 
data_2008src0992
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C5 H3 Mo Nd O8 S'
_chemical_formula_weight          463.31
 
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'
 'Nd'  'Nd'  -0.1943   3.0179
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_symmetry_cell_setting            triclinic
_symmetry_space_group_name_H-M    P-1
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, -y, -z'
 
_cell_length_a                    7.2720(15)
_cell_length_b                    7.4040(15)
_cell_length_c                    18.131(4)
_cell_angle_alpha                 86.13(3)
_cell_angle_beta                  78.47(3)
_cell_angle_gamma                 89.29(3)
_cell_volume                      954.3(3)
_cell_formula_units_Z             4
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     45889
_cell_measurement_theta_min       2.91
_cell_measurement_theta_max       27.48
 
_exptl_crystal_description        needle
_exptl_crystal_colour             purple
_exptl_crystal_size_max           0.14
_exptl_crystal_size_mid           0.02
_exptl_crystal_size_min           0.01
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     3.225
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              860
_exptl_absorpt_coefficient_mu     6.937
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.4434
_exptl_absorpt_correction_T_max   0.9339
_exptl_absorpt_process_details    'SADABS 2007/2 (Sheldrick, G.M., 2007)' 
 
_exptl_special_details
;
 ?
;
 
_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 APEX II CCD camera on κ-goniostat'
_diffrn_measurement_method          'φ & ω scans'
_diffrn_detector_area_resol_mean   '4096x4096pixels / 62x62mm'
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             16689
_diffrn_reflns_av_R_equivalents   0.0885
_diffrn_reflns_av_sigmaI/netI     0.0785
_diffrn_reflns_limit_h_min        -9
_diffrn_reflns_limit_h_max        9
_diffrn_reflns_limit_k_min        -9
_diffrn_reflns_limit_k_max        9
_diffrn_reflns_limit_l_min        -23
_diffrn_reflns_limit_l_max        23
_diffrn_reflns_theta_min          3.06
_diffrn_reflns_theta_max          27.48
_reflns_number_total              4360
_reflns_number_gt                 3500
_reflns_threshold_expression      >2σ(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     ?
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics     ?
_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 > 2σ(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.

 The crystals were of poor quality which led to high wR values together 
 with low C-C bond precision (checkcif alert B). The largest remaining 
 electron densities are near the Nd atoms suggesting that a much smaller 
 secondary crystal may have been 'stuck' on to the side, or there is a small
 element of disorder or twinning. The remaining electron densities are only 
 minimal (alert C's in checkcif) and the thermal ellipsoids of the atoms are
 good indicating that the model is appropriate.

 Additional symmetry along the b axis was investigated and found to be only
 pseudo.
;
 
_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)+(0.0245P)²+78.3731P] 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          4360
_refine_ls_number_parameters      277
_refine_ls_number_restraints      148
_refine_ls_R_factor_all           0.1004
_refine_ls_R_factor_gt            0.0728
_refine_ls_wR_factor_ref          0.1690
_refine_ls_wR_factor_gt           0.1524
_refine_ls_goodness_of_fit_ref    1.067
_refine_ls_restrained_S_all       1.052
_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
C1 C 0.209(2) 0.439(2) 0.8763(9) 0.018(3) Uani 1 1 d U . .
C2 C 0.018(2) 0.416(2) 0.9050(8) 0.016(3) Uani 1 1 d U . .
H2 H -0.0590 0.3661 0.8750 0.020 Uiso 1 1 calc R . .
C3 C -0.060(2) 0.465(2) 0.9772(9) 0.019(3) Uani 1 1 d U . .
C5 C -0.248(3) 0.432(3) 1.0105(11) 0.032(4) Uani 1 1 d U . .
H5 H -0.3254 0.3747 0.9824 0.039 Uiso 1 1 calc R . .
C6 C 0.325(3) 0.5234(19) 0.9185(10) 0.023(3) Uani 1 1 d U . .
H6 H 0.4535 0.5481 0.8975 0.028 Uiso 1 1 calc R . .
C21 C -0.090(2) 0.899(2) 0.8820(8) 0.016(3) Uani 1 1 d U . .
C22 C -0.258(3) 0.895(2) 0.9389(10) 0.028(3) Uani 1 1 d U . .
H22 H -0.3728 0.8564 0.9273 0.034 Uiso 1 1 calc R . .
C23 C -0.255(2) 0.946(2) 1.0095(10) 0.024(3) Uani 1 1 d U . .
H23 H -0.3671 0.9428 1.0472 0.029 Uiso 1 1 calc R . .
C24 C -0.081(2) 1.005(2) 1.0263(8) 0.017(3) Uani 1 1 d U . .
C26 C 0.075(2) 0.944(2) 0.9007(9) 0.018(3) Uani 1 1 d U . .
H26 H 0.1878 0.9411 0.8639 0.022 Uiso 1 1 calc R . .
O1 O 0.4568(15) 0.2337(14) 0.8020(6) 0.019(2) Uani 1 1 d U . .
O2 O 0.1701(14) 0.2913(15) 0.7548(6) 0.0182(19) Uani 1 1 d U . .
O3 O 0.4043(16) 0.5279(14) 0.7461(6) 0.020(2) Uani 1 1 d U . .
O21 O -0.2574(15) 0.7243(14) 0.8003(6) 0.019(2) Uani 1 1 d U . .
O22 O 0.0725(14) 0.7699(15) 0.7573(6) 0.0157(19) Uani 1 1 d U . .
O23 O -0.1373(15) 0.0206(14) 0.7509(6) 0.019(2) Uani 1 1 d U . .
O30 O 0.4442(14) 0.8893(14) 0.7484(6) 0.0159(19) Uani 1 1 d U . .
O31 O -0.1945(14) 0.3777(14) 0.7520(6) 0.0166(19) Uani 1 1 d U . .
O32 O -0.2924(14) 0.2235(14) 0.6247(6) 0.0159(11) Uani 1 1 d U . .
O33 O 0.0323(14) 0.5653(14) 0.6234(6) 0.0157(17) Uani 1 1 d U . .
O34 O 0.4013(15) 0.4455(14) 0.5938(6) 0.0170(18) Uani 1 1 d U . .
O35 O 0.0752(14) 0.2843(14) 0.5157(5) 0.0142(18) Uani 1 1 d U . .
O36 O 0.3399(14) 0.0748(14) 0.6236(5) 0.0143(17) Uani 1 1 d U . .
O37 O 0.4037(15) 0.7951(15) 0.5154(6) 0.019(2) Uani 1 1 d U . .
O38 O 0.6679(14) 0.7364(14) 0.6220(6) 0.0159(11) Uani 1 1 d U . .
O39 O 0.0126(14) -0.0657(14) 0.5982(6) 0.0159(11) Uani 1 1 d U . .
S1 S 0.3164(5) 0.3674(5) 0.7885(2) 0.0141(7) Uani 1 1 d U . .
S2 S -0.1034(5) 0.8482(5) 0.7907(2) 0.0136(7) Uani 1 1 d U . .
Mo1 Mo 0.51517(17) 0.23799(16) 0.58071(7) 0.0120(3) Uani 1 1 d U . .
Mo2 Mo -0.09456(17) 0.73717(16) 0.58021(7) 0.0123(3) Uani 1 1 d U . .
Nd1 Nd 0.01840(11) 0.23610(10) 0.64935(4) 0.01265(19) Uani 1 1 d U . .
Nd2 Nd 0.32995(11) 0.74381(10) 0.64687(4) 0.01263(19) Uani 1 1 d U . .
 
 
_geom_special_details
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 C2 1.39(2) . ?
C1 C6 1.42(2) . ?
C1 S1 1.741(16) . ?
C2 C3 1.39(2) . ?
C2 H2 0.9500 . ?
C3 C5 1.40(2) . ?
C3 C3 1.44(3) 2_567 ?
C5 C6 1.36(3) 2_567 ?
C5 H5 0.9500 . ?
C6 C5 1.36(3) 2_567 ?
C6 H6 0.9500 . ?
C21 C26 1.36(2) . ?
C21 C22 1.43(2) . ?
C21 S2 1.745(15) . ?
C22 C23 1.36(2) . ?
C22 H22 0.9500 . ?
C23 C24 1.44(2) . ?
C23 H23 0.9500 . ?
C24 C24 1.36(3) 2_577 ?
C24 C26 1.41(2) 2_577 ?
C26 C24 1.41(2) 2_577 ?
C26 H26 0.9500 . ?
O1 S1 1.458(11) . ?
O2 S1 1.463(11) . ?
O2 Nd1 2.450(10) . ?
O3 S1 1.452(11) . ?
O3 Nd2 2.462(11) . ?
O21 S2 1.432(11) . ?
O22 S2 1.435(11) . ?
O22 Nd2 2.469(10) . ?
O23 S2 1.466(11) 1_545 ?
O23 Nd1 2.456(11) . ?
O30 Nd2 2.478(10) . ?
O31 Nd1 2.456(10) . ?
O32 Mo1 1.743(10) 1_455 ?
O32 Nd1 2.394(10) . ?
O33 Mo2 1.791(11) . ?
O33 Nd1 2.451(10) . ?
O33 Nd2 2.670(10) . ?
O34 Mo1 1.744(10) . ?
O34 Nd2 2.476(10) . ?
O35 Mo2 1.734(10) 2_566 ?
O35 Nd1 2.379(10) . ?
O36 Mo1 1.790(10) . ?
O36 Nd2 2.458(10) 1_545 ?
O36 Nd1 2.584(10) . ?
O37 Mo1 1.757(10) 2_666 ?
O37 Nd2 2.342(10) . ?
O38 Mo2 1.742(10) 1_655 ?
O38 Nd2 2.409(10) . ?
O39 Mo2 1.743(10) 1_545 ?
O39 Nd1 2.480(10) . ?
O39 Nd2 2.943(11) 1_545 ?
S2 O23 1.466(11) 1_565 ?
Mo1 O32 1.743(10) 1_655 ?
Mo1 O37 1.757(10) 2_666 ?
Mo1 Nd1 3.5779(17) . ?
Mo2 O35 1.734(10) 2_566 ?
Mo2 O38 1.742(10) 1_455 ?
Mo2 O39 1.743(10) 1_565 ?
Mo2 Nd2 3.5350(16) . ?
Nd2 O36 2.458(11) 1_565 ?
Nd2 O39 2.943(11) 1_565 ?
 
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
C2 C1 C6 120.4(15) . . ?
C2 C1 S1 122.2(12) . . ?
C6 C1 S1 117.4(12) . . ?
C1 C2 C3 120.6(13) . . ?
C1 C2 H2 119.7 . . ?
C3 C2 H2 119.7 . . ?
C2 C3 C5 122.5(15) . . ?
C2 C3 C3 118.8(18) . 2_567 ?
C5 C3 C3 118.3(19) . 2_567 ?
C6 C5 C3 122.8(18) 2_567 . ?
C6 C5 H5 118.6 2_567 . ?
C3 C5 H5 118.6 . . ?
C5 C6 C1 118.6(17) 2_567 . ?
C5 C6 H6 120.7 2_567 . ?
C1 C6 H6 120.7 . . ?
C26 C21 C22 119.1(14) . . ?
C26 C21 S2 121.9(12) . . ?
C22 C21 S2 119.1(12) . . ?
C23 C22 C21 120.6(16) . . ?
C23 C22 H22 119.7 . . ?
C21 C22 H22 119.7 . . ?
C22 C23 C24 119.2(15) . . ?
C22 C23 H23 120.4 . . ?
C24 C23 H23 120.4 . . ?
C24 C24 C26 120.0(19) 2_577 2_577 ?
C24 C24 C23 119.8(19) 2_577 . ?
C26 C24 C23 119.9(14) 2_577 . ?
C21 C26 C24 121.1(14) . 2_577 ?
C21 C26 H26 119.5 . . ?
C24 C26 H26 119.5 2_577 . ?
S1 O2 Nd1 153.7(7) . . ?
S1 O3 Nd2 135.9(6) . . ?
S2 O22 Nd2 149.4(7) . . ?
S2 O23 Nd1 140.8(7) 1_545 . ?
Mo1 O32 Nd1 163.2(6) 1_455 . ?
Mo2 O33 Nd1 137.8(5) . . ?
Mo2 O33 Nd2 103.1(4) . . ?
Nd1 O33 Nd2 118.7(4) . . ?
Mo1 O34 Nd2 156.8(6) . . ?
Mo2 O35 Nd1 165.2(6) 2_566 . ?
Mo1 O36 Nd2 135.5(5) . 1_545 ?
Mo1 O36 Nd1 108.4(5) . . ?
Nd2 O36 Nd1 115.5(4) 1_545 . ?
Mo1 O37 Nd2 161.6(6) 2_666 . ?
Mo2 O38 Nd2 165.4(6) 1_655 . ?
Mo2 O39 Nd1 154.7(6) 1_545 . ?
Mo2 O39 Nd2 94.5(4) 1_545 1_545 ?
Nd1 O39 Nd2 103.4(3) . 1_545 ?
O3 S1 O1 111.0(7) . . ?
O3 S1 O2 113.2(6) . . ?
O1 S1 O2 112.5(6) . . ?
O3 S1 C1 105.6(7) . . ?
O1 S1 C1 106.5(7) . . ?
O2 S1 C1 107.6(7) . . ?
O21 S2 O22 113.0(6) . . ?
O21 S2 O23 113.1(7) . 1_565 ?
O22 S2 O23 111.6(7) . 1_565 ?
O21 S2 C21 104.7(7) . . ?
O22 S2 C21 107.7(7) . . ?
O23 S2 C21 106.0(7) 1_565 . ?
O32 Mo1 O34 111.0(5) 1_655 . ?
O32 Mo1 O37 107.8(5) 1_655 2_666 ?
O34 Mo1 O37 111.7(5) . 2_666 ?
O32 Mo1 O36 110.8(5) 1_655 . ?
O34 Mo1 O36 104.0(5) . . ?
O37 Mo1 O36 111.5(5) 2_666 . ?
O32 Mo1 Nd1 133.5(3) 1_655 . ?
O34 Mo1 Nd1 61.8(3) . . ?
O37 Mo1 Nd1 117.5(4) 2_666 . ?
O36 Mo1 Nd1 43.3(3) . . ?
O35 Mo2 O38 108.2(5) 2_566 1_455 ?
O35 Mo2 O39 111.9(5) 2_566 1_565 ?
O38 Mo2 O39 110.4(5) 1_455 1_565 ?
O35 Mo2 O33 112.5(5) 2_566 . ?
O38 Mo2 O33 111.9(5) 1_455 . ?
O39 Mo2 O33 102.0(5) 1_565 . ?
O35 Mo2 Nd2 116.5(3) 2_566 . ?
O38 Mo2 Nd2 135.2(3) 1_455 . ?
O39 Mo2 Nd2 56.1(3) 1_565 . ?
O33 Mo2 Nd2 47.4(3) . . ?
O35 Nd1 O32 78.2(3) . . ?
O35 Nd1 O2 139.4(3) . . ?
O32 Nd1 O2 138.4(3) . . ?
O35 Nd1 O33 74.4(3) . . ?
O32 Nd1 O33 91.8(3) . . ?
O2 Nd1 O33 85.4(4) . . ?
O35 Nd1 O31 133.2(4) . . ?
O32 Nd1 O31 72.2(3) . . ?
O2 Nd1 O31 67.6(3) . . ?
O33 Nd1 O31 71.3(3) . . ?
O35 Nd1 O23 140.5(3) . . ?
O32 Nd1 O23 77.9(4) . . ?
O2 Nd1 O23 76.4(4) . . ?
O33 Nd1 O23 137.1(3) . . ?
O31 Nd1 O23 65.9(4) . . ?
O35 Nd1 O39 73.2(3) . . ?
O32 Nd1 O39 77.6(3) . . ?
O2 Nd1 O39 122.9(4) . . ?
O33 Nd1 O39 147.3(3) . . ?
O31 Nd1 O39 131.5(3) . . ?
O23 Nd1 O39 71.3(3) . . ?
O35 Nd1 O36 83.6(3) . . ?
O32 Nd1 O36 142.3(3) . . ?
O2 Nd1 O36 73.3(3) . . ?
O33 Nd1 O36 114.8(3) . . ?
O31 Nd1 O36 139.9(3) . . ?
O23 Nd1 O36 96.9(3) . . ?
O39 Nd1 O36 65.5(3) . . ?
O35 Nd1 Mo1 71.9(2) . . ?
O32 Nd1 Mo1 149.3(2) . . ?
O2 Nd1 Mo1 72.0(2) . . ?
O33 Nd1 Mo1 86.6(2) . . ?
O31 Nd1 Mo1 134.9(2) . . ?
O23 Nd1 Mo1 122.5(3) . . ?
O39 Nd1 Mo1 87.4(2) . . ?
O36 Nd1 Mo1 28.3(2) . . ?
O37 Nd2 O38 78.1(4) . . ?
O37 Nd2 O36 74.8(3) . 1_565 ?
O38 Nd2 O36 89.8(3) . 1_565 ?
O37 Nd2 O3 139.3(4) . . ?
O38 Nd2 O3 76.0(4) . . ?
O36 Nd2 O3 135.3(3) 1_565 . ?
O37 Nd2 O22 142.4(4) . . ?
O38 Nd2 O22 137.3(3) . . ?
O36 Nd2 O22 90.5(3) 1_565 . ?
O3 Nd2 O22 74.1(4) . . ?
O37 Nd2 O34 73.0(4) . . ?
O38 Nd2 O34 77.3(3) . . ?
O36 Nd2 O34 147.1(3) 1_565 . ?
O3 Nd2 O34 71.1(4) . . ?
O22 Nd2 O34 119.5(4) . . ?
O37 Nd2 O30 131.5(4) . . ?
O38 Nd2 O30 70.7(3) . . ?
O36 Nd2 O30 69.0(3) 1_565 . ?
O3 Nd2 O30 66.2(4) . . ?
O22 Nd2 O30 69.6(3) . . ?
O34 Nd2 O30 131.3(4) . . ?
O37 Nd2 O33 85.2(3) . . ?
O38 Nd2 O33 142.0(3) . . ?
O36 Nd2 O33 118.6(3) 1_565 . ?
O3 Nd2 O33 96.4(3) . . ?
O22 Nd2 O33 71.6(3) . . ?
O34 Nd2 O33 65.1(3) . . ?
O30 Nd2 O33 140.6(3) . . ?
O37 Nd2 O39 71.8(3) . 1_565 ?
O38 Nd2 O39 141.8(3) . 1_565 ?
O36 Nd2 O39 60.2(3) 1_565 1_565 ?
O3 Nd2 O39 141.8(3) . 1_565 ?
O22 Nd2 O39 70.9(3) . 1_565 ?
O34 Nd2 O39 114.3(3) . 1_565 ?
O30 Nd2 O39 113.6(3) . 1_565 ?
O33 Nd2 O39 58.3(3) . 1_565 ?
O37 Nd2 Mo2 72.3(3) . . ?
O38 Nd2 Mo2 149.6(2) . . ?
O36 Nd2 Mo2 89.2(2) 1_565 . ?
O3 Nd2 Mo2 123.6(3) . . ?
O22 Nd2 Mo2 73.1(2) . . ?
O34 Nd2 Mo2 87.3(2) . . ?
O30 Nd2 Mo2 136.1(2) . . ?
O33 Nd2 Mo2 29.6(2) . . ?
O39 Nd2 Mo2 29.5(2) 1_565 . ?
 
_diffrn_measured_fraction_theta_max    0.993
_diffrn_reflns_theta_full              27.48
_diffrn_measured_fraction_theta_full   0.993
_refine_diff_density_max    4.768
_refine_diff_density_min   -2.254
_refine_diff_density_rms    0.458
