# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Sion-2_H2O
_database_code_depnum_ccdc_archive 'CCDC 1503699'
_audit_update_record             
;
2017-05-01 deposited with the CCDC.
2017-05-16 downloaded from the CCDC.
;
_audit_creation_date             2017-04-25
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H6 O13 Tb, 3(H2 O)'
_chemical_formula_sum            'C12 H12 O16 Tb'
_chemical_formula_weight         571.14
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0040 0.0020 '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 0.0120 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.0760 4.2260 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.5715(9)
_cell_length_b                   10.1208(10)
_cell_length_c                   11.6980(13)
_cell_angle_alpha                113.409(10)
_cell_angle_beta                 101.145(9)
_cell_angle_gamma                105.464(8)
_cell_volume                     943.19(18)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1984
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      24.2520
_cell_measurement_theta_min      2.0440
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.885
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.37235
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            beige
_exptl_crystal_density_diffrn    2.011
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             554
_exptl_crystal_size_max          0.565
_exptl_crystal_size_mid          0.173
_exptl_crystal_size_min          0.071
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0645
_diffrn_reflns_av_unetI/netI     0.0890
_diffrn_reflns_Laue_measured_fraction_full 0.810
_diffrn_reflns_Laue_measured_fraction_max 0.793
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6544
_diffrn_reflns_point_group_measured_fraction_full 0.810
_diffrn_reflns_point_group_measured_fraction_max 0.793
_diffrn_reflns_theta_full        25.416
_diffrn_reflns_theta_max         25.661
_diffrn_reflns_theta_min         2.029
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.810
_diffrn_measured_fraction_theta_max 0.793
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -95.00 140.00   1.00   12.00    --    0.00   0.00   0.00  235
  2  ω    -15.00 130.00   1.00   12.00    --    0.00  40.00   0.00  145
  3  ω    -80.00  60.00   1.00   12.00    --    0.00 -40.00   0.00  140
  4  ω    -90.00  65.00   1.00   12.00    --    0.00  65.00   0.00  155
;
_diffrn_measurement_device_type  'Oxford diffraction, KM 6, Onyx'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0595590000
_diffrn_orient_matrix_UB_12      -0.0761549000
_diffrn_orient_matrix_UB_13      -0.0340861000
_diffrn_orient_matrix_UB_21      0.0534674000
_diffrn_orient_matrix_UB_22      -0.0325671000
_diffrn_orient_matrix_UB_23      -0.0222671000
_diffrn_orient_matrix_UB_31      0.0195788000
_diffrn_orient_matrix_UB_32      -0.0089948000
_diffrn_orient_matrix_UB_33      0.0579297000
_diffrn_radiation_monochromator  'Si 111'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7153
_diffrn_source                   
;
ESRF, Swiss-Norwegian Beamline BM01
;
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2142
_reflns_number_total             2780
_reflns_odcompleteness_completeness 79.48
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.66
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         1.820
_refine_diff_density_min         -4.956
_refine_diff_density_rms         0.302
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     264
_refine_ls_number_reflns         2780
_refine_ls_number_restraints     42
_refine_ls_R_factor_all          0.1008
_refine_ls_R_factor_gt           0.0770
_refine_ls_restrained_S_all      1.060
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1547P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1941
_refine_ls_wR_factor_ref         0.2209
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C5) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C12)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O4) \\sim Ueq, Uanis(C3) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C8) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3.a Aromatic/amide H refined with riding coordinates:
 C4(H4A), C7(H7), C12(H12)
3.b Tetrahedral OH refined with riding coordinates:
 O4(H4)
3.c Idealised tetrahedral OH refined as rotating group:
 O6(H6), O9(H9)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb 0.63804(8) 0.58918(8) 0.86884(8) 0.0314(4) Uani 1 1 d . . . . .
O1 O 0.4082(12) 0.5066(14) 0.8896(13) 0.043(3) Uani 1 1 d . . . . .
O2 O 0.2245(13) 0.3443(13) 0.9129(13) 0.047(3) Uani 1 1 d . . . . .
O3 O 0.4407(11) 0.3784(12) 0.6543(12) 0.041(3) Uani 1 1 d . . . . .
O4 O 0.0280(12) 0.0490(11) 0.1973(11) 0.032(3) Uani 1 1 d . U . . .
H4 H -0.0362 0.0002 0.1201 0.048 Uiso 1 1 calc R . . . .
O5 O -0.1894(12) 0.0267(12) 0.2429(11) 0.036(3) Uani 1 1 d . . . . .
O6 O -0.1920(12) 0.1016(14) 0.4763(13) 0.042(3) Uani 1 1 d . . . . .
H6 H -0.2300 0.0816 0.3976 0.062 Uiso 1 1 calc GR . . . .
O7 O 0.7689(11) 0.5130(12) 0.7160(11) 0.035(3) Uani 1 1 d . . . . .
O8 O 0.6070(12) 0.3893(12) 0.5096(13) 0.040(3) Uani 1 1 d . . . . .
O9 O 1.0591(12) 0.6148(13) 0.7687(12) 0.036(3) Uani 1 1 d . . . . .
H9 H 0.9852 0.5654 0.7833 0.055 Uiso 1 1 calc GR . . . .
O10 O 0.6567(14) 0.3532(12) 0.8548(13) 0.041(3) Uani 1 1 d . . . . .
O11 O 0.8821(12) 0.7976(13) 0.9431(12) 0.039(3) Uani 1 1 d . . . . .
O12 O 0.5604(12) 0.7025(13) 0.7399(13) 0.042(3) Uani 1 1 d . . . . .
O13 O 0.6069(14) 0.8218(12) 1.0103(14) 0.051(3) Uani 1 1 d . . . . .
C1 C 0.2838(18) 0.3896(18) 0.8402(18) 0.035(4) Uani 1 1 d . U . . .
C2 C 0.2049(18) 0.3084(17) 0.6992(16) 0.033(4) Uani 1 1 d . . . . .
C3 C 0.2850(17) 0.3046(16) 0.6062(16) 0.026(3) Uani 1 1 d . U . . .
C4 C 0.2019(18) 0.2259(17) 0.4704(17) 0.032(4) Uani 1 1 d . . . . .
H4A H 0.2568 0.2221 0.4104 0.038 Uiso 1 1 calc R . . . .
C5 C 0.0437(17) 0.1538(15) 0.4206(16) 0.029(4) Uani 1 1 d . U . . .
C6 C -0.0341(17) 0.1621(17) 0.5146(17) 0.031(4) Uani 1 1 d . . . . .
C7 C 0.0448(17) 0.2327(17) 0.6446(17) 0.032(4) Uani 1 1 d . . . . .
H7 H -0.0115 0.2311 0.7029 0.038 Uiso 1 1 calc R . . . .
C8 C -0.0432(17) 0.0719(17) 0.2808(17) 0.029(3) Uani 1 1 d . U . . .
C9 C 0.7395(17) 0.4580(16) 0.5901(15) 0.027(4) Uani 1 1 d . . . . .
C10 C 0.8758(16) 0.4771(15) 0.5441(16) 0.027(4) Uani 1 1 d . . . . .
C11 C 1.0272(17) 0.5560(16) 0.6341(16) 0.028(3) Uani 1 1 d . U . . .
C12 C 0.8501(16) 0.4220(15) 0.4103(14) 0.024(3) Uani 1 1 d . U . . .
H12 H 0.7479 0.3690 0.3490 0.029 Uiso 1 1 calc R . . . .
O3W O 0.6818(16) 1.188(2) 1.0150(18) 0.119(9) Uani 1 1 d . . . . .
O1W O 0.7078(13) 0.9960(13) 0.7942(12) 0.041(3) Uani 1 1 d . . . . .
O2W O -0.3804(12) 0.1020(13) 0.6207(12) 0.040(3) Uani 1 1 d . . . . .


_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 2.232(11) . ?
Tb1 O2 2.359(14) 2_667 ?
Tb1 O3 2.486(11) . ?
Tb1 O7 2.375(10) . ?
Tb1 O10 2.385(10) . ?
Tb1 O11 2.407(10) . ?
Tb1 O12 2.353(13) . ?
Tb1 O13 2.417(10) . ?
O1 C1 1.262(19) . ?
O2 Tb1 2.359(13) 2_667 ?
O2 C1 1.27(2) . ?
O3 C3 1.358(17) . ?
O4 H4 0.8400 . ?
O4 C8 1.278(18) . ?
O5 C8 1.274(18) . ?
O6 H6 0.8400 . ?
O6 C6 1.373(18) . ?
O7 C9 1.290(18) . ?
O8 C9 1.236(18) . ?
O9 H9 0.8400 . ?
O9 C11 1.378(19) . ?
C1 C2 1.44(2) . ?
C2 C3 1.44(2) . ?
C2 C7 1.40(2) . ?
C3 C4 1.40(2) . ?
C4 H4A 0.9500 . ?
C4 C5 1.38(2) . ?
C5 C6 1.43(2) . ?
C5 C8 1.44(2) . ?
C6 C7 1.34(2) . ?
C7 H7 0.9500 . ?
C9 C10 1.50(2) . ?
C10 C11 1.40(2) . ?
C10 C12 1.38(2) . ?
C11 C12 1.37(2) 2_766 ?
C12 C11 1.37(2) 2_766 ?
C12 H12 0.9500 . ?

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 O2 93.7(4) . 2_667 ?
O1 Tb1 O3 68.3(4) . . ?
O1 Tb1 O7 139.9(4) . . ?
O1 Tb1 O10 86.8(4) . . ?
O1 Tb1 O11 148.6(4) . . ?
O1 Tb1 O12 94.4(4) . . ?
O1 Tb1 O13 74.5(4) . . ?
O2 Tb1 O3 145.5(4) 2_667 . ?
O2 Tb1 O7 114.1(4) 2_667 . ?
O2 Tb1 O10 75.2(4) 2_667 . ?
O2 Tb1 O11 71.5(4) 2_667 . ?
O2 Tb1 O13 74.3(4) 2_667 . ?
O7 Tb1 O3 72.7(4) . . ?
O7 Tb1 O10 74.2(4) . . ?
O7 Tb1 O11 70.8(4) . . ?
O7 Tb1 O13 138.8(4) . . ?
O10 Tb1 O3 74.6(4) . . ?
O10 Tb1 O11 114.4(4) . . ?
O10 Tb1 O13 142.8(5) . . ?
O11 Tb1 O3 137.5(4) . . ?
O11 Tb1 O13 74.9(4) . . ?
O12 Tb1 O2 141.3(4) . 2_667 ?
O12 Tb1 O3 71.6(4) . . ?
O12 Tb1 O7 81.7(4) . . ?
O12 Tb1 O10 142.9(4) . . ?
O12 Tb1 O11 82.4(4) . . ?
O12 Tb1 O13 71.6(4) . . ?
O13 Tb1 O3 124.3(4) . . ?
C1 O1 Tb1 142.7(11) . . ?
C1 O2 Tb1 124.1(11) . 2_667 ?
C3 O3 Tb1 136.5(10) . . ?
C8 O4 H4 109.5 . . ?
C6 O6 H6 109.5 . . ?
C9 O7 Tb1 137.3(9) . . ?
C11 O9 H9 109.5 . . ?
O1 C1 O2 121.1(16) . . ?
O1 C1 C2 119.6(15) . . ?
O2 C1 C2 119.2(14) . . ?
C1 C2 C3 122.4(14) . . ?
C7 C2 C1 121.8(15) . . ?
C7 C2 C3 115.8(15) . . ?
O3 C3 C2 118.2(14) . . ?
O3 C3 C4 121.9(14) . . ?
C4 C3 C2 119.8(14) . . ?
C3 C4 H4A 118.8 . . ?
C5 C4 C3 122.5(15) . . ?
C5 C4 H4A 118.8 . . ?
C4 C5 C6 116.9(15) . . ?
C4 C5 C8 123.0(15) . . ?
C6 C5 C8 120.1(13) . . ?
O6 C6 C5 121.7(15) . . ?
C7 C6 O6 117.2(15) . . ?
C7 C6 C5 121.1(14) . . ?
C2 C7 H7 118.1 . . ?
C6 C7 C2 123.9(16) . . ?
C6 C7 H7 118.1 . . ?
O4 C8 C5 119.5(13) . . ?
O5 C8 O4 121.2(15) . . ?
O5 C8 C5 119.3(14) . . ?
O7 C9 C10 116.5(13) . . ?
O8 C9 O7 122.8(14) . . ?
O8 C9 C10 120.7(14) . . ?
C11 C10 C9 121.5(15) . . ?
C12 C10 C9 118.6(13) . . ?
C12 C10 C11 119.8(14) . . ?
O9 C11 C10 122.2(14) . . ?
C12 C11 O9 117.5(13) 2_766 . ?
C12 C11 C10 120.3(15) 2_766 . ?
C10 C12 H12 120.1 . . ?
C11 C12 C10 119.8(14) 2_766 . ?
C11 C12 H12 120.1 2_766 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Tb1 O1 C1 O2 132.4(16) . . . . ?
Tb1 O1 C1 C2 -50(3) . . . . ?
Tb1 O2 C1 O1 -20(2) 2_667 . . . ?
Tb1 O2 C1 C2 162.0(11) 2_667 . . . ?
Tb1 O3 C3 C2 -22(2) . . . . ?
Tb1 O3 C3 C4 158.6(11) . . . . ?
Tb1 O7 C9 O8 -21(2) . . . . ?
Tb1 O7 C9 C10 160.4(9) . . . . ?
O1 C1 C2 C3 28(2) . . . . ?
O1 C1 C2 C7 -149.4(16) . . . . ?
O2 C1 C2 C3 -153.4(15) . . . . ?
O2 C1 C2 C7 29(2) . . . . ?
O3 C3 C4 C5 -178.4(13) . . . . ?
O6 C6 C7 C2 -175.7(14) . . . . ?
O7 C9 C10 C11 -2.4(19) . . . . ?
O7 C9 C10 C12 -179.1(12) . . . . ?
O8 C9 C10 C11 179.4(13) . . . . ?
O8 C9 C10 C12 3(2) . . . . ?
C1 C2 C3 O3 1(2) . . . . ?
C1 C2 C3 C4 -179.0(14) . . . . ?
C1 C2 C7 C6 176.7(15) . . . . ?
C2 C3 C4 C5 2(2) . . . . ?
C3 C2 C7 C6 -1(2) . . . . ?
C3 C4 C5 C6 0(2) . . . . ?
C3 C4 C5 C8 -179.8(13) . . . . ?
C4 C5 C6 O6 176.5(13) . . . . ?
C4 C5 C6 C7 -2(2) . . . . ?
C4 C5 C8 O4 8(2) . . . . ?
C4 C5 C8 O5 -170.4(13) . . . . ?
C5 C6 C7 C2 3(2) . . . . ?
C6 C5 C8 O4 -171.6(13) . . . . ?
C6 C5 C8 O5 10(2) . . . . ?
C7 C2 C3 O3 179.1(13) . . . . ?
C7 C2 C3 C4 -1(2) . . . . ?
C8 C5 C6 O6 -4(2) . . . . ?
C8 C5 C6 C7 177.5(14) . . . . ?
C9 C10 C11 O9 3(2) . . . . ?
C9 C10 C11 C12 -177.0(13) . . . 2_766 ?
C9 C10 C12 C11 177.1(13) . . . 2_766 ?
C11 C10 C12 C11 0(2) . . . 2_766 ?
C12 C10 C11 O9 179.3(13) . . . . ?
C12 C10 C11 C12 0(2) . . . 2_766 ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.831
_oxdiff_exptl_absorpt_empirical_full_min 0.609
# start Validation Reply Form
_vrf_PLAT029_Sion-2_H2O          
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.810 Note  
RESPONSE: The data were collected upon the spindle rotation. Therefore, 
		  a limited portion of the reciprocal space could be probed.
;
_vrf_PLAT972_Sion-2_H2O          
;
PROBLEM: Check Calcd Residual Density  0.80A From     Tb1      -4.52 eA-3  
RESPONSE: Electron density minima about Tb-atoms are artifacts caused by finite 
		  Fourier sum truncation.
;
_vrf_PLAT043_Sion-2_H2O          
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..       6.04 Check 
RESPONSE: Reported molecular weight accounts for hydrogen
		  atoms attached to water, of which the location 
		  was not resolved.
;
_vrf_PLAT306_Sion-2_H2O          
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        O1W Check 
RESPONSE: Hydrogen atoms attached the free solvent water molecules could not be 
	      localised in chemically reasonable positions; difference-Fourier maps 
		  do not provide any hint about the location of H-atoms.
;
_vrf_PLAT342_Sion-2_H2O          
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.02083 Ang.  
RESPONSE: Low bond precision is due to the limited completeness of data and 
		  partial disorder of free solvent molecules. 
;
_vrf_PLAT430_Sion-2_H2O          
;
PROBLEM: Short Inter D...A Contact  O1W    ..  O3W     ..       2.65 Ang.  
RESPONSE: This short contact is due to specific interactions between free water 
		  molecules.
;
_vrf_PLAT911_Sion-2_H2O          
;
PROBLEM: Missing # FCF Refl Between THmin & STh/L=  0.600        649 Report
RESPONSE: Deleted overflow reflections. 
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_SION-1
_database_code_depnum_ccdc_archive 'CCDC 1503702'
_audit_update_record             
;
2017-05-01 deposited with the CCDC.
2017-05-16 downloaded from the CCDC.
;
_audit_creation_date             2017-04-25
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C11 H10 N O7 Tb'
_chemical_formula_sum            'C11 H10 N O7 Tb'
_chemical_formula_weight         427.12
_chemical_melting_point          ?
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'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   13.388(3)
_cell_length_b                   6.6366(12)
_cell_length_c                   15.567(2)
_cell_angle_alpha                90
_cell_angle_beta                 98.599(14)
_cell_angle_gamma                90
_cell_volume                     1367.6(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5339
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.375
_cell_measurement_theta_min      2.173
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    5.200
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5862
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1157 before and 0.0610 after correction. The Ratio of minimum to maximum transmission is 0.7857. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.074
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             816
_exptl_crystal_preparation       ?
_exptl_crystal_recrystallization_method ?
_exptl_crystal_size_max          0.062
_exptl_crystal_size_mid          0.059
_exptl_crystal_size_min          0.024
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0666
_diffrn_reflns_av_unetI/netI     0.0711
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            14568
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.539
_diffrn_reflns_theta_min         2.647
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_special_details          ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3034
_reflns_number_total             4070
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.910
_refine_diff_density_min         -1.001
_refine_diff_density_rms         0.234
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     225
_refine_ls_number_reflns         4070
_refine_ls_number_restraints     40
_refine_ls_R_factor_all          0.0681
_refine_ls_R_factor_gt           0.0369
_refine_ls_restrained_S_all      1.079
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0047P)²+2.2406P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0496
_refine_ls_wR_factor_ref         0.0552
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 N1-C2B \\sim N1-C3B
 with sigma of 0.02
 N1-C2A \\sim N1-C3A
 with sigma of 0.02
3. Restrained planarity
 N1, C3A, C1A, C2A
 with sigma of 0.1
 N1, C1B, C2B, C3B
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C3B) \\sim Ueq, Uanis(C2A) \\sim Ueq, Uanis(C3A) \\sim Ueq, Uanis(C2B)
\\sim Ueq: with sigma of 0.0075 and sigma for terminal atoms of 0.015
Uanis(O1B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O1A) \\sim Ueq: with sigma of 0.003 and sigma for terminal atoms of 0.006
5. Others
 Sof(C1A)=Sof(H1AA)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(H2AC)=Sof(C3A)=Sof(H3AA)=
 Sof(H3AB)=Sof(H3AC)=1-FVAR(1)
 Sof(C1B)=Sof(H1BA)=Sof(C2B)=Sof(H2BA)=Sof(H2BB)=Sof(H2BC)=Sof(C3B)=Sof(H3BA)=
 Sof(H3BB)=Sof(H3BC)=FVAR(1)
 Sof(O1B)=Sof(H1B)=Sof(H13)=1-FVAR(2)
 Sof(O1A)=Sof(H1A)=Sof(H14)=FVAR(2)
6.a Aromatic/amide H refined with riding coordinates:
 C1A(H1AA), C1B(H1BA), C4(H4), C13(H13), C14(H14)
6.b Idealised Me refined as rotating group:
 C2A(H2AA,H2AB,H2AC), C2B(H2BA,H2BB,H2BC), C3A(H3AA,H3AB,H3AC), C3B(H3BA,H3BB,
 H3BC)
6.c Idealised tetrahedral OH refined as rotating group:
 O1A(H1A), O1B(H1B)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb 0.33134(2) 0.57866(3) 0.28752(2) 0.00976(5) Uani 1 1 d . . . . .
O1A O -0.0445(4) 0.1572(7) 0.4010(3) 0.0479(16) Uani 0.830(7) 1 d . U P A 1
H1A H 0.0008 0.1283 0.3731 0.072 Uiso 0.830(7) 1 calc GR . P A 1
O1B O -0.1333(19) 0.203(3) 0.5311(17) 0.052(8) Uani 0.170(7) 1 d . U P A 2
H1B H -0.1581 0.2231 0.5754 0.078 Uiso 0.170(7) 1 calc GR . P A 2
O2 O 0.4346(2) 0.6658(4) 0.4018(2) 0.0237(8) Uani 1 1 d . . . . .
O3 O 0.4814(3) 0.4197(5) 0.2546(2) 0.0352(8) Uani 1 1 d . . . . .
O7 O 0.7130(2) 1.0908(4) 0.67639(17) 0.0139(6) Uani 1 1 d . . . . .
O8 O 0.6800(2) 0.7698(4) 0.67351(18) 0.0165(7) Uani 1 1 d . . . . .
O9 O 0.1919(2) 0.5440(4) 0.3591(2) 0.0251(8) Uani 1 1 d . . . . .
O11 O 0.1029(3) 0.2666(5) 0.3188(2) 0.0310(8) Uani 1 1 d . . . . .
N1 N 0.6245(4) 0.2571(9) 0.3116(4) 0.0627(16) Uani 1 1 d D . . . .
C1A C 0.5361(12) 0.279(2) 0.2633(11) 0.044(4) Uani 0.411(11) 1 d . . P B 2
H1AA H 0.5129 0.1667 0.2308 0.053 Uiso 0.411(11) 1 calc R . P B 2
C1B C 0.5554(8) 0.3786(16) 0.3138(8) 0.042(3) Uani 0.589(11) 1 d . . P B 1
H1BA H 0.5574 0.4500 0.3655 0.050 Uiso 0.589(11) 1 calc R . P B 1
C2A C 0.6791(17) 0.070(3) 0.3289(16) 0.097(8) Uani 0.411(11) 1 d D U P B 2
H2AA H 0.6701 0.0213 0.3853 0.145 Uiso 0.411(11) 1 calc GR . P B 2
H2AB H 0.7496 0.0930 0.3275 0.145 Uiso 0.411(11) 1 calc GR . P B 2
H2AC H 0.6538 -0.0274 0.2856 0.145 Uiso 0.411(11) 1 calc GR . P B 2
C2B C 0.6243(13) 0.145(2) 0.2281(10) 0.136(8) Uani 0.589(11) 1 d D U P B 1
H2BA H 0.5918 0.0168 0.2315 0.205 Uiso 0.589(11) 1 calc GR . P B 1
H2BB H 0.6926 0.1242 0.2181 0.205 Uiso 0.589(11) 1 calc GR . P B 1
H2BC H 0.5884 0.2217 0.1810 0.205 Uiso 0.589(11) 1 calc GR . P B 1
C3 C 0.4640(3) 0.8286(6) 0.4484(3) 0.0160(9) Uani 1 1 d . . . . .
C3A C 0.6552(15) 0.431(3) 0.3730(12) 0.091(7) Uani 0.411(11) 1 d D U P B 2
H3AA H 0.6269 0.5540 0.3475 0.136 Uiso 0.411(11) 1 calc GR . P B 2
H3AB H 0.7275 0.4417 0.3833 0.136 Uiso 0.411(11) 1 calc GR . P B 2
H3AC H 0.6306 0.4078 0.4270 0.136 Uiso 0.411(11) 1 calc GR . P B 2
C3B C 0.7057(10) 0.196(2) 0.3789(10) 0.091(5) Uani 0.589(11) 1 d D U P B 1
H3BA H 0.7112 0.2909 0.4260 0.136 Uiso 0.589(11) 1 calc GR . P B 1
H3BB H 0.7681 0.1929 0.3556 0.136 Uiso 0.589(11) 1 calc GR . P B 1
H3BC H 0.6916 0.0647 0.3998 0.136 Uiso 0.589(11) 1 calc GR . P B 1
C4 C 0.5407(3) 0.8102(5) 0.5198(3) 0.0163(9) Uani 1 1 d . . . . .
H4 H 0.5682 0.6837 0.5340 0.020 Uiso 1 1 calc R . . . .
C5 C 0.5772(3) 0.9765(6) 0.5706(3) 0.0143(9) Uani 1 1 d . . . . .
C6 C 0.6587(3) 0.9429(6) 0.6425(2) 0.0110(8) Uani 1 1 d . . . . .
C10 C 0.1231(3) 0.4214(7) 0.3667(3) 0.0215(9) Uani 1 1 d . . . . .
C12 C 0.0592(4) 0.4583(6) 0.4355(3) 0.0227(11) Uani 1 1 d . . . . .
C13 C -0.0176(4) 0.3255(7) 0.4504(3) 0.0324(13) Uani 1 1 d . . . . .
H13 H -0.0296 0.2092 0.4171 0.039 Uiso 0.170(7) 1 calc R . P A 2
C14 C -0.0757(4) 0.3673(7) 0.5147(3) 0.0306(12) Uani 1 1 d . . . . .
H14 H -0.1263 0.2781 0.5246 0.037 Uiso 0.830(7) 1 calc R . P A 1


_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 O2 2.162(3) . ?
Tb1 O3 2.391(3) . ?
Tb1 O7 2.362(3) 3_676 ?
Tb1 O7 2.439(3) 4_575 ?
Tb1 O8 2.682(3) 4_575 ?
Tb1 O8 2.401(3) 3_666 ?
Tb1 O9 2.324(3) . ?
Tb1 O11 2.346(3) 2 ?
Tb1 C6 2.983(4) 4_575 ?
O1A H1A 0.8200 . ?
O1A C13 1.374(5) . ?
O1B H1B 0.8200 . ?
O1B C14 1.38(2) . ?
O2 C3 1.328(4) . ?
O3 C1A 1.180(14) . ?
O3 C1B 1.278(11) . ?
O7 Tb1 2.362(3) 3_676 ?
O7 Tb1 2.439(3) 4_676 ?
O7 C6 1.287(4) . ?
O8 Tb1 2.682(3) 4_676 ?
O8 Tb1 2.401(3) 3_666 ?
O8 C6 1.262(4) . ?
O9 C10 1.248(5) . ?
O11 Tb1 2.346(3) 2_545 ?
O11 C10 1.275(5) . ?
N1 C1A 1.312(17) . ?
N1 C1B 1.231(11) . ?
N1 C2A 1.444(16) . ?
N1 C2B 1.498(13) . ?
N1 C3A 1.516(16) . ?
N1 C3B 1.451(12) . ?
C1A H1AA 0.9300 . ?
C1B H1BA 0.9300 . ?
C2A H2AA 0.9600 . ?
C2A H2AB 0.9600 . ?
C2A H2AC 0.9600 . ?
C2B H2BA 0.9600 . ?
C2B H2BB 0.9600 . ?
C2B H2BC 0.9600 . ?
C3 C4 1.401(6) . ?
C3 C5 1.420(5) 3_676 ?
C3A H3AA 0.9600 . ?
C3A H3AB 0.9600 . ?
C3A H3AC 0.9600 . ?
C3B H3BA 0.9600 . ?
C3B H3BB 0.9600 . ?
C3B H3BC 0.9600 . ?
C4 H4 0.9300 . ?
C4 C5 1.401(5) . ?
C5 C3 1.420(5) 3_676 ?
C5 C6 1.460(5) . ?
C6 Tb1 2.983(4) 4_676 ?
C10 C12 1.487(6) . ?
C12 C13 1.400(6) . ?
C12 C14 1.392(6) 3_566 ?
C13 H13 0.9300 . ?
C13 C14 1.384(6) . ?
C14 C12 1.392(6) 3_566 ?
C14 H14 0.9300 . ?

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 Tb1 O3 80.79(12) . . ?
O2 Tb1 O7 73.04(9) . 3_676 ?
O2 Tb1 O7 167.05(10) . 4_575 ?
O2 Tb1 O8 96.11(9) . 3_666 ?
O2 Tb1 O8 140.45(9) . 4_575 ?
O2 Tb1 O9 95.33(12) . . ?
O2 Tb1 O11 100.20(13) . 2 ?
O2 Tb1 C6 164.40(10) . 4_575 ?
O3 Tb1 O7 97.01(11) . 4_575 ?
O3 Tb1 O8 73.49(11) . 3_666 ?
O3 Tb1 O8 126.85(11) . 4_575 ?
O3 Tb1 C6 113.43(11) . 4_575 ?
O7 Tb1 O3 135.22(11) 3_676 . ?
O7 Tb1 O7 115.93(6) 3_676 4_575 ?
O7 Tb1 O8 50.00(8) 4_575 4_575 ?
O7 Tb1 O8 143.76(10) 3_676 3_666 ?
O7 Tb1 O8 67.49(8) 3_676 4_575 ?
O7 Tb1 C6 24.97(9) 4_575 4_575 ?
O7 Tb1 C6 91.75(9) 3_676 4_575 ?
O8 Tb1 O7 71.11(9) 3_666 4_575 ?
O8 Tb1 O8 117.28(7) 3_666 4_575 ?
O8 Tb1 C6 94.24(9) 3_666 4_575 ?
O8 Tb1 C6 25.02(9) 4_575 4_575 ?
O9 Tb1 O3 145.05(11) . . ?
O9 Tb1 O7 79.11(10) . 4_575 ?
O9 Tb1 O7 74.30(10) . 3_676 ?
O9 Tb1 O8 76.85(11) . 4_575 ?
O9 Tb1 O8 72.43(10) . 3_666 ?
O9 Tb1 O11 143.48(11) . 2 ?
O9 Tb1 C6 76.74(11) . 4_575 ?
O11 Tb1 O3 70.60(11) 2 . ?
O11 Tb1 O7 78.96(10) 2 3_676 ?
O11 Tb1 O7 90.98(11) 2 4_575 ?
O11 Tb1 O8 70.12(11) 2 4_575 ?
O11 Tb1 O8 137.27(11) 2 3_666 ?
O11 Tb1 C6 79.73(12) 2 4_575 ?
C13 O1A H1A 109.5 . . ?
C14 O1B H1B 109.5 . . ?
C3 O2 Tb1 140.2(3) . . ?
C1A O3 Tb1 148.3(8) . . ?
C1B O3 Tb1 121.7(6) . . ?
Tb1 O7 Tb1 114.79(10) 3_676 4_676 ?
C6 O7 Tb1 131.2(2) . 3_676 ?
C6 O7 Tb1 101.9(2) . 4_676 ?
Tb1 O8 Tb1 105.30(9) 3_666 4_676 ?
C6 O8 Tb1 90.9(2) . 4_676 ?
C6 O8 Tb1 162.6(3) . 3_666 ?
C10 O9 Tb1 140.1(3) . . ?
C10 O11 Tb1 140.5(3) . 2_545 ?
C1A N1 C2A 126.3(14) . . ?
C1A N1 C3A 114.3(11) . . ?
C1B N1 C2B 116.5(10) . . ?
C1B N1 C3B 130.3(11) . . ?
C2A N1 C3A 117.0(13) . . ?
C3B N1 C2B 113.1(10) . . ?
O3 C1A N1 130.2(16) . . ?
O3 C1A H1AA 114.9 . . ?
N1 C1A H1AA 114.9 . . ?
O3 C1B H1BA 115.7 . . ?
N1 C1B O3 128.6(12) . . ?
N1 C1B H1BA 115.7 . . ?
N1 C2A H2AA 109.5 . . ?
N1 C2A H2AB 109.5 . . ?
N1 C2A H2AC 109.5 . . ?
H2AA C2A H2AB 109.5 . . ?
H2AA C2A H2AC 109.5 . . ?
H2AB C2A H2AC 109.5 . . ?
N1 C2B H2BA 109.5 . . ?
N1 C2B H2BB 109.5 . . ?
N1 C2B H2BC 109.5 . . ?
H2BA C2B H2BB 109.5 . . ?
H2BA C2B H2BC 109.5 . . ?
H2BB C2B H2BC 109.5 . . ?
O2 C3 C4 119.0(4) . . ?
O2 C3 C5 123.6(4) . 3_676 ?
C4 C3 C5 117.4(3) . 3_676 ?
N1 C3A H3AA 109.5 . . ?
N1 C3A H3AB 109.5 . . ?
N1 C3A H3AC 109.5 . . ?
H3AA C3A H3AB 109.5 . . ?
H3AA C3A H3AC 109.5 . . ?
H3AB C3A H3AC 109.5 . . ?
N1 C3B H3BA 109.5 . . ?
N1 C3B H3BB 109.5 . . ?
N1 C3B H3BC 109.5 . . ?
H3BA C3B H3BB 109.5 . . ?
H3BA C3B H3BC 109.5 . . ?
H3BB C3B H3BC 109.5 . . ?
C3 C4 H4 119.0 . . ?
C3 C4 C5 122.1(4) . . ?
C5 C4 H4 119.0 . . ?
C3 C5 C6 121.4(3) 3_676 . ?
C4 C5 C3 120.6(4) . 3_676 ?
C4 C5 C6 118.0(3) . . ?
O7 C6 Tb1 53.15(19) . 4_676 ?
O7 C6 C5 120.6(3) . . ?
O8 C6 Tb1 64.0(2) . 4_676 ?
O8 C6 O7 117.2(3) . . ?
O8 C6 C5 122.2(3) . . ?
C5 C6 Tb1 173.7(3) . 4_676 ?
O9 C10 O11 124.4(4) . . ?
O9 C10 C12 118.3(4) . . ?
O11 C10 C12 117.4(4) . . ?
C13 C12 C10 122.1(4) . . ?
C14 C12 C10 118.5(4) 3_566 . ?
C14 C12 C13 119.3(4) 3_566 . ?
O1A C13 C12 123.8(4) . . ?
O1A C13 C14 116.0(4) . . ?
C12 C13 H13 120.0 . . ?
C14 C13 C12 120.0(4) . . ?
C14 C13 H13 120.0 . . ?
O1B C14 C12 126.8(10) . 3_566 ?
O1B C14 C13 111.4(9) . . ?
C12 C14 H14 119.7 3_566 . ?
C13 C14 C12 120.6(4) . 3_566 ?
C13 C14 H14 119.7 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Tb1 O2 C3 C4 -177.5(3) . . . . ?
Tb1 O2 C3 C5 1.7(8) . . . 3_676 ?
Tb1 O3 C1A N1 -103.3(19) . . . . ?
Tb1 O3 C1B N1 160.2(7) . . . . ?
Tb1 O7 C6 Tb1 -139.0(3) 3_676 . . 4_676 ?
Tb1 O7 C6 O8 0.1(4) 4_676 . . . ?
Tb1 O7 C6 O8 -138.9(3) 3_676 . . . ?
Tb1 O7 C6 C5 42.0(5) 3_676 . . . ?
Tb1 O7 C6 C5 -179.1(3) 4_676 . . . ?
Tb1 O8 C6 Tb1 159.1(9) 3_666 . . 4_676 ?
Tb1 O8 C6 O7 -0.1(3) 4_676 . . . ?
Tb1 O8 C6 O7 159.0(7) 3_666 . . . ?
Tb1 O8 C6 C5 179.1(3) 4_676 . . . ?
Tb1 O8 C6 C5 -21.9(11) 3_666 . . . ?
Tb1 O9 C10 O11 -11.4(8) . . . . ?
Tb1 O9 C10 C12 169.4(3) . . . . ?
Tb1 O11 C10 O9 9.8(8) 2_545 . . . ?
Tb1 O11 C10 C12 -171.0(3) 2_545 . . . ?
O1A C13 C14 C12 -175.6(5) . . . 3_566 ?
O2 C3 C4 C5 178.4(4) . . . . ?
O9 C10 C12 C13 -178.1(5) . . . . ?
O9 C10 C12 C14 3.0(7) . . . 3_566 ?
O11 C10 C12 C13 2.7(7) . . . . ?
O11 C10 C12 C14 -176.2(5) . . . 3_566 ?
C2A N1 C1A O3 169.4(16) . . . . ?
C2B N1 C1B O3 1.7(15) . . . . ?
C3 C4 C5 C3 0.9(7) . . . 3_676 ?
C3 C4 C5 C6 -178.7(4) . . . . ?
C3 C5 C6 O7 -18.2(6) 3_676 . . . ?
C3 C5 C6 O8 162.7(4) 3_676 . . . ?
C3A N1 C1A O3 8(2) . . . . ?
C3B N1 C1B O3 -175.2(11) . . . . ?
C4 C5 C6 O7 161.4(4) . . . . ?
C4 C5 C6 O8 -17.7(6) . . . . ?
C5 C3 C4 C5 -0.9(7) 3_676 . . . ?
C10 C12 C13 O1A -3.6(9) . . . . ?
C10 C12 C13 C14 -179.4(5) . . . . ?
C12 C13 C14 O1B -168.2(14) . . . . ?
C12 C13 C14 C12 0.5(9) . . . 3_566 ?
C14 C12 C13 O1A 175.3(6) 3_566 . . . ?
C14 C12 C13 C14 -0.5(9) 3_566 . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
# start Validation Reply Form
_vrf_PLAT220_SION-1              
;
PROBLEM: Non-Solvent Resd 1   C   Ueq(max)/Ueq(min) Range       10.0 Ratio 
RESPONSE: Larger than usual U(eq)'s for carbon atoms are predominatly due to 
		  terminal disordered C2A, C2B, C3A, and C3B atoms, which belong to 
		  the DMF ligand with a considerable vibrational degree of freedom.
;
_vrf_PLAT430_SION-1              
;
PROBLEM: Short Inter D...A Contact  O7     ..  O8      ..       2.82 Ang.  
RESPONSE: O7 and O8 are both located in the coordination sphere of Tb1 as 
		  parts of a Tb(III)-O 1D chain. There is not any hydrogen bonding 
		  between them.
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Sion-1_H2O
_database_code_depnum_ccdc_archive 'CCDC 1503700'
_audit_update_record             
;
2017-05-01 deposited with the CCDC.
2017-05-16 downloaded from the CCDC.
;
_audit_creation_date             2016-09-06
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.08.25 svn.r3337 for OlexSys, GUI svn.r5221)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C8 H3 O7 Tb, 4(H2 O)'
_chemical_formula_sum            'C8 H11 O11 Tb'
_chemical_formula_weight         442.08
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0040 0.0020 'Calculated using XDISP in WinGX (Farrugia, 1999)'
H H 0.0000 0.0000 'Calculated using XDISP in WinGX (Farrugia, 1999)'
O O 0.0130 0.0070 'Calculated using XDISP in WinGX (Farrugia, 1999)'
Tb Tb -0.1250 4.8270 'Calculated using XDISP in WinGX (Farrugia, 1999)'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   12.3720(10)
_cell_length_b                   6.5373(4)
_cell_length_c                   16.4809(12)
_cell_angle_alpha                90
_cell_angle_beta                 99.121(5)
_cell_angle_gamma                90
_cell_volume                     1316.11(17)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6994
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.577
_cell_measurement_theta_min      2.729
_shelx_estimated_absorpt_T_max   0.935
_shelx_estimated_absorpt_T_min   0.877
_exptl_absorpt_coefficient_mu    6.762
_exptl_absorpt_correction_T_max  0.7466
_exptl_absorpt_correction_T_min  0.5543
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1088 before and 0.0836 after correction.
The Ratio of minimum to maximum transmission is 0.7424.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'reddish orange'
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.231
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.015
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0874
_diffrn_reflns_av_unetI/netI     0.0605
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            15766
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        27.706
_diffrn_reflns_theta_max         28.961
_diffrn_reflns_theta_min         2.440
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker D8 with PHOTON 100 detector'
_diffrn_measurement_method       'φ and ω shutterless scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7749
_diffrn_source                   
;
Advanced Light Source, station 11.3.1
;
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2184
_reflns_number_total             2673
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_data_collection       'Bruker APEX2 Bruker-AXS, Madison WI'
_computing_cell_refinement       'SAINT V8.34A Bruker-AXS, Madison WI'
_computing_data_reduction        'SAINT V8.34A Bruker-AXS, Madison WI'
_computing_structure_solution    'SHELXT 2014/4 Bruker-AXS, Madison WI'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    
;
Bruker SHELXTL Bruker-AXS, Madison WI
and local programs
;
_computing_publication_material  'Bruker SHELXTL Bruker-AXS, Madison WI'
_refine_diff_density_max         8.267
_refine_diff_density_min         -10.674
_refine_diff_density_rms         0.554
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.166
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         2673
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.1247
_refine_ls_R_factor_gt           0.1081
_refine_ls_restrained_S_all      1.159
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+294.2910P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2569
_refine_ls_wR_factor_ref         0.2649
_refine_special_details          
;
A lot of effort has been utaken to refine this low-quality structure.
However, several electron density peaks still cannot be interpreted in a
chemically correct way.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O6) \\sim Ueq, Uanis(O2) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(O5) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C5) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C8(H8)
3.b Idealised tetrahedral OH refined as rotating group:
 O3(H3)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     'intrinsic phasing'
_atom_sites_solution_secondary   diffmap
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb 0.65734(9) 0.08206(17) 0.21733(6) 0.0096(3) Uani 1 1 d . . . . .
O1 O 0.6056(17) 0.263(3) 0.3262(11) 0.027(4) Uani 1 1 d . . . . .
O2 O 0.6991(13) 0.554(3) 0.3556(9) 0.013(3) Uani 1 1 d . U . . .
O3 O 0.660(2) 0.780(3) 0.4763(14) 0.043(6) Uani 1 1 d . . . . .
H3 H 0.6991 0.7363 0.4429 0.065 Uiso 1 1 calc GR . . . .
O4 O 0.5172(15) -0.102(3) 0.2656(11) 0.023(4) Uani 1 1 d . . . . .
O5 O 0.7068(13) 0.405(3) 0.1823(9) 0.015(3) Uani 1 1 d . U . . .
O6 O 0.6747(13) 0.727(3) 0.1795(9) 0.014(3) Uani 1 1 d . U . . .
O7 O 0.5410(14) 0.171(2) 0.1069(9) 0.013(3) Uani 1 1 d . . . . .
C1 C 0.627(2) 0.428(4) 0.3693(14) 0.019(5) Uani 1 1 d . . . . .
C2 C 0.562(2) 0.465(4) 0.4366(15) 0.017(5) Uani 1 1 d . U . . .
C3 C 0.581(2) 0.640(4) 0.4850(15) 0.019(5) Uani 1 1 d . U . . .
C4 C 0.483(2) 0.329(4) 0.4536(16) 0.020(5) Uani 1 1 d . . . . .
H4 H 0.4720 0.2073 0.4217 0.024 Uiso 1 1 calc R . . . .
C5 C 0.6492(17) 0.564(4) 0.1495(12) 0.010(4) Uani 1 1 d . U . . .
C6 C 0.571(2) 0.526(4) 0.0731(16) 0.018(5) Uani 1 1 d . . . . .
C7 C 0.524(2) 0.326(4) 0.0546(17) 0.020(5) Uani 1 1 d . . . . .
C8 C 0.456(2) 0.308(4) -0.0215(15) 0.016(5) Uani 1 1 d . . . . .
H8 H 0.4278 0.1774 -0.0385 0.019 Uiso 1 1 calc R . . . .
O3W O 0.3383(19) 0.135(3) 0.2732(14) 0.037(5) Uani 1 1 d . . . . .
O4W O 0.4339(18) 0.526(3) 0.2256(13) 0.035(5) Uani 1 1 d . . . . .
O1W O 0.3233(17) 0.041(3) 0.1014(12) 0.029(5) Uani 1 1 d . . . . .
O2W O 0.2546(18) 0.458(3) 0.0974(14) 0.037(5) Uani 1 1 d . . . . .


_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 2.321(17) . ?
Tb1 O2 2.304(15) 2_645 ?
Tb1 O4 2.350(17) . ?
Tb1 O5 2.455(16) 2_645 ?
Tb1 O5 2.296(18) . ?
Tb1 O6 2.420(17) 1_545 ?
Tb1 O6 2.645(16) 2_645 ?
Tb1 O7 2.211(15) . ?
Tb1 C5 2.98(2) 2_645 ?
O1 C1 1.29(3) . ?
O2 Tb1 2.304(15) 2_655 ?
O2 C1 1.26(3) . ?
O3 H3 0.8400 . ?
O3 C3 1.36(3) . ?
O5 Tb1 2.455(16) 2_655 ?
O5 C5 1.33(3) . ?
O6 Tb1 2.645(16) 2_655 ?
O6 Tb1 2.420(17) 1_565 ?
O6 C5 1.20(3) . ?
O7 C7 1.33(3) . ?
C1 C2 1.49(3) . ?
C2 C3 1.40(3) . ?
C2 C4 1.38(3) . ?
C3 C4 1.40(3) 3_666 ?
C4 C3 1.40(3) 3_666 ?
C4 H4 0.9500 . ?
C5 Tb1 2.98(2) 2_655 ?
C5 C6 1.48(3) . ?
C6 C7 1.44(3) . ?
C6 C8 1.39(3) 3_665 ?
C7 C8 1.40(3) . ?
C8 C6 1.39(3) 3_665 ?
C8 H8 0.9500 . ?

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 O4 71.9(6) . . ?
O1 Tb1 O5 87.9(7) . 2_645 ?
O1 Tb1 O6 66.7(6) . 2_645 ?
O1 Tb1 O6 137.2(6) . 1_545 ?
O1 Tb1 C5 74.9(7) . 2_645 ?
O2 Tb1 O1 140.6(6) 2_645 . ?
O2 Tb1 O4 143.8(6) 2_645 . ?
O2 Tb1 O5 79.2(5) 2_645 2_645 ?
O2 Tb1 O6 71.5(6) 2_645 1_545 ?
O2 Tb1 O6 76.8(5) 2_645 2_645 ?
O2 Tb1 C5 77.6(5) 2_645 2_645 ?
O4 Tb1 O5 89.6(6) . 2_645 ?
O4 Tb1 O6 120.8(6) . 2_645 ?
O4 Tb1 O6 72.4(6) . 1_545 ?
O4 Tb1 C5 106.2(6) . 2_645 ?
O5 Tb1 O1 81.0(6) . . ?
O5 Tb1 O2 71.5(6) . 2_645 ?
O5 Tb1 O4 142.7(6) . . ?
O5 Tb1 O5 115.0(4) . 2_645 ?
O5 Tb1 O6 67.6(5) . 2_645 ?
O5 Tb1 O6 141.0(5) . 1_545 ?
O5 Tb1 O6 49.6(5) 2_645 2_645 ?
O5 Tb1 C5 90.4(6) . 2_645 ?
O5 Tb1 C5 26.0(6) 2_645 2_645 ?
O6 Tb1 O5 69.0(6) 1_545 2_645 ?
O6 Tb1 O6 114.7(4) 1_545 2_645 ?
O6 Tb1 C5 93.3(6) 1_545 2_645 ?
O6 Tb1 C5 23.6(6) 2_645 2_645 ?
O7 Tb1 O1 106.2(7) . . ?
O7 Tb1 O2 92.7(6) . 2_645 ?
O7 Tb1 O4 89.7(6) . . ?
O7 Tb1 O5 164.9(6) . 2_645 ?
O7 Tb1 O5 73.5(6) . . ?
O7 Tb1 O6 96.5(6) . 1_545 ?
O7 Tb1 O6 141.0(5) . 2_645 ?
O7 Tb1 C5 163.3(6) . 2_645 ?
C1 O1 Tb1 142.3(16) . . ?
C1 O2 Tb1 140.4(16) . 2_655 ?
C3 O3 H3 109.5 . . ?
Tb1 O5 Tb1 116.5(6) . 2_655 ?
C5 O5 Tb1 132.5(14) . . ?
C5 O5 Tb1 99.9(13) . 2_655 ?
Tb1 O6 Tb1 105.7(6) 1_565 2_655 ?
C5 O6 Tb1 158.9(15) . 1_565 ?
C5 O6 Tb1 94.2(14) . 2_655 ?
C7 O7 Tb1 138.8(15) . . ?
O1 C1 C2 117(2) . . ?
O2 C1 O1 122(2) . . ?
O2 C1 C2 120(2) . . ?
C3 C2 C1 120(2) . . ?
C4 C2 C1 122(2) . . ?
C4 C2 C3 118(2) . . ?
O3 C3 C2 123(2) . . ?
O3 C3 C4 119(2) . 3_666 ?
C2 C3 C4 118(2) . 3_666 ?
C2 C4 C3 124(2) . 3_666 ?
C2 C4 H4 118.1 . . ?
C3 C4 H4 118.1 3_666 . ?
O5 C5 Tb1 54.2(10) . 2_655 ?
O5 C5 C6 116.8(19) . . ?
O6 C5 Tb1 62.2(12) . 2_655 ?
O6 C5 O5 116.2(19) . . ?
O6 C5 C6 126(2) . . ?
C6 C5 Tb1 166.4(16) . 2_655 ?
C7 C6 C5 121(2) . . ?
C8 C6 C5 117(2) 3_665 . ?
C8 C6 C7 122(2) 3_665 . ?
O7 C7 C6 122(2) . . ?
O7 C7 C8 122(2) . . ?
C8 C7 C6 116(2) . . ?
C6 C8 C7 122(2) 3_665 . ?
C6 C8 H8 118.8 3_665 . ?
C7 C8 H8 118.8 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Tb1 O1 C1 O2 0(5) . . . . ?
Tb1 O1 C1 C2 -180(2) . . . . ?
Tb1 O2 C1 O1 -13(4) 2_655 . . . ?
Tb1 O2 C1 C2 167.4(16) 2_655 . . . ?
Tb1 O5 C5 Tb1 140.6(18) . . . 2_655 ?
Tb1 O5 C5 O6 -4(2) 2_655 . . . ?
Tb1 O5 C5 O6 136.6(17) . . . . ?
Tb1 O5 C5 C6 -51(3) . . . . ?
Tb1 O5 C5 C6 167.9(17) 2_655 . . . ?
Tb1 O6 C5 Tb1 -161(4) 1_565 . . 2_655 ?
Tb1 O6 C5 O5 -157(3) 1_565 . . . ?
Tb1 O6 C5 O5 3.7(19) 2_655 . . . ?
Tb1 O6 C5 C6 32(6) 1_565 . . . ?
Tb1 O6 C5 C6 -167(2) 2_655 . . . ?
Tb1 O7 C7 C6 -18(4) . . . . ?
Tb1 O7 C7 C8 163.7(18) . . . . ?
Tb1 C5 C6 C7 72(8) 2_655 . . . ?
Tb1 C5 C6 C8 -109(7) 2_655 . . 3_665 ?
O1 C1 C2 C3 -180(2) . . . . ?
O1 C1 C2 C4 1(4) . . . . ?
O2 C1 C2 C3 0(4) . . . . ?
O2 C1 C2 C4 -180(2) . . . . ?
O5 C5 C6 C7 26(3) . . . . ?
O5 C5 C6 C8 -155(2) . . . 3_665 ?
O6 C5 C6 C7 -163(2) . . . . ?
O6 C5 C6 C8 16(4) . . . 3_665 ?
O7 C7 C8 C6 174(2) . . . 3_665 ?
C1 C2 C3 O3 -2(4) . . . . ?
C1 C2 C3 C4 179(2) . . . 3_666 ?
C1 C2 C4 C3 -178(3) . . . 3_666 ?
C3 C2 C4 C3 2(5) . . . 3_666 ?
C4 C2 C3 O3 177(3) . . . . ?
C4 C2 C3 C4 -2(4) . . . 3_666 ?
C5 C6 C7 O7 5(4) . . . . ?
C5 C6 C7 C8 -176(2) . . . . ?
C6 C7 C8 C6 -5(4) . . . 3_665 ?
C8 C6 C7 O7 -174(2) 3_665 . . . ?
C8 C6 C7 C8 5(4) 3_665 . . . ?

_shelx_SHELXL_version_number     2014/7

_olex2_submission_special_instructions 'No special instructions were received'
# start Validation Reply Form
_vrf_DIFMN02_Sion-1_H2O          
;
PROBLEM: The minimum difference density is < -0.1*ZMAX*1.00
RESPONSE: Inconsistent minima of electron density in the difference-Fourier 
		  maps can occur for such type of soft crystals with massive amount
		  of disordered solvent molecules.
;
_vrf_PLAT043_Sion-1_H2O          
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..       8.05 Check 
RESPONSE: Reported molecular weight accounts for hydrogen atoms attached to 
		  water, of which the location was not resolved.
;
_vrf_PLAT097_Sion-1_H2O          
;
PROBLEM: Large Reported Max.  (Positive) Residual Density       8.27 eA-3  
RESPONSE: All intense (stronger than 1.7 e/A^3) electron density maxima 
		  are located close to cental Tb-atom, in places where no atoms 
		  are expected. Local maxima of electron density about O-atoms 
		  are due to disordered O-atoms (both carboxylate and/or solvent 
		  molecule) that cannot be refined in a chemically reasonable way.
;
_vrf_PLAT098_Sion-1_H2O          
;
PROBLEM: Large Reported Min.  (Negative) Residual Density     -10.67 eA-3  
RESPONSE: Unresolved disorder (observed as electron density maxima 
		  mentioned above), unaccounted for by the model, causes the 
		  appearance of local electron density minima.
;
_vrf_PLAT306_Sion-1_H2O          
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        O1W Check 
RESPONSE: Hydrogen atoms attached to the free solvent water molecules 
		  could not be localised in chemically reasonable positions; 
		  difference-Fourier maps do not provide any hint about the 
		  location of H-atoms.
;
_vrf_PLAT342_Sion-1_H2O          
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............     0.0375 Ang.  
RESPONSE: Low bond precision can occur in strongly disordered structures.
;
_vrf_PLAT430_Sion-1_H2O          
;
PROBLEM: Short Inter D...A Contact  O1W    ..  O7      ..       2.81 Ang.  
RESPONSE: This short contact is due to specific interactions between main 
		  framework O-atoms and free water molecules.
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Sion-2
_database_code_depnum_ccdc_archive 'CCDC 1503701'
_audit_update_record             
;
2016-09-09 deposited with the CCDC.
2017-05-16 downloaded from the CCDC.
;
_audit_creation_date             2016-04-26
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C18 H20 N2 O11 Tb, C3 H7 N O'
_chemical_formula_sum            'C21 H27 N3 O12 Tb'
_chemical_formula_weight         672.37
_chemical_melting_point          ?
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'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.4608(8)
_cell_length_b                   10.9006(10)
_cell_length_c                   12.5293(10)
_cell_angle_alpha                104.610(5)
_cell_angle_beta                 107.840(4)
_cell_angle_gamma                97.204(4)
_cell_volume                     1283.78(19)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9775
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      36.459
_cell_measurement_theta_min      2.918
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.821
_exptl_absorpt_correction_T_max  0.7474
_exptl_absorpt_correction_T_min  0.6344
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1357 before and 0.0536 after correction.
The Ratio of minimum to maximum transmission is 0.8488.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.739
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             670
_exptl_crystal_size_max          0.221
_exptl_crystal_size_mid          0.146
_exptl_crystal_size_min          0.059
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0389
_diffrn_reflns_av_unetI/netI     0.0244
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            38205
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.322
_diffrn_reflns_theta_min         2.920
_diffrn_ambient_temperature      149.72
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5942
_reflns_number_total             6365
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.701
_refine_diff_density_min         -1.062
_refine_diff_density_rms         0.092
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         6365
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0211
_refine_ls_R_factor_gt           0.0180
_refine_ls_restrained_S_all      1.080
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0186P)²+0.8886P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0421
_refine_ls_wR_factor_ref         0.0433
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O1B) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.02
3. Others
 Sof(C1B)=Sof(H1BA)=Sof(C2B)=Sof(H2BA)=Sof(H2BB)=Sof(H2BC)=Sof(C3B)=Sof(H3BA)=
 Sof(H3BB)=Sof(H3BC)=1-FVAR(1)
 Sof(C1A)=Sof(H1AA)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(H2AC)=Sof(C3A)=Sof(H3AA)=
 Sof(H3AB)=Sof(H3AC)=FVAR(1)
 Sof(O1B)=Sof(H1B)=Sof(H12A)=1-FVAR(2)
 Sof(O1A)=Sof(H1A)=Sof(H14)=FVAR(2)
4.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C8(H8), C10(H10), C12(H12A), C13(H13), C14(H14), C1A(H1AA), C1B(H1BA)
4.b Tetrahedral OH refined with riding coordinates:
 O1B(H1B)
4.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,
 H18C), C2A(H2AA,H2AB,H2AC), C3A(H3AA,H3AB,H3AC), C2B(H2BA,H2BB,H2BC), C3B(H3BA,
 H3BB,H3BC)
4.d Idealised tetrahedral OH refined as rotating group:
 O9(H9), O12(H12), O1A(H1A)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb 0.09524(2) 0.54648(2) 0.68252(2) 0.00936(3) Uani 1 1 d . . . . .
O2 O -0.03522(14) 0.33485(13) 0.58669(12) 0.0147(3) Uani 1 1 d . . . . .
O3 O 0.15492(14) 0.48617(14) 0.51705(13) 0.0161(3) Uani 1 1 d . . . . .
O4 O -0.08158(15) 0.27329(13) 0.39172(12) 0.0161(3) Uani 1 1 d . . . . .
O5 O 0.05737(16) 0.48406(15) 0.84097(13) 0.0221(3) Uani 1 1 d . . . . .
O6 O 0.12999(14) 0.42331(14) 0.32845(13) 0.0174(3) Uani 1 1 d . . . . .
O7 O 0.16541(14) 0.76304(14) 0.84965(12) 0.0182(3) Uani 1 1 d . . . . .
O8 O 0.32058(15) 0.68080(14) 0.78648(13) 0.0203(3) Uani 1 1 d . . . . .
O9 O 0.0450(2) -0.04900(16) 0.71314(14) 0.0313(4) Uani 1 1 d . . . . .
H9 H 0.0641 -0.1222 0.7096 0.047 Uiso 1 1 calc GR . . . .
O11 O 0.24896(16) 0.40546(16) 0.73393(15) 0.0269(4) Uani 1 1 d . . . . .
O12 O 0.66009(16) 0.6067(2) 0.73618(13) 0.0324(4) Uani 1 1 d . . . . .
H12 H 0.7435 0.6077 0.7467 0.049 Uiso 1 1 calc GR . . . .
N1 N -0.0129(2) 0.30860(19) 0.89185(17) 0.0248(4) Uani 1 1 d . . . . .
O1A O 0.23375(17) 1.00531(17) 0.99287(16) 0.0224(5) Uani 0.890(5) 1 d . . P A 1
H1A H 0.1779 0.9373 0.9445 0.034 Uiso 0.890(5) 1 calc GR . P A 1
O1B O 0.5955(14) 0.8009(15) 0.8823(15) 0.032(5) Uani 0.110(5) 1 d . U P A 2
H1B H 0.5355 0.7334 0.8382 0.048 Uiso 0.110(5) 1 calc R . P A 2
N2 N 0.4283(2) 0.3319(2) 0.83040(18) 0.0278(4) Uani 1 1 d . . . . .
C1 C -0.0262(2) 0.12082(18) 0.49287(17) 0.0132(4) Uani 1 1 d . . . . .
C2 C 0.20588(19) 0.46266(18) 0.43686(18) 0.0132(4) Uani 1 1 d . . . . .
C3 C 0.35746(19) 0.48144(19) 0.46797(17) 0.0135(4) Uani 1 1 d . . . . .
C4 C -0.04941(19) 0.25248(18) 0.49086(17) 0.0123(4) Uani 1 1 d . . . . .
C5 C 0.4421(2) 0.5356(2) 0.58566(17) 0.0172(4) Uani 1 1 d . . . . .
H5 H 0.4020 0.5606 0.6441 0.021 Uiso 1 1 calc R . . . .
C6 C 0.5841(2) 0.5537(2) 0.61907(17) 0.0176(4) Uani 1 1 d . . . . .
C7 C 0.2880(2) 0.77184(19) 0.85071(17) 0.0139(4) Uani 1 1 d . . . . .
C8 C -0.0030(2) 0.09086(19) 0.59755(18) 0.0175(4) Uani 1 1 d . . . . .
H8 H -0.0052 0.1537 0.6647 0.021 Uiso 1 1 calc R . . . .
C9 C 0.0234(2) -0.0282(2) 0.60684(18) 0.0173(4) Uani 1 1 d . . . . .
C10 C -0.0313(2) 0.3876(2) 0.82730(19) 0.0207(4) Uani 1 1 d . . . . .
H10 H -0.1179 0.3702 0.7661 0.025 Uiso 1 1 calc R . . . .
N3 N 0.4760(3) 0.1523(2) 0.4537(2) 0.0402(5) Uani 1 1 d . . . . .
C11 C 0.3962(2) 0.89084(19) 0.92804(16) 0.0137(4) Uani 1 1 d . . . . .
C12 C 0.3636(2) 0.9983(2) 0.99486(17) 0.0155(4) Uani 1 1 d . . . . .
H12A H 0.2714 0.9970 0.9913 0.019 Uiso 0.110(5) 1 calc R . P A 2
C13 C 0.3703(2) 0.4229(2) 0.7954(2) 0.0245(5) Uani 1 1 d . . . . .
H13 H 0.4265 0.5076 0.8194 0.029 Uiso 1 1 calc R . . . .
C14 C 0.5322(2) 0.89356(19) 0.93387(17) 0.0158(4) Uani 1 1 d . . . . .
H14 H 0.5535 0.8204 0.8885 0.019 Uiso 0.890(5) 1 calc R . P A 1
C15 C -0.1210(3) 0.1983(3) 0.8714(3) 0.0401(7) Uani 1 1 d . . . . .
H15A H -0.1482 0.2097 0.9408 0.060 Uiso 1 1 calc GR . . . .
H15B H -0.0869 0.1182 0.8567 0.060 Uiso 1 1 calc GR . . . .
H15C H -0.2008 0.1927 0.8027 0.060 Uiso 1 1 calc GR . . . .
O10 O 0.6063(3) 0.2237(3) 0.6482(2) 0.0756(8) Uani 1 1 d . . . . .
C16 C 0.1145(3) 0.3282(3) 0.9884(3) 0.0518(8) Uani 1 1 d . . . . .
H16A H 0.1804 0.4032 0.9925 0.078 Uiso 1 1 calc GR . . . .
H16B H 0.1528 0.2505 0.9755 0.078 Uiso 1 1 calc GR . . . .
H16C H 0.0966 0.3444 1.0625 0.078 Uiso 1 1 calc GR . . . .
C17 C 0.3528(3) 0.2008(3) 0.7969(3) 0.0472(7) Uani 1 1 d . . . . .
H17A H 0.3360 0.1837 0.8652 0.071 Uiso 1 1 calc GR . . . .
H17B H 0.4061 0.1407 0.7687 0.071 Uiso 1 1 calc GR . . . .
H17C H 0.2646 0.1882 0.7339 0.071 Uiso 1 1 calc GR . . . .
C18 C 0.5755(3) 0.3633(3) 0.9009(3) 0.0487(8) Uani 1 1 d . . . . .
H18A H 0.6231 0.3096 0.8578 0.073 Uiso 1 1 calc GR . . . .
H18B H 0.5880 0.3460 0.9760 0.073 Uiso 1 1 calc GR . . . .
H18C H 0.6139 0.4553 0.9158 0.073 Uiso 1 1 calc GR . . . .
C1A C 0.5941(6) 0.1930(5) 0.5452(5) 0.0503(14) Uani 0.649(6) 1 d . . P B 1
H1AA H 0.6765 0.1985 0.5279 0.060 Uiso 0.649(6) 1 calc R . P B 1
C2A C 0.4693(7) 0.1129(6) 0.3336(5) 0.0602(17) Uani 0.649(6) 1 d . . P B 1
H2AA H 0.5621 0.1332 0.3309 0.090 Uiso 0.649(6) 1 calc GR . P B 1
H2AB H 0.4102 0.1595 0.2892 0.090 Uiso 0.649(6) 1 calc GR . P B 1
H2AC H 0.4313 0.0192 0.2985 0.090 Uiso 0.649(6) 1 calc GR . P B 1
C3A C 0.3455(6) 0.1391(6) 0.4749(6) 0.0592(16) Uani 0.649(6) 1 d . . P B 1
H3AA H 0.3034 0.0468 0.4539 0.089 Uiso 0.649(6) 1 calc GR . P B 1
H3AB H 0.2831 0.1803 0.4266 0.089 Uiso 0.649(6) 1 calc GR . P B 1
H3AC H 0.3626 0.1816 0.5584 0.089 Uiso 0.649(6) 1 calc GR . P B 1
C1B C 0.4961(13) 0.2021(12) 0.5664(11) 0.063(3) Uani 0.351(6) 1 d . . P B 2
H1BA H 0.4193 0.2231 0.5864 0.076 Uiso 0.351(6) 1 calc R . P B 2
C2B C 0.5984(13) 0.1424(12) 0.4172(11) 0.068(3) Uani 0.351(6) 1 d . . P B 2
H2BA H 0.6815 0.1967 0.4820 0.101 Uiso 0.351(6) 1 calc GR . P B 2
H2BB H 0.5867 0.1724 0.3480 0.101 Uiso 0.351(6) 1 calc GR . P B 2
H2BC H 0.6075 0.0518 0.3976 0.101 Uiso 0.351(6) 1 calc GR . P B 2
C3B C 0.3435(13) 0.1200(12) 0.3586(12) 0.085(5) Uani 0.351(6) 1 d . . P B 2
H3BA H 0.2725 0.1419 0.3914 0.127 Uiso 0.351(6) 1 calc GR . P B 2
H3BB H 0.3201 0.0268 0.3161 0.127 Uiso 0.351(6) 1 calc GR . P B 2
H3BC H 0.3488 0.1695 0.3041 0.127 Uiso 0.351(6) 1 calc GR . P B 2


_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 O2 2.3313(14) . ?
Tb1 O3 2.3084(14) . ?
Tb1 O4 2.3783(14) 2_566 ?
Tb1 O5 2.3783(15) . ?
Tb1 O6 2.3869(14) 2_566 ?
Tb1 O7 2.5742(15) . ?
Tb1 O8 2.3849(14) . ?
Tb1 O11 2.4183(15) . ?
Tb1 C2 3.0213(19) 2_566 ?
Tb1 C7 2.8432(19) . ?
O2 C4 1.258(2) . ?
O3 C2 1.262(2) . ?
O4 Tb1 2.3783(14) 2_566 ?
O4 C4 1.270(2) . ?
O5 C10 1.250(3) . ?
O6 Tb1 2.3869(14) 2_566 ?
O6 C2 1.272(2) . ?
O7 C7 1.269(2) . ?
O8 C7 1.264(2) . ?
O9 H9 0.8400 . ?
O9 C9 1.363(2) . ?
O11 C13 1.228(3) . ?
O12 H12 0.8400 . ?
O12 C6 1.364(2) . ?
N1 C10 1.316(3) . ?
N1 C15 1.455(3) . ?
N1 C16 1.447(3) . ?
O1A H1A 0.8400 . ?
O1A C12 1.363(2) . ?
O1B H1B 0.8400 . ?
O1B C14 1.406(13) . ?
N2 C13 1.324(3) . ?
N2 C17 1.433(4) . ?
N2 C18 1.467(3) . ?
C1 C4 1.490(3) . ?
C1 C8 1.388(3) . ?
C1 C9 1.405(3) 2_556 ?
C2 Tb1 3.0213(18) 2_566 ?
C2 C3 1.486(2) . ?
C3 C5 1.392(3) . ?
C3 C6 1.402(3) 2_666 ?
C5 H5 0.9500 . ?
C5 C6 1.387(3) . ?
C6 C3 1.402(3) 2_666 ?
C7 C11 1.493(3) . ?
C8 H8 0.9500 . ?
C8 C9 1.386(3) . ?
C9 C1 1.405(3) 2_556 ?
C10 H10 0.9500 . ?
N3 C1A 1.332(6) . ?
N3 C2A 1.434(6) . ?
N3 C3A 1.466(6) . ?
N3 C1B 1.317(12) . ?
N3 C2B 1.493(11) . ?
N3 C3B 1.456(11) . ?
C11 C12 1.404(3) . ?
C11 C14 1.398(3) . ?
C12 H12A 0.9500 . ?
C12 C14 1.387(3) 2_677 ?
C13 H13 0.9500 . ?
C14 C12 1.388(3) 2_677 ?
C14 H14 0.9500 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
O10 C1A 1.211(6) . ?
O10 C1B 1.233(13) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C1A H1AA 0.9500 . ?
C2A H2AA 0.9800 . ?
C2A H2AB 0.9800 . ?
C2A H2AC 0.9800 . ?
C3A H3AA 0.9800 . ?
C3A H3AB 0.9800 . ?
C3A H3AC 0.9800 . ?
C1B H1BA 0.9500 . ?
C2B H2BA 0.9800 . ?
C2B H2BB 0.9800 . ?
C2B H2BC 0.9800 . ?
C3B H3BA 0.9800 . ?
C3B H3BB 0.9800 . ?
C3B H3BC 0.9800 . ?

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 Tb1 O4 126.69(5) . 2_566 ?
O2 Tb1 O5 78.25(5) . . ?
O2 Tb1 O6 78.69(5) . 2_566 ?
O2 Tb1 O7 151.35(5) . . ?
O2 Tb1 O8 146.07(5) . . ?
O2 Tb1 O11 74.04(5) . . ?
O2 Tb1 C2 67.36(5) . 2_566 ?
O2 Tb1 C7 163.41(5) . . ?
O3 Tb1 O2 77.34(5) . . ?
O3 Tb1 O4 75.84(5) . 2_566 ?
O3 Tb1 O5 146.03(5) . . ?
O3 Tb1 O6 122.28(5) . 2_566 ?
O3 Tb1 O7 131.17(5) . . ?
O3 Tb1 O8 88.77(5) . . ?
O3 Tb1 O11 78.29(6) . . ?
O3 Tb1 C2 98.80(5) . 2_566 ?
O3 Tb1 C7 109.95(5) . . ?
O4 Tb1 O5 138.11(5) 2_566 . ?
O4 Tb1 O6 78.15(5) 2_566 2_566 ?
O4 Tb1 O7 68.30(5) 2_566 . ?
O4 Tb1 O8 77.78(5) 2_566 . ?
O4 Tb1 O11 140.94(5) 2_566 . ?
O4 Tb1 C2 72.38(5) 2_566 2_566 ?
O4 Tb1 C7 69.90(5) 2_566 . ?
O5 Tb1 O6 74.90(5) . 2_566 ?
O5 Tb1 O7 76.54(5) . . ?
O5 Tb1 O8 98.67(5) . . ?
O5 Tb1 O11 72.51(6) . . ?
O5 Tb1 C2 93.19(5) . 2_566 ?
O5 Tb1 C7 88.57(5) . . ?
O6 Tb1 O7 81.79(5) 2_566 . ?
O6 Tb1 O11 140.88(5) 2_566 . ?
O6 Tb1 C2 23.70(5) 2_566 2_566 ?
O6 Tb1 C7 107.78(5) 2_566 . ?
O7 Tb1 C2 100.65(5) . 2_566 ?
O7 Tb1 C7 26.51(5) . . ?
O8 Tb1 O6 133.70(5) . 2_566 ?
O8 Tb1 O7 52.61(5) . . ?
O8 Tb1 O11 72.88(5) . . ?
O8 Tb1 C2 146.22(5) . 2_566 ?
O8 Tb1 C7 26.16(5) . . ?
O11 Tb1 O7 110.52(5) . . ?
O11 Tb1 C2 140.87(5) . 2_566 ?
O11 Tb1 C7 92.51(6) . . ?
C7 Tb1 C2 124.09(5) . 2_566 ?
C4 O2 Tb1 132.76(12) . . ?
C2 O3 Tb1 171.24(13) . . ?
C4 O4 Tb1 138.29(12) . 2_566 ?
C10 O5 Tb1 123.76(14) . . ?
C2 O6 Tb1 107.36(12) . 2_566 ?
C7 O7 Tb1 88.65(11) . . ?
C7 O8 Tb1 97.59(12) . . ?
C9 O9 H9 109.5 . . ?
C13 O11 Tb1 134.70(15) . . ?
C6 O12 H12 109.5 . . ?
C10 N1 C15 121.6(2) . . ?
C10 N1 C16 121.9(2) . . ?
C16 N1 C15 116.5(2) . . ?
C12 O1A H1A 109.5 . . ?
C14 O1B H1B 109.5 . . ?
C13 N2 C17 121.9(2) . . ?
C13 N2 C18 119.6(2) . . ?
C17 N2 C18 118.4(2) . . ?
C8 C1 C4 118.65(17) . . ?
C8 C1 C9 119.40(18) . 2_556 ?
C9 C1 C4 121.93(17) 2_556 . ?
O3 C2 Tb1 73.34(10) . 2_566 ?
O3 C2 O6 121.36(17) . . ?
O3 C2 C3 120.09(18) . . ?
O6 C2 Tb1 48.94(9) . 2_566 ?
O6 C2 C3 118.55(17) . . ?
C3 C2 Tb1 163.65(14) . 2_566 ?
C5 C3 C2 119.03(17) . . ?
C5 C3 C6 119.84(17) . 2_666 ?
C6 C3 C2 121.13(17) 2_666 . ?
O2 C4 O4 124.76(18) . . ?
O2 C4 C1 118.14(17) . . ?
O4 C4 C1 117.10(17) . . ?
C3 C5 H5 119.5 . . ?
C6 C5 C3 121.10(18) . . ?
C6 C5 H5 119.5 . . ?
O12 C6 C3 123.29(17) . 2_666 ?
O12 C6 C5 117.65(18) . . ?
C5 C6 C3 119.06(18) . 2_666 ?
O7 C7 Tb1 64.84(10) . . ?
O7 C7 C11 120.23(17) . . ?
O8 C7 Tb1 56.25(10) . . ?
O8 C7 O7 120.90(17) . . ?
O8 C7 C11 118.87(17) . . ?
C11 C7 Tb1 173.24(14) . . ?
C1 C8 H8 119.1 . . ?
C9 C8 C1 121.81(18) . . ?
C9 C8 H8 119.1 . . ?
O9 C9 C1 123.48(18) . 2_556 ?
O9 C9 C8 117.72(18) . . ?
C8 C9 C1 118.80(18) . 2_556 ?
O5 C10 N1 124.5(2) . . ?
O5 C10 H10 117.8 . . ?
N1 C10 H10 117.8 . . ?
C1A N3 C2A 123.1(4) . . ?
C1A N3 C3A 119.4(4) . . ?
C2A N3 C3A 117.4(4) . . ?
C1B N3 C2B 118.6(8) . . ?
C1B N3 C3B 124.9(9) . . ?
C3B N3 C2B 116.0(9) . . ?
C12 C11 C7 121.15(17) . . ?
C14 C11 C7 118.81(17) . . ?
C14 C11 C12 120.04(17) . . ?
O1A C12 C11 124.08(18) . . ?
O1A C12 C14 116.80(18) . 2_677 ?
C11 C12 H12A 120.4 . . ?
C14 C12 C11 119.11(18) 2_677 . ?
C14 C12 H12A 120.4 2_677 . ?
O11 C13 N2 124.5(2) . . ?
O11 C13 H13 117.8 . . ?
N2 C13 H13 117.8 . . ?
C11 C14 O1B 132.7(6) . . ?
C11 C14 H14 119.6 . . ?
C12 C14 O1B 106.4(6) 2_677 . ?
C12 C14 C11 120.85(18) 2_677 . ?
C12 C14 H14 119.6 2_677 . ?
N1 C15 H15A 109.5 . . ?
N1 C15 H15B 109.5 . . ?
N1 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N1 C16 H16A 109.5 . . ?
N1 C16 H16B 109.5 . . ?
N1 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N2 C17 H17A 109.5 . . ?
N2 C17 H17B 109.5 . . ?
N2 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N2 C18 H18A 109.5 . . ?
N2 C18 H18B 109.5 . . ?
N2 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N3 C1A H1AA 116.9 . . ?
O10 C1A N3 126.2(5) . . ?
O10 C1A H1AA 116.9 . . ?
N3 C2A H2AA 109.5 . . ?
N3 C2A H2AB 109.5 . . ?
N3 C2A H2AC 109.5 . . ?
H2AA C2A H2AB 109.5 . . ?
H2AA C2A H2AC 109.5 . . ?
H2AB C2A H2AC 109.5 . . ?
N3 C3A H3AA 109.5 . . ?
N3 C3A H3AB 109.5 . . ?
N3 C3A H3AC 109.5 . . ?
H3AA C3A H3AB 109.5 . . ?
H3AA C3A H3AC 109.5 . . ?
H3AB C3A H3AC 109.5 . . ?
N3 C1B H1BA 117.2 . . ?
O10 C1B N3 125.6(9) . . ?
O10 C1B H1BA 117.2 . . ?
N3 C2B H2BA 109.5 . . ?
N3 C2B H2BB 109.5 . . ?
N3 C2B H2BC 109.5 . . ?
H2BA C2B H2BB 109.5 . . ?
H2BA C2B H2BC 109.5 . . ?
H2BB C2B H2BC 109.5 . . ?
N3 C3B H3BA 109.5 . . ?
N3 C3B H3BB 109.5 . . ?
N3 C3B H3BC 109.5 . . ?
H3BA C3B H3BB 109.5 . . ?
H3BA C3B H3BC 109.5 . . ?
H3BB C3B H3BC 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Tb1 O2 C4 O4 -53.0(3) . . . . ?
Tb1 O2 C4 C1 126.60(16) . . . . ?
Tb1 O4 C4 O2 13.6(3) 2_566 . . . ?
Tb1 O4 C4 C1 -165.96(13) 2_566 . . . ?
Tb1 O5 C10 N1 140.54(18) . . . . ?
Tb1 O6 C2 O3 12.6(2) 2_566 . . . ?
Tb1 O6 C2 C3 -167.10(14) 2_566 . . . ?
Tb1 O7 C7 O8 -4.85(19) . . . . ?
Tb1 O7 C7 C11 174.94(16) . . . . ?
Tb1 O8 C7 O7 5.3(2) . . . . ?
Tb1 O8 C7 C11 -174.51(15) . . . . ?
Tb1 O11 C13 N2 166.08(17) . . . . ?
Tb1 C2 C3 C5 137.5(4) 2_566 . . . ?
Tb1 C2 C3 C6 -42.1(6) 2_566 . . 2_666 ?
O3 C2 C3 C5 -5.5(3) . . . . ?
O3 C2 C3 C6 174.92(19) . . . 2_666 ?
O6 C2 C3 C5 174.19(19) . . . . ?
O6 C2 C3 C6 -5.4(3) . . . 2_666 ?
O7 C7 C11 C12 -4.2(3) . . . . ?
O7 C7 C11 C14 175.25(18) . . . . ?
O8 C7 C11 C12 175.55(19) . . . . ?
O8 C7 C11 C14 -5.0(3) . . . . ?
C1 C8 C9 O9 180.0(2) . . . . ?
C1 C8 C9 C1 -0.2(3) . . . 2_556 ?
C2 C3 C5 C6 179.3(2) . . . . ?
C3 C5 C6 O12 -179.6(2) . . . . ?
C3 C5 C6 C3 1.1(4) . . . 2_666 ?
C4 C1 C8 C9 -178.06(19) . . . . ?
C6 C3 C5 C6 -1.1(4) 2_666 . . . ?
C7 C11 C12 O1A -1.9(3) . . . . ?
C7 C11 C12 C14 179.54(18) . . . 2_677 ?
C7 C11 C14 O1B -2.6(11) . . . . ?
C7 C11 C14 C12 -179.56(18) . . . 2_677 ?
C8 C1 C4 O2 6.0(3) . . . . ?
C8 C1 C4 O4 -174.34(18) . . . . ?
C9 C1 C4 O2 -172.16(18) 2_556 . . . ?
C9 C1 C4 O4 7.5(3) 2_556 . . . ?
C9 C1 C8 C9 0.2(4) 2_556 . . . ?
C12 C11 C14 O1B 176.9(11) . . . . ?
C12 C11 C14 C12 -0.1(3) . . . 2_677 ?
C14 C11 C12 O1A 178.6(2) . . . . ?
C14 C11 C12 C14 0.1(3) . . . 2_677 ?
C15 N1 C10 O5 179.7(2) . . . . ?
C16 N1 C10 O5 1.1(4) . . . . ?
C17 N2 C13 O11 1.2(4) . . . . ?
C18 N2 C13 O11 178.2(2) . . . . ?
C2A N3 C1A O10 -177.7(5) . . . . ?
C3A N3 C1A O10 -1.3(7) . . . . ?
C2B N3 C1B O10 -11.9(14) . . . . ?
C3B N3 C1B O10 176.1(9) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
