# Electronic Supplementary Material (ESI) for Physical Chemistry Chemical Physics.
# This journal is © the Owner Societies 2016

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1
_database_code_depnum_ccdc_archive 'CCDC 1472878'
_audit_update_record             
;
2016-04-07 deposited with the CCDC.
2016-06-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'Li O4 P Pb'
_chemical_formula_weight         309.10

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Li Li -0.0003 0.0001 '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'
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   Pna2(1)

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

_cell_length_a                   8.027(8)
_cell_length_b                   18.689(18)
_cell_length_c                   4.965(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     744.9(12)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1448
_cell_measurement_theta_min      2.76
_cell_measurement_theta_max      27.33

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.305
_exptl_crystal_size_mid          0.148
_exptl_crystal_size_min          0.095
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    5.513
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1056
_exptl_absorpt_coefficient_mu    45.584
_exptl_absorpt_correction_type   Numerical
_exptl_absorpt_correction_T_min  0.2939
_exptl_absorpt_correction_T_max  0.7456
_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            4301
_diffrn_reflns_av_R_equivalents  0.0548
_diffrn_reflns_av_sigmaI/netI    0.0653
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_theta_min         2.76
_diffrn_reflns_theta_max         27.39
_reflns_number_total             1486
_reflns_number_gt                1319
_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)+(0.0379P)²+0.0000P] where P=(Fo²+2Fc²)/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       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.018(19)
_refine_ls_number_reflns         1486
_refine_ls_number_parameters     127
_refine_ls_number_restraints     31
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0352
_refine_ls_wR_factor_ref         0.0853
_refine_ls_wR_factor_gt          0.0811
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.017
_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 0.32569(6) 0.44650(3) 0.08852(12) 0.01205(15) Uani 1 1 d . . .
Pb2 Pb 0.47267(6) 0.22895(3) 0.0729(2) 0.01542(16) Uani 1 1 d . . .
P1 P 0.2670(4) 0.07157(19) 0.0379(10) 0.0075(8) Uani 1 1 d . . .
P2 P 0.2877(5) 0.32044(19) 0.5339(9) 0.0077(9) Uani 1 1 d . . .
Li1 Li 0.491(3) 0.0592(12) -0.461(6) 0.011(5) Uani 1 1 d U . .
Li2 Li 0.180(3) 0.1489(13) -0.464(6) 0.012(6) Uani 1 1 d U . .
O1 O 0.2815(13) 0.0738(6) 0.346(2) 0.009(2) Uani 1 1 d . . .
O2 O 0.2479(13) 0.1478(6) -0.079(2) 0.012(2) Uani 1 1 d U . .
O3 O 0.1367(13) 0.3645(6) 0.454(2) 0.017(3) Uani 1 1 d . . .
O4 O 0.3087(14) 0.3180(7) 0.842(2) 0.016(3) Uani 1 1 d . . .
O5 O 0.1082(13) 0.0275(6) -0.044(2) 0.011(2) Uani 1 1 d U . .
O6 O 0.4160(14) 0.0342(6) -0.093(2) 0.011(2) Uani 1 1 d . . .
O7 O 0.4436(13) 0.3531(6) 0.399(2) 0.013(2) Uani 1 1 d . . .
O8 O 0.2695(14) 0.2445(6) 0.420(2) 0.014(2) Uani 1 1 d U . .


_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 O5 2.410(10) 3 ?
Pb1 O5 2.431(11) 4 ?
Pb1 O7 2.513(12) . ?
Pb1 O4 2.698(12) 1_554 ?
Pb1 Li1 3.31(2) 4 ?
Pb1 Li1 3.50(3) 3_456 ?
Pb2 O8 2.389(11) . ?
Pb2 O4 2.411(12) 1_554 ?
Pb2 O2 2.474(11) . ?
Pb2 Li2 3.61(2) 1_556 ?
P1 O6 1.529(11) . ?
P1 O1 1.534(11) . ?
P1 O2 1.546(12) . ?
P1 O5 1.571(11) . ?
P1 Li2 2.95(3) 1_556 ?
P1 Li1 3.08(3) 1_556 ?
P2 O3 1.519(11) . ?
P2 O8 1.536(12) . ?
P2 O4 1.542(11) . ?
P2 O7 1.546(11) . ?
Li1 O3 1.89(2) 3_554 ?
Li1 O1 1.95(3) 1_554 ?
Li1 O6 1.98(3) . ?
Li1 O6 2.01(3) 2_654 ?
Li1 Li2 3.01(3) . ?
Li1 P1 3.08(3) 1_554 ?
Li1 Pb1 3.31(2) 4_544 ?
Li1 Li1 3.33(3) 2_654 ?
Li1 Li1 3.33(3) 2_655 ?
Li1 Pb1 3.50(3) 3_554 ?
Li2 O1 1.88(3) 1_554 ?
Li2 O2 1.99(3) . ?
Li2 O8 2.01(3) 1_554 ?
Li2 O7 2.01(3) 3_454 ?
Li2 P1 2.95(3) 1_554 ?
Li2 Pb2 3.61(2) 1_554 ?
O1 Li2 1.88(3) 1_556 ?
O1 Li1 1.95(3) 1_556 ?
O3 Li1 1.89(2) 3_456 ?
O4 Pb2 2.411(12) 1_556 ?
O4 Pb1 2.698(12) 1_556 ?
O5 Pb1 2.410(10) 3_455 ?
O5 Pb1 2.431(10) 4_544 ?
O6 Li1 2.01(3) 2_655 ?
O7 Li2 2.01(3) 3_556 ?
O8 Li2 2.01(3) 1_556 ?

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
O5 Pb1 O5 82.7(3) 3 4 ?
O5 Pb1 O7 87.3(3) 3 . ?
O5 Pb1 O7 83.7(4) 4 . ?
O5 Pb1 O4 96.0(4) 3 1_554 ?
O5 Pb1 O4 154.9(4) 4 1_554 ?
O7 Pb1 O4 71.2(3) . 1_554 ?
O5 Pb1 Li1 125.0(5) 3 4 ?
O5 Pb1 Li1 80.0(5) 4 4 ?
O7 Pb1 Li1 141.0(5) . 4 ?
O4 Pb1 Li1 119.6(5) 1_554 4 ?
O5 Pb1 Li1 154.6(5) 3 3_456 ?
O5 Pb1 Li1 72.9(5) 4 3_456 ?
O7 Pb1 Li1 82.9(5) . 3_456 ?
O4 Pb1 Li1 102.9(5) 1_554 3_456 ?
Li1 Pb1 Li1 58.5(5) 4 3_456 ?
O8 Pb2 O4 83.4(4) . 1_554 ?
O8 Pb2 O2 78.2(4) . . ?
O4 Pb2 O2 83.1(4) 1_554 . ?
O8 Pb2 Li2 31.5(5) . 1_556 ?
O4 Pb2 Li2 103.4(5) 1_554 1_556 ?
O2 Pb2 Li2 57.7(5) . 1_556 ?
O6 P1 O1 112.1(6) . . ?
O6 P1 O2 109.9(6) . . ?
O1 P1 O2 110.9(6) . . ?
O6 P1 O5 106.6(6) . . ?
O1 P1 O5 109.4(6) . . ?
O2 P1 O5 107.8(6) . . ?
O6 P1 Li2 140.0(6) . 1_556 ?
O1 P1 Li2 33.8(7) . 1_556 ?
O2 P1 Li2 80.7(7) . 1_556 ?
O5 P1 Li2 106.3(6) . 1_556 ?
O6 P1 Li1 81.5(6) . 1_556 ?
O1 P1 Li1 32.0(6) . 1_556 ?
O2 P1 Li1 115.5(6) . 1_556 ?
O5 P1 Li1 130.0(6) . 1_556 ?
Li2 P1 Li1 59.8(7) 1_556 1_556 ?
O3 P2 O8 109.2(7) . . ?
O3 P2 O4 111.3(7) . . ?
O8 P2 O4 110.5(7) . . ?
O3 P2 O7 108.5(7) . . ?
O8 P2 O7 106.3(6) . . ?
O4 P2 O7 110.8(6) . . ?
O3 Li1 O1 108.5(13) 3_554 1_554 ?
O3 Li1 O6 124.9(15) 3_554 . ?
O1 Li1 O6 103.0(11) 1_554 . ?
O3 Li1 O6 110.5(13) 3_554 2_654 ?
O1 Li1 O6 106.4(12) 1_554 2_654 ?
O6 Li1 O6 102.0(11) . 2_654 ?
O3 Li1 Li2 95.3(10) 3_554 . ?
O1 Li1 Li2 37.4(7) 1_554 . ?
O6 Li1 Li2 83.4(10) . . ?
O6 Li1 Li2 142.4(12) 2_654 . ?
O3 Li1 P1 97.1(11) 3_554 1_554 ?
O1 Li1 P1 24.6(5) 1_554 1_554 ?
O6 Li1 P1 126.0(10) . 1_554 ?
O6 Li1 P1 91.1(10) 2_654 1_554 ?
Li2 Li1 P1 58.0(7) . 1_554 ?
O3 Li1 Pb1 166.2(12) 3_554 4_544 ?
O1 Li1 Pb1 57.7(6) 1_554 4_544 ?
O6 Li1 Pb1 63.1(7) . 4_544 ?
O6 Li1 Pb1 75.9(7) 2_654 4_544 ?
Li2 Li1 Pb1 73.6(7) . 4_544 ?
P1 Li1 Pb1 70.1(5) 1_554 4_544 ?
O3 Li1 Li1 107.8(11) 3_554 2_654 ?
O1 Li1 Li1 76.4(8) 1_554 2_654 ?
O6 Li1 Li1 123.0(13) . 2_654 ?
O6 Li1 Li1 33.2(9) 2_654 2_654 ?
Li2 Li1 Li1 113.8(10) . 2_654 ?
P1 Li1 Li1 58.2(4) 1_554 2_654 ?
Pb1 Li1 Li1 70.5(8) 4_544 2_654 ?
O3 Li1 Li1 129.8(13) 3_554 2_655 ?
O1 Li1 Li1 119.8(13) 1_554 2_655 ?
O6 Li1 Li1 33.7(4) . 2_655 ?
O6 Li1 Li1 69.4(12) 2_654 2_655 ?
Li2 Li1 Li1 114.3(11) . 2_655 ?
P1 Li1 Li1 132.7(11) 1_554 2_655 ?
Pb1 Li1 Li1 63.6(8) 4_544 2_655 ?
Li1 Li1 Li1 96.4(12) 2_654 2_655 ?
O3 Li1 Pb1 53.5(7) 3_554 3_554 ?
O1 Li1 Pb1 110.6(12) 1_554 3_554 ?
O6 Li1 Pb1 144.7(11) . 3_554 ?
O6 Li1 Pb1 58.6(7) 2_654 3_554 ?
Li2 Li1 Pb1 130.7(10) . 3_554 ?
P1 Li1 Pb1 86.2(7) 1_554 3_554 ?
Pb1 Li1 Pb1 128.2(8) 4_544 3_554 ?
Li1 Li1 Pb1 57.9(6) 2_654 3_554 ?
Li1 Li1 Pb1 115.0(10) 2_655 3_554 ?
O1 Li2 O2 110.8(13) 1_554 . ?
O1 Li2 O8 111.3(13) 1_554 1_554 ?
O2 Li2 O8 100.8(12) . 1_554 ?
O1 Li2 O7 103.0(13) 1_554 3_454 ?
O2 Li2 O7 125.7(13) . 3_454 ?
O8 Li2 O7 104.9(12) 1_554 3_454 ?
O1 Li2 P1 27.0(6) 1_554 1_554 ?
O2 Li2 P1 137.4(11) . 1_554 ?
O8 Li2 P1 96.3(10) 1_554 1_554 ?
O7 Li2 P1 86.0(10) 3_454 1_554 ?
O1 Li2 Li1 39.2(8) 1_554 . ?
O2 Li2 Li1 76.2(9) . . ?
O8 Li2 Li1 101.5(10) 1_554 . ?
O7 Li2 Li1 140.5(13) 3_454 . ?
P1 Li2 Li1 62.2(7) 1_554 . ?
O1 Li2 Pb2 72.9(8) 1_554 1_554 ?
O2 Li2 Pb2 115.9(9) . 1_554 ?
O8 Li2 Pb2 38.4(6) 1_554 1_554 ?
O7 Li2 Pb2 113.9(11) 3_454 1_554 ?
P1 Li2 Pb2 61.0(5) 1_554 1_554 ?
Li1 Li2 Pb2 72.2(7) . 1_554 ?
P1 O1 Li2 119.2(11) . 1_556 ?
P1 O1 Li1 123.4(10) . 1_556 ?
Li2 O1 Li1 103.4(12) 1_556 1_556 ?
P1 O2 Li2 113.4(9) . . ?
P1 O2 Pb2 112.2(6) . . ?
Li2 O2 Pb2 119.1(8) . . ?
P2 O3 Li1 147.5(12) . 3_456 ?
P2 O4 Pb2 123.5(6) . 1_556 ?
P2 O4 Pb1 115.4(6) . 1_556 ?
Pb2 O4 Pb1 111.8(4) 1_556 1_556 ?
P1 O5 Pb1 126.0(6) . 3_455 ?
P1 O5 Pb1 110.0(5) . 4_544 ?
Pb1 O5 Pb1 122.4(4) 3_455 4_544 ?
P1 O6 Li1 121.4(9) . . ?
P1 O6 Li1 123.4(10) . 2_655 ?
Li1 O6 Li1 113.1(10) . 2_655 ?
P2 O7 Li2 127.4(10) . 3_556 ?
P2 O7 Pb1 103.6(5) . . ?
Li2 O7 Pb1 125.1(9) 3_556 . ?
P2 O8 Li2 138.5(10) . 1_556 ?
P2 O8 Pb2 108.3(6) . . ?
Li2 O8 Pb2 110.1(9) 1_556 . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        27.39
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.855
_refine_diff_density_min         -3.809
_refine_diff_density_rms         0.508
