# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry
# This journal is © The Royal Society of Chemistry 2012


data_global

_journal_coden_Cambridge         1145

loop_
_publ_author_name
'Yu, Hongwei'
'Pan, Shi-Lie'
'Wu, Hongping'
'Zhang, Fangfang'
'Li, Hongyi'
'Yang, Zhihua'

_publ_contact_author_name        'Pan, Shi-Lie'
_publ_contact_author_email       slpan@ms.xjb.ac.cn

_publ_section_title              
;
A New Congruent-Melting Oxyborate, Pb4O(BO3)2 with Optimally
Aligned BO3 Triangles Adopted Layered-type Arrangement
;

# Attachment '- Pb4B2O7.cif'

data_1
_database_code_depnum_ccdc_archive 'CCDC 844322'
#TrackingRef '- Pb4B2O7.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'B2 O7 Pb4'
_chemical_formula_weight         962.38

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'Aba2 '

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

_cell_length_a                   15.4598(16)
_cell_length_b                   10.8050(11)
_cell_length_c                   9.9452(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1661.3(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    7.696
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3152
_exptl_absorpt_coefficient_mu    80.825
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.0134
_exptl_absorpt_correction_T_max  0.1505
_exptl_absorpt_process_details   ?

_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       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7012
_diffrn_reflns_av_R_equivalents  0.0532
_diffrn_reflns_av_sigmaI/netI    0.0521
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.63
_diffrn_reflns_theta_max         27.56
_reflns_number_total             1877
_reflns_number_gt                1718
_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 F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0309P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   ?
_refine_ls_hydrogen_treatment    ?
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00098(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(3)
_refine_ls_number_reflns         1877
_refine_ls_number_parameters     120
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_gt           0.0301
_refine_ls_wR_factor_ref         0.0712
_refine_ls_wR_factor_gt          0.0695
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_restrained_S_all      1.063
_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 0.38215(3) 1.04924(4) 0.22669(4) 0.01570(16) Uani 1 1 d . . .
Pb2 Pb 0.37724(3) 0.69620(4) 0.22039(4) 0.01395(16) Uani 1 1 d . . .
Pb3 Pb 0.19947(4) 0.87341(4) 0.38993(6) 0.01351(16) Uani 1 1 d . . .
Pb4 Pb 0.41790(4) 0.87573(4) 0.52989(7) 0.01624(17) Uani 1 1 d . . .
B1 B 0.2547(12) 0.6207(11) 0.492(2) 0.012(4) Uani 1 1 d . . .
B2 B 0.5065(12) 0.6103(13) 0.4858(19) 0.016(4) Uani 1 1 d . . .
O1 O 0.2583(8) 0.6207(6) 0.3460(12) 0.017(2) Uani 1 1 d . . .
O2 O 0.3425(7) 0.8729(7) 0.3342(12) 0.016(2) Uani 1 1 d . . .
O3 O 0.4453(8) 0.8811(8) 0.1028(13) 0.020(3) Uani 1 1 d . . .
O4 O 0.2376(7) 0.7321(9) 0.5540(12) 0.022(2) Uani 1 1 d . . .
O5 O 0.2362(7) 1.0136(9) 0.5571(11) 0.019(2) Uani 1 1 d . . .
O6 O 0.5000 1.0000 0.4091(16) 0.029(4) Uani 1 2 d S . .
O7 O 0.4694(8) 0.7087(9) 0.4269(12) 0.033(3) Uani 1 1 d . . .
O8 O 0.5000 0.5000 0.4119(18) 0.024(4) Uani 1 2 d S . .

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
Pb1 0.0196(3) 0.0130(3) 0.0145(3) 0.0008(2) 0.0037(3) -0.0011(2)
Pb2 0.0153(3) 0.0130(3) 0.0135(3) -0.0013(2) 0.0008(3) 0.00211(19)
Pb3 0.0110(3) 0.0149(3) 0.0146(3) -0.0002(2) -0.0011(2) 0.00024(18)
Pb4 0.0196(4) 0.0168(3) 0.0124(3) 0.0002(2) -0.0024(2) -0.00184(19)
B1 0.010(9) 0.014(8) 0.013(9) 0.004(6) 0.002(6) 0.000(6)
B2 0.016(10) 0.017(8) 0.016(9) -0.004(7) 0.005(7) 0.004(6)
O1 0.022(6) 0.017(5) 0.011(6) 0.004(3) 0.009(4) 0.001(4)
O2 0.016(6) 0.017(5) 0.016(6) 0.002(4) -0.007(5) 0.001(4)
O3 0.028(7) 0.017(5) 0.015(6) 0.000(4) 0.005(5) 0.004(4)
O4 0.023(6) 0.023(5) 0.021(6) -0.011(5) 0.002(5) -0.003(5)
O5 0.028(6) 0.015(5) 0.013(6) 0.002(4) 0.005(5) -0.004(4)
O6 0.056(12) 0.023(8) 0.007(8) 0.000 0.000 -0.015(8)
O7 0.056(9) 0.023(6) 0.022(7) -0.004(5) -0.011(6) 0.010(5)
O8 0.036(10) 0.012(7) 0.024(10) 0.000 0.000 0.004(6)

_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 2.270(9) . ?
Pb1 O3 2.402(10) . ?
Pb1 O5 2.518(11) 8_544 ?
Pb1 O1 2.593(12) 4 ?
Pb1 O6 2.625(11) . ?
Pb2 O2 2.284(9) . ?
Pb2 O1 2.368(11) . ?
Pb2 O4 2.458(12) 8_544 ?
Pb2 O7 2.503(12) . ?
Pb2 O3 2.543(10) . ?
Pb3 O2 2.279(12) . ?
Pb3 O4 2.310(12) . ?
Pb3 O5 2.319(11) . ?
Pb4 O6 2.204(9) . ?
Pb4 O7 2.223(11) . ?
Pb4 O2 2.269(11) . ?
Pb4 Pb4 3.6953(11) 2_675 ?
B1 O5 1.335(16) 4_545 ?
B1 O4 1.380(17) . ?
B1 O1 1.45(2) . ?
B2 O7 1.34(2) . ?
B2 O3 1.38(2) 6_665 ?
B2 O8 1.404(18) . ?
O1 Pb1 2.593(12) 4_545 ?
O3 B2 1.38(2) 6_664 ?
O4 Pb2 2.458(12) 8_545 ?
O5 B1 1.335(16) 4 ?
O5 Pb1 2.518(11) 8_545 ?
O6 Pb4 2.204(9) 2_675 ?
O6 Pb1 2.625(11) 2_675 ?
O8 B2 1.404(18) 2_665 ?

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 O3 73.5(4) . . ?
O2 Pb1 O5 89.5(4) . 8_544 ?
O3 Pb1 O5 80.6(4) . 8_544 ?
O2 Pb1 O1 78.9(3) . 4 ?
O3 Pb1 O1 143.2(3) . 4 ?
O5 Pb1 O1 75.1(4) 8_544 4 ?
O2 Pb1 O6 72.1(3) . . ?
O3 Pb1 O6 85.4(4) . . ?
O5 Pb1 O6 159.4(2) 8_544 . ?
O1 Pb1 O6 109.0(4) 4 . ?
O2 Pb2 O1 81.0(3) . . ?
O2 Pb2 O4 91.8(4) . 8_544 ?
O1 Pb2 O4 81.3(4) . 8_544 ?
O2 Pb2 O7 71.5(4) . . ?
O1 Pb2 O7 91.6(4) . . ?
O4 Pb2 O7 162.8(4) 8_544 . ?
O2 Pb2 O3 70.6(4) . . ?
O1 Pb2 O3 146.6(3) . . ?
O4 Pb2 O3 82.2(4) 8_544 . ?
O7 Pb2 O3 95.7(4) . . ?
O2 Pb3 O4 85.6(4) . . ?
O2 Pb3 O5 86.5(4) . . ?
O4 Pb3 O5 82.1(4) . . ?
O6 Pb4 O7 92.1(4) . . ?
O6 Pb4 O2 80.6(4) . . ?
O7 Pb4 O2 77.2(4) . . ?
O6 Pb4 Pb4 33.0(3) . 2_675 ?
O7 Pb4 Pb4 110.1(3) . 2_675 ?
O2 Pb4 Pb4 111.3(2) . 2_675 ?
O5 B1 O4 123.9(18) 4_545 . ?
O5 B1 O1 118.9(12) 4_545 . ?
O4 B1 O1 117.2(12) . . ?
O7 B2 O3 122.9(13) . 6_665 ?
O7 B2 O8 114.4(16) . . ?
O3 B2 O8 122.4(14) 6_665 . ?
B1 O1 Pb2 123.9(10) . . ?
B1 O1 Pb1 115.2(9) . 4_545 ?
Pb2 O1 Pb1 120.8(5) . 4_545 ?
Pb4 O2 Pb1 104.7(4) . . ?
Pb4 O2 Pb3 106.9(5) . . ?
Pb1 O2 Pb3 112.0(4) . . ?
Pb4 O2 Pb2 108.4(4) . . ?
Pb1 O2 Pb2 113.9(5) . . ?
Pb3 O2 Pb2 110.5(4) . . ?
B2 O3 Pb1 126.8(9) 6_664 . ?
B2 O3 Pb2 131.4(9) 6_664 . ?
Pb1 O3 Pb2 101.0(4) . . ?
B1 O4 Pb3 107.9(10) . . ?
B1 O4 Pb2 107.7(9) . 8_545 ?
Pb3 O4 Pb2 113.3(5) . 8_545 ?
B1 O5 Pb3 104.0(10) 4 . ?
B1 O5 Pb1 105.7(10) 4 8_545 ?
Pb3 O5 Pb1 113.7(4) . 8_545 ?
Pb4 O6 Pb4 113.9(7) 2_675 . ?
Pb4 O6 Pb1 130.76(14) 2_675 . ?
Pb4 O6 Pb1 95.77(10) . . ?
Pb4 O6 Pb1 95.77(10) 2_675 2_675 ?
Pb4 O6 Pb1 130.76(14) . 2_675 ?
Pb1 O6 Pb1 92.6(5) . 2_675 ?
B2 O7 Pb4 126.5(11) . . ?
B2 O7 Pb2 124.0(10) . . ?
Pb4 O7 Pb2 102.6(4) . . ?
B2 O8 B2 117(2) . 2_665 ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.56
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         2.464
_refine_diff_density_min         -1.571
_refine_diff_density_rms         0.426