 
data_c:\crystal\x-red32\y2mo3o 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum             'Mo3 O12 Y2' 
_chemical_formula_weight          657.64 
 
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'Y'  'Y'  -2.7962   3.5667 
 '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' 
 'O'  'O'   0.0106   0.0060 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            orthorhombic 
_symmetry_space_group_name_H-M    Pba2
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, -y, z' 
 '-x+1/2, y+1/2, z' 
 'x+1/2, -y+1/2, z' 
 
_cell_length_a                    10.3021(3) 
_cell_length_b                    10.3241(3) 
_cell_length_c                    10.5725(3) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 90.00 
_cell_volume                      1124.49(6) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     36720
_cell_measurement_theta_min       0.41
_cell_measurement_theta_max       35.63
 
_exptl_crystal_description        'lath-shaped' 
_exptl_crystal_colour             colourless
_exptl_crystal_size_max           0.069 
_exptl_crystal_size_mid           0.058
_exptl_crystal_size_min           0.030 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     3.885 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1200 
_exptl_absorpt_coefficient_mu     13.514 
_exptl_absorpt_correction_type    numerical
_exptl_absorpt_correction_T_min   0.3597 
_exptl_absorpt_correction_T_max   0.6108
_exptl_absorpt_process_details    
'programs X-SHAPE and HABITUS by w. Herrendorf, Univ. Giessen, 1995' 
 
_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   'Nonius Kappa-CCD'
_diffrn_measurement_method        'four-circle, ccd-detector'
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             49356 
_diffrn_reflns_av_R_equivalents   0.1005 
_diffrn_reflns_av_sigmaI/netI     0.0470 
_diffrn_reflns_limit_h_min        -16 
_diffrn_reflns_limit_h_max        16 
_diffrn_reflns_limit_k_min        -16 
_diffrn_reflns_limit_k_max        16 
_diffrn_reflns_limit_l_min        -17 
_diffrn_reflns_limit_l_max        17 
_diffrn_reflns_theta_min          2.79 
_diffrn_reflns_theta_max          35.65 
_reflns_number_total              5187 
_reflns_number_gt                 4585 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        'Nonius Collect-Software'
_computing_cell_refinement        'Denzo (W. Minor & Z. Otwinowski)'
_computing_data_reduction         'Denzo (W. Minor & Z. Otwinowski)'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1997)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_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 > 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)+(0.0308P)²+2.3454P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_refine_ls_extinction_method      SHELXL 
_refine_ls_extinction_coef        0.00166(12) 
_refine_ls_extinction_expression 
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^' 
_refine_ls_abs_structure_details 
 'Flack H D (1983), Acta Cryst. A39, 876-881' 
_refine_ls_abs_structure_Flack    -0.014(4) 
_refine_ls_number_reflns          5187 
_refine_ls_number_parameters      156 
_refine_ls_number_restraints      1 
_refine_ls_R_factor_all           0.0470 
_refine_ls_R_factor_gt            0.0370 
_refine_ls_wR_factor_ref          0.0755 
_refine_ls_wR_factor_gt           0.0721 
_refine_ls_goodness_of_fit_ref    1.032 
_refine_ls_restrained_S_all       1.032 
_refine_ls_shift/su_max           0.002 
_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 
Y1 Y 0.31369(16) 0.99654(13) 0.73702(11) 0.0081(3) Uani 1 1 d . . . 
Y2 Y 0.00547(11) 0.81362(15) 0.26206(12) 0.0094(3) Uani 1 1 d . . . 
Mo1 Mo 0.24341(14) 0.24428(15) 1.0003(3) 0.00998(8) Uani 1 1 d . . . 
Mo2 Mo 0.29545(13) 0.99026(8) 0.35711(9) 0.0094(2) Uani 1 1 d . . . 
Mo3 Mo 0.9974(2) 0.79347(13) 0.64275(9) 0.0088(2) Uani 1 1 d . . . 
O1 O 0.1697(11) 0.3581(10) 0.9009(10) 0.0210(19) Uani 1 1 d . . . 
O2 O 0.6811(11) 0.8748(11) 0.9051(11) 0.025(2) Uani 1 1 d . . . 
O3 O 0.8746(9) 0.8288(9) 0.0923(10) 0.0171(17) Uani 1 1 d . . . 
O4 O 0.3578(9) 0.3186(10) 0.1002(10) 0.0178(17) Uani 1 1 d . . . 
O5 O 0.1192(8) 0.6205(7) 0.2938(8) 0.0214(16) Uani 1 1 d . . . 
O6 O 0.6505(8) 0.1591(7) 0.3040(8) 0.0232(17) Uani 1 1 d . . . 
O7 O 0.1189(7) 0.8815(7) 0.7193(8) 0.0217(15) Uani 1 1 d . . . 
O8 O 0.6579(8) 0.3494(8) 0.6849(8) 0.0232(15) Uani 1 1 d . . . 
O9 O 0.3065(14) 0.9895(8) 0.5177(13) 0.030(3) Uani 1 1 d . . . 
O10 O 0.0163(7) 0.8065(12) 0.4766(12) 0.020(2) Uani 1 1 d . . . 
O11 O 0.1300(13) 0.0045(4) 0.3123(14) 0.012(2) Uani 1 1 d . . . 
O12 O 0.0049(5) 0.6252(12) 0.6935(14) 0.011(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 
Y1 O2 2.219(11) 2_675 ? 
Y1 O1 2.252(10) 3 ? 
Y1 O9 2.321(14) . ? 
Y1 O8 2.325(7) 4_465 ? 
Y1 O12 2.338(9) 3 ? 
Y1 O7 2.339(7) . ? 
Y1 O12 2.382(8) 4_565 ? 
Y1 Y1 3.839(3) 2_675 ? 
Y2 O4 2.217(10) 3 ? 
Y2 O3 2.250(10) 1_455 ? 
Y2 O10 2.272(13) . ? 
Y2 O6 2.308(7) 3 ? 
Y2 O5 2.337(6) . ? 
Y2 O11 2.399(9) 2_565 ? 
Y2 O11 2.411(8) 1_565 ? 
Y2 Y2 3.850(3) 2_575 ? 
Mo1 O3 1.731(9) 2_666 ? 
Mo1 O1 1.750(10) . ? 
Mo1 O4 1.759(9) 1_556 ? 
Mo1 O2 1.769(11) 2_665 ? 
Mo2 O9 1.702(13) . ? 
Mo2 O6 1.733(7) 2_665 ? 
Mo2 O5 1.740(6) 3 ? 
Mo2 O11 1.775(13) 1_565 ? 
Mo3 O7 1.746(8) 1_655 ? 
Mo3 O8 1.758(7) 3_655 ? 
Mo3 O10 1.773(13) 1_655 ? 
Mo3 O12 1.820(13) 1_655 ? 
O1 Y1 2.252(10) 3_545 ? 
O2 Mo1 1.769(11) 2_665 ? 
O2 Y1 2.219(11) 2_675 ? 
O3 Mo1 1.731(9) 2_664 ? 
O3 Y2 2.250(10) 1_655 ? 
O4 Mo1 1.759(9) 1_554 ? 
O4 Y2 2.217(10) 3_545 ? 
O5 Mo2 1.740(6) 3_545 ? 
O6 Mo2 1.733(7) 2_665 ? 
O6 Y2 2.308(7) 3_545 ? 
O7 Mo3 1.746(7) 1_455 ? 
O8 Mo3 1.758(7) 3_645 ? 
O8 Y1 2.325(7) 4_565 ? 
O10 Mo3 1.773(13) 1_455 ? 
O11 Mo2 1.775(13) 1_545 ? 
O11 Y2 2.399(9) 2_565 ? 
O11 Y2 2.411(8) 1_545 ? 
O12 Mo3 1.820(13) 1_455 ? 
O12 Y1 2.338(8) 3_545 ? 
O12 Y1 2.382(8) 4_465 ? 
 
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 
O2 Y1 O1 76.2(5) 2_675 3 ? 
O2 Y1 O9 145.0(4) 2_675 . ? 
O1 Y1 O9 138.7(4) 3 . ? 
O2 Y1 O8 78.3(4) 2_675 4_465 ? 
O1 Y1 O8 132.0(4) 3 4_465 ? 
O9 Y1 O8 76.3(4) . 4_465 ? 
O2 Y1 O12 78.4(5) 2_675 3 ? 
O1 Y1 O12 116.8(5) 3 3 ? 
O9 Y1 O12 81.2(5) . 3 ? 
O8 Y1 O12 96.7(4) 4_465 3 ? 
O2 Y1 O7 112.9(4) 2_675 . ? 
O1 Y1 O7 78.7(3) 3 . ? 
O9 Y1 O7 82.9(4) . . ? 
O8 Y1 O7 74.7(2) 4_465 . ? 
O12 Y1 O7 163.4(4) 3 . ? 
O2 Y1 O12 116.8(5) 2_675 4_565 ? 
O1 Y1 O12 75.6(4) 3 4_565 ? 
O9 Y1 O12 79.4(5) . 4_565 ? 
O8 Y1 O12 152.4(4) 4_465 4_565 ? 
O12 Y1 O12 66.5(5) 3 4_565 ? 
O7 Y1 O12 115.2(3) . 4_565 ? 
O2 Y1 Y1 88.0(3) 2_675 2_675 ? 
O1 Y1 Y1 86.3(3) 3 2_675 ? 
O9 Y1 Y1 91.9(4) . 2_675 ? 
O8 Y1 Y1 132.6(3) 4_465 2_675 ? 
O12 Y1 Y1 35.9(3) 3 2_675 ? 
O7 Y1 Y1 150.1(2) . 2_675 ? 
O12 Y1 Y1 35.2(3) 4_565 2_675 ? 
O4 Y2 O3 76.3(5) 3 1_455 ? 
O4 Y2 O10 137.7(3) 3 . ? 
O3 Y2 O10 145.9(3) 1_455 . ? 
O4 Y2 O6 127.4(4) 3 3 ? 
O3 Y2 O6 77.5(3) 1_455 3 ? 
O10 Y2 O6 79.6(3) . 3 ? 
O4 Y2 O5 79.2(3) 3 . ? 
O3 Y2 O5 118.3(4) 1_455 . ? 
O10 Y2 O5 78.7(4) . . ? 
O6 Y2 O5 74.4(3) 3 . ? 
O4 Y2 O11 121.5(4) 3 2_565 ? 
O3 Y2 O11 76.9(4) 1_455 2_565 ? 
O10 Y2 O11 80.4(4) . 2_565 ? 
O6 Y2 O11 95.4(4) 3 2_565 ? 
O5 Y2 O11 158.1(4) . 2_565 ? 
O4 Y2 O11 79.2(4) 3 1_565 ? 
O3 Y2 O11 116.0(4) 1_455 1_565 ? 
O10 Y2 O11 77.3(4) . 1_565 ? 
O6 Y2 O11 153.3(4) 3 1_565 ? 
O5 Y2 O11 113.5(4) . 1_565 ? 
O11 Y2 O11 67.7(5) 2_565 1_565 ? 
O4 Y2 Y2 89.7(3) 3 2_575 ? 
O3 Y2 Y2 85.0(2) 1_455 2_575 ? 
O10 Y2 Y2 91.9(3) . 2_575 ? 
O6 Y2 Y2 132.1(3) 3 2_575 ? 
O5 Y2 Y2 150.2(3) . 2_575 ? 
O11 Y2 Y2 36.9(3) 2_565 2_575 ? 
O11 Y2 Y2 36.7(3) 1_565 2_575 ? 
O3 Mo1 O1 109.0(6) 2_666 . ? 
O3 Mo1 O4 108.8(7) 2_666 1_556 ? 
O1 Mo1 O4 111.0(6) . 1_556 ? 
O3 Mo1 O2 109.0(6) 2_666 2_665 ? 
O1 Mo1 O2 108.4(7) . 2_665 ? 
O4 Mo1 O2 110.5(6) 1_556 2_665 ? 
O9 Mo2 O6 107.3(4) . 2_665 ? 
O9 Mo2 O5 110.7(4) . 3 ? 
O6 Mo2 O5 113.6(4) 2_665 3 ? 
O9 Mo2 O11 109.3(7) . 1_565 ? 
O6 Mo2 O11 107.2(3) 2_665 1_565 ? 
O5 Mo2 O11 108.6(4) 3 1_565 ? 
O7 Mo3 O8 111.3(3) 1_655 3_655 ? 
O7 Mo3 O10 110.0(4) 1_655 1_655 ? 
O8 Mo3 O10 109.0(4) 3_655 1_655 ? 
O7 Mo3 O12 109.2(4) 1_655 1_655 ? 
O8 Mo3 O12 106.1(3) 3_655 1_655 ? 
O10 Mo3 O12 111.1(6) 1_655 1_655 ? 
Mo1 O1 Y1 148.8(6) . 3_545 ? 
Mo1 O2 Y1 149.4(6) 2_665 2_675 ? 
Mo1 O3 Y2 147.1(6) 2_664 1_655 ? 
Mo1 O4 Y2 151.5(6) 1_554 3_545 ? 
Mo2 O5 Y2 165.4(5) 3_545 . ? 
Mo2 O6 Y2 154.3(5) 2_665 3_545 ? 
Mo3 O7 Y1 156.4(4) 1_455 . ? 
Mo3 O8 Y1 155.9(5) 3_645 4_565 ? 
Mo2 O9 Y1 177.1(7) . . ? 
Mo3 O10 Y2 170.5(4) 1_455 . ? 
Mo2 O11 Y2 133.0(4) 1_545 2_565 ? 
Mo2 O11 Y2 120.2(3) 1_545 1_545 ? 
Y2 O11 Y2 106.3(5) 2_565 1_545 ? 
Mo3 O12 Y1 129.4(4) 1_455 3_545 ? 
Mo3 O12 Y1 121.7(3) 1_455 4_465 ? 
Y1 O12 Y1 108.9(5) 3_545 4_465 ? 
 
_diffrn_measured_fraction_theta_max    0.999 
_diffrn_reflns_theta_full              35.65 
_diffrn_measured_fraction_theta_full   0.999 
_refine_diff_density_max    1.170 
_refine_diff_density_min   -1.658 
_refine_diff_density_rms    0.230 
