Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _publ_contact_author_email CZLU@MS.FJIRSM.AC.CN _publ_contact_author_name 'Prof Can-Zhong Lu' _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name 'Can-Zhong Lu' 'Hong-Wei Ma' 'Chuan-De Wu' 'Wenbin Yang' ; Xiao-Ping Zhan ; 'Quanzheng Zhang' data_b3 _database_code_CSD 201691 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H30 Mo8 N O30.50 S4' _chemical_formula_weight 1476.05 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M P4/nnc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y+1/2, x, z' 'y, -x+1/2, z' '-x+1/2, y, -z+1/2' 'x, -y+1/2, -z+1/2' 'y, x, -z+1/2' '-y+1/2, -x+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y-1/2, -x, -z' '-y, x-1/2, -z' 'x-1/2, -y, z-1/2' '-x, y-1/2, z-1/2' '-y, -x, z-1/2' 'y-1/2, x-1/2, z-1/2' _cell_length_a 14.8640(7) _cell_length_b 14.8640(7) _cell_length_c 21.4507(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4739.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.29 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.069 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2820 _exptl_absorpt_coefficient_mu 2.296 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.798613 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens Smart CCD' _diffrn_measurement_method omega-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10576 _diffrn_reflns_av_R_equivalents 0.0696 _diffrn_reflns_av_sigmaI/netI 0.0414 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 25.05 _reflns_number_total 2105 _reflns_number_gt 1490 _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^)+(0.2500P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00042(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2105 _refine_ls_number_parameters 113 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1011 _refine_ls_R_factor_gt 0.0659 _refine_ls_wR_factor_ref 0.3075 _refine_ls_wR_factor_gt 0.2534 _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_restrained_S_all 0.999 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.43690(3) -0.56777(3) 0.371456(19) 0.03926(14) Uani 1 1 d . . . Mo2 Mo 0.27380(3) -0.49082(3) 0.371551(18) 0.03983(14) Uani 1 1 d . . . O1 O 0.3463(2) -0.5509(2) 0.30815(15) 0.0436(10) Uani 1 1 d . . . O2 O 0.2971(3) -0.3824(3) 0.36239(17) 0.0568(12) Uani 1 1 d . . . O3 O 0.5083(3) -0.4823(3) 0.36202(16) 0.0582(13) Uani 1 1 d . . . O4 O 0.2107(3) -0.6403(2) 0.38156(15) 0.0492(12) Uani 1 1 d . . . O5 O 0.4936(2) -0.6621(2) 0.31198(15) 0.0382(9) Uani 1 1 d . . . O6 O 0.1551(2) -0.4854(2) 0.42473(15) 0.0421(10) Uani 1 1 d . . . S1 S 0.35685(10) -0.52825(10) 0.46002(6) 0.0539(4) Uani 1 1 d . . . C1 C 0.2039(5) -0.7256(7) 0.3814(3) 0.026(2) Uani 0.50 1 d P . . O1W O 0.1715(3) -0.5108(3) 0.54860(19) 0.0852(17) Uani 1 1 d . . . O2W O 0.2500 -0.7500 0.2500 0.078(4) Uani 1 8 d S . . N1 N 0.2500 -0.4528(16) 0.7500 0.136(8) Uiso 0.50 2 d SP . . H1A H 0.2488 -0.4105 0.7829 0.163 Uiso 0.50 1 d P . . C2 C 0.1621(10) -0.4662(11) 0.7480(8) 0.108(6) Uiso 0.50 1 d P . . H2A H 0.1317 -0.4093 0.7476 0.161 Uiso 0.50 1 calc PR . . H2B H 0.1438 -0.5000 0.7840 0.161 Uiso 0.50 1 calc PR . . H2C H 0.1471 -0.4992 0.7109 0.161 Uiso 0.50 1 calc PR . . O3W O 0.2892(7) -0.3763(7) 0.5809(5) 0.097(3) Uiso 0.50 1 d P . . 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 0.0348(2) 0.0397(3) 0.0433(3) -0.00791(18) 0.00211(18) -0.00143(18) Mo2 0.0388(3) 0.0371(2) 0.0435(2) -0.00439(18) 0.00592(18) 0.00215(19) O1 0.0426(18) 0.0477(18) 0.0404(17) -0.0100(15) 0.0014(15) 0.0034(16) O2 0.055(2) 0.047(2) 0.069(2) -0.0141(18) 0.0074(19) -0.0122(19) O3 0.055(2) 0.053(2) 0.066(2) -0.0075(19) 0.0017(19) -0.013(2) O4 0.081(3) 0.0313(18) 0.0349(17) 0.0034(13) 0.0068(16) 0.0170(18) O5 0.0369(17) 0.0367(17) 0.0411(16) -0.0118(14) 0.0024(14) -0.0004(13) O6 0.0409(17) 0.0354(17) 0.0498(19) -0.0119(14) 0.0084(15) 0.0067(14) S1 0.0500(7) 0.0677(9) 0.0439(7) -0.0103(6) 0.0016(6) 0.0120(7) C1 0.017(4) 0.043(5) 0.019(3) -0.007(4) -0.003(3) -0.013(4) O1W 0.058(3) 0.138(4) 0.060(2) -0.023(3) 0.012(2) 0.001(3) O2W 0.092(5) 0.092(5) 0.050(7) 0.000 0.000 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 1.668(4) . ? Mo1 O1 1.929(3) . ? Mo1 O5 2.075(3) . ? Mo1 O6 2.080(3) 4_645 ? Mo1 S1 2.3174(14) . ? Mo1 O4 2.424(4) 4_645 ? Mo1 Mo2 2.6806(7) . ? Mo2 O2 1.660(4) . ? Mo2 O1 1.951(3) . ? Mo2 O6 2.102(3) . ? Mo2 O5 2.108(3) 3_445 ? Mo2 S1 2.3313(15) . ? Mo2 O4 2.421(4) . ? O4 C1 1.272(10) . ? O4 C1 1.339(10) 4_645 ? O4 Mo1 2.424(4) 3_445 ? O5 Mo2 2.108(3) 4_645 ? O6 Mo1 2.080(3) 3_445 ? C1 C1 1.096(12) 4_645 ? C1 C1 1.096(12) 3_445 ? C1 O4 1.339(10) 3_445 ? C1 C1 1.550(17) 2_535 ? N1 C2 1.322(15) 5_556 ? N1 C2 1.322(15) . ? 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 O1 105.05(17) . . ? O3 Mo1 O5 100.47(16) . . ? O1 Mo1 O5 86.49(13) . . ? O3 Mo1 O6 100.89(16) . 4_645 ? O1 Mo1 O6 148.84(14) . 4_645 ? O5 Mo1 O6 71.96(13) . 4_645 ? O3 Mo1 S1 103.48(13) . . ? O1 Mo1 S1 100.70(10) . . ? O5 Mo1 S1 152.14(10) . . ? O6 Mo1 S1 89.60(10) 4_645 . ? O3 Mo1 O4 168.41(17) . 4_645 ? O1 Mo1 O4 81.19(13) . 4_645 ? O5 Mo1 O4 69.81(12) . 4_645 ? O6 Mo1 O4 70.51(12) 4_645 4_645 ? S1 Mo1 O4 84.60(9) . 4_645 ? O3 Mo1 Mo2 104.51(15) . . ? O1 Mo1 Mo2 46.66(10) . . ? O5 Mo1 Mo2 131.02(9) . . ? O6 Mo1 Mo2 140.19(9) 4_645 . ? S1 Mo1 Mo2 55.03(4) . . ? O4 Mo1 Mo2 86.90(9) 4_645 . ? O2 Mo2 O1 104.26(17) . . ? O2 Mo2 O6 101.66(16) . . ? O1 Mo2 O6 149.22(13) . . ? O2 Mo2 O5 101.49(16) . 3_445 ? O1 Mo2 O5 87.84(13) . 3_445 ? O6 Mo2 O5 70.88(13) . 3_445 ? O2 Mo2 S1 102.56(14) . . ? O1 Mo2 S1 99.54(10) . . ? O6 Mo2 S1 90.67(10) . . ? O5 Mo2 S1 152.18(9) 3_445 . ? O2 Mo2 O4 169.17(18) . . ? O1 Mo2 O4 81.72(13) . . ? O6 Mo2 O4 70.24(12) . . ? O5 Mo2 O4 69.39(12) 3_445 . ? S1 Mo2 O4 85.06(9) . . ? O2 Mo2 Mo1 103.03(15) . . ? O1 Mo2 Mo1 45.95(10) . . ? O6 Mo2 Mo1 140.86(9) . . ? O5 Mo2 Mo1 131.68(9) 3_445 . ? S1 Mo2 Mo1 54.54(4) . . ? O4 Mo2 Mo1 87.64(10) . . ? Mo1 O1 Mo2 87.39(13) . . ? C1 O4 C1 49.6(7) . 4_645 ? C1 O4 Mo2 161.0(5) . . ? C1 O4 Mo2 112.0(4) 4_645 . ? C1 O4 Mo1 113.7(4) . 3_445 ? C1 O4 Mo1 162.6(4) 4_645 3_445 ? Mo2 O4 Mo1 84.11(11) . 3_445 ? Mo1 O5 Mo2 101.78(14) . 4_645 ? Mo1 O6 Mo2 101.80(14) 3_445 . ? Mo1 S1 Mo2 70.43(4) . . ? C1 C1 C1 90.000(1) 4_645 3_445 ? C1 C1 O4 68.4(9) 4_645 . ? C1 C1 O4 158.4(9) 3_445 . ? C1 C1 O4 152.0(9) 4_645 3_445 ? C1 C1 O4 62.0(9) 3_445 3_445 ? O4 C1 O4 139.6(7) . 3_445 ? C1 C1 C1 45.000(3) 4_645 2_535 ? C1 C1 C1 45.000(1) 3_445 2_535 ? O4 C1 C1 113.4(9) . 2_535 ? O4 C1 C1 107.0(9) 3_445 2_535 ? C2 N1 C2 163(3) 5_556 . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.620 _refine_diff_density_min -0.969 _refine_diff_density_rms 0.310