#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:08:04 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179953 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/48/7024818.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_7024818
loop_
_publ_author_name
'Langley, Stuart K.'
'Moubaraki, Boujemaa'
'Forsyth, Craig M.'
'Gass, Ian A.'
'Murray, Keith S.'
_publ_section_title
;
 Structure and magnetism of new lanthanide 6-wheel compounds utilizing
 triethanolamine as a stabilizing ligand.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1705
_journal_page_last               1708
_journal_paper_doi               10.1039/b921843b
_journal_volume                  39
_journal_year                    2010
_chemical_formula_sum            'C44 H110 Dy6 N12 O44'
_chemical_formula_weight         2486.44
_chemical_name_common            Dy6(tea)
_chemical_name_systematic
;
?
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   16.7756(3)
_cell_length_b                   16.7756(3)
_cell_length_c                   24.9858(9)
_cell_measurement_reflns_used    9926
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      30.43
_cell_measurement_theta_min      2.43
_cell_volume                     6089.5(3)
_computing_cell_refinement       'Bruker Apex2 V2.0'
_computing_data_collection       'Bruker Apex2 V2.0'
_computing_data_reduction        'Bruker Apex2 V2.0'
_computing_molecular_graphics    X-Seed
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker X8 Apex CCD'
_diffrn_measurement_method       'thin slice phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0417
_diffrn_reflns_av_sigmaI/netI    0.0292
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            15739
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.15
_exptl_absorpt_coefficient_mu    5.549
_exptl_absorpt_correction_T_max  0.330
_exptl_absorpt_correction_T_min  0.125
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.034
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3618
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.173
_refine_diff_density_min         -1.128
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     167
_refine_ls_number_reflns         3108
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0207
_refine_ls_R_factor_gt           0.0205
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0305P)²+12.3527P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0539
_refine_ls_wR_factor_ref         0.0541
_reflns_number_gt                3082
_reflns_number_total             3108
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b921843b.txt
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      R-3
_cod_database_code               7024818
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'
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_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'
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
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) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
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) .
