#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:33:25 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179116 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/78/4307891.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4307891
loop_
_publ_author_name
'Christian Lorber'
'Robert Choukroun'
'Laure Vendier'
_publ_contact_author
;
Christian Lorber
;
_publ_contact_author_address
;
Laboratoire de Chimie de Coordination
205 Route de Narbonne
31077 Toulouse Cedex 04
;
_publ_contact_author_email       lorber@lcc-toulouse.fr
_publ_section_title
;
Reaction of p-Toluenesulfonylamide and M(NMe2)4 (M = Ti, V): Generation of
Electron-Deficient Imido Complexes of Early Transition Metals
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3192
_journal_page_last               3202
_journal_paper_doi               10.1021/ic062404j
_journal_volume                  46
_journal_year                    2007
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C30 H30 Cl4 N6 O V2'
_chemical_formula_sum            'C30 H30 Cl4 N6 O V2'
_chemical_formula_weight         734.28
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                98.44(3)
_cell_angle_beta                 96.79(3)
_cell_angle_gamma                98.97(3)
_cell_formula_units_Z            4
_cell_length_a                   15.306(3)
_cell_length_b                   15.806(3)
_cell_length_c                   16.916(3)
_cell_measurement_reflns_used    4000
_cell_measurement_temperature    180
_cell_measurement_theta_max      26.05
_cell_measurement_theta_min      1.65
_cell_measurement_wavelength     0.71073
_cell_volume                     3956.7(14)
_computing_cell_refinement       'Stoe IPDS software (Stoe, 1996)'
_computing_data_collection       'Stoe IPDS software (Stoe, 1996)'
_computing_data_reduction        'XRED (Stoe, 1.08, 1996)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      180
_diffrn_measured_fraction_theta_full 0.919
_diffrn_measured_fraction_theta_max 0.919
_diffrn_measurement_device       'Stoe IPDS'
_diffrn_measurement_method       φ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0
_diffrn_reflns_av_unetI/netI     0.7025
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            15915
_diffrn_reflns_theta_full        26.22
_diffrn_reflns_theta_max         26.22
_diffrn_reflns_theta_min         1.96
_diffrn_standards_decay_%        0.1
_diffrn_standards_interval_time  4
_diffrn_standards_number         200
_exptl_absorpt_coefficient_mu    0.771
_exptl_absorpt_correction_T_max  0.955
_exptl_absorpt_correction_T_min  0.861
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
        (See: Walker, N. & Stuart, D. (1983) Acta Cryst. A39, 158-166)
;
_exptl_crystal_colour            'yellow orange'
_exptl_crystal_density_diffrn    1.233
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.195
_refine_diff_density_min         -0.599
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.679
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     776
_refine_ls_number_reflns         15915
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      0.679
_refine_ls_R_factor_all          0.3463
_refine_ls_R_factor_gt           0.1096
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0462P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1953
_refine_ls_wR_factor_ref         0.2596
_reflns_number_gt                7033
_reflns_number_total             15915
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            ic062404jsi20061215_111655_1.cif
_cod_data_source_block           (8)
_cod_original_cell_volume        3956.8(14)
_cod_database_code               4307891
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
C1 C 0.2884(6) 0.1290(6) 0.0596(6) 0.032(2) Uani 1 1 d . . .
H1 H 0.3359 0.1351 0.101 0.039 Uiso 1 1 calc R . .
C2 C 0.3096(8) 0.1406(8) -0.0159(7) 0.063(4) Uani 1 1 d . . .
H2 H 0.3678 0.1557 -0.0262 0.076 Uiso 1 1 calc R . .
C3 C 0.2339(8) 0.1273(9) -0.0757(7) 0.063(4) Uani 1 1 d . . .
H3 H 0.2417 0.1354 -0.128 0.075 Uiso 1 1 calc R . .
C4 C 0.1546(9) 0.1042(9) -0.0596(7) 0.074(4) Uani 1 1 d . . .
H4 H 0.1059 0.0931 -0.1005 0.088 Uiso 1 1 calc R . .
C5 C 0.1413(7) 0.0958(7) 0.0208(7) 0.047(3) Uani 1 1 d . . .
H5 H 0.0834 0.0794 0.0316 0.056 Uiso 1 1 calc R . .
C6 C 0.0933(6) 0.2533(7) 0.1588(5) 0.035(3) Uani 1 1 d . . .
H6 H 0.1403 0.2637 0.1293 0.042 Uiso 1 1 calc R . .
C7 C 0.0345(7) 0.3090(7) 0.1615(6) 0.048(3) Uani 1 1 d . . .
H7 H 0.0436 0.3579 0.1369 0.058 Uiso 1 1 calc R . .
C8 C -0.0370(8) 0.2938(8) 0.1997(6) 0.049(3) Uani 1 1 d . . .
H8 H -0.0786 0.3308 0.2007 0.059 Uiso 1 1 calc R . .
C9 C -0.0474(7) 0.2191(8) 0.2389(6) 0.054(3) Uani 1 1 d . . .
H9 H -0.0946 0.2071 0.2678 0.065 Uiso 1 1 calc R . .
C10 C 0.0135(7) 0.1677(8) 0.2322(7) 0.052(3) Uani 1 1 d . . .
H10 H 0.0045 0.1168 0.2539 0.063 Uiso 1 1 calc R . .
C11 C 0.1705(7) 0.1626(7) 0.3824(7) 0.050(3) Uani 1 1 d . . .
H11 H 0.1718 0.2156 0.3644 0.06 Uiso 1 1 calc R . .
C12 C 0.1657(7) 0.1616(8) 0.4637(7) 0.054(3) Uani 1 1 d . . .
H12 H 0.1691 0.2127 0.4998 0.065 Uiso 1 1 calc R . .
C13 C 0.1557(8) 0.0819(9) 0.4891(7) 0.065(4) Uani 1 1 d . . .
H13 H 0.1453 0.078 0.5416 0.078 Uiso 1 1 calc R . .
C14 C 0.1614(8) 0.0035(9) 0.4329(6) 0.067(4) Uani 1 1 d . . .
H14 H 0.1654 -0.0488 0.451 0.08 Uiso 1 1 calc R . .
C15 C 0.1605(7) 0.0102(8) 0.3503(7) 0.054(3) Uani 1 1 d U . .
H15 H 0.1514 -0.0397 0.3115 0.065 Uiso 1 1 calc R . .
C16 C 0.2393(6) -0.1004(7) 0.0555(6) 0.049(3) Uani 1 1 d . . .
H16 H 0.198 -0.0968 0.0914 0.059 Uiso 1 1 calc R . .
C17 C 0.2079(9) -0.1302(8) -0.0271(7) 0.069(4) Uani 1 1 d . . .
H17 H 0.148 -0.1524 -0.0461 0.083 Uiso 1 1 calc R . .
C18 C 0.2740(9) -0.1239(8) -0.0795(7) 0.063(4) Uani 1 1 d . . .
H18 H 0.2565 -0.139 -0.135 0.076 Uiso 1 1 calc R . .
C19 C 0.3618(10) -0.0963(9) -0.0505(7) 0.074(4) Uani 1 1 d . . .
H19 H 0.4047 -0.0918 -0.0849 0.088 Uiso 1 1 calc R . .
C20 C 0.3849(8) -0.0754(7) 0.0318(7) 0.049(3) Uani 1 1 d . . .
H20 H 0.445 -0.0589 0.053 0.059 Uiso 1 1 calc R . .
C21 C 0.4525(6) -0.1957(7) 0.1693(6) 0.043(3) Uani 1 1 d . . .
H21 H 0.3974 -0.2167 0.1376 0.051 Uiso 1 1 calc R . .
C22 C 0.5146(7) -0.2465(7) 0.1676(6) 0.046(3) Uani 1 1 d . . .
H22 H 0.5024 -0.3003 0.134 0.056 Uiso 1 1 calc R . .
C23 C 0.5975(7) -0.2192(7) 0.2161(6) 0.049(3) Uani 1 1 d . . .
H23 H 0.6417 -0.2535 0.2155 0.058 Uiso 1 1 calc R . .
C24 C 0.6109(7) -0.1393(8) 0.2646(7) 0.050(3) Uani 1 1 d . . .
H24 H 0.664 -0.1197 0.2999 0.06 Uiso 1 1 calc R . .
C25 C 0.5467(6) -0.0884(7) 0.2616(6) 0.040(3) Uani 1 1 d . . .
H25 H 0.5593 -0.0332 0.2928 0.048 Uiso 1 1 calc R . .
C26 C 0.3884(8) -0.0408(9) 0.4002(7) 0.059(4) Uani 1 1 d . . .
H26 H 0.3829 -0.1004 0.3837 0.071 Uiso 1 1 calc R . .
C27 C 0.3919(9) -0.0085(11) 0.4818(8) 0.075(4) Uani 1 1 d . . .
H27 H 0.391 -0.0462 0.5192 0.09 Uiso 1 1 calc R . .
C28 C 0.3967(10) 0.0763(13) 0.5064(9) 0.084(5) Uani 1 1 d . . .
H28 H 0.3972 0.0975 0.5608 0.1 Uiso 1 1 calc R . .
C29 C 0.4011(9) 0.1341(10) 0.4500(10) 0.088(6) Uani 1 1 d . . .
H29 H 0.406 0.1936 0.4664 0.106 Uiso 1 1 calc R . .
C30 C 0.3976(7) 0.0977(7) 0.3660(6) 0.047(3) Uani 1 1 d . . .
H30 H 0.3988 0.1337 0.3272 0.057 Uiso 1 1 calc R . .
C31 C 0.3688(7) 0.5672(7) 0.6452(6) 0.039(3) Uani 1 1 d . . .
H31 H 0.3292 0.5849 0.6076 0.047 Uiso 1 1 calc R . .
C32 C 0.4563(8) 0.6072(8) 0.6609(6) 0.058(3) Uani 1 1 d . . .
H32 H 0.4744 0.6528 0.6342 0.07 Uiso 1 1 calc R . .
C33 C 0.5189(8) 0.5831(9) 0.7142(7) 0.066(4) Uani 1 1 d . . .
H33 H 0.5792 0.6072 0.7202 0.08 Uiso 1 1 calc R . .
C34 C 0.4864(7) 0.5186(6) 0.7604(6) 0.039(2) Uani 1 1 d U . .
H34 H 0.5229 0.5066 0.8039 0.047 Uiso 1 1 calc R . .
C35 C 0.3981(7) 0.4743(8) 0.7381(6) 0.050(3) Uani 1 1 d . . .
H35 H 0.3788 0.4253 0.7601 0.061 Uiso 1 1 calc R . .
C36 C 0.2442(7) 0.4028(7) 0.5035(6) 0.039(3) Uani 1 1 d . . .
H36 H 0.2959 0.3929 0.5327 0.047 Uiso 1 1 calc R . .
C37 C 0.2404(8) 0.3906(7) 0.4206(6) 0.052(3) Uani 1 1 d . . .
H37 H 0.2884 0.3773 0.3953 0.062 Uiso 1 1 calc R . .
C38 C 0.1605(8) 0.3994(7) 0.3775(6) 0.043(3) Uani 1 1 d . . .
H38 H 0.1533 0.3895 0.3214 0.052 Uiso 1 1 calc R . .
C39 C 0.0903(9) 0.4229(8) 0.4174(7) 0.065(4) Uani 1 1 d . . .
H39 H 0.0363 0.4298 0.3898 0.078 Uiso 1 1 calc R . .
C40 C 0.1076(7) 0.4353(7) 0.5026(6) 0.043(3) Uani 1 1 d . . .
H40 H 0.0621 0.4507 0.5306 0.052 Uiso 1 1 calc R . .
C41 C 0.0189(7) 0.3183(7) 0.6363(6) 0.049(3) Uani 1 1 d . . .
H41 H 0.049 0.2884 0.5999 0.059 Uiso 1 1 calc R . .
C42 C -0.0688(7) 0.2798(8) 0.6453(7) 0.057(4) Uani 1 1 d . . .
H42 H -0.0954 0.2248 0.6177 0.069 Uiso 1 1 calc R . .
C43 C -0.1109(7) 0.3267(8) 0.6951(7) 0.068(4) Uani 1 1 d . . .
H43 H -0.1717 0.3084 0.6951 0.082 Uiso 1 1 calc R . .
C44 C -0.0660(8) 0.4049(8) 0.7495(7) 0.057(3) Uani 1 1 d U . .
H44 H -0.0909 0.4312 0.7921 0.069 Uiso 1 1 calc R . .
C45 C 0.0166(6) 0.4361(6) 0.7318(5) 0.030(2) Uani 1 1 d . . .
H45 H 0.0451 0.4903 0.7598 0.036 Uiso 1 1 calc R . .
C46 C 0.3308(7) 0.6441(7) 0.8476(6) 0.042(3) Uani 1 1 d U . .
H46 H 0.2764 0.6382 0.8146 0.05 Uiso 1 1 calc R . .
C47 C 0.4020(7) 0.7077(7) 0.8414(7) 0.048(3) Uani 1 1 d . . .
H47 H 0.3953 0.7441 0.8034 0.057 Uiso 1 1 calc R . .
C48 C 0.4787(8) 0.7173(7) 0.8887(7) 0.063(4) Uani 1 1 d . . .
H48 H 0.524 0.7637 0.8878 0.075 Uiso 1 1 calc R . .
C49 C 0.4922(7) 0.6576(7) 0.9402(6) 0.042(3) Uani 1 1 d . . .
H49 H 0.548 0.66 0.9697 0.05 Uiso 1 1 calc R . .
C50 C 0.4218(6) 0.5960(7) 0.9460(6) 0.040(3) Uani 1 1 d . . .
H50 H 0.4304 0.557 0.9812 0.048 Uiso 1 1 calc R . .
C51 C 0.2663(6) 0.5812(6) 1.0768(6) 0.037(3) Uani 1 1 d . . .
H51 H 0.264 0.6284 1.0501 0.045 Uiso 1 1 calc R . .
C52 C 0.2798(7) 0.5952(7) 1.1625(6) 0.044(3) Uani 1 1 d . . .
H52 H 0.2854 0.6513 1.1908 0.053 Uiso 1 1 calc R . .
C53 C 0.2848(7) 0.5261(8) 1.2053(6) 0.041(3) Uani 1 1 d . . .
H53 H 0.2965 0.5348 1.2614 0.05 Uiso 1 1 calc R . .
C54 C 0.2709(7) 0.4429(7) 1.1582(6) 0.048(3) Uani 1 1 d . . .
H54 H 0.2689 0.3938 1.1827 0.057 Uiso 1 1 calc R . .
C55 C 0.2600(6) 0.4348(6) 1.0733(5) 0.032(2) Uani 1 1 d . . .
H55 H 0.2549 0.3796 1.0432 0.039 Uiso 1 1 calc R . .
C56 C 0.0574(6) 0.3806(7) 0.9420(6) 0.037(3) Uani 1 1 d . . .
H56 H 0.0607 0.4303 0.98 0.045 Uiso 1 1 calc R . .
C57 C -0.0144(7) 0.3196(7) 0.9334(7) 0.049(3) Uani 1 1 d . . .
H57 H -0.0597 0.3275 0.9644 0.059 Uiso 1 1 calc R . .
C58 C -0.0223(8) 0.2428(7) 0.8772(6) 0.054(3) Uani 1 1 d . . .
H58 H -0.0695 0.1969 0.8739 0.065 Uiso 1 1 calc R . .
C59 C 0.0415(7) 0.2380(6) 0.8280(6) 0.044(3) Uani 1 1 d . . .
H59 H 0.0355 0.1913 0.7861 0.053 Uiso 1 1 calc R . .
C60 C 0.1124(7) 0.3010(7) 0.8410(6) 0.049(3) Uani 1 1 d U . .
H60 H 0.1566 0.2949 0.8083 0.059 Uiso 1 1 calc R . .
N1 N 0.2058(5) 0.1098(5) 0.0787(4) 0.031(2) Uani 1 1 d . . .
N2 N 0.0875(5) 0.1837(6) 0.1963(5) 0.038(2) Uani 1 1 d . . .
N3 N 0.1735(6) 0.0922(6) 0.3276(5) 0.052(3) Uani 1 1 d . . .
N4 N 0.3238(5) -0.0778(5) 0.0832(4) 0.0298(19) Uani 1 1 d . . .
N5 N 0.4654(5) -0.1141(5) 0.2152(4) 0.031(2) Uani 1 1 d . . .
N6 N 0.3927(6) 0.0121(6) 0.3440(5) 0.047(2) Uani 1 1 d . . .
N7 N 0.3401(5) 0.5024(5) 0.6842(4) 0.033(2) Uani 1 1 d . . .
N8 N 0.1822(6) 0.4272(6) 0.5460(5) 0.043(2) Uani 1 1 d . . .
N9 N 0.0601(5) 0.3956(5) 0.6779(4) 0.039(2) Uani 1 1 d . . .
N10 N 0.3421(5) 0.5888(5) 0.9043(4) 0.031(2) Uani 1 1 d . . .
N11 N 0.2567(5) 0.5010(5) 1.0336(4) 0.0284(19) Uani 1 1 d . . .
N12 N 0.1264(5) 0.3758(5) 0.8996(4) 0.0277(19) Uani 1 1 d . . .
O1 O 0.2766(4) 0.0334(4) 0.2095(4) 0.0286(14) Uani 1 1 d . . .
O2 O 0.2170(4) 0.4639(4) 0.7888(4) 0.0259(14) Uani 1 1 d . . .
Cl1 Cl 0.29407(16) 0.23696(16) 0.24805(15) 0.0423(7) Uani 1 1 d . . .
Cl2 Cl 0.07003(17) -0.01839(18) 0.16047(16) 0.0464(7) Uani 1 1 d . . .
Cl3 Cl 0.47923(17) 0.07811(17) 0.19331(16) 0.0440(7) Uani 1 1 d . . .
Cl4 Cl 0.26571(17) -0.16000(18) 0.23846(15) 0.0442(7) Uani 1 1 d . . .
Cl8 Cl 0.33851(17) 0.38388(17) 0.90790(15) 0.0394(6) Uani 1 1 d . . .
Cl5 Cl 0.16117(16) 0.58645(17) 0.66736(14) 0.0392(6) Uani 1 1 d . . .
Cl7 Cl 0.13181(17) 0.57946(17) 0.91475(15) 0.0416(7) Uani 1 1 d . . .
Cl6 Cl 0.23430(16) 0.30231(16) 0.66318(14) 0.0386(6) Uani 1 1 d . . .
V1 V 0.19275(11) 0.09965(12) 0.20386(10) 0.0329(4) Uani 1 1 d . . .
V2 V 0.36000(11) -0.03203(11) 0.21315(10) 0.0324(4) Uani 1 1 d . . .
V3 V 0.20058(11) 0.44774(11) 0.68179(9) 0.0304(4) Uani 1 1 d . . .
V4 V 0.23269(11) 0.48010(11) 0.89683(9) 0.0282(4) Uani 1 1 d . . .
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 0 '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 0.006 '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'
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 C1 C2 126.1(9) . . ?
C1 C2 C3 113.3(11) . . ?
C4 C3 C2 121.5(12) . . ?
C3 C4 C5 119.9(10) . . ?
N1 C5 C4 122.3(10) . . ?
N2 C6 C7 123.5(9) . . ?
C8 C7 C6 120.2(12) . . ?
C7 C8 C9 118.3(12) . . ?
C10 C9 C8 117.2(11) . . ?
C9 C10 N2 125.1(12) . . ?
N3 C11 C12 124.6(12) . . ?
C13 C12 C11 117.7(11) . . ?
C12 C13 C14 119.8(12) . . ?
C15 C14 C13 117.7(13) . . ?
N3 C15 C14 119.6(11) . . ?
N4 C16 C17 122.4(11) . . ?
C16 C17 C18 115.5(11) . . ?
C19 C18 C17 121.5(11) . . ?
C18 C19 C20 117.4(12) . . ?
N4 C20 C19 122.7(11) . . ?
C22 C21 N5 123.9(9) . . ?
C21 C22 C23 120.3(9) . . ?
C24 C23 C22 116.9(10) . . ?
C25 C24 C23 120.4(10) . . ?
N5 C25 C24 123.4(9) . . ?
N6 C26 C27 121.9(12) . . ?
C28 C27 C26 120.1(13) . . ?
C27 C28 C29 120.0(14) . . ?
C28 C29 C30 117.9(13) . . ?
N6 C30 C29 119.9(12) . . ?
N7 C31 C32 119.9(10) . . ?
C31 C32 C33 123.1(12) . . ?
C32 C33 C34 116.6(11) . . ?
C35 C34 C33 118.0(9) . . ?
N7 C35 C34 120.6(11) . . ?
N8 C36 C37 127.1(10) . . ?
C36 C37 C38 115.8(10) . . ?
C37 C38 C39 120.9(10) . . ?
C38 C39 C40 115.1(11) . . ?
N8 C40 C39 126.0(10) . . ?
N9 C41 C42 122.9(10) . . ?
C43 C42 C41 116.4(10) . . ?
C42 C43 C44 122.7(10) . . ?
C45 C44 C43 113.2(10) . . ?
N9 C45 C44 125.9(9) . . ?
C47 C46 N10 119.1(9) . . ?
C48 C47 C46 120.8(11) . . ?
C47 C48 C49 119.8(10) . . ?
C50 C49 C48 118.5(10) . . ?
N10 C50 C49 123.1(11) . . ?
N11 C51 C52 121.2(10) . . ?
C53 C52 C51 121.3(9) . . ?
C52 C53 C54 115.8(9) . . ?
C53 C54 C55 119.2(11) . . ?
N11 C55 C54 124.1(9) . . ?
C57 C56 N12 124.6(10) . . ?
C56 C57 C58 120.0(11) . . ?
C59 C58 C57 117.6(9) . . ?
C60 C59 C58 118.7(9) . . ?
C59 C60 N12 125.5(10) . . ?
C5 N1 C1 116.7(9) . . ?
C5 N1 V1 125.3(7) . . ?
C1 N1 V1 118.0(6) . . ?
C6 N2 C10 115.4(9) . . ?
C6 N2 V1 123.8(7) . . ?
C10 N2 V1 120.8(8) . . ?
C11 N3 C15 119.0(10) . . ?
C11 N3 V1 123.0(8) . . ?
C15 N3 V1 118.0(7) . . ?
C16 N4 C20 120.1(9) . . ?
C16 N4 V2 117.2(7) . . ?
C20 N4 V2 122.4(7) . . ?
C25 N5 C21 114.9(8) . . ?
C25 N5 V2 123.2(6) . . ?
C21 N5 V2 121.9(6) . . ?
C30 N6 C26 120.1(10) . . ?
C30 N6 V2 113.5(7) . . ?
C26 N6 V2 124.7(8) . . ?
C31 N7 C35 120.7(9) . . ?
C31 N7 V3 124.2(6) . . ?
C35 N7 V3 114.6(7) . . ?
C40 N8 C36 114.9(9) . . ?
C40 N8 V3 122.4(7) . . ?
C36 N8 V3 122.7(7) . . ?
C45 N9 C41 117.5(9) . . ?
C45 N9 V3 117.0(6) . . ?
C41 N9 V3 124.4(7) . . ?
C50 N10 C46 118.2(9) . . ?
C50 N10 V4 124.7(7) . . ?
C46 N10 V4 115.7(6) . . ?
C55 N11 C51 118.2(8) . . ?
C55 N11 V4 121.3(6) . . ?
C51 N11 V4 120.5(7) . . ?
C56 N12 C60 113.1(8) . . ?
C56 N12 V4 125.8(6) . . ?
C60 N12 V4 119.5(7) . . ?
V2 O1 V1 178.8(4) . . ?
V3 O2 V4 179.6(4) . . ?
O1 V1 N3 91.0(3) . . ?
O1 V1 N1 91.8(3) . . ?
N3 V1 N1 177.1(3) . . ?
O1 V1 N2 179.7(4) . . ?
N3 V1 N2 89.2(3) . . ?
N1 V1 N2 87.9(3) . . ?
O1 V1 Cl2 95.6(2) . . ?
N3 V1 Cl2 88.7(3) . . ?
N1 V1 Cl2 90.3(2) . . ?
N2 V1 Cl2 84.6(2) . . ?
O1 V1 Cl1 95.8(2) . . ?
N3 V1 Cl1 90.3(2) . . ?
N1 V1 Cl1 90.0(2) . . ?
N2 V1 Cl1 83.9(2) . . ?
Cl2 V1 Cl1 168.56(12) . . ?
O1 V2 N4 89.6(3) . . ?
O1 V2 N6 89.8(3) . . ?
N4 V2 N6 178.4(3) . . ?
O1 V2 N5 178.9(3) . . ?
N4 V2 N5 89.5(3) . . ?
N6 V2 N5 91.2(3) . . ?
O1 V2 Cl3 95.8(2) . . ?
N4 V2 Cl3 92.2(2) . . ?
N6 V2 Cl3 89.3(3) . . ?
N5 V2 Cl3 83.7(2) . . ?
O1 V2 Cl4 96.4(2) . . ?
N4 V2 Cl4 89.7(2) . . ?
N6 V2 Cl4 89.0(3) . . ?
N5 V2 Cl4 84.2(2) . . ?
Cl3 V2 Cl4 167.72(12) . . ?
O2 V3 N7 89.6(3) . . ?
O2 V3 N9 91.0(3) . . ?
N7 V3 N9 178.6(3) . . ?
O2 V3 N8 179.0(3) . . ?
N7 V3 N8 89.5(3) . . ?
N9 V3 N8 89.9(3) . . ?
O2 V3 Cl5 97.2(2) . . ?
N7 V3 Cl5 89.7(2) . . ?
N9 V3 Cl5 89.0(2) . . ?
N8 V3 Cl5 83.2(3) . . ?
O2 V3 Cl6 95.8(2) . . ?
N7 V3 Cl6 90.7(2) . . ?
N9 V3 Cl6 90.4(2) . . ?
N8 V3 Cl6 83.8(3) . . ?
Cl5 V3 Cl6 166.97(10) . . ?
O2 V4 N12 92.8(3) . . ?
O2 V4 N10 91.6(3) . . ?
N12 V4 N10 175.5(3) . . ?
O2 V4 N11 178.4(3) . . ?
N12 V4 N11 88.3(3) . . ?
N10 V4 N11 87.2(3) . . ?
O2 V4 Cl7 96.5(2) . . ?
N12 V4 Cl7 89.2(2) . . ?
N10 V4 Cl7 89.9(2) . . ?
N11 V4 Cl7 84.7(2) . . ?
O2 V4 Cl8 95.1(2) . . ?
N12 V4 Cl8 90.1(2) . . ?
N10 V4 Cl8 89.9(2) . . ?
N11 V4 Cl8 83.8(2) . . ?
Cl7 V4 Cl8 168.45(11) . . ?
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
C1 N1 1.341(11) . ?
C1 C2 1.385(14) . ?
C2 C3 1.412(15) . ?
C3 C4 1.285(16) . ?
C4 C5 1.421(16) . ?
C5 N1 1.273(12) . ?
C6 N2 1.345(12) . ?
C6 C7 1.354(13) . ?
C7 C8 1.342(15) . ?
C8 C9 1.433(15) . ?
C9 C10 1.333(15) . ?
C10 N2 1.354(12) . ?
C11 N3 1.351(13) . ?
C11 C12 1.388(14) . ?
C12 C13 1.380(16) . ?
C13 C14 1.468(16) . ?
C14 C15 1.415(15) . ?
C15 N3 1.398(14) . ?
C16 N4 1.298(11) . ?
C16 C17 1.407(14) . ?
C17 C18 1.425(17) . ?
C18 C19 1.355(16) . ?
C19 C20 1.373(14) . ?
C20 N4 1.350(12) . ?
C21 C22 1.336(13) . ?
C21 N5 1.377(12) . ?
C22 C23 1.396(13) . ?
C23 C24 1.374(14) . ?
C24 C25 1.364(13) . ?
C25 N5 1.359(11) . ?
C26 N6 1.355(14) . ?
C26 C27 1.391(16) . ?
C27 C28 1.332(19) . ?
C28 C29 1.42(2) . ?
C29 C30 1.444(16) . ?
C30 N6 1.337(13) . ?
C31 N7 1.345(12) . ?
C31 C32 1.366(14) . ?
C32 C33 1.374(16) . ?
C33 C34 1.437(15) . ?
C34 C35 1.402(13) . ?
C35 N7 1.366(13) . ?
C36 N8 1.326(12) . ?
C36 C37 1.379(13) . ?
C37 C38 1.385(15) . ?
C38 C39 1.404(16) . ?
C39 C40 1.412(14) . ?
C40 N8 1.318(12) . ?
C41 N9 1.338(11) . ?
C41 C42 1.419(14) . ?
C42 C43 1.330(15) . ?
C43 C44 1.448(15) . ?
C44 C45 1.368(14) . ?
C45 N9 1.336(11) . ?
C46 C47 1.387(13) . ?
C46 N10 1.404(13) . ?
C47 C48 1.315(14) . ?
C48 C49 1.397(15) . ?
C49 C50 1.359(14) . ?
C50 N10 1.315(11) . ?
C51 N11 1.345(11) . ?
C51 C52 1.418(13) . ?
C52 C53 1.404(15) . ?
C53 C54 1.405(14) . ?
C54 C55 1.411(13) . ?
C55 N11 1.327(12) . ?
C56 C57 1.323(13) . ?
C56 N12 1.349(12) . ?
C57 C58 1.407(15) . ?
C58 C59 1.360(15) . ?
C59 C60 1.327(13) . ?
C60 N12 1.397(12) . ?
N1 V1 2.177(8) . ?
N2 V1 2.247(9) . ?
N3 V1 2.165(9) . ?
N4 V2 2.187(8) . ?
N5 V2 2.223(8) . ?
N6 V2 2.195(8) . ?
N7 V3 2.168(8) . ?
N8 V3 2.250(8) . ?
N9 V3 2.169(8) . ?
N10 V4 2.181(8) . ?
N11 V4 2.266(8) . ?
N12 V4 2.139(8) . ?
O1 V2 1.765(7) . ?
O1 V1 1.781(7) . ?
O2 V3 1.772(6) . ?
O2 V4 1.790(6) . ?
Cl1 V1 2.424(3) . ?
Cl2 V1 2.393(3) . ?
Cl3 V2 2.408(3) . ?
Cl4 V2 2.418(3) . ?
Cl8 V4 2.398(3) . ?
Cl5 V3 2.401(3) . ?
Cl7 V4 2.381(3) . ?
Cl6 V3 2.418(3) . ?
