#------------------------------------------------------------------------------
#$Date: 2016-03-25 12:57:49 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179820 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/16/7011603.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_7011603
loop_
_publ_author_name
'Davies, Sian C.'
'Hughes, David L.'
'Konkol, Martin'
'Richards, Raymond L.'
'Sanders, J. Roger'
'Sobota, Piotr'
_publ_section_title
;
 Synthesis, structure and chemistry of vanadium(iv) and vanadium(v)
 compounds with substituted hydrazido(1--) and hydrazido(2--) ligands
;
_journal_issue                   14
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2811
_journal_paper_doi               10.1039/b202098j
_journal_year                    2002
_chemical_formula_moiety         'C19 H22 N3 S3 V'
_chemical_formula_structural     '[V(N{CH2CH2S}3)(NNCPh2)]'
_chemical_formula_sum            'C19 H22 N3 S3 V'
_chemical_formula_weight         439.52
_chemical_name_common            'complex 3'
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 98.709(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.5275(7)
_cell_length_b                   15.3503(15)
_cell_length_c                   17.491(2)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      11
_cell_measurement_theta_min      10
_cell_volume                     1997.8(4)
_computing_cell_refinement       'CAD4/EXPRESS (Enraf-Nonius, 1992)'
_computing_data_collection       'CAD4/EXPRESS (Enraf-Nonius, 1992)'
_computing_data_reduction        'CAD4 (Hursthouse, 1976)'
_computing_molecular_graphics    'ORTEP (Johnson, 1971)'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf-Nonius CAD4 diffractometer'
_diffrn_measurement_method       'scintillation counter; ω/θ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.022
_diffrn_reflns_av_sigmaI/netI    0.0515
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            6583
_diffrn_reflns_theta_max         30.0
_diffrn_reflns_theta_min         1.5
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  '10000 s'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.818
_exptl_absorpt_correction_T_max  0.996
_exptl_absorpt_correction_T_min  0.903
_exptl_absorpt_correction_type   'semi-empirical psi-scans'
_exptl_crystal_colour            'Blood red'
_exptl_crystal_density_diffrn    1.461
_exptl_crystal_description       'hollow square tubes'
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.293
_refine_diff_density_min         -0.220
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.043
_refine_ls_goodness_of_fit_obs   1.090
_refine_ls_hydrogen_treatment
;
Coordinates were included in idealised positions and subsequently refined 
freely.  Isotropic displacement parameters were refined freely.
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     323
_refine_ls_number_reflns         5814
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_restrained_S_obs      1.090
_refine_ls_R_factor_all          0.0609
_refine_ls_R_factor_obs          0.0369
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0212P)²+0.4907P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0919
_refine_ls_wR_factor_obs         0.0785
_reflns_number_observed          3978
_reflns_number_total             5814
_reflns_observed_criterion       I>2sigma(I)
_cod_data_source_file            b202098j.txt
_cod_data_source_block           roger56
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0212P)^2^+0.4907P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0212P)^2^+0.4907P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1997.8(3)
_cod_original_sg_symbol_H-M      'P 21 / n'
_cod_database_code               7011603
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x+1/2, -y+1/2, z+1/2'
'-x, -y, -z'
'-x-1/2, y-1/2, -z-1/2'
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
V V 0.18242(4) 0.40817(2) 0.15845(2) 0.03121(9) Uani 1 d . .
S1 S 0.35044(7) 0.52526(4) 0.13590(3) 0.04514(14) Uani 1 d . .
S2 S 0.18615(8) 0.36587(4) 0.28292(3) 0.04828(15) Uani 1 d . .
S3 S -0.04577(8) 0.36523(4) 0.06746(3) 0.04542(14) Uani 1 d . .
N4 N -0.0125(2) 0.50745(10) 0.18679(9) 0.0320(3) Uani 1 d . .
C14 C 0.2040(3) 0.61558(14) 0.15162(14) 0.0426(5) Uani 1 d . .
H14A H 0.2762(33) 0.6651(16) 0.1698(14) 0.056(7) Uiso 1 d . .
H14B H 0.1359(33) 0.6331(16) 0.1020(15) 0.055(7) Uiso 1 d . .
C41 C 0.0828(3) 0.59049(13) 0.20917(13) 0.0390(4) Uani 1 d . .
H41A H 0.1508(27) 0.5821(13) 0.2605(12) 0.034(5) Uiso 1 d . .
H41B H -0.0031(30) 0.6353(15) 0.2098(13) 0.047(6) Uiso 1 d . .
C24 C 0.0338(4) 0.4432(2) 0.31808(13) 0.0498(6) Uani 1 d . .
H24A H -0.0220(37) 0.4144(17) 0.3549(16) 0.066(8) Uiso 1 d . .
H24B H 0.1066(36) 0.4906(18) 0.3463(15) 0.068(8) Uiso 1 d . .
C42 C -0.1010(3) 0.4767(2) 0.25262(14) 0.0446(5) Uani 1 d . .
H42A H -0.1846(32) 0.4286(16) 0.2314(14) 0.054(7) Uiso 1 d . .
H42B H -0.1674(31) 0.5253(16) 0.2669(14) 0.053(7) Uiso 1 d . .
C34 C -0.2268(3) 0.4390(2) 0.0824(2) 0.0485(5) Uani 1 d . .
H34A H -0.2965(37) 0.4484(18) 0.0342(17) 0.068(8) Uiso 1 d . .
H34B H -0.3084(35) 0.4097(16) 0.1146(15) 0.058(7) Uiso 1 d . .
C43 C -0.1525(3) 0.52320(15) 0.11780(14) 0.0424(5) Uani 1 d . .
H43A H -0.0946(31) 0.5579(15) 0.0811(13) 0.047(6) Uiso 1 d . .
H43B H -0.2483(34) 0.5611(16) 0.1328(14) 0.056(7) Uiso 1 d . .
N5 N 0.3343(2) 0.33129(11) 0.14346(9) 0.0365(4) Uani 1 d . .
N6 N 0.4657(2) 0.27458(11) 0.14845(9) 0.0365(4) Uani 1 d . .
C6 C 0.4930(2) 0.22803(11) 0.08885(10) 0.0303(4) Uani 1 d . .
C611 C 0.6487(2) 0.16884(12) 0.09993(10) 0.0311(4) Uani 1 d . .
C612 C 0.7918(3) 0.18251(15) 0.15885(12) 0.0407(5) Uani 1 d . .
H612 H 0.7906(29) 0.2323(15) 0.1884(13) 0.044(6) Uiso 1 d . .
C613 C 0.9334(3) 0.1249(2) 0.17019(15) 0.0526(6) Uani 1 d . .
H613 H 1.0265(38) 0.1357(18) 0.2109(16) 0.073(9) Uiso 1 d . .
C614 C 0.9362(3) 0.0528(2) 0.1237(2) 0.0559(6) Uani 1 d . .
H614 H 1.0273(36) 0.0104(17) 0.1327(15) 0.065(8) Uiso 1 d . .
C615 C 0.7979(4) 0.0389(2) 0.0643(2) 0.0547(6) Uani 1 d . .
H615 H 0.7948(33) -0.0097(18) 0.0297(15) 0.063(8) Uiso 1 d . .
C616 C 0.6542(3) 0.09675(14) 0.05185(13) 0.0420(5) Uani 1 d . .
H616 H 0.5643(28) 0.0884(13) 0.0116(12) 0.033(5) Uiso 1 d . .
C621 C 0.3739(3) 0.22987(12) 0.01321(10) 0.0326(4) Uani 1 d . .
C622 C 0.1956(3) 0.20438(14) 0.00677(13) 0.0433(5) Uani 1 d . .
H622 H 0.1478(30) 0.1899(15) 0.0515(13) 0.048(7) Uiso 1 d . .
C623 C 0.0916(4) 0.1985(2) -0.0655(2) 0.0546(6) Uani 1 d . .
H623 H -0.0174(35) 0.1803(17) -0.0666(14) 0.057(8) Uiso 1 d . .
C624 C 0.1620(4) 0.2188(2) -0.13082(14) 0.0557(7) Uani 1 d . .
H624 H 0.0843(35) 0.2122(17) -0.1824(15) 0.069(8) Uiso 1 d . .
C625 C 0.3367(4) 0.2478(2) -0.12453(13) 0.0584(7) Uani 1 d . .
H625 H 0.3881(34) 0.2596(17) -0.1719(15) 0.064(8) Uiso 1 d . .
C626 C 0.4437(3) 0.2523(2) -0.05306(13) 0.0462(5) Uani 1 d . .
H626 H 0.5549(31) 0.2680(15) -0.0488(13) 0.047(7) Uiso 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 0.0000 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'
S S 0.1246 0.1234 '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
N5 V N4 176.08(7) . . ?
N5 V S3 98.46(6) . . ?
N4 V S3 84.26(5) . . ?
N5 V S1 96.79(6) . . ?
N4 V S1 84.24(4) . . ?
S3 V S1 119.62(3) . . ?
N5 V S2 92.22(6) . . ?
N4 V S2 83.97(4) . . ?
S3 V S2 119.41(3) . . ?
S1 V S2 117.90(3) . . ?
C14 S1 V 102.20(7) . . ?
C24 S2 V 102.74(8) . . ?
C34 S3 V 102.93(8) . . ?
C41 N4 C42 108.8(2) . . ?
C41 N4 C43 109.1(2) . . ?
C42 N4 C43 109.3(2) . . ?
C41 N4 V 109.77(11) . . ?
C42 N4 V 110.00(12) . . ?
C43 N4 V 109.82(12) . . ?
C41 C14 S1 110.38(15) . . ?
C41 C14 H14A 110.5(15) . . ?
S1 C14 H14A 109.1(15) . . ?
C41 C14 H14B 112.0(14) . . ?
S1 C14 H14B 108.9(14) . . ?
H14A C14 H14B 105.8(20) . . ?
N4 C41 C14 111.1(2) . . ?
N4 C41 H41A 107.2(12) . . ?
C14 C41 H41A 111.3(12) . . ?
N4 C41 H41B 108.9(14) . . ?
C14 C41 H41B 107.8(13) . . ?
H41A C41 H41B 110.5(18) . . ?
C42 C24 S2 110.7(2) . . ?
C42 C24 H24A 111.4(17) . . ?
S2 C24 H24A 107.2(16) . . ?
C42 C24 H24B 112.7(16) . . ?
S2 C24 H24B 108.5(16) . . ?
H24A C24 H24B 106.1(22) . . ?
N4 C42 C24 111.6(2) . . ?
N4 C42 H42A 106.0(14) . . ?
C24 C42 H42A 110.2(14) . . ?
N4 C42 H42B 105.5(14) . . ?
C24 C42 H42B 112.9(14) . . ?
H42A C42 H42B 110.4(19) . . ?
C43 C34 S3 110.7(2) . . ?
C43 C34 H34A 111.2(17) . . ?
S3 C34 H34A 107.3(17) . . ?
C43 C34 H34B 112.1(14) . . ?
S3 C34 H34B 109.7(14) . . ?
H34A C34 H34B 105.6(22) . . ?
N4 C43 C34 111.5(2) . . ?
N4 C43 H43A 106.6(13) . . ?
C34 C43 H43A 111.7(13) . . ?
N4 C43 H43B 109.5(14) . . ?
C34 C43 H43B 111.9(14) . . ?
H43A C43 H43B 105.4(19) . . ?
N6 N5 V 167.00(14) . . ?
C6 N6 N5 121.2(2) . . ?
N6 C6 C611 116.8(2) . . ?
N6 C6 C621 123.8(2) . . ?
C611 C6 C621 119.4(2) . . ?
C612 C611 C616 118.5(2) . . ?
C612 C611 C6 121.1(2) . . ?
C616 C611 C6 120.4(2) . . ?
C613 C612 C611 120.4(2) . . ?
C613 C612 H612 121.6(14) . . ?
C611 C612 H612 117.9(14) . . ?
C614 C613 C612 120.9(2) . . ?
C614 C613 H613 121.1(17) . . ?
C612 C613 H613 118.0(17) . . ?
C615 C614 C613 119.7(2) . . ?
C615 C614 H614 118.0(16) . . ?
C613 C614 H614 122.2(16) . . ?
C614 C615 C616 120.2(2) . . ?
C614 C615 H615 122.8(15) . . ?
C616 C615 H615 117.0(16) . . ?
C615 C616 C611 120.4(2) . . ?
C615 C616 H616 120.1(13) . . ?
C611 C616 H616 119.5(13) . . ?
C622 C621 C626 119.1(2) . . ?
C622 C621 C6 120.9(2) . . ?
C626 C621 C6 119.8(2) . . ?
C623 C622 C621 119.9(2) . . ?
C623 C622 H622 120.7(14) . . ?
C621 C622 H622 119.3(14) . . ?
C624 C623 C622 120.7(2) . . ?
C624 C623 H623 122.9(17) . . ?
C622 C623 H623 116.4(17) . . ?
C623 C624 C625 119.6(2) . . ?
C623 C624 H624 118.8(15) . . ?
C625 C624 H624 121.6(15) . . ?
C624 C625 C626 120.5(2) . . ?
C624 C625 H625 119.0(15) . . ?
C626 C625 H625 120.2(15) . . ?
C625 C626 C621 120.1(2) . . ?
C625 C626 H626 121.1(16) . . ?
C621 C626 H626 118.8(16) . . ?
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
V N5 1.691(2) . ?
V N4 2.2229(15) . ?
V S3 2.2562(7) . ?
V S1 2.2665(6) . ?
V S2 2.2679(7) . ?
S1 C14 1.818(2) . ?
S2 C24 1.821(2) . ?
S3 C34 1.821(2) . ?
N4 C41 1.486(3) . ?
N4 C42 1.492(2) . ?
N4 C43 1.497(3) . ?
C14 C41 1.507(3) . ?
C14 H14A 0.96(3) . ?
C14 H14B 0.98(2) . ?
C41 H41A 0.97(2) . ?
C41 H41B 0.95(2) . ?
C24 C42 1.501(3) . ?
C24 H24A 0.93(3) . ?
C24 H24B 1.00(3) . ?
C42 H42A 1.00(2) . ?
C42 H42B 0.95(2) . ?
C34 C43 1.504(3) . ?
C34 H34A 0.93(3) . ?
C34 H34B 1.00(3) . ?
C43 H43A 0.98(2) . ?
C43 H43B 0.99(2) . ?
N5 N6 1.311(2) . ?
N6 C6 1.306(2) . ?
C6 C611 1.473(2) . ?
C6 C621 1.482(3) . ?
C611 C612 1.389(3) . ?
C611 C616 1.394(3) . ?
C612 C613 1.376(3) . ?
C612 H612 0.92(2) . ?
C613 C614 1.375(4) . ?
C613 H613 0.94(3) . ?
C614 C615 1.372(4) . ?
C614 H614 0.94(3) . ?
C615 C616 1.390(3) . ?
C615 H615 0.96(3) . ?
C616 H616 0.91(2) . ?
C621 C622 1.386(3) . ?
C621 C626 1.386(3) . ?
C622 C623 1.386(3) . ?
C622 H622 0.94(2) . ?
C623 C624 1.367(4) . ?
C623 H623 0.86(3) . ?
C624 C625 1.377(4) . ?
C624 H624 1.00(3) . ?
C625 C626 1.382(3) . ?
C625 H625 0.98(3) . ?
C626 H626 0.86(2) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
V S1 C14 C41 28.8(2) . . . . ?
S1 C14 C41 N4 -51.9(2) . . . . ?
C14 C41 N4 V 48.5(2) . . . . ?
V S2 C24 C42 26.5(2) . . . . ?
S2 C24 C42 N4 -49.8(2) . . . . ?
C24 C42 N4 V 48.2(2) . . . . ?
V S3 C34 C43 26.4(2) . . . . ?
S3 C34 C43 N4 -49.5(2) . . . . ?
C34 C43 N4 V 47.8(2) . . . . ?
V N5 N6 C6 179.1(6) . . . . ?
