# 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_[Li(Me~6~[18]aneN~6~)][BArF]
_database_code_depnum_ccdc_archive 'CCDC 1051099'
_audit_update_record             
;
2015-02-24 deposited with the CCDC.
2015-06-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H12 B F24, C18 H42 Li N6'
_chemical_formula_sum            'C50 H54 B F24 Li N6'
_chemical_formula_weight         1212.74

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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 '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'

_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                   13.180(3)
_cell_length_b                   16.887(4)
_cell_length_c                   24.300(5)
_cell_angle_alpha                90
_cell_angle_beta                 92.212(3)
_cell_angle_gamma                90
_cell_volume                     5404.6(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    14009
_cell_measurement_theta_min      2.3
_cell_measurement_theta_max      27.5

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.490
_exptl_crystal_F_000             2480
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    0.146
_shelx_estimated_absorpt_T_min   0.991
_shelx_estimated_absorpt_T_max   0.994
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.680
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'CrystalClear-SM Expert 2.1 b29 (Rigaku, 2013)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Sealed Tube'
_diffrn_radiation_monochromator  Mirrors
_diffrn_measurement_specimen_support Fiber
_diffrn_detector                 CCD
_diffrn_measurement_device       
;
AFC12 (Right): Kappa 3 circle
;
_diffrn_measurement_device_type  
;
Rigaku Saturn724+ (2x2 bin mode)
;
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_reflns_number            25326
_diffrn_reflns_av_unetI/netI     0.0651
_diffrn_reflns_av_R_equivalents  0.0533
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         2.939
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.971
_reflns_number_total             9506
_reflns_number_gt                5786
_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       
;
CrystalClear-SM Expert 2.1 b29 (Rigaku, 2013)
;
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.1 b29 (Rigaku, 2013)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.1 b29 (Rigaku, 2013)
;
_computing_structure_solution    'SUPERFLIP (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'ORTEP-III (Farrugia, 2012)'
_computing_publication_material  
'PLATON (Spek, 2003), WinGX (Farrugia, 1999) and enCIFer (Allen et al., 2004).'

_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)+(0.0971P)²+13.1817P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9506
_refine_ls_number_parameters     789
_refine_ls_number_restraints     78
_refine_ls_R_factor_all          0.1402
_refine_ls_R_factor_gt           0.0836
_refine_ls_wR_factor_ref         0.2379
_refine_ls_wR_factor_gt          0.1998
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_restrained_S_all      1.065
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
C1 C 0.1908(3) 0.3266(2) 0.10420(17) 0.0248(9) Uani 1 1 d . . . . .
C2 C 0.2169(3) 0.2941(3) 0.05377(17) 0.0277(9) Uani 1 1 d . . . . .
H2 H 0.2707 0.3173 0.0344 0.033 Uiso 1 1 calc R U . . .
C3 C 0.1665(3) 0.2289(3) 0.03107(17) 0.0285(10) Uani 1 1 d . . . . .
C4 C 0.0849(3) 0.1958(3) 0.05652(18) 0.0320(10) Uani 1 1 d . . . . .
H4 H 0.0499 0.1517 0.0406 0.038 Uiso 1 1 calc R U . . .
C5 C 0.0551(3) 0.2282(3) 0.10566(18) 0.0309(10) Uani 1 1 d . . . . .
C6 C 0.1079(3) 0.2920(3) 0.12912(17) 0.0266(9) Uani 1 1 d . . . . .
H6 H 0.0869 0.3127 0.1632 0.032 Uiso 1 1 calc R U . . .
C7 C 0.2007(4) 0.1950(3) -0.02211(19) 0.0369(11) Uani 1 1 d . . . . .
C8 C -0.0326(4) 0.1940(3) 0.13445(19) 0.0415(12) Uani 1 1 d . . . . .
C9 C 0.3641(3) 0.4126(2) 0.10973(17) 0.0264(9) Uani 1 1 d . . . . .
C10 C 0.4125(3) 0.4846(2) 0.09938(17) 0.0259(9) Uani 1 1 d . . . . .
H10 H 0.3756 0.5325 0.1030 0.031 Uiso 1 1 calc R U . . .
C11 C 0.5126(3) 0.4882(3) 0.08404(17) 0.0291(10) Uani 1 1 d . . . . .
C12 C 0.5691(3) 0.4200(3) 0.07784(18) 0.0326(10) Uani 1 1 d . . . . .
H12 H 0.6371 0.4224 0.0663 0.039 Uiso 1 1 calc R U . . .
C13 C 0.5239(3) 0.3483(3) 0.08894(19) 0.0326(10) Uani 1 1 d . . . . .
C14 C 0.4242(3) 0.3448(3) 0.10499(18) 0.0286(10) Uani 1 1 d . . . . .
H14 H 0.3957 0.2947 0.1131 0.034 Uiso 1 1 calc R U . . .
C15 C 0.5632(4) 0.5669(3) 0.07669(18) 0.0338(11) Uani 1 1 d . . . . .
C16 C 0.5832(4) 0.2735(3) 0.0824(3) 0.0486(14) Uani 1 1 d . . . . .
C17 C 0.1739(3) 0.4787(2) 0.10880(17) 0.0271(9) Uani 1 1 d . . . . .
C18 C 0.1817(3) 0.5123(3) 0.05647(18) 0.0286(10) Uani 1 1 d . . . . .
H18 H 0.2367 0.4971 0.0346 0.034 Uiso 1 1 calc R U . . .
C19 C 0.1120(3) 0.5668(3) 0.03546(19) 0.0323(10) Uani 1 1 d . . . . .
C20 C 0.0302(3) 0.5910(3) 0.0660(2) 0.0356(11) Uani 1 1 d . . . . .
H20 H -0.0174 0.6287 0.0517 0.043 Uiso 1 1 calc R U . . .
C21 C 0.0210(3) 0.5585(3) 0.11746(19) 0.0337(11) Uani 1 1 d . . . . .
C22 C 0.0903(3) 0.5033(3) 0.13809(18) 0.0307(10) Uani 1 1 d . . . . .
H22 H 0.0807 0.4813 0.1735 0.037 Uiso 1 1 calc R U . . .
C23 C 0.1252(4) 0.6034(3) -0.0198(2) 0.0422(13) Uani 1 1 d . . . . .
C24 C -0.0655(4) 0.5829(4) 0.1516(2) 0.0482(14) Uani 1 1 d . . . . .
C25 C 0.2599(3) 0.4006(2) 0.19752(17) 0.0241(9) Uani 1 1 d . . . . .
C26 C 0.2800(3) 0.3289(3) 0.22440(17) 0.0275(9) Uani 1 1 d . . . . .
H26 H 0.2810 0.2818 0.2031 0.033 Uiso 1 1 calc R U . . .
C27 C 0.2986(3) 0.3233(3) 0.28073(18) 0.0302(10) Uani 1 1 d . . . . .
C28 C 0.2948(3) 0.3900(3) 0.31345(19) 0.0351(11) Uani 1 1 d . . . . .
H28 H 0.3048 0.3861 0.3523 0.042 Uiso 1 1 calc R U . . .
C29 C 0.2764(3) 0.4623(3) 0.28867(19) 0.0337(11) Uani 1 1 d . . . . .
C30 C 0.2600(3) 0.4677(3) 0.23176(18) 0.0307(10) Uani 1 1 d . . . . .
H30 H 0.2485 0.5184 0.2156 0.037 Uiso 1 1 calc R U . . .
C31 C 0.3235(4) 0.2437(3) 0.30546(18) 0.0349(11) Uani 1 1 d . . . . .
C32 C 0.2758(4) 0.5354(3) 0.3227(2) 0.0496(14) Uani 1 1 d . . . . .
C33 C 0.3040(6) 0.9228(5) 0.2829(3) 0.086(2) Uani 1 1 d . . . . .
H33A H 0.2547 0.8809 0.2899 0.129 Uiso 1 1 calc R U . . .
H33B H 0.2687 0.9738 0.2795 0.129 Uiso 1 1 calc R U . . .
H33C H 0.3545 0.9251 0.3135 0.129 Uiso 1 1 calc R U . . .
C34 C 0.4294(5) 0.9681(4) 0.2206(3) 0.077(2) Uani 1 1 d . . . . .
H34A H 0.4707 0.9498 0.1899 0.093 Uiso 1 1 calc R U . . .
H34B H 0.4755 0.9767 0.2531 0.093 Uiso 1 1 calc R U . . .
C35 C 0.3781(4) 1.0449(3) 0.2049(2) 0.0541(15) Uani 1 1 d . . . . .
H35A H 0.3434 1.0659 0.2372 0.065 Uiso 1 1 calc R U . . .
H35B H 0.4304 1.0838 0.1948 0.065 Uiso 1 1 calc R U . . .
C36 C 0.2143(5) 1.0865(3) 0.1688(3) 0.0673(18) Uani 1 1 d . . . . .
H36A H 0.1854 1.0713 0.2038 0.101 Uiso 1 1 calc R U . . .
H36B H 0.1635 1.0790 0.1388 0.101 Uiso 1 1 calc R U . . .
H36C H 0.2347 1.1423 0.1704 0.101 Uiso 1 1 calc R U . . .
C37 C 0.3455(6) 1.0628(4) 0.1071(3) 0.0708(19) Uani 1 1 d . . . . .
H37A H 0.3756 1.1161 0.1122 0.085 Uiso 1 1 calc R U . . .
H37B H 0.2896 1.0671 0.0788 0.085 Uiso 1 1 calc R U . . .
C38 C 0.4246(5) 1.0077(4) 0.0868(3) 0.074(2) Uani 1 1 d . . . . .
H38A H 0.4502 1.0287 0.0518 0.088 Uiso 1 1 calc R U . . .
H38B H 0.4824 1.0061 0.1140 0.088 Uiso 1 1 calc R U . . .
C39 C 0.4706(5) 0.8687(5) 0.0750(3) 0.080(2) Uani 1 1 d . . . . .
H39A H 0.4430 0.8157 0.0678 0.121 Uiso 1 1 calc R U . . .
H39B H 0.5093 0.8687 0.1103 0.121 Uiso 1 1 calc R U . . .
H39C H 0.5153 0.8837 0.0454 0.121 Uiso 1 1 calc R U . . .
C40 C 0.3257(5) 0.9224(4) 0.0253(2) 0.0580(16) Uani 1 1 d . . . . .
H40A H 0.3693 0.9051 -0.0048 0.070 Uiso 1 1 calc R U . . .
H40B H 0.2991 0.9757 0.0160 0.070 Uiso 1 1 calc R U . . .
C41 C 0.2367(5) 0.8643(4) 0.0299(2) 0.0632(17) Uani 1 1 d . . . . .
H41A H 0.2005 0.8594 -0.0064 0.076 Uiso 1 1 calc R U . . .
H41B H 0.2633 0.8114 0.0405 0.076 Uiso 1 1 calc R U . . .
C42 C 0.1047(5) 0.9562(4) 0.0503(3) 0.0687(18) Uani 1 1 d . . . . .
H42A H 0.1490 1.0006 0.0414 0.103 Uiso 1 1 calc R U . . .
H42B H 0.0582 0.9726 0.0787 0.103 Uiso 1 1 calc R U . . .
H42C H 0.0655 0.9398 0.0172 0.103 Uiso 1 1 calc R U . . .
C43 C 0.0977(5) 0.8235(4) 0.0824(2) 0.0610(16) Uani 1 1 d . . . . .
H43A H 0.1386 0.7759 0.0918 0.073 Uiso 1 1 calc R U . . .
H43B H 0.0544 0.8112 0.0493 0.073 Uiso 1 1 calc R U . . .
C44 C 0.0289(4) 0.8452(4) 0.1318(2) 0.0640(17) Uani 1 1 d . . . . .
H44A H -0.0134 0.8917 0.1215 0.077 Uiso 1 1 calc R U . . .
H44B H -0.0172 0.8003 0.1388 0.077 Uiso 1 1 calc R U . . .
C45 C 0.0339(5) 0.9222(5) 0.2132(3) 0.073(2) Uani 1 1 d . . . . .
H45A H -0.0335 0.9014 0.2210 0.110 Uiso 1 1 calc R U . . .
H45B H 0.0265 0.9704 0.1909 0.110 Uiso 1 1 calc R U . . .
H45C H 0.0708 0.9347 0.2479 0.110 Uiso 1 1 calc R U . . .
C46 C 0.1008(5) 0.7909(4) 0.2170(2) 0.0639(17) Uani 1 1 d . . . . .
H46A H 0.0326 0.7678 0.2215 0.077 Uiso 1 1 calc R U . . .
H46B H 0.1284 0.8058 0.2540 0.077 Uiso 1 1 calc R U . . .
C47 C 0.1675(5) 0.7289(4) 0.1940(3) 0.0635(17) Uani 1 1 d . . . . .
H47A H 0.1708 0.6833 0.2195 0.076 Uiso 1 1 calc R U . . .
H47B H 0.1367 0.7102 0.1585 0.076 Uiso 1 1 calc R U . . .
C48 C 0.3226(5) 0.7027(4) 0.1485(3) 0.0709(19) Uani 1 1 d . . . . .
H48A H 0.3180 0.6485 0.1625 0.106 Uiso 1 1 calc R U . . .
H48B H 0.3942 0.7181 0.1470 0.106 Uiso 1 1 calc R U . . .
H48C H 0.2907 0.7055 0.1114 0.106 Uiso 1 1 calc R U . . .
C49 C 0.3299(5) 0.7612(4) 0.2376(3) 0.0712(19) Uani 1 1 d . . . . .
H49A H 0.3662 0.7106 0.2442 0.085 Uiso 1 1 calc R U . . .
H49B H 0.2829 0.7691 0.2679 0.085 Uiso 1 1 calc R U . . .
C50 C 0.4088(5) 0.8307(4) 0.2379(3) 0.0726(19) Uani 1 1 d . . . . .
H50A H 0.4510 0.8297 0.2725 0.087 Uiso 1 1 calc R U . . .
H50B H 0.4542 0.8249 0.2067 0.087 Uiso 1 1 calc R U . . .
Li1 Li 0.2582(6) 0.9004(5) 0.1533(3) 0.0399(19) Uani 1 1 d . . . . .
B1 B 0.2468(4) 0.4061(3) 0.1301(2) 0.0262(11) Uani 1 1 d . . . . .
N1 N 0.3531(3) 0.9062(2) 0.23334(18) 0.0447(11) Uani 1 1 d . . . . .
N2 N 0.3038(3) 1.0369(2) 0.15889(18) 0.0473(11) Uani 1 1 d . . . . .
N3 N 0.3865(3) 0.9260(3) 0.07734(18) 0.0522(12) Uani 1 1 d . . . . .
N4 N 0.1658(3) 0.8906(2) 0.07059(17) 0.0408(10) Uani 1 1 d . . . . .
N5 N 0.0897(4) 0.8634(3) 0.18328(19) 0.0564(12) Uani 1 1 d . . . . .
N6 N 0.2708(4) 0.7564(3) 0.1849(2) 0.0569(13) Uani 1 1 d . . . . .
F1 F 0.1676(3) 0.2356(2) -0.06533(12) 0.0643(10) Uani 1 1 d . . . . .
F2 F 0.3007(2) 0.1914(3) -0.02438(14) 0.0797(12) Uani 1 1 d . . . . .
F3 F 0.1668(3) 0.12090(18) -0.03143(13) 0.0667(10) Uani 1 1 d . . . . .
F4 F -0.0746(3) 0.1331(3) 0.10746(14) 0.0963(15) Uani 1 1 d . U . . .
F5 F -0.0077(2) 0.16854(18) 0.18457(11) 0.0511(8) Uani 1 1 d . . . . .
F6 F -0.1059(2) 0.2466(3) 0.14131(15) 0.0742(11) Uani 1 1 d . . . . .
F7 F 0.4991(2) 0.62488(18) 0.06569(18) 0.0735(11) Uani 1 1 d . . . . .
F8 F 0.6173(3) 0.5872(2) 0.12114(14) 0.0855(13) Uani 1 1 d . . . . .
F9 F 0.6276(3) 0.56740(18) 0.03641(14) 0.0621(9) Uani 1 1 d . . . . .
F10A F 0.5392(14) 0.2243(9) 0.0498(7) 0.071(4) Uani 0.272(10) 1 d . U P A 1
F11A F 0.6716(16) 0.2757(10) 0.0859(8) 0.071(4) Uani 0.272(10) 1 d . . P A 1
F12A F 0.5694(13) 0.2263(8) 0.1323(6) 0.071(4) Uani 0.272(10) 1 d . U P A 1
F10B F 0.6701(5) 0.2745(4) 0.1139(3) 0.074(2) Uani 0.728(10) 1 d . U P A 2
F11B F 0.5340(4) 0.2087(3) 0.0907(4) 0.100(3) Uani 0.728(10) 1 d . U P A 2
F12B F 0.6189(5) 0.2663(3) 0.0314(2) 0.081(2) Uani 0.728(10) 1 d . U P A 2
F13 F 0.1775(2) 0.5591(2) -0.05330(11) 0.0546(8) Uani 1 1 d . . . . .
F14 F 0.1716(4) 0.6720(2) -0.01651(15) 0.0924(14) Uani 1 1 d . . . . .
F15 F 0.0361(2) 0.6155(2) -0.04730(14) 0.0702(11) Uani 1 1 d . . . . .
F16A F -0.1418(11) 0.5444(11) 0.1492(7) 0.078(5) Uani 0.416(15) 1 d . U P B 1
F17A F -0.0402(14) 0.5882(10) 0.2070(6) 0.067(5) Uani 0.416(15) 1 d . . P B 1
F18A F -0.0867(10) 0.6623(6) 0.1452(5) 0.063(4) Uani 0.416(15) 1 d . U P B 1
F16B F -0.0419(10) 0.6141(9) 0.1957(6) 0.088(4) Uani 0.584(15) 1 d . U P B 2
F17B F -0.1401(6) 0.6174(7) 0.1210(3) 0.077(4) Uani 0.584(15) 1 d . U P B 2
F18B F -0.1219(7) 0.5128(6) 0.1646(4) 0.061(2) Uani 0.584(15) 1 d . U P B 2
F19 F 0.4083(2) 0.21396(16) 0.28576(12) 0.0461(7) Uani 1 1 d . . . . .
F20 F 0.2526(2) 0.18986(18) 0.29326(15) 0.0601(9) Uani 1 1 d . . . . .
F21 F 0.3368(4) 0.24657(19) 0.35948(12) 0.0813(13) Uani 1 1 d . . . . .
F22 F 0.3661(3) 0.5746(2) 0.3205(2) 0.0983(15) Uani 1 1 d . U . . .
F23 F 0.2096(3) 0.58889(18) 0.30495(12) 0.0588(9) Uani 1 1 d . . . . .
F24 F 0.2647(4) 0.5235(2) 0.37503(14) 0.1017(16) Uani 1 1 d . U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C6 1.397(6) . ?
C1 C2 1.398(6) . ?
C1 B1 1.646(6) . ?
C2 C3 1.389(6) . ?
C2 H2 0.9500 . ?
C3 C4 1.379(6) . ?
C3 C7 1.498(6) . ?
C4 C5 1.384(6) . ?
C4 H4 0.9500 . ?
C5 C6 1.393(6) . ?
C5 C8 1.491(6) . ?
C6 H6 0.9500 . ?
C7 F1 1.315(5) . ?
C7 F2 1.323(6) . ?
C7 F3 1.345(6) . ?
C8 F5 1.321(5) . ?
C8 F6 1.327(6) . ?
C8 F4 1.329(6) . ?
C9 C14 1.399(6) . ?
C9 C10 1.401(6) . ?
C9 B1 1.644(6) . ?
C10 C11 1.386(6) . ?
C10 H10 0.9500 . ?
C11 C12 1.384(6) . ?
C11 C15 1.501(6) . ?
C12 C13 1.381(6) . ?
C12 H12 0.9500 . ?
C13 C14 1.386(6) . ?
C13 C16 1.496(7) . ?
C14 H14 0.9500 . ?
C15 F7 1.315(5) . ?
C15 F8 1.316(5) . ?
C15 F9 1.320(5) . ?
C16 F11A 1.17(2) . ?
C16 F10A 1.272(16) . ?
C16 F11B 1.292(7) . ?
C16 F12B 1.348(8) . ?
C16 F10B 1.351(8) . ?
C16 F12A 1.468(16) . ?
C17 C22 1.397(6) . ?
C17 C18 1.400(6) . ?
C17 B1 1.631(6) . ?
C18 C19 1.383(6) . ?
C18 H18 0.9500 . ?
C19 C20 1.393(6) . ?
C19 C23 1.495(6) . ?
C20 C21 1.376(6) . ?
C20 H20 0.9500 . ?
C21 C22 1.385(6) . ?
C21 C24 1.494(7) . ?
C22 H22 0.9500 . ?
C23 F14 1.312(6) . ?
C23 F13 1.319(6) . ?
C23 F15 1.344(6) . ?
C24 F16A 1.197(14) . ?
C24 F16B 1.223(13) . ?
C24 F17B 1.342(8) . ?
C24 F17A 1.377(17) . ?
C24 F18A 1.377(10) . ?
C24 F18B 1.438(11) . ?
C25 C26 1.397(6) . ?
C25 C30 1.406(6) . ?
C25 B1 1.642(6) . ?
C26 C27 1.384(6) . ?
C26 H26 0.9500 . ?
C27 C28 1.379(6) . ?
C27 C31 1.505(6) . ?
C28 C29 1.379(7) . ?
C28 H28 0.9500 . ?
C29 C30 1.395(6) . ?
C29 C32 1.486(7) . ?
C30 H30 0.9500 . ?
C31 F21 1.319(5) . ?
C31 F20 1.329(6) . ?
C31 F19 1.331(5) . ?
C32 F24 1.302(6) . ?
C32 F23 1.317(6) . ?
C32 F22 1.364(7) . ?
C33 N1 1.417(8) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 N1 1.492(8) . ?
C34 C35 1.504(9) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 N2 1.463(7) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 N2 1.475(7) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 N2 1.460(8) . ?
C37 C38 1.496(10) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C38 N3 1.483(8) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 N3 1.474(8) . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 N3 1.472(7) . ?
C40 C41 1.536(9) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C41 N4 1.455(7) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 N4 1.444(7) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 N4 1.482(7) . ?
C43 C44 1.575(9) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 N5 1.492(7) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C45 N5 1.449(8) . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 N5 1.477(8) . ?
C46 C47 1.489(9) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 N6 1.463(8) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 N6 1.455(8) . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C49 N6 1.475(7) . ?
C49 C50 1.568(9) . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C50 N1 1.473(7) . ?
C50 H50A 0.9900 . ?
C50 H50B 0.9900 . ?
Li1 N1 2.274(9) . ?
Li1 N4 2.315(9) . ?
Li1 N2 2.384(9) . ?
Li1 N5 2.445(10) . ?
Li1 N6 2.554(9) . ?
Li1 N3 2.587(9) . ?

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
C6 C1 C2 116.0(4) . . ?
C6 C1 B1 121.5(4) . . ?
C2 C1 B1 122.2(4) . . ?
C3 C2 C1 121.9(4) . . ?
C3 C2 H2 119.0 . . ?
C1 C2 H2 119.0 . . ?
C4 C3 C2 120.8(4) . . ?
C4 C3 C7 119.8(4) . . ?
C2 C3 C7 119.3(4) . . ?
C3 C4 C5 118.6(4) . . ?
C3 C4 H4 120.7 . . ?
C5 C4 H4 120.7 . . ?
C4 C5 C6 120.3(4) . . ?
C4 C5 C8 120.2(4) . . ?
C6 C5 C8 119.5(4) . . ?
C5 C6 C1 122.2(4) . . ?
C5 C6 H6 118.9 . . ?
C1 C6 H6 118.9 . . ?
F1 C7 F2 107.0(4) . . ?
F1 C7 F3 104.6(4) . . ?
F2 C7 F3 105.9(4) . . ?
F1 C7 C3 112.9(4) . . ?
F2 C7 C3 112.8(4) . . ?
F3 C7 C3 113.1(4) . . ?
F5 C8 F6 105.0(4) . . ?
F5 C8 F4 106.7(4) . . ?
F6 C8 F4 106.8(4) . . ?
F5 C8 C5 112.9(4) . . ?
F6 C8 C5 112.4(4) . . ?
F4 C8 C5 112.6(4) . . ?
C14 C9 C10 115.6(4) . . ?
C14 C9 B1 120.8(4) . . ?
C10 C9 B1 123.5(4) . . ?
C11 C10 C9 122.1(4) . . ?
C11 C10 H10 119.0 . . ?
C9 C10 H10 119.0 . . ?
C12 C11 C10 121.0(4) . . ?
C12 C11 C15 118.7(4) . . ?
C10 C11 C15 120.2(4) . . ?
C13 C12 C11 118.0(4) . . ?
C13 C12 H12 121.0 . . ?
C11 C12 H12 121.0 . . ?
C12 C13 C14 120.9(4) . . ?
C12 C13 C16 119.2(4) . . ?
C14 C13 C16 119.9(4) . . ?
C13 C14 C9 122.3(4) . . ?
C13 C14 H14 118.8 . . ?
C9 C14 H14 118.8 . . ?
F7 C15 F8 107.2(4) . . ?
F7 C15 F9 105.7(4) . . ?
F8 C15 F9 105.3(4) . . ?
F7 C15 C11 113.5(4) . . ?
F8 C15 C11 111.3(4) . . ?
F9 C15 C11 113.3(4) . . ?
F11A C16 F10A 119.7(12) . . ?
F11B C16 F12B 105.1(6) . . ?
F11B C16 F10B 110.0(6) . . ?
F12B C16 F10B 101.7(5) . . ?
F11A C16 F12A 96.5(12) . . ?
F10A C16 F12A 95.2(11) . . ?
F11A C16 C13 119.4(9) . . ?
F10A C16 C13 112.9(8) . . ?
F11B C16 C13 115.5(4) . . ?
F12B C16 C13 112.1(5) . . ?
F10B C16 C13 111.4(5) . . ?
F12A C16 C13 106.8(7) . . ?
C22 C17 C18 115.4(4) . . ?
C22 C17 B1 121.9(4) . . ?
C18 C17 B1 122.0(4) . . ?
C19 C18 C17 122.3(4) . . ?
C19 C18 H18 118.9 . . ?
C17 C18 H18 118.9 . . ?
C18 C19 C20 121.0(4) . . ?
C18 C19 C23 120.6(4) . . ?
C20 C19 C23 118.4(4) . . ?
C21 C20 C19 117.6(4) . . ?
C21 C20 H20 121.2 . . ?
C19 C20 H20 121.2 . . ?
C20 C21 C22 121.1(4) . . ?
C20 C21 C24 119.4(4) . . ?
C22 C21 C24 119.4(4) . . ?
C21 C22 C17 122.5(4) . . ?
C21 C22 H22 118.7 . . ?
C17 C22 H22 118.7 . . ?
F14 C23 F13 106.6(4) . . ?
F14 C23 F15 107.0(4) . . ?
F13 C23 F15 104.3(4) . . ?
F14 C23 C19 112.3(4) . . ?
F13 C23 C19 113.6(4) . . ?
F15 C23 C19 112.3(4) . . ?
F16B C24 F17B 117.0(9) . . ?
F16A C24 F17A 104.7(11) . . ?
F16A C24 F18A 110.9(9) . . ?
F17A C24 F18A 95.1(9) . . ?
F16B C24 F18B 106.2(9) . . ?
F17B C24 F18B 96.0(7) . . ?
F16A C24 C21 118.7(8) . . ?
F16B C24 C21 115.6(8) . . ?
F17B C24 C21 111.7(5) . . ?
F17A C24 C21 113.6(8) . . ?
F18A C24 C21 111.2(5) . . ?
F18B C24 C21 107.8(5) . . ?
C26 C25 C30 115.3(4) . . ?
C26 C25 B1 121.7(4) . . ?
C30 C25 B1 122.8(4) . . ?
C27 C26 C25 123.0(4) . . ?
C27 C26 H26 118.5 . . ?
C25 C26 H26 118.5 . . ?
C28 C27 C26 120.4(4) . . ?
C28 C27 C31 120.7(4) . . ?
C26 C27 C31 118.9(4) . . ?
C29 C28 C27 118.7(4) . . ?
C29 C28 H28 120.6 . . ?
C27 C28 H28 120.6 . . ?
C28 C29 C30 120.6(4) . . ?
C28 C29 C32 119.8(4) . . ?
C30 C29 C32 119.5(4) . . ?
C29 C30 C25 122.0(4) . . ?
C29 C30 H30 119.0 . . ?
C25 C30 H30 119.0 . . ?
F21 C31 F20 108.3(4) . . ?
F21 C31 F19 106.9(4) . . ?
F20 C31 F19 104.8(4) . . ?
F21 C31 C27 112.5(4) . . ?
F20 C31 C27 112.4(4) . . ?
F19 C31 C27 111.5(4) . . ?
F24 C32 F23 109.1(5) . . ?
F24 C32 F22 104.1(5) . . ?
F23 C32 F22 102.8(5) . . ?
F24 C32 C29 114.7(5) . . ?
F23 C32 C29 113.9(4) . . ?
F22 C32 C29 111.0(4) . . ?
N1 C33 H33A 109.5 . . ?
N1 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
N1 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
N1 C34 C35 110.9(5) . . ?
N1 C34 H34A 109.5 . . ?
C35 C34 H34A 109.5 . . ?
N1 C34 H34B 109.5 . . ?
C35 C34 H34B 109.5 . . ?
H34A C34 H34B 108.1 . . ?
N2 C35 C34 113.3(5) . . ?
N2 C35 H35A 108.9 . . ?
C34 C35 H35A 108.9 . . ?
N2 C35 H35B 108.9 . . ?
C34 C35 H35B 108.9 . . ?
H35A C35 H35B 107.7 . . ?
N2 C36 H36A 109.5 . . ?
N2 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
N2 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
N2 C37 C38 112.9(5) . . ?
N2 C37 H37A 109.0 . . ?
C38 C37 H37A 109.0 . . ?
N2 C37 H37B 109.0 . . ?
C38 C37 H37B 109.0 . . ?
H37A C37 H37B 107.8 . . ?
N3 C38 C37 113.1(5) . . ?
N3 C38 H38A 109.0 . . ?
C37 C38 H38A 109.0 . . ?
N3 C38 H38B 109.0 . . ?
C37 C38 H38B 109.0 . . ?
H38A C38 H38B 107.8 . . ?
N3 C39 H39A 109.5 . . ?
N3 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
N3 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
N3 C40 C41 110.8(5) . . ?
N3 C40 H40A 109.5 . . ?
C41 C40 H40A 109.5 . . ?
N3 C40 H40B 109.5 . . ?
C41 C40 H40B 109.5 . . ?
H40A C40 H40B 108.1 . . ?
N4 C41 C40 111.5(5) . . ?
N4 C41 H41A 109.3 . . ?
C40 C41 H41A 109.3 . . ?
N4 C41 H41B 109.3 . . ?
C40 C41 H41B 109.3 . . ?
H41A C41 H41B 108.0 . . ?
N4 C42 H42A 109.5 . . ?
N4 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
N4 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
N4 C43 C44 109.9(5) . . ?
N4 C43 H43A 109.7 . . ?
C44 C43 H43A 109.7 . . ?
N4 C43 H43B 109.7 . . ?
C44 C43 H43B 109.7 . . ?
H43A C43 H43B 108.2 . . ?
N5 C44 C43 112.4(5) . . ?
N5 C44 H44A 109.1 . . ?
C43 C44 H44A 109.1 . . ?
N5 C44 H44B 109.1 . . ?
C43 C44 H44B 109.1 . . ?
H44A C44 H44B 107.9 . . ?
N5 C45 H45A 109.5 . . ?
N5 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
N5 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
N5 C46 C47 114.9(5) . . ?
N5 C46 H46A 108.5 . . ?
C47 C46 H46A 108.5 . . ?
N5 C46 H46B 108.5 . . ?
C47 C46 H46B 108.5 . . ?
H46A C46 H46B 107.5 . . ?
N6 C47 C46 113.6(5) . . ?
N6 C47 H47A 108.8 . . ?
C46 C47 H47A 108.8 . . ?
N6 C47 H47B 108.8 . . ?
C46 C47 H47B 108.8 . . ?
H47A C47 H47B 107.7 . . ?
N6 C48 H48A 109.5 . . ?
N6 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
N6 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
N6 C49 C50 112.0(5) . . ?
N6 C49 H49A 109.2 . . ?
C50 C49 H49A 109.2 . . ?
N6 C49 H49B 109.2 . . ?
C50 C49 H49B 109.2 . . ?
H49A C49 H49B 107.9 . . ?
N1 C50 C49 108.6(5) . . ?
N1 C50 H50A 110.0 . . ?
C49 C50 H50A 110.0 . . ?
N1 C50 H50B 110.0 . . ?
C49 C50 H50B 110.0 . . ?
H50A C50 H50B 108.4 . . ?
N1 Li1 N4 177.7(4) . . ?
N1 Li1 N2 77.3(3) . . ?
N4 Li1 N2 104.0(3) . . ?
N1 Li1 N5 103.4(4) . . ?
N4 Li1 N5 77.7(3) . . ?
N2 Li1 N5 117.4(4) . . ?
N1 Li1 N6 75.9(3) . . ?
N4 Li1 N6 102.6(3) . . ?
N2 Li1 N6 152.9(4) . . ?
N5 Li1 N6 73.5(3) . . ?
N1 Li1 N3 104.5(3) . . ?
N4 Li1 N3 74.3(3) . . ?
N2 Li1 N3 73.1(3) . . ?
N5 Li1 N3 151.8(4) . . ?
N6 Li1 N3 109.7(3) . . ?
C17 B1 C25 113.4(3) . . ?
C17 B1 C9 113.8(4) . . ?
C25 B1 C9 103.9(3) . . ?
C17 B1 C1 104.0(3) . . ?
C25 B1 C1 111.3(3) . . ?
C9 B1 C1 110.6(3) . . ?
C33 N1 C50 110.4(5) . . ?
C33 N1 C34 111.9(5) . . ?
C50 N1 C34 106.5(5) . . ?
C33 N1 Li1 118.8(4) . . ?
C50 N1 Li1 106.5(4) . . ?
C34 N1 Li1 101.8(4) . . ?
C37 N2 C35 111.6(5) . . ?
C37 N2 C36 107.5(5) . . ?
C35 N2 C36 109.8(4) . . ?
C37 N2 Li1 110.0(4) . . ?
C35 N2 Li1 107.0(4) . . ?
C36 N2 Li1 110.9(4) . . ?
C40 N3 C39 108.9(5) . . ?
C40 N3 C38 110.0(5) . . ?
C39 N3 C38 111.5(5) . . ?
C40 N3 Li1 104.9(4) . . ?
C39 N3 Li1 115.5(4) . . ?
C38 N3 Li1 105.8(4) . . ?
C42 N4 C41 111.5(5) . . ?
C42 N4 C43 108.6(5) . . ?
C41 N4 C43 107.9(4) . . ?
C42 N4 Li1 120.6(4) . . ?
C41 N4 Li1 106.3(4) . . ?
C43 N4 Li1 100.9(4) . . ?
C45 N5 C46 109.4(5) . . ?
C45 N5 C44 107.2(5) . . ?
C46 N5 C44 109.4(5) . . ?
C45 N5 Li1 117.4(4) . . ?
C46 N5 Li1 107.8(4) . . ?
C44 N5 Li1 105.5(4) . . ?
C48 N6 C47 110.9(5) . . ?
C48 N6 C49 108.5(5) . . ?
C47 N6 C49 110.5(5) . . ?
C48 N6 Li1 115.9(4) . . ?
C47 N6 Li1 107.3(4) . . ?
C49 N6 Li1 103.5(4) . . ?

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
C6 C1 C2 C3 -2.9(6) . . . . ?
B1 C1 C2 C3 -177.3(4) . . . . ?
C1 C2 C3 C4 3.1(6) . . . . ?
C1 C2 C3 C7 -177.7(4) . . . . ?
C2 C3 C4 C5 -0.9(6) . . . . ?
C7 C3 C4 C5 179.9(4) . . . . ?
C3 C4 C5 C6 -1.1(6) . . . . ?
C3 C4 C5 C8 -179.9(4) . . . . ?
C4 C5 C6 C1 1.1(6) . . . . ?
C8 C5 C6 C1 180.0(4) . . . . ?
C2 C1 C6 C5 0.9(6) . . . . ?
B1 C1 C6 C5 175.3(4) . . . . ?
C4 C3 C7 F1 99.8(5) . . . . ?
C2 C3 C7 F1 -79.4(5) . . . . ?
C4 C3 C7 F2 -138.9(5) . . . . ?
C2 C3 C7 F2 41.9(6) . . . . ?
C4 C3 C7 F3 -18.8(6) . . . . ?
C2 C3 C7 F3 162.0(4) . . . . ?
C4 C5 C8 F5 120.4(5) . . . . ?
C6 C5 C8 F5 -58.4(6) . . . . ?
C4 C5 C8 F6 -121.1(5) . . . . ?
C6 C5 C8 F6 60.0(6) . . . . ?
C4 C5 C8 F4 -0.5(7) . . . . ?
C6 C5 C8 F4 -179.3(4) . . . . ?
C14 C9 C10 C11 1.7(6) . . . . ?
B1 C9 C10 C11 177.7(4) . . . . ?
C9 C10 C11 C12 0.5(6) . . . . ?
C9 C10 C11 C15 -176.3(4) . . . . ?
C10 C11 C12 C13 -1.8(6) . . . . ?
C15 C11 C12 C13 175.0(4) . . . . ?
C11 C12 C13 C14 1.0(7) . . . . ?
C11 C12 C13 C16 179.8(5) . . . . ?
C12 C13 C14 C9 1.3(7) . . . . ?
C16 C13 C14 C9 -177.6(4) . . . . ?
C10 C9 C14 C13 -2.5(6) . . . . ?
B1 C9 C14 C13 -178.7(4) . . . . ?
C12 C11 C15 F7 159.2(4) . . . . ?
C10 C11 C15 F7 -24.0(6) . . . . ?
C12 C11 C15 F8 -79.8(5) . . . . ?
C10 C11 C15 F8 97.0(5) . . . . ?
C12 C11 C15 F9 38.6(6) . . . . ?
C10 C11 C15 F9 -144.5(4) . . . . ?
C12 C13 C16 F11A 24.8(14) . . . . ?
C14 C13 C16 F11A -156.4(12) . . . . ?
C12 C13 C16 F10A -124.1(11) . . . . ?
C14 C13 C16 F10A 54.7(12) . . . . ?
C12 C13 C16 F11B -176.4(7) . . . . ?
C14 C13 C16 F11B 2.5(9) . . . . ?
C12 C13 C16 F12B -56.1(7) . . . . ?
C14 C13 C16 F12B 122.8(5) . . . . ?
C12 C13 C16 F10B 57.2(7) . . . . ?
C14 C13 C16 F10B -124.0(6) . . . . ?
C12 C13 C16 F12A 132.6(8) . . . . ?
C14 C13 C16 F12A -48.6(9) . . . . ?
C22 C17 C18 C19 0.8(6) . . . . ?
B1 C17 C18 C19 171.6(4) . . . . ?
C17 C18 C19 C20 0.1(7) . . . . ?
C17 C18 C19 C23 177.8(4) . . . . ?
C18 C19 C20 C21 -0.4(7) . . . . ?
C23 C19 C20 C21 -178.1(5) . . . . ?
C19 C20 C21 C22 -0.3(7) . . . . ?
C19 C20 C21 C24 179.9(5) . . . . ?
C20 C21 C22 C17 1.3(7) . . . . ?
C24 C21 C22 C17 -178.9(5) . . . . ?
C18 C17 C22 C21 -1.5(6) . . . . ?
B1 C17 C22 C21 -172.3(4) . . . . ?
C18 C19 C23 F14 -95.1(6) . . . . ?
C20 C19 C23 F14 82.6(6) . . . . ?
C18 C19 C23 F13 26.0(7) . . . . ?
C20 C19 C23 F13 -156.3(4) . . . . ?
C18 C19 C23 F15 144.2(5) . . . . ?
C20 C19 C23 F15 -38.1(7) . . . . ?
C20 C21 C24 F16A 93.0(13) . . . . ?
C22 C21 C24 F16A -86.8(13) . . . . ?
C20 C21 C24 F16B -119.2(10) . . . . ?
C22 C21 C24 F16B 60.9(11) . . . . ?
C20 C21 C24 F17B 17.9(10) . . . . ?
C22 C21 C24 F17B -161.9(8) . . . . ?
C20 C21 C24 F17A -143.3(9) . . . . ?
C22 C21 C24 F17A 36.9(10) . . . . ?
C20 C21 C24 F18A -37.4(10) . . . . ?
C22 C21 C24 F18A 142.7(9) . . . . ?
C20 C21 C24 F18B 122.2(6) . . . . ?
C22 C21 C24 F18B -57.6(7) . . . . ?
C30 C25 C26 C27 0.2(6) . . . . ?
B1 C25 C26 C27 175.2(4) . . . . ?
C25 C26 C27 C28 1.9(7) . . . . ?
C25 C26 C27 C31 -177.7(4) . . . . ?
C26 C27 C28 C29 -2.6(7) . . . . ?
C31 C27 C28 C29 177.0(4) . . . . ?
C27 C28 C29 C30 1.2(7) . . . . ?
C27 C28 C29 C32 -177.7(4) . . . . ?
C28 C29 C30 C25 1.0(7) . . . . ?
C32 C29 C30 C25 179.9(4) . . . . ?
C26 C25 C30 C29 -1.6(6) . . . . ?
B1 C25 C30 C29 -176.6(4) . . . . ?
C28 C27 C31 F21 2.0(7) . . . . ?
C26 C27 C31 F21 -178.4(4) . . . . ?
C28 C27 C31 F20 124.6(5) . . . . ?
C26 C27 C31 F20 -55.8(6) . . . . ?
C28 C27 C31 F19 -118.1(5) . . . . ?
C26 C27 C31 F19 61.6(5) . . . . ?
C28 C29 C32 F24 -18.5(7) . . . . ?
C30 C29 C32 F24 162.6(5) . . . . ?
C28 C29 C32 F23 -145.3(5) . . . . ?
C30 C29 C32 F23 35.8(7) . . . . ?
C28 C29 C32 F22 99.2(6) . . . . ?
C30 C29 C32 F22 -79.8(6) . . . . ?
N1 C34 C35 N2 -55.8(7) . . . . ?
N2 C37 C38 N3 59.1(7) . . . . ?
N3 C40 C41 N4 63.8(7) . . . . ?
N4 C43 C44 N5 -60.0(7) . . . . ?
N5 C46 C47 N6 57.8(7) . . . . ?
N6 C49 C50 N1 64.3(7) . . . . ?
C22 C17 B1 C25 -34.0(6) . . . . ?
C18 C17 B1 C25 155.8(4) . . . . ?
C22 C17 B1 C9 -152.5(4) . . . . ?
C18 C17 B1 C9 37.3(6) . . . . ?
C22 C17 B1 C1 87.1(5) . . . . ?
C18 C17 B1 C1 -83.1(5) . . . . ?
C26 C25 B1 C17 152.3(4) . . . . ?
C30 C25 B1 C17 -33.0(5) . . . . ?
C26 C25 B1 C9 -83.6(5) . . . . ?
C30 C25 B1 C9 91.0(5) . . . . ?
C26 C25 B1 C1 35.5(5) . . . . ?
C30 C25 B1 C1 -149.9(4) . . . . ?
C14 C9 B1 C17 -154.8(4) . . . . ?
C10 C9 B1 C17 29.3(6) . . . . ?
C14 C9 B1 C25 81.4(5) . . . . ?
C10 C9 B1 C25 -94.5(5) . . . . ?
C14 C9 B1 C1 -38.2(5) . . . . ?
C10 C9 B1 C1 145.9(4) . . . . ?
C6 C1 B1 C17 -80.6(4) . . . . ?
C2 C1 B1 C17 93.5(4) . . . . ?
C6 C1 B1 C25 41.8(5) . . . . ?
C2 C1 B1 C25 -144.1(4) . . . . ?
C6 C1 B1 C9 156.9(4) . . . . ?
C2 C1 B1 C9 -29.0(5) . . . . ?
C49 C50 N1 C33 71.4(7) . . . . ?
C49 C50 N1 C34 -166.9(5) . . . . ?
C49 C50 N1 Li1 -58.8(6) . . . . ?
C35 C34 N1 C33 -69.5(7) . . . . ?
C35 C34 N1 C50 169.7(5) . . . . ?
C35 C34 N1 Li1 58.4(6) . . . . ?
C38 C37 N2 C35 70.3(6) . . . . ?
C38 C37 N2 C36 -169.2(5) . . . . ?
C38 C37 N2 Li1 -48.3(6) . . . . ?
C34 C35 N2 C37 -100.1(6) . . . . ?
C34 C35 N2 C36 140.8(6) . . . . ?
C34 C35 N2 Li1 20.3(6) . . . . ?
C41 C40 N3 C39 93.0(6) . . . . ?
C41 C40 N3 C38 -144.6(5) . . . . ?
C41 C40 N3 Li1 -31.2(6) . . . . ?
C37 C38 N3 C40 77.4(6) . . . . ?
C37 C38 N3 C39 -161.6(6) . . . . ?
C37 C38 N3 Li1 -35.3(6) . . . . ?
C40 C41 N4 C42 74.5(6) . . . . ?
C40 C41 N4 C43 -166.4(5) . . . . ?
C40 C41 N4 Li1 -58.8(6) . . . . ?
C44 C43 N4 C42 -66.4(6) . . . . ?
C44 C43 N4 C41 172.6(5) . . . . ?
C44 C43 N4 Li1 61.3(5) . . . . ?
C47 C46 N5 C45 -173.0(5) . . . . ?
C47 C46 N5 C44 69.9(6) . . . . ?
C47 C46 N5 Li1 -44.3(6) . . . . ?
C43 C44 N5 C45 147.9(6) . . . . ?
C43 C44 N5 C46 -93.6(6) . . . . ?
C43 C44 N5 Li1 22.1(6) . . . . ?
C46 C47 N6 C48 -163.5(5) . . . . ?
C46 C47 N6 C49 76.2(6) . . . . ?
C46 C47 N6 Li1 -36.0(6) . . . . ?
C50 C49 N6 C48 91.5(6) . . . . ?
C50 C49 N6 C47 -146.7(6) . . . . ?
C50 C49 N6 Li1 -32.2(6) . . . . ?

_refine_diff_density_max         1.037
_refine_diff_density_min         -0.403
_refine_diff_density_rms         0.074

_shelxl_version_number           2013-4

_exptl_crystal_recrystallization_method 'Layering: CH2Cl2/hexane'
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
####################################################################### 
# 
# 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_[K(Me~6~[18]aneN~6~)][BArF]
_database_code_depnum_ccdc_archive 'CCDC 1051100'
_audit_update_record             
;
2015-02-24 deposited with the CCDC.
2015-06-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H12 B F24, C18 H42 K N6'
_chemical_formula_sum            'C50 H54 B F24 K N6'
_chemical_formula_weight         1244.90

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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 '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'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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, -z'

_cell_length_a                   10.349(2)
_cell_length_b                   10.587(3)
_cell_length_c                   25.748(6)
_cell_angle_alpha                81.880(9)
_cell_angle_beta                 83.812(8)
_cell_angle_gamma                88.221(9)
_cell_volume                     2776.3(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5056
_cell_measurement_theta_min      2.4
_cell_measurement_theta_max      27.4

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_F_000             1272
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.217
_shelx_estimated_absorpt_T_min   0.985
_shelx_estimated_absorpt_T_max   0.989
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.791
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'CrystalClear-SM Expert 2.1 b29 (Rigaku, 2013)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_source_power             2.475
_diffrn_source_voltage           45.0
_diffrn_source_current           55.0
_diffrn_source                   'Rotating Anode'

_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_radiation_collimation    'Confocal mirrors, VHF Varimax '

_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_detector_area_resol_mean 28.5714

_diffrn_measurement_device       'four-circle κ diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC12 (Right)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_reflns_number            37145
_diffrn_reflns_av_unetI/netI     0.0505
_diffrn_reflns_av_R_equivalents  0.0467
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         2.927
_diffrn_reflns_theta_max         27.469
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             12627
_reflns_number_gt                9222
_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       
;
CrystalClear-SM Expert 2.1 b29 (Rigaku, 2013)
;
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.1 b29 (Rigaku, 2013)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.1 b29 (Rigaku, 2013)
;
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'ORTEP-III (Farrugia, 2012)'
_computing_publication_material  
'PLATON (Spek, 2003), WinGX (Farrugia, 1999) and enCIFer (Allen et al., 2004).'

_refine_special_details          
;
Two CF3 groups were refined to model the rotational disorder present. 
An isotropic thermal parameter of 0.01 or 0.005 was applied to the
disordered fluorines.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0580P)²+1.1850P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         12627
_refine_ls_number_parameters     776
_refine_ls_number_restraints     840
_refine_ls_R_factor_all          0.0736
_refine_ls_R_factor_gt           0.0495
_refine_ls_wR_factor_ref         0.1340
_refine_ls_wR_factor_gt          0.1205
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_restrained_S_all      1.043
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
C1 C 0.57664(19) 0.52997(17) 0.28314(7) 0.0197(4) Uani 1 1 d . U . . .
C2 C 0.5844(2) 0.46316(18) 0.33406(7) 0.0208(4) Uani 1 1 d . U . . .
H2 H 0.5161 0.4075 0.3493 0.025 Uiso 1 1 calc R U . . .
C3 C 0.6887(2) 0.47570(18) 0.36293(7) 0.0209(4) Uani 1 1 d . U . . .
C4 C 0.7913(2) 0.55537(18) 0.34207(8) 0.0213(4) Uani 1 1 d . U . . .
H4 H 0.8626 0.5637 0.3617 0.026 Uiso 1 1 calc R U . . .
C5 C 0.7871(2) 0.62303(18) 0.29145(8) 0.0214(4) Uani 1 1 d . U . . .
C6 C 0.68182(19) 0.61079(18) 0.26337(8) 0.0210(4) Uani 1 1 d . U . . .
H6 H 0.6806 0.6590 0.2294 0.025 Uiso 1 1 calc R U . . .
C7 C 0.6857(2) 0.40446(19) 0.41803(8) 0.0242(4) Uani 1 1 d . U . . .
C8 C 0.8960(2) 0.71101(19) 0.26889(8) 0.0256(4) Uani 1 1 d . U . . .
C9 C 0.43624(19) 0.63805(18) 0.20650(7) 0.0198(4) Uani 1 1 d . U . . .
C10 C 0.3423(2) 0.73161(18) 0.21801(8) 0.0228(4) Uani 1 1 d . U . . .
H10 H 0.2840 0.7155 0.2492 0.027 Uiso 1 1 calc R U . . .
C11 C 0.3315(2) 0.84789(18) 0.18502(8) 0.0251(4) Uani 1 1 d . U . . .
C12 C 0.4136(2) 0.87558(18) 0.13837(8) 0.0252(4) Uani 1 1 d . U . . .
H12 H 0.4059 0.9541 0.1159 0.030 Uiso 1 1 calc R U . . .
C13 C 0.5069(2) 0.78478(18) 0.12596(7) 0.0227(4) Uani 1 1 d . U . . .
C14 C 0.5179(2) 0.66893(18) 0.15943(7) 0.0218(4) Uani 1 1 d . U . . .
H14 H 0.5832 0.6090 0.1498 0.026 Uiso 1 1 calc R U . . .
C15 C 0.2307(2) 0.9457(2) 0.19957(10) 0.0391(6) Uani 1 1 d D U . . .
C16 C 0.6026(2) 0.8118(2) 0.07756(8) 0.0314(5) Uani 1 1 d . U . . .
C17 C 0.32294(19) 0.46719(17) 0.28560(7) 0.0194(4) Uani 1 1 d . U . . .
C18 C 0.28799(19) 0.52239(18) 0.33168(7) 0.0203(4) Uani 1 1 d . U . . .
H18 H 0.3428 0.5849 0.3404 0.024 Uiso 1 1 calc R U . . .
C19 C 0.17491(19) 0.48846(18) 0.36528(7) 0.0213(4) Uani 1 1 d . U . . .
C20 C 0.0911(2) 0.39947(18) 0.35353(8) 0.0217(4) Uani 1 1 d . U . . .
H20 H 0.0154 0.3751 0.3766 0.026 Uiso 1 1 calc R U . . .
C21 C 0.12086(19) 0.34666(18) 0.30695(8) 0.0210(4) Uani 1 1 d . U . . .
C22 C 0.23434(19) 0.37906(17) 0.27406(7) 0.0204(4) Uani 1 1 d . U . . .
H22 H 0.2526 0.3405 0.2429 0.025 Uiso 1 1 calc R U . . .
C23 C 0.1478(2) 0.5481(2) 0.41486(8) 0.0287(5) Uani 1 1 d . U . . .
C24 C 0.0257(2) 0.25534(19) 0.29297(8) 0.0260(4) Uani 1 1 d . U . . .
C25 C 0.50423(19) 0.38485(17) 0.21518(7) 0.0202(4) Uani 1 1 d . U . . .
C26 C 0.46822(19) 0.37535(18) 0.16490(7) 0.0207(4) Uani 1 1 d . U . . .
H26 H 0.4172 0.4420 0.1482 0.025 Uiso 1 1 calc R U . . .
C27 C 0.5052(2) 0.27055(18) 0.13845(8) 0.0222(4) Uani 1 1 d . U . . .
C28 C 0.5769(2) 0.16952(18) 0.16189(8) 0.0235(4) Uani 1 1 d . U . . .
H28 H 0.6010 0.0981 0.1442 0.028 Uiso 1 1 calc R U . . .
C29 C 0.6128(2) 0.17569(18) 0.21228(8) 0.0234(4) Uani 1 1 d . U . . .
C30 C 0.5777(2) 0.28102(18) 0.23784(8) 0.0226(4) Uani 1 1 d . U . . .
H30 H 0.6044 0.2830 0.2719 0.027 Uiso 1 1 calc R U . . .
C31 C 0.4658(2) 0.2710(2) 0.08422(8) 0.0267(4) Uani 1 1 d . U . . .
C32 C 0.6905(2) 0.06593(19) 0.23767(9) 0.0292(5) Uani 1 1 d . U . . .
C33 C -0.1378(2) 0.1675(2) 0.01126(9) 0.0308(5) Uani 1 1 d . U . . .
H33A H -0.2296 0.1841 0.0241 0.037 Uiso 1 1 calc R U . . .
H33B H -0.1205 0.0748 0.0196 0.037 Uiso 1 1 calc R U . . .
C34 C 0.0832(2) 0.2032(2) 0.02657(9) 0.0366(5) Uani 1 1 d . U . . .
H34A H 0.0980 0.1124 0.0385 0.055 Uiso 1 1 calc R U . . .
H34B H 0.1377 0.2543 0.0442 0.055 Uiso 1 1 calc R U . . .
H34C H 0.1056 0.2209 -0.0117 0.055 Uiso 1 1 calc R U . . .
C35 C -0.0908(2) 0.2064(2) 0.09672(8) 0.0317(5) Uani 1 1 d . U . . .
H35A H -0.0731 0.1147 0.1077 0.038 Uiso 1 1 calc R U . . .
H35B H -0.1855 0.2214 0.1038 0.038 Uiso 1 1 calc R U . . .
C36 C -0.0208(2) 0.2837(2) 0.13022(8) 0.0316(5) Uani 1 1 d . U . . .
H36A H -0.0604 0.2662 0.1672 0.038 Uiso 1 1 calc R U . . .
H36B H 0.0711 0.2545 0.1294 0.038 Uiso 1 1 calc R U . . .
C37 C -0.1577(2) 0.4729(2) 0.12049(10) 0.0401(6) Uani 1 1 d . U . . .
H37A H -0.1912 0.4545 0.1578 0.060 Uiso 1 1 calc R U . . .
H37B H -0.2125 0.4320 0.0992 0.060 Uiso 1 1 calc R U . . .
H37C H -0.1586 0.5654 0.1095 0.060 Uiso 1 1 calc R U . . .
C38 C 0.0619(3) 0.4867(2) 0.14282(8) 0.0341(5) Uani 1 1 d . U . . .
H38A H 0.1474 0.4421 0.1414 0.041 Uiso 1 1 calc R U . . .
H38B H 0.0250 0.4778 0.1803 0.041 Uiso 1 1 calc R U . . .
C39 C 0.0826(3) 0.6289(2) 0.12266(8) 0.0350(5) Uani 1 1 d . U . . .
H39A H 0.0013 0.6766 0.1315 0.042 Uiso 1 1 calc R U . . .
H39B H 0.1512 0.6604 0.1413 0.042 Uiso 1 1 calc R U . . .
C40 C 0.2472(2) 0.5994(2) 0.05111(10) 0.0405(6) Uani 1 1 d . U . . .
H40A H 0.3128 0.6349 0.0694 0.061 Uiso 1 1 calc R U . . .
H40B H 0.2698 0.6187 0.0129 0.061 Uiso 1 1 calc R U . . .
H40C H 0.2442 0.5067 0.0613 0.061 Uiso 1 1 calc R U . . .
C41 C 0.1190(2) 0.7950(2) 0.04869(9) 0.0318(5) Uani 1 1 d . U . . .
H41A H 0.1891 0.8331 0.0644 0.038 Uiso 1 1 calc R U . . .
H41B H 0.0352 0.8314 0.0626 0.038 Uiso 1 1 calc R U . . .
C42 C 0.8007(3) 0.0045(2) 0.43302(10) 0.0410(6) Uani 1 1 d . U . . .
H42A H 0.8866 -0.0132 0.4152 0.061 Uiso 1 1 calc R U . . .
H42B H 0.8093 0.0646 0.4581 0.061 Uiso 1 1 calc R U . . .
H42C H 0.7434 0.0417 0.4068 0.061 Uiso 1 1 calc R U . . .
C43 C 0.8276(2) -0.1710(2) 0.50235(9) 0.0310(5) Uani 1 1 d . U . . .
H43A H 0.9177 -0.1802 0.4858 0.037 Uiso 1 1 calc R U . . .
H43B H 0.7961 -0.2576 0.5168 0.037 Uiso 1 1 calc R U . . .
C44 C 0.7320(2) -0.2070(2) 0.42455(9) 0.0310(5) Uani 1 1 d . U . . .
H44A H 0.7064 -0.2903 0.4451 0.037 Uiso 1 1 calc R U . . .
H44B H 0.8177 -0.2191 0.4046 0.037 Uiso 1 1 calc R U . . .
C45 C 0.6326(2) -0.1663(2) 0.38553(8) 0.0319(5) Uani 1 1 d . U . . .
H45A H 0.6663 -0.0918 0.3607 0.038 Uiso 1 1 calc R U . . .
H45B H 0.6229 -0.2367 0.3647 0.038 Uiso 1 1 calc R U . . .
C46 C 0.4466(2) -0.2446(2) 0.44386(9) 0.0355(5) Uani 1 1 d . U . . .
H46A H 0.4375 -0.3127 0.4224 0.053 Uiso 1 1 calc R U . . .
H46B H 0.3608 -0.2213 0.4602 0.053 Uiso 1 1 calc R U . . .
H46C H 0.5030 -0.2745 0.4715 0.053 Uiso 1 1 calc R U . . .
C47 C 0.4199(2) -0.0832(2) 0.36919(8) 0.0325(5) Uani 1 1 d . U . . .
H47A H 0.4038 -0.1527 0.3488 0.039 Uiso 1 1 calc R U . . .
H47B H 0.4664 -0.0150 0.3446 0.039 Uiso 1 1 calc R U . . .
C48 C 0.2897(2) -0.0299(2) 0.39055(9) 0.0324(5) Uani 1 1 d . U . . .
H48A H 0.2454 0.0138 0.3606 0.039 Uiso 1 1 calc R U . . .
H48B H 0.2346 -0.1016 0.4081 0.039 Uiso 1 1 calc R U . . .
C49 C 0.1708(2) 0.0928(2) 0.45241(9) 0.0309(5) Uani 1 1 d . U . . .
H49A H 0.1236 0.0128 0.4657 0.037 Uiso 1 1 calc R U . . .
H49B H 0.1219 0.1414 0.4249 0.037 Uiso 1 1 calc R U . . .
C50 C 0.3693(2) 0.1755(2) 0.40227(9) 0.0342(5) Uani 1 1 d . U . . .
H50A H 0.3214 0.2168 0.3735 0.051 Uiso 1 1 calc R U . . .
H50B H 0.4569 0.1517 0.3880 0.051 Uiso 1 1 calc R U . . .
H50C H 0.3752 0.2346 0.4279 0.051 Uiso 1 1 calc R U . . .
B1 B 0.4582(2) 0.5061(2) 0.24742(8) 0.0197(4) Uani 1 1 d . U . . .
N1 N -0.05359(18) 0.23626(16) 0.03952(6) 0.0250(4) Uani 1 1 d . U . . .
N2 N -0.02453(18) 0.42337(16) 0.11307(7) 0.0269(4) Uani 1 1 d . U . . .
N3 N 0.11973(19) 0.65599(16) 0.06553(7) 0.0276(4) Uani 1 1 d . U . . .
N4 N 0.74535(18) -0.11481(16) 0.46148(7) 0.0275(4) Uani 1 1 d . U . . .
N5 N 0.50405(18) -0.13287(16) 0.41026(7) 0.0262(4) Uani 1 1 d . U . . .
N6 N 0.30071(18) 0.06053(16) 0.42831(7) 0.0266(4) Uani 1 1 d . U . . .
F1 F 0.64998(18) 0.28287(12) 0.42133(5) 0.0496(4) Uani 1 1 d . U . . .
F2 F 0.59970(17) 0.45577(14) 0.45192(5) 0.0533(4) Uani 1 1 d . U . . .
F3 F 0.79835(15) 0.40139(19) 0.43815(6) 0.0605(5) Uani 1 1 d . U . . .
F4 F 0.89911(17) 0.81229(15) 0.29442(6) 0.0552(5) Uani 1 1 d . U . . .
F5 F 1.01151(14) 0.65226(15) 0.26905(8) 0.0604(5) Uani 1 1 d . U . . .
F6 F 0.88773(14) 0.76128(14) 0.21845(5) 0.0424(3) Uani 1 1 d . U . . .
F7A F 0.2947(9) 1.0206(9) 0.2339(4) 0.071(3) Uani 0.223(5) 1 d . U P A 1
F8A F 0.1382(8) 0.9111(8) 0.2254(5) 0.050(2) Uani 0.223(5) 1 d . U P A 1
F9A F 0.2050(13) 1.0277(11) 0.1632(4) 0.076(3) Uani 0.223(5) 1 d . U P A 1
F7B F 0.1248(3) 0.9412(3) 0.17252(16) 0.0938(12) Uani 0.777(5) 1 d D U P A 2
F8B F 0.2698(3) 1.06254(18) 0.18813(16) 0.0746(12) Uani 0.777(5) 1 d D U P A 2
F9B F 0.1779(4) 0.9245(3) 0.24915(11) 0.0726(10) Uani 0.777(5) 1 d D U P A 2
F10 F 0.71959(18) 0.8435(2) 0.08966(6) 0.0702(6) Uani 1 1 d . U . . .
F11 F 0.5650(2) 0.90631(15) 0.04241(6) 0.0651(5) Uani 1 1 d . U . . .
F12 F 0.62589(16) 0.71085(13) 0.05208(5) 0.0444(4) Uani 1 1 d . U . . .
F13 F 0.23789(15) 0.51521(14) 0.44839(5) 0.0435(4) Uani 1 1 d . U . . .
F14 F 0.14714(17) 0.67600(13) 0.40540(6) 0.0496(4) Uani 1 1 d . U . . .
F15 F 0.03392(15) 0.51422(17) 0.44176(6) 0.0571(5) Uani 1 1 d . U . . .
F16 F 0.07341(14) 0.18966(14) 0.25470(7) 0.0489(4) Uani 1 1 d . U . . .
F17 F -0.07966(14) 0.31636(14) 0.27495(6) 0.0450(4) Uani 1 1 d . U . . .
F18 F -0.0186(2) 0.17184(17) 0.33412(6) 0.0727(6) Uani 1 1 d . U . . .
F19 F 0.51701(15) 0.17287(13) 0.06087(5) 0.0435(4) Uani 1 1 d . U . . .
F20 F 0.50111(16) 0.37788(13) 0.05173(5) 0.0436(4) Uani 1 1 d . U . . .
F21 F 0.33657(14) 0.26414(16) 0.08450(6) 0.0477(4) Uani 1 1 d . U . . .
F22 F 0.62403(15) -0.04391(12) 0.24641(6) 0.0427(4) Uani 1 1 d . U . . .
F23 F 0.80052(16) 0.04340(15) 0.20818(6) 0.0593(5) Uani 1 1 d . U . . .
F24 F 0.72459(16) 0.08431(12) 0.28486(6) 0.0440(4) Uani 1 1 d . U . . .
K1 K 0.0000 0.5000 0.0000 0.03072(16) Uani 1 2 d S U P . .
K2 K 0.5000 0.0000 0.5000 0.03549(17) Uani 1 2 d S U P . .


_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
C1 C2 1.408(3) . ?
C1 C6 1.411(3) . ?
C1 B1 1.655(3) . ?
C2 C3 1.395(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.390(3) . ?
C3 C7 1.507(3) . ?
C4 C5 1.400(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.390(3) . ?
C5 C8 1.499(3) . ?
C6 H6 0.9500 . ?
C7 F3 1.324(3) . ?
C7 F2 1.336(2) . ?
C7 F1 1.339(2) . ?
C8 F5 1.330(2) . ?
C8 F4 1.337(2) . ?
C8 F6 1.343(2) . ?
C9 C14 1.405(3) . ?
C9 C10 1.406(3) . ?
C9 B1 1.652(3) . ?
C10 C11 1.402(3) . ?
C10 H10 0.9500 . ?
C11 C12 1.395(3) . ?
C11 C15 1.503(3) . ?
C12 C13 1.386(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.405(3) . ?
C13 C16 1.506(3) . ?
C14 H14 0.9500 . ?
C15 F8A 1.144(8) . ?
C15 F9A 1.229(8) . ?
C15 F8B 1.297(3) . ?
C15 F9B 1.325(3) . ?
C15 F7B 1.367(4) . ?
C15 F7A 1.485(9) . ?
C16 F11 1.330(3) . ?
C16 F12 1.334(2) . ?
C16 F10 1.346(3) . ?
C17 C18 1.404(3) . ?
C17 C22 1.411(3) . ?
C17 B1 1.649(3) . ?
C18 C19 1.403(3) . ?
C18 H18 0.9500 . ?
C19 C20 1.385(3) . ?
C19 C23 1.498(3) . ?
C20 C21 1.395(3) . ?
C20 H20 0.9500 . ?
C21 C22 1.394(3) . ?
C21 C24 1.506(3) . ?
C22 H22 0.9500 . ?
C23 F15 1.333(3) . ?
C23 F14 1.342(3) . ?
C23 F13 1.343(3) . ?
C24 F16 1.329(2) . ?
C24 F18 1.330(2) . ?
C24 F17 1.342(2) . ?
C25 C26 1.403(3) . ?
C25 C30 1.411(3) . ?
C25 B1 1.656(3) . ?
C26 C27 1.404(3) . ?
C26 H26 0.9500 . ?
C27 C28 1.387(3) . ?
C27 C31 1.495(3) . ?
C28 C29 1.398(3) . ?
C28 H28 0.9500 . ?
C29 C30 1.393(3) . ?
C29 C32 1.505(3) . ?
C30 H30 0.9500 . ?
C31 F19 1.339(2) . ?
C31 F21 1.341(3) . ?
C31 F20 1.344(2) . ?
C32 F23 1.334(3) . ?
C32 F24 1.343(3) . ?
C32 F22 1.348(2) . ?
C33 N1 1.465(3) . ?
C33 C41 1.531(3) 2_565 ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 N1 1.462(3) . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 N1 1.473(3) . ?
C35 C36 1.520(3) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 N2 1.483(3) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C37 N2 1.462(3) . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 N2 1.472(3) . ?
C38 C39 1.535(3) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 N3 1.470(3) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C40 N3 1.465(3) . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 N3 1.474(3) . ?
C41 C33 1.531(3) 2_565 ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 N4 1.468(3) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 N4 1.474(3) . ?
C43 C49 1.523(3) 2_656 ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 N4 1.475(3) . ?
C44 C45 1.525(3) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C45 N5 1.467(3) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 N5 1.464(3) . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 N5 1.472(3) . ?
C47 C48 1.523(3) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 N6 1.472(3) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C49 N6 1.471(3) . ?
C49 C43 1.523(3) 2_656 ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C50 N6 1.468(3) . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?
N1 K1 2.8831(18) . ?
N2 K1 2.8957(18) . ?
N3 K1 2.9111(18) . ?
N4 K2 2.9180(19) . ?
N5 K2 2.8659(17) . ?
N6 K2 2.9115(18) . ?
K1 N1 2.8831(18) 2_565 ?
K1 N2 2.8958(18) 2_565 ?
K1 N3 2.9111(18) 2_565 ?
K1 C34 3.230(3) 2_565 ?
K1 C40 3.266(3) 2_565 ?
K1 C37 3.325(3) 2_565 ?
K2 N5 2.8659(17) 2_656 ?
K2 N6 2.9115(19) 2_656 ?
K2 N4 2.9180(19) 2_656 ?
K2 C46 3.228(2) 2_656 ?
K2 C50 3.297(2) 2_656 ?
K2 C42 3.390(3) 2_656 ?

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
C2 C1 C6 115.26(18) . . ?
C2 C1 B1 122.02(17) . . ?
C6 C1 B1 122.56(17) . . ?
C3 C2 C1 122.44(18) . . ?
C3 C2 H2 118.8 . . ?
C1 C2 H2 118.8 . . ?
C4 C3 C2 120.79(18) . . ?
C4 C3 C7 120.63(18) . . ?
C2 C3 C7 118.55(18) . . ?
C3 C4 C5 118.34(19) . . ?
C3 C4 H4 120.8 . . ?
C5 C4 H4 120.8 . . ?
C6 C5 C4 120.26(18) . . ?
C6 C5 C8 120.88(18) . . ?
C4 C5 C8 118.84(18) . . ?
C5 C6 C1 122.90(18) . . ?
C5 C6 H6 118.5 . . ?
C1 C6 H6 118.5 . . ?
F3 C7 F2 105.98(18) . . ?
F3 C7 F1 106.24(18) . . ?
F2 C7 F1 104.97(18) . . ?
F3 C7 C3 113.96(18) . . ?
F2 C7 C3 111.97(17) . . ?
F1 C7 C3 113.03(16) . . ?
F5 C8 F4 108.32(19) . . ?
F5 C8 F6 105.28(17) . . ?
F4 C8 F6 104.38(17) . . ?
F5 C8 C5 112.27(17) . . ?
F4 C8 C5 112.52(17) . . ?
F6 C8 C5 113.49(17) . . ?
C14 C9 C10 115.25(17) . . ?
C14 C9 B1 121.77(17) . . ?
C10 C9 B1 122.79(17) . . ?
C11 C10 C9 122.31(18) . . ?
C11 C10 H10 118.8 . . ?
C9 C10 H10 118.8 . . ?
C12 C11 C10 121.11(18) . . ?
C12 C11 C15 118.65(18) . . ?
C10 C11 C15 120.25(19) . . ?
C13 C12 C11 117.78(18) . . ?
C13 C12 H12 121.1 . . ?
C11 C12 H12 121.1 . . ?
C12 C13 C14 120.80(18) . . ?
C12 C13 C16 120.24(18) . . ?
C14 C13 C16 118.89(18) . . ?
C13 C14 C9 122.74(18) . . ?
C13 C14 H14 118.6 . . ?
C9 C14 H14 118.6 . . ?
F8A C15 F9A 110.9(8) . . ?
F8B C15 F9B 110.2(3) . . ?
F8B C15 F7B 104.9(3) . . ?
F9B C15 F7B 101.7(3) . . ?
F8A C15 F7A 103.1(7) . . ?
F9A C15 F7A 102.5(8) . . ?
F8A C15 C11 118.2(5) . . ?
F9A C15 C11 115.4(5) . . ?
F8B C15 C11 114.0(2) . . ?
F9B C15 C11 114.1(2) . . ?
F7B C15 C11 110.8(2) . . ?
F7A C15 C11 104.4(4) . . ?
F11 C16 F12 106.42(18) . . ?
F11 C16 F10 106.7(2) . . ?
F12 C16 F10 105.0(2) . . ?
F11 C16 C13 113.52(19) . . ?
F12 C16 C13 112.82(18) . . ?
F10 C16 C13 111.79(18) . . ?
C18 C17 C22 115.70(18) . . ?
C18 C17 B1 121.38(17) . . ?
C22 C17 B1 122.91(16) . . ?
C19 C18 C17 122.25(18) . . ?
C19 C18 H18 118.9 . . ?
C17 C18 H18 118.9 . . ?
C20 C19 C18 120.72(17) . . ?
C20 C19 C23 120.50(18) . . ?
C18 C19 C23 118.77(18) . . ?
C19 C20 C21 118.27(18) . . ?
C19 C20 H20 120.9 . . ?
C21 C20 H20 120.9 . . ?
C22 C21 C20 120.85(18) . . ?
C22 C21 C24 121.19(17) . . ?
C20 C21 C24 117.96(18) . . ?
C21 C22 C17 122.15(17) . . ?
C21 C22 H22 118.9 . . ?
C17 C22 H22 118.9 . . ?
F15 C23 F14 106.90(18) . . ?
F15 C23 F13 105.93(18) . . ?
F14 C23 F13 105.98(18) . . ?
F15 C23 C19 113.07(18) . . ?
F14 C23 C19 112.29(17) . . ?
F13 C23 C19 112.14(18) . . ?
F16 C24 F18 107.62(18) . . ?
F16 C24 F17 104.64(17) . . ?
F18 C24 F17 105.89(19) . . ?
F16 C24 C21 113.63(18) . . ?
F18 C24 C21 112.64(17) . . ?
F17 C24 C21 111.81(16) . . ?
C26 C25 C30 115.59(17) . . ?
C26 C25 B1 122.64(17) . . ?
C30 C25 B1 121.71(17) . . ?
C25 C26 C27 122.17(18) . . ?
C25 C26 H26 118.9 . . ?
C27 C26 H26 118.9 . . ?
C28 C27 C26 120.89(18) . . ?
C28 C27 C31 120.83(17) . . ?
C26 C27 C31 118.29(18) . . ?
C27 C28 C29 118.16(17) . . ?
C27 C28 H28 120.9 . . ?
C29 C28 H28 120.9 . . ?
C30 C29 C28 120.58(18) . . ?
C30 C29 C32 121.33(19) . . ?
C28 C29 C32 118.08(17) . . ?
C29 C30 C25 122.59(19) . . ?
C29 C30 H30 118.7 . . ?
C25 C30 H30 118.7 . . ?
F19 C31 F21 106.30(17) . . ?
F19 C31 F20 106.70(17) . . ?
F21 C31 F20 105.90(18) . . ?
F19 C31 C27 113.01(17) . . ?
F21 C31 C27 111.97(17) . . ?
F20 C31 C27 112.46(17) . . ?
F23 C32 F24 106.4(2) . . ?
F23 C32 F22 106.53(17) . . ?
F24 C32 F22 105.62(17) . . ?
F23 C32 C29 112.46(17) . . ?
F24 C32 C29 113.11(17) . . ?
F22 C32 C29 112.24(19) . . ?
N1 C33 C41 113.57(18) . 2_565 ?
N1 C33 H33A 108.9 . . ?
C41 C33 H33A 108.9 2_565 . ?
N1 C33 H33B 108.9 . . ?
C41 C33 H33B 108.9 2_565 . ?
H33A C33 H33B 107.7 . . ?
N1 C34 H34A 109.5 . . ?
N1 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
N1 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
N1 C35 C36 114.47(18) . . ?
N1 C35 H35A 108.6 . . ?
C36 C35 H35A 108.6 . . ?
N1 C35 H35B 108.6 . . ?
C36 C35 H35B 108.6 . . ?
H35A C35 H35B 107.6 . . ?
N2 C36 C35 114.20(18) . . ?
N2 C36 H36A 108.7 . . ?
C35 C36 H36A 108.7 . . ?
N2 C36 H36B 108.7 . . ?
C35 C36 H36B 108.7 . . ?
H36A C36 H36B 107.6 . . ?
N2 C37 H37A 109.5 . . ?
N2 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
N2 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
N2 C38 C39 114.34(18) . . ?
N2 C38 H38A 108.7 . . ?
C39 C38 H38A 108.7 . . ?
N2 C38 H38B 108.7 . . ?
C39 C38 H38B 108.7 . . ?
H38A C38 H38B 107.6 . . ?
N3 C39 C38 113.77(17) . . ?
N3 C39 H39A 108.8 . . ?
C38 C39 H39A 108.8 . . ?
N3 C39 H39B 108.8 . . ?
C38 C39 H39B 108.8 . . ?
H39A C39 H39B 107.7 . . ?
N3 C40 H40A 109.5 . . ?
N3 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
N3 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
N3 C41 C33 113.72(17) . 2_565 ?
N3 C41 H41A 108.8 . . ?
C33 C41 H41A 108.8 2_565 . ?
N3 C41 H41B 108.8 . . ?
C33 C41 H41B 108.8 2_565 . ?
H41A C41 H41B 107.7 . . ?
N4 C42 H42A 109.5 . . ?
N4 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
N4 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
N4 C43 C49 113.71(17) . 2_656 ?
N4 C43 H43A 108.8 . . ?
C49 C43 H43A 108.8 2_656 . ?
N4 C43 H43B 108.8 . . ?
C49 C43 H43B 108.8 2_656 . ?
H43A C43 H43B 107.7 . . ?
N4 C44 C45 113.77(17) . . ?
N4 C44 H44A 108.8 . . ?
C45 C44 H44A 108.8 . . ?
N4 C44 H44B 108.8 . . ?
C45 C44 H44B 108.8 . . ?
H44A C44 H44B 107.7 . . ?
N5 C45 C44 114.13(17) . . ?
N5 C45 H45A 108.7 . . ?
C44 C45 H45A 108.7 . . ?
N5 C45 H45B 108.7 . . ?
C44 C45 H45B 108.7 . . ?
H45A C45 H45B 107.6 . . ?
N5 C46 H46A 109.5 . . ?
N5 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
N5 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
N5 C47 C48 113.97(17) . . ?
N5 C47 H47A 108.8 . . ?
C48 C47 H47A 108.8 . . ?
N5 C47 H47B 108.8 . . ?
C48 C47 H47B 108.8 . . ?
H47A C47 H47B 107.7 . . ?
N6 C48 C47 113.67(19) . . ?
N6 C48 H48A 108.8 . . ?
C47 C48 H48A 108.8 . . ?
N6 C48 H48B 108.8 . . ?
C47 C48 H48B 108.8 . . ?
H48A C48 H48B 107.7 . . ?
N6 C49 C43 113.97(18) . 2_656 ?
N6 C49 H49A 108.8 . . ?
C43 C49 H49A 108.8 2_656 . ?
N6 C49 H49B 108.8 . . ?
C43 C49 H49B 108.8 2_656 . ?
H49A C49 H49B 107.7 . . ?
N6 C50 H50A 109.5 . . ?
N6 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
N6 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C17 B1 C9 110.65(16) . . ?
C17 B1 C1 110.81(15) . . ?
C9 B1 C1 108.37(15) . . ?
C17 B1 C25 108.30(15) . . ?
C9 B1 C25 111.53(15) . . ?
C1 B1 C25 107.13(16) . . ?
C34 N1 C33 111.05(17) . . ?
C34 N1 C35 110.49(18) . . ?
C33 N1 C35 109.38(17) . . ?
C34 N1 K1 89.88(13) . . ?
C33 N1 K1 118.18(12) . . ?
C35 N1 K1 116.22(12) . . ?
C37 N2 C38 110.94(18) . . ?
C37 N2 C36 110.32(18) . . ?
C38 N2 C36 109.58(17) . . ?
C37 N2 K1 93.62(13) . . ?
C38 N2 K1 116.16(13) . . ?
C36 N2 K1 115.18(12) . . ?
C40 N3 C39 110.98(19) . . ?
C40 N3 C41 110.97(19) . . ?
C39 N3 C41 109.83(16) . . ?
C40 N3 K1 90.32(13) . . ?
C39 N3 K1 116.39(13) . . ?
C41 N3 K1 116.81(12) . . ?
C42 N4 C43 110.71(19) . . ?
C42 N4 C44 110.42(18) . . ?
C43 N4 C44 109.58(16) . . ?
C42 N4 K2 95.51(13) . . ?
C43 N4 K2 115.66(12) . . ?
C44 N4 K2 114.17(13) . . ?
C46 N5 C45 110.08(17) . . ?
C46 N5 C47 110.91(18) . . ?
C45 N5 C47 109.65(16) . . ?
C46 N5 K2 90.42(12) . . ?
C45 N5 K2 116.48(13) . . ?
C47 N5 K2 117.63(12) . . ?
C50 N6 C49 111.14(17) . . ?
C50 N6 C48 110.65(18) . . ?
C49 N6 C48 109.86(17) . . ?
C50 N6 K2 91.61(13) . . ?
C49 N6 K2 116.28(13) . . ?
C48 N6 K2 115.97(13) . . ?
N1 K1 N1 180.0 2_565 . ?
N1 K1 N2 118.14(5) 2_565 . ?
N1 K1 N2 61.86(5) . . ?
N1 K1 N2 61.86(5) 2_565 2_565 ?
N1 K1 N2 118.14(5) . 2_565 ?
N2 K1 N2 180.0 . 2_565 ?
N1 K1 N3 60.67(5) 2_565 . ?
N1 K1 N3 119.33(5) . . ?
N2 K1 N3 61.35(5) . . ?
N2 K1 N3 118.65(5) 2_565 . ?
N1 K1 N3 119.33(5) 2_565 2_565 ?
N1 K1 N3 60.67(5) . 2_565 ?
N2 K1 N3 118.65(5) . 2_565 ?
N2 K1 N3 61.35(5) 2_565 2_565 ?
N3 K1 N3 180.0 . 2_565 ?
N1 K1 C34 26.92(6) 2_565 2_565 ?
N1 K1 C34 153.08(6) . 2_565 ?
N2 K1 C34 110.05(5) . 2_565 ?
N2 K1 C34 69.95(5) 2_565 2_565 ?
N3 K1 C34 68.90(6) . 2_565 ?
N3 K1 C34 111.10(6) 2_565 2_565 ?
N1 K1 C40 111.32(6) 2_565 2_565 ?
N1 K1 C40 68.68(6) . 2_565 ?
N2 K1 C40 110.45(6) . 2_565 ?
N2 K1 C40 69.55(6) 2_565 2_565 ?
N3 K1 C40 153.36(6) . 2_565 ?
N3 K1 C40 26.64(6) 2_565 2_565 ?
C34 K1 C40 93.24(6) 2_565 2_565 ?
N1 K1 C37 69.35(6) 2_565 2_565 ?
N1 K1 C37 110.65(6) . 2_565 ?
N2 K1 C37 153.97(6) . 2_565 ?
N2 K1 C37 26.02(6) 2_565 2_565 ?
N3 K1 C37 110.67(6) . 2_565 ?
N3 K1 C37 69.33(6) 2_565 2_565 ?
C34 K1 C37 87.15(6) 2_565 2_565 ?
C40 K1 C37 87.03(7) 2_565 2_565 ?
N5 K2 N5 180.0 2_656 . ?
N5 K2 N6 61.11(5) 2_656 2_656 ?
N5 K2 N6 118.89(5) . 2_656 ?
N5 K2 N6 118.89(5) 2_656 . ?
N5 K2 N6 61.11(5) . . ?
N6 K2 N6 180.0 2_656 . ?
N5 K2 N4 61.79(5) 2_656 2_656 ?
N5 K2 N4 118.21(5) . 2_656 ?
N6 K2 N4 118.97(5) 2_656 2_656 ?
N6 K2 N4 61.03(5) . 2_656 ?
N5 K2 N4 118.21(5) 2_656 . ?
N5 K2 N4 61.79(5) . . ?
N6 K2 N4 61.04(5) 2_656 . ?
N6 K2 N4 118.96(5) . . ?
N4 K2 N4 180.0 2_656 . ?
N5 K2 C46 26.98(5) 2_656 2_656 ?
N5 K2 C46 153.02(5) . 2_656 ?
N6 K2 C46 69.58(6) 2_656 2_656 ?
N6 K2 C46 110.42(6) . 2_656 ?
N4 K2 C46 69.69(6) 2_656 2_656 ?
N4 K2 C46 110.31(6) . 2_656 ?
N5 K2 C50 68.75(6) 2_656 2_656 ?
N5 K2 C50 111.25(6) . 2_656 ?
N6 K2 C50 26.42(5) 2_656 2_656 ?
N6 K2 C50 153.58(5) . 2_656 ?
N4 K2 C50 110.52(6) 2_656 2_656 ?
N4 K2 C50 69.48(6) . 2_656 ?
C46 K2 C50 87.02(6) 2_656 2_656 ?
N5 K2 C42 69.16(6) 2_656 2_656 ?
N5 K2 C42 110.84(6) . 2_656 ?
N6 K2 C42 111.09(6) 2_656 2_656 ?
N6 K2 C42 68.91(6) . 2_656 ?
N4 K2 C42 25.53(5) 2_656 2_656 ?
N4 K2 C42 154.47(5) . 2_656 ?
C46 K2 C42 86.67(6) 2_656 2_656 ?
C50 K2 C42 93.43(6) 2_656 2_656 ?

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
C6 C1 C2 C3 -0.1(3) . . . . ?
B1 C1 C2 C3 175.23(17) . . . . ?
C1 C2 C3 C4 -0.4(3) . . . . ?
C1 C2 C3 C7 177.48(17) . . . . ?
C2 C3 C4 C5 0.2(3) . . . . ?
C7 C3 C4 C5 -177.65(17) . . . . ?
C3 C4 C5 C6 0.5(3) . . . . ?
C3 C4 C5 C8 178.95(17) . . . . ?
C4 C5 C6 C1 -1.1(3) . . . . ?
C8 C5 C6 C1 -179.52(17) . . . . ?
C2 C1 C6 C5 0.9(3) . . . . ?
B1 C1 C6 C5 -174.42(17) . . . . ?
C4 C3 C7 F3 -14.9(3) . . . . ?
C2 C3 C7 F3 167.17(18) . . . . ?
C4 C3 C7 F2 105.4(2) . . . . ?
C2 C3 C7 F2 -72.6(2) . . . . ?
C4 C3 C7 F1 -136.3(2) . . . . ?
C2 C3 C7 F1 45.7(3) . . . . ?
C6 C5 C8 F5 -126.8(2) . . . . ?
C4 C5 C8 F5 54.8(2) . . . . ?
C6 C5 C8 F4 110.7(2) . . . . ?
C4 C5 C8 F4 -67.7(2) . . . . ?
C6 C5 C8 F6 -7.5(3) . . . . ?
C4 C5 C8 F6 174.06(17) . . . . ?
C14 C9 C10 C11 -0.5(3) . . . . ?
B1 C9 C10 C11 174.64(19) . . . . ?
C9 C10 C11 C12 0.8(3) . . . . ?
C9 C10 C11 C15 -179.0(2) . . . . ?
C10 C11 C12 C13 -0.5(3) . . . . ?
C15 C11 C12 C13 179.3(2) . . . . ?
C11 C12 C13 C14 0.0(3) . . . . ?
C11 C12 C13 C16 -176.96(19) . . . . ?
C12 C13 C14 C9 0.3(3) . . . . ?
C16 C13 C14 C9 177.32(19) . . . . ?
C10 C9 C14 C13 -0.1(3) . . . . ?
B1 C9 C14 C13 -175.26(18) . . . . ?
C12 C11 C15 F8A 153.2(8) . . . . ?
C10 C11 C15 F8A -27.0(8) . . . . ?
C12 C11 C15 F9A 18.6(9) . . . . ?
C10 C11 C15 F9A -161.6(9) . . . . ?
C12 C11 C15 F8B -37.7(4) . . . . ?
C10 C11 C15 F8B 142.1(3) . . . . ?
C12 C11 C15 F9B -165.6(3) . . . . ?
C10 C11 C15 F9B 14.2(4) . . . . ?
C12 C11 C15 F7B 80.4(3) . . . . ?
C10 C11 C15 F7B -99.8(3) . . . . ?
C12 C11 C15 F7A -93.1(5) . . . . ?
C10 C11 C15 F7A 86.7(5) . . . . ?
C12 C13 C16 F11 -19.0(3) . . . . ?
C14 C13 C16 F11 164.0(2) . . . . ?
C12 C13 C16 F12 -140.2(2) . . . . ?
C14 C13 C16 F12 42.8(3) . . . . ?
C12 C13 C16 F10 101.8(2) . . . . ?
C14 C13 C16 F10 -75.2(3) . . . . ?
C22 C17 C18 C19 2.5(3) . . . . ?
B1 C17 C18 C19 -178.53(17) . . . . ?
C17 C18 C19 C20 -1.2(3) . . . . ?
C17 C18 C19 C23 177.46(18) . . . . ?
C18 C19 C20 C21 -1.3(3) . . . . ?
C23 C19 C20 C21 -179.90(18) . . . . ?
C19 C20 C21 C22 2.3(3) . . . . ?
C19 C20 C21 C24 -176.77(17) . . . . ?
C20 C21 C22 C17 -1.0(3) . . . . ?
C24 C21 C22 C17 178.11(17) . . . . ?
C18 C17 C22 C21 -1.4(3) . . . . ?
B1 C17 C22 C21 179.59(17) . . . . ?
C20 C19 C23 F15 -5.2(3) . . . . ?
C18 C19 C23 F15 176.15(19) . . . . ?
C20 C19 C23 F14 -126.3(2) . . . . ?
C18 C19 C23 F14 55.1(3) . . . . ?
C20 C19 C23 F13 114.5(2) . . . . ?
C18 C19 C23 F13 -64.1(2) . . . . ?
C22 C21 C24 F16 14.4(3) . . . . ?
C20 C21 C24 F16 -166.49(18) . . . . ?
C22 C21 C24 F18 137.1(2) . . . . ?
C20 C21 C24 F18 -43.8(3) . . . . ?
C22 C21 C24 F17 -103.8(2) . . . . ?
C20 C21 C24 F17 75.3(2) . . . . ?
C30 C25 C26 C27 -1.2(3) . . . . ?
B1 C25 C26 C27 -178.42(18) . . . . ?
C25 C26 C27 C28 1.6(3) . . . . ?
C25 C26 C27 C31 -178.02(18) . . . . ?
C26 C27 C28 C29 -0.8(3) . . . . ?
C31 C27 C28 C29 178.88(19) . . . . ?
C27 C28 C29 C30 -0.4(3) . . . . ?
C27 C28 C29 C32 179.94(18) . . . . ?
C28 C29 C30 C25 0.8(3) . . . . ?
C32 C29 C30 C25 -179.57(19) . . . . ?
C26 C25 C30 C29 0.0(3) . . . . ?
B1 C25 C30 C29 177.26(19) . . . . ?
C28 C27 C31 F19 -5.9(3) . . . . ?
C26 C27 C31 F19 173.79(18) . . . . ?
C28 C27 C31 F21 114.1(2) . . . . ?
C26 C27 C31 F21 -66.2(2) . . . . ?
C28 C27 C31 F20 -126.8(2) . . . . ?
C26 C27 C31 F20 52.9(3) . . . . ?
C30 C29 C32 F23 -123.0(2) . . . . ?
C28 C29 C32 F23 56.6(3) . . . . ?
C30 C29 C32 F24 -2.5(3) . . . . ?
C28 C29 C32 F24 177.15(18) . . . . ?
C30 C29 C32 F22 116.9(2) . . . . ?
C28 C29 C32 F22 -63.5(2) . . . . ?
N1 C35 C36 N2 50.6(3) . . . . ?
N2 C38 C39 N3 -50.3(3) . . . . ?
N4 C44 C45 N5 -52.8(3) . . . . ?
N5 C47 C48 N6 49.5(3) . . . . ?
C18 C17 B1 C9 -83.4(2) . . . . ?
C22 C17 B1 C9 95.5(2) . . . . ?
C18 C17 B1 C1 36.9(2) . . . . ?
C22 C17 B1 C1 -144.22(17) . . . . ?
C18 C17 B1 C25 154.09(17) . . . . ?
C22 C17 B1 C25 -27.0(2) . . . . ?
C14 C9 B1 C17 -158.47(17) . . . . ?
C10 C9 B1 C17 26.7(3) . . . . ?
C14 C9 B1 C1 79.8(2) . . . . ?
C10 C9 B1 C1 -95.0(2) . . . . ?
C14 C9 B1 C25 -37.8(3) . . . . ?
C10 C9 B1 C25 147.36(18) . . . . ?
C2 C1 B1 C17 31.4(2) . . . . ?
C6 C1 B1 C17 -153.58(17) . . . . ?
C2 C1 B1 C9 153.00(17) . . . . ?
C6 C1 B1 C9 -32.0(2) . . . . ?
C2 C1 B1 C25 -86.5(2) . . . . ?
C6 C1 B1 C25 88.5(2) . . . . ?
C26 C25 B1 C17 92.8(2) . . . . ?
C30 C25 B1 C17 -84.2(2) . . . . ?
C26 C25 B1 C9 -29.2(3) . . . . ?
C30 C25 B1 C9 153.81(18) . . . . ?
C26 C25 B1 C1 -147.60(18) . . . . ?
C30 C25 B1 C1 35.4(2) . . . . ?
C41 C33 N1 C34 -65.2(2) 2_565 . . . ?
C41 C33 N1 C35 172.59(19) 2_565 . . . ?
C41 C33 N1 K1 36.6(2) 2_565 . . . ?
C36 C35 N1 C34 64.1(2) . . . . ?
C36 C35 N1 C33 -173.34(19) . . . . ?
C36 C35 N1 K1 -36.3(2) . . . . ?
C39 C38 N2 C37 -67.0(2) . . . . ?
C39 C38 N2 C36 170.99(19) . . . . ?
C39 C38 N2 K1 38.3(2) . . . . ?
C35 C36 N2 C37 66.0(2) . . . . ?
C35 C36 N2 C38 -171.53(19) . . . . ?
C35 C36 N2 K1 -38.3(2) . . . . ?
C38 C39 N3 C40 -65.0(3) . . . . ?
C38 C39 N3 C41 171.9(2) . . . . ?
C38 C39 N3 K1 36.3(2) . . . . ?
C33 C41 N3 C40 65.0(3) 2_565 . . . ?
C33 C41 N3 C39 -171.9(2) 2_565 . . . ?
C33 C41 N3 K1 -36.5(2) 2_565 . . . ?
C49 C43 N4 C42 67.6(2) 2_656 . . . ?
C49 C43 N4 C44 -170.34(19) 2_656 . . . ?
C49 C43 N4 K2 -39.6(2) 2_656 . . . ?
C45 C44 N4 C42 -66.4(2) . . . . ?
C45 C44 N4 C43 171.37(19) . . . . ?
C45 C44 N4 K2 39.8(2) . . . . ?
C44 C45 N5 C46 -63.3(2) . . . . ?
C44 C45 N5 C47 174.46(18) . . . . ?
C44 C45 N5 K2 37.7(2) . . . . ?
C48 C47 N5 C46 65.5(2) . . . . ?
C48 C47 N5 C45 -172.67(19) . . . . ?
C48 C47 N5 K2 -36.5(2) . . . . ?
C43 C49 N6 C50 -65.3(2) 2_656 . . . ?
C43 C49 N6 C48 171.86(18) 2_656 . . . ?
C43 C49 N6 K2 37.6(2) 2_656 . . . ?
C47 C48 N6 C50 64.9(2) . . . . ?
C47 C48 N6 C49 -172.00(18) . . . . ?
C47 C48 N6 K2 -37.6(2) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C34 H34B F21 0.98 2.41 3.277(3) 146.6 .
C45 H45A F24 0.99 2.54 3.514(3) 168.8 .
C48 H48B F14 0.99 2.56 3.442(3) 148.2 1_545

_refine_diff_density_max         0.725
_refine_diff_density_min         -0.416
_refine_diff_density_rms         0.056

_shelxl_version_number           2013-4

_exptl_crystal_recrystallization_method 'Layering: CH2Cl2/hexane'
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
####################################################################### 
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# This file contains crystal structure data downloaded from the 
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# 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_[Rb(Me~6~[18]aneN~6~)][BArF]
_database_code_depnum_ccdc_archive 'CCDC 1051101'
_audit_update_record             
;
2015-02-24 deposited with the CCDC.
2015-06-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C50 H54 B F24 N6 Rb'
_chemical_formula_sum            'C50 H54 B F24 N6 Rb'
_chemical_formula_weight         1291.27

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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 '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'
Rb Rb -0.9393 2.9676 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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, -z'

_cell_length_a                   10.3279(10)
_cell_length_b                   10.5938(10)
_cell_length_c                   25.779(2)
_cell_angle_alpha                81.581(3)
_cell_angle_beta                 83.317(3)
_cell_angle_gamma                88.067(3)
_cell_volume                     2770.8(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9092
_cell_measurement_theta_min      2.4
_cell_measurement_theta_max      27.5

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.548
_exptl_crystal_F_000             1308
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    1.016
_shelx_estimated_absorpt_T_min   0.932
_shelx_estimated_absorpt_T_max   0.942
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.785
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'CrystalClear-SM Expert 2.1 b29 (Rigaku, 2013)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_source_power             2.475
_diffrn_source_voltage           45.0
_diffrn_source_current           55.0
_diffrn_source                   'Rotating Anode'

_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_radiation_collimation    'Confocal mirrors, VHF Varimax '

_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_detector_area_resol_mean 28.5714

_diffrn_measurement_device       'four-circle κ diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC12 (Right)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_reflns_number            36473
_diffrn_reflns_av_unetI/netI     0.0456
_diffrn_reflns_av_R_equivalents  0.0420
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         2.931
_diffrn_reflns_theta_max         27.482
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             12647
_reflns_number_gt                9533
_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       
;
CrystalClear-SM Expert 2.1 b29 (Rigaku, 2013)
;
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.1 b29 (Rigaku, 2013)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.1 b29 (Rigaku, 2013)
;
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'ORTEP-III (Farrugia, 2012)'
_computing_publication_material  
'PLATON (Spek, 2003), WinGX (Farrugia, 1999) and enCIFer (Allen et al., 2004).'

_refine_special_details          
;
One CF3 group was refined to account for rotational disorder with 
an isotropic thermal parameter restraint of 0.05 applied to some 
of the disordered fluorines. Three of the disordered fluorines were
restrained to have identical displacement parameters.  
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0665P)²+1.6619P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         12647
_refine_ls_number_parameters     770
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0717
_refine_ls_R_factor_gt           0.0517
_refine_ls_wR_factor_ref         0.1434
_refine_ls_wR_factor_gt          0.1323
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_restrained_S_all      1.128
_refine_ls_shift/su_max          0.001
_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
C1 C 0.0006(2) 0.6139(2) 0.28572(9) 0.0209(4) Uani 1 1 d . . . . .
C2 C 0.0355(2) 0.6232(2) 0.33586(9) 0.0216(4) Uani 1 1 d . . . . .
H2 H 0.0859 0.5562 0.3528 0.026 Uiso 1 1 calc R U . . .
C3 C -0.0015(2) 0.7280(2) 0.36189(9) 0.0226(5) Uani 1 1 d . . . . .
C4 C -0.0721(2) 0.8293(2) 0.33821(9) 0.0256(5) Uani 1 1 d . . . . .
H4 H -0.0962 0.9010 0.3557 0.031 Uiso 1 1 calc R U . . .
C5 C -0.1067(2) 0.8233(2) 0.28813(9) 0.0240(5) Uani 1 1 d . . . . .
C6 C -0.0721(2) 0.7183(2) 0.26282(9) 0.0234(5) Uani 1 1 d . . . . .
H6 H -0.0983 0.7166 0.2288 0.028 Uiso 1 1 calc R U . . .
C7 C 0.0367(2) 0.7277(2) 0.41610(10) 0.0281(5) Uani 1 1 d . . . . .
C8 C -0.1836(3) 0.9335(2) 0.26241(10) 0.0319(5) Uani 1 1 d . . . . .
C9 C -0.0718(2) 0.4699(2) 0.21805(8) 0.0199(4) Uani 1 1 d . . . . .
C10 C -0.1768(2) 0.3888(2) 0.23798(9) 0.0214(4) Uani 1 1 d . . . . .
H10 H -0.1759 0.3400 0.2719 0.026 Uiso 1 1 calc R U . . .
C11 C -0.2817(2) 0.3775(2) 0.20968(9) 0.0208(4) Uani 1 1 d . . . . .
C12 C -0.2855(2) 0.4450(2) 0.15929(9) 0.0220(4) Uani 1 1 d . . . . .
H12 H -0.3565 0.4369 0.1397 0.026 Uiso 1 1 calc R U . . .
C13 C -0.1827(2) 0.5245(2) 0.13854(9) 0.0217(4) Uani 1 1 d . . . . .
C14 C -0.0790(2) 0.5363(2) 0.16741(9) 0.0214(4) Uani 1 1 d . . . . .
H14 H -0.0102 0.5919 0.1521 0.026 Uiso 1 1 calc R U . . .
C15 C -0.3909(2) 0.2892(2) 0.23237(9) 0.0254(5) Uani 1 1 d . . . . .
C16 C -0.1793(2) 0.5962(2) 0.08396(9) 0.0262(5) Uani 1 1 d . . . . .
C17 C 0.0673(2) 0.3617(2) 0.29459(9) 0.0206(4) Uani 1 1 d . . . . .
C18 C 0.1614(2) 0.2679(2) 0.28370(9) 0.0239(5) Uani 1 1 d . . . . .
H18 H 0.2213 0.2841 0.2527 0.029 Uiso 1 1 calc R U . . .
C19 C 0.1704(2) 0.1520(2) 0.31653(10) 0.0276(5) Uani 1 1 d . . . . .
C20 C 0.0865(2) 0.1248(2) 0.36284(10) 0.0273(5) Uani 1 1 d . . . . .
H20 H 0.0934 0.0463 0.3856 0.033 Uiso 1 1 calc R U . . .
C21 C -0.0075(2) 0.2157(2) 0.37473(9) 0.0255(5) Uani 1 1 d . . . . .
C22 C -0.0169(2) 0.3310(2) 0.34138(9) 0.0227(5) Uani 1 1 d . . . . .
H22 H -0.0827 0.3912 0.3506 0.027 Uiso 1 1 calc R U . . .
C23 C 0.2713(3) 0.0551(3) 0.30250(13) 0.0414(7) Uani 1 1 d . . . . .
C24 C -0.1050(3) 0.1886(3) 0.42264(10) 0.0343(6) Uani 1 1 d . . . . .
C25 C 0.1821(2) 0.5312(2) 0.21524(8) 0.0198(4) Uani 1 1 d . . . . .
C26 C 0.2701(2) 0.6196(2) 0.22635(9) 0.0206(4) Uani 1 1 d . . . . .
H26 H 0.2512 0.6581 0.2575 0.025 Uiso 1 1 calc R U . . .
C27 C 0.3840(2) 0.6523(2) 0.19321(9) 0.0212(4) Uani 1 1 d . . . . .
C28 C 0.4144(2) 0.5991(2) 0.14704(9) 0.0226(5) Uani 1 1 d . . . . .
H28 H 0.4904 0.6236 0.1237 0.027 Uiso 1 1 calc R U . . .
C29 C 0.3311(2) 0.5094(2) 0.13581(9) 0.0223(4) Uani 1 1 d . . . . .
C30 C 0.2182(2) 0.4757(2) 0.16951(9) 0.0217(4) Uani 1 1 d . . . . .
H30 H 0.1637 0.4129 0.1611 0.026 Uiso 1 1 calc R U . . .
C31 C 0.4782(2) 0.7444(2) 0.20659(10) 0.0274(5) Uani 1 1 d . . . . .
C32 C 0.3597(2) 0.4488(3) 0.08662(10) 0.0286(5) Uani 1 1 d . . . . .
C33 C -0.3272(2) 1.1749(3) -0.00102(10) 0.0315(5) Uani 1 1 d . . . . .
H33A H -0.2926 1.2602 -0.0159 0.038 Uiso 1 1 calc R U . . .
H33B H -0.4174 1.1871 0.0154 0.038 Uiso 1 1 calc R U . . .
C34 C -0.3089(4) 1.0016(3) 0.06960(13) 0.0518(8) Uani 1 1 d . . . . .
H34A H -0.3938 1.0239 0.0875 0.078 Uiso 1 1 calc R U . . .
H34B H -0.2528 0.9623 0.0959 0.078 Uiso 1 1 calc R U . . .
H34C H -0.3211 0.9412 0.0452 0.078 Uiso 1 1 calc R U . . .
C35 C -0.2299(2) 1.2085(3) 0.07612(10) 0.0314(5) Uani 1 1 d . . . . .
H35A H -0.3149 1.2233 0.0965 0.038 Uiso 1 1 calc R U . . .
H35B H -0.2024 1.2908 0.0549 0.038 Uiso 1 1 calc R U . . .
C36 C -0.1301(2) 1.1669(3) 0.11485(10) 0.0319(5) Uani 1 1 d . . . . .
H36A H -0.1219 1.2361 0.1362 0.038 Uiso 1 1 calc R U . . .
H36B H -0.1633 1.0910 0.1393 0.038 Uiso 1 1 calc R U . . .
C37 C 0.0574(3) 1.2495(3) 0.05830(14) 0.0513(8) Uani 1 1 d . . . . .
H37A H 0.0654 1.3147 0.0810 0.077 Uiso 1 1 calc R U . . .
H37B H 0.0014 1.2823 0.0310 0.077 Uiso 1 1 calc R U . . .
H37C H 0.1439 1.2281 0.0416 0.077 Uiso 1 1 calc R U . . .
C38 C 0.0839(3) 1.0832(3) 0.12999(10) 0.0320(5) Uani 1 1 d . . . . .
H38A H 0.0367 1.0145 0.1543 0.038 Uiso 1 1 calc R U . . .
H38B H 0.1009 1.1511 0.1508 0.038 Uiso 1 1 calc R U . . .
C39 C 0.2146(3) 1.0291(3) 0.10786(10) 0.0331(6) Uani 1 1 d . . . . .
H39A H 0.2688 1.1004 0.0889 0.040 Uiso 1 1 calc R U . . .
H39B H 0.2607 0.9876 0.1376 0.040 Uiso 1 1 calc R U . . .
C40 C 0.3314(2) 0.9035(3) 0.04606(10) 0.0302(5) Uani 1 1 d . . . . .
H40A H 0.3818 0.8548 0.0730 0.036 Uiso 1 1 calc R U . . .
H40B H 0.3783 0.9834 0.0321 0.036 Uiso 1 1 calc R U . . .
C41 C 0.1356(3) 0.8219(3) 0.09958(12) 0.0395(6) Uani 1 1 d . . . . .
H41A H 0.1861 0.7816 0.1276 0.059 Uiso 1 1 calc R U . . .
H41B H 0.1274 0.7619 0.0747 0.059 Uiso 1 1 calc R U . . .
H41C H 0.0486 0.8458 0.1151 0.059 Uiso 1 1 calc R U . . .
C42 C 0.2491(3) 0.3972(4) 0.44702(15) 0.0655(11) Uani 1 1 d . . . . .
H42A H 0.1871 0.3610 0.4274 0.098 Uiso 1 1 calc R U . . .
H42B H 0.2505 0.4901 0.4371 0.098 Uiso 1 1 calc R U . . .
H42C H 0.2223 0.3765 0.4850 0.098 Uiso 1 1 calc R U . . .
C43 C 0.3825(3) 0.2062(3) 0.45181(10) 0.0347(6) Uani 1 1 d . . . . .
H43A H 0.4680 0.1712 0.4385 0.042 Uiso 1 1 calc R U . . .
H43B H 0.3144 0.1662 0.4359 0.042 Uiso 1 1 calc R U . . .
C44 C 0.4207(3) 0.3720(3) 0.37757(10) 0.0359(6) Uani 1 1 d . . . . .
H44A H 0.3544 0.3395 0.3583 0.043 Uiso 1 1 calc R U . . .
H44B H 0.5035 0.3254 0.3695 0.043 Uiso 1 1 calc R U . . .
C45 C 0.4403(3) 0.5132(3) 0.35720(10) 0.0352(6) Uani 1 1 d . . . . .
H45A H 0.4750 0.5223 0.3194 0.042 Uiso 1 1 calc R U . . .
H45B H 0.3544 0.5576 0.3597 0.042 Uiso 1 1 calc R U . . .
C46 C 0.6619(3) 0.5284(3) 0.37542(17) 0.0581(9) Uani 1 1 d . . . . .
H46A H 0.6641 0.4356 0.3859 0.087 Uiso 1 1 calc R U . . .
H46B H 0.7190 0.5685 0.3959 0.087 Uiso 1 1 calc R U . . .
H46C H 0.6922 0.5485 0.3377 0.087 Uiso 1 1 calc R U . . .
C47 C 0.5230(3) 0.7157(3) 0.36956(10) 0.0334(6) Uani 1 1 d . . . . .
H47A H 0.4304 0.7437 0.3715 0.040 Uiso 1 1 calc R U . . .
H47B H 0.5611 0.7353 0.3323 0.040 Uiso 1 1 calc R U . . .
C48 C 0.5939(3) 0.7925(3) 0.40285(10) 0.0338(6) Uani 1 1 d . . . . .
H48A H 0.6887 0.7745 0.3964 0.041 Uiso 1 1 calc R U . . .
H48B H 0.5793 0.8844 0.3909 0.041 Uiso 1 1 calc R U . . .
C49 C 0.4190(3) 0.8070(5) 0.47128(15) 0.0810(15) Uani 1 1 d . . . . .
H49A H 0.3947 0.7927 0.5095 0.122 Uiso 1 1 calc R U . . .
H49B H 0.3621 0.7575 0.4542 0.122 Uiso 1 1 calc R U . . .
H49C H 0.4092 0.8979 0.4580 0.122 Uiso 1 1 calc R U . . .
C50 C 0.3609(3) 0.1690(3) 0.51178(10) 0.0347(6) Uani 1 1 d . . . . .
H50A H 0.2691 0.1885 0.5242 0.042 Uiso 1 1 calc R U . . .
H50B H 0.3748 0.0756 0.5203 0.042 Uiso 1 1 calc R U . . .
B1 B 0.0459(2) 0.4931(2) 0.25385(10) 0.0205(5) Uani 1 1 d . . . . .
N1 N -0.2478(2) 1.1172(2) 0.04004(8) 0.0288(4) Uani 1 1 d . . . . .
N2 N 0.00010(19) 1.13584(19) 0.08989(8) 0.0263(4) Uani 1 1 d . . . . .
N3 N 0.20219(19) 0.93617(19) 0.07180(8) 0.0260(4) Uani 1 1 d . . . . .
N4 N 0.3793(2) 0.3437(2) 0.43436(8) 0.0308(5) Uani 1 1 d . . . . .
N5 N 0.52886(19) 0.5766(2) 0.38549(8) 0.0285(4) Uani 1 1 d . . . . .
N6 N 0.55405(19) 0.7665(2) 0.45944(8) 0.0280(4) Uani 1 1 d . . . . .
F1 F 0.16638(15) 0.7296(2) 0.41612(7) 0.0536(5) Uani 1 1 d . . . . .
F2 F -0.00293(17) 0.62287(16) 0.44897(6) 0.0431(4) Uani 1 1 d . . . . .
F3 F -0.01189(18) 0.82711(17) 0.43864(7) 0.0469(4) Uani 1 1 d . . . . .
F4 F -0.11706(18) 1.04196(15) 0.25356(7) 0.0460(4) Uani 1 1 d . . . . .
F5 F -0.29465(19) 0.9558(2) 0.29129(8) 0.0676(6) Uani 1 1 d . . . . .
F6 F -0.21626(18) 0.91534(16) 0.21530(7) 0.0495(4) Uani 1 1 d . . . . .
F7 F -0.38272(15) 0.23801(17) 0.28262(6) 0.0420(4) Uani 1 1 d . . . . .
F8 F -0.50664(14) 0.34804(18) 0.23258(9) 0.0614(6) Uani 1 1 d . . . . .
F9 F -0.39409(19) 0.18973(18) 0.20642(7) 0.0572(5) Uani 1 1 d . . . . .
F10 F -0.28681(18) 0.5902(2) 0.06202(7) 0.0736(7) Uani 1 1 d . . . . .
F11 F -0.0843(2) 0.5539(2) 0.05114(7) 0.0719(7) Uani 1 1 d . . . . .
F12 F -0.1552(2) 0.71908(16) 0.08154(7) 0.0596(6) Uani 1 1 d . . . . .
F13A F 0.2171(9) -0.0124(9) 0.2660(4) 0.080(3) Uani 0.260(6) 1 d . . P A 1
F14A F 0.3703(10) 0.0905(10) 0.2825(6) 0.080(3) Uani 0.260(6) 1 d . . P A 1
F15A F 0.2771(10) -0.0398(10) 0.3398(5) 0.080(3) Uani 0.260(6) 1 d . . P A 1
F13B F 0.3786(3) 0.0608(4) 0.3294(2) 0.0995(17) Uani 0.740(6) 1 d . . P A 2
F14B F 0.2353(3) -0.0626(3) 0.31441(17) 0.0637(9) Uani 0.740(6) 1 d . U P A 2
F15B F 0.3284(4) 0.0759(3) 0.25349(14) 0.0680(10) Uani 0.740(6) 1 d . U P A 2
F16 F -0.22215(19) 0.1601(3) 0.41011(7) 0.0725(7) Uani 1 1 d . . . . .
F17 F -0.0706(2) 0.09302(19) 0.45770(7) 0.0673(6) Uani 1 1 d . . . . .
F18 F -0.12807(18) 0.28876(17) 0.44852(7) 0.0493(4) Uani 1 1 d . . . . .
F19 F 0.42872(16) 0.81033(17) 0.24433(8) 0.0532(5) Uani 1 1 d . . . . .
F20 F 0.58341(15) 0.68484(17) 0.22493(8) 0.0478(4) Uani 1 1 d . . . . .
F21 F 0.5228(2) 0.8261(2) 0.16511(7) 0.0776(8) Uani 1 1 d . . . . .
F22 F 0.35800(19) 0.32157(16) 0.09637(7) 0.0492(4) Uani 1 1 d . . . . .
F23 F 0.47498(16) 0.4811(2) 0.05999(7) 0.0579(6) Uani 1 1 d . . . . .
F25 F 0.27059(16) 0.48302(17) 0.05268(6) 0.0429(4) Uani 1 1 d . . . . .
Rb1 Rb -0.02070(5) 0.96563(5) 0.00896(2) 0.02949(13) Uani 0.5 1 d . . P . .
Rb2 Rb 0.44449(5) 0.52035(5) 0.50404(2) 0.03120(12) Uani 0.5 1 d . . P . .


_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
C1 C2 1.400(3) . ?
C1 C6 1.411(3) . ?
C1 B1 1.646(3) . ?
C2 C3 1.400(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.384(3) . ?
C3 C7 1.495(3) . ?
C4 C5 1.390(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.387(3) . ?
C5 C8 1.505(3) . ?
C6 H6 0.9500 . ?
C7 F3 1.332(3) . ?
C7 F2 1.339(3) . ?
C7 F1 1.340(3) . ?
C8 F5 1.327(3) . ?
C8 F4 1.335(3) . ?
C8 F6 1.340(3) . ?
C9 C14 1.398(3) . ?
C9 C10 1.408(3) . ?
C9 B1 1.654(3) . ?
C10 C11 1.393(3) . ?
C10 H10 0.9500 . ?
C11 C12 1.392(3) . ?
C11 C15 1.498(3) . ?
C12 C13 1.385(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.393(3) . ?
C13 C16 1.495(3) . ?
C14 H14 0.9500 . ?
C15 F8 1.329(3) . ?
C15 F9 1.332(3) . ?
C15 F7 1.340(3) . ?
C16 F10 1.311(3) . ?
C16 F12 1.325(3) . ?
C16 F11 1.329(3) . ?
C17 C18 1.400(3) . ?
C17 C22 1.406(3) . ?
C17 B1 1.642(3) . ?
C18 C19 1.393(3) . ?
C18 H18 0.9500 . ?
C19 C20 1.391(3) . ?
C19 C23 1.489(4) . ?
C20 C21 1.386(3) . ?
C20 H20 0.9500 . ?
C21 C22 1.394(3) . ?
C21 C24 1.499(3) . ?
C22 H22 0.9500 . ?
C23 F14A 1.139(11) . ?
C23 F15A 1.291(11) . ?
C23 F14B 1.297(4) . ?
C23 F15B 1.321(4) . ?
C23 F13B 1.381(5) . ?
C23 F13A 1.435(11) . ?
C24 F17 1.323(3) . ?
C24 F18 1.335(3) . ?
C24 F16 1.343(3) . ?
C25 C30 1.400(3) . ?
C25 C26 1.408(3) . ?
C25 B1 1.651(3) . ?
C26 C27 1.393(3) . ?
C26 H26 0.9500 . ?
C27 C28 1.390(3) . ?
C27 C31 1.502(3) . ?
C28 C29 1.386(3) . ?
C28 H28 0.9500 . ?
C29 C30 1.394(3) . ?
C29 C32 1.499(3) . ?
C30 H30 0.9500 . ?
C31 F21 1.322(3) . ?
C31 F19 1.325(3) . ?
C31 F20 1.337(3) . ?
C32 F23 1.332(3) . ?
C32 F22 1.335(3) . ?
C32 F25 1.347(3) . ?
C33 N1 1.465(3) . ?
C33 C40 1.528(4) 2_575 ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 N1 1.465(3) . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 N1 1.466(3) . ?
C35 C36 1.528(4) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 N2 1.470(3) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C37 N2 1.453(3) . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 N2 1.462(3) . ?
C38 C39 1.530(4) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 N3 1.468(3) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C40 N3 1.473(3) . ?
C40 C33 1.528(4) 2_575 ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C41 N3 1.462(3) . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 N4 1.462(4) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 N4 1.460(3) . ?
C43 C50 1.531(4) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 N4 1.467(3) . ?
C44 C45 1.522(4) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C45 N5 1.470(3) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 N5 1.458(4) . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 N5 1.472(3) . ?
C47 C48 1.525(4) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 N6 1.457(3) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C49 N6 1.457(4) . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C50 N6 1.460(3) 2_666 ?
C50 H50A 0.9900 . ?
C50 H50B 0.9900 . ?
N1 Rb1 2.899(2) . ?
N1 Rb1 3.066(2) 2_575 ?
N2 Rb1 2.890(2) 2_575 ?
N2 Rb1 2.980(2) . ?
N3 Rb1 2.948(2) . ?
N3 Rb1 3.012(2) 2_575 ?
N4 Rb2 2.921(2) . ?
N4 Rb2 3.071(2) 2_666 ?
N5 Rb2 2.924(2) 2_666 ?
N5 Rb2 3.056(2) . ?
N6 C50 1.460(3) 2_666 ?
N6 Rb2 2.902(2) . ?
N6 Rb2 3.047(2) 2_666 ?
F12 Rb1 3.2345(18) . ?
Rb1 Rb1 0.8960(10) 2_575 ?
Rb1 N2 2.890(2) 2_575 ?
Rb1 N3 3.012(2) 2_575 ?
Rb1 N1 3.066(2) 2_575 ?
Rb1 C37 3.116(4) 2_575 ?
Rb1 C41 3.613(3) 2_575 ?
Rb2 Rb2 1.2172(11) 2_666 ?
Rb2 N5 2.924(2) 2_666 ?
Rb2 N6 3.047(2) 2_666 ?
Rb2 N4 3.071(2) 2_666 ?
Rb2 C46 3.147(4) 2_666 ?
Rb2 C49 3.695(5) 2_666 ?
Rb2 C42 3.716(4) 2_666 ?

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
C2 C1 C6 115.5(2) . . ?
C2 C1 B1 122.9(2) . . ?
C6 C1 B1 121.5(2) . . ?
C1 C2 C3 122.1(2) . . ?
C1 C2 H2 118.9 . . ?
C3 C2 H2 118.9 . . ?
C4 C3 C2 120.9(2) . . ?
C4 C3 C7 120.7(2) . . ?
C2 C3 C7 118.4(2) . . ?
C3 C4 C5 118.2(2) . . ?
C3 C4 H4 120.9 . . ?
C5 C4 H4 120.9 . . ?
C6 C5 C4 120.8(2) . . ?
C6 C5 C8 121.1(2) . . ?
C4 C5 C8 118.1(2) . . ?
C5 C6 C1 122.4(2) . . ?
C5 C6 H6 118.8 . . ?
C1 C6 H6 118.8 . . ?
F3 C7 F2 106.6(2) . . ?
F3 C7 F1 106.6(2) . . ?
F2 C7 F1 105.7(2) . . ?
F3 C7 C3 113.2(2) . . ?
F2 C7 C3 112.2(2) . . ?
F1 C7 C3 112.01(19) . . ?
F5 C8 F4 107.0(2) . . ?
F5 C8 F6 105.9(2) . . ?
F4 C8 F6 105.6(2) . . ?
F5 C8 C5 112.5(2) . . ?
F4 C8 C5 112.2(2) . . ?
F6 C8 C5 113.0(2) . . ?
C14 C9 C10 115.3(2) . . ?
C14 C9 B1 122.37(19) . . ?
C10 C9 B1 122.16(19) . . ?
C11 C10 C9 122.3(2) . . ?
C11 C10 H10 118.8 . . ?
C9 C10 H10 118.8 . . ?
C12 C11 C10 120.7(2) . . ?
C12 C11 C15 118.8(2) . . ?
C10 C11 C15 120.4(2) . . ?
C13 C12 C11 118.0(2) . . ?
C13 C12 H12 121.0 . . ?
C11 C12 H12 121.0 . . ?
C12 C13 C14 120.8(2) . . ?
C12 C13 C16 120.4(2) . . ?
C14 C13 C16 118.8(2) . . ?
C13 C14 C9 122.8(2) . . ?
C13 C14 H14 118.6 . . ?
C9 C14 H14 118.6 . . ?
F8 C15 F9 108.0(2) . . ?
F8 C15 F7 105.32(19) . . ?
F9 C15 F7 104.9(2) . . ?
F8 C15 C11 112.2(2) . . ?
F9 C15 C11 112.36(19) . . ?
F7 C15 C11 113.49(19) . . ?
F10 C16 F12 106.3(2) . . ?
F10 C16 F11 105.9(2) . . ?
F12 C16 F11 104.3(2) . . ?
F10 C16 C13 114.39(19) . . ?
F12 C16 C13 113.1(2) . . ?
F11 C16 C13 112.0(2) . . ?
C18 C17 C22 115.2(2) . . ?
C18 C17 B1 123.41(19) . . ?
C22 C17 B1 121.14(19) . . ?
C19 C18 C17 122.6(2) . . ?
C19 C18 H18 118.7 . . ?
C17 C18 H18 118.7 . . ?
C20 C19 C18 120.9(2) . . ?
C20 C19 C23 118.9(2) . . ?
C18 C19 C23 120.2(2) . . ?
C21 C20 C19 117.9(2) . . ?
C21 C20 H20 121.1 . . ?
C19 C20 H20 121.1 . . ?
C20 C21 C22 120.9(2) . . ?
C20 C21 C24 120.1(2) . . ?
C22 C21 C24 119.0(2) . . ?
C21 C22 C17 122.6(2) . . ?
C21 C22 H22 118.7 . . ?
C17 C22 H22 118.7 . . ?
F14A C23 F15A 114.3(8) . . ?
F14B C23 F15B 110.2(3) . . ?
F14B C23 F13B 104.1(3) . . ?
F15B C23 F13B 99.6(3) . . ?
F14A C23 F13A 106.5(9) . . ?
F15A C23 F13A 97.2(7) . . ?
F14A C23 C19 118.0(5) . . ?
F15A C23 C19 112.4(5) . . ?
F14B C23 C19 115.2(2) . . ?
F15B C23 C19 115.1(3) . . ?
F13B C23 C19 111.0(3) . . ?
F13A C23 C19 105.6(4) . . ?
F17 C24 F18 106.1(2) . . ?
F17 C24 F16 106.7(2) . . ?
F18 C24 F16 104.6(2) . . ?
F17 C24 C21 113.9(2) . . ?
F18 C24 C21 112.8(2) . . ?
F16 C24 C21 111.9(2) . . ?
C30 C25 C26 115.66(19) . . ?
C30 C25 B1 121.80(19) . . ?
C26 C25 B1 122.53(19) . . ?
C27 C26 C25 122.2(2) . . ?
C27 C26 H26 118.9 . . ?
C25 C26 H26 118.9 . . ?
C28 C27 C26 120.7(2) . . ?
C28 C27 C31 118.1(2) . . ?
C26 C27 C31 121.2(2) . . ?
C29 C28 C27 118.4(2) . . ?
C29 C28 H28 120.8 . . ?
C27 C28 H28 120.8 . . ?
C28 C29 C30 120.6(2) . . ?
C28 C29 C32 120.5(2) . . ?
C30 C29 C32 118.9(2) . . ?
C29 C30 C25 122.4(2) . . ?
C29 C30 H30 118.8 . . ?
C25 C30 H30 118.8 . . ?
F21 C31 F19 108.1(2) . . ?
F21 C31 F20 105.8(2) . . ?
F19 C31 F20 104.6(2) . . ?
F21 C31 C27 112.4(2) . . ?
F19 C31 C27 113.39(19) . . ?
F20 C31 C27 112.0(2) . . ?
F23 C32 F22 107.1(2) . . ?
F23 C32 F25 106.0(2) . . ?
F22 C32 F25 105.8(2) . . ?
F23 C32 C29 113.0(2) . . ?
F22 C32 C29 112.5(2) . . ?
F25 C32 C29 111.8(2) . . ?
N1 C33 C40 114.3(2) . 2_575 ?
N1 C33 H33A 108.7 . . ?
C40 C33 H33A 108.7 2_575 . ?
N1 C33 H33B 108.7 . . ?
C40 C33 H33B 108.7 2_575 . ?
H33A C33 H33B 107.6 . . ?
N1 C34 H34A 109.5 . . ?
N1 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
N1 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
N1 C35 C36 114.7(2) . . ?
N1 C35 H35A 108.6 . . ?
C36 C35 H35A 108.6 . . ?
N1 C35 H35B 108.6 . . ?
C36 C35 H35B 108.6 . . ?
H35A C35 H35B 107.6 . . ?
N2 C36 C35 114.4(2) . . ?
N2 C36 H36A 108.6 . . ?
C35 C36 H36A 108.6 . . ?
N2 C36 H36B 108.6 . . ?
C35 C36 H36B 108.6 . . ?
H36A C36 H36B 107.6 . . ?
N2 C37 H37A 109.5 . . ?
N2 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
N2 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
N2 C38 C39 114.3(2) . . ?
N2 C38 H38A 108.7 . . ?
C39 C38 H38A 108.7 . . ?
N2 C38 H38B 108.7 . . ?
C39 C38 H38B 108.7 . . ?
H38A C38 H38B 107.6 . . ?
N3 C39 C38 113.7(2) . . ?
N3 C39 H39A 108.8 . . ?
C38 C39 H39A 108.8 . . ?
N3 C39 H39B 108.8 . . ?
C38 C39 H39B 108.8 . . ?
H39A C39 H39B 107.7 . . ?
N3 C40 C33 114.3(2) . 2_575 ?
N3 C40 H40A 108.7 . . ?
C33 C40 H40A 108.7 2_575 . ?
N3 C40 H40B 108.7 . . ?
C33 C40 H40B 108.7 2_575 . ?
H40A C40 H40B 107.6 . . ?
N3 C41 H41A 109.5 . . ?
N3 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
N3 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
N4 C42 H42A 109.5 . . ?
N4 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
N4 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
N4 C43 C50 114.1(2) . . ?
N4 C43 H43A 108.7 . . ?
C50 C43 H43A 108.7 . . ?
N4 C43 H43B 108.7 . . ?
C50 C43 H43B 108.7 . . ?
H43A C43 H43B 107.6 . . ?
N4 C44 C45 114.5(2) . . ?
N4 C44 H44A 108.6 . . ?
C45 C44 H44A 108.6 . . ?
N4 C44 H44B 108.6 . . ?
C45 C44 H44B 108.6 . . ?
H44A C44 H44B 107.6 . . ?
N5 C45 C44 114.5(2) . . ?
N5 C45 H45A 108.6 . . ?
C44 C45 H45A 108.6 . . ?
N5 C45 H45B 108.6 . . ?
C44 C45 H45B 108.6 . . ?
H45A C45 H45B 107.6 . . ?
N5 C46 H46A 109.5 . . ?
N5 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
N5 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
N5 C47 C48 114.6(2) . . ?
N5 C47 H47A 108.6 . . ?
C48 C47 H47A 108.6 . . ?
N5 C47 H47B 108.6 . . ?
C48 C47 H47B 108.6 . . ?
H47A C47 H47B 107.6 . . ?
N6 C48 C47 114.8(2) . . ?
N6 C48 H48A 108.6 . . ?
C47 C48 H48A 108.6 . . ?
N6 C48 H48B 108.6 . . ?
C47 C48 H48B 108.6 . . ?
H48A C48 H48B 107.6 . . ?
N6 C49 H49A 109.5 . . ?
N6 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
N6 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
N6 C50 C43 114.2(2) 2_666 . ?
N6 C50 H50A 108.7 2_666 . ?
C43 C50 H50A 108.7 . . ?
N6 C50 H50B 108.7 2_666 . ?
C43 C50 H50B 108.7 . . ?
H50A C50 H50B 107.6 . . ?
C17 B1 C1 111.66(18) . . ?
C17 B1 C25 110.44(18) . . ?
C1 B1 C25 108.32(18) . . ?
C17 B1 C9 108.55(18) . . ?
C1 B1 C9 107.55(17) . . ?
C25 B1 C9 110.28(17) . . ?
C33 N1 C34 110.5(2) . . ?
C33 N1 C35 110.3(2) . . ?
C34 N1 C35 109.9(2) . . ?
C33 N1 Rb1 118.09(15) . . ?
C34 N1 Rb1 89.40(18) . . ?
C35 N1 Rb1 116.46(14) . . ?
C33 N1 Rb1 110.76(14) . 2_575 ?
C34 N1 Rb1 106.38(18) . 2_575 ?
C35 N1 Rb1 108.85(14) . 2_575 ?
Rb1 N1 Rb1 16.98(2) . 2_575 ?
C37 N2 C38 110.4(2) . . ?
C37 N2 C36 109.9(2) . . ?
C38 N2 C36 110.34(19) . . ?
C37 N2 Rb1 84.85(18) . 2_575 ?
C38 N2 Rb1 119.35(15) . 2_575 ?
C36 N2 Rb1 118.65(14) . 2_575 ?
C37 N2 Rb1 102.27(18) . . ?
C38 N2 Rb1 113.30(15) . . ?
C36 N2 Rb1 110.40(14) . . ?
Rb1 N2 Rb1 17.47(2) 2_575 . ?
C41 N3 C39 110.9(2) . . ?
C41 N3 C40 111.1(2) . . ?
C39 N3 C40 110.37(19) . . ?
C41 N3 Rb1 84.82(14) . . ?
C39 N3 Rb1 118.03(14) . . ?
C40 N3 Rb1 118.69(14) . . ?
C41 N3 Rb1 102.06(15) . 2_575 ?
C39 N3 Rb1 111.24(14) . 2_575 ?
C40 N3 Rb1 110.93(14) . 2_575 ?
Rb1 N3 Rb1 17.25(2) . 2_575 ?
C43 N4 C42 110.8(2) . . ?
C43 N4 C44 110.6(2) . . ?
C42 N4 C44 110.5(2) . . ?
C43 N4 Rb2 120.17(15) . . ?
C42 N4 Rb2 81.2(2) . . ?
C44 N4 Rb2 119.25(15) . . ?
C43 N4 Rb2 110.27(14) . 2_666 ?
C42 N4 Rb2 104.5(2) . 2_666 ?
C44 N4 Rb2 110.06(15) . 2_666 ?
Rb2 N4 Rb2 23.27(3) . 2_666 ?
C46 N5 C45 110.5(2) . . ?
C46 N5 C47 110.4(2) . . ?
C45 N5 C47 110.2(2) . . ?
C46 N5 Rb2 84.82(19) . 2_666 ?
C45 N5 Rb2 119.42(15) . 2_666 ?
C47 N5 Rb2 118.30(14) . 2_666 ?
C46 N5 Rb2 108.2(2) . . ?
C45 N5 Rb2 109.27(14) . . ?
C47 N5 Rb2 108.23(14) . . ?
Rb2 N5 Rb2 23.36(3) 2_666 . ?
C49 N6 C48 110.3(2) . . ?
C49 N6 C50 110.3(2) . 2_666 ?
C48 N6 C50 110.5(2) . 2_666 ?
C49 N6 Rb2 81.2(2) . . ?
C48 N6 Rb2 119.11(15) . . ?
C50 N6 Rb2 120.91(15) 2_666 . ?
C49 N6 Rb2 104.6(2) . 2_666 ?
C48 N6 Rb2 109.97(15) . 2_666 ?
C50 N6 Rb2 111.00(15) 2_666 2_666 ?
Rb2 N6 Rb2 23.45(3) . 2_666 ?
C16 F12 Rb1 144.78(16) . . ?
Rb1 Rb1 N2 86.96(7) 2_575 2_575 ?
Rb1 Rb1 N1 92.09(8) 2_575 . ?
N2 Rb1 N1 119.93(6) 2_575 . ?
Rb1 Rb1 N3 85.41(7) 2_575 . ?
N2 Rb1 N3 119.29(6) 2_575 . ?
N1 Rb1 N3 120.47(6) . . ?
Rb1 Rb1 N2 75.57(7) 2_575 . ?
N2 Rb1 N2 162.53(2) 2_575 . ?
N1 Rb1 N2 61.78(6) . . ?
N3 Rb1 N2 60.09(6) . . ?
Rb1 Rb1 N3 77.35(7) 2_575 2_575 ?
N2 Rb1 N3 60.35(6) 2_575 2_575 ?
N1 Rb1 N3 60.95(6) . 2_575 ?
N3 Rb1 N3 162.75(2) . 2_575 ?
N2 Rb1 N3 114.45(6) . 2_575 ?
Rb1 Rb1 N1 70.92(7) 2_575 2_575 ?
N2 Rb1 N1 60.84(6) 2_575 2_575 ?
N1 Rb1 N1 163.02(2) . 2_575 ?
N3 Rb1 N1 59.80(6) . 2_575 ?
N2 Rb1 N1 111.98(6) . 2_575 ?
N3 Rb1 N1 113.28(6) 2_575 2_575 ?
Rb1 Rb1 C37 114.54(9) 2_575 2_575 ?
N2 Rb1 C37 27.67(7) 2_575 2_575 ?
N1 Rb1 C37 117.97(7) . 2_575 ?
N3 Rb1 C37 116.78(7) . 2_575 ?
N2 Rb1 C37 169.66(7) . 2_575 ?
N3 Rb1 C37 71.49(7) 2_575 2_575 ?
N1 Rb1 C37 71.20(7) 2_575 2_575 ?
Rb1 Rb1 F12 175.17(8) 2_575 . ?
N2 Rb1 F12 96.67(5) 2_575 . ?
N1 Rb1 F12 88.85(6) . . ?
N3 Rb1 F12 90.03(5) . . ?
N2 Rb1 F12 100.78(5) . . ?
N3 Rb1 F12 107.21(5) 2_575 . ?
N1 Rb1 F12 108.07(6) 2_575 . ?
C37 Rb1 F12 69.00(6) 2_575 . ?
Rb1 Rb1 C41 54.04(7) 2_575 2_575 ?
N2 Rb1 C41 65.08(6) 2_575 2_575 ?
N1 Rb1 C41 66.53(6) . 2_575 ?
N3 Rb1 C41 139.44(6) . 2_575 ?
N2 Rb1 C41 103.42(6) . 2_575 ?
N3 Rb1 C41 23.32(6) 2_575 2_575 ?
N1 Rb1 C41 101.83(6) 2_575 2_575 ?
C37 Rb1 C41 85.11(8) 2_575 2_575 ?
F12 Rb1 C41 130.48(6) . 2_575 ?
Rb2 Rb2 N6 84.98(6) 2_666 . ?
Rb2 Rb2 N4 85.27(6) 2_666 . ?
N6 Rb2 N4 119.90(6) . . ?
Rb2 Rb2 N5 84.41(6) 2_666 2_666 ?
N6 Rb2 N5 118.57(6) . 2_666 ?
N4 Rb2 N5 119.18(6) . 2_666 ?
Rb2 Rb2 N6 71.57(6) 2_666 2_666 ?
N6 Rb2 N6 156.55(3) . 2_666 ?
N4 Rb2 N6 59.50(6) . 2_666 ?
N5 Rb2 N6 60.37(6) 2_666 2_666 ?
Rb2 Rb2 N5 72.24(6) 2_666 . ?
N6 Rb2 N5 60.50(6) . . ?
N4 Rb2 N5 60.04(6) . . ?
N5 Rb2 N5 156.64(3) 2_666 . ?
N6 Rb2 N5 110.31(6) 2_666 . ?
Rb2 Rb2 N4 71.46(6) 2_666 2_666 ?
N6 Rb2 N4 59.41(6) . 2_666 ?
N4 Rb2 N4 156.73(3) . 2_666 ?
N5 Rb2 N4 59.83(6) 2_666 2_666 ?
N6 Rb2 N4 110.95(6) 2_666 2_666 ?
N5 Rb2 N4 110.74(6) . 2_666 ?
Rb2 Rb2 C46 111.88(8) 2_666 2_666 ?
N6 Rb2 C46 119.16(8) . 2_666 ?
N4 Rb2 C46 119.48(8) . 2_666 ?
N5 Rb2 C46 27.47(7) 2_666 2_666 ?
N6 Rb2 C46 71.63(7) 2_666 2_666 ?
N5 Rb2 C46 175.88(7) . 2_666 ?
N4 Rb2 C46 71.31(7) 2_666 2_666 ?
Rb2 Rb2 C49 49.15(7) 2_666 2_666 ?
N6 Rb2 C49 134.12(7) . 2_666 ?
N4 Rb2 C49 63.71(7) . 2_666 ?
N5 Rb2 C49 64.64(7) 2_666 2_666 ?
N6 Rb2 C49 22.43(7) 2_666 2_666 ?
N5 Rb2 C49 98.58(7) . 2_666 ?
N4 Rb2 C49 99.32(7) 2_666 2_666 ?
C46 Rb2 C49 84.45(9) 2_666 2_666 ?
Rb2 Rb2 C42 49.07(7) 2_666 2_666 ?
N6 Rb2 C42 63.59(7) . 2_666 ?
N4 Rb2 C42 134.34(7) . 2_666 ?
N5 Rb2 C42 64.19(7) 2_666 2_666 ?
N6 Rb2 C42 99.32(7) 2_666 2_666 ?
N5 Rb2 C42 98.95(7) . 2_666 ?
N4 Rb2 C42 22.39(7) 2_666 2_666 ?
C46 Rb2 C42 84.16(8) 2_666 2_666 ?
C49 Rb2 C42 82.50(9) 2_666 2_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
C6 C1 C2 C3 1.2(3) . . . . ?
B1 C1 C2 C3 178.54(19) . . . . ?
C1 C2 C3 C4 -1.7(3) . . . . ?
C1 C2 C3 C7 178.1(2) . . . . ?
C2 C3 C4 C5 0.8(3) . . . . ?
C7 C3 C4 C5 -178.9(2) . . . . ?
C3 C4 C5 C6 0.4(3) . . . . ?
C3 C4 C5 C8 180.0(2) . . . . ?
C4 C5 C6 C1 -0.9(3) . . . . ?
C8 C5 C6 C1 179.6(2) . . . . ?
C2 C1 C6 C5 0.1(3) . . . . ?
B1 C1 C6 C5 -177.3(2) . . . . ?
C4 C3 C7 F3 4.6(3) . . . . ?
C2 C3 C7 F3 -175.2(2) . . . . ?
C4 C3 C7 F2 125.2(2) . . . . ?
C2 C3 C7 F2 -54.5(3) . . . . ?
C4 C3 C7 F1 -116.0(2) . . . . ?
C2 C3 C7 F1 64.2(3) . . . . ?
C6 C5 C8 F5 122.2(3) . . . . ?
C4 C5 C8 F5 -57.4(3) . . . . ?
C6 C5 C8 F4 -117.1(2) . . . . ?
C4 C5 C8 F4 63.3(3) . . . . ?
C6 C5 C8 F6 2.2(3) . . . . ?
C4 C5 C8 F6 -177.4(2) . . . . ?
C14 C9 C10 C11 -1.3(3) . . . . ?
B1 C9 C10 C11 174.3(2) . . . . ?
C9 C10 C11 C12 1.4(3) . . . . ?
C9 C10 C11 C15 179.6(2) . . . . ?
C10 C11 C12 C13 -0.7(3) . . . . ?
C15 C11 C12 C13 -178.9(2) . . . . ?
C11 C12 C13 C14 -0.1(3) . . . . ?
C11 C12 C13 C16 178.0(2) . . . . ?
C12 C13 C14 C9 0.2(3) . . . . ?
C16 C13 C14 C9 -178.0(2) . . . . ?
C10 C9 C14 C13 0.5(3) . . . . ?
B1 C9 C14 C13 -175.1(2) . . . . ?
C12 C11 C15 F8 -55.3(3) . . . . ?
C10 C11 C15 F8 126.5(2) . . . . ?
C12 C11 C15 F9 66.7(3) . . . . ?
C10 C11 C15 F9 -111.5(3) . . . . ?
C12 C11 C15 F7 -174.5(2) . . . . ?
C10 C11 C15 F7 7.2(3) . . . . ?
C12 C13 C16 F10 8.7(3) . . . . ?
C14 C13 C16 F10 -173.0(2) . . . . ?
C12 C13 C16 F12 130.7(2) . . . . ?
C14 C13 C16 F12 -51.1(3) . . . . ?
C12 C13 C16 F11 -111.8(3) . . . . ?
C14 C13 C16 F11 66.5(3) . . . . ?
C22 C17 C18 C19 0.5(3) . . . . ?
B1 C17 C18 C19 -174.1(2) . . . . ?
C17 C18 C19 C20 -1.2(4) . . . . ?
C17 C18 C19 C23 179.1(2) . . . . ?
C18 C19 C20 C21 1.0(4) . . . . ?
C23 C19 C20 C21 -179.3(2) . . . . ?
C19 C20 C21 C22 -0.3(3) . . . . ?
C19 C20 C21 C24 176.8(2) . . . . ?
C20 C21 C22 C17 -0.3(3) . . . . ?
C24 C21 C22 C17 -177.4(2) . . . . ?
C18 C17 C22 C21 0.2(3) . . . . ?
B1 C17 C22 C21 174.9(2) . . . . ?
C20 C19 C23 F14A -143.8(10) . . . . ?
C18 C19 C23 F14A 35.9(10) . . . . ?
C20 C19 C23 F15A -7.5(8) . . . . ?
C18 C19 C23 F15A 172.2(7) . . . . ?
C20 C19 C23 F14B 36.6(5) . . . . ?
C18 C19 C23 F14B -143.7(3) . . . . ?
C20 C19 C23 F15B 166.5(3) . . . . ?
C18 C19 C23 F15B -13.8(4) . . . . ?
C20 C19 C23 F13B -81.4(4) . . . . ?
C18 C19 C23 F13B 98.3(4) . . . . ?
C20 C19 C23 F13A 97.3(5) . . . . ?
C18 C19 C23 F13A -83.0(5) . . . . ?
C20 C21 C24 F17 18.0(4) . . . . ?
C22 C21 C24 F17 -164.9(2) . . . . ?
C20 C21 C24 F18 139.1(2) . . . . ?
C22 C21 C24 F18 -43.7(3) . . . . ?
C20 C21 C24 F16 -103.2(3) . . . . ?
C22 C21 C24 F16 73.9(3) . . . . ?
C30 C25 C26 C27 1.7(3) . . . . ?
B1 C25 C26 C27 -179.2(2) . . . . ?
C25 C26 C27 C28 0.7(3) . . . . ?
C25 C26 C27 C31 -178.4(2) . . . . ?
C26 C27 C28 C29 -2.3(3) . . . . ?
C31 C27 C28 C29 176.9(2) . . . . ?
C27 C28 C29 C30 1.4(3) . . . . ?
C27 C28 C29 C32 -179.8(2) . . . . ?
C28 C29 C30 C25 1.1(3) . . . . ?
C32 C29 C30 C25 -177.7(2) . . . . ?
C26 C25 C30 C29 -2.6(3) . . . . ?
B1 C25 C30 C29 178.3(2) . . . . ?
C28 C27 C31 F21 43.1(3) . . . . ?
C26 C27 C31 F21 -137.7(2) . . . . ?
C28 C27 C31 F19 166.1(2) . . . . ?
C26 C27 C31 F19 -14.7(3) . . . . ?
C28 C27 C31 F20 -75.8(3) . . . . ?
C26 C27 C31 F20 103.4(3) . . . . ?
C28 C29 C32 F23 6.2(3) . . . . ?
C30 C29 C32 F23 -175.0(2) . . . . ?
C28 C29 C32 F22 127.7(2) . . . . ?
C30 C29 C32 F22 -53.5(3) . . . . ?
C28 C29 C32 F25 -113.3(2) . . . . ?
C30 C29 C32 F25 65.5(3) . . . . ?
N1 C35 C36 N2 55.7(3) . . . . ?
N2 C38 C39 N3 -52.7(3) . . . . ?
N4 C44 C45 N5 53.7(3) . . . . ?
N5 C47 C48 N6 -54.4(3) . . . . ?
N4 C43 C50 N6 -51.9(3) . . . 2_666 ?
C18 C17 B1 C1 -146.6(2) . . . . ?
C22 C17 B1 C1 39.1(3) . . . . ?
C18 C17 B1 C25 -26.1(3) . . . . ?
C22 C17 B1 C25 159.66(19) . . . . ?
C18 C17 B1 C9 95.0(2) . . . . ?
C22 C17 B1 C9 -79.3(2) . . . . ?
C2 C1 B1 C17 28.6(3) . . . . ?
C6 C1 B1 C17 -154.18(19) . . . . ?
C2 C1 B1 C25 -93.2(2) . . . . ?
C6 C1 B1 C25 84.0(2) . . . . ?
C2 C1 B1 C9 147.6(2) . . . . ?
C6 C1 B1 C9 -35.2(3) . . . . ?
C30 C25 B1 C17 82.8(2) . . . . ?
C26 C25 B1 C17 -96.2(2) . . . . ?
C30 C25 B1 C1 -154.6(2) . . . . ?
C26 C25 B1 C1 26.3(3) . . . . ?
C30 C25 B1 C9 -37.2(3) . . . . ?
C26 C25 B1 C9 143.8(2) . . . . ?
C14 C9 B1 C17 -152.9(2) . . . . ?
C10 C9 B1 C17 31.8(3) . . . . ?
C14 C9 B1 C1 86.2(2) . . . . ?
C10 C9 B1 C1 -89.1(2) . . . . ?
C14 C9 B1 C25 -31.8(3) . . . . ?
C10 C9 B1 C25 153.0(2) . . . . ?
C40 C33 N1 C34 -68.6(3) 2_575 . . . ?
C40 C33 N1 C35 169.6(2) 2_575 . . . ?
C40 C33 N1 Rb1 32.2(3) 2_575 . . . ?
C40 C33 N1 Rb1 49.0(2) 2_575 . . 2_575 ?
C36 C35 N1 C33 -170.2(2) . . . . ?
C36 C35 N1 C34 67.7(3) . . . . ?
C36 C35 N1 Rb1 -32.0(3) . . . . ?
C36 C35 N1 Rb1 -48.5(2) . . . 2_575 ?
C39 C38 N2 C37 -67.2(3) . . . . ?
C39 C38 N2 C36 171.2(2) . . . . ?
C39 C38 N2 Rb1 28.5(3) . . . 2_575 ?
C39 C38 N2 Rb1 46.8(2) . . . . ?
C35 C36 N2 C37 64.6(3) . . . . ?
C35 C36 N2 C38 -173.4(2) . . . . ?
C35 C36 N2 Rb1 -30.5(3) . . . 2_575 ?
C35 C36 N2 Rb1 -47.4(2) . . . . ?
C38 C39 N3 C41 -65.0(3) . . . . ?
C38 C39 N3 C40 171.4(2) . . . . ?
C38 C39 N3 Rb1 30.4(3) . . . . ?
C38 C39 N3 Rb1 47.8(2) . . . 2_575 ?
C33 C40 N3 C41 66.4(3) 2_575 . . . ?
C33 C40 N3 C39 -170.2(2) 2_575 . . . ?
C33 C40 N3 Rb1 -29.4(3) 2_575 . . . ?
C33 C40 N3 Rb1 -46.4(2) 2_575 . . 2_575 ?
C50 C43 N4 C42 -66.0(3) . . . . ?
C50 C43 N4 C44 171.2(2) . . . . ?
C50 C43 N4 Rb2 25.8(3) . . . . ?
C50 C43 N4 Rb2 49.2(2) . . . 2_666 ?
C45 C44 N4 C43 -171.2(2) . . . . ?
C45 C44 N4 C42 65.7(3) . . . . ?
C45 C44 N4 Rb2 -25.5(3) . . . . ?
C45 C44 N4 Rb2 -49.1(3) . . . 2_666 ?
C44 C45 N5 C46 67.9(3) . . . . ?
C44 C45 N5 C47 -169.8(2) . . . . ?
C44 C45 N5 Rb2 -27.8(3) . . . 2_666 ?
C44 C45 N5 Rb2 -51.0(2) . . . . ?
C48 C47 N5 C46 -67.2(3) . . . . ?
C48 C47 N5 C45 170.5(2) . . . . ?
C48 C47 N5 Rb2 28.1(3) . . . 2_666 ?
C48 C47 N5 Rb2 51.1(2) . . . . ?
C47 C48 N6 C49 -65.5(3) . . . . ?
C47 C48 N6 C50 172.3(2) . . . 2_666 ?
C47 C48 N6 Rb2 25.6(3) . . . . ?
C47 C48 N6 Rb2 49.4(3) . . . 2_666 ?
F10 C16 F12 Rb1 -85.8(3) . . . . ?
F11 C16 F12 Rb1 25.9(4) . . . . ?
C13 C16 F12 Rb1 147.9(2) . . . . ?

_refine_diff_density_max         1.076
_refine_diff_density_min         -0.566
_refine_diff_density_rms         0.065

_shelxl_version_number           2013-4

_exptl_crystal_recrystallization_method 'Layering: CH2Cl2/hexane'
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
####################################################################### 
# 
# 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_[K(Me~3~tacn)~2~][BArF]
_database_code_depnum_ccdc_archive 'CCDC 1051102'
_audit_update_record             
;
2015-02-24 deposited with the CCDC.
2015-06-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H12 B F24, C18 H42 K N6'
_chemical_formula_sum            'C50 H54 B F24 K N6'
_chemical_formula_weight         1244.90

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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 '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'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   43.534(3)
_cell_length_b                   12.7141(9)
_cell_length_c                   21.2417(15)
_cell_angle_alpha                90
_cell_angle_beta                 101.647(10)
_cell_angle_gamma                90
_cell_volume                     11515.1(15)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    19909
_cell_measurement_theta_min      2.3
_cell_measurement_theta_max      27.5

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_F_000             5088
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.040
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    0.210
_shelx_estimated_absorpt_T_min   0.992
_shelx_estimated_absorpt_T_max   0.998
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.628
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'CrystalClear-SM Expert 3.1 b27 (Rigaku, 2012)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_source_power             2.475
_diffrn_source_voltage           45.0
_diffrn_source_current           55.0
_diffrn_source                   'Rotating Anode'

_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_radiation_collimation    'Confocal mirrors, VHF Varimax '

_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_detector_area_resol_mean 28.5714

_diffrn_measurement_device       'four-circle κ diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC12 (Right)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_reflns_number            21703
_diffrn_reflns_av_unetI/netI     0.1080
_diffrn_reflns_av_R_equivalents  0.1116
_diffrn_reflns_limit_h_min       -51
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         3.000
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measured_fraction_theta_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_point_group_measured_fraction_full 0.989
_reflns_number_total             10049
_reflns_number_gt                5829
_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       
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 2012)
;
_computing_cell_refinement       
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 2012)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 2012)
;
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'ORTEP-III (Farrugia, 2012)'
_computing_publication_material  
'PLATON (Spek, 2003), WinGX (Farrugia, 1999) and enCIFer (Allen et al., 2004).'

_refine_special_details          
; 
The high R1 and wR2 values are a result of poor crystal quality
combined with a large amount of positional disorder within the
BArF anion. Recollection did not afford a higher quality dataset. 
This explains the PLATON alerts RFACR01_ALERT_3_B and RFACG01_ALERT_3_C. 

Three of the CF3 groups were refined to account for rotational disorder 
with a global isotropic thermal parameter restraint of 0.006 applied to 
all fluorines.   
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1364P)²+65.8194P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10049
_refine_ls_number_parameters     813
_refine_ls_number_restraints     1165
_refine_ls_R_factor_all          0.1630
_refine_ls_R_factor_gt           0.1007
_refine_ls_wR_factor_ref         0.2963
_refine_ls_wR_factor_gt          0.2506
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_restrained_S_all      1.046
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001

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
C1 C 0.34559(12) 0.2675(4) 0.3423(2) 0.0226(11) Uani 1 1 d . U . . .
C2 C 0.31543(13) 0.2270(5) 0.3381(2) 0.0288(12) Uani 1 1 d . U . . .
H2 H 0.3128 0.1643 0.3608 0.035 Uiso 1 1 calc R U . . .
C3 C 0.28902(13) 0.2758(5) 0.3016(3) 0.0329(13) Uani 1 1 d . U . . .
C4 C 0.29181(13) 0.3663(5) 0.2674(3) 0.0315(13) Uani 1 1 d . U . . .
H4 H 0.2738 0.4000 0.2429 0.038 Uiso 1 1 calc R U . . .
C5 C 0.32173(12) 0.4069(4) 0.2700(2) 0.0255(11) Uani 1 1 d . U . . .
C6 C 0.34776(13) 0.3577(4) 0.3070(2) 0.0245(11) Uani 1 1 d . U . . .
H6 H 0.3679 0.3872 0.3080 0.029 Uiso 1 1 calc R U . . .
C7 C 0.25749(16) 0.2277(6) 0.3008(3) 0.0504(17) Uani 1 1 d . U . . .
C8 C 0.32537(13) 0.5044(5) 0.2337(3) 0.0295(12) Uani 1 1 d D U . . .
C9 C 0.37260(11) 0.2850(4) 0.4593(2) 0.0215(11) Uani 1 1 d . U . . .
C10 C 0.35527(12) 0.2449(4) 0.5020(2) 0.0219(11) Uani 1 1 d . U . . .
H10 H 0.3473 0.1754 0.4954 0.026 Uiso 1 1 calc R U . . .
C11 C 0.34911(13) 0.3017(4) 0.5538(3) 0.0278(12) Uani 1 1 d . U . . .
C12 C 0.35996(13) 0.4053(4) 0.5641(3) 0.0298(12) Uani 1 1 d . U . . .
H12 H 0.3556 0.4457 0.5989 0.036 Uiso 1 1 calc R U . . .
C13 C 0.37724(12) 0.4471(4) 0.5220(3) 0.0285(12) Uani 1 1 d . U . . .
C14 C 0.38327(12) 0.3893(4) 0.4705(3) 0.0253(11) Uani 1 1 d . U . . .
H14 H 0.3949 0.4207 0.4420 0.030 Uiso 1 1 calc R U . . .
C15 C 0.33076(15) 0.2523(5) 0.5979(3) 0.0381(14) Uani 1 1 d . U . . .
C16 C 0.38980(16) 0.5563(5) 0.5324(3) 0.0410(14) Uani 1 1 d . U . . .
C17 C 0.37545(12) 0.0949(4) 0.4044(2) 0.0222(11) Uani 1 1 d . U . . .
C18 C 0.39279(13) 0.0509(4) 0.4610(2) 0.0260(12) Uani 1 1 d . U . . .
H18 H 0.4037 0.0968 0.4932 0.031 Uiso 1 1 calc R U . . .
C19 C 0.39486(15) -0.0559(5) 0.4722(3) 0.0332(13) Uani 1 1 d . U . . .
C20 C 0.37896(16) -0.1260(5) 0.4269(3) 0.0372(14) Uani 1 1 d . U . . .
H20 H 0.3797 -0.1996 0.4345 0.045 Uiso 1 1 calc R U . . .
C21 C 0.36181(15) -0.0840(5) 0.3698(3) 0.0359(14) Uani 1 1 d . U . . .
C22 C 0.36035(13) 0.0224(4) 0.3587(3) 0.0278(12) Uani 1 1 d . U . . .
H22 H 0.3488 0.0477 0.3188 0.033 Uiso 1 1 calc R U . . .
C23 C 0.41354(17) -0.0966(5) 0.5351(3) 0.0460(16) Uani 1 1 d . U . . .
C24 C 0.34448(17) -0.1587(5) 0.3189(3) 0.0522(17) Uani 1 1 d D U . . .
C25 C 0.40919(12) 0.2448(4) 0.3722(2) 0.0233(11) Uani 1 1 d . U . . .
C26 C 0.43681(12) 0.2632(4) 0.4178(2) 0.0258(12) Uani 1 1 d . U . . .
H26 H 0.4359 0.2654 0.4621 0.031 Uiso 1 1 calc R U . . .
C27 C 0.46563(13) 0.2784(5) 0.3996(3) 0.0283(12) Uani 1 1 d . U . . .
C28 C 0.46810(13) 0.2768(4) 0.3357(3) 0.0273(12) Uani 1 1 d . U . . .
H28 H 0.4877 0.2881 0.3235 0.033 Uiso 1 1 calc R U . . .
C29 C 0.44114(13) 0.2581(4) 0.2902(2) 0.0267(12) Uani 1 1 d . U . . .
C30 C 0.41236(12) 0.2426(4) 0.3082(2) 0.0226(11) Uani 1 1 d . U . . .
H30 H 0.3943 0.2300 0.2757 0.027 Uiso 1 1 calc R U . . .
C31 C 0.49407(14) 0.2963(6) 0.4508(3) 0.0408(15) Uani 1 1 d . U . . .
C32 C 0.44310(14) 0.2586(5) 0.2203(3) 0.0356(13) Uani 1 1 d . U . . .
C33 C 0.3175(2) 0.2460(8) 0.1178(5) 0.080(3) Uani 1 1 d . U . . .
H33A H 0.3047 0.2971 0.1356 0.121 Uiso 1 1 calc R U . . .
H33B H 0.3261 0.2793 0.0836 0.121 Uiso 1 1 calc R U . . .
H33C H 0.3347 0.2216 0.1518 0.121 Uiso 1 1 calc R U . . .
C34 C 0.3156(2) 0.0808(8) 0.0621(6) 0.090(3) Uani 1 1 d . U . . .
H34A H 0.3378 0.1032 0.0708 0.107 Uiso 1 1 calc R U . . .
H34B H 0.3146 0.0124 0.0840 0.107 Uiso 1 1 calc R U . . .
C35 C 0.3062(2) 0.0641(9) -0.0040(5) 0.088(3) Uani 1 1 d . U . . .
H35A H 0.3158 -0.0029 -0.0141 0.105 Uiso 1 1 calc R U . . .
H35B H 0.3156 0.1206 -0.0259 0.105 Uiso 1 1 calc R U . . .
C36 C 0.2693(2) 0.0740(7) -0.1019(4) 0.065(2) Uani 1 1 d . U . . .
H36A H 0.2769 0.1439 -0.1108 0.098 Uiso 1 1 calc R U . . .
H36B H 0.2470 0.0676 -0.1221 0.098 Uiso 1 1 calc R U . . .
H36C H 0.2813 0.0202 -0.1195 0.098 Uiso 1 1 calc R U . . .
C37 C 0.2571(3) -0.0339(7) -0.0151(5) 0.088(3) Uani 1 1 d . U . . .
H37A H 0.2488 -0.0743 -0.0548 0.106 Uiso 1 1 calc R U . . .
H37B H 0.2729 -0.0788 0.0125 0.106 Uiso 1 1 calc R U . . .
C38 C 0.2325(3) -0.0174(8) 0.0168(5) 0.089(3) Uani 1 1 d . U . . .
H38A H 0.2292 -0.0844 0.0383 0.107 Uiso 1 1 calc R U . . .
H38B H 0.2134 -0.0051 -0.0166 0.107 Uiso 1 1 calc R U . . .
C39 C 0.2032(2) 0.0868(8) 0.0779(4) 0.078(3) Uani 1 1 d . U . . .
H39A H 0.1901 0.1211 0.0407 0.116 Uiso 1 1 calc R U . . .
H39B H 0.2056 0.1335 0.1153 0.116 Uiso 1 1 calc R U . . .
H39C H 0.1933 0.0209 0.0872 0.116 Uiso 1 1 calc R U . . .
C40 C 0.2564(2) 0.0444(8) 0.1229(4) 0.080(3) Uani 1 1 d . U . . .
H40A H 0.2451 0.0428 0.1589 0.096 Uiso 1 1 calc R U . . .
H40B H 0.2652 -0.0267 0.1197 0.096 Uiso 1 1 calc R U . . .
C41 C 0.2823(3) 0.1173(9) 0.1397(4) 0.091(3) Uani 1 1 d . U . . .
H41A H 0.2745 0.1789 0.1603 0.109 Uiso 1 1 calc R U . . .
H41B H 0.2984 0.0829 0.1730 0.109 Uiso 1 1 calc R U . . .
C42 C 0.06023(19) 0.2622(7) 0.3795(3) 0.063(2) Uani 1 1 d . U . . .
H42A H 0.0505 0.1950 0.3869 0.094 Uiso 1 1 calc R U . . .
H42B H 0.0474 0.3202 0.3904 0.094 Uiso 1 1 calc R U . . .
H42C H 0.0813 0.2662 0.4065 0.094 Uiso 1 1 calc R U . . .
C43 C 0.0814(2) 0.1936(9) 0.2898(5) 0.0873(13) Uani 1 1 d . U . . .
H43A H 0.0923 0.1533 0.3277 0.105 Uiso 1 1 calc R U . . .
H43B H 0.0978 0.2313 0.2724 0.105 Uiso 1 1 calc R U . . .
C44 C 0.0663(2) 0.1167(6) 0.2404(4) 0.067(2) Uani 1 1 d . U . . .
H44A H 0.0829 0.0864 0.2201 0.080 Uiso 1 1 calc R U . . .
H44B H 0.0578 0.0586 0.2628 0.080 Uiso 1 1 calc R U . . .
C45 C 0.0232(2) 0.0657(6) 0.1589(4) 0.065(2) Uani 1 1 d . U . . .
H45A H 0.0053 0.0912 0.1270 0.098 Uiso 1 1 calc R U . . .
H45B H 0.0156 0.0242 0.1916 0.098 Uiso 1 1 calc R U . . .
H45C H 0.0366 0.0215 0.1378 0.098 Uiso 1 1 calc R U . . .
C46 C 0.0523(3) 0.2198(7) 0.1422(4) 0.074(2) Uani 1 1 d . U . . .
H46A H 0.0755 0.2185 0.1531 0.089 Uiso 1 1 calc R U . . .
H46B H 0.0460 0.1848 0.0999 0.089 Uiso 1 1 calc R U . . .
C47 C 0.0432(3) 0.3255(9) 0.1337(5) 0.0873(13) Uani 1 1 d . U . . .
H47A H 0.0226 0.3274 0.1037 0.105 Uiso 1 1 calc R U . . .
H47B H 0.0584 0.3613 0.1121 0.105 Uiso 1 1 calc R U . . .
C48 C 0.0229(2) 0.4828(6) 0.1666(4) 0.064(2) Uani 1 1 d . U . . .
H48A H 0.0348 0.5235 0.1404 0.096 Uiso 1 1 calc R U . . .
H48B H 0.0195 0.5258 0.2028 0.096 Uiso 1 1 calc R U . . .
H48C H 0.0026 0.4624 0.1402 0.096 Uiso 1 1 calc R U . . .
C49 C 0.0691(2) 0.4174(9) 0.2317(5) 0.0873(13) Uani 1 1 d . U . . .
H49A H 0.0866 0.3865 0.2145 0.105 Uiso 1 1 calc R U . . .
H49B H 0.0713 0.4948 0.2305 0.105 Uiso 1 1 calc R U . . .
C50 C 0.0721(3) 0.3871(9) 0.2937(5) 0.0873(13) Uani 1 1 d . U . . .
H50A H 0.0596 0.4369 0.3142 0.105 Uiso 1 1 calc R U . . .
H50B H 0.0943 0.3975 0.3147 0.105 Uiso 1 1 calc R U . . .
B1 B 0.37603(13) 0.2210(5) 0.3935(3) 0.0211(12) Uani 1 1 d . U . . .
N1 N 0.29804(14) 0.1568(5) 0.0916(3) 0.0520(14) Uani 1 1 d . U . . .
N2 N 0.27317(15) 0.0596(4) -0.0332(3) 0.0494(14) Uani 1 1 d . U . . .
N3 N 0.23367(14) 0.0646(5) 0.0640(3) 0.0486(14) Uani 1 1 d . U . . .
N4 N 0.06241(14) 0.2701(6) 0.3118(3) 0.0576(16) Uani 1 1 d . U . . .
N5 N 0.04119(13) 0.1543(4) 0.1892(2) 0.0420(12) Uani 1 1 d . U . . .
N6 N 0.04054(14) 0.3886(5) 0.1909(3) 0.0509(14) Uani 1 1 d . U . . .
F1 F 0.24956(11) 0.2306(5) 0.3564(2) 0.0812(15) Uani 1 1 d . U . . .
F2 F 0.25688(10) 0.1251(4) 0.2857(2) 0.0734(13) Uani 1 1 d . U . . .
F3 F 0.23535(10) 0.2698(5) 0.2562(3) 0.0954(19) Uani 1 1 d . U . . .
F4A F 0.35463(10) 0.5303(4) 0.2330(3) 0.068(2) Uani 0.880(8) 1 d . U P A 1
F5A F 0.31360(15) 0.5895(4) 0.2571(3) 0.0557(15) Uani 0.880(8) 1 d . U P A 1
F6A F 0.30968(14) 0.5012(4) 0.17351(19) 0.0668(18) Uani 0.880(8) 1 d . U P A 1
F4B F 0.3400(8) 0.579(2) 0.2722(12) 0.047(7) Uani 0.120(8) 1 d D U P A 2
F5B F 0.3450(8) 0.480(2) 0.1939(14) 0.035(7) Uani 0.120(8) 1 d . U P A 2
F6B F 0.3011(7) 0.569(3) 0.222(2) 0.056(7) Uani 0.120(8) 1 d D U P A 2
F7 F 0.33358(13) 0.2979(3) 0.65353(18) 0.0641(13) Uani 1 1 d . U . . .
F8 F 0.30030(10) 0.2432(5) 0.5709(2) 0.0896(18) Uani 1 1 d . U . . .
F9 F 0.33929(12) 0.1521(3) 0.6119(2) 0.0649(12) Uani 1 1 d . U . . .
F10A F 0.37357(19) 0.6152(5) 0.5650(5) 0.075(3) Uani 0.749(11) 1 d . U P B 1
F11A F 0.41852(15) 0.5582(5) 0.5652(5) 0.082(3) Uani 0.749(11) 1 d . U P B 1
F12A F 0.3895(3) 0.6058(6) 0.4781(4) 0.095(3) Uani 0.749(11) 1 d . U P B 1
F10B F 0.4151(5) 0.5766(14) 0.5058(12) 0.060(5) Uani 0.251(11) 1 d . U P B 2
F11B F 0.3947(7) 0.5879(17) 0.5898(9) 0.075(6) Uani 0.251(11) 1 d . U P B 2
F12B F 0.3707(5) 0.6268(14) 0.4999(13) 0.062(5) Uani 0.251(11) 1 d . U P B 2
F13 F 0.44174(13) -0.0483(4) 0.5511(3) 0.0869(16) Uani 1 1 d . U . . .
F14 F 0.42007(12) -0.1950(3) 0.5353(2) 0.0765(15) Uani 1 1 d . U . . .
F15 F 0.40085(15) -0.0721(5) 0.5837(2) 0.104(2) Uani 1 1 d . U . . .
F16A F 0.3273(3) -0.2290(9) 0.3442(7) 0.063(3) Uani 0.491(13) 1 d . U P C 1
F17A F 0.3592(3) -0.2001(15) 0.2825(7) 0.088(4) Uani 0.491(13) 1 d . U P C 1
F18A F 0.3197(3) -0.1078(7) 0.2788(5) 0.082(4) Uani 0.491(13) 1 d D U P C 1
F16B F 0.3465(3) -0.1289(9) 0.2623(4) 0.070(4) Uani 0.509(13) 1 d . U P C 2
F17B F 0.3611(2) -0.2529(7) 0.3228(7) 0.074(4) Uani 0.509(13) 1 d D U P C 2
F18B F 0.3187(3) -0.1838(13) 0.3284(7) 0.073(4) Uani 0.509(13) 1 d . U P C 2
F19 F 0.50398(13) 0.2080(5) 0.4824(3) 0.0954(18) Uani 1 1 d . U . . .
F20 F 0.48914(10) 0.3611(5) 0.4959(2) 0.0871(17) Uani 1 1 d . U . . .
F21 F 0.51832(10) 0.3323(5) 0.4293(2) 0.0828(16) Uani 1 1 d . U . . .
F22 F 0.45737(10) 0.3446(3) 0.20422(17) 0.0521(10) Uani 1 1 d . U . . .
F23 F 0.46085(11) 0.1786(3) 0.20592(18) 0.0578(11) Uani 1 1 d . U . . .
F24 F 0.41579(9) 0.2530(4) 0.18104(17) 0.0696(14) Uani 1 1 d . U . . .
K1 K 0.2500 0.2500 0.0000 0.0370(5) Uani 1 2 d S U P . .
K2 K 0.0000 0.26939(15) 0.2500 0.0347(5) Uani 1 2 d S TU P . .


_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
C1 C6 1.385(8) . ?
C1 C2 1.397(8) . ?
C1 B1 1.645(7) . ?
C2 C3 1.396(8) . ?
C2 H2 0.9500 . ?
C3 C4 1.378(8) . ?
C3 C7 1.500(9) . ?
C4 C5 1.392(8) . ?
C4 H4 0.9500 . ?
C5 C6 1.391(7) . ?
C5 C8 1.485(8) . ?
C6 H6 0.9500 . ?
C7 F1 1.297(9) . ?
C7 F3 1.320(8) . ?
C7 F2 1.343(9) . ?
C8 F4A 1.319(7) . ?
C8 F6A 1.323(7) . ?
C8 F6B 1.326(10) . ?
C8 F4B 1.331(10) . ?
C8 F5A 1.336(8) . ?
C8 F5B 1.35(3) . ?
C9 C10 1.388(8) . ?
C9 C14 1.409(8) . ?
C9 B1 1.650(8) . ?
C10 C11 1.386(8) . ?
C10 H10 0.9500 . ?
C11 C12 1.402(8) . ?
C11 C15 1.488(9) . ?
C12 C13 1.386(8) . ?
C12 H12 0.9500 . ?
C13 C14 1.387(8) . ?
C13 C16 1.492(8) . ?
C14 H14 0.9500 . ?
C15 F7 1.300(7) . ?
C15 F8 1.340(8) . ?
C15 F9 1.344(8) . ?
C16 F11B 1.26(2) . ?
C16 F11A 1.303(9) . ?
C16 F12A 1.312(9) . ?
C16 F10A 1.318(9) . ?
C16 F12B 1.319(19) . ?
C16 F10B 1.361(18) . ?
C17 C18 1.401(7) . ?
C17 C22 1.403(7) . ?
C17 B1 1.620(8) . ?
C18 C19 1.378(8) . ?
C18 H18 0.9500 . ?
C19 C20 1.390(9) . ?
C19 C23 1.507(9) . ?
C20 C21 1.396(9) . ?
C20 H20 0.9500 . ?
C21 C22 1.373(9) . ?
C21 C24 1.519(8) . ?
C22 H22 0.9500 . ?
C23 F14 1.282(8) . ?
C23 F15 1.304(8) . ?
C23 F13 1.353(9) . ?
C24 F17A 1.218(13) . ?
C24 F18B 1.220(14) . ?
C24 F16B 1.282(12) . ?
C24 F16A 1.344(14) . ?
C24 F17B 1.392(8) . ?
C24 F18A 1.392(8) . ?
C25 C30 1.395(7) . ?
C25 C26 1.403(7) . ?
C25 B1 1.627(8) . ?
C26 C27 1.399(8) . ?
C26 H26 0.9500 . ?
C27 C28 1.383(8) . ?
C27 C31 1.491(8) . ?
C28 C29 1.382(8) . ?
C28 H28 0.9500 . ?
C29 C30 1.396(8) . ?
C29 C32 1.503(8) . ?
C30 H30 0.9500 . ?
C31 F20 1.314(8) . ?
C31 F21 1.315(8) . ?
C31 F19 1.335(9) . ?
C32 F24 1.310(7) . ?
C32 F22 1.336(7) . ?
C32 F23 1.350(7) . ?
C33 N1 1.456(10) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 C35 1.397(13) . ?
C34 N1 1.450(11) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 N2 1.448(11) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 N2 1.448(9) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 C38 1.394(13) . ?
C37 N2 1.470(11) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C38 N3 1.441(10) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 N3 1.443(10) . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 C41 1.448(13) . ?
C40 N3 1.453(10) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C41 N1 1.430(11) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 N4 1.464(10) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 N4 1.415(12) . ?
C43 C44 1.487(12) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 N5 1.459(9) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C45 N5 1.446(9) . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 C47 1.401(13) . ?
C46 N5 1.457(10) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 N6 1.480(12) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 N6 1.460(10) . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C49 C50 1.352(14) . ?
C49 N6 1.413(11) . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C50 N4 1.613(13) . ?
C50 H50A 0.9900 . ?
C50 H50B 0.9900 . ?
N1 K1 2.815(6) . ?
N2 K1 2.768(5) . ?
N3 K1 2.881(6) . ?
N4 K2 2.768(6) . ?
N5 K2 2.821(6) . ?
N6 K2 2.808(6) . ?
K1 N2 2.768(5) 7 ?
K1 N1 2.815(6) 7 ?
K1 N3 2.881(6) 7 ?
K1 C36 3.337(7) 7 ?
K1 C35 3.415(9) 7 ?
K1 C33 3.453(9) 7 ?
K1 C41 3.456(9) 7 ?
K1 C38 3.518(9) 7 ?
K2 N4 2.768(6) 2 ?
K2 N6 2.808(6) 2 ?
K2 N5 2.821(6) 2 ?
K2 C42 3.397(7) 2 ?
K2 C50 3.430(10) 2 ?
K2 C47 3.469(11) 2 ?
K2 C48 3.494(8) 2 ?
K2 C45 3.502(8) 2 ?
K2 C44 3.519(8) 2 ?

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
C6 C1 C2 115.9(5) . . ?
C6 C1 B1 121.5(4) . . ?
C2 C1 B1 122.1(5) . . ?
C3 C2 C1 122.0(5) . . ?
C3 C2 H2 119.0 . . ?
C1 C2 H2 119.0 . . ?
C4 C3 C2 120.9(5) . . ?
C4 C3 C7 120.8(5) . . ?
C2 C3 C7 118.3(5) . . ?
C3 C4 C5 118.0(5) . . ?
C3 C4 H4 121.0 . . ?
C5 C4 H4 121.0 . . ?
C6 C5 C4 120.3(5) . . ?
C6 C5 C8 120.6(5) . . ?
C4 C5 C8 119.1(5) . . ?
C1 C6 C5 122.8(5) . . ?
C1 C6 H6 118.6 . . ?
C5 C6 H6 118.6 . . ?
F1 C7 F3 110.6(6) . . ?
F1 C7 F2 104.4(6) . . ?
F3 C7 F2 104.3(7) . . ?
F1 C7 C3 112.9(6) . . ?
F3 C7 C3 112.1(5) . . ?
F2 C7 C3 111.9(6) . . ?
F4A C8 F6A 108.0(5) . . ?
F6B C8 F4B 86(3) . . ?
F4A C8 F5A 104.2(6) . . ?
F6A C8 F5A 102.9(5) . . ?
F6B C8 F5B 127(2) . . ?
F4B C8 F5B 105(2) . . ?
F4A C8 C5 114.8(5) . . ?
F6A C8 C5 112.8(5) . . ?
F6B C8 C5 117.0(17) . . ?
F4B C8 C5 111.4(14) . . ?
F5A C8 C5 113.1(5) . . ?
F5B C8 C5 106.4(12) . . ?
C10 C9 C14 116.1(5) . . ?
C10 C9 B1 121.7(5) . . ?
C14 C9 B1 121.6(5) . . ?
C11 C10 C9 123.0(5) . . ?
C11 C10 H10 118.5 . . ?
C9 C10 H10 118.5 . . ?
C10 C11 C12 120.0(5) . . ?
C10 C11 C15 119.7(5) . . ?
C12 C11 C15 120.3(5) . . ?
C13 C12 C11 117.9(5) . . ?
C13 C12 H12 121.0 . . ?
C11 C12 H12 121.0 . . ?
C12 C13 C14 121.4(5) . . ?
C12 C13 C16 119.4(5) . . ?
C14 C13 C16 119.2(5) . . ?
C13 C14 C9 121.5(5) . . ?
C13 C14 H14 119.2 . . ?
C9 C14 H14 119.2 . . ?
F7 C15 F8 109.4(5) . . ?
F7 C15 F9 104.6(5) . . ?
F8 C15 F9 102.6(6) . . ?
F7 C15 C11 114.8(5) . . ?
F8 C15 C11 112.2(5) . . ?
F9 C15 C11 112.3(5) . . ?
F11A C16 F12A 107.5(8) . . ?
F11A C16 F10A 105.5(7) . . ?
F12A C16 F10A 106.0(8) . . ?
F11B C16 F12B 104.8(17) . . ?
F11B C16 F10B 110.3(16) . . ?
F12B C16 F10B 97.5(15) . . ?
F11B C16 C13 115.2(11) . . ?
F11A C16 C13 112.3(6) . . ?
F12A C16 C13 112.2(6) . . ?
F10A C16 C13 112.8(6) . . ?
F12B C16 C13 112.4(9) . . ?
F10B C16 C13 114.7(8) . . ?
C18 C17 C22 115.3(5) . . ?
C18 C17 B1 119.8(4) . . ?
C22 C17 B1 124.7(5) . . ?
C19 C18 C17 123.2(5) . . ?
C19 C18 H18 118.4 . . ?
C17 C18 H18 118.4 . . ?
C18 C19 C20 120.4(5) . . ?
C18 C19 C23 119.8(6) . . ?
C20 C19 C23 119.8(6) . . ?
C19 C20 C21 117.5(5) . . ?
C19 C20 H20 121.3 . . ?
C21 C20 H20 121.3 . . ?
C22 C21 C20 121.6(5) . . ?
C22 C21 C24 119.7(6) . . ?
C20 C21 C24 118.7(6) . . ?
C21 C22 C17 122.0(5) . . ?
C21 C22 H22 119.0 . . ?
C17 C22 H22 119.0 . . ?
F14 C23 F15 111.0(6) . . ?
F14 C23 F13 104.6(6) . . ?
F15 C23 F13 101.6(7) . . ?
F14 C23 C19 114.7(6) . . ?
F15 C23 C19 112.4(6) . . ?
F13 C23 C19 111.5(5) . . ?
F18B C24 F16B 118.1(11) . . ?
F17A C24 F16A 111.8(11) . . ?
F18B C24 F17B 104.4(10) . . ?
F16B C24 F17B 100.2(9) . . ?
F17A C24 F18A 104.7(11) . . ?
F16A C24 F18A 97.4(9) . . ?
F17A C24 C21 118.1(8) . . ?
F18B C24 C21 112.8(8) . . ?
F16B C24 C21 111.3(7) . . ?
F16A C24 C21 111.6(8) . . ?
F17B C24 C21 108.6(7) . . ?
F18A C24 C21 110.9(6) . . ?
C30 C25 C26 115.9(5) . . ?
C30 C25 B1 122.4(4) . . ?
C26 C25 B1 121.6(5) . . ?
C27 C26 C25 121.5(5) . . ?
C27 C26 H26 119.2 . . ?
C25 C26 H26 119.2 . . ?
C28 C27 C26 121.4(5) . . ?
C28 C27 C31 120.1(5) . . ?
C26 C27 C31 118.5(5) . . ?
C29 C28 C27 117.8(5) . . ?
C29 C28 H28 121.1 . . ?
C27 C28 H28 121.1 . . ?
C28 C29 C30 121.0(5) . . ?
C28 C29 C32 118.7(5) . . ?
C30 C29 C32 120.3(5) . . ?
C25 C30 C29 122.3(5) . . ?
C25 C30 H30 118.8 . . ?
C29 C30 H30 118.8 . . ?
F20 C31 F21 107.3(6) . . ?
F20 C31 F19 104.2(6) . . ?
F21 C31 F19 105.5(6) . . ?
F20 C31 C27 113.2(5) . . ?
F21 C31 C27 113.9(5) . . ?
F19 C31 C27 112.0(6) . . ?
F24 C32 F22 106.9(5) . . ?
F24 C32 F23 107.6(5) . . ?
F22 C32 F23 104.0(5) . . ?
F24 C32 C29 113.8(5) . . ?
F22 C32 C29 112.2(5) . . ?
F23 C32 C29 111.7(5) . . ?
N1 C33 H33A 109.5 . . ?
N1 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
N1 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C35 C34 N1 117.6(7) . . ?
C35 C34 H34A 107.9 . . ?
N1 C34 H34A 107.9 . . ?
C35 C34 H34B 107.9 . . ?
N1 C34 H34B 107.9 . . ?
H34A C34 H34B 107.2 . . ?
C34 C35 N2 120.0(8) . . ?
C34 C35 H35A 107.3 . . ?
N2 C35 H35A 107.3 . . ?
C34 C35 H35B 107.3 . . ?
N2 C35 H35B 107.3 . . ?
H35A C35 H35B 106.9 . . ?
N2 C36 H36A 109.5 . . ?
N2 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
N2 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C38 C37 N2 117.3(8) . . ?
C38 C37 H37A 108.0 . . ?
N2 C37 H37A 108.0 . . ?
C38 C37 H37B 108.0 . . ?
N2 C37 H37B 108.0 . . ?
H37A C37 H37B 107.2 . . ?
C37 C38 N3 121.7(8) . . ?
C37 C38 H38A 106.9 . . ?
N3 C38 H38A 106.9 . . ?
C37 C38 H38B 106.9 . . ?
N3 C38 H38B 106.9 . . ?
H38A C38 H38B 106.7 . . ?
N3 C39 H39A 109.5 . . ?
N3 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
N3 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C41 C40 N3 117.4(7) . . ?
C41 C40 H40A 108.0 . . ?
N3 C40 H40A 108.0 . . ?
C41 C40 H40B 108.0 . . ?
N3 C40 H40B 108.0 . . ?
H40A C40 H40B 107.2 . . ?
N1 C41 C40 120.7(8) . . ?
N1 C41 H41A 107.2 . . ?
C40 C41 H41A 107.2 . . ?
N1 C41 H41B 107.2 . . ?
C40 C41 H41B 107.2 . . ?
H41A C41 H41B 106.8 . . ?
N4 C42 H42A 109.5 . . ?
N4 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
N4 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
N4 C43 C44 118.7(8) . . ?
N4 C43 H43A 107.6 . . ?
C44 C43 H43A 107.6 . . ?
N4 C43 H43B 107.6 . . ?
C44 C43 H43B 107.6 . . ?
H43A C43 H43B 107.1 . . ?
N5 C44 C43 117.9(7) . . ?
N5 C44 H44A 107.8 . . ?
C43 C44 H44A 107.8 . . ?
N5 C44 H44B 107.8 . . ?
C43 C44 H44B 107.8 . . ?
H44A C44 H44B 107.2 . . ?
N5 C45 H45A 109.5 . . ?
N5 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
N5 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C47 C46 N5 120.7(8) . . ?
C47 C46 H46A 107.1 . . ?
N5 C46 H46A 107.1 . . ?
C47 C46 H46B 107.1 . . ?
N5 C46 H46B 107.1 . . ?
H46A C46 H46B 106.8 . . ?
C46 C47 N6 118.8(9) . . ?
C46 C47 H47A 107.6 . . ?
N6 C47 H47A 107.6 . . ?
C46 C47 H47B 107.6 . . ?
N6 C47 H47B 107.6 . . ?
H47A C47 H47B 107.0 . . ?
N6 C48 H48A 109.5 . . ?
N6 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
N6 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C50 C49 N6 114.9(9) . . ?
C50 C49 H49A 108.5 . . ?
N6 C49 H49A 108.5 . . ?
C50 C49 H49B 108.5 . . ?
N6 C49 H49B 108.5 . . ?
H49A C49 H49B 107.5 . . ?
C49 C50 N4 121.1(9) . . ?
C49 C50 H50A 107.0 . . ?
N4 C50 H50A 107.0 . . ?
C49 C50 H50B 107.0 . . ?
N4 C50 H50B 107.0 . . ?
H50A C50 H50B 106.8 . . ?
C17 B1 C25 105.3(4) . . ?
C17 B1 C1 114.6(4) . . ?
C25 B1 C1 113.0(4) . . ?
C17 B1 C9 111.1(4) . . ?
C25 B1 C9 112.4(4) . . ?
C1 B1 C9 100.6(4) . . ?
C41 N1 C34 116.4(8) . . ?
C41 N1 C33 109.0(7) . . ?
C34 N1 C33 111.6(7) . . ?
C41 N1 K1 104.2(5) . . ?
C34 N1 K1 111.3(5) . . ?
C33 N1 K1 103.3(5) . . ?
C35 N2 C36 109.3(7) . . ?
C35 N2 C37 113.9(8) . . ?
C36 N2 C37 113.6(7) . . ?
C35 N2 K1 103.8(5) . . ?
C36 N2 K1 99.9(4) . . ?
C37 N2 K1 115.1(5) . . ?
C38 N3 C39 112.2(7) . . ?
C38 N3 C40 113.2(8) . . ?
C39 N3 C40 110.7(7) . . ?
C38 N3 K1 103.9(5) . . ?
C39 N3 K1 105.1(5) . . ?
C40 N3 K1 111.2(5) . . ?
C43 N4 C42 115.8(7) . . ?
C43 N4 C50 110.9(7) . . ?
C42 N4 C50 111.7(7) . . ?
C43 N4 K2 115.1(5) . . ?
C42 N4 K2 102.3(4) . . ?
C50 N4 K2 99.6(5) . . ?
C45 N5 C46 111.5(6) . . ?
C45 N5 C44 109.4(6) . . ?
C46 N5 C44 113.3(7) . . ?
C45 N5 K2 105.7(5) . . ?
C46 N5 K2 110.3(4) . . ?
C44 N5 K2 106.2(5) . . ?
C49 N6 C48 109.8(7) . . ?
C49 N6 C47 116.0(7) . . ?
C48 N6 C47 106.2(7) . . ?
C49 N6 K2 114.9(6) . . ?
C48 N6 K2 105.5(5) . . ?
C47 N6 K2 103.6(5) . . ?
N2 K1 N2 180.0 7 . ?
N2 K1 N1 63.24(18) 7 7 ?
N2 K1 N1 116.76(18) . 7 ?
N2 K1 N1 116.76(18) 7 . ?
N2 K1 N1 63.24(18) . . ?
N1 K1 N1 180.0(2) 7 . ?
N2 K1 N3 62.75(17) 7 7 ?
N2 K1 N3 117.25(17) . 7 ?
N1 K1 N3 63.18(18) 7 7 ?
N1 K1 N3 116.82(18) . 7 ?
N2 K1 N3 117.25(17) 7 . ?
N2 K1 N3 62.75(17) . . ?
N1 K1 N3 116.82(18) 7 . ?
N1 K1 N3 63.18(18) . . ?
N3 K1 N3 180.0 7 . ?
N2 K1 C36 25.3(2) 7 7 ?
N2 K1 C36 154.7(2) . 7 ?
N1 K1 C36 85.3(2) 7 7 ?
N1 K1 C36 94.7(2) . 7 ?
N3 K1 C36 82.89(19) 7 7 ?
N3 K1 C36 97.11(19) . 7 ?
N2 K1 C35 24.3(2) 7 7 ?
N2 K1 C35 155.7(2) . 7 ?
N1 K1 C35 44.7(2) 7 7 ?
N1 K1 C35 135.3(2) . 7 ?
N3 K1 C35 72.1(2) 7 7 ?
N3 K1 C35 107.9(2) . 7 ?
C36 K1 C35 40.9(2) 7 7 ?
N2 K1 C33 82.6(2) 7 7 ?
N2 K1 C33 97.4(2) . 7 ?
N1 K1 C33 24.2(2) 7 7 ?
N1 K1 C33 155.8(2) . 7 ?
N3 K1 C33 84.3(2) 7 7 ?
N3 K1 C33 95.7(2) . 7 ?
C36 K1 C33 99.9(2) 7 7 ?
C35 K1 C33 59.9(2) 7 7 ?
N2 K1 C41 71.7(2) 7 7 ?
N2 K1 C41 108.3(2) . 7 ?
N1 K1 C41 23.6(2) 7 7 ?
N1 K1 C41 156.4(2) . 7 ?
N3 K1 C41 44.9(2) 7 7 ?
N3 K1 C41 135.1(2) . 7 ?
C36 K1 C41 96.8(3) 7 7 ?
C35 K1 C41 60.9(3) 7 7 ?
C33 K1 C41 39.8(2) 7 7 ?
N2 K1 C38 43.8(2) 7 7 ?
N2 K1 C38 136.2(2) . 7 ?
N1 K1 C38 70.7(2) 7 7 ?
N1 K1 C38 109.3(2) . 7 ?
N3 K1 C38 23.42(19) 7 7 ?
N3 K1 C38 156.58(19) . 7 ?
C36 K1 C38 60.4(2) 7 7 ?
C35 K1 C38 60.3(3) 7 7 ?
C33 K1 C38 94.7(3) 7 7 ?
C41 K1 C38 60.0(3) 7 7 ?
N4 K2 N4 179.6(3) . 2 ?
N4 K2 N6 115.57(18) . 2 ?
N4 K2 N6 64.22(19) 2 2 ?
N4 K2 N6 64.22(19) . . ?
N4 K2 N6 115.57(18) 2 . ?
N6 K2 N6 114.7(3) 2 . ?
N4 K2 N5 64.21(16) . . ?
N4 K2 N5 115.99(18) 2 . ?
N6 K2 N5 178.56(18) 2 . ?
N6 K2 N5 63.92(17) . . ?
N4 K2 N5 115.99(18) . 2 ?
N4 K2 N5 64.21(16) 2 2 ?
N6 K2 N5 63.92(17) 2 2 ?
N6 K2 N5 178.56(18) . 2 ?
N5 K2 N5 117.5(2) . 2 ?
N4 K2 C42 155.12(19) . 2 ?
N4 K2 C42 24.90(19) 2 2 ?
N6 K2 C42 85.7(2) 2 2 ?
N6 K2 C42 95.99(19) . 2 ?
N5 K2 C42 94.21(19) . 2 ?
N5 K2 C42 84.19(17) 2 2 ?
N4 K2 C50 152.0(2) . 2 ?
N4 K2 C50 27.6(2) 2 2 ?
N6 K2 C50 42.5(2) 2 2 ?
N6 K2 C50 105.5(2) . 2 ?
N5 K2 C50 137.2(2) . 2 ?
N5 K2 C50 73.7(2) 2 2 ?
C42 K2 C50 43.8(2) 2 2 ?
N4 K2 C47 106.5(2) . 2 ?
N4 K2 C47 73.4(2) 2 2 ?
N6 K2 C47 24.5(2) 2 2 ?
N6 K2 C47 133.5(2) . 2 ?
N5 K2 C47 156.8(2) . 2 ?
N5 K2 C47 45.1(2) 2 2 ?
C42 K2 C47 98.1(2) 2 2 ?
C50 K2 C47 60.3(2) 2 2 ?
N4 K2 C48 96.34(19) . 2 ?
N4 K2 C48 83.4(2) 2 2 ?
N6 K2 C48 23.73(19) 2 2 ?
N6 K2 C48 94.4(2) . 2 ?
N5 K2 C48 155.19(19) . 2 ?
N5 K2 C48 84.14(19) 2 2 ?
C42 K2 C48 100.3(2) 2 2 ?
C50 K2 C48 57.3(2) 2 2 ?
C47 K2 C48 39.5(2) 2 2 ?
N4 K2 C45 96.1(2) . 2 ?
N4 K2 C45 84.20(19) 2 2 ?
N6 K2 C45 82.8(2) 2 2 ?
N6 K2 C45 157.5(2) . 2 ?
N5 K2 C45 98.6(2) . 2 ?
N5 K2 C45 23.42(18) 2 2 ?
C42 K2 C45 99.54(19) 2 2 ?
C50 K2 C45 97.0(2) 2 2 ?
C47 K2 C45 60.0(2) 2 2 ?
C48 K2 C45 98.7(2) 2 2 ?
N4 K2 C44 135.4(2) . 2 ?
N4 K2 C44 44.85(18) 2 2 ?
N6 K2 C44 71.0(2) 2 2 ?
N6 K2 C44 157.04(18) . 2 ?
N5 K2 C44 110.2(2) . 2 ?
N5 K2 C44 23.46(17) 2 2 ?
C42 K2 C44 61.57(19) 2 2 ?
C50 K2 C44 62.6(2) 2 2 ?
C47 K2 C44 60.2(2) 2 2 ?
C48 K2 C44 94.5(2) 2 2 ?
C45 K2 C44 39.48(18) 2 2 ?

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
C6 C1 C2 C3 -1.3(8) . . . . ?
B1 C1 C2 C3 170.5(5) . . . . ?
C1 C2 C3 C4 0.6(9) . . . . ?
C1 C2 C3 C7 -179.0(6) . . . . ?
C2 C3 C4 C5 0.6(9) . . . . ?
C7 C3 C4 C5 -179.8(6) . . . . ?
C3 C4 C5 C6 -1.0(8) . . . . ?
C3 C4 C5 C8 -180.0(5) . . . . ?
C2 C1 C6 C5 0.9(8) . . . . ?
B1 C1 C6 C5 -171.0(5) . . . . ?
C4 C5 C6 C1 0.2(8) . . . . ?
C8 C5 C6 C1 179.2(5) . . . . ?
C4 C3 C7 F1 -114.2(7) . . . . ?
C2 C3 C7 F1 65.4(9) . . . . ?
C4 C3 C7 F3 11.5(10) . . . . ?
C2 C3 C7 F3 -168.9(7) . . . . ?
C4 C3 C7 F2 128.4(6) . . . . ?
C2 C3 C7 F2 -52.0(8) . . . . ?
C6 C5 C8 F4A 8.4(8) . . . . ?
C4 C5 C8 F4A -172.7(6) . . . . ?
C6 C5 C8 F6A 132.6(6) . . . . ?
C4 C5 C8 F6A -48.4(7) . . . . ?
C6 C5 C8 F6B -153(2) . . . . ?
C4 C5 C8 F6B 26(2) . . . . ?
C6 C5 C8 F4B -56(2) . . . . ?
C4 C5 C8 F4B 122.6(19) . . . . ?
C6 C5 C8 F5A -111.1(6) . . . . ?
C4 C5 C8 F5A 67.9(7) . . . . ?
C6 C5 C8 F5B 58.0(18) . . . . ?
C4 C5 C8 F5B -123.1(17) . . . . ?
C14 C9 C10 C11 -1.4(7) . . . . ?
B1 C9 C10 C11 -172.7(5) . . . . ?
C9 C10 C11 C12 1.4(8) . . . . ?
C9 C10 C11 C15 -179.0(5) . . . . ?
C10 C11 C12 C13 -1.2(8) . . . . ?
C15 C11 C12 C13 179.3(5) . . . . ?
C11 C12 C13 C14 1.1(8) . . . . ?
C11 C12 C13 C16 -178.6(5) . . . . ?
C12 C13 C14 C9 -1.1(8) . . . . ?
C16 C13 C14 C9 178.5(5) . . . . ?
C10 C9 C14 C13 1.3(7) . . . . ?
B1 C9 C14 C13 172.6(5) . . . . ?
C10 C11 C15 F7 161.5(5) . . . . ?
C12 C11 C15 F7 -18.9(8) . . . . ?
C10 C11 C15 F8 -72.8(7) . . . . ?
C12 C11 C15 F8 106.8(7) . . . . ?
C10 C11 C15 F9 42.2(8) . . . . ?
C12 C11 C15 F9 -138.2(6) . . . . ?
C12 C13 C16 F11B 26.9(19) . . . . ?
C14 C13 C16 F11B -152.8(18) . . . . ?
C12 C13 C16 F11A 94.4(8) . . . . ?
C14 C13 C16 F11A -85.2(8) . . . . ?
C12 C13 C16 F12A -144.3(8) . . . . ?
C14 C13 C16 F12A 36.0(10) . . . . ?
C12 C13 C16 F10A -24.6(9) . . . . ?
C14 C13 C16 F10A 155.7(7) . . . . ?
C12 C13 C16 F12B -93.2(15) . . . . ?
C14 C13 C16 F12B 87.2(15) . . . . ?
C12 C13 C16 F10B 156.6(14) . . . . ?
C14 C13 C16 F10B -23.0(15) . . . . ?
C22 C17 C18 C19 -0.8(8) . . . . ?
B1 C17 C18 C19 -176.3(5) . . . . ?
C17 C18 C19 C20 -1.0(9) . . . . ?
C17 C18 C19 C23 -178.8(5) . . . . ?
C18 C19 C20 C21 1.7(9) . . . . ?
C23 C19 C20 C21 179.5(6) . . . . ?
C19 C20 C21 C22 -0.6(9) . . . . ?
C19 C20 C21 C24 179.3(6) . . . . ?
C20 C21 C22 C17 -1.2(9) . . . . ?
C24 C21 C22 C17 178.8(5) . . . . ?
C18 C17 C22 C21 1.9(8) . . . . ?
B1 C17 C22 C21 177.2(5) . . . . ?
C18 C19 C23 F14 -164.7(6) . . . . ?
C20 C19 C23 F14 17.5(9) . . . . ?
C18 C19 C23 F15 67.2(9) . . . . ?
C20 C19 C23 F15 -110.6(8) . . . . ?
C18 C19 C23 F13 -46.0(8) . . . . ?
C20 C19 C23 F13 136.2(7) . . . . ?
C22 C21 C24 F17A 97.1(14) . . . . ?
C20 C21 C24 F17A -82.8(14) . . . . ?
C22 C21 C24 F18B -95.8(12) . . . . ?
C20 C21 C24 F18B 84.2(12) . . . . ?
C22 C21 C24 F16B 39.6(11) . . . . ?
C20 C21 C24 F16B -140.3(9) . . . . ?
C22 C21 C24 F16A -131.1(9) . . . . ?
C20 C21 C24 F16A 49.0(11) . . . . ?
C22 C21 C24 F17B 149.0(9) . . . . ?
C20 C21 C24 F17B -31.0(11) . . . . ?
C22 C21 C24 F18A -23.6(10) . . . . ?
C20 C21 C24 F18A 156.5(9) . . . . ?
C30 C25 C26 C27 0.1(8) . . . . ?
B1 C25 C26 C27 176.7(5) . . . . ?
C25 C26 C27 C28 0.5(9) . . . . ?
C25 C26 C27 C31 -179.3(5) . . . . ?
C26 C27 C28 C29 -0.9(8) . . . . ?
C31 C27 C28 C29 178.9(6) . . . . ?
C27 C28 C29 C30 0.6(8) . . . . ?
C27 C28 C29 C32 178.5(5) . . . . ?
C26 C25 C30 C29 -0.3(8) . . . . ?
B1 C25 C30 C29 -176.9(5) . . . . ?
C28 C29 C30 C25 0.0(8) . . . . ?
C32 C29 C30 C25 -177.9(5) . . . . ?
C28 C27 C31 F20 137.3(6) . . . . ?
C26 C27 C31 F20 -42.9(8) . . . . ?
C28 C27 C31 F21 14.4(9) . . . . ?
C26 C27 C31 F21 -165.9(6) . . . . ?
C28 C27 C31 F19 -105.3(7) . . . . ?
C26 C27 C31 F19 74.5(8) . . . . ?
C28 C29 C32 F24 -172.1(5) . . . . ?
C30 C29 C32 F24 5.8(8) . . . . ?
C28 C29 C32 F22 -50.5(7) . . . . ?
C30 C29 C32 F22 127.4(6) . . . . ?
C28 C29 C32 F23 65.8(7) . . . . ?
C30 C29 C32 F23 -116.3(6) . . . . ?
N1 C34 C35 N2 -40.5(15) . . . . ?
N2 C37 C38 N3 -37.9(16) . . . . ?
N3 C40 C41 N1 -41.7(15) . . . . ?
N4 C43 C44 N5 38.7(14) . . . . ?
N5 C46 C47 N6 38.3(14) . . . . ?
N6 C49 C50 N4 44.9(14) . . . . ?
C18 C17 B1 C25 78.1(6) . . . . ?
C22 C17 B1 C25 -97.0(6) . . . . ?
C18 C17 B1 C1 -157.1(5) . . . . ?
C22 C17 B1 C1 27.8(7) . . . . ?
C18 C17 B1 C9 -43.9(6) . . . . ?
C22 C17 B1 C9 141.0(5) . . . . ?
C30 C25 B1 C17 88.9(6) . . . . ?
C26 C25 B1 C17 -87.4(6) . . . . ?
C30 C25 B1 C1 -36.9(7) . . . . ?
C26 C25 B1 C1 146.7(5) . . . . ?
C30 C25 B1 C9 -149.9(5) . . . . ?
C26 C25 B1 C9 33.7(7) . . . . ?
C6 C1 B1 C17 -152.0(5) . . . . ?
C2 C1 B1 C17 36.6(7) . . . . ?
C6 C1 B1 C25 -31.3(7) . . . . ?
C2 C1 B1 C25 157.3(5) . . . . ?
C6 C1 B1 C9 88.8(6) . . . . ?
C2 C1 B1 C9 -82.6(6) . . . . ?
C10 C9 B1 C17 -32.1(6) . . . . ?
C14 C9 B1 C17 157.1(5) . . . . ?
C10 C9 B1 C25 -149.8(5) . . . . ?
C14 C9 B1 C25 39.3(7) . . . . ?
C10 C9 B1 C1 89.7(5) . . . . ?
C14 C9 B1 C1 -81.1(5) . . . . ?
C40 C41 N1 C34 -66.4(12) . . . . ?
C40 C41 N1 C33 166.3(10) . . . . ?
C40 C41 N1 K1 56.6(11) . . . . ?
C35 C34 N1 C41 118.1(11) . . . . ?
C35 C34 N1 C33 -115.9(11) . . . . ?
C35 C34 N1 K1 -1.1(12) . . . . ?
C34 C35 N2 C36 162.7(10) . . . . ?
C34 C35 N2 C37 -69.0(12) . . . . ?
C34 C35 N2 K1 56.8(11) . . . . ?
C38 C37 N2 C35 119.0(11) . . . . ?
C38 C37 N2 C36 -115.0(10) . . . . ?
C38 C37 N2 K1 -0.7(13) . . . . ?
C37 C38 N3 C39 164.0(11) . . . . ?
C37 C38 N3 C40 -69.8(13) . . . . ?
C37 C38 N3 K1 51.0(12) . . . . ?
C41 C40 N3 C38 117.0(10) . . . . ?
C41 C40 N3 C39 -116.0(10) . . . . ?
C41 C40 N3 K1 0.4(11) . . . . ?
C44 C43 N4 C42 114.9(10) . . . . ?
C44 C43 N4 C50 -116.5(10) . . . . ?
C44 C43 N4 K2 -4.3(12) . . . . ?
C49 C50 N4 C43 63.0(12) . . . . ?
C49 C50 N4 C42 -166.2(9) . . . . ?
C49 C50 N4 K2 -58.7(10) . . . . ?
C47 C46 N5 C45 119.1(10) . . . . ?
C47 C46 N5 C44 -117.0(10) . . . . ?
C47 C46 N5 K2 2.0(11) . . . . ?
C43 C44 N5 C45 -162.0(9) . . . . ?
C43 C44 N5 C46 73.0(10) . . . . ?
C43 C44 N5 K2 -48.3(10) . . . . ?
C50 C49 N6 C48 116.0(10) . . . . ?
C50 C49 N6 C47 -123.7(10) . . . . ?
C50 C49 N6 K2 -2.7(12) . . . . ?
C46 C47 N6 C49 72.9(12) . . . . ?
C46 C47 N6 C48 -164.9(9) . . . . ?
C46 C47 N6 K2 -54.0(10) . . . . ?

_refine_diff_density_max         1.565
_refine_diff_density_min         -0.613
_refine_diff_density_rms         0.096

_shelxl_version_number           2013-4

_exptl_crystal_recrystallization_method 'Layering: CH2Cl2/hexane'
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
####################################################################### 
# 
# 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_[Li(Me~4~cyclen)(OH~2~)][BArF]
_database_code_depnum_ccdc_archive 'CCDC 1051103'
_audit_update_record             
;
2015-02-24 deposited with the CCDC.
2015-06-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H12 B F24, C12 H30 Li N4 O'
_chemical_formula_sum            'C44 H42 B F24 Li N4 O'
_chemical_formula_weight         1116.56

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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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, -z'

_cell_length_a                   12.729(2)
_cell_length_b                   12.7358(17)
_cell_length_c                   18.368(4)
_cell_angle_alpha                79.000(10)
_cell_angle_beta                 89.445(11)
_cell_angle_gamma                63.418(7)
_cell_volume                     2604.3(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4699
_cell_measurement_theta_min      2.6
_cell_measurement_theta_max      27.4

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_F_000             1132
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    0.145
_shelx_estimated_absorpt_T_min   0.990
_shelx_estimated_absorpt_T_max   0.994
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.568
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'CrystalClear-SM Expert 2.1 b29 (Rigaku, 2013)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_source_power             2.475
_diffrn_source_voltage           45.0
_diffrn_source_current           55.0
_diffrn_source                   'Rotating Anode'

_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_radiation_collimation    'Confocal mirrors, VHF Varimax '

_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_detector_area_resol_mean 28.5714

_diffrn_measurement_device       'four-circle κ diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC12 (Right)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_reflns_number            29717
_diffrn_reflns_av_unetI/netI     0.0481
_diffrn_reflns_av_R_equivalents  0.0536
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.012
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.974
_reflns_number_total             9170
_reflns_number_gt                6731
_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       
;
CrystalClear-SM Expert 2.1 b29 (Rigaku, 2013)
;
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.1 b29 (Rigaku, 2013)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.1 b29 (Rigaku, 2013)
;
_computing_structure_solution    'SUPERFLIP (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'ORTEP-III (Farrugia, 2012)'
_computing_publication_material  
'PLATON (Spek, 2003), WinGX (Farrugia, 1999) and enCIFer (Allen et al., 2004).'

_refine_special_details          
;
Four of the CF3 groups were refined to account for rotational 
disorder with an isotropic thermal parameter restraint of 0.01 
applied to the disordered fluorines. 

Two locations for the water molecule bonded to lithium were 
observed in the difference density map. Together the assigned 
electron density is consistent with one fully-occupied water
molecule although ADP restraints had to be used to obtain 
sensible ellipsoids. Hydrogens could not be located on either 
oxygen which explain the PLAT041, PLAT043 and PLAT068 level C
alerts. Attempts to model the water molecules as other moieties
(for example methoxide, peroxide, dinitrogen) were unsuccessful.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1730P)²+4.0056P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9170
_refine_ls_number_parameters     795
_refine_ls_number_restraints     1055
_refine_ls_R_factor_all          0.1195
_refine_ls_R_factor_gt           0.0992
_refine_ls_wR_factor_ref         0.3031
_refine_ls_wR_factor_gt          0.2832
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_restrained_S_all      1.069
_refine_ls_shift/su_max          0.004
_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
C1 C 0.5961(3) 0.2757(3) 0.34066(19) 0.0273(8) Uani 1 1 d . U . . .
C2 C 0.6035(3) 0.1634(3) 0.3760(2) 0.0322(8) Uani 1 1 d . U . . .
H2 H 0.5405 0.1458 0.3665 0.039 Uiso 1 1 calc R U . . .
C3 C 0.7000(4) 0.0779(3) 0.4242(2) 0.0374(9) Uani 1 1 d . U . . .
C4 C 0.7922(4) 0.0993(4) 0.4404(2) 0.0405(10) Uani 1 1 d . U . . .
H4 H 0.8578 0.0404 0.4734 0.049 Uiso 1 1 calc R U . . .
C5 C 0.7880(4) 0.2108(4) 0.4071(2) 0.0389(9) Uani 1 1 d . U . . .
C6 C 0.6914(3) 0.2952(3) 0.3581(2) 0.0308(8) Uani 1 1 d . U . . .
H6 H 0.6906 0.3692 0.3355 0.037 Uiso 1 1 calc R U . . .
C7 C 0.7030(5) -0.0414(4) 0.4596(3) 0.0583(13) Uani 1 1 d . U . . .
C8 C 0.8857(4) 0.2387(5) 0.4238(3) 0.0572(12) Uani 1 1 d D U . . .
C9 C 0.3720(3) 0.3473(3) 0.29741(19) 0.0248(7) Uani 1 1 d . U . . .
C10 C 0.3002(3) 0.3967(3) 0.35220(19) 0.0256(7) Uani 1 1 d . U . . .
H10 H 0.3134 0.4520 0.3742 0.031 Uiso 1 1 calc R U . . .
C11 C 0.2102(3) 0.3683(3) 0.37592(19) 0.0282(8) Uani 1 1 d . U . . .
C12 C 0.1856(3) 0.2901(3) 0.3448(2) 0.0310(8) Uani 1 1 d . U . . .
H12 H 0.1235 0.2713 0.3605 0.037 Uiso 1 1 calc R U . . .
C13 C 0.2549(3) 0.2401(3) 0.2898(2) 0.0308(8) Uani 1 1 d . U . . .
C14 C 0.3454(3) 0.2674(3) 0.2674(2) 0.0284(8) Uani 1 1 d . U . . .
H14 H 0.3916 0.2306 0.2301 0.034 Uiso 1 1 calc R U . . .
C15 C 0.1401(4) 0.4239(4) 0.4371(2) 0.0395(9) Uani 1 1 d . U . . .
C16 C 0.2303(4) 0.1555(4) 0.2532(3) 0.0451(10) Uani 1 1 d D U . . .
C17 C 0.4505(3) 0.5118(3) 0.28156(19) 0.0255(7) Uani 1 1 d . U . . .
C18 C 0.4655(3) 0.5477(3) 0.34707(19) 0.0280(8) Uani 1 1 d . U . . .
H18 H 0.5035 0.4879 0.3908 0.034 Uiso 1 1 calc R U . . .
C19 C 0.4264(4) 0.6680(3) 0.3498(2) 0.0331(8) Uani 1 1 d . U . . .
C20 C 0.3675(4) 0.7590(3) 0.2876(2) 0.0363(9) Uani 1 1 d . U . . .
H20 H 0.3395 0.8411 0.2896 0.044 Uiso 1 1 calc R U . . .
C21 C 0.3511(4) 0.7254(3) 0.2225(2) 0.0347(9) Uani 1 1 d . U . . .
C22 C 0.3926(3) 0.6055(3) 0.2196(2) 0.0293(8) Uani 1 1 d . U . . .
H22 H 0.3815 0.5859 0.1738 0.035 Uiso 1 1 calc R U . . .
C23 C 0.4467(5) 0.6997(4) 0.4210(2) 0.0479(11) Uani 1 1 d D U . . .
C24 C 0.2911(5) 0.8201(4) 0.1538(3) 0.0521(12) Uani 1 1 d . U . . .
C25 C 0.5306(3) 0.3491(3) 0.19510(19) 0.0271(8) Uani 1 1 d . U . . .
C26 C 0.4516(4) 0.3731(3) 0.1346(2) 0.0327(8) Uani 1 1 d . U . . .
H26 H 0.3701 0.4012 0.1415 0.039 Uiso 1 1 calc R U . . .
C27 C 0.4903(4) 0.3564(4) 0.0633(2) 0.0400(10) Uani 1 1 d . U . . .
C28 C 0.6070(4) 0.3178(4) 0.0508(2) 0.0435(10) Uani 1 1 d . U . . .
H28 H 0.6327 0.3071 0.0028 0.052 Uiso 1 1 calc R U . . .
C29 C 0.6865(4) 0.2947(4) 0.1099(2) 0.0409(10) Uani 1 1 d . U . . .
C30 C 0.6482(4) 0.3097(3) 0.1806(2) 0.0333(8) Uani 1 1 d . U . . .
H30 H 0.7047 0.2923 0.2202 0.040 Uiso 1 1 calc R U . . .
C31 C 0.4027(6) 0.3732(5) 0.0029(3) 0.0573(13) Uani 1 1 d . U . . .
C32 C 0.8160(5) 0.2511(5) 0.1011(3) 0.0558(12) Uani 1 1 d . U . . .
C33 C 0.8032(7) 0.6282(7) 0.3281(3) 0.0801(19) Uani 1 1 d . U . . .
H33A H 0.7725 0.7058 0.3430 0.120 Uiso 1 1 calc R U . . .
H33B H 0.8868 0.5804 0.3458 0.120 Uiso 1 1 calc R U . . .
H33C H 0.7590 0.5853 0.3498 0.120 Uiso 1 1 calc R U . . .
C34 C 0.8630(7) 0.5289(5) 0.2199(3) 0.0729(16) Uani 1 1 d . U . . .
H34A H 0.9360 0.4802 0.2536 0.088 Uiso 1 1 calc R U . . .
H34B H 0.8169 0.4830 0.2238 0.088 Uiso 1 1 calc R U . . .
C35 C 0.8951(6) 0.5471(5) 0.1426(4) 0.0710(16) Uani 1 1 d . U . . .
H35A H 0.9416 0.4684 0.1289 0.085 Uiso 1 1 calc R U . . .
H35B H 0.8228 0.5926 0.1080 0.085 Uiso 1 1 calc R U . . .
C36 C 1.0863(5) 0.5398(6) 0.1663(4) 0.0792(19) Uani 1 1 d . U . . .
H36A H 1.0900 0.5111 0.2201 0.119 Uiso 1 1 calc R U . . .
H36B H 1.1282 0.5888 0.1565 0.119 Uiso 1 1 calc R U . . .
H36C H 1.1232 0.4710 0.1423 0.119 Uiso 1 1 calc R U . . .
C37 C 0.9618(6) 0.6684(6) 0.0521(3) 0.0698(15) Uani 1 1 d . U . . .
H37A H 1.0315 0.6834 0.0455 0.084 Uiso 1 1 calc R U . . .
H37B H 0.9683 0.6097 0.0217 0.084 Uiso 1 1 calc R U . . .
C38 C 0.8586(7) 0.7772(6) 0.0257(3) 0.0738(16) Uani 1 1 d . U . . .
H38A H 0.8654 0.8098 -0.0266 0.089 Uiso 1 1 calc R U . . .
H38B H 0.7898 0.7604 0.0265 0.089 Uiso 1 1 calc R U . . .
C39 C 0.9176(5) 0.9193(5) 0.0495(4) 0.0696(16) Uani 1 1 d . U . . .
H39A H 0.9993 0.8596 0.0656 0.104 Uiso 1 1 calc R U . . .
H39B H 0.8960 0.9860 0.0751 0.104 Uiso 1 1 calc R U . . .
H39C H 0.9097 0.9495 -0.0044 0.104 Uiso 1 1 calc R U . . .
C40 C 0.7093(7) 0.9645(6) 0.0562(5) 0.099(2) Uani 1 1 d . U . . .
H40A H 0.7078 1.0387 0.0664 0.118 Uiso 1 1 calc R U . . .
H40B H 0.6796 0.9814 0.0035 0.118 Uiso 1 1 calc R U . . .
C41 C 0.6325(6) 0.9343(6) 0.1027(4) 0.097(2) Uani 1 1 d D U . . .
H41A H 0.5536 1.0046 0.0949 0.117 Uiso 1 1 calc R U . . .
H41B H 0.6243 0.8683 0.0865 0.117 Uiso 1 1 calc R U . . .
C42 C 0.6384(10) 1.0058(6) 0.2064(7) 0.138(4) Uani 1 1 d . U . . .
H42A H 0.6866 1.0439 0.1846 0.207 Uiso 1 1 calc R U . . .
H42B H 0.6530 0.9858 0.2608 0.207 Uiso 1 1 calc R U . . .
H42C H 0.5548 1.0612 0.1923 0.207 Uiso 1 1 calc R U . . .
C43 C 0.6094(6) 0.8259(6) 0.2226(4) 0.0775(17) Uani 1 1 d . U . . .
H43A H 0.6095 0.8321 0.2755 0.093 Uiso 1 1 calc R U . . .
H43B H 0.5263 0.8611 0.2022 0.093 Uiso 1 1 calc R U . . .
C44 C 0.6678(5) 0.7018(5) 0.2182(3) 0.0678(15) Uani 1 1 d . U . . .
H44A H 0.6623 0.6946 0.1658 0.081 Uiso 1 1 calc R U . . .
H44B H 0.6283 0.6586 0.2478 0.081 Uiso 1 1 calc R U . . .
Li1 Li 0.8510(7) 0.7708(7) 0.1825(4) 0.0414(14) Uani 1 1 d . U . . .
B1 B 0.4873(4) 0.3708(4) 0.2786(2) 0.0258(8) Uani 1 1 d . U . . .
N1 N 0.7898(4) 0.6481(4) 0.2459(2) 0.0570(11) Uani 1 1 d . U . . .
N2 N 0.9631(4) 0.6123(3) 0.1366(3) 0.0550(10) Uani 1 1 d . U . . .
N3 N 0.8393(4) 0.8635(4) 0.0678(2) 0.0572(11) Uani 1 1 d . U . . .
N4 N 0.6684(4) 0.8988(4) 0.1795(3) 0.0750(14) Uani 1 1 d D U . . .
F1A F 0.6434(13) -0.0379(8) 0.5243(5) 0.076(3) Uani 0.513(18) 1 d . U P A 1
F2A F 0.6381(13) -0.0753(11) 0.4179(6) 0.067(3) Uani 0.513(18) 1 d . U P A 1
F3A F 0.8026(8) -0.1316(9) 0.4786(9) 0.087(4) Uani 0.513(18) 1 d . U P A 1
F4A F 0.8477(5) 0.3347(5) 0.4569(4) 0.087(2) Uani 0.730(12) 1 d . U P B 1
F5A F 0.9753(7) 0.1544(6) 0.4640(6) 0.102(3) Uani 0.730(12) 1 d . U P B 1
F6A F 0.9231(7) 0.2768(9) 0.3597(4) 0.100(3) Uani 0.730(12) 1 d . U P B 1
F1B F 0.7997(13) -0.1265(9) 0.4330(11) 0.104(5) Uani 0.487(18) 1 d . U P A 2
F2B F 0.7356(18) -0.0660(9) 0.5301(5) 0.106(5) Uani 0.487(18) 1 d . U P A 2
F3B F 0.6154(13) -0.0500(16) 0.4472(15) 0.146(8) Uani 0.487(18) 1 d . U P A 2
F4B F 0.9896(10) 0.1429(12) 0.4212(11) 0.067(4) Uani 0.270(12) 1 d D U P B 2
F5B F 0.8918(16) 0.3285(13) 0.3779(10) 0.073(5) Uani 0.270(12) 1 d D U P B 2
F6B F 0.8948(16) 0.247(2) 0.4951(9) 0.095(5) Uani 0.270(12) 1 d . U P B 2
F7 F 0.0516(2) 0.3975(3) 0.45171(15) 0.0537(7) Uani 1 1 d . U . . .
F8 F 0.2056(3) 0.3893(5) 0.50006(17) 0.1001(15) Uani 1 1 d . U . . .
F9 F 0.0942(4) 0.5428(3) 0.4200(2) 0.0859(12) Uani 1 1 d . U . . .
F10A F 0.3118(11) 0.0927(15) 0.2144(9) 0.089(4) Uani 0.433(14) 1 d . U P C 1
F11A F 0.2151(15) 0.0741(9) 0.3033(6) 0.081(3) Uani 0.433(14) 1 d . U P C 1
F12A F 0.1306(11) 0.2112(8) 0.2106(8) 0.086(4) Uani 0.433(14) 1 d . U P C 1
F13A F 0.3933(6) 0.6619(5) 0.4760(2) 0.0747(18) Uani 0.765(10) 1 d . U P D 1
F14A F 0.5562(6) 0.6413(10) 0.4474(5) 0.121(4) Uani 0.765(10) 1 d . U P D 1
F15A F 0.4019(8) 0.8152(4) 0.4184(3) 0.095(3) Uani 0.765(10) 1 d . U P D 1
F10B F 0.1498(9) 0.1261(11) 0.2823(6) 0.085(3) Uani 0.567(14) 1 d D U P C 2
F11B F 0.2048(13) 0.1950(8) 0.1810(4) 0.088(3) Uani 0.567(14) 1 d . U P C 2
F12B F 0.3283(6) 0.0507(5) 0.2595(7) 0.078(3) Uani 0.567(14) 1 d D U P C 2
F13B F 0.4978(19) 0.7725(16) 0.4096(7) 0.060(4) Uani 0.235(10) 1 d . U P D 2
F14B F 0.3489(11) 0.752(2) 0.4531(11) 0.094(6) Uani 0.235(10) 1 d D U P D 2
F15B F 0.5313(17) 0.6157(12) 0.4697(10) 0.084(7) Uani 0.235(10) 1 d D U P D 2
F16 F 0.2303(3) 0.7925(3) 0.11022(18) 0.0769(11) Uani 1 1 d . U . . .
F17 F 0.2283(4) 0.9278(2) 0.16544(18) 0.0986(15) Uani 1 1 d . U . . .
F18 F 0.3716(4) 0.8325(4) 0.1074(2) 0.1081(15) Uani 1 1 d . U . . .
F19 F 0.2943(3) 0.4593(4) 0.00749(18) 0.0885(12) Uani 1 1 d . U . . .
F20 F 0.3952(4) 0.2717(4) 0.00269(18) 0.0958(14) Uani 1 1 d . U . . .
F21 F 0.4308(3) 0.4059(3) -0.06554(14) 0.0668(9) Uani 1 1 d . U . . .
F22 F 0.8463(3) 0.2291(4) 0.0348(2) 0.0837(11) Uani 1 1 d . U . . .
F23 F 0.8856(3) 0.1441(3) 0.1496(2) 0.0899(12) Uani 1 1 d . U . . .
F24 F 0.8551(3) 0.3254(3) 0.1168(2) 0.0742(10) Uani 1 1 d . U . . .
O1A O 0.9399(6) 0.8155(7) 0.2477(4) 0.0551(13) Uani 0.5 1 d . U P E 1
O1B O 1.0462(6) 0.7386(7) 0.2588(4) 0.0551(13) Uani 0.5 1 d . U P F 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
C1 C6 1.394(6) . ?
C1 C2 1.415(5) . ?
C1 B1 1.639(5) . ?
C2 C3 1.390(5) . ?
C2 H2 0.9500 . ?
C3 C4 1.366(6) . ?
C3 C7 1.518(6) . ?
C4 C5 1.413(6) . ?
C4 H4 0.9500 . ?
C5 C6 1.396(6) . ?
C5 C8 1.486(7) . ?
C6 H6 0.9500 . ?
C7 F3B 1.196(15) . ?
C7 F3A 1.265(10) . ?
C7 F2B 1.298(11) . ?
C7 F2A 1.384(12) . ?
C7 F1B 1.388(13) . ?
C7 F1A 1.401(10) . ?
C8 F5A 1.271(7) . ?
C8 F5B 1.317(9) . ?
C8 F6B 1.345(15) . ?
C8 F4B 1.348(9) . ?
C8 F6A 1.351(9) . ?
C8 F4A 1.360(8) . ?
C9 C10 1.398(5) . ?
C9 C14 1.408(5) . ?
C9 B1 1.646(5) . ?
C10 C11 1.391(5) . ?
C10 H10 0.9500 . ?
C11 C12 1.385(6) . ?
C11 C15 1.509(5) . ?
C12 C13 1.389(6) . ?
C12 H12 0.9500 . ?
C13 C14 1.382(5) . ?
C13 C16 1.514(6) . ?
C14 H14 0.9500 . ?
C15 F8 1.313(5) . ?
C15 F7 1.323(5) . ?
C15 F9 1.328(6) . ?
C16 F10A 1.299(10) . ?
C16 F11B 1.314(8) . ?
C16 F12A 1.315(10) . ?
C16 F10B 1.316(6) . ?
C16 F11A 1.330(10) . ?
C16 F12B 1.344(6) . ?
C17 C22 1.404(5) . ?
C17 C18 1.409(5) . ?
C17 B1 1.654(5) . ?
C18 C19 1.394(5) . ?
C18 H18 0.9500 . ?
C19 C20 1.395(6) . ?
C19 C23 1.498(6) . ?
C20 C21 1.391(6) . ?
C20 H20 0.9500 . ?
C21 C22 1.387(5) . ?
C21 C24 1.498(6) . ?
C22 H22 0.9500 . ?
C23 F14A 1.296(8) . ?
C23 F15A 1.309(6) . ?
C23 F15B 1.313(9) . ?
C23 F14B 1.317(9) . ?
C23 F13B 1.338(14) . ?
C23 F13A 1.344(6) . ?
C24 F17 1.302(5) . ?
C24 F16 1.314(6) . ?
C24 F18 1.370(7) . ?
C25 C30 1.390(6) . ?
C25 C26 1.399(6) . ?
C25 B1 1.655(5) . ?
C26 C27 1.415(5) . ?
C26 H26 0.9500 . ?
C27 C28 1.373(7) . ?
C27 C31 1.498(7) . ?
C28 C29 1.387(7) . ?
C28 H28 0.9500 . ?
C29 C30 1.400(5) . ?
C29 C32 1.503(7) . ?
C30 H30 0.9500 . ?
C31 F20 1.338(6) . ?
C31 F19 1.339(7) . ?
C31 F21 1.344(6) . ?
C32 F22 1.319(6) . ?
C32 F24 1.325(6) . ?
C32 F23 1.380(7) . ?
C33 N1 1.481(6) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 C35 1.478(9) . ?
C34 N1 1.550(8) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 N2 1.433(7) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 N2 1.463(7) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 C38 1.416(9) . ?
C37 N2 1.577(8) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C38 N3 1.394(8) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 N3 1.465(6) . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 C41 1.423(10) . ?
C40 N3 1.561(8) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C41 N4 1.410(7) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 N4 1.427(8) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 C44 1.432(9) . ?
C43 N4 1.544(8) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 N1 1.439(8) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
Li1 O1A 1.976(9) . ?
Li1 N4 2.154(9) . ?
Li1 N3 2.180(8) . ?
Li1 N1 2.186(8) . ?
Li1 N2 2.207(8) . ?

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
C6 C1 C2 115.4(3) . . ?
C6 C1 B1 122.8(3) . . ?
C2 C1 B1 121.6(3) . . ?
C3 C2 C1 122.2(4) . . ?
C3 C2 H2 118.9 . . ?
C1 C2 H2 118.9 . . ?
C4 C3 C2 121.2(4) . . ?
C4 C3 C7 119.2(4) . . ?
C2 C3 C7 119.6(4) . . ?
C3 C4 C5 118.6(4) . . ?
C3 C4 H4 120.7 . . ?
C5 C4 H4 120.7 . . ?
C6 C5 C4 119.6(4) . . ?
C6 C5 C8 119.9(4) . . ?
C4 C5 C8 120.5(4) . . ?
C1 C6 C5 122.9(4) . . ?
C1 C6 H6 118.5 . . ?
C5 C6 H6 118.5 . . ?
F3B C7 F2B 113.4(12) . . ?
F3A C7 F2A 107.0(9) . . ?
F3B C7 F1B 111.2(14) . . ?
F2B C7 F1B 102.3(9) . . ?
F3A C7 F1A 104.0(8) . . ?
F2A C7 F1A 98.4(8) . . ?
F3B C7 C3 115.3(8) . . ?
F3A C7 C3 118.1(6) . . ?
F2B C7 C3 108.8(6) . . ?
F2A C7 C3 113.6(6) . . ?
F1B C7 C3 104.7(7) . . ?
F1A C7 C3 113.6(5) . . ?
F5B C8 F6B 111.3(13) . . ?
F5B C8 F4B 104.5(11) . . ?
F6B C8 F4B 100.4(12) . . ?
F5A C8 F6A 108.0(7) . . ?
F5A C8 F4A 107.1(6) . . ?
F6A C8 F4A 102.8(6) . . ?
F5A C8 C5 116.6(5) . . ?
F5B C8 C5 117.1(8) . . ?
F6B C8 C5 112.7(8) . . ?
F4B C8 C5 109.1(8) . . ?
F6A C8 C5 109.9(5) . . ?
F4A C8 C5 111.5(4) . . ?
C10 C9 C14 114.8(3) . . ?
C10 C9 B1 120.8(3) . . ?
C14 C9 B1 124.0(3) . . ?
C11 C10 C9 122.7(3) . . ?
C11 C10 H10 118.6 . . ?
C9 C10 H10 118.6 . . ?
C12 C11 C10 121.0(3) . . ?
C12 C11 C15 120.4(4) . . ?
C10 C11 C15 118.5(3) . . ?
C11 C12 C13 117.6(4) . . ?
C11 C12 H12 121.2 . . ?
C13 C12 H12 121.2 . . ?
C14 C13 C12 121.0(4) . . ?
C14 C13 C16 119.5(3) . . ?
C12 C13 C16 119.6(4) . . ?
C13 C14 C9 122.9(3) . . ?
C13 C14 H14 118.6 . . ?
C9 C14 H14 118.6 . . ?
F8 C15 F7 106.4(4) . . ?
F8 C15 F9 106.2(4) . . ?
F7 C15 F9 106.9(4) . . ?
F8 C15 C11 112.0(4) . . ?
F7 C15 C11 113.5(3) . . ?
F9 C15 C11 111.4(3) . . ?
F10A C16 F12A 107.6(9) . . ?
F11B C16 F10B 109.7(7) . . ?
F10A C16 F11A 104.4(9) . . ?
F12A C16 F11A 103.7(8) . . ?
F11B C16 F12B 103.8(7) . . ?
F10B C16 F12B 104.8(7) . . ?
F10A C16 C13 116.3(6) . . ?
F11B C16 C13 112.2(4) . . ?
F12A C16 C13 112.3(5) . . ?
F10B C16 C13 115.5(5) . . ?
F11A C16 C13 111.6(6) . . ?
F12B C16 C13 110.0(5) . . ?
C22 C17 C18 115.5(3) . . ?
C22 C17 B1 121.4(3) . . ?
C18 C17 B1 122.9(3) . . ?
C19 C18 C17 122.1(3) . . ?
C19 C18 H18 118.9 . . ?
C17 C18 H18 118.9 . . ?
C18 C19 C20 121.0(3) . . ?
C18 C19 C23 119.4(3) . . ?
C20 C19 C23 119.6(4) . . ?
C21 C20 C19 117.7(3) . . ?
C21 C20 H20 121.2 . . ?
C19 C20 H20 121.2 . . ?
C22 C21 C20 121.0(3) . . ?
C22 C21 C24 119.4(3) . . ?
C20 C21 C24 119.5(3) . . ?
C21 C22 C17 122.6(3) . . ?
C21 C22 H22 118.7 . . ?
C17 C22 H22 118.7 . . ?
F14A C23 F15A 113.1(7) . . ?
F15B C23 F14B 111.0(12) . . ?
F15B C23 F13B 94.6(12) . . ?
F14B C23 F13B 108.4(13) . . ?
F14A C23 F13A 101.6(6) . . ?
F15A C23 F13A 103.5(5) . . ?
F14A C23 C19 112.1(5) . . ?
F15A C23 C19 114.3(4) . . ?
F15B C23 C19 117.3(9) . . ?
F14B C23 C19 112.9(8) . . ?
F13B C23 C19 111.0(7) . . ?
F13A C23 C19 111.1(4) . . ?
F17 C24 F16 110.7(5) . . ?
F17 C24 F18 103.6(4) . . ?
F16 C24 F18 101.3(4) . . ?
F17 C24 C21 114.9(4) . . ?
F16 C24 C21 113.9(4) . . ?
F18 C24 C21 111.2(4) . . ?
C30 C25 C26 116.1(3) . . ?
C30 C25 B1 121.4(3) . . ?
C26 C25 B1 122.4(3) . . ?
C25 C26 C27 121.5(4) . . ?
C25 C26 H26 119.3 . . ?
C27 C26 H26 119.3 . . ?
C28 C27 C26 121.0(4) . . ?
C28 C27 C31 120.3(4) . . ?
C26 C27 C31 118.5(4) . . ?
C27 C28 C29 118.3(4) . . ?
C27 C28 H28 120.8 . . ?
C29 C28 H28 120.8 . . ?
C28 C29 C30 120.5(4) . . ?
C28 C29 C32 121.7(4) . . ?
C30 C29 C32 117.8(4) . . ?
C25 C30 C29 122.6(4) . . ?
C25 C30 H30 118.7 . . ?
C29 C30 H30 118.7 . . ?
F20 C31 F19 108.1(5) . . ?
F20 C31 F21 105.5(4) . . ?
F19 C31 F21 104.9(4) . . ?
F20 C31 C27 111.8(4) . . ?
F19 C31 C27 113.0(4) . . ?
F21 C31 C27 112.9(4) . . ?
F22 C32 F24 108.8(4) . . ?
F22 C32 F23 104.2(4) . . ?
F24 C32 F23 103.5(5) . . ?
F22 C32 C29 113.9(5) . . ?
F24 C32 C29 112.6(4) . . ?
F23 C32 C29 113.0(4) . . ?
N1 C33 H33A 109.5 . . ?
N1 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
N1 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C35 C34 N1 113.1(4) . . ?
C35 C34 H34A 109.0 . . ?
N1 C34 H34A 109.0 . . ?
C35 C34 H34B 109.0 . . ?
N1 C34 H34B 109.0 . . ?
H34A C34 H34B 107.8 . . ?
N2 C35 C34 109.4(5) . . ?
N2 C35 H35A 109.8 . . ?
C34 C35 H35A 109.8 . . ?
N2 C35 H35B 109.8 . . ?
C34 C35 H35B 109.8 . . ?
H35A C35 H35B 108.2 . . ?
N2 C36 H36A 109.5 . . ?
N2 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
N2 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C38 C37 N2 113.1(4) . . ?
C38 C37 H37A 108.9 . . ?
N2 C37 H37A 108.9 . . ?
C38 C37 H37B 108.9 . . ?
N2 C37 H37B 108.9 . . ?
H37A C37 H37B 107.8 . . ?
N3 C38 C37 112.9(5) . . ?
N3 C38 H38A 109.0 . . ?
C37 C38 H38A 109.0 . . ?
N3 C38 H38B 109.0 . . ?
C37 C38 H38B 109.0 . . ?
H38A C38 H38B 107.8 . . ?
N3 C39 H39A 109.5 . . ?
N3 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
N3 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C41 C40 N3 113.2(5) . . ?
C41 C40 H40A 108.9 . . ?
N3 C40 H40A 108.9 . . ?
C41 C40 H40B 108.9 . . ?
N3 C40 H40B 108.9 . . ?
H40A C40 H40B 107.7 . . ?
N4 C41 C40 115.5(7) . . ?
N4 C41 H41A 108.4 . . ?
C40 C41 H41A 108.4 . . ?
N4 C41 H41B 108.4 . . ?
C40 C41 H41B 108.4 . . ?
H41A C41 H41B 107.5 . . ?
N4 C42 H42A 109.5 . . ?
N4 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
N4 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C44 C43 N4 112.6(5) . . ?
C44 C43 H43A 109.1 . . ?
N4 C43 H43A 109.1 . . ?
C44 C43 H43B 109.1 . . ?
N4 C43 H43B 109.1 . . ?
H43A C43 H43B 107.8 . . ?
C43 C44 N1 110.7(6) . . ?
C43 C44 H44A 109.5 . . ?
N1 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
N1 C44 H44B 109.5 . . ?
H44A C44 H44B 108.1 . . ?
O1A Li1 N4 106.3(4) . . ?
O1A Li1 N3 109.6(4) . . ?
N4 Li1 N3 84.7(3) . . ?
O1A Li1 N1 111.6(4) . . ?
N4 Li1 N1 82.6(3) . . ?
N3 Li1 N1 138.8(4) . . ?
O1A Li1 N2 113.7(4) . . ?
N4 Li1 N2 140.0(4) . . ?
N3 Li1 N2 82.1(3) . . ?
N1 Li1 N2 82.9(3) . . ?
C1 B1 C9 107.8(3) . . ?
C1 B1 C17 112.1(3) . . ?
C9 B1 C17 107.9(3) . . ?
C1 B1 C25 108.1(3) . . ?
C9 B1 C25 112.8(3) . . ?
C17 B1 C25 108.3(3) . . ?
C44 N1 C33 111.4(5) . . ?
C44 N1 C34 111.4(5) . . ?
C33 N1 C34 110.4(5) . . ?
C44 N1 Li1 102.6(4) . . ?
C33 N1 Li1 117.1(4) . . ?
C34 N1 Li1 103.5(4) . . ?
C35 N2 C36 114.4(5) . . ?
C35 N2 C37 109.3(5) . . ?
C36 N2 C37 107.7(5) . . ?
C35 N2 Li1 102.8(4) . . ?
C36 N2 Li1 119.1(5) . . ?
C37 N2 Li1 102.8(3) . . ?
C38 N3 C39 110.9(5) . . ?
C38 N3 C40 112.6(6) . . ?
C39 N3 C40 108.5(4) . . ?
C38 N3 Li1 104.5(4) . . ?
C39 N3 Li1 117.9(4) . . ?
C40 N3 Li1 102.3(4) . . ?
C41 N4 C42 106.9(7) . . ?
C41 N4 C43 112.4(6) . . ?
C42 N4 C43 110.6(5) . . ?
C41 N4 Li1 102.6(4) . . ?
C42 N4 Li1 119.5(6) . . ?
C43 N4 Li1 104.7(4) . . ?

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
C6 C1 C2 C3 -0.6(6) . . . . ?
B1 C1 C2 C3 174.6(4) . . . . ?
C1 C2 C3 C4 0.8(6) . . . . ?
C1 C2 C3 C7 -179.4(4) . . . . ?
C2 C3 C4 C5 0.0(7) . . . . ?
C7 C3 C4 C5 -179.9(4) . . . . ?
C3 C4 C5 C6 -0.8(6) . . . . ?
C3 C4 C5 C8 179.3(4) . . . . ?
C2 C1 C6 C5 -0.3(5) . . . . ?
B1 C1 C6 C5 -175.5(4) . . . . ?
C4 C5 C6 C1 1.0(6) . . . . ?
C8 C5 C6 C1 -179.1(4) . . . . ?
C4 C3 C7 F3B 174.6(18) . . . . ?
C2 C3 C7 F3B -5.3(19) . . . . ?
C4 C3 C7 F3A -26.7(12) . . . . ?
C2 C3 C7 F3A 153.4(10) . . . . ?
C4 C3 C7 F2B 45.9(11) . . . . ?
C2 C3 C7 F2B -134.0(10) . . . . ?
C4 C3 C7 F2A -153.3(8) . . . . ?
C2 C3 C7 F2A 26.9(9) . . . . ?
C4 C3 C7 F1B -62.9(10) . . . . ?
C2 C3 C7 F1B 117.3(10) . . . . ?
C4 C3 C7 F1A 95.4(8) . . . . ?
C2 C3 C7 F1A -84.5(8) . . . . ?
C6 C5 C8 F5A -174.4(8) . . . . ?
C4 C5 C8 F5A 5.5(10) . . . . ?
C6 C5 C8 F5B -16.7(13) . . . . ?
C4 C5 C8 F5B 163.1(12) . . . . ?
C6 C5 C8 F6B 114.3(13) . . . . ?
C4 C5 C8 F6B -65.8(13) . . . . ?
C6 C5 C8 F4B -135.1(10) . . . . ?
C4 C5 C8 F4B 44.8(11) . . . . ?
C6 C5 C8 F6A -51.2(8) . . . . ?
C4 C5 C8 F6A 128.7(7) . . . . ?
C6 C5 C8 F4A 62.2(7) . . . . ?
C4 C5 C8 F4A -117.9(6) . . . . ?
C14 C9 C10 C11 0.7(5) . . . . ?
B1 C9 C10 C11 -172.5(3) . . . . ?
C9 C10 C11 C12 -1.3(5) . . . . ?
C9 C10 C11 C15 178.2(3) . . . . ?
C10 C11 C12 C13 0.8(5) . . . . ?
C15 C11 C12 C13 -178.7(3) . . . . ?
C11 C12 C13 C14 0.3(5) . . . . ?
C11 C12 C13 C16 -179.1(4) . . . . ?
C12 C13 C14 C9 -0.9(6) . . . . ?
C16 C13 C14 C9 178.5(4) . . . . ?
C10 C9 C14 C13 0.4(5) . . . . ?
B1 C9 C14 C13 173.3(3) . . . . ?
C12 C11 C15 F8 115.6(5) . . . . ?
C10 C11 C15 F8 -63.9(5) . . . . ?
C12 C11 C15 F7 -4.9(5) . . . . ?
C10 C11 C15 F7 175.6(3) . . . . ?
C12 C11 C15 F9 -125.6(4) . . . . ?
C10 C11 C15 F9 54.9(5) . . . . ?
C14 C13 C16 F10A 14.7(12) . . . . ?
C12 C13 C16 F10A -165.9(11) . . . . ?
C14 C13 C16 F11B -59.1(8) . . . . ?
C12 C13 C16 F11B 120.3(8) . . . . ?
C14 C13 C16 F12A -109.8(10) . . . . ?
C12 C13 C16 F12A 69.5(10) . . . . ?
C14 C13 C16 F10B 174.2(8) . . . . ?
C12 C13 C16 F10B -6.4(9) . . . . ?
C14 C13 C16 F11A 134.3(8) . . . . ?
C12 C13 C16 F11A -46.4(9) . . . . ?
C14 C13 C16 F12B 55.9(7) . . . . ?
C12 C13 C16 F12B -124.8(7) . . . . ?
C22 C17 C18 C19 -0.5(5) . . . . ?
B1 C17 C18 C19 -175.4(4) . . . . ?
C17 C18 C19 C20 1.6(6) . . . . ?
C17 C18 C19 C23 -179.1(4) . . . . ?
C18 C19 C20 C21 -1.1(6) . . . . ?
C23 C19 C20 C21 179.6(4) . . . . ?
C19 C20 C21 C22 -0.4(6) . . . . ?
C19 C20 C21 C24 -178.4(4) . . . . ?
C20 C21 C22 C17 1.5(6) . . . . ?
C24 C21 C22 C17 179.5(4) . . . . ?
C18 C17 C22 C21 -1.0(6) . . . . ?
B1 C17 C22 C21 173.9(4) . . . . ?
C18 C19 C23 F14A 52.5(8) . . . . ?
C20 C19 C23 F14A -128.2(7) . . . . ?
C18 C19 C23 F15A -177.1(6) . . . . ?
C20 C19 C23 F15A 2.2(8) . . . . ?
C18 C19 C23 F15B 21.5(14) . . . . ?
C20 C19 C23 F15B -159.2(13) . . . . ?
C18 C19 C23 F14B -109.5(14) . . . . ?
C20 C19 C23 F14B 69.8(14) . . . . ?
C18 C19 C23 F13B 128.6(11) . . . . ?
C20 C19 C23 F13B -52.1(12) . . . . ?
C18 C19 C23 F13A -60.5(6) . . . . ?
C20 C19 C23 F13A 118.8(5) . . . . ?
C22 C21 C24 F17 162.5(5) . . . . ?
C20 C21 C24 F17 -19.5(7) . . . . ?
C22 C21 C24 F16 33.4(7) . . . . ?
C20 C21 C24 F16 -148.6(5) . . . . ?
C22 C21 C24 F18 -80.2(6) . . . . ?
C20 C21 C24 F18 97.8(5) . . . . ?
C30 C25 C26 C27 0.8(5) . . . . ?
B1 C25 C26 C27 178.6(3) . . . . ?
C25 C26 C27 C28 -1.1(6) . . . . ?
C25 C26 C27 C31 174.6(4) . . . . ?
C26 C27 C28 C29 0.4(6) . . . . ?
C31 C27 C28 C29 -175.2(4) . . . . ?
C27 C28 C29 C30 0.5(6) . . . . ?
C27 C28 C29 C32 179.4(4) . . . . ?
C26 C25 C30 C29 0.1(5) . . . . ?
B1 C25 C30 C29 -177.7(3) . . . . ?
C28 C29 C30 C25 -0.8(6) . . . . ?
C32 C29 C30 C25 -179.7(4) . . . . ?
C28 C27 C31 F20 87.7(6) . . . . ?
C26 C27 C31 F20 -88.0(6) . . . . ?
C28 C27 C31 F19 -150.0(4) . . . . ?
C26 C27 C31 F19 34.3(6) . . . . ?
C28 C27 C31 F21 -31.1(7) . . . . ?
C26 C27 C31 F21 153.2(4) . . . . ?
C28 C29 C32 F22 -4.7(7) . . . . ?
C30 C29 C32 F22 174.2(4) . . . . ?
C28 C29 C32 F24 119.8(5) . . . . ?
C30 C29 C32 F24 -61.3(6) . . . . ?
C28 C29 C32 F23 -123.3(5) . . . . ?
C30 C29 C32 F23 55.6(6) . . . . ?
N1 C34 C35 N2 59.4(7) . . . . ?
N2 C37 C38 N3 55.7(7) . . . . ?
N3 C40 C41 N4 54.0(10) . . . . ?
N4 C43 C44 N1 57.5(7) . . . . ?
C6 C1 B1 C9 -157.3(3) . . . . ?
C2 C1 B1 C9 27.8(4) . . . . ?
C6 C1 B1 C17 -38.8(5) . . . . ?
C2 C1 B1 C17 146.3(3) . . . . ?
C6 C1 B1 C25 80.5(4) . . . . ?
C2 C1 B1 C25 -94.4(4) . . . . ?
C10 C9 B1 C1 81.7(4) . . . . ?
C14 C9 B1 C1 -90.8(4) . . . . ?
C10 C9 B1 C17 -39.6(4) . . . . ?
C14 C9 B1 C17 148.0(3) . . . . ?
C10 C9 B1 C25 -159.1(3) . . . . ?
C14 C9 B1 C25 28.4(4) . . . . ?
C22 C17 B1 C1 156.8(3) . . . . ?
C18 C17 B1 C1 -28.6(5) . . . . ?
C22 C17 B1 C9 -84.7(4) . . . . ?
C18 C17 B1 C9 89.8(4) . . . . ?
C22 C17 B1 C25 37.7(5) . . . . ?
C18 C17 B1 C25 -147.8(3) . . . . ?
C30 C25 B1 C1 -30.8(4) . . . . ?
C26 C25 B1 C1 151.5(3) . . . . ?
C30 C25 B1 C9 -149.8(3) . . . . ?
C26 C25 B1 C9 32.5(5) . . . . ?
C30 C25 B1 C17 90.9(4) . . . . ?
C26 C25 B1 C17 -86.8(4) . . . . ?
C43 C44 N1 C33 73.9(6) . . . . ?
C43 C44 N1 C34 -162.4(5) . . . . ?
C43 C44 N1 Li1 -52.2(6) . . . . ?
C35 C34 N1 C44 79.7(6) . . . . ?
C35 C34 N1 C33 -156.0(6) . . . . ?
C35 C34 N1 Li1 -29.8(6) . . . . ?
C34 C35 N2 C36 77.7(6) . . . . ?
C34 C35 N2 C37 -161.5(5) . . . . ?
C34 C35 N2 Li1 -52.8(6) . . . . ?
C38 C37 N2 C35 81.7(6) . . . . ?
C38 C37 N2 C36 -153.5(6) . . . . ?
C38 C37 N2 Li1 -27.0(6) . . . . ?
C37 C38 N3 C39 77.0(6) . . . . ?
C37 C38 N3 C40 -161.3(5) . . . . ?
C37 C38 N3 Li1 -51.1(6) . . . . ?
C41 C40 N3 C38 85.0(8) . . . . ?
C41 C40 N3 C39 -151.9(7) . . . . ?
C41 C40 N3 Li1 -26.6(9) . . . . ?
C40 C41 N4 C42 79.0(8) . . . . ?
C40 C41 N4 C43 -159.5(6) . . . . ?
C40 C41 N4 Li1 -47.6(7) . . . . ?
C44 C43 N4 C41 82.1(7) . . . . ?
C44 C43 N4 C42 -158.5(8) . . . . ?
C44 C43 N4 Li1 -28.5(7) . . . . ?

_refine_diff_density_max         1.357
_refine_diff_density_min         -0.679
_refine_diff_density_rms         0.091

_shelxl_version_number           2013-4

_exptl_crystal_recrystallization_method 'Layering: CH2Cl2/hexane'
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
####################################################################### 
# 
# 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_[Na(Me~4~cyclen)(thf)][BArF]
_database_code_depnum_ccdc_archive 'CCDC 1051104'
_audit_update_record             
;
2015-02-24 deposited with the CCDC.
2015-06-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H12 B F24, C16 H36 N4 Na O'
_chemical_formula_sum            'C48 H48 B F24 N4 Na O'
_chemical_formula_weight         1186.70

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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 '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'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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, -z'

_cell_length_a                   12.7958(9)
_cell_length_b                   12.8488(9)
_cell_length_c                   18.2627(13)
_cell_angle_alpha                89.433(4)
_cell_angle_beta                 79.005(4)
_cell_angle_gamma                64.414(3)
_cell_volume                     2649.5(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    25098
_cell_measurement_theta_min      2.3
_cell_measurement_theta_max      27.5

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.487
_exptl_crystal_F_000             1208
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    0.155
_shelx_estimated_absorpt_T_min   0.988
_shelx_estimated_absorpt_T_max   0.991
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.725
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'CrystalClear-SM Expert 3.1 b27 (Rigaku, 2012)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_source_power             2.475
_diffrn_source_voltage           45.0
_diffrn_source_current           55.0
_diffrn_source                   'Rotating Anode'

_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_radiation_collimation    'Confocal mirrors, VHF Varimax '

_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_detector_area_resol_mean 28.5714

_diffrn_measurement_device       'four-circle κ diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC12 (Right)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_reflns_number            26141
_diffrn_reflns_av_unetI/netI     0.0502
_diffrn_reflns_av_R_equivalents  0.0481
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.995
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.975
_reflns_number_total             9344
_reflns_number_gt                6523
_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       
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 2012)
;
_computing_cell_refinement       
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 2012)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 2012)
;
_computing_structure_solution    'SUPERFLIP (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'ORTEP-III (Farrugia, 2012)'
_computing_publication_material  
'PLATON (Spek, 2003), WinGX (Farrugia, 1999) and enCIFer (Allen et al., 2004).'

_refine_special_details          
;
Four of the CF3 groups were refined to account for rotational disorder 
with an isotropic thermal parameter restraint of 0.005 applied to some 
of the disordered fluorines. 

The macrocycle contained positional disorder of the ethylene linkers. 
Initial refinement cycles led to the two orientations of each ethylene 
group converging to exactly 50% occupancy hence this value was fixed 
for final refinement cycles.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1048P)²+3.5170P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9344
_refine_ls_number_parameters     899
_refine_ls_number_restraints     1454
_refine_ls_R_factor_all          0.1086
_refine_ls_R_factor_gt           0.0784
_refine_ls_wR_factor_ref         0.2249
_refine_ls_wR_factor_gt          0.2019
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_restrained_S_all      1.462
_refine_ls_shift/su_max          0.001
_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
C1 C -0.0120(3) 0.5485(3) 0.21691(18) 0.0267(7) Uani 1 1 d . U . . .
C2 C -0.0464(3) 0.5310(3) 0.15119(19) 0.0299(7) Uani 1 1 d . U . . .
H2 H 0.0131 0.4940 0.1076 0.036 Uiso 1 1 calc R U . . .
C3 C -0.1637(3) 0.5658(3) 0.14761(19) 0.0334(8) Uani 1 1 d . U . . .
C4 C -0.2543(3) 0.6227(3) 0.2089(2) 0.0371(8) Uani 1 1 d . U . . .
H4 H -0.3348 0.6468 0.2063 0.045 Uiso 1 1 calc R U . . .
C5 C -0.2234(3) 0.6436(3) 0.27455(19) 0.0346(8) Uani 1 1 d . U . . .
C6 C -0.1048(3) 0.6055(3) 0.27797(19) 0.0306(7) Uani 1 1 d . U . . .
H6 H -0.0862 0.6189 0.3239 0.037 Uiso 1 1 calc R U . . .
C7 C -0.1943(4) 0.5454(4) 0.0752(2) 0.0448(9) Uani 1 1 d . U . . .
C8 C -0.3164(4) 0.7038(4) 0.3422(2) 0.0527(11) Uani 1 1 d . U . . .
C9 C 0.1459(3) 0.4762(3) 0.30533(18) 0.0278(7) Uani 1 1 d . U . . .
C10 C 0.1220(3) 0.5568(3) 0.36500(19) 0.0329(8) Uani 1 1 d . U . . .
H10 H 0.0949 0.6363 0.3561 0.039 Uiso 1 1 calc R U . . .
C11 C 0.1367(3) 0.5242(3) 0.4366(2) 0.0388(8) Uani 1 1 d . U . . .
C12 C 0.1733(4) 0.4101(4) 0.4528(2) 0.0419(9) Uani 1 1 d . U . . .
H12 H 0.1828 0.3880 0.5018 0.050 Uiso 1 1 calc R U . . .
C13 C 0.1957(3) 0.3293(3) 0.3955(2) 0.0398(9) Uani 1 1 d . U . . .
C14 C 0.1826(3) 0.3618(3) 0.3237(2) 0.0344(8) Uani 1 1 d . U . . .
H14 H 0.1993 0.3037 0.2856 0.041 Uiso 1 1 calc R U . . .
C15 C 0.1202(4) 0.6123(4) 0.4953(2) 0.0548(11) Uani 1 1 d . U . . .
C16 C 0.2378(5) 0.2032(4) 0.4089(3) 0.0574(12) Uani 1 1 d . U . . .
C17 C 0.2201(3) 0.4050(3) 0.16007(18) 0.0277(7) Uani 1 1 d . U . . .
C18 C 0.3293(3) 0.3976(3) 0.1230(2) 0.0344(8) Uani 1 1 d . U . . .
H18 H 0.3473 0.4608 0.1297 0.041 Uiso 1 1 calc R U . . .
C19 C 0.4131(3) 0.3003(3) 0.0762(2) 0.0406(9) Uani 1 1 d . U . . .
C20 C 0.3901(4) 0.2070(3) 0.0643(2) 0.0445(9) Uani 1 1 d . U . . .
H20 H 0.4469 0.1410 0.0324 0.053 Uiso 1 1 calc R U . . .
C21 C 0.2817(4) 0.2122(3) 0.1002(2) 0.0390(8) Uani 1 1 d . U . . .
C22 C 0.1986(3) 0.3095(3) 0.14653(19) 0.0327(8) Uani 1 1 d . U . . .
H22 H 0.1248 0.3112 0.1698 0.039 Uiso 1 1 calc R U . . .
C23 C 0.5300(4) 0.2974(4) 0.0400(3) 0.0615(12) Uani 1 1 d . U . . .
C24 C 0.2506(4) 0.1145(4) 0.0906(3) 0.0583(11) Uani 1 1 d D U . . .
C25 C 0.1535(3) 0.6265(3) 0.19987(17) 0.0249(7) Uani 1 1 d . U . . .
C26 C 0.1045(3) 0.6976(3) 0.14502(18) 0.0270(7) Uani 1 1 d . U . . .
H26 H 0.0478 0.6857 0.1238 0.032 Uiso 1 1 calc R U . . .
C27 C 0.1361(3) 0.7852(3) 0.12042(18) 0.0290(7) Uani 1 1 d . U . . .
C28 C 0.2167(3) 0.8070(3) 0.15088(19) 0.0306(7) Uani 1 1 d . U . . .
H28 H 0.2372 0.8675 0.1349 0.037 Uiso 1 1 calc R U . . .
C29 C 0.2664(3) 0.7378(3) 0.2055(2) 0.0312(7) Uani 1 1 d . U . . .
C30 C 0.2359(3) 0.6492(3) 0.22849(19) 0.0302(7) Uani 1 1 d . U . . .
H30 H 0.2726 0.6023 0.2652 0.036 Uiso 1 1 calc R U . . .
C31 C 0.0842(4) 0.8554(3) 0.0599(2) 0.0423(9) Uani 1 1 d . U . . .
C32 C 0.3528(4) 0.7586(4) 0.2404(3) 0.0470(10) Uani 1 1 d . U . . .
C33 C 0.8594(5) 0.2218(5) 0.1694(3) 0.0737(15) Uani 1 1 d . U . . .
H33A H 0.9087 0.2620 0.1533 0.111 Uiso 1 1 calc R U . . .
H33B H 0.7854 0.2594 0.1513 0.111 Uiso 1 1 calc R U . . .
H33C H 0.9019 0.1408 0.1489 0.111 Uiso 1 1 calc R U . . .
C34 C 0.9636(4) -0.0880(4) 0.3277(3) 0.0568(12) Uani 1 1 d . U . . .
H34A H 1.0367 -0.1176 0.3470 0.085 Uiso 1 1 calc R U . . .
H34B H 0.9832 -0.0966 0.2729 0.085 Uiso 1 1 calc R U . . .
H34C H 0.9188 -0.1318 0.3460 0.085 Uiso 1 1 calc R U . . .
C35 C 0.5778(4) 0.0812(4) 0.4724(3) 0.0554(12) Uani 1 1 d . U . . .
H35A H 0.6248 -0.0005 0.4541 0.083 Uiso 1 1 calc R U . . .
H35B H 0.5026 0.1116 0.4555 0.083 Uiso 1 1 calc R U . . .
H35C H 0.5621 0.0883 0.5273 0.083 Uiso 1 1 calc R U . . .
C36 C 0.4730(4) 0.3861(5) 0.3130(3) 0.0675(14) Uani 1 1 d . U . . .
H36A H 0.4267 0.4677 0.3317 0.101 Uiso 1 1 calc R U . . .
H36B H 0.4277 0.3428 0.3313 0.101 Uiso 1 1 calc R U . . .
H36C H 0.4902 0.3798 0.2581 0.101 Uiso 1 1 calc R U . . .
C37A C 0.9175(11) 0.2141(10) 0.2901(6) 0.071(2) Uani 0.5 1 d D U P A 1
H37A H 0.8821 0.2626 0.3382 0.085 Uiso 0.5 1 calc R U P A 1
H37B H 0.9775 0.2359 0.2608 0.085 Uiso 0.5 1 calc R U P A 1
C38A C 0.9718(8) 0.0873(8) 0.3031(8) 0.064(3) Uani 0.5 1 d D U P A 1
H38A H 1.0404 0.0720 0.3264 0.077 Uiso 0.5 1 calc R U P A 1
H38B H 1.0037 0.0434 0.2534 0.077 Uiso 0.5 1 calc R U P A 1
C39A C 0.8796(8) 0.0751(9) 0.4250(5) 0.061(2) Uani 0.5 1 d D U P A 1
H39A H 0.8715 0.1553 0.4256 0.073 Uiso 0.5 1 calc R U P A 1
H39B H 0.9487 0.0262 0.4466 0.073 Uiso 0.5 1 calc R U P A 1
C40A C 0.7677(9) 0.0720(11) 0.4687(6) 0.057(2) Uani 0.5 1 d D U P A 1
H40A H 0.7579 0.0978 0.5215 0.068 Uiso 0.5 1 calc R U P A 1
H40B H 0.7810 -0.0099 0.4676 0.068 Uiso 0.5 1 calc R U P A 1
C41A C 0.6090(11) 0.2575(7) 0.4790(5) 0.063(2) Uani 0.5 1 d D U P A 1
H41A H 0.6786 0.2720 0.4803 0.076 Uiso 0.5 1 calc R U P A 1
H41B H 0.5633 0.2660 0.5306 0.076 Uiso 0.5 1 calc R U P A 1
C42A C 0.5321(10) 0.3381(11) 0.4288(6) 0.070(3) Uani 0.5 1 d D U P A 1
H42A H 0.5024 0.4180 0.4514 0.085 Uiso 0.5 1 calc R U P A 1
H42B H 0.4623 0.3220 0.4326 0.085 Uiso 0.5 1 calc R U P A 1
C43A C 0.6472(8) 0.4002(8) 0.3447(7) 0.072(3) Uani 0.5 1 d D U P A 1
H43A H 0.6875 0.3790 0.3875 0.086 Uiso 0.5 1 calc R U P A 1
H43B H 0.5967 0.4848 0.3493 0.086 Uiso 0.5 1 calc R U P A 1
C44A C 0.7358(13) 0.3606(9) 0.2699(7) 0.079(3) Uani 0.5 1 d D U P A 1
H44A H 0.7800 0.4081 0.2653 0.095 Uiso 0.5 1 calc R U P A 1
H44B H 0.6894 0.3808 0.2300 0.095 Uiso 0.5 1 calc R U P A 1
C37B C 0.9613(7) 0.1413(9) 0.2701(5) 0.0434(19) Uani 0.5 1 d D U P A 2
H37C H 0.9996 0.0712 0.2347 0.052 Uiso 0.5 1 calc R U P A 2
H37D H 1.0127 0.1817 0.2628 0.052 Uiso 0.5 1 calc R U P A 2
C38B C 0.9503(7) 0.1041(7) 0.3522(4) 0.0359(17) Uani 0.5 1 d D U P A 2
H38C H 1.0295 0.0614 0.3644 0.043 Uiso 0.5 1 calc R U P A 2
H38D H 0.9031 0.1725 0.3886 0.043 Uiso 0.5 1 calc R U P A 2
C39B C 0.8424(7) 0.0239(6) 0.4387(4) 0.0305(15) Uani 0.5 1 d D U P A 2
H39C H 0.8180 -0.0397 0.4421 0.037 Uiso 0.5 1 calc R U P A 2
H39D H 0.9058 0.0049 0.4673 0.037 Uiso 0.5 1 calc R U P A 2
C40B C 0.7336(7) 0.1397(7) 0.4748(4) 0.0344(17) Uani 0.5 1 d D U P A 2
H40C H 0.7135 0.1378 0.5298 0.041 Uiso 0.5 1 calc R U P A 2
H40D H 0.7512 0.2068 0.4640 0.041 Uiso 0.5 1 calc R U P A 2
C41B C 0.5400(7) 0.2790(7) 0.4561(5) 0.0350(16) Uani 0.5 1 d D U P A 2
H41C H 0.4694 0.2814 0.4401 0.042 Uiso 0.5 1 calc R U P A 2
H41D H 0.5172 0.3044 0.5101 0.042 Uiso 0.5 1 calc R U P A 2
C42B C 0.5799(7) 0.3644(6) 0.4119(4) 0.0395(18) Uani 0.5 1 d D U P A 2
H42C H 0.5226 0.4457 0.4285 0.047 Uiso 0.5 1 calc R U P A 2
H42D H 0.6590 0.3523 0.4189 0.047 Uiso 0.5 1 calc R U P A 2
C43B C 0.6621(7) 0.3940(7) 0.2867(5) 0.0385(17) Uani 0.5 1 d D U P A 2
H43C H 0.6553 0.3870 0.2341 0.046 Uiso 0.5 1 calc R U P A 2
H43D H 0.6301 0.4773 0.3025 0.046 Uiso 0.5 1 calc R U P A 2
C44B C 0.7943(7) 0.3328(7) 0.2916(5) 0.0445(19) Uani 0.5 1 d D U P A 2
H44C H 0.8377 0.3765 0.2684 0.053 Uiso 0.5 1 calc R U P A 2
H44D H 0.8036 0.3222 0.3442 0.053 Uiso 0.5 1 calc R U P A 2
C45 C 0.5578(6) 0.0255(7) 0.2161(4) 0.105(2) Uani 1 1 d . U . . .
H45A H 0.5030 0.1020 0.2030 0.126 Uiso 1 1 calc R U . . .
H45B H 0.5160 0.0037 0.2605 0.126 Uiso 1 1 calc R U . . .
C46 C 0.5986(6) -0.0637(6) 0.1517(3) 0.0830(17) Uani 1 1 d . U . . .
H46A H 0.5536 -0.0322 0.1117 0.100 Uiso 1 1 calc R U . . .
H46B H 0.5891 -0.1334 0.1681 0.100 Uiso 1 1 calc R U . . .
C47 C 0.7268(7) -0.0916(8) 0.1250(5) 0.124(3) Uani 1 1 d . U . . .
H47A H 0.7735 -0.1742 0.1065 0.149 Uiso 1 1 calc R U . . .
H47B H 0.7368 -0.0434 0.0841 0.149 Uiso 1 1 calc R U . . .
C48 C 0.7619(8) -0.0675(9) 0.1860(5) 0.145(3) Uani 1 1 d . U . . .
H48A H 0.8287 -0.0473 0.1701 0.174 Uiso 1 1 calc R U . . .
H48B H 0.7884 -0.1360 0.2154 0.174 Uiso 1 1 calc R U . . .
B1 B 0.1265(3) 0.5141(3) 0.2205(2) 0.0263(8) Uani 1 1 d . U . . .
N1 N 0.8327(4) 0.2265(4) 0.2511(2) 0.0668(11) Uani 1 1 d D U . . .
N2 N 0.8930(3) 0.0327(3) 0.3530(2) 0.0493(8) Uani 1 1 d D U . . .
N3 N 0.6432(3) 0.1470(3) 0.4432(2) 0.0526(9) Uani 1 1 d D U . . .
N4 N 0.5831(3) 0.3390(3) 0.3393(3) 0.0655(10) Uani 1 1 d D U . . .
O1 O 0.6615(3) 0.0295(4) 0.2315(2) 0.0879(13) Uani 1 1 d . U . . .
F1 F -0.1196(3) 0.4439(3) 0.03917(16) 0.0814(9) Uani 1 1 d . U . . .
F2 F -0.1820(4) 0.6175(3) 0.02577(16) 0.0914(11) Uani 1 1 d . U . . .
F3 F -0.2985(3) 0.5516(5) 0.08242(17) 0.1312(17) Uani 1 1 d . U . . .
F4 F -0.4255(2) 0.7502(3) 0.33066(14) 0.0678(8) Uani 1 1 d . U . . .
F5 F -0.3155(3) 0.6331(4) 0.39653(15) 0.0962(12) Uani 1 1 d . U . . .
F6 F -0.2999(3) 0.7864(3) 0.37445(19) 0.1007(13) Uani 1 1 d . U . . .
F7 F 0.0360(4) 0.7174(3) 0.48914(16) 0.0936(11) Uani 1 1 d . U . . .
F8 F 0.0902(3) 0.5883(3) 0.56511(13) 0.0652(7) Uani 1 1 d . U . . .
F9 F 0.2212(3) 0.6215(3) 0.49345(16) 0.0919(11) Uani 1 1 d . U . . .
F10 F 0.2383(4) 0.1836(3) 0.47984(18) 0.0942(11) Uani 1 1 d . U . . .
F11 F 0.3510(3) 0.1401(3) 0.3720(2) 0.0932(11) Uani 1 1 d . U . . .
F12 F 0.1746(3) 0.1565(2) 0.38456(16) 0.0696(8) Uani 1 1 d . U . . .
F13A F 0.6140(5) 0.1992(4) 0.0132(5) 0.092(3) Uani 0.666(12) 1 d . U P B 1
F14A F 0.5225(6) 0.3669(8) -0.0192(5) 0.104(3) Uani 0.666(12) 1 d . U P B 1
F15A F 0.5727(5) 0.3477(8) 0.0826(4) 0.098(3) Uani 0.666(12) 1 d . U P B 1
F16A F 0.1505(8) 0.1436(13) 0.0676(9) 0.076(3) Uani 0.64(4) 1 d . U P C 1
F17A F 0.2369(18) 0.0705(13) 0.1582(6) 0.086(4) Uani 0.64(4) 1 d . U P C 1
F18A F 0.3414(14) 0.0262(11) 0.0476(9) 0.089(4) Uani 0.64(4) 1 d . U P C 1
F19A F 0.1376(10) 0.7884(6) -0.0060(4) 0.097(2) Uani 0.5 1 d . U P D 1
F20A F 0.1083(6) 0.9435(5) 0.0484(3) 0.0472(12) Uani 0.5 1 d . U P D 1
F21A F -0.0285(7) 0.8962(10) 0.0739(6) 0.106(3) Uani 0.5 1 d . U P D 1
F22A F 0.4549(4) 0.6585(4) 0.2347(5) 0.081(2) Uani 0.774(12) 1 d . U P E 1
F23A F 0.3886(7) 0.8314(6) 0.2093(5) 0.090(2) Uani 0.774(12) 1 d . U P E 1
F24A F 0.3183(6) 0.7830(10) 0.3129(3) 0.104(3) Uani 0.774(12) 1 d . U P E 1
F13B F 0.5247(12) 0.3882(10) 0.0286(11) 0.086(4) Uani 0.334(12) 1 d . U P B 2
F14B F 0.6062(9) 0.2314(18) 0.0831(10) 0.125(7) Uani 0.334(12) 1 d . U P B 2
F15B F 0.5618(13) 0.2386(14) -0.0265(8) 0.094(4) Uani 0.334(12) 1 d . U P B 2
F16B F 0.178(3) 0.142(3) 0.041(2) 0.105(7) Uani 0.36(4) 1 d D U P C 2
F17B F 0.193(3) 0.087(2) 0.1504(13) 0.098(7) Uani 0.36(4) 1 d D U P C 2
F18B F 0.336(2) 0.0164(16) 0.0530(11) 0.056(4) Uani 0.36(4) 1 d D U P C 2
F19B F 0.0173(9) 0.9674(5) 0.0839(4) 0.095(2) Uani 0.5 1 d . U P D 2
F20B F 0.0168(7) 0.8256(6) 0.0288(4) 0.0621(18) Uani 0.5 1 d . U P D 2
F21B F 0.1621(6) 0.8610(10) 0.0035(5) 0.099(2) Uani 0.5 1 d . U P D 2
F22B F 0.3045(14) 0.8635(16) 0.2761(16) 0.088(7) Uani 0.226(12) 1 d . U P E 2
F23B F 0.404(2) 0.686(2) 0.2834(14) 0.082(5) Uani 0.226(12) 1 d . U P E 2
F24B F 0.4361(19) 0.766(3) 0.1907(12) 0.093(7) Uani 0.226(12) 1 d . U P E 2
Na1 Na 0.70849(13) 0.13211(13) 0.30682(8) 0.0417(4) Uani 1 1 d . U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C6 1.396(5) . ?
C1 C2 1.406(5) . ?
C1 B1 1.646(5) . ?
C2 C3 1.383(5) . ?
C2 H2 0.9500 . ?
C3 C4 1.387(5) . ?
C3 C7 1.505(5) . ?
C4 C5 1.393(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.393(5) . ?
C5 C8 1.485(5) . ?
C6 H6 0.9500 . ?
C7 F3 1.282(5) . ?
C7 F1 1.322(5) . ?
C7 F2 1.323(5) . ?
C8 F4 1.318(5) . ?
C8 F6 1.330(5) . ?
C8 F5 1.337(6) . ?
C9 C14 1.396(5) . ?
C9 C10 1.406(5) . ?
C9 B1 1.651(5) . ?
C10 C11 1.392(5) . ?
C10 H10 0.9500 . ?
C11 C12 1.381(5) . ?
C11 C15 1.485(6) . ?
C12 C13 1.380(6) . ?
C12 H12 0.9500 . ?
C13 C14 1.392(5) . ?
C13 C16 1.505(6) . ?
C14 H14 0.9500 . ?
C15 F8 1.332(5) . ?
C15 F7 1.335(6) . ?
C15 F9 1.343(5) . ?
C16 F10 1.317(5) . ?
C16 F12 1.331(5) . ?
C16 F11 1.354(6) . ?
C17 C18 1.395(5) . ?
C17 C22 1.402(5) . ?
C17 B1 1.641(5) . ?
C18 C19 1.399(5) . ?
C18 H18 0.9500 . ?
C19 C20 1.380(6) . ?
C19 C23 1.500(6) . ?
C20 C21 1.390(6) . ?
C20 H20 0.9500 . ?
C21 C22 1.393(5) . ?
C21 C24 1.492(6) . ?
C22 H22 0.9500 . ?
C23 F13B 1.158(13) . ?
C23 F13A 1.276(6) . ?
C23 F15B 1.333(13) . ?
C23 F15A 1.340(7) . ?
C23 F14B 1.361(13) . ?
C23 F14A 1.387(8) . ?
C24 F16A 1.321(11) . ?
C24 F17B 1.331(10) . ?
C24 F18A 1.336(10) . ?
C24 F18B 1.341(10) . ?
C24 F16B 1.352(10) . ?
C24 F17A 1.365(10) . ?
C25 C30 1.396(5) . ?
C25 C26 1.399(5) . ?
C25 B1 1.647(5) . ?
C26 C27 1.395(4) . ?
C26 H26 0.9500 . ?
C27 C28 1.387(5) . ?
C27 C31 1.489(5) . ?
C28 C29 1.388(5) . ?
C28 H28 0.9500 . ?
C29 C30 1.392(5) . ?
C29 C32 1.492(5) . ?
C30 H30 0.9500 . ?
C31 F21A 1.277(8) . ?
C31 F20A 1.300(6) . ?
C31 F20B 1.300(6) . ?
C31 F21B 1.314(7) . ?
C31 F19B 1.342(7) . ?
C31 F19A 1.363(8) . ?
C32 F23B 1.250(17) . ?
C32 F23A 1.292(6) . ?
C32 F24B 1.301(19) . ?
C32 F24A 1.308(6) . ?
C32 F22B 1.330(14) . ?
C32 F22A 1.368(6) . ?
C33 N1 1.461(6) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 N2 1.442(5) . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 N3 1.461(5) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 N4 1.449(6) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37A N1 1.362(10) . ?
C37A C38A 1.507(11) . ?
C37A H37A 0.9900 . ?
C37A H37B 0.9900 . ?
C38A N2 1.609(10) . ?
C38A H38A 0.9900 . ?
C38A H38B 0.9900 . ?
C39A N2 1.378(8) . ?
C39A C40A 1.518(11) . ?
C39A H39A 0.9900 . ?
C39A H39B 0.9900 . ?
C40A N3 1.622(10) . ?
C40A H40A 0.9900 . ?
C40A H40B 0.9900 . ?
C41A N3 1.417(8) . ?
C41A C42A 1.524(11) . ?
C41A H41A 0.9900 . ?
C41A H41B 0.9900 . ?
C42A N4 1.642(11) . ?
C42A H42A 0.9900 . ?
C42A H42B 0.9900 . ?
C43A N4 1.376(9) . ?
C43A C44A 1.527(12) . ?
C43A H43A 0.9900 . ?
C43A H43B 0.9900 . ?
C44A N1 1.621(11) . ?
C44A H44A 0.9900 . ?
C44A H44B 0.9900 . ?
C37B C38B 1.568(9) . ?
C37B N1 1.638(9) . ?
C37B H37C 0.9900 . ?
C37B H37D 0.9900 . ?
C38B N2 1.398(8) . ?
C38B H38C 0.9900 . ?
C38B H38D 0.9900 . ?
C39B C40B 1.570(9) . ?
C39B N2 1.598(7) . ?
C39B H39C 0.9900 . ?
C39B H39D 0.9900 . ?
C40B N3 1.356(8) . ?
C40B H40C 0.9900 . ?
C40B H40D 0.9900 . ?
C41B C42B 1.557(8) . ?
C41B N3 1.622(8) . ?
C41B H41C 0.9900 . ?
C41B H41D 0.9900 . ?
C42B N4 1.357(8) . ?
C42B H42C 0.9900 . ?
C42B H42D 0.9900 . ?
C43B C44B 1.548(9) . ?
C43B N4 1.636(8) . ?
C43B H43C 0.9900 . ?
C43B H43D 0.9900 . ?
C44B N1 1.399(8) . ?
C44B H44C 0.9900 . ?
C44B H44D 0.9900 . ?
C45 O1 1.429(7) . ?
C45 C46 1.499(9) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 C47 1.500(9) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 C48 1.363(11) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 O1 1.457(8) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
N1 Na1 2.461(4) . ?
N2 Na1 2.460(4) . ?
N3 Na1 2.452(4) . ?
N4 Na1 2.444(4) . ?
O1 Na1 2.243(4) . ?

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
C6 C1 C2 115.3(3) . . ?
C6 C1 B1 121.8(3) . . ?
C2 C1 B1 122.8(3) . . ?
C3 C2 C1 122.4(3) . . ?
C3 C2 H2 118.8 . . ?
C1 C2 H2 118.8 . . ?
C2 C3 C4 121.2(3) . . ?
C2 C3 C7 119.6(3) . . ?
C4 C3 C7 119.1(3) . . ?
C3 C4 C5 117.8(3) . . ?
C3 C4 H4 121.1 . . ?
C5 C4 H4 121.1 . . ?
C6 C5 C4 120.4(3) . . ?
C6 C5 C8 119.2(3) . . ?
C4 C5 C8 120.3(3) . . ?
C5 C6 C1 122.9(3) . . ?
C5 C6 H6 118.6 . . ?
C1 C6 H6 118.6 . . ?
F3 C7 F1 106.9(4) . . ?
F3 C7 F2 108.9(4) . . ?
F1 C7 F2 101.5(3) . . ?
F3 C7 C3 114.1(3) . . ?
F1 C7 C3 112.9(3) . . ?
F2 C7 C3 111.6(3) . . ?
F4 C8 F6 107.7(4) . . ?
F4 C8 F5 105.6(4) . . ?
F6 C8 F5 103.3(4) . . ?
F4 C8 C5 114.5(3) . . ?
F6 C8 C5 112.5(3) . . ?
F5 C8 C5 112.3(4) . . ?
C14 C9 C10 115.1(3) . . ?
C14 C9 B1 122.2(3) . . ?
C10 C9 B1 122.7(3) . . ?
C11 C10 C9 122.3(3) . . ?
C11 C10 H10 118.8 . . ?
C9 C10 H10 118.8 . . ?
C12 C11 C10 121.0(3) . . ?
C12 C11 C15 119.4(3) . . ?
C10 C11 C15 119.4(4) . . ?
C13 C12 C11 117.9(3) . . ?
C13 C12 H12 121.1 . . ?
C11 C12 H12 121.1 . . ?
C12 C13 C14 121.0(3) . . ?
C12 C13 C16 120.7(3) . . ?
C14 C13 C16 118.3(4) . . ?
C13 C14 C9 122.7(3) . . ?
C13 C14 H14 118.7 . . ?
C9 C14 H14 118.7 . . ?
F8 C15 F7 105.1(4) . . ?
F8 C15 F9 104.5(3) . . ?
F7 C15 F9 107.9(4) . . ?
F8 C15 C11 114.5(4) . . ?
F7 C15 C11 113.3(4) . . ?
F9 C15 C11 110.9(4) . . ?
F10 C16 F12 108.3(4) . . ?
F10 C16 F11 105.3(4) . . ?
F12 C16 F11 105.7(4) . . ?
F10 C16 C13 113.1(4) . . ?
F12 C16 C13 112.8(4) . . ?
F11 C16 C13 111.1(4) . . ?
C18 C17 C22 115.8(3) . . ?
C18 C17 B1 122.2(3) . . ?
C22 C17 B1 121.9(3) . . ?
C17 C18 C19 122.3(3) . . ?
C17 C18 H18 118.9 . . ?
C19 C18 H18 118.9 . . ?
C20 C19 C18 120.8(4) . . ?
C20 C19 C23 120.1(3) . . ?
C18 C19 C23 119.1(4) . . ?
C19 C20 C21 118.3(3) . . ?
C19 C20 H20 120.9 . . ?
C21 C20 H20 120.9 . . ?
C20 C21 C22 120.6(3) . . ?
C20 C21 C24 121.5(3) . . ?
C22 C21 C24 117.9(4) . . ?
C21 C22 C17 122.3(3) . . ?
C21 C22 H22 118.8 . . ?
C17 C22 H22 118.8 . . ?
F13B C23 F15B 106.6(11) . . ?
F13A C23 F15A 107.4(6) . . ?
F13B C23 F14B 118.0(13) . . ?
F15B C23 F14B 107.5(11) . . ?
F13A C23 F14A 104.3(6) . . ?
F15A C23 F14A 98.0(6) . . ?
F13B C23 C19 113.4(7) . . ?
F13A C23 C19 117.3(4) . . ?
F15B C23 C19 106.1(7) . . ?
F15A C23 C19 114.6(4) . . ?
F14B C23 C19 104.6(6) . . ?
F14A C23 C19 113.1(5) . . ?
F16A C24 F18A 112.2(11) . . ?
F17B C24 F18B 108.5(16) . . ?
F17B C24 F16B 104.2(14) . . ?
F18B C24 F16B 97(2) . . ?
F16A C24 F17A 106.1(8) . . ?
F18A C24 F17A 103.9(10) . . ?
F16A C24 C21 114.7(8) . . ?
F17B C24 C21 118.1(13) . . ?
F18A C24 C21 110.5(10) . . ?
F18B C24 C21 117.3(15) . . ?
F16B C24 C21 108.7(14) . . ?
F17A C24 C21 108.8(7) . . ?
C30 C25 C26 115.5(3) . . ?
C30 C25 B1 123.0(3) . . ?
C26 C25 B1 121.0(3) . . ?
C27 C26 C25 122.3(3) . . ?
C27 C26 H26 118.9 . . ?
C25 C26 H26 118.9 . . ?
C28 C27 C26 120.8(3) . . ?
C28 C27 C31 119.3(3) . . ?
C26 C27 C31 119.9(3) . . ?
C27 C28 C29 118.0(3) . . ?
C27 C28 H28 121.0 . . ?
C29 C28 H28 121.0 . . ?
C28 C29 C30 120.5(3) . . ?
C28 C29 C32 120.0(3) . . ?
C30 C29 C32 119.4(3) . . ?
C29 C30 C25 122.8(3) . . ?
C29 C30 H30 118.6 . . ?
C25 C30 H30 118.6 . . ?
F21A C31 F20A 106.3(6) . . ?
F20B C31 F21B 104.5(6) . . ?
F20B C31 F19B 104.8(6) . . ?
F21B C31 F19B 102.2(7) . . ?
F21A C31 F19A 113.6(7) . . ?
F20A C31 F19A 103.1(5) . . ?
F21A C31 C27 111.7(4) . . ?
F20A C31 C27 114.1(4) . . ?
F20B C31 C27 117.1(4) . . ?
F21B C31 C27 114.8(4) . . ?
F19B C31 C27 112.0(4) . . ?
F19A C31 C27 107.8(4) . . ?
F23B C32 F24B 106.3(15) . . ?
F23A C32 F24A 110.9(5) . . ?
F23B C32 F22B 108.3(13) . . ?
F24B C32 F22B 99.7(13) . . ?
F23A C32 F22A 103.6(5) . . ?
F24A C32 F22A 102.1(5) . . ?
F23B C32 C29 117.0(8) . . ?
F23A C32 C29 115.6(4) . . ?
F24B C32 C29 112.2(10) . . ?
F24A C32 C29 113.3(4) . . ?
F22B C32 C29 111.8(7) . . ?
F22A C32 C29 110.1(4) . . ?
N1 C33 H33A 109.5 . . ?
N1 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
N1 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
N2 C34 H34A 109.5 . . ?
N2 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
N2 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
N3 C35 H35A 109.5 . . ?
N3 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
N3 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
N4 C36 H36A 109.5 . . ?
N4 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
N4 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
N1 C37A C38A 104.2(9) . . ?
N1 C37A H37A 110.9 . . ?
C38A C37A H37A 110.9 . . ?
N1 C37A H37B 110.9 . . ?
C38A C37A H37B 110.9 . . ?
H37A C37A H37B 108.9 . . ?
C37A C38A N2 120.1(7) . . ?
C37A C38A H38A 107.3 . . ?
N2 C38A H38A 107.3 . . ?
C37A C38A H38B 107.3 . . ?
N2 C38A H38B 107.3 . . ?
H38A C38A H38B 106.9 . . ?
N2 C39A C40A 105.5(8) . . ?
N2 C39A H39A 110.6 . . ?
C40A C39A H39A 110.6 . . ?
N2 C39A H39B 110.6 . . ?
C40A C39A H39B 110.6 . . ?
H39A C39A H39B 108.8 . . ?
C39A C40A N3 119.0(7) . . ?
C39A C40A H40A 107.6 . . ?
N3 C40A H40A 107.6 . . ?
C39A C40A H40B 107.6 . . ?
N3 C40A H40B 107.6 . . ?
H40A C40A H40B 107.0 . . ?
N3 C41A C42A 102.1(8) . . ?
N3 C41A H41A 111.4 . . ?
C42A C41A H41A 111.4 . . ?
N3 C41A H41B 111.4 . . ?
C42A C41A H41B 111.4 . . ?
H41A C41A H41B 109.2 . . ?
C41A C42A N4 122.1(8) . . ?
C41A C42A H42A 106.8 . . ?
N4 C42A H42A 106.8 . . ?
C41A C42A H42B 106.8 . . ?
N4 C42A H42B 106.8 . . ?
H42A C42A H42B 106.7 . . ?
N4 C43A C44A 100.9(9) . . ?
N4 C43A H43A 111.6 . . ?
C44A C43A H43A 111.6 . . ?
N4 C43A H43B 111.6 . . ?
C44A C43A H43B 111.6 . . ?
H43A C43A H43B 109.4 . . ?
C43A C44A N1 120.7(8) . . ?
C43A C44A H44A 107.1 . . ?
N1 C44A H44A 107.1 . . ?
C43A C44A H44B 107.1 . . ?
N1 C44A H44B 107.1 . . ?
H44A C44A H44B 106.8 . . ?
C38B C37B N1 112.5(6) . . ?
C38B C37B H37C 109.1 . . ?
N1 C37B H37C 109.1 . . ?
C38B C37B H37D 109.1 . . ?
N1 C37B H37D 109.1 . . ?
H37C C37B H37D 107.8 . . ?
N2 C38B C37B 104.5(6) . . ?
N2 C38B H38C 110.9 . . ?
C37B C38B H38C 110.9 . . ?
N2 C38B H38D 110.9 . . ?
C37B C38B H38D 110.9 . . ?
H38C C38B H38D 108.9 . . ?
C40B C39B N2 112.1(5) . . ?
C40B C39B H39C 109.2 . . ?
N2 C39B H39C 109.2 . . ?
C40B C39B H39D 109.2 . . ?
N2 C39B H39D 109.2 . . ?
H39C C39B H39D 107.9 . . ?
N3 C40B C39B 105.5(6) . . ?
N3 C40B H40C 110.6 . . ?
C39B C40B H40C 110.6 . . ?
N3 C40B H40D 110.6 . . ?
C39B C40B H40D 110.6 . . ?
H40C C40B H40D 108.8 . . ?
C42B C41B N3 112.3(5) . . ?
C42B C41B H41C 109.1 . . ?
N3 C41B H41C 109.1 . . ?
C42B C41B H41D 109.1 . . ?
N3 C41B H41D 109.1 . . ?
H41C C41B H41D 107.9 . . ?
N4 C42B C41B 104.6(6) . . ?
N4 C42B H42C 110.8 . . ?
C41B C42B H42C 110.8 . . ?
N4 C42B H42D 110.8 . . ?
C41B C42B H42D 110.8 . . ?
H42C C42B H42D 108.9 . . ?
C44B C43B N4 112.2(5) . . ?
C44B C43B H43C 109.2 . . ?
N4 C43B H43C 109.2 . . ?
C44B C43B H43D 109.2 . . ?
N4 C43B H43D 109.2 . . ?
H43C C43B H43D 107.9 . . ?
N1 C44B C43B 101.9(7) . . ?
N1 C44B H44C 111.4 . . ?
C43B C44B H44C 111.4 . . ?
N1 C44B H44D 111.4 . . ?
C43B C44B H44D 111.4 . . ?
H44C C44B H44D 109.3 . . ?
O1 C45 C46 106.7(5) . . ?
O1 C45 H45A 110.4 . . ?
C46 C45 H45A 110.4 . . ?
O1 C45 H45B 110.4 . . ?
C46 C45 H45B 110.4 . . ?
H45A C45 H45B 108.6 . . ?
C45 C46 C47 104.0(5) . . ?
C45 C46 H46A 111.0 . . ?
C47 C46 H46A 111.0 . . ?
C45 C46 H46B 111.0 . . ?
C47 C46 H46B 111.0 . . ?
H46A C46 H46B 109.0 . . ?
C48 C47 C46 105.1(7) . . ?
C48 C47 H47A 110.7 . . ?
C46 C47 H47A 110.7 . . ?
C48 C47 H47B 110.7 . . ?
C46 C47 H47B 110.7 . . ?
H47A C47 H47B 108.8 . . ?
C47 C48 O1 108.2(8) . . ?
C47 C48 H48A 110.1 . . ?
O1 C48 H48A 110.1 . . ?
C47 C48 H48B 110.1 . . ?
O1 C48 H48B 110.1 . . ?
H48A C48 H48B 108.4 . . ?
C17 B1 C1 112.0(3) . . ?
C17 B1 C25 107.8(3) . . ?
C1 B1 C25 108.6(3) . . ?
C17 B1 C9 108.2(3) . . ?
C1 B1 C9 108.4(3) . . ?
C25 B1 C9 111.9(3) . . ?
C37A N1 C33 120.0(6) . . ?
C44B N1 C33 118.5(5) . . ?
C37A N1 C44A 104.9(9) . . ?
C33 N1 C44A 99.9(6) . . ?
C44B N1 C37B 106.4(6) . . ?
C33 N1 C37B 102.6(4) . . ?
C37A N1 Na1 112.4(5) . . ?
C44B N1 Na1 108.9(4) . . ?
C33 N1 Na1 116.2(3) . . ?
C44A N1 Na1 99.1(5) . . ?
C37B N1 Na1 102.1(4) . . ?
C39A N2 C34 122.3(5) . . ?
C38B N2 C34 118.4(4) . . ?
C38B N2 C39B 107.2(5) . . ?
C34 N2 C39B 101.0(4) . . ?
C39A N2 C38A 103.4(7) . . ?
C34 N2 C38A 99.8(5) . . ?
C39A N2 Na1 110.9(4) . . ?
C38B N2 Na1 110.3(4) . . ?
C34 N2 Na1 116.3(3) . . ?
C39B N2 Na1 101.1(3) . . ?
C38A N2 Na1 99.4(5) . . ?
C40B N3 C35 118.6(5) . . ?
C41A N3 C35 118.4(5) . . ?
C41A N3 C40A 101.1(7) . . ?
C35 N3 C40A 100.3(4) . . ?
C40B N3 C41B 109.5(5) . . ?
C35 N3 C41B 102.1(4) . . ?
C40B N3 Na1 108.2(4) . . ?
C41A N3 Na1 114.5(4) . . ?
C35 N3 Na1 116.5(3) . . ?
C40A N3 Na1 101.4(4) . . ?
C41B N3 Na1 99.7(3) . . ?
C42B N4 C36 118.5(5) . . ?
C43A N4 C36 123.3(6) . . ?
C42B N4 C43B 108.0(5) . . ?
C36 N4 C43B 103.2(4) . . ?
C43A N4 C42A 99.0(8) . . ?
C36 N4 C42A 99.9(5) . . ?
C42B N4 Na1 108.9(4) . . ?
C43A N4 Na1 112.7(5) . . ?
C36 N4 Na1 115.6(3) . . ?
C43B N4 Na1 100.7(4) . . ?
C42A N4 Na1 100.3(4) . . ?
C45 O1 C48 106.1(5) . . ?
C45 O1 Na1 138.6(4) . . ?
C48 O1 Na1 115.2(4) . . ?
O1 Na1 N4 121.00(16) . . ?
O1 Na1 N3 121.24(15) . . ?
N4 Na1 N3 76.05(14) . . ?
O1 Na1 N2 118.34(15) . . ?
N4 Na1 N2 120.63(13) . . ?
N3 Na1 N2 75.61(13) . . ?
O1 Na1 N1 119.03(16) . . ?
N4 Na1 N1 75.31(15) . . ?
N3 Na1 N1 119.71(13) . . ?
N2 Na1 N1 75.42(14) . . ?

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
C6 C1 C2 C3 -1.2(5) . . . . ?
B1 C1 C2 C3 -176.5(3) . . . . ?
C1 C2 C3 C4 1.6(5) . . . . ?
C1 C2 C3 C7 179.4(3) . . . . ?
C2 C3 C4 C5 -0.2(5) . . . . ?
C7 C3 C4 C5 -178.0(4) . . . . ?
C3 C4 C5 C6 -1.4(5) . . . . ?
C3 C4 C5 C8 -179.8(4) . . . . ?
C4 C5 C6 C1 1.8(5) . . . . ?
C8 C5 C6 C1 -179.8(4) . . . . ?
C2 C1 C6 C5 -0.5(5) . . . . ?
B1 C1 C6 C5 174.9(3) . . . . ?
C2 C3 C7 F3 162.3(4) . . . . ?
C4 C3 C7 F3 -19.9(6) . . . . ?
C2 C3 C7 F1 39.9(5) . . . . ?
C4 C3 C7 F1 -142.3(4) . . . . ?
C2 C3 C7 F2 -73.7(5) . . . . ?
C4 C3 C7 F2 104.1(4) . . . . ?
C6 C5 C8 F4 171.1(4) . . . . ?
C4 C5 C8 F4 -10.5(6) . . . . ?
C6 C5 C8 F6 47.7(6) . . . . ?
C4 C5 C8 F6 -134.0(4) . . . . ?
C6 C5 C8 F5 -68.4(5) . . . . ?
C4 C5 C8 F5 109.9(4) . . . . ?
C14 C9 C10 C11 1.5(5) . . . . ?
B1 C9 C10 C11 178.9(3) . . . . ?
C9 C10 C11 C12 -1.5(6) . . . . ?
C9 C10 C11 C15 174.6(4) . . . . ?
C10 C11 C12 C13 0.5(6) . . . . ?
C15 C11 C12 C13 -175.6(4) . . . . ?
C11 C12 C13 C14 0.4(6) . . . . ?
C11 C12 C13 C16 179.0(4) . . . . ?
C12 C13 C14 C9 -0.4(6) . . . . ?
C16 C13 C14 C9 -179.0(4) . . . . ?
C10 C9 C14 C13 -0.5(5) . . . . ?
B1 C9 C14 C13 -178.0(3) . . . . ?
C12 C11 C15 F8 -28.8(6) . . . . ?
C10 C11 C15 F8 155.0(4) . . . . ?
C12 C11 C15 F7 -149.4(4) . . . . ?
C10 C11 C15 F7 34.4(6) . . . . ?
C12 C11 C15 F9 89.1(5) . . . . ?
C10 C11 C15 F9 -87.0(5) . . . . ?
C12 C13 C16 F10 6.3(6) . . . . ?
C14 C13 C16 F10 -175.1(4) . . . . ?
C12 C13 C16 F12 129.7(4) . . . . ?
C14 C13 C16 F12 -51.8(6) . . . . ?
C12 C13 C16 F11 -111.9(5) . . . . ?
C14 C13 C16 F11 66.7(5) . . . . ?
C22 C17 C18 C19 -1.1(5) . . . . ?
B1 C17 C18 C19 174.6(3) . . . . ?
C17 C18 C19 C20 0.7(6) . . . . ?
C17 C18 C19 C23 -178.3(4) . . . . ?
C18 C19 C20 C21 -0.3(6) . . . . ?
C23 C19 C20 C21 178.7(4) . . . . ?
C19 C20 C21 C22 0.3(6) . . . . ?
C19 C20 C21 C24 -179.5(4) . . . . ?
C20 C21 C22 C17 -0.9(6) . . . . ?
C24 C21 C22 C17 179.0(4) . . . . ?
C18 C17 C22 C21 1.2(5) . . . . ?
B1 C17 C22 C21 -174.5(3) . . . . ?
C20 C19 C23 F13B 151.3(12) . . . . ?
C18 C19 C23 F13B -29.8(13) . . . . ?
C20 C19 C23 F13A -15.6(9) . . . . ?
C18 C19 C23 F13A 163.4(7) . . . . ?
C20 C19 C23 F15B 34.7(10) . . . . ?
C18 C19 C23 F15B -146.4(9) . . . . ?
C20 C19 C23 F15A -142.9(6) . . . . ?
C18 C19 C23 F15A 36.0(8) . . . . ?
C20 C19 C23 F14B -78.8(12) . . . . ?
C18 C19 C23 F14B 100.1(12) . . . . ?
C20 C19 C23 F14A 106.0(7) . . . . ?
C18 C19 C23 F14A -75.1(7) . . . . ?
C20 C21 C24 F16A -125.1(9) . . . . ?
C22 C21 C24 F16A 55.0(9) . . . . ?
C20 C21 C24 F17B 140(2) . . . . ?
C22 C21 C24 F17B -40(2) . . . . ?
C20 C21 C24 F18A 2.8(10) . . . . ?
C22 C21 C24 F18A -177.0(9) . . . . ?
C20 C21 C24 F18B 7.3(12) . . . . ?
C22 C21 C24 F18B -172.5(11) . . . . ?
C20 C21 C24 F16B -101(2) . . . . ?
C22 C21 C24 F16B 79(2) . . . . ?
C20 C21 C24 F17A 116.3(10) . . . . ?
C22 C21 C24 F17A -63.6(10) . . . . ?
C30 C25 C26 C27 0.1(5) . . . . ?
B1 C25 C26 C27 -172.7(3) . . . . ?
C25 C26 C27 C28 -1.3(5) . . . . ?
C25 C26 C27 C31 177.8(3) . . . . ?
C26 C27 C28 C29 1.1(5) . . . . ?
C31 C27 C28 C29 -177.9(3) . . . . ?
C27 C28 C29 C30 0.1(5) . . . . ?
C27 C28 C29 C32 -179.5(3) . . . . ?
C28 C29 C30 C25 -1.3(5) . . . . ?
C32 C29 C30 C25 178.3(3) . . . . ?
C26 C25 C30 C29 1.1(5) . . . . ?
B1 C25 C30 C29 173.8(3) . . . . ?
C28 C27 C31 F21A -129.9(7) . . . . ?
C26 C27 C31 F21A 51.1(8) . . . . ?
C28 C27 C31 F20A -9.2(6) . . . . ?
C26 C27 C31 F20A 171.7(5) . . . . ?
C28 C27 C31 F20B 174.4(6) . . . . ?
C26 C27 C31 F20B -4.7(7) . . . . ?
C28 C27 C31 F21B 51.3(8) . . . . ?
C26 C27 C31 F21B -127.7(7) . . . . ?
C28 C27 C31 F19B -64.6(7) . . . . ?
C26 C27 C31 F19B 116.4(6) . . . . ?
C28 C27 C31 F19A 104.7(6) . . . . ?
C26 C27 C31 F19A -74.4(7) . . . . ?
C28 C29 C32 F23B -172.8(16) . . . . ?
C30 C29 C32 F23B 7.6(17) . . . . ?
C28 C29 C32 F23A -9.4(7) . . . . ?
C30 C29 C32 F23A 171.1(6) . . . . ?
C28 C29 C32 F24B -49.6(16) . . . . ?
C30 C29 C32 F24B 130.8(15) . . . . ?
C28 C29 C32 F24A 120.1(6) . . . . ?
C30 C29 C32 F24A -59.4(7) . . . . ?
C28 C29 C32 F22B 61.5(16) . . . . ?
C30 C29 C32 F22B -118.1(16) . . . . ?
C28 C29 C32 F22A -126.3(5) . . . . ?
C30 C29 C32 F22A 54.1(6) . . . . ?
N1 C37A C38A N2 -63.6(13) . . . . ?
N2 C39A C40A N3 -60.7(12) . . . . ?
N3 C41A C42A N4 -58.7(13) . . . . ?
N4 C43A C44A N1 -64.5(14) . . . . ?
N1 C37B C38B N2 68.0(8) . . . . ?
N2 C39B C40B N3 71.2(7) . . . . ?
N3 C41B C42B N4 72.2(8) . . . . ?
N4 C43B C44B N1 73.0(8) . . . . ?
O1 C45 C46 C47 -9.7(8) . . . . ?
C45 C46 C47 C48 26.1(10) . . . . ?
C46 C47 C48 O1 -32.8(11) . . . . ?
C18 C17 B1 C1 144.6(3) . . . . ?
C22 C17 B1 C1 -40.0(4) . . . . ?
C18 C17 B1 C25 25.1(4) . . . . ?
C22 C17 B1 C25 -159.5(3) . . . . ?
C18 C17 B1 C9 -96.1(4) . . . . ?
C22 C17 B1 C9 79.3(4) . . . . ?
C6 C1 B1 C17 155.8(3) . . . . ?
C2 C1 B1 C17 -29.2(4) . . . . ?
C6 C1 B1 C25 -85.2(4) . . . . ?
C2 C1 B1 C25 89.8(3) . . . . ?
C6 C1 B1 C9 36.5(4) . . . . ?
C2 C1 B1 C9 -148.5(3) . . . . ?
C30 C25 B1 C17 -88.2(4) . . . . ?
C26 C25 B1 C17 84.0(4) . . . . ?
C30 C25 B1 C1 150.2(3) . . . . ?
C26 C25 B1 C1 -37.6(4) . . . . ?
C30 C25 B1 C9 30.6(4) . . . . ?
C26 C25 B1 C9 -157.1(3) . . . . ?
C14 C9 B1 C17 -31.0(4) . . . . ?
C10 C9 B1 C17 151.8(3) . . . . ?
C14 C9 B1 C1 90.7(4) . . . . ?
C10 C9 B1 C1 -86.6(4) . . . . ?
C14 C9 B1 C25 -149.6(3) . . . . ?
C10 C9 B1 C25 33.1(4) . . . . ?
C38A C37A N1 C44B 151.2(10) . . . . ?
C38A C37A N1 C33 -95.1(8) . . . . ?
C38A C37A N1 C44A 153.9(8) . . . . ?
C38A C37A N1 C37B -30.2(7) . . . . ?
C38A C37A N1 Na1 47.2(10) . . . . ?
C43B C44B N1 C37A -164.9(7) . . . . ?
C43B C44B N1 C33 79.5(7) . . . . ?
C43B C44B N1 C44A 20.0(9) . . . . ?
C43B C44B N1 C37B -165.7(5) . . . . ?
C43B C44B N1 Na1 -56.4(6) . . . . ?
C43A C44A N1 C37A -77.2(13) . . . . ?
C43A C44A N1 C44B -72.3(13) . . . . ?
C43A C44A N1 C33 157.9(11) . . . . ?
C43A C44A N1 C37B -80.5(15) . . . . ?
C43A C44A N1 Na1 39.1(13) . . . . ?
C38B C37B N1 C37A 69.4(10) . . . . ?
C38B C37B N1 C44B 70.8(8) . . . . ?
C38B C37B N1 C33 -164.1(7) . . . . ?
C38B C37B N1 C44A 75.3(11) . . . . ?
C38B C37B N1 Na1 -43.3(7) . . . . ?
C40A C39A N2 C38B 155.3(9) . . . . ?
C40A C39A N2 C34 -93.0(8) . . . . ?
C40A C39A N2 C39B -30.2(6) . . . . ?
C40A C39A N2 C38A 156.1(8) . . . . ?
C40A C39A N2 Na1 50.4(9) . . . . ?
C37B C38B N2 C39A -158.9(7) . . . . ?
C37B C38B N2 C34 84.3(6) . . . . ?
C37B C38B N2 C39B -162.4(5) . . . . ?
C37B C38B N2 C38A 22.4(7) . . . . ?
C37B C38B N2 Na1 -53.2(6) . . . . ?
C40B C39B N2 C39A 66.5(8) . . . . ?
C40B C39B N2 C38B 72.0(7) . . . . ?
C40B C39B N2 C34 -163.4(5) . . . . ?
C40B C39B N2 C38A 76.2(9) . . . . ?
C40B C39B N2 Na1 -43.5(6) . . . . ?
C37A C38A N2 C39A -73.1(12) . . . . ?
C37A C38A N2 C38B -71.9(11) . . . . ?
C37A C38A N2 C34 160.1(10) . . . . ?
C37A C38A N2 C39B -79.1(14) . . . . ?
C37A C38A N2 Na1 41.1(11) . . . . ?
C39B C40B N3 C41A -165.6(7) . . . . ?
C39B C40B N3 C35 80.9(6) . . . . ?
C39B C40B N3 C40A 25.5(8) . . . . ?
C39B C40B N3 C41B -162.6(5) . . . . ?
C39B C40B N3 Na1 -54.9(6) . . . . ?
C42A C41A N3 C40B 148.0(9) . . . . ?
C42A C41A N3 C35 -98.2(8) . . . . ?
C42A C41A N3 C40A 153.5(8) . . . . ?
C42A C41A N3 C41B -27.2(7) . . . . ?
C42A C41A N3 Na1 45.4(9) . . . . ?
C39A C40A N3 C40B -72.5(11) . . . . ?
C39A C40A N3 C41A -83.4(10) . . . . ?
C39A C40A N3 C35 154.7(9) . . . . ?
C39A C40A N3 C41B -84.0(12) . . . . ?
C39A C40A N3 Na1 34.7(10) . . . . ?
C42B C41B N3 C40B 67.6(8) . . . . ?
C42B C41B N3 C41A 72.5(9) . . . . ?
C42B C41B N3 C35 -165.8(6) . . . . ?
C42B C41B N3 C40A 73.4(10) . . . . ?
C42B C41B N3 Na1 -45.8(7) . . . . ?
C41B C42B N4 C43A -161.9(8) . . . . ?
C41B C42B N4 C36 80.7(7) . . . . ?
C41B C42B N4 C43B -162.6(5) . . . . ?
C41B C42B N4 C42A 23.6(8) . . . . ?
C41B C42B N4 Na1 -54.1(6) . . . . ?
C44A C43A N4 C42B 154.1(10) . . . . ?
C44A C43A N4 C36 -94.9(9) . . . . ?
C44A C43A N4 C43B -26.9(7) . . . . ?
C44A C43A N4 C42A 156.9(8) . . . . ?
C44A C43A N4 Na1 51.7(9) . . . . ?
C44B C43B N4 C42B 67.5(8) . . . . ?
C44B C43B N4 C43A 66.5(9) . . . . ?
C44B C43B N4 C36 -166.2(6) . . . . ?
C44B C43B N4 C42A 72.2(10) . . . . ?
C44B C43B N4 Na1 -46.5(7) . . . . ?
C41A C42A N4 C42B -71.9(12) . . . . ?
C41A C42A N4 C43A -77.1(12) . . . . ?
C41A C42A N4 C36 156.6(10) . . . . ?
C41A C42A N4 C43B -80.7(13) . . . . ?
C41A C42A N4 Na1 38.2(12) . . . . ?
C46 C45 O1 C48 -9.0(9) . . . . ?
C46 C45 O1 Na1 175.3(5) . . . . ?
C47 C48 O1 C45 26.9(10) . . . . ?
C47 C48 O1 Na1 -156.3(7) . . . . ?

_refine_diff_density_max         0.749
_refine_diff_density_min         -0.533
_refine_diff_density_rms         0.067

_shelxl_version_number           2013-4


_exptl_crystal_recrystallization_method 'Layering: CH2Cl2/hexane'
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
