# Electronic Supplementary Material (ESI) for Dalton Transactions.
# 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. 
# 
#######################################################################

data_libarf4h2o
_database_code_depnum_ccdc_archive 'CCDC 1886445'
_audit_update_record             
;
2018-12-20 deposited with the CCDC.
2019-01-31 downloaded from the CCDC.
;
_audit_creation_date             2018-12-17
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.5(C64 H28 B2 F48 Li2 O2)'
_chemical_formula_sum            'C32 H14 B F24 Li O'
_chemical_formula_weight         888.18
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C32 H12 B1 F24 Li1'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li 0.0008 0.0003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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      tetragonal
_space_group_IT_number           85
_space_group_name_H-M_alt        'P 4/n'
_space_group_name_Hall           '-P 4a'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-y+1/2, x, z'
'y, -x+1/2, z'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'y-1/2, -x, -z'
'-y, x-1/2, -z'

_cell_length_a                   13.45985(14)
_cell_length_b                   13.45985(14)
_cell_length_c                   9.66072(16)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1750.21(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    11247
_cell_measurement_temperature    150.0(3)
_cell_measurement_theta_max      75.8330
_cell_measurement_theta_min      4.5410
_shelx_estimated_absorpt_T_max   0.819
_shelx_estimated_absorpt_T_min   0.769
_exptl_absorpt_coefficient_mu    1.736
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92535
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.685
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             876
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0207
_diffrn_reflns_av_unetI/netI     0.0079
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            22082
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.216
_diffrn_reflns_theta_min         4.577
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.0(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4102
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     59.00 125.00   1.00    1.00    --   42.66 178.00-120.00   66
  2  ω     63.00  98.00   1.00    1.00    --   42.66 178.00-180.00   35
  3  ω     60.00  97.00   1.00    1.00    --   42.66 178.00 -30.00   37
  4  ω     42.00  79.00   1.00    3.00    --  111.00 -45.00  30.00   37
  5  ω     47.00  75.00   1.00    3.00    --  111.00 -30.00-120.00   28
  6  ω     60.00 139.00   1.00    3.00    --  111.00 -61.00 -60.00   79
  7  ω     57.00  89.00   1.00    3.00    --  111.00 -30.00  30.00   32
  8  ω     52.00 103.00   1.00    3.00    --  111.00 -99.00 -85.00   51
  9  ω     42.00  67.00   1.00    3.00    --  111.00 -30.00 -30.00   25
 10  ω     44.00  98.00   1.00    3.00    --  111.00 -45.00 150.00   54
 11  ω    -99.00 -18.00   1.00    1.00    --  -42.66 -57.00 -30.00   81
 12  ω    -55.00 -28.00   1.00    1.00    --  -42.66 -57.00-120.00   27
 13  ω     42.00  68.00   1.00    3.00    --  111.00 -45.00 -30.00   26
 14  ω    143.00 169.00   1.00    3.00    --  111.00  45.00 -30.00   26
 15  ω     81.00 128.00   1.00    3.00    --  111.00  77.00 -90.00   47
 16  ω    121.00 174.00   1.00    3.00    --  111.00 125.00-180.00   53
 17  ω    135.00 172.00   1.00    3.00    --  111.00  45.00 -90.00   37
 18  ω     88.00 130.00   1.00    3.00    --  111.00  45.00 -90.00   42
 19  ω     84.00 110.00   1.00    3.00    --  111.00  61.00-120.00   26
 20  ω    141.00 167.00   1.00    3.00    --  111.00  61.00-120.00   26
 21  ω     96.00 131.00   1.00    3.00    --  111.00  45.00 -30.00   35
 22  ω    136.00 161.00   1.00    3.00    --  111.00  77.00 -90.00   25
 23  ω     84.00 111.00   1.00    3.00    --  111.00  77.00-120.00   27
 24  ω     62.00  90.00   1.00    3.00    --  111.00 -30.00 -90.00   28
 25  ω    -74.00 -48.00   1.00    1.00    --  -42.66  77.00 120.00   26
 26  ω      4.00  31.00   1.00    1.00    --  -42.66  77.00 120.00   27
 27  ω     91.00 116.00   1.00    1.00    --   42.66 178.00  30.00   25
 28  ω     32.00  96.00   1.00    3.00    --  111.00 -95.00-150.00   64
 29  ω     39.00  85.00   1.00    3.00    --  111.00 -30.00-180.00   46
 30  ω    145.00 177.00   1.00    3.00    --  111.00  45.00  30.00   32
 31  ω     97.00 123.00   1.00    3.00    --  111.00  61.00 -60.00   26
 32  ω    126.00 152.00   1.00    3.00    --  111.00  61.00-180.00   26
 33  ω     85.00 111.00   1.00    3.00    --  111.00  61.00-180.00   26
 34  ω    134.00 175.00   1.00    3.00    --  111.00  61.00 -60.00   41
 35  ω    116.00 155.00   1.00    3.00    --  111.00  30.00-150.00   39
 36  ω     -2.00  25.00   1.00    1.00    --  -42.66  38.00  30.00   27
 37  ω   -115.00 -16.00   1.00    1.00    --  -42.66 -19.00-150.00   99
 38  ω     56.00  83.00   1.00    1.00    --   42.66 -99.00 -30.00   27
 39  ω     90.00 121.00   1.00    3.00    --  111.00-131.00 119.02   31
 40  ω    125.00 152.00   1.00    3.00    --  111.00 125.00 150.00   27
 41  ω     43.00  89.00   1.00    3.00    --  111.00 -45.00-120.00   46
 42  ω     42.00  68.00   1.00    3.00    --  111.00-131.00 119.02   26
 43  ω     36.00  62.00   1.00    3.00    --  111.00 -30.00 -60.00   26
 44  ω     56.00  82.00   1.00    3.00    --  111.00-125.00 -90.00   26
 45  ω     43.00  81.00   1.00    3.00    --  111.00 -45.00  90.00   38
 46  ω     78.00 104.00   1.00    3.00    --  111.00-125.00-150.00   26
 47  ω     65.00  92.00   1.00    3.00    --  111.00-125.00   0.00   27
 48  ω     36.00  61.00   1.00    3.00    --  111.00 -30.00   0.00   25
 49  ω    106.00 133.00   1.00    3.00    --  111.00 125.00-150.00   27
 50  ω     75.00 118.00   1.00    3.00    --  111.00-125.00-180.00   43
 51  ω     81.00 142.00   1.00    3.00    --  111.00 -77.00   0.00   61
 52  ω     97.00 130.00   1.00    3.00    --  111.00-141.00  40.39   33
 53  ω     92.00 118.00   1.00    3.00    --  111.00-125.00-120.00   26
 54  ω     91.00 117.00   1.00    3.00    --  111.00-125.00 -60.00   26
 55  ω     46.00  91.00   1.00    3.00    --  111.00-141.00  40.39   45
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0914619000
_diffrn_orient_matrix_UB_12      0.0677943000
_diffrn_orient_matrix_UB_13      -0.0167063000
_diffrn_orient_matrix_UB_21      -0.0583373000
_diffrn_orient_matrix_UB_22      0.0658260000
_diffrn_orient_matrix_UB_23      -0.1020234000
_diffrn_orient_matrix_UB_31      -0.0365667000
_diffrn_orient_matrix_UB_32      0.0645689000
_diffrn_orient_matrix_UB_33      0.1213873000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1744
_reflns_number_total             1826
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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         0.430
_refine_diff_density_min         -0.333
_refine_diff_density_rms         0.050
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         1826
_refine_ls_number_restraints     231
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_gt           0.0523
_refine_ls_restrained_S_all      1.488
_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)+(0.0640P)²+1.3632P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1380
_refine_ls_wR_factor_ref         0.1390
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 F5-F6 \\sim F5-F4 \\sim F5A-F6A \\sim F5A-F4A
 with sigma of 0.04
 C8-F5 \\sim C8-F5A \\sim C8-F6 \\sim C8-F6A \\sim C8-F4A \\sim C8-F4
 with sigma of 0.02
 F2-F3 \\sim F2-F1 \\sim F2A-F3A \\sim F2A-F1A \\sim F3A-F1A \\sim F3-F1
 with sigma of 0.04
 C7-F2 \\sim C7-F2A \\sim C7-F3A \\sim C7-F3 \\sim C7-F1 \\sim C7-F1A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
F5 \\sim F4 \\sim C8 \\sim F6 \\sim F5A \\sim F4A \\sim F6A: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.01
F2 \\sim F3 \\sim F1 \\sim C7 \\sim F2A \\sim F3A \\sim F1A: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.01
4. Rigid body (RIGU) restrains
 F5, F4, C8, F6, F5A, F4A, F6A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F2, F3, F1, F2A, F3A, F1A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(F5A)=Sof(F4A)=Sof(F6A)=1-FVAR(1)
 Sof(F5)=Sof(F4)=Sof(F6)=FVAR(1)
 Sof(F2A)=Sof(F3A)=Sof(F1A)=1-FVAR(2)
 Sof(F2)=Sof(F3)=Sof(F1)=FVAR(2)
 Fixed Sof: H1A(0.25) H1B(0.25)
6.a Rotating group:
 O1(H1A,H1B)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C6(H6), C4(H4)
;
_atom_sites_solution_hydrogens   mixed
_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
F2 F 0.6184(7) 0.5035(5) 0.1819(9) 0.0499(14) Uani 0.640(16) 1 d D U . A 1
O1 O 0.750000 0.750000 0.4527(3) 0.0477(7) Uani 1 4 d S T P A .
H1A H 0.819269 0.764764 0.520671 0.071 Uiso 0.25 1 d GR . . . .
H1B H 0.735324 0.680709 0.520681 0.071 Uiso 0.25 1 d GR . . . .
F3 F 0.6161(5) 0.6140(7) 0.0239(6) 0.0586(14) Uani 0.640(16) 1 d D U . A 1
F1 F 0.6308(3) 0.6573(3) 0.2392(7) 0.0452(10) Uani 0.640(16) 1 d D U . A 1
F5 F 0.3387(8) 0.4562(7) 0.4867(10) 0.0685(17) Uani 0.487(5) 1 d D U . B 1
C2 C 0.42027(12) 0.66415(12) 0.08185(18) 0.0261(4) Uani 1 1 d . . . . .
H2 H 0.452634 0.696724 0.009922 0.031 Uiso 1 1 calc R . . . .
C1 C 0.31855(12) 0.67944(12) 0.10031(17) 0.0249(4) Uani 1 1 d . . . . .
C3 C 0.47484(13) 0.60139(13) 0.16820(19) 0.0292(4) Uani 1 1 d . . . . .
C6 C 0.27546(14) 0.62902(13) 0.21163(19) 0.0301(4) Uani 1 1 d . . . . .
H6 H 0.208088 0.637966 0.228978 0.036 Uiso 1 1 calc R . . . .
C5 C 0.32936(15) 0.56603(14) 0.2974(2) 0.0357(4) Uani 1 1 d . . . . .
C4 C 0.43023(15) 0.55134(14) 0.2767(2) 0.0348(4) Uani 1 1 d . . . . .
H4 H 0.466645 0.509283 0.333800 0.042 Uiso 1 1 calc R . . . .
C7 C 0.58410(14) 0.59187(14) 0.1477(2) 0.0378(5) Uani 1 1 d D U . . .
B1 B 0.250000 0.750000 0.000000 0.0236(7) Uani 1 4 d S T P . .
F4 F 0.1998(4) 0.4763(6) 0.3940(6) 0.0929(17) Uani 0.487(5) 1 d D U . B 1
C8 C 0.2782(2) 0.5143(2) 0.4132(3) 0.0643(7) Uani 1 1 d D U . . .
F6 F 0.2573(4) 0.5878(3) 0.5198(5) 0.0860(15) Uani 0.487(5) 1 d D U . B 1
Li1 Li 0.750000 0.750000 0.2620(8) 0.0391(14) Uani 1 4 d S T P . .
F5A F 0.2360(4) 0.4208(4) 0.3496(5) 0.0802(13) Uani 0.513(5) 1 d D U . B 2
F4A F 0.1926(4) 0.5489(4) 0.4488(6) 0.0923(17) Uani 0.513(5) 1 d D U . B 2
F6A F 0.3317(8) 0.4791(7) 0.5084(10) 0.080(2) Uani 0.513(5) 1 d D U . B 2
F2A F 0.6283(13) 0.5154(9) 0.2094(14) 0.046(2) Uani 0.360(16) 1 d D U . A 2
F3A F 0.6078(10) 0.5823(7) 0.0107(10) 0.0474(16) Uani 0.360(16) 1 d D U . A 2
F1A F 0.6372(5) 0.6748(6) 0.1785(15) 0.0542(18) Uani 0.360(16) 1 d D U . 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
F2 C7 1.317(6) . ?
O1 H1A 1.1578 . ?
O1 H1B 1.1579 . ?
O1 Li1 1.842(8) . ?
F3 C7 1.306(6) . ?
F1 C7 1.397(4) . ?
F1 Li1 2.045(4) . ?
F5 C8 1.334(7) . ?
C2 H2 0.9300 . ?
C2 C1 1.396(2) . ?
C2 C3 1.396(2) . ?
C1 C6 1.398(2) . ?
C1 B1 1.6409(17) . ?
C3 C4 1.383(3) . ?
C3 C7 1.489(3) . ?
C6 H6 0.9300 . ?
C6 C5 1.390(3) . ?
C5 C4 1.387(3) . ?
C5 C8 1.487(3) . ?
C4 H4 0.9300 . ?
C7 F2A 1.330(10) . ?
C7 F3A 1.368(9) . ?
C7 F1A 1.358(6) . ?
F4 C8 1.186(5) . ?
C8 F6 1.456(5) . ?
C8 F5A 1.510(5) . ?
C8 F4A 1.289(5) . ?
C8 F6A 1.261(8) . ?
Li1 F1A 1.995(7) 2_665 ?
Li1 F1A 1.995(7) . ?
Li1 F1A 1.995(7) 3_655 ?
Li1 F1A 1.995(7) 4_565 ?

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
H1A O1 H1B 87.3 . . ?
Li1 O1 H1A 124.6 . . ?
Li1 O1 H1B 124.6 . . ?
C7 F1 Li1 143.7(5) . . ?
C1 C2 H2 119.0 . . ?
C1 C2 C3 121.93(16) . . ?
C3 C2 H2 119.0 . . ?
C2 C1 C6 115.70(15) . . ?
C2 C1 B1 124.15(13) . . ?
C6 C1 B1 120.14(13) . . ?
C2 C3 C7 119.49(17) . . ?
C4 C3 C2 121.28(17) . . ?
C4 C3 C7 119.16(17) . . ?
C1 C6 H6 118.7 . . ?
C5 C6 C1 122.58(17) . . ?
C5 C6 H6 118.7 . . ?
C6 C5 C8 119.50(19) . . ?
C4 C5 C6 120.78(18) . . ?
C4 C5 C8 119.71(18) . . ?
C3 C4 C5 117.72(17) . . ?
C3 C4 H4 121.1 . . ?
C5 C4 H4 121.1 . . ?
F2 C7 F1 104.6(4) . . ?
F2 C7 C3 113.0(5) . . ?
F3 C7 F2 108.7(5) . . ?
F3 C7 F1 106.7(3) . . ?
F3 C7 C3 115.3(3) . . ?
F1 C7 C3 107.8(2) . . ?
F2A C7 C3 116.7(8) . . ?
F2A C7 F3A 104.8(8) . . ?
F2A C7 F1A 107.6(7) . . ?
F3A C7 C3 111.5(6) . . ?
F1A C7 C3 114.8(3) . . ?
F1A C7 F3A 99.6(6) . . ?
C1 B1 C1 110.41(6) 8_665 2_565 ?
C1 B1 C1 110.41(6) 8_665 . ?
C1 B1 C1 110.41(6) 7_565 2_565 ?
C1 B1 C1 107.60(11) 2_565 . ?
C1 B1 C1 110.41(6) 7_565 . ?
C1 B1 C1 107.60(11) 7_565 8_665 ?
F5 C8 C5 113.1(6) . . ?
F5 C8 F6 98.0(5) . . ?
C5 C8 F5A 105.0(3) . . ?
F4 C8 F5 111.9(6) . . ?
F4 C8 C5 119.7(3) . . ?
F4 C8 F6 103.4(5) . . ?
F6 C8 C5 107.6(2) . . ?
F4A C8 C5 116.5(2) . . ?
F4A C8 F5A 94.2(4) . . ?
F6A C8 C5 117.4(6) . . ?
F6A C8 F5A 101.5(5) . . ?
F6A C8 F4A 116.8(6) . . ?
O1 Li1 F1 96.2(3) . . ?
O1 Li1 F1 96.2(3) . 2_665 ?
O1 Li1 F1 96.2(3) . 3_655 ?
O1 Li1 F1 96.2(3) . 4_565 ?
O1 Li1 F1A 113.8(5) . 2_665 ?
O1 Li1 F1A 113.8(5) . 3_655 ?
O1 Li1 F1A 113.8(5) . . ?
O1 Li1 F1A 113.8(5) . 4_565 ?
F1 Li1 F1 89.34(6) 3_655 . ?
F1 Li1 F1 89.34(6) 4_565 . ?
F1 Li1 F1 167.7(6) 2_665 . ?
F1 Li1 F1 167.7(6) 3_655 4_565 ?
F1 Li1 F1 89.34(6) 2_665 4_565 ?
F1 Li1 F1 89.34(6) 2_665 3_655 ?
F1A Li1 F1 91.3(3) 3_655 2_665 ?
F1A Li1 F1 149.7(7) 4_565 3_655 ?
F1A Li1 F1 18.1(3) 3_655 3_655 ?
F1A Li1 F1 18.1(3) 2_665 2_665 ?
F1A Li1 F1 83.7(3) 2_665 3_655 ?
F1A Li1 F1 91.3(3) . 3_655 ?
F1A Li1 F1 83.7(3) 4_565 2_665 ?
F1A Li1 F1 149.7(7) . 2_665 ?
F1A Li1 F1A 80.6(4) 3_655 . ?
F1A Li1 F1A 132.3(10) 3_655 4_565 ?
F1A Li1 F1A 80.6(4) 2_665 4_565 ?
F1A Li1 F1A 132.3(10) 2_665 . ?
F1A Li1 F1A 80.6(4) 2_665 3_655 ?
F1A Li1 F1A 80.6(4) 4_565 . ?
C7 F1A Li1 154.9(8) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.111
_oxdiff_exptl_absorpt_empirical_full_min 0.939
_chemical_properties_physical    Hygroscopic
####################################################################### 
# 
# 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_kbarf4
_database_code_depnum_ccdc_archive 'CCDC 1886447'
_audit_update_record             
;
2018-12-20 deposited with the CCDC.
2019-01-31 downloaded from the CCDC.
;
_audit_creation_date             2018-12-15
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.5(C64 H24 B2 F48 K2)'
_chemical_formula_sum            'C32 H12 B F24 K'
_chemical_formula_weight         902.33
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C54 H66 B1 Co1 F24 N3 P2'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.3868 1.0657 '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      tetragonal
_space_group_IT_number           85
_space_group_name_H-M_alt        'P 4/n'
_space_group_name_Hall           '-P 4a'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-y+1/2, x, z'
'y, -x+1/2, z'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'y-1/2, -x, -z'
'-y, x-1/2, -z'

_cell_length_a                   13.4834(3)
_cell_length_b                   13.4834(3)
_cell_length_c                   9.4747(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1722.52(12)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1829
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      74.7320
_cell_measurement_theta_min      4.6120
_shelx_estimated_absorpt_T_max   0.677
_shelx_estimated_absorpt_T_min   0.603
_exptl_absorpt_coefficient_mu    2.819
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88231
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.740
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0214
_diffrn_reflns_av_unetI/netI     0.0214
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4443
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.811
_diffrn_reflns_theta_min         4.638
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5035
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -47.00  30.00   1.00    1.00    --  -41.77  37.00 150.00   77
  2  ω     50.00  95.00   1.00    1.00    --   41.77-125.00 150.00   45
  3  ω     50.00 121.00   1.00    1.50    --  111.00-125.00 120.00   71
  4  ω     59.00  89.00   1.00    1.50    --  111.00 -30.00  90.00   30
  5  ω     41.00  68.00   1.00    1.50    --  111.00 -45.00  90.00   27
  6  ω     40.00  98.00   1.00    1.50    --  111.00 -45.00 -30.00   58
  7  ω     65.00  94.00   1.00    1.50    --  111.00-125.00 -60.00   29
  8  ω     38.00  85.00   1.00    1.50    --  111.00 -30.00 -90.00   47
  9  ω     44.00  88.00   1.00    1.50    --  111.00 -30.00-180.00   44
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0762435000
_diffrn_orient_matrix_UB_12      -0.0846036000
_diffrn_orient_matrix_UB_13      -0.0127627000
_diffrn_orient_matrix_UB_21      0.0023583000
_diffrn_orient_matrix_UB_22      0.0141804000
_diffrn_orient_matrix_UB_23      -0.1613759000
_diffrn_orient_matrix_UB_31      0.0849700000
_diffrn_orient_matrix_UB_32      0.0755153000
_diffrn_orient_matrix_UB_33      0.0158551000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1554
_reflns_number_total             1783
_reflns_odcompleteness_completeness 99.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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       'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)'
_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         0.670
_refine_diff_density_min         -0.391
_refine_diff_density_rms         0.061
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         1783
_refine_ls_number_restraints     224
_refine_ls_R_factor_all          0.0580
_refine_ls_R_factor_gt           0.0514
_refine_ls_restrained_S_all      1.248
_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)+(0.0660P)²+2.2072P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1315
_refine_ls_wR_factor_ref         0.1378
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 F2-F3 \\sim F2-F1 \\sim F2A-F3A \\sim F2A-F1A \\sim F3A-F1A \\sim F3-F1
 with sigma of 0.04
 F2-C7 \\sim F2A-C7 \\sim F1-C7 \\sim F1A-C7 \\sim F3-C7 \\sim F3A-C7
 with sigma of 0.02
 F5-F6 \\sim F4-F6 \\sim F4-F5 \\sim F6A-F5A \\sim F6A-F4A \\sim F5A-F4A
 with sigma of 0.04
 C8A-F6A \\sim C8A-F5A \\sim C8A-F4A \\sim C8-F6 \\sim C8-F4 \\sim C8-F5
 with sigma of 0.02
3. Restrained planarity
 C8A, C5, C4, C3, C2, C1, C6
 with sigma of 0.1
 C8, C5, C4, C3, C2, C1, C6
 with sigma of 0.1
4. Rigid bond restraints
 C8, F6, F4, F5, C8A, F6A, F5A, F4A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
F2 \\sim F1 \\sim F3 \\sim C7 \\sim F3A \\sim F1A \\sim F2A: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C8 \\sim C8A: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
F5A \\sim F5 \\sim F6A \\sim F6 \\sim F4A \\sim F4: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.01
Uanis(C8A) = Uanis(C8)
6. Rigid body (RIGU) restrains
 F2, F1, F3, C7, F3A, F1A, F2A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 Sof(F3A)=Sof(F1A)=Sof(F2A)=1-FVAR(1)
 Sof(F2)=Sof(F1)=Sof(F3)=FVAR(1)
 Sof(C8A)=Sof(F6A)=Sof(F5A)=Sof(F4A)=1-FVAR(2)
 Sof(C8)=Sof(F6)=Sof(F4)=Sof(F5)=FVAR(2)
8.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C6(H6), C4(H4)
;
_atom_sites_solution_hydrogens   geom
_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
K1 K 0.250000 0.250000 0.57117(10) 0.0259(3) Uani 1 4 d S T P . .
F2 F 0.3825(19) 0.5005(10) 0.817(3) 0.044(3) Uani 0.43(6) 1 d D U . A 1
F1 F 0.377(2) 0.3529(19) 0.739(3) 0.056(5) Uani 0.43(6) 1 d D U . A 1
F3 F 0.3858(13) 0.378(3) 0.959(2) 0.066(5) Uani 0.43(6) 1 d D U . A 1
C1 C 0.68376(15) 0.32220(14) 0.8973(2) 0.0173(4) Uani 1 1 d . . . . .
C2 C 0.58197(16) 0.33751(15) 0.9106(2) 0.0188(4) Uani 1 1 d . . . . .
H2 H 0.546769 0.303101 0.982346 0.023 Uiso 1 1 calc R . . . .
C6 C 0.73053(16) 0.37402(16) 0.7871(2) 0.0223(5) Uani 1 1 d . . . . .
H6 H 0.799528 0.364543 0.771919 0.027 Uiso 1 1 calc R . . . .
C3 C 0.53024(16) 0.40167(15) 0.8220(2) 0.0216(5) Uani 1 1 d . . . . .
C4 C 0.57791(17) 0.45338(17) 0.7161(2) 0.0268(5) Uani 1 1 d . . . . .
H4 H 0.542587 0.497602 0.656388 0.032 Uiso 1 1 calc R . . . .
C5 C 0.67892(18) 0.43865(17) 0.6998(2) 0.0280(5) Uani 1 1 d . . . . .
C7 C 0.42012(17) 0.41173(17) 0.8372(3) 0.0294(5) Uani 1 1 d D U . . .
B1 B 0.750000 0.250000 1.000000 0.0159(8) Uani 1 4 d S T P . .
C8 C 0.7325(8) 0.4832(8) 0.5769(13) 0.0486(12) Uani 0.538(5) 1 d D U . B 1
F3A F 0.3886(10) 0.4055(10) 0.9703(8) 0.0454(19) Uani 0.57(6) 1 d D U . A 2
F1A F 0.3688(16) 0.3435(12) 0.7644(17) 0.046(2) Uani 0.57(6) 1 d D U . A 2
F2A F 0.3891(14) 0.4993(8) 0.790(2) 0.046(3) Uani 0.57(6) 1 d D U . A 2
F6 F 0.6985(6) 0.5704(4) 0.5430(8) 0.097(2) Uani 0.538(5) 1 d D U . B 1
F4 F 0.7257(4) 0.4310(4) 0.4554(4) 0.0809(15) Uani 0.538(5) 1 d D U . B 1
F5 F 0.8280(4) 0.4908(6) 0.5909(8) 0.073(2) Uani 0.538(5) 1 d D U . B 1
C8A C 0.7327(10) 0.5006(9) 0.5932(15) 0.0486(12) Uani 0.462(5) 1 d D U . B 2
F6A F 0.7652(5) 0.5896(4) 0.6507(7) 0.0899(19) Uani 0.462(5) 1 d D U . B 2
F5A F 0.8154(6) 0.4614(6) 0.5542(10) 0.081(2) Uani 0.462(5) 1 d D U . B 2
F4A F 0.6767(6) 0.5328(7) 0.4918(7) 0.080(2) Uani 0.462(5) 1 d D U . B 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
K1 F1 2.715(12) . ?
K1 F1 2.715(12) 4 ?
K1 F1 2.715(12) 3 ?
K1 F1 2.715(12) 2 ?
K1 F1A 2.739(10) . ?
K1 F1A 2.739(10) 2 ?
K1 F1A 2.739(10) 4 ?
K1 F1A 2.739(10) 3 ?
K1 F6 2.742(5) 7_566 ?
K1 F6 2.742(5) 6_556 ?
K1 F6 2.742(5) 5_666 ?
K1 F6 2.742(5) 8_656 ?
F2 C7 1.315(11) . ?
F1 C7 1.356(11) . ?
F3 C7 1.323(10) . ?
C1 C2 1.394(3) . ?
C1 C6 1.406(3) . ?
C1 B1 1.641(2) . ?
C2 H2 0.9500 . ?
C2 C3 1.393(3) . ?
C6 H6 0.9500 . ?
C6 C5 1.389(3) . ?
C3 C4 1.381(3) . ?
C3 C7 1.498(3) . ?
C4 H4 0.9500 . ?
C4 C5 1.385(3) . ?
C5 C8 1.496(15) . ?
C5 C8A 1.498(18) . ?
C7 F3A 1.334(8) . ?
C7 F1A 1.342(9) . ?
C7 F2A 1.331(8) . ?
C8 F6 1.302(10) . ?
C8 F4 1.353(10) . ?
C8 F5 1.298(10) . ?
C8A F6A 1.389(11) . ?
C8A F5A 1.288(12) . ?
C8A F4A 1.297(12) . ?

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 K1 F1 69.9(8) . 3 ?
F1 K1 F1 108.3(16) . 2 ?
F1 K1 F1 69.9(8) 3 2 ?
F1 K1 F1 108.3(16) 3 4 ?
F1 K1 F1 69.9(8) . 4 ?
F1 K1 F1 69.9(8) 4 2 ?
F1 K1 F1A 66.4(9) . 3 ?
F1 K1 F1A 6.1(10) 2 2 ?
F1 K1 F1A 66.4(9) 3 2 ?
F1 K1 F1A 6.1(10) 3 3 ?
F1 K1 F1A 67.5(10) 4 2 ?
F1 K1 F1A 102.2(8) 4 3 ?
F1 K1 F1A 6.1(10) 4 4 ?
F1 K1 F1A 66.4(9) 2 4 ?
F1 K1 F1A 67.5(10) . 4 ?
F1 K1 F1A 102.2(8) 3 4 ?
F1 K1 F1A 102.2(8) . 2 ?
F1 K1 F1A 67.5(10) 2 3 ?
F1 K1 F6 147.3(6) . 6_556 ?
F1 K1 F6 147.3(6) 2 5_666 ?
F1 K1 F6 131.1(6) 2 8_656 ?
F1 K1 F6 67.7(8) 3 7_566 ?
F1 K1 F6 78.7(7) 4 6_556 ?
F1 K1 F6 78.7(7) 2 7_566 ?
F1 K1 F6 131.1(6) . 7_566 ?
F1 K1 F6 78.7(7) 3 5_666 ?
F1 K1 F6 67.7(8) 4 8_656 ?
F1 K1 F6 147.3(6) 4 7_566 ?
F1 K1 F6 67.7(8) . 5_666 ?
F1 K1 F6 147.3(6) 3 8_656 ?
F1 K1 F6 131.1(6) 4 5_666 ?
F1 K1 F6 67.7(8) 2 6_556 ?
F1 K1 F6 78.7(7) . 8_656 ?
F1 K1 F6 131.1(6) 3 6_556 ?
F1A K1 F1A 63.5(5) 4 2 ?
F1A K1 F1A 63.5(5) 3 2 ?
F1A K1 F1A 96.2(9) . 2 ?
F1A K1 F1A 63.5(5) . 3 ?
F1A K1 F6 131.6(5) . 7_566 ?
F1A K1 F6 73.1(4) 3 7_566 ?
F1A K1 F6 82.2(5) 4 6_556 ?
F1A K1 F6 144.9(4) 4 7_566 ?
F1A K1 F6 82.2(5) 2 7_566 ?
F1A K1 F6 144.9(4) . 6_556 ?
F1A K1 F6 73.1(4) 2 6_556 ?
F1A K1 F6 131.6(5) 3 6_556 ?
F6 K1 F6 81.05(14) 6_556 7_566 ?
F6 K1 F6 81.05(14) 7_566 5_666 ?
F6 K1 F6 133.5(4) 7_566 8_656 ?
F6 K1 F6 81.05(14) 5_666 8_656 ?
F6 K1 F6 81.05(14) 6_556 8_656 ?
F6 K1 F6 133.5(4) 6_556 5_666 ?
C7 F1 K1 167(2) . . ?
C2 C1 C6 115.81(19) . . ?
C2 C1 B1 124.77(16) . . ?
C6 C1 B1 119.42(16) . . ?
C1 C2 H2 119.0 . . ?
C3 C2 C1 122.0(2) . . ?
C3 C2 H2 119.0 . . ?
C1 C6 H6 119.0 . . ?
C5 C6 C1 122.0(2) . . ?
C5 C6 H6 119.0 . . ?
C2 C3 C7 119.6(2) . . ?
C4 C3 C2 121.2(2) . . ?
C4 C3 C7 119.1(2) . . ?
C3 C4 H4 121.1 . . ?
C3 C4 C5 117.8(2) . . ?
C5 C4 H4 121.1 . . ?
C6 C5 C8 118.3(4) . . ?
C6 C5 C8A 120.6(5) . . ?
C4 C5 C6 121.1(2) . . ?
C4 C5 C8 120.3(4) . . ?
C4 C5 C8A 118.1(5) . . ?
F2 C7 F1 105.4(13) . . ?
F2 C7 F3 107.8(12) . . ?
F2 C7 C3 116.8(12) . . ?
F1 C7 C3 108.0(13) . . ?
F3 C7 F1 104.2(12) . . ?
F3 C7 C3 113.5(8) . . ?
F3A C7 C3 113.7(6) . . ?
F3A C7 F1A 106.2(9) . . ?
F1A C7 C3 113.6(10) . . ?
F2A C7 C3 111.0(9) . . ?
F2A C7 F3A 106.0(9) . . ?
F2A C7 F1A 105.8(10) . . ?
C1 B1 C1 110.59(7) 7_667 . ?
C1 B1 C1 110.59(7) 2_655 8_657 ?
C1 B1 C1 107.26(14) 2_655 . ?
C1 B1 C1 107.26(14) 7_667 8_657 ?
C1 B1 C1 110.59(7) 7_667 2_655 ?
C1 B1 C1 110.59(7) 8_657 . ?
F6 C8 C5 112.7(8) . . ?
F6 C8 F4 103.6(9) . . ?
F4 C8 C5 114.9(8) . . ?
F5 C8 C5 115.5(8) . . ?
F5 C8 F6 107.7(11) . . ?
F5 C8 F4 101.2(8) . . ?
C7 F1A K1 163.8(13) . . ?
C8 F6 K1 143.7(7) . 5_666 ?
F6A C8A C5 111.7(9) . . ?
F5A C8A C5 112.6(10) . . ?
F5A C8A F6A 101.2(10) . . ?
F5A C8A F4A 115.4(13) . . ?
F4A C8A C5 113.9(10) . . ?
F4A C8A F6A 100.7(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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
K1 F1 C7 F2 -57(9) . . . . ?
K1 F1 C7 F3 56(9) . . . . ?
K1 F1 C7 C3 177(9) . . . . ?
C1 C2 C3 C4 0.0(3) . . . . ?
C1 C2 C3 C7 177.3(2) . . . . ?
C1 C6 C5 C4 -1.3(4) . . . . ?
C1 C6 C5 C8 -174.3(4) . . . . ?
C1 C6 C5 C8A 173.6(5) . . . . ?
C2 C1 C6 C5 1.9(3) . . . . ?
C2 C1 B1 C1 9.73(19) . . . 8_657 ?
C2 C1 B1 C1 130.4(2) . . . 2_655 ?
C2 C1 B1 C1 -108.9(2) . . . 7_667 ?
C2 C3 C4 C5 0.6(3) . . . . ?
C2 C3 C7 F2 143.6(15) . . . . ?
C2 C3 C7 F1 -97.9(16) . . . . ?
C2 C3 C7 F3 17(2) . . . . ?
C2 C3 C7 F3A 35.5(7) . . . . ?
C2 C3 C7 F1A -86.0(9) . . . . ?
C2 C3 C7 F2A 154.8(10) . . . . ?
C6 C1 C2 C3 -1.2(3) . . . . ?
C6 C1 B1 C1 -170.60(18) . . . 8_657 ?
C6 C1 B1 C1 70.74(12) . . . 7_667 ?
C6 C1 B1 C1 -49.93(15) . . . 2_655 ?
C6 C5 C8 F6 -150.6(7) . . . . ?
C6 C5 C8 F4 91.1(7) . . . . ?
C6 C5 C8 F5 -26.3(9) . . . . ?
C6 C5 C8A F6A -87.3(8) . . . . ?
C6 C5 C8A F5A 25.8(10) . . . . ?
C6 C5 C8A F4A 159.5(7) . . . . ?
C3 C4 C5 C6 0.0(3) . . . . ?
C3 C4 C5 C8 172.9(4) . . . . ?
C3 C4 C5 C8A -175.1(5) . . . . ?
C3 C7 F1A K1 -111(5) . . . . ?
C4 C3 C7 F2 -39.1(15) . . . . ?
C4 C3 C7 F1 79.4(16) . . . . ?
C4 C3 C7 F3 -166(2) . . . . ?
C4 C3 C7 F3A -147.2(7) . . . . ?
C4 C3 C7 F1A 91.3(9) . . . . ?
C4 C3 C7 F2A -27.8(10) . . . . ?
C4 C5 C8 F6 36.3(9) . . . . ?
C4 C5 C8 F4 -82.0(8) . . . . ?
C4 C5 C8 F5 160.6(6) . . . . ?
C4 C5 C8A F6A 87.8(8) . . . . ?
C4 C5 C8A F5A -159.2(7) . . . . ?
C4 C5 C8A F4A -25.4(10) . . . . ?
C5 C8 F6 K1 150.1(8) . . . 5_666 ?
C5 C8A F6A K1 -144.4(5) . . . 5_666 ?
C5 C8A F4A K1 141.5(5) . . . 5_666 ?
C7 C3 C4 C5 -176.7(2) . . . . ?
B1 C1 C2 C3 178.44(16) . . . . ?
B1 C1 C6 C5 -177.85(18) . . . . ?
F3A C7 F1A K1 124(5) . . . . ?
F2A C7 F1A K1 12(5) . . . . ?
F4 C8 F6 K1 -85.1(12) . . . 5_666 ?
F5 C8 F6 K1 21.6(16) . . . 5_666 ?
F6A C8A F4A K1 21.8(11) . . . 5_666 ?
F5A C8A F6A K1 95.6(9) . . . 5_666 ?
F5A C8A F4A K1 -86.1(10) . . . 5_666 ?
F4A C8A F6A K1 -23.2(11) . . . 5_666 ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.135
_oxdiff_exptl_absorpt_empirical_full_min 0.904
_chemical_properties_physical    Hygroscopic
####################################################################### 
# 
# 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_nabarf4
_database_code_depnum_ccdc_archive 'CCDC 1886446'
_audit_update_record             
;
2018-12-20 deposited with the CCDC.
2019-01-31 downloaded from the CCDC.
;
_audit_creation_date             2018-12-15
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.5(C64 H24 B2 F48 Na2)'
_chemical_formula_sum            'C32 H12 B F24 Na'
_chemical_formula_weight         886.22
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C32 H12 B1 F24 Na1'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.1353 0.1239 '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      tetragonal
_space_group_IT_number           85
_space_group_name_H-M_alt        'P 4/n'
_space_group_name_Hall           '-P 4a'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-y+1/2, x, z'
'y, -x+1/2, z'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'y-1/2, -x, -z'
'-y, x-1/2, -z'

_cell_length_a                   13.3508(2)
_cell_length_b                   13.3508(2)
_cell_length_c                   9.3819(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1672.27(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    8506
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      76.2950
_cell_measurement_theta_min      4.6660
_shelx_estimated_absorpt_T_max   0.803
_shelx_estimated_absorpt_T_min   0.724
_exptl_absorpt_coefficient_mu    1.916
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72099
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.760
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             872
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_av_unetI/netI     0.0165
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            15966
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.356
_diffrn_reflns_theta_min         4.684
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5035
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     22.00  49.00   1.00    1.00    --    0.00 -99.00  60.00   27
  2  ω     14.00  43.00   1.00    1.00    --    0.00 -99.00-180.00   29
  3  ω   -103.00  -5.00   1.00    4.00    --  -60.50  77.00-150.00   98
  4  ω   -118.00 -93.00   1.00    4.00    --  -60.50 -94.00 -60.00   25
  5  ω     64.00 116.00   1.00    4.00    --   60.50-125.00 150.00   52
  6  ω    141.00 176.00   1.00   16.00    --  121.00 111.00 150.00   35
  7  ω     35.00  90.00   1.00   16.00    --  121.00 -37.00 120.00   55
  8  ω     77.00 130.00   1.00   16.00    --  121.00  77.00   0.00   53
  9  ω    101.00 127.00   1.00   16.00    --  121.00 111.00 150.00   26
 10  ω    145.00 173.00   1.00   16.00    --  121.00  77.00   0.00   28
 11  ω     45.00  83.00   1.00   16.00    --  121.00 -37.00  30.00   38
 12  ω     28.00  63.00   1.00   16.00    --  121.00 -25.00   0.00   35
 13  ω     32.00  94.00   1.00   16.00    --  121.00-111.00-180.00   62
 14  ω      1.00  26.00   1.00    1.00    --    0.00 -99.00  60.00   25
 15  ω      5.00  30.00   1.00    1.00    --    0.00-101.00-128.00   25
 16  ω   -154.00 -80.00   1.00    4.00    --  -60.50 -94.00-180.00   74
 17  ω      5.00  37.00   1.00    4.00    --   60.50  30.00-180.00   32
 18  ω    124.00 151.00   1.00    4.00    --   60.50 125.00  30.00   27
 19  ω    118.00 146.00   1.00    4.00    --   60.50  30.00-180.00   28
 20  ω     67.00 105.00   1.00   16.00    --  121.00 -50.00-150.00   38
 21  ω    120.00 146.00   1.00   16.00    --  121.00  37.00  90.00   26
 22  ω    137.00 164.00   1.00   16.00    --  121.00 -77.00-150.00   27
 23  ω     81.00 111.00   1.00   16.00    --  121.00-111.00  60.00   30
 24  ω     29.00  55.00   1.00   16.00    --  121.00-111.00  60.00   26
 25  ω     30.00  65.00   1.00   16.00    --  121.00 -37.00-150.00   35
 26  ω     34.00  88.00   1.00   16.00    --  121.00 -25.00-150.00   54
 27  ω     85.00 119.00   1.00   16.00    --  121.00 -77.00-150.00   34
 28  ω     21.00  48.00   1.00   16.00    --  121.00 -77.00-150.00   27
 29  ω      1.00  27.00   1.00    1.00    --    0.00 -99.00  90.00   26
 30  ω      2.00  28.00   1.00    1.00    --    0.00 -99.00 -90.00   26
 31  ω    -98.00 -73.00   1.00    4.00    --  -60.50-125.00 -30.00   25
 32  ω   -142.00-114.00   1.00    4.00    --  -60.50-125.00 -30.00   28
 33  ω   -143.00 -91.00   1.00    4.00    --  -60.50 -94.00 120.00   52
 34  ω    127.00 152.00   1.00    4.00    --   60.50 125.00  90.00   25
 35  ω    114.00 141.00   1.00    4.00    --   60.50 125.00 150.00   27
 36  ω    150.00 177.00   1.00   16.00    --  121.00  50.00-150.00   27
 37  ω    136.00 166.00   1.00   16.00    --  121.00 111.00 120.00   30
 38  ω    150.00 176.00   1.00   16.00    --  121.00 111.00  30.00   26
 39  ω     34.00  71.00   1.00   16.00    --  121.00 -37.00 -90.00   37
 40  ω    110.00 136.00   1.00   16.00    --  121.00  50.00-150.00   26
 41  ω    145.00 173.00   1.00   16.00    --  121.00 111.00-180.00   28
 42  ω    109.00 135.00   1.00   16.00    --  121.00  50.00 120.00   26
 43  ω     64.00  90.00   1.00    1.00    --    0.00  37.00-120.00   26
 44  ω    -34.00  -8.00   1.00    1.00    --    0.00  37.00-120.00   26
 45  ω     -4.00  23.00   1.00    1.00    --    0.00  37.00-120.00   27
 46  ω     -6.00  26.00   1.00    4.00    --  -60.50  30.00 -60.00   32
 47  ω    -48.00 -15.00   1.00    4.00    --  -60.50  30.00 -60.00   33
 48  ω   -146.00 -82.00   1.00    4.00    --  -60.50 -94.00 -90.00   64
 49  ω    -79.00 -53.00   1.00    4.00    --  -60.50 125.00 -30.00   26
 50  ω     35.00 120.00   1.00    4.00    --   60.50  30.00-180.00   85
 51  ω     96.00 122.00   1.00    4.00    --   60.50 125.00 120.00   26
 52  ω     61.00  87.00   1.00   16.00    --  121.00-111.00   0.00   26
 53  ω     79.00 105.00   1.00   16.00    --  121.00-111.00  90.00   26
 54  ω     50.00  76.00   1.00   16.00    --  121.00-111.00 -90.00   26
 55  ω     45.00 111.00   1.00   16.00    --  121.00-111.00-150.00   66
 56  ω    152.00 177.00   1.00   16.00    --  121.00 111.00  90.00   25
 57  ω     47.00 112.00   1.00   16.00    --  121.00-111.00 120.00   65
 58  ω     80.00 130.00   1.00   16.00    --  121.00  50.00 150.00   50
 59  ω     73.00 112.00   1.00   16.00    --  121.00-111.00  30.00   39
 60  ω     89.00 174.00   1.00   16.00    --  121.00 -12.00-180.00   85
 61  ω     32.00  68.00   1.00   16.00    --  121.00 -12.00-180.00   36
 62  ω     46.00 109.00   1.00   16.00    --  121.00-111.00 150.00   63
 63  ω     78.00 106.00   1.00   16.00    --  121.00-111.00 -30.00   28
 64  ω     46.00  72.00   1.00   16.00    --  121.00 -37.00-150.00   26
 65  ω    109.00 147.00   1.00   16.00    --  121.00 111.00-180.00   38
 66  ω     79.00 112.00   1.00   16.00    --  121.00-111.00 -90.00   33
 67  ω    141.00 166.00   1.00   16.00    --  121.00  50.00 150.00   25
 68  ω     60.00  86.00   1.00   16.00    --  121.00-111.00-120.00   26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0830135000
_diffrn_orient_matrix_UB_12      -0.0758576000
_diffrn_orient_matrix_UB_13      0.0366261000
_diffrn_orient_matrix_UB_21      -0.0419119000
_diffrn_orient_matrix_UB_22      0.0094967000
_diffrn_orient_matrix_UB_23      -0.1524285000
_diffrn_orient_matrix_UB_31      0.0684564000
_diffrn_orient_matrix_UB_32      -0.0862975000
_diffrn_orient_matrix_UB_33      -0.0489514000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1693
_reflns_number_total             1762
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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         0.536
_refine_diff_density_min         -0.474
_refine_diff_density_rms         0.067
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     160
_refine_ls_number_reflns         1762
_refine_ls_number_restraints     138
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_gt           0.0610
_refine_ls_restrained_S_all      1.195
_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)+(0.0608P)²+2.8250P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1530
_refine_ls_wR_factor_ref         0.1541
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 F6-F5 \\sim F6-F4 \\sim F5A-F4A \\sim F5A-F6A \\sim F5-F4 \\sim F4A-F6A
 with sigma of 0.02
 C8-F6 \\sim C8-F5A \\sim C8-F5 \\sim C8-F4A \\sim C8-F4 \\sim C8-F6A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C8 \\sim F4 \\sim F5 \\sim F6 \\sim F4A \\sim F5A \\sim F6A: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.01
4. Rigid body (RIGU) restrains
 C8, F4, F5, F6, F4A, F5A, F6A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(F4A)=Sof(F5A)=Sof(F6A)=1-FVAR(1)
 Sof(F4)=Sof(F5)=Sof(F6)=FVAR(1)
6.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C6(H6)
;
_atom_sites_solution_hydrogens   geom
_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
Na1 Na 0.250000 0.250000 0.5854(2) 0.0351(5) Uani 1 4 d S T P . .
F1 F 0.37081(13) 0.34661(15) 0.7304(3) 0.0599(6) Uani 1 1 d . . . . .
F2 F 0.38116(13) 0.49699(13) 0.8032(2) 0.0518(5) Uani 1 1 d . . . . .
F3 F 0.38047(14) 0.3778(2) 0.9524(3) 0.0809(9) Uani 1 1 d . . . . .
C1 C 0.68336(17) 0.32281(16) 0.8962(2) 0.0222(5) Uani 1 1 d . . . . .
C2 C 0.58001(17) 0.33565(17) 0.9071(2) 0.0239(5) Uani 1 1 d . . . . .
H2 H 0.544509 0.299967 0.978694 0.029 Uiso 1 1 calc R . . . .
C3 C 0.52719(17) 0.39909(18) 0.8165(3) 0.0264(5) Uani 1 1 d . . . . .
C4 C 0.57552(19) 0.45242(19) 0.7107(3) 0.0299(5) Uani 1 1 d . . . . .
H4 H 0.539459 0.496159 0.649514 0.036 Uiso 1 1 calc R . . . .
C5 C 0.67847(18) 0.44028(19) 0.6964(3) 0.0285(5) Uani 1 1 d . . . . .
C6 C 0.73077(17) 0.37606(18) 0.7863(2) 0.0257(5) Uani 1 1 d . . . . .
H6 H 0.800837 0.367995 0.772945 0.031 Uiso 1 1 calc R . . . .
C7 C 0.41625(19) 0.4064(2) 0.8280(3) 0.0333(6) Uani 1 1 d . . . . .
C8 C 0.7318(2) 0.4924(2) 0.5780(3) 0.0424(7) Uani 1 1 d D U . . .
B1 B 0.750000 0.250000 1.000000 0.0221(9) Uani 1 4 d S T P . .
F4 F 0.7125(2) 0.4515(2) 0.4499(2) 0.0796(9) Uani 0.902(3) 1 d D U . A 1
F5 F 0.7073(2) 0.58906(18) 0.5645(3) 0.0712(9) Uani 0.902(3) 1 d D U . A 1
F6 F 0.83037(14) 0.48953(18) 0.5869(2) 0.0513(6) Uani 0.902(3) 1 d D U . A 1
F4A F 0.6676(12) 0.5417(15) 0.5001(19) 0.056(3) Uani 0.098(3) 1 d D U . A 2
F5A F 0.7855(14) 0.5632(13) 0.6479(19) 0.064(3) Uani 0.098(3) 1 d D U . A 2
F6A F 0.7917(14) 0.4417(14) 0.502(2) 0.065(3) Uani 0.098(3) 1 d D U . 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
Na1 F1 2.473(2) . ?
Na1 F1 2.473(2) 2 ?
Na1 F1 2.473(2) 3 ?
Na1 F1 2.473(2) 4 ?
Na1 F5 2.631(2) 6_556 ?
Na1 F5 2.631(2) 7_566 ?
Na1 F5 2.631(2) 8_656 ?
Na1 F5 2.631(2) 5_666 ?
F1 C7 1.358(3) . ?
F2 C7 1.318(3) . ?
F3 C7 1.317(3) . ?
C1 C2 1.394(3) . ?
C1 C6 1.403(3) . ?
C1 B1 1.639(2) . ?
C2 H2 0.9500 . ?
C2 C3 1.392(3) . ?
C3 C4 1.381(4) . ?
C3 C7 1.488(3) . ?
C4 H4 0.9500 . ?
C4 C5 1.390(3) . ?
C5 C6 1.391(3) . ?
C5 C8 1.492(4) . ?
C6 H6 0.9500 . ?
C8 F4 1.345(4) . ?
C8 F5 1.337(4) . ?
C8 F6 1.319(3) . ?
C8 F4A 1.305(11) . ?
C8 F5A 1.355(12) . ?
C8 F6A 1.269(12) . ?

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 Na1 F1 72.38(7) . 3 ?
F1 Na1 F1 72.38(7) . 4 ?
F1 Na1 F1 113.23(15) 3 4 ?
F1 Na1 F1 72.38(7) 3 2 ?
F1 Na1 F1 113.23(15) . 2 ?
F1 Na1 F1 72.38(7) 2 4 ?
F1 Na1 F5 149.49(7) . 6_556 ?
F1 Na1 F5 74.14(10) 2 6_556 ?
F1 Na1 F5 74.14(10) . 5_666 ?
F1 Na1 F5 135.54(8) 3 6_556 ?
F1 Na1 F5 82.80(8) . 8_656 ?
F1 Na1 F5 135.54(8) 2 8_656 ?
F1 Na1 F5 82.80(8) 2 7_566 ?
F1 Na1 F5 149.49(7) 4 7_566 ?
F1 Na1 F5 74.14(10) 4 8_656 ?
F1 Na1 F5 149.49(7) 2 5_666 ?
F1 Na1 F5 135.54(8) . 7_566 ?
F1 Na1 F5 82.80(8) 4 6_556 ?
F1 Na1 F5 74.14(10) 3 7_566 ?
F1 Na1 F5 82.80(8) 3 5_666 ?
F1 Na1 F5 135.54(8) 4 5_666 ?
F1 Na1 F5 149.49(7) 3 8_656 ?
F5 Na1 F5 73.40(8) 6_556 7_566 ?
F5 Na1 F5 73.40(8) 7_566 5_666 ?
F5 Na1 F5 115.37(17) 7_566 8_656 ?
F5 Na1 F5 73.40(8) 5_666 8_656 ?
F5 Na1 F5 73.40(8) 6_556 8_656 ?
F5 Na1 F5 115.37(17) 6_556 5_666 ?
C7 F1 Na1 165.70(18) . . ?
C2 C1 C6 116.0(2) . . ?
C2 C1 B1 124.51(18) . . ?
C6 C1 B1 119.49(18) . . ?
C1 C2 H2 119.0 . . ?
C3 C2 C1 122.1(2) . . ?
C3 C2 H2 119.0 . . ?
C2 C3 C7 120.0(2) . . ?
C4 C3 C2 121.0(2) . . ?
C4 C3 C7 118.9(2) . . ?
C3 C4 H4 120.9 . . ?
C3 C4 C5 118.1(2) . . ?
C5 C4 H4 120.9 . . ?
C4 C5 C6 120.6(2) . . ?
C4 C5 C8 119.3(2) . . ?
C6 C5 C8 120.0(2) . . ?
C1 C6 H6 118.9 . . ?
C5 C6 C1 122.1(2) . . ?
C5 C6 H6 118.9 . . ?
F1 C7 C3 110.9(2) . . ?
F2 C7 F1 105.1(2) . . ?
F2 C7 C3 113.6(2) . . ?
F3 C7 F1 105.4(3) . . ?
F3 C7 F2 107.1(2) . . ?
F3 C7 C3 114.0(2) . . ?
F4 C8 C5 112.6(3) . . ?
F5 C8 C5 113.8(3) . . ?
F5 C8 F4 105.1(3) . . ?
F6 C8 C5 114.6(2) . . ?
F6 C8 F4 103.6(3) . . ?
F6 C8 F5 106.2(3) . . ?
F4A C8 C5 109.8(9) . . ?
F4A C8 F5A 105.5(10) . . ?
F5A C8 C5 102.6(9) . . ?
F6A C8 C5 118.1(10) . . ?
F6A C8 F4A 111.6(11) . . ?
F6A C8 F5A 108.2(10) . . ?
C1 B1 C1 107.07(15) 7_667 8_657 ?
C1 B1 C1 110.69(8) 7_667 2_655 ?
C1 B1 C1 110.69(8) . 8_657 ?
C1 B1 C1 110.69(8) 2_655 8_657 ?
C1 B1 C1 110.68(8) . 7_667 ?
C1 B1 C1 107.07(15) . 2_655 ?
C8 F5 Na1 141.8(2) . 5_666 ?

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
Na1 F1 C7 F2 -64.2(8) . . . . ?
Na1 F1 C7 F3 48.7(8) . . . . ?
Na1 F1 C7 C3 172.6(7) . . . . ?
C1 C2 C3 C4 0.1(4) . . . . ?
C1 C2 C3 C7 177.0(2) . . . . ?
C2 C1 C6 C5 1.9(3) . . . . ?
C2 C1 B1 C1 -111.0(3) . . . 7_667 ?
C2 C1 B1 C1 128.3(2) . . . 2_655 ?
C2 C1 B1 C1 7.5(2) . . . 8_657 ?
C2 C3 C4 C5 0.6(4) . . . . ?
C2 C3 C7 F1 -97.3(3) . . . . ?
C2 C3 C7 F2 144.5(2) . . . . ?
C2 C3 C7 F3 21.5(4) . . . . ?
C3 C4 C5 C6 0.0(4) . . . . ?
C3 C4 C5 C8 176.6(2) . . . . ?
C4 C3 C7 F1 79.8(3) . . . . ?
C4 C3 C7 F2 -38.4(4) . . . . ?
C4 C3 C7 F3 -161.5(3) . . . . ?
C4 C5 C6 C1 -1.4(4) . . . . ?
C4 C5 C8 F4 -72.4(4) . . . . ?
C4 C5 C8 F5 47.1(4) . . . . ?
C4 C5 C8 F6 169.5(3) . . . . ?
C4 C5 C8 F4A -2.0(11) . . . . ?
C4 C5 C8 F5A 109.8(9) . . . . ?
C4 C5 C8 F6A -131.4(11) . . . . ?
C5 C8 F5 Na1 177.5(3) . . . 5_666 ?
C6 C1 C2 C3 -1.3(3) . . . . ?
C6 C1 B1 C1 -50.84(16) . . . 2_655 ?
C6 C1 B1 C1 69.89(14) . . . 7_667 ?
C6 C1 B1 C1 -171.6(2) . . . 8_657 ?
C6 C5 C8 F4 104.2(3) . . . . ?
C6 C5 C8 F5 -136.4(3) . . . . ?
C6 C5 C8 F6 -13.9(4) . . . . ?
C6 C5 C8 F4A 174.6(11) . . . . ?
C6 C5 C8 F5A -73.6(9) . . . . ?
C6 C5 C8 F6A 45.1(12) . . . . ?
C7 C3 C4 C5 -176.4(2) . . . . ?
C8 C5 C6 C1 -177.9(2) . . . . ?
B1 C1 C2 C3 179.58(18) . . . . ?
B1 C1 C6 C5 -178.89(19) . . . . ?
F4 C8 F5 Na1 -58.9(5) . . . 5_666 ?
F6 C8 F5 Na1 50.5(5) . . . 5_666 ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.756
_oxdiff_exptl_absorpt_empirical_full_min 0.741
_chemical_properties_physical    Hygroscopic
