#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/87/7028721.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_7028721
loop_
_publ_author_name
'Cozzolino, Anthony F.'
'Silvia, Jared S.'
'Lopez, Nazario'
'Cummins, Christopher C.'
_publ_section_title
;
 Experimental and computational studies on the formation of cyanate from
 early metal terminal nitrido ligands and carbon monoxide.
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4639
_journal_page_last               4652
_journal_paper_doi               10.1039/c3dt52738g
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C6 H16 Cl1 N2 V0.5, C26 H42 N4 V, C7 H8'
_chemical_formula_sum            'C39 H66 Cl N6 V1.5'
_chemical_formula_weight         730.84
_chemical_name_common
bis(2-dimethylamino-5-methylphenyl(tertbutyl)amido)-vanadium
_chemical_name_systematic
; 
bis(2-dimethylamino-5-methylphenyl(tertbutyl)amido)-vanadium 
bis(tetramethylethylenediamine)vanadiumdichloride
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.421(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.6314(19)
_cell_length_b                   9.6863(11)
_cell_length_c                   24.542(3)
_cell_measurement_reflns_used    9642
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.4095
_cell_measurement_theta_min      2.294
_cell_volume                     4076.9(8)
_computing_cell_refinement       'SAINT 7.46A (Bruker-AXS, 2008)'
_computing_data_collection       'APEX2 3.0 (Bruker-AXS, 2008)'
_computing_data_reduction        'SAINT 7.46A (Bruker-AXS, 2008)'
_computing_molecular_graphics    'WINGX (Farrugia, 1999)'
_computing_publication_material  'WINGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker Smart APEX CCD'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0234
_diffrn_reflns_av_unetI/netI     0.0328
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            24332
_diffrn_reflns_theta_full        30.49
_diffrn_reflns_theta_max         30.49
_diffrn_reflns_theta_min         1.19
_exptl_absorpt_coefficient_mu    0.450
_exptl_absorpt_correction_T_max  0.9154
_exptl_absorpt_correction_T_min  0.7741
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.191
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1574
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.403
_refine_diff_density_min         -0.361
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.795
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     612
_refine_ls_number_reflns         12330
_refine_ls_number_restraints     154
_refine_ls_restrained_S_all      0.803
_refine_ls_R_factor_all          0.0618
_refine_ls_R_factor_gt           0.0432
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0556P)²+2.2684P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1096
_refine_ls_wR_factor_ref         0.1280
_reflns_number_gt                9299
_reflns_number_total             12330
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt52738g.txt
_cod_data_source_block           10228
_cod_original_cell_volume        4076.8(8)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C39 H66 Cl N6 V1.50'
_cod_database_code               7028721
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'
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 0.315092(14) 0.99204(2) 0.256651(10) 0.01862(7) Uani 1 1 d . . .
N1 N 0.38513(7) 1.08439(13) 0.32401(5) 0.0198(2) Uani 1 1 d . . .
N121 N 0.42720(8) 1.00141(12) 0.23051(6) 0.0235(3) Uani 1 1 d . . .
C11 C 0.46384(8) 1.06203(14) 0.33027(6) 0.0206(3) Uani 1 1 d . . .
C12 C 0.48819(9) 1.01222(14) 0.28246(7) 0.0231(3) Uani 1 1 d . . .
C13 C 0.56598(10) 0.98683(15) 0.28399(9) 0.0314(4) Uani 1 1 d . . .
H13 H 0.5803 0.9553 0.2511 0.038 Uiso 1 1 calc R . .
C14 C 0.62351(10) 1.00664(17) 0.33278(10) 0.0366(4) Uani 1 1 d . . .
H14 H 0.6765 0.9867 0.3335 0.044 Uiso 1 1 calc R . .
C15 C 0.60278(9) 1.05564(18) 0.38024(8) 0.0333(4) Uani 1 1 d . . .
C16 C 0.52448(9) 1.08194(17) 0.37897(7) 0.0271(3) Uani 1 1 d . . .
H16 H 0.5113 1.1145 0.4121 0.033 Uiso 1 1 calc R . .
C151 C 0.66381(11) 1.0843(2) 0.43349(10) 0.0482(5) Uani 1 1 d . . .
H15A H 0.7085 1.0228 0.4354 0.072 Uiso 1 1 calc R . .
H15B H 0.6415 1.0680 0.4660 0.072 Uiso 1 1 calc R . .
H15C H 0.6810 1.1805 0.4336 0.072 Uiso 1 1 calc R . .
C17 C 0.35476(9) 1.15136(17) 0.36884(6) 0.0243(3) Uani 1 1 d . . .
C171 C 0.38904(10) 1.29683(18) 0.38319(7) 0.0302(3) Uani 1 1 d . . .
H17A H 0.4454 1.2898 0.3984 0.045 Uiso 1 1 calc R . .
H17B H 0.3647 1.3396 0.4111 0.045 Uiso 1 1 calc R . .
H17C H 0.3788 1.3536 0.3492 0.045 Uiso 1 1 calc R . .
C172 C 0.36422(11) 1.0609(2) 0.42142(7) 0.0349(4) Uani 1 1 d . . .
H17D H 0.3416 0.9696 0.4108 0.052 Uiso 1 1 calc R . .
H17E H 0.3373 1.1044 0.4477 0.052 Uiso 1 1 calc R . .
H17F H 0.4198 1.0511 0.4393 0.052 Uiso 1 1 calc R . .
C173 C 0.26703(10) 1.1712(2) 0.34525(8) 0.0350(4) Uani 1 1 d . . .
H17G H 0.2585 1.2287 0.3115 0.053 Uiso 1 1 calc R . .
H17H H 0.2442 1.2166 0.3734 0.053 Uiso 1 1 calc R . .
H17I H 0.2422 1.0811 0.3358 0.053 Uiso 1 1 calc R . .
C121 C 0.43739(12) 0.88044(19) 0.19575(9) 0.0374(4) Uani 1 1 d . . .
H12A H 0.4862 0.8901 0.1834 0.056 Uiso 1 1 calc R . .
H12B H 0.3935 0.8755 0.1629 0.056 Uiso 1 1 calc R . .
H12C H 0.4392 0.7959 0.2179 0.056 Uiso 1 1 calc R . .
C122 C 0.43101(12) 1.12969(18) 0.19796(7) 0.0328(4) Uani 1 1 d . . .
H12D H 0.4214 1.2098 0.2198 0.049 Uiso 1 1 calc R . .
H12E H 0.3914 1.1261 0.1626 0.049 Uiso 1 1 calc R . .
H12F H 0.4828 1.1377 0.1900 0.049 Uiso 1 1 calc R . .
N2 N 0.22961(7) 0.85300(13) 0.25877(5) 0.0213(2) Uani 1 1 d . . .
N221 N 0.22219(9) 1.06238(14) 0.18601(6) 0.0303(3) Uani 1 1 d . . .
C21 C 0.15495(9) 0.89588(15) 0.23389(6) 0.0224(3) Uani 1 1 d . . .
C22 C 0.14878(10) 1.01123(16) 0.19724(7) 0.0292(3) Uani 1 1 d . . .
C23 C 0.07745(12) 1.0660(2) 0.17057(9) 0.0449(5) Uani 1 1 d . . .
H23 H 0.0756 1.1427 0.1461 0.054 Uiso 1 1 calc R . .
C24 C 0.00835(12) 1.0106(2) 0.17896(10) 0.0468(5) Uani 1 1 d . . .
H24 H -0.0403 1.0503 0.1610 0.056 Uiso 1 1 calc R . .
C25 C 0.01093(10) 0.89767(19) 0.21356(8) 0.0340(4) Uani 1 1 d . . .
C26 C 0.08287(9) 0.84125(17) 0.24052(7) 0.0259(3) Uani 1 1 d . . .
H26 H 0.0836 0.7634 0.2642 0.031 Uiso 1 1 calc R . .
C251 C -0.06311(10) 0.8328(2) 0.22256(10) 0.0442(5) Uani 1 1 d . . .
H25A H -0.0756 0.8720 0.2562 0.066 Uiso 1 1 calc R . .
H25B H -0.0558 0.7328 0.2273 0.066 Uiso 1 1 calc R . .
H25C H -0.1060 0.8513 0.1900 0.066 Uiso 1 1 calc R . .
C27 C 0.24436(9) 0.72270(17) 0.29072(8) 0.0310(4) Uani 1 1 d . . .
C271 C 0.33341(10) 0.70671(19) 0.30758(10) 0.0427(5) Uani 1 1 d . . .
H27A H 0.3562 0.7857 0.3306 0.064 Uiso 1 1 calc R . .
H27B H 0.3541 0.7029 0.2738 0.064 Uiso 1 1 calc R . .
H27C H 0.3468 0.6213 0.3291 0.064 Uiso 1 1 calc R . .
C272 C 0.21510(12) 0.7258(3) 0.34516(8) 0.0481(6) Uani 1 1 d . . .
H27D H 0.1582 0.7352 0.3360 0.072 Uiso 1 1 calc R . .
H27E H 0.2386 0.8042 0.3682 0.072 Uiso 1 1 calc R . .
H27F H 0.2299 0.6398 0.3659 0.072 Uiso 1 1 calc R . .
C273 C 0.21183(11) 0.59795(19) 0.25405(10) 0.0434(5) Uani 1 1 d . . .
H27G H 0.2273 0.5126 0.2752 0.065 Uiso 1 1 calc R . .
H27H H 0.2326 0.5979 0.2203 0.065 Uiso 1 1 calc R . .
H27I H 0.1548 0.6037 0.2433 0.065 Uiso 1 1 calc R . .
C221 C 0.23169(13) 0.9979(2) 0.13314(8) 0.0430(5) Uani 1 1 d . . .
H22A H 0.2340 0.8973 0.1375 0.065 Uiso 1 1 calc R . .
H22B H 0.2800 1.0310 0.1244 0.065 Uiso 1 1 calc R . .
H22C H 0.1873 1.0228 0.1026 0.065 Uiso 1 1 calc R . .
C222 C 0.22302(13) 1.21546(19) 0.18026(9) 0.0466(5) Uani 1 1 d . . .
H22D H 0.1857 1.2430 0.1458 0.070 Uiso 1 1 calc R . .
H22E H 0.2754 1.2459 0.1786 0.070 Uiso 1 1 calc R . .
H22F H 0.2085 1.2582 0.2126 0.070 Uiso 1 1 calc R . .
V2 V 0.0000 0.5000 0.0000 0.01870(8) Uani 1 2 d S . .
Cl2 Cl 0.12244(5) 0.38281(13) 0.04695(3) 0.0355(2) Uani 0.679(2) 1 d P A 1
N3 N 0.05896(14) 0.7129(2) 0.02004(11) 0.0392(6) Uani 0.679(2) 1 d PU A 1
N4 N -0.02961(15) 0.5351(3) 0.08591(10) 0.0367(6) Uani 0.679(2) 1 d PDU A 1
C31 C 0.1429(2) 0.7141(4) 0.0251(3) 0.0808(16) Uani 0.679(2) 1 d P A 1
H31A H 0.1539 0.6912 -0.0112 0.121 Uiso 0.679(2) 1 calc PR A 1
H31B H 0.1677 0.6459 0.0531 0.121 Uiso 0.679(2) 1 calc PR A 1
H31C H 0.1635 0.8062 0.0368 0.121 Uiso 0.679(2) 1 calc PR A 1
C32 C 0.0283(3) 0.8250(4) -0.0176(3) 0.113(3) Uani 0.679(2) 1 d P A 1
H32A H 0.0343 0.8030 -0.0553 0.169 Uiso 0.679(2) 1 calc PR A 1
H32B H 0.0569 0.9100 -0.0044 0.169 Uiso 0.679(2) 1 calc PR A 1
H32C H -0.0271 0.8380 -0.0184 0.169 Uiso 0.679(2) 1 calc PR A 1
C33 C 0.0476(5) 0.7415(9) 0.0764(3) 0.102(2) Uani 0.679(2) 1 d PDU A 1
H33A H 0.0962 0.7142 0.1034 0.123 Uiso 0.679(2) 1 calc PR A 1
H33B H 0.0428 0.8428 0.0795 0.123 Uiso 0.679(2) 1 calc PR A 1
C43 C -0.0137(7) 0.6826(9) 0.0945(4) 0.063(2) Uani 0.385(10) 1 d PDU A 3
H43A H -0.0617 0.7328 0.0760 0.076 Uiso 0.385(10) 1 calc PR A 3
H43B H -0.0049 0.7008 0.1352 0.076 Uiso 0.385(10) 1 calc PR A 3
C41 C 0.0037(4) 0.4392(7) 0.12975(19) 0.097(2) Uani 0.679(2) 1 d P A 1
H41A H -0.0133 0.3454 0.1179 0.146 Uiso 0.679(2) 1 calc PR A 1
H41B H -0.0137 0.4627 0.1638 0.146 Uiso 0.679(2) 1 calc PR A 1
H41C H 0.0607 0.4443 0.1375 0.146 Uiso 0.679(2) 1 calc PR A 1
C42 C -0.1122(3) 0.5458(7) 0.08568(17) 0.0879(19) Uani 0.679(2) 1 d P A 1
H42A H -0.1376 0.4566 0.0751 0.132 Uiso 0.679(2) 1 calc PR A 1
H42B H -0.1367 0.6163 0.0586 0.132 Uiso 0.679(2) 1 calc PR A 1
H42C H -0.1179 0.5715 0.1231 0.132 Uiso 0.679(2) 1 calc PR A 1
C44 C 0.0294(7) 0.6472(11) 0.1102(4) 0.052(3) Uani 0.294(11) 1 d PDU A 4
H44A H 0.0094 0.6963 0.1394 0.063 Uiso 0.294(11) 1 calc PR A 4
H44B H 0.0783 0.6005 0.1293 0.063 Uiso 0.294(11) 1 calc PR A 4
Cl3 Cl 0.09714(11) 0.3205(2) 0.03925(6) 0.0299(4) Uani 0.321(2) 1 d P A 2
N5 N 0.0511(3) 0.6398(6) 0.0762(2) 0.0358(11) Uani 0.321(2) 1 d PU A 2
N6 N -0.0775(2) 0.4300(5) 0.05914(18) 0.0299(10) Uani 0.321(2) 1 d PDU A 2
C51 C 0.1327(4) 0.6187(11) 0.1021(3) 0.073(3) Uani 0.321(2) 1 d P A 2
H51D H 0.1644 0.6466 0.0760 0.110 Uiso 0.321(2) 1 calc PR A 2
H51E H 0.1419 0.5208 0.1115 0.110 Uiso 0.321(2) 1 calc PR A 2
H51F H 0.1472 0.6743 0.1363 0.110 Uiso 0.321(2) 1 calc PR A 2
C52 C 0.0321(10) 0.7855(11) 0.0639(7) 0.080(5) Uani 0.321(2) 1 d P A 2
H52D H 0.0527 0.8149 0.0320 0.120 Uiso 0.321(2) 1 calc PR A 2
H52E H 0.0554 0.8417 0.0967 0.120 Uiso 0.321(2) 1 calc PR A 2
H52F H -0.0247 0.7974 0.0548 0.120 Uiso 0.321(2) 1 calc PR A 2
C53 C 0.0078(7) 0.5950(11) 0.1164(5) 0.068(2) Uani 0.321(2) 1 d PDU A 2
H53C H 0.0444 0.5991 0.1537 0.081 Uiso 0.321(2) 1 calc PR A 2
H53D H -0.0324 0.6664 0.1165 0.081 Uiso 0.321(2) 1 calc PR A 2
C63 C -0.0295(7) 0.4695(13) 0.1136(4) 0.032(3) Uani 0.153(7) 1 d PDU A 3
H63C H -0.0631 0.4704 0.1408 0.039 Uiso 0.153(7) 1 calc PR A 3
H63D H 0.0105 0.3971 0.1258 0.039 Uiso 0.153(7) 1 calc PR A 3
C64 C -0.0654(7) 0.5465(12) 0.1029(5) 0.037(3) Uani 0.168(7) 1 d PDU A 4
H64A H -0.1013 0.6234 0.0881 0.045 Uiso 0.168(7) 1 calc PR A 4
H64B H -0.0793 0.5117 0.1373 0.045 Uiso 0.168(7) 1 calc PR A 4
C61 C -0.0703(7) 0.2838(12) 0.0737(7) 0.133(7) Uani 0.321(2) 1 d P A 2
H61D H -0.1214 0.2393 0.0618 0.199 Uiso 0.321(2) 1 calc PR A 2
H61E H -0.0513 0.2739 0.1143 0.199 Uiso 0.321(2) 1 calc PR A 2
H61F H -0.0335 0.2399 0.0547 0.199 Uiso 0.321(2) 1 calc PR A 2
C62 C -0.1598(3) 0.4565(10) 0.0405(3) 0.057(2) Uani 0.321(2) 1 d P A 2
H62D H -0.1741 0.4608 -0.0005 0.086 Uiso 0.321(2) 1 calc PR A 2
H62E H -0.1723 0.5447 0.0560 0.086 Uiso 0.321(2) 1 calc PR A 2
H62F H -0.1890 0.3821 0.0534 0.086 Uiso 0.321(2) 1 calc PR A 2
C1T C 0.1894(3) 0.4390(5) 0.4609(2) 0.0481(13) Uani 0.454(5) 1 d P B 1
H1T1 H 0.1726 0.5353 0.4547 0.072 Uiso 0.454(5) 1 calc PR B 1
H1T2 H 0.1563 0.3916 0.4820 0.072 Uiso 0.454(5) 1 calc PR B 1
H1T3 H 0.1849 0.3931 0.4247 0.072 Uiso 0.454(5) 1 calc PR B 1
C2T C 0.2725(4) 0.4346(7) 0.4935(3) 0.0318(13) Uani 0.454(5) 1 d P B 1
C3T C 0.3048(6) 0.3155(9) 0.5209(3) 0.0328(14) Uani 0.454(5) 1 d P B 1
H3T H 0.2729 0.2363 0.5204 0.039 Uiso 0.454(5) 1 calc PR B 1
C4T C 0.3816(6) 0.3098(9) 0.5486(3) 0.0422(14) Uani 0.454(5) 1 d P B 1
H4T H 0.4024 0.2270 0.5668 0.051 Uiso 0.454(5) 1 calc PR B 1
C5T C 0.4296(4) 0.4249(9) 0.5501(2) 0.0455(14) Uani 0.454(5) 1 d P B 1
H5T H 0.4830 0.4208 0.5691 0.055 Uiso 0.454(5) 1 calc PR B 1
C6T C 0.3990(9) 0.5427(12) 0.5242(7) 0.047(3) Uani 0.454(5) 1 d P B 1
H6T H 0.4312 0.6221 0.5265 0.056 Uiso 0.454(5) 1 calc PR B 1
C7T C 0.3194(13) 0.551(3) 0.4935(11) 0.039(3) Uani 0.454(5) 1 d P B 1
H7T H 0.2992 0.6321 0.4738 0.047 Uiso 0.454(5) 1 calc PR B 1
C1T' C 0.4799(3) 0.2944(6) 0.56782(18) 0.0653(16) Uani 0.546(5) 1 d P B 2
H1T4 H 0.4706 0.2284 0.5958 0.098 Uiso 0.546(5) 1 calc PR B 2
H1T5 H 0.5192 0.3619 0.5859 0.098 Uiso 0.546(5) 1 calc PR B 2
H1T6 H 0.4987 0.2449 0.5387 0.098 Uiso 0.546(5) 1 calc PR B 2
C2T' C 0.4060(4) 0.3670(6) 0.54212(18) 0.0363(11) Uani 0.546(5) 1 d P B 2
C3T' C 0.3350(6) 0.3014(8) 0.5364(3) 0.0453(18) Uani 0.546(5) 1 d P B 2
H3T' H 0.3336 0.2116 0.5517 0.054 Uiso 0.546(5) 1 calc PR B 2
C4T' C 0.2669(5) 0.3626(10) 0.5095(3) 0.0570(16) Uani 0.546(5) 1 d P B 2
H4T' H 0.2190 0.3144 0.5058 0.068 Uiso 0.546(5) 1 calc PR B 2
C5T' C 0.2668(5) 0.4922(10) 0.4877(3) 0.0537(16) Uani 0.546(5) 1 d P B 2
H5T' H 0.2198 0.5338 0.4676 0.064 Uiso 0.546(5) 1 calc PR B 2
C6T' C 0.3370(11) 0.561(3) 0.4958(10) 0.046(3) Uani 0.546(5) 1 d P B 2
H6T' H 0.3374 0.6540 0.4833 0.055 Uiso 0.546(5) 1 calc PR B 2
C7T' C 0.4046(8) 0.5013(8) 0.5208(5) 0.0418(17) Uani 0.546(5) 1 d P B 2
H7T' H 0.4521 0.5504 0.5241 0.050 Uiso 0.546(5) 1 calc PR B 2
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'
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
N1 V1 N2 125.93(5) . .
N1 V1 N221 135.03(5) . .
N2 V1 N221 78.71(5) . .
N1 V1 N121 78.62(5) . .
N2 V1 N121 138.71(5) . .
N221 V1 N121 108.07(6) . .
C11 N1 C17 120.99(12) . .
C11 N1 V1 115.38(10) . .
C17 N1 V1 122.85(9) . .
C12 N121 C121 113.15(14) . .
C12 N121 C122 106.95(12) . .
C121 N121 C122 108.92(14) . .
C12 N121 V1 105.90(9) . .
C121 N121 V1 111.65(10) . .
C122 N121 V1 110.13(11) . .
N1 C11 C16 127.94(14) . .
N1 C11 C12 116.75(13) . .
C16 C11 C12 115.32(14) . .
C13 C12 C11 121.58(16) . .
C13 C12 N121 122.12(15) . .
C11 C12 N121 116.08(13) . .
C12 C13 C14 121.21(17) . .
C12 C13 H13 119.4 . .
C14 C13 H13 119.4 . .
C15 C14 C13 119.32(15) . .
C15 C14 H14 120.3 . .
C13 C14 H14 120.3 . .
C14 C15 C16 119.78(17) . .
C14 C15 C151 121.08(17) . .
C16 C15 C151 119.13(19) . .
C15 C16 C11 122.76(17) . .
C15 C16 H16 118.6 . .
C11 C16 H16 118.6 . .
C15 C151 H15A 109.5 . .
C15 C151 H15B 109.5 . .
H15A C151 H15B 109.5 . .
C15 C151 H15C 109.5 . .
H15A C151 H15C 109.5 . .
H15B C151 H15C 109.5 . .
N1 C17 C173 106.37(12) . .
N1 C17 C172 112.76(14) . .
C173 C17 C172 106.99(14) . .
N1 C17 C171 112.33(13) . .
C173 C17 C171 106.21(14) . .
C172 C17 C171 111.65(13) . .
C17 C171 H17A 109.5 . .
C17 C171 H17B 109.5 . .
H17A C171 H17B 109.5 . .
C17 C171 H17C 109.5 . .
H17A C171 H17C 109.5 . .
H17B C171 H17C 109.5 . .
C17 C172 H17D 109.5 . .
C17 C172 H17E 109.5 . .
H17D C172 H17E 109.5 . .
C17 C172 H17F 109.5 . .
H17D C172 H17F 109.5 . .
H17E C172 H17F 109.5 . .
C17 C173 H17G 109.5 . .
C17 C173 H17H 109.5 . .
H17G C173 H17H 109.5 . .
C17 C173 H17I 109.5 . .
H17G C173 H17I 109.5 . .
H17H C173 H17I 109.5 . .
N121 C121 H12A 109.5 . .
N121 C121 H12B 109.5 . .
H12A C121 H12B 109.5 . .
N121 C121 H12C 109.5 . .
H12A C121 H12C 109.5 . .
H12B C121 H12C 109.5 . .
N121 C122 H12D 109.5 . .
N121 C122 H12E 109.5 . .
H12D C122 H12E 109.5 . .
N121 C122 H12F 109.5 . .
H12D C122 H12F 109.5 . .
H12E C122 H12F 109.5 . .
C21 N2 C27 121.63(13) . .
C21 N2 V1 115.24(10) . .
C27 N2 V1 122.69(10) . .
C22 N221 C221 107.75(13) . .
C22 N221 C222 112.42(16) . .
C221 N221 C222 109.31(16) . .
C22 N221 V1 105.96(10) . .
C221 N221 V1 110.14(12) . .
C222 N221 V1 111.17(10) . .
N2 C21 C26 128.61(14) . .
N2 C21 C22 116.18(14) . .
C26 C21 C22 115.20(14) . .
C23 C22 C21 121.92(17) . .
C23 C22 N221 121.72(16) . .
C21 C22 N221 116.21(14) . .
C22 C23 C24 120.95(19) . .
C22 C23 H23 119.5 . .
C24 C23 H23 119.5 . .
C25 C24 C23 119.53(17) . .
C25 C24 H24 120.2 . .
C23 C24 H24 120.2 . .
C24 C25 C26 119.86(18) . .
C24 C25 C251 120.94(17) . .
C26 C25 C251 119.20(19) . .
C25 C26 C21 122.52(17) . .
C25 C26 H26 118.7 . .
C21 C26 H26 118.7 . .
C25 C251 H25A 109.5 . .
C25 C251 H25B 109.5 . .
H25A C251 H25B 109.5 . .
C25 C251 H25C 109.5 . .
H25A C251 H25C 109.5 . .
H25B C251 H25C 109.5 . .
N2 C27 C271 105.80(13) . .
N2 C27 C273 111.43(15) . .
C271 C27 C273 107.33(16) . .
N2 C27 C272 113.01(16) . .
C271 C27 C272 107.19(16) . .
C273 C27 C272 111.64(16) . .
C27 C271 H27A 109.5 . .
C27 C271 H27B 109.5 . .
H27A C271 H27B 109.5 . .
C27 C271 H27C 109.5 . .
H27A C271 H27C 109.5 . .
H27B C271 H27C 109.5 . .
C27 C272 H27D 109.5 . .
C27 C272 H27E 109.5 . .
H27D C272 H27E 109.5 . .
C27 C272 H27F 109.5 . .
H27D C272 H27F 109.5 . .
H27E C272 H27F 109.5 . .
C27 C273 H27G 109.5 . .
C27 C273 H27H 109.5 . .
H27G C273 H27H 109.5 . .
C27 C273 H27I 109.5 . .
H27G C273 H27I 109.5 . .
H27H C273 H27I 109.5 . .
N221 C221 H22A 109.5 . .
N221 C221 H22B 109.5 . .
H22A C221 H22B 109.5 . .
N221 C221 H22C 109.5 . .
H22A C221 H22C 109.5 . .
H22B C221 H22C 109.5 . .
N221 C222 H22D 109.5 . .
N221 C222 H22E 109.5 . .
H22D C222 H22E 109.5 . .
N221 C222 H22F 109.5 . .
H22D C222 H22F 109.5 . .
H22E C222 H22F 109.5 . .
N3 V2 N3 180.00(14) 3_565 .
N3 V2 N4 98.03(10) 3_565 .
N3 V2 N4 81.97(10) . .
N3 V2 N4 81.97(10) 3_565 3_565
N3 V2 N4 98.03(10) . 3_565
N4 V2 N4 180.0 . 3_565
N3 V2 N6 115.48(14) 3_565 3_565
N3 V2 N6 64.52(14) . 3_565
N4 V2 N6 145.10(14) . 3_565
N4 V2 N6 34.90(14) 3_565 3_565
N3 V2 N6 64.52(14) 3_565 .
N3 V2 N6 115.48(14) . .
N4 V2 N6 34.90(14) . .
N4 V2 N6 145.10(14) 3_565 .
N6 V2 N6 180.00(14) 3_565 .
N3 V2 N5 40.03(15) 3_565 3_565
N3 V2 N5 139.97(15) . 3_565
N4 V2 N5 133.98(15) . 3_565
N4 V2 N5 46.02(15) 3_565 3_565
N6 V2 N5 80.85(18) 3_565 3_565
N6 V2 N5 99.15(18) . 3_565
N3 V2 N5 139.97(15) 3_565 .
N3 V2 N5 40.03(15) . .
N4 V2 N5 46.02(15) . .
N4 V2 N5 133.98(15) 3_565 .
N6 V2 N5 99.15(18) 3_565 .
N6 V2 N5 80.85(18) . .
N5 V2 N5 180.00(19) 3_565 .
N3 V2 Cl3 107.93(9) 3_565 3_565
N3 V2 Cl3 72.07(9) . 3_565
N4 V2 Cl3 88.23(8) . 3_565
N4 V2 Cl3 91.77(8) 3_565 3_565
N6 V2 Cl3 90.33(12) 3_565 3_565
N6 V2 Cl3 89.67(12) . 3_565
N5 V2 Cl3 89.54(14) 3_565 3_565
N5 V2 Cl3 90.46(14) . 3_565
N3 V2 Cl3 72.07(9) 3_565 .
N3 V2 Cl3 107.93(9) . .
N4 V2 Cl3 91.77(8) . .
N4 V2 Cl3 88.23(8) 3_565 .
N6 V2 Cl3 89.67(12) 3_565 .
N6 V2 Cl3 90.33(12) . .
N5 V2 Cl3 90.46(14) 3_565 .
N5 V2 Cl3 89.54(14) . .
Cl3 V2 Cl3 180.0 3_565 .
N3 V2 Cl2 90.54(7) 3_565 3_565
N3 V2 Cl2 89.46(7) . 3_565
N4 V2 Cl2 89.99(7) . 3_565
N4 V2 Cl2 90.01(7) 3_565 3_565
N6 V2 Cl2 98.72(11) 3_565 3_565
N6 V2 Cl2 81.28(11) . 3_565
N5 V2 Cl2 76.00(13) 3_565 3_565
N5 V2 Cl2 104.00(13) . 3_565
Cl3 V2 Cl2 17.40(4) 3_565 3_565
Cl3 V2 Cl2 162.60(4) . 3_565
N3 V2 Cl2 89.46(7) 3_565 .
N3 V2 Cl2 90.54(7) . .
N4 V2 Cl2 90.01(7) . .
N4 V2 Cl2 89.99(7) 3_565 .
N6 V2 Cl2 81.28(11) 3_565 .
N6 V2 Cl2 98.72(11) . .
N5 V2 Cl2 104.00(13) 3_565 .
N5 V2 Cl2 76.00(13) . .
Cl3 V2 Cl2 162.60(4) 3_565 .
Cl3 V2 Cl2 17.40(4) . .
Cl2 V2 Cl2 180.00(3) 3_565 .
C32 N3 C31 105.7(4) . .
C32 N3 C33 110.3(5) . .
C31 N3 C33 106.0(4) . .
C32 N3 V2 116.8(2) . .
C31 N3 V2 115.1(2) . .
C33 N3 V2 102.5(3) . .
C41 N4 C42 106.4(4) . .
C41 N4 C43 119.5(6) . .
C42 N4 C43 95.1(5) . .
C41 N4 C44 92.6(6) . .
C42 N4 C44 122.7(5) . .
C43 N4 C44 32.6(5) . .
C41 N4 V2 116.6(2) . .
C42 N4 V2 116.3(2) . .
C43 N4 V2 101.5(3) . .
C44 N4 V2 100.6(4) . .
N3 C31 H31A 109.5 . .
N3 C31 H31B 109.5 . .
H31A C31 H31B 109.5 . .
N3 C31 H31C 109.5 . .
H31A C31 H31C 109.5 . .
H31B C31 H31C 109.5 . .
N3 C32 H32A 109.5 . .
N3 C32 H32B 109.5 . .
H32A C32 H32B 109.5 . .
N3 C32 H32C 109.5 . .
H32A C32 H32C 109.5 . .
H32B C32 H32C 109.5 . .
C44 C33 C43 36.1(6) . .
C44 C33 N3 124.5(6) . .
C43 C33 N3 120.8(5) . .
C44 C33 H33A 72.2 . .
C43 C33 H33A 107.1 . .
N3 C33 H33A 107.1 . .
C44 C33 H33B 126.6 . .
C43 C33 H33B 107.1 . .
N3 C33 H33B 107.1 . .
H33A C33 H33B 106.8 . .
C33 C43 N4 119.6(7) . .
C33 C43 H43A 107.4 . .
N4 C43 H43A 107.4 . .
C33 C43 H43B 107.4 . .
N4 C43 H43B 107.4 . .
H43A C43 H43B 106.9 . .
N4 C41 H41A 109.5 . .
N4 C41 H41B 109.5 . .
H41A C41 H41B 109.5 . .
N4 C41 H41C 109.5 . .
H41A C41 H41C 109.5 . .
H41B C41 H41C 109.5 . .
N4 C42 H42A 109.5 . .
N4 C42 H42B 109.5 . .
H42A C42 H42B 109.5 . .
N4 C42 H42C 109.5 . .
H42A C42 H42C 109.5 . .
H42B C42 H42C 109.5 . .
C33 C44 N4 119.3(7) . .
C33 C44 H44A 107.5 . .
N4 C44 H44A 107.5 . .
C33 C44 H44B 107.5 . .
N4 C44 H44B 107.5 . .
H44A C44 H44B 107.0 . .
C51 N5 C53 106.7(8) . .
C51 N5 C52 112.6(9) . .
C53 N5 C52 107.2(10) . .
C51 N5 V2 115.7(4) . .
C53 N5 V2 102.0(5) . .
C52 N5 V2 111.7(7) . .
C62 N6 C63 124.8(7) . .
C62 N6 C61 105.9(7) . .
C63 N6 C61 91.8(9) . .
C62 N6 C64 93.2(7) . .
C63 N6 C64 37.8(7) . .
C61 N6 C64 123.5(9) . .
C62 N6 V2 116.6(3) . .
C63 N6 V2 101.4(5) . .
C61 N6 V2 114.1(4) . .
C64 N6 V2 102.5(5) . .
N5 C51 H51D 109.5 . .
N5 C51 H51E 109.5 . .
H51D C51 H51E 109.5 . .
N5 C51 H51F 109.5 . .
H51D C51 H51F 109.5 . .
H51E C51 H51F 109.5 . .
N5 C52 H52D 109.5 . .
N5 C52 H52E 109.5 . .
H52D C52 H52E 109.5 . .
N5 C52 H52F 109.5 . .
H52D C52 H52F 109.5 . .
H52E C52 H52F 109.5 . .
C64 C53 C63 42.0(8) . .
C64 C53 N5 124.5(11) . .
C63 C53 N5 123.5(8) . .
C64 C53 H53C 128.8 . .
C63 C53 H53C 106.5 . .
N5 C53 H53C 106.5 . .
C64 C53 H53D 66.3 . .
C63 C53 H53D 106.5 . .
N5 C53 H53D 106.5 . .
H53C C53 H53D 106.5 . .
C53 C63 N6 116.5(10) . .
C53 C63 H63C 108.2 . .
N6 C63 H63C 108.2 . .
C53 C63 H63D 108.2 . .
N6 C63 H63D 108.2 . .
H63C C63 H63D 107.3 . .
C53 C64 N6 113.5(9) . .
C53 C64 H64A 108.9 . .
N6 C64 H64A 108.9 . .
C53 C64 H64B 108.9 . .
N6 C64 H64B 108.9 . .
H64A C64 H64B 107.7 . .
N6 C61 H61D 109.5 . .
N6 C61 H61E 109.5 . .
H61D C61 H61E 109.5 . .
N6 C61 H61F 109.5 . .
H61D C61 H61F 109.5 . .
H61E C61 H61F 109.5 . .
N6 C62 H62D 109.5 . .
N6 C62 H62E 109.5 . .
H62D C62 H62E 109.5 . .
N6 C62 H62F 109.5 . .
H62D C62 H62F 109.5 . .
H62E C62 H62F 109.5 . .
C3T C2T C7T 119.5(13) . .
C3T C2T C1T 121.5(7) . .
C7T C2T C1T 118.9(12) . .
C4T C3T C2T 121.4(8) . .
C4T C3T H3T 119.3 . .
C2T C3T H3T 119.3 . .
C3T C4T C5T 120.3(8) . .
C3T C4T H4T 119.8 . .
C5T C4T H4T 119.8 . .
C6T C5T C4T 119.2(8) . .
C6T C5T H5T 120.4 . .
C4T C5T H5T 120.4 . .
C5T C6T C7T 121.8(15) . .
C5T C6T H6T 119.1 . .
C7T C6T H6T 119.1 . .
C2T C7T C6T 118(2) . .
C2T C7T H7T 121.2 . .
C6T C7T H7T 121.2 . .
C2T' C1T' H1T4 109.5 . .
C2T' C1T' H1T5 109.5 . .
H1T4 C1T' H1T5 109.5 . .
C2T' C1T' H1T6 109.5 . .
H1T4 C1T' H1T6 109.5 . .
H1T5 C1T' H1T6 109.5 . .
C3T' C2T' C7T' 116.9(7) . .
C3T' C2T' C1T' 120.6(7) . .
C7T' C2T' C1T' 122.5(8) . .
C4T' C3T' C2T' 121.6(7) . .
C4T' C3T' H3T' 119.2 . .
C2T' C3T' H3T' 119.2 . .
C5T' C4T' C3T' 120.7(7) . .
C5T' C4T' H4T' 119.7 . .
C3T' C4T' H4T' 119.7 . .
C4T' C5T' C6T' 118.0(13) . .
C4T' C5T' H5T' 121.0 . .
C6T' C5T' H5T' 121.0 . .
C7T' C6T' C5T' 122(2) . .
C7T' C6T' H6T' 119.0 . .
C5T' C6T' H6T' 119.0 . .
C6T' C7T' C2T' 120.7(14) . .
C6T' C7T' H7T' 119.6 . .
C2T' C7T' H7T' 119.6 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
V1 N1 2.0274(12) .
V1 N2 2.0309(13) .
V1 N221 2.1987(14) .
V1 N121 2.2171(14) .
N1 C11 1.3776(18) .
N1 C17 1.4803(19) .
N121 C12 1.469(2) .
N121 C121 1.485(2) .
N121 C122 1.487(2) .
C11 C16 1.420(2) .
C11 C12 1.424(2) .
C12 C13 1.385(2) .
C13 C14 1.391(3) .
C13 H13 0.9500 .
C14 C15 1.383(3) .
C14 H14 0.9500 .
C15 C16 1.397(2) .
C15 C151 1.513(3) .
C16 H16 0.9500 .
C151 H15A 0.9800 .
C151 H15B 0.9800 .
C151 H15C 0.9800 .
C17 C173 1.533(2) .
C17 C172 1.536(2) .
C17 C171 1.541(2) .
C171 H17A 0.9800 .
C171 H17B 0.9800 .
C171 H17C 0.9800 .
C172 H17D 0.9800 .
C172 H17E 0.9800 .
C172 H17F 0.9800 .
C173 H17G 0.9800 .
C173 H17H 0.9800 .
C173 H17I 0.9800 .
C121 H12A 0.9800 .
C121 H12B 0.9800 .
C121 H12C 0.9800 .
C122 H12D 0.9800 .
C122 H12E 0.9800 .
C122 H12F 0.9800 .
N2 C21 1.3802(19) .
N2 C27 1.4768(19) .
N221 C22 1.470(2) .
N221 C221 1.484(3) .
N221 C222 1.490(2) .
C21 C26 1.420(2) .
C21 C22 1.423(2) .
C22 C23 1.382(2) .
C23 C24 1.390(3) .
C23 H23 0.9500 .
C24 C25 1.379(3) .
C24 H24 0.9500 .
C25 C26 1.398(2) .
C25 C251 1.511(3) .
C26 H26 0.9500 .
C251 H25A 0.9800 .
C251 H25B 0.9800 .
C251 H25C 0.9800 .
C27 C271 1.536(2) .
C27 C273 1.536(3) .
C27 C272 1.540(3) .
C271 H27A 0.9800 .
C271 H27B 0.9800 .
C271 H27C 0.9800 .
C272 H27D 0.9800 .
C272 H27E 0.9800 .
C272 H27F 0.9800 .
C273 H27G 0.9800 .
C273 H27H 0.9800 .
C273 H27I 0.9800 .
C221 H22A 0.9800 .
C221 H22B 0.9800 .
C221 H22C 0.9800 .
C222 H22D 0.9800 .
C222 H22E 0.9800 .
C222 H22F 0.9800 .
V2 N3 2.310(2) 3_565
V2 N3 2.310(2) .
V2 N4 2.312(2) .
V2 N4 2.312(2) 3_565
V2 N6 2.313(4) 3_565
V2 N6 2.313(4) .
V2 N5 2.315(6) 3_565
V2 N5 2.315(6) .
V2 Cl3 2.4739(13) 3_565
V2 Cl3 2.4739(13) .
V2 Cl2 2.4742(7) 3_565
V2 Cl2 2.4742(7) .
N3 C32 1.446(5) .
N3 C31 1.456(4) .
N3 C33 1.468(7) .
N4 C41 1.439(5) .
N4 C42 1.459(5) .
N4 C43 1.462(8) .
N4 C44 1.525(8) .
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 C44 1.323(11) .
C33 C43 1.385(10) .
C33 H33A 0.9900 .
C33 H33B 0.9900 .
C43 H43A 0.9900 .
C43 H43B 0.9900 .
C41 H41A 0.9800 .
C41 H41B 0.9800 .
C41 H41C 0.9800 .
C42 H42A 0.9800 .
C42 H42B 0.9800 .
C42 H42C 0.9800 .
C44 H44A 0.9900 .
C44 H44B 0.9900 .
N5 C51 1.446(8) .
N5 C53 1.448(10) .
N5 C52 1.466(10) .
N6 C62 1.440(7) .
N6 C63 1.457(11) .
N6 C61 1.459(10) .
N6 C64 1.539(11) .
C51 H51D 0.9800 .
C51 H51E 0.9800 .
C51 H51F 0.9800 .
C52 H52D 0.9800 .
C52 H52E 0.9800 .
C52 H52F 0.9800 .
C53 C64 1.341(13) .
C53 C63 1.377(12) .
C53 H53C 0.9900 .
C53 H53D 0.9900 .
C63 H63C 0.9900 .
C63 H63D 0.9900 .
C64 H64A 0.9900 .
C64 H64B 0.9900 .
C61 H61D 0.9800 .
C61 H61E 0.9800 .
C61 H61F 0.9800 .
C62 H62D 0.9800 .
C62 H62E 0.9800 .
C62 H62F 0.9800 .
C1T C2T 1.498(9) .
C1T H1T1 0.9800 .
C1T H1T2 0.9800 .
C1T H1T3 0.9800 .
C2T C3T 1.390(9) .
C2T C7T 1.40(2) .
C3T C4T 1.368(9) .
C3T H3T 0.9500 .
C4T C5T 1.394(9) .
C4T H4T 0.9500 .
C5T C6T 1.355(15) .
C5T H5T 0.9500 .
C6T C7T 1.43(3) .
C6T H6T 0.9500 .
C7T H7T 0.9500 .
C1T' C2T' 1.486(7) .
C1T' H1T4 0.9800 .
C1T' H1T5 0.9800 .
C1T' H1T6 0.9800 .
C2T' C3T' 1.383(9) .
C2T' C7T' 1.400(12) .
C3T' C4T' 1.365(9) .
C3T' H3T' 0.9500 .
C4T' C5T' 1.364(9) .
C4T' H4T' 0.9500 .
C5T' C6T' 1.381(19) .
C5T' H5T' 0.9500 .
C6T' C7T' 1.34(2) .
C6T' H6T' 0.9500 .
C7T' H7T' 0.9500 .
