 
data_x 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
  'Ba Co4 O18 P4' 
_chemical_formula_weight          784.99 
 
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source  
 'Ba'  'Ba'  -0.3244   2.2819 
 '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' 
 'O'  'O'   0.0106   0.0060 
 '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' 
 
 
_symmetry_cell_setting            'orthorhombic' 
_symmetry_space_group_name_H-M    'Pnma' 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x+1/2, -y, z+1/2' 
 'x+1/2, -y+1/2, -z+1/2' 
 '-x, y+1/2, -z' 
 '-x, -y, -z' 
 'x-1/2, y, -z-1/2' 
 '-x-1/2, y-1/2, z-1/2' 
 'x, -y-1/2, z' 
 
_cell_length_a                    18.453(2) 
_cell_length_b                    8.3383(9) 
_cell_length_c                    9.4995(13) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 90.00 
_cell_volume                      1461.7(3) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     3785 
_cell_measurement_theta_min       2.1438 
_cell_measurement_theta_max       27.4835 
 
_exptl_crystal_description        'Prism' 
_exptl_crystal_colour             'Purple' 
_exptl_crystal_size_max           0.9200 
_exptl_crystal_size_mid           0.2400 
_exptl_crystal_size_min           0.1900 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     3.567 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1496 
_exptl_absorpt_coefficient_mu     7.640 
_exptl_absorpt_correction_type    'Multi-scan'
_exptl_absorpt_correction_T_min   0.7149 
_exptl_absorpt_correction_T_max   1.0000
_exptl_absorpt_process_details    ? 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       293(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   
;
Mercury2 (1x1 bin mode)
; 
_diffrn_measurement_method        'CCD_Profile_fitting' 
_diffrn_detector_area_resol_mean  13.6612 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             1916 
_diffrn_reflns_av_R_equivalents   0.0719 
_diffrn_reflns_av_sigmaI/netI     0.0592 
_diffrn_reflns_limit_h_min        -23 
_diffrn_reflns_limit_h_max        23 
_diffrn_reflns_limit_k_min        -10 
_diffrn_reflns_limit_k_max        10 
_diffrn_reflns_limit_l_min        -8 
_diffrn_reflns_limit_l_max        11 
_diffrn_reflns_theta_min          2.41 
_diffrn_reflns_theta_max          27.46 
_reflns_number_total              1750 
_reflns_number_gt                 1483 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_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)+(0.0463P)²+3.4642P] 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          1750 
_refine_ls_number_parameters      143 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0619 
_refine_ls_R_factor_gt            0.0492 
_refine_ls_wR_factor_ref          0.1190 
_refine_ls_wR_factor_gt           0.1112 
_refine_ls_goodness_of_fit_ref    1.157 
_refine_ls_restrained_S_all       1.157 
_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 
Co1 Co 0.27186(5) -0.05805(10) 0.37480(10) 0.0125(2) Uani 1 1 d . . . 
Co2 Co 0.12201(5) 0.43935(11) 0.60146(11) 0.0137(2) Uani 1 1 d . . . 
P1 P 0.25187(12) 0.2500 0.1662(3) 0.0108(5) Uani 1 2 d S . . 
P2 P 0.02416(13) 0.7500 0.5209(3) 0.0122(5) Uani 1 2 d S . . 
P3 P 0.42916(12) -0.2500 0.3847(3) 0.0119(5) Uani 1 2 d S . . 
P4 P 0.27156(12) 0.2500 0.5907(3) 0.0110(5) Uani 1 2 d S . . 
O1 O 0.1588(2) 0.0021(5) 0.3960(5) 0.0139(10) Uani 1 1 d . . . 
O2 O 0.0709(3) 0.7500 0.3786(7) 0.0143(15) Uani 1 2 d S . . 
O3 O 0.1761(3) 0.2500 0.2337(7) 0.0139(14) Uani 1 2 d S . . 
O4 O 0.1890(3) 0.2500 0.5642(7) 0.0109(13) Uani 1 2 d S . . 
O5 O 0.2580(4) -0.2500 0.5071(7) 0.0137(14) Uani 1 2 d S . . 
O6 O 0.2787(4) 0.2500 0.7523(7) 0.0159(14) Uani 1 2 d S . . 
O7 O 0.0549(3) 0.2500 0.5273(7) 0.0142(14) Uani 1 2 d S . . 
O8 O 0.2962(2) 0.1002(5) 0.2108(5) 0.0156(10) Uani 1 1 d . . . 
O9 O 0.3894(2) -0.1001(6) 0.3299(6) 0.0172(11) Uani 1 1 d . . . 
O10 O 0.3073(2) 0.1017(5) 0.5235(5) 0.0158(10) Uani 1 1 d . . . 
O11 O 0.0436(2) 0.6024(6) 0.6092(5) 0.0158(10) Uani 1 1 d . . . 
O12 O 0.5104(4) -0.2500 0.3545(8) 0.0191(16) Uani 1 2 d S . . 
O13 O 0.4292(3) -0.2500 0.5522(8) 0.0199(16) Uani 1 2 d S . . 
Ba Ba 0.41838(3) 0.2500 0.37261(7) 0.01552(19) Uani 1 2 d S . . 
 
 
_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 
Co1 O10 2.048(5) . ? 
Co1 O5 2.051(4) . ? 
Co1 O8 2.090(5) . ? 
Co1 O1 2.156(4) . ? 
Co1 O6 2.188(5) 2_554 ? 
Co1 O9 2.239(5) . ? 
Co1 Ba 3.7293(10) . ? 
Co2 O11 1.986(5) . ? 
Co2 O4 2.037(4) . ? 
Co2 O1 2.124(5) 8_565 ? 
Co2 O7 2.126(4) . ? 
Co2 O9 2.205(5) 7_666 ? 
Co2 O8 2.270(5) 7_666 ? 
Co2 Ba 3.7283(11) 2_565 ? 
P1 O5 1.522(7) 2_554 ? 
P1 O3 1.538(6) . ? 
P1 O8 1.553(5) 8_565 ? 
P1 O8 1.553(5) . ? 
P1 Ba 3.645(2) . ? 
P2 O7 1.530(7) 5_566 ? 
P2 O11 1.533(5) 8_575 ? 
P2 O11 1.533(5) . ? 
P2 O2 1.604(7) . ? 
P2 Ba 3.505(3) 2_565 ? 
P3 O12 1.527(7) . ? 
P3 O9 1.539(5) 8 ? 
P3 O9 1.539(5) . ? 
P3 O13 1.591(8) . ? 
P3 Ba 3.637(2) 5_656 ? 
P4 O10 1.540(5) 8_565 ? 
P4 O10 1.540(5) . ? 
P4 O6 1.540(7) . ? 
P4 O4 1.544(6) . ? 
P4 Ba 3.411(2) . ? 
O1 Co2 2.124(5) 8_565 ? 
O4 Co2 2.037(4) 8_565 ? 
O5 P1 1.522(7) 2 ? 
O5 Co1 2.051(4) 8 ? 
O6 Co1 2.188(5) 7_666 ? 
O6 Co1 2.188(5) 2 ? 
O7 P2 1.530(7) 5_566 ? 
O7 Co2 2.126(4) 8_565 ? 
O8 Co2 2.270(4) 7_655 ? 
O8 Ba 3.001(5) . ? 
O9 Co2 2.205(5) 7_655 ? 
O9 Ba 2.996(5) . ? 
O10 Ba 2.790(5) . ? 
O11 Ba 2.875(5) 2_565 ? 
O12 Ba 2.907(7) 5_656 ? 
O13 Ba 2.902(6) 5_656 ? 
Ba O10 2.790(5) 8_565 ? 
Ba O11 2.875(5) 7_655 ? 
Ba O11 2.875(5) 2_564 ? 
Ba O13 2.902(6) 5_656 ? 
Ba O12 2.907(7) 5_656 ? 
Ba O9 2.996(5) 8_565 ? 
Ba O8 3.001(5) 8_565 ? 
Ba P2 3.505(3) 2_564 ? 
 
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 
O10 Co1 O5 97.2(2) . . ? 
O10 Co1 O8 91.99(19) . . ? 
O5 Co1 O8 167.4(2) . . ? 
O10 Co1 O1 95.35(18) . . ? 
O5 Co1 O1 90.2(2) . . ? 
O8 Co1 O1 97.51(18) . . ? 
O10 Co1 O6 168.1(2) . 2_554 ? 
O5 Co1 O6 72.7(2) . 2_554 ? 
O8 Co1 O6 99.0(2) . 2_554 ? 
O1 Co1 O6 78.9(2) . 2_554 ? 
O10 Co1 O9 85.64(18) . . ? 
O5 Co1 O9 96.6(2) . . ? 
O8 Co1 O9 75.45(18) . . ? 
O1 Co1 O9 172.93(18) . . ? 
O6 Co1 O9 101.4(2) 2_554 . ? 
O10 Co1 Ba 47.52(13) . . ? 
O5 Co1 Ba 129.13(19) . . ? 
O8 Co1 Ba 53.50(13) . . ? 
O1 Co1 Ba 122.83(12) . . ? 
O6 Co1 Ba 144.10(18) 2_554 . ? 
O9 Co1 Ba 53.44(12) . . ? 
O11 Co2 O4 168.3(2) . . ? 
O11 Co2 O1 96.29(19) . 8_565 ? 
O4 Co2 O1 79.9(2) . 8_565 ? 
O11 Co2 O7 95.55(19) . . ? 
O4 Co2 O7 73.8(2) . . ? 
O1 Co2 O7 93.0(2) 8_565 . ? 
O11 Co2 O9 89.76(18) . 7_666 ? 
O4 Co2 O9 96.5(2) . 7_666 ? 
O1 Co2 O9 165.84(18) 8_565 7_666 ? 
O7 Co2 O9 99.2(2) . 7_666 ? 
O11 Co2 O8 93.59(18) . 7_666 ? 
O4 Co2 O8 97.69(19) . 7_666 ? 
O1 Co2 O8 94.16(17) 8_565 7_666 ? 
O7 Co2 O8 167.71(18) . 7_666 ? 
O9 Co2 O8 72.63(17) 7_666 7_666 ? 
O11 Co2 Ba 49.70(14) . 2_565 ? 
O4 Co2 Ba 141.27(19) . 2_565 ? 
O1 Co2 Ba 122.63(13) 8_565 2_565 ? 
O7 Co2 Ba 128.94(18) . 2_565 ? 
O9 Co2 Ba 53.47(12) 7_666 2_565 ? 
O8 Co2 Ba 53.58(12) 7_666 2_565 ? 
O5 P1 O3 107.8(4) 2_554 . ? 
O5 P1 O8 109.6(2) 2_554 8_565 ? 
O3 P1 O8 111.4(2) . 8_565 ? 
O5 P1 O8 109.6(2) 2_554 . ? 
O3 P1 O8 111.4(2) . . ? 
O8 P1 O8 107.2(4) 8_565 . ? 
O5 P1 Ba 129.5(3) 2_554 . ? 
O3 P1 Ba 122.8(3) . . ? 
O8 P1 Ba 53.75(19) 8_565 . ? 
O8 P1 Ba 53.75(19) . . ? 
O7 P2 O11 112.8(2) 5_566 8_575 ? 
O7 P2 O11 112.8(2) 5_566 . ? 
O11 P2 O11 106.9(4) 8_575 . ? 
O7 P2 O2 105.2(4) 5_566 . ? 
O11 P2 O2 109.6(2) 8_575 . ? 
O11 P2 O2 109.6(2) . . ? 
O7 P2 Ba 125.0(3) 5_566 2_565 ? 
O11 P2 Ba 53.64(19) 8_575 2_565 ? 
O11 P2 Ba 53.64(19) . 2_565 ? 
O2 P2 Ba 129.8(3) . 2_565 ? 
O12 P3 O9 113.8(2) . 8 ? 
O12 P3 O9 113.8(2) . . ? 
O9 P3 O9 108.5(4) 8 . ? 
O12 P3 O13 100.8(4) . . ? 
O9 P3 O13 109.8(3) 8 . ? 
O9 P3 O13 109.8(3) . . ? 
O12 P3 Ba 50.2(3) . 5_656 ? 
O9 P3 Ba 125.6(2) 8 5_656 ? 
O9 P3 Ba 125.6(2) . 5_656 ? 
O13 P3 Ba 50.6(2) . 5_656 ? 
O10 P4 O10 106.8(4) 8_565 . ? 
O10 P4 O6 112.1(2) 8_565 . ? 
O10 P4 O6 112.1(2) . . ? 
O10 P4 O4 110.8(2) 8_565 . ? 
O10 P4 O4 110.8(2) . . ? 
O6 P4 O4 104.3(4) . . ? 
O10 P4 Ba 53.70(18) 8_565 . ? 
O10 P4 Ba 53.70(18) . . ? 
O6 P4 Ba 122.5(3) . . ? 
O4 P4 Ba 133.2(3) . . ? 
Co2 O1 Co1 116.6(2) 8_565 . ? 
P4 O4 Co2 124.80(19) . . ? 
P4 O4 Co2 124.80(19) . 8_565 ? 
Co2 O4 Co2 101.7(3) . 8_565 ? 
P1 O5 Co1 128.56(15) 2 8 ? 
P1 O5 Co1 128.56(15) 2 . ? 
Co1 O5 Co1 102.6(3) 8 . ? 
P4 O6 Co1 119.6(2) . 7_666 ? 
P4 O6 Co1 119.6(2) . 2 ? 
Co1 O6 Co1 94.0(3) 7_666 2 ? 
P2 O7 Co2 130.89(15) 5_566 . ? 
P2 O7 Co2 130.89(15) 5_566 8_565 ? 
Co2 O7 Co2 95.9(3) . 8_565 ? 
P1 O8 Co1 126.7(3) . . ? 
P1 O8 Co2 134.5(3) . 7_655 ? 
Co1 O8 Co2 96.38(18) . 7_655 ? 
P1 O8 Ba 101.6(2) . . ? 
Co1 O8 Ba 92.44(16) . . ? 
Co2 O8 Ba 88.91(14) 7_655 . ? 
P3 O9 Co2 120.0(3) . 7_655 ? 
P3 O9 Co1 121.6(3) . . ? 
Co2 O9 Co1 94.09(19) 7_655 . ? 
P3 O9 Ba 131.3(3) . . ? 
Co2 O9 Ba 90.27(15) 7_655 . ? 
Co1 O9 Ba 89.67(15) . . ? 
P4 O10 Co1 132.2(3) . . ? 
P4 O10 Ba 99.9(2) . . ? 
Co1 O10 Ba 99.71(18) . . ? 
P2 O11 Co2 134.4(3) . . ? 
P2 O11 Ba 100.9(2) . 2_565 ? 
Co2 O11 Ba 98.51(17) . 2_565 ? 
P3 O12 Ba 106.0(4) . 5_656 ? 
P3 O13 Ba 104.3(3) . 5_656 ? 
O10 Ba O10 52.62(18) . 8_565 ? 
O10 Ba O11 115.86(13) . 7_655 ? 
O10 Ba O11 144.66(14) 8_565 7_655 ? 
O10 Ba O11 144.66(14) . 2_564 ? 
O10 Ba O11 115.86(13) 8_565 2_564 ? 
O11 Ba O11 50.70(18) 7_655 2_564 ? 
O10 Ba O13 125.85(15) . 5_656 ? 
O10 Ba O13 125.85(15) 8_565 5_656 ? 
O11 Ba O13 88.74(16) 7_655 5_656 ? 
O11 Ba O13 88.74(16) 2_564 5_656 ? 
O10 Ba O12 82.76(15) . 5_656 ? 
O10 Ba O12 82.76(15) 8_565 5_656 ? 
O11 Ba O12 131.77(15) 7_655 5_656 ? 
O11 Ba O12 131.77(15) 2_564 5_656 ? 
O13 Ba O12 48.9(2) 5_656 5_656 ? 
O10 Ba O9 60.43(13) . . ? 
O10 Ba O9 111.74(13) 8_565 . ? 
O11 Ba O9 60.55(13) 7_655 . ? 
O11 Ba O9 110.06(14) 2_564 . ? 
O13 Ba O9 101.90(9) 5_656 . ? 
O12 Ba O9 101.62(10) 5_656 . ? 
O10 Ba O9 111.74(13) . 8_565 ? 
O10 Ba O9 60.43(13) 8_565 8_565 ? 
O11 Ba O9 110.06(14) 7_655 8_565 ? 
O11 Ba O9 60.55(13) 2_564 8_565 ? 
O13 Ba O9 101.90(9) 5_656 8_565 ? 
O12 Ba O9 101.62(10) 5_656 8_565 ? 
O9 Ba O9 154.12(19) . 8_565 ? 
O10 Ba O8 61.74(14) . . ? 
O10 Ba O8 84.00(13) 8_565 . ? 
O11 Ba O8 63.85(13) 7_655 . ? 
O11 Ba O8 85.16(13) 2_564 . ? 
O13 Ba O8 148.67(12) 5_656 . ? 
O12 Ba O8 142.79(13) 5_656 . ? 
O9 Ba O8 52.48(13) . . ? 
O9 Ba O8 101.68(13) 8_565 . ? 
O10 Ba O8 84.00(13) . 8_565 ? 
O10 Ba O8 61.74(13) 8_565 8_565 ? 
O11 Ba O8 85.16(13) 7_655 8_565 ? 
O11 Ba O8 63.85(12) 2_564 8_565 ? 
O13 Ba O8 148.67(12) 5_656 8_565 ? 
O12 Ba O8 142.79(13) 5_656 8_565 ? 
O9 Ba O8 101.68(13) . 8_565 ? 
O9 Ba O8 52.48(13) 8_565 8_565 ? 
O8 Ba O8 49.21(17) . 8_565 ? 
O10 Ba P4 26.41(9) . . ? 
O10 Ba P4 26.41(9) 8_565 . ? 
O11 Ba P4 136.24(10) 7_655 . ? 
O11 Ba P4 136.24(10) 2_564 . ? 
O13 Ba P4 128.34(15) 5_656 . ? 
O12 Ba P4 79.46(14) 5_656 . ? 
O9 Ba P4 86.59(9) . . ? 
O9 Ba P4 86.59(9) 8_565 . ? 
O8 Ba P4 73.40(10) . . ? 
O8 Ba P4 73.40(10) 8_565 . ? 
O10 Ba P2 135.38(10) . 2_564 ? 
O10 Ba P2 135.38(10) 8_565 2_564 ? 
O11 Ba P2 25.42(9) 7_655 2_564 ? 
O11 Ba P2 25.42(9) 2_564 2_564 ? 
O13 Ba P2 86.64(15) 5_656 2_564 ? 
O12 Ba P2 135.52(14) 5_656 2_564 ? 
O9 Ba P2 85.69(10) . 2_564 ? 
O9 Ba P2 85.69(10) 8_565 2_564 ? 
O8 Ba P2 74.88(10) . 2_564 ? 
O8 Ba P2 74.88(10) 8_565 2_564 ? 
P4 Ba P2 145.02(6) . 2_564 ? 
 
_diffrn_measured_fraction_theta_max    0.980 
_diffrn_reflns_theta_full              27.46 
_diffrn_measured_fraction_theta_full   0.980 
_refine_diff_density_max    1.581 
_refine_diff_density_min   -2.042 
_refine_diff_density_rms    0.257 
