# Supplementary Material (ESI) for Dalton Transactions
# This journal is (c) The Royal Society of Chemistry 2010

data_global
_journal_name_full               'Dalton Trans.'

_journal_coden_Cambridge         0222

_publ_contact_author_name        'Wen-Dan Cheng'
_publ_contact_author_email       Wen-Dan

_publ_section_title              
;
Lone Electron-Pair Enhancement of SHG responses in
Eulytite-Type Compounds: AII3MIII(PO4)3 (A = Pb, M = Bi; A = Ba, M = Bi, La)
;
loop_
_publ_author_name
'Wen-Dan Cheng'
'Zhangzhen He'
'Chen- Sheng Lin'
'Xin-Song Lin'
;
Jin-Yun Wang
;
'Hao Zhang'
'Wei-Long Zhang'

# Attachment 'Zwl-dalton-cif.txt'

data_a
_database_code_depnum_ccdc_archive 'CCDC 266453'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            'Cs-Hf-W-O Values Set for Hf/W'
_chemical_melting_point          ?
_chemical_formula_moiety         'Bi O12 P3 Pb3'
_chemical_formula_sum            'Bi O12 P3 Pb3'
_chemical_formula_weight         1115.99

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'
P P 0.1023 0.0942 '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'
Bi Bi -4.1077 10.2566 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           cubic
_symmetry_space_group_name_H-M   I-43d

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'
'y+1/4, x+1/4, z+1/4'
'-y+1/4, -x+3/4, z+3/4'
'y+3/4, -x+1/4, -z+3/4'
'-y+3/4, x+3/4, -z+1/4'
'x+1/4, z+1/4, y+1/4'
'-x+3/4, z+3/4, -y+1/4'
'-x+1/4, -z+3/4, y+3/4'
'x+3/4, -z+1/4, -y+3/4'
'z+1/4, y+1/4, x+1/4'
'z+3/4, -y+1/4, -x+3/4'
'-z+3/4, y+3/4, -x+1/4'
'-z+1/4, -y+3/4, x+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-x+1/2, y+1, -z+1'
'x+1, -y+1, -z+1/2'
'z+1/2, x+1/2, y+1/2'
'z+1, -x+1, -y+1/2'
'-z+1, -x+1/2, y+1'
'-z+1/2, x+1, -y+1'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, z+1, -x+1'
'y+1, -z+1, -x+1/2'
'-y+1, -z+1/2, x+1'
'y+3/4, x+3/4, z+3/4'
'-y+3/4, -x+5/4, z+5/4'
'y+5/4, -x+3/4, -z+5/4'
'-y+5/4, x+5/4, -z+3/4'
'x+3/4, z+3/4, y+3/4'
'-x+5/4, z+5/4, -y+3/4'
'-x+3/4, -z+5/4, y+5/4'
'x+5/4, -z+3/4, -y+5/4'
'z+3/4, y+3/4, x+3/4'
'z+5/4, -y+3/4, -x+5/4'
'-z+5/4, y+5/4, -x+3/4'
'-z+3/4, -y+5/4, x+5/4'

_cell_length_a                   10.3663(7)
_cell_length_b                   10.3663(7)
_cell_length_c                   10.3663(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1113.96(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    639
_cell_measurement_theta_min      2.7786
_cell_measurement_theta_max      27.3833

_exptl_crystal_description       Prism
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    6.651
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1880
_exptl_absorpt_coefficient_mu    61.445
_exptl_absorpt_correction_type   'Multi-scan '
_exptl_absorpt_correction_T_min  0.065
_exptl_absorpt_correction_T_max  0.086
_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
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_detector_area_resol_mean 13.6612
_diffrn_standards_number         850
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        none
_diffrn_reflns_number            3853
_diffrn_reflns_av_R_equivalents  0.0871
_diffrn_reflns_av_sigmaI/netI    0.0255
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         4.82
_diffrn_reflns_theta_max         27.38
_reflns_number_total             214
_reflns_number_gt                214
_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 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^)+(0.0380P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/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       0.0017(2)
_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(4)
_refine_ls_number_reflns         214
_refine_ls_number_parameters     16
_refine_ls_number_restraints     23
_refine_ls_R_factor_all          0.0212
_refine_ls_R_factor_gt           0.0212
_refine_ls_wR_factor_ref         0.0584
_refine_ls_wR_factor_gt          0.0584
_refine_ls_goodness_of_fit_ref   1.198
_refine_ls_restrained_S_all      1.139
_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
Bi1 Bi 0.07522(3) 0.07522(3) 0.07522(3) 0.0138(3) Uani 0.25 3 d SPU . .
Pb1 Pb 0.07522(3) 0.07522(3) 0.07522(3) 0.0138(3) Uani 0.75 3 d SPU . .
P1 P 0.2500 0.3750 0.0000 0.0093(8) Uani 1 4 d SU . .
O1 O 0.1390(8) 0.2912(8) 0.0513(9) 0.0285(18) Uani 1 1 d U . .

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
Bi1 0.0138(3) 0.0138(3) 0.0138(3) 0.00125(17) 0.00125(17) 0.00125(17)
Pb1 0.0138(3) 0.0138(3) 0.0138(3) 0.00125(17) 0.00125(17) 0.00125(17)
P1 0.0086(11) 0.0107(17) 0.0086(11) 0.000 0.000 0.000
O1 0.018(4) 0.021(3) 0.047(6) 0.005(3) 0.014(3) -0.005(3)

_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
Bi1 O1 2.347(8) . ?
Bi1 O1 2.347(8) 5 ?
Bi1 O1 2.347(8) 9 ?
Bi1 O1 2.629(8) 30_445 ?
Bi1 O1 2.629(8) 34_544 ?
Bi1 O1 2.629(8) 26_454 ?
P1 O1 1.537(9) 46_454 ?
P1 O1 1.537(8) . ?
P1 O1 1.537(9) 27_544 ?
P1 O1 1.537(8) 24_554 ?
O1 Pb1 2.629(8) 26_454 ?
O1 Bi1 2.629(8) 26_454 ?

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 Bi1 O1 82.1(3) . 5 ?
O1 Bi1 O1 82.1(3) . 9 ?
O1 Bi1 O1 82.1(3) 5 9 ?
O1 Bi1 O1 152.6(4) . 30_445 ?
O1 Bi1 O1 74.1(3) 5 30_445 ?
O1 Bi1 O1 81.51(13) 9 30_445 ?
O1 Bi1 O1 81.51(13) . 34_544 ?
O1 Bi1 O1 152.6(4) 5 34_544 ?
O1 Bi1 O1 74.1(3) 9 34_544 ?
O1 Bi1 O1 114.53(15) 30_445 34_544 ?
O1 Bi1 O1 74.1(3) . 26_454 ?
O1 Bi1 O1 81.51(13) 5 26_454 ?
O1 Bi1 O1 152.6(4) 9 26_454 ?
O1 Bi1 O1 114.53(15) 30_445 26_454 ?
O1 Bi1 O1 114.53(15) 34_544 26_454 ?
O1 P1 O1 108.6(3) 46_454 . ?
O1 P1 O1 108.6(3) 46_454 27_544 ?
O1 P1 O1 111.2(6) . 27_544 ?
O1 P1 O1 111.2(6) 46_454 24_554 ?
O1 P1 O1 108.6(3) . 24_554 ?
O1 P1 O1 108.6(3) 27_544 24_554 ?
P1 O1 Bi1 141.9(5) . . ?
P1 O1 Pb1 111.5(4) . 26_454 ?
Bi1 O1 Pb1 104.8(3) . 26_454 ?
P1 O1 Bi1 111.5(4) . 26_454 ?
Bi1 O1 Bi1 104.8(3) . 26_454 ?
Pb1 O1 Bi1 0.000(7) 26_454 26_454 ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         1.314
_refine_diff_density_min         -1.310
_refine_diff_density_rms         0.263