# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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_sad
_audit_block_doi                 10.5517/cc13pjnz
_database_code_depnum_ccdc_archive 'CCDC 1033591'
_audit_update_record             
;
2014-11-11 deposited with the CCDC.
2015-03-02 downloaded from the CCDC.
;
_audit_creation_date             2014-11-05
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'0.5(C24 H60 Al2 F24 Li6 O30 P12), 0.14(C4 H10 O)'
_chemical_formula_sum            'C12.55 H31.38 Al F12 Li3 O15.14 P6'
_chemical_formula_weight         886.21
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Al Al 0.0645 0.0514 '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      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3'
_space_group_name_Hall           '-R 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   17.4058(4)
_cell_length_b                   17.4058(4)
_cell_length_c                   21.4947(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     5639.6(3)
_cell_formula_units_Z            6
_cell_measurement_reflns_used    6176
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.735
_cell_measurement_theta_min      2.340
_shelx_estimated_absorpt_T_max   0.936
_shelx_estimated_absorpt_T_min   0.928
_exptl_absorpt_coefficient_mu    0.422
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6659
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.1247 before and 0.0431 after correction. The Ratio of minimum to maximum transmission is 0.8926. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.566
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2687
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.16
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0329
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            22369
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.011
_diffrn_reflns_theta_min         2.843
_diffrn_ambient_temperature      100
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker Smart APEX II Quazar'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2953
_reflns_number_total             3662
_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, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2008)'
_refine_diff_density_max         0.420
_refine_diff_density_min         -0.331
_refine_diff_density_rms         0.056
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     188
_refine_ls_number_reflns         3662
_refine_ls_number_restraints     184
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_gt           0.0337
_refine_ls_restrained_S_all      1.076
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0358P)²+7.2552P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0824
_refine_ls_wR_factor_ref         0.0883
_refine_special_details          ?
_olex2_refinement_description    
;
1. Others
 Fixed Sof: C1C(0.046) H1CA(0.046) H1CB(0.046) H1CC(0.046) C2C(0.046)
 H2CA(0.046) H2CB(0.046) O3C(0.046) C4C(0.046) H4CA(0.046) H4CB(0.046)
 C5C(0.046) H5CA(0.046) H5CB(0.046) H5CC(0.046)
 Fixed U13: Al1(0)
 Fixed U23: Al1(0)
 Fixed Uiso: H1A(0.053) H1B(0.053) H2A(0.084) H2B(0.084) H2C(0.084) H3A(0.046)
 H3B(0.046) H4A(0.068) H4B(0.068) H4C(0.068) C1C(0.05) H1CA(0.075) H1CB(0.075)
 H1CC(0.075) C2C(0.05) H2CA(0.06) H2CB(0.06) O3C(0.05) C4C(0.05) H4CA(0.06)
 H4CB(0.06) C5C(0.05) H5CA(0.075) H5CB(0.075) H5CC(0.075)
 Fixed X: Al1(0.3333) H1A(0.7665) H1B(0.7249) H2A(0.6661) H2B(0.7075)
 H2C(0.6108) H3A(0.6966) H3B(0.5985) H4A(0.591) H4B(0.5447) H4C(0.6424)
 H1CA(0.3004) H1CB(0.2908) H1CC(0.3852) H2CA(0.2367) H2CB(0.3318) H4CA(0.3361)
 H4CB(0.2535) H5CA(0.3665) H5CB(0.4339) H5CC(0.3521)
 Fixed Y: Al1(0.6667) H1A(0.7141) H1B(0.727) H2A(0.5653) H2B(0.5887)
 H2C(0.5748) H3A(0.6937) H3B(0.617) H4A(0.7035) H4B(0.7145) H4C(0.7906)
 H1CA(0.6322) H1CB(0.7062) H1CC(0.7118) H2CA(0.5778) H2CB(0.5835) H4CA(0.5814)
 H4CB(0.5941) H5CA(0.6596) H5CB(0.7208) H5CC(0.7334)
 Fixed Z: H1A(0.415) H1B(0.3523) H2A(0.4166) H2B(0.3481) H2C(0.3607)
 H3A(0.5088) H3B(0.4904) H4A(0.5709) H4B(0.5099) H4C(0.5288) H1CA(0.5197)
 H1CB(0.5574) H1CC(0.5528) H2CA(0.6168) H2CB(0.6121) H4CA(0.7063) H4CB(0.7257)
 H5CA(0.8004) H5CB(0.7473) H5CC(0.7665)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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
P2 P 0.20264(2) 0.48935(2) 0.26850(2) 0.01685(9) Uani 1 1 d . . . . .
Al1 Al 0.3333 0.6667 0.34100(3) 0.01606(15) Uani 1 3 d S T P A .
P1A P 0.4629(3) 0.8348(4) 0.4229(3) 0.0243(5) Uani 0.623(17) 1 d D U P A 1
F1A F 0.4808(3) 0.9258(2) 0.4015(5) 0.0597(16) Uani 0.623(17) 1 d D U P A 1
F2A F 0.4401(3) 0.8401(7) 0.4909(3) 0.0685(19) Uani 0.623(17) 1 d D U P A 1
P1B P 0.4573(5) 0.8218(5) 0.4295(4) 0.0243(5) Uani 0.377(17) 1 d D U P A 2
F1B F 0.4255(5) 0.7929(10) 0.4959(3) 0.057(2) Uani 0.377(17) 1 d D U P A 2
F2B F 0.4678(5) 0.9140(6) 0.4332(6) 0.054(2) Uani 0.377(17) 1 d D U P A 2
F3 F 0.13018(6) 0.51477(6) 0.26543(5) 0.0298(2) Uani 1 1 d . . . . .
F4 F 0.21291(7) 0.47718(7) 0.19903(4) 0.0329(2) Uani 1 1 d . . . . .
O1 O 0.65357(8) 0.71513(8) 0.42814(6) 0.0337(3) Uani 1 1 d . . . . .
O2 O 0.54336(7) 0.82944(8) 0.42000(5) 0.0290(3) Uani 1 1 d D U . . .
O3 O 0.38012(7) 0.76882(7) 0.39098(5) 0.0225(2) Uani 1 1 d D U . . .
O4 O 0.28593(6) 0.56594(6) 0.28998(5) 0.0193(2) Uani 1 1 d . . . . .
O5 O 0.16762(7) 0.40346(6) 0.30001(5) 0.0215(2) Uani 1 1 d . . . . .
C1 C 0.71034(14) 0.69385(14) 0.39205(11) 0.0444(5) Uani 1 1 d . . . . .
H1A H 0.7665 0.7141 0.4150 0.053 Uiso 1 1 calc R U . . .
H1B H 0.7249 0.7270 0.3523 0.053 Uiso 1 1 calc R U . . .
C2 C 0.67025(17) 0.59739(16) 0.37818(11) 0.0558(6) Uani 1 1 d . . . . .
H2A H 0.6661 0.5653 0.4166 0.084 Uiso 1 1 calc R U . . .
H2B H 0.7075 0.5887 0.3481 0.084 Uiso 1 1 calc R U . . .
H2C H 0.6108 0.5748 0.3607 0.084 Uiso 1 1 calc R U . . .
C3 C 0.63955(13) 0.68194(13) 0.49046(8) 0.0384(4) Uani 1 1 d . . . . .
H3A H 0.6966 0.6937 0.5088 0.046 Uiso 1 1 calc R U . . .
H3B H 0.5985 0.6170 0.4904 0.046 Uiso 1 1 calc R U . . .
C4 C 0.60112(14) 0.72644(14) 0.52826(9) 0.0454(5) Uani 1 1 d . . . . .
H4A H 0.5910 0.7035 0.5709 0.068 Uiso 1 1 calc R U . . .
H4B H 0.5447 0.7145 0.5099 0.068 Uiso 1 1 calc R U . . .
H4C H 0.6424 0.7906 0.5288 0.068 Uiso 1 1 calc R U . . .
Li1 Li 0.62271(17) 0.79664(18) 0.38871(12) 0.0242(5) Uani 1 1 d . . . . .
C1C C 0.321(5) 0.672(6) 0.5560(15) 0.050 Uiso 0.046 1 d D U P B -1
H1CA H 0.3004 0.6322 0.5197 0.075 Uiso 0.046 1 calc R U P B -1
H1CB H 0.2908 0.7062 0.5574 0.075 Uiso 0.046 1 calc R U P B -1
H1CC H 0.3852 0.7118 0.5528 0.075 Uiso 0.046 1 calc R U P B -1
C2C C 0.301(4) 0.619(3) 0.6124(18) 0.050 Uiso 0.046 1 d D U P B -1
H2CA H 0.2367 0.5778 0.6168 0.060 Uiso 0.046 1 calc R U P B -1
H2CB H 0.3318 0.5835 0.6121 0.060 Uiso 0.046 1 calc R U P B -1
O3C O 0.334(7) 0.682(3) 0.6613(13) 0.050 Uiso 0.046 1 d D U P B -1
C4C C 0.317(4) 0.625(2) 0.7139(17) 0.050 Uiso 0.046 1 d D U P B -1
H4CA H 0.3361 0.5814 0.7063 0.060 Uiso 0.046 1 calc R U P B -1
H4CB H 0.2535 0.5941 0.7257 0.060 Uiso 0.046 1 calc R U P B -1
C5C C 0.372(3) 0.690(3) 0.7609(18) 0.050 Uiso 0.046 1 d D U P B -1
H5CA H 0.3665 0.6596 0.8004 0.075 Uiso 0.046 1 calc R U P B -1
H5CB H 0.4339 0.7208 0.7473 0.075 Uiso 0.046 1 calc R U P B -1
H5CC H 0.3521 0.7334 0.7665 0.075 Uiso 0.046 1 calc R U P B -1


_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
P2 F3 1.5326(9) . ?
P2 F4 1.5313(10) . ?
P2 O4 1.4695(10) . ?
P2 O5 1.4676(10) . ?
Al1 O3 1.8791(11) . ?
Al1 O3 1.8791(11) 2_665 ?
Al1 O3 1.8792(11) 3_565 ?
Al1 O4 1.8737(11) 3_565 ?
Al1 O4 1.8737(11) . ?
Al1 O4 1.8737(11) 2_665 ?
P1A F1A 1.524(5) . ?
P1A F2A 1.528(5) . ?
P1A O2 1.451(5) . ?
P1A O3 1.487(5) . ?
P1B F1B 1.523(8) . ?
P1B F2B 1.522(8) . ?
P1B O2 1.451(8) . ?
P1B O3 1.449(8) . ?
O1 C1 1.443(2) . ?
O1 C3 1.431(2) . ?
O1 Li1 1.945(3) . ?
O2 Li1 1.864(3) . ?
O5 Li1 1.976(3) 18_545 ?
O5 Li1 1.976(3) 3_565 ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.491(3) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.492(3) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
Li1 O5 1.976(3) 2_665 ?
Li1 O5 1.976(3) 17 ?
C1C H1CA 0.9800 . ?
C1C H1CB 0.9800 . ?
C1C H1CC 0.9800 . ?
C1C C2C 1.46(2) . ?
C2C H2CA 0.9900 . ?
C2C H2CB 0.9900 . ?
C2C O3C 1.42(2) . ?
O3C C4C 1.43(2) . ?
C4C H4CA 0.9900 . ?
C4C H4CB 0.9900 . ?
C4C C5C 1.457(19) . ?
C5C H5CA 0.9800 . ?
C5C H5CB 0.9800 . ?
C5C H5CC 0.9800 . ?

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
F4 P2 F3 99.66(6) . . ?
O4 P2 F3 109.43(6) . . ?
O4 P2 F4 107.54(6) . . ?
O5 P2 F3 109.35(6) . . ?
O5 P2 F4 109.08(6) . . ?
O5 P2 O4 119.87(6) . . ?
O3 Al1 O3 90.56(5) . 3_565 ?
O3 Al1 O3 90.56(5) 2_665 . ?
O3 Al1 O3 90.56(5) 2_665 3_565 ?
O4 Al1 O3 89.64(4) 3_565 . ?
O4 Al1 O3 178.82(5) 3_565 3_565 ?
O4 Al1 O3 90.60(4) 3_565 2_665 ?
O4 Al1 O3 90.60(4) 2_665 . ?
O4 Al1 O3 90.60(4) . 3_565 ?
O4 Al1 O3 89.64(4) 2_665 3_565 ?
O4 Al1 O3 178.82(6) 2_665 2_665 ?
O4 Al1 O3 178.83(5) . . ?
O4 Al1 O3 89.64(4) . 2_665 ?
O4 Al1 O4 89.20(5) . 2_665 ?
O4 Al1 O4 89.20(5) 3_565 2_665 ?
O4 Al1 O4 89.20(5) . 3_565 ?
F1A P1A F2A 98.6(3) . . ?
O2 P1A F1A 110.6(3) . . ?
O2 P1A F2A 109.5(3) . . ?
O2 P1A O3 121.6(3) . . ?
O3 P1A F1A 106.2(3) . . ?
O3 P1A F2A 107.9(3) . . ?
F2B P1B F1B 97.5(6) . . ?
O2 P1B F1B 110.5(6) . . ?
O2 P1B F2B 109.6(5) . . ?
O3 P1B F1B 104.9(5) . . ?
O3 P1B F2B 106.6(5) . . ?
O3 P1B O2 124.3(6) . . ?
C1 O1 Li1 115.31(13) . . ?
C3 O1 C1 113.60(14) . . ?
C3 O1 Li1 130.46(14) . . ?
P1A O2 Li1 157.3(2) . . ?
P1B O2 Li1 155.8(3) . . ?
P1A O3 Al1 142.1(2) . . ?
P1B O3 Al1 138.9(3) . . ?
P2 O4 Al1 143.69(7) . . ?
P2 O5 Li1 129.59(10) . 3_565 ?
P2 O5 Li1 134.23(10) . 18_545 ?
Li1 O5 Li1 89.10(12) 18_545 3_565 ?
O1 C1 H1A 108.8 . . ?
O1 C1 H1B 108.8 . . ?
O1 C1 C2 113.69(18) . . ?
H1A C1 H1B 107.7 . . ?
C2 C1 H1A 108.8 . . ?
C2 C1 H1B 108.8 . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
O1 C3 H3A 109.8 . . ?
O1 C3 H3B 109.8 . . ?
O1 C3 C4 109.31(15) . . ?
H3A C3 H3B 108.3 . . ?
C4 C3 H3A 109.8 . . ?
C4 C3 H3B 109.8 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
O1 Li1 O5 108.66(14) . 2_665 ?
O1 Li1 O5 105.63(13) . 17 ?
O2 Li1 O1 125.70(15) . . ?
O2 Li1 O5 110.74(14) . 17 ?
O2 Li1 O5 109.61(13) . 2_665 ?
O5 Li1 O5 90.90(12) 17 2_665 ?
H1CA C1C H1CB 109.5 . . ?
H1CA C1C H1CC 109.5 . . ?
H1CB C1C H1CC 109.5 . . ?
C2C C1C H1CA 109.5 . . ?
C2C C1C H1CB 109.5 . . ?
C2C C1C H1CC 109.5 . . ?
C1C C2C H2CA 110.8 . . ?
C1C C2C H2CB 110.8 . . ?
H2CA C2C H2CB 108.9 . . ?
O3C C2C C1C 105(3) . . ?
O3C C2C H2CA 110.8 . . ?
O3C C2C H2CB 110.8 . . ?
C2C O3C C4C 101(3) . . ?
O3C C4C H4CA 111.6 . . ?
O3C C4C H4CB 111.6 . . ?
O3C C4C C5C 101(3) . . ?
H4CA C4C H4CB 109.4 . . ?
C5C C4C H4CA 111.6 . . ?
C5C C4C H4CB 111.6 . . ?
C4C C5C H5CA 109.5 . . ?
C4C C5C H5CB 109.5 . . ?
C4C C5C H5CC 109.5 . . ?
H5CA C5C H5CB 109.5 . . ?
H5CA C5C H5CC 109.5 . . ?
H5CB C5C H5CC 109.5 . . ?

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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
P1A O2 Li1 O1 -112.0(7) . . . . ?
P1A O2 Li1 O5 20.4(7) . . . 2_665 ?
P1A O2 Li1 O5 119.2(7) . . . 17 ?
F1A P1A O2 Li1 -104.0(9) . . . . ?
F1A P1A O3 Al1 127.3(5) . . . . ?
F2A P1A O2 Li1 148.4(8) . . . . ?
F2A P1A O3 Al1 -127.8(5) . . . . ?
P1B O2 Li1 O1 -88.2(8) . . . . ?
P1B O2 Li1 O5 143.0(8) . . . 17 ?
P1B O2 Li1 O5 44.2(8) . . . 2_665 ?
F1B P1B O2 Li1 108.3(10) . . . . ?
F1B P1B O3 Al1 -100.5(7) . . . . ?
F2B P1B O2 Li1 -145.3(8) . . . . ?
F2B P1B O3 Al1 156.7(6) . . . . ?
F3 P2 O4 Al1 32.29(13) . . . . ?
F3 P2 O5 Li1 -93.59(13) . . . 3_565 ?
F3 P2 O5 Li1 125.45(14) . . . 18_545 ?
F4 P2 O4 Al1 139.63(11) . . . . ?
F4 P2 O5 Li1 158.37(12) . . . 3_565 ?
F4 P2 O5 Li1 17.42(15) . . . 18_545 ?
O2 P1A O3 Al1 -0.2(8) . . . . ?
O2 P1B O3 Al1 27.8(9) . . . . ?
O3 Al1 O3 P1A 43.5(4) 3_565 . . . ?
O3 Al1 O3 P1A 134.1(4) 2_665 . . . ?
O3 Al1 O3 P1B 120.3(5) 2_665 . . . ?
O3 Al1 O3 P1B 29.7(5) 3_565 . . . ?
O3 Al1 O4 P2 26.06(12) 2_665 . . . ?
O3 Al1 O4 P2 116.61(12) 3_565 . . . ?
O3 P1A O2 Li1 21.5(11) . . . . ?
O3 P1B O2 Li1 -17.6(13) . . . . ?
O4 P2 O5 Li1 -107.08(14) . . . 18_545 ?
O4 P2 O5 Li1 33.87(15) . . . 3_565 ?
O4 Al1 O3 P1A -135.3(4) 3_565 . . . ?
O4 Al1 O3 P1A -46.1(4) 2_665 . . . ?
O4 Al1 O3 P1B -149.1(5) 3_565 . . . ?
O4 Al1 O3 P1B -59.9(5) 2_665 . . . ?
O4 Al1 O4 P2 -153.76(10) 2_665 . . . ?
O4 Al1 O4 P2 -64.55(14) 3_565 . . . ?
O5 P2 O4 Al1 -95.14(12) . . . . ?
C1 O1 C3 C4 165.23(16) . . . . ?
C3 O1 C1 C2 67.8(2) . . . . ?
Li1 O1 C1 C2 -120.35(18) . . . . ?
Li1 O1 C3 C4 -5.1(2) . . . . ?
C1C C2C O3C C4C -177(5) . . . . ?
C2C O3C C4C C5C 165(6) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_p21c
_audit_block_doi                 10.5517/cc13pjx7
_database_code_depnum_ccdc_archive 'CCDC 1033599'
_audit_update_record             
;
2014-11-11 deposited with the CCDC.
2015-03-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'B F8 O8 P4, Li'
_chemical_formula_sum            'B F8 Li O8 P4'
_chemical_formula_weight         421.63

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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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.
;

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

_cell_length_a                   7.9074(2)
_cell_length_b                   14.0602(4)
_cell_length_c                   13.7851(3)
_cell_angle_alpha                90
_cell_angle_beta                 121.9130(10)
_cell_angle_gamma                90
_cell_volume                     1300.97(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.153
_exptl_crystal_F_000             816
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.714
_shelx_estimated_absorpt_T_min   0.913
_shelx_estimated_absorpt_T_max   0.932
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.715
_exptl_absorpt_correction_T_max  0.747
_exptl_absorpt_process_details   'SADABS 2008/1'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'INCOATEC Mo-Microsource'
_diffrn_measurement_device_type  'Bruker Smart APEXII'
_diffrn_measurement_method       'Omega Scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            38648
_diffrn_reflns_av_unetI/netI     0.0141
_diffrn_reflns_av_R_equivalents  0.0206
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.264
_diffrn_reflns_theta_max         36.289
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measured_fraction_theta_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_point_group_measured_fraction_full 0.987
_reflns_number_total             6227
_reflns_number_gt                5637
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'Brukar Apex2'
_computing_cell_refinement       'Brukar Apex2'
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0407P)²+0.5022P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6227
_refine_ls_number_parameters     224
_refine_ls_number_restraints     181
_refine_ls_R_factor_all          0.0320
_refine_ls_R_factor_gt           0.0284
_refine_ls_wR_factor_ref         0.0793
_refine_ls_wR_factor_gt          0.0772
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.051
_refine_ls_shift/su_max          0.002
_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_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 0.60733(4) 0.89988(2) 0.62486(2) 0.01929(5) Uani 1 1 d . . . . .
P3 P 0.74814(3) 0.62828(2) 0.81618(2) 0.01654(5) Uani 1 1 d . . . . .
P4 P 0.86041(3) 0.89143(2) 1.01007(2) 0.01491(5) Uani 1 1 d . . . . .
F1 F 0.38668(12) 0.88782(7) 0.57778(10) 0.0475(2) Uani 1 1 d . . . . .
F2 F 0.61438(13) 0.87353(5) 0.52025(6) 0.03291(16) Uani 1 1 d . . . . .
F5 F 0.84924(12) 0.55635(5) 0.91238(7) 0.03554(17) Uani 1 1 d . . . . .
F6 F 0.79827(14) 0.58717(6) 0.73216(8) 0.03715(18) Uani 1 1 d . . . . .
F7 F 0.78995(11) 0.80601(5) 1.04809(6) 0.02923(14) Uani 1 1 d . . . . .
F8 F 0.72191(9) 0.96854(5) 1.00585(5) 0.02285(11) Uani 1 1 d . . . . .
O1 O 0.70661(11) 0.81572(5) 0.70461(6) 0.01995(12) Uani 1 1 d . . . . .
O2 O 0.67909(15) 0.99501(5) 0.66508(7) 0.02991(17) Uani 1 1 d . . . . .
O3 O 1.04447(11) 0.85083(5) 0.85096(7) 0.02360(14) Uani 1 1 d D U . . .
O5 O 0.87957(10) 0.71574(5) 0.86733(6) 0.01796(11) Uani 1 1 d . . . . .
O6 O 0.53671(12) 0.63641(7) 0.76789(7) 0.02883(16) Uani 1 1 d . . . . .
O7 O 0.78261(10) 0.87372(5) 0.88439(5) 0.01713(11) Uani 1 1 d . . . . .
O8 O 1.07015(10) 0.91120(5) 1.08874(6) 0.02073(12) Uani 1 1 d . . . . .
B1 B 0.85388(14) 0.81388(6) 0.82709(8) 0.01568(14) Uani 1 1 d . . . . .
Li2 Li 0.2821(3) 0.60845(12) 0.74682(15) 0.0200(3) Uani 1 1 d D . . . .
O4_a O 1.2027(7) 0.7157(2) 0.8032(7) 0.0263(2) Uani 0.8230(10) 1 d D U P A 1
P2_a P 1.22246(5) 0.80592(2) 0.85794(4) 0.01904(7) Uani 0.8230(10) 1 d D U P A
1
F3_a F 1.37935(17) 0.80571(9) 0.98586(10) 0.0509(3) Uani 0.8230(10) 1 d D U P A
1
F4_a F 1.3087(2) 0.88344(7) 0.82146(16) 0.0491(3) Uani 0.8230(10) 1 d D U P A 1
O4A_b O 1.203(3) 0.7094(10) 0.802(4) 0.0263(2) Uani 0.1770(10) 1 d D U P A 2
P2A_b P 1.1808(2) 0.81291(11) 0.80960(19) 0.01904(7) Uani 0.1770(10) 1 d D U P
A 2
F3A_b F 1.3835(8) 0.8522(5) 0.9039(8) 0.071(2) Uani 0.1770(10) 1 d D U P A 2
F4A_b F 1.1207(11) 0.8702(3) 0.7077(6) 0.0592(17) Uani 0.1770(10) 1 d D U P A 2


_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 O2 1.4443(8) . ?
P1 F1 1.5155(9) . ?
P1 F2 1.5183(7) . ?
P1 O1 1.5207(7) . ?
P3 O6 1.4404(8) . ?
P3 F5 1.5165(7) . ?
P3 O5 1.5214(7) . ?
P3 F6 1.5225(7) . ?
P4 O8 1.4499(7) . ?
P4 F8 1.5201(6) . ?
P4 O7 1.5216(7) . ?
P4 F7 1.5286(6) . ?
O1 B1 1.4590(12) . ?
O2 Li2 1.9285(19) 2_656 ?
O3 B1 1.4577(12) . ?
O3 P2_a 1.4986(8) . ?
O3 P2A_b 1.5563(18) . ?
O5 B1 1.4609(11) . ?
O6 Li2 1.917(2) . ?
O7 B1 1.4560(11) . ?
O8 Li2 1.9423(19) 4_676 ?
Li2 O4A_b 1.87(2) 1_455 ?
Li2 O2 1.9285(19) 2_646 ?
Li2 O8 1.9422(19) 4_475 ?
Li2 O4_a 1.945(4) 1_455 ?
O4_a P2_a 1.442(4) . ?
O4_a Li2 1.945(4) 1_655 ?
P2_a F4_a 1.5061(11) . ?
P2_a F3_a 1.5284(11) . ?
O4A_b P2A_b 1.477(13) . ?
O4A_b Li2 1.87(2) 1_655 ?
P2A_b F4A_b 1.463(5) . ?
P2A_b F3A_b 1.537(5) . ?

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 P1 F1 113.44(6) . . ?
O2 P1 F2 112.73(5) . . ?
F1 P1 F2 100.25(6) . . ?
O2 P1 O1 119.69(5) . . ?
F1 P1 O1 105.08(5) . . ?
F2 P1 O1 103.45(4) . . ?
O6 P3 F5 113.80(5) . . ?
O6 P3 O5 119.45(5) . . ?
F5 P3 O5 102.62(4) . . ?
O6 P3 F6 112.58(5) . . ?
F5 P3 F6 100.56(5) . . ?
O5 P3 F6 105.70(4) . . ?
O8 P4 F8 114.08(4) . . ?
O8 P4 O7 119.81(4) . . ?
F8 P4 O7 102.93(4) . . ?
O8 P4 F7 111.98(4) . . ?
F8 P4 F7 100.82(4) . . ?
O7 P4 F7 105.10(4) . . ?
B1 O1 P1 129.91(6) . . ?
P1 O2 Li2 155.12(9) . 2_656 ?
B1 O3 P2_a 133.48(6) . . ?
B1 O3 P2A_b 128.98(9) . . ?
B1 O5 P3 131.58(6) . . ?
P3 O6 Li2 157.42(8) . . ?
B1 O7 P4 132.28(6) . . ?
P4 O8 Li2 141.19(7) . 4_676 ?
O7 B1 O3 108.79(7) . . ?
O7 B1 O1 108.45(7) . . ?
O3 B1 O1 110.64(8) . . ?
O7 B1 O5 110.84(7) . . ?
O3 B1 O5 109.35(7) . . ?
O1 B1 O5 108.77(7) . . ?
O4A_b Li2 O6 109.4(5) 1_455 . ?
O4A_b Li2 O2 110.4(11) 1_455 2_646 ?
O6 Li2 O2 105.63(9) . 2_646 ?
O4A_b Li2 O8 106.8(11) 1_455 4_475 ?
O6 Li2 O8 114.42(10) . 4_475 ?
O2 Li2 O8 110.16(9) 2_646 4_475 ?
O6 Li2 O4_a 108.38(13) . 1_455 ?
O2 Li2 O4_a 111.5(2) 2_646 1_455 ?
O8 Li2 O4_a 106.8(2) 4_475 1_455 ?
P2_a O4_a Li2 157.2(2) . 1_655 ?
O4_a P2_a O3 119.93(16) . . ?
O4_a P2_a F4_a 113.9(3) . . ?
O3 P2_a F4_a 104.44(6) . . ?
O4_a P2_a F3_a 113.5(3) . . ?
O3 P2_a F3_a 103.70(6) . . ?
F4_a P2_a F3_a 98.74(9) . . ?
P2A_b O4A_b Li2 149(2) . 1_655 ?
F4A_b P2A_b O4A_b 117.7(16) . . ?
F4A_b P2A_b F3A_b 106.2(5) . . ?
O4A_b P2A_b F3A_b 107.7(12) . . ?
F4A_b P2A_b O3 103.1(2) . . ?
O4A_b P2A_b O3 119.7(9) . . ?
F3A_b P2A_b O3 100.5(3) . . ?

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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 P1 O1 B1 9.74(11) . . . . ?
F1 P1 O1 B1 -119.14(9) . . . . ?
F2 P1 O1 B1 136.15(9) . . . . ?
F1 P1 O2 Li2 52.6(2) . . . 2_656 ?
F2 P1 O2 Li2 165.65(18) . . . 2_656 ?
O1 P1 O2 Li2 -72.4(2) . . . 2_656 ?
O6 P3 O5 B1 -43.66(10) . . . . ?
F5 P3 O5 B1 -170.63(8) . . . . ?
F6 P3 O5 B1 84.42(9) . . . . ?
F5 P3 O6 Li2 -2.5(2) . . . . ?
O5 P3 O6 Li2 -124.1(2) . . . . ?
F6 P3 O6 Li2 111.1(2) . . . . ?
O8 P4 O7 B1 47.25(10) . . . . ?
F8 P4 O7 B1 175.13(8) . . . . ?
F7 P4 O7 B1 -79.72(9) . . . . ?
F8 P4 O8 Li2 90.32(12) . . . 4_676 ?
O7 P4 O8 Li2 -147.09(11) . . . 4_676 ?
F7 P4 O8 Li2 -23.39(13) . . . 4_676 ?
P4 O7 B1 O3 -66.47(10) . . . . ?
P4 O7 B1 O1 173.13(6) . . . . ?
P4 O7 B1 O5 53.79(11) . . . . ?
P2_a O3 B1 O7 152.04(8) . . . . ?
P2A_b O3 B1 O7 -179.75(12) . . . . ?
P2_a O3 B1 O1 -88.92(11) . . . . ?
P2A_b O3 B1 O1 -60.72(15) . . . . ?
P2_a O3 B1 O5 30.86(13) . . . . ?
P2A_b O3 B1 O5 59.07(15) . . . . ?
P1 O1 B1 O7 50.75(11) . . . . ?
P1 O1 B1 O3 -68.49(10) . . . . ?
P1 O1 B1 O5 171.38(7) . . . . ?
P3 O5 B1 O7 99.62(9) . . . . ?
P3 O5 B1 O3 -140.45(7) . . . . ?
P3 O5 B1 O1 -19.53(11) . . . . ?
Li2 O4_a P2_a O3 170.9(13) 1_655 . . . ?
Li2 O4_a P2_a F4_a 46.2(15) 1_655 . . . ?
Li2 O4_a P2_a F3_a -65.8(15) 1_655 . . . ?
B1 O3 P2_a O4_a 20.7(4) . . . . ?
P2A_b O3 P2_a O4_a -66.9(4) . . . . ?
B1 O3 P2_a F4_a 149.83(11) . . . . ?
P2A_b O3 P2_a F4_a 62.18(17) . . . . ?
B1 O3 P2_a F3_a -107.21(11) . . . . ?
P2A_b O3 P2_a F3_a 165.14(18) . . . . ?
Li2 O4A_b P2A_b F4A_b 38(4) 1_655 . . . ?
Li2 O4A_b P2A_b F3A_b -82(5) 1_655 . . . ?
Li2 O4A_b P2A_b O3 164(3) 1_655 . . . ?
B1 O3 P2A_b F4A_b 94.9(3) . . . . ?
P2_a O3 P2A_b F4A_b -154.0(4) . . . . ?
B1 O3 P2A_b O4A_b -38.1(18) . . . . ?
P2_a O3 P2A_b O4A_b 73.0(18) . . . . ?
B1 O3 P2A_b F3A_b -155.6(4) . . . . ?
P2_a O3 P2A_b F3A_b -44.5(4) . . . . ?

_refine_diff_density_max         0.785
_refine_diff_density_min         -0.603
_refine_diff_density_rms         0.065

_shelxl_version_number           2014-1

