#------------------------------------------------------------------------------
#$Date: 2016-03-25 22:51:44 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180017 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/11/7031117.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7031117
loop_
_publ_author_name
'Romero, Nuria'
'Vendier, Laure'
'Dinoi, Chiara'
'Etienne, Michel'
_publ_section_title
;
 Highly fluorinated hydrotris(indazolyl)borate calcium complexes: the
 structure and reactivity heavily depend on the ligand's electronic
 properties.
;
_journal_issue                   26
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10114
_journal_page_last               10119
_journal_paper_doi               10.1039/c4dt00884g
_journal_volume                  43
_journal_year                    2014
_chemical_compound_source        'synthesis as described'
_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_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 101.987(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.6950(5)
_cell_length_b                   18.0160(10)
_cell_length_c                   17.448(2)
_cell_measurement_reflns_used    5948
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      29.2898
_cell_measurement_theta_min      3.1612
_cell_measurement_wavelength     0.71073
_cell_volume                     3903.6(5)
_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_collection
;
        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_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      180(2)
_diffrn_detector_area_resol_mean 16.1978
_diffrn_measured_fraction_theta_full 0.876
_diffrn_measured_fraction_theta_max 0.876
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_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_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0401
_diffrn_reflns_av_unetI/netI     0.046
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            34745
_diffrn_reflns_theta_full        29.34
_diffrn_reflns_theta_max         29.34
_diffrn_reflns_theta_min         3.28
_exptl_absorpt_coefficient_mu    0.198
_exptl_absorpt_correction_T_max  0.990
_exptl_absorpt_correction_T_min  0.977
_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_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.532
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1824
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.241
_refine_diff_density_min         -0.263
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     622
_refine_ls_number_reflns         9405
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0834
_refine_ls_R_factor_gt           0.0454
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0380P)²+1.1258P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0895
_refine_ls_wR_factor_ref         0.1042
_reflns_number_gt                6252
_reflns_number_total             9405
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            c4dt00884g2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7031117--7031118.cif.'
_cod_database_code               7031117
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'
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
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_
_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
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 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
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 .
