# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2013


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#                                CCDC 
# 
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# 
#  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 
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data_ms120203
_database_code_depnum_ccdc_archive 'CCDC 891100'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C35 H47 Cl3 N3 V, C2 H3 N'
_chemical_formula_sum            'C37 H50 Cl3 N4 V'
_exptl_crystal_recrystallization_method MeCN
_chemical_melting_point          ?
_exptl_crystal_description       plate
_exptl_crystal_colour            black
_diffrn_ambient_temperature      173(1)
_chemical_formula_weight         708.10
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'
Cl Cl 0.1484 0.1585 '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'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_int_tables_number      14
_chemical_absolute_configuration ?
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_cell_length_a                   17.658(9)
_cell_length_b                   13.195(6)
_cell_length_c                   16.613(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 104.052(7)
_cell_angle_gamma                90.00
_cell_volume                     3755(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(1)
_cell_measurement_reflns_used    6748
_cell_measurement_theta_min      2.47
_cell_measurement_theta_max      26.54
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.253
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1496
_exptl_absorpt_coefficient_mu    0.508
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7853
_exptl_absorpt_correction_T_max  0.9750
_exptl_absorpt_process_details   'TWINABS (Sheldrick, 2004)'
_exptl_special_details           
;
Crystal decay was monitored by repeating the initial 50 frames
at the end of the data collection and analyzing duplicate
reflections
;
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              K760
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker AXS SMART1000/P4'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            15624
_diffrn_reflns_av_R_equivalents  0.0683
_diffrn_reflns_av_sigmaI/netI    0.1201
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.19
_diffrn_reflns_theta_max         27.50
_reflns_number_total             8380
_reflns_number_gt                4720
_reflns_threshold_expression     'I > 2\s(I)'
_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'Bruker SHELXTL (Sheldrick, 2008)'
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0577P)^2^] where P=(Fo^2^+2Fc^2^)/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         8380
_refine_ls_number_parameters     417
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1070
_refine_ls_R_factor_gt           0.0495
_refine_ls_wR_factor_ref         0.1210
_refine_ls_wR_factor_gt          0.1072
_refine_ls_goodness_of_fit_ref   0.945
_refine_ls_restrained_S_all      0.945
_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 0.22284(2) 0.37239(3) 0.13157(3) 0.02261(12) Uani 1 1 d . . .
Cl3 Cl 0.32171(4) 0.25967(6) 0.13405(5) 0.0457(2) Uani 1 1 d . . .
Cl1 Cl 0.20801(4) 0.33664(6) 0.26187(4) 0.0408(2) Uani 1 1 d . . .
Cl2 Cl 0.12508(4) 0.49549(5) 0.10226(4) 0.03008(17) Uani 1 1 d . . .
N1 N 0.31413(11) 0.49083(15) 0.14899(12) 0.0232(5) Uani 1 1 d . . .
N2 N 0.22955(12) 0.40915(15) 0.01281(12) 0.0232(5) Uani 1 1 d . . .
N3 N 0.14115(11) 0.26884(15) 0.05146(12) 0.0217(5) Uani 1 1 d . . .
C8 C 0.36228(15) 0.52474(19) 0.22924(16) 0.0273(6) Uani 1 1 d . . .
C9 C 0.43718(15) 0.4818(2) 0.25997(17) 0.0336(7) Uani 1 1 d . . .
C10 C 0.47847(17) 0.5106(2) 0.33981(19) 0.0431(8) Uani 1 1 d . . .
H10 H 0.5289 0.4830 0.3620 0.052 Uiso 1 1 calc R . .
C11 C 0.44821(19) 0.5774(3) 0.3868(2) 0.0513(9) Uani 1 1 d . . .
H11 H 0.4767 0.5944 0.4413 0.062 Uiso 1 1 calc R . .
C12 C 0.37566(18) 0.6198(2) 0.35384(18) 0.0427(8) Uani 1 1 d . . .
H12 H 0.3553 0.6672 0.3862 0.051 Uiso 1 1 calc R . .
C13 C 0.33147(15) 0.59520(19) 0.27490(16) 0.0294(6) Uani 1 1 d . . .
C14 C 0.47610(16) 0.4094(2) 0.21162(19) 0.0404(7) Uani 1 1 d . . .
H14 H 0.4377 0.3921 0.1585 0.048 Uiso 1 1 calc R . .
C15 C 0.5002(2) 0.3111(3) 0.2600(2) 0.0574(10) Uani 1 1 d . . .
H15A H 0.5436 0.3249 0.3081 0.086 Uiso 1 1 calc R . .
H15B H 0.5167 0.2613 0.2239 0.086 Uiso 1 1 calc R . .
H15C H 0.4558 0.2843 0.2790 0.086 Uiso 1 1 calc R . .
C16 C 0.54764(17) 0.4579(3) 0.1904(2) 0.0610(10) Uani 1 1 d . . .
H16A H 0.5324 0.5217 0.1608 0.092 Uiso 1 1 calc R . .
H16B H 0.5689 0.4116 0.1552 0.092 Uiso 1 1 calc R . .
H16C H 0.5875 0.4712 0.2417 0.092 Uiso 1 1 calc R . .
C17 C 0.25377(16) 0.64859(19) 0.24112(17) 0.0305(6) Uani 1 1 d . . .
H17 H 0.2330 0.6262 0.1824 0.037 Uiso 1 1 calc R . .
C19 C 0.19355(17) 0.6211(2) 0.28972(18) 0.0398(7) Uani 1 1 d . . .
H19A H 0.1886 0.5472 0.2916 0.060 Uiso 1 1 calc R . .
H19B H 0.1430 0.6507 0.2624 0.060 Uiso 1 1 calc R . .
H19C H 0.2105 0.6476 0.3463 0.060 Uiso 1 1 calc R . .
C18 C 0.2638(2) 0.7635(2) 0.2410(2) 0.0495(9) Uani 1 1 d . . .
H18A H 0.2819 0.7877 0.2982 0.074 Uiso 1 1 calc R . .
H18B H 0.2137 0.7953 0.2150 0.074 Uiso 1 1 calc R . .
H18C H 0.3024 0.7812 0.2097 0.074 Uiso 1 1 calc R . .
C1 C 0.32606(14) 0.52677(19) 0.08160(16) 0.0277(6) Uani 1 1 d . . .
C20 C 0.38045(17) 0.6120(2) 0.07545(18) 0.0437(8) Uani 1 1 d . . .
H20A H 0.4137 0.5920 0.0379 0.052 Uiso 1 1 calc R . .
H20B H 0.4150 0.6255 0.1309 0.052 Uiso 1 1 calc R . .
C21 C 0.3357(2) 0.7083(2) 0.0427(2) 0.0594(10) Uani 1 1 d . . .
H21A H 0.3012 0.6949 -0.0121 0.089 Uiso 1 1 calc R . .
H21B H 0.3727 0.7620 0.0380 0.089 Uiso 1 1 calc R . .
H21C H 0.3045 0.7298 0.0810 0.089 Uiso 1 1 calc R . .
C2 C 0.27957(15) 0.48062(19) 0.00281(16) 0.0276(6) Uani 1 1 d . . .
C3 C 0.28622(18) 0.5051(2) -0.07655(17) 0.0378(7) Uani 1 1 d . . .
H3 H 0.3228 0.5544 -0.0847 0.045 Uiso 1 1 calc R . .
C4 C 0.23828(18) 0.4558(2) -0.14372(17) 0.0398(7) Uani 1 1 d . . .
H4 H 0.2419 0.4720 -0.1984 0.048 Uiso 1 1 calc R . .
C5 C 0.18566(16) 0.3840(2) -0.13220(16) 0.0328(7) Uani 1 1 d . . .
H5 H 0.1524 0.3508 -0.1782 0.039 Uiso 1 1 calc R . .
C6 C 0.18227(14) 0.36127(18) -0.05181(15) 0.0235(6) Uani 1 1 d . . .
C7 C 0.13169(14) 0.28255(18) -0.02736(15) 0.0229(6) Uani 1 1 d . . .
C22 C 0.07238(15) 0.2287(2) -0.09393(15) 0.0286(6) Uani 1 1 d . . .
H22A H 0.0521 0.1691 -0.0696 0.034 Uiso 1 1 calc R . .
H22B H 0.0978 0.2041 -0.1372 0.034 Uiso 1 1 calc R . .
C23 C 0.00376(17) 0.2990(2) -0.13404(17) 0.0430(8) Uani 1 1 d . . .
H23A H -0.0158 0.3326 -0.0905 0.064 Uiso 1 1 calc R . .
H23B H -0.0382 0.2589 -0.1692 0.064 Uiso 1 1 calc R . .
H23C H 0.0217 0.3502 -0.1679 0.064 Uiso 1 1 calc R . .
C24 C 0.10133(14) 0.18706(18) 0.08221(14) 0.0231(6) Uani 1 1 d . . .
C25 C 0.03136(15) 0.20569(19) 0.10603(15) 0.0249(6) Uani 1 1 d . . .
C26 C 0.00034(16) 0.1273(2) 0.14362(16) 0.0306(6) Uani 1 1 d . . .
H26 H -0.0460 0.1386 0.1617 0.037 Uiso 1 1 calc R . .
C27 C 0.03574(16) 0.0328(2) 0.15529(17) 0.0355(7) Uani 1 1 d . . .
H27 H 0.0143 -0.0196 0.1822 0.043 Uiso 1 1 calc R . .
C28 C 0.10176(17) 0.0153(2) 0.12791(17) 0.0345(7) Uani 1 1 d . . .
H28 H 0.1245 -0.0504 0.1347 0.041 Uiso 1 1 calc R . .
C29 C 0.13661(15) 0.09068(19) 0.09045(15) 0.0274(6) Uani 1 1 d . . .
C30 C -0.01346(15) 0.3043(2) 0.08859(16) 0.0288(6) Uani 1 1 d . . .
H30 H 0.0140 0.3489 0.0561 0.035 Uiso 1 1 calc R . .
C31 C -0.01645(18) 0.3604(2) 0.16888(18) 0.0394(7) Uani 1 1 d . . .
H31A H -0.0475 0.3211 0.1993 0.059 Uiso 1 1 calc R . .
H31B H -0.0404 0.4272 0.1550 0.059 Uiso 1 1 calc R . .
H31C H 0.0367 0.3688 0.2035 0.059 Uiso 1 1 calc R . .
C32 C -0.09761(16) 0.2863(2) 0.03581(19) 0.0443(8) Uani 1 1 d . . .
H32A H -0.0957 0.2484 -0.0144 0.066 Uiso 1 1 calc R . .
H32B H -0.1233 0.3516 0.0202 0.066 Uiso 1 1 calc R . .
H32C H -0.1270 0.2473 0.0682 0.066 Uiso 1 1 calc R . .
C33 C 0.20727(15) 0.06480(19) 0.05748(16) 0.0293(6) Uani 1 1 d . . .
H33 H 0.2277 0.1295 0.0395 0.035 Uiso 1 1 calc R . .
C34 C 0.1847(2) -0.0044(2) -0.0187(2) 0.0517(9) Uani 1 1 d . . .
H34A H 0.1664 -0.0697 -0.0024 0.078 Uiso 1 1 calc R . .
H34B H 0.2303 -0.0153 -0.0415 0.078 Uiso 1 1 calc R . .
H34C H 0.1429 0.0275 -0.0608 0.078 Uiso 1 1 calc R . .
C35 C 0.27352(17) 0.0161(2) 0.12402(19) 0.0453(8) Uani 1 1 d . . .
H35A H 0.2871 0.0606 0.1726 0.068 Uiso 1 1 calc R . .
H35B H 0.3194 0.0065 0.1014 0.068 Uiso 1 1 calc R . .
H35C H 0.2562 -0.0496 0.1403 0.068 Uiso 1 1 calc R . .
N4 N 0.4616(3) 0.1633(4) 0.4912(3) 0.1289(19) Uani 1 1 d . . .
C36 C 0.4213(3) 0.2284(4) 0.4684(3) 0.0685(11) Uani 1 1 d . . .
C37 C 0.3686(2) 0.3099(4) 0.4386(3) 0.0904(15) Uani 1 1 d . . .
H37A H 0.3285 0.2872 0.3903 0.136 Uiso 1 1 calc R . .
H37B H 0.3975 0.3668 0.4227 0.136 Uiso 1 1 calc R . .
H37C H 0.3438 0.3316 0.4825 0.136 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
V1 0.0246(2) 0.0239(2) 0.0193(2) 0.00317(18) 0.00513(18) -0.00279(19)
Cl3 0.0333(4) 0.0363(4) 0.0635(5) -0.0066(4) 0.0038(4) 0.0015(3)
Cl1 0.0514(5) 0.0471(5) 0.0249(4) 0.0079(3) 0.0110(3) -0.0090(4)
Cl2 0.0295(4) 0.0256(4) 0.0352(4) 0.0008(3) 0.0080(3) 0.0008(3)
N1 0.0223(11) 0.0252(12) 0.0222(12) 0.0011(9) 0.0053(9) -0.0036(9)
N2 0.0252(11) 0.0241(11) 0.0217(11) 0.0033(9) 0.0085(9) -0.0003(9)
N3 0.0224(11) 0.0232(11) 0.0201(11) 0.0024(9) 0.0064(9) 0.0025(9)
C8 0.0273(14) 0.0274(14) 0.0272(15) 0.0023(11) 0.0064(12) -0.0084(11)
C9 0.0263(14) 0.0392(17) 0.0338(16) 0.0046(13) 0.0043(13) -0.0068(12)
C10 0.0271(16) 0.053(2) 0.0421(18) 0.0000(15) -0.0050(14) -0.0024(14)
C11 0.050(2) 0.056(2) 0.0377(19) -0.0108(16) -0.0076(16) -0.0077(17)
C12 0.0496(19) 0.0410(18) 0.0352(17) -0.0078(14) 0.0057(15) -0.0051(15)
C13 0.0324(15) 0.0235(14) 0.0308(15) 0.0012(11) 0.0047(13) -0.0059(12)
C14 0.0274(16) 0.0543(19) 0.0395(18) 0.0009(15) 0.0082(14) 0.0034(14)
C15 0.050(2) 0.059(2) 0.058(2) 0.0006(18) 0.0046(18) 0.0162(17)
C16 0.0284(17) 0.098(3) 0.058(2) 0.006(2) 0.0142(16) 0.0013(18)
C17 0.0361(16) 0.0257(15) 0.0293(15) 0.0003(11) 0.0074(13) 0.0012(12)
C19 0.0437(18) 0.0427(18) 0.0355(17) 0.0003(14) 0.0144(14) 0.0030(14)
C18 0.059(2) 0.0267(17) 0.063(2) 0.0018(15) 0.0143(18) -0.0003(15)
C1 0.0237(14) 0.0301(15) 0.0297(15) 0.0055(12) 0.0074(12) -0.0046(11)
C20 0.0422(18) 0.053(2) 0.0342(17) 0.0098(15) 0.0057(14) -0.0245(16)
C21 0.083(3) 0.043(2) 0.046(2) 0.0124(16) 0.0041(19) -0.0271(19)
C2 0.0291(14) 0.0293(15) 0.0268(14) 0.0036(11) 0.0112(12) -0.0034(12)
C3 0.0475(18) 0.0426(18) 0.0272(16) 0.0060(13) 0.0166(14) -0.0094(15)
C4 0.0562(19) 0.0457(18) 0.0226(15) 0.0036(13) 0.0192(14) -0.0070(16)
C5 0.0429(17) 0.0351(16) 0.0221(14) 0.0006(12) 0.0110(13) -0.0015(14)
C6 0.0276(14) 0.0240(14) 0.0201(13) 0.0004(11) 0.0081(11) 0.0026(11)
C7 0.0223(13) 0.0224(13) 0.0238(14) -0.0008(11) 0.0051(11) 0.0047(11)
C22 0.0331(15) 0.0302(15) 0.0209(14) -0.0043(11) 0.0037(12) -0.0028(12)
C23 0.0386(17) 0.060(2) 0.0271(16) 0.0006(15) 0.0014(13) 0.0046(16)
C24 0.0246(13) 0.0245(14) 0.0178(13) 0.0005(10) 0.0007(11) -0.0047(11)
C25 0.0283(14) 0.0268(14) 0.0177(13) -0.0014(11) 0.0020(11) -0.0052(11)
C26 0.0335(15) 0.0331(16) 0.0263(14) 0.0020(12) 0.0096(12) -0.0058(13)
C27 0.0408(17) 0.0302(16) 0.0341(16) 0.0071(12) 0.0065(14) -0.0115(13)
C28 0.0407(17) 0.0250(15) 0.0350(16) 0.0071(12) 0.0036(14) -0.0013(13)
C29 0.0294(15) 0.0272(15) 0.0230(14) 0.0015(11) 0.0011(12) -0.0029(12)
C30 0.0288(14) 0.0297(15) 0.0293(15) 0.0005(12) 0.0099(12) -0.0011(12)
C31 0.0480(18) 0.0338(17) 0.0435(18) 0.0006(13) 0.0249(15) 0.0048(14)
C32 0.0303(16) 0.0474(19) 0.053(2) 0.0147(16) 0.0060(15) -0.0031(14)
C33 0.0357(15) 0.0212(14) 0.0298(15) 0.0005(11) 0.0059(13) 0.0045(12)
C34 0.056(2) 0.047(2) 0.053(2) -0.0182(16) 0.0143(17) 0.0053(16)
C35 0.0379(17) 0.0426(19) 0.054(2) 0.0150(15) 0.0092(15) 0.0117(14)
N4 0.152(4) 0.139(4) 0.126(4) 0.018(3) 0.092(4) 0.065(4)
C36 0.064(3) 0.089(3) 0.061(3) -0.008(2) 0.032(2) 0.000(2)
C37 0.057(3) 0.121(4) 0.089(3) 0.039(3) 0.012(2) -0.006(3)
_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 N2 2.063(2) . ?
V1 N3 2.188(2) . ?
V1 N1 2.213(2) . ?
V1 Cl3 2.2862(12) . ?
V1 Cl1 2.2918(13) . ?
V1 Cl2 2.3339(11) . ?
N1 C1 1.280(3) . ?
N1 C8 1.466(3) . ?
N2 C2 1.330(3) . ?
N2 C6 1.347(3) . ?
N3 C7 1.292(3) . ?
N3 C24 1.447(3) . ?
C8 C13 1.391(4) . ?
C8 C9 1.415(4) . ?
C9 C10 1.402(4) . ?
C9 C14 1.516(4) . ?
C10 C11 1.368(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.383(4) . ?
C11 H11 0.9500 . ?
C12 C13 1.392(4) . ?
C12 H12 0.9500 . ?
C13 C17 1.523(4) . ?
C14 C15 1.530(4) . ?
C14 C16 1.531(4) . ?
C14 H14 1.0000 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C18 1.527(4) . ?
C17 C19 1.527(4) . ?
C17 H17 1.0000 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C1 C2 1.495(4) . ?
C1 C20 1.498(4) . ?
C20 C21 1.525(4) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C2 C3 1.390(4) . ?
C3 C4 1.388(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.373(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.384(4) . ?
C5 H5 0.9500 . ?
C6 C7 1.489(3) . ?
C7 C22 1.504(3) . ?
C22 C23 1.543(4) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 C25 1.408(4) . ?
C24 C29 1.408(4) . ?
C25 C26 1.388(4) . ?
C25 C30 1.514(4) . ?
C26 C27 1.387(4) . ?
C26 H26 0.9500 . ?
C27 C28 1.370(4) . ?
C27 H27 0.9500 . ?
C28 C29 1.393(4) . ?
C28 H28 0.9500 . ?
C29 C33 1.518(4) . ?
C30 C31 1.538(4) . ?
C30 C32 1.550(4) . ?
C30 H30 1.0000 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 C34 1.532(4) . ?
C33 C35 1.541(4) . ?
C33 H33 1.0000 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
N4 C36 1.121(5) . ?
C36 C37 1.430(6) . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
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
N2 V1 N3 75.38(8) . . ?
N2 V1 N1 75.52(8) . . ?
N3 V1 N1 150.72(8) . . ?
N2 V1 Cl3 87.10(6) . . ?
N3 V1 Cl3 89.57(7) . . ?
N1 V1 Cl3 85.89(7) . . ?
N2 V1 Cl1 176.42(6) . . ?
N3 V1 Cl1 103.67(6) . . ?
N1 V1 Cl1 105.57(6) . . ?
Cl3 V1 Cl1 96.37(3) . . ?
N2 V1 Cl2 81.27(6) . . ?
N3 V1 Cl2 87.87(6) . . ?
N1 V1 Cl2 90.81(7) . . ?
Cl3 V1 Cl2 168.36(3) . . ?
Cl1 V1 Cl2 95.27(3) . . ?
C1 N1 C8 120.0(2) . . ?
C1 N1 V1 114.62(16) . . ?
C8 N1 V1 125.28(15) . . ?
C2 N2 C6 122.4(2) . . ?
C2 N2 V1 118.71(16) . . ?
C6 N2 V1 118.93(17) . . ?
C7 N3 C24 120.5(2) . . ?
C7 N3 V1 115.66(16) . . ?
C24 N3 V1 123.78(15) . . ?
C13 C8 C9 121.7(2) . . ?
C13 C8 N1 118.8(2) . . ?
C9 C8 N1 119.4(2) . . ?
C10 C9 C8 117.3(3) . . ?
C10 C9 C14 118.3(3) . . ?
C8 C9 C14 124.4(2) . . ?
C11 C10 C9 121.9(3) . . ?
C11 C10 H10 119.1 . . ?
C9 C10 H10 119.1 . . ?
C10 C11 C12 119.2(3) . . ?
C10 C11 H11 120.4 . . ?
C12 C11 H11 120.4 . . ?
C11 C12 C13 122.1(3) . . ?
C11 C12 H12 118.9 . . ?
C13 C12 H12 118.9 . . ?
C8 C13 C12 117.7(3) . . ?
C8 C13 C17 123.0(2) . . ?
C12 C13 C17 119.2(3) . . ?
C9 C14 C15 111.1(3) . . ?
C9 C14 C16 111.3(3) . . ?
C15 C14 C16 109.6(3) . . ?
C9 C14 H14 108.3 . . ?
C15 C14 H14 108.3 . . ?
C16 C14 H14 108.3 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C13 C17 C18 111.4(2) . . ?
C13 C17 C19 112.1(2) . . ?
C18 C17 C19 109.5(3) . . ?
C13 C17 H17 107.9 . . ?
C18 C17 H17 107.9 . . ?
C19 C17 H17 107.9 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N1 C1 C2 116.3(2) . . ?
N1 C1 C20 125.6(2) . . ?
C2 C1 C20 118.1(2) . . ?
C1 C20 C21 111.4(2) . . ?
C1 C20 H20A 109.4 . . ?
C21 C20 H20A 109.4 . . ?
C1 C20 H20B 109.4 . . ?
C21 C20 H20B 109.4 . . ?
H20A C20 H20B 108.0 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N2 C2 C3 119.7(2) . . ?
N2 C2 C1 114.8(2) . . ?
C3 C2 C1 125.5(2) . . ?
C4 C3 C2 118.6(3) . . ?
C4 C3 H3 120.7 . . ?
C2 C3 H3 120.7 . . ?
C5 C4 C3 120.9(3) . . ?
C5 C4 H4 119.6 . . ?
C3 C4 H4 119.6 . . ?
C4 C5 C6 118.2(2) . . ?
C4 C5 H5 120.9 . . ?
C6 C5 H5 120.9 . . ?
N2 C6 C5 120.3(2) . . ?
N2 C6 C7 114.0(2) . . ?
C5 C6 C7 125.7(2) . . ?
N3 C7 C6 115.8(2) . . ?
N3 C7 C22 125.1(2) . . ?
C6 C7 C22 119.1(2) . . ?
C7 C22 C23 111.5(2) . . ?
C7 C22 H22A 109.3 . . ?
C23 C22 H22A 109.3 . . ?
C7 C22 H22B 109.3 . . ?
C23 C22 H22B 109.3 . . ?
H22A C22 H22B 108.0 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C25 C24 C29 121.9(2) . . ?
C25 C24 N3 120.3(2) . . ?
C29 C24 N3 117.8(2) . . ?
C26 C25 C24 117.8(2) . . ?
C26 C25 C30 118.8(2) . . ?
C24 C25 C30 123.4(2) . . ?
C27 C26 C25 121.3(3) . . ?
C27 C26 H26 119.4 . . ?
C25 C26 H26 119.4 . . ?
C28 C27 C26 119.7(3) . . ?
C28 C27 H27 120.1 . . ?
C26 C27 H27 120.1 . . ?
C27 C28 C29 122.1(3) . . ?
C27 C28 H28 118.9 . . ?
C29 C28 H28 118.9 . . ?
C28 C29 C24 117.1(3) . . ?
C28 C29 C33 119.4(2) . . ?
C24 C29 C33 123.4(2) . . ?
C25 C30 C31 112.0(2) . . ?
C25 C30 C32 111.2(2) . . ?
C31 C30 C32 109.6(2) . . ?
C25 C30 H30 108.0 . . ?
C31 C30 H30 108.0 . . ?
C32 C30 H30 108.0 . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C29 C33 C34 111.1(2) . . ?
C29 C33 C35 112.5(2) . . ?
C34 C33 C35 110.1(2) . . ?
C29 C33 H33 107.6 . . ?
C34 C33 H33 107.6 . . ?
C35 C33 H33 107.6 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C33 C35 H35A 109.5 . . ?
C33 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C33 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
N4 C36 C37 178.9(6) . . ?
C36 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C36 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
_diffrn_measured_fraction_theta_max 0.972
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.549
_refine_diff_density_min         -0.433
_refine_diff_density_rms         0.071


data_ms111277
_database_code_depnum_ccdc_archive 'CCDC 891101'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C31 H23 Cl3 N3 V, C2 H3 N'
_chemical_formula_sum            'C33 H26 Cl3 N4 V'
_exptl_crystal_recrystallization_method MeCN
_chemical_melting_point          ?
_exptl_crystal_description       Plate
_exptl_crystal_colour            Brown
_diffrn_ambient_temperature      198(1)
_chemical_formula_weight         635.87
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'
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           orthorhombic
_symmetry_space_group_name_H-M   'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_int_tables_number      61
_chemical_absolute_configuration ?
loop_
_symmetry_equiv_pos_as_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'
'-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                   19.323(2)
_cell_length_b                   11.4292(14)
_cell_length_c                   27.637(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     6103.4(13)
_cell_formula_units_Z            8
_cell_measurement_temperature    198(1)
_cell_measurement_reflns_used    9590
_cell_measurement_theta_min      2.20
_cell_measurement_theta_max      27.73
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.01
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.384
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2608
_exptl_absorpt_coefficient_mu    0.617
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8365
_exptl_absorpt_correction_T_max  0.9939
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_special_details           
;
Crystal decay was monitored by repeating the initial 50 frames
at the end of the data collection and analyzing duplicate
reflections
;
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              K760
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker AXS SMART1000/P4'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            39589
_diffrn_reflns_av_R_equivalents  0.1213
_diffrn_reflns_av_sigmaI/netI    0.1063
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         1.47
_diffrn_reflns_theta_max         27.49
_reflns_number_total             6941
_reflns_number_gt                3524
_reflns_threshold_expression     'I > 2\s(I)'
_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'Bruker SHELXTL (Sheldrick, 2008)'
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0186P)^2^+25.0815P] where P=(Fo^2^+2Fc^2^)/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         6941
_refine_ls_number_parameters     371
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1619
_refine_ls_R_factor_gt           0.0651
_refine_ls_wR_factor_ref         0.1702
_refine_ls_wR_factor_gt          0.1201
_refine_ls_goodness_of_fit_ref   1.161
_refine_ls_restrained_S_all      1.161
_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 0.16183(4) 0.08160(8) 0.29523(3) 0.0212(2) Uani 1 1 d . . .
Cl1 Cl 0.04301(7) 0.09501(14) 0.29144(6) 0.0374(4) Uani 1 1 d . . .
Cl2 Cl 0.16186(7) -0.11141(11) 0.32341(5) 0.0328(3) Uani 1 1 d . . .
Cl3 Cl 0.17521(7) 0.26928(12) 0.26484(6) 0.0366(4) Uani 1 1 d . . .
N1 N 0.1877(2) 0.1339(4) 0.36783(15) 0.0235(10) Uani 1 1 d . . .
N2 N 0.26908(19) 0.0776(4) 0.29788(16) 0.0214(9) Uani 1 1 d . . .
N3 N 0.1942(2) 0.0170(4) 0.22554(15) 0.0241(10) Uani 1 1 d . . .
C1 C 0.2532(3) 0.1299(4) 0.37937(18) 0.0228(11) Uani 1 1 d . . .
C2 C 0.3009(3) 0.0995(5) 0.33990(19) 0.0249(12) Uani 1 1 d . . .
C3 C 0.3725(3) 0.0910(5) 0.3432(2) 0.0273(13) Uani 1 1 d . . .
H3 H 0.3952 0.1040 0.3732 0.033 Uiso 1 1 calc R . .
C4 C 0.4098(3) 0.0636(5) 0.3027(2) 0.0303(14) Uani 1 1 d . . .
H4 H 0.4587 0.0570 0.3046 0.036 Uiso 1 1 calc R . .
C5 C 0.3763(3) 0.0453(5) 0.2590(2) 0.0263(13) Uani 1 1 d . . .
H5 H 0.4019 0.0295 0.2303 0.032 Uiso 1 1 calc R . .
C6 C 0.3041(3) 0.0507(4) 0.25796(19) 0.0232(12) Uani 1 1 d . . .
C7 C 0.2601(3) 0.0198(4) 0.21594(18) 0.0222(12) Uani 1 1 d . . .
C8 C 0.1389(3) 0.1695(5) 0.4042(2) 0.0297(13) Uani 1 1 d . . .
C9 C 0.1420(3) 0.2811(6) 0.4233(2) 0.0390(16) Uani 1 1 d . . .
H9 H 0.1757 0.3352 0.4121 0.047 Uiso 1 1 calc R . .
C10 C 0.0955(3) 0.3133(7) 0.4591(2) 0.0515(19) Uani 1 1 d . . .
H10 H 0.0971 0.3898 0.4725 0.062 Uiso 1 1 calc R . .
C11 C 0.0474(3) 0.2351(8) 0.4752(2) 0.058(2) Uani 1 1 d . . .
H11 H 0.0169 0.2567 0.5007 0.069 Uiso 1 1 calc R . .
C12 C 0.0423(3) 0.1254(8) 0.4551(2) 0.055(2) Uani 1 1 d . . .
H12 H 0.0075 0.0729 0.4660 0.067 Uiso 1 1 calc R . .
C13 C 0.0880(3) 0.0909(6) 0.4187(2) 0.0417(16) Uani 1 1 d . . .
H13 H 0.0845 0.0157 0.4043 0.050 Uiso 1 1 calc R . .
C14 C 0.2810(3) 0.1466(5) 0.42910(19) 0.0276(13) Uani 1 1 d . . .
C15 C 0.3238(3) 0.2412(6) 0.4402(2) 0.0345(14) Uani 1 1 d . . .
H15 H 0.3347 0.2978 0.4162 0.041 Uiso 1 1 calc R . .
C16 C 0.3503(3) 0.2517(6) 0.4863(2) 0.0445(17) Uani 1 1 d . . .
H16 H 0.3784 0.3172 0.4942 0.053 Uiso 1 1 calc R . .
C17 C 0.3366(3) 0.1685(7) 0.5210(2) 0.0485(18) Uani 1 1 d . . .
H17 H 0.3553 0.1765 0.5527 0.058 Uiso 1 1 calc R . .
C18 C 0.2955(3) 0.0735(6) 0.5098(2) 0.0432(16) Uani 1 1 d . . .
H18 H 0.2869 0.0152 0.5336 0.052 Uiso 1 1 calc R . .
C19 C 0.2669(3) 0.0625(5) 0.4642(2) 0.0346(14) Uani 1 1 d . . .
H19 H 0.2379 -0.0021 0.4568 0.042 Uiso 1 1 calc R . .
C20 C 0.2924(3) -0.0054(5) 0.1684(2) 0.0271(13) Uani 1 1 d . . .
C21 C 0.3356(3) 0.0774(6) 0.1483(2) 0.0362(14) Uani 1 1 d . . .
H21 H 0.3433 0.1495 0.1645 0.043 Uiso 1 1 calc R . .
C22 C 0.3678(3) 0.0552(6) 0.1044(2) 0.0467(18) Uani 1 1 d . . .
H22 H 0.3974 0.1123 0.0904 0.056 Uiso 1 1 calc R . .
C23 C 0.3569(3) -0.0492(7) 0.0811(2) 0.0512(19) Uani 1 1 d . . .
H23 H 0.3786 -0.0635 0.0508 0.061 Uiso 1 1 calc R . .
C24 C 0.3147(3) -0.1335(6) 0.1013(2) 0.0447(17) Uani 1 1 d . . .
H24 H 0.3081 -0.2061 0.0852 0.054 Uiso 1 1 calc R . .
C25 C 0.2819(3) -0.1123(5) 0.1451(2) 0.0326(14) Uani 1 1 d . . .
H25 H 0.2526 -0.1698 0.1591 0.039 Uiso 1 1 calc R . .
C26 C 0.1442(3) -0.0118(5) 0.1888(2) 0.0269(13) Uani 1 1 d . . .
C27 C 0.1354(3) 0.0588(6) 0.1487(2) 0.0369(15) Uani 1 1 d . . .
H27 H 0.1635 0.1262 0.1444 0.044 Uiso 1 1 calc R . .
C28 C 0.0849(3) 0.0305(7) 0.1146(2) 0.0498(19) Uani 1 1 d . . .
H28 H 0.0782 0.0784 0.0869 0.060 Uiso 1 1 calc R . .
C29 C 0.0446(3) -0.0682(7) 0.1216(3) 0.055(2) Uani 1 1 d . . .
H29 H 0.0106 -0.0887 0.0983 0.066 Uiso 1 1 calc R . .
C30 C 0.0531(3) -0.1362(7) 0.1618(3) 0.0510(19) Uani 1 1 d . . .
H30 H 0.0246 -0.2029 0.1663 0.061 Uiso 1 1 calc R . .
C31 C 0.1028(3) -0.1093(5) 0.1960(2) 0.0369(15) Uani 1 1 d . . .
H31 H 0.1084 -0.1568 0.2239 0.044 Uiso 1 1 calc R . .
C32 C 0.9950(3) 0.8009(6) 0.3683(3) 0.0442(17) Uani 1 1 d . . .
C33 C 0.9731(3) 0.8127(6) 0.3184(2) 0.0454(17) Uani 1 1 d . . .
H33A H 0.9729 0.7356 0.3029 0.068 Uiso 1 1 calc R . .
H33B H 1.0052 0.8645 0.3012 0.068 Uiso 1 1 calc R . .
H33C H 0.9264 0.8460 0.3173 0.068 Uiso 1 1 calc R . .
N4 N 1.0116(3) 0.7910(7) 0.4074(2) 0.0659(19) Uani 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
V1 0.0170(4) 0.0190(4) 0.0276(5) 0.0014(4) -0.0004(4) -0.0001(4)
Cl1 0.0212(6) 0.0399(9) 0.0512(9) 0.0006(8) -0.0034(7) 0.0011(6)
Cl2 0.0354(7) 0.0206(7) 0.0423(8) 0.0078(6) 0.0061(7) -0.0004(6)
Cl3 0.0345(8) 0.0205(7) 0.0550(10) 0.0069(7) -0.0068(7) -0.0023(6)
N1 0.023(2) 0.024(3) 0.024(2) 0.001(2) -0.0002(19) 0.0010(19)
N2 0.021(2) 0.017(2) 0.027(2) 0.003(2) -0.0005(19) -0.0023(18)
N3 0.028(2) 0.019(2) 0.026(2) -0.0028(19) -0.001(2) 0.000(2)
C1 0.024(3) 0.018(3) 0.027(3) -0.001(2) 0.000(2) -0.003(2)
C2 0.026(3) 0.018(3) 0.031(3) 0.002(2) 0.003(2) -0.001(2)
C3 0.023(3) 0.025(3) 0.034(3) 0.003(3) -0.006(2) -0.001(2)
C4 0.021(3) 0.025(3) 0.045(4) -0.001(3) -0.001(3) 0.000(2)
C5 0.023(3) 0.021(3) 0.035(3) 0.001(3) 0.007(2) 0.000(2)
C6 0.024(3) 0.018(3) 0.028(3) 0.002(2) 0.003(2) -0.005(2)
C7 0.025(3) 0.015(3) 0.027(3) 0.004(2) -0.002(2) -0.001(2)
C8 0.023(3) 0.041(4) 0.026(3) 0.005(3) -0.001(2) 0.004(3)
C9 0.028(3) 0.052(4) 0.036(4) -0.008(3) -0.003(3) 0.008(3)
C10 0.039(4) 0.068(5) 0.048(4) -0.018(4) -0.003(3) 0.014(4)
C11 0.032(3) 0.104(7) 0.037(4) -0.009(4) -0.003(3) 0.021(4)
C12 0.026(3) 0.094(7) 0.046(4) 0.022(4) 0.005(3) -0.001(4)
C13 0.028(3) 0.056(4) 0.041(4) 0.012(3) 0.004(3) -0.002(3)
C14 0.020(3) 0.035(3) 0.027(3) 0.000(3) 0.000(2) 0.005(2)
C15 0.031(3) 0.046(4) 0.026(3) 0.004(3) -0.002(2) -0.004(3)
C16 0.035(3) 0.059(5) 0.039(4) -0.009(3) -0.007(3) -0.005(3)
C17 0.046(4) 0.076(5) 0.023(3) 0.000(3) -0.009(3) 0.013(4)
C18 0.046(4) 0.053(4) 0.031(3) 0.015(3) 0.001(3) 0.007(4)
C19 0.034(3) 0.033(4) 0.037(3) 0.004(3) 0.005(3) 0.004(3)
C20 0.022(3) 0.028(3) 0.030(3) 0.004(3) -0.001(2) 0.005(2)
C21 0.031(3) 0.040(4) 0.038(3) 0.003(3) 0.007(3) -0.001(3)
C22 0.045(4) 0.055(5) 0.040(4) 0.015(4) 0.013(3) 0.005(3)
C23 0.048(4) 0.073(6) 0.033(4) 0.004(4) 0.006(3) 0.024(4)
C24 0.055(4) 0.046(4) 0.033(4) -0.003(3) -0.006(3) 0.019(4)
C25 0.037(3) 0.031(3) 0.030(3) -0.002(3) -0.002(3) 0.005(3)
C26 0.019(3) 0.028(3) 0.034(3) -0.006(3) 0.001(2) 0.003(2)
C27 0.035(3) 0.034(4) 0.041(4) -0.004(3) -0.003(3) 0.005(3)
C28 0.039(4) 0.071(5) 0.039(4) -0.012(4) -0.010(3) 0.016(4)
C29 0.028(3) 0.079(6) 0.059(5) -0.042(4) -0.009(3) 0.002(4)
C30 0.033(3) 0.054(5) 0.066(5) -0.024(4) 0.005(4) -0.012(3)
C31 0.032(3) 0.036(4) 0.043(4) -0.012(3) 0.002(3) -0.002(3)
C32 0.027(3) 0.046(4) 0.060(5) 0.001(4) 0.010(3) 0.003(3)
C33 0.043(4) 0.041(4) 0.052(4) 0.003(3) -0.005(3) 0.004(3)
N4 0.043(3) 0.102(6) 0.053(4) 0.005(4) 0.005(3) 0.003(4)
_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 N2 2.074(4) . ?
V1 N1 2.153(4) . ?
V1 N3 2.155(4) . ?
V1 Cl1 2.3033(15) . ?
V1 Cl3 2.3181(17) . ?
V1 Cl2 2.3393(16) . ?
N1 C1 1.305(6) . ?
N1 C8 1.437(7) . ?
N2 C6 1.330(6) . ?
N2 C2 1.337(7) . ?
N3 C7 1.301(6) . ?
N3 C26 1.440(7) . ?
C1 C2 1.470(7) . ?
C1 C14 1.488(7) . ?
C2 C3 1.390(7) . ?
C3 C4 1.368(7) . ?
C3 H3 0.9500 . ?
C4 C5 1.387(8) . ?
C4 H4 0.9500 . ?
C5 C6 1.397(7) . ?
C5 H5 0.9500 . ?
C6 C7 1.482(7) . ?
C7 C20 1.482(7) . ?
C8 C9 1.382(8) . ?
C8 C13 1.391(8) . ?
C9 C10 1.387(8) . ?
C9 H9 0.9500 . ?
C10 C11 1.364(10) . ?
C10 H10 0.9500 . ?
C11 C12 1.375(10) . ?
C11 H11 0.9500 . ?
C12 C13 1.395(9) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C14 C19 1.392(8) . ?
C14 C15 1.396(8) . ?
C15 C16 1.378(8) . ?
C15 H15 0.9500 . ?
C16 C17 1.378(9) . ?
C16 H16 0.9500 . ?
C17 C18 1.380(9) . ?
C17 H17 0.9500 . ?
C18 C19 1.382(8) . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
C20 C21 1.379(8) . ?
C20 C25 1.396(8) . ?
C21 C22 1.386(8) . ?
C21 H21 0.9500 . ?
C22 C23 1.372(10) . ?
C22 H22 0.9500 . ?
C23 C24 1.381(9) . ?
C23 H23 0.9500 . ?
C24 C25 1.390(8) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
C26 C27 1.382(8) . ?
C26 C31 1.386(8) . ?
C27 C28 1.395(8) . ?
C27 H27 0.9500 . ?
C28 C29 1.385(10) . ?
C28 H28 0.9500 . ?
C29 C30 1.365(10) . ?
C29 H29 0.9500 . ?
C30 C31 1.381(8) . ?
C30 H30 0.9500 . ?
C31 H31 0.9500 . ?
C32 N4 1.131(8) . ?
C32 C33 1.450(9) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
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
N2 V1 N1 74.98(17) . . ?
N2 V1 N3 74.58(17) . . ?
N1 V1 N3 149.38(16) . . ?
N2 V1 Cl1 177.40(14) . . ?
N1 V1 Cl1 104.81(12) . . ?
N3 V1 Cl1 105.75(12) . . ?
N2 V1 Cl3 85.53(13) . . ?
N1 V1 Cl3 93.14(13) . . ?
N3 V1 Cl3 87.74(13) . . ?
Cl1 V1 Cl3 91.90(6) . . ?
N2 V1 Cl2 88.11(13) . . ?
N1 V1 Cl2 87.22(13) . . ?
N3 V1 Cl2 88.55(12) . . ?
Cl1 V1 Cl2 94.48(6) . . ?
Cl3 V1 Cl2 173.30(7) . . ?
C1 N1 C8 118.4(4) . . ?
C1 N1 V1 116.3(3) . . ?
C8 N1 V1 125.2(3) . . ?
C6 N2 C2 122.0(4) . . ?
C6 N2 V1 118.9(3) . . ?
C2 N2 V1 119.0(3) . . ?
C7 N3 C26 121.3(4) . . ?
C7 N3 V1 117.3(3) . . ?
C26 N3 V1 120.9(3) . . ?
N1 C1 C2 115.7(5) . . ?
N1 C1 C14 124.8(5) . . ?
C2 C1 C14 119.3(5) . . ?
N2 C2 C3 120.1(5) . . ?
N2 C2 C1 113.6(4) . . ?
C3 C2 C1 126.3(5) . . ?
C4 C3 C2 119.1(5) . . ?
C4 C3 H3 120.4 . . ?
C2 C3 H3 120.4 . . ?
C3 C4 C5 120.2(5) . . ?
C3 C4 H4 119.9 . . ?
C5 C4 H4 119.9 . . ?
C4 C5 C6 118.4(5) . . ?
C4 C5 H5 120.8 . . ?
C6 C5 H5 120.8 . . ?
N2 C6 C5 120.1(5) . . ?
N2 C6 C7 114.4(4) . . ?
C5 C6 C7 125.3(5) . . ?
N3 C7 C6 114.1(5) . . ?
N3 C7 C20 126.0(5) . . ?
C6 C7 C20 119.9(4) . . ?
C9 C8 C13 121.1(6) . . ?
C9 C8 N1 120.0(5) . . ?
C13 C8 N1 118.9(6) . . ?
C8 C9 C10 119.3(6) . . ?
C8 C9 H9 120.4 . . ?
C10 C9 H9 120.4 . . ?
C11 C10 C9 120.1(7) . . ?
C11 C10 H10 120.0 . . ?
C9 C10 H10 120.0 . . ?
C10 C11 C12 120.9(7) . . ?
C10 C11 H11 119.6 . . ?
C12 C11 H11 119.6 . . ?
C11 C12 C13 120.3(7) . . ?
C11 C12 H12 119.8 . . ?
C13 C12 H12 119.8 . . ?
C8 C13 C12 118.2(7) . . ?
C8 C13 H13 120.9 . . ?
C12 C13 H13 120.9 . . ?
C19 C14 C15 119.9(5) . . ?
C19 C14 C1 119.0(5) . . ?
C15 C14 C1 121.0(5) . . ?
C16 C15 C14 119.3(6) . . ?
C16 C15 H15 120.3 . . ?
C14 C15 H15 120.3 . . ?
C15 C16 C17 120.9(6) . . ?
C15 C16 H16 119.5 . . ?
C17 C16 H16 119.5 . . ?
C16 C17 C18 119.8(6) . . ?
C16 C17 H17 120.1 . . ?
C18 C17 H17 120.1 . . ?
C17 C18 C19 120.4(6) . . ?
C17 C18 H18 119.8 . . ?
C19 C18 H18 119.8 . . ?
C18 C19 C14 119.7(6) . . ?
C18 C19 H19 120.2 . . ?
C14 C19 H19 120.2 . . ?
C21 C20 C25 120.1(5) . . ?
C21 C20 C7 118.6(5) . . ?
C25 C20 C7 121.2(5) . . ?
C20 C21 C22 119.9(6) . . ?
C20 C21 H21 120.0 . . ?
C22 C21 H21 120.0 . . ?
C23 C22 C21 120.1(6) . . ?
C23 C22 H22 119.9 . . ?
C21 C22 H22 119.9 . . ?
C22 C23 C24 120.5(6) . . ?
C22 C23 H23 119.8 . . ?
C24 C23 H23 119.8 . . ?
C23 C24 C25 120.0(6) . . ?
C23 C24 H24 120.0 . . ?
C25 C24 H24 120.0 . . ?
C24 C25 C20 119.3(6) . . ?
C24 C25 H25 120.4 . . ?
C20 C25 H25 120.4 . . ?
C27 C26 C31 120.9(5) . . ?
C27 C26 N3 120.9(5) . . ?
C31 C26 N3 118.1(5) . . ?
C26 C27 C28 119.5(6) . . ?
C26 C27 H27 120.2 . . ?
C28 C27 H27 120.2 . . ?
C29 C28 C27 119.2(7) . . ?
C29 C28 H28 120.4 . . ?
C27 C28 H28 120.4 . . ?
C30 C29 C28 120.7(6) . . ?
C30 C29 H29 119.7 . . ?
C28 C29 H29 119.7 . . ?
C29 C30 C31 120.9(7) . . ?
C29 C30 H30 119.5 . . ?
C31 C30 H30 119.5 . . ?
C30 C31 C26 118.8(6) . . ?
C30 C31 H31 120.6 . . ?
C26 C31 H31 120.6 . . ?
N4 C32 C33 179.4(8) . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.580
_refine_diff_density_min         -0.479
_refine_diff_density_rms         0.105