data_KFeMo _audit_creation_date 2007-04-23T16:52:02-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _publ_requested_category FI #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'Fe2 Mo O12 P2, 2K' _chemical_formula_sum 'Fe2 K2 Mo O12 P2' _chemical_formula_weight 539.78 _chemical_absolute_configuration ad #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'y, z, x' 'z, x, y' 'x+1/2, -y+1/2, -z' 'y+1/2, -z+1/2, -x' 'z+1/2, -x+1/2, -y' '-y, z+1/2, -x+1/2' '-z, x+1/2, -y+1/2' '-z+1/2, -x, y+1/2' '-x+1/2, -y, z+1/2' '-y+1/2, -z, x+1/2' '-x, y+1/2, -z+1/2' _cell_length_a 10.0405(6) _cell_length_b 10.0405(6) _cell_length_c 10.0405(6) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1012.20(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5704 _cell_measurement_theta_min 2.87 _cell_measurement_theta_max 25.41 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description tetrahedron _exptl_crystal_colour brown _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 3.542 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1032 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 5.252 _exptl_absorpt_correction_type refdelf _exptl_absorpt_process_details ; (See: Walker, N. & Stuart, D. (1983) Acta Cryst. A39, 158-166) ; _exptl_absorpt_correction_T_min 0.605 _exptl_absorpt_correction_T_max 0.882 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_probe x-ray _diffrn_source 'fine focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS-1' _diffrn_measurement_method '\f oscilations' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 5704 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.87 _diffrn_reflns_theta_max 25.41 _diffrn_reflns_theta_full 25.41 _diffrn_measured_fraction_theta_full 1 _diffrn_measured_fraction_theta_max 1 _reflns_number_total 634 _reflns_number_gt 624 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'CrysAlis CCD (Oxford Diffraction Ltd., 2005)' _computing_cell_refinement 'CrysAlis CCD (Oxford Diffraction Ltd., 2005)' _computing_data_reduction 'CrysAlis RED (Oxford Diffraction Ltd., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ 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/[\s^2^(Fo^2^)+(0.0000P)^2^+9.8004P] where P=(Fo^2^+2Fc^2^)/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_number_reflns 634 _refine_ls_number_parameters 60 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0408 _refine_ls_R_factor_gt 0.0401 _refine_ls_wR_factor_ref 0.0868 _refine_ls_wR_factor_gt 0.0866 _refine_ls_goodness_of_fit_ref 1.289 _refine_ls_restrained_S_all 1.304 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(8) _refine_diff_density_max 0.683 _refine_diff_density_min -0.637 _refine_diff_density_rms 0.139 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 K1 K 0.7081(3) 0.7081(3) 0.7081(3) 0.0503(11) Uani 1 3 d S . . K2 K 0.93238(19) 0.93238(19) 0.93238(19) 0.0353(8) Uani 1 3 d S . . Fe1 Fe 0.14194(13) 0.14194(13) 0.14194(13) 0.0270(5) Uani 1 3 d S . . Fe2 Fe 0.41450(16) 0.41450(16) 0.41450(16) 0.0401(7) Uani 1 3 d S . . P1 P 0.45275(13) 0.22573(13) 0.12746(13) 0.0189(3) Uani 0.6909(8) 1 d P . . Mo1 Mo 0.45275(13) 0.22573(13) 0.12746(13) 0.0189(3) Uani 0.3131(7) 1 d P . . O1 O 0.3053(7) 0.2342(8) 0.0770(8) 0.0463(19) Uani 1 1 d . . . O2 O 0.5462(8) 0.2996(7) 0.0198(7) 0.0421(18) Uani 1 1 d . . . O3 O 0.5038(7) 0.0809(7) 0.1520(8) 0.0445(19) Uani 1 1 d . . . O4 O 0.4745(8) 0.3057(8) 0.2603(8) 0.047(2) 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 K1 0.0503(11) 0.0503(11) 0.0503(11) 0.0053(13) 0.0053(13) 0.0053(13) K2 0.0353(8) 0.0353(8) 0.0353(8) -0.0095(9) -0.0095(9) -0.0095(9) Fe1 0.0270(5) 0.0270(5) 0.0270(5) -0.0012(5) -0.0012(5) -0.0012(5) Fe2 0.0401(7) 0.0401(7) 0.0401(7) 0.0044(7) 0.0044(7) 0.0044(7) P1 0.0182(7) 0.0190(6) 0.0195(7) 0.0006(5) 0.0001(5) 0.0015(5) Mo1 0.0182(7) 0.0190(6) 0.0195(7) 0.0006(5) 0.0001(5) 0.0015(5) O1 0.031(4) 0.048(4) 0.060(5) 0.013(4) -0.001(3) -0.022(3) O2 0.047(4) 0.040(4) 0.039(4) 0.015(3) 0.021(4) 0.009(3) O3 0.039(4) 0.047(4) 0.048(4) 0.004(4) 0.010(4) 0.014(3) O4 0.051(5) 0.055(5) 0.035(4) -0.013(3) 0.004(4) -0.008(4) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 K1 O1 2.878(9) 5_556 ? K1 O1 2.878(9) 9_565 ? K1 O1 2.878(9) 12_655 ? K1 O2 3.109(8) 7_656 ? K1 O2 3.109(8) 10_665 ? K1 O2 3.109(8) 6_566 ? K1 O4 3.233(8) 10_665 ? K1 O4 3.233(8) 7_656 ? K1 O4 3.233(8) 6_566 ? K1 Mo1 3.562(3) 10_665 ? K1 P1 3.562(3) 10_665 ? K1 P1 3.562(3) 7_656 ? K2 O3 2.890(9) 7_656 ? K2 O3 2.890(8) 10_665 ? K2 O3 2.890(9) 6_566 ? K2 O2 2.963(8) 11_665 ? K2 O2 2.963(8) 8_656 ? K2 O2 2.963(8) 4_566 ? K2 O4 3.094(9) 7_656 ? K2 O4 3.094(9) 10_665 ? K2 O4 3.094(9) 6_566 ? K2 O4 3.292(9) 11_665 ? K2 O4 3.292(9) 8_656 ? K2 O4 3.292(9) 4_566 ? Fe1 O2 1.976(7) 8_545 ? Fe1 O2 1.976(7) 11_554 ? Fe1 O2 1.976(7) 4_455 ? Fe1 O1 1.994(7) 2 ? Fe1 O1 1.994(7) . ? Fe1 O1 1.994(7) 3 ? Fe1 K2 3.645(4) 1_444 ? Fe1 K1 3.881(2) 4_456 ? Fe1 K1 3.881(2) 7_645 ? Fe1 K1 3.881(2) 9_564 ? Fe2 O3 1.977(7) 5_556 ? Fe2 O3 1.977(7) 9_565 ? Fe2 O3 1.977(7) 12_655 ? Fe2 O4 1.988(8) 2 ? Fe2 O4 1.988(8) . ? Fe2 O4 1.988(8) 3 ? Fe2 K2 3.8113(13) 9_664 ? Fe2 K2 3.8113(13) 4_466 ? Fe2 K2 3.8113(13) 7_646 ? P1 O3 1.562(7) . ? P1 O1 1.567(7) . ? P1 O4 1.572(8) . ? P1 O2 1.612(7) . ? P1 K2 3.491(2) 4_466 ? P1 K1 3.562(3) 9_664 ? P1 K2 3.636(2) 9_664 ? P1 K1 3.741(4) 7_645 ? O1 K1 2.878(9) 7_645 ? O2 Fe1 1.976(7) 4 ? O2 K2 2.963(8) 4_466 ? O2 K1 3.109(8) 9_664 ? O3 Fe2 1.977(7) 7_645 ? O3 K2 2.890(8) 9_664 ? O4 K2 3.094(9) 9_664 ? O4 K1 3.233(8) 9_664 ? O4 K2 3.292(9) 4_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 K1 O1 92.8(3) 5_556 9_565 ? O1 K1 O1 92.8(3) 5_556 12_655 ? O1 K1 O1 92.8(3) 9_565 12_655 ? O1 K1 O2 55.56(17) 5_556 7_656 ? O1 K1 O2 82.79(19) 9_565 7_656 ? O1 K1 O2 147.5(3) 12_655 7_656 ? O1 K1 O2 82.79(19) 5_556 10_665 ? O1 K1 O2 147.5(3) 9_565 10_665 ? O1 K1 O2 55.56(17) 12_655 10_665 ? O2 K1 O2 119.15(5) 7_656 10_665 ? O1 K1 O2 147.5(3) 5_556 6_566 ? O1 K1 O2 55.56(17) 9_565 6_566 ? O1 K1 O2 82.79(19) 12_655 6_566 ? O2 K1 O2 119.15(5) 7_656 6_566 ? O2 K1 O2 119.15(5) 10_665 6_566 ? O1 K1 O4 82.8(2) 5_556 10_665 ? O1 K1 O4 164.6(2) 9_565 10_665 ? O1 K1 O4 102.21(19) 12_655 10_665 ? O2 K1 O4 82.5(2) 7_656 10_665 ? O2 K1 O4 46.80(19) 10_665 10_665 ? O2 K1 O4 129.6(2) 6_566 10_665 ? O1 K1 O4 102.21(19) 5_556 7_656 ? O1 K1 O4 82.8(2) 9_565 7_656 ? O1 K1 O4 164.6(2) 12_655 7_656 ? O2 K1 O4 46.80(19) 7_656 7_656 ? O2 K1 O4 129.6(2) 10_665 7_656 ? O2 K1 O4 82.5(2) 6_566 7_656 ? O4 K1 O4 83.7(3) 10_665 7_656 ? O1 K1 O4 164.6(2) 5_556 6_566 ? O1 K1 O4 102.21(19) 9_565 6_566 ? O1 K1 O4 82.8(2) 12_655 6_566 ? O2 K1 O4 129.6(2) 7_656 6_566 ? O2 K1 O4 82.5(2) 10_665 6_566 ? O2 K1 O4 46.80(19) 6_566 6_566 ? O4 K1 O4 83.7(3) 10_665 6_566 ? O4 K1 O4 83.7(3) 7_656 6_566 ? O1 K1 Mo1 95.04(15) 5_556 10_665 ? O1 K1 Mo1 168.59(13) 9_565 10_665 ? O1 K1 Mo1 78.57(14) 12_655 10_665 ? O2 K1 Mo1 108.52(15) 7_656 10_665 ? O2 K1 Mo1 26.88(13) 10_665 10_665 ? O2 K1 Mo1 115.33(16) 6_566 10_665 ? O4 K1 Mo1 26.18(14) 10_665 10_665 ? O4 K1 Mo1 103.6(2) 7_656 10_665 ? O4 K1 Mo1 69.60(16) 6_566 10_665 ? O1 K1 P1 95.04(15) 5_556 10_665 ? O1 K1 P1 168.59(13) 9_565 10_665 ? O1 K1 P1 78.57(14) 12_655 10_665 ? O2 K1 P1 108.52(15) 7_656 10_665 ? O2 K1 P1 26.88(13) 10_665 10_665 ? O2 K1 P1 115.33(16) 6_566 10_665 ? O4 K1 P1 26.18(14) 10_665 10_665 ? O4 K1 P1 103.6(2) 7_656 10_665 ? O4 K1 P1 69.60(16) 6_566 10_665 ? Mo1 K1 P1 0.00(4) 10_665 10_665 ? O1 K1 P1 78.57(14) 5_556 7_656 ? O1 K1 P1 95.04(15) 9_565 7_656 ? O1 K1 P1 168.59(13) 12_655 7_656 ? O2 K1 P1 26.88(13) 7_656 7_656 ? O2 K1 P1 115.33(16) 10_665 7_656 ? O2 K1 P1 108.52(15) 6_566 7_656 ? O4 K1 P1 69.60(16) 10_665 7_656 ? O4 K1 P1 26.18(14) 7_656 7_656 ? O4 K1 P1 103.6(2) 6_566 7_656 ? Mo1 K1 P1 94.67(10) 10_665 7_656 ? P1 K1 P1 94.67(10) 10_665 7_656 ? O3 K2 O3 100.5(2) 7_656 10_665 ? O3 K2 O3 100.5(2) 7_656 6_566 ? O3 K2 O3 100.5(2) 10_665 6_566 ? O3 K2 O2 96.6(2) 7_656 11_665 ? O3 K2 O2 100.5(2) 10_665 11_665 ? O3 K2 O2 150.0(2) 6_566 11_665 ? O3 K2 O2 100.5(2) 7_656 8_656 ? O3 K2 O2 150.0(2) 10_665 8_656 ? O3 K2 O2 96.6(2) 6_566 8_656 ? O2 K2 O2 55.9(2) 11_665 8_656 ? O3 K2 O2 150.0(2) 7_656 4_566 ? O3 K2 O2 96.6(2) 10_665 4_566 ? O3 K2 O2 100.5(2) 6_566 4_566 ? O2 K2 O2 55.9(2) 11_665 4_566 ? O2 K2 O2 55.9(2) 8_656 4_566 ? O3 K2 O4 49.7(2) 7_656 7_656 ? O3 K2 O4 116.1(2) 10_665 7_656 ? O3 K2 O4 52.1(2) 6_566 7_656 ? O2 K2 O4 132.5(2) 11_665 7_656 ? O2 K2 O4 93.78(19) 8_656 7_656 ? O2 K2 O4 139.1(2) 4_566 7_656 ? O3 K2 O4 52.1(2) 7_656 10_665 ? O3 K2 O4 49.7(2) 10_665 10_665 ? O3 K2 O4 116.1(2) 6_566 10_665 ? O2 K2 O4 93.78(19) 11_665 10_665 ? O2 K2 O4 139.1(2) 8_656 10_665 ? O2 K2 O4 132.5(2) 4_566 10_665 ? O4 K2 O4 88.3(2) 7_656 10_665 ? O3 K2 O4 116.1(2) 7_656 6_566 ? O3 K2 O4 52.1(2) 10_665 6_566 ? O3 K2 O4 49.7(2) 6_566 6_566 ? O2 K2 O4 139.1(2) 11_665 6_566 ? O2 K2 O4 132.5(2) 8_656 6_566 ? O2 K2 O4 93.78(19) 4_566 6_566 ? O4 K2 O4 88.3(2) 7_656 6_566 ? O4 K2 O4 88.3(2) 10_665 6_566 ? O3 K2 O4 55.7(2) 7_656 11_665 ? O3 K2 O4 85.45(19) 10_665 11_665 ? O3 K2 O4 156.1(2) 6_566 11_665 ? O2 K2 O4 47.18(18) 11_665 11_665 ? O2 K2 O4 88.9(2) 8_656 11_665 ? O2 K2 O4 101.8(2) 4_566 11_665 ? O4 K2 O4 104.49(4) 7_656 11_665 ? O4 K2 O4 51.4(3) 10_665 11_665 ? O4 K2 O4 136.29(16) 6_566 11_665 ? O3 K2 O4 85.45(19) 7_656 8_656 ? O3 K2 O4 156.1(2) 10_665 8_656 ? O3 K2 O4 55.7(2) 6_566 8_656 ? O2 K2 O4 101.8(2) 11_665 8_656 ? O2 K2 O4 47.18(18) 8_656 8_656 ? O2 K2 O4 88.9(2) 4_566 8_656 ? O4 K2 O4 51.4(3) 7_656 8_656 ? O4 K2 O4 136.29(16) 10_665 8_656 ? O4 K2 O4 104.49(4) 6_566 8_656 ? O4 K2 O4 116.26(9) 11_665 8_656 ? O3 K2 O4 156.1(2) 7_656 4_566 ? O3 K2 O4 55.7(2) 10_665 4_566 ? O3 K2 O4 85.45(18) 6_566 4_566 ? O2 K2 O4 88.9(2) 11_665 4_566 ? O2 K2 O4 101.8(2) 8_656 4_566 ? O2 K2 O4 47.18(18) 4_566 4_566 ? O4 K2 O4 136.29(16) 7_656 4_566 ? O4 K2 O4 104.49(4) 10_665 4_566 ? O4 K2 O4 51.4(3) 6_566 4_566 ? O4 K2 O4 116.26(9) 11_665 4_566 ? O4 K2 O4 116.26(9) 8_656 4_566 ? O2 Fe1 O2 89.4(3) 8_545 11_554 ? O2 Fe1 O2 89.4(3) 8_545 4_455 ? O2 Fe1 O2 89.4(3) 11_554 4_455 ? O2 Fe1 O1 88.8(3) 8_545 2 ? O2 Fe1 O1 89.6(3) 11_554 2 ? O2 Fe1 O1 177.9(3) 4_455 2 ? O2 Fe1 O1 177.9(3) 8_545 . ? O2 Fe1 O1 88.8(3) 11_554 . ? O2 Fe1 O1 89.6(3) 4_455 . ? O1 Fe1 O1 92.2(3) 2 . ? O2 Fe1 O1 89.6(3) 8_545 3 ? O2 Fe1 O1 177.9(3) 11_554 3 ? O2 Fe1 O1 88.8(3) 4_455 3 ? O1 Fe1 O1 92.2(3) 2 3 ? O1 Fe1 O1 92.2(3) . 3 ? O2 Fe1 K2 54.3(2) 8_545 1_444 ? O2 Fe1 K2 54.3(2) 11_554 1_444 ? O2 Fe1 K2 54.3(2) 4_455 1_444 ? O1 Fe1 K2 123.7(2) 2 1_444 ? O1 Fe1 K2 123.7(2) . 1_444 ? O1 Fe1 K2 123.7(2) 3 1_444 ? O2 Fe1 K1 65.5(2) 8_545 4_456 ? O2 Fe1 K1 52.7(2) 11_554 4_456 ? O2 Fe1 K1 132.1(2) 4_455 4_456 ? O1 Fe1 K1 46.0(2) 2 4_456 ? O1 Fe1 K1 114.0(2) . 4_456 ? O1 Fe1 K1 128.4(3) 3 4_456 ? K2 Fe1 K1 78.46(4) 1_444 4_456 ? O2 Fe1 K1 132.1(2) 8_545 7_645 ? O2 Fe1 K1 65.5(2) 11_554 7_645 ? O2 Fe1 K1 52.7(2) 4_455 7_645 ? O1 Fe1 K1 128.4(3) 2 7_645 ? O1 Fe1 K1 46.0(2) . 7_645 ? O1 Fe1 K1 114.0(2) 3 7_645 ? K2 Fe1 K1 78.46(4) 1_444 7_645 ? K1 Fe1 K1 116.10(2) 4_456 7_645 ? O2 Fe1 K1 52.7(2) 8_545 9_564 ? O2 Fe1 K1 132.1(2) 11_554 9_564 ? O2 Fe1 K1 65.5(2) 4_455 9_564 ? O1 Fe1 K1 114.0(2) 2 9_564 ? O1 Fe1 K1 128.4(3) . 9_564 ? O1 Fe1 K1 46.0(2) 3 9_564 ? K2 Fe1 K1 78.46(4) 1_444 9_564 ? K1 Fe1 K1 116.10(2) 4_456 9_564 ? K1 Fe1 K1 116.10(2) 7_645 9_564 ? O3 Fe2 O3 94.3(3) 5_556 9_565 ? O3 Fe2 O3 94.3(3) 5_556 12_655 ? O3 Fe2 O3 94.3(3) 9_565 12_655 ? O3 Fe2 O4 94.3(3) 5_556 2 ? O3 Fe2 O4 83.2(3) 9_565 2 ? O3 Fe2 O4 171.2(3) 12_655 2 ? O3 Fe2 O4 83.2(3) 5_556 . ? O3 Fe2 O4 171.2(3) 9_565 . ? O3 Fe2 O4 94.3(3) 12_655 . ? O4 Fe2 O4 88.5(3) 2 . ? O3 Fe2 O4 171.2(3) 5_556 3 ? O3 Fe2 O4 94.3(3) 9_565 3 ? O3 Fe2 O4 83.2(3) 12_655 3 ? O4 Fe2 O4 88.5(3) 2 3 ? O4 Fe2 O4 88.5(3) . 3 ? O3 Fe2 K2 48.0(2) 5_556 9_664 ? O3 Fe2 K2 118.4(2) 9_565 9_664 ? O3 Fe2 K2 128.4(2) 12_655 9_664 ? O4 Fe2 K2 59.7(3) 2 9_664 ? O4 Fe2 K2 54.0(2) . 9_664 ? O4 Fe2 K2 128.1(2) 3 9_664 ? O3 Fe2 K2 118.4(2) 5_556 4_466 ? O3 Fe2 K2 128.4(2) 9_565 4_466 ? O3 Fe2 K2 48.0(2) 12_655 4_466 ? O4 Fe2 K2 128.1(2) 2 4_466 ? O4 Fe2 K2 59.7(3) . 4_466 ? O4 Fe2 K2 54.0(2) 3 4_466 ? K2 Fe2 K2 113.12(4) 9_664 4_466 ? O3 Fe2 K2 128.4(2) 5_556 7_646 ? O3 Fe2 K2 48.0(2) 9_565 7_646 ? O3 Fe2 K2 118.4(2) 12_655 7_646 ? O4 Fe2 K2 54.0(2) 2 7_646 ? O4 Fe2 K2 128.1(2) . 7_646 ? O4 Fe2 K2 59.7(3) 3 7_646 ? K2 Fe2 K2 113.12(4) 9_664 7_646 ? K2 Fe2 K2 113.12(4) 4_466 7_646 ? O3 P1 O1 114.3(4) . . ? O3 P1 O4 107.2(4) . . ? O1 P1 O4 112.2(4) . . ? O3 P1 O2 110.1(4) . . ? O1 P1 O2 107.9(4) . . ? O4 P1 O2 104.7(4) . . ? O3 P1 K2 164.2(3) . 4_466 ? O1 P1 K2 80.5(3) . 4_466 ? O4 P1 K2 69.6(3) . 4_466 ? O2 P1 K2 57.7(3) . 4_466 ? O3 P1 K1 79.9(3) . 9_664 ? O1 P1 K1 165.1(3) . 9_664 ? O4 P1 K1 65.1(3) . 9_664 ? O2 P1 K1 60.7(3) . 9_664 ? K2 P1 K1 84.94(6) 4_466 9_664 ? O3 P1 K2 49.9(3) . 9_664 ? O1 P1 K2 126.5(3) . 9_664 ? O4 P1 K2 57.6(3) . 9_664 ? O2 P1 K2 125.5(3) . 9_664 ? K2 P1 K2 126.35(6) 4_466 9_664 ? K1 P1 K2 65.60(8) 9_664 9_664 ? O3 P1 K1 103.9(3) . 7_645 ? O1 P1 K1 45.9(3) . 7_645 ? O4 P1 K1 148.0(3) . 7_645 ? O2 P1 K1 70.7(3) . 7_645 ? K2 P1 K1 82.31(6) 4_466 7_645 ? K1 P1 K1 128.78(8) 9_664 7_645 ? K2 P1 K1 151.01(6) 9_664 7_645 ? P1 O1 Fe1 130.3(5) . . ? P1 O1 K1 111.2(4) . 7_645 ? Fe1 O1 K1 104.1(3) . 7_645 ? P1 O2 Fe1 166.1(5) . 4 ? P1 O2 K2 94.9(3) . 4_466 ? Fe1 O2 K2 92.9(2) 4 4_466 ? P1 O2 K1 92.4(3) . 9_664 ? Fe1 O2 K1 97.0(3) 4 9_664 ? K2 O2 K1 103.3(2) 4_466 9_664 ? P1 O3 Fe2 150.4(5) . 7_645 ? P1 O3 K2 105.6(4) . 9_664 ? Fe2 O3 K2 101.4(3) 7_645 9_664 ? P1 O4 Fe2 154.1(5) . . ? P1 O4 K2 97.0(4) . 9_664 ? Fe2 O4 K2 94.7(3) . 9_664 ? P1 O4 K1 88.7(3) . 9_664 ? Fe2 O4 K1 116.6(3) . 9_664 ? K2 O4 K1 76.1(2) 9_664 9_664 ? P1 O4 K2 83.8(3) . 4_466 ? Fe2 O4 K2 88.8(3) . 4_466 ? K2 O4 K2 169.8(3) 9_664 4_466 ? K1 O4 K2 93.8(2) 9_664 4_466 ? ########End data_KScW _audit_creation_date 2010-02-11 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _audit_update_record ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'O12 P2 Sc2 W, 2(K)' _chemical_formula_sum 'K2 O12 P2 Sc2 W' _chemical_formula_weight 604.37 _chemical_absolute_configuration ad _symmetry_cell_setting cubic _symmetry_space_group_name_H-M 'P 21 3' _symmetry_space_group_name_Hall 'P 2ac 2ab 3' _symmetry_Int_Tables_number 198 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' 'y, z, x' '-y+1/2, -z, x+1/2' 'y+1/2, -z+1/2, -x' '-y, z+1/2, -x+1/2' 'z, x, y' '-z, x+1/2, -y+1/2' '-z+1/2, -x, y+1/2' 'z+1/2, -x+1/2, -y' _cell_length_a 10.3372(2) _cell_length_b 10.3372(2) _cell_length_c 10.3372(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1104.61(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3627 _cell_measurement_theta_min 2.79 _cell_measurement_theta_max 29.96 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description tetrahedron _exptl_crystal_colour colorless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.07 _exptl_crystal_density_diffrn 3.634 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1120 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 12.583 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Blessing, 1995)' _exptl_absorpt_correction_T_min 0.2735 _exptl_absorpt_correction_T_max 0.4092 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_probe x-ray _diffrn_source 'fine focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type XCalibur-3 _diffrn_measurement_method '\f and \w scans' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_av_R_equivalents 0.0635 _diffrn_reflns_av_unetI/netI 0.0751 _diffrn_reflns_number 3627 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.79 _diffrn_reflns_theta_max 29.96 _diffrn_reflns_theta_full 29.96 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_total 1087 _reflns_number_gt 912 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'CrysAlis CCD (Oxford Diffraction Ltd., 2006)' _computing_cell_refinement 'CrysAlis CCD (Oxford Diffraction Ltd., 2006)' _computing_data_reduction 'CrysAlis RED (Oxford Diffraction Ltd., 2006)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens undef #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ 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/[\s^2^(Fo^2^)+(0.0101P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment undef _refine_ls_extinction_method SHELXL _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_coef 0.0016(2) _refine_ls_number_reflns 1087 _refine_ls_number_parameters 61 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0447 _refine_ls_R_factor_gt 0.0324 _refine_ls_wR_factor_ref 0.0486 _refine_ls_wR_factor_gt 0.0468 _refine_ls_goodness_of_fit_ref 0.871 _refine_ls_restrained_S_all 0.871 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details '463 Friedel pairs (Flack, 1983)' _refine_ls_abs_structure_Flack -0.01(2) _refine_diff_density_max 0.555 _refine_diff_density_min -0.655 _refine_diff_density_rms 0.129 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sc Sc 0.2519 0.3716 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.849 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 K1 K 0.7037(2) 0.7037(2) 0.7037(2) 0.0768(12) Uani 1 3 d S . . K2 K 0.93087(16) 0.93087(16) 0.93087(16) 0.0549(9) Uani 1 3 d S . . Sc1 Sc 0.14242(11) 0.14242(11) 0.14242(11) 0.0254(4) Uani 1 3 d S . . Sc2 Sc 0.41445(14) 0.41445(14) 0.41445(14) 0.0447(7) Uani 1 3 d S . . P1 P 0.45564(5) 0.22799(5) 0.12863(5) 0.01481(12) Uani 0.67 1 d P . . W1 W 0.45564(5) 0.22799(5) 0.12863(5) 0.01481(12) Uani 0.33 1 d P . . O1 O 0.3105(4) 0.2322(5) 0.0791(5) 0.0453(13) Uani 1 1 d . . . O2 O 0.5432(6) 0.3000(5) 0.0204(5) 0.0507(15) Uani 1 1 d . . . O3 O 0.5067(4) 0.0860(4) 0.1506(5) 0.0460(14) Uani 1 1 d . . . O4 O 0.4782(5) 0.3073(5) 0.2566(5) 0.0584(17) 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 K1 0.0768(12) 0.0768(12) 0.0768(12) 0.0007(13) 0.0007(13) 0.0007(13) K2 0.0549(9) 0.0549(9) 0.0549(9) -0.0114(8) -0.0114(8) -0.0114(8) Sc1 0.0254(4) 0.0254(4) 0.0254(4) -0.0006(5) -0.0006(5) -0.0006(5) Sc2 0.0447(7) 0.0447(7) 0.0447(7) 0.0003(6) 0.0003(6) 0.0003(6) P1 0.0147(3) 0.0153(2) 0.0144(3) -0.0027(2) 0.0011(2) 0.0000(2) W1 0.0147(3) 0.0153(2) 0.0144(3) -0.0027(2) 0.0011(2) 0.0000(2) O1 0.027(2) 0.053(3) 0.056(3) 0.020(3) -0.003(2) -0.004(2) O2 0.061(3) 0.048(3) 0.043(3) 0.019(2) 0.031(3) 0.000(3) O3 0.043(3) 0.037(3) 0.058(3) 0.001(2) 0.004(3) 0.012(2) O4 0.071(4) 0.061(3) 0.043(3) -0.029(3) 0.005(3) -0.009(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 K1 O1 2.942(5) 7_556 ? K1 O1 2.942(5) 11_565 ? K1 O1 2.942(5) 4_655 ? K1 O2 3.231(6) 12_566 ? K1 O2 3.231(6) 8_656 ? K1 O2 3.231(6) 2_665 ? K1 O4 3.336(6) 12_566 ? K1 O4 3.336(6) 8_656 ? K1 O4 3.336(6) 2_665 ? K1 P1 3.675(2) 2_665 ? K1 W1 3.675(2) 2_665 ? K1 W1 3.675(2) 12_566 ? K2 O3 2.974(6) 2_665 ? K2 O3 2.974(6) 8_656 ? K2 O3 2.974(6) 12_566 ? K2 O2 3.056(6) 6_665 ? K2 O2 3.056(6) 10_656 ? K2 O2 3.056(6) 3_566 ? K2 O4 3.192(6) 12_566 ? K2 O4 3.192(6) 8_656 ? K2 O4 3.192(6) 2_665 ? K2 O4 3.365(6) 6_665 ? K2 O4 3.365(6) 3_566 ? K2 O4 3.365(6) 10_656 ? Sc1 O2 2.059(5) 6_554 ? Sc1 O2 2.059(5) 10_545 ? Sc1 O2 2.059(5) 3_455 ? Sc1 O1 2.076(5) 5 ? Sc1 O1 2.076(5) 9 ? Sc1 O1 2.076(5) . ? Sc1 W1 3.3595(14) 5 ? Sc1 W1 3.3595(14) 9 ? Sc1 K2 3.788(3) 1_444 ? Sc1 K1 3.9662(15) 3_456 ? Sc1 K1 3.9662(15) 2_564 ? Sc2 O3 2.064(4) 7_556 ? Sc2 O3 2.064(4) 4_655 ? Sc2 O3 2.064(4) 11_565 ? Sc2 O4 2.079(5) . ? Sc2 O4 2.079(5) 5 ? Sc2 O4 2.079(5) 9 ? Sc2 K2 3.9151(12) 2_664 ? Sc2 K2 3.9151(12) 4_646 ? Sc2 K2 3.9151(12) 3_466 ? P1 O4 1.574(5) . ? P1 O3 1.576(4) . ? P1 O1 1.586(4) . ? P1 O2 1.620(5) . ? P1 K2 3.5888(15) 3_466 ? P1 K1 3.675(2) 2_664 ? P1 K2 3.7195(17) 2_664 ? P1 K1 3.818(3) 4_645 ? O1 K1 2.942(5) 4_645 ? O2 Sc1 2.059(5) 3 ? O2 K2 3.056(6) 3_466 ? O2 K1 3.231(6) 2_664 ? O3 Sc2 2.064(4) 4_645 ? O3 K2 2.974(6) 2_664 ? O4 K2 3.192(6) 2_664 ? O4 K1 3.336(6) 2_664 ? O4 K2 3.365(6) 3_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 K1 O1 93.17(18) 7_556 11_565 ? O1 K1 O1 93.17(18) 7_556 4_655 ? O1 K1 O1 93.17(18) 11_565 4_655 ? O1 K1 O2 149.67(19) 7_556 12_566 ? O1 K1 O2 57.24(12) 11_565 12_566 ? O1 K1 O2 82.98(14) 4_655 12_566 ? O1 K1 O2 57.24(12) 7_556 8_656 ? O1 K1 O2 82.98(14) 11_565 8_656 ? O1 K1 O2 149.67(19) 4_655 8_656 ? O2 K1 O2 118.53(5) 12_566 8_656 ? O1 K1 O2 82.98(14) 7_556 2_665 ? O1 K1 O2 149.67(19) 11_565 2_665 ? O1 K1 O2 57.24(12) 4_655 2_665 ? O2 K1 O2 118.53(5) 12_566 2_665 ? O2 K1 O2 118.53(5) 8_656 2_665 ? O1 K1 O4 164.04(15) 7_556 12_566 ? O1 K1 O4 102.45(12) 11_565 12_566 ? O1 K1 O4 82.85(14) 4_655 12_566 ? O2 K1 O4 45.36(12) 12_566 12_566 ? O2 K1 O4 127.40(17) 8_656 12_566 ? O2 K1 O4 81.89(14) 2_665 12_566 ? O1 K1 O4 102.45(12) 7_556 8_656 ? O1 K1 O4 82.85(14) 11_565 8_656 ? O1 K1 O4 164.04(15) 4_655 8_656 ? O2 K1 O4 81.89(14) 12_566 8_656 ? O2 K1 O4 45.36(12) 8_656 8_656 ? O2 K1 O4 127.40(17) 2_665 8_656 ? O4 K1 O4 82.94(17) 12_566 8_656 ? O1 K1 O4 82.85(14) 7_556 2_665 ? O1 K1 O4 164.04(15) 11_565 2_665 ? O1 K1 O4 102.45(12) 4_655 2_665 ? O2 K1 O4 127.40(17) 12_566 2_665 ? O2 K1 O4 81.89(14) 8_656 2_665 ? O2 K1 O4 45.36(12) 2_665 2_665 ? O4 K1 O4 82.94(17) 12_566 2_665 ? O4 K1 O4 82.94(17) 8_656 2_665 ? O1 K1 P1 94.84(11) 7_556 2_665 ? O1 K1 P1 169.45(9) 11_565 2_665 ? O1 K1 P1 79.55(9) 4_655 2_665 ? O2 K1 P1 113.81(11) 12_566 2_665 ? O2 K1 P1 107.16(11) 8_656 2_665 ? O2 K1 P1 26.14(9) 2_665 2_665 ? O4 K1 P1 69.27(10) 12_566 2_665 ? O4 K1 P1 102.06(14) 8_656 2_665 ? O4 K1 P1 25.36(9) 2_665 2_665 ? O1 K1 W1 94.84(11) 7_556 2_665 ? O1 K1 W1 169.45(9) 11_565 2_665 ? O1 K1 W1 79.55(9) 4_655 2_665 ? O2 K1 W1 113.81(11) 12_566 2_665 ? O2 K1 W1 107.16(11) 8_656 2_665 ? O2 K1 W1 26.14(9) 2_665 2_665 ? O4 K1 W1 69.27(10) 12_566 2_665 ? O4 K1 W1 102.06(14) 8_656 2_665 ? O4 K1 W1 25.36(9) 2_665 2_665 ? P1 K1 W1 0.000(16) 2_665 2_665 ? O1 K1 W1 169.45(9) 7_556 12_566 ? O1 K1 W1 79.55(9) 11_565 12_566 ? O1 K1 W1 94.84(11) 4_655 12_566 ? O2 K1 W1 26.14(9) 12_566 12_566 ? O2 K1 W1 113.81(11) 8_656 12_566 ? O2 K1 W1 107.16(11) 2_665 12_566 ? O4 K1 W1 25.36(9) 12_566 12_566 ? O4 K1 W1 69.27(10) 8_656 12_566 ? O4 K1 W1 102.06(14) 2_665 12_566 ? P1 K1 W1 93.36(7) 2_665 12_566 ? W1 K1 W1 93.36(7) 2_665 12_566 ? O3 K2 O3 99.60(13) 2_665 8_656 ? O3 K2 O3 99.60(13) 2_665 12_566 ? O3 K2 O3 99.60(14) 8_656 12_566 ? O3 K2 O2 100.51(15) 2_665 6_665 ? O3 K2 O2 97.58(13) 8_656 6_665 ? O3 K2 O2 150.87(15) 12_566 6_665 ? O3 K2 O2 150.87(15) 2_665 10_656 ? O3 K2 O2 100.51(15) 8_656 10_656 ? O3 K2 O2 97.58(13) 12_566 10_656 ? O2 K2 O2 56.04(16) 6_665 10_656 ? O3 K2 O2 97.58(13) 2_665 3_566 ? O3 K2 O2 150.87(15) 8_656 3_566 ? O3 K2 O2 100.51(15) 12_566 3_566 ? O2 K2 O2 56.04(16) 6_665 3_566 ? O2 K2 O2 56.04(16) 10_656 3_566 ? O3 K2 O4 52.28(13) 2_665 12_566 ? O3 K2 O4 114.90(17) 8_656 12_566 ? O3 K2 O4 48.77(12) 12_566 12_566 ? O2 K2 O4 139.29(15) 6_665 12_566 ? O2 K2 O4 133.10(14) 10_656 12_566 ? O2 K2 O4 94.21(13) 3_566 12_566 ? O3 K2 O4 114.90(17) 2_665 8_656 ? O3 K2 O4 48.77(12) 8_656 8_656 ? O3 K2 O4 52.28(13) 12_566 8_656 ? O2 K2 O4 133.10(15) 6_665 8_656 ? O2 K2 O4 94.21(13) 10_656 8_656 ? O2 K2 O4 139.29(15) 3_566 8_656 ? O4 K2 O4 87.60(16) 12_566 8_656 ? O3 K2 O4 48.77(12) 2_665 2_665 ? O3 K2 O4 52.28(13) 8_656 2_665 ? O3 K2 O4 114.90(17) 12_566 2_665 ? O2 K2 O4 94.21(13) 6_665 2_665 ? O2 K2 O4 139.29(15) 10_656 2_665 ? O2 K2 O4 133.10(15) 3_566 2_665 ? O4 K2 O4 87.60(16) 12_566 2_665 ? O4 K2 O4 87.60(16) 8_656 2_665 ? O3 K2 O4 86.17(13) 2_665 6_665 ? O3 K2 O4 56.94(12) 8_656 6_665 ? O3 K2 O4 156.54(14) 12_566 6_665 ? O2 K2 O4 46.18(12) 6_665 6_665 ? O2 K2 O4 87.35(15) 10_656 6_665 ? O2 K2 O4 101.23(16) 3_566 6_665 ? O4 K2 O4 137.36(11) 12_566 6_665 ? O4 K2 O4 104.63(3) 8_656 6_665 ? O4 K2 O4 53.19(19) 2_665 6_665 ? O3 K2 O4 56.94(12) 2_665 3_566 ? O3 K2 O4 156.54(14) 8_656 3_566 ? O3 K2 O4 86.17(13) 12_566 3_566 ? O2 K2 O4 87.35(15) 6_665 3_566 ? O2 K2 O4 101.23(16) 10_656 3_566 ? O2 K2 O4 46.18(12) 3_566 3_566 ? O4 K2 O4 53.19(19) 12_566 3_566 ? O4 K2 O4 137.36(11) 8_656 3_566 ? O4 K2 O4 104.63(3) 2_665 3_566 ? O4 K2 O4 115.48(7) 6_665 3_566 ? O3 K2 O4 156.54(14) 2_665 10_656 ? O3 K2 O4 86.17(13) 8_656 10_656 ? O3 K2 O4 56.94(12) 12_566 10_656 ? O2 K2 O4 101.23(16) 6_665 10_656 ? O2 K2 O4 46.18(12) 10_656 10_656 ? O2 K2 O4 87.35(15) 3_566 10_656 ? O4 K2 O4 104.63(3) 12_566 10_656 ? O4 K2 O4 53.19(19) 8_656 10_656 ? O4 K2 O4 137.36(11) 2_665 10_656 ? O4 K2 O4 115.48(7) 6_665 10_656 ? O4 K2 O4 115.48(7) 3_566 10_656 ? O2 Sc1 O2 88.4(2) 6_554 10_545 ? O2 Sc1 O2 88.4(2) 6_554 3_455 ? O2 Sc1 O2 88.4(2) 10_545 3_455 ? O2 Sc1 O1 91.74(19) 6_554 5 ? O2 Sc1 O1 88.1(2) 10_545 5 ? O2 Sc1 O1 176.5(2) 3_455 5 ? O2 Sc1 O1 176.5(2) 6_554 9 ? O2 Sc1 O1 91.74(19) 10_545 9 ? O2 Sc1 O1 88.1(2) 3_455 9 ? O1 Sc1 O1 91.7(2) 5 9 ? O2 Sc1 O1 88.1(2) 6_554 . ? O2 Sc1 O1 176.5(2) 10_545 . ? O2 Sc1 O1 91.74(19) 3_455 . ? O1 Sc1 O1 91.7(2) 5 . ? O1 Sc1 O1 91.7(2) 9 . ? O2 Sc1 W1 111.70(15) 6_554 5 ? O2 Sc1 W1 85.16(15) 10_545 5 ? O2 Sc1 W1 158.63(16) 3_455 5 ? O1 Sc1 W1 20.31(13) 5 5 ? O1 Sc1 W1 71.79(16) 9 5 ? O1 Sc1 W1 95.88(15) . 5 ? O2 Sc1 W1 158.63(16) 6_554 9 ? O2 Sc1 W1 111.70(15) 10_545 9 ? O2 Sc1 W1 85.16(15) 3_455 9 ? O1 Sc1 W1 95.88(15) 5 9 ? O1 Sc1 W1 20.31(13) 9 9 ? O1 Sc1 W1 71.79(16) . 9 ? W1 Sc1 W1 78.36(4) 5 9 ? O2 Sc1 K2 53.64(15) 6_554 1_444 ? O2 Sc1 K2 53.64(15) 10_545 1_444 ? O2 Sc1 K2 53.64(15) 3_455 1_444 ? O1 Sc1 K2 124.02(15) 5 1_444 ? O1 Sc1 K2 124.02(15) 9 1_444 ? O1 Sc1 K2 124.02(15) . 1_444 ? W1 Sc1 K2 133.15(3) 5 1_444 ? W1 Sc1 K2 133.15(3) 9 1_444 ? O2 Sc1 K1 54.31(17) 6_554 3_456 ? O2 Sc1 K1 64.21(17) 10_545 3_456 ? O2 Sc1 K1 131.91(16) 3_455 3_456 ? O1 Sc1 K1 46.25(14) 5 3_456 ? O1 Sc1 K1 128.75(17) 9 3_456 ? O1 Sc1 K1 113.35(15) . 3_456 ? W1 Sc1 K1 62.16(4) 5 3_456 ? W1 Sc1 K1 140.40(6) 9 3_456 ? K2 Sc1 K1 78.64(3) 1_444 3_456 ? O2 Sc1 K1 131.91(16) 6_554 2_564 ? O2 Sc1 K1 54.31(17) 10_545 2_564 ? O2 Sc1 K1 64.21(17) 3_455 2_564 ? O1 Sc1 K1 113.35(15) 5 2_564 ? O1 Sc1 K1 46.25(14) 9 2_564 ? O1 Sc1 K1 128.75(17) . 2_564 ? W1 Sc1 K1 95.78(3) 5 2_564 ? W1 Sc1 K1 62.16(4) 9 2_564 ? K2 Sc1 K1 78.64(3) 1_444 2_564 ? K1 Sc1 K1 116.22(2) 3_456 2_564 ? O3 Sc2 O3 94.0(2) 7_556 4_655 ? O3 Sc2 O3 94.0(2) 7_556 11_565 ? O3 Sc2 O3 94.0(2) 4_655 11_565 ? O3 Sc2 O4 82.2(2) 7_556 . ? O3 Sc2 O4 94.44(19) 4_655 . ? O3 Sc2 O4 171.0(2) 11_565 . ? O3 Sc2 O4 94.44(19) 7_556 5 ? O3 Sc2 O4 171.0(2) 4_655 5 ? O3 Sc2 O4 82.2(2) 11_565 5 ? O4 Sc2 O4 90.0(2) . 5 ? O3 Sc2 O4 171.0(2) 7_556 9 ? O3 Sc2 O4 82.2(2) 4_655 9 ? O3 Sc2 O4 94.44(19) 11_565 9 ? O4 Sc2 O4 90.0(2) . 9 ? O4 Sc2 O4 90.0(2) 5 9 ? O3 Sc2 K2 48.33(16) 7_556 2_664 ? O3 Sc2 K2 129.52(14) 4_655 2_664 ? O3 Sc2 K2 117.10(14) 11_565 2_664 ? O4 Sc2 K2 54.46(16) . 2_664 ? O4 Sc2 K2 59.24(16) 5 2_664 ? O4 Sc2 K2 129.23(18) 9 2_664 ? O3 Sc2 K2 129.52(14) 7_556 4_646 ? O3 Sc2 K2 117.10(14) 4_655 4_646 ? O3 Sc2 K2 48.33(16) 11_565 4_646 ? O4 Sc2 K2 129.23(18) . 4_646 ? O4 Sc2 K2 54.46(16) 5 4_646 ? O4 Sc2 K2 59.24(16) 9 4_646 ? K2 Sc2 K2 113.22(3) 2_664 4_646 ? O3 Sc2 K2 117.10(14) 7_556 3_466 ? O3 Sc2 K2 48.33(16) 4_655 3_466 ? O3 Sc2 K2 129.52(14) 11_565 3_466 ? O4 Sc2 K2 59.24(16) . 3_466 ? O4 Sc2 K2 129.23(18) 5 3_466 ? O4 Sc2 K2 54.46(16) 9 3_466 ? K2 Sc2 K2 113.22(3) 2_664 3_466 ? K2 Sc2 K2 113.22(3) 4_646 3_466 ? O4 P1 O3 108.3(3) . . ? O4 P1 O1 113.4(3) . . ? O3 P1 O1 112.9(3) . . ? O4 P1 O2 105.0(3) . . ? O3 P1 O2 109.9(3) . . ? O1 P1 O2 107.0(3) . . ? O4 P1 K2 69.1(2) . 3_466 ? O3 P1 K2 164.48(17) . 3_466 ? O1 P1 K2 81.4(2) . 3_466 ? O2 P1 K2 57.98(19) . 3_466 ? O4 P1 K1 65.2(2) . 2_664 ? O3 P1 K1 80.07(18) . 2_664 ? O1 P1 K1 165.8(2) . 2_664 ? O2 P1 K1 61.5(2) . 2_664 ? K2 P1 K1 85.16(4) 3_466 2_664 ? O4 P1 K2 58.5(2) . 2_664 ? O3 P1 K2 50.4(2) . 2_664 ? O1 P1 K2 125.57(18) . 2_664 ? O2 P1 K2 127.4(2) . 2_664 ? K2 P1 K2 126.89(4) 3_466 2_664 ? K1 P1 K2 66.76(6) 2_664 2_664 ? O4 P1 K1 148.7(2) . 4_645 ? O3 P1 K1 102.3(2) . 4_645 ? O1 P1 K1 45.84(18) . 4_645 ? O2 P1 K1 69.5(2) . 4_645 ? K2 P1 K1 83.09(4) 3_466 4_645 ? K1 P1 K1 128.02(6) 2_664 4_645 ? K2 P1 K1 149.63(4) 2_664 4_645 ? P1 O1 Sc1 132.7(3) . . ? P1 O1 K1 111.4(2) . 4_645 ? Sc1 O1 K1 103.10(18) . 4_645 ? P1 O2 Sc1 167.3(4) . 3 ? P1 O2 K2 95.3(2) . 3_466 ? Sc1 O2 K2 93.51(17) 3 3_466 ? P1 O2 K1 92.4(2) . 2_664 ? Sc1 O2 K1 94.5(2) 3 2_664 ? K2 O2 K1 102.81(16) 3_466 2_664 ? P1 O3 Sc2 152.3(4) . 4_645 ? P1 O3 K2 105.5(2) . 2_664 ? Sc2 O3 K2 100.43(19) 4_645 2_664 ? P1 O4 Sc2 152.9(4) . . ? P1 O4 K2 96.7(2) . 2_664 ? Sc2 O4 K2 93.53(19) . 2_664 ? P1 O4 K1 89.4(2) . 2_664 ? Sc2 O4 K1 117.3(2) . 2_664 ? K2 O4 K1 77.07(14) 2_664 2_664 ? P1 O4 K2 85.0(2) . 3_466 ? Sc2 O4 K2 88.69(19) . 3_466 ? K2 O4 K2 171.21(19) 2_664 3_466 ? K1 O4 K2 94.35(16) 2_664 3_466 ? ########End data_KScMo _audit_creation_date 2010-02-11T11:29:49-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _publ_requested_category FI #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'O12 Mo P2 Sc2, 2(K)' _chemical_formula_sum 'K2 Mo O12 P2 Sc2' _chemical_formula_weight 517.35 _chemical_absolute_configuration ad #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting cubic _symmetry_space_group_name_H-M 'P 21 3' _symmetry_space_group_name_Hall 'P 2ac 2ab 3' _symmetry_Int_Tables_number 198 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' 'y, z, x' '-y+1/2, -z, x+1/2' 'y+1/2, -z+1/2, -x' '-y, z+1/2, -x+1/2' 'z, x, y' '-z, x+1/2, -y+1/2' '-z+1/2, -x, y+1/2' 'z+1/2, -x+1/2, -y' _cell_length_a 10.3179(2) _cell_length_b 10.3179(2) _cell_length_c 10.3179(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1098.43(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3723 _cell_measurement_theta_min 3.42 _cell_measurement_theta_max 29.94 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description tetrahedron _exptl_crystal_colour colorless _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.07 _exptl_crystal_density_diffrn 3.128 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 992 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 3.425 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Blessing, 1995)' _exptl_absorpt_correction_T_min 0.7214 _exptl_absorpt_correction_T_max 0.7683 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_probe x-ray _diffrn_source 'fine focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type XCalibur-3 _diffrn_measurement_method '\f and \w scans' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_av_unetI/netI 0.0683 _diffrn_reflns_number 3723 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.42 _diffrn_reflns_theta_max 29.94 _diffrn_reflns_theta_full 29.94 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_total 3723 _reflns_number_gt 3332 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'CrysAlis CCD (Oxford Diffraction Ltd., 2006)' _computing_cell_refinement 'CrysAlis CCD (Oxford Diffraction Ltd., 2006)' _computing_data_reduction 'CrysAlis RED (Oxford Diffraction Ltd., 2006)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens undef #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Twinning was detected. Following twin law was determined 2-axis ( 0 1 1 ) [ 0 1 1 ], Angle () [] = 0.00 Deg, Freq = 372 (-1.000 0.000 0.000) (h1) (h2) Nr Overlap = 3723 ( 0.000 0.000 1.000) * (k1) = (k2) BASF = 0.38 ( 0.000 1.000 0.000) (l1) (l2) DEL-R =-0.089 The refinment was done with MERG 0 and BASF 0.38 and determined twin matrix. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0357P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment undef _refine_ls_extinction_method none _refine_ls_number_reflns 3723 _refine_ls_number_parameters 61 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0458 _refine_ls_R_factor_gt 0.0399 _refine_ls_wR_factor_ref 0.0802 _refine_ls_wR_factor_gt 0.0789 _refine_ls_goodness_of_fit_ref 0.969 _refine_ls_restrained_S_all 0.969 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details '(Flack, 1983)' _refine_ls_abs_structure_Flack 0.18(9) _refine_diff_density_max 0.444 _refine_diff_density_min -0.399 _refine_diff_density_rms 0.088 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sc Sc 0.2519 0.3716 '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' 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 K1 K 0.70371(15) 0.70371(15) 0.70371(15) 0.0812(9) Uani 1 3 d S . . K2 K 0.93114(10) 0.93114(10) 0.93114(10) 0.0537(5) Uani 1 3 d S . . Sc1 Sc 0.14322(7) 0.14322(7) 0.14322(7) 0.0273(3) Uani 1 3 d S . . Sc2 Sc 0.41430(9) 0.41430(9) 0.41430(9) 0.0401(3) Uani 1 3 d S . . P1 P 0.45769(5) 0.22906(5) 0.12701(5) 0.01777(9) Uani 0.67 1 d P . . Mo1 Mo 0.45769(5) 0.22906(5) 0.12701(5) 0.01777(9) Uani 0.33 1 d P . . O1 O 0.3123(3) 0.2334(3) 0.0794(3) 0.0443(8) Uani 1 1 d . . . O2 O 0.5478(3) 0.3012(3) 0.0214(3) 0.0445(8) Uani 1 1 d . . . O3 O 0.5065(3) 0.0863(3) 0.1510(3) 0.0480(9) Uani 1 1 d . . . O4 O 0.4770(3) 0.3082(4) 0.2551(3) 0.0557(11) 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 K1 0.0812(9) 0.0812(9) 0.0812(9) 0.0016(8) 0.0016(8) 0.0016(8) K2 0.0537(5) 0.0537(5) 0.0537(5) -0.0119(5) -0.0119(5) -0.0119(5) Sc1 0.0273(3) 0.0273(3) 0.0273(3) -0.0012(3) -0.0012(3) -0.0012(3) Sc2 0.0401(3) 0.0401(3) 0.0401(3) -0.0005(4) -0.0005(4) -0.0005(4) P1 0.0177(3) 0.0186(3) 0.0170(3) -0.0022(2) 0.0020(2) -0.0003(2) Mo1 0.0177(3) 0.0186(3) 0.0170(3) -0.0022(2) 0.0020(2) -0.0003(2) O1 0.0312(15) 0.0392(16) 0.062(2) 0.0042(16) -0.0030(14) -0.0105(13) O2 0.052(2) 0.0479(19) 0.0336(16) 0.0126(13) 0.0163(16) -0.0017(14) O3 0.0446(18) 0.0406(17) 0.059(2) 0.0035(16) 0.0016(15) 0.0233(14) O4 0.055(2) 0.069(2) 0.0425(19) -0.0258(17) 0.0082(17) -0.0169(17) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 K1 O1 2.942(3) 4_655 ? K1 O1 2.942(3) 11_565 ? K1 O1 2.942(3) 7_556 ? K1 O2 3.180(3) 2_665 ? K1 O2 3.180(3) 12_566 ? K1 O2 3.180(3) 8_656 ? K1 O4 3.339(4) 12_566 ? K1 O4 3.339(4) 2_665 ? K1 O4 3.339(4) 8_656 ? K1 Mo1 3.6487(15) 12_566 ? K1 P1 3.6487(15) 12_566 ? K1 P1 3.6487(15) 2_665 ? K2 O3 2.967(3) 2_665 ? K2 O3 2.967(3) 12_566 ? K2 O3 2.967(3) 8_656 ? K2 O2 3.052(3) 3_566 ? K2 O2 3.052(3) 6_665 ? K2 O2 3.052(3) 10_656 ? K2 O4 3.209(4) 12_566 ? K2 O4 3.209(4) 2_665 ? K2 O4 3.209(4) 8_656 ? K2 O4 3.339(4) 3_566 ? K2 O4 3.339(4) 10_656 ? K2 O4 3.339(4) 6_665 ? Sc1 O2 2.045(3) 3_455 ? Sc1 O2 2.045(3) 6_554 ? Sc1 O2 2.045(3) 10_545 ? Sc1 O1 2.084(3) 9 ? Sc1 O1 2.084(3) . ? Sc1 O1 2.084(3) 5 ? Sc1 Mo1 3.3676(11) 9 ? Sc1 Mo1 3.3676(11) 5 ? Sc1 K2 3.790(2) 1_444 ? Sc1 K1 3.9620(10) 2_564 ? Sc1 K1 3.9620(10) 4_645 ? Sc2 O3 2.066(3) 4_655 ? Sc2 O3 2.066(3) 7_556 ? Sc2 O3 2.066(3) 11_565 ? Sc2 O4 2.077(4) 9 ? Sc2 O4 2.077(4) . ? Sc2 O4 2.077(4) 5 ? Sc2 K2 3.9086(7) 3_466 ? Sc2 K2 3.9086(7) 2_664 ? Sc2 K2 3.9086(7) 4_646 ? P1 O4 1.566(3) . ? P1 O3 1.576(3) . ? P1 O1 1.579(3) . ? P1 O2 1.615(3) . ? P1 K2 3.5675(10) 3_466 ? P1 K1 3.6487(15) 2_664 ? P1 K2 3.7276(11) 2_664 ? P1 K1 3.806(2) 4_645 ? O1 K1 2.942(3) 4_645 ? O2 Sc1 2.045(3) 3 ? O2 K2 3.052(3) 3_466 ? O2 K1 3.180(3) 2_664 ? O3 Sc2 2.066(3) 4_645 ? O3 K2 2.967(3) 2_664 ? O4 K2 3.209(4) 2_664 ? O4 K2 3.339(4) 3_466 ? O4 K1 3.339(4) 2_664 ? 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 K1 O1 93.07(12) 4_655 11_565 ? O1 K1 O1 93.07(12) 4_655 7_556 ? O1 K1 O1 93.07(12) 11_565 7_556 ? O1 K1 O2 57.29(7) 4_655 2_665 ? O1 K1 O2 149.46(12) 11_565 2_665 ? O1 K1 O2 82.34(8) 7_556 2_665 ? O1 K1 O2 82.34(8) 4_655 12_566 ? O1 K1 O2 57.29(7) 11_565 12_566 ? O1 K1 O2 149.46(12) 7_556 12_566 ? O2 K1 O2 118.70(3) 2_665 12_566 ? O1 K1 O2 149.46(12) 4_655 8_656 ? O1 K1 O2 82.34(8) 11_565 8_656 ? O1 K1 O2 57.29(7) 7_556 8_656 ? O2 K1 O2 118.70(3) 2_665 8_656 ? O2 K1 O2 118.70(3) 12_566 8_656 ? O1 K1 O4 82.50(9) 4_655 12_566 ? O1 K1 O4 102.53(8) 11_565 12_566 ? O1 K1 O4 163.96(9) 7_556 12_566 ? O2 K1 O4 82.30(9) 2_665 12_566 ? O2 K1 O4 45.41(8) 12_566 12_566 ? O2 K1 O4 128.01(10) 8_656 12_566 ? O1 K1 O4 102.53(8) 4_655 2_665 ? O1 K1 O4 163.96(9) 11_565 2_665 ? O1 K1 O4 82.50(9) 7_556 2_665 ? O2 K1 O4 45.41(8) 2_665 2_665 ? O2 K1 O4 128.01(10) 12_566 2_665 ? O2 K1 O4 82.30(9) 8_656 2_665 ? O4 K1 O4 83.43(11) 12_566 2_665 ? O1 K1 O4 163.96(9) 4_655 8_656 ? O1 K1 O4 82.50(9) 11_565 8_656 ? O1 K1 O4 102.53(8) 7_556 8_656 ? O2 K1 O4 128.01(10) 2_665 8_656 ? O2 K1 O4 82.30(9) 12_566 8_656 ? O2 K1 O4 45.41(8) 8_656 8_656 ? O4 K1 O4 83.43(11) 12_566 8_656 ? O4 K1 O4 83.43(11) 2_665 8_656 ? O1 K1 Mo1 94.40(6) 4_655 12_566 ? O1 K1 Mo1 79.55(6) 11_565 12_566 ? O1 K1 Mo1 169.76(6) 7_556 12_566 ? O2 K1 Mo1 107.62(7) 2_665 12_566 ? O2 K1 Mo1 26.22(5) 12_566 12_566 ? O2 K1 Mo1 114.18(7) 8_656 12_566 ? O4 K1 Mo1 25.41(6) 12_566 12_566 ? O4 K1 Mo1 102.65(9) 2_665 12_566 ? O4 K1 Mo1 69.66(7) 8_656 12_566 ? O1 K1 P1 94.40(6) 4_655 12_566 ? O1 K1 P1 79.55(6) 11_565 12_566 ? O1 K1 P1 169.76(6) 7_556 12_566 ? O2 K1 P1 107.62(7) 2_665 12_566 ? O2 K1 P1 26.22(5) 12_566 12_566 ? O2 K1 P1 114.18(7) 8_656 12_566 ? O4 K1 P1 25.41(6) 12_566 12_566 ? O4 K1 P1 102.65(9) 2_665 12_566 ? O4 K1 P1 69.66(7) 8_656 12_566 ? Mo1 K1 P1 0.00(2) 12_566 12_566 ? O1 K1 P1 79.55(6) 4_655 2_665 ? O1 K1 P1 169.76(6) 11_565 2_665 ? O1 K1 P1 94.40(6) 7_556 2_665 ? O2 K1 P1 26.22(5) 2_665 2_665 ? O2 K1 P1 114.18(7) 12_566 2_665 ? O2 K1 P1 107.62(7) 8_656 2_665 ? O4 K1 P1 69.66(7) 12_566 2_665 ? O4 K1 P1 25.41(6) 2_665 2_665 ? O4 K1 P1 102.65(9) 8_656 2_665 ? Mo1 K1 P1 93.83(5) 12_566 2_665 ? P1 K1 P1 93.83(5) 12_566 2_665 ? O3 K2 O3 99.52(9) 2_665 12_566 ? O3 K2 O3 99.52(9) 2_665 8_656 ? O3 K2 O3 99.52(9) 12_566 8_656 ? O3 K2 O2 97.21(8) 2_665 3_566 ? O3 K2 O2 101.41(9) 12_566 3_566 ? O3 K2 O2 150.53(10) 8_656 3_566 ? O3 K2 O2 101.41(9) 2_665 6_665 ? O3 K2 O2 150.53(10) 12_566 6_665 ? O3 K2 O2 97.21(8) 8_656 6_665 ? O2 K2 O2 55.57(9) 3_566 6_665 ? O3 K2 O2 150.53(10) 2_665 10_656 ? O3 K2 O2 97.21(8) 12_566 10_656 ? O3 K2 O2 101.41(9) 8_656 10_656 ? O2 K2 O2 55.57(9) 3_566 10_656 ? O2 K2 O2 55.57(9) 6_665 10_656 ? O3 K2 O4 52.47(8) 2_665 12_566 ? O3 K2 O4 48.53(9) 12_566 12_566 ? O3 K2 O4 114.87(11) 8_656 12_566 ? O2 K2 O4 94.56(8) 3_566 12_566 ? O2 K2 O4 140.21(10) 6_665 12_566 ? O2 K2 O4 132.11(8) 10_656 12_566 ? O3 K2 O4 48.53(9) 2_665 2_665 ? O3 K2 O4 114.87(11) 12_566 2_665 ? O3 K2 O4 52.47(8) 8_656 2_665 ? O2 K2 O4 132.11(9) 3_566 2_665 ? O2 K2 O4 94.56(8) 6_665 2_665 ? O2 K2 O4 140.21(10) 10_656 2_665 ? O4 K2 O4 87.65(9) 12_566 2_665 ? O3 K2 O4 114.87(11) 2_665 8_656 ? O3 K2 O4 52.47(8) 12_566 8_656 ? O3 K2 O4 48.53(9) 8_656 8_656 ? O2 K2 O4 140.21(10) 3_566 8_656 ? O2 K2 O4 132.11(8) 6_665 8_656 ? O2 K2 O4 94.56(8) 10_656 8_656 ? O4 K2 O4 87.65(9) 12_566 8_656 ? O4 K2 O4 87.65(9) 2_665 8_656 ? O3 K2 O4 57.14(8) 2_665 3_566 ? O3 K2 O4 85.89(8) 12_566 3_566 ? O3 K2 O4 156.66(9) 8_656 3_566 ? O2 K2 O4 46.19(8) 3_566 3_566 ? O2 K2 O4 88.27(9) 6_665 3_566 ? O2 K2 O4 100.38(10) 10_656 3_566 ? O4 K2 O4 53.07(12) 12_566 3_566 ? O4 K2 O4 104.612(18) 2_665 3_566 ? O4 K2 O4 137.30(7) 8_656 3_566 ? O3 K2 O4 156.66(9) 2_665 10_656 ? O3 K2 O4 57.14(8) 12_566 10_656 ? O3 K2 O4 85.89(8) 8_656 10_656 ? O2 K2 O4 88.27(9) 3_566 10_656 ? O2 K2 O4 100.38(10) 6_665 10_656 ? O2 K2 O4 46.19(8) 10_656 10_656 ? O4 K2 O4 104.611(18) 12_566 10_656 ? O4 K2 O4 137.30(7) 2_665 10_656 ? O4 K2 O4 53.07(12) 8_656 10_656 ? O4 K2 O4 115.53(5) 3_566 10_656 ? O3 K2 O4 85.89(8) 2_665 6_665 ? O3 K2 O4 156.66(9) 12_566 6_665 ? O3 K2 O4 57.14(8) 8_656 6_665 ? O2 K2 O4 100.38(10) 3_566 6_665 ? O2 K2 O4 46.19(8) 6_665 6_665 ? O2 K2 O4 88.27(9) 10_656 6_665 ? O4 K2 O4 137.30(7) 12_566 6_665 ? O4 K2 O4 53.07(12) 2_665 6_665 ? O4 K2 O4 104.611(18) 8_656 6_665 ? O4 K2 O4 115.53(5) 3_566 6_665 ? O4 K2 O4 115.53(5) 10_656 6_665 ? O2 Sc1 O2 88.16(12) 3_455 6_554 ? O2 Sc1 O2 88.16(12) 3_455 10_545 ? O2 Sc1 O2 88.16(12) 6_554 10_545 ? O2 Sc1 O1 89.11(13) 3_455 9 ? O2 Sc1 O1 177.14(14) 6_554 9 ? O2 Sc1 O1 90.88(12) 10_545 9 ? O2 Sc1 O1 90.88(12) 3_455 . ? O2 Sc1 O1 89.11(13) 6_554 . ? O2 Sc1 O1 177.14(14) 10_545 . ? O1 Sc1 O1 91.80(13) 9 . ? O2 Sc1 O1 177.14(14) 3_455 5 ? O2 Sc1 O1 90.88(12) 6_554 5 ? O2 Sc1 O1 89.11(13) 10_545 5 ? O1 Sc1 O1 91.80(13) 9 5 ? O1 Sc1 O1 91.80(13) . 5 ? O2 Sc1 Mo1 85.68(9) 3_455 9 ? O2 Sc1 Mo1 160.19(9) 6_554 9 ? O2 Sc1 Mo1 110.41(9) 10_545 9 ? O1 Sc1 Mo1 19.99(9) 9 9 ? O1 Sc1 Mo1 72.19(10) . 9 ? O1 Sc1 Mo1 96.10(10) 5 9 ? O2 Sc1 Mo1 160.19(9) 3_455 5 ? O2 Sc1 Mo1 110.41(9) 6_554 5 ? O2 Sc1 Mo1 85.68(9) 10_545 5 ? O1 Sc1 Mo1 72.19(10) 9 5 ? O1 Sc1 Mo1 96.10(10) . 5 ? O1 Sc1 Mo1 19.99(9) 5 5 ? Mo1 Sc1 Mo1 78.90(3) 9 5 ? O2 Sc1 K2 53.44(9) 3_455 1_444 ? O2 Sc1 K2 53.44(9) 6_554 1_444 ? O2 Sc1 K2 53.44(9) 10_545 1_444 ? O1 Sc1 K2 123.98(9) 9 1_444 ? O1 Sc1 K2 123.98(9) . 1_444 ? O1 Sc1 K2 123.98(9) 5 1_444 ? Mo1 Sc1 K2 132.803(19) 9 1_444 ? Mo1 Sc1 K2 132.803(19) 5 1_444 ? O2 Sc1 K1 65.44(9) 3_455 2_564 ? O2 Sc1 K1 131.31(10) 6_554 2_564 ? O2 Sc1 K1 52.93(9) 10_545 2_564 ? O1 Sc1 K1 46.42(9) 9 2_564 ? O1 Sc1 K1 128.90(11) . 2_564 ? O1 Sc1 K1 113.43(10) 5 2_564 ? Mo1 Sc1 K1 61.94(3) 9 2_564 ? Mo1 Sc1 K1 96.06(2) 5 2_564 ? K2 Sc1 K1 78.43(2) 1_444 2_564 ? O2 Sc1 K1 52.93(9) 3_455 4_645 ? O2 Sc1 K1 65.44(9) 6_554 4_645 ? O2 Sc1 K1 131.31(10) 10_545 4_645 ? O1 Sc1 K1 113.43(10) 9 4_645 ? O1 Sc1 K1 46.42(9) . 4_645 ? O1 Sc1 K1 128.90(11) 5 4_645 ? Mo1 Sc1 K1 96.06(2) 9 4_645 ? Mo1 Sc1 K1 140.67(4) 5 4_645 ? K2 Sc1 K1 78.43(2) 1_444 4_645 ? K1 Sc1 K1 116.084(14) 2_564 4_645 ? O3 Sc2 O3 93.96(13) 4_655 7_556 ? O3 Sc2 O3 93.96(13) 4_655 11_565 ? O3 Sc2 O3 93.96(13) 7_556 11_565 ? O3 Sc2 O4 82.75(13) 4_655 9 ? O3 Sc2 O4 171.48(14) 7_556 9 ? O3 Sc2 O4 94.11(13) 11_565 9 ? O3 Sc2 O4 94.11(13) 4_655 . ? O3 Sc2 O4 82.75(13) 7_556 . ? O3 Sc2 O4 171.48(14) 11_565 . ? O4 Sc2 O4 89.62(13) 9 . ? O3 Sc2 O4 171.48(14) 4_655 5 ? O3 Sc2 O4 94.11(13) 7_556 5 ? O3 Sc2 O4 82.75(13) 11_565 5 ? O4 Sc2 O4 89.62(13) 9 5 ? O4 Sc2 O4 89.62(13) . 5 ? O3 Sc2 K2 48.31(9) 4_655 3_466 ? O3 Sc2 K2 117.10(9) 7_556 3_466 ? O3 Sc2 K2 129.51(9) 11_565 3_466 ? O4 Sc2 K2 55.08(11) 9 3_466 ? O4 Sc2 K2 58.67(11) . 3_466 ? O4 Sc2 K2 129.04(10) 5 3_466 ? O3 Sc2 K2 129.51(9) 4_655 2_664 ? O3 Sc2 K2 48.31(9) 7_556 2_664 ? O3 Sc2 K2 117.10(9) 11_565 2_664 ? O4 Sc2 K2 129.04(10) 9 2_664 ? O4 Sc2 K2 55.08(10) . 2_664 ? O4 Sc2 K2 58.67(11) 5 2_664 ? K2 Sc2 K2 113.231(19) 3_466 2_664 ? O3 Sc2 K2 117.10(9) 4_655 4_646 ? O3 Sc2 K2 129.51(9) 7_556 4_646 ? O3 Sc2 K2 48.31(9) 11_565 4_646 ? O4 Sc2 K2 58.67(11) 9 4_646 ? O4 Sc2 K2 129.04(10) . 4_646 ? O4 Sc2 K2 55.08(11) 5 4_646 ? K2 Sc2 K2 113.231(19) 3_466 4_646 ? K2 Sc2 K2 113.231(19) 2_664 4_646 ? O4 P1 O3 108.3(2) . . ? O4 P1 O1 111.59(16) . . ? O3 P1 O1 112.26(17) . . ? O4 P1 O2 104.82(18) . . ? O3 P1 O2 110.67(16) . . ? O1 P1 O2 108.92(16) . . ? O4 P1 K2 68.85(14) . 3_466 ? O3 P1 K2 165.78(12) . 3_466 ? O1 P1 K2 81.18(12) . 3_466 ? O2 P1 K2 58.49(11) . 3_466 ? O4 P1 K1 66.19(12) . 2_664 ? O3 P1 K1 80.67(12) . 2_664 ? O1 P1 K1 166.32(13) . 2_664 ? O2 P1 K1 60.47(12) . 2_664 ? K2 P1 K1 85.59(3) 3_466 2_664 ? O4 P1 K2 58.79(14) . 2_664 ? O3 P1 K2 49.86(12) . 2_664 ? O1 P1 K2 124.52(12) . 2_664 ? O2 P1 K2 126.54(11) . 2_664 ? K2 P1 K2 126.94(3) 3_466 2_664 ? K1 P1 K2 66.87(4) 2_664 2_664 ? O4 P1 K1 147.98(14) . 4_645 ? O3 P1 K1 102.48(13) . 4_645 ? O1 P1 K1 46.18(12) . 4_645 ? O2 P1 K1 71.26(12) . 4_645 ? K2 P1 K1 83.29(3) 3_466 4_645 ? K1 P1 K1 128.79(4) 2_664 4_645 ? K2 P1 K1 149.19(3) 2_664 4_645 ? P1 O1 Sc1 133.2(2) . . ? P1 O1 K1 111.04(16) . 4_645 ? Sc1 O1 K1 102.70(11) . 4_645 ? P1 O2 Sc1 165.2(2) . 3 ? P1 O2 K2 94.69(13) . 3_466 ? Sc1 O2 K2 93.99(10) 3 3_466 ? P1 O2 K1 93.32(13) . 2_664 ? Sc1 O2 K1 96.19(12) 3 2_664 ? K2 O2 K1 103.75(9) 3_466 2_664 ? P1 O3 Sc2 151.4(2) . 4_645 ? P1 O3 K2 106.18(14) . 2_664 ? Sc2 O3 K2 100.35(12) 4_645 2_664 ? P1 O4 Sc2 154.5(2) . . ? P1 O4 K2 96.53(16) . 2_664 ? Sc2 O4 K2 92.86(12) . 2_664 ? P1 O4 K2 85.20(15) . 3_466 ? Sc2 O4 K2 89.23(12) . 3_466 ? K2 O4 K2 170.92(11) 2_664 3_466 ? P1 O4 K1 88.40(14) . 2_664 ? Sc2 O4 K1 116.88(12) . 2_664 ? K2 O4 K1 76.70(9) 2_664 2_664 ? K2 O4 K1 94.47(9) 3_466 2_664 ? ########End