# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_JSU-S2-Dy
_database_code_depnum_ccdc_archive 'CCDC 1983839'
loop_
_audit_author_name
_audit_author_address
'Olivier Roubeau'
;Instituto de Ciencia de Materiales de Aragon (ICMA), CSIC and Universidad de Zaragoza
Spain
;
_audit_update_record             
;
2020-05-05 deposited with the CCDC.	2020-05-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C116 H104 Cl4 Dy4 N24 O12 S8, 16(C5 H5 N), H2 O'
_chemical_formula_sum            'C196 H186 Cl4 Dy4 N40 O13 S8'
_chemical_formula_weight         4358.12

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_H-M_alt        'I 41/a'
_space_group_name_Hall           '-I 4ad'

_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+1/2, z'
'-y+3/4, x+1/4, z+1/4'
'y+1/4, -x+1/4, z+1/4'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1, z+1/2'
'-y+5/4, x+3/4, z+3/4'
'y+3/4, -x+3/4, z+3/4'
'-x, -y, -z'
'x, y-1/2, -z'
'y-3/4, -x-1/4, -z-1/4'
'-y-1/4, x-1/4, -z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y, -z+1/2'
'y-1/4, -x+1/4, -z+1/4'
'-y+1/4, x+1/4, -z+1/4'

_cell_length_a                   36.8408(13)
_cell_length_b                   36.8408(13)
_cell_length_c                   14.8390(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     20140(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    5488
_cell_measurement_theta_min      3.0920
_cell_measurement_theta_max      20.9300

_exptl_crystal_description       lath
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.437
_exptl_crystal_F_000             8824
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    1.671
_shelx_estimated_absorpt_T_min   0.680
_shelx_estimated_absorpt_T_max   0.936
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.87437
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_detector_area_resol_mean 16.3990
_diffrn_measurement_method       '/p and /w scans'
_diffrn_reflns_number            26610
_diffrn_reflns_av_unetI/netI     0.0786
_diffrn_reflns_av_R_equivalents  0.0722
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.087
_diffrn_reflns_theta_max         23.256
_diffrn_reflns_theta_full        23.256
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             7220
_reflns_number_gt                5005
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL & local programs'
_refine_special_details          
;All non-hydrogens were refined anisotropically, except the disordered
 coordinated water molecule O3 and O4. Hydrogens were placed
 geometrically on their carrier atom and refined with a riding model
 where possible. The hydrogen on the central water O1W 
 was refined with its thermal parameter 1.5 times that of O1W and half
 occupancy, due to symmetry. The central water is indeed
 disordered by symmetry over two orientations corresponding to hydrogen
 bonds with the four nearby imine N4 generated by symmetry. 
 The coordinated water and chloride are mutually disordered over their
 relative positions (Cl1:O3 and O4:Cl2).
 At the end of the refinement, there remain a rather large portion of
 the cell with only weak electron density peaks, that could not be
 modelled satisfactorily as solvent molecules. The corresponding
 void space was thus analyzed and taken into account with 
 PLATON/SQUEEZE that recovered a total of 1315 electrons per cell
 over 4 voids of ca. 1557 cubic angstroms and 4 voids of 334
 cubic angstrom, resulting in an improvement of ca 4.5% in R1.
 The electron content/void volume are reasonable for respectively
 10/2 diffuse pyridine solvent molecules per void, i.e. a total of
 48 additional pyridine molecules per cell, 12 per [Dy4] formula unit.
 This was reflected in the formula, weight etc.,SQUEEZE
;

_vrf_THETM01_JSU-S2-Dy           
;
PROBLEM:  The value of sine(theta_max)/wavelength is less than 0.575
            Calculated sin(theta_max)/wavelength =    0.5555 
RESPONSE: Crystals systematically damaged upon removal from the
mother liquor, likely resulting from loss/disordering of lattice
solvent upon exposure to air. Even by fast manipulation and mounting in
the cold N2 stream, this result in rather poor diffraction, with
the present data being cut at 0.90 angstrom. The remaining large voids
of diffuse electron density are also likely associated with this.
Altogether this result in poor values of theta_full and theta_max
;

_vrf_FORMU01_JSU-S2-Dy           
;
PROBLEM:  The ratio of given/expected absorption coefficient lies
               outside the range 0.90 <> 1.10
RESPONSE: Large voids with only diffuse electron density were
taken into account with PLATON/SQUEEZE that recovered a total of 
1315 electrons per cell over 4 voids of ca. 1557 cubic angstroms 
and 4 voids of 334 cubic angstrom. The electron content/void volume
are reasonable for respectively 10/2 diffuse pyridine solvent molecules
per void, i.e. a total of 48 additional pyridine molecules per cell, 
12 per [Dy4] formula unit. This was reflected in the formula, resulting
in a discrepancy with that from the atom sites. 
;

_vrf_CELLZ01_JSU-S2-Dy           
;
PROBLEM:  Difference between formula and atom_site contents detected.
RESPONSE: Large voids with only diffuse electron density were
taken into account with PLATON/SQUEEZE that recovered a total of 
1315 electrons per cell over 4 voids of ca. 1557 cubic angstroms 
and 4 voids of 334 cubic angstrom. The electron content/void volume
are reasonable for respectively 10/2 diffuse pyridine solvent molecules
per void, i.e. a total of 48 additional pyridine molecules per cell, 
12 per [Dy4] formula unit. This was reflected in the formula, resulting
in a discrepancy with that from the atom sites. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0656P)²+259.7452P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7220
_refine_ls_number_parameters     442
_refine_ls_number_restraints     93
_refine_ls_R_factor_all          0.1113
_refine_ls_R_factor_gt           0.0798
_refine_ls_wR_factor_ref         0.1946
_refine_ls_wR_factor_gt          0.1783
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.063
_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
Dy1 Dy 0.42886(2) 0.12302(2) 0.67597(4) 0.0610(2) Uani 1 1 d D . . . .
S1 S 0.46713(10) 0.03218(8) 0.9918(2) 0.0764(9) Uani 1 1 d . . . . .
S2 S 0.47319(7) 0.19493(8) 1.0590(2) 0.0638(8) Uani 1 1 d . . . . .
O1 O 0.42952(19) 0.10607(18) 0.8229(5) 0.0608(19) Uani 1 1 d . . . . .
O2 O 0.39014(19) 0.2605(2) 1.0870(5) 0.066(2) Uani 1 1 d . . . . .
O1W O 0.500000 0.250000 0.875000 0.095(6) Uani 1 4 d DS T P . .
H1W H 0.477(2) 0.252(9) 0.903(12) 0.142 Uiso 0.5 1 d D U P . .
Cl1 Cl 0.3745(3) 0.0773(3) 0.6353(9) 0.091(3) Uani 0.596(14) 1 d D U P A 1
O3 O 0.4072(4) 0.1650(5) 0.5634(13) 0.060(4) Uani 0.596(14) 1 d D U P A 1
Cl2 Cl 0.4245(4) 0.1757(3) 0.5477(7) 0.073(4) Uani 0.404(14) 1 d D U P A 2
O4 O 0.3812(11) 0.0833(11) 0.622(3) 0.085(10) Uiso 0.404(14) 1 d D U P A 2
N1 N 0.4591(3) 0.0903(2) 0.5409(6) 0.080(3) Uani 1 1 d . . . . .
N2 N 0.4656(3) 0.0682(2) 0.7104(7) 0.061(2) Uani 1 1 d . . . . .
N3 N 0.4690(3) 0.0571(2) 0.8002(6) 0.066(3) Uani 1 1 d . . . . .
N4 N 0.4408(2) 0.2669(2) 0.9967(6) 0.053(2) Uani 1 1 d D . . . .
N5 N 0.4296(2) 0.3021(3) 0.9893(6) 0.056(2) Uani 1 1 d . . . . .
N6 N 0.4086(2) 0.3723(2) 0.9898(6) 0.060(2) Uani 1 1 d . . . . .
C1 C 0.4541(5) 0.1012(4) 0.4564(11) 0.119(4) Uani 1 1 d . U . . .
H1A H 0.436192 0.119002 0.443194 0.143 Uiso 1 1 calc R U . . .
C2 C 0.4748(5) 0.0865(4) 0.3876(12) 0.122(4) Uani 1 1 d . U . . .
H2A H 0.470572 0.093959 0.327199 0.147 Uiso 1 1 calc R U . . .
C3 C 0.5012(5) 0.0617(4) 0.4051(10) 0.120(4) Uani 1 1 d . U . . .
H3A H 0.517112 0.053543 0.358814 0.144 Uiso 1 1 calc R U . . .
C4 C 0.5043(5) 0.0487(4) 0.4911(10) 0.113(4) Uani 1 1 d . U . . .
H4A H 0.520508 0.029423 0.504598 0.136 Uiso 1 1 calc R U . . .
C5 C 0.4835(4) 0.0640(3) 0.5575(9) 0.080(4) Uani 1 1 d . . . . .
C6 C 0.4855(4) 0.0514(3) 0.6513(8) 0.076(4) Uani 1 1 d . . . . .
H6A H 0.500762 0.031674 0.668021 0.092 Uiso 1 1 calc R U . . .
C7 C 0.4479(3) 0.0789(3) 0.8507(7) 0.050(3) Uani 1 1 d . . . . .
C8 C 0.4452(3) 0.0691(3) 0.9456(8) 0.064(3) Uani 1 1 d . . . . .
C9 C 0.4269(3) 0.0879(3) 1.0088(8) 0.065(3) Uani 1 1 d . . . . .
H9A H 0.413683 0.109469 0.996002 0.077 Uiso 1 1 calc R U . . .
C10 C 0.4292(4) 0.0722(3) 1.0977(9) 0.075(4) Uani 1 1 d . . . . .
C11 C 0.4500(3) 0.0415(3) 1.0975(9) 0.075(4) Uani 1 1 d . . . . .
C12 C 0.4609(4) 0.0186(3) 1.1773(8) 0.094(5) Uani 1 1 d . . . . .
H12A H 0.440041 0.004237 1.197492 0.141 Uiso 1 1 calc R U . . .
H12B H 0.469093 0.034348 1.226478 0.141 Uiso 1 1 calc R U . . .
H12C H 0.480691 0.002239 1.159796 0.141 Uiso 1 1 calc R U . . .
C13 C 0.4116(4) 0.0890(4) 1.1752(9) 0.084(4) Uani 1 1 d . . . . .
C14 C 0.3893(5) 0.0658(4) 1.2394(11) 0.131(7) Uani 1 1 d . . . . .
H14A H 0.404880 0.048564 1.272773 0.157 Uiso 1 1 calc R U . . .
H14B H 0.370351 0.052064 1.206547 0.157 Uiso 1 1 calc R U . . .
C15 C 0.3719(5) 0.0943(4) 1.3044(11) 0.125(6) Uani 1 1 d . . . . .
H15A H 0.345126 0.093804 1.299474 0.150 Uiso 1 1 calc R U . . .
H15B H 0.378715 0.089020 1.367626 0.150 Uiso 1 1 calc R U . . .
C16 C 0.3868(4) 0.1322(4) 1.2757(10) 0.108(5) Uani 1 1 d . . . . .
H16A H 0.366721 0.148919 1.259764 0.129 Uiso 1 1 calc R U . . .
H16B H 0.401423 0.143272 1.324449 0.129 Uiso 1 1 calc R U . . .
C17 C 0.4099(3) 0.1239(4) 1.1946(8) 0.075(4) Uani 1 1 d . . . . .
C18 C 0.4279(3) 0.1536(3) 1.1468(8) 0.063(3) Uani 1 1 d . . . . .
C19 C 0.4099(3) 0.1874(3) 1.1243(8) 0.066(3) Uani 1 1 d . . . . .
H19A H 0.385520 0.192240 1.141031 0.080 Uiso 1 1 calc R U . . .
C20 C 0.4304(3) 0.2116(3) 1.0776(8) 0.062(3) Uani 1 1 d . . . . .
C21 C 0.4630(3) 0.1557(3) 1.1154(7) 0.062(3) Uani 1 1 d . . . . .
C22 C 0.4932(3) 0.1286(3) 1.1265(9) 0.080(4) Uani 1 1 d . . . . .
H22A H 0.488895 0.114022 1.180774 0.121 Uiso 1 1 calc R U . . .
H22B H 0.516384 0.141386 1.132219 0.121 Uiso 1 1 calc R U . . .
H22C H 0.493969 0.112586 1.073726 0.121 Uiso 1 1 calc R U . . .
C23 C 0.4197(3) 0.2486(3) 1.0521(7) 0.055(3) Uani 1 1 d . . . . .
C24 C 0.4473(3) 0.3242(3) 0.9414(7) 0.057(3) Uani 1 1 d . . . . .
H24A H 0.467201 0.315892 0.906355 0.068 Uiso 1 1 calc R U . . .
C25 C 0.4373(3) 0.3616(3) 0.9398(7) 0.059(3) Uani 1 1 d . . . . .
C26 C 0.4574(3) 0.3867(3) 0.8897(8) 0.073(3) Uani 1 1 d . . . . .
H26A H 0.477491 0.378811 0.854595 0.088 Uiso 1 1 calc R U . . .
C27 C 0.4480(4) 0.4227(4) 0.8915(10) 0.096(4) Uani 1 1 d . . . . .
H27A H 0.461139 0.440061 0.857105 0.115 Uiso 1 1 calc R U . . .
C28 C 0.4191(4) 0.4331(3) 0.9445(10) 0.092(4) Uani 1 1 d . . . . .
H28A H 0.412573 0.458026 0.948354 0.110 Uiso 1 1 calc R U . . .
C29 C 0.3999(4) 0.4076(3) 0.9918(9) 0.080(4) Uani 1 1 d . . . . .
H29A H 0.379680 0.415116 1.026954 0.096 Uiso 1 1 calc R U . . .
N1S N 0.4090(4) -0.0134(2) 0.7159(9) 0.174(5) Uani 1 1 d G U . . .
C1S C 0.4339(3) -0.0206(3) 0.7840(9) 0.145(4) Uani 1 1 d G U . . .
H1SA H 0.447548 -0.001414 0.809928 0.173 Uiso 1 1 calc R U . . .
C2S C 0.4388(3) -0.0560(3) 0.8143(8) 0.141(4) Uani 1 1 d G U . . .
H2SA H 0.455750 -0.060963 0.860865 0.170 Uiso 1 1 calc R U . . .
C3S C 0.4188(4) -0.0841(2) 0.7764(9) 0.143(4) Uani 1 1 d G U . . .
H3SA H 0.422099 -0.108319 0.797114 0.171 Uiso 1 1 calc R U . . .
C4S C 0.3939(4) -0.0769(3) 0.7083(9) 0.178(5) Uani 1 1 d G U . . .
H4SA H 0.380246 -0.096126 0.682425 0.214 Uiso 1 1 calc R U . . .
C5S C 0.3890(4) -0.0415(4) 0.6780(9) 0.185(5) Uani 1 1 d G U . . .
H5SB H 0.372044 -0.036577 0.631487 0.222 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
Dy1 O1 2.268(7) . ?
Dy1 O2 2.330(7) 12_657 ?
Dy1 O3 2.412(19) . ?
Dy1 O4 2.42(2) . ?
Dy1 N2 2.484(9) . ?
Dy1 N5 2.533(9) 12_657 ?
Dy1 N1 2.591(10) . ?
Dy1 N6 2.615(9) 12_657 ?
Dy1 Cl1 2.686(8) . ?
Dy1 Cl2 2.723(9) . ?
S1 C8 1.724(11) . ?
S1 C11 1.725(14) . ?
S2 C21 1.711(12) . ?
S2 C20 1.713(11) . ?
O1 C7 1.277(12) . ?
O2 C23 1.282(12) . ?
O1W H1W 0.95(2) . ?
N1 C1 1.331(16) . ?
N1 C5 1.342(15) . ?
N2 C6 1.302(14) . ?
N2 N3 1.400(12) . ?
N3 C7 1.346(13) . ?
N4 C23 1.319(12) . ?
N4 N5 1.365(11) . ?
N5 C24 1.261(12) . ?
N6 C29 1.337(14) . ?
N6 C25 1.352(13) . ?
C1 C2 1.39(2) . ?
C1 H1A 0.9500 . ?
C2 C3 1.36(2) . ?
C2 H2A 0.9500 . ?
C3 C4 1.368(19) . ?
C3 H3A 0.9500 . ?
C4 C5 1.370(18) . ?
C4 H4A 0.9500 . ?
C5 C6 1.469(16) . ?
C6 H6A 0.9500 . ?
C7 C8 1.458(15) . ?
C8 C9 1.347(15) . ?
C9 C10 1.444(16) . ?
C9 H9A 0.9500 . ?
C10 C11 1.365(15) . ?
C10 C13 1.460(17) . ?
C11 C12 1.510(15) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C17 1.317(17) . ?
C13 C14 1.521(18) . ?
C14 C15 1.56(2) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.559(19) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C17 1.507(16) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C18 1.462(16) . ?
C18 C21 1.375(14) . ?
C18 C19 1.448(14) . ?
C19 C20 1.358(14) . ?
C19 H19A 0.9500 . ?
C20 C23 1.470(14) . ?
C21 C22 1.507(14) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C24 C25 1.427(15) . ?
C24 H24A 0.9500 . ?
C25 C26 1.398(15) . ?
C26 C27 1.372(17) . ?
C26 H26A 0.9500 . ?
C27 C28 1.378(18) . ?
C27 H27A 0.9500 . ?
C28 C29 1.373(17) . ?
C28 H28A 0.9500 . ?
C29 H29A 0.9500 . ?
N1S C1S 1.3900 . ?
N1S C5S 1.3900 . ?
C1S C2S 1.3900 . ?
C1S H1SA 0.9500 . ?
C2S C3S 1.3900 . ?
C2S H2SA 0.9500 . ?
C3S C4S 1.3900 . ?
C3S H3SA 0.9500 . ?
C4S C5S 1.3900 . ?
C4S H4SA 0.9500 . ?
C5S H5SB 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Dy1 O2 98.2(3) . 12_657 ?
O1 Dy1 O3 147.8(4) . . ?
O2 Dy1 O3 94.9(4) 12_657 . ?
O1 Dy1 O4 99.2(12) . . ?
O2 Dy1 O4 146.2(13) 12_657 . ?
O1 Dy1 N2 64.7(3) . . ?
O2 Dy1 N2 73.4(3) 12_657 . ?
O3 Dy1 N2 147.5(5) . . ?
O4 Dy1 N2 88.3(12) . . ?
O1 Dy1 N5 75.3(3) . 12_657 ?
O2 Dy1 N5 63.4(3) 12_657 12_657 ?
O3 Dy1 N5 84.7(4) . 12_657 ?
O4 Dy1 N5 149.6(13) . 12_657 ?
N2 Dy1 N5 114.6(3) . 12_657 ?
O1 Dy1 N1 127.6(3) . . ?
O2 Dy1 N1 69.5(3) 12_657 . ?
O3 Dy1 N1 84.6(5) . . ?
O4 Dy1 N1 77.0(13) . . ?
N2 Dy1 N1 63.0(3) . . ?
N5 Dy1 N1 130.4(3) 12_657 . ?
O1 Dy1 N6 71.7(3) . 12_657 ?
O2 Dy1 N6 126.6(3) 12_657 12_657 ?
O3 Dy1 N6 76.8(5) . 12_657 ?
O4 Dy1 N6 86.5(13) . 12_657 ?
N2 Dy1 N6 134.6(3) . 12_657 ?
N5 Dy1 N6 63.3(3) 12_657 12_657 ?
N1 Dy1 N6 156.0(3) . 12_657 ?
O1 Dy1 Cl1 92.9(3) . . ?
O2 Dy1 Cl1 150.0(3) 12_657 . ?
O3 Dy1 Cl1 90.0(5) . . ?
N2 Dy1 Cl1 86.7(3) . . ?
N5 Dy1 Cl1 146.5(4) 12_657 . ?
N1 Dy1 Cl1 81.7(4) . . ?
N6 Dy1 Cl1 83.3(4) 12_657 . ?
O1 Dy1 Cl2 150.3(3) . . ?
O2 Dy1 Cl2 78.8(3) 12_657 . ?
O4 Dy1 Cl2 99.0(12) . . ?
N2 Dy1 Cl2 139.1(3) . . ?
N5 Dy1 Cl2 77.1(3) 12_657 . ?
N1 Dy1 Cl2 79.5(3) . . ?
N6 Dy1 Cl2 86.2(3) 12_657 . ?
C8 S1 C11 91.9(6) . . ?
C21 S2 C20 91.2(5) . . ?
C7 O1 Dy1 122.1(7) . . ?
C23 O2 Dy1 121.6(7) . 11_667 ?
C1 N1 C5 119.0(12) . . ?
C1 N1 Dy1 121.9(9) . . ?
C5 N1 Dy1 118.8(8) . . ?
C6 N2 N3 116.8(10) . . ?
C6 N2 Dy1 123.8(8) . . ?
N3 N2 Dy1 118.9(7) . . ?
C7 N3 N2 107.6(9) . . ?
C23 N4 N5 110.9(9) . . ?
C24 N5 N4 120.0(9) . . ?
C24 N5 Dy1 121.8(8) . 11_667 ?
N4 N5 Dy1 118.2(6) . 11_667 ?
C29 N6 C25 118.9(10) . . ?
C29 N6 Dy1 124.7(8) . 11_667 ?
C25 N6 Dy1 116.3(7) . 11_667 ?
N1 C1 C2 120.0(15) . . ?
N1 C1 H1A 120.0 . . ?
C2 C1 H1A 120.0 . . ?
C3 C2 C1 121.1(16) . . ?
C3 C2 H2A 119.4 . . ?
C1 C2 H2A 119.4 . . ?
C2 C3 C4 118.1(16) . . ?
C2 C3 H3A 120.9 . . ?
C4 C3 H3A 120.9 . . ?
C3 C4 C5 118.8(15) . . ?
C3 C4 H4A 120.6 . . ?
C5 C4 H4A 120.6 . . ?
N1 C5 C4 122.6(13) . . ?
N1 C5 C6 115.9(13) . . ?
C4 C5 C6 121.4(12) . . ?
N2 C6 C5 117.2(11) . . ?
N2 C6 H6A 121.4 . . ?
C5 C6 H6A 121.4 . . ?
O1 C7 N3 126.6(10) . . ?
O1 C7 C8 118.0(10) . . ?
N3 C7 C8 115.4(10) . . ?
C9 C8 C7 125.4(10) . . ?
C9 C8 S1 111.4(9) . . ?
C7 C8 S1 123.2(9) . . ?
C8 C9 C10 113.5(10) . . ?
C8 C9 H9A 123.2 . . ?
C10 C9 H9A 123.2 . . ?
C11 C10 C9 111.3(11) . . ?
C11 C10 C13 127.2(12) . . ?
C9 C10 C13 121.5(11) . . ?
C10 C11 C12 127.6(12) . . ?
C10 C11 S1 111.9(9) . . ?
C12 C11 S1 120.3(9) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C17 C13 C10 127.4(12) . . ?
C17 C13 C14 112.8(12) . . ?
C10 C13 C14 119.6(13) . . ?
C13 C14 C15 103.3(12) . . ?
C13 C14 H14A 111.1 . . ?
C15 C14 H14A 111.1 . . ?
C13 C14 H14B 111.1 . . ?
C15 C14 H14B 111.1 . . ?
H14A C14 H14B 109.1 . . ?
C16 C15 C14 106.8(12) . . ?
C16 C15 H15A 110.4 . . ?
C14 C15 H15A 110.4 . . ?
C16 C15 H15B 110.4 . . ?
C14 C15 H15B 110.4 . . ?
H15A C15 H15B 108.6 . . ?
C17 C16 C15 103.6(12) . . ?
C17 C16 H16A 111.0 . . ?
C15 C16 H16A 111.0 . . ?
C17 C16 H16B 111.0 . . ?
C15 C16 H16B 111.0 . . ?
H16A C16 H16B 109.0 . . ?
C13 C17 C18 127.1(12) . . ?
C13 C17 C16 113.5(11) . . ?
C18 C17 C16 119.4(12) . . ?
C21 C18 C19 107.5(10) . . ?
C21 C18 C17 129.2(10) . . ?
C19 C18 C17 123.2(10) . . ?
C20 C19 C18 115.3(10) . . ?
C20 C19 H19A 122.3 . . ?
C18 C19 H19A 122.3 . . ?
C19 C20 C23 126.2(10) . . ?
C19 C20 S2 111.0(8) . . ?
C23 C20 S2 122.6(8) . . ?
C18 C21 C22 128.2(11) . . ?
C18 C21 S2 114.9(8) . . ?
C22 C21 S2 116.8(9) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O2 C23 N4 125.3(10) . . ?
O2 C23 C20 116.2(9) . . ?
N4 C23 C20 118.5(10) . . ?
N5 C24 C25 120.0(11) . . ?
N5 C24 H24A 120.0 . . ?
C25 C24 H24A 120.0 . . ?
N6 C25 C26 120.9(11) . . ?
N6 C25 C24 118.3(10) . . ?
C26 C25 C24 120.7(11) . . ?
C27 C26 C25 119.7(13) . . ?
C27 C26 H26A 120.2 . . ?
C25 C26 H26A 120.2 . . ?
C26 C27 C28 118.4(13) . . ?
C26 C27 H27A 120.8 . . ?
C28 C27 H27A 120.8 . . ?
C29 C28 C27 120.0(13) . . ?
C29 C28 H28A 120.0 . . ?
C27 C28 H28A 120.0 . . ?
N6 C29 C28 122.0(13) . . ?
N6 C29 H29A 119.0 . . ?
C28 C29 H29A 119.0 . . ?
C1S N1S C5S 120.0 . . ?
C2S C1S N1S 120.0 . . ?
C2S C1S H1SA 120.0 . . ?
N1S C1S H1SA 120.0 . . ?
C1S C2S C3S 120.0 . . ?
C1S C2S H2SA 120.0 . . ?
C3S C2S H2SA 120.0 . . ?
C4S C3S C2S 120.0 . . ?
C4S C3S H3SA 120.0 . . ?
C2S C3S H3SA 120.0 . . ?
C5S C4S C3S 120.0 . . ?
C5S C4S H4SA 120.0 . . ?
C3S C4S H4SA 120.0 . . ?
C4S C5S N1S 120.0 . . ?
C4S C5S H5SB 120.0 . . ?
N1S C5S H5SB 120.0 . . ?

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
O1W H1W N4 0.95(2) 2.00(4) 2.898(8) 158(10) . yes

_refine_diff_density_max         1.183
_refine_diff_density_min         -0.738
_refine_diff_density_rms         0.108



####################################################################### 
# 
# 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_JSU-S2-Tb
_database_code_depnum_ccdc_archive 'CCDC 1983840'
loop_
_audit_author_name
_audit_author_address
'Olivier Roubeau'
;Instituto de Ciencia de Materiales de Aragon (ICMA), CSIC and Universidad de Zaragoza
Spain
;
_audit_update_record             
;
2020-05-05 deposited with the CCDC.	2020-05-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C116 H104 Cl4 N24 O12 S8 Tb4, 12(C5 H5 N), 2(C H4 O), H2 O'
_chemical_formula_sum            'C178 H174 Cl4 N36 O15 S8 Tb4'
_chemical_formula_weight         4091.48

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0040 0.0020
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
H H 0.0000 0.0000
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
N N 0.0076 0.0040
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
O O 0.0132 0.0074
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
S S 0.1431 0.1480
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
Cl Cl 0.1697 0.1896
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
Tb Tb -0.1250 4.8273
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'

_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_H-M_alt        'I 41/a'
_space_group_name_Hall           '-I 4ad'

_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+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'

_cell_length_a                   36.8830(14)
_cell_length_b                   36.8830(14)
_cell_length_c                   14.7878(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     20116.7(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9875
_cell_measurement_theta_min      2.63
_cell_measurement_theta_max      26.79

_exptl_crystal_description       lath
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_F_000             8280
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    1.981
_shelx_estimated_absorpt_T_min   0.505
_shelx_estimated_absorpt_T_max   0.827
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.511
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_process_details   'SADABS-2014/4 - Bruker AXS'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.7749
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'Advanced Light Source station 11.3.1'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'Bruker D8 with PHOTON 100 detector'
_diffrn_measurement_method       'shutterless /f and /w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            118426
_diffrn_reflns_av_unetI/netI     0.0231
_diffrn_reflns_av_R_equivalents  0.0566
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.349
_diffrn_reflns_theta_max         26.851
_diffrn_reflns_theta_full        26.775
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             8314
_reflns_number_gt                6778
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'Bruker APEX 2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL & local programs'
_refine_special_details          
;All non-hydrogens were refined anisotropically, except the partial
 lattice methanol O1S-C20S and the disordered partial coordinated
 water oxygens O3 and O4. Hydrogens were placed
 geometrically on their carrier atom and refined with a riding model
 where possible where possible. The hydrogen on the central water O1W 
 was refined with its thermal parameter 1.5 times that of O1W and half
 occupancy, due to symmetry. The central water is indeed
 disordered by symmetry over two orientations corresponding to hydrogen
 bonds with the four nearby imine N4 generated by symmetry. 
 The coordinated water and chloride are mutually disordered over their
 relative positions (Cl1:O3 and O4:Cl2). This disorder is mirrored in the two
 positions of one of the lattice pyridine molecules, which probably
 form a hydrogen bond with O4. Due to this disorder O3 and O4 were
 refined isotropically and their hydrogens were omitted from the model
 as they could not be found nor fixed satisfactorily. Hydrogens on the
 partial lattice methanol molecule O1S-C20S were also omitted for the
 same reason. The lattice pyridine molecules as well as the ligand
 pyridine ring N1 > C5 were refined with displacement parameters restraints.
 At the end of the refinement, there remain some portions of
 the cell with only weak electron density peaks, that could not be
 modelled satisfactorily as solvent molecules. The corresponding
 void space was thus analyzed and taken into account with 
 PLATON/SQUEEZE that recovered a total of 328 electrons per cell
 over 4 voids of ca. 656 cubic angstroms (each with 82 electrons), 
 resulting in an improvement of ca 0.5% in R1.
 The electron content/void volume are reasonable for 2 diffuse pyridine
 solvent molecules per void, i.e. a total of 8 additional pyridine 
 molecules per cell, 2 per [Tb4] formula unit. This as well as the omitted
 hydrogens was reflected in the formula, weight etc.,SQUEEZE
;

_vrf_PLAT027_JSU-S2-Tb           
;
PROBLEM:  _diffrn_reflns_theta_full value (too) Low ......      26.77 Degree 
RESPONSE: Crystals systematically damaged upon removal from the
mother liquor, likely resulting from loss/disordering of lattice
solvent upon exposure to air. Even by fast manipulation and mounting in
the cold N2 stream, and using synchrotron radiation, this results in not
ideal diffraction, the present data being cut at 0.86 angstrom. The 
remaining large voids of diffuse electron density are also likely 
associated with this. Altogether this results in relatively poor values
of theta_full and theta_max.
;

_vrf_THETM01_JSU-S2-Tb           
;
PROBLEM:  The value of sine(theta_max)/wavelength is less than 0.590
            Calculated sin(theta_max)/wavelength =    0.5829 
RESPONSE: Crystals systematically damaged upon removal from the
mother liquor, likely resulting from loss/disordering of lattice
solvent upon exposure to air. Even by fast manipulation and mounting in
the cold N2 stream, and using synchrotron radiation, this results in not
ideal diffraction, the present data being cut at 0.86 angstrom. The 
remaining large voids of diffuse electron density are also likely 
associated with this. Altogether this results in relatively poor values
of theta_full and theta_max.
;

_vrf_PLAT201_JSU-S2-Tb           
;
PROBLEM:  Isotropic non-H Atoms in Main Residue(s) .......          1 Report
              O4
RESPONSE: The coordinated water and chloride ions are mutually disordered over
their respective positions (Cl1:O3 and O4:Cl2). Both partial oxygens O3 and O4
were refined isotropically due to this disorder.
;

_vrf_PLAT430_JSU-S2-Tb           
;
PROBLEM:  Short Inter D...A Contact  O4       ..N1S      .       2.70 Ang.  
                                        -1/4+y,7/4-x,-1/4+z  =      4_464 Check 
RESPONSE: The coordinated water and chloride ions are mutually disordered over
their respective positions (Cl1:O3 and O4:Cl2). Both partial oxygens O3 and O4
were refined isotropically due to this disorder. Their hydrogens were omitted 
from the model as they could not be found nor fixed satisfactorily. This short
contact likely corresponds to one of the hydrogen bonds these missing hydrogens
would participate in.
;

_vrf_FORMU01_JSU-S2-Tb           
;
PROBLEM:  There is a discrepancy between the atom counts in the            _chemical_formula_sum and _chemical_formula_moiety. 
RESPONSE: Hydrogens on the disordered coordinated water molecule O3:O4
and on the partial lattice methanol molecule were omitted in the
structural model but included in the formula. The formula also
includes the content of diffuse solvent voids taken into account
through PLATON/SQUEEZE and estimated to 8 pyridine molecules per
cell, 2 per formula unit.
;

_vrf_CELLZ01_JSU-S2-Tb           
;
PROBLEM:  Difference between formula and atom_site contents detected. 
RESPONSE: Hydrogens on the disordered coordinated water molecule O3:O4
and on the partial lattice methanol molecule were omitted in the
structural model but included in the formula. The formula also
includes the content of diffuse solvent voids taken into account
through PLATON/SQUEEZE and estimated to 8 pyridine molecules per
cell, 2 per formula unit.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0916P)²+392.9011P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8314
_refine_ls_number_parameters     532
_refine_ls_number_restraints     218
_refine_ls_R_factor_all          0.0913
_refine_ls_R_factor_gt           0.0722
_refine_ls_wR_factor_ref         0.2065
_refine_ls_wR_factor_gt          0.1849
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_restrained_S_all      1.048
_refine_ls_shift/su_max          0.002
_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 0.62715(2) 0.82138(2) 0.42550(3) 0.04935(19) Uani 1 1 d . . . . .
Cl1 Cl 0.67224(14) 0.87738(18) 0.3870(5) 0.0659(17) Uani 0.599(10) 1 d . U P A
1
Cl2 Cl 0.57389(15) 0.82416(17) 0.2963(4) 0.052(2) Uiso 0.401(10) 1 d . U P A 1
S1 S 0.71752(6) 0.78252(7) 0.74308(16) 0.0540(6) Uani 1 1 d . . . . .
S2 S 0.55476(7) 0.77656(6) 0.80776(15) 0.0533(6) Uani 1 1 d . . . . .
O1 O 0.64416(15) 0.82023(16) 0.5736(4) 0.0509(14) Uani 1 1 d . . . . .
O2 O 0.48927(19) 0.85963(15) 0.8360(4) 0.0594(17) Uani 1 1 d . . . . .
O3 O 0.6723(6) 0.8659(5) 0.3662(13) 0.036(5) Uiso 0.401(10) 1 d . U P A 2
O4 O 0.5847(3) 0.8433(3) 0.3136(7) 0.048(3) Uiso 0.599(10) 1 d . U P A 2
N1 N 0.6597(2) 0.7909(3) 0.2906(6) 0.073(3) Uani 1 1 d . . . . .
N2 N 0.68155(16) 0.78341(19) 0.4622(5) 0.0436(16) Uani 1 1 d . . . . .
N3 N 0.69274(17) 0.78097(19) 0.5504(5) 0.0449(16) Uani 1 1 d . . . . .
N4 N 0.48279(18) 0.80910(16) 0.7455(4) 0.0405(15) Uani 1 1 d D . . . .
N5 N 0.44743(18) 0.82055(16) 0.7402(4) 0.0386(14) Uani 1 1 d . . . . .
N6 N 0.37748(19) 0.84156(18) 0.7404(5) 0.0501(17) Uani 1 1 d . . . . .
C1 C 0.6491(3) 0.7952(5) 0.2061(8) 0.101(3) Uani 1 1 d . U . . .
H1A H 0.631765 0.813462 0.192420 0.121 Uiso 1 1 calc R U . . .
C2 C 0.6629(4) 0.7736(5) 0.1357(9) 0.106(3) Uani 1 1 d . U . . .
H2A H 0.653849 0.775841 0.075778 0.127 Uiso 1 1 calc R U . . .
C3 C 0.6892(4) 0.7496(5) 0.1556(8) 0.103(3) Uani 1 1 d . U . . .
H3A H 0.699741 0.735470 0.108685 0.124 Uiso 1 1 calc R U . . .
C4 C 0.7010(3) 0.7452(4) 0.2433(8) 0.096(3) Uani 1 1 d . U . . .
H4A H 0.719024 0.727698 0.257932 0.115 Uiso 1 1 calc R U . . .
C5 C 0.6863(2) 0.7666(3) 0.3084(6) 0.064(3) Uani 1 1 d . . . . .
C6 C 0.6979(2) 0.7641(3) 0.4032(7) 0.057(2) Uani 1 1 d . . . . .
H6A H 0.717239 0.748526 0.420213 0.069 Uiso 1 1 calc R U . . .
C7 C 0.6715(2) 0.8015(2) 0.6011(6) 0.0444(19) Uani 1 1 d . . . . .
C8 C 0.6802(2) 0.8037(2) 0.6969(6) 0.047(2) Uani 1 1 d . . . . .
C9 C 0.6620(2) 0.8223(2) 0.7607(7) 0.055(2) Uani 1 1 d . . . . .
H9A H 0.640795 0.835983 0.747838 0.065 Uiso 1 1 calc R U . . .
C10 C 0.6771(2) 0.8200(3) 0.8481(7) 0.057(2) Uani 1 1 d . . . . .
C11 C 0.7078(2) 0.7988(3) 0.8493(7) 0.058(2) Uani 1 1 d . . . . .
C12 C 0.7309(3) 0.7880(3) 0.9272(6) 0.067(3) Uani 1 1 d . . . . .
H12B H 0.750860 0.772719 0.905717 0.101 Uiso 1 1 calc R U . . .
H12C H 0.740716 0.809694 0.956379 0.101 Uiso 1 1 calc R U . . .
H12D H 0.716253 0.774333 0.970869 0.101 Uiso 1 1 calc R U . . .
C13 C 0.6607(3) 0.8373(3) 0.9282(8) 0.079(3) Uani 1 1 d . U . . .
C14 C 0.6827(3) 0.8589(4) 0.9932(9) 0.092(3) Uani 1 1 d . U . . .
H14A H 0.696899 0.877744 0.961391 0.111 Uiso 1 1 calc R U . . .
H14B H 0.699475 0.843128 1.027568 0.111 Uiso 1 1 calc R U . . .
C15 C 0.6546(3) 0.8760(4) 1.0557(9) 0.097(3) Uani 1 1 d . U . . .
H15A H 0.659389 0.868973 1.119191 0.116 Uiso 1 1 calc R U . . .
H15B H 0.655663 0.902765 1.051205 0.116 Uiso 1 1 calc R U . . .
C16 C 0.6175(3) 0.8623(4) 1.0259(9) 0.094(3) Uani 1 1 d . U . . .
H16A H 0.605636 0.848427 1.075026 0.113 Uiso 1 1 calc R U . . .
H16B H 0.601577 0.882696 1.008248 0.113 Uiso 1 1 calc R U . . .
C17 C 0.6252(3) 0.8384(3) 0.9469(7) 0.072(3) Uani 1 1 d . . . . .
C18 C 0.5952(3) 0.8208(2) 0.8954(6) 0.056(2) Uani 1 1 d . . . . .
C19 C 0.5621(3) 0.8397(2) 0.8749(6) 0.055(2) Uani 1 1 d . . . . .
H19A H 0.557495 0.863811 0.893951 0.066 Uiso 1 1 calc R U . . .
C20 C 0.5378(3) 0.8197(2) 0.8252(6) 0.049(2) Uani 1 1 d . . . . .
C21 C 0.5944(3) 0.7860(2) 0.8646(6) 0.050(2) Uani 1 1 d . . . . .
C23 C 0.6217(3) 0.7562(3) 0.8761(7) 0.063(3) Uani 1 1 d . . . . .
H23A H 0.613058 0.734253 0.845458 0.094 Uiso 1 1 calc R U . . .
H23B H 0.644940 0.763633 0.849784 0.094 Uiso 1 1 calc R U . . .
H23C H 0.625002 0.751079 0.940658 0.094 Uiso 1 1 calc R U . . .
C24 C 0.5013(3) 0.8304(2) 0.8015(6) 0.049(2) Uani 1 1 d . . . . .
C25 C 0.4257(2) 0.8026(2) 0.6901(5) 0.0421(18) Uani 1 1 d . . . . .
H25A H 0.434144 0.783002 0.654022 0.051 Uiso 1 1 calc R U . . .
C26 C 0.3875(2) 0.8129(2) 0.6899(6) 0.047(2) Uani 1 1 d . . . . .
C27 C 0.3628(3) 0.7927(3) 0.6392(7) 0.059(2) Uani 1 1 d . . . . .
H27A H 0.370776 0.772859 0.603581 0.071 Uiso 1 1 calc R U . . .
C28 C 0.3267(3) 0.8021(3) 0.6417(9) 0.074(3) Uani 1 1 d . . . . .
H28A H 0.309429 0.788681 0.607944 0.089 Uiso 1 1 calc R U . . .
C29 C 0.3161(3) 0.8309(3) 0.6930(9) 0.077(3) Uani 1 1 d . . . . .
H29A H 0.291272 0.837685 0.695967 0.092 Uiso 1 1 calc R U . . .
C30 C 0.3423(3) 0.8504(3) 0.7414(8) 0.065(3) Uani 1 1 d . . . . .
H30A H 0.334829 0.870659 0.776287 0.078 Uiso 1 1 calc R U . . .
O1W O 0.500000 0.750000 0.625000 0.070(4) Uani 1 4 d DS T P . .
H1W H 0.492(6) 0.765(3) 0.673(9) 0.105 Uiso 0.5 1 d D U P . .
N1S N 0.83488(17) 0.8300(3) 0.5305(7) 0.115(3) Uani 1 1 d G U . . .
C1S C 0.8065(2) 0.8096(3) 0.5662(6) 0.101(3) Uani 1 1 d G U . . .
H1SA H 0.811207 0.792194 0.612011 0.121 Uiso 1 1 calc R U . . .
C2S C 0.77140(19) 0.8148(3) 0.5348(7) 0.102(3) Uani 1 1 d G U . . .
H2SA H 0.752041 0.800938 0.559221 0.122 Uiso 1 1 calc R U . . .
C3S C 0.7646(2) 0.8403(3) 0.4678(8) 0.130(4) Uani 1 1 d G U . . .
H3SA H 0.740564 0.843889 0.446332 0.156 Uiso 1 1 calc R U . . .
C4S C 0.7929(3) 0.8607(3) 0.4321(8) 0.152(4) Uani 1 1 d G U . . .
H4SA H 0.788254 0.878096 0.386232 0.183 Uiso 1 1 calc R U . . .
C5S C 0.8281(2) 0.8555(3) 0.4634(8) 0.145(4) Uani 1 1 d G U . . .
H5SA H 0.847421 0.869353 0.439021 0.174 Uiso 1 1 calc R U . . .
N2S N 0.7280(6) 0.6776(3) 0.3669(12) 0.206(7) Uani 1 1 d G U . . .
C6S C 0.6986(5) 0.6610(6) 0.4085(11) 0.213(7) Uani 1 1 d G U . . .
H6SA H 0.681931 0.675067 0.442781 0.255 Uiso 1 1 calc R U . . .
C7S C 0.6935(5) 0.6238(6) 0.4000(13) 0.232(7) Uani 1 1 d G U . . .
H7SA H 0.673339 0.612469 0.428507 0.278 Uiso 1 1 calc R U . . .
C8S C 0.7178(7) 0.6032(4) 0.3499(14) 0.235(7) Uani 1 1 d G U . . .
H8SA H 0.714304 0.577789 0.344136 0.282 Uiso 1 1 calc R U . . .
C9S C 0.7472(6) 0.6198(6) 0.3083(12) 0.224(7) Uani 1 1 d G U . . .
H9SA H 0.763861 0.605707 0.274041 0.268 Uiso 1 1 calc R U . . .
C10S C 0.7523(5) 0.6570(6) 0.3168(11) 0.206(7) Uani 1 1 d G U . . .
H10A H 0.772453 0.668305 0.288315 0.248 Uiso 1 1 calc R U . . .
N3S N 0.5550(3) 0.8022(3) 0.2009(7) 0.062(3) Uani 0.5 1 d G U P B -2
C11S C 0.5344(4) 0.8170(3) 0.1314(8) 0.066(3) Uani 0.5 1 d G U P B -2
H11A H 0.524804 0.840817 0.137212 0.079 Uiso 0.5 1 calc R U P B -2
C12S C 0.5280(4) 0.7971(4) 0.0533(7) 0.071(3) Uani 0.5 1 d G U P B -2
H12A H 0.513884 0.807204 0.005801 0.085 Uiso 0.5 1 calc R U P B -2
C13S C 0.5421(4) 0.7623(3) 0.0448(7) 0.071(3) Uani 0.5 1 d G U P B -2
H13A H 0.537644 0.748661 -0.008599 0.085 Uiso 0.5 1 calc R U P B -2
C14S C 0.5627(4) 0.7475(3) 0.1143(9) 0.069(3) Uani 0.5 1 d G U P B -2
H14C H 0.572324 0.723732 0.108412 0.083 Uiso 0.5 1 calc R U P B -2
C15S C 0.5692(3) 0.7675(3) 0.1923(8) 0.064(3) Uani 0.5 1 d G U P B -2
H15C H 0.583243 0.757344 0.239824 0.076 Uiso 0.5 1 calc R U P B -2
C20S C 0.7054(12) 0.8983(7) 0.642(3) 0.146(11) Uani 0.5 1 d . U P . .
O1S O 0.7419(10) 0.9005(7) 0.731(2) 0.196(11) Uani 0.5 1 d . U 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
Tb1 O1 2.278(6) . ?
Tb1 O2 2.335(7) 15_566 ?
Tb1 O4 2.418(10) . ?
Tb1 O3 2.50(2) . ?
Tb1 N2 2.506(6) . ?
Tb1 N5 2.529(6) 15_566 ?
Tb1 N1 2.585(9) . ?
Tb1 N6 2.613(7) 15_566 ?
Tb1 Cl1 2.712(5) . ?
Tb1 Cl2 2.742(6) . ?
S1 C11 1.719(10) . ?
S1 C8 1.722(8) . ?
S2 C21 1.723(9) . ?
S2 C20 1.728(8) . ?
O1 C7 1.289(10) . ?
O2 C24 1.274(10) . ?
N1 C1 1.319(14) . ?
N1 C5 1.353(13) . ?
N2 C6 1.278(12) . ?
N2 N3 1.371(9) . ?
N3 C7 1.322(11) . ?
N4 C24 1.330(10) . ?
N4 N5 1.373(9) . ?
N5 C25 1.277(10) . ?
N6 C30 1.337(12) . ?
N6 C26 1.346(11) . ?
C1 C2 1.407(19) . ?
C1 H1A 0.9500 . ?
C2 C3 1.348(19) . ?
C2 H2A 0.9500 . ?
C3 C4 1.378(17) . ?
C3 H3A 0.9500 . ?
C4 C5 1.359(16) . ?
C4 H4A 0.9500 . ?
C5 C6 1.469(13) . ?
C6 H6A 0.9500 . ?
C7 C8 1.455(12) . ?
C8 C9 1.347(13) . ?
C9 C10 1.410(13) . ?
C9 H9A 0.9500 . ?
C10 C11 1.375(13) . ?
C10 C13 1.475(14) . ?
C11 C12 1.487(13) . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C12 H12D 0.9800 . ?
C13 C17 1.337(16) . ?
C13 C14 1.489(15) . ?
C14 C15 1.523(17) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.525(17) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C17 1.490(14) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C18 1.494(14) . ?
C18 C21 1.360(12) . ?
C18 C19 1.437(12) . ?
C19 C20 1.375(12) . ?
C19 H19A 0.9500 . ?
C20 C24 1.443(13) . ?
C21 C23 1.503(12) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C25 C26 1.458(12) . ?
C25 H25A 0.9500 . ?
C26 C27 1.395(13) . ?
C27 C28 1.375(14) . ?
C27 H27A 0.9500 . ?
C28 C29 1.363(16) . ?
C28 H28A 0.9500 . ?
C29 C30 1.401(15) . ?
C29 H29A 0.9500 . ?
C30 H30A 0.9500 . ?
O1W H1W 0.95(2) . ?
N1S C1S 1.3900 . ?
N1S C5S 1.3900 . ?
C1S C2S 1.3900 . ?
C1S H1SA 0.9500 . ?
C2S C3S 1.3900 . ?
C2S H2SA 0.9500 . ?
C3S C4S 1.3900 . ?
C3S H3SA 0.9500 . ?
C4S C5S 1.3900 . ?
C4S H4SA 0.9500 . ?
C5S H5SA 0.9500 . ?
N2S C6S 1.3900 . ?
N2S C10S 1.3900 . ?
C6S C7S 1.3900 . ?
C6S H6SA 0.9500 . ?
C7S C8S 1.3900 . ?
C7S H7SA 0.9500 . ?
C8S C9S 1.3900 . ?
C8S H8SA 0.9500 . ?
C9S C10S 1.3900 . ?
C9S H9SA 0.9500 . ?
C10S H10A 0.9500 . ?
N3S C11S 1.3900 . ?
N3S C15S 1.3900 . ?
C11S C12S 1.3900 . ?
C11S H11A 0.9500 . ?
C12S C13S 1.3900 . ?
C12S H12A 0.9500 . ?
C13S C14S 1.3900 . ?
C13S H13A 0.9500 . ?
C14S C15S 1.3900 . ?
C14S H14C 0.9500 . ?
C15S H15C 0.9500 . ?
C20S O1S 1.88(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
O1 Tb1 O2 97.4(2) . 15_566 ?
O1 Tb1 O4 147.4(3) . . ?
O2 Tb1 O4 95.2(3) 15_566 . ?
O1 Tb1 O3 99.5(5) . . ?
O2 Tb1 O3 142.0(5) 15_566 . ?
O4 Tb1 O3 88.4(5) . . ?
O1 Tb1 N2 63.9(2) . . ?
O2 Tb1 N2 72.7(2) 15_566 . ?
O4 Tb1 N2 148.6(3) . . ?
O3 Tb1 N2 84.8(5) . . ?
O1 Tb1 N5 75.4(2) . 15_566 ?
O2 Tb1 N5 62.9(2) 15_566 15_566 ?
O4 Tb1 N5 83.9(3) . 15_566 ?
O3 Tb1 N5 154.7(5) . 15_566 ?
N2 Tb1 N5 113.6(2) . 15_566 ?
O1 Tb1 N1 127.3(2) . . ?
O2 Tb1 N1 69.9(3) 15_566 . ?
O4 Tb1 N1 85.3(3) . . ?
O3 Tb1 N1 72.8(5) . . ?
N2 Tb1 N1 63.4(2) . . ?
N5 Tb1 N1 130.1(3) 15_566 . ?
O1 Tb1 N6 72.2(2) . 15_566 ?
O2 Tb1 N6 126.0(2) 15_566 15_566 ?
O4 Tb1 N6 76.1(3) . 15_566 ?
O3 Tb1 N6 91.6(5) . 15_566 ?
N2 Tb1 N6 134.6(2) . 15_566 ?
N5 Tb1 N6 63.2(2) 15_566 15_566 ?
N1 Tb1 N6 156.1(2) . 15_566 ?
O1 Tb1 Cl1 92.7(2) . . ?
O2 Tb1 Cl1 152.1(2) 15_566 . ?
N2 Tb1 Cl1 88.86(19) . . ?
N5 Tb1 Cl1 145.0(2) 15_566 . ?
N1 Tb1 Cl1 83.3(3) . . ?
N6 Tb1 Cl1 81.9(2) 15_566 . ?
O1 Tb1 Cl2 150.19(18) . . ?
O2 Tb1 Cl2 77.7(2) 15_566 . ?
N2 Tb1 Cl2 138.2(2) . . ?
N5 Tb1 Cl2 76.24(18) 15_566 . ?
N1 Tb1 Cl2 79.1(2) . . ?
N6 Tb1 Cl2 86.8(2) 15_566 . ?
Cl1 Tb1 Cl2 105.34(18) . . ?
C11 S1 C8 92.2(4) . . ?
C21 S2 C20 92.8(4) . . ?
C7 O1 Tb1 122.0(5) . . ?
C24 O2 Tb1 122.7(6) . 12_767 ?
C1 N1 C5 118.6(10) . . ?
C1 N1 Tb1 122.7(7) . . ?
C5 N1 Tb1 118.3(6) . . ?
C6 N2 N3 118.1(7) . . ?
C6 N2 Tb1 122.8(6) . . ?
N3 N2 Tb1 118.9(5) . . ?
C7 N3 N2 108.9(6) . . ?
C24 N4 N5 110.1(7) . . ?
C25 N5 N4 118.0(6) . . ?
C25 N5 Tb1 122.9(5) . 12_767 ?
N4 N5 Tb1 119.1(4) . 12_767 ?
C30 N6 C26 117.7(8) . . ?
C30 N6 Tb1 124.9(6) . 12_767 ?
C26 N6 Tb1 117.4(6) . 12_767 ?
N1 C1 C2 121.7(12) . . ?
N1 C1 H1A 119.1 . . ?
C2 C1 H1A 119.1 . . ?
C3 C2 C1 118.1(13) . . ?
C3 C2 H2A 120.9 . . ?
C1 C2 H2A 120.9 . . ?
C2 C3 C4 120.7(13) . . ?
C2 C3 H3A 119.6 . . ?
C4 C3 H3A 119.6 . . ?
C5 C4 C3 118.1(12) . . ?
C5 C4 H4A 120.9 . . ?
C3 C4 H4A 120.9 . . ?
N1 C5 C4 122.6(10) . . ?
N1 C5 C6 116.0(9) . . ?
C4 C5 C6 121.4(10) . . ?
N2 C6 C5 118.6(8) . . ?
N2 C6 H6A 120.7 . . ?
C5 C6 H6A 120.7 . . ?
O1 C7 N3 126.2(8) . . ?
O1 C7 C8 116.8(8) . . ?
N3 C7 C8 116.9(7) . . ?
C9 C8 C7 126.9(7) . . ?
C9 C8 S1 110.6(6) . . ?
C7 C8 S1 122.5(6) . . ?
C8 C9 C10 114.4(8) . . ?
C8 C9 H9A 122.8 . . ?
C10 C9 H9A 122.8 . . ?
C11 C10 C9 111.8(9) . . ?
C11 C10 C13 125.0(9) . . ?
C9 C10 C13 123.2(8) . . ?
C10 C11 C12 129.3(9) . . ?
C10 C11 S1 111.0(7) . . ?
C12 C11 S1 119.7(7) . . ?
C11 C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C12 H12D 109.5 . . ?
H12B C12 H12D 109.5 . . ?
H12C C12 H12D 109.5 . . ?
C17 C13 C10 125.5(9) . . ?
C17 C13 C14 112.4(10) . . ?
C10 C13 C14 121.8(11) . . ?
C13 C14 C15 104.1(10) . . ?
C13 C14 H14A 110.9 . . ?
C15 C14 H14A 110.9 . . ?
C13 C14 H14B 110.9 . . ?
C15 C14 H14B 110.9 . . ?
H14A C14 H14B 109.0 . . ?
C16 C15 C14 107.3(9) . . ?
C16 C15 H15A 110.3 . . ?
C14 C15 H15A 110.3 . . ?
C16 C15 H15B 110.3 . . ?
C14 C15 H15B 110.3 . . ?
H15A C15 H15B 108.5 . . ?
C17 C16 C15 104.5(10) . . ?
C17 C16 H16A 110.9 . . ?
C15 C16 H16A 110.9 . . ?
C17 C16 H16B 110.9 . . ?
C15 C16 H16B 110.9 . . ?
H16A C16 H16B 108.9 . . ?
C13 C17 C16 111.6(10) . . ?
C13 C17 C18 127.3(9) . . ?
C16 C17 C18 121.0(10) . . ?
C21 C18 C19 111.6(8) . . ?
C21 C18 C17 126.6(8) . . ?
C19 C18 C17 121.8(8) . . ?
C20 C19 C18 114.1(8) . . ?
C20 C19 H19A 123.0 . . ?
C18 C19 H19A 123.0 . . ?
C19 C20 C24 126.2(8) . . ?
C19 C20 S2 109.6(6) . . ?
C24 C20 S2 123.6(6) . . ?
C18 C21 C23 129.7(8) . . ?
C18 C21 S2 111.8(7) . . ?
C23 C21 S2 118.4(7) . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
O2 C24 N4 124.7(8) . . ?
O2 C24 C20 117.4(8) . . ?
N4 C24 C20 118.0(7) . . ?
N5 C25 C26 118.1(7) . . ?
N5 C25 H25A 120.9 . . ?
C26 C25 H25A 120.9 . . ?
N6 C26 C27 122.4(8) . . ?
N6 C26 C25 118.0(8) . . ?
C27 C26 C25 119.5(8) . . ?
C28 C27 C26 119.0(9) . . ?
C28 C27 H27A 120.5 . . ?
C26 C27 H27A 120.5 . . ?
C29 C28 C27 119.3(10) . . ?
C29 C28 H28A 120.4 . . ?
C27 C28 H28A 120.4 . . ?
C28 C29 C30 119.0(10) . . ?
C28 C29 H29A 120.5 . . ?
C30 C29 H29A 120.5 . . ?
N6 C30 C29 122.7(9) . . ?
N6 C30 H30A 118.7 . . ?
C29 C30 H30A 118.7 . . ?
C1S N1S C5S 120.0 . . ?
N1S C1S C2S 120.0 . . ?
N1S C1S H1SA 120.0 . . ?
C2S C1S H1SA 120.0 . . ?
C3S C2S C1S 120.0 . . ?
C3S C2S H2SA 120.0 . . ?
C1S C2S H2SA 120.0 . . ?
C2S C3S C4S 120.0 . . ?
C2S C3S H3SA 120.0 . . ?
C4S C3S H3SA 120.0 . . ?
C5S C4S C3S 120.0 . . ?
C5S C4S H4SA 120.0 . . ?
C3S C4S H4SA 120.0 . . ?
C4S C5S N1S 120.0 . . ?
C4S C5S H5SA 120.0 . . ?
N1S C5S H5SA 120.0 . . ?
C6S N2S C10S 120.0 . . ?
C7S C6S N2S 120.0 . . ?
C7S C6S H6SA 120.0 . . ?
N2S C6S H6SA 120.0 . . ?
C6S C7S C8S 120.0 . . ?
C6S C7S H7SA 120.0 . . ?
C8S C7S H7SA 120.0 . . ?
C9S C8S C7S 120.0 . . ?
C9S C8S H8SA 120.0 . . ?
C7S C8S H8SA 120.0 . . ?
C8S C9S C10S 120.0 . . ?
C8S C9S H9SA 120.0 . . ?
C10S C9S H9SA 120.0 . . ?
C9S C10S N2S 120.0 . . ?
C9S C10S H10A 120.0 . . ?
N2S C10S H10A 120.0 . . ?
C11S N3S C15S 120.0 . . ?
C12S C11S N3S 120.0 . . ?
C12S C11S H11A 120.0 . . ?
N3S C11S H11A 120.0 . . ?
C13S C12S C11S 120.0 . . ?
C13S C12S H12A 120.0 . . ?
C11S C12S H12A 120.0 . . ?
C12S C13S C14S 120.0 . . ?
C12S C13S H13A 120.0 . . ?
C14S C13S H13A 120.0 . . ?
C15S C14S C13S 120.0 . . ?
C15S C14S H14C 120.0 . . ?
C13S C14S H14C 120.0 . . ?
C14S C15S N3S 120.0 . . ?
C14S C15S H15C 120.0 . . ?
N3S C15S H15C 120.0 . . ?

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
O1W H1W N4 0.95(2) 1.98(4) 2.886(6) 159(10) . yes

_refine_diff_density_max         1.661
_refine_diff_density_min         -1.662
_refine_diff_density_rms         0.139



