#------------------------------------------------------------------------------
#$Date: 2016-02-16 18:55:33 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176466 $
#$URL: svn://www.crystallography.net/cod/cif/8/10/11/8101165.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_8101165
loop_
_publ_author_name
'Haussühl, Eiken'
'Haussühl, Siegfried'
'Schreuer, Jürgen'
_publ_section_title
;
Crystal structure of bis(triethylenetetramine) tris(zirconium) hexa
(nitrilotriacetate) tetrahydrate, (NH₃(CH₂)₂NH(CH₂)₂NH₂
(CH₂)₂NH₃)₂(Zr)₃(N(CH₂COO)₃)₆ · 4H₂O
;
_journal_issue                   1
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              98
_journal_page_last               100
_journal_volume                  215
_journal_year                    2000
_chemical_formula_structural
;
NH3 (CH2)2 NH (CH2)2 NH2 (CH2)2 NH3)  (Zr)1.5 (N(CH2COO)3)3 (H2O)2
;
_chemical_formula_sum            'C24 H43 N7 O20 Zr1.5'
_chemical_formula_weight         886.48
_chemical_name_common
;
triethylenetetramine 1.5 zirconium tris(nitrilotriacetate) dihydrate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_cell_angle_alpha                90.00
_cell_angle_beta                 116.41(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   39.146(8)
_cell_length_b                   9.445(2)
_cell_length_c                   21.076(4)
_cell_measurement_temperature    293(2)
_cell_volume                     6979(2)
_diffrn_ambient_temperature      293(2)
_exptl_crystal_density_diffrn    1.687
_exptl_crystal_density_meas      1.685(2)
_refine_ls_R_factor_obs          0.0271
_refine_ls_wR_factor_obs         0.0728
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C24 H43 N7 O20 Zr1.50'
_cod_database_code               8101165
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zr1 Zr 0.176538(6) 0.83454(2) 0.281726(10) 0.02459(8) Uani 1 d . . .
Zr2 Zr 0.0000 0.23979(3) 0.2500 0.02670(9) Uani 1 d S . .
N1 N 0.21581(5) 1.0445(2) 0.29248(10) 0.0300(4) Uani 1 d . . .
N2 N 0.18067(5) 0.63910(19) 0.36264(9) 0.0273(4) Uani 1 d . . .
N3 N 0.05213(5) 0.1383(2) 0.22969(10) 0.0331(4) Uani 1 d . . .
N4 N 0.16234(7) 0.8639(3) 0.00211(15) 0.0509(6) Uani 1 d . . .
N5 N 0.10209(7) 0.8828(3) 0.04546(12) 0.0455(5) Uani 1 d . . .
N6 N 0.08369(7) 0.6055(3) 0.06716(11) 0.0461(5) Uani 1 d . . .
N7 N 0.04909(8) 0.3952(3) -0.10210(13) 0.0511(6) Uani 1 d . . .
C11 C 0.23737(7) 1.0794(3) 0.36833(13) 0.0356(5) Uani 1 d . . .
C12 C 0.24158(7) 1.0139(3) 0.25977(13) 0.0365(5) Uani 1 d . . .
C13 C 0.18902(8) 1.1604(3) 0.25384(15) 0.0400(6) Uani 1 d . . .
C14 C 0.21339(7) 1.0443(2) 0.40631(12) 0.0345(5) Uani 1 d . . .
C15 C 0.22303(6) 0.9128(2) 0.19806(12) 0.0313(5) Uani 1 d . . .
C16 C 0.15191(7) 1.1042(2) 0.19582(12) 0.0324(5) Uani 1 d . . .
C21 C 0.21956(7) 0.6352(3) 0.42120(12) 0.0354(5) Uani 1 d . . .
C22 C 0.15149(7) 0.6615(3) 0.38828(14) 0.0347(5) Uani 1 d . . .
C23 C 0.17297(7) 0.5068(2) 0.32049(13) 0.0324(5) Uani 1 d . . .
C24 C 0.24787(6) 0.6984(3) 0.39847(12) 0.0319(5) Uani 1 d . . .
C25 C 0.11811(7) 0.7458(3) 0.33614(14) 0.0376(5) Uani 1 d . . .
C26 C 0.14723(7) 0.5332(2) 0.24282(12) 0.0341(5) Uani 1 d . . .
C31 C 0.04204(7) -0.0102(3) 0.20804(14) 0.0380(5) Uani 1 d . . .
C32 C 0.08751(7) 0.1478(3) 0.29716(16) 0.0472(7) Uani 1 d . . .
C33 C 0.05536(10) 0.2196(3) 0.17254(18) 0.0507(7) Uani 1 d . . .
C34 C -0.00058(7) -0.0219(3) 0.16157(13) 0.0363(5) Uani 1 d . . .
C36 C 0.03140(7) 0.3508(3) 0.14848(14) 0.0457(7) Uani 1 d . . .
C35 C 0.08722(7) 0.2787(3) 0.33782(13) 0.0358(5) Uani 1 d . . .
C41 C 0.14320(9) 0.9981(3) 0.00268(18) 0.0535(7) Uani 1 d . . .
C42 C 0.10307(9) 0.9783(3) -0.00759(17) 0.0513(7) Uani 1 d . . .
C43 C 0.06407(9) 0.8568(4) 0.0388(2) 0.0576(8) Uani 1 d . . .
C44 C 0.06569(9) 0.7308(4) 0.08418(18) 0.0546(7) Uani 1 d . . .
C45 C 0.05879(10) 0.5598(4) -0.00701(17) 0.0659(9) Uani 1 d . . .
H45A H 0.0334 0.5401 -0.0120 0.85(12) Uiso 1 calc R . .
H45B H 0.0568 0.6362 -0.0392 0.85(12) Uiso 1 calc R . .
C46 C 0.07346(14) 0.4357(4) -0.02597(18) 0.0878(14) Uani 1 d . . .
H46A H 0.0742 0.3577 0.0046 0.089(4) Uiso 1 calc R . .
H46B H 0.0993 0.4537 -0.0188 0.089(4) Uiso 1 calc R . .
O14A O 0.22017(6) 1.1021(2) 0.46243(10) 0.0533(5) Uani 1 d . . .
O14B O 0.18740(5) 0.94886(17) 0.37642(8) 0.0351(4) Uani 1 d . . .
O15A O 0.23526(6) 0.9016(2) 0.15437(10) 0.0461(4) Uani 1 d . . .
O15B O 0.19485(5) 0.84020(17) 0.19745(8) 0.0355(4) Uani 1 d . . .
O16A O 0.13939(5) 0.99155(18) 0.21282(9) 0.0366(4) Uani 1 d . . .
O16B O 0.13499(5) 1.16560(19) 0.13930(10) 0.0449(4) Uani 1 d . . .
O24A O 0.28198(5) 0.6962(2) 0.43928(9) 0.0455(4) Uani 1 d . . .
O24B O 0.23359(4) 0.75802(17) 0.33692(8) 0.0324(3) Uani 1 d . . .
O25A O 0.08886(6) 0.7540(3) 0.34429(13) 0.0655(6) Uani 1 d . . .
O25B O 0.12268(5) 0.80982(19) 0.28744(9) 0.0389(4) Uani 1 d . . .
O26A O 0.12413(6) 0.4455(2) 0.20617(10) 0.0580(6) Uani 1 d . . .
O26B O 0.15376(5) 0.65106(17) 0.21932(9) 0.0391(4) Uani 1 d . . .
O34A O -0.01368(6) -0.1188(2) 0.11927(12) 0.0581(5) Uani 1 d . . .
O34B O -0.02075(4) 0.07551(18) 0.17244(8) 0.0348(4) Uani 1 d . . .
O35A O 0.11705(5) 0.3206(2) 0.38641(10) 0.0499(5) Uani 1 d . . .
O35B O 0.05453(5) 0.33539(18) 0.32009(10) 0.0403(4) Uani 1 d . . .
O36A O 0.03358(6) 0.4264(3) 0.10335(13) 0.0749(8) Uani 1 d . . .
O36B O 0.00864(5) 0.3742(2) 0.17622(10) 0.0471(5) Uani 1 d . . .
OW1 O 0.17022(9) 0.3576(3) 0.09179(19) 0.0821(8) Uani 1 d . . .
OW2 O 0.16108(7) 0.6324(2) 0.08607(11) 0.0521(5) Uani 1 d . . .
H11A H 0.2457(8) 1.173(3) 0.3745(16) 0.050(8) Uiso 1 d . . .
H11B H 0.2605(8) 1.017(3) 0.3892(14) 0.046(8) Uiso 1 d . . .
H12A H 0.2636(8) 0.964(3) 0.2921(15) 0.046(8) Uiso 1 d . . .
H12B H 0.2486(8) 1.099(3) 0.2446(15) 0.047(8) Uiso 1 d . . .
H13A H 0.2016(9) 1.229(3) 0.2350(16) 0.057(9) Uiso 1 d . . .
H13B H 0.1820(8) 1.209(3) 0.2839(15) 0.051(8) Uiso 1 d . . .
H21A H 0.2276(8) 0.544(3) 0.4389(14) 0.042(7) Uiso 1 d . . .
H21B H 0.2187(8) 0.694(3) 0.4566(16) 0.051(8) Uiso 1 d . . .
H22A H 0.1635(9) 0.718(3) 0.4308(16) 0.054(8) Uiso 1 d . . .
H22B H 0.1431(8) 0.575(3) 0.3993(15) 0.047(8) Uiso 1 d . . .
H23A H 0.1636(7) 0.441(3) 0.3399(13) 0.036(7) Uiso 1 d . . .
H23B H 0.1965(8) 0.478(3) 0.3207(14) 0.043(7) Uiso 1 d . . .
H31A H 0.0470(8) -0.069(3) 0.2473(15) 0.045(8) Uiso 1 d . . .
H31B H 0.0555(8) -0.044(3) 0.1823(16) 0.052(8) Uiso 1 d . . .
H32A H 0.1081(10) 0.146(4) 0.2883(18) 0.067(10) Uiso 1 d . . .
H32B H 0.0888(10) 0.058(4) 0.3277(18) 0.074(11) Uiso 1 d . . .
H33A H 0.0495(11) 0.169(4) 0.136(2) 0.082(12) Uiso 1 d . . .
H33B H 0.0801(12) 0.246(4) 0.186(2) 0.085(12) Uiso 1 d . . .
H41A H 0.1439(11) 1.059(4) -0.035(2) 0.089(4) Uiso 1 d . . .
H41B H 0.1594(11) 1.044(4) 0.046(2) 0.089(4) Uiso 1 d . . .
H42A H 0.0931(11) 1.072(4) -0.005(2) 0.089(4) Uiso 1 d . . .
H42B H 0.0858(11) 0.929(4) -0.052(2) 0.089(4) Uiso 1 d . . .
H43A H 0.0497(12) 0.824(4) -0.010(2) 0.089(4) Uiso 1 d . . .
H43B H 0.0486(11) 0.941(4) 0.048(2) 0.089(4) Uiso 1 d . . .
H44A H 0.0839(11) 0.745(4) 0.140(2) 0.089(4) Uiso 1 d . . .
H44B H 0.0373(12) 0.705(4) 0.075(2) 0.089(4) Uiso 1 d . . .
H4A H 0.1659(11) 0.796(4) 0.035(2) 0.083(7) Uiso 1 d . . .
H4B H 0.1860(11) 0.877(4) 0.001(2) 0.083(7) Uiso 1 d . . .
H4C H 0.1469(11) 0.813(4) -0.037(2) 0.083(7) Uiso 1 d . . .
H5A H 0.1148(10) 0.917(4) 0.0889(19) 0.073(11) Uiso 1 d . . .
H6A H 0.0903(9) 0.534(4) 0.0997(17) 0.061(9) Uiso 1 d . . .
H6B H 0.1096(8) 0.624(3) 0.0723(15) 0.047(8) Uiso 1 d . . .
H7A H 0.0295(11) 0.334(4) -0.111(2) 0.080(7) Uiso 1 d . . .
H7B H 0.0652(11) 0.343(4) -0.122(2) 0.080(7) Uiso 1 d . . .
H7C H 0.0372(11) 0.452(4) -0.128(2) 0.080(7) Uiso 1 d . . .
HW1A H 0.1601(11) 0.300(4) 0.109(2) 0.081(12) Uiso 1 d . . .
HW1B H 0.1837(12) 0.309(5) 0.083(2) 0.089(13) Uiso 1 d . . .
HW2A H 0.1705(12) 0.666(4) 0.119(2) 0.088(9) Uiso 1 d . . .
HW2B H 0.1655(11) 0.537(5) 0.086(2) 0.088(9) Uiso 1 d . . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zr1 O26B 2.1177(16) . ?
Zr1 O16A 2.1316(17) . ?
Zr1 O24B 2.1336(17) . ?
Zr1 O14B 2.1389(16) . ?
Zr1 O25B 2.1770(16) . ?
Zr1 O15B 2.1920(16) . ?
Zr1 N1 2.4573(19) . ?
Zr1 N2 2.4690(19) . ?
Zr2 O34B 2.1350(16) 2 ?
Zr2 O34B 2.1350(16) . ?
Zr2 O36B 2.1472(18) 2 ?
Zr2 O36B 2.1473(18) . ?
Zr2 O35B 2.1790(18) 2 ?
Zr2 O35B 2.1791(18) . ?
Zr2 N3 2.458(2) 2 ?
Zr2 N3 2.4584(19) . ?
N1 C11 1.475(3) . ?
N1 C12 1.482(3) . ?
N1 C13 1.483(3) . ?
N2 C21 1.474(3) . ?
N2 C22 1.480(3) . ?
N2 C23 1.484(3) . ?
N3 C31 1.474(3) . ?
N3 C33 1.480(3) . ?
N3 C32 1.482(3) . ?
N4 C41 1.475(4) . ?
N4 H4A 0.90(4) . ?
N4 H4B 0.94(4) . ?
N4 H4C 0.91(4) . ?
N5 C42 1.450(4) . ?
N5 C43 1.453(4) . ?
N5 H5A 0.89(4) . ?
N6 C45 1.491(4) . ?
N6 C44 1.500(4) . ?
N6 H6A 0.91(3) . ?
N6 H6B 0.99(3) . ?
N7 C46 1.506(4) . ?
N7 H7A 0.91(4) . ?
N7 H7B 1.02(4) . ?
N7 H7C 0.76(4) . ?
C11 C14 1.517(3) . ?
C11 H11A 0.93(3) . ?
C11 H11B 1.00(3) . ?
C12 C15 1.513(3) . ?
C12 H12A 0.95(3) . ?
C12 H12B 0.95(3) . ?
C13 C16 1.519(4) . ?
C13 H13A 1.00(3) . ?
C13 H13B 0.92(3) . ?
C14 O14A 1.220(3) . ?
C14 O14B 1.294(3) . ?
C15 O15A 1.217(3) . ?
C15 O15B 1.294(3) . ?
C16 O16B 1.222(3) . ?
C16 O16A 1.287(3) . ?
C21 C24 1.512(3) . ?
C21 H21A 0.94(3) . ?
C21 H21B 0.94(3) . ?
C22 C25 1.507(4) . ?
C22 H22A 0.97(3) . ?
C22 H22B 0.95(3) . ?
C23 C26 1.513(3) . ?
C23 H23A 0.91(3) . ?
C23 H23B 0.96(3) . ?
C24 O24A 1.226(3) . ?
C24 O24B 1.291(3) . ?
C25 O25A 1.234(3) . ?
C25 O25B 1.271(3) . ?
C26 O26A 1.216(3) . ?
C26 O26B 1.290(3) . ?
C31 C34 1.517(3) . ?
C31 H31A 0.94(3) . ?
C31 H31B 0.96(3) . ?
C32 C35 1.508(4) . ?
C32 H32A 0.91(4) . ?
C32 H32B 1.05(4) . ?
C33 C36 1.499(4) . ?
C33 H33A 0.85(4) . ?
C33 H33B 0.92(4) . ?
C34 O34A 1.220(3) . ?
C34 O34B 1.298(3) . ?
C36 O36A 1.223(3) . ?
C36 O36B 1.284(3) . ?
C35 O35A 1.227(3) . ?
C35 O35B 1.280(3) . ?
C41 C42 1.499(4) . ?
C41 H41A 0.99(4) . ?
C41 H41B 0.95(4) . ?
C42 H42A 0.98(4) . ?
C42 H42B 0.99(4) . ?
C43 C44 1.510(5) . ?
C43 H43A 0.98(4) . ?
C43 H43B 1.07(4) . ?
C44 H44A 1.07(4) . ?
C44 H44B 1.07(4) . ?
C45 C46 1.438(5) . ?
C45 H45A 0.9700 . ?
C45 H45B 0.9700 . ?
C46 H46A 0.9700 . ?
C46 H46B 0.9700 . ?
OW1 HW1A 0.85(4) . ?
OW1 HW1B 0.79(4) . ?
OW2 HW2A 0.71(4) . ?
OW2 HW2B 0.91(4) . ?
