# Supplementary Material (ESI) for Chemical Communications
# This journal is (c) The Royal Society of Chemistry 2006

data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182

_publ_contact_author_name        'Christopher L. Cahill'
_publ_contact_author_address     
;
Department of Chemistry
George Washington University
725 21st Street, NW
Washington, DC 20052
;
_publ_contact_author_email       cahill@gwu.edu
_publ_contact_author_phone       202-994-6959
_publ_contact_author_fax         202-994-5873

_publ_section_title              
;
An Unusually High Thermal Stability within a Novel
Lanthanide 1,3,5-Cyclohexanetricarboxylate Framework:
Synthesis, Structure, and Thermal Data.
;

loop_
_publ_author_name
_publ_author_address

'D.T.de Lill'
;Department of Chemistry
The George Washington University
725 21st Street, NW
Washington, DC 20052
;
C.L.Cahill
;Department of Chemistry
The George Washington University
725 21st Street, NW
Washington, DC 20052

AND

Carnegie Insitution of Washington
Geophysical Laboratory
5251 Broad Branch Road, NW
Washington, DC 20015
;

data_DD3_48
_database_code_depnum_ccdc_archive 'CCDC 614837'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C9 H9 Er O6'
_chemical_formula_sum            'C9 H9 Er O6'
_chemical_formula_weight         380.42

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_H-M   R-3c

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'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'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'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'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-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'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-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'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'

_cell_length_a                   8.820(3)
_cell_length_b                   8.820(3)
_cell_length_c                   20.727(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     1396.4(11)
_cell_formula_units_Z            6
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    4700
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       plate
_exptl_crystal_colour            'light pink'
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.714
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1074
_exptl_absorpt_coefficient_mu    9.025
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.051
_exptl_absorpt_correction_T_max  0.165
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      295(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 Apex CCD'
_diffrn_measurement_method       'omega and Phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7981
_diffrn_reflns_av_R_equivalents  0.0618
_diffrn_reflns_av_sigmaI/netI    0.0208
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         3.31
_diffrn_reflns_theta_max         30.31
_reflns_number_total             457
_reflns_number_gt                357
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX II (Bruker AXS, 2005)'
_computing_cell_refinement       'SAINTPLUS (Bruker AXS, 2005)'
_computing_data_reduction        'SAINTPLUS (Bruker AXS, 2005)'
_computing_structure_solution    'SHELXS (Sheldrick, 2004)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  'WINGX (Farrugia, 1998)'

_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.
;

_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^)+(0.0287P)^2^+0.0000P] 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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         457
_refine_ls_number_parameters     34
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0262
_refine_ls_R_factor_gt           0.0176
_refine_ls_wR_factor_ref         0.0435
_refine_ls_wR_factor_gt          0.0414
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_restrained_S_all      1.085
_refine_ls_shift/su_max          0.000
_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
Er1 Er 0.0000 0.0000 0.0000 0.01221(11) Uani 1 6 d S . .
O1 O -0.2029(3) 0.0011(4) 0.06170(13) 0.0284(6) Uani 1 1 d . . .
C1 C -0.3333 0.0038(5) 0.0833 0.0177(9) Uani 1 2 d S . .
C3 C -0.4982(5) 0.1685(5) 0.0833 0.0197(10) Uani 1 2 d SD . .
H3 H -0.5880 0.0914 0.0555 0.09(3) Uiso 1 1 d RD . .
C2 C -0.3369(9) 0.1676(9) 0.0590(3) 0.0172(14) Uani 0.50 1 d P . .

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
Er1 0.00897(12) 0.00897(12) 0.01869(16) 0.000 0.000 0.00448(6)
O1 0.0188(13) 0.0290(15) 0.0397(15) 0.0006(12) 0.0111(11) 0.0135(12)
C1 0.015(2) 0.0122(15) 0.027(2) 0.0009(9) 0.0019(18) 0.0077(11)
C3 0.0113(16) 0.0113(16) 0.035(3) -0.0001(11) 0.0001(11) 0.0042(19)
C2 0.010(3) 0.012(3) 0.030(3) 0.002(3) 0.004(3) 0.006(3)

_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
Er1 O1 2.203(3) 3 ?
Er1 O1 2.203(3) 21 ?
Er1 O1 2.203(3) 2 ?
Er1 O1 2.203(3) . ?
Er1 O1 2.203(3) 19 ?
Er1 O1 2.203(3) 20 ?
O1 C1 1.246(3) . ?
C1 O1 1.246(3) 18_444 ?
C1 C2 1.545(8) 18_444 ?
C1 C2 1.545(8) . ?
C3 C2 1.513(7) 16_454 ?
C3 C2 1.513(7) . ?
C3 C2 1.558(7) 3_455 ?
C3 C2 1.558(7) 18_444 ?
C3 H3 0.9400 . ?
C2 C2 1.012(13) 18_444 ?
C2 C3 1.558(7) 2_565 ?

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
O1 Er1 O1 180.00(17) 3 21 ?
O1 Er1 O1 89.70(11) 3 2 ?
O1 Er1 O1 90.30(11) 21 2 ?
O1 Er1 O1 89.70(11) 3 . ?
O1 Er1 O1 90.30(11) 21 . ?
O1 Er1 O1 89.70(11) 2 . ?
O1 Er1 O1 90.30(11) 3 19 ?
O1 Er1 O1 89.70(11) 21 19 ?
O1 Er1 O1 90.30(11) 2 19 ?
O1 Er1 O1 180.00(11) . 19 ?
O1 Er1 O1 90.30(11) 3 20 ?
O1 Er1 O1 89.70(11) 21 20 ?
O1 Er1 O1 180.00(17) 2 20 ?
O1 Er1 O1 90.30(11) . 20 ?
O1 Er1 O1 89.70(11) 19 20 ?
C1 O1 Er1 165.6(2) . . ?
O1 C1 O1 122.6(5) 18_444 . ?
O1 C1 C2 110.5(3) 18_444 18_444 ?
O1 C1 C2 123.9(3) . 18_444 ?
O1 C1 C2 123.9(3) 18_444 . ?
O1 C1 C2 110.5(3) . . ?
C2 C1 C2 38.2(5) 18_444 . ?
C2 C3 C2 124.3(6) 16_454 . ?
C2 C3 C2 38.4(5) 16_454 3_455 ?
C2 C3 C2 109.3(5) . 3_455 ?
C2 C3 C2 109.3(5) 16_454 18_444 ?
C2 C3 C2 38.4(5) . 18_444 ?
C2 C3 C2 122.1(6) 3_455 18_444 ?
C2 C3 H3 119.1 16_454 . ?
C2 C3 H3 104.2 . . ?
C2 C3 H3 95.5 3_455 . ?
C2 C3 H3 131.5 18_444 . ?
C2 C2 C3 73.2(7) 18_444 . ?
C2 C2 C1 70.9(2) 18_444 . ?
C3 C2 C1 110.8(4) . . ?
C2 C2 C3 68.4(6) 18_444 2_565 ?
C3 C2 C3 110.2(5) . 2_565 ?
C1 C2 C3 108.4(4) . 2_565 ?

_diffrn_measured_fraction_theta_max 0.964
_diffrn_reflns_theta_full        30.31
_diffrn_measured_fraction_theta_full 0.964
_refine_diff_density_max         0.857
_refine_diff_density_min         -0.546
_refine_diff_density_rms         0.131

#===END

data_DD3_49
_database_code_depnum_ccdc_archive 'CCDC 614838'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C9 H9 O6 Tb'
_chemical_formula_sum            'C9 H9 O6 Tb'
_chemical_formula_weight         372.08

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_H-M   R-3c

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'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'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'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'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-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'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-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'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'

_cell_length_a                   8.9133(12)
_cell_length_b                   8.9133(12)
_cell_length_c                   20.654(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     1421.1(5)
_cell_formula_units_Z            6
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    4264
_cell_measurement_theta_min      0.836
_cell_measurement_theta_max      0.928

_exptl_crystal_description       'rectangular plate'
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.609
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1056
_exptl_absorpt_coefficient_mu    7.475
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.706
_exptl_absorpt_correction_T_max  0.861
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      295(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 Apex CCD'
_diffrn_measurement_method       'omega and Phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7319
_diffrn_reflns_av_R_equivalents  0.0605
_diffrn_reflns_av_sigmaI/netI    0.0248
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         3.29
_diffrn_reflns_theta_max         30.27
_reflns_number_total             471
_reflns_number_gt                356
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX II (Bruker AXS, 2005)'
_computing_cell_refinement       'SAINTPLUS (Bruker AXS, 2005)'
_computing_data_reduction        'SAINTPLUS (Bruker AXS, 2005)'
_computing_structure_solution    'SHELXS (Sheldrick, 2004)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  'WINGX (Farrugia, 1998)'

_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.
;

_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^)+(0.0191P)^2^+0.0000P] 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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(3)
_refine_ls_number_reflns         471
_refine_ls_number_parameters     34
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0305
_refine_ls_R_factor_gt           0.0184
_refine_ls_wR_factor_ref         0.0440
_refine_ls_wR_factor_gt          0.0412
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_restrained_S_all      1.073
_refine_ls_shift/su_max          0.000
_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
Tb1 Tb 0.0000 0.0000 0.0000 0.01159(11) Uani 1 6 d S . .
O1 O -0.2023(3) 0.0053(4) 0.06265(13) 0.0269(6) Uani 1 1 d . . .
C1 C -0.3333 0.0069(5) 0.0833 0.0177(10) Uani 1 2 d S . .
C3 C -0.4969(6) 0.1698(6) 0.0833 0.0192(11) Uani 1 2 d SD . .
H3 H -0.5853 0.0962 0.0550 0.11(3) Uiso 1 1 d RD . .
C2 C -0.3377(10) 0.1682(9) 0.0587(3) 0.0155(14) Uani 0.50 1 d P . .

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
Tb1 0.00818(12) 0.00818(12) 0.01839(18) 0.000 0.000 0.00409(6)
O1 0.0189(13) 0.0262(14) 0.0386(15) -0.0002(12) 0.0103(12) 0.0136(12)
C1 0.012(2) 0.0122(16) 0.029(3) 0.0020(9) 0.0040(19) 0.0061(11)
C3 0.0122(17) 0.0122(17) 0.032(3) -0.0010(12) 0.0010(12) 0.006(2)
C2 0.010(3) 0.010(3) 0.026(3) 0.003(3) 0.002(3) 0.006(3)

_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
Tb1 O1 2.239(2) 21 ?
Tb1 O1 2.239(2) 3 ?
Tb1 O1 2.239(2) . ?
Tb1 O1 2.239(2) 19 ?
Tb1 O1 2.239(2) 20 ?
Tb1 O1 2.239(2) 2 ?
O1 C1 1.250(3) . ?
C1 O1 1.250(3) 18_444 ?
C1 C2 1.544(8) 18_444 ?
C1 C2 1.544(8) . ?
C3 C2 1.515(8) 16_454 ?
C3 C2 1.515(8) . ?
C3 C2 1.569(7) 3_455 ?
C3 C2 1.569(7) 18_444 ?
C3 H3 0.9363 . ?
C2 C2 1.021(13) 18_444 ?
C2 C3 1.569(7) 2_565 ?

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
O1 Tb1 O1 180.00(17) 21 3 ?
O1 Tb1 O1 90.05(10) 21 . ?
O1 Tb1 O1 89.95(10) 3 . ?
O1 Tb1 O1 89.95(10) 21 19 ?
O1 Tb1 O1 90.05(10) 3 19 ?
O1 Tb1 O1 180.00(14) . 19 ?
O1 Tb1 O1 89.95(10) 21 20 ?
O1 Tb1 O1 90.05(10) 3 20 ?
O1 Tb1 O1 90.05(10) . 20 ?
O1 Tb1 O1 89.95(10) 19 20 ?
O1 Tb1 O1 90.05(10) 21 2 ?
O1 Tb1 O1 89.95(10) 3 2 ?
O1 Tb1 O1 89.95(10) . 2 ?
O1 Tb1 O1 90.05(10) 19 2 ?
O1 Tb1 O1 180.00(14) 20 2 ?
C1 O1 Tb1 164.7(2) . . ?
O1 C1 O1 122.9(5) 18_444 . ?
O1 C1 C2 110.9(3) 18_444 18_444 ?
O1 C1 C2 123.1(4) . 18_444 ?
O1 C1 C2 123.1(4) 18_444 . ?
O1 C1 C2 110.9(3) . . ?
C2 C1 C2 38.6(5) 18_444 . ?
C2 C3 C2 124.7(6) 16_454 . ?
C2 C3 C2 38.6(5) 16_454 3_455 ?
C2 C3 C2 109.4(5) . 3_455 ?
C2 C3 C2 109.4(5) 16_454 18_444 ?
C2 C3 C2 38.6(5) . 18_444 ?
C2 C3 C2 122.0(6) 3_455 18_444 ?
C2 C3 H3 117.9 16_454 . ?
C2 C3 H3 104.3 . . ?
C2 C3 H3 94.1 3_455 . ?
C2 C3 H3 132.5 18_444 . ?
C2 C2 C3 73.6(7) 18_444 . ?
C2 C2 C1 70.7(3) 18_444 . ?
C3 C2 C1 111.0(5) . . ?
C2 C2 C3 67.8(7) 18_444 2_565 ?
C3 C2 C3 109.9(5) . 2_565 ?
C1 C2 C3 108.1(4) . 2_565 ?

_diffrn_measured_fraction_theta_max 0.977
_diffrn_reflns_theta_full        30.27
_diffrn_measured_fraction_theta_full 0.977
_refine_diff_density_max         1.374
_refine_diff_density_min         -0.455
_refine_diff_density_rms         0.130