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

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#
#                 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.
#
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#  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
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#  data retrieval see:
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data_afh345

_audit_creation_method           SHELXTL
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H56 Cl2 N O4 V'
_chemical_formula_weight         688.66

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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   P2(1)/n

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                   16.6922(12)
_cell_length_b                   10.7697(8)
_cell_length_c                   20.4145(15)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.0439(10)
_cell_angle_gamma                90.00
_cell_volume                     3664.7(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    88(2)
_cell_measurement_reflns_used    9289
_cell_measurement_theta_min      2.25
_cell_measurement_theta_max      28.07

_exptl_crystal_description       polyhedron
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.23
_exptl_crystal_density_meas      not_measured
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1472
_exptl_absorpt_coefficient_mu    0.453
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8476
_exptl_absorpt_correction_T_max  0.9033
_exptl_absorpt_process_details   'Bruker TWINABS'

_exptl_special_details           
; 
 A purple crystal of approximate dimensions 0.23 x 0.30 x 0.38 mm
 was mounted on a glass fiber and transferred to a Bruker SMART
 APEX II diffractometer.  The APEX2 program package and the CELL_NOW
 were used to determine the unit-cell parameters.  Data was collected
 using a 20 sec/frame scan time for a sphere of diffraction data.  The
 raw frame data was processed using SAINT and TWINABS to yield the
 reflection data file (HKLF 5 format).  Subsequent calculations were
 carried out using the SHELXTL program. There was one molecule of
 tetrahydrofuran solvent present.

 APEX2  Version 2011.4-1, Bruker AXS, Inc.; Madison, WI  2011. 
 Sheldrick, G. M. CELL_NOW, Version 2008-2, Bruker AXS, Inc.; Madison, WI  2008. 
 SAINT  Version 7.68a, Bruker AXS, Inc.; Madison, WI  2009.
 Sheldrick, G. M. TWINABS, Version 2008/4, Bruker AXS, Inc.; Madison, WI  2008. 
 Sheldrick, G. M. SHELXTL, Version 2008/4, Bruker AXS, Inc.; Madison, WI  2008. 
  

;

_diffrn_ambient_temperature      88(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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            7481
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0298
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.54
_diffrn_reflns_theta_max         26.37
_reflns_number_total             7482
_reflns_number_gt                6866
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_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.  The structure
 was refined as a non-merohedral twin, BASF = 0.484.
;

_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)+(0.0317P)²+3.9620P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7482
_refine_ls_number_parameters     410
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0473
_refine_ls_R_factor_gt           0.0410
_refine_ls_wR_factor_ref         0.0994
_refine_ls_wR_factor_gt          0.0961
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_restrained_S_all      1.111
_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 0.49264(3) 0.22649(5) 0.147366(19) 0.01654(10) Uani 1 1 d . . .
Cl1 Cl 0.42380(5) 0.03864(7) 0.13182(4) 0.02693(17) Uani 1 1 d . . .
Cl2 Cl 0.55197(5) 0.42223(7) 0.13661(4) 0.02875(17) Uani 1 1 d . . .
O1 O 0.58789(12) 0.15040(19) 0.16592(9) 0.0185(4) Uani 1 1 d . . .
O2 O 0.39978(12) 0.30295(19) 0.16704(9) 0.0191(4) Uani 1 1 d . . .
O3 O 0.50161(11) 0.2165(2) 0.04709(8) 0.0245(5) Uani 1 1 d . . .
N1 N 0.49903(15) 0.2236(2) 0.24524(9) 0.0157(4) Uani 1 1 d . . .
C1 C 0.61613(17) 0.1242(3) 0.22683(13) 0.0161(6) Uani 1 1 d . . .
C2 C 0.68916(16) 0.0629(3) 0.24265(13) 0.0173(6) Uani 1 1 d . . .
C3 C 0.70667(17) 0.0435(3) 0.30850(14) 0.0180(6) Uani 1 1 d . . .
H3A H 0.7562 0.0048 0.3211 0.022 Uiso 1 1 calc R . .
C4 C 0.65567(16) 0.0774(2) 0.35840(13) 0.0165(5) Uani 1 1 d . . .
C5 C 0.58398(18) 0.1375(3) 0.34125(13) 0.0181(6) Uani 1 1 d . . .
H5A H 0.5485 0.1605 0.3741 0.022 Uiso 1 1 calc R . .
C6 C 0.56444(16) 0.1640(3) 0.27518(13) 0.0165(5) Uani 1 1 d . . .
C7 C 0.74493(17) 0.0251(3) 0.18810(14) 0.0202(6) Uani 1 1 d . . .
C8 C 0.8182(2) -0.0453(4) 0.21604(16) 0.0339(8) Uani 1 1 d . . .
H8A H 0.8480 0.0070 0.2482 0.051 Uiso 1 1 calc R . .
H8B H 0.8529 -0.0666 0.1805 0.051 Uiso 1 1 calc R . .
H8C H 0.8009 -0.1215 0.2374 0.051 Uiso 1 1 calc R . .
C9 C 0.69951(19) -0.0591(3) 0.13800(16) 0.0293(7) Uani 1 1 d . . .
H9A H 0.6836 -0.1357 0.1596 0.044 Uiso 1 1 calc R . .
H9B H 0.7344 -0.0793 0.1024 0.044 Uiso 1 1 calc R . .
H9C H 0.6516 -0.0159 0.1200 0.044 Uiso 1 1 calc R . .
C10 C 0.7718(2) 0.1439(3) 0.15428(15) 0.0275(7) Uani 1 1 d . . .
H10A H 0.7976 0.1997 0.1869 0.041 Uiso 1 1 calc R . .
H10B H 0.7249 0.1853 0.1331 0.041 Uiso 1 1 calc R . .
H10C H 0.8099 0.1228 0.1212 0.041 Uiso 1 1 calc R . .
C11 C 0.68023(17) 0.0532(3) 0.43080(13) 0.0188(6) Uani 1 1 d . . .
C12 C 0.7263(2) -0.0687(3) 0.43961(16) 0.0384(9) Uani 1 1 d . . .
H12A H 0.7382 -0.0840 0.4864 0.058 Uiso 1 1 calc R . .
H12B H 0.7766 -0.0634 0.4171 0.058 Uiso 1 1 calc R . .
H12C H 0.6938 -0.1370 0.4209 0.058 Uiso 1 1 calc R . .
C13 C 0.6083(2) 0.0486(4) 0.47373(15) 0.0360(8) Uani 1 1 d . . .
H13A H 0.6265 0.0266 0.5187 0.054 Uiso 1 1 calc R . .
H13B H 0.5701 -0.0139 0.4565 0.054 Uiso 1 1 calc R . .
H13C H 0.5822 0.1301 0.4736 0.054 Uiso 1 1 calc R . .
C14 C 0.7352(3) 0.1596(4) 0.45478(17) 0.0426(10) Uani 1 1 d . . .
H14A H 0.7524 0.1458 0.5009 0.064 Uiso 1 1 calc R . .
H14B H 0.7060 0.2384 0.4506 0.064 Uiso 1 1 calc R . .
H14C H 0.7824 0.1626 0.4282 0.064 Uiso 1 1 calc R . .
C15 C 0.38128(17) 0.3294(3) 0.22792(13) 0.0161(6) Uani 1 1 d . . .
C16 C 0.31182(16) 0.3941(2) 0.24431(13) 0.0157(6) Uani 1 1 d . . .
C17 C 0.30347(17) 0.4130(3) 0.31088(13) 0.0176(6) Uani 1 1 d . . .
H17A H 0.2566 0.4542 0.3240 0.021 Uiso 1 1 calc R . .
C18 C 0.36053(16) 0.3744(3) 0.36010(13) 0.0162(5) Uani 1 1 d . . .
C19 C 0.42790(17) 0.3103(2) 0.34224(13) 0.0162(6) Uani 1 1 d . . .
H19A H 0.4669 0.2834 0.3748 0.019 Uiso 1 1 calc R . .
C20 C 0.43826(16) 0.2856(3) 0.27581(13) 0.0161(5) Uani 1 1 d . . .
C21 C 0.25134(17) 0.4379(3) 0.19084(13) 0.0192(6) Uani 1 1 d . . .
C22 C 0.2916(2) 0.5271(3) 0.14355(15) 0.0274(7) Uani 1 1 d . . .
H22A H 0.3088 0.6024 0.1672 0.041 Uiso 1 1 calc R . .
H22B H 0.2532 0.5492 0.1074 0.041 Uiso 1 1 calc R . .
H22C H 0.3383 0.4864 0.1259 0.041 Uiso 1 1 calc R . .
C23 C 0.21762(18) 0.3243(3) 0.15309(15) 0.0237(6) Uani 1 1 d . . .
H23A H 0.1932 0.2672 0.1837 0.036 Uiso 1 1 calc R . .
H23B H 0.2612 0.2818 0.1318 0.036 Uiso 1 1 calc R . .
H23C H 0.1770 0.3513 0.1197 0.036 Uiso 1 1 calc R . .
C24 C 0.18127(19) 0.5078(3) 0.21912(16) 0.0272(7) Uani 1 1 d . . .
H24A H 0.1533 0.4529 0.2486 0.041 Uiso 1 1 calc R . .
H24B H 0.1440 0.5350 0.1833 0.041 Uiso 1 1 calc R . .
H24C H 0.2017 0.5805 0.2436 0.041 Uiso 1 1 calc R . .
C25 C 0.34729(18) 0.4052(3) 0.43238(13) 0.0200(6) Uani 1 1 d . . .
C26 C 0.4115(2) 0.3476(3) 0.47893(14) 0.0306(7) Uani 1 1 d . . .
H26A H 0.4099 0.2570 0.4746 0.046 Uiso 1 1 calc R . .
H26B H 0.4014 0.3709 0.5242 0.046 Uiso 1 1 calc R . .
H26C H 0.4644 0.3780 0.4679 0.046 Uiso 1 1 calc R . .
C27 C 0.26521(19) 0.3575(3) 0.45014(14) 0.0273(7) Uani 1 1 d . . .
H27A H 0.2624 0.2676 0.4428 0.041 Uiso 1 1 calc R . .
H27B H 0.2233 0.3988 0.4226 0.041 Uiso 1 1 calc R . .
H27C H 0.2572 0.3753 0.4964 0.041 Uiso 1 1 calc R . .
C28 C 0.3505(2) 0.5465(3) 0.44126(16) 0.0348(8) Uani 1 1 d . . .
H28A H 0.4012 0.5782 0.4259 0.052 Uiso 1 1 calc R . .
H28B H 0.3466 0.5669 0.4878 0.052 Uiso 1 1 calc R . .
H28C H 0.3056 0.5847 0.4158 0.052 Uiso 1 1 calc R . .
C29 C 0.57636(18) 0.2226(4) 0.01324(15) 0.0328(7) Uani 1 1 d . . .
H29A H 0.5973 0.1382 0.0052 0.039 Uiso 1 1 calc R . .
H29B H 0.6176 0.2702 0.0393 0.039 Uiso 1 1 calc R . .
C30 C 0.5542(2) 0.2872(4) -0.05019(16) 0.0362(8) Uani 1 1 d . . .
H30A H 0.5882 0.2586 -0.0855 0.043 Uiso 1 1 calc R . .
H30B H 0.5597 0.3784 -0.0455 0.043 Uiso 1 1 calc R . .
C31 C 0.4676(2) 0.2506(3) -0.06435(14) 0.0315(8) Uani 1 1 d . . .
H31A H 0.4387 0.3137 -0.0919 0.038 Uiso 1 1 calc R . .
H31B H 0.4635 0.1691 -0.0867 0.038 Uiso 1 1 calc R . .
C32 C 0.4354(2) 0.2444(5) 0.00248(16) 0.0485(11) Uani 1 1 d . . .
H32A H 0.4110 0.3248 0.0139 0.058 Uiso 1 1 calc R . .
H32B H 0.3939 0.1788 0.0041 0.058 Uiso 1 1 calc R . .
O4 O 0.5105(2) 0.6830(4) 0.34664(13) 0.0756(11) Uani 1 1 d . . .
C33 C 0.5251(3) 0.8089(5) 0.3284(3) 0.085(2) Uani 1 1 d . . .
H33A H 0.5754 0.8399 0.3506 0.102 Uiso 1 1 calc R . .
H33B H 0.4803 0.8631 0.3405 0.102 Uiso 1 1 calc R . .
C34 C 0.5318(3) 0.8074(4) 0.2569(3) 0.0777(18) Uani 1 1 d . . .
H34A H 0.5159 0.8885 0.2374 0.093 Uiso 1 1 calc R . .
H34B H 0.5872 0.7878 0.2454 0.093 Uiso 1 1 calc R . .
C35 C 0.4761(3) 0.7094(4) 0.23455(18) 0.0530(11) Uani 1 1 d . . .
H35A H 0.4957 0.6661 0.1958 0.064 Uiso 1 1 calc R . .
H35B H 0.4221 0.7438 0.2232 0.064 Uiso 1 1 calc R . .
C36 C 0.4742(2) 0.6242(3) 0.29163(17) 0.0368(8) Uani 1 1 d . . .
H36A H 0.4180 0.6028 0.3001 0.044 Uiso 1 1 calc R . .
H36B H 0.5032 0.5466 0.2823 0.044 Uiso 1 1 calc R . .


_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 O1 1.811(2) . ?
V1 O2 1.819(2) . ?
V1 N1 1.9955(19) . ?
V1 O3 2.0632(18) . ?
V1 Cl1 2.3399(9) . ?
V1 Cl2 2.3443(9) . ?
O1 C1 1.336(3) . ?
O2 C15 1.327(3) . ?
O3 C32 1.426(4) . ?
O3 C29 1.460(3) . ?
N1 C6 1.381(4) . ?
N1 C20 1.390(3) . ?
C1 C2 1.409(4) . ?
C1 C6 1.412(4) . ?
C2 C3 1.376(4) . ?
C2 C7 1.543(4) . ?
C3 C4 1.410(4) . ?
C4 C5 1.389(4) . ?
C4 C11 1.535(4) . ?
C5 C6 1.400(4) . ?
C7 C8 1.525(4) . ?
C7 C10 1.532(4) . ?
C7 C9 1.537(4) . ?
C11 C13 1.524(4) . ?
C11 C12 1.528(4) . ?
C11 C14 1.532(4) . ?
C15 C16 1.408(4) . ?
C15 C20 1.409(4) . ?
C16 C17 1.388(4) . ?
C16 C21 1.522(4) . ?
C17 C18 1.410(4) . ?
C18 C19 1.384(4) . ?
C18 C25 1.540(4) . ?
C19 C20 1.402(4) . ?
C21 C24 1.530(4) . ?
C21 C23 1.537(4) . ?
C21 C22 1.541(4) . ?
C25 C27 1.525(4) . ?
C25 C26 1.526(4) . ?
C25 C28 1.533(4) . ?
C29 C30 1.499(5) . ?
C30 C31 1.512(4) . ?
C31 C32 1.494(4) . ?
O4 C36 1.399(5) . ?
O4 C33 1.431(7) . ?
C33 C34 1.468(8) . ?
C34 C35 1.463(6) . ?
C35 C36 1.485(5) . ?

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
O1 V1 O2 155.21(8) . . ?
O1 V1 N1 77.51(9) . . ?
O2 V1 N1 77.70(9) . . ?
O1 V1 O3 94.29(8) . . ?
O2 V1 O3 110.50(8) . . ?
N1 V1 O3 171.80(9) . . ?
O1 V1 Cl1 93.24(7) . . ?
O2 V1 Cl1 90.18(7) . . ?
N1 V1 Cl1 97.00(8) . . ?
O3 V1 Cl1 83.19(7) . . ?
O1 V1 Cl2 93.21(7) . . ?
O2 V1 Cl2 89.01(7) . . ?
N1 V1 Cl2 96.18(8) . . ?
O3 V1 Cl2 84.29(7) . . ?
Cl1 V1 Cl2 166.31(3) . . ?
C1 O1 V1 123.55(18) . . ?
C15 O2 V1 123.18(18) . . ?
C32 O3 C29 110.0(2) . . ?
C32 O3 V1 121.87(18) . . ?
C29 O3 V1 125.20(17) . . ?
C6 N1 C20 127.11(19) . . ?
C6 N1 V1 116.71(18) . . ?
C20 N1 V1 116.14(18) . . ?
O1 C1 C2 124.8(3) . . ?
O1 C1 C6 112.8(2) . . ?
C2 C1 C6 122.4(2) . . ?
C3 C2 C1 115.6(2) . . ?
C3 C2 C7 124.1(2) . . ?
C1 C2 C7 120.4(2) . . ?
C2 C3 C4 124.1(3) . . ?
C5 C4 C3 118.9(2) . . ?
C5 C4 C11 120.3(2) . . ?
C3 C4 C11 120.7(2) . . ?
C4 C5 C6 119.4(3) . . ?
N1 C6 C5 131.2(2) . . ?
N1 C6 C1 109.3(2) . . ?
C5 C6 C1 119.5(2) . . ?
C8 C7 C10 109.6(3) . . ?
C8 C7 C9 108.3(3) . . ?
C10 C7 C9 109.8(3) . . ?
C8 C7 C2 111.3(2) . . ?
C10 C7 C2 107.9(2) . . ?
C9 C7 C2 109.9(2) . . ?
C13 C11 C12 108.1(3) . . ?
C13 C11 C14 108.5(3) . . ?
C12 C11 C14 108.4(3) . . ?
C13 C11 C4 112.4(2) . . ?
C12 C11 C4 111.5(2) . . ?
C14 C11 C4 107.8(2) . . ?
O2 C15 C16 124.3(2) . . ?
O2 C15 C20 113.3(2) . . ?
C16 C15 C20 122.3(2) . . ?
C17 C16 C15 115.6(2) . . ?
C17 C16 C21 124.0(2) . . ?
C15 C16 C21 120.4(2) . . ?
C16 C17 C18 123.7(3) . . ?
C19 C18 C17 119.1(2) . . ?
C19 C18 C25 121.3(2) . . ?
C17 C18 C25 119.6(2) . . ?
C18 C19 C20 119.6(3) . . ?
N1 C20 C19 131.0(2) . . ?
N1 C20 C15 109.4(2) . . ?
C19 C20 C15 119.6(2) . . ?
C16 C21 C24 111.9(2) . . ?
C16 C21 C23 108.9(2) . . ?
C24 C21 C23 108.3(2) . . ?
C16 C21 C22 110.4(2) . . ?
C24 C21 C22 107.3(2) . . ?
C23 C21 C22 110.0(2) . . ?
C27 C25 C26 109.0(2) . . ?
C27 C25 C28 109.4(3) . . ?
C26 C25 C28 108.1(3) . . ?
C27 C25 C18 109.4(2) . . ?
C26 C25 C18 112.2(2) . . ?
C28 C25 C18 108.7(2) . . ?
O3 C29 C30 104.6(2) . . ?
C29 C30 C31 103.5(3) . . ?
C32 C31 C30 102.9(3) . . ?
O3 C32 C31 106.8(3) . . ?
C36 O4 C33 107.0(4) . . ?
O4 C33 C34 105.7(3) . . ?
C35 C34 C33 103.8(4) . . ?
C34 C35 C36 103.9(4) . . ?
O4 C36 C35 108.9(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 V1 O1 C1 3.4(4) . . . . ?
N1 V1 O1 C1 2.4(2) . . . . ?
O3 V1 O1 C1 -177.4(2) . . . . ?
Cl1 V1 O1 C1 -94.0(2) . . . . ?
Cl2 V1 O1 C1 98.0(2) . . . . ?
O1 V1 O2 C15 3.9(4) . . . . ?
N1 V1 O2 C15 4.9(2) . . . . ?
O3 V1 O2 C15 -175.2(2) . . . . ?
Cl1 V1 O2 C15 102.0(2) . . . . ?
Cl2 V1 O2 C15 -91.7(2) . . . . ?
O1 V1 O3 C32 169.0(3) . . . . ?
O2 V1 O3 C32 -11.4(3) . . . . ?
N1 V1 O3 C32 168.1(7) . . . . ?
Cl1 V1 O3 C32 76.2(3) . . . . ?
Cl2 V1 O3 C32 -98.2(3) . . . . ?
O1 V1 O3 C29 -32.5(3) . . . . ?
O2 V1 O3 C29 147.1(3) . . . . ?
N1 V1 O3 C29 -33.5(8) . . . . ?
Cl1 V1 O3 C29 -125.3(3) . . . . ?
Cl2 V1 O3 C29 60.3(3) . . . . ?
O1 V1 N1 C6 -3.4(2) . . . . ?
O2 V1 N1 C6 177.0(2) . . . . ?
O3 V1 N1 C6 -2.5(8) . . . . ?
Cl1 V1 N1 C6 88.4(2) . . . . ?
Cl2 V1 N1 C6 -95.3(2) . . . . ?
O1 V1 N1 C20 174.5(2) . . . . ?
O2 V1 N1 C20 -5.1(2) . . . . ?
O3 V1 N1 C20 175.4(6) . . . . ?
Cl1 V1 N1 C20 -93.7(2) . . . . ?
Cl2 V1 N1 C20 82.6(2) . . . . ?
V1 O1 C1 C2 178.6(2) . . . . ?
V1 O1 C1 C6 -1.0(3) . . . . ?
O1 C1 C2 C3 -179.2(3) . . . . ?
C6 C1 C2 C3 0.4(4) . . . . ?
O1 C1 C2 C7 2.5(4) . . . . ?
C6 C1 C2 C7 -177.9(3) . . . . ?
C1 C2 C3 C4 2.0(4) . . . . ?
C7 C2 C3 C4 -179.7(3) . . . . ?
C2 C3 C4 C5 -1.9(4) . . . . ?
C2 C3 C4 C11 -179.5(3) . . . . ?
C3 C4 C5 C6 -0.6(4) . . . . ?
C11 C4 C5 C6 177.0(3) . . . . ?
C20 N1 C6 C5 7.6(5) . . . . ?
V1 N1 C6 C5 -174.7(3) . . . . ?
C20 N1 C6 C1 -173.9(3) . . . . ?
V1 N1 C6 C1 3.7(3) . . . . ?
C4 C5 C6 N1 -178.8(3) . . . . ?
C4 C5 C6 C1 2.9(4) . . . . ?
O1 C1 C6 N1 -1.9(3) . . . . ?
C2 C1 C6 N1 178.5(3) . . . . ?
O1 C1 C6 C5 176.8(2) . . . . ?
C2 C1 C6 C5 -2.9(4) . . . . ?
C3 C2 C7 C8 4.6(4) . . . . ?
C1 C2 C7 C8 -177.2(3) . . . . ?
C3 C2 C7 C10 -115.8(3) . . . . ?
C1 C2 C7 C10 62.4(3) . . . . ?
C3 C2 C7 C9 124.5(3) . . . . ?
C1 C2 C7 C9 -57.3(3) . . . . ?
C5 C4 C11 C13 24.5(4) . . . . ?
C3 C4 C11 C13 -157.9(3) . . . . ?
C5 C4 C11 C12 146.2(3) . . . . ?
C3 C4 C11 C12 -36.3(4) . . . . ?
C5 C4 C11 C14 -95.0(3) . . . . ?
C3 C4 C11 C14 82.6(3) . . . . ?
V1 O2 C15 C16 176.6(2) . . . . ?
V1 O2 C15 C20 -3.7(3) . . . . ?
O2 C15 C16 C17 -179.8(3) . . . . ?
C20 C15 C16 C17 0.6(4) . . . . ?
O2 C15 C16 C21 0.6(4) . . . . ?
C20 C15 C16 C21 -179.0(3) . . . . ?
C15 C16 C17 C18 1.7(4) . . . . ?
C21 C16 C17 C18 -178.7(3) . . . . ?
C16 C17 C18 C19 -2.2(4) . . . . ?
C16 C17 C18 C25 177.2(3) . . . . ?
C17 C18 C19 C20 0.2(4) . . . . ?
C25 C18 C19 C20 -179.2(3) . . . . ?
C6 N1 C20 C19 3.6(5) . . . . ?
V1 N1 C20 C19 -174.1(2) . . . . ?
C6 N1 C20 C15 -177.8(3) . . . . ?
V1 N1 C20 C15 4.5(3) . . . . ?
C18 C19 C20 N1 -179.6(3) . . . . ?
C18 C19 C20 C15 2.0(4) . . . . ?
O2 C15 C20 N1 -0.9(3) . . . . ?
C16 C15 C20 N1 178.8(3) . . . . ?
O2 C15 C20 C19 177.9(2) . . . . ?
C16 C15 C20 C19 -2.4(4) . . . . ?
C17 C16 C21 C24 1.3(4) . . . . ?
C15 C16 C21 C24 -179.1(3) . . . . ?
C17 C16 C21 C23 -118.4(3) . . . . ?
C15 C16 C21 C23 61.2(3) . . . . ?
C17 C16 C21 C22 120.7(3) . . . . ?
C15 C16 C21 C22 -59.7(3) . . . . ?
C19 C18 C25 C27 -126.1(3) . . . . ?
C17 C18 C25 C27 54.5(3) . . . . ?
C19 C18 C25 C26 -5.1(4) . . . . ?
C17 C18 C25 C26 175.6(3) . . . . ?
C19 C18 C25 C28 114.5(3) . . . . ?
C17 C18 C25 C28 -64.9(4) . . . . ?
C32 O3 C29 C30 14.1(4) . . . . ?
V1 O3 C29 C30 -146.6(2) . . . . ?
O3 C29 C30 C31 -30.2(4) . . . . ?
C29 C30 C31 C32 34.8(4) . . . . ?
C29 O3 C32 C31 8.2(4) . . . . ?
V1 O3 C32 C31 169.6(2) . . . . ?
C30 C31 C32 O3 -26.8(4) . . . . ?
C36 O4 C33 C34 -25.8(5) . . . . ?
O4 C33 C34 C35 33.4(5) . . . . ?
C33 C34 C35 C36 -27.6(5) . . . . ?
C33 O4 C36 C35 8.0(5) . . . . ?
C34 C35 C36 O4 12.7(5) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.592
_refine_diff_density_min         -0.346
_refine_diff_density_rms         0.064

_database_code_depnum_ccdc_archive 'CCDC 1015033'
#######################################################################
#
#                 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_afh295

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C37 H62 Cl2 N Nb O3'
_chemical_formula_weight         732.68

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

_shelx_space_group_comment       
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;

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

_cell_length_a                   14.5710(10)
_cell_length_b                   15.9423(11)
_cell_length_c                   17.0831(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3968.3(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    143(2)
_cell_measurement_reflns_used    9357
_cell_measurement_theta_min      2.24
_cell_measurement_theta_max      28.20

_exptl_crystal_description       prism
_exptl_crystal_colour            purple
_exptl_crystal_density_meas      not_measured
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.226
_exptl_crystal_F_000             1560
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.459
_exptl_crystal_size_mid          0.301
_exptl_crystal_size_min          0.174
_exptl_absorpt_coefficient_mu    0.470
_shelx_estimated_absorpt_T_min   0.813
_shelx_estimated_absorpt_T_max   0.923
_exptl_absorpt_correction_type   Numerical
_exptl_absorpt_correction_T_min  0.8456
_exptl_absorpt_correction_T_max  0.9450
_exptl_absorpt_process_details   'Bruker SADABS'

_exptl_special_details           
; 
 A purple crystal of approximate dimensions 0.459 x 0.301 x 
 0.174 mm was mounted on a glass fiber and transferred to a Bruker
 SMART APEX II diffractometer.  The APEX2 program package was used
 to determine the unit-cell parameters and for data collection 
 (20s sec/frame scan time for a sphere of diffraction data).  
 The raw frame data was processed using SAINT and SADABS to yield
 the reflection data file.  Subsequent calculations were carried out
 using the SHELXTL program.  The diffraction symmetry was mmm and the
 systematic absences were consistent with the orthorhombic space group
 P212121 that was later determined to be correct.

 APEX2 Version 2011.4-1, Bruker AXS, Inc.; Madison, WI 2011.
 SAINT  Version 7.68a, Bruker AXS, Inc.; Madison, WI  2007.
 Sheldrick, G. M. SADABS, Version 2008/1, Bruker AXS, Inc.; Madison, WI  2008. 
 Sheldrick, G. M. SHELXTL, Version 2014/2, Bruker AXS, Inc.; Madison, WI  2014
  
;

_diffrn_ambient_temperature      143(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            45745
_diffrn_reflns_av_unetI/netI     0.0172
_diffrn_reflns_av_R_equivalents  0.0220
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.747
_diffrn_reflns_theta_max         28.506
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             9374
_reflns_number_gt                9111
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.812
_reflns_Friedel_fraction_max     0.950
_reflns_Friedel_fraction_full    1.000

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 

 The structure was solved by direct methods and refined on F2 by
 full-matrix least-squares techniques.  The analytical scattering
 factors5 for neutral atoms were used throughout the analysis.  
 Hydrogen atoms were included using a riding model.  There was one
 molecule of pentane solvent present. At convergence, wR2 = 0.0587
 and Goof = 1.058 for 414 variables refined against 9374 data
 (0.74 Å), R1 = 0.0228 for those 9111 data with I > 2.0 sigma(I).  
 The model was refined as a two-component inversion twin

;

_computing_data_collection       'Bruker APEX2 2011.4-1, 2011'
_computing_cell_refinement       'Bruker SAINT 7.68a, 2009'
_computing_data_reduction        'Bruker SAINT 7.68a, 2009'
_computing_structure_solution    'Bruker SHELXTL 2008/4'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refined as a 2-component inversion twin. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0319P)²+1.1694P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.38(3)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         9374
_refine_ls_number_parameters     414
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0241
_refine_ls_R_factor_gt           0.0228
_refine_ls_wR_factor_ref         0.0587
_refine_ls_wR_factor_gt          0.0580
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.058
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Nb1 Nb -0.44982(2) 0.73256(2) -0.08971(2) 0.01724(5) Uani 1 1 d . . . . .
Cl1 Cl -0.49427(4) 0.72276(4) 0.04601(3) 0.02894(13) Uani 1 1 d . . . . .
Cl2 Cl -0.35822(4) 0.72891(5) -0.20566(3) 0.02966(12) Uani 1 1 d . . . . .
O1 O -0.48449(10) 0.84735(9) -0.09655(10) 0.0199(3) Uani 1 1 d . . . . .
O2 O -0.47978(10) 0.61757(9) -0.10155(10) 0.0204(3) Uani 1 1 d . . . . .
O3 O -0.31538(11) 0.76464(13) -0.03668(10) 0.0298(4) Uani 1 1 d . . . . .
N1 N -0.57734(11) 0.73133(13) -0.14329(10) 0.0181(3) Uani 1 1 d . . . . .
C1 C -0.62075(15) 0.80925(14) -0.15447(13) 0.0178(4) Uani 1 1 d . . . . .
C2 C -0.56638(15) 0.87495(14) -0.12531(13) 0.0178(4) Uani 1 1 d . . . . .
C3 C -0.59420(16) 0.95885(14) -0.12472(13) 0.0178(4) Uani 1 1 d . . . . .
C4 C -0.67999(16) 0.97444(14) -0.15732(13) 0.0189(4) Uani 1 1 d . . . . .
H4A H -0.7014 1.0307 -0.1586 0.023 Uiso 1 1 calc R U . . .
C5 C -0.73651(15) 0.91161(15) -0.18839(13) 0.0190(4) Uani 1 1 d . . . . .
C6 C -0.70699(15) 0.82879(14) -0.18636(13) 0.0194(4) Uani 1 1 d . . . . .
H6A H -0.7450 0.7855 -0.2065 0.023 Uiso 1 1 calc R U . . .
C7 C -0.53362(14) 1.02823(13) -0.08985(14) 0.0199(4) Uani 1 1 d . . . . .
C8 C -0.44353(19) 1.03320(16) -0.13635(15) 0.0289(5) Uani 1 1 d . . . . .
H8A H -0.4569 1.0481 -0.1908 0.043 Uiso 1 1 calc R U . . .
H8B H -0.4126 0.9787 -0.1347 0.043 Uiso 1 1 calc R U . . .
H8C H -0.4037 1.0760 -0.1131 0.043 Uiso 1 1 calc R U . . .
C9 C -0.51390(19) 1.00944(16) -0.00322(14) 0.0267(5) Uani 1 1 d . . . . .
H9A H -0.5716 1.0096 0.0262 0.040 Uiso 1 1 calc R U . . .
H9B H -0.4728 1.0525 0.0180 0.040 Uiso 1 1 calc R U . . .
H9C H -0.4847 0.9543 0.0014 0.040 Uiso 1 1 calc R U . . .
C10 C -0.58040(18) 1.11425(15) -0.09399(18) 0.0313(5) Uani 1 1 d . . . . .
H10A H -0.6389 1.1122 -0.0657 0.047 Uiso 1 1 calc R U . . .
H10B H -0.5917 1.1290 -0.1488 0.047 Uiso 1 1 calc R U . . .
H10C H -0.5405 1.1566 -0.0701 0.047 Uiso 1 1 calc R U . . .
C11 C -0.83051(16) 0.93553(15) -0.22221(14) 0.0225(5) Uani 1 1 d . . . . .
C12 C -0.81683(18) 0.99831(18) -0.28951(16) 0.0299(5) Uani 1 1 d . . . . .
H12A H -0.7812 0.9718 -0.3314 0.045 Uiso 1 1 calc R U . . .
H12B H -0.7838 1.0477 -0.2701 0.045 Uiso 1 1 calc R U . . .
H12C H -0.8768 1.0155 -0.3100 0.045 Uiso 1 1 calc R U . . .
C13 C -0.88291(18) 0.85960(17) -0.25423(17) 0.0327(6) Uani 1 1 d . . . . .
H13A H -0.8462 0.8323 -0.2950 0.049 Uiso 1 1 calc R U . . .
H13B H -0.9415 0.8782 -0.2765 0.049 Uiso 1 1 calc R U . . .
H13C H -0.8945 0.8198 -0.2117 0.049 Uiso 1 1 calc R U . . .
C14 C -0.88848(17) 0.97475(17) -0.15721(16) 0.0282(5) Uani 1 1 d . . . . .
H14A H -0.9010 0.9326 -0.1168 0.042 Uiso 1 1 calc R U . . .
H14B H -0.9466 0.9949 -0.1792 0.042 Uiso 1 1 calc R U . . .
H14C H -0.8550 1.0219 -0.1340 0.042 Uiso 1 1 calc R U . . .
C15 C -0.61490(15) 0.65228(14) -0.16214(13) 0.0175(4) Uani 1 1 d . . . . .
C16 C -0.55824(16) 0.58799(14) -0.13493(12) 0.0177(4) Uani 1 1 d . . . . .
C17 C -0.58016(16) 0.50308(14) -0.14028(13) 0.0185(4) Uani 1 1 d . . . . .
C18 C -0.66290(16) 0.48477(14) -0.17811(13) 0.0208(5) Uani 1 1 d . . . . .
H18A H -0.6809 0.4277 -0.1828 0.025 Uiso 1 1 calc R U . . .
C19 C -0.71995(16) 0.54612(15) -0.20919(13) 0.0202(4) Uani 1 1 d . . . . .
C20 C -0.69578(16) 0.63020(15) -0.20124(13) 0.0201(4) Uani 1 1 d . . . . .
H20A H -0.7342 0.6726 -0.2224 0.024 Uiso 1 1 calc R U . . .
C21 C -0.51738(17) 0.43506(14) -0.10560(14) 0.0226(5) Uani 1 1 d . . . . .
C22 C -0.42356(19) 0.43861(18) -0.14504(18) 0.0350(6) Uani 1 1 d . . . . .
H22A H -0.3829 0.3969 -0.1211 0.052 Uiso 1 1 calc R U . . .
H22B H -0.3972 0.4947 -0.1383 0.052 Uiso 1 1 calc R U . . .
H22C H -0.4303 0.4265 -0.2010 0.052 Uiso 1 1 calc R U . . .
C23 C -0.5079(2) 0.44958(18) -0.01758(16) 0.0358(6) Uani 1 1 d . . . . .
H23A H -0.4662 0.4076 0.0046 0.054 Uiso 1 1 calc R U . . .
H23B H -0.5682 0.4447 0.0073 0.054 Uiso 1 1 calc R U . . .
H23C H -0.4830 0.5058 -0.0082 0.054 Uiso 1 1 calc R U . . .
C24 C -0.5565(2) 0.34720(16) -0.1184(2) 0.0450(8) Uani 1 1 d . . . . .
H24A H -0.5147 0.3055 -0.0959 0.068 Uiso 1 1 calc R U . . .
H24B H -0.5633 0.3368 -0.1746 0.068 Uiso 1 1 calc R U . . .
H24C H -0.6165 0.3429 -0.0929 0.068 Uiso 1 1 calc R U . . .
C25 C -0.81277(17) 0.52369(16) -0.24766(15) 0.0253(5) Uani 1 1 d . . . . .
C26 C -0.8179(2) 0.42999(18) -0.26852(19) 0.0404(7) Uani 1 1 d . . . . .
H26A H -0.7663 0.4152 -0.3026 0.061 Uiso 1 1 calc R U . . .
H26B H -0.8757 0.4185 -0.2958 0.061 Uiso 1 1 calc R U . . .
H26C H -0.8150 0.3965 -0.2205 0.061 Uiso 1 1 calc R U . . .
C27 C -0.8265(2) 0.57352(19) -0.32300(17) 0.0361(6) Uani 1 1 d . . . . .
H27A H -0.8314 0.6334 -0.3105 0.054 Uiso 1 1 calc R U . . .
H27B H -0.8829 0.5548 -0.3489 0.054 Uiso 1 1 calc R U . . .
H27C H -0.7741 0.5644 -0.3579 0.054 Uiso 1 1 calc R U . . .
C28 C -0.8892(2) 0.5446(2) -0.19013(19) 0.0461(8) Uani 1 1 d . . . . .
H28A H -0.8868 0.6045 -0.1771 0.069 Uiso 1 1 calc R U . . .
H28B H -0.8814 0.5114 -0.1424 0.069 Uiso 1 1 calc R U . . .
H28C H -0.9487 0.5316 -0.2139 0.069 Uiso 1 1 calc R U . . .
C29 C -0.2483(2) 0.90293(19) -0.01105(18) 0.0394(7) Uani 1 1 d . . . . .
H29A H -0.2431 0.9469 0.0288 0.059 Uiso 1 1 calc R U . . .
H29B H -0.2778 0.9260 -0.0579 0.059 Uiso 1 1 calc R U . . .
H29C H -0.1870 0.8822 -0.0246 0.059 Uiso 1 1 calc R U . . .
C30 C -0.30523(19) 0.83178(18) 0.02051(16) 0.0328(6) Uani 1 1 d . . . . .
H30A H -0.2758 0.8092 0.0683 0.039 Uiso 1 1 calc R U . . .
H30B H -0.3667 0.8531 0.0352 0.039 Uiso 1 1 calc R U . . .
C31 C -0.23068(17) 0.71790(19) -0.04957(17) 0.0372(7) Uani 1 1 d . . . . .
H31A H -0.1832 0.7370 -0.0121 0.045 Uiso 1 1 calc R U . . .
H31B H -0.2079 0.7285 -0.1032 0.045 Uiso 1 1 calc R U . . .
C32 C -0.2475(2) 0.6261(2) -0.0389(2) 0.0438(7) Uani 1 1 d . . . . .
H32A H -0.1897 0.5954 -0.0452 0.066 Uiso 1 1 calc R U . . .
H32B H -0.2918 0.6067 -0.0780 0.066 Uiso 1 1 calc R U . . .
H32C H -0.2721 0.6160 0.0137 0.066 Uiso 1 1 calc R U . . .
C33 C -0.2504(3) 0.2583(3) -0.0454(2) 0.0751(12) Uani 1 1 d . . . . .
H33A H -0.2556 0.2325 -0.0973 0.113 Uiso 1 1 calc R U . . .
H33B H -0.1917 0.2423 -0.0216 0.113 Uiso 1 1 calc R U . . .
H33C H -0.2534 0.3194 -0.0504 0.113 Uiso 1 1 calc R U . . .
C34 C -0.3276(3) 0.2285(3) 0.0054(2) 0.0702(11) Uani 1 1 d . . . . .
H34A H -0.3228 0.1669 0.0113 0.084 Uiso 1 1 calc R U . . .
H34B H -0.3864 0.2407 -0.0214 0.084 Uiso 1 1 calc R U . . .
C35 C -0.3296(2) 0.2676(2) 0.0850(2) 0.0481(7) Uani 1 1 d . . . . .
H35A H -0.3259 0.3292 0.0792 0.058 Uiso 1 1 calc R U . . .
H35B H -0.2747 0.2490 0.1144 0.058 Uiso 1 1 calc R U . . .
C36 C -0.4148(3) 0.2461(2) 0.1326(3) 0.0654(11) Uani 1 1 d . . . . .
H36A H -0.4211 0.1844 0.1356 0.079 Uiso 1 1 calc R U . . .
H36B H -0.4696 0.2683 0.1053 0.079 Uiso 1 1 calc R U . . .
C37 C -0.4119(3) 0.2830(2) 0.2183(3) 0.0666(12) Uani 1 1 d . . . . .
H37A H -0.4687 0.2684 0.2458 0.100 Uiso 1 1 calc R U . . .
H37B H -0.4059 0.3442 0.2158 0.100 Uiso 1 1 calc R U . . .
H37C H -0.3593 0.2594 0.2464 0.100 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Nb1 O2 1.8953(15) . ?
Nb1 O1 1.9020(15) . ?
Nb1 N1 2.0714(16) . ?
Nb1 O3 2.2181(16) . ?
Nb1 Cl2 2.3893(6) . ?
Nb1 Cl1 2.4123(6) . ?
O1 C2 1.363(3) . ?
O2 C16 1.362(3) . ?
O3 C30 1.457(3) . ?
O3 C31 1.458(3) . ?
N1 C1 1.407(3) . ?
N1 C15 1.411(3) . ?
C1 C2 1.405(3) . ?
C1 C6 1.405(3) . ?
C2 C3 1.398(3) . ?
C3 C4 1.391(3) . ?
C3 C7 1.535(3) . ?
C4 C5 1.401(3) . ?
C5 C6 1.389(3) . ?
C5 C11 1.535(3) . ?
C7 C10 1.533(3) . ?
C7 C8 1.536(3) . ?
C7 C9 1.537(3) . ?
C11 C14 1.529(3) . ?
C11 C13 1.532(3) . ?
C11 C12 1.537(3) . ?
C15 C16 1.396(3) . ?
C15 C20 1.400(3) . ?
C16 C17 1.394(3) . ?
C17 C18 1.399(3) . ?
C17 C21 1.537(3) . ?
C18 C19 1.389(3) . ?
C19 C20 1.393(3) . ?
C19 C25 1.546(3) . ?
C21 C22 1.525(4) . ?
C21 C23 1.528(3) . ?
C21 C24 1.528(3) . ?
C25 C28 1.523(4) . ?
C25 C27 1.526(4) . ?
C25 C26 1.538(4) . ?
C29 C30 1.505(4) . ?
C31 C32 1.495(4) . ?
C33 C34 1.497(6) . ?
C34 C35 1.497(5) . ?
C35 C36 1.523(5) . ?
C36 C37 1.578(6) . ?

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
O2 Nb1 O1 149.64(6) . . ?
O2 Nb1 N1 74.76(7) . . ?
O1 Nb1 N1 75.15(7) . . ?
O2 Nb1 O3 118.04(7) . . ?
O1 Nb1 O3 92.17(7) . . ?
N1 Nb1 O3 167.13(8) . . ?
O2 Nb1 Cl2 90.95(5) . . ?
O1 Nb1 Cl2 96.94(6) . . ?
N1 Nb1 Cl2 97.73(5) . . ?
O3 Nb1 Cl2 81.42(5) . . ?
O2 Nb1 Cl1 88.74(5) . . ?
O1 Nb1 Cl1 92.87(6) . . ?
N1 Nb1 Cl1 100.56(5) . . ?
O3 Nb1 Cl1 81.93(5) . . ?
Cl2 Nb1 Cl1 160.95(2) . . ?
C2 O1 Nb1 124.41(13) . . ?
C16 O2 Nb1 124.96(14) . . ?
C30 O3 C31 113.01(19) . . ?
C30 O3 Nb1 122.21(15) . . ?
C31 O3 Nb1 124.60(16) . . ?
C1 N1 C15 125.67(16) . . ?
C1 N1 Nb1 117.06(14) . . ?
C15 N1 Nb1 117.20(15) . . ?
C2 C1 C6 118.5(2) . . ?
C2 C1 N1 110.90(18) . . ?
C6 C1 N1 130.6(2) . . ?
O1 C2 C3 124.1(2) . . ?
O1 C2 C1 112.38(19) . . ?
C3 C2 C1 123.5(2) . . ?
C4 C3 C2 115.4(2) . . ?
C4 C3 C7 122.9(2) . . ?
C2 C3 C7 121.7(2) . . ?
C3 C4 C5 123.5(2) . . ?
C6 C5 C4 119.2(2) . . ?
C6 C5 C11 121.5(2) . . ?
C4 C5 C11 119.3(2) . . ?
C5 C6 C1 119.8(2) . . ?
C10 C7 C3 111.77(19) . . ?
C10 C7 C8 108.0(2) . . ?
C3 C7 C8 109.13(19) . . ?
C10 C7 C9 107.6(2) . . ?
C3 C7 C9 109.92(18) . . ?
C8 C7 C9 110.4(2) . . ?
C14 C11 C13 107.9(2) . . ?
C14 C11 C5 108.74(19) . . ?
C13 C11 C5 112.5(2) . . ?
C14 C11 C12 110.4(2) . . ?
C13 C11 C12 108.2(2) . . ?
C5 C11 C12 109.1(2) . . ?
C16 C15 C20 118.2(2) . . ?
C16 C15 N1 110.52(19) . . ?
C20 C15 N1 131.3(2) . . ?
O2 C16 C17 123.8(2) . . ?
O2 C16 C15 112.43(19) . . ?
C17 C16 C15 123.8(2) . . ?
C16 C17 C18 115.5(2) . . ?
C16 C17 C21 121.6(2) . . ?
C18 C17 C21 122.9(2) . . ?
C19 C18 C17 123.1(2) . . ?
C18 C19 C20 119.3(2) . . ?
C18 C19 C25 121.6(2) . . ?
C20 C19 C25 119.0(2) . . ?
C19 C20 C15 120.1(2) . . ?
C22 C21 C23 110.4(2) . . ?
C22 C21 C24 107.8(2) . . ?
C23 C21 C24 108.3(2) . . ?
C22 C21 C17 109.7(2) . . ?
C23 C21 C17 109.1(2) . . ?
C24 C21 C17 111.7(2) . . ?
C28 C25 C27 109.5(3) . . ?
C28 C25 C26 109.1(2) . . ?
C27 C25 C26 107.7(2) . . ?
C28 C25 C19 108.4(2) . . ?
C27 C25 C19 110.7(2) . . ?
C26 C25 C19 111.5(2) . . ?
O3 C30 C29 111.7(2) . . ?
O3 C31 C32 110.0(2) . . ?
C33 C34 C35 114.2(3) . . ?
C34 C35 C36 114.1(3) . . ?
C35 C36 C37 112.9(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 Nb1 O2 C16 8.2(2) . . . . ?
N1 Nb1 O2 C16 0.47(16) . . . . ?
O3 Nb1 O2 C16 -178.07(15) . . . . ?
Cl2 Nb1 O2 C16 -97.28(16) . . . . ?
Cl1 Nb1 O2 C16 101.77(16) . . . . ?
C15 N1 C1 C2 176.6(2) . . . . ?
Nb1 N1 C1 C2 -0.3(2) . . . . ?
C15 N1 C1 C6 -1.0(4) . . . . ?
Nb1 N1 C1 C6 -177.94(19) . . . . ?
Nb1 O1 C2 C3 174.96(16) . . . . ?
Nb1 O1 C2 C1 -4.0(3) . . . . ?
C6 C1 C2 O1 -179.67(19) . . . . ?
N1 C1 C2 O1 2.4(3) . . . . ?
C6 C1 C2 C3 1.4(3) . . . . ?
N1 C1 C2 C3 -176.6(2) . . . . ?
O1 C2 C3 C4 179.6(2) . . . . ?
C1 C2 C3 C4 -1.6(3) . . . . ?
O1 C2 C3 C7 -0.8(3) . . . . ?
C1 C2 C3 C7 178.0(2) . . . . ?
C2 C3 C4 C5 0.6(3) . . . . ?
C7 C3 C4 C5 -179.1(2) . . . . ?
C3 C4 C5 C6 0.7(3) . . . . ?
C3 C4 C5 C11 179.3(2) . . . . ?
C4 C5 C6 C1 -1.0(3) . . . . ?
C11 C5 C6 C1 -179.6(2) . . . . ?
C2 C1 C6 C5 0.0(3) . . . . ?
N1 C1 C6 C5 177.5(2) . . . . ?
C4 C3 C7 C10 1.3(3) . . . . ?
C2 C3 C7 C10 -178.3(2) . . . . ?
C4 C3 C7 C8 -118.1(2) . . . . ?
C2 C3 C7 C8 62.2(3) . . . . ?
C4 C3 C7 C9 120.7(2) . . . . ?
C2 C3 C7 C9 -58.9(3) . . . . ?
C6 C5 C11 C14 117.6(2) . . . . ?
C4 C5 C11 C14 -61.0(3) . . . . ?
C6 C5 C11 C13 -1.9(3) . . . . ?
C4 C5 C11 C13 179.5(2) . . . . ?
C6 C5 C11 C12 -121.9(2) . . . . ?
C4 C5 C11 C12 59.5(3) . . . . ?
C1 N1 C15 C16 -172.9(2) . . . . ?
Nb1 N1 C15 C16 4.0(2) . . . . ?
C1 N1 C15 C20 6.7(4) . . . . ?
Nb1 N1 C15 C20 -176.4(2) . . . . ?
Nb1 O2 C16 C17 -177.51(16) . . . . ?
Nb1 O2 C16 C15 1.6(3) . . . . ?
C20 C15 C16 O2 176.90(19) . . . . ?
N1 C15 C16 O2 -3.4(3) . . . . ?
C20 C15 C16 C17 -4.0(3) . . . . ?
N1 C15 C16 C17 175.7(2) . . . . ?
O2 C16 C17 C18 -178.7(2) . . . . ?
C15 C16 C17 C18 2.3(3) . . . . ?
O2 C16 C17 C21 2.1(3) . . . . ?
C15 C16 C17 C21 -176.9(2) . . . . ?
C16 C17 C18 C19 0.5(3) . . . . ?
C21 C17 C18 C19 179.7(2) . . . . ?
C17 C18 C19 C20 -1.6(4) . . . . ?
C17 C18 C19 C25 -177.5(2) . . . . ?
C18 C19 C20 C15 -0.1(3) . . . . ?
C25 C19 C20 C15 175.9(2) . . . . ?
C16 C15 C20 C19 2.8(3) . . . . ?
N1 C15 C20 C19 -176.8(2) . . . . ?
C16 C17 C21 C22 -61.0(3) . . . . ?
C18 C17 C21 C22 119.8(3) . . . . ?
C16 C17 C21 C23 59.9(3) . . . . ?
C18 C17 C21 C23 -119.2(3) . . . . ?
C16 C17 C21 C24 179.6(2) . . . . ?
C18 C17 C21 C24 0.4(3) . . . . ?
C18 C19 C25 C28 102.9(3) . . . . ?
C20 C19 C25 C28 -73.0(3) . . . . ?
C18 C19 C25 C27 -137.0(2) . . . . ?
C20 C19 C25 C27 47.1(3) . . . . ?
C18 C19 C25 C26 -17.1(3) . . . . ?
C20 C19 C25 C26 166.9(2) . . . . ?
C31 O3 C30 C29 70.9(3) . . . . ?
Nb1 O3 C30 C29 -113.8(2) . . . . ?
C30 O3 C31 C32 126.9(3) . . . . ?
Nb1 O3 C31 C32 -48.2(3) . . . . ?
C33 C34 C35 C36 172.4(3) . . . . ?
C34 C35 C36 C37 176.1(3) . . . . ?

_refine_diff_density_max         0.532
_refine_diff_density_min         -0.297
_refine_diff_density_rms         0.047

_shelxl_version_number           2014-2


_database_code_depnum_ccdc_archive 'CCDC 1015034'
#######################################################################
#
#                 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_afh346

_audit_creation_method           SHELXL-2012
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C31.50 H44 Cl3 N O2 V'
_chemical_formula_weight         625.96

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;

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

_cell_length_a                   9.5015(8)
_cell_length_b                   22.5812(19)
_cell_length_c                   31.221(3)
_cell_angle_alpha                90
_cell_angle_beta                 91.0821(14)
_cell_angle_gamma                90
_cell_volume                     6697.3(10)
_cell_formula_units_Z            8
_cell_measurement_temperature    143(2)
_cell_measurement_reflns_used    9933
_cell_measurement_theta_min      2.25
_cell_measurement_theta_max      27.11

_exptl_crystal_description       plate
_exptl_crystal_colour            purple
_exptl_crystal_density_meas      not_measured
_exptl_crystal_density_method    not_measured
_exptl_crystal_density_diffrn    1.242
_exptl_crystal_F_000             2640
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.316
_exptl_crystal_size_mid          0.241
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    0.562
_shelx_estimated_absorpt_T_min   0.842
_shelx_estimated_absorpt_T_max   0.967
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.753
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_process_details   'Bruker TWINABS'

_exptl_special_details           
; 
 A purple crystal of approximate dimensions 0.06 x 0.24 x 0.32 mm was
 mounted on a glass fiber and transferred to a Bruker SMART APEX II
 diffractometer.  The APEX2 program package and the CELL_NOW program were
 used to determine the unit-cell parameters.  Data was collected using
 a 45 sec/frame scan time for a sphere of diffraction data.  The raw
 frame data was processed using SAINT and TWINABS to yield the reflection
 data file (HKLF 5 format).

 APEX2  Version 2011.4-1, Bruker AXS, Inc.; Madison, WI  2011. 
 Sheldrick, G. M. CELL_NOW, Version 2008-2, Bruker AXS, Inc.; Madison, WI  2008.
 Sheldrick, G. M. TWINABS, Version 2008/4, Bruker AXS, Inc.; Madison, WI  2008. 
;

_diffrn_ambient_temperature      143(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            18750
_diffrn_reflns_av_unetI/netI     0.0646
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_theta_min         1.586
_diffrn_reflns_theta_max         24.712
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.914
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.914
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.914
_reflns_number_total             18750
_reflns_number_gt                12680
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. These statistics refer to single and 
 composite reflections containing twin component 1 only. 
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT, v7.68a'
_computing_data_reduction        'Bruker SAINT, v7.68a'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refined as a 2-component twin. The structure was solved by direct 
 methods and refined on F2 by full-matrix least-squares techniques.
 The analytical scattering factors6 for neutral atoms were used 
 throughout the analysis.  Hydrogen atoms were included using a 
 riding model.  There were two molecules of the formula-unit present
 and one-half molecule of toluene solvent present per formula-unit. 
 At convergence, wR2 = 0.1287 and Goof = 1.022 for 720 variables 
 refined against 18750 data (0.85Å), R1 = 0.0590 for those 12680 
 with I > 2.0 sigma(I).  

;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
; 
 w=1/[σ²(Fo²)+(0.0371P)²+10.1485P] 
 where P=(Fo²+2Fc²)/3 
;
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         18750
_refine_ls_number_parameters     720
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1041
_refine_ls_R_factor_gt           0.0590
_refine_ls_wR_factor_ref         0.1287
_refine_ls_wR_factor_gt          0.1124
_refine_ls_goodness_of_fit_ref   1.022
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.32029(7) 0.04601(3) 0.12457(3) 0.0265(2) Uani 1 1 d . . . . .
Cl1 Cl 0.51813(13) -0.00597(7) 0.12579(4) 0.0547(4) Uani 1 1 d . . . . .
Cl2 Cl 0.43779(12) 0.13601(6) 0.12879(4) 0.0425(3) Uani 1 1 d . . . . .
Cl3 Cl 0.17737(13) -0.03752(5) 0.12016(4) 0.0439(3) Uani 1 1 d . . . . .
N1 N 0.1317(3) 0.09721(15) 0.12536(12) 0.0208(8) Uani 1 1 d . . . . .
O1 O 0.2782(3) 0.05101(13) 0.18189(9) 0.0252(7) Uani 1 1 d . . . . .
O2 O 0.2797(3) 0.05980(13) 0.06729(9) 0.0259(7) Uani 1 1 d . . . . .
C1 C 0.0808(4) 0.10700(19) 0.16474(14) 0.0218(10) Uani 1 1 d . . . . .
C2 C 0.1673(4) 0.07734(18) 0.19652(14) 0.0198(10) Uani 1 1 d . . . . .
C3 C 0.1320(4) 0.07636(18) 0.24023(14) 0.0207(10) Uani 1 1 d . . . . .
C4 C 0.0137(4) 0.10777(18) 0.25019(15) 0.0225(10) Uani 1 1 d . . . . .
H4A H -0.0153 0.1071 0.2791 0.027 Uiso 1 1 calc R U . . .
C5 C -0.0696(4) 0.14149(18) 0.22031(15) 0.0219(10) Uani 1 1 d . . . . .
C6 C -0.0370(4) 0.14032(18) 0.17820(15) 0.0231(10) Uani 1 1 d . . . . .
H6A H -0.0927 0.1617 0.1579 0.028 Uiso 1 1 calc R U . . .
C7 C 0.2198(4) 0.04111(19) 0.27295(14) 0.0230(10) Uani 1 1 d . . . . .
C8 C 0.1556(5) 0.0444(2) 0.31724(15) 0.0368(12) Uani 1 1 d . . . . .
H8A H 0.1532 0.0857 0.3268 0.055 Uiso 1 1 calc R U . . .
H8B H 0.2127 0.0210 0.3375 0.055 Uiso 1 1 calc R U . . .
H8C H 0.0596 0.0285 0.3159 0.055 Uiso 1 1 calc R U . . .
C9 C 0.2254(5) -0.02406(19) 0.26002(16) 0.0317(12) Uani 1 1 d . . . . .
H9A H 0.1296 -0.0400 0.2580 0.048 Uiso 1 1 calc R U . . .
H9B H 0.2797 -0.0463 0.2816 0.048 Uiso 1 1 calc R U . . .
H9C H 0.2706 -0.0277 0.2322 0.048 Uiso 1 1 calc R U . . .
C10 C 0.3699(4) 0.0669(2) 0.27528(15) 0.0301(11) Uani 1 1 d . . . . .
H10A H 0.3658 0.1084 0.2842 0.045 Uiso 1 1 calc R U . . .
H10B H 0.4126 0.0642 0.2470 0.045 Uiso 1 1 calc R U . . .
H10C H 0.4267 0.0443 0.2961 0.045 Uiso 1 1 calc R U . . .
C11 C -0.1941(4) 0.17658(19) 0.23719(15) 0.0254(11) Uani 1 1 d . . . . .
C12 C -0.1450(5) 0.2156(2) 0.27463(17) 0.0422(14) Uani 1 1 d . . . . .
H12A H -0.1086 0.1905 0.2979 0.063 Uiso 1 1 calc R U . . .
H12B H -0.2244 0.2390 0.2848 0.063 Uiso 1 1 calc R U . . .
H12C H -0.0704 0.2422 0.2651 0.063 Uiso 1 1 calc R U . . .
C13 C -0.3051(4) 0.1331(2) 0.25322(17) 0.0380(13) Uani 1 1 d . . . . .
H13A H -0.3414 0.1094 0.2291 0.057 Uiso 1 1 calc R U . . .
H13B H -0.3827 0.1552 0.2659 0.057 Uiso 1 1 calc R U . . .
H13C H -0.2624 0.1068 0.2748 0.057 Uiso 1 1 calc R U . . .
C14 C -0.2594(5) 0.2162(2) 0.20279(17) 0.0387(13) Uani 1 1 d . . . . .
H14A H -0.2987 0.1917 0.1796 0.058 Uiso 1 1 calc R U . . .
H14B H -0.1870 0.2425 0.1914 0.058 Uiso 1 1 calc R U . . .
H14C H -0.3344 0.2401 0.2152 0.058 Uiso 1 1 calc R U . . .
C15 C 0.0815(4) 0.11303(18) 0.08619(14) 0.0207(10) Uani 1 1 d . . . . .
C16 C 0.1703(4) 0.08979(18) 0.05342(14) 0.0217(10) Uani 1 1 d . . . . .
C17 C 0.1398(4) 0.09767(18) 0.00932(14) 0.0206(10) Uani 1 1 d . . . . .
C18 C 0.0218(4) 0.13114(18) 0.00056(15) 0.0214(10) Uani 1 1 d . . . . .
H18A H -0.0008 0.1389 -0.0287 0.026 Uiso 1 1 calc R U . . .
C19 C -0.0694(4) 0.15516(18) 0.03206(15) 0.0215(10) Uani 1 1 d . . . . .
C20 C -0.0402(4) 0.14594(18) 0.07394(15) 0.0218(10) Uani 1 1 d . . . . .
H20A H -0.1007 0.1613 0.0951 0.026 Uiso 1 1 calc R U . . .
C21 C 0.2298(4) 0.06901(19) -0.02493(14) 0.0222(10) Uani 1 1 d . . . . .
C22 C 0.2170(5) 0.00170(19) -0.02124(16) 0.0354(12) Uani 1 1 d . . . . .
H22A H 0.1195 -0.0102 -0.0274 0.053 Uiso 1 1 calc R U . . .
H22B H 0.2439 -0.0107 0.0079 0.053 Uiso 1 1 calc R U . . .
H22C H 0.2793 -0.0172 -0.0418 0.053 Uiso 1 1 calc R U . . .
C23 C 0.1817(5) 0.0874(2) -0.06977(15) 0.0350(12) Uani 1 1 d . . . . .
H23A H 0.0841 0.0747 -0.0748 0.052 Uiso 1 1 calc R U . . .
H23B H 0.2424 0.0688 -0.0909 0.052 Uiso 1 1 calc R U . . .
H23C H 0.1876 0.1306 -0.0725 0.052 Uiso 1 1 calc R U . . .
C24 C 0.3844(4) 0.0873(2) -0.01906(15) 0.0287(11) Uani 1 1 d . . . . .
H24A H 0.3918 0.1306 -0.0203 0.043 Uiso 1 1 calc R U . . .
H24B H 0.4401 0.0698 -0.0419 0.043 Uiso 1 1 calc R U . . .
H24C H 0.4200 0.0733 0.0088 0.043 Uiso 1 1 calc R U . . .
C25 C -0.1983(4) 0.19072(18) 0.01656(15) 0.0234(10) Uani 1 1 d . . . . .
C26 C -0.2924(4) 0.2077(2) 0.05371(16) 0.0406(14) Uani 1 1 d . . . . .
H26A H -0.2389 0.2323 0.0742 0.061 Uiso 1 1 calc R U . . .
H26B H -0.3248 0.1718 0.0681 0.061 Uiso 1 1 calc R U . . .
H26C H -0.3738 0.2301 0.0427 0.061 Uiso 1 1 calc R U . . .
C27 C -0.2831(4) 0.1532(2) -0.01580(16) 0.0332(12) Uani 1 1 d . . . . .
H27A H -0.3162 0.1171 -0.0017 0.050 Uiso 1 1 calc R U . . .
H27B H -0.2231 0.1425 -0.0398 0.050 Uiso 1 1 calc R U . . .
H27C H -0.3642 0.1760 -0.0265 0.050 Uiso 1 1 calc R U . . .
C28 C -0.1491(4) 0.24759(19) -0.00510(16) 0.0314(12) Uani 1 1 d . . . . .
H28A H -0.0972 0.2720 0.0158 0.047 Uiso 1 1 calc R U . . .
H28B H -0.2310 0.2696 -0.0161 0.047 Uiso 1 1 calc R U . . .
H28C H -0.0875 0.2376 -0.0289 0.047 Uiso 1 1 calc R U . . .
V2 V 0.67175(8) -0.06939(4) 0.37751(3) 0.0326(2) Uani 1 1 d . . . . .
Cl4 Cl 0.46270(13) -0.02582(7) 0.37638(5) 0.0567(4) Uani 1 1 d . . . . .
Cl5 Cl 0.79391(13) 0.01956(6) 0.37283(5) 0.0476(4) Uani 1 1 d . . . . .
Cl6 Cl 0.57197(12) -0.16334(6) 0.38262(4) 0.0455(4) Uani 1 1 d . . . . .
N2 N 0.8666(3) -0.11631(16) 0.38009(12) 0.0262(9) Uani 1 1 d . . . . .
O3 O 0.7176(3) -0.07157(13) 0.43513(10) 0.0284(8) Uani 1 1 d . . . . .
O4 O 0.7125(3) -0.08303(14) 0.32069(10) 0.0325(8) Uani 1 1 d . . . . .
C29 C 0.9177(4) -0.12614(19) 0.42020(15) 0.0236(10) Uani 1 1 d . . . . .
C30 C 0.8299(4) -0.09710(19) 0.45118(15) 0.0234(10) Uani 1 1 d . . . . .
C31 C 0.8655(4) -0.09551(18) 0.49513(14) 0.0206(10) Uani 1 1 d . . . . .
C32 C 0.9835(4) -0.12734(18) 0.50658(15) 0.0233(10) Uani 1 1 d . . . . .
H32A H 1.0118 -0.1273 0.5359 0.028 Uiso 1 1 calc R U . . .
C33 C 1.0670(4) -0.16068(19) 0.47740(16) 0.0243(11) Uani 1 1 d . . . . .
C34 C 1.0353(4) -0.15893(19) 0.43489(16) 0.0267(11) Uani 1 1 d . . . . .
H34A H 1.0919 -0.1797 0.4151 0.032 Uiso 1 1 calc R U . . .
C35 C 0.7783(4) -0.06020(19) 0.52653(14) 0.0233(10) Uani 1 1 d . . . . .
C36 C 0.8431(5) -0.0622(2) 0.57147(15) 0.0374(13) Uani 1 1 d . . . . .
H36A H 0.8480 -0.1034 0.5813 0.056 Uiso 1 1 calc R U . . .
H36B H 0.7848 -0.0392 0.5910 0.056 Uiso 1 1 calc R U . . .
H36C H 0.9381 -0.0454 0.5711 0.056 Uiso 1 1 calc R U . . .
C37 C 0.6286(4) -0.0855(2) 0.52812(15) 0.0298(11) Uani 1 1 d . . . . .
H37A H 0.6328 -0.1272 0.5369 0.045 Uiso 1 1 calc R U . . .
H37B H 0.5837 -0.0826 0.4997 0.045 Uiso 1 1 calc R U . . .
H37C H 0.5737 -0.0630 0.5488 0.045 Uiso 1 1 calc R U . . .
C38 C 0.7717(5) 0.00488(19) 0.51254(16) 0.0325(12) Uani 1 1 d . . . . .
H38A H 0.7174 0.0276 0.5332 0.049 Uiso 1 1 calc R U . . .
H38B H 0.7262 0.0077 0.4842 0.049 Uiso 1 1 calc R U . . .
H38C H 0.8674 0.0209 0.5113 0.049 Uiso 1 1 calc R U . . .
C39 C 1.1907(4) -0.1971(2) 0.49581(16) 0.0299(12) Uani 1 1 d . . . . .
C40 C 1.1401(5) -0.2359(2) 0.53269(18) 0.0454(15) Uani 1 1 d . . . . .
H40A H 1.0664 -0.2628 0.5221 0.068 Uiso 1 1 calc R U . . .
H40B H 1.1023 -0.2107 0.5553 0.068 Uiso 1 1 calc R U . . .
H40C H 1.2194 -0.2590 0.5443 0.068 Uiso 1 1 calc R U . . .
C41 C 1.3028(5) -0.1542(2) 0.51343(19) 0.0430(15) Uani 1 1 d . . . . .
H41A H 1.3418 -0.1313 0.4898 0.065 Uiso 1 1 calc R U . . .
H41B H 1.3783 -0.1768 0.5277 0.065 Uiso 1 1 calc R U . . .
H41C H 1.2600 -0.1272 0.5340 0.065 Uiso 1 1 calc R U . . .
C42 C 1.2560(5) -0.2364(2) 0.46162(18) 0.0477(15) Uani 1 1 d . . . . .
H42A H 1.1841 -0.2632 0.4497 0.071 Uiso 1 1 calc R U . . .
H42B H 1.3327 -0.2598 0.4746 0.071 Uiso 1 1 calc R U . . .
H42C H 1.2932 -0.2116 0.4387 0.071 Uiso 1 1 calc R U . . .
C43 C 0.9163(4) -0.1324(2) 0.34172(15) 0.0261(11) Uani 1 1 d . . . . .
C44 C 0.8248(4) -0.11050(19) 0.30785(14) 0.0241(10) Uani 1 1 d . . . . .
C45 C 0.8567(4) -0.11792(18) 0.26412(14) 0.0205(10) Uani 1 1 d . . . . .
C46 C 0.9745(4) -0.15121(18) 0.25658(15) 0.0226(10) Uani 1 1 d . . . . .
H46A H 0.9975 -0.1586 0.2276 0.027 Uiso 1 1 calc R U . . .
C47 C 1.0651(4) -0.17567(19) 0.28913(15) 0.0248(11) Uani 1 1 d . . . . .
C48 C 1.0372(4) -0.16506(19) 0.33081(15) 0.0263(11) Uani 1 1 d . . . . .
H48A H 1.0989 -0.1796 0.3527 0.032 Uiso 1 1 calc R U . . .
C49 C 0.7663(4) -0.08865(19) 0.22906(14) 0.0245(11) Uani 1 1 d . . . . .
C50 C 0.6133(4) -0.1095(2) 0.23112(16) 0.0334(12) Uani 1 1 d . . . . .
H50A H 0.6097 -0.1527 0.2282 0.050 Uiso 1 1 calc R U . . .
H50B H 0.5582 -0.0912 0.2078 0.050 Uiso 1 1 calc R U . . .
H50C H 0.5740 -0.0980 0.2587 0.050 Uiso 1 1 calc R U . . .
C51 C 0.7710(5) -0.0215(2) 0.23520(18) 0.0413(14) Uani 1 1 d . . . . .
H51A H 0.8683 -0.0077 0.2328 0.062 Uiso 1 1 calc R U . . .
H51B H 0.7357 -0.0115 0.2636 0.062 Uiso 1 1 calc R U . . .
H51C H 0.7120 -0.0024 0.2131 0.062 Uiso 1 1 calc R U . . .
C52 C 0.8197(5) -0.1034(2) 0.18481(16) 0.0464(15) Uani 1 1 d . . . . .
H52A H 0.9167 -0.0892 0.1823 0.070 Uiso 1 1 calc R U . . .
H52B H 0.7599 -0.0840 0.1631 0.070 Uiso 1 1 calc R U . . .
H52C H 0.8171 -0.1463 0.1805 0.070 Uiso 1 1 calc R U . . .
C53 C 1.1928(4) -0.21221(19) 0.27522(15) 0.0272(11) Uani 1 1 d . . . . .
C54 C 1.2842(5) -0.2310(2) 0.31364(18) 0.0482(15) Uani 1 1 d . . . . .
H54A H 1.2281 -0.2549 0.3332 0.072 Uiso 1 1 calc R U . . .
H54B H 1.3193 -0.1957 0.3287 0.072 Uiso 1 1 calc R U . . .
H54C H 1.3640 -0.2545 0.3037 0.072 Uiso 1 1 calc R U . . .
C55 C 1.2820(5) -0.1764(2) 0.24432(19) 0.0474(16) Uani 1 1 d . . . . .
H55A H 1.2230 -0.1631 0.2201 0.071 Uiso 1 1 calc R U . . .
H55B H 1.3586 -0.2012 0.2338 0.071 Uiso 1 1 calc R U . . .
H55C H 1.3216 -0.1418 0.2593 0.071 Uiso 1 1 calc R U . . .
C56 C 1.1405(4) -0.26856(19) 0.25276(17) 0.0349(13) Uani 1 1 d . . . . .
H56A H 1.0798 -0.2578 0.2283 0.052 Uiso 1 1 calc R U . . .
H56B H 1.0871 -0.2926 0.2729 0.052 Uiso 1 1 calc R U . . .
H56C H 1.2213 -0.2913 0.2427 0.052 Uiso 1 1 calc R U . . .
C57 C 0.2342(8) -0.2281(3) 0.12957(19) 0.0628(18) Uani 1 1 d . . . . .
C58 C 0.2410(8) -0.2887(3) 0.1313(2) 0.072(2) Uani 1 1 d . . . . .
H58A H 0.3300 -0.3078 0.1333 0.086 Uiso 1 1 calc R U . . .
C59 C 0.1200(8) -0.3219(3) 0.13019(19) 0.067(2) Uani 1 1 d . . . . .
H59A H 0.1283 -0.3638 0.1310 0.080 Uiso 1 1 calc R U . . .
C60 C -0.0139(8) -0.2973(3) 0.12794(19) 0.070(2) Uani 1 1 d . . . . .
H60A H -0.0962 -0.3212 0.1277 0.084 Uiso 1 1 calc R U . . .
C61 C -0.0212(7) -0.2359(3) 0.12608(19) 0.0622(18) Uani 1 1 d . . . . .
H61A H -0.1105 -0.2170 0.1240 0.075 Uiso 1 1 calc R U . . .
C62 C 0.0999(8) -0.2017(3) 0.1272(2) 0.0668(19) Uani 1 1 d . . . . .
H62A H 0.0922 -0.1597 0.1264 0.080 Uiso 1 1 calc R U . . .
C63 C 0.3700(8) -0.1930(4) 0.1305(2) 0.101(3) Uani 1 1 d . . . . .
H63A H 0.4221 -0.2011 0.1572 0.151 Uiso 1 1 calc R U . . .
H63B H 0.3485 -0.1506 0.1287 0.151 Uiso 1 1 calc R U . . .
H63C H 0.4274 -0.2044 0.1061 0.151 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O1 1.844(3) . ?
V1 O2 1.849(3) . ?
V1 N1 2.133(3) . ?
V1 Cl1 2.2158(13) . ?
V1 Cl2 2.3212(15) . ?
V1 Cl3 2.3268(15) . ?
N1 C1 1.348(5) . ?
N1 C15 1.352(5) . ?
O1 C2 1.300(4) . ?
O2 C16 1.307(5) . ?
C1 C6 1.419(5) . ?
C1 C2 1.442(6) . ?
C2 C3 1.412(6) . ?
C3 C4 1.370(5) . ?
C3 C7 1.530(6) . ?
C4 C5 1.431(6) . ?
C5 C6 1.357(6) . ?
C5 C11 1.526(5) . ?
C7 C8 1.523(6) . ?
C7 C9 1.527(6) . ?
C7 C10 1.541(5) . ?
C11 C14 1.521(6) . ?
C11 C12 1.529(6) . ?
C11 C13 1.532(6) . ?
C15 C20 1.421(5) . ?
C15 C16 1.437(6) . ?
C16 C17 1.413(6) . ?
C17 C18 1.375(5) . ?
C17 C21 1.526(6) . ?
C18 C19 1.430(6) . ?
C19 C20 1.348(6) . ?
C19 C25 1.536(5) . ?
C21 C23 1.522(6) . ?
C21 C22 1.529(6) . ?
C21 C24 1.534(5) . ?
C25 C26 1.527(6) . ?
C25 C28 1.529(6) . ?
C25 C27 1.536(6) . ?
V2 O3 1.844(3) . ?
V2 O4 1.849(3) . ?
V2 N2 2.133(3) . ?
V2 Cl4 2.2163(14) . ?
V2 Cl5 2.3258(17) . ?
V2 Cl6 2.3303(17) . ?
N2 C43 1.346(6) . ?
N2 C29 1.353(5) . ?
O3 C30 1.305(5) . ?
O4 C44 1.304(5) . ?
C29 C34 1.409(6) . ?
C29 C30 1.447(6) . ?
C30 C31 1.408(6) . ?
C31 C32 1.374(5) . ?
C31 C35 1.521(6) . ?
C32 C33 1.433(6) . ?
C33 C34 1.356(6) . ?
C33 C39 1.536(6) . ?
C35 C36 1.522(6) . ?
C35 C38 1.534(6) . ?
C35 C37 1.535(5) . ?
C39 C42 1.530(7) . ?
C39 C40 1.532(6) . ?
C39 C41 1.534(6) . ?
C43 C48 1.412(6) . ?
C43 C44 1.444(6) . ?
C44 C45 1.414(6) . ?
C45 C46 1.372(5) . ?
C45 C49 1.529(6) . ?
C46 C47 1.431(6) . ?
C47 C48 1.354(6) . ?
C47 C53 1.536(6) . ?
C49 C52 1.518(6) . ?
C49 C51 1.528(6) . ?
C49 C50 1.530(5) . ?
C53 C54 1.528(6) . ?
C53 C55 1.528(6) . ?
C53 C56 1.531(6) . ?
C57 C58 1.371(8) . ?
C57 C62 1.409(8) . ?
C57 C63 1.515(9) . ?
C58 C59 1.373(9) . ?
C59 C60 1.389(8) . ?
C60 C61 1.391(8) . ?
C61 C62 1.385(8) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 V1 O2 152.02(12) . . ?
O1 V1 N1 76.01(13) . . ?
O2 V1 N1 76.10(13) . . ?
O1 V1 Cl1 102.41(9) . . ?
O2 V1 Cl1 105.51(9) . . ?
N1 V1 Cl1 178.15(12) . . ?
O1 V1 Cl2 90.24(10) . . ?
O2 V1 Cl2 89.93(10) . . ?
N1 V1 Cl2 85.87(10) . . ?
Cl1 V1 Cl2 93.20(6) . . ?
O1 V1 Cl3 88.28(10) . . ?
O2 V1 Cl3 88.19(10) . . ?
N1 V1 Cl3 87.17(10) . . ?
Cl1 V1 Cl3 93.76(6) . . ?
Cl2 V1 Cl3 173.04(5) . . ?
C1 N1 C15 130.9(3) . . ?
C1 N1 V1 114.6(3) . . ?
C15 N1 V1 114.5(3) . . ?
C2 O1 V1 124.1(3) . . ?
C16 O2 V1 123.9(3) . . ?
N1 C1 C6 131.0(4) . . ?
N1 C1 C2 110.0(3) . . ?
C6 C1 C2 119.0(4) . . ?
O1 C2 C3 122.8(4) . . ?
O1 C2 C1 115.2(4) . . ?
C3 C2 C1 122.0(4) . . ?
C4 C3 C2 115.0(4) . . ?
C4 C3 C7 123.9(4) . . ?
C2 C3 C7 121.2(4) . . ?
C3 C4 C5 125.0(4) . . ?
C6 C5 C4 119.2(4) . . ?
C6 C5 C11 122.5(4) . . ?
C4 C5 C11 118.3(4) . . ?
C5 C6 C1 119.5(4) . . ?
C8 C7 C9 107.6(4) . . ?
C8 C7 C3 111.0(3) . . ?
C9 C7 C3 110.3(4) . . ?
C8 C7 C10 109.0(4) . . ?
C9 C7 C10 109.8(3) . . ?
C3 C7 C10 109.1(3) . . ?
C14 C11 C5 111.7(4) . . ?
C14 C11 C12 108.4(4) . . ?
C5 C11 C12 109.6(3) . . ?
C14 C11 C13 109.5(4) . . ?
C5 C11 C13 108.8(4) . . ?
C12 C11 C13 108.8(4) . . ?
N1 C15 C20 130.8(4) . . ?
N1 C15 C16 110.2(3) . . ?
C20 C15 C16 119.0(4) . . ?
O2 C16 C17 122.3(4) . . ?
O2 C16 C15 115.3(4) . . ?
C17 C16 C15 122.4(4) . . ?
C18 C17 C16 114.5(4) . . ?
C18 C17 C21 124.0(4) . . ?
C16 C17 C21 121.5(4) . . ?
C17 C18 C19 125.0(4) . . ?
C20 C19 C18 119.5(4) . . ?
C20 C19 C25 122.3(4) . . ?
C18 C19 C25 118.2(4) . . ?
C19 C20 C15 119.5(4) . . ?
C23 C21 C17 111.5(3) . . ?
C23 C21 C22 108.5(4) . . ?
C17 C21 C22 108.8(4) . . ?
C23 C21 C24 107.8(4) . . ?
C17 C21 C24 110.5(3) . . ?
C22 C21 C24 109.7(3) . . ?
C26 C25 C28 108.3(4) . . ?
C26 C25 C19 111.6(4) . . ?
C28 C25 C19 109.2(3) . . ?
C26 C25 C27 109.4(4) . . ?
C28 C25 C27 109.5(4) . . ?
C19 C25 C27 108.9(3) . . ?
O3 V2 O4 151.88(12) . . ?
O3 V2 N2 76.17(13) . . ?
O4 V2 N2 75.88(13) . . ?
O3 V2 Cl4 102.86(10) . . ?
O4 V2 Cl4 105.23(10) . . ?
N2 V2 Cl4 176.33(12) . . ?
O3 V2 Cl5 88.59(11) . . ?
O4 V2 Cl5 88.26(11) . . ?
N2 V2 Cl5 89.86(11) . . ?
Cl4 V2 Cl5 93.66(6) . . ?
O3 V2 Cl6 89.88(11) . . ?
O4 V2 Cl6 90.40(11) . . ?
N2 V2 Cl6 84.21(11) . . ?
Cl4 V2 Cl6 92.27(6) . . ?
Cl5 V2 Cl6 174.07(6) . . ?
C43 N2 C29 130.8(4) . . ?
C43 N2 V2 114.8(3) . . ?
C29 N2 V2 114.4(3) . . ?
C30 O3 V2 124.3(3) . . ?
C44 O4 V2 124.2(3) . . ?
N2 C29 C34 131.0(4) . . ?
N2 C29 C30 110.0(4) . . ?
C34 C29 C30 119.0(4) . . ?
O3 C30 C31 122.9(4) . . ?
O3 C30 C29 114.9(4) . . ?
C31 C30 C29 122.1(4) . . ?
C32 C31 C30 114.9(4) . . ?
C32 C31 C35 124.0(4) . . ?
C30 C31 C35 121.2(4) . . ?
C31 C32 C33 124.6(4) . . ?
C34 C33 C32 119.5(4) . . ?
C34 C33 C39 122.4(4) . . ?
C32 C33 C39 118.1(4) . . ?
C33 C34 C29 119.6(4) . . ?
C31 C35 C36 111.2(4) . . ?
C31 C35 C38 109.8(4) . . ?
C36 C35 C38 107.8(4) . . ?
C31 C35 C37 110.0(3) . . ?
C36 C35 C37 108.5(4) . . ?
C38 C35 C37 109.5(3) . . ?
C42 C39 C40 109.2(4) . . ?
C42 C39 C41 109.2(4) . . ?
C40 C39 C41 108.5(4) . . ?
C42 C39 C33 111.6(4) . . ?
C40 C39 C33 109.8(4) . . ?
C41 C39 C33 108.6(4) . . ?
N2 C43 C48 131.0(4) . . ?
N2 C43 C44 110.0(4) . . ?
C48 C43 C44 118.9(4) . . ?
O4 C44 C45 123.0(4) . . ?
O4 C44 C43 115.0(4) . . ?
C45 C44 C43 122.0(4) . . ?
C46 C45 C44 114.9(4) . . ?
C46 C45 C49 124.3(4) . . ?
C44 C45 C49 120.8(4) . . ?
C45 C46 C47 124.8(4) . . ?
C48 C47 C46 119.2(4) . . ?
C48 C47 C53 122.4(4) . . ?
C46 C47 C53 118.3(4) . . ?
C47 C48 C43 119.9(4) . . ?
C52 C49 C51 108.8(4) . . ?
C52 C49 C45 111.3(3) . . ?
C51 C49 C45 108.9(4) . . ?
C52 C49 C50 107.8(4) . . ?
C51 C49 C50 109.0(3) . . ?
C45 C49 C50 111.0(4) . . ?
C54 C53 C55 109.2(4) . . ?
C54 C53 C56 107.6(4) . . ?
C55 C53 C56 109.3(4) . . ?
C54 C53 C47 111.6(4) . . ?
C55 C53 C47 110.1(4) . . ?
C56 C53 C47 109.0(3) . . ?
C58 C57 C62 117.8(7) . . ?
C58 C57 C63 118.8(7) . . ?
C62 C57 C63 123.4(7) . . ?
C57 C58 C59 120.4(7) . . ?
C58 C59 C60 123.2(7) . . ?
C59 C60 C61 116.5(7) . . ?
C62 C61 C60 120.9(6) . . ?
C61 C62 C57 121.1(6) . . ?

_refine_diff_density_max         0.626
_refine_diff_density_min         -0.532
_refine_diff_density_rms         0.084

_shelxl_version_number           2012-9


_database_code_depnum_ccdc_archive 'CCDC 1015035'
#######################################################################
#
#                 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_afh301

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H40 Cl3 N Nb O2'
_chemical_formula_weight         621.87

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_H-M_alt        'F d d 2'
_space_group_name_Hall           'F 2 -2d'

_shelx_space_group_comment       
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;

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

_cell_length_a                   18.7255(12)
_cell_length_b                   27.2787(17)
_cell_length_c                   11.9550(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6106.7(7)
_cell_formula_units_Z            8
_cell_measurement_temperature    143(2)
_cell_measurement_reflns_used    7259
_cell_measurement_theta_min      2.64
_cell_measurement_theta_max      28.36

_exptl_crystal_description       prism
_exptl_crystal_colour            green
_exptl_crystal_density_meas      not_measured
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_F_000             2584
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.255
_exptl_crystal_size_mid          0.147
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    0.681
_shelx_estimated_absorpt_T_min   0.846
_shelx_estimated_absorpt_T_max   0.923
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.8904
_exptl_absorpt_correction_T_max  0.9809
_exptl_absorpt_process_details   'Bruker SADABS'

_exptl_special_details           
; 
 A green crystal of approximate dimensions 0.25 x 0.15 x 0.12 mm
 was mounted on a glass fiber and transferred to a Bruker SMART
 APEX II diffractometer.  The APEX2 program package was used to
 determine the unit-cell parameters and for data collection 
 (30 sec/frame scan time for a hemisphere of diffraction data).
 The raw frame data was processed using SAINT and SADABS to yield
 the reflection data file.  Subsequent calculations were carried out
 using the SHELXTL program.  The diffraction symmetry was mmm and
 the systematic absences were consistent with the orthorhombic space
 group Fdd2 that was later determined to be correct.
 
 APEX2 Version 2011.4-1, Bruker AXS, Inc.; Madison, WI 2011.
 SAINT  Version 7.68a, Bruker AXS, Inc.; Madison, WI  2007.
 Sheldrick, G. M. SADABS, Version 2008/1, Bruker AXS, Inc.; Madison, WI  2008. 
 Sheldrick, G. M. SHELXTL, Version 2014/2, Bruker AXS, Inc.; Madison, WI  2014
 Parsons, S., Flack, H. D., Wagner, T.,  Acta Cryst. B69, 2013, 249-259).
;

_diffrn_ambient_temperature      143(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            13033
_diffrn_reflns_av_unetI/netI     0.0225
_diffrn_reflns_av_R_equivalents  0.0213
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.155
_diffrn_reflns_theta_max         28.545
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.922
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             3580
_reflns_number_gt                3406
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.861
_reflns_Friedel_fraction_max     0.895
_reflns_Friedel_fraction_full    0.999

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences.  The structure wassolved by direct methods
 and refined on F2 by full-matrix least-squarestechniques.  The
 analytical scattering factors for neutral atoms were
 used throughout the analysis.  Hydrogen atoms were included using a
 riding model. The molecule was located on a two-fold rotatgion axis.
 At convergence, wR2 = 0.0473 and Goof = 1.078 for 166
 variables refined against 3580 data (0.70 Å), R1 = 0.0198 for those
 3406 data with I > 2.0s(I). The absolulte structure was assigned by 
 refinement of the Flack Parameter
;

_computing_data_collection       'Bruker APEX2 2011.4-1, 2011'
_computing_cell_refinement       'Bruker SAINT 7.68a, 2009'
_computing_data_reduction        'Bruker SAINT 7.68a, 2009'
_computing_structure_solution    'Bruker SHELXTL 2008/4'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 ? 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0230P)²+3.2131P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 
; 
 Flack x determined using 1524 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.005(12)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         3580
_refine_ls_number_parameters     166
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0220
_refine_ls_R_factor_gt           0.0198
_refine_ls_wR_factor_ref         0.0473
_refine_ls_wR_factor_gt          0.0464
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_restrained_S_all      1.078
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Nb1 Nb 0.0000 0.5000 1.24428(2) 0.01578(7) Uani 1 2 d S T P . .
Cl1 Cl 0.0000 0.5000 1.43874(9) 0.0312(3) Uani 1 2 d S T P . .
Cl2 Cl 0.12675(3) 0.49368(2) 1.23786(7) 0.02662(13) Uani 1 1 d . . . . .
O1 O -0.00885(9) 0.43337(6) 1.19856(13) 0.0175(3) Uani 1 1 d . . . . .
N1 N 0.0000 0.5000 1.0592(3) 0.0146(7) Uani 1 2 d S T P . .
C1 C -0.01564(11) 0.45571(8) 1.01121(19) 0.0147(4) Uani 1 1 d . . . . .
C2 C -0.02083(12) 0.41826(8) 1.09357(19) 0.0149(4) Uani 1 1 d . . . . .
C3 C -0.03650(12) 0.36925(8) 1.06742(19) 0.0158(5) Uani 1 1 d . . . . .
C4 C -0.04658(12) 0.35984(8) 0.9546(2) 0.0174(5) Uani 1 1 d . . . . .
H4A H -0.0570 0.3271 0.9331 0.021 Uiso 1 1 calc R U . . .
C5 C -0.04238(12) 0.39569(9) 0.86930(19) 0.0166(4) Uani 1 1 d . . . . .
C6 C -0.02784(12) 0.44357(8) 0.89805(18) 0.0156(4) Uani 1 1 d . . . . .
H6A H -0.0260 0.4682 0.8421 0.019 Uiso 1 1 calc R U . . .
C7 C -0.04362(13) 0.33056(8) 1.1594(2) 0.0181(5) Uani 1 1 d . . . . .
C8 C -0.06959(15) 0.28144(8) 1.1110(2) 0.0258(5) Uani 1 1 d . . . . .
H8A H -0.0340 0.2688 1.0582 0.039 Uiso 1 1 calc R U . . .
H8B H -0.1151 0.2864 1.0720 0.039 Uiso 1 1 calc R U . . .
H8C H -0.0762 0.2578 1.1719 0.039 Uiso 1 1 calc R U . . .
C9 C 0.02921(13) 0.32221(9) 1.2153(2) 0.0239(5) Uani 1 1 d . . . . .
H9A H 0.0470 0.3533 1.2456 0.036 Uiso 1 1 calc R U . . .
H9B H 0.0631 0.3096 1.1599 0.036 Uiso 1 1 calc R U . . .
H9C H 0.0240 0.2984 1.2762 0.036 Uiso 1 1 calc R U . . .
C10 C -0.09852(13) 0.34778(9) 1.2469(3) 0.0244(5) Uani 1 1 d . . . . .
H10A H -0.0800 0.3767 1.2860 0.037 Uiso 1 1 calc R U . . .
H10B H -0.1071 0.3214 1.3010 0.037 Uiso 1 1 calc R U . . .
H10C H -0.1434 0.3562 1.2094 0.037 Uiso 1 1 calc R U . . .
C11 C -0.05366(12) 0.37943(8) 0.7476(2) 0.0196(4) Uani 1 1 d . . . . .
C12 C -0.04630(16) 0.42200(9) 0.6651(2) 0.0273(6) Uani 1 1 d . . . . .
H12A H 0.0013 0.4366 0.6725 0.041 Uiso 1 1 calc R U . . .
H12B H -0.0827 0.4468 0.6814 0.041 Uiso 1 1 calc R U . . .
H12C H -0.0527 0.4098 0.5886 0.041 Uiso 1 1 calc R U . . .
C13 C -0.12841(14) 0.35717(10) 0.7341(3) 0.0316(6) Uani 1 1 d . . . . .
H13A H -0.1348 0.3461 0.6568 0.047 Uiso 1 1 calc R U . . .
H13B H -0.1645 0.3820 0.7518 0.047 Uiso 1 1 calc R U . . .
H13C H -0.1336 0.3292 0.7850 0.047 Uiso 1 1 calc R U . . .
C14 C 0.00256(15) 0.34026(10) 0.7189(2) 0.0296(7) Uani 1 1 d . . . . .
H14A H 0.0504 0.3546 0.7248 0.044 Uiso 1 1 calc R U . . .
H14B H -0.0052 0.3285 0.6424 0.044 Uiso 1 1 calc R U . . .
H14C H -0.0017 0.3128 0.7713 0.044 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Nb1 O1 1.9051(16) 2_565 ?
Nb1 O1 1.9051(16) . ?
Nb1 N1 2.213(3) . ?
Nb1 Cl1 2.3247(11) . ?
Nb1 Cl2 2.3810(6) . ?
Nb1 Cl2 2.3810(6) 2_565 ?
O1 C2 1.340(3) . ?
N1 C1 1.369(3) . ?
N1 C1 1.369(3) 2_565 ?
C1 C6 1.411(3) . ?
C1 C2 1.422(3) . ?
C2 C3 1.404(3) . ?
C3 C4 1.386(3) . ?
C3 C7 1.530(3) . ?
C4 C5 1.415(3) . ?
C5 C6 1.378(3) . ?
C5 C11 1.536(3) . ?
C7 C9 1.536(3) . ?
C7 C8 1.538(3) . ?
C7 C10 1.539(3) . ?
C11 C12 1.529(3) . ?
C11 C13 1.534(3) . ?
C11 C14 1.539(3) . ?

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
O1 Nb1 O1 146.66(10) 2_565 . ?
O1 Nb1 N1 73.33(5) 2_565 . ?
O1 Nb1 N1 73.33(5) . . ?
O1 Nb1 Cl1 106.67(5) 2_565 . ?
O1 Nb1 Cl1 106.67(5) . . ?
N1 Nb1 Cl1 180.0 . . ?
O1 Nb1 Cl2 88.46(5) 2_565 . ?
O1 Nb1 Cl2 90.48(5) . . ?
N1 Nb1 Cl2 88.15(2) . . ?
Cl1 Nb1 Cl2 91.85(2) . . ?
O1 Nb1 Cl2 90.48(5) 2_565 2_565 ?
O1 Nb1 Cl2 88.46(5) . 2_565 ?
N1 Nb1 Cl2 88.15(2) . 2_565 ?
Cl1 Nb1 Cl2 91.85(2) . 2_565 ?
Cl2 Nb1 Cl2 176.31(4) . 2_565 ?
C2 O1 Nb1 125.22(14) . . ?
C1 N1 C1 130.5(3) . 2_565 ?
C1 N1 Nb1 114.77(16) . . ?
C1 N1 Nb1 114.77(16) 2_565 . ?
N1 C1 C6 130.0(2) . . ?
N1 C1 C2 111.0(2) . . ?
C6 C1 C2 118.9(2) . . ?
O1 C2 C3 122.4(2) . . ?
O1 C2 C1 114.59(19) . . ?
C3 C2 C1 123.0(2) . . ?
C4 C3 C2 114.9(2) . . ?
C4 C3 C7 124.1(2) . . ?
C2 C3 C7 121.0(2) . . ?
C3 C4 C5 124.5(2) . . ?
C6 C5 C4 119.1(2) . . ?
C6 C5 C11 122.5(2) . . ?
C4 C5 C11 118.4(2) . . ?
C5 C6 C1 119.6(2) . . ?
C3 C7 C9 109.73(19) . . ?
C3 C7 C8 111.0(2) . . ?
C9 C7 C8 108.4(2) . . ?
C3 C7 C10 109.63(19) . . ?
C9 C7 C10 110.1(2) . . ?
C8 C7 C10 108.1(2) . . ?
C12 C11 C13 108.4(2) . . ?
C12 C11 C5 112.27(19) . . ?
C13 C11 C5 109.8(2) . . ?
C12 C11 C14 108.8(2) . . ?
C13 C11 C14 109.0(2) . . ?
C5 C11 C14 108.49(19) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 N1 C1 C6 -7.7(2) 2_565 . . . ?
Nb1 N1 C1 C6 172.3(2) . . . . ?
C1 N1 C1 C2 173.69(19) 2_565 . . . ?
Nb1 N1 C1 C2 -6.32(19) . . . . ?
Nb1 O1 C2 C3 -171.09(17) . . . . ?
Nb1 O1 C2 C1 9.5(3) . . . . ?
N1 C1 C2 O1 -0.7(3) . . . . ?
C6 C1 C2 O1 -179.56(19) . . . . ?
N1 C1 C2 C3 179.89(19) . . . . ?
C6 C1 C2 C3 1.1(3) . . . . ?
O1 C2 C3 C4 -179.3(2) . . . . ?
C1 C2 C3 C4 0.0(3) . . . . ?
O1 C2 C3 C7 2.5(3) . . . . ?
C1 C2 C3 C7 -178.2(2) . . . . ?
C2 C3 C4 C5 -0.4(4) . . . . ?
C7 C3 C4 C5 177.9(2) . . . . ?
C3 C4 C5 C6 -0.5(4) . . . . ?
C3 C4 C5 C11 179.0(2) . . . . ?
C4 C5 C6 C1 1.6(3) . . . . ?
C11 C5 C6 C1 -177.8(2) . . . . ?
N1 C1 C6 C5 179.5(2) . . . . ?
C2 C1 C6 C5 -1.9(3) . . . . ?
C4 C3 C7 C9 114.9(3) . . . . ?
C2 C3 C7 C9 -67.0(3) . . . . ?
C4 C3 C7 C8 -4.9(3) . . . . ?
C2 C3 C7 C8 173.2(2) . . . . ?
C4 C3 C7 C10 -124.2(3) . . . . ?
C2 C3 C7 C10 54.0(3) . . . . ?
C6 C5 C11 C12 0.4(3) . . . . ?
C4 C5 C11 C12 -179.1(2) . . . . ?
C6 C5 C11 C13 -120.2(2) . . . . ?
C4 C5 C11 C13 60.3(3) . . . . ?
C6 C5 C11 C14 120.7(2) . . . . ?
C4 C5 C11 C14 -58.8(3) . . . . ?

_refine_diff_density_max         0.246
_refine_diff_density_min         -0.333
_refine_diff_density_rms         0.044

_shelxl_version_number           2014-2



#==END


_database_code_depnum_ccdc_archive 'CCDC 1015036'
