# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Konstantin V. Domasevitch' _publ_contact_author_email DK@MAIL.UNIV.KIEV.UA _publ_section_title ; Metal oxide-organic frameworks (MOOFs), a new series of coordination hybrids constructed from molybdenum(VI) oxide and bitopic 1,2,4-triazole linkers ; loop_ _publ_author_name 'Konstantin V. Domasevitch' 'Ekaterina D. Butova' 'Andrey A. Fokin' 'Harald Krautscheid' 'Daniel Lassig' ; J.Lincke ; 'Andrey B. Lysenko' 'P Schreiner' 'Ganna A Senchyk' # Attachment 'Cif_data.cif' data_(1) _database_code_depnum_ccdc_archive 'CCDC 752797' #TrackingRef 'Cif_data.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Molybdenum(VI) oxide 2:1 complex with 1,2-bis(1,2,4-triazol-4-yl)ethane ; _chemical_name_common ;Molybdenum(VI) oxide 2:1 complex with 1,2-bis(1,2,4-triazol-4- yl)ethane ; _chemical_melting_point ? _chemical_formula_moiety 'C12 H16 Mo4 N12 O12' _chemical_formula_sum 'C12 H16 Mo4 N12 O12' _chemical_formula_weight 904.13 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c n' _space_group_name_Hall '-P 2n 2ab' _symmetry_Int_Tables_number 60 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y, z-1/2' _cell_length_a 15.2779(16) _cell_length_b 12.6491(13) _cell_length_c 12.1712(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2352.1(4) _cell_formula_units_Z 4 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 2.09 _cell_measurement_theta_max 26.28 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_diffrn 2.553 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1744 _exptl_absorpt_coefficient_mu 2.172 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.7508 _exptl_absorpt_correction_T_max 0.8807 _exptl_absorpt_process_details 'X-RED (Stoe & Cie, 2001) and X-SHAPE (Stoe & Cie, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe Imaging plate diffraction system' _diffrn_measurement_method '\f oscillation scans' _diffrn_standards_decay_% 0 _diffrn_reflns_number 10718 _diffrn_reflns_av_R_equivalents 0.0710 _diffrn_reflns_av_sigmaI/netI 0.1020 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 26.28 _reflns_number_total 2342 _reflns_number_gt 1279 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS Software (Stoe & Cie, 2000)' _computing_cell_refinement 'IPDS Software (Stoe & Cie, 2000)' _computing_data_reduction 'IPDS Software (Stoe & Cie, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e (Brandenburg, 1999)' _computing_publication_material 'WinGX 1.70.01 (Farrugia, 1999)' #------------------------------- Refinement data-----------------------# _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^)+(0.0678P)^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_number_reflns 2342 _refine_ls_number_parameters 190 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0805 _refine_ls_R_factor_gt 0.0543 _refine_ls_wR_factor_ref 0.1369 _refine_ls_wR_factor_gt 0.1194 _refine_ls_goodness_of_fit_ref 0.998 _refine_ls_restrained_S_all 0.986 _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 0.75313(8) 0.62643(6) 0.40570(8) 0.0109(4) Uani 1 1 d . A -1 Mo2 Mo 0.65433(7) 0.74699(8) 0.65596(8) 0.0127(4) Uani 1 1 d . A -1 O1 O 0.6847(5) 0.6635(5) 0.5293(6) 0.017(2) Uani 1 1 d . A -1 O2 O 0.8186(6) 0.6651(5) 0.2772(6) 0.017(2) Uani 1 1 d . A -1 O3 O 0.8322(6) 0.5497(6) 0.4657(6) 0.024(2) Uani 1 1 d . A -1 O4 O 0.6822(6) 0.5399(6) 0.3483(6) 0.025(2) Uani 1 1 d . A -1 O5 O 0.5791(6) 0.8295(6) 0.5954(6) 0.028(2) Uani 1 1 d . A -1 O6 O 0.5937(6) 0.6521(6) 0.7177(6) 0.027(2) Uani 1 1 d . A -1 N1 N 0.8223(7) 0.7789(8) 0.4824(10) 0.0201(13) Uani 1 1 d U A -1 N2 N 0.7849(7) 0.8338(7) 0.5700(8) 0.0199(13) Uani 1 1 d U A -1 N3 N 0.9130(7) 0.9020(7) 0.5353(8) 0.0202(13) Uani 1 1 d U A -1 N4 N 0.6779(7) 0.7720(7) 0.3263(7) 0.0148(12) Uani 1 1 d U A -1 N5 N 0.7127(7) 0.8282(7) 0.2345(8) 0.0147(12) Uani 1 1 d U A -1 N6 N 0.5972(7) 0.9097(7) 0.2837(7) 0.0146(12) Uani 1 1 d U A -1 C1 C 0.8973(9) 0.8235(9) 0.4604(10) 0.0200(14) Uani 1 1 d U A -1 H1 H 0.9347 0.8046 0.4022 0.024 Uiso 1 1 calc R A -1 C2 C 0.8386(9) 0.9063(9) 0.5971(10) 0.0200(13) Uani 1 1 d U A -1 H2 H 0.8283 0.9564 0.6526 0.024 Uiso 1 1 calc R A -1 C3 C 0.9952(9) 0.9683(9) 0.5482(9) 0.0220(17) Uani 1 1 d U A -1 H3A H 1.0467 0.9214 0.5579 0.026 Uiso 1 1 d . B -1 H3B H 0.9925 1.0105 0.6151 0.026 Uiso 1 1 d . C -1 C4 C 0.6077(9) 0.8253(8) 0.3549(9) 0.0147(12) Uani 1 1 d U A -1 H4 H 0.5706 0.8088 0.4140 0.018 Uiso 1 1 calc R A -1 C5 C 0.6652(9) 0.9074(8) 0.2113(10) 0.0147(12) Uani 1 1 d U A -1 H5 H 0.6753 0.9560 0.1542 0.018 Uiso 1 1 calc R A -1 C6 C 0.5304(9) 0.9950(8) 0.2959(9) 0.0153(15) Uani 1 1 d U A -1 H6A H 0.5594 1.0627 0.3043 0.018 Uiso 1 1 d . D -1 H6B H 0.4985 0.9832 0.3651 0.018 Uiso 1 1 d . E -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0135(8) 0.0107(6) 0.0085(6) 0.0005(5) 0.0025(5) 0.0010(5) Mo2 0.0091(7) 0.0193(6) 0.0098(6) -0.0036(5) -0.0001(6) 0.0018(5) O1 0.014(6) 0.015(4) 0.023(5) -0.006(4) 0.002(4) -0.004(4) O2 0.024(6) 0.015(4) 0.012(5) -0.003(4) 0.003(4) 0.007(4) O3 0.030(7) 0.031(5) 0.012(5) 0.001(4) -0.001(4) 0.012(4) O4 0.014(6) 0.035(5) 0.024(5) -0.011(4) 0.005(5) -0.015(4) O5 0.028(7) 0.043(5) 0.012(5) -0.012(4) -0.011(4) 0.022(5) O6 0.037(7) 0.031(5) 0.012(5) -0.011(4) 0.012(4) -0.010(4) N1 0.013(4) 0.023(3) 0.024(3) -0.011(2) 0.000(3) -0.001(2) N2 0.013(4) 0.023(3) 0.024(3) -0.010(2) 0.000(3) -0.001(2) N3 0.014(4) 0.023(3) 0.024(3) -0.011(2) 0.000(3) -0.001(2) N4 0.011(3) 0.019(2) 0.015(3) 0.000(2) 0.004(2) 0.004(2) N5 0.011(3) 0.018(2) 0.015(3) 0.000(2) 0.004(2) 0.004(2) N6 0.011(3) 0.018(2) 0.015(3) 0.001(2) 0.004(2) 0.004(2) C1 0.014(4) 0.023(3) 0.024(3) -0.011(2) 0.000(3) -0.001(2) C2 0.014(4) 0.023(3) 0.024(3) -0.010(2) 0.000(3) -0.001(2) C3 0.015(4) 0.025(3) 0.026(3) -0.010(3) 0.000(3) -0.001(3) C4 0.011(3) 0.019(2) 0.015(3) 0.000(2) 0.004(2) 0.004(2) C5 0.011(3) 0.018(2) 0.015(3) 0.001(2) 0.004(2) 0.004(2) C6 0.010(4) 0.019(3) 0.017(3) 0.002(3) 0.004(3) 0.004(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 O4 1.691(8) . ? Mo1 O3 1.713(8) . ? Mo1 O1 1.891(8) . ? Mo1 O2 1.921(8) . ? Mo1 N4 2.376(9) . ? Mo1 N1 2.389(9) . ? Mo2 O6 1.692(8) . ? Mo2 O5 1.718(8) . ? Mo2 O1 1.925(7) . ? Mo2 N2 2.506(11) . ? N1 C1 1.305(15) . ? N1 N2 1.395(13) . ? N2 C2 1.274(15) . ? N3 C2 1.364(16) . ? N3 C1 1.370(14) . ? N3 C3 1.518(16) . ? N4 C4 1.314(15) . ? N4 N5 1.427(12) . ? N5 C5 1.268(14) . ? N6 C5 1.363(15) . ? N6 C4 1.385(14) . ? N6 C6 1.492(15) . ? C1 H1 0.9400 . ? C2 H2 0.9400 . ? C3 H3A 0.9923 . ? C3 H3B 0.9742 . ? C4 H4 0.9400 . ? C5 H5 0.9400 . ? C6 H6A 0.9690 . ? C6 H6B 0.9848 . ? 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 O4 Mo1 O3 105.1(4) . . ? O4 Mo1 O1 97.8(4) . . ? O3 Mo1 O1 101.0(3) . . ? O4 Mo1 O2 99.3(3) . . ? O3 Mo1 O2 97.2(4) . . ? O1 Mo1 O2 150.8(3) . . ? O4 Mo1 N4 91.3(4) . . ? O3 Mo1 N4 162.5(4) . . ? O1 Mo1 N4 82.2(3) . . ? O2 Mo1 N4 73.9(3) . . ? O4 Mo1 N1 165.3(4) . . ? O3 Mo1 N1 88.8(4) . . ? O1 Mo1 N1 74.5(3) . . ? O2 Mo1 N1 83.2(4) . . ? N4 Mo1 N1 75.4(4) . . ? O6 Mo2 O5 104.8(5) . . ? O6 Mo2 O1 95.7(3) . . ? O5 Mo2 O1 98.7(3) . . ? O6 Mo2 N2 158.7(4) . . ? O5 Mo2 N2 95.0(4) . . ? O1 Mo2 N2 73.4(3) . . ? Mo1 O1 Mo2 155.0(4) . . ? C1 N1 N2 107.6(10) . . ? C1 N1 Mo1 131.1(8) . . ? N2 N1 Mo1 121.3(8) . . ? C2 N2 N1 106.9(11) . . ? C2 N2 Mo2 136.1(9) . . ? N1 N2 Mo2 115.3(7) . . ? C2 N3 C1 104.5(10) . . ? C2 N3 C3 127.6(9) . . ? C1 N3 C3 127.9(10) . . ? C4 N4 N5 104.8(9) . . ? C4 N4 Mo1 133.3(7) . . ? N5 N4 Mo1 121.6(7) . . ? C5 N5 N4 110.8(10) . . ? C5 N6 C4 107.4(10) . . ? C5 N6 C6 127.0(9) . . ? C4 N6 C6 125.1(9) . . ? N1 C1 N3 109.3(11) . . ? N1 C1 H1 125.4 . . ? N3 C1 H1 125.4 . . ? N2 C2 N3 111.5(11) . . ? N2 C2 H2 124.3 . . ? N3 C2 H2 124.3 . . ? N3 C3 H3A 109.8 . . ? N3 C3 H3B 110.8 . . ? H3A C3 H3B 105.2 . . ? N4 C4 N6 109.0(10) . . ? N4 C4 H4 125.5 . . ? N6 C4 H4 125.5 . . ? N5 C5 N6 108.0(10) . . ? N5 C5 H5 126.0 . . ? N6 C5 H5 126.0 . . ? N6 C6 H6A 109.7 . . ? N6 C6 H6B 108.3 . . ? H6A C6 H6B 105.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 Mo1 O1 Mo2 -167.5(11) . . . . ? O3 Mo1 O1 Mo2 85.3(11) . . . . ? O2 Mo1 O1 Mo2 -42.1(15) . . . . ? N4 Mo1 O1 Mo2 -77.2(11) . . . . ? N1 Mo1 O1 Mo2 -0.3(10) . . . . ? O6 Mo2 O1 Mo1 -158.2(11) . . . . ? O5 Mo2 O1 Mo1 95.8(11) . . . . ? N2 Mo2 O1 Mo1 3.2(10) . . . . ? O4 Mo1 N1 C1 -129.5(15) . . . . ? O3 Mo1 N1 C1 68.7(14) . . . . ? O1 Mo1 N1 C1 170.5(14) . . . . ? O2 Mo1 N1 C1 -28.6(13) . . . . ? N4 Mo1 N1 C1 -103.7(14) . . . . ? O4 Mo1 N1 N2 54(2) . . . . ? O3 Mo1 N1 N2 -107.4(10) . . . . ? O1 Mo1 N1 N2 -5.6(9) . . . . ? O2 Mo1 N1 N2 155.2(10) . . . . ? N4 Mo1 N1 N2 80.1(10) . . . . ? C1 N1 N2 C2 -0.9(14) . . . . ? Mo1 N1 N2 C2 176.0(9) . . . . ? C1 N1 N2 Mo2 -168.6(9) . . . . ? Mo1 N1 N2 Mo2 8.3(12) . . . . ? O6 Mo2 N2 C2 -107.7(14) . . . . ? O5 Mo2 N2 C2 93.5(12) . . . . ? O1 Mo2 N2 C2 -168.9(13) . . . . ? O6 Mo2 N2 N1 55.2(13) . . . . ? O5 Mo2 N2 N1 -103.6(8) . . . . ? O1 Mo2 N2 N1 -6.0(8) . . . . ? O4 Mo1 N4 C4 82.3(11) . . . . ? O3 Mo1 N4 C4 -117.3(14) . . . . ? O1 Mo1 N4 C4 -15.4(10) . . . . ? O2 Mo1 N4 C4 -178.4(11) . . . . ? N1 Mo1 N4 C4 -91.4(11) . . . . ? O4 Mo1 N4 N5 -105.3(8) . . . . ? O3 Mo1 N4 N5 55.1(14) . . . . ? O1 Mo1 N4 N5 157.0(8) . . . . ? O2 Mo1 N4 N5 -6.0(7) . . . . ? N1 Mo1 N4 N5 81.0(8) . . . . ? C4 N4 N5 C5 -0.7(13) . . . . ? Mo1 N4 N5 C5 -174.9(8) . . . . ? N2 N1 C1 N3 3.7(15) . . . . ? Mo1 N1 C1 N3 -172.8(9) . . . . ? C2 N3 C1 N1 -4.9(14) . . . . ? C3 N3 C1 N1 174.1(11) . . . . ? N1 N2 C2 N3 -2.3(14) . . . . ? Mo2 N2 C2 N3 161.6(9) . . . . ? C1 N3 C2 N2 4.4(14) . . . . ? C3 N3 C2 N2 -174.6(10) . . . . ? N5 N4 C4 N6 1.2(12) . . . . ? Mo1 N4 C4 N6 174.5(7) . . . . ? C5 N6 C4 N4 -1.3(13) . . . . ? C6 N6 C4 N4 -173.4(10) . . . . ? N4 N5 C5 N6 -0.1(14) . . . . ? C4 N6 C5 N5 0.8(13) . . . . ? C6 N6 C5 N5 172.7(11) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 26.28 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.142 _refine_diff_density_min -1.108 _refine_diff_density_rms 0.223 #============================================================================== data_(2) _database_code_depnum_ccdc_archive 'CCDC 752798' #TrackingRef 'Cif_data.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Molybdenum(VI) oxide 2:1 complex with 1,3-bis(1,2,4-triazol-4-yl)propane ; _chemical_name_common ;Molybdenum(VI) oxide 2:1 complex with 1,3-bis(1,2,4-triazol-4- yl)propane ; _chemical_melting_point ? _chemical_formula_moiety 'C7 H10 Mo2 N6 O6' _chemical_formula_sum 'C7 H10 Mo2 N6 O6' _chemical_formula_weight 466.09 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _space_group_name_Hall 'P 2ac 2ab' _symmetry_Int_Tables_number 19 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 9.4050(4) _cell_length_b 11.7467(5) _cell_length_c 11.9594(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1321.25(10) _cell_formula_units_Z 4 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 26.67 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.22 _exptl_crystal_density_diffrn 2.343 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 904 _exptl_absorpt_coefficient_mu 1.937 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.6228 _exptl_absorpt_correction_T_max 0.6752 _exptl_absorpt_process_details 'X-RED (Stoe & Cie, 2001) and X-SHAPE (Stoe & Cie, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe Imaging plate diffraction system' _diffrn_measurement_method '\f oscillation scans' _diffrn_standards_decay_% 0 _diffrn_reflns_number 9294 _diffrn_reflns_av_R_equivalents 0.0354 _diffrn_reflns_av_sigmaI/netI 0.0428 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.43 _diffrn_reflns_theta_max 26.67 _reflns_number_total 2585 _reflns_number_gt 2366 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS Software (Stoe & Cie, 2000)' _computing_cell_refinement 'IPDS Software (Stoe & Cie, 2000)' _computing_data_reduction 'IPDS Software (Stoe & Cie, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e (Brandenburg, 1999)' _computing_publication_material 'WinGX 1.70.01 (Farrugia, 1999)' #------------------------------- Refinement data-----------------------# _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^)+(0.0224P)^2^+0.2557P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.04(6) _refine_ls_number_reflns 2585 _refine_ls_number_parameters 190 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0351 _refine_ls_R_factor_gt 0.0293 _refine_ls_wR_factor_ref 0.0541 _refine_ls_wR_factor_gt 0.0527 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_restrained_S_all 1.088 _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 0.37015(4) 1.07414(3) -0.13496(3) 0.01563(10) Uani 1 1 d . . . Mo2 Mo 0.37082(4) 1.09371(3) 0.16816(3) 0.01549(11) Uani 1 1 d . . . O1 O 0.4197(3) 1.1188(2) 0.0147(2) 0.0175(7) Uani 1 1 d . . . O2 O 0.5317(3) 1.0247(3) -0.1774(2) 0.0301(9) Uani 1 1 d . . . O3 O 0.3555(4) 1.2043(2) -0.1971(2) 0.0285(8) Uani 1 1 d . . . O4 O 0.2510(3) 1.0132(3) 0.2705(2) 0.0180(7) Uani 1 1 d . . . O5 O 0.5331(3) 1.0575(3) 0.2204(2) 0.0273(8) Uani 1 1 d . . . O6 O 0.3456(4) 1.2302(3) 0.2141(2) 0.0290(9) Uani 1 1 d . . . N1 N 0.3361(4) 0.9040(3) -0.0295(3) 0.0233(9) Uani 1 1 d . . . N2 N 0.3590(4) 0.9092(3) 0.0838(3) 0.0216(8) Uani 1 1 d . . . N3 N 0.3179(4) 0.7332(3) 0.0397(3) 0.0251(10) Uani 1 1 d . . . N4 N 0.6512(4) 0.3952(3) -0.0722(3) 0.0177(8) Uani 1 1 d . . . N5 N 0.6486(4) 0.3943(3) 0.0427(3) 0.0182(8) Uani 1 1 d . . . N6 N 0.4298(3) 0.3946(3) -0.0181(3) 0.0173(8) Uani 1 1 d . . . C1 C 0.3112(6) 0.7974(4) -0.0533(4) 0.0324(14) Uani 1 1 d . . . H1 H 0.2915 0.7698 -0.1245 0.039 Uiso 1 1 calc R . . C2 C 0.3480(5) 0.8054(4) 0.1222(3) 0.0208(11) Uani 1 1 d . . . H2 H 0.3595 0.7848 0.1968 0.025 Uiso 1 1 calc R . . C3 C 0.5190(5) 0.3948(4) -0.1063(4) 0.0197(10) Uani 1 1 d . . . H3 H 0.4906 0.3947 -0.1808 0.024 Uiso 1 1 calc R . . C4 C 0.5157(5) 0.3940(4) 0.0736(4) 0.0183(10) Uani 1 1 d . . . H4 H 0.4842 0.3935 0.1473 0.022 Uiso 1 1 calc R . . C5 C 0.3051(8) 0.6092(4) 0.0556(4) 0.0553(19) Uani 1 1 d . . . H5A H 0.2431 0.5957 0.1190 0.066 Uiso 1 1 calc R . . H5B H 0.3982 0.5796 0.0749 0.066 Uiso 1 1 calc R . . C6 C 0.2496(5) 0.5424(4) -0.0417(4) 0.0236(12) Uani 1 1 d . . . H6A H 0.2973 0.5661 -0.1097 0.028 Uiso 1 1 calc R . . H6B H 0.1485 0.5562 -0.0506 0.028 Uiso 1 1 calc R . . C7 C 0.2759(4) 0.4157(4) -0.0211(4) 0.0220(11) Uani 1 1 d . . . H7A H 0.2333 0.3930 0.0493 0.026 Uiso 1 1 calc R . . H7B H 0.2327 0.3712 -0.0804 0.026 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 0.0178(2) 0.01911(19) 0.00995(18) -0.00068(15) 0.00029(18) -0.0042(2) Mo2 0.0181(2) 0.0188(2) 0.00955(18) -0.00128(15) 0.00043(17) -0.0046(2) O1 0.0168(14) 0.0229(17) 0.0128(15) -0.0009(13) 0.0018(13) -0.0075(12) O2 0.0242(18) 0.048(2) 0.0186(18) -0.0090(16) 0.0014(15) -0.0013(17) O3 0.045(2) 0.0232(17) 0.0171(16) 0.0041(13) -0.0018(18) -0.0110(19) O4 0.0225(15) 0.0200(18) 0.0114(15) 0.0016(14) -0.0018(13) -0.0025(13) O5 0.0203(17) 0.047(2) 0.0144(16) 0.0039(16) -0.0031(14) -0.0022(17) O6 0.045(2) 0.0240(17) 0.0182(16) -0.0032(14) 0.0092(17) -0.0080(18) N1 0.033(2) 0.023(2) 0.0140(19) -0.0010(18) -0.0034(17) 0.0003(18) N2 0.029(2) 0.023(2) 0.0135(18) -0.0025(16) 0.0008(18) 0.001(2) N3 0.037(2) 0.017(2) 0.022(2) -0.0009(18) -0.0097(18) 0.0029(17) N4 0.017(2) 0.027(2) 0.0094(17) 0.0016(16) 0.0031(16) -0.0025(19) N5 0.019(2) 0.022(2) 0.0137(19) -0.0024(15) 0.0005(17) -0.0007(18) N6 0.0174(17) 0.016(2) 0.0190(19) 0.0047(18) 0.0013(17) -0.0024(15) C1 0.060(4) 0.021(3) 0.017(3) -0.002(2) -0.020(2) 0.001(2) C2 0.029(3) 0.021(2) 0.013(2) 0.0009(19) 0.003(2) 0.002(2) C3 0.023(3) 0.020(3) 0.015(2) 0.002(2) -0.001(2) -0.006(2) C4 0.021(2) 0.017(3) 0.017(2) -0.001(2) 0.000(2) -0.001(2) C5 0.110(5) 0.017(3) 0.039(3) 0.001(3) -0.033(3) 0.000(3) C6 0.018(2) 0.024(3) 0.029(3) -0.001(2) -0.008(2) 0.003(2) C7 0.015(2) 0.020(3) 0.031(3) -0.005(3) -0.006(2) -0.002(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 O2 1.704(3) . ? Mo1 O3 1.705(3) . ? Mo1 O4 1.905(3) 2_574 ? Mo1 O1 1.922(3) . ? Mo1 N1 2.384(4) . ? Mo1 N5 2.387(3) 4_465 ? Mo2 O5 1.703(3) . ? Mo2 O6 1.712(3) . ? Mo2 O4 1.914(3) . ? Mo2 O1 1.915(3) . ? Mo2 N4 2.367(3) 4_465 ? Mo2 N2 2.393(3) . ? N1 C1 1.305(6) . ? N1 N2 1.374(5) . ? N2 C2 1.307(5) . ? N3 C2 1.331(5) . ? N3 C1 1.346(6) . ? N3 C5 1.473(6) . ? N4 C3 1.309(5) . ? N4 N5 1.374(4) . ? N5 C4 1.303(5) . ? N6 C3 1.348(5) . ? N6 C4 1.362(5) . ? N6 C7 1.469(5) . ? C1 H1 0.9300 . ? C2 H2 0.9300 . ? C3 H3 0.9300 . ? C4 H4 0.9300 . ? C5 C6 1.497(7) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C7 1.529(6) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 H7A 0.9700 . ? C7 H7B 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 O3 104.36(17) . . ? O2 Mo1 O4 99.95(15) . 2_574 ? O3 Mo1 O4 100.13(15) . 2_574 ? O2 Mo1 O1 98.90(12) . . ? O3 Mo1 O1 100.38(13) . . ? O4 Mo1 O1 147.62(12) 2_574 . ? O2 Mo1 N1 89.52(15) . . ? O3 Mo1 N1 166.12(15) . . ? O4 Mo1 N1 77.42(12) 2_574 . ? O1 Mo1 N1 76.65(11) . . ? O2 Mo1 N5 165.72(14) . 4_465 ? O3 Mo1 N5 89.52(15) . 4_465 ? O4 Mo1 N5 80.53(12) 2_574 4_465 ? O1 Mo1 N5 74.86(11) . 4_465 ? N1 Mo1 N5 76.61(12) . 4_465 ? O5 Mo2 O6 103.89(16) . . ? O5 Mo2 O4 99.77(14) . . ? O6 Mo2 O4 100.16(15) . . ? O5 Mo2 O1 100.07(12) . . ? O6 Mo2 O1 101.34(13) . . ? O4 Mo2 O1 146.14(12) . . ? O5 Mo2 N4 166.85(14) . 4_465 ? O6 Mo2 N4 89.06(14) . 4_465 ? O4 Mo2 N4 79.85(12) . 4_465 ? O1 Mo2 N4 74.69(11) . 4_465 ? O5 Mo2 N2 88.28(15) . . ? O6 Mo2 N2 167.80(15) . . ? O4 Mo2 N2 78.14(13) . . ? O1 Mo2 N2 75.32(12) . . ? N4 Mo2 N2 78.75(12) 4_465 . ? Mo2 O1 Mo1 142.39(14) . . ? Mo1 O4 Mo2 176.31(18) 2_575 . ? C1 N1 N2 106.6(4) . . ? C1 N1 Mo1 135.5(3) . . ? N2 N1 Mo1 117.6(3) . . ? C2 N2 N1 107.0(4) . . ? C2 N2 Mo2 134.5(3) . . ? N1 N2 Mo2 117.6(3) . . ? C2 N3 C1 105.4(4) . . ? C2 N3 C5 123.5(4) . . ? C1 N3 C5 131.1(4) . . ? C3 N4 N5 107.2(3) . . ? C3 N4 Mo2 132.7(3) . 4_565 ? N5 N4 Mo2 120.1(3) . 4_565 ? C4 N5 N4 107.5(3) . . ? C4 N5 Mo1 135.0(3) . 4_565 ? N4 N5 Mo1 116.4(3) . 4_565 ? C3 N6 C4 105.1(3) . . ? C3 N6 C7 126.4(4) . . ? C4 N6 C7 127.2(4) . . ? N1 C1 N3 110.5(4) . . ? N1 C1 H1 124.8 . . ? N3 C1 H1 124.8 . . ? N2 C2 N3 110.5(4) . . ? N2 C2 H2 124.7 . . ? N3 C2 H2 124.7 . . ? N4 C3 N6 110.3(4) . . ? N4 C3 H3 124.9 . . ? N6 C3 H3 124.9 . . ? N5 C4 N6 109.9(4) . . ? N5 C4 H4 125.0 . . ? N6 C4 H4 125.0 . . ? N3 C5 C6 116.5(4) . . ? N3 C5 H5A 108.2 . . ? C6 C5 H5A 108.2 . . ? N3 C5 H5B 108.2 . . ? C6 C5 H5B 108.2 . . ? H5A C5 H5B 107.3 . . ? C5 C6 C7 109.2(4) . . ? C5 C6 H6A 109.8 . . ? C7 C6 H6A 109.8 . . ? C5 C6 H6B 109.8 . . ? C7 C6 H6B 109.8 . . ? H6A C6 H6B 108.3 . . ? N6 C7 C6 109.1(4) . . ? N6 C7 H7A 109.9 . . ? C6 C7 H7A 109.9 . . ? N6 C7 H7B 109.9 . . ? C6 C7 H7B 109.9 . . ? H7A C7 H7B 108.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O5 Mo2 O1 Mo1 125.8(3) . . . . ? O6 Mo2 O1 Mo1 -127.6(3) . . . . ? O4 Mo2 O1 Mo1 0.8(4) . . . . ? N4 Mo2 O1 Mo1 -41.8(2) 4_465 . . . ? N2 Mo2 O1 Mo1 40.3(2) . . . . ? O2 Mo1 O1 Mo2 -122.6(3) . . . . ? O3 Mo1 O1 Mo2 130.9(3) . . . . ? O4 Mo1 O1 Mo2 2.4(4) 2_574 . . . ? N1 Mo1 O1 Mo2 -35.2(2) . . . . ? N5 Mo1 O1 Mo2 44.3(2) 4_465 . . . ? O2 Mo1 N1 C1 -71.2(5) . . . . ? O3 Mo1 N1 C1 110.4(7) . . . . ? O4 Mo1 N1 C1 29.1(5) 2_574 . . . ? O1 Mo1 N1 C1 -170.4(5) . . . . ? N5 Mo1 N1 C1 112.2(5) 4_465 . . . ? O2 Mo1 N1 N2 101.3(3) . . . . ? O3 Mo1 N1 N2 -77.2(7) . . . . ? O4 Mo1 N1 N2 -158.4(3) 2_574 . . . ? O1 Mo1 N1 N2 2.0(3) . . . . ? N5 Mo1 N1 N2 -75.3(3) 4_465 . . . ? C1 N1 N2 C2 0.5(5) . . . . ? Mo1 N1 N2 C2 -173.9(3) . . . . ? C1 N1 N2 Mo2 -170.1(3) . . . . ? Mo1 N1 N2 Mo2 15.4(4) . . . . ? O5 Mo2 N2 C2 67.8(5) . . . . ? O6 Mo2 N2 C2 -115.7(7) . . . . ? O4 Mo2 N2 C2 -32.5(5) . . . . ? O1 Mo2 N2 C2 168.7(5) . . . . ? N4 Mo2 N2 C2 -114.4(5) 4_465 . . . ? O5 Mo2 N2 N1 -124.8(3) . . . . ? O6 Mo2 N2 N1 51.7(8) . . . . ? O4 Mo2 N2 N1 134.9(3) . . . . ? O1 Mo2 N2 N1 -23.9(3) . . . . ? N4 Mo2 N2 N1 53.0(3) 4_465 . . . ? C3 N4 N5 C4 -0.3(5) . . . . ? Mo2 N4 N5 C4 176.6(3) 4_565 . . . ? C3 N4 N5 Mo1 -170.1(3) . . . 4_565 ? Mo2 N4 N5 Mo1 6.8(4) 4_565 . . 4_565 ? N2 N1 C1 N3 -0.4(6) . . . . ? Mo1 N1 C1 N3 172.6(3) . . . . ? C2 N3 C1 N1 0.1(6) . . . . ? C5 N3 C1 N1 -176.5(5) . . . . ? N1 N2 C2 N3 -0.5(5) . . . . ? Mo2 N2 C2 N3 167.8(3) . . . . ? C1 N3 C2 N2 0.3(6) . . . . ? C5 N3 C2 N2 177.2(5) . . . . ? N5 N4 C3 N6 0.5(5) . . . . ? Mo2 N4 C3 N6 -175.9(3) 4_565 . . . ? C4 N6 C3 N4 -0.5(5) . . . . ? C7 N6 C3 N4 167.7(4) . . . . ? N4 N5 C4 N6 0.0(5) . . . . ? Mo1 N5 C4 N6 167.1(3) 4_565 . . . ? C3 N6 C4 N5 0.3(5) . . . . ? C7 N6 C4 N5 -167.7(4) . . . . ? C2 N3 C5 C6 171.1(5) . . . . ? C1 N3 C5 C6 -12.8(9) . . . . ? N3 C5 C6 C7 166.9(5) . . . . ? C3 N6 C7 C6 -73.1(5) . . . . ? C4 N6 C7 C6 92.5(5) . . . . ? C5 C6 C7 N6 -64.6(5) . . . . ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 26.67 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 0.512 _refine_diff_density_min -0.772 _refine_diff_density_rms 0.120 #============================================================================== data_(3) _database_code_depnum_ccdc_archive 'CCDC 752799' #TrackingRef 'Cif_data.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Molybdenum(VI) oxide 2:1 complex with trans-1,4-bis(1,2,4-triazol-4-yl)cyclohexane ; _chemical_name_common ; Molybdenum(VI) oxide 2:1 complex with trans-1,4-bis(1,2,4- triazol-4-yl)cyclohexane ; _chemical_melting_point ? _chemical_formula_moiety 'C10 H14 Mo2 N6 O6' _chemical_formula_sum 'C10 H14 Mo2 N6 O6' _chemical_formula_weight 506.15 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'I b c a' _space_group_name_Hall '-I 2b 2c' _symmetry_Int_Tables_number 73 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-x+1/2, y+1, -z+1' 'x+1, -y+1, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'x+1/2, -y, z' '-x, y, z+1/2' _cell_length_a 12.0221(7) _cell_length_b 13.0629(8) _cell_length_c 19.4476(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3054.1(4) _cell_formula_units_Z 8 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 3.11 _cell_measurement_theta_max 28.04 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.22 _exptl_crystal_density_diffrn 2.202 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1984 _exptl_absorpt_coefficient_mu 1.686 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.6877 _exptl_absorpt_correction_T_max 0.7080 _exptl_absorpt_process_details 'X-RED (Stoe & Cie, 2001) and X-SHAPE (Stoe & Cie, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe Imaging plate diffraction system' _diffrn_measurement_method '\f oscillation scans' _diffrn_standards_decay_% 0 _diffrn_reflns_number 10248 _diffrn_reflns_av_R_equivalents 0.0539 _diffrn_reflns_av_sigmaI/netI 0.0340 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 28.04 _reflns_number_total 1830 _reflns_number_gt 1378 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS Software (Stoe & Cie, 2000)' _computing_cell_refinement 'IPDS Software (Stoe & Cie, 2000)' _computing_data_reduction 'IPDS Software (Stoe & Cie, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e (Brandenburg, 1999)' _computing_publication_material 'WinGX 1.70.01 (Farrugia, 1999)' #------------------------------- Refinement data-----------------------# _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^)+(0.0225P)^2^+8.2038P] 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_number_reflns 1830 _refine_ls_number_parameters 110 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0658 _refine_ls_R_factor_gt 0.0550 _refine_ls_wR_factor_ref 0.0942 _refine_ls_wR_factor_gt 0.0926 _refine_ls_goodness_of_fit_ref 1.230 _refine_ls_restrained_S_all 1.230 _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 0.2500 0.12518(5) 0.5000 0.01664(15) Uani 1 2 d S . . Mo2 Mo 0.0000 0.2500 0.57802(3) 0.01500(15) Uani 1 2 d S . . O1 O 0.1891(4) 0.0457(3) 0.4408(2) 0.0309(10) Uani 1 1 d . . . O2 O 0.1216(3) 0.1610(3) 0.55470(17) 0.0181(7) Uani 1 1 d . . . O3 O -0.0668(4) 0.1671(4) 0.6321(2) 0.0280(9) Uani 1 1 d . . . N1 N 0.1688(4) 0.2699(3) 0.4463(2) 0.0174(9) Uani 1 1 d . . . N2 N 0.0848(4) 0.3240(3) 0.4773(2) 0.0167(9) Uani 1 1 d . . . N3 N 0.1242(4) 0.3970(3) 0.3792(2) 0.0177(9) Uani 1 1 d . . . C1 C 0.1909(5) 0.3144(4) 0.3878(3) 0.0212(11) Uani 1 1 d . . . H1 H 0.2452 0.2924 0.3563 0.025 Uiso 1 1 calc R . . C2 C 0.0601(5) 0.4002(4) 0.4366(2) 0.0193(11) Uani 1 1 d . . . H2 H 0.0057 0.4501 0.4457 0.023 Uiso 1 1 calc R . . C3 C 0.1232(5) 0.4715(4) 0.3218(3) 0.0214(11) Uani 1 1 d . . . H3 H 0.1237 0.5414 0.3415 0.026 Uiso 1 1 calc R . . C4 C 0.2261(6) 0.4587(8) 0.2784(4) 0.065(3) Uani 1 1 d . . . H4A H 0.2268 0.3904 0.2576 0.078 Uiso 1 1 calc R . . H4B H 0.2926 0.4658 0.3071 0.078 Uiso 1 1 calc R . . C5 C 0.0208(5) 0.4600(6) 0.2790(3) 0.0403(19) Uani 1 1 d . . . H5A H -0.0453 0.4691 0.3079 0.048 Uiso 1 1 calc R . . H5B H 0.0183 0.3910 0.2592 0.048 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 0.0161(3) 0.0150(3) 0.0188(3) 0.000 0.0021(2) 0.000 Mo2 0.0142(3) 0.0187(3) 0.0122(2) 0.000 0.000 -0.0003(3) O1 0.028(2) 0.027(2) 0.038(2) -0.0150(18) 0.0063(19) -0.0041(18) O2 0.017(2) 0.0205(17) 0.0170(16) 0.0051(14) 0.0027(14) 0.0018(15) O3 0.023(2) 0.035(2) 0.027(2) 0.0133(18) 0.0058(16) -0.0014(18) N1 0.015(2) 0.021(2) 0.0160(18) 0.0018(16) 0.0015(16) 0.0023(17) N2 0.016(2) 0.017(2) 0.0167(18) -0.0022(16) 0.0031(16) 0.0000(17) N3 0.018(2) 0.021(2) 0.0140(18) 0.0058(16) 0.0004(16) -0.0028(18) C1 0.017(3) 0.029(3) 0.018(2) 0.002(2) 0.001(2) 0.002(2) C2 0.024(3) 0.018(2) 0.016(2) -0.0011(18) 0.004(2) -0.002(2) C3 0.030(3) 0.020(2) 0.014(2) 0.007(2) -0.003(2) -0.006(2) C4 0.015(4) 0.125(9) 0.054(5) 0.066(6) 0.003(3) 0.006(4) C5 0.014(4) 0.069(5) 0.038(4) 0.034(4) -0.001(2) -0.006(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 O1 1.714(4) . ? Mo1 O1 1.714(4) 7_545 ? Mo1 O2 1.932(4) . ? Mo1 O2 1.932(4) 7_545 ? Mo1 N1 2.370(4) 7_545 ? Mo1 N1 2.370(4) . ? Mo2 O3 1.710(4) 6_454 ? Mo2 O3 1.710(4) . ? Mo2 O2 1.922(4) 6_454 ? Mo2 O2 1.922(4) . ? Mo2 N2 2.411(4) 6_454 ? Mo2 N2 2.411(4) . ? N1 C1 1.305(7) . ? N1 N2 1.372(6) . ? N2 C2 1.306(7) . ? N3 C1 1.355(7) . ? N3 C2 1.357(6) . ? N3 C3 1.480(6) . ? C1 H1 0.9400 . ? C2 H2 0.9400 . ? C3 C5 1.494(8) . ? C3 C4 1.506(9) . ? C3 H3 0.9900 . ? C4 C4 1.545(13) 8_455 ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C5 C5 1.538(11) 8_455 ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mo1 O1 105.4(3) . 7_545 ? O1 Mo1 O2 100.11(19) . . ? O1 Mo1 O2 96.79(18) 7_545 . ? O1 Mo1 O2 96.79(18) . 7_545 ? O1 Mo1 O2 100.11(19) 7_545 7_545 ? O2 Mo1 O2 151.9(2) . 7_545 ? O1 Mo1 N1 162.73(19) . 7_545 ? O1 Mo1 N1 90.64(19) 7_545 7_545 ? O2 Mo1 N1 83.86(16) . 7_545 ? O2 Mo1 N1 73.75(15) 7_545 7_545 ? O1 Mo1 N1 90.64(19) . . ? O1 Mo1 N1 162.73(19) 7_545 . ? O2 Mo1 N1 73.75(15) . . ? O2 Mo1 N1 83.86(16) 7_545 . ? N1 Mo1 N1 74.2(2) 7_545 . ? O3 Mo2 O3 104.1(3) 6_454 . ? O3 Mo2 O2 96.85(18) 6_454 6_454 ? O3 Mo2 O2 99.84(19) . 6_454 ? O3 Mo2 O2 99.84(19) 6_454 . ? O3 Mo2 O2 96.85(18) . . ? O2 Mo2 O2 152.7(2) 6_454 . ? O3 Mo2 N2 162.26(19) 6_454 6_454 ? O3 Mo2 N2 92.71(18) . 6_454 ? O2 Mo2 N2 74.28(15) 6_454 6_454 ? O2 Mo2 N2 83.54(15) . 6_454 ? O3 Mo2 N2 92.71(18) 6_454 . ? O3 Mo2 N2 162.26(19) . . ? O2 Mo2 N2 83.54(15) 6_454 . ? O2 Mo2 N2 74.28(15) . . ? N2 Mo2 N2 71.3(2) 6_454 . ? Mo2 O2 Mo1 152.2(2) . . ? C1 N1 N2 107.7(4) . . ? C1 N1 Mo1 131.0(4) . . ? N2 N1 Mo1 121.4(3) . . ? C2 N2 N1 107.1(4) . . ? C2 N2 Mo2 134.6(4) . . ? N1 N2 Mo2 117.5(3) . . ? C1 N3 C2 105.0(4) . . ? C1 N3 C3 128.4(5) . . ? C2 N3 C3 126.5(5) . . ? N1 C1 N3 110.0(5) . . ? N1 C1 H1 125.0 . . ? N3 C1 H1 125.0 . . ? N2 C2 N3 110.3(5) . . ? N2 C2 H2 124.9 . . ? N3 C2 H2 124.9 . . ? N3 C3 C5 111.1(5) . . ? N3 C3 C4 110.0(5) . . ? C5 C3 C4 110.7(5) . . ? N3 C3 H3 108.3 . . ? C5 C3 H3 108.3 . . ? C4 C3 H3 108.3 . . ? C3 C4 C4 108.9(7) . 8_455 ? C3 C4 H4A 109.9 . . ? C4 C4 H4A 109.9 8_455 . ? C3 C4 H4B 109.9 . . ? C4 C4 H4B 109.9 8_455 . ? H4A C4 H4B 108.3 . . ? C3 C5 C5 109.9(5) . 8_455 ? C3 C5 H5A 109.7 . . ? C5 C5 H5A 109.7 8_455 . ? C3 C5 H5B 109.7 . . ? C5 C5 H5B 109.7 8_455 . ? H5A C5 H5B 108.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Mo2 O2 Mo1 -85.8(5) 6_454 . . . ? O3 Mo2 O2 Mo1 168.6(5) . . . . ? O2 Mo2 O2 Mo1 41.1(4) 6_454 . . . ? N2 Mo2 O2 Mo1 76.6(5) 6_454 . . . ? N2 Mo2 O2 Mo1 4.3(4) . . . . ? O1 Mo1 O2 Mo2 -95.6(5) . . . . ? O1 Mo1 O2 Mo2 157.4(5) 7_545 . . . ? O2 Mo1 O2 Mo2 30.6(4) 7_545 . . . ? N1 Mo1 O2 Mo2 67.5(5) 7_545 . . . ? N1 Mo1 O2 Mo2 -7.9(4) . . . . ? O1 Mo1 N1 C1 -71.8(5) . . . . ? O1 Mo1 N1 C1 129.4(7) 7_545 . . . ? O2 Mo1 N1 C1 -172.2(5) . . . . ? O2 Mo1 N1 C1 25.0(5) 7_545 . . . ? N1 Mo1 N1 C1 99.8(5) 7_545 . . . ? O1 Mo1 N1 N2 109.7(4) . . . . ? O1 Mo1 N1 N2 -49.2(8) 7_545 . . . ? O2 Mo1 N1 N2 9.3(3) . . . . ? O2 Mo1 N1 N2 -153.6(4) 7_545 . . . ? N1 Mo1 N1 N2 -78.8(4) 7_545 . . . ? C1 N1 N2 C2 -0.7(6) . . . . ? Mo1 N1 N2 C2 178.1(3) . . . . ? C1 N1 N2 Mo2 170.3(4) . . . . ? Mo1 N1 N2 Mo2 -10.9(5) . . . . ? O3 Mo2 N2 C2 -87.1(5) 6_454 . . . ? O3 Mo2 N2 C2 111.6(7) . . . . ? O2 Mo2 N2 C2 9.5(5) 6_454 . . . ? O2 Mo2 N2 C2 173.4(5) . . . . ? N2 Mo2 N2 C2 85.0(5) 6_454 . . . ? O3 Mo2 N2 N1 105.0(4) 6_454 . . . ? O3 Mo2 N2 N1 -56.2(7) . . . . ? O2 Mo2 N2 N1 -158.4(4) 6_454 . . . ? O2 Mo2 N2 N1 5.6(3) . . . . ? N2 Mo2 N2 N1 -82.8(3) 6_454 . . . ? N2 N1 C1 N3 0.2(6) . . . . ? Mo1 N1 C1 N3 -178.4(3) . . . . ? C2 N3 C1 N1 0.3(6) . . . . ? C3 N3 C1 N1 177.7(5) . . . . ? N1 N2 C2 N3 0.9(6) . . . . ? Mo2 N2 C2 N3 -167.9(4) . . . . ? C1 N3 C2 N2 -0.7(6) . . . . ? C3 N3 C2 N2 -178.2(5) . . . . ? C1 N3 C3 C5 110.3(7) . . . . ? C2 N3 C3 C5 -72.9(7) . . . . ? C1 N3 C3 C4 -12.7(9) . . . . ? C2 N3 C3 C4 164.2(6) . . . . ? N3 C3 C4 C4 -176.8(8) . . . 8_455 ? C5 C3 C4 C4 60.0(11) . . . 8_455 ? N3 C3 C5 C5 178.6(7) . . . 8_455 ? C4 C3 C5 C5 -58.8(9) . . . 8_455 ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 28.04 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.691 _refine_diff_density_min -0.646 _refine_diff_density_rms 0.149 #============================================================================== data_(4) _database_code_depnum_ccdc_archive 'CCDC 752800' #TrackingRef 'Cif_data.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Molybdenum(VI) oxide 2:1 complex with 1,3-bis(1,2,4-triazol-4-yl)adamantane Hexahydrate ; _chemical_name_common ; Molybdenum(VI) oxide 2:1 complex with 1,3-bis(1,2,4-triazol-4- yl)adamantane Hexahydrate ; _chemical_melting_point ? _chemical_formula_moiety 'C14 H18 Mo2 N6 O6, 6(H2 O)' _chemical_formula_sum 'C14 H30 Mo2 N6 O12' _chemical_formula_weight 666.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n m a' _space_group_name_Hall '-P 2ac 2n' _symmetry_Int_Tables_number 62 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' _cell_length_a 15.1155(9) _cell_length_b 12.4471(7) _cell_length_c 12.4209(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2336.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 2.12 _cell_measurement_theta_max 27.36 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.19 _exptl_crystal_density_diffrn 1.894 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1344 _exptl_absorpt_coefficient_mu 1.145 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.7551 _exptl_absorpt_correction_T_max 0.8119 _exptl_absorpt_process_details 'X-RED (Stoe & Cie, 2001) and X-SHAPE (Stoe & Cie, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe Imaging plate diffraction system' _diffrn_measurement_method '\f oscillation scans' _diffrn_standards_decay_% 0 _diffrn_reflns_number 8721 _diffrn_reflns_av_R_equivalents 0.0454 _diffrn_reflns_av_sigmaI/netI 0.0315 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 27.36 _reflns_number_total 2735 _reflns_number_gt 2268 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS Software (Stoe & Cie, 2000)' _computing_cell_refinement 'IPDS Software (Stoe & Cie, 2000)' _computing_data_reduction 'IPDS Software (Stoe & Cie, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e (Brandenburg, 1999)' _computing_publication_material 'WinGX 1.70.01 (Farrugia, 1999)' #------------------------------- Refinement data-----------------------# _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^)+(0.0395P)^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_number_reflns 2735 _refine_ls_number_parameters 169 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0339 _refine_ls_R_factor_gt 0.0251 _refine_ls_wR_factor_ref 0.0632 _refine_ls_wR_factor_gt 0.0609 _refine_ls_goodness_of_fit_ref 0.987 _refine_ls_restrained_S_all 0.987 _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 -0.060694(11) 0.397157(14) 0.086067(13) 0.01132(7) Uani 1 1 d . . . O1 O -0.08802(13) 0.2500 0.12276(17) 0.0130(4) Uani 1 2 d S . . O2 O -0.03059(11) 0.44287(14) 0.21130(13) 0.0206(3) Uani 1 1 d . . . O3 O 0.0000 0.5000 0.0000 0.0161(5) Uani 1 2 d S . . O4 O -0.16577(10) 0.44338(14) 0.06935(14) 0.0220(4) Uani 1 1 d . . . N1 N 0.21165(15) 0.2500 0.0395(2) 0.0137(5) Uani 1 2 d S . . N2 N 0.07644(11) 0.30574(16) 0.06862(14) 0.0150(4) Uani 1 1 d . . . N3 N 0.42830(16) 0.2500 -0.2530(2) 0.0144(5) Uani 1 2 d S . . N4 N 0.43252(11) 0.30533(16) -0.41946(14) 0.0156(4) Uani 1 1 d . . . C1 C 0.15825(14) 0.33677(19) 0.05091(19) 0.0173(4) Uani 1 1 d . . . H1 H 0.1770 0.4087 0.0467 0.021 Uiso 1 1 calc R . . C2 C 0.42996(15) 0.33648(19) -0.31864(17) 0.0175(5) Uani 1 1 d . . . H2 H 0.4294 0.4084 -0.2955 0.021 Uiso 1 1 calc R . . C3 C 0.30823(18) 0.2500 0.0145(2) 0.0130(5) Uani 1 2 d S . . C4 C 0.3195(2) 0.2500 -0.1079(2) 0.0148(6) Uani 1 2 d S . . H4 H 0.2917 0.3130 -0.1386 0.018 Uiso 1 1 d . . . C5 C 0.4188(2) 0.2500 -0.1335(2) 0.0150(6) Uani 1 2 d S . . C6 C 0.46238(15) 0.1492(2) -0.08617(17) 0.0171(4) Uani 1 1 d . . . H6A H 0.4352 0.0847 -0.1171 0.021 Uiso 1 1 calc R . . H6B H 0.5256 0.1485 -0.1037 0.021 Uiso 1 1 calc R . . C7 C 0.44985(14) 0.1497(2) 0.03604(18) 0.0178(4) Uani 1 1 d . . . H7 H 0.4780 0.0849 0.0670 0.021 Uiso 1 1 calc R . . C8 C 0.35027(14) 0.1487(2) 0.06282(17) 0.0166(4) Uani 1 1 d . . . H8A H 0.3224 0.0844 0.0324 0.020 Uiso 1 1 calc R . . H8B H 0.3417 0.1478 0.1410 0.020 Uiso 1 1 calc R . . C9 C 0.4926(2) 0.2500 0.0848(3) 0.0196(7) Uani 1 2 d S . . H9A H 0.5562 0.2500 0.0697 0.024 Uiso 1 2 calc SR . . H9B H 0.4844 0.2500 0.1630 0.024 Uiso 1 2 calc SR . . O5 O 0.72115(16) 0.2500 0.1140(2) 0.0322(6) Uani 1 2 d S . . H1W H 0.7776 0.2500 0.1235 0.048 Uiso 1 2 d S . . H2W H 0.7113 0.2500 0.0484 0.048 Uiso 1 2 d S . . O6 O 0.34704(14) -0.0661(2) -0.2049(2) 0.0453(6) Uani 1 1 d . . . H3W H 0.3983 -0.0712 -0.2253 0.068 Uiso 1 1 d . . . H4W H 0.3303 -0.1265 -0.1773 0.068 Uiso 1 1 d . . . O7 O 0.7008(3) 0.2500 -0.1022(3) 0.0595(10) Uani 1 2 d S . . H5W H 0.7054 0.1947 -0.1469 0.089 Uiso 1 1 d . . . O8 O 0.20789(18) 0.0626(2) -0.2810(2) 0.0572(7) Uani 1 1 d . . . H6W H 0.1806 0.0406 -0.2274 0.086 Uiso 1 1 d . . . H7W H 0.2604 0.0312 -0.2777 0.086 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.01283(10) 0.00700(11) 0.01412(10) -0.00021(6) 0.00196(6) -0.00004(6) O1 0.0138(9) 0.0102(11) 0.0149(9) 0.000 0.0022(8) 0.000 O2 0.0291(8) 0.0146(8) 0.0180(8) -0.0006(7) 0.0021(7) -0.0038(7) O3 0.0201(10) 0.0098(12) 0.0184(10) 0.0001(8) 0.0046(8) -0.0011(8) O4 0.0184(8) 0.0145(8) 0.0332(9) 0.0043(7) 0.0043(6) 0.0002(6) N1 0.0104(11) 0.0114(13) 0.0194(12) 0.000 0.0008(9) 0.000 N2 0.0127(7) 0.0115(10) 0.0207(9) 0.0008(7) 0.0022(6) 0.0002(7) N3 0.0182(11) 0.0109(12) 0.0141(11) 0.000 0.0027(9) 0.000 N4 0.0194(8) 0.0103(10) 0.0170(8) -0.0003(7) 0.0014(7) 0.0002(7) C1 0.0160(9) 0.0117(12) 0.0243(10) 0.0018(9) 0.0023(8) -0.0010(8) C2 0.0241(11) 0.0110(12) 0.0175(10) -0.0017(8) 0.0022(8) -0.0027(9) C3 0.0098(12) 0.0129(15) 0.0164(13) 0.000 0.0018(11) 0.000 C4 0.0150(13) 0.0129(14) 0.0164(13) 0.000 -0.0027(11) 0.000 C5 0.0188(14) 0.0125(15) 0.0137(13) 0.000 0.0013(11) 0.000 C6 0.0182(10) 0.0152(11) 0.0180(10) 0.0012(9) 0.0022(8) 0.0023(9) C7 0.0169(10) 0.0188(12) 0.0177(10) 0.0033(9) -0.0015(8) 0.0038(9) C8 0.0151(9) 0.0172(11) 0.0175(10) 0.0028(9) 0.0005(8) 0.0000(8) C9 0.0172(14) 0.0247(19) 0.0171(14) 0.000 -0.0018(11) 0.000 O5 0.0163(11) 0.0237(14) 0.0565(17) 0.000 0.0025(11) 0.000 O6 0.0424(11) 0.0319(12) 0.0618(15) 0.0035(11) 0.0190(11) -0.0075(10) O7 0.075(3) 0.042(2) 0.062(2) 0.000 -0.0044(19) 0.000 O8 0.0862(19) 0.0401(14) 0.0453(13) 0.0107(12) -0.0006(13) -0.0232(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 O4 1.7019(16) . ? Mo1 O2 1.7177(16) . ? Mo1 O3 1.90346(18) . ? Mo1 O1 1.9322(7) . ? Mo1 N4 2.3662(18) 6 ? Mo1 N2 2.3745(17) . ? N1 C1 1.356(3) 8_565 ? N1 C1 1.356(3) . ? N1 C3 1.493(3) . ? N2 C1 1.314(3) . ? N2 N2 1.387(4) 8_565 ? N3 C2 1.351(3) 8_565 ? N3 C2 1.351(3) . ? N3 C5 1.491(4) . ? N4 C2 1.312(3) . ? N4 N4 1.377(4) 8_565 ? C1 H1 0.9400 . ? C2 H2 0.9400 . ? C3 C4 1.530(4) . ? C3 C8 1.534(3) 8_565 ? C3 C8 1.534(3) . ? C4 C5 1.535(4) . ? C4 H4 0.9677 . ? C5 C6 1.534(3) 8_565 ? C5 C6 1.534(3) . ? C6 C7 1.530(3) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 C9 1.531(3) . ? C7 C8 1.542(3) . ? C7 H7 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C9 C7 1.531(3) 8_565 ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? O5 H1W 0.8606 . ? O5 H2W 0.8286 . ? O6 H3W 0.8171 . ? O6 H4W 0.8642 . ? O7 H5W 0.8866 . ? O8 H6W 0.8301 . ? O8 H7W 0.8851 . ? 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 O4 Mo1 O2 104.22(8) . . ? O4 Mo1 O3 98.85(6) . . ? O2 Mo1 O3 99.10(6) . . ? O4 Mo1 O1 98.61(8) . . ? O2 Mo1 O1 99.03(9) . . ? O3 Mo1 O1 150.81(6) . . ? O4 Mo1 N4 90.92(7) . 6 ? O2 Mo1 N4 164.46(7) . 6 ? O3 Mo1 N4 81.64(5) . 6 ? O1 Mo1 N4 74.88(8) . 6 ? O4 Mo1 N2 164.90(7) . . ? O2 Mo1 N2 90.58(7) . . ? O3 Mo1 N2 81.39(5) . . ? O1 Mo1 N2 75.75(7) . . ? N4 Mo1 N2 74.13(6) 6 . ? Mo1 O1 Mo1 142.88(11) . 8_565 ? Mo1 O3 Mo1 180.000(8) . 5_565 ? C1 N1 C1 105.6(2) 8_565 . ? C1 N1 C3 127.16(12) 8_565 . ? C1 N1 C3 127.16(12) . . ? C1 N2 N2 107.10(13) . 8_565 ? C1 N2 Mo1 134.10(16) . . ? N2 N2 Mo1 118.63(5) 8_565 . ? C2 N3 C2 105.7(3) 8_565 . ? C2 N3 C5 127.07(13) 8_565 . ? C2 N3 C5 127.07(13) . . ? C2 N4 N4 107.19(13) . 8_565 ? C2 N4 Mo1 133.92(16) . 6_655 ? N4 N4 Mo1 118.88(5) 8_565 6_655 ? N2 C1 N1 110.1(2) . . ? N2 C1 H1 125.0 . . ? N1 C1 H1 125.0 . . ? N4 C2 N3 110.0(2) . . ? N4 C2 H2 125.0 . . ? N3 C2 H2 125.0 . . ? N1 C3 C4 108.4(2) . . ? N1 C3 C8 108.90(15) . 8_565 ? C4 C3 C8 110.04(15) . 8_565 ? N1 C3 C8 108.90(15) . . ? C4 C3 C8 110.04(15) . . ? C8 C3 C8 110.5(2) 8_565 . ? C3 C4 C5 108.3(2) . . ? C3 C4 H4 110.1 . . ? C5 C4 H4 110.1 . . ? N3 C5 C6 109.88(16) . 8_565 ? N3 C5 C6 109.88(16) . . ? C6 C5 C6 109.8(3) 8_565 . ? N3 C5 C4 107.5(2) . . ? C6 C5 C4 109.90(16) 8_565 . ? C6 C5 C4 109.90(16) . . ? C7 C6 C5 108.9(2) . . ? C7 C6 H6A 109.9 . . ? C5 C6 H6A 109.9 . . ? C7 C6 H6B 109.9 . . ? C5 C6 H6B 109.9 . . ? H6A C6 H6B 108.3 . . ? C6 C7 C9 110.1(2) . . ? C6 C7 C8 109.57(18) . . ? C9 C7 C8 109.5(2) . . ? C6 C7 H7 109.2 . . ? C9 C7 H7 109.2 . . ? C8 C7 H7 109.2 . . ? C3 C8 C7 108.28(19) . . ? C3 C8 H8A 110.0 . . ? C7 C8 H8A 110.0 . . ? C3 C8 H8B 110.0 . . ? C7 C8 H8B 110.0 . . ? H8A C8 H8B 108.4 . . ? C7 C9 C7 109.3(3) . 8_565 ? C7 C9 H9A 109.8 . . ? C7 C9 H9A 109.8 8_565 . ? C7 C9 H9B 109.8 . . ? C7 C9 H9B 109.8 8_565 . ? H9A C9 H9B 108.3 . . ? H1W O5 H2W 108.2 . . ? H3W O6 H4W 109.5 . . ? H6W O8 H7W 105.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 Mo1 O1 Mo1 128.54(19) . . . 8_565 ? O2 Mo1 O1 Mo1 -125.46(19) . . . 8_565 ? O3 Mo1 O1 Mo1 2.4(3) . . . 8_565 ? N4 Mo1 O1 Mo1 39.92(18) 6 . . 8_565 ? N2 Mo1 O1 Mo1 -37.16(18) . . . 8_565 ? O4 Mo1 N2 C1 117.6(3) . . . . ? O2 Mo1 N2 C1 -73.7(2) . . . . ? O3 Mo1 N2 C1 25.5(2) . . . . ? O1 Mo1 N2 C1 -172.8(2) . . . . ? N4 Mo1 N2 C1 109.2(2) 6 . . . ? O4 Mo1 N2 N2 -57.0(3) . . . 8_565 ? O2 Mo1 N2 N2 111.83(6) . . . 8_565 ? O1 Mo1 N2 N2 12.66(6) . . . 8_565 ? N4 Mo1 N2 N2 -65.36(5) 6 . . 8_565 ? N2 N2 C1 N1 -0.1(2) 8_565 . . . ? Mo1 N2 C1 N1 -175.06(16) . . . . ? C1 N1 C1 N2 0.1(3) 8_565 . . . ? C3 N1 C1 N2 177.6(2) . . . . ? N4 N4 C2 N3 0.0(2) 8_565 . . . ? Mo1 N4 C2 N3 -178.69(16) 6_655 . . . ? C2 N3 C2 N4 0.0(3) 8_565 . . . ? C5 N3 C2 N4 -175.3(2) . . . . ? C1 N1 C3 C4 88.4(3) 8_565 . . . ? C1 N1 C3 C4 -88.4(3) . . . . ? C1 N1 C3 C8 -151.9(2) 8_565 . . 8_565 ? C1 N1 C3 C8 31.3(4) . . . 8_565 ? C1 N1 C3 C8 -31.3(4) 8_565 . . . ? C1 N1 C3 C8 151.9(2) . . . . ? N1 C3 C4 C5 180.0 . . . . ? C8 C3 C4 C5 61.02(16) 8_565 . . . ? C8 C3 C4 C5 -61.02(16) . . . . ? C2 N3 C5 C6 153.3(2) 8_565 . . 8_565 ? C2 N3 C5 C6 -32.4(4) . . . 8_565 ? C2 N3 C5 C6 32.4(4) 8_565 . . . ? C2 N3 C5 C6 -153.3(2) . . . . ? C2 N3 C5 C4 -87.2(3) 8_565 . . . ? C2 N3 C5 C4 87.2(3) . . . . ? C3 C4 C5 N3 180.0 . . . . ? C3 C4 C5 C6 -60.47(17) . . . 8_565 ? C3 C4 C5 C6 60.47(17) . . . . ? N3 C5 C6 C7 -178.65(19) . . . . ? C6 C5 C6 C7 60.4(3) 8_565 . . . ? C4 C5 C6 C7 -60.6(3) . . . . ? C5 C6 C7 C9 -59.9(2) . . . . ? C5 C6 C7 C8 60.6(3) . . . . ? N1 C3 C8 C7 179.82(19) . . . . ? C4 C3 C8 C7 61.2(2) . . . . ? C8 C3 C8 C7 -60.6(3) 8_565 . . . ? C6 C7 C8 C3 -60.7(3) . . . . ? C9 C7 C8 C3 60.2(2) . . . . ? C6 C7 C9 C7 59.5(3) . . . 8_565 ? C8 C7 C9 C7 -61.0(3) . . . 8_565 ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.36 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.606 _refine_diff_density_min -0.771 _refine_diff_density_rms 0.087 #============================================================================== data_(5) _database_code_depnum_ccdc_archive 'CCDC 752801' #TrackingRef 'Cif_data.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Molybdenum(VI) oxide 2:1 complex with 4,9-bis(1,2,4-triazol-4-yl)diamantane Semihydrate ; _chemical_name_common ; Molybdenum(VI) oxide 2:1 complex with 4,9-bis(1,2,4-triazol-4- yl)diamantane Semihydrate ; _chemical_melting_point ? _chemical_formula_moiety 'C18 H22 Mo2 N6 O6, 0.5(H2 O)' _chemical_formula_sum 'C18 H23 Mo2 N6 O6.50' _chemical_formula_weight 619.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'C m m a' _space_group_name_Hall '-C 2b 2' _symmetry_Int_Tables_number 67 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z' '-x, y+1/2, -z' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1, z' '-x+1/2, y+1, -z' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y-1/2, -z' 'x, -y-1/2, z' '-x, y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, y, -z' 'x+1/2, -y, z' '-x+1/2, y+1/2, z' _cell_length_a 12.4256(9) _cell_length_b 16.6809(16) _cell_length_c 10.4993(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2176.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 7657 _cell_measurement_theta_min 3.81 _cell_measurement_theta_max 27.85 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.09 _exptl_crystal_density_diffrn 1.890 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1236 _exptl_absorpt_coefficient_mu 1.204 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.8215 _exptl_absorpt_correction_T_max 0.8994 _exptl_absorpt_process_details 'X-RED (Stoe & Cie, 2001) and X-SHAPE (Stoe & Cie, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe Imaging plate diffraction system' _diffrn_measurement_method '\f oscillation scans' _diffrn_standards_decay_% 0 _diffrn_reflns_number 7657 _diffrn_reflns_av_R_equivalents 0.0378 _diffrn_reflns_av_sigmaI/netI 0.0331 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.81 _diffrn_reflns_theta_max 27.85 _reflns_number_total 1389 _reflns_number_gt 1123 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS Software (Stoe & Cie, 2000)' _computing_cell_refinement 'IPDS Software (Stoe & Cie, 2000)' _computing_data_reduction 'IPDS Software (Stoe & Cie, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e (Brandenburg, 1999)' _computing_publication_material 'WinGX 1.70.01 (Farrugia, 1999)' #------------------------------- Refinement data-----------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0346P)^2^+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_number_reflns 1389 _refine_ls_number_parameters 88 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0305 _refine_ls_R_factor_gt 0.0230 _refine_ls_wR_factor_ref 0.0530 _refine_ls_wR_factor_gt 0.0524 _refine_ls_goodness_of_fit_ref 0.919 _refine_ls_restrained_S_all 0.919 _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 0.14763(2) 0.7500 0.36072(2) 0.01571(9) Uani 1 2 d S . . O1 O 0.2500 0.7500 0.5000 0.0187(6) Uani 1 4 d S . . O2 O 0.0000 0.7500 0.3044(3) 0.0198(6) Uani 1 4 d S . . O3 O 0.19444(14) 0.66892(11) 0.27729(17) 0.0320(4) Uani 1 1 d . . . N1 N 0.05539(17) 0.83569(12) 0.50615(19) 0.0241(4) Uani 1 1 d . . . N2 N 0.0000 0.90011(16) 0.6754(3) 0.0211(6) Uani 1 2 d S . . C1 C 0.0869(2) 0.87409(14) 0.6081(2) 0.0257(5) Uani 1 1 d . . . H1 H 0.1590 0.8825 0.6316 0.031 Uiso 1 1 calc R . . C2 C 0.0000 0.93904(18) 0.8033(3) 0.0196(6) Uani 1 2 d S . . C3 C 0.0000 0.8746(2) 0.9064(4) 0.0306(8) Uani 1 2 d S . . H3 H 0.0639 0.8406 0.8975 0.037 Uiso 1 1 d . . . C4 C 0.0000 0.91539(19) 1.0387(3) 0.0282(8) Uani 1 2 d S . . H4 H 0.0000 0.8740 1.1063 0.034 Uiso 1 2 calc SR . . C5 C 0.1009(2) 0.99128(16) 0.8152(2) 0.0300(5) Uani 1 1 d . . . H5A H 0.1013 1.0323 0.7483 0.036 Uiso 1 1 calc R . . H5B H 0.1656 0.9582 0.8056 0.036 Uiso 1 1 calc R . . C6 C 0.1003(2) 1.03165(15) 0.9481(2) 0.0282(5) Uani 1 1 d . . . H6 H 0.1654 1.0654 0.9570 0.034 Uiso 1 1 calc R . . O4 O -0.2500 0.7500 1.0000 0.098(4) Uani 0.50 4 d SP . . 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 0.01178(14) 0.02361(13) 0.01173(12) 0.000 0.00084(11) 0.000 O1 0.0100(17) 0.0291(16) 0.0170(14) 0.000 -0.0029(12) 0.000 O2 0.0152(18) 0.0327(16) 0.0115(14) 0.000 0.000 0.000 O3 0.0214(10) 0.0430(10) 0.0316(10) -0.0171(8) -0.0038(7) 0.0058(7) N1 0.0150(11) 0.0313(10) 0.0260(10) -0.0080(8) -0.0006(8) 0.0009(8) N2 0.0141(15) 0.0247(13) 0.0244(13) -0.0091(10) 0.000 0.000 C1 0.0155(13) 0.0336(12) 0.0280(13) -0.0106(9) -0.0003(9) 0.0008(9) C2 0.0132(17) 0.0257(15) 0.0200(15) -0.0083(12) 0.000 0.000 C3 0.038(2) 0.0232(15) 0.0310(18) -0.0069(14) 0.000 0.000 C4 0.041(2) 0.0183(15) 0.0258(17) -0.0010(12) 0.000 0.000 C5 0.0222(14) 0.0399(14) 0.0280(11) -0.0126(10) 0.0068(11) -0.0106(10) C6 0.0178(14) 0.0376(12) 0.0292(12) -0.0130(10) 0.0056(10) -0.0118(10) O4 0.101(12) 0.133(11) 0.061(7) 0.000 -0.020(7) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 O3 1.7132(17) . ? Mo1 O3 1.7132(17) 11_575 ? Mo1 O2 1.9272(9) . ? Mo1 O1 1.9382(3) . ? Mo1 N1 2.3850(19) . ? Mo1 N1 2.3850(19) 11_575 ? N1 C1 1.308(3) . ? N1 N1 1.377(4) 12 ? N2 C1 1.361(3) 12 ? N2 C1 1.361(3) . ? N2 C2 1.492(4) . ? C1 H1 0.9400 . ? C2 C3 1.526(5) . ? C2 C5 1.532(3) . ? C2 C5 1.532(3) 12 ? C3 C4 1.547(5) . ? C3 H3 0.9802 . ? C4 C6 1.534(3) 4_577 ? C4 C6 1.534(3) 9_577 ? C4 H4 0.9900 . ? C5 C6 1.549(3) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 C6 1.518(5) 4_577 ? C6 C4 1.534(3) 9_577 ? C6 H6 0.9900 . ? 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 O3 Mo1 O3 104.28(14) . 11_575 ? O3 Mo1 O2 99.58(8) . . ? O3 Mo1 O2 99.58(8) 11_575 . ? O3 Mo1 O1 99.38(6) . . ? O3 Mo1 O1 99.38(6) 11_575 . ? O2 Mo1 O1 148.88(8) . . ? O3 Mo1 N1 164.51(8) . . ? O3 Mo1 N1 90.99(8) 11_575 . ? O2 Mo1 N1 74.87(8) . . ? O1 Mo1 N1 80.35(5) . . ? O3 Mo1 N1 90.99(8) . 11_575 ? O3 Mo1 N1 164.51(8) 11_575 11_575 ? O2 Mo1 N1 74.87(8) . 11_575 ? O1 Mo1 N1 80.35(5) . 11_575 ? N1 Mo1 N1 73.65(10) . 11_575 ? Mo1 O1 Mo1 180.0 . 13_566 ? Mo1 O2 Mo1 144.28(16) 2_565 . ? C1 N1 N1 107.40(14) . 12 ? C1 N1 Mo1 132.39(17) . . ? N1 N1 Mo1 118.72(5) 12 . ? C1 N2 C1 104.9(3) 12 . ? C1 N2 C2 127.31(13) 12 . ? C1 N2 C2 127.31(13) . . ? N1 C1 N2 110.1(2) . . ? N1 C1 H1 124.9 . . ? N2 C1 H1 124.9 . . ? N2 C2 C3 109.4(2) . . ? N2 C2 C5 108.73(17) . . ? C3 C2 C5 110.06(19) . . ? N2 C2 C5 108.73(17) . 12 ? C3 C2 C5 110.06(19) . 12 ? C5 C2 C5 109.8(3) . 12 ? C2 C3 C4 109.1(3) . . ? C2 C3 H3 109.9 . . ? C4 C3 H3 109.9 . . ? C6 C4 C6 108.7(3) 4_577 9_577 ? C6 C4 C3 109.56(18) 4_577 . ? C6 C4 C3 109.56(18) 9_577 . ? C6 C4 H4 109.7 4_577 . ? C6 C4 H4 109.7 9_577 . ? C3 C4 H4 109.7 . . ? C2 C5 C6 108.5(2) . . ? C2 C5 H5A 110.0 . . ? C6 C5 H5A 110.0 . . ? C2 C5 H5B 110.0 . . ? C6 C5 H5B 110.0 . . ? H5A C5 H5B 108.4 . . ? C6 C6 C4 109.62(18) 4_577 9_577 ? C6 C6 C5 110.1(2) 4_577 . ? C4 C6 C5 109.6(2) 9_577 . ? C6 C6 H6 109.1 4_577 . ? C4 C6 H6 109.1 9_577 . ? C5 C6 H6 109.1 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Mo1 O2 Mo1 126.81(7) . . . 2_565 ? O3 Mo1 O2 Mo1 -126.81(7) 11_575 . . 2_565 ? O1 Mo1 O2 Mo1 0.0 . . . 2_565 ? N1 Mo1 O2 Mo1 -38.38(5) . . . 2_565 ? N1 Mo1 O2 Mo1 38.38(5) 11_575 . . 2_565 ? O3 Mo1 N1 C1 106.0(3) . . . . ? O3 Mo1 N1 C1 -83.7(2) 11_575 . . . ? O2 Mo1 N1 C1 176.7(2) . . . . ? O1 Mo1 N1 C1 15.7(2) . . . . ? N1 Mo1 N1 C1 98.3(2) 11_575 . . . ? O3 Mo1 N1 N1 -58.2(3) . . . 12 ? O3 Mo1 N1 N1 112.19(7) 11_575 . . 12 ? O2 Mo1 N1 N1 12.54(5) . . . 12 ? N1 Mo1 N1 N1 -65.78(5) 11_575 . . 12 ? N1 N1 C1 N2 -0.4(2) 12 . . . ? Mo1 N1 C1 N2 -165.88(18) . . . . ? C1 N2 C1 N1 0.7(4) 12 . . . ? C2 N2 C1 N1 173.4(3) . . . . ? C1 N2 C2 C3 85.6(3) 12 . . . ? C1 N2 C2 C3 -85.6(3) . . . . ? C1 N2 C2 C5 -154.2(3) 12 . . . ? C1 N2 C2 C5 34.6(4) . . . . ? C1 N2 C2 C5 -34.6(4) 12 . . 12 ? C1 N2 C2 C5 154.2(3) . . . 12 ? N2 C2 C3 C4 180.000(2) . . . . ? C5 C2 C3 C4 60.60(17) . . . . ? C5 C2 C3 C4 -60.60(17) 12 . . . ? C2 C3 C4 C6 -59.57(18) . . . 4_577 ? C2 C3 C4 C6 59.57(18) . . . 9_577 ? N2 C2 C5 C6 179.9(2) . . . . ? C3 C2 C5 C6 -60.3(3) . . . . ? C5 C2 C5 C6 61.0(4) 12 . . . ? C2 C5 C6 C6 59.9(2) . . . 4_577 ? C2 C5 C6 C4 -60.8(3) . . . 9_577 ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.85 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.693 _refine_diff_density_min -0.487 _refine_diff_density_rms 0.061 #============================================================================== data_(6) _database_code_depnum_ccdc_archive 'CCDC 752802' #TrackingRef 'Cif_data.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Molybdenum(VI) oxide 4:1 complex with 1,6-bis(1,2,4-triazol-4-yl)diamantane Dihydrate ; _chemical_name_common ; Molybdenum(VI) oxide 4:1 complex with 1,6-bis(1,2,4-triazol-4- yl)diamantane Dihydrate ; _chemical_melting_point ? _chemical_formula_moiety 'C18 H22 N6, 4(Mo O3), 2(H2 O)' _chemical_formula_sum 'C18 H26 Mo4 N6 O14' _chemical_formula_weight 934.21 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.3804(8) _cell_length_b 7.5670(10) _cell_length_c 11.5827(14) _cell_angle_alpha 85.928(12) _cell_angle_beta 86.074(10) _cell_angle_gamma 89.873(11) _cell_volume 643.72(13) _cell_formula_units_Z 1 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 5805 _cell_measurement_theta_min 3.54 _cell_measurement_theta_max 27.55 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 2.410 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 456 _exptl_absorpt_coefficient_mu 1.988 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.7287 _exptl_absorpt_correction_T_max 0.8572 _exptl_absorpt_process_details 'X-RED (Stoe & Cie, 2001) and X-SHAPE (Stoe & Cie, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe Imaging plate diffraction system' _diffrn_measurement_method '\f oscillation scans' _diffrn_standards_decay_% 0 _diffrn_reflns_number 5805 _diffrn_reflns_av_R_equivalents 0.0410 _diffrn_reflns_av_sigmaI/netI 0.0463 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.54 _diffrn_reflns_theta_max 27.55 _reflns_number_total 2923 _reflns_number_gt 2244 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS Software (Stoe & Cie, 2000)' _computing_cell_refinement 'IPDS Software (Stoe & Cie, 2000)' _computing_data_reduction 'IPDS Software (Stoe & Cie, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e (Brandenburg, 1999)' _computing_publication_material 'WinGX 1.70.01 (Farrugia, 1999)' #------------------------------- Refinement data-----------------------# _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^)+(0.0229P)^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_number_reflns 2923 _refine_ls_number_parameters 190 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0302 _refine_ls_R_factor_gt 0.0217 _refine_ls_wR_factor_ref 0.0486 _refine_ls_wR_factor_gt 0.0473 _refine_ls_goodness_of_fit_ref 0.935 _refine_ls_restrained_S_all 0.935 _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 0.37002(3) 0.66569(3) 0.55075(2) 0.01075(7) Uani 1 1 d . . . Mo2 Mo 0.13324(3) 0.36823(3) 0.416763(19) 0.01009(7) Uani 1 1 d . . . O1 O 0.3870(3) 0.4403(3) 0.43412(17) 0.0120(4) Uani 1 1 d . . . O2 O 0.1174(3) 0.6162(3) 0.51543(17) 0.0126(4) Uani 1 1 d . . . O3 O 0.4180(3) 0.8286(3) 0.4463(2) 0.0215(5) Uani 1 1 d . . . O4 O 0.3397(3) 0.7714(3) 0.6747(2) 0.0248(5) Uani 1 1 d . . . O5 O 0.1127(3) 0.4735(3) 0.28268(18) 0.0209(5) Uani 1 1 d . . . O6 O 0.1439(3) 0.1499(3) 0.3923(2) 0.0207(5) Uani 1 1 d . . . N1 N 0.2778(3) 0.3959(3) 0.6705(2) 0.0129(5) Uani 1 1 d . . . N2 N 0.1831(3) 0.2800(3) 0.6103(2) 0.0131(5) Uani 1 1 d . . . N3 N 0.1638(3) 0.1811(3) 0.7915(2) 0.0127(5) Uani 1 1 d . . . C1 C 0.2645(4) 0.3333(4) 0.7799(2) 0.0139(6) Uani 1 1 d . . . H1 H 0.3167 0.3858 0.8409 0.017 Uiso 1 1 calc R . . C2 C 0.1186(4) 0.1535(4) 0.6836(2) 0.0135(5) Uani 1 1 d . . . H2 H 0.0502 0.0568 0.6640 0.016 Uiso 1 1 calc R . . C3 C 0.1215(4) 0.0661(4) 0.9010(2) 0.0122(5) Uani 1 1 d . . . C4 C -0.0406(4) -0.0563(4) 0.8851(2) 0.0127(5) Uani 1 1 d . . . H4 H -0.0106 -0.1280 0.8182 0.015 Uiso 1 1 calc R . . C5 C -0.2145(4) 0.0510(4) 0.8637(2) 0.0153(6) Uani 1 1 d . . . H5A H -0.1959 0.1277 0.7920 0.018 Uiso 1 1 calc R . . H5B H -0.3155 -0.0298 0.8549 0.018 Uiso 1 1 calc R . . C6 C -0.2600(4) 0.1636(4) 0.9662(3) 0.0158(6) Uani 1 1 d . . . H6 H -0.3707 0.2337 0.9520 0.019 Uiso 1 1 calc R . . C7 C -0.1029(4) 0.2890(4) 0.9817(3) 0.0159(6) Uani 1 1 d . . . H7A H -0.1334 0.3603 1.0477 0.019 Uiso 1 1 calc R . . H7B H -0.0820 0.3695 0.9120 0.019 Uiso 1 1 calc R . . C8 C 0.0697(4) 0.1815(4) 1.0030(2) 0.0122(5) Uani 1 1 d . . . H8 H 0.1709 0.2639 1.0120 0.015 Uiso 1 1 calc R . . C9 C 0.2946(4) -0.0415(4) 0.9238(2) 0.0143(6) Uani 1 1 d . . . H9A H 0.3276 -0.1119 0.8578 0.017 Uiso 1 1 calc R . . H9B H 0.3955 0.0391 0.9332 0.017 Uiso 1 1 calc R . . O7 O 0.4407(6) 0.4103(6) 0.1235(4) 0.0777(13) Uani 1 1 d . . . H1W H 0.3411 0.4338 0.1628 0.116 Uiso 1 1 d . . . H2W H 0.5102 0.3594 0.1728 0.116 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.00896(14) 0.01077(11) 0.01270(12) -0.00207(10) -0.00073(9) -0.00008(9) Mo2 0.00866(14) 0.01239(12) 0.00948(12) -0.00179(10) -0.00147(9) 0.00050(9) O1 0.0089(10) 0.0142(9) 0.0132(9) -0.0004(8) -0.0016(8) -0.0018(8) O2 0.0104(10) 0.0138(9) 0.0140(9) -0.0012(8) -0.0022(8) 0.0012(8) O3 0.0202(13) 0.0167(10) 0.0263(11) 0.0068(9) -0.0011(10) -0.0001(9) O4 0.0225(13) 0.0263(11) 0.0270(12) -0.0130(10) 0.0001(10) 0.0000(10) O5 0.0181(12) 0.0303(12) 0.0139(9) 0.0025(9) -0.0033(9) 0.0022(10) O6 0.0206(12) 0.0170(10) 0.0252(11) -0.0065(9) -0.0017(10) -0.0006(9) N1 0.0112(12) 0.0145(11) 0.0132(11) -0.0013(9) -0.0016(9) -0.0015(9) N2 0.0125(13) 0.0138(11) 0.0133(11) -0.0013(9) -0.0021(10) 0.0004(9) N3 0.0141(13) 0.0135(11) 0.0106(10) -0.0008(9) -0.0003(9) -0.0006(9) C1 0.0139(15) 0.0167(13) 0.0111(12) -0.0005(11) -0.0006(11) -0.0044(11) C2 0.0137(15) 0.0153(12) 0.0117(12) -0.0025(11) -0.0007(11) -0.0023(11) C3 0.0129(14) 0.0130(12) 0.0101(12) 0.0018(10) 0.0000(11) -0.0018(10) C4 0.0135(15) 0.0148(12) 0.0097(12) 0.0004(11) -0.0004(11) -0.0021(11) C5 0.0127(15) 0.0220(14) 0.0110(12) 0.0017(12) -0.0032(11) -0.0030(12) C6 0.0132(15) 0.0175(13) 0.0163(13) 0.0017(12) -0.0008(11) 0.0034(11) C7 0.0183(16) 0.0131(12) 0.0158(13) 0.0011(11) 0.0008(12) 0.0018(11) C8 0.0148(15) 0.0118(12) 0.0102(12) -0.0014(10) -0.0006(11) -0.0026(11) C9 0.0116(15) 0.0181(13) 0.0129(13) -0.0004(12) 0.0010(11) 0.0012(11) O7 0.064(3) 0.080(3) 0.092(3) -0.026(3) -0.011(2) 0.009(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 O3 1.685(2) . ? Mo1 O4 1.694(2) . ? Mo1 O1 1.9767(19) 2_666 ? Mo1 O2 1.978(2) . ? Mo1 O1 2.248(2) . ? Mo1 N1 2.456(3) . ? Mo2 O6 1.697(2) . ? Mo2 O5 1.710(2) . ? Mo2 O2 1.966(2) 2_566 ? Mo2 O1 1.979(2) . ? Mo2 O2 2.264(2) . ? Mo2 N2 2.347(2) . ? N1 C1 1.318(4) . ? N1 N2 1.378(3) . ? N2 C2 1.302(4) . ? N3 C2 1.346(4) . ? N3 C1 1.365(4) . ? N3 C3 1.501(4) . ? C1 H1 0.9400 . ? C2 H2 0.9400 . ? C3 C9 1.541(4) . ? C3 C4 1.543(4) . ? C3 C8 1.545(4) . ? C4 C5 1.542(4) . ? C4 C8 1.553(4) 2_557 ? C4 H4 0.9900 . ? C5 C6 1.529(4) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 C9 1.526(4) 2_557 ? C6 C7 1.528(4) . ? C6 H6 0.9900 . ? C7 C8 1.535(4) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C8 C4 1.553(4) 2_557 ? C8 H8 0.9900 . ? C9 C6 1.526(4) 2_557 ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? O7 H1W 0.8626 . ? O7 H2W 0.8640 . ? 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 O3 Mo1 O4 104.61(12) . . ? O3 Mo1 O1 100.76(10) . 2_666 ? O4 Mo1 O1 101.83(10) . 2_666 ? O3 Mo1 O2 98.46(10) . . ? O4 Mo1 O2 102.24(10) . . ? O1 Mo1 O2 144.11(8) 2_666 . ? O3 Mo1 O1 96.66(10) . . ? O4 Mo1 O1 158.73(10) . . ? O1 Mo1 O1 73.80(9) 2_666 . ? O2 Mo1 O1 74.08(8) . . ? O3 Mo1 N1 168.28(10) . . ? O4 Mo1 N1 85.98(10) . . ? O1 Mo1 N1 81.59(8) 2_666 . ? O2 Mo1 N1 73.99(8) . . ? O1 Mo1 N1 72.83(8) . . ? O6 Mo2 O5 104.48(11) . . ? O6 Mo2 O2 100.54(10) . 2_566 ? O5 Mo2 O2 100.77(10) . 2_566 ? O6 Mo2 O1 105.32(10) . . ? O5 Mo2 O1 96.95(10) . . ? O2 Mo2 O1 143.72(8) 2_566 . ? O6 Mo2 O2 159.41(9) . . ? O5 Mo2 O2 96.00(10) . . ? O2 Mo2 O2 73.17(9) 2_566 . ? O1 Mo2 O2 73.69(8) . . ? O6 Mo2 N2 86.40(10) . . ? O5 Mo2 N2 168.32(11) . . ? O2 Mo2 N2 81.01(8) 2_566 . ? O1 Mo2 N2 75.74(9) . . ? O2 Mo2 N2 73.34(8) . . ? Mo1 O1 Mo2 140.04(11) 2_666 . ? Mo1 O1 Mo1 106.20(9) 2_666 . ? Mo2 O1 Mo1 105.95(9) . . ? Mo2 O2 Mo1 140.75(11) 2_566 . ? Mo2 O2 Mo2 106.83(9) 2_566 . ? Mo1 O2 Mo2 105.38(8) . . ? C1 N1 N2 106.3(2) . . ? C1 N1 Mo1 140.4(2) . . ? N2 N1 Mo1 112.33(16) . . ? C2 N2 N1 108.2(2) . . ? C2 N2 Mo2 134.0(2) . . ? N1 N2 Mo2 116.93(17) . . ? C2 N3 C1 105.2(2) . . ? C2 N3 C3 127.9(2) . . ? C1 N3 C3 126.8(2) . . ? N1 C1 N3 110.0(2) . . ? N1 C1 H1 125.0 . . ? N3 C1 H1 125.0 . . ? N2 C2 N3 110.3(3) . . ? N2 C2 H2 124.9 . . ? N3 C2 H2 124.9 . . ? N3 C3 C9 106.5(2) . . ? N3 C3 C4 109.6(2) . . ? C9 C3 C4 111.4(2) . . ? N3 C3 C8 110.3(2) . . ? C9 C3 C8 110.6(2) . . ? C4 C3 C8 108.4(2) . . ? C5 C4 C3 111.5(2) . . ? C5 C4 C8 110.3(2) . 2_557 ? C3 C4 C8 107.6(2) . 2_557 ? C5 C4 H4 109.1 . . ? C3 C4 H4 109.1 . . ? C8 C4 H4 109.1 2_557 . ? C6 C5 C4 109.3(2) . . ? C6 C5 H5A 109.8 . . ? C4 C5 H5A 109.8 . . ? C6 C5 H5B 109.8 . . ? C4 C5 H5B 109.8 . . ? H5A C5 H5B 108.3 . . ? C9 C6 C7 109.4(2) 2_557 . ? C9 C6 C5 109.0(2) 2_557 . ? C7 C6 C5 110.4(3) . . ? C9 C6 H6 109.3 2_557 . ? C7 C6 H6 109.3 . . ? C5 C6 H6 109.3 . . ? C6 C7 C8 109.7(2) . . ? C6 C7 H7A 109.7 . . ? C8 C7 H7A 109.7 . . ? C6 C7 H7B 109.7 . . ? C8 C7 H7B 109.7 . . ? H7A C7 H7B 108.2 . . ? C7 C8 C3 111.2(2) . . ? C7 C8 C4 110.4(2) . 2_557 ? C3 C8 C4 107.8(2) . 2_557 ? C7 C8 H8 109.1 . . ? C3 C8 H8 109.1 . . ? C4 C8 H8 109.1 2_557 . ? C6 C9 C3 109.3(2) 2_557 . ? C6 C9 H9A 109.8 2_557 . ? C3 C9 H9A 109.8 . . ? C6 C9 H9B 109.8 2_557 . ? C3 C9 H9B 109.8 . . ? H9A C9 H9B 108.3 . . ? H1W O7 H2W 105.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O6 Mo2 O1 Mo1 -9.33(19) . . . 2_666 ? O5 Mo2 O1 Mo1 -116.46(17) . . . 2_666 ? O2 Mo2 O1 Mo1 124.59(16) 2_566 . . 2_666 ? O2 Mo2 O1 Mo1 149.29(18) . . . 2_666 ? N2 Mo2 O1 Mo1 72.81(17) . . . 2_666 ? O6 Mo2 O1 Mo1 -151.78(10) . . . . ? O5 Mo2 O1 Mo1 101.09(10) . . . . ? O2 Mo2 O1 Mo1 -17.86(16) 2_566 . . . ? O2 Mo2 O1 Mo1 6.84(7) . . . . ? N2 Mo2 O1 Mo1 -69.64(9) . . . . ? O3 Mo1 O1 Mo1 99.31(11) . . . 2_666 ? O4 Mo1 O1 Mo1 -80.9(3) . . . 2_666 ? O1 Mo1 O1 Mo1 0.0 2_666 . . 2_666 ? O2 Mo1 O1 Mo1 -163.76(11) . . . 2_666 ? N1 Mo1 O1 Mo1 -86.01(9) . . . 2_666 ? O3 Mo1 O1 Mo2 -104.75(11) . . . . ? O4 Mo1 O1 Mo2 75.0(3) . . . . ? O1 Mo1 O1 Mo2 155.94(14) 2_666 . . . ? O2 Mo1 O1 Mo2 -7.82(8) . . . . ? N1 Mo1 O1 Mo2 69.94(9) . . . . ? O3 Mo1 O2 Mo2 -114.40(17) . . . 2_566 ? O4 Mo1 O2 Mo2 -7.35(18) . . . 2_566 ? O1 Mo1 O2 Mo2 123.78(16) 2_666 . . 2_566 ? O1 Mo1 O2 Mo2 151.04(18) . . . 2_566 ? N1 Mo1 O2 Mo2 74.78(16) . . . 2_566 ? O3 Mo1 O2 Mo2 101.37(11) . . . . ? O4 Mo1 O2 Mo2 -151.58(11) . . . . ? O1 Mo1 O2 Mo2 -20.46(17) 2_666 . . . ? O1 Mo1 O2 Mo2 6.81(7) . . . . ? N1 Mo1 O2 Mo2 -69.46(9) . . . . ? O6 Mo2 O2 Mo2 -74.8(3) . . . 2_566 ? O5 Mo2 O2 Mo2 99.47(11) . . . 2_566 ? O2 Mo2 O2 Mo2 0.0 2_566 . . 2_566 ? O1 Mo2 O2 Mo2 -165.03(10) . . . 2_566 ? N2 Mo2 O2 Mo2 -85.41(10) . . . 2_566 ? O6 Mo2 O2 Mo1 82.5(3) . . . . ? O5 Mo2 O2 Mo1 -103.26(11) . . . . ? O2 Mo2 O2 Mo1 157.27(14) 2_566 . . . ? O1 Mo2 O2 Mo1 -7.76(8) . . . . ? N2 Mo2 O2 Mo1 71.86(9) . . . . ? O3 Mo1 N1 C1 -174.8(4) . . . . ? O4 Mo1 N1 C1 -19.8(3) . . . . ? O1 Mo1 N1 C1 82.8(3) 2_666 . . . ? O2 Mo1 N1 C1 -123.8(3) . . . . ? O1 Mo1 N1 C1 158.3(3) . . . . ? O3 Mo1 N1 N2 -8.5(6) . . . . ? O4 Mo1 N1 N2 146.46(19) . . . . ? O1 Mo1 N1 N2 -110.94(18) 2_666 . . . ? O2 Mo1 N1 N2 42.49(17) . . . . ? O1 Mo1 N1 N2 -35.39(17) . . . . ? C1 N1 N2 C2 -0.5(3) . . . . ? Mo1 N1 N2 C2 -171.43(18) . . . . ? C1 N1 N2 Mo2 170.29(18) . . . . ? Mo1 N1 N2 Mo2 -0.7(2) . . . . ? O6 Mo2 N2 C2 -43.9(3) . . . . ? O5 Mo2 N2 C2 157.0(4) . . . . ? O2 Mo2 N2 C2 57.3(3) 2_566 . . . ? O1 Mo2 N2 C2 -150.7(3) . . . . ? O2 Mo2 N2 C2 132.3(3) . . . . ? O6 Mo2 N2 N1 148.3(2) . . . . ? O5 Mo2 N2 N1 -10.7(6) . . . . ? O2 Mo2 N2 N1 -110.45(19) 2_566 . . . ? O1 Mo2 N2 N1 41.48(18) . . . . ? O2 Mo2 N2 N1 -35.44(18) . . . . ? N2 N1 C1 N3 -0.1(3) . . . . ? Mo1 N1 C1 N3 166.7(2) . . . . ? C2 N3 C1 N1 0.7(3) . . . . ? C3 N3 C1 N1 178.0(2) . . . . ? N1 N2 C2 N3 0.9(3) . . . . ? Mo2 N2 C2 N3 -167.59(19) . . . . ? C1 N3 C2 N2 -1.0(3) . . . . ? C3 N3 C2 N2 -178.3(3) . . . . ? C2 N3 C3 C9 100.0(3) . . . . ? C1 N3 C3 C9 -76.8(3) . . . . ? C2 N3 C3 C4 -20.7(4) . . . . ? C1 N3 C3 C4 162.5(3) . . . . ? C2 N3 C3 C8 -139.9(3) . . . . ? C1 N3 C3 C8 43.3(4) . . . . ? N3 C3 C4 C5 -63.0(3) . . . . ? C9 C3 C4 C5 179.3(2) . . . . ? C8 C3 C4 C5 57.4(3) . . . . ? N3 C3 C4 C8 175.9(2) . . . 2_557 ? C9 C3 C4 C8 58.3(3) . . . 2_557 ? C8 C3 C4 C8 -63.7(3) . . . 2_557 ? C3 C4 C5 C6 -58.7(3) . . . . ? C8 C4 C5 C6 60.7(3) 2_557 . . . ? C4 C5 C6 C9 -61.3(3) . . . 2_557 ? C4 C5 C6 C7 58.9(3) . . . . ? C9 C6 C7 C8 60.7(3) 2_557 . . . ? C5 C6 C7 C8 -59.3(3) . . . . ? C6 C7 C8 C3 59.0(3) . . . . ? C6 C7 C8 C4 -60.7(3) . . . 2_557 ? N3 C3 C8 C7 62.6(3) . . . . ? C9 C3 C8 C7 -179.8(2) . . . . ? C4 C3 C8 C7 -57.4(3) . . . . ? N3 C3 C8 C4 -176.2(2) . . . 2_557 ? C9 C3 C8 C4 -58.6(3) . . . 2_557 ? C4 C3 C8 C4 63.8(3) . . . 2_557 ? N3 C3 C9 C6 -179.3(2) . . . 2_557 ? C4 C3 C9 C6 -59.8(3) . . . 2_557 ? C8 C3 C9 C6 60.8(3) . . . 2_557 ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 27.55 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.460 _refine_diff_density_min -0.853 _refine_diff_density_rms 0.105 #============================================================================== data_(7) _database_code_depnum_ccdc_archive 'CCDC 752803' #TrackingRef 'Cif_data.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Molybdenum(VI) oxide complex with 5-[4-(1,2,4-triazol-4-yl)phenyl]tetrazole ; _chemical_name_common ;Molybdenum(VI) oxide complex with 5-(4-(1,2,4-triazol-4- yl)phenyl)tetrazole ; _chemical_melting_point ? _chemical_formula_moiety 'C9 H7 Mo N7 O3' _chemical_formula_sum 'C9 H7 Mo N7 O3' _chemical_formula_weight 357.16 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'I 41/a' _space_group_name_Hall '-I 4ad' _symmetry_Int_Tables_number 88 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z' '-y+3/4, x+1/4, z+1/4' 'y+1/4, -x+1/4, z+1/4' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1, z+1/2' '-y+5/4, x+3/4, z+3/4' 'y+3/4, -x+3/4, z+3/4' '-x, -y, -z' 'x, y-1/2, -z' 'y-3/4, -x-1/4, -z-1/4' '-y-1/4, x-1/4, -z-1/4' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y, -z+1/2' 'y-1/4, -x+1/4, -z+1/4' '-y+1/4, x+1/4, -z+1/4' _cell_length_a 19.5123(11) _cell_length_b 19.5123(11) _cell_length_c 11.9438(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4547.4(4) _cell_formula_units_Z 16 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 9884 _cell_measurement_theta_min 2.00 _cell_measurement_theta_max 27.31 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.22 _exptl_crystal_density_diffrn 2.087 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2816 _exptl_absorpt_coefficient_mu 1.176 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.7419 _exptl_absorpt_correction_T_max 0.7819 _exptl_absorpt_process_details 'X-RED (Stoe & Cie, 2001) and X-SHAPE (Stoe & Cie, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe Imaging plate diffraction system' _diffrn_measurement_method '\f oscillation scans' _diffrn_standards_decay_% 0 _diffrn_reflns_number 9884 _diffrn_reflns_av_R_equivalents 0.0585 _diffrn_reflns_av_sigmaI/netI 0.0421 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 27.31 _reflns_number_total 2557 _reflns_number_gt 2206 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS Software (Stoe & Cie, 2000)' _computing_cell_refinement 'IPDS Software (Stoe & Cie, 2000)' _computing_data_reduction 'IPDS Software (Stoe & Cie, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e (Brandenburg, 1999)' _computing_publication_material 'WinGX 1.70.01 (Farrugia, 1999)' #------------------------------- Refinement data-----------------------# _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^)+(0.0453P)^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_number_reflns 2557 _refine_ls_number_parameters 181 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0343 _refine_ls_R_factor_gt 0.0273 _refine_ls_wR_factor_ref 0.0727 _refine_ls_wR_factor_gt 0.0701 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _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 0.324619(10) 0.029920(10) 0.251451(13) 0.01262(9) Uani 1 1 d . . . O1 O 0.32326(9) -0.03178(9) 0.37477(12) 0.0159(3) Uani 1 1 d . . . O2 O 0.34542(9) 0.10559(9) 0.31728(12) 0.0188(4) Uani 1 1 d . . . O3 O 0.39842(9) 0.00155(10) 0.19044(12) 0.0198(4) Uani 1 1 d . . . N1 N 0.21256(10) 0.03604(10) 0.32753(14) 0.0154(4) Uani 1 1 d . . . N2 N 0.19274(10) -0.00792(11) 0.41308(15) 0.0160(4) Uani 1 1 d . . . N3 N 0.10912(10) 0.06412(10) 0.38044(14) 0.0149(4) Uani 1 1 d . . . N4 N -0.14657(11) 0.26808(12) 0.48929(15) 0.0208(4) Uani 1 1 d . . . N5 N -0.20750(12) 0.29672(12) 0.46055(17) 0.0233(5) Uani 1 1 d . . . N6 N -0.22950(12) 0.27148(12) 0.36591(17) 0.0234(5) Uani 1 1 d . . . N7 N -0.18183(11) 0.22608(11) 0.33279(16) 0.0201(4) Uani 1 1 d . . . H1N H -0.1835 0.2019 0.2717 0.030 Uiso 1 1 calc R . . C1 C 0.13089(13) 0.00996(12) 0.44301(16) 0.0162(5) Uani 1 1 d . . . H1 H 0.1051 -0.0114 0.4996 0.019 Uiso 1 1 calc R . . C2 C 0.16196(12) 0.07795(12) 0.30988(16) 0.0155(4) Uani 1 1 d . . . H2 H 0.1619 0.1130 0.2558 0.019 Uiso 1 1 calc R . . C3 C 0.04662(12) 0.10155(12) 0.38769(18) 0.0163(5) Uani 1 1 d . . . C4 C 0.01575(13) 0.11112(14) 0.49130(17) 0.0187(5) Uani 1 1 d . . . H4 H 0.0342 0.0908 0.5560 0.022 Uiso 1 1 calc R . . C5 C -0.04293(13) 0.15120(14) 0.49760(18) 0.0193(5) Uani 1 1 d . . . H5 H -0.0644 0.1581 0.5671 0.023 Uiso 1 1 calc R . . C6 C -0.07021(12) 0.18127(13) 0.40139(18) 0.0173(5) Uani 1 1 d . . . C7 C -0.03816(13) 0.17019(13) 0.29799(17) 0.0178(5) Uani 1 1 d . . . H7 H -0.0562 0.1905 0.2330 0.021 Uiso 1 1 calc R . . C8 C 0.01962(13) 0.12978(13) 0.29054(18) 0.0175(5) Uani 1 1 d . . . H8 H 0.0404 0.1215 0.2208 0.021 Uiso 1 1 calc R . . C9 C -0.13137(13) 0.22402(13) 0.40896(18) 0.0172(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.01401(12) 0.01588(12) 0.00795(11) 0.00033(6) 0.00003(6) -0.00055(7) O1 0.0151(8) 0.0208(9) 0.0118(6) 0.0019(6) 0.0009(6) 0.0026(6) O2 0.0233(9) 0.0215(9) 0.0117(7) 0.0003(6) -0.0015(6) -0.0035(7) O3 0.0199(9) 0.0269(10) 0.0126(7) 0.0015(6) 0.0011(6) 0.0023(7) N1 0.0197(10) 0.0168(10) 0.0096(7) 0.0007(7) 0.0014(7) -0.0003(8) N2 0.0186(10) 0.0185(10) 0.0107(8) 0.0028(7) 0.0005(7) -0.0016(8) N3 0.0153(10) 0.0197(10) 0.0097(7) -0.0019(7) -0.0013(7) 0.0018(7) N4 0.0218(11) 0.0232(12) 0.0174(9) -0.0017(8) 0.0014(8) 0.0014(9) N5 0.0269(12) 0.0240(12) 0.0191(9) -0.0005(8) 0.0030(8) 0.0057(9) N6 0.0229(11) 0.0260(12) 0.0214(9) 0.0013(8) 0.0006(8) 0.0077(9) N7 0.0208(11) 0.0222(11) 0.0173(9) -0.0025(8) -0.0029(8) 0.0040(8) C1 0.0173(12) 0.0199(12) 0.0113(9) 0.0015(8) 0.0000(8) -0.0011(9) C2 0.0189(12) 0.0187(12) 0.0089(8) 0.0003(8) 0.0007(8) 0.0021(9) C3 0.0153(11) 0.0187(12) 0.0148(9) -0.0029(8) -0.0012(8) 0.0008(8) C4 0.0194(12) 0.0245(13) 0.0123(9) 0.0011(8) -0.0008(8) 0.0030(9) C5 0.0196(12) 0.0260(13) 0.0122(9) -0.0009(8) 0.0018(8) 0.0025(9) C6 0.0157(11) 0.0195(12) 0.0166(10) -0.0014(9) 0.0003(8) -0.0005(9) C7 0.0205(12) 0.0202(12) 0.0128(9) 0.0008(8) -0.0030(8) -0.0003(9) C8 0.0180(12) 0.0238(13) 0.0108(9) -0.0012(8) 0.0004(8) 0.0009(9) C9 0.0191(12) 0.0174(12) 0.0151(9) 0.0033(8) 0.0009(8) 0.0006(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 O3 1.7062(17) . ? Mo1 O2 1.7213(17) . ? Mo1 O1 1.9025(16) . ? Mo1 O1 1.9243(16) 7_444 ? Mo1 N1 2.371(2) . ? Mo1 N2 2.388(2) 7_444 ? O1 Mo1 1.9243(15) 4 ? N1 C2 1.299(3) . ? N1 N2 1.389(3) . ? N2 C1 1.306(3) . ? N2 Mo1 2.388(2) 4 ? N3 C2 1.359(3) . ? N3 C1 1.362(3) . ? N3 C3 1.424(3) . ? N4 C9 1.322(3) . ? N4 N5 1.358(3) . ? N5 N6 1.306(3) . ? N6 N7 1.344(3) . ? N7 C9 1.341(3) . ? N7 H1N 0.8700 . ? C1 H1 0.9400 . ? C2 H2 0.9400 . ? C3 C8 1.388(3) . ? C3 C4 1.389(3) . ? C4 C5 1.389(4) . ? C4 H4 0.9400 . ? C5 C6 1.396(3) . ? C5 H5 0.9400 . ? C6 C7 1.401(3) . ? C6 C9 1.459(3) . ? C7 C8 1.379(3) . ? C7 H7 0.9400 . ? C8 H8 0.9400 . ? 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 O3 Mo1 O2 105.92(9) . . ? O3 Mo1 O1 97.88(8) . . ? O2 Mo1 O1 101.10(7) . . ? O3 Mo1 O1 99.98(7) . 7_444 ? O2 Mo1 O1 94.85(7) . 7_444 ? O1 Mo1 O1 151.73(8) . 7_444 ? O3 Mo1 N1 163.42(8) . . ? O2 Mo1 N1 89.96(8) . . ? O1 Mo1 N1 73.87(7) . . ? O1 Mo1 N1 83.03(7) 7_444 . ? O3 Mo1 N2 92.30(8) . 7_444 ? O2 Mo1 N2 160.31(8) . 7_444 ? O1 Mo1 N2 83.33(7) . 7_444 ? O1 Mo1 N2 74.26(7) 7_444 7_444 ? N1 Mo1 N2 72.70(7) . 7_444 ? Mo1 O1 Mo1 152.84(10) . 4 ? C2 N1 N2 107.25(19) . . ? C2 N1 Mo1 132.09(16) . . ? N2 N1 Mo1 120.51(14) . . ? C1 N2 N1 107.08(18) . . ? C1 N2 Mo1 133.06(14) . 4 ? N1 N2 Mo1 117.61(14) . 4 ? C2 N3 C1 104.9(2) . . ? C2 N3 C3 125.8(2) . . ? C1 N3 C3 129.2(2) . . ? C9 N4 N5 106.30(19) . . ? N6 N5 N4 110.6(2) . . ? N5 N6 N7 106.0(2) . . ? C9 N7 N6 109.2(2) . . ? C9 N7 H1N 125.4 . . ? N6 N7 H1N 125.4 . . ? N2 C1 N3 110.20(19) . . ? N2 C1 H1 124.9 . . ? N3 C1 H1 124.9 . . ? N1 C2 N3 110.5(2) . . ? N1 C2 H2 124.7 . . ? N3 C2 H2 124.7 . . ? C8 C3 C4 121.8(2) . . ? C8 C3 N3 118.53(19) . . ? C4 C3 N3 119.6(2) . . ? C5 C4 C3 118.8(2) . . ? C5 C4 H4 120.6 . . ? C3 C4 H4 120.6 . . ? C4 C5 C6 120.4(2) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C5 C6 C7 119.4(2) . . ? C5 C6 C9 120.1(2) . . ? C7 C6 C9 120.5(2) . . ? C8 C7 C6 120.7(2) . . ? C8 C7 H7 119.7 . . ? C6 C7 H7 119.7 . . ? C7 C8 C3 118.9(2) . . ? C7 C8 H8 120.6 . . ? C3 C8 H8 120.6 . . ? N4 C9 N7 107.9(2) . . ? N4 C9 C6 126.9(2) . . ? N7 C9 C6 125.1(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Mo1 O1 Mo1 -168.9(2) . . . 4 ? O2 Mo1 O1 Mo1 83.1(2) . . . 4 ? O1 Mo1 O1 Mo1 -40.1(4) 7_444 . . 4 ? N1 Mo1 O1 Mo1 -3.64(19) . . . 4 ? N2 Mo1 O1 Mo1 -77.5(2) 7_444 . . 4 ? O3 Mo1 N1 C2 -129.2(3) . . . . ? O2 Mo1 N1 C2 67.3(2) . . . . ? O1 Mo1 N1 C2 168.9(2) . . . . ? O1 Mo1 N1 C2 -27.6(2) 7_444 . . . ? N2 Mo1 N1 C2 -103.2(2) 7_444 . . . ? O3 Mo1 N1 N2 55.9(3) . . . . ? O2 Mo1 N1 N2 -107.55(16) . . . . ? O1 Mo1 N1 N2 -5.98(15) . . . . ? O1 Mo1 N1 N2 157.56(17) 7_444 . . . ? N2 Mo1 N1 N2 81.93(16) 7_444 . . . ? C2 N1 N2 C1 -0.2(3) . . . . ? Mo1 N1 N2 C1 175.85(14) . . . . ? C2 N1 N2 Mo1 -165.35(15) . . . 4 ? Mo1 N1 N2 Mo1 10.7(2) . . . 4 ? C9 N4 N5 N6 0.0(3) . . . . ? N4 N5 N6 N7 -0.3(3) . . . . ? N5 N6 N7 C9 0.5(3) . . . . ? N1 N2 C1 N3 0.0(3) . . . . ? Mo1 N2 C1 N3 161.92(16) 4 . . . ? C2 N3 C1 N2 0.2(2) . . . . ? C3 N3 C1 N2 -177.2(2) . . . . ? N2 N1 C2 N3 0.3(3) . . . . ? Mo1 N1 C2 N3 -175.09(14) . . . . ? C1 N3 C2 N1 -0.3(2) . . . . ? C3 N3 C2 N1 177.2(2) . . . . ? C2 N3 C3 C8 34.2(3) . . . . ? C1 N3 C3 C8 -148.9(2) . . . . ? C2 N3 C3 C4 -143.4(2) . . . . ? C1 N3 C3 C4 33.6(4) . . . . ? C8 C3 C4 C5 -1.3(4) . . . . ? N3 C3 C4 C5 176.2(2) . . . . ? C3 C4 C5 C6 0.0(4) . . . . ? C4 C5 C6 C7 0.5(4) . . . . ? C4 C5 C6 C9 -179.2(2) . . . . ? C5 C6 C7 C8 0.3(4) . . . . ? C9 C6 C7 C8 -180.0(2) . . . . ? C6 C7 C8 C3 -1.6(4) . . . . ? C4 C3 C8 C7 2.1(4) . . . . ? N3 C3 C8 C7 -175.4(2) . . . . ? N5 N4 C9 N7 0.3(3) . . . . ? N5 N4 C9 C6 179.1(2) . . . . ? N6 N7 C9 N4 -0.5(3) . . . . ? N6 N7 C9 C6 -179.3(2) . . . . ? C5 C6 C9 N4 38.8(4) . . . . ? C7 C6 C9 N4 -141.0(3) . . . . ? C5 C6 C9 N7 -142.6(3) . . . . ? C7 C6 C9 N7 37.6(4) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.31 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.446 _refine_diff_density_min -1.571 _refine_diff_density_rms 0.098 # ------------- END of CIF -----------------#