  
data_tak3c2c 
  
_audit_creation_method            SHELXTL 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C16 H22 Mo' 
_chemical_formula_weight          310.28 
  
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'C'  'C'   0.0033   0.0016 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'H'  'H'   0.0000   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Mo'  'Mo'  -1.6832   0.6857 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
  
_symmetry_cell_setting            Monoclinic 
_symmetry_space_group_name_H-M    C2/c 
  
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, y, -z+1/2' 
 'x+1/2, y+1/2, z' 
 '-x+1/2, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x, -y, z-1/2' 
 '-x+1/2, -y+1/2, -z' 
 'x+1/2, -y+1/2, z-1/2' 
  
_cell_length_a                    32.751(10) 
_cell_length_b                    7.589(2) 
_cell_length_c                    10.966(3) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  106.612(5) 
_cell_angle_gamma                 90.00 
_cell_volume                      2611.8(14) 
_cell_formula_units_Z             8 
_cell_measurement_temperature     173(2) 
_cell_measurement_reflns_used     2378 
_cell_measurement_theta_min       2.60 
_cell_measurement_theta_max       28.02 
  
_exptl_crystal_description        plate 
_exptl_crystal_colour             yellow 
_exptl_crystal_size_max           0.23 
_exptl_crystal_size_mid           0.11 
_exptl_crystal_size_min           0.04 
_exptl_crystal_density_meas       0 
_exptl_crystal_density_diffrn     1.578 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1280 
_exptl_absorpt_coefficient_mu     0.979 
_exptl_absorpt_correction_type    'multi-scan' 
_exptl_absorpt_correction_T_min   0.737 
_exptl_absorpt_correction_T_max   1.000 
_exptl_absorpt_process_details    SADABS 
  
_exptl_special_details 
; 
 ? 
; 
  
_diffrn_ambient_temperature       173(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             7050 
_diffrn_reflns_av_R_equivalents   0.0317 
_diffrn_reflns_av_sigmaI/netI     0.0448 
_diffrn_reflns_limit_h_min        -39 
_diffrn_reflns_limit_h_max        40 
_diffrn_reflns_limit_k_min        -9 
_diffrn_reflns_limit_k_max        7 
_diffrn_reflns_limit_l_min        -14 
_diffrn_reflns_limit_l_max        12 
_diffrn_reflns_theta_min          2.60 
_diffrn_reflns_theta_max          27.00 
_reflns_number_total              2791 
_reflns_number_gt                 1990 
_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)+(0.1188P)²+0.0000P] 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          2791 
_refine_ls_number_parameters      162 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0815 
_refine_ls_R_factor_gt            0.0639 
_refine_ls_wR_factor_ref          0.1779 
_refine_ls_wR_factor_gt           0.1597 
_refine_ls_goodness_of_fit_ref    1.035 
_refine_ls_restrained_S_all       1.035 
_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 0.182485(13) 0.24963(5) 0.19326(4) 0.0132(2) Uani 1 1 d . . . 
C1 C 0.14834(15) 0.1830(7) 0.3416(4) 0.0154(10) Uani 1 1 d . . . 
H1A H 0.1357 0.2695 0.3895 0.019 Uiso 1 1 calc R . . 
C2 C 0.18890(16) 0.1028(7) 0.3861(4) 0.0191(11) Uani 1 1 d . . . 
H2A H 0.2106 0.1287 0.4689 0.023 Uiso 1 1 calc R . . 
C3 C 0.19330(17) -0.0213(7) 0.2959(5) 0.0215(12) Uani 1 1 d . . . 
H3A H 0.2184 -0.1002 0.3045 0.026 Uiso 1 1 calc R . . 
C4 C 0.15523(17) -0.0226(7) 0.1933(5) 0.0182(11) Uani 1 1 d . . . 
H4A H 0.1483 -0.1070 0.1202 0.022 Uiso 1 1 calc R . . 
C5 C 0.12695(15) 0.1053(6) 0.2199(4) 0.0145(10) Uani 1 1 d . . . 
C6 C 0.08258(16) 0.1510(7) 0.1331(4) 0.0162(11) Uani 1 1 d . . . 
C7 C 0.08226(15) 0.3465(7) 0.0839(4) 0.0174(11) Uani 1 1 d . . . 
C8 C 0.12654(15) 0.3914(6) 0.0718(4) 0.0162(10) Uani 1 1 d . . . 
C9 C 0.14807(16) 0.3156(7) -0.0134(4) 0.0164(10) Uani 1 1 d . . . 
H9A H 0.1357 0.2285 -0.0825 0.020 Uiso 1 1 calc R . . 
C10 C 0.18853(16) 0.3958(7) 0.0113(5) 0.0193(11) Uani 1 1 d . . . 
H10A H 0.2102 0.3697 -0.0346 0.023 Uiso 1 1 calc R . . 
C11 C 0.19309(17) 0.5207(7) 0.1089(5) 0.0223(12) Uani 1 1 d . . . 
H11A H 0.2182 0.6000 0.1427 0.027 Uiso 1 1 calc R . . 
C12 C 0.15489(17) 0.5212(6) 0.1467(4) 0.0177(11) Uani 1 1 d . . . 
H12A H 0.1479 0.6053 0.2080 0.021 Uiso 1 1 calc R . . 
C13 C 0.07213(18) 0.0211(8) 0.0205(5) 0.0273(13) Uani 1 1 d . . . 
H13A H 0.0725 -0.0996 0.0526 0.041 Uiso 1 1 calc R . . 
H13B H 0.0934 0.0325 -0.0261 0.041 Uiso 1 1 calc R . . 
H13C H 0.0438 0.0476 -0.0366 0.041 Uiso 1 1 calc R . . 
C14 C 0.04911(17) 0.1180(8) 0.2037(5) 0.0262(13) Uani 1 1 d . . . 
H14A H 0.0508 -0.0049 0.2322 0.039 Uiso 1 1 calc R . . 
H14B H 0.0206 0.1416 0.1465 0.039 Uiso 1 1 calc R . . 
H14C H 0.0545 0.1963 0.2777 0.039 Uiso 1 1 calc R . . 
C15 C 0.04894(17) 0.3788(8) -0.0430(5) 0.0273(13) Uani 1 1 d . . . 
H15A H 0.0503 0.5020 -0.0684 0.041 Uiso 1 1 calc R . . 
H15B H 0.0205 0.3539 -0.0345 0.041 Uiso 1 1 calc R . . 
H15C H 0.0545 0.3013 -0.1079 0.041 Uiso 1 1 calc R . . 
C16 C 0.07207(18) 0.4765(8) 0.1787(5) 0.0238(12) Uani 1 1 d . . . 
H16A H 0.0720 0.5970 0.1464 0.036 Uiso 1 1 calc R . . 
H16B H 0.0937 0.4664 0.2611 0.036 Uiso 1 1 calc R . . 
H16C H 0.0440 0.4492 0.1889 0.036 Uiso 1 1 calc R . . 
H1 H 0.221(2) 0.357(9) 0.304(6) 0.06(2) Uiso 1 1 d . . . 
H2 H 0.2237(19) 0.160(9) 0.149(6) 0.043(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 C8 2.212(5) . ? 
Mo1 C5 2.213(5) . ? 
Mo1 C12 2.250(5) . ? 
Mo1 C4 2.251(5) . ? 
Mo1 C9 2.280(4) . ? 
Mo1 C1 2.279(5) . ? 
Mo1 C11 2.322(5) . ? 
Mo1 C3 2.322(5) . ? 
Mo1 C10 2.341(5) . ? 
Mo1 C2 2.346(5) . ? 
Mo1 H1 1.68(7) . ? 
Mo1 H2 1.70(6) . ? 
C1 C2 1.415(7) . ? 
C1 C5 1.445(6) . ? 
C1 H1A 1.0000 . ? 
C2 C3 1.403(7) . ? 
C2 H2A 1.0000 . ? 
C3 C4 1.421(7) . ? 
C3 H3A 1.0000 . ? 
C4 C5 1.428(7) . ? 
C4 H4A 1.0000 . ? 
C5 C6 1.532(6) . ? 
C6 C14 1.533(7) . ? 
C6 C13 1.540(7) . ? 
C6 C7 1.578(8) . ? 
C7 C15 1.523(6) . ? 
C7 C8 1.532(7) . ? 
C7 C16 1.537(7) . ? 
C8 C12 1.439(7) . ? 
C8 C9 1.442(7) . ? 
C9 C10 1.412(7) . ? 
C9 H9A 1.0000 . ? 
C10 C11 1.406(7) . ? 
C10 H10A 1.0000 . ? 
C11 C12 1.426(8) . ? 
C11 H11A 1.0000 . ? 
C12 H12A 1.0000 . ? 
C13 H13A 0.9800 . ? 
C13 H13B 0.9800 . ? 
C13 H13C 0.9800 . ? 
C14 H14A 0.9800 . ? 
C14 H14B 0.9800 . ? 
C14 H14C 0.9800 . ? 
C15 H15A 0.9800 . ? 
C15 H15B 0.9800 . ? 
C15 H15C 0.9800 . ? 
C16 H16A 0.9800 . ? 
C16 H16B 0.9800 . ? 
C16 H16C 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 
C8 Mo1 C5 75.49(17) . . ? 
C8 Mo1 C12 37.62(17) . . ? 
C5 Mo1 C12 101.03(19) . . ? 
C8 Mo1 C4 100.74(19) . . ? 
C5 Mo1 C4 37.30(18) . . ? 
C12 Mo1 C4 135.0(2) . . ? 
C8 Mo1 C9 37.40(18) . . ? 
C5 Mo1 C9 92.78(18) . . ? 
C12 Mo1 C9 61.36(18) . . ? 
C4 Mo1 C9 96.82(19) . . ? 
C8 Mo1 C1 92.67(18) . . ? 
C5 Mo1 C1 37.49(16) . . ? 
C12 Mo1 C1 96.78(19) . . ? 
C4 Mo1 C1 61.35(18) . . ? 
C9 Mo1 C1 123.68(17) . . ? 
C8 Mo1 C11 61.43(18) . . ? 
C5 Mo1 C11 135.50(18) . . ? 
C12 Mo1 C11 36.31(19) . . ? 
C4 Mo1 C11 156.62(18) . . ? 
C9 Mo1 C11 59.80(18) . . ? 
C1 Mo1 C11 129.9(2) . . ? 
C8 Mo1 C3 135.06(19) . . ? 
C5 Mo1 C3 61.00(18) . . ? 
C12 Mo1 C3 156.49(19) . . ? 
C4 Mo1 C3 36.15(17) . . ? 
C9 Mo1 C3 129.79(19) . . ? 
C1 Mo1 C3 59.71(19) . . ? 
C11 Mo1 C3 163.35(18) . . ? 
C8 Mo1 C10 60.90(18) . . ? 
C5 Mo1 C10 128.31(17) . . ? 
C12 Mo1 C10 59.92(18) . . ? 
C4 Mo1 C10 124.43(18) . . ? 
C9 Mo1 C10 35.55(18) . . ? 
C1 Mo1 C10 153.16(18) . . ? 
C11 Mo1 C10 35.09(18) . . ? 
C3 Mo1 C10 142.60(19) . . ? 
C8 Mo1 C2 128.25(18) . . ? 
C5 Mo1 C2 60.74(17) . . ? 
C12 Mo1 C2 124.50(19) . . ? 
C4 Mo1 C2 59.80(17) . . ? 
C9 Mo1 C2 153.12(19) . . ? 
C1 Mo1 C2 35.60(17) . . ? 
C11 Mo1 C2 142.65(18) . . ? 
C3 Mo1 C2 34.97(18) . . ? 
C10 Mo1 C2 170.43(17) . . ? 
C8 Mo1 H1 121(2) . . ? 
C5 Mo1 H1 128(2) . . ? 
C12 Mo1 H1 84(2) . . ? 
C4 Mo1 H1 131(2) . . ? 
C9 Mo1 H1 132(2) . . ? 
C1 Mo1 H1 91(2) . . ? 
C11 Mo1 H1 72(2) . . ? 
C3 Mo1 H1 96(2) . . ? 
C10 Mo1 H1 99(2) . . ? 
C2 Mo1 H1 74(2) . . ? 
C8 Mo1 H2 128(2) . . ? 
C5 Mo1 H2 126(2) . . ? 
C12 Mo1 H2 127(2) . . ? 
C4 Mo1 H2 89(2) . . ? 
C9 Mo1 H2 91(2) . . ? 
C1 Mo1 H2 135(2) . . ? 
C11 Mo1 H2 91(2) . . ? 
C3 Mo1 H2 76(2) . . ? 
C10 Mo1 H2 71(2) . . ? 
C2 Mo1 H2 101(2) . . ? 
H1 Mo1 H2 85(3) . . ? 
C2 C1 C5 107.6(4) . . ? 
C2 C1 Mo1 74.8(3) . . ? 
C5 C1 Mo1 68.8(3) . . ? 
C2 C1 H1A 126.1 . . ? 
C5 C1 H1A 126.1 . . ? 
Mo1 C1 H1A 126.1 . . ? 
C3 C2 C1 108.7(4) . . ? 
C3 C2 Mo1 71.6(3) . . ? 
C1 C2 Mo1 69.6(3) . . ? 
C3 C2 H2A 125.6 . . ? 
C1 C2 H2A 125.6 . . ? 
Mo1 C2 H2A 125.6 . . ? 
C2 C3 C4 108.6(5) . . ? 
C2 C3 Mo1 73.5(3) . . ? 
C4 C3 Mo1 69.2(3) . . ? 
C2 C3 H3A 125.7 . . ? 
C4 C3 H3A 125.7 . . ? 
Mo1 C3 H3A 125.7 . . ? 
C3 C4 C5 107.9(4) . . ? 
C3 C4 Mo1 74.7(3) . . ? 
C5 C4 Mo1 69.9(3) . . ? 
C3 C4 H4A 125.9 . . ? 
C5 C4 H4A 125.9 . . ? 
Mo1 C4 H4A 125.9 . . ? 
C4 C5 C1 107.1(4) . . ? 
C4 C5 C6 125.6(4) . . ? 
C1 C5 C6 127.2(4) . . ? 
C4 C5 Mo1 72.8(3) . . ? 
C1 C5 Mo1 73.8(3) . . ? 
C6 C5 Mo1 118.4(3) . . ? 
C5 C6 C14 109.7(4) . . ? 
C5 C6 C13 107.9(4) . . ? 
C14 C6 C13 105.9(4) . . ? 
C5 C6 C7 109.7(4) . . ? 
C14 C6 C7 113.0(4) . . ? 
C13 C6 C7 110.5(4) . . ? 
C15 C7 C8 109.5(4) . . ? 
C15 C7 C16 106.1(4) . . ? 
C8 C7 C16 108.0(4) . . ? 
C15 C7 C6 113.4(4) . . ? 
C8 C7 C6 108.9(4) . . ? 
C16 C7 C6 110.8(4) . . ? 
C12 C8 C9 106.7(4) . . ? 
C12 C8 C7 125.1(4) . . ? 
C9 C8 C7 128.2(4) . . ? 
C12 C8 Mo1 72.6(3) . . ? 
C9 C8 Mo1 73.9(3) . . ? 
C7 C8 Mo1 118.8(3) . . ? 
C10 C9 C8 108.1(4) . . ? 
C10 C9 Mo1 74.6(3) . . ? 
C8 C9 Mo1 68.7(2) . . ? 
C10 C9 H9A 125.9 . . ? 
C8 C9 H9A 125.9 . . ? 
Mo1 C9 H9A 125.9 . . ? 
C11 C10 C9 109.0(5) . . ? 
C11 C10 Mo1 71.7(3) . . ? 
C9 C10 Mo1 69.9(3) . . ? 
C11 C10 H10A 125.5 . . ? 
C9 C10 H10A 125.5 . . ? 
Mo1 C10 H10A 125.5 . . ? 
C10 C11 C12 108.2(5) . . ? 
C10 C11 Mo1 73.2(3) . . ? 
C12 C11 Mo1 69.1(3) . . ? 
C10 C11 H11A 125.9 . . ? 
C12 C11 H11A 125.9 . . ? 
Mo1 C11 H11A 125.9 . . ? 
C11 C12 C8 108.0(4) . . ? 
C11 C12 Mo1 74.6(3) . . ? 
C8 C12 Mo1 69.8(3) . . ? 
C11 C12 H12A 125.9 . . ? 
C8 C12 H12A 125.9 . . ? 
Mo1 C12 H12A 125.9 . . ? 
C6 C13 H13A 109.5 . . ? 
C6 C13 H13B 109.5 . . ? 
H13A C13 H13B 109.5 . . ? 
C6 C13 H13C 109.5 . . ? 
H13A C13 H13C 109.5 . . ? 
H13B C13 H13C 109.5 . . ? 
C6 C14 H14A 109.5 . . ? 
C6 C14 H14B 109.5 . . ? 
H14A C14 H14B 109.5 . . ? 
C6 C14 H14C 109.5 . . ? 
H14A C14 H14C 109.5 . . ? 
H14B C14 H14C 109.5 . . ? 
C7 C15 H15A 109.5 . . ? 
C7 C15 H15B 109.5 . . ? 
H15A C15 H15B 109.5 . . ? 
C7 C15 H15C 109.5 . . ? 
H15A C15 H15C 109.5 . . ? 
H15B C15 H15C 109.5 . . ? 
C7 C16 H16A 109.5 . . ? 
C7 C16 H16B 109.5 . . ? 
H16A C16 H16B 109.5 . . ? 
C7 C16 H16C 109.5 . . ? 
H16A C16 H16C 109.5 . . ? 
H16B C16 H16C 109.5 . . ? 
  
_diffrn_measured_fraction_theta_max    0.983 
_diffrn_reflns_theta_full              27.00 
_diffrn_measured_fraction_theta_full   0.983 
_refine_diff_density_max    6.041 
_refine_diff_density_min   -1.236 
_refine_diff_density_rms    0.213 
