# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_2

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'Ba O6 Pb Si2'
_chemical_formula_weight         496.71

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'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ba Ba -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'Cmcm '

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x, y, -z+1/2'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x, y, -z-1/2'
'x, -y, z-1/2'
'-x, y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z-1/2'
'x+1/2, -y+1/2, z-1/2'
'-x+1/2, y+1/2, z'

_cell_length_a                   5.5092(17)
_cell_length_b                   15.450(5)
_cell_length_c                   7.287(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     620.2(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    817
_cell_measurement_theta_min      3.84
_cell_measurement_theta_max      27.55

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.096
_exptl_crystal_size_mid          0.091
_exptl_crystal_size_min          0.054
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    5.319
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             856
_exptl_absorpt_coefficient_mu    33.771
_exptl_absorpt_correction_type   Numerical
_exptl_absorpt_correction_T_min  0.5361
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   Face-indexed

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            1879
_diffrn_reflns_av_R_equivalents  0.0334
_diffrn_reflns_av_sigmaI/netI    0.0284
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.64
_diffrn_reflns_theta_max         27.55
_reflns_number_total             427
_reflns_number_gt                385
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0194P)²+4.0096P] 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       0.00067(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         427
_refine_ls_number_parameters     33
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0238
_refine_ls_R_factor_gt           0.0202
_refine_ls_wR_factor_ref         0.0494
_refine_ls_wR_factor_gt          0.0474
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_restrained_S_all      1.067
_refine_ls_shift/su_max          0.001
_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
Pb1 Pb 0.5000 0.57367(2) 0.2500 0.01123(19) Uani 1 4 d S . .
Ba1 Ba 0.0000 0.78078(4) 0.2500 0.0103(2) Uani 1 4 d S . .
Si1 Si 1.0000 0.60364(13) 0.5303(3) 0.0089(4) Uani 1 2 d S . .
O1 O 1.0000 0.6232(7) 0.7500 0.034(2) Uani 1 4 d S . .
O2 O 0.7578(6) 0.6466(2) 0.4494(5) 0.0162(8) Uani 1 1 d . . .
O3 O 1.0000 0.5000 0.5000 0.0239(19) Uani 1 4 d SU . .


_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
Pb1 O2 2.324(4) . ?
Pb1 O2 2.324(4) 3_655 ?
Pb1 O2 2.324(4) 12_655 ?
Pb1 O2 2.324(4) 10_556 ?
Ba1 O2 2.841(4) 8_466 ?
Ba1 O2 2.841(4) 6_564 ?
Ba1 O2 2.841(4) 13_566 ?
Ba1 O2 2.841(4) 15_465 ?
Ba1 O2 2.861(4) 10_456 ?
Ba1 O2 2.861(4) 3_655 ?
Ba1 O2 2.861(4) 1_455 ?
Ba1 O2 2.861(4) 12_655 ?
Ba1 O1 3.129(5) 13_666 ?
Ba1 O1 3.129(5) 13_566 ?
Si1 O2 1.603(4) 12_755 ?
Si1 O2 1.603(4) . ?
Si1 O3 1.616(2) . ?
Si1 O1 1.629(3) . ?
O1 Si1 1.629(3) 10_557 ?
O1 Ba1 3.129(5) 13_666 ?
O1 Ba1 3.129(5) 13_566 ?
O2 Ba1 2.841(4) 13_566 ?
O2 Ba1 2.861(4) 1_655 ?
O3 Si1 1.616(2) 9_766 ?

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 Pb1 O2 121.96(18) . 3_655 ?
O2 Pb1 O2 75.36(18) . 12_655 ?
O2 Pb1 O2 77.41(19) 3_655 12_655 ?
O2 Pb1 O2 77.4(2) . 10_556 ?
O2 Pb1 O2 75.36(18) 3_655 10_556 ?
O2 Pb1 O2 121.96(18) 12_655 10_556 ?
O2 Pb1 Ba1 39.96(10) . 1_655 ?
O2 Pb1 Ba1 91.78(9) 3_655 1_655 ?
O2 Pb1 Ba1 91.78(9) 12_655 1_655 ?
O2 Pb1 Ba1 39.96(10) 10_556 1_655 ?
O2 Pb1 Ba1 91.78(9) . . ?
O2 Pb1 Ba1 39.96(10) 3_655 . ?
O2 Pb1 Ba1 39.96(10) 12_655 . ?
O2 Pb1 Ba1 91.78(9) 10_556 . ?
Ba1 Pb1 Ba1 81.45(3) 1_655 . ?
O2 Ba1 O2 133.50(15) 8_466 6_564 ?
O2 Ba1 O2 59.99(14) 8_466 13_566 ?
O2 Ba1 O2 100.86(15) 6_564 13_566 ?
O2 Ba1 O2 100.86(15) 8_466 15_465 ?
O2 Ba1 O2 59.99(14) 6_564 15_465 ?
O2 Ba1 O2 133.50(15) 13_566 15_465 ?
O2 Ba1 O2 155.58(10) 8_466 10_456 ?
O2 Ba1 O2 70.20(12) 6_564 10_456 ?
O2 Ba1 O2 116.38(7) 13_566 10_456 ?
O2 Ba1 O2 97.33(8) 15_465 10_456 ?
O2 Ba1 O2 116.38(7) 8_466 3_655 ?
O2 Ba1 O2 97.33(8) 6_564 3_655 ?
O2 Ba1 O2 155.58(10) 13_566 3_655 ?
O2 Ba1 O2 70.20(12) 15_465 3_655 ?
O2 Ba1 O2 55.59(14) 10_456 3_655 ?
O2 Ba1 O2 97.33(8) 8_466 1_455 ?
O2 Ba1 O2 116.38(7) 6_564 1_455 ?
O2 Ba1 O2 70.20(12) 13_566 1_455 ?
O2 Ba1 O2 155.58(10) 15_465 1_455 ?
O2 Ba1 O2 61.04(15) 10_456 1_455 ?
O2 Ba1 O2 87.17(15) 3_655 1_455 ?
O2 Ba1 O2 70.20(12) 8_466 12_655 ?
O2 Ba1 O2 155.58(10) 6_564 12_655 ?
O2 Ba1 O2 97.33(8) 13_566 12_655 ?
O2 Ba1 O2 116.38(7) 15_465 12_655 ?
O2 Ba1 O2 87.17(15) 10_456 12_655 ?
O2 Ba1 O2 61.04(15) 3_655 12_655 ?
O2 Ba1 O2 55.59(14) 1_455 12_655 ?
O2 Ba1 O1 51.15(8) 8_466 13_666 ?
O2 Ba1 O1 104.65(13) 6_564 13_666 ?
O2 Ba1 O1 104.65(13) 13_566 13_666 ?
O2 Ba1 O1 51.15(8) 15_465 13_666 ?
O2 Ba1 O1 138.94(13) 10_456 13_666 ?
O2 Ba1 O1 86.16(16) 3_655 13_666 ?
O2 Ba1 O1 138.94(13) 1_455 13_666 ?
O2 Ba1 O1 86.16(16) 12_655 13_666 ?
O2 Ba1 O1 104.65(13) 8_466 13_566 ?
O2 Ba1 O1 51.15(8) 6_564 13_566 ?
O2 Ba1 O1 51.15(8) 13_566 13_566 ?
O2 Ba1 O1 104.65(13) 15_465 13_566 ?
O2 Ba1 O1 86.16(16) 10_456 13_566 ?
O2 Ba1 O1 138.94(13) 3_655 13_566 ?
O2 Ba1 O1 86.16(16) 1_455 13_566 ?
O2 Ba1 O1 138.94(13) 12_655 13_566 ?
O1 Ba1 O1 123.4(3) 13_666 13_566 ?
O2 Ba1 Si1 141.02(8) 8_466 10_456 ?
O2 Ba1 Si1 81.68(8) 6_564 10_456 ?
O2 Ba1 Si1 141.02(8) 13_566 10_456 ?
O2 Ba1 Si1 81.68(8) 15_465 10_456 ?
O2 Ba1 Si1 27.84(7) 10_456 10_456 ?
O2 Ba1 Si1 27.84(7) 3_655 10_456 ?
O2 Ba1 Si1 73.93(8) 1_455 10_456 ?
O2 Ba1 Si1 73.93(8) 12_655 10_456 ?
O1 Ba1 Si1 112.34(13) 13_666 10_456 ?
O1 Ba1 Si1 112.34(13) 13_566 10_456 ?
O2 Ba1 Si1 81.68(8) 8_466 1_455 ?
O2 Ba1 Si1 141.02(8) 6_564 1_455 ?
O2 Ba1 Si1 81.68(8) 13_566 1_455 ?
O2 Ba1 Si1 141.02(8) 15_465 1_455 ?
O2 Ba1 Si1 73.93(8) 10_456 1_455 ?
O2 Ba1 Si1 73.93(8) 3_655 1_455 ?
O2 Ba1 Si1 27.84(7) 1_455 1_455 ?
O2 Ba1 Si1 27.84(7) 12_655 1_455 ?
O1 Ba1 Si1 112.34(13) 13_666 1_455 ?
O1 Ba1 Si1 112.34(13) 13_566 1_455 ?
Si1 Ba1 Si1 73.47(7) 10_456 1_455 ?
O2 Si1 O2 112.7(3) 12_755 . ?
O2 Si1 O3 111.12(15) 12_755 . ?
O2 Si1 O3 111.12(15) . . ?
O2 Si1 O1 106.5(2) 12_755 . ?
O2 Si1 O1 106.5(2) . . ?
O3 Si1 O1 108.5(4) . . ?
O2 Si1 Ba1 56.49(15) 12_755 1_655 ?
O2 Si1 Ba1 56.49(15) . 1_655 ?
O3 Si1 Ba1 135.42(10) . 1_655 ?
O1 Si1 Ba1 116.1(4) . 1_655 ?
O2 Si1 Ba1 47.98(15) 12_755 13_666 ?
O2 Si1 Ba1 125.90(16) . 13_666 ?
O3 Si1 Ba1 122.97(5) . 13_666 ?
O1 Si1 Ba1 58.58(17) . 13_666 ?
Ba1 Si1 Ba1 82.55(4) 1_655 13_666 ?
O2 Si1 Ba1 125.90(16) 12_755 13_566 ?
O2 Si1 Ba1 47.98(15) . 13_566 ?
O3 Si1 Ba1 122.97(5) . 13_566 ?
O1 Si1 Ba1 58.58(17) . 13_566 ?
Ba1 Si1 Ba1 82.55(4) 1_655 13_566 ?
Ba1 Si1 Ba1 97.91(5) 13_666 13_566 ?
Si1 O1 Si1 158.6(7) . 10_557 ?
Si1 O1 Ba1 95.04(14) . 13_666 ?
Si1 O1 Ba1 95.04(14) 10_557 13_666 ?
Si1 O1 Ba1 95.04(14) . 13_566 ?
Si1 O1 Ba1 95.04(14) 10_557 13_566 ?
Ba1 O1 Ba1 123.4(3) 13_666 13_566 ?
Si1 O2 Pb1 122.5(2) . . ?
Si1 O2 Ba1 107.24(19) . 13_566 ?
Pb1 O2 Ba1 111.59(13) . 13_566 ?
Si1 O2 Ba1 95.67(16) . 1_655 ?
Pb1 O2 Ba1 108.59(15) . 1_655 ?
Ba1 O2 Ba1 109.80(12) 13_566 1_655 ?
Si1 O3 Si1 180.00(2) 9_766 . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.55
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.413
_refine_diff_density_min         -1.506
_refine_diff_density_rms         0.245
_database_code_depnum_ccdc_archive 'CCDC 969031'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_2

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'Ba2 O10 Pb S Si2'
_chemical_formula_weight         730.11

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'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ba Ba -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   7.2520(11)
_cell_length_b                   5.4841(8)
_cell_length_c                   24.352(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     968.5(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1054
_cell_measurement_theta_min      3.27
_cell_measurement_theta_max      26.80

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.105
_exptl_crystal_size_mid          0.077
_exptl_crystal_size_min          0.039
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    5.007
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1272
_exptl_absorpt_coefficient_mu    25.886
_exptl_absorpt_correction_type   Numerical
_exptl_absorpt_correction_T_min  0.6921
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   Face-indexed

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5705
_diffrn_reflns_av_R_equivalents  0.0547
_diffrn_reflns_av_sigmaI/netI    0.0454
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         2.93
_diffrn_reflns_theta_max         27.51
_reflns_number_total             1229
_reflns_number_gt                986
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0224P)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       0.00073(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1229
_refine_ls_number_parameters     89
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0440
_refine_ls_R_factor_gt           0.0297
_refine_ls_wR_factor_ref         0.0608
_refine_ls_wR_factor_gt          0.0566
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.038
_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
Pb1 Pb 0.64505(6) 1.2500 0.202712(18) 0.01217(14) Uani 1 2 d S . .
Ba1 Ba 1.13906(10) 1.2500 0.10988(3) 0.01221(18) Uani 1 2 d S . .
Ba2 Ba 0.66073(9) 0.7500 0.07098(3) 0.01047(17) Uani 1 2 d S . .
S1 S 1.2093(4) 0.7500 0.01407(12) 0.0105(6) Uani 1 2 d S . .
Si1 Si 0.8713(4) 0.7500 0.31774(13) 0.0100(6) Uani 1 2 d S . .
Si2 Si 0.9343(4) 0.7500 0.18640(12) 0.0092(6) Uani 1 2 d S . .
O1 O 0.8508(8) 0.9901(9) 0.1593(2) 0.0189(13) Uani 1 1 d . . .
O2 O 1.3160(7) 0.9682(9) 0.0296(2) 0.0150(12) Uani 1 1 d . . .
O3 O 0.6539(12) 0.7500 0.3264(4) 0.041(3) Uani 1 2 d SU . .
O4 O 1.1859(11) 0.7500 -0.0460(3) 0.0206(19) Uani 1 2 d S . .
O5 O 1.0341(12) 0.7500 0.0425(4) 0.025(2) Uani 1 2 d S . .
O6 O 0.9491(8) 0.9928(8) 0.3456(2) 0.0188(13) Uani 1 1 d U . .
O7 O 0.9122(11) 0.7500 0.2523(3) 0.023(2) Uani 1 2 d SU . .


_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
Pb1 O1 2.319(5) . ?
Pb1 O1 2.319(5) 7_585 ?
Pb1 O6 2.323(5) 6_556 ?
Pb1 O6 2.323(5) 4_475 ?
Ba1 O1 2.801(6) . ?
Ba1 O1 2.801(6) 7_585 ?
Ba1 O2 2.803(5) . ?
Ba1 O2 2.803(5) 7_585 ?
Ba1 O4 2.823(8) 5_775 ?
Ba1 O6 2.867(6) 4_575 ?
Ba1 O6 2.867(6) 6_656 ?
Ba1 O3 3.153(5) 6_666 ?
Ba1 O3 3.153(5) 6_656 ?
Ba1 O5 3.285(5) . ?
Ba1 O5 3.285(5) 1_565 ?
Ba2 O5 2.795(8) . ?
Ba2 O6 2.873(6) 6_556 ?
Ba2 O6 2.873(6) 4_465 ?
Ba2 O1 2.874(6) . ?
Ba2 O1 2.874(6) 7_575 ?
Ba2 O2 2.901(5) 3_745 ?
Ba2 O2 2.901(5) 5_775 ?
Ba2 O2 2.949(5) 7_475 ?
Ba2 O2 2.949(5) 1_455 ?
Ba2 O4 3.021(3) 5_775 ?
Ba2 O4 3.021(3) 5_765 ?
S1 O5 1.447(8) . ?
S1 O4 1.473(9) . ?
S1 O2 1.475(5) . ?
S1 O2 1.475(5) 7_575 ?
Si1 O3 1.590(9) . ?
Si1 O6 1.598(5) . ?
Si1 O6 1.598(5) 7_575 ?
Si1 O7 1.621(9) . ?
Si2 O1 1.593(5) 7_575 ?
Si2 O1 1.593(5) . ?
Si2 O7 1.612(9) . ?
Si2 O3 1.623(9) 6_656 ?
O2 Ba2 2.901(5) 5_775 ?
O2 Ba2 2.949(5) 1_655 ?
O3 Si2 1.623(9) 6_556 ?
O3 Ba1 3.153(5) 6_556 ?
O3 Ba1 3.153(5) 6_546 ?
O4 Ba1 2.823(8) 5_775 ?
O4 Ba2 3.021(3) 5_775 ?
O4 Ba2 3.021(3) 5_765 ?
O5 Ba1 3.285(5) 1_545 ?
O6 Pb1 2.323(5) 6_656 ?
O6 Ba1 2.867(6) 6_556 ?
O6 Ba2 2.873(6) 6_656 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Pb1 O1 75.9(3) . 7_585 ?
O1 Pb1 O6 77.8(2) . 6_556 ?
O1 Pb1 O6 122.4(2) 7_585 6_556 ?
O1 Pb1 O6 122.4(2) . 4_475 ?
O1 Pb1 O6 77.8(2) 7_585 4_475 ?
O6 Pb1 O6 74.8(3) 6_556 4_475 ?
O1 Pb1 Ba2 92.02(14) . 1_565 ?
O1 Pb1 Ba2 40.26(15) 7_585 1_565 ?
O6 Pb1 Ba2 91.48(13) 6_556 1_565 ?
O6 Pb1 Ba2 40.26(15) 4_475 1_565 ?
O1 Ba1 O1 61.2(2) . 7_585 ?
O1 Ba1 O2 111.14(15) . . ?
O1 Ba1 O2 157.17(16) 7_585 . ?
O1 Ba1 O2 157.17(16) . 7_585 ?
O1 Ba1 O2 111.14(15) 7_585 7_585 ?
O2 Ba1 O2 66.9(2) . 7_585 ?
O1 Ba1 O4 67.28(18) . 5_775 ?
O1 Ba1 O4 67.28(18) 7_585 5_775 ?
O2 Ba1 O4 89.89(18) . 5_775 ?
O2 Ba1 O4 89.89(18) 7_585 5_775 ?
O1 Ba1 O6 132.31(17) . 4_575 ?
O1 Ba1 O6 99.94(15) 7_585 4_575 ?
O2 Ba1 O6 100.12(15) . 4_575 ?
O2 Ba1 O6 68.48(16) 7_585 4_575 ?
O4 Ba1 O6 149.63(11) 5_775 4_575 ?
O1 Ba1 O6 99.94(15) . 6_656 ?
O1 Ba1 O6 132.31(17) 7_585 6_656 ?
O2 Ba1 O6 68.48(16) . 6_656 ?
O2 Ba1 O6 100.12(15) 7_585 6_656 ?
O4 Ba1 O6 149.63(11) 5_775 6_656 ?
O6 Ba1 O6 58.94(19) 4_575 6_656 ?
O1 Ba1 O3 104.9(2) . 6_666 ?
O1 Ba1 O3 51.1(2) 7_585 6_666 ?
O2 Ba1 O3 143.8(2) . 6_666 ?
O2 Ba1 O3 81.3(2) 7_585 6_666 ?
O4 Ba1 O3 107.44(17) 5_775 6_666 ?
O6 Ba1 O3 50.2(2) 4_575 6_666 ?
O6 Ba1 O3 102.41(19) 6_656 6_666 ?
O1 Ba1 O3 51.1(2) . 6_656 ?
O1 Ba1 O3 104.9(2) 7_585 6_656 ?
O2 Ba1 O3 81.3(2) . 6_656 ?
O2 Ba1 O3 143.8(2) 7_585 6_656 ?
O4 Ba1 O3 107.44(17) 5_775 6_656 ?
O6 Ba1 O3 102.41(19) 4_575 6_656 ?
O6 Ba1 O3 50.2(2) 6_656 6_656 ?
O3 Ba1 O3 120.8(3) 6_666 6_656 ?
O1 Ba1 O5 67.48(18) . . ?
O1 Ba1 O5 117.79(18) 7_585 . ?
O2 Ba1 O5 45.37(17) . . ?
O2 Ba1 O5 102.59(17) 7_585 . ?
O4 Ba1 O5 62.06(15) 5_775 . ?
O6 Ba1 O5 141.37(18) 4_575 . ?
O6 Ba1 O5 87.70(17) 6_656 . ?
O3 Ba1 O5 168.5(2) 6_666 . ?
O3 Ba1 O5 61.8(2) 6_656 . ?
O1 Ba1 O5 117.79(18) . 1_565 ?
O1 Ba1 O5 67.48(18) 7_585 1_565 ?
O2 Ba1 O5 102.59(17) . 1_565 ?
O2 Ba1 O5 45.37(17) 7_585 1_565 ?
O4 Ba1 O5 62.06(15) 5_775 1_565 ?
O6 Ba1 O5 87.70(17) 4_575 1_565 ?
O6 Ba1 O5 141.37(18) 6_656 1_565 ?
O3 Ba1 O5 61.8(2) 6_666 1_565 ?
O3 Ba1 O5 168.5(2) 6_656 1_565 ?
O5 Ba1 O5 113.2(3) . 1_565 ?
O1 Ba1 Si2 81.88(11) . 1_565 ?
O1 Ba1 Si2 24.59(12) 7_585 1_565 ?
O2 Ba1 Si2 163.97(12) . 1_565 ?
O2 Ba1 Si2 97.39(11) 7_585 1_565 ?
O4 Ba1 Si2 86.64(12) 5_775 1_565 ?
O6 Ba1 Si2 75.84(12) 4_575 1_565 ?
O6 Ba1 Si2 119.87(12) 6_656 1_565 ?
O3 Ba1 Si2 26.48(17) 6_666 1_565 ?
O3 Ba1 Si2 114.69(17) 6_656 1_565 ?
O5 Ba1 Si2 142.33(15) . 1_565 ?
O5 Ba1 Si2 62.06(13) 1_565 1_565 ?
O5 Ba2 O6 133.87(18) . 6_556 ?
O5 Ba2 O6 133.87(18) . 4_465 ?
O6 Ba2 O6 55.23(19) 6_556 4_465 ?
O5 Ba2 O1 73.8(2) . . ?
O6 Ba2 O1 60.98(15) 6_556 . ?
O6 Ba2 O1 86.55(16) 4_465 . ?
O5 Ba2 O1 73.8(2) . 7_575 ?
O6 Ba2 O1 86.55(16) 6_556 7_575 ?
O6 Ba2 O1 60.98(15) 4_465 7_575 ?
O1 Ba2 O1 54.5(2) . 7_575 ?
O5 Ba2 O2 74.58(18) . 3_745 ?
O6 Ba2 O2 151.02(16) 6_556 3_745 ?
O6 Ba2 O2 112.40(15) 4_465 3_745 ?
O1 Ba2 O2 147.99(16) . 3_745 ?
O1 Ba2 O2 111.09(14) 7_575 3_745 ?
O5 Ba2 O2 74.58(18) . 5_775 ?
O6 Ba2 O2 112.40(15) 6_556 5_775 ?
O6 Ba2 O2 151.02(16) 4_465 5_775 ?
O1 Ba2 O2 111.09(14) . 5_775 ?
O1 Ba2 O2 147.99(16) 7_575 5_775 ?
O2 Ba2 O2 64.4(2) 3_745 5_775 ?
O5 Ba2 O2 137.42(18) . 7_475 ?
O6 Ba2 O2 88.67(15) 6_556 7_475 ?
O6 Ba2 O2 66.45(15) 4_465 7_475 ?
O1 Ba2 O2 148.02(16) . 7_475 ?
O1 Ba2 O2 118.45(14) 7_575 7_475 ?
O2 Ba2 O2 62.91(18) 3_745 7_475 ?
O2 Ba2 O2 88.68(11) 5_775 7_475 ?
O5 Ba2 O2 137.42(18) . 1_455 ?
O6 Ba2 O2 66.45(15) 6_556 1_455 ?
O6 Ba2 O2 88.67(15) 4_465 1_455 ?
O1 Ba2 O2 118.45(14) . 1_455 ?
O1 Ba2 O2 148.02(16) 7_575 1_455 ?
O2 Ba2 O2 88.68(11) 3_745 1_455 ?
O2 Ba2 O2 62.91(18) 5_775 1_455 ?
O2 Ba2 O2 47.88(19) 7_475 1_455 ?
O5 Ba2 O4 66.00(14) . 5_775 ?
O6 Ba2 O4 85.31(17) 6_556 5_775 ?
O6 Ba2 O4 139.44(18) 4_465 5_775 ?
O1 Ba2 O4 63.77(19) . 5_775 ?
O1 Ba2 O4 112.95(18) 7_575 5_775 ?
O2 Ba2 O4 106.98(18) 3_745 5_775 ?
O2 Ba2 O4 47.56(19) 5_775 5_775 ?
O2 Ba2 O4 127.71(18) 7_475 5_775 ?
O2 Ba2 O4 82.82(17) 1_455 5_775 ?
O5 Ba2 O4 66.00(14) . 5_765 ?
O6 Ba2 O4 139.44(18) 6_556 5_765 ?
O6 Ba2 O4 85.31(17) 4_465 5_765 ?
O1 Ba2 O4 112.95(18) . 5_765 ?
O1 Ba2 O4 63.77(19) 7_575 5_765 ?
O2 Ba2 O4 47.56(18) 3_745 5_765 ?
O2 Ba2 O4 106.98(18) 5_775 5_765 ?
O2 Ba2 O4 82.82(17) 7_475 5_765 ?
O2 Ba2 O4 127.71(18) 1_455 5_765 ?
O4 Ba2 O4 130.4(3) 5_775 5_765 ?
O5 Ba2 Si1 142.14(19) . 6_556 ?
O6 Ba2 Si1 27.62(10) 6_556 6_556 ?
O6 Ba2 Si1 27.62(10) 4_465 6_556 ?
O1 Ba2 Si1 72.67(13) . 6_556 ?
O1 Ba2 Si1 72.67(13) 7_575 6_556 ?
O2 Ba2 Si1 134.68(11) 3_745 6_556 ?
O2 Ba2 Si1 134.68(11) 5_775 6_556 ?
O2 Ba2 Si1 75.58(12) 7_475 6_556 ?
O2 Ba2 Si1 75.58(12) 1_455 6_556 ?
O4 Ba2 Si1 112.62(15) 5_775 6_556 ?
O4 Ba2 Si1 112.62(15) 5_765 6_556 ?
O5 S1 O4 111.9(5) . . ?
O5 S1 O2 109.8(3) . . ?
O4 S1 O2 108.4(3) . . ?
O5 S1 O2 109.8(3) . 7_575 ?
O4 S1 O2 108.4(3) . 7_575 ?
O2 S1 O2 108.5(5) . 7_575 ?
O5 S1 Ba2 128.5(4) . 1_655 ?
O4 S1 Ba2 119.6(3) . 1_655 ?
O2 S1 Ba2 54.3(2) . 1_655 ?
O2 S1 Ba2 54.3(2) 7_575 1_655 ?
O5 S1 Ba2 120.68(18) . 5_765 ?
O4 S1 Ba2 56.85(13) . 5_765 ?
O2 S1 Ba2 129.4(3) . 5_765 ?
O2 S1 Ba2 52.1(2) 7_575 5_765 ?
Ba2 S1 Ba2 89.03(5) 1_655 5_765 ?
O5 S1 Ba2 120.68(18) . 5_775 ?
O4 S1 Ba2 56.85(13) . 5_775 ?
O2 S1 Ba2 52.1(2) . 5_775 ?
O2 S1 Ba2 129.4(3) 7_575 5_775 ?
Ba2 S1 Ba2 89.03(5) 1_655 5_775 ?
Ba2 S1 Ba2 100.62(7) 5_765 5_775 ?
O5 S1 Ba1 64.5(2) . 1_545 ?
O4 S1 Ba1 128.40(10) . 1_545 ?
O2 S1 Ba1 121.4(3) . 1_545 ?
O2 S1 Ba1 45.3(2) 7_575 1_545 ?
Ba2 S1 Ba1 83.04(5) 1_655 1_545 ?
Ba2 S1 Ba1 80.195(17) 5_765 1_545 ?
Ba2 S1 Ba1 172.02(9) 5_775 1_545 ?
O3 Si1 O6 107.1(3) . . ?
O3 Si1 O6 107.1(3) . 7_575 ?
O6 Si1 O6 112.9(5) . 7_575 ?
O3 Si1 O7 108.1(5) . . ?
O6 Si1 O7 110.7(3) . . ?
O6 Si1 O7 110.7(3) 7_575 . ?
O3 Si1 Ba2 120.2(4) . 6_656 ?
O6 Si1 Ba2 56.5(2) . 6_656 ?
O6 Si1 Ba2 56.5(2) 7_575 6_656 ?
O7 Si1 Ba2 131.7(3) . 6_656 ?
O3 Si1 Ba1 58.78(19) . 6_546 ?
O6 Si1 Ba1 125.5(3) . 6_546 ?
O6 Si1 Ba1 48.3(2) 7_575 6_546 ?
O7 Si1 Ba1 123.81(15) . 6_546 ?
Ba2 Si1 Ba1 84.33(6) 6_656 6_546 ?
O3 Si1 Ba1 58.78(19) . 6_556 ?
O6 Si1 Ba1 48.3(2) . 6_556 ?
O6 Si1 Ba1 125.5(3) 7_575 6_556 ?
O7 Si1 Ba1 123.81(15) . 6_556 ?
Ba2 Si1 Ba1 84.33(6) 6_656 6_556 ?
Ba1 Si1 Ba1 96.72(8) 6_546 6_556 ?
O1 Si2 O1 111.6(5) 7_575 . ?
O1 Si2 O7 112.0(3) 7_575 . ?
O1 Si2 O7 112.0(3) . . ?
O1 Si2 O3 107.1(3) 7_575 6_656 ?
O1 Si2 O3 107.1(3) . 6_656 ?
O7 Si2 O3 106.7(5) . 6_656 ?
O1 Si2 Ba1 47.0(2) 7_575 1_545 ?
O1 Si2 Ba1 124.5(3) . 1_545 ?
O7 Si2 Ba1 123.44(14) . 1_545 ?
O3 Si2 Ba1 60.04(19) 6_656 1_545 ?
Si2 O1 Pb1 124.3(3) . . ?
Si2 O1 Ba1 108.4(3) . . ?
Pb1 O1 Ba1 111.31(19) . . ?
Si2 O1 Ba2 96.5(2) . . ?
Pb1 O1 Ba2 108.3(2) . . ?
Ba1 O1 Ba2 105.65(19) . . ?
S1 O2 Ba1 112.7(3) . . ?
S1 O2 Ba2 104.2(3) . 5_775 ?
Ba1 O2 Ba2 108.77(17) . 5_775 ?
S1 O2 Ba2 101.7(3) . 1_655 ?
Ba1 O2 Ba2 111.94(18) . 1_655 ?
Ba2 O2 Ba2 117.09(18) 5_775 1_655 ?
Si1 O3 Si2 161.4(7) . 6_556 ?
Si1 O3 Ba1 95.7(3) . 6_556 ?
Si2 O3 Ba1 93.5(2) 6_556 6_556 ?
Si1 O3 Ba1 95.7(3) . 6_546 ?
Si2 O3 Ba1 93.5(2) 6_556 6_546 ?
Ba1 O3 Ba1 120.8(3) 6_556 6_546 ?
S1 O4 Ba1 130.0(4) . 5_775 ?
S1 O4 Ba2 99.1(2) . 5_775 ?
Ba1 O4 Ba2 101.33(17) 5_775 5_775 ?
S1 O4 Ba2 99.1(2) . 5_765 ?
Ba1 O4 Ba2 101.33(17) 5_775 5_765 ?
Ba2 O4 Ba2 130.4(3) 5_775 5_765 ?
S1 O5 Ba2 165.8(6) . . ?
S1 O5 Ba1 92.0(3) . . ?
Ba2 O5 Ba1 95.76(17) . . ?
S1 O5 Ba1 92.0(3) . 1_545 ?
Ba2 O5 Ba1 95.76(17) . 1_545 ?
Ba1 O5 Ba1 113.2(3) . 1_545 ?
Si1 O6 Pb1 120.4(3) . 6_656 ?
Si1 O6 Ba1 107.1(3) . 6_556 ?
Pb1 O6 Ba1 111.88(18) 6_656 6_556 ?
Si1 O6 Ba2 95.9(2) . 6_656 ?
Pb1 O6 Ba2 108.2(2) 6_656 6_656 ?
Ba1 O6 Ba2 112.33(19) 6_556 6_656 ?
Si2 O7 Si1 175.1(6) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.51
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.543
_refine_diff_density_min         -1.432
_refine_diff_density_rms         0.321
_database_code_depnum_ccdc_archive 'CCDC 969032'
