 
data_22
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'H54 O68 Sr4 W12'
_chemical_formula_weight          3699.11
 
loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'O'  'O'   0.0106   0.0060
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Sr'  'Sr'  -1.5307   3.2498
 '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'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_symmetry_cell_setting            'monoclinic'
_symmetry_space_group_name_H-M    'P 21/n'
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x+1/2, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x-1/2, -y-1/2, z-1/2'
 
_cell_length_a                    15.8131(4)
_cell_length_b                    12.3772(3)
_cell_length_c                    15.9268(4)
_cell_angle_alpha                 90.00
_cell_angle_beta                  101.166(2)
_cell_angle_gamma                 90.00
_cell_volume                      3058.22(13)
_cell_formula_units_Z             2
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     ?
_cell_measurement_theta_min       3.09
_cell_measurement_theta_max       29.14
 
_exptl_crystal_description       'prism'
_exptl_crystal_colour            'colorless'
_exptl_crystal_size_max           0.21
_exptl_crystal_size_mid           0.11
_exptl_crystal_size_min           0.10
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     4.017
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              3276
_exptl_absorpt_coefficient_mu     26.044
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.579
_exptl_absorpt_correction_T_max   1.000
_exptl_absorpt_process_details    '(SADABS; Bruker, 2002)'
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       293(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   ?
_diffrn_measurement_method        ?
_diffrn_detector_area_resol_mean  ?
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             11876
_diffrn_reflns_av_R_equivalents   0.0408
_diffrn_reflns_av_sigmaI/netI     0.0705
_diffrn_reflns_limit_h_min        -18
_diffrn_reflns_limit_h_max        17
_diffrn_reflns_limit_k_min        -14
_diffrn_reflns_limit_k_max        11
_diffrn_reflns_limit_l_min        -14
_diffrn_reflns_limit_l_max        18
_diffrn_reflns_theta_min          3.10
_diffrn_reflns_theta_max          25.00
_reflns_number_total              5339
_reflns_number_gt                 3510
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection        'SMART (Bruker, 2002)'
_computing_cell_refinement        'SMART (Bruker, 2002)'
_computing_data_reduction         'SAINT (Bruker, 2002)'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     'DIAMOND (Brandenburg, 1999)'
_computing_publication_material   '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)+(0.0010P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    none
_refine_ls_hydrogen_treatment     none
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          5339
_refine_ls_number_parameters      383
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0536
_refine_ls_R_factor_gt            0.0335
_refine_ls_wR_factor_ref          0.0558
_refine_ls_wR_factor_gt           0.0547
_refine_ls_goodness_of_fit_ref    1.126
_refine_ls_restrained_S_all       1.126
_refine_ls_shift/su_max           0.005
_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
W1 W 0.34152(3) 0.06836(5) 0.04247(4) 0.02811(14) Uani 1 1 d . . .
W2 W 0.48100(4) -0.06450(5) 0.24249(4) 0.02974(14) Uani 1 1 d . . .
W3 W 0.35334(4) -0.20141(5) 0.05367(4) 0.03021(16) Uani 1 1 d . . .
W4 W 0.46739(4) 0.20127(5) 0.23772(4) 0.03063(16) Uani 1 1 d . . .
W5 W 0.48191(4) 0.31568(5) 0.05281(4) 0.02838(15) Uani 1 1 d . . .
W6 W 0.36769(3) -0.07784(5) -0.12935(4) 0.02748(14) Uani 1 1 d . . .
Sr1 Sr 0.32662(9) 0.45537(11) -0.15497(10) 0.0381(4) Uani 1 1 d . . .
Sr2 Sr 0.26916(9) 0.05438(12) 0.32311(10) 0.0389(4) Uani 1 1 d . . .
O1 O 0.4071(6) 0.0605(7) 0.1576(6) 0.032(2) Uani 1 1 d . . .
O2 O 0.4145(6) 0.2885(8) 0.1461(6) 0.031(2) Uani 1 1 d . . .
O3 O 0.2911(5) -0.0802(8) 0.0744(6) 0.030(2) Uani 1 1 d . . .
O4 O 0.5352(6) 0.2941(8) 0.2969(7) 0.038(3) Uani 1 1 d . . .
O5 O 0.4011(6) -0.0627(9) 0.3042(7) 0.041(2) Uani 1 1 d . . .
O6 O 0.4277(5) -0.0617(7) 0.0096(5) 0.0205(19) Uani 1 1 d . . .
O7 O 0.4502(6) -0.1880(8) -0.1353(6) 0.031(2) Uani 1 1 d . . .
O8 O 0.5297(5) 0.0750(8) 0.2839(6) 0.033(2) Uani 1 1 d . . .
O9 O 0.2963(6) -0.0976(8) -0.2210(7) 0.044(3) Uani 1 1 d . . .
O10 O 0.2981(5) 0.0181(7) -0.0742(6) 0.024(2) Uani 1 1 d . . .
O11 O 0.3122(6) -0.1958(8) -0.0643(7) 0.033(2) Uani 1 1 d . . .
O12 O 0.5492(6) 0.4100(8) 0.1100(7) 0.042(3) Uani 1 1 d . . .
O13 O 0.3820(7) 0.1976(8) 0.2897(8) 0.049(3) Uani 1 1 d . . .
O14 O 0.5487(7) 0.2823(7) -0.0299(7) 0.037(3) Uani 1 1 d . . .
O15 O 0.4337(6) 0.0290(7) -0.1536(7) 0.038(3) Uani 1 1 d . . .
O16 O 0.4304(6) -0.1676(8) 0.1624(7) 0.038(3) Uani 1 1 d . . .
O17 O 0.4004(6) 0.3934(7) -0.0085(6) 0.033(2) Uani 1 1 d . . .
O18 O 0.4079(6) 0.1676(7) 0.0052(6) 0.025(2) Uani 1 1 d . . .
O19 O 0.5585(6) -0.1439(8) 0.3021(8) 0.044(3) Uani 1 1 d . . .
O20 O 0.2924(6) -0.3020(9) 0.0890(7) 0.040(3) Uani 1 1 d . . .
O21 O 0.2531(7) 0.1444(8) 0.0565(8) 0.045(3) Uani 1 1 d . . .
O1W O 0.2971(9) 0.2448(10) -0.1556(9) 0.073(4) Uani 1 1 d . . .
O2W O 0.3460(9) 0.5448(14) -0.2955(9) 0.100(6) Uani 1 1 d . . .
O3W O 0.1835(9) 0.3984(17) -0.0933(9) 0.116(7) Uani 1 1 d . . .
O4W O 0.4549(8) 0.3546(10) -0.2033(11) 0.085(5) Uani 1 1 d . . .
O5W O 0.2350(9) 0.6265(12) -0.1483(17) 0.166(11) Uani 1 1 d . . .
O6W O 0.2535(7) -0.1183(9) 0.4083(10) 0.064(4) Uani 1 1 d . . .
O7W O 0.3659(8) 0.0779(13) 0.4719(9) 0.077(4) Uani 1 1 d . . .
O8W O 0.2098(9) -0.0913(11) 0.2095(9) 0.077(4) Uani 1 1 d . . .
O9W O 0.1834(8) 0.1941(11) 0.2103(9) 0.075(4) Uani 1 1 d . . .
O10W O 0.1037(8) 0.0170(10) 0.3125(12) 0.091(6) Uani 1 1 d . . .
O11W O 0.5397(11) 0.1442(17) 0.5187(13) 0.135(7) Uani 1 1 d . . .
O12W O 0.0816(14) 0.161(3) -0.0239(17) 0.216(14) Uani 1 1 d . . .
O13W O 0.041(2) 0.028(2) 0.133(2) 0.098(10) Uiso 0.50 1 d P . .
O14W O 0.1234(17) -0.149(3) -0.048(4) 0.17(2) Uani 0.50 1 d P . .
 
 
_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
W1 O21 1.735(9) . ?
W1 O18 1.791(8) . ?
W1 O1 1.927(10) . ?
W1 O10 1.954(9) . ?
W1 O3 2.105(9) . ?
W1 O6 2.236(8) . ?
W2 O19 1.709(12) . ?
W2 O5 1.745(9) . ?
W2 O16 1.871(10) . ?
W2 O8 1.952(10) . ?
W2 O15 2.181(8) 3_655 ?
W2 O1 2.230(10) . ?
W3 O20 1.734(10) . ?
W3 O3 1.858(9) . ?
W3 O11 1.867(10) . ?
W3 O14 1.941(9) 3_655 ?
W3 O16 1.960(11) . ?
W3 O6 2.276(8) . ?
W4 O13 1.716(10) . ?
W4 O4 1.723(10) . ?
W4 O2 1.877(10) . ?
W4 O8 1.917(10) . ?
W4 O1 2.259(10) . ?
W4 O7 2.283(8) 3_655 ?
W5 O12 1.718(11) . ?
W5 O17 1.747(10) . ?
W5 O14 1.888(9) . ?
W5 O2 2.017(8) . ?
W5 O7 2.197(10) 3_655 ?
W5 O18 2.226(9) . ?
W6 O9 1.682(12) . ?
W6 O15 1.773(9) . ?
W6 O7 1.902(9) . ?
W6 O10 1.941(8) . ?
W6 O11 2.080(9) . ?
W6 O6 2.242(9) . ?
Sr1 O17 2.518(11) . ?
Sr1 O2W 2.567(13) . ?
Sr1 O12 2.569(10) 3_665 ?
Sr1 O9 2.573(12) 2_554 ?
Sr1 O5W 2.579(12) . ?
Sr1 O4W 2.620(12) . ?
Sr1 O1W 2.647(13) . ?
Sr1 O3W 2.728(12) . ?
Sr2 O20 2.568(10) 2 ?
Sr2 O6W 2.568(12) . ?
Sr2 O7W 2.576(14) . ?
Sr2 O8W 2.598(14) . ?
Sr2 O5 2.605(10) . ?
Sr2 O10W 2.630(11) . ?
Sr2 O13 2.641(11) . ?
Sr2 O9W 2.668(15) . ?
O7 W5 2.197(10) 3_655 ?
O7 W4 2.283(8) 3_655 ?
O9 Sr1 2.573(12) 2_544 ?
O12 Sr1 2.569(10) 3_665 ?
O14 W3 1.941(9) 3_655 ?
O15 W2 2.181(8) 3_655 ?
O20 Sr2 2.568(10) 2_545 ?
 
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
O21 W1 O18 102.1(4) . . ?
O21 W1 O1 101.7(5) . . ?
O18 W1 O1 96.2(4) . . ?
O21 W1 O10 98.7(5) . . ?
O18 W1 O10 91.4(4) . . ?
O1 W1 O10 156.1(4) . . ?
O21 W1 O3 95.2(4) . . ?
O18 W1 O3 162.4(4) . . ?
O1 W1 O3 83.4(4) . . ?
O10 W1 O3 82.6(4) . . ?
O21 W1 O6 164.5(4) . . ?
O18 W1 O6 89.6(3) . . ?
O1 W1 O6 86.9(3) . . ?
O10 W1 O6 70.5(3) . . ?
O3 W1 O6 72.8(3) . . ?
O19 W2 O5 102.4(5) . . ?
O19 W2 O16 98.8(5) . . ?
O5 W2 O16 97.6(4) . . ?
O19 W2 O8 97.3(5) . . ?
O5 W2 O8 94.6(4) . . ?
O16 W2 O8 157.2(4) . . ?
O19 W2 O15 90.6(4) . 3_655 ?
O5 W2 O15 165.8(4) . 3_655 ?
O16 W2 O15 86.1(4) . 3_655 ?
O8 W2 O15 77.8(3) . 3_655 ?
O19 W2 O1 166.2(4) . . ?
O5 W2 O1 88.9(4) . . ?
O16 W2 O1 87.4(4) . . ?
O8 W2 O1 73.6(4) . . ?
O15 W2 O1 77.5(3) 3_655 . ?
O20 W3 O3 100.1(4) . . ?
O20 W3 O11 104.3(4) . . ?
O3 W3 O11 93.2(4) . . ?
O20 W3 O14 102.0(4) . 3_655 ?
O3 W3 O14 157.0(4) . 3_655 ?
O11 W3 O14 87.6(4) . 3_655 ?
O20 W3 O16 99.0(5) . . ?
O3 W3 O16 86.1(4) . . ?
O11 W3 O16 156.5(4) . . ?
O14 W3 O16 84.2(4) 3_655 . ?
O20 W3 O6 176.5(4) . . ?
O3 W3 O6 76.4(3) . . ?
O11 W3 O6 76.2(4) . . ?
O14 W3 O6 81.5(3) 3_655 . ?
O16 W3 O6 80.8(3) . . ?
O13 W4 O4 102.6(5) . . ?
O13 W4 O2 96.7(5) . . ?
O4 W4 O2 100.3(5) . . ?
O13 W4 O8 100.8(4) . . ?
O4 W4 O8 96.6(4) . . ?
O2 W4 O8 152.4(4) . . ?
O13 W4 O1 88.1(4) . . ?
O4 W4 O1 166.8(4) . . ?
O2 W4 O1 85.9(4) . . ?
O8 W4 O1 73.5(4) . . ?
O13 W4 O7 162.7(5) . 3_655 ?
O4 W4 O7 93.3(4) . 3_655 ?
O2 W4 O7 73.5(4) . 3_655 ?
O8 W4 O7 83.9(3) . 3_655 ?
O1 W4 O7 77.2(3) . 3_655 ?
O12 W5 O17 103.7(5) . . ?
O12 W5 O14 98.4(4) . . ?
O17 W5 O14 100.5(4) . . ?
O12 W5 O2 94.8(4) . . ?
O17 W5 O2 93.7(4) . . ?
O14 W5 O2 157.6(4) . . ?
O12 W5 O7 89.5(4) . 3_655 ?
O17 W5 O7 162.2(3) . 3_655 ?
O14 W5 O7 89.1(4) . 3_655 ?
O2 W5 O7 73.0(3) . 3_655 ?
O12 W5 O18 166.1(4) . . ?
O17 W5 O18 88.9(4) . . ?
O14 W5 O18 84.9(4) . . ?
O2 W5 O18 78.2(3) . . ?
O7 W5 O18 77.0(3) 3_655 . ?
O9 W6 O15 104.2(5) . . ?
O9 W6 O7 101.8(4) . . ?
O15 W6 O7 94.9(4) . . ?
O9 W6 O10 97.9(4) . . ?
O15 W6 O10 93.0(4) . . ?
O7 W6 O10 156.3(4) . . ?
O9 W6 O11 93.0(4) . . ?
O15 W6 O11 162.7(5) . . ?
O7 W6 O11 83.2(4) . . ?
O10 W6 O11 82.7(3) . . ?
O9 W6 O6 162.7(3) . . ?
O15 W6 O6 89.7(4) . . ?
O7 W6 O6 87.1(4) . . ?
O10 W6 O6 70.6(3) . . ?
O11 W6 O6 73.1(4) . . ?
O17 Sr1 O2W 145.8(3) . . ?
O17 Sr1 O12 75.4(3) . 3_665 ?
O2W Sr1 O12 75.5(4) . 3_665 ?
O17 Sr1 O9 141.2(3) . 2_554 ?
O2W Sr1 O9 68.9(3) . 2_554 ?
O12 Sr1 O9 143.3(3) 3_665 2_554 ?
O17 Sr1 O5W 112.0(6) . . ?
O2W Sr1 O5W 81.0(7) . . ?
O12 Sr1 O5W 82.0(4) 3_665 . ?
O9 Sr1 O5W 83.9(5) 2_554 . ?
O17 Sr1 O4W 83.2(4) . . ?
O2W Sr1 O4W 73.7(5) . . ?
O12 Sr1 O4W 78.3(4) 3_665 . ?
O9 Sr1 O4W 99.5(4) 2_554 . ?
O5W Sr1 O4W 151.1(6) . . ?
O17 Sr1 O1W 75.7(4) . . ?
O2W Sr1 O1W 118.2(5) . . ?
O12 Sr1 O1W 139.8(4) 3_665 . ?
O9 Sr1 O1W 68.9(4) 2_554 . ?
O5W Sr1 O1W 135.1(5) . . ?
O4W Sr1 O1W 71.1(4) . . ?
O17 Sr1 O3W 81.7(4) . . ?
O2W Sr1 O3W 132.2(5) . . ?
O12 Sr1 O3W 135.2(4) 3_665 . ?
O9 Sr1 O3W 69.8(4) 2_554 . ?
O5W Sr1 O3W 71.7(6) . . ?
O4W Sr1 O3W 136.5(5) . . ?
O1W Sr1 O3W 65.7(5) . . ?
O20 Sr2 O6W 101.7(4) 2 . ?
O20 Sr2 O7W 68.9(4) 2 . ?
O6W Sr2 O7W 73.1(5) . . ?
O20 Sr2 O8W 137.4(4) 2 . ?
O6W Sr2 O8W 74.4(4) . . ?
O7W Sr2 O8W 142.1(5) . . ?
O20 Sr2 O5 147.7(3) 2 . ?
O6W Sr2 O5 76.1(3) . . ?
O7W Sr2 O5 79.8(4) . . ?
O8W Sr2 O5 73.9(4) . . ?
O20 Sr2 O10W 71.3(4) 2 . ?
O6W Sr2 O10W 72.0(4) . . ?
O7W Sr2 O10W 119.0(5) . . ?
O8W Sr2 O10W 67.2(4) . . ?
O5 Sr2 O10W 134.7(4) . . ?
O20 Sr2 O13 89.3(3) 2 . ?
O6W Sr2 O13 143.4(4) . . ?
O7W Sr2 O13 78.8(4) . . ?
O8W Sr2 O13 119.5(3) . . ?
O5 Sr2 O13 76.3(3) . . ?
O10W Sr2 O13 143.9(4) . . ?
O20 Sr2 O9W 73.8(4) 2 . ?
O6W Sr2 O9W 143.8(4) . . ?
O7W Sr2 O9W 132.8(5) . . ?
O8W Sr2 O9W 85.0(5) . . ?
O5 Sr2 O9W 126.6(3) . . ?
O10W Sr2 O9W 72.6(4) . . ?
O13 Sr2 O9W 72.8(4) . . ?
W1 O1 W2 137.2(5) . . ?
W1 O1 W4 126.1(4) . . ?
W2 O1 W4 94.5(4) . . ?
W4 O2 W5 116.7(4) . . ?
W3 O3 W1 115.1(4) . . ?
W2 O5 Sr2 139.1(6) . . ?
W1 O6 W6 97.7(3) . . ?
W1 O6 W3 95.8(3) . . ?
W6 O6 W3 95.3(3) . . ?
W6 O7 W5 138.3(5) . 3_655 ?
W6 O7 W4 125.4(5) . 3_655 ?
W5 O7 W4 95.5(3) 3_655 3_655 ?
W4 O8 W2 116.9(5) . . ?
W6 O9 Sr1 155.5(5) . 2_544 ?
W6 O10 W1 120.0(4) . . ?
W3 O11 W6 115.4(5) . . ?
W5 O12 Sr1 161.8(5) . 3_665 ?
W4 O13 Sr2 137.8(5) . . ?
W5 O14 W3 145.5(6) . 3_655 ?
W6 O15 W2 139.1(5) . 3_655 ?
W2 O16 W3 149.1(6) . . ?
W5 O17 Sr1 147.7(4) . . ?
W1 O18 W5 139.1(5) . . ?
W3 O20 Sr2 165.3(6) . 2_545 ?
 
_diffrn_measured_fraction_theta_max    0.993
_diffrn_reflns_theta_full              25.00
_diffrn_measured_fraction_theta_full   0.993
_refine_diff_density_max    2.032
_refine_diff_density_min   -1.240
_refine_diff_density_rms    0.258
