#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/79/7007971.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_7007971
loop_
_publ_author_name
'Tajika, Yasunobu'
'Tsuge, Kiyoshi'
'Sasaki, Yoichi'
_publ_section_title
;
 Mononuclear oxovanadium complexes of tris(2-pyridylmethyl)amine.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1438
_journal_page_last               1447
_journal_paper_doi               10.1039/b414532a
_journal_year                    2005
_chemical_formula_sum            'C20 H26 N4 O7 S V'
_chemical_formula_weight         517.45
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_cell_angle_alpha                90
_cell_angle_beta                 108.883(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.583(3)
_cell_length_b                   13.466(3)
_cell_length_c                   15.253(4)
_cell_measurement_reflns_used    8326
_cell_measurement_temperature    153.1
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.9
_cell_volume                     2251.1(10)
_computing_cell_refinement       CRYSTALCLEAR
_computing_data_collection       CRYSTALCLEAR
_computing_data_reduction        'teXsan Ver. 1.11'
_computing_publication_material  'teXsan Ver. 1.11'
_computing_structure_refinement  'teXsan Ver. 1.10'
_computing_structure_solution    MULTAN88
_diffrn_ambient_temperature      153.1500
_diffrn_detector_area_resol_mean 14.6199
_diffrn_measured_fraction_theta_full 85.1000
_diffrn_measured_fraction_theta_max 27.4835
_diffrn_measurement_details
;
scan:
Number of images: 360
Slice: -76.0000 - 104.0000
Image width: 0.5000
Exp time: 45.0000
Rotation axis: Omega
Omega: 0.0000
Chi: 45.0000
Phi: 0.0000
XTD: 40.7558
2theta: 14.0669
scan:
Number of images: 120
Slice: -16.0000 - 44.0000
Image width: 0.5000
Exp time: 45.0000
Rotation axis: Omega
Omega: 0.0000
Chi: 45.0000
Phi: 90.0000
XTD: 40.7558
2theta: 14.0669
;
_diffrn_measurement_device
;
Mercury CCD (2x2 bin mode)
;
_diffrn_measurement_device_details
;
AFC8: Eulerian 3-circle
;
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_source         'Sealed Tube'
_diffrn_radiation_type           Molybdenum
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0140
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        27.4835
_diffrn_reflns_theta_max         27.4835
_diffrn_reflns_theta_min         3.8737
_diffrn_source_current           50.0000
_diffrn_source_power             2.5000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    0.583
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7548
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.527
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_size_max          0.72
_exptl_crystal_size_mid          0.41
_exptl_crystal_size_min          0.33
_refine_diff_density_max         0.73
_refine_diff_density_min         -0.43
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.629
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     298
_refine_ls_number_reflns         4385
_refine_ls_R_factor_gt           0.0448
_refine_ls_shift/su_max          0.0008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²) + (0.08000(Max(Fo²,0) + 2Fc²)/3)²]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1507
_reflns_number_gt                4085
_reflns_number_total             4385
_reflns_threshold_expression     F²>2.0σ(F²)
_cod_data_source_file            b414532a.txt
_cod_data_source_block           '[VO(SO4)(tpa)]'
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' 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 
;
_cod_original_cell_volume        2251.1(9)
_cod_original_formula_sum        'C20 H26 N4 O7 S V '
_cod_database_code               7007971
#BEGIN Tags that were not found in dictionaries:
_diffrn_number_total             11166
_diffrn_reflns_av_sigmai/deti    0.0294
#END Tags that were not found in dictionaries
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,1/2+y,1/2-z
-x,-y,-z
x,1/2-y,1/2+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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
V(1) V 0.43259(2) 0.08557(2) 0.32894(2) 0.0141(1) Uani 1.00 d . . .
S(1) S 0.69304(4) 0.08478(3) 0.30307(3) 0.0193(1) Uani 1.00 d . . .
O(1) O 0.4628(1) -0.00899(9) 0.39560(8) 0.0214(3) Uani 1.00 d . . .
O(2) O 0.5526(1) 0.08383(9) 0.26380(9) 0.0215(3) Uani 1.00 d . . .
O(3) O 0.7328(1) -0.0061(1) 0.2703(1) 0.0443(5) Uani 1.00 d . . .
O(4) O 0.7346(1) 0.17299(10) 0.26809(9) 0.0279(3) Uani 1.00 d . . .
O(5) O 0.7279(1) 0.0848(1) 0.4039(1) 0.0370(4) Uani 1.00 d . . .
O(7) O 0.1121(2) 0.0179(1) 0.8292(1) 0.0396(4) Uani 1.00 d . . .
O(8) O 0.8842(2) 0.2937(1) 0.0333(1) 0.0445(5) Uani 1.00 d . . .
N(1) N 0.3456(1) 0.21310(10) 0.23133(9) 0.0171(3) Uani 1.00 d . . .
N(2) N 0.5124(1) 0.21350(10) 0.40486(10) 0.0171(3) Uani 1.00 d . . .
N(3) N 0.2823(1) 0.12858(10) 0.37266(9) 0.0163(3) Uani 1.00 d . . .
N(4) N 0.3091(1) 0.0171(1) 0.21118(9) 0.0170(3) Uani 1.00 d . . .
C(1) C 0.4395(2) 0.2933(1) 0.2555(1) 0.0188(4) Uani 1.00 d . . .
C(2) C 0.4927(1) 0.3011(1) 0.3586(1) 0.0178(4) Uani 1.00 d . . .
C(3) C 0.5258(2) 0.3907(1) 0.4044(1) 0.0224(4) Uani 1.00 d . . .
C(4) C 0.5841(2) 0.3900(1) 0.4997(1) 0.0260(4) Uani 1.00 d . . .
C(5) C 0.6062(2) 0.3002(1) 0.5465(1) 0.0244(4) Uani 1.00 d . . .
C(6) C 0.5675(2) 0.2135(1) 0.4973(1) 0.0213(4) Uani 1.00 d . . .
C(7) C 0.2300(1) 0.2464(1) 0.2438(1) 0.0204(4) Uani 1.00 d . . .
C(8) C 0.2113(1) 0.2058(1) 0.3303(1) 0.0179(4) Uani 1.00 d . . .
C(9) C 0.1205(2) 0.2428(1) 0.3623(1) 0.0220(4) Uani 1.00 d . . .
C(10) C 0.0987(2) 0.1979(1) 0.4368(1) 0.0240(4) Uani 1.00 d . . .
C(11) C 0.1707(2) 0.1175(1) 0.4798(1) 0.0228(4) Uani 1.00 d . . .
C(12) C 0.2622(2) 0.0864(1) 0.4466(1) 0.0194(4) Uani 1.00 d . . .
C(13) C 0.3251(2) 0.1731(1) 0.1374(1) 0.0208(4) Uani 1.00 d . . .
C(14) C 0.2711(2) 0.0703(1) 0.1316(1) 0.0176(4) Uani 1.00 d . . .
C(15) C 0.1923(2) 0.0307(1) 0.0502(1) 0.0238(4) Uani 1.00 d . . .
C(16) C 0.1529(2) -0.0668(1) 0.0505(1) 0.0268(5) Uani 1.00 d . . .
C(17) C 0.1919(2) -0.1212(1) 0.1322(1) 0.0244(4) Uani 1.00 d . . .
C(18) C 0.2690(2) -0.0772(1) 0.2105(1) 0.0199(4) Uani 1.00 d . . .
C(19) C 0.0237(2) -0.0559(2) 0.7905(2) 0.0348(5) Uani 1.00 d . . .
C(20) C 0.9004(2) 0.3451(2) 0.1153(2) 0.0514(7) Uani 1.00 d . . .
H(1) H 0.5022 0.2780 0.2301 0.0226 Uiso 1.00 calc . . .
H(2) H 0.4027 0.3547 0.2309 0.0226 Uiso 1.00 calc . . .
H(3) H 0.5090 0.4516 0.3713 0.0269 Uiso 1.00 calc . . .
H(4) H 0.6086 0.4506 0.5324 0.0312 Uiso 1.00 calc . . .
H(5) H 0.6473 0.2983 0.6114 0.0293 Uiso 1.00 calc . . .
H(6) H 0.5801 0.1521 0.5297 0.0255 Uiso 1.00 calc . . .
H(7) H 0.2305 0.3169 0.2470 0.0245 Uiso 1.00 calc . . .
H(8) H 0.1640 0.2252 0.1918 0.0245 Uiso 1.00 calc . . .
H(9) H 0.0736 0.2987 0.3331 0.0264 Uiso 1.00 calc . . .
H(10) H 0.0354 0.2214 0.4585 0.0288 Uiso 1.00 calc . . .
H(11) H 0.1571 0.0849 0.5309 0.0274 Uiso 1.00 calc . . .
H(12) H 0.3131 0.0330 0.4770 0.0233 Uiso 1.00 calc . . .
H(13) H 0.2704 0.2151 0.0930 0.0249 Uiso 1.00 calc . . .
H(14) H 0.4005 0.1698 0.1254 0.0249 Uiso 1.00 calc . . .
H(15) H 0.1657 0.0695 -0.0047 0.0286 Uiso 1.00 calc . . .
H(16) H 0.1000 -0.0959 -0.0046 0.0322 Uiso 1.00 calc . . .
H(17) H 0.1655 -0.1878 0.1338 0.0293 Uiso 1.00 calc . . .
H(18) H 0.2951 -0.1145 0.2664 0.0239 Uiso 1.00 calc . . .
H(19) H -0.0435 -0.0271 0.7440 0.0417 Uiso 1.00 calc . . .
H(20) H 0.0586 -0.1066 0.7638 0.0417 Uiso 1.00 calc . . .
H(21) H -0.0035 -0.0836 0.8376 0.0417 Uiso 1.00 calc . . .
H(22) H 0.8992 0.2997 0.1627 0.0617 Uiso 1.00 calc . . .
H(23) H 0.9767 0.3786 0.1328 0.0617 Uiso 1.00 calc . . .
H(24) H 0.8365 0.3921 0.1066 0.0617 Uiso 1.00 calc . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.003 0.002
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
H H 0.000 0.000
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.2)
;
N N 0.006 0.003
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
O O 0.011 0.006
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
S S 0.125 0.123
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
V V 0.300 0.529
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O(1) V(1) O(2) 105.61(6) . . . yes
O(1) V(1) N(1) 167.24(6) . . . yes
O(1) V(1) N(2) 109.53(6) . . . yes
O(1) V(1) N(3) 92.88(6) . . . yes
O(1) V(1) N(4) 98.15(6) . . . yes
O(2) V(1) N(1) 85.05(5) . . . yes
O(2) V(1) N(2) 91.80(5) . . . yes
O(2) V(1) N(3) 161.51(5) . . . yes
O(2) V(1) N(4) 87.70(5) . . . yes
N(1) V(1) N(2) 76.50(5) . . . yes
N(1) V(1) N(3) 76.55(5) . . . yes
N(1) V(1) N(4) 74.90(5) . . . yes
N(2) V(1) N(3) 82.19(5) . . . yes
N(2) V(1) N(4) 151.34(5) . . . yes
N(3) V(1) N(4) 89.31(5) . . . yes
O(2) S(1) O(3) 105.75(8) . . . yes
O(2) S(1) O(4) 107.39(8) . . . yes
O(2) S(1) O(5) 107.89(8) . . . yes
O(3) S(1) O(4) 112.65(10) . . . yes
O(3) S(1) O(5) 110.6(1) . . . yes
O(4) S(1) O(5) 112.17(9) . . . yes
V(1) O(2) S(1) 129.63(8) . . . yes
V(1) N(1) C(1) 104.56(9) . . . yes
V(1) N(1) C(7) 111.72(10) . . . yes
V(1) N(1) C(13) 104.89(10) . . . yes
C(1) N(1) C(7) 111.5(1) . . . yes
C(1) N(1) C(13) 112.3(1) . . . yes
C(7) N(1) C(13) 111.5(1) . . . yes
V(1) N(2) C(2) 117.0(1) . . . yes
V(1) N(2) C(6) 123.3(1) . . . yes
C(2) N(2) C(6) 119.2(1) . . . yes
V(1) N(3) C(8) 119.4(1) . . . yes
V(1) N(3) C(12) 121.7(1) . . . yes
C(8) N(3) C(12) 118.7(1) . . . yes
V(1) N(4) C(14) 117.7(1) . . . yes
V(1) N(4) C(18) 123.6(1) . . . yes
C(14) N(4) C(18) 118.7(1) . . . yes
N(1) C(1) C(2) 109.2(1) . . . yes
N(1) C(1) H(1) 109.5 . . . no
N(1) C(1) H(2) 109.5 . . . no
C(2) C(1) H(1) 109.5 . . . no
C(2) C(1) H(2) 109.5 . . . no
H(1) C(1) H(2) 109.5 . . . no
N(2) C(2) C(1) 115.4(1) . . . yes
N(2) C(2) C(3) 121.5(2) . . . yes
C(1) C(2) C(3) 123.0(1) . . . yes
C(2) C(3) C(4) 119.0(2) . . . yes
C(2) C(3) H(3) 120.5 . . . no
C(4) C(3) H(3) 120.5 . . . no
C(3) C(4) C(5) 119.3(2) . . . yes
C(3) C(4) H(4) 120.3 . . . no
C(5) C(4) H(4) 120.3 . . . no
C(4) C(5) C(6) 119.0(2) . . . yes
C(4) C(5) H(5) 120.5 . . . no
C(6) C(5) H(5) 120.5 . . . no
N(2) C(6) C(5) 121.9(2) . . . yes
N(2) C(6) H(6) 119.0 . . . no
C(5) C(6) H(6) 119.0 . . . no
N(1) C(7) C(8) 113.2(1) . . . yes
N(1) C(7) H(7) 108.5 . . . no
N(1) C(7) H(8) 108.5 . . . no
C(8) C(7) H(7) 108.5 . . . no
C(8) C(7) H(8) 108.5 . . . no
H(7) C(7) H(8) 109.5 . . . no
N(3) C(8) C(7) 117.3(1) . . . yes
N(3) C(8) C(9) 121.4(2) . . . yes
C(7) C(8) C(9) 121.2(1) . . . yes
C(8) C(9) C(10) 119.5(2) . . . yes
C(8) C(9) H(9) 120.2 . . . no
C(10) C(9) H(9) 120.2 . . . no
C(9) C(10) C(11) 119.1(2) . . . yes
C(9) C(10) H(10) 120.4 . . . no
C(11) C(10) H(10) 120.4 . . . no
C(10) C(11) C(12) 118.5(2) . . . yes
C(10) C(11) H(11) 120.8 . . . no
C(12) C(11) H(11) 120.8 . . . no
N(3) C(12) C(11) 122.7(2) . . . yes
N(3) C(12) H(12) 118.7 . . . no
C(11) C(12) H(12) 118.6 . . . no
N(1) C(13) C(14) 109.0(1) . . . yes
N(1) C(13) H(13) 109.6 . . . no
N(1) C(13) H(14) 109.6 . . . no
C(14) C(13) H(13) 109.6 . . . no
C(14) C(13) H(14) 109.6 . . . no
H(13) C(13) H(14) 109.5 . . . no
N(4) C(14) C(13) 115.2(1) . . . yes
N(4) C(14) C(15) 121.8(2) . . . yes
C(13) C(14) C(15) 123.0(2) . . . yes
C(14) C(15) C(16) 118.8(2) . . . yes
C(14) C(15) H(15) 120.6 . . . no
C(16) C(15) H(15) 120.6 . . . no
C(15) C(16) C(17) 119.3(2) . . . yes
C(15) C(16) H(16) 120.4 . . . no
C(17) C(16) H(16) 120.4 . . . no
C(16) C(17) C(18) 119.0(2) . . . yes
C(16) C(17) H(17) 120.5 . . . no
C(18) C(17) H(17) 120.5 . . . no
N(4) C(18) C(17) 122.5(2) . . . yes
N(4) C(18) H(18) 118.8 . . . no
C(17) C(18) H(18) 118.8 . . . no
O(7) C(19) H(19) 109.5 . . . no
O(7) C(19) H(20) 109.5 . . . no
O(7) C(19) H(21) 109.5 . . . no
H(19) C(19) H(20) 109.5 . . . no
H(19) C(19) H(21) 109.5 . . . no
H(20) C(19) H(21) 109.5 . . . no
O(8) C(20) H(22) 109.5 . . . no
O(8) C(20) H(23) 109.5 . . . no
O(8) C(20) H(24) 109.5 . . . no
H(22) C(20) H(23) 109.5 . . . no
H(22) C(20) H(24) 109.5 . . . no
H(23) C(20) H(24) 109.5 . . . no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V(1) O(1) 1.596(1) . . yes
V(1) O(2) 1.953(1) . . yes
V(1) N(1) 2.282(1) . . yes
V(1) N(2) 2.114(1) . . yes
V(1) N(3) 2.136(1) . . yes
V(1) N(4) 2.112(1) . . yes
S(1) O(2) 1.541(1) . . yes
S(1) O(3) 1.452(1) . . yes
S(1) O(4) 1.447(1) . . yes
S(1) O(5) 1.459(2) . . yes
O(7) C(19) 1.412(3) . . yes
O(8) C(20) 1.388(3) . . yes
N(1) C(1) 1.492(2) . . yes
N(1) C(7) 1.483(2) . . yes
N(1) C(13) 1.476(2) . . yes
N(2) C(2) 1.355(2) . . yes
N(2) C(6) 1.347(2) . . yes
N(3) C(8) 1.353(2) . . yes
N(3) C(12) 1.349(2) . . yes
N(4) C(14) 1.355(2) . . yes
N(4) C(18) 1.350(2) . . yes
C(1) C(2) 1.496(2) . . yes
C(1) H(1) 0.950 . . no
C(1) H(2) 0.950 . . no
C(2) C(3) 1.385(2) . . yes
C(3) C(4) 1.390(3) . . yes
C(3) H(3) 0.950 . . no
C(4) C(5) 1.386(3) . . yes
C(4) H(4) 0.950 . . no
C(5) C(6) 1.382(2) . . yes
C(5) H(5) 0.950 . . no
C(6) H(6) 0.950 . . no
C(7) C(8) 1.507(2) . . yes
C(7) H(7) 0.950 . . no
C(7) H(8) 0.950 . . no
C(8) C(9) 1.388(2) . . yes
C(9) C(10) 1.382(3) . . yes
C(9) H(9) 0.950 . . no
C(10) C(11) 1.395(3) . . yes
C(10) H(10) 0.950 . . no
C(11) C(12) 1.380(2) . . yes
C(11) H(11) 0.950 . . no
C(12) H(12) 0.950 . . no
C(13) C(14) 1.509(2) . . yes
C(13) H(13) 0.950 . . no
C(13) H(14) 0.950 . . no
C(14) C(15) 1.388(2) . . yes
C(15) C(16) 1.390(3) . . yes
C(15) H(15) 0.950 . . no
C(16) C(17) 1.389(3) . . yes
C(16) H(16) 0.950 . . no
C(17) C(18) 1.374(3) . . yes
C(17) H(17) 0.950 . . no
C(18) H(18) 0.950 . . no
C(19) H(19) 0.950 . . no
C(19) H(20) 0.950 . . no
C(19) H(21) 0.950 . . no
C(20) H(22) 0.950 . . no
C(20) H(23) 0.950 . . no
C(20) H(24) 0.950 . . no
