data_global
_journal_name_full               'Dalton Trans.'

_journal_coden_Cambridge         0222

_publ_contact_author_name        'Keith Murray'
_publ_contact_author_email       KEITH.MURRAY@SCI.MONASH.EDU.AU

_publ_section_title              
;
Structure and magnetism of new lanthanide 6-wheel compounds
utilizing triethanolamine as a stabilizing ligand.
;
loop_
_publ_author_name
'Keith Murray'
'Craig M Forsyth'
'Ian A Gass'
'Stuart K. Langley'
'Boujemaa Moubaraki'

# Attachment 'StuartLangleyDy6final.CIF'

#==========================================================================
data_1
_database_code_depnum_ccdc_archive 'CCDC 751869'

_chemical_name_systematic        
;
?
;
_chemical_name_common            Dy6(tea)
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44 H110 Dy6 N12 O44'
_chemical_formula_weight         2486.44

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   R-3
_symmetry_space_group_name_Hall  '-R 3'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   16.7756(3)
_cell_length_b                   16.7756(3)
_cell_length_c                   24.9858(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     6089.5(3)
_cell_formula_units_Z            3
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    9926
_cell_measurement_theta_min      2.43
_cell_measurement_theta_max      30.43

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.034
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3618
_exptl_absorpt_coefficient_mu    5.549
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.125
_exptl_absorpt_correction_T_max  0.330
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker X8 Apex CCD'
_diffrn_measurement_method       'thin slice phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            15739
_diffrn_reflns_av_R_equivalents  0.0417
_diffrn_reflns_av_sigmaI/netI    0.0292
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         2.15
_diffrn_reflns_theta_max         27.49
_reflns_number_total             3108
_reflns_number_gt                3082
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker Apex2 V2.0'
_computing_cell_refinement       'Bruker Apex2 V2.0'
_computing_data_reduction        'Bruker Apex2 V2.0'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    X-Seed
_computing_publication_material  CIFTAB

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
The Dy6 compound was merohedrally twinned and was solved using the
appropriate twin command.
The asymmetric unit contains one Dysprosium ion as well as one
teaH2-, one nitrate, with one methanol solvent molecule at full
occupancy and one lying on the crystallographic c-axis
at one-third occupancy
The MeoH lying on the 3-fold axis is diorderded over two sites
each at 0.16667 occupancy. A Exyz command is placed on atoms
C10 and C10a with EADP commands being placed
on C10 and C10a and O7 and O7a.
The hydrogen atom found on the protonated
teaH2- arm is restrained in place by DFIX and DANG commands.
All non-H atoms were refined anisotrpically. All H-atoms were placed
in calculated positions except for H3.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0305P)^2^+12.3527P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3108
_refine_ls_number_parameters     167
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0207
_refine_ls_R_factor_gt           0.0205
_refine_ls_wR_factor_ref         0.0541
_refine_ls_wR_factor_gt          0.0539
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_restrained_S_all      1.081
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.007942(13) 0.226195(12) 0.000238(13) 0.01117(6) Uani 1 1 d . . .
O1 O 0.1280(2) 0.24022(18) 0.05283(9) 0.0149(6) Uani 1 1 d . . .
O2 O -0.0930(3) 0.1015(3) 0.04792(9) 0.0169(6) Uani 1 1 d . . .
O3 O -0.0960(3) 0.2872(3) 0.00991(17) 0.0274(8) Uani 1 1 d D . .
H3 H -0.1456(17) 0.2554(14) -0.0097(13) 0.033 Uiso 1 1 d D . .
O4 O 0.1079(2) 0.3974(2) -0.00396(15) 0.0213(7) Uani 1 1 d . . .
O5 O 0.0337(2) 0.3340(2) -0.07723(13) 0.0215(6) Uani 1 1 d . . .
O6 O -0.2009(4) 0.3095(4) -0.0634(3) 0.0684(15) Uani 1 1 d D . .
H6 H -0.2473 0.3029 -0.0467 0.082 Uiso 1 1 calc R . .
O7 O 0.3333 0.6667 0.0055(11) 0.095(4) Uani 0.50 3 d SP A 1
H7 H 0.2886 0.6173 0.0156 0.115 Uiso 0.17 1 d P B 1
O7A O 0.3333 0.6667 -0.1093(10) 0.095(4) Uani 0.50 3 d SP C 2
H7A H 0.2802 0.6506 -0.1181 0.115 Uiso 0.17 1 d P D 2
N1 N -0.0016(2) 0.2763(3) 0.09664(15) 0.0218(8) Uani 1 1 d . . .
C1 C 0.1422(3) 0.2723(3) 0.10646(14) 0.0192(8) Uani 1 1 d . . .
H1A H 0.2090 0.3121 0.1132 0.023 Uiso 1 1 calc R . .
H1B H 0.1185 0.2193 0.1313 0.023 Uiso 1 1 calc R . .
C2 C 0.0935(3) 0.3261(3) 0.11664(17) 0.0214(9) Uani 1 1 d . . .
H2A H 0.0931 0.3371 0.1555 0.026 Uiso 1 1 calc R . .
H2B H 0.1274 0.3867 0.0986 0.026 Uiso 1 1 calc R . .
C3 C -0.0712(3) 0.1054(3) 0.10273(16) 0.0236(10) Uani 1 1 d . . .
H3A H -0.0127 0.1048 0.1067 0.028 Uiso 1 1 calc R . .
H3B H -0.1202 0.0504 0.1212 0.028 Uiso 1 1 calc R . .
C4 C -0.0617(3) 0.1909(3) 0.12816(19) 0.0267(10) Uani 1 1 d . . .
H4A H -0.1236 0.1841 0.1319 0.032 Uiso 1 1 calc R . .
H4B H -0.0356 0.1977 0.1645 0.032 Uiso 1 1 calc R . .
C5 C -0.1226(4) 0.3045(4) 0.0608(2) 0.0327(12) Uani 1 1 d D . .
H5A H -0.1745 0.2473 0.0755 0.039 Uiso 1 1 calc R . .
H5B H -0.1420 0.3512 0.0575 0.039 Uiso 1 1 calc R . .
C6 C -0.0407(4) 0.3388(4) 0.0962(2) 0.0307(12) Uani 1 1 d . . .
H6A H -0.0582 0.3451 0.1331 0.037 Uiso 1 1 calc R . .
H6B H 0.0071 0.4005 0.0838 0.037 Uiso 1 1 calc R . .
N7 N 0.0842(3) 0.4074(3) -0.05049(18) 0.0230(8) Uani 1 1 d . . .
O8 O 0.1087(3) 0.4830(2) -0.07032(16) 0.0361(9) Uani 1 1 d . . .
C9 C -0.1465(7) 0.4016(7) -0.0792(5) 0.101(4) Uani 1 1 d . . .
H9A H -0.1487 0.4419 -0.0516 0.152 Uiso 1 1 calc R . .
H9B H -0.1701 0.4115 -0.1130 0.152 Uiso 1 1 calc R . .
H9C H -0.0827 0.4159 -0.0841 0.152 Uiso 1 1 calc R . .
C10 C 0.3333 0.6667 -0.0498(7) 0.073(4) Uani 0.50 3 d SP A 1
H10A H 0.2982 0.6950 -0.0649 0.109 Uiso 0.166 1 d P E 1
H10B H 0.3050 0.6032 -0.0649 0.109 Uiso 0.166 1 d P F 1
H10C H 0.3968 0.7018 -0.0649 0.109 Uiso 0.166 1 d P G 1
C10A C 0.3333 0.6667 -0.0498(7) 0.073(4) Uani 0.50 3 d SP C 2
H10D H 0.3796 0.6520 -0.0388 0.109 Uiso 0.166 1 d P H 2
H10E H 0.2724 0.6204 -0.0388 0.109 Uiso 0.166 1 d P I 2
H10F H 0.3480 0.7276 -0.0388 0.109 Uiso 0.166 1 d P J 2

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Dy1 0.01074(8) 0.01110(9) 0.01149(9) -0.00063(7) 0.00074(7) 0.00533(7)
O1 0.0170(16) 0.0186(13) 0.0112(11) -0.0033(10) -0.0018(13) 0.0105(12)
O2 0.0185(17) 0.0191(16) 0.0079(10) 0.0019(13) 0.0022(14) 0.0055(12)
O3 0.028(2) 0.0307(18) 0.0317(18) -0.0106(16) -0.0076(17) 0.0208(15)
O4 0.0238(17) 0.0152(16) 0.0216(18) -0.0001(14) -0.0027(14) 0.0074(14)
O5 0.0247(17) 0.0165(15) 0.0209(17) 0.0018(13) -0.0009(14) 0.0086(13)
O6 0.063(4) 0.064(3) 0.082(4) 0.003(3) -0.004(3) 0.034(3)
O7 0.073(6) 0.073(6) 0.140(13) 0.000 0.000 0.037(3)
O7A 0.073(6) 0.073(6) 0.140(13) 0.000 0.000 0.037(3)
N1 0.0171(18) 0.0248(19) 0.0224(19) -0.0082(17) 0.0017(15) 0.0096(17)
C1 0.023(2) 0.0229(19) 0.0146(16) -0.0050(14) -0.0021(18) 0.013(2)
C2 0.019(2) 0.025(2) 0.0194(19) -0.0101(17) -0.0015(16) 0.0101(19)
C3 0.021(2) 0.027(2) 0.0103(17) 0.0020(16) -0.0024(15) 0.003(2)
C4 0.021(2) 0.036(3) 0.015(2) -0.007(2) 0.0007(17) 0.009(2)
C5 0.025(2) 0.032(3) 0.047(3) -0.017(3) 0.003(2) 0.019(2)
C6 0.028(3) 0.035(3) 0.031(3) -0.018(2) 0.000(2) 0.017(2)
N7 0.0220(19) 0.0186(19) 0.027(2) -0.0005(17) 0.0018(16) 0.0094(17)
O8 0.047(2) 0.0143(16) 0.041(2) 0.0079(15) -0.0012(18) 0.0115(17)
C9 0.096(7) 0.073(6) 0.154(10) 0.053(7) 0.049(8) 0.057(6)
C10 0.036(4) 0.036(4) 0.146(14) 0.000 0.000 0.0182(19)
C10A 0.036(4) 0.036(4) 0.146(14) 0.000 0.000 0.0182(19)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
Dy1 O2 2.242(4) 11 ?
Dy1 O2 2.263(4) . ?
Dy1 O1 2.284(3) 12 ?
Dy1 O1 2.316(3) . ?
Dy1 O3 2.434(3) . ?
Dy1 O4 2.501(3) . ?
Dy1 O5 2.534(3) . ?
Dy1 N1 2.582(4) . ?
Dy1 N7 2.932(4) . ?
Dy1 Dy1 3.72975(17) 12 ?
Dy1 Dy1 3.72975(17) 11 ?
O1 C1 1.419(4) . ?
O1 Dy1 2.284(3) 11 ?
O2 C3 1.411(4) . ?
O2 Dy1 2.242(4) 12 ?
O3 C5 1.425(6) . ?
O4 N7 1.267(6) . ?
O5 N7 1.280(5) . ?
O6 C9 1.402(10) . ?
O7 C10 1.38(3) . ?
N1 C2 1.470(5) . ?
N1 C6 1.488(6) . ?
N1 C4 1.498(6) . ?
C1 C2 1.512(6) . ?
C3 C4 1.504(7) . ?
C5 C6 1.487(8) . ?
N7 O8 1.225(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Dy1 O2 110.68(14) 11 . ?
O2 Dy1 O1 89.30(10) 11 12 ?
O2 Dy1 O1 69.88(10) . 12 ?
O2 Dy1 O1 69.65(10) 11 . ?
O2 Dy1 O1 90.36(11) . . ?
O1 Dy1 O1 144.27(12) 12 . ?
O2 Dy1 O3 152.36(12) 11 . ?
O2 Dy1 O3 88.49(12) . . ?
O1 Dy1 O3 78.55(11) 12 . ?
O1 Dy1 O3 132.06(12) . . ?
O2 Dy1 O4 95.87(11) 11 . ?
O2 Dy1 O4 147.75(11) . . ?
O1 Dy1 O4 130.33(11) 12 . ?
O1 Dy1 O4 81.80(11) . . ?
O3 Dy1 O4 74.43(11) . . ?
O2 Dy1 O5 82.49(10) 11 . ?
O2 Dy1 O5 147.50(11) . . ?
O1 Dy1 O5 81.10(11) 12 . ?
O1 Dy1 O5 122.11(10) . . ?
O3 Dy1 O5 71.23(13) . . ?
O4 Dy1 O5 51.05(11) . . ?
O2 Dy1 N1 137.93(11) 11 . ?
O2 Dy1 N1 70.74(12) . . ?
O1 Dy1 N1 126.89(10) 12 . ?
O1 Dy1 N1 68.29(11) . . ?
O3 Dy1 N1 66.21(13) . . ?
O4 Dy1 N1 77.32(13) . . ?
O5 Dy1 N1 119.76(13) . . ?
O2 Dy1 N7 91.09(10) 11 . ?
O2 Dy1 N7 157.35(11) . . ?
O1 Dy1 N7 105.50(11) 12 . ?
O1 Dy1 N7 103.50(11) . . ?
O3 Dy1 N7 68.91(13) . . ?
O4 Dy1 N7 25.41(12) . . ?
O5 Dy1 N7 25.79(11) . . ?
N1 Dy1 N7 97.57(13) . . ?
O2 Dy1 Dy1 104.78(8) 11 12 ?
O2 Dy1 Dy1 33.93(8) . 12 ?
O1 Dy1 Dy1 36.11(7) 12 12 ?
O1 Dy1 Dy1 120.51(7) . 12 ?
O3 Dy1 Dy1 79.75(10) . 12 ?
O4 Dy1 Dy1 153.65(9) . 12 ?
O5 Dy1 Dy1 115.14(8) . 12 ?
N1 Dy1 Dy1 97.13(8) . 12 ?
N7 Dy1 Dy1 135.96(8) . 12 ?
O2 Dy1 Dy1 34.29(7) 11 11 ?
O2 Dy1 Dy1 105.27(7) . 11 ?
O1 Dy1 Dy1 120.04(7) 12 11 ?
O1 Dy1 Dy1 35.53(7) . 11 ?
O3 Dy1 Dy1 159.59(10) . 11 ?
O4 Dy1 Dy1 86.23(9) . 11 ?
O5 Dy1 Dy1 101.71(8) . 11 ?
N1 Dy1 Dy1 103.68(8) . 11 ?
N7 Dy1 Dy1 96.22(8) . 11 ?
Dy1 Dy1 Dy1 120.0 12 11 ?
C1 O1 Dy1 127.7(3) . 11 ?
C1 O1 Dy1 123.2(3) . . ?
Dy1 O1 Dy1 108.36(9) 11 . ?
C3 O2 Dy1 133.2(3) . 12 ?
C3 O2 Dy1 114.3(3) . . ?
Dy1 O2 Dy1 111.78(10) 12 . ?
C5 O3 Dy1 122.5(3) . . ?
N7 O4 Dy1 96.7(3) . . ?
N7 O5 Dy1 94.7(3) . . ?
C2 N1 C6 109.7(4) . . ?
C2 N1 C4 112.7(4) . . ?
C6 N1 C4 110.8(4) . . ?
C2 N1 Dy1 106.0(2) . . ?
C6 N1 Dy1 110.0(3) . . ?
C4 N1 Dy1 107.5(3) . . ?
O1 C1 C2 110.3(4) . . ?
N1 C2 C1 111.1(3) . . ?
O2 C3 C4 110.8(4) . . ?
N1 C4 C3 112.9(4) . . ?
O3 C5 C6 106.6(4) . . ?
C5 C6 N1 112.3(4) . . ?
O8 N7 O4 122.9(4) . . ?
O8 N7 O5 120.2(4) . . ?
O4 N7 O5 116.9(4) . . ?
O8 N7 Dy1 174.0(3) . . ?
O4 N7 Dy1 57.9(2) . . ?
O5 N7 Dy1 59.5(2) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.49
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.173
_refine_diff_density_min         -1.128
_refine_diff_density_rms         0.139

# Attachment 'StuartLangleyGd6final.CIF'

#==========================================================================
data_2
_database_code_depnum_ccdc_archive 'CCDC 751870'

_chemical_name_systematic        
;
?
;
_chemical_name_common            Gd6(tea)
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44 H110 Gd6 N12 O44'
_chemical_formula_weight         2454.94

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   R-3
_symmetry_space_group_name_Hall  '-R 3'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   16.8519(12)
_cell_length_b                   16.8519(12)
_cell_length_c                   25.031(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     6156.1(8)
_cell_formula_units_Z            3
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    9946
_cell_measurement_theta_min      2.91
_cell_measurement_theta_max      30.59

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.987
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3582
_exptl_absorpt_coefficient_mu    4.875
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.164
_exptl_absorpt_correction_T_max  0.377
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker X8 Apex CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            47563
_diffrn_reflns_av_R_equivalents  0.0332
_diffrn_reflns_av_sigmaI/netI    0.0118
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         2.14
_diffrn_reflns_theta_max         27.47
_reflns_number_total             3143
_reflns_number_gt                3133
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker Apex2 V2.0'
_computing_cell_refinement       'Bruker Apex2 V2.0'
_computing_data_reduction        'Bruker Apex2 V2.0'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    x-seed
_computing_publication_material  CIFTAB

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
The compound was merohedrally twinned and was solved using the
appropriate twin command.
The asymmetric unit contains one Gadolnium ion as well as one
teaH2-, one nitrate, with one methanol solvent molecule at full
occupancy and one lying on the crystallographic c-axis
at one-third occupancy
The MeoH lying on the 3-fold axis is diorderded over two sites
each at 0.16667 occupancy, some restraints are placed on the molecule.
The hydrogen atom found on the protonated
teaH2- arm is restrained in place.
All non-H atoms were refined anisotrpically. All H-atoms were placed
in calculated positions except for H3.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0271P)^2^+8.4839P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3143
_refine_ls_number_parameters     167
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0139
_refine_ls_R_factor_gt           0.0138
_refine_ls_wR_factor_ref         0.0393
_refine_ls_wR_factor_gt          0.0392
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_restrained_S_all      1.100
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Gd1 Gd 0.008191(9) 0.227966(8) 0.000165(8) 0.01464(4) Uani 1 1 d . . .
O1 O 0.12836(15) 0.24117(12) 0.05331(6) 0.0188(4) Uani 1 1 d . . .
O2 O -0.09337(17) 0.10265(17) 0.04827(6) 0.0215(4) Uani 1 1 d . . .
O3 O -0.09590(18) 0.28940(19) 0.01103(12) 0.0347(5) Uani 1 1 d D . .
H3 H -0.1501(10) 0.2579(14) -0.0041(11) 0.042 Uiso 1 1 d D . .
O4 O 0.10835(18) 0.40038(15) -0.00490(11) 0.0295(5) Uani 1 1 d . . .
O5 O 0.03312(16) 0.33690(15) -0.07697(9) 0.0274(4) Uani 1 1 d . . .
O6 O -0.2008(3) 0.3108(3) -0.06153(19) 0.0770(11) Uani 1 1 d D . .
H6 H -0.2442 0.3054 -0.0424 0.092 Uiso 1 1 calc R . .
O7 O 0.3333 0.6667 0.0037(9) 0.108(4) Uani 0.50 3 d SP A 1
H7 H 0.2886 0.6173 0.0156 0.130 Uiso 0.17 1 d P B 1
O7A O 0.3333 0.6667 -0.1109(8) 0.108(4) Uani 0.50 3 d SP C 2
H7A H 0.2802 0.6506 -0.1181 0.130 Uiso 0.17 1 d P D 2
N1 N -0.00162(16) 0.27616(19) 0.09753(10) 0.0274(5) Uani 1 1 d . . .
C1 C 0.1418(2) 0.27275(19) 0.10656(9) 0.0245(5) Uani 1 1 d . . .
H1A H 0.2082 0.3122 0.1135 0.029 Uiso 1 1 calc R . .
H1B H 0.1179 0.2198 0.1312 0.029 Uiso 1 1 calc R . .
C2 C 0.09364(19) 0.3262(2) 0.11710(11) 0.0276(6) Uani 1 1 d . . .
H2A H 0.0937 0.3373 0.1560 0.033 Uiso 1 1 calc R . .
H2B H 0.1270 0.3865 0.0990 0.033 Uiso 1 1 calc R . .
C3 C -0.0703(2) 0.1055(2) 0.10259(10) 0.0282(6) Uani 1 1 d . . .
H3A H -0.0119 0.1051 0.1058 0.034 Uiso 1 1 calc R . .
H3B H -0.1186 0.0506 0.1211 0.034 Uiso 1 1 calc R . .
C4 C -0.0605(2) 0.1907(2) 0.12856(12) 0.0329(7) Uani 1 1 d . . .
H4A H -0.1221 0.1836 0.1329 0.039 Uiso 1 1 calc R . .
H4B H -0.0339 0.1970 0.1646 0.039 Uiso 1 1 calc R . .
C5 C -0.1221(3) 0.3046(3) 0.06273(17) 0.0406(9) Uani 1 1 d D . .
H5A H -0.1731 0.2468 0.0771 0.049 Uiso 1 1 calc R . .
H5B H -0.1423 0.3504 0.0605 0.049 Uiso 1 1 calc R . .
C6 C -0.0403(3) 0.3387(3) 0.09785(16) 0.0403(9) Uani 1 1 d . . .
H6A H -0.0576 0.3445 0.1348 0.048 Uiso 1 1 calc R . .
H6B H 0.0072 0.4002 0.0857 0.048 Uiso 1 1 calc R . .
N7 N 0.0845(2) 0.40984(19) -0.05090(12) 0.0278(5) Uani 1 1 d . . .
O8 O 0.1090(2) 0.48485(17) -0.07063(12) 0.0469(7) Uani 1 1 d . . .
C9 C -0.1487(6) 0.4006(5) -0.0782(3) 0.107(3) Uani 1 1 d . . .
H9A H -0.1480 0.4416 -0.0502 0.161 Uiso 1 1 calc R . .
H9B H -0.1751 0.4096 -0.1109 0.161 Uiso 1 1 calc R . .
H9C H -0.0859 0.4143 -0.0853 0.161 Uiso 1 1 calc R . .
C10 C 0.3333 0.6667 -0.0525(5) 0.080(3) Uani 0.50 3 d SP A 1
H10A H 0.2982 0.6950 -0.0649 0.120 Uiso 0.166 1 d P E 1
H10B H 0.3050 0.6032 -0.0649 0.120 Uiso 0.166 1 d P F 1
H10C H 0.3968 0.7018 -0.0649 0.120 Uiso 0.166 1 d P G 1
C10A C 0.3333 0.6667 -0.0525(5) 0.080(3) Uani 0.50 3 d SP C 2
H10D H 0.3796 0.6520 -0.0388 0.120 Uiso 0.166 1 d P H 2
H10E H 0.2724 0.6204 -0.0388 0.120 Uiso 0.166 1 d P I 2
H10F H 0.3480 0.7276 -0.0388 0.120 Uiso 0.166 1 d P J 2

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Gd1 0.01383(6) 0.01472(6) 0.01499(6) -0.00062(4) 0.00090(5) 0.00685(4)
O1 0.0202(10) 0.0232(9) 0.0150(7) -0.0039(6) -0.0016(8) 0.0124(8)
O2 0.0212(11) 0.0233(10) 0.0118(7) 0.0029(8) 0.0010(8) 0.0050(8)
O3 0.0331(13) 0.0372(12) 0.0436(14) -0.0092(11) -0.0051(12) 0.0250(10)
O4 0.0304(11) 0.0185(10) 0.0331(13) 0.0014(9) -0.0045(10) 0.0074(9)
O5 0.0294(12) 0.0213(10) 0.0282(11) 0.0030(9) -0.0020(9) 0.0101(9)
O6 0.069(3) 0.077(3) 0.091(3) 0.003(2) -0.006(2) 0.041(2)
O7 0.076(4) 0.076(4) 0.172(12) 0.000 0.000 0.038(2)
O7A 0.076(4) 0.076(4) 0.172(12) 0.000 0.000 0.038(2)
N1 0.0181(11) 0.0302(13) 0.0306(12) -0.0150(11) 0.0003(9) 0.0097(11)
C1 0.0255(15) 0.0310(13) 0.0179(10) -0.0076(9) -0.0021(11) 0.0148(13)
C2 0.0235(13) 0.0328(15) 0.0256(13) -0.0129(12) -0.0032(10) 0.0134(13)
C3 0.0251(15) 0.0308(16) 0.0133(11) 0.0018(10) -0.0027(10) 0.0025(13)
C4 0.0256(14) 0.0471(19) 0.0175(12) -0.0055(13) 0.0041(11) 0.0117(14)
C5 0.0309(16) 0.043(2) 0.057(2) -0.0235(19) -0.0016(17) 0.0251(16)
C6 0.0333(17) 0.043(2) 0.0460(19) -0.0259(17) -0.0027(15) 0.0203(16)
N7 0.0285(13) 0.0204(12) 0.0334(14) 0.0026(11) 0.0022(11) 0.0114(11)
O8 0.0604(18) 0.0190(11) 0.0531(16) 0.0097(11) -0.0022(14) 0.0138(12)
C9 0.118(6) 0.084(5) 0.144(7) 0.053(5) 0.048(5) 0.069(4)
C10 0.048(3) 0.048(3) 0.144(10) 0.000 0.000 0.0241(16)
C10A 0.048(3) 0.048(3) 0.144(10) 0.000 0.000 0.0241(16)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
Gd1 O2 2.270(2) 11 ?
Gd1 O2 2.286(2) . ?
Gd1 O1 2.312(2) 12 ?
Gd1 O1 2.339(2) . ?
Gd1 O3 2.457(2) . ?
Gd1 O4 2.530(2) . ?
Gd1 O5 2.550(2) . ?
Gd1 N1 2.600(2) . ?
Gd1 N7 2.956(3) . ?
Gd1 Gd1 3.7745(3) 12 ?
Gd1 Gd1 3.7745(3) 11 ?
O1 C1 1.411(3) . ?
O1 Gd1 2.312(2) 11 ?
O2 C3 1.408(3) . ?
O2 Gd1 2.270(2) 12 ?
O3 C5 1.431(5) . ?
O4 N7 1.256(4) . ?
O5 N7 1.274(4) . ?
O6 C9 1.380(7) . ?
O7 C10 1.40(2) . ?
N1 C2 1.475(3) . ?
N1 C6 1.490(4) . ?
N1 C4 1.494(4) . ?
C1 C2 1.507(4) . ?
C3 C4 1.508(5) . ?
C5 C6 1.487(5) . ?
N7 O8 1.221(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Gd1 O2 110.63(10) 11 . ?
O2 Gd1 O1 89.26(6) 11 12 ?
O2 Gd1 O1 69.70(7) . 12 ?
O2 Gd1 O1 69.50(6) 11 . ?
O2 Gd1 O1 90.06(7) . . ?
O1 Gd1 O1 143.70(8) 12 . ?
O2 Gd1 O3 153.14(8) 11 . ?
O2 Gd1 O3 88.19(8) . . ?
O1 Gd1 O3 79.26(8) 12 . ?
O1 Gd1 O3 131.57(8) . . ?
O2 Gd1 O4 95.81(8) 11 . ?
O2 Gd1 O4 148.07(8) . . ?
O1 Gd1 O4 130.13(8) 12 . ?
O1 Gd1 O4 82.56(8) . . ?
O3 Gd1 O4 74.25(8) . . ?
O2 Gd1 O5 83.32(7) 11 . ?
O2 Gd1 O5 147.32(7) . . ?
O1 Gd1 O5 81.50(7) 12 . ?
O1 Gd1 O5 122.62(7) . . ?
O3 Gd1 O5 71.09(9) . . ?
O4 Gd1 O5 50.23(8) . . ?
O2 Gd1 N1 137.44(7) 11 . ?
O2 Gd1 N1 70.10(8) . . ?
O1 Gd1 N1 126.78(7) 12 . ?
O1 Gd1 N1 67.94(7) . . ?
O3 Gd1 N1 66.07(9) . . ?
O4 Gd1 N1 78.37(9) . . ?
O5 Gd1 N1 119.88(9) . . ?
O2 Gd1 N7 91.26(7) 11 . ?
O2 Gd1 N7 157.24(8) . . ?
O1 Gd1 N7 105.71(7) 12 . ?
O1 Gd1 N7 103.91(7) . . ?
O3 Gd1 N7 69.08(9) . . ?
O4 Gd1 N7 24.95(9) . . ?
O5 Gd1 N7 25.39(7) . . ?
N1 Gd1 N7 98.28(9) . . ?
O2 Gd1 Gd1 104.87(5) 11 12 ?
O2 Gd1 Gd1 33.91(5) . 12 ?
O1 Gd1 Gd1 35.98(5) 12 12 ?
O1 Gd1 Gd1 120.18(4) . 12 ?
O3 Gd1 Gd1 79.80(7) . 12 ?
O4 Gd1 Gd1 153.36(6) . 12 ?
O5 Gd1 Gd1 115.16(5) . 12 ?
N1 Gd1 Gd1 96.66(6) . 12 ?
N7 Gd1 Gd1 135.88(6) . 12 ?
O2 Gd1 Gd1 34.18(5) 11 11 ?
O2 Gd1 Gd1 105.22(5) . 11 ?
O1 Gd1 Gd1 119.84(4) 12 11 ?
O1 Gd1 Gd1 35.51(4) . 11 ?
O3 Gd1 Gd1 159.36(7) . 11 ?
O4 Gd1 Gd1 86.48(6) . 11 ?
O5 Gd1 Gd1 102.31(5) . 11 ?
N1 Gd1 Gd1 103.31(5) . 11 ?
N7 Gd1 Gd1 96.38(6) . 11 ?
Gd1 Gd1 Gd1 120.0 12 11 ?
C1 O1 Gd1 127.88(19) . 11 ?
C1 O1 Gd1 122.75(19) . . ?
Gd1 O1 Gd1 108.51(6) 11 . ?
C3 O2 Gd1 133.33(19) . 12 ?
C3 O2 Gd1 114.23(19) . . ?
Gd1 O2 Gd1 111.91(6) 12 . ?
C5 O3 Gd1 121.6(2) . . ?
N7 O4 Gd1 96.86(18) . . ?
N7 O5 Gd1 95.43(17) . . ?
C2 N1 C6 109.2(3) . . ?
C2 N1 C4 112.8(3) . . ?
C6 N1 C4 111.3(3) . . ?
C2 N1 Gd1 105.62(16) . . ?
C6 N1 Gd1 110.1(2) . . ?
C4 N1 Gd1 107.54(18) . . ?
O1 C1 C2 111.0(2) . . ?
N1 C2 C1 110.9(2) . . ?
O2 C3 C4 110.2(3) . . ?
N1 C4 C3 113.4(2) . . ?
O3 C5 C6 107.1(3) . . ?
C5 C6 N1 111.9(3) . . ?
O8 N7 O4 122.6(3) . . ?
O8 N7 O5 120.5(3) . . ?
O4 N7 O5 117.0(3) . . ?
O8 N7 Gd1 174.3(2) . . ?
O4 N7 Gd1 58.19(15) . . ?
O5 N7 Gd1 59.18(15) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.47
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.026
_refine_diff_density_min         -0.953
_refine_diff_density_rms         0.087