  
data_tak2 
  
_audit_creation_method            SHELXTL 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C23 H30 Mo O5 S' 
_chemical_formula_weight          514.47 
  
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'C'  'C'   0.0033   0.0016 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'H'  'H'   0.0000   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'O'  'O'   0.0106   0.0060 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'S'  'S'   0.1246   0.1234 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Mo'  'Mo'  -1.6832   0.6857 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
  
_symmetry_cell_setting            Monoclinic 
_symmetry_space_group_name_H-M    P2(1)/n 
  
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x+1/2, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x-1/2, -y-1/2, z-1/2' 
  
_cell_length_a                    17.207(2) 
_cell_length_b                    7.7689(11) 
_cell_length_c                    17.786(3) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  110.320(3) 
_cell_angle_gamma                 90.00 
_cell_volume                      2229.7(5) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     153(2) 
_cell_measurement_reflns_used     4721 
_cell_measurement_theta_min       2.53 
_cell_measurement_theta_max       28.09 
  
_exptl_crystal_description        Plate 
_exptl_crystal_colour             Green/Yellow 
_exptl_crystal_size_max           0.32 
_exptl_crystal_size_mid           0.12 
_exptl_crystal_size_min           0.03 
_exptl_crystal_density_meas       0 
_exptl_crystal_density_diffrn     1.533 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1064 
_exptl_absorpt_coefficient_mu     0.714 
_exptl_absorpt_correction_type    'multi-scan' 
_exptl_absorpt_correction_T_min   0.577 
_exptl_absorpt_correction_T_max   1.000 
_exptl_absorpt_process_details    SADABS 
  
_exptl_special_details 
; 
 ? 
; 
  
_diffrn_ambient_temperature       153(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   'CCD area detector' 
_diffrn_measurement_method        'phi and omega scans' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             13693 
_diffrn_reflns_av_R_equivalents   0.0409 
_diffrn_reflns_av_sigmaI/netI     0.0496 
_diffrn_reflns_limit_h_min        -19 
_diffrn_reflns_limit_h_max        21 
_diffrn_reflns_limit_k_min        -10 
_diffrn_reflns_limit_k_max        10 
_diffrn_reflns_limit_l_min        -23 
_diffrn_reflns_limit_l_max        18 
_diffrn_reflns_theta_min          1.42 
_diffrn_reflns_theta_max          28.19 
_reflns_number_total              5118 
_reflns_number_gt                 4402 
_reflns_threshold_expression      >2sigma(I) 
  
_computing_data_collection        'Bruker SMART' 
_computing_cell_refinement        'Bruker SMART' 
_computing_data_reduction         'Bruker SAINT' 
_computing_structure_solution     'Bruker SHELXTL' 
_computing_structure_refinement   'Bruker SHELXTL' 
_computing_molecular_graphics     'Bruker SHELXTL' 
_computing_publication_material   'Bruker SHELXTL' 
  
_refine_special_details 
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0736P)²+1.5088P] where P=(Fo²+2Fc²)/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          5118 
_refine_ls_number_parameters      283 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0599 
_refine_ls_R_factor_gt            0.0499 
_refine_ls_wR_factor_ref          0.1282 
_refine_ls_wR_factor_gt           0.1218 
_refine_ls_goodness_of_fit_ref    1.084 
_refine_ls_restrained_S_all       1.084 
_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 0.915250(18) 0.43332(3) 0.025959(16) 0.01165(11) Uani 1 1 d . . . 
S1 S 0.13292(6) 0.86852(11) 0.29502(5) 0.0193(2) Uani 1 1 d . . . 
O1 O 1.04465(16) 0.4542(3) 0.06184(16) 0.0155(5) Uani 1 1 d . . . 
O2 O 0.1368(2) 0.1994(4) 0.1484(2) 0.0332(7) Uani 1 1 d . . . 
O3 O 0.06919(18) 0.9444(3) 0.22531(17) 0.0260(6) Uani 1 1 d . . . 
O4 O 0.20269(18) 0.8039(4) 0.27461(18) 0.0303(7) Uani 1 1 d . . . 
O5 O 0.15599(19) 0.9811(4) 0.36443(17) 0.0286(6) Uani 1 1 d . . . 
C1 C 0.8048(2) 0.2420(4) -0.0393(2) 0.0174(7) Uani 1 1 d . . . 
H1A H 0.7455 0.2756 -0.0667 0.021 Uiso 1 1 calc R . . 
C2 C 0.8641(2) 0.2228(4) -0.0766(2) 0.0185(7) Uani 1 1 d . . . 
H2A H 0.8544 0.2399 -0.1349 0.022 Uiso 1 1 calc R . . 
C3 C 0.9393(2) 0.1695(4) -0.0178(2) 0.0180(7) Uani 1 1 d . . . 
H3A H 0.9906 0.1356 -0.0284 0.022 Uiso 1 1 calc R . . 
C4 C 0.9266(2) 0.1505(4) 0.0580(2) 0.0177(7) Uani 1 1 d . . . 
H4A H 0.9664 0.0981 0.1080 0.021 Uiso 1 1 calc R . . 
C5 C 0.8422(2) 0.1945(4) 0.0441(2) 0.0142(7) Uani 1 1 d . . . 
C6 C 0.7997(2) 0.1855(4) 0.1059(2) 0.0170(7) Uani 1 1 d . . . 
C7 C 0.7676(2) 0.3748(5) 0.1128(2) 0.0180(7) Uani 1 1 d . . . 
C8 C 0.8273(2) 0.4981(4) 0.0941(2) 0.0176(7) Uani 1 1 d . . . 
C9 C 0.9104(2) 0.5361(5) 0.1445(2) 0.0179(7) Uani 1 1 d . . . 
H9A H 0.9398 0.4860 0.1988 0.022 Uiso 1 1 calc R . . 
C10 C 0.9383(2) 0.6776(4) 0.1096(2) 0.0169(7) Uani 1 1 d . . . 
H10A H 0.9925 0.7384 0.1340 0.020 Uiso 1 1 calc R . . 
C11 C 0.8758(2) 0.7232(4) 0.0376(2) 0.0168(7) Uani 1 1 d . . . 
H11A H 0.8785 0.8205 0.0018 0.020 Uiso 1 1 calc R . . 
C12 C 0.8072(2) 0.6127(4) 0.0255(2) 0.0164(7) Uani 1 1 d . . . 
H12A H 0.7522 0.6224 -0.0185 0.020 Uiso 1 1 calc R . . 
C13 C 0.8627(3) 0.1218(5) 0.1859(2) 0.0240(8) Uani 1 1 d . . . 
H13A H 0.8808 0.0051 0.1790 0.036 Uiso 1 1 calc R . . 
H13B H 0.8366 0.1207 0.2269 0.036 Uiso 1 1 calc R . . 
H13C H 0.9107 0.1989 0.2027 0.036 Uiso 1 1 calc R . . 
C14 C 0.7293(3) 0.0506(5) 0.0791(3) 0.0256(9) Uani 1 1 d . . . 
H14A H 0.7528 -0.0630 0.0761 0.038 Uiso 1 1 calc R . . 
H14B H 0.6898 0.0822 0.0263 0.038 Uiso 1 1 calc R . . 
H14C H 0.7007 0.0472 0.1181 0.038 Uiso 1 1 calc R . . 
C15 C 0.7669(3) 0.4161(5) 0.1974(3) 0.0291(9) Uani 1 1 d . . . 
H15A H 0.7467 0.5337 0.1983 0.044 Uiso 1 1 calc R . . 
H15B H 0.8233 0.4060 0.2364 0.044 Uiso 1 1 calc R . . 
H15C H 0.7304 0.3349 0.2112 0.044 Uiso 1 1 calc R . . 
C16 C 0.6780(2) 0.4060(5) 0.0541(3) 0.0254(9) Uani 1 1 d . . . 
H16A H 0.6611 0.5239 0.0605 0.038 Uiso 1 1 calc R . . 
H16B H 0.6403 0.3244 0.0658 0.038 Uiso 1 1 calc R . . 
H16C H 0.6762 0.3892 -0.0011 0.038 Uiso 1 1 calc R . . 
C17 C 0.0867(2) 0.6843(5) 0.3226(2) 0.0202(8) Uani 1 1 d . . . 
C18 C 0.1087(3) 0.5188(5) 0.3084(2) 0.0256(8) Uani 1 1 d . . . 
H18A H 0.1483 0.5022 0.2829 0.031 Uiso 1 1 calc R . . 
C19 C 0.0727(3) 0.3774(5) 0.3313(3) 0.0288(9) Uani 1 1 d . . . 
H19A H 0.0870 0.2648 0.3199 0.035 Uiso 1 1 calc R . . 
C20 C 0.0161(3) 0.3976(5) 0.3707(2) 0.0289(9) Uani 1 1 d . . . 
C21 C -0.0057(3) 0.5657(6) 0.3842(3) 0.0341(10) Uani 1 1 d . . . 
H21A H -0.0453 0.5828 0.4097 0.041 Uiso 1 1 calc R . . 
C22 C 0.0294(3) 0.7073(5) 0.3608(3) 0.0321(10) Uani 1 1 d . . . 
H22A H 0.0142 0.8202 0.3709 0.039 Uiso 1 1 calc R . . 
C23 C -0.0225(3) 0.2445(6) 0.3966(3) 0.0398(11) Uani 1 1 d . . . 
H23A H 0.0001 0.1381 0.3829 0.060 Uiso 1 1 calc R . . 
H23B H -0.0827 0.2468 0.3691 0.060 Uiso 1 1 calc R . . 
H23C H -0.0100 0.2493 0.4547 0.060 Uiso 1 1 calc R . . 
H1O H 1.068(3) 0.390(7) 0.089(3) 0.026(14) Uiso 1 1 d . . . 
H2O H 0.187(3) 0.228(6) 0.174(3) 0.027(12) Uiso 1 1 d . . . 
H3O H 0.121(4) 0.131(9) 0.175(4) 0.055(18) Uiso 1 1 d . . . 
  
  
_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 2.099(3) . ? 
Mo1 O1 2.104(3) 3_765 ? 
Mo1 C4 2.262(3) . ? 
Mo1 C3 2.280(3) . ? 
Mo1 C9 2.284(4) . ? 
Mo1 C8 2.299(4) . ? 
Mo1 C12 2.321(3) . ? 
Mo1 C5 2.326(3) . ? 
Mo1 C10 2.359(3) . ? 
Mo1 C1 2.374(3) . ? 
Mo1 C2 2.380(3) . ? 
Mo1 C11 2.381(3) . ? 
S1 O5 1.451(3) . ? 
S1 O4 1.459(3) . ? 
S1 O3 1.464(3) . ? 
S1 C17 1.787(4) . ? 
O1 Mo1 2.104(3) 3_765 ? 
C1 C2 1.406(5) . ? 
C1 C5 1.444(5) . ? 
C2 C3 1.414(5) . ? 
C3 C4 1.446(5) . ? 
C4 C5 1.429(5) . ? 
C5 C6 1.518(5) . ? 
C6 C13 1.541(5) . ? 
C6 C14 1.547(5) . ? 
C6 C7 1.591(5) . ? 
C7 C8 1.524(5) . ? 
C7 C15 1.542(5) . ? 
C7 C16 1.551(5) . ? 
C8 C9 1.430(5) . ? 
C8 C12 1.452(5) . ? 
C9 C10 1.426(5) . ? 
C10 C11 1.402(5) . ? 
C11 C12 1.414(5) . ? 
C17 C18 1.387(5) . ? 
C17 C22 1.389(6) . ? 
C18 C19 1.391(6) . ? 
C19 C20 1.390(6) . ? 
C20 C21 1.402(6) . ? 
C20 C23 1.511(6) . ? 
C21 C22 1.386(6) . ? 
  
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 66.85(12) . 3_765 ? 
O1 Mo1 C4 90.50(11) . . ? 
O1 Mo1 C4 124.65(12) 3_765 . ? 
O1 Mo1 C3 82.79(12) . . ? 
O1 Mo1 C3 88.56(11) 3_765 . ? 
C4 Mo1 C3 37.12(13) . . ? 
O1 Mo1 C9 93.87(12) . . ? 
O1 Mo1 C9 131.84(11) 3_765 . ? 
C4 Mo1 C9 97.74(13) . . ? 
C3 Mo1 C9 134.30(13) . . ? 
O1 Mo1 C8 130.23(12) . . ? 
O1 Mo1 C8 138.23(11) 3_765 . ? 
C4 Mo1 C8 95.46(13) . . ? 
C3 Mo1 C8 127.38(13) . . ? 
C9 Mo1 C8 36.36(13) . . ? 
O1 Mo1 C12 135.92(11) . . ? 
O1 Mo1 C12 102.50(11) 3_765 . ? 
C4 Mo1 C12 125.71(13) . . ? 
C3 Mo1 C12 141.11(13) . . ? 
C9 Mo1 C12 60.49(13) . . ? 
C8 Mo1 C12 36.64(12) . . ? 
O1 Mo1 C5 125.96(11) . . ? 
O1 Mo1 C5 140.04(11) 3_765 . ? 
C4 Mo1 C5 36.26(12) . . ? 
C3 Mo1 C5 60.07(12) . . ? 
C9 Mo1 C5 87.48(12) . . ? 
C8 Mo1 C5 67.37(12) . . ? 
C12 Mo1 C5 90.51(12) . . ? 
O1 Mo1 C10 79.49(11) . . ? 
O1 Mo1 C10 96.18(11) 3_765 . ? 
C4 Mo1 C10 129.92(13) . . ? 
C3 Mo1 C10 158.08(14) . . ? 
C9 Mo1 C10 35.72(12) . . ? 
C8 Mo1 C10 59.24(13) . . ? 
C12 Mo1 C10 58.55(13) . . ? 
C5 Mo1 C10 122.35(12) . . ? 
O1 Mo1 C1 141.42(11) . . ? 
O1 Mo1 C1 108.08(11) 3_765 . ? 
C4 Mo1 C1 59.97(13) . . ? 
C3 Mo1 C1 58.65(13) . . ? 
C9 Mo1 C1 112.98(13) . . ? 
C8 Mo1 C1 80.39(12) . . ? 
C12 Mo1 C1 82.53(13) . . ? 
C5 Mo1 C1 35.77(12) . . ? 
C10 Mo1 C1 137.98(13) . . ? 
O1 Mo1 C2 110.92(11) . . ? 
O1 Mo1 C2 81.11(11) 3_765 . ? 
C4 Mo1 C2 60.14(13) . . ? 
C3 Mo1 C2 35.24(13) . . ? 
C9 Mo1 C2 145.69(13) . . ? 
C8 Mo1 C2 114.76(13) . . ? 
C12 Mo1 C2 109.12(13) . . ? 
C5 Mo1 C2 58.94(12) . . ? 
C10 Mo1 C2 166.68(13) . . ? 
C1 Mo1 C2 34.40(12) . . ? 
O1 Mo1 C11 101.80(11) . . ? 
O1 Mo1 C11 81.28(11) 3_765 . ? 
C4 Mo1 C11 154.07(13) . . ? 
C3 Mo1 C11 166.01(13) . . ? 
C9 Mo1 C11 59.09(12) . . ? 
C8 Mo1 C11 59.19(12) . . ? 
C12 Mo1 C11 34.97(12) . . ? 
C5 Mo1 C11 123.95(12) . . ? 
C10 Mo1 C11 34.41(12) . . ? 
C1 Mo1 C11 115.51(13) . . ? 
C2 Mo1 C11 132.52(13) . . ? 
O5 S1 O4 114.43(18) . . ? 
O5 S1 O3 112.39(17) . . ? 
O4 S1 O3 111.54(18) . . ? 
O5 S1 C17 105.40(18) . . ? 
O4 S1 C17 106.00(18) . . ? 
O3 S1 C17 106.33(17) . . ? 
Mo1 O1 Mo1 113.16(12) . 3_765 ? 
C2 C1 C5 108.7(3) . . ? 
C2 C1 Mo1 73.02(19) . . ? 
C5 C1 Mo1 70.28(19) . . ? 
C1 C2 C3 108.0(3) . . ? 
C1 C2 Mo1 72.58(19) . . ? 
C3 C2 Mo1 68.53(18) . . ? 
C2 C3 C4 109.0(3) . . ? 
C2 C3 Mo1 76.23(19) . . ? 
C4 C3 Mo1 70.74(18) . . ? 
C5 C4 C3 106.7(3) . . ? 
C5 C4 Mo1 74.32(19) . . ? 
C3 C4 Mo1 72.14(18) . . ? 
C4 C5 C1 107.6(3) . . ? 
C4 C5 C6 125.4(3) . . ? 
C1 C5 C6 126.9(3) . . ? 
C4 C5 Mo1 69.43(18) . . ? 
C1 C5 Mo1 73.95(19) . . ? 
C6 C5 Mo1 123.8(2) . . ? 
C5 C6 C13 108.8(3) . . ? 
C5 C6 C14 109.3(3) . . ? 
C13 C6 C14 106.9(3) . . ? 
C5 C6 C7 106.3(3) . . ? 
C13 C6 C7 112.2(3) . . ? 
C14 C6 C7 113.2(3) . . ? 
C8 C7 C15 108.4(3) . . ? 
C8 C7 C16 110.0(3) . . ? 
C15 C7 C16 106.4(3) . . ? 
C8 C7 C6 106.6(3) . . ? 
C15 C7 C6 112.9(3) . . ? 
C16 C7 C6 112.5(3) . . ? 
C9 C8 C12 107.2(3) . . ? 
C9 C8 C7 126.5(3) . . ? 
C12 C8 C7 126.0(3) . . ? 
C9 C8 Mo1 71.2(2) . . ? 
C12 C8 Mo1 72.5(2) . . ? 
C7 C8 Mo1 126.5(2) . . ? 
C10 C9 C8 107.5(3) . . ? 
C10 C9 Mo1 75.0(2) . . ? 
C8 C9 Mo1 72.4(2) . . ? 
C11 C10 C9 109.0(3) . . ? 
C11 C10 Mo1 73.67(19) . . ? 
C9 C10 Mo1 69.27(19) . . ? 
C10 C11 C12 108.7(3) . . ? 
C10 C11 Mo1 71.92(19) . . ? 
C12 C11 Mo1 70.17(19) . . ? 
C11 C12 C8 107.6(3) . . ? 
C11 C12 Mo1 74.9(2) . . ? 
C8 C12 Mo1 70.9(2) . . ? 
C18 C17 C22 119.5(4) . . ? 
C18 C17 S1 121.1(3) . . ? 
C22 C17 S1 119.4(3) . . ? 
C17 C18 C19 120.1(4) . . ? 
C18 C19 C20 121.3(4) . . ? 
C19 C20 C21 117.9(4) . . ? 
C19 C20 C23 121.6(4) . . ? 
C21 C20 C23 120.5(4) . . ? 
C22 C21 C20 121.1(4) . . ? 
C21 C22 C17 120.1(4) . . ? 
  
loop_ 
 _geom_hbond_atom_site_label_D 
 _geom_hbond_atom_site_label_H 
 _geom_hbond_atom_site_label_A 
 _geom_hbond_distance_DH 
 _geom_hbond_distance_HA 
 _geom_hbond_distance_DA 
 _geom_hbond_angle_DHA 
 _geom_hbond_site_symmetry_A 
O1 H1O O2  0.72(5) 1.95(5) 2.666(4) 170(5) 1_655 
O2 H2O O4  0.85(5) 1.89(5) 2.745(4) 176(5) 2_545 
O2 H3O O3  0.81(7) 2.07(7) 2.873(4) 171(6) 1_545 
  
_diffrn_measured_fraction_theta_max    0.931 
_diffrn_reflns_theta_full              28.19 
_diffrn_measured_fraction_theta_full   0.931 
_refine_diff_density_max    2.065 
_refine_diff_density_min   -1.484 
_refine_diff_density_rms    0.136 
