# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_1

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C78 H32 B2 Ca F24 N12, C4 H8 O, C4 H10 O'
_chemical_formula_sum            'C86 H50 B2 Ca F24 N12 O2'
_chemical_formula_weight         1801.08
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_Int_Tables_number      14
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   12.6950(5)
_cell_length_b                   18.0160(10)
_cell_length_c                   17.448(2)
_cell_angle_alpha                90
_cell_angle_beta                 101.987(6)
_cell_angle_gamma                90
_cell_volume                     3903.6(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    5948
_cell_measurement_theta_min      3.1612
_cell_measurement_theta_max      29.2898
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_exptl_crystal_density_diffrn    1.532
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1824
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.198
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
        (compiled Jan 23 2012,18:06:46)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.977
_exptl_absorpt_correction_T_max  0.990

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      180(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_detector_area_resol_mean 16.1978
_diffrn_orient_matrix_ub_11      0.0370258
_diffrn_orient_matrix_ub_12      0.0252049
_diffrn_orient_matrix_ub_13      0.0223942
_diffrn_orient_matrix_ub_21      0.0420271
_diffrn_orient_matrix_ub_22      -0.0151286
_diffrn_orient_matrix_ub_23      -0.0163595
_diffrn_orient_matrix_ub_31      -0.0113488
_diffrn_orient_matrix_ub_32      0.0261914
_diffrn_orient_matrix_ub_33      -0.0309864
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_av_R_equivalents  0.0401
_diffrn_reflns_av_unetI/netI     0.046
_diffrn_reflns_number            34745
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         3.28
_diffrn_reflns_theta_max         29.34
_diffrn_reflns_theta_full        29.34
_diffrn_measured_fraction_theta_full 0.876
_diffrn_measured_fraction_theta_max 0.876
_reflns_number_total             9405
_reflns_number_gt                6252
_reflns_threshold_expression     >2σ(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
        (compiled Jan 23 2012,18:06:46)
;
_computing_cell_refinement       
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
        (compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction        
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
        (compiled Jan 23 2012,18:06:46)
;
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0380P)²+1.1258P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         9405
_refine_ls_number_parameters     622
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0834
_refine_ls_R_factor_gt           0.0454
_refine_ls_wR_factor_ref         0.1042
_refine_ls_wR_factor_gt          0.0895
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_restrained_S_all      1.019
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.241
_refine_diff_density_min         -0.263
_refine_diff_density_rms         0.045

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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'
Ca Ca 0.2262 0.3064 '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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.63226(15) 0.54926(11) 0.20488(11) 0.0356(4) Uani 1 1 d . . .
C2 C 0.58923(19) 0.59097(14) 0.13915(12) 0.0506(6) Uani 1 1 d . . .
H2 H 0.5135 0.5972 0.1237 0.061 Uiso 1 1 calc R . .
C3 C 0.6571(2) 0.62361(17) 0.09604(14) 0.0702(8) Uani 1 1 d . . .
H3 H 0.6278 0.6527 0.0512 0.084 Uiso 1 1 calc R . .
C4 C 0.7661(2) 0.61408(18) 0.11785(16) 0.0768(9) Uani 1 1 d . . .
H4 H 0.8123 0.6374 0.0887 0.092 Uiso 1 1 calc R . .
C5 C 0.8093(2) 0.57109(17) 0.18161(16) 0.0656(8) Uani 1 1 d . . .
H5 H 0.885 0.5638 0.1956 0.079 Uiso 1 1 calc R . .
C6 C 0.74268(17) 0.53821(13) 0.22565(13) 0.0463(5) Uani 1 1 d . . .
H6 H 0.7725 0.5084 0.2697 0.056 Uiso 1 1 calc R . .
C7 C 0.55953(14) 0.51645(10) 0.25185(10) 0.0294(4) Uani 1 1 d . . .
C8 C 0.47370(14) 0.46658(10) 0.22939(10) 0.0290(4) Uani 1 1 d . . .
C9 C 0.43502(13) 0.45370(10) 0.29885(10) 0.0265(4) Uani 1 1 d . . .
C10 C 0.35068(14) 0.40313(10) 0.29807(10) 0.0290(4) Uani 1 1 d . . .
C11 C 0.30519(15) 0.36958(11) 0.22983(12) 0.0354(4) Uani 1 1 d . . .
C12 C 0.34296(17) 0.38223(11) 0.16030(11) 0.0401(5) Uani 1 1 d . . .
C13 C 0.42587(16) 0.42913(11) 0.15988(11) 0.0368(5) Uani 1 1 d . . .
C21 C 0.77995(14) 0.45295(10) 0.62409(11) 0.0319(4) Uani 1 1 d . . .
C22 C 0.82694(16) 0.47678(12) 0.69974(11) 0.0378(5) Uani 1 1 d . . .
H22 H 0.8687 0.521 0.7069 0.045 Uiso 1 1 calc R . .
C23 C 0.81285(18) 0.43621(13) 0.76425(13) 0.0491(6) Uani 1 1 d . . .
H23 H 0.8447 0.4528 0.8155 0.059 Uiso 1 1 calc R . .
C24 C 0.75271(18) 0.37186(14) 0.75431(14) 0.0570(7) Uani 1 1 d . . .
H24 H 0.7416 0.3449 0.7987 0.068 Uiso 1 1 calc R . .
C25 C 0.70878(17) 0.34671(13) 0.67997(15) 0.0541(6) Uani 1 1 d . . .
H25 H 0.6686 0.3019 0.6732 0.065 Uiso 1 1 calc R . .
C26 C 0.72296(15) 0.38647(11) 0.61522(13) 0.0412(5) Uani 1 1 d . . .
H26 H 0.6935 0.3683 0.5642 0.049 Uiso 1 1 calc R . .
C27 C 0.78481(14) 0.49947(10) 0.55564(10) 0.0286(4) Uani 1 1 d . . .
C28 C 0.87134(14) 0.54336(10) 0.53995(11) 0.0309(4) Uani 1 1 d . . .
C29 C 0.98007(15) 0.55355(12) 0.57643(12) 0.0407(5) Uani 1 1 d . . .
C30 C 1.04118(16) 0.60170(14) 0.54473(14) 0.0503(6) Uani 1 1 d . . .
C31 C 0.99767(17) 0.63957(13) 0.47550(15) 0.0509(6) Uani 1 1 d . . .
C32 C 0.89375(16) 0.62941(12) 0.43703(12) 0.0405(5) Uani 1 1 d . . .
C33 C 0.82844(14) 0.58035(10) 0.46933(11) 0.0303(4) Uani 1 1 d . . .
C41 C 0.46950(14) 0.70897(10) 0.58236(11) 0.0286(4) Uani 1 1 d . . .
C42 C 0.38919(15) 0.66544(11) 0.60309(11) 0.0337(4) Uani 1 1 d . . .
H42 H 0.3524 0.6298 0.5672 0.04 Uiso 1 1 calc R . .
C43 C 0.36251(16) 0.67372(12) 0.67587(12) 0.0403(5) Uani 1 1 d . . .
H43 H 0.3072 0.6441 0.6893 0.048 Uiso 1 1 calc R . .
C44 C 0.41621(17) 0.72496(12) 0.72883(12) 0.0429(5) Uani 1 1 d . . .
H44 H 0.3982 0.7303 0.7788 0.051 Uiso 1 1 calc R . .
C45 C 0.49612(17) 0.76841(12) 0.70897(12) 0.0428(5) Uani 1 1 d . . .
H45 H 0.5334 0.8034 0.7455 0.051 Uiso 1 1 calc R . .
C46 C 0.52226(15) 0.76122(10) 0.63614(12) 0.0348(4) Uani 1 1 d . . .
H46 H 0.5764 0.792 0.6226 0.042 Uiso 1 1 calc R . .
C47 C 0.50281(13) 0.70098(10) 0.50629(10) 0.0265(4) Uani 1 1 d . . .
C48 C 0.51347(14) 0.75830(10) 0.45188(11) 0.0295(4) Uani 1 1 d . . .
C49 C 0.55459(14) 0.72257(10) 0.39257(11) 0.0295(4) Uani 1 1 d . . .
C50 C 0.57079(17) 0.76256(12) 0.32673(12) 0.0412(5) Uani 1 1 d . . .
C51 C 0.54608(19) 0.83639(13) 0.32292(13) 0.0502(6) Uani 1 1 d . . .
C52 C 0.50583(18) 0.87219(12) 0.38173(14) 0.0492(6) Uani 1 1 d . . .
C53 C 0.48918(15) 0.83438(11) 0.44548(12) 0.0378(5) Uani 1 1 d . . .
N1 N 0.49118(11) 0.49334(8) 0.35955(8) 0.0269(3) Uani 1 1 d . . .
N2 N 0.56681(11) 0.53134(8) 0.32899(8) 0.0267(3) Uani 1 1 d . . .
N3 N 0.69806(11) 0.50974(8) 0.49873(8) 0.0268(3) Uani 1 1 d . . .
N4 N 0.72357(11) 0.55872(8) 0.44458(8) 0.0274(3) Uani 1 1 d . . .
N5 N 0.53339(11) 0.63655(8) 0.48053(8) 0.0261(3) Uani 1 1 d . . .
N6 N 0.56737(12) 0.64902(8) 0.41125(8) 0.0282(3) Uani 1 1 d . . .
Ca1 Ca 0.5 0.5 0.5 0.02455(12) Uani 1 2 d S . .
F10 F 0.31504(8) 0.38785(6) 0.36401(6) 0.0357(3) Uani 1 1 d . . .
F11 F 0.22193(9) 0.32273(7) 0.22711(7) 0.0508(3) Uani 1 1 d . . .
F12 F 0.29420(11) 0.34553(8) 0.09528(7) 0.0609(4) Uani 1 1 d . . .
F13 F 0.46288(10) 0.43924(7) 0.09368(6) 0.0533(3) Uani 1 1 d . . .
F29 F 1.02522(9) 0.51511(7) 0.64092(7) 0.0525(3) Uani 1 1 d . . .
F30 F 1.14570(9) 0.61232(9) 0.57755(9) 0.0731(5) Uani 1 1 d . . .
F31 F 1.06124(11) 0.68720(9) 0.44631(10) 0.0754(5) Uani 1 1 d . . .
F32 F 0.85763(10) 0.66687(7) 0.36994(8) 0.0567(4) Uani 1 1 d . . .
F50 F 0.60579(12) 0.73092(7) 0.26733(7) 0.0630(4) Uani 1 1 d . . .
F51 F 0.55902(14) 0.87625(8) 0.26032(9) 0.0809(5) Uani 1 1 d . . .
F52 F 0.48273(13) 0.94526(7) 0.37297(10) 0.0766(5) Uani 1 1 d . . .
F53 F 0.44948(10) 0.87008(6) 0.50061(8) 0.0517(3) Uani 1 1 d . . .
B1 B 0.63814(16) 0.59235(12) 0.37728(12) 0.0285(4) Uani 1 1 d . . .
H1 H 0.6766 0.6196 0.3413 0.034 Uiso 1 1 calc R . .
O1 O 0.7829(3) 0.3485(3) -0.0526(3) 0.0590(13) Uani 0.5 1 d P A 1
C61 C 0.6615(4) 0.3317(3) 0.0331(4) 0.0638(14) Uani 0.5 1 d P A 1
H61A H 0.5835 0.3225 0.0282 0.077 Uiso 0.5 1 calc PR A 1
H61B H 0.7007 0.3088 0.0824 0.077 Uiso 0.5 1 calc PR A 1
C62 C 0.6835(9) 0.4133(7) 0.0333(6) 0.080(3) Uani 0.5 1 d P A 1
H62A H 0.7292 0.4298 0.0835 0.096 Uiso 0.5 1 calc PR A 1
H62B H 0.6162 0.4427 0.0224 0.096 Uiso 0.5 1 calc PR A 1
C63 C 0.7442(5) 0.4179(4) -0.0349(5) 0.0572(15) Uani 0.5 1 d P A 1
H63A H 0.6951 0.4378 -0.082 0.069 Uiso 0.5 1 calc PR A 1
H63B H 0.8054 0.4528 -0.0205 0.069 Uiso 0.5 1 calc PR A 1
C64 C 0.7019(10) 0.2977(10) -0.0401(7) 0.071(3) Uani 0.5 1 d P A 1
H64A H 0.7322 0.2474 -0.0281 0.085 Uiso 0.5 1 calc PR A 1
H64B H 0.6423 0.2949 -0.0866 0.085 Uiso 0.5 1 calc PR A 1
O2 O 0.7135(6) 0.3501(4) -0.0574(3) 0.0878(17) Uani 0.5 1 d P B 2
C71 C 0.7154(9) 0.4030(7) 0.0101(5) 0.092(3) Uani 0.5 1 d P B 2
H71A H 0.6428 0.4217 0.0124 0.11 Uiso 0.5 1 calc PR B 2
H71B H 0.75 0.381 0.0611 0.11 Uiso 0.5 1 calc PR B 2
C72 C 0.7824(8) 0.4600(6) -0.0158(6) 0.120(3) Uani 0.5 1 d P B 2
H72A H 0.848 0.4371 -0.0263 0.18 Uiso 0.5 1 calc PR B 2
H72B H 0.8019 0.4976 0.0253 0.18 Uiso 0.5 1 calc PR B 2
H72C H 0.7423 0.4834 -0.0637 0.18 Uiso 0.5 1 calc PR B 2
C73 C 0.6639(12) 0.2889(11) -0.0332(10) 0.108(5) Uani 0.5 1 d P B 2
H73A H 0.5999 0.3034 -0.0125 0.129 Uiso 0.5 1 calc PR B 2
H73B H 0.7142 0.2608 0.0076 0.129 Uiso 0.5 1 calc PR B 2
C74 C 0.6293(7) 0.2400(4) -0.1149(6) 0.121(3) Uani 0.5 1 d P B 2
H74A H 0.5787 0.2688 -0.1538 0.181 Uiso 0.5 1 calc PR B 2
H74B H 0.595 0.1936 -0.1038 0.181 Uiso 0.5 1 calc PR B 2
H74C H 0.6936 0.2287 -0.1355 0.181 Uiso 0.5 1 calc PR B 2



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 1.385(3) . ?
C1 C6 1.388(3) . ?
C1 C7 1.479(3) . ?
C2 C3 1.387(3) . ?
C2 H2 0.95 . ?
C3 C4 1.368(4) . ?
C3 H3 0.95 . ?
C4 C5 1.373(4) . ?
C4 H4 0.95 . ?
C5 C6 1.388(3) . ?
C5 H5 0.95 . ?
C6 H6 0.95 . ?
C7 N2 1.357(2) . ?
C7 C8 1.404(3) . ?
C8 C13 1.410(2) . ?
C8 C9 1.418(2) . ?
C9 N1 1.351(2) . ?
C9 C10 1.404(2) . ?
C10 F10 1.349(2) . ?
C10 C11 1.353(3) . ?
C11 F11 1.346(2) . ?
C11 C12 1.412(3) . ?
C12 F12 1.347(2) . ?
C12 C13 1.351(3) . ?
C13 F13 1.347(2) . ?
C21 C26 1.391(3) . ?
C21 C22 1.398(3) . ?
C21 C27 1.471(3) . ?
C22 C23 1.385(3) . ?
C22 H22 0.95 . ?
C23 C24 1.379(3) . ?
C23 H23 0.95 . ?
C24 C25 1.378(3) . ?
C24 H24 0.95 . ?
C25 C26 1.381(3) . ?
C25 H25 0.95 . ?
C26 H26 0.95 . ?
C27 N3 1.334(2) . ?
C27 C28 1.425(3) . ?
C28 C29 1.407(3) . ?
C28 C33 1.407(3) . ?
C29 F29 1.344(2) . ?
C29 C30 1.356(3) . ?
C30 F30 1.345(2) . ?
C30 C31 1.398(3) . ?
C31 F31 1.348(2) . ?
C31 C32 1.363(3) . ?
C32 F32 1.347(2) . ?
C32 C33 1.407(3) . ?
C33 N4 1.368(2) . ?
C41 C42 1.392(3) . ?
C41 C46 1.398(3) . ?
C41 C47 1.481(2) . ?
C42 C43 1.389(3) . ?
C42 H42 0.95 . ?
C43 C44 1.382(3) . ?
C43 H43 0.95 . ?
C44 C45 1.381(3) . ?
C44 H44 0.95 . ?
C45 C46 1.385(3) . ?
C45 H45 0.95 . ?
C46 H46 0.95 . ?
C47 N5 1.331(2) . ?
C47 C48 1.428(2) . ?
C48 C53 1.404(3) . ?
C48 C49 1.408(3) . ?
C49 N6 1.366(2) . ?
C49 C50 1.407(3) . ?
C50 F50 1.337(2) . ?
C50 C51 1.365(3) . ?
C51 F51 1.345(2) . ?
C51 C52 1.396(3) . ?
C52 F52 1.350(2) . ?
C52 C53 1.358(3) . ?
C53 F53 1.339(2) . ?
N1 N2 1.3740(19) . ?
N1 Ca1 2.4328(14) . ?
N2 B1 1.556(3) . ?
N3 N4 1.379(2) . ?
N3 Ca1 2.5252(14) . ?
N4 B1 1.547(2) . ?
N5 N6 1.3837(19) . ?
N5 Ca1 2.5311(14) . ?
N6 B1 1.556(3) . ?
Ca1 N1 2.4328(14) 3_666 ?
Ca1 N3 2.5252(14) 3_666 ?
Ca1 N5 2.5311(14) 3_666 ?
B1 H1 1 . ?
O1 C63 1.401(8) . ?
O1 C64 1.428(14) . ?
C61 C62 1.497(14) . ?
C61 C64 1.594(13) . ?
C61 H61A 0.99 . ?
C61 H61B 0.99 . ?
C62 C63 1.548(9) . ?
C62 H62A 0.99 . ?
C62 H62B 0.99 . ?
C63 H63A 0.99 . ?
C63 H63B 0.99 . ?
C64 H64A 0.99 . ?
C64 H64B 0.99 . ?
O2 C73 1.379(17) . ?
O2 C71 1.512(12) . ?
C71 C72 1.463(15) . ?
C71 H71A 0.99 . ?
C71 H71B 0.99 . ?
C72 H72A 0.98 . ?
C72 H72B 0.98 . ?
C72 H72C 0.98 . ?
C73 C74 1.656(19) . ?
C73 H73A 0.99 . ?
C73 H73B 0.99 . ?
C74 H74A 0.98 . ?
C74 H74B 0.98 . ?
C74 H74C 0.98 . ?

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 119.84(19) . . ?
C2 C1 C7 119.44(18) . . ?
C6 C1 C7 120.72(18) . . ?
C1 C2 C3 119.8(2) . . ?
C1 C2 H2 120.1 . . ?
C3 C2 H2 120.1 . . ?
C4 C3 C2 120.2(3) . . ?
C4 C3 H3 119.9 . . ?
C2 C3 H3 119.9 . . ?
C3 C4 C5 120.5(2) . . ?
C3 C4 H4 119.8 . . ?
C5 C4 H4 119.8 . . ?
C4 C5 C6 120.2(2) . . ?
C4 C5 H5 119.9 . . ?
C6 C5 H5 119.9 . . ?
C1 C6 C5 119.5(2) . . ?
C1 C6 H6 120.2 . . ?
C5 C6 H6 120.2 . . ?
N2 C7 C8 107.01(15) . . ?
N2 C7 C1 123.29(16) . . ?
C8 C7 C1 129.69(16) . . ?
C7 C8 C13 135.79(17) . . ?
C7 C8 C9 104.63(15) . . ?
C13 C8 C9 119.54(17) . . ?
N1 C9 C10 128.89(16) . . ?
N1 C9 C8 111.31(15) . . ?
C10 C9 C8 119.78(16) . . ?
F10 C10 C11 120.12(16) . . ?
F10 C10 C9 120.95(15) . . ?
C11 C10 C9 118.93(17) . . ?
F11 C11 C10 119.98(18) . . ?
F11 C11 C12 118.37(17) . . ?
C10 C11 C12 121.65(17) . . ?
F12 C12 C13 121.64(18) . . ?
F12 C12 C11 117.74(18) . . ?
C13 C12 C11 120.62(17) . . ?
F13 C13 C12 120.02(17) . . ?
F13 C13 C8 120.55(17) . . ?
C12 C13 C8 119.43(18) . . ?
C26 C21 C22 118.65(19) . . ?
C26 C21 C27 120.59(17) . . ?
C22 C21 C27 120.66(17) . . ?
C23 C22 C21 120.2(2) . . ?
C23 C22 H22 119.9 . . ?
C21 C22 H22 119.9 . . ?
C24 C23 C22 120.2(2) . . ?
C24 C23 H23 119.9 . . ?
C22 C23 H23 119.9 . . ?
C25 C24 C23 120.0(2) . . ?
C25 C24 H24 120 . . ?
C23 C24 H24 120 . . ?
C24 C25 C26 120.2(2) . . ?
C24 C25 H25 119.9 . . ?
C26 C25 H25 119.9 . . ?
C25 C26 C21 120.6(2) . . ?
C25 C26 H26 119.7 . . ?
C21 C26 H26 119.7 . . ?
N3 C27 C28 109.28(16) . . ?
N3 C27 C21 121.08(16) . . ?
C28 C27 C21 129.49(16) . . ?
C29 C28 C33 119.95(18) . . ?
C29 C28 C27 135.11(19) . . ?
C33 C28 C27 104.91(15) . . ?
F29 C29 C30 119.37(18) . . ?
F29 C29 C28 121.28(19) . . ?
C30 C29 C28 119.3(2) . . ?
F30 C30 C29 121.0(2) . . ?
F30 C30 C31 118.4(2) . . ?
C29 C30 C31 120.53(19) . . ?
F31 C31 C32 119.6(2) . . ?
F31 C31 C30 118.5(2) . . ?
C32 C31 C30 121.9(2) . . ?
F32 C32 C31 118.74(19) . . ?
F32 C32 C33 122.71(18) . . ?
C31 C32 C33 118.5(2) . . ?
N4 C33 C28 108.41(16) . . ?
N4 C33 C32 131.92(18) . . ?
C28 C33 C32 119.68(17) . . ?
C42 C41 C46 118.66(17) . . ?
C42 C41 C47 122.59(16) . . ?
C46 C41 C47 118.74(16) . . ?
C43 C42 C41 120.52(18) . . ?
C43 C42 H42 119.7 . . ?
C41 C42 H42 119.7 . . ?
C44 C43 C42 120.22(19) . . ?
C44 C43 H43 119.9 . . ?
C42 C43 H43 119.9 . . ?
C45 C44 C43 119.79(19) . . ?
C45 C44 H44 120.1 . . ?
C43 C44 H44 120.1 . . ?
C44 C45 C46 120.38(19) . . ?
C44 C45 H45 119.8 . . ?
C46 C45 H45 119.8 . . ?
C45 C46 C41 120.42(18) . . ?
C45 C46 H46 119.8 . . ?
C41 C46 H46 119.8 . . ?
N5 C47 C48 109.36(15) . . ?
N5 C47 C41 123.01(16) . . ?
C48 C47 C41 127.55(16) . . ?
C53 C48 C49 119.78(17) . . ?
C53 C48 C47 135.16(18) . . ?
C49 C48 C47 105.00(15) . . ?
N6 C49 C50 131.39(18) . . ?
N6 C49 C48 108.18(15) . . ?
C50 C49 C48 120.36(17) . . ?
F50 C50 C51 119.18(18) . . ?
F50 C50 C49 122.90(18) . . ?
C51 C50 C49 117.88(19) . . ?
F51 C51 C50 119.6(2) . . ?
F51 C51 C52 118.4(2) . . ?
C50 C51 C52 122.01(19) . . ?
F52 C52 C53 121.0(2) . . ?
F52 C52 C51 118.1(2) . . ?
C53 C52 C51 120.90(19) . . ?
F53 C53 C52 119.55(18) . . ?
F53 C53 C48 121.39(18) . . ?
C52 C53 C48 119.06(19) . . ?
C9 N1 N2 104.87(13) . . ?
C9 N1 Ca1 136.22(11) . . ?
N2 N1 Ca1 118.46(10) . . ?
C7 N2 N1 112.16(14) . . ?
C7 N2 B1 126.09(15) . . ?
N1 N2 B1 121.12(13) . . ?
C27 N3 N4 108.88(14) . . ?
C27 N3 Ca1 130.81(12) . . ?
N4 N3 Ca1 115.23(10) . . ?
C33 N4 N3 108.51(14) . . ?
C33 N4 B1 127.65(15) . . ?
N3 N4 B1 122.89(13) . . ?
C47 N5 N6 108.60(14) . . ?
C47 N5 Ca1 137.17(11) . . ?
N6 N5 Ca1 111.49(10) . . ?
C49 N6 N5 108.83(14) . . ?
C49 N6 B1 126.50(15) . . ?
N5 N6 B1 122.38(14) . . ?
N1 Ca1 N1 180 . 3_666 ?
N1 Ca1 N3 80.34(5) . . ?
N1 Ca1 N3 99.66(5) 3_666 . ?
N1 Ca1 N3 99.66(5) . 3_666 ?
N1 Ca1 N3 80.34(5) 3_666 3_666 ?
N3 Ca1 N3 180 . 3_666 ?
N1 Ca1 N5 83.50(5) . . ?
N1 Ca1 N5 96.50(5) 3_666 . ?
N3 Ca1 N5 74.72(5) . . ?
N3 Ca1 N5 105.28(5) 3_666 . ?
N1 Ca1 N5 96.50(5) . 3_666 ?
N1 Ca1 N5 83.50(5) 3_666 3_666 ?
N3 Ca1 N5 105.28(5) . 3_666 ?
N3 Ca1 N5 74.72(5) 3_666 3_666 ?
N5 Ca1 N5 180 . 3_666 ?
N4 B1 N2 111.83(15) . . ?
N4 B1 N6 109.70(14) . . ?
N2 B1 N6 110.64(14) . . ?
N4 B1 H1 108.2 . . ?
N2 B1 H1 108.2 . . ?
N6 B1 H1 108.2 . . ?
C63 O1 C64 104.0(7) . . ?
C62 C61 C64 106.8(7) . . ?
C62 C61 H61A 110.4 . . ?
C64 C61 H61A 110.4 . . ?
C62 C61 H61B 110.4 . . ?
C64 C61 H61B 110.4 . . ?
H61A C61 H61B 108.6 . . ?
C61 C62 C63 100.0(6) . . ?
C61 C62 H62A 111.8 . . ?
C63 C62 H62A 111.8 . . ?
C61 C62 H62B 111.8 . . ?
C63 C62 H62B 111.8 . . ?
H62A C62 H62B 109.5 . . ?
O1 C63 C62 112.0(6) . . ?
O1 C63 H63A 109.2 . . ?
C62 C63 H63A 109.2 . . ?
O1 C63 H63B 109.2 . . ?
C62 C63 H63B 109.2 . . ?
H63A C63 H63B 107.9 . . ?
O1 C64 C61 103.7(9) . . ?
O1 C64 H64A 111 . . ?
C61 C64 H64A 111 . . ?
O1 C64 H64B 111 . . ?
C61 C64 H64B 111 . . ?
H64A C64 H64B 109 . . ?
C73 O2 C71 101.5(10) . . ?
C72 C71 O2 96.8(8) . . ?
C72 C71 H71A 112.4 . . ?
O2 C71 H71A 112.4 . . ?
C72 C71 H71B 112.4 . . ?
O2 C71 H71B 112.4 . . ?
H71A C71 H71B 110 . . ?
C71 C72 H72A 109.5 . . ?
C71 C72 H72B 109.5 . . ?
H72A C72 H72B 109.5 . . ?
C71 C72 H72C 109.5 . . ?
H72A C72 H72C 109.5 . . ?
H72B C72 H72C 109.5 . . ?
O2 C73 C74 102.6(10) . . ?
O2 C73 H73A 111.3 . . ?
C74 C73 H73A 111.3 . . ?
O2 C73 H73B 111.3 . . ?
C74 C73 H73B 111.3 . . ?
H73A C73 H73B 109.2 . . ?
C73 C74 H74A 109.5 . . ?
C73 C74 H74B 109.5 . . ?
H74A C74 H74B 109.5 . . ?
C73 C74 H74C 109.5 . . ?
H74A C74 H74C 109.5 . . ?
H74B C74 H74C 109.5 . . ?

#===END


_database_code_depnum_ccdc_archive 'CCDC 981307'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_3

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         '4(C24 B F21 N6), 2(C24 H48 Ca O6), 3(C6 H12)'
_chemical_formula_sum            'C162 H132 B4 Ca2 F84 N24 O12'
_chemical_formula_weight         4326.32
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           TRIGONAL
_symmetry_space_group_name_H-M   'R -3 c'
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_Int_Tables_number      167
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'y, x, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'y+2/3, x+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'y+1/3, x+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-y, -x, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-y+2/3, -x+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'
'-y+1/3, -x+2/3, z+1/6'

_cell_length_a                   19.6190(5)
_cell_length_b                   19.6190(5)
_cell_length_c                   81.338(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     27112.9(14)
_cell_formula_units_Z            6
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    6362
_cell_measurement_theta_min      3.3869
_cell_measurement_theta_max      40.7788
_cell_measurement_wavelength     1.54184

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_exptl_crystal_density_diffrn    1.59
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             13104
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    1.926
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
        (compiled Jan 23 2012,18:06:46)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.6532
_exptl_absorpt_correction_T_max  0.8782

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      180(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_detector_area_resol_mean 16.1978
_diffrn_orient_matrix_ub_11      -0.0237796
_diffrn_orient_matrix_ub_12      0.0206969
_diffrn_orient_matrix_ub_13      0.016509
_diffrn_orient_matrix_ub_21      0.0802417
_diffrn_orient_matrix_ub_22      0.0765406
_diffrn_orient_matrix_ub_23      0.0008838
_diffrn_orient_matrix_ub_31      -0.0348687
_diffrn_orient_matrix_ub_32      0.0439969
_diffrn_orient_matrix_ub_33      -0.0092574
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_av_R_equivalents  0.0355
_diffrn_reflns_av_unetI/netI     0.0262
_diffrn_reflns_number            16169
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -68
_diffrn_reflns_limit_l_max       63
_diffrn_reflns_theta_min         3.39
_diffrn_reflns_theta_max         40.82
_diffrn_reflns_theta_full        40.82
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_reflns_number_total             1902
_reflns_number_gt                1552
_reflns_threshold_expression     >2σ(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
        (compiled Jan 23 2012,18:06:46)
;
_computing_cell_refinement       
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
        (compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction        
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
        (compiled Jan 23 2012,18:06:46)
;
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0866P)²+181.1944P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         1902
_refine_ls_number_parameters     434
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0664
_refine_ls_R_factor_gt           0.0527
_refine_ls_wR_factor_ref         0.1472
_refine_ls_wR_factor_gt          0.134
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_restrained_S_all      1.035
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.491
_refine_diff_density_min         -0.273
_refine_diff_density_rms         0.052

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.009 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.3641 1.2855 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 1.0310(6) 0.2656(6) 0.53284(14) 0.058(3) Uani 1 1 d . . .
C2 C 1.0423(6) 0.2044(8) 0.53792(13) 0.040(2) Uani 1 1 d . . .
C3 C 0.9994(6) 0.1311(7) 0.53055(12) 0.036(2) Uani 1 1 d . . .
C4 C 0.9439(6) 0.1184(6) 0.51836(13) 0.045(2) Uani 1 1 d . . .
C5 C 0.9344(6) 0.1798(9) 0.51378(11) 0.060(3) Uani 1 1 d . . .
C6 C 0.9782(8) 0.2530(7) 0.52098(17) 0.068(3) Uani 1 1 d . . .
C7 C 1.0903(5) 0.1965(6) 0.54960(11) 0.040(2) Uani 1 1 d . . .
C8 C 1.1491(7) 0.2522(7) 0.56061(14) 0.080(3) Uani 1 1 d . . .
C21 C 0.6329(6) 0.1491(6) 0.52435(10) 0.050(2) Uani 1 1 d . . .
C22 C 0.7016(6) 0.1691(8) 0.53318(12) 0.051(3) Uani 1 1 d . . .
C23 C 0.7263(7) 0.2423(7) 0.54033(11) 0.041(2) Uani 1 1 d . . .
C24 C 0.7934(8) 0.2755(6) 0.55015(12) 0.056(2) Uani 1 1 d . . .
C25 C 0.8351(6) 0.2383(9) 0.55258(11) 0.063(2) Uani 1 1 d . . .
C26 C 0.8096(8) 0.1651(10) 0.54565(15) 0.064(3) Uani 1 1 d . . .
C28 C 0.5802(7) 0.0786(6) 0.51500(15) 0.072(3) Uani 1 1 d . . .
O1 O 1.3061(3) 0.5596(2) 0.52768(5) 0.0439(13) Uani 1 1 d . . .
C52 C 1.3295(5) 0.5015(5) 0.53048(10) 0.068(2) Uani 1 1 d . . .
H52A H 1.3226 0.4858 0.5422 0.081 Uiso 1 1 calc R . .
H52B H 1.3854 0.5228 0.5275 0.081 Uiso 1 1 calc R . .
C53 C 1.2774(5) 0.4326(4) 0.51983(10) 0.068(2) Uani 1 1 d . . .
H53A H 1.3073 0.4089 0.5151 0.081 Uiso 1 1 calc R . .
H53B H 1.2327 0.392 0.5263 0.081 Uiso 1 1 calc R . .
C54 C 1.2496(6) 0.4638(6) 0.50690(12) 0.098(3) Uani 1 1 d . . .
H54A H 1.28 0.4713 0.4967 0.117 Uiso 1 1 calc R . .
H54B H 1.1933 0.4269 0.5046 0.117 Uiso 1 1 calc R . .
C55 C 1.2606(5) 0.5386(5) 0.51269(10) 0.070(3) Uani 1 1 d . . .
H55A H 1.2886 0.5798 0.5043 0.084 Uiso 1 1 calc R . .
H55B H 1.2089 0.5343 0.5148 0.084 Uiso 1 1 calc R . .
O2 O 1.4171(3) 0.6423(3) 0.56088(5) 0.0506(14) Uani 1 1 d . . .
C57 C 1.4981(5) 0.6662(5) 0.55752(11) 0.082(3) Uani 1 1 d . . .
H57A H 1.5329 0.7214 0.561 0.098 Uiso 1 1 calc R . .
H57B H 1.5058 0.662 0.5456 0.098 Uiso 1 1 calc R . .
C58 C 1.5161(6) 0.6132(7) 0.56691(15) 0.114(4) Uani 1 1 d . . .
H58A H 1.5079 0.5678 0.5601 0.136 Uiso 1 1 calc R . .
H58B H 1.5713 0.6413 0.5708 0.136 Uiso 1 1 calc R . .
C59 C 1.4621(7) 0.5876(7) 0.58051(15) 0.138(5) Uani 1 1 d . . .
H59A H 1.4883 0.6198 0.5904 0.166 Uiso 1 1 calc R . .
H59B H 1.4441 0.5318 0.5831 0.166 Uiso 1 1 calc R . .
C60 C 1.3959(5) 0.5965(5) 0.57594(10) 0.084(3) Uani 1 1 d . . .
H60A H 1.3842 0.6239 0.5848 0.1 Uiso 1 1 calc R . .
H60B H 1.3487 0.5443 0.5742 0.1 Uiso 1 1 calc R . .
N1 N 1.0780(4) 0.1234(5) 0.54960(7) 0.0425(16) Uani 1 1 d . . .
N2 N 1.0223(4) 0.0827(4) 0.53793(9) 0.0350(16) Uani 1 1 d . . .
N3 N 0.6179(4) 0.2071(5) 0.52590(8) 0.0470(17) Uani 1 1 d . . .
N4 N 0.6739(6) 0.2639(4) 0.53564(9) 0.0455(19) Uani 1 1 d . . .
F1 F 1.0691(3) 0.3384(3) 0.53940(6) 0.0850(15) Uani 1 1 d . . .
F4 F 0.9004(3) 0.0466(3) 0.51182(5) 0.0615(13) Uani 1 1 d . . .
F5 F 0.8807(3) 0.1654(3) 0.50186(6) 0.0906(16) Uani 1 1 d . . .
F6 F 0.9619(3) 0.3083(3) 0.51547(6) 0.1020(18) Uani 1 1 d . . .
F8 F 1.1181(4) 0.2894(4) 0.56941(9) 0.167(3) Uani 1 1 d . . .
F9 F 1.2064(4) 0.3136(3) 0.55374(7) 0.138(3) Uani 1 1 d . . .
F10 F 1.1768(4) 0.2271(3) 0.57142(8) 0.152(3) Uani 1 1 d . . .
F11 F 0.6162(4) 0.0631(3) 0.50342(8) 0.129(2) Uani 1 1 d . . .
F12 F 0.5480(3) 0.0151(3) 0.52418(7) 0.119(2) Uani 1 1 d . . .
F13 F 0.5237(4) 0.0837(3) 0.50792(7) 0.122(2) Uani 1 1 d . . .
F24 F 0.8186(3) 0.3465(3) 0.55710(5) 0.0761(14) Uani 1 1 d . . .
F25 F 0.8997(3) 0.2708(3) 0.56209(6) 0.0938(16) Uani 1 1 d . . .
F26 F 0.8520(3) 0.1288(3) 0.54935(5) 0.0937(16) Uani 1 1 d . . .
Ca1 Ca 1.3333 0.6667 0.54458(3) 0.0323(8) Uani 1 3 d S . .
B1 B 1 0 0.53150(18) 0.037(4) Uani 1 3 d S . .
B2 B 0.6667 0.3333 0.5425(2) 0.046(4) Uani 1 3 d S . .
F27 F 0.7232(3) 0.0581(3) 0.52969(6) 0.0865(15) Uani 1 1 d . . .
C27 C 0.7430(9) 0.1306(6) 0.53606(12) 0.065(3) Uani 1 1 d . . .
C100 C 0.8300(11) 0.4967(11) 0.5833 0.144(7) Uani 1 2 d S . .
H10A H 0.7871 0.4805 0.5752 0.173 Uiso 0.5 1 calc PR . .
H10B H 0.8139 0.4537 0.5915 0.173 Uiso 0.5 1 calc PR . .
C101 C 0.9010(9) 0.5107(11) 0.5751(2) 0.179(8) Uani 1 1 d . . .
H10C H 0.9024 0.461 0.5744 0.215 Uiso 1 1 calc R . .
H10D H 0.9021 0.5298 0.5638 0.215 Uiso 1 1 calc R . .
C104 C 0.9581(12) 0.6248(12) 0.5833 0.28(2) Uani 1 2 d SD . .
H10E H 0.9891 0.6538 0.5931 0.332 Uiso 0.5 1 calc PR . .
H10F H 0.9872 0.6558 0.5736 0.332 Uiso 0.5 1 calc PR . .
C103 C 0.9578(12) 0.5595(11) 0.5828(2) 0.219(9) Uani 1 1 d D . .
H10G H 1.0066 0.5676 0.5774 0.263 Uiso 1 1 calc R . .
H10H H 0.9563 0.5402 0.5941 0.263 Uiso 1 1 calc R . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 1.344(11) . ?
C1 F1 1.347(9) . ?
C1 C2 1.388(11) . ?
C2 C3 1.388(9) . ?
C2 C7 1.401(10) . ?
C3 N2 1.374(9) . ?
C3 C4 1.399(10) . ?
C4 F4 1.340(9) . ?
C4 C5 1.361(11) . ?
C5 F5 1.353(9) . ?
C5 C6 1.381(12) . ?
C6 F6 1.354(10) . ?
C7 N1 1.330(8) . ?
C7 C8 1.438(12) . ?
C8 F10 1.256(10) . ?
C8 F9 1.293(10) . ?
C8 F8 1.363(11) . ?
C21 N3 1.317(9) . ?
C21 C22 1.399(11) . ?
C21 C28 1.459(12) . ?
C22 C27 1.380(13) . ?
C22 C23 1.391(10) . ?
C23 N4 1.348(10) . ?
C23 C24 1.392(12) . ?
C24 F24 1.347(10) . ?
C24 C25 1.357(11) . ?
C25 F25 1.343(9) . ?
C25 C26 1.382(12) . ?
C26 F26 1.373(9) . ?
C26 C27 1.375(12) . ?
C28 F13 1.296(10) . ?
C28 F11 1.302(10) . ?
C28 F12 1.313(10) . ?
O1 C55 1.444(8) . ?
O1 C52 1.444(8) . ?
O1 Ca1 2.337(4) . ?
C52 C53 1.496(10) . ?
C52 H52A 0.99 . ?
C52 H52B 0.99 . ?
C53 C54 1.453(10) . ?
C53 H53A 0.99 . ?
C53 H53B 0.99 . ?
C54 C55 1.452(10) . ?
C54 H54A 0.99 . ?
C54 H54B 0.99 . ?
C55 H55A 0.99 . ?
C55 H55B 0.99 . ?
O2 C57 1.441(9) . ?
O2 C60 1.452(8) . ?
O2 Ca1 2.339(4) . ?
C57 C58 1.470(11) . ?
C57 H57A 0.99 . ?
C57 H57B 0.99 . ?
C58 C59 1.437(12) . ?
C58 H58A 0.99 . ?
C58 H58B 0.99 . ?
C59 C60 1.442(11) . ?
C59 H59A 0.99 . ?
C59 H59B 0.99 . ?
C60 H60A 0.99 . ?
C60 H60B 0.99 . ?
N1 N2 1.364(7) . ?
N2 B1 1.546(8) . ?
N3 N4 1.360(7) . ?
N4 B2 1.543(9) . ?
Ca1 O1 2.337(4) 3_775 ?
Ca1 O1 2.337(4) 2_755 ?
Ca1 O2 2.339(4) 2_755 ?
Ca1 O2 2.339(4) 3_775 ?
B1 N2 1.546(8) 2_645 ?
B1 N2 1.546(8) 3_765 ?
B2 N4 1.543(9) 2_655 ?
B2 N4 1.543(9) 3_665 ?
F27 C27 1.375(10) . ?
C100 C101 1.441(17) 18_545 ?
C100 C101 1.441(17) . ?
C100 H10A 0.99 . ?
C100 H10B 0.99 . ?
C101 C103 1.22(2) . ?
C101 H10C 0.99 . ?
C101 H10D 0.99 . ?
C104 C103 1.278(15) 18_545 ?
C104 C103 1.278(15) . ?
C104 H10E 0.99 . ?
C104 H10F 0.99 . ?
C103 H10G 0.99 . ?
C103 H10H 0.99 . ?

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 F1 116.7(13) . . ?
C6 C1 C2 119.7(9) . . ?
F1 C1 C2 123.6(13) . . ?
C3 C2 C1 119.5(11) . . ?
C3 C2 C7 105.7(9) . . ?
C1 C2 C7 134.9(14) . . ?
N2 C3 C2 106.9(9) . . ?
N2 C3 C4 132.8(11) . . ?
C2 C3 C4 120.3(10) . . ?
F4 C4 C5 121.7(12) . . ?
F4 C4 C3 119.9(11) . . ?
C5 C4 C3 118.4(8) . . ?
F5 C5 C4 116.6(13) . . ?
F5 C5 C6 122.5(13) . . ?
C4 C5 C6 120.9(8) . . ?
C1 C6 F6 124.0(13) . . ?
C1 C6 C5 121.2(9) . . ?
F6 C6 C5 114.8(14) . . ?
N1 C7 C2 110.5(8) . . ?
N1 C7 C8 117.7(11) . . ?
C2 C7 C8 131.8(12) . . ?
F10 C8 F9 108.8(10) . . ?
F10 C8 F8 103.7(9) . . ?
F9 C8 F8 98.2(9) . . ?
F10 C8 C7 118.5(9) . . ?
F9 C8 C7 115.7(9) . . ?
F8 C8 C7 109.3(10) . . ?
N3 C21 C22 107.9(9) . . ?
N3 C21 C28 120.7(11) . . ?
C22 C21 C28 131.4(13) . . ?
C27 C22 C23 119.8(11) . . ?
C27 C22 C21 133.0(15) . . ?
C23 C22 C21 107.2(10) . . ?
N4 C23 C22 106.2(10) . . ?
N4 C23 C24 134.9(12) . . ?
C22 C23 C24 119.0(11) . . ?
F24 C24 C25 119.2(14) . . ?
F24 C24 C23 119.9(13) . . ?
C25 C24 C23 121.0(9) . . ?
F25 C25 C24 120.6(15) . . ?
F25 C25 C26 119.6(15) . . ?
C24 C25 C26 119.8(9) . . ?
F26 C26 C27 122.7(16) . . ?
F26 C26 C25 116.9(15) . . ?
C27 C26 C25 120.4(9) . . ?
F13 C28 F11 106.4(10) . . ?
F13 C28 F12 107.7(9) . . ?
F11 C28 F12 104.4(9) . . ?
F13 C28 C21 112.8(9) . . ?
F11 C28 C21 112.8(9) . . ?
F12 C28 C21 112.3(9) . . ?
C55 O1 C52 107.7(5) . . ?
C55 O1 Ca1 125.7(4) . . ?
C52 O1 Ca1 126.6(4) . . ?
O1 C52 C53 106.2(6) . . ?
O1 C52 H52A 110.5 . . ?
C53 C52 H52A 110.5 . . ?
O1 C52 H52B 110.5 . . ?
C53 C52 H52B 110.5 . . ?
H52A C52 H52B 108.7 . . ?
C54 C53 C52 105.6(6) . . ?
C54 C53 H53A 110.6 . . ?
C52 C53 H53A 110.6 . . ?
C54 C53 H53B 110.6 . . ?
C52 C53 H53B 110.6 . . ?
H53A C53 H53B 108.7 . . ?
C55 C54 C53 107.1(7) . . ?
C55 C54 H54A 110.3 . . ?
C53 C54 H54A 110.3 . . ?
C55 C54 H54B 110.3 . . ?
C53 C54 H54B 110.3 . . ?
H54A C54 H54B 108.6 . . ?
O1 C55 C54 108.7(6) . . ?
O1 C55 H55A 110 . . ?
C54 C55 H55A 110 . . ?
O1 C55 H55B 110 . . ?
C54 C55 H55B 110 . . ?
H55A C55 H55B 108.3 . . ?
C57 O2 C60 106.8(5) . . ?
C57 O2 Ca1 126.8(5) . . ?
C60 O2 Ca1 126.3(5) . . ?
O2 C57 C58 106.8(7) . . ?
O2 C57 H57A 110.4 . . ?
C58 C57 H57A 110.4 . . ?
O2 C57 H57B 110.4 . . ?
C58 C57 H57B 110.4 . . ?
H57A C57 H57B 108.6 . . ?
C59 C58 C57 104.5(8) . . ?
C59 C58 H58A 110.9 . . ?
C57 C58 H58A 110.9 . . ?
C59 C58 H58B 110.9 . . ?
C57 C58 H58B 110.9 . . ?
H58A C58 H58B 108.9 . . ?
C58 C59 C60 108.1(8) . . ?
C58 C59 H59A 110.1 . . ?
C60 C59 H59A 110.1 . . ?
C58 C59 H59B 110.1 . . ?
C60 C59 H59B 110.1 . . ?
H59A C59 H59B 108.4 . . ?
C59 C60 O2 107.2(7) . . ?
C59 C60 H60A 110.3 . . ?
O2 C60 H60A 110.3 . . ?
C59 C60 H60B 110.3 . . ?
O2 C60 H60B 110.3 . . ?
H60A C60 H60B 108.5 . . ?
C7 N1 N2 106.9(6) . . ?
N1 N2 C3 110.0(6) . . ?
N1 N2 B1 124.9(9) . . ?
C3 N2 B1 124.0(9) . . ?
C21 N3 N4 109.0(7) . . ?
C23 N4 N3 109.8(6) . . ?
C23 N4 B2 126.7(10) . . ?
N3 N4 B2 122.6(9) . . ?
O1 Ca1 O1 88.94(17) 3_775 . ?
O1 Ca1 O1 88.94(17) 3_775 2_755 ?
O1 Ca1 O1 88.94(17) . 2_755 ?
O1 Ca1 O2 88.99(16) 3_775 2_755 ?
O1 Ca1 O2 177.93(18) . 2_755 ?
O1 Ca1 O2 91.04(16) 2_755 2_755 ?
O1 Ca1 O2 91.04(16) 3_775 3_775 ?
O1 Ca1 O2 88.99(16) . 3_775 ?
O1 Ca1 O2 177.93(18) 2_755 3_775 ?
O2 Ca1 O2 91.03(17) 2_755 3_775 ?
O1 Ca1 O2 177.93(19) 3_775 . ?
O1 Ca1 O2 91.04(16) . . ?
O1 Ca1 O2 88.99(16) 2_755 . ?
O2 Ca1 O2 91.03(17) 2_755 . ?
O2 Ca1 O2 91.03(17) 3_775 . ?
N2 B1 N2 109.2(6) . 2_645 ?
N2 B1 N2 109.2(6) . 3_765 ?
N2 B1 N2 109.2(6) 2_645 3_765 ?
N4 B2 N4 107.8(7) . 2_655 ?
N4 B2 N4 107.8(7) . 3_665 ?
N4 B2 N4 107.8(7) 2_655 3_665 ?
F27 C27 C26 115.6(16) . . ?
F27 C27 C22 124.4(14) . . ?
C26 C27 C22 120.0(9) . . ?
C101 C100 C101 109(2) 18_545 . ?
C101 C100 H10A 109.8 18_545 . ?
C101 C100 H10A 109.8 . . ?
C101 C100 H10B 109.8 18_545 . ?
C101 C100 H10B 109.8 . . ?
H10A C100 H10B 108.2 . . ?
C103 C101 C100 109(2) . . ?
C103 C101 H10C 109.8 . . ?
C100 C101 H10C 109.8 . . ?
C103 C101 H10D 109.8 . . ?
C100 C101 H10D 109.8 . . ?
H10C C101 H10D 108.3 . . ?
C103 C104 C103 119(3) 18_545 . ?
C103 C104 H10E 107.4 18_545 . ?
C103 C104 H10E 107.4 . . ?
C103 C104 H10F 107.4 18_545 . ?
C103 C104 H10F 107.4 . . ?
H10E C104 H10F 107 . . ?
C101 C103 C104 111(3) . . ?
C101 C103 H10G 109.5 . . ?
C104 C103 H10G 109.5 . . ?
C101 C103 H10H 109.5 . . ?
C104 C103 H10H 109.5 . . ?
H10G C103 H10H 108.1 . . ?

#===END

_database_code_depnum_ccdc_archive 'CCDC 981308'
