# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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. 
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data_22
_database_code_depnum_ccdc_archive 'CCDC 1874768'
_audit_update_record             
;
2018-12-26 deposited with the CCDC.
2019-01-15 downloaded from the CCDC.
;
_audit_creation_date             2018-11-07
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.06(F32 Li16 O32 P16)'
_chemical_formula_sum            'F2 Li O2 P'
_chemical_formula_weight         107.91
_chemical_melting_point          ?
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'
F F 0.0171 0.0103 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_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'
'-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                   9.672(8)
_cell_length_b                   19.310(15)
_cell_length_c                   8.055(6)
_cell_angle_alpha                90
_cell_angle_beta                 108.567(8)
_cell_angle_gamma                90
_cell_volume                     1426.0(19)
_cell_formula_units_Z            16
_cell_measurement_reflns_used    814
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.21
_cell_measurement_theta_min      2.46
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.651
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6543
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0510 before and 0.0407 after correction.
The Ratio of minimum to maximum transmission is 0.8775.
The λ/2 correction factor is 0.0015.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.011
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.123
_exptl_crystal_size_mid          0.106
_exptl_crystal_size_min          0.074
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0263
_diffrn_reflns_av_unetI/netI     0.0323
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            4295
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.404
_diffrn_reflns_theta_min         2.109
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1101
_reflns_number_total             1618
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.540
_refine_diff_density_min         -0.466
_refine_diff_density_rms         0.067
_refine_ls_extinction_coef       0.0029(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     111
_refine_ls_number_reflns         1618
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0730
_refine_ls_R_factor_gt           0.0482
_refine_ls_restrained_S_all      1.048
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0656P)²+2.1741P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1314
_refine_ls_wR_factor_ref         0.1535
_refine_special_details          ?
_olex2_refinement_description    
;
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.500000 0.81025(5) 0.750000 0.0375(4) Uani 1 2 d S T P . .
P2 P 0.26362(9) 0.56316(4) 0.73976(11) 0.0400(3) Uani 1 1 d . . . . .
P3 P 0.500000 0.31217(6) 0.750000 0.0465(4) Uani 1 2 d S T P . .
F1 F 0.4414(3) 0.86112(13) 0.8543(3) 0.1028(10) Uani 1 1 d . . . . .
F2 F 0.1815(3) 0.61313(14) 0.8185(4) 0.1002(10) Uani 1 1 d . . . . .
F3 F 0.1439(3) 0.51193(14) 0.6542(3) 0.1004(10) Uani 1 1 d . . . . .
F4 F 0.6097(4) 0.26115(16) 0.8550(5) 0.1487(16) Uani 1 1 d . . . . .
O1 O 0.3769(2) 0.77274(9) 0.6302(2) 0.0374(5) Uani 1 1 d . . . . .
O2 O 0.3067(2) 0.59965(10) 0.6039(3) 0.0412(6) Uani 1 1 d . . . . .
O3 O 0.3757(2) 0.52739(10) 0.8799(3) 0.0449(6) Uani 1 1 d . . . . .
O4 O 0.4360(3) 0.34907(10) 0.8663(3) 0.0444(6) Uani 1 1 d . . . . .
Li1 Li 0.3151(5) 0.6882(2) 0.5019(6) 0.0367(11) Uani 1 1 d . . . . .
Li2 Li 0.4325(6) 0.4373(2) 0.9761(6) 0.0394(12) Uani 1 1 d . . . . .


_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
P1 F1 1.515(2) 2_656 ?
P1 F1 1.515(2) . ?
P1 O1 1.464(2) . ?
P1 O1 1.464(2) 2_656 ?
P1 Li1 3.077(5) 7_566 ?
P1 Li1 3.077(5) 8_566 ?
P2 F2 1.512(2) . ?
P2 F3 1.512(2) . ?
P2 O2 1.469(2) . ?
P2 O3 1.465(2) . ?
P2 Li2 3.064(6) 6_565 ?
P2 Li2 3.097(6) 5_667 ?
P3 F4 1.497(3) 2_656 ?
P3 F4 1.497(3) . ?
P3 O4 1.462(2) . ?
P3 O4 1.462(2) 2_656 ?
P3 Li1 3.103(5) 6_566 ?
P3 Li1 3.103(5) 5_666 ?
O1 Li1 1.973(5) 7_566 ?
O1 Li1 1.922(5) . ?
O2 Li1 1.910(5) . ?
O2 Li2 1.962(6) 6_565 ?
O3 Li2 1.969(6) 5_667 ?
O3 Li2 1.912(5) . ?
O4 Li1 1.973(5) 6_566 ?
O4 Li2 1.926(5) . ?
Li1 Li1 2.694(9) 7_566 ?
Li1 Li2 2.713(7) 6_565 ?
Li2 Li2 2.718(9) 5_667 ?

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
F1 P1 F1 99.2(3) . 2_656 ?
F1 P1 Li1 83.82(14) 2_656 8_566 ?
F1 P1 Li1 83.82(14) . 7_566 ?
F1 P1 Li1 95.46(14) . 8_566 ?
F1 P1 Li1 95.46(14) 2_656 7_566 ?
O1 P1 F1 108.47(14) 2_656 2_656 ?
O1 P1 F1 108.96(14) 2_656 . ?
O1 P1 F1 108.96(14) . 2_656 ?
O1 P1 F1 108.47(14) . . ?
O1 P1 O1 120.67(17) 2_656 . ?
O1 P1 Li1 150.07(12) . 8_566 ?
O1 P1 Li1 31.01(12) 2_656 8_566 ?
O1 P1 Li1 31.01(12) . 7_566 ?
O1 P1 Li1 150.07(12) 2_656 7_566 ?
Li1 P1 Li1 178.89(17) 8_566 7_566 ?
F2 P2 F3 100.4(2) . . ?
F2 P2 Li2 101.16(16) . 5_667 ?
F2 P2 Li2 139.48(14) . 6_565 ?
F3 P2 Li2 138.04(14) . 5_667 ?
F3 P2 Li2 100.47(16) . 6_565 ?
O2 P2 F2 108.53(14) . . ?
O2 P2 F3 109.37(15) . . ?
O2 P2 Li2 97.15(14) . 5_667 ?
O2 P2 Li2 31.24(12) . 6_565 ?
O3 P2 F2 109.67(15) . . ?
O3 P2 F3 108.31(15) . . ?
O3 P2 O2 118.95(15) . . ?
O3 P2 Li2 96.03(15) . 6_565 ?
O3 P2 Li2 30.01(12) . 5_667 ?
Li2 P2 Li2 85.53(15) 6_565 5_667 ?
F4 P3 F4 97.7(4) . 2_656 ?
F4 P3 Li1 94.67(15) . 6_566 ?
F4 P3 Li1 94.67(15) 2_656 5_666 ?
F4 P3 Li1 85.15(15) 2_656 6_566 ?
F4 P3 Li1 85.15(15) . 5_666 ?
O4 P3 F4 108.31(16) 2_656 . ?
O4 P3 F4 108.31(16) . 2_656 ?
O4 P3 F4 109.11(16) 2_656 2_656 ?
O4 P3 F4 109.12(16) . . ?
O4 P3 O4 121.67(18) 2_656 . ?
O4 P3 Li1 150.45(13) . 5_666 ?
O4 P3 Li1 150.45(13) 2_656 6_566 ?
O4 P3 Li1 29.81(12) 2_656 5_666 ?
O4 P3 Li1 29.81(12) . 6_566 ?
Li1 P3 Li1 179.73(17) 6_566 5_666 ?
P1 O1 Li1 145.38(19) . . ?
P1 O1 Li1 126.51(19) . 7_566 ?
Li1 O1 Li1 87.5(2) . 7_566 ?
P2 O2 Li1 144.2(2) . . ?
P2 O2 Li2 125.92(19) . 6_565 ?
Li1 O2 Li2 88.9(2) . 6_565 ?
P2 O3 Li2 128.14(19) . 5_667 ?
P2 O3 Li2 142.0(2) . . ?
Li2 O3 Li2 88.9(2) . 5_667 ?
P3 O4 Li1 128.57(19) . 6_566 ?
P3 O4 Li2 143.0(2) . . ?
Li2 O4 Li1 88.2(2) . 6_566 ?
P1 Li1 P3 102.99(16) 7_566 5_666 ?
O1 Li1 P1 114.79(19) . 7_566 ?
O1 Li1 P1 22.47(9) 7_566 7_566 ?
O1 Li1 P3 102.0(2) . 5_666 ?
O1 Li1 P3 106.7(2) 7_566 5_666 ?
O1 Li1 O1 92.5(2) . 7_566 ?
O1 Li1 O4 117.6(3) 7_566 6_565 ?
O1 Li1 O4 118.0(3) . 6_565 ?
O1 Li1 Li1 47.02(16) . 7_566 ?
O1 Li1 Li1 45.47(15) 7_566 7_566 ?
O1 Li1 Li2 137.2(3) . 6_565 ?
O1 Li1 Li2 130.2(3) 7_566 6_565 ?
O2 Li1 P1 97.1(2) . 7_566 ?
O2 Li1 P3 113.1(2) . 5_666 ?
O2 Li1 O1 125.3(3) . . ?
O2 Li1 O1 114.4(3) . 7_566 ?
O2 Li1 O4 91.5(2) . 6_565 ?
O2 Li1 Li1 135.6(4) . 7_566 ?
O2 Li1 Li2 46.31(16) . 6_565 ?
O4 Li1 P1 106.0(2) 6_565 7_566 ?
O4 Li1 P3 21.62(9) 6_565 5_666 ?
O4 Li1 Li1 132.4(3) 6_565 7_566 ?
O4 Li1 Li2 45.19(16) 6_565 6_565 ?
Li1 Li1 P1 67.8(2) 7_566 7_566 ?
Li1 Li1 P3 111.1(3) 7_566 5_666 ?
Li1 Li1 Li2 175.0(3) 7_566 6_565 ?
Li2 Li1 P1 108.0(2) 6_565 7_566 ?
Li2 Li1 P3 66.76(17) 6_565 5_666 ?
P2 Li2 P2 94.47(15) 6_566 5_667 ?
O2 Li2 P2 102.3(2) 6_566 5_667 ?
O2 Li2 P2 22.84(9) 6_566 6_566 ?
O2 Li2 O3 116.2(3) 6_566 5_667 ?
O2 Li2 Li1 44.75(16) 6_566 6_566 ?
O2 Li2 Li2 126.9(3) 6_566 5_667 ?
O3 Li2 P2 101.7(2) 5_667 6_566 ?
O3 Li2 P2 21.84(9) 5_667 5_667 ?
O3 Li2 P2 97.8(2) . 6_566 ?
O3 Li2 P2 112.6(2) . 5_667 ?
O3 Li2 O2 113.4(3) . 6_566 ?
O3 Li2 O3 91.1(2) . 5_667 ?
O3 Li2 O4 131.6(3) . . ?
O3 Li2 Li1 140.4(3) . 6_566 ?
O3 Li2 Li1 127.1(3) 5_667 6_566 ?
O3 Li2 Li2 46.42(16) . 5_667 ?
O3 Li2 Li2 44.69(16) 5_667 5_667 ?
O4 Li2 P2 100.7(2) . 5_667 ?
O4 Li2 P2 114.0(2) . 6_566 ?
O4 Li2 O2 91.3(2) . 6_566 ?
O4 Li2 O3 115.2(3) . 5_667 ?
O4 Li2 Li1 46.62(16) . 6_566 ?
O4 Li2 Li2 140.8(4) . 5_667 ?
Li1 Li2 P2 67.39(16) 6_566 6_566 ?
Li1 Li2 P2 105.2(2) 6_566 5_667 ?
Li1 Li2 Li2 168.1(3) 6_566 5_667 ?
Li2 Li2 P2 104.0(3) 5_667 6_566 ?
Li2 Li2 P2 66.3(2) 5_667 5_667 ?

_olex2_submission_special_instructions 'No special instructions were received'
