 
data_c:\crystal\x-red32\y2mo3o12 
 
_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            tetragonal 
_symmetry_space_group_name_H-M    P-421m
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 'x+1/2, -y+1/2, -z' 
 '-x, -y, z' 
 '-x+1/2, y+1/2, -z' 
 '-y+1/2, -x+1/2, z' 
 '-y, x, -z' 
 'y, -x, -z' 
 'y+1/2, x+1/2, z' 
 
_cell_length_a                    7.2927(2) 
_cell_length_b                    7.2927(2) 
_cell_length_c                    10.5726(3) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 90.00 
_cell_volume                      562.29(3) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     4989 
_cell_measurement_theta_min       0.41
_cell_measurement_theta_max       28.28
 
_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     3.884 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              600 
_exptl_absorpt_coefficient_mu     13.513 
_exptl_absorpt_correction_type    numerical
_exptl_absorpt_correction_T_min   0.3874 
_exptl_absorpt_correction_T_max   0.6511
_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             6614 
_diffrn_reflns_av_R_equivalents   0.0868 
_diffrn_reflns_av_sigmaI/netI     0.0375 
_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        -14 
_diffrn_reflns_limit_l_max        14 
_diffrn_reflns_theta_min          1.93 
_diffrn_reflns_theta_max          28.23 
_reflns_number_total              771 
_reflns_number_gt                 724 
_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)+(0.0106P)²+0.7878P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_refine_ls_extinction_method      SHELXL 
_refine_ls_extinction_coef        0.0038(5) 
_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    -0.010(8) 
_refine_ls_number_reflns          771 
_refine_ls_number_parameters      46 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0252 
_refine_ls_R_factor_gt            0.0221 
_refine_ls_wR_factor_ref          0.0439 
_refine_ls_wR_factor_gt           0.0431 
_refine_ls_goodness_of_fit_ref    1.058 
_refine_ls_restrained_S_all       1.058 
_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 
Y Y 0.31358(5) 0.81358(5) 0.26252(5) 0.00749(15) Uani 1 2 d S . . 
Mo1 Mo 0.0000 0.0000 0.0000 0.01066(18) Uani 1 4 d S . . 
Mo2 Mo 0.29449(5) 0.79449(5) 0.64282(5) 0.00913(14) Uani 1 2 d S . . 
O1 O 0.0427(5) 0.1900(5) 0.9036(3) 0.0217(8) Uani 1 1 d . . . 
O2 O 0.2738(8) 0.5061(6) 0.2994(4) 0.0580(17) Uani 1 1 d . . . 
O3 O 0.3063(5) 0.8063(5) 0.4793(4) 0.0322(13) Uani 1 2 d S . . 
O4 O 0.1282(4) 0.6282(4) 0.6914(4) 0.0105(10) Uani 1 2 d S . . 
 
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 
Y 0.00796(18) 0.00796(18) 0.0065(3) -0.00060(15) -0.00060(15) -0.0014(2) 
Mo1 0.0131(3) 0.0131(3) 0.0059(3) 0.000 0.000 0.000 
Mo2 0.00968(18) 0.00968(18) 0.0080(3) 0.00056(15) 0.00056(15) -0.0035(2) 
O1 0.030(2) 0.0220(18) 0.0134(16) 0.0053(15) 0.0029(14) -0.0008(16) 
O2 0.112(5) 0.0095(18) 0.053(3) 0.005(2) 0.046(3) 0.008(3) 
O3 0.045(2) 0.045(2) 0.007(3) 0.0023(15) 0.0023(15) -0.025(3) 
O4 0.0108(14) 0.0108(14) 0.010(2) 0.0017(11) 0.0017(11) -0.0035(17) 
 
_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 
Y O1 2.235(4) 7_566 ? 
Y O1 2.235(4) 4_556 ? 
Y O3 2.293(4) . ? 
Y O2 2.295(4) . ? 
Y O2 2.295(4) 8_455 ? 
Y O4 2.384(3) 4_556 ? 
Y O4 2.384(3) 2_566 ? 
Y Y 3.8452(11) 3_675 ? 
Mo1 O1 1.748(4) 3_554 ? 
Mo1 O1 1.748(4) 7_556 ? 
Mo1 O1 1.748(4) 1_554 ? 
Mo1 O1 1.748(4) 6_556 ? 
Mo2 O2 1.733(4) 7_566 ? 
Mo2 O2 1.733(4) 4_556 ? 
Mo2 O3 1.733(4) . ? 
Mo2 O4 1.790(5) . ? 
O1 Mo1 1.748(4) 1_556 ? 
O1 Y 2.235(4) 4_546 ? 
O2 Mo2 1.733(4) 4_546 ? 
O4 Y 2.384(3) 4_546 ? 
O4 Y 2.384(3) 2_466 ? 
 
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 
O1 Y O1 76.2(2) 7_566 4_556 ? 
O1 Y O3 141.89(10) 7_566 . ? 
O1 Y O3 141.89(10) 4_556 . ? 
O1 Y O2 122.75(17) 7_566 . ? 
O1 Y O2 78.38(14) 4_556 . ? 
O3 Y O2 78.72(15) . . ? 
O1 Y O2 78.38(14) 7_566 8_455 ? 
O1 Y O2 122.75(17) 4_556 8_455 ? 
O3 Y O2 78.72(15) . 8_455 ? 
O2 Y O2 74.0(3) . 8_455 ? 
O1 Y O4 77.35(14) 7_566 4_556 ? 
O1 Y O4 117.73(14) 4_556 4_556 ? 
O3 Y O4 79.76(15) . 4_556 ? 
O2 Y O4 158.20(16) . 4_556 ? 
O2 Y O4 105.13(17) 8_455 4_556 ? 
O1 Y O4 117.73(14) 7_566 2_566 ? 
O1 Y O4 77.35(14) 4_556 2_566 ? 
O3 Y O4 79.76(15) . 2_566 ? 
O2 Y O4 105.13(17) . 2_566 ? 
O2 Y O4 158.20(16) 8_455 2_566 ? 
O4 Y O4 67.38(19) 4_556 2_566 ? 
O1 Y Y 87.34(9) 7_566 3_675 ? 
O1 Y Y 87.34(9) 4_556 3_675 ? 
O3 Y Y 91.88(13) . 3_675 ? 
O2 Y Y 141.30(15) . 3_675 ? 
O2 Y Y 141.30(15) 8_455 3_675 ? 
O4 Y Y 36.24(9) 4_556 3_675 ? 
O4 Y Y 36.24(9) 2_566 3_675 ? 
O1 Mo1 O1 109.89(12) 3_554 7_556 ? 
O1 Mo1 O1 108.6(2) 3_554 1_554 ? 
O1 Mo1 O1 109.89(12) 7_556 1_554 ? 
O1 Mo1 O1 109.89(12) 3_554 6_556 ? 
O1 Mo1 O1 108.6(2) 7_556 6_556 ? 
O1 Mo1 O1 109.89(12) 1_554 6_556 ? 
O2 Mo2 O2 112.8(4) 7_566 4_556 ? 
O2 Mo2 O3 108.76(17) 7_566 . ? 
O2 Mo2 O3 108.76(17) 4_556 . ? 
O2 Mo2 O4 107.90(17) 7_566 . ? 
O2 Mo2 O4 107.90(17) 4_556 . ? 
O3 Mo2 O4 110.7(2) . . ? 
Mo1 O1 Y 149.5(2) 1_556 4_546 ? 
Mo2 O2 Y 165.2(2) 4_546 . ? 
Mo2 O3 Y 177.9(3) . . ? 
Mo2 O4 Y 126.15(9) . 4_546 ? 
Mo2 O4 Y 126.15(9) . 2_466 ? 
Y O4 Y 107.53(18) 4_546 2_466 ? 
 
_diffrn_measured_fraction_theta_max    1.000 
_diffrn_reflns_theta_full              28.23 
_diffrn_measured_fraction_theta_full   1.000 
_refine_diff_density_max    0.570 
_refine_diff_density_min   -0.530 
_refine_diff_density_rms    0.126 
