 
data_2009src0059p21c
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C10 H10 La2 O16 S2 W2'
_chemical_formula_weight          1095.82
 
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'
 'La'  'La'  -0.2871   2.4523
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'W'  'W'  -0.8490   6.8722
 '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    P21/c
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x, -y-1/2, z-1/2'
 
_cell_length_a                    17.1242(11)
_cell_length_b                    7.4638(5)
_cell_length_c                    7.6228(5)
_cell_angle_alpha                 90.00
_cell_angle_beta                  91.048(4)
_cell_angle_gamma                 90.00
_cell_volume                      974.12(11)
_cell_formula_units_Z             2
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     44821
_cell_measurement_theta_min       2.91
_cell_measurement_theta_max       27.48
 
_exptl_crystal_description        lath
_exptl_crystal_colour             colourless
_exptl_crystal_size_max           0.10
_exptl_crystal_size_mid           0.04
_exptl_crystal_size_min           0.01
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     3.736
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              984
_exptl_absorpt_coefficient_mu     16.365
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.2914
_exptl_absorpt_correction_T_max   0.8535
_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             10570
_diffrn_reflns_av_R_equivalents   0.0782
_diffrn_reflns_av_sigmaI/netI     0.0627
_diffrn_reflns_limit_h_min        -22
_diffrn_reflns_limit_h_max        22
_diffrn_reflns_limit_k_min        -9
_diffrn_reflns_limit_k_max        9
_diffrn_reflns_limit_l_min        -9
_diffrn_reflns_limit_l_max        9
_diffrn_reflns_theta_min          2.98
_diffrn_reflns_theta_max          27.47
_reflns_number_total              2214
_reflns_number_gt                 1871
_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.

 ISOR command used for atoms C1, C2, C3, C4, C5 and C6 as these were non-
 positive definites.

 Hydrogen atoms on water molecule fixed used DFIX, DANG. Thermal parameter
 refined isotropically.

 Second WGHT parameter larger than usual - this is due to the difference in
 the weights of the atoms present. To try to address this problem a number
 of absorption corrections were tried, of which this was found to give the
 best results.
;
 
_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)+(0.0000P)²+73.8004P] 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          2214
_refine_ls_number_parameters      153
_refine_ls_number_restraints      33
_refine_ls_R_factor_all           0.0770
_refine_ls_R_factor_gt            0.0595
_refine_ls_wR_factor_ref          0.1255
_refine_ls_wR_factor_gt           0.1166
_refine_ls_goodness_of_fit_ref    1.121
_refine_ls_restrained_S_all       1.113
_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 0.0963(9) 0.393(2) 0.062(2) 0.018(3) Uani 1 1 d U . .
C2 C 0.0741(9) 0.227(2) 0.114(2) 0.015(3) Uani 1 1 d U . .
H2 H 0.1124 0.1414 0.1494 0.019 Uiso 1 1 calc R . .
C3 C -0.0058(9) 0.181(2) 0.1167(18) 0.016(3) Uani 1 1 d U . .
H3 H -0.0211 0.0654 0.1557 0.019 Uiso 1 1 calc R . .
C4 C 0.0401(9) 0.524(2) -0.003(2) 0.018(3) Uani 1 1 d U . .
C5 C 0.0618(9) 0.697(2) -0.0627(19) 0.013(3) Uani 1 1 d U . .
H5 H 0.1155 0.7289 -0.0658 0.016 Uiso 1 1 calc R . .
O3 O 0.3919(7) 0.4440(16) 0.0492(15) 0.026(3) Uani 1 1 d . . .
O4 O 0.3734(7) 0.4058(14) 0.4103(15) 0.023(3) Uani 1 1 d . . .
O21 O 0.1973(7) 0.6050(15) 0.2107(14) 0.023(3) Uani 1 1 d . . .
O22 O 0.2246(7) 0.5021(17) -0.0850(15) 0.025(3) Uani 1 1 d . . .
O23 O 0.2348(7) 0.2951(16) 0.1598(15) 0.024(3) Uani 1 1 d . . .
O1W O 0.2403(7) -0.0725(16) 0.0649(15) 0.023(3) Uani 1 1 d D . .
H2W H 0.226(12) -0.08(2) -0.042(8) 0.05(7) Uiso 1 1 d D . .
H1W H 0.222(9) -0.165(13) 0.116(16) 0.01(4) Uiso 1 1 d D . .
O1 O 0.5145(7) 0.5808(15) 0.2828(13) 0.019(2) Uani 1 1 d . . .
O2 O 0.3685(6) 0.7686(15) 0.2565(14) 0.020(2) Uani 1 1 d . . .
La1 La 0.34450(5) 0.09171(11) 0.23768(11) 0.0138(2) Uani 1 1 d . . .
W1 W 0.41341(4) 0.55515(8) 0.25077(8) 0.01361(18) Uani 1 1 d . . .
S1 S 0.1956(2) 0.4537(5) 0.0875(5) 0.0169(8) Uani 1 1 d . . .
 
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
C1 0.018(6) 0.018(6) 0.018(6) -0.006(5) -0.001(5) -0.003(5)
C2 0.012(6) 0.014(6) 0.021(6) -0.005(5) 0.000(5) 0.007(5)
C3 0.025(7) 0.017(6) 0.005(5) -0.007(5) 0.001(5) 0.000(5)
C4 0.019(6) 0.019(6) 0.016(6) -0.001(5) -0.003(5) 0.006(5)
C5 0.015(6) 0.011(6) 0.015(6) 0.000(5) 0.001(5) -0.003(5)
O3 0.030(7) 0.027(7) 0.021(6) 0.001(5) 0.010(5) 0.004(5)
O4 0.028(7) 0.007(5) 0.033(7) 0.003(5) -0.004(5) 0.004(5)
O21 0.038(7) 0.015(6) 0.015(5) 0.003(4) -0.001(5) -0.006(5)
O22 0.021(6) 0.031(7) 0.024(6) 0.004(5) 0.000(5) 0.004(5)
O23 0.016(6) 0.024(6) 0.031(6) 0.008(5) -0.007(5) 0.006(5)
O1W 0.032(7) 0.020(6) 0.017(6) 0.006(4) -0.006(5) -0.017(5)
O1 0.030(6) 0.018(6) 0.011(5) 0.004(4) 0.007(4) -0.003(5)
O2 0.018(6) 0.015(6) 0.027(6) 0.001(5) -0.005(5) -0.001(4)
La1 0.0168(4) 0.0108(4) 0.0137(4) 0.0002(3) 0.0001(3) 0.0005(3)
W1 0.0168(3) 0.0096(3) 0.0145(3) -0.0001(2) 0.0001(2) -0.0001(2)
S1 0.0190(19) 0.0141(18) 0.0177(18) 0.0020(14) 0.0005(14) -0.0006(15)
 
_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 1.36(2) . ?
C1 C4 1.45(2) . ?
C1 S1 1.768(16) . ?
C2 C3 1.41(2) . ?
C2 H2 0.9500 . ?
C3 C5 1.38(2) 3_565 ?
C3 H3 0.9500 . ?
C4 C5 1.42(2) . ?
C4 C4 1.42(3) 3_565 ?
C5 C3 1.38(2) 3_565 ?
C5 H5 0.9500 . ?
O3 W1 1.779(12) . ?
O3 La1 2.510(12) 4_565 ?
O4 W1 1.795(11) . ?
O4 La1 2.553(12) 4_566 ?
O4 La1 2.729(11) . ?
O21 S1 1.469(12) . ?
O22 S1 1.459(12) . ?
O22 La1 2.575(12) 4_565 ?
O23 S1 1.464(12) . ?
O23 La1 2.480(11) . ?
O1W La1 2.518(11) . ?
O1W H2W 0.85(2) . ?
O1W H1W 0.85(2) . ?
O1 W1 1.755(12) . ?
O1 La1 2.423(12) 2_655 ?
O2 W1 1.770(11) . ?
O2 La1 2.450(11) 1_565 ?
La1 O1 2.423(12) 2_645 ?
La1 O2 2.450(11) 1_545 ?
La1 O3 2.510(12) 4_566 ?
La1 O4 2.553(12) 4_565 ?
La1 O22 2.575(12) 4_566 ?
La1 W1 3.6555(10) . ?
 
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 C4 121.9(14) . . ?
C2 C1 S1 118.5(12) . . ?
C4 C1 S1 119.5(12) . . ?
C1 C2 C3 120.1(14) . . ?
C1 C2 H2 119.9 . . ?
C3 C2 H2 119.9 . . ?
C5 C3 C2 120.3(14) 3_565 . ?
C5 C3 H3 119.9 3_565 . ?
C2 C3 H3 119.9 . . ?
C5 C4 C4 120.0(18) . 3_565 ?
C5 C4 C1 123.2(14) . . ?
C4 C4 C1 116.8(18) 3_565 . ?
C3 C5 C4 120.7(14) 3_565 . ?
C3 C5 H5 119.6 3_565 . ?
C4 C5 H5 119.6 . . ?
W1 O3 La1 157.7(7) . 4_565 ?
W1 O4 La1 137.8(6) . 4_566 ?
W1 O4 La1 106.0(5) . . ?
La1 O4 La1 116.2(4) 4_566 . ?
S1 O22 La1 133.9(7) . 4_565 ?
S1 O23 La1 157.8(7) . . ?
La1 O1W H2W 136(10) . . ?
La1 O1W H1W 114(10) . . ?
H2W O1W H1W 108(5) . . ?
W1 O1 La1 167.5(6) . 2_655 ?
W1 O2 La1 163.2(6) . 1_565 ?
O1 La1 O2 78.7(4) 2_645 1_545 ?
O1 La1 O23 139.2(4) 2_645 . ?
O2 La1 O23 137.9(4) 1_545 . ?
O1 La1 O3 75.7(4) 2_645 4_566 ?
O2 La1 O3 77.8(4) 1_545 4_566 ?
O23 La1 O3 121.5(4) . 4_566 ?
O1 La1 O1W 130.4(4) 2_645 . ?
O2 La1 O1W 70.6(4) 1_545 . ?
O23 La1 O1W 69.3(4) . . ?
O3 La1 O1W 131.1(4) 4_566 . ?
O1 La1 O4 74.1(4) 2_645 4_565 ?
O2 La1 O4 91.7(4) 1_545 4_565 ?
O23 La1 O4 85.5(4) . 4_565 ?
O3 La1 O4 149.4(4) 4_566 4_565 ?
O1W La1 O4 68.9(4) . 4_565 ?
O1 La1 O22 146.0(4) 2_645 4_566 ?
O2 La1 O22 80.6(4) 1_545 4_566 ?
O23 La1 O22 71.6(4) . 4_566 ?
O3 La1 O22 73.8(4) 4_566 4_566 ?
O1W La1 O22 65.0(4) . 4_566 ?
O4 La1 O22 133.3(4) 4_565 4_566 ?
O1 La1 O4 83.6(4) 2_645 . ?
O2 La1 O4 142.0(3) 1_545 . ?
O23 La1 O4 73.7(4) . . ?
O3 La1 O4 65.3(4) 4_566 . ?
O1W La1 O4 142.3(4) . . ?
O4 La1 O4 115.4(3) 4_565 . ?
O22 La1 O4 96.9(4) 4_566 . ?
O1 La1 W1 73.3(3) 2_645 . ?
O2 La1 W1 151.2(3) 1_545 . ?
O23 La1 W1 70.7(3) . . ?
O3 La1 W1 88.6(3) 4_566 . ?
O1W La1 W1 134.5(3) . . ?
O4 La1 W1 87.2(2) 4_565 . ?
O22 La1 W1 120.2(3) 4_566 . ?
O4 La1 W1 28.2(2) . . ?
O1 W1 O2 109.0(5) . . ?
O1 W1 O3 111.1(5) . . ?
O2 W1 O3 111.0(5) . . ?
O1 W1 O4 111.2(5) . . ?
O2 W1 O4 111.8(5) . . ?
O3 W1 O4 102.7(5) . . ?
O1 W1 La1 115.1(4) . . ?
O2 W1 La1 135.4(4) . . ?
O3 W1 La1 58.2(4) . . ?
O4 W1 La1 45.9(4) . . ?
O22 S1 O23 112.2(7) . . ?
O22 S1 O21 112.5(7) . . ?
O23 S1 O21 112.2(7) . . ?
O22 S1 C1 107.9(7) . . ?
O23 S1 C1 105.4(7) . . ?
O21 S1 C1 106.1(7) . . ?
 
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
O1W H2W O21  0.85(2) 1.95(3) 2.796(15) 176(22) 4_565
O1W H2W S1  0.85(2) 3.01(6) 3.810(12) 158(13) 4_565
O1W H1W S1  0.85(2) 2.89(9) 3.622(12) 145(13) 1_545
O1W H1W O21  0.85(2) 1.92(4) 2.756(15) 169(16) 1_545
 
_diffrn_measured_fraction_theta_max    0.998
_diffrn_reflns_theta_full              27.47
_diffrn_measured_fraction_theta_full   0.998
_refine_diff_density_max    2.082
_refine_diff_density_min   -2.510
_refine_diff_density_rms    0.468
