# 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

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C56 H56 N16 Ni O42 V3 W12'
_chemical_formula_weight         4042.90

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
W W -0.8490 6.8722 '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'
C C 0.0033 0.0016 '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'
Ni Ni 0.3393 1.1124 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   I41/a

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y+3/4, x+1/4, z+1/4'
'-x+1/2, -y, z+1/2'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-y+5/4, x+3/4, z+3/4'
'-x+1, -y+1/2, z+1'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'y-3/4, -x-1/4, -z-1/4'
'x-1/2, y, -z-1/2'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'y-1/4, -x+1/4, -z+1/4'
'x, y+1/2, -z'
'-y-1/4, x-1/4, -z-1/4'

_cell_length_a                   22.927(5)
_cell_length_b                   22.927(5)
_cell_length_c                   15.430(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     8111(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3565
_cell_measurement_theta_min      3.18
_cell_measurement_theta_max      25.00

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.22
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.311
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             7300
_exptl_absorpt_coefficient_mu    17.593
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.0836
_exptl_absorpt_correction_T_max  0.1129
_exptl_absorpt_process_details   'ABSCOR by T.Higashi    8 March, 1995'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID IP'
_diffrn_measurement_method       Oscillation
_diffrn_detector_area_resol_mean 0.01
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        none
_diffrn_reflns_number            29180
_diffrn_reflns_av_R_equivalents  0.0749
_diffrn_reflns_av_sigmaI/netI    0.0695
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.18
_diffrn_reflns_theta_max         25.00
_reflns_number_total             3565
_reflns_number_gt                3152
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       auto
_computing_cell_refinement       auto
_computing_data_reduction        auto
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    auto
_computing_publication_material  auto

_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)+(0.1000P)²+790.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   none
_refine_ls_hydrogen_treatment    none
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3565
_refine_ls_number_parameters     287
_refine_ls_number_restraints     81
_refine_ls_R_factor_all          0.0684
_refine_ls_R_factor_gt           0.0604
_refine_ls_wR_factor_ref         0.1869
_refine_ls_wR_factor_gt          0.1820
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_restrained_S_all      1.096
_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
W1 W 0.10522(3) 0.21516(3) 0.28338(5) 0.0225(3) Uani 1 1 d . . .
W2 W 0.02428(3) 0.35798(3) 0.28388(5) 0.0237(3) Uani 1 1 d . . .
W3 W 0.07619(4) 0.11597(3) 0.13247(5) 0.0239(3) Uani 1 1 d . . .
V1 V 0.0000 0.2500 0.3856(4) 0.0510(16) Uani 1 2 d S . .
V2 V 0.0000 0.2500 0.1250 0.0380(18) Uani 1 4 d S . .
O1 O 0.0235(4) 0.0888(5) 0.2223(7) 0.012(2) Uani 1 1 d U . .
O2 O 0.1249(4) 0.1457(5) 0.2254(7) 0.012(2) Uani 1 1 d U . .
O3 O 0.0501(5) 0.4051(5) 0.3597(8) 0.017(2) Uani 1 1 d U . .
O4 O -0.0422(5) 0.3257(5) 0.3468(7) 0.013(2) Uani 1 1 d . . .
O5 O 0.1110(5) 0.1669(5) 0.0522(7) 0.014(2) Uani 1 1 d . . .
O6 O 0.0618(4) 0.2843(4) 0.3187(7) 0.009(2) Uani 1 1 d U . .
O7 O 0.1387(5) 0.2621(5) 0.1969(7) 0.013(2) Uani 1 1 d . . .
O8 O 0.1118(5) 0.0534(5) 0.1131(8) 0.018(3) Uani 1 1 d . . .
O9 O 0.0276(4) 0.2002(4) 0.1845(7) 0.011(2) Uani 1 1 d . . .
O10 O 0.1575(5) 0.2138(5) 0.3603(8) 0.017(3) Uani 1 1 d . . .
O11 O 0.0000 0.2500 0.4879(10) 0.008(3) Uani 1 2 d SU . .
Ni1 Ni 0.0000 0.2500 0.6250 0.0086(8) Uani 1 4 d SU . .
N2 N 0.1751(6) 0.1986(6) 0.5836(10) 0.018(3) Uani 1 1 d . . .
N3 N 0.0887(7) 0.2364(7) 0.6250(10) 0.022(3) Uani 1 1 d . . .
C1 C 0.2587(8) 0.0703(9) 0.6047(14) 0.028(4) Uani 1 1 d . . .
H1A H 0.2952 0.0880 0.6031 0.033 Uiso 1 1 calc R . .
C2 C 0.1822(8) 0.2166(8) 0.6688(14) 0.025(4) Uani 1 1 d . . .
H2A H 0.2152 0.2129 0.7036 0.029 Uiso 1 1 calc R . .
C3 C 0.1186(8) 0.2101(8) 0.5599(13) 0.021(4) Uani 1 1 d U . .
H3A H 0.1027 0.2011 0.5061 0.026 Uiso 1 1 calc R . .
C4 C 0.2162(7) 0.1606(8) 0.5343(12) 0.019(4) Uani 1 1 d . . .
H4A H 0.2558 0.1746 0.5408 0.023 Uiso 1 1 calc R . .
H4B H 0.2063 0.1609 0.4731 0.023 Uiso 1 1 calc R . .
C5 C 0.2525(8) 0.0154(8) 0.6409(12) 0.024(4) Uani 1 1 d . . .
H5A H 0.2849 -0.0038 0.6632 0.029 Uiso 1 1 calc R . .
C6 C 0.1983(8) -0.0113(8) 0.6442(12) 0.020(4) Uani 1 1 d . . .
C7 C 0.1569(9) 0.0710(9) 0.5685(13) 0.031(5) Uani 1 1 d . . .
H7A H 0.1256 0.0892 0.5411 0.037 Uiso 1 1 calc R . .
C8 C 0.1294(9) 0.2413(8) 0.6904(12) 0.025(4) Uani 1 1 d U . .
H8A H 0.1219 0.2593 0.7433 0.030 Uiso 1 1 calc R . .
C9 C 0.2107(8) 0.0986(8) 0.5709(12) 0.021(4) Uani 1 1 d . . .
C10 C 0.1492(8) 0.0166(8) 0.6064(14) 0.024(4) Uani 1 1 d . . .
H10A H 0.1127 -0.0011 0.6070 0.029 Uiso 1 1 calc R . .
C11 C 0.1896(9) -0.0672(9) 0.6898(13) 0.031(4) Uani 1 1 d . . .
H11A H 0.2113 -0.0659 0.7437 0.037 Uiso 1 1 calc R . .
H11B H 0.1487 -0.0707 0.7045 0.037 Uiso 1 1 calc R . .
C14 C 0.2625(8) -0.1918(7) 0.6129(13) 0.057(6) Uani 1 1 d GDU . .
H14A H 0.2912 -0.2204 0.6162 0.069 Uiso 1 1 calc R . .
C13 C 0.2513(7) -0.1504(7) 0.6735(11) 0.062(7) Uani 1 1 d GDU . .
H13A H 0.2711 -0.1456 0.7257 0.075 Uiso 1 1 calc R . .
N4 N 0.2063(5) -0.1173(5) 0.6447(9) 0.026(3) Uani 1 1 d GDU . .
C12 C 0.1896(8) -0.1382(7) 0.5663(9) 0.058(6) Uani 1 1 d GDU . .
H12A H 0.1596 -0.1235 0.5320 0.070 Uiso 1 1 calc R . .
N1 N 0.2243(10) -0.1843(7) 0.5466(10) 0.073(6) Uani 1 1 d GDU . .


_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
W1 O10 1.687(12) . ?
W1 O7 1.878(11) . ?
W1 O2 1.883(11) . ?
W1 O6 1.950(10) . ?
W1 O4 1.980(10) 7_454 ?
W1 O9 2.369(11) . ?
W1 V1 2.991(4) . ?
W2 O3 1.699(12) . ?
W2 O1 1.896(11) 7_454 ?
W2 O5 1.894(11) 12_666 ?
W2 O4 1.954(10) . ?
W2 O6 1.970(10) . ?
W2 O9 2.354(10) 7_454 ?
W2 V1 2.984(4) . ?
W3 O8 1.678(11) . ?
W3 O5 1.880(11) . ?
W3 O7 1.915(11) 14 ?
W3 O2 1.941(11) . ?
W3 O1 1.942(10) . ?
W3 O9 2.369(10) . ?
V1 O11 1.578(16) . ?
V1 O6 1.920(10) 7_454 ?
V1 O6 1.920(10) . ?
V1 O4 2.075(12) . ?
V1 O4 2.075(12) 7_454 ?
V1 W2 2.984(4) 7_454 ?
V1 W1 2.991(4) 7_454 ?
V2 O9 1.597(11) 7_454 ?
V2 O9 1.597(11) 12_666 ?
V2 O9 1.597(11) . ?
V2 O9 1.597(11) 14 ?
O1 W2 1.896(11) 7_454 ?
O4 W1 1.980(10) 7_454 ?
O5 W2 1.894(11) 14 ?
O7 W3 1.915(11) 12_666 ?
O9 W2 2.354(10) 7_454 ?
O11 Ni1 2.116(15) . ?
Ni1 N3 2.057(16) 12_667 ?
Ni1 N3 2.057(16) . ?
Ni1 N3 2.057(16) 7_454 ?
Ni1 N3 2.057(16) 14_556 ?
Ni1 O11 2.116(15) 14_556 ?
N2 C2 1.39(3) . ?
N2 C3 1.37(2) . ?
N2 C4 1.49(2) . ?
N3 C3 1.36(2) . ?
N3 C8 1.38(2) . ?
C1 C9 1.38(3) . ?
C1 C5 1.38(3) . ?
C1 H1A 0.9300 . ?
C2 C8 1.38(3) . ?
C2 H2A 0.9300 . ?
C3 H3A 0.9300 . ?
C4 C9 1.53(2) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.39(3) . ?
C5 H5A 0.9300 . ?
C6 C10 1.42(2) . ?
C6 C11 1.48(3) . ?
C7 C9 1.39(3) . ?
C7 C10 1.39(3) . ?
C7 H7A 0.9300 . ?
C8 H8A 0.9300 . ?
C10 H10A 0.9300 . ?
C11 N4 1.40(2) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C14 N1 1.357(8) . ?
C14 C13 1.357(8) . ?
C14 H14A 0.9300 . ?
C13 N4 1.357(8) . ?
C13 H13A 0.9300 . ?
N4 C12 1.357(8) . ?
C12 N1 1.357(8) . ?
C12 H12A 0.9300 . ?

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
O10 W1 O7 102.7(5) . . ?
O10 W1 O2 98.6(5) . . ?
O7 W1 O2 92.9(5) . . ?
O10 W1 O6 100.4(5) . . ?
O7 W1 O6 86.6(5) . . ?
O2 W1 O6 160.7(4) . . ?
O10 W1 O4 99.3(5) . 7_454 ?
O7 W1 O4 156.9(5) . 7_454 ?
O2 W1 O4 90.6(5) . 7_454 ?
O6 W1 O4 82.7(4) . 7_454 ?
O10 W1 O9 169.7(4) . . ?
O7 W1 O9 86.1(4) . . ?
O2 W1 O9 75.6(4) . . ?
O6 W1 O9 85.1(4) . . ?
O4 W1 O9 72.7(4) 7_454 . ?
O10 W1 V1 101.9(4) . . ?
O7 W1 V1 123.4(3) . . ?
O2 W1 V1 132.1(3) . . ?
O6 W1 V1 39.0(3) . . ?
O4 W1 V1 43.7(3) 7_454 . ?
O9 W1 V1 76.8(3) . . ?
O3 W2 O1 97.9(5) . 7_454 ?
O3 W2 O5 102.2(5) . 12_666 ?
O1 W2 O5 92.1(5) 7_454 12_666 ?
O3 W2 O4 99.8(5) . . ?
O1 W2 O4 92.4(5) 7_454 . ?
O5 W2 O4 156.6(5) 12_666 . ?
O3 W2 O6 101.8(5) . . ?
O1 W2 O6 160.2(4) 7_454 . ?
O5 W2 O6 84.9(4) 12_666 . ?
O4 W2 O6 83.1(4) . . ?
O3 W2 O9 169.9(5) . 7_454 ?
O1 W2 O9 75.3(4) 7_454 7_454 ?
O5 W2 O9 85.6(4) 12_666 7_454 ?
O4 W2 O9 73.4(4) . 7_454 ?
O6 W2 O9 85.0(4) . 7_454 ?
O3 W2 V1 103.3(4) . . ?
O1 W2 V1 133.6(3) 7_454 . ?
O5 W2 V1 122.1(3) 12_666 . ?
O4 W2 V1 43.8(3) . . ?
O6 W2 V1 39.3(3) . . ?
O9 W2 V1 77.2(3) 7_454 . ?
O8 W3 O5 102.0(5) . . ?
O8 W3 O7 102.2(5) . 14 ?
O5 W3 O7 86.5(5) . 14 ?
O8 W3 O2 98.7(5) . . ?
O5 W3 O2 91.4(5) . . ?
O7 W3 O2 159.0(4) 14 . ?
O8 W3 O1 98.9(5) . . ?
O5 W3 O1 159.1(5) . . ?
O7 W3 O1 87.8(5) 14 . ?
O2 W3 O1 86.8(5) . . ?
O8 W3 O9 170.4(5) . . ?
O5 W3 O9 85.2(4) . . ?
O7 W3 O9 84.4(4) 14 . ?
O2 W3 O9 74.6(4) . . ?
O1 W3 O9 74.2(4) . . ?
O11 V1 O6 122.5(4) . 7_454 ?
O11 V1 O6 122.5(4) . . ?
O6 V1 O6 115.0(7) 7_454 . ?
O11 V1 O4 106.7(4) . . ?
O6 V1 O4 81.0(4) 7_454 . ?
O6 V1 O4 81.2(4) . . ?
O11 V1 O4 106.7(4) . 7_454 ?
O6 V1 O4 81.2(4) 7_454 7_454 ?
O6 V1 O4 81.0(4) . 7_454 ?
O4 V1 O4 146.5(7) . 7_454 ?
O11 V1 W2 121.73(11) . . ?
O6 V1 W2 101.2(4) 7_454 . ?
O6 V1 W2 40.6(3) . . ?
O4 V1 W2 40.7(3) . . ?
O4 V1 W2 117.1(4) 7_454 . ?
O11 V1 W2 121.73(11) . 7_454 ?
O6 V1 W2 40.6(3) 7_454 7_454 ?
O6 V1 W2 101.2(4) . 7_454 ?
O4 V1 W2 117.1(4) . 7_454 ?
O4 V1 W2 40.7(3) 7_454 7_454 ?
W2 V1 W2 116.5(2) . 7_454 ?
O11 V1 W1 121.82(11) . . ?
O6 V1 W1 101.7(4) 7_454 . ?
O6 V1 W1 39.8(3) . . ?
O4 V1 W1 116.6(4) . . ?
O4 V1 W1 41.3(3) 7_454 . ?
W2 V1 W1 78.10(11) . . ?
W2 V1 W1 69.61(9) 7_454 . ?
O11 V1 W1 121.82(11) . 7_454 ?
O6 V1 W1 39.8(3) 7_454 7_454 ?
O6 V1 W1 101.7(4) . 7_454 ?
O4 V1 W1 41.3(3) . 7_454 ?
O4 V1 W1 116.6(4) 7_454 7_454 ?
W2 V1 W1 69.61(9) . 7_454 ?
W2 V1 W1 78.10(11) 7_454 7_454 ?
W1 V1 W1 116.4(2) . 7_454 ?
O9 V2 O9 109.3(4) 7_454 12_666 ?
O9 V2 O9 109.8(7) 7_454 . ?
O9 V2 O9 109.3(4) 12_666 . ?
O9 V2 O9 109.3(4) 7_454 14 ?
O9 V2 O9 109.8(7) 12_666 14 ?
O9 V2 O9 109.3(4) . 14 ?
W2 O1 W3 120.7(5) 7_454 . ?
W1 O2 W3 120.7(5) . . ?
W2 O4 W1 120.2(6) . 7_454 ?
W2 O4 V1 95.5(5) . . ?
W1 O4 V1 95.0(5) 7_454 . ?
W3 O5 W2 152.8(7) . 14 ?
V1 O6 W1 101.2(4) . . ?
V1 O6 W2 100.1(4) . . ?
W1 O6 W2 147.5(6) . . ?
W1 O7 W3 150.6(6) . 12_666 ?
V2 O9 W2 125.4(5) . 7_454 ?
V2 O9 W1 124.4(5) . . ?
W2 O9 W1 92.4(4) 7_454 . ?
V2 O9 W3 125.1(6) . . ?
W2 O9 W3 89.8(3) 7_454 . ?
W1 O9 W3 89.1(4) . . ?
V1 O11 Ni1 180.000(1) . . ?
N3 Ni1 N3 90.000(4) 12_667 . ?
N3 Ni1 N3 90.000(2) 12_667 7_454 ?
N3 Ni1 N3 180.0(8) . 7_454 ?
N3 Ni1 N3 180.0(8) 12_667 14_556 ?
N3 Ni1 N3 90.000(1) . 14_556 ?
N3 Ni1 N3 90.000(4) 7_454 14_556 ?
N3 Ni1 O11 90.0(4) 12_667 14_556 ?
N3 Ni1 O11 90.0(4) . 14_556 ?
N3 Ni1 O11 90.0(4) 7_454 14_556 ?
N3 Ni1 O11 90.0(4) 14_556 14_556 ?
N3 Ni1 O11 90.0(4) 12_667 . ?
N3 Ni1 O11 90.0(4) . . ?
N3 Ni1 O11 90.0(4) 7_454 . ?
N3 Ni1 O11 90.0(4) 14_556 . ?
O11 Ni1 O11 180.000(1) 14_556 . ?
C2 N2 C3 107.7(15) . . ?
C2 N2 C4 125.7(15) . . ?
C3 N2 C4 125.0(15) . . ?
C3 N3 C8 103.7(16) . . ?
C3 N3 Ni1 124.5(12) . . ?
C8 N3 Ni1 131.0(13) . . ?
C9 C1 C5 119.8(17) . . ?
C9 C1 H1A 120.1 . . ?
C5 C1 H1A 120.1 . . ?
C8 C2 N2 104.4(16) . . ?
C8 C2 H2A 127.8 . . ?
N2 C2 H2A 127.8 . . ?
N3 C3 N2 111.5(16) . . ?
N3 C3 H3A 124.3 . . ?
N2 C3 H3A 124.3 . . ?
N2 C4 C9 107.6(13) . . ?
N2 C4 H4A 110.2 . . ?
C9 C4 H4A 110.2 . . ?
N2 C4 H4B 110.2 . . ?
C9 C4 H4B 110.2 . . ?
H4A C4 H4B 108.5 . . ?
C6 C5 C1 120.6(16) . . ?
C6 C5 H5A 119.7 . . ?
C1 C5 H5A 119.7 . . ?
C5 C6 C10 119.8(17) . . ?
C5 C6 C11 121.4(17) . . ?
C10 C6 C11 118.7(16) . . ?
C9 C7 C10 120.8(17) . . ?
C9 C7 H7A 119.6 . . ?
C10 C7 H7A 119.6 . . ?
C2 C8 N3 112.6(17) . . ?
C2 C8 H8A 123.7 . . ?
N3 C8 H8A 123.7 . . ?
C7 C9 C1 120.3(17) . . ?
C7 C9 C4 119.0(16) . . ?
C1 C9 C4 120.7(16) . . ?
C7 C10 C6 118.5(17) . . ?
C7 C10 H10A 120.8 . . ?
C6 C10 H10A 120.8 . . ?
N4 C11 C6 116.2(16) . . ?
N4 C11 H11A 108.2 . . ?
C6 C11 H11A 108.2 . . ?
N4 C11 H11B 108.2 . . ?
C6 C11 H11B 108.2 . . ?
H11A C11 H11B 107.4 . . ?
N1 C14 C13 108.0 . . ?
N1 C14 H14A 126.0 . . ?
C13 C14 H14A 126.0 . . ?
N4 C13 C14 108.0 . . ?
N4 C13 H13A 126.0 . . ?
C14 C13 H13A 126.0 . . ?
C13 N4 C12 108.0 . . ?
C13 N4 C11 120.4(13) . . ?
C12 N4 C11 131.1(13) . . ?
N4 C12 N1 108.0 . . ?
N4 C12 H12A 126.0 . . ?
N1 C12 H12A 126.0 . . ?
C14 N1 C12 108.0 . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         2.487
_refine_diff_density_min         -4.100
_refine_diff_density_rms         0.373
_database_code_depnum_ccdc_archive 'CCDC 1005395'
