 
data_2009src0060p-1
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C20 H20 La4 O32 S4 W4'
_chemical_formula_weight          2191.64
 
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'
 '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'
 
_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                    7.2550(2)
_cell_length_b                    8.1110(2)
_cell_length_c                    16.9310(4)
_cell_angle_alpha                 80.4080(10)
_cell_angle_beta                  78.6810(10)
_cell_angle_gamma                 89.6740(10)
_cell_volume                      962.90(4)
_cell_formula_units_Z             1
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     30099
_cell_measurement_theta_min       2.91
_cell_measurement_theta_max       27.48
 
_exptl_crystal_description        blade
_exptl_crystal_colour             colourless
_exptl_crystal_size_max           0.14
_exptl_crystal_size_mid           0.03
_exptl_crystal_size_min           0.01
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     3.780
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              984
_exptl_absorpt_coefficient_mu     16.555
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.2052
_exptl_absorpt_correction_T_max   0.8519
_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             19673
_diffrn_reflns_av_R_equivalents   0.0598
_diffrn_reflns_av_sigmaI/netI     0.0494
_diffrn_reflns_limit_h_min        -9
_diffrn_reflns_limit_h_max        9
_diffrn_reflns_limit_k_min        -10
_diffrn_reflns_limit_k_max        10
_diffrn_reflns_limit_l_min        -21
_diffrn_reflns_limit_l_max        21
_diffrn_reflns_theta_min          3.02
_diffrn_reflns_theta_max          27.48
_reflns_number_total              4394
_reflns_number_gt                 3837
_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.

 Hydrogen atoms on the water molecules O1w and O2w could not be located
 from the difference map. This is not surprising when heavy atoms are
 involved in the structure. The location of one of the hydrogens on each of
 the water molecules can be deduced from the short contact with the sulphate
 oxygen: O1w-H...O3 and O2w-H...O23, however the location of the second
 hydrogen is not certain.

 The second WGHT parameter is higher than usual due to the large difference
 in atom weights present in the structure.

 As there are 2 independent W2O8 units present in the structure (though half
 of each is related by symmetry) the formula is therefore that shown above.
 Checkcif brings up errors due to the manner it calculates Z and the formula,
 however the values given here are correct.

 O32 and O36 were modelled using the ISOR restraint due to the former being
 a non-positive definite, and the latter having a very small ADP in one
 direction. This appears to be a trend for oxygen atoms that are positioned
 within a lattice surrounded by 3 co-ordinating cations.
;
 
_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+23.9597P] 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          4394
_refine_ls_number_parameters      289
_refine_ls_number_restraints      18
_refine_ls_R_factor_all           0.0483
_refine_ls_R_factor_gt            0.0387
_refine_ls_wR_factor_ref          0.0827
_refine_ls_wR_factor_gt           0.0779
_refine_ls_goodness_of_fit_ref    1.119
_refine_ls_restrained_S_all       1.118
_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 -0.3243(15) -0.0386(13) 0.0882(6) 0.019(2) Uani 1 1 d . . .
H1 H -0.4531 -0.0316 0.1126 0.023 Uiso 1 1 calc R . .
C2 C -0.2083(14) -0.1515(12) 0.1261(6) 0.014(2) Uani 1 1 d . . .
C3 C -0.0207(14) -0.1586(12) 0.0959(6) 0.0131(19) Uani 1 1 d . . .
H3 H 0.0560 -0.2312 0.1248 0.016 Uiso 1 1 calc R . .
C4 C 0.0588(13) -0.0555(12) 0.0204(6) 0.0126(19) Uani 1 1 d . . .
C5 C -0.2508(14) 0.0599(14) 0.0168(7) 0.020(2) Uani 1 1 d . . .
H5 H -0.3303 0.1346 -0.0094 0.024 Uiso 1 1 calc R . .
O1 O -0.1619(9) -0.3825(8) 0.2471(4) 0.0121(13) Uani 1 1 d . . .
O2 O -0.3965(9) -0.1760(9) 0.2756(4) 0.0140(14) Uani 1 1 d . . .
O3 O -0.4525(9) -0.3892(9) 0.1980(4) 0.0137(14) Uani 1 1 d . . .
S1 S -0.3125(3) -0.2843(3) 0.21788(14) 0.0105(4) Uani 1 1 d . . .
C21 C 0.2485(14) -0.6484(12) 0.0688(6) 0.0131(19) Uani 1 1 d . . .
H21 H 0.3604 -0.6945 0.0833 0.016 Uiso 1 1 calc R . .
C22 C 0.0728(12) -0.6842(11) 0.1238(6) 0.0097(18) Uani 1 1 d . . .
C23 C -0.0907(13) -0.6246(12) 0.1042(6) 0.0124(19) Uani 1 1 d . . .
H23 H -0.2065 -0.6535 0.1413 0.015 Uiso 1 1 calc R . .
C24 C -0.0882(13) -0.5184(12) 0.0277(6) 0.014(2) Uani 1 1 d . . .
C25 C -0.2553(14) -0.4530(14) 0.0052(6) 0.019(2) Uani 1 1 d . . .
H25 H -0.3728 -0.4794 0.0415 0.023 Uiso 1 1 calc R . .
O21 O 0.1016(9) -0.6859(9) 0.2739(4) 0.0148(14) Uani 1 1 d . . .
O22 O -0.1147(9) -0.8844(8) 0.2464(4) 0.0140(14) Uani 1 1 d . . .
O23 O 0.2210(9) -0.9213(8) 0.2099(4) 0.0110(13) Uani 1 1 d U . .
S21 S 0.0692(3) -0.8035(3) 0.22033(14) 0.0090(4) Uani 1 1 d . . .
O1W O 0.2032(9) -0.3005(9) 0.2620(4) 0.0176(15) Uani 1 1 d . . .
O2W O -0.4925(10) -0.7997(10) 0.2646(5) 0.0209(16) Uani 1 1 d . . .
O31 O -0.3126(9) -0.6755(8) 0.3739(4) 0.0108(13) Uani 1 1 d . . .
O32 O -0.0855(9) -0.6520(8) 0.5124(4) 0.0117(13) Uani 1 1 d U . .
O33 O -0.0819(8) -0.9309(8) 0.4498(4) 0.0111(13) Uani 1 1 d . . .
O34 O -0.5770(9) -0.8448(8) 0.4859(4) 0.0144(14) Uani 1 1 d . . .
O35 O -0.6948(9) -0.5674(8) 0.3848(4) 0.0114(13) Uani 1 1 d . . .
O36 O -0.6283(8) -0.5702(8) 0.5504(4) 0.0089(13) Uani 1 1 d U . .
O37 O -0.3030(9) -0.9271(9) 0.6121(4) 0.0140(14) Uani 1 1 d . . .
O38 O 0.0711(9) -0.8237(8) 0.6259(4) 0.0120(13) Uani 1 1 d . . .
La1 La -0.03323(7) -0.48556(6) 0.37024(3) 0.00781(12) Uani 1 1 d . . .
La2 La -0.34937(7) -0.98592(6) 0.37284(3) 0.00791(12) Uani 1 1 d . . .
W1 W -0.07814(5) -0.86908(4) 0.55628(2) 0.00807(10) Uani 1 1 d . . .
W2 W -0.52622(5) -0.62816(4) 0.44272(2) 0.00780(10) Uani 1 1 d . . .
 
 
_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 C5 1.346(15) . ?
C1 C2 1.402(15) . ?
C2 C3 1.362(14) . ?
C2 S1 1.772(10) . ?
C3 C4 1.423(13) . ?
C4 C5 1.415(14) 2 ?
C4 C4 1.426(19) 2 ?
C5 C4 1.415(14) 2 ?
O1 S1 1.464(7) . ?
O1 La1 2.468(7) . ?
O2 S1 1.464(7) . ?
O2 La2 2.506(7) 1_565 ?
O3 S1 1.452(7) . ?
C21 C25 1.372(14) 2_545 ?
C21 C22 1.422(13) . ?
C22 C23 1.358(13) . ?
C22 S21 1.751(10) . ?
C23 C24 1.428(14) . ?
C24 C25 1.415(14) . ?
C24 C24 1.431(19) 2_545 ?
C25 C21 1.372(14) 2_545 ?
O21 S21 1.471(7) . ?
O21 La1 2.549(7) . ?
O22 S21 1.444(7) . ?
O22 La2 2.481(7) . ?
O23 S21 1.458(6) . ?
O1W La1 2.536(7) . ?
O2W La2 2.554(7) . ?
O31 W2 1.828(7) . ?
O31 La2 2.537(6) . ?
O31 La1 2.537(6) . ?
O32 W1 1.798(6) . ?
O32 La1 2.514(7) . ?
O32 La1 2.713(7) 2_546 ?
O33 W1 1.955(6) . ?
O33 W1 1.995(6) 2_536 ?
O33 La2 2.619(6) . ?
O34 W2 1.797(7) . ?
O34 La2 2.511(7) 2_436 ?
O34 La2 2.678(7) . ?
O35 W2 1.733(6) . ?
O35 La1 2.587(6) 1_455 ?
O36 W2 1.961(6) . ?
O36 W2 1.998(6) 2_446 ?
O36 La1 2.634(6) 2_446 ?
O37 W1 1.742(6) . ?
O37 La2 2.575(7) 2_436 ?
O38 W1 1.830(7) . ?
O38 La1 2.532(7) 2_546 ?
O38 La2 2.536(7) 2_536 ?
La1 O38 2.532(7) 2_546 ?
La1 O35 2.587(6) 1_655 ?
La1 O36 2.634(6) 2_446 ?
La1 O32 2.713(7) 2_546 ?
La1 W1 3.4769(6) 2_546 ?
La1 W2 3.6725(6) . ?
La2 O2 2.506(7) 1_545 ?
La2 O34 2.511(7) 2_436 ?
La2 O38 2.536(7) 2_536 ?
La2 O37 2.575(7) 2_436 ?
La2 W2 3.4601(6) . ?
La2 W1 3.6596(6) 2_536 ?
W1 O33 1.995(6) 2_536 ?
W1 W1 3.1465(7) 2_536 ?
W1 La1 3.4769(6) 2_546 ?
W1 La2 3.6596(6) 2_536 ?
W2 O36 1.998(6) 2_446 ?
W2 W2 3.1421(7) 2_446 ?
 
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
C5 C1 C2 119.2(10) . . ?
C3 C2 C1 122.4(9) . . ?
C3 C2 S1 119.8(8) . . ?
C1 C2 S1 117.7(8) . . ?
C2 C3 C4 118.9(9) . . ?
C5 C4 C3 122.6(9) 2 . ?
C5 C4 C4 118.1(11) 2 2 ?
C3 C4 C4 119.3(11) . 2 ?
C1 C5 C4 122.0(10) . 2 ?
S1 O1 La1 143.3(4) . . ?
S1 O2 La2 148.0(4) . 1_565 ?
O3 S1 O1 112.0(4) . . ?
O3 S1 O2 112.2(4) . . ?
O1 S1 O2 111.4(4) . . ?
O3 S1 C2 106.9(4) . . ?
O1 S1 C2 107.1(4) . . ?
O2 S1 C2 106.9(4) . . ?
C25 C21 C22 119.6(9) 2_545 . ?
C23 C22 C21 121.8(9) . . ?
C23 C22 S21 119.4(7) . . ?
C21 C22 S21 118.8(7) . . ?
C22 C23 C24 120.0(9) . . ?
C25 C24 C23 121.7(9) . . ?
C25 C24 C24 119.9(11) . 2_545 ?
C23 C24 C24 118.4(11) . 2_545 ?
C21 C25 C24 120.3(9) 2_545 . ?
S21 O21 La1 148.7(4) . . ?
S21 O22 La2 140.5(4) . . ?
O22 S21 O23 113.1(4) . . ?
O22 S21 O21 111.9(4) . . ?
O23 S21 O21 111.6(4) . . ?
O22 S21 C22 106.5(4) . . ?
O23 S21 C22 106.5(4) . . ?
O21 S21 C22 106.6(4) . . ?
W2 O31 La2 103.7(3) . . ?
W2 O31 La1 113.6(3) . . ?
La2 O31 La1 133.5(3) . . ?
W1 O32 La1 135.9(3) . . ?
W1 O32 La1 98.8(3) . 2_546 ?
La1 O32 La1 118.0(2) . 2_546 ?
W1 O33 W1 105.6(3) . 2_536 ?
W1 O33 La2 134.2(3) . . ?
W1 O33 La2 104.2(3) 2_536 . ?
W2 O34 La2 136.1(3) . 2_436 ?
W2 O34 La2 99.4(3) . . ?
La2 O34 La2 115.9(2) 2_436 . ?
W2 O35 La1 152.1(3) . 1_455 ?
W2 O36 W2 105.1(3) . 2_446 ?
W2 O36 La1 134.8(3) . 2_446 ?
W2 O36 La1 104.1(3) 2_446 2_446 ?
W1 O37 La2 153.7(4) . 2_436 ?
W1 O38 La1 104.6(3) . 2_546 ?
W1 O38 La2 112.9(3) . 2_536 ?
La1 O38 La2 133.0(3) 2_546 2_536 ?
O1 La1 O32 148.1(2) . . ?
O1 La1 O38 76.7(2) . 2_546 ?
O32 La1 O38 110.9(2) . 2_546 ?
O1 La1 O1W 68.1(2) . . ?
O32 La1 O1W 143.7(2) . . ?
O38 La1 O1W 66.4(2) 2_546 . ?
O1 La1 O31 73.0(2) . . ?
O32 La1 O31 77.1(2) . . ?
O38 La1 O31 121.4(2) 2_546 . ?
O1W La1 O31 136.9(2) . . ?
O1 La1 O21 77.3(2) . . ?
O32 La1 O21 106.4(2) . . ?
O38 La1 O21 141.3(2) 2_546 . ?
O1W La1 O21 77.4(2) . . ?
O31 La1 O21 76.7(2) . . ?
O1 La1 O35 130.3(2) . 1_655 ?
O32 La1 O35 77.9(2) . 1_655 ?
O38 La1 O35 109.4(2) 2_546 1_655 ?
O1W La1 O35 70.0(2) . 1_655 ?
O31 La1 O35 128.5(2) . 1_655 ?
O21 La1 O35 68.4(2) . 1_655 ?
O1 La1 O36 84.3(2) . 2_446 ?
O32 La1 O36 70.7(2) . 2_446 ?
O38 La1 O36 69.6(2) 2_546 2_446 ?
O1W La1 O36 132.1(2) . 2_446 ?
O31 La1 O36 58.7(2) . 2_446 ?
O21 La1 O36 135.0(2) . 2_446 ?
O35 La1 O36 145.0(2) 1_655 2_446 ?
O1 La1 O32 136.4(2) . 2_546 ?
O32 La1 O32 62.0(2) . 2_546 ?
O38 La1 O32 59.9(2) 2_546 2_546 ?
O1W La1 O32 89.6(2) . 2_546 ?
O31 La1 O32 132.4(2) . 2_546 ?
O21 La1 O32 135.7(2) . 2_546 ?
O35 La1 O32 67.4(2) 1_655 2_546 ?
O36 La1 O32 84.25(19) 2_446 2_546 ?
O1 La1 W1 105.83(16) . 2_546 ?
O32 La1 W1 90.30(15) . 2_546 ?
O38 La1 W1 30.62(15) 2_546 2_546 ?
O1W La1 W1 69.97(17) . 2_546 ?
O31 La1 W1 140.49(15) . 2_546 ?
O21 La1 W1 142.63(15) . 2_546 ?
O35 La1 W1 83.38(15) 1_655 2_546 ?
O36 La1 W1 81.82(13) 2_446 2_546 ?
O32 La1 W1 30.74(13) 2_546 2_546 ?
O1 La1 W2 79.73(15) . . ?
O32 La1 W2 68.53(15) . . ?
O38 La1 W2 99.28(15) 2_546 . ?
O1W La1 W2 146.89(16) . . ?
O31 La1 W2 27.14(15) . . ?
O21 La1 W2 103.80(15) . . ?
O35 La1 W2 141.92(15) 1_655 . ?
O36 La1 W2 31.86(13) 2_446 . ?
O32 La1 W2 109.36(14) 2_546 . ?
W1 La1 W2 113.465(16) 2_546 . ?
O22 La2 O2 75.3(2) . 1_545 ?
O22 La2 O34 148.9(2) . 2_436 ?
O2 La2 O34 107.2(2) 1_545 2_436 ?
O22 La2 O38 73.1(2) . 2_536 ?
O2 La2 O38 77.2(2) 1_545 2_536 ?
O34 La2 O38 77.2(2) 2_436 2_536 ?
O22 La2 O31 76.1(2) . . ?
O2 La2 O31 139.0(2) 1_545 . ?
O34 La2 O31 112.6(2) 2_436 . ?
O38 La2 O31 121.0(2) 2_536 . ?
O22 La2 O2W 67.4(2) . . ?
O2 La2 O2W 75.9(2) 1_545 . ?
O34 La2 O2W 143.8(2) 2_436 . ?
O38 La2 O2W 136.4(2) 2_536 . ?
O31 La2 O2W 66.2(2) . . ?
O22 La2 O37 128.8(2) . 2_436 ?
O2 La2 O37 67.4(2) 1_545 2_436 ?
O34 La2 O37 77.5(2) 2_436 2_436 ?
O38 La2 O37 127.3(2) 2_536 2_436 ?
O31 La2 O37 111.3(2) . 2_436 ?
O2W La2 O37 70.4(2) . 2_436 ?
O22 La2 O33 85.3(2) . . ?
O2 La2 O33 135.6(2) 1_545 . ?
O34 La2 O33 71.3(2) 2_436 . ?
O38 La2 O33 58.9(2) 2_536 . ?
O31 La2 O33 69.6(2) . . ?
O2W La2 O33 132.1(2) . . ?
O37 La2 O33 145.7(2) 2_436 . ?
O22 La2 O34 136.0(2) . . ?
O2 La2 O34 135.0(2) 1_545 . ?
O34 La2 O34 64.1(2) 2_436 . ?
O38 La2 O34 134.6(2) 2_536 . ?
O31 La2 O34 60.4(2) . . ?
O2W La2 O34 87.9(2) . . ?
O37 La2 O34 67.6(2) 2_436 . ?
O33 La2 O34 85.9(2) . . ?
O22 La2 W2 105.15(16) . . ?
O2 La2 W2 141.05(16) 1_545 . ?
O34 La2 W2 92.04(15) 2_436 . ?
O38 La2 W2 141.14(15) 2_536 . ?
O31 La2 W2 30.88(15) . . ?
O2W La2 W2 69.11(17) . . ?
O37 La2 W2 84.93(15) 2_436 . ?
O33 La2 W2 82.28(14) . . ?
O34 La2 W2 30.83(14) . . ?
O22 La2 W1 80.94(16) . 2_536 ?
O2 La2 W1 104.63(15) 1_545 2_536 ?
O34 La2 W1 68.31(15) 2_436 2_536 ?
O38 La2 W1 27.43(15) 2_536 2_536 ?
O31 La2 W1 99.26(14) . 2_536 ?
O2W La2 W1 147.25(17) . 2_536 ?
O37 La2 W1 140.89(16) 2_436 2_536 ?
O33 La2 W1 31.90(14) . 2_536 ?
O34 La2 W1 110.99(15) . 2_536 ?
W2 La2 W1 113.978(16) . 2_536 ?
O37 W1 O32 106.6(3) . . ?
O37 W1 O38 109.1(3) . . ?
O32 W1 O38 92.5(3) . . ?
O37 W1 O33 103.3(3) . . ?
O32 W1 O33 89.8(3) . . ?
O38 W1 O33 145.3(3) . . ?
O37 W1 O33 110.5(3) . 2_536 ?
O32 W1 O33 142.0(3) . 2_536 ?
O38 W1 O33 82.9(3) . 2_536 ?
O33 W1 O33 74.4(3) . 2_536 ?
O37 W1 W1 111.4(2) . 2_536 ?
O32 W1 W1 119.8(2) . 2_536 ?
O38 W1 W1 115.6(2) . 2_536 ?
O33 W1 W1 37.63(19) . 2_536 ?
O33 W1 W1 36.76(18) 2_536 2_536 ?
O37 W1 La1 103.5(2) . 2_546 ?
O32 W1 La1 50.4(2) . 2_546 ?
O38 W1 La1 44.8(2) . 2_546 ?
O33 W1 La1 137.0(2) . 2_546 ?
O33 W1 La1 124.86(18) 2_536 2_546 ?
W1 W1 La1 144.749(19) 2_536 2_546 ?
O37 W1 La2 122.9(2) . 2_536 ?
O32 W1 La2 117.7(2) . 2_536 ?
O38 W1 La2 39.7(2) . 2_536 ?
O33 W1 La2 110.61(18) . 2_536 ?
O33 W1 La2 43.94(18) 2_536 2_536 ?
W1 W1 La2 76.245(15) 2_536 2_536 ?
La1 W1 La2 81.226(14) 2_546 2_536 ?
O35 W2 O34 106.4(3) . . ?
O35 W2 O31 108.2(3) . . ?
O34 W2 O31 92.8(3) . . ?
O35 W2 O36 105.0(3) . . ?
O34 W2 O36 88.8(3) . . ?
O31 W2 O36 144.8(3) . . ?
O35 W2 O36 110.2(3) . 2_446 ?
O34 W2 O36 142.6(3) . 2_446 ?
O31 W2 O36 82.8(3) . 2_446 ?
O36 W2 O36 74.9(3) . 2_446 ?
O35 W2 W2 112.4(2) . 2_446 ?
O34 W2 W2 119.5(2) . 2_446 ?
O31 W2 W2 115.5(2) . 2_446 ?
O36 W2 W2 37.89(17) . 2_446 ?
O36 W2 W2 37.06(18) 2_446 2_446 ?
O35 W2 La2 103.5(2) . . ?
O34 W2 La2 49.8(2) . . ?
O31 W2 La2 45.43(19) . . ?
O36 W2 La2 135.01(19) . . ?
O36 W2 La2 125.15(18) 2_446 . ?
W2 W2 La2 143.85(2) 2_446 . ?
O35 W2 La1 121.0(2) . . ?
O34 W2 La1 118.8(2) . . ?
O31 W2 La1 39.29(19) . . ?
O36 W2 La1 111.36(17) . . ?
O36 W2 La1 44.08(18) 2_446 . ?
W2 W2 La1 76.730(15) 2_446 . ?
La2 W2 La1 81.585(14) . . ?
 
_diffrn_measured_fraction_theta_max    0.996
_diffrn_reflns_theta_full              27.48
_diffrn_measured_fraction_theta_full   0.996
_refine_diff_density_max    2.116
_refine_diff_density_min   -1.758
_refine_diff_density_rms    0.355
