 
data_bart2 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'H2 Fe Ge3 O10 Pb' 
_chemical_formula_weight          642.83 
 
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' 
 'Fe'  'Fe'   0.3463   0.8444 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Ge'  'Ge'   0.1547   1.8001 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Pb'  'Pb'  -3.3944  10.1111 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            ? 
_symmetry_space_group_name_H-M    ? 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, y+1/2, -z' 
 '-x, -y, -z' 
 'x, -y-1/2, z' 
 
_cell_length_a                    5.8279(2) 
_cell_length_b                    13.6150(4) 
_cell_length_c                    6.3097(2) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  127.314(2) 
_cell_angle_gamma                 90.00 
_cell_volume                      398.18(2) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
 
_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           ? 
_exptl_crystal_size_mid           ? 
_exptl_crystal_size_min           ? 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     5.362 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              572 
_exptl_absorpt_coefficient_mu     34.083 
_exptl_absorpt_correction_type    ? 
_exptl_absorpt_correction_T_min   ? 
_exptl_absorpt_correction_T_max   ? 
_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   ? 
_diffrn_measurement_method        ? 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             8260 
_diffrn_reflns_av_R_equivalents   0.0340 
_diffrn_reflns_av_sigmaI/netI     0.0328 
_diffrn_reflns_limit_h_min        -9 
_diffrn_reflns_limit_h_max        9 
_diffrn_reflns_limit_k_min        -19 
_diffrn_reflns_limit_k_max        21 
_diffrn_reflns_limit_l_min        -10 
_diffrn_reflns_limit_l_max        10 
_diffrn_reflns_theta_min          2.99 
_diffrn_reflns_theta_max          35.05 
_reflns_number_total              1797 
_reflns_number_gt                 1593 
_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)+(0.0178P)²+0.0000P] where P=(Fo²+2Fc²)/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      SHELXL 
_refine_ls_extinction_coef        0.0024(2) 
_refine_ls_extinction_expression 
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^' 
_refine_ls_number_reflns          1797 
_refine_ls_number_parameters      83 
_refine_ls_number_restraints      2 
_refine_ls_R_factor_all           0.0283 
_refine_ls_R_factor_gt            0.0230 
_refine_ls_wR_factor_ref          0.0441 
_refine_ls_wR_factor_gt           0.0430 
_refine_ls_goodness_of_fit_ref    1.029 
_refine_ls_restrained_S_all       1.031 
_refine_ls_shift/su_max           0.004 
_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_symetry_multiplicity 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
Pb Pb 0.32487(4) 0.7500 0.67674(3) 0.01488(6) Uani 1 2 d S . . 
Fe Fe 0.5000 0.0000 0.0000 0.00769(12) Uani 1 2 d S . . 
Ge1 Ge 0.5000 0.0000 0.5000 0.00773(9) Uani 1 2 d S . . 
Ge2 Ge 0.96137(6) 0.12998(3) 0.99604(6) 0.00688(7) Uani 1 1 d . . . 
O1 O 0.9013(7) 0.7500 0.9350(7) 0.0157(7) Uani 1 2 d S . . 
O2 O 0.7512(5) 0.11151(19) 0.6545(4) 0.0128(5) Uani 1 1 d . . . 
O3 O 0.7821(5) 0.38529(19) 0.1337(4) 0.0114(4) Uani 1 1 d . . . 
O4 O 0.2837(4) 0.06250(19) 0.1610(4) 0.0088(4) Uani 1 1 d . . . 
O5H O 0.2893(5) 0.0524(2) 0.6036(4) 0.0116(5) Uani 1 1 d D . . 
O6W O 0.7617(9) 0.7500 0.3216(8) 0.0239(8) Uani 1 2 d SD . . 
H1 H 0.144(8) 0.077(4) 0.497(8) 0.030 Uiso 1 1 d D . . 
H2 H 0.712(9) 0.799(3) 0.356(9) 0.030 Uiso 1 1 d 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 
Pb 0.01415(8) 0.01555(11) 0.01618(8) 0.000 0.00984(7) 0.000 
Fe 0.0082(3) 0.0087(4) 0.0066(2) -0.00110(19) 0.0047(2) -0.0016(2) 
Ge1 0.00759(18) 0.0100(3) 0.00554(16) 0.00176(14) 0.00397(15) 0.00282(14) 
Ge2 0.00581(13) 0.00720(18) 0.00654(12) 0.00011(10) 0.00318(10) 0.00054(10) 
O1 0.0105(14) 0.0064(19) 0.0266(17) 0.000 0.0093(13) 0.000 
O2 0.0120(10) 0.0146(14) 0.0084(8) -0.0001(8) 0.0044(8) -0.0031(8) 
O3 0.0129(10) 0.0117(13) 0.0132(9) 0.0042(8) 0.0097(8) 0.0040(8) 
O4 0.0083(9) 0.0119(12) 0.0063(8) 0.0032(8) 0.0044(7) 0.0053(7) 
O5H 0.0087(9) 0.0179(15) 0.0074(8) 0.0017(8) 0.0046(8) 0.0037(8) 
O6W 0.028(2) 0.012(2) 0.033(2) 0.000 0.0190(17) 0.000 
 
_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 
Pb O3 2.473(2) 2_656 ? 
Pb O3 2.473(2) 3_666 ? 
Pb O6W 2.623(4) 1_455 ? 
Pb O2 2.645(2) 2_656 ? 
Pb O2 2.645(2) 3_666 ? 
Pb O1 2.703(3) . ? 
Fe O3 2.042(2) 4_565 ? 
Fe O3 2.042(2) 2_645 ? 
Fe O5H 2.133(2) 1_554 ? 
Fe O5H 2.133(2) 3_656 ? 
Fe O4 2.213(2) 3_655 ? 
Fe O4 2.213(2) . ? 
Ge1 O5H 1.849(2) 3_656 ? 
Ge1 O5H 1.849(2) . ? 
Ge1 O4 1.902(2) 3_656 ? 
Ge1 O4 1.902(2) . ? 
Ge1 O2 1.915(2) . ? 
Ge1 O2 1.915(2) 3_656 ? 
Ge2 O3 1.729(2) 4_566 ? 
Ge2 O2 1.734(2) . ? 
Ge2 O1 1.7544(12) 3_767 ? 
Ge2 O4 1.757(2) 1_656 ? 
O1 Ge2 1.7544(12) 3_767 ? 
O1 Ge2 1.7544(12) 2_757 ? 
O2 Pb 2.645(2) 3_666 ? 
O3 Ge2 1.729(2) 4_564 ? 
O3 Fe 2.042(2) 2_655 ? 
O3 Pb 2.473(2) 3_666 ? 
O4 Ge2 1.757(2) 1_454 ? 
O5H Fe 2.133(2) 1_556 ? 
O5H H1 0.77(4) . ? 
O6W Pb 2.623(4) 1_655 ? 
O6W H2 0.81(4) . ? 
 
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 Pb O3 96.29(11) 2_656 3_666 ? 
O3 Pb O6W 82.03(8) 2_656 1_455 ? 
O3 Pb O6W 82.03(8) 3_666 1_455 ? 
O3 Pb O2 160.47(7) 2_656 2_656 ? 
O3 Pb O2 83.14(8) 3_666 2_656 ? 
O6W Pb O2 78.55(8) 1_455 2_656 ? 
O3 Pb O2 83.14(8) 2_656 3_666 ? 
O3 Pb O2 160.47(7) 3_666 3_666 ? 
O6W Pb O2 78.55(8) 1_455 3_666 ? 
O2 Pb O2 90.93(11) 2_656 3_666 ? 
O3 Pb O1 107.09(7) 2_656 . ? 
O3 Pb O1 107.09(7) 3_666 . ? 
O6W Pb O1 165.86(12) 1_455 . ? 
O2 Pb O1 91.61(7) 2_656 . ? 
O2 Pb O1 91.61(7) 3_666 . ? 
O3 Fe O3 180.00(9) 4_565 2_645 ? 
O3 Fe O5H 88.59(9) 4_565 1_554 ? 
O3 Fe O5H 91.41(9) 2_645 1_554 ? 
O3 Fe O5H 91.41(9) 4_565 3_656 ? 
O3 Fe O5H 88.59(9) 2_645 3_656 ? 
O5H Fe O5H 180.00(14) 1_554 3_656 ? 
O3 Fe O4 86.79(9) 4_565 3_655 ? 
O3 Fe O4 93.21(9) 2_645 3_655 ? 
O5H Fe O4 70.95(8) 1_554 3_655 ? 
O5H Fe O4 109.05(8) 3_656 3_655 ? 
O3 Fe O4 93.21(9) 4_565 . ? 
O3 Fe O4 86.79(9) 2_645 . ? 
O5H Fe O4 109.05(8) 1_554 . ? 
O5H Fe O4 70.95(8) 3_656 . ? 
O4 Fe O4 180.00(13) 3_655 . ? 
O5H Ge1 O5H 180.0 3_656 . ? 
O5H Ge1 O4 95.48(9) 3_656 3_656 ? 
O5H Ge1 O4 84.52(9) . 3_656 ? 
O5H Ge1 O4 84.52(9) 3_656 . ? 
O5H Ge1 O4 95.48(9) . . ? 
O4 Ge1 O4 180.00(10) 3_656 . ? 
O5H Ge1 O2 91.13(11) 3_656 . ? 
O5H Ge1 O2 88.87(11) . . ? 
O4 Ge1 O2 90.07(10) 3_656 . ? 
O4 Ge1 O2 89.93(10) . . ? 
O5H Ge1 O2 88.87(11) 3_656 3_656 ? 
O5H Ge1 O2 91.13(11) . 3_656 ? 
O4 Ge1 O2 89.93(10) 3_656 3_656 ? 
O4 Ge1 O2 90.07(10) . 3_656 ? 
O2 Ge1 O2 180.00(10) . 3_656 ? 
O3 Ge2 O2 114.84(11) 4_566 . ? 
O3 Ge2 O1 108.13(14) 4_566 3_767 ? 
O2 Ge2 O1 108.40(14) . 3_767 ? 
O3 Ge2 O4 113.22(10) 4_566 1_656 ? 
O2 Ge2 O4 110.89(11) . 1_656 ? 
O1 Ge2 O4 100.19(13) 3_767 1_656 ? 
Ge2 O1 Ge2 137.32(19) 3_767 2_757 ? 
Ge2 O1 Pb 111.28(10) 3_767 . ? 
Ge2 O1 Pb 111.28(10) 2_757 . ? 
Ge2 O2 Ge1 119.58(13) . . ? 
Ge2 O2 Pb 122.17(12) . 3_666 ? 
Ge1 O2 Pb 116.90(9) . 3_666 ? 
Ge2 O3 Fe 117.68(12) 4_564 2_655 ? 
Ge2 O3 Pb 124.03(13) 4_564 3_666 ? 
Fe O3 Pb 113.18(9) 2_655 3_666 ? 
Ge2 O4 Ge1 129.93(11) 1_454 . ? 
Ge2 O4 Fe 129.13(10) 1_454 . ? 
Ge1 O4 Fe 99.83(9) . . ? 
Ge1 O5H Fe 104.58(10) . 1_556 ? 
Ge1 O5H H1 118(4) . . ? 
Fe O5H H1 136(4) 1_556 . ? 
Pb O6W H2 104(3) 1_655 . ? 
 
loop_ 
 _geom_hbond_atom_site_label_D 
 _geom_hbond_atom_site_label_H 
 _geom_hbond_atom_site_label_A 
 _geom_hbond_distance_DH 
 _geom_hbond_distance_HA 
 _geom_hbond_distance_DA 
 _geom_hbond_angle_DHA 
 _geom_hbond_site_symmetry_A 
O5H H1 O3  0.77(4) 2.02(4) 2.761(3) 160(5) 4_465 
O6W H2 O5H  0.81(4) 2.03(4) 2.777(3) 152(5) 3_666 
 
_diffrn_measured_fraction_theta_max    0.986 
_diffrn_reflns_theta_full              35.05 
_diffrn_measured_fraction_theta_full   0.986 
_refine_diff_density_max    1.953 
_refine_diff_density_min   -1.194 
_refine_diff_density_rms    0.256 
