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


#=======================================================================
data_I
#=======================================================================

# 5. CHEMICAL DATA

_chemical_name_systematic
; ?
;
_chemical_name_common                    ?
_chemical_formula_moiety                 'F3 Li9 Mg3 O16 P4'
_chemical_formula_structural             ?
_chemical_formula_analytical             ?
_chemical_formula_iupac                  ?
_chemical_formula_sum                    'F3 Li9 Mg3 O16 P4'
_chemical_formula_weight                 572.3
_chemical_melting_point                  ?
_chemical_compound_source                ?
_chemical_absolute_configuration         ?

#=======================================================================

# 6. CRYSTAL DATA

_symmetry_cell_setting                   hexagonal
_symmetry_space_group_name_H-M           'P 63'
_symmetry_space_group_name_Hall          'P 6c'
_symmetry_Int_Tables_number              173
loop_
 _symmetry_equiv_pos_site_id
 _symmetry_equiv_pos_as_xyz
 1   x,y,z
 2   -y,x-y,z
 3   -x+y,-x,z
 4   -x,-y,z+1/2
 5   y,-x+y,z+1/2
 6   x-y,x,z+1/2
_cell_length_a                           12.6159(6)
_cell_length_b                           12.6159(6)
_cell_length_c                           5.0082(4)
_cell_angle_alpha                        90
_cell_angle_beta                         90
_cell_angle_gamma                        120
_cell_volume                             690.32(7)

loop_
 _jana_cell_twin_matrix_id
 _jana_cell_twin_volume_fraction
 _jana_cell_twin_matrix_1_1
 _jana_cell_twin_matrix_1_2
 _jana_cell_twin_matrix_1_3
 _jana_cell_twin_matrix_2_1
 _jana_cell_twin_matrix_2_2
 _jana_cell_twin_matrix_2_3
 _jana_cell_twin_matrix_3_1
 _jana_cell_twin_matrix_3_2
 _jana_cell_twin_matrix_3_3
1 0.4364(17)
1 0 0
0 1 0
0 0 1
2 0.5636(17)
-1 0 0
-1 1 0
0 0 -1
_cell_formula_units_Z                    2

_cell_measurement_reflns_used            ?
_cell_measurement_theta_min              ?
_cell_measurement_theta_max              ?
_cell_measurement_temperature            293
_cell_special_details
; ?
;

_exptl_crystal_density_diffrn            2.7522
_exptl_crystal_density_meas              ?
_exptl_crystal_density_method            ?
_exptl_crystal_F_000                     556

_exptl_absorpt_coefficient_mu            0.82
_exptl_crystal_description               needle
_exptl_crystal_size_max                  0.420
_exptl_crystal_size_mid                  0.140
_exptl_crystal_size_min                  0.100
_exptl_crystal_size_rad                  ?
_exptl_crystal_colour                    colorless
_exptl_absorpt_correction_type           gaussian
_exptl_absorpt_process_details           ?
_exptl_absorpt_correction_T_min          0.7784
_exptl_absorpt_correction_T_max          0.9328
#=======================================================================

# 7. EXPERIMENTAL DATA

_exptl_special_details                   ?

_diffrn_ambient_temperature              293
_diffrn_source                           ?
_diffrn_source_power                     ?
_diffrn_source_voltage                   ?
_diffrn_source_current                   ?
_diffrn_radiation_type                   'Mo K\a'
_diffrn_radiation_source                 'X-ray tube'
_diffrn_radiation_wavelength             0.71073
_diffrn_radiation_monochromator          graphite
_diffrn_measurement_device               'four-cycle diffractometer'
_diffrn_measurement_device_type          'Bruker CCD'
_diffrn_detector                         ?
_diffrn_detector_area_resol_mean         ?
_diffrn_measurement_method               ?
_diffrn_measurement_specimen_support     ?

_diffrn_reflns_number                    5888
_diffrn_reflns_theta_min                 1.86
_diffrn_reflns_theta_max                 27.82
_diffrn_reflns_theta_full                27.82
_diffrn_measured_fraction_theta_max      0.99
_diffrn_measured_fraction_theta_full     0.99
_diffrn_reflns_av_R_equivalents          0.0519
_diffrn_reflns_av_sigmaI/netI            0.0289
_diffrn_reflns_limit_h_min               -15
_diffrn_reflns_limit_h_max               16
_diffrn_reflns_limit_k_min               -16
_diffrn_reflns_limit_k_max               16
_diffrn_reflns_limit_l_min               -6
_diffrn_reflns_limit_l_max               6
_diffrn_reflns_reduction_process         ?

_diffrn_standards_number                 ?
_diffrn_standards_interval_count         ?
_diffrn_standards_interval_time          ?
_diffrn_standards_decay_%                ?
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
  ? ? ?

#=======================================================================

# 8. REFINEMENT DATA

_refine_special_details
; ?
;

_reflns_number_total                     1084
_reflns_number_gt                        1080
_reflns_threshold_expression             'I>0σ(I)'

_refine_ls_structure_factor_coef         Fsqd
_refine_ls_R_factor_gt                   0.0220
_refine_ls_wR_factor_gt                  0.0519
_refine_ls_R_factor_all                  0.0220
_refine_ls_wR_factor_ref                 0.0519
_refine_ls_goodness_of_fit_ref           1.18
_refine_ls_goodness_of_fit_gt            1.18
_refine_ls_restrained_S_gt               ?
_refine_ls_restrained_S_all              ?
_refine_ls_number_reflns                 1080
_refine_ls_number_parameters             107
_refine_ls_number_restraints             0
_refine_ls_number_constraints            1
_refine_ls_weighting_scheme              sigma
_refine_ls_weighting_details             'w=1/(σ²(I)+0.0009I²)'
_refine_ls_hydrogen_treatment            ?
_refine_ls_shift/su_max                  0.0003
_refine_ls_shift/su_mean                 0.0000
_refine_diff_density_max                 0.19
_refine_diff_density_min                 -0.30
_refine_ls_extinction_method
 'B-C type 1 Gaussian isotropic (Becker & Coppens, 1974)'
_refine_ls_extinction_coef               700(500)
_refine_ls_abs_structure_details         ?
_refine_ls_abs_structure_Flack           ?
_refine_ls_abs_structure_Rogers          ?

loop_
 _atom_type_symbol
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 F   0.0171  0.0103
 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
 Li -0.0003  0.0001
 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
 Mg  0.0486  0.0363
 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
 O   0.0106  0.0060
 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
 P   0.1023  0.0942
 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'

_computing_data_collection               ?
_computing_cell_refinement               ?
_computing_data_reduction                ?
_computing_structure_solution            ?
_computing_structure_refinement          ?
_computing_molecular_graphics            ?
_computing_publication_material          ?

#=======================================================================

# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_adp_type
 _atom_site_U_iso_or_equiv
 _atom_site_symmetry_multiplicity
 _atom_site_occupancy
 _atom_site_calc_flag
 _atom_site_refinement_flags
 _atom_site_disorder_assembly
 _atom_site_disorder_group
  Li1 Li 0.0835(5) 0.9160(5) 0.3461(12) Uani 0.020(2) 6 1 d . . .
  Li2 Li 0.5706(6) 0.1748(5) 0.2996(12) Uani 0.027(2) 6 1 d . . .
  Li3 Li 0.4209(4) 0.0862(3) 0.7711(18) Uani 0.0049(14) 6 1 d . . .
  Mg1 Mg 0.35849(8) 0.93255(8) 0.2687(4) Uani 0.0091(3) 6 1 d . . .
  P1 P 0.31899(5) 0.16576(5) 0.254236 Uani 0.0077(2) 6 1 d . . .
  P2 P 0.666667 0.333333 0.7954(2) Uani 0.0077(3) 2 1 d . . .
  O1 O 0.59815(19) 0.39568(20) 0.6860(4) Uani 0.0105(7) 6 1 d . . .
  O2 O 0.17791(13) 0.08608(18) 0.2531(5) Uani 0.0129(7) 6 1 d . . .
  O3 O 0.37792(19) 0.09711(17) 0.3819(4) Uani 0.0121(8) 6 1 d . . .
  O4 O 0.3581(2) 0.28440(17) 0.4062(4) Uani 0.0127(8) 6 1 d . . .
  O5 O 0.36001(17) 0.19409(16) 0.9581(4) Uani 0.0116(7) 6 1 d . . .
  O6 O 0.666667 0.333333 0.1022(7) Uani 0.0133(8) 2 1 d . . .
  F1 F 0.52264(13) 0.03892(12) 0.0741(3) Uani 0.0128(6) 6 1 d . . .



#=======================================================================

# 10. MOLECULAR GEOMETRY


loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_site_symmetry_1
 _geom_bond_site_symmetry_2
 _geom_bond_distance
 _geom_bond_publ_flag
  Li1 P1 . 5_565 2.631(7) ?
  Li1 O2 . 1_565 1.920(6) ?
  Li1 O2 . 3_565 1.973(6) ?
  Li1 O2 . 5_565 2.042(6) ?
  Li1 O5 . 5_564 2.184(8) ?
  Li2 O1 . 2_655 1.975(6) ?
  Li2 O3 . . 2.159(7) ?
  Li2 O4 . 2_655 2.754(9) ?
  Li2 O6 . . 2.006(5) ?
  Li2 F1 . . 1.882(6) ?
  Li2 F1 . 4_655 2.715(6) ?
  Li3 O1 . 2_655 2.072(4) ?
  Li3 O3 . . 2.046(9) ?
  Li3 O4 . 5_555 2.005(5) ?
  Li3 O5 . . 2.089(7) ?
  Li3 F1 . 1_556 2.252(7) ?
  Li3 F1 . 4_655 2.258(6) ?
  Mg1 O1 . 5_564 2.023(4) ?
  Mg1 O3 . 1_565 2.045(3) ?
  Mg1 O4 . 5_564 2.026(3) ?
  Mg1 O5 . 5_564 2.041(2) ?
  Mg1 F1 . 1_565 2.0642(18) ?
  Mg1 F1 . 4_665 2.044(2) ?
  P1 O2 . . 1.5456(15) ?
  P1 O3 . . 1.535(3) ?
  P1 O4 . . 1.525(2) ?
  P1 O5 . 1_554 1.553(2) ?
  P2 O1 . . 1.532(3) ?
  P2 O1 . 2_655 1.532(3) ?
  P2 O1 . 3_665 1.532(3) ?
  P2 O6 . 1_556 1.536(4) ?
  O1 O1 . 2_655 2.477(5) ?
  O1 O1 . 3_665 2.477(4) ?
  O1 O6 . 1_556 2.528(4) ?
  O1 F1 . 3_666 2.640(3) ?
  O1 F1 . 6_555 2.697(4) ?
  O2 O3 . . 2.540(3) ?
  O2 O4 . . 2.515(2) ?
  O2 O5 . 1_554 2.487(3) ?
  O3 O4 . . 2.500(4) ?
  O3 O5 . 1_554 2.516(3) ?
  O3 F1 . . 2.755(3) ?
  O3 F1 . 4_655 2.757(3) ?
  O4 O5 . 1_554 2.522(3) ?
  O4 F1 . 3_665 2.796(2) ?
  O4 F1 . 6_555 2.737(2) ?
  F1 F1 . 4_654 2.646(2) ?
  F1 F1 . 4_655 2.646(2) ?

loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_2
 _geom_angle_site_symmetry_3
 _geom_angle
 _geom_angle_publ_flag
  O2 Li1 O2 1_565 . 3_565 119.8(4) ?
  O2 Li1 O2 1_565 . 5_565 106.3(3) ?
  O2 Li1 O5 1_565 . 5_564 113.9(3) ?
  O2 Li1 O2 3_565 . 5_565 104.3(3) ?
  O2 Li1 O5 3_565 . 5_564 124.5(3) ?
  O2 Li1 O5 5_565 . 5_564 72.0(2) ?
  O1 Li2 O3 2_655 . . 89.3(3) ?
  O1 Li2 O4 2_655 . 2_655 76.0(3) ?
  O1 Li2 O6 2_655 . . 109.7(3) ?
  O1 Li2 F1 2_655 . . 133.8(4) ?
  O1 Li2 F1 2_655 . 4_655 68.14(19) ?
  O3 Li2 O4 . . 2_655 127.7(2) ?
  O3 Li2 O6 . . . 121.9(4) ?
  O3 Li2 F1 . . . 85.7(2) ?
  O3 Li2 F1 . . 4_655 67.79(15) ?
  O4 Li2 O6 2_655 . . 110.3(3) ?
  O4 Li2 F1 2_655 . . 71.4(3) ?
  O4 Li2 F1 2_655 . 4_655 60.05(16) ?
  O6 Li2 F1 . . . 111.8(3) ?
  O6 Li2 F1 . . 4_655 170.3(4) ?
  F1 Li2 F1 . . 4_655 67.50(17) ?
  O1 Li3 O3 2_655 . . 89.8(3) ?
  O1 Li3 O4 2_655 . 5_555 151.1(3) ?
  O1 Li3 O5 2_655 . . 106.0(2) ?
  O1 Li3 F1 2_655 . 1_556 75.13(19) ?
  O1 Li3 F1 2_655 . 4_655 76.9(2) ?
  O3 Li3 O4 . . 5_555 105.4(3) ?
  O3 Li3 O5 . . . 100.8(3) ?
  O3 Li3 F1 . . 1_556 149.9(3) ?
  O3 Li3 F1 . . 4_655 79.5(3) ?
  O4 Li3 O5 5_555 . . 95.4(3) ?
  O4 Li3 F1 5_555 . 1_556 79.8(3) ?
  O4 Li3 F1 5_555 . 4_655 81.75(18) ?
  O5 Li3 F1 . . 1_556 108.3(4) ?
  O5 Li3 F1 . . 4_655 177.1(2) ?
  F1 Li3 F1 1_556 . 4_655 71.85(18) ?
  O1 Mg1 O3 5_564 . 1_565 161.98(10) ?
  O1 Mg1 O4 5_564 . 5_564 94.61(13) ?
  O1 Mg1 O5 5_564 . 5_564 100.11(11) ?
  O1 Mg1 F1 5_564 . 1_565 82.59(9) ?
  O1 Mg1 F1 5_564 . 4_665 80.96(9) ?
  O3 Mg1 O4 1_565 . 5_564 96.12(13) ?
  O3 Mg1 O5 1_565 . 5_564 93.36(12) ?
  O3 Mg1 F1 1_565 . 1_565 84.19(8) ?
  O3 Mg1 F1 1_565 . 4_665 84.77(10) ?
  O4 Mg1 O5 5_564 . 5_564 94.83(9) ?
  O4 Mg1 F1 5_564 . 1_565 83.99(10) ?
  O4 Mg1 F1 5_564 . 4_665 163.99(10) ?
  O5 Mg1 F1 5_564 . 1_565 177.14(12) ?
  O5 Mg1 F1 5_564 . 4_665 101.09(11) ?
  F1 Mg1 F1 1_565 . 4_665 80.19(7) ?
  O2 P1 O3 . . . 111.08(11) ?
  O2 P1 O4 . . . 110.03(14) ?
  O2 P1 O5 . . 1_554 106.81(12) ?
  O3 P1 O4 . . . 109.62(12) ?
  O3 P1 O5 . . 1_554 109.16(13) ?
  O4 P1 O5 . . 1_554 110.11(11) ?
  O1 P2 O1 . . 2_655 107.93(14) ?
  O1 P2 O1 . . 3_665 107.93(14) ?
  O1 P2 O6 . . 1_556 110.97(9) ?
  O1 P2 O1 2_655 . 3_665 107.94(13) ?
  O1 P2 O6 2_655 . 1_556 110.97(9) ?
  O1 P2 O6 3_665 . 1_556 110.97(9) ?

loop_
 _geom_torsion_atom_site_label_1
 _geom_torsion_atom_site_label_2
 _geom_torsion_atom_site_label_3
 _geom_torsion_atom_site_label_4
 _geom_torsion_site_symmetry_1
 _geom_torsion_site_symmetry_2
 _geom_torsion_site_symmetry_3
 _geom_torsion_site_symmetry_4
 _geom_torsion
 _geom_torsion_publ_flag
 ? ? ? ? ? ? ? ? ? ?

loop_
 _geom_hbond_atom_site_label_D
 _geom_hbond_atom_site_label_H
 _geom_hbond_atom_site_label_A
 _geom_hbond_site_symmetry_D
 _geom_hbond_site_symmetry_H
 _geom_hbond_site_symmetry_A
 _geom_hbond_distance_DH
 _geom_hbond_distance_HA
 _geom_hbond_distance_DA
 _geom_hbond_angle_DHA
 _geom_hbond_publ_flag
 ? ? ? ? ? ? ? ? ? ? ?


#=======================================================================

# 11. STRUCTURE-FACTOR LIST

