#------------------------------------------------------------------------------
#$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $
#$Revision: 25271 $
#$URL: svn://www.crystallography.net/cod/cif/2/2003481.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_2003481
loop_
_publ_author_name
'Neves, A.'
'Vencato, I.'
'H\"orner, M.'
'Fenner, H.'
_publ_contact_author
;
    Dr Ivo Vencato
    Depto. F\'isica - UFSC
    88040 - 900 Florian\'opolis, SC
    Brazil
;
_publ_section_title
;
 \m-[<i>N</i>,<i>N</i>-Bis(2-pyridylmethyl-1\k<i>N</i>)-<i>N</i>',<i>N</i>'-bis(2-pyridylmethyl-2\k<i>N</i>)-1,3-diaminopropan-2-olato]-1\k<i>N</i>,2\k<i>N</i>',1:2\k^2^<i>O</i>-bis(dioxovanadium)(1+)
 Iodide Dihydrate, [(VO~2~)~2~(TPHPN)]I.2H~2~O
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              809
_journal_page_last               811
_journal_volume                  51
_journal_year                    1995
_chemical_formula_analytical     '(C~27~ H~29~ N~6~ O (VO~2~)~2~)I.2(H~2~O)'
_chemical_formula_sum            'C27 H33 I N6 O7 V2'
_chemical_formula_weight         782.38
_chemical_name_systematic
;
Bis-dioxo ((N,N,N',N'-tetrakis (2-pyridylmethyl-2-ol-1,3-propanediamine)
-divanadium (V) Iodide dihydrate ((VO~2~)~2~ (TPHPN))I.2H~2~O
;
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_type_scat_source
;
 International Tables for X-ray Crystallography (1974, Vol.IV,
 Table 2.2A)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.88(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.369(4)
_cell_length_b                   14.399(7)
_cell_length_c                   13.772(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293
_cell_measurement_theta_max      18.0
_cell_measurement_theta_min      12.0
_cell_volume                     3047.4(18)
_computing_cell_refinement       'SDP (Frenz, 1978)'
_computing_data_collection       'SDP (Frenz, 1978)'
_computing_data_reduction        'SDP (Frenz, 1978)'
_computing_molecular_graphics    'ORTEP (Johnson, 1965)'
_computing_publication_material  'SDP (Frenz, 1978)'
_computing_structure_refinement  'SDP(Frenz, 1978)'
_computing_structure_solution    'SHELX86(VMS version; Sheldrick, 1985)'
_diffrn_measurement_device       'Enraf-Nonius CAD-4'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.028
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            5222
_diffrn_reflns_theta_max         24.0
_diffrn_standards_decay_%        0.6
_diffrn_standards_interval_time  40
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.65
_exptl_absorpt_correction_T_max  1.11
_exptl_absorpt_correction_T_min  0.88
_exptl_absorpt_correction_type   ' empirical (DIFABS;  Walker & Stuart,1983)'
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_density_diffrn    1.705
_exptl_crystal_description       'trapezoidal plate'
_exptl_crystal_F_000             1472
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.74
_refine_diff_density_min         -0.72
_refine_ls_extinction_coef       4.657E-8(3)
_refine_ls_extinction_method     ' Zachariasen (1963)'
_refine_ls_goodness_of_fit_obs   2.70
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         4177
_refine_ls_R_factor_obs          0.0424
_refine_ls_shift/esd_max         0.01
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      1/[\s^2^(F)]
_refine_ls_wR_factor_obs         0.0516
_reflns_number_observed          4177
_reflns_number_total             4380
_reflns_observed_criterion       'I > 3.0\s(I)'
_[local]_cod_data_source_file    mu1137.cif
_[local]_cod_data_source_block   mu1137
_[local]_cod_cif_authors_sg_H-M  'P 21/c'
_[local]_cod_chemical_formula_sum_orig 'C27 H33 I1 N6 O7 V2'
_cod_original_cell_volume        3047(3)
_cod_database_code               2003481
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
I 0.0530(2) 0.0554(3) 0.0533(2) -0.0045(2) -0.0005(2) -0.0001(2)
V1 0.0426(5) 0.0389(6) 0.0360(5) 0.0002(5) 0.0059(5) -0.0016(5)
V2 0.0402(5) 0.0357(5) 0.0398(5) 0.0014(5) -0.0002(5) -0.0004(5)
O1 0.044(2) 0.054(3) 0.061(3) 0.004(2) 0.010(2) -0.002(2)
O2 0.058(3) 0.060(3) 0.041(2) -0.006(2) 0.011(2) -0.008(2)
O3 0.060(3) 0.049(3) 0.050(3) 0.002(2) 0.001(2) 0.010(2)
O4 0.054(3) 0.044(2) 0.046(2) 0.002(2) 0.000(2) -0.007(2)
O5 0.037(2) 0.046(2) 0.032(2) 0.002(2) 0.000(2) -0.006(2)
OW1 0.078(4) 0.053(4) 0.400(10) 0.018(3) 0.064(6) 0.042(6)
OW2 0.310(10) 0.144(8) 0.180(10) -0.046(9) 0.040(10) 0.005(8)
N1 0.034(2) 0.035(3) 0.039(3) -0.002(2) 0.000(2) -0.004(2)
N2 0.042(3) 0.041(3) 0.039(3) 0.002(2) 0.002(2) 0.000(2)
N11 0.040(3) 0.040(3) 0.041(3) 0.004(2) 0.005(2) -0.003(2)
N21 0.042(3) 0.041(3) 0.041(3) -0.002(2) 0.005(2) 0.001(2)
N31 0.046(3) 0.044(3) 0.040(3) -0.003(3) -0.001(2) 0.004(3)
N41 0.048(3) 0.044(3) 0.038(3) 0.002(3) -0.001(2) 0.002(3)
C1 0.041(3) 0.043(3) 0.044(3) 0.002(3) -0.005(3) 0.001(3)
C2 0.043(3) 0.045(4) 0.050(4) -0.006(3) -0.002(3) -0.007(3)
C3 0.042(3) 0.044(3) 0.035(3) -0.001(3) 0.002(3) -0.004(3)
C4 0.042(3) 0.043(3) 0.040(3) 0.002(3) 0.006(3) -0.005(3)
C5 0.040(3) 0.053(4) 0.038(3) 0.000(3) 0.002(3) -0.004(3)
C6 0.061(4) 0.041(4) 0.055(4) 0.010(3) 0.003(3) -0.001(3)
C7 0.038(3) 0.060(4) 0.050(4) -0.001(3) 0.009(3) -0.002(3)
C11 0.034(3) 0.043(3) 0.042(3) 0.005(3) 0.007(3) 0.000(3)
C12 0.049(4) 0.049(4) 0.054(4) 0.006(3) 0.003(3) 0.004(3)
C13 0.069(4) 0.042(4) 0.062(4) 0.007(4) 0.010(4) 0.005(4)
C14 0.061(4) 0.046(4) 0.063(4) 0.001(4) 0.010(4) -0.006(4)
C15 0.046(3) 0.040(3) 0.051(4) 0.002(3) 0.006(3) -0.005(3)
C21 0.038(3) 0.041(3) 0.051(4) -0.005(3) 0.010(3) 0.002(3)
C22 0.048(3) 0.044(4) 0.055(4) -0.010(3) 0.012(3) -0.003(3)
C23 0.057(4) 0.042(4) 0.070(4) -0.002(3) 0.018(4) 0.005(4)
C24 0.058(4) 0.055(4) 0.061(4) 0.000(4) 0.008(4) 0.016(4)
C25 0.052(4) 0.048(4) 0.048(4) -0.002(3) 0.006(3) 0.006(3)
C31 0.044(3) 0.044(4) 0.049(4) -0.002(3) 0.003(3) 0.008(3)
C32 0.044(4) 0.065(5) 0.069(5) -0.001(4) 0.007(4) 0.000(4)
C33 0.048(4) 0.091(6) 0.075(5) -0.016(4) -0.005(4) 0.007(5)
C34 0.058(4) 0.068(5) 0.062(4) -0.012(4) -0.008(4) -0.002(4)
C35 0.050(4) 0.050(4) 0.048(4) -0.004(3) -0.006(3) -0.002(3)
C41 0.050(4) 0.042(4) 0.049(4) 0.005(3) -0.005(3) -0.001(3)
C42 0.123(7) 0.042(4) 0.068(5) 0.015(5) 0.007(5) 0.005(4)
C43 0.160(9) 0.058(5) 0.067(5) 0.007(6) -0.002(6) 0.025(4)
C44 0.118(7) 0.066(5) 0.047(4) 0.002(5) -0.005(5) 0.015(4)
C45 0.066(4) 0.055(4) 0.047(4) -0.003(4) 0.003(3) 0.003(4)
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
I 0.30242(3) 0.38482(4) 0.05607(4)
V(1) 0.38539(7) -0.17838(8) 0.20864(8)
V(2) 0.15124(7) -0.23569(7) 0.21657(8)
O(1) 0.4903(3) -0.1761(3) 0.1973(3)
O(2) 0.3462(3) -0.2041(3) 0.1027(3)
O(3) 0.1438(3) -0.3117(3) 0.3038(3)
O(4) 0.1787(3) -0.2936(3) 0.1216(3)
O(5) 0.2514(3) -0.1647(3) 0.2613(3)
O(W1) 0.1333(5) -1.0111(5) 0.6749(9)
O(W2) 0.3625(9) 0.3147(8) 0.4161(9)
N(1) 0.3992(3) -0.1398(3) 0.3684(4)
N(2) 0.0874(3) -0.1247(4) 0.3102(4)
N(11) 0.3864(3) -0.3063(4) 0.2822(4)
N(21) 0.3755(3) -0.0325(4) 0.2088(4)
N(31) 0.0147(3) -0.2484(4) 0.1885(4)
N(41) 0.1280(3) -0.1064(4) 0.1200(4)
C(1) 0.4534(4) -0.2149(5) 0.4098(5)
C(2) 0.4430(4) -0.0480(5) 0.3684(5)
C(3) 0.3131(4) -0.1366(4) 0.4181(4)
C(4) 0.2423(4) -0.1086(5) 0.3460(4)
C(5) 0.1536(4) -0.1203(5) 0.3899(4)
C(6) 0.0716(5) -0.0331(5) 0.2637(5)
C(7) 0.0046(4) -0.1683(5) 0.3408(5)
C(11) 0.4229(4) -0.3060(4) 0.3716(5)
C(12) 0.4344(4) -0.3881(5) 0.4246(5)
C(13) 0.4073(5) -0.4708(5) 0.3823(6)
C(14) 0.3681(5) -0.4692(5) 0.2915(5)
C(15) 0.3586(4) -0.3862(5) 0.2435(5)
C(21) 0.4071(4) 0.0120(5) 0.2883(5)
C(22) 0.4046(4) 0.1085(5) 0.2939(5)
C(23) 0.3689(5) 0.1585(5) 0.2193(6)
C(24) 0.3354(5) 0.1129(5) 0.1397(5)
C(25) 0.3401(4) 0.0173(5) 0.1366(5)
C(31) -0.0390(4) -0.2114(5) 0.2534(5)
C(32) -0.1283(5) -0.2168(6) 0.2416(6)
C(33) -0.1616(5) -0.2633(7) 0.1615(6)
C(34) -0.1058(5) -0.3033(6) 0.0953(6)
C(35) -0.0186(4) -0.2937(5) 0.1122(5)
C(41) 0.0975(4) -0.0288(5) 0.1598(5)
C(42) 0.0886(7) 0.0516(6) 0.1059(6)
C(43) 0.1083(8) 0.0524(6) 0.0119(7)
C(44) 0.1430(7) -0.0263(6) -0.0316(6)
C(45) 0.1511(5) -0.1043(5) 0.0252(5)
H12 0.4601 -0.3868 0.4893
H13 0.4161 -0.5290 0.4160
H14 0.3469 -0.5261 0.2618
H15 0.3308 -0.3852 0.1798
H22 0.4282 0.1399 0.3505
H23 0.3671 0.2255 0.2227
H24 0.3085 0.1475 0.0870
H25 0.3167 -0.0150 0.0802
H32 -0.1665 -0.1887 0.2884
H33 -0.2240 -0.2673 0.1515
H34 -0.1285 -0.3368 0.0390
H35 0.0214 -0.3211 0.0667
H42 0.0658 0.1072 0.1368
H43 0.1001 0.1081 -0.0271
H44 0.1611 -0.0264 -0.0995
H45 0.1744 -0.1607 -0.0037
H111 0.4495 -0.2142 0.4793
H112 0.5129 -0.2053 0.3932
H211 0.5044 -0.0560 0.3599
H212 0.4347 -0.0177 0.4297
H311 0.3154 -0.0933 0.4709
H312 0.2995 -0.1966 0.4442
H411 0.2481 -0.0442 0.3277
H511 0.1524 -0.1769 0.4275
H512 0.1411 -0.0700 0.4331
H611 0.1030 0.0135 0.2994
H612 0.0105 -0.0185 0.2678
H711 -0.0327 -0.1227 0.3691
H712 0.0162 -0.2151 0.3894
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
O(1) V(1) O(2) 106.00(10) yes
O(1) V(1) O(5) 164.90(10) yes
O(1) V(1) N(1) 90.60(10) yes
O(1) V(1) N(11) 93.70(10) yes
O(1) V(1) N(21) 93.10(10) yes
O(2) V(1) O(5) 88.90(10) yes
O(2) V(1) N(1) 163.40(10) yes
O(2) V(1) N(11) 103.60(10) yes
O(2) V(1) N(21) 101.70(10) yes
O(5) V(1) N(1) 74.60(10) yes
O(5) V(1) N(11) 85.4(2) yes
O(5) V(1) N(21) 80.90(10) yes
N(1) V(1) N(11) 75.40(10) yes
N(1) V(1) N(21) 76.20(10) yes
N(11) V(1) N(21) 150.90(10) yes
O(3) V(2) O(4) 105.80(10) yes
O(3) V(2) O(5) 100.70(10) yes
O(3) V(2) N(2) 91.10(10) yes
O(3) V(2) N(31) 89.80(10) yes
O(3) V(2) N(41) 162.20(10) yes
O(4) V(2) O(5) 108.30(10) yes
O(4) V(2) N(2) 160.10(10) yes
O(4) V(2) N(31) 94.50(10) yes
O(4) V(2) N(41) 89.40(10) yes
O(5) V(2) N(2) 78.3(2) yes
O(5) V(2) N(31) 151.10(10) yes
O(5) V(2) N(41) 82.70(10) yes
N(2) V(2) N(31) 74.50(10) yes
N(2) V(2) N(41) 72.40(10) yes
V(1) O(5) V(2) 126.20(10) yes
N(1) C(1) C(11) 109.7(4) no
N(1) C(2) C(21) 110.6(3) no
N(1) C(3) C(4) 109.7(3) no
N(2) C(5) C(4) 108.7(4) no
N(2) C(6) C(41) 113.9(3) no
N(2) C(7) C(31) 108.8(3) no
N(11) C(11) C(1) 117.0(3) no
N(11) C(11) C(12) 121.5(4) no
N(11) C(15) C(14) 121.8(4) no
N(21) C(21) C(2) 116.4(3) no
N(21) C(21) C(22) 120.5(4) no
N(21) C(25) C(24) 122.3(4) no
N(31) C(31) C(7) 115.3(3) no
N(31) C(31) C(32) 121.4(5) no
N(31) C(35) C(34) 123.3(4) no
N(41) C(41) C(6) 117.4(4) no
N(41) C(41) C(42) 121.0(4) no
N(41) C(45) C(44) 122.9(4) no
C(1) C(11) C(12) 121.6(4) no
C(1) N(1) C(2) 113.6(3) no
C(1) N(1) C(3) 110.0(3) no
C(2) N(1) C(3) 112.1(3) no
C(2) C(21) C(22) 123.0(4) no
C(3) C(4) C(5) 110.6(3) no
C(5) N(2) C(6) 112.7(3) no
C(5) N(2) C(7) 112.8(3) no
C(6) N(2) C(7) 111.2(3) no
C(6) C(41) C(42) 121.6(5) no
C(7) C(31) C(32) 123.2(4) no
C(11) N(11) C(15) 119.7(3) no
C(11) C(12) C(13) 118.1(4) no
C(12) C(13) C(14) 119.4(4) no
C(13) C(14) C(15) 119.5(4) no
C(21) N(21) C(25) 119.0(3) no
C(21) C(22) C(23) 119.8(4) no
C(22) C(23) C(24) 119.4(4) no
C(23) C(24) C(25) 118.9(4) no
C(31) N(31) C(35) 119.3(4) no
C(31) C(32) C(33) 118.5(4) no
C(32) C(33) C(34) 120.1(4) no
C(33) C(34) C(35) 117.5(4) no
C(41) N(41) C(45) 118.3(4) no
C(41) C(42) C(43) 120.5(5) no
C(42) C(43) C(44) 120.3(5) no
C(43) C(44) C(45) 116.9(5) no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
V(1) O(1) 1.624(3) yes
V(1) O(2) 1.614(3) yes
V(1) O(5) 2.204(2) yes
V(1) N(1) 2.275(4) yes
V(1) N(11) 2.103(3) yes
V(1) N(21) 2.106(3) yes
V(2) O(3) 1.631(3) yes
V(2) O(4) 1.612(3) yes
V(2) O(5) 1.940(2) yes
V(2) N(2) 2.284(3) yes
V(2) N(31) 2.136(3) yes
V(2) N(41) 2.313(3) yes
V(1) V(2) 3.690(3) yes
O(5) C(4) 1.428(4) no
N(1) C(1) 1.475(5) no
N(1) C(2) 1.483(5) no
N(1) C(3) 1.501(5) no
N(2) C(5) 1.486(5) no
N(2) C(6) 1.485(5) no
N(2) C(7) 1.485(5) no
N(11) C(11) 1.345(5) no
N(11) C(15) 1.335(5) no
N(21) C(21) 1.353(5) no
N(21) C(25) 1.335(6) no
N(31) C(31) 1.337(6) no
N(31) C(35) 1.332(5) no
N(41) C(41) 1.333(6) no
N(41) C(45) 1.358(5) no
C(1) C(11) 1.486(5) no
C(2) C(21) 1.500(6) no
C(3) C(4) 1.516(5) no
C(4) C(5) 1.510(5) no
C(6) C(41) 1.493(6) no
C(7) C(31) 1.503(6) no
C(11) C(12) 1.400(6) no
C(12) C(13) 1.387(6) no
C(13) C(14) 1.379(6) no
C(14) C(15) 1.373(6) no
C(21) C(22) 1.392(6) no
C(22) C(23) 1.363(6) no
C(23) C(24) 1.371(7) no
C(24) C(25) 1.379(6) no
C(31) C(32) 1.381(6) no
C(32) C(33) 1.381(7) no
C(33) C(34) 1.386(7) no
C(34) C(35) 1.365(6) no
C(41) C(42) 1.381(6) no
C(42) C(43) 1.335(7) no
C(43) C(44) 1.392(8) no
C(44) C(45) 1.374(6) no