# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_SION2_100K
_database_code_depnum_ccdc_archive 'CCDC 1871302'
loop_
_audit_author_name
_audit_author_address
'Andrzej Gladysiak'
;Ecole polytechnique f?d?rale de Lausanne
Switzerland
;
_audit_update_record             
;
2018-10-03 deposited with the CCDC.	2019-08-12 downloaded from the CCDC.
;
_audit_creation_date             2018-07-09
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_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          ?
_chemical_oxdiff_formula         'C21 H27 N3 O12 Tb1'
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                   10.5096(6)
_cell_length_b                   10.9768(4)
_cell_length_c                   12.5019(6)
_cell_angle_alpha                104.759(4)
_cell_angle_beta                 107.340(5)
_cell_angle_gamma                97.380(4)
_cell_volume                     1298.23(12)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5009
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.4880
_cell_measurement_theta_min      2.0730
_shelx_estimated_absorpt_T_max   0.829
_shelx_estimated_absorpt_T_min   0.605
_exptl_absorpt_coefficient_mu    2.790
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80799
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.720
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             670
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0174
_diffrn_reflns_av_unetI/netI     0.0261
_diffrn_reflns_Laue_measured_fraction_full 0.714
_diffrn_reflns_Laue_measured_fraction_max 0.652
_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       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8177
_diffrn_reflns_point_group_measured_fraction_full 0.714
_diffrn_reflns_point_group_measured_fraction_max 0.652
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.431
_diffrn_reflns_theta_min         1.977
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            PILATUS2M
_diffrn_measured_fraction_theta_full 0.714
_diffrn_measured_fraction_theta_max 0.652
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      0.00 360.00   1.00    1.00    --    0.00   0.00   0.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  PILATUS@SNBL
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0597171000
_diffrn_orient_matrix_UB_12      -0.0137259000
_diffrn_orient_matrix_UB_13      0.0360613000
_diffrn_orient_matrix_UB_21      -0.0286008000
_diffrn_orient_matrix_UB_22      -0.0676179000
_diffrn_orient_matrix_UB_23      -0.0272211000
_diffrn_orient_matrix_UB_31      0.0307492000
_diffrn_orient_matrix_UB_32      0.0000326000
_diffrn_orient_matrix_UB_33      -0.0438156000
_diffrn_radiation_monochromator  'Si (111)'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           ?
_diffrn_radiation_wavelength     0.7142
_diffrn_source                   
'European Synchrotron Radiation Facility, BM01 beamline'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3950
_reflns_number_total             4196
_reflns_odcompleteness_completeness 70.39
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.51
_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 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (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    'XT (Sheldrick, 2015)'
_refine_diff_density_max         1.905
_refine_diff_density_min         -1.531
_refine_diff_density_rms         0.114
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         4196
_refine_ls_number_restraints     75
_refine_ls_R_factor_all          0.0349
_refine_ls_R_factor_gt           0.0330
_refine_ls_restrained_S_all      1.096
_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)+(0.0705P)²+0.6708P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0938
_refine_ls_wR_factor_ref         0.0948
_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
 O1B-C11 \\sim C11-O1A
 with sigma of 0.02
 O1A-C12 \\sim O1B-C14
 with sigma of 0.02
3. Restrained planarity
 O1B, C14, C11, C12, O8, C7, O7
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
O3 \\sim C2: within 2A with sigma of 0.002 and sigma for terminal atoms of 0.004
5. Rigid body (RIGU) restrains
 C1A, N3, C2A, C3A, O10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O10, C1B, N3, C3B, C2B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O3, C2, O6, C3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. 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)
7.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C8(H8), C10(H10), C12(H12A), C13(H13), C14(H14), C1A(H1AA), C1B(H1BA)
7.b Tetrahedral OH refined with riding coordinates:
 O1B(H1B)
7.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)
7.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 0.09419(2) 0.54650(2) 0.68266(2) 0.02445(11) Uani 1 1 d . . . . .
O2 O -0.0365(3) 0.3346(3) 0.5869(3) 0.0267(7) Uani 1 1 d . . . . .
O3 O 0.1537(3) 0.4851(3) 0.5157(3) 0.0284(6) Uani 1 1 d . U . . .
O4 O -0.0827(3) 0.2727(3) 0.3919(3) 0.0295(7) Uani 1 1 d . . . . .
O5 O 0.0558(3) 0.4848(3) 0.8415(3) 0.0342(8) Uani 1 1 d . . . . .
O6 O 0.1304(3) 0.4227(3) 0.3275(3) 0.0308(7) Uani 1 1 d . U . . .
O7 O 0.1641(3) 0.7641(3) 0.8509(3) 0.0331(8) Uani 1 1 d . . . . .
O8 O 0.3193(3) 0.6806(3) 0.7868(3) 0.0342(8) Uani 1 1 d . . . . .
O9 O 0.0440(5) -0.0487(3) 0.7139(3) 0.0426(9) Uani 1 1 d . . . . .
H9 H 0.0660 -0.1201 0.7112 0.064 Uiso 1 1 calc GR . . . .
O11 O 0.2480(4) 0.4047(3) 0.7332(3) 0.0395(8) Uani 1 1 d . . . . .
O12 O 0.6584(4) 0.6069(4) 0.7373(3) 0.0445(9) Uani 1 1 d . . . . .
H12 H 0.7408 0.6046 0.7484 0.067 Uiso 1 1 calc GR . . . .
N1 N -0.0147(5) 0.3079(4) 0.8913(4) 0.0363(10) Uani 1 1 d . . . . .
O1A O 0.2339(4) 1.0071(4) 0.9930(4) 0.0361(13) Uani 0.866(11) 1 d D . P A 1
H1A H 0.1790 0.9373 0.9490 0.054 Uiso 0.866(11) 1 calc GR . P A 1
O1B O 0.587(2) 0.801(2) 0.8790(19) 0.061(12) Uani 0.134(11) 1 d D . P A 2
H1B H 0.5246 0.7349 0.8367 0.092 Uiso 0.134(11) 1 calc R . P A 2
N2 N 0.4273(5) 0.3326(4) 0.8312(4) 0.0413(11) Uani 1 1 d . . . . .
C1 C -0.0269(5) 0.1202(4) 0.4929(4) 0.0287(10) Uani 1 1 d . . . . .
C2 C 0.2055(5) 0.4625(4) 0.4370(4) 0.0286(8) Uani 1 1 d . U . . .
C3 C 0.3571(5) 0.4810(4) 0.4664(4) 0.0303(11) Uani 1 1 d . U . . .
C4 C -0.0502(4) 0.2526(4) 0.4906(4) 0.0270(10) Uani 1 1 d . . . . .
C5 C 0.4407(5) 0.5352(4) 0.5864(4) 0.0325(11) Uani 1 1 d . . . . .
H5 H 0.4005 0.5598 0.6450 0.039 Uiso 1 1 calc R . . . .
C6 C 0.5830(5) 0.5527(5) 0.6186(4) 0.0318(11) Uani 1 1 d . . . . .
C7 C 0.2867(4) 0.7725(4) 0.8503(4) 0.0269(10) Uani 1 1 d . . . . .
C8 C -0.0036(5) 0.0908(4) 0.5973(4) 0.0310(10) Uani 1 1 d . . . . .
H8 H -0.0054 0.1535 0.6647 0.037 Uiso 1 1 calc R . . . .
C9 C 0.0226(5) -0.0286(4) 0.6064(4) 0.0299(10) Uani 1 1 d . . . . .
C10 C -0.0338(5) 0.3876(4) 0.8281(4) 0.0360(12) Uani 1 1 d . . . . .
H10 H -0.1204 0.3712 0.7685 0.043 Uiso 1 1 calc R . . . .
N3 N 0.4762(5) 0.1527(5) 0.4539(5) 0.0476(11) Uani 1 1 d . U . . .
C11 C 0.3965(4) 0.8913(4) 0.9286(4) 0.0281(10) Uani 1 1 d D . . . .
C12 C 0.3636(5) 0.9989(4) 0.9949(4) 0.0309(11) Uani 1 1 d D . . . .
H12A H 0.2720 0.9984 0.9913 0.037 Uiso 0.134(11) 1 calc R . P A 2
C13 C 0.3683(5) 0.4226(5) 0.7952(5) 0.0367(11) Uani 1 1 d . . . . .
H13 H 0.4236 0.5071 0.8192 0.044 Uiso 1 1 calc R . . . .
C14 C 0.5312(5) 0.8932(4) 0.9338(4) 0.0291(10) Uani 1 1 d D . . . .
H14 H 0.5519 0.8200 0.8882 0.035 Uiso 0.866(11) 1 calc R . P A 1
C15 C -0.1244(7) 0.1968(5) 0.8707(6) 0.0490(14) Uani 1 1 d . . . . .
H15A H -0.1569 0.2116 0.9377 0.074 Uiso 1 1 calc GR . . . .
H15B H -0.0887 0.1180 0.8621 0.074 Uiso 1 1 calc GR . . . .
H15C H -0.2003 0.1871 0.7987 0.074 Uiso 1 1 calc GR . . . .
O10 O 0.6019(6) 0.2220(6) 0.6495(5) 0.0791(16) Uani 1 1 d . U . . .
C16 C 0.1117(7) 0.3265(6) 0.9886(6) 0.0570(17) Uani 1 1 d . . . . .
H16A H 0.1756 0.4046 0.9972 0.086 Uiso 1 1 calc GR . . . .
H16B H 0.1527 0.2516 0.9724 0.086 Uiso 1 1 calc GR . . . .
H16C H 0.0917 0.3357 1.0616 0.086 Uiso 1 1 calc GR . . . .
C17 C 0.3507(7) 0.1997(5) 0.7974(6) 0.0519(15) Uani 1 1 d . . . . .
H17A H 0.3282 0.1849 0.8644 0.078 Uiso 1 1 calc GR . . . .
H17B H 0.4064 0.1398 0.7742 0.078 Uiso 1 1 calc GR . . . .
H17C H 0.2662 0.1852 0.7310 0.078 Uiso 1 1 calc GR . . . .
C18 C 0.5728(7) 0.3637(7) 0.9027(6) 0.0596(18) Uani 1 1 d . . . . .
H18A H 0.6200 0.3068 0.8624 0.089 Uiso 1 1 calc GR . . . .
H18B H 0.5829 0.3514 0.9795 0.089 Uiso 1 1 calc GR . . . .
H18C H 0.6126 0.4539 0.9142 0.089 Uiso 1 1 calc GR . . . .
C1A C 0.5934(11) 0.1920(10) 0.5447(10) 0.054(2) Uani 0.625(10) 1 d . U P B 1
H1AA H 0.6761 0.1974 0.5280 0.065 Uiso 0.625(10) 1 calc R . P B 1
C2A C 0.4708(14) 0.1144(12) 0.3318(11) 0.064(3) Uani 0.625(10) 1 d . U P B 1
H2AA H 0.5622 0.1402 0.3290 0.096 Uiso 0.625(10) 1 calc GR . P B 1
H2AB H 0.4077 0.1567 0.2869 0.096 Uiso 0.625(10) 1 calc GR . P B 1
H2AC H 0.4387 0.0204 0.2974 0.096 Uiso 0.625(10) 1 calc GR . P B 1
C3A C 0.3440(12) 0.1370(12) 0.4722(12) 0.063(3) Uani 0.625(10) 1 d . U P B 1
H3AA H 0.3013 0.0449 0.4469 0.094 Uiso 0.625(10) 1 calc GR . P B 1
H3AB H 0.2841 0.1806 0.4259 0.094 Uiso 0.625(10) 1 calc GR . P B 1
H3AC H 0.3584 0.1751 0.5559 0.094 Uiso 0.625(10) 1 calc GR . P B 1
C1B C 0.490(2) 0.201(2) 0.5675(17) 0.063(4) Uani 0.375(10) 1 d . U P B 2
H1BA H 0.4119 0.2198 0.5867 0.076 Uiso 0.375(10) 1 calc R . P B 2
C2B C 0.600(2) 0.145(2) 0.4241(19) 0.063(5) Uani 0.375(10) 1 d . U P B 2
H2BA H 0.6807 0.1822 0.4959 0.094 Uiso 0.375(10) 1 calc GR . P B 2
H2BB H 0.6034 0.1926 0.3683 0.094 Uiso 0.375(10) 1 calc GR . P B 2
H2BC H 0.5993 0.0540 0.3883 0.094 Uiso 0.375(10) 1 calc GR . P B 2
C3B C 0.344(2) 0.122(2) 0.357(2) 0.073(6) Uani 0.375(10) 1 d . U P B 2
H3BA H 0.2709 0.1325 0.3899 0.109 Uiso 0.375(10) 1 calc GR . P B 2
H3BB H 0.3263 0.0327 0.3068 0.109 Uiso 0.375(10) 1 calc GR . P B 2
H3BC H 0.3472 0.1808 0.3100 0.109 Uiso 0.375(10) 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 2.348(3) . ?
Tb1 O3 2.318(4) . ?
Tb1 O4 2.400(3) 2_566 ?
Tb1 O5 2.378(4) . ?
Tb1 O6 2.398(3) 2_566 ?
Tb1 O7 2.596(3) . ?
Tb1 O8 2.398(3) . ?
Tb1 O11 2.444(3) . ?
O2 C4 1.261(6) . ?
O3 C2 1.248(7) . ?
O4 Tb1 2.400(3) 2_566 ?
O4 C4 1.263(6) . ?
O5 C10 1.269(6) . ?
O6 Tb1 2.398(3) 2_566 ?
O6 C2 1.284(6) . ?
O7 C7 1.283(6) . ?
O8 C7 1.267(6) . ?
O9 H9 0.8400 . ?
O9 C9 1.375(6) . ?
O11 C13 1.230(6) . ?
O12 H12 0.8400 . ?
O12 C6 1.382(6) . ?
N1 C10 1.316(6) . ?
N1 C15 1.478(7) . ?
N1 C16 1.458(7) . ?
O1A H1A 0.8400 . ?
O1A C12 1.372(7) . ?
O1B H1B 0.8400 . ?
O1B C14 1.367(15) . ?
N2 C13 1.335(6) . ?
N2 C17 1.461(7) . ?
N2 C18 1.466(7) . ?
C1 C4 1.510(5) . ?
C1 C8 1.382(7) . ?
C1 C9 1.401(7) 2_556 ?
C2 C3 1.498(7) . ?
C3 C5 1.415(6) . ?
C3 C6 1.387(8) 2_666 ?
C5 H5 0.9500 . ?
C5 C6 1.401(7) . ?
C6 C3 1.387(8) 2_666 ?
C7 C11 1.510(5) . ?
C8 H8 0.9500 . ?
C8 C9 1.399(6) . ?
C9 C1 1.401(7) 2_556 ?
C10 H10 0.9500 . ?
N3 C1A 1.331(11) . ?
N3 C2A 1.457(13) . ?
N3 C3A 1.470(13) . ?
N3 C1B 1.34(2) . ?
N3 C2B 1.46(2) . ?
N3 C3B 1.48(2) . ?
C11 C12 1.407(6) . ?
C11 C14 1.394(7) . ?
C12 H12A 0.9500 . ?
C12 C14 1.399(6) 2_677 ?
C13 H13 0.9500 . ?
C14 C12 1.399(6) 2_677 ?
C14 H14 0.9500 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
O10 C1A 1.240(13) . ?
O10 C1B 1.26(2) . ?
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 127.00(10) . 2_566 ?
O2 Tb1 O5 78.11(11) . . ?
O2 Tb1 O6 78.76(11) . 2_566 ?
O2 Tb1 O7 151.29(12) . . ?
O2 Tb1 O8 146.03(11) . . ?
O2 Tb1 O11 73.94(11) . . ?
O3 Tb1 O2 77.23(11) . . ?
O3 Tb1 O4 75.88(11) . 2_566 ?
O3 Tb1 O5 145.85(11) . . ?
O3 Tb1 O6 122.15(11) . 2_566 ?
O3 Tb1 O7 131.34(11) . . ?
O3 Tb1 O8 89.07(12) . . ?
O3 Tb1 O11 78.05(13) . . ?
O4 Tb1 O7 68.10(11) 2_566 . ?
O4 Tb1 O11 140.54(13) 2_566 . ?
O5 Tb1 O4 138.26(12) . 2_566 ?
O5 Tb1 O6 75.02(12) . 2_566 ?
O5 Tb1 O7 76.67(11) . . ?
O5 Tb1 O8 98.55(12) . . ?
O5 Tb1 O11 72.65(13) . . ?
O6 Tb1 O4 78.32(11) 2_566 2_566 ?
O6 Tb1 O7 81.66(11) 2_566 . ?
O6 Tb1 O11 141.10(12) 2_566 . ?
O8 Tb1 O4 77.59(11) . 2_566 ?
O8 Tb1 O6 133.62(11) . 2_566 ?
O8 Tb1 O7 52.62(11) . . ?
O8 Tb1 O11 72.86(11) . . ?
O11 Tb1 O7 110.80(11) . . ?
C4 O2 Tb1 132.5(3) . . ?
C2 O3 Tb1 170.3(3) . . ?
C4 O4 Tb1 138.1(3) . 2_566 ?
C10 O5 Tb1 123.9(3) . . ?
C2 O6 Tb1 107.0(3) . 2_566 ?
C7 O7 Tb1 88.2(3) . . ?
C7 O8 Tb1 97.7(3) . . ?
C9 O9 H9 109.5 . . ?
C13 O11 Tb1 134.4(3) . . ?
C6 O12 H12 109.5 . . ?
C10 N1 C15 121.2(5) . . ?
C10 N1 C16 122.7(5) . . ?
C16 N1 C15 116.0(5) . . ?
C12 O1A H1A 109.5 . . ?
C14 O1B H1B 109.5 . . ?
C13 N2 C17 121.3(5) . . ?
C13 N2 C18 120.5(5) . . ?
C17 N2 C18 118.1(5) . . ?
C8 C1 C4 119.0(4) . . ?
C8 C1 C9 119.2(4) . 2_556 ?
C9 C1 C4 121.8(4) 2_556 . ?
O3 C2 O6 121.1(4) . . ?
O3 C2 C3 121.4(4) . . ?
O6 C2 C3 117.6(5) . . ?
C5 C3 C2 117.8(5) . . ?
C6 C3 C2 122.6(4) 2_666 . ?
C6 C3 C5 119.6(4) 2_666 . ?
O2 C4 O4 124.8(4) . . ?
O2 C4 C1 117.8(4) . . ?
O4 C4 C1 117.3(4) . . ?
C3 C5 H5 120.0 . . ?
C6 C5 C3 119.9(5) . . ?
C6 C5 H5 120.0 . . ?
O12 C6 C3 122.7(4) . 2_666 ?
O12 C6 C5 116.8(5) . . ?
C3 C6 C5 120.5(4) 2_666 . ?
O7 C7 C11 120.3(4) . . ?
O8 C7 O7 121.1(4) . . ?
O8 C7 C11 118.6(4) . . ?
C1 C8 H8 119.0 . . ?
C1 C8 C9 121.9(4) . . ?
C9 C8 H8 119.0 . . ?
O9 C9 C1 123.6(4) . 2_556 ?
O9 C9 C8 117.5(4) . . ?
C8 C9 C1 118.9(4) . 2_556 ?
O5 C10 N1 124.4(5) . . ?
O5 C10 H10 117.8 . . ?
N1 C10 H10 117.8 . . ?
C1A N3 C2A 122.6(8) . . ?
C1A N3 C3A 121.1(8) . . ?
C2A N3 C3A 116.2(8) . . ?
C1B N3 C2B 118.4(13) . . ?
C1B N3 C3B 122.7(15) . . ?
C2B N3 C3B 118.5(14) . . ?
C12 C11 C7 120.6(4) . . ?
C14 C11 C7 119.1(4) . . ?
C14 C11 C12 120.3(4) . . ?
O1A C12 C11 124.5(4) . . ?
O1A C12 C14 117.0(4) . 2_677 ?
C11 C12 H12A 120.7 . . ?
C14 C12 C11 118.6(4) 2_677 . ?
C14 C12 H12A 120.7 2_677 . ?
O11 C13 N2 125.0(5) . . ?
O11 C13 H13 117.5 . . ?
N2 C13 H13 117.5 . . ?
O1B C14 C11 130.5(12) . . ?
O1B C14 C12 108.4(12) . 2_677 ?
C11 C14 C12 121.1(4) . 2_677 ?
C11 C14 H14 119.5 . . ?
C12 C14 H14 119.5 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 117.8 . . ?
O10 C1A N3 124.4(10) . . ?
O10 C1A H1AA 117.8 . . ?
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 119.0 . . ?
O10 C1B N3 122.0(18) . . ?
O10 C1B H1BA 119.0 . . ?
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 -53.6(6) . . . . ?
Tb1 O2 C4 C1 126.6(4) . . . . ?
Tb1 O4 C4 O2 15.2(8) 2_566 . . . ?
Tb1 O4 C4 C1 -165.1(3) 2_566 . . . ?
Tb1 O5 C10 N1 139.1(4) . . . . ?
Tb1 O6 C2 O3 12.8(5) 2_566 . . . ?
Tb1 O6 C2 C3 -166.9(3) 2_566 . . . ?
Tb1 O7 C7 O8 -6.0(4) . . . . ?
Tb1 O7 C7 C11 175.8(4) . . . . ?
Tb1 O8 C7 O7 6.6(5) . . . . ?
Tb1 O8 C7 C11 -175.2(3) . . . . ?
Tb1 O11 C13 N2 165.5(4) . . . . ?
O3 C2 C3 C5 -5.1(6) . . . . ?
O3 C2 C3 C6 174.9(4) . . . 2_666 ?
O6 C2 C3 C5 174.6(4) . . . . ?
O6 C2 C3 C6 -5.3(6) . . . 2_666 ?
O7 C7 C11 C12 -5.9(7) . . . . ?
O7 C7 C11 C14 174.5(4) . . . . ?
O8 C7 C11 C12 175.9(4) . . . . ?
O8 C7 C11 C14 -3.7(6) . . . . ?
C1 C8 C9 O9 -179.8(5) . . . . ?
C1 C8 C9 C1 0.8(8) . . . 2_556 ?
C2 C3 C5 C6 179.0(4) . . . . ?
C3 C5 C6 O12 179.6(4) . . . . ?
C3 C5 C6 C3 1.0(8) . . . 2_666 ?
C4 C1 C8 C9 -178.2(4) . . . . ?
C6 C3 C5 C6 -1.0(8) 2_666 . . . ?
C7 C11 C12 O1A -1.4(7) . . . . ?
C7 C11 C12 C14 180.0(4) . . . 2_677 ?
C7 C11 C14 O1B -1.1(12) . . . . ?
C7 C11 C14 C12 -180.0(4) . . . 2_677 ?
C8 C1 C4 O2 5.6(6) . . . . ?
C8 C1 C4 O4 -174.1(4) . . . . ?
C9 C1 C4 O2 -171.7(4) 2_556 . . . ?
C9 C1 C4 O4 8.5(7) 2_556 . . . ?
C9 C1 C8 C9 -0.8(8) 2_556 . . . ?
C12 C11 C14 O1B 179.3(12) . . . . ?
C12 C11 C14 C12 0.4(8) . . . 2_677 ?
C14 C11 C12 O1A 178.3(5) . . . . ?
C14 C11 C12 C14 -0.4(7) . . . 2_677 ?
C15 N1 C10 O5 179.8(5) . . . . ?
C16 N1 C10 O5 2.9(9) . . . . ?
C17 N2 C13 O11 0.7(9) . . . . ?
C18 N2 C13 O11 178.5(6) . . . . ?
C2A N3 C1A O10 -177.9(10) . . . . ?
C3A N3 C1A O10 -2.4(15) . . . . ?
C2B N3 C1B O10 -10(2) . . . . ?
C3B N3 C1B O10 177.2(15) . . . . ?

_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 1.128
_oxdiff_exptl_absorpt_empirical_full_min 0.872

# start Validation Reply Form
_vrf_PLAT029_SION2_100K          
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.714 Why?  
RESPONSE: The data were collected upon the spindle rotation. Therefore, a 
		  limited portion of the reciprocal space could be probed.
;
# 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_SION2_120K
_database_code_depnum_ccdc_archive 'CCDC 1871305'
loop_
_audit_author_name
_audit_author_address
'Andrzej Gladysiak'
;Ecole polytechnique f?d?rale de Lausanne
Switzerland
;
_audit_update_record             
;
2018-10-03 deposited with the CCDC.	2019-08-12 downloaded from the CCDC.
;
_audit_creation_date             2018-07-09
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_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          ?
_chemical_oxdiff_formula         'C21 H27 N3 O12 Tb'
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                   10.5156(6)
_cell_length_b                   10.9858(4)
_cell_length_c                   12.5290(6)
_cell_angle_alpha                104.707(4)
_cell_angle_beta                 107.578(5)
_cell_angle_gamma                97.265(4)
_cell_volume                     1301.80(12)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5160
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      31.4680
_cell_measurement_theta_min      1.9480
_shelx_estimated_absorpt_T_max   0.829
_shelx_estimated_absorpt_T_min   0.606
_exptl_absorpt_coefficient_mu    2.782
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81926
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.715
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             670
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0166
_diffrn_reflns_av_unetI/netI     0.0250
_diffrn_reflns_Laue_measured_fraction_full 0.716
_diffrn_reflns_Laue_measured_fraction_max 0.654
_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       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8235
_diffrn_reflns_point_group_measured_fraction_full 0.716
_diffrn_reflns_point_group_measured_fraction_max 0.654
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.426
_diffrn_reflns_theta_min         1.974
_diffrn_ambient_temperature      120.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            PILATUS2M
_diffrn_measured_fraction_theta_full 0.716
_diffrn_measured_fraction_theta_max 0.654
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      0.00 360.00   1.00    1.00    --    0.00   0.00   0.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  PILATUS@SNBL
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0598284000
_diffrn_orient_matrix_UB_12      -0.0136848000
_diffrn_orient_matrix_UB_13      0.0361699000
_diffrn_orient_matrix_UB_21      -0.0285537000
_diffrn_orient_matrix_UB_22      -0.0675335000
_diffrn_orient_matrix_UB_23      -0.0271222000
_diffrn_orient_matrix_UB_31      0.0306586000
_diffrn_orient_matrix_UB_32      -0.0000295000
_diffrn_orient_matrix_UB_33      -0.0436884000
_diffrn_radiation_monochromator  'Si (111)'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           ?
_diffrn_radiation_wavelength     0.7142
_diffrn_source                   
'European Synchrotron Radiation Facility, BM01 beamline'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3969
_reflns_number_total             4216
_reflns_odcompleteness_completeness 70.54
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.51
_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 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (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    'XT (Sheldrick, 2015)'
_refine_diff_density_max         1.516
_refine_diff_density_min         -1.404
_refine_diff_density_rms         0.108
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         4216
_refine_ls_number_restraints     73
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0309
_refine_ls_restrained_S_all      1.107
_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)+(0.0695P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0886
_refine_ls_wR_factor_ref         0.0896
_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 planarity
 O1B, C14, C11, C12, O8, C7, O7
 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
O3 \\sim C2: within 2A with sigma of 0.002 and sigma for terminal atoms of 0.004
4. Rigid body (RIGU) restrains
 C1A, N3, C2A, C3A, O10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O10, C1B, N3, C3B, C2B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O3, C2, O6, C3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. 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)
6.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C8(H8), C10(H10), C12(H12A), C13(H13), C14(H14), C1A(H1AA), C1B(H1BA)
6.b Tetrahedral OH refined with riding coordinates:
 O1B(H1B)
6.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)
6.d Idealised tetrahedral OH refined as rotating group:
 O9(H9), O12(H12), O1A(H1A)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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 0.09500(2) 0.54663(2) 0.68273(2) 0.02506(10) Uani 1 1 d . . . . .
O2 O -0.0353(3) 0.3348(2) 0.5868(3) 0.0277(6) Uani 1 1 d . . . . .
O3 O 0.1547(3) 0.4857(3) 0.5161(3) 0.0298(6) Uani 1 1 d . U . . .
O4 O -0.0816(3) 0.2731(2) 0.3920(2) 0.0310(7) Uani 1 1 d . . . . .
O5 O 0.0572(3) 0.4845(3) 0.8411(3) 0.0367(7) Uani 1 1 d . . . . .
O6 O 0.1298(3) 0.4231(3) 0.3285(3) 0.0320(7) Uani 1 1 d . U . . .
O7 O 0.1650(3) 0.7632(3) 0.8508(3) 0.0340(7) Uani 1 1 d . . . . .
O8 O 0.3201(3) 0.6809(3) 0.7867(3) 0.0358(7) Uani 1 1 d . . . . .
O9 O 0.0442(4) -0.0491(3) 0.7135(3) 0.0468(9) Uani 1 1 d . . . . .
H9 H 0.0500 -0.1260 0.7073 0.070 Uiso 1 1 calc GR . . . .
O11 O 0.2495(3) 0.4058(3) 0.7346(3) 0.0431(8) Uani 1 1 d . . . . .
O12 O 0.6598(3) 0.6062(4) 0.7369(3) 0.0473(9) Uani 1 1 d . . . . .
H12 H 0.7420 0.6032 0.7481 0.071 Uiso 1 1 calc GR . . . .
N1 N -0.0130(4) 0.3084(4) 0.8911(4) 0.0392(9) Uani 1 1 d . . . . .
O1A O 0.2343(4) 1.0051(3) 0.9936(4) 0.0394(12) Uani 0.865(10) 1 d . . P A 1
H1A H 0.1802 0.9342 0.9514 0.059 Uiso 0.865(10) 1 calc GR . P A 1
O1B O 0.594(3) 0.801(2) 0.8769(19) 0.061(11) Uani 0.135(10) 1 d . . P A 2
H1B H 0.5340 0.7337 0.8339 0.092 Uiso 0.135(10) 1 calc R . P A 2
N2 N 0.4286(4) 0.3325(4) 0.8312(4) 0.0446(10) Uani 1 1 d . . . . .
C1 C -0.0264(4) 0.1205(3) 0.4930(4) 0.0290(9) Uani 1 1 d . . . . .
C2 C 0.2054(4) 0.4629(4) 0.4373(4) 0.0294(8) Uani 1 1 d . U . . .
C3 C 0.3576(4) 0.4814(4) 0.4674(4) 0.0296(9) Uani 1 1 d . U . . .
C4 C -0.0487(4) 0.2529(3) 0.4906(4) 0.0279(9) Uani 1 1 d . . . . .
C5 C 0.4417(4) 0.5356(4) 0.5864(4) 0.0343(10) Uani 1 1 d . . . . .
H5 H 0.4021 0.5609 0.6451 0.041 Uiso 1 1 calc R . . . .
C6 C 0.5839(5) 0.5524(4) 0.6183(4) 0.0330(10) Uani 1 1 d . . . . .
C7 C 0.2873(4) 0.7724(4) 0.8499(4) 0.0300(9) Uani 1 1 d . . . . .
C8 C -0.0026(5) 0.0912(4) 0.5973(4) 0.0330(9) Uani 1 1 d . . . . .
H8 H -0.0039 0.1539 0.6647 0.040 Uiso 1 1 calc R . . . .
C9 C 0.0234(5) -0.0288(4) 0.6060(4) 0.0312(9) Uani 1 1 d . . . . .
C10 C -0.0327(5) 0.3877(4) 0.8280(4) 0.0401(11) Uani 1 1 d . . . . .
H10 H -0.1197 0.3717 0.7687 0.048 Uiso 1 1 calc R . . . .
N3 N 0.4764(5) 0.1528(4) 0.4541(5) 0.0523(11) Uani 1 1 d . U . . .
C11 C 0.3967(4) 0.8913(3) 0.9287(3) 0.0287(9) Uani 1 1 d . . . . .
C12 C 0.3641(4) 0.9983(4) 0.9948(4) 0.0330(10) Uani 1 1 d . . . . .
H12A H 0.2723 0.9976 0.9907 0.040 Uiso 0.135(10) 1 calc R . P A 2
C13 C 0.3702(5) 0.4232(5) 0.7954(4) 0.0411(11) Uani 1 1 d . . . . .
H13 H 0.4260 0.5070 0.8187 0.049 Uiso 1 1 calc R . . . .
C14 C 0.5313(4) 0.8939(4) 0.9331(4) 0.0296(9) Uani 1 1 d . . . . .
H14 H 0.5520 0.8217 0.8865 0.036 Uiso 0.865(10) 1 calc R . P A 1
C15 C -0.1234(6) 0.1980(5) 0.8720(6) 0.0539(14) Uani 1 1 d . . . . .
H15A H -0.1547 0.2140 0.9395 0.081 Uiso 1 1 calc GR . . . .
H15B H -0.0883 0.1189 0.8637 0.081 Uiso 1 1 calc GR . . . .
H15C H -0.2000 0.1882 0.8003 0.081 Uiso 1 1 calc GR . . . .
O10 O 0.6042(7) 0.2227(6) 0.6485(5) 0.0896(17) Uani 1 1 d . U . . .
C16 C 0.1124(7) 0.3274(6) 0.9890(6) 0.0644(17) Uani 1 1 d . . . . .
H16A H 0.1767 0.4049 0.9972 0.097 Uiso 1 1 calc GR . . . .
H16B H 0.1532 0.2523 0.9742 0.097 Uiso 1 1 calc GR . . . .
H16C H 0.0918 0.3379 1.0616 0.097 Uiso 1 1 calc GR . . . .
C17 C 0.3520(7) 0.2002(5) 0.7983(6) 0.0578(15) Uani 1 1 d . . . . .
H17A H 0.3304 0.1860 0.8656 0.087 Uiso 1 1 calc GR . . . .
H17B H 0.4072 0.1401 0.7750 0.087 Uiso 1 1 calc GR . . . .
H17C H 0.2669 0.1858 0.7323 0.087 Uiso 1 1 calc GR . . . .
C18 C 0.5733(7) 0.3637(7) 0.9021(6) 0.0667(17) Uani 1 1 d . . . . .
H18A H 0.6202 0.3057 0.8627 0.100 Uiso 1 1 calc GR . . . .
H18B H 0.5840 0.3534 0.9796 0.100 Uiso 1 1 calc GR . . . .
H18C H 0.6132 0.4532 0.9118 0.100 Uiso 1 1 calc GR . . . .
C1A C 0.5938(11) 0.1924(10) 0.5440(9) 0.060(2) Uani 0.630(9) 1 d . U P B 1
H1AA H 0.6759 0.1979 0.5267 0.073 Uiso 0.630(9) 1 calc R . P B 1
C2A C 0.4685(14) 0.1133(13) 0.3311(11) 0.072(3) Uani 0.630(9) 1 d . U P B 1
H2AA H 0.5598 0.1364 0.3273 0.109 Uiso 0.630(9) 1 calc GR . P B 1
H2AB H 0.4067 0.1573 0.2869 0.109 Uiso 0.630(9) 1 calc GR . P B 1
H2AC H 0.4337 0.0197 0.2968 0.109 Uiso 0.630(9) 1 calc GR . P B 1
C3A C 0.3441(12) 0.1380(12) 0.4742(11) 0.070(3) Uani 0.630(9) 1 d . U P B 1
H3AA H 0.2862 0.0531 0.4246 0.105 Uiso 0.630(9) 1 calc GR . P B 1
H3AB H 0.2980 0.2055 0.4542 0.105 Uiso 0.630(9) 1 calc GR . P B 1
H3AC H 0.3608 0.1456 0.5572 0.105 Uiso 0.630(9) 1 calc GR . P B 1
C1B C 0.489(2) 0.198(2) 0.5640(17) 0.072(5) Uani 0.370(9) 1 d . U P B 2
H1BA H 0.4106 0.2124 0.5828 0.087 Uiso 0.370(9) 1 calc R . P B 2
C2B C 0.599(2) 0.144(2) 0.4238(19) 0.072(5) Uani 0.370(9) 1 d . U P B 2
H2BA H 0.6778 0.2039 0.4875 0.109 Uiso 0.370(9) 1 calc GR . P B 2
H2BB H 0.5875 0.1654 0.3509 0.109 Uiso 0.370(9) 1 calc GR . P B 2
H2BC H 0.6126 0.0554 0.4127 0.109 Uiso 0.370(9) 1 calc GR . P B 2
C3B C 0.344(2) 0.123(2) 0.3577(19) 0.076(5) Uani 0.370(9) 1 d . U P B 2
H3BA H 0.2726 0.1407 0.3907 0.114 Uiso 0.370(9) 1 calc GR . P B 2
H3BB H 0.3221 0.0311 0.3119 0.114 Uiso 0.370(9) 1 calc GR . P B 2
H3BC H 0.3497 0.1756 0.3065 0.114 Uiso 0.370(9) 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 2.349(3) . ?
Tb1 O3 2.321(3) . ?
Tb1 O4 2.399(3) 2_566 ?
Tb1 O5 2.379(3) . ?
Tb1 O6 2.396(3) 2_566 ?
Tb1 O7 2.591(3) . ?
Tb1 O8 2.399(3) . ?
Tb1 O11 2.442(3) . ?
O2 C4 1.264(5) . ?
O3 C2 1.244(6) . ?
O4 Tb1 2.399(3) 2_566 ?
O4 C4 1.263(5) . ?
O5 C10 1.270(6) . ?
O6 Tb1 2.396(3) 2_566 ?
O6 C2 1.279(5) . ?
O7 C7 1.281(6) . ?
O8 C7 1.267(5) . ?
O9 H9 0.8400 . ?
O9 C9 1.378(6) . ?
O11 C13 1.228(6) . ?
O12 H12 0.8400 . ?
O12 C6 1.383(5) . ?
N1 C10 1.313(6) . ?
N1 C15 1.484(7) . ?
N1 C16 1.453(7) . ?
O1A H1A 0.8400 . ?
O1A C12 1.372(6) . ?
O1B H1B 0.8400 . ?
O1B C14 1.43(2) . ?
N2 C13 1.336(6) . ?
N2 C17 1.459(7) . ?
N2 C18 1.456(7) . ?
C1 C4 1.508(5) . ?
C1 C8 1.382(6) . ?
C1 C9 1.397(6) 2_556 ?
C2 C3 1.503(6) . ?
C3 C5 1.407(6) . ?
C3 C6 1.388(7) 2_666 ?
C5 H5 0.9500 . ?
C5 C6 1.400(6) . ?
C6 C3 1.388(7) 2_666 ?
C7 C11 1.511(5) . ?
C8 H8 0.9500 . ?
C8 C9 1.404(5) . ?
C9 C1 1.397(6) 2_556 ?
C10 H10 0.9500 . ?
N3 C1A 1.326(11) . ?
N3 C2A 1.464(13) . ?
N3 C3A 1.484(13) . ?
N3 C1B 1.30(2) . ?
N3 C2B 1.45(2) . ?
N3 C3B 1.47(2) . ?
C11 C12 1.402(6) . ?
C11 C14 1.396(6) . ?
C12 H12A 0.9500 . ?
C12 C14 1.399(5) 2_677 ?
C13 H13 0.9500 . ?
C14 C12 1.399(5) 2_677 ?
C14 H14 0.9500 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
O10 C1A 1.232(12) . ?
O10 C1B 1.28(2) . ?
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 126.84(9) . 2_566 ?
O2 Tb1 O5 78.07(10) . . ?
O2 Tb1 O6 78.75(10) . 2_566 ?
O2 Tb1 O7 151.31(10) . . ?
O2 Tb1 O8 146.01(10) . . ?
O2 Tb1 O11 74.06(10) . . ?
O3 Tb1 O2 77.28(10) . . ?
O3 Tb1 O4 75.95(10) . 2_566 ?
O3 Tb1 O5 145.80(10) . . ?
O3 Tb1 O6 122.04(10) . 2_566 ?
O3 Tb1 O7 131.29(10) . . ?
O3 Tb1 O8 88.86(11) . . ?
O3 Tb1 O11 78.31(12) . . ?
O4 Tb1 O7 68.28(10) 2_566 . ?
O4 Tb1 O11 140.88(12) 2_566 . ?
O5 Tb1 O4 138.23(11) . 2_566 ?
O5 Tb1 O6 75.21(11) . 2_566 ?
O5 Tb1 O7 76.65(10) . . ?
O5 Tb1 O8 98.71(11) . . ?
O5 Tb1 O11 72.37(12) . . ?
O6 Tb1 O4 77.98(10) 2_566 2_566 ?
O6 Tb1 O7 81.87(10) 2_566 . ?
O6 Tb1 O8 133.73(10) 2_566 . ?
O6 Tb1 O11 141.11(11) 2_566 . ?
O8 Tb1 O4 77.73(10) . 2_566 ?
O8 Tb1 O7 52.60(11) . . ?
O8 Tb1 O11 72.79(11) . . ?
O11 Tb1 O7 110.39(11) . . ?
C4 O2 Tb1 132.4(3) . . ?
C2 O3 Tb1 170.8(3) . . ?
C4 O4 Tb1 138.2(2) . 2_566 ?
C10 O5 Tb1 124.1(3) . . ?
C2 O6 Tb1 107.5(3) . 2_566 ?
C7 O7 Tb1 88.4(2) . . ?
C7 O8 Tb1 97.6(2) . . ?
C9 O9 H9 109.5 . . ?
C13 O11 Tb1 134.9(3) . . ?
C6 O12 H12 109.5 . . ?
C10 N1 C15 121.4(4) . . ?
C10 N1 C16 122.9(4) . . ?
C16 N1 C15 115.5(4) . . ?
C12 O1A H1A 109.5 . . ?
C14 O1B H1B 109.5 . . ?
C13 N2 C17 121.8(4) . . ?
C13 N2 C18 119.9(5) . . ?
C18 N2 C17 118.3(4) . . ?
C8 C1 C4 119.0(4) . . ?
C8 C1 C9 119.2(4) . 2_556 ?
C9 C1 C4 121.7(4) 2_556 . ?
O3 C2 O6 121.1(4) . . ?
O3 C2 C3 120.8(4) . . ?
O6 C2 C3 118.1(4) . . ?
C5 C3 C2 118.3(4) . . ?
C6 C3 C2 122.0(4) 2_666 . ?
C6 C3 C5 119.8(4) 2_666 . ?
O2 C4 C1 117.8(4) . . ?
O4 C4 O2 124.8(3) . . ?
O4 C4 C1 117.5(4) . . ?
C3 C5 H5 120.0 . . ?
C6 C5 C3 120.0(5) . . ?
C6 C5 H5 120.0 . . ?
O12 C6 C3 123.1(4) . 2_666 ?
O12 C6 C5 116.6(4) . . ?
C3 C6 C5 120.2(4) 2_666 . ?
O7 C7 C11 120.2(4) . . ?
O8 C7 O7 121.0(3) . . ?
O8 C7 C11 118.8(4) . . ?
C1 C8 H8 119.2 . . ?
C1 C8 C9 121.7(4) . . ?
C9 C8 H8 119.2 . . ?
O9 C9 C1 123.7(4) . 2_556 ?
O9 C9 C8 117.2(4) . . ?
C1 C9 C8 119.1(4) 2_556 . ?
O5 C10 N1 124.2(4) . . ?
O5 C10 H10 117.9 . . ?
N1 C10 H10 117.9 . . ?
C1A N3 C2A 123.1(8) . . ?
C1A N3 C3A 120.7(8) . . ?
C2A N3 C3A 116.1(8) . . ?
C1B N3 C2B 118.9(14) . . ?
C1B N3 C3B 122.6(14) . . ?
C2B N3 C3B 118.3(13) . . ?
C12 C11 C7 121.0(4) . . ?
C14 C11 C7 118.8(4) . . ?
C14 C11 C12 120.3(3) . . ?
O1A C12 C11 124.1(4) . . ?
O1A C12 C14 116.9(4) . 2_677 ?
C11 C12 H12A 120.5 . . ?
C14 C12 C11 119.0(4) 2_677 . ?
C14 C12 H12A 120.5 2_677 . ?
O11 C13 N2 124.7(5) . . ?
O11 C13 H13 117.6 . . ?
N2 C13 H13 117.6 . . ?
O1B C14 C11 132.5(11) . . ?
O1B C14 C12 106.8(11) . 2_677 ?
C11 C14 C12 120.7(4) . 2_677 ?
C11 C14 H14 119.6 . . ?
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 117.6 . . ?
O10 C1A N3 124.8(10) . . ?
O10 C1A H1AA 117.6 . . ?
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 118.6 . . ?
O10 C1B N3 122.9(18) . . ?
O10 C1B H1BA 118.6 . . ?
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 -53.9(6) . . . . ?
Tb1 O2 C4 C1 127.3(3) . . . . ?
Tb1 O4 C4 O2 15.1(7) 2_566 . . . ?
Tb1 O4 C4 C1 -166.1(3) 2_566 . . . ?
Tb1 O5 C10 N1 139.2(4) . . . . ?
Tb1 O6 C2 O3 13.0(4) 2_566 . . . ?
Tb1 O6 C2 C3 -167.1(3) 2_566 . . . ?
Tb1 O7 C7 O8 -6.4(4) . . . . ?
Tb1 O7 C7 C11 176.1(3) . . . . ?
Tb1 O8 C7 O7 7.0(4) . . . . ?
Tb1 O8 C7 C11 -175.5(3) . . . . ?
Tb1 O11 C13 N2 166.0(4) . . . . ?
O3 C2 C3 C5 -5.5(6) . . . . ?
O3 C2 C3 C6 175.1(4) . . . 2_666 ?
O6 C2 C3 C5 174.6(4) . . . . ?
O6 C2 C3 C6 -4.8(6) . . . 2_666 ?
O7 C7 C11 C12 -6.5(6) . . . . ?
O7 C7 C11 C14 174.7(4) . . . . ?
O8 C7 C11 C12 176.0(4) . . . . ?
O8 C7 C11 C14 -2.8(6) . . . . ?
C1 C8 C9 O9 -179.3(4) . . . . ?
C1 C8 C9 C1 0.5(7) . . . 2_556 ?
C2 C3 C5 C6 178.9(4) . . . . ?
C3 C5 C6 O12 -179.9(4) . . . . ?
C3 C5 C6 C3 1.6(7) . . . 2_666 ?
C4 C1 C8 C9 -177.8(4) . . . . ?
C6 C3 C5 C6 -1.6(7) 2_666 . . . ?
C7 C11 C12 O1A -0.4(7) . . . . ?
C7 C11 C12 C14 179.8(4) . . . 2_677 ?
C7 C11 C14 O1B -1.5(11) . . . . ?
C7 C11 C14 C12 -179.7(4) . . . 2_677 ?
C8 C1 C4 O2 4.7(6) . . . . ?
C8 C1 C4 O4 -174.1(4) . . . . ?
C9 C1 C4 O2 -172.5(4) 2_556 . . . ?
C9 C1 C4 O4 8.6(6) 2_556 . . . ?
C9 C1 C8 C9 -0.5(7) 2_556 . . . ?
C12 C11 C14 O1B 179.6(11) . . . . ?
C12 C11 C14 C12 1.4(7) . . . 2_677 ?
C14 C11 C12 O1A 178.4(4) . . . . ?
C14 C11 C12 C14 -1.4(7) . . . 2_677 ?
C15 N1 C10 O5 179.2(5) . . . . ?
C16 N1 C10 O5 4.0(9) . . . . ?
C17 N2 C13 O11 1.1(8) . . . . ?
C18 N2 C13 O11 179.3(6) . . . . ?
C2A N3 C1A O10 -177.7(10) . . . . ?
C3A N3 C1A O10 -1.9(15) . . . . ?
C2B N3 C1B O10 -7(3) . . . . ?
C3B N3 C1B O10 179.1(15) . . . . ?

_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 1.136
_oxdiff_exptl_absorpt_empirical_full_min 0.895

# start Validation Reply Form
_vrf_PLAT029_SION2_120K          
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.716 Why?  
RESPONSE: The data were collected upon the spindle rotation. Therefore, a 
		  limited portion of the reciprocal space could be probed.
;
# 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_SION2_200K
_database_code_depnum_ccdc_archive 'CCDC 1871304'
loop_
_audit_author_name
_audit_author_address
'Andrzej Gladysiak'
;Ecole polytechnique f?d?rale de Lausanne
Switzerland
;
_audit_update_record             
;
2018-10-03 deposited with the CCDC.	2019-08-12 downloaded from the CCDC.
;
_audit_creation_date             2018-07-09
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_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          ?
_chemical_oxdiff_formula         'C21 H27 N3 O12 Tb'
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                   10.5213(5)
_cell_length_b                   10.9954(5)
_cell_length_c                   12.6323(5)
_cell_angle_alpha                104.438(4)
_cell_angle_beta                 108.872(4)
_cell_angle_gamma                96.664(4)
_cell_volume                     1307.93(11)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5749
_cell_measurement_temperature    200.0
_cell_measurement_theta_max      31.7660
_cell_measurement_theta_min      1.9570
_shelx_estimated_absorpt_T_max   0.830
_shelx_estimated_absorpt_T_min   0.607
_exptl_absorpt_coefficient_mu    2.769
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80216
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.707
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             670
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0172
_diffrn_reflns_av_unetI/netI     0.0249
_diffrn_reflns_Laue_measured_fraction_full 0.747
_diffrn_reflns_Laue_measured_fraction_max 0.681
_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       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8611
_diffrn_reflns_point_group_measured_fraction_full 0.747
_diffrn_reflns_point_group_measured_fraction_max 0.681
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.425
_diffrn_reflns_theta_min         1.968
_diffrn_ambient_temperature      200.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            PILATUS2M
_diffrn_measured_fraction_theta_full 0.747
_diffrn_measured_fraction_theta_max 0.681
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      0.00 360.00   1.00    1.00    --    0.00   0.00   0.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  PILATUS@SNBL
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0603422000
_diffrn_orient_matrix_UB_12      -0.0139778000
_diffrn_orient_matrix_UB_13      0.0367913000
_diffrn_orient_matrix_UB_21      -0.0287492000
_diffrn_orient_matrix_UB_22      -0.0672353000
_diffrn_orient_matrix_UB_23      -0.0270670000
_diffrn_orient_matrix_UB_31      0.0304491000
_diffrn_orient_matrix_UB_32      -0.0002229000
_diffrn_orient_matrix_UB_33      -0.0430178000
_diffrn_radiation_monochromator  'Si (111)'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           ?
_diffrn_radiation_wavelength     0.7142
_diffrn_source                   
'European Synchrotron Radiation Facility, BM01 beamline'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4215
_reflns_number_total             4413
_reflns_odcompleteness_completeness 73.48
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.51
_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 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (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    'XT (Sheldrick, 2015)'
_refine_diff_density_max         1.162
_refine_diff_density_min         -1.452
_refine_diff_density_rms         0.101
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         4413
_refine_ls_number_restraints     58
_refine_ls_R_factor_all          0.0300
_refine_ls_R_factor_gt           0.0288
_refine_ls_restrained_S_all      1.073
_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)+(0.0600P)²+0.4583P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0784
_refine_ls_wR_factor_ref         0.0792
_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. Rigid bond restraints
 O3, C2
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.005
3. Uiso/Uaniso restraints and constraints
O3 \\sim C2: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.01
Uanis(O1B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C1A, N3, C2A, C3A, O10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O10, C1B, N3, C3B, C2B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. 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)
6.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C8(H8), C10(H10), C12(H12A), C13(H13), C14(H14), C1A(H1AA), C1B(H1BA)
6.b Tetrahedral OH refined with riding coordinates:
 O1B(H1B)
6.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)
6.d Idealised tetrahedral OH refined as rotating group:
 O9(H9), O12(H12), O1A(H1A)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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 0.09897(2) 0.54735(2) 0.68294(2) 0.02660(9) Uani 1 1 d . . . . .
O2 O -0.0265(3) 0.3354(2) 0.5875(2) 0.0332(6) Uani 1 1 d . . . . .
O3 O 0.1581(3) 0.4899(2) 0.5197(3) 0.0353(5) Uani 1 1 d . U . . .
O4 O -0.0764(3) 0.2747(2) 0.3930(2) 0.0363(6) Uani 1 1 d . . . . .
O5 O 0.0633(3) 0.4831(3) 0.8402(2) 0.0428(7) Uani 1 1 d . . . . .
O6 O 0.1277(3) 0.4271(3) 0.3315(2) 0.0377(6) Uani 1 1 d . . . . .
O7 O 0.1696(3) 0.7597(2) 0.8502(2) 0.0372(6) Uani 1 1 d . . . . .
O8 O 0.3241(3) 0.6843(3) 0.7844(3) 0.0455(7) Uani 1 1 d . . . . .
O9 O 0.0453(5) -0.0498(3) 0.7116(3) 0.0600(10) Uani 1 1 d . . . . .
H9 H 0.0466 -0.1277 0.7044 0.090 Uiso 1 1 calc GR . . . .
O11 O 0.2588(3) 0.4121(3) 0.7395(3) 0.0579(9) Uani 1 1 d . . . . .
O12 O 0.6663(3) 0.6027(4) 0.7355(3) 0.0559(9) Uani 1 1 d . . . . .
H12 H 0.7491 0.6028 0.7452 0.084 Uiso 1 1 calc GR . . . .
N1 N -0.0072(5) 0.3118(4) 0.8924(4) 0.0518(10) Uani 1 1 d . . . . .
O1A O 0.2355(3) 0.9968(3) 0.9969(3) 0.0472(11) Uani 0.884(10) 1 d . . P A 1
H1A H 0.1803 0.9293 0.9486 0.071 Uiso 0.884(10) 1 calc GR . P A 1
O1B O 0.593(3) 0.804(2) 0.882(3) 0.060(10) Uani 0.116(10) 1 d . U P A 2
H1B H 0.5316 0.7375 0.8396 0.091 Uiso 0.116(10) 1 calc R . P A 2
N2 N 0.4329(5) 0.3310(5) 0.8316(4) 0.0643(12) Uani 1 1 d . . . . .
C1 C -0.0236(4) 0.1209(3) 0.4934(3) 0.0322(8) Uani 1 1 d . . . . .
C2 C 0.2061(4) 0.4657(3) 0.4396(4) 0.0338(6) Uani 1 1 d . U . . .
C3 C 0.3580(4) 0.4828(3) 0.4683(3) 0.0332(9) Uani 1 1 d . . . . .
C4 C -0.0435(4) 0.2536(3) 0.4909(3) 0.0316(8) Uani 1 1 d . . . . .
C5 C 0.4452(4) 0.5350(4) 0.5868(3) 0.0375(9) Uani 1 1 d . . . . .
H5 H 0.4073 0.5591 0.6458 0.045 Uiso 1 1 calc R . . . .
C6 C 0.5870(4) 0.5515(4) 0.6181(3) 0.0366(9) Uani 1 1 d . . . . .
C7 C 0.2912(4) 0.7719(3) 0.8490(3) 0.0334(8) Uani 1 1 d . . . . .
C8 C -0.0006(4) 0.0907(3) 0.5970(4) 0.0394(9) Uani 1 1 d . . . . .
H8 H -0.0012 0.1533 0.6639 0.047 Uiso 1 1 calc R . . . .
C9 C 0.0234(5) -0.0291(3) 0.6059(3) 0.0380(9) Uani 1 1 d . . . . .
C10 C -0.0261(5) 0.3885(4) 0.8264(4) 0.0470(11) Uani 1 1 d . . . . .
H10 H -0.1127 0.3712 0.7645 0.056 Uiso 1 1 calc R . . . .
N3 N 0.4779(6) 0.1532(5) 0.4536(5) 0.0795(14) Uani 1 1 d . U . . .
C11 C 0.3981(4) 0.8909(3) 0.9276(3) 0.0336(8) Uani 1 1 d . . . . .
C12 C 0.3640(4) 0.9940(3) 0.9958(4) 0.0360(9) Uani 1 1 d . . . . .
H12A H 0.2722 0.9904 0.9927 0.043 Uiso 0.116(10) 1 calc R . P A 2
C13 C 0.3771(5) 0.4237(6) 0.7976(5) 0.0585(13) Uani 1 1 d . . . . .
H13 H 0.4358 0.5058 0.8214 0.070 Uiso 1 1 calc R . . . .
C14 C 0.5327(4) 0.8978(3) 0.9317(3) 0.0364(9) Uani 1 1 d . . . . .
H14 H 0.5545 0.8279 0.8844 0.044 Uiso 0.884(10) 1 calc R . P A 1
C15 C -0.1158(8) 0.2042(6) 0.8737(7) 0.0804(19) Uani 1 1 d . . . . .
H15A H -0.1365 0.2146 0.9452 0.121 Uiso 1 1 calc GR . . . .
H15B H -0.0850 0.1235 0.8547 0.121 Uiso 1 1 calc GR . . . .
H15C H -0.1986 0.2023 0.8085 0.121 Uiso 1 1 calc GR . . . .
O10 O 0.6112(8) 0.2268(8) 0.6457(6) 0.123(2) Uani 1 1 d . U . . .
C16 C 0.1191(8) 0.3307(7) 0.9899(6) 0.094(2) Uani 1 1 d . . . . .
H16A H 0.1688 0.4203 1.0159 0.141 Uiso 1 1 calc GR . . . .
H16B H 0.1761 0.2736 0.9653 0.141 Uiso 1 1 calc GR . . . .
H16C H 0.0982 0.3110 1.0547 0.141 Uiso 1 1 calc GR . . . .
C17 C 0.3604(9) 0.2010(8) 0.8007(8) 0.109(3) Uani 1 1 d . . . . .
H17A H 0.3494 0.1845 0.8704 0.163 Uiso 1 1 calc GR . . . .
H17B H 0.4125 0.1419 0.7708 0.163 Uiso 1 1 calc GR . . . .
H17C H 0.2696 0.1877 0.7400 0.163 Uiso 1 1 calc GR . . . .
C18 C 0.5802(8) 0.3626(9) 0.9018(8) 0.110(3) Uani 1 1 d . . . . .
H18A H 0.6257 0.3022 0.8641 0.164 Uiso 1 1 calc GR . . . .
H18B H 0.5939 0.3562 0.9806 0.164 Uiso 1 1 calc GR . . . .
H18C H 0.6197 0.4504 0.9078 0.164 Uiso 1 1 calc GR . . . .
C1A C 0.5994(17) 0.1931(14) 0.5409(14) 0.091(4) Uani 0.548(11) 1 d . U P B 1
H1AA H 0.6803 0.1960 0.5227 0.110 Uiso 0.548(11) 1 calc R . P B 1
C2A C 0.455(2) 0.1146(18) 0.3307(15) 0.112(6) Uani 0.548(11) 1 d . U P B 1
H2AA H 0.5389 0.1463 0.3192 0.168 Uiso 0.548(11) 1 calc GR . P B 1
H2AB H 0.3799 0.1505 0.2892 0.168 Uiso 0.548(11) 1 calc GR . P B 1
H2AC H 0.4301 0.0205 0.2995 0.168 Uiso 0.548(11) 1 calc GR . P B 1
C3A C 0.3473(16) 0.1420(17) 0.4781(16) 0.104(5) Uani 0.548(11) 1 d . U P B 1
H3AA H 0.3428 0.0763 0.5176 0.156 Uiso 0.548(11) 1 calc GR . P B 1
H3AB H 0.2682 0.1175 0.4039 0.156 Uiso 0.548(11) 1 calc GR . P B 1
H3AC H 0.3456 0.2249 0.5287 0.156 Uiso 0.548(11) 1 calc GR . P B 1
C1B C 0.500(2) 0.203(2) 0.5640(17) 0.105(5) Uani 0.452(11) 1 d . U P B 2
H1BA H 0.4231 0.2220 0.5837 0.126 Uiso 0.452(11) 1 calc R . P B 2
C2B C 0.600(2) 0.143(2) 0.423(2) 0.110(6) Uani 0.452(11) 1 d . U P B 2
H2BA H 0.6599 0.2281 0.4506 0.164 Uiso 0.452(11) 1 calc GR . P B 2
H2BB H 0.5718 0.1075 0.3381 0.164 Uiso 0.452(11) 1 calc GR . P B 2
H2BC H 0.6492 0.0856 0.4614 0.164 Uiso 0.452(11) 1 calc GR . P B 2
C3B C 0.346(2) 0.120(2) 0.3605(18) 0.103(6) Uani 0.452(11) 1 d . U P B 2
H3BA H 0.2789 0.1551 0.3911 0.155 Uiso 0.452(11) 1 calc GR . P B 2
H3BB H 0.3161 0.0260 0.3287 0.155 Uiso 0.452(11) 1 calc GR . P B 2
H3BC H 0.3523 0.1554 0.2982 0.155 Uiso 0.452(11) 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 2.342(2) . ?
Tb1 O3 2.304(3) . ?
Tb1 O4 2.388(2) 2_566 ?
Tb1 O5 2.388(3) . ?
Tb1 O6 2.388(3) 2_566 ?
Tb1 O7 2.567(3) . ?
Tb1 O8 2.401(3) . ?
Tb1 O11 2.426(3) . ?
O2 C4 1.266(5) . ?
O3 C2 1.256(5) . ?
O4 Tb1 2.388(2) 2_566 ?
O4 C4 1.260(5) . ?
O5 C10 1.254(5) . ?
O6 Tb1 2.388(3) 2_566 ?
O6 C2 1.275(5) . ?
O7 C7 1.277(5) . ?
O8 C7 1.257(5) . ?
O9 H9 0.8400 . ?
O9 C9 1.361(5) . ?
O11 C13 1.196(6) . ?
O12 H12 0.8400 . ?
O12 C6 1.373(5) . ?
N1 C10 1.314(6) . ?
N1 C15 1.460(7) . ?
N1 C16 1.441(7) . ?
O1A H1A 0.8400 . ?
O1A C12 1.361(5) . ?
O1B H1B 0.8400 . ?
O1B C14 1.39(3) . ?
N2 C13 1.327(6) . ?
N2 C17 1.434(9) . ?
N2 C18 1.463(8) . ?
C1 C4 1.505(4) . ?
C1 C8 1.383(6) . ?
C1 C9 1.401(6) 2_556 ?
C2 C3 1.498(5) . ?
C3 C5 1.405(5) . ?
C3 C6 1.386(7) 2_666 ?
C5 H5 0.9500 . ?
C5 C6 1.391(6) . ?
C6 C3 1.386(7) 2_666 ?
C7 C11 1.500(4) . ?
C8 H8 0.9500 . ?
C8 C9 1.394(5) . ?
C9 C1 1.401(6) 2_556 ?
C10 H10 0.9500 . ?
N3 C1A 1.327(15) . ?
N3 C2A 1.434(18) . ?
N3 C3A 1.500(17) . ?
N3 C1B 1.29(2) . ?
N3 C2B 1.46(2) . ?
N3 C3B 1.434(18) . ?
C11 C12 1.401(6) . ?
C11 C14 1.393(6) . ?
C12 H12A 0.9500 . ?
C12 C14 1.395(5) 2_677 ?
C13 H13 0.9500 . ?
C14 C12 1.395(5) 2_677 ?
C14 H14 0.9500 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
O10 C1A 1.243(17) . ?
O10 C1B 1.23(2) . ?
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 126.50(9) . 2_566 ?
O2 Tb1 O5 77.81(9) . . ?
O2 Tb1 O6 78.85(9) . 2_566 ?
O2 Tb1 O7 151.65(10) . . ?
O2 Tb1 O8 145.64(9) . . ?
O2 Tb1 O11 74.25(11) . . ?
O3 Tb1 O2 77.33(9) . . ?
O3 Tb1 O4 76.06(9) . 2_566 ?
O3 Tb1 O5 145.94(10) . . ?
O3 Tb1 O6 122.06(9) . 2_566 ?
O3 Tb1 O7 131.00(9) . . ?
O3 Tb1 O8 87.50(10) . . ?
O3 Tb1 O11 78.97(12) . . ?
O4 Tb1 O5 137.95(10) 2_566 . ?
O4 Tb1 O6 77.43(10) 2_566 2_566 ?
O4 Tb1 O7 69.16(9) 2_566 . ?
O4 Tb1 O8 77.64(10) 2_566 . ?
O4 Tb1 O11 141.70(12) 2_566 . ?
O5 Tb1 O7 76.55(9) . . ?
O5 Tb1 O8 100.38(11) . . ?
O5 Tb1 O11 72.10(12) . . ?
O6 Tb1 O5 74.83(10) 2_566 . ?
O6 Tb1 O7 82.94(9) 2_566 . ?
O6 Tb1 O8 134.41(10) 2_566 . ?
O6 Tb1 O11 140.86(11) 2_566 . ?
O8 Tb1 O7 52.57(10) . . ?
O8 Tb1 O11 72.67(11) . . ?
O11 Tb1 O7 108.68(11) . . ?
C4 O2 Tb1 133.6(2) . . ?
C2 O3 Tb1 172.5(2) . . ?
C4 O4 Tb1 138.8(2) . 2_566 ?
C10 O5 Tb1 124.3(3) . . ?
C2 O6 Tb1 108.7(3) . 2_566 ?
C7 O7 Tb1 89.0(2) . . ?
C7 O8 Tb1 97.2(2) . . ?
C9 O9 H9 109.5 . . ?
C13 O11 Tb1 138.7(4) . . ?
C6 O12 H12 109.5 . . ?
C10 N1 C15 121.7(5) . . ?
C10 N1 C16 122.6(5) . . ?
C16 N1 C15 115.7(5) . . ?
C12 O1A H1A 109.5 . . ?
C14 O1B H1B 109.5 . . ?
C13 N2 C17 124.7(5) . . ?
C13 N2 C18 117.7(6) . . ?
C17 N2 C18 117.6(5) . . ?
C8 C1 C4 119.1(3) . . ?
C8 C1 C9 119.5(3) . 2_556 ?
C9 C1 C4 121.3(3) 2_556 . ?
O3 C2 O6 121.4(3) . . ?
O3 C2 C3 120.8(3) . . ?
O6 C2 C3 117.8(4) . . ?
C5 C3 C2 118.0(4) . . ?
C6 C3 C2 121.9(3) 2_666 . ?
C6 C3 C5 120.1(3) 2_666 . ?
O2 C4 C1 117.3(3) . . ?
O4 C4 O2 125.1(3) . . ?
O4 C4 C1 117.6(3) . . ?
C3 C5 H5 119.9 . . ?
C6 C5 C3 120.1(4) . . ?
C6 C5 H5 119.9 . . ?
O12 C6 C3 123.1(3) . 2_666 ?
O12 C6 C5 117.2(4) . . ?
C3 C6 C5 119.7(3) 2_666 . ?
O7 C7 C11 119.9(4) . . ?
O8 C7 O7 121.0(3) . . ?
O8 C7 C11 119.1(4) . . ?
C1 C8 H8 119.1 . . ?
C1 C8 C9 121.8(4) . . ?
C9 C8 H8 119.1 . . ?
O9 C9 C1 123.7(3) . 2_556 ?
O9 C9 C8 117.6(3) . . ?
C8 C9 C1 118.7(4) . 2_556 ?
O5 C10 N1 124.0(4) . . ?
O5 C10 H10 118.0 . . ?
N1 C10 H10 118.0 . . ?
C1A N3 C2A 126.0(14) . . ?
C1A N3 C3A 120.8(11) . . ?
C2A N3 C3A 113.2(12) . . ?
C1B N3 C2B 116.2(15) . . ?
C1B N3 C3B 124.9(16) . . ?
C3B N3 C2B 118.7(14) . . ?
C12 C11 C7 121.0(4) . . ?
C14 C11 C7 118.9(3) . . ?
C14 C11 C12 120.1(3) . . ?
O1A C12 C11 124.5(3) . . ?
O1A C12 C14 116.7(4) . 2_677 ?
C11 C12 H12A 120.6 . . ?
C14 C12 C11 118.8(4) 2_677 . ?
C14 C12 H12A 120.6 2_677 . ?
O11 C13 N2 125.2(6) . . ?
O11 C13 H13 117.4 . . ?
N2 C13 H13 117.4 . . ?
O1B C14 C12 108.6(11) . 2_677 ?
C11 C14 O1B 130.0(11) . . ?
C11 C14 C12 121.0(4) . 2_677 ?
C11 C14 H14 119.5 . . ?
C12 C14 H14 119.5 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 118.8 . . ?
O10 C1A N3 122.3(15) . . ?
O10 C1A H1AA 118.8 . . ?
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 117.1 . . ?
O10 C1B N3 126(2) . . ?
O10 C1B H1BA 117.1 . . ?
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 -49.6(5) . . . . ?
Tb1 O2 C4 C1 130.7(3) . . . . ?
Tb1 O4 C4 O2 10.0(7) 2_566 . . . ?
Tb1 O4 C4 C1 -170.3(3) 2_566 . . . ?
Tb1 O5 C10 N1 142.5(4) . . . . ?
Tb1 O6 C2 O3 11.1(4) 2_566 . . . ?
Tb1 O6 C2 C3 -168.2(2) 2_566 . . . ?
Tb1 O7 C7 O8 -5.4(4) . . . . ?
Tb1 O7 C7 C11 176.1(3) . . . . ?
Tb1 O8 C7 O7 5.8(4) . . . . ?
Tb1 O8 C7 C11 -175.7(3) . . . . ?
Tb1 O11 C13 N2 166.5(4) . . . . ?
O3 C2 C3 C5 -4.3(5) . . . . ?
O3 C2 C3 C6 175.5(4) . . . 2_666 ?
O6 C2 C3 C5 175.0(3) . . . . ?
O6 C2 C3 C6 -5.1(5) . . . 2_666 ?
O7 C7 C11 C12 -5.3(5) . . . . ?
O7 C7 C11 C14 175.0(3) . . . . ?
O8 C7 C11 C12 176.2(4) . . . . ?
O8 C7 C11 C14 -3.6(5) . . . . ?
C1 C8 C9 O9 179.8(4) . . . . ?
C1 C8 C9 C1 -0.2(7) . . . 2_556 ?
C2 C3 C5 C6 179.3(4) . . . . ?
C3 C5 C6 O12 -179.9(4) . . . . ?
C3 C5 C6 C3 0.6(7) . . . 2_666 ?
C4 C1 C8 C9 -177.7(4) . . . . ?
C6 C3 C5 C6 -0.6(7) 2_666 . . . ?
C7 C11 C12 O1A -0.4(6) . . . . ?
C7 C11 C12 C14 179.5(3) . . . 2_677 ?
C7 C11 C14 O1B -8(2) . . . . ?
C7 C11 C14 C12 -179.4(4) . . . 2_677 ?
C8 C1 C4 O2 5.9(5) . . . . ?
C8 C1 C4 O4 -173.8(4) . . . . ?
C9 C1 C4 O2 -172.0(4) 2_556 . . . ?
C9 C1 C4 O4 8.3(6) 2_556 . . . ?
C9 C1 C8 C9 0.2(7) 2_556 . . . ?
C12 C11 C14 O1B 173(2) . . . . ?
C12 C11 C14 C12 0.8(7) . . . 2_677 ?
C14 C11 C12 O1A 179.4(4) . . . . ?
C14 C11 C12 C14 -0.8(6) . . . 2_677 ?
C15 N1 C10 O5 178.9(5) . . . . ?
C16 N1 C10 O5 1.2(9) . . . . ?
C17 N2 C13 O11 1.9(10) . . . . ?
C18 N2 C13 O11 179.5(7) . . . . ?
C2A N3 C1A O10 179.0(13) . . . . ?
C3A N3 C1A O10 -2.5(18) . . . . ?
C2B N3 C1B O10 -9(3) . . . . ?
C3B N3 C1B O10 176.6(16) . . . . ?

_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 1.145
_oxdiff_exptl_absorpt_empirical_full_min 0.851

# start Validation Reply Form
_vrf_PLAT029_SION2_200K          
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.747 Why?  
RESPONSE: The data were collected upon the spindle rotation. Therefore, a 
		  limited portion of the reciprocal space could be probed.
;
# 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_SION2_180K
_database_code_depnum_ccdc_archive 'CCDC 1871306'
loop_
_audit_author_name
_audit_author_address
'Andrzej Gladysiak'
;Ecole polytechnique f?d?rale de Lausanne
Switzerland
;
_audit_update_record             
;
2018-10-03 deposited with the CCDC.	2019-08-12 downloaded from the CCDC.
;
_audit_creation_date             2018-07-09
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_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          ?
_chemical_oxdiff_formula         'C21 H27 N3 O12 Tb'
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                   10.5256(6)
_cell_length_b                   10.9947(5)
_cell_length_c                   12.6032(6)
_cell_angle_alpha                104.523(4)
_cell_angle_beta                 108.540(5)
_cell_angle_gamma                96.829(4)
_cell_volume                     1306.91(12)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5524
_cell_measurement_temperature    180.0
_cell_measurement_theta_max      31.7590
_cell_measurement_theta_min      1.9570
_shelx_estimated_absorpt_T_max   0.830
_shelx_estimated_absorpt_T_min   0.607
_exptl_absorpt_coefficient_mu    2.771
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81662
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.709
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             670
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0175
_diffrn_reflns_av_unetI/netI     0.0261
_diffrn_reflns_Laue_measured_fraction_full 0.736
_diffrn_reflns_Laue_measured_fraction_max 0.673
_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       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8523
_diffrn_reflns_point_group_measured_fraction_full 0.736
_diffrn_reflns_point_group_measured_fraction_max 0.673
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.433
_diffrn_reflns_theta_min         1.969
_diffrn_ambient_temperature      180.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            PILATUS2M
_diffrn_measured_fraction_theta_full 0.736
_diffrn_measured_fraction_theta_max 0.673
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      0.00 360.00   1.00    1.00    --    0.00   0.00   0.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  PILATUS@SNBL
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0602328000
_diffrn_orient_matrix_UB_12      -0.0139584000
_diffrn_orient_matrix_UB_13      0.0364861000
_diffrn_orient_matrix_UB_21      -0.0287806000
_diffrn_orient_matrix_UB_22      -0.0672994000
_diffrn_orient_matrix_UB_23      -0.0271044000
_diffrn_orient_matrix_UB_31      0.0302876000
_diffrn_orient_matrix_UB_32      -0.0001889000
_diffrn_orient_matrix_UB_33      -0.0433256000
_diffrn_radiation_monochromator  'Si (111)'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           ?
_diffrn_radiation_wavelength     0.7142
_diffrn_source                   
'European Synchrotron Radiation Facility, BM01 beamline'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4129
_reflns_number_total             4360
_reflns_odcompleteness_completeness 72.53
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.51
_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 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (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    'XT (Sheldrick, 2015)'
_refine_diff_density_max         2.068
_refine_diff_density_min         -3.813
_refine_diff_density_rms         0.157
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         4360
_refine_ls_number_restraints     58
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0430
_refine_ls_restrained_S_all      0.995
_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)+(0.1080P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1147
_refine_ls_wR_factor_ref         0.1160
_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. Rigid bond restraints
 O3, C2
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.005
3. Uiso/Uaniso restraints and constraints
O3 \\sim C2: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.01
Uanis(O1B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C1A, N3, C2A, C3A, O10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O10, C1B, N3, C3B, C2B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. 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)
6.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C8(H8), C10(H10), C12(H12A), C13(H13), C14(H14), C1A(H1AA), C1B(H1BA)
6.b Tetrahedral OH refined with riding coordinates:
 O1B(H1B)
6.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)
6.d Idealised tetrahedral OH refined as rotating group:
 O9(H9), O12(H12), O1A(H1A)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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 0.09785(2) 0.54715(2) 0.68290(2) 0.02741(13) Uani 1 1 d . . . . .
O2 O -0.0292(3) 0.3355(3) 0.5873(3) 0.0323(7) Uani 1 1 d . . . . .
O3 O 0.1574(3) 0.4885(3) 0.5186(3) 0.0345(6) Uani 1 1 d . U . . .
O4 O -0.0778(4) 0.2745(3) 0.3926(3) 0.0360(8) Uani 1 1 d . . . . .
O5 O 0.0613(4) 0.4835(3) 0.8398(3) 0.0414(8) Uani 1 1 d . . . . .
O6 O 0.1282(3) 0.4258(3) 0.3307(3) 0.0380(8) Uani 1 1 d . . . . .
O7 O 0.1680(3) 0.7608(3) 0.8504(3) 0.0378(8) Uani 1 1 d . . . . .
O8 O 0.3228(4) 0.6832(3) 0.7850(3) 0.0439(9) Uani 1 1 d . . . . .
O9 O 0.0454(6) -0.0491(4) 0.7126(4) 0.0581(13) Uani 1 1 d . . . . .
H9 H 0.0363 -0.1283 0.7042 0.087 Uiso 1 1 calc GR . . . .
O11 O 0.2560(4) 0.4102(4) 0.7390(4) 0.0556(11) Uani 1 1 d . . . . .
O12 O 0.6643(4) 0.6036(5) 0.7362(4) 0.0563(12) Uani 1 1 d . . . . .
H12 H 0.7449 0.5937 0.7477 0.084 Uiso 1 1 calc GR . . . .
N1 N -0.0088(6) 0.3100(5) 0.8916(5) 0.0488(12) Uani 1 1 d . . . . .
O1A O 0.2352(4) 0.9991(4) 0.9959(4) 0.0458(15) Uani 0.879(13) 1 d . . P A 1
H1A H 0.1823 0.9274 0.9553 0.069 Uiso 0.879(13) 1 calc GR . P A 1
O1B O 0.588(3) 0.801(3) 0.884(3) 0.056(11) Uani 0.121(13) 1 d . U P A 2
H1B H 0.5259 0.7358 0.8417 0.084 Uiso 0.121(13) 1 calc R . P A 2
N2 N 0.4321(6) 0.3322(5) 0.8313(5) 0.0578(14) Uani 1 1 d . . . . .
C1 C -0.0244(5) 0.1208(4) 0.4932(4) 0.0319(10) Uani 1 1 d . . . . .
C2 C 0.2059(5) 0.4652(4) 0.4391(5) 0.0336(7) Uani 1 1 d . U . . .
C3 C 0.3574(5) 0.4821(4) 0.4678(4) 0.0334(11) Uani 1 1 d . . . . .
C4 C -0.0451(5) 0.2534(4) 0.4907(4) 0.0317(10) Uani 1 1 d . . . . .
C5 C 0.4443(5) 0.5354(5) 0.5868(4) 0.0364(11) Uani 1 1 d . . . . .
H5 H 0.4062 0.5603 0.6458 0.044 Uiso 1 1 calc R . . . .
C6 C 0.5860(5) 0.5518(5) 0.6180(5) 0.0380(12) Uani 1 1 d . . . . .
C7 C 0.2899(5) 0.7720(4) 0.8494(4) 0.0323(10) Uani 1 1 d . . . . .
C8 C -0.0010(6) 0.0914(4) 0.5967(4) 0.0391(12) Uani 1 1 d . . . . .
H8 H -0.0016 0.1542 0.6637 0.047 Uiso 1 1 calc R . . . .
C9 C 0.0237(6) -0.0292(4) 0.6060(5) 0.0377(11) Uani 1 1 d . . . . .
C10 C -0.0289(6) 0.3887(5) 0.8277(5) 0.0483(14) Uani 1 1 d . . . . .
H10 H -0.1168 0.3735 0.7685 0.058 Uiso 1 1 calc R . . . .
N3 N 0.4779(8) 0.1531(6) 0.4543(7) 0.0747(17) Uani 1 1 d . U . . .
C11 C 0.3973(5) 0.8916(4) 0.9283(4) 0.0324(10) Uani 1 1 d . . . . .
C12 C 0.3646(5) 0.9954(5) 0.9952(5) 0.0371(11) Uani 1 1 d . . . . .
H12A H 0.2727 0.9928 0.9914 0.045 Uiso 0.121(13) 1 calc R . P A 2
C13 C 0.3750(7) 0.4235(7) 0.7977(6) 0.0519(14) Uani 1 1 d . . . . .
H13 H 0.4324 0.5064 0.8217 0.062 Uiso 1 1 calc R . . . .
C14 C 0.5325(5) 0.8964(5) 0.9319(4) 0.0344(11) Uani 1 1 d . . . . .
H14 H 0.5539 0.8259 0.8846 0.041 Uiso 0.879(13) 1 calc R . P A 1
C15 C -0.1183(10) 0.2027(8) 0.8729(8) 0.075(2) Uani 1 1 d . . . . .
H15A H -0.1406 0.2141 0.9440 0.112 Uiso 1 1 calc GR . . . .
H15B H -0.0876 0.1218 0.8551 0.112 Uiso 1 1 calc GR . . . .
H15C H -0.2000 0.2002 0.8069 0.112 Uiso 1 1 calc GR . . . .
O10 O 0.6090(9) 0.2257(10) 0.6467(7) 0.115(3) Uani 1 1 d . U . . .
C16 C 0.1171(10) 0.3290(9) 0.9891(8) 0.087(3) Uani 1 1 d . . . . .
H16A H 0.1726 0.4151 1.0084 0.131 Uiso 1 1 calc GR . . . .
H16B H 0.1684 0.2642 0.9677 0.131 Uiso 1 1 calc GR . . . .
H16C H 0.0958 0.3205 1.0575 0.131 Uiso 1 1 calc GR . . . .
C17 C 0.3580(10) 0.2013(9) 0.8004(10) 0.095(3) Uani 1 1 d . . . . .
H17A H 0.3435 0.1862 0.8695 0.142 Uiso 1 1 calc GR . . . .
H17B H 0.4112 0.1416 0.7730 0.142 Uiso 1 1 calc GR . . . .
H17C H 0.2690 0.1874 0.7377 0.142 Uiso 1 1 calc GR . . . .
C18 C 0.5781(9) 0.3615(11) 0.9034(10) 0.098(3) Uani 1 1 d . . . . .
H18A H 0.6202 0.2920 0.8740 0.148 Uiso 1 1 calc GR . . . .
H18B H 0.5888 0.3695 0.9852 0.148 Uiso 1 1 calc GR . . . .
H18C H 0.6232 0.4426 0.8994 0.148 Uiso 1 1 calc GR . . . .
C1A C 0.596(2) 0.1920(17) 0.5408(15) 0.090(4) Uani 0.597(14) 1 d . U P B 1
H1AA H 0.6766 0.1950 0.5223 0.108 Uiso 0.597(14) 1 calc R . P B 1
C2A C 0.453(3) 0.113(3) 0.3319(19) 0.119(7) Uani 0.597(14) 1 d . U P B 1
H2AA H 0.5314 0.1550 0.3178 0.178 Uiso 0.597(14) 1 calc GR . P B 1
H2AB H 0.3698 0.1375 0.2896 0.178 Uiso 0.597(14) 1 calc GR . P B 1
H2AC H 0.4422 0.0196 0.3039 0.178 Uiso 0.597(14) 1 calc GR . P B 1
C3A C 0.3466(19) 0.1403(19) 0.4789(19) 0.099(5) Uani 0.597(14) 1 d . U P B 1
H3AA H 0.2890 0.0543 0.4339 0.149 Uiso 0.597(14) 1 calc GR . P B 1
H3AB H 0.2973 0.2053 0.4557 0.149 Uiso 0.597(14) 1 calc GR . P B 1
H3AC H 0.3682 0.1532 0.5631 0.149 Uiso 0.597(14) 1 calc GR . P B 1
C1B C 0.497(4) 0.204(3) 0.561(3) 0.109(8) Uani 0.403(14) 1 d . U P B 2
H1BA H 0.4204 0.2273 0.5785 0.131 Uiso 0.403(14) 1 calc R . P B 2
C2B C 0.601(3) 0.146(3) 0.419(3) 0.110(8) Uani 0.403(14) 1 d . U P B 2
H2BA H 0.6695 0.2264 0.4620 0.164 Uiso 0.403(14) 1 calc GR . P B 2
H2BB H 0.5731 0.1323 0.3345 0.164 Uiso 0.403(14) 1 calc GR . P B 2
H2BC H 0.6397 0.0740 0.4384 0.164 Uiso 0.403(14) 1 calc GR . P B 2
C3B C 0.341(3) 0.122(3) 0.364(2) 0.096(7) Uani 0.403(14) 1 d . U P B 2
H3BA H 0.2769 0.1553 0.4003 0.144 Uiso 0.403(14) 1 calc GR . P B 2
H3BB H 0.3104 0.0288 0.3289 0.144 Uiso 0.403(14) 1 calc GR . P B 2
H3BC H 0.3434 0.1623 0.3035 0.144 Uiso 0.403(14) 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 2.342(3) . ?
Tb1 O3 2.313(4) . ?
Tb1 O4 2.388(3) 2_566 ?
Tb1 O5 2.380(4) . ?
Tb1 O6 2.390(3) 2_566 ?
Tb1 O7 2.574(3) . ?
Tb1 O8 2.399(3) . ?
Tb1 O11 2.433(4) . ?
O2 C4 1.269(6) . ?
O3 C2 1.248(7) . ?
O4 Tb1 2.388(3) 2_566 ?
O4 C4 1.261(6) . ?
O5 C10 1.266(7) . ?
O6 Tb1 2.390(3) 2_566 ?
O6 C2 1.277(6) . ?
O7 C7 1.278(6) . ?
O8 C7 1.262(6) . ?
O9 H9 0.8400 . ?
O9 C9 1.367(7) . ?
O11 C13 1.204(7) . ?
O12 H12 0.8400 . ?
O12 C6 1.380(6) . ?
N1 C10 1.315(7) . ?
N1 C15 1.463(9) . ?
N1 C16 1.442(9) . ?
O1A H1A 0.8400 . ?
O1A C12 1.370(7) . ?
O1B H1B 0.8400 . ?
O1B C14 1.36(3) . ?
N2 C13 1.321(7) . ?
N2 C17 1.446(10) . ?
N2 C18 1.462(10) . ?
C1 C4 1.506(6) . ?
C1 C8 1.376(7) . ?
C1 C9 1.397(7) 2_556 ?
C2 C3 1.496(7) . ?
C3 C5 1.410(6) . ?
C3 C6 1.388(9) 2_666 ?
C5 H5 0.9500 . ?
C5 C6 1.392(7) . ?
C6 C3 1.388(9) 2_666 ?
C7 C11 1.508(6) . ?
C8 H8 0.9500 . ?
C8 C9 1.408(6) . ?
C9 C1 1.397(7) 2_556 ?
C10 H10 0.9500 . ?
N3 C1A 1.300(18) . ?
N3 C2A 1.42(2) . ?
N3 C3A 1.51(2) . ?
N3 C1B 1.26(3) . ?
N3 C2B 1.50(3) . ?
N3 C3B 1.46(3) . ?
C11 C12 1.388(7) . ?
C11 C14 1.403(7) . ?
C12 H12A 0.9500 . ?
C12 C14 1.394(6) 2_677 ?
C13 H13 0.9500 . ?
C14 C12 1.394(6) 2_677 ?
C14 H14 0.9500 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
O10 C1A 1.249(19) . ?
O10 C1B 1.27(3) . ?
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 126.54(11) . 2_566 ?
O2 Tb1 O5 77.78(12) . . ?
O2 Tb1 O6 78.74(12) . 2_566 ?
O2 Tb1 O7 151.45(12) . . ?
O2 Tb1 O8 145.84(12) . . ?
O2 Tb1 O11 74.29(14) . . ?
O3 Tb1 O2 77.37(12) . . ?
O3 Tb1 O4 76.10(12) . 2_566 ?
O3 Tb1 O5 145.83(12) . . ?
O3 Tb1 O6 122.09(12) . 2_566 ?
O3 Tb1 O7 131.13(11) . . ?
O3 Tb1 O8 87.82(13) . . ?
O3 Tb1 O11 78.96(15) . . ?
O4 Tb1 O7 68.89(11) 2_566 . ?
O4 Tb1 O8 77.69(13) 2_566 . ?
O4 Tb1 O11 141.69(15) 2_566 . ?
O5 Tb1 O4 138.02(13) . 2_566 ?
O5 Tb1 O6 74.91(13) . 2_566 ?
O5 Tb1 O7 76.63(12) . . ?
O5 Tb1 O8 100.03(13) . . ?
O5 Tb1 O11 71.98(15) . . ?
O6 Tb1 O4 77.51(12) 2_566 2_566 ?
O6 Tb1 O7 82.55(12) 2_566 . ?
O6 Tb1 O8 134.22(12) 2_566 . ?
O6 Tb1 O11 140.80(14) 2_566 . ?
O8 Tb1 O7 52.67(13) . . ?
O8 Tb1 O11 72.72(14) . . ?
O11 Tb1 O7 109.10(14) . . ?
C4 O2 Tb1 133.2(3) . . ?
C2 O3 Tb1 172.0(3) . . ?
C4 O4 Tb1 138.8(3) . 2_566 ?
C10 O5 Tb1 125.1(4) . . ?
C2 O6 Tb1 108.4(3) . 2_566 ?
C7 O7 Tb1 88.7(3) . . ?
C7 O8 Tb1 97.2(3) . . ?
C9 O9 H9 109.5 . . ?
C13 O11 Tb1 137.6(4) . . ?
C6 O12 H12 109.5 . . ?
C10 N1 C15 121.2(6) . . ?
C10 N1 C16 122.7(6) . . ?
C16 N1 C15 116.0(6) . . ?
C12 O1A H1A 109.5 . . ?
C14 O1B H1B 109.5 . . ?
C13 N2 C17 123.5(6) . . ?
C13 N2 C18 119.8(7) . . ?
C17 N2 C18 116.7(6) . . ?
C8 C1 C4 119.0(4) . . ?
C8 C1 C9 119.6(4) . 2_556 ?
C9 C1 C4 121.3(4) 2_556 . ?
O3 C2 O6 121.3(4) . . ?
O3 C2 C3 121.0(5) . . ?
O6 C2 C3 117.8(5) . . ?
C5 C3 C2 118.0(5) . . ?
C6 C3 C2 122.4(4) 2_666 . ?
C6 C3 C5 119.6(5) 2_666 . ?
O2 C4 C1 117.5(4) . . ?
O4 C4 O2 124.8(4) . . ?
O4 C4 C1 117.7(4) . . ?
C3 C5 H5 119.9 . . ?
C6 C5 C3 120.1(5) . . ?
C6 C5 H5 119.9 . . ?
O12 C6 C3 122.9(5) . 2_666 ?
O12 C6 C5 116.8(5) . . ?
C5 C6 C3 120.3(5) . 2_666 ?
O7 C7 C11 119.7(4) . . ?
O8 C7 O7 121.1(4) . . ?
O8 C7 C11 119.2(4) . . ?
C1 C8 H8 119.1 . . ?
C1 C8 C9 121.8(5) . . ?
C9 C8 H8 119.1 . . ?
O9 C9 C1 124.1(4) . 2_556 ?
O9 C9 C8 117.3(5) . . ?
C1 C9 C8 118.6(5) 2_556 . ?
O5 C10 N1 124.3(5) . . ?
O5 C10 H10 117.9 . . ?
N1 C10 H10 117.9 . . ?
C1A N3 C2A 127.6(16) . . ?
C1A N3 C3A 120.1(13) . . ?
C2A N3 C3A 112.2(15) . . ?
C1B N3 C2B 118(2) . . ?
C1B N3 C3B 121(2) . . ?
C3B N3 C2B 120.1(19) . . ?
C12 C11 C7 121.5(4) . . ?
C12 C11 C14 120.3(4) . . ?
C14 C11 C7 118.2(4) . . ?
O1A C12 C11 124.0(4) . . ?
O1A C12 C14 116.4(5) . 2_677 ?
C11 C12 H12A 120.2 . . ?
C11 C12 C14 119.6(5) . 2_677 ?
C14 C12 H12A 120.2 2_677 . ?
O11 C13 N2 125.3(7) . . ?
O11 C13 H13 117.3 . . ?
N2 C13 H13 117.3 . . ?
O1B C14 C11 129.3(15) . . ?
O1B C14 C12 110.1(14) . 2_677 ?
C11 C14 H14 119.9 . . ?
C12 C14 C11 120.1(5) 2_677 . ?
C12 C14 H14 119.9 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 118.1 . . ?
O10 C1A N3 123.9(18) . . ?
O10 C1A H1AA 118.1 . . ?
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 O10 126(3) . . ?
N3 C1B H1BA 117.0 . . ?
O10 C1B H1BA 117.0 . . ?
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 -51.0(7) . . . . ?
Tb1 O2 C4 C1 129.6(4) . . . . ?
Tb1 O4 C4 O2 11.4(8) 2_566 . . . ?
Tb1 O4 C4 C1 -169.2(3) 2_566 . . . ?
Tb1 O5 C10 N1 140.0(5) . . . . ?
Tb1 O6 C2 O3 12.1(5) 2_566 . . . ?
Tb1 O6 C2 C3 -168.1(3) 2_566 . . . ?
Tb1 O7 C7 O8 -5.6(5) . . . . ?
Tb1 O7 C7 C11 175.9(4) . . . . ?
Tb1 O8 C7 O7 6.0(5) . . . . ?
Tb1 O8 C7 C11 -175.5(4) . . . . ?
Tb1 O11 C13 N2 167.4(5) . . . . ?
O3 C2 C3 C5 -5.3(7) . . . . ?
O3 C2 C3 C6 175.2(4) . . . 2_666 ?
O6 C2 C3 C5 174.9(4) . . . . ?
O6 C2 C3 C6 -4.6(7) . . . 2_666 ?
O7 C7 C11 C12 -5.6(7) . . . . ?
O7 C7 C11 C14 175.0(4) . . . . ?
O8 C7 C11 C12 175.8(5) . . . . ?
O8 C7 C11 C14 -3.5(7) . . . . ?
C1 C8 C9 O9 -179.8(5) . . . . ?
C1 C8 C9 C1 0.1(9) . . . 2_556 ?
C2 C3 C5 C6 179.3(5) . . . . ?
C3 C5 C6 O12 -179.5(5) . . . . ?
C3 C5 C6 C3 1.2(8) . . . 2_666 ?
C4 C1 C8 C9 -177.8(5) . . . . ?
C6 C3 C5 C6 -1.1(8) 2_666 . . . ?
C7 C11 C12 O1A 0.0(8) . . . . ?
C7 C11 C12 C14 179.2(4) . . . 2_677 ?
C7 C11 C14 O1B -8(2) . . . . ?
C7 C11 C14 C12 -179.2(4) . . . 2_677 ?
C8 C1 C4 O2 5.3(7) . . . . ?
C8 C1 C4 O4 -174.1(5) . . . . ?
C9 C1 C4 O2 -172.3(5) 2_556 . . . ?
C9 C1 C4 O4 8.2(7) 2_556 . . . ?
C9 C1 C8 C9 -0.1(9) 2_556 . . . ?
C12 C11 C14 O1B 172(2) . . . . ?
C12 C11 C14 C12 1.4(8) . . . 2_677 ?
C14 C11 C12 O1A 179.4(5) . . . . ?
C14 C11 C12 C14 -1.4(8) . . . 2_677 ?
C15 N1 C10 O5 179.7(7) . . . . ?
C16 N1 C10 O5 4.4(11) . . . . ?
C17 N2 C13 O11 0.7(12) . . . . ?
C18 N2 C13 O11 -179.6(8) . . . . ?
C2A N3 C1A O10 180.0(18) . . . . ?
C3A N3 C1A O10 -3(2) . . . . ?
C2B N3 C1B O10 -16(4) . . . . ?
C3B N3 C1B O10 175(2) . . . . ?

_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 1.218
_oxdiff_exptl_absorpt_empirical_full_min 0.753

# start Validation Reply Form
_vrf_PLAT029_SION2_180K          
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.736 Why?  
RESPONSE: The data were collected upon the spindle rotation. Therefore, a 
		  limited portion of the reciprocal space could be probed.
;
_vrf_PLAT972_SION2_180K          
;
PROBLEM: Check Calcd Resid. Dens.  0.83A   From Tb1            -3.75 eA-3  
RESPONSE: Electron density minimum in the vicinity of a heavy atom (Tb1)
		  may be the result of a finite Fourier sum truncation. 
;
# 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_SION2_140K
_database_code_depnum_ccdc_archive 'CCDC 1871308'
loop_
_audit_author_name
_audit_author_address
'Andrzej Gladysiak'
;Ecole polytechnique f?d?rale de Lausanne
Switzerland
;
_audit_update_record             
;
2018-10-03 deposited with the CCDC.	2019-08-12 downloaded from the CCDC.
;
_audit_creation_date             2018-07-09
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_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          ?
_chemical_oxdiff_formula         'C21 H27 N3 O12 Tb'
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                   10.4937(6)
_cell_length_b                   10.9559(4)
_cell_length_c                   12.5321(6)
_cell_angle_alpha                104.652(4)
_cell_angle_beta                 107.923(4)
_cell_angle_gamma                97.114(4)
_cell_volume                     1294.06(11)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5141
_cell_measurement_temperature    140.0
_cell_measurement_theta_max      31.7270
_cell_measurement_theta_min      2.0850
_shelx_estimated_absorpt_T_max   0.828
_shelx_estimated_absorpt_T_min   0.604
_exptl_absorpt_coefficient_mu    2.798
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80033
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.726
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             670
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0162
_diffrn_reflns_av_unetI/netI     0.0244
_diffrn_reflns_Laue_measured_fraction_full 0.724
_diffrn_reflns_Laue_measured_fraction_max 0.662
_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       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8291
_diffrn_reflns_point_group_measured_fraction_full 0.724
_diffrn_reflns_point_group_measured_fraction_max 0.662
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.432
_diffrn_reflns_theta_min         1.979
_diffrn_ambient_temperature      140.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            PILATUS2M
_diffrn_measured_fraction_theta_full 0.724
_diffrn_measured_fraction_theta_max 0.662
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      0.00 360.00   1.00    1.00    --    0.00   0.00   0.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  PILATUS@SNBL
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0600547000
_diffrn_orient_matrix_UB_12      -0.0139527000
_diffrn_orient_matrix_UB_13      0.0363041000
_diffrn_orient_matrix_UB_21      -0.0288260000
_diffrn_orient_matrix_UB_22      -0.0676334000
_diffrn_orient_matrix_UB_23      -0.0272569000
_diffrn_orient_matrix_UB_31      0.0306145000
_diffrn_orient_matrix_UB_32      -0.0000800000
_diffrn_orient_matrix_UB_33      -0.0436279000
_diffrn_radiation_monochromator  'Si (111)'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           ?
_diffrn_radiation_wavelength     0.7142
_diffrn_source                   
'European Synchrotron Radiation Facility, BM01 beamline'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4001
_reflns_number_total             4244
_reflns_odcompleteness_completeness 71.19
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.51
_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 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (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    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         1.295
_refine_diff_density_min         -1.448
_refine_diff_density_rms         0.108
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         4244
_refine_ls_number_restraints     58
_refine_ls_R_factor_all          0.0311
_refine_ls_R_factor_gt           0.0295
_refine_ls_restrained_S_all      1.066
_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)+(0.0703P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0857
_refine_ls_wR_factor_ref         0.0866
_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. Rigid bond restraints
 O3, C2
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.005
3. Uiso/Uaniso restraints and constraints
O3 \\sim C2: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.01
Uanis(O1B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C1A, N3, C2A, C3A, O10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O10, C1B, N3, C3B, C2B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. 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)
6.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C8(H8), C10(H10), C12(H12A), C13(H13), C14(H14), C1A(H1AA), C1B(H1BA)
6.b Tetrahedral OH refined with riding coordinates:
 O1B(H1B)
6.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)
6.d Idealised tetrahedral OH refined as rotating group:
 O9(H9), O12(H12), O1A(H1A)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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 0.09582(2) 0.54674(2) 0.68278(2) 0.02516(10) Uani 1 1 d . . . . .
O2 O -0.0335(3) 0.3349(2) 0.5870(2) 0.0282(6) Uani 1 1 d . . . . .
O3 O 0.1555(3) 0.4864(2) 0.5170(3) 0.0318(5) Uani 1 1 d . U . . .
O4 O -0.0806(3) 0.2733(2) 0.3920(2) 0.0320(6) Uani 1 1 d . . . . .
O5 O 0.0588(3) 0.4843(3) 0.8406(3) 0.0371(7) Uani 1 1 d . . . . .
O6 O 0.1294(3) 0.4238(3) 0.3294(3) 0.0336(7) Uani 1 1 d . . . . .
O7 O 0.1658(3) 0.7625(3) 0.8505(3) 0.0343(7) Uani 1 1 d . . . . .
O8 O 0.3209(3) 0.6812(3) 0.7861(3) 0.0368(7) Uani 1 1 d . . . . .
O9 O 0.0453(4) -0.0490(3) 0.7131(3) 0.0503(9) Uani 1 1 d . . . . .
H9 H 0.0412 -0.1280 0.7051 0.075 Uiso 1 1 calc GR . . . .
O11 O 0.2515(3) 0.4069(3) 0.7355(3) 0.0457(8) Uani 1 1 d . . . . .
O12 O 0.6612(3) 0.6057(4) 0.7360(3) 0.0498(9) Uani 1 1 d . . . . .
H12 H 0.7436 0.6027 0.7468 0.075 Uiso 1 1 calc GR . . . .
N1 N -0.0117(4) 0.3094(4) 0.8915(4) 0.0411(9) Uani 1 1 d . . . . .
O1A O 0.2343(4) 1.0038(3) 0.9940(4) 0.0400(12) Uani 0.873(10) 1 d . . P A 1
H1A H 0.1806 0.9321 0.9531 0.060 Uiso 0.873(10) 1 calc GR . P A 1
O1B O 0.593(3) 0.800(3) 0.880(2) 0.054(9) Uani 0.127(10) 1 d . U P A 2
H1B H 0.5324 0.7334 0.8376 0.080 Uiso 0.127(10) 1 calc R . P A 2
N2 N 0.4292(4) 0.3321(4) 0.8309(4) 0.0485(10) Uani 1 1 d . . . . .
C1 C -0.0266(4) 0.1205(3) 0.4933(4) 0.0298(8) Uani 1 1 d . . . . .
C2 C 0.2057(4) 0.4632(4) 0.4375(4) 0.0310(6) Uani 1 1 d . U . . .
C3 C 0.3577(4) 0.4815(4) 0.4677(4) 0.0294(9) Uani 1 1 d . . . . .
C4 C -0.0480(4) 0.2532(3) 0.4908(3) 0.0278(8) Uani 1 1 d . . . . .
C5 C 0.4427(4) 0.5356(4) 0.5865(4) 0.0354(10) Uani 1 1 d . . . . .
H5 H 0.4033 0.5605 0.6454 0.042 Uiso 1 1 calc R . . . .
C6 C 0.5845(4) 0.5528(4) 0.6184(4) 0.0342(10) Uani 1 1 d . . . . .
C7 C 0.2880(4) 0.7721(3) 0.8497(3) 0.0303(9) Uani 1 1 d . . . . .
C8 C -0.0027(5) 0.0911(4) 0.5971(4) 0.0356(9) Uani 1 1 d . . . . .
H8 H -0.0043 0.1537 0.6645 0.043 Uiso 1 1 calc R . . . .
C9 C 0.0240(5) -0.0288(4) 0.6061(4) 0.0331(9) Uani 1 1 d . . . . .
C10 C -0.0319(5) 0.3879(4) 0.8279(4) 0.0408(11) Uani 1 1 d . . . . .
H10 H -0.1195 0.3721 0.7686 0.049 Uiso 1 1 calc R . . . .
N3 N 0.4760(5) 0.1529(5) 0.4542(5) 0.0598(12) Uani 1 1 d . U . . .
C11 C 0.3963(4) 0.8909(3) 0.9287(3) 0.0299(9) Uani 1 1 d . . . . .
C12 C 0.3640(4) 0.9976(4) 0.9952(4) 0.0342(10) Uani 1 1 d . . . . .
H12A H 0.2721 0.9963 0.9917 0.041 Uiso 0.127(10) 1 calc R . P A 2
C13 C 0.3712(5) 0.4233(5) 0.7961(4) 0.0425(11) Uani 1 1 d . . . . .
H13 H 0.4274 0.5074 0.8204 0.051 Uiso 1 1 calc R . . . .
C14 C 0.5319(4) 0.8943(4) 0.9333(3) 0.0300(9) Uani 1 1 d . . . . .
H14 H 0.5530 0.8219 0.8871 0.036 Uiso 0.873(10) 1 calc R . P A 1
C15 C -0.1217(7) 0.1992(6) 0.8722(6) 0.0577(14) Uani 1 1 d . . . . .
H15A H -0.1498 0.2132 0.9412 0.087 Uiso 1 1 calc GR . . . .
H15B H -0.0876 0.1194 0.8602 0.087 Uiso 1 1 calc GR . . . .
H15C H -0.2005 0.1920 0.8023 0.087 Uiso 1 1 calc GR . . . .
O10 O 0.6075(7) 0.2234(7) 0.6479(5) 0.0956(17) Uani 1 1 d . U . . .
C16 C 0.1145(7) 0.3277(6) 0.9882(6) 0.0708(18) Uani 1 1 d . . . . .
H16A H 0.1752 0.4098 1.0013 0.106 Uiso 1 1 calc GR . . . .
H16B H 0.1599 0.2565 0.9691 0.106 Uiso 1 1 calc GR . . . .
H16C H 0.0941 0.3293 1.0597 0.106 Uiso 1 1 calc GR . . . .
C17 C 0.3539(7) 0.2018(6) 0.7991(6) 0.0690(17) Uani 1 1 d . . . . .
H17A H 0.3402 0.1855 0.8686 0.104 Uiso 1 1 calc GR . . . .
H17B H 0.4055 0.1415 0.7690 0.104 Uiso 1 1 calc GR . . . .
H17C H 0.2644 0.1895 0.7379 0.104 Uiso 1 1 calc GR . . . .
C18 C 0.5748(7) 0.3630(7) 0.9024(7) 0.0753(19) Uani 1 1 d . . . . .
H18A H 0.6218 0.3054 0.8625 0.113 Uiso 1 1 calc GR . . . .
H18B H 0.5856 0.3512 0.9795 0.113 Uiso 1 1 calc GR . . . .
H18C H 0.6147 0.4529 0.9134 0.113 Uiso 1 1 calc GR . . . .
C1A C 0.5961(12) 0.1927(10) 0.5424(9) 0.067(3) Uani 0.640(10) 1 d . U P B 1
H1AA H 0.6775 0.1980 0.5239 0.080 Uiso 0.640(10) 1 calc R . P B 1
C2A C 0.4646(15) 0.1134(13) 0.3318(11) 0.081(3) Uani 0.640(10) 1 d . U P B 1
H2AA H 0.5547 0.1387 0.3262 0.122 Uiso 0.640(10) 1 calc GR . P B 1
H2AB H 0.3992 0.1554 0.2878 0.122 Uiso 0.640(10) 1 calc GR . P B 1
H2AC H 0.4323 0.0193 0.2985 0.122 Uiso 0.640(10) 1 calc GR . P B 1
C3A C 0.3443(12) 0.1374(12) 0.4739(12) 0.078(3) Uani 0.640(10) 1 d . U P B 1
H3AA H 0.2869 0.0518 0.4247 0.117 Uiso 0.640(10) 1 calc GR . P B 1
H3AB H 0.2969 0.2043 0.4529 0.117 Uiso 0.640(10) 1 calc GR . P B 1
H3AC H 0.3614 0.1457 0.5571 0.117 Uiso 0.640(10) 1 calc GR . P B 1
C1B C 0.493(2) 0.201(2) 0.5630(18) 0.075(5) Uani 0.360(10) 1 d . U P B 2
H1BA H 0.4157 0.2205 0.5823 0.091 Uiso 0.360(10) 1 calc R . P B 2
C2B C 0.598(3) 0.141(2) 0.422(2) 0.084(6) Uani 0.360(10) 1 d . U P B 2
H2BA H 0.6361 0.2236 0.4143 0.126 Uiso 0.360(10) 1 calc GR . P B 2
H2BB H 0.5725 0.0728 0.3471 0.126 Uiso 0.360(10) 1 calc GR . P B 2
H2BC H 0.6667 0.1201 0.4837 0.126 Uiso 0.360(10) 1 calc GR . P B 2
C3B C 0.343(2) 0.121(2) 0.361(2) 0.080(6) Uani 0.360(10) 1 d . U P B 2
H3BA H 0.2720 0.1361 0.3957 0.120 Uiso 0.360(10) 1 calc GR . P B 2
H3BB H 0.3224 0.0299 0.3141 0.120 Uiso 0.360(10) 1 calc GR . P B 2
H3BC H 0.3439 0.1757 0.3100 0.120 Uiso 0.360(10) 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 2.340(2) . ?
Tb1 O3 2.314(3) . ?
Tb1 O4 2.390(3) 2_566 ?
Tb1 O5 2.371(3) . ?
Tb1 O6 2.389(3) 2_566 ?
Tb1 O7 2.579(3) . ?
Tb1 O8 2.391(3) . ?
Tb1 O11 2.433(3) . ?
O2 C4 1.260(5) . ?
O3 C2 1.250(6) . ?
O4 Tb1 2.390(3) 2_566 ?
O4 C4 1.262(5) . ?
O5 C10 1.272(6) . ?
O6 Tb1 2.389(3) 2_566 ?
O6 C2 1.270(5) . ?
O7 C7 1.277(5) . ?
O8 C7 1.265(5) . ?
O9 H9 0.8400 . ?
O9 C9 1.369(6) . ?
O11 C13 1.215(6) . ?
O12 H12 0.8400 . ?
O12 C6 1.371(5) . ?
N1 C10 1.307(6) . ?
N1 C15 1.477(7) . ?
N1 C16 1.445(7) . ?
O1A H1A 0.8400 . ?
O1A C12 1.366(6) . ?
O1B H1B 0.8400 . ?
O1B C14 1.41(3) . ?
N2 C13 1.329(6) . ?
N2 C17 1.436(7) . ?
N2 C18 1.459(7) . ?
C1 C4 1.505(5) . ?
C1 C8 1.374(6) . ?
C1 C9 1.399(6) 2_556 ?
C2 C3 1.496(6) . ?
C3 C5 1.403(6) . ?
C3 C6 1.388(7) 2_666 ?
C5 H5 0.9500 . ?
C5 C6 1.392(6) . ?
C6 C3 1.388(7) 2_666 ?
C7 C11 1.502(5) . ?
C8 H8 0.9500 . ?
C8 C9 1.401(5) . ?
C9 C1 1.399(6) 2_556 ?
C10 H10 0.9500 . ?
N3 C1A 1.328(11) . ?
N3 C2A 1.447(13) . ?
N3 C3A 1.474(13) . ?
N3 C1B 1.28(2) . ?
N3 C2B 1.46(2) . ?
N3 C3B 1.45(2) . ?
C11 C12 1.398(6) . ?
C11 C14 1.402(6) . ?
C12 H12A 0.9500 . ?
C12 C14 1.393(5) 2_677 ?
C13 H13 0.9500 . ?
C14 C12 1.393(5) 2_677 ?
C14 H14 0.9500 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
O10 C1A 1.242(12) . ?
O10 C1B 1.28(2) . ?
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 126.79(9) . 2_566 ?
O2 Tb1 O5 78.05(10) . . ?
O2 Tb1 O6 78.77(10) . 2_566 ?
O2 Tb1 O7 151.35(10) . . ?
O2 Tb1 O8 145.87(10) . . ?
O2 Tb1 O11 74.10(10) . . ?
O3 Tb1 O2 77.29(10) . . ?
O3 Tb1 O4 76.04(10) . 2_566 ?
O3 Tb1 O5 145.79(10) . . ?
O3 Tb1 O6 122.05(10) . 2_566 ?
O3 Tb1 O7 131.26(9) . . ?
O3 Tb1 O8 88.49(10) . . ?
O3 Tb1 O11 78.32(12) . . ?
O4 Tb1 O7 68.41(9) 2_566 . ?
O4 Tb1 O8 77.73(10) 2_566 . ?
O4 Tb1 O11 141.01(12) 2_566 . ?
O5 Tb1 O4 138.15(11) . 2_566 ?
O5 Tb1 O6 75.23(11) . 2_566 ?
O5 Tb1 O7 76.60(10) . . ?
O5 Tb1 O8 99.03(11) . . ?
O5 Tb1 O11 72.35(12) . . ?
O6 Tb1 O4 77.82(10) 2_566 2_566 ?
O6 Tb1 O7 82.05(9) 2_566 . ?
O6 Tb1 O8 133.96(10) 2_566 . ?
O6 Tb1 O11 141.14(11) 2_566 . ?
O8 Tb1 O7 52.73(10) . . ?
O8 Tb1 O11 72.69(11) . . ?
O11 Tb1 O7 110.13(11) . . ?
C4 O2 Tb1 132.7(3) . . ?
C2 O3 Tb1 171.3(3) . . ?
C4 O4 Tb1 138.1(2) . 2_566 ?
C10 O5 Tb1 124.5(3) . . ?
C2 O6 Tb1 108.0(3) . 2_566 ?
C7 O7 Tb1 88.4(2) . . ?
C7 O8 Tb1 97.4(2) . . ?
C9 O9 H9 109.5 . . ?
C13 O11 Tb1 135.5(3) . . ?
C6 O12 H12 109.5 . . ?
C10 N1 C15 121.2(4) . . ?
C10 N1 C16 123.0(5) . . ?
C16 N1 C15 115.7(4) . . ?
C12 O1A H1A 109.5 . . ?
C14 O1B H1B 109.5 . . ?
C13 N2 C17 122.2(5) . . ?
C13 N2 C18 119.8(5) . . ?
C17 N2 C18 117.9(5) . . ?
C8 C1 C4 119.2(4) . . ?
C8 C1 C9 119.4(3) . 2_556 ?
C9 C1 C4 121.3(4) 2_556 . ?
O3 C2 O6 121.1(4) . . ?
O3 C2 C3 120.5(4) . . ?
O6 C2 C3 118.4(4) . . ?
C5 C3 C2 118.4(4) . . ?
C6 C3 C2 121.7(4) 2_666 . ?
C6 C3 C5 119.8(4) 2_666 . ?
O2 C4 O4 125.2(3) . . ?
O2 C4 C1 117.5(3) . . ?
O4 C4 C1 117.3(3) . . ?
C3 C5 H5 119.9 . . ?
C6 C5 C3 120.2(5) . . ?
C6 C5 H5 119.9 . . ?
O12 C6 C3 123.0(4) . 2_666 ?
O12 C6 C5 117.0(4) . . ?
C3 C6 C5 120.0(4) 2_666 . ?
O7 C7 C11 119.8(4) . . ?
O8 C7 O7 121.1(3) . . ?
O8 C7 C11 119.1(4) . . ?
C1 C8 H8 119.1 . . ?
C1 C8 C9 121.7(4) . . ?
C9 C8 H8 119.1 . . ?
O9 C9 C1 124.0(3) . 2_556 ?
O9 C9 C8 117.2(4) . . ?
C1 C9 C8 118.9(4) 2_556 . ?
O5 C10 N1 124.0(4) . . ?
O5 C10 H10 118.0 . . ?
N1 C10 H10 118.0 . . ?
C1A N3 C2A 122.6(9) . . ?
C1A N3 C3A 122.4(8) . . ?
C2A N3 C3A 114.9(9) . . ?
C1B N3 C2B 118.2(15) . . ?
C1B N3 C3B 122.7(15) . . ?
C3B N3 C2B 118.9(15) . . ?
C12 C11 C7 121.4(4) . . ?
C12 C11 C14 120.0(3) . . ?
C14 C11 C7 118.5(4) . . ?
O1A C12 C11 123.9(3) . . ?
O1A C12 C14 116.9(4) . 2_677 ?
C11 C12 H12A 120.4 . . ?
C14 C12 C11 119.2(4) 2_677 . ?
C14 C12 H12A 120.4 2_677 . ?
O11 C13 N2 124.8(5) . . ?
O11 C13 H13 117.6 . . ?
N2 C13 H13 117.6 . . ?
O1B C14 C11 131.7(11) . . ?
O1B C14 C12 107.5(11) . 2_677 ?
C11 C14 H14 119.6 . . ?
C12 C14 C11 120.7(4) 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 118.3 . . ?
O10 C1A N3 123.3(10) . . ?
O10 C1A H1AA 118.3 . . ?
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 O10 124.4(19) . . ?
N3 C1B H1BA 117.8 . . ?
O10 C1B H1BA 117.8 . . ?
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 -52.6(5) . . . . ?
Tb1 O2 C4 C1 128.3(3) . . . . ?
Tb1 O4 C4 O2 13.5(7) 2_566 . . . ?
Tb1 O4 C4 C1 -167.3(3) 2_566 . . . ?
Tb1 O5 C10 N1 139.6(4) . . . . ?
Tb1 O6 C2 O3 12.7(4) 2_566 . . . ?
Tb1 O6 C2 C3 -167.2(3) 2_566 . . . ?
Tb1 O7 C7 O8 -6.1(4) . . . . ?
Tb1 O7 C7 C11 176.2(3) . . . . ?
Tb1 O8 C7 O7 6.7(4) . . . . ?
Tb1 O8 C7 C11 -175.7(3) . . . . ?
Tb1 O11 C13 N2 166.3(4) . . . . ?
O3 C2 C3 C5 -5.4(5) . . . . ?
O3 C2 C3 C6 175.0(4) . . . 2_666 ?
O6 C2 C3 C5 174.6(4) . . . . ?
O6 C2 C3 C6 -5.0(6) . . . 2_666 ?
O7 C7 C11 C12 -6.4(6) . . . . ?
O7 C7 C11 C14 174.7(4) . . . . ?
O8 C7 C11 C12 176.0(4) . . . . ?
O8 C7 C11 C14 -3.0(6) . . . . ?
C1 C8 C9 O9 -179.4(4) . . . . ?
C1 C8 C9 C1 0.2(7) . . . 2_556 ?
C2 C3 C5 C6 179.3(4) . . . . ?
C3 C5 C6 O12 -179.8(4) . . . . ?
C3 C5 C6 C3 1.2(7) . . . 2_666 ?
C4 C1 C8 C9 -177.1(4) . . . . ?
C6 C3 C5 C6 -1.1(7) 2_666 . . . ?
C7 C11 C12 O1A -0.5(7) . . . . ?
C7 C11 C12 C14 -179.7(4) . . . 2_677 ?
C7 C11 C14 O1B -4.1(19) . . . . ?
C7 C11 C14 C12 179.7(4) . . . 2_677 ?
C8 C1 C4 O2 4.8(6) . . . . ?
C8 C1 C4 O4 -174.4(4) . . . . ?
C9 C1 C4 O2 -172.1(4) 2_556 . . . ?
C9 C1 C4 O4 8.7(6) 2_556 . . . ?
C9 C1 C8 C9 -0.2(7) 2_556 . . . ?
C12 C11 C14 O1B 176.9(19) . . . . ?
C12 C11 C14 C12 0.8(7) . . . 2_677 ?
C14 C11 C12 O1A 178.5(4) . . . . ?
C14 C11 C12 C14 -0.8(7) . . . 2_677 ?
C15 N1 C10 O5 180.0(5) . . . . ?
C16 N1 C10 O5 3.5(8) . . . . ?
C17 N2 C13 O11 0.1(9) . . . . ?
C18 N2 C13 O11 179.1(6) . . . . ?
C2A N3 C1A O10 -177.9(10) . . . . ?
C3A N3 C1A O10 -2.1(14) . . . . ?
C2B N3 C1B O10 -10(3) . . . . ?
C3B N3 C1B O10 176.1(16) . . . . ?

_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 1.145
_oxdiff_exptl_absorpt_empirical_full_min 0.861

# start Validation Reply Form
_vrf_PLAT029_SION2_140K          
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.724 Why?  
RESPONSE: The data were collected upon the spindle rotation. Therefore, a 
		  limited portion of the reciprocal space could be probed.
;
# 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_SION2_240K
_database_code_depnum_ccdc_archive 'CCDC 1871307'
loop_
_audit_author_name
_audit_author_address
'Andrzej Gladysiak'
;Ecole polytechnique f?d?rale de Lausanne
Switzerland
;
_audit_update_record             
;
2018-10-03 deposited with the CCDC.	2019-08-12 downloaded from the CCDC.
;
_audit_creation_date             2018-07-09
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_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          ?
_chemical_oxdiff_formula         'C21 H27 N3 O12 Tb'
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                   10.5121(6)
_cell_length_b                   10.9835(5)
_cell_length_c                   12.6782(5)
_cell_angle_alpha                104.175(4)
_cell_angle_beta                 109.639(4)
_cell_angle_gamma                96.452(4)
_cell_volume                     1305.96(12)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5799
_cell_measurement_temperature    240.0
_cell_measurement_theta_max      31.8610
_cell_measurement_theta_min      2.1000
_shelx_estimated_absorpt_T_max   0.830
_shelx_estimated_absorpt_T_min   0.607
_exptl_absorpt_coefficient_mu    2.773
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78641
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.710
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             670
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0162
_diffrn_reflns_av_unetI/netI     0.0231
_diffrn_reflns_Laue_measured_fraction_full 0.743
_diffrn_reflns_Laue_measured_fraction_max 0.681
_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       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8597
_diffrn_reflns_point_group_measured_fraction_full 0.743
_diffrn_reflns_point_group_measured_fraction_max 0.681
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.428
_diffrn_reflns_theta_min         1.967
_diffrn_ambient_temperature      240.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            PILATUS2M
_diffrn_measured_fraction_theta_full 0.743
_diffrn_measured_fraction_theta_max 0.681
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      0.00 360.00   1.00    1.00    --    0.00   0.00   0.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  PILATUS@SNBL
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0607900000
_diffrn_orient_matrix_UB_12      -0.0140685000
_diffrn_orient_matrix_UB_13      0.0372153000
_diffrn_orient_matrix_UB_21      -0.0289161000
_diffrn_orient_matrix_UB_22      -0.0671874000
_diffrn_orient_matrix_UB_23      -0.0270054000
_diffrn_orient_matrix_UB_31      0.0303309000
_diffrn_orient_matrix_UB_32      -0.0002330000
_diffrn_orient_matrix_UB_33      -0.0426888000
_diffrn_radiation_monochromator  'Si (111)'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           ?
_diffrn_radiation_wavelength     0.7142
_diffrn_source                   
'European Synchrotron Radiation Facility, BM01 beamline'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4188
_reflns_number_total             4401
_reflns_odcompleteness_completeness 73.37
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.51
_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 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (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    'XT (Sheldrick, 2015)'
_refine_diff_density_max         1.431
_refine_diff_density_min         -1.386
_refine_diff_density_rms         0.091
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         4401
_refine_ls_number_restraints     58
_refine_ls_R_factor_all          0.0280
_refine_ls_R_factor_gt           0.0267
_refine_ls_restrained_S_all      1.072
_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)+(0.0552P)²+0.5328P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0735
_refine_ls_wR_factor_ref         0.0743
_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. Rigid bond restraints
 O3, C2
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.005
3. Uiso/Uaniso restraints and constraints
O3 \\sim C2: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.01
Uanis(O1B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C1A, N3, C2A, C3A, O10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O10, C1B, N3, C3B, C2B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. 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)
6.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C8(H8), C10(H10), C12(H12A), C13(H13), C14(H14), C1A(H1AA), C1B(H1BA)
6.b Tetrahedral OH refined with riding coordinates:
 O1B(H1B)
6.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)
6.d Idealised tetrahedral OH refined as rotating group:
 O9(H9), O12(H12), O1A(H1A)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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 0.10126(2) 0.54756(2) 0.68277(2) 0.02683(8) Uani 1 1 d . . . . .
O2 O -0.0216(3) 0.3356(2) 0.5872(2) 0.0359(6) Uani 1 1 d . . . . .
O3 O 0.1601(3) 0.4922(2) 0.5212(3) 0.0379(5) Uani 1 1 d . U . . .
O4 O -0.0740(3) 0.2756(2) 0.3938(2) 0.0374(6) Uani 1 1 d . . . . .
O5 O 0.0667(3) 0.4816(3) 0.8386(2) 0.0463(7) Uani 1 1 d . . . . .
O6 O 0.1263(3) 0.4288(3) 0.3334(2) 0.0396(6) Uani 1 1 d . . . . .
O7 O 0.1720(3) 0.7572(2) 0.8493(2) 0.0389(6) Uani 1 1 d . . . . .
O8 O 0.3259(3) 0.6865(3) 0.7828(3) 0.0509(8) Uani 1 1 d . . . . .
O9 O 0.0453(5) -0.0506(3) 0.7106(3) 0.0669(11) Uani 1 1 d . . . . .
H9 H 0.0559 -0.1252 0.7057 0.100 Uiso 1 1 calc GR . . . .
O11 O 0.2648(4) 0.4168(4) 0.7425(4) 0.0673(10) Uani 1 1 d . . . . .
O12 O 0.6698(3) 0.6007(4) 0.7340(3) 0.0601(10) Uani 1 1 d . . . . .
H12 H 0.7524 0.6144 0.7423 0.090 Uiso 1 1 calc GR . . . .
N1 N -0.0031(5) 0.3129(4) 0.8932(4) 0.0584(11) Uani 1 1 d . . . . .
O1A O 0.2356(3) 0.9916(4) 0.9973(4) 0.0512(12) Uani 0.884(9) 1 d . . P A 1
H1A H 0.1842 0.9203 0.9572 0.077 Uiso 0.884(9) 1 calc GR . P A 1
O1B O 0.595(2) 0.808(2) 0.879(3) 0.061(9) Uani 0.116(9) 1 d . U P A 2
H1B H 0.5349 0.7420 0.8370 0.091 Uiso 0.116(9) 1 calc R . P A 2
N2 N 0.4336(5) 0.3283(5) 0.8297(5) 0.0753(14) Uani 1 1 d . . . . .
C1 C -0.0223(4) 0.1213(3) 0.4935(3) 0.0337(8) Uani 1 1 d . . . . .
C2 C 0.2063(4) 0.4676(3) 0.4403(4) 0.0359(6) Uani 1 1 d . U . . .
C3 C 0.3579(4) 0.4839(3) 0.4690(3) 0.0343(9) Uani 1 1 d . . . . .
C4 C -0.0405(4) 0.2544(3) 0.4921(3) 0.0318(8) Uani 1 1 d . . . . .
C5 C 0.4465(4) 0.5343(4) 0.5868(3) 0.0377(9) Uani 1 1 d . . . . .
H5 H 0.4100 0.5570 0.6454 0.045 Uiso 1 1 calc R . . . .
C6 C 0.5892(4) 0.5508(4) 0.6175(3) 0.0389(9) Uani 1 1 d . . . . .
C7 C 0.2933(4) 0.7718(3) 0.8485(3) 0.0349(8) Uani 1 1 d . . . . .
C8 C 0.0006(5) 0.0902(3) 0.5967(3) 0.0423(9) Uani 1 1 d . . . . .
H8 H 0.0011 0.1520 0.6629 0.051 Uiso 1 1 calc R . . . .
C9 C 0.0231(5) -0.0298(3) 0.6054(3) 0.0405(9) Uani 1 1 d . . . . .
C10 C -0.0226(5) 0.3882(4) 0.8256(4) 0.0509(11) Uani 1 1 d . . . . .
H10 H -0.1089 0.3707 0.7638 0.061 Uiso 1 1 calc R . . . .
N3 N 0.4782(7) 0.1531(6) 0.4527(6) 0.0939(17) Uani 1 1 d . U . . .
C11 C 0.3989(4) 0.8910(3) 0.9268(3) 0.0347(8) Uani 1 1 d . . . . .
C12 C 0.3643(4) 0.9912(4) 0.9959(4) 0.0390(9) Uani 1 1 d . . . . .
H12A H 0.2732 0.9858 0.9930 0.047 Uiso 0.116(9) 1 calc R . P A 2
C13 C 0.3807(6) 0.4238(7) 0.7983(5) 0.0752(17) Uani 1 1 d . . . . .
H13 H 0.4414 0.5039 0.8231 0.090 Uiso 1 1 calc R . . . .
C14 C 0.5329(4) 0.9001(4) 0.9306(3) 0.0388(9) Uani 1 1 d . . . . .
H14 H 0.5549 0.8323 0.8831 0.047 Uiso 0.884(9) 1 calc R . P A 1
C15 C -0.1128(9) 0.2065(7) 0.8742(8) 0.099(2) Uani 1 1 d . . . . .
H15A H -0.1390 0.2214 0.9420 0.148 Uiso 1 1 calc GR . . . .
H15B H -0.0802 0.1270 0.8631 0.148 Uiso 1 1 calc GR . . . .
H15C H -0.1924 0.2005 0.8049 0.148 Uiso 1 1 calc GR . . . .
O10 O 0.6137(9) 0.2266(9) 0.6444(7) 0.149(3) Uani 1 1 d . U . . .
C16 C 0.1215(10) 0.3323(9) 0.9903(7) 0.120(3) Uani 1 1 d . . . . .
H16A H 0.1614 0.4236 1.0253 0.180 Uiso 1 1 calc GR . . . .
H16B H 0.1860 0.2892 0.9641 0.180 Uiso 1 1 calc GR . . . .
H16C H 0.1026 0.2975 1.0481 0.180 Uiso 1 1 calc GR . . . .
C17 C 0.3695(11) 0.1977(10) 0.7994(9) 0.147(5) Uani 1 1 d . . . . .
H17A H 0.3749 0.1757 0.8701 0.220 Uiso 1 1 calc GR . . . .
H17B H 0.4163 0.1441 0.7588 0.220 Uiso 1 1 calc GR . . . .
H17C H 0.2733 0.1837 0.7484 0.220 Uiso 1 1 calc GR . . . .
C18 C 0.5853(10) 0.3643(10) 0.9008(9) 0.125(3) Uani 1 1 d . . . . .
H18A H 0.6307 0.3024 0.8670 0.188 Uiso 1 1 calc GR . . . .
H18B H 0.6014 0.3648 0.9809 0.188 Uiso 1 1 calc GR . . . .
H18C H 0.6225 0.4492 0.9007 0.188 Uiso 1 1 calc GR . . . .
C1A C 0.602(2) 0.1939(17) 0.5438(18) 0.113(5) Uani 0.527(12) 1 d . U P B 1
H1AA H 0.6830 0.1966 0.5272 0.136 Uiso 0.527(12) 1 calc R . P B 1
C2A C 0.454(3) 0.114(2) 0.3311(19) 0.138(7) Uani 0.527(12) 1 d . U P B 1
H2AA H 0.5354 0.1482 0.3193 0.207 Uiso 0.527(12) 1 calc GR . P B 1
H2AB H 0.3761 0.1462 0.2891 0.207 Uiso 0.527(12) 1 calc GR . P B 1
H2AC H 0.4331 0.0209 0.3017 0.207 Uiso 0.527(12) 1 calc GR . P B 1
C3A C 0.351(2) 0.143(2) 0.480(2) 0.130(6) Uani 0.527(12) 1 d . U P B 1
H3AA H 0.3250 0.0577 0.4848 0.195 Uiso 0.527(12) 1 calc GR . P B 1
H3AB H 0.2761 0.1589 0.4183 0.195 Uiso 0.527(12) 1 calc GR . P B 1
H3AC H 0.3681 0.2063 0.5544 0.195 Uiso 0.527(12) 1 calc GR . P B 1
C1B C 0.504(3) 0.203(2) 0.5631(19) 0.118(6) Uani 0.473(12) 1 d . U P B 2
H1BA H 0.4282 0.2239 0.5825 0.142 Uiso 0.473(12) 1 calc R . P B 2
C2B C 0.601(3) 0.140(2) 0.420(2) 0.127(7) Uani 0.473(12) 1 d . U P B 2
H2BA H 0.6322 0.2183 0.4042 0.191 Uiso 0.473(12) 1 calc GR . P B 2
H2BB H 0.5752 0.0677 0.3497 0.191 Uiso 0.473(12) 1 calc GR . P B 2
H2BC H 0.6745 0.1270 0.4836 0.191 Uiso 0.473(12) 1 calc GR . P B 2
C3B C 0.345(2) 0.115(2) 0.356(2) 0.124(7) Uani 0.473(12) 1 d . U P B 2
H3BA H 0.2767 0.1502 0.3833 0.187 Uiso 0.473(12) 1 calc GR . P B 2
H3BB H 0.3172 0.0223 0.3273 0.187 Uiso 0.473(12) 1 calc GR . P B 2
H3BC H 0.3514 0.1481 0.2933 0.187 Uiso 0.473(12) 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 2.334(2) . ?
Tb1 O3 2.297(3) . ?
Tb1 O4 2.378(2) 2_566 ?
Tb1 O5 2.384(3) . ?
Tb1 O6 2.381(3) 2_566 ?
Tb1 O7 2.548(3) . ?
Tb1 O8 2.396(3) . ?
Tb1 O11 2.409(3) . ?
O2 C4 1.250(5) . ?
O3 C2 1.260(5) . ?
O4 Tb1 2.378(2) 2_566 ?
O4 C4 1.264(5) . ?
O5 C10 1.247(6) . ?
O6 Tb1 2.381(3) 2_566 ?
O6 C2 1.263(5) . ?
O7 C7 1.271(5) . ?
O8 C7 1.253(5) . ?
O9 H9 0.8300 . ?
O9 C9 1.356(5) . ?
O11 C13 1.167(6) . ?
O12 H12 0.8300 . ?
O12 C6 1.363(5) . ?
N1 C10 1.315(6) . ?
N1 C15 1.458(8) . ?
N1 C16 1.414(8) . ?
O1A H1A 0.8300 . ?
O1A C12 1.359(6) . ?
O1B H1B 0.8300 . ?
O1B C14 1.41(3) . ?
N2 C13 1.324(6) . ?
N2 C17 1.414(10) . ?
N2 C18 1.493(10) . ?
C1 C4 1.499(4) . ?
C1 C8 1.383(5) . ?
C1 C9 1.399(6) 2_556 ?
C2 C3 1.489(5) . ?
C3 C5 1.395(5) . ?
C3 C6 1.382(7) 2_666 ?
C5 H5 0.9400 . ?
C5 C6 1.395(5) . ?
C6 C3 1.382(7) 2_666 ?
C7 C11 1.493(4) . ?
C8 H8 0.9400 . ?
C8 C9 1.388(5) . ?
C9 C1 1.398(6) 2_556 ?
C10 H10 0.9400 . ?
N3 C1A 1.36(2) . ?
N3 C2A 1.42(2) . ?
N3 C3A 1.49(2) . ?
N3 C1B 1.29(2) . ?
N3 C2B 1.49(2) . ?
N3 C3B 1.45(2) . ?
C11 C12 1.394(6) . ?
C11 C14 1.385(6) . ?
C12 H12A 0.9400 . ?
C12 C14 1.396(5) 2_677 ?
C13 H13 0.9400 . ?
C14 C12 1.396(5) 2_677 ?
C14 H14 0.9400 . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C15 H15C 0.9700 . ?
O10 C1A 1.20(2) . ?
O10 C1B 1.21(2) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C16 H16C 0.9700 . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C17 H17C 0.9700 . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C18 H18C 0.9700 . ?
C1A H1AA 0.9400 . ?
C2A H2AA 0.9700 . ?
C2A H2AB 0.9700 . ?
C2A H2AC 0.9700 . ?
C3A H3AA 0.9700 . ?
C3A H3AB 0.9700 . ?
C3A H3AC 0.9700 . ?
C1B H1BA 0.9400 . ?
C2B H2BA 0.9700 . ?
C2B H2BB 0.9700 . ?
C2B H2BC 0.9700 . ?
C3B H3BA 0.9700 . ?
C3B H3BB 0.9700 . ?
C3B H3BC 0.9700 . ?

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 126.27(9) . 2_566 ?
O2 Tb1 O5 77.70(10) . . ?
O2 Tb1 O6 79.19(10) . 2_566 ?
O2 Tb1 O7 151.85(10) . . ?
O2 Tb1 O8 145.56(10) . . ?
O2 Tb1 O11 74.73(12) . . ?
O3 Tb1 O2 77.22(10) . . ?
O3 Tb1 O4 76.13(9) . 2_566 ?
O3 Tb1 O5 145.92(10) . . ?
O3 Tb1 O6 122.08(9) . 2_566 ?
O3 Tb1 O7 130.92(9) . . ?
O3 Tb1 O8 86.81(10) . . ?
O3 Tb1 O11 79.37(12) . . ?
O4 Tb1 O5 137.87(10) 2_566 . ?
O4 Tb1 O6 76.95(10) 2_566 2_566 ?
O4 Tb1 O7 69.64(9) 2_566 . ?
O4 Tb1 O8 77.41(10) 2_566 . ?
O4 Tb1 O11 141.84(12) 2_566 . ?
O5 Tb1 O7 76.55(9) . . ?
O5 Tb1 O8 101.41(11) . . ?
O5 Tb1 O11 72.01(13) . . ?
O6 Tb1 O5 74.75(11) 2_566 . ?
O6 Tb1 O7 83.24(9) 2_566 . ?
O6 Tb1 O8 134.41(10) 2_566 . ?
O6 Tb1 O11 141.21(12) 2_566 . ?
O8 Tb1 O7 52.55(10) . . ?
O8 Tb1 O11 72.42(12) . . ?
O11 Tb1 O7 107.50(12) . . ?
C4 O2 Tb1 134.8(2) . . ?
C2 O3 Tb1 173.5(2) . . ?
C4 O4 Tb1 138.8(2) . 2_566 ?
C10 O5 Tb1 125.1(3) . . ?
C2 O6 Tb1 109.5(3) . 2_566 ?
C7 O7 Tb1 89.5(2) . . ?
C7 O8 Tb1 97.1(2) . . ?
C9 O9 H9 109.5 . . ?
C13 O11 Tb1 142.0(4) . . ?
C6 O12 H12 109.5 . . ?
C10 N1 C15 121.0(5) . . ?
C10 N1 C16 122.7(5) . . ?
C16 N1 C15 116.2(5) . . ?
C12 O1A H1A 109.5 . . ?
C14 O1B H1B 109.5 . . ?
C13 N2 C17 129.4(7) . . ?
C13 N2 C18 114.1(6) . . ?
C17 N2 C18 116.4(7) . . ?
C8 C1 C4 118.9(3) . . ?
C8 C1 C9 119.3(3) . 2_556 ?
C9 C1 C4 121.7(3) 2_556 . ?
O3 C2 O6 121.4(3) . . ?
O3 C2 C3 120.4(3) . . ?
O6 C2 C3 118.2(4) . . ?
C5 C3 C2 118.2(4) . . ?
C6 C3 C2 121.6(3) 2_666 . ?
C6 C3 C5 120.3(3) 2_666 . ?
O2 C4 O4 125.0(3) . . ?
O2 C4 C1 118.0(3) . . ?
O4 C4 C1 117.0(3) . . ?
C3 C5 H5 120.0 . . ?
C3 C5 C6 120.0(4) . . ?
C6 C5 H5 120.0 . . ?
O12 C6 C3 123.3(4) . 2_666 ?
O12 C6 C5 117.0(4) . . ?
C3 C6 C5 119.7(3) 2_666 . ?
O7 C7 C11 120.0(3) . . ?
O8 C7 O7 120.6(3) . . ?
O8 C7 C11 119.3(4) . . ?
C1 C8 H8 119.0 . . ?
C1 C8 C9 121.9(4) . . ?
C9 C8 H8 119.0 . . ?
O9 C9 C1 123.9(3) . 2_556 ?
O9 C9 C8 117.4(3) . . ?
C8 C9 C1 118.7(4) . 2_556 ?
O5 C10 N1 123.9(4) . . ?
O5 C10 H10 118.1 . . ?
N1 C10 H10 118.1 . . ?
C1A N3 C2A 127.4(18) . . ?
C1A N3 C3A 118.1(15) . . ?
C2A N3 C3A 114.5(15) . . ?
C1B N3 C2B 116.4(17) . . ?
C1B N3 C3B 127.4(19) . . ?
C3B N3 C2B 116.0(16) . . ?
C12 C11 C7 120.9(4) . . ?
C14 C11 C7 118.8(3) . . ?
C14 C11 C12 120.3(3) . . ?
O1A C12 C11 124.6(3) . . ?
O1A C12 C14 116.6(4) . 2_677 ?
C11 C12 H12A 120.6 . . ?
C11 C12 C14 118.9(4) . 2_677 ?
C14 C12 H12A 120.6 2_677 . ?
O11 C13 N2 125.5(7) . . ?
O11 C13 H13 117.3 . . ?
N2 C13 H13 117.3 . . ?
O1B C14 C11 130.3(11) . . ?
O1B C14 C12 108.5(10) . 2_677 ?
C11 C14 C12 120.8(4) . 2_677 ?
C11 C14 H14 119.6 . . ?
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 118.4 . . ?
O10 C1A N3 123(2) . . ?
O10 C1A H1AA 118.4 . . ?
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 116.4 . . ?
O10 C1B N3 127(3) . . ?
O10 C1B H1BA 116.4 . . ?
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 -47.7(5) . . . . ?
Tb1 O2 C4 C1 132.4(3) . . . . ?
Tb1 O4 C4 O2 7.5(6) 2_566 . . . ?
Tb1 O4 C4 C1 -172.5(3) 2_566 . . . ?
Tb1 O5 C10 N1 143.8(4) . . . . ?
Tb1 O6 C2 O3 11.0(4) 2_566 . . . ?
Tb1 O6 C2 C3 -168.9(2) 2_566 . . . ?
Tb1 O7 C7 O8 -4.5(4) . . . . ?
Tb1 O7 C7 C11 175.9(3) . . . . ?
Tb1 O8 C7 O7 4.8(4) . . . . ?
Tb1 O8 C7 C11 -175.6(3) . . . . ?
Tb1 O11 C13 N2 167.3(4) . . . . ?
O3 C2 C3 C5 -3.8(5) . . . . ?
O3 C2 C3 C6 175.4(4) . . . 2_666 ?
O6 C2 C3 C5 176.1(3) . . . . ?
O6 C2 C3 C6 -4.6(5) . . . 2_666 ?
O7 C7 C11 C12 -4.3(5) . . . . ?
O7 C7 C11 C14 175.2(4) . . . . ?
O8 C7 C11 C12 176.1(4) . . . . ?
O8 C7 C11 C14 -4.4(5) . . . . ?
C1 C8 C9 O9 179.7(4) . . . . ?
C1 C8 C9 C1 0.0(7) . . . 2_556 ?
C2 C3 C5 C6 179.8(4) . . . . ?
C3 C5 C6 O12 179.8(4) . . . . ?
C3 C5 C6 C3 -0.6(7) . . . 2_666 ?
C4 C1 C8 C9 -177.7(4) . . . . ?
C6 C3 C5 C6 0.6(7) 2_666 . . . ?
C7 C11 C12 O1A -1.2(6) . . . . ?
C7 C11 C12 C14 178.8(3) . . . 2_677 ?
C7 C11 C14 O1B -7(2) . . . . ?
C7 C11 C14 C12 -178.8(4) . . . 2_677 ?
C8 C1 C4 O2 6.4(5) . . . . ?
C8 C1 C4 O4 -173.6(4) . . . . ?
C9 C1 C4 O2 -171.3(4) 2_556 . . . ?
C9 C1 C4 O4 8.8(5) 2_556 . . . ?
C9 C1 C8 C9 0.0(7) 2_556 . . . ?
C12 C11 C14 O1B 172.8(19) . . . . ?
C12 C11 C14 C12 0.6(7) . . . 2_677 ?
C14 C11 C12 O1A 179.4(4) . . . . ?
C14 C11 C12 C14 -0.6(6) . . . 2_677 ?
C15 N1 C10 O5 179.0(6) . . . . ?
C16 N1 C10 O5 1.6(10) . . . . ?
C17 N2 C13 O11 4.4(13) . . . . ?
C18 N2 C13 O11 179.8(7) . . . . ?
C2A N3 C1A O10 179.2(17) . . . . ?
C3A N3 C1A O10 -3(2) . . . . ?
C2B N3 C1B O10 -10(3) . . . . ?
C3B N3 C1B O10 174.5(18) . . . . ?

_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 1.191
_oxdiff_exptl_absorpt_empirical_full_min 0.866

# start Validation Reply Form
_vrf_PLAT029_SION2_240K          
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.743 Why?  
RESPONSE: The data were collected upon the spindle rotation. Therefore, a 
		  limited portion of the reciprocal space could be probed.
;
# 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_SION2_160K
_database_code_depnum_ccdc_archive 'CCDC 1871303'
loop_
_audit_author_name
_audit_author_address
'Andrzej Gladysiak'
;Ecole polytechnique f?d?rale de Lausanne
Switzerland
;
_audit_update_record             
;
2018-10-03 deposited with the CCDC.	2019-08-12 downloaded from the CCDC.
;
_audit_creation_date             2018-07-09
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_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          ?
_chemical_oxdiff_formula         'C21 H37 N3 O12 Tb'
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                   10.5194(6)
_cell_length_b                   10.9889(4)
_cell_length_c                   12.5734(6)
_cell_angle_alpha                104.589(4)
_cell_angle_beta                 108.172(5)
_cell_angle_gamma                96.992(4)
_cell_volume                     1304.34(12)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5369
_cell_measurement_temperature    160.0
_cell_measurement_theta_max      31.7770
_cell_measurement_theta_min      1.9530
_shelx_estimated_absorpt_T_max   0.829
_shelx_estimated_absorpt_T_min   0.607
_exptl_absorpt_coefficient_mu    2.776
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80921
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.712
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             670
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0166
_diffrn_reflns_av_unetI/netI     0.0245
_diffrn_reflns_Laue_measured_fraction_full 0.729
_diffrn_reflns_Laue_measured_fraction_max 0.666
_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       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8395
_diffrn_reflns_point_group_measured_fraction_full 0.729
_diffrn_reflns_point_group_measured_fraction_max 0.666
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.427
_diffrn_reflns_theta_min         1.972
_diffrn_ambient_temperature      160.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            PILATUS2M
_diffrn_measured_fraction_theta_full 0.729
_diffrn_measured_fraction_theta_max 0.666
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      0.00 360.00   1.00    1.00    --    0.00   0.00   0.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  PILATUS@SNBL
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0600809000
_diffrn_orient_matrix_UB_12      -0.0138823000
_diffrn_orient_matrix_UB_13      0.0363571000
_diffrn_orient_matrix_UB_21      -0.0287156000
_diffrn_orient_matrix_UB_22      -0.0673955000
_diffrn_orient_matrix_UB_23      -0.0271216000
_diffrn_orient_matrix_UB_31      0.0304336000
_diffrn_orient_matrix_UB_32      -0.0001264000
_diffrn_orient_matrix_UB_33      -0.0434693000
_diffrn_radiation_monochromator  'Si (111)'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           ?
_diffrn_radiation_wavelength     0.7142
_diffrn_source                   
'European Synchrotron Radiation Facility, BM01 beamline'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4075
_reflns_number_total             4303
_reflns_odcompleteness_completeness 71.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.51
_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 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (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    'XT (Sheldrick, 2015)'
_refine_diff_density_max         1.027
_refine_diff_density_min         -1.234
_refine_diff_density_rms         0.101
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         4303
_refine_ls_number_restraints     58
_refine_ls_R_factor_all          0.0291
_refine_ls_R_factor_gt           0.0276
_refine_ls_restrained_S_all      1.049
_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)+(0.0647P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0785
_refine_ls_wR_factor_ref         0.0792
_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. Rigid bond restraints
 O3, C2
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.005
3. Uiso/Uaniso restraints and constraints
O3 \\sim C2: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.01
Uanis(O1B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C1A, N3, C2A, C3A, O10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O10, C1B, N3, C3B, C2B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. 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)
6.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C8(H8), C10(H10), C12(H12A), C13(H13), C14(H14), C1A(H1AA), C1B(H1BA)
6.b Tetrahedral OH refined with riding coordinates:
 O1B(H1B)
6.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)
6.d Idealised tetrahedral OH refined as rotating group:
 O9(H9), O12(H12), O1A(H1A)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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 0.09680(2) 0.54694(2) 0.68285(2) 0.02564(9) Uani 1 1 d . . . . .
O2 O -0.0311(3) 0.3351(2) 0.5872(2) 0.0297(6) Uani 1 1 d . . . . .
O3 O 0.1564(3) 0.4875(2) 0.5177(2) 0.0327(5) Uani 1 1 d . U . . .
O4 O -0.0789(3) 0.2740(2) 0.3923(2) 0.0338(6) Uani 1 1 d . . . . .
O5 O 0.0598(3) 0.4839(3) 0.8405(2) 0.0401(6) Uani 1 1 d . . . . .
O6 O 0.1288(2) 0.4250(2) 0.3300(2) 0.0343(6) Uani 1 1 d . . . . .
O7 O 0.1670(3) 0.7617(2) 0.8508(2) 0.0354(6) Uani 1 1 d . . . . .
O8 O 0.3217(3) 0.6822(2) 0.7857(2) 0.0390(6) Uani 1 1 d . . . . .
O9 O 0.0452(4) -0.0489(3) 0.7130(3) 0.0536(9) Uani 1 1 d . . . . .
H9 H 0.0369 -0.1281 0.7047 0.080 Uiso 1 1 calc GR . . . .
O11 O 0.2536(3) 0.4082(3) 0.7371(3) 0.0501(8) Uani 1 1 d . . . . .
O12 O 0.6625(3) 0.6046(4) 0.7360(3) 0.0520(8) Uani 1 1 d . . . . .
H12 H 0.7457 0.6073 0.7463 0.078 Uiso 1 1 calc GR . . . .
N1 N -0.0105(4) 0.3098(3) 0.8913(3) 0.0451(9) Uani 1 1 d . . . . .
O1A O 0.2345(3) 1.0019(3) 0.9952(3) 0.0420(11) Uani 0.864(9) 1 d . . P A 1
H1A H 0.1807 0.9310 0.9531 0.063 Uiso 0.864(9) 1 calc GR . P A 1
O1B O 0.590(2) 0.798(2) 0.882(2) 0.062(9) Uani 0.136(9) 1 d . U P A 2
H1B H 0.5276 0.7326 0.8395 0.093 Uiso 0.136(9) 1 calc R . P A 2
N2 N 0.4304(4) 0.3318(4) 0.8312(4) 0.0538(10) Uani 1 1 d . . . . .
C1 C -0.0256(4) 0.1209(3) 0.4933(3) 0.0305(8) Uani 1 1 d . . . . .
C2 C 0.2057(4) 0.4642(3) 0.4379(4) 0.0315(6) Uani 1 1 d . U . . .
C3 C 0.3574(4) 0.4818(3) 0.4674(3) 0.0305(8) Uani 1 1 d . . . . .
C4 C -0.0472(3) 0.2531(3) 0.4905(3) 0.0293(8) Uani 1 1 d . . . . .
C5 C 0.4433(4) 0.5350(4) 0.5865(4) 0.0360(9) Uani 1 1 d . . . . .
H5 H 0.4044 0.5591 0.6454 0.043 Uiso 1 1 calc R . . . .
C6 C 0.5858(4) 0.5523(4) 0.6182(3) 0.0344(9) Uani 1 1 d . . . . .
C7 C 0.2889(4) 0.7719(3) 0.8493(3) 0.0309(8) Uani 1 1 d . . . . .
C8 C -0.0021(4) 0.0908(3) 0.5965(3) 0.0358(9) Uani 1 1 d . . . . .
H8 H -0.0035 0.1532 0.6637 0.043 Uiso 1 1 calc R . . . .
C9 C 0.0240(4) -0.0292(3) 0.6058(3) 0.0344(8) Uani 1 1 d . . . . .
C10 C -0.0298(5) 0.3881(4) 0.8276(4) 0.0424(10) Uani 1 1 d . . . . .
H10 H -0.1170 0.3719 0.7676 0.051 Uiso 1 1 calc R . . . .
N3 N 0.4764(5) 0.1530(4) 0.4543(5) 0.0663(12) Uani 1 1 d . U . . .
C11 C 0.3970(4) 0.8915(3) 0.9283(3) 0.0318(8) Uani 1 1 d . . . . .
C12 C 0.3640(4) 0.9965(3) 0.9955(3) 0.0342(8) Uani 1 1 d . . . . .
H12A H 0.2723 0.9943 0.9924 0.041 Uiso 0.136(9) 1 calc R . P A 2
C13 C 0.3730(5) 0.4233(5) 0.7966(4) 0.0483(11) Uani 1 1 d . . . . .
H13 H 0.4300 0.5065 0.8202 0.058 Uiso 1 1 calc R . . . .
C14 C 0.5319(4) 0.8951(3) 0.9324(3) 0.0326(8) Uani 1 1 d . . . . .
H14 H 0.5530 0.8234 0.8860 0.039 Uiso 0.864(9) 1 calc R . P A 1
C15 C -0.1198(7) 0.2007(5) 0.8726(6) 0.0659(15) Uani 1 1 d . . . . .
H15A H -0.1457 0.2140 0.9424 0.099 Uiso 1 1 calc GR . . . .
H15B H -0.0867 0.1207 0.8587 0.099 Uiso 1 1 calc GR . . . .
H15C H -0.1998 0.1950 0.8041 0.099 Uiso 1 1 calc GR . . . .
O10 O 0.6086(7) 0.2248(6) 0.6471(5) 0.1046(18) Uani 1 1 d . U . . .
C16 C 0.1159(7) 0.3284(6) 0.9888(6) 0.0792(19) Uani 1 1 d . . . . .
H16A H 0.1748 0.4118 1.0041 0.119 Uiso 1 1 calc GR . . . .
H16B H 0.1634 0.2594 0.9690 0.119 Uiso 1 1 calc GR . . . .
H16C H 0.0950 0.3265 1.0591 0.119 Uiso 1 1 calc GR . . . .
C17 C 0.3561(7) 0.2017(6) 0.7989(6) 0.0782(18) Uani 1 1 d . . . . .
H17A H 0.3387 0.1862 0.8671 0.117 Uiso 1 1 calc GR . . . .
H17B H 0.4102 0.1420 0.7728 0.117 Uiso 1 1 calc GR . . . .
H17C H 0.2686 0.1879 0.7349 0.117 Uiso 1 1 calc GR . . . .
C18 C 0.5770(7) 0.3624(7) 0.9021(6) 0.085(2) Uani 1 1 d . . . . .
H18A H 0.6237 0.3064 0.8609 0.127 Uiso 1 1 calc GR . . . .
H18B H 0.5890 0.3485 0.9784 0.127 Uiso 1 1 calc GR . . . .
H18C H 0.6162 0.4526 0.9145 0.127 Uiso 1 1 calc GR . . . .
C1A C 0.5978(13) 0.1931(11) 0.5428(10) 0.074(3) Uani 0.597(10) 1 d . U P B 1
H1AA H 0.6789 0.1974 0.5244 0.089 Uiso 0.597(10) 1 calc R . P B 1
C2A C 0.4629(18) 0.1129(14) 0.3318(11) 0.092(4) Uani 0.597(10) 1 d . U P B 1
H2AA H 0.5508 0.1427 0.3248 0.138 Uiso 0.597(10) 1 calc GR . P B 1
H2AB H 0.3926 0.1502 0.2871 0.138 Uiso 0.597(10) 1 calc GR . P B 1
H2AC H 0.4362 0.0187 0.3004 0.138 Uiso 0.597(10) 1 calc GR . P B 1
C3A C 0.3450(13) 0.1385(12) 0.4748(12) 0.084(3) Uani 0.597(10) 1 d . U P B 1
H3AA H 0.2916 0.0501 0.4333 0.126 Uiso 0.597(10) 1 calc GR . P B 1
H3AB H 0.2929 0.1988 0.4454 0.126 Uiso 0.597(10) 1 calc GR . P B 1
H3AC H 0.3633 0.1570 0.5593 0.126 Uiso 0.597(10) 1 calc GR . P B 1
C1B C 0.497(2) 0.201(2) 0.5618(16) 0.093(5) Uani 0.403(10) 1 d . U P B 2
H1BA H 0.4196 0.2215 0.5809 0.112 Uiso 0.403(10) 1 calc R . P B 2
C2B C 0.603(2) 0.144(2) 0.425(2) 0.104(6) Uani 0.403(10) 1 d . U P B 2
H2BA H 0.6764 0.2181 0.4775 0.155 Uiso 0.403(10) 1 calc GR . P B 2
H2BB H 0.5833 0.1438 0.3430 0.155 Uiso 0.403(10) 1 calc GR . P B 2
H2BC H 0.6305 0.0642 0.4335 0.155 Uiso 0.403(10) 1 calc GR . P B 2
C3B C 0.345(2) 0.1205(18) 0.3619(17) 0.086(5) Uani 0.403(10) 1 d . U P B 2
H3BA H 0.2757 0.1455 0.3955 0.129 Uiso 0.403(10) 1 calc GR . P B 2
H3BB H 0.3198 0.0275 0.3221 0.129 Uiso 0.403(10) 1 calc GR . P B 2
H3BC H 0.3485 0.1665 0.3052 0.129 Uiso 0.403(10) 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 2.344(2) . ?
Tb1 O3 2.315(3) . ?
Tb1 O4 2.391(2) 2_566 ?
Tb1 O5 2.381(3) . ?
Tb1 O6 2.392(3) 2_566 ?
Tb1 O7 2.582(3) . ?
Tb1 O8 2.397(3) . ?
Tb1 O11 2.438(3) . ?
O2 C4 1.265(4) . ?
O3 C2 1.252(5) . ?
O4 Tb1 2.391(2) 2_566 ?
O4 C4 1.262(5) . ?
O5 C10 1.266(5) . ?
O6 Tb1 2.392(3) 2_566 ?
O6 C2 1.272(5) . ?
O7 C7 1.280(5) . ?
O8 C7 1.260(5) . ?
O9 H9 0.8400 . ?
O9 C9 1.372(5) . ?
O11 C13 1.211(5) . ?
O12 H12 0.8400 . ?
O12 C6 1.374(5) . ?
N1 C10 1.308(5) . ?
N1 C15 1.472(7) . ?
N1 C16 1.450(7) . ?
O1A H1A 0.8400 . ?
O1A C12 1.369(5) . ?
O1B H1B 0.8400 . ?
O1B C14 1.40(2) . ?
N2 C13 1.330(5) . ?
N2 C17 1.434(7) . ?
N2 C18 1.467(7) . ?
C1 C4 1.505(4) . ?
C1 C8 1.374(5) . ?
C1 C9 1.398(5) 2_556 ?
C2 C3 1.498(5) . ?
C3 C5 1.410(5) . ?
C3 C6 1.381(7) 2_666 ?
C5 H5 0.9500 . ?
C5 C6 1.400(5) . ?
C6 C3 1.381(7) 2_666 ?
C7 C11 1.510(4) . ?
C8 H8 0.9500 . ?
C8 C9 1.406(5) . ?
C9 C1 1.398(5) 2_556 ?
C10 H10 0.9500 . ?
N3 C1A 1.338(12) . ?
N3 C2A 1.448(14) . ?
N3 C3A 1.481(13) . ?
N3 C1B 1.26(2) . ?
N3 C2B 1.49(2) . ?
N3 C3B 1.437(17) . ?
C11 C12 1.400(6) . ?
C11 C14 1.399(6) . ?
C12 H12A 0.9500 . ?
C12 C14 1.399(5) 2_677 ?
C13 H13 0.9500 . ?
C14 C12 1.399(5) 2_677 ?
C14 H14 0.9500 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
O10 C1A 1.234(13) . ?
O10 C1B 1.27(2) . ?
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 126.67(8) . 2_566 ?
O2 Tb1 O5 77.95(9) . . ?
O2 Tb1 O6 78.82(9) . 2_566 ?
O2 Tb1 O7 151.45(9) . . ?
O2 Tb1 O8 145.78(9) . . ?
O2 Tb1 O11 74.05(10) . . ?
O3 Tb1 O2 77.27(9) . . ?
O3 Tb1 O4 76.08(9) . 2_566 ?
O3 Tb1 O5 145.84(9) . . ?
O3 Tb1 O6 122.05(9) . 2_566 ?
O3 Tb1 O7 131.21(9) . . ?
O3 Tb1 O8 88.23(9) . . ?
O3 Tb1 O11 78.64(11) . . ?
O4 Tb1 O6 77.63(9) 2_566 2_566 ?
O4 Tb1 O7 68.70(8) 2_566 . ?
O4 Tb1 O8 77.80(9) 2_566 . ?
O4 Tb1 O11 141.44(11) 2_566 . ?
O5 Tb1 O4 138.04(10) . 2_566 ?
O5 Tb1 O6 75.04(10) . 2_566 ?
O5 Tb1 O7 76.57(9) . . ?
O5 Tb1 O8 99.47(10) . . ?
O5 Tb1 O11 72.19(11) . . ?
O6 Tb1 O7 82.36(9) 2_566 . ?
O6 Tb1 O8 134.09(9) 2_566 . ?
O6 Tb1 O11 140.91(11) 2_566 . ?
O8 Tb1 O7 52.63(9) . . ?
O8 Tb1 O11 72.76(10) . . ?
O11 Tb1 O7 109.63(10) . . ?
C4 O2 Tb1 133.3(2) . . ?
C2 O3 Tb1 171.7(2) . . ?
C4 O4 Tb1 138.6(2) . 2_566 ?
C10 O5 Tb1 124.5(3) . . ?
C2 O6 Tb1 108.2(2) . 2_566 ?
C7 O7 Tb1 88.4(2) . . ?
C7 O8 Tb1 97.4(2) . . ?
C9 O9 H9 109.5 . . ?
C13 O11 Tb1 136.4(3) . . ?
C6 O12 H12 109.5 . . ?
C10 N1 C15 121.6(4) . . ?
C10 N1 C16 122.7(4) . . ?
C16 N1 C15 115.6(4) . . ?
C12 O1A H1A 109.5 . . ?
C14 O1B H1B 109.5 . . ?
C13 N2 C17 122.9(5) . . ?
C13 N2 C18 119.4(5) . . ?
C17 N2 C18 117.7(5) . . ?
C8 C1 C4 119.5(3) . . ?
C8 C1 C9 119.1(3) . 2_556 ?
C9 C1 C4 121.3(3) 2_556 . ?
O3 C2 O6 121.2(3) . . ?
O3 C2 C3 120.7(3) . . ?
O6 C2 C3 118.1(4) . . ?
C5 C3 C2 118.2(4) . . ?
C6 C3 C2 122.0(3) 2_666 . ?
C6 C3 C5 119.8(3) 2_666 . ?
O2 C4 C1 117.3(3) . . ?
O4 C4 O2 125.0(3) . . ?
O4 C4 C1 117.7(3) . . ?
C3 C5 H5 119.9 . . ?
C6 C5 C3 120.1(4) . . ?
C6 C5 H5 119.9 . . ?
O12 C6 C3 123.3(3) . 2_666 ?
O12 C6 C5 116.7(4) . . ?
C3 C6 C5 120.0(4) 2_666 . ?
O7 C7 C11 119.6(3) . . ?
O8 C7 O7 121.2(3) . . ?
O8 C7 C11 119.2(3) . . ?
C1 C8 H8 118.9 . . ?
C1 C8 C9 122.2(4) . . ?
C9 C8 H8 118.9 . . ?
O9 C9 C1 124.2(3) . 2_556 ?
O9 C9 C8 117.1(3) . . ?
C1 C9 C8 118.7(3) 2_556 . ?
O5 C10 N1 124.4(4) . . ?
O5 C10 H10 117.8 . . ?
N1 C10 H10 117.8 . . ?
C1A N3 C2A 123.0(10) . . ?
C1A N3 C3A 122.2(8) . . ?
C2A N3 C3A 114.6(9) . . ?
C1B N3 C2B 115.5(15) . . ?
C1B N3 C3B 124.2(15) . . ?
C3B N3 C2B 119.9(13) . . ?
C12 C11 C7 121.2(3) . . ?
C14 C11 C7 118.3(3) . . ?
C14 C11 C12 120.5(3) . . ?
O1A C12 C11 124.3(3) . . ?
O1A C12 C14 116.7(3) . 2_677 ?
C11 C12 H12A 120.5 . . ?
C14 C12 C11 119.0(4) 2_677 . ?
C14 C12 H12A 120.5 2_677 . ?
O11 C13 N2 124.8(5) . . ?
O11 C13 H13 117.6 . . ?
N2 C13 H13 117.6 . . ?
O1B C14 C11 130.0(11) . . ?
O1B C14 C12 109.2(10) . 2_677 ?
C11 C14 C12 120.5(3) . 2_677 ?
C11 C14 H14 119.7 . . ?
C12 C14 H14 119.7 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 118.6 . . ?
O10 C1A N3 122.7(11) . . ?
O10 C1A H1AA 118.6 . . ?
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 O10 127(2) . . ?
N3 C1B H1BA 116.6 . . ?
O10 C1B H1BA 116.6 . . ?
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 -50.6(5) . . . . ?
Tb1 O2 C4 C1 128.8(3) . . . . ?
Tb1 O4 C4 O2 11.2(6) 2_566 . . . ?
Tb1 O4 C4 C1 -168.3(3) 2_566 . . . ?
Tb1 O5 C10 N1 140.1(4) . . . . ?
Tb1 O6 C2 O3 12.3(4) 2_566 . . . ?
Tb1 O6 C2 C3 -167.7(2) 2_566 . . . ?
Tb1 O7 C7 O8 -6.2(4) . . . . ?
Tb1 O7 C7 C11 176.1(3) . . . . ?
Tb1 O8 C7 O7 6.7(4) . . . . ?
Tb1 O8 C7 C11 -175.5(3) . . . . ?
Tb1 O11 C13 N2 166.5(4) . . . . ?
O3 C2 C3 C5 -5.0(5) . . . . ?
O3 C2 C3 C6 175.0(3) . . . 2_666 ?
O6 C2 C3 C5 175.0(3) . . . . ?
O6 C2 C3 C6 -5.0(5) . . . 2_666 ?
O7 C7 C11 C12 -5.8(5) . . . . ?
O7 C7 C11 C14 174.4(3) . . . . ?
O8 C7 C11 C12 176.4(4) . . . . ?
O8 C7 C11 C14 -3.3(5) . . . . ?
C1 C8 C9 O9 -179.6(4) . . . . ?
C1 C8 C9 C1 -0.2(7) . . . 2_556 ?
C2 C3 C5 C6 179.5(3) . . . . ?
C3 C5 C6 O12 -180.0(4) . . . . ?
C3 C5 C6 C3 0.5(6) . . . 2_666 ?
C4 C1 C8 C9 -177.5(4) . . . . ?
C6 C3 C5 C6 -0.5(6) 2_666 . . . ?
C7 C11 C12 O1A -0.9(6) . . . . ?
C7 C11 C12 C14 179.9(3) . . . 2_677 ?
C7 C11 C14 O1B -6.6(18) . . . . ?
C7 C11 C14 C12 -179.8(3) . . . 2_677 ?
C8 C1 C4 O2 5.9(5) . . . . ?
C8 C1 C4 O4 -174.7(4) . . . . ?
C9 C1 C4 O2 -171.8(4) 2_556 . . . ?
C9 C1 C4 O4 7.6(5) 2_556 . . . ?
C9 C1 C8 C9 0.2(7) 2_556 . . . ?
C12 C11 C14 O1B 173.6(17) . . . . ?
C12 C11 C14 C12 0.4(6) . . . 2_677 ?
C14 C11 C12 O1A 178.8(4) . . . . ?
C14 C11 C12 C14 -0.4(6) . . . 2_677 ?
C15 N1 C10 O5 179.3(5) . . . . ?
C16 N1 C10 O5 3.0(8) . . . . ?
C17 N2 C13 O11 1.5(8) . . . . ?
C18 N2 C13 O11 179.3(6) . . . . ?
C2A N3 C1A O10 -178.5(10) . . . . ?
C3A N3 C1A O10 -2.5(15) . . . . ?
C2B N3 C1B O10 -11(3) . . . . ?
C3B N3 C1B O10 175.8(16) . . . . ?

_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 1.142
_oxdiff_exptl_absorpt_empirical_full_min 0.897

# start Validation Reply Form
_vrf_PLAT029_SION2_160K          
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.729 Why?  
RESPONSE: The data were collected upon the spindle rotation. Therefore, a 
		  limited portion of the reciprocal space could be probed.
;
# 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 
# 
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# Please retain this information to preserve the provenance of 
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data_SION2_280K
_database_code_depnum_ccdc_archive 'CCDC 1871310'
loop_
_audit_author_name
_audit_author_address
'Andrzej Gladysiak'
;Ecole polytechnique f?d?rale de Lausanne
Switzerland
;
_audit_update_record             
;
2018-10-03 deposited with the CCDC.	2019-08-12 downloaded from the CCDC.
;
_audit_creation_date             2018-07-09
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_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          ?
_chemical_oxdiff_formula         'C21 H27 N3 O12 Tb'
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                   10.5333(6)
_cell_length_b                   11.0035(5)
_cell_length_c                   12.7511(5)
_cell_angle_alpha                103.784(5)
_cell_angle_beta                 110.271(4)
_cell_angle_gamma                96.437(4)
_cell_volume                     1315.34(12)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5642
_cell_measurement_temperature    280.0
_cell_measurement_theta_max      31.7030
_cell_measurement_theta_min      1.9420
_shelx_estimated_absorpt_T_max   0.831
_shelx_estimated_absorpt_T_min   0.609
_exptl_absorpt_coefficient_mu    2.753
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77864
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.698
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             670
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0169
_diffrn_reflns_av_unetI/netI     0.0251
_diffrn_reflns_Laue_measured_fraction_full 0.743
_diffrn_reflns_Laue_measured_fraction_max 0.679
_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       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8650
_diffrn_reflns_point_group_measured_fraction_full 0.743
_diffrn_reflns_point_group_measured_fraction_max 0.679
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.431
_diffrn_reflns_theta_min         1.960
_diffrn_ambient_temperature      280.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            PILATUS2M
_diffrn_measured_fraction_theta_full 0.743
_diffrn_measured_fraction_theta_max 0.679
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      0.00 360.00   1.00    1.00    --    0.00   0.00   0.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  PILATUS@SNBL
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0614524000
_diffrn_orient_matrix_UB_12      -0.0145441000
_diffrn_orient_matrix_UB_13      0.0363453000
_diffrn_orient_matrix_UB_21      -0.0296301000
_diffrn_orient_matrix_UB_22      -0.0668469000
_diffrn_orient_matrix_UB_23      -0.0268099000
_diffrn_orient_matrix_UB_31      0.0286378000
_diffrn_orient_matrix_UB_32      -0.0001896000
_diffrn_orient_matrix_UB_33      -0.0432552000
_diffrn_radiation_monochromator  'Si (111)'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           ?
_diffrn_radiation_wavelength     0.7142
_diffrn_source                   
'European Synchrotron Radiation Facility, BM01 beamline'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4217
_reflns_number_total             4430
_reflns_odcompleteness_completeness 73.09
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.51
_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 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (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    'XT (Sheldrick, 2015)'
_refine_diff_density_max         1.159
_refine_diff_density_min         -1.195
_refine_diff_density_rms         0.082
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         4430
_refine_ls_number_restraints     127
_refine_ls_R_factor_all          0.0272
_refine_ls_R_factor_gt           0.0259
_refine_ls_restrained_S_all      1.085
_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)+(0.0470P)²+0.6549P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0693
_refine_ls_wR_factor_ref         0.0698
_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
 C18A-N2 \\sim N2-C18B
 with sigma of 0.01
 C17B-N2 \\sim N2-C17A
 with sigma of 0.01
 C13B-N2 \\sim N2-C13A
 with sigma of 0.01
 C13B-O11B \\sim O11A-C13A
 with sigma of 0.01
 C18B-C17B \\sim C17A-C18A
 with sigma of 0.01
3. Restrained planarity
 C13B, C17B, C18B, N2, O11B
 with sigma of 0.1
 C13A, C17A, C18A, N2, O11A
 with sigma of 0.1
4. Rigid bond restraints
 C2, O3
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.005
5. Uiso/Uaniso restraints and constraints
C2 \\sim O3: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.01
Uanis(O1B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C15) \\sim Ueq, Uanis(C16) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C1A) = Uanis(C1B)
Uanis(C3A) = Uanis(C3B)
Uanis(C2A) = Uanis(C2B)
Uanis(O1A) = Uanis(O1B)
Uanis(O11B) = Uanis(O11A)
Uanis(C13A) = Uanis(C13B)
Uanis(C18B) = Uanis(C18A)
Uanis(C17B) = Uanis(C17A)
6. Rigid body (RIGU) restrains
 C1A, C2A, C3A, N3, O10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1B, C2B, C3B, N3, O10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C13A, C17A, C18A, N2, O11A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C13B, C17B, C18B, N2, O11B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. 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(H12)=Sof(O1B)=Sof(H1B)=1-FVAR(2)
 Sof(H14)=Sof(O1A)=Sof(H1A)=FVAR(2)
 Sof(C13B)=Sof(H13B)=Sof(C17B)=Sof(H17D)=Sof(H17E)=Sof(H17F)=Sof(C18B)=
 Sof(H18D)=Sof(H18E)=Sof(H18F)=Sof(O11B)=1-FVAR(3)
 Sof(C13A)=Sof(H13A)=Sof(C17A)=Sof(H17A)=Sof(H17B)=Sof(H17C)=Sof(C18A)=
 Sof(H18A)=Sof(H18B)=Sof(H18C)=Sof(O11A)=FVAR(3)
8.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C8(H8), C10(H10), C12(H12), C13A(H13A), C13B(H13B), C14(H14),
 C1A(H1AA), C1B(H1BA)
8.b Tetrahedral OH refined with riding coordinates:
 O1B(H1B)
8.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17A(H17A,H17B,H17C), C17B(H17D,
 H17E,H17F), C18A(H18A,H18B,H18C), C18B(H18D,H18E,H18F), C2A(H2AA,H2AB,H2AC),
 C2B(H2BA,H2BB,H2BC), C3A(H3AA,H3AB,H3AC), C3B(H3BA,H3BB,H3BC)
8.d Idealised tetrahedral OH refined as rotating group:
 O1A(H1A), O9(H9), O12(H12A)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
C1 C -0.0220(4) 0.1214(3) 0.4935(3) 0.0377(8) Uani 1 1 d . . . . .
C2 C 0.2065(4) 0.4693(3) 0.4418(4) 0.0399(6) Uani 1 1 d . U . . .
C3 C 0.3581(4) 0.4850(3) 0.4699(3) 0.0361(8) Uani 1 1 d . . . . .
C4 C -0.0384(4) 0.2544(3) 0.4925(3) 0.0350(8) Uani 1 1 d . . . . .
C5 C 0.4492(4) 0.5352(4) 0.5871(4) 0.0446(9) Uani 1 1 d . . . . .
H5 H 0.4150 0.5587 0.6454 0.054 Uiso 1 1 calc R . . . .
C6 C 0.5914(4) 0.5500(4) 0.6162(3) 0.0426(9) Uani 1 1 d . . . . .
C7 C 0.2949(4) 0.7712(3) 0.8473(3) 0.0395(9) Uani 1 1 d . . . . .
C8 C 0.0016(5) 0.0895(3) 0.5960(4) 0.0481(10) Uani 1 1 d . . . . .
H8 H 0.0028 0.1502 0.6612 0.058 Uiso 1 1 calc R . . . .
C9 C 0.0235(5) -0.0301(3) 0.6045(3) 0.0464(10) Uani 1 1 d . . . . .
C10 C -0.0180(6) 0.3871(5) 0.8256(4) 0.0611(12) Uani 1 1 d . . . . .
H10 H -0.1037 0.3699 0.7642 0.073 Uiso 1 1 calc R . . . .
C11 C 0.3993(4) 0.8906(3) 0.9266(3) 0.0402(9) Uani 1 1 d . . . . .
C12 C 0.3642(4) 0.9890(4) 0.9960(4) 0.0425(9) Uani 1 1 d . . . . .
H12 H 0.2741 0.9820 0.9930 0.051 Uiso 0.117(6) 1 calc R . P A 2
C13A C 0.3856(7) 0.4264(7) 0.8002(6) 0.0633(18) Uani 0.689(9) 1 d D U P B 1
H13A H 0.4474 0.5046 0.8257 0.076 Uiso 0.689(9) 1 calc R . P B 1
C13B C 0.3062(12) 0.3366(16) 0.7558(13) 0.0633(18) Uani 0.311(9) 1 d D U P B 2
H13B H 0.2443 0.2583 0.7147 0.076 Uiso 0.311(9) 1 calc R . P B 2
C14 C 0.5342(4) 0.9024(4) 0.9305(3) 0.0437(9) Uani 1 1 d . . . . .
H14 H 0.5565 0.8370 0.8833 0.052 Uiso 0.883(6) 1 calc R . P A 1
C15 C -0.1099(9) 0.2072(8) 0.8749(8) 0.117(3) Uani 1 1 d . U . . .
H15A H -0.1289 0.2188 0.9446 0.176 Uiso 1 1 calc GR . . . .
H15B H -0.0808 0.1278 0.8579 0.176 Uiso 1 1 calc GR . . . .
H15C H -0.1923 0.2055 0.8106 0.176 Uiso 1 1 calc GR . . . .
C16 C 0.1253(11) 0.3316(10) 0.9881(8) 0.149(4) Uani 1 1 d . U . . .
H16A H 0.1605 0.4217 1.0269 0.224 Uiso 1 1 calc GR . . . .
H16B H 0.1912 0.2962 0.9606 0.224 Uiso 1 1 calc GR . . . .
H16C H 0.1098 0.2899 1.0421 0.224 Uiso 1 1 calc GR . . . .
C17A C 0.3574(13) 0.2014(11) 0.7999(14) 0.134(5) Uani 0.689(9) 1 d D U P B 1
H17A H 0.3533 0.1854 0.8696 0.201 Uiso 0.689(9) 1 calc GR . P B 1
H17B H 0.4002 0.1398 0.7653 0.201 Uiso 0.689(9) 1 calc GR . P B 1
H17C H 0.2652 0.1942 0.7453 0.201 Uiso 0.689(9) 1 calc GR . P B 1
C17B C 0.419(3) 0.1896(13) 0.807(3) 0.134(5) Uani 0.311(9) 1 d D U P B 2
H17D H 0.3540 0.1599 0.8376 0.201 Uiso 0.311(9) 1 calc GR . P B 2
H17E H 0.5062 0.1694 0.8440 0.201 Uiso 0.311(9) 1 calc GR . P B 2
H17F H 0.3839 0.1485 0.7238 0.201 Uiso 0.311(9) 1 calc GR . P B 2
C18A C 0.5867(12) 0.3505(14) 0.8989(15) 0.136(5) Uani 0.689(9) 1 d D U P B 1
H18A H 0.6300 0.4340 0.9031 0.204 Uiso 0.689(9) 1 calc GR . P B 1
H18B H 0.6264 0.2871 0.8626 0.204 Uiso 0.689(9) 1 calc GR . P B 1
H18C H 0.6013 0.3463 0.9765 0.204 Uiso 0.689(9) 1 calc GR . P B 1
C18B C 0.5758(18) 0.403(2) 0.902(3) 0.136(5) Uani 0.311(9) 1 d D U P B 2
H18D H 0.5915 0.4758 0.8750 0.204 Uiso 0.311(9) 1 calc GR . P B 2
H18E H 0.6429 0.3523 0.8969 0.204 Uiso 0.311(9) 1 calc GR . P B 2
H18F H 0.5845 0.4325 0.9818 0.204 Uiso 0.311(9) 1 calc GR . P B 2
N1 N -0.0008(5) 0.3124(4) 0.8923(4) 0.0696(12) Uani 1 1 d . . . . .
N2 N 0.4356(6) 0.3256(5) 0.8285(5) 0.0861(15) Uani 1 1 d D U . . .
O1A O 0.2358(4) 0.9863(4) 0.9962(4) 0.0604(11) Uani 0.883(6) 1 d . . P A 1
H1A H 0.1853 0.9166 0.9542 0.091 Uiso 0.883(6) 1 calc GR . P A 1
O1B O 0.596(3) 0.809(3) 0.884(3) 0.0604(11) Uani 0.117(6) 1 d . U P A 2
H1B H 0.5370 0.7438 0.8430 0.091 Uiso 0.117(6) 1 calc R . P A 2
O2 O -0.0175(3) 0.3351(2) 0.5875(2) 0.0401(6) Uani 1 1 d . . . . .
O3 O 0.1619(3) 0.4939(2) 0.5218(3) 0.0416(5) Uani 1 1 d . U . . .
O4 O -0.0724(3) 0.2764(2) 0.3944(2) 0.0419(6) Uani 1 1 d . . . . .
O5 O 0.0702(3) 0.4791(3) 0.8369(2) 0.0524(7) Uani 1 1 d . . . . .
O6 O 0.1246(3) 0.4319(3) 0.3353(2) 0.0445(6) Uani 1 1 d . . . . .
O7 O 0.1743(3) 0.7545(3) 0.8483(2) 0.0449(6) Uani 1 1 d . . . . .
O8 O 0.3282(3) 0.6881(3) 0.7821(3) 0.0565(8) Uani 1 1 d . . . . .
O9 O 0.0467(5) -0.0517(3) 0.7093(3) 0.0755(12) Uani 1 1 d . . . . .
H9 H 0.0610 -0.1240 0.7054 0.113 Uiso 1 1 calc GR . . . .
O11A O 0.274(3) 0.421(3) 0.7479(17) 0.0742(18) Uani 0.689(9) 1 d D U P B 1
O11B O 0.261(6) 0.420(6) 0.737(4) 0.0742(18) Uani 0.311(9) 1 d D U P B 2
O12 O 0.6743(3) 0.5996(4) 0.7328(3) 0.0688(10) Uani 1 1 d . . . . .
H12A H 0.7547 0.5961 0.7422 0.103 Uiso 1 1 calc GR . . . .
Tb1 Tb 0.10340(2) 0.54731(2) 0.68257(2) 0.02992(8) Uani 1 1 d . . . . .
C1A C 0.604(3) 0.191(2) 0.539(2) 0.137(4) Uani 0.507(9) 1 d . U P C 1
H1AA H 0.6826 0.1900 0.5222 0.165 Uiso 0.507(9) 1 calc R . P C 1
C1B C 0.503(3) 0.204(2) 0.563(2) 0.137(4) Uani 0.493(9) 1 d . U P C 2
H1BA H 0.4288 0.2237 0.5824 0.165 Uiso 0.493(9) 1 calc R . P C 2
C2A C 0.453(3) 0.111(2) 0.330(2) 0.152(5) Uani 0.507(9) 1 d . U P C 1
H2AA H 0.5291 0.1517 0.3167 0.227 Uiso 0.507(9) 1 calc GR . P C 1
H2AB H 0.3692 0.1320 0.2861 0.227 Uiso 0.507(9) 1 calc GR . P C 1
H2AC H 0.4446 0.0194 0.3058 0.227 Uiso 0.507(9) 1 calc GR . P C 1
C2B C 0.601(3) 0.142(2) 0.419(2) 0.152(5) Uani 0.493(9) 1 d . U P C 2
H2BA H 0.6605 0.2245 0.4457 0.227 Uiso 0.493(9) 1 calc GR . P C 2
H2BB H 0.5694 0.1082 0.3359 0.227 Uiso 0.493(9) 1 calc GR . P C 2
H2BC H 0.6501 0.0847 0.4556 0.227 Uiso 0.493(9) 1 calc GR . P C 2
C3A C 0.348(2) 0.143(2) 0.475(2) 0.141(4) Uani 0.507(9) 1 d . U P C 1
H3AA H 0.3124 0.0555 0.4652 0.211 Uiso 0.507(9) 1 calc GR . P C 1
H3AB H 0.2810 0.1737 0.4198 0.211 Uiso 0.507(9) 1 calc GR . P C 1
H3AC H 0.3673 0.1944 0.5528 0.211 Uiso 0.507(9) 1 calc GR . P C 1
C3B C 0.347(3) 0.114(2) 0.357(2) 0.141(4) Uani 0.493(9) 1 d . U P C 2
H3BA H 0.2785 0.1469 0.3829 0.211 Uiso 0.493(9) 1 calc GR . P C 2
H3BB H 0.3209 0.0223 0.3287 0.211 Uiso 0.493(9) 1 calc GR . P C 2
H3BC H 0.3515 0.1470 0.2947 0.211 Uiso 0.493(9) 1 calc GR . P C 2
N3 N 0.4790(8) 0.1531(6) 0.4522(7) 0.111(2) Uani 1 1 d . U . . .
O10 O 0.6161(9) 0.2268(9) 0.6414(7) 0.164(3) Uani 1 1 d . U . . .


_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
C1 C4 1.495(4) . ?
C1 C8 1.381(5) . ?
C1 C9 1.399(5) 2_556 ?
C2 C3 1.489(5) . ?
C2 O3 1.250(5) . ?
C2 O6 1.266(5) . ?
C3 C5 1.398(5) . ?
C3 C6 1.374(6) 2_666 ?
C4 O2 1.250(4) . ?
C4 O4 1.267(4) . ?
C5 H5 0.9300 . ?
C5 C6 1.393(5) . ?
C6 C3 1.374(6) 2_666 ?
C6 O12 1.371(5) . ?
C7 C11 1.494(4) . ?
C7 O7 1.268(5) . ?
C7 O8 1.250(5) . ?
C8 H8 0.9300 . ?
C8 C9 1.384(5) . ?
C9 C1 1.399(5) 2_556 ?
C9 O9 1.356(5) . ?
C10 H10 0.9300 . ?
C10 N1 1.301(6) . ?
C10 O5 1.240(6) . ?
C11 C12 1.397(6) . ?
C11 C14 1.395(6) . ?
C12 H12 0.9300 . ?
C12 C14 1.391(5) 2_677 ?
C12 O1A 1.351(6) . ?
C13A H13A 0.9300 . ?
C13A N2 1.352(7) . ?
C13A O11A 1.12(2) . ?
C13B H13B 0.9300 . ?
C13B N2 1.396(10) . ?
C13B O11B 1.12(2) . ?
C14 C12 1.391(5) 2_677 ?
C14 H14 0.9300 . ?
C14 O1B 1.40(3) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C15 N1 1.454(8) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C16 N1 1.411(9) . ?
C17A H17A 0.9600 . ?
C17A H17B 0.9600 . ?
C17A H17C 0.9600 . ?
C17A N2 1.408(11) . ?
C17B H17D 0.9600 . ?
C17B H17E 0.9600 . ?
C17B H17F 0.9600 . ?
C17B N2 1.433(13) . ?
C18A H18A 0.9600 . ?
C18A H18B 0.9600 . ?
C18A H18C 0.9600 . ?
C18A N2 1.486(11) . ?
C18B H18D 0.9600 . ?
C18B H18E 0.9600 . ?
C18B H18F 0.9600 . ?
C18B N2 1.472(13) . ?
O1A H1A 0.8200 . ?
O1B H1B 0.8200 . ?
O2 Tb1 2.336(2) . ?
O3 Tb1 2.305(3) . ?
O4 Tb1 2.379(2) 2_566 ?
O5 Tb1 2.383(3) . ?
O6 Tb1 2.375(3) 2_566 ?
O7 Tb1 2.539(3) . ?
O8 Tb1 2.403(3) . ?
O9 H9 0.8200 . ?
O11A Tb1 2.436(7) . ?
O11B Tb1 2.324(15) . ?
O12 H12A 0.8200 . ?
Tb1 O4 2.379(2) 2_566 ?
Tb1 O6 2.375(3) 2_566 ?
C1A H1AA 0.9300 . ?
C1A N3 1.33(2) . ?
C1A O10 1.22(3) . ?
C1B H1BA 0.9300 . ?
C1B N3 1.31(3) . ?
C1B O10 1.21(2) . ?
C2A H2AA 0.9600 . ?
C2A H2AB 0.9600 . ?
C2A H2AC 0.9600 . ?
C2A N3 1.43(2) . ?
C2B H2BA 0.9600 . ?
C2B H2BB 0.9600 . ?
C2B H2BC 0.9600 . ?
C2B N3 1.49(3) . ?
C3A H3AA 0.9600 . ?
C3A H3AB 0.9600 . ?
C3A H3AC 0.9600 . ?
C3A N3 1.50(2) . ?
C3B H3BA 0.9600 . ?
C3B H3BB 0.9600 . ?
C3B H3BC 0.9600 . ?
C3B N3 1.43(2) . ?

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
C8 C1 C4 118.9(3) . . ?
C8 C1 C9 118.9(3) . 2_556 ?
C9 C1 C4 122.1(3) 2_556 . ?
O3 C2 C3 120.6(4) . . ?
O3 C2 O6 121.0(3) . . ?
O6 C2 C3 118.4(4) . . ?
C5 C3 C2 118.4(4) . . ?
C6 C3 C2 121.5(3) 2_666 . ?
C6 C3 C5 120.1(3) 2_666 . ?
O2 C4 C1 118.2(3) . . ?
O2 C4 O4 125.0(3) . . ?
O4 C4 C1 116.9(3) . . ?
C3 C5 H5 120.1 . . ?
C6 C5 C3 119.8(4) . . ?
C6 C5 H5 120.1 . . ?
C3 C6 C5 120.2(4) 2_666 . ?
O12 C6 C3 123.3(3) . 2_666 ?
O12 C6 C5 116.5(4) . . ?
O7 C7 C11 119.6(4) . . ?
O8 C7 C11 119.6(4) . . ?
O8 C7 O7 120.8(3) . . ?
C1 C8 H8 119.0 . . ?
C1 C8 C9 122.0(4) . . ?
C9 C8 H8 119.0 . . ?
C8 C9 C1 119.0(4) . 2_556 ?
O9 C9 C1 123.5(3) . 2_556 ?
O9 C9 C8 117.5(4) . . ?
N1 C10 H10 117.2 . . ?
O5 C10 H10 117.2 . . ?
O5 C10 N1 125.5(5) . . ?
C12 C11 C7 121.4(4) . . ?
C14 C11 C7 118.5(4) . . ?
C14 C11 C12 120.1(3) . . ?
C11 C12 H12 120.5 . . ?
C14 C12 C11 119.1(4) 2_677 . ?
C14 C12 H12 120.5 2_677 . ?
O1A C12 C11 124.0(3) . . ?
O1A C12 C14 116.9(4) . 2_677 ?
N2 C13A H13A 118.1 . . ?
O11A C13A H13A 118.1 . . ?
O11A C13A N2 123.7(17) . . ?
N2 C13B H13B 113.3 . . ?
O11B C13B H13B 113.3 . . ?
O11B C13B N2 133(4) . . ?
C11 C14 H14 119.6 . . ?
C11 C14 O1B 129.0(11) . . ?
C12 C14 C11 120.8(4) 2_677 . ?
C12 C14 H14 119.6 2_677 . ?
C12 C14 O1B 109.3(11) 2_677 . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N1 C15 H15A 109.5 . . ?
N1 C15 H15B 109.5 . . ?
N1 C15 H15C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N1 C16 H16A 109.5 . . ?
N1 C16 H16B 109.5 . . ?
N1 C16 H16C 109.5 . . ?
H17A C17A H17B 109.5 . . ?
H17A C17A H17C 109.5 . . ?
H17B C17A H17C 109.5 . . ?
N2 C17A H17A 109.5 . . ?
N2 C17A H17B 109.5 . . ?
N2 C17A H17C 109.5 . . ?
H17D C17B H17E 109.5 . . ?
H17D C17B H17F 109.5 . . ?
H17E C17B H17F 109.5 . . ?
N2 C17B H17D 109.5 . . ?
N2 C17B H17E 109.5 . . ?
N2 C17B H17F 109.5 . . ?
H18A C18A H18B 109.5 . . ?
H18A C18A H18C 109.5 . . ?
H18B C18A H18C 109.5 . . ?
N2 C18A H18A 109.5 . . ?
N2 C18A H18B 109.5 . . ?
N2 C18A H18C 109.5 . . ?
H18D C18B H18E 109.5 . . ?
H18D C18B H18F 109.5 . . ?
H18E C18B H18F 109.5 . . ?
N2 C18B H18D 109.5 . . ?
N2 C18B H18E 109.5 . . ?
N2 C18B H18F 109.5 . . ?
C10 N1 C15 122.5(6) . . ?
C10 N1 C16 121.3(6) . . ?
C16 N1 C15 116.2(6) . . ?
C13A N2 C17A 126.0(7) . . ?
C13A N2 C18A 116.3(8) . . ?
C13B N2 C17B 102.0(13) . . ?
C13B N2 C18B 140.7(13) . . ?
C17A N2 C18A 117.6(8) . . ?
C17B N2 C18B 116.7(12) . . ?
C12 O1A H1A 109.5 . . ?
C14 O1B H1B 109.5 . . ?
C4 O2 Tb1 135.5(2) . . ?
C2 O3 Tb1 174.0(2) . . ?
C4 O4 Tb1 138.9(2) . 2_566 ?
C10 O5 Tb1 126.3(3) . . ?
C2 O6 Tb1 110.5(3) . 2_566 ?
C7 O7 Tb1 89.8(2) . . ?
C7 O8 Tb1 96.6(2) . . ?
C9 O9 H9 109.5 . . ?
C13A O11A Tb1 144(2) . . ?
C13B O11B Tb1 162(6) . . ?
C6 O12 H12A 109.5 . . ?
O2 Tb1 O4 126.26(9) . 2_566 ?
O2 Tb1 O5 77.43(10) . . ?
O2 Tb1 O6 79.27(10) . 2_566 ?
O2 Tb1 O7 151.94(10) . . ?
O2 Tb1 O8 145.40(10) . . ?
O2 Tb1 O11A 75.8(8) . . ?
O3 Tb1 O2 77.18(10) . . ?
O3 Tb1 O4 76.24(9) . 2_566 ?
O3 Tb1 O5 145.76(10) . . ?
O3 Tb1 O6 121.99(9) . 2_566 ?
O3 Tb1 O7 130.88(9) . . ?
O3 Tb1 O8 86.45(11) . . ?
O3 Tb1 O11A 80.1(4) . . ?
O3 Tb1 O11B 78.3(8) . . ?
O4 Tb1 O5 137.88(11) 2_566 . ?
O4 Tb1 O7 69.92(9) 2_566 . ?
O4 Tb1 O8 77.35(11) 2_566 . ?
O4 Tb1 O11A 141.7(7) 2_566 . ?
O5 Tb1 O7 76.68(10) . . ?
O5 Tb1 O8 102.04(11) . . ?
O5 Tb1 O11A 71.7(4) . . ?
O6 Tb1 O4 76.70(10) 2_566 2_566 ?
O6 Tb1 O5 74.75(11) 2_566 . ?
O6 Tb1 O7 83.64(9) 2_566 . ?
O6 Tb1 O8 134.59(10) 2_566 . ?
O6 Tb1 O11A 141.6(7) 2_566 . ?
O8 Tb1 O7 52.50(10) . . ?
O8 Tb1 O11A 71.5(8) . . ?
O11A Tb1 O7 105.9(7) . . ?
O11B Tb1 O2 74(2) . . ?
O11B Tb1 O4 142.0(16) . 2_566 ?
O11B Tb1 O5 72.8(10) . . ?
O11B Tb1 O6 141.3(17) . 2_566 ?
O11B Tb1 O7 108.5(17) . . ?
O11B Tb1 O8 73(2) . . ?
N3 C1A H1AA 119.5 . . ?
O10 C1A H1AA 119.5 . . ?
O10 C1A N3 121(3) . . ?
N3 C1B H1BA 118.1 . . ?
O10 C1B H1BA 118.1 . . ?
O10 C1B N3 124(3) . . ?
H2AA C2A H2AB 109.5 . . ?
H2AA C2A H2AC 109.5 . . ?
H2AB C2A H2AC 109.5 . . ?
N3 C2A H2AA 109.5 . . ?
N3 C2A H2AB 109.5 . . ?
N3 C2A H2AC 109.5 . . ?
H2BA C2B H2BB 109.5 . . ?
H2BA C2B H2BC 109.5 . . ?
H2BB C2B H2BC 109.5 . . ?
N3 C2B H2BA 109.5 . . ?
N3 C2B H2BB 109.5 . . ?
N3 C2B H2BC 109.5 . . ?
H3AA C3A H3AB 109.5 . . ?
H3AA C3A H3AC 109.5 . . ?
H3AB C3A H3AC 109.5 . . ?
N3 C3A H3AA 109.5 . . ?
N3 C3A H3AB 109.5 . . ?
N3 C3A H3AC 109.5 . . ?
H3BA C3B H3BB 109.5 . . ?
H3BA C3B H3BC 109.5 . . ?
H3BB C3B H3BC 109.5 . . ?
N3 C3B H3BA 109.5 . . ?
N3 C3B H3BB 109.5 . . ?
N3 C3B H3BC 109.5 . . ?
C1A N3 C2A 125.4(19) . . ?
C1A N3 C3A 122.0(16) . . ?
C1B N3 C2B 117.7(17) . . ?
C1B N3 C3B 126.5(19) . . ?
C2A N3 C3A 112.5(15) . . ?
C3B N3 C2B 115.7(16) . . ?

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
C1 C4 O2 Tb1 134.2(3) . . . . ?
C1 C4 O4 Tb1 -174.5(3) . . . 2_566 ?
C1 C8 C9 C1 0.2(7) . . . 2_556 ?
C1 C8 C9 O9 179.5(4) . . . . ?
C2 C3 C5 C6 179.5(4) . . . . ?
C3 C2 O6 Tb1 -169.6(2) . . . 2_566 ?
C3 C5 C6 C3 -0.2(7) . . . 2_666 ?
C3 C5 C6 O12 -179.9(4) . . . . ?
C4 C1 C8 C9 -177.2(4) . . . . ?
C6 C3 C5 C6 0.2(7) 2_666 . . . ?
C7 C11 C12 C14 179.2(3) . . . 2_677 ?
C7 C11 C12 O1A -1.2(6) . . . . ?
C7 C11 C14 C12 -179.2(4) . . . 2_677 ?
C7 C11 C14 O1B -11.8(18) . . . . ?
C8 C1 C4 O2 6.4(5) . . . . ?
C8 C1 C4 O4 -173.7(4) . . . . ?
C9 C1 C4 O2 -170.6(4) 2_556 . . . ?
C9 C1 C4 O4 9.3(6) 2_556 . . . ?
C9 C1 C8 C9 -0.1(7) 2_556 . . . ?
C11 C7 O7 Tb1 176.5(3) . . . . ?
C11 C7 O8 Tb1 -176.2(3) . . . . ?
C12 C11 C14 C12 0.8(7) . . . 2_677 ?
C12 C11 C14 O1B 168.2(18) . . . . ?
C14 C11 C12 C14 -0.7(7) . . . 2_677 ?
C14 C11 C12 O1A 178.9(4) . . . . ?
N1 C10 O5 Tb1 144.8(5) . . . . ?
N2 C13A O11A Tb1 169.7(13) . . . . ?
N2 C13B O11B Tb1 -155(8) . . . . ?
O2 C4 O4 Tb1 5.4(6) . . . 2_566 ?
O3 C2 C3 C5 -3.9(5) . . . . ?
O3 C2 C3 C6 175.4(4) . . . 2_666 ?
O3 C2 O6 Tb1 9.7(4) . . . 2_566 ?
O4 C4 O2 Tb1 -45.7(6) . . . . ?
O5 C10 N1 C15 179.0(7) . . . . ?
O5 C10 N1 C16 0.5(11) . . . . ?
O6 C2 C3 C5 175.4(4) . . . . ?
O6 C2 C3 C6 -5.3(5) . . . 2_666 ?
O7 C7 C11 C12 -4.8(6) . . . . ?
O7 C7 C11 C14 175.1(4) . . . . ?
O7 C7 O8 Tb1 5.0(4) . . . . ?
O8 C7 C11 C12 176.4(4) . . . . ?
O8 C7 C11 C14 -3.7(6) . . . . ?
O8 C7 O7 Tb1 -4.7(4) . . . . ?
O11A C13A N2 C17A -1.5(15) . . . . ?
O11A C13A N2 C18A -179.9(10) . . . . ?
O11B C13B N2 C17B -179.1(14) . . . . ?
O11B C13B N2 C18B -9(3) . . . . ?
O10 C1A N3 C2A 179.5(18) . . . . ?
O10 C1A N3 C3A -5(3) . . . . ?
O10 C1B N3 C2B -10(3) . . . . ?
O10 C1B N3 C3B 174.4(18) . . . . ?

_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 1.157
_oxdiff_exptl_absorpt_empirical_full_min 0.859

# start Validation Reply Form
_vrf_PLAT029_SION2_280K          
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.743 Why?  
RESPONSE: The data were collected upon the spindle rotation. Therefore, a 
		  limited portion of the reciprocal space could be probed.
;
# 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_SION2_260K
_database_code_depnum_ccdc_archive 'CCDC 1871309'
loop_
_audit_author_name
_audit_author_address
'Andrzej Gladysiak'
;Ecole polytechnique f?d?rale de Lausanne
Switzerland
;
_audit_update_record             
;
2018-10-03 deposited with the CCDC.	2019-08-12 downloaded from the CCDC.
;
_audit_creation_date             2018-07-09
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_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          ?
_chemical_oxdiff_formula         'C21 H27 N3 O12 Tb'
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                   10.5371(6)
_cell_length_b                   11.0161(5)
_cell_length_c                   12.7345(5)
_cell_angle_alpha                104.005(5)
_cell_angle_beta                 109.918(4)
_cell_angle_gamma                96.448(4)
_cell_volume                     1317.37(12)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5736
_cell_measurement_temperature    260.0
_cell_measurement_theta_max      31.8610
_cell_measurement_theta_min      1.9420
_shelx_estimated_absorpt_T_max   0.831
_shelx_estimated_absorpt_T_min   0.609
_exptl_absorpt_coefficient_mu    2.749
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78486
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.695
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             670
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0155
_diffrn_reflns_av_unetI/netI     0.0229
_diffrn_reflns_Laue_measured_fraction_full 0.743
_diffrn_reflns_Laue_measured_fraction_max 0.678
_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       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8661
_diffrn_reflns_point_group_measured_fraction_full 0.743
_diffrn_reflns_point_group_measured_fraction_max 0.678
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.433
_diffrn_reflns_theta_min         1.960
_diffrn_ambient_temperature      260.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            PILATUS2M
_diffrn_measured_fraction_theta_full 0.743
_diffrn_measured_fraction_theta_max 0.678
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      0.00 360.00   1.00    1.00    --    0.00   0.00   0.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  PILATUS@SNBL
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0606563000
_diffrn_orient_matrix_UB_12      -0.0143057000
_diffrn_orient_matrix_UB_13      0.0371829000
_diffrn_orient_matrix_UB_21      -0.0291809000
_diffrn_orient_matrix_UB_22      -0.0668817000
_diffrn_orient_matrix_UB_23      -0.0270006000
_diffrn_orient_matrix_UB_31      0.0302447000
_diffrn_orient_matrix_UB_32      -0.0002147000
_diffrn_orient_matrix_UB_33      -0.0424112000
_diffrn_radiation_monochromator  'Si (111)'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           ?
_diffrn_radiation_wavelength     0.7142
_diffrn_source                   
'European Synchrotron Radiation Facility, BM01 beamline'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4214
_reflns_number_total             4426
_reflns_odcompleteness_completeness 73.19
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.51
_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 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (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    'XT (Sheldrick, 2015)'
_refine_diff_density_max         1.019
_refine_diff_density_min         -1.137
_refine_diff_density_rms         0.084
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         4426
_refine_ls_number_restraints     115
_refine_ls_R_factor_all          0.0262
_refine_ls_R_factor_gt           0.0249
_refine_ls_restrained_S_all      1.089
_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)+(0.0536P)²+0.1424P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0700
_refine_ls_wR_factor_ref         0.0706
_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
 C18A-N2 \\sim N2-C18B
 with sigma of 0.01
 C17B-N2 \\sim N2-C17A
 with sigma of 0.01
 C13B-N2 \\sim N2-C13A
 with sigma of 0.01
 C13B-O11B \\sim O11A-C13A
 with sigma of 0.01
 C18B-C17B \\sim C17A-C18A
 with sigma of 0.01
3. Restrained planarity
 C13B, C17B, C18B, N2, O11B
 with sigma of 0.1
 C13A, C17A, C18A, N2, O11A
 with sigma of 0.1
4. Rigid bond restraints
 C2, O3
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.005
5. Uiso/Uaniso restraints and constraints
C2 \\sim O3: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.01
Uanis(O1B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C1A) = Uanis(C1B)
Uanis(C3A) = Uanis(C3B)
Uanis(C2A) = Uanis(C2B)
Uanis(O1A) = Uanis(O1B)
Uanis(O11B) = Uanis(O11A)
Uanis(C13A) = Uanis(C13B)
Uanis(C18B) = Uanis(C18A)
Uanis(C17B) = Uanis(C17A)
6. Rigid body (RIGU) restrains
 C1A, C2A, C3A, N3, O10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1B, C2B, C3B, N3, O10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C13A, C17A, C18A, N2, O11A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C13B, C17B, C18B, N2, O11B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. 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(H12)=Sof(O1B)=Sof(H1B)=1-FVAR(2)
 Sof(H14)=Sof(O1A)=Sof(H1A)=FVAR(2)
 Sof(C13B)=Sof(H13B)=Sof(C17B)=Sof(H17D)=Sof(H17E)=Sof(H17F)=Sof(C18B)=
 Sof(H18D)=Sof(H18E)=Sof(H18F)=Sof(O11B)=1-FVAR(3)
 Sof(C13A)=Sof(H13A)=Sof(C17A)=Sof(H17A)=Sof(H17B)=Sof(H17C)=Sof(C18A)=
 Sof(H18A)=Sof(H18B)=Sof(H18C)=Sof(O11A)=FVAR(3)
8.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C8(H8), C10(H10), C12(H12), C13A(H13A), C13B(H13B), C14(H14),
 C1A(H1AA), C1B(H1BA)
8.b Tetrahedral OH refined with riding coordinates:
 O1B(H1B)
8.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17A(H17A,H17B,H17C), C17B(H17D,
 H17E,H17F), C18A(H18A,H18B,H18C), C18B(H18D,H18E,H18F), C2A(H2AA,H2AB,H2AC),
 C2B(H2BA,H2BB,H2BC), C3A(H3AA,H3AB,H3AC), C3B(H3BA,H3BB,H3BC)
8.d Idealised tetrahedral OH refined as rotating group:
 O1A(H1A), O9(H9), O12(H12A)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
C1 C -0.0220(4) 0.1212(3) 0.4936(3) 0.0365(8) Uani 1 1 d . . . . .
C2 C 0.2062(3) 0.4683(3) 0.4415(3) 0.0372(5) Uani 1 1 d . U . . .
C3 C 0.3583(3) 0.4843(3) 0.4694(3) 0.0366(8) Uani 1 1 d . . . . .
C4 C -0.0397(3) 0.2541(3) 0.4921(3) 0.0346(7) Uani 1 1 d . . . . .
C5 C 0.4480(4) 0.5345(4) 0.5867(3) 0.0402(8) Uani 1 1 d . . . . .
H5 H 0.4126 0.5572 0.6447 0.048 Uiso 1 1 calc R . . . .
C6 C 0.5902(4) 0.5506(4) 0.6173(3) 0.0400(9) Uani 1 1 d . . . . .
C7 C 0.2939(3) 0.7715(3) 0.8473(3) 0.0374(8) Uani 1 1 d . . . . .
C8 C 0.0012(4) 0.0897(3) 0.5958(3) 0.0455(9) Uani 1 1 d . . . . .
H8 H 0.0024 0.1507 0.6611 0.055 Uiso 1 1 calc R . . . .
C9 C 0.0229(4) -0.0301(3) 0.6048(3) 0.0436(9) Uani 1 1 d . . . . .
C10 C -0.0206(5) 0.3875(4) 0.8251(4) 0.0559(11) Uani 1 1 d . . . . .
H10 H -0.1057 0.3699 0.7636 0.067 Uiso 1 1 calc R . . . .
C11 C 0.3994(3) 0.8909(3) 0.9269(3) 0.0373(8) Uani 1 1 d . . . . .
C12 C 0.3644(4) 0.9899(3) 0.9960(3) 0.0414(8) Uani 1 1 d . . . . .
H12 H 0.2745 0.9834 0.9932 0.050 Uiso 0.124(6) 1 calc R . P A 2
C13A C 0.3836(6) 0.4262(6) 0.7996(5) 0.0578(15) Uani 0.715(8) 1 d D U P B 1
H13A H 0.4444 0.5047 0.8238 0.069 Uiso 0.715(8) 1 calc R . P B 1
C13B C 0.3057(12) 0.3383(15) 0.7570(13) 0.0578(15) Uani 0.285(8) 1 d D U P B 2
H13B H 0.2456 0.2590 0.7168 0.069 Uiso 0.285(8) 1 calc R . P B 2
C14 C 0.5337(4) 0.9011(3) 0.9305(3) 0.0404(8) Uani 1 1 d . . . . .
H14 H 0.5558 0.8349 0.8836 0.049 Uiso 0.876(6) 1 calc R . P A 1
C15 C -0.1128(8) 0.2074(7) 0.8741(7) 0.108(2) Uani 1 1 d . . . . .
H15A H -0.1404 0.2241 0.9398 0.162 Uiso 1 1 calc GR . . . .
H15B H -0.0800 0.1292 0.8662 0.162 Uiso 1 1 calc GR . . . .
H15C H -0.1904 0.1998 0.8041 0.162 Uiso 1 1 calc GR . . . .
C16 C 0.1255(10) 0.3322(8) 0.9896(7) 0.135(4) Uani 1 1 d . . . . .
H16A H 0.1677 0.4218 1.0214 0.202 Uiso 1 1 calc GR . . . .
H16B H 0.1864 0.2859 0.9633 0.202 Uiso 1 1 calc GR . . . .
H16C H 0.1079 0.3017 1.0489 0.202 Uiso 1 1 calc GR . . . .
C17A C 0.3561(11) 0.2032(9) 0.8007(12) 0.121(4) Uani 0.715(8) 1 d D U P B 1
H17A H 0.3462 0.1894 0.8694 0.182 Uiso 0.715(8) 1 calc GR . P B 1
H17B H 0.4021 0.1411 0.7708 0.182 Uiso 0.715(8) 1 calc GR . P B 1
H17C H 0.2665 0.1943 0.7422 0.182 Uiso 0.715(8) 1 calc GR . P B 1
C17B C 0.415(3) 0.1909(12) 0.807(3) 0.121(4) Uani 0.285(8) 1 d D U P B 2
H17D H 0.3207 0.1557 0.7924 0.182 Uiso 0.285(8) 1 calc GR . P B 2
H17E H 0.4753 0.1719 0.8741 0.182 Uiso 0.285(8) 1 calc GR . P B 2
H17F H 0.4356 0.1539 0.7401 0.182 Uiso 0.285(8) 1 calc GR . P B 2
C18A C 0.5858(10) 0.3502(11) 0.9008(13) 0.125(4) Uani 0.715(8) 1 d D U P B 1
H18A H 0.6343 0.4203 0.8874 0.187 Uiso 0.715(8) 1 calc GR . P B 1
H18B H 0.6195 0.2746 0.8784 0.187 Uiso 0.715(8) 1 calc GR . P B 1
H18C H 0.6007 0.3705 0.9823 0.187 Uiso 0.715(8) 1 calc GR . P B 1
C18B C 0.5771(17) 0.401(2) 0.903(3) 0.125(4) Uani 0.285(8) 1 d D U P B 2
H18D H 0.6031 0.4615 0.8667 0.187 Uiso 0.285(8) 1 calc GR . P B 2
H18E H 0.6396 0.3442 0.9112 0.187 Uiso 0.285(8) 1 calc GR . P B 2
H18F H 0.5808 0.4469 0.9790 0.187 Uiso 0.285(8) 1 calc GR . P B 2
N1 N -0.0024(5) 0.3130(4) 0.8927(3) 0.0630(10) Uani 1 1 d . . . . .
N2 N 0.4345(5) 0.3270(5) 0.8295(4) 0.0785(13) Uani 1 1 d D U . . .
O1A O 0.2356(3) 0.9887(3) 0.9973(3) 0.0553(10) Uani 0.876(6) 1 d . . P A 1
H1A H 0.1817 0.9243 0.9476 0.083 Uiso 0.876(6) 1 calc GR . P A 1
O1B O 0.594(2) 0.808(2) 0.882(2) 0.0553(10) Uani 0.124(6) 1 d . U P A 2
H1B H 0.5345 0.7429 0.8404 0.083 Uiso 0.124(6) 1 calc R . P A 2
O2 O -0.0195(3) 0.33558(19) 0.5877(2) 0.0379(5) Uani 1 1 d . . . . .
O3 O 0.1611(2) 0.4930(2) 0.5213(2) 0.0391(5) Uani 1 1 d . U . . .
O4 O -0.0731(3) 0.2762(2) 0.3939(2) 0.0397(6) Uani 1 1 d . . . . .
O5 O 0.0685(3) 0.4806(3) 0.8376(2) 0.0490(7) Uani 1 1 d . . . . .
O6 O 0.1255(2) 0.4304(2) 0.3341(2) 0.0425(6) Uani 1 1 d . . . . .
O7 O 0.1733(3) 0.7559(2) 0.8488(2) 0.0418(6) Uani 1 1 d . . . . .
O8 O 0.3271(3) 0.6875(3) 0.7821(3) 0.0536(7) Uani 1 1 d . . . . .
O9 O 0.0457(5) -0.0511(3) 0.7100(3) 0.0718(11) Uani 1 1 d . . . . .
H9 H 0.0487 -0.1265 0.7037 0.108 Uiso 1 1 calc GR . . . .
O11A O 0.2715(19) 0.419(2) 0.7470(13) 0.0685(15) Uani 0.715(8) 1 d D U P B 1
O11B O 0.256(5) 0.419(5) 0.735(4) 0.0685(15) Uani 0.285(8) 1 d D U P B 2
O12 O 0.6718(3) 0.6003(4) 0.7337(2) 0.0635(9) Uani 1 1 d . . . . .
H12A H 0.7528 0.6004 0.7429 0.095 Uiso 1 1 calc GR . . . .
Tb1 Tb 0.10232(2) 0.54752(2) 0.68263(2) 0.02834(8) Uani 1 1 d . . . . .
C1A C 0.604(2) 0.1937(19) 0.5435(18) 0.125(4) Uani 0.512(8) 1 d . U P C 1
H1AA H 0.6835 0.1959 0.5268 0.150 Uiso 0.512(8) 1 calc R . P C 1
C1B C 0.504(2) 0.205(2) 0.5610(18) 0.125(4) Uani 0.488(8) 1 d . U P C 2
H1BA H 0.4308 0.2284 0.5796 0.150 Uiso 0.488(8) 1 calc R . P C 2
C2A C 0.455(3) 0.111(2) 0.3296(19) 0.140(4) Uani 0.512(8) 1 d . U P C 1
H2AA H 0.5408 0.1308 0.3195 0.209 Uiso 0.512(8) 1 calc GR . P C 1
H2AB H 0.3902 0.1544 0.2886 0.209 Uiso 0.512(8) 1 calc GR . P C 1
H2AC H 0.4191 0.0204 0.2989 0.209 Uiso 0.512(8) 1 calc GR . P C 1
C2B C 0.605(2) 0.144(2) 0.424(2) 0.140(4) Uani 0.488(8) 1 d . U P C 2
H2BA H 0.6599 0.2279 0.4451 0.209 Uiso 0.488(8) 1 calc GR . P C 2
H2BB H 0.5762 0.1040 0.3409 0.209 Uiso 0.488(8) 1 calc GR . P C 2
H2BC H 0.6579 0.0931 0.4655 0.209 Uiso 0.488(8) 1 calc GR . P C 2
C3A C 0.3516(19) 0.1438(19) 0.4788(18) 0.131(4) Uani 0.512(8) 1 d . U P C 1
H3AA H 0.3231 0.0584 0.4801 0.196 Uiso 0.512(8) 1 calc GR . P C 1
H3AB H 0.2796 0.1632 0.4191 0.196 Uiso 0.512(8) 1 calc GR . P C 1
H3AC H 0.3694 0.2035 0.5535 0.196 Uiso 0.512(8) 1 calc GR . P C 1
C3B C 0.344(2) 0.117(2) 0.3565(19) 0.131(4) Uani 0.488(8) 1 d . U P C 2
H3BA H 0.2794 0.1582 0.3822 0.196 Uiso 0.488(8) 1 calc GR . P C 2
H3BB H 0.3116 0.0259 0.3319 0.196 Uiso 0.488(8) 1 calc GR . P C 2
H3BC H 0.3516 0.1436 0.2921 0.196 Uiso 0.488(8) 1 calc GR . P C 2
N3 N 0.4798(7) 0.1533(6) 0.4534(6) 0.1017(17) Uani 1 1 d . U . . .
O10 O 0.6162(9) 0.2266(8) 0.6429(6) 0.157(3) Uani 1 1 d . U . . .


_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
C1 C4 1.500(4) . ?
C1 C8 1.377(5) . ?
C1 C9 1.399(5) 2_556 ?
C2 C3 1.498(5) . ?
C2 O3 1.248(5) . ?
C2 O6 1.273(4) . ?
C3 C5 1.397(5) . ?
C3 C6 1.382(6) 2_666 ?
C4 O2 1.258(4) . ?
C4 O4 1.270(4) . ?
C5 H5 0.9300 . ?
C5 C6 1.392(5) . ?
C6 C3 1.382(6) 2_666 ?
C6 O12 1.368(4) . ?
C7 C11 1.501(4) . ?
C7 O7 1.270(5) . ?
C7 O8 1.252(5) . ?
C8 H8 0.9300 . ?
C8 C9 1.389(4) . ?
C9 C1 1.399(5) 2_556 ?
C9 O9 1.361(5) . ?
C10 H10 0.9300 . ?
C10 N1 1.309(5) . ?
C10 O5 1.249(5) . ?
C11 C12 1.395(5) . ?
C11 C14 1.391(5) . ?
C12 H12 0.9300 . ?
C12 C14 1.397(4) 2_677 ?
C12 O1A 1.362(5) . ?
C13A H13A 0.9300 . ?
C13A N2 1.348(6) . ?
C13A O11A 1.124(17) . ?
C13B H13B 0.9300 . ?
C13B N2 1.396(9) . ?
C13B O11B 1.123(19) . ?
C14 C12 1.397(4) 2_677 ?
C14 H14 0.9300 . ?
C14 O1B 1.40(2) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C15 N1 1.462(8) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C16 N1 1.435(8) . ?
C17A H17A 0.9600 . ?
C17A H17B 0.9600 . ?
C17A H17C 0.9600 . ?
C17A N2 1.406(10) . ?
C17B H17D 0.9600 . ?
C17B H17E 0.9600 . ?
C17B H17F 0.9600 . ?
C17B N2 1.435(12) . ?
C18A H18A 0.9600 . ?
C18A H18B 0.9600 . ?
C18A H18C 0.9600 . ?
C18A N2 1.497(9) . ?
C18B H18D 0.9600 . ?
C18B H18E 0.9600 . ?
C18B H18F 0.9600 . ?
C18B N2 1.483(12) . ?
O1A H1A 0.8200 . ?
O1B H1B 0.8200 . ?
O2 Tb1 2.337(2) . ?
O3 Tb1 2.306(3) . ?
O4 Tb1 2.380(2) 2_566 ?
O5 Tb1 2.385(3) . ?
O6 Tb1 2.383(2) 2_566 ?
O7 Tb1 2.548(2) . ?
O8 Tb1 2.404(3) . ?
O9 H9 0.8200 . ?
O11A Tb1 2.449(6) . ?
O11B Tb1 2.306(14) . ?
O12 H12A 0.8200 . ?
Tb1 O4 2.380(2) 2_566 ?
Tb1 O6 2.383(2) 2_566 ?
C1A H1AA 0.9300 . ?
C1A N3 1.35(2) . ?
C1A O10 1.19(2) . ?
C1B H1BA 0.9300 . ?
C1B N3 1.27(2) . ?
C1B O10 1.23(2) . ?
C2A H2AA 0.9600 . ?
C2A H2AB 0.9600 . ?
C2A H2AC 0.9600 . ?
C2A N3 1.45(2) . ?
C2B H2BA 0.9600 . ?
C2B H2BB 0.9600 . ?
C2B H2BC 0.9600 . ?
C2B N3 1.50(2) . ?
C3A H3AA 0.9600 . ?
C3A H3AB 0.9600 . ?
C3A H3AC 0.9600 . ?
C3A N3 1.49(2) . ?
C3B H3BA 0.9600 . ?
C3B H3BB 0.9600 . ?
C3B H3BC 0.9600 . ?
C3B N3 1.47(2) . ?

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
C8 C1 C4 119.1(3) . . ?
C8 C1 C9 119.1(3) . 2_556 ?
C9 C1 C4 121.8(3) 2_556 . ?
O3 C2 C3 120.8(3) . . ?
O3 C2 O6 121.5(3) . . ?
O6 C2 C3 117.7(4) . . ?
C5 C3 C2 118.0(4) . . ?
C6 C3 C2 121.6(3) 2_666 . ?
C6 C3 C5 120.4(3) 2_666 . ?
O2 C4 C1 118.0(3) . . ?
O2 C4 O4 124.8(3) . . ?
O4 C4 C1 117.2(3) . . ?
C3 C5 H5 119.9 . . ?
C6 C5 C3 120.2(4) . . ?
C6 C5 H5 119.9 . . ?
C3 C6 C5 119.4(3) 2_666 . ?
O12 C6 C3 123.5(3) . 2_666 ?
O12 C6 C5 117.1(4) . . ?
O7 C7 C11 119.6(3) . . ?
O8 C7 C11 119.4(3) . . ?
O8 C7 O7 121.0(3) . . ?
C1 C8 H8 118.8 . . ?
C1 C8 C9 122.3(3) . . ?
C9 C8 H8 118.8 . . ?
C8 C9 C1 118.6(3) . 2_556 ?
O9 C9 C1 123.8(3) . 2_556 ?
O9 C9 C8 117.6(3) . . ?
N1 C10 H10 117.7 . . ?
O5 C10 H10 117.7 . . ?
O5 C10 N1 124.6(4) . . ?
C12 C11 C7 121.1(3) . . ?
C14 C11 C7 118.5(3) . . ?
C14 C11 C12 120.4(3) . . ?
C11 C12 H12 120.5 . . ?
C11 C12 C14 119.1(3) . 2_677 ?
C14 C12 H12 120.5 2_677 . ?
O1A C12 C11 124.4(3) . . ?
O1A C12 C14 116.5(3) . 2_677 ?
N2 C13A H13A 118.3 . . ?
O11A C13A H13A 118.3 . . ?
O11A C13A N2 123.3(13) . . ?
N2 C13B H13B 111.8 . . ?
O11B C13B H13B 111.8 . . ?
O11B C13B N2 136(4) . . ?
C11 C14 C12 120.5(3) . 2_677 ?
C11 C14 H14 119.7 . . ?
C11 C14 O1B 129.2(9) . . ?
C12 C14 H14 119.7 2_677 . ?
C12 C14 O1B 109.7(9) 2_677 . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N1 C15 H15A 109.5 . . ?
N1 C15 H15B 109.5 . . ?
N1 C15 H15C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N1 C16 H16A 109.5 . . ?
N1 C16 H16B 109.5 . . ?
N1 C16 H16C 109.5 . . ?
H17A C17A H17B 109.5 . . ?
H17A C17A H17C 109.5 . . ?
H17B C17A H17C 109.5 . . ?
N2 C17A H17A 109.5 . . ?
N2 C17A H17B 109.5 . . ?
N2 C17A H17C 109.5 . . ?
H17D C17B H17E 109.5 . . ?
H17D C17B H17F 109.5 . . ?
H17E C17B H17F 109.5 . . ?
N2 C17B H17D 109.5 . . ?
N2 C17B H17E 109.5 . . ?
N2 C17B H17F 109.5 . . ?
H18A C18A H18B 109.5 . . ?
H18A C18A H18C 109.5 . . ?
H18B C18A H18C 109.5 . . ?
N2 C18A H18A 109.5 . . ?
N2 C18A H18B 109.5 . . ?
N2 C18A H18C 109.5 . . ?
H18D C18B H18E 109.5 . . ?
H18D C18B H18F 109.5 . . ?
H18E C18B H18F 109.5 . . ?
N2 C18B H18D 109.5 . . ?
N2 C18B H18E 109.5 . . ?
N2 C18B H18F 109.5 . . ?
C10 N1 C15 121.4(5) . . ?
C10 N1 C16 121.9(5) . . ?
C16 N1 C15 116.7(5) . . ?
C13A N2 C17A 125.2(6) . . ?
C13A N2 C18A 117.9(7) . . ?
C13B N2 C17B 101.3(12) . . ?
C13B N2 C18B 142.2(12) . . ?
C17A N2 C18A 116.9(6) . . ?
C17B N2 C18B 115.8(11) . . ?
C12 O1A H1A 109.5 . . ?
C14 O1B H1B 109.5 . . ?
C4 O2 Tb1 135.1(2) . . ?
C2 O3 Tb1 173.8(2) . . ?
C4 O4 Tb1 139.0(2) . 2_566 ?
C10 O5 Tb1 125.6(3) . . ?
C2 O6 Tb1 109.6(2) . 2_566 ?
C7 O7 Tb1 89.5(2) . . ?
C7 O8 Tb1 96.7(2) . . ?
C9 O9 H9 109.5 . . ?
C13A O11A Tb1 142.6(17) . . ?
C13B O11B Tb1 165(5) . . ?
C6 O12 H12A 109.5 . . ?
O2 Tb1 O4 126.34(8) . 2_566 ?
O2 Tb1 O5 77.48(9) . . ?
O2 Tb1 O6 79.17(9) . 2_566 ?
O2 Tb1 O7 151.85(9) . . ?
O2 Tb1 O8 145.51(9) . . ?
O2 Tb1 O11A 75.5(6) . . ?
O3 Tb1 O2 77.27(9) . . ?
O3 Tb1 O4 76.25(9) . 2_566 ?
O3 Tb1 O5 145.82(9) . . ?
O3 Tb1 O6 122.09(9) . 2_566 ?
O3 Tb1 O7 130.88(8) . . ?
O3 Tb1 O8 86.57(10) . . ?
O3 Tb1 O11A 80.0(3) . . ?
O3 Tb1 O11B 78.2(8) . . ?
O4 Tb1 O5 137.82(10) 2_566 . ?
O4 Tb1 O6 76.86(9) 2_566 2_566 ?
O4 Tb1 O7 69.75(8) 2_566 . ?
O4 Tb1 O8 77.33(9) 2_566 . ?
O4 Tb1 O11A 141.8(5) 2_566 . ?
O5 Tb1 O7 76.64(9) . . ?
O5 Tb1 O8 101.81(10) . . ?
O5 Tb1 O11A 71.6(4) . . ?
O6 Tb1 O5 74.67(10) 2_566 . ?
O6 Tb1 O7 83.49(9) 2_566 . ?
O6 Tb1 O8 134.53(9) 2_566 . ?
O6 Tb1 O11A 141.3(5) 2_566 . ?
O8 Tb1 O7 52.52(9) . . ?
O8 Tb1 O11A 71.8(6) . . ?
O11A Tb1 O7 106.3(5) . . ?
O11B Tb1 O2 73.1(17) . . ?
O11B Tb1 O4 142.3(14) . 2_566 ?
O11B Tb1 O5 72.6(9) . . ?
O11B Tb1 O6 140.8(14) . 2_566 ?
O11B Tb1 O7 109.1(14) . . ?
O11B Tb1 O8 73.9(17) . . ?
N3 C1A H1AA 118.6 . . ?
O10 C1A H1AA 118.6 . . ?
O10 C1A N3 123(2) . . ?
N3 C1B H1BA 116.9 . . ?
O10 C1B H1BA 116.9 . . ?
O10 C1B N3 126(2) . . ?
H2AA C2A H2AB 109.5 . . ?
H2AA C2A H2AC 109.5 . . ?
H2AB C2A H2AC 109.5 . . ?
N3 C2A H2AA 109.5 . . ?
N3 C2A H2AB 109.5 . . ?
N3 C2A H2AC 109.5 . . ?
H2BA C2B H2BB 109.5 . . ?
H2BA C2B H2BC 109.5 . . ?
H2BB C2B H2BC 109.5 . . ?
N3 C2B H2BA 109.5 . . ?
N3 C2B H2BB 109.5 . . ?
N3 C2B H2BC 109.5 . . ?
H3AA C3A H3AB 109.5 . . ?
H3AA C3A H3AC 109.5 . . ?
H3AB C3A H3AC 109.5 . . ?
N3 C3A H3AA 109.5 . . ?
N3 C3A H3AB 109.5 . . ?
N3 C3A H3AC 109.5 . . ?
H3BA C3B H3BB 109.5 . . ?
H3BA C3B H3BC 109.5 . . ?
H3BB C3B H3BC 109.5 . . ?
N3 C3B H3BA 109.5 . . ?
N3 C3B H3BB 109.5 . . ?
N3 C3B H3BC 109.5 . . ?
C1A N3 C2A 126.5(15) . . ?
C1A N3 C3A 119.2(13) . . ?
C1B N3 C2B 115.3(15) . . ?
C1B N3 C3B 126.3(16) . . ?
C2A N3 C3A 114.2(13) . . ?
C3B N3 C2B 118.0(14) . . ?

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
C1 C4 O2 Tb1 133.1(3) . . . . ?
C1 C4 O4 Tb1 -173.5(2) . . . 2_566 ?
C1 C8 C9 C1 0.4(7) . . . 2_556 ?
C1 C8 C9 O9 179.6(4) . . . . ?
C2 C3 C5 C6 179.7(3) . . . . ?
C3 C2 O6 Tb1 -169.3(2) . . . 2_566 ?
C3 C5 C6 C3 -0.5(6) . . . 2_666 ?
C3 C5 C6 O12 180.0(4) . . . . ?
C4 C1 C8 C9 -177.9(4) . . . . ?
C6 C3 C5 C6 0.5(6) 2_666 . . . ?
C7 C11 C12 C14 179.6(3) . . . 2_677 ?
C7 C11 C12 O1A -0.6(6) . . . . ?
C7 C11 C14 C12 -179.5(3) . . . 2_677 ?
C7 C11 C14 O1B -9.9(16) . . . . ?
C8 C1 C4 O2 6.7(5) . . . . ?
C8 C1 C4 O4 -173.9(4) . . . . ?
C9 C1 C4 O2 -170.7(4) 2_556 . . . ?
C9 C1 C4 O4 8.7(5) 2_556 . . . ?
C9 C1 C8 C9 -0.4(7) 2_556 . . . ?
C11 C7 O7 Tb1 176.7(3) . . . . ?
C11 C7 O8 Tb1 -176.4(3) . . . . ?
C12 C11 C14 C12 0.5(6) . . . 2_677 ?
C12 C11 C14 O1B 170.2(15) . . . . ?
C14 C11 C12 C14 -0.5(6) . . . 2_677 ?
C14 C11 C12 O1A 179.3(4) . . . . ?
N1 C10 O5 Tb1 144.7(4) . . . . ?
N2 C13A O11A Tb1 169.2(10) . . . . ?
N2 C13B O11B Tb1 -149(10) . . . . ?
O2 C4 O4 Tb1 5.9(6) . . . 2_566 ?
O3 C2 C3 C5 -3.6(5) . . . . ?
O3 C2 C3 C6 175.6(3) . . . 2_666 ?
O3 C2 O6 Tb1 9.9(4) . . . 2_566 ?
O4 C4 O2 Tb1 -46.2(5) . . . . ?
O5 C10 N1 C15 178.6(6) . . . . ?
O5 C10 N1 C16 -0.2(10) . . . . ?
O6 C2 C3 C5 175.5(3) . . . . ?
O6 C2 C3 C6 -5.3(5) . . . 2_666 ?
O7 C7 C11 C12 -5.2(5) . . . . ?
O7 C7 C11 C14 174.9(3) . . . . ?
O7 C7 O8 Tb1 5.2(4) . . . . ?
O8 C7 C11 C12 176.4(4) . . . . ?
O8 C7 C11 C14 -3.6(5) . . . . ?
O8 C7 O7 Tb1 -4.8(4) . . . . ?
O11A C13A N2 C17A -0.6(13) . . . . ?
O11A C13A N2 C18A -179.5(10) . . . . ?
O11B C13B N2 C17B -179.5(15) . . . . ?
O11B C13B N2 C18B -10(3) . . . . ?
O10 C1A N3 C2A -179.8(17) . . . . ?
O10 C1A N3 C3A -3(2) . . . . ?
O10 C1B N3 C2B -13(3) . . . . ?
O10 C1B N3 C3B 174.4(16) . . . . ?

_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 1.161
_oxdiff_exptl_absorpt_empirical_full_min 0.839

# start Validation Reply Form
_vrf_PLAT029_SION2_260K          
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.743 Why?  
RESPONSE: The data were collected upon the spindle rotation. Therefore, a 
		  limited portion of the reciprocal space could be probed.
;
# 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_SION2_220K
_database_code_depnum_ccdc_archive 'CCDC 1871311'
loop_
_audit_author_name
_audit_author_address
'Andrzej Gladysiak'
;Ecole polytechnique f?d?rale de Lausanne
Switzerland
;
_audit_update_record             
;
2018-10-03 deposited with the CCDC.	2019-08-12 downloaded from the CCDC.
;
_audit_creation_date             2018-07-09
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_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          ?
_chemical_oxdiff_formula         'C21 H27 N3 O12 Tb'
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                   10.5190(6)
_cell_length_b                   10.9933(5)
_cell_length_c                   12.6565(5)
_cell_angle_alpha                104.317(4)
_cell_angle_beta                 109.262(4)
_cell_angle_gamma                96.536(4)
_cell_volume                     1307.83(12)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5759
_cell_measurement_temperature    220.0
_cell_measurement_theta_max      31.9260
_cell_measurement_theta_min      2.0920
_shelx_estimated_absorpt_T_max   0.830
_shelx_estimated_absorpt_T_min   0.607
_exptl_absorpt_coefficient_mu    2.769
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77258
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.707
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             670
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0176
_diffrn_reflns_av_unetI/netI     0.0259
_diffrn_reflns_Laue_measured_fraction_full 0.747
_diffrn_reflns_Laue_measured_fraction_max 0.684
_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       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8658
_diffrn_reflns_point_group_measured_fraction_full 0.747
_diffrn_reflns_point_group_measured_fraction_max 0.684
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.431
_diffrn_reflns_theta_min         1.967
_diffrn_ambient_temperature      220.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            PILATUS2M
_diffrn_measured_fraction_theta_full 0.747
_diffrn_measured_fraction_theta_max 0.684
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      0.00 360.00   1.00    1.00    --    0.00   0.00   0.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  PILATUS@SNBL
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0605786000
_diffrn_orient_matrix_UB_12      -0.0139922000
_diffrn_orient_matrix_UB_13      0.0370018000
_diffrn_orient_matrix_UB_21      -0.0287806000
_diffrn_orient_matrix_UB_22      -0.0671920000
_diffrn_orient_matrix_UB_23      -0.0270263000
_diffrn_orient_matrix_UB_31      0.0303666000
_diffrn_orient_matrix_UB_32      -0.0002225000
_diffrn_orient_matrix_UB_33      -0.0428559000
_diffrn_radiation_monochromator  'Si (111)'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           ?
_diffrn_radiation_wavelength     0.7142
_diffrn_source                   
'European Synchrotron Radiation Facility, BM01 beamline'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4230
_reflns_number_total             4433
_reflns_odcompleteness_completeness 73.65
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.51
_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 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (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    'XT (Sheldrick, 2015)'
_refine_diff_density_max         1.689
_refine_diff_density_min         -1.426
_refine_diff_density_rms         0.107
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         4433
_refine_ls_number_restraints     58
_refine_ls_R_factor_all          0.0325
_refine_ls_R_factor_gt           0.0313
_refine_ls_restrained_S_all      1.047
_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)+(0.0664P)²+0.6025P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0836
_refine_ls_wR_factor_ref         0.0846
_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. Rigid bond restraints
 O3, C2
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.005
3. Uiso/Uaniso restraints and constraints
O3 \\sim C2: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.01
Uanis(O1B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C1A, N3, C2A, C3A, O10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O10, C1B, N3, C3B, C2B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. 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)
6.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C8(H8), C10(H10), C12(H12A), C13(H13), C14(H14), C1A(H1AA), C1B(H1BA)
6.b Tetrahedral OH refined with riding coordinates:
 O1B(H1B)
6.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)
6.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 0.10010(2) 0.54749(2) 0.68289(2) 0.02727(9) Uani 1 1 d . . . . .
O2 O -0.0238(3) 0.3356(2) 0.5875(2) 0.0358(6) Uani 1 1 d . . . . .
O3 O 0.1592(3) 0.4908(3) 0.5202(3) 0.0369(5) Uani 1 1 d . U . . .
O4 O -0.0752(3) 0.2753(2) 0.3934(2) 0.0365(6) Uani 1 1 d . . . . .
O5 O 0.0650(3) 0.4825(3) 0.8393(3) 0.0445(7) Uani 1 1 d . . . . .
O6 O 0.1272(3) 0.4279(3) 0.3323(3) 0.0395(7) Uani 1 1 d . . . . .
O7 O 0.1710(3) 0.7584(3) 0.8498(3) 0.0386(7) Uani 1 1 d . . . . .
O8 O 0.3249(3) 0.6852(3) 0.7837(3) 0.0480(8) Uani 1 1 d . . . . .
O9 O 0.0454(5) -0.0500(3) 0.7111(3) 0.0653(12) Uani 1 1 d . . . . .
H9 H 0.0472 -0.1268 0.7042 0.098 Uiso 1 1 calc GR . . . .
O11 O 0.2619(4) 0.4143(4) 0.7410(4) 0.0632(10) Uani 1 1 d . . . . .
O12 O 0.6682(3) 0.6023(4) 0.7349(3) 0.0591(10) Uani 1 1 d . . . . .
H12 H 0.7504 0.6044 0.7442 0.089 Uiso 1 1 calc GR . . . .
N1 N -0.0054(5) 0.3121(4) 0.8923(4) 0.0565(11) Uani 1 1 d . . . . .
O1A O 0.2350(4) 0.9942(4) 0.9971(4) 0.0500(13) Uani 0.881(11) 1 d . . P A 1
H1A H 0.1827 0.9239 0.9552 0.075 Uiso 0.881(11) 1 calc GR . P A 1
O1B O 0.591(3) 0.806(3) 0.884(3) 0.065(11) Uani 0.119(11) 1 d . U P A 2
H1B H 0.5307 0.7408 0.8425 0.098 Uiso 0.119(11) 1 calc R . P A 2
N2 N 0.4332(5) 0.3300(5) 0.8314(5) 0.0700(14) Uani 1 1 d . . . . .
C1 C -0.0232(4) 0.1209(3) 0.4932(3) 0.0340(9) Uani 1 1 d . . . . .
C2 C 0.2062(4) 0.4665(4) 0.4403(4) 0.0355(6) Uani 1 1 d . U . . .
C3 C 0.3579(4) 0.4834(4) 0.4684(4) 0.0356(10) Uani 1 1 d . . . . .
C4 C -0.0418(4) 0.2538(3) 0.4914(3) 0.0329(9) Uani 1 1 d . . . . .
C5 C 0.4458(4) 0.5351(4) 0.5870(4) 0.0380(9) Uani 1 1 d . . . . .
H5 H 0.4087 0.5589 0.6453 0.046 Uiso 1 1 calc R . . . .
C6 C 0.5883(4) 0.5512(4) 0.6181(4) 0.0375(10) Uani 1 1 d . . . . .
C7 C 0.2919(4) 0.7719(3) 0.8485(3) 0.0355(9) Uani 1 1 d . . . . .
C8 C -0.0002(5) 0.0907(4) 0.5966(4) 0.0419(10) Uani 1 1 d . . . . .
H8 H 0.0000 0.1530 0.6627 0.050 Uiso 1 1 calc R . . . .
C9 C 0.0229(5) -0.0294(4) 0.6061(4) 0.0404(10) Uani 1 1 d . . . . .
C10 C -0.0239(5) 0.3886(5) 0.8264(4) 0.0491(11) Uani 1 1 d . . . . .
H10 H -0.1100 0.3717 0.7651 0.059 Uiso 1 1 calc R . . . .
N3 N 0.4784(7) 0.1537(6) 0.4537(6) 0.0877(17) Uani 1 1 d . U . . .
C11 C 0.3986(4) 0.8911(3) 0.9271(3) 0.0354(9) Uani 1 1 d . . . . .
C12 C 0.3643(4) 0.9924(4) 0.9962(4) 0.0374(9) Uani 1 1 d . . . . .
H12A H 0.2734 0.9875 0.9936 0.045 Uiso 0.119(11) 1 calc R . P A 2
C13 C 0.3789(6) 0.4243(6) 0.7987(5) 0.0662(16) Uani 1 1 d . . . . .
H13 H 0.4380 0.5052 0.8234 0.079 Uiso 1 1 calc R . . . .
C14 C 0.5329(4) 0.8990(4) 0.9309(4) 0.0381(9) Uani 1 1 d . . . . .
H14 H 0.5547 0.8304 0.8839 0.046 Uiso 0.881(11) 1 calc R . P A 1
C15 C -0.1147(9) 0.2061(7) 0.8741(7) 0.088(2) Uani 1 1 d . . . . .
H15A H -0.1311 0.2144 0.9464 0.132 Uiso 1 1 calc GR . . . .
H15B H -0.0874 0.1253 0.8511 0.132 Uiso 1 1 calc GR . . . .
H15C H -0.1985 0.2078 0.8126 0.132 Uiso 1 1 calc GR . . . .
O10 O 0.6117(9) 0.2268(8) 0.6444(6) 0.133(3) Uani 1 1 d . U . . .
C16 C 0.1199(10) 0.3319(8) 0.9910(7) 0.105(3) Uani 1 1 d . . . . .
H16A H 0.1564 0.4233 1.0294 0.158 Uiso 1 1 calc GR . . . .
H16B H 0.1868 0.2936 0.9643 0.158 Uiso 1 1 calc GR . . . .
H16C H 0.1012 0.2920 1.0462 0.158 Uiso 1 1 calc GR . . . .
C17 C 0.3653(11) 0.2004(9) 0.8013(9) 0.129(4) Uani 1 1 d . . . . .
H17A H 0.3625 0.1814 0.8715 0.194 Uiso 1 1 calc GR . . . .
H17B H 0.4149 0.1441 0.7663 0.194 Uiso 1 1 calc GR . . . .
H17C H 0.2720 0.1868 0.7456 0.194 Uiso 1 1 calc GR . . . .
C18 C 0.5796(10) 0.3614(11) 0.9032(10) 0.126(4) Uani 1 1 d . . . . .
H18A H 0.6282 0.3135 0.8601 0.190 Uiso 1 1 calc GR . . . .
H18B H 0.5929 0.3388 0.9750 0.190 Uiso 1 1 calc GR . . . .
H18C H 0.6151 0.4527 0.9226 0.190 Uiso 1 1 calc GR . . . .
C1A C 0.601(2) 0.1942(16) 0.5403(16) 0.099(4) Uani 0.539(12) 1 d . U P B 1
H1AA H 0.6806 0.1983 0.5225 0.118 Uiso 0.539(12) 1 calc R . P B 1
C2A C 0.451(3) 0.113(2) 0.3300(18) 0.131(7) Uani 0.539(12) 1 d . U P B 1
H2AA H 0.5254 0.1572 0.3150 0.197 Uiso 0.539(12) 1 calc GR . P B 1
H2AB H 0.3650 0.1337 0.2880 0.197 Uiso 0.539(12) 1 calc GR . P B 1
H2AC H 0.4441 0.0211 0.3034 0.197 Uiso 0.539(12) 1 calc GR . P B 1
C3A C 0.348(2) 0.1438(18) 0.4800(19) 0.114(5) Uani 0.539(12) 1 d . U P B 1
H3AA H 0.3275 0.0621 0.4937 0.171 Uiso 0.539(12) 1 calc GR . P B 1
H3AB H 0.2722 0.1497 0.4137 0.171 Uiso 0.539(12) 1 calc GR . P B 1
H3AC H 0.3609 0.2134 0.5494 0.171 Uiso 0.539(12) 1 calc GR . P B 1
C1B C 0.502(3) 0.205(2) 0.5627(19) 0.110(6) Uani 0.461(12) 1 d . U P B 2
H1BA H 0.4270 0.2273 0.5817 0.132 Uiso 0.461(12) 1 calc R . P B 2
C2B C 0.602(2) 0.143(2) 0.424(2) 0.113(6) Uani 0.461(12) 1 d . U P B 2
H2BA H 0.6605 0.2273 0.4500 0.170 Uiso 0.461(12) 1 calc GR . P B 2
H2BB H 0.5740 0.1061 0.3402 0.170 Uiso 0.461(12) 1 calc GR . P B 2
H2BC H 0.6515 0.0876 0.4639 0.170 Uiso 0.461(12) 1 calc GR . P B 2
C3B C 0.345(2) 0.118(2) 0.360(2) 0.113(7) Uani 0.461(12) 1 d . U P B 2
H3BA H 0.2784 0.1514 0.3903 0.170 Uiso 0.461(12) 1 calc GR . P B 2
H3BB H 0.3177 0.0252 0.3290 0.170 Uiso 0.461(12) 1 calc GR . P B 2
H3BC H 0.3500 0.1538 0.2984 0.170 Uiso 0.461(12) 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 2.337(2) . ?
Tb1 O3 2.305(3) . ?
Tb1 O4 2.383(2) 2_566 ?
Tb1 O5 2.385(3) . ?
Tb1 O6 2.387(3) 2_566 ?
Tb1 O7 2.557(3) . ?
Tb1 O8 2.398(3) . ?
Tb1 O11 2.420(3) . ?
O2 C4 1.262(5) . ?
O3 C2 1.250(6) . ?
O4 Tb1 2.383(2) 2_566 ?
O4 C4 1.262(5) . ?
O5 C10 1.250(6) . ?
O6 Tb1 2.387(3) 2_566 ?
O6 C2 1.274(5) . ?
O7 C7 1.269(5) . ?
O8 C7 1.255(5) . ?
O9 H9 0.8300 . ?
O9 C9 1.352(6) . ?
O11 C13 1.182(6) . ?
O12 H12 0.8300 . ?
O12 C6 1.367(5) . ?
N1 C10 1.311(6) . ?
N1 C15 1.456(8) . ?
N1 C16 1.435(8) . ?
O1A H1A 0.8300 . ?
O1A C12 1.366(6) . ?
O1B H1B 0.8300 . ?
O1B C14 1.36(3) . ?
N2 C13 1.327(6) . ?
N2 C17 1.417(10) . ?
N2 C18 1.455(10) . ?
C1 C4 1.501(5) . ?
C1 C8 1.379(6) . ?
C1 C9 1.403(6) 2_556 ?
C2 C3 1.495(5) . ?
C3 C5 1.405(5) . ?
C3 C6 1.383(7) 2_666 ?
C5 H5 0.9400 . ?
C5 C6 1.395(6) . ?
C6 C3 1.383(7) 2_666 ?
C7 C11 1.500(5) . ?
C8 H8 0.9400 . ?
C8 C9 1.397(5) . ?
C9 C1 1.403(6) 2_556 ?
C10 H10 0.9400 . ?
N3 C1A 1.323(18) . ?
N3 C2A 1.44(2) . ?
N3 C3A 1.51(2) . ?
N3 C1B 1.28(2) . ?
N3 C2B 1.47(2) . ?
N3 C3B 1.44(2) . ?
C11 C12 1.397(6) . ?
C11 C14 1.389(6) . ?
C12 H12A 0.9400 . ?
C12 C14 1.397(5) 2_677 ?
C13 H13 0.9400 . ?
C14 C12 1.396(5) 2_677 ?
C14 H14 0.9400 . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C15 H15C 0.9700 . ?
O10 C1A 1.24(2) . ?
O10 C1B 1.22(2) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C16 H16C 0.9700 . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C17 H17C 0.9700 . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C18 H18C 0.9700 . ?
C1A H1AA 0.9400 . ?
C2A H2AA 0.9700 . ?
C2A H2AB 0.9700 . ?
C2A H2AC 0.9700 . ?
C3A H3AA 0.9700 . ?
C3A H3AB 0.9700 . ?
C3A H3AC 0.9700 . ?
C1B H1BA 0.9400 . ?
C2B H2BA 0.9700 . ?
C2B H2BB 0.9700 . ?
C2B H2BC 0.9700 . ?
C3B H3BA 0.9700 . ?
C3B H3BB 0.9700 . ?
C3B H3BC 0.9700 . ?

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 126.42(9) . 2_566 ?
O2 Tb1 O5 77.73(10) . . ?
O2 Tb1 O6 79.05(10) . 2_566 ?
O2 Tb1 O7 151.79(11) . . ?
O2 Tb1 O8 145.53(10) . . ?
O2 Tb1 O11 74.41(12) . . ?
O3 Tb1 O2 77.26(10) . . ?
O3 Tb1 O4 76.12(10) . 2_566 ?
O3 Tb1 O5 145.88(10) . . ?
O3 Tb1 O6 122.13(10) . 2_566 ?
O3 Tb1 O7 130.93(10) . . ?
O3 Tb1 O8 87.17(11) . . ?
O3 Tb1 O11 79.11(13) . . ?
O4 Tb1 O5 137.93(11) 2_566 . ?
O4 Tb1 O6 77.23(10) 2_566 2_566 ?
O4 Tb1 O7 69.42(9) 2_566 . ?
O4 Tb1 O8 77.57(11) 2_566 . ?
O4 Tb1 O11 141.77(13) 2_566 . ?
O5 Tb1 O6 74.76(11) . 2_566 ?
O5 Tb1 O7 76.58(10) . . ?
O5 Tb1 O8 100.86(12) . . ?
O5 Tb1 O11 72.06(13) . . ?
O6 Tb1 O7 83.15(10) 2_566 . ?
O6 Tb1 O8 134.42(10) 2_566 . ?
O6 Tb1 O11 141.00(13) 2_566 . ?
O8 Tb1 O7 52.49(10) . . ?
O8 Tb1 O11 72.53(12) . . ?
O11 Tb1 O7 108.07(12) . . ?
C4 O2 Tb1 134.2(3) . . ?
C2 O3 Tb1 173.0(3) . . ?
C4 O4 Tb1 139.0(2) . 2_566 ?
C10 O5 Tb1 124.9(3) . . ?
C2 O6 Tb1 108.9(3) . 2_566 ?
C7 O7 Tb1 89.3(2) . . ?
C7 O8 Tb1 97.1(2) . . ?
C9 O9 H9 109.5 . . ?
C13 O11 Tb1 140.0(4) . . ?
C6 O12 H12 109.5 . . ?
C10 N1 C15 121.7(5) . . ?
C10 N1 C16 122.4(5) . . ?
C16 N1 C15 115.7(5) . . ?
C12 O1A H1A 109.5 . . ?
C14 O1B H1B 109.5 . . ?
C13 N2 C17 127.2(6) . . ?
C13 N2 C18 116.9(7) . . ?
C17 N2 C18 115.9(7) . . ?
C8 C1 C4 118.8(4) . . ?
C8 C1 C9 119.8(3) . 2_556 ?
C9 C1 C4 121.3(4) 2_556 . ?
O3 C2 O6 121.6(4) . . ?
O3 C2 C3 121.0(4) . . ?
O6 C2 C3 117.4(4) . . ?
C5 C3 C2 117.6(4) . . ?
C6 C3 C2 122.0(4) 2_666 . ?
C6 C3 C5 120.4(4) 2_666 . ?
O2 C4 C1 117.8(3) . . ?
O4 C4 O2 124.8(3) . . ?
O4 C4 C1 117.4(3) . . ?
C3 C5 H5 120.0 . . ?
C6 C5 C3 119.9(4) . . ?
C6 C5 H5 120.0 . . ?
O12 C6 C3 123.2(4) . 2_666 ?
O12 C6 C5 117.1(4) . . ?
C3 C6 C5 119.7(4) 2_666 . ?
O7 C7 C11 120.0(4) . . ?
O8 C7 O7 120.9(3) . . ?
O8 C7 C11 119.1(4) . . ?
C1 C8 H8 119.0 . . ?
C1 C8 C9 122.1(4) . . ?
C9 C8 H8 119.0 . . ?
O9 C9 C1 123.9(3) . 2_556 ?
O9 C9 C8 117.9(4) . . ?
C8 C9 C1 118.2(4) . 2_556 ?
O5 C10 N1 124.6(5) . . ?
O5 C10 H10 117.7 . . ?
N1 C10 H10 117.7 . . ?
C1A N3 C2A 127.0(17) . . ?
C1A N3 C3A 120.4(13) . . ?
C2A N3 C3A 112.6(15) . . ?
C1B N3 C2B 115.2(17) . . ?
C1B N3 C3B 125.4(19) . . ?
C3B N3 C2B 119.1(16) . . ?
C12 C11 C7 120.8(4) . . ?
C14 C11 C7 118.9(4) . . ?
C14 C11 C12 120.3(3) . . ?
O1A C12 C11 124.5(4) . . ?
O1A C12 C14 116.5(4) . 2_677 ?
C11 C12 H12A 120.5 . . ?
C14 C12 C11 118.9(4) 2_677 . ?
C14 C12 H12A 120.5 2_677 . ?
O11 C13 N2 125.0(6) . . ?
O11 C13 H13 117.5 . . ?
N2 C13 H13 117.5 . . ?
O1B C14 C11 129.4(14) . . ?
O1B C14 C12 109.2(13) . 2_677 ?
C11 C14 C12 120.8(4) . 2_677 ?
C11 C14 H14 119.6 . . ?
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 119.3 . . ?
O10 C1A N3 121.4(19) . . ?
O10 C1A H1AA 119.3 . . ?
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 116.6 . . ?
O10 C1B N3 127(2) . . ?
O10 C1B H1BA 116.6 . . ?
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 -48.8(6) . . . . ?
Tb1 O2 C4 C1 131.8(3) . . . . ?
Tb1 O4 C4 O2 9.0(7) 2_566 . . . ?
Tb1 O4 C4 C1 -171.5(3) 2_566 . . . ?
Tb1 O5 C10 N1 142.8(4) . . . . ?
Tb1 O6 C2 O3 10.8(4) 2_566 . . . ?
Tb1 O6 C2 C3 -168.4(3) 2_566 . . . ?
Tb1 O7 C7 O8 -5.4(4) . . . . ?
Tb1 O7 C7 C11 176.1(3) . . . . ?
Tb1 O8 C7 O7 5.8(4) . . . . ?
Tb1 O8 C7 C11 -175.7(3) . . . . ?
Tb1 O11 C13 N2 166.7(5) . . . . ?
O3 C2 C3 C5 -3.9(6) . . . . ?
O3 C2 C3 C6 175.5(4) . . . 2_666 ?
O6 C2 C3 C5 175.3(4) . . . . ?
O6 C2 C3 C6 -5.3(6) . . . 2_666 ?
O7 C7 C11 C12 -4.7(6) . . . . ?
O7 C7 C11 C14 174.9(4) . . . . ?
O8 C7 C11 C12 176.8(4) . . . . ?
O8 C7 C11 C14 -3.6(6) . . . . ?
C1 C8 C9 O9 179.6(5) . . . . ?
C1 C8 C9 C1 0.4(7) . . . 2_556 ?
C2 C3 C5 C6 179.1(4) . . . . ?
C3 C5 C6 O12 179.8(4) . . . . ?
C3 C5 C6 C3 0.4(7) . . . 2_666 ?
C4 C1 C8 C9 -177.7(4) . . . . ?
C6 C3 C5 C6 -0.4(7) 2_666 . . . ?
C7 C11 C12 O1A -1.4(7) . . . . ?
C7 C11 C12 C14 179.3(4) . . . 2_677 ?
C7 C11 C14 O1B -10(2) . . . . ?
C7 C11 C14 C12 -179.3(4) . . . 2_677 ?
C8 C1 C4 O2 5.8(6) . . . . ?
C8 C1 C4 O4 -173.7(4) . . . . ?
C9 C1 C4 O2 -171.3(4) 2_556 . . . ?
C9 C1 C4 O4 9.2(6) 2_556 . . . ?
C9 C1 C8 C9 -0.4(8) 2_556 . . . ?
C12 C11 C14 O1B 170(2) . . . . ?
C12 C11 C14 C12 0.3(7) . . . 2_677 ?
C14 C11 C12 O1A 179.0(4) . . . . ?
C14 C11 C12 C14 -0.3(7) . . . 2_677 ?
C15 N1 C10 O5 178.6(6) . . . . ?
C16 N1 C10 O5 2.5(10) . . . . ?
C17 N2 C13 O11 2.3(12) . . . . ?
C18 N2 C13 O11 -179.6(8) . . . . ?
C2A N3 C1A O10 -180.0(16) . . . . ?
C3A N3 C1A O10 -1(2) . . . . ?
C2B N3 C1B O10 -12(3) . . . . ?
C3B N3 C1B O10 174.1(18) . . . . ?

_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 1.166
_oxdiff_exptl_absorpt_empirical_full_min 0.828

# start Validation Reply Form
_vrf_PLAT029_SION2_220K          
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.747 Why?  
RESPONSE: The data were collected upon the spindle rotation. Therefore, a 
		  limited portion of the reciprocal space could be probed.
;
# 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_SION2_320K
_database_code_depnum_ccdc_archive 'CCDC 1871312'
loop_
_audit_author_name
_audit_author_address
'Andrzej Gladysiak'
;Ecole polytechnique f?d?rale de Lausanne
Switzerland
;
_audit_update_record             
;
2018-10-03 deposited with the CCDC.	2019-08-12 downloaded from the CCDC.
;
_audit_creation_date             2018-07-09
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_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          ?
_chemical_oxdiff_formula         'C21 H27 N3 O12 Tb'
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                   10.5861(8)
_cell_length_b                   11.0497(6)
_cell_length_c                   12.8741(10)
_cell_angle_alpha                103.021(6)
_cell_angle_beta                 111.135(7)
_cell_angle_gamma                96.698(5)
_cell_volume                     1335.67(18)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5096
_cell_measurement_temperature    320.0
_cell_measurement_theta_max      31.8460
_cell_measurement_theta_min      2.2160
_shelx_estimated_absorpt_T_max   0.833
_shelx_estimated_absorpt_T_min   0.613
_exptl_absorpt_coefficient_mu    2.711
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80722
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.672
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             670
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0202
_diffrn_reflns_av_unetI/netI     0.0304
_diffrn_reflns_Laue_measured_fraction_full 0.736
_diffrn_reflns_Laue_measured_fraction_max 0.675
_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       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8727
_diffrn_reflns_point_group_measured_fraction_full 0.736
_diffrn_reflns_point_group_measured_fraction_max 0.675
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.432
_diffrn_reflns_theta_min         1.948
_diffrn_ambient_temperature      320.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            PILATUS2M
_diffrn_measured_fraction_theta_full 0.736
_diffrn_measured_fraction_theta_max 0.675
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      0.00 360.00   1.00    1.00    --    0.00   0.00   0.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  PILATUS@SNBL
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0626368000
_diffrn_orient_matrix_UB_12      -0.0152275000
_diffrn_orient_matrix_UB_13      0.0340957000
_diffrn_orient_matrix_UB_21      -0.0302979000
_diffrn_orient_matrix_UB_22      -0.0662218000
_diffrn_orient_matrix_UB_23      -0.0273976000
_diffrn_orient_matrix_UB_31      0.0255112000
_diffrn_orient_matrix_UB_32      0.0017338000
_diffrn_orient_matrix_UB_33      -0.0441104000
_diffrn_radiation_monochromator  'Si (111)'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           ?
_diffrn_radiation_wavelength     0.7142
_diffrn_source                   
'European Synchrotron Radiation Facility, BM01 beamline'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4172
_reflns_number_total             4471
_reflns_odcompleteness_completeness 72.56
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.51
_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 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (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    'XT (Sheldrick, 2015)'
_refine_diff_density_max         1.557
_refine_diff_density_min         -1.208
_refine_diff_density_rms         0.099
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         4471
_refine_ls_number_restraints     135
_refine_ls_R_factor_all          0.0346
_refine_ls_R_factor_gt           0.0324
_refine_ls_restrained_S_all      1.086
_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)+(0.0724P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0922
_refine_ls_wR_factor_ref         0.0937
_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
 C18A-N2 \\sim N2-C18B
 with sigma of 0.01
 C17B-N2 \\sim N2-C17A
 with sigma of 0.01
 C13B-N2 \\sim N2-C13A
 with sigma of 0.01
 C13B-O11B \\sim O11A-C13A
 with sigma of 0.01
 C18B-C17B \\sim C17A-C18A
 with sigma of 0.01
3. Restrained planarity
 C13B, C17B, C18B, N2, O11B
 with sigma of 0.1
 C13A, C17A, C18A, N2, O11A
 with sigma of 0.1
4. Rigid bond restraints
 C2, O3
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.005
 O3, C2, O6
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Uiso/Uaniso restraints and constraints
C2 \\sim O3: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.01
C2 \\sim O6: within 2A with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(O1B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C15) \\sim Ueq, Uanis(C16) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C1A) = Uanis(C1B)
Uanis(C3A) = Uanis(C3B)
Uanis(C2A) = Uanis(C2B)
Uanis(O1A) = Uanis(O1B)
Uanis(O11B) = Uanis(O11A)
Uanis(C13A) = Uanis(C13B)
Uanis(C18B) = Uanis(C18A)
Uanis(C17B) = Uanis(C17A)
6. Rigid body (RIGU) restrains
 C1A, C2A, C3A, N3, O10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1B, C2B, C3B, N3, O10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C13A, C17A, C18A, N2, O11A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C13B, C17B, C18B, N2, O11B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. 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(H12)=Sof(O1B)=Sof(H1B)=1-FVAR(2)
 Sof(H14)=Sof(O1A)=Sof(H1A)=FVAR(2)
 Sof(C13B)=Sof(H13B)=Sof(C17B)=Sof(H17D)=Sof(H17E)=Sof(H17F)=Sof(C18B)=
 Sof(H18D)=Sof(H18E)=Sof(H18F)=Sof(O11B)=1-FVAR(3)
 Sof(C13A)=Sof(H13A)=Sof(C17A)=Sof(H17A)=Sof(H17B)=Sof(H17C)=Sof(C18A)=
 Sof(H18A)=Sof(H18B)=Sof(H18C)=Sof(O11A)=FVAR(3)
8.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C8(H8), C10(H10), C12(H12), C13A(H13A), C13B(H13B), C14(H14),
 C1A(H1AA), C1B(H1BA)
8.b Tetrahedral OH refined with riding coordinates:
 O1B(H1B)
8.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17A(H17A,H17B,H17C), C17B(H17D,
 H17E,H17F), C18A(H18A,H18B,H18C), C18B(H18D,H18E,H18F), C2A(H2AA,H2AB,H2AC),
 C2B(H2BA,H2BB,H2BC), C3A(H3AA,H3AB,H3AC), C3B(H3BA,H3BB,H3BC)
8.d Idealised tetrahedral OH refined as rotating group:
 O1A(H1A), O9(H9), O12(H12A)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
C1 C -0.0202(5) 0.1220(4) 0.4929(4) 0.0448(10) Uani 1 1 d . . . . .
C2 C 0.2065(4) 0.4715(4) 0.4437(4) 0.0479(6) Uani 1 1 d . U . . .
C3 C 0.3580(4) 0.4861(4) 0.4707(4) 0.0459(11) Uani 1 1 d . . . . .
C4 C -0.0363(4) 0.2545(3) 0.4924(4) 0.0414(10) Uani 1 1 d . . . . .
C5 C 0.4517(5) 0.5351(5) 0.5878(4) 0.0543(12) Uani 1 1 d . . . . .
H5 H 0.4191 0.5581 0.6459 0.065 Uiso 1 1 calc R . . . .
C6 C 0.5942(5) 0.5490(5) 0.6164(5) 0.0532(13) Uani 1 1 d . . . . .
C7 C 0.2974(5) 0.7696(4) 0.8453(4) 0.0490(11) Uani 1 1 d . . . . .
C8 C 0.0035(6) 0.0880(4) 0.5952(4) 0.0544(12) Uani 1 1 d . . . . .
H8 H 0.0054 0.1476 0.6599 0.065 Uiso 1 1 calc R . . . .
C9 C 0.0242(6) -0.0317(4) 0.6040(4) 0.0561(13) Uani 1 1 d . . . . .
C10 C -0.0145(7) 0.3852(6) 0.8238(6) 0.0736(17) Uani 1 1 d . . . . .
H10 H -0.1005 0.3683 0.7622 0.088 Uiso 1 1 calc R . . . .
C11 C 0.4005(5) 0.8903(4) 0.9268(4) 0.0484(11) Uani 1 1 d . . . . .
C12 C 0.3643(5) 0.9851(5) 0.9954(5) 0.0542(12) Uani 1 1 d . . . . .
H12 H 0.2745 0.9753 0.9924 0.065 Uiso 0.119(8) 1 calc R . P A 2
C13A C 0.3902(10) 0.4265(9) 0.7997(9) 0.073(2) Uani 0.628(10) 1 d D U P B 1
H13A H 0.4501 0.5054 0.8247 0.087 Uiso 0.628(10) 1 calc R . P B 1
C13B C 0.3109(13) 0.3394(15) 0.7534(14) 0.073(2) Uani 0.372(10) 1 d D U P B 2
H13B H 0.2399 0.2691 0.7047 0.087 Uiso 0.372(10) 1 calc R . P B 2
C14 C 0.5357(5) 0.9051(4) 0.9315(4) 0.0516(11) Uani 1 1 d . . . . .
H14 H 0.5591 0.8414 0.8856 0.062 Uiso 0.881(8) 1 calc R . P A 1
C15 C -0.1068(14) 0.2045(12) 0.8719(12) 0.148(4) Uani 1 1 d . U . . .
H15A H -0.1378 0.2209 0.9342 0.222 Uiso 1 1 calc GR . . . .
H15B H -0.0715 0.1281 0.8688 0.222 Uiso 1 1 calc GR . . . .
H15C H -0.1831 0.1941 0.7996 0.222 Uiso 1 1 calc GR . . . .
C16 C 0.1317(16) 0.3283(14) 0.9841(12) 0.165(5) Uani 1 1 d . U . . .
H16A H 0.1749 0.4172 1.0152 0.247 Uiso 1 1 calc GR . . . .
H16B H 0.1901 0.2824 0.9560 0.247 Uiso 1 1 calc GR . . . .
H16C H 0.1182 0.2971 1.0441 0.247 Uiso 1 1 calc GR . . . .
C17A C 0.3596(18) 0.2017(15) 0.7982(19) 0.149(6) Uani 0.628(10) 1 d D U P B 1
H17A H 0.3226 0.1973 0.8556 0.223 Uiso 0.628(10) 1 calc GR . P B 1
H17B H 0.4169 0.1408 0.7960 0.223 Uiso 0.628(10) 1 calc GR . P B 1
H17C H 0.2847 0.1831 0.7233 0.223 Uiso 0.628(10) 1 calc GR . P B 1
C17B C 0.424(3) 0.1900(15) 0.801(3) 0.149(6) Uani 0.372(10) 1 d D U P B 2
H17D H 0.3714 0.1574 0.8402 0.223 Uiso 0.372(10) 1 calc GR . P B 2
H17E H 0.5138 0.1702 0.8274 0.223 Uiso 0.372(10) 1 calc GR . P B 2
H17F H 0.3759 0.1518 0.7188 0.223 Uiso 0.372(10) 1 calc GR . P B 2
C18A C 0.5931(15) 0.3489(19) 0.8966(19) 0.153(7) Uani 0.628(10) 1 d D U P B 1
H18A H 0.6143 0.3943 0.9759 0.229 Uiso 0.628(10) 1 calc GR . P B 1
H18B H 0.6406 0.3992 0.8644 0.229 Uiso 0.628(10) 1 calc GR . P B 1
H18C H 0.6226 0.2698 0.8939 0.229 Uiso 0.628(10) 1 calc GR . P B 1
C18B C 0.579(2) 0.405(2) 0.906(3) 0.153(7) Uani 0.372(10) 1 d D U P B 2
H18D H 0.5858 0.4869 0.8921 0.229 Uiso 0.372(10) 1 calc GR . P B 2
H18E H 0.6492 0.3655 0.8910 0.229 Uiso 0.372(10) 1 calc GR . P B 2
H18F H 0.5919 0.4154 0.9854 0.229 Uiso 0.372(10) 1 calc GR . P B 2
N1 N 0.0023(8) 0.3107(6) 0.8918(5) 0.0880(19) Uani 1 1 d . . . . .
N2 N 0.4381(7) 0.3227(7) 0.8267(6) 0.101(2) Uani 1 1 d D U . . .
O1A O 0.2351(5) 0.9784(5) 0.9939(5) 0.0722(15) Uani 0.881(8) 1 d . . P A 1
H1A H 0.1834 0.9126 0.9457 0.108 Uiso 0.881(8) 1 calc GR . P A 1
O1B O 0.593(3) 0.814(3) 0.882(3) 0.0722(15) Uani 0.119(8) 1 d . U P A 2
H1B H 0.5327 0.7502 0.8414 0.108 Uiso 0.119(8) 1 calc R . P A 2
O2 O -0.0129(4) 0.3344(3) 0.5874(3) 0.0471(8) Uani 1 1 d . . . . .
O3 O 0.1644(3) 0.4963(3) 0.5236(3) 0.0491(6) Uani 1 1 d . U . . .
O4 O -0.0716(4) 0.2774(3) 0.3949(3) 0.0502(8) Uani 1 1 d . . . . .
O5 O 0.0742(4) 0.4759(3) 0.8347(3) 0.0637(10) Uani 1 1 d . . . . .
O6 O 0.1223(3) 0.4353(3) 0.3374(3) 0.0516(7) Uani 1 1 d . U . . .
O7 O 0.1770(3) 0.7499(3) 0.8475(3) 0.0538(8) Uani 1 1 d . . . . .
O8 O 0.3315(4) 0.6902(3) 0.7820(4) 0.0668(11) Uani 1 1 d . . . . .
O9 O 0.0483(7) -0.0540(4) 0.7078(4) 0.0929(18) Uani 1 1 d . . . . .
H9 H 0.0696 -0.1232 0.7062 0.139 Uiso 1 1 calc GR . . . .
O11A O 0.2688(11) 0.4124(11) 0.7430(13) 0.076(2) Uani 0.628(10) 1 d D U P B 1
O11B O 0.294(2) 0.4449(18) 0.754(2) 0.076(2) Uani 0.372(10) 1 d D U P B 2
O12 O 0.6800(4) 0.5970(6) 0.7304(3) 0.0794(14) Uani 1 1 d . . . . .
H12A H 0.7606 0.6116 0.7368 0.119 Uiso 1 1 calc GR . . . .
Tb1 Tb 0.10643(2) 0.54644(2) 0.68224(2) 0.03650(10) Uani 1 1 d . . . . .
C1A C 0.612(4) 0.189(3) 0.540(3) 0.178(7) Uani 0.535(13) 1 d . U P C 1
H1AA H 0.6907 0.1866 0.5239 0.213 Uiso 0.535(13) 1 calc R . P C 1
C1B C 0.500(5) 0.198(4) 0.555(3) 0.178(7) Uani 0.465(13) 1 d . U P C 2
H1BA H 0.4241 0.2134 0.5717 0.213 Uiso 0.465(13) 1 calc R . P C 2
C2A C 0.438(4) 0.112(3) 0.329(3) 0.182(8) Uani 0.535(13) 1 d . U P C 1
H2AA H 0.5136 0.1428 0.3098 0.273 Uiso 0.535(13) 1 calc GR . P C 1
H2AB H 0.3596 0.1458 0.2918 0.273 Uiso 0.535(13) 1 calc GR . P C 1
H2AC H 0.4140 0.0212 0.3019 0.273 Uiso 0.535(13) 1 calc GR . P C 1
C2B C 0.597(4) 0.143(4) 0.420(3) 0.182(8) Uani 0.465(13) 1 d . U P C 2
H2BA H 0.6813 0.1853 0.4867 0.273 Uiso 0.465(13) 1 calc GR . P C 2
H2BB H 0.5896 0.1809 0.3587 0.273 Uiso 0.465(13) 1 calc GR . P C 2
H2BC H 0.5983 0.0543 0.3941 0.273 Uiso 0.465(13) 1 calc GR . P C 2
C3A C 0.351(3) 0.145(3) 0.475(3) 0.168(6) Uani 0.535(13) 1 d . U P C 1
H3AA H 0.3119 0.0571 0.4632 0.251 Uiso 0.535(13) 1 calc GR . P C 1
H3AB H 0.2842 0.1793 0.4240 0.251 Uiso 0.535(13) 1 calc GR . P C 1
H3AC H 0.3736 0.1919 0.5546 0.251 Uiso 0.535(13) 1 calc GR . P C 1
C3B C 0.332(4) 0.122(3) 0.358(3) 0.168(6) Uani 0.465(13) 1 d . U P C 2
H3BA H 0.2671 0.1294 0.3941 0.251 Uiso 0.465(13) 1 calc GR . P C 2
H3BB H 0.3114 0.0371 0.3083 0.251 Uiso 0.465(13) 1 calc GR . P C 2
H3BC H 0.3242 0.1810 0.3121 0.251 Uiso 0.465(13) 1 calc GR . P C 2
N3 N 0.4793(14) 0.1535(9) 0.4512(11) 0.144(3) Uani 1 1 d . U . . .
O10 O 0.6187(14) 0.2238(13) 0.6394(11) 0.200(5) Uani 1 1 d . U . . .


_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
C1 C4 1.495(5) . ?
C1 C8 1.395(7) . ?
C1 C9 1.394(7) 2_556 ?
C2 C3 1.494(6) . ?
C2 O3 1.251(7) . ?
C2 O6 1.271(6) . ?
C3 C5 1.406(6) . ?
C3 C6 1.386(8) 2_666 ?
C4 O2 1.257(5) . ?
C4 O4 1.267(5) . ?
C5 H5 0.9300 . ?
C5 C6 1.397(7) . ?
C6 C3 1.386(8) 2_666 ?
C6 O12 1.355(6) . ?
C7 C11 1.508(5) . ?
C7 O7 1.278(7) . ?
C7 O8 1.237(7) . ?
C8 H8 0.9300 . ?
C8 C9 1.388(6) . ?
C9 C1 1.394(7) 2_556 ?
C9 O9 1.353(7) . ?
C10 H10 0.9300 . ?
C10 N1 1.313(8) . ?
C10 O5 1.236(7) . ?
C11 C12 1.395(8) . ?
C11 C14 1.399(7) . ?
C12 H12 0.9300 . ?
C12 C14 1.394(6) 2_677 ?
C12 O1A 1.354(7) . ?
C13A H13A 0.9300 . ?
C13A N2 1.371(9) . ?
C13A O11A 1.197(12) . ?
C13B H13B 0.9300 . ?
C13B N2 1.399(11) . ?
C13B O11B 1.199(14) . ?
C14 C12 1.394(6) 2_677 ?
C14 H14 0.9300 . ?
C14 O1B 1.38(4) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C15 N1 1.453(12) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C16 N1 1.409(13) . ?
C17A H17A 0.9600 . ?
C17A H17B 0.9600 . ?
C17A H17C 0.9600 . ?
C17A N2 1.383(14) . ?
C17B H17D 0.9600 . ?
C17B H17E 0.9600 . ?
C17B H17F 0.9600 . ?
C17B N2 1.406(15) . ?
C18A H18A 0.9600 . ?
C18A H18B 0.9600 . ?
C18A H18C 0.9600 . ?
C18A N2 1.514(14) . ?
C18B H18D 0.9600 . ?
C18B H18E 0.9600 . ?
C18B H18F 0.9600 . ?
C18B N2 1.503(16) . ?
O1A H1A 0.8200 . ?
O1B H1B 0.8200 . ?
O2 Tb1 2.342(3) . ?
O3 Tb1 2.308(4) . ?
O4 Tb1 2.384(3) 2_566 ?
O5 Tb1 2.385(4) . ?
O6 Tb1 2.380(3) 2_566 ?
O7 Tb1 2.539(3) . ?
O8 Tb1 2.417(3) . ?
O9 H9 0.8200 . ?
O11A Tb1 2.431(10) . ?
O11B Tb1 2.392(18) . ?
O12 H12A 0.8200 . ?
Tb1 O4 2.384(3) 2_566 ?
Tb1 O6 2.380(3) 2_566 ?
C1A H1AA 0.9300 . ?
C1A N3 1.39(4) . ?
C1A O10 1.23(4) . ?
C1B H1BA 0.9300 . ?
C1B N3 1.24(4) . ?
C1B O10 1.28(4) . ?
C2A H2AA 0.9600 . ?
C2A H2AB 0.9600 . ?
C2A H2AC 0.9600 . ?
C2A N3 1.42(3) . ?
C2B H2BA 0.9600 . ?
C2B H2BB 0.9600 . ?
C2B H2BC 0.9600 . ?
C2B N3 1.45(4) . ?
C3A H3AA 0.9600 . ?
C3A H3AB 0.9600 . ?
C3A H3AC 0.9600 . ?
C3A N3 1.50(3) . ?
C3B H3BA 0.9600 . ?
C3B H3BB 0.9600 . ?
C3B H3BC 0.9600 . ?
C3B N3 1.53(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C8 C1 C4 118.8(4) . . ?
C9 C1 C4 122.7(4) 2_556 . ?
C9 C1 C8 118.5(4) 2_556 . ?
O3 C2 C3 120.7(4) . . ?
O3 C2 O6 121.2(4) . . ?
O6 C2 C3 118.1(5) . . ?
C5 C3 C2 118.1(5) . . ?
C6 C3 C2 121.4(4) 2_666 . ?
C6 C3 C5 120.5(4) 2_666 . ?
O2 C4 C1 118.3(4) . . ?
O2 C4 O4 125.1(4) . . ?
O4 C4 C1 116.6(4) . . ?
C3 C5 H5 120.2 . . ?
C6 C5 C3 119.7(5) . . ?
C6 C5 H5 120.2 . . ?
C3 C6 C5 119.8(4) 2_666 . ?
O12 C6 C3 122.9(4) . 2_666 ?
O12 C6 C5 117.3(5) . . ?
O7 C7 C11 118.2(5) . . ?
O8 C7 C11 120.2(5) . . ?
O8 C7 O7 121.5(4) . . ?
C1 C8 H8 118.8 . . ?
C9 C8 C1 122.4(4) . . ?
C9 C8 H8 118.8 . . ?
C8 C9 C1 119.2(4) . 2_556 ?
O9 C9 C1 123.3(4) . 2_556 ?
O9 C9 C8 117.5(4) . . ?
N1 C10 H10 117.2 . . ?
O5 C10 H10 117.2 . . ?
O5 C10 N1 125.5(7) . . ?
C12 C11 C7 122.0(5) . . ?
C12 C11 C14 120.3(4) . . ?
C14 C11 C7 117.7(5) . . ?
C11 C12 H12 120.4 . . ?
C14 C12 C11 119.3(5) 2_677 . ?
C14 C12 H12 120.4 2_677 . ?
O1A C12 C11 123.6(4) . . ?
O1A C12 C14 117.1(5) . 2_677 ?
N2 C13A H13A 121.0 . . ?
O11A C13A H13A 121.0 . . ?
O11A C13A N2 118.0(10) . . ?
N2 C13B H13B 120.3 . . ?
O11B C13B H13B 120.3 . . ?
O11B C13B N2 119.4(18) . . ?
C11 C14 H14 119.8 . . ?
C12 C14 C11 120.4(5) 2_677 . ?
C12 C14 H14 119.8 2_677 . ?
O1B C14 C11 127.4(13) . . ?
O1B C14 C12 111.6(13) . 2_677 ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N1 C15 H15A 109.5 . . ?
N1 C15 H15B 109.5 . . ?
N1 C15 H15C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N1 C16 H16A 109.5 . . ?
N1 C16 H16B 109.5 . . ?
N1 C16 H16C 109.5 . . ?
H17A C17A H17B 109.5 . . ?
H17A C17A H17C 109.5 . . ?
H17B C17A H17C 109.5 . . ?
N2 C17A H17A 109.5 . . ?
N2 C17A H17B 109.5 . . ?
N2 C17A H17C 109.5 . . ?
H17D C17B H17E 109.5 . . ?
H17D C17B H17F 109.5 . . ?
H17E C17B H17F 109.5 . . ?
N2 C17B H17D 109.5 . . ?
N2 C17B H17E 109.5 . . ?
N2 C17B H17F 109.5 . . ?
H18A C18A H18B 109.5 . . ?
H18A C18A H18C 109.5 . . ?
H18B C18A H18C 109.5 . . ?
N2 C18A H18A 109.5 . . ?
N2 C18A H18B 109.5 . . ?
N2 C18A H18C 109.5 . . ?
H18D C18B H18E 109.5 . . ?
H18D C18B H18F 109.5 . . ?
H18E C18B H18F 109.5 . . ?
N2 C18B H18D 109.5 . . ?
N2 C18B H18E 109.5 . . ?
N2 C18B H18F 109.5 . . ?
C10 N1 C15 122.1(8) . . ?
C10 N1 C16 120.0(8) . . ?
C16 N1 C15 117.8(8) . . ?
C13A N2 C17A 126.6(10) . . ?
C13A N2 C18A 114.4(10) . . ?
C13B N2 C17B 104.4(14) . . ?
C13B N2 C18B 137.0(14) . . ?
C17A N2 C18A 119.0(10) . . ?
C17B N2 C18B 117.9(13) . . ?
C12 O1A H1A 109.5 . . ?
C14 O1B H1B 109.5 . . ?
C4 O2 Tb1 136.1(3) . . ?
C2 O3 Tb1 175.1(3) . . ?
C4 O4 Tb1 139.0(3) . 2_566 ?
C10 O5 Tb1 126.8(4) . . ?
C2 O6 Tb1 111.2(3) . 2_566 ?
C7 O7 Tb1 89.5(3) . . ?
C7 O8 Tb1 96.2(3) . . ?
C9 O9 H9 109.5 . . ?
C13A O11A Tb1 137.4(9) . . ?
C13B O11B Tb1 138.1(18) . . ?
C6 O12 H12A 109.5 . . ?
O2 Tb1 O4 126.21(11) . 2_566 ?
O2 Tb1 O5 77.39(12) . . ?
O2 Tb1 O6 79.61(12) . 2_566 ?
O2 Tb1 O7 151.69(13) . . ?
O2 Tb1 O8 145.53(13) . . ?
O2 Tb1 O11A 72.5(3) . . ?
O2 Tb1 O11B 81.4(6) . . ?
O3 Tb1 O2 77.04(12) . . ?
O3 Tb1 O4 76.55(12) . 2_566 ?
O3 Tb1 O5 145.78(13) . . ?
O3 Tb1 O6 122.09(12) . 2_566 ?
O3 Tb1 O7 131.26(11) . . ?
O3 Tb1 O8 86.29(13) . . ?
O3 Tb1 O11A 79.7(4) . . ?
O3 Tb1 O11B 79.3(7) . . ?
O4 Tb1 O5 137.52(13) 2_566 . ?
O4 Tb1 O7 70.35(11) 2_566 . ?
O4 Tb1 O8 77.15(13) 2_566 . ?
O4 Tb1 O11A 144.2(3) 2_566 . ?
O4 Tb1 O11B 136.7(6) 2_566 . ?
O5 Tb1 O7 76.28(12) . . ?
O5 Tb1 O8 102.60(15) . . ?
O5 Tb1 O11A 71.1(4) . . ?
O5 Tb1 O11B 74.6(7) . . ?
O6 Tb1 O4 76.24(12) 2_566 2_566 ?
O6 Tb1 O5 74.57(13) 2_566 . ?
O6 Tb1 O7 83.55(12) 2_566 . ?
O6 Tb1 O8 134.22(12) 2_566 . ?
O6 Tb1 O11A 139.5(3) 2_566 . ?
O6 Tb1 O11B 146.6(6) 2_566 . ?
O8 Tb1 O7 52.50(13) . . ?
O8 Tb1 O11A 75.0(3) . . ?
O11A Tb1 O7 108.1(3) . . ?
O11B Tb1 O7 101.4(6) . . ?
O11B Tb1 O8 65.9(6) . . ?
N3 C1A H1AA 121.8 . . ?
O10 C1A H1AA 121.8 . . ?
O10 C1A N3 116(4) . . ?
N3 C1B H1BA 117.8 . . ?
N3 C1B O10 124(4) . . ?
O10 C1B H1BA 117.8 . . ?
H2AA C2A H2AB 109.5 . . ?
H2AA C2A H2AC 109.5 . . ?
H2AB C2A H2AC 109.5 . . ?
N3 C2A H2AA 109.5 . . ?
N3 C2A H2AB 109.5 . . ?
N3 C2A H2AC 109.5 . . ?
H2BA C2B H2BB 109.5 . . ?
H2BA C2B H2BC 109.5 . . ?
H2BB C2B H2BC 109.5 . . ?
N3 C2B H2BA 109.5 . . ?
N3 C2B H2BB 109.5 . . ?
N3 C2B H2BC 109.5 . . ?
H3AA C3A H3AB 109.5 . . ?
H3AA C3A H3AC 109.5 . . ?
H3AB C3A H3AC 109.5 . . ?
N3 C3A H3AA 109.5 . . ?
N3 C3A H3AB 109.5 . . ?
N3 C3A H3AC 109.5 . . ?
H3BA C3B H3BB 109.5 . . ?
H3BA C3B H3BC 109.5 . . ?
H3BB C3B H3BC 109.5 . . ?
N3 C3B H3BA 109.5 . . ?
N3 C3B H3BB 109.5 . . ?
N3 C3B H3BC 109.5 . . ?
C1A N3 C2A 129(3) . . ?
C1A N3 C3A 122(2) . . ?
C1B N3 C2B 119(3) . . ?
C1B N3 C3B 120(3) . . ?
C2A N3 C3A 108(2) . . ?
C2B N3 C3B 121(2) . . ?

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
C1 C4 O2 Tb1 135.4(4) . . . . ?
C1 C4 O4 Tb1 -175.5(3) . . . 2_566 ?
C1 C8 C9 C1 -0.5(9) . . . 2_556 ?
C1 C8 C9 O9 179.1(6) . . . . ?
C2 C3 C5 C6 179.4(5) . . . . ?
C3 C2 O6 Tb1 -170.3(3) . . . 2_566 ?
C3 C5 C6 C3 -0.3(9) . . . 2_666 ?
C3 C5 C6 O12 179.8(5) . . . . ?
C4 C1 C8 C9 -177.7(5) . . . . ?
C6 C3 C5 C6 0.4(9) 2_666 . . . ?
C7 C11 C12 C14 -179.7(4) . . . 2_677 ?
C7 C11 C12 O1A -1.0(8) . . . . ?
C7 C11 C14 C12 179.7(4) . . . 2_677 ?
C7 C11 C14 O1B -10(2) . . . . ?
C8 C1 C4 O2 7.6(7) . . . . ?
C8 C1 C4 O4 -173.1(4) . . . . ?
C9 C1 C4 O2 -170.6(5) 2_556 . . . ?
C9 C1 C4 O4 8.7(7) 2_556 . . . ?
C9 C1 C8 C9 0.5(9) 2_556 . . . ?
C11 C7 O7 Tb1 177.2(4) . . . . ?
C11 C7 O8 Tb1 -176.9(4) . . . . ?
C12 C11 C14 C12 -0.1(9) . . . 2_677 ?
C12 C11 C14 O1B 170(2) . . . . ?
C14 C11 C12 C14 0.1(9) . . . 2_677 ?
C14 C11 C12 O1A 178.8(5) . . . . ?
N1 C10 O5 Tb1 146.1(6) . . . . ?
N2 C13A O11A Tb1 170.8(11) . . . . ?
N2 C13B O11B Tb1 -168(2) . . . . ?
O2 C4 O4 Tb1 3.8(8) . . . 2_566 ?
O3 C2 C3 C5 -3.5(7) . . . . ?
O3 C2 C3 C6 175.6(5) . . . 2_666 ?
O3 C2 O6 Tb1 8.5(5) . . . 2_566 ?
O4 C4 O2 Tb1 -43.9(7) . . . . ?
O5 C10 N1 C15 -179.0(10) . . . . ?
O5 C10 N1 C16 -2.4(15) . . . . ?
O6 C2 C3 C5 175.4(4) . . . . ?
O6 C2 C3 C6 -5.6(7) . . . 2_666 ?
O7 C7 C11 C12 -6.1(7) . . . . ?
O7 C7 C11 C14 174.1(5) . . . . ?
O7 C7 O8 Tb1 6.0(5) . . . . ?
O8 C7 C11 C12 176.7(5) . . . . ?
O8 C7 C11 C14 -3.1(7) . . . . ?
O8 C7 O7 Tb1 -5.7(5) . . . . ?
O11A C13A N2 C17A -2.2(16) . . . . ?
O11A C13A N2 C18A 179.0(10) . . . . ?
O11B C13B N2 C17B -178.1(12) . . . . ?
O11B C13B N2 C18B -8(2) . . . . ?
O10 C1A N3 C2A 178(2) . . . . ?
O10 C1A N3 C3A -6(4) . . . . ?
O10 C1B N3 C2B -7(5) . . . . ?
O10 C1B N3 C3B 178(3) . . . . ?

_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 1.161
_oxdiff_exptl_absorpt_empirical_full_min 0.881

# start Validation Reply Form
_vrf_PLAT029_SION2_320K          
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.736 Why?  
RESPONSE: The data were collected upon the spindle rotation. Therefore, a 
		  limited portion of the reciprocal space could be probed.
;
# 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_SION2_120K_cool
_database_code_depnum_ccdc_archive 'CCDC 1941012'
loop_
_audit_author_name
_audit_author_address
'Andrzej Gladysiak'
;Ecole polytechnique federale de Lausanne
Switzerland
;
_audit_update_record             
;
2019-07-16 deposited with the CCDC.	2019-08-12 downloaded from the CCDC.
;
_audit_creation_date             2019-05-27
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C18 H20 N2 O11 Tb'
_chemical_formula_sum            'C18 H20 N2 O11 Tb'
_chemical_formula_weight         599.28
_chemical_melting_point          ?
_chemical_oxdiff_formula         C21H27N3O12Tb
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0045 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'
N N 0.0083 0.0040 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0145 0.0076 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.0972 4.9386 '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                   10.6311(6)
_cell_length_b                   11.1791(5)
_cell_length_c                   11.3767(5)
_cell_angle_alpha                96.958(4)
_cell_angle_beta                 110.894(5)
_cell_angle_gamma                101.422(4)
_cell_volume                     1210.70(11)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3208
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      32.2210
_cell_measurement_theta_min      2.1400
_shelx_estimated_absorpt_T_max   0.775
_shelx_estimated_absorpt_T_min   0.514
_exptl_absorpt_coefficient_mu    3.839
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86950
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.644
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             590
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0084
_diffrn_reflns_av_unetI/netI     0.0132
_diffrn_reflns_Laue_measured_fraction_full 0.713
_diffrn_reflns_Laue_measured_fraction_max 0.547
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6772
_diffrn_reflns_point_group_measured_fraction_full 0.713
_diffrn_reflns_point_group_measured_fraction_max 0.547
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         32.158
_diffrn_reflns_theta_min         2.097
_diffrn_ambient_temperature      120.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            PILATUS2M
_diffrn_measured_fraction_theta_full 0.713
_diffrn_measured_fraction_theta_max 0.547
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      0.00 360.00   1.00    1.00    --    0.00   0.00   0.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  PILATUS@SNBL
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0667389000
_diffrn_orient_matrix_UB_12      -0.0037505000
_diffrn_orient_matrix_UB_13      -0.0132848000
_diffrn_orient_matrix_UB_21      0.0459244000
_diffrn_orient_matrix_UB_22      0.0517033000
_diffrn_orient_matrix_UB_23      0.0620897000
_diffrn_orient_matrix_UB_31      0.0109966000
_diffrn_orient_matrix_UB_32      -0.0516459000
_diffrn_orient_matrix_UB_33      0.0407396000
_diffrn_radiation_monochromator  'Si (111)'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.78405
_diffrn_source                   
'European Synchrotron Radiation Facility, BM01 beamline'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3308
_reflns_number_total             3474
_reflns_odcompleteness_completeness 62.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     29.34
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         6.598
_refine_diff_density_min         -2.166
_refine_diff_density_rms         0.251
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     292
_refine_ls_number_reflns         3474
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.0705
_refine_ls_R_factor_gt           0.0688
_refine_ls_restrained_S_all      6.414
_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)+(0.1485P)²+5.0408P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1812
_refine_ls_wR_factor_ref         0.1859
_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
 C17-C13 \\sim C13-C18
 with sigma of 0.02
 C12_$8-O1 \\sim O1-C11
 with sigma of 0.05
3. Restrained planarity
 C13, C17, C18, N2, O11
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C17) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
5.a Me refined with riding coordinates:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C)
5.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C8(H8), C12(H12), C13(H13), C16(H16)
5.c Tetrahedral OH refined with riding coordinates:
 O1(H1), O12(H12A)
5.d Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C15(H15A,H15B,H15C)
5.e Idealised tetrahedral OH refined as rotating group:
 O9(H9)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
C1 C -0.0208(8) 0.1211(9) 0.4964(10) 0.036(3) Uani 1 1 d . . . . .
C2 C 0.2051(8) 0.4848(9) 0.4310(9) 0.033(2) Uani 1 1 d . . . . .
C3 C 0.3574(8) 0.4947(9) 0.4664(10) 0.037(2) Uani 1 1 d . . . . .
C4 C -0.0357(9) 0.2518(9) 0.4998(11) 0.038(3) Uani 1 1 d . . . . .
C5 C 0.4505(10) 0.5366(11) 0.5945(9) 0.044(3) Uani 1 1 d . . . . .
H5 H 0.417365 0.561908 0.658243 0.053 Uiso 1 1 calc R . . . .
C6 C 0.5939(10) 0.5420(12) 0.6308(10) 0.045(3) Uani 1 1 d . . . . .
C7 C 0.3019(8) 0.7602(9) 0.8598(9) 0.035(2) Uani 1 1 d . . . . .
C8 C 0.0038(10) 0.0741(10) 0.6093(10) 0.042(3) Uani 1 1 d . . . . .
H8 H 0.006024 0.124672 0.683825 0.051 Uiso 1 1 calc R . . . .
C9 C 0.0249(10) -0.0444(10) 0.6155(9) 0.036(2) Uani 1 1 d . . . . .
C10 C 0.0497(13) 0.1787(14) 0.9907(15) 0.061(4) Uani 1 1 d . . . . .
H10A H 0.017013 0.180206 1.061095 0.091 Uiso 1 1 calc GR . . . .
H10B H 0.150481 0.187747 1.025217 0.091 Uiso 1 1 calc GR . . . .
H10C H 0.001963 0.099260 0.928458 0.091 Uiso 1 1 calc GR . . . .
C11 C 0.4010(9) 0.8855(9) 0.9322(10) 0.041(3) Uani 1 1 d D . . . .
C12 C 0.3626(10) 0.9689(11) 0.9934(12) 0.054(3) Uani 1 1 d D . . . .
H12 H 0.271063 0.949482 0.992588 0.064 Uiso 1 1 calc R . . A 2
C13 C 0.3102(12) 0.3295(12) 0.7220(12) 0.065(4) Uani 1 1 d D . . . .
H13 H 0.241478 0.279915 0.642733 0.078 Uiso 1 1 calc R . . . .
C14 C 0.5428(9) 0.9094(11) 0.9374(12) 0.050(3) Uani 1 1 d . . . . .
C15 C -0.1278(13) 0.2758(15) 0.8586(15) 0.064(4) Uani 1 1 d . . . . .
H15A H -0.169375 0.294517 0.920677 0.095 Uiso 1 1 calc GR . . . .
H15B H -0.178091 0.192535 0.804496 0.095 Uiso 1 1 calc GR . . . .
H15C H -0.134126 0.337971 0.804471 0.095 Uiso 1 1 calc GR . . . .
C16 C 0.1171(12) 0.3730(14) 0.9346(12) 0.052(4) Uani 1 1 d . . . . .
H16 H 0.210730 0.372873 0.982819 0.062 Uiso 1 1 calc R . . . .
C17 C 0.434(3) 0.175(2) 0.703(3) 0.129(8) Uani 1 1 d D U . . .
H17A H 0.522637 0.157746 0.750953 0.194 Uiso 1 1 calc R . . . .
H17B H 0.356646 0.105627 0.695438 0.194 Uiso 1 1 calc R . . . .
H17C H 0.428049 0.184792 0.617107 0.194 Uiso 1 1 calc R . . . .
C18 C 0.5325(17) 0.367(2) 0.8938(19) 0.096(6) Uani 1 1 d D . . . .
H18A H 0.609630 0.327089 0.919020 0.143 Uiso 1 1 calc R . . . .
H18B H 0.566458 0.451098 0.882460 0.143 Uiso 1 1 calc R . . . .
H18C H 0.495140 0.372107 0.960960 0.143 Uiso 1 1 calc R . . . .
N1 N 0.0199(9) 0.2793(10) 0.9283(9) 0.046(2) Uani 1 1 d . . . . .
N2 N 0.4235(12) 0.2936(12) 0.7738(13) 0.073(4) Uani 1 1 d . . . . .
O1 O 0.5935(8) 0.8190(9) 0.8806(12) 0.080(4) Uani 1 1 d D . . . .
H1 H 0.527034 0.756482 0.836614 0.121 Uiso 1 1 calc R . . . .
O2 O -0.0088(6) 0.3208(6) 0.6075(7) 0.0360(16) Uani 1 1 d . . . . .
O3 O 0.1594(6) 0.5048(7) 0.5171(7) 0.0402(18) Uani 1 1 d . . . . .
O4 O -0.0720(7) 0.2867(7) 0.3911(7) 0.0378(17) Uani 1 1 d . . . . .
O5 O 0.0978(9) 0.4649(9) 0.8820(8) 0.050(2) Uani 1 1 d . . . . .
O6 O 0.1223(6) 0.4579(7) 0.3104(7) 0.0400(17) Uani 1 1 d . . . . .
O7 O 0.1855(6) 0.7308(7) 0.8711(6) 0.0373(16) Uani 1 1 d . . . . .
O8 O 0.3366(7) 0.6847(7) 0.7904(8) 0.046(2) Uani 1 1 d . . . . .
O9 O 0.0468(10) -0.0812(8) 0.7297(8) 0.053(2) Uani 1 1 d . . . . .
H9 H 0.054722 -0.154717 0.722035 0.079 Uiso 1 1 calc GR . . . .
O11 O 0.2861(7) 0.4241(8) 0.7692(9) 0.055(2) Uani 1 1 d . . . . .
O12 O 0.6793(7) 0.5816(10) 0.7579(8) 0.061(3) Uani 1 1 d . . . . .
H12A H 0.761116 0.580390 0.767734 0.092 Uiso 1 1 calc R . . . .
Tb1 Tb 0.10700(3) 0.53538(3) 0.69967(4) 0.0307(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
C1 C4 1.499(15) . ?
C1 C8 1.405(17) . ?
C1 C9 1.428(12) 2_556 ?
C2 C3 1.500(11) . ?
C2 O3 1.255(11) . ?
C2 O6 1.297(12) . ?
C3 C5 1.394(13) . ?
C3 C6 1.428(13) 2_666 ?
C4 O2 1.269(11) . ?
C4 O4 1.291(14) . ?
C5 H5 0.9500 . ?
C5 C6 1.417(13) . ?
C6 O12 1.365(12) . ?
C7 C11 1.506(12) . ?
C7 O7 1.272(11) . ?
C7 O8 1.281(11) . ?
C8 H8 0.9500 . ?
C8 C9 1.393(16) . ?
C9 O9 1.365(14) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C10 N1 1.43(2) . ?
C11 C12 1.310(14) . ?
C11 C14 1.456(12) . ?
C12 H12 0.9500 . ?
C12 C14 1.455(13) 2_677 ?
C13 H13 0.9500 . ?
C13 N2 1.305(18) . ?
C13 O11 1.241(15) . ?
C14 O1 1.427(12) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C15 N1 1.475(16) . ?
C16 H16 0.9500 . ?
C16 N1 1.293(17) . ?
C16 O5 1.265(18) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C17 N2 1.51(2) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C18 N2 1.45(2) . ?
O1 H1 0.8400 . ?
O2 Tb1 2.381(6) . ?
O3 Tb1 2.339(7) . ?
O4 Tb1 2.383(8) 2_566 ?
O5 Tb1 2.333(10) . ?
O6 Tb1 2.416(6) 2_566 ?
O7 Tb1 2.521(6) . ?
O8 Tb1 2.445(6) . ?
O9 H9 0.8400 . ?
O11 Tb1 2.430(8) . ?
O12 H12A 0.8400 . ?

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
C8 C1 C4 118.6(8) . . ?
C8 C1 C9 118.8(9) . 2_556 ?
C9 C1 C4 122.5(10) 2_556 . ?
O3 C2 C3 120.3(8) . . ?
O3 C2 O6 120.7(7) . . ?
O6 C2 C3 119.0(8) . . ?
C5 C3 C2 120.0(8) . . ?
C5 C3 C6 120.2(8) . 2_666 ?
C6 C3 C2 119.8(8) 2_666 . ?
O2 C4 C1 118.7(10) . . ?
O2 C4 O4 124.9(9) . . ?
O4 C4 C1 116.4(8) . . ?
C3 C5 H5 119.6 . . ?
C3 C5 C6 120.9(8) . . ?
C6 C5 H5 119.6 . . ?
C5 C6 C3 118.9(8) . 2_666 ?
O12 C6 C3 123.0(8) . 2_666 ?
O12 C6 C5 118.1(8) . . ?
O7 C7 C11 118.8(8) . . ?
O7 C7 O8 121.3(8) . . ?
O8 C7 C11 120.0(8) . . ?
C1 C8 H8 119.0 . . ?
C9 C8 C1 122.0(8) . . ?
C9 C8 H8 119.0 . . ?
C8 C9 C1 119.2(10) . 2_556 ?
O9 C9 C1 123.6(10) . 2_556 ?
O9 C9 C8 117.2(8) . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N1 C10 H10A 109.5 . . ?
N1 C10 H10B 109.5 . . ?
N1 C10 H10C 109.5 . . ?
C12 C11 C7 120.9(8) . . ?
C12 C11 C14 120.8(8) . . ?
C14 C11 C7 118.2(8) . . ?
C11 C12 H12 119.3 . . ?
C11 C12 C14 121.3(9) . 2_677 ?
C14 C12 H12 119.3 2_677 . ?
N2 C13 H13 117.8 . . ?
O11 C13 H13 117.8 . . ?
O11 C13 N2 124.4(12) . . ?
C12 C14 C11 117.8(8) 2_677 . ?
O1 C14 C11 123.3(8) . . ?
O1 C14 C12 118.8(8) . 2_677 ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N1 C15 H15A 109.5 . . ?
N1 C15 H15B 109.5 . . ?
N1 C15 H15C 109.5 . . ?
N1 C16 H16 117.3 . . ?
O5 C16 H16 117.3 . . ?
O5 C16 N1 125.3(12) . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N2 C17 H17A 109.5 . . ?
N2 C17 H17B 109.5 . . ?
N2 C17 H17C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N2 C18 H18A 109.5 . . ?
N2 C18 H18B 109.5 . . ?
N2 C18 H18C 109.5 . . ?
C10 N1 C15 117.7(11) . . ?
C16 N1 C10 122.2(11) . . ?
C16 N1 C15 120.0(13) . . ?
C13 N2 C17 116.9(14) . . ?
C13 N2 C18 120.0(13) . . ?
C18 N2 C17 123.1(16) . . ?
C14 O1 H1 109.5 . . ?
C4 O2 Tb1 133.1(7) . . ?
C2 O3 Tb1 170.7(7) . . ?
C4 O4 Tb1 141.8(6) . 2_566 ?
C16 O5 Tb1 139.0(7) . . ?
C2 O6 Tb1 107.2(5) . 2_566 ?
C7 O7 Tb1 90.8(5) . . ?
C7 O8 Tb1 94.1(5) . . ?
C9 O9 H9 109.5 . . ?
C13 O11 Tb1 135.5(8) . . ?
C6 O12 H12A 109.5 . . ?
O2 Tb1 O4 128.9(2) . 2_566 ?
O2 Tb1 O6 81.9(2) . 2_566 ?
O2 Tb1 O7 153.5(3) . . ?
O2 Tb1 O8 142.9(2) . . ?
O2 Tb1 O11 74.5(3) . . ?
O3 Tb1 O2 78.1(2) . . ?
O3 Tb1 O4 75.4(2) . 2_566 ?
O3 Tb1 O6 123.1(2) . 2_566 ?
O3 Tb1 O7 128.3(2) . . ?
O3 Tb1 O8 83.1(2) . . ?
O3 Tb1 O11 79.0(3) . . ?
O4 Tb1 O6 77.3(3) 2_566 2_566 ?
O4 Tb1 O7 68.3(2) 2_566 . ?
O4 Tb1 O8 75.1(3) 2_566 . ?
O4 Tb1 O11 139.2(3) 2_566 . ?
O5 Tb1 O2 79.9(3) . . ?
O5 Tb1 O3 147.7(3) . . ?
O5 Tb1 O4 136.8(3) . 2_566 ?
O5 Tb1 O6 76.3(3) . 2_566 ?
O5 Tb1 O7 75.2(3) . . ?
O5 Tb1 O8 101.0(3) . . ?
O5 Tb1 O11 72.4(3) . . ?
O6 Tb1 O7 83.5(2) 2_566 . ?
O6 Tb1 O8 134.8(2) 2_566 . ?
O6 Tb1 O11 143.4(3) 2_566 . ?
O8 Tb1 O7 53.2(2) . . ?
O11 Tb1 O7 105.9(3) . . ?
O11 Tb1 O8 70.7(3) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O1 H1 O8 0.84 1.88 2.602(10) 144.0 . yes
O9 H9 O4 0.84 1.92 2.641(10) 143.5 2_556 yes
O12 H12A O6 0.84 1.85 2.589(10) 146.4 2_666 yes

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
C1 C4 O2 Tb1 139.8(7) . . . . ?
C1 C4 O4 Tb1 -174.8(6) . . . 2_566 ?
C1 C8 C9 C1 -0.3(16) . . . 2_556 ?
C1 C8 C9 O9 -179.5(9) . . . . ?
C2 C3 C5 C6 177.5(11) . . . . ?
C3 C2 O6 Tb1 -176.6(7) . . . 2_566 ?
C3 C5 C6 C3 1(2) . . . 2_666 ?
C3 C5 C6 O12 -178.8(12) . . . . ?
C4 C1 C8 C9 -177.1(9) . . . . ?
C6 C3 C5 C6 -1(2) 2_666 . . . ?
C7 C11 C12 C14 -179.4(12) . . . 2_677 ?
C7 C11 C14 C12 179.5(12) . . . 2_677 ?
C7 C11 C14 O1 -2(2) . . . . ?
C8 C1 C4 O2 8.6(12) . . . . ?
C8 C1 C4 O4 -173.3(8) . . . . ?
C9 C1 C4 O2 -168.8(8) 2_556 . . . ?
C9 C1 C4 O4 9.4(12) 2_556 . . . ?
C9 C1 C8 C9 0.3(15) 2_556 . . . ?
C11 C7 O7 Tb1 173.2(9) . . . . ?
C11 C7 O8 Tb1 -172.9(9) . . . . ?
C12 C11 C14 C12 -3(2) . . . 2_677 ?
C12 C11 C14 O1 175.3(14) . . . . ?
C14 C11 C12 C14 3(2) . . . 2_677 ?
N1 C16 O5 Tb1 -100.6(15) . . . . ?
N2 C13 O11 Tb1 172.7(10) . . . . ?
O2 C4 O4 Tb1 3.2(15) . . . 2_566 ?
O3 C2 C3 C5 -5.5(16) . . . . ?
O3 C2 C3 C6 172.9(11) . . . 2_666 ?
O3 C2 O6 Tb1 1.9(12) . . . 2_566 ?
O4 C4 O2 Tb1 -38.2(13) . . . . ?
O5 C16 N1 C10 -179.9(11) . . . . ?
O5 C16 N1 C15 -2.0(18) . . . . ?
O6 C2 C3 C5 173.1(11) . . . . ?
O6 C2 C3 C6 -8.6(16) . . . 2_666 ?
O7 C7 C11 C12 -8.0(18) . . . . ?
O7 C7 C11 C14 169.2(11) . . . . ?
O7 C7 O8 Tb1 8.3(11) . . . . ?
O8 C7 C11 C12 173.2(13) . . . . ?
O8 C7 C11 C14 -9.6(17) . . . . ?
O8 C7 O7 Tb1 -8.1(11) . . . . ?
O11 C13 N2 C17 179.2(11) . . . . ?
O11 C13 N2 C18 -0.9(18) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.500 0.000 0.500 210.5 0.0 ?


_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 1.282
_oxdiff_exptl_absorpt_empirical_full_min 0.833

# start Validation Reply Form
_vrf_PLAT027_SION2_120K_cool     
;
PROBLEM: _diffrn_reflns_theta_full value (too) Low ......      26.00 Degree
RESPONSE: Our value of max sin(theta)/lambda of 0.56 is close to the recommended 
		  value of 0.60. Higer values of sin(theta)/lambda were not available due 
		  to the beamline experimental set-up limitations. 
;
_vrf_PLAT029_SION2_120K_cool     
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.713 Why?  
RESPONSE: The data were collected upon the spindle rotation. Therefore, a 
		  limited portion of the reciprocal space could be probed.
;
# 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_SION2_340K
_database_code_depnum_ccdc_archive 'CCDC 1871315'
loop_
_audit_author_name
_audit_author_address
'Andrzej Gladysiak'
;Ecole polytechnique f?d?rale de Lausanne
Switzerland
;
_audit_update_record             
;
2018-10-03 deposited with the CCDC.	2019-08-12 downloaded from the CCDC.
;
_audit_creation_date             2018-07-09
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_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          ?
_chemical_oxdiff_formula         'C21 H27 N3 O12 Tb'
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                   10.5964(10)
_cell_length_b                   11.0355(7)
_cell_length_c                   12.9523(13)
_cell_angle_alpha                102.131(7)
_cell_angle_beta                 112.002(9)
_cell_angle_gamma                97.133(6)
_cell_volume                     1338.1(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4239
_cell_measurement_temperature    340.0
_cell_measurement_theta_max      31.7740
_cell_measurement_theta_min      2.2370
_shelx_estimated_absorpt_T_max   0.833
_shelx_estimated_absorpt_T_min   0.614
_exptl_absorpt_coefficient_mu    2.706
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78654
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.669
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             670
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0261
_diffrn_reflns_av_unetI/netI     0.0406
_diffrn_reflns_Laue_measured_fraction_full 0.735
_diffrn_reflns_Laue_measured_fraction_max 0.673
_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       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8638
_diffrn_reflns_point_group_measured_fraction_full 0.735
_diffrn_reflns_point_group_measured_fraction_max 0.673
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.430
_diffrn_reflns_theta_min         1.946
_diffrn_ambient_temperature      340.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            PILATUS2M
_diffrn_measured_fraction_theta_full 0.735
_diffrn_measured_fraction_theta_max 0.673
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      0.00 360.00   1.00    1.00    --    0.00   0.00   0.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  PILATUS@SNBL
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0639016000
_diffrn_orient_matrix_UB_12      -0.0154918000
_diffrn_orient_matrix_UB_13      0.0324493000
_diffrn_orient_matrix_UB_21      -0.0306692000
_diffrn_orient_matrix_UB_22      -0.0659894000
_diffrn_orient_matrix_UB_23      -0.0283101000
_diffrn_orient_matrix_UB_31      0.0232227000
_diffrn_orient_matrix_UB_32      0.0043114000
_diffrn_orient_matrix_UB_33      -0.0445092000
_diffrn_radiation_monochromator  'Si (111)'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           ?
_diffrn_radiation_wavelength     0.7142
_diffrn_source                   
'European Synchrotron Radiation Facility, BM01 beamline'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4032
_reflns_number_total             4465
_reflns_odcompleteness_completeness 72.42
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.51
_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 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (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    'XT (Sheldrick, 2015)'
_refine_diff_density_max         1.864
_refine_diff_density_min         -1.688
_refine_diff_density_rms         0.109
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         4465
_refine_ls_number_restraints     141
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0416
_refine_ls_restrained_S_all      1.069
_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)+(0.0840P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1110
_refine_ls_wR_factor_ref         0.1132
_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
 C18A-N2 \\sim N2-C18B
 with sigma of 0.01
 C17B-N2 \\sim N2-C17A
 with sigma of 0.01
 C13B-N2 \\sim N2-C13A
 with sigma of 0.01
 C13B-O11B \\sim O11A-C13A
 with sigma of 0.01
 C18B-C17B \\sim C17A-C18A
 with sigma of 0.01
3. Restrained planarity
 C13B, C17B, C18B, N2, O11B
 with sigma of 0.1
 C13A, C17A, C18A, N2, O11A
 with sigma of 0.1
4. Rigid bond restraints
 C2, O3
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.005
 O3, C2, O6
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Uiso/Uaniso restraints and constraints
C2 \\sim O3: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.01
C2 \\sim O6: within 2A with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(O1B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C15) \\sim Ueq, Uanis(C16) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(O9) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C1A) = Uanis(C1B)
Uanis(C3A) = Uanis(C3B)
Uanis(C2A) = Uanis(C2B)
Uanis(O1A) = Uanis(O1B)
Uanis(O11B) = Uanis(O11A)
Uanis(C13A) = Uanis(C13B)
Uanis(C18B) = Uanis(C18A)
Uanis(C17B) = Uanis(C17A)
6. Rigid body (RIGU) restrains
 C1A, C2A, C3A, N3, O10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1B, C2B, C3B, N3, O10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C13A, C17A, C18A, N2, O11A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C13B, C17B, C18B, N2, O11B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. 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(H12)=Sof(O1B)=Sof(H1B)=1-FVAR(2)
 Sof(H14)=Sof(O1A)=Sof(H1A)=FVAR(2)
 Sof(C13B)=Sof(H13B)=Sof(C17B)=Sof(H17D)=Sof(H17E)=Sof(H17F)=Sof(C18B)=
 Sof(H18D)=Sof(H18E)=Sof(H18F)=Sof(O11B)=1-FVAR(3)
 Sof(C13A)=Sof(H13A)=Sof(C17A)=Sof(H17A)=Sof(H17B)=Sof(H17C)=Sof(C18A)=
 Sof(H18A)=Sof(H18B)=Sof(H18C)=Sof(O11A)=FVAR(3)
8.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C8(H8), C10(H10), C12(H12), C13A(H13A), C13B(H13B), C14(H14),
 C1A(H1AA), C1B(H1BA)
8.b Tetrahedral OH refined with riding coordinates:
 O1B(H1B)
8.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17A(H17A,H17B,H17C), C17B(H17D,
 H17E,H17F), C18A(H18A,H18B,H18C), C18B(H18D,H18E,H18F), C2A(H2AA,H2AB,H2AC),
 C2B(H2BA,H2BB,H2BC), C3A(H3AA,H3AB,H3AC), C3B(H3BA,H3BB,H3BC)
8.d Idealised tetrahedral OH refined as rotating group:
 O1A(H1A), O9(H9), O12(H12A)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
C1 C -0.0205(6) 0.1214(5) 0.4926(5) 0.0536(14) Uani 1 1 d . . . . .
C2 C 0.2066(6) 0.4754(5) 0.4463(6) 0.0559(8) Uani 1 1 d . U . . .
C3 C 0.3578(5) 0.4875(5) 0.4717(5) 0.0524(14) Uani 1 1 d . . . . .
C4 C -0.0350(5) 0.2547(4) 0.4930(5) 0.0504(13) Uani 1 1 d . . . . .
C5 C 0.4553(6) 0.5351(6) 0.5872(5) 0.0603(15) Uani 1 1 d . . . . .
H5 H 0.4252 0.5582 0.6458 0.072 Uiso 1 1 calc R . . . .
C6 C 0.5961(6) 0.5477(6) 0.6141(6) 0.0600(16) Uani 1 1 d . . . . .
C7 C 0.3000(6) 0.7687(5) 0.8442(5) 0.0578(15) Uani 1 1 d . . . . .
C8 C 0.0057(8) 0.0869(5) 0.5955(5) 0.0630(16) Uani 1 1 d . . . . .
H8 H 0.0094 0.1458 0.6601 0.076 Uiso 1 1 calc R . . . .
C9 C 0.0264(8) -0.0327(5) 0.6032(5) 0.0613(16) Uani 1 1 d . . . . .
C10 C -0.0102(11) 0.3809(8) 0.8244(8) 0.091(2) Uani 1 1 d . . . . .
H10 H -0.0979 0.3651 0.7638 0.109 Uiso 1 1 calc R . . . .
C11 C 0.4021(6) 0.8890(5) 0.9255(5) 0.0532(13) Uani 1 1 d . . . . .
C12 C 0.3635(6) 0.9811(6) 0.9938(5) 0.0602(15) Uani 1 1 d . . . . .
H12 H 0.2732 0.9681 0.9898 0.072 Uiso 0.156(9) 1 calc R . P A 2
C13A C 0.3955(14) 0.4263(12) 0.7997(13) 0.087(3) Uani 0.574(12) 1 d D U P B 1
H13A H 0.4571 0.5049 0.8249 0.105 Uiso 0.574(12) 1 calc R . P B 1
C13B C 0.3139(15) 0.3389(18) 0.7527(16) 0.087(3) Uani 0.426(12) 1 d D U P B 2
H13B H 0.2409 0.2691 0.7055 0.105 Uiso 0.426(12) 1 calc R . P B 2
C14 C 0.5387(6) 0.9086(6) 0.9329(6) 0.0616(16) Uani 1 1 d . . . . .
H14 H 0.5640 0.8471 0.8882 0.074 Uiso 0.844(9) 1 calc R . P A 1
C15 C -0.1021(17) 0.2020(17) 0.8739(16) 0.166(6) Uani 1 1 d . U . . .
H15A H -0.0901 0.1889 0.9477 0.250 Uiso 1 1 calc GR . . . .
H15B H -0.0966 0.1263 0.8248 0.250 Uiso 1 1 calc GR . . . .
H15C H -0.1917 0.2211 0.8383 0.250 Uiso 1 1 calc GR . . . .
C16 C 0.134(2) 0.3216(19) 0.9821(17) 0.197(8) Uani 1 1 d . U . . .
H16A H 0.1444 0.3908 1.0460 0.295 Uiso 1 1 calc GR . . . .
H16B H 0.2080 0.3396 0.9584 0.295 Uiso 1 1 calc GR . . . .
H16C H 0.1367 0.2447 1.0056 0.295 Uiso 1 1 calc GR . . . .
C17A C 0.362(2) 0.1960(19) 0.793(2) 0.171(8) Uani 0.574(12) 1 d D U P B 1
H17A H 0.3486 0.1801 0.8585 0.256 Uiso 0.574(12) 1 calc GR . P B 1
H17B H 0.4104 0.1365 0.7678 0.256 Uiso 0.574(12) 1 calc GR . P B 1
H17C H 0.2726 0.1866 0.7308 0.256 Uiso 0.574(12) 1 calc GR . P B 1
C17B C 0.430(3) 0.1867(19) 0.803(3) 0.171(8) Uani 0.426(12) 1 d D U P B 2
H17D H 0.3498 0.1482 0.8114 0.256 Uiso 0.426(12) 1 calc GR . P B 2
H17E H 0.5127 0.1707 0.8573 0.256 Uiso 0.426(12) 1 calc GR . P B 2
H17F H 0.4212 0.1512 0.7254 0.256 Uiso 0.426(12) 1 calc GR . P B 2
C18A C 0.5940(18) 0.337(2) 0.893(2) 0.148(7) Uani 0.574(12) 1 d D U P B 1
H18A H 0.6344 0.4250 0.9357 0.222 Uiso 0.574(12) 1 calc GR . P B 1
H18B H 0.6378 0.3109 0.8422 0.222 Uiso 0.574(12) 1 calc GR . P B 1
H18C H 0.6081 0.2862 0.9467 0.222 Uiso 0.574(12) 1 calc GR . P B 1
C18B C 0.585(2) 0.397(3) 0.901(3) 0.148(7) Uani 0.426(12) 1 d D U P B 2
H18D H 0.6300 0.4221 0.8539 0.222 Uiso 0.426(12) 1 calc GR . P B 2
H18E H 0.6377 0.3463 0.9450 0.222 Uiso 0.426(12) 1 calc GR . P B 2
H18F H 0.5810 0.4711 0.9522 0.222 Uiso 0.426(12) 1 calc GR . P B 2
N1 N 0.0067(11) 0.3071(8) 0.8904(8) 0.108(3) Uani 1 1 d . . . . .
N2 N 0.4406(9) 0.3205(9) 0.8239(8) 0.119(3) Uani 1 1 d D U . . .
O1A O 0.2341(6) 0.9707(7) 0.9916(6) 0.083(2) Uani 0.844(9) 1 d . . P A 1
H1A H 0.1876 0.8986 0.9544 0.125 Uiso 0.844(9) 1 calc GR . P A 1
O1B O 0.597(3) 0.825(3) 0.887(3) 0.083(2) Uani 0.156(9) 1 d . U P A 2
H1B H 0.5377 0.7597 0.8452 0.125 Uiso 0.156(9) 1 calc R . P A 2
O2 O -0.0095(4) 0.3331(3) 0.5869(4) 0.0542(9) Uani 1 1 d . . . . .
O3 O 0.1663(4) 0.4991(4) 0.5263(4) 0.0568(7) Uani 1 1 d . U . . .
O4 O -0.0714(4) 0.2786(3) 0.3958(3) 0.0577(10) Uani 1 1 d . . . . .
O5 O 0.0787(6) 0.4711(4) 0.8333(4) 0.0765(14) Uani 1 1 d . . . . .
O6 O 0.1202(4) 0.4400(4) 0.3396(4) 0.0596(8) Uani 1 1 d . U . . .
O7 O 0.1795(4) 0.7455(4) 0.8454(4) 0.0625(11) Uani 1 1 d . . . . .
O8 O 0.3342(5) 0.6915(4) 0.7820(4) 0.0722(13) Uani 1 1 d . . . . .
O9 O 0.0515(9) -0.0568(5) 0.7070(5) 0.098(2) Uani 1 1 d . U . . .
H9 H 0.0809 -0.1221 0.7080 0.147 Uiso 1 1 calc GR . . . .
O11A O 0.2741(17) 0.4130(17) 0.7450(18) 0.087(3) Uani 0.574(12) 1 d D U P B 1
O11B O 0.298(3) 0.443(2) 0.752(3) 0.087(3) Uani 0.426(12) 1 d D U P B 2
O12 O 0.6847(5) 0.5952(7) 0.7288(5) 0.0884(18) Uani 1 1 d . . . . .
H12A H 0.7653 0.6126 0.7352 0.133 Uiso 1 1 calc GR . . . .
Tb1 Tb 0.10940(2) 0.54518(2) 0.68192(2) 0.04345(13) Uani 1 1 d . . . . .
C1A C 0.616(6) 0.189(4) 0.542(4) 0.194(9) Uani 0.532(15) 1 d . U P C 1
H1AA H 0.6966 0.1866 0.5304 0.233 Uiso 0.532(15) 1 calc R . P C 1
C1B C 0.480(7) 0.188(5) 0.553(5) 0.194(9) Uani 0.468(15) 1 d . U P C 2
H1BA H 0.3998 0.1904 0.5662 0.233 Uiso 0.468(15) 1 calc R . P C 2
C2A C 0.452(5) 0.112(4) 0.329(4) 0.190(9) Uani 0.532(15) 1 d . U P C 1
H2AA H 0.5233 0.1603 0.3150 0.285 Uiso 0.532(15) 1 calc GR . P C 1
H2AB H 0.3627 0.1269 0.2835 0.285 Uiso 0.532(15) 1 calc GR . P C 1
H2AC H 0.4507 0.0236 0.3065 0.285 Uiso 0.532(15) 1 calc GR . P C 1
C2B C 0.605(5) 0.147(4) 0.422(4) 0.190(9) Uani 0.468(15) 1 d . U P C 2
H2BA H 0.6889 0.1921 0.4889 0.285 Uiso 0.468(15) 1 calc GR . P C 2
H2BB H 0.5953 0.1860 0.3604 0.285 Uiso 0.468(15) 1 calc GR . P C 2
H2BC H 0.6090 0.0601 0.3975 0.285 Uiso 0.468(15) 1 calc GR . P C 2
C3A C 0.345(5) 0.151(4) 0.474(4) 0.196(10) Uani 0.532(15) 1 d . U P C 1
H3AA H 0.2648 0.1088 0.4028 0.294 Uiso 0.532(15) 1 calc GR . P C 1
H3AB H 0.3378 0.2364 0.5020 0.294 Uiso 0.532(15) 1 calc GR . P C 1
H3AC H 0.3485 0.1059 0.5306 0.294 Uiso 0.532(15) 1 calc GR . P C 1
C3B C 0.341(6) 0.116(4) 0.351(4) 0.196(10) Uani 0.468(15) 1 d . U P C 2
H3BA H 0.2706 0.1367 0.3769 0.294 Uiso 0.468(15) 1 calc GR . P C 2
H3BB H 0.3192 0.0256 0.3153 0.294 Uiso 0.468(15) 1 calc GR . P C 2
H3BC H 0.3433 0.1602 0.2952 0.294 Uiso 0.468(15) 1 calc GR . P C 2
N3 N 0.4807(19) 0.1533(11) 0.4522(14) 0.158(4) Uani 1 1 d . U . . .
O10 O 0.6149(18) 0.2225(15) 0.6385(13) 0.213(6) Uani 1 1 d . U . . .


_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
C1 C4 1.497(6) . ?
C1 C8 1.400(8) . ?
C1 C9 1.385(9) 2_556 ?
C2 C3 1.492(8) . ?
C2 O3 1.253(8) . ?
C2 O6 1.280(7) . ?
C3 C5 1.399(8) . ?
C3 C6 1.377(10) 2_666 ?
C4 O2 1.247(7) . ?
C4 O4 1.268(7) . ?
C5 H5 0.9300 . ?
C5 C6 1.380(9) . ?
C6 C3 1.377(10) 2_666 ?
C6 O12 1.367(8) . ?
C7 C11 1.497(7) . ?
C7 O7 1.277(8) . ?
C7 O8 1.230(8) . ?
C8 H8 0.9300 . ?
C8 C9 1.383(7) . ?
C9 C1 1.385(9) 2_556 ?
C9 O9 1.359(8) . ?
C10 H10 0.9300 . ?
C10 N1 1.281(11) . ?
C10 O5 1.237(10) . ?
C11 C12 1.407(9) . ?
C11 C14 1.400(9) . ?
C12 H12 0.9300 . ?
C12 C14 1.386(8) 2_677 ?
C12 O1A 1.350(9) . ?
C13A H13A 0.9300 . ?
C13A N2 1.368(11) . ?
C13A O11A 1.185(17) . ?
C13B H13B 0.9300 . ?
C13B N2 1.383(12) . ?
C13B O11B 1.187(18) . ?
C14 C12 1.386(8) 2_677 ?
C14 H14 0.9300 . ?
C14 O1B 1.34(4) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C15 N1 1.448(16) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C16 N1 1.384(18) . ?
C17A H17A 0.9600 . ?
C17A H17B 0.9600 . ?
C17A H17C 0.9600 . ?
C17A N2 1.406(19) . ?
C17B H17D 0.9600 . ?
C17B H17E 0.9600 . ?
C17B H17F 0.9600 . ?
C17B N2 1.426(19) . ?
C18A H18A 0.9600 . ?
C18A H18B 0.9600 . ?
C18A H18C 0.9600 . ?
C18A N2 1.498(17) . ?
C18B H18D 0.9600 . ?
C18B H18E 0.9600 . ?
C18B H18F 0.9600 . ?
C18B N2 1.494(18) . ?
O1A H1A 0.8200 . ?
O1B H1B 0.8200 . ?
O2 Tb1 2.339(3) . ?
O3 Tb1 2.289(5) . ?
O4 Tb1 2.381(3) 2_566 ?
O5 Tb1 2.389(5) . ?
O6 Tb1 2.374(4) 2_566 ?
O7 Tb1 2.524(4) . ?
O8 Tb1 2.411(4) . ?
O9 H9 0.8200 . ?
O11A Tb1 2.430(14) . ?
O11B Tb1 2.387(19) . ?
O12 H12A 0.8200 . ?
Tb1 O4 2.381(3) 2_566 ?
Tb1 O6 2.374(4) 2_566 ?
C1A H1AA 0.9300 . ?
C1A N3 1.41(5) . ?
C1A O10 1.22(5) . ?
C1B H1BA 0.9300 . ?
C1B N3 1.28(5) . ?
C1B O10 1.39(6) . ?
C2A H2AA 0.9600 . ?
C2A H2AB 0.9600 . ?
C2A H2AC 0.9600 . ?
C2A N3 1.47(4) . ?
C2B H2BA 0.9600 . ?
C2B H2BB 0.9600 . ?
C2B H2BC 0.9600 . ?
C2B N3 1.51(5) . ?
C3A H3AA 0.9600 . ?
C3A H3AB 0.9600 . ?
C3A H3AC 0.9600 . ?
C3A N3 1.57(4) . ?
C3B H3BA 0.9600 . ?
C3B H3BB 0.9600 . ?
C3B H3BC 0.9600 . ?
C3B N3 1.50(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C8 C1 C4 118.2(5) . . ?
C9 C1 C4 123.0(5) 2_556 . ?
C9 C1 C8 118.8(5) 2_556 . ?
O3 C2 C3 121.3(5) . . ?
O3 C2 O6 121.5(5) . . ?
O6 C2 C3 117.2(6) . . ?
C5 C3 C2 118.4(6) . . ?
C6 C3 C2 122.3(5) 2_666 . ?
C6 C3 C5 119.3(5) 2_666 . ?
O2 C4 C1 118.8(5) . . ?
O2 C4 O4 125.1(5) . . ?
O4 C4 C1 116.1(5) . . ?
C3 C5 H5 119.9 . . ?
C6 C5 C3 120.1(6) . . ?
C6 C5 H5 119.9 . . ?
C3 C6 C5 120.6(6) 2_666 . ?
O12 C6 C3 122.8(5) . 2_666 ?
O12 C6 C5 116.6(6) . . ?
O7 C7 C11 118.4(6) . . ?
O8 C7 C11 120.5(6) . . ?
O8 C7 O7 121.0(5) . . ?
C1 C8 H8 119.3 . . ?
C9 C8 C1 121.5(6) . . ?
C9 C8 H8 119.3 . . ?
C8 C9 C1 119.8(6) . 2_556 ?
O9 C9 C1 123.3(5) . 2_556 ?
O9 C9 C8 117.0(5) . . ?
N1 C10 H10 116.8 . . ?
O5 C10 H10 116.8 . . ?
O5 C10 N1 126.3(9) . . ?
C12 C11 C7 121.5(6) . . ?
C14 C11 C7 118.6(6) . . ?
C14 C11 C12 120.0(5) . . ?
C11 C12 H12 120.3 . . ?
C14 C12 C11 119.4(6) 2_677 . ?
C14 C12 H12 120.3 2_677 . ?
O1A C12 C11 124.0(5) . . ?
O1A C12 C14 116.5(6) . 2_677 ?
N2 C13A H13A 121.6 . . ?
O11A C13A H13A 121.6 . . ?
O11A C13A N2 116.7(15) . . ?
N2 C13B H13B 119.8 . . ?
O11B C13B H13B 119.8 . . ?
O11B C13B N2 120(2) . . ?
C11 C14 H14 119.7 . . ?
C12 C14 C11 120.6(6) 2_677 . ?
C12 C14 H14 119.7 2_677 . ?
O1B C14 C11 127.4(14) . . ?
O1B C14 C12 111.5(14) . 2_677 ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N1 C15 H15A 109.5 . . ?
N1 C15 H15B 109.5 . . ?
N1 C15 H15C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N1 C16 H16A 109.5 . . ?
N1 C16 H16B 109.5 . . ?
N1 C16 H16C 109.5 . . ?
H17A C17A H17B 109.5 . . ?
H17A C17A H17C 109.5 . . ?
H17B C17A H17C 109.5 . . ?
N2 C17A H17A 109.5 . . ?
N2 C17A H17B 109.5 . . ?
N2 C17A H17C 109.5 . . ?
H17D C17B H17E 109.5 . . ?
H17D C17B H17F 109.5 . . ?
H17E C17B H17F 109.5 . . ?
N2 C17B H17D 109.5 . . ?
N2 C17B H17E 109.5 . . ?
N2 C17B H17F 109.5 . . ?
H18A C18A H18B 109.5 . . ?
H18A C18A H18C 109.5 . . ?
H18B C18A H18C 109.5 . . ?
N2 C18A H18A 109.5 . . ?
N2 C18A H18B 109.5 . . ?
N2 C18A H18C 109.5 . . ?
H18D C18B H18E 109.5 . . ?
H18D C18B H18F 109.5 . . ?
H18E C18B H18F 109.5 . . ?
N2 C18B H18D 109.5 . . ?
N2 C18B H18E 109.5 . . ?
N2 C18B H18F 109.5 . . ?
C10 N1 C15 123.4(11) . . ?
C10 N1 C16 121.3(11) . . ?
C16 N1 C15 115.3(11) . . ?
C13A N2 C17A 128.6(13) . . ?
C13A N2 C18A 116.9(13) . . ?
C13B N2 C17B 107.5(16) . . ?
C13B N2 C18B 138.6(15) . . ?
C17A N2 C18A 114.5(13) . . ?
C17B N2 C18B 113.2(14) . . ?
C12 O1A H1A 109.5 . . ?
C14 O1B H1B 109.5 . . ?
C4 O2 Tb1 136.9(4) . . ?
C2 O3 Tb1 175.8(4) . . ?
C4 O4 Tb1 139.0(3) . 2_566 ?
C10 O5 Tb1 128.2(5) . . ?
C2 O6 Tb1 111.6(4) . 2_566 ?
C7 O7 Tb1 89.9(4) . . ?
C7 O8 Tb1 96.4(4) . . ?
C9 O9 H9 109.5 . . ?
C13A O11A Tb1 138.1(14) . . ?
C13B O11B Tb1 138(2) . . ?
C6 O12 H12A 109.5 . . ?
O2 Tb1 O4 125.95(14) . 2_566 ?
O2 Tb1 O5 77.42(16) . . ?
O2 Tb1 O6 79.68(15) . 2_566 ?
O2 Tb1 O7 151.70(16) . . ?
O2 Tb1 O8 145.79(16) . . ?
O2 Tb1 O11A 72.6(5) . . ?
O2 Tb1 O11B 80.6(7) . . ?
O3 Tb1 O2 76.95(15) . . ?
O3 Tb1 O4 76.56(15) . 2_566 ?
O3 Tb1 O5 145.71(17) . . ?
O3 Tb1 O6 122.12(15) . 2_566 ?
O3 Tb1 O7 131.34(14) . . ?
O3 Tb1 O8 86.25(16) . . ?
O3 Tb1 O11A 80.0(5) . . ?
O3 Tb1 O11B 78.5(7) . . ?
O4 Tb1 O5 137.55(17) 2_566 . ?
O4 Tb1 O7 70.54(14) 2_566 . ?
O4 Tb1 O8 77.03(16) 2_566 . ?
O4 Tb1 O11A 144.6(5) 2_566 . ?
O4 Tb1 O11B 137.0(7) 2_566 . ?
O5 Tb1 O7 76.26(16) . . ?
O5 Tb1 O8 102.86(18) . . ?
O5 Tb1 O11A 70.8(5) . . ?
O6 Tb1 O4 76.04(15) 2_566 2_566 ?
O6 Tb1 O5 74.58(18) 2_566 . ?
O6 Tb1 O7 83.47(15) 2_566 . ?
O6 Tb1 O8 133.95(15) 2_566 . ?
O6 Tb1 O11A 139.3(5) 2_566 . ?
O6 Tb1 O11B 146.7(7) 2_566 . ?
O8 Tb1 O7 52.43(16) . . ?
O8 Tb1 O11A 75.3(5) . . ?
O11A Tb1 O7 107.9(5) . . ?
O11B Tb1 O5 75.1(7) . . ?
O11B Tb1 O7 102.4(7) . . ?
O11B Tb1 O8 66.8(7) . . ?
N3 C1A H1AA 123.6 . . ?
O10 C1A H1AA 123.6 . . ?
O10 C1A N3 113(4) . . ?
N3 C1B H1BA 124.7 . . ?
N3 C1B O10 111(5) . . ?
O10 C1B H1BA 124.7 . . ?
H2AA C2A H2AB 109.5 . . ?
H2AA C2A H2AC 109.5 . . ?
H2AB C2A H2AC 109.5 . . ?
N3 C2A H2AA 109.5 . . ?
N3 C2A H2AB 109.5 . . ?
N3 C2A H2AC 109.5 . . ?
H2BA C2B H2BB 109.5 . . ?
H2BA C2B H2BC 109.5 . . ?
H2BB C2B H2BC 109.5 . . ?
N3 C2B H2BA 109.5 . . ?
N3 C2B H2BB 109.5 . . ?
N3 C2B H2BC 109.5 . . ?
H3AA C3A H3AB 109.5 . . ?
H3AA C3A H3AC 109.5 . . ?
H3AB C3A H3AC 109.5 . . ?
N3 C3A H3AA 109.5 . . ?
N3 C3A H3AB 109.5 . . ?
N3 C3A H3AC 109.5 . . ?
H3BA C3B H3BB 109.5 . . ?
H3BA C3B H3BC 109.5 . . ?
H3BB C3B H3BC 109.5 . . ?
N3 C3B H3BA 109.5 . . ?
N3 C3B H3BB 109.5 . . ?
N3 C3B H3BC 109.5 . . ?
C1A N3 C2A 124(3) . . ?
C1A N3 C3A 123(3) . . ?
C1B N3 C2B 128(4) . . ?
C1B N3 C3B 116(4) . . ?
C2A N3 C3A 113(3) . . ?
C3B N3 C2B 115(3) . . ?

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
C1 C4 O2 Tb1 136.6(5) . . . . ?
C1 C4 O4 Tb1 -176.9(4) . . . 2_566 ?
C1 C8 C9 C1 -0.3(12) . . . 2_556 ?
C1 C8 C9 O9 179.8(7) . . . . ?
C2 C3 C5 C6 -179.9(6) . . . . ?
C3 C2 O6 Tb1 -172.0(4) . . . 2_566 ?
C3 C5 C6 C3 -0.8(11) . . . 2_666 ?
C3 C5 C6 O12 179.8(7) . . . . ?
C4 C1 C8 C9 -177.2(6) . . . . ?
C6 C3 C5 C6 0.8(11) 2_666 . . . ?
C7 C11 C12 C14 -179.5(6) . . . 2_677 ?
C7 C11 C12 O1A -0.8(11) . . . . ?
C7 C11 C14 C12 179.5(6) . . . 2_677 ?
C7 C11 C14 O1B -10(3) . . . . ?
C8 C1 C4 O2 7.2(8) . . . . ?
C8 C1 C4 O4 -173.7(6) . . . . ?
C9 C1 C4 O2 -170.2(6) 2_556 . . . ?
C9 C1 C4 O4 8.9(9) 2_556 . . . ?
C9 C1 C8 C9 0.3(12) 2_556 . . . ?
C11 C7 O7 Tb1 177.5(5) . . . . ?
C11 C7 O8 Tb1 -177.3(5) . . . . ?
C12 C11 C14 C12 -0.7(11) . . . 2_677 ?
C12 C11 C14 O1B 170(2) . . . . ?
C14 C11 C12 C14 0.6(11) . . . 2_677 ?
C14 C11 C12 O1A 179.4(7) . . . . ?
N1 C10 O5 Tb1 145.9(9) . . . . ?
N2 C13A O11A Tb1 172.8(16) . . . . ?
N2 C13B O11B Tb1 -167(2) . . . . ?
O2 C4 O4 Tb1 2.2(10) . . . 2_566 ?
O3 C2 C3 C5 -4.6(9) . . . . ?
O3 C2 C3 C6 174.7(6) . . . 2_666 ?
O3 C2 O6 Tb1 7.9(7) . . . 2_566 ?
O4 C4 O2 Tb1 -42.4(9) . . . . ?
O5 C10 N1 C15 -179.3(14) . . . . ?
O5 C10 N1 C16 -1(2) . . . . ?
O6 C2 C3 C5 175.3(6) . . . . ?
O6 C2 C3 C6 -5.4(9) . . . 2_666 ?
O7 C7 C11 C12 -6.2(9) . . . . ?
O7 C7 C11 C14 173.6(6) . . . . ?
O7 C7 O8 Tb1 6.3(7) . . . . ?
O8 C7 C11 C12 177.2(6) . . . . ?
O8 C7 C11 C14 -2.9(9) . . . . ?
O8 C7 O7 Tb1 -6.0(7) . . . . ?
O11A C13A N2 C17A -0.2(19) . . . . ?
O11A C13A N2 C18A -179.8(12) . . . . ?
O11B C13B N2 C17B -177.5(12) . . . . ?
O11B C13B N2 C18B -9(2) . . . . ?
O10 C1A N3 C2A 178(3) . . . . ?
O10 C1A N3 C3A -3(5) . . . . ?
O10 C1B N3 C2B 0(5) . . . . ?
O10 C1B N3 C3B -179(3) . . . . ?

_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 1.157
_oxdiff_exptl_absorpt_empirical_full_min 0.875

# start Validation Reply Form
_vrf_PLAT029_SION2_340K          
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.735 Why?  
RESPONSE: The data were collected upon the spindle rotation. Therefore, a 
		  limited portion of the reciprocal space could be probed.
;
# 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_SION2_300K
_database_code_depnum_ccdc_archive 'CCDC 1871313'
loop_
_audit_author_name
_audit_author_address
'Andrzej Gladysiak'
;Ecole polytechnique f?d?rale de Lausanne
Switzerland
;
_audit_update_record             
;
2018-10-03 deposited with the CCDC.	2019-08-12 downloaded from the CCDC.
;
_audit_creation_date             2018-07-09
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_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          ?
_chemical_oxdiff_formula         'C21 H27 N3 O12 Tb'
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                   10.5445(7)
_cell_length_b                   11.0141(6)
_cell_length_c                   12.7860(8)
_cell_angle_alpha                103.484(5)
_cell_angle_beta                 110.657(6)
_cell_angle_gamma                96.519(5)
_cell_volume                     1319.52(15)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5433
_cell_measurement_temperature    300.0
_cell_measurement_theta_max      31.8680
_cell_measurement_theta_min      1.9350
_shelx_estimated_absorpt_T_max   0.831
_shelx_estimated_absorpt_T_min   0.610
_exptl_absorpt_coefficient_mu    2.745
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79544
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.692
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             670
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0185
_diffrn_reflns_av_unetI/netI     0.0271
_diffrn_reflns_Laue_measured_fraction_full 0.743
_diffrn_reflns_Laue_measured_fraction_max 0.680
_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       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8650
_diffrn_reflns_point_group_measured_fraction_full 0.743
_diffrn_reflns_point_group_measured_fraction_max 0.680
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.429
_diffrn_reflns_theta_min         1.957
_diffrn_ambient_temperature      300.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            PILATUS2M
_diffrn_measured_fraction_theta_full 0.743
_diffrn_measured_fraction_theta_max 0.680
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      0.00 360.00   1.00    1.00    --    0.00   0.00   0.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  PILATUS@SNBL
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0618134000
_diffrn_orient_matrix_UB_12      -0.0147029000
_diffrn_orient_matrix_UB_13      0.0360151000
_diffrn_orient_matrix_UB_21      -0.0298104000
_diffrn_orient_matrix_UB_22      -0.0666789000
_diffrn_orient_matrix_UB_23      -0.0269725000
_diffrn_orient_matrix_UB_31      0.0280095000
_diffrn_orient_matrix_UB_32      0.0003611000
_diffrn_orient_matrix_UB_33      -0.0433120000
_diffrn_radiation_monochromator  'Si (111)'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           ?
_diffrn_radiation_wavelength     0.7142
_diffrn_source                   
'European Synchrotron Radiation Facility, BM01 beamline'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4185
_reflns_number_total             4443
_reflns_odcompleteness_completeness 73.14
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.51
_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 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (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    'XT (Sheldrick, 2015)'
_refine_diff_density_max         1.198
_refine_diff_density_min         -1.163
_refine_diff_density_rms         0.090
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         4443
_refine_ls_number_restraints     129
_refine_ls_R_factor_all          0.0303
_refine_ls_R_factor_gt           0.0285
_refine_ls_restrained_S_all      1.101
_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)+(0.0594P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0774
_refine_ls_wR_factor_ref         0.0784
_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
 C18A-N2 \\sim N2-C18B
 with sigma of 0.01
 C17B-N2 \\sim N2-C17A
 with sigma of 0.01
 C13B-N2 \\sim N2-C13A
 with sigma of 0.01
 C13B-O11B \\sim O11A-C13A
 with sigma of 0.01
 C18B-C17B \\sim C17A-C18A
 with sigma of 0.01
3. Restrained planarity
 C13B, C17B, C18B, N2, O11B
 with sigma of 0.1
 C13A, C17A, C18A, N2, O11A
 with sigma of 0.1
4. Rigid bond restraints
 O3, C2, O6
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Uiso/Uaniso restraints and constraints
C2 \\sim O6: within 2A with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(O1B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C15) \\sim Ueq, Uanis(C16) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C1A) = Uanis(C1B)
Uanis(C3A) = Uanis(C3B)
Uanis(C2A) = Uanis(C2B)
Uanis(O1A) = Uanis(O1B)
Uanis(O11B) = Uanis(O11A)
Uanis(C13A) = Uanis(C13B)
Uanis(C18B) = Uanis(C18A)
Uanis(C17B) = Uanis(C17A)
6. Rigid body (RIGU) restrains
 C1A, C2A, C3A, N3, O10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1B, C2B, C3B, N3, O10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C13A, C17A, C18A, N2, O11A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C13B, C17B, C18B, N2, O11B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. 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(H12)=Sof(O1B)=Sof(H1B)=1-FVAR(2)
 Sof(H14)=Sof(O1A)=Sof(H1A)=FVAR(2)
 Sof(C13B)=Sof(H13B)=Sof(C17B)=Sof(H17D)=Sof(H17E)=Sof(H17F)=Sof(C18B)=
 Sof(H18D)=Sof(H18E)=Sof(H18F)=Sof(O11B)=1-FVAR(3)
 Sof(C13A)=Sof(H13A)=Sof(C17A)=Sof(H17A)=Sof(H17B)=Sof(H17C)=Sof(C18A)=
 Sof(H18A)=Sof(H18B)=Sof(H18C)=Sof(O11A)=FVAR(3)
8.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C8(H8), C10(H10), C12(H12), C13A(H13A), C13B(H13B), C14(H14),
 C1A(H1AA), C1B(H1BA)
8.b Tetrahedral OH refined with riding coordinates:
 O1B(H1B)
8.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17A(H17A,H17B,H17C), C17B(H17D,
 H17E,H17F), C18A(H18A,H18B,H18C), C18B(H18D,H18E,H18F), C2A(H2AA,H2AB,H2AC),
 C2B(H2BA,H2BB,H2BC), C3A(H3AA,H3AB,H3AC), C3B(H3BA,H3BB,H3BC)
8.d Idealised tetrahedral OH refined as rotating group:
 O1A(H1A), O9(H9), O12(H12A)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
C1 C -0.0214(4) 0.1216(3) 0.4935(3) 0.0423(9) Uani 1 1 d . . . . .
C2 C 0.2060(4) 0.4704(3) 0.4430(4) 0.0420(7) Uani 1 1 d . U . . .
C3 C 0.3582(4) 0.4858(4) 0.4705(3) 0.0399(9) Uani 1 1 d . . . . .
C4 C -0.0374(4) 0.2543(3) 0.4919(3) 0.0375(8) Uani 1 1 d . . . . .
C5 C 0.4504(4) 0.5349(4) 0.5872(4) 0.0481(10) Uani 1 1 d . . . . .
H5 H 0.4169 0.5579 0.6456 0.058 Uiso 1 1 calc R . . . .
C6 C 0.5928(4) 0.5494(4) 0.6161(4) 0.0462(10) Uani 1 1 d . . . . .
C7 C 0.2957(4) 0.7704(3) 0.8464(3) 0.0428(9) Uani 1 1 d . . . . .
C8 C 0.0029(5) 0.0886(3) 0.5954(4) 0.0515(11) Uani 1 1 d . . . . .
H8 H 0.0053 0.1491 0.6608 0.062 Uiso 1 1 calc R . . . .
C9 C 0.0238(5) -0.0314(3) 0.6042(3) 0.0489(10) Uani 1 1 d . . . . .
C10 C -0.0171(6) 0.3861(5) 0.8240(5) 0.0662(13) Uani 1 1 d . . . . .
H10 H -0.1027 0.3684 0.7620 0.079 Uiso 1 1 calc R . . . .
C11 C 0.4000(4) 0.8902(3) 0.9263(3) 0.0443(9) Uani 1 1 d . . . . .
C12 C 0.3642(4) 0.9875(4) 0.9953(4) 0.0475(9) Uani 1 1 d . . . . .
H12 H 0.2740 0.9797 0.9920 0.057 Uiso 0.123(7) 1 calc R . P A 2
C13A C 0.3874(8) 0.4262(7) 0.7996(7) 0.0670(18) Uani 0.656(9) 1 d D U P B 1
H13A H 0.4468 0.5057 0.8242 0.080 Uiso 0.656(9) 1 calc R . P B 1
C13B C 0.3075(12) 0.3398(13) 0.7575(12) 0.0670(18) Uani 0.344(9) 1 d D U P B 2
H13B H 0.2359 0.2688 0.7117 0.080 Uiso 0.344(9) 1 calc R . P B 2
C14 C 0.5346(4) 0.9041(4) 0.9311(4) 0.0491(10) Uani 1 1 d . . . . .
H14 H 0.5574 0.8396 0.8842 0.059 Uiso 0.877(7) 1 calc R . P A 1
C15 C -0.1073(10) 0.2058(9) 0.8746(9) 0.124(3) Uani 1 1 d . U . . .
H15A H -0.1376 0.2236 0.9381 0.187 Uiso 1 1 calc GR . . . .
H15B H -0.0715 0.1293 0.8716 0.187 Uiso 1 1 calc GR . . . .
H15C H -0.1843 0.1943 0.8023 0.187 Uiso 1 1 calc GR . . . .
C16 C 0.1273(12) 0.3307(11) 0.9869(9) 0.152(4) Uani 1 1 d . U . . .
H16A H 0.1616 0.4204 1.0269 0.227 Uiso 1 1 calc GR . . . .
H16B H 0.1933 0.2977 0.9586 0.227 Uiso 1 1 calc GR . . . .
H16C H 0.1136 0.2867 1.0400 0.227 Uiso 1 1 calc GR . . . .
C17A C 0.3579(15) 0.2017(12) 0.8006(15) 0.141(5) Uani 0.656(9) 1 d D U P B 1
H17A H 0.3506 0.1874 0.8697 0.211 Uiso 0.656(9) 1 calc GR . P B 1
H17B H 0.4026 0.1398 0.7696 0.211 Uiso 0.656(9) 1 calc GR . P B 1
H17C H 0.2668 0.1935 0.7432 0.211 Uiso 0.656(9) 1 calc GR . P B 1
C17B C 0.420(3) 0.1898(13) 0.805(3) 0.141(5) Uani 0.344(9) 1 d D U P B 2
H17D H 0.3478 0.1568 0.8267 0.211 Uiso 0.344(9) 1 calc GR . P B 2
H17E H 0.5058 0.1706 0.8503 0.211 Uiso 0.344(9) 1 calc GR . P B 2
H17F H 0.3969 0.1511 0.7237 0.211 Uiso 0.344(9) 1 calc GR . P B 2
C18A C 0.5872(13) 0.3460(15) 0.8988(16) 0.147(5) Uani 0.656(9) 1 d D U P B 1
H18A H 0.6140 0.4183 0.9667 0.220 Uiso 0.656(9) 1 calc GR . P B 1
H18B H 0.6379 0.3621 0.8524 0.220 Uiso 0.656(9) 1 calc GR . P B 1
H18C H 0.6072 0.2715 0.9226 0.220 Uiso 0.656(9) 1 calc GR . P B 1
C18B C 0.5773(18) 0.400(2) 0.901(3) 0.147(5) Uani 0.344(9) 1 d D U P B 2
H18D H 0.5951 0.4699 0.8706 0.220 Uiso 0.344(9) 1 calc GR . P B 2
H18E H 0.6430 0.3473 0.8985 0.220 Uiso 0.344(9) 1 calc GR . P B 2
H18F H 0.5862 0.4339 0.9798 0.220 Uiso 0.344(9) 1 calc GR . P B 2
N1 N 0.0006(6) 0.3119(5) 0.8924(4) 0.0790(14) Uani 1 1 d . . . . .
N2 N 0.4360(6) 0.3245(6) 0.8285(5) 0.0954(17) Uani 1 1 d D U . . .
O1A O 0.2354(4) 0.9830(4) 0.9959(4) 0.0642(12) Uani 0.877(7) 1 d . . P A 1
H1A H 0.1848 0.9139 0.9529 0.096 Uiso 0.877(7) 1 calc GR . P A 1
O1B O 0.595(3) 0.811(3) 0.885(3) 0.0642(12) Uani 0.123(7) 1 d . U P A 2
H1B H 0.5353 0.7468 0.8436 0.096 Uiso 0.123(7) 1 calc R . P A 2
O2 O -0.0157(3) 0.3351(2) 0.5874(2) 0.0429(6) Uani 1 1 d . . . . .
O3 O 0.1629(3) 0.4950(3) 0.5231(3) 0.0458(6) Uani 1 1 d . U . . .
O4 O -0.0714(3) 0.2767(2) 0.3945(2) 0.0461(7) Uani 1 1 d . . . . .
O5 O 0.0716(4) 0.4777(3) 0.8360(3) 0.0581(8) Uani 1 1 d . . . . .
O6 O 0.1235(3) 0.4333(3) 0.3364(3) 0.0472(6) Uani 1 1 d . U . . .
O7 O 0.1757(3) 0.7527(3) 0.8482(2) 0.0477(7) Uani 1 1 d . . . . .
O8 O 0.3297(3) 0.6892(3) 0.7823(3) 0.0607(9) Uani 1 1 d . . . . .
O9 O 0.0476(6) -0.0524(3) 0.7089(3) 0.0831(14) Uani 1 1 d . . . . .
H9 H 0.0587 -0.1256 0.7048 0.125 Uiso 1 1 calc GR . . . .
O11A O 0.2653(9) 0.4110(8) 0.7414(10) 0.0685(19) Uani 0.656(9) 1 d D U P B 1
O11B O 0.290(2) 0.4458(15) 0.756(2) 0.0685(19) Uani 0.344(9) 1 d D U P B 2
O12 O 0.6768(4) 0.5984(5) 0.7320(3) 0.0728(11) Uani 1 1 d . . . . .
H12A H 0.7581 0.6021 0.7403 0.109 Uiso 1 1 calc GR . . . .
Tb1 Tb 0.10469(2) 0.54699(2) 0.68247(2) 0.03246(9) Uani 1 1 d . . . . .
C1A C 0.606(3) 0.189(2) 0.538(2) 0.150(4) Uani 0.532(10) 1 d . U P C 1
H1AA H 0.6844 0.1863 0.5208 0.180 Uiso 0.532(10) 1 calc R . P C 1
C1B C 0.502(4) 0.201(3) 0.559(2) 0.150(4) Uani 0.468(10) 1 d . U P C 2
H1BA H 0.4272 0.2190 0.5770 0.180 Uiso 0.468(10) 1 calc R . P C 2
C2A C 0.443(3) 0.112(2) 0.331(2) 0.151(5) Uani 0.532(10) 1 d . U P C 1
H2AA H 0.5253 0.1143 0.3155 0.226 Uiso 0.532(10) 1 calc GR . P C 1
H2AB H 0.3897 0.1676 0.2954 0.226 Uiso 0.532(10) 1 calc GR . P C 1
H2AC H 0.3882 0.0266 0.3003 0.226 Uiso 0.532(10) 1 calc GR . P C 1
C2B C 0.599(3) 0.142(3) 0.418(2) 0.151(5) Uani 0.468(10) 1 d . U P C 2
H2BA H 0.6748 0.2140 0.4676 0.226 Uiso 0.468(10) 1 calc GR . P C 2
H2BB H 0.5734 0.1414 0.3383 0.226 Uiso 0.468(10) 1 calc GR . P C 2
H2BC H 0.6279 0.0646 0.4280 0.226 Uiso 0.468(10) 1 calc GR . P C 2
C3A C 0.353(2) 0.147(2) 0.481(2) 0.156(5) Uani 0.532(10) 1 d . U P C 1
H3AA H 0.3217 0.0610 0.4797 0.234 Uiso 0.532(10) 1 calc GR . P C 1
H3AB H 0.2810 0.1712 0.4247 0.234 Uiso 0.532(10) 1 calc GR . P C 1
H3AC H 0.3765 0.2038 0.5577 0.234 Uiso 0.532(10) 1 calc GR . P C 1
C3B C 0.339(3) 0.119(3) 0.361(2) 0.156(5) Uani 0.468(10) 1 d . U P C 2
H3BA H 0.2734 0.1321 0.3973 0.234 Uiso 0.468(10) 1 calc GR . P C 2
H3BB H 0.3189 0.0305 0.3176 0.234 Uiso 0.468(10) 1 calc GR . P C 2
H3BC H 0.3314 0.1710 0.3097 0.234 Uiso 0.468(10) 1 calc GR . P C 2
N3 N 0.4792(10) 0.1538(7) 0.4517(8) 0.124(2) Uani 1 1 d . U . . .
O10 O 0.6166(11) 0.2253(10) 0.6407(8) 0.181(4) Uani 1 1 d . U . . .


_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
C1 C4 1.494(4) . ?
C1 C8 1.379(6) . ?
C1 C9 1.393(6) 2_556 ?
C2 C3 1.496(5) . ?
C2 O3 1.248(5) . ?
C2 O6 1.266(5) . ?
C3 C5 1.394(5) . ?
C3 C6 1.377(7) 2_666 ?
C4 O2 1.259(5) . ?
C4 O4 1.261(4) . ?
C5 H5 0.9300 . ?
C5 C6 1.394(6) . ?
C6 C3 1.377(7) 2_666 ?
C6 O12 1.365(5) . ?
C7 C11 1.498(5) . ?
C7 O7 1.268(5) . ?
C7 O8 1.241(5) . ?
C8 H8 0.9300 . ?
C8 C9 1.388(5) . ?
C9 C1 1.393(6) 2_556 ?
C9 O9 1.353(5) . ?
C10 H10 0.9300 . ?
C10 N1 1.312(6) . ?
C10 O5 1.237(6) . ?
C11 C12 1.398(6) . ?
C11 C14 1.389(6) . ?
C12 H12 0.9300 . ?
C12 C14 1.389(5) 2_677 ?
C12 O1A 1.356(6) . ?
C13A H13A 0.9300 . ?
C13A N2 1.358(7) . ?
C13A O11A 1.208(10) . ?
C13B H13B 0.9300 . ?
C13B N2 1.395(10) . ?
C13B O11B 1.208(11) . ?
C14 C12 1.389(5) 2_677 ?
C14 H14 0.9300 . ?
C14 O1B 1.39(3) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C15 N1 1.450(9) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C16 N1 1.403(10) . ?
C17A H17A 0.9600 . ?
C17A H17B 0.9600 . ?
C17A H17C 0.9600 . ?
C17A N2 1.396(12) . ?
C17B H17D 0.9600 . ?
C17B H17E 0.9600 . ?
C17B H17F 0.9600 . ?
C17B N2 1.421(13) . ?
C18A H18A 0.9600 . ?
C18A H18B 0.9600 . ?
C18A H18C 0.9600 . ?
C18A N2 1.486(12) . ?
C18B H18D 0.9600 . ?
C18B H18E 0.9600 . ?
C18B H18F 0.9600 . ?
C18B N2 1.469(14) . ?
O1A H1A 0.8200 . ?
O1B H1B 0.8200 . ?
O2 Tb1 2.335(2) . ?
O3 Tb1 2.297(3) . ?
O4 Tb1 2.380(2) 2_566 ?
O5 Tb1 2.383(3) . ?
O6 Tb1 2.372(3) 2_566 ?
O7 Tb1 2.538(3) . ?
O8 Tb1 2.408(3) . ?
O9 H9 0.8200 . ?
O11A Tb1 2.425(8) . ?
O11B Tb1 2.370(16) . ?
O12 H12A 0.8200 . ?
Tb1 O4 2.380(2) 2_566 ?
Tb1 O6 2.372(3) 2_566 ?
C1A H1AA 0.9300 . ?
C1A N3 1.34(3) . ?
C1A O10 1.24(3) . ?
C1B H1BA 0.9300 . ?
C1B N3 1.27(3) . ?
C1B O10 1.24(3) . ?
C2A H2AA 0.9600 . ?
C2A H2AB 0.9600 . ?
C2A H2AC 0.9600 . ?
C2A N3 1.39(2) . ?
C2B H2BA 0.9600 . ?
C2B H2BB 0.9600 . ?
C2B H2BC 0.9600 . ?
C2B N3 1.48(3) . ?
C3A H3AA 0.9600 . ?
C3A H3AB 0.9600 . ?
C3A H3AC 0.9600 . ?
C3A N3 1.50(2) . ?
C3B H3BA 0.9600 . ?
C3B H3BB 0.9600 . ?
C3B H3BC 0.9600 . ?
C3B N3 1.46(3) . ?

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
C8 C1 C4 119.6(3) . . ?
C8 C1 C9 118.7(3) . 2_556 ?
C9 C1 C4 121.6(3) 2_556 . ?
O3 C2 C3 120.5(4) . . ?
O3 C2 O6 121.5(4) . . ?
O6 C2 C3 117.9(4) . . ?
C5 C3 C2 118.4(4) . . ?
C6 C3 C2 121.4(4) 2_666 . ?
C6 C3 C5 120.2(4) 2_666 . ?
O2 C4 C1 117.9(3) . . ?
O2 C4 O4 125.0(3) . . ?
O4 C4 C1 117.2(3) . . ?
C3 C5 H5 120.1 . . ?
C3 C5 C6 119.9(4) . . ?
C6 C5 H5 120.1 . . ?
C3 C6 C5 119.9(4) 2_666 . ?
O12 C6 C3 123.5(4) . 2_666 ?
O12 C6 C5 116.7(4) . . ?
O7 C7 C11 119.2(4) . . ?
O8 C7 C11 119.4(4) . . ?
O8 C7 O7 121.4(3) . . ?
C1 C8 H8 118.7 . . ?
C1 C8 C9 122.6(4) . . ?
C9 C8 H8 118.7 . . ?
C8 C9 C1 118.7(4) . 2_556 ?
O9 C9 C1 124.0(3) . 2_556 ?
O9 C9 C8 117.2(4) . . ?
N1 C10 H10 117.6 . . ?
O5 C10 H10 117.6 . . ?
O5 C10 N1 124.8(5) . . ?
C12 C11 C7 121.4(4) . . ?
C14 C11 C7 118.8(4) . . ?
C14 C11 C12 119.8(3) . . ?
C11 C12 H12 120.5 . . ?
C14 C12 C11 119.0(4) 2_677 . ?
C14 C12 H12 120.5 2_677 . ?
O1A C12 C11 124.1(4) . . ?
O1A C12 C14 117.0(4) . 2_677 ?
N2 C13A H13A 120.8 . . ?
O11A C13A H13A 120.8 . . ?
O11A C13A N2 118.4(8) . . ?
N2 C13B H13B 120.2 . . ?
O11B C13B H13B 120.2 . . ?
O11B C13B N2 119.6(16) . . ?
C11 C14 C12 121.2(4) . 2_677 ?
C11 C14 H14 119.4 . . ?
C12 C14 H14 119.4 2_677 . ?
O1B C14 C11 127.9(11) . . ?
O1B C14 C12 109.9(11) . 2_677 ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N1 C15 H15A 109.5 . . ?
N1 C15 H15B 109.5 . . ?
N1 C15 H15C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N1 C16 H16A 109.5 . . ?
N1 C16 H16B 109.5 . . ?
N1 C16 H16C 109.5 . . ?
H17A C17A H17B 109.5 . . ?
H17A C17A H17C 109.5 . . ?
H17B C17A H17C 109.5 . . ?
N2 C17A H17A 109.5 . . ?
N2 C17A H17B 109.5 . . ?
N2 C17A H17C 109.5 . . ?
H17D C17B H17E 109.5 . . ?
H17D C17B H17F 109.5 . . ?
H17E C17B H17F 109.5 . . ?
N2 C17B H17D 109.5 . . ?
N2 C17B H17E 109.5 . . ?
N2 C17B H17F 109.5 . . ?
H18A C18A H18B 109.5 . . ?
H18A C18A H18C 109.5 . . ?
H18B C18A H18C 109.5 . . ?
N2 C18A H18A 109.5 . . ?
N2 C18A H18B 109.5 . . ?
N2 C18A H18C 109.5 . . ?
H18D C18B H18E 109.5 . . ?
H18D C18B H18F 109.5 . . ?
H18E C18B H18F 109.5 . . ?
N2 C18B H18D 109.5 . . ?
N2 C18B H18E 109.5 . . ?
N2 C18B H18F 109.5 . . ?
C10 N1 C15 122.5(6) . . ?
C10 N1 C16 121.2(6) . . ?
C16 N1 C15 116.3(6) . . ?
C13A N2 C17A 126.6(8) . . ?
C13A N2 C18A 117.0(8) . . ?
C13B N2 C17B 104.0(12) . . ?
C13B N2 C18B 139.4(13) . . ?
C17A N2 C18A 116.4(9) . . ?
C17B N2 C18B 115.8(12) . . ?
C12 O1A H1A 109.5 . . ?
C14 O1B H1B 109.5 . . ?
C4 O2 Tb1 135.7(3) . . ?
C2 O3 Tb1 174.7(3) . . ?
C4 O4 Tb1 138.9(2) . 2_566 ?
C10 O5 Tb1 126.2(3) . . ?
C2 O6 Tb1 110.6(3) . 2_566 ?
C7 O7 Tb1 89.6(2) . . ?
C7 O8 Tb1 96.3(2) . . ?
C9 O9 H9 109.5 . . ?
C13A O11A Tb1 136.4(6) . . ?
C13B O11B Tb1 138.8(15) . . ?
C6 O12 H12A 109.5 . . ?
O2 Tb1 O4 126.17(9) . 2_566 ?
O2 Tb1 O5 77.39(10) . . ?
O2 Tb1 O6 79.32(10) . 2_566 ?
O2 Tb1 O7 151.83(10) . . ?
O2 Tb1 O8 145.55(10) . . ?
O2 Tb1 O11A 72.4(2) . . ?
O2 Tb1 O11B 81.8(5) . . ?
O3 Tb1 O2 77.13(10) . . ?
O3 Tb1 O4 76.57(10) . 2_566 ?
O3 Tb1 O5 145.73(11) . . ?
O3 Tb1 O6 122.02(10) . 2_566 ?
O3 Tb1 O7 131.04(9) . . ?
O3 Tb1 O8 86.38(11) . . ?
O3 Tb1 O11A 79.4(3) . . ?
O3 Tb1 O11B 80.2(6) . . ?
O4 Tb1 O5 137.56(11) 2_566 . ?
O4 Tb1 O7 70.06(9) 2_566 . ?
O4 Tb1 O8 77.35(11) 2_566 . ?
O4 Tb1 O11A 144.2(3) 2_566 . ?
O5 Tb1 O7 76.54(10) . . ?
O5 Tb1 O8 102.33(12) . . ?
O5 Tb1 O11A 71.3(3) . . ?
O6 Tb1 O4 76.32(10) 2_566 2_566 ?
O6 Tb1 O5 74.66(11) 2_566 . ?
O6 Tb1 O7 83.69(10) 2_566 . ?
O6 Tb1 O8 134.44(10) 2_566 . ?
O6 Tb1 O11A 139.4(3) 2_566 . ?
O8 Tb1 O7 52.43(10) . . ?
O8 Tb1 O11A 75.0(2) . . ?
O11A Tb1 O7 108.6(2) . . ?
O11B Tb1 O4 137.1(5) . 2_566 ?
O11B Tb1 O5 73.8(6) . . ?
O11B Tb1 O6 146.0(6) . 2_566 ?
O11B Tb1 O7 100.9(5) . . ?
O11B Tb1 O8 65.6(5) . . ?
N3 C1A H1AA 120.5 . . ?
O10 C1A H1AA 120.5 . . ?
O10 C1A N3 119(3) . . ?
N3 C1B H1BA 117.4 . . ?
O10 C1B H1BA 117.4 . . ?
O10 C1B N3 125(3) . . ?
H2AA C2A H2AB 109.5 . . ?
H2AA C2A H2AC 109.5 . . ?
H2AB C2A H2AC 109.5 . . ?
N3 C2A H2AA 109.5 . . ?
N3 C2A H2AB 109.5 . . ?
N3 C2A H2AC 109.5 . . ?
H2BA C2B H2BB 109.5 . . ?
H2BA C2B H2BC 109.5 . . ?
H2BB C2B H2BC 109.5 . . ?
N3 C2B H2BA 109.5 . . ?
N3 C2B H2BB 109.5 . . ?
N3 C2B H2BC 109.5 . . ?
H3AA C3A H3AB 109.5 . . ?
H3AA C3A H3AC 109.5 . . ?
H3AB C3A H3AC 109.5 . . ?
N3 C3A H3AA 109.5 . . ?
N3 C3A H3AB 109.5 . . ?
N3 C3A H3AC 109.5 . . ?
H3BA C3B H3BB 109.5 . . ?
H3BA C3B H3BC 109.5 . . ?
H3BB C3B H3BC 109.5 . . ?
N3 C3B H3BA 109.5 . . ?
N3 C3B H3BB 109.5 . . ?
N3 C3B H3BC 109.5 . . ?
C1A N3 C2A 129(2) . . ?
C1A N3 C3A 119.7(17) . . ?
C1B N3 C2B 118(2) . . ?
C1B N3 C3B 121(2) . . ?
C2A N3 C3A 111.4(16) . . ?
C3B N3 C2B 120.0(18) . . ?

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
C1 C4 O2 Tb1 134.8(3) . . . . ?
C1 C4 O4 Tb1 -175.5(3) . . . 2_566 ?
C1 C8 C9 C1 0.6(8) . . . 2_556 ?
C1 C8 C9 O9 179.6(5) . . . . ?
C2 C3 C5 C6 179.4(4) . . . . ?
C3 C2 O6 Tb1 -169.8(3) . . . 2_566 ?
C3 C5 C6 C3 -0.6(7) . . . 2_666 ?
C3 C5 C6 O12 179.8(4) . . . . ?
C4 C1 C8 C9 -177.5(4) . . . . ?
C6 C3 C5 C6 0.6(7) 2_666 . . . ?
C7 C11 C12 C14 179.2(4) . . . 2_677 ?
C7 C11 C12 O1A -0.4(7) . . . . ?
C7 C11 C14 C12 -179.2(4) . . . 2_677 ?
C7 C11 C14 O1B -11.6(18) . . . . ?
C8 C1 C4 O2 6.2(6) . . . . ?
C8 C1 C4 O4 -174.0(4) . . . . ?
C9 C1 C4 O2 -170.7(4) 2_556 . . . ?
C9 C1 C4 O4 9.1(6) 2_556 . . . ?
C9 C1 C8 C9 -0.6(8) 2_556 . . . ?
C11 C7 O7 Tb1 176.7(3) . . . . ?
C11 C7 O8 Tb1 -176.4(3) . . . . ?
C12 C11 C14 C12 0.9(7) . . . 2_677 ?
C12 C11 C14 O1B 168.5(18) . . . . ?
C14 C11 C12 C14 -0.9(7) . . . 2_677 ?
C14 C11 C12 O1A 179.5(5) . . . . ?
N1 C10 O5 Tb1 145.8(5) . . . . ?
N2 C13A O11A Tb1 169.2(8) . . . . ?
N2 C13B O11B Tb1 -169.8(18) . . . . ?
O2 C4 O4 Tb1 4.3(7) . . . 2_566 ?
O3 C2 C3 C5 -3.5(6) . . . . ?
O3 C2 C3 C6 175.3(4) . . . 2_666 ?
O3 C2 O6 Tb1 9.4(4) . . . 2_566 ?
O4 C4 O2 Tb1 -45.1(6) . . . . ?
O5 C10 N1 C15 179.8(7) . . . . ?
O5 C10 N1 C16 -1.0(12) . . . . ?
O6 C2 C3 C5 175.7(4) . . . . ?
O6 C2 C3 C6 -5.5(6) . . . 2_666 ?
O7 C7 C11 C12 -5.5(6) . . . . ?
O7 C7 C11 C14 174.6(4) . . . . ?
O7 C7 O8 Tb1 5.6(4) . . . . ?
O8 C7 C11 C12 176.4(4) . . . . ?
O8 C7 C11 C14 -3.5(6) . . . . ?
O8 C7 O7 Tb1 -5.3(4) . . . . ?
O11A C13A N2 C17A -2.1(15) . . . . ?
O11A C13A N2 C18A 179.1(10) . . . . ?
O11B C13B N2 C17B -178.1(11) . . . . ?
O11B C13B N2 C18B -10(2) . . . . ?
O10 C1A N3 C2A 178.9(18) . . . . ?
O10 C1A N3 C3A -6(3) . . . . ?
O10 C1B N3 C2B -9(3) . . . . ?
O10 C1B N3 C3B 175(2) . . . . ?

_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 1.147
_oxdiff_exptl_absorpt_empirical_full_min 0.828

# start Validation Reply Form
_vrf_PLAT029_SION2_300K          
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.743 Why?  
RESPONSE: The data were collected upon the spindle rotation. Therefore, a 
		  limited portion of the reciprocal space could be probed.
;
# 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_SION2_180K_cool
_database_code_depnum_ccdc_archive 'CCDC 1941014'
loop_
_audit_author_name
_audit_author_address
'Andrzej Gladysiak'
;Ecole polytechnique federale de Lausanne
Switzerland
;
_audit_update_record             
;
2019-07-16 deposited with the CCDC.	2019-08-12 downloaded from the CCDC.
;
_audit_creation_date             2019-05-27
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C18 H20 N2 O11 Tb'
_chemical_formula_sum            'C18 H20 N2 O11 Tb'
_chemical_formula_weight         599.28
_chemical_melting_point          ?
_chemical_oxdiff_formula         C21H27N3O12Tb
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0045 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'
N N 0.0083 0.0040 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0145 0.0076 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.0972 4.9386 '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                   10.6430(6)
_cell_length_b                   11.1747(5)
_cell_length_c                   11.4401(6)
_cell_angle_alpha                96.900(4)
_cell_angle_beta                 111.066(5)
_cell_angle_gamma                101.426(4)
_cell_volume                     1216.97(12)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3142
_cell_measurement_temperature    180.0
_cell_measurement_theta_max      32.2150
_cell_measurement_theta_min      2.1300
_shelx_estimated_absorpt_T_max   0.776
_shelx_estimated_absorpt_T_min   0.515
_exptl_absorpt_coefficient_mu    3.819
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84131
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.635
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             590
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0085
_diffrn_reflns_av_unetI/netI     0.0131
_diffrn_reflns_Laue_measured_fraction_full 0.713
_diffrn_reflns_Laue_measured_fraction_max 0.542
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6784
_diffrn_reflns_point_group_measured_fraction_full 0.713
_diffrn_reflns_point_group_measured_fraction_max 0.542
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         32.226
_diffrn_reflns_theta_min         2.098
_diffrn_ambient_temperature      180.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            PILATUS2M
_diffrn_measured_fraction_theta_full 0.713
_diffrn_measured_fraction_theta_max 0.542
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      0.00 360.00   1.00    1.00    --    0.00   0.00   0.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  PILATUS@SNBL
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0667381000
_diffrn_orient_matrix_UB_12      -0.0036479000
_diffrn_orient_matrix_UB_13      -0.0130528000
_diffrn_orient_matrix_UB_21      0.0459502000
_diffrn_orient_matrix_UB_22      0.0515920000
_diffrn_orient_matrix_UB_23      0.0619459000
_diffrn_orient_matrix_UB_31      0.0109706000
_diffrn_orient_matrix_UB_32      -0.0518011000
_diffrn_orient_matrix_UB_33      0.0404128000
_diffrn_radiation_monochromator  'Si (111)'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.78405
_diffrn_source                   
'European Synchrotron Radiation Facility, BM01 beamline'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3320
_reflns_number_total             3477
_reflns_odcompleteness_completeness 62.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     29.34
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         6.780
_refine_diff_density_min         -2.839
_refine_diff_density_rms         0.303
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     292
_refine_ls_number_reflns         3477
_refine_ls_number_restraints     34
_refine_ls_R_factor_all          0.0788
_refine_ls_R_factor_gt           0.0771
_refine_ls_restrained_S_all      6.526
_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)+(0.1632P)²+4.1499P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1982
_refine_ls_wR_factor_ref         0.2016
_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
 C17-C13 \\sim C13-C18
 with sigma of 0.02
 C12_$6-O1 \\sim O1-C11
 with sigma of 0.05
3. Restrained planarity
 C13, C17, C18, N2, O11
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C17) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
5. Rigid body (RIGU) restrains
 O11, C13, N2, C18, C17
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Me refined with riding coordinates:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C)
6.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C8(H8), C12(H12), C13(H13), C16(H16)
6.c Tetrahedral OH refined with riding coordinates:
 O1(H1), O12(H12A)
6.d Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C15(H15A,H15B,H15C)
6.e Idealised tetrahedral OH refined as rotating group:
 O9(H9)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
C1 C -0.0208(9) 0.1204(9) 0.4972(10) 0.038(3) Uani 1 1 d . . . . .
C2 C 0.2047(9) 0.4850(9) 0.4305(10) 0.037(2) Uani 1 1 d . . . . .
C3 C 0.3573(9) 0.4947(10) 0.4664(10) 0.039(3) Uani 1 1 d . . . . .
C4 C -0.0363(9) 0.2523(10) 0.4992(11) 0.042(3) Uani 1 1 d . . . . .
C5 C 0.4519(10) 0.5382(12) 0.5939(10) 0.046(3) Uani 1 1 d . . . . .
H5 H 0.419606 0.564911 0.657439 0.055 Uiso 1 1 calc R . . . .
C6 C 0.5937(10) 0.5429(12) 0.6294(10) 0.045(3) Uani 1 1 d . . . . .
C7 C 0.3022(9) 0.7601(9) 0.8596(10) 0.035(2) Uani 1 1 d . . . . .
C8 C 0.0032(12) 0.0730(11) 0.6093(10) 0.044(3) Uani 1 1 d . . . . .
H8 H 0.004566 0.122984 0.683306 0.053 Uiso 1 1 calc R . . . .
C9 C 0.0248(11) -0.0449(10) 0.6147(10) 0.039(3) Uani 1 1 d . . . . .
C10 C 0.0496(16) 0.1786(15) 0.9906(17) 0.066(4) Uani 1 1 d . . . . .
H10A H 0.017783 0.180105 1.061122 0.099 Uiso 1 1 calc GR . . . .
H10B H 0.150259 0.186994 1.024394 0.099 Uiso 1 1 calc GR . . . .
H10C H 0.000911 0.099370 0.928439 0.099 Uiso 1 1 calc GR . . . .
C11 C 0.4009(9) 0.8857(10) 0.9323(11) 0.045(3) Uani 1 1 d D . . . .
C12 C 0.3620(10) 0.9675(12) 0.9919(14) 0.056(3) Uani 1 1 d D . . . .
H12 H 0.270615 0.947022 0.990995 0.068 Uiso 1 1 calc R . . A 2
C13 C 0.3112(14) 0.3295(13) 0.7216(14) 0.070(4) Uani 1 1 d D U . . .
H13 H 0.242065 0.279963 0.642821 0.084 Uiso 1 1 calc R . . . .
C14 C 0.5438(10) 0.9086(12) 0.9390(13) 0.056(4) Uani 1 1 d . . . . .
C15 C -0.1278(15) 0.2773(17) 0.8585(18) 0.075(4) Uani 1 1 d . . . . .
H15A H -0.173062 0.285920 0.918933 0.112 Uiso 1 1 calc GR . . . .
H15B H -0.175934 0.198055 0.796247 0.112 Uiso 1 1 calc GR . . . .
H15C H -0.132087 0.346628 0.813551 0.112 Uiso 1 1 calc GR . . . .
C16 C 0.1179(13) 0.3721(15) 0.9323(13) 0.054(4) Uani 1 1 d . . . . .
H16 H 0.211847 0.370524 0.977087 0.065 Uiso 1 1 calc R . . . .
C17 C 0.434(3) 0.177(2) 0.698(3) 0.138(9) Uani 1 1 d D U . . .
H17A H 0.522993 0.159147 0.744625 0.207 Uiso 1 1 calc R . . . .
H17B H 0.357021 0.107011 0.689779 0.207 Uiso 1 1 calc R . . . .
H17C H 0.427458 0.188942 0.613185 0.207 Uiso 1 1 calc R . . . .
C18 C 0.535(2) 0.366(2) 0.891(2) 0.108(7) Uani 1 1 d D U . . .
H18A H 0.611825 0.326684 0.914556 0.162 Uiso 1 1 calc R . . . .
H18B H 0.567904 0.450945 0.879788 0.162 Uiso 1 1 calc R . . . .
H18C H 0.498399 0.370865 0.958226 0.162 Uiso 1 1 calc R . . . .
N1 N 0.0202(10) 0.2792(11) 0.9296(10) 0.052(3) Uani 1 1 d . . . . .
N2 N 0.4246(14) 0.2937(14) 0.7715(15) 0.080(4) Uani 1 1 d . U . . .
O1 O 0.5948(9) 0.8181(10) 0.8827(13) 0.088(4) Uani 1 1 d D . . . .
H1 H 0.528387 0.755573 0.838692 0.132 Uiso 1 1 calc R . . . .
O2 O -0.0090(7) 0.3204(7) 0.6069(7) 0.0399(18) Uani 1 1 d . . . . .
O3 O 0.1604(7) 0.5044(7) 0.5187(8) 0.0428(18) Uani 1 1 d . . . . .
O4 O -0.0718(7) 0.2864(7) 0.3917(7) 0.0395(17) Uani 1 1 d . . . . .
O5 O 0.0980(10) 0.4636(10) 0.8806(8) 0.054(2) Uani 1 1 d . . . . .
O6 O 0.1220(6) 0.4582(7) 0.3119(7) 0.0424(18) Uani 1 1 d . . . . .
O7 O 0.1853(7) 0.7302(7) 0.8697(7) 0.0401(17) Uani 1 1 d . . . . .
O8 O 0.3377(7) 0.6852(7) 0.7914(8) 0.049(2) Uani 1 1 d . . . . .
O9 O 0.0462(11) -0.0812(9) 0.7287(8) 0.057(2) Uani 1 1 d . . . . .
H9 H 0.048506 -0.156337 0.720219 0.086 Uiso 1 1 calc GR . . . .
O11 O 0.2865(8) 0.4234(9) 0.7692(10) 0.059(2) Uani 1 1 d . U . . .
O12 O 0.6808(8) 0.5834(12) 0.7565(8) 0.069(3) Uani 1 1 d . . . . .
H12A H 0.762442 0.581992 0.765664 0.103 Uiso 1 1 calc R . . . .
Tb1 Tb 0.10766(3) 0.53520(4) 0.69931(4) 0.0319(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
C1 C4 1.514(15) . ?
C1 C8 1.405(18) . ?
C1 C9 1.428(13) 2_556 ?
C2 C3 1.503(11) . ?
C2 O3 1.271(12) . ?
C2 O6 1.282(13) . ?
C3 C5 1.399(14) . ?
C3 C6 1.427(14) 2_666 ?
C4 O2 1.270(12) . ?
C4 O4 1.279(15) . ?
C5 H5 0.9500 . ?
C5 C6 1.404(13) . ?
C6 O12 1.373(13) . ?
C7 C11 1.507(12) . ?
C7 O7 1.273(12) . ?
C7 O8 1.277(11) . ?
C8 H8 0.9500 . ?
C8 C9 1.387(17) . ?
C9 O9 1.366(15) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C10 N1 1.42(2) . ?
C11 C12 1.294(15) . ?
C11 C14 1.463(13) . ?
C12 H12 0.9500 . ?
C12 C14 1.471(15) 2_677 ?
C13 H13 0.9500 . ?
C13 N2 1.301(19) . ?
C13 O11 1.241(16) . ?
C14 O1 1.430(13) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C15 N1 1.485(18) . ?
C16 H16 0.9500 . ?
C16 N1 1.305(19) . ?
C16 O5 1.258(19) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C17 N2 1.50(3) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C18 N2 1.45(2) . ?
O1 H1 0.8400 . ?
O2 Tb1 2.384(7) . ?
O3 Tb1 2.333(7) . ?
O4 Tb1 2.391(8) 2_566 ?
O5 Tb1 2.339(10) . ?
O6 Tb1 2.418(6) 2_566 ?
O7 Tb1 2.518(6) . ?
O8 Tb1 2.451(7) . ?
O9 H9 0.8400 . ?
O11 Tb1 2.432(8) . ?
O12 H12A 0.8400 . ?

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
C8 C1 C4 119.2(9) . . ?
C8 C1 C9 119.3(10) . 2_556 ?
C9 C1 C4 121.4(11) 2_556 . ?
O3 C2 C3 119.1(9) . . ?
O3 C2 O6 121.4(8) . . ?
O6 C2 C3 119.5(8) . . ?
C5 C3 C2 120.5(9) . . ?
C5 C3 C6 119.5(8) . 2_666 ?
C6 C3 C2 120.0(9) 2_666 . ?
O2 C4 C1 117.7(11) . . ?
O2 C4 O4 125.7(10) . . ?
O4 C4 C1 116.6(9) . . ?
C3 C5 H5 119.5 . . ?
C3 C5 C6 120.9(9) . . ?
C6 C5 H5 119.5 . . ?
C5 C6 C3 119.5(9) . 2_666 ?
O12 C6 C3 122.2(9) . 2_666 ?
O12 C6 C5 118.3(9) . . ?
O7 C7 C11 118.7(8) . . ?
O7 C7 O8 121.3(8) . . ?
O8 C7 C11 119.9(9) . . ?
C1 C8 H8 119.2 . . ?
C9 C8 C1 121.6(9) . . ?
C9 C8 H8 119.2 . . ?
C8 C9 C1 119.0(10) . 2_556 ?
O9 C9 C1 124.6(10) . 2_556 ?
O9 C9 C8 116.3(9) . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N1 C10 H10A 109.5 . . ?
N1 C10 H10B 109.5 . . ?
N1 C10 H10C 109.5 . . ?
C12 C11 C7 120.8(9) . . ?
C12 C11 C14 121.4(9) . . ?
C14 C11 C7 117.7(9) . . ?
C11 C12 H12 119.3 . . ?
C11 C12 C14 121.4(9) . 2_677 ?
C14 C12 H12 119.3 2_677 . ?
N2 C13 H13 117.5 . . ?
O11 C13 H13 117.5 . . ?
O11 C13 N2 125.0(14) . . ?
C11 C14 C12 116.9(9) . 2_677 ?
O1 C14 C11 123.6(9) . . ?
O1 C14 C12 119.4(9) . 2_677 ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N1 C15 H15A 109.5 . . ?
N1 C15 H15B 109.5 . . ?
N1 C15 H15C 109.5 . . ?
N1 C16 H16 117.3 . . ?
O5 C16 H16 117.3 . . ?
O5 C16 N1 125.3(13) . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N2 C17 H17A 109.5 . . ?
N2 C17 H17B 109.5 . . ?
N2 C17 H17C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N2 C18 H18A 109.5 . . ?
N2 C18 H18B 109.5 . . ?
N2 C18 H18C 109.5 . . ?
C10 N1 C15 118.5(12) . . ?
C16 N1 C10 122.6(13) . . ?
C16 N1 C15 118.9(14) . . ?
C13 N2 C17 116.5(16) . . ?
C13 N2 C18 120.0(15) . . ?
C18 N2 C17 123.4(18) . . ?
C14 O1 H1 109.5 . . ?
C4 O2 Tb1 132.7(7) . . ?
C2 O3 Tb1 172.1(7) . . ?
C4 O4 Tb1 141.6(6) . 2_566 ?
C16 O5 Tb1 138.8(8) . . ?
C2 O6 Tb1 107.7(5) . 2_566 ?
C7 O7 Tb1 91.0(5) . . ?
C7 O8 Tb1 93.9(5) . . ?
C9 O9 H9 109.5 . . ?
C13 O11 Tb1 135.5(9) . . ?
C6 O12 H12A 109.5 . . ?
O2 Tb1 O4 128.6(3) . 2_566 ?
O2 Tb1 O6 81.7(2) . 2_566 ?
O2 Tb1 O7 153.3(3) . . ?
O2 Tb1 O8 143.2(2) . . ?
O2 Tb1 O11 74.6(3) . . ?
O3 Tb1 O2 78.1(3) . . ?
O3 Tb1 O4 75.7(3) . 2_566 ?
O3 Tb1 O5 147.3(3) . . ?
O3 Tb1 O6 123.2(3) . 2_566 ?
O3 Tb1 O7 128.5(3) . . ?
O3 Tb1 O8 83.3(3) . . ?
O3 Tb1 O11 78.9(3) . . ?
O4 Tb1 O6 77.1(3) 2_566 2_566 ?
O4 Tb1 O7 68.4(3) 2_566 . ?
O4 Tb1 O8 75.3(3) 2_566 . ?
O4 Tb1 O11 139.5(3) 2_566 . ?
O5 Tb1 O2 79.7(3) . . ?
O5 Tb1 O4 136.9(3) . 2_566 ?
O5 Tb1 O6 76.4(3) . 2_566 ?
O5 Tb1 O7 75.4(3) . . ?
O5 Tb1 O8 100.9(3) . . ?
O5 Tb1 O11 72.2(3) . . ?
O6 Tb1 O7 83.4(2) 2_566 . ?
O6 Tb1 O8 134.6(2) 2_566 . ?
O6 Tb1 O11 143.4(3) 2_566 . ?
O8 Tb1 O7 53.1(2) . . ?
O11 Tb1 O7 106.1(3) . . ?
O11 Tb1 O8 70.8(3) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O1 H1 O8 0.84 1.87 2.598(11) 143.7 . yes
O9 H9 O4 0.84 1.93 2.644(11) 141.6 2_556 yes
O12 H12A O6 0.84 1.85 2.589(10) 146.8 2_666 yes

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
C1 C4 O2 Tb1 139.8(8) . . . . ?
C1 C4 O4 Tb1 -175.2(7) . . . 2_566 ?
C1 C8 C9 C1 -0.8(17) . . . 2_556 ?
C1 C8 C9 O9 -179.6(10) . . . . ?
C2 C3 C5 C6 177.4(12) . . . . ?
C3 C2 O6 Tb1 -176.8(8) . . . 2_566 ?
C3 C5 C6 C3 1(2) . . . 2_666 ?
C3 C5 C6 O12 -178.3(13) . . . . ?
C4 C1 C8 C9 -176.9(10) . . . . ?
C6 C3 C5 C6 -1(2) 2_666 . . . ?
C7 C11 C12 C14 -178.7(13) . . . 2_677 ?
C7 C11 C14 C12 178.8(13) . . . 2_677 ?
C7 C11 C14 O1 -1(2) . . . . ?
C8 C1 C4 O2 8.9(13) . . . . ?
C8 C1 C4 O4 -173.2(9) . . . . ?
C9 C1 C4 O2 -168.7(9) 2_556 . . . ?
C9 C1 C4 O4 9.2(13) 2_556 . . . ?
C9 C1 C8 C9 0.8(17) 2_556 . . . ?
C11 C7 O7 Tb1 173.1(10) . . . . ?
C11 C7 O8 Tb1 -172.9(10) . . . . ?
C12 C11 C14 C12 -5(3) . . . 2_677 ?
C12 C11 C14 O1 175.4(15) . . . . ?
C14 C11 C12 C14 5(3) . . . 2_677 ?
N1 C16 O5 Tb1 -103.7(16) . . . . ?
N2 C13 O11 Tb1 171.3(10) . . . . ?
O2 C4 O4 Tb1 2.4(16) . . . 2_566 ?
O3 C2 C3 C5 -7.2(17) . . . . ?
O3 C2 C3 C6 171.5(11) . . . 2_666 ?
O3 C2 O6 Tb1 2.9(13) . . . 2_566 ?
O4 C4 O2 Tb1 -37.8(14) . . . . ?
O5 C16 N1 C10 -179.7(12) . . . . ?
O5 C16 N1 C15 1(2) . . . . ?
O6 C2 C3 C5 172.4(12) . . . . ?
O6 C2 C3 C6 -8.8(17) . . . 2_666 ?
O7 C7 C11 C12 -7.9(19) . . . . ?
O7 C7 C11 C14 168.6(12) . . . . ?
O7 C7 O8 Tb1 8.3(12) . . . . ?
O8 C7 C11 C12 173.4(13) . . . . ?
O8 C7 C11 C14 -10.2(18) . . . . ?
O8 C7 O7 Tb1 -8.1(12) . . . . ?
O11 C13 N2 C17 -180.0(11) . . . . ?
O11 C13 N2 C18 -0.9(19) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.500 0.000 0.500 209.9 0.0 ?


_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 1.517
_oxdiff_exptl_absorpt_empirical_full_min 0.734

# start Validation Reply Form
_vrf_PLAT027_SION2_180K_cool     
;
PROBLEM: _diffrn_reflns_theta_full value (too) Low ......      26.00 Degree
RESPONSE: Our value of max sin(theta)/lambda of 0.56 is close to the recommended 
		  value of 0.60. Higer values of sin(theta)/lambda were not available due 
		  to the beamline experimental set-up limitations. 
;
_vrf_PLAT029_SION2_180K_cool     
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.713 Why?  
RESPONSE: The data were collected upon the spindle rotation. Therefore, a 
		  limited portion of the reciprocal space could be probed.
;
# 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_SION2_100K_cool
_database_code_depnum_ccdc_archive 'CCDC 1941013'
loop_
_audit_author_name
_audit_author_address
'Andrzej Gladysiak'
;Ecole polytechnique federale de Lausanne
Switzerland
;
_audit_update_record             
;
2019-07-16 deposited with the CCDC.	2019-08-12 downloaded from the CCDC.
;
_audit_creation_date             2019-05-27
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C18 H20 N2 O11 Tb'
_chemical_formula_sum            'C18 H20 N2 O11 Tb'
_chemical_formula_weight         599.28
_chemical_melting_point          ?
_chemical_oxdiff_formula         C21H27N3O12Tb
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0045 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'
N N 0.0083 0.0040 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0145 0.0076 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.0972 4.9386 '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                   10.6219(6)
_cell_length_b                   11.1750(5)
_cell_length_c                   11.3531(5)
_cell_angle_alpha                96.985(4)
_cell_angle_beta                 110.840(5)
_cell_angle_gamma                101.422(4)
_cell_volume                     1207.06(11)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3172
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      31.9480
_cell_measurement_theta_min      2.1420
_shelx_estimated_absorpt_T_max   0.774
_shelx_estimated_absorpt_T_min   0.513
_exptl_absorpt_coefficient_mu    3.851
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80711
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.649
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             590
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0096
_diffrn_reflns_av_unetI/netI     0.0152
_diffrn_reflns_Laue_measured_fraction_full 0.715
_diffrn_reflns_Laue_measured_fraction_max 0.546
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6750
_diffrn_reflns_point_group_measured_fraction_full 0.715
_diffrn_reflns_point_group_measured_fraction_max 0.546
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         32.216
_diffrn_reflns_theta_min         2.098
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            PILATUS2M
_diffrn_measured_fraction_theta_full 0.715
_diffrn_measured_fraction_theta_max 0.546
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      0.00 360.00   1.00    1.00    --    0.00   0.00   0.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  PILATUS@SNBL
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0667901000
_diffrn_orient_matrix_UB_12      -0.0037701000
_diffrn_orient_matrix_UB_13      -0.0133387000
_diffrn_orient_matrix_UB_21      0.0459235000
_diffrn_orient_matrix_UB_22      0.0517699000
_diffrn_orient_matrix_UB_23      0.0621689000
_diffrn_orient_matrix_UB_31      0.0110023000
_diffrn_orient_matrix_UB_32      -0.0516218000
_diffrn_orient_matrix_UB_33      0.0408499000
_diffrn_radiation_monochromator  'Si (111)'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           ?
_diffrn_radiation_wavelength     0.78405
_diffrn_source                   
'European Synchrotron Radiation Facility, BM01 beamline'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3300
_reflns_number_total             3473
_reflns_odcompleteness_completeness 62.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     29.34
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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    'XT (Sheldrick, 2015)'
_refine_diff_density_max         5.369
_refine_diff_density_min         -1.523
_refine_diff_density_rms         0.248
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     292
_refine_ls_number_reflns         3473
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.0629
_refine_ls_R_factor_gt           0.0614
_refine_ls_restrained_S_all      6.399
_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)+(0.1424P)²+1.8371P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1632
_refine_ls_wR_factor_ref         0.1656
_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
 C17-C13 \\sim C13-C18
 with sigma of 0.02
 C12_$6-O1 \\sim O1-C11
 with sigma of 0.05
3. Restrained planarity
 C13, C17, C18, N2, O11
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C17) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
5.a Me refined with riding coordinates:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C)
5.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C8(H8), C12(H12), C13(H13), C16(H16)
5.c Tetrahedral OH refined with riding coordinates:
 O1(H1), O12(H12A)
5.d Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C15(H15A,H15B,H15C)
5.e Idealised tetrahedral OH refined as rotating group:
 O9(H9)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
C1 C -0.0211(7) 0.1212(7) 0.4962(8) 0.035(2) Uani 1 1 d . . . . .
C2 C 0.2047(7) 0.4847(7) 0.4294(8) 0.0317(19) Uani 1 1 d . . . . .
C3 C 0.3573(7) 0.4944(8) 0.4653(8) 0.039(2) Uani 1 1 d . . . . .
C4 C -0.0368(7) 0.2515(7) 0.4995(8) 0.035(2) Uani 1 1 d . . . . .
C5 C 0.4498(8) 0.5359(9) 0.5941(8) 0.043(2) Uani 1 1 d . . . . .
H5 H 0.415897 0.560446 0.657763 0.052 Uiso 1 1 calc R . . . .
C6 C 0.5930(8) 0.5418(9) 0.6309(8) 0.041(2) Uani 1 1 d . . . . .
C7 C 0.3017(7) 0.7608(8) 0.8602(8) 0.034(2) Uani 1 1 d . . . . .
C8 C 0.0043(9) 0.0745(8) 0.6099(8) 0.039(2) Uani 1 1 d . . . . .
H8 H 0.007519 0.125461 0.684842 0.047 Uiso 1 1 calc R . . . .
C9 C 0.0249(8) -0.0448(8) 0.6154(7) 0.035(2) Uani 1 1 d . . . . .
C10 C 0.0495(10) 0.1775(11) 0.9917(10) 0.053(3) Uani 1 1 d . . . . .
H10A H 0.007675 0.173536 1.055885 0.079 Uiso 1 1 calc GR . . . .
H10B H 0.150664 0.190694 1.034490 0.079 Uiso 1 1 calc GR . . . .
H10C H 0.009919 0.098972 0.927355 0.079 Uiso 1 1 calc GR . . . .
C11 C 0.4020(7) 0.8863(8) 0.9318(8) 0.039(2) Uani 1 1 d D . . . .
C12 C 0.3629(8) 0.9705(9) 0.9954(10) 0.052(3) Uani 1 1 d D . . . .
H12 H 0.271759 0.951113 0.995551 0.063 Uiso 1 1 calc R . . A 2
C13 C 0.3105(10) 0.3282(10) 0.7236(11) 0.066(3) Uani 1 1 d D . . . .
H13 H 0.241525 0.277732 0.644853 0.079 Uiso 1 1 calc R . . . .
C14 C 0.5429(8) 0.9104(9) 0.9367(9) 0.046(2) Uani 1 1 d . . . . .
C15 C -0.1279(10) 0.2752(14) 0.8582(12) 0.066(3) Uani 1 1 d . . . . .
H15A H -0.168021 0.301115 0.919523 0.099 Uiso 1 1 calc GR . . . .
H15B H -0.179393 0.189846 0.810141 0.099 Uiso 1 1 calc GR . . . .
H15C H -0.134612 0.331759 0.798021 0.099 Uiso 1 1 calc GR . . . .
C16 C 0.1174(10) 0.3706(11) 0.9358(9) 0.047(3) Uani 1 1 d . . . . .
H16 H 0.210963 0.369224 0.982679 0.056 Uiso 1 1 calc R . . . .
C17 C 0.436(2) 0.1749(17) 0.709(2) 0.119(7) Uani 1 1 d D U . . .
H17A H 0.526185 0.159899 0.758091 0.178 Uiso 1 1 calc R . . . .
H17B H 0.360439 0.104924 0.701918 0.178 Uiso 1 1 calc R . . . .
H17C H 0.431082 0.182729 0.621967 0.178 Uiso 1 1 calc R . . . .
C18 C 0.5325(13) 0.3687(19) 0.8976(14) 0.094(5) Uani 1 1 d D . . . .
H18A H 0.610292 0.329667 0.923579 0.141 Uiso 1 1 calc R . . . .
H18B H 0.565898 0.453027 0.886111 0.141 Uiso 1 1 calc R . . . .
H18C H 0.494482 0.373624 0.964515 0.141 Uiso 1 1 calc R . . . .
N1 N 0.0206(8) 0.2794(8) 0.9292(7) 0.045(2) Uani 1 1 d . . . . .
N2 N 0.4229(10) 0.2935(10) 0.7755(10) 0.065(3) Uani 1 1 d . . . . .
O1 O 0.5932(7) 0.8200(8) 0.8808(9) 0.077(3) Uani 1 1 d D . . . .
H1 H 0.526636 0.757450 0.836862 0.116 Uiso 1 1 calc R . . . .
O2 O -0.0086(6) 0.3205(5) 0.6075(6) 0.0362(14) Uani 1 1 d . . . . .
O3 O 0.1595(5) 0.5048(5) 0.5181(6) 0.0401(15) Uani 1 1 d . . . . .
O4 O -0.0717(6) 0.2858(5) 0.3914(5) 0.0342(13) Uani 1 1 d . . . . .
O5 O 0.0978(7) 0.4642(7) 0.8836(6) 0.0502(19) Uani 1 1 d . . . . .
O6 O 0.1228(5) 0.4579(6) 0.3103(6) 0.0375(14) Uani 1 1 d . . . . .
O7 O 0.1854(5) 0.7307(5) 0.8715(5) 0.0358(13) Uani 1 1 d . . . . .
O8 O 0.3366(5) 0.6850(6) 0.7903(6) 0.0458(18) Uani 1 1 d . . . . .
O9 O 0.0473(8) -0.0807(6) 0.7305(7) 0.0492(17) Uani 1 1 d . . . . .
H9 H 0.058295 -0.153274 0.724051 0.074 Uiso 1 1 calc GR . . . .
O11 O 0.2866(6) 0.4236(7) 0.7702(7) 0.0533(18) Uani 1 1 d . . . . .
O12 O 0.6782(6) 0.5825(9) 0.7580(6) 0.061(2) Uani 1 1 d . . . . .
H12A H 0.760193 0.581334 0.767904 0.092 Uiso 1 1 calc R . . . .
Tb1 Tb 0.10679(3) 0.53548(3) 0.69977(3) 0.0291(2) 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
C1 C4 1.496(12) . ?
C1 C8 1.408(14) . ?
C1 C9 1.422(10) 2_556 ?
C2 C3 1.502(9) . ?
C2 O3 1.275(9) . ?
C2 O6 1.279(10) . ?
C3 C5 1.397(11) . ?
C3 C6 1.421(10) 2_666 ?
C4 O2 1.267(9) . ?
C4 O4 1.280(11) . ?
C5 H5 0.9500 . ?
C5 C6 1.413(10) . ?
C6 O12 1.362(10) . ?
C7 C11 1.509(10) . ?
C7 O7 1.270(9) . ?
C7 O8 1.287(9) . ?
C8 H8 0.9500 . ?
C8 C9 1.399(13) . ?
C9 O9 1.367(12) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C10 N1 1.440(16) . ?
C11 C12 1.335(11) . ?
C11 C14 1.447(10) . ?
C12 H12 0.9500 . ?
C12 C14 1.429(11) 2_677 ?
C13 H13 0.9500 . ?
C13 N2 1.289(15) . ?
C13 O11 1.243(12) . ?
C14 O1 1.417(10) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C15 N1 1.482(13) . ?
C16 H16 0.9500 . ?
C16 N1 1.271(14) . ?
C16 O5 1.280(14) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C17 N2 1.504(17) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C18 N2 1.471(16) . ?
O1 H1 0.8400 . ?
O2 Tb1 2.383(5) . ?
O3 Tb1 2.326(6) . ?
O4 Tb1 2.392(6) 2_566 ?
O5 Tb1 2.348(8) . ?
O6 Tb1 2.416(5) 2_566 ?
O7 Tb1 2.519(5) . ?
O8 Tb1 2.448(5) . ?
O9 H9 0.8400 . ?
O11 Tb1 2.440(7) . ?
O12 H12A 0.8400 . ?

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
C8 C1 C4 118.5(7) . . ?
C8 C1 C9 118.8(8) . 2_556 ?
C9 C1 C4 122.6(8) 2_556 . ?
O3 C2 C3 119.4(7) . . ?
O3 C2 O6 121.3(6) . . ?
O6 C2 C3 119.3(6) . . ?
C5 C3 C2 119.7(7) . . ?
C5 C3 C6 120.1(6) . 2_666 ?
C6 C3 C2 120.2(7) 2_666 . ?
O2 C4 C1 118.6(8) . . ?
O2 C4 O4 125.3(8) . . ?
O4 C4 C1 116.1(6) . . ?
C3 C5 H5 119.6 . . ?
C3 C5 C6 120.8(7) . . ?
C6 C5 H5 119.6 . . ?
C5 C6 C3 119.1(7) . 2_666 ?
O12 C6 C3 122.7(7) . 2_666 ?
O12 C6 C5 118.3(7) . . ?
O7 C7 C11 119.7(6) . . ?
O7 C7 O8 121.1(7) . . ?
O8 C7 C11 119.3(6) . . ?
C1 C8 H8 119.1 . . ?
C9 C8 C1 121.7(7) . . ?
C9 C8 H8 119.1 . . ?
C8 C9 C1 119.5(8) . 2_556 ?
O9 C9 C1 123.9(8) . 2_556 ?
O9 C9 C8 116.6(7) . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N1 C10 H10A 109.5 . . ?
N1 C10 H10B 109.5 . . ?
N1 C10 H10C 109.5 . . ?
C12 C11 C7 120.2(7) . . ?
C12 C11 C14 120.8(7) . . ?
C14 C11 C7 118.9(7) . . ?
C11 C12 H12 119.7 . . ?
C11 C12 C14 120.5(7) . 2_677 ?
C14 C12 H12 119.7 2_677 . ?
N2 C13 H13 117.9 . . ?
O11 C13 H13 117.9 . . ?
O11 C13 N2 124.2(10) . . ?
C12 C14 C11 118.5(7) 2_677 . ?
O1 C14 C11 123.1(7) . . ?
O1 C14 C12 118.4(7) . 2_677 ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N1 C15 H15A 109.5 . . ?
N1 C15 H15B 109.5 . . ?
N1 C15 H15C 109.5 . . ?
N1 C16 H16 117.7 . . ?
N1 C16 O5 124.6(10) . . ?
O5 C16 H16 117.7 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N2 C17 H17A 109.5 . . ?
N2 C17 H17B 109.5 . . ?
N2 C17 H17C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N2 C18 H18A 109.5 . . ?
N2 C18 H18B 109.5 . . ?
N2 C18 H18C 109.5 . . ?
C10 N1 C15 117.3(9) . . ?
C16 N1 C10 121.9(9) . . ?
C16 N1 C15 120.8(11) . . ?
C13 N2 C17 118.1(11) . . ?
C13 N2 C18 119.8(11) . . ?
C18 N2 C17 122.0(13) . . ?
C14 O1 H1 109.5 . . ?
C4 O2 Tb1 133.3(6) . . ?
C2 O3 Tb1 171.6(6) . . ?
C4 O4 Tb1 141.5(5) . 2_566 ?
C16 O5 Tb1 138.5(6) . . ?
C2 O6 Tb1 107.4(4) . 2_566 ?
C7 O7 Tb1 91.1(4) . . ?
C7 O8 Tb1 94.0(4) . . ?
C9 O9 H9 109.5 . . ?
C13 O11 Tb1 135.7(7) . . ?
C6 O12 H12A 109.5 . . ?
O2 Tb1 O4 129.0(2) . 2_566 ?
O2 Tb1 O6 81.95(19) . 2_566 ?
O2 Tb1 O7 153.5(2) . . ?
O2 Tb1 O8 142.80(19) . . ?
O2 Tb1 O11 74.4(2) . . ?
O3 Tb1 O2 78.1(2) . . ?
O3 Tb1 O4 75.6(2) . 2_566 ?
O3 Tb1 O5 147.4(3) . . ?
O3 Tb1 O6 123.2(2) . 2_566 ?
O3 Tb1 O7 128.3(2) . . ?
O3 Tb1 O8 82.9(2) . . ?
O3 Tb1 O11 79.0(2) . . ?
O4 Tb1 O6 77.3(2) 2_566 2_566 ?
O4 Tb1 O7 68.32(19) 2_566 . ?
O4 Tb1 O8 75.0(2) 2_566 . ?
O4 Tb1 O11 139.3(2) 2_566 . ?
O5 Tb1 O2 79.8(2) . . ?
O5 Tb1 O4 136.9(2) . 2_566 ?
O5 Tb1 O6 76.5(2) . 2_566 ?
O5 Tb1 O7 75.2(2) . . ?
O5 Tb1 O8 101.1(2) . . ?
O5 Tb1 O11 72.1(3) . . ?
O6 Tb1 O7 83.57(18) 2_566 . ?
O6 Tb1 O8 134.84(19) 2_566 . ?
O6 Tb1 O11 143.3(2) 2_566 . ?
O8 Tb1 O7 53.24(18) . . ?
O11 Tb1 O7 105.8(2) . . ?
O11 Tb1 O8 70.8(2) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O1 H1 O8 0.84 1.87 2.600(8) 144.5 . yes
O9 H9 O4 0.84 1.92 2.637(8) 143.0 2_556 yes
O12 H12A O6 0.84 1.85 2.594(8) 146.4 2_666 yes

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
C1 C4 O2 Tb1 139.8(6) . . . . ?
C1 C4 O4 Tb1 -174.9(5) . . . 2_566 ?
C1 C8 C9 C1 0.4(13) . . . 2_556 ?
C1 C8 C9 O9 -179.3(7) . . . . ?
C2 C3 C5 C6 177.8(9) . . . . ?
C3 C2 O6 Tb1 -176.8(6) . . . 2_566 ?
C3 C5 C6 C3 0.4(18) . . . 2_666 ?
C3 C5 C6 O12 -179.8(10) . . . . ?
C4 C1 C8 C9 -177.7(7) . . . . ?
C6 C3 C5 C6 -0.4(18) 2_666 . . . ?
C7 C11 C12 C14 -179.9(10) . . . 2_677 ?
C7 C11 C14 C12 179.9(10) . . . 2_677 ?
C7 C11 C14 O1 -2.1(16) . . . . ?
C8 C1 C4 O2 9.1(10) . . . . ?
C8 C1 C4 O4 -174.2(7) . . . . ?
C9 C1 C4 O2 -168.1(7) 2_556 . . . ?
C9 C1 C4 O4 8.6(10) 2_556 . . . ?
C9 C1 C8 C9 -0.4(13) 2_556 . . . ?
C11 C7 O7 Tb1 173.0(8) . . . . ?
C11 C7 O8 Tb1 -172.8(8) . . . . ?
C12 C11 C14 C12 -3.8(19) . . . 2_677 ?
C12 C11 C14 O1 174.1(11) . . . . ?
C14 C11 C12 C14 3.9(19) . . . 2_677 ?
N1 C16 O5 Tb1 -101.3(12) . . . . ?
N2 C13 O11 Tb1 172.6(8) . . . . ?
O2 C4 O4 Tb1 1.6(13) . . . 2_566 ?
O3 C2 C3 C5 -5.6(13) . . . . ?
O3 C2 C3 C6 172.6(9) . . . 2_666 ?
O3 C2 O6 Tb1 2.4(10) . . . 2_566 ?
O4 C4 O2 Tb1 -36.6(11) . . . . ?
O5 C16 N1 C10 -179.1(9) . . . . ?
O5 C16 N1 C15 -0.2(14) . . . . ?
O6 C2 C3 C5 173.6(9) . . . . ?
O6 C2 C3 C6 -8.2(13) . . . 2_666 ?
O7 C7 C11 C12 -7.2(15) . . . . ?
O7 C7 C11 C14 169.0(9) . . . . ?
O7 C7 O8 Tb1 8.4(10) . . . . ?
O8 C7 C11 C12 174.0(10) . . . . ?
O8 C7 C11 C14 -9.8(14) . . . . ?
O8 C7 O7 Tb1 -8.2(9) . . . . ?
O11 C13 N2 C17 179.3(10) . . . . ?
O11 C13 N2 C18 0.1(16) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.500 0.000 0.500 211.6 7.5 ?


_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 1.271
_oxdiff_exptl_absorpt_empirical_full_min 0.612

# start Validation Reply Form
_vrf_PLAT027_SION2_100K_cool     
;
PROBLEM: _diffrn_reflns_theta_full value (too) Low ......      26.00 Degree
RESPONSE: Our value of max sin(theta)/lambda of 0.56 is close to the recommended 
		  value of 0.60. Higer values of sin(theta)/lambda were not available due 
		  to the beamline experimental set-up limitations. 
;
_vrf_PLAT029_SION2_100K_cool     
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.715 Why?  
RESPONSE: The data were collected upon the spindle rotation. Therefore, a 
		  limited portion of the reciprocal space could be probed.
;
# 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_SION2_360K
_database_code_depnum_ccdc_archive 'CCDC 1871314'
loop_
_audit_author_name
_audit_author_address
'Andrzej Gladysiak'
;Ecole polytechnique federale de Lausanne
Switzerland
;
_audit_update_record             
;
2019-05-29 deposited with the CCDC.	2019-08-12 downloaded from the CCDC.
;
_audit_creation_date             2019-05-29
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C18 H20 N2 O11 Tb'
_chemical_formula_sum            'C19.01 H22.36 N2.34 O11.34 Tb'
_chemical_formula_weight         623.95
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C21 H27 N3 O12 Tb'
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                   10.6610(13)
_cell_length_b                   11.0866(11)
_cell_length_c                   13.1016(15)
_cell_angle_alpha                100.439(10)
_cell_angle_beta                 112.923(12)
_cell_angle_gamma                98.339(9)
_cell_volume                     1362.3(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3370
_cell_measurement_temperature    360.0
_cell_measurement_theta_max      30.7490
_cell_measurement_theta_min      1.9090
_shelx_estimated_absorpt_T_max   0.836
_shelx_estimated_absorpt_T_min   0.619
_exptl_absorpt_coefficient_mu    2.649
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38720
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.521
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             617
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0612
_diffrn_reflns_av_unetI/netI     0.0743
_diffrn_reflns_Laue_measured_fraction_full 0.764
_diffrn_reflns_Laue_measured_fraction_max 0.752
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            7880
_diffrn_reflns_point_group_measured_fraction_full 0.764
_diffrn_reflns_point_group_measured_fraction_max 0.752
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.510
_diffrn_reflns_theta_min         1.932
_diffrn_ambient_temperature      360.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            PILATUS2M
_diffrn_measured_fraction_theta_full 0.764
_diffrn_measured_fraction_theta_max 0.752
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      0.00 360.00   1.00    1.00    --    0.00   0.00   0.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  PILATUS@SNBL
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0658365000
_diffrn_orient_matrix_UB_12      -0.0149533000
_diffrn_orient_matrix_UB_13      0.0280517000
_diffrn_orient_matrix_UB_21      -0.0315550000
_diffrn_orient_matrix_UB_22      -0.0653357000
_diffrn_orient_matrix_UB_23      -0.0282740000
_diffrn_orient_matrix_UB_31      0.0166758000
_diffrn_orient_matrix_UB_32      0.0074971000
_diffrn_orient_matrix_UB_33      -0.0466090000
_diffrn_radiation_monochromator  'Si (111)'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7142
_diffrn_source                   
'European Synchrotron Radiation Facility, BM01 beamline'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3210
_reflns_number_total             4198
_reflns_odcompleteness_completeness 75.27
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.51
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (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    'XT (Sheldrick, 2015)'
_refine_diff_density_max         4.370
_refine_diff_density_min         -2.979
_refine_diff_density_rms         0.265
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         4198
_refine_ls_number_restraints     146
_refine_ls_R_factor_all          0.1130
_refine_ls_R_factor_gt           0.0996
_refine_ls_restrained_S_all      1.095
_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)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2571
_refine_ls_wR_factor_ref         0.2788
_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
 O11-C13
 1.21 with sigma of 0.02
 O5-C10
 1.21 with sigma of 0.02
 C10-N1
 1.4 with sigma of 0.02
 C13-N2
 1.4 with sigma of 0.02
 N1-C16
 1.45 with sigma of 0.02
 N1-C15
 1.45 with sigma of 0.02
 N2-C17
 1.45 with sigma of 0.02
 N2-C18
 1.45 with sigma of 0.02
 C17-C13 \\sim C13-C18
 with sigma of 0.02
3. Restrained planarity
 O11, C13, N2, C17, C18
 with sigma of 0.1
4. Rigid bond restraints
 O3, C2
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.005
 C2, O3
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.005
 O3, C2, O6
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Uiso/Uaniso restraints and constraints
O3 \\sim C2: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.01
C13 \\sim N2 \\sim C18 \\sim C17: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002
C10 \\sim N1 \\sim C16 \\sim C15: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002
C2 \\sim O3: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.01
C2 \\sim O6: within 2A with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(O1B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C15) \\sim Ueq, Uanis(C16) \\sim Ueq: with sigma of 0.025 and sigma for
terminal atoms of 0.05
Uanis(C17) \\sim Ueq, Uanis(C18) \\sim Ueq: with sigma of 0.025 and sigma for
terminal atoms of 0.05
Uanis(O9) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
6. Rigid body (RIGU) restrains
 O11, C13, N2, C18, C17
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O5, C10, N1, C16, C15
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 Sof(O1B)=Sof(H1B)=Sof(H12A)=1-FVAR(1)
 Sof(O1A)=Sof(H1A)=Sof(H14)=FVAR(1)
8.a Me refined with riding coordinates:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,
 H18C)
8.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C8(H8), C10(H10), C12(H12A), C13(H13), C14(H14)
8.c Tetrahedral OH refined with riding coordinates:
 O9(H9), O12(H12), O1A(H1A), O1B(H1B)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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 0.11381(5) 0.54265(5) 0.68144(5) 0.0592(4) Uani 1 1 d . . . . .
O2 O -0.0042(12) 0.3313(9) 0.5881(10) 0.077(3) Uani 1 1 d . . . . .
O3 O 0.1700(10) 0.5013(11) 0.5290(10) 0.0781(19) Uani 1 1 d . U . . .
O4 O -0.0728(12) 0.2813(10) 0.3996(9) 0.080(3) Uani 1 1 d . . . . .
O5 O 0.0855(14) 0.4623(13) 0.8341(10) 0.097(3) Uani 1 1 d D U . . .
O6 O 0.1154(10) 0.4480(10) 0.3431(10) 0.079(2) Uani 1 1 d . U . . .
O7 O 0.1844(11) 0.7342(11) 0.8432(9) 0.079(3) Uani 1 1 d . . . . .
O8 O 0.3428(12) 0.6928(11) 0.7841(11) 0.092(4) Uani 1 1 d . . . . .
O9 O 0.0525(18) -0.0610(14) 0.7057(12) 0.115(5) Uani 1 1 d . U . . .
H9 H 0.039444 -0.137707 0.696527 0.172 Uiso 1 1 calc R . . . .
O11 O 0.2879(14) 0.4246(15) 0.7485(13) 0.113(5) Uani 1 1 d D U . . .
O12 O 0.6877(12) 0.5948(17) 0.7262(11) 0.105(5) Uani 1 1 d . . . . .
H12 H 0.767857 0.594054 0.734454 0.158 Uiso 1 1 calc R . . . .
N1 N 0.019(3) 0.300(3) 0.892(3) 0.174(6) Uani 1 1 d D U . . .
O1A O 0.2348(17) 0.9559(17) 0.9881(18) 0.116(8) Uani 0.79(3) 1 d . . P A 1
H1A H 0.186209 0.886886 0.945162 0.173 Uiso 0.79(3) 1 calc R . P A 1
O1B O 0.596(5) 0.824(5) 0.899(5) 0.077(18) Uani 0.21(3) 1 d . U P A 2
H1B H 0.533000 0.761516 0.858049 0.115 Uiso 0.21(3) 1 calc R . P A 2
N2 N 0.463(2) 0.332(3) 0.830(2) 0.197(6) Uani 1 1 d D U . . .
C1 C -0.0175(15) 0.1210(13) 0.4926(12) 0.068(4) Uani 1 1 d . . . . .
C2 C 0.2075(15) 0.4794(16) 0.4486(16) 0.0779(19) Uani 1 1 d . U . . .
C3 C 0.3581(14) 0.4917(13) 0.4727(13) 0.065(3) Uani 1 1 d . . . . .
C4 C -0.0309(14) 0.2557(13) 0.4905(14) 0.068(4) Uani 1 1 d . . . . .
C5 C 0.4576(14) 0.5345(16) 0.5876(14) 0.073(4) Uani 1 1 d . . . . .
H5 H 0.428011 0.553178 0.645442 0.087 Uiso 1 1 calc R . . . .
C6 C 0.6000(14) 0.5494(17) 0.6161(14) 0.073(4) Uani 1 1 d . . . . .
C7 C 0.3053(15) 0.7642(17) 0.8405(16) 0.082(5) Uani 1 1 d . . . . .
C8 C 0.0109(18) 0.0821(16) 0.5920(14) 0.077(4) Uani 1 1 d . . . . .
H8 H 0.017004 0.139192 0.656156 0.092 Uiso 1 1 calc R . . . .
C9 C 0.0303(16) -0.0329(14) 0.6017(13) 0.070(4) Uani 1 1 d . . . . .
C10 C -0.009(3) 0.379(3) 0.823(3) 0.174(6) Uani 1 1 d D U . . .
H10 H -0.099371 0.369453 0.767535 0.208 Uiso 1 1 calc R . . . .
C11 C 0.4005(14) 0.8910(15) 0.9245(13) 0.074(4) Uani 1 1 d . . . . .
C12 C 0.3620(15) 0.9731(14) 0.9879(14) 0.067(4) Uani 1 1 d . . . . .
H12A H 0.270841 0.954677 0.981349 0.081 Uiso 0.21(3) 1 calc R . P A 2
C13 C 0.398(2) 0.423(3) 0.802(2) 0.197(6) Uani 1 1 d D U . . .
H13 H 0.458262 0.503209 0.833170 0.237 Uiso 1 1 calc R . . . .
C14 C 0.5438(15) 0.9127(16) 0.9352(14) 0.077(4) Uani 1 1 d . . . . .
H14 H 0.572138 0.854310 0.893561 0.092 Uiso 0.79(3) 1 calc R . P A 1
C15 C -0.089(3) 0.192(3) 0.876(3) 0.175(6) Uani 1 1 d D U . . .
H15A H -0.050790 0.146742 0.932304 0.262 Uiso 1 1 calc R . . . .
H15B H -0.165694 0.221368 0.885000 0.262 Uiso 1 1 calc R . . . .
H15C H -0.122465 0.137092 0.800531 0.262 Uiso 1 1 calc R . . . .
C16 C 0.165(3) 0.298(4) 0.956(3) 0.175(6) Uani 1 1 d D U . . .
H16A H 0.168771 0.237453 1.001255 0.263 Uiso 1 1 calc R . . . .
H16B H 0.205112 0.273903 0.904130 0.263 Uiso 1 1 calc R . . . .
H16C H 0.216024 0.379920 1.006366 0.263 Uiso 1 1 calc R . . . .
C17 C 0.391(3) 0.201(3) 0.790(3) 0.199(7) Uani 1 1 d D U . . .
H17A H 0.456286 0.151257 0.819741 0.298 Uiso 1 1 calc R . . . .
H17B H 0.318198 0.188523 0.815112 0.298 Uiso 1 1 calc R . . . .
H17C H 0.350720 0.176147 0.707343 0.298 Uiso 1 1 calc R . . . .
C18 C 0.614(2) 0.371(4) 0.908(3) 0.198(7) Uani 1 1 d D U . . .
H18A H 0.649005 0.297802 0.922497 0.297 Uiso 1 1 calc R . . . .
H18B H 0.664049 0.415850 0.874183 0.297 Uiso 1 1 calc R . . . .
H18C H 0.627367 0.425250 0.979748 0.297 Uiso 1 1 calc R . . . .


_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 2.341(10) . ?
Tb1 O3 2.288(12) . ?
Tb1 O4 2.401(10) 2_566 ?
Tb1 O5 2.433(13) . ?
Tb1 O6 2.358(10) 2_566 ?
Tb1 O7 2.496(11) . ?
Tb1 O8 2.447(12) . ?
Tb1 O11 2.404(13) . ?
O2 C4 1.29(2) . ?
O3 C2 1.26(2) . ?
O4 C4 1.201(18) . ?
O5 C10 1.205(17) . ?
O6 C2 1.291(19) . ?
O7 C7 1.30(2) . ?
O8 C7 1.20(2) . ?
O9 H9 0.8200 . ?
O9 C9 1.39(2) . ?
O11 C13 1.112(16) . ?
O12 H12 0.8200 . ?
O12 C6 1.33(2) . ?
N1 C10 1.355(18) . ?
N1 C15 1.457(18) . ?
N1 C16 1.457(18) . ?
O1A H1A 0.8200 . ?
O1A C12 1.34(2) . ?
O1B H1B 0.8200 . ?
O1B C14 1.30(6) . ?
N2 C13 1.334(18) . ?
N2 C17 1.431(19) . ?
N2 C18 1.481(18) . ?
C1 C4 1.524(18) . ?
C1 C8 1.38(2) . ?
C1 C9 1.38(2) 2_556 ?
C2 C3 1.49(2) . ?
C3 C5 1.40(2) . ?
C3 C6 1.43(2) 2_666 ?
C5 H5 0.9300 . ?
C5 C6 1.391(19) . ?
C7 C11 1.54(2) . ?
C8 H8 0.9300 . ?
C8 C9 1.34(2) . ?
C10 H10 0.9300 . ?
C11 C12 1.34(2) . ?
C11 C14 1.46(2) . ?
C12 H12A 0.9300 . ?
C12 C14 1.42(2) 2_677 ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?

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 125.5(3) . 2_566 ?
O2 Tb1 O5 77.4(4) . . ?
O2 Tb1 O6 79.8(4) . 2_566 ?
O2 Tb1 O7 150.9(4) . . ?
O2 Tb1 O8 145.5(4) . . ?
O2 Tb1 O11 75.1(5) . . ?
O3 Tb1 O2 76.6(4) . . ?
O3 Tb1 O4 76.4(4) . 2_566 ?
O3 Tb1 O5 145.1(5) . . ?
O3 Tb1 O6 122.0(4) . 2_566 ?
O3 Tb1 O7 132.4(4) . . ?
O3 Tb1 O8 86.6(4) . . ?
O3 Tb1 O11 79.2(5) . . ?
O4 Tb1 O5 138.3(5) 2_566 . ?
O4 Tb1 O7 72.3(4) 2_566 . ?
O4 Tb1 O8 77.7(4) 2_566 . ?
O4 Tb1 O11 142.1(5) 2_566 . ?
O5 Tb1 O7 75.3(4) . . ?
O5 Tb1 O8 102.3(5) . . ?
O6 Tb1 O4 75.9(4) 2_566 2_566 ?
O6 Tb1 O5 75.2(4) 2_566 . ?
O6 Tb1 O7 83.8(4) 2_566 . ?
O6 Tb1 O8 134.1(4) 2_566 . ?
O6 Tb1 O11 142.0(5) 2_566 . ?
O8 Tb1 O7 52.4(4) . . ?
O11 Tb1 O5 71.9(5) . . ?
O11 Tb1 O7 105.2(5) . . ?
O11 Tb1 O8 72.2(5) . . ?
C4 O2 Tb1 135.1(10) . . ?
C2 O3 Tb1 177.0(10) . . ?
C4 O4 Tb1 141.1(10) . 2_566 ?
C10 O5 Tb1 126.3(18) . . ?
C2 O6 Tb1 114.6(10) . 2_566 ?
C7 O7 Tb1 90.0(10) . . ?
C7 O8 Tb1 94.8(10) . . ?
C9 O9 H9 109.5 . . ?
C13 O11 Tb1 149(2) . . ?
C6 O12 H12 109.5 . . ?
C10 N1 C15 121(2) . . ?
C10 N1 C16 118(2) . . ?
C16 N1 C15 118(3) . . ?
C12 O1A H1A 109.5 . . ?
C14 O1B H1B 109.5 . . ?
C13 N2 C17 122.7(18) . . ?
C13 N2 C18 117.0(17) . . ?
C17 N2 C18 120(3) . . ?
C8 C1 C4 120.8(14) . . ?
C9 C1 C4 122.8(13) 2_556 . ?
C9 C1 C8 116.4(13) 2_556 . ?
O3 C2 O6 120.2(13) . . ?
O3 C2 C3 121.2(14) . . ?
O6 C2 C3 118.6(16) . . ?
C5 C3 C2 117.8(14) . . ?
C5 C3 C6 120.4(12) . 2_666 ?
C6 C3 C2 121.5(13) 2_666 . ?
O2 C4 C1 115.9(13) . . ?
O4 C4 O2 125.4(13) . . ?
O4 C4 C1 118.6(14) . . ?
C3 C5 H5 119.6 . . ?
C6 C5 C3 120.8(15) . . ?
C6 C5 H5 119.6 . . ?
O12 C6 C3 124.2(13) . 2_666 ?
O12 C6 C5 117.2(15) . . ?
C5 C6 C3 118.5(13) . 2_666 ?
O7 C7 C11 114.5(18) . . ?
O8 C7 O7 121.8(15) . . ?
O8 C7 C11 123.4(16) . . ?
C1 C8 H8 117.9 . . ?
C9 C8 C1 124.1(15) . . ?
C9 C8 H8 117.9 . . ?
C1 C9 O9 122.4(13) 2_556 . ?
C8 C9 O9 118.0(15) . . ?
C8 C9 C1 119.4(13) . 2_556 ?
O5 C10 N1 119(2) . . ?
O5 C10 H10 120.5 . . ?
N1 C10 H10 120.5 . . ?
C12 C11 C7 125.0(15) . . ?
C12 C11 C14 121.2(14) . . ?
C14 C11 C7 113.7(16) . . ?
O1A C12 C14 113.5(16) . 2_677 ?
C11 C12 O1A 124.7(15) . . ?
C11 C12 H12A 119.1 . . ?
C11 C12 C14 121.9(14) . 2_677 ?
C14 C12 H12A 119.1 2_677 . ?
O11 C13 N2 134(2) . . ?
O11 C13 H13 113.0 . . ?
N2 C13 H13 113.0 . . ?
O1B C14 C11 123(3) . . ?
C11 C14 H14 121.6 . . ?
C12 C14 C11 116.9(16) 2_677 . ?
C12 C14 H14 121.6 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 . . ?

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 -45(2) . . . . ?
Tb1 O2 C4 C1 139.4(11) . . . . ?
Tb1 O4 C4 O2 9(3) 2_566 . . . ?
Tb1 O4 C4 C1 -175.9(11) 2_566 . . . ?
Tb1 O5 C10 N1 145(3) . . . . ?
Tb1 O6 C2 O3 6(2) 2_566 . . . ?
Tb1 O6 C2 C3 -172.6(10) 2_566 . . . ?
Tb1 O7 C7 O8 -10.0(19) . . . . ?
Tb1 O7 C7 C11 176.1(13) . . . . ?
Tb1 O8 C7 O7 10.3(19) . . . . ?
Tb1 O8 C7 C11 -176.5(15) . . . . ?
Tb1 O11 C13 N2 172(2) . . . . ?
O3 C2 C3 C5 -3(2) . . . . ?
O3 C2 C3 C6 171.2(16) . . . 2_666 ?
O6 C2 C3 C5 175.6(15) . . . . ?
O6 C2 C3 C6 -10(2) . . . 2_666 ?
O7 C7 C11 C12 -7(2) . . . . ?
O7 C7 C11 C14 169.8(14) . . . . ?
O8 C7 C11 C12 179.5(17) . . . . ?
O8 C7 C11 C14 -4(3) . . . . ?
C1 C8 C9 O9 -177.4(15) . . . . ?
C1 C8 C9 C1 -2(3) . . . 2_556 ?
C2 C3 C5 C6 -179.3(15) . . . . ?
C3 C5 C6 O12 177.5(17) . . . . ?
C3 C5 C6 C3 -6(3) . . . 2_666 ?
C4 C1 C8 C9 -176.9(15) . . . . ?
C6 C3 C5 C6 6(3) 2_666 . . . ?
C7 C11 C12 O1A 1(3) . . . . ?
C7 C11 C12 C14 179.1(14) . . . 2_677 ?
C7 C11 C14 O1B -15(4) . . . . ?
C7 C11 C14 C12 -179.3(13) . . . 2_677 ?
C8 C1 C4 O2 5(2) . . . . ?
C8 C1 C4 O4 -170.8(16) . . . . ?
C9 C1 C4 O2 -174.1(15) 2_556 . . . ?
C9 C1 C4 O4 10(2) 2_556 . . . ?
C9 C1 C8 C9 2(3) 2_556 . . . ?
C12 C11 C14 O1B 162(3) . . . . ?
C12 C11 C14 C12 -3(3) . . . 2_677 ?
C14 C11 C12 O1A -175.7(17) . . . . ?
C14 C11 C12 C14 3(3) . . . 2_677 ?
C15 N1 C10 O5 -176(4) . . . . ?
C16 N1 C10 O5 -15(6) . . . . ?
C17 N2 C13 O11 1(4) . . . . ?
C18 N2 C13 O11 -178(3) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.028 0.000 -0.028 364.6 27.1 ?


_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 2.193
_oxdiff_exptl_absorpt_empirical_full_min 0.543

# start Validation Reply Form
_vrf_PLAT029_SION2_360K          
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.764 Why?  
RESPONSE: The data were collected upon the spindle rotation. Therefore, a 
		  limited portion of the reciprocal space could be probed.
;
# 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_SION2_380K
_database_code_depnum_ccdc_archive 'CCDC 1871316'
loop_
_audit_author_name
_audit_author_address
'Andrzej Gladysiak'
;Ecole polytechnique federale de Lausanne
Switzerland
;
_audit_update_record             
;
2019-05-29 deposited with the CCDC.	2019-08-12 downloaded from the CCDC.
;
_audit_creation_date             2019-05-29
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C18 H20 N2 O11 Tb'
_chemical_formula_sum            'C18 H20 N2 O11 Tb'
_chemical_formula_weight         599.28
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C21 H27 N3 O12 Tb'
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                   10.6786(15)
_cell_length_b                   11.0643(14)
_cell_length_c                   13.078(3)
_cell_angle_alpha                98.788(14)
_cell_angle_beta                 113.593(18)
_cell_angle_gamma                99.692(11)
_cell_volume                     1353.7(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2347
_cell_measurement_temperature    380.0
_cell_measurement_theta_max      25.7430
_cell_measurement_theta_min      1.9210
_shelx_estimated_absorpt_T_max   0.836
_shelx_estimated_absorpt_T_min   0.618
_exptl_absorpt_coefficient_mu    2.662
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.28610
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.470
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             590
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0583
_diffrn_reflns_av_unetI/netI     0.0961
_diffrn_reflns_Laue_measured_fraction_full 0.733
_diffrn_reflns_Laue_measured_fraction_max 0.722
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            7717
_diffrn_reflns_point_group_measured_fraction_full 0.733
_diffrn_reflns_point_group_measured_fraction_max 0.722
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.511
_diffrn_reflns_theta_min         1.935
_diffrn_ambient_temperature      380.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            PILATUS2M
_diffrn_measured_fraction_theta_full 0.733
_diffrn_measured_fraction_theta_max 0.722
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      0.00 360.00   1.00    1.00    --    0.00   0.00   0.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  PILATUS@SNBL
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0673581000
_diffrn_orient_matrix_UB_12      -0.0130799000
_diffrn_orient_matrix_UB_13      0.0268784000
_diffrn_orient_matrix_UB_21      -0.0315185000
_diffrn_orient_matrix_UB_22      -0.0657871000
_diffrn_orient_matrix_UB_23      -0.0264320000
_diffrn_orient_matrix_UB_31      0.0127053000
_diffrn_orient_matrix_UB_32      0.0077512000
_diffrn_orient_matrix_UB_33      -0.0485231000
_diffrn_radiation_monochromator  'Si (111)'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7142
_diffrn_source                   
'European Synchrotron Radiation Facility, BM01 beamline'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2987
_reflns_number_total             3995
_reflns_odcompleteness_completeness 72.20
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.51
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (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    'XT (Sheldrick, 2015)'
_refine_diff_density_max         2.882
_refine_diff_density_min         -3.132
_refine_diff_density_rms         0.302
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.189
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         3995
_refine_ls_number_restraints     159
_refine_ls_R_factor_all          0.1373
_refine_ls_R_factor_gt           0.1222
_refine_ls_restrained_S_all      1.180
_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)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2995
_refine_ls_wR_factor_ref         0.3150
_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
 O11-C13
 1.21 with sigma of 0.02
 O5-C10
 1.21 with sigma of 0.02
 C10-N1
 1.4 with sigma of 0.02
 C13-N2
 1.4 with sigma of 0.02
 N1-C16
 1.45 with sigma of 0.02
 N1-C15
 1.45 with sigma of 0.02
 N2-C17
 1.45 with sigma of 0.02
 N2-C18
 1.45 with sigma of 0.02
 O11-C13
 1.2 with sigma of 0.04
 O5-C10
 1.2 with sigma of 0.04
 C17-N2 \\sim N2-C18
 with sigma of 0.02
 C17-C13 \\sim C13-C18
 with sigma of 0.02
 C15-N1 \\sim N1-C16
 with sigma of 0.02
 C15-C10 \\sim C10-C16
 with sigma of 0.02
3. Restrained planarity
 O11, C13, N2, C17, C18
 with sigma of 0.1
 O5, C10, N1, C15, C16
 with sigma of 0.1
4. Rigid bond restraints
 O3, C2
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.005
 C2, O3
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.005
 O3, C2, O6
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Uiso/Uaniso restraints and constraints
O3 \\sim C2: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.01
C13 \\sim N2 \\sim C18 \\sim C17: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002
C10 \\sim N1 \\sim C16 \\sim C15: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002
C2 \\sim O3: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.01
C2 \\sim O6: within 2A with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(O1B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C15) \\sim Ueq, Uanis(C16) \\sim Ueq: with sigma of 0.025 and sigma for
terminal atoms of 0.05
Uanis(C17) \\sim Ueq, Uanis(C18) \\sim Ueq: with sigma of 0.025 and sigma for
terminal atoms of 0.05
Uanis(O9) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O8) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
6. Rigid body (RIGU) restrains
 O11, C13, N2, C18, C17
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O5, C10, N1, C16, C15
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 Sof(O1B)=Sof(H1B)=Sof(H12A)=1-FVAR(1)
 Sof(O1A)=Sof(H1A)=Sof(H14)=FVAR(1)
8.a Me refined with riding coordinates:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,
 H18C)
8.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C8(H8), C10(H10), C12(H12A), C13(H13), C14(H14)
8.c Tetrahedral OH refined with riding coordinates:
 O9(H9), O12(H12), O1A(H1A), O1B(H1B)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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 0.11600(6) 0.54046(6) 0.68175(6) 0.0764(5) Uani 1 1 d . . . . .
O2 O -0.0013(15) 0.3260(10) 0.5897(13) 0.099(4) Uani 1 1 d . . . . .
O3 O 0.1739(13) 0.5072(12) 0.5300(12) 0.093(2) Uani 1 1 d . U . . .
O4 O -0.0730(13) 0.2822(10) 0.3986(11) 0.089(3) Uani 1 1 d . . . . .
O5 O 0.0923(19) 0.4570(16) 0.8291(13) 0.121(5) Uani 1 1 d D U . . .
O6 O 0.1152(13) 0.4533(12) 0.3440(12) 0.094(2) Uani 1 1 d . U . . .
O7 O 0.1845(13) 0.7306(12) 0.8408(11) 0.095(4) Uani 1 1 d . . . . .
O8 O 0.3457(14) 0.6945(13) 0.7883(13) 0.097(4) Uani 1 1 d . U . . .
O9 O 0.056(2) -0.0644(17) 0.7053(15) 0.128(5) Uani 1 1 d . U . . .
H9 H 0.043177 -0.141173 0.697063 0.193 Uiso 1 1 calc R . . . .
O11 O 0.2951(18) 0.428(2) 0.7532(17) 0.137(6) Uani 1 1 d D U . . .
O12 O 0.6961(16) 0.585(2) 0.7289(15) 0.150(8) Uani 1 1 d . . . . .
H12 H 0.775525 0.583458 0.735545 0.225 Uiso 1 1 calc R . . . .
N1 N 0.022(3) 0.286(3) 0.895(3) 0.241(9) Uani 1 1 d D U . . .
O1A O 0.229(2) 0.942(3) 0.990(2) 0.120(11) Uani 0.62(4) 1 d . . P A 1
H1A H 0.180648 0.872487 0.946682 0.180 Uiso 0.62(4) 1 calc R . P A 1
O1B O 0.598(5) 0.833(5) 0.901(4) 0.124(18) Uani 0.38(4) 1 d . U P A 2
H1B H 0.534191 0.770095 0.860140 0.186 Uiso 0.38(4) 1 calc R . P A 2
N2 N 0.473(3) 0.329(4) 0.834(3) 0.258(9) Uani 1 1 d D U . . .
C1 C -0.0179(19) 0.1203(16) 0.4945(16) 0.087(5) Uani 1 1 d . . . . .
C2 C 0.206(2) 0.4865(18) 0.450(2) 0.093(2) Uani 1 1 d . U . . .
C3 C 0.3545(16) 0.4938(18) 0.4720(15) 0.080(4) Uani 1 1 d . . . . .
C4 C -0.0331(18) 0.2539(15) 0.4919(17) 0.080(4) Uani 1 1 d . . . . .
C5 C 0.4627(19) 0.540(2) 0.5908(17) 0.100(6) Uani 1 1 d . . . . .
H5 H 0.438779 0.565962 0.650039 0.120 Uiso 1 1 calc R . . . .
C6 C 0.5998(19) 0.543(2) 0.6131(18) 0.102(6) Uani 1 1 d . . . . .
C7 C 0.308(2) 0.7630(19) 0.8428(18) 0.093(5) Uani 1 1 d . . . . .
C8 C 0.011(2) 0.0797(19) 0.5954(16) 0.098(6) Uani 1 1 d . . . . .
H8 H 0.016887 0.132991 0.660233 0.118 Uiso 1 1 calc R . . . .
C9 C 0.031(2) -0.0348(17) 0.5989(16) 0.094(6) Uani 1 1 d . . . . .
C10 C 0.002(4) 0.373(3) 0.827(4) 0.241(9) Uani 1 1 d D U . . .
H10 H -0.089952 0.365036 0.773614 0.289 Uiso 1 1 calc R . . . .
C11 C 0.4023(18) 0.8884(18) 0.9249(17) 0.093(5) Uani 1 1 d . . . . .
C12 C 0.3655(19) 0.9672(18) 0.9875(18) 0.095(6) Uani 1 1 d . . . . .
H12A H 0.273453 0.944774 0.979280 0.114 Uiso 0.38(4) 1 calc R . P A 2
C13 C 0.411(3) 0.426(5) 0.808(3) 0.258(9) Uani 1 1 d D U . . .
H13 H 0.473605 0.505599 0.839865 0.309 Uiso 1 1 calc R . . . .
C14 C 0.5458(19) 0.917(2) 0.9339(18) 0.100(6) Uani 1 1 d . . . . .
H14 H 0.576057 0.863878 0.891609 0.119 Uiso 0.62(4) 1 calc R . P A 1
C15 C -0.094(5) 0.184(4) 0.874(4) 0.242(9) Uani 1 1 d D U . . .
H15A H -0.063139 0.133360 0.928044 0.363 Uiso 1 1 calc R . . . .
H15B H -0.167721 0.217514 0.882299 0.363 Uiso 1 1 calc R . . . .
H15C H -0.129420 0.132946 0.797158 0.363 Uiso 1 1 calc R . . . .
C16 C 0.163(5) 0.287(5) 0.972(4) 0.242(9) Uani 1 1 d D U . . .
H16A H 0.158874 0.222021 1.013152 0.363 Uiso 1 1 calc R . . . .
H16B H 0.215553 0.270865 0.929449 0.363 Uiso 1 1 calc R . . . .
H16C H 0.207898 0.367623 1.026386 0.363 Uiso 1 1 calc R . . . .
C17 C 0.385(5) 0.201(4) 0.788(5) 0.258(9) Uani 1 1 d D U . . .
H17A H 0.442958 0.143340 0.813665 0.387 Uiso 1 1 calc R . . . .
H17B H 0.313441 0.191358 0.814864 0.387 Uiso 1 1 calc R . . . .
H17C H 0.341957 0.181719 0.705626 0.387 Uiso 1 1 calc R . . . .
C18 C 0.623(3) 0.363(6) 0.911(5) 0.258(9) Uani 1 1 d D U . . .
H18A H 0.653549 0.286780 0.922915 0.387 Uiso 1 1 calc R . . . .
H18B H 0.675033 0.408767 0.878330 0.387 Uiso 1 1 calc R . . . .
H18C H 0.639650 0.413800 0.984012 0.387 Uiso 1 1 calc R . . . .


_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 2.360(11) . ?
Tb1 O3 2.301(15) . ?
Tb1 O4 2.391(12) 2_566 ?
Tb1 O5 2.342(17) . ?
Tb1 O6 2.369(12) 2_566 ?
Tb1 O7 2.493(13) . ?
Tb1 O8 2.448(13) . ?
Tb1 O11 2.407(17) . ?
O2 C4 1.28(2) . ?
O3 C2 1.22(2) . ?
O4 C4 1.23(2) . ?
O5 C10 1.207(17) . ?
O6 C2 1.28(2) . ?
O7 C7 1.30(3) . ?
O8 C7 1.19(3) . ?
O9 H9 0.8200 . ?
O9 C9 1.41(3) . ?
O11 C13 1.160(17) . ?
O12 H12 0.8200 . ?
O12 C6 1.39(3) . ?
N1 C10 1.397(19) . ?
N1 C15 1.431(16) . ?
N1 C16 1.433(16) . ?
O1A H1A 0.8200 . ?
O1A C12 1.45(3) . ?
O1B H1B 0.8200 . ?
O1B C14 1.26(5) . ?
N2 C13 1.367(19) . ?
N2 C17 1.450(16) . ?
N2 C18 1.459(16) . ?
C1 C4 1.52(2) . ?
C1 C8 1.39(3) . ?
C1 C9 1.37(3) 2_556 ?
C2 C3 1.48(2) . ?
C3 C5 1.46(2) . ?
C3 C6 1.42(3) 2_666 ?
C5 H5 0.9300 . ?
C5 C6 1.37(3) . ?
C7 C11 1.52(2) . ?
C8 H8 0.9300 . ?
C8 C9 1.32(3) . ?
C10 H10 0.9300 . ?
C11 C12 1.32(3) . ?
C11 C14 1.46(3) . ?
C12 H12A 0.9300 . ?
C12 C14 1.42(3) 2_677 ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?

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 126.5(4) . 2_566 ?
O2 Tb1 O6 80.8(5) . 2_566 ?
O2 Tb1 O7 150.9(5) . . ?
O2 Tb1 O8 145.4(5) . . ?
O2 Tb1 O11 75.5(7) . . ?
O3 Tb1 O2 77.5(5) . . ?
O3 Tb1 O4 76.5(5) . 2_566 ?
O3 Tb1 O5 144.9(5) . . ?
O3 Tb1 O6 122.4(5) . 2_566 ?
O3 Tb1 O7 131.5(4) . . ?
O3 Tb1 O8 87.0(5) . . ?
O3 Tb1 O11 79.6(6) . . ?
O4 Tb1 O7 71.1(4) 2_566 . ?
O4 Tb1 O8 78.0(4) 2_566 . ?
O4 Tb1 O11 141.9(6) 2_566 . ?
O5 Tb1 O2 76.8(6) . . ?
O5 Tb1 O4 138.4(6) . 2_566 ?
O5 Tb1 O6 76.1(6) . 2_566 ?
O5 Tb1 O7 76.1(5) . . ?
O5 Tb1 O8 101.2(6) . . ?
O5 Tb1 O11 71.1(6) . . ?
O6 Tb1 O4 75.1(5) 2_566 2_566 ?
O6 Tb1 O7 82.8(4) 2_566 . ?
O6 Tb1 O8 132.9(5) 2_566 . ?
O6 Tb1 O11 143.0(6) 2_566 . ?
O8 Tb1 O7 52.0(4) . . ?
O11 Tb1 O7 105.1(6) . . ?
O11 Tb1 O8 71.4(6) . . ?
C4 O2 Tb1 135.1(13) . . ?
C2 O3 Tb1 178.2(13) . . ?
C4 O4 Tb1 140.5(11) . 2_566 ?
C10 O5 Tb1 131(2) . . ?
C2 O6 Tb1 112.8(13) . 2_566 ?
C7 O7 Tb1 90.6(11) . . ?
C7 O8 Tb1 95.5(12) . . ?
C9 O9 H9 109.5 . . ?
C13 O11 Tb1 152(3) . . ?
C6 O12 H12 109.5 . . ?
C10 N1 C15 120(2) . . ?
C10 N1 C16 119(2) . . ?
C15 N1 C16 120(4) . . ?
C12 O1A H1A 109.5 . . ?
C14 O1B H1B 109.5 . . ?
C13 N2 C17 119(2) . . ?
C13 N2 C18 118(2) . . ?
C17 N2 C18 123(4) . . ?
C8 C1 C4 120.1(17) . . ?
C9 C1 C4 123.1(17) 2_556 . ?
C9 C1 C8 116.7(17) 2_556 . ?
O3 C2 O6 123.7(18) . . ?
O3 C2 C3 120.6(18) . . ?
O6 C2 C3 115.6(19) . . ?
C5 C3 C2 117.8(17) . . ?
C6 C3 C2 125.2(16) 2_666 . ?
C6 C3 C5 117.0(15) 2_666 . ?
O2 C4 C1 115.0(16) . . ?
O4 C4 O2 126.8(16) . . ?
O4 C4 C1 118.1(16) . . ?
C3 C5 H5 120.7 . . ?
C6 C5 C3 118.6(19) . . ?
C6 C5 H5 120.7 . . ?
O12 C6 C3 120.6(17) . 2_666 ?
C5 C6 O12 115(2) . . ?
C5 C6 C3 124.4(17) . 2_666 ?
O7 C7 C11 115(2) . . ?
O8 C7 O7 121.2(17) . . ?
O8 C7 C11 123(2) . . ?
C1 C8 H8 120.0 . . ?
C9 C8 C1 120.0(19) . . ?
C9 C8 H8 120.0 . . ?
C1 C9 O9 122.7(16) 2_556 . ?
C8 C9 O9 113.9(19) . . ?
C8 C9 C1 123.2(18) . 2_556 ?
O5 C10 N1 127(3) . . ?
O5 C10 H10 116.6 . . ?
N1 C10 H10 116.6 . . ?
C12 C11 C7 125.4(19) . . ?
C12 C11 C14 120.2(17) . . ?
C14 C11 C7 114(2) . . ?
C11 C12 O1A 123.7(18) . . ?
C11 C12 H12A 117.2 . . ?
C11 C12 C14 125.5(19) . 2_677 ?
C14 C12 O1A 110.7(19) 2_677 . ?
C14 C12 H12A 117.2 2_677 . ?
O11 C13 N2 133(3) . . ?
O11 C13 H13 113.7 . . ?
N2 C13 H13 113.7 . . ?
O1B C14 C11 122(3) . . ?
C11 C14 H14 122.9 . . ?
C12 C14 C11 114(2) 2_677 . ?
C12 C14 H14 122.9 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 . . ?

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 -39(3) . . . . ?
Tb1 O2 C4 C1 140.9(14) . . . . ?
Tb1 O4 C4 O2 3(3) 2_566 . . . ?
Tb1 O4 C4 C1 -177.1(12) 2_566 . . . ?
Tb1 O5 C10 N1 144(3) . . . . ?
Tb1 O6 C2 O3 7(2) 2_566 . . . ?
Tb1 O6 C2 C3 -175.7(12) 2_566 . . . ?
Tb1 O7 C7 O8 -8(2) . . . . ?
Tb1 O7 C7 C11 175.6(16) . . . . ?
Tb1 O8 C7 O7 9(2) . . . . ?
Tb1 O8 C7 C11 -175.7(18) . . . . ?
Tb1 O11 C13 N2 174(3) . . . . ?
O3 C2 C3 C5 -7(3) . . . . ?
O3 C2 C3 C6 172(2) . . . 2_666 ?
O6 C2 C3 C5 175.8(19) . . . . ?
O6 C2 C3 C6 -6(3) . . . 2_666 ?
O7 C7 C11 C12 -4(3) . . . . ?
O7 C7 C11 C14 174.4(18) . . . . ?
O8 C7 C11 C12 -180(2) . . . . ?
O8 C7 C11 C14 -1(3) . . . . ?
C1 C8 C9 O9 -178.6(19) . . . . ?
C1 C8 C9 C1 -3(4) . . . 2_556 ?
C2 C3 C5 C6 178(2) . . . . ?
C3 C5 C6 O12 -178(2) . . . . ?
C3 C5 C6 C3 1(4) . . . 2_666 ?
C4 C1 C8 C9 -176.9(19) . . . . ?
C6 C3 C5 C6 -1(4) 2_666 . . . ?
C7 C11 C12 O1A 3(4) . . . . ?
C7 C11 C12 C14 179(2) . . . 2_677 ?
C7 C11 C14 O1B -18(4) . . . . ?
C7 C11 C14 C12 -178.7(17) . . . 2_677 ?
C8 C1 C4 O2 8(3) . . . . ?
C8 C1 C4 O4 -172.6(18) . . . . ?
C9 C1 C4 O2 -172.0(19) 2_556 . . . ?
C9 C1 C4 O4 8(3) 2_556 . . . ?
C9 C1 C8 C9 3(3) 2_556 . . . ?
C12 C11 C14 O1B 161(3) . . . . ?
C12 C11 C14 C12 0(4) . . . 2_677 ?
C14 C11 C12 O1A -175(2) . . . . ?
C14 C11 C12 C14 0(4) . . . 2_677 ?
C15 N1 C10 O5 -174(3) . . . . ?
C16 N1 C10 O5 -5(3) . . . . ?
C17 N2 C13 O11 0(4) . . . . ?
C18 N2 C13 O11 -177(3) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.500 0.000 0.500 353.9 0.0 ?


_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 2.622
_oxdiff_exptl_absorpt_empirical_full_min 0.442

# start Validation Reply Form
_vrf_PLAT029_SION2_380K          
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.733 Why?  
RESPONSE: The data were collected upon the spindle rotation. Therefore, a 
		  limited portion of the reciprocal space could be probed.
;
_vrf_PLAT973_SION2_380K          
;
PROBLEM: Check Calcd Positive Resid. Density on       Tb1       2.73 eA-3  
RESPONSE: Electron density maximum in the vicinity of a heavy atom (Tb1)
		  may be the result of a finite Fourier sum truncation. 
;
# 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_SION2_240K_cool
_database_code_depnum_ccdc_archive 'CCDC 1941018'
loop_
_audit_author_name
_audit_author_address
'Andrzej Gladysiak'
;Ecole polytechnique federale de Lausanne
Switzerland
;
_audit_update_record             
;
2019-07-16 deposited with the CCDC.	2019-08-12 downloaded from the CCDC.
;
_audit_creation_date             2019-05-27
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C18 H20 N2 O11 Tb'
_chemical_formula_sum            'C18 H20 N2 O11 Tb'
_chemical_formula_weight         599.28
_chemical_melting_point          ?
_chemical_oxdiff_formula         C21H27N3O12Tb
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0045 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'
N N 0.0083 0.0040 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0145 0.0076 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.0972 4.9386 '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                   10.6404(6)
_cell_length_b                   11.1598(5)
_cell_length_c                   11.4981(5)
_cell_angle_alpha                96.878(4)
_cell_angle_beta                 111.214(5)
_cell_angle_gamma                101.458(4)
_cell_volume                     1219.70(11)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3203
_cell_measurement_temperature    240.0
_cell_measurement_theta_max      32.2600
_cell_measurement_theta_min      2.1170
_shelx_estimated_absorpt_T_max   0.776
_shelx_estimated_absorpt_T_min   0.516
_exptl_absorpt_coefficient_mu    3.811
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94170
_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            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.632
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             590
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0100
_diffrn_reflns_av_unetI/netI     0.0118
_diffrn_reflns_Laue_measured_fraction_full 0.713
_diffrn_reflns_Laue_measured_fraction_max 0.544
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6812
_diffrn_reflns_point_group_measured_fraction_full 0.713
_diffrn_reflns_point_group_measured_fraction_max 0.544
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         32.237
_diffrn_reflns_theta_min         2.101
_diffrn_ambient_temperature      240.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            PILATUS2M
_diffrn_measured_fraction_theta_full 0.713
_diffrn_measured_fraction_theta_max 0.544
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      0.00 360.00   1.00    1.00    --    0.00   0.00   0.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  PILATUS@SNBL
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0668927000
_diffrn_orient_matrix_UB_12      -0.0034235000
_diffrn_orient_matrix_UB_13      -0.0127716000
_diffrn_orient_matrix_UB_21      0.0459500000
_diffrn_orient_matrix_UB_22      0.0515536000
_diffrn_orient_matrix_UB_23      0.0618802000
_diffrn_orient_matrix_UB_31      0.0109604000
_diffrn_orient_matrix_UB_32      -0.0520172000
_diffrn_orient_matrix_UB_33      0.0400535000
_diffrn_radiation_monochromator  'Si (111)'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.78405
_diffrn_source                   
'European Synchrotron Radiation Facility, BM01 beamline'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3304
_reflns_number_total             3501
_reflns_odcompleteness_completeness 54.42
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     32.24
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         7.077
_refine_diff_density_min         -2.816
_refine_diff_density_rms         0.298
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     292
_refine_ls_number_reflns         3501
_refine_ls_number_restraints     34
_refine_ls_R_factor_all          0.0854
_refine_ls_R_factor_gt           0.0833
_refine_ls_restrained_S_all      6.260
_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)+(0.1953P)²+2.4729P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2161
_refine_ls_wR_factor_ref         0.2214
_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
 C12_$6-O1 \\sim O1-C11
 with sigma of 0.05
 C17-C13 \\sim C13-C18
 with sigma of 0.02
3. Restrained planarity
 C13, C17, C18, N2, O11
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C17) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
5. Rigid body (RIGU) restrains
 O11, C13, N2, C18, C17
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Me refined with riding coordinates:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C)
6.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C8(H8), C12(H12), C13(H13), C16(H16)
6.c Tetrahedral OH refined with riding coordinates:
 O1(H1), O12(H12A)
6.d Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C15(H15A,H15B,H15C)
6.e Idealised tetrahedral OH refined as rotating group:
 O9(H9)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
C1 C -0.0202(10) 0.1211(10) 0.4968(10) 0.045(3) Uani 1 1 d . . . . .
C2 C 0.2052(9) 0.4854(10) 0.4320(11) 0.043(3) Uani 1 1 d . . . . .
C3 C 0.3576(9) 0.4935(11) 0.4665(10) 0.041(3) Uani 1 1 d . . . . .
C4 C -0.0369(10) 0.2518(10) 0.4984(11) 0.042(3) Uani 1 1 d . . . . .
C5 C 0.4528(11) 0.5399(13) 0.5931(11) 0.056(3) Uani 1 1 d . . . . .
H5 H 0.421150 0.568107 0.655176 0.067 Uiso 1 1 calc R . . . .
C6 C 0.5955(12) 0.5450(14) 0.6289(11) 0.056(4) Uani 1 1 d . . . . .
C7 C 0.3033(10) 0.7592(10) 0.8609(11) 0.042(3) Uani 1 1 d . . . . .
C8 C 0.0016(13) 0.0724(11) 0.6065(11) 0.050(3) Uani 1 1 d . . . . .
H8 H 0.000346 0.121165 0.678436 0.060 Uiso 1 1 calc R . . . .
C9 C 0.0250(12) -0.0447(11) 0.6142(10) 0.046(3) Uani 1 1 d . . . . .
C10 C 0.0507(19) 0.1786(18) 0.9909(19) 0.082(5) Uani 1 1 d . . . . .
H10A H 0.005189 0.172011 1.050101 0.124 Uiso 1 1 calc GR . . . .
H10B H 0.150894 0.195421 1.037176 0.124 Uiso 1 1 calc GR . . . .
H10C H 0.016911 0.100786 0.928262 0.124 Uiso 1 1 calc GR . . . .
C11 C 0.4013(10) 0.8849(10) 0.9327(10) 0.045(3) Uani 1 1 d D . . . .
C12 C 0.3614(11) 0.9648(13) 0.9895(14) 0.063(4) Uani 1 1 d D . . . .
H12 H 0.269430 0.944798 0.985088 0.076 Uiso 1 1 calc R . . A 2
C13 C 0.3095(14) 0.3296(14) 0.7181(15) 0.073(4) Uani 1 1 d D U . . .
H13 H 0.241961 0.282751 0.638810 0.088 Uiso 1 1 calc R . . . .
C14 C 0.5434(11) 0.9111(12) 0.9372(14) 0.065(4) Uani 1 1 d . . . . .
C15 C -0.1261(16) 0.281(2) 0.8614(19) 0.085(5) Uani 1 1 d . . . . .
H15A H -0.167863 0.289278 0.923307 0.128 Uiso 1 1 calc GR . . . .
H15B H -0.176697 0.204112 0.798589 0.128 Uiso 1 1 calc GR . . . .
H15C H -0.130634 0.351641 0.819147 0.128 Uiso 1 1 calc GR . . . .
C16 C 0.1174(16) 0.3700(18) 0.9321(15) 0.065(4) Uani 1 1 d . . . . .
H16 H 0.209882 0.367996 0.977960 0.078 Uiso 1 1 calc R . . . .
C17 C 0.440(3) 0.181(2) 0.702(3) 0.136(9) Uani 1 1 d D U . . .
H17A H 0.529008 0.165854 0.751203 0.203 Uiso 1 1 calc R . . . .
H17B H 0.364840 0.109731 0.690607 0.203 Uiso 1 1 calc R . . . .
H17C H 0.437725 0.193614 0.619173 0.203 Uiso 1 1 calc R . . . .
C18 C 0.532(2) 0.360(3) 0.887(2) 0.130(9) Uani 1 1 d D U . . .
H18A H 0.607052 0.318928 0.909240 0.195 Uiso 1 1 calc R . . . .
H18B H 0.567610 0.444719 0.879484 0.195 Uiso 1 1 calc R . . . .
H18C H 0.495953 0.363336 0.953463 0.195 Uiso 1 1 calc R . . . .
N1 N 0.0194(12) 0.2804(11) 0.9262(11) 0.057(3) Uani 1 1 d . . . . .
N2 N 0.4240(15) 0.2932(16) 0.7699(17) 0.094(5) Uani 1 1 d . U . . .
O1 O 0.5956(10) 0.8202(11) 0.8840(14) 0.100(5) Uani 1 1 d D . . . .
H1 H 0.530181 0.758079 0.840333 0.150 Uiso 1 1 calc R . . . .
O2 O -0.0101(8) 0.3203(7) 0.6055(7) 0.0415(17) Uani 1 1 d . . . . .
O3 O 0.1617(7) 0.5066(8) 0.5186(8) 0.049(2) Uani 1 1 d . . . . .
O4 O -0.0719(8) 0.2853(7) 0.3934(7) 0.0472(19) Uani 1 1 d . . . . .
O5 O 0.0976(11) 0.4619(11) 0.8799(10) 0.065(3) Uani 1 1 d . . . . .
O6 O 0.1217(7) 0.4578(8) 0.3142(7) 0.0454(19) Uani 1 1 d . . . . .
O7 O 0.1851(7) 0.7289(7) 0.8683(7) 0.0476(19) Uani 1 1 d . . . . .
O8 O 0.3388(8) 0.6852(8) 0.7919(9) 0.055(2) Uani 1 1 d . . . . .
O9 O 0.0447(12) -0.0810(10) 0.7276(9) 0.068(3) Uani 1 1 d . . . . .
H9 H 0.094017 -0.131054 0.736931 0.101 Uiso 1 1 calc GR . . . .
O11 O 0.2864(9) 0.4219(10) 0.7683(10) 0.066(3) Uani 1 1 d . U . . .
O12 O 0.6820(9) 0.5866(12) 0.7541(8) 0.075(3) Uani 1 1 d . . . . .
H12A H 0.762794 0.585342 0.763528 0.113 Uiso 1 1 calc R . . . .
Tb1 Tb 0.10827(3) 0.53494(4) 0.69876(4) 0.0357(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
C1 C4 1.503(16) . ?
C1 C8 1.394(19) . ?
C1 C9 1.425(14) 2_556 ?
C2 C3 1.505(12) . ?
C2 O3 1.258(13) . ?
C2 O6 1.281(13) . ?
C3 C5 1.399(15) . ?
C3 C6 1.416(15) 2_666 ?
C4 O2 1.270(12) . ?
C4 O4 1.255(15) . ?
C5 H5 0.9400 . ?
C5 C6 1.409(15) . ?
C6 O12 1.359(14) . ?
C7 C11 1.502(13) . ?
C7 O7 1.272(13) . ?
C7 O8 1.280(12) . ?
C8 H8 0.9400 . ?
C8 C9 1.385(18) . ?
C9 O9 1.368(16) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 H10C 0.9700 . ?
C10 N1 1.46(2) . ?
C11 C12 1.270(16) . ?
C11 C14 1.462(15) . ?
C12 H12 0.9400 . ?
C12 C14 1.483(16) 2_677 ?
C13 H13 0.9400 . ?
C13 N2 1.32(2) . ?
C13 O11 1.230(18) . ?
C14 O1 1.427(14) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C15 H15C 0.9700 . ?
C15 N1 1.46(2) . ?
C16 H16 0.9400 . ?
C16 N1 1.27(2) . ?
C16 O5 1.26(2) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C17 H17C 0.9700 . ?
C17 N2 1.47(3) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C18 H18C 0.9700 . ?
C18 N2 1.41(3) . ?
O1 H1 0.8300 . ?
O2 Tb1 2.384(7) . ?
O3 Tb1 2.341(8) . ?
O4 Tb1 2.412(9) 2_566 ?
O5 Tb1 2.357(12) . ?
O6 Tb1 2.416(6) 2_566 ?
O7 Tb1 2.507(7) . ?
O8 Tb1 2.451(7) . ?
O9 H9 0.8300 . ?
O11 Tb1 2.433(9) . ?
O12 H12A 0.8300 . ?

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
C8 C1 C4 119.6(9) . . ?
C8 C1 C9 118.5(10) . 2_556 ?
C9 C1 C4 121.9(11) 2_556 . ?
O3 C2 C3 119.9(9) . . ?
O3 C2 O6 121.0(8) . . ?
O6 C2 C3 119.1(8) . . ?
C5 C3 C2 119.6(9) . . ?
C5 C3 C6 120.2(9) . 2_666 ?
C6 C3 C2 120.1(9) 2_666 . ?
O2 C4 C1 117.9(11) . . ?
O4 C4 C1 116.6(9) . . ?
O4 C4 O2 125.5(10) . . ?
C3 C5 H5 119.5 . . ?
C3 C5 C6 120.9(9) . . ?
C6 C5 H5 119.5 . . ?
C5 C6 C3 118.8(10) . 2_666 ?
O12 C6 C3 123.0(10) . 2_666 ?
O12 C6 C5 118.2(9) . . ?
O7 C7 C11 119.2(9) . . ?
O7 C7 O8 121.1(9) . . ?
O8 C7 C11 119.7(9) . . ?
C1 C8 H8 118.6 . . ?
C9 C8 C1 122.9(9) . . ?
C9 C8 H8 118.6 . . ?
C8 C9 C1 118.6(11) . 2_556 ?
O9 C9 C1 124.5(11) . 2_556 ?
O9 C9 C8 116.8(9) . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N1 C10 H10A 109.5 . . ?
N1 C10 H10B 109.5 . . ?
N1 C10 H10C 109.5 . . ?
C12 C11 C7 120.3(10) . . ?
C12 C11 C14 121.4(10) . . ?
C14 C11 C7 118.2(9) . . ?
C11 C12 H12 119.3 . . ?
C11 C12 C14 121.4(10) . 2_677 ?
C14 C12 H12 119.3 2_677 . ?
N2 C13 H13 118.3 . . ?
O11 C13 H13 118.3 . . ?
O11 C13 N2 123.3(14) . . ?
C11 C14 C12 117.1(9) . 2_677 ?
O1 C14 C11 123.0(10) . . ?
O1 C14 C12 119.7(9) . 2_677 ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N1 C15 H15A 109.5 . . ?
N1 C15 H15B 109.5 . . ?
N1 C15 H15C 109.5 . . ?
N1 C16 H16 118.2 . . ?
O5 C16 H16 118.2 . . ?
O5 C16 N1 123.7(15) . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N2 C17 H17A 109.5 . . ?
N2 C17 H17B 109.5 . . ?
N2 C17 H17C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N2 C18 H18A 109.5 . . ?
N2 C18 H18B 109.5 . . ?
N2 C18 H18C 109.5 . . ?
C15 N1 C10 118.9(14) . . ?
C16 N1 C10 120.4(15) . . ?
C16 N1 C15 120.5(16) . . ?
C13 N2 C17 118.8(17) . . ?
C13 N2 C18 121.8(17) . . ?
C18 N2 C17 119.4(19) . . ?
C14 O1 H1 109.5 . . ?
C4 O2 Tb1 132.8(7) . . ?
C2 O3 Tb1 171.4(8) . . ?
C4 O4 Tb1 141.7(6) . 2_566 ?
C16 O5 Tb1 139.2(9) . . ?
C2 O6 Tb1 108.3(6) . 2_566 ?
C7 O7 Tb1 91.5(6) . . ?
C7 O8 Tb1 93.8(6) . . ?
C9 O9 H9 109.5 . . ?
C13 O11 Tb1 134.3(10) . . ?
C6 O12 H12A 109.5 . . ?
O2 Tb1 O4 128.1(3) . 2_566 ?
O2 Tb1 O6 81.5(3) . 2_566 ?
O2 Tb1 O7 153.1(3) . . ?
O2 Tb1 O8 143.6(3) . . ?
O2 Tb1 O11 74.7(3) . . ?
O3 Tb1 O2 78.7(3) . . ?
O3 Tb1 O4 74.9(3) . 2_566 ?
O3 Tb1 O5 147.9(3) . . ?
O3 Tb1 O6 122.8(3) . 2_566 ?
O3 Tb1 O7 128.2(3) . . ?
O3 Tb1 O8 83.2(3) . . ?
O3 Tb1 O11 79.3(3) . . ?
O4 Tb1 O6 76.8(3) 2_566 2_566 ?
O4 Tb1 O7 68.7(3) 2_566 . ?
O4 Tb1 O8 75.5(3) 2_566 . ?
O4 Tb1 O11 139.7(3) 2_566 . ?
O5 Tb1 O2 79.7(3) . . ?
O5 Tb1 O4 137.2(3) . 2_566 ?
O5 Tb1 O6 76.7(3) . 2_566 ?
O5 Tb1 O7 75.3(3) . . ?
O5 Tb1 O8 101.0(3) . . ?
O5 Tb1 O11 72.2(4) . . ?
O6 Tb1 O7 83.2(2) 2_566 . ?
O6 Tb1 O8 134.5(3) 2_566 . ?
O6 Tb1 O11 143.5(3) 2_566 . ?
O8 Tb1 O7 53.2(2) . . ?
O11 Tb1 O7 106.4(3) . . ?
O11 Tb1 O8 71.1(3) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O1 H1 O8 0.83 1.88 2.597(12) 144.0 . yes
O9 H9 O4 0.83 2.06 2.647(12) 127.8 2_556 yes
O12 H12A O6 0.83 1.86 2.594(11) 146.4 2_666 yes

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
C1 C4 O2 Tb1 138.5(8) . . . . ?
C1 C4 O4 Tb1 -174.6(7) . . . 2_566 ?
C1 C8 C9 C1 -3.0(19) . . . 2_556 ?
C1 C8 C9 O9 -179.9(11) . . . . ?
C2 C3 C5 C6 178.0(13) . . . . ?
C3 C2 O6 Tb1 -177.2(8) . . . 2_566 ?
C3 C5 C6 C3 2(2) . . . 2_666 ?
C3 C5 C6 O12 -177.5(15) . . . . ?
C4 C1 C8 C9 -176.6(10) . . . . ?
C6 C3 C5 C6 -2(2) 2_666 . . . ?
C7 C11 C12 C14 179.1(14) . . . 2_677 ?
C7 C11 C14 C12 -179.1(14) . . . 2_677 ?
C7 C11 C14 O1 -4(2) . . . . ?
C8 C1 C4 O2 10.2(15) . . . . ?
C8 C1 C4 O4 -172.1(10) . . . . ?
C9 C1 C4 O2 -169.4(10) 2_556 . . . ?
C9 C1 C4 O4 8.2(15) 2_556 . . . ?
C9 C1 C8 C9 3.0(19) 2_556 . . . ?
C11 C7 O7 Tb1 172.1(11) . . . . ?
C11 C7 O8 Tb1 -172.0(10) . . . . ?
C12 C11 C14 C12 0(3) . . . 2_677 ?
C12 C11 C14 O1 174.5(16) . . . . ?
C14 C11 C12 C14 0(3) . . . 2_677 ?
N1 C16 O5 Tb1 -103.2(17) . . . . ?
N2 C13 O11 Tb1 171.6(11) . . . . ?
O2 C4 O4 Tb1 2.9(18) . . . 2_566 ?
O3 C2 C3 C5 -8.1(18) . . . . ?
O3 C2 C3 C6 172.2(12) . . . 2_666 ?
O3 C2 O6 Tb1 2.3(13) . . . 2_566 ?
O4 C4 O2 Tb1 -38.9(15) . . . . ?
O5 C16 N1 C10 -179.1(14) . . . . ?
O5 C16 N1 C15 -3(2) . . . . ?
O6 C2 C3 C5 171.3(12) . . . . ?
O6 C2 C3 C6 -8.4(18) . . . 2_666 ?
O7 C7 C11 C12 -7(2) . . . . ?
O7 C7 C11 C14 171.7(13) . . . . ?
O7 C7 O8 Tb1 6.9(13) . . . . ?
O8 C7 C11 C12 171.9(14) . . . . ?
O8 C7 C11 C14 -9.4(19) . . . . ?
O8 C7 O7 Tb1 -6.8(13) . . . . ?
O11 C13 N2 C17 179.6(12) . . . . ?
O11 C13 N2 C18 -2(2) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.500 0.000 0.500 213.8 0.0 ?


_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 1.415
_oxdiff_exptl_absorpt_empirical_full_min 0.728

# start Validation Reply Form
_vrf_PLAT027_SION2_240K_cool     
;
PROBLEM: _diffrn_reflns_theta_full value (too) Low ......      26.00 Degree
RESPONSE: Our value of max sin(theta)/lambda of 0.56 is close to the recommended 
		  value of 0.60. Higer values of sin(theta)/lambda were not available due 
		  to the beamline experimental set-up limitations.
;
_vrf_PLAT029_SION2_240K_cool     
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.713 Why?  
RESPONSE: The data were collected upon the spindle rotation. Therefore, a 
		  limited portion of the reciprocal space could be probed.
;
# 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_SION2_160K_cool
_database_code_depnum_ccdc_archive 'CCDC 1941015'
loop_
_audit_author_name
_audit_author_address
'Andrzej Gladysiak'
;Ecole polytechnique federale de Lausanne
Switzerland
;
_audit_update_record             
;
2019-07-16 deposited with the CCDC.	2019-08-12 downloaded from the CCDC.
;
_audit_creation_date             2019-05-27
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C18 H20 N2 O11 Tb'
_chemical_formula_sum            'C18 H20 N2 O11 Tb'
_chemical_formula_weight         599.28
_chemical_melting_point          ?
_chemical_oxdiff_formula         C21H27N3O12Tb
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0045 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'
N N 0.0083 0.0040 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0145 0.0076 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.0972 4.9386 '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                   10.6385(6)
_cell_length_b                   11.1794(5)
_cell_length_c                   11.4206(5)
_cell_angle_alpha                96.942(4)
_cell_angle_beta                 111.003(5)
_cell_angle_gamma                101.423(4)
_cell_volume                     1215.29(11)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3160
_cell_measurement_temperature    160.0
_cell_measurement_theta_max      31.9410
_cell_measurement_theta_min      2.1120
_shelx_estimated_absorpt_T_max   0.776
_shelx_estimated_absorpt_T_min   0.515
_exptl_absorpt_coefficient_mu    3.825
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82610
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.638
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             590
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0088
_diffrn_reflns_av_unetI/netI     0.0133
_diffrn_reflns_Laue_measured_fraction_full 0.712
_diffrn_reflns_Laue_measured_fraction_max 0.540
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6767
_diffrn_reflns_point_group_measured_fraction_full 0.712
_diffrn_reflns_point_group_measured_fraction_max 0.540
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         32.249
_diffrn_reflns_theta_min         2.097
_diffrn_ambient_temperature      160.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            PILATUS2M
_diffrn_measured_fraction_theta_full 0.712
_diffrn_measured_fraction_theta_max 0.540
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      0.00 360.00   1.00    1.00    --    0.00   0.00   0.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  PILATUS@SNBL
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0667667000
_diffrn_orient_matrix_UB_12      -0.0036733000
_diffrn_orient_matrix_UB_13      -0.0130891000
_diffrn_orient_matrix_UB_21      0.0459099000
_diffrn_orient_matrix_UB_22      0.0516393000
_diffrn_orient_matrix_UB_23      0.0619938000
_diffrn_orient_matrix_UB_31      0.0109651000
_diffrn_orient_matrix_UB_32      -0.0517178000
_diffrn_orient_matrix_UB_33      0.0405196000
_diffrn_radiation_monochromator  'Si (111)'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.78405
_diffrn_source                   
'European Synchrotron Radiation Facility, BM01 beamline'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3313
_reflns_number_total             3465
_reflns_odcompleteness_completeness 62.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     29.34
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         5.944
_refine_diff_density_min         -0.826
_refine_diff_density_rms         0.217
_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     292
_refine_ls_number_reflns         3465
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.0635
_refine_ls_R_factor_gt           0.0620
_refine_ls_restrained_S_all      6.354
_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)+(0.1311P)²+5.5583P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1674
_refine_ls_wR_factor_ref         0.1698
_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
 C17-C13 \\sim C13-C18
 with sigma of 0.02
 C12_$7-O1 \\sim O1-C11
 with sigma of 0.05
3. Restrained planarity
 C13, C17, C18, N2, O11
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C17) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
5.a Me refined with riding coordinates:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C)
5.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C8(H8), C12(H12), C13(H13), C16(H16)
5.c Tetrahedral OH refined with riding coordinates:
 O1(H1), O12(H12A)
5.d Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C15(H15A,H15B,H15C)
5.e Idealised tetrahedral OH refined as rotating group:
 O9(H9)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
C1 C -0.0209(8) 0.1210(9) 0.4969(9) 0.036(2) Uani 1 1 d . . . . .
C2 C 0.2049(8) 0.4854(9) 0.4307(9) 0.037(2) Uani 1 1 d . . . . .
C3 C 0.3570(8) 0.4939(9) 0.4661(9) 0.037(2) Uani 1 1 d . . . . .
C4 C -0.0365(8) 0.2520(9) 0.4986(10) 0.039(3) Uani 1 1 d . . . . .
C5 C 0.4512(9) 0.5378(11) 0.5943(10) 0.048(3) Uani 1 1 d . . . . .
H5 H 0.418723 0.564209 0.657834 0.058 Uiso 1 1 calc R . . . .
C6 C 0.5940(9) 0.5430(11) 0.6296(9) 0.047(3) Uani 1 1 d . . . . .
C7 C 0.3013(8) 0.7597(8) 0.8596(9) 0.035(2) Uani 1 1 d . . . . .
C8 C 0.0036(10) 0.0735(10) 0.6095(10) 0.044(3) Uani 1 1 d . . . . .
H8 H 0.005532 0.123623 0.683795 0.053 Uiso 1 1 calc R . . . .
C9 C 0.0250(10) -0.0449(9) 0.6147(9) 0.039(2) Uani 1 1 d . . . . .
C10 C 0.0508(14) 0.1787(13) 0.9919(15) 0.066(4) Uani 1 1 d . . . . .
H10A H 0.018331 0.180430 1.062169 0.099 Uiso 1 1 calc GR . . . .
H10B H 0.151715 0.188392 1.026475 0.099 Uiso 1 1 calc GR . . . .
H10C H 0.003492 0.098856 0.930437 0.099 Uiso 1 1 calc GR . . . .
C11 C 0.4015(9) 0.8857(9) 0.9316(10) 0.043(3) Uani 1 1 d D . . . .
C12 C 0.3626(9) 0.9689(11) 0.9926(12) 0.053(3) Uani 1 1 d D . . . .
H12 H 0.270811 0.949341 0.990912 0.064 Uiso 1 1 calc R . . A 2
C13 C 0.3099(12) 0.3295(11) 0.7207(12) 0.067(4) Uani 1 1 d D . . . .
H13 H 0.241183 0.280782 0.641177 0.081 Uiso 1 1 calc R . . . .
C14 C 0.5430(9) 0.9094(11) 0.9375(12) 0.056(3) Uani 1 1 d . . . . .
C15 C -0.1269(13) 0.2763(16) 0.8585(15) 0.072(4) Uani 1 1 d . . . . .
H15A H -0.169140 0.294029 0.919912 0.107 Uiso 1 1 calc GR . . . .
H15B H -0.176998 0.193461 0.803472 0.107 Uiso 1 1 calc GR . . . .
H15C H -0.132572 0.339337 0.805514 0.107 Uiso 1 1 calc GR . . . .
C16 C 0.1180(12) 0.3727(14) 0.9333(12) 0.056(3) Uani 1 1 d . . . . .
H16 H 0.211717 0.371589 0.979578 0.068 Uiso 1 1 calc R . . . .
C17 C 0.435(3) 0.177(2) 0.702(3) 0.138(9) Uani 1 1 d D U . . .
H17A H 0.524550 0.159974 0.749902 0.207 Uiso 1 1 calc R . . . .
H17B H 0.358607 0.106784 0.693153 0.207 Uiso 1 1 calc R . . . .
H17C H 0.430351 0.187796 0.616670 0.207 Uiso 1 1 calc R . . . .
C18 C 0.5324(17) 0.366(2) 0.8919(19) 0.106(6) Uani 1 1 d D . . . .
H18A H 0.609596 0.325893 0.916740 0.159 Uiso 1 1 calc R . . . .
H18B H 0.566322 0.450188 0.881436 0.159 Uiso 1 1 calc R . . . .
H18C H 0.495012 0.370053 0.958791 0.159 Uiso 1 1 calc R . . . .
N1 N 0.0196(9) 0.2794(9) 0.9282(9) 0.050(2) Uani 1 1 d . . . . .
N2 N 0.4240(12) 0.2934(12) 0.7724(13) 0.077(4) Uani 1 1 d . . . . .
O1 O 0.5941(8) 0.8203(9) 0.8811(11) 0.085(4) Uani 1 1 d D . . . .
H1 H 0.527923 0.757613 0.837010 0.128 Uiso 1 1 calc R . . . .
O2 O -0.0087(6) 0.3212(6) 0.6067(6) 0.0373(15) Uani 1 1 d . . . . .
O3 O 0.1599(6) 0.5051(6) 0.5176(7) 0.0421(17) Uani 1 1 d . . . . .
O4 O -0.0717(7) 0.2862(6) 0.3917(6) 0.0397(16) Uani 1 1 d . . . . .
O5 O 0.0979(9) 0.4641(9) 0.8815(8) 0.055(2) Uani 1 1 d . . . . .
O6 O 0.1222(6) 0.4576(7) 0.3118(7) 0.0420(17) Uani 1 1 d . . . . .
O7 O 0.1854(6) 0.7305(6) 0.8697(6) 0.0405(16) Uani 1 1 d . . . . .
O8 O 0.3373(6) 0.6847(7) 0.7914(7) 0.047(2) Uani 1 1 d . . . . .
O9 O 0.0467(10) -0.0814(8) 0.7293(7) 0.056(2) Uani 1 1 d . . . . .
H9 H 0.051833 -0.155789 0.721312 0.083 Uiso 1 1 calc GR . . . .
O11 O 0.2865(7) 0.4234(8) 0.7697(9) 0.059(2) Uani 1 1 d . . . . .
O12 O 0.6804(7) 0.5836(10) 0.7569(7) 0.066(3) Uani 1 1 d . . . . .
H12A H 0.762188 0.582422 0.766575 0.099 Uiso 1 1 calc R . . . .
Tb1 Tb 0.10743(3) 0.53526(3) 0.69943(3) 0.0318(2) 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
C1 C4 1.505(14) . ?
C1 C8 1.407(16) . ?
C1 C9 1.427(12) 2_556 ?
C2 C3 1.501(10) . ?
C2 O3 1.262(11) . ?
C2 O6 1.284(11) . ?
C3 C5 1.402(13) . ?
C3 C6 1.422(12) 2_666 ?
C4 O2 1.276(11) . ?
C4 O4 1.272(13) . ?
C5 H5 0.9500 . ?
C5 C6 1.412(12) . ?
C6 O12 1.373(12) . ?
C7 C11 1.515(11) . ?
C7 O7 1.262(11) . ?
C7 O8 1.280(10) . ?
C8 H8 0.9500 . ?
C8 C9 1.392(15) . ?
C9 O9 1.372(14) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C10 N1 1.442(19) . ?
C11 C12 1.313(14) . ?
C11 C14 1.451(12) . ?
C12 H12 0.9500 . ?
C12 C14 1.456(13) 2_677 ?
C13 H13 0.9500 . ?
C13 N2 1.312(17) . ?
C13 O11 1.240(14) . ?
C14 O1 1.418(12) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C15 N1 1.465(16) . ?
C16 H16 0.9500 . ?
C16 N1 1.302(17) . ?
C16 O5 1.258(17) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C17 N2 1.49(2) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C18 N2 1.44(2) . ?
O1 H1 0.8400 . ?
O2 Tb1 2.378(6) . ?
O3 Tb1 2.340(7) . ?
O4 Tb1 2.394(8) 2_566 ?
O5 Tb1 2.342(9) . ?
O6 Tb1 2.418(6) 2_566 ?
O7 Tb1 2.517(6) . ?
O8 Tb1 2.448(6) . ?
O9 H9 0.8400 . ?
O11 Tb1 2.435(8) . ?
O12 H12A 0.8400 . ?

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
C8 C1 C4 119.4(8) . . ?
C8 C1 C9 118.9(9) . 2_556 ?
C9 C1 C4 121.6(9) 2_556 . ?
O3 C2 C3 119.9(8) . . ?
O3 C2 O6 120.9(7) . . ?
O6 C2 C3 119.2(7) . . ?
C5 C3 C2 119.9(8) . . ?
C5 C3 C6 119.8(7) . 2_666 ?
C6 C3 C2 120.3(8) 2_666 . ?
O2 C4 C1 117.9(9) . . ?
O4 C4 C1 116.9(8) . . ?
O4 C4 O2 125.2(9) . . ?
C3 C5 H5 119.7 . . ?
C3 C5 C6 120.5(8) . . ?
C6 C5 H5 119.7 . . ?
C5 C6 C3 119.6(8) . 2_666 ?
O12 C6 C3 122.5(8) . 2_666 ?
O12 C6 C5 117.8(8) . . ?
O7 C7 C11 119.2(7) . . ?
O7 C7 O8 121.7(7) . . ?
O8 C7 C11 119.1(8) . . ?
C1 C8 H8 119.1 . . ?
C9 C8 C1 121.7(8) . . ?
C9 C8 H8 119.1 . . ?
C8 C9 C1 119.4(10) . 2_556 ?
O9 C9 C1 124.1(9) . 2_556 ?
O9 C9 C8 116.5(8) . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N1 C10 H10A 109.5 . . ?
N1 C10 H10B 109.5 . . ?
N1 C10 H10C 109.5 . . ?
C12 C11 C7 120.4(8) . . ?
C12 C11 C14 121.0(8) . . ?
C14 C11 C7 118.5(8) . . ?
C11 C12 H12 119.3 . . ?
C11 C12 C14 121.4(8) . 2_677 ?
C14 C12 H12 119.3 2_677 . ?
N2 C13 H13 118.1 . . ?
O11 C13 H13 118.1 . . ?
O11 C13 N2 123.8(12) . . ?
C11 C14 C12 117.5(8) . 2_677 ?
O1 C14 C11 123.7(8) . . ?
O1 C14 C12 118.8(8) . 2_677 ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N1 C15 H15A 109.5 . . ?
N1 C15 H15B 109.5 . . ?
N1 C15 H15C 109.5 . . ?
N1 C16 H16 117.6 . . ?
O5 C16 H16 117.6 . . ?
O5 C16 N1 124.8(12) . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N2 C17 H17A 109.5 . . ?
N2 C17 H17B 109.5 . . ?
N2 C17 H17C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N2 C18 H18A 109.5 . . ?
N2 C18 H18B 109.5 . . ?
N2 C18 H18C 109.5 . . ?
C10 N1 C15 118.5(11) . . ?
C16 N1 C10 121.6(11) . . ?
C16 N1 C15 120.0(13) . . ?
C13 N2 C17 117.2(14) . . ?
C13 N2 C18 120.1(13) . . ?
C18 N2 C17 122.7(16) . . ?
C14 O1 H1 109.5 . . ?
C4 O2 Tb1 133.3(6) . . ?
C2 O3 Tb1 171.2(7) . . ?
C4 O4 Tb1 141.7(6) . 2_566 ?
C16 O5 Tb1 138.7(7) . . ?
C2 O6 Tb1 107.6(5) . 2_566 ?
C7 O7 Tb1 90.9(5) . . ?
C7 O8 Tb1 93.7(5) . . ?
C9 O9 H9 109.5 . . ?
C13 O11 Tb1 134.7(8) . . ?
C6 O12 H12A 109.5 . . ?
O2 Tb1 O4 128.6(2) . 2_566 ?
O2 Tb1 O6 81.9(2) . 2_566 ?
O2 Tb1 O7 153.7(2) . . ?
O2 Tb1 O8 143.1(2) . . ?
O2 Tb1 O11 74.6(3) . . ?
O3 Tb1 O2 78.1(2) . . ?
O3 Tb1 O4 75.4(2) . 2_566 ?
O3 Tb1 O5 147.7(3) . . ?
O3 Tb1 O6 122.9(2) . 2_566 ?
O3 Tb1 O7 128.2(2) . . ?
O3 Tb1 O8 83.3(2) . . ?
O3 Tb1 O11 79.3(3) . . ?
O4 Tb1 O6 77.0(3) 2_566 2_566 ?
O4 Tb1 O7 68.2(2) 2_566 . ?
O4 Tb1 O8 75.3(2) 2_566 . ?
O4 Tb1 O11 139.5(3) 2_566 . ?
O5 Tb1 O2 80.0(3) . . ?
O5 Tb1 O4 136.8(3) . 2_566 ?
O5 Tb1 O6 76.6(3) . 2_566 ?
O5 Tb1 O7 75.4(3) . . ?
O5 Tb1 O8 100.8(3) . . ?
O5 Tb1 O11 72.2(3) . . ?
O6 Tb1 O7 83.4(2) 2_566 . ?
O6 Tb1 O8 134.6(2) 2_566 . ?
O6 Tb1 O11 143.5(3) 2_566 . ?
O8 Tb1 O7 53.1(2) . . ?
O11 Tb1 O7 106.0(3) . . ?
O11 Tb1 O8 70.8(3) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O1 H1 O8 0.84 1.88 2.605(10) 143.8 . yes
O9 H9 O4 0.84 1.92 2.638(10) 142.3 2_556 yes
O12 H12A O6 0.84 1.85 2.591(9) 146.3 2_666 yes

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
C1 C4 O2 Tb1 139.7(7) . . . . ?
C1 C4 O4 Tb1 -175.1(6) . . . 2_566 ?
C1 C8 C9 C1 -0.5(15) . . . 2_556 ?
C1 C8 C9 O9 -179.5(9) . . . . ?
C2 C3 C5 C6 178.2(11) . . . . ?
C3 C2 O6 Tb1 -177.2(7) . . . 2_566 ?
C3 C5 C6 C3 1(2) . . . 2_666 ?
C3 C5 C6 O12 -178.3(12) . . . . ?
C4 C1 C8 C9 -177.1(8) . . . . ?
C6 C3 C5 C6 -1(2) 2_666 . . . ?
C7 C11 C12 C14 180.0(12) . . . 2_677 ?
C7 C11 C14 C12 -179.9(11) . . . 2_677 ?
C7 C11 C14 O1 -1(2) . . . . ?
C8 C1 C4 O2 9.0(12) . . . . ?
C8 C1 C4 O4 -173.4(8) . . . . ?
C9 C1 C4 O2 -168.5(8) 2_556 . . . ?
C9 C1 C4 O4 9.0(12) 2_556 . . . ?
C9 C1 C8 C9 0.5(15) 2_556 . . . ?
C11 C7 O7 Tb1 172.9(9) . . . . ?
C11 C7 O8 Tb1 -172.7(9) . . . . ?
C12 C11 C14 C12 -3(2) . . . 2_677 ?
C12 C11 C14 O1 175.6(14) . . . . ?
C14 C11 C12 C14 3(2) . . . 2_677 ?
N1 C16 O5 Tb1 -102.5(14) . . . . ?
N2 C13 O11 Tb1 172.0(9) . . . . ?
O2 C4 O4 Tb1 2.2(15) . . . 2_566 ?
O3 C2 C3 C5 -7.4(15) . . . . ?
O3 C2 C3 C6 172.2(10) . . . 2_666 ?
O3 C2 O6 Tb1 3.0(12) . . . 2_566 ?
O4 C4 O2 Tb1 -37.6(13) . . . . ?
O5 C16 N1 C10 -179.0(11) . . . . ?
O5 C16 N1 C15 -0.2(18) . . . . ?
O6 C2 C3 C5 172.8(11) . . . . ?
O6 C2 C3 C6 -7.6(15) . . . 2_666 ?
O7 C7 C11 C12 -7.3(17) . . . . ?
O7 C7 C11 C14 169.4(11) . . . . ?
O7 C7 O8 Tb1 8.3(11) . . . . ?
O8 C7 C11 C12 173.6(12) . . . . ?
O8 C7 C11 C14 -9.7(16) . . . . ?
O8 C7 O7 Tb1 -8.0(11) . . . . ?
O11 C13 N2 C17 179.2(11) . . . . ?
O11 C13 N2 C18 -1.2(17) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.500 0.000 0.500 210.0 0.0 ?


_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 1.193
_oxdiff_exptl_absorpt_empirical_full_min 0.911

# start Validation Reply Form
_vrf_PLAT027_SION2_160K_cool     
;
PROBLEM: _diffrn_reflns_theta_full value (too) Low ......      26.00 Degree
RESPONSE: Our value of max sin(theta)/lambda of 0.56 is close to the recommended 
		  value of 0.60. Higer values of sin(theta)/lambda were not available due 
		  to the beamline experimental set-up limitations. 
;
_vrf_PLAT029_SION2_160K_cool     
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.712 Why?  
RESPONSE: The data were collected upon the spindle rotation. Therefore, a 
		  limited portion of the reciprocal space could be probed.
;
# 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_SION2_280K_cool
_database_code_depnum_ccdc_archive 'CCDC 1941022'
loop_
_audit_author_name
_audit_author_address
'Andrzej Gladysiak'
;Ecole polytechnique federale de Lausanne
Switzerland
;
_audit_update_record             
;
2019-07-16 deposited with the CCDC.	2019-08-12 downloaded from the CCDC.
;
_audit_creation_date             2019-05-28
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C18 H20 N2 O11 Tb'
_chemical_formula_sum            'C18 H20 N2 O11 Tb'
_chemical_formula_weight         599.28
_chemical_melting_point          ?
_chemical_oxdiff_formula         C21H27N3O12Tb
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0045 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'
N N 0.0083 0.0040 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0145 0.0076 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.0972 4.9386 '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                   10.6648(6)
_cell_length_b                   11.1779(5)
_cell_length_c                   11.5682(6)
_cell_angle_alpha                96.856(4)
_cell_angle_beta                 111.320(5)
_cell_angle_gamma                101.494(4)
_cell_volume                     1230.80(12)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3079
_cell_measurement_temperature    280.0
_cell_measurement_theta_max      32.3100
_cell_measurement_theta_min      2.1380
_shelx_estimated_absorpt_T_max   0.778
_shelx_estimated_absorpt_T_min   0.519
_exptl_absorpt_coefficient_mu    3.776
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81975
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.617
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             590
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0102
_diffrn_reflns_av_unetI/netI     0.0149
_diffrn_reflns_Laue_measured_fraction_full 0.713
_diffrn_reflns_Laue_measured_fraction_max 0.542
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6890
_diffrn_reflns_point_group_measured_fraction_full 0.713
_diffrn_reflns_point_group_measured_fraction_max 0.542
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         32.297
_diffrn_reflns_theta_min         2.098
_diffrn_ambient_temperature      280.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            PILATUS2M
_diffrn_measured_fraction_theta_full 0.713
_diffrn_measured_fraction_theta_max 0.542
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      0.00 360.00   1.00    1.00    --    0.00   0.00   0.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  PILATUS@SNBL
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0667647000
_diffrn_orient_matrix_UB_12      -0.0033730000
_diffrn_orient_matrix_UB_13      -0.0126238000
_diffrn_orient_matrix_UB_21      0.0459654000
_diffrn_orient_matrix_UB_22      0.0513867000
_diffrn_orient_matrix_UB_23      0.0616611000
_diffrn_orient_matrix_UB_31      0.0108726000
_diffrn_orient_matrix_UB_32      -0.0520403000
_diffrn_orient_matrix_UB_33      0.0397051000
_diffrn_radiation_monochromator  'Si (111)'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.78405
_diffrn_source                   
'European Synchrotron Radiation Facility, BM01 beamline'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3337
_reflns_number_total             3536
_reflns_odcompleteness_completeness 63.03
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     29.34
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         5.477
_refine_diff_density_min         -0.818
_refine_diff_density_rms         0.225
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     292
_refine_ls_number_reflns         3536
_refine_ls_number_restraints     34
_refine_ls_R_factor_all          0.0662
_refine_ls_R_factor_gt           0.0640
_refine_ls_restrained_S_all      6.346
_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)+(0.1357P)²+4.2052P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1719
_refine_ls_wR_factor_ref         0.1759
_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
 C12_$10-O1 \\sim O1-C11
 with sigma of 0.05
 C17-C13 \\sim C13-C18
 with sigma of 0.02
3. Restrained planarity
 C13, C17, C18, N2, O11
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C17) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
5. Rigid body (RIGU) restrains
 O11, C13, N2, C18, C17
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Me refined with riding coordinates:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C)
6.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C8(H8), C12(H12), C13(H13), C16(H16)
6.c Tetrahedral OH refined with riding coordinates:
 O1(H1), O12(H12A)
6.d Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C15(H15A,H15B,H15C)
6.e Idealised tetrahedral OH refined as rotating group:
 O9(H9)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
C1 C -0.0210(9) 0.1201(9) 0.4962(9) 0.043(2) Uani 1 1 d . . . . .
C2 C 0.2055(9) 0.4861(9) 0.4329(9) 0.044(2) Uani 1 1 d . . . . .
C3 C 0.3578(8) 0.4947(10) 0.4666(9) 0.046(2) Uani 1 1 d . . . . .
C4 C -0.0367(9) 0.2530(9) 0.4975(10) 0.044(3) Uani 1 1 d . . . . .
C5 C 0.4536(9) 0.5407(12) 0.5929(10) 0.058(3) Uani 1 1 d . . . . .
H5 H 0.422679 0.568110 0.654242 0.069 Uiso 1 1 calc R . . . .
C6 C 0.5951(10) 0.5458(12) 0.6278(10) 0.056(3) Uani 1 1 d . . . . .
C7 C 0.3033(9) 0.7597(8) 0.8592(9) 0.042(2) Uani 1 1 d . . . . .
C8 C 0.0021(12) 0.0739(10) 0.6071(10) 0.052(3) Uani 1 1 d . . . . .
H8 H 0.003119 0.123178 0.678322 0.062 Uiso 1 1 calc R . . . .
C9 C 0.0239(11) -0.0453(10) 0.6132(9) 0.047(2) Uani 1 1 d . . . . .
C10 C 0.0509(19) 0.1778(16) 0.9908(18) 0.090(5) Uani 1 1 d . . . . .
H10A H 0.014304 0.176500 1.055374 0.135 Uiso 1 1 calc GR . . . .
H10B H 0.149978 0.189373 1.028915 0.135 Uiso 1 1 calc GR . . . .
H10C H 0.008375 0.100107 0.929844 0.135 Uiso 1 1 calc GR . . . .
C11 C 0.4019(9) 0.8853(9) 0.9309(10) 0.049(3) Uani 1 1 d D . . . .
C12 C 0.3620(10) 0.9671(11) 0.9910(12) 0.064(3) Uani 1 1 d D . . . .
H12 H 0.271823 0.947291 0.988074 0.077 Uiso 1 1 calc R . . A 2
C13 C 0.3123(14) 0.3302(13) 0.7187(14) 0.087(5) Uani 1 1 d D U . . .
H13 H 0.245451 0.283464 0.640821 0.104 Uiso 1 1 calc R . . . .
C14 C 0.5435(10) 0.9118(11) 0.9378(13) 0.069(4) Uani 1 1 d . . . . .
C15 C -0.1258(15) 0.2798(19) 0.8616(18) 0.095(5) Uani 1 1 d . . . . .
H15A H -0.167709 0.287709 0.921865 0.142 Uiso 1 1 calc GR . . . .
H15B H -0.175068 0.202887 0.800195 0.142 Uiso 1 1 calc GR . . . .
H15C H -0.130495 0.348620 0.819265 0.142 Uiso 1 1 calc GR . . . .
C16 C 0.1177(15) 0.3699(16) 0.9309(14) 0.070(4) Uani 1 1 d . . . . .
H16 H 0.209413 0.368424 0.975686 0.084 Uiso 1 1 calc R . . . .
C17 C 0.436(3) 0.179(2) 0.695(3) 0.165(9) Uani 1 1 d D U . . .
H17A H 0.522696 0.161895 0.741424 0.248 Uiso 1 1 calc R . . . .
H17B H 0.360001 0.109698 0.683182 0.248 Uiso 1 1 calc R . . . .
H17C H 0.432348 0.193490 0.613835 0.248 Uiso 1 1 calc R . . . .
C18 C 0.534(2) 0.363(3) 0.888(2) 0.150(10) Uani 1 1 d D U . . .
H18A H 0.608109 0.322172 0.909818 0.225 Uiso 1 1 calc R . . . .
H18B H 0.568441 0.446073 0.879987 0.225 Uiso 1 1 calc R . . . .
H18C H 0.497670 0.365378 0.952535 0.225 Uiso 1 1 calc R . . . .
N1 N 0.0204(11) 0.2799(11) 0.9277(10) 0.065(3) Uani 1 1 d . . . . .
N2 N 0.4236(14) 0.2934(14) 0.7679(16) 0.101(5) Uani 1 1 d . U . . .
O1 O 0.5947(9) 0.8222(10) 0.8820(13) 0.113(5) Uani 1 1 d D . . . .
H1 H 0.530015 0.761081 0.838988 0.169 Uiso 1 1 calc R . . . .
O2 O -0.0100(7) 0.3206(6) 0.6043(7) 0.0468(17) Uani 1 1 d . . . . .
O3 O 0.1625(7) 0.5067(7) 0.5199(7) 0.0527(18) Uani 1 1 d . . . . .
O4 O -0.0722(7) 0.2861(7) 0.3921(7) 0.0481(17) Uani 1 1 d . . . . .
O5 O 0.0976(10) 0.4613(10) 0.8769(8) 0.068(2) Uani 1 1 d . . . . .
O6 O 0.1219(6) 0.4585(8) 0.3156(7) 0.0521(18) Uani 1 1 d . . . . .
O7 O 0.1861(6) 0.7291(6) 0.8677(6) 0.0481(17) Uani 1 1 d . . . . .
O8 O 0.3388(7) 0.6857(7) 0.7913(8) 0.060(2) Uani 1 1 d . . . . .
O9 O 0.0442(12) -0.0810(9) 0.7259(8) 0.072(3) Uani 1 1 d . . . . .
H9 H 0.059861 -0.150011 0.721877 0.108 Uiso 1 1 calc GR . . . .
O11 O 0.2874(8) 0.4229(9) 0.7671(10) 0.073(2) Uani 1 1 d . U . . .
O12 O 0.6835(8) 0.5878(12) 0.7535(8) 0.086(3) Uani 1 1 d . . . . .
H12A H 0.762976 0.586367 0.762244 0.129 Uiso 1 1 calc R . . . .
Tb1 Tb 0.10866(3) 0.53481(3) 0.69822(3) 0.0370(2) 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
C1 C4 1.526(14) . ?
C1 C8 1.398(17) . ?
C1 C9 1.418(12) 2_556 ?
C2 C3 1.505(11) . ?
C2 O3 1.265(11) . ?
C2 O6 1.281(12) . ?
C3 C5 1.403(13) . ?
C3 C6 1.421(13) 2_666 ?
C4 O2 1.270(11) . ?
C4 O4 1.263(14) . ?
C5 H5 0.9300 . ?
C5 C6 1.401(12) . ?
C6 O12 1.375(13) . ?
C7 C11 1.505(12) . ?
C7 O7 1.272(11) . ?
C7 O8 1.277(11) . ?
C8 H8 0.9300 . ?
C8 C9 1.403(16) . ?
C9 O9 1.363(14) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C10 N1 1.45(2) . ?
C11 C12 1.311(14) . ?
C11 C14 1.450(13) . ?
C12 H12 0.9300 . ?
C12 C14 1.453(14) 2_677 ?
C13 H13 0.9300 . ?
C13 N2 1.288(19) . ?
C13 O11 1.240(16) . ?
C14 O1 1.427(12) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C15 N1 1.466(18) . ?
C16 H16 0.9300 . ?
C16 N1 1.280(19) . ?
C16 O5 1.27(2) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C17 N2 1.50(3) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C18 N2 1.45(2) . ?
O1 H1 0.8200 . ?
O2 Tb1 2.385(6) . ?
O3 Tb1 2.337(7) . ?
O4 Tb1 2.401(8) 2_566 ?
O5 Tb1 2.347(10) . ?
O6 Tb1 2.422(6) 2_566 ?
O7 Tb1 2.517(6) . ?
O8 Tb1 2.455(6) . ?
O9 H9 0.8200 . ?
O11 Tb1 2.433(8) . ?
O12 H12A 0.8200 . ?

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
C8 C1 C4 118.8(8) . . ?
C8 C1 C9 119.8(9) . 2_556 ?
C9 C1 C4 121.3(10) 2_556 . ?
O3 C2 C3 119.8(9) . . ?
O3 C2 O6 121.2(8) . . ?
O6 C2 C3 119.0(8) . . ?
C5 C3 C2 119.7(8) . . ?
C5 C3 C6 119.7(8) . 2_666 ?
C6 C3 C2 120.6(8) 2_666 . ?
O2 C4 C1 117.3(10) . . ?
O4 C4 C1 116.6(8) . . ?
O4 C4 O2 126.2(9) . . ?
C3 C5 H5 119.6 . . ?
C6 C5 C3 120.9(8) . . ?
C6 C5 H5 119.6 . . ?
C5 C6 C3 119.4(8) . 2_666 ?
O12 C6 C3 122.2(8) . 2_666 ?
O12 C6 C5 118.4(8) . . ?
O7 C7 C11 119.2(7) . . ?
O7 C7 O8 121.2(8) . . ?
O8 C7 C11 119.5(8) . . ?
C1 C8 H8 119.3 . . ?
C1 C8 C9 121.3(9) . . ?
C9 C8 H8 119.3 . . ?
C8 C9 C1 118.9(10) . 2_556 ?
O9 C9 C1 124.9(10) . 2_556 ?
O9 C9 C8 116.2(8) . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N1 C10 H10A 109.5 . . ?
N1 C10 H10B 109.5 . . ?
N1 C10 H10C 109.5 . . ?
C12 C11 C7 120.3(8) . . ?
C12 C11 C14 120.7(8) . . ?
C14 C11 C7 119.0(8) . . ?
C11 C12 H12 119.5 . . ?
C11 C12 C14 121.1(9) . 2_677 ?
C14 C12 H12 119.5 2_677 . ?
N2 C13 H13 117.4 . . ?
O11 C13 H13 117.4 . . ?
O11 C13 N2 125.1(14) . . ?
C11 C14 C12 118.2(8) . 2_677 ?
O1 C14 C11 122.7(9) . . ?
O1 C14 C12 119.1(8) . 2_677 ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N1 C15 H15A 109.5 . . ?
N1 C15 H15B 109.5 . . ?
N1 C15 H15C 109.5 . . ?
N1 C16 H16 117.8 . . ?
O5 C16 H16 117.8 . . ?
O5 C16 N1 124.5(14) . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N2 C17 H17A 109.5 . . ?
N2 C17 H17B 109.5 . . ?
N2 C17 H17C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N2 C18 H18A 109.5 . . ?
N2 C18 H18B 109.5 . . ?
N2 C18 H18C 109.5 . . ?
C10 N1 C15 118.5(13) . . ?
C16 N1 C10 121.6(14) . . ?
C16 N1 C15 119.8(15) . . ?
C13 N2 C17 117.5(16) . . ?
C13 N2 C18 120.7(16) . . ?
C18 N2 C17 121.7(19) . . ?
C14 O1 H1 109.5 . . ?
C4 O2 Tb1 132.7(7) . . ?
C2 O3 Tb1 172.0(7) . . ?
C4 O4 Tb1 141.2(6) . 2_566 ?
C16 O5 Tb1 140.2(8) . . ?
C2 O6 Tb1 108.6(5) . 2_566 ?
C7 O7 Tb1 91.2(5) . . ?
C7 O8 Tb1 93.9(5) . . ?
C9 O9 H9 109.5 . . ?
C13 O11 Tb1 135.3(9) . . ?
C6 O12 H12A 109.5 . . ?
O2 Tb1 O4 127.9(2) . 2_566 ?
O2 Tb1 O6 81.3(2) . 2_566 ?
O2 Tb1 O7 153.3(3) . . ?
O2 Tb1 O8 143.8(2) . . ?
O2 Tb1 O11 75.0(3) . . ?
O3 Tb1 O2 78.5(3) . . ?
O3 Tb1 O4 75.2(3) . 2_566 ?
O3 Tb1 O5 147.6(3) . . ?
O3 Tb1 O6 122.8(2) . 2_566 ?
O3 Tb1 O7 128.1(2) . . ?
O3 Tb1 O8 83.1(3) . . ?
O3 Tb1 O11 78.9(3) . . ?
O4 Tb1 O6 76.6(3) 2_566 2_566 ?
O4 Tb1 O7 68.5(2) 2_566 . ?
O4 Tb1 O8 75.4(3) 2_566 . ?
O4 Tb1 O11 139.5(3) 2_566 . ?
O5 Tb1 O2 79.7(3) . . ?
O5 Tb1 O4 137.1(3) . 2_566 ?
O5 Tb1 O6 76.7(3) . 2_566 ?
O5 Tb1 O7 75.5(3) . . ?
O5 Tb1 O8 101.2(3) . . ?
O5 Tb1 O11 72.4(4) . . ?
O6 Tb1 O7 83.4(2) 2_566 . ?
O6 Tb1 O8 134.5(2) 2_566 . ?
O6 Tb1 O11 143.9(3) 2_566 . ?
O8 Tb1 O7 53.0(2) . . ?
O11 Tb1 O7 106.2(3) . . ?
O11 Tb1 O8 71.0(3) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O1 H1 O8 0.82 1.89 2.599(11) 144.7 . yes
O9 H9 O4 0.82 1.95 2.651(10) 143.1 2_556 yes
O12 H12A O6 0.82 1.87 2.599(10) 146.6 2_666 yes

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
C1 C4 O2 Tb1 139.1(7) . . . . ?
C1 C4 O4 Tb1 -175.3(6) . . . 2_566 ?
C1 C8 C9 C1 -0.5(17) . . . 2_556 ?
C1 C8 C9 O9 -179.5(10) . . . . ?
C2 C3 C5 C6 177.8(12) . . . . ?
C3 C2 O6 Tb1 -176.9(7) . . . 2_566 ?
C3 C5 C6 C3 1(2) . . . 2_666 ?
C3 C5 C6 O12 -177.9(13) . . . . ?
C4 C1 C8 C9 -177.0(9) . . . . ?
C6 C3 C5 C6 -1(2) 2_666 . . . ?
C7 C11 C12 C14 179.1(13) . . . 2_677 ?
C7 C11 C14 C12 -179.1(12) . . . 2_677 ?
C7 C11 C14 O1 -2(2) . . . . ?
C8 C1 C4 O2 8.9(13) . . . . ?
C8 C1 C4 O4 -172.6(9) . . . . ?
C9 C1 C4 O2 -168.6(9) 2_556 . . . ?
C9 C1 C4 O4 9.9(13) 2_556 . . . ?
C9 C1 C8 C9 0.6(17) 2_556 . . . ?
C11 C7 O7 Tb1 172.6(9) . . . . ?
C11 C7 O8 Tb1 -172.4(9) . . . . ?
C12 C11 C14 C12 -2(2) . . . 2_677 ?
C12 C11 C14 O1 175.1(15) . . . . ?
C14 C11 C12 C14 2(2) . . . 2_677 ?
N1 C16 O5 Tb1 -104.5(17) . . . . ?
N2 C13 O11 Tb1 172.0(11) . . . . ?
O2 C4 O4 Tb1 3.0(16) . . . 2_566 ?
O3 C2 C3 C5 -8.0(16) . . . . ?
O3 C2 C3 C6 170.6(11) . . . 2_666 ?
O3 C2 O6 Tb1 2.7(12) . . . 2_566 ?
O4 C4 O2 Tb1 -39.2(13) . . . . ?
O5 C16 N1 C10 179.5(13) . . . . ?
O5 C16 N1 C15 -2(2) . . . . ?
O6 C2 C3 C5 171.6(11) . . . . ?
O6 C2 C3 C6 -9.8(16) . . . 2_666 ?
O7 C7 C11 C12 -6.8(18) . . . . ?
O7 C7 C11 C14 170.0(12) . . . . ?
O7 C7 O8 Tb1 7.8(11) . . . . ?
O8 C7 C11 C12 173.4(12) . . . . ?
O8 C7 C11 C14 -9.7(17) . . . . ?
O8 C7 O7 Tb1 -7.6(11) . . . . ?
O11 C13 N2 C17 -179.7(11) . . . . ?
O11 C13 N2 C18 -1.2(19) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.500 0.000 0.500 213.3 0.0 ?


_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 1.225
_oxdiff_exptl_absorpt_empirical_full_min 0.723

# start Validation Reply Form
_vrf_PLAT027_SION2_280K_cool     
;
PROBLEM: _diffrn_reflns_theta_full value (too) Low ......      26.00 Degree
RESPONSE: Our value of max sin(theta)/lambda of 0.56 is close to the recommended 
		  value of 0.60. Higer values of sin(theta)/lambda were not available due 
		  to the beamline experimental set-up limitations.
;
_vrf_PLAT029_SION2_280K_cool     
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.713 Why?  
RESPONSE: The data were collected upon the spindle rotation. Therefore, a 
		  limited portion of the reciprocal space could be probed.
;
# 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_SION2_140K_cool
_database_code_depnum_ccdc_archive 'CCDC 1941021'
loop_
_audit_author_name
_audit_author_address
'Andrzej Gladysiak'
;Ecole polytechnique federale de Lausanne
Switzerland
;
_audit_update_record             
;
2019-07-16 deposited with the CCDC.	2019-08-12 downloaded from the CCDC.
;
_audit_creation_date             2019-05-27
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C18 H20 N2 O11 Tb'
_chemical_formula_sum            'C18 H20 N2 O11 Tb'
_chemical_formula_weight         599.28
_chemical_melting_point          ?
_chemical_oxdiff_formula         C21H27N3O12Tb
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0045 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'
N N 0.0083 0.0040 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0145 0.0076 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.0972 4.9386 '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                   10.6338(6)
_cell_length_b                   11.1768(5)
_cell_length_c                   11.3943(5)
_cell_angle_alpha                96.944(4)
_cell_angle_beta                 110.943(5)
_cell_angle_gamma                101.427(4)
_cell_volume                     1212.21(11)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3195
_cell_measurement_temperature    140.0
_cell_measurement_theta_max      31.9400
_cell_measurement_theta_min      2.0700
_shelx_estimated_absorpt_T_max   0.775
_shelx_estimated_absorpt_T_min   0.514
_exptl_absorpt_coefficient_mu    3.834
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83535
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.642
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             590
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0086
_diffrn_reflns_av_unetI/netI     0.0132
_diffrn_reflns_Laue_measured_fraction_full 0.713
_diffrn_reflns_Laue_measured_fraction_max 0.545
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6761
_diffrn_reflns_point_group_measured_fraction_full 0.713
_diffrn_reflns_point_group_measured_fraction_max 0.545
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         32.139
_diffrn_reflns_theta_min         2.097
_diffrn_ambient_temperature      140.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            PILATUS2M
_diffrn_measured_fraction_theta_full 0.713
_diffrn_measured_fraction_theta_max 0.545
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      0.00 360.00   1.00    1.00    --    0.00   0.00   0.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  PILATUS@SNBL
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0667609000
_diffrn_orient_matrix_UB_12      -0.0037037000
_diffrn_orient_matrix_UB_13      -0.0131931000
_diffrn_orient_matrix_UB_21      0.0459147000
_diffrn_orient_matrix_UB_22      0.0516831000
_diffrn_orient_matrix_UB_23      0.0620589000
_diffrn_orient_matrix_UB_31      0.0109835000
_diffrn_orient_matrix_UB_32      -0.0516933000
_diffrn_orient_matrix_UB_33      0.0406474000
_diffrn_radiation_monochromator  'Si (111)'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.78405
_diffrn_source                   
'European Synchrotron Radiation Facility, BM01 beamline'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3303
_reflns_number_total             3466
_reflns_odcompleteness_completeness 62.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     29.34
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         5.904
_refine_diff_density_min         -0.791
_refine_diff_density_rms         0.218
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     292
_refine_ls_number_reflns         3466
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.0627
_refine_ls_R_factor_gt           0.0609
_refine_ls_restrained_S_all      6.441
_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)+(0.1325P)²+4.8710P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1662
_refine_ls_wR_factor_ref         0.1704
_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
 C17-C13 \\sim C13-C18
 with sigma of 0.02
 C12_$6-O1 \\sim O1-C11
 with sigma of 0.05
3. Restrained planarity
 C13, C17, C18, N2, O11
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C17) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
5.a Me refined with riding coordinates:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C)
5.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C8(H8), C12(H12), C13(H13), C16(H16)
5.c Tetrahedral OH refined with riding coordinates:
 O1(H1), O12(H12A)
5.d Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C15(H15A,H15B,H15C)
5.e Idealised tetrahedral OH refined as rotating group:
 O9(H9)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
C1 C -0.0208(8) 0.1210(8) 0.4965(9) 0.037(2) Uani 1 1 d . . . . .
C2 C 0.2050(8) 0.4853(8) 0.4310(9) 0.037(2) Uani 1 1 d . . . . .
C3 C 0.3575(8) 0.4941(9) 0.4663(8) 0.036(2) Uani 1 1 d . . . . .
C4 C -0.0362(8) 0.2522(8) 0.4989(10) 0.038(2) Uani 1 1 d . . . . .
C5 C 0.4507(9) 0.5373(11) 0.5938(9) 0.046(3) Uani 1 1 d . . . . .
H5 H 0.417814 0.564150 0.657105 0.055 Uiso 1 1 calc R . . . .
C6 C 0.5939(9) 0.5419(11) 0.6305(9) 0.048(3) Uani 1 1 d . . . . .
C7 C 0.3016(8) 0.7597(8) 0.8598(9) 0.034(2) Uani 1 1 d . . . . .
C8 C 0.0036(10) 0.0736(10) 0.6092(10) 0.043(3) Uani 1 1 d . . . . .
H8 H 0.005759 0.123868 0.683695 0.051 Uiso 1 1 calc R . . . .
C9 C 0.0248(10) -0.0451(9) 0.6148(9) 0.040(2) Uani 1 1 d . . . . .
C10 C 0.0503(13) 0.1779(13) 0.9924(14) 0.061(4) Uani 1 1 d . . . . .
H10A H 0.017685 0.179721 1.062662 0.092 Uiso 1 1 calc GR . . . .
H10B H 0.151115 0.186679 1.026970 0.092 Uiso 1 1 calc GR . . . .
H10C H 0.002437 0.098277 0.930404 0.092 Uiso 1 1 calc GR . . . .
C11 C 0.4016(8) 0.8855(9) 0.9312(9) 0.041(2) Uani 1 1 d D . . . .
C12 C 0.3624(9) 0.9694(10) 0.9926(12) 0.054(3) Uani 1 1 d D . . . .
H12 H 0.270491 0.950124 0.990758 0.065 Uiso 1 1 calc R . . A 2
C13 C 0.3100(12) 0.3296(11) 0.7213(12) 0.067(4) Uani 1 1 d D . . . .
H13 H 0.241539 0.280983 0.641512 0.080 Uiso 1 1 calc R . . . .
C14 C 0.5429(9) 0.9095(10) 0.9371(11) 0.053(3) Uani 1 1 d . . . . .
C15 C -0.1270(12) 0.2752(15) 0.8589(14) 0.068(4) Uani 1 1 d . . . . .
H15A H -0.168961 0.294140 0.920417 0.102 Uiso 1 1 calc GR . . . .
H15B H -0.176899 0.191771 0.805121 0.102 Uiso 1 1 calc GR . . . .
H15C H -0.133374 0.337105 0.804381 0.102 Uiso 1 1 calc GR . . . .
C16 C 0.1177(12) 0.3729(14) 0.9343(12) 0.056(3) Uani 1 1 d . . . . .
H16 H 0.211510 0.372501 0.981234 0.067 Uiso 1 1 calc R . . . .
C17 C 0.436(2) 0.177(2) 0.705(2) 0.130(8) Uani 1 1 d D U . . .
H17A H 0.525176 0.160335 0.753625 0.195 Uiso 1 1 calc R . . . .
H17B H 0.359266 0.106795 0.696628 0.195 Uiso 1 1 calc R . . . .
H17C H 0.431206 0.186591 0.619212 0.195 Uiso 1 1 calc R . . . .
C18 C 0.5318(16) 0.367(2) 0.8936(17) 0.098(6) Uani 1 1 d D . . . .
H18A H 0.609213 0.327093 0.919360 0.148 Uiso 1 1 calc R . . . .
H18B H 0.565554 0.450908 0.882672 0.148 Uiso 1 1 calc R . . . .
H18C H 0.493622 0.371129 0.960106 0.148 Uiso 1 1 calc R . . . .
N1 N 0.0205(9) 0.2793(9) 0.9290(9) 0.049(2) Uani 1 1 d . . . . .
N2 N 0.4240(11) 0.2933(12) 0.7735(12) 0.074(4) Uani 1 1 d . . . . .
O1 O 0.5940(8) 0.8200(9) 0.8813(11) 0.082(3) Uani 1 1 d D . . . .
H1 H 0.527815 0.757270 0.837264 0.123 Uiso 1 1 calc R . . . .
O2 O -0.0088(6) 0.3215(6) 0.6067(6) 0.0373(15) Uani 1 1 d . . . . .
O3 O 0.1597(6) 0.5051(6) 0.5177(7) 0.0398(16) Uani 1 1 d . . . . .
O4 O -0.0717(6) 0.2864(6) 0.3919(6) 0.0390(16) Uani 1 1 d . . . . .
O5 O 0.0976(8) 0.4646(8) 0.8818(7) 0.052(2) Uani 1 1 d . . . . .
O6 O 0.1224(6) 0.4577(7) 0.3109(7) 0.0413(16) Uani 1 1 d . . . . .
O7 O 0.1855(6) 0.7306(6) 0.8704(6) 0.0387(16) Uani 1 1 d . . . . .
O8 O 0.3370(6) 0.6850(6) 0.7909(7) 0.0458(19) Uani 1 1 d . . . . .
O9 O 0.0469(9) -0.0812(8) 0.7299(7) 0.054(2) Uani 1 1 d . . . . .
H9 H 0.056468 -0.154255 0.723166 0.080 Uiso 1 1 calc GR . . . .
O11 O 0.2866(7) 0.4235(8) 0.7701(8) 0.058(2) Uani 1 1 d . . . . .
O12 O 0.6797(7) 0.5832(10) 0.7572(7) 0.063(3) Uani 1 1 d . . . . .
H12A H 0.761491 0.581998 0.766902 0.095 Uiso 1 1 calc R . . . .
Tb1 Tb 0.10720(3) 0.53532(3) 0.69956(3) 0.0312(2) 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
C1 C4 1.506(14) . ?
C1 C8 1.406(16) . ?
C1 C9 1.420(12) 2_556 ?
C2 C3 1.504(10) . ?
C2 O3 1.259(11) . ?
C2 O6 1.293(11) . ?
C3 C5 1.392(12) . ?
C3 C6 1.425(12) 2_666 ?
C4 O2 1.273(10) . ?
C4 O4 1.271(13) . ?
C5 H5 0.9500 . ?
C5 C6 1.416(12) . ?
C6 O12 1.363(11) . ?
C7 C11 1.511(11) . ?
C7 O7 1.266(11) . ?
C7 O8 1.277(10) . ?
C8 H8 0.9500 . ?
C8 C9 1.394(15) . ?
C9 O9 1.372(14) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C10 N1 1.444(19) . ?
C11 C12 1.322(13) . ?
C11 C14 1.448(12) . ?
C12 H12 0.9500 . ?
C12 C14 1.452(13) 2_677 ?
C13 H13 0.9500 . ?
C13 N2 1.313(17) . ?
C13 O11 1.239(14) . ?
C14 O1 1.418(12) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C15 N1 1.473(15) . ?
C16 H16 0.9500 . ?
C16 N1 1.295(17) . ?
C16 O5 1.264(17) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C17 N2 1.49(2) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C18 N2 1.447(19) . ?
O1 H1 0.8400 . ?
O2 Tb1 2.375(6) . ?
O3 Tb1 2.335(6) . ?
O4 Tb1 2.391(8) 2_566 ?
O5 Tb1 2.338(9) . ?
O6 Tb1 2.419(6) 2_566 ?
O7 Tb1 2.518(6) . ?
O8 Tb1 2.448(6) . ?
O9 H9 0.8400 . ?
O11 Tb1 2.437(8) . ?
O12 H12A 0.8400 . ?

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
C8 C1 C4 119.1(8) . . ?
C8 C1 C9 118.9(9) . 2_556 ?
C9 C1 C4 121.9(9) 2_556 . ?
O3 C2 C3 120.1(8) . . ?
O3 C2 O6 121.1(7) . . ?
O6 C2 C3 118.8(7) . . ?
C5 C3 C2 119.8(7) . . ?
C5 C3 C6 120.2(7) . 2_666 ?
C6 C3 C2 120.0(7) 2_666 . ?
O2 C4 C1 118.4(9) . . ?
O4 C4 C1 116.7(8) . . ?
O4 C4 O2 124.9(9) . . ?
C3 C5 H5 119.5 . . ?
C3 C5 C6 121.0(8) . . ?
C6 C5 H5 119.5 . . ?
C5 C6 C3 118.8(8) . 2_666 ?
O12 C6 C3 122.9(8) . 2_666 ?
O12 C6 C5 118.3(8) . . ?
O7 C7 C11 119.2(7) . . ?
O7 C7 O8 121.7(7) . . ?
O8 C7 C11 119.1(8) . . ?
C1 C8 H8 119.1 . . ?
C9 C8 C1 121.9(8) . . ?
C9 C8 H8 119.1 . . ?
C8 C9 C1 119.2(10) . 2_556 ?
O9 C9 C1 124.2(9) . 2_556 ?
O9 C9 C8 116.5(8) . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N1 C10 H10A 109.5 . . ?
N1 C10 H10B 109.5 . . ?
N1 C10 H10C 109.5 . . ?
C12 C11 C7 120.3(8) . . ?
C12 C11 C14 120.8(8) . . ?
C14 C11 C7 118.8(8) . . ?
C11 C12 H12 119.4 . . ?
C11 C12 C14 121.3(8) . 2_677 ?
C14 C12 H12 119.4 2_677 . ?
N2 C13 H13 118.1 . . ?
O11 C13 H13 118.1 . . ?
O11 C13 N2 123.8(11) . . ?
C11 C14 C12 117.9(8) . 2_677 ?
O1 C14 C11 123.4(8) . . ?
O1 C14 C12 118.7(8) . 2_677 ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N1 C15 H15A 109.5 . . ?
N1 C15 H15B 109.5 . . ?
N1 C15 H15C 109.5 . . ?
N1 C16 H16 117.4 . . ?
O5 C16 H16 117.4 . . ?
O5 C16 N1 125.2(12) . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N2 C17 H17A 109.5 . . ?
N2 C17 H17B 109.5 . . ?
N2 C17 H17C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N2 C18 H18A 109.5 . . ?
N2 C18 H18B 109.5 . . ?
N2 C18 H18C 109.5 . . ?
C10 N1 C15 117.5(10) . . ?
C16 N1 C10 122.5(11) . . ?
C16 N1 C15 119.9(13) . . ?
C13 N2 C17 117.7(13) . . ?
C13 N2 C18 119.6(12) . . ?
C18 N2 C17 122.7(15) . . ?
C14 O1 H1 109.5 . . ?
C4 O2 Tb1 133.5(6) . . ?
C2 O3 Tb1 171.1(6) . . ?
C4 O4 Tb1 141.8(5) . 2_566 ?
C16 O5 Tb1 138.7(7) . . ?
C2 O6 Tb1 107.2(5) . 2_566 ?
C7 O7 Tb1 90.8(5) . . ?
C7 O8 Tb1 93.8(5) . . ?
C9 O9 H9 109.5 . . ?
C13 O11 Tb1 134.7(8) . . ?
C6 O12 H12A 109.5 . . ?
O2 Tb1 O4 128.5(2) . 2_566 ?
O2 Tb1 O6 81.9(2) . 2_566 ?
O2 Tb1 O7 153.7(2) . . ?
O2 Tb1 O8 143.1(2) . . ?
O2 Tb1 O11 74.7(2) . . ?
O3 Tb1 O2 78.0(2) . . ?
O3 Tb1 O4 75.3(2) . 2_566 ?
O3 Tb1 O5 147.8(3) . . ?
O3 Tb1 O6 123.1(2) . 2_566 ?
O3 Tb1 O7 128.2(2) . . ?
O3 Tb1 O8 83.1(2) . . ?
O3 Tb1 O11 79.3(3) . . ?
O4 Tb1 O6 77.2(2) 2_566 2_566 ?
O4 Tb1 O7 68.4(2) 2_566 . ?
O4 Tb1 O8 75.2(2) 2_566 . ?
O4 Tb1 O11 139.4(3) 2_566 . ?
O5 Tb1 O2 80.1(3) . . ?
O5 Tb1 O4 136.8(3) . 2_566 ?
O5 Tb1 O6 76.3(3) . 2_566 ?
O5 Tb1 O7 75.2(3) . . ?
O5 Tb1 O8 101.0(3) . . ?
O5 Tb1 O11 72.2(3) . . ?
O6 Tb1 O7 83.4(2) 2_566 . ?
O6 Tb1 O8 134.6(2) 2_566 . ?
O6 Tb1 O11 143.3(3) 2_566 . ?
O8 Tb1 O7 53.1(2) . . ?
O11 Tb1 O7 105.9(2) . . ?
O11 Tb1 O8 70.8(3) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O1 H1 O8 0.84 1.88 2.605(10) 143.9 . yes
O9 H9 O4 0.84 1.92 2.643(10) 142.8 2_556 yes
O12 H12A O6 0.84 1.85 2.588(9) 146.4 2_666 yes

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
C1 C4 O2 Tb1 139.4(7) . . . . ?
C1 C4 O4 Tb1 -174.9(6) . . . 2_566 ?
C1 C8 C9 C1 -0.4(15) . . . 2_556 ?
C1 C8 C9 O9 -179.7(8) . . . . ?
C2 C3 C5 C6 177.5(11) . . . . ?
C3 C2 O6 Tb1 -177.1(7) . . . 2_566 ?
C3 C5 C6 C3 2(2) . . . 2_666 ?
C3 C5 C6 O12 -178.9(12) . . . . ?
C4 C1 C8 C9 -177.2(8) . . . . ?
C6 C3 C5 C6 -2(2) 2_666 . . . ?
C7 C11 C12 C14 179.4(12) . . . 2_677 ?
C7 C11 C14 C12 -179.4(11) . . . 2_677 ?
C7 C11 C14 O1 -1.4(19) . . . . ?
C8 C1 C4 O2 9.0(12) . . . . ?
C8 C1 C4 O4 -173.3(8) . . . . ?
C9 C1 C4 O2 -168.6(8) 2_556 . . . ?
C9 C1 C4 O4 9.1(12) 2_556 . . . ?
C9 C1 C8 C9 0.4(15) 2_556 . . . ?
C11 C7 O7 Tb1 172.7(9) . . . . ?
C11 C7 O8 Tb1 -172.5(8) . . . . ?
C12 C11 C14 C12 -3(2) . . . 2_677 ?
C12 C11 C14 O1 175.2(13) . . . . ?
C14 C11 C12 C14 3(2) . . . 2_677 ?
N1 C16 O5 Tb1 -101.9(14) . . . . ?
N2 C13 O11 Tb1 172.4(9) . . . . ?
O2 C4 O4 Tb1 2.6(15) . . . 2_566 ?
O3 C2 C3 C5 -7.0(15) . . . . ?
O3 C2 C3 C6 172.9(10) . . . 2_666 ?
O3 C2 O6 Tb1 2.6(11) . . . 2_566 ?
O4 C4 O2 Tb1 -38.0(12) . . . . ?
O5 C16 N1 C10 -179.3(11) . . . . ?
O5 C16 N1 C15 -0.7(17) . . . . ?
O6 C2 C3 C5 172.8(10) . . . . ?
O6 C2 C3 C6 -7.3(15) . . . 2_666 ?
O7 C7 C11 C12 -7.3(17) . . . . ?
O7 C7 C11 C14 169.2(11) . . . . ?
O7 C7 O8 Tb1 8.1(11) . . . . ?
O8 C7 C11 C12 173.2(12) . . . . ?
O8 C7 C11 C14 -10.2(16) . . . . ?
O8 C7 O7 Tb1 -7.8(10) . . . . ?
O11 C13 N2 C17 178.7(11) . . . . ?
O11 C13 N2 C18 -1.3(17) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.500 0.000 0.500 211.5 0.0 ?


_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 1.168
_oxdiff_exptl_absorpt_empirical_full_min 0.899

# start Validation Reply Form
_vrf_PLAT027_SION2_140K_cool     
;
PROBLEM: _diffrn_reflns_theta_full value (too) Low ......      26.00 Degree
RESPONSE: Our value of max sin(theta)/lambda of 0.56 is close to the recommended 
		  value of 0.60. Higer values of sin(theta)/lambda were not available due 
		  to the beamline experimental set-up limitations. 
;
_vrf_PLAT029_SION2_140K_cool     
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.713 Why?  
RESPONSE: The data were collected upon the spindle rotation. Therefore, a 
		  limited portion of the reciprocal space could be probed.
;
# 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_SION2_220K_cool
_database_code_depnum_ccdc_archive 'CCDC 1941019'
loop_
_audit_author_name
_audit_author_address
'Andrzej Gladysiak'
;Ecole polytechnique federale de Lausanne
Switzerland
;
_audit_update_record             
;
2019-07-16 deposited with the CCDC.	2019-08-12 downloaded from the CCDC.
;
_audit_creation_date             2019-05-27
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C18 H20 N2 O11 Tb'
_chemical_formula_sum            'C18 H20 N2 O11 Tb'
_chemical_formula_weight         599.28
_chemical_melting_point          ?
_chemical_oxdiff_formula         C21H27N3O12Tb
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0045 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'
N N 0.0083 0.0040 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0145 0.0076 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.0972 4.9386 '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                   10.6410(6)
_cell_length_b                   11.1651(5)
_cell_length_c                   11.4787(5)
_cell_angle_alpha                96.891(4)
_cell_angle_beta                 111.171(5)
_cell_angle_gamma                101.441(4)
_cell_volume                     1218.74(11)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3163
_cell_measurement_temperature    220.0
_cell_measurement_theta_max      32.2410
_cell_measurement_theta_min      2.0790
_shelx_estimated_absorpt_T_max   0.776
_shelx_estimated_absorpt_T_min   0.516
_exptl_absorpt_coefficient_mu    3.814
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82784
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.633
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             590
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0087
_diffrn_reflns_av_unetI/netI     0.0133
_diffrn_reflns_Laue_measured_fraction_full 0.713
_diffrn_reflns_Laue_measured_fraction_max 0.543
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6812
_diffrn_reflns_point_group_measured_fraction_full 0.713
_diffrn_reflns_point_group_measured_fraction_max 0.543
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         32.248
_diffrn_reflns_theta_min         2.100
_diffrn_ambient_temperature      220.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            PILATUS2M
_diffrn_measured_fraction_theta_full 0.713
_diffrn_measured_fraction_theta_max 0.543
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      0.00 360.00   1.00    1.00    --    0.00   0.00   0.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  PILATUS@SNBL
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0667511000
_diffrn_orient_matrix_UB_12      -0.0036114000
_diffrn_orient_matrix_UB_13      -0.0129825000
_diffrn_orient_matrix_UB_21      0.0460903000
_diffrn_orient_matrix_UB_22      0.0515501000
_diffrn_orient_matrix_UB_23      0.0618902000
_diffrn_orient_matrix_UB_31      0.0109526000
_diffrn_orient_matrix_UB_32      -0.0519508000
_diffrn_orient_matrix_UB_33      0.0401624000
_diffrn_radiation_monochromator  'Si (111)'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.78405
_diffrn_source                   
'European Synchrotron Radiation Facility, BM01 beamline'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3337
_reflns_number_total             3496
_reflns_odcompleteness_completeness 63.03
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     29.34
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         6.321
_refine_diff_density_min         -1.378
_refine_diff_density_rms         0.238
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     292
_refine_ls_number_reflns         3496
_refine_ls_number_restraints     34
_refine_ls_R_factor_all          0.0700
_refine_ls_R_factor_gt           0.0683
_refine_ls_restrained_S_all      6.330
_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)+(0.1429P)²+5.2724P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1800
_refine_ls_wR_factor_ref         0.1827
_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
 C17-C13 \\sim C13-C18
 with sigma of 0.02
 C12_$8-O1 \\sim O1-C11
 with sigma of 0.05
3. Restrained planarity
 C13, C17, C18, N2, O11
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C17) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
5. Rigid body (RIGU) restrains
 O11, C13, N2, C18, C17
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Me refined with riding coordinates:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C)
6.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C8(H8), C12(H12), C13(H13), C16(H16)
6.c Tetrahedral OH refined with riding coordinates:
 O1(H1), O12(H12A)
6.d Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C15(H15A,H15B,H15C)
6.e Idealised tetrahedral OH refined as rotating group:
 O9(H9)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
C1 C -0.0209(9) 0.1204(9) 0.4968(10) 0.039(2) Uani 1 1 d . . . . .
C2 C 0.2050(8) 0.4854(9) 0.4316(10) 0.040(2) Uani 1 1 d . . . . .
C3 C 0.3573(8) 0.4939(10) 0.4665(10) 0.041(2) Uani 1 1 d . . . . .
C4 C -0.0365(9) 0.2522(9) 0.4983(10) 0.042(3) Uani 1 1 d . . . . .
C5 C 0.4524(10) 0.5394(12) 0.5940(11) 0.053(3) Uani 1 1 d . . . . .
H5 H 0.420849 0.566759 0.656563 0.064 Uiso 1 1 calc R . . . .
C6 C 0.5942(10) 0.5441(12) 0.6286(10) 0.051(3) Uani 1 1 d . . . . .
C7 C 0.3024(9) 0.7596(9) 0.8601(10) 0.039(2) Uani 1 1 d . . . . .
C8 C 0.0024(12) 0.0728(10) 0.6078(10) 0.048(3) Uani 1 1 d . . . . .
H8 H 0.002351 0.121998 0.680268 0.058 Uiso 1 1 calc R . . . .
C9 C 0.0254(11) -0.0448(10) 0.6146(9) 0.041(2) Uani 1 1 d . . . . .
C10 C 0.0495(18) 0.1785(16) 0.9904(17) 0.077(4) Uani 1 1 d . . . . .
H10A H 0.015661 0.178906 1.058357 0.115 Uiso 1 1 calc GR . . . .
H10B H 0.149440 0.187987 1.025967 0.115 Uiso 1 1 calc GR . . . .
H10C H 0.003256 0.099916 0.928638 0.115 Uiso 1 1 calc GR . . . .
C11 C 0.4015(9) 0.8847(9) 0.9323(10) 0.044(3) Uani 1 1 d D . . . .
C12 C 0.3626(10) 0.9676(12) 0.9907(13) 0.058(3) Uani 1 1 d D . . . .
H12 H 0.270874 0.948449 0.986866 0.070 Uiso 1 1 calc R . . A 2
C13 C 0.3108(13) 0.3297(12) 0.7198(13) 0.071(4) Uani 1 1 d D U . . .
H13 H 0.242763 0.281758 0.641197 0.085 Uiso 1 1 calc R . . . .
C14 C 0.5434(10) 0.9101(11) 0.9378(13) 0.062(4) Uani 1 1 d . . . . .
C15 C -0.1265(15) 0.2793(17) 0.8610(17) 0.080(4) Uani 1 1 d . . . . .
H15A H -0.167571 0.293770 0.922629 0.121 Uiso 1 1 calc GR . . . .
H15B H -0.177191 0.198892 0.803563 0.121 Uiso 1 1 calc GR . . . .
H15C H -0.131630 0.344740 0.812340 0.121 Uiso 1 1 calc GR . . . .
C16 C 0.1180(13) 0.3723(16) 0.9319(13) 0.062(4) Uani 1 1 d . . . . .
H16 H 0.210987 0.371060 0.976837 0.074 Uiso 1 1 calc R . . . .
C17 C 0.437(3) 0.179(2) 0.698(3) 0.143(8) Uani 1 1 d D U . . .
H17A H 0.525052 0.162259 0.744862 0.214 Uiso 1 1 calc R . . . .
H17B H 0.360682 0.108928 0.688239 0.214 Uiso 1 1 calc R . . . .
H17C H 0.431471 0.191854 0.614640 0.214 Uiso 1 1 calc R . . . .
C18 C 0.533(2) 0.363(2) 0.887(2) 0.122(8) Uani 1 1 d D U . . .
H18A H 0.609257 0.322782 0.909811 0.184 Uiso 1 1 calc R . . . .
H18B H 0.567544 0.447259 0.878265 0.184 Uiso 1 1 calc R . . . .
H18C H 0.497893 0.366613 0.954167 0.184 Uiso 1 1 calc R . . . .
N1 N 0.0198(10) 0.2801(11) 0.9283(10) 0.055(3) Uani 1 1 d . . . . .
N2 N 0.4248(13) 0.2938(14) 0.7701(15) 0.089(4) Uani 1 1 d . U . . .
O1 O 0.5952(9) 0.8208(10) 0.8826(13) 0.097(4) Uani 1 1 d D . . . .
H1 H 0.529891 0.758667 0.838916 0.145 Uiso 1 1 calc R . . . .
O2 O -0.0093(7) 0.3205(6) 0.6059(7) 0.0407(17) Uani 1 1 d . . . . .
O3 O 0.1614(7) 0.5060(7) 0.5189(7) 0.0470(18) Uani 1 1 d . . . . .
O4 O -0.0723(7) 0.2858(7) 0.3920(6) 0.0435(17) Uani 1 1 d . . . . .
O5 O 0.0973(10) 0.4631(9) 0.8793(9) 0.060(2) Uani 1 1 d . . . . .
O6 O 0.1221(6) 0.4580(7) 0.3135(7) 0.0451(18) Uani 1 1 d . . . . .
O7 O 0.1857(7) 0.7299(7) 0.8689(7) 0.0444(17) Uani 1 1 d . . . . .
O8 O 0.3380(7) 0.6851(7) 0.7915(8) 0.053(2) Uani 1 1 d . . . . .
O9 O 0.0454(11) -0.0810(9) 0.7274(8) 0.063(2) Uani 1 1 d . . . . .
H9 H 0.055925 -0.152900 0.721373 0.095 Uiso 1 1 calc GR . . . .
O11 O 0.2866(8) 0.4224(9) 0.7687(9) 0.063(2) Uani 1 1 d . U . . .
O12 O 0.6822(8) 0.5849(11) 0.7552(8) 0.074(3) Uani 1 1 d . . . . .
H12A H 0.762745 0.583481 0.764003 0.110 Uiso 1 1 calc R . . . .
Tb1 Tb 0.10809(3) 0.53503(3) 0.69896(4) 0.0337(2) 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
C1 C4 1.512(15) . ?
C1 C8 1.398(17) . ?
C1 C9 1.425(12) 2_556 ?
C2 C3 1.503(11) . ?
C2 O3 1.262(12) . ?
C2 O6 1.280(12) . ?
C3 C5 1.404(14) . ?
C3 C6 1.421(14) 2_666 ?
C4 O2 1.272(11) . ?
C4 O4 1.266(14) . ?
C5 H5 0.9400 . ?
C5 C6 1.403(13) . ?
C6 O12 1.373(13) . ?
C7 C11 1.502(12) . ?
C7 O7 1.264(11) . ?
C7 O8 1.280(11) . ?
C8 H8 0.9400 . ?
C8 C9 1.389(16) . ?
C9 O9 1.359(14) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 H10C 0.9700 . ?
C10 N1 1.44(2) . ?
C11 C12 1.297(14) . ?
C11 C14 1.456(13) . ?
C12 H12 0.9400 . ?
C12 C14 1.462(14) 2_677 ?
C13 H13 0.9400 . ?
C13 N2 1.307(19) . ?
C13 O11 1.234(16) . ?
C14 O1 1.420(13) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C15 H15C 0.9700 . ?
C15 N1 1.465(18) . ?
C16 H16 0.9400 . ?
C16 N1 1.299(19) . ?
C16 O5 1.257(19) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C17 H17C 0.9700 . ?
C17 N2 1.49(2) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C18 H18C 0.9700 . ?
C18 N2 1.42(2) . ?
O1 H1 0.8300 . ?
O2 Tb1 2.382(6) . ?
O3 Tb1 2.336(7) . ?
O4 Tb1 2.399(8) 2_566 ?
O5 Tb1 2.340(10) . ?
O6 Tb1 2.419(6) 2_566 ?
O7 Tb1 2.515(6) . ?
O8 Tb1 2.447(6) . ?
O9 H9 0.8300 . ?
O11 Tb1 2.433(8) . ?
O12 H12A 0.8300 . ?

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
C8 C1 C4 119.5(8) . . ?
C8 C1 C9 119.2(9) . 2_556 ?
C9 C1 C4 121.3(10) 2_556 . ?
O3 C2 C3 119.6(9) . . ?
O3 C2 O6 121.4(8) . . ?
O6 C2 C3 119.1(8) . . ?
C5 C3 C2 119.8(8) . . ?
C5 C3 C6 119.8(8) . 2_666 ?
C6 C3 C2 120.5(8) 2_666 . ?
O2 C4 C1 117.4(10) . . ?
O4 C4 C1 116.7(8) . . ?
O4 C4 O2 125.8(10) . . ?
C3 C5 H5 119.8 . . ?
C6 C5 C3 120.3(9) . . ?
C6 C5 H5 119.8 . . ?
C5 C6 C3 119.9(9) . 2_666 ?
O12 C6 C3 122.0(8) . 2_666 ?
O12 C6 C5 118.2(9) . . ?
O7 C7 C11 119.2(8) . . ?
O7 C7 O8 121.3(8) . . ?
O8 C7 C11 119.5(8) . . ?
C1 C8 H8 118.9 . . ?
C9 C8 C1 122.2(9) . . ?
C9 C8 H8 118.9 . . ?
C8 C9 C1 118.6(10) . 2_556 ?
O9 C9 C1 124.7(10) . 2_556 ?
O9 C9 C8 116.6(9) . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N1 C10 H10A 109.5 . . ?
N1 C10 H10B 109.5 . . ?
N1 C10 H10C 109.5 . . ?
C12 C11 C7 120.8(9) . . ?
C12 C11 C14 120.6(9) . . ?
C14 C11 C7 118.6(8) . . ?
C11 C12 H12 118.9 . . ?
C11 C12 C14 122.1(9) . 2_677 ?
C14 C12 H12 118.9 2_677 . ?
N2 C13 H13 117.8 . . ?
O11 C13 H13 117.8 . . ?
O11 C13 N2 124.3(13) . . ?
C11 C14 C12 117.3(9) . 2_677 ?
O1 C14 C11 123.4(9) . . ?
O1 C14 C12 119.2(9) . 2_677 ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N1 C15 H15A 109.5 . . ?
N1 C15 H15B 109.5 . . ?
N1 C15 H15C 109.5 . . ?
N1 C16 H16 117.7 . . ?
O5 C16 H16 117.7 . . ?
O5 C16 N1 124.5(13) . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N2 C17 H17A 109.5 . . ?
N2 C17 H17B 109.5 . . ?
N2 C17 H17C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N2 C18 H18A 109.5 . . ?
N2 C18 H18B 109.5 . . ?
N2 C18 H18C 109.5 . . ?
C10 N1 C15 118.3(12) . . ?
C16 N1 C10 122.2(13) . . ?
C16 N1 C15 119.5(14) . . ?
C13 N2 C17 117.2(16) . . ?
C13 N2 C18 121.0(15) . . ?
C18 N2 C17 121.8(18) . . ?
C14 O1 H1 109.5 . . ?
C4 O2 Tb1 132.8(7) . . ?
C2 O3 Tb1 171.8(7) . . ?
C4 O4 Tb1 141.4(6) . 2_566 ?
C16 O5 Tb1 139.0(8) . . ?
C2 O6 Tb1 108.0(5) . 2_566 ?
C7 O7 Tb1 91.2(5) . . ?
C7 O8 Tb1 93.9(5) . . ?
C9 O9 H9 109.5 . . ?
C13 O11 Tb1 134.9(9) . . ?
C6 O12 H12A 109.5 . . ?
O2 Tb1 O4 128.4(2) . 2_566 ?
O2 Tb1 O6 81.6(2) . 2_566 ?
O2 Tb1 O7 153.4(3) . . ?
O2 Tb1 O8 143.4(2) . . ?
O2 Tb1 O11 74.6(3) . . ?
O3 Tb1 O2 78.4(3) . . ?
O3 Tb1 O4 75.2(3) . 2_566 ?
O3 Tb1 O5 147.8(3) . . ?
O3 Tb1 O6 122.9(2) . 2_566 ?
O3 Tb1 O7 128.1(3) . . ?
O3 Tb1 O8 83.1(3) . . ?
O3 Tb1 O11 79.2(3) . . ?
O4 Tb1 O6 76.9(3) 2_566 2_566 ?
O4 Tb1 O7 68.4(2) 2_566 . ?
O4 Tb1 O8 75.3(3) 2_566 . ?
O4 Tb1 O11 139.6(3) 2_566 . ?
O5 Tb1 O2 79.8(3) . . ?
O5 Tb1 O4 136.8(3) . 2_566 ?
O5 Tb1 O6 76.5(3) . 2_566 ?
O5 Tb1 O7 75.3(3) . . ?
O5 Tb1 O8 101.0(3) . . ?
O5 Tb1 O11 72.4(3) . . ?
O6 Tb1 O7 83.4(2) 2_566 . ?
O6 Tb1 O8 134.5(2) 2_566 . ?
O6 Tb1 O11 143.4(3) 2_566 . ?
O8 Tb1 O7 53.1(2) . . ?
O11 Tb1 O7 106.2(3) . . ?
O11 Tb1 O8 71.1(3) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O1 H1 O8 0.83 1.89 2.605(11) 143.9 . yes
O9 H9 O4 0.83 1.93 2.641(11) 143.0 2_556 yes
O12 H12A O6 0.83 1.85 2.585(10) 146.9 2_666 yes

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
C1 C4 O2 Tb1 139.5(7) . . . . ?
C1 C4 O4 Tb1 -175.0(6) . . . 2_566 ?
C1 C8 C9 C1 -2.0(17) . . . 2_556 ?
C1 C8 C9 O9 -179.4(10) . . . . ?
C2 C3 C5 C6 178.0(12) . . . . ?
C3 C2 O6 Tb1 -177.1(7) . . . 2_566 ?
C3 C5 C6 C3 2(2) . . . 2_666 ?
C3 C5 C6 O12 -177.7(13) . . . . ?
C4 C1 C8 C9 -176.3(9) . . . . ?
C6 C3 C5 C6 -2(2) 2_666 . . . ?
C7 C11 C12 C14 179.7(13) . . . 2_677 ?
C7 C11 C14 C12 -179.7(12) . . . 2_677 ?
C7 C11 C14 O1 -3(2) . . . . ?
C8 C1 C4 O2 9.2(13) . . . . ?
C8 C1 C4 O4 -172.6(9) . . . . ?
C9 C1 C4 O2 -169.0(9) 2_556 . . . ?
C9 C1 C4 O4 9.2(13) 2_556 . . . ?
C9 C1 C8 C9 2.0(17) 2_556 . . . ?
C11 C7 O7 Tb1 172.9(10) . . . . ?
C11 C7 O8 Tb1 -172.7(9) . . . . ?
C12 C11 C14 C12 -1(2) . . . 2_677 ?
C12 C11 C14 O1 176.1(15) . . . . ?
C14 C11 C12 C14 1(3) . . . 2_677 ?
N1 C16 O5 Tb1 -104.2(15) . . . . ?
N2 C13 O11 Tb1 171.0(10) . . . . ?
O2 C4 O4 Tb1 3.1(16) . . . 2_566 ?
O3 C2 C3 C5 -7.8(16) . . . . ?
O3 C2 C3 C6 172.0(11) . . . 2_666 ?
O3 C2 O6 Tb1 2.6(12) . . . 2_566 ?
O4 C4 O2 Tb1 -38.5(13) . . . . ?
O5 C16 N1 C10 -179.9(12) . . . . ?
O5 C16 N1 C15 -1.0(19) . . . . ?
O6 C2 C3 C5 171.9(12) . . . . ?
O6 C2 C3 C6 -8.3(16) . . . 2_666 ?
O7 C7 C11 C12 -8.2(18) . . . . ?
O7 C7 C11 C14 170.5(12) . . . . ?
O7 C7 O8 Tb1 7.6(12) . . . . ?
O8 C7 C11 C12 172.1(13) . . . . ?
O8 C7 C11 C14 -9.3(18) . . . . ?
O8 C7 O7 Tb1 -7.4(11) . . . . ?
O11 C13 N2 C17 179.8(11) . . . . ?
O11 C13 N2 C18 -1.3(19) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.500 0.000 0.500 210.2 0.0 ?


_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 1.240
_oxdiff_exptl_absorpt_empirical_full_min 0.885

# start Validation Reply Form
_vrf_PLAT027_SION2_220K_cool     
;
PROBLEM: _diffrn_reflns_theta_full value (too) Low ......      26.00 Degree
RESPONSE: Our value of max sin(theta)/lambda of 0.56 is close to the recommended 
		  value of 0.60. Higer values of sin(theta)/lambda were not available due 
		  to the beamline experimental set-up limitations.
;
_vrf_PLAT029_SION2_220K_cool     
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.713 Why?  
RESPONSE: The data were collected upon the spindle rotation. Therefore, a 
		  limited portion of the reciprocal space could be probed.
;
# 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_SION2_320K_cool
_database_code_depnum_ccdc_archive 'CCDC 1941020'
loop_
_audit_author_name
_audit_author_address
'Andrzej Gladysiak'
;Ecole polytechnique federale de Lausanne
Switzerland
;
_audit_update_record             
;
2019-07-16 deposited with the CCDC.	2019-08-12 downloaded from the CCDC.
;
_audit_creation_date             2019-05-28
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C18 H20 N2 O11 Tb'
_chemical_formula_sum            'C18 H20 N2 O11 Tb'
_chemical_formula_weight         599.28
_chemical_melting_point          ?
_chemical_oxdiff_formula         C21H27N3O12Tb
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0045 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'
N N 0.0083 0.0040 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0145 0.0076 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.0972 4.9386 '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                   10.6527(6)
_cell_length_b                   11.1484(5)
_cell_length_c                   11.6012(6)
_cell_angle_alpha                96.768(4)
_cell_angle_beta                 111.444(5)
_cell_angle_gamma                101.555(5)
_cell_volume                     1228.51(12)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3006
_cell_measurement_temperature    320.0
_cell_measurement_theta_max      32.3670
_cell_measurement_theta_min      2.4510
_shelx_estimated_absorpt_T_max   0.778
_shelx_estimated_absorpt_T_min   0.518
_exptl_absorpt_coefficient_mu    3.783
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85168
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.620
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             590
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0089
_diffrn_reflns_av_unetI/netI     0.0136
_diffrn_reflns_Laue_measured_fraction_full 0.716
_diffrn_reflns_Laue_measured_fraction_max 0.542
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6887
_diffrn_reflns_point_group_measured_fraction_full 0.716
_diffrn_reflns_point_group_measured_fraction_max 0.542
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         32.318
_diffrn_reflns_theta_min         2.104
_diffrn_ambient_temperature      320.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            PILATUS2M
_diffrn_measured_fraction_theta_full 0.716
_diffrn_measured_fraction_theta_max 0.542
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      0.00 360.00   1.00    1.00    --    0.00   0.00   0.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  PILATUS@SNBL
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0668323000
_diffrn_orient_matrix_UB_12      -0.0033215000
_diffrn_orient_matrix_UB_13      -0.0125735000
_diffrn_orient_matrix_UB_21      0.0462114000
_diffrn_orient_matrix_UB_22      0.0513390000
_diffrn_orient_matrix_UB_23      0.0616577000
_diffrn_orient_matrix_UB_31      0.0108048000
_diffrn_orient_matrix_UB_32      -0.0523713000
_diffrn_orient_matrix_UB_33      0.0394280000
_diffrn_radiation_monochromator  'Si (111)'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.78405
_diffrn_source                   
'European Synchrotron Radiation Facility, BM01 beamline'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3335
_reflns_number_total             3536
_reflns_odcompleteness_completeness 63.20
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     29.34
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         5.656
_refine_diff_density_min         -0.898
_refine_diff_density_rms         0.220
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     292
_refine_ls_number_reflns         3536
_refine_ls_number_restraints     34
_refine_ls_R_factor_all          0.0677
_refine_ls_R_factor_gt           0.0657
_refine_ls_restrained_S_all      6.487
_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)+(0.1334P)²+3.4738P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1734
_refine_ls_wR_factor_ref         0.1765
_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
 C12_$10-O1 \\sim O1-C11
 with sigma of 0.05
 C17-C13 \\sim C13-C18
 with sigma of 0.02
3. Restrained planarity
 C13, C17, C18, N2, O11
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C17) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
5. Rigid body (RIGU) restrains
 O11, C13, N2, C18, C17
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Me refined with riding coordinates:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C)
6.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C8(H8), C12(H12), C13(H13), C16(H16)
6.c Tetrahedral OH refined with riding coordinates:
 O1(H1), O12(H12A)
6.d Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C15(H15A,H15B,H15C)
6.e Idealised tetrahedral OH refined as rotating group:
 O9(H9)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
C1 C -0.0209(10) 0.1200(9) 0.4969(9) 0.049(3) Uani 1 1 d . . . . .
C2 C 0.2052(8) 0.4874(9) 0.4338(9) 0.047(2) Uani 1 1 d . . . . .
C3 C 0.3584(8) 0.4945(9) 0.4672(9) 0.047(2) Uani 1 1 d . . . . .
C4 C -0.0376(9) 0.2515(9) 0.4976(10) 0.047(3) Uani 1 1 d . . . . .
C5 C 0.4539(9) 0.5412(12) 0.5910(10) 0.065(3) Uani 1 1 d . . . . .
H5 H 0.423061 0.569920 0.651698 0.078 Uiso 1 1 calc R . . . .
C6 C 0.5961(9) 0.5463(12) 0.6276(10) 0.059(3) Uani 1 1 d . . . . .
C7 C 0.3042(9) 0.7596(9) 0.8592(10) 0.047(2) Uani 1 1 d . . . . .
C8 C 0.0023(12) 0.0733(10) 0.6063(10) 0.056(3) Uani 1 1 d . . . . .
H8 H 0.003852 0.122622 0.677524 0.067 Uiso 1 1 calc R . . . .
C9 C 0.0236(11) -0.0467(10) 0.6125(10) 0.053(3) Uani 1 1 d . . . . .
C10 C 0.0488(19) 0.1772(16) 0.990(2) 0.097(5) Uani 1 1 d . . . . .
H10A H 0.007477 0.174530 1.051293 0.146 Uiso 1 1 calc GR . . . .
H10B H 0.147997 0.190214 1.032721 0.146 Uiso 1 1 calc GR . . . .
H10C H 0.009745 0.099368 0.929355 0.146 Uiso 1 1 calc GR . . . .
C11 C 0.4016(9) 0.8857(9) 0.9313(10) 0.053(3) Uani 1 1 d D . . . .
C12 C 0.3632(10) 0.9644(12) 0.9901(13) 0.071(4) Uani 1 1 d D . . . .
H12 H 0.272752 0.943269 0.986696 0.085 Uiso 1 1 calc R . . A 2
C13 C 0.3133(15) 0.3312(13) 0.7179(14) 0.087(4) Uani 1 1 d D U . . .
H13 H 0.246636 0.285471 0.639526 0.105 Uiso 1 1 calc R . . . .
C14 C 0.5440(10) 0.9128(12) 0.9368(13) 0.074(4) Uani 1 1 d . . . . .
C15 C -0.1268(16) 0.281(2) 0.861(2) 0.116(7) Uani 1 1 d . . . . .
H15A H -0.170056 0.282306 0.920474 0.173 Uiso 1 1 calc GR . . . .
H15B H -0.175838 0.206866 0.794922 0.173 Uiso 1 1 calc GR . . . .
H15C H -0.130256 0.353620 0.824903 0.173 Uiso 1 1 calc GR . . . .
C16 C 0.1173(16) 0.3681(16) 0.9289(15) 0.078(4) Uani 1 1 d . . . . .
H16 H 0.209315 0.366282 0.972674 0.094 Uiso 1 1 calc R . . . .
C17 C 0.437(3) 0.180(2) 0.693(3) 0.171(10) Uani 1 1 d D U . . .
H17A H 0.523390 0.161709 0.738521 0.257 Uiso 1 1 calc R . . . .
H17B H 0.360231 0.109963 0.679487 0.257 Uiso 1 1 calc R . . . .
H17C H 0.433645 0.195527 0.612065 0.257 Uiso 1 1 calc R . . . .
C18 C 0.534(2) 0.363(3) 0.888(2) 0.167(11) Uani 1 1 d D U . . .
H18A H 0.609010 0.323103 0.910449 0.250 Uiso 1 1 calc R . . . .
H18B H 0.568552 0.447125 0.880874 0.250 Uiso 1 1 calc R . . . .
H18C H 0.496674 0.364551 0.951443 0.250 Uiso 1 1 calc R . . . .
N1 N 0.0203(11) 0.2787(12) 0.9266(10) 0.073(3) Uani 1 1 d . . . . .
N2 N 0.4248(14) 0.2937(15) 0.7669(16) 0.109(5) Uani 1 1 d . U . . .
O1 O 0.5957(10) 0.8241(11) 0.8805(14) 0.125(6) Uani 1 1 d D . . . .
H1 H 0.531010 0.762621 0.837326 0.187 Uiso 1 1 calc R . . . .
O2 O -0.0098(7) 0.3208(6) 0.6039(7) 0.0507(17) Uani 1 1 d . . . . .
O3 O 0.1629(7) 0.5071(7) 0.5197(7) 0.0561(18) Uani 1 1 d . . . . .
O4 O -0.0723(7) 0.2862(7) 0.3925(7) 0.0549(18) Uani 1 1 d . . . . .
O5 O 0.0965(10) 0.4609(10) 0.8747(9) 0.076(3) Uani 1 1 d . . . . .
O6 O 0.1217(6) 0.4592(7) 0.3175(7) 0.0544(18) Uani 1 1 d . . . . .
O7 O 0.1863(7) 0.7282(7) 0.8671(6) 0.0540(18) Uani 1 1 d . . . . .
O8 O 0.3400(7) 0.6856(7) 0.7913(8) 0.065(2) Uani 1 1 d . . . . .
O9 O 0.0441(12) -0.0807(9) 0.7256(8) 0.080(3) Uani 1 1 d . . . . .
H9 H 0.059354 -0.149929 0.722701 0.120 Uiso 1 1 calc GR . . . .
O11 O 0.2883(8) 0.4227(9) 0.7669(10) 0.080(3) Uani 1 1 d . U . . .
O12 O 0.6845(8) 0.5893(12) 0.7523(8) 0.092(4) Uani 1 1 d . . . . .
H12A H 0.764097 0.587891 0.761085 0.138 Uiso 1 1 calc R . . . .
Tb1 Tb 0.10910(3) 0.53467(3) 0.69748(3) 0.0400(2) 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
C1 C4 1.512(14) . ?
C1 C8 1.385(17) . ?
C1 C9 1.414(13) 2_556 ?
C2 C3 1.516(11) . ?
C2 O3 1.249(11) . ?
C2 O6 1.273(12) . ?
C3 C5 1.383(13) . ?
C3 C6 1.419(13) 2_666 ?
C4 O2 1.273(11) . ?
C4 O4 1.270(14) . ?
C5 H5 0.9300 . ?
C5 C6 1.402(12) . ?
C6 O12 1.367(12) . ?
C7 C11 1.502(11) . ?
C7 O7 1.273(11) . ?
C7 O8 1.280(11) . ?
C8 H8 0.9300 . ?
C8 C9 1.406(16) . ?
C9 O9 1.362(15) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C10 N1 1.45(2) . ?
C11 C12 1.268(14) . ?
C11 C14 1.462(13) . ?
C12 H12 0.9300 . ?
C12 C14 1.463(15) 2_677 ?
C13 H13 0.9300 . ?
C13 N2 1.29(2) . ?
C13 O11 1.231(16) . ?
C14 O1 1.427(13) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C15 N1 1.48(2) . ?
C16 H16 0.9300 . ?
C16 N1 1.274(19) . ?
C16 O5 1.29(2) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C17 N2 1.50(3) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C18 N2 1.45(3) . ?
O1 H1 0.8200 . ?
O2 Tb1 2.375(6) . ?
O3 Tb1 2.337(7) . ?
O4 Tb1 2.395(8) 2_566 ?
O5 Tb1 2.341(10) . ?
O6 Tb1 2.417(6) 2_566 ?
O7 Tb1 2.512(6) . ?
O8 Tb1 2.453(7) . ?
O9 H9 0.8200 . ?
O11 Tb1 2.433(8) . ?
O12 H12A 0.8200 . ?

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
C8 C1 C4 119.3(8) . . ?
C8 C1 C9 120.1(9) . 2_556 ?
C9 C1 C4 120.5(10) 2_556 . ?
O3 C2 C3 120.0(9) . . ?
O3 C2 O6 121.4(8) . . ?
O6 C2 C3 118.6(8) . . ?
C5 C3 C2 119.6(8) . . ?
C5 C3 C6 120.0(7) . 2_666 ?
C6 C3 C2 120.4(8) 2_666 . ?
O2 C4 C1 117.8(10) . . ?
O4 C4 C1 117.2(8) . . ?
O4 C4 O2 125.0(9) . . ?
C3 C5 H5 119.1 . . ?
C3 C5 C6 121.8(8) . . ?
C6 C5 H5 119.1 . . ?
C5 C6 C3 118.1(8) . 2_666 ?
O12 C6 C3 122.8(8) . 2_666 ?
O12 C6 C5 119.0(9) . . ?
O7 C7 C11 118.9(8) . . ?
O7 C7 O8 121.1(8) . . ?
O8 C7 C11 120.1(8) . . ?
C1 C8 H8 119.1 . . ?
C1 C8 C9 121.8(9) . . ?
C9 C8 H8 119.1 . . ?
C8 C9 C1 118.1(10) . 2_556 ?
O9 C9 C1 126.5(10) . 2_556 ?
O9 C9 C8 115.4(8) . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N1 C10 H10A 109.5 . . ?
N1 C10 H10B 109.5 . . ?
N1 C10 H10C 109.5 . . ?
C12 C11 C7 121.0(9) . . ?
C12 C11 C14 120.9(9) . . ?
C14 C11 C7 118.1(8) . . ?
C11 C12 H12 118.8 . . ?
C11 C12 C14 122.5(9) . 2_677 ?
C14 C12 H12 118.8 2_677 . ?
N2 C13 H13 117.4 . . ?
O11 C13 H13 117.4 . . ?
O11 C13 N2 125.2(15) . . ?
C11 C14 C12 116.6(9) . 2_677 ?
O1 C14 C11 123.2(9) . . ?
O1 C14 C12 120.2(9) . 2_677 ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N1 C15 H15A 109.5 . . ?
N1 C15 H15B 109.5 . . ?
N1 C15 H15C 109.5 . . ?
N1 C16 H16 117.8 . . ?
N1 C16 O5 124.3(15) . . ?
O5 C16 H16 117.8 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N2 C17 H17A 109.5 . . ?
N2 C17 H17B 109.5 . . ?
N2 C17 H17C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N2 C18 H18A 109.5 . . ?
N2 C18 H18B 109.5 . . ?
N2 C18 H18C 109.5 . . ?
C10 N1 C15 118.3(14) . . ?
C16 N1 C10 122.4(14) . . ?
C16 N1 C15 119.2(16) . . ?
C13 N2 C17 117.4(16) . . ?
C13 N2 C18 119.9(17) . . ?
C18 N2 C17 122.7(19) . . ?
C14 O1 H1 109.5 . . ?
C4 O2 Tb1 133.5(7) . . ?
C2 O3 Tb1 172.3(7) . . ?
C4 O4 Tb1 141.7(6) . 2_566 ?
C16 O5 Tb1 139.7(9) . . ?
C2 O6 Tb1 108.8(5) . 2_566 ?
C7 O7 Tb1 91.3(5) . . ?
C7 O8 Tb1 93.8(5) . . ?
C9 O9 H9 109.5 . . ?
C13 O11 Tb1 134.8(10) . . ?
C6 O12 H12A 109.5 . . ?
O2 Tb1 O4 127.8(2) . 2_566 ?
O2 Tb1 O6 81.1(2) . 2_566 ?
O2 Tb1 O7 153.0(3) . . ?
O2 Tb1 O8 143.9(2) . . ?
O2 Tb1 O11 75.2(3) . . ?
O3 Tb1 O2 78.6(3) . . ?
O3 Tb1 O4 75.2(3) . 2_566 ?
O3 Tb1 O5 147.9(3) . . ?
O3 Tb1 O6 122.5(2) . 2_566 ?
O3 Tb1 O7 128.4(2) . . ?
O3 Tb1 O8 83.2(3) . . ?
O3 Tb1 O11 79.1(3) . . ?
O4 Tb1 O6 76.4(3) 2_566 2_566 ?
O4 Tb1 O7 68.8(2) 2_566 . ?
O4 Tb1 O8 75.7(3) 2_566 . ?
O4 Tb1 O11 139.7(3) 2_566 . ?
O5 Tb1 O2 79.7(3) . . ?
O5 Tb1 O4 136.8(3) . 2_566 ?
O5 Tb1 O6 76.5(3) . 2_566 ?
O5 Tb1 O7 75.2(3) . . ?
O5 Tb1 O8 101.3(3) . . ?
O5 Tb1 O11 72.7(4) . . ?
O6 Tb1 O7 83.5(2) 2_566 . ?
O6 Tb1 O8 134.7(2) 2_566 . ?
O6 Tb1 O11 143.8(3) 2_566 . ?
O8 Tb1 O7 53.2(2) . . ?
O11 Tb1 O7 106.0(3) . . ?
O11 Tb1 O8 70.8(3) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O1 H1 O8 0.82 1.89 2.598(11) 144.4 . yes
O9 H9 O4 0.82 1.96 2.657(11) 141.8 2_556 yes
O12 H12A O6 0.82 1.88 2.603(10) 146.2 2_666 yes

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
C1 C4 O2 Tb1 138.2(7) . . . . ?
C1 C4 O4 Tb1 -175.3(7) . . . 2_566 ?
C1 C8 C9 C1 0.0(18) . . . 2_556 ?
C1 C8 C9 O9 -179.5(10) . . . . ?
C2 C3 C5 C6 178.1(12) . . . . ?
C3 C2 O6 Tb1 -177.8(7) . . . 2_566 ?
C3 C5 C6 C3 2(2) . . . 2_666 ?
C3 C5 C6 O12 -177.7(14) . . . . ?
C4 C1 C8 C9 -177.7(9) . . . . ?
C6 C3 C5 C6 -2(2) 2_666 . . . ?
C7 C11 C12 C14 178.9(13) . . . 2_677 ?
C7 C11 C14 C12 -178.8(12) . . . 2_677 ?
C7 C11 C14 O1 -2(2) . . . . ?
C8 C1 C4 O2 9.8(13) . . . . ?
C8 C1 C4 O4 -173.2(9) . . . . ?
C9 C1 C4 O2 -167.8(9) 2_556 . . . ?
C9 C1 C4 O4 9.1(13) 2_556 . . . ?
C9 C1 C8 C9 0.0(18) 2_556 . . . ?
C11 C7 O7 Tb1 172.2(9) . . . . ?
C11 C7 O8 Tb1 -172.0(9) . . . . ?
C12 C11 C14 C12 -2(2) . . . 2_677 ?
C12 C11 C14 O1 175.1(16) . . . . ?
C14 C11 C12 C14 2(3) . . . 2_677 ?
N1 C16 O5 Tb1 -106.0(17) . . . . ?
N2 C13 O11 Tb1 171.8(11) . . . . ?
O2 C4 O4 Tb1 1.4(16) . . . 2_566 ?
O3 C2 C3 C5 -9.8(16) . . . . ?
O3 C2 C3 C6 170.2(11) . . . 2_666 ?
O3 C2 O6 Tb1 3.3(12) . . . 2_566 ?
O4 C4 O2 Tb1 -38.5(13) . . . . ?
O5 C16 N1 C10 -179.1(14) . . . . ?
O5 C16 N1 C15 -2(2) . . . . ?
O6 C2 C3 C5 171.3(12) . . . . ?
O6 C2 C3 C6 -8.7(16) . . . 2_666 ?
O7 C7 C11 C12 -6.1(18) . . . . ?
O7 C7 C11 C14 171.0(12) . . . . ?
O7 C7 O8 Tb1 7.9(12) . . . . ?
O8 C7 C11 C12 173.8(13) . . . . ?
O8 C7 C11 C14 -9.1(18) . . . . ?
O8 C7 O7 Tb1 -7.7(11) . . . . ?
O11 C13 N2 C17 -179.9(11) . . . . ?
O11 C13 N2 C18 -1.4(19) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.500 0.000 0.500 212.0 2.4 ?


_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 1.191
_oxdiff_exptl_absorpt_empirical_full_min 0.900

# start Validation Reply Form
_vrf_PLAT027_SION2_320K_cool     
;
PROBLEM: _diffrn_reflns_theta_full value (too) Low ......      26.00 Degree
RESPONSE: Our value of max sin(theta)/lambda of 0.56 is close to the recommended 
		  value of 0.60. Higer values of sin(theta)/lambda were not available due 
		  to the beamline experimental set-up limitations.
;
_vrf_PLAT029_SION2_320K_cool     
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.716 Why?  
RESPONSE: The data were collected upon the spindle rotation. Therefore, a 
		  limited portion of the reciprocal space could be probed.
;
# 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_SION2_300K_cool
_database_code_depnum_ccdc_archive 'CCDC 1941025'
loop_
_audit_author_name
_audit_author_address
'Andrzej Gladysiak'
;Ecole polytechnique federale de Lausanne
Switzerland
;
_audit_update_record             
;
2019-07-16 deposited with the CCDC.	2019-08-12 downloaded from the CCDC.
;
_audit_creation_date             2019-05-28
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C18 H20 N2 O11 Tb'
_chemical_formula_sum            'C18 H20 N2 O11 Tb'
_chemical_formula_weight         599.28
_chemical_melting_point          ?
_chemical_oxdiff_formula         C21H27N3O12Tb
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0045 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'
N N 0.0083 0.0040 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0145 0.0076 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.0972 4.9386 '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                   10.6648(6)
_cell_length_b                   11.1682(5)
_cell_length_c                   11.5897(6)
_cell_angle_alpha                96.798(4)
_cell_angle_beta                 111.386(5)
_cell_angle_gamma                101.528(4)
_cell_volume                     1231.45(12)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3040
_cell_measurement_temperature    300.0
_cell_measurement_theta_max      32.3250
_cell_measurement_theta_min      2.1200
_shelx_estimated_absorpt_T_max   0.778
_shelx_estimated_absorpt_T_min   0.519
_exptl_absorpt_coefficient_mu    3.774
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81764
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.616
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             590
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0101
_diffrn_reflns_av_unetI/netI     0.0148
_diffrn_reflns_Laue_measured_fraction_full 0.713
_diffrn_reflns_Laue_measured_fraction_max 0.544
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6903
_diffrn_reflns_point_group_measured_fraction_full 0.713
_diffrn_reflns_point_group_measured_fraction_max 0.544
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         32.286
_diffrn_reflns_theta_min         2.100
_diffrn_ambient_temperature      300.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            PILATUS2M
_diffrn_measured_fraction_theta_full 0.713
_diffrn_measured_fraction_theta_max 0.544
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      0.00 360.00   1.00    1.00    --    0.00   0.00   0.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  PILATUS@SNBL
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0666331000
_diffrn_orient_matrix_UB_12      -0.0035023000
_diffrn_orient_matrix_UB_13      -0.0127558000
_diffrn_orient_matrix_UB_21      0.0462506000
_diffrn_orient_matrix_UB_22      0.0513387000
_diffrn_orient_matrix_UB_23      0.0615793000
_diffrn_orient_matrix_UB_31      0.0108306000
_diffrn_orient_matrix_UB_32      -0.0521694000
_diffrn_orient_matrix_UB_33      0.0395774000
_diffrn_radiation_monochromator  'Si (111)'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.78405
_diffrn_source                   
'European Synchrotron Radiation Facility, BM01 beamline'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3338
_reflns_number_total             3547
_reflns_odcompleteness_completeness 63.16
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     29.34
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         6.272
_refine_diff_density_min         -1.430
_refine_diff_density_rms         0.243
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     292
_refine_ls_number_reflns         3547
_refine_ls_number_restraints     34
_refine_ls_R_factor_all          0.0743
_refine_ls_R_factor_gt           0.0721
_refine_ls_restrained_S_all      6.612
_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)+(0.1474P)²+3.6056P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1905
_refine_ls_wR_factor_ref         0.1940
_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
 C12_$9-O1 \\sim O1-C11
 with sigma of 0.05
 C17-C13 \\sim C13-C18
 with sigma of 0.02
3. Restrained planarity
 C13, C17, C18, N2, O11
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C17) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
5. Rigid body (RIGU) restrains
 O11, C13, N2, C18, C17
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Me refined with riding coordinates:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C)
6.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C8(H8), C12(H12), C13(H13), C16(H16)
6.c Tetrahedral OH refined with riding coordinates:
 O1(H1), O12(H12A)
6.d Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C15(H15A,H15B,H15C)
6.e Idealised tetrahedral OH refined as rotating group:
 O9(H9)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
C1 C -0.0209(10) 0.1204(10) 0.4962(10) 0.046(3) Uani 1 1 d . . . . .
C2 C 0.2054(9) 0.4866(10) 0.4334(10) 0.046(3) Uani 1 1 d . . . . .
C3 C 0.3580(9) 0.4943(10) 0.4665(10) 0.046(3) Uani 1 1 d . . . . .
C4 C -0.0369(9) 0.2522(9) 0.4975(11) 0.045(3) Uani 1 1 d . . . . .
C5 C 0.4538(10) 0.5405(13) 0.5925(11) 0.060(3) Uani 1 1 d . . . . .
H5 H 0.422826 0.567681 0.653703 0.072 Uiso 1 1 calc R . . . .
C6 C 0.5956(10) 0.5463(13) 0.6275(11) 0.056(3) Uani 1 1 d . . . . .
C7 C 0.3040(9) 0.7601(9) 0.8592(10) 0.046(3) Uani 1 1 d . . . . .
C8 C 0.0024(12) 0.0730(11) 0.6072(11) 0.053(3) Uani 1 1 d . . . . .
H8 H 0.003483 0.122030 0.678473 0.063 Uiso 1 1 calc R . . . .
C9 C 0.0238(12) -0.0458(11) 0.6130(10) 0.049(3) Uani 1 1 d . . . . .
C10 C 0.049(2) 0.1776(18) 0.991(2) 0.095(6) Uani 1 1 d . . . . .
H10A H 0.006957 0.174364 1.051586 0.143 Uiso 1 1 calc GR . . . .
H10B H 0.148082 0.191005 1.034256 0.143 Uiso 1 1 calc GR . . . .
H10C H 0.010950 0.100065 0.929984 0.143 Uiso 1 1 calc GR . . . .
C11 C 0.4015(9) 0.8861(10) 0.9321(10) 0.049(3) Uani 1 1 d D . . . .
C12 C 0.3622(11) 0.9644(13) 0.9893(14) 0.070(4) Uani 1 1 d D . . . .
H12 H 0.271581 0.943758 0.985397 0.084 Uiso 1 1 calc R . . A 2
C13 C 0.3120(15) 0.3315(14) 0.7179(15) 0.085(5) Uani 1 1 d D U . . .
H13 H 0.245682 0.286065 0.639250 0.103 Uiso 1 1 calc R . . . .
C14 C 0.5437(11) 0.9120(12) 0.9376(15) 0.073(4) Uani 1 1 d . . . . .
C15 C -0.1258(17) 0.282(2) 0.862(2) 0.100(6) Uani 1 1 d . . . . .
H15A H -0.168766 0.283452 0.922041 0.150 Uiso 1 1 calc GR . . . .
H15B H -0.174951 0.208619 0.795928 0.150 Uiso 1 1 calc GR . . . .
H15C H -0.129000 0.355100 0.826667 0.150 Uiso 1 1 calc GR . . . .
C16 C 0.1174(15) 0.3695(18) 0.9302(15) 0.074(5) Uani 1 1 d . . . . .
H16 H 0.209136 0.368380 0.975304 0.089 Uiso 1 1 calc R . . . .
C17 C 0.436(3) 0.182(2) 0.693(3) 0.166(10) Uani 1 1 d D U . . .
H17A H 0.522443 0.162816 0.738243 0.249 Uiso 1 1 calc R . . . .
H17B H 0.359477 0.111894 0.678606 0.249 Uiso 1 1 calc R . . . .
H17C H 0.433700 0.198459 0.612590 0.249 Uiso 1 1 calc R . . . .
C18 C 0.533(2) 0.361(3) 0.886(2) 0.154(11) Uani 1 1 d D U . . .
H18A H 0.607056 0.320385 0.908204 0.231 Uiso 1 1 calc R . . . .
H18B H 0.568097 0.444882 0.879318 0.231 Uiso 1 1 calc R . . . .
H18C H 0.496406 0.363327 0.950617 0.231 Uiso 1 1 calc R . . . .
N1 N 0.0205(12) 0.2795(12) 0.9272(11) 0.067(3) Uani 1 1 d . . . . .
N2 N 0.4248(15) 0.2939(16) 0.7680(17) 0.103(5) Uani 1 1 d . U . . .
O1 O 0.5959(10) 0.8215(11) 0.8825(15) 0.115(6) Uani 1 1 d D . . . .
H1 H 0.531281 0.760207 0.839388 0.173 Uiso 1 1 calc R . . . .
O2 O -0.0094(7) 0.3207(6) 0.6044(7) 0.0467(18) Uani 1 1 d . . . . .
O3 O 0.1629(7) 0.5070(8) 0.5195(8) 0.054(2) Uani 1 1 d . . . . .
O4 O -0.0720(8) 0.2859(7) 0.3927(7) 0.0516(19) Uani 1 1 d . . . . .
O5 O 0.0973(11) 0.4610(11) 0.8759(10) 0.071(3) Uani 1 1 d . . . . .
O6 O 0.1216(7) 0.4584(8) 0.3162(7) 0.0516(19) Uani 1 1 d . . . . .
O7 O 0.1860(7) 0.7288(7) 0.8675(7) 0.0507(19) Uani 1 1 d . . . . .
O8 O 0.3393(7) 0.6859(8) 0.7912(9) 0.062(2) Uani 1 1 d . . . . .
O9 O 0.0442(13) -0.0809(9) 0.7261(9) 0.075(3) Uani 1 1 d . . . . .
H9 H 0.067057 -0.146799 0.724906 0.112 Uiso 1 1 calc GR . . . .
O11 O 0.2875(9) 0.4221(10) 0.7671(11) 0.079(3) Uani 1 1 d . U . . .
O12 O 0.6843(8) 0.5880(13) 0.7530(9) 0.087(4) Uani 1 1 d . . . . .
H12A H 0.763756 0.586541 0.761543 0.130 Uiso 1 1 calc R . . . .
Tb1 Tb 0.10886(3) 0.53475(4) 0.69789(4) 0.0381(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
C1 C4 1.515(15) . ?
C1 C8 1.407(18) . ?
C1 C9 1.417(13) 2_556 ?
C2 C3 1.511(11) . ?
C2 O3 1.254(12) . ?
C2 O6 1.282(13) . ?
C3 C5 1.402(14) . ?
C3 C6 1.416(14) 2_666 ?
C4 O2 1.275(12) . ?
C4 O4 1.261(15) . ?
C5 H5 0.9300 . ?
C5 C6 1.401(13) . ?
C6 O12 1.374(14) . ?
C7 C11 1.506(12) . ?
C7 O7 1.279(12) . ?
C7 O8 1.279(12) . ?
C8 H8 0.9300 . ?
C8 C9 1.396(17) . ?
C9 O9 1.367(16) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C10 N1 1.45(2) . ?
C11 C12 1.263(16) . ?
C11 C14 1.461(14) . ?
C12 H12 0.9300 . ?
C12 C14 1.476(16) 2_677 ?
C13 H13 0.9300 . ?
C13 N2 1.31(2) . ?
C13 O11 1.223(18) . ?
C14 O1 1.440(14) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C15 N1 1.47(2) . ?
C16 H16 0.9300 . ?
C16 N1 1.28(2) . ?
C16 O5 1.28(2) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C17 N2 1.49(3) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C18 N2 1.42(3) . ?
O1 H1 0.8200 . ?
O2 Tb1 2.380(7) . ?
O3 Tb1 2.343(8) . ?
O4 Tb1 2.405(9) 2_566 ?
O5 Tb1 2.344(11) . ?
O6 Tb1 2.421(6) 2_566 ?
O7 Tb1 2.517(7) . ?
O8 Tb1 2.456(7) . ?
O9 H9 0.8200 . ?
O11 Tb1 2.436(9) . ?
O12 H12A 0.8200 . ?

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
C8 C1 C4 119.1(9) . . ?
C8 C1 C9 119.5(10) . 2_556 ?
C9 C1 C4 121.4(11) 2_556 . ?
O3 C2 C3 120.1(9) . . ?
O3 C2 O6 121.3(8) . . ?
O6 C2 C3 118.6(8) . . ?
C5 C3 C2 119.3(9) . . ?
C5 C3 C6 119.9(8) . 2_666 ?
C6 C3 C2 120.8(9) 2_666 . ?
O2 C4 C1 117.6(11) . . ?
O4 C4 C1 116.7(9) . . ?
O4 C4 O2 125.7(10) . . ?
C3 C5 H5 119.5 . . ?
C6 C5 C3 121.0(9) . . ?
C6 C5 H5 119.5 . . ?
C5 C6 C3 119.1(9) . 2_666 ?
O12 C6 C3 122.2(9) . 2_666 ?
O12 C6 C5 118.6(9) . . ?
O7 C7 C11 118.6(8) . . ?
O7 C7 O8 120.9(8) . . ?
O8 C7 C11 120.4(9) . . ?
C1 C8 H8 119.2 . . ?
C9 C8 C1 121.6(9) . . ?
C9 C8 H8 119.2 . . ?
C8 C9 C1 119.0(11) . 2_556 ?
O9 C9 C1 125.3(10) . 2_556 ?
O9 C9 C8 115.7(9) . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N1 C10 H10A 109.5 . . ?
N1 C10 H10B 109.5 . . ?
N1 C10 H10C 109.5 . . ?
C12 C11 C7 120.7(9) . . ?
C12 C11 C14 121.6(9) . . ?
C14 C11 C7 117.7(9) . . ?
C11 C12 H12 119.2 . . ?
C11 C12 C14 121.7(10) . 2_677 ?
C14 C12 H12 119.2 2_677 . ?
N2 C13 H13 117.7 . . ?
O11 C13 H13 117.7 . . ?
O11 C13 N2 124.6(16) . . ?
C11 C14 C12 116.7(9) . 2_677 ?
O1 C14 C11 123.3(9) . . ?
O1 C14 C12 119.9(9) . 2_677 ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N1 C15 H15A 109.5 . . ?
N1 C15 H15B 109.5 . . ?
N1 C15 H15C 109.5 . . ?
N1 C16 H16 117.6 . . ?
N1 C16 O5 124.7(15) . . ?
O5 C16 H16 117.6 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N2 C17 H17A 109.5 . . ?
N2 C17 H17B 109.5 . . ?
N2 C17 H17C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N2 C18 H18A 109.5 . . ?
N2 C18 H18B 109.5 . . ?
N2 C18 H18C 109.5 . . ?
C10 N1 C15 118.4(14) . . ?
C16 N1 C10 122.5(15) . . ?
C16 N1 C15 119.0(16) . . ?
C13 N2 C17 116.7(18) . . ?
C13 N2 C18 120.9(18) . . ?
C18 N2 C17 122(2) . . ?
C14 O1 H1 109.5 . . ?
C4 O2 Tb1 133.1(7) . . ?
C2 O3 Tb1 172.0(8) . . ?
C4 O4 Tb1 141.5(6) . 2_566 ?
C16 O5 Tb1 140.4(9) . . ?
C2 O6 Tb1 108.6(6) . 2_566 ?
C7 O7 Tb1 91.3(5) . . ?
C7 O8 Tb1 94.1(6) . . ?
C9 O9 H9 109.5 . . ?
C13 O11 Tb1 134.7(10) . . ?
C6 O12 H12A 109.5 . . ?
O2 Tb1 O4 127.9(3) . 2_566 ?
O2 Tb1 O6 81.4(3) . 2_566 ?
O2 Tb1 O7 153.1(3) . . ?
O2 Tb1 O8 143.8(2) . . ?
O2 Tb1 O11 74.9(3) . . ?
O3 Tb1 O2 78.6(3) . . ?
O3 Tb1 O4 75.1(3) . 2_566 ?
O3 Tb1 O5 147.7(3) . . ?
O3 Tb1 O6 122.8(3) . 2_566 ?
O3 Tb1 O7 128.2(3) . . ?
O3 Tb1 O8 83.1(3) . . ?
O3 Tb1 O11 79.1(3) . . ?
O4 Tb1 O6 76.4(3) 2_566 2_566 ?
O4 Tb1 O7 68.7(3) 2_566 . ?
O4 Tb1 O8 75.5(3) 2_566 . ?
O4 Tb1 O11 139.8(3) 2_566 . ?
O5 Tb1 O2 79.7(3) . . ?
O5 Tb1 O4 137.0(3) . 2_566 ?
O5 Tb1 O6 76.7(3) . 2_566 ?
O5 Tb1 O7 75.4(3) . . ?
O5 Tb1 O8 101.3(4) . . ?
O5 Tb1 O11 72.4(4) . . ?
O6 Tb1 O7 83.3(2) 2_566 . ?
O6 Tb1 O8 134.4(3) 2_566 . ?
O6 Tb1 O11 143.7(4) 2_566 . ?
O8 Tb1 O7 53.2(2) . . ?
O11 Tb1 O7 106.3(3) . . ?
O11 Tb1 O8 71.2(3) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O1 H1 O8 0.82 1.89 2.599(12) 144.2 . yes
O9 H9 O4 0.82 1.96 2.654(11) 141.3 2_556 yes
O12 H12A O6 0.82 1.87 2.596(11) 146.7 2_666 yes

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
C1 C4 O2 Tb1 138.9(8) . . . . ?
C1 C4 O4 Tb1 -175.4(7) . . . 2_566 ?
C1 C8 C9 C1 -0.5(19) . . . 2_556 ?
C1 C8 C9 O9 -179.6(11) . . . . ?
C2 C3 C5 C6 178.4(12) . . . . ?
C3 C2 O6 Tb1 -177.3(8) . . . 2_566 ?
C3 C5 C6 C3 1(2) . . . 2_666 ?
C3 C5 C6 O12 -177.6(14) . . . . ?
C4 C1 C8 C9 -177.2(10) . . . . ?
C6 C3 C5 C6 -1(2) 2_666 . . . ?
C7 C11 C12 C14 179.4(14) . . . 2_677 ?
C7 C11 C14 C12 -179.4(13) . . . 2_677 ?
C7 C11 C14 O1 -3(2) . . . . ?
C8 C1 C4 O2 9.4(14) . . . . ?
C8 C1 C4 O4 -172.8(9) . . . . ?
C9 C1 C4 O2 -168.2(9) 2_556 . . . ?
C9 C1 C4 O4 9.5(14) 2_556 . . . ?
C9 C1 C8 C9 0.5(19) 2_556 . . . ?
C11 C7 O7 Tb1 172.7(10) . . . . ?
C11 C7 O8 Tb1 -172.5(10) . . . . ?
C12 C11 C14 C12 -2(3) . . . 2_677 ?
C12 C11 C14 O1 174.7(17) . . . . ?
C14 C11 C12 C14 2(3) . . . 2_677 ?
N1 C16 O5 Tb1 -104.5(18) . . . . ?
N2 C13 O11 Tb1 171.7(11) . . . . ?
O2 C4 O4 Tb1 2.2(17) . . . 2_566 ?
O3 C2 C3 C5 -8.4(18) . . . . ?
O3 C2 C3 C6 170.5(12) . . . 2_666 ?
O3 C2 O6 Tb1 2.9(14) . . . 2_566 ?
O4 C4 O2 Tb1 -38.6(14) . . . . ?
O5 C16 N1 C10 -179.8(15) . . . . ?
O5 C16 N1 C15 -3(2) . . . . ?
O6 C2 C3 C5 171.8(12) . . . . ?
O6 C2 C3 C6 -9.2(17) . . . 2_666 ?
O7 C7 C11 C12 -7(2) . . . . ?
O7 C7 C11 C14 170.5(13) . . . . ?
O7 C7 O8 Tb1 7.9(12) . . . . ?
O8 C7 C11 C12 173.0(14) . . . . ?
O8 C7 C11 C14 -9.1(19) . . . . ?
O8 C7 O7 Tb1 -7.7(12) . . . . ?
O11 C13 N2 C17 -179.5(12) . . . . ?
O11 C13 N2 C18 -2(2) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.500 0.000 0.500 214.5 0.0 ?


_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 1.269
_oxdiff_exptl_absorpt_empirical_full_min 0.864

# start Validation Reply Form
_vrf_PLAT027_SION2_300K_cool     
;
PROBLEM: _diffrn_reflns_theta_full value (too) Low ......      26.00 Degree
RESPONSE: Our value of max sin(theta)/lambda of 0.56 is close to the recommended 
		  value of 0.60. Higer values of sin(theta)/lambda were not available due 
		  to the beamline experimental set-up limitations.
;
_vrf_PLAT029_SION2_300K_cool     
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.713 Why?  
RESPONSE: The data were collected upon the spindle rotation. Therefore, a 
		  limited portion of the reciprocal space could be probed.
;
# 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_SION2_200K_cool
_database_code_depnum_ccdc_archive 'CCDC 1941016'
loop_
_audit_author_name
_audit_author_address
'Andrzej Gladysiak'
;Ecole polytechnique federale de Lausanne
Switzerland
;
_audit_update_record             
;
2019-07-16 deposited with the CCDC.	2019-08-12 downloaded from the CCDC.
;
_audit_creation_date             2019-05-27
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C18 H20 N2 O11 Tb'
_chemical_formula_sum            'C18 H20 N2 O11 Tb'
_chemical_formula_weight         599.28
_chemical_melting_point          ?
_chemical_oxdiff_formula         C21H27N3O12Tb
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0045 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'
N N 0.0083 0.0040 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0145 0.0076 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.0972 4.9386 '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                   10.6568(6)
_cell_length_b                   11.1912(5)
_cell_length_c                   11.4798(5)
_cell_angle_alpha                96.941(4)
_cell_angle_beta                 111.109(5)
_cell_angle_gamma                101.425(4)
_cell_volume                     1223.96(11)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3173
_cell_measurement_temperature    200.0
_cell_measurement_theta_max      32.3440
_cell_measurement_theta_min      2.1530
_shelx_estimated_absorpt_T_max   0.777
_shelx_estimated_absorpt_T_min   0.517
_exptl_absorpt_coefficient_mu    3.798
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83777
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.626
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             590
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0094
_diffrn_reflns_av_unetI/netI     0.0143
_diffrn_reflns_Laue_measured_fraction_full 0.710
_diffrn_reflns_Laue_measured_fraction_max 0.544
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6812
_diffrn_reflns_point_group_measured_fraction_full 0.710
_diffrn_reflns_point_group_measured_fraction_max 0.544
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         32.163
_diffrn_reflns_theta_min         2.095
_diffrn_ambient_temperature      200.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            PILATUS2M
_diffrn_measured_fraction_theta_full 0.710
_diffrn_measured_fraction_theta_max 0.544
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      0.00 360.00   1.00    1.00    --    0.00   0.00   0.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  PILATUS@SNBL
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0666148000
_diffrn_orient_matrix_UB_12      -0.0036745000
_diffrn_orient_matrix_UB_13      -0.0130459000
_diffrn_orient_matrix_UB_21      0.0460085000
_diffrn_orient_matrix_UB_22      0.0514951000
_diffrn_orient_matrix_UB_23      0.0618193000
_diffrn_orient_matrix_UB_31      0.0109384000
_diffrn_orient_matrix_UB_32      -0.0517648000
_diffrn_orient_matrix_UB_33      0.0401956000
_diffrn_radiation_monochromator  'Si (111)'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.78405
_diffrn_source                   
'European Synchrotron Radiation Facility, BM01 beamline'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3328
_reflns_number_total             3491
_reflns_odcompleteness_completeness 62.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     29.34
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         8.364
_refine_diff_density_min         -2.171
_refine_diff_density_rms         0.323
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     292
_refine_ls_number_reflns         3491
_refine_ls_number_restraints     34
_refine_ls_R_factor_all          0.0896
_refine_ls_R_factor_gt           0.0880
_refine_ls_restrained_S_all      6.401
_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)+(0.1895P)²+5.1814P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2255
_refine_ls_wR_factor_ref         0.2286
_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
 C17-C13 \\sim C13-C18
 with sigma of 0.02
 C12_$8-O1 \\sim O1-C11
 with sigma of 0.05
3. Restrained planarity
 C13, C17, C18, N2, O11
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C17) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
5. Rigid body (RIGU) restrains
 O11, C13, N2, C18, C17
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Me refined with riding coordinates:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C)
6.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C8(H8), C12(H12), C13(H13), C16(H16)
6.c Tetrahedral OH refined with riding coordinates:
 O1(H1), O12(H12A)
6.d Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C15(H15A,H15B,H15C)
6.e Idealised tetrahedral OH refined as rotating group:
 O9(H9)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
C1 C -0.0202(11) 0.1210(11) 0.4973(11) 0.039(3) Uani 1 1 d . . . . .
C2 C 0.2048(10) 0.4843(11) 0.4319(12) 0.040(3) Uani 1 1 d . . . . .
C3 C 0.3572(10) 0.4939(11) 0.4667(11) 0.037(3) Uani 1 1 d . . . . .
C4 C -0.0361(11) 0.2515(11) 0.4988(12) 0.041(3) Uani 1 1 d . . . . .
C5 C 0.4527(12) 0.5397(14) 0.5940(12) 0.051(4) Uani 1 1 d . . . . .
H5 H 0.420945 0.567792 0.657191 0.062 Uiso 1 1 calc R . . . .
C6 C 0.5944(12) 0.5443(14) 0.6289(12) 0.050(4) Uani 1 1 d . . . . .
C7 C 0.3024(11) 0.7596(10) 0.8604(11) 0.037(3) Uani 1 1 d . . . . .
C8 C 0.0026(13) 0.0722(12) 0.6078(12) 0.045(3) Uani 1 1 d . . . . .
H8 H 0.002342 0.121364 0.681177 0.054 Uiso 1 1 calc R . . . .
C9 C 0.0254(13) -0.0443(12) 0.6143(11) 0.041(3) Uani 1 1 d . . . . .
C10 C 0.0486(19) 0.1782(18) 0.990(2) 0.075(5) Uani 1 1 d . . . . .
H10A H 0.008885 0.176384 1.055212 0.112 Uiso 1 1 calc GR . . . .
H10B H 0.149630 0.190423 1.031418 0.112 Uiso 1 1 calc GR . . . .
H10C H 0.006999 0.099087 0.927579 0.112 Uiso 1 1 calc GR . . . .
C11 C 0.4004(11) 0.8858(11) 0.9332(12) 0.043(3) Uani 1 1 d D . . . .
C12 C 0.3612(12) 0.9636(15) 0.9902(15) 0.059(4) Uani 1 1 d D . . . .
H12 H 0.269580 0.942252 0.988229 0.071 Uiso 1 1 calc R . . A 2
C13 C 0.3094(15) 0.3289(14) 0.7205(15) 0.069(4) Uani 1 1 d D U . . .
H13 H 0.239869 0.279610 0.641978 0.083 Uiso 1 1 calc R . . . .
C14 C 0.5434(12) 0.9092(14) 0.9381(15) 0.058(4) Uani 1 1 d . . . . .
C15 C -0.1269(17) 0.278(2) 0.860(2) 0.077(5) Uani 1 1 d . . . . .
H15A H -0.167693 0.293860 0.922645 0.115 Uiso 1 1 calc GR . . . .
H15B H -0.177958 0.196815 0.803039 0.115 Uiso 1 1 calc GR . . . .
H15C H -0.133096 0.343495 0.809753 0.115 Uiso 1 1 calc GR . . . .
C16 C 0.1186(16) 0.3728(19) 0.9328(16) 0.062(5) Uani 1 1 d . . . . .
H16 H 0.212149 0.371825 0.979471 0.074 Uiso 1 1 calc R . . . .
C17 C 0.436(3) 0.179(2) 0.702(3) 0.126(9) Uani 1 1 d D U . . .
H17A H 0.526431 0.163656 0.749200 0.189 Uiso 1 1 calc R . . . .
H17B H 0.360964 0.108645 0.694187 0.189 Uiso 1 1 calc R . . . .
H17C H 0.429893 0.189714 0.616514 0.189 Uiso 1 1 calc R . . . .
C18 C 0.533(2) 0.363(3) 0.886(2) 0.115(9) Uani 1 1 d D U . . .
H18A H 0.609527 0.322837 0.908706 0.172 Uiso 1 1 calc R . . . .
H18B H 0.566512 0.447797 0.876301 0.172 Uiso 1 1 calc R . . . .
H18C H 0.497829 0.367221 0.954461 0.172 Uiso 1 1 calc R . . . .
N1 N 0.0194(12) 0.2801(12) 0.9266(11) 0.052(3) Uani 1 1 d . . . . .
N2 N 0.4244(15) 0.2936(16) 0.7707(17) 0.086(5) Uani 1 1 d . U . . .
O1 O 0.5957(11) 0.8181(12) 0.8822(15) 0.091(5) Uani 1 1 d D . . . .
H1 H 0.529620 0.755464 0.838147 0.137 Uiso 1 1 calc R . . . .
O2 O -0.0090(8) 0.3210(7) 0.6065(8) 0.0386(19) Uani 1 1 d . . . . .
O3 O 0.1613(8) 0.5056(8) 0.5183(8) 0.044(2) Uani 1 1 d . . . . .
O4 O -0.0719(8) 0.2859(8) 0.3926(8) 0.043(2) Uani 1 1 d . . . . .
O5 O 0.0978(11) 0.4639(11) 0.8803(10) 0.058(3) Uani 1 1 d . . . . .
O6 O 0.1215(7) 0.4578(8) 0.3128(8) 0.043(2) Uani 1 1 d . . . . .
O7 O 0.1856(8) 0.7297(8) 0.8690(8) 0.043(2) Uani 1 1 d . . . . .
O8 O 0.3381(8) 0.6850(9) 0.7915(9) 0.051(3) Uani 1 1 d . . . . .
O9 O 0.0464(13) -0.0810(10) 0.7287(9) 0.061(3) Uani 1 1 d . . . . .
H9 H 0.070708 -0.147878 0.726635 0.091 Uiso 1 1 calc GR . . . .
O11 O 0.2864(9) 0.4220(10) 0.7690(11) 0.062(3) Uani 1 1 d . U . . .
O12 O 0.6815(9) 0.5843(13) 0.7557(9) 0.068(3) Uani 1 1 d . . . . .
H12A H 0.762971 0.582892 0.764882 0.102 Uiso 1 1 calc R . . . .
Tb1 Tb 0.10789(4) 0.53510(4) 0.69915(4) 0.0325(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
C1 C4 1.501(17) . ?
C1 C8 1.40(2) . ?
C1 C9 1.430(15) 2_556 ?
C2 C3 1.504(13) . ?
C2 O3 1.254(14) . ?
C2 O6 1.292(15) . ?
C3 C5 1.406(16) . ?
C3 C6 1.427(16) 2_666 ?
C4 O2 1.280(13) . ?
C4 O4 1.272(17) . ?
C5 H5 0.9500 . ?
C5 C6 1.404(16) . ?
C6 O12 1.373(15) . ?
C7 C11 1.512(14) . ?
C7 O7 1.266(14) . ?
C7 O8 1.285(13) . ?
C8 H8 0.9500 . ?
C8 C9 1.379(19) . ?
C9 O9 1.377(17) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C10 N1 1.45(3) . ?
C11 C12 1.250(18) . ?
C11 C14 1.473(16) . ?
C12 H12 0.9500 . ?
C12 C14 1.510(18) 2_677 ?
C13 H13 0.9500 . ?
C13 N2 1.31(2) . ?
C13 O11 1.231(18) . ?
C14 O1 1.444(15) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C15 N1 1.46(2) . ?
C16 H16 0.9500 . ?
C16 N1 1.30(2) . ?
C16 O5 1.26(2) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C17 N2 1.47(3) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C18 N2 1.41(3) . ?
O1 H1 0.8400 . ?
O2 Tb1 2.381(7) . ?
O3 Tb1 2.346(8) . ?
O4 Tb1 2.407(10) 2_566 ?
O5 Tb1 2.345(12) . ?
O6 Tb1 2.416(7) 2_566 ?
O7 Tb1 2.516(8) . ?
O8 Tb1 2.454(8) . ?
O9 H9 0.8400 . ?
O11 Tb1 2.442(10) . ?
O12 H12A 0.8400 . ?

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
C8 C1 C4 120.0(10) . . ?
C8 C1 C9 118.3(11) . 2_556 ?
C9 C1 C4 121.8(12) 2_556 . ?
O3 C2 C3 119.8(10) . . ?
O3 C2 O6 121.1(9) . . ?
O6 C2 C3 119.1(9) . . ?
C5 C3 C2 120.1(10) . . ?
C5 C3 C6 119.6(9) . 2_666 ?
C6 C3 C2 120.3(10) 2_666 . ?
O2 C4 C1 118.1(12) . . ?
O4 C4 C1 117.1(10) . . ?
O4 C4 O2 124.7(11) . . ?
C3 C5 H5 119.6 . . ?
C6 C5 C3 120.8(10) . . ?
C6 C5 H5 119.6 . . ?
C5 C6 C3 119.6(10) . 2_666 ?
O12 C6 C3 122.3(10) . 2_666 ?
O12 C6 C5 118.1(10) . . ?
O7 C7 C11 118.6(9) . . ?
O7 C7 O8 121.3(9) . . ?
O8 C7 C11 120.1(10) . . ?
C1 C8 H8 118.7 . . ?
C9 C8 C1 122.7(10) . . ?
C9 C8 H8 118.7 . . ?
C8 C9 C1 119.0(12) . 2_556 ?
O9 C9 C1 124.2(12) . 2_556 ?
O9 C9 C8 116.7(10) . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N1 C10 H10A 109.5 . . ?
N1 C10 H10B 109.5 . . ?
N1 C10 H10C 109.5 . . ?
C12 C11 C7 120.4(11) . . ?
C12 C11 C14 122.5(10) . . ?
C14 C11 C7 117.0(10) . . ?
C11 C12 H12 119.3 . . ?
C11 C12 C14 121.3(11) . 2_677 ?
C14 C12 H12 119.3 2_677 . ?
N2 C13 H13 118.0 . . ?
O11 C13 H13 118.0 . . ?
O11 C13 N2 124.0(15) . . ?
C11 C14 C12 116.1(10) . 2_677 ?
O1 C14 C11 124.1(10) . . ?
O1 C14 C12 119.8(10) . 2_677 ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N1 C15 H15A 109.5 . . ?
N1 C15 H15B 109.5 . . ?
N1 C15 H15C 109.5 . . ?
N1 C16 H16 118.1 . . ?
O5 C16 H16 118.1 . . ?
O5 C16 N1 123.9(15) . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N2 C17 H17A 109.5 . . ?
N2 C17 H17B 109.5 . . ?
N2 C17 H17C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N2 C18 H18A 109.5 . . ?
N2 C18 H18B 109.5 . . ?
N2 C18 H18C 109.5 . . ?
C10 N1 C15 117.5(14) . . ?
C16 N1 C10 121.8(15) . . ?
C16 N1 C15 120.7(16) . . ?
C13 N2 C17 117.7(18) . . ?
C13 N2 C18 121.1(17) . . ?
C18 N2 C17 121(2) . . ?
C14 O1 H1 109.5 . . ?
C4 O2 Tb1 133.2(8) . . ?
C2 O3 Tb1 171.4(9) . . ?
C4 O4 Tb1 142.1(7) . 2_566 ?
C16 O5 Tb1 138.8(9) . . ?
C2 O6 Tb1 108.0(6) . 2_566 ?
C7 O7 Tb1 91.4(6) . . ?
C7 O8 Tb1 93.7(6) . . ?
C9 O9 H9 109.5 . . ?
C13 O11 Tb1 134.8(10) . . ?
C6 O12 H12A 109.5 . . ?
O2 Tb1 O4 128.4(3) . 2_566 ?
O2 Tb1 O6 81.7(3) . 2_566 ?
O2 Tb1 O7 153.4(3) . . ?
O2 Tb1 O8 143.3(3) . . ?
O2 Tb1 O11 74.5(3) . . ?
O3 Tb1 O2 78.4(3) . . ?
O3 Tb1 O4 75.2(3) . 2_566 ?
O3 Tb1 O6 123.0(3) . 2_566 ?
O3 Tb1 O7 128.1(3) . . ?
O3 Tb1 O8 83.1(3) . . ?
O3 Tb1 O11 79.2(4) . . ?
O4 Tb1 O6 76.9(3) 2_566 2_566 ?
O4 Tb1 O7 68.5(3) 2_566 . ?
O4 Tb1 O8 75.4(3) 2_566 . ?
O4 Tb1 O11 139.7(3) 2_566 . ?
O5 Tb1 O2 79.9(3) . . ?
O5 Tb1 O3 147.8(4) . . ?
O5 Tb1 O4 136.9(3) . 2_566 ?
O5 Tb1 O6 76.5(4) . 2_566 ?
O5 Tb1 O7 75.2(3) . . ?
O5 Tb1 O8 100.9(4) . . ?
O5 Tb1 O11 72.3(4) . . ?
O6 Tb1 O7 83.4(3) 2_566 . ?
O6 Tb1 O8 134.6(3) 2_566 . ?
O6 Tb1 O11 143.3(4) 2_566 . ?
O8 Tb1 O7 53.1(3) . . ?
O11 Tb1 O7 106.2(3) . . ?
O11 Tb1 O8 71.1(3) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O1 H1 O8 0.84 1.88 2.605(13) 143.2 . yes
O9 H9 O4 0.84 1.94 2.649(13) 141.3 2_556 yes
O12 H12A O6 0.84 1.85 2.597(12) 146.8 2_666 yes

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
C1 C4 O2 Tb1 139.1(9) . . . . ?
C1 C4 O4 Tb1 -174.7(8) . . . 2_566 ?
C1 C8 C9 C1 -3(2) . . . 2_556 ?
C1 C8 C9 O9 180.0(11) . . . . ?
C2 C3 C5 C6 177.3(14) . . . . ?
C3 C2 O6 Tb1 -176.4(9) . . . 2_566 ?
C3 C5 C6 C3 2(3) . . . 2_666 ?
C3 C5 C6 O12 -176.9(15) . . . . ?
C4 C1 C8 C9 -176.4(11) . . . . ?
C6 C3 C5 C6 -2(3) 2_666 . . . ?
C7 C11 C12 C14 -179.1(15) . . . 2_677 ?
C7 C11 C14 C12 179.2(14) . . . 2_677 ?
C7 C11 C14 O1 -2(2) . . . . ?
C8 C1 C4 O2 9.6(15) . . . . ?
C8 C1 C4 O4 -172.4(10) . . . . ?
C9 C1 C4 O2 -169.4(10) 2_556 . . . ?
C9 C1 C4 O4 8.6(15) 2_556 . . . ?
C9 C1 C8 C9 3(2) 2_556 . . . ?
C11 C7 O7 Tb1 172.7(11) . . . . ?
C11 C7 O8 Tb1 -172.5(11) . . . . ?
C12 C11 C14 C12 -4(3) . . . 2_677 ?
C12 C11 C14 O1 174.9(18) . . . . ?
C14 C11 C12 C14 4(3) . . . 2_677 ?
N1 C16 O5 Tb1 -102.8(18) . . . . ?
N2 C13 O11 Tb1 170.6(12) . . . . ?
O2 C4 O4 Tb1 3.2(19) . . . 2_566 ?
O3 C2 C3 C5 -6.9(19) . . . . ?
O3 C2 C3 C6 172.5(13) . . . 2_666 ?
O3 C2 O6 Tb1 1.4(14) . . . 2_566 ?
O4 C4 O2 Tb1 -38.8(16) . . . . ?
O5 C16 N1 C10 -179.0(14) . . . . ?
O5 C16 N1 C15 -2(2) . . . . ?
O6 C2 C3 C5 171.0(13) . . . . ?
O6 C2 C3 C6 -9.6(19) . . . 2_666 ?
O7 C7 C11 C12 -7(2) . . . . ?
O7 C7 C11 C14 170.2(13) . . . . ?
O7 C7 O8 Tb1 7.6(14) . . . . ?
O8 C7 C11 C12 173.0(15) . . . . ?
O8 C7 C11 C14 -10(2) . . . . ?
O8 C7 O7 Tb1 -7.4(13) . . . . ?
O11 C13 N2 C17 179.5(12) . . . . ?
O11 C13 N2 C18 -1(2) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.500 0.000 0.500 213.1 0.0 ?


_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 1.566
_oxdiff_exptl_absorpt_empirical_full_min 0.762

# start Validation Reply Form
_vrf_PLAT027_SION2_200K_cool     
;
PROBLEM: _diffrn_reflns_theta_full value (too) Low ......      26.00 Degree
RESPONSE: Our value of max sin(theta)/lambda of 0.56 is close to the recommended 
		  value of 0.60. Higer values of sin(theta)/lambda were not available due 
		  to the beamline experimental set-up limitations. 
;
_vrf_PLAT029_SION2_200K_cool     
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.710 Why?  
RESPONSE: The data were collected upon the spindle rotation. Therefore, a 
		  limited portion of the reciprocal space could be probed.
;
# 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_SION2_340K_cool
_database_code_depnum_ccdc_archive 'CCDC 1941023'
loop_
_audit_author_name
_audit_author_address
'Andrzej Gladysiak'
;Ecole polytechnique federale de Lausanne
Switzerland
;
_audit_update_record             
;
2019-07-16 deposited with the CCDC.	2019-08-12 downloaded from the CCDC.
;
_audit_creation_date             2019-05-28
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C18 H20 N2 O11 Tb'
_chemical_formula_sum            'C18 H20 N2 O11 Tb'
_chemical_formula_weight         599.28
_chemical_melting_point          ?
_chemical_oxdiff_formula         C21H27N3O12Tb
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0045 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'
N N 0.0083 0.0040 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0145 0.0076 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.0972 4.9386 '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                   10.6765(7)
_cell_length_b                   11.1609(5)
_cell_length_c                   11.6592(6)
_cell_angle_alpha                96.727(4)
_cell_angle_beta                 111.531(5)
_cell_angle_gamma                101.573(5)
_cell_volume                     1238.03(13)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2938
_cell_measurement_temperature    340.0
_cell_measurement_theta_max      32.2610
_cell_measurement_theta_min      2.0830
_shelx_estimated_absorpt_T_max   0.779
_shelx_estimated_absorpt_T_min   0.521
_exptl_absorpt_coefficient_mu    3.754
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78887
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.608
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             590
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0093
_diffrn_reflns_av_unetI/netI     0.0143
_diffrn_reflns_Laue_measured_fraction_full 0.715
_diffrn_reflns_Laue_measured_fraction_max 0.548
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6921
_diffrn_reflns_point_group_measured_fraction_full 0.715
_diffrn_reflns_point_group_measured_fraction_max 0.548
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         32.204
_diffrn_reflns_theta_min         2.101
_diffrn_ambient_temperature      340.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            PILATUS2M
_diffrn_measured_fraction_theta_full 0.715
_diffrn_measured_fraction_theta_max 0.548
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      0.00 360.00   1.00    1.00    --    0.00   0.00   0.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  PILATUS@SNBL
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0668867000
_diffrn_orient_matrix_UB_12      -0.0029869000
_diffrn_orient_matrix_UB_13      -0.0122460000
_diffrn_orient_matrix_UB_21      0.0459115000
_diffrn_orient_matrix_UB_22      0.0511542000
_diffrn_orient_matrix_UB_23      0.0615482000
_diffrn_orient_matrix_UB_31      0.0107931000
_diffrn_orient_matrix_UB_32      -0.0524588000
_diffrn_orient_matrix_UB_33      0.0390822000
_diffrn_radiation_monochromator  'Si (111)'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.78405
_diffrn_source                   
'European Synchrotron Radiation Facility, BM01 beamline'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3370
_reflns_number_total             3566
_reflns_odcompleteness_completeness 63.24
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     29.34
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         5.610
_refine_diff_density_min         -0.772
_refine_diff_density_rms         0.224
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     292
_refine_ls_number_reflns         3566
_refine_ls_number_restraints     34
_refine_ls_R_factor_all          0.0701
_refine_ls_R_factor_gt           0.0680
_refine_ls_restrained_S_all      6.203
_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)+(0.1391P)²+4.6194P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1785
_refine_ls_wR_factor_ref         0.1821
_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
 C12_$8-O1 \\sim O1-C11
 with sigma of 0.05
 C17-C13 \\sim C13-C18
 with sigma of 0.02
3. Restrained planarity
 C13, C17, C18, N2, O11
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C17) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
5. Rigid body (RIGU) restrains
 O11, C13, N2, C18, C17
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Me refined with riding coordinates:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C)
6.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C8(H8), C12(H12), C13(H13), C16(H16)
6.c Tetrahedral OH refined with riding coordinates:
 O1(H1), O12(H12A)
6.d Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C15(H15A,H15B,H15C)
6.e Idealised tetrahedral OH refined as rotating group:
 O9(H9)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
C1 C -0.0209(11) 0.1201(10) 0.4966(10) 0.053(3) Uani 1 1 d . . . . .
C2 C 0.2054(9) 0.4876(10) 0.4339(10) 0.052(3) Uani 1 1 d . . . . .
C3 C 0.3580(8) 0.4949(10) 0.4673(10) 0.052(3) Uani 1 1 d . . . . .
C4 C -0.0370(9) 0.2522(9) 0.4973(11) 0.051(3) Uani 1 1 d . . . . .
C5 C 0.4543(10) 0.5417(13) 0.5909(11) 0.068(4) Uani 1 1 d . . . . .
H5 H 0.424141 0.570816 0.651578 0.081 Uiso 1 1 calc R . . . .
C6 C 0.5962(10) 0.5462(13) 0.6266(10) 0.064(3) Uani 1 1 d . . . . .
C7 C 0.3046(9) 0.7588(10) 0.8577(10) 0.051(3) Uani 1 1 d . . . . .
C8 C 0.0024(12) 0.0743(11) 0.6062(10) 0.058(3) Uani 1 1 d . . . . .
H8 H 0.004742 0.124046 0.677135 0.070 Uiso 1 1 calc R . . . .
C9 C 0.0227(12) -0.0460(11) 0.6121(10) 0.056(3) Uani 1 1 d . . . . .
C10 C 0.047(2) 0.1766(19) 0.988(2) 0.111(6) Uani 1 1 d . . . . .
H10A H 0.002104 0.173007 1.046419 0.166 Uiso 1 1 calc GR . . . .
H10B H 0.145411 0.189225 1.033689 0.166 Uiso 1 1 calc GR . . . .
H10C H 0.009424 0.099580 0.926901 0.166 Uiso 1 1 calc GR . . . .
C11 C 0.4014(9) 0.8850(9) 0.9316(10) 0.053(3) Uani 1 1 d D . . . .
C12 C 0.3629(11) 0.9623(13) 0.9899(14) 0.077(4) Uani 1 1 d D . . . .
H12 H 0.272833 0.940754 0.986852 0.092 Uiso 1 1 calc R . . A 2
C13 C 0.3131(15) 0.3307(14) 0.7177(15) 0.091(5) Uani 1 1 d D U . . .
H13 H 0.245493 0.283842 0.640597 0.110 Uiso 1 1 calc R . . . .
C14 C 0.5434(11) 0.9136(13) 0.9370(14) 0.079(4) Uani 1 1 d . . . . .
C15 C -0.1257(18) 0.283(2) 0.862(2) 0.120(7) Uani 1 1 d . . . . .
H15A H -0.165158 0.292227 0.923298 0.180 Uiso 1 1 calc GR . . . .
H15B H -0.178124 0.206434 0.800785 0.180 Uiso 1 1 calc GR . . . .
H15C H -0.129136 0.352248 0.820458 0.180 Uiso 1 1 calc GR . . . .
C16 C 0.1171(16) 0.3693(18) 0.9266(16) 0.083(5) Uani 1 1 d . . . . .
H16 H 0.209258 0.368419 0.970259 0.099 Uiso 1 1 calc R . . . .
C17 C 0.436(3) 0.181(2) 0.694(3) 0.179(10) Uani 1 1 d D U . . .
H17A H 0.523724 0.163513 0.739387 0.268 Uiso 1 1 calc R . . . .
H17B H 0.361009 0.110745 0.683100 0.268 Uiso 1 1 calc R . . . .
H17C H 0.431340 0.194382 0.612770 0.268 Uiso 1 1 calc R . . . .
C18 C 0.534(3) 0.364(3) 0.885(2) 0.175(12) Uani 1 1 d D U . . .
H18A H 0.609309 0.324444 0.906955 0.263 Uiso 1 1 calc R . . . .
H18B H 0.567267 0.447656 0.877252 0.263 Uiso 1 1 calc R . . . .
H18C H 0.497437 0.364981 0.948576 0.263 Uiso 1 1 calc R . . . .
N1 N 0.0221(13) 0.2791(13) 0.9259(12) 0.079(3) Uani 1 1 d . . . . .
N2 N 0.4251(15) 0.2940(16) 0.7657(17) 0.116(5) Uani 1 1 d . U . . .
O1 O 0.5954(11) 0.8250(12) 0.8791(15) 0.133(6) Uani 1 1 d D . . . .
H1 H 0.530871 0.763621 0.835928 0.200 Uiso 1 1 calc R . . . .
O2 O -0.0095(7) 0.3200(6) 0.6037(7) 0.0537(18) Uani 1 1 d . . . . .
O3 O 0.1634(7) 0.5077(8) 0.5201(8) 0.060(2) Uani 1 1 d . . . . .
O4 O -0.0725(8) 0.2860(7) 0.3924(7) 0.059(2) Uani 1 1 d . . . . .
O5 O 0.0966(11) 0.4600(11) 0.8731(9) 0.078(3) Uani 1 1 d . . . . .
O6 O 0.1217(6) 0.4593(8) 0.3181(7) 0.0572(19) Uani 1 1 d . . . . .
O7 O 0.1863(7) 0.7275(7) 0.8663(7) 0.0575(19) Uani 1 1 d . . . . .
O8 O 0.3403(7) 0.6865(7) 0.7916(9) 0.069(3) Uani 1 1 d . . . . .
O9 O 0.0436(14) -0.0803(10) 0.7247(9) 0.086(3) Uani 1 1 d . . . . .
H9 H 0.074351 -0.142051 0.726849 0.129 Uiso 1 1 calc GR . . . .
O11 O 0.2883(9) 0.4227(10) 0.7657(11) 0.087(3) Uani 1 1 d . U . . .
O12 O 0.6845(9) 0.5891(13) 0.7514(8) 0.093(4) Uani 1 1 d . . . . .
H12A H 0.764091 0.587825 0.760417 0.139 Uiso 1 1 calc R . . . .
Tb1 Tb 0.10938(3) 0.53469(3) 0.69702(4) 0.0420(2) 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
C1 C4 1.517(15) . ?
C1 C8 1.389(18) . ?
C1 C9 1.422(14) 2_556 ?
C2 C3 1.512(11) . ?
C2 O3 1.257(12) . ?
C2 O6 1.274(13) . ?
C3 C5 1.388(14) . ?
C3 C6 1.420(14) 2_666 ?
C4 O2 1.274(12) . ?
C4 O4 1.268(15) . ?
C5 H5 0.9300 . ?
C5 C6 1.404(13) . ?
C6 O12 1.372(13) . ?
C7 C11 1.507(12) . ?
C7 O7 1.286(12) . ?
C7 O8 1.259(12) . ?
C8 H8 0.9300 . ?
C8 C9 1.407(17) . ?
C9 O9 1.363(16) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C10 N1 1.44(2) . ?
C11 C12 1.258(15) . ?
C11 C14 1.462(14) . ?
C12 H12 0.9300 . ?
C12 C14 1.478(16) 2_677 ?
C13 H13 0.9300 . ?
C13 N2 1.29(2) . ?
C13 O11 1.232(18) . ?
C14 O1 1.443(14) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C15 N1 1.49(2) . ?
C16 H16 0.9300 . ?
C16 N1 1.28(2) . ?
C16 O5 1.26(2) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C17 N2 1.48(3) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C18 N2 1.44(3) . ?
O1 H1 0.8200 . ?
O2 Tb1 2.385(6) . ?
O3 Tb1 2.340(8) . ?
O4 Tb1 2.398(9) 2_566 ?
O5 Tb1 2.343(11) . ?
O6 Tb1 2.424(6) 2_566 ?
O7 Tb1 2.511(7) . ?
O8 Tb1 2.461(7) . ?
O9 H9 0.8200 . ?
O11 Tb1 2.434(9) . ?
O12 H12A 0.8200 . ?

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
C8 C1 C4 118.9(9) . . ?
C8 C1 C9 120.1(10) . 2_556 ?
C9 C1 C4 121.0(11) 2_556 . ?
O3 C2 C3 119.7(9) . . ?
O3 C2 O6 121.5(8) . . ?
O6 C2 C3 118.8(8) . . ?
C5 C3 C2 119.9(8) . . ?
C5 C3 C6 119.5(8) . 2_666 ?
C6 C3 C2 120.5(9) 2_666 . ?
O2 C4 C1 117.0(11) . . ?
O4 C4 C1 117.0(9) . . ?
O4 C4 O2 126.0(10) . . ?
C3 C5 H5 119.2 . . ?
C3 C5 C6 121.7(9) . . ?
C6 C5 H5 119.2 . . ?
C5 C6 C3 118.8(9) . 2_666 ?
O12 C6 C3 122.8(8) . 2_666 ?
O12 C6 C5 118.5(9) . . ?
O7 C7 C11 117.7(8) . . ?
O8 C7 C11 120.6(9) . . ?
O8 C7 O7 121.6(8) . . ?
C1 C8 H8 119.3 . . ?
C1 C8 C9 121.3(9) . . ?
C9 C8 H8 119.3 . . ?
C8 C9 C1 118.6(11) . 2_556 ?
O9 C9 C1 125.7(11) . 2_556 ?
O9 C9 C8 115.6(9) . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N1 C10 H10A 109.5 . . ?
N1 C10 H10B 109.5 . . ?
N1 C10 H10C 109.5 . . ?
C12 C11 C7 121.4(9) . . ?
C12 C11 C14 120.7(9) . . ?
C14 C11 C7 117.9(9) . . ?
C11 C12 H12 119.0 . . ?
C11 C12 C14 122.0(10) . 2_677 ?
C14 C12 H12 119.0 2_677 . ?
N2 C13 H13 117.3 . . ?
O11 C13 H13 117.3 . . ?
O11 C13 N2 125.4(16) . . ?
C11 C14 C12 117.2(9) . 2_677 ?
O1 C14 C11 122.8(9) . . ?
O1 C14 C12 119.9(9) . 2_677 ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N1 C15 H15A 109.5 . . ?
N1 C15 H15B 109.5 . . ?
N1 C15 H15C 109.5 . . ?
N1 C16 H16 117.2 . . ?
O5 C16 H16 117.2 . . ?
O5 C16 N1 125.5(16) . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N2 C17 H17A 109.5 . . ?
N2 C17 H17B 109.5 . . ?
N2 C17 H17C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N2 C18 H18A 109.5 . . ?
N2 C18 H18B 109.5 . . ?
N2 C18 H18C 109.5 . . ?
C10 N1 C15 117.2(15) . . ?
C16 N1 C10 125.0(16) . . ?
C16 N1 C15 117.7(17) . . ?
C13 N2 C17 117.7(18) . . ?
C13 N2 C18 119.8(18) . . ?
C18 N2 C17 123(2) . . ?
C14 O1 H1 109.5 . . ?
C4 O2 Tb1 132.8(7) . . ?
C2 O3 Tb1 172.3(8) . . ?
C4 O4 Tb1 141.3(6) . 2_566 ?
C16 O5 Tb1 140.2(10) . . ?
C2 O6 Tb1 108.9(5) . 2_566 ?
C7 O7 Tb1 90.8(5) . . ?
C7 O8 Tb1 93.8(6) . . ?
C9 O9 H9 109.5 . . ?
C13 O11 Tb1 135.2(10) . . ?
C6 O12 H12A 109.5 . . ?
O2 Tb1 O4 128.0(3) . 2_566 ?
O2 Tb1 O6 81.2(3) . 2_566 ?
O2 Tb1 O7 152.8(3) . . ?
O2 Tb1 O8 144.0(2) . . ?
O2 Tb1 O11 75.0(3) . . ?
O3 Tb1 O2 78.8(3) . . ?
O3 Tb1 O4 75.2(3) . 2_566 ?
O3 Tb1 O5 147.8(4) . . ?
O3 Tb1 O6 122.6(3) . 2_566 ?
O3 Tb1 O7 128.4(3) . . ?
O3 Tb1 O8 83.3(3) . . ?
O3 Tb1 O11 79.0(3) . . ?
O4 Tb1 O6 76.4(3) 2_566 2_566 ?
O4 Tb1 O7 68.9(3) 2_566 . ?
O4 Tb1 O8 75.6(3) 2_566 . ?
O4 Tb1 O11 139.7(3) 2_566 . ?
O5 Tb1 O2 79.4(3) . . ?
O5 Tb1 O4 137.0(3) . 2_566 ?
O5 Tb1 O6 76.5(3) . 2_566 ?
O5 Tb1 O7 75.3(3) . . ?
O5 Tb1 O8 101.3(4) . . ?
O5 Tb1 O11 72.8(4) . . ?
O6 Tb1 O7 83.4(2) 2_566 . ?
O6 Tb1 O8 134.4(2) 2_566 . ?
O6 Tb1 O11 143.9(3) 2_566 . ?
O8 Tb1 O7 53.1(2) . . ?
O11 Tb1 O7 106.1(3) . . ?
O11 Tb1 O8 71.0(3) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O1 H1 O8 0.82 1.89 2.598(12) 144.0 . yes
O9 H9 O4 0.82 1.99 2.663(12) 138.9 2_556 yes
O12 H12A O6 0.82 1.89 2.608(11) 146.0 2_666 yes

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
C1 C4 O2 Tb1 139.0(8) . . . . ?
C1 C4 O4 Tb1 -175.4(7) . . . 2_566 ?
C1 C8 C9 C1 0.9(19) . . . 2_556 ?
C1 C8 C9 O9 -179.5(11) . . . . ?
C2 C3 C5 C6 177.8(13) . . . . ?
C3 C2 O6 Tb1 -177.8(8) . . . 2_566 ?
C3 C5 C6 C3 2(2) . . . 2_666 ?
C3 C5 C6 O12 -177.5(14) . . . . ?
C4 C1 C8 C9 -177.9(10) . . . . ?
C6 C3 C5 C6 -2(2) 2_666 . . . ?
C7 C11 C12 C14 179.9(14) . . . 2_677 ?
C7 C11 C14 C12 -179.8(13) . . . 2_677 ?
C7 C11 C14 O1 -2(2) . . . . ?
C8 C1 C4 O2 9.2(14) . . . . ?
C8 C1 C4 O4 -172.9(10) . . . . ?
C9 C1 C4 O2 -167.8(10) 2_556 . . . ?
C9 C1 C4 O4 10.2(14) 2_556 . . . ?
C9 C1 C8 C9 -0.9(19) 2_556 . . . ?
C11 C7 O7 Tb1 172.9(10) . . . . ?
C11 C7 O8 Tb1 -172.7(10) . . . . ?
C12 C11 C14 C12 -2(3) . . . 2_677 ?
C12 C11 C14 O1 175.7(17) . . . . ?
C14 C11 C12 C14 2(3) . . . 2_677 ?
N1 C16 O5 Tb1 -106.3(19) . . . . ?
N2 C13 O11 Tb1 171.2(12) . . . . ?
O2 C4 O4 Tb1 2.3(17) . . . 2_566 ?
O3 C2 C3 C5 -9.7(18) . . . . ?
O3 C2 C3 C6 170.1(12) . . . 2_666 ?
O3 C2 O6 Tb1 3.3(13) . . . 2_566 ?
O4 C4 O2 Tb1 -38.7(14) . . . . ?
O5 C16 N1 C10 -179.4(16) . . . . ?
O5 C16 N1 C15 -3(3) . . . . ?
O6 C2 C3 C5 171.4(12) . . . . ?
O6 C2 C3 C6 -8.9(17) . . . 2_666 ?
O7 C7 C11 C12 -6.8(19) . . . . ?
O7 C7 C11 C14 171.2(12) . . . . ?
O7 C7 O8 Tb1 8.4(13) . . . . ?
O8 C7 C11 C12 174.2(14) . . . . ?
O8 C7 C11 C14 -7.7(19) . . . . ?
O8 C7 O7 Tb1 -8.2(12) . . . . ?
O11 C13 N2 C17 180.0(12) . . . . ?
O11 C13 N2 C18 0(2) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.500 0.000 0.500 213.4 0.0 ?
2 0.233 0.148 0.859 8.1 0.1 ?
3 0.767 0.852 0.141 8.1 0.0 ?


_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 1.202
_oxdiff_exptl_absorpt_empirical_full_min 0.885

# start Validation Reply Form
_vrf_PLAT027_SION2_340K_cool     
;
PROBLEM: _diffrn_reflns_theta_full value (too) Low ......      26.00 Degree
RESPONSE: Our value of max sin(theta)/lambda of 0.56 is close to the recommended 
		  value of 0.60. Higer values of sin(theta)/lambda were not available due 
		  to the beamline experimental set-up limitations.
;
_vrf_PLAT029_SION2_340K_cool     
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.715 Why?  
RESPONSE: The data were collected upon the spindle rotation. Therefore, a 
		  limited portion of the reciprocal space could be probed.
;
# 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_SION2_360K_cool
_database_code_depnum_ccdc_archive 'CCDC 1941024'
loop_
_audit_author_name
_audit_author_address
'Andrzej Gladysiak'
;Ecole polytechnique federale de Lausanne
Switzerland
;
_audit_update_record             
;
2019-07-16 deposited with the CCDC.	2019-08-12 downloaded from the CCDC.
;
_audit_creation_date             2019-05-28
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C18 H20 N2 O11 Tb'
_chemical_formula_sum            'C18 H20 N2 O11 Tb'
_chemical_formula_weight         599.28
_chemical_melting_point          ?
_chemical_oxdiff_formula         C21H27N3O12Tb
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0045 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'
N N 0.0083 0.0040 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0145 0.0076 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.0972 4.9386 '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                   10.6634(8)
_cell_length_b                   11.1405(7)
_cell_length_c                   11.6932(8)
_cell_angle_alpha                96.751(5)
_cell_angle_beta                 111.604(7)
_cell_angle_gamma                101.562(6)
_cell_volume                     1237.08(16)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2785
_cell_measurement_temperature    360.0
_cell_measurement_theta_max      32.2970
_cell_measurement_theta_min      2.0980
_shelx_estimated_absorpt_T_max   0.779
_shelx_estimated_absorpt_T_min   0.520
_exptl_absorpt_coefficient_mu    3.757
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78438
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'light orange'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.609
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             590
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0121
_diffrn_reflns_av_unetI/netI     0.0180
_diffrn_reflns_Laue_measured_fraction_full 0.713
_diffrn_reflns_Laue_measured_fraction_max 0.542
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6912
_diffrn_reflns_point_group_measured_fraction_full 0.713
_diffrn_reflns_point_group_measured_fraction_max 0.542
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         32.328
_diffrn_reflns_theta_min         2.105
_diffrn_ambient_temperature      360.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            PILATUS2M
_diffrn_measured_fraction_theta_full 0.713
_diffrn_measured_fraction_theta_max 0.542
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      0.00 360.00   1.00    1.00    --    0.00   0.00   0.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  PILATUS@SNBL
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0663349000
_diffrn_orient_matrix_UB_12      -0.0034848000
_diffrn_orient_matrix_UB_13      -0.0131009000
_diffrn_orient_matrix_UB_21      0.0469667000
_diffrn_orient_matrix_UB_22      0.0509078000
_diffrn_orient_matrix_UB_23      0.0615055000
_diffrn_orient_matrix_UB_31      0.0107772000
_diffrn_orient_matrix_UB_32      -0.0528665000
_diffrn_orient_matrix_UB_33      0.0385552000
_diffrn_radiation_monochromator  'Si (111)'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.78405
_diffrn_source                   
'European Synchrotron Radiation Facility, BM01 beamline'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3338
_reflns_number_total             3565
_reflns_odcompleteness_completeness 63.09
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     29.34
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         6.201
_refine_diff_density_min         -1.145
_refine_diff_density_rms         0.241
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     291
_refine_ls_number_reflns         3565
_refine_ls_number_restraints     60
_refine_ls_R_factor_all          0.0771
_refine_ls_R_factor_gt           0.0748
_refine_ls_restrained_S_all      6.432
_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)+(0.1435P)²+4.7065P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1937
_refine_ls_wR_factor_ref         0.1974
_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
 C14-O1
 1.38 with sigma of 0.02
 C12_$4-O1 \\sim O1-C11
 with sigma of 0.05
 C17-C13 \\sim C13-C18
 with sigma of 0.02
 C12-C11 \\sim C11-C14
 with sigma of 0.02
3. Restrained planarity
 C13, C17, C18, N2, O11
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C17) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
5. Rigid body (RIGU) restrains
 O11, C13, N2, C18, C17
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C12, C11, C7, C14, O1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Me refined with riding coordinates:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C)
6.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C8(H8), C12(H12), C13(H13), C16(H16)
6.c Tetrahedral OH refined with riding coordinates:
 O1(H1), O9(H9), O12(H12A)
6.d Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C15(H15A,H15B,H15C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
C1 C -0.0209(12) 0.1211(11) 0.4954(11) 0.055(3) Uani 1 1 d . . . . .
C2 C 0.2060(10) 0.4886(11) 0.4351(11) 0.055(3) Uani 1 1 d . . . . .
C3 C 0.3587(9) 0.4943(11) 0.4679(11) 0.056(3) Uani 1 1 d . . . . .
C4 C -0.0364(10) 0.2522(10) 0.4973(11) 0.052(3) Uani 1 1 d . . . . .
C5 C 0.4546(11) 0.5437(15) 0.5903(11) 0.071(4) Uani 1 1 d . . . . .
H5 H 0.425044 0.575083 0.650382 0.085 Uiso 1 1 calc R . . . .
C6 C 0.5973(11) 0.5470(14) 0.6253(11) 0.063(3) Uani 1 1 d . . . . .
C7 C 0.3049(10) 0.7587(11) 0.8580(11) 0.057(3) Uani 1 1 d . U . . .
C8 C 0.0015(15) 0.0728(12) 0.6056(13) 0.067(4) Uani 1 1 d . . . . .
H8 H 0.001933 0.121660 0.675952 0.080 Uiso 1 1 calc R . . . .
C9 C 0.0232(13) -0.0466(11) 0.6118(11) 0.059(3) Uani 1 1 d . . . . .
C10 C 0.048(3) 0.177(2) 0.989(3) 0.121(7) Uani 1 1 d . . . . .
H10A H 0.008976 0.177088 1.050583 0.181 Uiso 1 1 calc GR . . . .
H10B H 0.147335 0.187339 1.029492 0.181 Uiso 1 1 calc GR . . . .
H10C H 0.005953 0.098836 0.928615 0.181 Uiso 1 1 calc GR . . . .
C11 C 0.4034(9) 0.8845(10) 0.9297(11) 0.056(3) Uani 1 1 d D U . . .
C12 C 0.3625(12) 0.9644(13) 0.9923(14) 0.075(4) Uani 1 1 d D U . . .
H12 H 0.273322 0.942386 0.991591 0.090 Uiso 1 1 calc R . . A 2
C13 C 0.3136(17) 0.3316(15) 0.7153(18) 0.096(5) Uani 1 1 d D U . . .
H13 H 0.248016 0.286496 0.636635 0.115 Uiso 1 1 calc R . . . .
C14 C 0.5416(11) 0.9119(14) 0.9369(15) 0.085(5) Uani 1 1 d D U . . .
C15 C -0.124(2) 0.282(3) 0.860(3) 0.135(9) Uani 1 1 d . . . . .
H15A H -0.162820 0.298810 0.920997 0.203 Uiso 1 1 calc GR . . . .
H15B H -0.178418 0.203282 0.803763 0.203 Uiso 1 1 calc GR . . . .
H15C H -0.126873 0.347611 0.813408 0.203 Uiso 1 1 calc GR . . . .
C16 C 0.1185(19) 0.370(2) 0.9266(18) 0.093(6) Uani 1 1 d . . . . .
H16 H 0.211059 0.370219 0.971122 0.112 Uiso 1 1 calc R . . . .
C17 C 0.437(4) 0.181(3) 0.689(3) 0.192(11) Uani 1 1 d D U . . .
H17A H 0.523024 0.161664 0.734616 0.288 Uiso 1 1 calc R . . . .
H17B H 0.359664 0.111155 0.674329 0.288 Uiso 1 1 calc R . . . .
H17C H 0.434933 0.198773 0.610309 0.288 Uiso 1 1 calc R . . . .
C18 C 0.532(3) 0.363(4) 0.887(3) 0.203(16) Uani 1 1 d D U . . .
H18A H 0.606967 0.323130 0.910098 0.304 Uiso 1 1 calc R . . . .
H18B H 0.566818 0.447718 0.882247 0.304 Uiso 1 1 calc R . . . .
H18C H 0.492742 0.362598 0.948905 0.304 Uiso 1 1 calc R . . . .
N1 N 0.0229(14) 0.2775(14) 0.9261(13) 0.083(4) Uani 1 1 d . . . . .
N2 N 0.4256(17) 0.2957(18) 0.7665(19) 0.121(6) Uani 1 1 d . U . . .
O1 O 0.5959(12) 0.8242(13) 0.8800(17) 0.146(7) Uani 1 1 d D U . . .
H1 H 0.532136 0.762234 0.836587 0.219 Uiso 1 1 calc R . . . .
O2 O -0.0093(8) 0.3202(7) 0.6029(8) 0.058(2) Uani 1 1 d . . . . .
O3 O 0.1648(8) 0.5084(9) 0.5219(9) 0.065(2) Uani 1 1 d . . . . .
O4 O -0.0722(9) 0.2861(8) 0.3936(8) 0.064(2) Uani 1 1 d . . . . .
O5 O 0.0967(13) 0.4592(12) 0.8717(10) 0.082(3) Uani 1 1 d . . . . .
O6 O 0.1215(7) 0.4606(9) 0.3194(8) 0.061(2) Uani 1 1 d . . . . .
O7 O 0.1869(8) 0.7276(8) 0.8664(7) 0.060(2) Uani 1 1 d . . . . .
O8 O 0.3408(8) 0.6871(8) 0.7913(10) 0.072(3) Uani 1 1 d . . . . .
O9 O 0.0440(14) -0.0808(11) 0.7243(10) 0.094(4) Uani 1 1 d . . . . .
H9 H 0.055337 -0.151587 0.720160 0.141 Uiso 1 1 calc R . . . .
O11 O 0.2889(10) 0.4228(11) 0.7655(12) 0.095(4) Uani 1 1 d . U . . .
O12 O 0.6863(9) 0.5913(15) 0.7501(9) 0.101(5) Uani 1 1 d . . . . .
H12A H 0.765974 0.590015 0.759331 0.152 Uiso 1 1 calc R . . . .
Tb1 Tb 0.10974(4) 0.53476(4) 0.69631(4) 0.0447(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
C1 C4 1.502(16) . ?
C1 C8 1.41(2) . ?
C1 C9 1.408(15) 2_556 ?
C2 C3 1.515(12) . ?
C2 O3 1.259(14) . ?
C2 O6 1.277(14) . ?
C3 C5 1.381(15) . ?
C3 C6 1.403(15) 2_666 ?
C4 O2 1.270(13) . ?
C4 O4 1.258(16) . ?
C5 H5 0.9300 . ?
C5 C6 1.414(14) . ?
C6 O12 1.377(14) . ?
C7 C11 1.502(13) . ?
C7 O7 1.280(13) . ?
C7 O8 1.259(14) . ?
C8 H8 0.9300 . ?
C8 C9 1.401(19) . ?
C9 O9 1.365(17) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C10 N1 1.43(3) . ?
C11 C12 1.325(13) . ?
C11 C14 1.413(12) . ?
C12 H12 0.9300 . ?
C12 C14 1.475(16) 2_677 ?
C13 H13 0.9300 . ?
C13 N2 1.29(2) . ?
C13 O11 1.24(2) . ?
C14 O1 1.445(13) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C15 N1 1.49(2) . ?
C16 H16 0.9300 . ?
C16 N1 1.29(2) . ?
C16 O5 1.26(3) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C17 N2 1.53(3) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C18 N2 1.44(3) . ?
O1 H1 0.8200 . ?
O2 Tb1 2.380(7) . ?
O3 Tb1 2.324(9) . ?
O4 Tb1 2.399(10) 2_566 ?
O5 Tb1 2.346(12) . ?
O6 Tb1 2.416(7) 2_566 ?
O7 Tb1 2.516(7) . ?
O8 Tb1 2.460(7) . ?
O9 H9 0.8200 . ?
O11 Tb1 2.432(10) . ?
O12 H12A 0.8200 . ?

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
C8 C1 C4 119.0(10) . . ?
C9 C1 C4 121.8(12) 2_556 . ?
C9 C1 C8 119.2(11) 2_556 . ?
O3 C2 C3 119.6(10) . . ?
O3 C2 O6 121.7(9) . . ?
O6 C2 C3 118.7(9) . . ?
C5 C3 C2 119.2(9) . . ?
C5 C3 C6 120.3(9) . 2_666 ?
C6 C3 C2 120.4(9) 2_666 . ?
O2 C4 C1 117.7(11) . . ?
O4 C4 C1 116.7(9) . . ?
O4 C4 O2 125.6(11) . . ?
C3 C5 H5 119.6 . . ?
C3 C5 C6 120.8(10) . . ?
C6 C5 H5 119.6 . . ?
C3 C6 C5 118.8(10) 2_666 . ?
O12 C6 C3 123.3(9) . 2_666 ?
O12 C6 C5 117.9(10) . . ?
O7 C7 C11 118.9(9) . . ?
O8 C7 C11 119.0(9) . . ?
O8 C7 O7 122.0(9) . . ?
C1 C8 H8 119.1 . . ?
C9 C8 C1 121.8(11) . . ?
C9 C8 H8 119.1 . . ?
C8 C9 C1 119.0(12) . 2_556 ?
O9 C9 C1 125.5(12) . 2_556 ?
O9 C9 C8 115.5(10) . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N1 C10 H10A 109.5 . . ?
N1 C10 H10B 109.5 . . ?
N1 C10 H10C 109.5 . . ?
C12 C11 C7 119.6(9) . . ?
C12 C11 C14 121.0(9) . . ?
C14 C11 C7 119.3(9) . . ?
C11 C12 H12 120.0 . . ?
C11 C12 C14 120.0(9) . 2_677 ?
C14 C12 H12 120.0 2_677 . ?
N2 C13 H13 118.3 . . ?
O11 C13 H13 118.3 . . ?
O11 C13 N2 123.4(18) . . ?
C11 C14 C12 118.8(9) . 2_677 ?
C11 C14 O1 123.6(11) . . ?
O1 C14 C12 117.6(9) . 2_677 ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N1 C15 H15A 109.5 . . ?
N1 C15 H15B 109.5 . . ?
N1 C15 H15C 109.5 . . ?
N1 C16 H16 117.2 . . ?
O5 C16 H16 117.2 . . ?
O5 C16 N1 125.5(19) . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N2 C17 H17A 109.5 . . ?
N2 C17 H17B 109.5 . . ?
N2 C17 H17C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N2 C18 H18A 109.5 . . ?
N2 C18 H18B 109.5 . . ?
N2 C18 H18C 109.5 . . ?
C10 N1 C15 118.4(18) . . ?
C16 N1 C10 125.2(19) . . ?
C16 N1 C15 116(2) . . ?
C13 N2 C17 115(2) . . ?
C13 N2 C18 121(2) . . ?
C18 N2 C17 124(3) . . ?
C14 O1 H1 109.5 . . ?
C4 O2 Tb1 132.9(8) . . ?
C2 O3 Tb1 173.1(9) . . ?
C4 O4 Tb1 141.7(7) . 2_566 ?
C16 O5 Tb1 140.9(11) . . ?
C2 O6 Tb1 109.3(6) . 2_566 ?
C7 O7 Tb1 90.6(6) . . ?
C7 O8 Tb1 93.8(6) . . ?
C9 O9 H9 109.5 . . ?
C13 O11 Tb1 134.2(12) . . ?
C6 O12 H12A 109.5 . . ?
O2 Tb1 O4 127.7(3) . 2_566 ?
O2 Tb1 O6 80.8(3) . 2_566 ?
O2 Tb1 O7 152.6(3) . . ?
O2 Tb1 O8 144.1(3) . . ?
O2 Tb1 O11 75.1(4) . . ?
O3 Tb1 O2 78.9(3) . . ?
O3 Tb1 O4 75.1(3) . 2_566 ?
O3 Tb1 O5 147.6(4) . . ?
O3 Tb1 O6 122.9(3) . 2_566 ?
O3 Tb1 O7 128.5(3) . . ?
O3 Tb1 O8 83.1(3) . . ?
O3 Tb1 O11 78.9(4) . . ?
O4 Tb1 O6 76.6(3) 2_566 2_566 ?
O4 Tb1 O7 69.4(3) 2_566 . ?
O4 Tb1 O8 75.8(3) 2_566 . ?
O4 Tb1 O11 139.8(4) 2_566 . ?
O5 Tb1 O2 79.3(4) . . ?
O5 Tb1 O4 137.2(4) . 2_566 ?
O5 Tb1 O6 76.4(4) . 2_566 ?
O5 Tb1 O7 75.1(4) . . ?
O5 Tb1 O8 101.3(4) . . ?
O5 Tb1 O11 72.5(4) . . ?
O6 Tb1 O7 83.7(3) 2_566 . ?
O6 Tb1 O8 134.6(3) 2_566 . ?
O6 Tb1 O11 143.6(4) 2_566 . ?
O8 Tb1 O7 53.0(3) . . ?
O11 Tb1 O7 105.9(4) . . ?
O11 Tb1 O8 71.1(4) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O1 H1 O8 0.82 1.89 2.587(14) 142.7 . yes
O9 H9 O4 0.82 1.97 2.657(13) 141.6 2_556 yes
O12 H12A O6 0.82 1.89 2.605(12) 145.4 2_666 yes

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
C1 C4 O2 Tb1 138.8(9) . . . . ?
C1 C4 O4 Tb1 -175.4(8) . . . 2_566 ?
C1 C8 C9 C1 -1(2) . . . 2_556 ?
C1 C8 C9 O9 179.7(12) . . . . ?
C2 C3 C5 C6 178.0(14) . . . . ?
C3 C2 O6 Tb1 -178.7(9) . . . 2_566 ?
C3 C5 C6 C3 3(3) . . . 2_666 ?
C3 C5 C6 O12 -176.6(16) . . . . ?
C4 C1 C8 C9 -177.1(11) . . . . ?
C6 C3 C5 C6 -4(3) 2_666 . . . ?
C7 C11 C12 C14 179.9(15) . . . 2_677 ?
C7 C11 C14 C12 -179.9(15) . . . 2_677 ?
C7 C11 C14 O1 -1(3) . . . . ?
C8 C1 C4 O2 9.7(16) . . . . ?
C8 C1 C4 O4 -172.0(11) . . . . ?
C9 C1 C4 O2 -168.1(11) 2_556 . . . ?
C9 C1 C4 O4 10.2(16) 2_556 . . . ?
C9 C1 C8 C9 1(2) 2_556 . . . ?
C11 C7 O7 Tb1 172.1(11) . . . . ?
C11 C7 O8 Tb1 -171.9(11) . . . . ?
C12 C11 C14 C12 -5(3) . . . 2_677 ?
C12 C11 C14 O1 174.3(18) . . . . ?
C14 C11 C12 C14 5(3) . . . 2_677 ?
N1 C16 O5 Tb1 -107(2) . . . . ?
N2 C13 O11 Tb1 172.1(12) . . . . ?
O2 C4 O4 Tb1 2.7(19) . . . 2_566 ?
O3 C2 C3 C5 -12.0(19) . . . . ?
O3 C2 C3 C6 169.6(13) . . . 2_666 ?
O3 C2 O6 Tb1 3.0(15) . . . 2_566 ?
O4 C4 O2 Tb1 -39.3(16) . . . . ?
O5 C16 N1 C10 -179.7(19) . . . . ?
O5 C16 N1 C15 -3(3) . . . . ?
O6 C2 C3 C5 169.7(14) . . . . ?
O6 C2 C3 C6 -8.7(19) . . . 2_666 ?
O7 C7 C11 C12 -5(2) . . . . ?
O7 C7 C11 C14 170.2(14) . . . . ?
O7 C7 O8 Tb1 7.9(14) . . . . ?
O8 C7 C11 C12 174.8(15) . . . . ?
O8 C7 C11 C14 -10(2) . . . . ?
O8 C7 O7 Tb1 -7.7(14) . . . . ?
O11 C13 N2 C17 -179.8(12) . . . . ?
O11 C13 N2 C18 -1(2) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.500 0.000 0.500 211.8 0.0 ?
2 0.233 0.156 0.859 7.3 -0.1 ?
3 0.767 0.844 0.141 7.3 0.0 ?


_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 1.283
_oxdiff_exptl_absorpt_empirical_full_min 0.795

# start Validation Reply Form
_vrf_PLAT027_SION2_360K_cool     
;
PROBLEM: _diffrn_reflns_theta_full value (too) Low ......      26.00 Degree
RESPONSE: Our value of max sin(theta)/lambda of 0.56 is close to the recommended 
		  value of 0.60. Higer values of sin(theta)/lambda were not available due 
		  to the beamline experimental set-up limitations.
;
_vrf_PLAT029_SION2_360K_cool     
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.713 Why?  
RESPONSE: The data were collected upon the spindle rotation. Therefore, a 
		  limited portion of the reciprocal space could be probed.
;
# 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_SION2_260K_cool
_database_code_depnum_ccdc_archive 'CCDC 1941017'
loop_
_audit_author_name
_audit_author_address
'Andrzej Gladysiak'
;Ecole polytechnique federale de Lausanne
Switzerland
;
_audit_update_record             
;
2019-07-16 deposited with the CCDC.	2019-08-12 downloaded from the CCDC.
;
_audit_creation_date             2019-05-27
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C18 H20 N2 O11 Tb'
_chemical_formula_sum            'C18 H20 N2 O11 Tb'
_chemical_formula_weight         599.28
_chemical_melting_point          ?
_chemical_oxdiff_formula         C21H27N3O12Tb
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0045 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'
N N 0.0083 0.0040 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0145 0.0076 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.0972 4.9386 '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                   10.6565(6)
_cell_length_b                   11.1667(5)
_cell_length_c                   11.5332(6)
_cell_angle_alpha                96.830(4)
_cell_angle_beta                 111.282(5)
_cell_angle_gamma                101.473(4)
_cell_volume                     1225.53(12)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3110
_cell_measurement_temperature    260.0
_cell_measurement_theta_max      31.9620
_cell_measurement_theta_min      2.0770
_shelx_estimated_absorpt_T_max   0.777
_shelx_estimated_absorpt_T_min   0.518
_exptl_absorpt_coefficient_mu    3.793
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79637
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.624
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             590
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0099
_diffrn_reflns_av_unetI/netI     0.0150
_diffrn_reflns_Laue_measured_fraction_full 0.713
_diffrn_reflns_Laue_measured_fraction_max 0.547
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6851
_diffrn_reflns_point_group_measured_fraction_full 0.713
_diffrn_reflns_point_group_measured_fraction_max 0.547
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         32.172
_diffrn_reflns_theta_min         2.099
_diffrn_ambient_temperature      260.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            PILATUS2M
_diffrn_measured_fraction_theta_full 0.713
_diffrn_measured_fraction_theta_max 0.547
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      0.00 360.00   1.00    1.00    --    0.00   0.00   0.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  PILATUS@SNBL
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0667012000
_diffrn_orient_matrix_UB_12      -0.0035051000
_diffrn_orient_matrix_UB_13      -0.0128327000
_diffrn_orient_matrix_UB_21      0.0460908000
_diffrn_orient_matrix_UB_22      0.0514390000
_diffrn_orient_matrix_UB_23      0.0617333000
_diffrn_orient_matrix_UB_31      0.0109253000
_diffrn_orient_matrix_UB_32      -0.0520567000
_diffrn_orient_matrix_UB_33      0.0398870000
_diffrn_radiation_monochromator  'Si (111)'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.78405
_diffrn_source                   
'European Synchrotron Radiation Facility, BM01 beamline'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3340
_reflns_number_total             3518
_reflns_odcompleteness_completeness 63.06
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     29.34
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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    'XT (Sheldrick, 2015)'
_refine_diff_density_max         5.576
_refine_diff_density_min         -0.779
_refine_diff_density_rms         0.220
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     292
_refine_ls_number_reflns         3518
_refine_ls_number_restraints     34
_refine_ls_R_factor_all          0.0640
_refine_ls_R_factor_gt           0.0621
_refine_ls_restrained_S_all      6.496
_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)+(0.1314P)²+3.6368P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1686
_refine_ls_wR_factor_ref         0.1715
_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
 C12_$7-O1 \\sim O1-C11
 with sigma of 0.05
 C17-C13 \\sim C13-C18
 with sigma of 0.02
3. Restrained planarity
 C13, C17, C18, N2, O11
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C17) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
5. Rigid body (RIGU) restrains
 O11, C13, N2, C18, C17
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Me refined with riding coordinates:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C)
6.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C8(H8), C12(H12), C13(H13), C16(H16)
6.c Tetrahedral OH refined with riding coordinates:
 O1(H1), O12(H12A)
6.d Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C15(H15A,H15B,H15C)
6.e Idealised tetrahedral OH refined as rotating group:
 O9(H9)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
C1 C -0.0210(9) 0.1201(8) 0.4966(9) 0.042(2) Uani 1 1 d . . . . .
C2 C 0.2050(8) 0.4862(9) 0.4323(9) 0.044(2) Uani 1 1 d . . . . .
C3 C 0.3574(8) 0.4946(9) 0.4664(9) 0.044(2) Uani 1 1 d . . . . .
C4 C -0.0367(8) 0.2524(8) 0.4981(9) 0.041(2) Uani 1 1 d . . . . .
C5 C 0.4533(9) 0.5402(11) 0.5932(10) 0.056(3) Uani 1 1 d . . . . .
H5 H 0.422271 0.567235 0.654771 0.067 Uiso 1 1 calc R . . . .
C6 C 0.5946(9) 0.5454(12) 0.6281(9) 0.055(3) Uani 1 1 d . . . . .
C7 C 0.3027(8) 0.7596(8) 0.8600(9) 0.040(2) Uani 1 1 d . . . . .
C8 C 0.0018(11) 0.0731(10) 0.6074(9) 0.049(3) Uani 1 1 d . . . . .
H8 H 0.002086 0.121935 0.678727 0.059 Uiso 1 1 calc R . . . .
C9 C 0.0241(10) -0.0454(9) 0.6136(9) 0.044(2) Uani 1 1 d . . . . .
C10 C 0.0501(18) 0.1781(15) 0.9907(17) 0.083(4) Uani 1 1 d . . . . .
H10A H 0.014475 0.177563 1.056105 0.125 Uiso 1 1 calc GR . . . .
H10B H 0.149168 0.188760 1.027967 0.125 Uiso 1 1 calc GR . . . .
H10C H 0.006462 0.100312 0.929713 0.125 Uiso 1 1 calc GR . . . .
C11 C 0.4024(8) 0.8852(9) 0.9315(9) 0.047(2) Uani 1 1 d D . . . .
C12 C 0.3626(10) 0.9675(11) 0.9911(12) 0.060(3) Uani 1 1 d D . . . .
H12 H 0.272178 0.947740 0.987855 0.072 Uiso 1 1 calc R . . A 2
C13 C 0.3112(13) 0.3304(12) 0.7190(13) 0.081(4) Uani 1 1 d D U . . .
H13 H 0.243957 0.283664 0.641144 0.098 Uiso 1 1 calc R . . . .
C14 C 0.5437(10) 0.9109(11) 0.9376(12) 0.065(4) Uani 1 1 d . . . . .
C15 C -0.1256(14) 0.2803(18) 0.8613(17) 0.091(5) Uani 1 1 d . . . . .
H15A H -0.165304 0.296080 0.922345 0.136 Uiso 1 1 calc GR . . . .
H15B H -0.176866 0.200525 0.805402 0.136 Uiso 1 1 calc GR . . . .
H15C H -0.130458 0.344466 0.812550 0.136 Uiso 1 1 calc GR . . . .
C16 C 0.1177(13) 0.3703(15) 0.9312(13) 0.065(4) Uani 1 1 d . . . . .
H16 H 0.209428 0.368607 0.975966 0.079 Uiso 1 1 calc R . . . .
C17 C 0.436(3) 0.180(2) 0.696(3) 0.159(9) Uani 1 1 d D U . . .
H17A H 0.523805 0.163150 0.743095 0.239 Uiso 1 1 calc R . . . .
H17B H 0.361188 0.109986 0.684883 0.239 Uiso 1 1 calc R . . . .
H17C H 0.432896 0.193738 0.614734 0.239 Uiso 1 1 calc R . . . .
C18 C 0.534(2) 0.364(2) 0.888(2) 0.139(9) Uani 1 1 d D U . . .
H18A H 0.608637 0.323603 0.910612 0.208 Uiso 1 1 calc R . . . .
H18B H 0.567865 0.447015 0.879708 0.208 Uiso 1 1 calc R . . . .
H18C H 0.497875 0.366610 0.953314 0.208 Uiso 1 1 calc R . . . .
N1 N 0.0203(10) 0.2800(10) 0.9278(9) 0.061(3) Uani 1 1 d . . . . .
N2 N 0.4234(13) 0.2933(14) 0.7681(15) 0.097(4) Uani 1 1 d . U . . .
O1 O 0.5948(9) 0.8217(10) 0.8830(13) 0.107(5) Uani 1 1 d D . . . .
H1 H 0.530160 0.760452 0.839926 0.160 Uiso 1 1 calc R . . . .
O2 O -0.0098(7) 0.3205(6) 0.6046(7) 0.0446(16) Uani 1 1 d . . . . .
O3 O 0.1621(6) 0.5062(7) 0.5199(7) 0.0508(18) Uani 1 1 d . . . . .
O4 O -0.0719(7) 0.2860(6) 0.3924(6) 0.0468(17) Uani 1 1 d . . . . .
O5 O 0.0979(9) 0.4621(9) 0.8777(8) 0.065(2) Uani 1 1 d . . . . .
O6 O 0.1221(6) 0.4582(7) 0.3151(6) 0.0489(17) Uani 1 1 d . . . . .
O7 O 0.1858(6) 0.7294(6) 0.8682(6) 0.0464(16) Uani 1 1 d . . . . .
O8 O 0.3387(6) 0.6852(7) 0.7916(7) 0.057(2) Uani 1 1 d . . . . .
O9 O 0.0447(11) -0.0806(8) 0.7264(8) 0.070(2) Uani 1 1 d . . . . .
H9 H 0.047531 -0.153864 0.719054 0.105 Uiso 1 1 calc GR . . . .
O11 O 0.2870(8) 0.4225(8) 0.7675(9) 0.069(2) Uani 1 1 d . U . . .
O12 O 0.6833(7) 0.5871(11) 0.7540(7) 0.081(3) Uani 1 1 d . . . . .
H12A H 0.762730 0.585560 0.762395 0.122 Uiso 1 1 calc R . . . .
Tb1 Tb 0.10848(3) 0.53489(3) 0.69849(3) 0.0356(2) 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
C1 C4 1.518(13) . ?
C1 C8 1.397(16) . ?
C1 C9 1.421(12) 2_556 ?
C2 C3 1.506(10) . ?
C2 O3 1.265(11) . ?
C2 O6 1.275(12) . ?
C3 C5 1.404(13) . ?
C3 C6 1.424(13) 2_666 ?
C4 O2 1.267(10) . ?
C4 O4 1.265(13) . ?
C5 H5 0.9300 . ?
C5 C6 1.397(12) . ?
C6 O12 1.374(12) . ?
C7 C11 1.507(11) . ?
C7 O7 1.266(11) . ?
C7 O8 1.284(10) . ?
C8 H8 0.9300 . ?
C8 C9 1.395(15) . ?
C9 O9 1.358(14) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C10 N1 1.45(2) . ?
C11 C12 1.310(13) . ?
C11 C14 1.449(12) . ?
C12 H12 0.9300 . ?
C12 C14 1.455(13) 2_677 ?
C13 H13 0.9300 . ?
C13 N2 1.297(18) . ?
C13 O11 1.230(15) . ?
C14 O1 1.414(12) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C15 N1 1.464(17) . ?
C16 H16 0.9300 . ?
C16 N1 1.280(18) . ?
C16 O5 1.273(18) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C17 N2 1.49(2) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C18 N2 1.45(2) . ?
O1 H1 0.8200 . ?
O2 Tb1 2.384(6) . ?
O3 Tb1 2.333(7) . ?
O4 Tb1 2.400(7) 2_566 ?
O5 Tb1 2.341(10) . ?
O6 Tb1 2.422(6) 2_566 ?
O7 Tb1 2.516(6) . ?
O8 Tb1 2.451(6) . ?
O9 H9 0.8200 . ?
O11 Tb1 2.432(8) . ?
O12 H12A 0.8200 . ?

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
C8 C1 C4 119.1(8) . . ?
C8 C1 C9 119.6(9) . 2_556 ?
C9 C1 C4 121.3(9) 2_556 . ?
O3 C2 C3 119.5(8) . . ?
O3 C2 O6 121.7(7) . . ?
O6 C2 C3 118.8(8) . . ?
C5 C3 C2 119.8(8) . . ?
C5 C3 C6 119.4(7) . 2_666 ?
C6 C3 C2 120.8(8) 2_666 . ?
O2 C4 C1 117.7(9) . . ?
O4 C4 C1 116.6(8) . . ?
O4 C4 O2 125.7(9) . . ?
C3 C5 H5 119.5 . . ?
C6 C5 C3 121.0(8) . . ?
C6 C5 H5 119.5 . . ?
C5 C6 C3 119.6(8) . 2_666 ?
O12 C6 C3 121.7(8) . 2_666 ?
O12 C6 C5 118.7(8) . . ?
O7 C7 C11 119.7(7) . . ?
O7 C7 O8 121.3(7) . . ?
O8 C7 C11 119.0(8) . . ?
C1 C8 H8 119.2 . . ?
C9 C8 C1 121.6(8) . . ?
C9 C8 H8 119.2 . . ?
C8 C9 C1 118.8(9) . 2_556 ?
O9 C9 C1 125.2(9) . 2_556 ?
O9 C9 C8 116.0(8) . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N1 C10 H10A 109.5 . . ?
N1 C10 H10B 109.5 . . ?
N1 C10 H10C 109.5 . . ?
C12 C11 C7 120.0(8) . . ?
C12 C11 C14 120.9(8) . . ?
C14 C11 C7 119.1(8) . . ?
C11 C12 H12 119.2 . . ?
C11 C12 C14 121.6(8) . 2_677 ?
C14 C12 H12 119.2 2_677 . ?
N2 C13 H13 117.5 . . ?
O11 C13 H13 117.5 . . ?
O11 C13 N2 125.0(13) . . ?
C11 C14 C12 117.5(8) . 2_677 ?
O1 C14 C11 123.0(8) . . ?
O1 C14 C12 119.4(8) . 2_677 ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N1 C15 H15A 109.5 . . ?
N1 C15 H15B 109.5 . . ?
N1 C15 H15C 109.5 . . ?
N1 C16 H16 117.7 . . ?
O5 C16 H16 117.7 . . ?
O5 C16 N1 124.6(13) . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N2 C17 H17A 109.5 . . ?
N2 C17 H17B 109.5 . . ?
N2 C17 H17C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N2 C18 H18A 109.5 . . ?
N2 C18 H18B 109.5 . . ?
N2 C18 H18C 109.5 . . ?
C10 N1 C15 118.5(12) . . ?
C16 N1 C10 121.8(13) . . ?
C16 N1 C15 119.7(14) . . ?
C13 N2 C17 118.1(15) . . ?
C13 N2 C18 120.2(15) . . ?
C18 N2 C17 121.6(17) . . ?
C14 O1 H1 109.5 . . ?
C4 O2 Tb1 133.1(6) . . ?
C2 O3 Tb1 172.4(7) . . ?
C4 O4 Tb1 141.4(6) . 2_566 ?
C16 O5 Tb1 139.8(8) . . ?
C2 O6 Tb1 108.3(5) . 2_566 ?
C7 O7 Tb1 91.3(5) . . ?
C7 O8 Tb1 93.8(5) . . ?
C9 O9 H9 109.5 . . ?
C13 O11 Tb1 135.1(9) . . ?
C6 O12 H12A 109.5 . . ?
O2 Tb1 O4 127.9(2) . 2_566 ?
O2 Tb1 O6 81.5(2) . 2_566 ?
O2 Tb1 O7 153.4(2) . . ?
O2 Tb1 O8 143.6(2) . . ?
O2 Tb1 O11 74.9(3) . . ?
O3 Tb1 O2 78.3(2) . . ?
O3 Tb1 O4 75.3(2) . 2_566 ?
O3 Tb1 O5 147.6(3) . . ?
O3 Tb1 O6 122.8(2) . 2_566 ?
O3 Tb1 O7 128.3(2) . . ?
O3 Tb1 O8 83.2(2) . . ?
O3 Tb1 O11 78.9(3) . . ?
O4 Tb1 O6 76.6(3) 2_566 2_566 ?
O4 Tb1 O7 68.6(2) 2_566 . ?
O4 Tb1 O8 75.6(3) 2_566 . ?
O4 Tb1 O11 139.7(3) 2_566 . ?
O5 Tb1 O2 79.9(3) . . ?
O5 Tb1 O4 137.0(3) . 2_566 ?
O5 Tb1 O6 76.8(3) . 2_566 ?
O5 Tb1 O7 75.4(3) . . ?
O5 Tb1 O8 101.0(3) . . ?
O5 Tb1 O11 72.4(3) . . ?
O6 Tb1 O7 83.4(2) 2_566 . ?
O6 Tb1 O8 134.5(2) 2_566 . ?
O6 Tb1 O11 143.8(3) 2_566 . ?
O8 Tb1 O7 53.1(2) . . ?
O11 Tb1 O7 106.3(3) . . ?
O11 Tb1 O8 71.0(3) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O1 H1 O8 0.82 1.89 2.600(10) 144.7 . yes
O9 H9 O4 0.82 1.96 2.651(10) 141.5 2_556 yes
O12 H12A O6 0.82 1.86 2.591(9) 147.0 2_666 yes

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
C1 C4 O2 Tb1 139.0(7) . . . . ?
C1 C4 O4 Tb1 -175.4(6) . . . 2_566 ?
C1 C8 C9 C1 -1.1(16) . . . 2_556 ?
C1 C8 C9 O9 -179.9(10) . . . . ?
C2 C3 C5 C6 178.1(11) . . . . ?
C3 C2 O6 Tb1 -177.1(7) . . . 2_566 ?
C3 C5 C6 C3 1(2) . . . 2_666 ?
C3 C5 C6 O12 -177.9(12) . . . . ?
C4 C1 C8 C9 -176.7(9) . . . . ?
C6 C3 C5 C6 -1(2) 2_666 . . . ?
C7 C11 C12 C14 179.2(12) . . . 2_677 ?
C7 C11 C14 C12 -179.2(12) . . . 2_677 ?
C7 C11 C14 O1 -2(2) . . . . ?
C8 C1 C4 O2 9.3(12) . . . . ?
C8 C1 C4 O4 -172.7(8) . . . . ?
C9 C1 C4 O2 -168.4(8) 2_556 . . . ?
C9 C1 C4 O4 9.6(12) 2_556 . . . ?
C9 C1 C8 C9 1.1(17) 2_556 . . . ?
C11 C7 O7 Tb1 172.5(9) . . . . ?
C11 C7 O8 Tb1 -172.3(8) . . . . ?
C12 C11 C14 C12 -2(2) . . . 2_677 ?
C12 C11 C14 O1 175.1(14) . . . . ?
C14 C11 C12 C14 2(2) . . . 2_677 ?
N1 C16 O5 Tb1 -104.0(15) . . . . ?
N2 C13 O11 Tb1 171.6(10) . . . . ?
O2 C4 O4 Tb1 2.4(15) . . . 2_566 ?
O3 C2 C3 C5 -8.4(16) . . . . ?
O3 C2 C3 C6 170.5(11) . . . 2_666 ?
O3 C2 O6 Tb1 3.4(12) . . . 2_566 ?
O4 C4 O2 Tb1 -38.8(13) . . . . ?
O5 C16 N1 C10 179.9(12) . . . . ?
O5 C16 N1 C15 -2(2) . . . . ?
O6 C2 C3 C5 172.1(11) . . . . ?
O6 C2 C3 C6 -9.0(16) . . . 2_666 ?
O7 C7 C11 C12 -7.0(17) . . . . ?
O7 C7 C11 C14 170.3(11) . . . . ?
O7 C7 O8 Tb1 7.7(11) . . . . ?
O8 C7 C11 C12 173.0(12) . . . . ?
O8 C7 C11 C14 -9.7(16) . . . . ?
O8 C7 O7 Tb1 -7.5(10) . . . . ?
O11 C13 N2 C17 -179.6(11) . . . . ?
O11 C13 N2 C18 -1.3(19) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.500 0.000 0.500 213.7 0.0 ?


_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 1.224
_oxdiff_exptl_absorpt_empirical_full_min 0.761

# start Validation Reply Form
_vrf_PLAT027_SION2_260K_cool     
;
PROBLEM: _diffrn_reflns_theta_full value (too) Low ......      26.00 Degree
RESPONSE: Our value of max sin(theta)/lambda of 0.56 is close to the recommended 
		  value of 0.60. Higer values of sin(theta)/lambda were not available due 
		  to the beamline experimental set-up limitations.
;
_vrf_PLAT029_SION2_260K_cool     
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.713 Why?  
RESPONSE: The data were collected upon the spindle rotation. Therefore, a 
		  limited portion of the reciprocal space could be probed.
;
# end Validation Reply Form
