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


data_DE-VF
# start Validation Reply Form
_vrf_RINTA01_DE-VF               
;
PROBLEM: The value of Rint is greater than 0.25
RESPONSE: The value of Rint for this compound is high due to overall 
poor crystal quality which ultimately resulted in broad reflections 
and weak diffraction at high angles even when synchrotron radiation 
is used. The crystallographic result described in this short 
communication corresponds to the best solution.

;
_vrf_PLAT020_DE-VF               
;
PROBLEM: The value of Rint is greater than 0.12 .........      0.280      
RESPONSE: As explained above
;
_vrf_PLAT213_DE-VF               
;
PROBLEM: Atom V1              has ADP max/min Ratio .....        6.7 oblat
RESPONSE: Unresolved disorder
;
# end Validation Reply Form


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'F12 V3, C2 H8 N, 2(H4 N)'
_chemical_formula_sum            'C2 H16 F12 N3 V3'
_chemical_formula_weight         463.00

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'
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'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/m'
_symmetry_space_group_name_Hall  '-P 2yb'

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

_cell_length_a                   6.932(5)
_cell_length_b                   12.876(8)
_cell_length_c                   7.444(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.550(7)
_cell_angle_gamma                90.00
_cell_volume                     662.3(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4001
_cell_measurement_theta_min      6.901
_cell_measurement_theta_max      69.300

_exptl_crystal_description       Plate
_exptl_crystal_colour            Brown
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.322
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             452
_exptl_absorpt_coefficient_mu    2.797
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5366
_exptl_absorpt_correction_T_max  0.7468
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.77490
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         '11.3.1 ALS. LBNL.CA'
_diffrn_radiation_monochromator  'Si (111) Crystal'
_diffrn_measurement_device_type  'Bruker AXS APEXII'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean none
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            9941
_diffrn_reflns_av_R_equivalents  0.2800
_diffrn_reflns_av_sigmaI/netI    0.1389
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         3.45
_diffrn_reflns_theta_max         34.81
_reflns_number_total             2218
_reflns_number_gt                1871
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEXII (Bruker, 2006)'
_computing_cell_refinement       'SAINT (Bruker, 2006)'
_computing_data_reduction        'SAINT (Bruker, 2006)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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 > 2sigma(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)+(0.1206P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    none
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2218
_refine_ls_number_parameters     115
_refine_ls_number_restraints     22
_refine_ls_R_factor_all          0.0807
_refine_ls_R_factor_gt           0.0756
_refine_ls_wR_factor_ref         0.1961
_refine_ls_wR_factor_gt          0.1911
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_restrained_S_all      1.022
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.0000 0.0000 0.5000 0.0071(2) Uani 1 2 d SU . .
V2 V -0.03196(10) 0.2500 0.24381(8) 0.0069(2) Uani 1 2 d SU . .
V3 V 0.0000 0.0000 0.0000 0.0072(2) Uani 1 2 d S . .
F1 F 0.0621(3) -0.03567(15) 0.2578(2) 0.0126(4) Uani 1 1 d . . .
F2 F 0.2523(3) 0.05332(14) 0.5541(2) 0.0121(4) Uani 1 1 d . . .
F3 F -0.0844(3) 0.14019(14) 0.4179(2) 0.0113(4) Uani 1 1 d . . .
F4 F -0.2982(4) 0.2500 0.1673(4) 0.0137(5) Uani 1 2 d S . .
C1 C 0.4058(9) 0.2500 0.8357(7) 0.0338(14) Uani 1 2 d S . .
H1A H 0.4137 0.1892 0.9128 0.041 Uiso 0.50 1 calc PR . .
H1B H 0.4137 0.3108 0.9128 0.041 Uiso 0.50 1 calc PR . .
F5 F 0.0187(3) 0.14750(15) 0.0579(2) 0.0137(4) Uani 1 1 d . . .
N1 N 0.2157(6) 0.2500 0.7294(5) 0.0199(8) Uani 1 2 d S . .
H11A H 0.1214 0.2500 0.8038 0.030 Uiso 1 2 calc SR . .
H11B H 0.2058 0.1936 0.6602 0.030 Uiso 0.50 1 calc PR . .
H11C H 0.2058 0.3064 0.6602 0.030 Uiso 0.50 1 calc PR . .
F6 F 0.2277(4) 0.2500 0.3308(4) 0.0132(5) Uani 1 2 d S . .
F7 F 0.2648(3) 0.00069(15) -0.0321(3) 0.0162(5) Uani 1 1 d . . .
N2 N 0.4837(4) 0.0812(2) 0.2589(3) 0.0139(5) Uani 1 1 d D . .
C2 C 0.5748(9) 0.2500 0.7233(9) 0.0386(15) Uani 1 2 d S . .
H2A H 0.6926 0.2500 0.8003 0.058 Uiso 1 2 calc SR . .
H2B H 0.5702 0.3109 0.6486 0.058 Uiso 0.50 1 calc PR . .
H2C H 0.5702 0.1891 0.6486 0.058 Uiso 0.50 1 calc PR . .
H1 H 0.559(6) 0.034(3) 0.309(6) 0.046 Uiso 1 1 d D . .
H3 H 0.425(6) 0.055(3) 0.164(4) 0.046 Uiso 1 1 d D . .
H2 H 0.554(6) 0.133(2) 0.231(6) 0.046 Uiso 1 1 d D . .
H4 H 0.403(5) 0.100(3) 0.334(5) 0.046 Uiso 1 1 d D . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
V1 0.0107(4) 0.0091(4) 0.0011(3) 0.00088(18) -0.0028(3) -0.00034(19)
V2 0.0103(3) 0.0080(3) 0.0019(3) 0.000 -0.0031(2) 0.000
V3 0.0105(4) 0.0090(4) 0.0016(3) -0.00103(18) -0.0019(3) 0.0001(2)
F1 0.0206(9) 0.0148(9) 0.0020(7) 0.0004(6) -0.0020(6) 0.0034(7)
F2 0.0121(8) 0.0165(9) 0.0070(7) 0.0016(6) -0.0045(6) -0.0020(7)
F3 0.0166(9) 0.0108(8) 0.0061(7) 0.0030(6) -0.0010(6) 0.0013(6)
F4 0.0124(12) 0.0137(12) 0.0140(12) 0.000 -0.0066(9) 0.000
C1 0.029(3) 0.057(4) 0.013(2) 0.000 -0.011(2) 0.000
F5 0.0251(10) 0.0109(8) 0.0048(7) -0.0015(6) -0.0002(6) -0.0008(7)
N1 0.024(2) 0.0221(19) 0.0127(17) 0.000 -0.0015(15) 0.000
F6 0.0107(11) 0.0141(12) 0.0139(12) 0.000 -0.0044(9) 0.000
F7 0.0108(9) 0.0276(12) 0.0098(9) -0.0044(6) -0.0020(7) -0.0017(6)
N2 0.0147(12) 0.0172(14) 0.0094(11) -0.0015(8) -0.0010(9) -0.0003(9)
C2 0.026(3) 0.056(4) 0.032(3) 0.000 -0.010(2) 0.000

_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
V1 F2 1.892(2) . ?
V1 F2 1.892(2) 3_556 ?
V1 F1 1.941(2) 3_556 ?
V1 F1 1.941(2) . ?
V1 F3 1.979(2) . ?
V1 F3 1.979(2) 3_556 ?
V2 F6 1.864(3) . ?
V2 F4 1.888(3) . ?
V2 F5 1.964(2) 4_565 ?
V2 F5 1.964(2) . ?
V2 F3 1.9713(19) 4_565 ?
V2 F3 1.9714(19) . ?
V3 F7 1.870(2) 3 ?
V3 F7 1.870(2) . ?
V3 F5 1.950(2) 3 ?
V3 F5 1.950(2) . ?
V3 F1 1.987(2) . ?
V3 F1 1.987(2) 3 ?
C1 N1 1.482(7) . ?
C1 C2 1.492(9) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
N1 H11A 0.8900 . ?
N1 H11B 0.8900 . ?
N1 H11C 0.8900 . ?
N2 H1 0.863(17) . ?
N2 H3 0.859(16) . ?
N2 H2 0.857(17) . ?
N2 H4 0.857(16) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?

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
F2 V1 F2 180.0 . 3_556 ?
F2 V1 F1 89.20(8) . 3_556 ?
F2 V1 F1 90.80(8) 3_556 3_556 ?
F2 V1 F1 90.81(8) . . ?
F2 V1 F1 89.19(8) 3_556 . ?
F1 V1 F1 180.0 3_556 . ?
F2 V1 F3 88.88(8) . . ?
F2 V1 F3 91.12(8) 3_556 . ?
F1 V1 F3 89.36(8) 3_556 . ?
F1 V1 F3 90.64(8) . . ?
F2 V1 F3 91.12(8) . 3_556 ?
F2 V1 F3 88.88(8) 3_556 3_556 ?
F1 V1 F3 90.64(8) 3_556 3_556 ?
F1 V1 F3 89.36(8) . 3_556 ?
F3 V1 F3 180.0 . 3_556 ?
F6 V2 F4 177.23(11) . . ?
F6 V2 F5 91.33(9) . 4_565 ?
F4 V2 F5 90.72(9) . 4_565 ?
F6 V2 F5 91.33(9) . . ?
F4 V2 F5 90.72(9) . . ?
F5 V2 F5 84.45(12) 4_565 . ?
F6 V2 F3 89.72(8) . 4_565 ?
F4 V2 F3 88.35(8) . 4_565 ?
F5 V2 F3 91.94(9) 4_565 4_565 ?
F5 V2 F3 176.27(7) . 4_565 ?
F6 V2 F3 89.72(8) . . ?
F4 V2 F3 88.35(8) . . ?
F5 V2 F3 176.27(7) 4_565 . ?
F5 V2 F3 91.94(9) . . ?
F3 V2 F3 91.65(12) 4_565 . ?
F7 V3 F7 180.0 3 . ?
F7 V3 F5 88.57(8) 3 3 ?
F7 V3 F5 91.43(8) . 3 ?
F7 V3 F5 91.43(8) 3 . ?
F7 V3 F5 88.57(8) . . ?
F5 V3 F5 180.0 3 . ?
F7 V3 F1 90.87(8) 3 . ?
F7 V3 F1 89.13(9) . . ?
F5 V3 F1 89.66(8) 3 . ?
F5 V3 F1 90.34(8) . . ?
F7 V3 F1 89.13(8) 3 3 ?
F7 V3 F1 90.87(9) . 3 ?
F5 V3 F1 90.34(8) 3 3 ?
F5 V3 F1 89.66(8) . 3 ?
F1 V3 F1 180.0 . 3 ?
V1 F1 V3 142.67(11) . . ?
V2 F3 V1 142.33(10) . . ?
N1 C1 C2 113.9(4) . . ?
N1 C1 H1A 108.8 . . ?
C2 C1 H1A 108.8 . . ?
N1 C1 H1B 108.8 . . ?
C2 C1 H1B 108.8 . . ?
H1A C1 H1B 107.7 . . ?
V3 F5 V2 142.95(10) . . ?
C1 N1 H11A 109.5 . . ?
C1 N1 H11B 109.5 . . ?
H11A N1 H11B 109.5 . . ?
C1 N1 H11C 109.5 . . ?
H11A N1 H11C 109.5 . . ?
H11B N1 H11C 109.5 . . ?
H1 N2 H3 109(3) . . ?
H1 N2 H2 108(2) . . ?
H3 N2 H2 110(2) . . ?
H1 N2 H4 108(2) . . ?
H3 N2 H4 111(3) . . ?
H2 N2 H4 110(3) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.961
_diffrn_reflns_theta_full        34.81
_diffrn_measured_fraction_theta_full 0.961
_refine_diff_density_max         1.909
_refine_diff_density_min         -2.027
_refine_diff_density_rms         0.524
_database_code_depnum_ccdc_archive 'CCDC 973935'

data_TTB-VF

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'F4 V, H4 N'
_chemical_formula_sum            'F4 H4 N V'
_chemical_formula_weight         144.98

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0.0000 0.0000 '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'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.0687 2.1097 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           TETRAGONAL
_symmetry_space_group_name_H-M   'P 42/n c m'
_symmetry_space_group_name_Hall  '-P 4ac 2ac'

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

_cell_length_a                   12.270(4)
_cell_length_b                   12.270(4)
_cell_length_c                   12.723(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1915.5(14)
_cell_formula_units_Z            20
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    1819
_cell_measurement_theta_min      41.0
_cell_measurement_theta_max      69.5

_exptl_crystal_description       Prism
_exptl_crystal_colour            Brown
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.514
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1400
_exptl_absorpt_coefficient_mu    21.580
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.831
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  Confocal
_diffrn_measurement_method       'profile data from φ-scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18807
_diffrn_reflns_av_R_equivalents  0.0422
_diffrn_reflns_av_sigmaI/netI    0.0148
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         5.10
_diffrn_reflns_theta_max         68.08
_reflns_number_total             937
_reflns_number_gt                931
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear-SM Expert 2.1 b6 (Rigaku, 2011)'
_computing_cell_refinement       'CrystalClear-SM Expert 2.1 b6 (Rigaku, 2011)'
_computing_data_reduction        'CrystalClear-SM Expert 2.1 b6 (Rigaku, 2011)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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 > 2sigma(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)+(0.0276P)²+0.7753P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         937
_refine_ls_number_parameters     103
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0195
_refine_ls_R_factor_gt           0.0194
_refine_ls_wR_factor_ref         0.0509
_refine_ls_wR_factor_gt          0.0508
_refine_ls_goodness_of_fit_ref   1.195
_refine_ls_restrained_S_all      1.195
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.2500 0.2500 0.25612(3) 0.00892(15) Uani 1 4 d S . .
V2 V 0.17251(2) -0.04415(2) 0.242797(19) 0.00989(12) Uani 1 1 d . . .
F4 F 0.13271(8) -0.04683(7) 0.38329(7) 0.0230(2) Uani 1 1 d . . .
F2 F 0.2500 0.2500 0.11033(15) 0.0399(6) Uani 1 4 d S . .
F1 F 0.2500 0.2500 0.40362(14) 0.0305(5) Uani 1 4 d S . .
F6 F 0.11074(7) -0.18633(7) 0.21941(7) 0.0190(2) Uani 1 1 d . . .
F7 F 0.03164(7) 0.03164(7) 0.20594(10) 0.0164(3) Uani 1 2 d S . .
F5 F 0.20720(8) -0.04165(6) 0.09664(7) 0.0200(2) Uani 1 1 d . . .
F3 F 0.25105(9) 0.09248(8) 0.25848(7) 0.0254(2) Uani 1 1 d . . .
N1 N 0.7500 0.2500 0.5000 0.0206(6) Uani 1 4 d S . .
N2 N 0.09118(12) 0.09118(12) 0.55351(17) 0.0190(4) Uani 1 2 d S . .
N3 N 0.09630(13) 0.09630(13) -0.03821(17) 0.0217(4) Uani 1 2 d S . .
H34 H 0.1433(18) 0.1433(18) -0.054(2) 0.024(7) Uiso 1 2 d S . .
H31 H 0.1277(19) 0.0461(16) -0.004(2) 0.040(6) Uiso 1 1 d . . .
H11 H 0.7486(16) 0.1893(18) 0.4609(19) 0.042(6) Uiso 1 1 d . . .
H21 H 0.138(2) 0.138(2) 0.569(3) 0.036(8) Uiso 1 2 d S . .
H32 H 0.0676(18) 0.0676(18) -0.092(3) 0.032(8) Uiso 1 2 d S . .
H23 H 0.082(3) 0.082(3) 0.492(4) 0.075(14) Uiso 1 2 d S . .
H22 H 0.032(2) 0.109(2) 0.569(3) 0.081(12) Uiso 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
V1 0.00838(19) 0.00838(19) 0.0100(2) 0.000 0.000 -0.00082(19)
V2 0.00805(17) 0.00746(17) 0.01416(18) -0.00069(8) 0.00062(8) -0.00002(8)
F4 0.0218(5) 0.0299(5) 0.0173(5) -0.0029(3) 0.0018(4) 0.0058(4)
F2 0.0540(9) 0.0540(9) 0.0117(9) 0.000 0.000 0.0353(12)
F1 0.0399(7) 0.0399(7) 0.0118(8) 0.000 0.000 0.0212(9)
F6 0.0181(5) 0.0113(4) 0.0277(5) 0.0000(3) 0.0004(4) -0.0036(3)
F7 0.0123(4) 0.0123(4) 0.0246(7) -0.0016(3) -0.0016(3) 0.0028(4)
F5 0.0227(5) 0.0193(5) 0.0178(4) 0.0023(3) 0.0044(4) 0.0027(3)
F3 0.0163(5) 0.0098(5) 0.0502(6) -0.0027(4) -0.0042(4) -0.0010(4)
N1 0.0205(9) 0.0205(9) 0.0209(14) 0.000 0.000 -0.0036(10)
N2 0.0184(6) 0.0184(6) 0.0201(10) -0.0037(6) -0.0037(6) 0.0001(8)
N3 0.0231(7) 0.0231(7) 0.0191(10) 0.0028(6) 0.0028(6) -0.0021(9)

_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
V1 F2 1.855(2) . ?
V1 F1 1.8767(19) . ?
V1 F3 1.9330(11) 3 ?
V1 F3 1.9330(11) . ?
V1 F3 1.9330(11) 8 ?
V1 F3 1.9331(11) 6 ?
V2 F4 1.8533(11) . ?
V2 F5 1.9079(11) . ?
V2 F6 1.9252(11) . ?
V2 F3 1.9440(12) . ?
V2 F6 1.9745(11) 10_656 ?
V2 F7 2.0180(8) . ?
F6 V2 1.9746(11) 12_556 ?
F7 V2 2.0179(8) 6 ?
N1 H11 0.90(2) . ?
N2 H21 0.84(3) . ?
N2 H23 0.80(5) . ?
N2 H22 0.78(3) . ?
N3 H34 0.84(3) . ?
N3 H31 0.85(2) . ?
N3 H32 0.84(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
F2 V1 F1 180.0 . . ?
F2 V1 F3 90.89(3) . 3 ?
F1 V1 F3 89.11(3) . 3 ?
F2 V1 F3 90.89(3) . . ?
F1 V1 F3 89.11(3) . . ?
F3 V1 F3 178.22(6) 3 . ?
F2 V1 F3 90.89(3) . 8 ?
F1 V1 F3 89.11(3) . 8 ?
F3 V1 F3 90.75(6) 3 8 ?
F3 V1 F3 89.23(6) . 8 ?
F2 V1 F3 90.89(3) . 6 ?
F1 V1 F3 89.11(3) . 6 ?
F3 V1 F3 89.23(6) 3 6 ?
F3 V1 F3 90.75(6) . 6 ?
F3 V1 F3 178.22(6) 8 6 ?
F4 V2 F5 177.61(4) . . ?
F4 V2 F6 91.68(4) . . ?
F5 V2 F6 87.23(4) . . ?
F4 V2 F3 92.69(4) . . ?
F5 V2 F3 88.60(4) . . ?
F6 V2 F3 172.97(4) . . ?
F4 V2 F6 89.37(4) . 10_656 ?
F5 V2 F6 92.77(4) . 10_656 ?
F6 V2 F6 90.46(5) . 10_656 ?
F3 V2 F6 84.09(4) . 10_656 ?
F4 V2 F7 90.38(5) . . ?
F5 V2 F7 87.55(5) . . ?
F6 V2 F7 92.55(4) . . ?
F3 V2 F7 92.92(4) . . ?
F6 V2 F7 176.98(4) 10_656 . ?
V2 F6 V2 156.94(6) . 12_556 ?
V2 F7 V2 137.35(6) 6 . ?
V1 F3 V2 149.03(6) . . ?
H21 N2 H23 115(4) . . ?
H21 N2 H22 113(2) . . ?
H23 N2 H22 99(3) . . ?
H34 N3 H31 108.2(17) . . ?
H34 N3 H32 112(3) . . ?
H31 N3 H32 107.5(19) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        68.08
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.346
_refine_diff_density_min         -0.519
_refine_diff_density_rms         0.066
_database_code_depnum_ccdc_archive 'CCDC 973936'
