1 1 d . . . H23 H 0.1583 0.6898 0.1835 0.062(11) Uiso 1 1 calc R . . C24 C 0.1048(3) 0.4111(6) 0.19716(16) 0.0568(9) Uani 1 1 d . . . H24 H 0.0612 0.3925 0.1595 0.063(11) Uiso 1 1 calc R . . C25 C 0.1118(3) 0.2615(6) 0.23804(14) 0.0470(8) Uani 1 1 d . . . H25 H 0.0738 0.1415 0.2275 0.056(11) Uiso 1 1 calc R . . C26 C 0.1742(3) 0.2858(5) 0.29465(13) 0.0351(7) Uani 1 1 d . . . C3 C 0.3316(2) 0.3408(4) 0.51066(13) 0.0316(6) Uani 1 1 d . . . C31 C 0.3713(2) 0.3881(4) 0.57364(13) 0.0330(6) Uani 1 1 d . . . C32 C 0.3650(3) 0.2412(5) 0.61585(14) 0.0409(7) Uani 1 1 d . . . H32 H 0.3412 0.1144 0.6030 0.054(11) Uiso 1 1 calc R . . C33 C 0.3924(3) 0.2758(6) 0.67558(16) 0.0524(9) Uani 1 1 d . . . H33 H 0.3870 0.1751 0.7028 0.069(13) Uiso 1 1 calc R . . C34 C 0.4285(3) 0.4658(6) 0.69426(16) 0.0575(10) Uani 1 1 d . . . H34 H 0.4474 0.4922 0.7346 0.049(10) Uiso 1 1 calc R . . C35 C 0.4367(3) 0.6142(6) 0.65458(15) 0.0489(9) Uani 1 1 d . . . H35 H 0.4619 0.7393 0.6684 0.049(10) Uiso 1 1 calc R . . C36 C 0.4078(2) 0.5822(5) 0.59333(14) 0.0365(6) Uani 1 1 d . . . N5 N 0.4062(2) 0.7405(4) 0.55559(12) 0.0428(6) Uani 1 1 d . . . H51 H 0.4227 0.8575 0.5695 0.051 Uiso 1 1 calc R . . H52 H 0.3886 0.7228 0.5180 0.051 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 0.03065(12) 0.02125(12) 0.03796(14) -0.00271(12) 0.00361(9) -0.00052(12) O1 0.0433(12) 0.0280(11) 0.0534(14) 0.0020(10) 0.0047(10) -0.0053(9) O2 0.0369(12) 0.0378(12) 0.0827(18) -0.0158(13) 0.0121(12) 0.0012(10) O3 0.0568(14) 0.0358(12) 0.0348(12) -0.0028(9) 0.0053(10) -0.0085(10) O4 0.0445(12) 0.0252(10) 0.0387(12) 0.0019(9) -0.0020(9) -0.0030(9) N1 0.0256(11) 0.0268(12) 0.0372(13) -0.0013(10) 0.0048(9) -0.0001(9) N2 0.0299(11) 0.0283(13) 0.0356(13) -0.0057(10) 0.0027(10) -0.0020(10) N3 0.0307(12) 0.0324(13) 0.0365(13) -0.0021(11) 0.0046(10) -0.0007(11) C11 0.0382(16) 0.0316(16) 0.079(3) 0.0035(17) 0.0175(16) 0.0036(15) C12 0.0412(19) 0.048(2) 0.100(3) 0.007(2) 0.027(2) 0.0128(17) N4 0.0296(13) 0.0573(18) 0.0557(17) 0.0037(15) 0.0139(12) 0.0013(13) C13 0.0359(16) 0.0405(17) 0.0369(16) 0.0023(14) 0.0054(13) -0.0012(14) C2 0.0311(14) 0.0277(13) 0.0380(16) -0.0002(12) 0.0068(12) 0.0004(12) C21 0.0330(14) 0.0356(18) 0.0393(16) 0.0018(13) 0.0111(12) 0.0029(12) C22 0.056(2) 0.042(2) 0.0465(19) 0.0057(15) 0.0112(16) 0.0022(16) C23 0.073(2) 0.060(2) 0.0439(19) 0.018(2) 0.0058(18) 0.013(2) C24 0.055(2) 0.074(3) 0.0380(18) 0.004(2) -0.0001(15) 0.003(2) C25 0.0436(18) 0.058(2) 0.0392(18) -0.0052(17) 0.0063(14) -0.0037(17) C26 0.0331(15) 0.0395(16) 0.0346(16) -0.0037(14) 0.0110(12) 0.0025(13) C3 0.0253(13) 0.0265(13) 0.0416(17) -0.0026(13) 0.0012(12) 0.0047(11) C31 0.0249(13) 0.0351(17) 0.0380(16) -0.0033(13) 0.0019(11) 0.0055(12) C32 0.0348(16) 0.0391(18) 0.0467(18) -0.0010(15) 0.0008(14) 0.0035(14) C33 0.049(2) 0.065(2) 0.0396(18) 0.0021(19) -0.0004(15) 0.0062(18) C34 0.050(2) 0.081(3) 0.0374(19) -0.0109(19) -0.0028(15) 0.002(2) C35 0.0394(17) 0.054(2) 0.051(2) -0.0200(17) -0.0016(15) -0.0046(16) C36 0.0220(12) 0.0390(16) 0.0469(17) -0.0111(16) 0.0010(11) 0.0022(14) N5 0.0452(15) 0.0316(14) 0.0509(16) -0.0114(13) 0.0056(13) -0.0036(12) _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 1.702(2) . ? Mo1 O1 1.707(2) . ? Mo1 O3 1.920(2) . ? Mo1 O4 2.010(2) . ? Mo1 N1 2.235(2) . ? Mo1 N3 2.377(2) . ? O3 C26 1.343(4) . ? O4 C3 1.324(3) . ? N1 C2 1.285(4) . ? N1 N2 1.402(3) . ? N2 C3 1.299(4) . ? N3 C13 1.323(4) . ? N3 C11 1.367(4) . ? C11 C12 1.355(4) . ? C11 H11 0.9300 . ? C12 N4 1.351(4) . ? C12 H12 0.9300 . ? N4 C13 1.327(4) . ? N4 H4 0.8600 . ? C13 H13 0.9300 . ? C2 C21 1.440(4) . ? C2 H21 0.9300 . ? C21 C22 1.401(4) . ? C21 C26 1.413(4) . ? C22 C23 1.382(5) . ? C22 H22 0.9300 . ? C23 C24 1.380(5) . ? C23 H23 0.9300 . ? C24 C25 1.370(5) . ? C24 H24 0.9300 . ? C25 C26 1.382(4) . ? C25 H25 0.9300 . ? C3 C31 1.474(4) . ? C31 C32 1.394(4) . ? C31 C36 1.423(4) . ? C32 C33 1.373(5) . ? C32 H32 0.9300 . ? C33 C34 1.391(5) . ? C33 H33 0.9300 . ? C34 C35 1.365(5) . ? C34 H34 0.9300 . ? C35 C36 1.404(4) . ? C35 H35 0.9300 . ? C36 N5 1.372(4) . ? N5 H51 0.8600 . ? N5 H52 0.8600 . ? 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 O1 105.21(11) . . ? O2 Mo1 O3 98.55(12) . . ? O1 Mo1 O3 103.16(10) . . ? O2 Mo1 O4 95.07(11) . . ? O1 Mo1 O4 97.80(10) . . ? O3 Mo1 O4 150.94(9) . . ? O2 Mo1 N1 93.23(10) . . ? O1 Mo1 N1 159.83(9) . . ? O3 Mo1 N1 81.66(9) . . ? O4 Mo1 N1 72.01(8) . . ? O2 Mo1 N3 171.38(10) . . ? O1 Mo1 N3 83.11(9) . . ? O3 Mo1 N3 81.42(9) . . ? O4 Mo1 N3 81.35(8) . . ? N1 Mo1 N3 78.22(8) . . ? C26 O3 Mo1 139.1(2) . . ? C3 O4 Mo1 119.86(19) . . ? C2 N1 N2 116.0(2) . . ? C2 N1 Mo1 129.1(2) . . ? N2 N1 Mo1 114.79(16) . . ? C3 N2 N1 110.1(2) . . ? C13 N3 C11 105.1(3) . . ? C13 N3 Mo1 124.2(2) . . ? C11 N3 Mo1 130.6(2) . . ? C12 C11 N3 109.4(3) . . ? C12 C11 H11 125.3 . . ? N3 C11 H11 125.3 . . ? N4 C12 C11 106.4(3) . . ? N4 C12 H12 126.8 . . ? C11 C12 H12 126.8 . . ? C13 N4 C12 107.6(3) . . ? C13 N4 H4 126.2 . . ? C12 N4 H4 126.2 . . ? N3 C13 N4 111.6(3) . . ? N3 C13 H13 124.2 . . ? N4 C13 H13 124.2 . . ? N1 C2 C21 123.9(3) . . ? N1 C2 H21 118.1 . . ? C21 C2 H21 118.1 . . ? C22 C21 C26 118.2(3) . . ? C22 C21 C2 118.5(3) . . ? C26 C21 C2 123.1(3) . . ? C23 C22 C21 121.0(4) . . ? C23 C22 H22 119.5 . . ? C21 C22 H22 119.5 . . ? C24 C23 C22 119.7(3) . . ? C24 C23 H23 120.2 . . ? C22 C23 H23 120.2 . . ? C25 C24 C23 120.3(3) . . ? C25 C24 H24 119.8 . . ? C23 C24 H24 119.8 . . ? C24 C25 C26 121.2(4) . . ? C24 C25 H25 119.4 . . ? C26 C25 H25 119.4 . . ? O3 C26 C25 118.2(3) . . ? O3 C26 C21 122.3(3) . . ? C25 C26 C21 119.5(3) . . ? N2 C3 O4 122.6(3) . . ? N2 C3 C31 121.0(3) . . ? O4 C3 C31 116.3(3) . . ? C32 C31 C36 118.6(3) . . ? C32 C31 C3 118.9(3) . . ? C36 C31 C3 122.4(3) . . ? C33 C32 C31 122.8(3) . . ? C33 C32 H32 118.6 . . ? C31 C32 H32 118.6 . . ? C32 C33 C34 118.1(4) . . ? C32 C33 H33 121.0 . . ? C34 C33 H33 121.0 . . ? C35 C34 C33 121.2(3) . . ? C35 C34 H34 119.4 . . ? C33 C34 H34 119.4 . . ? C34 C35 C36 121.5(3) . . ? C34 C35 H35 119.3 . . ? C36 C35 H35 119.3 . . ? N5 C36 C35 119.1(3) . . ? N5 C36 C31 122.8(3) . . ? C35 C36 C31 117.8(3) . . ? C36 N5 H51 120.0 . . ? C36 N5 H52 120.0 . . ? H51 N5 H52 120.0 . . ? 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 O2 Mo1 O3 C26 -89.5(3) . . . . ? O1 Mo1 O3 C26 162.6(3) . . . . ? O4 Mo1 O3 C26 27.5(4) . . . . ? N1 Mo1 O3 C26 2.5(3) . . . . ? N3 Mo1 O3 C26 81.8(3) . . . . ? O2 Mo1 O4 C3 85.1(2) . . . . ? O1 Mo1 O4 C3 -168.8(2) . . . . ? O3 Mo1 O4 C3 -32.7(3) . . . . ? N1 Mo1 O4 C3 -6.65(18) . . . . ? N3 Mo1 O4 C3 -87.0(2) . . . . ? O2 Mo1 N1 C2 88.7(2) . . . . ? O1 Mo1 N1 C2 -115.1(3) . . . . ? O3 Mo1 N1 C2 -9.5(2) . . . . ? O4 Mo1 N1 C2 -177.0(3) . . . . ? N3 Mo1 N1 C2 -92.4(2) . . . . ? O2 Mo1 N1 N2 -87.50(18) . . . . ? O1 Mo1 N1 N2 68.8(3) . . . . ? O3 Mo1 N1 N2 174.33(18) . . . . ? O4 Mo1 N1 N2 6.80(16) . . . . ? N3 Mo1 N1 N2 91.41(17) . . . . ? C2 N1 N2 C3 177.3(2) . . . . ? Mo1 N1 N2 C3 -6.0(3) . . . . ? O2 Mo1 N3 C13 -162.1(7) . . . . ? O1 Mo1 N3 C13 2.9(2) . . . . ? O3 Mo1 N3 C13 107.4(2) . . . . ? O4 Mo1 N3 C13 -96.1(2) . . . . ? N1 Mo1 N3 C13 -169.4(2) . . . . ? O2 Mo1 N3 C11 22.9(8) . . . . ? O1 Mo1 N3 C11 -172.1(3) . . . . ? O3 Mo1 N3 C11 -67.6(3) . . . . ? O4 Mo1 N3 C11 88.9(3) . . . . ? N1 Mo1 N3 C11 15.6(3) . . . . ? C13 N3 C11 C12 -0.5(4) . . . . ? Mo1 N3 C11 C12 175.3(3) . . . . ? N3 C11 C12 N4 0.4(5) . . . . ? C11 C12 N4 C13 -0.1(4) . . . . ? C11 N3 C13 N4 0.4(4) . . . . ? Mo1 N3 C13 N4 -175.7(2) . . . . ? C12 N4 C13 N3 -0.2(4) . . . . ? N2 N1 C2 C21 -172.4(2) . . . . ? Mo1 N1 C2 C21 11.5(4) . . . . ? N1 C2 C21 C22 172.2(3) . . . . ? N1 C2 C21 C26 -3.9(4) . . . . ? C26 C21 C22 C23 1.0(5) . . . . ? C2 C21 C22 C23 -175.3(3) . . . . ? C21 C22 C23 C24 0.0(5) . . . . ? C22 C23 C24 C25 -1.0(6) . . . . ? C23 C24 C25 C26 1.1(5) . . . . ? Mo1 O3 C26 C25 -176.1(2) . . . . ? Mo1 O3 C26 C21 2.5(5) . . . . ? C24 C25 C26 O3 178.6(3) . . . . ? C24 C25 C26 C21 -0.1(5) . . . . ? C22 C21 C26 O3 -179.6(3) . . . . ? C2 C21 C26 O3 -3.5(4) . . . . ? C22 C21 C26 C25 -0.9(4) . . . . ? C2 C21 C26 C25 175.2(3) . . . . ? N1 N2 C3 O4 0.5(4) . . . . ? N1 N2 C3 C31 -177.0(2) . . . . ? Mo1 O4 C3 N2 6.1(4) . . . . ? Mo1 O4 C3 C31 -176.33(17) . . . . ? N2 C3 C31 C32 -176.8(3) . . . . ? O4 C3 C31 C32 5.6(4) . . . . ? N2 C3 C31 C36 7.8(4) . . . . ? O4 C3 C31 C36 -169.8(2) . . . . ? C36 C31 C32 C33 0.1(4) . . . . ? C3 C31 C32 C33 -175.5(3) . . . . ? C31 C32 C33 C34 -0.3(5) . . . . ? C32 C33 C34 C35 0.0(5) . . . . ? C33 C34 C35 C36 0.7(5) . . . . ? C34 C35 C36 N5 173.6(3) . . . . ? C34 C35 C36 C31 -1.0(5) . . . . ? C32 C31 C36 N5 -173.8(3) . . . . ? C3 C31 C36 N5 1.6(4) . . . . ? C32 C31 C36 C35 0.6(4) . . . . ? C3 C31 C36 C35 176.0(3) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.309 _refine_diff_density_min -0.507 _refine_diff_density_rms 0.071 #===END