 
data_r3 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'B45 K21 O90 Yb8' 
_chemical_formula_weight          4131.87 
 
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'B'  'B'   0.0013   0.0007 
 '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' 
 'O'  'O'   0.0106   0.0060 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Yb'  'Yb'  -0.3850   5.5486 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            trigonal 
_symmetry_space_group_name_H-M    R32 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-y, x-y, z' 
 '-x+y, -x, z' 
 'y, x, -z' 
 '-x, -x+y, -z' 
 'x-y, -y, -z' 
 'x+2/3, y+1/3, z+1/3' 
 '-y+2/3, x-y+1/3, z+1/3' 
 '-x+y+2/3, -x+1/3, z+1/3' 
 'y+2/3, x+1/3, -z+1/3' 
 '-x+2/3, -x+y+1/3, -z+1/3' 
 'x-y+2/3, -y+1/3, -z+1/3' 
 'x+1/3, y+2/3, z+2/3' 
 '-y+1/3, x-y+2/3, z+2/3' 
 '-x+y+1/3, -x+2/3, z+2/3' 
 'y+1/3, x+2/3, -z+2/3' 
 '-x+1/3, -x+y+2/3, -z+2/3' 
 'x-y+1/3, -y+2/3, -z+2/3' 
 
_cell_length_a                    13.2068(19) 
_cell_length_b                    13.2068(19) 
_cell_length_c                    14.760(3) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 120.00 
_cell_volume                      2229.5(6) 
_cell_formula_units_Z             1 
_cell_measurement_temperature     153(2) 
_cell_measurement_reflns_used     3324 
_cell_measurement_theta_min       3.0850
_cell_measurement_theta_max       31.4816 
 
_exptl_crystal_description        'Chunk'
_exptl_crystal_colour             'Colorless'
_exptl_crystal_size_max           0.4450
_exptl_crystal_size_mid           0.3350
_exptl_crystal_size_min           0.3100
_exptl_crystal_density_meas       none
_exptl_crystal_density_diffrn     3.077 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1904 
_exptl_absorpt_coefficient_mu     9.422 
_exptl_absorpt_correction_type    numerical 
_exptl_absorpt_correction_T_min   0.1
_exptl_absorpt_correction_T_max   0.2 
_exptl_absorpt_process_details    'face indexed'
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       153(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'Rotating Anode'
_diffrn_radiation_monochromator    'Graphite Monochromator' 
_diffrn_measurement_device_type   'Rigaku AFC10 diffractometer'
_diffrn_measurement_method        'dtprofit.ref' 
_diffrn_detector_area_resol_mean  28.5714
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             5127 
_diffrn_reflns_av_R_equivalents   0.0337 
_diffrn_reflns_av_sigmaI/netI     0.0453 
_diffrn_reflns_limit_h_min        -16 
_diffrn_reflns_limit_h_max        16 
_diffrn_reflns_limit_k_min        -16 
_diffrn_reflns_limit_k_max        13 
_diffrn_reflns_limit_l_min        -15 
_diffrn_reflns_limit_l_max        18 
_diffrn_reflns_theta_min          3.08 
_diffrn_reflns_theta_max          26.31 
_reflns_number_total              1016 
_reflns_number_gt                 956 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement        'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction         'CrystalClear (Rigaku Inc., 2008)'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material   'Diamond' 
 
_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)+(0.0100P)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      SHELXL 
_refine_ls_extinction_coef        0.00425(11) 
_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    -0.049(14) 
_refine_ls_number_reflns          1016 
_refine_ls_number_parameters      88 
_refine_ls_number_restraints      78 
_refine_ls_R_factor_all           0.0191 
_refine_ls_R_factor_gt            0.0173 
_refine_ls_wR_factor_ref          0.0415 
_refine_ls_wR_factor_gt           0.0412 
_refine_ls_goodness_of_fit_ref    0.953 
_refine_ls_restrained_S_all       0.985 
_refine_ls_shift/su_max           0.006 
_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 
Yb1 Yb 0.6667 0.3333 1.05216(2) 0.00262(12) Uani 1 3 d SU . . 
Yb2 Yb 0.6667 0.3333 0.8333 0.0085(3) Uani 0.677(2) 6 d SPU . . 
K1 K 0.6667 0.79645(12) 0.8333 0.0094(4) Uani 1 2 d SU . . 
K2 K 1.0000 1.0000 1.0000 0.0091(5) Uani 1 6 d SU . . 
K3 K 0.8244(2) 0.6667 0.6667 0.0155(4) Uani 1 2 d SU . . 
B1 B 0.9054(5) 0.7744(4) 0.8597(4) 0.0049(13) Uani 1 1 d U . . 
B2 B 1.0000 0.7515(7) 1.0000 0.0085(15) Uani 1 2 d SU . . 
B3 B 0.8105(5) 0.5847(5) 0.9386(4) 0.0067(13) Uani 1 1 d U . . 
O1 O 0.7243(4) 0.4747(3) 0.9440(2) 0.0067(8) Uani 1 1 d U . . 
O2 O 0.8965(3) 0.8393(3) 0.7951(2) 0.0047(8) Uani 1 1 d U . . 
O3 O 0.8957(3) 0.6342(3) 1.0053(2) 0.0078(8) Uani 1 1 d U . . 
O4 O 0.8139(4) 0.6574(3) 0.8673(2) 0.0109(9) Uani 1 1 d U . . 
O5 O 0.9972(3) 0.8147(3) 0.9197(2) 0.0065(8) Uani 1 1 d U . . 
 
 
_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 
Yb1 O2 2.176(3) 8_655 ? 
Yb1 O2 2.176(3) 7_445 ? 
Yb1 O2 2.176(3) 9_565 ? 
Yb1 O1 2.279(3) 3_665 ? 
Yb1 O1 2.279(3) 2_655 ? 
Yb1 O1 2.279(3) . ? 
Yb1 Yb2 3.2299(7) . ? 
Yb1 K3 3.8912(5) 8_655 ? 
Yb1 K3 3.8912(6) 7_445 ? 
Yb1 K3 3.891(3) 9_565 ? 
Yb1 K2 4.1501(9) 7_445 ? 
Yb1 K1 4.1986(6) 8_655 ? 
Yb2 O1 2.305(3) 17_656 ? 
Yb2 O1 2.305(3) 3_665 ? 
Yb2 O1 2.305(3) . ? 
Yb2 O1 2.305(3) 2_655 ? 
Yb2 O1 2.305(3) 18_556 ? 
Yb2 O1 2.305(3) 16_546 ? 
Yb2 Yb1 3.2300(7) 16_546 ? 
Yb2 K3 4.5388(5) 8_655 ? 
Yb2 K3 4.5388(5) 3_665 ? 
Yb2 K3 4.5388(5) 2_655 ? 
Yb2 K3 4.5388(5) 7_445 ? 
K1 O5 2.755(4) 18_566 ? 
K1 O5 2.755(4) 3_675 ? 
K1 O2 2.852(3) 17_656 ? 
K1 O2 2.852(3) . ? 
K1 O3 2.852(4) 4_557 ? 
K1 O3 2.852(4) 14_654 ? 
K1 O4 3.314(5) . ? 
K1 O4 3.314(5) 17_656 ? 
K1 B1 3.330(6) . ? 
K1 B1 3.330(6) 17_656 ? 
K1 B2 3.3945(13) 14_654 ? 
K1 B2 3.3945(13) 3_675 ? 
K2 O5 2.702(3) 6_677 ? 
K2 O5 2.702(3) 3_675 ? 
K2 O5 2.702(3) . ? 
K2 O5 2.702(3) 5_767 ? 
K2 O5 2.702(3) 2_765 ? 
K2 O5 2.702(3) 4_557 ? 
K2 B2 3.282(9) 2_765 ? 
K2 B2 3.282(9) . ? 
K2 B2 3.282(9) 3_675 ? 
K2 B1 3.317(5) 6_677 ? 
K2 B1 3.317(5) . ? 
K2 B1 3.317(5) 3_675 ? 
K3 O2 2.743(3) 12_566 ? 
K3 O2 2.743(3) . ? 
K3 O3 2.843(5) 15_664 ? 
K3 O3 2.843(5) 16_546 ? 
K3 O4 2.964(3) 12_566 ? 
K3 O4 2.964(3) . ? 
K3 B1 3.124(5) 12_566 ? 
K3 B1 3.124(5) . ? 
K3 O1 3.203(5) 14_654 ? 
K3 O1 3.203(5) 17_656 ? 
K3 B3 3.422(6) 15_664 ? 
K3 B3 3.422(6) 16_546 ? 
B1 O2 1.326(6) . ? 
B1 O5 1.377(6) . ? 
B1 O4 1.412(6) . ? 
B1 K1 3.504(6) 2_765 ? 
B2 O5 1.461(6) 5_767 ? 
B2 O5 1.461(6) . ? 
B2 O3 1.473(6) . ? 
B2 O3 1.473(6) 5_767 ? 
B2 K1 3.3944(12) 2_765 ? 
B2 K1 3.3944(12) 9_565 ? 
B2 K3 3.440(9) 8_655 ? 
B3 O1 1.326(6) . ? 
B3 O3 1.388(7) . ? 
B3 O4 1.410(6) . ? 
B3 K3 3.422(6) 8_655 ? 
B3 K1 3.569(6) 9_565 ? 
O1 K3 3.203(5) 9_565 ? 
O2 Yb1 2.176(3) 13_554 ? 
O3 K3 2.843(5) 8_655 ? 
O3 K1 2.852(4) 9_565 ? 
O5 K1 2.755(4) 2_765 ? 
 
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 Yb1 O2 95.69(11) 8_655 7_445 ? 
O2 Yb1 O2 95.69(11) 8_655 9_565 ? 
O2 Yb1 O2 95.68(11) 7_445 9_565 ? 
O2 Yb1 O1 85.76(12) 8_655 3_665 ? 
O2 Yb1 O1 102.10(14) 7_445 3_665 ? 
O2 Yb1 O1 161.93(13) 9_565 3_665 ? 
O2 Yb1 O1 161.93(13) 8_655 2_655 ? 
O2 Yb1 O1 85.76(13) 7_445 2_655 ? 
O2 Yb1 O1 102.10(14) 9_565 2_655 ? 
O1 Yb1 O1 76.35(11) 3_665 2_655 ? 
O2 Yb1 O1 102.10(14) 8_655 . ? 
O2 Yb1 O1 161.93(13) 7_445 . ? 
O2 Yb1 O1 85.76(12) 9_565 . ? 
O1 Yb1 O1 76.35(11) 3_665 . ? 
O1 Yb1 O1 76.35(11) 2_655 . ? 
O2 Yb1 Yb2 121.13(8) 8_655 . ? 
O2 Yb1 Yb2 121.13(8) 7_445 . ? 
O2 Yb1 Yb2 121.13(8) 9_565 . ? 
O1 Yb1 Yb2 45.53(7) 3_665 . ? 
O1 Yb1 Yb2 45.53(7) 2_655 . ? 
O1 Yb1 Yb2 45.53(7) . . ? 
O2 Yb1 K3 43.17(8) 8_655 8_655 ? 
O2 Yb1 K3 127.96(9) 7_445 8_655 ? 
O2 Yb1 K3 114.91(9) 9_565 8_655 ? 
O1 Yb1 K3 55.38(12) 3_665 8_655 ? 
O1 Yb1 K3 123.67(8) 2_655 8_655 ? 
O1 Yb1 K3 66.29(12) . 8_655 ? 
Yb2 Yb1 K3 78.588(5) . 8_655 ? 
O2 Yb1 K3 114.91(9) 8_655 7_445 ? 
O2 Yb1 K3 43.17(8) 7_445 7_445 ? 
O2 Yb1 K3 127.95(9) 9_565 7_445 ? 
O1 Yb1 K3 66.30(13) 3_665 7_445 ? 
O1 Yb1 K3 55.38(12) 2_655 7_445 ? 
O1 Yb1 K3 123.67(8) . 7_445 ? 
Yb2 Yb1 K3 78.588(5) . 7_445 ? 
K3 Yb1 K3 116.187(3) 8_655 7_445 ? 
O2 Yb1 K3 127.95(9) 8_655 9_565 ? 
O2 Yb1 K3 114.90(9) 7_445 9_565 ? 
O2 Yb1 K3 43.17(8) 9_565 9_565 ? 
O1 Yb1 K3 123.67(7) 3_665 9_565 ? 
O1 Yb1 K3 66.30(12) 2_655 9_565 ? 
O1 Yb1 K3 55.38(12) . 9_565 ? 
Yb2 Yb1 K3 78.589(5) . 9_565 ? 
K3 Yb1 K3 116.185(3) 8_655 9_565 ? 
K3 Yb1 K3 116.185(3) 7_445 9_565 ? 
O2 Yb1 K2 58.87(8) 8_655 7_445 ? 
O2 Yb1 K2 58.87(8) 7_445 7_445 ? 
O2 Yb1 K2 58.87(8) 9_565 7_445 ? 
O1 Yb1 K2 134.47(7) 3_665 7_445 ? 
O1 Yb1 K2 134.47(7) 2_655 7_445 ? 
O1 Yb1 K2 134.47(7) . 7_445 ? 
Yb2 Yb1 K2 180.0 . 7_445 ? 
K3 Yb1 K2 101.412(5) 8_655 7_445 ? 
K3 Yb1 K2 101.412(5) 7_445 7_445 ? 
K3 Yb1 K2 101.411(5) 9_565 7_445 ? 
O2 Yb1 K1 38.87(8) 8_655 8_655 ? 
O2 Yb1 K1 67.17(8) 7_445 8_655 ? 
O2 Yb1 K1 122.84(8) 9_565 8_655 ? 
O1 Yb1 K1 68.21(7) 3_665 8_655 ? 
O1 Yb1 K1 128.33(12) 2_655 8_655 ? 
O1 Yb1 K1 126.65(12) . 8_655 ? 
Yb2 Yb1 K1 113.737(7) . 8_655 ? 
K3 Yb1 K1 60.94(4) 8_655 8_655 ? 
K3 Yb1 K1 76.05(4) 7_445 8_655 ? 
K3 Yb1 K1 164.96(3) 9_565 8_655 ? 
K2 Yb1 K1 66.264(7) 7_445 8_655 ? 
O1 Yb2 O1 171.4(2) 17_656 3_665 ? 
O1 Yb2 O1 99.67(19) 17_656 . ? 
O1 Yb2 O1 75.32(11) 3_665 . ? 
O1 Yb2 O1 110.50(19) 17_656 2_655 ? 
O1 Yb2 O1 75.32(11) 3_665 2_655 ? 
O1 Yb2 O1 75.32(11) . 2_655 ? 
O1 Yb2 O1 75.32(11) 17_656 18_556 ? 
O1 Yb2 O1 110.50(19) 3_665 18_556 ? 
O1 Yb2 O1 171.4(2) . 18_556 ? 
O1 Yb2 O1 99.67(19) 2_655 18_556 ? 
O1 Yb2 O1 75.32(11) 17_656 16_546 ? 
O1 Yb2 O1 99.67(19) 3_665 16_546 ? 
O1 Yb2 O1 110.5(2) . 16_546 ? 
O1 Yb2 O1 171.4(2) 2_655 16_546 ? 
O1 Yb2 O1 75.32(11) 18_556 16_546 ? 
O1 Yb2 Yb1 135.13(7) 17_656 . ? 
O1 Yb2 Yb1 44.87(7) 3_665 . ? 
O1 Yb2 Yb1 44.87(7) . . ? 
O1 Yb2 Yb1 44.87(7) 2_655 . ? 
O1 Yb2 Yb1 135.13(7) 18_556 . ? 
O1 Yb2 Yb1 135.13(7) 16_546 . ? 
O1 Yb2 Yb1 44.87(7) 17_656 16_546 ? 
O1 Yb2 Yb1 135.13(7) 3_665 16_546 ? 
O1 Yb2 Yb1 135.13(7) . 16_546 ? 
O1 Yb2 Yb1 135.13(7) 2_655 16_546 ? 
O1 Yb2 Yb1 44.87(7) 18_556 16_546 ? 
O1 Yb2 Yb1 44.87(7) 16_546 16_546 ? 
Yb1 Yb2 Yb1 180.0 . 16_546 ? 
O1 Yb2 K3 129.87(13) 17_656 8_655 ? 
O1 Yb2 K3 41.57(13) 3_665 8_655 ? 
O1 Yb2 K3 52.60(12) . 8_655 ? 
O1 Yb2 K3 101.72(7) 2_655 8_655 ? 
O1 Yb2 K3 135.92(13) 18_556 8_655 ? 
O1 Yb2 K3 78.05(7) 16_546 8_655 ? 
Yb1 Yb2 K3 57.180(7) . 8_655 ? 
Yb1 Yb2 K3 122.820(6) 16_546 8_655 ? 
O1 Yb2 K3 101.72(7) 17_656 3_665 ? 
O1 Yb2 K3 78.05(7) 3_665 3_665 ? 
O1 Yb2 K3 135.92(13) . 3_665 ? 
O1 Yb2 K3 129.87(13) 2_655 3_665 ? 
O1 Yb2 K3 52.60(12) 18_556 3_665 ? 
O1 Yb2 K3 41.57(12) 16_546 3_665 ? 
Yb1 Yb2 K3 122.820(6) . 3_665 ? 
Yb1 Yb2 K3 57.179(6) 16_546 3_665 ? 
K3 Yb2 K3 84.46(5) 8_655 3_665 ? 
O1 Yb2 K3 52.60(13) 17_656 2_655 ? 
O1 Yb2 K3 135.92(13) 3_665 2_655 ? 
O1 Yb2 K3 129.87(13) . 2_655 ? 
O1 Yb2 K3 78.05(7) 2_655 2_655 ? 
O1 Yb2 K3 41.57(12) 18_556 2_655 ? 
O1 Yb2 K3 101.72(7) 16_546 2_655 ? 
Yb1 Yb2 K3 122.820(6) . 2_655 ? 
Yb1 Yb2 K3 57.181(6) 16_546 2_655 ? 
K3 Yb2 K3 177.01(7) 8_655 2_655 ? 
K3 Yb2 K3 93.403(9) 3_665 2_655 ? 
O1 Yb2 K3 135.92(13) 17_656 7_445 ? 
O1 Yb2 K3 52.60(13) 3_665 7_445 ? 
O1 Yb2 K3 101.72(7) . 7_445 ? 
O1 Yb2 K3 41.57(12) 2_655 7_445 ? 
O1 Yb2 K3 78.05(7) 18_556 7_445 ? 
O1 Yb2 K3 129.87(13) 16_546 7_445 ? 
Yb1 Yb2 K3 57.180(7) . 7_445 ? 
Yb1 Yb2 K3 122.820(7) 16_546 7_445 ? 
K3 Yb2 K3 93.403(9) 8_655 7_445 ? 
K3 Yb2 K3 88.81(5) 3_665 7_445 ? 
K3 Yb2 K3 84.46(5) 2_655 7_445 ? 
O5 K1 O5 102.27(16) 18_566 3_675 ? 
O5 K1 O2 73.97(9) 18_566 17_656 ? 
O5 K1 O2 134.01(10) 3_675 17_656 ? 
O5 K1 O2 134.01(10) 18_566 . ? 
O5 K1 O2 73.97(9) 3_675 . ? 
O2 K1 O2 141.03(14) 17_656 . ? 
O5 K1 O3 88.25(11) 18_566 4_557 ? 
O5 K1 O3 50.18(10) 3_675 4_557 ? 
O2 K1 O3 83.86(9) 17_656 4_557 ? 
O2 K1 O3 117.63(9) . 4_557 ? 
O5 K1 O3 50.18(10) 18_566 14_654 ? 
O5 K1 O3 88.25(11) 3_675 14_654 ? 
O2 K1 O3 117.63(9) 17_656 14_654 ? 
O2 K1 O3 83.86(9) . 14_654 ? 
O3 K1 O3 115.36(15) 4_557 14_654 ? 
O5 K1 O4 156.96(10) 18_566 . ? 
O5 K1 O4 98.26(9) 3_675 . ? 
O2 K1 O4 98.96(10) 17_656 . ? 
O2 K1 O4 43.83(9) . . ? 
O3 K1 O4 113.15(9) 4_557 . ? 
O3 K1 O4 120.89(10) 14_654 . ? 
O5 K1 O4 98.26(9) 18_566 17_656 ? 
O5 K1 O4 156.96(10) 3_675 17_656 ? 
O2 K1 O4 43.83(9) 17_656 17_656 ? 
O2 K1 O4 98.96(10) . 17_656 ? 
O3 K1 O4 120.89(10) 4_557 17_656 ? 
O3 K1 O4 113.15(9) 14_654 17_656 ? 
O4 K1 O4 64.05(12) . 17_656 ? 
O5 K1 B1 156.80(12) 18_566 . ? 
O5 K1 B1 77.55(11) 3_675 . ? 
O2 K1 B1 123.06(12) 17_656 . ? 
O2 K1 B1 23.15(11) . . ? 
O3 K1 B1 108.00(11) 4_557 . ? 
O3 K1 B1 106.88(11) 14_654 . ? 
O4 K1 B1 24.54(11) . . ? 
O4 K1 B1 87.65(11) 17_656 . ? 
O5 K1 B1 77.55(11) 18_566 17_656 ? 
O5 K1 B1 156.80(12) 3_675 17_656 ? 
O2 K1 B1 23.15(11) 17_656 17_656 ? 
O2 K1 B1 123.06(12) . 17_656 ? 
O3 K1 B1 106.89(11) 4_557 17_656 ? 
O3 K1 B1 108.00(12) 14_654 17_656 ? 
O4 K1 B1 87.65(11) . 17_656 ? 
O4 K1 B1 24.54(11) 17_656 17_656 ? 
B1 K1 B1 111.80(18) . 17_656 ? 
O5 K1 B2 24.80(12) 18_566 14_654 ? 
O5 K1 B2 96.95(15) 3_675 14_654 ? 
O2 K1 B2 95.12(16) 17_656 14_654 ? 
O2 K1 B2 109.21(12) . 14_654 ? 
O3 K1 B2 103.46(9) 4_557 14_654 ? 
O3 K1 B2 25.42(13) 14_654 14_654 ? 
O4 K1 B2 141.85(7) . 14_654 ? 
O4 K1 B2 106.06(14) 17_656 14_654 ? 
B1 K1 B2 132.09(13) . 14_654 ? 
B1 K1 B2 91.87(17) 17_656 14_654 ? 
O5 K1 B2 96.95(15) 18_566 3_675 ? 
O5 K1 B2 24.80(12) 3_675 3_675 ? 
O2 K1 B2 109.21(12) 17_656 3_675 ? 
O2 K1 B2 95.12(16) . 3_675 ? 
O3 K1 B2 25.42(13) 4_557 3_675 ? 
O3 K1 B2 103.46(9) 14_654 3_675 ? 
O4 K1 B2 106.06(14) . 3_675 ? 
O4 K1 B2 141.85(7) 17_656 3_675 ? 
B1 K1 B2 91.87(17) . 3_675 ? 
B1 K1 B2 132.10(13) 17_656 3_675 ? 
B2 K1 B2 102.35(18) 14_654 3_675 ? 
O5 K2 O5 125.30(16) 6_677 3_675 ? 
O5 K2 O5 127.89(16) 6_677 . ? 
O5 K2 O5 102.21(9) 3_675 . ? 
O5 K2 O5 102.21(9) 6_677 5_767 ? 
O5 K2 O5 127.89(16) 3_675 5_767 ? 
O5 K2 O5 52.04(15) . 5_767 ? 
O5 K2 O5 52.04(15) 6_677 2_765 ? 
O5 K2 O5 102.21(9) 3_675 2_765 ? 
O5 K2 O5 102.21(9) . 2_765 ? 
O5 K2 O5 125.30(16) 5_767 2_765 ? 
O5 K2 O5 102.21(9) 6_677 4_557 ? 
O5 K2 O5 52.04(15) 3_675 4_557 ? 
O5 K2 O5 125.30(16) . 4_557 ? 
O5 K2 O5 102.21(9) 5_767 4_557 ? 
O5 K2 O5 127.89(15) 2_765 4_557 ? 
O5 K2 B2 26.02(7) 6_677 2_765 ? 
O5 K2 B2 116.05(8) 3_675 2_765 ? 
O5 K2 B2 117.35(8) . 2_765 ? 
O5 K2 B2 116.05(8) 5_767 2_765 ? 
O5 K2 B2 26.02(7) 2_765 2_765 ? 
O5 K2 B2 117.35(8) 4_557 2_765 ? 
O5 K2 B2 117.35(8) 6_677 . ? 
O5 K2 B2 117.35(8) 3_675 . ? 
O5 K2 B2 26.02(7) . . ? 
O5 K2 B2 26.02(7) 5_767 . ? 
O5 K2 B2 116.05(8) 2_765 . ? 
O5 K2 B2 116.05(8) 4_557 . ? 
B2 K2 B2 120.000(2) 2_765 . ? 
O5 K2 B2 116.05(8) 6_677 3_675 ? 
O5 K2 B2 26.02(7) 3_675 3_675 ? 
O5 K2 B2 116.05(8) . 3_675 ? 
O5 K2 B2 117.35(8) 5_767 3_675 ? 
O5 K2 B2 117.35(8) 2_765 3_675 ? 
O5 K2 B2 26.02(7) 4_557 3_675 ? 
B2 K2 B2 120.000(1) 2_765 3_675 ? 
B2 K2 B2 120.000(4) . 3_675 ? 
O5 K2 B1 23.74(12) 6_677 6_677 ? 
O5 K2 B1 109.26(12) 3_675 6_677 ? 
O5 K2 B1 148.41(13) . 6_677 ? 
O5 K2 B1 107.08(12) 5_767 6_677 ? 
O5 K2 B1 68.89(12) 2_765 6_677 ? 
O5 K2 B1 78.47(12) 4_557 6_677 ? 
B2 K2 B1 44.79(9) 2_765 6_677 ? 
B2 K2 B1 129.60(10) . 6_677 ? 
B2 K2 B1 94.15(10) 3_675 6_677 ? 
O5 K2 B1 148.41(13) 6_677 . ? 
O5 K2 B1 78.47(12) 3_675 . ? 
O5 K2 B1 23.74(12) . . ? 
O5 K2 B1 68.89(12) 5_767 . ? 
O5 K2 B1 107.08(12) 2_765 . ? 
O5 K2 B1 109.26(13) 4_557 . ? 
B2 K2 B1 129.60(10) 2_765 . ? 
B2 K2 B1 44.79(9) . . ? 
B2 K2 B1 94.15(10) 3_675 . ? 
B1 K2 B1 171.7(2) 6_677 . ? 
O5 K2 B1 109.26(12) 6_677 3_675 ? 
O5 K2 B1 23.74(12) 3_675 3_675 ? 
O5 K2 B1 107.08(12) . 3_675 ? 
O5 K2 B1 148.41(13) 5_767 3_675 ? 
O5 K2 B1 78.47(12) 2_765 3_675 ? 
O5 K2 B1 68.89(12) 4_557 3_675 ? 
B2 K2 B1 94.15(10) 2_765 3_675 ? 
B2 K2 B1 129.60(10) . 3_675 ? 
B2 K2 B1 44.79(9) 3_675 3_675 ? 
B1 K2 B1 100.81(19) 6_677 3_675 ? 
B1 K2 B1 85.13(13) . 3_675 ? 
O2 K3 O2 172.17(18) 12_566 . ? 
O2 K3 O3 112.52(12) 12_566 15_664 ? 
O2 K3 O3 74.98(10) . 15_664 ? 
O2 K3 O3 74.98(10) 12_566 16_546 ? 
O2 K3 O3 112.52(12) . 16_546 ? 
O3 K3 O3 49.73(14) 15_664 16_546 ? 
O2 K3 O4 48.24(9) 12_566 12_566 ? 
O2 K3 O4 131.49(9) . 12_566 ? 
O3 K3 O4 92.05(11) 15_664 12_566 ? 
O3 K3 O4 90.62(11) 16_546 12_566 ? 
O2 K3 O4 131.49(9) 12_566 . ? 
O2 K3 O4 48.24(9) . . ? 
O3 K3 O4 90.62(11) 15_664 . ? 
O3 K3 O4 92.05(11) 16_546 . ? 
O4 K3 O4 177.05(19) 12_566 . ? 
O2 K3 B1 25.05(11) 12_566 12_566 ? 
O2 K3 B1 157.16(11) . 12_566 ? 
O3 K3 B1 94.97(13) 15_664 12_566 ? 
O3 K3 B1 72.86(13) 16_546 12_566 ? 
O4 K3 B1 26.66(11) 12_566 12_566 ? 
O4 K3 B1 154.10(12) . 12_566 ? 
O2 K3 B1 157.16(11) 12_566 . ? 
O2 K3 B1 25.05(11) . . ? 
O3 K3 B1 72.86(13) 15_664 . ? 
O3 K3 B1 94.97(13) 16_546 . ? 
O4 K3 B1 154.10(12) 12_566 . ? 
O4 K3 B1 26.66(11) . . ? 
B1 K3 B1 166.8(2) 12_566 . ? 
O2 K3 O1 115.96(10) 12_566 14_654 ? 
O2 K3 O1 60.74(9) . 14_654 ? 
O3 K3 O1 88.39(9) 15_664 14_654 ? 
O3 K3 O1 134.87(11) 16_546 14_654 ? 
O4 K3 O1 72.58(9) 12_566 14_654 ? 
O4 K3 O1 106.27(8) . 14_654 ? 
B1 K3 O1 99.16(11) 12_566 14_654 ? 
B1 K3 O1 85.78(11) . 14_654 ? 
O2 K3 O1 60.74(9) 12_566 17_656 ? 
O2 K3 O1 115.97(10) . 17_656 ? 
O3 K3 O1 134.87(11) 15_664 17_656 ? 
O3 K3 O1 88.38(9) 16_546 17_656 ? 
O4 K3 O1 106.27(9) 12_566 17_656 ? 
O4 K3 O1 72.58(9) . 17_656 ? 
B1 K3 O1 85.78(11) 12_566 17_656 ? 
B1 K3 O1 99.16(12) . 17_656 ? 
O1 K3 O1 136.17(14) 14_654 17_656 ? 
O2 K3 B3 108.82(12) 12_566 15_664 ? 
O2 K3 B3 77.10(12) . 15_664 ? 
O3 K3 B3 23.34(12) 15_664 15_664 ? 
O3 K3 B3 66.34(12) 16_546 15_664 ? 
O4 K3 B3 74.41(12) 12_566 15_664 ? 
O4 K3 B3 107.82(13) . 15_664 ? 
B1 K3 B3 85.70(14) 12_566 15_664 ? 
B1 K3 B3 84.74(14) . 15_664 ? 
O1 K3 B3 68.82(11) 14_654 15_664 ? 
O1 K3 B3 154.71(12) 17_656 15_664 ? 
O2 K3 B3 77.10(12) 12_566 16_546 ? 
O2 K3 B3 108.82(12) . 16_546 ? 
O3 K3 B3 66.34(12) 15_664 16_546 ? 
O3 K3 B3 23.34(12) 16_546 16_546 ? 
O4 K3 B3 107.82(13) 12_566 16_546 ? 
O4 K3 B3 74.42(12) . 16_546 ? 
B1 K3 B3 84.74(14) 12_566 16_546 ? 
B1 K3 B3 85.70(14) . 16_546 ? 
O1 K3 B3 154.71(12) 14_654 16_546 ? 
O1 K3 B3 68.82(11) 17_656 16_546 ? 
B3 K3 B3 86.71(19) 15_664 16_546 ? 
O2 B1 O5 124.0(4) . . ? 
O2 B1 O4 117.5(4) . . ? 
O5 B1 O4 118.6(4) . . ? 
O2 B1 K3 61.2(2) . . ? 
O5 B1 K3 142.9(4) . . ? 
O4 B1 K3 70.3(2) . . ? 
O2 B1 K2 89.1(3) . . ? 
O5 B1 K2 52.2(2) . . ? 
O4 B1 K2 131.7(3) . . ? 
K3 B1 K2 150.21(18) . . ? 
O2 B1 K1 57.7(2) . . ? 
O5 B1 K1 137.0(3) . . ? 
O4 B1 K1 77.1(3) . . ? 
K3 B1 K1 79.04(13) . . ? 
K2 B1 K1 86.70(13) . . ? 
O2 B1 K1 97.7(3) . 2_765 ? 
O5 B1 K1 47.0(2) . 2_765 ? 
O4 B1 K1 126.5(3) . 2_765 ? 
K3 B1 K1 97.49(15) . 2_765 ? 
K2 B1 K1 83.93(12) . 2_765 ? 
K1 B1 K1 153.85(17) . 2_765 ? 
O5 B2 O5 108.5(6) 5_767 . ? 
O5 B2 O3 108.4(2) 5_767 . ? 
O5 B2 O3 111.5(2) . . ? 
O5 B2 O3 111.5(2) 5_767 5_767 ? 
O5 B2 O3 108.4(2) . 5_767 ? 
O3 B2 O3 108.6(6) . 5_767 ? 
O5 B2 K2 54.2(3) 5_767 . ? 
O5 B2 K2 54.2(3) . . ? 
O3 B2 K2 125.7(3) . . ? 
O3 B2 K2 125.7(3) 5_767 . ? 
O5 B2 K1 122.3(3) 5_767 2_765 ? 
O5 B2 K1 52.29(14) . 2_765 ? 
O3 B2 K1 129.3(3) . 2_765 ? 
O3 B2 K1 56.24(15) 5_767 2_765 ? 
K2 B2 K1 86.22(15) . 2_765 ? 
O5 B2 K1 52.29(14) 5_767 9_565 ? 
O5 B2 K1 122.3(3) . 9_565 ? 
O3 B2 K1 56.24(15) . 9_565 ? 
O3 B2 K1 129.3(3) 5_767 9_565 ? 
K2 B2 K1 86.22(15) . 9_565 ? 
K1 B2 K1 172.4(3) 2_765 9_565 ? 
O5 B2 K3 125.8(3) 5_767 8_655 ? 
O5 B2 K3 125.8(3) . 8_655 ? 
O3 B2 K3 54.3(3) . 8_655 ? 
O3 B2 K3 54.3(3) 5_767 8_655 ? 
K2 B2 K3 180.0 . 8_655 ? 
K1 B2 K3 93.78(15) 2_765 8_655 ? 
K1 B2 K3 93.78(15) 9_565 8_655 ? 
O1 B3 O3 121.5(5) . . ? 
O1 B3 O4 120.5(5) . . ? 
O3 B3 O4 117.8(4) . . ? 
O1 B3 K3 88.3(3) . 8_655 ? 
O3 B3 K3 54.2(3) . 8_655 ? 
O4 B3 K3 131.6(4) . 8_655 ? 
O1 B3 K1 97.4(3) . 9_565 ? 
O3 B3 K1 48.8(2) . 9_565 ? 
O4 B3 K1 119.1(3) . 9_565 ? 
K3 B3 K1 91.04(13) 8_655 9_565 ? 
B3 O1 Yb1 133.8(3) . . ? 
B3 O1 Yb2 126.8(3) . . ? 
Yb1 O1 Yb2 89.60(10) . . ? 
B3 O1 K3 101.4(3) . 9_565 ? 
Yb1 O1 K3 88.78(13) . 9_565 ? 
Yb2 O1 K3 109.91(16) . 9_565 ? 
B1 O2 Yb1 141.9(3) . 13_554 ? 
B1 O2 K3 93.8(3) . . ? 
Yb1 O2 K3 103.95(11) 13_554 . ? 
B1 O2 K1 99.1(3) . . ? 
Yb1 O2 K1 112.53(13) 13_554 . ? 
K3 O2 K1 94.53(12) . . ? 
B3 O3 B2 124.7(4) . . ? 
B3 O3 K3 102.4(3) . 8_655 ? 
B2 O3 K3 100.9(3) . 8_655 ? 
B3 O3 K1 109.8(3) . 9_565 ? 
B2 O3 K1 98.3(2) . 9_565 ? 
K3 O3 K1 122.33(12) 8_655 9_565 ? 
B3 O4 B1 121.6(4) . . ? 
B3 O4 K3 139.4(3) . . ? 
B1 O4 K3 83.0(3) . . ? 
B3 O4 K1 131.5(3) . . ? 
B1 O4 K1 78.4(3) . . ? 
K3 O4 K1 81.60(9) . . ? 
B1 O5 B2 124.8(4) . . ? 
B1 O5 K2 104.0(3) . . ? 
B2 O5 K2 99.7(3) . . ? 
B1 O5 K1 111.6(3) . 2_765 ? 
B2 O5 K1 102.9(2) . 2_765 ? 
K2 O5 K1 113.48(13) . 2_765 ? 
 
_diffrn_measured_fraction_theta_max    0.995 
_diffrn_reflns_theta_full              26.31 
_diffrn_measured_fraction_theta_full   0.995 
_refine_diff_density_max    1.123 
_refine_diff_density_min   -0.570 
_refine_diff_density_rms    0.109 
