#------------------------------------------------------------------------------
#$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $
#$Revision: 25271 $
#$URL: svn://www.crystallography.net/cod/cif/2/2006242.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2006242
loop_
_publ_author_name
'Kanamori, K.'
'Miyazaki, K.'
'Okamoto, K.-I.'
_publ_contact_author
;
KAN KANAMORI
Department of Chemistry,
Faculty of Science,
Toyama University,
Gofuku 3190, Toyama 930, Japan
;
_publ_section_title
;
Sodium
(N-Ethylethylenediamine-N,N',N'-triacetato)oxovanadium(IV)
Trihydrate
;
_journal_issue 6
_journal_name_full 'Acta Crystallographica Section C'
_journal_page_first 673
_journal_page_last 675
_journal_volume 53
_journal_year 1997
_chemical_formula_iupac 'Na[V O (C10 H15 N2 O6)] , 3H2 O'
_chemical_formula_moiety 'C10 H21 N2 Na O10 V'
_chemical_formula_sum 'C10 H21 N2 Na O10 V'
_chemical_formula_weight 403.21
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2yab'
_symmetry_space_group_name_H-M 'P 1 21/a 1'
_cell_angle_alpha 90
_cell_angle_beta 101.400(10)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 17.329(5)
_cell_length_b 13.631(3)
_cell_length_c 6.943(2)
_cell_measurement_reflns_used 25
_cell_measurement_temperature 296
_cell_measurement_theta_max 25.0
_cell_measurement_theta_min 21.0
_cell_volume 1607.7(7)
_computing_cell_refinement 'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_collection 'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_reduction
'TEXSAN (Molecular Structure Corporation, 1995)'
_computing_molecular_graphics TEXSAN
_computing_publication_material TEXSAN
_computing_structure_refinement TEXSAN
_computing_structure_solution TEXSAN
_diffrn_ambient_temperature 296
_diffrn_measurement_device 'Enraf Nonius CAD-4'
_diffrn_measurement_method '\w/2\q scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'Enraf Nonius sealed tube'
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.7107
_diffrn_reflns_av_R_equivalents 1.93
_diffrn_reflns_av_sigmaI/netI 0.033
_diffrn_reflns_limit_h_max 24
_diffrn_reflns_limit_h_min 0
_diffrn_reflns_limit_k_max 19
_diffrn_reflns_limit_k_min -19
_diffrn_reflns_limit_l_max 9
_diffrn_reflns_limit_l_min -9
_diffrn_reflns_number 10101
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max 30.00
_diffrn_reflns_theta_min 1.00
_diffrn_standards_decay_% 0.75
_diffrn_standards_interval_count 120
_diffrn_standards_number 3
_exptl_absorpt_coefficient_mu 0.698
_exptl_absorpt_correction_T_max 0.882
_exptl_absorpt_correction_T_min 0.816
_exptl_absorpt_correction_type '\y scan'
_exptl_crystal_colour blue
_exptl_crystal_density_diffrn 1.666
_exptl_crystal_density_meas 'not measured'
_exptl_crystal_description column
_exptl_crystal_F_000 836.00
_exptl_crystal_size_max 0.450
_exptl_crystal_size_mid 0.400
_exptl_crystal_size_min 0.180
_refine_diff_density_max 0.48
_refine_diff_density_min -0.28
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_obs 1.398
_refine_ls_hydrogen_treatment 'noref and water H atoms not located'
_refine_ls_matrix_type full
_refine_ls_number_constraints 0
_refine_ls_number_parameters 217
_refine_ls_number_reflns 4120
_refine_ls_number_restraints 0
_refine_ls_R_factor_obs 0.0381
_refine_ls_shift/esd_max 0.0010
_refine_ls_shift/esd_mean 0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.00063|Fo|^2^]'
_refine_ls_wR_factor_obs 0.0617
_reflns_number_observed 4120
_reflns_number_total 6025
_reflns_observed_criterion >1.5\s(I)
_[local]_cod_data_source_file oa1015.cif
_[local]_cod_data_source_block global
_[local]_cod_cif_authors_sg_H-M 'P 21/a '
_[local]_cod_chemical_formula_sum_orig 'C10 H21 N2 Na O10 V '
_cod_original_cell_volume 1607.6(6)
_cod_database_code 2006242
loop_
_symmetry_equiv_pos_as_xyz
' +x, +y, +z'
'1/2-x,1/2+y, -z'
' -x, -y, -z'
'1/2+x,1/2-y, +z'
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
V 0.0246(2) 0.01860(10) 0.01670(10) 0.00217(9) 0.00527(10) 0.00085(9)
Na 0.0359(4) 0.0319(4) 0.0333(4) -0.0037(3) 0.0072(3) 0.0004(3)
O1 0.0329(6) 0.0249(6) 0.0248(6) 0.0055(5) 0.0012(5) -0.0007(5)
O1w 0.0570(10) 0.0377(8) 0.0422(9) -0.0022(7) 0.0021(7) -0.0029(7)
O2 0.0353(7) 0.0319(7) 0.0356(7) 0.0140(5) 0.0031(6) 0.0005(6)
O2w 0.0339(7) 0.0466(8) 0.0382(8) -0.0027(6) 0.0053(6) -0.0003(7)
O3 0.0338(7) 0.0300(6) 0.0253(6) -0.0022(5) 0.0110(5) 0.0028(5)
O3w 0.0478(9) 0.0421(8) 0.0630(10) -0.0029(7) 0.0272(8) 0.0056(8)
O4 0.0490(10) 0.0540(10) 0.0700(10) -0.0182(8) 0.0320(10) -0.0087(9)
O5 0.0272(6) 0.0296(6) 0.0306(6) 0.0067(5) 0.0093(5) 0.0092(5)
O6 0.0383(7) 0.0343(7) 0.0405(8) 0.0134(6) 0.0105(6) 0.0116(6)
O7 0.0470(8) 0.0268(6) 0.0262(6) -0.0001(6) 0.0058(6) -0.0050(5)
N1 0.0291(7) 0.0259(7) 0.0208(6) 0.0001(5) 0.0029(5) -0.0014(5)
N2 0.0271(7) 0.0261(7) 0.0240(7) 0.0036(5) 0.0085(5) 0.0046(5)
C1 0.0290(8) 0.0230(7) 0.0237(8) 0.0041(6) 0.0064(6) 0.0036(6)
C2 0.0325(8) 0.0216(7) 0.0276(8) 0.0010(6) 0.0041(7) -0.0027(6)
C3 0.0309(9) 0.0275(8) 0.0420(10) 0.0006(7) 0.0126(8) 0.0014(7)
C4 0.0286(9) 0.0350(9) 0.0350(9) -0.0021(7) 0.0019(7) -0.0052(8)
C5 0.0283(8) 0.0274(8) 0.0242(8) 0.0042(6) 0.0055(6) 0.0022(6)
C6 0.0316(9) 0.0282(8) 0.0380(10) 0.0058(7) 0.0117(8) 0.0114(7)
C7 0.0470(10) 0.0347(9) 0.0177(7) 0.0028(8) 0.0027(7) -0.0023(7)
C8 0.0480(10) 0.0321(8) 0.0243(8) 0.0063(8) 0.0184(8) 0.0023(7)
C9 0.0263(8) 0.0396(10) 0.0367(10) 0.0009(7) 0.0095(7) 0.0069(8)
C10 0.0390(10) 0.0520(10) 0.0550(10) -0.0009(10) 0.0250(10) 0.0120(10)
loop_
_atom_site_label
_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_calc_flag
_atom_site_occupancy
V 0.23081(2) 0.15237(2) 0.53057(4) 0.01980(7) Uani d 1.00
Na 0.01899(5) 0.40162(6) 0.16270(10) 0.0336(2) Uani d 1.00
O1 0.14644(8) 0.25387(9) 0.4511(2) 0.0281(3) Uani d 1.00
O1w -0.00010(10) 0.22700(10) 0.1793(3) 0.0468(5) Uani d 1.00
O2 0.08643(8) 0.39140(10) 0.5120(2) 0.0348(4) Uani d 1.00
O2w -0.01601(9) 0.41580(10) -0.1940(2) 0.0398(4) Uani d 1.00
O3 0.31134(8) 0.22861(10) 0.4250(2) 0.0290(3) Uani d 1.00
O3w -0.10310(10) 0.42130(10) 0.2654(3) 0.0486(5) Uani d 1.00
O4 0.41310(10) 0.3311(2) 0.4742(3) 0.0551(6) Uani d 1.00
O5 0.31911(7) 0.07641(10) 0.6890(2) 0.0286(3) Uani d 1.00
O6 0.34528(9) -0.05740(10) 0.8730(2) 0.0373(4) Uani d 1.00
O7 0.19645(9) 0.07510(10) 0.3606(2) 0.0335(3) Uani d 1.00
N1 0.26688(9) 0.27610(10) 0.7558(2) 0.0255(3) Uani d 1.00
N2 0.17399(9) 0.10180(10) 0.7594(2) 0.0253(3) Uani d 1.00
C1 0.14270(10) 0.33420(10) 0.5444(3) 0.0251(4) Uani d 1.00
C2 0.21360(10) 0.36010(10) 0.7010(3) 0.0275(4) Uani d 1.00
C3 0.35940(10) 0.28830(10) 0.5324(3) 0.0328(5) Uani d 1.00
C4 0.34840(10) 0.3015(2) 0.7434(3) 0.0335(4) Uani d 1.00
C5 0.30090(10) 0.00790(10) 0.8021(3) 0.0266(4) Uani d 1.00
C6 0.21770(10) 0.01150(10) 0.8393(3) 0.0321(4) Uani d 1.00
C7 0.25710(10) 0.2335(2) 0.9450(3) 0.0335(5) Uani d 1.00
C8 0.17930(10) 0.17980(10) 0.9140(3) 0.0332(5) Uani d 1.00
C9 0.08970(10) 0.0767(2) 0.6787(3) 0.0337(5) Uani d 1.00
C10 0.04490(10) 0.0380(2) 0.8289(4) 0.0466(6) Uani d 1.00
H1 0.1959 0.3822 0.8146 0.0330 Uiso calc 1.00
H2 0.2419 0.4112 0.6529 0.0330 Uiso calc 1.00
H3 0.3587 0.3678 0.7823 0.0402 Uiso calc 1.00
H4 0.3839 0.2598 0.8278 0.0402 Uiso calc 1.00
H5 0.2201 0.0093 0.9771 0.0385 Uiso calc 1.00
H6 0.1898 -0.0441 0.7793 0.0385 Uiso calc 1.00
H7 0.2989 0.1890 0.9911 0.0402 Uiso calc 1.00
H8 0.2575 0.2843 1.0389 0.0402 Uiso calc 1.00
H9 0.1380 0.2257 0.8745 0.0399 Uiso calc 1.00
H10 0.1738 0.1500 1.0343 0.0399 Uiso calc 1.00
H11 0.0638 0.1342 0.6216 0.0405 Uiso calc 1.00
H12 0.0884 0.0280 0.5801 0.0405 Uiso calc 1.00
H13 0.0390 0.0903 0.9192 0.0587 Uiso calc 1.00
H14 -0.0053 0.0164 0.7665 0.0587 Uiso calc 1.00
H15 0.0738 -0.0138 0.9017 0.0587 Uiso calc 1.00
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Na 0.036 0.025
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
V 0.300 0.529
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
C 0.003 0.002
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
H 0.000 0.000
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.2)
;
O 0.011 0.006
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
N 0.006 0.003
;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_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 V O3 1_555 1_555 1_555 93.69(6) no
O1 V O5 1_555 1_555 1_555 161.54(6) yes
O1 V O7 1_555 1_555 1_555 96.09(7) yes
O1 V N1 1_555 1_555 1_555 76.52(5) yes
O1 V N2 1_555 1_555 1_555 90.51(6) no
O3 V O5 1_555 1_555 1_555 87.52(6) no
O3 V O7 1_555 1_555 1_555 104.88(7) yes
O3 V N1 1_555 1_555 1_555 75.61(6) yes
O3 V N2 1_555 1_555 1_555 154.00(6) yes
O5 V O7 1_555 1_555 1_555 101.40(7) yes
O5 V N1 1_555 1_555 1_555 85.98(6) no
O5 V N2 1_555 1_555 1_555 80.70(6) yes
O7 V N1 1_555 1_555 1_555 172.61(7) yes
O7 V N2 1_555 1_555 1_555 100.15(7) yes
N1 V N2 1_555 1_555 1_555 80.48(6) yes
V O1 C1 1_555 1_555 1_555 123.80(10) no
V O3 C3 1_555 1_555 1_555 122.40(10) no
V O5 C5 1_555 1_555 1_555 117.20(10) no
V N1 C2 1_555 1_555 1_555 108.80(10) no
V N1 C4 1_555 1_555 1_555 105.50(10) no
V N1 C7 1_555 1_555 1_555 104.70(10) no
C2 N1 C4 1_555 1_555 1_555 111.20(10) no
C2 N1 C7 1_555 1_555 1_555 111.10(10) no
C4 N1 C7 1_555 1_555 1_555 115.10(10) no
V N2 C6 1_555 1_555 1_555 105.50(10) no
V N2 C8 1_555 1_555 1_555 109.30(10) no
V N2 C9 1_555 1_555 1_555 110.70(10) no
C6 N2 C8 1_555 1_555 1_555 111.3(2) no
C6 N2 C9 1_555 1_555 1_555 109.60(10) no
C8 N2 C9 1_555 1_555 1_555 110.4(2) no
O1 C1 O2 1_555 1_555 1_555 124.4(2) no
O1 C1 C2 1_555 1_555 1_555 116.60(10) no
O2 C1 C2 1_555 1_555 1_555 118.9(2) no
N1 C2 C1 1_555 1_555 1_555 112.50(10) no
N1 C2 H1 1_555 1_555 1_555 108.7(2) no
N1 C2 H2 1_555 1_555 1_555 108.7(2) no
C1 C2 H1 1_555 1_555 1_555 108.7(2) no
C1 C2 H2 1_555 1_555 1_555 108.7(2) no
H1 C2 H2 1_555 1_555 1_555 109.5(2) no
O3 C3 O4 1_555 1_555 1_555 123.5(2) no
O3 C3 C4 1_555 1_555 1_555 116.2(2) no
O4 C3 C4 1_555 1_555 1_555 120.3(2) no
N1 C4 C3 1_555 1_555 1_555 109.3(2) no
N1 C4 H3 1_555 1_555 1_555 109.5(2) no
N1 C4 H4 1_555 1_555 1_555 109.5(2) no
C3 C4 H3 1_555 1_555 1_555 109.5(2) no
C3 C4 H4 1_555 1_555 1_555 109.5(2) no
H3 C4 H4 1_555 1_555 1_555 109.5(2) no
O5 C5 O6 1_555 1_555 1_555 124.2(2) no
O5 C5 C6 1_555 1_555 1_555 115.60(10) no
O6 C5 C6 1_555 1_555 1_555 120.1(2) no
N2 C6 C5 1_555 1_555 1_555 113.20(10) no
N2 C6 H5 1_555 1_555 1_555 108.5(2) no
N2 C6 H6 1_555 1_555 1_555 108.5(2) no
C5 C6 H5 1_555 1_555 1_555 108.5(2) no
C5 C6 H6 1_555 1_555 1_555 108.5(2) no
H5 C6 H6 1_555 1_555 1_555 109.5(2) no
N1 C7 C8 1_555 1_555 1_555 108.60(10) no
N1 C7 H7 1_555 1_555 1_555 109.7(2) no
N1 C7 H8 1_555 1_555 1_555 109.7(2) no
C8 C7 H7 1_555 1_555 1_555 109.7(2) no
C8 C7 H8 1_555 1_555 1_555 109.7(2) no
H7 C7 H8 1_555 1_555 1_555 109.5(2) no
N2 C8 C7 1_555 1_555 1_555 111.9(2) no
N2 C8 H9 1_555 1_555 1_555 108.9(2) no
N2 C8 H10 1_555 1_555 1_555 108.9(2) no
C7 C8 H9 1_555 1_555 1_555 108.9(2) no
C7 C8 H10 1_555 1_555 1_555 108.9(2) no
H9 C8 H10 1_555 1_555 1_555 109.5(2) no
N2 C9 C10 1_555 1_555 1_555 114.6(2) no
N2 C9 H11 1_555 1_555 1_555 108.2(2) no
N2 C9 H12 1_555 1_555 1_555 108.2(2) no
C10 C9 H11 1_555 1_555 1_555 108.2(2) no
C10 C9 H12 1_555 1_555 1_555 108.2(2) no
H11 C9 H12 1_555 1_555 1_555 109.5(2) no
C9 C10 H13 1_555 1_555 1_555 108.9(2) no
C9 C10 H14 1_555 1_555 1_555 110.2(2) no
C9 C10 H15 1_555 1_555 1_555 109.8(2) no
H13 C10 H14 1_555 1_555 1_555 108.8(2) no
H13 C10 H15 1_555 1_555 1_555 108.4(3) no
H14 C10 H15 1_555 1_555 1_555 110.7(3) no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
V O1 1_555 1_555 2.0090(10) yes
V O3 1_555 1_555 1.9920(10) yes
V O5 1_555 1_555 1.9890(10) yes
V O7 1_555 1_555 1.6060(10) yes
V N1 1_555 1_555 2.301(2) yes
V N2 1_555 1_555 2.142(2) yes
O1 C1 1_555 1_555 1.280(2) no
O2 C1 1_555 1_555 1.234(2) no
O3 C3 1_555 1_555 1.290(3) no
O4 C3 1_555 1_555 1.233(3) no
O5 C5 1_555 1_555 1.298(2) no
O6 C5 1_555 1_555 1.215(2) no
N1 C2 1_555 1_555 1.472(2) no
N1 C4 1_555 1_555 1.474(3) no
N1 C7 1_555 1_555 1.477(2) no
N2 C6 1_555 1_555 1.493(2) no
N2 C8 1_555 1_555 1.500(3) no
N2 C9 1_555 1_555 1.498(2) no
C1 C2 1_555 1_555 1.513(3) no
C2 H1 1_555 1_555 0.950 no
C2 H2 1_555 1_555 0.950 no
C3 C4 1_555 1_555 1.525(3) no
C4 H3 1_555 1_555 0.950 no
C4 H4 1_555 1_555 0.950 no
C5 C6 1_555 1_555 1.515(3) no
C6 H5 1_555 1_555 0.950 no
C6 H6 1_555 1_555 0.950 no
C7 C8 1_555 1_555 1.511(3) no
C7 H7 1_555 1_555 0.950 no
C7 H8 1_555 1_555 0.950 no
C8 H9 1_555 1_555 0.950 no
C8 H10 1_555 1_555 0.950 no
C9 C10 1_555 1_555 1.512(3) no
C9 H11 1_555 1_555 0.950 no
C9 H12 1_555 1_555 0.950 no
C10 H13 1_555 1_555 0.968 no
C10 H14 1_555 1_555 0.940 no
C10 H15 1_555 1_555 0.950 no