#------------------------------------------------------------------------------
#$Date: 2013-12-28 13:58:47 +0000 (Sat, 28 Dec 2013) $
#$Revision: 91933 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/34/2003481.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-[N,N-Bis(2-pyridylmethyl-1\kN)-N',N'-bis(2-pyridylmethyl-2\kN)-1,3-diaminopropan-2-olato]-1\kN,2\kN',1:2\k^2^O-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_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_B_iso_or_equiv
I 0.30242(3) 0.38482(4) 0.05607(4) 4.26(1)
V(1) 0.38539(7) -0.17838(8) 0.20864(8) 3.09(2)
V(2) 0.15124(7) -0.23569(7) 0.21657(8) 3.04(2)
O(1) 0.4903(3) -0.1761(3) 0.1973(3) 4.2(1)
O(2) 0.3462(3) -0.2041(3) 0.1027(3) 4.2(1)
O(3) 0.1438(3) -0.3117(3) 0.3038(3) 4.2(1)
O(4) 0.1787(3) -0.2936(3) 0.1216(3) 3.8(1)
O(5) 0.2514(3) -0.1647(3) 0.2613(3) 3.01(8)
O(W1) 0.1333(5) -1.0111(5) 0.6749(9) 13.9(3)
O(W2) 0.3625(9) 0.3147(8) 0.4161(9) 16.5(4)
N(1) 0.3992(3) -0.1398(3) 0.3684(4) 2.8(1)
N(2) 0.0874(3) -0.1247(4) 0.3102(4) 3.2(1)
N(11) 0.3864(3) -0.3063(4) 0.2822(4) 3.2(1)
N(21) 0.3755(3) -0.0325(4) 0.2088(4) 3.3(1)
N(31) 0.0147(3) -0.2484(4) 0.1885(4) 3.4(1)
N(41) 0.1280(3) -0.1064(4) 0.1200(4) 3.4(1)
C(1) 0.4534(4) -0.2149(5) 0.4098(5) 3.4(1)
C(2) 0.4430(4) -0.0480(5) 0.3684(5) 3.6(1)
C(3) 0.3131(4) -0.1366(4) 0.4181(4) 3.2(1)
C(4) 0.2423(4) -0.1086(5) 0.3460(4) 3.3(1)
C(5) 0.1536(4) -0.1203(5) 0.3899(4) 3.4(1)
C(6) 0.0716(5) -0.0331(5) 0.2637(5) 4.1(2)
C(7) 0.0046(4) -0.1683(5) 0.3408(5) 3.9(1)
C(11) 0.4229(4) -0.3060(4) 0.3716(5) 3.1(1)
C(12) 0.4344(4) -0.3881(5) 0.4246(5) 4.0(1)
C(13) 0.4073(5) -0.4708(5) 0.3823(6) 4.6(2)
C(14) 0.3681(5) -0.4692(5) 0.2915(5) 4.5(2)
C(15) 0.3586(4) -0.3862(5) 0.2435(5) 3.6(1)
C(21) 0.4071(4) 0.0120(5) 0.2883(5) 3.4(1)
C(22) 0.4046(4) 0.1085(5) 0.2939(5) 3.9(1)
C(23) 0.3689(5) 0.1585(5) 0.2193(6) 4.4(2)
C(24) 0.3354(5) 0.1129(5) 0.1397(5) 4.6(2)
C(25) 0.3401(4) 0.0173(5) 0.1366(5) 3.9(1)
C(31) -0.0390(4) -0.2114(5) 0.2534(5) 3.6(1)
C(32) -0.1283(5) -0.2168(6) 0.2416(6) 4.7(2)
C(33) -0.1616(5) -0.2633(7) 0.1615(6) 5.6(2)
C(34) -0.1058(5) -0.3033(6) 0.0953(6) 4.9(2)
C(35) -0.0186(4) -0.2937(5) 0.1122(5) 3.9(1)
C(41) 0.0975(4) -0.0288(5) 0.1598(5) 3.7(1)
C(42) 0.0886(7) 0.0516(6) 0.1059(6) 6.1(2)
C(43) 0.1083(8) 0.0524(6) 0.0119(7) 7.5(3)
C(44) 0.1430(7) -0.0263(6) -0.0316(6) 6.1(2)
C(45) 0.1511(5) -0.1043(5) 0.0252(5) 4.4(2)
H12 0.4601 -0.3868 0.4893 5.0
H13 0.4161 -0.5290 0.4160 5.0
H14 0.3469 -0.5261 0.2618 5.0
H15 0.3308 -0.3852 0.1798 5.0
H22 0.4282 0.1399 0.3505 5.0
H23 0.3671 0.2255 0.2227 5.0
H24 0.3085 0.1475 0.0870 5.0
H25 0.3167 -0.0150 0.0802 5.0
H32 -0.1665 -0.1887 0.2884 5.0
H33 -0.2240 -0.2673 0.1515 5.0
H34 -0.1285 -0.3368 0.0390 5.0
H35 0.0214 -0.3211 0.0667 5.0
H42 0.0658 0.1072 0.1368 5.0
H43 0.1001 0.1081 -0.0271 5.0
H44 0.1611 -0.0264 -0.0995 5.0
H45 0.1744 -0.1607 -0.0037 5.0
H111 0.4495 -0.2142 0.4793 5.0
H112 0.5129 -0.2053 0.3932 5.0
H211 0.5044 -0.0560 0.3599 5.0
H212 0.4347 -0.0177 0.4297 5.0
H311 0.3154 -0.0933 0.4709 5.0
H312 0.2995 -0.1966 0.4442 5.0
H411 0.2481 -0.0442 0.3277 5.0
H511 0.1524 -0.1769 0.4275 5.0
H512 0.1411 -0.0700 0.4331 5.0
H611 0.1030 0.0135 0.2994 5.0
H612 0.0105 -0.0185 0.2678 5.0
H711 -0.0327 -0.1227 0.3691 5.0
H712 0.0162 -0.2151 0.3894 5.0
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_22
_atom_site_aniso_U_23
_atom_site_aniso_U_33
I 0.0530(2) -0.0045(2) -0.0005(2) 0.0554(3) -0.0001(2) 0.0533(2)
V1 0.0426(5) 0.0002(5) 0.0059(5) 0.0389(6) -0.0016(5) 0.0360(5)
V2 0.0402(5) 0.0014(5) -0.0002(5) 0.0357(5) -0.0004(5) 0.0398(5)
O1 0.044(2) 0.004(2) 0.010(2) 0.054(3) -0.002(2) 0.061(3)
O2 0.058(3) -0.006(2) 0.011(2) 0.060(3) -0.008(2) 0.041(2)
O3 0.060(3) 0.002(2) 0.001(2) 0.049(3) 0.010(2) 0.050(3)
O4 0.054(3) 0.002(2) 0.000(2) 0.044(2) -0.007(2) 0.046(2)
O5 0.037(2) 0.002(2) -0.000(2) 0.046(2) -0.006(2) 0.032(2)
OW1 0.078(4) 0.018(3) 0.064(6) 0.053(4) 0.042(6) 0.40(1)
OW2 0.31(1) -0.046(9) 0.04(1) 0.144(8) 0.005(8) 0.18(1)
N1 0.034(2) -0.002(2) 0.000(2) 0.035(3) -0.004(2) 0.039(3)
N2 0.042(3) 0.002(2) 0.002(2) 0.041(3) -0.000(2) 0.039(3)
N11 0.040(3) 0.004(2) 0.005(2) 0.040(3) -0.003(2) 0.041(3)
N21 0.042(3) -0.002(2) 0.005(2) 0.041(3) 0.001(2) 0.041(3)
N31 0.046(3) -0.003(3) -0.001(2) 0.044(3) 0.004(3) 0.040(3)
N41 0.048(3) 0.002(3) -0.001(2) 0.044(3) 0.002(3) 0.038(3)
C1 0.041(3) 0.002(3) -0.005(3) 0.043(3) 0.001(3) 0.044(3)
C2 0.043(3) -0.006(3) -0.002(3) 0.045(4) -0.007(3) 0.050(4)
C3 0.042(3) -0.001(3) 0.002(3) 0.044(3) -0.004(3) 0.035(3)
C4 0.042(3) 0.002(3) 0.006(3) 0.043(3) -0.005(3) 0.040(3)
C5 0.040(3) -0.000(3) 0.002(3) 0.053(4) -0.004(3) 0.038(3)
C6 0.061(4) 0.010(3) 0.003(3) 0.041(4) -0.001(3) 0.055(4)
C7 0.038(3) -0.001(3) 0.009(3) 0.060(4) -0.002(3) 0.050(4)
C11 0.034(3) 0.005(3) 0.007(3) 0.043(3) -0.000(3) 0.042(3)
C12 0.049(4) 0.006(3) 0.003(3) 0.049(4) 0.004(3) 0.054(4)
C13 0.069(4) 0.007(4) 0.010(4) 0.042(4) 0.005(4) 0.062(4)
C14 0.061(4) 0.001(4) 0.010(4) 0.046(4) -0.006(4) 0.063(4)
C15 0.046(3) 0.002(3) 0.006(3) 0.040(3) -0.005(3) 0.051(4)
C21 0.038(3) -0.005(3) 0.010(3) 0.041(3) 0.002(3) 0.051(4)
C22 0.048(3) -0.010(3) 0.012(3) 0.044(4) -0.003(3) 0.055(4)
C23 0.057(4) -0.002(3) 0.018(4) 0.042(4) 0.005(4) 0.070(4)
C24 0.058(4) -0.000(4) 0.008(4) 0.055(4) 0.016(4) 0.061(4)
C25 0.052(4) -0.002(3) 0.006(3) 0.048(4) 0.006(3) 0.048(4)
C31 0.044(3) -0.002(3) 0.003(3) 0.044(4) 0.008(3) 0.049(4)
C32 0.044(4) -0.001(4) 0.007(4) 0.065(5) 0.000(4) 0.069(5)
C33 0.048(4) -0.016(4) -0.005(4) 0.091(6) 0.007(5) 0.075(5)
C34 0.058(4) -0.012(4) -0.008(4) 0.068(5) -0.002(4) 0.062(4)
C35 0.050(4) -0.004(3) -0.006(3) 0.050(4) -0.002(3) 0.048(4)
C41 0.050(4) 0.005(3) -0.005(3) 0.042(4) -0.001(3) 0.049(4)
C42 0.123(7) 0.015(5) 0.007(5) 0.042(4) 0.005(4) 0.068(5)
C43 0.160(9) 0.007(6) -0.002(6) 0.058(5) 0.025(4) 0.067(5)
C44 0.118(7) 0.002(5) -0.005(5) 0.066(5) 0.015(4) 0.047(4)
C45 0.066(4) -0.003(4) 0.003(3) 0.055(4) 0.003(4) 0.047(4)
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
_journal_paper_doi 10.1107/S0108270194009066