# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2011 data_publication_text _journal_name_full CrystEngComm #TrackingRef 'Uzarevic_et_al_cif.cif' _journal_coden_Cambridge 1350 _publ_section_title ; Mechanosensitive metal-ligand bonds in the design of new coordination compounds ; loop_ _publ_contact_author_name _publ_contact_author_email 'Uzarevic, Krunoslav' kruno@chem.pmf.hr _publ_contact_author_address ; Department of Chemistry, Faculty of Science, University of Zagreb Horvatovac 102a HR-10000 Zagreb Croatia ; loop_ _publ_author_name _publ_author_address K.Uzarevic ;Laboratory of General and Inorganic Chemistry Chemistry Department Faculty of Science, University of Zagreb Horvatovac 102a HR-10000 Zagreb Croatia ; M.Rubcic ;Laboratory of General and Inorganic Chemistry Chemistry Department Faculty of Science, University of Zagreb Horvatovac 102a HR-10000 Zagreb Croatia ; M.Radic ;Undergraduate student, Chemistry Department Faculty of Science, University of Zagreb Horvatovac 102a HR-10000 Zagreb Croatia ; A.Puskaric ;Undergraduate student, Chemistry Department Faculty of Science, University of Zagreb Horvatovac 102a HR-10000 Zagreb Croatia ; M.Cindric ;Laboratory of General and Inorganic Chemistry Chemistry Department Faculty of Science, University of Zagreb Horvatovac 102a HR-10000 Zagreb Croatia ; data_I(Me) _database_code_depnum_ccdc_archive 'CCDC 799774' #TrackingRef 'Uzarevic_et_al_cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; (Methanol)cis-dioxo(N-3-methoxysalicylidene-2-amino-3 -hydroxypyridine)molybdenum(VI) ; _chemical_name_common ; (Methanol)cis-dioxo(N-3-methoxysalicylidene-2-amino-3 - hydroxypyridine)molybdenum(VI) ; _chemical_melting_point ? _chemical_formula_moiety 'C14 H14 Mo N2 O6' _chemical_formula_sum 'C14 H14 Mo N2 O6' _chemical_formula_weight 402.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.1890(7) _cell_length_b 10.9898(9) _cell_length_c 17.930(2) _cell_angle_alpha 90.00 _cell_angle_beta 105.346(9) _cell_angle_gamma 90.00 _cell_volume 1556.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 2805 _cell_measurement_theta_min 4.2190 _cell_measurement_theta_max 29.0616 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.717 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 808 _exptl_absorpt_coefficient_mu 0.875 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.85389 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.3426 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6270 _diffrn_reflns_av_R_equivalents 0.0149 _diffrn_reflns_av_sigmaI/netI 0.0256 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 4.22 _diffrn_reflns_theta_max 26.50 _reflns_number_total 3210 _reflns_number_gt 2381 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) ; _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is 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^)+(0.0378P)^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 3210 _refine_ls_number_parameters 212 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0357 _refine_ls_R_factor_gt 0.0240 _refine_ls_wR_factor_ref 0.0616 _refine_ls_wR_factor_gt 0.0593 _refine_ls_goodness_of_fit_ref 0.923 _refine_ls_restrained_S_all 0.923 _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 0.26466(2) 0.253623(17) 0.386254(10) 0.03967(8) Uani 1 1 d . . . O1 O 0.0592(2) 0.28076(16) 0.34283(10) 0.0596(5) Uani 1 1 d . . . O2 O 0.3065(2) 0.11427(15) 0.35468(9) 0.0545(4) Uani 1 1 d . . . O3 O 0.36645(19) 0.34894(14) 0.31558(8) 0.0480(4) Uani 1 1 d . . . O4 O 0.2410(2) 0.21969(14) 0.48934(9) 0.0487(4) Uani 1 1 d . . . O5 O 0.1191(2) 0.09108(16) 0.58427(10) 0.0650(5) Uani 1 1 d . . . O6 O 0.5481(2) 0.24660(15) 0.45629(10) 0.0501(4) Uani 1 1 d D . . H6O H 0.572(3) 0.277(3) 0.4987(12) 0.075 Uiso 1 1 d D . . N1 N 0.3768(2) 0.64452(16) 0.40273(9) 0.0409(4) Uani 1 1 d . . . N2 N 0.3021(2) 0.44516(15) 0.43782(8) 0.0341(4) Uani 1 1 d . . . C1 C 0.3570(2) 0.52593(19) 0.38837(10) 0.0347(5) Uani 1 1 d . . . C2 C 0.3865(3) 0.4694(2) 0.32298(11) 0.0397(5) Uani 1 1 d . . . C3 C 0.4384(3) 0.5420(2) 0.27022(12) 0.0527(6) Uani 1 1 d . . . H3 H 0.4601 0.5080 0.2263 0.063 Uiso 1 1 calc R . . C4 C 0.4570(3) 0.6637(2) 0.28382(13) 0.0570(6) Uani 1 1 d . . . H4 H 0.4906 0.7141 0.2489 0.068 Uiso 1 1 calc R . . C5 C 0.4254(3) 0.7119(2) 0.34998(14) 0.0513(6) Uani 1 1 d . . . H5 H 0.4386 0.7953 0.3583 0.062 Uiso 1 1 calc R . . C6 C 0.2498(2) 0.4838(2) 0.49578(11) 0.0369(5) Uani 1 1 d . . . H6 H 0.2514 0.5673 0.5041 0.044 Uiso 1 1 calc R . . C7 C 0.1901(2) 0.4087(2) 0.54795(11) 0.0373(5) Uani 1 1 d . . . C8 C 0.1831(3) 0.2814(2) 0.54150(12) 0.0387(5) Uani 1 1 d . . . C9 C 0.1197(3) 0.2130(2) 0.59500(13) 0.0450(5) Uani 1 1 d . . . C10 C 0.0679(3) 0.2724(2) 0.65264(13) 0.0511(6) Uani 1 1 d . . . H10 H 0.0264 0.2274 0.6876 0.061 Uiso 1 1 calc R . . C11 C 0.0769(3) 0.3983(3) 0.65928(12) 0.0531(6) Uani 1 1 d . . . H11 H 0.0424 0.4367 0.6988 0.064 Uiso 1 1 calc R . . C12 C 0.1364(3) 0.4665(2) 0.60796(11) 0.0451(5) Uani 1 1 d . . . H12 H 0.1415 0.5508 0.6126 0.054 Uiso 1 1 calc R . . C13 C 0.0325(4) 0.0187(3) 0.62730(17) 0.0782(9) Uani 1 1 d . . . H13A H 0.0286 -0.0641 0.6099 0.117 Uiso 1 1 calc R . . H13B H -0.0807 0.0488 0.6198 0.117 Uiso 1 1 calc R . . H13C H 0.0912 0.0226 0.6812 0.117 Uiso 1 1 calc R . . C14 C 0.6690(4) 0.1607(4) 0.45043(19) 0.1192(15) Uani 1 1 d . . . H14A H 0.7751 0.1801 0.4865 0.179 Uiso 1 1 calc R . . H14B H 0.6824 0.1613 0.3988 0.179 Uiso 1 1 calc R . . H14C H 0.6327 0.0814 0.4619 0.179 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 0.04896(12) 0.03889(12) 0.03528(11) -0.00962(9) 0.01839(8) -0.00953(9) O1 0.0560(10) 0.0645(12) 0.0578(11) -0.0133(8) 0.0139(8) -0.0075(9) O2 0.0721(11) 0.0457(10) 0.0511(10) -0.0193(8) 0.0258(8) -0.0123(9) O3 0.0698(10) 0.0441(9) 0.0375(8) -0.0072(7) 0.0273(7) -0.0054(8) O4 0.0694(10) 0.0403(9) 0.0455(9) -0.0033(7) 0.0310(8) -0.0080(8) O5 0.0824(13) 0.0533(11) 0.0708(12) 0.0076(9) 0.0407(10) -0.0161(10) O6 0.0505(9) 0.0559(10) 0.0440(9) -0.0138(8) 0.0125(7) 0.0019(9) N1 0.0464(10) 0.0397(11) 0.0359(9) 0.0010(8) 0.0098(8) -0.0063(9) N2 0.0387(9) 0.0380(10) 0.0278(8) -0.0017(7) 0.0127(7) -0.0046(8) C1 0.0359(11) 0.0395(12) 0.0284(10) 0.0011(9) 0.0083(8) -0.0037(9) C2 0.0432(12) 0.0474(13) 0.0299(10) -0.0003(9) 0.0120(9) -0.0040(10) C3 0.0632(15) 0.0648(17) 0.0349(12) 0.0016(11) 0.0216(11) -0.0075(14) C4 0.0679(16) 0.0598(17) 0.0464(14) 0.0151(12) 0.0206(12) -0.0135(14) C5 0.0614(15) 0.0453(13) 0.0472(14) 0.0077(11) 0.0144(12) -0.0124(12) C6 0.0416(11) 0.0359(11) 0.0345(11) -0.0040(9) 0.0122(9) -0.0020(10) C7 0.0370(11) 0.0454(13) 0.0313(10) -0.0014(9) 0.0120(9) -0.0014(10) C8 0.0390(11) 0.0496(14) 0.0290(11) 0.0000(9) 0.0116(9) -0.0060(10) C9 0.0426(12) 0.0535(14) 0.0407(12) 0.0066(10) 0.0145(10) -0.0061(11) C10 0.0460(12) 0.0760(19) 0.0353(12) 0.0075(11) 0.0174(10) -0.0046(13) C11 0.0503(14) 0.0795(19) 0.0347(12) -0.0018(12) 0.0202(10) 0.0068(14) C12 0.0480(13) 0.0551(15) 0.0349(11) -0.0034(10) 0.0157(10) 0.0039(11) C13 0.079(2) 0.073(2) 0.091(2) 0.0318(17) 0.0366(17) -0.0164(17) C14 0.088(2) 0.136(4) 0.111(3) -0.068(3) -0.0150(19) 0.054(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 O1 1.6828(18) . ? Mo1 O2 1.6988(15) . ? Mo1 O4 1.9450(14) . ? Mo1 O3 1.9892(14) . ? Mo1 N2 2.2868(16) . ? Mo1 O6 2.3297(17) . ? O3 C2 1.336(3) . ? O4 C8 1.339(2) . ? O5 C9 1.353(3) . ? O5 C13 1.421(3) . ? O6 C14 1.392(3) . ? O6 H6O 0.808(17) . ? N1 C1 1.330(3) . ? N1 C5 1.342(3) . ? N2 C6 1.296(2) . ? N2 C1 1.410(2) . ? C1 C2 1.403(3) . ? C2 C3 1.387(3) . ? C3 C4 1.361(3) . ? C3 H3 0.9300 . ? C4 C5 1.384(3) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C7 1.427(3) . ? C6 H6 0.9300 . ? C7 C8 1.403(3) . ? C7 C12 1.416(3) . ? C8 C9 1.421(3) . ? C9 C10 1.381(3) . ? C10 C11 1.390(3) . ? C10 H10 0.9300 . ? C11 C12 1.372(3) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mo1 O2 105.71(8) . . ? O1 Mo1 O4 97.74(8) . . ? O2 Mo1 O4 102.92(7) . . ? O1 Mo1 O3 98.51(8) . . ? O2 Mo1 O3 96.14(6) . . ? O4 Mo1 O3 150.50(7) . . ? O1 Mo1 N2 91.98(7) . . ? O2 Mo1 N2 161.30(7) . . ? O4 Mo1 N2 80.14(6) . . ? O3 Mo1 N2 74.86(5) . . ? O1 Mo1 O6 170.62(7) . . ? O2 Mo1 O6 83.66(7) . . ? O4 Mo1 O6 79.46(7) . . ? O3 Mo1 O6 80.51(6) . . ? N2 Mo1 O6 78.74(6) . . ? C2 O3 Mo1 121.31(12) . . ? C8 O4 Mo1 135.16(14) . . ? C9 O5 C13 117.4(2) . . ? C14 O6 Mo1 127.50(17) . . ? C14 O6 H6O 111(2) . . ? Mo1 O6 H6O 117(2) . . ? C1 N1 C5 116.63(18) . . ? C6 N2 C1 121.76(18) . . ? C6 N2 Mo1 126.03(13) . . ? C1 N2 Mo1 110.87(11) . . ? N1 C1 C2 123.82(18) . . ? N1 C1 N2 122.56(17) . . ? C2 C1 N2 113.62(18) . . ? O3 C2 C3 123.63(19) . . ? O3 C2 C1 118.56(17) . . ? C3 C2 C1 117.8(2) . . ? C4 C3 C2 118.9(2) . . ? C4 C3 H3 120.6 . . ? C2 C3 H3 120.6 . . ? C3 C4 C5 119.5(2) . . ? C3 C4 H4 120.3 . . ? C5 C4 H4 120.3 . . ? N1 C5 C4 123.4(2) . . ? N1 C5 H5 118.3 . . ? C4 C5 H5 118.3 . . ? N2 C6 C7 125.4(2) . . ? N2 C6 H6 117.3 . . ? C7 C6 H6 117.3 . . ? C8 C7 C12 119.73(19) . . ? C8 C7 C6 122.40(18) . . ? C12 C7 C6 117.9(2) . . ? O4 C8 C7 123.25(18) . . ? O4 C8 C9 117.6(2) . . ? C7 C8 C9 119.1(2) . . ? O5 C9 C10 125.7(2) . . ? O5 C9 C8 114.6(2) . . ? C10 C9 C8 119.6(2) . . ? C9 C10 C11 121.0(2) . . ? C9 C10 H10 119.5 . . ? C11 C10 H10 119.5 . . ? C12 C11 C10 120.4(2) . . ? C12 C11 H11 119.8 . . ? C10 C11 H11 119.8 . . ? C11 C12 C7 120.1(2) . . ? C11 C12 H12 120.0 . . ? C7 C12 H12 120.0 . . ? O5 C13 H13A 109.5 . . ? O5 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? O5 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O6 C14 H14A 109.5 . . ? O6 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? O6 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.282 _refine_diff_density_min -0.562 _refine_diff_density_rms 0.061 #===END data_I(Et) _database_code_depnum_ccdc_archive 'CCDC 799775' #TrackingRef 'Uzarevic_et_al_cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; (Ethanol)cis-dioxo(N-3-methoxysalicylidene-2-amino -3-hydroxypyridine)molybdenum(VI) ; _chemical_name_common ; (Ethanol)cis-dioxo(N-3-methoxysalicylidene-2-amino -3- hydroxypyridine)molybdenum(VI) ; _chemical_melting_point ? _chemical_formula_moiety 'C15 H16 Mo N2 O6' _chemical_formula_sum 'C15 H16 Mo N2 O6' _chemical_formula_weight 416.24 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-p 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.0992(16) _cell_length_b 11.4036(11) _cell_length_c 17.993(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.474(16) _cell_angle_gamma 90.00 _cell_volume 1639.2(4) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 1963 _cell_measurement_theta_min 4.2279 _cell_measurement_theta_max 29.0190 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.687 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 840 _exptl_absorpt_coefficient_mu 0.834 _exptl_absorpt_correction_T_min 0.71440 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.3426 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11592 _diffrn_reflns_av_R_equivalents 0.0528 _diffrn_reflns_av_sigmaI/netI 0.0641 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 4.25 _diffrn_reflns_theta_max 27.00 _reflns_number_total 3549 _reflns_number_gt 2062 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) ; _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is 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 [0.00000+1.00000exp(2.00(sin\q/\l)^2^)]/ [\s^2^(Fo^2^)+0.0000+0.0000*P+(0.0368P)^2^+0.0000sin\q/\l] where P = 0.33333Fo^2^ + 0.66667Fc^2^ ; _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 3549 _refine_ls_number_parameters 218 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0730 _refine_ls_R_factor_gt 0.0331 _refine_ls_wR_factor_ref 0.0777 _refine_ls_wR_factor_gt 0.0702 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C13 C 0.4411(6) 0.5363(4) -0.1582(2) 0.0737(13) Uani 1 1 d . . . H13A H 0.4274 0.4544 -0.1486 0.111 Uiso 1 1 calc R . . H13B H 0.5581 0.5540 -0.1542 0.111 Uiso 1 1 calc R . . H13C H 0.3849 0.5551 -0.2080 0.111 Uiso 1 1 calc R . . C14 C -0.1769(6) 0.6854(4) 0.0590(3) 0.0857(13) Uani 1 1 d DU . . H14A H -0.2811 0.7289 0.0538 0.103 Uiso 1 1 calc R A 1 H14B H -0.1530 0.6530 0.1094 0.103 Uiso 1 1 calc R A 1 C15A C -0.1886(16) 0.5896(7) 0.0013(5) 0.0857(13) Uani 0.600(12) 1 d PDU B 1 H15A H -0.2758 0.5359 0.0086 0.129 Uiso 0.600(12) 1 calc PR B 1 H15B H -0.0839 0.5485 0.0065 0.129 Uiso 0.600(12) 1 calc PR B 1 H15C H -0.2137 0.6230 -0.0483 0.129 Uiso 0.600(12) 1 calc PR B 1 C15B C -0.283(2) 0.6218(13) -0.0047(5) 0.0857(13) Uani 0.400(12) 1 d PDU B 2 H15D H -0.3664 0.5767 0.0145 0.129 Uiso 0.400(12) 1 calc PR B 2 H15E H -0.2131 0.5703 -0.0284 0.129 Uiso 0.400(12) 1 calc PR B 2 H15F H -0.3357 0.6775 -0.0409 0.129 Uiso 0.400(12) 1 calc PR B 2 O6 O -0.0442(3) 0.7594(2) 0.04506(13) 0.0499(6) Uani 1 1 d D B . H6O H -0.067(5) 0.794(3) 0.0054(15) 0.075 Uiso 1 1 d D . . Mo1 Mo 0.23301(4) 0.75270(3) 0.103354(15) 0.03795(10) Uani 1 1 d . . . O4 O 0.2604(3) 0.72393(18) 0.00009(14) 0.0482(6) Uani 1 1 d . B . O3 O 0.1328(3) 0.84264(19) 0.17951(12) 0.0446(6) Uani 1 1 d . B . N2 N 0.2010(3) 0.9389(2) 0.05737(14) 0.0337(6) Uani 1 1 d . B . C9 C 0.3810(5) 0.7221(3) -0.1104(2) 0.0477(9) Uani 1 1 d . B . C1 C 0.1370(4) 1.0142(3) 0.10796(18) 0.0347(7) Uani 1 1 d . . . C7 C 0.3225(4) 0.9080(3) -0.05462(18) 0.0379(8) Uani 1 1 d . B . C6 C 0.2572(4) 0.9787(3) -0.00008(18) 0.0379(8) Uani 1 1 d . . . H6 H 0.2558 1.0595 -0.0071 0.045 Uiso 1 1 calc R B . O5 O 0.3711(4) 0.6040(2) -0.10427(15) 0.0641(8) Uani 1 1 d . . . O2 O 0.1845(3) 0.61873(19) 0.13345(14) 0.0515(7) Uani 1 1 d . B . N1 N 0.1108(4) 1.1279(2) 0.09356(16) 0.0416(7) Uani 1 1 d . B . C8 C 0.3216(4) 0.7858(3) -0.05244(19) 0.0389(8) Uani 1 1 d . . . C10 C 0.4398(5) 0.7823(3) -0.1665(2) 0.0538(10) Uani 1 1 d . . . H10 H 0.4808 0.7410 -0.2041 0.065 Uiso 1 1 calc R B . C3 C 0.0444(5) 1.0243(3) 0.2262(2) 0.0505(9) Uani 1 1 d . . . H3 H 0.0198 0.9901 0.2700 0.061 Uiso 1 1 calc R B . C2 C 0.1049(4) 0.9582(3) 0.17262(18) 0.0384(8) Uani 1 1 d . B . O1 O 0.4357(3) 0.7739(2) 0.13966(15) 0.0562(7) Uani 1 1 d . B . C12 C 0.3820(5) 0.9652(3) -0.1131(2) 0.0507(9) Uani 1 1 d . . . H12 H 0.3826 1.0467 -0.1146 0.061 Uiso 1 1 calc R B . C11 C 0.4394(5) 0.9029(4) -0.1681(2) 0.0608(11) Uani 1 1 d . B . H11 H 0.4785 0.9422 -0.2071 0.073 Uiso 1 1 calc R . . C5 C 0.0540(5) 1.1908(3) 0.1472(2) 0.0516(9) Uani 1 1 d . . . H5 H 0.0359 1.2707 0.1393 0.062 Uiso 1 1 calc R B . C4 C 0.0214(5) 1.1426(3) 0.2132(2) 0.0549(10) Uani 1 1 d . B . H4 H -0.0162 1.1899 0.2491 0.066 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 C13 0.084(3) 0.077(3) 0.064(3) -0.030(2) 0.023(2) 0.014(3) C14 0.073(3) 0.089(3) 0.093(3) 0.018(2) 0.007(3) -0.031(2) C15A 0.073(3) 0.089(3) 0.093(3) 0.018(2) 0.007(3) -0.031(2) C15B 0.073(3) 0.089(3) 0.093(3) 0.018(2) 0.007(3) -0.031(2) O6 0.0541(14) 0.0545(15) 0.0415(13) 0.0098(13) 0.0089(11) -0.0115(14) Mo1 0.05223(17) 0.03205(14) 0.03294(14) 0.00558(16) 0.01695(11) 0.00308(17) O4 0.0717(17) 0.0349(15) 0.0446(14) -0.0016(9) 0.0295(12) 0.0012(11) O3 0.0663(16) 0.0395(13) 0.0331(13) 0.0046(10) 0.0228(11) 0.0022(12) N2 0.0447(15) 0.0305(13) 0.0279(14) -0.0007(11) 0.0117(12) -0.0021(12) C9 0.056(2) 0.051(3) 0.0386(19) -0.0031(15) 0.0155(16) 0.0058(17) C1 0.0405(19) 0.0312(16) 0.0337(18) -0.0019(13) 0.0098(14) -0.0031(14) C7 0.0423(19) 0.0424(19) 0.0312(18) 0.0023(14) 0.0130(15) -0.0023(16) C6 0.048(2) 0.0317(17) 0.0347(18) 0.0050(13) 0.0107(15) -0.0015(15) O5 0.093(2) 0.0511(16) 0.0563(18) -0.0153(13) 0.0356(16) 0.0100(15) O2 0.0782(18) 0.0335(13) 0.0467(15) 0.0102(11) 0.0220(13) 0.0008(12) N1 0.0524(18) 0.0340(15) 0.0390(16) -0.0049(12) 0.0098(14) 0.0029(13) C8 0.046(2) 0.0456(19) 0.0296(17) -0.0008(13) 0.0188(14) 0.0002(15) C10 0.064(3) 0.067(3) 0.036(2) -0.0064(16) 0.0237(18) 0.0034(19) C3 0.066(2) 0.058(2) 0.0314(19) -0.0021(16) 0.0194(17) 0.006(2) C2 0.046(2) 0.0401(18) 0.0309(18) -0.0033(14) 0.0110(15) 0.0012(16) O1 0.0586(16) 0.0534(18) 0.0568(16) 0.0110(12) 0.0099(12) 0.0025(12) C12 0.063(2) 0.053(2) 0.040(2) 0.0096(17) 0.0210(18) -0.0058(19) C11 0.067(3) 0.085(3) 0.037(2) 0.009(2) 0.0265(19) -0.008(2) C5 0.065(3) 0.041(2) 0.050(2) -0.0092(17) 0.0122(19) 0.0061(19) C4 0.072(3) 0.052(2) 0.045(2) -0.0161(17) 0.020(2) 0.010(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C13 O5 1.428(4) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 O6 1.421(5) . ? C14 C15B 1.4991(10) . ? C14 C15A 1.4995(10) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15A H15A 0.9600 . ? C15A H15B 0.9600 . ? C15A H15C 0.9600 . ? C15B H15D 0.9600 . ? C15B H15E 0.9600 . ? C15B H15F 0.9600 . ? O6 Mo1 2.318(3) . ? O6 H6O 0.810(18) . ? Mo1 O1 1.681(3) . ? Mo1 O2 1.689(2) . ? Mo1 O4 1.935(2) . ? Mo1 O3 1.989(2) . ? Mo1 N2 2.278(2) . ? O4 C8 1.338(4) . ? O3 C2 1.339(4) . ? N2 C6 1.279(4) . ? N2 C1 1.411(4) . ? C9 O5 1.354(4) . ? C9 C10 1.370(5) . ? C9 C8 1.418(5) . ? C1 N1 1.332(4) . ? C1 C2 1.389(4) . ? C7 C12 1.390(4) . ? C7 C8 1.394(4) . ? C7 C6 1.437(4) . ? C6 H6 0.9300 . ? N1 C5 1.343(4) . ? C10 C11 1.375(5) . ? C10 H10 0.9300 . ? C3 C2 1.376(4) . ? C3 C4 1.377(5) . ? C3 H3 0.9300 . ? C12 C11 1.361(5) . ? C12 H12 0.9300 . ? C11 H11 0.9300 . ? C5 C4 1.372(5) . ? C5 H5 0.9300 . ? C4 H4 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 C13 H13A 109.5 . . ? O5 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? O5 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O6 C14 C15B 120.4(6) . . ? O6 C14 C15A 105.9(5) . . ? C15B C14 C15A 32.4(6) . . ? O6 C14 H14A 110.5 . . ? C15B C14 H14A 78.2 . . ? C15A C14 H14A 110.5 . . ? O6 C14 H14B 110.5 . . ? C15B C14 H14B 122.1 . . ? C15A C14 H14B 110.5 . . ? H14A C14 H14B 108.7 . . ? C14 C15A H15A 109.5 . . ? C14 C15A H15B 109.5 . . ? H15A C15A H15B 109.5 . . ? C14 C15A H15C 109.5 . . ? H15A C15A H15C 109.5 . . ? H15B C15A H15C 109.5 . . ? C14 C15B H15D 109.5 . . ? C14 C15B H15E 109.5 . . ? H15D C15B H15E 109.5 . . ? C14 C15B H15F 109.5 . . ? H15D C15B H15F 109.5 . . ? H15E C15B H15F 109.5 . . ? C14 O6 Mo1 127.2(3) . . ? C14 O6 H6O 112(3) . . ? Mo1 O6 H6O 118(3) . . ? O1 Mo1 O2 105.63(12) . . ? O1 Mo1 O4 97.96(12) . . ? O2 Mo1 O4 102.95(10) . . ? O1 Mo1 O3 98.12(12) . . ? O2 Mo1 O3 95.89(10) . . ? O4 Mo1 O3 150.85(10) . . ? O1 Mo1 N2 93.01(10) . . ? O2 Mo1 N2 160.24(11) . . ? O4 Mo1 N2 80.41(9) . . ? O3 Mo1 N2 74.61(9) . . ? O1 Mo1 O6 169.17(10) . . ? O2 Mo1 O6 85.17(11) . . ? O4 Mo1 O6 80.03(10) . . ? O3 Mo1 O6 79.62(10) . . ? N2 Mo1 O6 76.17(9) . . ? C8 O4 Mo1 134.7(2) . . ? C2 O3 Mo1 121.70(19) . . ? C6 N2 C1 121.5(3) . . ? C6 N2 Mo1 126.1(2) . . ? C1 N2 Mo1 111.41(19) . . ? O5 C9 C10 126.2(3) . . ? O5 C9 C8 114.7(3) . . ? C10 C9 C8 119.1(3) . . ? N1 C1 C2 124.4(3) . . ? N1 C1 N2 122.0(3) . . ? C2 C1 N2 113.5(3) . . ? C12 C7 C8 119.6(3) . . ? C12 C7 C6 117.8(3) . . ? C8 C7 C6 122.5(3) . . ? N2 C6 C7 124.9(3) . . ? N2 C6 H6 117.5 . . ? C7 C6 H6 117.5 . . ? C9 O5 C13 116.5(3) . . ? C1 N1 C5 116.2(3) . . ? O4 C8 C7 123.4(3) . . ? O4 C8 C9 117.4(3) . . ? C7 C8 C9 119.1(3) . . ? C9 C10 C11 121.1(4) . . ? C9 C10 H10 119.4 . . ? C11 C10 H10 119.4 . . ? C2 C3 C4 118.1(3) . . ? C2 C3 H3 120.9 . . ? C4 C3 H3 120.9 . . ? O3 C2 C3 123.3(3) . . ? O3 C2 C1 118.6(3) . . ? C3 C2 C1 118.1(3) . . ? C11 C12 C7 120.5(4) . . ? C11 C12 H12 119.7 . . ? C7 C12 H12 119.7 . . ? C12 C11 C10 120.4(4) . . ? C12 C11 H11 119.8 . . ? C10 C11 H11 119.8 . . ? N1 C5 C4 123.1(4) . . ? N1 C5 H5 118.5 . . ? C4 C5 H5 118.5 . . ? C5 C4 C3 120.0(3) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.388 _refine_diff_density_min -0.423 _refine_diff_density_rms 0.067 #===END data_I(Pr) _database_code_depnum_ccdc_archive 'CCDC 799776' #TrackingRef 'Uzarevic_et_al_cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; cis-dioxo(N-3-methoxysalicylidene-2-amino -3-hydroxypyridine)(propanol)molybdenum(VI) ; _chemical_name_common ; cis-dioxo(N-3-methoxysalicylidene-2-amino -3- hydroxypyridine)(propanol)molybdenum(VI) ; _chemical_melting_point ? _chemical_formula_moiety 'C16 H18 Mo N2 O6' _chemical_formula_sum 'C16 H18 Mo N2 O6' _chemical_formula_weight 430.26 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.7894(4) _cell_length_b 10.0907(7) _cell_length_c 12.5937(5) _cell_angle_alpha 86.293(4) _cell_angle_beta 81.553(4) _cell_angle_gamma 69.096(5) _cell_volume 914.61(9) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 3593 _cell_measurement_theta_min 4.2437 _cell_measurement_theta_max 28.8922 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.562 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 436 _exptl_absorpt_coefficient_mu 0.750 _exptl_absorpt_correction_T_min 0.91404 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.3426 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6752 _diffrn_reflns_av_R_equivalents 0.0224 _diffrn_reflns_av_sigmaI/netI 0.0468 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 4.25 _diffrn_reflns_theta_max 26.50 _reflns_number_total 3761 _reflns_number_gt 2947 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) ; _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is 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^)+(0.0826P)^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 3761 _refine_ls_number_parameters 218 _refine_ls_number_restraints 60 _refine_ls_R_factor_all 0.0596 _refine_ls_R_factor_gt 0.0461 _refine_ls_wR_factor_ref 0.1259 _refine_ls_wR_factor_gt 0.1207 _refine_ls_goodness_of_fit_ref 0.982 _refine_ls_restrained_S_all 0.975 _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 0.59530(5) 0.22711(3) 0.18144(3) 0.04289(15) Uani 1 1 d . . . O1 O 0.3861(4) 0.2431(4) 0.1491(2) 0.0635(9) Uani 1 1 d . . . O2 O 0.5498(4) 0.3407(3) 0.2836(2) 0.0563(8) Uani 1 1 d . . . O3 O 0.6648(4) 0.3510(3) 0.0683(2) 0.0540(8) Uani 1 1 d . . . O4 O 0.6463(4) 0.0444(3) 0.2522(2) 0.0477(7) Uani 1 1 d . . . O5 O 0.5399(6) -0.1097(4) 0.4030(2) 0.0716(10) Uani 1 1 d . . . O6 O 0.9026(5) 0.1704(4) 0.2032(3) 0.0776(8) Uani 1 1 d DU B . N1 N 0.8667(5) 0.1016(4) -0.1473(3) 0.0473(8) Uani 1 1 d . . . N2 N 0.7385(4) 0.0832(3) 0.0368(2) 0.0381(7) Uani 1 1 d . . . C1 C 0.7858(5) 0.1600(4) -0.0523(3) 0.0404(9) Uani 1 1 d . . . C2 C 0.7418(6) 0.3041(4) -0.0307(3) 0.0457(9) Uani 1 1 d . . . C3 C 0.7802(6) 0.3904(5) -0.1142(4) 0.0561(11) Uani 1 1 d . . . H3 H 0.7521 0.4866 -0.1036 0.067 Uiso 1 1 calc R . . C4 C 0.8600(7) 0.3316(5) -0.2123(4) 0.0616(13) Uani 1 1 d . . . H4 H 0.8876 0.3872 -0.2693 0.074 Uiso 1 1 calc R . . C5 C 0.8993(7) 0.1876(5) -0.2257(3) 0.0574(12) Uani 1 1 d . . . H5 H 0.9514 0.1494 -0.2932 0.069 Uiso 1 1 calc R . . C6 C 0.7462(6) -0.0469(4) 0.0290(3) 0.0441(9) Uani 1 1 d . . . H6 H 0.7875 -0.0892 -0.0379 0.053 Uiso 1 1 calc R . . C7 C 0.6950(6) -0.1291(4) 0.1168(3) 0.0422(9) Uani 1 1 d . . . C8 C 0.6435(6) -0.0804(4) 0.2232(3) 0.0420(9) Uani 1 1 d . . . C9 C 0.5908(6) -0.1668(5) 0.3025(3) 0.0511(10) Uani 1 1 d . . . C10 C 0.5941(7) -0.2998(5) 0.2786(4) 0.0594(12) Uani 1 1 d . . . H10 H 0.5592 -0.3564 0.3323 0.071 Uiso 1 1 calc R . . C11 C 0.6501(8) -0.3482(5) 0.1733(4) 0.0639(13) Uani 1 1 d . . . H11 H 0.6526 -0.4376 0.1571 0.077 Uiso 1 1 calc R . . C12 C 0.7006(7) -0.2662(5) 0.0949(4) 0.0565(12) Uani 1 1 d . . . H12 H 0.7397 -0.3006 0.0254 0.068 Uiso 1 1 calc R . . C13 C 0.4685(12) -0.1849(8) 0.4855(4) 0.107(2) Uani 1 1 d . . . H13A H 0.4393 -0.1342 0.5515 0.160 Uiso 1 1 calc R . . H13B H 0.5594 -0.2774 0.4941 0.160 Uiso 1 1 calc R . . H13C H 0.3583 -0.1944 0.4669 0.160 Uiso 1 1 calc R . . C14 C 0.9736(6) 0.2573(5) 0.2516(4) 0.0776(8) Uani 1 1 d DU . . H14A H 0.9237 0.3497 0.2177 0.093 Uiso 1 1 calc R A 1 H14B H 1.1054 0.2223 0.2261 0.093 Uiso 1 1 calc R A 1 C15B C 0.961(2) 0.2878(8) 0.3680(4) 0.0776(8) Uani 0.402(6) 1 d PDU B 1 H15C H 0.8338 0.3454 0.3942 0.093 Uiso 0.402(6) 1 calc PR B 1 H15D H 1.0390 0.3418 0.3757 0.093 Uiso 0.402(6) 1 calc PR B 1 C16B C 1.0189(19) 0.1533(12) 0.4355(6) 0.0776(8) Uani 0.402(6) 1 d PDU B 1 H16D H 1.0053 0.1774 0.5095 0.116 Uiso 0.402(6) 1 calc PR B 1 H16E H 1.1461 0.0980 0.4120 0.116 Uiso 0.402(6) 1 calc PR B 1 H16F H 0.9422 0.0992 0.4277 0.116 Uiso 0.402(6) 1 calc PR B 1 C15A C 1.0552(8) 0.1773(5) 0.3476(5) 0.0776(8) Uani 0.598(6) 1 d PDU B 2 H15A H 1.1741 0.1053 0.3239 0.093 Uiso 0.598(6) 1 calc PR B 2 H15B H 0.9742 0.1297 0.3837 0.093 Uiso 0.598(6) 1 calc PR B 2 C16A C 1.0816(13) 0.2739(9) 0.4260(5) 0.0776(8) Uani 0.598(6) 1 d PDU B 2 H16A H 1.1290 0.2196 0.4875 0.116 Uiso 0.598(6) 1 calc PR B 2 H16B H 0.9647 0.3466 0.4484 0.116 Uiso 0.598(6) 1 calc PR B 2 H16C H 1.1678 0.3168 0.3918 0.116 Uiso 0.598(6) 1 calc PR B 2 H6O H 0.968(8) 0.100(4) 0.178(5) 0.116 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0529(2) 0.0292(2) 0.0437(2) -0.00264(13) -0.00133(14) -0.01251(15) O1 0.0528(18) 0.067(2) 0.0637(19) 0.0018(17) -0.0076(15) -0.0134(16) O2 0.073(2) 0.0405(16) 0.0521(17) -0.0102(13) 0.0060(14) -0.0202(15) O3 0.076(2) 0.0282(14) 0.0518(16) -0.0035(12) 0.0037(14) -0.0151(14) O4 0.0719(19) 0.0378(15) 0.0398(14) -0.0005(12) -0.0090(13) -0.0263(14) O5 0.122(3) 0.061(2) 0.0422(16) 0.0012(15) 0.0025(17) -0.051(2) O6 0.0713(18) 0.0715(19) 0.095(2) -0.0149(15) -0.0157(14) -0.0267(15) N1 0.056(2) 0.0416(19) 0.0387(17) 0.0008(15) -0.0057(14) -0.0105(16) N2 0.0478(18) 0.0270(15) 0.0385(16) -0.0001(13) -0.0083(13) -0.0110(14) C1 0.040(2) 0.033(2) 0.042(2) 0.0038(16) -0.0082(16) -0.0062(16) C2 0.047(2) 0.032(2) 0.052(2) 0.0040(17) -0.0035(18) -0.0091(18) C3 0.063(3) 0.037(2) 0.062(3) 0.008(2) -0.003(2) -0.013(2) C4 0.066(3) 0.053(3) 0.057(3) 0.016(2) -0.003(2) -0.015(2) C5 0.066(3) 0.055(3) 0.043(2) 0.003(2) -0.004(2) -0.013(2) C6 0.057(2) 0.041(2) 0.0346(19) -0.0030(16) -0.0067(16) -0.0176(19) C7 0.057(2) 0.0300(19) 0.044(2) 0.0021(16) -0.0130(17) -0.0185(18) C8 0.050(2) 0.033(2) 0.045(2) -0.0009(16) -0.0119(17) -0.0146(17) C9 0.069(3) 0.043(2) 0.048(2) 0.0055(19) -0.012(2) -0.027(2) C10 0.087(3) 0.048(3) 0.057(3) 0.011(2) -0.014(2) -0.040(3) C11 0.100(4) 0.039(2) 0.067(3) 0.003(2) -0.023(3) -0.037(3) C12 0.089(3) 0.042(2) 0.048(2) -0.0029(19) -0.016(2) -0.030(2) C13 0.189(7) 0.098(5) 0.053(3) 0.005(3) 0.017(4) -0.088(5) C14 0.0713(18) 0.0715(19) 0.095(2) -0.0149(15) -0.0157(14) -0.0267(15) C15B 0.0713(18) 0.0715(19) 0.095(2) -0.0149(15) -0.0157(14) -0.0267(15) C16B 0.0713(18) 0.0715(19) 0.095(2) -0.0149(15) -0.0157(14) -0.0267(15) C15A 0.0713(18) 0.0715(19) 0.095(2) -0.0149(15) -0.0157(14) -0.0267(15) C16A 0.0713(18) 0.0715(19) 0.095(2) -0.0149(15) -0.0157(14) -0.0267(15) _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 1.687(3) . ? Mo1 O2 1.691(3) . ? Mo1 O4 1.929(3) . ? Mo1 O3 1.978(3) . ? Mo1 N2 2.293(3) . ? Mo1 O6 2.308(4) . ? O3 C2 1.338(5) . ? O4 C8 1.342(5) . ? O5 C9 1.370(5) . ? O5 C13 1.412(6) . ? O6 C14 1.400(6) . ? O6 H6O 0.77(2) . ? N1 C5 1.328(5) . ? N1 C1 1.334(5) . ? N2 C6 1.302(5) . ? N2 C1 1.402(5) . ? C1 C2 1.406(6) . ? C2 C3 1.388(6) . ? C3 C4 1.368(6) . ? C3 H3 0.9300 . ? C4 C5 1.390(7) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C7 1.435(5) . ? C6 H6 0.9300 . ? C7 C8 1.408(5) . ? C7 C12 1.412(6) . ? C8 C9 1.396(6) . ? C9 C10 1.385(6) . ? C10 C11 1.395(7) . ? C10 H10 0.9300 . ? C11 C12 1.352(6) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 C15B 1.4992(10) . ? C14 C15A 1.4999(10) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15B C16B 1.5150(10) . ? C15B H15C 0.9700 . ? C15B H15D 0.9700 . ? C16B H16D 0.9600 . ? C16B H16E 0.9600 . ? C16B H16F 0.9600 . ? C15A C16A 1.51500(13) . ? C15A H15A 0.9700 . ? C15A H15B 0.9700 . ? C16A H16A 0.9600 . ? C16A H16B 0.9600 . ? C16A H16C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mo1 O2 105.27(16) . . ? O1 Mo1 O4 96.92(15) . . ? O2 Mo1 O4 103.68(13) . . ? O1 Mo1 O3 99.23(15) . . ? O2 Mo1 O3 96.06(13) . . ? O4 Mo1 O3 150.15(13) . . ? O1 Mo1 N2 90.21(14) . . ? O2 Mo1 N2 163.17(14) . . ? O4 Mo1 N2 80.49(11) . . ? O3 Mo1 N2 74.53(11) . . ? O1 Mo1 O6 169.22(15) . . ? O2 Mo1 O6 85.43(15) . . ? O4 Mo1 O6 78.89(14) . . ? O3 Mo1 O6 80.63(15) . . ? N2 Mo1 O6 79.33(13) . . ? C2 O3 Mo1 122.1(3) . . ? C8 O4 Mo1 133.1(2) . . ? C9 O5 C13 117.9(4) . . ? C14 O6 Mo1 125.0(3) . . ? C14 O6 H6O 120(6) . . ? Mo1 O6 H6O 115(6) . . ? C5 N1 C1 117.0(4) . . ? C6 N2 C1 121.9(3) . . ? C6 N2 Mo1 125.4(3) . . ? C1 N2 Mo1 111.5(2) . . ? N1 C1 N2 123.4(4) . . ? N1 C1 C2 123.6(4) . . ? N2 C1 C2 113.0(3) . . ? O3 C2 C3 123.6(4) . . ? O3 C2 C1 118.7(3) . . ? C3 C2 C1 117.7(4) . . ? C4 C3 C2 118.9(4) . . ? C4 C3 H3 120.5 . . ? C2 C3 H3 120.5 . . ? C3 C4 C5 119.1(4) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? N1 C5 C4 123.6(4) . . ? N1 C5 H5 118.2 . . ? C4 C5 H5 118.2 . . ? N2 C6 C7 124.3(3) . . ? N2 C6 H6 117.9 . . ? C7 C6 H6 117.9 . . ? C8 C7 C12 119.1(4) . . ? C8 C7 C6 123.0(4) . . ? C12 C7 C6 117.9(4) . . ? O4 C8 C9 118.4(3) . . ? O4 C8 C7 123.0(4) . . ? C9 C8 C7 118.7(4) . . ? O5 C9 C10 124.3(4) . . ? O5 C9 C8 114.6(4) . . ? C10 C9 C8 121.1(4) . . ? C9 C10 C11 119.6(4) . . ? C9 C10 H10 120.2 . . ? C11 C10 H10 120.2 . . ? C12 C11 C10 120.5(4) . . ? C12 C11 H11 119.8 . . ? C10 C11 H11 119.8 . . ? C11 C12 C7 121.0(4) . . ? C11 C12 H12 119.5 . . ? C7 C12 H12 119.5 . . ? O5 C13 H13A 109.5 . . ? O5 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? O5 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O6 C14 C15B 129.7(6) . . ? O6 C14 C15A 107.0(4) . . ? C15B C14 C15A 43.8(4) . . ? O6 C14 H14A 104.8 . . ? C15B C14 H14A 104.8 . . ? C15A C14 H14A 145.9 . . ? O6 C14 H14B 104.8 . . ? C15B C14 H14B 104.8 . . ? C15A C14 H14B 77.5 . . ? H14A C14 H14B 105.8 . . ? C14 C15B C16B 112.08(8) . . ? C14 C15B H15C 109.2 . . ? C16B C15B H15C 109.2 . . ? C14 C15B H15D 109.2 . . ? C16B C15B H15D 109.2 . . ? H15C C15B H15D 107.9 . . ? C15B C16B H16D 109.5 . . ? C15B C16B H16E 109.5 . . ? H16D C16B H16E 109.5 . . ? C15B C16B H16F 109.5 . . ? H16D C16B H16F 109.5 . . ? H16E C16B H16F 109.5 . . ? C14 C15A C16A 112.04(6) . . ? C14 C15A H15A 109.2 . . ? C16A C15A H15A 109.2 . . ? C14 C15A H15B 109.2 . . ? C16A C15A H15B 109.2 . . ? H15A C15A H15B 107.9 . . ? C15A C16A H16A 109.5 . . ? C15A C16A H16B 109.5 . . ? H16A C16A H16B 109.5 . . ? C15A C16A H16C 109.5 . . ? H16A C16A H16C 109.5 . . ? H16B C16A H16C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.602 _refine_diff_density_min -1.391 _refine_diff_density_rms 0.090 #===END data_I(Gp)_x_CH3CN _database_code_depnum_ccdc_archive 'CCDC 799777' #TrackingRef 'Uzarevic_et_al_cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; cis-dioxo(N-3-methoxysalicylidene-2-amino-3-hydroxypyridine) (4-methylpyridine)molybdenum(VI) acetonitrile solvate ; _chemical_name_common ; cis-dioxo(N-3-methoxysalicylidene-2-amino-3-hydroxypyridine) (4-methylpyridine)molybdenum(VI) acetonitrile solvate ; _chemical_melting_point ? _chemical_formula_moiety 'C19 H17 Mo N3 O5, C2 H3 N' _chemical_formula_sum 'C21 H20 Mo N4 O5' _chemical_formula_weight 504.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.8879(3) _cell_length_b 14.5134(5) _cell_length_c 16.4716(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.433(3) _cell_angle_gamma 90.00 _cell_volume 2124.69(13) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 3307 _cell_measurement_theta_min 4.2032 _cell_measurement_theta_max 29.7352 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.577 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1024 _exptl_absorpt_coefficient_mu 0.658 _exptl_absorpt_correction_T_min 0.90298 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET) (compiled Sep 15 2009,11:49:04) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.3426 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9891 _diffrn_reflns_av_R_equivalents 0.0390 _diffrn_reflns_av_sigmaI/netI 0.1102 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 4.38 _diffrn_reflns_theta_max 26.50 _reflns_number_total 4400 _reflns_number_gt 2552 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) ; _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is 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 [0.00000+1.00000exp(3.00(sin\q/\l)^2^)]/ [\s^2^(Fo^2^)+0.0000+0.0000*P+(0.0225P)^2^+0.0000sin\q/\l] where P = 0.33333Fo^2^ + 0.66667Fc^2^ ; _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 4400 _refine_ls_number_parameters 281 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0877 _refine_ls_R_factor_gt 0.0361 _refine_ls_wR_factor_ref 0.0670 _refine_ls_wR_factor_gt 0.0579 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _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 C2S C 0.5183(5) 0.9818(3) 0.3120(3) 0.0760(14) Uani 1 1 d . . . H2S1 H 0.4870 0.9197 0.3224 0.114 Uiso 1 1 calc R . . H2S2 H 0.6259 0.9858 0.3161 0.114 Uiso 1 1 calc R . . H2S3 H 0.4866 0.9996 0.2584 0.114 Uiso 1 1 calc R . . C1S C 0.4522(6) 1.0416(3) 0.3698(3) 0.0710(13) Uani 1 1 d . . . N1S N 0.3994(6) 1.0882(3) 0.4149(3) 0.1248(19) Uani 1 1 d . . . Mo1 Mo 0.11011(3) 0.91739(2) 0.201901(18) 0.03553(9) Uani 1 1 d . . . O3 O -0.0722(2) 0.84058(15) 0.21480(13) 0.0389(6) Uani 1 1 d . . . O4 O 0.2065(2) 1.03653(15) 0.19122(12) 0.0392(6) Uani 1 1 d . . . O1 O 0.1767(2) 0.87082(16) 0.11472(13) 0.0474(6) Uani 1 1 d . . . N3 N -0.0178(3) 1.00085(19) 0.30772(15) 0.0391(7) Uani 1 1 d . . . O5 O 0.4477(3) 1.13814(17) 0.17884(15) 0.0541(7) Uani 1 1 d . . . N2 N -0.0722(3) 0.99182(18) 0.12996(15) 0.0322(6) Uani 1 1 d . . . C6 C -0.0533(4) 1.0632(2) 0.08471(18) 0.0360(8) Uani 1 1 d . . . H6 H -0.1333 1.0812 0.0516 0.043 Uiso 1 1 calc R . . C1 C -0.2094(4) 0.9423(2) 0.13027(18) 0.0326(8) Uani 1 1 d . . . C5 C -0.4508(4) 0.9170(3) 0.0934(2) 0.0507(9) Uani 1 1 d . . . H5 H -0.5375 0.9354 0.0659 0.061 Uiso 1 1 calc R . . C8 C 0.2061(4) 1.1012(2) 0.13285(18) 0.0333(8) Uani 1 1 d . . . C2 C -0.2022(4) 0.8613(2) 0.17541(19) 0.0335(8) Uani 1 1 d . . . C7 C 0.0814(4) 1.1169(2) 0.08165(19) 0.0353(8) Uani 1 1 d . . . C9 C 0.3334(4) 1.1583(2) 0.1264(2) 0.0423(9) Uani 1 1 d . . . C33 C -0.1636(4) 1.0921(3) 0.4353(2) 0.0470(9) Uani 1 1 d . . . O2 O 0.2081(3) 0.86797(16) 0.27896(14) 0.0512(6) Uani 1 1 d . . . C31 C -0.0786(4) 0.9557(2) 0.3697(2) 0.0434(9) Uani 1 1 d . . . H31 H -0.0723 0.8917 0.3699 0.052 Uiso 1 1 calc R . . N1 N -0.3294(3) 0.9712(2) 0.08906(16) 0.0422(7) Uani 1 1 d . . . C32 C -0.1499(4) 0.9978(3) 0.4332(2) 0.0489(10) Uani 1 1 d . . . H32 H -0.1891 0.9623 0.4751 0.059 Uiso 1 1 calc R . . C35 C -0.0301(4) 1.0927(3) 0.3101(2) 0.0501(9) Uani 1 1 d . . . H35 H 0.0122 1.1269 0.2683 0.060 Uiso 1 1 calc R . . C4 C -0.4547(4) 0.8360(3) 0.1361(2) 0.0519(10) Uani 1 1 d . . . H4 H -0.5420 0.8006 0.1364 0.062 Uiso 1 1 calc R . . C3 C -0.3290(4) 0.8071(2) 0.1785(2) 0.0446(9) Uani 1 1 d . . . H3 H -0.3299 0.7526 0.2083 0.054 Uiso 1 1 calc R . . C10 C 0.3348(5) 1.2279(3) 0.0697(2) 0.0511(10) Uani 1 1 d . . . H10 H 0.4192 1.2654 0.0653 0.061 Uiso 1 1 calc R . . C11 C 0.2117(5) 1.2429(3) 0.0192(2) 0.0521(10) Uani 1 1 d . . . H11 H 0.2143 1.2900 -0.0190 0.062 Uiso 1 1 calc R . . C34 C -0.1024(5) 1.1391(3) 0.3714(2) 0.0538(10) Uani 1 1 d . . . H34 H -0.1098 1.2030 0.3694 0.065 Uiso 1 1 calc R . . C12 C 0.0876(4) 1.1892(2) 0.0253(2) 0.0443(9) Uani 1 1 d . . . H12 H 0.0053 1.2005 -0.0084 0.053 Uiso 1 1 calc R . . C13 C 0.5856(4) 1.1863(3) 0.1697(3) 0.0810(14) Uani 1 1 d . . . H13A H 0.6558 1.1662 0.2106 0.121 Uiso 1 1 calc R . . H13B H 0.5682 1.2512 0.1755 0.121 Uiso 1 1 calc R . . H13C H 0.6259 1.1740 0.1169 0.121 Uiso 1 1 calc R . . C36 C -0.2426(5) 1.1411(3) 0.5030(2) 0.0674(12) Uani 1 1 d . . . H36A H -0.2773 1.0968 0.5419 0.101 Uiso 0.50 1 calc PR . . H36B H -0.3269 1.1746 0.4814 0.101 Uiso 0.50 1 calc PR . . H36C H -0.1741 1.1831 0.5290 0.101 Uiso 0.50 1 calc PR . . H36D H -0.2416 1.2062 0.4930 0.101 Uiso 0.50 1 calc PR . . H36E H -0.1919 1.1284 0.5535 0.101 Uiso 0.50 1 calc PR . . H36F H -0.3448 1.1199 0.5059 0.101 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 C2S 0.055(3) 0.082(3) 0.091(3) -0.023(3) -0.011(3) 0.010(3) C1S 0.067(3) 0.059(3) 0.087(3) 0.005(3) 0.020(3) 0.008(3) N1S 0.153(5) 0.088(3) 0.135(4) -0.002(3) 0.072(4) 0.027(3) Mo1 0.02725(14) 0.03438(16) 0.04494(17) 0.00135(18) -0.00073(11) 0.00017(19) O3 0.0323(13) 0.0363(14) 0.0482(14) 0.0039(11) 0.0006(11) -0.0042(11) O4 0.0323(13) 0.0395(14) 0.0458(14) 0.0042(11) -0.0013(11) -0.0079(12) O1 0.0316(13) 0.0515(15) 0.0591(15) -0.0063(12) 0.0047(11) -0.0009(12) N3 0.0397(17) 0.0384(18) 0.0390(16) 0.0024(14) 0.0020(14) -0.0016(15) O5 0.0322(14) 0.0535(17) 0.0766(18) -0.0100(14) -0.0019(13) -0.0166(13) N2 0.0271(15) 0.0322(16) 0.0372(16) -0.0018(13) 0.0013(12) -0.0043(13) C6 0.0322(18) 0.043(2) 0.0332(17) -0.0006(16) 0.0015(14) 0.0042(17) C1 0.0252(17) 0.035(2) 0.0376(19) -0.0052(15) 0.0060(14) -0.0015(15) C5 0.0281(18) 0.063(3) 0.061(2) -0.006(2) -0.0001(16) 0.000(2) C8 0.0355(18) 0.029(2) 0.0351(18) -0.0058(16) 0.0080(15) -0.0041(16) C2 0.0283(18) 0.034(2) 0.0378(19) -0.0049(16) 0.0095(15) -0.0012(17) C7 0.036(2) 0.0324(19) 0.0373(19) 0.0012(16) 0.0077(15) -0.0048(16) C9 0.037(2) 0.038(2) 0.053(2) -0.0131(19) 0.0109(18) -0.0066(18) C33 0.049(2) 0.048(3) 0.044(2) -0.002(2) -0.0023(17) 0.003(2) O2 0.0432(15) 0.0506(16) 0.0598(15) 0.0074(13) -0.0056(12) 0.0081(13) C31 0.046(2) 0.036(2) 0.048(2) 0.0098(18) 0.0025(18) 0.0023(19) N1 0.0312(17) 0.0456(19) 0.0497(18) -0.0008(15) -0.0011(14) 0.0005(15) C32 0.053(3) 0.053(3) 0.041(2) 0.0095(19) 0.0086(19) -0.002(2) C35 0.067(3) 0.036(2) 0.047(2) 0.008(2) 0.0111(18) -0.003(2) C4 0.032(2) 0.060(3) 0.064(3) -0.005(2) 0.0065(19) -0.014(2) C3 0.040(2) 0.045(2) 0.049(2) -0.0049(18) 0.0127(18) -0.0116(19) C10 0.051(3) 0.043(2) 0.059(2) -0.010(2) 0.024(2) -0.022(2) C11 0.068(3) 0.038(2) 0.050(2) 0.0037(19) 0.017(2) -0.010(2) C34 0.075(3) 0.034(2) 0.052(2) -0.0007(19) 0.007(2) 0.000(2) C12 0.050(2) 0.040(2) 0.043(2) 0.0013(18) 0.0057(18) -0.006(2) C13 0.039(3) 0.072(3) 0.132(4) -0.007(3) 0.000(3) -0.027(2) C36 0.074(3) 0.067(3) 0.062(3) -0.017(2) 0.017(2) -0.003(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C2S C1S 1.418(6) . ? C2S H2S1 0.9600 . ? C2S H2S2 0.9600 . ? C2S H2S3 0.9600 . ? C1S N1S 1.111(5) . ? Mo1 O2 1.693(2) . ? Mo1 O1 1.698(2) . ? Mo1 O4 1.939(2) . ? Mo1 O3 1.979(2) . ? Mo1 N2 2.273(3) . ? Mo1 N3 2.414(3) . ? O3 C2 1.355(4) . ? O4 C8 1.344(3) . ? N3 C31 1.331(4) . ? N3 C35 1.339(4) . ? O5 C9 1.360(4) . ? O5 C13 1.420(4) . ? N2 C6 1.288(4) . ? N2 C1 1.415(4) . ? C6 C7 1.430(4) . ? C6 H6 0.9300 . ? C1 N1 1.328(4) . ? C1 C2 1.393(4) . ? C5 N1 1.337(4) . ? C5 C4 1.370(5) . ? C5 H5 0.9300 . ? C8 C7 1.406(4) . ? C8 C9 1.407(4) . ? C2 C3 1.376(4) . ? C7 C12 1.403(4) . ? C9 C10 1.376(5) . ? C33 C34 1.371(5) . ? C33 C32 1.375(5) . ? C33 C36 1.502(5) . ? C31 C32 1.371(5) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C35 C34 1.377(5) . ? C35 H35 0.9300 . ? C4 C3 1.379(5) . ? C4 H4 0.9300 . ? C3 H3 0.9300 . ? C10 C11 1.387(5) . ? C10 H10 0.9300 . ? C11 C12 1.354(5) . ? C11 H11 0.9300 . ? C34 H34 0.9300 . ? C12 H12 0.9300 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C36 H36D 0.9600 . ? C36 H36E 0.9600 . ? C36 H36F 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1S C2S H2S1 109.5 . . ? C1S C2S H2S2 109.5 . . ? H2S1 C2S H2S2 109.5 . . ? C1S C2S H2S3 109.5 . . ? H2S1 C2S H2S3 109.5 . . ? H2S2 C2S H2S3 109.5 . . ? N1S C1S C2S 179.5(6) . . ? O2 Mo1 O1 106.54(11) . . ? O2 Mo1 O4 102.74(10) . . ? O1 Mo1 O4 96.96(10) . . ? O2 Mo1 O3 95.62(10) . . ? O1 Mo1 O3 99.06(10) . . ? O4 Mo1 O3 151.04(9) . . ? O2 Mo1 N2 162.29(10) . . ? O1 Mo1 N2 89.99(10) . . ? O4 Mo1 N2 80.95(9) . . ? O3 Mo1 N2 75.10(9) . . ? O2 Mo1 N3 85.04(10) . . ? O1 Mo1 N3 168.41(10) . . ? O4 Mo1 N3 80.14(9) . . ? O3 Mo1 N3 79.33(9) . . ? N2 Mo1 N3 78.49(9) . . ? C2 O3 Mo1 121.30(19) . . ? C8 O4 Mo1 133.58(18) . . ? C31 N3 C35 115.7(3) . . ? C31 N3 Mo1 120.2(2) . . ? C35 N3 Mo1 124.1(2) . . ? C9 O5 C13 117.9(3) . . ? C6 N2 C1 121.7(3) . . ? C6 N2 Mo1 126.1(2) . . ? C1 N2 Mo1 111.57(19) . . ? N2 C6 C7 124.8(3) . . ? N2 C6 H6 117.6 . . ? C7 C6 H6 117.6 . . ? N1 C1 C2 124.9(3) . . ? N1 C1 N2 121.8(3) . . ? C2 C1 N2 113.2(3) . . ? N1 C5 C4 123.8(3) . . ? N1 C5 H5 118.1 . . ? C4 C5 H5 118.1 . . ? O4 C8 C7 122.7(3) . . ? O4 C8 C9 117.9(3) . . ? C7 C8 C9 119.4(3) . . ? O3 C2 C3 123.5(3) . . ? O3 C2 C1 118.6(3) . . ? C3 C2 C1 117.9(3) . . ? C12 C7 C8 118.9(3) . . ? C12 C7 C6 117.9(3) . . ? C8 C7 C6 123.2(3) . . ? O5 C9 C10 125.3(3) . . ? O5 C9 C8 115.0(3) . . ? C10 C9 C8 119.7(3) . . ? C34 C33 C32 116.2(3) . . ? C34 C33 C36 121.7(4) . . ? C32 C33 C36 122.1(3) . . ? N3 C31 C32 124.0(3) . . ? N3 C31 H31 118.0 . . ? C32 C31 H31 118.0 . . ? C1 N1 C5 115.6(3) . . ? C31 C32 C33 120.2(3) . . ? C31 C32 H32 119.9 . . ? C33 C32 H32 119.9 . . ? N3 C35 C34 123.2(3) . . ? N3 C35 H35 118.4 . . ? C34 C35 H35 118.4 . . ? C5 C4 C3 119.8(3) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C2 C3 C4 117.9(3) . . ? C2 C3 H3 121.0 . . ? C4 C3 H3 121.0 . . ? C9 C10 C11 120.7(4) . . ? C9 C10 H10 119.6 . . ? C11 C10 H10 119.6 . . ? C12 C11 C10 120.4(3) . . ? C12 C11 H11 119.8 . . ? C10 C11 H11 119.8 . . ? C33 C34 C35 120.6(4) . . ? C33 C34 H34 119.7 . . ? C35 C34 H34 119.7 . . ? C11 C12 C7 121.0(4) . . ? C11 C12 H12 119.5 . . ? C7 C12 H12 119.5 . . ? O5 C13 H13A 109.5 . . ? O5 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? O5 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C33 C36 H36D 109.5 . . ? H36A C36 H36D 141.1 . . ? H36B C36 H36D 56.3 . . ? H36C C36 H36D 56.3 . . ? C33 C36 H36E 109.5 . . ? H36A C36 H36E 56.3 . . ? H36B C36 H36E 141.1 . . ? H36C C36 H36E 56.3 . . ? H36D C36 H36E 109.5 . . ? C33 C36 H36F 109.5 . . ? H36A C36 H36F 56.3 . . ? H36B C36 H36F 56.3 . . ? H36C C36 H36F 141.1 . . ? H36D C36 H36F 109.5 . . ? H36E C36 H36F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.376 _refine_diff_density_min -0.359 _refine_diff_density_rms 0.064 #===END data_I(Im)_x_CH3CN _database_code_depnum_ccdc_archive 'CCDC 799778' #TrackingRef 'Uzarevic_et_al_cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; (Imidazole)cis-dioxo(N-3-methoxysalicylidene-2-amino -3-hydroxypyridine)molybdenum(VI) acetonitrile solvate ; _chemical_name_common ; (Imidazole)cis-dioxo(N-3-methoxysalicylidene-2-amino -3- hydroxypyridine)molybdenum(VI) acetonitrile solvate ; _chemical_melting_point ? _chemical_formula_moiety 'C16 H14 Mo N4 O5, C2 H3 N' _chemical_formula_sum 'C18 H17 Mo N5 O5' _chemical_formula_weight 479.31 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.5668(3) _cell_length_b 19.3973(7) _cell_length_c 14.5305(6) _cell_angle_alpha 90.00 _cell_angle_beta 116.626(3) _cell_angle_gamma 90.00 _cell_volume 1906.55(13) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 2323 _cell_measurement_theta_min 4.1431 _cell_measurement_theta_max 28.7144 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.670 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 968 _exptl_absorpt_coefficient_mu 0.730 _exptl_absorpt_correction_T_min 0.97121 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.3426 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7292 _diffrn_reflns_av_R_equivalents 0.0424 _diffrn_reflns_av_sigmaI/netI 0.1015 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 4.15 _diffrn_reflns_theta_max 25.50 _reflns_number_total 3536 _reflns_number_gt 2154 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) ; _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is 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 [0.00000+1.00000exp(3.00(sin\q/\l)^2^)]/ [\s^2^(Fo^2^)+0.0000+0.0000*P+(0.0158P)^2^+0.0000sin\q/\l] where P = 0.33333Fo^2^ + 0.66667Fc^2^ ; _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 3536 _refine_ls_number_parameters 266 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0720 _refine_ls_R_factor_gt 0.0333 _refine_ls_wR_factor_ref 0.0615 _refine_ls_wR_factor_gt 0.0552 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.024 _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 0.13814(5) 0.824336(17) 0.05457(2) 0.02996(10) Uani 1 1 d . . . O1 O -0.1026(4) 0.84788(13) -0.0078(2) 0.0453(7) Uani 1 1 d . . . O2 O 0.1344(4) 0.74082(12) 0.08760(19) 0.0403(7) Uani 1 1 d . . . O3 O 0.1799(4) 0.80739(12) -0.06800(19) 0.0392(7) Uani 1 1 d . . . O4 O 0.1953(4) 0.87080(12) 0.18316(19) 0.0362(6) Uani 1 1 d . . . O5 O 0.1918(4) 0.88832(13) 0.35701(19) 0.0426(7) Uani 1 1 d . . . N1 N 0.2632(4) 0.98226(17) -0.1230(2) 0.0381(8) Uani 1 1 d . . . N2 N 0.2308(4) 0.92832(15) 0.0180(2) 0.0297(7) Uani 1 1 d . . . N3 N 0.4856(4) 0.81088(14) 0.1383(2) 0.0323(7) Uani 1 1 d . . . N4 N 0.8056(5) 0.8231(2) 0.2084(3) 0.0490(9) Uani 1 1 d D . . H4N H 0.918(4) 0.839(2) 0.226(3) 0.059 Uiso 1 1 d D . . C1 C 0.2359(5) 0.92554(19) -0.0790(3) 0.0305(9) Uani 1 1 d . . . C2 C 0.2063(5) 0.8600(2) -0.1205(3) 0.0321(9) Uani 1 1 d . . . C3 C 0.2040(6) 0.8520(2) -0.2155(3) 0.0460(11) Uani 1 1 d . . . H3 H 0.1852 0.8089 -0.2463 0.055 Uiso 1 1 calc R . . C4 C 0.2300(6) 0.9094(2) -0.2629(3) 0.0500(12) Uani 1 1 d . . . H4 H 0.2286 0.9056 -0.3270 0.060 Uiso 1 1 calc R . . C5 C 0.2581(6) 0.9724(2) -0.2155(3) 0.0477(11) Uani 1 1 d . . . H5 H 0.2747 1.0106 -0.2495 0.057 Uiso 1 1 calc R . . C6 C 0.2540(5) 0.98508(18) 0.0673(3) 0.0315(9) Uani 1 1 d . . . H6 H 0.2744 1.0249 0.0377 0.038 Uiso 1 1 calc R . . C7 C 0.2506(5) 0.99144(18) 0.1652(3) 0.0309(9) Uani 1 1 d . . . C8 C 0.2238(5) 0.93570(18) 0.2183(3) 0.0281(8) Uani 1 1 d . . . C9 C 0.2242(5) 0.94609(19) 0.3136(3) 0.0307(9) Uani 1 1 d . . . C10 C 0.2533(6) 1.0108(2) 0.3555(3) 0.0439(11) Uani 1 1 d . . . H10 H 0.2550 1.0174 0.4193 0.053 Uiso 1 1 calc R . . C11 C 0.2802(6) 1.0664(2) 0.3031(3) 0.0460(11) Uani 1 1 d . . . H11 H 0.2978 1.1104 0.3314 0.055 Uiso 1 1 calc R . . C12 C 0.2810(5) 1.05705(19) 0.2107(3) 0.0420(10) Uani 1 1 d . . . H12 H 0.3019 1.0946 0.1771 0.050 Uiso 1 1 calc R . . C13 C 0.1958(7) 0.8957(2) 0.4560(3) 0.0616(13) Uani 1 1 d . . . H13A H 0.1713 0.8518 0.4785 0.092 Uiso 1 1 calc R . . H13B H 0.0957 0.9278 0.4514 0.092 Uiso 1 1 calc R . . H13C H 0.3232 0.9124 0.5045 0.092 Uiso 1 1 calc R . . C31 C 0.6315(6) 0.8492(2) 0.1435(3) 0.0445(11) Uani 1 1 d . . . H31 H 0.6157 0.8897 0.1065 0.053 Uiso 1 1 calc R . . C32 C 0.7721(6) 0.7649(2) 0.2482(3) 0.0492(11) Uani 1 1 d . . . H32 H 0.8660 0.7359 0.2963 0.059 Uiso 1 1 calc R . . C33 C 0.5756(6) 0.7575(2) 0.2044(3) 0.0425(10) Uani 1 1 d . . . H33 H 0.5094 0.7212 0.2170 0.051 Uiso 1 1 calc R . . N1S N 0.7092(7) 0.9075(3) 0.4150(4) 0.0890(16) Uani 1 1 d . . . C1S C 0.6653(8) 0.8563(3) 0.4337(4) 0.0647(15) Uani 1 1 d . . . C2S C 0.6092(8) 0.7912(3) 0.4579(4) 0.0845(18) Uani 1 1 d . . . H2S1 H 0.6624 0.7866 0.5312 0.127 Uiso 1 1 calc R . . H2S2 H 0.6596 0.7550 0.4313 0.127 Uiso 1 1 calc R . . H2S3 H 0.4676 0.7883 0.4274 0.127 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 0.03154(17) 0.02889(16) 0.02853(16) -0.00038(19) 0.01265(12) -0.0041(2) O1 0.0315(15) 0.0488(17) 0.0512(17) 0.0094(13) 0.0146(13) 0.0005(13) O2 0.0466(17) 0.0335(15) 0.0390(17) -0.0020(12) 0.0177(14) -0.0096(13) O3 0.0472(16) 0.0379(17) 0.0337(15) -0.0088(12) 0.0192(13) -0.0074(13) O4 0.0525(17) 0.0283(15) 0.0343(15) 0.0006(12) 0.0253(13) -0.0024(13) O5 0.0537(18) 0.0525(18) 0.0267(15) -0.0006(13) 0.0226(14) -0.0086(15) N1 0.0358(19) 0.048(2) 0.034(2) 0.0061(16) 0.0186(16) -0.0008(17) N2 0.0320(18) 0.0319(18) 0.0252(17) -0.0006(14) 0.0128(14) -0.0019(15) N3 0.0303(17) 0.033(2) 0.0328(17) 0.0023(15) 0.0131(14) 0.0010(16) N4 0.0288(19) 0.056(2) 0.056(2) 0.000(2) 0.0131(18) 0.003(2) C1 0.028(2) 0.039(2) 0.026(2) 0.0019(17) 0.0123(17) 0.0001(19) C2 0.025(2) 0.042(2) 0.029(2) -0.0008(18) 0.0114(17) 0.0027(18) C3 0.046(3) 0.063(3) 0.033(2) -0.011(2) 0.020(2) -0.008(2) C4 0.047(3) 0.077(3) 0.035(3) 0.001(2) 0.026(2) 0.002(3) C5 0.044(3) 0.063(3) 0.044(3) 0.017(2) 0.027(2) 0.000(2) C6 0.032(2) 0.028(2) 0.033(2) 0.0050(17) 0.0133(18) 0.0026(18) C7 0.027(2) 0.034(2) 0.029(2) -0.0017(17) 0.0110(17) 0.0008(18) C8 0.025(2) 0.030(2) 0.029(2) -0.0002(17) 0.0112(17) 0.0039(18) C9 0.024(2) 0.039(2) 0.028(2) -0.0022(18) 0.0106(17) -0.0010(18) C10 0.049(3) 0.051(3) 0.033(3) -0.008(2) 0.020(2) 0.003(2) C11 0.059(3) 0.033(2) 0.043(3) -0.012(2) 0.020(2) -0.004(2) C12 0.050(3) 0.034(2) 0.040(3) -0.0011(19) 0.018(2) -0.003(2) C13 0.080(3) 0.079(4) 0.034(3) -0.003(2) 0.033(3) -0.012(3) C31 0.043(3) 0.039(2) 0.047(3) 0.003(2) 0.017(2) 0.001(2) C32 0.040(3) 0.058(3) 0.046(3) 0.011(2) 0.015(2) 0.012(2) C33 0.039(2) 0.039(2) 0.048(3) 0.012(2) 0.019(2) 0.006(2) N1S 0.080(4) 0.087(4) 0.110(4) -0.002(3) 0.051(3) 0.001(3) C1S 0.058(4) 0.083(4) 0.057(3) -0.001(3) 0.028(3) 0.020(3) C2S 0.111(5) 0.072(4) 0.093(5) 0.014(3) 0.067(4) 0.022(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 O2 1.693(2) . ? Mo1 O1 1.694(2) . ? Mo1 O4 1.941(2) . ? Mo1 O3 1.971(2) . ? Mo1 N2 2.275(3) . ? Mo1 N3 2.365(3) . ? O3 C2 1.342(4) . ? O4 C8 1.339(4) . ? O5 C9 1.361(4) . ? O5 C13 1.432(4) . ? N1 C1 1.334(4) . ? N1 C5 1.341(4) . ? N2 C6 1.282(4) . ? N2 C1 1.428(4) . ? N3 C31 1.304(4) . ? N3 C33 1.368(4) . ? N4 C31 1.329(5) . ? N4 C32 1.343(5) . ? N4 H4N 0.834(18) . ? C1 C2 1.381(5) . ? C2 C3 1.381(5) . ? C3 C4 1.368(5) . ? C3 H3 0.9300 . ? C4 C5 1.373(6) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C7 1.440(5) . ? C6 H6 0.9300 . ? C7 C8 1.395(5) . ? C7 C12 1.405(5) . ? C8 C9 1.398(4) . ? C9 C10 1.369(5) . ? C10 C11 1.387(5) . ? C10 H10 0.9300 . ? C11 C12 1.357(5) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C31 H31 0.9300 . ? C32 C33 1.338(5) . ? C32 H32 0.9300 . ? C33 H33 0.9300 . ? N1S C1S 1.119(6) . ? C1S C2S 1.425(7) . ? C2S H2S1 0.9600 . ? C2S H2S2 0.9600 . ? C2S H2S3 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Mo1 O1 105.01(12) . . ? O2 Mo1 O4 101.32(11) . . ? O1 Mo1 O4 96.45(11) . . ? O2 Mo1 O3 97.26(10) . . ? O1 Mo1 O3 97.51(11) . . ? O4 Mo1 O3 152.96(10) . . ? O2 Mo1 N2 163.81(11) . . ? O1 Mo1 N2 90.35(11) . . ? O4 Mo1 N2 81.62(10) . . ? O3 Mo1 N2 75.26(10) . . ? O2 Mo1 N3 84.53(11) . . ? O1 Mo1 N3 170.44(11) . . ? O4 Mo1 N3 80.76(10) . . ? O3 Mo1 N3 81.66(10) . . ? N2 Mo1 N3 80.21(10) . . ? C2 O3 Mo1 120.8(2) . . ? C8 O4 Mo1 137.0(2) . . ? C9 O5 C13 117.2(3) . . ? C1 N1 C5 114.9(3) . . ? C6 N2 C1 121.8(3) . . ? C6 N2 Mo1 127.6(2) . . ? C1 N2 Mo1 110.2(2) . . ? C31 N3 C33 104.4(3) . . ? C31 N3 Mo1 133.1(3) . . ? C33 N3 Mo1 122.2(2) . . ? C31 N4 C32 107.9(3) . . ? C31 N4 H4N 129(3) . . ? C32 N4 H4N 123(3) . . ? N1 C1 C2 125.4(3) . . ? N1 C1 N2 121.3(3) . . ? C2 C1 N2 113.2(3) . . ? O3 C2 C3 123.0(3) . . ? O3 C2 C1 119.2(3) . . ? C3 C2 C1 117.8(4) . . ? C4 C3 C2 118.2(4) . . ? C4 C3 H3 120.9 . . ? C2 C3 H3 120.9 . . ? C3 C4 C5 119.7(4) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? N1 C5 C4 124.0(4) . . ? N1 C5 H5 118.0 . . ? C4 C5 H5 118.0 . . ? N2 C6 C7 124.6(3) . . ? N2 C6 H6 117.7 . . ? C7 C6 H6 117.7 . . ? C8 C7 C12 118.4(3) . . ? C8 C7 C6 123.5(3) . . ? C12 C7 C6 118.1(3) . . ? O4 C8 C7 123.8(3) . . ? O4 C8 C9 116.2(3) . . ? C7 C8 C9 120.0(3) . . ? O5 C9 C10 125.1(3) . . ? O5 C9 C8 114.8(3) . . ? C10 C9 C8 120.1(4) . . ? C9 C10 C11 120.2(4) . . ? C9 C10 H10 119.9 . . ? C11 C10 H10 119.9 . . ? C12 C11 C10 120.4(4) . . ? C12 C11 H11 119.8 . . ? C10 C11 H11 119.8 . . ? C11 C12 C7 121.0(4) . . ? C11 C12 H12 119.5 . . ? C7 C12 H12 119.5 . . ? O5 C13 H13A 109.5 . . ? O5 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? O5 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N3 C31 N4 111.6(4) . . ? N3 C31 H31 124.2 . . ? N4 C31 H31 124.2 . . ? C33 C32 N4 105.6(4) . . ? C33 C32 H32 127.2 . . ? N4 C32 H32 127.2 . . ? C32 C33 N3 110.5(4) . . ? C32 C33 H33 124.7 . . ? N3 C33 H33 124.7 . . ? N1S C1S C2S 179.7(6) . . ? C1S C2S H2S1 109.5 . . ? C1S C2S H2S2 109.5 . . ? H2S1 C2S H2S2 109.5 . . ? C1S C2S H2S3 109.5 . . ? H2S1 C2S H2S3 109.5 . . ? H2S2 C2S H2S3 109.5 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.269 _refine_diff_density_min -0.296 _refine_diff_density_rms 0.068 #===END data_I(Im) _database_code_depnum_ccdc_archive 'CCDC 799779' #TrackingRef 'Uzarevic_et_al_cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; (Imidazole)cis-dioxo(N-3-methoxysalicylidene -2-amino-3-hydroxypyridine)molybdenum(VI) ; _chemical_name_common ; (Imidazole)cis-dioxo(N-3-methoxysalicylidene -2-amino-3- hydroxypyridine)molybdenum(VI) ; _chemical_melting_point ? _chemical_formula_moiety 'C16 H14 Mo N4 O5' _chemical_formula_sum 'C16 H14 Mo N4 O5' _chemical_formula_weight 438.25 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-p 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.4565(4) _cell_length_b 17.8707(14) _cell_length_c 12.2079(9) _cell_angle_alpha 90.00 _cell_angle_beta 93.021(6) _cell_angle_gamma 90.00 _cell_volume 1624.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 4461 _cell_measurement_theta_min 4.1991 _cell_measurement_theta_max 32.4608 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.792 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 880 _exptl_absorpt_coefficient_mu 0.845 _exptl_absorpt_correction_T_min 0.97203 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.3426 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8797 _diffrn_reflns_av_R_equivalents 0.0211 _diffrn_reflns_av_sigmaI/netI 0.0312 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 4.21 _diffrn_reflns_theta_max 29.00 _reflns_number_total 4303 _reflns_number_gt 3437 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) ; _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is 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^)+(0.0352P)^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 4303 _refine_ls_number_parameters 238 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0338 _refine_ls_R_factor_gt 0.0241 _refine_ls_wR_factor_ref 0.0625 _refine_ls_wR_factor_gt 0.0605 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _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 C12 C 0.1654(2) 0.44088(12) 1.05845(15) 0.0304(4) Uani 1 1 d . . . H12 H 0.1999 0.4699 1.1192 0.036 Uiso 1 1 calc R . . C11 C 0.0614(3) 0.37863(12) 1.07175(17) 0.0355(4) Uani 1 1 d . . . H11 H 0.0294 0.3647 1.1415 0.043 Uiso 1 1 calc R . . C13 C -0.1455(3) 0.26864(15) 0.7869(2) 0.0558(7) Uani 1 1 d . . . H13A H -0.1693 0.2467 0.7158 0.084 Uiso 1 1 calc R . . H13B H -0.2501 0.2951 0.8084 0.084 Uiso 1 1 calc R . . H13C H -0.1160 0.2299 0.8393 0.084 Uiso 1 1 calc R . . Mo1 Mo 0.418751(19) 0.483857(9) 0.703137(12) 0.02436(6) Uani 1 1 d . . . O3 O 0.54555(16) 0.57955(8) 0.67571(11) 0.0304(3) Uani 1 1 d . . . O4 O 0.21474(17) 0.43171(7) 0.76090(10) 0.0301(3) Uani 1 1 d . . . N2 N 0.37315(18) 0.55536(8) 0.85318(12) 0.0245(3) Uani 1 1 d . . . O5 O 0.00043(19) 0.31911(8) 0.78275(12) 0.0407(3) Uani 1 1 d . . . N3 N 0.17763(19) 0.55738(9) 0.62762(12) 0.0281(3) Uani 1 1 d . . . N1 N 0.4443(2) 0.67684(9) 0.92430(14) 0.0337(4) Uani 1 1 d . . . O2 O 0.41942(17) 0.44445(8) 0.57603(11) 0.0329(3) Uani 1 1 d . . . C1 C 0.4541(2) 0.62636(10) 0.84526(15) 0.0262(4) Uani 1 1 d . . . O1 O 0.58538(18) 0.43962(9) 0.77739(12) 0.0418(4) Uani 1 1 d . . . C2 C 0.5437(2) 0.63614(11) 0.74855(16) 0.0277(4) Uani 1 1 d . . . C6 C 0.3126(2) 0.53171(10) 0.94360(15) 0.0257(4) Uani 1 1 d . . . H6 H 0.3293 0.5617 1.0055 0.031 Uiso 1 1 calc R . . C9 C 0.0533(2) 0.35542(11) 0.87724(16) 0.0293(4) Uani 1 1 d . . . C8 C 0.1688(2) 0.41688(10) 0.86345(14) 0.0253(4) Uani 1 1 d . . . C7 C 0.2205(2) 0.46143(10) 0.95464(15) 0.0249(4) Uani 1 1 d . . . C32 C 0.0202(3) 0.61456(13) 0.49246(18) 0.0417(5) Uani 1 1 d . . . H32 H -0.0108 0.6413 0.4289 0.050 Uiso 1 1 calc R . . N4 N -0.0936(2) 0.58365(11) 0.56305(16) 0.0406(4) Uani 1 1 d D . . H4N H -0.208(2) 0.5784(13) 0.5588(19) 0.049 Uiso 1 1 d D . . C5 C 0.5297(3) 0.74177(12) 0.90824(19) 0.0409(5) Uani 1 1 d . . . H5 H 0.5264 0.7785 0.9621 0.049 Uiso 1 1 calc R . . C3 C 0.6301(3) 0.70381(11) 0.73385(18) 0.0354(4) Uani 1 1 d . . . H3 H 0.6914 0.7132 0.6709 0.043 Uiso 1 1 calc R . . C31 C 0.0049(3) 0.54978(12) 0.64198(17) 0.0347(4) Uani 1 1 d . . . H31 H -0.0421 0.5240 0.7001 0.042 Uiso 1 1 calc R . . C33 C 0.1870(3) 0.59858(12) 0.53331(17) 0.0355(4) Uani 1 1 d . . . H33 H 0.2927 0.6133 0.5023 0.043 Uiso 1 1 calc R . . C10 C 0.0035(2) 0.33616(12) 0.98060(17) 0.0348(4) Uani 1 1 d . . . H10 H -0.0692 0.2946 0.9897 0.042 Uiso 1 1 calc R . . C4 C 0.6221(3) 0.75675(12) 0.81574(19) 0.0404(5) Uani 1 1 d . . . H4 H 0.6791 0.8026 0.8086 0.049 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 C12 0.0277(9) 0.0387(11) 0.0246(9) 0.0027(8) -0.0004(7) 0.0034(8) C11 0.0351(10) 0.0419(12) 0.0302(10) 0.0092(9) 0.0072(8) 0.0004(9) C13 0.0521(14) 0.0553(15) 0.0596(16) -0.0067(13) -0.0002(11) -0.0284(12) Mo1 0.02319(8) 0.02571(9) 0.02427(8) -0.00292(7) 0.00223(5) -0.00118(6) O3 0.0291(6) 0.0331(7) 0.0295(7) -0.0040(6) 0.0061(5) -0.0076(6) O4 0.0360(7) 0.0301(7) 0.0244(6) -0.0010(5) 0.0037(5) -0.0097(6) N2 0.0219(7) 0.0249(8) 0.0266(7) -0.0018(6) 0.0007(5) -0.0013(6) O5 0.0431(8) 0.0393(8) 0.0401(8) -0.0079(7) 0.0064(6) -0.0180(7) N3 0.0253(7) 0.0311(9) 0.0279(8) -0.0026(7) 0.0022(6) -0.0003(6) N1 0.0351(8) 0.0280(9) 0.0382(9) -0.0059(7) 0.0036(7) -0.0015(7) O2 0.0338(7) 0.0375(8) 0.0279(7) -0.0060(6) 0.0057(5) -0.0017(6) C1 0.0235(8) 0.0236(9) 0.0312(9) -0.0012(7) -0.0022(7) -0.0004(7) O1 0.0410(8) 0.0402(9) 0.0429(9) -0.0061(7) -0.0096(6) 0.0090(7) C2 0.0204(8) 0.0287(10) 0.0337(10) -0.0002(8) -0.0016(7) -0.0003(7) C6 0.0236(8) 0.0285(10) 0.0248(9) -0.0039(7) -0.0010(6) 0.0019(7) C9 0.0267(9) 0.0273(10) 0.0340(10) -0.0001(8) 0.0028(7) -0.0003(8) C8 0.0235(8) 0.0265(9) 0.0258(9) 0.0024(7) 0.0024(7) 0.0020(7) C7 0.0213(8) 0.0273(9) 0.0260(9) 0.0023(7) -0.0001(6) 0.0021(7) C32 0.0473(12) 0.0378(12) 0.0391(12) 0.0031(9) -0.0077(10) 0.0046(10) N4 0.0269(8) 0.0414(11) 0.0529(12) -0.0040(9) -0.0054(8) 0.0029(8) C5 0.0440(11) 0.0273(11) 0.0511(13) -0.0097(10) 0.0002(10) -0.0021(9) C3 0.0326(10) 0.0320(11) 0.0419(12) 0.0049(9) 0.0039(8) -0.0037(8) C31 0.0291(9) 0.0378(11) 0.0374(11) -0.0047(9) 0.0037(8) -0.0018(9) C33 0.0356(10) 0.0361(11) 0.0354(11) 0.0046(9) 0.0059(8) 0.0015(9) C10 0.0322(10) 0.0313(11) 0.0413(12) 0.0061(9) 0.0074(8) -0.0058(8) C4 0.0391(11) 0.0245(10) 0.0574(14) 0.0013(10) -0.0001(10) -0.0076(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 C12 C11 1.371(3) . ? C12 C7 1.402(2) . ? C12 H12 0.9300 . ? C11 C10 1.396(3) . ? C11 H11 0.9300 . ? C13 O5 1.416(2) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? Mo1 O1 1.6947(13) . ? Mo1 O2 1.7043(13) . ? Mo1 O4 1.9476(12) . ? Mo1 O3 1.9909(13) . ? Mo1 N2 2.2737(15) . ? Mo1 N3 2.3736(15) . ? O3 C2 1.347(2) . ? O4 C8 1.342(2) . ? N2 C6 1.286(2) . ? N2 C1 1.410(2) . ? O5 C9 1.364(2) . ? N3 C31 1.316(2) . ? N3 C33 1.372(2) . ? N1 C1 1.326(2) . ? N1 C5 1.343(3) . ? C1 C2 1.398(3) . ? C2 C3 1.387(3) . ? C6 C7 1.441(3) . ? C6 H6 0.9300 . ? C9 C10 1.378(3) . ? C9 C8 1.411(3) . ? C8 C7 1.406(2) . ? C32 C33 1.346(3) . ? C32 N4 1.358(3) . ? C32 H32 0.9300 . ? N4 C31 1.327(3) . ? N4 H4N 0.858(16) . ? C5 C4 1.380(3) . ? C5 H5 0.9300 . ? C3 C4 1.380(3) . ? C3 H3 0.9300 . ? C31 H31 0.9300 . ? C33 H33 0.9300 . ? C10 H10 0.9300 . ? C4 H4 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 C12 C7 120.96(18) . . ? C11 C12 H12 119.5 . . ? C7 C12 H12 119.5 . . ? C12 C11 C10 119.98(18) . . ? C12 C11 H11 120.0 . . ? C10 C11 H11 120.0 . . ? O5 C13 H13A 109.5 . . ? O5 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? O5 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O1 Mo1 O2 104.89(7) . . ? O1 Mo1 O4 98.49(7) . . ? O2 Mo1 O4 99.89(6) . . ? O1 Mo1 O3 98.59(7) . . ? O2 Mo1 O3 100.23(6) . . ? O4 Mo1 O3 149.18(5) . . ? O1 Mo1 N2 88.15(6) . . ? O2 Mo1 N2 166.78(6) . . ? O4 Mo1 N2 79.89(5) . . ? O3 Mo1 N2 75.24(5) . . ? O1 Mo1 N3 170.06(6) . . ? O2 Mo1 N3 85.05(6) . . ? O4 Mo1 N3 79.36(5) . . ? O3 Mo1 N3 79.39(5) . . ? N2 Mo1 N3 81.92(5) . . ? C2 O3 Mo1 120.81(12) . . ? C8 O4 Mo1 132.45(11) . . ? C6 N2 C1 121.70(15) . . ? C6 N2 Mo1 125.52(12) . . ? C1 N2 Mo1 111.57(11) . . ? C9 O5 C13 117.48(17) . . ? C31 N3 C33 105.13(16) . . ? C31 N3 Mo1 128.15(14) . . ? C33 N3 Mo1 123.51(12) . . ? C1 N1 C5 115.93(18) . . ? N1 C1 C2 125.21(18) . . ? N1 C1 N2 121.48(17) . . ? C2 C1 N2 113.31(16) . . ? O3 C2 C3 123.25(18) . . ? O3 C2 C1 119.06(17) . . ? C3 C2 C1 117.68(18) . . ? N2 C6 C7 123.88(16) . . ? N2 C6 H6 118.1 . . ? C7 C6 H6 118.1 . . ? O5 C9 C10 125.15(18) . . ? O5 C9 C8 114.88(17) . . ? C10 C9 C8 119.96(17) . . ? O4 C8 C7 123.67(16) . . ? O4 C8 C9 116.89(16) . . ? C7 C8 C9 119.32(17) . . ? C12 C7 C8 119.11(17) . . ? C12 C7 C6 118.47(17) . . ? C8 C7 C6 122.11(16) . . ? C33 C32 N4 105.94(19) . . ? C33 C32 H32 127.0 . . ? N4 C32 H32 127.0 . . ? C31 N4 C32 107.82(17) . . ? C31 N4 H4N 120.4(16) . . ? C32 N4 H4N 131.2(16) . . ? N1 C5 C4 123.2(2) . . ? N1 C5 H5 118.4 . . ? C4 C5 H5 118.4 . . ? C4 C3 C2 117.8(2) . . ? C4 C3 H3 121.1 . . ? C2 C3 H3 121.1 . . ? N3 C31 N4 111.37(19) . . ? N3 C31 H31 124.3 . . ? N4 C31 H31 124.3 . . ? C32 C33 N3 109.73(18) . . ? C32 C33 H33 125.1 . . ? N3 C33 H33 125.1 . . ? C9 C10 C11 120.47(18) . . ? C9 C10 H10 119.8 . . ? C11 C10 H10 119.8 . . ? C5 C4 C3 120.17(19) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 29.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.508 _refine_diff_density_min -0.519 _refine_diff_density_rms 0.063 #===END data_I(Bp) _database_code_depnum_ccdc_archive 'CCDC 799780' #TrackingRef 'Uzarevic_et_al_cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; (4,4'-bipyridine)bis(cis-dioxo(N-3-methoxysalicylidene -2-amino-3-hydroxypyridine))dimolybdenum(VI) ; _chemical_name_common ; (4,4'-bipyridine)bis(cis-dioxo(N-3-methoxysalicylidene -2- amino-3-hydroxypyridine))dimolybdenum(VI) ; _chemical_melting_point ? _chemical_formula_moiety 'C36 H28 Mo2 N6 O10' _chemical_formula_sum 'C36 H28 Mo2 N6 O10' _chemical_formula_weight 896.52 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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 triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.7871(6) _cell_length_b 12.8269(7) _cell_length_c 13.8071(6) _cell_angle_alpha 108.490(5) _cell_angle_beta 94.104(4) _cell_angle_gamma 113.811(5) _cell_volume 1762.67(19) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 7697 _cell_measurement_theta_min 4.0975 _cell_measurement_theta_max 32.5379 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.689 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 900 _exptl_absorpt_coefficient_mu 0.780 _exptl_absorpt_correction_T_min 0.82657 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.3426 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18949 _diffrn_reflns_av_R_equivalents 0.0325 _diffrn_reflns_av_sigmaI/netI 0.0668 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 4.11 _diffrn_reflns_theta_max 29.50 _reflns_number_total 9792 _reflns_number_gt 6320 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) ; _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is 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^)+(0.0551P)^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 9792 _refine_ls_number_parameters 487 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0719 _refine_ls_R_factor_gt 0.0396 _refine_ls_wR_factor_ref 0.1045 _refine_ls_wR_factor_gt 0.0983 _refine_ls_goodness_of_fit_ref 0.940 _refine_ls_restrained_S_all 0.940 _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 C112 C 0.6124(4) -0.2618(4) -0.0644(3) 0.0533(10) Uani 1 1 d . . . H112 H 0.6147 -0.2362 -0.1204 0.064 Uiso 1 1 calc R . . C110 C 0.6887(4) -0.3514(4) 0.0370(3) 0.0569(11) Uani 1 1 d . . . H110 H 0.7417 -0.3860 0.0482 0.068 Uiso 1 1 calc R . . C111 C 0.6915(4) -0.3122(4) -0.0458(3) 0.0640(12) Uani 1 1 d . . . H111 H 0.7469 -0.3198 -0.0891 0.077 Uiso 1 1 calc R . . Mo12 Mo 0.83728(3) 0.78137(3) 0.68925(2) 0.03267(8) Uani 1 1 d . . . Mo11 Mo 0.28623(3) -0.28708(3) 0.14131(2) 0.03183(8) Uani 1 1 d . . . C17 C 0.5288(3) -0.2488(3) 0.0006(2) 0.0378(8) Uani 1 1 d . . . N4 N 0.6954(3) 0.5627(3) 0.5808(2) 0.0373(6) Uani 1 1 d . . . O24 O 0.8147(2) 0.7946(2) 0.55348(16) 0.0364(5) Uani 1 1 d . . . O23 O 0.8701(2) 0.6980(2) 0.77873(16) 0.0365(5) Uani 1 1 d . . . O13 O 0.1695(2) -0.2164(2) 0.11894(17) 0.0382(5) Uani 1 1 d . . . N3 N 0.4080(3) -0.0705(3) 0.2566(2) 0.0354(6) Uani 1 1 d . . . O12 O 0.2488(2) -0.3066(2) 0.25280(17) 0.0427(6) Uani 1 1 d . . . O15 O 0.5996(3) -0.3740(3) 0.1864(2) 0.0564(7) Uani 1 1 d . . . O21 O 0.9597(2) 0.9236(2) 0.75618(18) 0.0475(6) Uani 1 1 d . . . C22 C 0.9537(3) 0.6508(3) 0.7652(2) 0.0353(7) Uani 1 1 d . . . O14 O 0.4566(2) -0.2733(2) 0.15545(17) 0.0396(6) Uani 1 1 d . . . N12 N 0.3552(3) -0.1982(3) 0.02334(19) 0.0329(6) Uani 1 1 d . . . O22 O 0.7058(2) 0.7850(2) 0.72762(18) 0.0472(6) Uani 1 1 d . . . C33 C 0.5178(3) 0.1793(3) 0.3870(3) 0.0354(7) Uani 1 1 d . . . C12 C 0.1804(3) -0.1591(3) 0.0515(2) 0.0333(7) Uani 1 1 d . . . N21 N 1.0939(3) 0.6086(3) 0.6570(2) 0.0515(8) Uani 1 1 d . . . O25 O 0.7692(3) 0.9014(3) 0.43423(19) 0.0509(7) Uani 1 1 d . . . C31 C 0.5098(3) 0.0133(3) 0.2414(3) 0.0389(8) Uani 1 1 d . . . H31 H 0.5440 -0.0133 0.1854 0.047 Uiso 1 1 calc R . . O11 O 0.2087(3) -0.4282(2) 0.04364(19) 0.0482(6) Uani 1 1 d . . . C18 C 0.5286(3) -0.2877(3) 0.0857(2) 0.0350(7) Uani 1 1 d . . . C43 C 0.5743(3) 0.3105(3) 0.4544(3) 0.0375(7) Uani 1 1 d . . . N22 N 0.9706(3) 0.7058(3) 0.6181(2) 0.0354(6) Uani 1 1 d . . . C29 C 0.8576(3) 0.8610(3) 0.4135(2) 0.0384(8) Uani 1 1 d . . . C26 C 1.0111(3) 0.7092(3) 0.5341(3) 0.0409(8) Uani 1 1 d . . . H26 H 1.0667 0.6752 0.5160 0.049 Uiso 1 1 calc R . . N11 N 0.2971(3) -0.0942(3) -0.0728(2) 0.0450(7) Uani 1 1 d . . . C28 C 0.8846(3) 0.8067(3) 0.4813(2) 0.0335(7) Uani 1 1 d . . . C11 C 0.2774(3) -0.1466(3) -0.0023(2) 0.0333(7) Uani 1 1 d . . . C16 C 0.4456(3) -0.1997(3) -0.0226(2) 0.0365(7) Uani 1 1 d . . . H16 H 0.4578 -0.1668 -0.0743 0.044 Uiso 1 1 calc R . . C45 C 0.6664(4) 0.5228(4) 0.4767(3) 0.0508(10) Uani 1 1 d . . . H45 H 0.6866 0.5810 0.4460 0.061 Uiso 1 1 calc R . . C35 C 0.3624(3) -0.0275(3) 0.3388(3) 0.0436(8) Uani 1 1 d . . . H35 H 0.2917 -0.0838 0.3518 0.052 Uiso 1 1 calc R . . C27 C 0.9764(3) 0.7615(3) 0.4674(3) 0.0402(8) Uani 1 1 d . . . C23 C 0.9836(3) 0.5983(3) 0.8295(3) 0.0420(8) Uani 1 1 d . . . H23 H 0.9467 0.5941 0.8863 0.050 Uiso 1 1 calc R . . C15 C 0.2158(4) -0.0508(4) -0.0906(3) 0.0515(10) Uani 1 1 d . . . H15 H 0.2252 -0.0149 -0.1404 0.062 Uiso 1 1 calc R . . C21 C 1.0108(3) 0.6520(3) 0.6803(3) 0.0380(8) Uani 1 1 d . . . C113 C 0.6669(4) -0.4396(4) 0.2017(3) 0.0646(12) Uani 1 1 d . . . H11A H 0.6530 -0.4571 0.2637 0.097 Uiso 1 1 calc R . . H11B H 0.7563 -0.3907 0.2097 0.097 Uiso 1 1 calc R . . H11C H 0.6370 -0.5154 0.1421 0.097 Uiso 1 1 calc R . . C34 C 0.4129(4) 0.0931(3) 0.4041(3) 0.0448(9) Uani 1 1 d . . . H34 H 0.3772 0.1172 0.4598 0.054 Uiso 1 1 calc R . . C211 C 1.0100(4) 0.8231(4) 0.3189(3) 0.0558(11) Uani 1 1 d . . . H211 H 1.0512 0.8282 0.2644 0.067 Uiso 1 1 calc R . . C13 C 0.0997(4) -0.1107(4) 0.0328(3) 0.0457(9) Uani 1 1 d . . . H13 H 0.0346 -0.1150 0.0681 0.055 Uiso 1 1 calc R . . C19 C 0.6084(3) -0.3398(3) 0.1028(3) 0.0422(8) Uani 1 1 d . . . C44 C 0.6082(4) 0.4009(4) 0.4123(3) 0.0514(10) Uani 1 1 d . . . H44 H 0.5913 0.3784 0.3398 0.062 Uiso 1 1 calc R . . C41 C 0.6552(4) 0.4761(4) 0.6211(3) 0.0501(9) Uani 1 1 d . . . H41 H 0.6680 0.5016 0.6937 0.060 Uiso 1 1 calc R . . C24 C 1.0701(4) 0.5521(4) 0.8072(3) 0.0520(10) Uani 1 1 d . . . H24 H 1.0927 0.5163 0.8492 0.062 Uiso 1 1 calc R . . C212 C 1.0371(4) 0.7703(4) 0.3840(3) 0.0495(9) Uani 1 1 d . . . H212 H 1.0964 0.7398 0.3728 0.059 Uiso 1 1 calc R . . C32 C 0.5669(3) 0.1361(3) 0.3029(3) 0.0433(8) Uani 1 1 d . . . H32 H 0.6380 0.1903 0.2887 0.052 Uiso 1 1 calc R . . C210 C 0.9217(4) 0.8687(4) 0.3343(3) 0.0488(9) Uani 1 1 d . . . H210 H 0.9051 0.9052 0.2902 0.059 Uiso 1 1 calc R . . C42 C 0.5965(4) 0.3526(4) 0.5631(3) 0.0545(10) Uani 1 1 d . . . H42 H 0.5714 0.2968 0.5962 0.065 Uiso 1 1 calc R . . C25 C 1.1226(4) 0.5594(4) 0.7221(3) 0.0563(11) Uani 1 1 d . . . H25 H 1.1814 0.5285 0.7089 0.068 Uiso 1 1 calc R . . C14 C 0.1183(4) -0.0559(4) -0.0396(3) 0.0515(10) Uani 1 1 d . . . H14 H 0.0654 -0.0225 -0.0540 0.062 Uiso 1 1 calc R . . C213 C 0.7310(4) 0.9490(4) 0.3651(3) 0.0623(12) Uani 1 1 d . . . H21A H 0.6678 0.9738 0.3887 0.093 Uiso 1 1 calc R . . H21B H 0.6958 0.8866 0.2956 0.093 Uiso 1 1 calc R . . H21C H 0.8035 1.0189 0.3644 0.093 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 C112 0.055(3) 0.068(3) 0.047(2) 0.024(2) 0.0296(19) 0.033(2) C110 0.057(3) 0.069(3) 0.065(3) 0.025(2) 0.022(2) 0.045(2) C111 0.061(3) 0.082(3) 0.068(3) 0.026(3) 0.036(2) 0.049(3) Mo12 0.04107(18) 0.03557(17) 0.03093(15) 0.01798(13) 0.01527(12) 0.02099(14) Mo11 0.03674(17) 0.03486(17) 0.03346(15) 0.01847(13) 0.01434(12) 0.01988(13) C17 0.038(2) 0.047(2) 0.0336(17) 0.0148(16) 0.0186(15) 0.0234(17) N4 0.0423(17) 0.0349(16) 0.0327(14) 0.0138(12) 0.0113(12) 0.0143(13) O24 0.0447(14) 0.0432(14) 0.0345(12) 0.0224(11) 0.0207(10) 0.0245(12) O23 0.0440(14) 0.0400(14) 0.0354(12) 0.0211(11) 0.0151(10) 0.0219(11) O13 0.0407(14) 0.0454(15) 0.0426(13) 0.0245(11) 0.0168(11) 0.0254(12) N3 0.0360(16) 0.0384(16) 0.0340(14) 0.0155(13) 0.0119(12) 0.0167(13) O12 0.0522(16) 0.0460(15) 0.0415(13) 0.0251(12) 0.0229(11) 0.0245(12) O15 0.0691(19) 0.072(2) 0.0560(16) 0.0338(15) 0.0168(14) 0.0505(17) O21 0.0586(17) 0.0371(14) 0.0413(14) 0.0181(11) 0.0070(12) 0.0148(12) C22 0.0374(19) 0.0287(17) 0.0368(17) 0.0134(14) 0.0053(14) 0.0119(15) O14 0.0450(14) 0.0564(16) 0.0394(12) 0.0268(12) 0.0191(11) 0.0352(13) N12 0.0358(16) 0.0359(16) 0.0323(14) 0.0167(12) 0.0119(12) 0.0176(13) O22 0.0552(16) 0.0639(18) 0.0450(14) 0.0299(13) 0.0270(12) 0.0385(14) C33 0.0355(19) 0.0348(19) 0.0376(17) 0.0161(15) 0.0087(14) 0.0157(15) C12 0.0358(19) 0.0337(18) 0.0309(16) 0.0119(14) 0.0070(14) 0.0164(15) N21 0.055(2) 0.064(2) 0.058(2) 0.0310(18) 0.0228(16) 0.0402(18) O25 0.0672(19) 0.0666(19) 0.0468(14) 0.0377(14) 0.0236(13) 0.0423(16) C31 0.038(2) 0.042(2) 0.0397(18) 0.0147(16) 0.0177(15) 0.0201(16) O11 0.0583(17) 0.0374(15) 0.0460(14) 0.0133(12) 0.0118(12) 0.0206(13) C18 0.0323(18) 0.0335(18) 0.0381(17) 0.0092(14) 0.0097(14) 0.0169(15) C43 0.0366(19) 0.0363(19) 0.0398(18) 0.0174(16) 0.0094(15) 0.0141(15) N22 0.0382(16) 0.0360(16) 0.0374(15) 0.0179(13) 0.0139(12) 0.0180(13) C29 0.043(2) 0.0346(19) 0.0328(17) 0.0150(15) 0.0085(15) 0.0111(16) C26 0.043(2) 0.040(2) 0.047(2) 0.0198(17) 0.0214(16) 0.0212(17) N11 0.0526(19) 0.051(2) 0.0452(17) 0.0298(15) 0.0133(14) 0.0270(16) C28 0.0384(19) 0.0307(17) 0.0273(15) 0.0129(13) 0.0126(13) 0.0095(14) C11 0.0363(18) 0.0336(18) 0.0342(16) 0.0150(14) 0.0076(14) 0.0181(15) C16 0.041(2) 0.040(2) 0.0331(17) 0.0164(15) 0.0132(15) 0.0203(16) C45 0.066(3) 0.039(2) 0.0371(19) 0.0194(17) 0.0048(17) 0.0111(19) C35 0.042(2) 0.042(2) 0.047(2) 0.0185(17) 0.0208(17) 0.0154(17) C27 0.037(2) 0.046(2) 0.0356(18) 0.0177(16) 0.0159(15) 0.0148(17) C23 0.049(2) 0.036(2) 0.0406(19) 0.0196(16) 0.0078(16) 0.0160(17) C15 0.062(3) 0.056(3) 0.052(2) 0.032(2) 0.0113(19) 0.032(2) C21 0.038(2) 0.038(2) 0.0424(18) 0.0193(16) 0.0109(15) 0.0177(16) C113 0.078(3) 0.052(3) 0.073(3) 0.024(2) 0.003(2) 0.040(2) C34 0.051(2) 0.040(2) 0.043(2) 0.0138(17) 0.0235(17) 0.0194(18) C211 0.048(2) 0.078(3) 0.046(2) 0.034(2) 0.0251(18) 0.023(2) C13 0.048(2) 0.053(2) 0.047(2) 0.0175(18) 0.0142(17) 0.033(2) C19 0.044(2) 0.043(2) 0.046(2) 0.0152(17) 0.0079(16) 0.0261(18) C44 0.070(3) 0.041(2) 0.0298(18) 0.0151(16) 0.0076(17) 0.0115(19) C41 0.065(3) 0.040(2) 0.0350(19) 0.0163(17) 0.0120(17) 0.0125(19) C24 0.062(3) 0.047(2) 0.057(2) 0.026(2) 0.006(2) 0.031(2) C212 0.043(2) 0.063(3) 0.044(2) 0.0229(19) 0.0244(17) 0.022(2) C32 0.036(2) 0.045(2) 0.048(2) 0.0209(18) 0.0154(16) 0.0147(17) C210 0.054(2) 0.050(2) 0.0387(19) 0.0272(18) 0.0140(17) 0.0121(19) C42 0.075(3) 0.037(2) 0.044(2) 0.0220(18) 0.0127(19) 0.013(2) C25 0.061(3) 0.060(3) 0.067(3) 0.028(2) 0.016(2) 0.042(2) C14 0.066(3) 0.055(3) 0.052(2) 0.0230(19) 0.0074(19) 0.042(2) C213 0.081(3) 0.067(3) 0.059(3) 0.038(2) 0.013(2) 0.041(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C112 C111 1.382(5) . ? C112 C17 1.403(4) . ? C112 H112 0.9300 . ? C110 C19 1.377(5) . ? C110 C111 1.384(6) . ? C110 H110 0.9300 . ? C111 H111 0.9300 . ? Mo12 O22 1.687(2) . ? Mo12 O21 1.696(3) . ? Mo12 O24 1.944(2) . ? Mo12 O23 1.981(2) . ? Mo12 N22 2.285(3) . ? Mo12 N4 2.469(3) . ? Mo11 O11 1.694(2) . ? Mo11 O12 1.697(2) . ? Mo11 O14 1.933(2) . ? Mo11 O13 1.983(2) . ? Mo11 N12 2.287(2) . ? Mo11 N3 2.442(3) . ? C17 C18 1.415(4) . ? C17 C16 1.429(4) . ? N4 C45 1.328(4) . ? N4 C41 1.332(4) . ? O24 C28 1.345(3) . ? O23 C22 1.344(4) . ? O13 C12 1.341(3) . ? N3 C31 1.333(4) . ? N3 C35 1.346(4) . ? O15 C19 1.355(4) . ? O15 C113 1.418(4) . ? C22 C23 1.376(4) . ? C22 C21 1.394(4) . ? O14 C18 1.346(4) . ? N12 C16 1.282(4) . ? N12 C11 1.414(4) . ? C33 C34 1.382(5) . ? C33 C32 1.392(4) . ? C33 C43 1.468(5) . ? C12 C13 1.379(4) . ? C12 C11 1.391(4) . ? N21 C21 1.322(4) . ? N21 C25 1.344(5) . ? O25 C29 1.350(4) . ? O25 C213 1.420(4) . ? C31 C32 1.366(5) . ? C31 H31 0.9300 . ? C18 C19 1.401(4) . ? C43 C42 1.388(5) . ? C43 C44 1.390(5) . ? N22 C26 1.293(4) . ? N22 C21 1.420(4) . ? C29 C210 1.380(4) . ? C29 C28 1.417(4) . ? C26 C27 1.424(5) . ? C26 H26 0.9300 . ? N11 C11 1.331(4) . ? N11 C15 1.333(4) . ? C28 C27 1.416(5) . ? C16 H16 0.9300 . ? C45 C44 1.368(5) . ? C45 H45 0.9300 . ? C35 C34 1.363(5) . ? C35 H35 0.9300 . ? C27 C212 1.409(4) . ? C23 C24 1.378(5) . ? C23 H23 0.9300 . ? C15 C14 1.380(5) . ? C15 H15 0.9300 . ? C113 H11A 0.9600 . ? C113 H11B 0.9600 . ? C113 H11C 0.9600 . ? C34 H34 0.9300 . ? C211 C212 1.373(5) . ? C211 C210 1.384(5) . ? C211 H211 0.9300 . ? C13 C14 1.376(5) . ? C13 H13 0.9300 . ? C44 H44 0.9300 . ? C41 C42 1.364(5) . ? C41 H41 0.9300 . ? C24 C25 1.378(5) . ? C24 H24 0.9300 . ? C212 H212 0.9300 . ? C32 H32 0.9300 . ? C210 H210 0.9300 . ? C42 H42 0.9300 . ? C25 H25 0.9300 . ? C14 H14 0.9300 . ? C213 H21A 0.9600 . ? C213 H21B 0.9600 . ? C213 H21C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C111 C112 C17 120.6(4) . . ? C111 C112 H112 119.7 . . ? C17 C112 H112 119.7 . . ? C19 C110 C111 120.8(3) . . ? C19 C110 H110 119.6 . . ? C111 C110 H110 119.6 . . ? C112 C111 C110 120.4(3) . . ? C112 C111 H111 119.8 . . ? C110 C111 H111 119.8 . . ? O22 Mo12 O21 106.65(13) . . ? O22 Mo12 O24 101.62(10) . . ? O21 Mo12 O24 98.09(11) . . ? O22 Mo12 O23 96.68(10) . . ? O21 Mo12 O23 97.99(10) . . ? O24 Mo12 O23 150.98(9) . . ? O22 Mo12 N22 160.29(12) . . ? O21 Mo12 N22 92.24(11) . . ? O24 Mo12 N22 80.73(9) . . ? O23 Mo12 N22 74.66(9) . . ? O22 Mo12 N4 85.40(12) . . ? O21 Mo12 N4 167.79(11) . . ? O24 Mo12 N4 80.99(9) . . ? O23 Mo12 N4 78.22(9) . . ? N22 Mo12 N4 75.57(10) . . ? O11 Mo11 O12 106.16(12) . . ? O11 Mo11 O14 98.65(11) . . ? O12 Mo11 O14 102.01(10) . . ? O11 Mo11 O13 99.95(11) . . ? O12 Mo11 O13 96.78(10) . . ? O14 Mo11 O13 148.64(10) . . ? O11 Mo11 N12 91.04(11) . . ? O12 Mo11 N12 162.06(11) . . ? O14 Mo11 N12 79.86(9) . . ? O13 Mo11 N12 74.78(9) . . ? O11 Mo11 N3 169.64(10) . . ? O12 Mo11 N3 84.13(10) . . ? O14 Mo11 N3 79.99(10) . . ? O13 Mo11 N3 77.20(9) . . ? N12 Mo11 N3 78.60(9) . . ? C112 C17 C18 118.2(3) . . ? C112 C17 C16 119.2(3) . . ? C18 C17 C16 122.6(3) . . ? C45 N4 C41 115.9(3) . . ? C45 N4 Mo12 121.2(2) . . ? C41 N4 Mo12 122.6(2) . . ? C28 O24 Mo12 135.8(2) . . ? C22 O23 Mo12 121.95(18) . . ? C12 O13 Mo11 121.49(19) . . ? C31 N3 C35 115.8(3) . . ? C31 N3 Mo11 126.4(2) . . ? C35 N3 Mo11 117.5(2) . . ? C19 O15 C113 118.2(3) . . ? O23 C22 C23 123.3(3) . . ? O23 C22 C21 118.7(3) . . ? C23 C22 C21 118.0(3) . . ? C18 O14 Mo11 132.7(2) . . ? C16 N12 C11 121.3(3) . . ? C16 N12 Mo11 127.2(2) . . ? C11 N12 Mo11 111.31(19) . . ? C34 C33 C32 117.0(3) . . ? C34 C33 C43 121.3(3) . . ? C32 C33 C43 121.6(3) . . ? O13 C12 C13 123.0(3) . . ? O13 C12 C11 119.3(3) . . ? C13 C12 C11 117.7(3) . . ? C21 N21 C25 115.3(3) . . ? C29 O25 C213 118.2(3) . . ? N3 C31 C32 124.0(3) . . ? N3 C31 H31 118.0 . . ? C32 C31 H31 118.0 . . ? O14 C18 C19 117.0(3) . . ? O14 C18 C17 122.6(3) . . ? C19 C18 C17 120.4(3) . . ? C42 C43 C44 115.7(3) . . ? C42 C43 C33 123.0(3) . . ? C44 C43 C33 121.4(3) . . ? C26 N22 C21 120.4(3) . . ? C26 N22 Mo12 128.2(2) . . ? C21 N22 Mo12 111.3(2) . . ? O25 C29 C210 125.8(3) . . ? O25 C29 C28 115.1(3) . . ? C210 C29 C28 119.0(3) . . ? N22 C26 C27 124.3(3) . . ? N22 C26 H26 117.8 . . ? C27 C26 H26 117.8 . . ? C11 N11 C15 115.4(3) . . ? O24 C28 C27 122.8(3) . . ? O24 C28 C29 117.0(3) . . ? C27 C28 C29 120.1(3) . . ? N11 C11 C12 125.4(3) . . ? N11 C11 N12 121.6(3) . . ? C12 C11 N12 113.1(3) . . ? N12 C16 C17 124.1(3) . . ? N12 C16 H16 117.9 . . ? C17 C16 H16 117.9 . . ? N4 C45 C44 123.7(3) . . ? N4 C45 H45 118.2 . . ? C44 C45 H45 118.2 . . ? N3 C35 C34 124.2(3) . . ? N3 C35 H35 117.9 . . ? C34 C35 H35 117.9 . . ? C212 C27 C28 118.2(3) . . ? C212 C27 C26 118.6(3) . . ? C28 C27 C26 123.3(3) . . ? C22 C23 C24 118.0(3) . . ? C22 C23 H23 121.0 . . ? C24 C23 H23 121.0 . . ? N11 C15 C14 123.7(3) . . ? N11 C15 H15 118.1 . . ? C14 C15 H15 118.1 . . ? N21 C21 C22 125.3(3) . . ? N21 C21 N22 121.7(3) . . ? C22 C21 N22 113.0(3) . . ? O15 C113 H11A 109.5 . . ? O15 C113 H11B 109.5 . . ? H11A C113 H11B 109.5 . . ? O15 C113 H11C 109.5 . . ? H11A C113 H11C 109.5 . . ? H11B C113 H11C 109.5 . . ? C35 C34 C33 119.4(3) . . ? C35 C34 H34 120.3 . . ? C33 C34 H34 120.3 . . ? C212 C211 C210 120.2(3) . . ? C212 C211 H211 119.9 . . ? C210 C211 H211 119.9 . . ? C14 C13 C12 118.0(3) . . ? C14 C13 H13 121.0 . . ? C12 C13 H13 121.0 . . ? O15 C19 C110 125.3(3) . . ? O15 C19 C18 115.1(3) . . ? C110 C19 C18 119.6(3) . . ? C45 C44 C43 120.3(3) . . ? C45 C44 H44 119.8 . . ? C43 C44 H44 119.8 . . ? N4 C41 C42 124.4(3) . . ? N4 C41 H41 117.8 . . ? C42 C41 H41 117.8 . . ? C25 C24 C23 119.5(3) . . ? C25 C24 H24 120.3 . . ? C23 C24 H24 120.3 . . ? C211 C212 C27 121.1(4) . . ? C211 C212 H212 119.4 . . ? C27 C212 H212 119.4 . . ? C31 C32 C33 119.5(3) . . ? C31 C32 H32 120.2 . . ? C33 C32 H32 120.2 . . ? C29 C210 C211 121.3(3) . . ? C29 C210 H210 119.3 . . ? C211 C210 H210 119.3 . . ? C41 C42 C43 119.8(3) . . ? C41 C42 H42 120.1 . . ? C43 C42 H42 120.1 . . ? N21 C25 C24 123.9(3) . . ? N21 C25 H25 118.1 . . ? C24 C25 H25 118.1 . . ? C13 C14 C15 119.8(3) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? O25 C213 H21A 109.5 . . ? O25 C213 H21B 109.5 . . ? H21A C213 H21B 109.5 . . ? O25 C213 H21C 109.5 . . ? H21A C213 H21C 109.5 . . ? H21B C213 H21C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 29.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.957 _refine_diff_density_min -0.538 _refine_diff_density_rms 0.113 #===END data_I(Bp)_x_CH2Cl2 _database_code_depnum_ccdc_archive 'CCDC 799781' #TrackingRef 'Uzarevic_et_al_cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; (4,4'-bipyridine)bis(cis-dioxo(N-3-methoxysalicylidene -2-amino-3-hydroxypyridine))dimolybdenum(VI) dichlormethane solvate ; _chemical_name_common ; (4,4'-bipyridine)bis(cis-dioxo(N-3-methoxysalicylidene -2- amino-3-hydroxypyridine))dimolybdenum(VI) dichlormethane solvate ; _chemical_melting_point ? _chemical_formula_moiety 'C36 H28 Mo2 N6 O10, 2(C H2 Cl2)' _chemical_formula_sum 'C38 H32 Cl4 Mo2 N6 O10' _chemical_formula_weight 1066.38 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.3420(12) _cell_length_b 13.4804(9) _cell_length_c 17.3437(16) _cell_angle_alpha 90.00 _cell_angle_beta 131.638(6) _cell_angle_gamma 90.00 _cell_volume 2156.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 4239 _cell_measurement_theta_min 4.3507 _cell_measurement_theta_max 29.0317 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.642 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1068 _exptl_absorpt_coefficient_mu 0.891 _exptl_absorpt_correction_T_min 0.86339 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET) (compiled Sep 15 2009,11:49:04) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.3426 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8185 _diffrn_reflns_av_R_equivalents 0.0237 _diffrn_reflns_av_sigmaI/netI 0.0474 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 4.36 _diffrn_reflns_theta_max 26.49 _reflns_number_total 4446 _reflns_number_gt 3222 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) ; _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is 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^)+(0.0552P)^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 4446 _refine_ls_number_parameters 272 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0522 _refine_ls_R_factor_gt 0.0348 _refine_ls_wR_factor_ref 0.0933 _refine_ls_wR_factor_gt 0.0896 _refine_ls_goodness_of_fit_ref 0.940 _refine_ls_restrained_S_all 0.940 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.38194(3) 0.195206(18) 0.64203(2) 0.03290(10) Uani 1 1 d . . . O1 O 0.3611(3) 0.23677(17) 0.54011(18) 0.0499(6) Uani 1 1 d . . . O2 O 0.2593(2) 0.25729(16) 0.63886(18) 0.0458(6) Uani 1 1 d . . . O3 O 0.5503(2) 0.27571(15) 0.75296(17) 0.0415(5) Uani 1 1 d . . . O4 O 0.2891(2) 0.06767(15) 0.58369(16) 0.0367(5) Uani 1 1 d . . . O5 O 0.0599(3) -0.02263(18) 0.4285(2) 0.0575(7) Uani 1 1 d . . . N1 N 0.8352(3) 0.1223(2) 0.8128(2) 0.0582(8) Uani 1 1 d . . . N2 N 0.5785(3) 0.10403(18) 0.69901(19) 0.0359(6) Uani 1 1 d . . . N3 N 0.4407(3) 0.11209(17) 0.78930(19) 0.0333(6) Uani 1 1 d . . . C1 C 0.7076(4) 0.1565(2) 0.7729(3) 0.0416(8) Uani 1 1 d . . . C2 C 0.6847(4) 0.2502(2) 0.7956(2) 0.0416(8) Uani 1 1 d . . . C3 C 0.8028(4) 0.3110(3) 0.8607(3) 0.0561(10) Uani 1 1 d . . . H3 H 0.7930 0.3739 0.8775 0.067 Uiso 1 1 calc R . . C4 C 0.9357(5) 0.2766(3) 0.9003(3) 0.0712(13) Uani 1 1 d . . . H4 H 1.0172 0.3168 0.9434 0.085 Uiso 1 1 calc R . . C5 C 0.9482(4) 0.1831(3) 0.8762(4) 0.0737(13) Uani 1 1 d . . . H5 H 1.0398 0.1607 0.9054 0.088 Uiso 1 1 calc R . . C6 C 0.5762(3) 0.0226(2) 0.6584(2) 0.0380(7) Uani 1 1 d . . . H6 H 0.6643 -0.0034 0.6836 0.046 Uiso 1 1 calc R . . C7 C 0.4461(4) -0.0300(2) 0.5769(2) 0.0361(7) Uani 1 1 d . . . C8 C 0.3095(3) -0.0036(2) 0.5408(2) 0.0327(7) Uani 1 1 d . . . C9 C 0.1864(4) -0.0554(2) 0.4572(3) 0.0429(8) Uani 1 1 d . . . C10 C 0.2011(4) -0.1332(2) 0.4139(3) 0.0493(9) Uani 1 1 d . . . H10 H 0.1195 -0.1681 0.3593 0.059 Uiso 1 1 calc R . . C11 C 0.3368(4) -0.1604(3) 0.4508(3) 0.0513(9) Uani 1 1 d . . . H11 H 0.3453 -0.2132 0.4206 0.062 Uiso 1 1 calc R . . C12 C 0.4568(4) -0.1107(2) 0.5304(3) 0.0435(8) Uani 1 1 d . . . H12 H 0.5472 -0.1299 0.5547 0.052 Uiso 1 1 calc R . . C13 C -0.0702(4) -0.0705(4) 0.3440(4) 0.0942(18) Uani 1 1 d . . . H13A H -0.1506 -0.0421 0.3332 0.141 Uiso 1 1 calc R . . H13B H -0.0638 -0.1400 0.3585 0.141 Uiso 1 1 calc R . . H13C H -0.0840 -0.0617 0.2830 0.141 Uiso 1 1 calc R . . C31 C 0.4808(4) 0.0173(2) 0.8151(3) 0.0451(8) Uani 1 1 d . . . H31 H 0.4936 -0.0198 0.7765 0.054 Uiso 1 1 calc R . . C32 C 0.5038(4) -0.0280(2) 0.8952(3) 0.0469(9) Uani 1 1 d . . . H32 H 0.5314 -0.0943 0.9095 0.056 Uiso 1 1 calc R . . C33 C 0.4868(3) 0.0231(2) 0.9553(2) 0.0326(7) Uani 1 1 d . . . C34 C 0.4430(4) 0.1202(2) 0.9274(3) 0.0490(9) Uani 1 1 d . . . H34 H 0.4272 0.1583 0.9638 0.059 Uiso 1 1 calc R . . C35 C 0.4224(4) 0.1610(2) 0.8462(3) 0.0478(9) Uani 1 1 d . . . H35 H 0.3939 0.2270 0.8300 0.057 Uiso 1 1 calc R . . Cl1 Cl -0.1516(2) 0.41387(19) 0.5591(2) 0.2238(15) Uani 1 1 d . . . Cl2 Cl 0.1009(2) 0.34633(14) 0.76392(16) 0.1352(7) Uani 1 1 d . . . C1S C 0.0278(6) 0.3887(4) 0.6424(5) 0.119(2) Uani 1 1 d . . . H1 H 0.0791 0.4484 0.6516 0.142 Uiso 1 1 calc R . . H2 H 0.0456 0.3390 0.6115 0.142 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 0.03690(16) 0.03068(15) 0.03499(15) 0.00258(12) 0.02551(13) 0.00013(12) O1 0.0599(16) 0.0480(12) 0.0471(14) 0.0087(11) 0.0377(13) -0.0004(12) O2 0.0493(14) 0.0414(12) 0.0501(14) 0.0044(11) 0.0344(12) 0.0083(11) O3 0.0428(13) 0.0365(11) 0.0465(13) -0.0063(10) 0.0302(12) -0.0067(10) O4 0.0373(12) 0.0411(12) 0.0408(12) -0.0062(9) 0.0297(11) -0.0062(10) O5 0.0400(14) 0.0552(14) 0.0686(17) -0.0170(13) 0.0325(14) -0.0098(12) N1 0.0385(17) 0.0651(19) 0.0525(19) -0.0085(16) 0.0224(16) 0.0008(16) N2 0.0389(15) 0.0368(14) 0.0349(14) -0.0002(11) 0.0258(13) -0.0037(12) N3 0.0396(14) 0.0301(12) 0.0364(14) -0.0012(10) 0.0278(13) -0.0026(11) C1 0.0359(18) 0.0461(17) 0.0378(18) -0.0014(15) 0.0224(16) -0.0023(15) C2 0.042(2) 0.0429(18) 0.0353(18) -0.0022(14) 0.0239(17) -0.0046(16) C3 0.050(2) 0.058(2) 0.049(2) -0.0129(18) 0.0279(19) -0.0098(19) C4 0.042(2) 0.076(3) 0.066(3) -0.018(2) 0.023(2) -0.017(2) C5 0.038(2) 0.084(3) 0.070(3) -0.013(2) 0.024(2) -0.005(2) C6 0.0386(18) 0.0390(17) 0.0409(18) 0.0041(14) 0.0283(16) 0.0034(14) C7 0.0464(19) 0.0322(15) 0.0397(17) 0.0003(13) 0.0328(16) -0.0017(14) C8 0.0427(18) 0.0276(14) 0.0336(16) 0.0007(12) 0.0278(15) -0.0045(13) C9 0.046(2) 0.0410(18) 0.045(2) -0.0014(14) 0.0318(17) -0.0084(15) C10 0.053(2) 0.046(2) 0.046(2) -0.0119(16) 0.0311(19) -0.0114(18) C11 0.070(3) 0.0390(17) 0.057(2) -0.0081(16) 0.048(2) -0.0039(18) C12 0.055(2) 0.0362(17) 0.052(2) 0.0021(15) 0.0408(19) 0.0035(16) C13 0.049(3) 0.085(3) 0.116(4) -0.041(3) 0.041(3) -0.020(2) C31 0.075(3) 0.0335(17) 0.052(2) 0.0036(14) 0.053(2) 0.0092(16) C32 0.078(3) 0.0326(16) 0.052(2) 0.0091(15) 0.052(2) 0.0128(17) C33 0.0401(17) 0.0316(15) 0.0314(16) -0.0034(12) 0.0260(15) -0.0028(13) C34 0.085(3) 0.0350(17) 0.047(2) -0.0011(14) 0.052(2) 0.0073(17) C35 0.078(3) 0.0288(15) 0.046(2) 0.0024(14) 0.046(2) 0.0099(17) Cl1 0.0750(12) 0.184(2) 0.269(3) -0.001(2) 0.0545(16) 0.0006(14) Cl2 0.1324(16) 0.1262(12) 0.1513(17) -0.0397(12) 0.0960(14) -0.0401(12) C1S 0.090(4) 0.090(4) 0.150(6) -0.002(4) 0.069(4) -0.002(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 O2 1.698(2) . ? Mo1 O1 1.703(2) . ? Mo1 O4 1.937(2) . ? Mo1 O3 1.971(2) . ? Mo1 N2 2.277(3) . ? Mo1 N3 2.417(2) . ? O3 C2 1.337(4) . ? O4 C8 1.338(3) . ? O5 C9 1.359(4) . ? O5 C13 1.420(5) . ? N1 C1 1.313(4) . ? N1 C5 1.338(5) . ? N2 C6 1.294(4) . ? N2 C1 1.403(4) . ? N3 C35 1.325(4) . ? N3 C31 1.336(4) . ? C1 C2 1.407(5) . ? C2 C3 1.374(5) . ? C3 C4 1.370(6) . ? C3 H3 0.9300 . ? C4 C5 1.369(6) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C7 1.436(4) . ? C6 H6 0.9300 . ? C7 C8 1.399(4) . ? C7 C12 1.412(4) . ? C8 C9 1.404(4) . ? C9 C10 1.372(5) . ? C10 C11 1.386(5) . ? C10 H10 0.9300 . ? C11 C12 1.353(5) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C31 C32 1.363(4) . ? C31 H31 0.9300 . ? C32 C33 1.377(4) . ? C32 H32 0.9300 . ? C33 C34 1.376(4) . ? C33 C33 1.491(5) 3_657 ? C34 C35 1.369(5) . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? Cl1 C1S 1.689(6) . ? Cl2 C1S 1.748(7) . ? C1S H1 0.9700 . ? C1S H2 0.9700 . ? 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 106.71(11) . . ? O2 Mo1 O4 102.44(10) . . ? O1 Mo1 O4 96.93(10) . . ? O2 Mo1 O3 95.68(10) . . ? O1 Mo1 O3 99.58(11) . . ? O4 Mo1 O3 150.78(9) . . ? O2 Mo1 N2 161.72(10) . . ? O1 Mo1 N2 90.61(10) . . ? O4 Mo1 N2 80.65(9) . . ? O3 Mo1 N2 75.26(9) . . ? O2 Mo1 N3 84.15(10) . . ? O1 Mo1 N3 168.96(10) . . ? O4 Mo1 N3 78.39(8) . . ? O3 Mo1 N3 80.91(9) . . ? N2 Mo1 N3 78.81(9) . . ? C2 O3 Mo1 120.94(19) . . ? C8 O4 Mo1 131.56(18) . . ? C9 O5 C13 117.8(3) . . ? C1 N1 C5 116.6(3) . . ? C6 N2 C1 121.7(3) . . ? C6 N2 Mo1 126.1(2) . . ? C1 N2 Mo1 111.1(2) . . ? C35 N3 C31 115.7(3) . . ? C35 N3 Mo1 118.47(19) . . ? C31 N3 Mo1 125.6(2) . . ? N1 C1 N2 122.7(3) . . ? N1 C1 C2 124.2(3) . . ? N2 C1 C2 113.0(3) . . ? O3 C2 C3 123.4(3) . . ? O3 C2 C1 118.9(3) . . ? C3 C2 C1 117.7(3) . . ? C4 C3 C2 118.3(4) . . ? C4 C3 H3 120.9 . . ? C2 C3 H3 120.9 . . ? C5 C4 C3 119.9(4) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? N1 C5 C4 123.2(4) . . ? N1 C5 H5 118.4 . . ? C4 C5 H5 118.4 . . ? N2 C6 C7 124.1(3) . . ? N2 C6 H6 118.0 . . ? C7 C6 H6 118.0 . . ? C8 C7 C12 118.8(3) . . ? C8 C7 C6 122.8(3) . . ? C12 C7 C6 118.4(3) . . ? O4 C8 C7 123.4(3) . . ? O4 C8 C9 117.1(3) . . ? C7 C8 C9 119.5(3) . . ? O5 C9 C10 125.9(3) . . ? O5 C9 C8 114.1(3) . . ? C10 C9 C8 119.9(3) . . ? C9 C10 C11 120.5(3) . . ? C9 C10 H10 119.7 . . ? C11 C10 H10 119.7 . . ? C12 C11 C10 120.6(3) . . ? C12 C11 H11 119.7 . . ? C10 C11 H11 119.7 . . ? C11 C12 C7 120.6(3) . . ? C11 C12 H12 119.7 . . ? C7 C12 H12 119.7 . . ? O5 C13 H13A 109.5 . . ? O5 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? O5 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N3 C31 C32 123.4(3) . . ? N3 C31 H31 118.3 . . ? C32 C31 H31 118.3 . . ? C31 C32 C33 120.9(3) . . ? C31 C32 H32 119.5 . . ? C33 C32 H32 119.5 . . ? C34 C33 C32 115.6(3) . . ? C34 C33 C33 121.8(3) . 3_657 ? C32 C33 C33 122.7(3) . 3_657 ? C35 C34 C33 120.3(3) . . ? C35 C34 H34 119.8 . . ? C33 C34 H34 119.8 . . ? N3 C35 C34 124.0(3) . . ? N3 C35 H35 118.0 . . ? C34 C35 H35 118.0 . . ? Cl1 C1S Cl2 115.5(4) . . ? Cl1 C1S H1 108.4 . . ? Cl2 C1S H1 108.4 . . ? Cl1 C1S H2 108.4 . . ? Cl2 C1S H2 108.4 . . ? H1 C1S H2 107.5 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.49 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.633 _refine_diff_density_min -0.684 _refine_diff_density_rms 0.071