data_K4Zn4(V2O7)2(IO3)4(H2O)
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          '2(I2 O13 V2 Zn2), 2(O0.50)2H, 4(K)'
_chemical_formula_sum 
 'H2 I4 K4 O27 V4 Zn4' 
_chemical_formula_weight          1563.26 
 
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'O'  'O'   0.0106   0.0060 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'K'  'K'   0.2009   0.2494 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'V'  'V'   0.3005   0.5294 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Zn'  'Zn'   0.2839   1.4301 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'I'  'I'  -0.4742   1.8119 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'H'  'H'   0.0000   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            hexagonal
_symmetry_space_group_name_H-M    P6(3)/m 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-y, x-y, z' 
 '-x+y, -x, z' 
 '-x, -y, z+1/2' 
 'y, -x+y, z+1/2' 
 'x-y, x, z+1/2' 
 '-x, -y, -z' 
 'y, -x+y, -z' 
 'x-y, x, -z' 
 'x, y, -z-1/2' 
 '-y, x-y, -z-1/2' 
 '-x+y, -x, -z-1/2' 
 
_cell_length_a                    5.5732(6) 
_cell_length_b                    5.5732(6) 
_cell_length_c                    25.339(4) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 120.00 
_cell_volume                      681.61(16) 
_cell_formula_units_Z             1 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used           727
_cell_measurement_theta_min             2.4112
_cell_measurement_theta_max             27.4333 
 
_exptl_crystal_description        'hexagonal plate' 
_exptl_crystal_colour             orange 
_exptl_crystal_size_max           0.13 
_exptl_crystal_size_mid           0.12 
_exptl_crystal_size_min           0.03 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     3.808 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              718 
_exptl_absorpt_coefficient_mu     10.011 
_exptl_absorpt_correction_type    'Multi-scan'
_exptl_absorpt_correction_T_min   0.4844 
_exptl_absorpt_correction_T_max   1.0000 
_exptl_absorpt_process_details     'Higashi'  
 
_exptl_special_details 
; 
 Higashi, T. . Program for Absorption Correction.

  Rigaku Corporation, Tokyo, Japan.
 
; 
 
_diffrn_ambient_temperature       293(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   ? 
_diffrn_measurement_method        'CCD_Profile_fitting'  
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             5152 
_diffrn_reflns_av_R_equivalents   0.0632 
_diffrn_reflns_av_sigmaI/netI     0.0293 
_diffrn_reflns_limit_h_min        -7 
_diffrn_reflns_limit_h_max        7 
_diffrn_reflns_limit_k_min        -7 
_diffrn_reflns_limit_k_max        7 
_diffrn_reflns_limit_l_min        -31 
_diffrn_reflns_limit_l_max        32 
_diffrn_reflns_theta_min          4.22 
_diffrn_reflns_theta_max          27.50 
_reflns_number_total              537 
_reflns_number_gt                 499 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_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)+(0.0198P)²+4.2645P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    none 
_refine_ls_hydrogen_treatment     none
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          537 
_refine_ls_number_parameters      36 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0387 
_refine_ls_R_factor_gt            0.0347 
_refine_ls_wR_factor_ref          0.0717 
_refine_ls_wR_factor_gt           0.0700 
_refine_ls_goodness_of_fit_ref    1.230 
_refine_ls_restrained_S_all       1.230 
_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 
K1 K 0.6667 0.3333 0.2500 0.0435(10) Uani 1 6 d S . . 
K2 K 1.0000 0.0000 0.5000 0.0303(7) Uani 1 6 d S . . 
Zn1 Zn 0.6667 0.3333 0.39287(4) 0.0159(3) Uani 1 3 d S . . 
V1 V 1.0000 1.0000 0.32055(6) 0.0113(3) Uani 1 3 d S . . 
I1 I 0.3333 0.6667 0.40108(2) 0.01350(19) Uani 1 3 d S . . 
O1 O 0.4178(8) 0.4350(8) 0.43552(15) 0.0187(8) Uani 1 1 d . . . 
O2 O 1.0000 1.0000 0.2500 0.039(3) Uani 1 6 d S . . 
O3 O 0.7616(9) 0.6822(8) 0.34161(15) 0.0211(9) Uani 1 1 d . . . 
O1W O 0.3333 0.6667 0.2500 0.039(6) Uani 0.50 6 d SP . . 
 
 
_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 O3 2.902(4) 11_656 ? 
K1 O3 2.902(4) 3_665 ? 
K1 O3 2.902(4) 12_666 ? 
K1 O3 2.902(4) . ? 
K1 O3 2.902(4) 2_655 ? 
K1 O3 2.902(4) 10_556 ? 
K1 O1W 3.2177(3) 1_655 ? 
K1 O1W 3.2177(3) 1_545 ? 
K1 O2 3.2177(3) 1_545 ? 
K1 O2 3.2177(3) . ? 
K1 O2 3.2177(3) 1_445 ? 
K1 O1W 3.2177(3) . ? 
K2 O1 2.885(4) 3_655 ? 
K2 O1 2.885(4) 8_656 ? 
K2 O1 2.885(4) 2_655 ? 
K2 O1 2.885(4) 9_656 ? 
K2 O1 2.885(4) 7_656 ? 
K2 O1 2.885(4) 1_655 ? 
K2 I1 4.0787(5) 1_545 ? 
K2 I1 4.0787(5) 7_766 ? 
K2 I1 4.0787(5) 7_666 ? 
K2 I1 4.0787(5) 1_645 ? 
K2 I1 4.0787(5) 7_656 ? 
K2 I1 4.0787(5) 1_655 ? 
Zn1 O1 2.049(4) 3_665 ? 
Zn1 O1 2.049(4) 2_655 ? 
Zn1 O1 2.049(4) . ? 
Zn1 O3 2.172(4) 2_655 ? 
Zn1 O3 2.172(4) 3_665 ? 
Zn1 O3 2.172(4) . ? 
V1 O3 1.683(4) 2_765 ? 
V1 O3 1.683(4) 3_675 ? 
V1 O3 1.683(4) . ? 
V1 O2 1.7877(15) . ? 
V1 K1 3.6809(8) 1_565 ? 
V1 K1 3.6809(8) 1_665 ? 
I1 O1 1.805(4) 2_665 ? 
I1 O1 1.805(4) 3_565 ? 
I1 O1 1.805(4) . ? 
I1 K2 4.0787(5) 1_565 ? 
I1 K2 4.0787(5) 1_465 ? 
I1 K2 4.0787(5) 1_455 ? 
O1 K2 2.885(4) 1_455 ? 
O2 V1 1.7877(15) 10_556 ? 
O2 K1 3.2177(3) 1_565 ? 
O2 K1 3.2177(4) 1_665 ? 
O1W K1 3.2177(4) 1_565 ? 
O1W K1 3.2177(3) 1_455 ? 
 
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 
O3 K1 O3 145.09(6) 11_656 3_665 ? 
O3 K1 O3 62.61(12) 11_656 12_666 ? 
O3 K1 O3 106.26(15) 3_665 12_666 ? 
O3 K1 O3 145.09(6) 11_656 . ? 
O3 K1 O3 62.61(12) 3_665 . ? 
O3 K1 O3 145.09(6) 12_666 . ? 
O3 K1 O3 106.26(15) 11_656 2_655 ? 
O3 K1 O3 62.61(12) 3_665 2_655 ? 
O3 K1 O3 145.09(6) 12_666 2_655 ? 
O3 K1 O3 62.61(12) . 2_655 ? 
O3 K1 O3 62.61(12) 11_656 10_556 ? 
O3 K1 O3 145.09(7) 3_665 10_556 ? 
O3 K1 O3 62.61(12) 12_666 10_556 ? 
O3 K1 O3 106.26(15) . 10_556 ? 
O3 K1 O3 145.09(6) 2_655 10_556 ? 
O3 K1 O1W 125.47(8) 11_656 1_655 ? 
O3 K1 O1W 65.02(9) 3_665 1_655 ? 
O3 K1 O1W 65.02(9) 12_666 1_655 ? 
O3 K1 O1W 80.91(9) . 1_655 ? 
O3 K1 O1W 125.47(8) 2_655 1_655 ? 
O3 K1 O1W 80.91(9) 10_556 1_655 ? 
O3 K1 O1W 65.02(8) 11_656 1_545 ? 
O3 K1 O1W 80.91(9) 3_665 1_545 ? 
O3 K1 O1W 80.91(9) 12_666 1_545 ? 
O3 K1 O1W 125.47(8) . 1_545 ? 
O3 K1 O1W 65.02(8) 2_655 1_545 ? 
O3 K1 O1W 125.47(8) 10_556 1_545 ? 
O1W K1 O1W 120.0 1_655 1_545 ? 
O3 K1 O2 99.09(9) 11_656 1_545 ? 
O3 K1 O2 54.53(8) 3_665 1_545 ? 
O3 K1 O2 54.53(8) 12_666 1_545 ? 
O3 K1 O2 114.98(8) . 1_545 ? 
O3 K1 O2 99.09(9) 2_655 1_545 ? 
O3 K1 O2 114.98(8) 10_556 1_545 ? 
O1W K1 O2 60.0 1_655 1_545 ? 
O1W K1 O2 60.0 1_545 1_545 ? 
O3 K1 O2 114.98(8) 11_656 . ? 
O3 K1 O2 99.09(9) 3_665 . ? 
O3 K1 O2 99.09(9) 12_666 . ? 
O3 K1 O2 54.53(8) . . ? 
O3 K1 O2 114.98(8) 2_655 . ? 
O3 K1 O2 54.53(8) 10_556 . ? 
O1W K1 O2 60.0 1_655 . ? 
O1W K1 O2 180.0 1_545 . ? 
O2 K1 O2 120.0 1_545 . ? 
O3 K1 O2 54.53(8) 11_656 1_445 ? 
O3 K1 O2 114.98(9) 3_665 1_445 ? 
O3 K1 O2 114.98(9) 12_666 1_445 ? 
O3 K1 O2 99.09(9) . 1_445 ? 
O3 K1 O2 54.53(8) 2_655 1_445 ? 
O3 K1 O2 99.09(9) 10_556 1_445 ? 
O1W K1 O2 180.0 1_655 1_445 ? 
O1W K1 O2 60.0 1_545 1_445 ? 
O2 K1 O2 120.0 1_545 1_445 ? 
O2 K1 O2 120.0 . 1_445 ? 
O3 K1 O1W 80.91(9) 11_656 . ? 
O3 K1 O1W 125.47(8) 3_665 . ? 
O3 K1 O1W 125.47(8) 12_666 . ? 
O3 K1 O1W 65.02(8) . . ? 
O3 K1 O1W 80.91(9) 2_655 . ? 
O3 K1 O1W 65.02(8) 10_556 . ? 
O1W K1 O1W 120.0 1_655 . ? 
O1W K1 O1W 120.0 1_545 . ? 
O2 K1 O1W 180.0 1_545 . ? 
O2 K1 O1W 60.0 . . ? 
O2 K1 O1W 60.0 1_445 . ? 
O1 K2 O1 88.91(11) 3_655 8_656 ? 
O1 K2 O1 91.09(11) 3_655 2_655 ? 
O1 K2 O1 180.000(1) 8_656 2_655 ? 
O1 K2 O1 180.000(2) 3_655 9_656 ? 
O1 K2 O1 91.09(11) 8_656 9_656 ? 
O1 K2 O1 88.91(11) 2_655 9_656 ? 
O1 K2 O1 88.91(11) 3_655 7_656 ? 
O1 K2 O1 91.09(11) 8_656 7_656 ? 
O1 K2 O1 88.91(11) 2_655 7_656 ? 
O1 K2 O1 91.09(11) 9_656 7_656 ? 
O1 K2 O1 91.09(11) 3_655 1_655 ? 
O1 K2 O1 88.91(11) 8_656 1_655 ? 
O1 K2 O1 91.09(11) 2_655 1_655 ? 
O1 K2 O1 88.91(11) 9_656 1_655 ? 
O1 K2 O1 180.000(1) 7_656 1_655 ? 
O1 K2 I1 71.01(8) 3_655 1_545 ? 
O1 K2 I1 157.23(8) 8_656 1_545 ? 
O1 K2 I1 22.77(8) 2_655 1_545 ? 
O1 K2 I1 108.99(8) 9_656 1_545 ? 
O1 K2 I1 78.26(8) 7_656 1_545 ? 
O1 K2 I1 101.74(8) 1_655 1_545 ? 
O1 K2 I1 108.99(8) 3_655 7_766 ? 
O1 K2 I1 22.77(8) 8_656 7_766 ? 
O1 K2 I1 157.23(8) 2_655 7_766 ? 
O1 K2 I1 71.01(8) 9_656 7_766 ? 
O1 K2 I1 101.74(8) 7_656 7_766 ? 
O1 K2 I1 78.26(8) 1_655 7_766 ? 
I1 K2 I1 180.0 1_545 7_766 ? 
O1 K2 I1 157.23(8) 3_655 7_666 ? 
O1 K2 I1 101.74(8) 8_656 7_666 ? 
O1 K2 I1 78.26(8) 2_655 7_666 ? 
O1 K2 I1 22.77(8) 9_656 7_666 ? 
O1 K2 I1 71.01(8) 7_656 7_666 ? 
O1 K2 I1 108.99(8) 1_655 7_666 ? 
I1 K2 I1 93.811(12) 1_545 7_666 ? 
I1 K2 I1 86.189(12) 7_766 7_666 ? 
O1 K2 I1 22.77(8) 3_655 1_645 ? 
O1 K2 I1 78.26(8) 8_656 1_645 ? 
O1 K2 I1 101.74(8) 2_655 1_645 ? 
O1 K2 I1 157.23(8) 9_656 1_645 ? 
O1 K2 I1 108.99(8) 7_656 1_645 ? 
O1 K2 I1 71.01(8) 1_655 1_645 ? 
I1 K2 I1 86.189(12) 1_545 1_645 ? 
I1 K2 I1 93.811(12) 7_766 1_645 ? 
I1 K2 I1 180.000(12) 7_666 1_645 ? 
O1 K2 I1 78.26(8) 3_655 7_656 ? 
O1 K2 I1 71.01(8) 8_656 7_656 ? 
O1 K2 I1 108.99(8) 2_655 7_656 ? 
O1 K2 I1 101.74(8) 9_656 7_656 ? 
O1 K2 I1 22.77(7) 7_656 7_656 ? 
O1 K2 I1 157.23(7) 1_655 7_656 ? 
I1 K2 I1 93.811(12) 1_545 7_656 ? 
I1 K2 I1 86.189(12) 7_766 7_656 ? 
I1 K2 I1 86.189(12) 7_666 7_656 ? 
I1 K2 I1 93.811(12) 1_645 7_656 ? 
O1 K2 I1 101.74(8) 3_655 1_655 ? 
O1 K2 I1 108.99(8) 8_656 1_655 ? 
O1 K2 I1 71.01(8) 2_655 1_655 ? 
O1 K2 I1 78.26(8) 9_656 1_655 ? 
O1 K2 I1 157.23(7) 7_656 1_655 ? 
O1 K2 I1 22.77(7) 1_655 1_655 ? 
I1 K2 I1 86.189(12) 1_545 1_655 ? 
I1 K2 I1 93.811(12) 7_766 1_655 ? 
I1 K2 I1 93.811(12) 7_666 1_655 ? 
I1 K2 I1 86.189(12) 1_645 1_655 ? 
I1 K2 I1 180.0 7_656 1_655 ? 
O1 Zn1 O1 94.75(15) 3_665 2_655 ? 
O1 Zn1 O1 94.75(15) 3_665 . ? 
O1 Zn1 O1 94.75(15) 2_655 . ? 
O1 Zn1 O3 175.02(16) 3_665 2_655 ? 
O1 Zn1 O3 87.91(15) 2_655 2_655 ? 
O1 Zn1 O3 89.22(16) . 2_655 ? 
O1 Zn1 O3 87.91(15) 3_665 3_665 ? 
O1 Zn1 O3 89.22(16) 2_655 3_665 ? 
O1 Zn1 O3 175.02(16) . 3_665 ? 
O3 Zn1 O3 87.91(15) 2_655 3_665 ? 
O1 Zn1 O3 89.22(16) 3_665 . ? 
O1 Zn1 O3 175.02(16) 2_655 . ? 
O1 Zn1 O3 87.91(15) . . ? 
O3 Zn1 O3 87.91(15) 2_655 . ? 
O3 Zn1 O3 87.91(15) 3_665 . ? 
O1 Zn1 K1 121.83(11) 3_665 . ? 
O1 Zn1 K1 121.83(11) 2_655 . ? 
O1 Zn1 K1 121.83(11) . . ? 
O3 Zn1 K1 53.27(11) 2_655 . ? 
O3 Zn1 K1 53.27(11) 3_665 . ? 
O3 Zn1 K1 53.27(11) . . ? 
O3 V1 O3 110.44(14) 2_765 3_675 ? 
O3 V1 O3 110.44(14) 2_765 . ? 
O3 V1 O3 110.44(14) 3_675 . ? 
O3 V1 O2 108.48(14) 2_765 . ? 
O3 V1 O2 108.48(14) 3_675 . ? 
O3 V1 O2 108.48(14) . . ? 
O3 V1 K1 138.71(15) 2_765 1_565 ? 
O3 V1 K1 50.01(14) 3_675 1_565 ? 
O3 V1 K1 110.68(15) . 1_565 ? 
O2 V1 K1 60.94(2) . 1_565 ? 
O3 V1 K1 110.68(15) 2_765 . ? 
O3 V1 K1 138.71(15) 3_675 . ? 
O3 V1 K1 50.01(14) . . ? 
O2 V1 K1 60.94(2) . . ? 
K1 V1 K1 98.41(3) 1_565 . ? 
O3 V1 K1 50.01(14) 2_765 1_665 ? 
O3 V1 K1 110.68(15) 3_675 1_665 ? 
O3 V1 K1 138.71(15) . 1_665 ? 
O2 V1 K1 60.94(2) . 1_665 ? 
K1 V1 K1 98.41(3) 1_565 1_665 ? 
K1 V1 K1 98.41(3) . 1_665 ? 
O1 I1 O1 98.60(16) 2_665 3_565 ? 
O1 I1 O1 98.60(16) 2_665 . ? 
O1 I1 O1 98.60(16) 3_565 . ? 
O1 I1 K2 38.21(12) 2_665 1_565 ? 
O1 I1 K2 111.71(12) 3_565 1_565 ? 
O1 I1 K2 61.62(13) . 1_565 ? 
O1 I1 K2 61.62(13) 2_665 1_465 ? 
O1 I1 K2 38.21(12) 3_565 1_465 ? 
O1 I1 K2 111.71(12) . 1_465 ? 
K2 I1 K2 86.189(12) 1_565 1_465 ? 
O1 I1 K2 111.71(12) 2_665 1_455 ? 
O1 I1 K2 61.62(13) 3_565 1_455 ? 
O1 I1 K2 38.21(12) . 1_455 ? 
K2 I1 K2 86.189(12) 1_565 1_455 ? 
K2 I1 K2 86.189(12) 1_465 1_455 ? 
I1 O1 Zn1 113.43(19) . . ? 
I1 O1 K2 119.03(17) . 1_455 ? 
Zn1 O1 K2 116.09(15) . 1_455 ? 
V1 O2 V1 180.0 10_556 . ? 
V1 O2 K1 90.0 10_556 1_565 ? 
V1 O2 K1 90.0 . 1_565 ? 
V1 O2 K1 90.0 10_556 . ? 
V1 O2 K1 90.0 . . ? 
K1 O2 K1 120.0 1_565 . ? 
V1 O2 K1 90.0 10_556 1_665 ? 
V1 O2 K1 90.0 . 1_665 ? 
K1 O2 K1 120.0 1_565 1_665 ? 
K1 O2 K1 120.0 . 1_665 ? 
V1 O3 Zn1 147.4(3) . . ? 
V1 O3 K1 103.59(17) . . ? 
Zn1 O3 K1 89.86(13) . . ? 
K1 O1W K1 120.0 1_565 1_455 ? 
K1 O1W K1 120.0 1_565 . ? 
K1 O1W K1 120.0 1_455 . ? 
 
_diffrn_measured_fraction_theta_max    0.985 
_diffrn_reflns_theta_full              27.50 
_diffrn_measured_fraction_theta_full   0.985 
_refine_diff_density_max    0.777 
_refine_diff_density_min   -1.076 
_refine_diff_density_rms    0.179 

#===end

data_K4Ni4(V2O7)2(IO3)4(H2O)
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety           '2(I2 Ni2 O13 V2), 2(O0.50), 4(K)'  
_chemical_formula_sum 
 'H2 I4 K4 Ni4 O27 V4' 
_chemical_formula_weight          1536.62 
 
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'H'  'H'   0.0000   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'I'  'I'  -0.4742   1.8119 
 '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' 
 'Ni'  'Ni'   0.3393   1.1124 
 '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' 
 'V'  'V'   0.3005   0.5294 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            hexagonal 
_symmetry_space_group_name_H-M   P6(3)/m
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 'x-y, x, z+1/2' 
 '-y, x-y, z' 
 '-x, -y, z+1/2' 
 '-x+y, -x, z' 
 'y, -x+y, z+1/2' 
 '-x, -y, -z' 
 '-x+y, -x, -z-1/2' 
 'y, -x+y, -z' 
 'x, y, -z-1/2' 
 'x-y, x, -z' 
 '-y, x-y, -z-1/2' 
 
_cell_length_a                    5.5379(2) 
_cell_length_b                    5.5379(2) 
_cell_length_c                    25.931(2) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 120.00 
_cell_volume                      688.72(6) 
_cell_formula_units_Z             1 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used    1876
_cell_measurement_theta_min       4.25 
_cell_measurement_theta_max       27.48
 
_exptl_crystal_description       'hexagonal plate' 
_exptl_crystal_colour             'light green' 
_exptl_crystal_size_max           0.11 
_exptl_crystal_size_mid           0.10 
_exptl_crystal_size_min           0.03  
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     3.705 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              710 
_exptl_absorpt_coefficient_mu     9.159 
_exptl_absorpt_correction_type    'Multi-scan' 
_exptl_absorpt_correction_T_min   0.4622
_exptl_absorpt_correction_T_max   1.0000 
_exptl_absorpt_process_details    'Higashi'
 
_exptl_special_details 
; 
 Higashi, T. . Program for Absorption Correction.

  Rigaku Corporation, Tokyo, Japan.
; 
 
_diffrn_ambient_temperature       293(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   ? 
_diffrn_measurement_method         'CCD_Profile_fitting'   
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             5852 
_diffrn_reflns_av_R_equivalents   0.0656 
_diffrn_reflns_av_sigmaI/netI     0.0331 
_diffrn_reflns_limit_h_min        -7 
_diffrn_reflns_limit_h_max        7 
_diffrn_reflns_limit_k_min        -7 
_diffrn_reflns_limit_k_max        7 
_diffrn_reflns_limit_l_min        -33 
_diffrn_reflns_limit_l_max        32 
_diffrn_reflns_theta_min          4.25 
_diffrn_reflns_theta_max          27.48 
_reflns_number_total              542 
_reflns_number_gt                 538 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_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)+(0.0152P)²+8.1237P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    none 
_refine_ls_hydrogen_treatment     none 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          542 
_refine_ls_number_parameters      38 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0521 
_refine_ls_R_factor_gt            0.0512 
_refine_ls_wR_factor_ref          0.0972 
_refine_ls_wR_factor_gt           0.0968 
_refine_ls_goodness_of_fit_ref    1.391 
_refine_ls_restrained_S_all       1.391 
_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 
K1 K 0.3333 0.6667 0.2500 0.035(3) Uani 0.68(2) 6 d SP . . 
K2 K 0.3333 0.6667 -0.0188(2) 0.055(2) Uani 0.658(10) 3 d SP . . 
Ni1 Ni 0.3333 0.6667 0.11578(7) 0.0170(4) Uani 1 3 d S . . 
V1 V 0.6667 0.3333 0.18147(8) 0.0121(5) Uani 1 3 d S . . 
I1 I 0.0000 1.0000 0.10291(3) 0.0148(3) Uani 1 3 d S . . 
O1 O 0.2157(11) 0.8911(11) 0.0689(2) 0.0197(12) Uani 1 1 d . . . 
O2 O 0.6667 0.3333 0.2500 0.054(6) Uani 1 6 d S . . 
O3 O 0.4364(13) 0.4235(12) 0.1596(2) 0.0224(12) Uani 1 1 d . . . 
O1W O 0.0000 1.0000 0.2500 0.025(6) Uani 0.50 6 d SP . . 
 
 
_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 O3 2.898(6) 5_565 ? 
K1 O3 2.898(6) 12_666 ? 
K1 O3 2.898(6) 3_665 ? 
K1 O3 2.898(6) 8_566 ? 
K1 O3 2.898(6) . ? 
K1 O3 2.898(6) 10_556 ? 
K1 O2 3.19731(11) 1_565 ? 
K1 O2 3.19731(11) 1_455 ? 
K1 O1W 3.19731(11) . ? 
K1 O1W 3.19731(11) 1_655 ? 
K1 O1W 3.19731(11) 1_545 ? 
K1 O2 3.19731(11) . ? 
K2 O1 2.795(6) 9_455 ? 
K2 O1 2.795(6) 7_675 ? 
K2 O1 2.795(6) 11_655 ? 
K2 O1 2.820(7) . ? 
K2 O1 2.820(7) 5_565 ? 
K2 O1 2.820(7) 3_665 ? 
K2 O1 3.330(6) 7_565 ? 
K2 O1 3.330(6) 11_665 ? 
K2 O1 3.330(6) 9 ? 
K2 K2 3.342(4) 7_675 ? 
K2 K2 3.342(4) 7_565 ? 
K2 K2 3.342(4) 7_665 ? 
Ni1 O3 2.049(6) 3_665 ? 
Ni1 O3 2.049(6) 5_565 ? 
Ni1 O3 2.049(6) . ? 
Ni1 O1 2.062(5) 3_665 ? 
Ni1 O1 2.062(5) . ? 
Ni1 O1 2.062(5) 5_565 ? 
V1 O3 1.683(6) 3_655 ? 
V1 O3 1.683(6) 5_665 ? 
V1 O3 1.683(6) . ? 
V1 O2 1.777(2) . ? 
V1 K1 3.6579(10) 1_655 ? 
V1 K1 3.6579(10) 1_545 ? 
I1 O1 1.813(5) 5_465 ? 
I1 O1 1.813(5) 3_675 ? 
I1 O1 1.813(5) . ? 
I1 K2 3.871(4) 7_565 ? 
I1 K2 3.871(4) 7_575 ? 
I1 K2 3.871(4) 7_675 ? 
O1 K2 2.795(6) 7_675 ? 
O1 K2 3.330(6) 7_565 ? 
O2 V1 1.777(2) 8_666 ? 
O2 K1 3.19731(11) 1_655 ? 
O2 K1 3.19731(11) 1_545 ? 
O1W K1 3.19731(11) 1_565 ? 
O1W K1 3.19731(11) 1_455 ? 
 
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 
O3 K1 O3 145.78(9) 5_565 12_666 ? 
O3 K1 O3 61.26(18) 5_565 3_665 ? 
O3 K1 O3 107.9(2) 12_666 3_665 ? 
O3 K1 O3 107.9(2) 5_565 8_566 ? 
O3 K1 O3 61.26(18) 12_666 8_566 ? 
O3 K1 O3 145.78(9) 3_665 8_566 ? 
O3 K1 O3 61.26(18) 5_565 . ? 
O3 K1 O3 145.78(9) 12_666 . ? 
O3 K1 O3 61.26(18) 3_665 . ? 
O3 K1 O3 145.78(9) 8_566 . ? 
O3 K1 O3 145.78(9) 5_565 10_556 ? 
O3 K1 O3 61.26(18) 12_666 10_556 ? 
O3 K1 O3 145.78(9) 3_665 10_556 ? 
O3 K1 O3 61.26(18) 8_566 10_556 ? 
O3 K1 O3 107.9(2) . 10_556 ? 
O3 K1 O2 99.82(12) 5_565 1_565 ? 
O3 K1 O2 55.05(11) 12_666 1_565 ? 
O3 K1 O2 55.05(11) 3_665 1_565 ? 
O3 K1 O2 99.82(12) 8_566 1_565 ? 
O3 K1 O2 113.73(12) . 1_565 ? 
O3 K1 O2 113.73(12) 10_556 1_565 ? 
O3 K1 O2 55.05(11) 5_565 1_455 ? 
O3 K1 O2 113.73(12) 12_666 1_455 ? 
O3 K1 O2 113.73(12) 3_665 1_455 ? 
O3 K1 O2 55.05(11) 8_566 1_455 ? 
O3 K1 O2 99.82(12) . 1_455 ? 
O3 K1 O2 99.82(12) 10_556 1_455 ? 
O2 K1 O2 120.0 1_565 1_455 ? 
O3 K1 O1W 66.27(12) 5_565 . ? 
O3 K1 O1W 80.18(12) 12_666 . ? 
O3 K1 O1W 80.18(12) 3_665 . ? 
O3 K1 O1W 66.27(12) 8_566 . ? 
O3 K1 O1W 124.95(11) . . ? 
O3 K1 O1W 124.95(11) 10_556 . ? 
O2 K1 O1W 60.0 1_565 . ? 
O2 K1 O1W 60.0 1_455 . ? 
O3 K1 O1W 124.95(11) 5_565 1_655 ? 
O3 K1 O1W 66.27(12) 12_666 1_655 ? 
O3 K1 O1W 66.27(12) 3_665 1_655 ? 
O3 K1 O1W 124.95(11) 8_566 1_655 ? 
O3 K1 O1W 80.18(12) . 1_655 ? 
O3 K1 O1W 80.18(12) 10_556 1_655 ? 
O2 K1 O1W 60.0 1_565 1_655 ? 
O2 K1 O1W 180.0 1_455 1_655 ? 
O1W K1 O1W 120.0 . 1_655 ? 
O3 K1 O1W 80.18(12) 5_565 1_545 ? 
O3 K1 O1W 124.95(11) 12_666 1_545 ? 
O3 K1 O1W 124.95(11) 3_665 1_545 ? 
O3 K1 O1W 80.18(12) 8_566 1_545 ? 
O3 K1 O1W 66.27(12) . 1_545 ? 
O3 K1 O1W 66.27(12) 10_556 1_545 ? 
O2 K1 O1W 180.0 1_565 1_545 ? 
O2 K1 O1W 60.0 1_455 1_545 ? 
O1W K1 O1W 120.0 . 1_545 ? 
O1W K1 O1W 120.0 1_655 1_545 ? 
O3 K1 O2 113.73(12) 5_565 . ? 
O3 K1 O2 99.82(12) 12_666 . ? 
O3 K1 O2 99.82(12) 3_665 . ? 
O3 K1 O2 113.73(12) 8_566 . ? 
O3 K1 O2 55.05(11) . . ? 
O3 K1 O2 55.05(11) 10_556 . ? 
O2 K1 O2 120.0 1_565 . ? 
O2 K1 O2 120.0 1_455 . ? 
O1W K1 O2 180.0 . . ? 
O1W K1 O2 60.0 1_655 . ? 
O1W K1 O2 60.0 1_545 . ? 
O1 K2 O1 100.1(2) 9_455 7_675 ? 
O1 K2 O1 100.1(2) 9_455 11_655 ? 
O1 K2 O1 100.1(2) 7_675 11_655 ? 
O1 K2 O1 88.3(2) 9_455 . ? 
O1 K2 O1 106.94(14) 7_675 . ? 
O1 K2 O1 149.8(2) 11_655 . ? 
O1 K2 O1 149.8(2) 9_455 5_565 ? 
O1 K2 O1 88.3(2) 7_675 5_565 ? 
O1 K2 O1 106.94(14) 11_655 5_565 ? 
O1 K2 O1 61.6(2) . 5_565 ? 
O1 K2 O1 106.94(14) 9_455 3_665 ? 
O1 K2 O1 149.8(2) 7_675 3_665 ? 
O1 K2 O1 88.3(2) 11_655 3_665 ? 
O1 K2 O1 61.6(2) . 3_665 ? 
O1 K2 O1 61.6(2) 5_565 3_665 ? 
O1 K2 O1 55.4(2) 9_455 7_565 ? 
O1 K2 O1 129.2(3) 7_675 7_565 ? 
O1 K2 O1 52.4(2) 11_655 7_565 ? 
O1 K2 O1 114.77(13) . 7_565 ? 
O1 K2 O1 136.53(17) 5_565 7_565 ? 
O1 K2 O1 78.50(19) 3_665 7_565 ? 
O1 K2 O1 52.4(2) 9_455 11_665 ? 
O1 K2 O1 55.4(2) 7_675 11_665 ? 
O1 K2 O1 129.2(3) 11_655 11_665 ? 
O1 K2 O1 78.50(19) . 11_665 ? 
O1 K2 O1 114.77(13) 5_565 11_665 ? 
O1 K2 O1 136.53(17) 3_665 11_665 ? 
O1 K2 O1 105.73(15) 7_565 11_665 ? 
O1 K2 O1 129.2(3) 9_455 9 ? 
O1 K2 O1 52.4(2) 7_675 9 ? 
O1 K2 O1 55.4(2) 11_655 9 ? 
O1 K2 O1 136.53(17) . 9 ? 
O1 K2 O1 78.50(19) 5_565 9 ? 
O1 K2 O1 114.77(13) 3_665 9 ? 
O1 K2 O1 105.73(15) 7_565 9 ? 
O1 K2 O1 105.73(15) 11_665 9 ? 
O1 K2 K2 96.97(13) 9_455 7_675 ? 
O1 K2 K2 53.82(14) 7_675 7_675 ? 
O1 K2 K2 151.15(17) 11_655 7_675 ? 
O1 K2 K2 53.12(18) . 7_675 ? 
O1 K2 K2 64.77(19) 5_565 7_675 ? 
O1 K2 K2 108.8(3) 3_665 7_675 ? 
O1 K2 K2 151.93(12) 7_565 7_675 ? 
O1 K2 K2 50.00(13) 11_665 7_675 ? 
O1 K2 K2 95.85(11) 9 7_675 ? 
O1 K2 K2 53.82(14) 9_455 7_565 ? 
O1 K2 K2 151.15(17) 7_675 7_565 ? 
O1 K2 K2 96.97(13) 11_655 7_565 ? 
O1 K2 K2 64.77(19) . 7_565 ? 
O1 K2 K2 108.8(3) 5_565 7_565 ? 
O1 K2 K2 53.12(18) 3_665 7_565 ? 
O1 K2 K2 50.00(13) 7_565 7_565 ? 
O1 K2 K2 95.85(11) 11_665 7_565 ? 
O1 K2 K2 151.93(12) 9 7_565 ? 
K2 K2 K2 111.88(19) 7_675 7_565 ? 
O1 K2 K2 151.15(17) 9_455 7_665 ? 
O1 K2 K2 96.97(13) 7_675 7_665 ? 
O1 K2 K2 53.82(14) 11_655 7_665 ? 
O1 K2 K2 108.8(3) . 7_665 ? 
O1 K2 K2 53.12(18) 5_565 7_665 ? 
O1 K2 K2 64.77(19) 3_665 7_665 ? 
O1 K2 K2 95.85(11) 7_565 7_665 ? 
O1 K2 K2 151.93(12) 11_665 7_665 ? 
O1 K2 K2 50.00(13) 9 7_665 ? 
K2 K2 K2 111.88(19) 7_675 7_665 ? 
K2 K2 K2 111.88(19) 7_565 7_665 ? 
O3 Ni1 O3 92.2(2) 3_665 5_565 ? 
O3 Ni1 O3 92.2(2) 3_665 . ? 
O3 Ni1 O3 92.2(2) 5_565 . ? 
O3 Ni1 O1 176.6(2) 3_665 3_665 ? 
O3 Ni1 O1 91.2(2) 5_565 3_665 ? 
O3 Ni1 O1 87.8(2) . 3_665 ? 
O3 Ni1 O1 91.2(2) 3_665 . ? 
O3 Ni1 O1 87.8(2) 5_565 . ? 
O3 Ni1 O1 176.6(2) . . ? 
O1 Ni1 O1 88.8(2) 3_665 . ? 
O3 Ni1 O1 87.8(2) 3_665 5_565 ? 
O3 Ni1 O1 176.6(2) 5_565 5_565 ? 
O3 Ni1 O1 91.2(2) . 5_565 ? 
O1 Ni1 O1 88.8(2) 3_665 5_565 ? 
O1 Ni1 O1 88.8(2) . 5_565 ? 
O3 Ni1 K1 56.31(16) 3_665 . ? 
O3 Ni1 K1 56.31(16) 5_565 . ? 
O3 Ni1 K1 56.31(16) . . ? 
O1 Ni1 K1 126.08(15) 3_665 . ? 
O1 Ni1 K1 126.08(15) . . ? 
O1 Ni1 K1 126.08(15) 5_565 . ? 
O3 Ni1 K2 123.69(16) 3_665 . ? 
O3 Ni1 K2 123.69(16) 5_565 . ? 
O3 Ni1 K2 123.69(16) . . ? 
O1 Ni1 K2 53.92(15) 3_665 . ? 
O1 Ni1 K2 53.92(15) . . ? 
O1 Ni1 K2 53.92(15) 5_565 . ? 
K1 Ni1 K2 180.0 . . ? 
O3 V1 O3 109.3(2) 3_655 5_665 ? 
O3 V1 O3 109.3(2) 3_655 . ? 
O3 V1 O3 109.3(2) 5_665 . ? 
O3 V1 O2 109.7(2) 3_655 . ? 
O3 V1 O2 109.7(2) 5_665 . ? 
O3 V1 O2 109.7(2) . . ? 
O3 V1 K1 112.8(2) 3_655 1_655 ? 
O3 V1 K1 50.62(19) 5_665 1_655 ? 
O3 V1 K1 137.5(2) . 1_655 ? 
O2 V1 K1 60.94(3) . 1_655 ? 
O3 V1 K1 50.62(19) 3_655 1_545 ? 
O3 V1 K1 137.5(2) 5_665 1_545 ? 
O3 V1 K1 112.8(2) . 1_545 ? 
O2 V1 K1 60.94(3) . 1_545 ? 
K1 V1 K1 98.40(3) 1_655 1_545 ? 
O3 V1 K1 137.5(2) 3_655 . ? 
O3 V1 K1 112.8(2) 5_665 . ? 
O3 V1 K1 50.62(19) . . ? 
O2 V1 K1 60.94(3) . . ? 
K1 V1 K1 98.40(3) 1_655 . ? 
K1 V1 K1 98.40(3) 1_545 . ? 
O1 I1 O1 98.4(2) 5_465 3_675 ? 
O1 I1 O1 98.4(2) 5_465 . ? 
O1 I1 O1 98.4(2) 3_675 . ? 
O1 I1 K2 41.83(17) 5_465 7_565 ? 
O1 I1 K2 115.82(19) 3_675 7_565 ? 
O1 I1 K2 59.22(18) . 7_565 ? 
O1 I1 K2 59.22(17) 5_465 7_575 ? 
O1 I1 K2 41.83(17) 3_675 7_575 ? 
O1 I1 K2 115.82(19) . 7_575 ? 
K2 I1 K2 91.35(11) 7_565 7_575 ? 
O1 I1 K2 115.82(19) 5_465 7_675 ? 
O1 I1 K2 59.22(18) 3_675 7_675 ? 
O1 I1 K2 41.83(17) . 7_675 ? 
K2 I1 K2 91.35(11) 7_565 7_675 ? 
K2 I1 K2 91.35(11) 7_575 7_675 ? 
I1 O1 Ni1 111.9(3) . . ? 
I1 O1 K2 112.5(2) . 7_675 ? 
Ni1 O1 K2 112.9(2) . 7_675 ? 
I1 O1 K2 151.0(3) . . ? 
Ni1 O1 K2 89.8(2) . . ? 
K2 O1 K2 73.06(14) 7_675 . ? 
I1 O1 K2 92.9(2) . 7_565 ? 
Ni1 O1 K2 95.05(19) . 7_565 ? 
K2 O1 K2 129.2(3) 7_675 7_565 ? 
K2 O1 K2 65.23(13) . 7_565 ? 
V1 O2 V1 180.0 . 8_666 ? 
V1 O2 K1 90.0 . 1_655 ? 
V1 O2 K1 90.0 8_666 1_655 ? 
V1 O2 K1 90.0 . 1_545 ? 
V1 O2 K1 90.0 8_666 1_545 ? 
K1 O2 K1 120.0 1_655 1_545 ? 
V1 O2 K1 90.0 . . ? 
V1 O2 K1 90.0 8_666 . ? 
K1 O2 K1 120.0 1_655 . ? 
K1 O2 K1 120.0 1_545 . ? 
V1 O3 Ni1 152.0(4) . . ? 
V1 O3 K1 102.7(2) . . ? 
Ni1 O3 K1 87.7(2) . . ? 
K1 O1W K1 120.0 . 1_565 ? 
K1 O1W K1 120.0 . 1_455 ? 
K1 O1W K1 120.0 1_565 1_455 ? 
 
_diffrn_measured_fraction_theta_max    0.991 
_diffrn_reflns_theta_full              27.48 
_diffrn_measured_fraction_theta_full   0.991 
_refine_diff_density_max    0.859 
_refine_diff_density_min   -1.406 
_refine_diff_density_rms    0.184 

#===end

data_K4Co4(V2O7)2(IO3)4(H2O) 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          '2(Co2 I2 O13 V2), 2(O0.50)2H, 4.0(K) '
_chemical_formula_sum 
 'Co4 H2 I4 K4 O27 V4' 
_chemical_formula_weight          1537.50 
 
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'O'  'O'   0.0106   0.0060 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'H'  'H'   0.0000   0.0000 
 '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' 
 'V'  'V'   0.3005   0.5294 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Co'  'Co'   0.3494   0.9721 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'I'  'I'  -0.4742   1.8119 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            hexagonal 
_symmetry_space_group_name_H-M    P6(3)/m 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-y, x-y, z' 
 '-x+y, -x, z' 
 '-x, -y, z+1/2' 
 'y, -x+y, z+1/2' 
 'x-y, x, z+1/2' 
 '-x, -y, -z' 
 'y, -x+y, -z' 
 'x-y, x, -z' 
 'x, y, -z-1/2' 
 '-y, x-y, -z-1/2' 
 '-x+y, -x, -z-1/2' 
 
_cell_length_a                    5.5840(2) 
_cell_length_b                    5.5840(2) 
_cell_length_c                    25.991(2) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 120.00 
_cell_volume                      701.85(6) 
_cell_formula_units_Z             1 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used    2659
_cell_measurement_theta_min             2.1056
_cell_measurement_theta_max             27.4680 
 
_exptl_crystal_description        Plate 
_exptl_crystal_colour             brown 
_exptl_crystal_size_max           0.3 
_exptl_crystal_size_mid           0.3 
_exptl_crystal_size_min           0.02 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     3.638 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              706 
_exptl_absorpt_coefficient_mu     8.668 
_exptl_absorpt_correction_type    'Multi-scan' 
_exptl_absorpt_correction_T_min   0.093 
_exptl_absorpt_correction_T_max   0.841 
_exptl_absorpt_process_details     'Higashi'  
 
_exptl_special_details 
; 
 Higashi, T. . Program for Absorption Correction.

  Rigaku Corporation, Tokyo, Japan.

; 
 
_diffrn_ambient_temperature       293(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   ? 
_diffrn_measurement_method        'CCD_Profile_fitting'  
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             5363 
_diffrn_reflns_av_R_equivalents   0.0288 
_diffrn_reflns_av_sigmaI/netI     0.0124 
_diffrn_reflns_limit_h_min        -7 
_diffrn_reflns_limit_h_max        6 
_diffrn_reflns_limit_k_min        -7 
_diffrn_reflns_limit_k_max        7 
_diffrn_reflns_limit_l_min        -33 
_diffrn_reflns_limit_l_max        33 
_diffrn_reflns_theta_min          4.21 
_diffrn_reflns_theta_max          27.47 
_reflns_number_total              553 
_reflns_number_gt                 534 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_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)+(0.0342P)²+2.2016P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    none 
_refine_ls_hydrogen_treatment     none
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          553 
_refine_ls_number_parameters      38 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0279 
_refine_ls_R_factor_gt            0.0270 
_refine_ls_wR_factor_ref          0.0697 
_refine_ls_wR_factor_gt           0.0689 
_refine_ls_goodness_of_fit_ref    1.212 
_refine_ls_restrained_S_all       1.212 
_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 
K1 K 0.3333 0.6667 0.2500 0.0320(12) Uani 0.657(10) 6 d SP . . 
K2 K 0.3333 0.6667 -0.01940(13) 0.0570(11) Uani 0.672(5) 3 d SP . . 
Co1 Co 0.3333 0.6667 0.11612(4) 0.0161(2) Uani 1 3 d S . . 
V1 V -0.3333 0.3333 0.18154(4) 0.0100(2) Uani 1 3 d S . . 
I1 I 0.0000 0.0000 0.102031(15) 0.01317(18) Uani 1 3 d S . . 
O1 O 0.1080(5) 0.3219(5) 0.06841(11) 0.0209(6) Uani 1 1 d . . . 
O2 O -0.3333 0.3333 0.2500 0.049(3) Uani 1 6 d S . . 
O3 O -0.0165(6) 0.5651(6) 0.15999(12) 0.0253(6) Uani 1 1 d . . . 
O1W O 0.0000 1.0000 0.2500 0.027(3) Uani 0.50 6 d SP . . 
 
 
_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 O3 2.916(3) 12_566 ? 
K1 O3 2.916(3) . ? 
K1 O3 2.916(3) 10_556 ? 
K1 O3 2.916(3) 11_666 ? 
K1 O3 2.916(3) 3_565 ? 
K1 O3 2.916(3) 2_665 ? 
K1 O2 3.22392(11) . ? 
K1 O2 3.22392(11) 1_665 ? 
K1 O1W 3.22392(11) . ? 
K1 O1W 3.22392(11) 1_655 ? 
K1 O1W 3.22392(12) 1_545 ? 
K1 O2 3.22392(11) 1_655 ? 
K2 O1 2.803(3) 7_565 ? 
K2 O1 2.803(3) 9_665 ? 
K2 O1 2.803(3) 8 ? 
K2 O1 2.842(4) 3_565 ? 
K2 O1 2.842(4) 2_665 ? 
K2 O1 2.842(4) . ? 
K2 O1 3.340(3) 9 ? 
K2 O1 3.340(3) 8_565 ? 
K2 O1 3.340(3) 7_665 ? 
K2 K2 3.378(2) 7_675 ? 
K2 K2 3.378(2) 7_565 ? 
K2 K2 3.378(2) 7_665 ? 
Co1 O3 2.081(3) 3_565 ? 
Co1 O3 2.081(3) . ? 
Co1 O3 2.081(3) 2_665 ? 
Co1 O1 2.099(3) . ? 
Co1 O1 2.099(3) 3_565 ? 
Co1 O1 2.099(3) 2_665 ? 
V1 O3 1.682(3) 3_455 ? 
V1 O3 1.682(3) . ? 
V1 O3 1.682(3) 2_565 ? 
V1 O2 1.7793(10) . ? 
V1 K1 3.6823(5) 1_445 ? 
V1 K1 3.6823(5) 1_455 ? 
I1 O1 1.809(3) 2 ? 
I1 O1 1.809(3) . ? 
I1 O1 1.809(3) 3 ? 
I1 K2 3.8738(19) 7 ? 
I1 K2 3.8738(19) 7_565 ? 
I1 K2 3.8738(19) 7_665 ? 
O1 K2 2.803(3) 7_565 ? 
O1 K2 3.340(3) 7_665 ? 
O2 V1 1.7793(10) 10_556 ? 
O2 K1 3.22392(12) 1_445 ? 
O2 K1 3.22392(11) 1_455 ? 
O1W K1 3.22392(11) 1_565 ? 
O1W K1 3.22392(11) 1_455 ? 
 
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 
O3 K1 O3 145.27(5) 12_566 . ? 
O3 K1 O3 62.26(9) 12_566 10_556 ? 
O3 K1 O3 106.69(11) . 10_556 ? 
O3 K1 O3 62.26(9) 12_566 11_666 ? 
O3 K1 O3 145.27(5) . 11_666 ? 
O3 K1 O3 62.26(9) 10_556 11_666 ? 
O3 K1 O3 106.69(12) 12_566 3_565 ? 
O3 K1 O3 62.26(9) . 3_565 ? 
O3 K1 O3 145.27(5) 10_556 3_565 ? 
O3 K1 O3 145.27(5) 11_666 3_565 ? 
O3 K1 O3 145.27(5) 12_566 2_665 ? 
O3 K1 O3 62.26(9) . 2_665 ? 
O3 K1 O3 145.27(5) 10_556 2_665 ? 
O3 K1 O3 106.69(11) 11_666 2_665 ? 
O3 K1 O3 62.26(9) 3_565 2_665 ? 
O3 K1 O2 114.32(7) 12_566 . ? 
O3 K1 O2 54.53(6) . . ? 
O3 K1 O2 54.53(5) 10_556 . ? 
O3 K1 O2 99.70(6) 11_666 . ? 
O3 K1 O2 114.32(7) 3_565 . ? 
O3 K1 O2 99.70(6) 2_665 . ? 
O3 K1 O2 54.53(5) 12_566 1_665 ? 
O3 K1 O2 99.70(6) . 1_665 ? 
O3 K1 O2 99.70(6) 10_556 1_665 ? 
O3 K1 O2 114.32(7) 11_666 1_665 ? 
O3 K1 O2 54.53(5) 3_565 1_665 ? 
O3 K1 O2 114.32(7) 2_665 1_665 ? 
O2 K1 O2 120.0 . 1_665 ? 
O3 K1 O1W 80.30(6) 12_566 . ? 
O3 K1 O1W 65.68(7) . . ? 
O3 K1 O1W 65.68(7) 10_556 . ? 
O3 K1 O1W 125.47(5) 11_666 . ? 
O3 K1 O1W 80.30(6) 3_565 . ? 
O3 K1 O1W 125.47(5) 2_665 . ? 
O2 K1 O1W 60.0 . . ? 
O2 K1 O1W 60.0 1_665 . ? 
O3 K1 O1W 65.68(7) 12_566 1_655 ? 
O3 K1 O1W 125.47(6) . 1_655 ? 
O3 K1 O1W 125.47(6) 10_556 1_655 ? 
O3 K1 O1W 80.30(6) 11_666 1_655 ? 
O3 K1 O1W 65.68(7) 3_565 1_655 ? 
O3 K1 O1W 80.30(6) 2_665 1_655 ? 
O2 K1 O1W 180.0 . 1_655 ? 
O2 K1 O1W 60.0 1_665 1_655 ? 
O1W K1 O1W 120.0 . 1_655 ? 
O3 K1 O1W 125.47(5) 12_566 1_545 ? 
O3 K1 O1W 80.30(6) . 1_545 ? 
O3 K1 O1W 80.30(6) 10_556 1_545 ? 
O3 K1 O1W 65.68(7) 11_666 1_545 ? 
O3 K1 O1W 125.47(5) 3_565 1_545 ? 
O3 K1 O1W 65.68(7) 2_665 1_545 ? 
O2 K1 O1W 60.0 . 1_545 ? 
O2 K1 O1W 180.0 1_665 1_545 ? 
O1W K1 O1W 120.0 . 1_545 ? 
O1W K1 O1W 120.0 1_655 1_545 ? 
O3 K1 O2 99.70(6) 12_566 1_655 ? 
O3 K1 O2 114.32(7) . 1_655 ? 
O3 K1 O2 114.32(7) 10_556 1_655 ? 
O3 K1 O2 54.53(5) 11_666 1_655 ? 
O3 K1 O2 99.70(6) 3_565 1_655 ? 
O3 K1 O2 54.53(5) 2_665 1_655 ? 
O2 K1 O2 120.0 . 1_655 ? 
O2 K1 O2 120.0 1_665 1_655 ? 
O1W K1 O2 180.0 . 1_655 ? 
O1W K1 O2 60.0 1_655 1_655 ? 
O1W K1 O2 60.0 1_545 1_655 ? 
O1 K2 O1 100.97(11) 7_565 9_665 ? 
O1 K2 O1 100.97(11) 7_565 8 ? 
O1 K2 O1 100.97(11) 9_665 8 ? 
O1 K2 O1 87.20(11) 7_565 3_565 ? 
O1 K2 O1 106.49(8) 9_665 3_565 ? 
O1 K2 O1 149.29(11) 8 3_565 ? 
O1 K2 O1 149.29(11) 7_565 2_665 ? 
O1 K2 O1 87.20(11) 9_665 2_665 ? 
O1 K2 O1 106.49(8) 8 2_665 ? 
O1 K2 O1 62.14(11) 3_565 2_665 ? 
O1 K2 O1 106.49(8) 7_565 . ? 
O1 K2 O1 149.29(11) 9_665 . ? 
O1 K2 O1 87.20(11) 8 . ? 
O1 K2 O1 62.14(11) 3_565 . ? 
O1 K2 O1 62.14(11) 2_665 . ? 
O1 K2 O1 56.22(10) 7_565 9 ? 
O1 K2 O1 130.51(15) 9_665 9 ? 
O1 K2 O1 52.17(10) 8 9 ? 
O1 K2 O1 114.34(7) 3_565 9 ? 
O1 K2 O1 136.17(9) 2_665 9 ? 
O1 K2 O1 77.59(10) . 9 ? 
O1 K2 O1 52.17(10) 7_565 8_565 ? 
O1 K2 O1 56.22(10) 9_665 8_565 ? 
O1 K2 O1 130.51(15) 8 8_565 ? 
O1 K2 O1 77.59(10) 3_565 8_565 ? 
O1 K2 O1 114.34(7) 2_665 8_565 ? 
O1 K2 O1 136.17(9) . 8_565 ? 
O1 K2 O1 106.37(8) 9 8_565 ? 
O1 K2 O1 130.51(15) 7_565 7_665 ? 
O1 K2 O1 52.17(10) 9_665 7_665 ? 
O1 K2 O1 56.22(10) 8 7_665 ? 
O1 K2 O1 136.17(9) 3_565 7_665 ? 
O1 K2 O1 77.59(10) 2_665 7_665 ? 
O1 K2 O1 114.34(7) . 7_665 ? 
O1 K2 O1 106.37(8) 9 7_665 ? 
O1 K2 O1 106.37(8) 8_565 7_665 ? 
O1 K2 K2 96.71(6) 7_565 7_675 ? 
O1 K2 K2 53.77(7) 9_665 7_675 ? 
O1 K2 K2 151.79(8) 8 7_675 ? 
O1 K2 K2 52.72(9) 3_565 7_675 ? 
O1 K2 K2 64.29(10) 2_665 7_675 ? 
O1 K2 K2 108.68(16) . 7_675 ? 
O1 K2 K2 152.34(5) 9 7_675 ? 
O1 K2 K2 50.04(6) 8_565 7_675 ? 
O1 K2 K2 95.62(5) 7_665 7_675 ? 
O1 K2 K2 53.77(7) 7_565 7_565 ? 
O1 K2 K2 151.79(8) 9_665 7_565 ? 
O1 K2 K2 96.71(6) 8 7_565 ? 
O1 K2 K2 64.29(10) 3_565 7_565 ? 
O1 K2 K2 108.68(16) 2_665 7_565 ? 
O1 K2 K2 52.72(9) . 7_565 ? 
O1 K2 K2 50.04(6) 9 7_565 ? 
O1 K2 K2 95.62(5) 8_565 7_565 ? 
O1 K2 K2 152.34(5) 7_665 7_565 ? 
K2 K2 K2 111.49(10) 7_675 7_565 ? 
O1 K2 K2 151.79(8) 7_565 7_665 ? 
O1 K2 K2 96.71(6) 9_665 7_665 ? 
O1 K2 K2 53.77(7) 8 7_665 ? 
O1 K2 K2 108.68(16) 3_565 7_665 ? 
O1 K2 K2 52.72(9) 2_665 7_665 ? 
O1 K2 K2 64.29(10) . 7_665 ? 
O1 K2 K2 95.62(5) 9 7_665 ? 
O1 K2 K2 152.34(5) 8_565 7_665 ? 
O1 K2 K2 50.04(6) 7_665 7_665 ? 
K2 K2 K2 111.49(10) 7_675 7_665 ? 
K2 K2 K2 111.49(10) 7_565 7_665 ? 
O3 Co1 O3 92.85(12) 3_565 . ? 
O3 Co1 O3 92.85(12) 3_565 2_665 ? 
O3 Co1 O3 92.85(12) . 2_665 ? 
O3 Co1 O1 175.82(12) 3_565 . ? 
O3 Co1 O1 91.33(11) . . ? 
O3 Co1 O1 87.17(11) 2_665 . ? 
O3 Co1 O1 91.33(11) 3_565 3_565 ? 
O3 Co1 O1 87.17(11) . 3_565 ? 
O3 Co1 O1 175.82(12) 2_665 3_565 ? 
O1 Co1 O1 88.65(11) . 3_565 ? 
O3 Co1 O1 87.17(11) 3_565 2_665 ? 
O3 Co1 O1 175.82(12) . 2_665 ? 
O3 Co1 O1 91.33(11) 2_665 2_665 ? 
O1 Co1 O1 88.65(11) . 2_665 ? 
O1 Co1 O1 88.65(11) 3_565 2_665 ? 
O3 Co1 K1 56.78(9) 3_565 . ? 
O3 Co1 K1 56.78(9) . . ? 
O3 Co1 K1 56.78(9) 2_665 . ? 
O1 Co1 K1 126.22(8) . . ? 
O1 Co1 K1 126.22(8) 3_565 . ? 
O1 Co1 K1 126.22(8) 2_665 . ? 
O3 Co1 K2 123.22(9) 3_565 . ? 
O3 Co1 K2 123.22(9) . . ? 
O3 Co1 K2 123.22(9) 2_665 . ? 
O1 Co1 K2 53.78(8) . . ? 
O1 Co1 K2 53.78(8) 3_565 . ? 
O1 Co1 K2 53.78(8) 2_665 . ? 
K1 Co1 K2 180.0 . . ? 
O3 V1 O3 109.49(11) 3_455 . ? 
O3 V1 O3 109.49(11) 3_455 2_565 ? 
O3 V1 O3 109.49(11) . 2_565 ? 
O3 V1 O2 109.46(11) 3_455 . ? 
O3 V1 O2 109.46(11) . . ? 
O3 V1 O2 109.46(11) 2_565 . ? 
O3 V1 K1 112.02(12) 3_455 . ? 
O3 V1 K1 50.47(10) . . ? 
O3 V1 K1 138.11(11) 2_565 . ? 
O2 V1 K1 61.106(14) . . ? 
O3 V1 K1 50.47(10) 3_455 1_445 ? 
O3 V1 K1 138.11(11) . 1_445 ? 
O3 V1 K1 112.02(12) 2_565 1_445 ? 
O2 V1 K1 61.106(14) . 1_445 ? 
K1 V1 K1 98.614(18) . 1_445 ? 
O3 V1 K1 138.11(11) 3_455 1_455 ? 
O3 V1 K1 112.02(12) . 1_455 ? 
O3 V1 K1 50.47(10) 2_565 1_455 ? 
O2 V1 K1 61.106(14) . 1_455 ? 
K1 V1 K1 98.614(18) . 1_455 ? 
K1 V1 K1 98.614(18) 1_445 1_455 ? 
O1 I1 O1 98.63(12) 2 . ? 
O1 I1 O1 98.63(12) 2 3 ? 
O1 I1 O1 98.63(12) . 3 ? 
O1 I1 K2 41.97(9) 2 7 ? 
O1 I1 K2 116.63(10) . 7 ? 
O1 I1 K2 59.47(9) 3 7 ? 
O1 I1 K2 59.47(9) 2 7_565 ? 
O1 I1 K2 41.97(8) . 7_565 ? 
O1 I1 K2 116.63(10) 3 7_565 ? 
K2 I1 K2 92.23(6) 7 7_565 ? 
O1 I1 K2 116.63(10) 2 7_665 ? 
O1 I1 K2 59.47(9) . 7_665 ? 
O1 I1 K2 41.97(9) 3 7_665 ? 
K2 I1 K2 92.23(6) 7 7_665 ? 
K2 I1 K2 92.23(6) 7_565 7_665 ? 
I1 O1 Co1 112.03(14) . . ? 
I1 O1 K2 112.45(12) . 7_565 ? 
Co1 O1 K2 112.22(11) . 7_565 ? 
I1 O1 K2 151.12(15) . . ? 
Co1 O1 K2 89.64(10) . . ? 
K2 O1 K2 73.51(8) 7_565 . ? 
I1 O1 K2 92.72(10) . 7_665 ? 
Co1 O1 K2 94.70(10) . 7_665 ? 
K2 O1 K2 130.51(15) 7_565 7_665 ? 
K2 O1 K2 65.66(7) . 7_665 ? 
V1 O2 V1 180.0 10_556 . ? 
V1 O2 K1 90.0 10_556 . ? 
V1 O2 K1 90.0 . . ? 
V1 O2 K1 90.0 10_556 1_445 ? 
V1 O2 K1 90.0 . 1_445 ? 
K1 O2 K1 120.0 . 1_445 ? 
V1 O2 K1 90.0 10_556 1_455 ? 
V1 O2 K1 90.0 . 1_455 ? 
K1 O2 K1 120.0 . 1_455 ? 
K1 O2 K1 120.0 1_445 1_455 ? 
V1 O3 Co1 151.1(2) . . ? 
V1 O3 K1 103.12(13) . . ? 
Co1 O3 K1 86.57(10) . . ? 
K1 O1W K1 120.0 . 1_565 ? 
K1 O1W K1 120.0 . 1_455 ? 
K1 O1W K1 120.0 1_565 1_455 ? 
 
_diffrn_measured_fraction_theta_max    0.982 
_diffrn_reflns_theta_full              27.47 
_diffrn_measured_fraction_theta_full   0.982 
_refine_diff_density_max    1.231 
_refine_diff_density_min   -1.181 
_refine_diff_density_rms    0.180 

#===end