# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry, 1999 # CCDC Number: 186/1532 data_moga _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H15 Mo N4 O8.50' _chemical_formula_weight 351.14 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mo' 'Mo' -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 2(1) /n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.0100(2) _cell_length_b 13.7821(3) _cell_length_c 12.6683(2) _cell_angle_alpha 90.00 _cell_angle_beta 105.3000(10) _cell_angle_gamma 90.00 _cell_volume 1180.54(5) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 4802 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 25.00 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.976 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 708 _exptl_absorpt_coefficient_mu 1.155 _exptl_absorpt_correction_type multi-scans _exptl_absorpt_correction_T_min 0.7588 _exptl_absorpt_correction_T_max 0.8710 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Siemens SMART CCD area-detector diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 5951 _diffrn_reflns_av_R_equivalents 0.0438 _diffrn_reflns_av_sigmaI/netI 0.0503 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2062 _reflns_number_gt 1714 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0545P)^2^+7.4805P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2062 _refine_ls_number_parameters 164 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0629 _refine_ls_R_factor_gt 0.0510 _refine_ls_wR_factor_ref 0.1302 _refine_ls_wR_factor_gt 0.1256 _refine_ls_goodness_of_fit_ref 1.105 _refine_ls_restrained_S_all 1.105 _refine_ls_shift/su_max 0.035 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.70273(9) 0.72051(4) 0.43776(4) 0.0155(2) Uani 1 1 d . . . N1 N 0.7199(8) 0.5042(4) 0.4485(4) 0.0202(12) Uani 1 1 d . . . H1A H 0.7053 0.4431 0.4281 0.024 Uiso 1 1 calc R . . N2 N 0.7476(9) 0.4618(4) 0.7126(5) 0.0223(13) Uani 1 1 d D . . H2C H 0.642(8) 0.446(6) 0.687(6) 0.027 Uiso 1 1 d D . . H2D H 0.751(12) 0.509(4) 0.744(6) 0.027 Uiso 1 1 d D . . N3 N 0.5904(9) 0.8370(4) 0.6086(5) 0.0262(14) Uani 1 1 d . . . H3A H 0.5962 0.8809 0.6598 0.031 Uiso 1 1 calc R . . N4 N 0.2718(13) 0.6711(5) 0.6785(6) 0.0391(19) Uani 1 1 d D . . H4C H 0.345(13) 0.661(8) 0.736(6) 0.047 Uiso 1 1 d D . . H4D H 0.240(14) 0.636(6) 0.628(6) 0.047 Uiso 1 1 d D . . O1 O 0.6555(7) 0.5853(3) 0.3789(3) 0.0191(10) Uani 1 1 d . . . O2 O 0.8270(7) 0.6255(3) 0.5715(3) 0.0225(11) Uani 1 1 d . . . O3 O 0.7283(7) 0.8284(3) 0.5440(4) 0.0228(11) Uani 1 1 d . . . O4 O 0.4551(7) 0.7071(3) 0.5064(4) 0.0198(10) Uani 1 1 d . . . O5 O 0.9282(7) 0.7523(4) 0.4215(4) 0.0238(11) Uani 1 1 d . . . O6 O 0.5433(7) 0.7578(3) 0.3168(4) 0.0236(11) Uani 1 1 d . . . C1 C 0.8020(10) 0.5338(5) 0.5453(5) 0.0188(14) Uani 1 1 d . . . C2 C 0.8727(11) 0.4586(5) 0.6337(6) 0.0251(16) Uani 1 1 d . . . H2A H 0.8649 0.3933 0.6003 0.030 Uiso 1 1 calc R . . H2B H 1.0124 0.4714 0.6729 0.030 Uiso 1 1 calc R . . C3 C 0.4553(10) 0.7706(4) 0.5809(5) 0.0178(14) Uani 1 1 d . . . C4 C 0.2948(11) 0.7694(5) 0.6393(5) 0.0232(15) Uani 1 1 d . . . H4A H 0.3286 0.8148 0.7020 0.028 Uiso 1 1 calc R . . H4B H 0.1687 0.7909 0.5888 0.028 Uiso 1 1 calc R . . O1S O 0.1915(8) 0.8584(4) 0.3057(5) 0.0391(14) Uiso 1 1 d . . . O2S O 0.1089(16) 0.9918(8) 0.4637(9) 0.036(3) Uiso 0.50 1 d P . . O3S O 0.1877(19) 0.5136(10) 0.8998(11) 0.050(3) Uiso 0.50 1 d P A 1 O4S O 0.312(2) 0.5157(11) 0.8111(11) 0.060(4) Uiso 0.50 1 d P B 2 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 0.0237(3) 0.0129(3) 0.0104(3) 0.0015(2) 0.0055(2) 0.0007(3) N1 0.029(3) 0.010(3) 0.023(3) 0.001(2) 0.009(3) 0.002(2) N2 0.027(3) 0.021(3) 0.018(3) 0.001(2) 0.003(3) -0.004(3) N3 0.039(4) 0.026(3) 0.019(3) -0.011(3) 0.016(3) -0.008(3) N4 0.067(6) 0.026(4) 0.036(4) -0.013(3) 0.035(4) -0.014(4) O1 0.026(3) 0.015(2) 0.014(2) -0.0014(18) 0.0025(19) -0.001(2) O2 0.037(3) 0.016(2) 0.013(2) 0.0017(19) 0.004(2) 0.002(2) O3 0.035(3) 0.017(2) 0.020(2) -0.008(2) 0.014(2) -0.012(2) O4 0.025(3) 0.020(2) 0.015(2) -0.0075(19) 0.0082(19) -0.005(2) O5 0.025(3) 0.027(3) 0.019(2) 0.000(2) 0.006(2) -0.002(2) O6 0.033(3) 0.024(3) 0.015(2) 0.0068(19) 0.009(2) 0.006(2) C1 0.022(3) 0.017(3) 0.019(3) 0.005(3) 0.007(3) 0.003(3) C2 0.029(4) 0.021(4) 0.027(4) 0.012(3) 0.010(3) 0.008(3) C3 0.029(4) 0.014(3) 0.011(3) 0.001(3) 0.004(3) 0.003(3) C4 0.031(4) 0.024(4) 0.014(3) 0.000(3) 0.005(3) 0.001(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 O5 1.704(5) . ? Mo1 O6 1.720(5) . ? Mo1 O3 1.982(4) . ? Mo1 O1 2.002(4) . ? Mo1 O2 2.137(4) . ? Mo1 O4 2.145(4) . ? N1 C1 1.276(8) . ? N1 O1 1.421(7) . ? N2 C2 1.495(9) . ? N3 C3 1.296(9) . ? N3 O3 1.427(7) . ? N4 C4 1.466(10) . ? O2 C1 1.306(8) . ? O4 C3 1.288(8) . ? C1 C2 1.510(9) . ? C3 C4 1.500(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Mo1 O6 102.8(2) . . ? O5 Mo1 O3 88.2(2) . . ? O6 Mo1 O3 107.6(2) . . ? O5 Mo1 O1 105.2(2) . . ? O6 Mo1 O1 86.7(2) . . ? O3 Mo1 O1 158.09(18) . . ? O5 Mo1 O2 93.2(2) . . ? O6 Mo1 O2 157.3(2) . . ? O3 Mo1 O2 88.66(19) . . ? O1 Mo1 O2 73.58(17) . . ? O5 Mo1 O4 161.2(2) . . ? O6 Mo1 O4 88.9(2) . . ? O3 Mo1 O4 74.19(18) . . ? O1 Mo1 O4 89.90(18) . . ? O2 Mo1 O4 80.20(18) . . ? C1 N1 O1 109.5(5) . . ? C3 N3 O3 110.1(5) . . ? N1 O1 Mo1 120.4(3) . . ? C1 O2 Mo1 113.1(4) . . ? N3 O3 Mo1 119.8(4) . . ? C3 O4 Mo1 113.2(4) . . ? N1 C1 O2 123.4(6) . . ? N1 C1 C2 118.0(6) . . ? O2 C1 C2 118.6(6) . . ? N2 C2 C1 109.9(6) . . ? O4 C3 N3 122.5(6) . . ? O4 C3 C4 119.8(6) . . ? N3 C3 C4 117.7(6) . . ? N4 C4 C3 110.0(6) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.442 _refine_diff_density_min -1.375 _refine_diff_density_rms 0.154