#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/87/2238743.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_2238743
loop_
_publ_author_name
'Chang, Kelvin B.'
'Smith, Matthew D.'
'Zeller, Matthias'
'Norquist, Alexander J.'
_publ_section_title
;
 catena-Poly[2,2',2''-nitrilotris(ethanaminium)
 [tri-μ-oxido-tris[dioxidovanadate(V)]] monohydrate]
;
_journal_coeditor_code           HP2060
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m570
_journal_page_last               m571
_journal_paper_doi               10.1107/S1600536813026056
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          '(C6 H21 N4) [V3 O9], H2 O'
_chemical_formula_moiety         'C6 H21 N4 3+, O9 V3 3-, H2 O'
_chemical_formula_sum            'C6 H23 N4 O10 V3'
_chemical_formula_weight         464.09
_chemical_name_systematic
;
catena-Poly[2,2',2''-nitrilotris(ethanaminium)
[tri-μ-oxido-tris[dioxidovanadate(V)]] monohydrate]
;
_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
_cell_angle_alpha                90
_cell_angle_beta                 100.565(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.6624(14)
_cell_length_b                   10.9179(15)
_cell_length_c                   15.768(2)
_cell_measurement_reflns_used    2067
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.5116
_cell_measurement_theta_min      2.6280
_cell_volume                     1635.2(4)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2009)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device       'Bruker SMART APEX CCD area-detector'
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area-detector'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.061
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            14279
_diffrn_reflns_theta_full        25.886
_diffrn_reflns_theta_max         30.100
_diffrn_reflns_theta_min         2.144
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.734
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6226
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2008)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.885
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.160
_refine_diff_density_max         1.44
_refine_diff_density_min         -0.68
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0022
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         2860
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0877
_refine_ls_R_factor_gt           0.0523
_refine_ls_shift/su_max          0.0003744
_refine_ls_shift/su_mean         0.0000250
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick
 w=1/[σ²(F²) + (0.03P)² + 7.47P]
 ,where P=(max(Fo²,0) + 2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1100
_refine_ls_wR_factor_gt          0.0997
_refine_ls_wR_factor_ref         0.0938
_reflns_number_gt                3195
_reflns_number_total             4719
_reflns_threshold_expression     I>2.0σ(I)
_cod_data_source_file            hp2060.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2238743
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x,y+1/2,-z+1/2
x,-y+1/2,z+1/2
loop_
_atom_site_type_symbol
_atom_site_label
_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
V V1 0.92597(7) 0.75226(7) 0.71937(5) 0.0135 Uani 1.0000
V V2 0.87185(7) 0.80317(7) 0.49412(4) 0.0120 Uani 1.0000
V V3 0.75379(8) 0.58481(7) 0.35925(5) 0.0152 Uani 1.0000
O O1 0.8914(4) 0.6089(3) 0.7288(2) 0.0320 Uani 1.0000
O O2 1.0944(3) 0.7734(3) 0.7595(2) 0.0217 Uani 1.0000
O O3 0.8219(5) 0.8480(4) 0.7734(2) 0.0498 Uani 1.0000
O O4 0.8935(3) 0.8036(3) 0.6095(2) 0.0244 Uani 1.0000
O O5 1.0270(3) 0.7839(3) 0.4659(2) 0.0220 Uani 1.0000
O O6 0.8112(4) 0.9374(3) 0.4625(2) 0.0379 Uani 1.0000
O O7 0.7512(4) 0.6883(4) 0.4472(2) 0.0354 Uani 1.0000
O O8 0.8542(4) 0.4695(4) 0.4011(3) 0.0429 Uani 1.0000
O O9 0.5943(3) 0.5335(3) 0.3264(2) 0.0233 Uani 1.0000
O O10 0.6272(4) 0.9517(3) 0.2942(2) 0.0326 Uani 1.0000
N N1 0.3633(3) 0.7571(3) 0.4750(2) 0.0124 Uani 1.0000
N N2 0.1483(4) 0.5617(3) 0.4189(2) 0.0186 Uani 1.0000
N N3 0.2327(4) 0.8310(4) 0.6220(2) 0.0199 Uani 1.0000
N N4 0.1714(4) 0.9305(3) 0.3650(2) 0.0173 Uani 1.0000
C C1 0.3965(4) 0.6257(4) 0.4704(3) 0.0144 Uani 1.0000
C C2 0.2953(4) 0.5559(4) 0.4031(3) 0.0161 Uani 1.0000
C C3 0.4414(4) 0.8077(4) 0.5560(3) 0.0180 Uani 1.0000
C C4 0.3751(4) 0.7766(4) 0.6334(3) 0.0178 Uani 1.0000
C C5 0.4008(5) 0.8229(4) 0.4007(3) 0.0195 Uani 1.0000
C C6 0.3272(4) 0.9449(4) 0.3853(3) 0.0186 Uani 1.0000
H H1 0.7169 0.9334 0.2807 0.0389 Uiso 1.0000
H H2 0.5660 0.9794 0.2437 0.0389 Uiso 1.0000
H H3 0.4912 0.6178 0.4588 0.0191 Uiso 1.0000
H H4 0.3936 0.5894 0.5259 0.0187 Uiso 1.0000
H H5 0.2977 0.5904 0.3470 0.0191 Uiso 1.0000
H H6 0.3247 0.4713 0.4050 0.0189 Uiso 1.0000
H H7 0.1445 0.5268 0.4736 0.0240 Uiso 1.0000
H H8 0.0880 0.5172 0.3752 0.0240 Uiso 1.0000
H H9 0.1185 0.6447 0.4180 0.0240 Uiso 1.0000
H H10 0.5379 0.7765 0.5656 0.0209 Uiso 1.0000
H H11 0.4435 0.8963 0.5511 0.0211 Uiso 1.0000
H H12 0.4324 0.8092 0.6858 0.0219 Uiso 1.0000
H H13 0.3682 0.6886 0.6390 0.0222 Uiso 1.0000
H H14 0.1764 0.7994 0.5709 0.0245 Uiso 1.0000
H H15 0.1904 0.8116 0.6701 0.0245 Uiso 1.0000
H H16 0.2399 0.9174 0.6173 0.0245 Uiso 1.0000
H H17 0.3702 0.7723 0.3497 0.0240 Uiso 1.0000
H H18 0.5027 0.8342 0.4091 0.0241 Uiso 1.0000
H H19 0.3508 0.9958 0.4366 0.0226 Uiso 1.0000
H H20 0.3573 0.9845 0.3373 0.0229 Uiso 1.0000
H H21 0.1284 1.0088 0.3561 0.0223 Uiso 1.0000
H H22 0.1465 0.8828 0.3140 0.0223 Uiso 1.0000
H H23 0.1400 0.8905 0.4115 0.0223 Uiso 1.0000
loop_
_atom_type_symbol
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C 2.3100 1.0200 1.5886 0.8650 20.8439 10.2075 0.5687 51.6512 0.2156 0.0033
0.0016 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.4930 0.3229 0.1402 0.0408 10.5109 26.1257 3.1424 57.7998 0.0030 0.0000
0.0000 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 12.2126 3.1322 2.0125 1.1663 0.0057 9.8933 28.9975 0.5826 -11.5290 0.0061
0.0033 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 3.0485 2.2868 1.5463 0.8670 13.2771 5.7011 0.3239 32.9089 0.2508 0.0106
0.0060 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
V 10.2971 7.3511 2.0703 2.0571 6.8657 0.4385 26.8938 102.4780 1.2199 0.3005
0.5294 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Te 19.9644 19.0138 6.1449 2.5239 4.8174 0.4209 28.5284 70.8403 4.3520 -0.5308
1.6751 'International Tables Vol C 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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 V1 O2 . . 107.86(17) no
O1 V1 O3 . . 112.5(2) no
O2 V1 O3 . . 109.83(19) no
O1 V1 O4 . . 112.94(18) no
O2 V1 O4 . . 108.21(15) no
O3 V1 O4 . . 105.41(17) no
V3 V2 O4 . . 128.76(12) no
V3 V2 O5 . . 87.55(11) no
O4 V2 O5 . . 109.31(15) no
V3 V2 O6 . . 113.39(14) no
O4 V2 O6 . . 106.12(17) no
O5 V2 O6 . . 109.05(19) no
V3 V2 O7 . . 24.27(11) no
O4 V2 O7 . . 111.67(17) no
O5 V2 O7 . . 110.85(16) no
O6 V2 O7 . . 109.7(2) no
V2 V3 O3 . 4_564 93.50(13) no
V2 V3 O7 . . 24.06(10) no
O3 V3 O7 4_564 . 112.99(19) no
V2 V3 O8 . . 100.80(15) no
O3 V3 O8 4_564 . 110.4(2) no
O7 V3 O8 . . 105.2(2) no
V2 V3 O9 . . 130.93(12) no
O3 V3 O9 4_564 . 111.19(18) no
O7 V3 O9 . . 108.37(16) no
O8 V3 O9 . . 108.46(19) no
V1 O3 V3 . 4_565 159.3(2) no
V2 O4 V1 . . 161.2(2) no
V3 O7 V2 . . 131.66(19) no
H1 O10 H2 . . 109.5 no
C1 N1 C3 . . 109.1(3) no
C1 N1 C5 . . 110.3(3) no
C3 N1 C5 . . 110.2(3) no
C2 N2 H7 . . 109.4 no
C2 N2 H8 . . 109.6 no
H7 N2 H8 . . 109.5 no
C2 N2 H9 . . 109.5 no
H7 N2 H9 . . 109.5 no
H8 N2 H9 . . 109.5 no
C4 N3 H14 . . 109.4 no
C4 N3 H15 . . 109.9 no
H14 N3 H15 . . 109.5 no
C4 N3 H16 . . 109.1 no
H14 N3 H16 . . 109.5 no
H15 N3 H16 . . 109.5 no
C6 N4 H21 . . 109.5 no
C6 N4 H22 . . 109.2 no
H21 N4 H22 . . 109.5 no
C6 N4 H23 . . 109.6 no
H21 N4 H23 . . 109.5 no
H22 N4 H23 . . 109.5 no
N1 C1 C2 . . 114.0(3) no
N1 C1 H3 . . 108.5 no
C2 C1 H3 . . 109.6 no
N1 C1 H4 . . 108.2 no
C2 C1 H4 . . 107.9 no
H3 C1 H4 . . 108.6 no
C1 C2 N2 . . 112.1(3) no
C1 C2 H5 . . 109.0 no
N2 C2 H5 . . 108.7 no
C1 C2 H6 . . 108.2 no
N2 C2 H6 . . 108.7 no
H5 C2 H6 . . 110.2 no
N1 C3 C4 . . 112.9(3) no
N1 C3 H10 . . 109.0 no
C4 C3 H10 . . 109.2 no
N1 C3 H11 . . 108.7 no
C4 C3 H11 . . 107.8 no
H10 C3 H11 . . 109.1 no
C3 C4 N3 . . 109.4(4) no
C3 C4 H12 . . 110.0 no
N3 C4 H12 . . 109.1 no
C3 C4 H13 . . 110.0 no
N3 C4 H13 . . 109.4 no
H12 C4 H13 . . 108.8 no
N1 C5 C6 . . 112.4(3) no
N1 C5 H17 . . 107.3 no
C6 C5 H17 . . 107.7 no
N1 C5 H18 . . 110.0 no
C6 C5 H18 . . 110.1 no
H17 C5 H18 . . 109.2 no
C5 C6 N4 . . 111.7(3) no
C5 C6 H19 . . 109.8 no
N4 C6 H19 . . 108.2 no
C5 C6 H20 . . 108.8 no
N4 C6 H20 . . 108.5 no
H19 C6 H20 . . 109.8 no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
V1 O1 . 1.613(3) yes
V1 O2 . 1.651(3) yes
V1 O3 . 1.773(4) yes
V1 O4 . 1.793(3) yes
V2 V3 . 3.2585(11) yes
V2 O4 . 1.793(3) yes
V2 O5 . 1.654(3) yes
V2 O6 . 1.623(4) yes
V2 O7 . 1.778(3) yes
V3 O3 4_564 1.769(4) yes
V3 O7 . 1.793(3) yes
V3 O8 . 1.651(4) yes
V3 O9 . 1.632(3) yes
O10 H1 . 0.950 no
O10 H2 . 0.950 no
N1 C1 . 1.475(5) no
N1 C3 . 1.468(5) no
N1 C5 . 1.475(5) no
N2 C2 . 1.488(5) no
N2 H7 . 0.950 no
N2 H8 . 0.950 no
N2 H9 . 0.950 no
N3 C4 . 1.479(6) no
N3 H14 . 0.950 no
N3 H15 . 0.950 no
N3 H16 . 0.950 no
N4 C6 . 1.489(5) no
N4 H21 . 0.950 no
N4 H22 . 0.950 no
N4 H23 . 0.950 no
C1 C2 . 1.510(6) no
C1 H3 . 0.969 no
C1 H4 . 0.966 no
C2 H5 . 0.967 no
C2 H6 . 0.966 no
C3 C4 . 1.517(6) no
C3 H10 . 0.978 no
C3 H11 . 0.970 no
C4 H12 . 0.975 no
C4 H13 . 0.968 no
C5 C6 . 1.508(6) no
C5 H17 . 0.976 no
C5 H18 . 0.977 no
C6 H19 . 0.974 no
C6 H20 . 0.962 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O10 H1 O1 4_564 0.950 2.058 2.997(6) 169.49(14) yes
O10 H2 O9 3_655 0.950 1.828 2.739(6) 159.72(15) yes
N2 H7 O8 2_666 0.950 1.974 2.864(6) 155.08(16) yes
N2 H8 O1 2_666 0.950 2.177 2.951(6) 137.77(13) yes
N2 H9 O5 1_455 0.950 1.976 2.850(6) 152.05(14) yes
C4 H13 O9 2_666 0.968 2.497 3.447(6) 166.90(12) yes
N3 H14 O5 1_455 0.950 1.995 2.912(6) 161.64(15) yes
N3 H15 O2 1_455 0.950 1.871 2.819(6) 175.82(15) yes
N3 H16 O6 2_676 0.950 2.027 2.853(6) 144.28(15) yes
N3 H16 O10 2_676 0.950 2.233 2.925(6) 128.97(13) yes
C6 H19 O6 2_676 0.974 2.535 3.222(6) 127.44(14) yes
N4 H21 O4 2_676 0.950 2.138 3.013(6) 152.40(13) yes
N4 H22 O2 4_464 0.950 1.935 2.796(6) 149.71(14) yes
N4 H23 O5 1_455 0.950 1.904 2.803(6) 156.83(14) yes
