# Supplementary Material (ESI) for Dalton Transactions
# This journal is (c) The Royal Society of Chemistry 2010

data_global
_journal_name_full               'Dalton Trans.'

_journal_coden_Cambridge         0222

_publ_contact_author_name        'Moris Eisen'
_publ_contact_author_email       CHMORIS@TECHUNIX.TECHNION.AC.IL

_publ_section_title              
;
Mono- and bis-amidinate 2,6-xylylimido vanadium
chlorides: synthesis, structure, and reactivity.
;
loop_
_publ_author_name
'Moris Eisen'
'Sinai Aharonovich'
'Mark Botoshanski'
'Kotohiro Nomura'
'Boris Tumanskii'
;
R.Waymouth
;

# Attachment 'complex_4.cif'

data_complex4
_database_code_depnum_ccdc_archive 'CCDC 757622'
#TrackingRef 'complex_4.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            complex4
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H63 Cl N5 Si4 V'
_chemical_formula_weight         788.68

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
V V 0.3005 0.5294 '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'
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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'C 2/c'

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

_cell_length_a                   38.736(8)
_cell_length_b                   12.597(2)
_cell_length_c                   18.715(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.5800(11)
_cell_angle_gamma                90.00
_cell_volume                     9072(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    240(1)
_cell_measurement_reflns_used    27667
_cell_measurement_theta_min      1.99
_cell_measurement_theta_max      25.33

_exptl_crystal_description       plate
_exptl_crystal_colour            red-brown
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.155
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3376
_exptl_absorpt_coefficient_mu    0.414
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.793
_exptl_absorpt_correction_T_max  0.978
_exptl_absorpt_process_details   
;
multi-scan from symmetry-related measurements
Sortav (Blessing 1995)
;
_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      240(1)
_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  'Nonius KappaCCD'
_diffrn_measurement_method       phi-scan
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            27667
_diffrn_reflns_av_R_equivalents  0.0722
_diffrn_reflns_av_sigmaI/netI    0.0718
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.99
_diffrn_reflns_theta_max         25.33
_reflns_number_total             8235
_reflns_number_gt                5133
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect (Nonius, 2006)'
_computing_cell_refinement       'DENZO HKL2000 (Otwinowski & Minor 1997)'
_computing_data_reduction        'DENZO HKL2000 (Otwinowski & Minor 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'TEXSAN (MSC, 1999)'
_computing_publication_material  ?

_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. Small unresolved disorder
at the ethyl-group atoms C30 and C31 lead to ubnormal bond lenghts and
because of that restrains were applied.
;

_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^)+(0.0804P)^2^+0.0000P] 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         8235
_refine_ls_number_parameters     442
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0984
_refine_ls_R_factor_gt           0.0512
_refine_ls_wR_factor_ref         0.1403
_refine_ls_wR_factor_gt          0.1253
_refine_ls_goodness_of_fit_ref   0.939
_refine_ls_restrained_S_all      0.960
_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 0.132282(14) 0.35019(4) 0.19518(3) 0.04096(16) Uani 1 1 d . . .
Cl1 Cl 0.15859(2) 0.38291(7) 0.09261(5) 0.0601(3) Uani 1 1 d . . .
Si1 Si 0.09326(2) 0.18809(7) 0.32569(5) 0.0489(2) Uani 1 1 d . . .
Si2 Si 0.22185(2) 0.30901(7) 0.24505(5) 0.0465(2) Uani 1 1 d . . .
Si3 Si 0.05284(3) 0.46084(8) 0.14154(6) 0.0589(3) Uani 1 1 d . . .
Si4 Si 0.12468(3) 0.08844(8) 0.09218(5) 0.0566(3) Uani 1 1 d . . .
N5 N 0.12598(6) 0.25458(18) 0.28620(13) 0.0385(6) Uani 1 1 d . . .
N2 N 0.17773(6) 0.28045(19) 0.24806(13) 0.0400(6) Uani 1 1 d . . .
N3 N 0.08343(7) 0.3568(2) 0.15252(14) 0.0459(6) Uani 1 1 d . . .
N4 N 0.11114(7) 0.2040(2) 0.13273(14) 0.0476(6) Uani 1 1 d . . .
N1 N 0.13747(7) 0.46989(19) 0.23261(14) 0.0463(6) Uani 1 1 d . . .
C3 C 0.16021(8) 0.2353(2) 0.29623(16) 0.0389(7) Uani 1 1 d . . .
C2 C 0.08483(8) 0.2659(3) 0.11321(17) 0.0484(8) Uani 1 1 d . . .
C1 C 0.14357(8) 0.5696(2) 0.2646(2) 0.0530(9) Uani 1 1 d . . .
C4 C 0.08764(12) 0.2383(5) 0.4167(2) 0.1021(17) Uani 1 1 d . . .
H4A H 0.1093 0.2337 0.4470 0.153 Uiso 1 1 calc R . .
H4B H 0.0705 0.1963 0.4369 0.153 Uiso 1 1 calc R . .
H4C H 0.0802 0.3110 0.4135 0.153 Uiso 1 1 calc R . .
C5 C 0.05131(9) 0.2062(4) 0.2699(2) 0.0796(13) Uani 1 1 d . . .
H5A H 0.0466 0.2807 0.2636 0.119 Uiso 1 1 calc R . .
H5B H 0.0332 0.1737 0.2932 0.119 Uiso 1 1 calc R . .
H5C H 0.0523 0.1737 0.2238 0.119 Uiso 1 1 calc R . .
C6 C 0.10141(12) 0.0426(3) 0.3306(3) 0.1030(18) Uani 1 1 d . . .
H6A H 0.1017 0.0148 0.2830 0.155 Uiso 1 1 calc R . .
H6B H 0.0833 0.0086 0.3532 0.155 Uiso 1 1 calc R . .
H6C H 0.1234 0.0294 0.3583 0.155 Uiso 1 1 calc R . .
C7 C 0.25096(9) 0.2655(3) 0.3259(2) 0.0680(11) Uani 1 1 d . . .
H7A H 0.2412 0.2867 0.3685 0.102 Uiso 1 1 calc R . .
H7B H 0.2734 0.2976 0.3255 0.102 Uiso 1 1 calc R . .
H7C H 0.2533 0.1896 0.3254 0.102 Uiso 1 1 calc R . .
C8 C 0.23714(9) 0.2447(3) 0.1656(2) 0.0652(10) Uani 1 1 d . . .
H8A H 0.2346 0.1692 0.1691 0.098 Uiso 1 1 calc R . .
H8B H 0.2612 0.2618 0.1637 0.098 Uiso 1 1 calc R . .
H8C H 0.2236 0.2698 0.1227 0.098 Uiso 1 1 calc R . .
C9 C 0.22605(9) 0.4552(3) 0.2396(2) 0.0668(10) Uani 1 1 d . . .
H9A H 0.2136 0.4801 0.1955 0.100 Uiso 1 1 calc R . .
H9B H 0.2501 0.4739 0.2409 0.100 Uiso 1 1 calc R . .
H9C H 0.2166 0.4874 0.2796 0.100 Uiso 1 1 calc R . .
C10 C 0.17770(8) 0.1711(2) 0.35732(16) 0.0410(7) Uani 1 1 d . . .
C11 C 0.17952(9) 0.2059(3) 0.42721(17) 0.0499(8) Uani 1 1 d . . .
H11 H 0.1681 0.2680 0.4374 0.060 Uiso 1 1 calc R . .
C12 C 0.19815(9) 0.1499(3) 0.48325(18) 0.0541(9) Uani 1 1 d . . .
H12 H 0.1994 0.1760 0.5300 0.065 Uiso 1 1 calc R . .
C13 C 0.21482(9) 0.0557(3) 0.47007(18) 0.0517(8) Uani 1 1 d . . .
C14 C 0.21212(9) 0.0205(3) 0.40047(19) 0.0571(9) Uani 1 1 d . . .
H14 H 0.2227 -0.0433 0.3907 0.069 Uiso 1 1 calc R . .
C15 C 0.19426(9) 0.0764(3) 0.34406(18) 0.0511(8) Uani 1 1 d . . .
H15 H 0.1934 0.0505 0.2973 0.061 Uiso 1 1 calc R . .
C16 C 0.23539(10) -0.0049(3) 0.5299(2) 0.0705(11) Uani 1 1 d . . .
H16A H 0.2311 0.0260 0.5755 0.085 Uiso 1 1 calc R . .
H16B H 0.2271 -0.0776 0.5291 0.085 Uiso 1 1 calc R . .
C17 C 0.27240(13) -0.0058(5) 0.5258(3) 0.136(3) Uani 1 1 d . . .
H17A H 0.2769 -0.0317 0.4795 0.204 Uiso 1 1 calc R . .
H17B H 0.2835 -0.0512 0.5627 0.204 Uiso 1 1 calc R . .
H17C H 0.2814 0.0650 0.5325 0.204 Uiso 1 1 calc R . .
C18 C 0.06182(12) 0.5477(4) 0.0658(3) 0.0943(15) Uani 1 1 d . . .
H18A H 0.0864 0.5594 0.0677 0.141 Uiso 1 1 calc R . .
H18B H 0.0502 0.6145 0.0693 0.141 Uiso 1 1 calc R . .
H18C H 0.0535 0.5142 0.0210 0.141 Uiso 1 1 calc R . .
C19 C 0.05563(11) 0.5344(3) 0.2274(2) 0.0847(13) Uani 1 1 d . . .
H19A H 0.0582 0.4851 0.2668 0.127 Uiso 1 1 calc R . .
H19B H 0.0348 0.5752 0.2292 0.127 Uiso 1 1 calc R . .
H19C H 0.0753 0.5812 0.2309 0.127 Uiso 1 1 calc R . .
C20 C 0.00722(10) 0.4131(4) 0.1231(3) 0.0924(15) Uani 1 1 d . . .
H20A H 0.0042 0.3768 0.0777 0.139 Uiso 1 1 calc R . .
H20B H -0.0084 0.4725 0.1216 0.139 Uiso 1 1 calc R . .
H20C H 0.0022 0.3652 0.1605 0.139 Uiso 1 1 calc R . .
C21 C 0.14141(13) 0.1180(4) 0.0051(2) 0.0951(16) Uani 1 1 d . . .
H21A H 0.1227 0.1430 -0.0288 0.143 Uiso 1 1 calc R . .
H21B H 0.1511 0.0547 -0.0131 0.143 Uiso 1 1 calc R . .
H21C H 0.1591 0.1716 0.0123 0.143 Uiso 1 1 calc R . .
C22 C 0.16054(10) 0.0339(3) 0.1545(2) 0.0665(10) Uani 1 1 d . . .
H22A H 0.1789 0.0852 0.1620 0.100 Uiso 1 1 calc R . .
H22B H 0.1692 -0.0296 0.1344 0.100 Uiso 1 1 calc R . .
H22C H 0.1522 0.0176 0.1997 0.100 Uiso 1 1 calc R . .
C23 C 0.08982(13) -0.0128(4) 0.0791(3) 0.120(2) Uani 1 1 d . . .
H23A H 0.0803 -0.0241 0.1237 0.180 Uiso 1 1 calc R . .
H23B H 0.0993 -0.0782 0.0636 0.180 Uiso 1 1 calc R . .
H23C H 0.0718 0.0115 0.0433 0.180 Uiso 1 1 calc R . .
C24 C 0.05941(9) 0.2459(3) 0.04853(19) 0.0558(9) Uani 1 1 d . . .
C25 C 0.06594(11) 0.2846(3) -0.0173(2) 0.0706(11) Uani 1 1 d . . .
H25 H 0.0856 0.3256 -0.0207 0.085 Uiso 1 1 calc R . .
C26 C 0.04349(13) 0.2631(4) -0.0783(2) 0.0956(15) Uani 1 1 d . . .
H26 H 0.0484 0.2887 -0.1227 0.115 Uiso 1 1 calc R . .
C27 C 0.01350(14) 0.2031(4) -0.0739(3) 0.0993(16) Uani 1 1 d D . .
C28 C 0.00719(12) 0.1650(4) -0.0087(3) 0.0931(15) Uani 1 1 d . . .
H28 H -0.0126 0.1243 -0.0051 0.112 Uiso 1 1 calc R . .
C29 C 0.02982(11) 0.1861(4) 0.0521(2) 0.0784(12) Uani 1 1 d . . .
H29 H 0.0250 0.1595 0.0963 0.094 Uiso 1 1 calc R . .
C30 C -0.0126(2) 0.1817(5) -0.1441(3) 0.154(3) Uani 1 1 d D . .
H30A H -0.0366 0.1898 -0.1343 0.185 Uiso 1 1 calc R . .
H30B H -0.0083 0.2301 -0.1824 0.185 Uiso 1 1 calc R . .
C31 C -0.00583(19) 0.0761(7) -0.1628(3) 0.170(3) Uani 1 1 d D . .
H31A H -0.0193 0.0587 -0.2076 0.255 Uiso 1 1 calc R . .
H31B H -0.0120 0.0292 -0.1259 0.255 Uiso 1 1 calc R . .
H31C H 0.0184 0.0683 -0.1678 0.255 Uiso 1 1 calc R . .
C32 C 0.15069(10) 0.6576(3) 0.2230(2) 0.0643(10) Uani 1 1 d . . .
C33 C 0.15647(11) 0.7547(3) 0.2591(3) 0.0790(13) Uani 1 1 d . . .
H33 H 0.1608 0.8149 0.2328 0.095 Uiso 1 1 calc R . .
C34 C 0.15592(12) 0.7630(3) 0.3308(3) 0.0885(14) Uani 1 1 d . . .
H34 H 0.1600 0.8286 0.3530 0.106 Uiso 1 1 calc R . .
C35 C 0.14954(11) 0.6769(3) 0.3713(3) 0.0746(12) Uani 1 1 d . . .
H35 H 0.1496 0.6841 0.4207 0.090 Uiso 1 1 calc R . .
C36 C 0.14297(9) 0.5786(3) 0.3394(2) 0.0600(9) Uani 1 1 d . . .
C37 C 0.13455(13) 0.4851(3) 0.3837(2) 0.0791(12) Uani 1 1 d . . .
H37A H 0.1105 0.4668 0.3724 0.119 Uiso 1 1 calc R . .
H37B H 0.1390 0.5026 0.4339 0.119 Uiso 1 1 calc R . .
H37C H 0.1487 0.4258 0.3733 0.119 Uiso 1 1 calc R . .
C38 C 0.15261(12) 0.6501(3) 0.1444(2) 0.0852(13) Uani 1 1 d . . .
H38A H 0.1747 0.6212 0.1360 0.128 Uiso 1 1 calc R . .
H38B H 0.1499 0.7195 0.1234 0.128 Uiso 1 1 calc R . .
H38C H 0.1344 0.6046 0.1231 0.128 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 0.0415(3) 0.0414(3) 0.0398(3) 0.0051(2) 0.0040(2) -0.0006(2)
Cl1 0.0593(6) 0.0736(6) 0.0491(5) 0.0097(4) 0.0135(4) -0.0084(4)
Si1 0.0435(5) 0.0539(5) 0.0508(6) 0.0123(4) 0.0113(4) -0.0012(4)
Si2 0.0396(5) 0.0476(5) 0.0529(6) -0.0015(4) 0.0083(4) -0.0038(4)
Si3 0.0480(6) 0.0653(6) 0.0627(7) 0.0106(5) 0.0030(5) 0.0114(5)
Si4 0.0630(7) 0.0554(6) 0.0508(6) -0.0092(5) 0.0044(5) -0.0012(5)
N5 0.0354(14) 0.0415(14) 0.0392(14) 0.0049(11) 0.0065(11) 0.0006(10)
N2 0.0383(14) 0.0423(14) 0.0396(14) 0.0029(12) 0.0054(11) -0.0019(11)
N3 0.0429(15) 0.0496(15) 0.0447(15) 0.0072(13) 0.0031(12) 0.0014(12)
N4 0.0446(16) 0.0529(16) 0.0451(15) -0.0015(13) 0.0045(12) -0.0013(13)
N1 0.0472(16) 0.0406(15) 0.0507(16) 0.0056(12) 0.0031(12) 0.0000(11)
C3 0.0446(19) 0.0356(16) 0.0368(17) -0.0015(13) 0.0052(14) 0.0017(13)
C2 0.045(2) 0.060(2) 0.0411(18) 0.0069(16) 0.0061(15) -0.0074(16)
C1 0.045(2) 0.0376(18) 0.076(3) 0.0024(18) 0.0038(17) 0.0025(14)
C4 0.087(3) 0.157(5) 0.069(3) -0.014(3) 0.040(3) -0.039(3)
C5 0.050(2) 0.107(3) 0.082(3) 0.035(3) 0.007(2) -0.009(2)
C6 0.078(3) 0.066(3) 0.172(5) 0.042(3) 0.044(3) 0.001(2)
C7 0.038(2) 0.085(3) 0.079(3) 0.011(2) -0.0028(18) -0.0080(18)
C8 0.057(2) 0.069(2) 0.074(3) -0.011(2) 0.023(2) 0.0008(18)
C9 0.055(2) 0.054(2) 0.093(3) -0.002(2) 0.017(2) -0.0138(17)
C10 0.0384(17) 0.0424(18) 0.0425(18) 0.0037(14) 0.0053(14) 0.0005(13)
C11 0.054(2) 0.0478(19) 0.047(2) 0.0020(16) 0.0045(16) 0.0076(15)
C12 0.060(2) 0.063(2) 0.0390(18) 0.0028(16) 0.0030(16) 0.0035(17)
C13 0.049(2) 0.058(2) 0.048(2) 0.0116(17) 0.0057(16) 0.0054(16)
C14 0.061(2) 0.0453(19) 0.065(2) 0.0075(17) 0.0076(19) 0.0151(16)
C15 0.058(2) 0.0500(19) 0.0449(19) 0.0010(16) 0.0044(16) 0.0086(16)
C16 0.066(3) 0.083(3) 0.061(2) 0.020(2) 0.002(2) 0.019(2)
C17 0.077(4) 0.235(7) 0.094(4) 0.045(4) 0.003(3) 0.063(4)
C18 0.094(3) 0.087(3) 0.101(4) 0.041(3) 0.012(3) 0.019(3)
C19 0.066(3) 0.089(3) 0.100(3) -0.016(3) 0.011(2) 0.028(2)
C20 0.047(2) 0.105(4) 0.121(4) 0.006(3) -0.005(2) 0.012(2)
C21 0.126(4) 0.109(4) 0.053(2) 0.002(2) 0.021(3) 0.049(3)
C22 0.085(3) 0.053(2) 0.061(2) -0.0009(18) 0.008(2) 0.0079(19)
C23 0.082(4) 0.090(3) 0.187(6) -0.063(4) 0.008(4) -0.021(3)
C24 0.052(2) 0.067(2) 0.046(2) -0.0005(17) -0.0006(16) -0.0051(17)
C25 0.068(3) 0.088(3) 0.053(2) 0.011(2) -0.006(2) -0.009(2)
C26 0.102(4) 0.130(4) 0.051(3) 0.017(3) -0.011(3) -0.007(3)
C27 0.088(4) 0.127(4) 0.074(3) -0.009(3) -0.030(3) -0.020(3)
C28 0.064(3) 0.133(4) 0.077(3) -0.004(3) -0.014(2) -0.027(3)
C29 0.063(3) 0.108(3) 0.061(3) 0.001(2) -0.003(2) -0.024(2)
C30 0.228(9) 0.121(5) 0.114(5) -0.043(4) 0.027(5) -0.057(5)
C31 0.142(6) 0.255(10) 0.106(5) -0.009(6) -0.021(4) -0.020(6)
C32 0.059(2) 0.047(2) 0.086(3) 0.008(2) 0.008(2) 0.0033(17)
C33 0.081(3) 0.042(2) 0.116(4) 0.006(2) 0.021(3) -0.0002(19)
C34 0.090(3) 0.053(3) 0.125(4) -0.026(3) 0.023(3) -0.005(2)
C35 0.084(3) 0.052(2) 0.090(3) -0.018(2) 0.014(2) 0.0023(19)
C36 0.058(2) 0.052(2) 0.070(3) -0.0110(19) 0.0061(19) 0.0054(16)
C37 0.122(4) 0.055(2) 0.061(2) -0.002(2) 0.012(2) 0.002(2)
C38 0.098(3) 0.056(2) 0.101(4) 0.027(2) 0.010(3) -0.009(2)

_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 N1 1.665(3) . ?
V1 N3 1.970(3) . ?
V1 N2 2.110(2) . ?
V1 N5 2.123(2) . ?
V1 N4 2.283(3) . ?
V1 Cl1 2.3112(11) . ?
V1 C2 2.493(3) . ?
V1 C3 2.524(3) . ?
Si1 N5 1.752(2) . ?
Si1 C5 1.843(4) . ?
Si1 C4 1.854(4) . ?
Si1 C6 1.860(4) . ?
Si2 N2 1.754(3) . ?
Si2 C8 1.849(4) . ?
Si2 C9 1.852(3) . ?
Si2 C7 1.863(4) . ?
Si3 N3 1.762(3) . ?
Si3 C19 1.848(4) . ?
Si3 C18 1.855(4) . ?
Si3 C20 1.861(4) . ?
Si4 N4 1.749(3) . ?
Si4 C22 1.841(4) . ?
Si4 C23 1.853(4) . ?
Si4 C21 1.859(4) . ?
N5 C3 1.340(4) . ?
N2 C3 1.318(4) . ?
N3 C2 1.366(4) . ?
N4 C2 1.302(4) . ?
N1 C1 1.400(4) . ?
C3 C10 1.498(4) . ?
C2 C24 1.492(5) . ?
C1 C32 1.398(5) . ?
C1 C36 1.409(5) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 C11 1.373(4) . ?
C10 C15 1.391(4) . ?
C11 C12 1.395(4) . ?
C11 H11 0.9300 . ?
C12 C13 1.386(5) . ?
C12 H12 0.9300 . ?
C13 C14 1.369(5) . ?
C13 C16 1.505(5) . ?
C14 C15 1.386(4) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 C17 1.445(6) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 C25 1.375(5) . ?
C24 C29 1.380(5) . ?
C25 C26 1.381(6) . ?
C25 H25 0.9300 . ?
C26 C27 1.396(6) . ?
C26 H26 0.9300 . ?
C27 C28 1.358(6) . ?
C27 C30 1.588(6) . ?
C28 C29 1.381(6) . ?
C28 H28 0.9300 . ?
C29 H29 0.9300 . ?
C30 C31 1.409(9) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 C33 1.402(5) . ?
C32 C38 1.484(6) . ?
C33 C34 1.350(6) . ?
C33 H33 0.9300 . ?
C34 C35 1.361(6) . ?
C34 H34 0.9300 . ?
C35 C36 1.385(5) . ?
C35 H35 0.9300 . ?
C36 C37 1.498(5) . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 V1 N3 101.31(12) . . ?
N1 V1 N2 97.22(11) . . ?
N3 V1 N2 156.81(10) . . ?
N1 V1 N5 101.29(11) . . ?
N3 V1 N5 98.97(10) . . ?
N2 V1 N5 63.51(9) . . ?
N1 V1 N4 164.83(11) . . ?
N3 V1 N4 63.58(10) . . ?
N2 V1 N4 97.78(10) . . ?
N5 V1 N4 83.43(9) . . ?
N1 V1 Cl1 98.30(9) . . ?
N3 V1 Cl1 98.64(8) . . ?
N2 V1 Cl1 92.30(7) . . ?
N5 V1 Cl1 150.43(7) . . ?
N4 V1 Cl1 83.40(7) . . ?
N1 V1 C2 133.60(12) . . ?
N3 V1 C2 33.08(11) . . ?
N2 V1 C2 128.92(11) . . ?
N5 V1 C2 96.18(10) . . ?
N4 V1 C2 31.26(10) . . ?
Cl1 V1 C2 85.93(8) . . ?
N1 V1 C3 100.56(11) . . ?
N3 V1 C3 129.61(10) . . ?
N2 V1 C3 31.45(9) . . ?
N5 V1 C3 32.06(9) . . ?
N4 V1 C3 91.08(10) . . ?
Cl1 V1 C3 122.18(7) . . ?
C2 V1 C3 116.07(10) . . ?
N5 Si1 C5 109.60(15) . . ?
N5 Si1 C4 113.05(17) . . ?
C5 Si1 C4 106.8(2) . . ?
N5 Si1 C6 111.43(16) . . ?
C5 Si1 C6 106.5(2) . . ?
C4 Si1 C6 109.1(3) . . ?
N2 Si2 C8 109.82(15) . . ?
N2 Si2 C9 107.32(14) . . ?
C8 Si2 C9 110.67(18) . . ?
N2 Si2 C7 114.50(15) . . ?
C8 Si2 C7 107.73(18) . . ?
C9 Si2 C7 106.77(18) . . ?
N3 Si3 C19 107.45(16) . . ?
N3 Si3 C18 110.19(17) . . ?
C19 Si3 C18 111.8(2) . . ?
N3 Si3 C20 113.12(17) . . ?
C19 Si3 C20 106.4(2) . . ?
C18 Si3 C20 107.8(2) . . ?
N4 Si4 C22 106.11(15) . . ?
N4 Si4 C23 112.30(19) . . ?
C22 Si4 C23 108.2(2) . . ?
N4 Si4 C21 111.44(17) . . ?
C22 Si4 C21 108.5(2) . . ?
C23 Si4 C21 110.1(3) . . ?
C3 N5 Si1 127.3(2) . . ?
C3 N5 V1 90.69(17) . . ?
Si1 N5 V1 139.91(14) . . ?
C3 N2 Si2 133.7(2) . . ?
C3 N2 V1 91.88(18) . . ?
Si2 N2 V1 131.56(13) . . ?
C2 N3 Si3 128.9(2) . . ?
C2 N3 V1 95.00(19) . . ?
Si3 N3 V1 132.90(15) . . ?
C2 N4 Si4 129.8(2) . . ?
C2 N4 V1 83.3(2) . . ?
Si4 N4 V1 141.79(15) . . ?
C1 N1 V1 177.2(2) . . ?
N2 C3 N5 113.9(3) . . ?
N2 C3 C10 122.1(3) . . ?
N5 C3 C10 124.0(3) . . ?
N2 C3 V1 56.66(15) . . ?
N5 C3 V1 57.25(14) . . ?
C10 C3 V1 177.6(2) . . ?
N4 C2 N3 115.4(3) . . ?
N4 C2 C24 123.3(3) . . ?
N3 C2 C24 121.0(3) . . ?
N4 C2 V1 65.43(18) . . ?
N3 C2 V1 51.92(15) . . ?
C24 C2 V1 160.6(2) . . ?
C32 C1 N1 120.5(3) . . ?
C32 C1 C36 121.1(3) . . ?
N1 C1 C36 118.4(3) . . ?
Si1 C4 H4A 109.5 . . ?
Si1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
Si1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
Si1 C5 H5A 109.5 . . ?
Si1 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
Si1 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
Si1 C6 H6A 109.5 . . ?
Si1 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
Si1 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Si2 C7 H7A 109.5 . . ?
Si2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
Si2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
Si2 C8 H8A 109.5 . . ?
Si2 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
Si2 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
Si2 C9 H9A 109.5 . . ?
Si2 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
Si2 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C11 C10 C15 118.0(3) . . ?
C11 C10 C3 121.6(3) . . ?
C15 C10 C3 120.3(3) . . ?
C10 C11 C12 121.4(3) . . ?
C10 C11 H11 119.3 . . ?
C12 C11 H11 119.3 . . ?
C13 C12 C11 120.7(3) . . ?
C13 C12 H12 119.6 . . ?
C11 C12 H12 119.6 . . ?
C14 C13 C12 117.4(3) . . ?
C14 C13 C16 121.3(3) . . ?
C12 C13 C16 121.3(3) . . ?
C13 C14 C15 122.5(3) . . ?
C13 C14 H14 118.7 . . ?
C15 C14 H14 118.7 . . ?
C14 C15 C10 120.0(3) . . ?
C14 C15 H15 120.0 . . ?
C10 C15 H15 120.0 . . ?
C17 C16 C13 114.1(4) . . ?
C17 C16 H16A 108.7 . . ?
C13 C16 H16A 108.7 . . ?
C17 C16 H16B 108.7 . . ?
C13 C16 H16B 108.7 . . ?
H16A C16 H16B 107.6 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
Si3 C18 H18A 109.5 . . ?
Si3 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
Si3 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
Si3 C19 H19A 109.5 . . ?
Si3 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
Si3 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
Si3 C20 H20A 109.5 . . ?
Si3 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
Si3 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
Si4 C21 H21A 109.5 . . ?
Si4 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
Si4 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
Si4 C22 H22A 109.5 . . ?
Si4 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
Si4 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
Si4 C23 H23A 109.5 . . ?
Si4 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
Si4 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C25 C24 C29 118.5(3) . . ?
C25 C24 C2 119.7(3) . . ?
C29 C24 C2 121.8(3) . . ?
C24 C25 C26 120.6(4) . . ?
C24 C25 H25 119.7 . . ?
C26 C25 H25 119.7 . . ?
C25 C26 C27 120.4(4) . . ?
C25 C26 H26 119.8 . . ?
C27 C26 H26 119.8 . . ?
C28 C27 C26 118.8(4) . . ?
C28 C27 C30 121.3(5) . . ?
C26 C27 C30 119.9(5) . . ?
C27 C28 C29 120.7(4) . . ?
C27 C28 H28 119.7 . . ?
C29 C28 H28 119.7 . . ?
C24 C29 C28 121.1(4) . . ?
C24 C29 H29 119.4 . . ?
C28 C29 H29 119.4 . . ?
C31 C30 C27 104.2(6) . . ?
C31 C30 H30A 110.9 . . ?
C27 C30 H30A 110.9 . . ?
C31 C30 H30B 110.9 . . ?
C27 C30 H30B 110.9 . . ?
H30A C30 H30B 108.9 . . ?
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 . . ?
C1 C32 C33 117.0(4) . . ?
C1 C32 C38 122.4(4) . . ?
C33 C32 C38 120.6(4) . . ?
C34 C33 C32 121.8(4) . . ?
C34 C33 H33 119.1 . . ?
C32 C33 H33 119.1 . . ?
C33 C34 C35 121.0(4) . . ?
C33 C34 H34 119.5 . . ?
C35 C34 H34 119.5 . . ?
C34 C35 C36 120.6(4) . . ?
C34 C35 H35 119.7 . . ?
C36 C35 H35 119.7 . . ?
C35 C36 C1 118.5(4) . . ?
C35 C36 C37 120.4(4) . . ?
C1 C36 C37 121.1(3) . . ?
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 . . ?
C32 C38 H38A 109.5 . . ?
C32 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C32 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        25.33
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         0.563
_refine_diff_density_min         -0.432
_refine_diff_density_rms         0.053

# Attachment 'complex_6.cif'

#Mono- and bis-amidinate 2,6-xylylimido vanadium chlorides: synthesis, structure, and reactivity.
#Sinai Aharonovich, Mark Botoshanski, Boris Tumanskii, Kotohiro Nomura, Robert M. Waymouth and Moris S. Eisen

data_complex6
_database_code_depnum_ccdc_archive 'CCDC 757623'
#TrackingRef 'complex_6.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            complex6
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C14 H25 Cl2 N3 V'
_chemical_formula_weight         357.21

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
V V 0.3005 0.5294 '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'
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'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P -1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.030(2)
_cell_length_b                   10.717(2)
_cell_length_c                   11.823(2)
_cell_angle_alpha                116.28(3)
_cell_angle_beta                 93.83(2)
_cell_angle_gamma                104.50(3)
_cell_volume                     864.5(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    230(1)
_cell_measurement_reflns_used    5169
_cell_measurement_theta_min      1.96
_cell_measurement_theta_max      25.02

_exptl_crystal_description       plate
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.01
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.375
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             374
_exptl_absorpt_coefficient_mu    0.879
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.915
_exptl_absorpt_correction_T_max  0.995
_exptl_absorpt_process_details   
;
multi-scan from symmetry-related measurements
Sortav (Blessing 1995)
;
_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      230(1)
_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  'Nonius KappaCCD'
_diffrn_measurement_method       phi-scan
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5142
_diffrn_reflns_av_R_equivalents  0.0746
_diffrn_reflns_av_sigmaI/netI    0.1028
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.96
_diffrn_reflns_theta_max         25.02
_reflns_number_total             2822
_reflns_number_gt                1718
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect (Nonius, 2006)'
_computing_cell_refinement       'DENZO HKL2000 (Otwinowski & Minor 1997)'
_computing_data_reduction        'DENZO HKL2000 (Otwinowski & Minor 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'TEXSAN (MSC, 1999)'
_computing_publication_material  ?

_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^)+(0.0769P)^2^+0.0000P] 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         2822
_refine_ls_number_parameters     175
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1599
_refine_ls_R_factor_gt           0.1115
_refine_ls_wR_factor_ref         0.2711
_refine_ls_wR_factor_gt          0.2598
_refine_ls_goodness_of_fit_ref   1.671
_refine_ls_restrained_S_all      1.671
_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 1.0114(2) 0.11645(17) 0.81044(16) 0.0447(5) Uani 1 1 d . . .
Cl1 Cl 1.2069(4) 0.2310(3) 1.0079(3) 0.0700(9) Uani 1 1 d . . .
Cl2 Cl 1.1830(3) -0.0322(3) 0.7109(3) 0.0663(8) Uani 1 1 d . . .
N1 N 1.0435(10) 0.2357(8) 0.7541(7) 0.0469(19) Uani 1 1 d . . .
N2 N 0.7787(10) -0.0744(9) 0.6789(7) 0.052(2) Uani 1 1 d . . .
N3 N 0.8063(10) 0.1703(8) 0.9182(7) 0.050(2) Uani 1 1 d . . .
C1 C 1.1131(12) 0.3497(9) 0.7237(8) 0.045(2) Uani 1 1 d . . .
C2 C 1.0003(14) 0.3995(11) 0.6708(9) 0.053(3) Uani 1 1 d . . .
C3 C 1.0771(16) 0.5165(12) 0.6493(10) 0.065(3) Uani 1 1 d . . .
H3 H 1.0041 0.5529 0.6150 0.078 Uiso 1 1 calc R . .
C4 C 1.2559(19) 0.5808(12) 0.6765(11) 0.075(3) Uani 1 1 d . . .
H4 H 1.3031 0.6612 0.6625 0.090 Uiso 1 1 calc R . .
C5 C 1.3674(17) 0.5270(11) 0.7248(10) 0.067(3) Uani 1 1 d . . .
H5 H 1.4899 0.5690 0.7410 0.080 Uiso 1 1 calc R . .
C6 C 1.2982(12) 0.4136(9) 0.7483(9) 0.048(2) Uani 1 1 d . . .
C7 C 0.8074(15) 0.3344(13) 0.6359(12) 0.072(3) Uani 1 1 d . . .
H7A H 0.7570 0.3845 0.5986 0.107 Uiso 1 1 calc R . .
H7B H 0.7619 0.3445 0.7124 0.107 Uiso 1 1 calc R . .
H7C H 0.7763 0.2314 0.5736 0.107 Uiso 1 1 calc R . .
C8 C 1.4175(12) 0.3646(12) 0.8117(11) 0.066(3) Uani 1 1 d . . .
H8A H 1.3483 0.2825 0.8208 0.099 Uiso 1 1 calc R . .
H8B H 1.4789 0.4448 0.8962 0.099 Uiso 1 1 calc R . .
H8C H 1.5022 0.3348 0.7592 0.099 Uiso 1 1 calc R . .
C9 C 0.6211(15) -0.0504(13) 0.7341(12) 0.092(3) Uani 1 1 d . . .
H9A H 0.5220 -0.0850 0.6633 0.110 Uiso 1 1 calc R . .
H9B H 0.5913 -0.1101 0.7774 0.110 Uiso 1 1 calc R . .
C10 C 0.6410(15) 0.0950(14) 0.8217(13) 0.092(3) Uani 1 1 d . . .
H10A H 0.5425 0.0972 0.8664 0.110 Uiso 1 1 calc R . .
H10B H 0.6351 0.1491 0.7737 0.110 Uiso 1 1 calc R . .
C11 C 0.7843(17) -0.2209(11) 0.6580(12) 0.077(3) Uani 1 1 d . . .
H11A H 0.8885 -0.2382 0.6253 0.115 Uiso 1 1 calc R . .
H11B H 0.6805 -0.2961 0.5960 0.115 Uiso 1 1 calc R . .
H11C H 0.7877 -0.2237 0.7390 0.115 Uiso 1 1 calc R . .
C13 C 0.8292(16) 0.3301(11) 0.9779(11) 0.068(3) Uani 1 1 d . . .
H13A H 0.8316 0.3602 0.9116 0.102 Uiso 1 1 calc R . .
H13B H 0.9388 0.3844 1.0410 0.102 Uiso 1 1 calc R . .
H13C H 0.7321 0.3498 1.0200 0.102 Uiso 1 1 calc R . .
C12 C 0.7567(18) -0.0790(12) 0.5520(9) 0.077(4) Uani 1 1 d . . .
H12A H 0.8622 -0.0877 0.5178 0.115 Uiso 1 1 calc R . .
H12B H 0.7364 0.0102 0.5614 0.115 Uiso 1 1 calc R . .
H12C H 0.6572 -0.1627 0.4933 0.115 Uiso 1 1 calc R . .
C14 C 0.7983(19) 0.1262(14) 1.0216(12) 0.080(4) Uani 1 1 d . . .
H14A H 0.9091 0.1771 1.0836 0.121 Uiso 1 1 calc R . .
H14B H 0.7767 0.0213 0.9837 0.121 Uiso 1 1 calc R . .
H14C H 0.7039 0.1516 1.0648 0.121 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 0.0335(9) 0.0493(10) 0.0496(10) 0.0233(8) 0.0038(7) 0.0117(7)
Cl1 0.0567(17) 0.0764(18) 0.0620(17) 0.0348(14) -0.0117(13) -0.0003(13)
Cl2 0.0409(14) 0.0642(16) 0.094(2) 0.0335(15) 0.0130(14) 0.0240(12)
N1 0.034(4) 0.051(4) 0.060(5) 0.028(4) 0.011(4) 0.016(3)
N2 0.030(4) 0.064(5) 0.051(5) 0.018(4) 0.006(4) 0.018(4)
N3 0.038(4) 0.050(4) 0.049(5) 0.014(4) 0.006(4) 0.009(3)
C1 0.050(6) 0.040(5) 0.044(5) 0.017(4) 0.009(4) 0.019(4)
C2 0.063(7) 0.059(6) 0.045(6) 0.028(5) 0.012(5) 0.029(5)
C3 0.077(9) 0.066(7) 0.058(7) 0.035(6) 0.012(6) 0.025(6)
C4 0.098(10) 0.059(7) 0.066(8) 0.033(6) 0.019(7) 0.012(7)
C5 0.087(9) 0.053(6) 0.054(7) 0.024(5) 0.020(6) 0.013(6)
C6 0.038(5) 0.037(5) 0.062(6) 0.018(4) 0.011(5) 0.008(4)
C7 0.054(7) 0.086(8) 0.086(8) 0.045(7) 0.012(6) 0.032(6)
C8 0.026(5) 0.079(7) 0.083(8) 0.035(6) 0.003(5) 0.008(5)
C9 0.038(5) 0.104(7) 0.077(6) -0.005(5) 0.003(4) 0.025(5)
C10 0.038(5) 0.104(7) 0.077(6) -0.005(5) 0.003(4) 0.025(5)
C11 0.084(9) 0.051(6) 0.095(9) 0.041(6) 0.015(7) 0.009(6)
C13 0.089(9) 0.057(6) 0.068(7) 0.028(5) 0.029(6) 0.038(6)
C12 0.107(10) 0.072(7) 0.033(6) 0.008(5) -0.009(6) 0.038(7)
C14 0.107(11) 0.086(8) 0.075(8) 0.054(7) 0.038(8) 0.036(8)

_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 N1 1.659(8) . ?
V1 N3 2.185(8) . ?
V1 N2 2.230(8) . ?
V1 Cl1 2.330(3) . ?
V1 Cl2 2.340(3) . ?
N1 C1 1.418(11) . ?
N2 C12 1.477(13) . ?
N2 C11 1.490(12) . ?
N2 C9 1.489(13) . ?
N3 C10 1.470(13) . ?
N3 C13 1.490(12) . ?
N3 C14 1.493(13) . ?
C1 C2 1.400(12) . ?
C1 C6 1.421(13) . ?
C2 C3 1.391(14) . ?
C2 C7 1.475(15) . ?
C3 C4 1.373(17) . ?
C3 H3 0.9400 . ?
C4 C5 1.394(17) . ?
C4 H4 0.9400 . ?
C5 C6 1.358(13) . ?
C5 H5 0.9400 . ?
C6 C8 1.504(14) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 H7C 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 H8C 0.9700 . ?
C9 C10 1.396(16) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 H11C 0.9700 . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 H13C 0.9700 . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C12 H12C 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 H14C 0.9700 . ?

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
N1 V1 N3 101.0(3) . . ?
N1 V1 N2 107.4(3) . . ?
N3 V1 N2 79.6(3) . . ?
N1 V1 Cl1 106.4(3) . . ?
N3 V1 Cl1 87.6(2) . . ?
N2 V1 Cl1 145.5(2) . . ?
N1 V1 Cl2 104.3(3) . . ?
N3 V1 Cl2 153.9(2) . . ?
N2 V1 Cl2 86.6(2) . . ?
Cl1 V1 Cl2 91.51(12) . . ?
C1 N1 V1 166.0(7) . . ?
C12 N2 C11 107.8(8) . . ?
C12 N2 C9 108.8(9) . . ?
C11 N2 C9 107.4(9) . . ?
C12 N2 V1 108.6(7) . . ?
C11 N2 V1 116.2(6) . . ?
C9 N2 V1 107.8(6) . . ?
C10 N3 C13 106.8(9) . . ?
C10 N3 C14 111.3(10) . . ?
C13 N3 C14 108.4(8) . . ?
C10 N3 V1 105.5(6) . . ?
C13 N3 V1 111.3(6) . . ?
C14 N3 V1 113.5(7) . . ?
C2 C1 N1 120.2(9) . . ?
C2 C1 C6 120.4(9) . . ?
N1 C1 C6 119.4(8) . . ?
C3 C2 C1 117.2(10) . . ?
C3 C2 C7 118.8(9) . . ?
C1 C2 C7 123.9(9) . . ?
C4 C3 C2 122.3(10) . . ?
C4 C3 H3 118.9 . . ?
C2 C3 H3 118.9 . . ?
C3 C4 C5 120.1(11) . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
C6 C5 C4 119.7(12) . . ?
C6 C5 H5 120.2 . . ?
C4 C5 H5 120.2 . . ?
C5 C6 C1 120.3(9) . . ?
C5 C6 C8 119.7(9) . . ?
C1 C6 C8 119.7(8) . . ?
C2 C7 H7A 109.5 . . ?
C2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C6 C8 H8A 109.5 . . ?
C6 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C6 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C10 C9 N2 114.7(11) . . ?
C10 C9 H9A 108.6 . . ?
N2 C9 H9A 108.6 . . ?
C10 C9 H9B 108.6 . . ?
N2 C9 H9B 108.6 . . ?
H9A C9 H9B 107.6 . . ?
C9 C10 N3 114.2(10) . . ?
C9 C10 H10A 108.7 . . ?
N3 C10 H10A 108.7 . . ?
C9 C10 H10B 108.7 . . ?
N3 C10 H10B 108.7 . . ?
H10A C10 H10B 107.6 . . ?
N2 C11 H11A 109.5 . . ?
N2 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N2 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N3 C13 H13A 109.5 . . ?
N3 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
N3 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N2 C12 H12A 109.5 . . ?
N2 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N2 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N3 C14 H14A 109.5 . . ?
N3 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
N3 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?

loop_
# start Validation Reply Form
_vrf_PLAT029_complex6
;
PROBLEM: _diffrn_measured_fraction_theta_full Low .0.92
RESPONSE: Low diffracted unstable crystals
;
_vrf_PLAT241_complex6            
;
PROBLEM: Check High Ueq as Compared to Neighbors for C55
RESPONSE: Partly disordered TMEDA moiety
;
_vrf_PLAT242_complex6            
;
PROBLEM: Check Low Ueq as Compared to Neighbors for Si3
RESPONSE: Partly disordered TMEDA moiety
;
_vrf_REFLT03_complex6            
;
PROBLEM: Reflection count < 95% complete
RESPONSE: Low diffracted unstable crystals
;
_vrf_RFACG01_complex6            
;
PROBLEM: The value of the R factor is > 0.10
RESPONSE: twinning of the crystal
;
_vrf_RFACR01_complex6            
;
PROBLEM: The value of the R factor is > 0.10
RESPONSE: twinning of the crystal
;
_vrf_PLAT360_complex6            
;
PROBLEM: Short C(sp3)-C(sp3) Bond C9 - C10 ... 1.40 Ang.
RESPONSE: Partly disordered TMEDA moiety
;

# end Validation Reply Form

_diffrn_measured_fraction_theta_max 0.923
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.923
_refine_diff_density_max         0.890
_refine_diff_density_min         -0.561
_refine_diff_density_rms         0.138

# END