# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 2018

####################################################################### 
# 
# 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_R1
_database_code_depnum_ccdc_archive 'CCDC 1564392'
_audit_update_record             
;
2017-07-25 deposited with the CCDC.
2018-02-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C224 H112 N16 O16 Tb'
_chemical_formula_weight         3442.21

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -9.1472 9.1891 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           79
_space_group_name_H-M_alt        'I 4'
_space_group_name_Hall           'I 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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'

_cell_length_a                   21.5284(5)
_cell_length_b                   21.5284(5)
_cell_length_c                   22.3817(14)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10373.3(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    153(2)
_cell_measurement_reflns_used    837
_cell_measurement_theta_min      2.9061
_cell_measurement_theta_max      67.8720

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.102
_exptl_crystal_F_000             3522
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_exptl_absorpt_coefficient_mu    2.170
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.21699
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      153(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'Enhance (Cu) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.2141
_diffrn_reflns_number            7511
_diffrn_reflns_av_unetI/netI     0.3629
_diffrn_reflns_av_R_equivalents  0.1319
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_theta_min         4.905
_diffrn_reflns_theta_max         62.888
_diffrn_reflns_theta_full        62.888
_diffrn_measured_fraction_theta_max 0.866
_diffrn_measured_fraction_theta_full 0.866
_diffrn_reflns_Laue_measured_fraction_max 0.866
_diffrn_reflns_Laue_measured_fraction_full 0.866
_diffrn_reflns_point_group_measured_fraction_max 0.865
_diffrn_reflns_point_group_measured_fraction_full 0.865
_reflns_number_total             4347
_reflns_number_gt                942
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.943
_reflns_Friedel_fraction_max     0.865
_reflns_Friedel_fraction_full    0.865

_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.
;

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component perfect inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           fullcycle
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1283P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as a perfect inversion twin.
;
_refine_ls_abs_structure_Flack   0.5
_chemical_absolute_configuration ?
_refine_ls_number_reflns         4347
_refine_ls_number_parameters     556
_refine_ls_number_restraints     1718
_refine_ls_R_factor_all          0.2408
_refine_ls_R_factor_gt           0.1319
_refine_ls_wR_factor_ref         0.3364
_refine_ls_wR_factor_gt          0.2762
_refine_ls_goodness_of_fit_ref   0.757
_refine_ls_restrained_S_all      0.660
_refine_ls_shift/su_max          0.069
_refine_ls_shift/su_mean         0.012

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 0.8889(12) -0.0783(13) 0.0545(18) 0.082(5) Uani 1 1 d . U . . .
C2 C 0.8208(6) -0.0735(8) 0.0536(10) 0.084(4) Uani 1 1 d G U . . .
C3 C 0.7741(9) -0.1181(6) 0.0528(10) 0.090(4) Uani 1 1 d G U . . .
H3 H 0.7845 -0.1610 0.0536 0.108 Uiso 1 1 calc R U . . .
C4 C 0.7121(8) -0.1000(7) 0.0509(11) 0.094(4) Uani 1 1 d G U . . .
C5 C 0.6969(6) -0.0372(9) 0.0497(11) 0.092(4) Uani 1 1 d G U . . .
C6 C 0.7436(8) 0.0074(6) 0.0505(10) 0.093(4) Uani 1 1 d G U . . .
H6 H 0.7332 0.0502 0.0497 0.111 Uiso 1 1 calc R U . . .
C7 C 0.8055(7) -0.0108(7) 0.0525(10) 0.086(4) Uani 1 1 d G U . . .
C8 C 0.8629(13) 0.0158(13) 0.0492(16) 0.089(5) Uani 1 1 d . U . . .
C9 C 0.5588(15) -0.1077(14) 0.0880(17) 0.100(4) Uani 1 1 d . U . . .
C10 C 0.6172(14) -0.1373(14) 0.0992(18) 0.100(4) Uani 1 1 d . U . . .
C11 C 0.6327(14) -0.1494(13) 0.1605(17) 0.098(5) Uani 1 1 d . U . . .
H11 H 0.6735 -0.1631 0.1698 0.118 Uiso 1 1 calc R U . . .
C12 C 0.5917(13) -0.1421(13) 0.2054(18) 0.101(5) Uani 1 1 d . U . . .
H12 H 0.6004 -0.1556 0.2449 0.121 Uiso 1 1 calc R U . . .
C13 C 0.5348(14) -0.1131(14) 0.190(2) 0.103(5) Uani 1 1 d . U . . .
C14 C 0.5161(13) -0.1009(12) 0.129(2) 0.102(4) Uani 1 1 d . U . . .
C15 C 0.4607(12) -0.0697(11) 0.130(2) 0.104(4) Uani 1 1 d . U . . .
H15 H 0.4498 -0.0571 0.0907 0.125 Uiso 1 1 calc R U . . .
C16 C 0.4194(13) -0.0521(12) 0.1663(15) 0.099(5) Uani 1 1 d . U . . .
H16 H 0.3814 -0.0323 0.1563 0.118 Uiso 1 1 calc R U . . .
C17 C 0.4399(14) -0.0672(13) 0.2239(17) 0.106(5) Uani 1 1 d . U . . .
H17 H 0.4143 -0.0561 0.2568 0.127 Uiso 1 1 calc R U . . .
C18 C 0.4979(13) -0.0987(13) 0.2359(18) 0.104(5) Uani 1 1 d . U . . .
H18 H 0.5094 -0.1090 0.2756 0.124 Uiso 1 1 calc R U . . .
N2 N 0.9142(11) -0.1330(11) 0.0556(12) 0.092(5) Uani 1 1 d . U . . .
C19 C 0.5558(14) -0.0877(15) 0.0232(18) 0.105(4) Uani 1 1 d . U . . .
C20 C 0.5976(14) -0.0423(14) 0.0041(17) 0.104(4) Uani 1 1 d . U . . .
C21 C 0.6026(14) -0.0221(13) -0.0568(18) 0.104(5) Uani 1 1 d . U . . .
H21 H 0.6337 0.0069 -0.0681 0.124 Uiso 1 1 calc R U . . .
C22 C 0.5648(14) -0.0437(14) -0.0961(16) 0.112(5) Uani 1 1 d . U . . .
H22 H 0.5701 -0.0297 -0.1360 0.134 Uiso 1 1 calc R U . . .
C23 C 0.5179(15) -0.0845(15) -0.0859(19) 0.110(5) Uani 1 1 d . U . . .
C24 C 0.5142(14) -0.1111(15) -0.0283(19) 0.108(4) Uani 1 1 d . U . . .
C25 C 0.4795(14) -0.1637(14) -0.0067(17) 0.110(5) Uani 1 1 d . U . . .
H25 H 0.4898 -0.1832 0.0300 0.131 Uiso 1 1 calc R U . . .
C26 C 0.4339(14) -0.1835(14) -0.0390(18) 0.112(6) Uani 1 1 d . U . . .
H26 H 0.4041 -0.2128 -0.0253 0.134 Uiso 1 1 calc R U . . .
C27 C 0.4329(14) -0.1580(15) -0.0949(17) 0.114(6) Uani 1 1 d . U . . .
H27 H 0.3997 -0.1704 -0.1202 0.137 Uiso 1 1 calc R U . . .
C28 C 0.4758(13) -0.1150(14) -0.1193(18) 0.111(5) Uani 1 1 d . U . . .
H28 H 0.4749 -0.1075 -0.1612 0.133 Uiso 1 1 calc R U . . .
C29 C 1.0376(11) 0.1359(13) 0.1922(17) 0.094(5) Uani 1 1 d D U . . .
C30 C 1.0828(7) 0.1766(9) 0.2059(10) 0.090(5) Uani 1 1 d G U . . .
C31 C 1.0886(7) 0.2407(8) 0.2108(9) 0.095(5) Uani 1 1 d G U . . .
H31 H 1.0525 0.2660 0.2125 0.114 Uiso 1 1 calc R U . . .
C32 C 1.1471(9) 0.2677(6) 0.2133(9) 0.099(4) Uani 1 1 d G U . . .
C33 C 1.1999(7) 0.2307(9) 0.2108(10) 0.105(4) Uani 1 1 d G U . . .
C34 C 1.1942(7) 0.1666(8) 0.2059(10) 0.095(4) Uani 1 1 d G U . . .
H34 H 1.2303 0.1412 0.2043 0.114 Uiso 1 1 calc R U . . .
C35 C 1.1356(9) 0.1395(6) 0.2035(10) 0.095(5) Uani 1 1 d G U . . .
C36 C 1.1190(12) 0.0784(12) 0.1960(19) 0.089(5) Uani 1 1 d D U . . .
C37 C 1.2663(14) 0.3666(15) 0.192(2) 0.108(4) Uani 1 1 d . U . . .
C38 C 1.2679(14) 0.3104(15) 0.1667(18) 0.107(4) Uani 1 1 d . U . . .
C39 C 1.2881(12) 0.2926(13) 0.1080(18) 0.112(5) Uani 1 1 d . U . . .
H39 H 1.2893 0.2503 0.0958 0.134 Uiso 1 1 calc R U . . .
C40 C 1.3058(13) 0.3399(14) 0.0703(17) 0.109(5) Uani 1 1 d . U . . .
H40 H 1.3223 0.3322 0.0316 0.131 Uiso 1 1 calc R U . . .
C41 C 1.2982(14) 0.3978(15) 0.0918(19) 0.112(5) Uani 1 1 d . U . . .
C42 C 1.2813(13) 0.4156(14) 0.1482(19) 0.109(4) Uani 1 1 d . U . . .
C43 C 1.2720(13) 0.4791(13) 0.1704(18) 0.113(4) Uani 1 1 d . U . . .
H43 H 1.2539 0.4873 0.2083 0.136 Uiso 1 1 calc R U . . .
C44 C 1.2918(12) 0.5269(13) 0.132(2) 0.117(5) Uani 1 1 d . U . . .
H44 H 1.2944 0.5685 0.1460 0.140 Uiso 1 1 calc R U . . .
C45 C 1.3084(14) 0.5122(14) 0.0696(18) 0.116(6) Uani 1 1 d . U . . .
H45 H 1.3154 0.5431 0.0400 0.139 Uiso 1 1 calc R U . . .
C46 C 1.3126(13) 0.4517(14) 0.0585(18) 0.114(5) Uani 1 1 d . U . . .
H46 H 1.3288 0.4428 0.0200 0.136 Uiso 1 1 calc R U . . .
N1 N 0.9116(10) -0.0174(10) 0.0663(10) 0.082(4) Uani 1 1 d . U . . .
C47 C 1.2529(16) 0.3742(14) 0.251(2) 0.110(4) Uani 1 1 d . U . . .
C48 C 1.1940(15) 0.3547(14) 0.2643(19) 0.108(4) Uani 1 1 d . U . . .
C49 C 1.1684(15) 0.3564(13) 0.3209(18) 0.111(5) Uani 1 1 d . U . . .
H49 H 1.1280 0.3401 0.3276 0.133 Uiso 1 1 calc R U . . .
C50 C 1.2003(15) 0.3808(13) 0.3659(19) 0.115(5) Uani 1 1 d . U . . .
H50 H 1.1824 0.3852 0.4044 0.138 Uiso 1 1 calc R U . . .
C51 C 1.2630(15) 0.4005(14) 0.354(2) 0.115(5) Uani 1 1 d . U . . .
C52 C 1.2808(15) 0.4038(14) 0.296(2) 0.112(4) Uani 1 1 d . U . . .
C53 C 1.3487(15) 0.4233(12) 0.2914(18) 0.119(5) Uani 1 1 d . U . . .
H53 H 1.3662 0.4201 0.2526 0.142 Uiso 1 1 calc R U . . .
C54 C 1.3886(16) 0.4449(12) 0.3345(17) 0.116(6) Uani 1 1 d . U . . .
H54 H 1.4313 0.4548 0.3292 0.140 Uiso 1 1 calc R U . . .
C55 C 1.3543(15) 0.4497(13) 0.3883(18) 0.117(6) Uani 1 1 d . U . . .
H55 H 1.3765 0.4696 0.4196 0.141 Uiso 1 1 calc R U . . .
C56 C 1.2900(14) 0.4297(13) 0.4064(18) 0.118(5) Uani 1 1 d . U . . .
H56 H 1.2710 0.4351 0.4443 0.142 Uiso 1 1 calc R U . . .
N3 N 1.0485(10) 0.0727(10) 0.1888(11) 0.088(5) Uani 1 1 d . U . . .
N4 N 1.1529(11) 0.0316(12) 0.1943(12) 0.095(5) Uani 1 1 d . U . . .
O1 O 0.6643(7) -0.1415(7) 0.0566(13) 0.112(7) Uani 1 1 d . . . . .
O2 O 0.6342(7) -0.0149(8) 0.0449(9) 0.089(6) Uani 1 1 d . . . . .
O3 O 1.2601(8) 0.2580(9) 0.2018(9) 0.097(6) Uani 1 1 d . U . . .
O4 O 1.1525(7) 0.3312(8) 0.2189(13) 0.123(9) Uani 1 1 d . . . . .
Tb1 Tb 1.0000 0.0000 0.1247(3) 0.1005(15) Uani 1 4 d S T P . .


_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 N2 1.30(3) . ?
C1 N1 1.42(3) . ?
C1 C2 1.47(3) . ?
C2 C3 1.3900 . ?
C2 C7 1.3900 . ?
C3 C4 1.3900 . ?
C4 O1 1.369(19) . ?
C4 C5 1.3900 . ?
C5 C6 1.3900 . ?
C5 O2 1.438(19) . ?
C6 C7 1.3900 . ?
C7 C8 1.36(3) . ?
C8 N1 1.33(3) . ?
C8 N2 1.52(3) 4_665 ?
C9 C14 1.31(4) . ?
C9 C10 1.43(4) . ?
C9 C19 1.51(4) . ?
C10 O1 1.40(4) . ?
C10 C11 1.44(3) . ?
C11 C12 1.35(4) . ?
C12 C13 1.41(4) . ?
C13 C18 1.33(4) . ?
C13 C14 1.45(6) . ?
C14 C15 1.37(3) . ?
C15 C16 1.26(4) . ?
C16 C17 1.40(4) . ?
C17 C18 1.45(3) . ?
N2 C8 1.52(3) 3_645 ?
C19 C20 1.40(4) . ?
C19 C24 1.54(4) . ?
C20 O2 1.34(3) . ?
C20 C21 1.44(4) . ?
C21 C22 1.29(4) . ?
C22 C23 1.36(4) . ?
C23 C28 1.35(4) . ?
C23 C24 1.41(4) . ?
C24 C25 1.44(4) . ?
C25 C26 1.29(4) . ?
C26 C27 1.37(4) . ?
C27 C28 1.42(4) . ?
C29 C30 1.34(3) . ?
C29 N3 1.38(3) . ?
C29 N4 1.53(3) 3_645 ?
C30 C31 1.3900 . ?
C30 C35 1.3900 . ?
C31 C32 1.3900 . ?
C32 O4 1.38(2) . ?
C32 C33 1.3900 . ?
C33 C34 1.3900 . ?
C33 O3 1.44(2) . ?
C34 C35 1.3900 . ?
C35 C36 1.37(3) . ?
C36 N4 1.24(3) . ?
C36 N3 1.53(3) . ?
C37 C38 1.33(4) . ?
C37 C47 1.37(5) . ?
C37 C42 1.47(4) . ?
C38 O3 1.38(3) . ?
C38 C39 1.44(4) . ?
C39 C40 1.38(4) . ?
C40 C41 1.35(4) . ?
C41 C42 1.37(4) . ?
C41 C46 1.41(4) . ?
C42 C43 1.47(4) . ?
C43 C44 1.41(4) . ?
C44 C45 1.47(5) . ?
C45 C46 1.33(3) . ?
N1 Tb1 2.34(2) . ?
C47 C52 1.33(4) . ?
C47 C48 1.37(4) . ?
C48 C49 1.38(4) . ?
C48 O4 1.45(4) . ?
C49 C50 1.33(4) . ?
C50 C51 1.44(4) . ?
C51 C52 1.37(5) . ?
C51 C56 1.45(4) . ?
C52 C53 1.52(4) . ?
C53 C54 1.37(4) . ?
C54 C55 1.42(4) . ?
C55 C56 1.50(4) . ?
N3 Tb1 2.37(2) . ?
N4 C29 1.54(3) 4_665 ?
Tb1 N1 2.34(2) 3_645 ?
Tb1 N1 2.34(2) 2_755 ?
Tb1 N1 2.34(2) 4_665 ?
Tb1 N3 2.37(2) 4_665 ?
Tb1 N3 2.37(2) 3_645 ?
Tb1 N3 2.37(2) 2_755 ?

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
N2 C1 N1 133(3) . . ?
N2 C1 C2 119(2) . . ?
N1 C1 C2 106(2) . . ?
C3 C2 C7 120.0 . . ?
C3 C2 C1 132.3(16) . . ?
C7 C2 C1 107.7(16) . . ?
C2 C3 C4 120.0 . . ?
O1 C4 C5 117.3(15) . . ?
O1 C4 C3 122.3(15) . . ?
C5 C4 C3 120.0 . . ?
C6 C5 C4 120.0 . . ?
C6 C5 O2 116.7(15) . . ?
C4 C5 O2 123.2(15) . . ?
C7 C6 C5 120.0 . . ?
C8 C7 C6 138.6(17) . . ?
C8 C7 C2 101.2(17) . . ?
C6 C7 C2 120.0 . . ?
N1 C8 C7 118(3) . . ?
N1 C8 N2 118(3) . 4_665 ?
C7 C8 N2 118(2) . 4_665 ?
C14 C9 C10 123(4) . . ?
C14 C9 C19 128(3) . . ?
C10 C9 C19 109(3) . . ?
O1 C10 C9 123(4) . . ?
O1 C10 C11 118(3) . . ?
C9 C10 C11 117(3) . . ?
C12 C11 C10 123(3) . . ?
C11 C12 C13 116(4) . . ?
C18 C13 C12 116(4) . . ?
C18 C13 C14 121(3) . . ?
C12 C13 C14 123(4) . . ?
C9 C14 C15 133(5) . . ?
C9 C14 C13 117(3) . . ?
C15 C14 C13 108(4) . . ?
C16 C15 C14 141(5) . . ?
C15 C16 C17 108(3) . . ?
C16 C17 C18 123(4) . . ?
C13 C18 C17 119(4) . . ?
C1 N2 C8 118(2) . 3_645 ?
C20 C19 C9 118(3) . . ?
C20 C19 C24 112(4) . . ?
C9 C19 C24 130(3) . . ?
O2 C20 C19 119(4) . . ?
O2 C20 C21 118(3) . . ?
C19 C20 C21 123(4) . . ?
C22 C21 C20 120(3) . . ?
C21 C22 C23 126(4) . . ?
C28 C23 C22 136(4) . . ?
C28 C23 C24 106(3) . . ?
C22 C23 C24 117(4) . . ?
C23 C24 C25 131(4) . . ?
C23 C24 C19 121(3) . . ?
C25 C24 C19 108(4) . . ?
C26 C25 C24 118(4) . . ?
C25 C26 C27 113(3) . . ?
C26 C27 C28 127(3) . . ?
C23 C28 C27 123(4) . . ?
C30 C29 N3 122(2) . . ?
C30 C29 N4 123(2) . 3_645 ?
N3 C29 N4 114(2) . 3_645 ?
C29 C30 C31 136.9(18) . . ?
C29 C30 C35 102.0(18) . . ?
C31 C30 C35 120.0 . . ?
C30 C31 C32 120.0 . . ?
O4 C32 C33 120.3(14) . . ?
O4 C32 C31 119.7(14) . . ?
C33 C32 C31 120.0 . . ?
C32 C33 C34 120.0 . . ?
C32 C33 O3 120.5(15) . . ?
C34 C33 O3 118.5(15) . . ?
C33 C34 C35 120.0 . . ?
C34 C35 C30 120.0 . . ?
C34 C35 C36 130.0(17) . . ?
C30 C35 C36 110.0(17) . . ?
N4 C36 C35 129(3) . . ?
N4 C36 N3 121(3) . . ?
C35 C36 N3 110.4(18) . . ?
C38 C37 C47 122(4) . . ?
C38 C37 C42 111(4) . . ?
C47 C37 C42 127(3) . . ?
C37 C38 O3 120(4) . . ?
C37 C38 C39 129(4) . . ?
O3 C38 C39 110(3) . . ?
C40 C39 C38 117(3) . . ?
C41 C40 C39 116(4) . . ?
C40 C41 C42 128(4) . . ?
C40 C41 C46 123(4) . . ?
C42 C41 C46 108(3) . . ?
C41 C42 C37 118(3) . . ?
C41 C42 C43 128(4) . . ?
C37 C42 C43 114(4) . . ?
C44 C43 C42 116(4) . . ?
C43 C44 C45 120(3) . . ?
C46 C45 C44 114(3) . . ?
C45 C46 C41 134(4) . . ?
C8 N1 C1 100(2) . . ?
C8 N1 Tb1 136(2) . . ?
C1 N1 Tb1 122.1(19) . . ?
C52 C47 C48 114(4) . . ?
C52 C47 C37 134(4) . . ?
C48 C47 C37 111(4) . . ?
C47 C48 C49 124(4) . . ?
C47 C48 O4 122(4) . . ?
C49 C48 O4 114(3) . . ?
C50 C49 C48 120(3) . . ?
C49 C50 C51 118(4) . . ?
C52 C51 C50 117(4) . . ?
C52 C51 C56 129(3) . . ?
C50 C51 C56 111(4) . . ?
C47 C52 C51 124(4) . . ?
C47 C52 C53 121(4) . . ?
C51 C52 C53 110(4) . . ?
C54 C53 C52 130(4) . . ?
C53 C54 C55 107(3) . . ?
C54 C55 C56 133(3) . . ?
C51 C56 C55 106(3) . . ?
C29 N3 C36 94.7(16) . . ?
C29 N3 Tb1 127(2) . . ?
C36 N3 Tb1 123.6(18) . . ?
C36 N4 C29 130(3) . 4_665 ?
C4 O1 C10 125(2) . . ?
C20 O2 C5 117(2) . . ?
C38 O3 C33 122(2) . . ?
C32 O4 C48 118(2) . . ?
N1 Tb1 N1 71.8(5) . 3_645 ?
N1 Tb1 N1 112.1(11) . 2_755 ?
N1 Tb1 N1 71.8(5) 3_645 2_755 ?
N1 Tb1 N1 71.8(5) . 4_665 ?
N1 Tb1 N1 112.1(11) 3_645 4_665 ?
N1 Tb1 N1 71.8(5) 2_755 4_665 ?
N1 Tb1 N3 143.7(7) . 4_665 ?
N1 Tb1 N3 82.8(7) 3_645 4_665 ?
N1 Tb1 N3 82.6(8) 2_755 4_665 ?
N1 Tb1 N3 143.5(7) 4_665 4_665 ?
N1 Tb1 N3 82.6(8) . 3_645 ?
N1 Tb1 N3 143.5(7) 3_645 3_645 ?
N1 Tb1 N3 143.7(7) 2_755 3_645 ?
N1 Tb1 N3 82.8(7) 4_665 3_645 ?
N3 Tb1 N3 105.2(12) 4_665 3_645 ?
N1 Tb1 N3 82.8(7) . 2_755 ?
N1 Tb1 N3 82.6(8) 3_645 2_755 ?
N1 Tb1 N3 143.5(7) 2_755 2_755 ?
N1 Tb1 N3 143.7(7) 4_665 2_755 ?
N3 Tb1 N3 68.4(6) 4_665 2_755 ?
N3 Tb1 N3 68.4(6) 3_645 2_755 ?
N1 Tb1 N3 143.5(7) . . ?
N1 Tb1 N3 143.7(7) 3_645 . ?
N1 Tb1 N3 82.8(7) 2_755 . ?
N1 Tb1 N3 82.6(8) 4_665 . ?
N3 Tb1 N3 68.4(6) 4_665 . ?
N3 Tb1 N3 68.4(6) 3_645 . ?
N3 Tb1 N3 105.2(12) 2_755 . ?

_refine_diff_density_max         0.760
_refine_diff_density_min         -0.352
_refine_diff_density_rms         0.072



####################################################################### 
# 
# 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_S1
_database_code_depnum_ccdc_archive 'CCDC 1564394'
_audit_update_record             
;
2017-07-25 deposited with the CCDC.
2018-02-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C228 H120 Cl8 N16 O16 Tb'
_chemical_formula_weight         3781.91

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -9.1472 9.1891 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           79
_space_group_name_H-M_alt        'I 4'
_space_group_name_Hall           'I 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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'

_cell_length_a                   21.5284(5)
_cell_length_b                   21.5284(5)
_cell_length_c                   22.3817(14)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10373.3(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    153(2)
_cell_measurement_reflns_used    3322
_cell_measurement_theta_min      3.9469
_cell_measurement_theta_max      66.7079

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.211
_exptl_crystal_F_000             3858
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_exptl_absorpt_coefficient_mu    3.139
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.84010
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      153(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'Enhance (Cu) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.2141
_diffrn_reflns_number            9281
_diffrn_reflns_av_unetI/netI     0.0937
_diffrn_reflns_av_R_equivalents  0.0407
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.950
_diffrn_reflns_theta_max         66.813
_diffrn_reflns_theta_full        66.813
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measured_fraction_theta_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.632
_diffrn_reflns_point_group_measured_fraction_full 0.632
_reflns_number_total             5824
_reflns_number_gt                5135
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.254
_reflns_Friedel_fraction_max     0.264
_reflns_Friedel_fraction_full    0.264

_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.
;

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           fullcycle
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1575P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 917 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.005(7)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         5824
_refine_ls_number_parameters     592
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0904
_refine_ls_R_factor_gt           0.0826
_refine_ls_wR_factor_ref         0.2305
_refine_ls_wR_factor_gt          0.2208
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_restrained_S_all      1.059
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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 0.0000 1.0000 0.87484(4) 0.0240(3) Uani 1 4 d S T P . .
C2B C 0.1141(4) 1.0783(4) 0.9420(5) 0.022(2) Uani 1 1 d . . . . .
C5 C 0.1363(4) 0.9787(4) 0.9431(5) 0.026(2) Uani 1 1 d . . . . .
C6 C 0.1960(4) 1.0112(4) 0.9482(5) 0.026(2) Uani 1 1 d . . . . .
C8B C 0.2275(4) 1.1200(4) 0.9456(5) 0.026(2) Uani 1 1 d . . . . .
H8B H 0.2177 1.1630 0.9435 0.031 Uiso 1 1 calc R U . . .
C3B C 0.1818(4) 1.0749(4) 0.9465(4) 0.0239(18) Uani 1 1 d . . . . .
N1B N 0.0894(3) 1.0203(3) 0.9378(4) 0.0254(17) Uani 1 1 d . . . . .
C7B C 0.2883(4) 1.0994(4) 0.9478(5) 0.027(2) Uani 1 1 d . . . . .
C7 C 0.2570(4) 0.9917(4) 0.9528(5) 0.029(2) Uani 1 1 d . . . . .
H7 H 0.2667 0.9487 0.9545 0.035 Uiso 1 1 calc R U . . .
N2B N 0.0837(3) 1.1328(3) 0.9431(4) 0.0248(16) Uani 1 1 d . . . . .
N1A N -0.0514(3) 0.9242(3) 0.8117(4) 0.0269(17) Uani 1 1 d . . . . .
C6B C 0.3037(4) 1.0358(4) 0.9547(5) 0.029(2) Uani 1 1 d . . . . .
C4A C -0.1375(4) 0.8598(4) 0.8007(5) 0.028(2) Uani 1 1 d . . . . .
O1B O 0.3630(3) 1.0144(3) 0.9579(3) 0.0300(15) Uani 1 1 d . . . . .
C20B C 0.4803(4) 1.0982(4) 0.8705(7) 0.0324(19) Uani 1 1 d . . . . .
C3A C -0.0833(4) 0.8227(4) 0.7985(5) 0.028(2) Uani 1 1 d . . . . .
C28B C 0.3808(4) 1.1348(4) 0.9010(6) 0.033(2) Uani 1 1 d . . . . .
N2A N -0.1546(3) 0.9719(4) 0.8049(4) 0.0289(18) Uani 1 1 d . . . . .
C17B C 0.4875(4) 1.1138(5) 1.0207(5) 0.035(2) Uani 1 1 d . . . . .
C12B C 0.4870(5) 1.0937(5) 1.0809(6) 0.042(3) Uani 1 1 d . . . . .
C9B C 0.4032(4) 1.0429(4) 0.9995(5) 0.030(2) Uani 1 1 d . . . . .
C8A C -0.0883(4) 0.7589(4) 0.7911(5) 0.030(2) Uani 1 1 d . . . . .
H8A H -0.0523 0.7336 0.7879 0.036 Uiso 1 1 calc R U . . .
C10B C 0.4012(5) 1.0226(5) 1.0582(6) 0.040(3) Uani 1 1 d . . . . .
H10 H 0.3717 0.9922 1.0703 0.048 Uiso 1 1 calc R U . . .
C26B C 0.4089(5) 1.1440(5) 0.7989(5) 0.034(2) Uani 1 1 d . . . . .
H26 H 0.3995 1.1567 0.7592 0.041 Uiso 1 1 calc R U . . .
C25B C 0.4664(5) 1.1150(4) 0.8106(5) 0.034(2) Uani 1 1 d . . . . .
C18B C 0.4436(4) 1.0880(4) 0.9785(5) 0.030(2) Uani 1 1 d . . . . .
C16B C 0.5305(5) 1.1607(6) 1.0026(6) 0.046(3) Uani 1 1 d . . . . .
H16 H 0.5309 1.1752 0.9625 0.055 Uiso 1 1 calc R U . . .
C1A C -0.1159(4) 0.9234(4) 0.8061(5) 0.025(2) Uani 1 1 d . . . . .
C19B C 0.4367(4) 1.1094(4) 0.9160(5) 0.031(2) Uani 1 1 d . . . . .
C11B C 0.4425(5) 1.0470(6) 1.0989(5) 0.042(3) Uani 1 1 d . . . . .
H11 H 0.4417 1.0331 1.1391 0.050 Uiso 1 1 calc R U . . .
C21B C 0.5375(4) 1.0661(4) 0.8811(5) 0.032(2) Uani 1 1 d . . . . .
H21 H 0.5489 1.0556 0.9209 0.039 Uiso 1 1 calc R U . . .
C24B C 0.5084(5) 1.0994(5) 0.7643(6) 0.039(3) Uani 1 1 d . . . . .
H24 H 0.4994 1.1118 0.7245 0.046 Uiso 1 1 calc R U . . .
C22B C 0.5757(5) 1.0503(5) 0.8350(6) 0.043(3) Uani 1 1 d . . . . .
H22 H 0.6127 1.0276 0.8429 0.051 Uiso 1 1 calc R U . . .
C14B C 0.5708(7) 1.1639(7) 1.1032(7) 0.063(4) Uani 1 1 d . . . . .
H14 H 0.5991 1.1807 1.1315 0.076 Uiso 1 1 calc R U . . .
C23B C 0.5611(5) 1.0672(5) 0.7756(6) 0.042(3) Uani 1 1 d . . . . .
H23 H 0.5881 1.0560 0.7438 0.050 Uiso 1 1 calc R U . . .
C13B C 0.5291(6) 1.1191(7) 1.1204(7) 0.055(3) Uani 1 1 d . . . . .
H13 H 0.5292 1.1052 1.1607 0.066 Uiso 1 1 calc R U . . .
C15B C 0.5715(6) 1.1845(6) 1.0440(8) 0.059(4) Uani 1 1 d . . . . .
H15 H 0.6006 1.2153 1.0322 0.070 Uiso 1 1 calc R U . . .
O2B O 0.3354(3) 1.1442(3) 0.9457(4) 0.0315(15) Uani 1 1 d . . . . .
C2A C -0.0311(4) 0.8647(4) 0.8055(5) 0.026(2) Uani 1 1 d . . . . .
C27B C 0.3676(4) 1.1538(5) 0.8418(5) 0.035(2) Uani 1 1 d . . . . .
H27 H 0.3292 1.1734 0.8328 0.042 Uiso 1 1 calc R U . . .
C5A C -0.1952(4) 0.8340(4) 0.7986(5) 0.0257(19) Uani 1 1 d . . . . .
H5A H -0.2313 0.8594 0.7987 0.031 Uiso 1 1 calc R U . . .
C6A C -0.2000(4) 0.7699(4) 0.7963(5) 0.028(2) Uani 1 1 d . . . . .
C7A C -0.1464(4) 0.7334(4) 0.7887(5) 0.027(2) Uani 1 1 d . . . . .
O1A O -0.2592(3) 0.7437(3) 0.7960(3) 0.0280(14) Uani 1 1 d . . . . .
O2A O -0.1514(3) 0.6697(3) 0.7809(4) 0.0328(16) Uani 1 1 d . . . . .
C9A C -0.2707(4) 0.6940(4) 0.8355(5) 0.030(2) Uani 1 1 d . . . . .
C10A C -0.2885(5) 0.7057(5) 0.8940(5) 0.036(2) Uani 1 1 d . . . . .
H10A H -0.2889 0.7471 0.9086 0.043 Uiso 1 1 calc R U . . .
C19A C -0.2473(4) 0.6267(4) 0.7494(5) 0.030(2) Uani 1 1 d . . . . .
C20A C -0.2858(5) 0.6010(4) 0.7027(5) 0.035(2) Uani 1 1 d . . . . .
C28A C -0.1894(4) 0.6484(4) 0.7343(5) 0.030(2) Uani 1 1 d . . . . .
C27A C -0.1670(5) 0.6468(5) 0.6769(5) 0.037(2) Uani 1 1 d . . . . .
H27A H -0.1273 0.6640 0.6684 0.044 Uiso 1 1 calc R U . . .
C18A C -0.2688(4) 0.6332(5) 0.8116(5) 0.029(2) Uani 1 1 d . . . . .
C17A C -0.2841(5) 0.5839(4) 0.8500(6) 0.038(3) Uani 1 1 d . . . . .
C25A C -0.2606(5) 0.5976(5) 0.6438(6) 0.041(3) Uani 1 1 d . . . . .
C11A C -0.3053(5) 0.6583(5) 0.9305(6) 0.042(3) Uani 1 1 d . . . . .
H11A H -0.3181 0.6666 0.9703 0.051 Uiso 1 1 calc R U . . .
C15A C -0.2947(6) 0.4729(5) 0.8695(10) 0.062(4) Uani 1 1 d . . . . .
H15A H -0.2908 0.4310 0.8567 0.074 Uiso 1 1 calc R U . . .
C24A C -0.2977(7) 0.5695(6) 0.5979(6) 0.052(3) Uani 1 1 d . . . . .
H24A H -0.2811 0.5646 0.5589 0.062 Uiso 1 1 calc R U . . .
C26A C -0.2013(6) 0.6205(5) 0.6314(6) 0.043(3) Uani 1 1 d . . . . .
H26A H -0.1848 0.6181 0.5921 0.052 Uiso 1 1 calc R U . . .
C16A C -0.2783(5) 0.5195(5) 0.8313(7) 0.046(3) Uani 1 1 d . . . . .
H16A H -0.2630 0.5099 0.7926 0.056 Uiso 1 1 calc R U . . .
C13A C -0.3203(7) 0.5449(6) 0.9466(7) 0.057(3) Uani 1 1 d . . . . .
H13A H -0.3336 0.5530 0.9863 0.068 Uiso 1 1 calc R U . . .
C12A C -0.3037(5) 0.5947(5) 0.9085(6) 0.042(3) Uani 1 1 d . . . . .
C22A C -0.3814(6) 0.5559(6) 0.6663(8) 0.056(4) Uani 1 1 d . . . . .
H22A H -0.4229 0.5427 0.6734 0.068 Uiso 1 1 calc R U . . .
C21A C -0.3480(5) 0.5805(5) 0.7133(7) 0.045(3) Uani 1 1 d . . . . .
H21A H -0.3660 0.5838 0.7519 0.053 Uiso 1 1 calc R U . . .
C23A C -0.3577(7) 0.5496(6) 0.6100(8) 0.061(4) Uani 1 1 d . . . . .
H23A H -0.3821 0.5315 0.5793 0.074 Uiso 1 1 calc R U . . .
C14A C -0.3171(8) 0.4850(6) 0.9263(8) 0.067(4) Uani 1 1 d . . . . .
H14A H -0.3302 0.4517 0.9512 0.080 Uiso 1 1 calc R U . . .
Cl2A Cl 0.4207(5) 0.2329(5) 0.6452(6) 0.168(3) Uiso 1 1 d . . . . .
Cl1A Cl 0.3271(6) 0.2446(5) 0.5507(6) 0.186(4) Uiso 1 1 d . . . . .
C1Z C 0.3805(14) 0.2810(14) 0.6017(15) 0.133(10) Uiso 1 1 d . . . . .
H1Z1 H 0.4102 0.3063 0.5783 0.159 Uiso 1 1 calc R U . . .
H1Z2 H 0.3568 0.3098 0.6277 0.159 Uiso 1 1 calc R 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
Tb1 N1B 2.425(8) . ?
Tb1 N1B 2.425(8) 3_665 ?
Tb1 N1B 2.425(8) 2_575 ?
Tb1 N1B 2.425(8) 4_465 ?
Tb1 N1A 2.427(8) 4_465 ?
Tb1 N1A 2.427(8) 2_575 ?
Tb1 N1A 2.427(8) 3_665 ?
Tb1 N1A 2.427(8) . ?
C2B N2B 1.342(12) . ?
C2B N1B 1.361(12) . ?
C2B C3B 1.462(12) . ?
C5 N2B 1.345(12) 4_465 ?
C5 N1B 1.357(12) . ?
C5 C6 1.467(13) . ?
C6 C7 1.383(13) . ?
C6 C3B 1.405(12) . ?
C8B C3B 1.383(12) . ?
C8B C7B 1.384(13) . ?
C7B O2B 1.399(11) . ?
C7B C6B 1.417(13) . ?
C7 C6B 1.384(14) . ?
N2B C5 1.345(12) 3_665 ?
N1A C2A 1.359(12) . ?
N1A C1A 1.394(12) . ?
C6B O1B 1.359(11) . ?
C4A C5A 1.362(13) . ?
C4A C3A 1.414(13) . ?
C4A C1A 1.451(13) . ?
O1B C9B 1.413(13) . ?
C20B C19B 1.406(16) . ?
C20B C25B 1.422(19) . ?
C20B C21B 1.431(12) . ?
C3A C8A 1.388(13) . ?
C3A C2A 1.450(13) . ?
C28B C19B 1.364(14) . ?
C28B O2B 1.414(13) . ?
C28B C27B 1.415(16) . ?
N2A C1A 1.335(13) . ?
N2A C2A 1.342(12) 4_465 ?
C17B C12B 1.413(18) . ?
C17B C16B 1.430(15) . ?
C17B C18B 1.447(15) . ?
C12B C13B 1.380(18) . ?
C12B C11B 1.446(16) . ?
C9B C10B 1.385(17) . ?
C9B C18B 1.386(14) . ?
C8A C7A 1.365(14) . ?
C10B C11B 1.376(18) . ?
C26B C27B 1.326(16) . ?
C26B C25B 1.412(15) . ?
C25B C24B 1.415(17) . ?
C18B C19B 1.480(16) . ?
C16B C15B 1.378(18) . ?
C21B C22B 1.365(16) . ?
C24B C23B 1.355(16) . ?
C22B C23B 1.414(18) . ?
C14B C13B 1.37(2) . ?
C14B C15B 1.40(2) . ?
C2A N2A 1.342(12) 3_665 ?
C5A C6A 1.385(13) . ?
C6A O1A 1.394(11) . ?
C6A C7A 1.407(13) . ?
C7A O2A 1.387(11) . ?
O1A C9A 1.409(12) . ?
O2A C28A 1.404(12) . ?
C9A C10A 1.388(16) . ?
C9A C18A 1.415(14) . ?
C10A C11A 1.356(17) . ?
C19A C28A 1.373(14) . ?
C19A C20A 1.445(15) . ?
C19A C18A 1.473(15) . ?
C20A C25A 1.428(17) . ?
C20A C21A 1.428(15) . ?
C28A C27A 1.372(16) . ?
C27A C26A 1.379(17) . ?
C18A C17A 1.405(15) . ?
C17A C12A 1.396(18) . ?
C17A C16A 1.453(15) . ?
C25A C26A 1.396(17) . ?
C25A C24A 1.435(17) . ?
C11A C12A 1.454(17) . ?
C15A C16A 1.37(2) . ?
C15A C14A 1.38(3) . ?
C24A C23A 1.39(2) . ?
C13A C14A 1.37(2) . ?
C13A C12A 1.416(18) . ?
C22A C23A 1.36(2) . ?
C22A C21A 1.381(18) . ?
Cl2A C1Z 1.66(3) . ?
Cl1A C1Z 1.80(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
N1B Tb1 N1B 70.2(2) . 3_665 ?
N1B Tb1 N1B 108.9(4) . 2_575 ?
N1B Tb1 N1B 70.2(2) 3_665 2_575 ?
N1B Tb1 N1B 70.2(2) . 4_465 ?
N1B Tb1 N1B 108.9(4) 3_665 4_465 ?
N1B Tb1 N1B 70.2(2) 2_575 4_465 ?
N1B Tb1 N1A 142.2(2) . 4_465 ?
N1B Tb1 N1A 81.7(3) 3_665 4_465 ?
N1B Tb1 N1A 83.5(3) 2_575 4_465 ?
N1B Tb1 N1A 145.3(2) 4_465 4_465 ?
N1B Tb1 N1A 81.7(3) . 2_575 ?
N1B Tb1 N1A 83.5(3) 3_665 2_575 ?
N1B Tb1 N1A 145.3(2) 2_575 2_575 ?
N1B Tb1 N1A 142.2(2) 4_465 2_575 ?
N1A Tb1 N1A 70.2(2) 4_465 2_575 ?
N1B Tb1 N1A 83.5(3) . 3_665 ?
N1B Tb1 N1A 145.3(2) 3_665 3_665 ?
N1B Tb1 N1A 142.2(2) 2_575 3_665 ?
N1B Tb1 N1A 81.7(3) 4_465 3_665 ?
N1A Tb1 N1A 108.7(4) 4_465 3_665 ?
N1A Tb1 N1A 70.2(2) 2_575 3_665 ?
N1B Tb1 N1A 145.3(2) . . ?
N1B Tb1 N1A 142.2(2) 3_665 . ?
N1B Tb1 N1A 81.7(3) 2_575 . ?
N1B Tb1 N1A 83.5(3) 4_465 . ?
N1A Tb1 N1A 70.2(2) 4_465 . ?
N1A Tb1 N1A 108.7(4) 2_575 . ?
N1A Tb1 N1A 70.2(2) 3_665 . ?
N2B C2B N1B 127.7(8) . . ?
N2B C2B C3B 121.9(8) . . ?
N1B C2B C3B 110.4(8) . . ?
N2B C5 N1B 128.1(9) 4_465 . ?
N2B C5 C6 121.8(8) 4_465 . ?
N1B C5 C6 110.0(8) . . ?
C7 C6 C3B 120.3(8) . . ?
C7 C6 C5 133.7(8) . . ?
C3B C6 C5 105.9(8) . . ?
C3B C8B C7B 116.6(8) . . ?
C8B C3B C6 122.0(8) . . ?
C8B C3B C2B 132.3(8) . . ?
C6 C3B C2B 105.5(8) . . ?
C5 N1B C2B 108.0(8) . . ?
C5 N1B Tb1 121.5(6) . . ?
C2B N1B Tb1 121.0(6) . . ?
C8B C7B O2B 117.5(8) . . ?
C8B C7B C6B 122.4(8) . . ?
O2B C7B C6B 120.1(8) . . ?
C6 C7 C6B 119.0(8) . . ?
C2B N2B C5 122.5(8) . 3_665 ?
C2A N1A C1A 107.5(8) . . ?
C2A N1A Tb1 123.1(6) . . ?
C1A N1A Tb1 120.9(6) . . ?
O1B C6B C7 116.9(8) . . ?
O1B C6B C7B 123.6(8) . . ?
C7 C6B C7B 119.3(8) . . ?
C5A C4A C3A 121.4(9) . . ?
C5A C4A C1A 132.8(9) . . ?
C3A C4A C1A 105.8(8) . . ?
C6B O1B C9B 117.5(8) . . ?
C19B C20B C25B 119.9(9) . . ?
C19B C20B C21B 122.5(12) . . ?
C25B C20B C21B 117.4(11) . . ?
C8A C3A C4A 119.9(9) . . ?
C8A C3A C2A 133.7(9) . . ?
C4A C3A C2A 106.4(8) . . ?
C19B C28B O2B 119.5(11) . . ?
C19B C28B C27B 121.6(10) . . ?
O2B C28B C27B 118.8(8) . . ?
C1A N2A C2A 123.3(8) . 4_465 ?
C12B C17B C16B 119.4(11) . . ?
C12B C17B C18B 120.0(9) . . ?
C16B C17B C18B 120.5(11) . . ?
C13B C12B C17B 119.0(11) . . ?
C13B C12B C11B 122.2(12) . . ?
C17B C12B C11B 118.9(11) . . ?
C10B C9B C18B 124.3(10) . . ?
C10B C9B O1B 118.0(9) . . ?
C18B C9B O1B 117.7(10) . . ?
C7A C8A C3A 118.3(8) . . ?
C11B C10B C9B 119.1(10) . . ?
C27B C26B C25B 121.6(11) . . ?
C26B C25B C24B 121.9(11) . . ?
C26B C25B C20B 118.2(10) . . ?
C24B C25B C20B 119.8(9) . . ?
C9B C18B C17B 117.1(10) . . ?
C9B C18B C19B 118.4(9) . . ?
C17B C18B C19B 124.3(9) . . ?
C15B C16B C17B 119.1(13) . . ?
N2A C1A N1A 127.9(8) . . ?
N2A C1A C4A 122.4(8) . . ?
N1A C1A C4A 109.7(8) . . ?
C28B C19B C20B 118.7(11) . . ?
C28B C19B C18B 116.6(10) . . ?
C20B C19B C18B 124.2(9) . . ?
C10B C11B C12B 120.6(11) . . ?
C22B C21B C20B 120.9(11) . . ?
C23B C24B C25B 121.3(11) . . ?
C21B C22B C23B 120.9(10) . . ?
C13B C14B C15B 119.7(13) . . ?
C24B C23B C22B 119.6(11) . . ?
C14B C13B C12B 122.0(14) . . ?
C16B C15B C14B 120.9(13) . . ?
C7B O2B C28B 115.3(7) . . ?
N2A C2A N1A 126.7(8) 3_665 . ?
N2A C2A C3A 122.8(8) 3_665 . ?
N1A C2A C3A 110.4(8) . . ?
C26B C27B C28B 119.8(9) . . ?
C4A C5A C6A 118.4(8) . . ?
C5A C6A O1A 118.1(8) . . ?
C5A C6A C7A 119.9(8) . . ?
O1A C6A C7A 121.7(8) . . ?
C8A C7A O2A 118.3(8) . . ?
C8A C7A C6A 121.4(8) . . ?
O2A C7A C6A 120.2(8) . . ?
C6A O1A C9A 117.7(7) . . ?
C7A O2A C28A 117.4(8) . . ?
C10A C9A O1A 120.1(8) . . ?
C10A C9A C18A 122.2(10) . . ?
O1A C9A C18A 117.5(9) . . ?
C11A C10A C9A 120.4(10) . . ?
C28A C19A C20A 118.2(10) . . ?
C28A C19A C18A 119.1(9) . . ?
C20A C19A C18A 122.7(9) . . ?
C25A C20A C21A 119.6(11) . . ?
C25A C20A C19A 118.0(10) . . ?
C21A C20A C19A 122.4(11) . . ?
C27A C28A C19A 122.8(10) . . ?
C27A C28A O2A 120.0(9) . . ?
C19A C28A O2A 117.2(10) . . ?
C28A C27A C26A 120.9(10) . . ?
C17A C18A C9A 117.5(10) . . ?
C17A C18A C19A 125.4(9) . . ?
C9A C18A C19A 117.0(9) . . ?
C12A C17A C18A 121.2(10) . . ?
C12A C17A C16A 117.1(11) . . ?
C18A C17A C16A 121.6(11) . . ?
C26A C25A C20A 120.9(11) . . ?
C26A C25A C24A 121.1(12) . . ?
C20A C25A C24A 118.0(11) . . ?
C10A C11A C12A 119.9(11) . . ?
C16A C15A C14A 121.8(12) . . ?
C23A C24A C25A 120.6(13) . . ?
C27A C26A C25A 119.2(11) . . ?
C15A C16A C17A 119.9(13) . . ?
C14A C13A C12A 120.1(14) . . ?
C17A C12A C13A 120.9(11) . . ?
C17A C12A C11A 118.8(11) . . ?
C13A C12A C11A 120.3(12) . . ?
C23A C22A C21A 123.1(12) . . ?
C22A C21A C20A 118.7(13) . . ?
C22A C23A C24A 119.9(12) . . ?
C13A C14A C15A 120.0(13) . . ?
Cl2A C1Z Cl1A 115.6(17) . . ?

_refine_diff_density_max         1.547
_refine_diff_density_min         -1.013
_refine_diff_density_rms         0.150



####################################################################### 
# 
# 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_R2
_database_code_depnum_ccdc_archive 'CCDC 1564393'
_audit_update_record             
;
2017-07-25 deposited with the CCDC.
2018-02-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C144 H72 N16 O8 Tb'
_chemical_formula_weight         2313.11

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -9.1472 9.1891 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           97
_space_group_name_H-M_alt        'I 4 2 2'
_space_group_name_Hall           'I 4 2'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x, z'
'-x, -y, z'
'y, -x, z'
'x, -y, -z'
'y, x, -z'
'-x, y, -z'
'-y, -x, -z'
'x+1/2, y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'y+1/2, x+1/2, -z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'

_cell_length_a                   24.4311(9)
_cell_length_b                   24.4311(9)
_cell_length_c                   23.9514(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     14296.1(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    1919
_cell_measurement_theta_min      3.6136
_cell_measurement_theta_max      67.0954

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.075
_exptl_crystal_F_000             4707
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_absorpt_coefficient_mu    2.879
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.31834
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'Enhance (Cu) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.2141
_diffrn_reflns_number            12946
_diffrn_reflns_av_unetI/netI     0.1870
_diffrn_reflns_av_R_equivalents  0.1458
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         3.691
_diffrn_reflns_theta_max         67.253
_diffrn_reflns_theta_full        67.253
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measured_fraction_theta_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.940
_diffrn_reflns_point_group_measured_fraction_full 0.941
_reflns_number_total             6047
_reflns_number_gt                3850
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.731
_reflns_Friedel_fraction_max     0.896
_reflns_Friedel_fraction_full    0.897

_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.
;

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1637P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 689 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.018(11)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         6047
_refine_ls_number_parameters     382
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1553
_refine_ls_R_factor_gt           0.1157
_refine_ls_wR_factor_ref         0.3347
_refine_ls_wR_factor_gt          0.2886
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.030
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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 0.0000 0.0000 0.13531(7) 0.0356(5) Uani 1 4 d S T P . .
O1 O 0.2994(4) 0.1136(5) 0.0502(6) 0.043(3) Uani 1 1 d . . . . .
O2 O 0.2372(4) 0.2132(4) 0.0597(5) 0.038(2) Uani 1 1 d . . . . .
N1 N -0.0279(5) -0.0762(6) 0.1945(5) 0.039(3) Uani 1 1 d . . . . .
N2 N -0.1249(6) -0.0589(6) 0.2008(6) 0.043(3) Uani 1 1 d . . . . .
N3 N 0.0693(5) 0.0413(5) 0.0764(5) 0.034(3) Uani 1 1 d . . . . .
N4 N 0.1343(5) -0.0344(5) 0.0708(5) 0.032(3) Uani 1 1 d . . . . .
C1 C -0.0822(8) -0.0901(8) 0.1996(6) 0.043(4) Uani 1 1 d . . . . .
C2 C -0.0855(7) -0.1498(7) 0.2057(7) 0.041(4) Uani 1 1 d . . . . .
C3 C -0.1283(8) -0.1866(8) 0.2071(8) 0.052(5) Uani 1 1 d . . . . .
H3 H -0.1650 -0.1738 0.2063 0.063 Uiso 1 1 calc R U . . .
C4 C -0.1178(8) -0.2408(7) 0.2097(7) 0.045(4) Uani 1 1 d . . . . .
H4 H -0.1478 -0.2656 0.2111 0.054 Uiso 1 1 calc R U . . .
C5 C -0.0666(9) -0.2610(8) 0.2105(8) 0.058(5) Uani 1 1 d . . . . .
H5 H -0.0608 -0.2994 0.2136 0.070 Uiso 1 1 calc R U . . .
C6 C -0.0217(9) -0.2254(7) 0.2066(8) 0.055(5) Uani 1 1 d . . . . .
H6 H 0.0147 -0.2388 0.2057 0.066 Uiso 1 1 calc R U . . .
C7 C -0.0325(7) -0.1707(7) 0.2043(7) 0.043(4) Uani 1 1 d . . . . .
C8 C 0.0042(8) -0.1225(6) 0.1990(5) 0.035(3) Uani 1 1 d . . . . .
C9 C 0.1205(6) 0.0191(6) 0.0716(7) 0.032(3) Uani 1 1 d . . . . .
C10 C 0.1600(6) 0.0642(6) 0.0666(6) 0.031(3) Uani 1 1 d . . . . .
C11 C 0.2165(6) 0.0639(7) 0.0606(7) 0.038(3) Uani 1 1 d . . . . .
H11 H 0.2363 0.0305 0.0584 0.045 Uiso 1 1 calc R U . . .
C12 C 0.2431(6) 0.1133(6) 0.0581(7) 0.037(3) Uani 1 1 d . . . . .
C13 C 0.2139(6) 0.1625(6) 0.0625(7) 0.035(3) Uani 1 1 d . . . . .
C14 C 0.1571(6) 0.1619(7) 0.0674(5) 0.030(3) Uani 1 1 d . . . . .
H14 H 0.1367 0.1949 0.0699 0.037 Uiso 1 1 calc R U . . .
C15 C 0.1316(6) 0.1118(6) 0.0685(5) 0.031(3) Uani 1 1 d . . . . .
C16 C 0.0743(6) 0.0955(6) 0.0728(6) 0.037(4) Uani 1 1 d . . . . .
C17 C 0.3376(8) 0.1394(9) -0.0964(9) 0.058(5) Uani 1 1 d . . . . .
H17 H 0.3379 0.1200 -0.1308 0.070 Uiso 1 1 calc R U . . .
C18 C 0.3190(8) 0.1138(9) -0.0479(10) 0.060(6) Uani 1 1 d . . . . .
H18 H 0.3075 0.0767 -0.0490 0.072 Uiso 1 1 calc R U . . .
C19 C 0.3171(5) 0.1428(6) 0.0024(10) 0.042(3) Uani 1 1 d . . . . .
C20 C 0.3365(6) 0.1949(6) 0.0070(7) 0.041(4) Uani 1 1 d . . . . .
C21 C 0.3540(7) 0.2228(8) -0.0400(8) 0.043(4) Uani 1 1 d . . . . .
C22 C 0.3556(7) 0.1936(9) -0.0940(7) 0.052(5) Uani 1 1 d . . . . .
C23 C 0.3717(7) 0.2243(11) -0.1425(9) 0.063(6) Uani 1 1 d . . . . .
H23 H 0.3736 0.2062 -0.1775 0.076 Uiso 1 1 calc R U . . .
C24 C 0.3836(8) 0.2759(10) -0.1400(10) 0.062(5) Uani 1 1 d . . . . .
H24 H 0.3925 0.2948 -0.1735 0.075 Uiso 1 1 calc R U . . .
C25 C 0.3835(7) 0.3049(9) -0.0891(9) 0.057(5) Uani 1 1 d . . . . .
H25 H 0.3934 0.3425 -0.0883 0.068 Uiso 1 1 calc R U . . .
C26 C 0.3689(7) 0.2783(8) -0.0404(8) 0.048(4) Uani 1 1 d . . . . .
H26 H 0.3689 0.2981 -0.0063 0.058 Uiso 1 1 calc R U . . .
C27 C 0.3228(9) 0.2582(10) 0.1747(9) 0.064(5) Uani 1 1 d . . . . .
H27 H 0.3184 0.2702 0.2122 0.077 Uiso 1 1 calc R U . . .
C28 C 0.2788(6) 0.2411(7) 0.1444(8) 0.044(4) Uani 1 1 d . . . . .
H28 H 0.2435 0.2418 0.1610 0.053 Uiso 1 1 calc R U . . .
C29 C 0.2845(6) 0.2231(6) 0.0907(7) 0.040(4) Uani 1 1 d . . . . .
C30 C 0.3350(7) 0.2193(7) 0.0625(7) 0.038(4) Uani 1 1 d . . . . .
C31 C 0.3818(6) 0.2365(7) 0.0934(8) 0.044(4) Uani 1 1 d . . . . .
C32 C 0.3765(8) 0.2576(10) 0.1485(9) 0.060(6) Uani 1 1 d . . . . .
C33 C 0.4241(10) 0.2789(12) 0.1759(11) 0.084(8) Uani 1 1 d . . . . .
H33 H 0.4202 0.2959 0.2113 0.100 Uiso 1 1 calc R U . . .
C34 C 0.4705(9) 0.2756(15) 0.1547(10) 0.101(11) Uani 1 1 d . . . . .
H34 H 0.5010 0.2894 0.1750 0.121 Uiso 1 1 calc R U . . .
C35 C 0.4801(8) 0.2506(12) 0.0981(10) 0.090(9) Uani 1 1 d . . . . .
H35 H 0.5159 0.2475 0.0829 0.108 Uiso 1 1 calc R U . . .
C36 C 0.4346(7) 0.2321(9) 0.0691(8) 0.059(5) Uani 1 1 d . . . . .
H36 H 0.4388 0.2166 0.0330 0.071 Uiso 1 1 calc R 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
Tb1 N3 2.423(13) . ?
Tb1 N3 2.423(13) 3 ?
Tb1 N3 2.423(13) 4 ?
Tb1 N3 2.423(13) 2 ?
Tb1 N1 2.438(13) . ?
Tb1 N1 2.438(13) 3 ?
Tb1 N1 2.438(13) 2 ?
Tb1 N1 2.438(13) 4 ?
O1 C12 1.390(18) . ?
O1 C19 1.42(2) . ?
O2 C13 1.364(18) . ?
O2 C29 1.393(19) . ?
N1 C1 1.37(2) . ?
N1 C8 1.38(2) . ?
N2 C1 1.29(3) . ?
N2 C8 1.34(2) 4 ?
N3 C16 1.334(18) . ?
N3 C9 1.37(2) . ?
N4 C9 1.350(19) . ?
N4 C16 1.360(19) 4 ?
C1 C2 1.47(3) . ?
C2 C3 1.38(2) . ?
C2 C7 1.39(2) . ?
C3 C4 1.35(2) . ?
C3 H3 0.9500 . ?
C4 C5 1.35(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.40(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.36(2) . ?
C6 H6 0.9500 . ?
C7 C8 1.49(2) . ?
C8 N2 1.34(2) 2 ?
C9 C10 1.47(2) . ?
C10 C15 1.36(2) . ?
C10 C11 1.39(2) . ?
C11 C12 1.37(2) . ?
C11 H11 0.9500 . ?
C12 C13 1.40(2) . ?
C13 C14 1.39(2) . ?
C14 C15 1.37(2) . ?
C14 H14 0.9500 . ?
C15 C16 1.46(2) . ?
C16 N4 1.360(19) 2 ?
C17 C18 1.39(3) . ?
C17 C22 1.40(3) . ?
C17 H17 0.9500 . ?
C18 C19 1.40(3) . ?
C18 H18 0.9500 . ?
C19 C20 1.36(2) . ?
C20 C21 1.38(2) . ?
C20 C30 1.46(2) . ?
C21 C26 1.40(3) . ?
C21 C22 1.48(2) . ?
C22 C23 1.44(3) . ?
C23 C24 1.30(3) . ?
C23 H23 0.9500 . ?
C24 C25 1.41(3) . ?
C24 H24 0.9500 . ?
C25 C26 1.38(3) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C27 C28 1.36(3) . ?
C27 C32 1.45(3) . ?
C27 H27 0.9500 . ?
C28 C29 1.37(2) . ?
C28 H28 0.9500 . ?
C29 C30 1.41(2) . ?
C30 C31 1.42(2) . ?
C31 C36 1.42(3) . ?
C31 C32 1.42(3) . ?
C32 C33 1.43(3) . ?
C33 C34 1.24(3) . ?
C33 H33 0.9500 . ?
C34 C35 1.51(3) . ?
C34 H34 0.9500 . ?
C35 C36 1.39(3) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 Tb1 N3 108.8(6) . 3 ?
N3 Tb1 N3 70.2(3) . 4 ?
N3 Tb1 N3 70.2(3) 3 4 ?
N3 Tb1 N3 70.2(3) . 2 ?
N3 Tb1 N3 70.2(3) 3 2 ?
N3 Tb1 N3 108.8(6) 4 2 ?
N3 Tb1 N1 148.4(4) . . ?
N3 Tb1 N1 79.9(4) 3 . ?
N3 Tb1 N1 85.5(4) 4 . ?
N3 Tb1 N1 139.1(4) 2 . ?
N3 Tb1 N1 79.9(4) . 3 ?
N3 Tb1 N1 148.4(4) 3 3 ?
N3 Tb1 N1 139.1(4) 4 3 ?
N3 Tb1 N1 85.5(4) 2 3 ?
N1 Tb1 N1 108.9(6) . 3 ?
N3 Tb1 N1 85.5(4) . 2 ?
N3 Tb1 N1 139.1(4) 3 2 ?
N3 Tb1 N1 79.9(4) 4 2 ?
N3 Tb1 N1 148.4(4) 2 2 ?
N1 Tb1 N1 70.2(3) . 2 ?
N1 Tb1 N1 70.2(3) 3 2 ?
N3 Tb1 N1 139.1(4) . 4 ?
N3 Tb1 N1 85.5(4) 3 4 ?
N3 Tb1 N1 148.4(4) 4 4 ?
N3 Tb1 N1 79.9(4) 2 4 ?
N1 Tb1 N1 70.2(3) . 4 ?
N1 Tb1 N1 70.2(3) 3 4 ?
N1 Tb1 N1 108.9(6) 2 4 ?
C12 O1 C19 114.5(12) . . ?
C13 O2 C29 118.6(12) . . ?
C1 N1 C8 109.9(15) . . ?
C1 N1 Tb1 120.7(12) . . ?
C8 N1 Tb1 120.8(11) . . ?
C1 N2 C8 123.5(15) . 4 ?
C16 N3 C9 107.7(12) . . ?
C16 N3 Tb1 121.0(10) . . ?
C9 N3 Tb1 121.6(10) . . ?
C9 N4 C16 121.3(13) . 4 ?
N2 C1 N1 129.4(17) . . ?
N2 C1 C2 122.7(15) . . ?
N1 C1 C2 107.9(17) . . ?
C3 C2 C7 117.7(17) . . ?
C3 C2 C1 133.7(18) . . ?
C7 C2 C1 108.2(15) . . ?
C4 C3 C2 119.8(19) . . ?
C4 C3 H3 120.1 . . ?
C2 C3 H3 120.1 . . ?
C5 C4 C3 122.4(17) . . ?
C5 C4 H4 118.8 . . ?
C3 C4 H4 118.8 . . ?
C4 C5 C6 119.9(18) . . ?
C4 C5 H5 120.1 . . ?
C6 C5 H5 120.1 . . ?
C7 C6 C5 117.4(19) . . ?
C7 C6 H6 121.3 . . ?
C5 C6 H6 121.3 . . ?
C6 C7 C2 122.6(18) . . ?
C6 C7 C8 131.6(17) . . ?
C2 C7 C8 105.8(15) . . ?
N2 C8 N1 127.4(15) 2 . ?
N2 C8 C7 124.4(14) 2 . ?
N1 C8 C7 108.2(16) . . ?
N4 C9 N3 127.7(13) . . ?
N4 C9 C10 124.0(14) . . ?
N3 C9 C10 108.2(13) . . ?
C15 C10 C11 121.1(14) . . ?
C15 C10 C9 107.7(13) . . ?
C11 C10 C9 131.2(14) . . ?
C12 C11 C10 118.1(14) . . ?
C12 C11 H11 120.9 . . ?
C10 C11 H11 120.9 . . ?
C11 C12 O1 118.6(14) . . ?
C11 C12 C13 120.7(14) . . ?
O1 C12 C13 120.7(14) . . ?
O2 C13 C14 115.4(13) . . ?
O2 C13 C12 124.2(13) . . ?
C14 C13 C12 120.3(14) . . ?
C15 C14 C13 117.5(15) . . ?
C15 C14 H14 121.2 . . ?
C13 C14 H14 121.2 . . ?
C10 C15 C14 122.1(14) . . ?
C10 C15 C16 105.1(12) . . ?
C14 C15 C16 132.8(13) . . ?
N3 C16 N4 128.9(14) . 2 ?
N3 C16 C15 111.3(13) . . ?
N4 C16 C15 119.7(13) 2 . ?
C18 C17 C22 119.6(19) . . ?
C18 C17 H17 120.2 . . ?
C22 C17 H17 120.2 . . ?
C17 C18 C19 120.1(19) . . ?
C17 C18 H18 119.9 . . ?
C19 C18 H18 119.9 . . ?
C20 C19 C18 122(2) . . ?
C20 C19 O1 120.7(19) . . ?
C18 C19 O1 116.8(15) . . ?
C19 C20 C21 120.1(18) . . ?
C19 C20 C30 116.7(17) . . ?
C21 C20 C30 123.2(15) . . ?
C20 C21 C26 124.2(17) . . ?
C20 C21 C22 118.9(16) . . ?
C26 C21 C22 116.9(17) . . ?
C17 C22 C23 123(2) . . ?
C17 C22 C21 118.9(17) . . ?
C23 C22 C21 118(2) . . ?
C24 C23 C22 122(2) . . ?
C24 C23 H23 118.9 . . ?
C22 C23 H23 118.9 . . ?
C23 C24 C25 122(2) . . ?
C23 C24 H24 119.0 . . ?
C25 C24 H24 119.0 . . ?
C26 C25 C24 120(2) . . ?
C26 C25 H25 120.2 . . ?
C24 C25 H25 120.2 . . ?
C25 C26 C21 122(2) . . ?
C25 C26 H26 119.1 . . ?
C21 C26 H26 119.1 . . ?
C28 C27 C32 118.7(18) . . ?
C28 C27 H27 120.7 . . ?
C32 C27 H27 120.7 . . ?
C27 C28 C29 121.3(16) . . ?
C27 C28 H28 119.3 . . ?
C29 C28 H28 119.3 . . ?
C28 C29 O2 118.2(14) . . ?
C28 C29 C30 124.0(15) . . ?
O2 C29 C30 117.4(14) . . ?
C29 C30 C31 115.8(15) . . ?
C29 C30 C20 118.9(14) . . ?
C31 C30 C20 125.1(16) . . ?
C36 C31 C30 119.6(17) . . ?
C36 C31 C32 119.4(16) . . ?
C30 C31 C32 121.0(17) . . ?
C31 C32 C33 118.8(19) . . ?
C31 C32 C27 119.0(18) . . ?
C33 C32 C27 122.2(19) . . ?
C34 C33 C32 122(2) . . ?
C34 C33 H33 119.0 . . ?
C32 C33 H33 119.0 . . ?
C33 C34 C35 122(2) . . ?
C33 C34 H34 118.8 . . ?
C35 C34 H34 118.8 . . ?
C36 C35 C34 117.3(19) . . ?
C36 C35 H35 121.3 . . ?
C34 C35 H35 121.3 . . ?
C35 C36 C31 119.9(18) . . ?
C35 C36 H36 120.0 . . ?
C31 C36 H36 120.0 . . ?

_refine_diff_density_max         2.204
_refine_diff_density_min         -1.478
_refine_diff_density_rms         0.174



####################################################################### 
# 
# 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_S2
_database_code_depnum_ccdc_archive 'CCDC 1564395'
_audit_update_record             
;
2017-07-25 deposited with the CCDC.
2018-02-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C144 H72 Cl0 N16 O8 Tb'
_chemical_formula_weight         2313.11

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -9.1472 9.1891 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           97
_space_group_name_H-M_alt        'I 4 2 2'
_space_group_name_Hall           'I 4 2'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x, z'
'-x, -y, z'
'y, -x, z'
'x, -y, -z'
'y, x, -z'
'-x, y, -z'
'-y, -x, -z'
'x+1/2, y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'y+1/2, x+1/2, -z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'

_cell_length_a                   24.354(3)
_cell_length_b                   24.354(3)
_cell_length_c                   23.9482(14)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     14204(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    1145
_cell_measurement_theta_min      3.6268
_cell_measurement_theta_max      67.6980

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.082
_exptl_crystal_F_000             4707
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_absorpt_coefficient_mu    2.898
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.38503
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'Enhance (Cu) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.2141
_diffrn_reflns_number            12663
_diffrn_reflns_av_unetI/netI     0.2613
_diffrn_reflns_av_R_equivalents  0.1434
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         3.691
_diffrn_reflns_theta_max         67.814
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measured_fraction_theta_full 0.968
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_Laue_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_point_group_measured_fraction_full 0.965
_reflns_number_total             6218
_reflns_number_gt                1978
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.789
_reflns_Friedel_fraction_max     0.955
_reflns_Friedel_fraction_full    0.961

_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.
;

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0789P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 290 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.030(17)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         6218
_refine_ls_number_parameters     382
_refine_ls_number_restraints     936
_refine_ls_R_factor_all          0.2052
_refine_ls_R_factor_gt           0.1092
_refine_ls_wR_factor_ref         0.2838
_refine_ls_wR_factor_gt          0.2244
_refine_ls_goodness_of_fit_ref   0.838
_refine_ls_restrained_S_all      0.798
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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 0.5000 0.5000 0.13531(7) 0.0727(9) Uani 1 4 d S T P . .
O1 O 0.2867(5) 0.2631(5) 0.0595(4) 0.059(3) Uani 1 1 d . . . . .
O2 O 0.3856(6) 0.2004(5) 0.0496(6) 0.068(4) Uani 1 1 d . . . . .
N1 N 0.5288(6) 0.4229(6) 0.1931(6) 0.054(4) Uani 1 1 d . U . . .
N2 N 0.6242(7) 0.4414(7) 0.2005(5) 0.056(4) Uani 1 1 d . . . . .
N3 N 0.4598(4) 0.4306(5) 0.0751(4) 0.031(3) Uani 1 1 d . . . . .
N4 N 0.5362(6) 0.3664(9) 0.0713(6) 0.081(6) Uani 1 1 d . . . . .
C1 C 0.5849(11) 0.4122(9) 0.1994(6) 0.066(4) Uani 1 1 d . U . . .
C2 C 0.5868(10) 0.3523(8) 0.2035(6) 0.065(4) Uani 1 1 d . U . . .
C3 C 0.6262(10) 0.3136(8) 0.2079(6) 0.074(4) Uani 1 1 d . U . . .
H3 H 0.6630 0.3262 0.2098 0.089 Uiso 1 1 calc R U . . .
C4 C 0.6184(9) 0.2571(8) 0.2099(6) 0.063(4) Uani 1 1 d . U . . .
H4 H 0.6479 0.2317 0.2113 0.076 Uiso 1 1 calc R U . . .
C5 C 0.5624(11) 0.2407(10) 0.2098(8) 0.084(5) Uani 1 1 d . U . . .
H5 H 0.5538 0.2028 0.2127 0.101 Uiso 1 1 calc R U . . .
C6 C 0.5239(9) 0.2749(8) 0.2060(6) 0.071(4) Uani 1 1 d . U . . .
H6 H 0.4875 0.2609 0.2048 0.085 Uiso 1 1 calc R U . . .
C7 C 0.5302(9) 0.3323(9) 0.2034(7) 0.071(4) Uani 1 1 d . U . . .
C8 C 0.4965(12) 0.3799(7) 0.1979(5) 0.066(4) Uani 1 1 d . U . . .
C9 C 0.4799(9) 0.3755(8) 0.0715(6) 0.055(4) Uani 1 1 d . U . . .
C10 C 0.4344(9) 0.3416(9) 0.0650(6) 0.059(4) Uani 1 1 d . U . . .
C11 C 0.4360(9) 0.2821(8) 0.0605(6) 0.062(4) Uani 1 1 d . U . . .
H11 H 0.4697 0.2624 0.0602 0.074 Uiso 1 1 calc R U . . .
C12 C 0.3864(9) 0.2561(8) 0.0566(6) 0.058(3) Uani 1 1 d . U . . .
C13 C 0.3371(9) 0.2823(8) 0.0615(6) 0.057(3) Uani 1 1 d . U . . .
C14 C 0.3377(9) 0.3421(8) 0.0665(5) 0.056(3) Uani 1 1 d . U . . .
H14 H 0.3046 0.3628 0.0674 0.067 Uiso 1 1 calc R U . . .
C15 C 0.3887(9) 0.3674(8) 0.0698(5) 0.061(4) Uani 1 1 d . U . . .
C16 C 0.4041(7) 0.4260(5) 0.0735(4) 0.034(3) Uani 1 1 d . U . . .
C17 C 0.3038(9) 0.1653(7) 0.0055(9) 0.071(3) Uani 1 1 d . U . . .
C18 C 0.3571(8) 0.1805(7) 0.0005(10) 0.066(3) Uani 1 1 d . U . . .
C19 C 0.3882(11) 0.1811(8) -0.0493(8) 0.075(4) Uani 1 1 d . U . . .
H19 H 0.4247 0.1948 -0.0508 0.090 Uiso 1 1 calc R U . . .
C20 C 0.3617(10) 0.1603(8) -0.0954(8) 0.079(4) Uani 1 1 d . U . . .
H20 H 0.3816 0.1559 -0.1292 0.095 Uiso 1 1 calc R U . . .
C21 C 0.3058(10) 0.1451(8) -0.0939(7) 0.068(4) Uani 1 1 d . U . . .
C22 C 0.2782(11) 0.1441(8) -0.0421(7) 0.069(4) Uani 1 1 d . U . . .
C23 C 0.2221(10) 0.1329(8) -0.0408(7) 0.075(4) Uani 1 1 d . U . . .
H23 H 0.2031 0.1369 -0.0064 0.090 Uiso 1 1 calc R U . . .
C24 C 0.1929(10) 0.1162(8) -0.0870(8) 0.084(5) Uani 1 1 d . U . . .
H24 H 0.1558 0.1045 -0.0847 0.100 Uiso 1 1 calc R U . . .
C25 C 0.2226(11) 0.1179(8) -0.1389(8) 0.079(5) Uani 1 1 d . U . . .
H25 H 0.2034 0.1104 -0.1727 0.095 Uiso 1 1 calc R U . . .
C26 C 0.2739(10) 0.1290(8) -0.1413(8) 0.079(4) Uani 1 1 d . U . . .
H26 H 0.2918 0.1265 -0.1764 0.094 Uiso 1 1 calc R U . . .
C27 C 0.2785(10) 0.1653(9) 0.0631(8) 0.073(4) Uani 1 1 d . U . . .
C28 C 0.2782(9) 0.2151(8) 0.0878(8) 0.069(4) Uani 1 1 d . U . . .
C29 C 0.2579(8) 0.2208(8) 0.1430(7) 0.073(4) Uani 1 1 d . U . . .
H29 H 0.2549 0.2564 0.1589 0.087 Uiso 1 1 calc R U . . .
C30 C 0.2426(9) 0.1760(8) 0.1738(8) 0.082(4) Uani 1 1 d . U . . .
H30 H 0.2321 0.1804 0.2117 0.098 Uiso 1 1 calc R U . . .
C31 C 0.2423(10) 0.1231(9) 0.1492(9) 0.081(4) Uani 1 1 d . U . . .
C32 C 0.2654(10) 0.1172(8) 0.0899(8) 0.077(4) Uani 1 1 d . U . . .
C33 C 0.2669(10) 0.0655(8) 0.0707(8) 0.078(4) Uani 1 1 d . U . . .
H33 H 0.2803 0.0609 0.0338 0.093 Uiso 1 1 calc R U . . .
C34 C 0.2524(10) 0.0216(8) 0.0959(8) 0.094(5) Uani 1 1 d . U . . .
H34 H 0.2587 -0.0137 0.0802 0.113 Uiso 1 1 calc R U . . .
C35 C 0.2238(11) 0.0289(8) 0.1540(9) 0.093(5) Uani 1 1 d . U . . .
H35 H 0.2089 -0.0021 0.1726 0.112 Uiso 1 1 calc R U . . .
C36 C 0.2207(10) 0.0748(9) 0.1756(9) 0.090(5) Uani 1 1 d . U . . .
H36 H 0.2034 0.0783 0.2110 0.109 Uiso 1 1 calc R 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
Tb1 N3 2.429(11) . ?
Tb1 N3 2.429(11) 4_565 ?
Tb1 N3 2.429(11) 3_665 ?
Tb1 N3 2.429(11) 2_655 ?
Tb1 N1 2.437(15) . ?
Tb1 N1 2.437(15) 2_655 ?
Tb1 N1 2.437(15) 3_665 ?
Tb1 N1 2.437(15) 4_565 ?
O1 C13 1.32(2) . ?
O1 C28 1.37(2) . ?
O2 C12 1.37(2) . ?
O2 C18 1.45(2) . ?
N1 C8 1.31(2) . ?
N1 C1 1.40(2) . ?
N2 C1 1.19(3) . ?
N2 C8 1.35(3) 2_655 ?
N3 C16 1.362(17) . ?
N3 C9 1.43(2) . ?
N4 C16 1.30(2) 2_655 ?
N4 C9 1.39(2) . ?
C1 C2 1.46(3) . ?
C2 C3 1.35(2) . ?
C2 C7 1.46(3) . ?
C3 C4 1.39(2) . ?
C3 H3 0.9500 . ?
C4 C5 1.42(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.26(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.41(3) . ?
C6 H6 0.9500 . ?
C7 C8 1.43(3) . ?
C8 N2 1.35(3) 4_565 ?
C9 C10 1.39(3) . ?
C10 C15 1.28(3) . ?
C10 C11 1.45(3) . ?
C11 C12 1.37(3) . ?
C11 H11 0.9500 . ?
C12 C13 1.36(3) . ?
C13 C14 1.46(3) . ?
C14 C15 1.39(2) . ?
C14 H14 0.9500 . ?
C15 C16 1.48(2) . ?
C16 N4 1.30(2) 4_565 ?
C17 C18 1.36(2) . ?
C17 C22 1.40(3) . ?
C17 C27 1.51(3) . ?
C18 C19 1.41(3) . ?
C19 C20 1.38(3) . ?
C19 H19 0.9500 . ?
C20 C21 1.41(3) . ?
C20 H20 0.9500 . ?
C21 C22 1.41(2) . ?
C21 C26 1.43(3) . ?
C22 C23 1.39(3) . ?
C23 C24 1.38(3) . ?
C23 H23 0.9500 . ?
C24 C25 1.44(3) . ?
C24 H24 0.9500 . ?
C25 C26 1.28(3) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C27 C28 1.35(2) . ?
C27 C32 1.37(3) . ?
C28 C29 1.42(2) . ?
C29 C30 1.37(2) . ?
C29 H29 0.9500 . ?
C30 C31 1.42(3) . ?
C30 H30 0.9500 . ?
C31 C36 1.43(3) . ?
C31 C32 1.54(3) . ?
C32 C33 1.34(2) . ?
C33 C34 1.28(2) . ?
C33 H33 0.9500 . ?
C34 C35 1.57(3) . ?
C34 H34 0.9500 . ?
C35 C36 1.23(3) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 Tb1 N3 69.3(3) . 4_565 ?
N3 Tb1 N3 107.1(5) . 3_665 ?
N3 Tb1 N3 69.3(3) 4_565 3_665 ?
N3 Tb1 N3 69.3(3) . 2_655 ?
N3 Tb1 N3 107.1(5) 4_565 2_655 ?
N3 Tb1 N3 69.3(3) 3_665 2_655 ?
N3 Tb1 N1 85.2(4) . . ?
N3 Tb1 N1 148.1(4) 4_565 . ?
N3 Tb1 N1 139.3(4) 3_665 . ?
N3 Tb1 N1 80.0(4) 2_655 . ?
N3 Tb1 N1 148.1(4) . 2_655 ?
N3 Tb1 N1 139.3(4) 4_565 2_655 ?
N3 Tb1 N1 80.0(4) 3_665 2_655 ?
N3 Tb1 N1 85.2(4) 2_655 2_655 ?
N1 Tb1 N1 71.2(3) . 2_655 ?
N3 Tb1 N1 139.3(4) . 3_665 ?
N3 Tb1 N1 80.0(4) 4_565 3_665 ?
N3 Tb1 N1 85.2(4) 3_665 3_665 ?
N3 Tb1 N1 148.1(4) 2_655 3_665 ?
N1 Tb1 N1 110.7(7) . 3_665 ?
N1 Tb1 N1 71.2(3) 2_655 3_665 ?
N3 Tb1 N1 80.0(4) . 4_565 ?
N3 Tb1 N1 85.2(4) 4_565 4_565 ?
N3 Tb1 N1 148.1(4) 3_665 4_565 ?
N3 Tb1 N1 139.3(4) 2_655 4_565 ?
N1 Tb1 N1 71.2(3) . 4_565 ?
N1 Tb1 N1 110.7(7) 2_655 4_565 ?
N1 Tb1 N1 71.2(3) 3_665 4_565 ?
C13 O1 C28 115.3(15) . . ?
C12 O2 C18 115.9(14) . . ?
C8 N1 C1 115.3(18) . . ?
C8 N1 Tb1 119.3(13) . . ?
C1 N1 Tb1 119.1(13) . . ?
C1 N2 C8 122(2) . 2_655 ?
C16 N3 C9 105.3(12) . . ?
C16 N3 Tb1 118.4(8) . . ?
C9 N3 Tb1 123.4(10) . . ?
C16 N4 C9 126(2) 2_655 . ?
N2 C1 N1 132(2) . . ?
N2 C1 C2 125(2) . . ?
N1 C1 C2 103(2) . . ?
C3 C2 C1 137(3) . . ?
C3 C2 C7 116(2) . . ?
C1 C2 C7 107.6(19) . . ?
C2 C3 C4 127(2) . . ?
C2 C3 H3 116.7 . . ?
C4 C3 H3 116.7 . . ?
C3 C4 C5 114.2(19) . . ?
C3 C4 H4 122.9 . . ?
C5 C4 H4 122.9 . . ?
C6 C5 C4 122(2) . . ?
C6 C5 H5 119.0 . . ?
C4 C5 H5 119.0 . . ?
C5 C6 C7 125(3) . . ?
C5 C6 H6 117.3 . . ?
C7 C6 H6 117.3 . . ?
C6 C7 C8 138(2) . . ?
C6 C7 C2 115.8(18) . . ?
C8 C7 C2 106(2) . . ?
N1 C8 N2 131.3(19) . 4_565 ?
N1 C8 C7 108(2) . . ?
N2 C8 C7 121(2) 4_565 . ?
N4 C9 C10 134(2) . . ?
N4 C9 N3 119.2(19) . . ?
C10 C9 N3 106.9(17) . . ?
C15 C10 C9 113(2) . . ?
C15 C10 C11 121(2) . . ?
C9 C10 C11 125(2) . . ?
C12 C11 C10 116(2) . . ?
C12 C11 H11 121.9 . . ?
C10 C11 H11 121.9 . . ?
C13 C12 O2 117.7(19) . . ?
C13 C12 C11 124(2) . . ?
O2 C12 C11 119(2) . . ?
O1 C13 C12 130.6(19) . . ?
O1 C13 C14 111.5(19) . . ?
C12 C13 C14 118(2) . . ?
C15 C14 C13 117(2) . . ?
C15 C14 H14 121.5 . . ?
C13 C14 H14 121.5 . . ?
C10 C15 C14 124(2) . . ?
C10 C15 C16 105.0(19) . . ?
C14 C15 C16 131.2(18) . . ?
N4 C16 N3 130.3(16) 4_565 . ?
N4 C16 C15 120.1(17) 4_565 . ?
N3 C16 C15 109.5(13) . . ?
C18 C17 C22 117(2) . . ?
C18 C17 C27 118(2) . . ?
C22 C17 C27 124(2) . . ?
C17 C18 C19 126(2) . . ?
C17 C18 O2 119(2) . . ?
C19 C18 O2 115.1(17) . . ?
C20 C19 C18 115(2) . . ?
C20 C19 H19 122.5 . . ?
C18 C19 H19 122.5 . . ?
C19 C20 C21 122(2) . . ?
C19 C20 H20 119.1 . . ?
C21 C20 H20 119.1 . . ?
C22 C21 C20 119(2) . . ?
C22 C21 C26 116(2) . . ?
C20 C21 C26 125.1(19) . . ?
C23 C22 C17 119.4(19) . . ?
C23 C22 C21 119(2) . . ?
C17 C22 C21 120(2) . . ?
C24 C23 C22 123(2) . . ?
C24 C23 H23 118.5 . . ?
C22 C23 H23 118.5 . . ?
C23 C24 C25 115(2) . . ?
C23 C24 H24 122.3 . . ?
C25 C24 H24 122.3 . . ?
C26 C25 C24 122(2) . . ?
C26 C25 H25 118.9 . . ?
C24 C25 H25 118.9 . . ?
C25 C26 C21 124(2) . . ?
C25 C26 H26 118.2 . . ?
C21 C26 H26 118.2 . . ?
C28 C27 C32 124.0(19) . . ?
C28 C27 C17 113.9(18) . . ?
C32 C27 C17 121.4(19) . . ?
C27 C28 O1 123.3(17) . . ?
C27 C28 C29 120.0(19) . . ?
O1 C28 C29 115.5(17) . . ?
C30 C29 C28 121.3(19) . . ?
C30 C29 H29 119.4 . . ?
C28 C29 H29 119.4 . . ?
C29 C30 C31 120.2(19) . . ?
C29 C30 H30 119.9 . . ?
C31 C30 H30 119.9 . . ?
C30 C31 C36 124(2) . . ?
C30 C31 C32 117.9(19) . . ?
C36 C31 C32 117.8(19) . . ?
C33 C32 C27 129(2) . . ?
C33 C32 C31 114.5(18) . . ?
C27 C32 C31 115.9(19) . . ?
C34 C33 C32 128(2) . . ?
C34 C33 H33 115.9 . . ?
C32 C33 H33 115.9 . . ?
C33 C34 C35 117(2) . . ?
C33 C34 H34 121.7 . . ?
C35 C34 H34 121.7 . . ?
C36 C35 C34 120(2) . . ?
C36 C35 H35 119.9 . . ?
C34 C35 H35 119.9 . . ?
C35 C36 C31 122(2) . . ?
C35 C36 H36 118.9 . . ?
C31 C36 H36 118.9 . . ?

_refine_diff_density_max         1.814
_refine_diff_density_min         -0.483
_refine_diff_density_rms         0.091



