data_2005src0805
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 Dr. A. G. W. Hodson
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          'C24 H16 Cl2 Mo2 N4 O4, 2(C2 H6 O S)'
_chemical_formula_sum
 'C28 H28 Cl2 Mo2 N4 O6 S2'
_chemical_formula_weight          843.44
 
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'
 'Cl'  'Cl'   0.1484   0.1585
 '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'
 
_symmetry_cell_setting            monoclinic
_symmetry_space_group_name_H-M    C2/c
_symmetry_space_group_name_hall   '-C 2yc'
 
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                    22.361(5)
_cell_length_b                    11.409(2)
_cell_length_c                    15.609(3)
_cell_angle_alpha                 90.00
_cell_angle_beta                  128.22(3)
_cell_angle_gamma                 90.00
_cell_volume                      3128.5(17)
_cell_formula_units_Z             4
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     3695
_cell_measurement_theta_min       2.910
_cell_measurement_theta_max       27.485
 
_exptl_crystal_description        Block
_exptl_crystal_colour             Red
_exptl_crystal_size_max           0.12
_exptl_crystal_size_mid           0.07
_exptl_crystal_size_min           0.04
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.791
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1688
_exptl_absorpt_coefficient_mu     1.155
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.8738
_exptl_absorpt_correction_T_max   0.9553
_exptl_absorpt_process_details       'SADABS V2.10 (Sheldrick, G.M., 2003)'

_diffrn_ambient_temperature           120(2)
_diffrn_radiation_wavelength           0.71073
_diffrn_radiation_type                      MoK\a
_diffrn_radiation_source                  'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_monochromator    '10cm confocal mirrors'
_diffrn_measurement_device_type  'Bruker-Nonius 95mm CCD camera on κ-goniostat'
_diffrn_measurement_method          'φ & ω scans'
_diffrn_detector_area_resol_mean   9.091
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             21247
_diffrn_reflns_av_R_equivalents   0.0527
_diffrn_reflns_av_sigmaI/netI     0.0407
_diffrn_reflns_limit_h_min        -28
_diffrn_reflns_limit_h_max        28
_diffrn_reflns_limit_k_min        -14
_diffrn_reflns_limit_k_max        14
_diffrn_reflns_limit_l_min        -20
_diffrn_reflns_limit_l_max        20
_diffrn_reflns_theta_min          3.11
_diffrn_reflns_theta_max          27.48
_reflns_number_total              3586
_reflns_number_gt                 3001
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection        
'COLLECT (Hooft, R.W.W., 1998)'
_computing_cell_refinement        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
#Although determined using DirAx, the cell is refined in the HKL
#package during data reduction
_computing_data_reduction         
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1997a)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997b)' 
_computing_molecular_graphics     'ORTEP3 for Windows (Farrugia, 1997)'
_computing_publication_material   ?
 
_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)+(0.0401P)²+11.7918P] where P=(Fo²+2Fc²)/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_extinction_coef        ?
_refine_ls_number_reflns          3586
_refine_ls_number_parameters      201
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0469
_refine_ls_R_factor_gt            0.0365
_refine_ls_wR_factor_ref          0.0929
_refine_ls_wR_factor_gt           0.0875
_refine_ls_goodness_of_fit_ref    1.058
_refine_ls_restrained_S_all       1.058
_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
C1 C 0.09448(18) -0.4029(3) 0.5713(3) 0.0186(7) Uani 1 1 d . . .
H1 H 0.0742 -0.4792 0.5447 0.022 Uiso 1 1 calc R . .
C2 C 0.15283(18) -0.3878(3) 0.6832(3) 0.0200(7) Uani 1 1 d . . .
H2 H 0.1707 -0.4530 0.7311 0.024 Uiso 1 1 calc R . .
C3 C 0.18399(18) -0.2796(3) 0.7234(3) 0.0204(7) Uani 1 1 d . . .
H3 H 0.2246 -0.2694 0.7989 0.024 Uiso 1 1 calc R . .
C4 C 0.15512(18) -0.1831(3) 0.6513(3) 0.0184(7) Uani 1 1 d . . .
C5 C 0.09516(17) -0.2046(3) 0.5406(2) 0.0159(6) Uani 1 1 d . . .
C6 C 0.05783(17) -0.1083(3) 0.4659(2) 0.0155(6) Uani 1 1 d . . .
C7 C 0.08152(18) 0.0069(3) 0.5034(3) 0.0181(6) Uani 1 1 d . . .
C8 C 0.03761(18) 0.0986(3) 0.4288(3) 0.0193(7) Uani 1 1 d . . .
H8 H 0.0518 0.1781 0.4501 0.023 Uiso 1 1 calc R . .
C9 C -0.02557(18) 0.0714(3) 0.3257(3) 0.0196(7) Uani 1 1 d . . .
H9 H -0.0569 0.1320 0.2755 0.024 Uiso 1 1 calc R . .
C10 C -0.04399(18) -0.0470(3) 0.2943(3) 0.0192(7) Uani 1 1 d . . .
H10 H -0.0879 -0.0645 0.2222 0.023 Uiso 1 1 calc R . .
C11 C 0.18097(18) -0.0661(3) 0.6860(3) 0.0200(7) Uani 1 1 d . . .
H11 H 0.2236 -0.0519 0.7598 0.024 Uiso 1 1 calc R . .
C12 C 0.14609(18) 0.0259(3) 0.6160(3) 0.0208(7) Uani 1 1 d . . .
H12 H 0.1644 0.1033 0.6414 0.025 Uiso 1 1 calc R . .
N1 N 0.06645(15) -0.3142(2) 0.5010(2) 0.0160(5) Uani 1 1 d . . .
N2 N -0.00247(15) -0.1354(2) 0.3615(2) 0.0161(5) Uani 1 1 d . . .
O1 O -0.01098(12) -0.4814(2) 0.33891(17) 0.0197(5) Uani 1 1 d . . .
O2 O -0.07803(12) -0.2971(2) 0.16652(17) 0.0184(5) Uani 1 1 d . . .
Cl1 Cl -0.12474(5) -0.30902(7) 0.31445(7) 0.02189(18) Uani 1 1 d . . .
Mo1 Mo -0.013350(15) -0.33516(2) 0.31906(2) 0.01523(10) Uani 1 1 d . . .
C21 C 0.2510(2) -0.0900(4) 0.4948(4) 0.0416(11) Uani 1 1 d . . .
H21A H 0.2037 -0.1260 0.4734 0.062 Uiso 1 1 calc R . .
H21B H 0.2945 -0.1269 0.5619 0.062 Uiso 1 1 calc R . .
H21C H 0.2552 -0.1013 0.4365 0.062 Uiso 1 1 calc R . .
C22 C 0.3407(2) 0.1016(4) 0.5547(4) 0.0385(10) Uani 1 1 d . . .
H22A H 0.3418 0.0824 0.4945 0.058 Uiso 1 1 calc R . .
H22B H 0.3805 0.0574 0.6198 0.058 Uiso 1 1 calc R . .
H22C H 0.3496 0.1858 0.5702 0.058 Uiso 1 1 calc R . .
O21 O 0.19153(15) 0.1171(2) 0.4077(2) 0.0336(6) Uani 1 1 d . . .
S21 S 0.25000(5) 0.06378(9) 0.51767(7) 0.0277(2) Uani 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
C1 N1 1.331(4) . ?
C1 C2 1.401(5) . ?
C1 H1 0.9500 . ?
C2 C3 1.364(5) . ?
C2 H2 0.9500 . ?
C3 C4 1.413(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.406(4) . ?
C4 C11 1.421(5) . ?
C5 N1 1.366(4) . ?
C5 C6 1.436(4) . ?
C6 N2 1.360(4) . ?
C6 C7 1.402(5) . ?
C7 C8 1.415(4) . ?
C7 C12 1.442(5) . ?
C8 C9 1.368(5) . ?
C8 H8 0.9500 . ?
C9 C10 1.409(5) . ?
C9 H9 0.9500 . ?
C10 N2 1.332(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.360(5) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
N1 Mo1 2.244(3) . ?
N2 Mo1 2.344(3) . ?
O1 Mo1 1.692(2) . ?
O2 Mo1 1.921(2) . ?
O2 Mo1 1.961(2) 2 ?
Cl1 Mo1 2.4651(10) . ?
Mo1 O2 1.961(2) 2 ?
Mo1 Mo1 2.5687(7) 2 ?
C21 S21 1.794(4) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 S21 1.784(4) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
O21 S21 1.499(3) . ?
 
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
N1 C1 C2 122.3(3) . . ?
N1 C1 H1 118.8 . . ?
C2 C1 H1 118.8 . . ?
C3 C2 C1 120.1(3) . . ?
C3 C2 H2 120.0 . . ?
C1 C2 H2 120.0 . . ?
C2 C3 C4 119.2(3) . . ?
C2 C3 H3 120.4 . . ?
C4 C3 H3 120.4 . . ?
C5 C4 C3 117.4(3) . . ?
C5 C4 C11 119.1(3) . . ?
C3 C4 C11 123.4(3) . . ?
N1 C5 C4 122.7(3) . . ?
N1 C5 C6 117.3(3) . . ?
C4 C5 C6 119.9(3) . . ?
N2 C6 C7 123.5(3) . . ?
N2 C6 C5 116.5(3) . . ?
C7 C6 C5 119.9(3) . . ?
C6 C7 C8 117.3(3) . . ?
C6 C7 C12 119.0(3) . . ?
C8 C7 C12 123.6(3) . . ?
C9 C8 C7 119.1(3) . . ?
C9 C8 H8 120.4 . . ?
C7 C8 H8 120.4 . . ?
C8 C9 C10 119.6(3) . . ?
C8 C9 H9 120.2 . . ?
C10 C9 H9 120.2 . . ?
N2 C10 C9 122.7(3) . . ?
N2 C10 H10 118.6 . . ?
C9 C10 H10 118.6 . . ?
C12 C11 C4 121.5(3) . . ?
C12 C11 H11 119.3 . . ?
C4 C11 H11 119.3 . . ?
C11 C12 C7 120.5(3) . . ?
C11 C12 H12 119.8 . . ?
C7 C12 H12 119.8 . . ?
C1 N1 C5 118.2(3) . . ?
C1 N1 Mo1 124.2(2) . . ?
C5 N1 Mo1 117.0(2) . . ?
C10 N2 C6 117.5(3) . . ?
C10 N2 Mo1 127.9(2) . . ?
C6 N2 Mo1 114.3(2) . . ?
Mo1 O2 Mo1 82.86(9) . 2 ?
O1 Mo1 O2 111.36(10) . . ?
O1 Mo1 O2 106.55(10) . 2 ?
O2 Mo1 O2 91.39(10) . 2 ?
O1 Mo1 N1 87.89(10) . . ?
O2 Mo1 N1 160.76(10) . . ?
O2 Mo1 N1 82.82(10) 2 . ?
O1 Mo1 N2 157.12(10) . . ?
O2 Mo1 N2 89.85(10) . . ?
O2 Mo1 N2 80.42(9) 2 . ?
N1 Mo1 N2 71.13(9) . . ?
O1 Mo1 Cl1 92.36(8) . . ?
O2 Mo1 Cl1 87.95(8) . . ?
O2 Mo1 Cl1 159.87(7) 2 . ?
N1 Mo1 Cl1 91.26(8) . . ?
N2 Mo1 Cl1 79.46(7) . . ?
O1 Mo1 Mo1 99.01(7) . 2 ?
O2 Mo1 Mo1 49.25(7) . 2 ?
O2 Mo1 Mo1 47.89(7) 2 2 ?
N1 Mo1 Mo1 130.28(7) . 2 ?
N2 Mo1 Mo1 101.51(6) . 2 ?
Cl1 Mo1 Mo1 136.96(4) . 2 ?
S21 C21 H21A 109.5 . . ?
S21 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
S21 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
S21 C22 H22A 109.5 . . ?
S21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
S21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O21 S21 C22 106.52(19) . . ?
O21 S21 C21 106.15(19) . . ?
C22 S21 C21 98.6(2) . . ?
 
_diffrn_measured_fraction_theta_max    0.997
_diffrn_reflns_theta_full              27.48
_diffrn_measured_fraction_theta_full   0.997
_refine_diff_density_max    1.412
_refine_diff_density_min   -0.850
_refine_diff_density_rms    0.115
