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

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

data_final_a
_database_code_depnum_ccdc_archive 'CCDC 1544440'
_audit_update_record             
;
2017-04-17 deposited with the CCDC.
2017-08-23 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT077_final_a             
;
PROBLEM: Unitcell contains non-integer number of atoms ..     Please Check
RESPONSE: Due to partially occupied water molecule
;
# Added during the CSD deposition process: Monday 17 April 2017 03:18 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C60 H44 La2 N6 O14 S6, 0.794(H2 O)'
_chemical_formula_sum            'C60 H45.59 La2 N6 O14.79 S6'
_chemical_formula_weight         1557.48

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
La La -0.2871 2.4523 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   12.0926(5)
_cell_length_b                   25.9263(10)
_cell_length_c                   9.6761(4)
_cell_angle_alpha                90
_cell_angle_beta                 98.3430(10)
_cell_angle_gamma                90
_cell_volume                     3001.5(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9850
_cell_measurement_theta_min      2.64
_cell_measurement_theta_max      27.11
_exptl_crystal_description       rhombus
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.723
_exptl_crystal_F_000             1552
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.534
_exptl_crystal_size_mid          0.247
_exptl_crystal_size_min          0.180
_exptl_absorpt_coefficient_mu    1.686
_shelx_estimated_absorpt_T_min   0.466
_shelx_estimated_absorpt_T_max   0.751
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.63910
_exptl_absorpt_correction_T_max  0.80621
_exptl_absorpt_process_details   'SADABS V2016/2 (Bruker, 2014)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_monochromator  'multilayer mirrors'
_diffrn_measurement_device       'Bruker D8 Quest/Photon 100'
_diffrn_measurement_method       'profile data from φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            32897
_diffrn_reflns_av_unetI/netI     0.0279
_diffrn_reflns_av_R_equivalents  0.0309
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.316
_diffrn_reflns_theta_max         27.130
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             6632
_reflns_number_gt                5839
_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.
 
 _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       'APEX2 V2014.9-0 (Bruker, 2014)'
_computing_cell_refinement       'SAINT V8.37A (Bruker, 2005)'
_computing_data_reduction        
; 
SAINT V8.37A, XPREP v2014/2, SADABS V2016/2 (Bruker, 2014) 
;
_computing_structure_solution    'SHELX-2014-5 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELX-2014-7 (Sheldrick, 2015)'
_computing_molecular_graphics    'SHELXLE v817 (Hubschle, 2011)'
_computing_publication_material  'XCIF V2014-2 (Bruker, 2014)'

_refine_special_details          
; 
Structure was phased by direct methods (Sheldrick, 2015).  Systematic 
conditions suggested the ambiguous space group.  The space group choice 
was confirmed by successful convergence of the full-matrix least-squares 
refinement on F².  The final map had no significant features.  A final 
analysis of variance between observed and calculated structure factors 
showed little dependence on amplitude and resolution. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0135P)²+2.7840P] 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         6632
_refine_ls_number_parameters     539
_refine_ls_number_restraints     1198
_refine_ls_R_factor_all          0.0322
_refine_ls_R_factor_gt           0.0246
_refine_ls_wR_factor_ref         0.0469
_refine_ls_wR_factor_gt          0.0453
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_restrained_S_all      1.022
_refine_ls_shift/su_max          0.005
_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
La1 La 0.51810(2) 0.59831(2) 0.59712(2) 0.01034(4) Uani 1 1 d . U . . .
O7 O 0.56392(13) 0.57100(6) 0.35610(17) 0.0215(4) Uani 1 1 d D U . . .
H7A H 0.6324(10) 0.5771(10) 0.349(3) 0.032 Uiso 1 1 d D U . . .
H7B H 0.534(2) 0.5459(7) 0.308(2) 0.032 Uiso 1 1 d D U . . .
O8 O 0.5004(4) 0.47124(16) 0.9011(4) 0.0264(15) Uani 0.397(6) 1 d D . P . .
H8A H 0.465(5) 0.5002(14) 0.891(7) 0.040 Uiso 0.397(6) 1 d D U P . .
H8B H 0.517(6) 0.467(3) 0.9898(16) 0.040 Uiso 0.397(6) 1 d D U P . .
N1 N 0.41255(14) 0.66946(6) 0.42531(18) 0.0135(4) Uani 1 1 d . U . . .
N2 N 0.55100(14) 0.69988(6) 0.65794(18) 0.0123(4) Uani 1 1 d . U . . .
N3 N 0.63043(16) 0.62501(7) 0.84405(19) 0.0182(4) Uani 1 1 d . U . . .
C1 C 0.34148(18) 0.65372(8) 0.3136(2) 0.0180(5) Uani 1 1 d . U . . .
H1 H 0.3352 0.6178 0.2954 0.022 Uiso 1 1 calc R U . . .
C2 C 0.27713(19) 0.68687(9) 0.2236(3) 0.0215(5) Uani 1 1 d . U . . .
H2 H 0.2282 0.6741 0.1455 0.026 Uiso 1 1 calc R U . . .
C3 C 0.28591(19) 0.73915(9) 0.2504(2) 0.0208(5) Uani 1 1 d . U . . .
H3 H 0.2436 0.7631 0.1900 0.025 Uiso 1 1 calc R U . . .
C4 C 0.35696(18) 0.75617(8) 0.3659(2) 0.0188(5) Uani 1 1 d . U . . .
H4 H 0.3629 0.7920 0.3867 0.023 Uiso 1 1 calc R U . . .
C5 C 0.41980(17) 0.72056(8) 0.4518(2) 0.0131(4) Uani 1 1 d . U . . .
C6 C 0.50056(17) 0.73717(8) 0.5749(2) 0.0130(4) Uani 1 1 d . U . . .
C7 C 0.52316(19) 0.78930(8) 0.6019(2) 0.0185(5) Uani 1 1 d . U . . .
H7 H 0.4872 0.8150 0.5411 0.022 Uiso 1 1 calc R U . . .
C8 C 0.5977(2) 0.80332(9) 0.7169(3) 0.0226(5) Uani 1 1 d . U . . .
H8 H 0.6134 0.8387 0.7370 0.027 Uiso 1 1 calc R U . . .
C9 C 0.64912(19) 0.76529(9) 0.8022(2) 0.0208(5) Uani 1 1 d . U . . .
H9 H 0.7006 0.7741 0.8824 0.025 Uiso 1 1 calc R U . . .
C10 C 0.62515(17) 0.71382(8) 0.7702(2) 0.0161(5) Uani 1 1 d . U . . .
C11 C 0.67701(18) 0.67201(9) 0.8628(2) 0.0171(5) Uani 1 1 d . U . . .
C12 C 0.76735(19) 0.68079(11) 0.9670(2) 0.0257(6) Uani 1 1 d . U . . .
H12 H 0.8020 0.7137 0.9761 0.031 Uiso 1 1 calc R U . . .
C13 C 0.8061(2) 0.64148(11) 1.0566(3) 0.0320(6) Uani 1 1 d . U . . .
H13 H 0.8667 0.6473 1.1290 0.038 Uiso 1 1 calc R U . . .
C14 C 0.7568(2) 0.59394(11) 1.0409(3) 0.0320(6) Uani 1 1 d . U . . .
H14 H 0.7811 0.5665 1.1031 0.038 Uiso 1 1 calc R U . . .
C15 C 0.6703(2) 0.58695(10) 0.9317(2) 0.0271(6) Uani 1 1 d . U . . .
H15 H 0.6377 0.5537 0.9181 0.033 Uiso 1 1 calc R U . . .
O1 O 0.41707(13) 0.56080(6) 0.80329(17) 0.0234(4) Uani 1 1 d . U . . .
O2 O 0.35141(12) 0.63379(6) 0.70302(16) 0.0177(3) Uani 1 1 d . U . . .
C16 C 0.34554(17) 0.59672(8) 0.7858(2) 0.0165(4) Uani 1 1 d D U . . .
S1 S 0.24262(13) 0.55658(7) 1.00331(18) 0.0178(3) Uani 0.692(3) 1 d D U P A 1
C17 C 0.2485(13) 0.5971(9) 0.865(2) 0.0138(9) Uani 0.692(3) 1 d D U P A 1
C18 C 0.1554(7) 0.6277(3) 0.8426(9) 0.0182(14) Uani 0.692(3) 1 d D U P A 1
H18 H 0.1444 0.6527 0.7702 0.022 Uiso 0.692(3) 1 calc R U P A 1
C19 C 0.0774(6) 0.6193(3) 0.9348(10) 0.0162(10) Uani 0.692(3) 1 d D U P A 1
H19 H 0.0088 0.6373 0.9324 0.019 Uiso 0.692(3) 1 calc R U P A 1
C20 C 0.1145(6) 0.5817(3) 1.0277(9) 0.0176(11) Uani 0.692(3) 1 d D U P A 1
H20 H 0.0741 0.5703 1.0992 0.021 Uiso 0.692(3) 1 calc R U P A 1
S1A S 0.1447(4) 0.6360(2) 0.8165(5) 0.0160(8) Uani 0.308(3) 1 d D U P A 2
C17A C 0.253(3) 0.595(2) 0.870(5) 0.0154(19) Uani 0.308(3) 1 d D U P A 2
C18A C 0.2341(11) 0.5659(6) 0.9822(16) 0.019(2) Uani 0.308(3) 1 d D U P A 2
H18A H 0.2867 0.5414 1.0253 0.023 Uiso 0.308(3) 1 calc R U P A 2
C19A C 0.1311(14) 0.5751(8) 1.029(2) 0.018(2) Uani 0.308(3) 1 d D U P A 2
H19A H 0.1051 0.5582 1.1051 0.021 Uiso 0.308(3) 1 calc R U P A 2
C20A C 0.0750(14) 0.6119(8) 0.947(2) 0.017(2) Uani 0.308(3) 1 d D U P A 2
H20A H 0.0029 0.6236 0.9607 0.021 Uiso 0.308(3) 1 calc R U P A 2
O3 O 0.37397(12) 0.47970(6) 0.34443(16) 0.0190(3) Uani 1 1 d . U . . .
O4 O 0.36175(12) 0.54757(6) 0.48198(17) 0.0202(3) Uani 1 1 d . U . . .
C21 C 0.31905(17) 0.51311(8) 0.4002(2) 0.0122(4) Uani 1 1 d D U . . .
S2 S 0.12532(14) 0.46547(7) 0.2634(2) 0.0163(4) Uani 0.552(3) 1 d D U P B 1
C22 C 0.19596(16) 0.51278(7) 0.3667(2) 0.0123(4) Uani 0.552(3) 1 d D U P B 1
C23 C 0.1214(6) 0.5471(3) 0.4099(10) 0.0184(15) Uani 0.552(3) 1 d D U P B 1
H23 H 0.1449 0.5750 0.4709 0.022 Uiso 0.552(3) 1 calc R U P B 1
C24 C 0.0086(6) 0.5384(5) 0.358(2) 0.0177(14) Uani 0.552(3) 1 d D U P B 1
H24 H -0.0519 0.5598 0.3746 0.021 Uiso 0.552(3) 1 calc R U P B 1
C25 C -0.0005(6) 0.4947(4) 0.2809(17) 0.0166(14) Uani 0.552(3) 1 d D U P B 1
H25 H -0.0705 0.4811 0.2395 0.020 Uiso 0.552(3) 1 calc R U P B 1
S2A S 0.12218(19) 0.56224(9) 0.4262(3) 0.0164(5) Uani 0.448(3) 1 d D U P B 2
C22A C 0.19596(16) 0.51278(7) 0.3667(2) 0.0123(4) Uani 0.448(3) 1 d D U P B 2
C23A C 0.1281(7) 0.4776(3) 0.2930(10) 0.0189(17) Uani 0.448(3) 1 d D U P B 2
H23A H 0.1561 0.4476 0.2534 0.023 Uiso 0.448(3) 1 calc R U P B 2
C24A C 0.0134(7) 0.4888(6) 0.280(2) 0.0178(16) Uani 0.448(3) 1 d D U P B 2
H24A H -0.0448 0.4688 0.2292 0.021 Uiso 0.448(3) 1 calc R U P B 2
C25A C -0.0007(7) 0.5329(6) 0.350(2) 0.0158(17) Uani 0.448(3) 1 d D U P B 2
H25A H -0.0724 0.5467 0.3578 0.019 Uiso 0.448(3) 1 calc R U P B 2
O5 O 0.70822(12) 0.63143(6) 0.56476(16) 0.0175(3) Uani 1 1 d . U . . .
O6 O 0.77703(12) 0.60305(6) 0.37602(16) 0.0190(3) Uani 1 1 d . U . . .
C26 C 0.78080(17) 0.63001(8) 0.4834(2) 0.0139(4) Uani 1 1 d D U . . .
S3 S 0.88894(19) 0.70420(9) 0.6600(2) 0.0180(4) Uani 0.572(3) 1 d D U P C 1
C27 C 0.87749(17) 0.66604(8) 0.5174(2) 0.0159(4) Uani 0.572(3) 1 d D U P C 1
C28 C 0.9627(7) 0.6749(4) 0.4410(8) 0.0240(16) Uani 0.572(3) 1 d D U P C 1
H28 H 0.9696 0.6563 0.3581 0.029 Uiso 0.572(3) 1 calc R U P C 1
C29 C 1.0388(8) 0.7134(3) 0.4943(9) 0.0226(13) Uani 0.572(3) 1 d D U P C 1
H29 H 1.1025 0.7238 0.4544 0.027 Uiso 0.572(3) 1 calc R U P C 1
C30 C 1.0069(8) 0.7334(5) 0.6120(10) 0.0175(13) Uani 0.572(3) 1 d D U P C 1
H30 H 1.0455 0.7608 0.6634 0.021 Uiso 0.572(3) 1 calc R U P C 1
S3A S 0.9701(3) 0.67609(15) 0.4045(3) 0.0266(6) Uani 0.428(3) 1 d D U P C 2
C27A C 0.87749(17) 0.66604(8) 0.5174(2) 0.0159(4) Uani 0.428(3) 1 d D U P C 2
C28A C 0.8978(10) 0.6999(5) 0.6279(10) 0.0191(18) Uani 0.428(3) 1 d D U P C 2
H28A H 0.8516 0.7013 0.6993 0.023 Uiso 0.428(3) 1 calc R U P C 2
C29A C 0.9911(11) 0.7323(6) 0.6285(14) 0.0199(16) Uani 0.428(3) 1 d D U P C 2
H29A H 1.0184 0.7560 0.7003 0.024 Uiso 0.428(3) 1 calc R U P C 2
C30A C 1.0356(10) 0.7243(4) 0.5098(12) 0.0218(17) Uani 0.428(3) 1 d D U P C 2
H30A H 1.0974 0.7433 0.4865 0.026 Uiso 0.428(3) 1 calc R U P C 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

_exptl_special_details           
; 
One distinct cell was identified using APEX2 (Bruker, 2014).  Three 
frame series were integrated and filtered for statistical outliers 
using SAINT (Bruker, 2014) then corrected for absorption by integration 
using SAINT/SADABS v2014/2 (Bruker, 2014) to sort, merge, and scale 
the combined data.  No decay correction was applied.   
;

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0.00 1.00 1.00 0.0950
0.00 -1.00 -1.00 0.1100
-1.00 2.00 -2.00 0.1140
1.00 -2.00 2.00 0.1320
-1.00 1.00 -1.00 0.1110
1.00 -1.00 1.00 0.1290
1.00 1.00 1.00 0.0990
-1.00 -2.00 -1.00 0.1060
2.00 -2.00 1.00 0.1410
2.00 1.00 1.00 0.0980
0.00 1.00 0.00 0.2640
0.00 -1.00 0.00 0.2080
-1.00 -1.00 0.00 0.0750
1.00 0.00 0.00 0.0900
-1.00 0.00 0.00 0.0640
1.00 1.00 -1.00 0.1550
-1.00 -1.00 1.00 0.0810
1.00 2.00 -2.00 0.1480
0.00 1.00 2.00 0.0830

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
La1 O3 2.4289(14) 3_666 ?
La1 O4 2.4363(14) . ?
La1 O5 2.5159(14) . ?
La1 O2 2.5609(14) . ?
La1 O7 2.5734(16) . ?
La1 N3 2.6630(18) . ?
La1 O1 2.6693(16) . ?
La1 N1 2.6795(17) . ?
La1 N2 2.7148(17) . ?
La1 C16 2.966(2) . ?
O7 H7A 0.855(10) . ?
O7 H7B 0.848(10) . ?
O8 H8A 0.860(10) . ?
O8 H8B 0.859(10) . ?
N1 C1 1.343(3) . ?
N1 C5 1.350(3) . ?
N2 C6 1.346(3) . ?
N2 C10 1.353(3) . ?
N3 C11 1.344(3) . ?
N3 C15 1.344(3) . ?
C1 C2 1.380(3) . ?
C1 H1 0.9500 . ?
C2 C3 1.381(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.380(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.392(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.490(3) . ?
C6 C7 1.396(3) . ?
C7 C8 1.375(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.375(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.391(3) . ?
C9 H9 0.9500 . ?
C10 C11 1.486(3) . ?
C11 C12 1.394(3) . ?
C12 C13 1.375(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.368(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.387(4) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
O1 C16 1.266(3) . ?
O2 C16 1.260(3) . ?
C16 C17A 1.480(7) . ?
C16 C17 1.493(4) . ?
S1 C17 1.708(4) . ?
S1 C20 1.728(5) . ?
C17 C18 1.369(6) . ?
C18 C19 1.406(8) . ?
C18 H18 0.9500 . ?
C19 C20 1.357(5) . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?
S1A C17A 1.704(7) . ?
S1A C20A 1.735(8) . ?
C17A C18A 1.368(8) . ?
C18A C19A 1.404(10) . ?
C18A H18A 0.9500 . ?
C19A C20A 1.356(7) . ?
C19A H19A 0.9500 . ?
C20A H20A 0.9500 . ?
O3 C21 1.260(2) . ?
O3 La1 2.4290(14) 3_666 ?
O4 C21 1.254(2) . ?
C21 C22A 1.477(3) . ?
C21 C22 1.477(3) . ?
S2 C22 1.728(2) . ?
S2 C25 1.729(6) . ?
C22 C23 1.374(6) . ?
C23 C24 1.402(8) . ?
C23 H23 0.9500 . ?
C24 C25 1.354(6) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
S2A C22A 1.709(3) . ?
S2A C25A 1.734(8) . ?
C22A C23A 1.358(6) . ?
C23A C24A 1.405(9) . ?
C23A H23A 0.9500 . ?
C24A C25A 1.357(6) . ?
C24A H24A 0.9500 . ?
C25A H25A 0.9500 . ?
O5 C26 1.262(3) . ?
O6 C26 1.247(3) . ?
C26 C27A 1.495(3) . ?
C26 C27 1.495(3) . ?
S3 C27 1.687(3) . ?
S3 C30 1.737(6) . ?
C27 C28 1.371(6) . ?
C28 C29 1.405(8) . ?
C28 H28 0.9500 . ?
C29 C30 1.357(6) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?
S3A C27A 1.694(3) . ?
S3A C30A 1.729(7) . ?
C27A C28A 1.378(7) . ?
C28A C29A 1.406(9) . ?
C28A H28A 0.9500 . ?
C29A C30A 1.353(7) . ?
C29A H29A 0.9500 . ?
C30A H30A 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
O3 La1 O4 90.68(5) 3_666 . ?
O3 La1 O5 80.99(5) 3_666 . ?
O4 La1 O5 142.18(5) . . ?
O3 La1 O2 129.31(5) 3_666 . ?
O4 La1 O2 76.90(5) . . ?
O5 La1 O2 135.54(5) . . ?
O3 La1 O7 78.63(5) 3_666 . ?
O4 La1 O7 72.05(5) . . ?
O5 La1 O7 70.14(5) . . ?
O2 La1 O7 138.32(5) . . ?
O3 La1 N3 79.67(5) 3_666 . ?
O4 La1 N3 144.26(6) . . ?
O5 La1 N3 70.52(5) . . ?
O2 La1 N3 82.89(5) . . ?
O7 La1 N3 137.37(5) . . ?
O3 La1 O1 79.13(5) 3_666 . ?
O4 La1 O1 74.69(5) . . ?
O5 La1 O1 137.98(5) . . ?
O2 La1 O1 50.18(5) . . ?
O7 La1 O1 139.39(5) . . ?
N3 La1 O1 69.72(5) . . ?
O3 La1 N1 155.39(5) 3_666 . ?
O4 La1 N1 79.62(5) . . ?
O5 La1 N1 92.84(5) . . ?
O2 La1 N1 70.69(5) . . ?
O7 La1 N1 76.88(5) . . ?
N3 La1 N1 120.85(5) . . ?
O1 La1 N1 119.08(5) . . ?
O3 La1 N2 134.45(5) 3_666 . ?
O4 La1 N2 134.63(5) . . ?
O5 La1 N2 65.68(5) . . ?
O2 La1 N2 70.36(5) . . ?
O7 La1 N2 114.79(5) . . ?
N3 La1 N2 60.91(5) . . ?
O1 La1 N2 105.07(5) . . ?
N1 La1 N2 60.56(5) . . ?
O3 La1 C16 104.32(6) 3_666 . ?
O4 La1 C16 72.87(6) . . ?
O5 La1 C16 144.95(5) . . ?
O2 La1 C16 25.00(5) . . ?
O7 La1 C16 144.82(6) . . ?
N3 La1 C16 76.35(6) . . ?
O1 La1 C16 25.26(5) . . ?
N1 La1 C16 94.43(6) . . ?
N2 La1 C16 88.51(5) . . ?
La1 O7 H7A 111.1(19) . . ?
La1 O7 H7B 125.2(19) . . ?
H7A O7 H7B 116(3) . . ?
H8A O8 H8B 105(6) . . ?
C1 N1 C5 117.86(18) . . ?
C1 N1 La1 118.81(13) . . ?
C5 N1 La1 123.08(14) . . ?
C6 N2 C10 118.53(18) . . ?
C6 N2 La1 121.87(13) . . ?
C10 N2 La1 119.48(13) . . ?
C11 N3 C15 118.4(2) . . ?
C11 N3 La1 120.39(14) . . ?
C15 N3 La1 117.71(15) . . ?
N1 C1 C2 123.7(2) . . ?
N1 C1 H1 118.2 . . ?
C2 C1 H1 118.2 . . ?
C1 C2 C3 118.2(2) . . ?
C1 C2 H2 120.9 . . ?
C3 C2 H2 120.9 . . ?
C4 C3 C2 119.2(2) . . ?
C4 C3 H3 120.4 . . ?
C2 C3 H3 120.4 . . ?
C3 C4 C5 119.6(2) . . ?
C3 C4 H4 120.2 . . ?
C5 C4 H4 120.2 . . ?
N1 C5 C4 121.5(2) . . ?
N1 C5 C6 116.90(18) . . ?
C4 C5 C6 121.55(19) . . ?
N2 C6 C7 121.6(2) . . ?
N2 C6 C5 117.22(18) . . ?
C7 C6 C5 121.15(19) . . ?
C8 C7 C6 119.7(2) . . ?
C8 C7 H7 120.2 . . ?
C6 C7 H7 120.2 . . ?
C7 C8 C9 118.8(2) . . ?
C7 C8 H8 120.6 . . ?
C9 C8 H8 120.6 . . ?
C8 C9 C10 119.5(2) . . ?
C8 C9 H9 120.2 . . ?
C10 C9 H9 120.2 . . ?
N2 C10 C9 121.8(2) . . ?
N2 C10 C11 117.49(19) . . ?
C9 C10 C11 120.6(2) . . ?
N3 C11 C12 121.0(2) . . ?
N3 C11 C10 116.64(19) . . ?
C12 C11 C10 122.4(2) . . ?
C13 C12 C11 119.6(2) . . ?
C13 C12 H12 120.2 . . ?
C11 C12 H12 120.2 . . ?
C14 C13 C12 119.7(2) . . ?
C14 C13 H13 120.2 . . ?
C12 C13 H13 120.2 . . ?
C13 C14 C15 118.1(2) . . ?
C13 C14 H14 121.0 . . ?
C15 C14 H14 121.0 . . ?
N3 C15 C14 123.2(2) . . ?
N3 C15 H15 118.4 . . ?
C14 C15 H15 118.4 . . ?
C16 O1 La1 90.59(13) . . ?
C16 O2 La1 95.78(12) . . ?
O2 C16 O1 123.1(2) . . ?
O2 C16 C17A 119.3(8) . . ?
O1 C16 C17A 117.6(8) . . ?
O2 C16 C17 116.4(4) . . ?
O1 C16 C17 120.6(4) . . ?
O2 C16 La1 59.21(11) . . ?
O1 C16 La1 64.15(11) . . ?
C17A C16 La1 175(3) . . ?
C17 C16 La1 173.0(8) . . ?
C17 S1 C20 90.9(2) . . ?
C18 C17 C16 127.6(4) . . ?
C18 C17 S1 110.8(3) . . ?
C16 C17 S1 121.6(3) . . ?
C17 C18 C19 114.8(5) . . ?
C17 C18 H18 122.6 . . ?
C19 C18 H18 122.6 . . ?
C20 C19 C18 110.1(6) . . ?
C20 C19 H19 125.0 . . ?
C18 C19 H19 125.0 . . ?
C19 C20 S1 113.4(5) . . ?
C19 C20 H20 123.3 . . ?
S1 C20 H20 123.3 . . ?
C17A S1A C20A 89.2(5) . . ?
C18A C17A C16 132.7(8) . . ?
C18A C17A S1A 112.2(5) . . ?
C16 C17A S1A 115.1(6) . . ?
C17A C18A C19A 114.6(8) . . ?
C17A C18A H18A 122.7 . . ?
C19A C18A H18A 122.7 . . ?
C20A C19A C18A 108.9(10) . . ?
C20A C19A H19A 125.5 . . ?
C18A C19A H19A 125.5 . . ?
C19A C20A S1A 115.0(10) . . ?
C19A C20A H20A 122.5 . . ?
S1A C20A H20A 122.5 . . ?
C21 O3 La1 140.52(14) . 3_666 ?
C21 O4 La1 153.45(14) . . ?
O4 C21 O3 124.46(19) . . ?
O4 C21 C22A 116.88(18) . . ?
O3 C21 C22A 118.65(18) . . ?
O4 C21 C22 116.88(18) . . ?
O3 C21 C22 118.65(18) . . ?
C22 S2 C25 90.0(3) . . ?
C23 C22 C21 127.9(3) . . ?
C23 C22 S2 110.2(3) . . ?
C21 C22 S2 121.93(15) . . ?
C22 C23 C24 115.8(6) . . ?
C22 C23 H23 122.1 . . ?
C24 C23 H23 122.1 . . ?
C25 C24 C23 109.1(8) . . ?
C25 C24 H24 125.4 . . ?
C23 C24 H24 125.4 . . ?
C24 C25 S2 114.8(7) . . ?
C24 C25 H25 122.6 . . ?
S2 C25 H25 122.6 . . ?
C22A S2A C25A 89.2(4) . . ?
C23A C22A C21 129.2(4) . . ?
C23A C22A S2A 112.1(4) . . ?
C21 C22A S2A 118.74(16) . . ?
C22A C23A C24A 115.0(7) . . ?
C22A C23A H23A 122.5 . . ?
C24A C23A H23A 122.5 . . ?
C25A C24A C23A 108.8(9) . . ?
C25A C24A H24A 125.6 . . ?
C23A C24A H24A 125.6 . . ?
C24A C25A S2A 114.9(8) . . ?
C24A C25A H25A 122.6 . . ?
S2A C25A H25A 122.6 . . ?
C26 O5 La1 142.99(14) . . ?
O6 C26 O5 126.3(2) . . ?
O6 C26 C27A 117.80(19) . . ?
O5 C26 C27A 115.89(19) . . ?
O6 C26 C27 117.80(19) . . ?
O5 C26 C27 115.89(19) . . ?
C27 S3 C30 90.6(3) . . ?
C28 C27 C26 127.6(4) . . ?
C28 C27 S3 111.3(4) . . ?
C26 C27 S3 121.01(16) . . ?
C27 C28 C29 115.1(6) . . ?
C27 C28 H28 122.4 . . ?
C29 C28 H28 122.4 . . ?
C30 C29 C28 109.2(7) . . ?
C30 C29 H29 125.4 . . ?
C28 C29 H29 125.4 . . ?
C29 C30 S3 113.7(6) . . ?
C29 C30 H30 123.1 . . ?
S3 C30 H30 123.1 . . ?
C27A S3A C30A 91.2(4) . . ?
C28A C27A C26 127.9(4) . . ?
C28A C27A S3A 110.0(4) . . ?
C26 C27A S3A 121.54(18) . . ?
C27A C28A C29A 115.9(7) . . ?
C27A C28A H28A 122.1 . . ?
C29A C28A H28A 122.1 . . ?
C30A C29A C28A 108.8(9) . . ?
C30A C29A H29A 125.6 . . ?
C28A C29A H29A 125.6 . . ?
C29A C30A S3A 114.0(8) . . ?
C29A C30A H30A 123.0 . . ?
S3A C30A H30A 123.0 . . ?

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
O7 H7A O6 0.855(10) 1.857(13) 2.688(2) 163(3) .
O7 H7B O8 0.848(10) 2.06(2) 2.727(4) 136(2) 3_666
O7 H7B O3 0.848(10) 2.65(2) 3.289(2) 133(2) .
O8 H8A O1 0.860(10) 1.84(3) 2.651(4) 156(7) .
O8 H8B O8 0.859(10) 1.94(6) 2.428(8) 115(6) 3_667
O8 H8B O1 0.859(10) 2.17(2) 3.007(4) 164(7) 3_667

_refine_diff_density_max         0.366
_refine_diff_density_min         -0.642
_refine_diff_density_rms         0.079

####################################################################### 
# 
# 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_14x
_database_code_depnum_ccdc_archive 'CCDC 1544452'
_audit_update_record             
;
2017-04-17 deposited with the CCDC.
2017-08-23 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         'C30 H22 N3 O7 S3 Tm'
_chemical_formula_sum            'C30 H22 N3 O7 S3 Tm'
_chemical_formula_weight         801.61

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'
Tm Tm -0.3139 5.2483 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   8.4070(4)
_cell_length_b                   20.3347(9)
_cell_length_c                   17.5788(8)
_cell_angle_alpha                90
_cell_angle_beta                 98.1531(16)
_cell_angle_gamma                90
_cell_volume                     2974.8(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9927
_cell_measurement_theta_min      2.32
_cell_measurement_theta_max      25.37
_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.790
_exptl_crystal_F_000             1584
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.163
_exptl_crystal_size_mid          0.076
_exptl_crystal_size_min          0.049
_exptl_absorpt_coefficient_mu    3.246
_shelx_estimated_absorpt_T_min   0.620
_shelx_estimated_absorpt_T_max   0.857
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.78800
_exptl_absorpt_correction_T_max  0.90179
_exptl_absorpt_process_details   'SADABS V2016/2 (Bruker, 2014)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_monochromator  'multilayer mirrors'
_diffrn_measurement_device       'Bruker D8 Quest/Photon 100'
_diffrn_measurement_method       'profile data from φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            70469
_diffrn_reflns_av_unetI/netI     0.0242
_diffrn_reflns_av_R_equivalents  0.0658
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.320
_diffrn_reflns_theta_max         25.398
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             5472
_reflns_number_gt                4735
_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.
 
 _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       'APEX2 V2014.9-0 (Bruker, 2014)'
_computing_cell_refinement       'SAINT V8.37A (Bruker, 2005)'
_computing_data_reduction        
; 
SAINT V8.37A, XPREP v2014/2, SADABS V2016/2 (Bruker, 2014) 
;
_computing_structure_solution    'SHELX-2014-5 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELX-2014-7 (Sheldrick, 2015)'
_computing_molecular_graphics    'SHELXLE v817 (Hubschle, 2011)'
_computing_publication_material  'XCIF V2014-2 (Bruker, 2014)'

_refine_special_details          
; 
Structure was phased by direct methods (Sheldrick, 2015).  Systematic 
conditions suggested the ambiguous space group.  The space group choice 
was confirmed by successful convergence of the full-matrix least-squares 
refinement on F².  The final map had no other significant features.  A 
final analysis of variance between observed and calculated structure 
factors showed little dependence on amplitude and resolution. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0137P)²+3.8293P] 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         5472
_refine_ls_number_parameters     514
_refine_ls_number_restraints     1082
_refine_ls_R_factor_all          0.0292
_refine_ls_R_factor_gt           0.0202
_refine_ls_wR_factor_ref         0.0392
_refine_ls_wR_factor_gt          0.0373
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      0.961
_refine_ls_shift/su_max          0.003
_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
Tm1 Tm 0.23293(2) 0.37245(2) 0.67074(2) 0.00826(4) Uani 1 1 d . U . . .
O1 O 0.4263(2) 0.33893(9) 0.76494(10) 0.0148(4) Uani 1 1 d . U . . .
O2 O 0.3217(2) 0.34027(11) 0.87560(11) 0.0237(5) Uani 1 1 d . U . . .
C16 C 0.4368(3) 0.34384(14) 0.83856(16) 0.0159(6) Uani 1 1 d D U . . .
S1 S 0.76381(15) 0.34182(9) 0.83522(7) 0.0203(4) Uani 0.746(3) 1 d D U P A 1
C17 C 0.5999(3) 0.35331(13) 0.88093(15) 0.0146(6) Uani 0.746(3) 1 d D U P A 1
C18 C 0.6440(9) 0.3686(4) 0.9563(4) 0.0191(15) Uani 0.746(3) 1 d D U P A 1
H18 H 0.5694 0.3750 0.9915 0.023 Uiso 0.746(3) 1 calc R U P A 1
C19 C 0.8118(8) 0.3740(10) 0.9770(5) 0.0212(11) Uani 0.746(3) 1 d D U P A 1
H19 H 0.8624 0.3878 1.0262 0.025 Uiso 0.746(3) 1 calc R U P A 1
C20 C 0.8925(8) 0.3571(10) 0.9182(5) 0.0220(13) Uani 0.746(3) 1 d D U P A 1
H20 H 1.0062 0.3541 0.9226 0.026 Uiso 0.746(3) 1 calc R U P A 1
S1B S 0.6240(6) 0.3817(3) 0.9730(3) 0.0161(11) Uani 0.254(3) 1 d D U P A 2
C17B C 0.5999(3) 0.35331(13) 0.88093(15) 0.0146(6) Uani 0.254(3) 1 d D U P A 2
C18B C 0.7456(14) 0.3442(11) 0.8569(8) 0.021(2) Uani 0.254(3) 1 d D U P A 2
H18B H 0.7574 0.3288 0.8070 0.025 Uiso 0.254(3) 1 calc R U P A 2
C19B C 0.8772(18) 0.360(3) 0.9132(15) 0.022(2) Uani 0.254(3) 1 d D U P A 2
H19B H 0.9857 0.3613 0.9040 0.026 Uiso 0.254(3) 1 calc R U P A 2
C20B C 0.8286(17) 0.372(3) 0.9824(14) 0.020(2) Uani 0.254(3) 1 d D U P A 2
H20B H 0.8987 0.3752 1.0297 0.024 Uiso 0.254(3) 1 calc R U P A 2
O3 O 0.3425(2) 0.47855(9) 0.65202(10) 0.0137(4) Uani 1 1 d . U . . .
O4 O 0.2389(2) 0.45993(9) 0.75877(10) 0.0145(4) Uani 1 1 d . U . . .
C21 C 0.3108(3) 0.49726(13) 0.71793(16) 0.0130(6) Uani 1 1 d D U . . .
S2 S 0.4557(3) 0.61753(8) 0.69801(11) 0.0183(4) Uani 0.743(3) 1 d D U P B 1
C22 C 0.3581(3) 0.56318(14) 0.74585(15) 0.0168(6) Uani 0.743(3) 1 d D U P B 1
C23 C 0.3172(15) 0.5897(6) 0.8136(5) 0.0230(17) Uani 0.743(3) 1 d D U P B 1
H23 H 0.2565 0.5674 0.8473 0.028 Uiso 0.743(3) 1 calc R U P B 1
C24 C 0.3792(7) 0.6552(3) 0.8256(3) 0.0302(12) Uani 0.743(3) 1 d D U P B 1
H24 H 0.3693 0.6807 0.8699 0.036 Uiso 0.743(3) 1 calc R U P B 1
C25 C 0.4535(7) 0.6767(2) 0.7666(3) 0.0216(12) Uani 0.743(3) 1 d D U P B 1
H25 H 0.4986 0.7194 0.7638 0.026 Uiso 0.743(3) 1 calc R U P B 1
S2B S 0.3390(11) 0.5905(4) 0.8303(3) 0.0243(13) Uani 0.257(3) 1 d D U P B 2
C22B C 0.3581(3) 0.56318(14) 0.74585(15) 0.0168(6) Uani 0.257(3) 1 d D U P B 2
C23B C 0.445(4) 0.6066(9) 0.7043(13) 0.018(2) Uani 0.257(3) 1 d D U P B 2
H23B H 0.4788 0.5969 0.6563 0.021 Uiso 0.257(3) 1 calc R U P B 2
C24B C 0.473(2) 0.6677(6) 0.7451(8) 0.020(2) Uani 0.257(3) 1 d D U P B 2
H24B H 0.5178 0.7058 0.7249 0.024 Uiso 0.257(3) 1 calc R U P B 2
C25B C 0.428(2) 0.6643(6) 0.8161(8) 0.025(2) Uani 0.257(3) 1 d D U P B 2
H25B H 0.4445 0.6984 0.8533 0.030 Uiso 0.257(3) 1 calc R U P B 2
O5 O 0.0537(3) 0.21295(10) 0.71978(12) 0.0306(6) Uani 1 1 d . U . . .
O6 O 0.1648(2) 0.26964(9) 0.63188(11) 0.0159(4) Uani 1 1 d . U . . .
C26 C 0.1239(3) 0.21612(14) 0.66203(16) 0.0158(6) Uani 1 1 d D U . . .
S3 S 0.1230(5) 0.07962(12) 0.66046(18) 0.0280(7) Uani 0.548(4) 1 d D U P C 1
C27 C 0.1622(3) 0.15446(14) 0.62411(16) 0.0174(6) Uani 0.548(4) 1 d D U P C 1
C28 C 0.2297(17) 0.1460(6) 0.5569(7) 0.0214(19) Uani 0.548(4) 1 d D U P C 1
H28 H 0.2632 0.1825 0.5296 0.026 Uiso 0.548(4) 1 calc R U P C 1
C29 C 0.246(2) 0.0815(5) 0.5311(7) 0.0252(18) Uani 0.548(4) 1 d D U P C 1
H29 H 0.2844 0.0685 0.4850 0.030 Uiso 0.548(4) 1 calc R U P C 1
C30 C 0.1979(18) 0.0413(6) 0.5848(5) 0.0303(18) Uani 0.548(4) 1 d D U P C 1
H30 H 0.2044 -0.0052 0.5812 0.036 Uiso 0.548(4) 1 calc R U P C 1
S3B S 0.2459(5) 0.15838(15) 0.5443(2) 0.0184(7) Uani 0.452(4) 1 d D U P C 2
C27B C 0.1622(3) 0.15446(14) 0.62411(16) 0.0174(6) Uani 0.452(4) 1 d D U P C 2
C28B C 0.144(2) 0.0915(6) 0.6510(9) 0.025(2) Uani 0.452(4) 1 d D U P C 2
H28B H 0.1027 0.0827 0.6975 0.030 Uiso 0.452(4) 1 calc R U P C 2
C29B C 0.192(2) 0.0421(7) 0.6043(7) 0.0290(19) Uani 0.452(4) 1 d D U P C 2
H29B H 0.1834 -0.0040 0.6120 0.035 Uiso 0.452(4) 1 calc R U P C 2
C30B C 0.253(2) 0.0721(5) 0.5455(8) 0.021(2) Uani 0.452(4) 1 d D U P C 2
H30B H 0.2977 0.0477 0.5074 0.026 Uiso 0.452(4) 1 calc R U P C 2
N1 N -0.0251(3) 0.42814(11) 0.63003(12) 0.0108(5) Uani 1 1 d . U . . .
N2 N 0.1533(3) 0.37833(11) 0.53009(12) 0.0098(4) Uani 1 1 d . U . . .
N3 N 0.4474(3) 0.34159(11) 0.59395(12) 0.0107(5) Uani 1 1 d . U . . .
C1 C -0.1087(3) 0.45453(13) 0.68224(16) 0.0139(6) Uani 1 1 d . U . . .
H1 H -0.0669 0.4503 0.7351 0.017 Uiso 1 1 calc R U . . .
C2 C -0.2522(3) 0.48749(13) 0.66270(16) 0.0160(6) Uani 1 1 d . U . . .
H2 H -0.3089 0.5047 0.7013 0.019 Uiso 1 1 calc R U . . .
C3 C -0.3116(3) 0.49487(14) 0.58566(16) 0.0170(6) Uani 1 1 d . U . . .
H3 H -0.4094 0.5178 0.5705 0.020 Uiso 1 1 calc R U . . .
C4 C -0.2268(3) 0.46847(13) 0.53100(16) 0.0140(6) Uani 1 1 d . U . . .
H4 H -0.2647 0.4736 0.4778 0.017 Uiso 1 1 calc R U . . .
C5 C -0.0858(3) 0.43436(13) 0.55484(15) 0.0119(6) Uani 1 1 d . U . . .
C6 C 0.0072(3) 0.40085(13) 0.50046(15) 0.0114(5) Uani 1 1 d . U . . .
C7 C -0.0558(4) 0.39157(14) 0.42363(16) 0.0181(6) Uani 1 1 d . U . . .
H7 H -0.1579 0.4091 0.4037 0.022 Uiso 1 1 calc R U . . .
C8 C 0.0320(4) 0.35657(14) 0.37703(16) 0.0197(7) Uani 1 1 d . U . . .
H8 H -0.0103 0.3486 0.3248 0.024 Uiso 1 1 calc R U . . .
C9 C 0.1818(3) 0.33313(14) 0.40684(16) 0.0177(6) Uani 1 1 d . U . . .
H9 H 0.2434 0.3084 0.3756 0.021 Uiso 1 1 calc R U . . .
C10 C 0.2419(3) 0.34613(13) 0.48348(15) 0.0124(6) Uani 1 1 d . U . . .
C11 C 0.4069(3) 0.32754(13) 0.51847(15) 0.0114(6) Uani 1 1 d . U . . .
C12 C 0.5162(3) 0.29927(13) 0.47573(16) 0.0154(6) Uani 1 1 d . U . . .
H12 H 0.4840 0.2883 0.4233 0.019 Uiso 1 1 calc R U . . .
C13 C 0.6715(4) 0.28724(13) 0.50978(17) 0.0180(6) Uani 1 1 d . U . . .
H13 H 0.7477 0.2686 0.4810 0.022 Uiso 1 1 calc R U . . .
C14 C 0.7142(3) 0.30274(13) 0.58646(17) 0.0154(6) Uani 1 1 d . U . . .
H14 H 0.8205 0.2954 0.6114 0.018 Uiso 1 1 calc R U . . .
C15 C 0.5982(3) 0.32926(13) 0.62623(16) 0.0147(6) Uani 1 1 d . U . . .
H15 H 0.6274 0.3392 0.6792 0.018 Uiso 1 1 calc R U . . .
O7 O 0.0774(2) 0.33739(10) 0.76282(11) 0.0150(4) Uani 1 1 d D U . . .
H7A H 0.141(3) 0.3391(16) 0.8052(10) 0.022 Uiso 1 1 d D U . . .
H7B H 0.054(4) 0.2970(7) 0.7536(17) 0.022 Uiso 1 1 d D U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

_exptl_special_details           
; 
One distinct cell was identified using APEX2 (Bruker, 2014).  Five 
frame series were integrated and filtered for statistical outliers 
using SAINT (Bruker, 2014) then corrected for absorption by integration 
using SAINT/SADABS v2014/2 (Bruker, 2014) to sort, merge, and scale 
the combined data.  No decay correction was applied.    
;

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0.00 -1.00 -1.00 0.0530
0.00 1.00 1.00 0.0050
-1.00 0.00 1.00 0.0140
-1.00 1.00 1.00 0.0150
1.00 -1.00 -1.00 0.0240
2.00 -2.00 -1.00 0.0230
0.00 -1.00 0.00 0.0280
0.00 1.00 0.00 0.0390
2.00 2.00 -1.00 0.0270
1.00 2.00 -1.00 0.0340
0.00 2.00 -1.00 0.0510
-1.00 2.00 -1.00 0.0480

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
Tm1 O6 2.2482(18) . ?
Tm1 O1 2.2551(18) . ?
Tm1 O7 2.3322(19) . ?
Tm1 O4 2.3537(18) . ?
Tm1 O3 2.3870(18) . ?
Tm1 N1 2.462(2) . ?
Tm1 N2 2.471(2) . ?
Tm1 N3 2.481(2) . ?
Tm1 C21 2.721(3) . ?
O1 C16 1.288(3) . ?
O2 C16 1.243(3) . ?
C16 C17B 1.477(4) . ?
C16 C17 1.477(4) . ?
S1 C17 1.707(3) . ?
S1 C20 1.717(7) . ?
C17 C18 1.361(7) . ?
C18 C19 1.410(10) . ?
C18 H18 0.9500 . ?
C19 C20 1.358(5) . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?
S1B C17B 1.704(5) . ?
S1B C20B 1.715(13) . ?
C17B C18B 1.363(10) . ?
C18B C19B 1.412(14) . ?
C18B H18B 0.9500 . ?
C19B C20B 1.360(9) . ?
C19B H19B 0.9500 . ?
C20B H20B 0.9500 . ?
O3 C21 1.283(3) . ?
O4 C21 1.257(3) . ?
C21 C22B 1.463(4) . ?
C21 C22 1.463(4) . ?
S2 C22 1.673(3) . ?
S2 C25 1.705(5) . ?
C22 C23 1.395(10) . ?
C23 C24 1.435(11) . ?
C23 H23 0.9500 . ?
C24 C25 1.357(6) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
S2B C22B 1.615(6) . ?
S2B C25B 1.712(10) . ?
C22B C23B 1.412(13) . ?
C23B C24B 1.439(14) . ?
C23B H23B 0.9500 . ?
C24B C25B 1.356(10) . ?
C24B H24B 0.9500 . ?
C25B H25B 0.9500 . ?
O5 C26 1.247(3) . ?
O6 C26 1.279(3) . ?
C26 C27B 1.477(4) . ?
C26 C27 1.477(4) . ?
S3 C27 1.701(3) . ?
S3 C30 1.735(9) . ?
C27 C28 1.391(10) . ?
C28 C29 1.401(15) . ?
C28 H28 0.9500 . ?
C29 C30 1.354(7) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?
S3B C27B 1.658(4) . ?
S3B C30B 1.756(10) . ?
C27B C28B 1.380(11) . ?
C28B C29B 1.394(16) . ?
C28B H28B 0.9500 . ?
C29B C30B 1.363(8) . ?
C29B H29B 0.9500 . ?
C30B H30B 0.9500 . ?
N1 C1 1.344(3) . ?
N1 C5 1.354(3) . ?
N2 C6 1.344(3) . ?
N2 C10 1.352(3) . ?
N3 C15 1.337(4) . ?
N3 C11 1.353(3) . ?
C1 C2 1.381(4) . ?
C1 H1 0.9500 . ?
C2 C3 1.383(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.384(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.386(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.484(4) . ?
C6 C7 1.392(4) . ?
C7 C8 1.376(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.379(4) . ?
C8 H8 0.9500 . ?
C9 C10 1.395(4) . ?
C9 H9 0.9500 . ?
C10 C11 1.484(4) . ?
C11 C12 1.391(4) . ?
C12 C13 1.378(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.381(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.387(4) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
O7 H7A 0.854(10) . ?
O7 H7B 0.855(10) . ?

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
O6 Tm1 O1 93.91(7) . . ?
O6 Tm1 O7 77.45(7) . . ?
O1 Tm1 O7 79.33(7) . . ?
O6 Tm1 O4 152.05(7) . . ?
O1 Tm1 O4 78.44(7) . . ?
O7 Tm1 O4 74.73(7) . . ?
O6 Tm1 O3 152.29(6) . . ?
O1 Tm1 O3 97.03(7) . . ?
O7 Tm1 O3 129.59(6) . . ?
O4 Tm1 O3 55.58(6) . . ?
O6 Tm1 N1 99.40(7) . . ?
O1 Tm1 N1 150.02(7) . . ?
O7 Tm1 N1 77.56(7) . . ?
O4 Tm1 N1 77.25(7) . . ?
O3 Tm1 N1 83.42(7) . . ?
O6 Tm1 N2 73.73(7) . . ?
O1 Tm1 N2 144.50(7) . . ?
O7 Tm1 N2 127.60(7) . . ?
O4 Tm1 N2 126.78(7) . . ?
O3 Tm1 N2 82.72(7) . . ?
N1 Tm1 N2 65.44(7) . . ?
O6 Tm1 N3 76.88(7) . . ?
O1 Tm1 N3 79.59(7) . . ?
O7 Tm1 N3 145.34(7) . . ?
O4 Tm1 N3 126.83(7) . . ?
O3 Tm1 N3 80.17(7) . . ?
N1 Tm1 N3 129.53(7) . . ?
N2 Tm1 N3 65.33(7) . . ?
O6 Tm1 C21 179.16(8) . . ?
O1 Tm1 C21 86.61(7) . . ?
O7 Tm1 C21 102.00(8) . . ?
O4 Tm1 C21 27.48(7) . . ?
O3 Tm1 C21 28.12(7) . . ?
N1 Tm1 C21 79.84(7) . . ?
N2 Tm1 C21 106.21(8) . . ?
N3 Tm1 C21 103.87(8) . . ?
C16 O1 Tm1 130.84(17) . . ?
O2 C16 O1 125.0(3) . . ?
O2 C16 C17B 118.7(2) . . ?
O1 C16 C17B 116.3(2) . . ?
O2 C16 C17 118.7(2) . . ?
O1 C16 C17 116.3(2) . . ?
C17 S1 C20 91.6(3) . . ?
C18 C17 C16 128.8(4) . . ?
C18 C17 S1 111.3(4) . . ?
C16 C17 S1 119.9(2) . . ?
C17 C18 C19 113.1(6) . . ?
C17 C18 H18 123.4 . . ?
C19 C18 H18 123.4 . . ?
C20 C19 C18 112.0(7) . . ?
C20 C19 H19 124.0 . . ?
C18 C19 H19 124.0 . . ?
C19 C20 S1 111.7(6) . . ?
C19 C20 H20 124.2 . . ?
S1 C20 H20 124.2 . . ?
C17B S1B C20B 92.0(7) . . ?
C18B C17B C16 129.5(6) . . ?
C18B C17B S1B 110.5(6) . . ?
C16 C17B S1B 120.0(3) . . ?
C17B C18B C19B 113.7(10) . . ?
C17B C18B H18B 123.2 . . ?
C19B C18B H18B 123.2 . . ?
C20B C19B C18B 111.3(15) . . ?
C20B C19B H19B 124.3 . . ?
C18B C19B H19B 124.3 . . ?
C19B C20B S1B 111.1(13) . . ?
C19B C20B H20B 124.5 . . ?
S1B C20B H20B 124.5 . . ?
C21 O3 Tm1 90.57(16) . . ?
C21 O4 Tm1 92.75(16) . . ?
O4 C21 O3 121.0(2) . . ?
O4 C21 C22B 119.4(2) . . ?
O3 C21 C22B 119.6(2) . . ?
O4 C21 C22 119.4(2) . . ?
O3 C21 C22 119.6(2) . . ?
O4 C21 Tm1 59.77(14) . . ?
O3 C21 Tm1 61.30(13) . . ?
C22B C21 Tm1 177.5(2) . . ?
C22 C21 Tm1 177.5(2) . . ?
C22 S2 C25 93.2(2) . . ?
C23 C22 C21 123.5(5) . . ?
C23 C22 S2 111.8(5) . . ?
C21 C22 S2 124.5(2) . . ?
C22 C23 C24 110.8(8) . . ?
C22 C23 H23 124.6 . . ?
C24 C23 H23 124.6 . . ?
C25 C24 C23 112.6(6) . . ?
C25 C24 H24 123.7 . . ?
C23 C24 H24 123.7 . . ?
C24 C25 S2 111.4(4) . . ?
C24 C25 H25 124.3 . . ?
S2 C25 H25 124.3 . . ?
C22B S2B C25B 93.7(6) . . ?
C23B C22B C21 122.3(8) . . ?
C23B C22B S2B 112.8(6) . . ?
C21 C22B S2B 124.4(4) . . ?
C22B C23B C24B 110.1(11) . . ?
C22B C23B H23B 125.0 . . ?
C24B C23B H23B 125.0 . . ?
C25B C24B C23B 111.5(12) . . ?
C25B C24B H24B 124.3 . . ?
C23B C24B H24B 124.3 . . ?
C24B C25B S2B 111.4(10) . . ?
C24B C25B H25B 124.3 . . ?
S2B C25B H25B 124.3 . . ?
C26 O6 Tm1 137.51(18) . . ?
O5 C26 O6 124.6(3) . . ?
O5 C26 C27B 118.8(2) . . ?
O6 C26 C27B 116.5(2) . . ?
O5 C26 C27 118.8(2) . . ?
O6 C26 C27 116.5(2) . . ?
C27 S3 C30 90.2(5) . . ?
C28 C27 C26 129.0(5) . . ?
C28 C27 S3 109.4(5) . . ?
C26 C27 S3 121.6(2) . . ?
C27 C28 C29 117.6(10) . . ?
C27 C28 H28 121.2 . . ?
C29 C28 H28 121.2 . . ?
C30 C29 C28 106.6(12) . . ?
C30 C29 H29 126.7 . . ?
C28 C29 H29 126.7 . . ?
C29 C30 S3 116.1(11) . . ?
C29 C30 H30 121.9 . . ?
S3 C30 H30 121.9 . . ?
C27B S3B C30B 87.7(5) . . ?
C28B C27B C26 126.2(6) . . ?
C28B C27B S3B 114.5(6) . . ?
C26 C27B S3B 119.1(2) . . ?
C27B C28B C29B 114.3(11) . . ?
C27B C28B H28B 122.8 . . ?
C29B C28B H28B 122.8 . . ?
C30B C29B C28B 107.2(14) . . ?
C30B C29B H29B 126.4 . . ?
C28B C29B H29B 126.4 . . ?
C29B C30B S3B 116.1(12) . . ?
C29B C30B H30B 122.0 . . ?
S3B C30B H30B 122.0 . . ?
C1 N1 C5 117.9(2) . . ?
C1 N1 Tm1 120.62(17) . . ?
C5 N1 Tm1 121.43(17) . . ?
C6 N2 C10 118.8(2) . . ?
C6 N2 Tm1 120.47(16) . . ?
C10 N2 Tm1 119.24(17) . . ?
C15 N3 C11 117.9(2) . . ?
C15 N3 Tm1 122.34(18) . . ?
C11 N3 Tm1 119.06(17) . . ?
N1 C1 C2 123.2(3) . . ?
N1 C1 H1 118.4 . . ?
C2 C1 H1 118.4 . . ?
C1 C2 C3 118.5(3) . . ?
C1 C2 H2 120.7 . . ?
C3 C2 H2 120.7 . . ?
C4 C3 C2 119.2(3) . . ?
C4 C3 H3 120.4 . . ?
C2 C3 H3 120.4 . . ?
C3 C4 C5 119.1(3) . . ?
C3 C4 H4 120.4 . . ?
C5 C4 H4 120.4 . . ?
N1 C5 C4 122.0(2) . . ?
N1 C5 C6 115.2(2) . . ?
C4 C5 C6 122.8(2) . . ?
N2 C6 C7 122.1(2) . . ?
N2 C6 C5 116.3(2) . . ?
C7 C6 C5 121.6(2) . . ?
C8 C7 C6 119.0(3) . . ?
C8 C7 H7 120.5 . . ?
C6 C7 H7 120.5 . . ?
C7 C8 C9 119.4(3) . . ?
C7 C8 H8 120.3 . . ?
C9 C8 H8 120.3 . . ?
C8 C9 C10 119.2(3) . . ?
C8 C9 H9 120.4 . . ?
C10 C9 H9 120.4 . . ?
N2 C10 C9 121.5(3) . . ?
N2 C10 C11 115.8(2) . . ?
C9 C10 C11 122.7(2) . . ?
N3 C11 C12 121.5(3) . . ?
N3 C11 C10 116.3(2) . . ?
C12 C11 C10 122.1(2) . . ?
C13 C12 C11 119.8(3) . . ?
C13 C12 H12 120.1 . . ?
C11 C12 H12 120.1 . . ?
C12 C13 C14 118.8(3) . . ?
C12 C13 H13 120.6 . . ?
C14 C13 H13 120.6 . . ?
C13 C14 C15 118.4(3) . . ?
C13 C14 H14 120.8 . . ?
C15 C14 H14 120.8 . . ?
N3 C15 C14 123.4(3) . . ?
N3 C15 H15 118.3 . . ?
C14 C15 H15 118.3 . . ?
Tm1 O7 H7A 104(2) . . ?
Tm1 O7 H7B 107(2) . . ?
H7A O7 H7B 108(3) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O7 H7A O2 0.854(10) 1.818(14) 2.646(3) 163(3) .
O7 H7B O5 0.855(10) 1.810(14) 2.641(3) 164(3) .

_refine_diff_density_max         0.367
_refine_diff_density_min         -0.620
_refine_diff_density_rms         0.082

####################################################################### 
# 
# 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_final_a_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1544443'
_audit_update_record             
;
2017-04-17 deposited with the CCDC.
2017-08-23 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT430_final_a             
;
PROBLEM: Short Inter D...A Contact  O8     ..  O8      ..       2.46 Ang.
RESPONSE: O8 is a partially occupied lattice water molecule. The H atoms could not be located in the difference map and thus were left out of the model. It likely that there is hydrogen bonding present.
;
_vrf_PLAT430_final_a_2           
;
PROBLEM: Short Inter D...A Contact  O1     ..  O8      ..       2.63 Ang.
RESPONSE: O8 is a partially occupied lattice water molecule. The H atoms could not be located in the difference map and thus were left out of the model. It likely that there is hydrogen bonding present.
;
# Added during the CSD deposition process: Monday 17 April 2017 03:19 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C60 H44 N6 Nd2 O14 S6, 0.634(O)'
_chemical_formula_sum            'C60 H44 N6 Nd2 O14.63 S6'
_chemical_formula_weight         1564.01

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nd Nd -0.1943 3.0179 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   11.9880(5)
_cell_length_b                   25.6332(11)
_cell_length_c                   9.6899(4)
_cell_angle_alpha                90
_cell_angle_beta                 98.0710(10)
_cell_angle_gamma                90
_cell_volume                     2948.1(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9931
_cell_measurement_theta_min      2.65
_cell_measurement_theta_max      27.09
_exptl_crystal_description       rhombus
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.762
_exptl_crystal_F_000             1558
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.201
_exptl_crystal_size_mid          0.082
_exptl_crystal_size_min          0.065
_exptl_absorpt_coefficient_mu    2.029
_shelx_estimated_absorpt_T_min   0.686
_shelx_estimated_absorpt_T_max   0.879
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.79975
_exptl_absorpt_correction_T_max  0.93672
_exptl_absorpt_process_details   'SADABS V2016/2 (Bruker, 2014)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_monochromator  'multilayer mirrors'
_diffrn_measurement_device       'Bruker D8 Quest/Photon 100'
_diffrn_measurement_method       'profile data from φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            30347
_diffrn_reflns_av_unetI/netI     0.0498
_diffrn_reflns_av_R_equivalents  0.0470
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.267
_diffrn_reflns_theta_max         27.124
_diffrn_reflns_theta_full        25.242
_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             6495
_reflns_number_gt                5138
_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.
 
 _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       'APEX2 V2014.9-0 (Bruker, 2014)'
_computing_cell_refinement       'SAINT V8.37A (Bruker, 2005)'
_computing_data_reduction        
; 
SAINT V8.37A, XPREP v2014/2, SADABS V2016/2 (Bruker, 2014) 
;
_computing_structure_solution    'SHELX-2014-5 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELX-2014-7 (Sheldrick, 2015)'
_computing_molecular_graphics    'SHELXLE v817 (Hubschle, 2011)'
_computing_publication_material  'XCIF V2014-2 (Bruker, 2014)'

_refine_special_details          
; 
Structure was phased by direct methods (Sheldrick, 2015).  Systematic 
conditions suggested the ambiguous space group.  The space group choice 
was confirmed by successful convergence of the full-matrix least-squares 
refinement on F².  The final map had no significant features.  A final 
analysis of variance between observed and calculated structure factors 
showed little dependence on amplitude and resolution. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0215P)²+2.9766P] 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         6495
_refine_ls_number_parameters     533
_refine_ls_number_restraints     1176
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0309
_refine_ls_wR_factor_ref         0.0570
_refine_ls_wR_factor_gt          0.0524
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_restrained_S_all      0.931
_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
Nd1 Nd 0.48279(2) 0.59830(2) 0.40164(2) 0.01007(5) Uani 1 1 d . U . . .
O7 O 0.43955(19) 0.57050(9) 0.6373(2) 0.0197(5) Uani 1 1 d D U . . .
H7A H 0.374(3) 0.5789(14) 0.639(4) 0.030 Uiso 1 1 d D U . . .
H7B H 0.461(3) 0.5473(13) 0.676(4) 0.030 Uiso 1 1 d D U . . .
O8 O 0.5023(6) 0.5292(3) 0.8999(8) 0.034(3) Uani 0.317(8) 1 d . . P . .
N1 N 0.58560(19) 0.66776(9) 0.5732(2) 0.0117(5) Uani 1 1 d . U . . .
N2 N 0.44898(18) 0.69816(9) 0.3403(2) 0.0119(5) Uani 1 1 d . U . . .
N3 N 0.3733(2) 0.62159(10) 0.1578(3) 0.0187(6) Uani 1 1 d . U . . .
C1 C 0.6557(2) 0.65187(12) 0.6854(3) 0.0152(7) Uani 1 1 d . U . . .
H1 H 0.6608 0.6156 0.7048 0.018 Uiso 1 1 calc R U . . .
C2 C 0.7211(3) 0.68558(12) 0.7746(3) 0.0197(7) Uani 1 1 d . U . . .
H2 H 0.7697 0.6727 0.8530 0.024 Uiso 1 1 calc R U . . .
C3 C 0.7138(2) 0.73826(12) 0.7470(3) 0.0196(7) Uani 1 1 d . U . . .
H3 H 0.7569 0.7625 0.8066 0.024 Uiso 1 1 calc R U . . .
C4 C 0.6429(2) 0.75525(12) 0.6311(3) 0.0168(7) Uani 1 1 d . U . . .
H4 H 0.6374 0.7914 0.6098 0.020 Uiso 1 1 calc R U . . .
C5 C 0.5795(2) 0.71938(11) 0.5456(3) 0.0124(6) Uani 1 1 d . U . . .
C6 C 0.4992(2) 0.73611(11) 0.4227(3) 0.0127(6) Uani 1 1 d . U . . .
C7 C 0.4758(3) 0.78862(11) 0.3944(3) 0.0174(6) Uani 1 1 d . U . . .
H7 H 0.5116 0.8149 0.4542 0.021 Uiso 1 1 calc R U . . .
C8 C 0.4012(3) 0.80220(13) 0.2800(3) 0.0207(7) Uani 1 1 d . U . . .
H8 H 0.3850 0.8379 0.2593 0.025 Uiso 1 1 calc R U . . .
C9 C 0.3500(2) 0.76353(12) 0.1954(3) 0.0194(7) Uani 1 1 d . U . . .
H9 H 0.2981 0.7722 0.1154 0.023 Uiso 1 1 calc R U . . .
C10 C 0.3749(2) 0.71173(12) 0.2279(3) 0.0146(6) Uani 1 1 d . U . . .
C11 C 0.3248(2) 0.66891(12) 0.1370(3) 0.0166(7) Uani 1 1 d . U . . .
C12 C 0.2354(3) 0.67686(15) 0.0309(3) 0.0247(8) Uani 1 1 d . U . . .
H12 H 0.1991 0.7099 0.0204 0.030 Uiso 1 1 calc R U . . .
C13 C 0.1998(3) 0.63668(16) -0.0586(3) 0.0315(9) Uani 1 1 d . U . . .
H13 H 0.1396 0.6419 -0.1321 0.038 Uiso 1 1 calc R U . . .
C14 C 0.2518(3) 0.58914(15) -0.0410(3) 0.0348(9) Uani 1 1 d . U . . .
H14 H 0.2301 0.5611 -0.1031 0.042 Uiso 1 1 calc R U . . .
C15 C 0.3369(3) 0.58308(14) 0.0697(3) 0.0301(9) Uani 1 1 d . U . . .
H15 H 0.3714 0.5498 0.0839 0.036 Uiso 1 1 calc R U . . .
O1 O 0.58449(17) 0.55900(8) 0.2038(2) 0.0239(5) Uani 1 1 d . U . . .
O2 O 0.64717(16) 0.63388(8) 0.3004(2) 0.0164(5) Uani 1 1 d . U . . .
C16 C 0.6546(2) 0.59611(12) 0.2184(3) 0.0160(6) Uani 1 1 d D U . . .
S1 S 0.75684(17) 0.55698(9) -0.0022(2) 0.0167(4) Uani 0.690(3) 1 d D U P A 1
C17 C 0.7518(13) 0.5975(9) 0.138(2) 0.0123(11) Uani 0.690(3) 1 d D U P A 1
C18 C 0.8440(8) 0.6286(4) 0.1595(11) 0.0163(16) Uani 0.690(3) 1 d D U P A 1
H18 H 0.8550 0.6539 0.2316 0.020 Uiso 0.690(3) 1 calc R U P A 1
C19 C 0.9228(8) 0.6202(5) 0.0653(12) 0.0157(12) Uani 0.690(3) 1 d D U P A 1
H19 H 0.9921 0.6384 0.0675 0.019 Uiso 0.690(3) 1 calc R U P A 1
C20 C 0.8850(7) 0.5826(4) -0.0284(11) 0.0158(13) Uani 0.690(3) 1 d D U P A 1
H20 H 0.9252 0.5715 -0.1011 0.019 Uiso 0.690(3) 1 calc R U P A 1
S1A S 0.8569(5) 0.6367(3) 0.1849(6) 0.0157(10) Uani 0.310(3) 1 d D U P A 2
C17A C 0.747(3) 0.595(2) 0.132(5) 0.014(2) Uani 0.310(3) 1 d D U P A 2
C18A C 0.7652(14) 0.5657(8) 0.0212(19) 0.016(2) Uani 0.310(3) 1 d D U P A 2
H18A H 0.7134 0.5400 -0.0191 0.019 Uiso 0.310(3) 1 calc R U P A 2
C19A C 0.8683(16) 0.5763(10) -0.029(2) 0.017(2) Uani 0.310(3) 1 d D U P A 2
H19A H 0.8935 0.5600 -0.1072 0.021 Uiso 0.310(3) 1 calc R U P A 2
C20A C 0.9255(18) 0.6135(11) 0.052(3) 0.016(2) Uani 0.310(3) 1 d D U P A 2
H20A H 0.9975 0.6258 0.0369 0.019 Uiso 0.310(3) 1 calc R U P A 2
O3 O 0.36393(16) 0.45246(8) 0.4880(2) 0.0175(5) Uani 1 1 d . U . . .
O4 O 0.37986(16) 0.51997(8) 0.3473(2) 0.0169(5) Uani 1 1 d . U . . .
C21 C 0.3224(2) 0.48714(11) 0.4033(3) 0.0114(6) Uani 1 1 d D U . . .
S2 S 0.12867(19) 0.53494(9) 0.2625(3) 0.0166(5) Uani 0.540(3) 1 d D U P B 1
C22 C 0.1985(2) 0.48750(10) 0.3683(3) 0.0110(6) Uani 0.540(3) 1 d D U P B 1
C23 C 0.1244(8) 0.4533(3) 0.4115(12) 0.0146(17) Uani 0.540(3) 1 d D U P B 1
H23 H 0.1474 0.4255 0.4739 0.018 Uiso 0.540(3) 1 calc R U P B 1
C24 C 0.0098(8) 0.4621(6) 0.357(2) 0.0168(16) Uani 0.540(3) 1 d D U P B 1
H24 H -0.0514 0.4403 0.3719 0.020 Uiso 0.540(3) 1 calc R U P B 1
C25 C 0.0011(8) 0.5063(6) 0.279(2) 0.0161(16) Uani 0.540(3) 1 d D U P B 1
H25 H -0.0690 0.5203 0.2371 0.019 Uiso 0.540(3) 1 calc R U P B 1
S2A S 0.1225(2) 0.43795(11) 0.4279(4) 0.0149(7) Uani 0.460(3) 1 d D U P B 2
C22A C 0.1985(2) 0.48750(10) 0.3683(3) 0.0110(6) Uani 0.460(3) 1 d D U P B 2
C23A C 0.1325(8) 0.5229(4) 0.2915(13) 0.0165(19) Uani 0.460(3) 1 d D U P B 2
H23A H 0.1617 0.5528 0.2508 0.020 Uiso 0.460(3) 1 calc R U P B 2
C24A C 0.0159(9) 0.5111(7) 0.278(2) 0.0178(18) Uani 0.460(3) 1 d D U P B 2
H24A H -0.0422 0.5309 0.2249 0.021 Uiso 0.460(3) 1 calc R U P B 2
C25A C -0.0004(9) 0.4673(7) 0.351(3) 0.0143(18) Uani 0.460(3) 1 d D U P B 2
H25A H -0.0731 0.4540 0.3597 0.017 Uiso 0.460(3) 1 calc R U P B 2
O5 O 0.22498(16) 0.60198(8) 0.6221(2) 0.0175(5) Uani 1 1 d . U . . .
O6 O 0.29451(16) 0.63029(8) 0.4325(2) 0.0157(5) Uani 1 1 d . U . . .
C26 C 0.2216(2) 0.62920(11) 0.5148(3) 0.0122(6) Uani 1 1 d D U . . .
S3 S 0.1133(2) 0.70497(12) 0.3399(3) 0.0173(5) Uani 0.583(3) 1 d D U P C 1
C27 C 0.1245(2) 0.66596(12) 0.4820(3) 0.0139(6) Uani 0.583(3) 1 d D U P C 1
C28 C 0.0389(10) 0.6758(6) 0.5594(10) 0.0210(18) Uani 0.583(3) 1 d D U P C 1
H28 H 0.0318 0.6574 0.6428 0.025 Uiso 0.583(3) 1 calc R U P C 1
C29 C -0.0372(12) 0.7150(4) 0.5066(13) 0.0208(16) Uani 0.583(3) 1 d D U P C 1
H29 H -0.1014 0.7258 0.5466 0.025 Uiso 0.583(3) 1 calc R U P C 1
C30 C -0.0043(10) 0.7349(6) 0.3894(13) 0.0155(16) Uani 0.583(3) 1 d D U P C 1
H30 H -0.0424 0.7629 0.3386 0.019 Uiso 0.583(3) 1 calc R U P C 1
S3A S 0.0319(4) 0.6758(2) 0.5951(4) 0.0255(9) Uani 0.417(3) 1 d D U P C 2
C27A C 0.1245(2) 0.66596(12) 0.4820(3) 0.0139(6) Uani 0.417(3) 1 d D U P C 2
C28A C 0.1030(13) 0.7000(6) 0.3709(13) 0.017(2) Uani 0.417(3) 1 d D U P C 2
H28A H 0.1488 0.7011 0.2985 0.020 Uiso 0.417(3) 1 calc R U P C 2
C29A C 0.0094(15) 0.7330(9) 0.3716(19) 0.019(2) Uani 0.417(3) 1 d D U P C 2
H29A H -0.0185 0.7570 0.3005 0.022 Uiso 0.417(3) 1 calc R U P C 2
C30A C -0.0341(16) 0.7246(6) 0.4910(18) 0.020(2) Uani 0.417(3) 1 d D U P C 2
H30A H -0.0959 0.7439 0.5156 0.023 Uiso 0.417(3) 1 calc R U P C 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

_exptl_special_details           
; 
One distinct cell was identified using APEX2 (Bruker, 2014).  Three 
frame series were integrated and filtered for statistical outliers 
using SAINT (Bruker, 2014) then corrected for absorption by integration 
using SAINT/SADABS v2014/2 (Bruker, 2014) to sort, merge, and scale 
the combined data.  No decay correction was applied.    
;

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
2.00 -1.00 1.00 0.0240
-2.00 1.00 -1.00 0.0360
0.00 2.00 -1.00 0.0490
-1.00 1.00 -1.00 0.0380
1.00 -1.00 1.00 0.0330
1.00 2.00 2.00 0.0370
-1.00 -2.00 -2.00 0.0320
2.00 0.00 1.00 0.0190
-2.00 0.00 -1.00 0.0320
0.00 1.00 0.00 0.0870
0.00 -1.00 0.00 0.1040
-4.00 0.00 -1.00 0.0310
4.00 0.00 1.00 0.0090
-4.00 -1.00 1.00 0.0320
4.00 1.00 -1.00 0.0140
0.00 1.00 1.00 0.0420

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
Nd1 O4 2.3768(19) . ?
Nd1 O3 2.3792(19) 3_666 ?
Nd1 O6 2.4588(19) . ?
Nd1 O2 2.494(2) . ?
Nd1 O7 2.514(2) . ?
Nd1 N3 2.606(2) . ?
Nd1 O1 2.614(2) . ?
Nd1 N1 2.622(2) . ?
Nd1 N2 2.646(2) . ?
Nd1 C16 2.903(3) . ?
O7 H7A 0.82(3) . ?
O7 H7B 0.73(3) . ?
N1 C1 1.341(3) . ?
N1 C5 1.350(4) . ?
N2 C6 1.346(4) . ?
N2 C10 1.351(4) . ?
N3 C15 1.338(4) . ?
N3 C11 1.348(4) . ?
C1 C2 1.385(4) . ?
C1 H1 0.9500 . ?
C2 C3 1.377(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.381(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.390(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.486(4) . ?
C6 C7 1.394(4) . ?
C7 C8 1.368(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.374(4) . ?
C8 H8 0.9500 . ?
C9 C10 1.387(4) . ?
C9 H9 0.9500 . ?
C10 C11 1.480(4) . ?
C11 C12 1.393(4) . ?
C12 C13 1.375(5) . ?
C12 H12 0.9500 . ?
C13 C14 1.369(5) . ?
C13 H13 0.9500 . ?
C14 C15 1.381(5) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
O1 C16 1.264(4) . ?
O2 C16 1.264(4) . ?
C16 C17A 1.479(7) . ?
C16 C17 1.489(5) . ?
S1 C17 1.719(5) . ?
S1 C20 1.722(6) . ?
C17 C18 1.355(8) . ?
C18 C19 1.419(10) . ?
C18 H18 0.9500 . ?
C19 C20 1.358(5) . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?
S1A C17A 1.718(8) . ?
S1A C20A 1.728(10) . ?
C17A C18A 1.353(10) . ?
C18A C19A 1.418(12) . ?
C18A H18A 0.9500 . ?
C19A C20A 1.358(8) . ?
C19A H19A 0.9500 . ?
C20A H20A 0.9500 . ?
O3 C21 1.264(3) . ?
O3 Nd1 2.3791(19) 3_666 ?
O4 C21 1.258(3) . ?
C21 C22A 1.477(4) . ?
C21 C22 1.477(4) . ?
S2 C25 1.723(8) . ?
S2 C22 1.729(3) . ?
C22 C23 1.356(8) . ?
C23 C24 1.419(11) . ?
C23 H23 0.9500 . ?
C24 C25 1.359(6) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
S2A C22A 1.710(3) . ?
S2A C25A 1.727(9) . ?
C22A C23A 1.356(8) . ?
C23A C24A 1.419(11) . ?
C23A H23A 0.9500 . ?
C24A C25A 1.360(7) . ?
C24A H24A 0.9500 . ?
C25A H25A 0.9500 . ?
O5 C26 1.249(3) . ?
O6 C26 1.263(3) . ?
C26 C27A 1.497(4) . ?
C26 C27 1.497(4) . ?
S3 C27 1.692(3) . ?
S3 C30 1.730(9) . ?
C27 C28 1.377(10) . ?
C28 C29 1.404(15) . ?
C28 H28 0.9500 . ?
C29 C30 1.354(7) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?
S3A C27A 1.684(4) . ?
S3A C30A 1.727(11) . ?
C27A C28A 1.382(11) . ?
C28A C29A 1.406(17) . ?
C28A H28A 0.9500 . ?
C29A C30A 1.350(8) . ?
C29A H29A 0.9500 . ?
C30A H30A 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
O4 Nd1 O3 88.95(7) . 3_666 ?
O4 Nd1 O6 81.48(7) . . ?
O3 Nd1 O6 142.37(7) 3_666 . ?
O4 Nd1 O2 129.51(7) . . ?
O3 Nd1 O2 76.92(7) 3_666 . ?
O6 Nd1 O2 135.67(6) . . ?
O4 Nd1 O7 78.17(7) . . ?
O3 Nd1 O7 71.44(7) 3_666 . ?
O6 Nd1 O7 70.99(7) . . ?
O2 Nd1 O7 137.38(7) . . ?
O4 Nd1 N3 79.21(7) . . ?
O3 Nd1 N3 142.34(8) 3_666 . ?
O6 Nd1 N3 71.31(7) . . ?
O2 Nd1 N3 83.39(7) . . ?
O7 Nd1 N3 138.27(8) . . ?
O4 Nd1 O1 78.06(7) . . ?
O3 Nd1 O1 73.05(7) 3_666 . ?
O6 Nd1 O1 138.45(7) . . ?
O2 Nd1 O1 51.45(6) . . ?
O7 Nd1 O1 137.19(7) . . ?
N3 Nd1 O1 69.57(8) . . ?
O4 Nd1 N1 153.79(7) . . ?
O3 Nd1 N1 79.74(7) 3_666 . ?
O6 Nd1 N1 93.11(7) . . ?
O2 Nd1 N1 70.97(7) . . ?
O7 Nd1 N1 75.84(7) . . ?
N3 Nd1 N1 123.45(7) . . ?
O1 Nd1 N1 120.03(7) . . ?
O4 Nd1 N2 135.16(7) . . ?
O3 Nd1 N2 135.58(7) 3_666 . ?
O6 Nd1 N2 65.82(7) . . ?
O2 Nd1 N2 70.27(7) . . ?
O7 Nd1 N2 115.68(7) . . ?
N3 Nd1 N2 62.17(8) . . ?
O1 Nd1 N2 106.30(7) . . ?
N1 Nd1 N2 61.90(7) . . ?
O4 Nd1 C16 103.84(8) . . ?
O3 Nd1 C16 72.22(8) 3_666 . ?
O6 Nd1 C16 145.40(7) . . ?
O2 Nd1 C16 25.68(7) . . ?
O7 Nd1 C16 143.56(8) . . ?
N3 Nd1 C16 76.13(8) . . ?
O1 Nd1 C16 25.82(7) . . ?
N1 Nd1 C16 95.17(8) . . ?
N2 Nd1 C16 88.90(8) . . ?
Nd1 O7 H7A 106(2) . . ?
Nd1 O7 H7B 126(3) . . ?
H7A O7 H7B 118(4) . . ?
C1 N1 C5 117.9(2) . . ?
C1 N1 Nd1 119.55(19) . . ?
C5 N1 Nd1 122.18(18) . . ?
C6 N2 C10 118.8(3) . . ?
C6 N2 Nd1 121.63(18) . . ?
C10 N2 Nd1 119.52(19) . . ?
C15 N3 C11 118.3(3) . . ?
C15 N3 Nd1 119.2(2) . . ?
C11 N3 Nd1 119.54(19) . . ?
N1 C1 C2 123.5(3) . . ?
N1 C1 H1 118.2 . . ?
C2 C1 H1 118.2 . . ?
C3 C2 C1 118.4(3) . . ?
C3 C2 H2 120.8 . . ?
C1 C2 H2 120.8 . . ?
C2 C3 C4 118.9(3) . . ?
C2 C3 H3 120.6 . . ?
C4 C3 H3 120.6 . . ?
C3 C4 C5 119.9(3) . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
N1 C5 C4 121.4(3) . . ?
N1 C5 C6 116.9(3) . . ?
C4 C5 C6 121.7(3) . . ?
N2 C6 C7 121.3(3) . . ?
N2 C6 C5 116.9(3) . . ?
C7 C6 C5 121.8(3) . . ?
C8 C7 C6 119.7(3) . . ?
C8 C7 H7 120.1 . . ?
C6 C7 H7 120.1 . . ?
C7 C8 C9 119.1(3) . . ?
C7 C8 H8 120.5 . . ?
C9 C8 H8 120.5 . . ?
C8 C9 C10 119.4(3) . . ?
C8 C9 H9 120.3 . . ?
C10 C9 H9 120.3 . . ?
N2 C10 C9 121.7(3) . . ?
N2 C10 C11 117.0(3) . . ?
C9 C10 C11 121.2(3) . . ?
N3 C11 C12 120.9(3) . . ?
N3 C11 C10 116.7(3) . . ?
C12 C11 C10 122.4(3) . . ?
C13 C12 C11 119.6(3) . . ?
C13 C12 H12 120.2 . . ?
C11 C12 H12 120.2 . . ?
C14 C13 C12 119.5(3) . . ?
C14 C13 H13 120.2 . . ?
C12 C13 H13 120.2 . . ?
C13 C14 C15 118.1(3) . . ?
C13 C14 H14 120.9 . . ?
C15 C14 H14 120.9 . . ?
N3 C15 C14 123.5(3) . . ?
N3 C15 H15 118.3 . . ?
C14 C15 H15 118.3 . . ?
C16 O1 Nd1 89.98(18) . . ?
C16 O2 Nd1 95.56(17) . . ?
O2 C16 O1 122.8(3) . . ?
O2 C16 C17A 119.6(9) . . ?
O1 C16 C17A 117.5(9) . . ?
O2 C16 C17 116.1(5) . . ?
O1 C16 C17 121.1(5) . . ?
O2 C16 Nd1 58.77(15) . . ?
O1 C16 Nd1 64.20(16) . . ?
C17A C16 Nd1 176.9(19) . . ?
C17 C16 Nd1 173.4(5) . . ?
C17 S1 C20 91.0(3) . . ?
C18 C17 C16 128.0(6) . . ?
C18 C17 S1 110.9(4) . . ?
C16 C17 S1 121.0(4) . . ?
C17 C18 C19 114.6(7) . . ?
C17 C18 H18 122.7 . . ?
C19 C18 H18 122.7 . . ?
C20 C19 C18 110.3(8) . . ?
C20 C19 H19 124.8 . . ?
C18 C19 H19 124.8 . . ?
C19 C20 S1 113.1(7) . . ?
C19 C20 H20 123.4 . . ?
S1 C20 H20 123.4 . . ?
C17A S1A C20A 89.4(6) . . ?
C18A C17A C16 132.6(10) . . ?
C18A C17A S1A 112.3(6) . . ?
C16 C17A S1A 115.0(7) . . ?
C17A C18A C19A 114.3(10) . . ?
C17A C18A H18A 122.9 . . ?
C19A C18A H18A 122.9 . . ?
C20A C19A C18A 109.3(13) . . ?
C20A C19A H19A 125.4 . . ?
C18A C19A H19A 125.4 . . ?
C19A C20A S1A 114.7(12) . . ?
C19A C20A H20A 122.6 . . ?
S1A C20A H20A 122.6 . . ?
C21 O3 Nd1 152.33(19) . 3_666 ?
C21 O4 Nd1 140.20(18) . . ?
O4 C21 O3 124.1(3) . . ?
O4 C21 C22A 119.4(3) . . ?
O3 C21 C22A 116.5(2) . . ?
O4 C21 C22 119.4(3) . . ?
O3 C21 C22 116.5(2) . . ?
C25 S2 C22 90.5(4) . . ?
C23 C22 C21 127.3(4) . . ?
C23 C22 S2 110.8(4) . . ?
C21 C22 S2 121.9(2) . . ?
C22 C23 C24 115.0(8) . . ?
C22 C23 H23 122.5 . . ?
C24 C23 H23 122.5 . . ?
C25 C24 C23 109.6(10) . . ?
C25 C24 H24 125.2 . . ?
C23 C24 H24 125.2 . . ?
C24 C25 S2 114.0(9) . . ?
C24 C25 H25 123.0 . . ?
S2 C25 H25 123.0 . . ?
C22A S2A C25A 89.7(5) . . ?
C23A C22A C21 128.4(5) . . ?
C23A C22A S2A 112.7(4) . . ?
C21 C22A S2A 118.9(2) . . ?
C22A C23A C24A 113.6(8) . . ?
C22A C23A H23A 123.2 . . ?
C24A C23A H23A 123.2 . . ?
C25A C24A C23A 109.8(11) . . ?
C25A C24A H24A 125.1 . . ?
C23A C24A H24A 125.1 . . ?
C24A C25A S2A 114.1(11) . . ?
C24A C25A H25A 122.9 . . ?
S2A C25A H25A 122.9 . . ?
C26 O6 Nd1 142.91(19) . . ?
O5 C26 O6 126.4(3) . . ?
O5 C26 C27A 117.5(3) . . ?
O6 C26 C27A 116.0(3) . . ?
O5 C26 C27 117.5(3) . . ?
O6 C26 C27 116.0(3) . . ?
C27 S3 C30 90.7(5) . . ?
C28 C27 C26 128.1(5) . . ?
C28 C27 S3 110.8(5) . . ?
C26 C27 S3 121.0(2) . . ?
C27 C28 C29 115.3(10) . . ?
C27 C28 H28 122.3 . . ?
C29 C28 H28 122.3 . . ?
C30 C29 C28 108.9(13) . . ?
C30 C29 H29 125.5 . . ?
C28 C29 H29 125.5 . . ?
C29 C30 S3 114.2(12) . . ?
C29 C30 H30 122.9 . . ?
S3 C30 H30 122.9 . . ?
C27A S3A C30A 91.0(7) . . ?
C28A C27A C26 128.1(6) . . ?
C28A C27A S3A 110.1(5) . . ?
C26 C27A S3A 121.3(2) . . ?
C27A C28A C29A 115.9(12) . . ?
C27A C28A H28A 122.0 . . ?
C29A C28A H28A 122.0 . . ?
C30A C29A C28A 108.3(17) . . ?
C30A C29A H29A 125.9 . . ?
C28A C29A H29A 125.9 . . ?
C29A C30A S3A 114.5(16) . . ?
C29A C30A H30A 122.7 . . ?
S3A C30A H30A 122.7 . . ?

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
O7 H7A O5 0.82(3) 1.86(3) 2.680(3) 173(4) .
O7 H7A O6 0.82(3) 2.47(3) 2.888(3) 112(3) .
O7 H7B O8 0.73(3) 2.21(3) 2.762(7) 134(4) .
O7 H7B O4 0.73(3) 2.60(3) 3.162(3) 135(4) 3_666

_refine_diff_density_max         0.460
_refine_diff_density_min         -0.560
_refine_diff_density_rms         0.111

####################################################################### 
# 
# 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_final_a_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 1544444'
_audit_update_record             
;
2017-04-17 deposited with the CCDC.
2017-08-23 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT415_final_a             
;
PROBLEM: Short Inter D-H..H-X       H15    ..  H8A     ..       2.06 Ang.
RESPONSE: H8A is a water hydrogen atom that was found in the difference map in a good hydrogen bond location. H8A is part of a partially occupied lattice water molecule and is 20% occupied.
;
# Added during the CSD deposition process: Monday 17 April 2017 03:19 PM
# end Validation Reply Form



_audit_creation_date             2017-04-06
_audit_creation_method           
;
Olex2 1.2
(compiled Mar 28 2017 19:26:29 for OlexSys, GUI svn.r5335)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C60 H44 N6 O14 S6 Sm2, 0.42(H2 O)'
_chemical_formula_sum            'C60 H44.84 N6 O14.42 S6 Sm2'
_chemical_formula_weight         1573.64
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   11.9398(4)
_cell_length_b                   25.4924(11)
_cell_length_c                   9.7089(4)
_cell_angle_alpha                90
_cell_angle_beta                 97.9830(10)
_cell_angle_gamma                90
_cell_volume                     2926.5(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9889
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.38
_cell_measurement_theta_min      2.26
_shelx_estimated_absorpt_T_max   0.914
_shelx_estimated_absorpt_T_min   0.772
_exptl_absorpt_coefficient_mu    2.275
_exptl_absorpt_correction_T_max  0.9579
_exptl_absorpt_correction_T_min  0.8744
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.0713 before and 0.0477 after correction.
The Ratio of minimum to maximum transmission is 0.9128.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.786
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       rhombus
_exptl_crystal_F_000             1564
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.106
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0398
_diffrn_reflns_av_unetI/netI     0.0371
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            29934
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.389
_diffrn_reflns_theta_min         2.349
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5012
_reflns_number_total             5971
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.451
_refine_diff_density_min         -0.556
_refine_diff_density_rms         0.094
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     525
_refine_ls_number_reflns         5971
_refine_ls_number_restraints     378
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_gt           0.0258
_refine_ls_restrained_S_all      1.024
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0144P)²+2.6849P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0439
_refine_ls_wR_factor_ref         0.0463
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O8-H8B = O8-H8A
 0.86 with sigma of 0.02
 H8A-H8B
 1.35 with sigma of 0.02
 S1A-C17 \\sim S1-C17
 with sigma of 0.02
 S1-C20 \\sim S1A-C20A
 with sigma of 0.02
 C20-C19 \\sim C20A-C19A
 with sigma of 0.02
 C18A-C17 \\sim C18-C17
 with sigma of 0.02
 C19A-C18A \\sim C19-C18
 with sigma of 0.02
 S2A-C22 \\sim S2-C22
 with sigma of 0.02
 S2A-C25A \\sim S2-C25
 with sigma of 0.02
 C25-C24 \\sim C25A-C24A
 with sigma of 0.02
 C23-C22 \\sim C23A-C22
 with sigma of 0.02
 C24A-C23A \\sim C24-C23
 with sigma of 0.02
 S3-C27 \\sim S3A-C27
 with sigma of 0.02
 S3-C30 \\sim S3A-C30A
 with sigma of 0.02
 C30-C29 \\sim C30A-C29A
 with sigma of 0.02
 C28A-C27 \\sim C28-C27
 with sigma of 0.02
 C29A-C28A \\sim C29-C28
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
S1 \\sim S1 \\sim S1 \\sim S1A \\sim S1A \\sim S1A \\sim C17 \\sim C17 \\sim
C17 \\sim C17 \\sim C17 \\sim C18 \\sim C18 \\sim C18 \\sim C18A \\sim C18A
\\sim C18A \\sim C19 \\sim C19 \\sim C19 \\sim C19A \\sim C19A \\sim C19A \\sim
C20 \\sim C20 \\sim C20 \\sim C20A \\sim C20A \\sim C20A: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02
S2 \\sim S2 \\sim S2 \\sim S2A \\sim S2A \\sim S2A \\sim C22 \\sim C22 \\sim
C22 \\sim C22 \\sim C22 \\sim C23 \\sim C23 \\sim C23 \\sim C23A \\sim C23A
\\sim C23A \\sim C24 \\sim C24 \\sim C24 \\sim C24A \\sim C24A \\sim C24A \\sim
C25 \\sim C25 \\sim C25 \\sim C25A \\sim C25A \\sim C25A: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02
S3 \\sim S3 \\sim S3 \\sim S3A \\sim S3A \\sim S3A \\sim C27 \\sim C27 \\sim
C27 \\sim C27 \\sim C27 \\sim C28 \\sim C28 \\sim C28 \\sim C28A \\sim C28A
\\sim C28A \\sim C29 \\sim C29 \\sim C29 \\sim C29A \\sim C29A \\sim C29A \\sim
C30 \\sim C30 \\sim C30 \\sim C30A \\sim C30A \\sim C30A: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(S1A)=Sof(C18A)=Sof(H18A)=Sof(C19A)=Sof(H19A)=Sof(C20A)=Sof(H20A)=1-FVAR(1)
 Sof(S1)=Sof(C18)=Sof(H18)=Sof(C19)=Sof(H19)=Sof(C20)=Sof(H20)=FVAR(1)
 Sof(S2A)=Sof(C23A)=Sof(H23A)=Sof(C24A)=Sof(H24A)=Sof(C25A)=Sof(H25A)=1-FVAR(2)
 Sof(S2)=Sof(C23)=Sof(H23)=Sof(C24)=Sof(H24)=Sof(C25)=Sof(H25)=FVAR(2)
 Sof(S3A)=Sof(C28A)=Sof(H28A)=Sof(C29A)=Sof(H29A)=Sof(C30A)=Sof(H30A)=1-FVAR(3)
 Sof(S3)=Sof(C28)=Sof(H28)=Sof(C29)=Sof(H29)=Sof(C30)=Sof(H30)=FVAR(3)
 Sof(O8)=Sof(H8A)=Sof(H8B)=FVAR(4)
5.a Rotating group:
 O7(H7A,H7B)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C12(H12), C13(H13),
 C14(H14), C15(H15), C18(H18), C18A(H18A), C19(H19), C19A(H19A), C20(H20),
 C20A(H20A), C23(H23), C23A(H23A), C24(H24), C24A(H24A), C25(H25), C25A(H25A),
 C28(H28), C28A(H28A), C29(H29), C29A(H29A), C30(H30), C30A(H30A)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Sm1 Sm 0.51625(2) 0.59810(2) 0.59925(2) 0.00923(4) Uani 1 1 d . . . . .
S1 S 0.2428(2) 0.55737(9) 1.0026(2) 0.0156(5) Uani 0.697(3) 1 d D U P A 1
S1A S 0.1427(6) 0.6373(3) 0.8139(7) 0.0136(12) Uani 0.303(3) 1 d D U P A 2
S2 S 0.8694(3) 0.53497(11) 0.7394(3) 0.0153(6) Uani 0.539(3) 1 d D U P B 1
S2A S 0.8774(3) 0.43838(12) 0.5709(4) 0.0143(7) Uani 0.461(3) 1 d D U P B 2
S3 S 0.9667(5) 0.6758(2) 0.4052(4) 0.0222(9) Uani 0.415(3) 1 d D U P C 1
S3A S 0.8853(3) 0.70524(13) 0.6607(3) 0.0151(6) Uani 0.585(3) 1 d D U P C 2
O1 O 0.41321(15) 0.55752(7) 0.7931(2) 0.0220(5) Uani 1 1 d . . . . .
O2 O 0.35336(14) 0.63359(7) 0.69868(19) 0.0147(4) Uani 1 1 d . . . . .
O3 O 0.61773(14) 0.51990(7) 0.65154(18) 0.0154(4) Uani 1 1 d . . . . .
O4 O 0.63574(14) 0.45269(7) 0.50912(19) 0.0150(4) Uani 1 1 d . . . . .
O5 O 0.77373(14) 0.60134(7) 0.37972(18) 0.0164(4) Uani 1 1 d . . . . .
O6 O 0.70370(14) 0.62965(7) 0.56912(18) 0.0149(4) Uani 1 1 d . . . . .
O7 O 0.55856(15) 0.56986(7) 0.36547(18) 0.0167(4) Uani 1 1 d . . . . .
H7A H 0.5413 0.5360 0.3504 0.025 Uiso 1 1 d GR . . . .
H7B H 0.6323 0.5741 0.3594 0.025 Uiso 1 1 d GR . . . .
O8 O 0.5031(8) 0.4691(3) 0.8957(9) 0.022(3) Uani 0.211(6) 1 d D . P . .
H8A H 0.480(11) 0.501(2) 0.877(12) 0.033 Uiso 0.211(6) 1 d DR . P . .
H8B H 0.524(12) 0.470(5) 0.984(3) 0.033 Uiso 0.211(6) 1 d DR . P . .
N1 N 0.41460(17) 0.66712(8) 0.4281(2) 0.0113(5) Uani 1 1 d . . . . .
N2 N 0.55037(17) 0.69709(8) 0.6609(2) 0.0112(5) Uani 1 1 d . . . . .
N3 N 0.62396(19) 0.61982(9) 0.8421(2) 0.0183(5) Uani 1 1 d . . . . .
C1 C 0.3447(2) 0.65116(11) 0.3155(3) 0.0152(6) Uani 1 1 d . . . . .
H1 H 0.3399 0.6147 0.2958 0.018 Uiso 1 1 calc R . . . .
C2 C 0.2793(2) 0.68514(11) 0.2267(3) 0.0179(6) Uani 1 1 d . . . . .
H2 H 0.2309 0.6723 0.1481 0.021 Uiso 1 1 calc R . . . .
C3 C 0.2865(2) 0.73811(11) 0.2555(3) 0.0183(6) Uani 1 1 d . . . . .
H3 H 0.2432 0.7625 0.1963 0.022 Uiso 1 1 calc R . . . .
C4 C 0.3571(2) 0.75523(10) 0.3713(3) 0.0151(6) Uani 1 1 d . . . . .
H4 H 0.3624 0.7916 0.3930 0.018 Uiso 1 1 calc R . . . .
C5 C 0.4207(2) 0.71885(10) 0.4562(3) 0.0120(6) Uani 1 1 d . . . . .
C6 C 0.5010(2) 0.73541(10) 0.5791(3) 0.0121(6) Uani 1 1 d . . . . .
C7 C 0.5247(2) 0.78844(10) 0.6072(3) 0.0159(6) Uani 1 1 d . . . . .
H7 H 0.4894 0.8149 0.5472 0.019 Uiso 1 1 calc R . . . .
C8 C 0.5994(2) 0.80177(11) 0.7224(3) 0.0199(7) Uani 1 1 d . . . . .
H8 H 0.6160 0.8376 0.7436 0.024 Uiso 1 1 calc R . . . .
C9 C 0.6498(2) 0.76263(11) 0.8066(3) 0.0183(6) Uani 1 1 d . . . . .
H9 H 0.7015 0.7712 0.8868 0.022 Uiso 1 1 calc R . . . .
C10 C 0.6247(2) 0.71026(11) 0.7737(3) 0.0142(6) Uani 1 1 d . . . . .
C11 C 0.6735(2) 0.66701(11) 0.8643(3) 0.0152(6) Uani 1 1 d . . . . .
C12 C 0.7629(2) 0.67447(13) 0.9707(3) 0.0233(7) Uani 1 1 d . . . . .
H12 H 0.8008 0.7073 0.9815 0.028 Uiso 1 1 calc R . . . .
C13 C 0.7957(3) 0.63368(14) 1.0603(3) 0.0305(8) Uani 1 1 d . . . . .
H13 H 0.8558 0.6384 1.1343 0.037 Uiso 1 1 calc R . . . .
C14 C 0.7412(3) 0.58622(13) 1.0422(3) 0.0317(8) Uani 1 1 d . . . . .
H14 H 0.7605 0.5580 1.1050 0.038 Uiso 1 1 calc R . . . .
C15 C 0.6578(3) 0.58084(12) 0.9306(3) 0.0290(8) Uani 1 1 d . . . . .
H15 H 0.6222 0.5476 0.9152 0.035 Uiso 1 1 calc R . . . .
C16 C 0.3443(2) 0.59536(11) 0.7799(3) 0.0146(6) Uani 1 1 d . . . . .
C17 C 0.2489(2) 0.59677(10) 0.8632(3) 0.0127(5) Uani 1 1 d D U . . .
C18 C 0.1535(10) 0.6286(5) 0.8405(12) 0.015(2) Uani 0.697(3) 1 d D U P A 1
H18 H 0.1427 0.6536 0.7672 0.017 Uiso 0.697(3) 1 calc R . P A 1
C18A C 0.233(2) 0.5659(9) 0.979(2) 0.015(3) Uani 0.303(3) 1 d D U P A 2
H18A H 0.2851 0.5399 1.0161 0.018 Uiso 0.303(3) 1 calc R . P A 2
C19 C 0.0741(10) 0.6215(4) 0.9330(10) 0.0131(14) Uani 0.697(3) 1 d D U P A 1
H19 H 0.0046 0.6398 0.9306 0.016 Uiso 0.697(3) 1 calc R . P A 1
C19A C 0.1328(18) 0.5765(10) 1.033(3) 0.015(2) Uani 0.303(3) 1 d D U P A 2
H19A H 0.1079 0.5606 1.1123 0.018 Uiso 0.303(3) 1 calc R . P A 2
C20 C 0.1135(7) 0.5839(4) 1.0265(12) 0.0138(15) Uani 0.697(3) 1 d D U P A 1
H20 H 0.0732 0.5730 1.0993 0.017 Uiso 0.697(3) 1 calc R . P A 1
C20A C 0.079(3) 0.6139(11) 0.952(3) 0.014(3) Uani 0.303(3) 1 d D U P A 2
H20A H 0.0083 0.6272 0.9694 0.017 Uiso 0.303(3) 1 calc R . P A 2
C21 C 0.6758(2) 0.48703(10) 0.5943(3) 0.0120(6) Uani 1 1 d . . . . .
C22 C 0.8000(2) 0.48773(9) 0.6313(3) 0.0099(5) Uani 1 1 d D U . . .
C23 C 0.8770(11) 0.4537(4) 0.5882(14) 0.016(2) Uani 0.539(3) 1 d D U P B 1
H23 H 0.8543 0.4260 0.5251 0.019 Uiso 0.539(3) 1 calc R . P B 1
C23A C 0.8671(12) 0.5233(5) 0.7079(13) 0.016(2) Uani 0.461(3) 1 d D U P B 2
H23A H 0.8371 0.5533 0.7481 0.019 Uiso 0.461(3) 1 calc R . P B 2
C24 C 0.9932(17) 0.4620(8) 0.643(3) 0.0157(19) Uani 0.539(3) 1 d D U P B 1
H24 H 1.0559 0.4411 0.6266 0.019 Uiso 0.539(3) 1 calc R . P B 1
C24A C 0.9853(18) 0.5127(9) 0.724(3) 0.016(2) Uani 0.461(3) 1 d D U P B 2
H24A H 1.0442 0.5325 0.7754 0.019 Uiso 0.461(3) 1 calc R . P B 2
C25 C 0.9956(15) 0.5056(7) 0.722(3) 0.015(2) Uani 0.539(3) 1 d D U P B 1
H25 H 1.0651 0.5195 0.7670 0.018 Uiso 0.539(3) 1 calc R . P B 1
C25A C 0.996(2) 0.4685(9) 0.650(3) 0.015(2) Uani 0.461(3) 1 d D U P B 2
H25A H 1.0690 0.4545 0.6431 0.017 Uiso 0.461(3) 1 calc R . P B 2
C26 C 0.7772(2) 0.62881(10) 0.4864(3) 0.0116(6) Uani 1 1 d . . . . .
C27 C 0.8743(2) 0.66564(10) 0.5192(3) 0.0132(6) Uani 1 1 d D U . . .
C28 C 0.8951(15) 0.7008(7) 0.6277(15) 0.017(3) Uani 0.415(3) 1 d D U P C 1
H28 H 0.8477 0.7025 0.6985 0.020 Uiso 0.415(3) 1 calc R . P C 1
C28A C 0.9599(12) 0.6752(7) 0.4426(11) 0.021(2) Uani 0.585(3) 1 d D U P C 2
H28A H 0.9676 0.6561 0.3605 0.025 Uiso 0.585(3) 1 calc R . P C 2
C29 C 0.9899(19) 0.7340(12) 0.629(2) 0.017(2) Uani 0.415(3) 1 d D U P C 1
H29 H 1.0186 0.7579 0.7003 0.020 Uiso 0.415(3) 1 calc R . P C 1
C29A C 1.0361(15) 0.7154(5) 0.4933(16) 0.0193(18) Uani 0.585(3) 1 d D U P C 2
H29A H 1.1000 0.7264 0.4525 0.023 Uiso 0.585(3) 1 calc R . P C 2
C30 C 1.032(2) 0.7249(7) 0.508(2) 0.018(2) Uani 0.415(3) 1 d D U P C 1
H30 H 1.0933 0.7445 0.4817 0.022 Uiso 0.415(3) 1 calc R . P C 1
C30A C 1.0025(13) 0.7355(8) 0.6106(16) 0.0161(19) Uani 0.585(3) 1 d D U P C 2
H30A H 1.0403 0.7639 0.6607 0.019 Uiso 0.585(3) 1 calc R . P C 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sm1 O1 2.6016(19) . ?
Sm1 O2 2.4606(17) . ?
Sm1 O3 2.3514(17) . ?
Sm1 O4 2.3550(17) 3_666 ?
Sm1 O6 2.4338(17) . ?
Sm1 O7 2.4986(18) . ?
Sm1 N1 2.602(2) . ?
Sm1 N2 2.612(2) . ?
Sm1 N3 2.584(2) . ?
Sm1 C16 2.880(3) . ?
S1 C17 1.695(3) . ?
S1 C20 1.730(7) . ?
S1A C17 1.653(7) . ?
S1A C20A 1.734(19) . ?
S2 C22 1.731(3) . ?
S2 C25 1.712(16) . ?
S2A C22 1.712(4) . ?
S2A C25A 1.702(19) . ?
S3 C27 1.688(5) . ?
S3 C30 1.718(16) . ?
S3A C27 1.695(3) . ?
S3A C30A 1.726(12) . ?
O1 C16 1.263(3) . ?
O2 C16 1.268(3) . ?
O3 C21 1.264(3) . ?
O4 Sm1 2.3550(17) 3_666 ?
O4 C21 1.253(3) . ?
O5 C26 1.246(3) . ?
O6 C26 1.270(3) . ?
O7 H7A 0.8955 . ?
O7 H7B 0.8974 . ?
O8 H8A 0.86(2) . ?
O8 H8B 0.86(2) . ?
N1 C1 1.343(3) . ?
N1 C5 1.347(3) . ?
N2 C6 1.342(3) . ?
N2 C10 1.353(3) . ?
N3 C11 1.345(3) . ?
N3 C15 1.339(4) . ?
C1 H1 0.9500 . ?
C1 C2 1.384(4) . ?
C2 H2 0.9500 . ?
C2 C3 1.379(4) . ?
C3 H3 0.9500 . ?
C3 C4 1.379(4) . ?
C4 H4 0.9500 . ?
C4 C5 1.394(4) . ?
C5 C6 1.484(4) . ?
C6 C7 1.400(4) . ?
C7 H7 0.9500 . ?
C7 C8 1.373(4) . ?
C8 H8 0.9500 . ?
C8 C9 1.375(4) . ?
C9 H9 0.9500 . ?
C9 C10 1.395(4) . ?
C10 C11 1.479(4) . ?
C11 C12 1.392(4) . ?
C12 H12 0.9500 . ?
C12 C13 1.377(4) . ?
C13 H13 0.9500 . ?
C13 C14 1.374(5) . ?
C14 H14 0.9500 . ?
C14 C15 1.373(4) . ?
C15 H15 0.9500 . ?
C16 C17 1.487(4) . ?
C17 C18 1.391(11) . ?
C17 C18A 1.404(16) . ?
C18 H18 0.9500 . ?
C18 C19 1.405(15) . ?
C18A H18A 0.9500 . ?
C18A C19A 1.40(2) . ?
C19 H19 0.9500 . ?
C19 C20 1.358(7) . ?
C19A H19A 0.9500 . ?
C19A C20A 1.342(15) . ?
C20 H20 0.9500 . ?
C20A H20A 0.9500 . ?
C21 C22 1.476(3) . ?
C22 C23 1.371(10) . ?
C22 C23A 1.362(11) . ?
C23 H23 0.9500 . ?
C23 C24 1.43(2) . ?
C23A H23A 0.9500 . ?
C23A C24A 1.42(2) . ?
C24 H24 0.9500 . ?
C24 C25 1.351(10) . ?
C24A H24A 0.9500 . ?
C24A C25A 1.348(12) . ?
C25 H25 0.9500 . ?
C25A H25A 0.9500 . ?
C26 C27 1.492(4) . ?
C27 C28 1.379(13) . ?
C27 C28A 1.366(11) . ?
C28 H28 0.9500 . ?
C28 C29 1.41(2) . ?
C28A H28A 0.9500 . ?
C28A C29A 1.413(18) . ?
C29 H29 0.9500 . ?
C29 C30 1.362(13) . ?
C29A H29A 0.9500 . ?
C29A C30A 1.360(10) . ?
C30 H30 0.9500 . ?
C30A H30A 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 Sm1 N1 120.36(6) . . ?
O1 Sm1 N2 107.03(6) . . ?
O1 Sm1 C16 26.00(7) . . ?
O2 Sm1 O1 51.94(6) . . ?
O2 Sm1 O7 137.13(6) . . ?
O2 Sm1 N1 71.21(6) . . ?
O2 Sm1 N2 70.22(6) . . ?
O2 Sm1 N3 83.31(6) . . ?
O2 Sm1 C16 25.97(7) . . ?
O3 Sm1 O1 77.76(6) . . ?
O3 Sm1 O2 129.70(6) . . ?
O3 Sm1 O4 88.42(6) . 3_666 ?
O3 Sm1 O6 81.44(6) . . ?
O3 Sm1 O7 77.81(6) . . ?
O3 Sm1 N1 153.11(6) . . ?
O3 Sm1 N2 135.25(6) . . ?
O3 Sm1 N3 78.95(7) . . ?
O3 Sm1 C16 103.74(7) . . ?
O4 Sm1 O1 72.07(6) 3_666 . ?
O4 Sm1 O2 77.02(6) 3_666 . ?
O4 Sm1 O6 142.41(6) 3_666 . ?
O4 Sm1 O7 71.11(6) 3_666 . ?
O4 Sm1 N1 79.88(6) 3_666 . ?
O4 Sm1 N2 136.00(6) 3_666 . ?
O4 Sm1 N3 141.30(7) 3_666 . ?
O4 Sm1 C16 71.85(7) 3_666 . ?
O6 Sm1 O1 138.89(6) . . ?
O6 Sm1 O2 135.71(6) . . ?
O6 Sm1 O7 71.38(6) . . ?
O6 Sm1 N1 93.15(6) . . ?
O6 Sm1 N2 65.89(6) . . ?
O6 Sm1 N3 71.90(7) . . ?
O6 Sm1 C16 145.73(7) . . ?
O7 Sm1 O1 135.90(6) . . ?
O7 Sm1 N1 75.52(6) . . ?
O7 Sm1 N2 116.20(6) . . ?
O7 Sm1 N3 138.83(6) . . ?
O7 Sm1 C16 142.87(7) . . ?
N1 Sm1 N2 62.42(6) . . ?
N1 Sm1 C16 95.54(7) . . ?
N2 Sm1 C16 89.18(7) . . ?
N3 Sm1 O1 69.55(7) . . ?
N3 Sm1 N1 124.52(7) . . ?
N3 Sm1 N2 62.75(7) . . ?
N3 Sm1 C16 75.89(7) . . ?
C17 S1 C20 90.8(4) . . ?
C17 S1A C20A 87.7(10) . . ?
C25 S2 C22 89.5(7) . . ?
C25A S2A C22 88.2(9) . . ?
C27 S3 C30 90.9(9) . . ?
C27 S3A C30A 90.7(6) . . ?
C16 O1 Sm1 89.40(15) . . ?
C16 O2 Sm1 95.83(15) . . ?
C21 O3 Sm1 139.87(16) . . ?
C21 O4 Sm1 151.53(17) . 3_666 ?
C26 O6 Sm1 142.99(16) . . ?
Sm1 O7 H7A 110.8 . . ?
Sm1 O7 H7B 110.5 . . ?
H7A O7 H7B 108.1 . . ?
H8A O8 H8B 104(3) . . ?
C1 N1 Sm1 119.79(16) . . ?
C1 N1 C5 118.1(2) . . ?
C5 N1 Sm1 121.71(17) . . ?
C6 N2 Sm1 121.73(16) . . ?
C6 N2 C10 118.9(2) . . ?
C10 N2 Sm1 119.29(17) . . ?
C11 N3 Sm1 119.33(17) . . ?
C15 N3 Sm1 119.62(19) . . ?
C15 N3 C11 118.3(2) . . ?
N1 C1 H1 118.3 . . ?
N1 C1 C2 123.4(3) . . ?
C2 C1 H1 118.3 . . ?
C1 C2 H2 120.9 . . ?
C3 C2 C1 118.2(3) . . ?
C3 C2 H2 120.9 . . ?
C2 C3 H3 120.4 . . ?
C2 C3 C4 119.2(3) . . ?
C4 C3 H3 120.4 . . ?
C3 C4 H4 120.2 . . ?
C3 C4 C5 119.5(2) . . ?
C5 C4 H4 120.2 . . ?
N1 C5 C4 121.5(2) . . ?
N1 C5 C6 116.9(2) . . ?
C4 C5 C6 121.6(2) . . ?
N2 C6 C5 116.7(2) . . ?
N2 C6 C7 121.8(2) . . ?
C7 C6 C5 121.4(2) . . ?
C6 C7 H7 120.4 . . ?
C8 C7 C6 119.2(3) . . ?
C8 C7 H7 120.4 . . ?
C7 C8 H8 120.5 . . ?
C7 C8 C9 119.1(3) . . ?
C9 C8 H8 120.5 . . ?
C8 C9 H9 120.1 . . ?
C8 C9 C10 119.7(3) . . ?
C10 C9 H9 120.1 . . ?
N2 C10 C9 121.3(3) . . ?
N2 C10 C11 117.2(2) . . ?
C9 C10 C11 121.5(2) . . ?
N3 C11 C10 116.3(2) . . ?
N3 C11 C12 121.1(3) . . ?
C12 C11 C10 122.5(3) . . ?
C11 C12 H12 120.4 . . ?
C13 C12 C11 119.2(3) . . ?
C13 C12 H12 120.4 . . ?
C12 C13 H13 120.1 . . ?
C14 C13 C12 119.8(3) . . ?
C14 C13 H13 120.1 . . ?
C13 C14 H14 121.1 . . ?
C15 C14 C13 117.9(3) . . ?
C15 C14 H14 121.1 . . ?
N3 C15 C14 123.6(3) . . ?
N3 C15 H15 118.2 . . ?
C14 C15 H15 118.2 . . ?
O1 C16 Sm1 64.59(14) . . ?
O1 C16 O2 122.7(2) . . ?
O1 C16 C17 120.1(2) . . ?
O2 C16 Sm1 58.21(13) . . ?
O2 C16 C17 117.2(2) . . ?
C17 C16 Sm1 174.73(19) . . ?
C16 C17 S1 122.7(2) . . ?
C16 C17 S1A 118.2(3) . . ?
C18 C17 S1 110.3(5) . . ?
C18 C17 C16 126.9(5) . . ?
C18A C17 S1A 113.3(9) . . ?
C18A C17 C16 128.4(10) . . ?
C17 C18 H18 122.2 . . ?
C17 C18 C19 115.7(9) . . ?
C19 C18 H18 122.2 . . ?
C17 C18A H18A 122.7 . . ?
C19A C18A C17 114.5(19) . . ?
C19A C18A H18A 122.7 . . ?
C18 C19 H19 125.8 . . ?
C20 C19 C18 108.5(11) . . ?
C20 C19 H19 125.8 . . ?
C18A C19A H19A 127.1 . . ?
C20A C19A C18A 106(3) . . ?
C20A C19A H19A 127.1 . . ?
S1 C20 H20 122.6 . . ?
C19 C20 S1 114.8(10) . . ?
C19 C20 H20 122.6 . . ?
S1A C20A H20A 120.8 . . ?
C19A C20A S1A 118(2) . . ?
C19A C20A H20A 120.8 . . ?
O3 C21 C22 118.6(2) . . ?
O4 C21 O3 124.8(2) . . ?
O4 C21 C22 116.6(2) . . ?
C21 C22 S2 122.4(2) . . ?
C21 C22 S2A 118.6(2) . . ?
C23 C22 S2 109.9(5) . . ?
C23 C22 C21 127.7(5) . . ?
C23A C22 S2A 111.9(6) . . ?
C23A C22 C21 129.5(6) . . ?
C22 C23 H23 121.6 . . ?
C22 C23 C24 116.7(12) . . ?
C24 C23 H23 121.6 . . ?
C22 C23A H23A 122.2 . . ?
C22 C23A C24A 115.5(14) . . ?
C24A C23A H23A 122.2 . . ?
C23 C24 H24 127.0 . . ?
C25 C24 C23 106(2) . . ?
C25 C24 H24 127.0 . . ?
C23A C24A H24A 127.2 . . ?
C25A C24A C23A 106(2) . . ?
C25A C24A H24A 127.2 . . ?
S2 C25 H25 121.1 . . ?
C24 C25 S2 117.8(19) . . ?
C24 C25 H25 121.1 . . ?
S2A C25A H25A 120.6 . . ?
C24A C25A S2A 119(2) . . ?
C24A C25A H25A 120.6 . . ?
O5 C26 O6 126.1(2) . . ?
O5 C26 C27 117.8(2) . . ?
O6 C26 C27 116.1(2) . . ?
C26 C27 S3 121.0(3) . . ?
C26 C27 S3A 121.2(2) . . ?
C28 C27 S3 109.7(7) . . ?
C28 C27 C26 128.6(8) . . ?
C28A C27 S3A 110.8(6) . . ?
C28A C27 C26 127.8(6) . . ?
C27 C28 H28 121.4 . . ?
C27 C28 C29 117.1(16) . . ?
C29 C28 H28 121.4 . . ?
C27 C28A H28A 122.1 . . ?
C27 C28A C29A 115.7(12) . . ?
C29A C28A H28A 122.1 . . ?
C28 C29 H29 126.8 . . ?
C30 C29 C28 106(2) . . ?
C30 C29 H29 126.8 . . ?
C28A C29A H29A 125.8 . . ?
C30A C29A C28A 108.3(17) . . ?
C30A C29A H29A 125.8 . . ?
S3 C30 H30 122.2 . . ?
C29 C30 S3 116(2) . . ?
C29 C30 H30 122.1 . . ?
S3A C30A H30A 122.8 . . ?
C29A C30A S3A 114.4(15) . . ?
C29A C30A H30A 122.8 . . ?

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
O7 H7A O3 0.90 2.37 3.098(3) 138.3 3_666
O7 H7B O5 0.90 1.81 2.677(2) 161.4 .
O8 H8A O1 0.86(2) 1.80(4) 2.633(9) 164(11) .
O8 H8B O1 0.86(2) 2.30(4) 3.122(9) 161(10) 3_667
O8 H8B O8 0.86(2) 2.00(10) 2.576(18) 123(9) 3_667

_olex2_submission_special_instructions 'No special instructions were received'


####################################################################### 
# 
# 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_final_a_CCDC3
_database_code_depnum_ccdc_archive 'CCDC 1544442'
_audit_update_record             
;
2017-04-17 deposited with the CCDC.
2017-08-23 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         'C60 H44 N6 O14 Pr2 S6, 0.642(H2 O)'
_chemical_formula_sum            'C60 H45.28 N6 O14.64 Pr2 S6'
_chemical_formula_weight         1558.74

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'
Pr Pr -0.2180 2.8214 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   12.0250(6)
_cell_length_b                   25.7370(11)
_cell_length_c                   9.6972(4)
_cell_angle_alpha                90
_cell_angle_beta                 98.165(2)
_cell_angle_gamma                90
_cell_volume                     2970.7(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9861
_cell_measurement_theta_min      2.26
_cell_measurement_theta_max      26.40
_exptl_crystal_description       rhombus
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.743
_exptl_crystal_F_000             1557
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.497
_exptl_crystal_size_mid          0.199
_exptl_crystal_size_min          0.157
_exptl_absorpt_coefficient_mu    1.905
_shelx_estimated_absorpt_T_min   0.451
_shelx_estimated_absorpt_T_max   0.754
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.57051
_exptl_absorpt_correction_T_max  0.81109
_exptl_absorpt_process_details   'SADABS V2016/2 (Bruker, 2014)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_monochromator  'multilayer mirrors'
_diffrn_measurement_device       'Bruker D8 Quest/Photon 100'
_diffrn_measurement_method       'profile data from φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            31948
_diffrn_reflns_av_unetI/netI     0.0305
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.264
_diffrn_reflns_theta_max         26.444
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             6091
_reflns_number_gt                5315
_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.
 
 _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       'APEX2 V2014.9-0 (Bruker, 2014)'
_computing_cell_refinement       'SAINT V8.37A (Bruker, 2005)'
_computing_data_reduction        
; 
SAINT V8.37A, XPREP v2014/2, SADABS V2016/2 (Bruker, 2014) 
;
_computing_structure_solution    'SHELX-2014-5 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELX-2014-7 (Sheldrick, 2015)'
_computing_molecular_graphics    'SHELXLE v817 (Hubschle, 2011)'
_computing_publication_material  'XCIF V2014-2 (Bruker, 2014)'

_refine_special_details          
; 
Structure was phased by direct methods (Sheldrick, 2015).  Systematic 
conditions suggested the ambiguous space group.  The space group choice 
was confirmed by successful convergence of the full-matrix least-squares 
refinement on F².  The final map had no significant features.  A final 
analysis of variance between observed and calculated structure factors 
showed little dependence on amplitude and resolution. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0137P)²+3.3835P] 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         6091
_refine_ls_number_parameters     539
_refine_ls_number_restraints     1200
_refine_ls_R_factor_all          0.0348
_refine_ls_R_factor_gt           0.0262
_refine_ls_wR_factor_ref         0.0490
_refine_ls_wR_factor_gt          0.0471
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_restrained_S_all      1.018
_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
Pr1 Pr 0.51738(2) 0.40169(2) 0.59783(2) 0.01084(5) Uani 1 1 d . U . . .
O7 O 0.56098(16) 0.42966(7) 0.3606(2) 0.0209(4) Uani 1 1 d D U . . .
H7A H 0.6295(11) 0.4230(12) 0.354(3) 0.031 Uiso 1 1 d D U . . .
H7B H 0.538(2) 0.4580(7) 0.321(3) 0.031 Uiso 1 1 d D U . . .
O8 O 0.5022(6) 0.5295(2) 0.8983(6) 0.030(2) Uani 0.321(6) 1 d D . P . .
H8A H 0.511(2) 0.535(4) 0.987(2) 0.045 Uiso 0.321(6) 1 d D U P . .
H8B H 0.467(8) 0.500(2) 0.885(11) 0.045 Uiso 0.321(6) 1 d D U P . .
N1 N 0.62742(19) 0.37744(9) 0.8425(2) 0.0195(5) Uani 1 1 d . U . . .
N2 N 0.55096(16) 0.30137(8) 0.6591(2) 0.0127(4) Uani 1 1 d . U . . .
N3 N 0.41334(17) 0.33170(8) 0.4265(2) 0.0138(4) Uani 1 1 d . U . . .
C1 C 0.6646(3) 0.41590(12) 0.9302(3) 0.0308(7) Uani 1 1 d . U . . .
H1 H 0.6308 0.4492 0.9157 0.037 Uiso 1 1 calc R U . . .
C2 C 0.7500(3) 0.40951(13) 1.0410(3) 0.0358(8) Uani 1 1 d . U . . .
H2 H 0.7721 0.4373 1.1034 0.043 Uiso 1 1 calc R U . . .
C3 C 0.8014(3) 0.36211(14) 1.0579(3) 0.0340(8) Uani 1 1 d . U . . .
H3 H 0.8618 0.3568 1.1311 0.041 Uiso 1 1 calc R U . . .
C4 C 0.7655(2) 0.32209(13) 0.9687(3) 0.0265(7) Uani 1 1 d . U . . .
H4 H 0.8014 0.2892 0.9785 0.032 Uiso 1 1 calc R U . . .
C5 C 0.6752(2) 0.33050(11) 0.8631(3) 0.0183(6) Uani 1 1 d . U . . .
C6 C 0.6251(2) 0.28784(10) 0.7716(3) 0.0167(5) Uani 1 1 d . U . . .
C7 C 0.6498(2) 0.23590(11) 0.8041(3) 0.0205(6) Uani 1 1 d . U . . .
H7 H 0.7015 0.2272 0.8841 0.025 Uiso 1 1 calc R U . . .
C8 C 0.5987(2) 0.19738(11) 0.7192(3) 0.0223(6) Uani 1 1 d . U . . .
H8 H 0.6148 0.1618 0.7397 0.027 Uiso 1 1 calc R U . . .
C9 C 0.5239(2) 0.21116(10) 0.6042(3) 0.0180(5) Uani 1 1 d . U . . .
H9 H 0.4882 0.1852 0.5440 0.022 Uiso 1 1 calc R U . . .
C10 C 0.5008(2) 0.26362(9) 0.5767(3) 0.0139(5) Uani 1 1 d . U . . .
C11 C 0.4203(2) 0.28019(9) 0.4537(3) 0.0137(5) Uani 1 1 d . U . . .
C12 C 0.3571(2) 0.24456(10) 0.3681(3) 0.0187(6) Uani 1 1 d . U . . .
H12 H 0.3628 0.2085 0.3892 0.022 Uiso 1 1 calc R U . . .
C13 C 0.2861(2) 0.26142(10) 0.2524(3) 0.0203(6) Uani 1 1 d . U . . .
H13 H 0.2433 0.2373 0.1927 0.024 Uiso 1 1 calc R U . . .
C14 C 0.2783(2) 0.31392(11) 0.2251(3) 0.0210(6) Uani 1 1 d . U . . .
H14 H 0.2297 0.3268 0.1467 0.025 Uiso 1 1 calc R U . . .
C15 C 0.3431(2) 0.34758(10) 0.3147(3) 0.0182(6) Uani 1 1 d . U . . .
H15 H 0.3375 0.3838 0.2959 0.022 Uiso 1 1 calc R U . . .
O1 O 0.41553(15) 0.44071(7) 0.7975(2) 0.0249(4) Uani 1 1 d . U . . .
O2 O 0.35248(14) 0.36623(7) 0.70049(18) 0.0172(4) Uani 1 1 d . U . . .
C16 C 0.3453(2) 0.40387(10) 0.7825(3) 0.0172(5) Uani 1 1 d D U . . .
S1 S 0.24316(15) 0.44318(8) 1.0024(2) 0.0180(4) Uani 0.691(3) 1 d D U P A 1
C17 C 0.2480(12) 0.4029(9) 0.862(2) 0.0138(11) Uani 0.691(3) 1 d D U P A 1
C18 C 0.1549(7) 0.3719(4) 0.8412(10) 0.0181(16) Uani 0.691(3) 1 d D U P A 1
H18 H 0.1433 0.3469 0.7685 0.022 Uiso 0.691(3) 1 calc R U P A 1
C19 C 0.0774(7) 0.3799(4) 0.9354(11) 0.0166(11) Uani 0.691(3) 1 d D U P A 1
H19 H 0.0085 0.3616 0.9336 0.020 Uiso 0.691(3) 1 calc R U P A 1
C20 C 0.1149(7) 0.4173(4) 1.0287(10) 0.0178(12) Uani 0.691(3) 1 d D U P A 1
H20 H 0.0750 0.4282 1.1013 0.021 Uiso 0.691(3) 1 calc R U P A 1
S1A S 0.1443(4) 0.3634(2) 0.8157(6) 0.0162(9) Uani 0.309(3) 1 d D U P A 2
C17A C 0.253(3) 0.405(2) 0.869(5) 0.015(2) Uani 0.309(3) 1 d D U P A 2
C18A C 0.2337(12) 0.4346(7) 0.9789(17) 0.018(2) Uani 0.309(3) 1 d D U P A 2
H18A H 0.2852 0.4602 1.0197 0.021 Uiso 0.309(3) 1 calc R U P A 2
C19A C 0.1305(15) 0.4245(9) 1.027(2) 0.019(2) Uani 0.309(3) 1 d D U P A 2
H19A H 0.1044 0.4413 1.1037 0.023 Uiso 0.309(3) 1 calc R U P A 2
C20A C 0.0744(16) 0.3871(10) 0.947(2) 0.017(2) Uani 0.309(3) 1 d D U P A 2
H20A H 0.0026 0.3747 0.9618 0.021 Uiso 0.309(3) 1 calc R U P A 2
O3 O 0.62191(14) 0.47983(7) 0.65319(18) 0.0188(4) Uani 1 1 d . U . . .
O4 O 0.63679(14) 0.54732(7) 0.51328(19) 0.0197(4) Uani 1 1 d . U . . .
C21 C 0.6784(2) 0.51298(9) 0.5968(3) 0.0127(5) Uani 1 1 d D U . . .
S2 S 0.87222(16) 0.46513(8) 0.7375(2) 0.0159(5) Uani 0.538(3) 1 d D U P B 1
C22 C 0.80211(19) 0.51260(9) 0.6325(2) 0.0119(5) Uani 0.538(3) 1 d D U P B 1
C23 C 0.8767(7) 0.5465(3) 0.5882(11) 0.0179(17) Uani 0.538(3) 1 d D U P B 1
H23 H 0.8536 0.5741 0.5256 0.021 Uiso 0.538(3) 1 calc R U P B 1
C24 C 0.9904(7) 0.5377(6) 0.642(2) 0.0181(15) Uani 0.538(3) 1 d D U P B 1
H24 H 1.0515 0.5590 0.6249 0.022 Uiso 0.538(3) 1 calc R U P B 1
C25 C 0.9990(7) 0.4942(5) 0.7212(19) 0.0170(15) Uani 0.538(3) 1 d D U P B 1
H25 H 1.0690 0.4808 0.7643 0.020 Uiso 0.538(3) 1 calc R U P B 1
S2A S 0.8774(2) 0.56201(10) 0.5727(3) 0.0163(6) Uani 0.462(3) 1 d D U P B 2
C22A C 0.80211(19) 0.51260(9) 0.6325(2) 0.0119(5) Uani 0.462(3) 1 d D U P B 2
C23A C 0.8694(7) 0.4771(3) 0.7064(11) 0.0168(18) Uani 0.462(3) 1 d D U P B 2
H23A H 0.8410 0.4470 0.7459 0.020 Uiso 0.462(3) 1 calc R U P B 2
C24A C 0.9850(8) 0.4886(6) 0.720(2) 0.0177(17) Uani 0.462(3) 1 d D U P B 2
H24A H 1.0431 0.4683 0.7700 0.021 Uiso 0.462(3) 1 calc R U P B 2
C25A C 1.0007(8) 0.5332(7) 0.650(3) 0.0161(17) Uani 0.462(3) 1 d D U P B 2
H25A H 1.0729 0.5473 0.6448 0.019 Uiso 0.462(3) 1 calc R U P B 2
O5 O 0.70610(14) 0.36940(7) 0.56659(18) 0.0174(4) Uani 1 1 d . U . . .
O6 O 0.77531(14) 0.39772(7) 0.37734(18) 0.0189(4) Uani 1 1 d . U . . .
C26 C 0.7789(2) 0.37058(9) 0.4844(3) 0.0138(5) Uani 1 1 d D U . . .
S3 S 0.8875(2) 0.29535(10) 0.6601(2) 0.0181(5) Uani 0.577(3) 1 d D U P C 1
C27 C 0.8760(2) 0.33408(10) 0.5177(2) 0.0148(5) Uani 0.577(3) 1 d D U P C 1
C28 C 0.9603(8) 0.3245(5) 0.4404(9) 0.0225(17) Uani 0.577(3) 1 d D U P C 1
H28 H 0.9667 0.3427 0.3566 0.027 Uiso 0.577(3) 1 calc R U P C 1
C29 C 1.0372(9) 0.2856(4) 0.4940(10) 0.0223(14) Uani 0.577(3) 1 d D U P C 1
H29 H 1.1015 0.2752 0.4542 0.027 Uiso 0.577(3) 1 calc R U P C 1
C30 C 1.0051(9) 0.2654(5) 0.6115(11) 0.0176(14) Uani 0.577(3) 1 d D U P C 1
H30 H 1.0433 0.2376 0.6621 0.021 Uiso 0.577(3) 1 calc R U P C 1
S3A S 0.9689(3) 0.32419(17) 0.4048(3) 0.0264(7) Uani 0.423(3) 1 d D U P C 2
C27A C 0.8760(2) 0.33408(10) 0.5177(2) 0.0148(5) Uani 0.423(3) 1 d D U P C 2
C28A C 0.8949(11) 0.2998(5) 0.6270(11) 0.019(2) Uani 0.423(3) 1 d D U P C 2
H28A H 0.8475 0.2979 0.6974 0.023 Uiso 0.423(3) 1 calc R U P C 2
C29A C 0.9898(13) 0.2675(7) 0.6270(15) 0.0214(18) Uani 0.423(3) 1 d D U P C 2
H29A H 1.0176 0.2438 0.6989 0.026 Uiso 0.423(3) 1 calc R U P C 2
C30A C 1.0348(12) 0.2755(5) 0.5084(14) 0.0225(19) Uani 0.423(3) 1 d D U P C 2
H30A H 1.0967 0.2562 0.4846 0.027 Uiso 0.423(3) 1 calc R U P C 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

_exptl_special_details           
; 
One distinct cell was identified using APEX2 (Bruker, 2014).  Three 
frame series were integrated and filtered for statistical outliers 
using SAINT (Bruker, 2014) then corrected for absorption by integration 
using SAINT/SADABS v2014/2 (Bruker, 2014) to sort, merge, and scale 
the combined data.  No decay correction was applied.    
;

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
2.00 -1.00 -1.00 0.0620
-2.00 1.00 1.00 0.0910
2.00 -1.00 -2.00 0.0590
1.00 1.00 -1.00 0.0940
-1.00 -1.00 1.00 0.1430
0.00 -1.00 -1.00 0.0730
0.00 -1.00 2.00 0.0940
0.00 1.00 -2.00 0.0760
1.00 2.00 2.00 0.0600
-1.00 1.00 -2.00 0.0880
-2.00 -1.00 -2.00 0.0930
0.00 1.00 0.00 0.1680
0.00 -1.00 0.00 0.2400
-2.00 -1.00 -1.00 0.0940
-2.00 1.00 0.00 0.0980
-1.00 2.00 1.00 0.1120
1.00 0.00 0.00 0.0500

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
Pr1 O3 2.3919(17) . ?
Pr1 O4 2.3986(17) 3_666 ?
Pr1 O5 2.4754(17) . ?
Pr1 O2 2.5133(17) . ?
Pr1 O7 2.5356(19) . ?
Pr1 N1 2.622(2) . ?
Pr1 O1 2.6331(18) . ?
Pr1 N3 2.642(2) . ?
Pr1 N2 2.667(2) . ?
Pr1 C16 2.923(3) . ?
O7 H7A 0.852(10) . ?
O7 H7B 0.849(10) . ?
O8 H8A 0.860(10) . ?
O8 H8B 0.861(11) . ?
N1 C1 1.339(4) . ?
N1 C5 1.341(3) . ?
N2 C10 1.345(3) . ?
N2 C6 1.353(3) . ?
N3 C15 1.339(3) . ?
N3 C11 1.352(3) . ?
C1 C2 1.387(4) . ?
C1 H1 0.9500 . ?
C2 C3 1.367(5) . ?
C2 H2 0.9500 . ?
C3 C4 1.375(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.398(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.485(4) . ?
C6 C7 1.396(4) . ?
C7 C8 1.376(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.376(4) . ?
C8 H8 0.9500 . ?
C9 C10 1.397(3) . ?
C9 H9 0.9500 . ?
C10 C11 1.488(3) . ?
C11 C12 1.389(4) . ?
C12 C13 1.380(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.378(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.386(4) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
O1 C16 1.264(3) . ?
O2 C16 1.264(3) . ?
C16 C17A 1.480(7) . ?
C16 C17 1.493(4) . ?
S1 C17 1.716(5) . ?
S1 C20 1.732(5) . ?
C17 C18 1.365(7) . ?
C18 C19 1.410(8) . ?
C18 H18 0.9500 . ?
C19 C20 1.354(5) . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?
S1A C17A 1.706(8) . ?
S1A C20A 1.733(9) . ?
C17A C18A 1.365(8) . ?
C18A C19A 1.411(11) . ?
C18A H18A 0.9500 . ?
C19A C20A 1.356(7) . ?
C19A H19A 0.9500 . ?
C20A H20A 0.9500 . ?
O3 C21 1.262(3) . ?
O4 C21 1.254(3) . ?
O4 Pr1 2.3985(17) 3_666 ?
C21 C22A 1.479(3) . ?
C21 C22 1.479(3) . ?
S2 C25 1.725(7) . ?
S2 C22 1.731(3) . ?
C22 C23 1.363(7) . ?
C23 C24 1.410(9) . ?
C23 H23 0.9500 . ?
C24 C25 1.354(6) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
S2A C22A 1.710(3) . ?
S2A C25A 1.732(8) . ?
C22A C23A 1.356(7) . ?
C23A C24A 1.409(10) . ?
C23A H23A 0.9500 . ?
C24A C25A 1.357(6) . ?
C24A H24A 0.9500 . ?
C25A H25A 0.9500 . ?
O5 C26 1.266(3) . ?
O6 C26 1.247(3) . ?
C26 C27A 1.498(3) . ?
C26 C27 1.498(3) . ?
S3 C27 1.693(3) . ?
S3 C30 1.733(6) . ?
C27 C28 1.366(7) . ?
C28 C29 1.411(9) . ?
C28 H28 0.9500 . ?
C29 C30 1.357(6) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?
S3A C27A 1.691(3) . ?
S3A C30A 1.727(8) . ?
C27A C28A 1.374(8) . ?
C28A C29A 1.412(10) . ?
C28A H28A 0.9500 . ?
C29A C30A 1.355(7) . ?
C29A H29A 0.9500 . ?
C30A H30A 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
O3 Pr1 O4 89.36(6) . 3_666 ?
O3 Pr1 O5 81.26(6) . . ?
O4 Pr1 O5 142.40(6) 3_666 . ?
O3 Pr1 O2 129.45(6) . . ?
O4 Pr1 O2 76.92(6) 3_666 . ?
O5 Pr1 O2 135.66(6) . . ?
O3 Pr1 O7 78.18(6) . . ?
O4 Pr1 O7 71.53(6) 3_666 . ?
O5 Pr1 O7 70.91(6) . . ?
O2 Pr1 O7 137.64(6) . . ?
O3 Pr1 N1 79.37(6) . . ?
O4 Pr1 N1 142.67(7) 3_666 . ?
O5 Pr1 N1 71.17(6) . . ?
O2 Pr1 N1 83.13(6) . . ?
O7 Pr1 N1 138.22(6) . . ?
O3 Pr1 O1 78.39(6) . . ?
O4 Pr1 O1 73.21(6) 3_666 . ?
O5 Pr1 O1 138.45(6) . . ?
O2 Pr1 O1 51.07(6) . . ?
O7 Pr1 O1 137.46(6) . . ?
N1 Pr1 O1 69.70(7) . . ?
O3 Pr1 N3 154.32(6) . . ?
O4 Pr1 N3 79.85(6) 3_666 . ?
O5 Pr1 N3 93.13(6) . . ?
O2 Pr1 N3 70.84(6) . . ?
O7 Pr1 N3 76.31(6) . . ?
N1 Pr1 N3 122.67(6) . . ?
O1 Pr1 N3 119.63(6) . . ?
O3 Pr1 N2 134.89(6) . . ?
O4 Pr1 N2 135.45(6) 3_666 . ?
O5 Pr1 N2 65.79(6) . . ?
O2 Pr1 N2 70.32(6) . . ?
O7 Pr1 N2 115.64(6) . . ?
N1 Pr1 N2 61.78(7) . . ?
O1 Pr1 N2 106.08(6) . . ?
N3 Pr1 N2 61.53(6) . . ?
O3 Pr1 C16 103.98(7) . . ?
O4 Pr1 C16 72.26(7) 3_666 . ?
O5 Pr1 C16 145.34(6) . . ?
O2 Pr1 C16 25.48(6) . . ?
O7 Pr1 C16 143.70(6) . . ?
N1 Pr1 C16 76.15(7) . . ?
O1 Pr1 C16 25.63(6) . . ?
N3 Pr1 C16 94.88(7) . . ?
N2 Pr1 C16 88.86(7) . . ?
Pr1 O7 H7A 109(2) . . ?
Pr1 O7 H7B 124(2) . . ?
H7A O7 H7B 113(3) . . ?
H8A O8 H8B 106(9) . . ?
C1 N1 C5 118.3(2) . . ?
C1 N1 Pr1 118.58(18) . . ?
C5 N1 Pr1 120.01(17) . . ?
C10 N2 C6 118.8(2) . . ?
C10 N2 Pr1 121.73(15) . . ?
C6 N2 Pr1 119.37(16) . . ?
C15 N3 C11 118.1(2) . . ?
C15 N3 Pr1 119.25(16) . . ?
C11 N3 Pr1 122.35(16) . . ?
N1 C1 C2 123.2(3) . . ?
N1 C1 H1 118.4 . . ?
C2 C1 H1 118.4 . . ?
C3 C2 C1 118.1(3) . . ?
C3 C2 H2 120.9 . . ?
C1 C2 H2 120.9 . . ?
C2 C3 C4 119.8(3) . . ?
C2 C3 H3 120.1 . . ?
C4 C3 H3 120.1 . . ?
C3 C4 C5 119.1(3) . . ?
C3 C4 H4 120.4 . . ?
C5 C4 H4 120.4 . . ?
N1 C5 C4 121.4(3) . . ?
N1 C5 C6 116.6(2) . . ?
C4 C5 C6 122.0(3) . . ?
N2 C6 C7 121.5(2) . . ?
N2 C6 C5 117.2(2) . . ?
C7 C6 C5 121.2(2) . . ?
C8 C7 C6 119.5(3) . . ?
C8 C7 H7 120.3 . . ?
C6 C7 H7 120.3 . . ?
C9 C8 C7 118.9(2) . . ?
C9 C8 H8 120.5 . . ?
C7 C8 H8 120.5 . . ?
C8 C9 C10 119.6(3) . . ?
C8 C9 H9 120.2 . . ?
C10 C9 H9 120.2 . . ?
N2 C10 C9 121.6(2) . . ?
N2 C10 C11 117.1(2) . . ?
C9 C10 C11 121.3(2) . . ?
N3 C11 C12 121.2(2) . . ?
N3 C11 C10 116.9(2) . . ?
C12 C11 C10 121.9(2) . . ?
C13 C12 C11 120.1(2) . . ?
C13 C12 H12 120.0 . . ?
C11 C12 H12 120.0 . . ?
C14 C13 C12 118.8(2) . . ?
C14 C13 H13 120.6 . . ?
C12 C13 H13 120.6 . . ?
C13 C14 C15 118.4(3) . . ?
C13 C14 H14 120.8 . . ?
C15 C14 H14 120.8 . . ?
N3 C15 C14 123.4(2) . . ?
N3 C15 H15 118.3 . . ?
C14 C15 H15 118.3 . . ?
C16 O1 Pr1 90.10(15) . . ?
C16 O2 Pr1 95.69(15) . . ?
O2 C16 O1 122.9(2) . . ?
O2 C16 C17A 119.3(9) . . ?
O1 C16 C17A 117.8(8) . . ?
O2 C16 C17 116.2(4) . . ?
O1 C16 C17 120.9(4) . . ?
O2 C16 Pr1 58.83(12) . . ?
O1 C16 Pr1 64.27(13) . . ?
C17A C16 Pr1 176.7(18) . . ?
C17 C16 Pr1 173.3(6) . . ?
C17 S1 C20 90.8(3) . . ?
C18 C17 C16 128.2(5) . . ?
C18 C17 S1 110.7(4) . . ?
C16 C17 S1 121.2(3) . . ?
C17 C18 C19 114.9(6) . . ?
C17 C18 H18 122.5 . . ?
C19 C18 H18 122.5 . . ?
C20 C19 C18 110.3(6) . . ?
C20 C19 H19 124.8 . . ?
C18 C19 H19 124.8 . . ?
C19 C20 S1 113.3(5) . . ?
C19 C20 H20 123.4 . . ?
S1 C20 H20 123.4 . . ?
C17A S1A C20A 89.5(5) . . ?
C18A C17A C16 132.5(10) . . ?
C18A C17A S1A 112.2(6) . . ?
C16 C17A S1A 115.1(6) . . ?
C17A C18A C19A 114.3(9) . . ?
C17A C18A H18A 122.8 . . ?
C19A C18A H18A 122.8 . . ?
C20A C19A C18A 109.3(11) . . ?
C20A C19A H19A 125.4 . . ?
C18A C19A H19A 125.4 . . ?
C19A C20A S1A 114.6(10) . . ?
C19A C20A H20A 122.7 . . ?
S1A C20A H20A 122.7 . . ?
C21 O3 Pr1 140.26(16) . . ?
C21 O4 Pr1 152.58(16) . 3_666 ?
O4 C21 O3 124.5(2) . . ?
O4 C21 C22A 116.8(2) . . ?
O3 C21 C22A 118.6(2) . . ?
O4 C21 C22 116.8(2) . . ?
O3 C21 C22 118.6(2) . . ?
C25 S2 C22 90.2(4) . . ?
C23 C22 C21 127.4(4) . . ?
C23 C22 S2 110.5(4) . . ?
C21 C22 S2 122.15(18) . . ?
C22 C23 C24 115.3(7) . . ?
C22 C23 H23 122.3 . . ?
C24 C23 H23 122.3 . . ?
C25 C24 C23 109.5(9) . . ?
C25 C24 H24 125.2 . . ?
C23 C24 H24 125.2 . . ?
C24 C25 S2 114.4(8) . . ?
C24 C25 H25 122.8 . . ?
S2 C25 H25 122.8 . . ?
C22A S2A C25A 89.8(4) . . ?
C23A C22A C21 129.3(4) . . ?
C23A C22A S2A 112.0(4) . . ?
C21 C22A S2A 118.65(18) . . ?
C22A C23A C24A 114.5(7) . . ?
C22A C23A H23A 122.8 . . ?
C24A C23A H23A 122.8 . . ?
C25A C24A C23A 109.7(10) . . ?
C25A C24A H24A 125.2 . . ?
C23A C24A H24A 125.2 . . ?
C24A C25A S2A 114.0(9) . . ?
C24A C25A H25A 123.0 . . ?
S2A C25A H25A 123.0 . . ?
C26 O5 Pr1 142.89(16) . . ?
O6 C26 O5 126.3(2) . . ?
O6 C26 C27A 117.7(2) . . ?
O5 C26 C27A 115.9(2) . . ?
O6 C26 C27 117.7(2) . . ?
O5 C26 C27 115.9(2) . . ?
C27 S3 C30 90.9(3) . . ?
C28 C27 C26 127.7(4) . . ?
C28 C27 S3 111.2(4) . . ?
C26 C27 S3 121.07(18) . . ?
C27 C28 C29 115.1(7) . . ?
C27 C28 H28 122.5 . . ?
C29 C28 H28 122.5 . . ?
C30 C29 C28 109.3(8) . . ?
C30 C29 H29 125.3 . . ?
C28 C29 H29 125.3 . . ?
C29 C30 S3 113.5(7) . . ?
C29 C30 H30 123.3 . . ?
S3 C30 H30 123.3 . . ?
C27A S3A C30A 91.3(4) . . ?
C28A C27A C26 127.4(5) . . ?
C28A C27A S3A 110.6(4) . . ?
C26 C27A S3A 121.4(2) . . ?
C27A C28A C29A 115.1(8) . . ?
C27A C28A H28A 122.5 . . ?
C29A C28A H28A 122.5 . . ?
C30A C29A C28A 109.3(10) . . ?
C30A C29A H29A 125.3 . . ?
C28A C29A H29A 125.3 . . ?
C29A C30A S3A 113.5(9) . . ?
C29A C30A H30A 123.3 . . ?
S3A C30A H30A 123.3 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O7 H7A O6 0.852(10) 1.854(13) 2.688(3) 166(3) .
O7 H7B O8 0.849(10) 2.14(3) 2.729(7) 126(3) 3_666
O7 H7B O3 0.849(10) 2.54(2) 3.193(3) 134(3) 3_666
O8 H8A O8 0.860(10) 2.02(9) 2.494(13) 114(8) 3_667
O8 H8A O1 0.860(10) 2.24(2) 3.072(6) 162(5) 3_667
O8 H8B O1 0.861(11) 1.82(4) 2.640(6) 159(10) .

_refine_diff_density_max         0.465
_refine_diff_density_min         -0.719
_refine_diff_density_rms         0.088

####################################################################### 
# 
# 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_final_a_CCDC4
_database_code_depnum_ccdc_archive 'CCDC 1544451'
_audit_update_record             
;
2017-04-17 deposited with the CCDC.
2017-08-23 downloaded from the CCDC.
;
_audit_creation_date             2017-04-06
_audit_creation_method           
;
Olex2 1.2
(compiled Mar 28 2017 19:26:29 for OlexSys, GUI svn.r5335)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C30 H22 Er N3 O7 S3'
_chemical_formula_sum            'C30 H22 Er N3 O7 S3'
_chemical_formula_weight         799.94
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Er Er -0.2586 4.9576 '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'

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

_cell_length_a                   16.5155(8)
_cell_length_b                   10.1553(5)
_cell_length_c                   17.0664(8)
_cell_angle_alpha                90
_cell_angle_beta                 92.993(2)
_cell_angle_gamma                90
_cell_volume                     2858.5(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9283
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.57
_cell_measurement_theta_min      2.33
_shelx_estimated_absorpt_T_max   0.372
_shelx_estimated_absorpt_T_min   0.246
_exptl_absorpt_coefficient_mu    3.210
_exptl_absorpt_correction_T_max  0.4767
_exptl_absorpt_correction_T_min  0.2869
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1077 before and 0.0602 after correction.
The Ratio of minimum to maximum transmission is 0.6018.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.859
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1580
_exptl_crystal_size_max          0.606
_exptl_crystal_size_mid          0.488
_exptl_crystal_size_min          0.384
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0440
_diffrn_reflns_av_unetI/netI     0.0277
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            42497
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.282
_diffrn_reflns_theta_min         2.335
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6634
_reflns_number_total             7098
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.797
_refine_diff_density_min         -1.773
_refine_diff_density_rms         0.124
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.186
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     514
_refine_ls_number_reflns         7098
_refine_ls_number_restraints     999
_refine_ls_R_factor_all          0.0272
_refine_ls_R_factor_gt           0.0241
_refine_ls_restrained_S_all      1.132
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0156P)²+4.2679P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0539
_refine_ls_wR_factor_ref         0.0548
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O7-H7A = O7-H7B
 0.86 with sigma of 0.02
 H7A-H7B
 1.35 with sigma of 0.02
 S1-C17 \\sim S1A-C17 \\sim S2A-C22 \\sim S2-C22 \\sim S3-C27 \\sim S3A-C27
 with sigma of 0.01
 S1A-C20A \\sim S1-C20 \\sim S2A-C25A \\sim S2-C25 \\sim S3-C30 \\sim S3A-C30A
 with sigma of 0.01
 C20A-C19A \\sim C20-C19 \\sim C25A-C24A \\sim C25-C24 \\sim C30-C29 \\sim
C30A-C29A
 with sigma of 0.01
 C18-C17 \\sim C18A-C17 \\sim C23-C22 \\sim C23A-C22 \\sim C28A-C27 \\sim
C28-C27
 with sigma of 0.01
 C19-C18 \\sim C19A-C18A \\sim C24-C23 \\sim C24A-C23A \\sim C29-C28 \\sim
C29A-C28A
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
S1 \\sim S1 \\sim S1 \\sim S1A \\sim S1A \\sim S1A \\sim C17 \\sim C17 \\sim
C17 \\sim C17 \\sim C17 \\sim C18 \\sim C18 \\sim C18 \\sim C18A \\sim C18A
\\sim C18A \\sim C19 \\sim C19 \\sim C19 \\sim C19A \\sim C19A \\sim C19A \\sim
C20 \\sim C20 \\sim C20 \\sim C20A \\sim C20A \\sim C20A: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02
S2 \\sim S2 \\sim S2 \\sim S2A \\sim S2A \\sim S2A \\sim C22 \\sim C22 \\sim
C22 \\sim C22 \\sim C22 \\sim C23 \\sim C23 \\sim C23 \\sim C23A \\sim C23A
\\sim C23A \\sim C24 \\sim C24 \\sim C24 \\sim C24A \\sim C24A \\sim C24A \\sim
C25 \\sim C25 \\sim C25 \\sim C25A \\sim C25A \\sim C25A: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02
S3 \\sim S3 \\sim S3 \\sim S3A \\sim S3A \\sim S3A \\sim C27 \\sim C27 \\sim
C27 \\sim C27 \\sim C27 \\sim C28 \\sim C28 \\sim C28 \\sim C28A \\sim C28A
\\sim C28A \\sim C29 \\sim C29 \\sim C29 \\sim C29A \\sim C29A \\sim C29A \\sim
C30 \\sim C30 \\sim C30 \\sim C30A \\sim C30A \\sim C30A: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(S1A)=Sof(C18A)=Sof(H18A)=Sof(C19A)=Sof(H19A)=Sof(C20A)=Sof(H20A)=1-FVAR(1)
 Sof(S1)=Sof(C18)=Sof(H18)=Sof(C19)=Sof(H19)=Sof(C20)=Sof(H20)=FVAR(1)
 Sof(S2A)=Sof(C23A)=Sof(H23A)=Sof(C24A)=Sof(H24A)=Sof(C25A)=Sof(H25A)=1-FVAR(2)
 Sof(S2)=Sof(C23)=Sof(H23)=Sof(C24)=Sof(H24)=Sof(C25)=Sof(H25)=FVAR(2)
 Sof(S3A)=Sof(C28A)=Sof(H28A)=Sof(C29A)=Sof(H29A)=Sof(C30A)=Sof(H30A)=1-FVAR(3)
 Sof(S3)=Sof(C28)=Sof(H28)=Sof(C29)=Sof(H29)=Sof(C30)=Sof(H30)=FVAR(3)
6.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C12(H12), C13(H13),
 C14(H14), C15(H15), C18(H18), C18A(H18A), C19(H19), C19A(H19A), C20(H20),
 C20A(H20A), C23(H23), C23A(H23A), C24(H24), C24A(H24A), C25(H25), C25A(H25A),
 C28(H28), C28A(H28A), C29(H29), C29A(H29A), C30(H30), C30A(H30A)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Er1 Er 0.45448(2) 0.28873(2) 0.70547(2) 0.00584(4) Uani 1 1 d . U . . .
S1 S 0.73932(9) 0.08118(13) 0.69569(13) 0.0180(3) Uani 0.745(3) 1 d D U P A 1
S1A S 0.7664(4) 0.3547(6) 0.6702(7) 0.0176(12) Uani 0.255(3) 1 d D U P A 2
S2 S 0.61129(10) -0.00872(14) 0.98345(9) 0.0142(3) Uani 0.718(4) 1 d D U P B 1
S2A S 0.6578(4) 0.2499(5) 0.9319(4) 0.0163(10) Uani 0.282(4) 1 d D U P B 2
S3 S 0.32769(10) 0.26895(12) 0.89618(7) 0.0145(3) Uani 0.802(3) 1 d D U P C 1
S3A S 0.2559(8) 0.5152(9) 0.9021(5) 0.0138(13) Uani 0.198(3) 1 d D U P C 2
O1 O 0.56563(11) 0.15511(18) 0.66353(11) 0.0126(4) Uani 1 1 d . U . . .
O2 O 0.58471(11) 0.36978(18) 0.67708(10) 0.0119(4) Uani 1 1 d . U . . .
O3 O 0.50768(12) 0.00416(18) 0.83268(12) 0.0177(4) Uani 1 1 d . U . . .
O4 O 0.52020(11) 0.22241(17) 0.81861(10) 0.0109(4) Uani 1 1 d . U . . .
O5 O 0.32357(11) 0.31704(18) 0.72403(11) 0.0122(4) Uani 1 1 d . U . . .
O6 O 0.23120(11) 0.47811(19) 0.72467(11) 0.0164(4) Uani 1 1 d . U . . .
O7 O 0.40731(11) 0.07116(18) 0.71495(10) 0.0108(3) Uani 1 1 d D U . . .
H7A H 0.3606(11) 0.059(3) 0.7315(17) 0.016 Uiso 1 1 d DR . . . .
H7B H 0.4384(14) 0.034(3) 0.7510(15) 0.016 Uiso 1 1 d DR . . . .
N1 N 0.46039(12) 0.4951(2) 0.78577(12) 0.0086(4) Uani 1 1 d . U . . .
N2 N 0.42163(12) 0.4938(2) 0.63082(12) 0.0084(4) Uani 1 1 d . U . . .
N3 N 0.42284(13) 0.2541(2) 0.56401(12) 0.0090(4) Uani 1 1 d . U . . .
C1 C 0.48084(15) 0.4935(3) 0.86346(15) 0.0116(5) Uani 1 1 d . U . . .
H1 H 0.4985 0.4129 0.8868 0.014 Uiso 1 1 calc R . . . .
C2 C 0.47729(16) 0.6041(3) 0.91059(15) 0.0136(5) Uani 1 1 d . U . . .
H2 H 0.4931 0.5994 0.9648 0.016 Uiso 1 1 calc R . . . .
C3 C 0.45043(17) 0.7213(3) 0.87758(16) 0.0151(5) Uani 1 1 d . U . . .
H3 H 0.4471 0.7984 0.9087 0.018 Uiso 1 1 calc R . . . .
C4 C 0.42854(17) 0.7241(3) 0.79835(16) 0.0149(5) Uani 1 1 d . U . . .
H4 H 0.4090 0.8033 0.7745 0.018 Uiso 1 1 calc R . . . .
C5 C 0.43525(15) 0.6104(2) 0.75361(15) 0.0094(5) Uani 1 1 d . U . . .
C6 C 0.41672(14) 0.6109(2) 0.66736(15) 0.0093(5) Uani 1 1 d . U . . .
C7 C 0.39617(16) 0.7264(3) 0.62695(16) 0.0133(5) Uani 1 1 d . U . . .
H7 H 0.3939 0.8080 0.6539 0.016 Uiso 1 1 calc R . . . .
C8 C 0.37911(17) 0.7199(3) 0.54697(17) 0.0162(5) Uani 1 1 d . U . . .
H8 H 0.3647 0.7973 0.5182 0.019 Uiso 1 1 calc R . . . .
C9 C 0.38324(16) 0.6002(3) 0.50919(15) 0.0142(5) Uani 1 1 d . U . . .
H9 H 0.3711 0.5942 0.4543 0.017 Uiso 1 1 calc R . . . .
C10 C 0.40528(14) 0.4885(3) 0.55224(15) 0.0101(5) Uani 1 1 d . U . . .
C11 C 0.40968(15) 0.3576(3) 0.51490(14) 0.0101(5) Uani 1 1 d . U . . .
C12 C 0.39964(16) 0.3404(3) 0.43378(15) 0.0137(5) Uani 1 1 d . U . . .
H12 H 0.3920 0.4143 0.4000 0.016 Uiso 1 1 calc R . . . .
C13 C 0.40107(17) 0.2138(3) 0.40334(16) 0.0164(5) Uani 1 1 d . U . . .
H13 H 0.3941 0.1999 0.3484 0.020 Uiso 1 1 calc R . . . .
C14 C 0.41282(16) 0.1075(3) 0.45372(15) 0.0150(5) Uani 1 1 d . U . . .
H14 H 0.4129 0.0200 0.4341 0.018 Uiso 1 1 calc R . . . .
C15 C 0.42438(15) 0.1322(3) 0.53332(15) 0.0125(5) Uani 1 1 d . U . . .
H15 H 0.4338 0.0598 0.5678 0.015 Uiso 1 1 calc R . . . .
C16 C 0.61245(15) 0.2533(3) 0.67110(14) 0.0100(5) Uani 1 1 d . U . . .
C17 C 0.70088(15) 0.2328(2) 0.67597(15) 0.0131(5) Uani 1 1 d D U . . .
C18 C 0.7614(5) 0.3257(8) 0.6722(8) 0.0123(13) Uani 0.745(3) 1 d D U P A 1
H18 H 0.7508 0.4161 0.6616 0.015 Uiso 0.745(3) 1 calc R . P A 1
C18A C 0.7363(10) 0.1114(12) 0.6903(15) 0.017(2) Uani 0.255(3) 1 d D U P A 2
H18A H 0.7052 0.0333 0.6950 0.021 Uiso 0.255(3) 1 calc R . P A 2
C19 C 0.8414(4) 0.2745(5) 0.6858(5) 0.0177(10) Uani 0.745(3) 1 d D U P A 1
H19 H 0.8901 0.3244 0.6851 0.021 Uiso 0.745(3) 1 calc R . P A 1
C19A C 0.8230(10) 0.1115(17) 0.6975(14) 0.018(2) Uani 0.255(3) 1 d D U P A 2
H19A H 0.8585 0.0390 0.7069 0.021 Uiso 0.255(3) 1 calc R . P A 2
C20 C 0.8368(3) 0.1426(5) 0.6998(4) 0.0170(11) Uani 0.745(3) 1 d D U P A 1
H20 H 0.8832 0.0893 0.7109 0.020 Uiso 0.745(3) 1 calc R . P A 1
C20A C 0.8421(10) 0.2403(15) 0.6878(16) 0.017(2) Uani 0.255(3) 1 d D U P A 2
H20A H 0.8973 0.2672 0.6906 0.021 Uiso 0.255(3) 1 calc R . P A 2
C21 C 0.53792(15) 0.1123(2) 0.85146(15) 0.0110(5) Uani 1 1 d . U . . .
C22 C 0.60008(15) 0.1173(2) 0.91776(15) 0.0118(5) Uani 1 1 d D U . . .
C23 C 0.6548(6) 0.2160(7) 0.9363(6) 0.0164(14) Uani 0.718(4) 1 d D U P B 1
H23 H 0.6572 0.2951 0.9068 0.020 Uiso 0.718(4) 1 calc R . P B 1
C23A C 0.6163(12) 0.0179(14) 0.9708(9) 0.016(2) Uani 0.282(4) 1 d D U P B 2
H23A H 0.5891 -0.0646 0.9684 0.020 Uiso 0.282(4) 1 calc R . P B 2
C24 C 0.7075(6) 0.1905(8) 1.0029(5) 0.0153(11) Uani 0.718(4) 1 d D U P B 1
H24 H 0.7491 0.2477 1.0228 0.018 Uiso 0.718(4) 1 calc R . P B 1
C24A C 0.6775(13) 0.049(2) 1.0297(14) 0.015(2) Uani 0.282(4) 1 d D U P B 2
H24A H 0.6967 -0.0044 1.0723 0.018 Uiso 0.282(4) 1 calc R . P B 2
C25 C 0.6892(4) 0.0718(7) 1.0336(5) 0.0140(11) Uani 0.718(4) 1 d D U P B 1
H25 H 0.7171 0.0363 1.0789 0.017 Uiso 0.718(4) 1 calc R . P B 1
C25A C 0.7026(16) 0.172(2) 1.0122(13) 0.016(2) Uani 0.282(4) 1 d D U P B 2
H25A H 0.7441 0.2144 1.0436 0.020 Uiso 0.282(4) 1 calc R . P B 2
C26 C 0.27791(14) 0.3986(2) 0.75807(15) 0.0100(5) Uani 1 1 d . U . . .
C27 C 0.28488(15) 0.3960(2) 0.84519(14) 0.0119(5) Uani 1 1 d D U . . .
C28 C 0.2622(8) 0.4943(8) 0.8944(4) 0.0103(12) Uani 0.802(3) 1 d D U P C 1
H28 H 0.2380 0.5743 0.8763 0.012 Uiso 0.802(3) 1 calc R . P C 1
C28A C 0.3206(18) 0.2924(18) 0.8861(11) 0.014(2) Uani 0.198(3) 1 d D U P C 2
H28A H 0.3388 0.2143 0.8619 0.017 Uiso 0.198(3) 1 calc R . P C 2
C29 C 0.2786(3) 0.4646(4) 0.9757(3) 0.0140(8) Uani 0.802(3) 1 d D U P C 1
H29 H 0.2660 0.5210 1.0178 0.017 Uiso 0.802(3) 1 calc R . P C 1
C29A C 0.3273(13) 0.3153(19) 0.9688(11) 0.014(2) Uani 0.198(3) 1 d D U P C 2
H29A H 0.3512 0.2569 1.0068 0.017 Uiso 0.198(3) 1 calc R . P C 2
C30 C 0.3147(3) 0.3448(4) 0.9844(2) 0.0141(8) Uani 0.802(3) 1 d D U P C 1
H30 H 0.3309 0.3073 1.0338 0.017 Uiso 0.802(3) 1 calc R . P C 1
C30A C 0.2940(13) 0.4334(18) 0.9841(9) 0.014(2) Uani 0.198(3) 1 d D U P C 2
H30A H 0.2918 0.4682 1.0356 0.016 Uiso 0.198(3) 1 calc R . P C 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Er1 O1 2.4208(18) . ?
Er1 O2 2.3764(18) . ?
Er1 O4 2.2675(17) . ?
Er1 O5 2.2201(18) . ?
Er1 O7 2.3512(18) . ?
Er1 N1 2.503(2) . ?
Er1 N2 2.486(2) . ?
Er1 N3 2.468(2) . ?
Er1 C16 2.728(3) . ?
S1 C17 1.693(3) . ?
S1 C20 1.725(4) . ?
S1A C17 1.651(5) . ?
S1A C20A 1.722(8) . ?
S2 C22 1.705(3) . ?
S2 C25 1.715(5) . ?
S2A C22 1.660(5) . ?
S2A C25A 1.715(8) . ?
S3 C27 1.691(3) . ?
S3 C30 1.715(4) . ?
S3A C27 1.638(6) . ?
S3A C30A 1.718(8) . ?
O1 C16 1.264(3) . ?
O2 C16 1.274(3) . ?
O3 C21 1.241(3) . ?
O4 C21 1.278(3) . ?
O5 C26 1.280(3) . ?
O6 C26 1.235(3) . ?
O7 H7A 0.844(17) . ?
O7 H7B 0.865(17) . ?
N1 C1 1.351(3) . ?
N1 C5 1.349(3) . ?
N2 C6 1.347(3) . ?
N2 C10 1.355(3) . ?
N3 C11 1.354(3) . ?
N3 C15 1.345(3) . ?
C1 H1 0.9500 . ?
C1 C2 1.384(4) . ?
C2 H2 0.9500 . ?
C2 C3 1.380(4) . ?
C3 H3 0.9500 . ?
C3 C4 1.382(4) . ?
C4 H4 0.9500 . ?
C4 C5 1.392(3) . ?
C5 C6 1.488(3) . ?
C6 C7 1.393(3) . ?
C7 H7 0.9500 . ?
C7 C8 1.381(4) . ?
C8 H8 0.9500 . ?
C8 C9 1.379(4) . ?
C9 H9 0.9500 . ?
C9 C10 1.390(4) . ?
C10 C11 1.478(4) . ?
C11 C12 1.396(3) . ?
C12 H12 0.9500 . ?
C12 C13 1.388(4) . ?
C13 H13 0.9500 . ?
C13 C14 1.387(4) . ?
C14 H14 0.9500 . ?
C14 C15 1.385(4) . ?
C15 H15 0.9500 . ?
C16 C17 1.473(3) . ?
C17 C18 1.378(7) . ?
C17 C18A 1.381(9) . ?
C18 H18 0.9500 . ?
C18 C19 1.428(8) . ?
C18A H18A 0.9500 . ?
C18A C19A 1.431(10) . ?
C19 H19 0.9500 . ?
C19 C20 1.364(5) . ?
C19A H19A 0.9500 . ?
C19A C20A 1.358(8) . ?
C20 H20 0.9500 . ?
C20A H20A 0.9500 . ?
C21 C22 1.489(3) . ?
C22 C23 1.375(7) . ?
C22 C23A 1.373(8) . ?
C23 H23 0.9500 . ?
C23 C24 1.418(8) . ?
C23A H23A 0.9500 . ?
C23A C24A 1.425(10) . ?
C24 H24 0.9500 . ?
C24 C25 1.354(5) . ?
C24A H24A 0.9500 . ?
C24A C25A 1.352(8) . ?
C25 H25 0.9500 . ?
C25A H25A 0.9500 . ?
C26 C27 1.485(3) . ?
C27 C28 1.369(6) . ?
C27 C28A 1.378(9) . ?
C28 H28 0.9500 . ?
C28 C29 1.433(8) . ?
C28A H28A 0.9500 . ?
C28A C29A 1.429(10) . ?
C29 H29 0.9500 . ?
C29 C30 1.360(5) . ?
C29A H29A 0.9500 . ?
C29A C30A 1.351(8) . ?
C30 H30 0.9500 . ?
C30A H30A 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 Er1 N1 128.51(6) . . ?
O1 Er1 N2 117.81(6) . . ?
O1 Er1 N3 75.88(6) . . ?
O1 Er1 C16 27.62(7) . . ?
O2 Er1 O1 54.94(6) . . ?
O2 Er1 N1 79.15(6) . . ?
O2 Er1 N2 77.35(6) . . ?
O2 Er1 N3 89.86(7) . . ?
O2 Er1 C16 27.84(7) . . ?
O4 Er1 O1 75.44(6) . . ?
O4 Er1 O2 83.01(6) . . ?
O4 Er1 O7 78.92(6) . . ?
O4 Er1 N1 77.24(6) . . ?
O4 Er1 N2 140.09(7) . . ?
O4 Er1 N3 149.10(7) . . ?
O4 Er1 C16 73.93(7) . . ?
O5 Er1 O1 150.92(6) . . ?
O5 Er1 O2 151.97(6) . . ?
O5 Er1 O4 110.08(7) . . ?
O5 Er1 O7 77.49(6) . . ?
O5 Er1 N1 79.85(7) . . ?
O5 Er1 N2 77.09(7) . . ?
O5 Er1 N3 90.00(7) . . ?
O5 Er1 C16 175.79(7) . . ?
O7 Er1 O1 75.68(6) . . ?
O7 Er1 O2 130.25(6) . . ?
O7 Er1 N1 138.82(6) . . ?
O7 Er1 N2 139.31(6) . . ?
O7 Er1 N3 83.08(7) . . ?
O7 Er1 C16 102.41(7) . . ?
N1 Er1 C16 102.57(7) . . ?
N2 Er1 N1 65.20(7) . . ?
N2 Er1 C16 100.71(7) . . ?
N3 Er1 N1 130.92(7) . . ?
N3 Er1 N2 65.72(7) . . ?
N3 Er1 C16 85.81(7) . . ?
C17 S1 C20 91.1(2) . . ?
C17 S1A C20A 87.5(8) . . ?
C22 S2 C25 91.3(3) . . ?
C22 S2A C25A 87.9(9) . . ?
C27 S3 C30 92.35(19) . . ?
C27 S3A C30A 91.2(8) . . ?
C16 O1 Er1 89.82(15) . . ?
C16 O2 Er1 91.60(15) . . ?
C21 O4 Er1 136.21(16) . . ?
C26 O5 Er1 138.59(16) . . ?
Er1 O7 H7A 119(2) . . ?
Er1 O7 H7B 106(2) . . ?
H7A O7 H7B 102(2) . . ?
C1 N1 Er1 121.88(16) . . ?
C5 N1 Er1 120.09(16) . . ?
C5 N1 C1 117.7(2) . . ?
C6 N2 Er1 121.26(16) . . ?
C6 N2 C10 118.6(2) . . ?
C10 N2 Er1 120.06(16) . . ?
C11 N3 Er1 120.90(16) . . ?
C15 N3 Er1 120.31(17) . . ?
C15 N3 C11 118.6(2) . . ?
N1 C1 H1 118.5 . . ?
N1 C1 C2 123.0(2) . . ?
C2 C1 H1 118.5 . . ?
C1 C2 H2 120.5 . . ?
C3 C2 C1 119.0(2) . . ?
C3 C2 H2 120.5 . . ?
C2 C3 H3 120.7 . . ?
C2 C3 C4 118.7(2) . . ?
C4 C3 H3 120.7 . . ?
C3 C4 H4 120.1 . . ?
C3 C4 C5 119.7(2) . . ?
C5 C4 H4 120.1 . . ?
N1 C5 C4 121.9(2) . . ?
N1 C5 C6 116.7(2) . . ?
C4 C5 C6 121.4(2) . . ?
N2 C6 C5 116.1(2) . . ?
N2 C6 C7 122.2(2) . . ?
C7 C6 C5 121.7(2) . . ?
C6 C7 H7 120.6 . . ?
C8 C7 C6 118.8(2) . . ?
C8 C7 H7 120.6 . . ?
C7 C8 H8 120.3 . . ?
C9 C8 C7 119.4(2) . . ?
C9 C8 H8 120.3 . . ?
C8 C9 H9 120.3 . . ?
C8 C9 C10 119.4(2) . . ?
C10 C9 H9 120.3 . . ?
N2 C10 C9 121.6(2) . . ?
N2 C10 C11 116.8(2) . . ?
C9 C10 C11 121.6(2) . . ?
N3 C11 C10 116.2(2) . . ?
N3 C11 C12 121.6(2) . . ?
C12 C11 C10 122.2(2) . . ?
C11 C12 H12 120.6 . . ?
C13 C12 C11 118.9(2) . . ?
C13 C12 H12 120.6 . . ?
C12 C13 H13 120.2 . . ?
C14 C13 C12 119.6(2) . . ?
C14 C13 H13 120.2 . . ?
C13 C14 H14 120.8 . . ?
C15 C14 C13 118.4(3) . . ?
C15 C14 H14 120.8 . . ?
N3 C15 C14 123.0(2) . . ?
N3 C15 H15 118.5 . . ?
C14 C15 H15 118.5 . . ?
O1 C16 Er1 62.56(13) . . ?
O1 C16 O2 121.3(2) . . ?
O1 C16 C17 119.6(2) . . ?
O2 C16 Er1 60.56(13) . . ?
O2 C16 C17 119.1(2) . . ?
C17 C16 Er1 164.37(17) . . ?
C16 C17 S1 120.0(2) . . ?
C16 C17 S1A 122.8(3) . . ?
C18 C17 S1 111.5(4) . . ?
C18 C17 C16 128.3(4) . . ?
C18A C17 S1A 114.1(8) . . ?
C18A C17 C16 123.0(8) . . ?
C17 C18 H18 122.9 . . ?
C17 C18 C19 114.2(7) . . ?
C19 C18 H18 122.9 . . ?
C17 C18A H18A 122.4 . . ?
C17 C18A C19A 115.3(15) . . ?
C19A C18A H18A 122.4 . . ?
C18 C19 H19 125.5 . . ?
C20 C19 C18 109.1(6) . . ?
C20 C19 H19 125.5 . . ?
C18A C19A H19A 128.4 . . ?
C20A C19A C18A 103.2(18) . . ?
C20A C19A H19A 128.4 . . ?
S1 C20 H20 122.9 . . ?
C19 C20 S1 114.1(5) . . ?
C19 C20 H20 122.9 . . ?
S1A C20A H20A 120.0 . . ?
C19A C20A S1A 120.0(16) . . ?
C19A C20A H20A 120.0 . . ?
O3 C21 O4 125.5(2) . . ?
O3 C21 C22 118.6(2) . . ?
O4 C21 C22 115.9(2) . . ?
C21 C22 S2 121.41(19) . . ?
C21 C22 S2A 120.4(3) . . ?
C23 C22 S2 110.4(4) . . ?
C23 C22 C21 128.2(4) . . ?
C23A C22 S2A 114.2(7) . . ?
C23A C22 C21 125.4(7) . . ?
C22 C23 H23 122.6 . . ?
C22 C23 C24 114.8(7) . . ?
C24 C23 H23 122.6 . . ?
C22 C23A H23A 123.0 . . ?
C22 C23A C24A 114.0(15) . . ?
C24A C23A H23A 123.0 . . ?
C23 C24 H24 125.3 . . ?
C25 C24 C23 109.5(8) . . ?
C25 C24 H24 125.3 . . ?
C23A C24A H24A 127.3 . . ?
C25A C24A C23A 105(2) . . ?
C25A C24A H24A 127.3 . . ?
S2 C25 H25 123.0 . . ?
C24 C25 S2 114.0(7) . . ?
C24 C25 H25 123.0 . . ?
S2A C25A H25A 120.8 . . ?
C24A C25A S2A 118.5(18) . . ?
C24A C25A H25A 120.8 . . ?
O5 C26 C27 115.2(2) . . ?
O6 C26 O5 125.6(2) . . ?
O6 C26 C27 119.1(2) . . ?
C26 C27 S3 122.48(19) . . ?
C26 C27 S3A 124.8(4) . . ?
C28 C27 S3 111.2(4) . . ?
C28 C27 C26 126.3(4) . . ?
C28A C27 S3A 113.2(9) . . ?
C28A C27 C26 121.9(9) . . ?
C27 C28 H28 123.3 . . ?
C27 C28 C29 113.4(6) . . ?
C29 C28 H28 123.3 . . ?
C27 C28A H28A 123.7 . . ?
C27 C28A C29A 112.6(16) . . ?
C29A C28A H28A 123.7 . . ?
C28 C29 H29 124.7 . . ?
C30 C29 C28 110.7(5) . . ?
C30 C29 H29 124.7 . . ?
C28A C29A H29A 125.5 . . ?
C30A C29A C28A 108.9(19) . . ?
C30A C29A H29A 125.5 . . ?
S3 C30 H30 123.8 . . ?
C29 C30 S3 112.4(4) . . ?
C29 C30 H30 123.8 . . ?
S3A C30A H30A 123.0 . . ?
C29A C30A S3A 114.0(16) . . ?
C29A C30A H30A 123.0 . . ?

_olex2_submission_special_instructions 'No special instructions were received'

####################################################################### 
# 
# 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_final_a_CCDC5
_database_code_depnum_ccdc_archive 'CCDC 1544454'
_audit_update_record             
;
2017-04-17 deposited with the CCDC.
2017-08-23 downloaded from the CCDC.
;
_audit_creation_date             2017-04-06
_audit_creation_method           
;
Olex2 1.2
(compiled Mar 28 2017 19:26:29 for OlexSys, GUI svn.r5335)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C30 H22 Lu N3 O7 S3'
_chemical_formula_sum            'C30 H22 Lu N3 O7 S3'
_chemical_formula_weight         807.65
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Lu Lu -0.4720 5.8584 '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'

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

_cell_length_a                   8.4315(5)
_cell_length_b                   20.2753(12)
_cell_length_c                   17.5412(11)
_cell_angle_alpha                90
_cell_angle_beta                 98.219(2)
_cell_angle_gamma                90
_cell_volume                     2967.9(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9882
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.11
_cell_measurement_theta_min      2.33
_shelx_estimated_absorpt_T_max   0.760
_shelx_estimated_absorpt_T_min   0.387
_exptl_absorpt_coefficient_mu    3.591
_exptl_absorpt_correction_T_max  0.8282
_exptl_absorpt_correction_T_min  0.4421
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1225 before and 0.0557 after correction.
The Ratio of minimum to maximum transmission is 0.5338.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.808
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1592
_exptl_crystal_size_max          0.326
_exptl_crystal_size_mid          0.081
_exptl_crystal_size_min          0.081
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0407
_diffrn_reflns_av_unetI/netI     0.0226
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            49796
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.326
_diffrn_ambient_temperature      100.01
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5596
_reflns_number_total             6067
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.431
_refine_diff_density_min         -1.110
_refine_diff_density_rms         0.087
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.155
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     514
_refine_ls_number_reflns         6067
_refine_ls_number_restraints     986
_refine_ls_R_factor_all          0.0247
_refine_ls_R_factor_gt           0.0208
_refine_ls_restrained_S_all      1.104
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0084P)²+4.0809P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0412
_refine_ls_wR_factor_ref         0.0420
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O7-H7A = O7-H7B
 0.86 with sigma of 0.02
 S1A-C17 \\sim S1-C17 \\sim S2-C22 \\sim S2A-C22 \\sim S3-C27 \\sim S3A-C27
 with sigma of 0.01
 S1A-C20A \\sim S1-C20 \\sim S2-C25 \\sim S2A-C25A \\sim S3-C30 \\sim S3A-C30A
 with sigma of 0.01
 C30-C29 \\sim C30A-C29A \\sim C25A-C24A \\sim C25-C24 \\sim C20-C19 \\sim
C20A-C19A
 with sigma of 0.01
 C28-C27 \\sim C28A-C27 \\sim C18-C17 \\sim C18A-C17 \\sim C23A-C22 \\sim
C23-C22
 with sigma of 0.01
 C29A-C28A \\sim C29-C28 \\sim C24A-C23A \\sim C24-C23 \\sim C19A-C18A \\sim
C19-C18
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
S1 \\sim S1 \\sim S1 \\sim S1A \\sim S1A \\sim S1A \\sim C17 \\sim C17 \\sim
C17 \\sim C17 \\sim C17 \\sim C18 \\sim C18 \\sim C18 \\sim C18A \\sim C18A
\\sim C18A \\sim C19 \\sim C19 \\sim C19 \\sim C19A \\sim C19A \\sim C19A \\sim
C20 \\sim C20 \\sim C20 \\sim C20A \\sim C20A \\sim C20A: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02
S2 \\sim S2 \\sim S2 \\sim S2A \\sim S2A \\sim S2A \\sim C22 \\sim C22 \\sim
C22 \\sim C22 \\sim C22 \\sim C23 \\sim C23 \\sim C23 \\sim C23A \\sim C23A
\\sim C23A \\sim C24 \\sim C24 \\sim C24 \\sim C24A \\sim C24A \\sim C24A \\sim
C25 \\sim C25 \\sim C25 \\sim C25A \\sim C25A \\sim C25A: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02
S3 \\sim S3A \\sim C28 \\sim C28A \\sim C29 \\sim C29A \\sim C30 \\sim C30A:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(S1A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C18) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(S1A)=Sof(C18A)=Sof(H18A)=Sof(C19A)=Sof(H19A)=Sof(C20A)=Sof(H20A)=1-FVAR(1)
 Sof(S1)=Sof(C18)=Sof(H18)=Sof(C19)=Sof(H19)=Sof(C20)=Sof(H20)=FVAR(1)
 Sof(S2A)=Sof(C23A)=Sof(H23A)=Sof(C24A)=Sof(H24A)=Sof(C25A)=Sof(H25A)=1-FVAR(2)
 Sof(S2)=Sof(C23)=Sof(H23)=Sof(C24)=Sof(H24)=Sof(C25)=Sof(H25)=FVAR(2)
 Sof(S3A)=Sof(C28A)=Sof(H28A)=Sof(C29A)=Sof(H29A)=Sof(C30A)=Sof(H30A)=1-FVAR(3)
 Sof(S3)=Sof(C28)=Sof(H28)=Sof(C29)=Sof(H29)=Sof(C30)=Sof(H30)=FVAR(3)
6.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C12(H12), C13(H13),
 C14(H14), C15(H15), C18(H18), C18A(H18A), C19(H19), C19A(H19A), C20(H20),
 C20A(H20A), C23(H23), C23A(H23A), C24(H24), C24A(H24A), C25(H25), C25A(H25A),
 C28(H28), C28A(H28A), C29(H29), C29A(H29A), C30(H30), C30A(H30A)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Lu1 Lu 0.76956(2) 0.62731(2) 0.32958(2) 0.00823(4) Uani 1 1 d . U . . .
S1 S 0.5428(3) 0.38287(8) 0.30248(11) 0.0170(4) Uani 0.721(4) 1 d D U P A 1
S1A S 0.6617(10) 0.4093(4) 0.1689(3) 0.0251(12) Uani 0.279(4) 1 d D U P A 2
S2 S 0.23874(14) 0.65833(9) 0.16561(7) 0.0197(4) Uani 0.731(4) 1 d D U P B 1
S2A S 0.3787(5) 0.6176(3) 0.0285(2) 0.0157(10) Uani 0.269(4) 1 d D U P B 2
S3 S 0.7559(5) 0.84096(13) 0.45632(17) 0.0165(6) Uani 0.460(4) 1 d D U P C 1
S3A S 0.8788(5) 0.92006(11) 0.34048(19) 0.0277(6) Uani 0.540(4) 1 d D U P C 2
O1 O 0.6579(2) 0.52238(8) 0.34801(10) 0.0132(4) Uani 1 1 d . U . . .
O2 O 0.7632(2) 0.54013(9) 0.24153(10) 0.0146(4) Uani 1 1 d . U . . .
O3 O 0.5764(2) 0.66003(9) 0.23640(9) 0.0144(4) Uani 1 1 d . U . . .
O4 O 0.6797(2) 0.65913(11) 0.12526(10) 0.0242(5) Uani 1 1 d . U . . .
O5 O 0.8379(2) 0.72926(8) 0.36851(10) 0.0153(4) Uani 1 1 d . U . . .
O6 O 0.9492(3) 0.78657(10) 0.28082(12) 0.0299(5) Uani 1 1 d . U . . .
O7 O 0.9240(2) 0.66182(9) 0.23789(10) 0.0142(4) Uani 1 1 d D U . . .
H7A H 0.859(3) 0.6606(15) 0.1969(13) 0.021 Uiso 1 1 d DR . . . .
H7B H 0.946(4) 0.7013(9) 0.2460(17) 0.021 Uiso 1 1 d DR . . . .
N1 N 0.5553(2) 0.65850(10) 0.40549(12) 0.0112(4) Uani 1 1 d . U . . .
N2 N 0.8483(2) 0.62169(10) 0.46980(11) 0.0094(4) Uani 1 1 d . U . . .
N3 N 1.0259(2) 0.57205(10) 0.36944(12) 0.0115(4) Uani 1 1 d . U . . .
C1 C 0.4038(3) 0.67041(12) 0.37308(15) 0.0132(5) Uani 1 1 d . U . . .
H1 H 0.3747 0.6601 0.3201 0.016 Uiso 1 1 calc R . . . .
C2 C 0.2879(3) 0.69681(12) 0.41261(15) 0.0157(5) Uani 1 1 d . U . . .
H2 H 0.1817 0.7038 0.3876 0.019 Uiso 1 1 calc R . . . .
C3 C 0.3306(3) 0.71272(13) 0.48957(16) 0.0172(6) Uani 1 1 d . U . . .
H3 H 0.2547 0.7316 0.5183 0.021 Uiso 1 1 calc R . . . .
C4 C 0.4858(3) 0.70059(13) 0.52363(15) 0.0155(5) Uani 1 1 d . U . . .
H4 H 0.5177 0.7115 0.5763 0.019 Uiso 1 1 calc R . . . .
C5 C 0.5952(3) 0.67255(12) 0.48121(14) 0.0115(5) Uani 1 1 d . U . . .
C6 C 0.7600(3) 0.65406(12) 0.51623(14) 0.0123(5) Uani 1 1 d . U . . .
C7 C 0.8197(3) 0.66693(13) 0.59308(15) 0.0179(6) Uani 1 1 d . U . . .
H7 H 0.7579 0.6914 0.6244 0.021 Uiso 1 1 calc R . . . .
C8 C 0.9699(3) 0.64369(14) 0.62322(15) 0.0190(6) Uani 1 1 d . U . . .
H8 H 1.0122 0.6518 0.6755 0.023 Uiso 1 1 calc R . . . .
C9 C 1.0573(3) 0.60844(13) 0.57616(15) 0.0168(6) Uani 1 1 d . U . . .
H9 H 1.1594 0.5909 0.5960 0.020 Uiso 1 1 calc R . . . .
C10 C 0.9938(3) 0.59897(12) 0.49939(14) 0.0118(5) Uani 1 1 d . U . . .
C11 C 1.0863(3) 0.56559(12) 0.44453(14) 0.0110(5) Uani 1 1 d . U . . .
C12 C 1.2270(3) 0.53122(12) 0.46840(15) 0.0144(5) Uani 1 1 d . U . . .
H12 H 1.2648 0.5259 0.5217 0.017 Uiso 1 1 calc R . . . .
C13 C 1.3119(3) 0.50479(13) 0.41351(15) 0.0166(6) Uani 1 1 d . U . . .
H13 H 1.4096 0.4818 0.4286 0.020 Uiso 1 1 calc R . . . .
C14 C 1.2516(3) 0.51253(13) 0.33630(15) 0.0162(5) Uani 1 1 d . U . . .
H14 H 1.3080 0.4954 0.2975 0.019 Uiso 1 1 calc R . . . .
C15 C 1.1083(3) 0.54549(12) 0.31667(15) 0.0137(5) Uani 1 1 d . U . . .
H15 H 1.0660 0.5496 0.2637 0.016 Uiso 1 1 calc R . . . .
C16 C 0.6897(3) 0.50306(12) 0.28245(14) 0.0123(5) Uani 1 1 d . U . . .
C17 C 0.6411(3) 0.43719(12) 0.25432(14) 0.0160(5) Uani 1 1 d D U . . .
C18 C 0.6775(15) 0.4108(5) 0.1864(4) 0.0223(17) Uani 0.721(4) 1 d D U P A 1
H18 H 0.7364 0.4333 0.1521 0.027 Uiso 0.721(4) 1 calc R . P A 1
C18A C 0.554(3) 0.3940(8) 0.2935(11) 0.017(2) Uani 0.279(4) 1 d D U P A 2
H18A H 0.5190 0.4042 0.3413 0.020 Uiso 0.279(4) 1 calc R . P A 2
C19 C 0.6157(7) 0.3453(3) 0.1739(3) 0.0290(11) Uani 0.721(4) 1 d D U P A 1
H19 H 0.6247 0.3201 0.1291 0.035 Uiso 0.721(4) 1 calc R . P A 1
C19A C 0.522(2) 0.3325(8) 0.2543(8) 0.019(2) Uani 0.279(4) 1 d D U P A 2
H19A H 0.4727 0.2954 0.2743 0.023 Uiso 0.279(4) 1 calc R . P A 2
C20 C 0.5430(7) 0.3235(3) 0.2333(3) 0.0198(11) Uani 0.721(4) 1 d D U P A 1
H20 H 0.4981 0.2807 0.2361 0.024 Uiso 0.721(4) 1 calc R . P A 1
C20A C 0.5714(18) 0.3355(6) 0.1845(9) 0.023(2) Uani 0.279(4) 1 d D U P A 2
H20A H 0.5580 0.3006 0.1480 0.027 Uiso 0.279(4) 1 calc R . P A 2
C21 C 0.5655(3) 0.65552(13) 0.16268(14) 0.0150(5) Uani 1 1 d . U . . .
C22 C 0.4020(3) 0.64671(13) 0.12016(14) 0.0145(5) Uani 1 1 d D U . . .
C23 C 0.3571(8) 0.6314(4) 0.0438(4) 0.0189(14) Uani 0.731(4) 1 d D U P B 1
H23 H 0.4326 0.6258 0.0090 0.023 Uiso 0.731(4) 1 calc R . P B 1
C23A C 0.2550(13) 0.6589(11) 0.1439(8) 0.022(2) Uani 0.269(4) 1 d D U P B 2
H23A H 0.2492 0.6733 0.1950 0.026 Uiso 0.269(4) 1 calc R . P B 2
C24 C 0.1889(7) 0.6245(6) 0.0207(7) 0.0188(13) Uani 0.731(4) 1 d D U P B 1
H24 H 0.1380 0.6107 -0.0285 0.023 Uiso 0.731(4) 1 calc R . P B 1
C24A C 0.112(3) 0.6494(18) 0.0904(13) 0.019(2) Uani 0.269(4) 1 d D U P B 2
H24A H 0.0028 0.6534 0.0974 0.023 Uiso 0.269(4) 1 calc R . P B 2
C25 C 0.1146(10) 0.6410(6) 0.0815(5) 0.0191(14) Uani 0.731(4) 1 d D U P B 1
H25 H 0.0012 0.6430 0.0779 0.023 Uiso 0.731(4) 1 calc R . P B 1
C25A C 0.1780(14) 0.6332(17) 0.0272(18) 0.017(2) Uani 0.269(4) 1 d D U P B 2
H25A H 0.1096 0.6302 -0.0207 0.021 Uiso 0.269(4) 1 calc R . P B 2
C26 C 0.8789(3) 0.78308(13) 0.33858(15) 0.0158(5) Uani 1 1 d . U . . .
C27 C 0.8401(3) 0.84479(12) 0.37660(14) 0.0161(5) Uani 1 1 d D U . . .
C28 C 0.864(2) 0.9067(4) 0.3483(9) 0.027(2) Uani 0.460(4) 1 d D U P C 1
H28 H 0.9104 0.9155 0.3032 0.032 Uiso 0.460(4) 1 calc R . P C 1
C28A C 0.7747(16) 0.8542(5) 0.4440(6) 0.020(2) Uani 0.540(4) 1 d D U P C 2
H28A H 0.7420 0.8178 0.4721 0.024 Uiso 0.540(4) 1 calc R . P C 2
C29 C 0.808(2) 0.9560(7) 0.3966(6) 0.0281(17) Uani 0.460(4) 1 d D U P C 1
H29 H 0.8131 1.0023 0.3890 0.034 Uiso 0.460(4) 1 calc R . P C 1
C29A C 0.7580(19) 0.9203(4) 0.4701(6) 0.0239(17) Uani 0.540(4) 1 d D U P C 2
H29A H 0.7202 0.9339 0.5162 0.029 Uiso 0.540(4) 1 calc R . P C 2
C30 C 0.747(2) 0.9258(4) 0.4548(7) 0.0233(19) Uani 0.460(4) 1 d D U P C 1
H30 H 0.7017 0.9501 0.4927 0.028 Uiso 0.460(4) 1 calc R . P C 1
C30A C 0.8072(17) 0.9596(6) 0.4156(5) 0.0289(16) Uani 0.540(4) 1 d D U P C 2
H30A H 0.8025 1.0063 0.4186 0.035 Uiso 0.540(4) 1 calc R . P C 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Lu1 O1 2.3672(17) . ?
Lu1 O2 2.3429(17) . ?
Lu1 O3 2.2366(17) . ?
Lu1 O5 2.2267(17) . ?
Lu1 O7 2.3179(18) . ?
Lu1 N1 2.475(2) . ?
Lu1 N2 2.4569(19) . ?
Lu1 N3 2.446(2) . ?
Lu1 C16 2.706(3) . ?
S1 C17 1.677(3) . ?
S1 C20 1.710(4) . ?
S1A C17 1.633(5) . ?
S1A C20A 1.720(8) . ?
S2 C22 1.703(3) . ?
S2 C25 1.719(5) . ?
S2A C22 1.697(4) . ?
S2A C25A 1.718(9) . ?
S3 C27 1.658(3) . ?
S3 C30 1.722(8) . ?
S3A C27 1.702(3) . ?
S3A C30A 1.724(7) . ?
O1 C16 1.279(3) . ?
O2 C16 1.262(3) . ?
O3 C21 1.287(3) . ?
O4 C21 1.243(3) . ?
O5 C26 1.280(3) . ?
O6 C26 1.247(3) . ?
O7 H7A 0.840(18) . ?
O7 H7B 0.830(18) . ?
N1 C1 1.344(3) . ?
N1 C5 1.353(3) . ?
N2 C6 1.350(3) . ?
N2 C10 1.343(3) . ?
N3 C11 1.349(3) . ?
N3 C15 1.347(3) . ?
C1 H1 0.9500 . ?
C1 C2 1.384(4) . ?
C2 H2 0.9500 . ?
C2 C3 1.385(4) . ?
C3 H3 0.9500 . ?
C3 C4 1.381(4) . ?
C4 H4 0.9500 . ?
C4 C5 1.387(4) . ?
C5 C6 1.485(4) . ?
C6 C7 1.395(4) . ?
C7 H7 0.9500 . ?
C7 C8 1.383(4) . ?
C8 H8 0.9500 . ?
C8 C9 1.382(4) . ?
C9 H9 0.9500 . ?
C9 C10 1.390(4) . ?
C10 C11 1.486(3) . ?
C11 C12 1.388(4) . ?
C12 H12 0.9500 . ?
C12 C13 1.387(4) . ?
C13 H13 0.9500 . ?
C13 C14 1.386(4) . ?
C14 H14 0.9500 . ?
C14 C15 1.381(4) . ?
C15 H15 0.9500 . ?
C16 C17 1.462(4) . ?
C17 C18 1.380(7) . ?
C17 C18A 1.387(9) . ?
C18 H18 0.9500 . ?
C18 C19 1.431(9) . ?
C18A H18A 0.9500 . ?
C18A C19A 1.430(10) . ?
C19 H19 0.9500 . ?
C19 C20 1.357(5) . ?
C19A H19A 0.9500 . ?
C19A C20A 1.351(8) . ?
C20 H20 0.9500 . ?
C20A H20A 0.9500 . ?
C21 C22 1.481(4) . ?
C22 C23 1.374(6) . ?
C22 C23A 1.385(8) . ?
C23 H23 0.9500 . ?
C23 C24 1.425(8) . ?
C23A H23A 0.9500 . ?
C23A C24A 1.430(10) . ?
C24 H24 0.9500 . ?
C24 C25 1.353(5) . ?
C24A H24A 0.9500 . ?
C24A C25A 1.351(8) . ?
C25 H25 0.9500 . ?
C25A H25A 0.9500 . ?
C26 C27 1.477(4) . ?
C27 C28 1.374(8) . ?
C27 C28A 1.388(7) . ?
C28 H28 0.9500 . ?
C28 C29 1.431(10) . ?
C28A H28A 0.9500 . ?
C28A C29A 1.430(9) . ?
C29 H29 0.9500 . ?
C29 C30 1.354(7) . ?
C29A H29A 0.9500 . ?
C29A C30A 1.354(6) . ?
C30 H30 0.9500 . ?
C30A H30A 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 Lu1 N1 79.70(6) . . ?
O1 Lu1 N2 82.96(6) . . ?
O1 Lu1 N3 84.35(6) . . ?
O1 Lu1 C16 28.19(7) . . ?
O2 Lu1 O1 55.93(6) . . ?
O2 Lu1 N1 126.71(6) . . ?
O2 Lu1 N2 127.04(6) . . ?
O2 Lu1 N3 77.23(6) . . ?
O2 Lu1 C16 27.76(7) . . ?
O3 Lu1 O1 95.98(6) . . ?
O3 Lu1 O2 78.25(6) . . ?
O3 Lu1 O7 79.98(6) . . ?
O3 Lu1 N1 78.83(6) . . ?
O3 Lu1 N2 144.06(6) . . ?
O3 Lu1 N3 150.00(6) . . ?
O3 Lu1 C16 85.95(7) . . ?
O5 Lu1 O1 151.99(6) . . ?
O5 Lu1 O2 152.01(6) . . ?
O5 Lu1 O3 94.48(7) . . ?
O5 Lu1 O7 77.65(7) . . ?
O5 Lu1 N1 76.97(7) . . ?
O5 Lu1 N2 73.44(6) . . ?
O5 Lu1 N3 99.11(7) . . ?
O5 Lu1 C16 179.43(7) . . ?
O7 Lu1 O1 129.79(6) . . ?
O7 Lu1 O2 74.48(6) . . ?
O7 Lu1 N1 145.30(7) . . ?
O7 Lu1 N2 127.62(7) . . ?
O7 Lu1 N3 77.02(7) . . ?
O7 Lu1 C16 102.07(7) . . ?
N1 Lu1 C16 103.49(7) . . ?
N2 Lu1 N1 65.59(7) . . ?
N2 Lu1 C16 106.41(7) . . ?
N3 Lu1 N1 130.27(7) . . ?
N3 Lu1 N2 65.88(7) . . ?
N3 Lu1 C16 80.34(7) . . ?
C17 S1 C20 93.1(2) . . ?
C17 S1A C20A 92.7(7) . . ?
C22 S2 C25 90.2(3) . . ?
C22 S2A C25A 86.0(10) . . ?
C27 S3 C30 87.9(5) . . ?
C27 S3A C30A 91.5(5) . . ?
C16 O1 Lu1 90.81(14) . . ?
C16 O2 Lu1 92.37(14) . . ?
C21 O3 Lu1 130.81(16) . . ?
C26 O5 Lu1 137.63(17) . . ?
Lu1 O7 H7A 103(2) . . ?
Lu1 O7 H7B 108(2) . . ?
H7A O7 H7B 106(3) . . ?
C1 N1 Lu1 122.76(16) . . ?
C1 N1 C5 117.7(2) . . ?
C5 N1 Lu1 118.95(16) . . ?
C6 N2 Lu1 119.22(16) . . ?
C10 N2 Lu1 120.26(16) . . ?
C10 N2 C6 119.0(2) . . ?
C11 N3 Lu1 121.24(16) . . ?
C15 N3 Lu1 120.55(16) . . ?
C15 N3 C11 118.2(2) . . ?
N1 C1 H1 118.2 . . ?
N1 C1 C2 123.6(2) . . ?
C2 C1 H1 118.2 . . ?
C1 C2 H2 120.8 . . ?
C1 C2 C3 118.3(2) . . ?
C3 C2 H2 120.8 . . ?
C2 C3 H3 120.7 . . ?
C4 C3 C2 118.6(2) . . ?
C4 C3 H3 120.7 . . ?
C3 C4 H4 119.9 . . ?
C3 C4 C5 120.2(2) . . ?
C5 C4 H4 119.9 . . ?
N1 C5 C4 121.5(2) . . ?
N1 C5 C6 116.1(2) . . ?
C4 C5 C6 122.4(2) . . ?
N2 C6 C5 115.9(2) . . ?
N2 C6 C7 121.4(2) . . ?
C7 C6 C5 122.7(2) . . ?
C6 C7 H7 120.3 . . ?
C8 C7 C6 119.3(2) . . ?
C8 C7 H7 120.3 . . ?
C7 C8 H8 120.5 . . ?
C9 C8 C7 119.0(2) . . ?
C9 C8 H8 120.5 . . ?
C8 C9 H9 120.5 . . ?
C8 C9 C10 119.0(2) . . ?
C10 C9 H9 120.5 . . ?
N2 C10 C9 122.1(2) . . ?
N2 C10 C11 116.2(2) . . ?
C9 C10 C11 121.7(2) . . ?
N3 C11 C10 115.4(2) . . ?
N3 C11 C12 122.0(2) . . ?
C12 C11 C10 122.6(2) . . ?
C11 C12 H12 120.4 . . ?
C13 C12 C11 119.2(2) . . ?
C13 C12 H12 120.4 . . ?
C12 C13 H13 120.6 . . ?
C14 C13 C12 118.8(2) . . ?
C14 C13 H13 120.6 . . ?
C13 C14 H14 120.5 . . ?
C15 C14 C13 119.0(2) . . ?
C15 C14 H14 120.5 . . ?
N3 C15 C14 122.8(2) . . ?
N3 C15 H15 118.6 . . ?
C14 C15 H15 118.6 . . ?
O1 C16 Lu1 60.99(12) . . ?
O1 C16 C17 119.9(2) . . ?
O2 C16 Lu1 59.88(13) . . ?
O2 C16 O1 120.8(2) . . ?
O2 C16 C17 119.3(2) . . ?
C17 C16 Lu1 177.43(18) . . ?
C16 C17 S1 124.4(2) . . ?
C16 C17 S1A 124.3(3) . . ?
C18 C17 S1 111.5(4) . . ?
C18 C17 C16 124.0(5) . . ?
C18A C17 S1A 111.7(7) . . ?
C18A C17 C16 123.5(7) . . ?
C17 C18 H18 124.1 . . ?
C17 C18 C19 111.8(7) . . ?
C19 C18 H18 124.1 . . ?
C17 C18A H18A 123.5 . . ?
C17 C18A C19A 113.0(14) . . ?
C19A C18A H18A 123.5 . . ?
C18 C19 H19 123.9 . . ?
C20 C19 C18 112.3(6) . . ?
C20 C19 H19 123.9 . . ?
C18A C19A H19A 125.2 . . ?
C20A C19A C18A 109.5(16) . . ?
C20A C19A H19A 125.2 . . ?
S1 C20 H20 124.4 . . ?
C19 C20 S1 111.2(5) . . ?
C19 C20 H20 124.4 . . ?
S1A C20A H20A 123.7 . . ?
C19A C20A S1A 112.6(13) . . ?
C19A C20A H20A 123.7 . . ?
O3 C21 C22 116.3(2) . . ?
O4 C21 O3 125.2(2) . . ?
O4 C21 C22 118.5(2) . . ?
C21 C22 S2 120.26(18) . . ?
C21 C22 S2A 119.5(2) . . ?
C23 C22 S2 111.0(3) . . ?
C23 C22 C21 128.7(3) . . ?
C23A C22 S2A 111.0(7) . . ?
C23A C22 C21 129.5(7) . . ?
C22 C23 H23 122.5 . . ?
C22 C23 C24 115.1(7) . . ?
C24 C23 H23 122.5 . . ?
C22 C23A H23A 120.5 . . ?
C22 C23A C24A 119.1(16) . . ?
C24A C23A H23A 120.5 . . ?
C23 C24 H24 126.1 . . ?
C25 C24 C23 107.8(9) . . ?
C25 C24 H24 126.1 . . ?
C23A C24A H24A 130.3 . . ?
C25A C24A C23A 99(2) . . ?
C25A C24A H24A 130.3 . . ?
S2 C25 H25 122.2 . . ?
C24 C25 S2 115.7(7) . . ?
C24 C25 H25 122.2 . . ?
S2A C25A H25A 118.2 . . ?
C24A C25A S2A 124(2) . . ?
C24A C25A H25A 118.2 . . ?
O5 C26 C27 116.5(2) . . ?
O6 C26 O5 124.7(2) . . ?
O6 C26 C27 118.8(2) . . ?
C26 C27 S3 119.4(2) . . ?
C26 C27 S3A 121.7(2) . . ?
C28 C27 S3 116.6(6) . . ?
C28 C27 C26 123.9(6) . . ?
C28A C27 S3A 108.3(4) . . ?
C28A C27 C26 130.0(4) . . ?
C27 C28 H28 124.8 . . ?
C27 C28 C29 110.4(11) . . ?
C29 C28 H28 124.8 . . ?
C27 C28A H28A 120.9 . . ?
C27 C28A C29A 118.1(8) . . ?
C29A C28A H28A 120.9 . . ?
C28 C29 H29 125.6 . . ?
C30 C29 C28 108.8(13) . . ?
C30 C29 H29 125.6 . . ?
C28A C29A H29A 127.2 . . ?
C30A C29A C28A 105.7(11) . . ?
C30A C29A H29A 127.2 . . ?
S3 C30 H30 121.9 . . ?
C29 C30 S3 116.3(11) . . ?
C29 C30 H30 121.9 . . ?
S3A C30A H30A 121.8 . . ?
C29A C30A S3A 116.3(10) . . ?
C29A C30A H30A 121.8 . . ?

_olex2_submission_special_instructions 'No special instructions were received'

####################################################################### 
# 
# 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_final_a_CCDC6
_database_code_depnum_ccdc_archive 'CCDC 1544453'
_audit_update_record             
;
2017-04-17 deposited with the CCDC.
2017-08-23 downloaded from the CCDC.
;
_audit_creation_date             2017-04-06
_audit_creation_method           
;
Olex2 1.2
(compiled Mar 28 2017 19:26:29 for OlexSys, GUI svn.r5335)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        'Yb Monomer'
_chemical_formula_moiety         'C30 H22 N3 O7 S3 Yb'
_chemical_formula_sum            'C30 H22 N3 O7 S3 Yb'
_chemical_formula_weight         805.72
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   8.4238(4)
_cell_length_b                   20.2807(9)
_cell_length_c                   17.5653(8)
_cell_angle_alpha                90
_cell_angle_beta                 98.119(2)
_cell_angle_gamma                90
_cell_volume                     2970.8(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9977
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      29.86
_cell_measurement_theta_min      2.33
_shelx_estimated_absorpt_T_max   0.814
_shelx_estimated_absorpt_T_min   0.622
_exptl_absorpt_coefficient_mu    3.412
_exptl_absorpt_correction_T_max  0.8775
_exptl_absorpt_correction_T_min  0.7148
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.0932 before and 0.0625 after correction.
The Ratio of minimum to maximum transmission is 0.8146.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.801
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1588
_exptl_crystal_size_max          0.154
_exptl_crystal_size_mid          0.079
_exptl_crystal_size_min          0.063
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0536
_diffrn_reflns_av_unetI/netI     0.0499
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            27956
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.102
_diffrn_reflns_theta_min         2.342
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5350
_reflns_number_total             6546
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.518
_refine_diff_density_min         -0.924
_refine_diff_density_rms         0.118
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     514
_refine_ls_number_reflns         6546
_refine_ls_number_restraints     999
_refine_ls_R_factor_all          0.0442
_refine_ls_R_factor_gt           0.0287
_refine_ls_restrained_S_all      0.974
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0146P)²+2.9240P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0519
_refine_ls_wR_factor_ref         0.0553
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O7-H7B = O7-H7A
 0.86 with sigma of 0.02
 H7B-H7A
 1.35 with sigma of 0.02
 S1A-C17 \\sim S1-C17 \\sim S2-C22 \\sim S2A-C22 \\sim S3A-C27 \\sim S3-C27
 with sigma of 0.01
 S1A-C20A \\sim S1-C20 \\sim S2A-C25A \\sim S2-C25 \\sim S3A-C30A \\sim S3-C30
 with sigma of 0.01
 C20-C19 \\sim C20A-C19A \\sim C25A-C24A \\sim C25-C24 \\sim C30-C29 \\sim
C30A-C29A
 with sigma of 0.01
 C18-C17 \\sim C18A-C17 \\sim C23A-C22 \\sim C23-C22 \\sim C28-C27 \\sim
C28A-C27
 with sigma of 0.01
 C19-C18 \\sim C19A-C18A \\sim C24-C23 \\sim C24A-C23A \\sim C29A-C28A \\sim
C29-C28
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
S1 \\sim C17 \\sim C18 \\sim C19 \\sim C20 \\sim S1A \\sim C18A \\sim C19A
\\sim C20A \\sim S1 \\sim C17 \\sim C18 \\sim C17 \\sim S1A \\sim C17 \\sim
C18A \\sim C17 \\sim S1 \\sim C20 \\sim C19 \\sim C18 \\sim S1A \\sim C20A
\\sim C19A \\sim C18A \\sim C20 \\sim C19 \\sim C20A \\sim C19A: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
S2 \\sim C22 \\sim C23 \\sim C24 \\sim C25 \\sim S2A \\sim C23A \\sim C24A
\\sim C25A \\sim S2 \\sim C22 \\sim C23 \\sim C22 \\sim S2A \\sim C22 \\sim
C23A \\sim C22 \\sim S2 \\sim C25 \\sim C24 \\sim C23 \\sim S2A \\sim C25A
\\sim C24A \\sim C23A \\sim C25 \\sim C24 \\sim C25A \\sim C24A: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
S3 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim S3A \\sim C28A \\sim C29A
\\sim C30A \\sim S3 \\sim C27 \\sim C28 \\sim C27 \\sim S3A \\sim C27 \\sim
C28A \\sim C27 \\sim S3 \\sim C30 \\sim C29 \\sim C28 \\sim S3A \\sim C30A
\\sim C29A \\sim C28A \\sim C30 \\sim C29 \\sim C30A \\sim C29A: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(S1A)=Sof(C18A)=Sof(H18A)=Sof(C19A)=Sof(H19A)=Sof(C20A)=Sof(H20A)=1-FVAR(1)
 Sof(S1)=Sof(C18)=Sof(H18)=Sof(C19)=Sof(H19)=Sof(C20)=Sof(H20)=FVAR(1)
 Sof(S2A)=Sof(C23A)=Sof(H23A)=Sof(C24A)=Sof(H24A)=Sof(C25A)=Sof(H25A)=1-FVAR(2)
 Sof(S2)=Sof(C23)=Sof(H23)=Sof(C24)=Sof(H24)=Sof(C25)=Sof(H25)=FVAR(2)
 Sof(S3A)=Sof(C28A)=Sof(H28A)=Sof(C29A)=Sof(H29A)=Sof(C30A)=Sof(H30A)=1-FVAR(3)
 Sof(S3)=Sof(C28)=Sof(H28)=Sof(C29)=Sof(H29)=Sof(C30)=Sof(H30)=FVAR(3)
6.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C12(H12), C13(H13),
 C14(H14), C15(H15), C18(H18), C19(H19), C20(H20), C23(H23), C24(H24), C25(H25),
  C28(H28), C29(H29), C30(H30), C18A(H18A), C19A(H19A), C20A(H20A), C23A(H23A),
 C24A(H24A), C25A(H25A), C28A(H28A), C29A(H29A), C30A(H30A)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Yb1 Yb 0.76823(2) 0.62743(2) 0.32921(2) 0.00953(5) Uani 1 1 d . U . . .
S1 S 0.5435(4) 0.38281(10) 0.30282(14) 0.0193(5) Uani 0.722(4) 1 d D U P A 1
S2 S 0.3778(7) 0.6183(4) 0.0277(3) 0.0179(13) Uani 0.261(4) 1 d D U P B 1
S3 S 0.7559(6) 0.84083(16) 0.4560(2) 0.0209(8) Uani 0.469(4) 1 d D U P C 1
O1 O 0.6578(3) 0.52212(11) 0.34810(13) 0.0140(5) Uani 1 1 d . U . . .
O2 O 0.7616(3) 0.54007(11) 0.24126(13) 0.0158(5) Uani 1 1 d . U . . .
O3 O 0.6782(3) 0.65920(14) 0.12461(14) 0.0253(6) Uani 1 1 d . U . . .
O4 O 0.5742(3) 0.66015(12) 0.23559(13) 0.0166(5) Uani 1 1 d . U . . .
O5 O 0.8371(3) 0.72937(11) 0.36787(13) 0.0166(5) Uani 1 1 d . U . . .
O6 O 0.9485(4) 0.78670(12) 0.28031(15) 0.0316(7) Uani 1 1 d . U . . .
O7 O 0.9223(3) 0.66213(12) 0.23707(13) 0.0161(5) Uani 1 1 d D U . . .
H7A H 0.858(4) 0.6602(16) 0.1953(14) 0.024 Uiso 1 1 d DR . . . .
H7B H 0.939(4) 0.7027(10) 0.2456(19) 0.024 Uiso 1 1 d DR . . . .
N1 N 0.5537(3) 0.65858(13) 0.40560(16) 0.0118(6) Uani 1 1 d . U . . .
N2 N 0.8474(3) 0.62179(13) 0.46968(15) 0.0106(6) Uani 1 1 d . U . . .
N3 N 1.0259(3) 0.57194(13) 0.36962(15) 0.0110(6) Uani 1 1 d . U . . .
C1 C 0.4032(4) 0.67077(16) 0.3734(2) 0.0144(7) Uani 1 1 d . U . . .
H1 H 0.3743 0.6607 0.3204 0.017 Uiso 1 1 calc R . . . .
C2 C 0.2873(4) 0.69706(16) 0.4127(2) 0.0170(8) Uani 1 1 d . U . . .
H2 H 0.1811 0.7042 0.3877 0.020 Uiso 1 1 calc R . . . .
C3 C 0.3300(4) 0.71280(16) 0.4895(2) 0.0184(8) Uani 1 1 d . U . . .
H3 H 0.2539 0.7315 0.5183 0.022 Uiso 1 1 calc R . . . .
C4 C 0.4849(4) 0.70077(16) 0.5234(2) 0.0171(8) Uani 1 1 d . U . . .
H4 H 0.5167 0.7117 0.5760 0.020 Uiso 1 1 calc R . . . .
C5 C 0.5945(4) 0.67278(15) 0.48096(19) 0.0117(7) Uani 1 1 d . U . . .
C6 C 0.7593(4) 0.65394(16) 0.51603(19) 0.0118(7) Uani 1 1 d . U . . .
C7 C 0.8186(4) 0.66648(17) 0.59285(19) 0.0182(8) Uani 1 1 d . U . . .
H7 H 0.7563 0.6906 0.6243 0.022 Uiso 1 1 calc R . . . .
C8 C 0.9688(4) 0.64349(18) 0.6228(2) 0.0208(8) Uani 1 1 d . U . . .
H8 H 1.0111 0.6516 0.6750 0.025 Uiso 1 1 calc R . . . .
C9 C 1.0562(4) 0.60872(17) 0.57604(19) 0.0178(8) Uani 1 1 d . U . . .
H9 H 1.1585 0.5913 0.5958 0.021 Uiso 1 1 calc R . . . .
C10 C 0.9930(4) 0.59935(16) 0.49928(19) 0.0125(7) Uani 1 1 d . U . . .
C11 C 1.0859(4) 0.56579(15) 0.44456(19) 0.0107(7) Uani 1 1 d . U . . .
C12 C 1.2271(4) 0.53138(16) 0.4686(2) 0.0153(7) Uani 1 1 d . U . . .
H12 H 1.2652 0.5262 0.5218 0.018 Uiso 1 1 calc R . . . .
C13 C 1.3110(4) 0.50484(17) 0.4136(2) 0.0179(8) Uani 1 1 d . U . . .
H13 H 1.4082 0.4815 0.4286 0.022 Uiso 1 1 calc R . . . .
C14 C 1.2520(4) 0.51258(16) 0.3370(2) 0.0161(7) Uani 1 1 d . U . . .
H14 H 1.3091 0.4956 0.2984 0.019 Uiso 1 1 calc R . . . .
C15 C 1.1083(4) 0.54541(16) 0.3172(2) 0.0144(7) Uani 1 1 d . U . . .
H15 H 1.0661 0.5493 0.2643 0.017 Uiso 1 1 calc R . . . .
C16 C 0.6883(4) 0.50287(16) 0.28211(19) 0.0133(7) Uani 1 1 d . U . . .
C17 C 0.6413(4) 0.43743(16) 0.25465(18) 0.0178(7) Uani 1 1 d D U . . .
C18 C 0.6784(17) 0.4098(6) 0.1879(5) 0.0262(19) Uani 0.722(4) 1 d D U P A 1
H18 H 0.7393 0.4319 0.1541 0.031 Uiso 0.722(4) 1 calc R . P A 1
C19 C 0.6173(9) 0.3451(3) 0.1743(4) 0.0303(14) Uani 0.722(4) 1 d D U P A 1
H19 H 0.6260 0.3202 0.1293 0.036 Uiso 0.722(4) 1 calc R . P A 1
C20 C 0.5448(8) 0.3234(3) 0.2338(3) 0.0213(13) Uani 0.722(4) 1 d D U P A 1
H20 H 0.5004 0.2806 0.2367 0.026 Uiso 0.722(4) 1 calc R . P A 1
C21 C 0.5634(4) 0.65560(18) 0.1615(2) 0.0173(7) Uani 1 1 d . U . . .
C22 C 0.4001(4) 0.64618(16) 0.11939(18) 0.0159(7) Uani 1 1 d D U . . .
C23 C 0.2535(16) 0.6578(14) 0.1435(11) 0.024(2) Uani 0.261(4) 1 d D U P B 1
H23 H 0.2445 0.6750 0.1930 0.029 Uiso 0.261(4) 1 calc R . P B 1
C24 C 0.118(5) 0.642(4) 0.0894(18) 0.024(2) Uani 0.261(4) 1 d D U P B 1
H24 H 0.0092 0.6399 0.0983 0.028 Uiso 0.261(4) 1 calc R . P B 1
C25 C 0.1751(17) 0.631(2) 0.022(3) 0.021(2) Uani 0.261(4) 1 d D U P B 1
H25 H 0.1065 0.6311 -0.0257 0.026 Uiso 0.261(4) 1 calc R . P B 1
C26 C 0.8779(4) 0.78337(17) 0.3380(2) 0.0171(8) Uani 1 1 d . U . . .
C27 C 0.8391(4) 0.84483(16) 0.37598(19) 0.0185(7) Uani 1 1 d D U . . .
C28 C 0.859(3) 0.9070(5) 0.3471(10) 0.028(2) Uani 0.469(4) 1 d D U P C 1
H28 H 0.9029 0.9161 0.3013 0.034 Uiso 0.469(4) 1 calc R . P C 1
C29 C 0.804(2) 0.9553(8) 0.3955(7) 0.0319(19) Uani 0.469(4) 1 d D U P C 1
H29 H 0.8077 1.0016 0.3874 0.038 Uiso 0.469(4) 1 calc R . P C 1
C30 C 0.746(3) 0.9258(4) 0.4552(9) 0.027(2) Uani 0.469(4) 1 d D U P C 1
H30 H 0.7035 0.9502 0.4938 0.033 Uiso 0.469(4) 1 calc R . P C 1
S1A S 0.6630(12) 0.4095(4) 0.1693(3) 0.0262(14) Uani 0.278(4) 1 d D U P A 2
C18A C 0.558(4) 0.3928(10) 0.2940(14) 0.019(2) Uani 0.278(4) 1 d D U P A 2
H18A H 0.5274 0.4027 0.3427 0.023 Uiso 0.278(4) 1 calc R . P A 2
C19A C 0.522(2) 0.3317(9) 0.2567(9) 0.022(2) Uani 0.278(4) 1 d D U P A 2
H19A H 0.4726 0.2947 0.2766 0.026 Uiso 0.278(4) 1 calc R . P A 2
C20A C 0.573(2) 0.3361(7) 0.1871(11) 0.026(2) Uani 0.278(4) 1 d D U P A 2
H20A H 0.5593 0.3012 0.1507 0.031 Uiso 0.278(4) 1 calc R . P A 2
S2A S 0.23713(19) 0.65783(11) 0.16495(9) 0.0225(4) Uani 0.739(4) 1 d D U P B 2
C23A C 0.3551(10) 0.6304(5) 0.0428(4) 0.0234(18) Uani 0.739(4) 1 d D U P B 2
H23A H 0.4299 0.6241 0.0077 0.028 Uiso 0.739(4) 1 calc R . P B 2
C24A C 0.1876(8) 0.6245(8) 0.0215(10) 0.0228(15) Uani 0.739(4) 1 d D U P B 2
H24A H 0.1363 0.6101 -0.0273 0.027 Uiso 0.739(4) 1 calc R . P B 2
C25A C 0.1111(17) 0.6425(12) 0.0812(6) 0.0239(14) Uani 0.739(4) 1 d D U P B 2
H25A H -0.0022 0.6463 0.0770 0.029 Uiso 0.739(4) 1 calc R . P B 2
S3A S 0.8776(6) 0.92022(13) 0.3404(2) 0.0300(8) Uani 0.531(4) 1 d D U P C 2
C28A C 0.771(2) 0.8535(6) 0.4428(7) 0.025(2) Uani 0.531(4) 1 d D U P C 2
H28A H 0.7345 0.8170 0.4696 0.030 Uiso 0.531(4) 1 calc R . P C 2
C29A C 0.757(2) 0.9191(5) 0.4693(8) 0.0279(19) Uani 0.531(4) 1 d D U P C 2
H29A H 0.7199 0.9322 0.5157 0.034 Uiso 0.531(4) 1 calc R . P C 2
C30A C 0.8059(19) 0.9595(7) 0.4156(5) 0.0299(18) Uani 0.531(4) 1 d D U P C 2
H30A H 0.8013 1.0062 0.4193 0.036 Uiso 0.531(4) 1 calc R . P C 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Yb1 O1 2.371(2) . ?
Yb1 O2 2.346(2) . ?
Yb1 O4 2.249(2) . ?
Yb1 O5 2.227(2) . ?
Yb1 O7 2.322(2) . ?
Yb1 H7A 2.65(3) . ?
Yb1 H7B 2.67(3) . ?
Yb1 N1 2.480(3) . ?
Yb1 N2 2.466(3) . ?
Yb1 N3 2.459(3) . ?
Yb1 C16 2.713(3) . ?
S1 C17 1.679(3) . ?
S1 C20 1.711(5) . ?
S2 C22 1.692(5) . ?
S2 C25 1.717(9) . ?
S3 C27 1.659(4) . ?
S3 C30 1.725(8) . ?
O1 C16 1.283(4) . ?
O2 C16 1.261(4) . ?
O3 C21 1.240(4) . ?
O4 C21 1.295(4) . ?
O5 C26 1.282(4) . ?
O6 C26 1.248(4) . ?
O7 H7A 0.850(17) . ?
O7 H7B 0.845(17) . ?
N1 C1 1.337(4) . ?
N1 C5 1.351(4) . ?
N2 C6 1.345(4) . ?
N2 C10 1.342(4) . ?
N3 C11 1.347(4) . ?
N3 C15 1.342(4) . ?
C1 H1 0.9500 . ?
C1 C2 1.380(5) . ?
C2 H2 0.9500 . ?
C2 C3 1.384(5) . ?
C3 H3 0.9500 . ?
C3 C4 1.378(5) . ?
C4 H4 0.9500 . ?
C4 C5 1.388(4) . ?
C5 C6 1.487(5) . ?
C6 C7 1.395(5) . ?
C7 H7 0.9500 . ?
C7 C8 1.381(5) . ?
C8 H8 0.9500 . ?
C8 C9 1.373(5) . ?
C9 H9 0.9500 . ?
C9 C10 1.391(5) . ?
C10 C11 1.487(5) . ?
C11 C12 1.393(4) . ?
C12 H12 0.9500 . ?
C12 C13 1.384(5) . ?
C13 H13 0.9500 . ?
C13 C14 1.375(5) . ?
C14 H14 0.9500 . ?
C14 C15 1.383(5) . ?
C15 H15 0.9500 . ?
C16 C17 1.448(5) . ?
C17 C18 1.376(8) . ?
C17 S1A 1.637(5) . ?
C17 C18A 1.386(10) . ?
C18 H18 0.9500 . ?
C18 C19 1.416(10) . ?
C19 H19 0.9500 . ?
C19 C20 1.356(6) . ?
C20 H20 0.9500 . ?
C21 C22 1.480(5) . ?
C22 C23 1.380(9) . ?
C22 S2A 1.700(3) . ?
C22 C23A 1.383(7) . ?
C23 H23 0.9500 . ?
C23 C24 1.416(12) . ?
C24 H24 0.9500 . ?
C24 C25 1.356(8) . ?
C25 H25 0.9500 . ?
C26 C27 1.472(5) . ?
C27 C28 1.378(9) . ?
C27 S3A 1.700(4) . ?
C27 C28A 1.390(9) . ?
C28 H28 0.9500 . ?
C28 C29 1.417(11) . ?
C29 H29 0.9500 . ?
C29 C30 1.357(7) . ?
C30 H30 0.9500 . ?
S1A C20A 1.721(9) . ?
C18A H18A 0.9500 . ?
C18A C19A 1.415(11) . ?
C19A H19A 0.9500 . ?
C19A C20A 1.352(8) . ?
C20A H20A 0.9500 . ?
S2A C25A 1.717(7) . ?
C23A H23A 0.9500 . ?
C23A C24A 1.412(9) . ?
C24A H24A 0.9500 . ?
C24A C25A 1.356(6) . ?
C25A H25A 0.9500 . ?
S3A C30A 1.724(7) . ?
C28A H28A 0.9500 . ?
C28A C29A 1.420(10) . ?
C29A H29A 0.9500 . ?
C29A C30A 1.358(7) . ?
C30A H30A 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 Yb1 H7A 121.0(6) . . ?
O1 Yb1 H7B 147.5(5) . . ?
O1 Yb1 N1 79.84(8) . . ?
O1 Yb1 N2 82.77(8) . . ?
O1 Yb1 N3 83.98(8) . . ?
O1 Yb1 C16 28.22(8) . . ?
O2 Yb1 O1 55.85(8) . . ?
O2 Yb1 H7A 65.7(7) . . ?
O2 Yb1 H7B 92.0(5) . . ?
O2 Yb1 N1 126.67(8) . . ?
O2 Yb1 N2 127.00(8) . . ?
O2 Yb1 N3 77.44(8) . . ?
O2 Yb1 C16 27.66(8) . . ?
O4 Yb1 O1 96.27(8) . . ?
O4 Yb1 O2 78.12(8) . . ?
O4 Yb1 O7 79.68(8) . . ?
O4 Yb1 H7A 63.0(6) . . ?
O4 Yb1 H7B 79.7(7) . . ?
O4 Yb1 N1 79.08(9) . . ?
O4 Yb1 N2 144.22(8) . . ?
O4 Yb1 N3 150.11(9) . . ?
O4 Yb1 C16 85.90(9) . . ?
O5 Yb1 O1 152.10(8) . . ?
O5 Yb1 O2 151.97(8) . . ?
O5 Yb1 O4 94.60(9) . . ?
O5 Yb1 O7 77.53(8) . . ?
O5 Yb1 H7A 86.8(6) . . ?
O5 Yb1 H7B 60.0(5) . . ?
O5 Yb1 N1 77.11(8) . . ?
O5 Yb1 N2 73.50(8) . . ?
O5 Yb1 N3 98.94(9) . . ?
O5 Yb1 C16 179.27(9) . . ?
O7 Yb1 O1 129.74(8) . . ?
O7 Yb1 O2 74.55(8) . . ?
O7 Yb1 H7A 18.1(5) . . ?
O7 Yb1 H7B 17.7(5) . . ?
O7 Yb1 N1 145.24(9) . . ?
O7 Yb1 N2 127.79(9) . . ?
O7 Yb1 N3 77.44(8) . . ?
O7 Yb1 C16 102.05(9) . . ?
H7A Yb1 H7B 29.3(5) . . ?
N1 Yb1 H7A 137.4(7) . . ?
N1 Yb1 H7B 129.8(6) . . ?
N1 Yb1 C16 103.52(9) . . ?
N2 Yb1 H7A 145.9(5) . . ?
N2 Yb1 H7B 119.1(6) . . ?
N2 Yb1 N1 65.48(9) . . ?
N2 Yb1 C16 106.40(9) . . ?
N3 Yb1 H7A 91.2(7) . . ?
N3 Yb1 H7B 84.2(7) . . ?
N3 Yb1 N1 129.89(9) . . ?
N3 Yb1 N2 65.61(9) . . ?
N3 Yb1 C16 80.38(9) . . ?
C16 Yb1 H7A 93.0(6) . . ?
C16 Yb1 H7B 119.6(5) . . ?
C17 S1 C20 93.1(3) . . ?
C22 S2 C25 88.7(17) . . ?
C27 S3 C30 88.2(6) . . ?
C16 O1 Yb1 90.87(19) . . ?
C16 O2 Yb1 92.60(19) . . ?
C21 O4 Yb1 130.9(2) . . ?
C26 O5 Yb1 137.9(2) . . ?
Yb1 O7 H7A 104(3) . . ?
Yb1 O7 H7B 105(2) . . ?
H7A O7 H7B 105(2) . . ?
C1 N1 Yb1 122.6(2) . . ?
C1 N1 C5 118.0(3) . . ?
C5 N1 Yb1 118.7(2) . . ?
C6 N2 Yb1 119.3(2) . . ?
C10 N2 Yb1 120.4(2) . . ?
C10 N2 C6 118.8(3) . . ?
C11 N3 Yb1 121.2(2) . . ?
C15 N3 Yb1 120.4(2) . . ?
C15 N3 C11 118.4(3) . . ?
N1 C1 H1 118.1 . . ?
N1 C1 C2 123.8(3) . . ?
C2 C1 H1 118.1 . . ?
C1 C2 H2 120.9 . . ?
C1 C2 C3 118.2(3) . . ?
C3 C2 H2 120.9 . . ?
C2 C3 H3 120.6 . . ?
C4 C3 C2 118.8(3) . . ?
C4 C3 H3 120.6 . . ?
C3 C4 H4 120.0 . . ?
C3 C4 C5 120.1(3) . . ?
C5 C4 H4 120.0 . . ?
N1 C5 C4 121.2(3) . . ?
N1 C5 C6 116.4(3) . . ?
C4 C5 C6 122.4(3) . . ?
N2 C6 C5 115.9(3) . . ?
N2 C6 C7 121.4(3) . . ?
C7 C6 C5 122.7(3) . . ?
C6 C7 H7 120.3 . . ?
C8 C7 C6 119.4(3) . . ?
C8 C7 H7 120.3 . . ?
C7 C8 H8 120.5 . . ?
C9 C8 C7 119.0(3) . . ?
C9 C8 H8 120.5 . . ?
C8 C9 H9 120.5 . . ?
C8 C9 C10 119.1(3) . . ?
C10 C9 H9 120.5 . . ?
N2 C10 C9 122.2(3) . . ?
N2 C10 C11 116.1(3) . . ?
C9 C10 C11 121.6(3) . . ?
N3 C11 C10 115.5(3) . . ?
N3 C11 C12 121.9(3) . . ?
C12 C11 C10 122.6(3) . . ?
C11 C12 H12 120.6 . . ?
C13 C12 C11 118.8(3) . . ?
C13 C12 H12 120.6 . . ?
C12 C13 H13 120.4 . . ?
C14 C13 C12 119.3(3) . . ?
C14 C13 H13 120.4 . . ?
C13 C14 H14 120.5 . . ?
C13 C14 C15 119.0(3) . . ?
C15 C14 H14 120.5 . . ?
N3 C15 C14 122.6(3) . . ?
N3 C15 H15 118.7 . . ?
C14 C15 H15 118.7 . . ?
O1 C16 Yb1 60.92(16) . . ?
O1 C16 C17 120.0(3) . . ?
O2 C16 Yb1 59.74(17) . . ?
O2 C16 O1 120.6(3) . . ?
O2 C16 C17 119.5(3) . . ?
C17 C16 Yb1 177.8(3) . . ?
C16 C17 S1 124.6(3) . . ?
C16 C17 S1A 124.1(4) . . ?
C18 C17 S1 110.3(5) . . ?
C18 C17 C16 125.0(5) . . ?
C18A C17 C16 124.4(9) . . ?
C18A C17 S1A 111.2(9) . . ?
C17 C18 H18 123.2 . . ?
C17 C18 C19 113.6(9) . . ?
C19 C18 H18 123.2 . . ?
C18 C19 H19 124.3 . . ?
C20 C19 C18 111.3(7) . . ?
C20 C19 H19 124.3 . . ?
S1 C20 H20 124.3 . . ?
C19 C20 S1 111.5(5) . . ?
C19 C20 H20 124.3 . . ?
O3 C21 O4 124.9(3) . . ?
O3 C21 C22 119.0(3) . . ?
O4 C21 C22 116.1(3) . . ?
C21 C22 S2 119.3(3) . . ?
C21 C22 S2A 120.2(2) . . ?
C23 C22 S2 111.4(9) . . ?
C23 C22 C21 129.3(9) . . ?
C23A C22 C21 128.6(4) . . ?
C23A C22 S2A 111.2(4) . . ?
C22 C23 H23 122.3 . . ?
C22 C23 C24 115(3) . . ?
C24 C23 H23 122.3 . . ?
C23 C24 H24 127.3 . . ?
C25 C24 C23 105(4) . . ?
C25 C24 H24 127.3 . . ?
S2 C25 H25 121.6 . . ?
C24 C25 S2 117(4) . . ?
C24 C25 H25 121.6 . . ?
O5 C26 C27 116.7(3) . . ?
O6 C26 O5 124.4(3) . . ?
O6 C26 C27 119.0(3) . . ?
C26 C27 S3 119.3(3) . . ?
C26 C27 S3A 121.9(3) . . ?
C28 C27 S3 116.4(7) . . ?
C28 C27 C26 124.1(7) . . ?
C28A C27 C26 129.4(5) . . ?
C28A C27 S3A 108.7(5) . . ?
C27 C28 H28 124.9 . . ?
C27 C28 C29 110.1(13) . . ?
C29 C28 H28 124.9 . . ?
C28 C29 H29 125.0 . . ?
C30 C29 C28 110.0(15) . . ?
C30 C29 H29 125.0 . . ?
S3 C30 H30 122.4 . . ?
C29 C30 S3 115.2(13) . . ?
C29 C30 H30 122.4 . . ?
C17 S1A C20A 91.3(8) . . ?
C17 C18A H18A 122.3 . . ?
C17 C18A C19A 115.5(17) . . ?
C19A C18A H18A 122.3 . . ?
C18A C19A H19A 126.7 . . ?
C20A C19A C18A 106.7(18) . . ?
C20A C19A H19A 126.7 . . ?
S1A C20A H20A 122.4 . . ?
C19A C20A S1A 115.1(15) . . ?
C19A C20A H20A 122.4 . . ?
C22 S2A C25A 90.8(6) . . ?
C22 C23A H23A 123.1 . . ?
C22 C23A C24A 113.8(10) . . ?
C24A C23A H23A 123.1 . . ?
C23A C24A H24A 125.1 . . ?
C25A C24A C23A 109.8(14) . . ?
C25A C24A H24A 125.1 . . ?
S2A C25A H25A 123.0 . . ?
C24A C25A S2A 114.1(13) . . ?
C24A C25A H25A 123.0 . . ?
C27 S3A C30A 91.6(6) . . ?
C27 C28A H28A 121.3 . . ?
C27 C28A C29A 117.3(11) . . ?
C29A C28A H28A 121.3 . . ?
C28A C29A H29A 126.6 . . ?
C30A C29A C28A 106.8(13) . . ?
C30A C29A H29A 126.6 . . ?
S3A C30A H30A 122.3 . . ?
C29A C30A S3A 115.4(11) . . ?
C29A C30A H30A 122.3 . . ?

_olex2_submission_original_sample_id RJB396
_olex2_submission_special_instructions 'No special instructions were received'

####################################################################### 
# 
# 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_final_a_CCDC7
_database_code_depnum_ccdc_archive 'CCDC 1544449'
_audit_update_record             
;
2017-04-17 deposited with the CCDC.
2017-08-23 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT415_final_a             
;
PROBLEM: Short Inter D-H..H-X       H1     ..  H8A     ..       1.55 Ang.
RESPONSE: Comments added to CIF
;
_vrf_PLAT415_final_a_2           
;
PROBLEM: Short Inter D-H..H-X       H1     ..  H8B     ..       1.91 Ang.
RESPONSE: Comments already added to CIF
;
# Added during the CSD deposition process: Monday 17 April 2017 03:19 PM
# end Validation Reply Form



_audit_creation_date             2017-04-06
_audit_creation_method           
;
Olex2 1.2
(compiled Mar 28 2017 19:26:29 for OlexSys, GUI svn.r5335)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C60 H44 Ho2 N6 O14 S6, 0.32(H2 O)'
_chemical_formula_sum            'C60 H44.63 Ho2 N6 O14.32 S6'
_chemical_formula_weight         1600.90
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ho Ho -0.2175 4.6783 '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'

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

_cell_length_a                   11.8674(6)
_cell_length_b                   25.2352(12)
_cell_length_c                   9.7280(5)
_cell_angle_alpha                90
_cell_angle_beta                 97.574(2)
_cell_angle_gamma                90
_cell_volume                     2887.9(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9129
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      31.58
_cell_measurement_theta_min      2.37
_shelx_estimated_absorpt_T_max   0.580
_shelx_estimated_absorpt_T_min   0.337
_exptl_absorpt_coefficient_mu    3.012
_exptl_absorpt_correction_T_max  0.6838
_exptl_absorpt_correction_T_min  0.3920
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1070 before and 0.0516 after correction.
The Ratio of minimum to maximum transmission is 0.5733.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.841
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1582
_exptl_crystal_size_max          0.462
_exptl_crystal_size_mid          0.358
_exptl_crystal_size_min          0.203
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0332
_diffrn_reflns_av_unetI/netI     0.0281
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            32543
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.102
_diffrn_reflns_theta_min         2.261
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5728
_reflns_number_total             6348
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.621
_refine_diff_density_min         -1.319
_refine_diff_density_rms         0.101
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.143
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     530
_refine_ls_number_reflns         6348
_refine_ls_number_restraints     1008
_refine_ls_R_factor_all          0.0306
_refine_ls_R_factor_gt           0.0248
_refine_ls_restrained_S_all      1.081
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0137P)²+3.4795P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0465
_refine_ls_wR_factor_ref         0.0477
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O7-H7A = O7-H7B
 0.86 with sigma of 0.02
 O8-H8A = O8-H8B
 0.86 with sigma of 0.02
 H7A-H7B
 1.35 with sigma of 0.02
 H8A-H8B
 1.35 with sigma of 0.02
 S3A-C27 \\sim S3-C27 \\sim S1A-C17 \\sim S1-C17 \\sim S2-C22 \\sim S2A-C22
 with sigma of 0.01
 S3A-C30A \\sim S3-C30 \\sim S1-C20 \\sim S1A-C20A \\sim S2A-C25A \\sim S2-C25
 with sigma of 0.01
 C30A-C29A \\sim C30-C29 \\sim C20A-C19A \\sim C20-C19 \\sim C25A-C24A \\sim
C25-C24
 with sigma of 0.01
 C23-C22 \\sim C23A-C22 \\sim C18A-C17 \\sim C18-C17 \\sim C28A-C27 \\sim
C28-C27
 with sigma of 0.01
 C24-C23 \\sim C24A-C23A \\sim C19A-C18A \\sim C19-C18 \\sim C29A-C28A \\sim
C29-C28
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
S2 \\sim S2 \\sim S2 \\sim C22 \\sim C22 \\sim C22 \\sim C22 \\sim C22 \\sim
C23 \\sim C23 \\sim C23 \\sim C24 \\sim C24 \\sim C24 \\sim C25 \\sim C25 \\sim
C25 \\sim S2A \\sim S2A \\sim S2A \\sim C23A \\sim C23A \\sim C23A \\sim C24A
\\sim C24A \\sim C24A \\sim C25A \\sim C25A \\sim C25A: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
S1 \\sim S1 \\sim S1 \\sim C17 \\sim C17 \\sim C17 \\sim C17 \\sim C17 \\sim
C18 \\sim C18 \\sim C18 \\sim C19 \\sim C19 \\sim C19 \\sim C20 \\sim C20 \\sim
C20 \\sim S1A \\sim S1A \\sim S1A \\sim C18A \\sim C18A \\sim C18A \\sim C19A
\\sim C19A \\sim C19A \\sim C20A \\sim C20A \\sim C20A: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
S3 \\sim S3 \\sim S3 \\sim C27 \\sim C27 \\sim C27 \\sim C27 \\sim C27 \\sim
C28 \\sim C28 \\sim C28 \\sim C29 \\sim C29 \\sim C29 \\sim C30 \\sim C30 \\sim
C30 \\sim S3A \\sim S3A \\sim S3A \\sim C28A \\sim C28A \\sim C28A \\sim C29A
\\sim C29A \\sim C29A \\sim C30A \\sim C30A \\sim C30A: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(O8) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(S1A)=Sof(C18A)=Sof(H18A)=Sof(C19A)=Sof(H19A)=Sof(C20A)=Sof(H20A)=1-FVAR(1)
 Sof(S1)=Sof(C18)=Sof(H18)=Sof(C19)=Sof(H19)=Sof(C20)=Sof(H20)=FVAR(1)
 Sof(S2A)=Sof(C23A)=Sof(H23A)=Sof(C24A)=Sof(H24A)=Sof(C25A)=Sof(H25A)=1-FVAR(2)
 Sof(S2)=Sof(C23)=Sof(H23)=Sof(C24)=Sof(H24)=Sof(C25)=Sof(H25)=FVAR(2)
 Sof(S3A)=Sof(C28A)=Sof(H28A)=Sof(C29A)=Sof(H29A)=Sof(C30A)=Sof(H30A)=1-FVAR(3)
 Sof(S3)=Sof(C28)=Sof(H28)=Sof(C29)=Sof(H29)=Sof(C30)=Sof(H30)=FVAR(3)
 Sof(O8)=Sof(H8A)=Sof(H8B)=FVAR(4)
6.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C12(H12), C13(H13),
 C14(H14), C15(H15), C18(H18), C18A(H18A), C19(H19), C19A(H19A), C20(H20),
 C20A(H20A), C23(H23), C23A(H23A), C24(H24), C24A(H24A), C25(H25), C25A(H25A),
 C28(H28), C28A(H28A), C29(H29), C29A(H29A), C30(H30), C30A(H30A)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ho1 Ho 0.51605(2) 0.40190(2) 0.59664(2) 0.00844(4) Uani 1 1 d . U . . .
S1 S 0.24340(17) 0.44247(8) 0.99886(19) 0.0155(4) Uani 0.663(3) 1 d D U P A 1
S1A S 0.1422(4) 0.3622(2) 0.8106(5) 0.0127(9) Uani 0.337(3) 1 d D U P A 2
S2 S 0.1338(2) 0.53554(10) 0.2629(3) 0.0146(5) Uani 0.508(3) 1 d D U P B 1
S2A S 0.1240(2) 0.43792(10) 0.4293(3) 0.0140(6) Uani 0.492(3) 1 d D U P B 2
S3 S 0.9639(3) 0.32400(19) 0.4004(3) 0.0207(7) Uani 0.398(3) 1 d D U P C 1
S3A S 0.88366(19) 0.29463(9) 0.6567(2) 0.0145(4) Uani 0.602(3) 1 d D U P C 2
O1 O 0.41296(16) 0.44397(7) 0.7855(2) 0.0198(4) Uani 1 1 d . U . . .
O2 O 0.35629(15) 0.36664(7) 0.69417(19) 0.0147(4) Uani 1 1 d . U . . .
O3 O 0.38700(15) 0.52041(7) 0.35336(19) 0.0146(4) Uani 1 1 d . U . . .
O4 O 0.36613(14) 0.45223(7) 0.49377(19) 0.0139(4) Uani 1 1 d . U . . .
O5 O 0.77099(15) 0.39923(7) 0.37587(19) 0.0162(4) Uani 1 1 d . U . . .
O6 O 0.70061(14) 0.37118(7) 0.56618(18) 0.0140(4) Uani 1 1 d . U . . .
O7 O 0.55633(16) 0.43082(8) 0.36877(19) 0.0149(4) Uani 1 1 d D U . . .
H7A H 0.6237(16) 0.4246(11) 0.364(3) 0.022 Uiso 1 1 d DR . . . .
H7B H 0.538(2) 0.4616(8) 0.343(3) 0.022 Uiso 1 1 d DR . . . .
O8 O 0.5048(13) 0.5310(6) 0.8962(14) 0.036(5) Uani 0.158(7) 1 d D U P . .
H8A H 0.534(19) 0.503(5) 0.865(18) 0.053 Uiso 0.158(7) 1 d DR . P . .
H8B H 0.50(2) 0.524(7) 0.982(7) 0.053 Uiso 0.158(7) 1 d DR . P . .
N1 N 0.62133(19) 0.38291(9) 0.8349(2) 0.0164(5) Uani 1 1 d . U . . .
N2 N 0.54986(17) 0.30464(8) 0.6572(2) 0.0103(4) Uani 1 1 d . U . . .
N3 N 0.41686(18) 0.33509(8) 0.4257(2) 0.0114(4) Uani 1 1 d . U . . .
C1 C 0.6514(3) 0.42256(12) 0.9242(3) 0.0258(7) Uani 1 1 d . U . . .
H1 H 0.6148 0.4559 0.9084 0.031 Uiso 1 1 calc R . . . .
C2 C 0.7338(3) 0.41692(13) 1.0386(3) 0.0303(7) Uani 1 1 d . U . . .
H2 H 0.7508 0.4453 1.1020 0.036 Uiso 1 1 calc R . . . .
C3 C 0.7902(3) 0.36936(13) 1.0580(3) 0.0269(7) Uani 1 1 d . U . . .
H3 H 0.8494 0.3649 1.1330 0.032 Uiso 1 1 calc R . . . .
C4 C 0.7596(2) 0.32816(13) 0.9671(3) 0.0227(6) Uani 1 1 d . U . . .
H4 H 0.7984 0.2952 0.9781 0.027 Uiso 1 1 calc R . . . .
C5 C 0.6715(2) 0.33541(11) 0.8593(3) 0.0154(6) Uani 1 1 d . U . . .
C6 C 0.6239(2) 0.29120(11) 0.7688(3) 0.0134(5) Uani 1 1 d . U . . .
C7 C 0.6495(2) 0.23858(11) 0.8031(3) 0.0172(6) Uani 1 1 d . U . . .
H7 H 0.7009 0.2302 0.8835 0.021 Uiso 1 1 calc R . . . .
C8 C 0.5995(2) 0.19904(11) 0.7193(3) 0.0194(6) Uani 1 1 d . U . . .
H8 H 0.6163 0.1629 0.7406 0.023 Uiso 1 1 calc R . . . .
C9 C 0.5246(2) 0.21244(10) 0.6041(3) 0.0162(6) Uani 1 1 d . U . . .
H9 H 0.4897 0.1857 0.5444 0.019 Uiso 1 1 calc R . . . .
C10 C 0.5008(2) 0.26577(10) 0.5761(3) 0.0119(5) Uani 1 1 d . U . . .
C11 C 0.4207(2) 0.28248(10) 0.4533(3) 0.0120(5) Uani 1 1 d . U . . .
C12 C 0.3562(2) 0.24620(11) 0.3695(3) 0.0151(5) Uani 1 1 d . U . . .
H12 H 0.3600 0.2095 0.3919 0.018 Uiso 1 1 calc R . . . .
C13 C 0.2867(2) 0.26353(11) 0.2536(3) 0.0180(6) Uani 1 1 d . U . . .
H13 H 0.2430 0.2390 0.1946 0.022 Uiso 1 1 calc R . . . .
C14 C 0.2814(2) 0.31728(11) 0.2245(3) 0.0185(6) Uani 1 1 d . U . . .
H14 H 0.2337 0.3304 0.1459 0.022 Uiso 1 1 calc R . . . .
C15 C 0.3474(2) 0.35132(11) 0.3130(3) 0.0147(5) Uani 1 1 d . U . . .
H15 H 0.3436 0.3882 0.2930 0.018 Uiso 1 1 calc R . . . .
C16 C 0.3456(2) 0.40526(11) 0.7745(3) 0.0146(5) Uani 1 1 d . U . . .
C17 C 0.2498(2) 0.40332(10) 0.8585(3) 0.0130(5) Uani 1 1 d D U . . .
C18 C 0.1551(7) 0.3714(4) 0.8358(10) 0.0118(16) Uani 0.663(3) 1 d D U P A 1
H18 H 0.1445 0.3467 0.7615 0.014 Uiso 0.663(3) 1 calc R . P A 1
C18A C 0.2329(14) 0.4339(7) 0.9721(14) 0.016(2) Uani 0.337(3) 1 d D U P A 2
H18A H 0.2860 0.4601 1.0090 0.019 Uiso 0.337(3) 1 calc R . P A 2
C19 C 0.0741(9) 0.3775(4) 0.9300(10) 0.0144(13) Uani 0.663(3) 1 d D U P A 1
H19 H 0.0046 0.3587 0.9276 0.017 Uiso 0.663(3) 1 calc R . P A 1
C19A C 0.1317(14) 0.4236(8) 1.030(2) 0.015(2) Uani 0.337(3) 1 d D U P A 2
H19A H 0.1069 0.4400 1.1086 0.018 Uiso 0.337(3) 1 calc R . P A 2
C20 C 0.1140(6) 0.4152(4) 1.0243(11) 0.0136(13) Uani 0.663(3) 1 d D U P A 1
H20 H 0.0739 0.4257 1.0981 0.016 Uiso 0.663(3) 1 calc R . P A 1
C20A C 0.0780(18) 0.3854(9) 0.9484(18) 0.013(2) Uani 0.337(3) 1 d D U P A 2
H20A H 0.0068 0.3717 0.9665 0.016 Uiso 0.337(3) 1 calc R . P A 2
C21 C 0.3269(2) 0.48722(10) 0.4088(3) 0.0100(5) Uani 1 1 d . U . . .
C22 C 0.2025(2) 0.48794(9) 0.3707(3) 0.0105(5) Uani 1 1 d D U . . .
C23 C 0.1247(8) 0.4536(4) 0.4150(12) 0.0136(17) Uani 0.508(3) 1 d D U P B 1
H23 H 0.1468 0.4260 0.4794 0.016 Uiso 0.508(3) 1 calc R . P B 1
C23A C 0.1362(8) 0.5243(4) 0.2936(11) 0.0163(18) Uani 0.492(3) 1 d D U P B 2
H23A H 0.1664 0.5548 0.2548 0.020 Uiso 0.492(3) 1 calc R . P B 2
C24 C 0.0103(11) 0.4618(7) 0.359(2) 0.0156(16) Uani 0.508(3) 1 d D U P B 1
H24 H -0.0523 0.4401 0.3744 0.019 Uiso 0.508(3) 1 calc R . P B 1
C24A C 0.0186(10) 0.5124(7) 0.276(2) 0.0154(16) Uani 0.492(3) 1 d D U P B 2
H24A H -0.0393 0.5324 0.2232 0.018 Uiso 0.492(3) 1 calc R . P B 2
C25 C 0.0050(9) 0.5060(7) 0.279(2) 0.0151(17) Uani 0.508(3) 1 d D U P B 1
H25 H -0.0651 0.5198 0.2354 0.018 Uiso 0.508(3) 1 calc R . P B 1
C25A C 0.0026(11) 0.4678(7) 0.349(2) 0.0140(17) Uani 0.492(3) 1 d D U P B 2
H25A H -0.0710 0.4538 0.3543 0.017 Uiso 0.492(3) 1 calc R . P B 2
C26 C 0.7744(2) 0.37191(10) 0.4832(3) 0.0106(5) Uani 1 1 d . U . . .
C27 C 0.8715(2) 0.33445(10) 0.5151(2) 0.0125(5) Uani 1 1 d D U . . .
C28 C 0.8923(13) 0.2990(6) 0.6237(12) 0.018(2) Uani 0.398(3) 1 d D U P C 1
H28 H 0.8451 0.2975 0.6951 0.021 Uiso 0.398(3) 1 calc R . P C 1
C28A C 0.9577(8) 0.3242(5) 0.4374(9) 0.0198(17) Uani 0.602(3) 1 d D U P C 2
H28A H 0.9650 0.3431 0.3546 0.024 Uiso 0.602(3) 1 calc R . P C 2
C29 C 0.9871(14) 0.2650(9) 0.6237(19) 0.0158(18) Uani 0.398(3) 1 d D U P C 1
H29 H 1.0156 0.2406 0.6940 0.019 Uiso 0.398(3) 1 calc R . P C 1
C29A C 1.0347(10) 0.2840(4) 0.4875(11) 0.0184(14) Uani 0.602(3) 1 d D U P C 2
H29A H 1.0989 0.2728 0.4463 0.022 Uiso 0.602(3) 1 calc R . P C 2
C30 C 1.0289(15) 0.2744(6) 0.5034(18) 0.017(2) Uani 0.398(3) 1 d D U P C 1
H30 H 1.0909 0.2547 0.4770 0.021 Uiso 0.398(3) 1 calc R . P C 1
C30A C 1.0011(9) 0.2641(6) 0.6050(12) 0.0142(15) Uani 0.602(3) 1 d D U P C 2
H30A H 1.0393 0.2356 0.6549 0.017 Uiso 0.602(3) 1 calc R . P C 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ho1 O1 2.5678(18) . ?
Ho1 O2 2.4002(17) . ?
Ho1 O3 2.2926(17) 3_666 ?
Ho1 O4 2.3044(17) . ?
Ho1 O6 2.3785(17) . ?
Ho1 O7 2.4401(18) . ?
Ho1 N1 2.530(2) . ?
Ho1 N2 2.544(2) . ?
Ho1 N3 2.545(2) . ?
Ho1 C16 2.831(3) . ?
S1 C17 1.695(3) . ?
S1 C20 1.730(6) . ?
S1A C17 1.664(4) . ?
S1A C20A 1.730(9) . ?
S2 C22 1.727(3) . ?
S2 C25 1.727(8) . ?
S2A C22 1.710(3) . ?
S2A C25A 1.722(8) . ?
S3 C27 1.685(4) . ?
S3 C30 1.721(8) . ?
S3A C27 1.696(3) . ?
S3A C30A 1.724(6) . ?
O1 C16 1.258(3) . ?
O2 C16 1.266(3) . ?
O3 Ho1 2.2926(17) 3_666 ?
O3 C21 1.266(3) . ?
O4 C21 1.256(3) . ?
O5 C26 1.247(3) . ?
O6 C26 1.267(3) . ?
O7 H7A 0.823(17) . ?
O7 H7B 0.836(16) . ?
O8 H8A 0.86(2) . ?
O8 H8B 0.86(2) . ?
N1 C1 1.342(4) . ?
N1 C5 1.345(4) . ?
N2 C6 1.348(3) . ?
N2 C10 1.343(3) . ?
N3 C11 1.354(3) . ?
N3 C15 1.346(3) . ?
C1 H1 0.9500 . ?
C1 C2 1.388(4) . ?
C2 H2 0.9500 . ?
C2 C3 1.375(5) . ?
C3 H3 0.9500 . ?
C3 C4 1.382(4) . ?
C4 H4 0.9500 . ?
C4 C5 1.392(4) . ?
C5 C6 1.485(4) . ?
C6 C7 1.393(4) . ?
C7 H7 0.9500 . ?
C7 C8 1.373(4) . ?
C8 H8 0.9500 . ?
C8 C9 1.378(4) . ?
C9 H9 0.9500 . ?
C9 C10 1.395(4) . ?
C10 C11 1.486(4) . ?
C11 C12 1.387(4) . ?
C12 H12 0.9500 . ?
C12 C13 1.377(4) . ?
C13 H13 0.9500 . ?
C13 C14 1.385(4) . ?
C14 H14 0.9500 . ?
C14 C15 1.384(4) . ?
C15 H15 0.9500 . ?
C16 C17 1.486(3) . ?
C17 C18 1.376(7) . ?
C17 C18A 1.384(8) . ?
C18 H18 0.9500 . ?
C18 C19 1.421(9) . ?
C18A H18A 0.9500 . ?
C18A C19A 1.416(11) . ?
C19 H19 0.9500 . ?
C19 C20 1.362(5) . ?
C19A H19A 0.9500 . ?
C19A C20A 1.354(8) . ?
C20 H20 0.9500 . ?
C20A H20A 0.9500 . ?
C21 C22 1.474(3) . ?
C22 C23 1.376(7) . ?
C22 C23A 1.366(7) . ?
C23 H23 0.9500 . ?
C23 C24 1.411(10) . ?
C23A H23A 0.9500 . ?
C23A C24A 1.415(10) . ?
C24 H24 0.9500 . ?
C24 C25 1.354(6) . ?
C24A H24A 0.9500 . ?
C24A C25A 1.353(7) . ?
C25 H25 0.9500 . ?
C25A H25A 0.9500 . ?
C26 C27 1.492(4) . ?
C27 C28 1.382(8) . ?
C27 C28A 1.374(7) . ?
C28 H28 0.9500 . ?
C28 C29 1.414(11) . ?
C28A H28A 0.9500 . ?
C28A C29A 1.409(9) . ?
C29 H29 0.9500 . ?
C29 C30 1.351(7) . ?
C29A H29A 0.9500 . ?
C29A C30A 1.355(6) . ?
C30 H30 0.9500 . ?
C30A H30A 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 Ho1 C16 26.37(7) . . ?
O2 Ho1 O1 52.75(6) . . ?
O2 Ho1 O7 136.85(6) . . ?
O2 Ho1 N1 83.57(7) . . ?
O2 Ho1 N2 70.09(6) . . ?
O2 Ho1 N3 72.01(6) . . ?
O2 Ho1 C16 26.40(7) . . ?
O3 Ho1 O1 76.57(6) 3_666 . ?
O3 Ho1 O2 129.32(6) 3_666 . ?
O3 Ho1 O4 87.59(6) 3_666 . ?
O3 Ho1 O6 81.98(6) 3_666 . ?
O3 Ho1 O7 77.53(6) 3_666 . ?
O3 Ho1 N1 78.13(7) 3_666 . ?
O3 Ho1 N2 135.77(7) 3_666 . ?
O3 Ho1 N3 151.77(6) 3_666 . ?
O3 Ho1 C16 102.93(7) 3_666 . ?
O4 Ho1 O1 70.70(6) . . ?
O4 Ho1 O2 76.77(6) . . ?
O4 Ho1 O6 142.80(6) . . ?
O4 Ho1 O7 70.92(6) . . ?
O4 Ho1 N1 139.65(7) . . ?
O4 Ho1 N2 136.18(6) . . ?
O4 Ho1 N3 79.47(7) . . ?
O4 Ho1 C16 71.10(7) . . ?
O6 Ho1 O1 139.23(6) . . ?
O6 Ho1 O2 135.79(6) . . ?
O6 Ho1 O7 71.97(6) . . ?
O6 Ho1 N1 72.58(7) . . ?
O6 Ho1 N2 66.08(6) . . ?
O6 Ho1 N3 93.26(6) . . ?
O6 Ho1 C16 146.07(7) . . ?
O7 Ho1 O1 134.05(6) . . ?
O7 Ho1 N1 139.18(7) . . ?
O7 Ho1 N2 117.07(6) . . ?
O7 Ho1 N3 74.56(6) . . ?
O7 Ho1 C16 141.96(7) . . ?
N1 Ho1 O1 69.33(7) . . ?
N1 Ho1 N2 63.98(7) . . ?
N1 Ho1 N3 127.09(7) . . ?
N1 Ho1 C16 75.64(7) . . ?
N2 Ho1 O1 107.99(6) . . ?
N2 Ho1 N3 63.72(7) . . ?
N2 Ho1 C16 89.49(7) . . ?
N3 Ho1 O1 121.23(6) . . ?
N3 Ho1 C16 96.48(7) . . ?
C17 S1 C20 91.0(3) . . ?
C17 S1A C20A 88.4(7) . . ?
C25 S2 C22 89.8(6) . . ?
C22 S2A C25A 89.1(6) . . ?
C27 S3 C30 90.5(7) . . ?
C27 S3A C30A 90.7(4) . . ?
C16 O1 Ho1 88.57(15) . . ?
C16 O2 Ho1 96.15(15) . . ?
C21 O3 Ho1 140.40(16) . 3_666 ?
C21 O4 Ho1 150.58(16) . . ?
C26 O6 Ho1 143.11(17) . . ?
Ho1 O7 H7A 108(2) . . ?
Ho1 O7 H7B 119(2) . . ?
H7A O7 H7B 112(2) . . ?
H8A O8 H8B 103(3) . . ?
C1 N1 Ho1 120.59(19) . . ?
C1 N1 C5 118.4(2) . . ?
C5 N1 Ho1 118.94(17) . . ?
C6 N2 Ho1 119.71(17) . . ?
C10 N2 Ho1 121.73(16) . . ?
C10 N2 C6 118.4(2) . . ?
C11 N3 Ho1 121.29(17) . . ?
C15 N3 Ho1 120.77(17) . . ?
C15 N3 C11 117.5(2) . . ?
N1 C1 H1 118.6 . . ?
N1 C1 C2 122.8(3) . . ?
C2 C1 H1 118.6 . . ?
C1 C2 H2 120.7 . . ?
C3 C2 C1 118.6(3) . . ?
C3 C2 H2 120.7 . . ?
C2 C3 H3 120.4 . . ?
C2 C3 C4 119.1(3) . . ?
C4 C3 H3 120.4 . . ?
C3 C4 H4 120.3 . . ?
C3 C4 C5 119.4(3) . . ?
C5 C4 H4 120.3 . . ?
N1 C5 C4 121.4(3) . . ?
N1 C5 C6 116.1(2) . . ?
C4 C5 C6 122.5(3) . . ?
N2 C6 C5 116.4(2) . . ?
N2 C6 C7 122.1(3) . . ?
C7 C6 C5 121.4(2) . . ?
C6 C7 H7 120.4 . . ?
C8 C7 C6 119.2(3) . . ?
C8 C7 H7 120.4 . . ?
C7 C8 H8 120.4 . . ?
C7 C8 C9 119.1(3) . . ?
C9 C8 H8 120.4 . . ?
C8 C9 H9 120.4 . . ?
C8 C9 C10 119.2(3) . . ?
C10 C9 H9 120.4 . . ?
N2 C10 C9 121.9(2) . . ?
N2 C10 C11 116.5(2) . . ?
C9 C10 C11 121.5(2) . . ?
N3 C11 C10 116.0(2) . . ?
N3 C11 C12 121.9(2) . . ?
C12 C11 C10 122.0(2) . . ?
C11 C12 H12 120.1 . . ?
C13 C12 C11 119.8(2) . . ?
C13 C12 H12 120.1 . . ?
C12 C13 H13 120.5 . . ?
C12 C13 C14 118.9(3) . . ?
C14 C13 H13 120.5 . . ?
C13 C14 H14 120.8 . . ?
C15 C14 C13 118.3(3) . . ?
C15 C14 H14 120.8 . . ?
N3 C15 C14 123.6(3) . . ?
N3 C15 H15 118.2 . . ?
C14 C15 H15 118.2 . . ?
O1 C16 Ho1 65.06(14) . . ?
O1 C16 O2 122.5(2) . . ?
O1 C16 C17 120.2(2) . . ?
O2 C16 Ho1 57.46(13) . . ?
O2 C16 C17 117.4(2) . . ?
C17 C16 Ho1 174.41(19) . . ?
C16 C17 S1 122.8(2) . . ?
C16 C17 S1A 118.8(2) . . ?
C18 C17 S1 110.4(4) . . ?
C18 C17 C16 126.8(4) . . ?
C18A C17 S1A 112.7(7) . . ?
C18A C17 C16 128.5(7) . . ?
C17 C18 H18 122.0 . . ?
C17 C18 C19 116.1(7) . . ?
C19 C18 H18 122.0 . . ?
C17 C18A H18A 122.1 . . ?
C17 C18A C19A 115.8(14) . . ?
C19A C18A H18A 122.1 . . ?
C18 C19 H19 126.1 . . ?
C20 C19 C18 107.8(9) . . ?
C20 C19 H19 126.1 . . ?
C18A C19A H19A 127.6 . . ?
C20A C19A C18A 104.9(19) . . ?
C20A C19A H19A 127.6 . . ?
S1 C20 H20 122.7 . . ?
C19 C20 S1 114.7(8) . . ?
C19 C20 H20 122.7 . . ?
S1A C20A H20A 120.9 . . ?
C19A C20A S1A 118.3(16) . . ?
C19A C20A H20A 120.9 . . ?
O3 C21 C22 119.1(2) . . ?
O4 C21 O3 124.4(2) . . ?
O4 C21 C22 116.5(2) . . ?
C21 C22 S2 122.59(19) . . ?
C21 C22 S2A 118.56(19) . . ?
C23 C22 S2 110.2(4) . . ?
C23 C22 C21 127.1(4) . . ?
C23A C22 S2A 112.2(5) . . ?
C23A C22 C21 129.2(5) . . ?
C22 C23 H23 122.0 . . ?
C22 C23 C24 115.9(10) . . ?
C24 C23 H23 122.0 . . ?
C22 C23A H23A 122.9 . . ?
C22 C23A C24A 114.2(11) . . ?
C24A C23A H23A 122.9 . . ?
C23 C24 H24 125.9 . . ?
C25 C24 C23 108.2(15) . . ?
C25 C24 H24 125.9 . . ?
C23A C24A H24A 125.7 . . ?
C25A C24A C23A 108.6(16) . . ?
C25A C24A H24A 125.7 . . ?
S2 C25 H25 122.2 . . ?
C24 C25 S2 115.7(14) . . ?
C24 C25 H25 122.2 . . ?
S2A C25A H25A 122.1 . . ?
C24A C25A S2A 115.7(14) . . ?
C24A C25A H25A 122.1 . . ?
O5 C26 O6 126.3(2) . . ?
O5 C26 C27 117.6(2) . . ?
O6 C26 C27 116.0(2) . . ?
C26 C27 S3 120.9(2) . . ?
C26 C27 S3A 121.66(19) . . ?
C28 C27 S3 109.8(6) . . ?
C28 C27 C26 128.7(6) . . ?
C28A C27 S3A 110.2(4) . . ?
C28A C27 C26 128.0(4) . . ?
C27 C28 H28 121.5 . . ?
C27 C28 C29 117.0(13) . . ?
C29 C28 H28 121.5 . . ?
C27 C28A H28A 121.9 . . ?
C27 C28A C29A 116.2(9) . . ?
C29A C28A H28A 121.9 . . ?
C28 C29 H29 127.0 . . ?
C30 C29 C28 106.1(17) . . ?
C30 C29 H29 127.0 . . ?
C28A C29A H29A 126.0 . . ?
C30A C29A C28A 108.0(11) . . ?
C30A C29A H29A 126.0 . . ?
S3 C30 H30 121.8 . . ?
C29 C30 S3 116.4(15) . . ?
C29 C30 H30 121.8 . . ?
S3A C30A H30A 122.6 . . ?
C29A C30A S3A 114.8(10) . . ?
C29A C30A H30A 122.6 . . ?

_olex2_submission_special_instructions 'No special instructions were received'

####################################################################### 
# 
# 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_final_a_CCDC8
_database_code_depnum_ccdc_archive 'CCDC 1544448'
_audit_update_record             
;
2017-04-17 deposited with the CCDC.
2017-08-23 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT415_final_a             
;
PROBLEM: Short Inter D-H..H-X       H1     ..  H8A     ..       2.08 Ang.  
RESPONSE: H8A is a water hydrogen atom which was found in the
difference map in a good hydrogen bond location. H8A is part of a
partially occupied lattice water molecule which is only present 15% of the
time.
;
# end Validation Reply Form


_audit_creation_date             2017-04-06
_audit_creation_method           
;
Olex2 1.2
(compiled Mar 28 2017 19:26:29 for OlexSys, GUI svn.r5335)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C60 H44 Dy2 N6 O14 S6, 0.3(H2 O)'
_chemical_formula_sum            'C60 H44.59 Dy2 N6 O14.30 S6'
_chemical_formula_weight         1595.69
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 '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'

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

_cell_length_a                   11.8744(6)
_cell_length_b                   25.2718(12)
_cell_length_c                   9.7179(5)
_cell_angle_alpha                90
_cell_angle_beta                 97.716(2)
_cell_angle_gamma                90
_cell_volume                     2889.8(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9094
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.17
_cell_measurement_theta_min      2.26
_shelx_estimated_absorpt_T_max   0.753
_shelx_estimated_absorpt_T_min   0.713
_exptl_absorpt_coefficient_mu    2.858
_exptl_absorpt_correction_T_max  0.8465
_exptl_absorpt_correction_T_min  0.7441
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.0699 before and 0.0516 after correction.
The Ratio of minimum to maximum transmission is 0.8790.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.834
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       rhombus
_exptl_crystal_F_000             1578
_exptl_crystal_size_max          0.127
_exptl_crystal_size_mid          0.117
_exptl_crystal_size_min          0.105
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0388
_diffrn_reflns_av_unetI/netI     0.0297
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            46480
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.176
_diffrn_reflns_theta_min         2.263
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6842
_reflns_number_total             7808
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.496
_refine_diff_density_min         -1.186
_refine_diff_density_rms         0.100
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     530
_refine_ls_number_reflns         7808
_refine_ls_number_restraints     1002
_refine_ls_R_factor_all          0.0326
_refine_ls_R_factor_gt           0.0244
_refine_ls_restrained_S_all      1.033
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0110P)²+3.4281P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0434
_refine_ls_wR_factor_ref         0.0451
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O7-H7B = O7-H7A
 0.86 with sigma of 0.02
 O8-H8B = O8-H8A
 0.86 with sigma of 0.02
 H7A-H7B
 1.35 with sigma of 0.02
 H8B-H8A
 1.35 with sigma of 0.02
 S1-C17 \\sim S1A-C17 \\sim S2A-C22 \\sim S2-C22 \\sim S3A-C27 \\sim S3-C27
 with sigma of 0.01
 S1-C20 \\sim S1A-C20A \\sim S2-C25 \\sim S2A-C25A \\sim S3A-C30A \\sim S3-C30
 with sigma of 0.01
 C20A-C19A \\sim C20-C19 \\sim C25-C24 \\sim C25A-C24A \\sim C30A-C29A \\sim
C30-C29
 with sigma of 0.01
 C18-C17 \\sim C18A-C17 \\sim C23A-C22 \\sim C23-C22 \\sim C28-C27 \\sim
C28A-C27
 with sigma of 0.01
 C19-C18 \\sim C19A-C18A \\sim C24-C23 \\sim C24A-C23A \\sim C29-C28 \\sim
C29A-C28A
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
S1 \\sim C17 \\sim C18 \\sim C19 \\sim C20 \\sim S1A \\sim C18A \\sim C19A
\\sim C20A \\sim S1 \\sim C17 \\sim C18 \\sim C17 \\sim S1A \\sim C17 \\sim
C18A \\sim C17 \\sim S1 \\sim C20 \\sim C19 \\sim C18 \\sim S1A \\sim C20A
\\sim C19A \\sim C18A \\sim C20 \\sim C19 \\sim C20A \\sim C19A: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
S2 \\sim C22 \\sim C23 \\sim C24 \\sim C25 \\sim S2A \\sim C23A \\sim C24A
\\sim C25A \\sim S2 \\sim C22 \\sim C23 \\sim C22 \\sim S2A \\sim C22 \\sim
C23A \\sim C22 \\sim S2 \\sim C25 \\sim C24 \\sim C23 \\sim S2A \\sim C25A
\\sim C24A \\sim C23A \\sim C25 \\sim C24 \\sim C25A \\sim C24A: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
S3 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim S3A \\sim C28A \\sim C29A
\\sim C30A \\sim S3 \\sim C27 \\sim C28 \\sim C27 \\sim S3A \\sim C27 \\sim
C28A \\sim C27 \\sim S3 \\sim C30 \\sim C29 \\sim C28 \\sim S3A \\sim C30A
\\sim C29A \\sim C28A \\sim C30 \\sim C29 \\sim C30A \\sim C29A: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(S1A)=Sof(C18A)=Sof(H18A)=Sof(C19A)=Sof(H19A)=Sof(C20A)=Sof(H20A)=1-FVAR(1)
 Sof(S1)=Sof(C18)=Sof(H18)=Sof(C19)=Sof(H19)=Sof(C20)=Sof(H20)=FVAR(1)
 Sof(S2A)=Sof(C23A)=Sof(H23A)=Sof(C24A)=Sof(H24A)=Sof(C25A)=Sof(H25A)=1-FVAR(2)
 Sof(S2)=Sof(C23)=Sof(H23)=Sof(C24)=Sof(H24)=Sof(C25)=Sof(H25)=FVAR(2)
 Sof(S3A)=Sof(C28A)=Sof(H28A)=Sof(C29A)=Sof(H29A)=Sof(C30A)=Sof(H30A)=1-FVAR(3)
 Sof(S3)=Sof(C28)=Sof(H28)=Sof(C29)=Sof(H29)=Sof(C30)=Sof(H30)=FVAR(3)
 Sof(O8)=Sof(H8A)=Sof(H8B)=FVAR(4)
6.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C12(H12), C13(H13),
 C14(H14), C15(H15), C18(H18), C19(H19), C20(H20), C23(H23), C24(H24), C25(H25),
  C28(H28), C29(H29), C30(H30), C18A(H18A), C19A(H19A), C20A(H20A), C23A(H23A),
 C24A(H24A), C25A(H25A), C28A(H28A), C29A(H29A), C30A(H30A)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.48415(2) 0.40205(2) 0.40193(2) 0.00797(3) Uani 1 1 d . U . . .
S1 S 0.75722(14) 0.44231(7) -0.00033(15) 0.0147(3) Uani 0.679(3) 1 d D U P A 1
S2 S 0.12378(18) 0.56168(8) 0.4296(3) 0.0128(4) Uani 0.483(3) 1 d D U P B 1
S3 S 0.11633(17) 0.29455(8) 0.34164(18) 0.0138(4) Uani 0.592(3) 1 d D U P C 1
O1 O 0.58789(14) 0.44400(6) 0.21285(17) 0.0192(4) Uani 1 1 d . U . . .
O2 O 0.64451(13) 0.36671(6) 0.30440(16) 0.0137(3) Uani 1 1 d . U . . .
O3 O 0.36539(13) 0.54756(6) 0.49369(16) 0.0136(3) Uani 1 1 d . U . . .
O4 O 0.38630(13) 0.47974(6) 0.35230(16) 0.0138(3) Uani 1 1 d . U . . .
O5 O 0.29897(13) 0.37111(6) 0.43199(16) 0.0139(3) Uani 1 1 d . U . . .
O6 O 0.22857(13) 0.39932(6) 0.62216(15) 0.0158(3) Uani 1 1 d . U . . .
O7 O 0.44343(14) 0.43063(6) 0.63106(16) 0.0147(3) Uani 1 1 d D U . . .
H7A H 0.3762(15) 0.4258(10) 0.639(3) 0.022 Uiso 1 1 d DR . . . .
H7B H 0.464(2) 0.4606(8) 0.660(3) 0.022 Uiso 1 1 d DR . . . .
O8 O 0.4949(11) 0.5315(5) 0.1028(12) 0.025(4) Uani 0.148(6) 1 d D U P D 1
H8A H 0.531(15) 0.502(4) 0.106(17) 0.037 Uiso 0.148(6) 1 d DR . P D 1
H8B H 0.471(16) 0.535(7) 0.016(5) 0.037 Uiso 0.148(6) 1 d DR . P D 1
N1 N 0.37899(17) 0.38283(8) 0.16214(19) 0.0161(4) Uani 1 1 d . U . . .
N2 N 0.45015(15) 0.30442(7) 0.34048(18) 0.0099(4) Uani 1 1 d . U . . .
N3 N 0.58377(16) 0.33463(7) 0.57270(18) 0.0106(4) Uani 1 1 d . U . . .
C1 C 0.3484(2) 0.42232(10) 0.0736(2) 0.0245(6) Uani 1 1 d . U . . .
H1 H 0.3852 0.4556 0.0896 0.029 Uiso 1 1 calc R . . . .
C2 C 0.2654(3) 0.41704(11) -0.0407(3) 0.0299(6) Uani 1 1 d . U . . .
H2 H 0.2480 0.4455 -0.1039 0.036 Uiso 1 1 calc R . . . .
C3 C 0.2092(2) 0.36968(12) -0.0599(2) 0.0269(6) Uani 1 1 d . U . . .
H3 H 0.1496 0.3654 -0.1347 0.032 Uiso 1 1 calc R . . . .
C4 C 0.2397(2) 0.32818(11) 0.0304(2) 0.0220(5) Uani 1 1 d . U . . .
H4 H 0.2009 0.2953 0.0190 0.026 Uiso 1 1 calc R . . . .
C5 C 0.32808(19) 0.33535(9) 0.1382(2) 0.0145(5) Uani 1 1 d . U . . .
C6 C 0.37608(18) 0.29129(9) 0.2285(2) 0.0129(4) Uani 1 1 d . U . . .
C7 C 0.3501(2) 0.23859(9) 0.1943(2) 0.0167(5) Uani 1 1 d . U . . .
H7 H 0.2984 0.2302 0.1140 0.020 Uiso 1 1 calc R . . . .
C8 C 0.4001(2) 0.19896(9) 0.2780(2) 0.0188(5) Uani 1 1 d . U . . .
H8 H 0.3832 0.1629 0.2568 0.023 Uiso 1 1 calc R . . . .
C9 C 0.4749(2) 0.21238(9) 0.3931(2) 0.0155(4) Uani 1 1 d . U . . .
H9 H 0.5098 0.1856 0.4529 0.019 Uiso 1 1 calc R . . . .
C10 C 0.49918(18) 0.26560(8) 0.4215(2) 0.0105(4) Uani 1 1 d . U . . .
C11 C 0.57905(19) 0.28225(8) 0.5444(2) 0.0111(4) Uani 1 1 d . U . . .
C12 C 0.6436(2) 0.24581(9) 0.6288(2) 0.0152(5) Uani 1 1 d . U . . .
H12 H 0.6397 0.2092 0.6064 0.018 Uiso 1 1 calc R . . . .
C13 C 0.7133(2) 0.26310(9) 0.7452(2) 0.0166(5) Uani 1 1 d . U . . .
H13 H 0.7565 0.2386 0.8046 0.020 Uiso 1 1 calc R . . . .
C14 C 0.7191(2) 0.31659(10) 0.7738(2) 0.0175(5) Uani 1 1 d . U . . .
H14 H 0.7674 0.3297 0.8523 0.021 Uiso 1 1 calc R . . . .
C15 C 0.65302(19) 0.35065(9) 0.6854(2) 0.0139(4) Uani 1 1 d . U . . .
H15 H 0.6569 0.3874 0.7057 0.017 Uiso 1 1 calc R . . . .
C16 C 0.65483(18) 0.40526(9) 0.2242(2) 0.0134(4) Uani 1 1 d . U . . .
C17 C 0.75094(18) 0.40312(8) 0.1400(2) 0.0117(4) Uani 1 1 d D U . . .
C18 C 0.8458(7) 0.3708(3) 0.1628(8) 0.0122(13) Uani 0.679(3) 1 d D U P A 1
H18 H 0.8568 0.3461 0.2371 0.015 Uiso 0.679(3) 1 calc R . P A 1
C19 C 0.9256(8) 0.3773(3) 0.0675(8) 0.0128(10) Uani 0.679(3) 1 d D U P A 1
H19 H 0.9946 0.3582 0.0688 0.015 Uiso 0.679(3) 1 calc R . P A 1
C20 C 0.8867(6) 0.4153(3) -0.0258(10) 0.0134(11) Uani 0.679(3) 1 d D U P A 1
H20 H 0.9272 0.4262 -0.0988 0.016 Uiso 0.679(3) 1 calc R . P A 1
C21 C 0.32621(18) 0.51279(8) 0.4079(2) 0.0097(4) Uani 1 1 d . U . . .
C22 C 0.20190(18) 0.51196(8) 0.3700(2) 0.0103(4) Uani 1 1 d D U . . .
C23 C 0.1354(7) 0.4762(3) 0.2913(9) 0.0158(16) Uani 0.483(3) 1 d D U P B 1
H23 H 0.1659 0.4461 0.2509 0.019 Uiso 0.483(3) 1 calc R . P B 1
C24 C 0.0179(9) 0.4874(6) 0.274(2) 0.0147(15) Uani 0.483(3) 1 d D U P B 1
H24 H -0.0401 0.4673 0.2214 0.018 Uiso 0.483(3) 1 calc R . P B 1
C25 C 0.0026(10) 0.5318(7) 0.347(2) 0.0133(16) Uani 0.483(3) 1 d D U P B 1
H25 H -0.0709 0.5458 0.3526 0.016 Uiso 0.483(3) 1 calc R . P B 1
C26 C 0.22532(18) 0.37182(8) 0.5149(2) 0.0106(4) Uani 1 1 d . U . . .
C27 C 0.12789(18) 0.33440(9) 0.4830(2) 0.0120(4) Uani 1 1 d D U . . .
C28 C 0.0420(7) 0.3242(4) 0.5617(8) 0.0206(15) Uani 0.592(3) 1 d D U P C 1
H28 H 0.0351 0.3430 0.6448 0.025 Uiso 0.592(3) 1 calc R . P C 1
C29 C -0.0350(9) 0.2840(3) 0.5108(10) 0.0173(13) Uani 0.592(3) 1 d D U P C 1
H29 H -0.0992 0.2727 0.5516 0.021 Uiso 0.592(3) 1 calc R . P C 1
C30 C -0.0012(8) 0.2643(5) 0.3934(11) 0.0144(14) Uani 0.592(3) 1 d D U P C 1
H30 H -0.0394 0.2358 0.3432 0.017 Uiso 0.592(3) 1 calc R . P C 1
S1A S 0.8582(4) 0.3622(2) 0.1887(5) 0.0123(7) Uani 0.321(3) 1 d D U P A 2
C18A C 0.7664(13) 0.4330(6) 0.0244(13) 0.016(2) Uani 0.321(3) 1 d D U P A 2
H18A H 0.7123 0.4584 -0.0147 0.019 Uiso 0.321(3) 1 calc R . P A 2
C19A C 0.8686(13) 0.4231(8) -0.031(2) 0.0147(19) Uani 0.321(3) 1 d D U P A 2
H19A H 0.8934 0.4392 -0.1104 0.018 Uiso 0.321(3) 1 calc R . P A 2
C20A C 0.9235(17) 0.3858(7) 0.0520(18) 0.013(2) Uani 0.321(3) 1 d D U P A 2
H20A H 0.9957 0.3729 0.0360 0.016 Uiso 0.321(3) 1 calc R . P A 2
S2A S 0.13322(17) 0.46458(8) 0.2615(2) 0.0141(4) Uani 0.517(3) 1 d D U P B 2
C23A C 0.1237(7) 0.5462(3) 0.4140(10) 0.0149(15) Uani 0.517(3) 1 d D U P B 2
H23A H 0.1459 0.5738 0.4782 0.018 Uiso 0.517(3) 1 calc R . P B 2
C24A C 0.0088(10) 0.5380(6) 0.359(2) 0.0149(15) Uani 0.517(3) 1 d D U P B 2
H24A H -0.0539 0.5594 0.3746 0.018 Uiso 0.517(3) 1 calc R . P B 2
C25A C 0.0046(8) 0.4940(6) 0.2785(19) 0.0129(15) Uani 0.517(3) 1 d D U P B 2
H25A H -0.0654 0.4801 0.2340 0.015 Uiso 0.517(3) 1 calc R . P B 2
S3A S 0.0352(3) 0.32436(17) 0.5972(3) 0.0214(6) Uani 0.408(3) 1 d D U P C 2
C28A C 0.1074(11) 0.2989(5) 0.3741(10) 0.0166(19) Uani 0.408(3) 1 d D U P C 2
H28A H 0.1544 0.2975 0.3025 0.020 Uiso 0.408(3) 1 calc R . P C 2
C29A C 0.0131(12) 0.2649(7) 0.3746(16) 0.0151(16) Uani 0.408(3) 1 d D U P C 2
H29A H -0.0150 0.2401 0.3047 0.018 Uiso 0.408(3) 1 calc R . P C 2
C30A C -0.0293(13) 0.2745(5) 0.4944(15) 0.0169(18) Uani 0.408(3) 1 d D U P C 2
H30A H -0.0913 0.2548 0.5205 0.020 Uiso 0.408(3) 1 calc R . P C 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 O1 2.5740(16) . ?
Dy1 O2 2.4096(15) . ?
Dy1 O3 2.3144(15) 3_666 ?
Dy1 O4 2.2992(15) . ?
Dy1 O5 2.3883(15) . ?
Dy1 O7 2.4500(15) . ?
Dy1 N1 2.5385(19) . ?
Dy1 N2 2.5578(17) . ?
Dy1 N3 2.5553(18) . ?
Dy1 C16 2.835(2) . ?
S1 C17 1.695(2) . ?
S1 C20 1.730(5) . ?
S2 C22 1.708(3) . ?
S2 C25 1.724(7) . ?
S3 C27 1.694(3) . ?
S3 C30 1.725(6) . ?
O1 C16 1.257(3) . ?
O2 C16 1.264(3) . ?
O3 Dy1 2.3143(15) 3_666 ?
O3 C21 1.257(3) . ?
O4 C21 1.266(3) . ?
O5 C26 1.266(3) . ?
O6 C26 1.249(3) . ?
O7 H7A 0.822(16) . ?
O7 H7B 0.835(16) . ?
O8 H8A 0.86(2) . ?
O8 H8B 0.86(2) . ?
N1 C1 1.336(3) . ?
N1 C5 1.349(3) . ?
N2 C6 1.346(3) . ?
N2 C10 1.341(3) . ?
N3 C11 1.352(3) . ?
N3 C15 1.341(3) . ?
C1 H1 0.9500 . ?
C1 C2 1.389(4) . ?
C2 H2 0.9500 . ?
C2 C3 1.371(4) . ?
C3 H3 0.9500 . ?
C3 C4 1.384(4) . ?
C4 H4 0.9500 . ?
C4 C5 1.392(3) . ?
C5 C6 1.483(3) . ?
C6 C7 1.397(3) . ?
C7 H7 0.9500 . ?
C7 C8 1.374(4) . ?
C8 H8 0.9500 . ?
C8 C9 1.374(3) . ?
C9 H9 0.9500 . ?
C9 C10 1.395(3) . ?
C10 C11 1.483(3) . ?
C11 C12 1.393(3) . ?
C12 H12 0.9500 . ?
C12 C13 1.379(3) . ?
C13 H13 0.9500 . ?
C13 C14 1.380(3) . ?
C14 H14 0.9500 . ?
C14 C15 1.383(3) . ?
C15 H15 0.9500 . ?
C16 C17 1.492(3) . ?
C17 C18 1.385(6) . ?
C17 S1A 1.659(4) . ?
C17 C18A 1.386(7) . ?
C18 H18 0.9500 . ?
C18 C19 1.420(8) . ?
C19 H19 0.9500 . ?
C19 C20 1.360(5) . ?
C20 H20 0.9500 . ?
C21 C22 1.473(3) . ?
C22 C23 1.365(6) . ?
C22 S2A 1.726(3) . ?
C22 C23A 1.378(6) . ?
C23 H23 0.9500 . ?
C23 C24 1.412(9) . ?
C24 H24 0.9500 . ?
C24 C25 1.351(6) . ?
C25 H25 0.9500 . ?
C26 C27 1.494(3) . ?
C27 C28 1.379(6) . ?
C27 S3A 1.684(3) . ?
C27 C28A 1.384(7) . ?
C28 H28 0.9500 . ?
C28 C29 1.412(9) . ?
C29 H29 0.9500 . ?
C29 C30 1.353(6) . ?
C30 H30 0.9500 . ?
S1A C20A 1.731(8) . ?
C18A H18A 0.9500 . ?
C18A C19A 1.417(10) . ?
C19A H19A 0.9500 . ?
C19A C20A 1.351(7) . ?
C20A H20A 0.9500 . ?
S2A C25A 1.727(7) . ?
C23A H23A 0.9500 . ?
C23A C24A 1.413(9) . ?
C24A H24A 0.9500 . ?
C24A C25A 1.354(6) . ?
C25A H25A 0.9500 . ?
S3A C30A 1.723(8) . ?
C28A H28A 0.9500 . ?
C28A C29A 1.412(10) . ?
C29A H29A 0.9500 . ?
C29A C30A 1.351(7) . ?
C30A H30A 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 C16 26.30(6) . . ?
O2 Dy1 O1 52.60(5) . . ?
O2 Dy1 O7 136.85(5) . . ?
O2 Dy1 N1 83.42(6) . . ?
O2 Dy1 N2 70.06(5) . . ?
O2 Dy1 N3 71.76(5) . . ?
O2 Dy1 C16 26.32(6) . . ?
O3 Dy1 O1 70.79(5) 3_666 . ?
O3 Dy1 O2 76.82(5) 3_666 . ?
O3 Dy1 O5 142.73(5) 3_666 . ?
O3 Dy1 O7 71.00(5) 3_666 . ?
O3 Dy1 N1 139.76(6) 3_666 . ?
O3 Dy1 N2 136.18(6) 3_666 . ?
O3 Dy1 N3 79.60(6) 3_666 . ?
O3 Dy1 C16 71.24(6) 3_666 . ?
O4 Dy1 O1 77.02(5) . . ?
O4 Dy1 O2 129.62(5) . . ?
O4 Dy1 O3 87.75(5) . 3_666 ?
O4 Dy1 O5 81.81(5) . . ?
O4 Dy1 O7 77.47(5) . . ?
O4 Dy1 N1 78.37(6) . . ?
O4 Dy1 N2 135.66(6) . . ?
O4 Dy1 N3 151.94(5) . . ?
O4 Dy1 C16 103.31(6) . . ?
O5 Dy1 O1 139.36(5) . . ?
O5 Dy1 O2 135.72(5) . . ?
O5 Dy1 O7 71.82(5) . . ?
O5 Dy1 N1 72.67(6) . . ?
O5 Dy1 N2 66.03(5) . . ?
O5 Dy1 N3 93.20(6) . . ?
O5 Dy1 C16 146.00(6) . . ?
O7 Dy1 O1 134.36(5) . . ?
O7 Dy1 N1 139.28(6) . . ?
O7 Dy1 N2 116.89(6) . . ?
O7 Dy1 N3 74.75(6) . . ?
O7 Dy1 C16 142.16(6) . . ?
N1 Dy1 O1 69.34(6) . . ?
N1 Dy1 N2 63.79(6) . . ?
N1 Dy1 N3 126.61(6) . . ?
N1 Dy1 C16 75.52(6) . . ?
N2 Dy1 O1 107.84(5) . . ?
N2 Dy1 C16 89.35(6) . . ?
N3 Dy1 O1 120.94(5) . . ?
N3 Dy1 N2 63.46(6) . . ?
N3 Dy1 C16 96.22(6) . . ?
C17 S1 C20 91.2(3) . . ?
C22 S2 C25 88.7(5) . . ?
C27 S3 C30 90.4(4) . . ?
C16 O1 Dy1 88.53(13) . . ?
C16 O2 Dy1 95.98(13) . . ?
C21 O3 Dy1 150.54(14) . 3_666 ?
C21 O4 Dy1 140.53(14) . . ?
C26 O5 Dy1 143.04(14) . . ?
Dy1 O7 H7A 110.7(19) . . ?
Dy1 O7 H7B 119.3(18) . . ?
H7A O7 H7B 111(2) . . ?
H8A O8 H8B 103(3) . . ?
C1 N1 Dy1 120.39(16) . . ?
C1 N1 C5 118.5(2) . . ?
C5 N1 Dy1 118.82(15) . . ?
C6 N2 Dy1 119.48(14) . . ?
C10 N2 Dy1 121.75(14) . . ?
C10 N2 C6 118.65(19) . . ?
C11 N3 Dy1 121.19(14) . . ?
C15 N3 Dy1 120.58(14) . . ?
C15 N3 C11 117.78(19) . . ?
N1 C1 H1 118.5 . . ?
N1 C1 C2 123.1(3) . . ?
C2 C1 H1 118.5 . . ?
C1 C2 H2 120.9 . . ?
C3 C2 C1 118.2(3) . . ?
C3 C2 H2 120.9 . . ?
C2 C3 H3 120.2 . . ?
C2 C3 C4 119.6(2) . . ?
C4 C3 H3 120.2 . . ?
C3 C4 H4 120.5 . . ?
C3 C4 C5 119.0(2) . . ?
C5 C4 H4 120.5 . . ?
N1 C5 C4 121.4(2) . . ?
N1 C5 C6 116.0(2) . . ?
C4 C5 C6 122.6(2) . . ?
N2 C6 C5 116.79(19) . . ?
N2 C6 C7 121.8(2) . . ?
C7 C6 C5 121.3(2) . . ?
C6 C7 H7 120.3 . . ?
C8 C7 C6 119.4(2) . . ?
C8 C7 H7 120.3 . . ?
C7 C8 H8 120.6 . . ?
C9 C8 C7 118.8(2) . . ?
C9 C8 H8 120.6 . . ?
C8 C9 H9 120.2 . . ?
C8 C9 C10 119.5(2) . . ?
C10 C9 H9 120.2 . . ?
N2 C10 C9 121.8(2) . . ?
N2 C10 C11 116.46(18) . . ?
C9 C10 C11 121.7(2) . . ?
N3 C11 C10 116.51(19) . . ?
N3 C11 C12 121.5(2) . . ?
C12 C11 C10 121.9(2) . . ?
C11 C12 H12 120.1 . . ?
C13 C12 C11 119.7(2) . . ?
C13 C12 H12 120.1 . . ?
C12 C13 H13 120.5 . . ?
C12 C13 C14 119.0(2) . . ?
C14 C13 H13 120.5 . . ?
C13 C14 H14 120.8 . . ?
C13 C14 C15 118.4(2) . . ?
C15 C14 H14 120.8 . . ?
N3 C15 C14 123.6(2) . . ?
N3 C15 H15 118.2 . . ?
C14 C15 H15 118.2 . . ?
O1 C16 Dy1 65.17(12) . . ?
O1 C16 O2 122.8(2) . . ?
O1 C16 C17 120.1(2) . . ?
O2 C16 Dy1 57.70(11) . . ?
O2 C16 C17 117.1(2) . . ?
C17 C16 Dy1 174.39(16) . . ?
C16 C17 S1 122.66(17) . . ?
C16 C17 S1A 118.7(2) . . ?
C18 C17 S1 110.5(3) . . ?
C18 C17 C16 126.8(3) . . ?
C18A C17 C16 128.2(6) . . ?
C18A C17 S1A 113.0(6) . . ?
C17 C18 H18 122.3 . . ?
C17 C18 C19 115.3(6) . . ?
C19 C18 H18 122.3 . . ?
C18 C19 H19 125.7 . . ?
C20 C19 C18 108.6(8) . . ?
C20 C19 H19 125.7 . . ?
S1 C20 H20 122.8 . . ?
C19 C20 S1 114.3(7) . . ?
C19 C20 H20 122.8 . . ?
O3 C21 O4 124.4(2) . . ?
O3 C21 C22 116.42(18) . . ?
O4 C21 C22 119.19(19) . . ?
C21 C22 S2 118.46(16) . . ?
C21 C22 S2A 122.54(16) . . ?
C23 C22 S2 112.2(4) . . ?
C23 C22 C21 129.4(4) . . ?
C23A C22 C21 127.4(4) . . ?
C23A C22 S2A 110.0(4) . . ?
C22 C23 H23 122.6 . . ?
C22 C23 C24 114.9(9) . . ?
C24 C23 H23 122.6 . . ?
C23 C24 H24 126.1 . . ?
C25 C24 C23 107.8(14) . . ?
C25 C24 H24 126.1 . . ?
S2 C25 H25 121.8 . . ?
C24 C25 S2 116.4(13) . . ?
C24 C25 H25 121.8 . . ?
O5 C26 C27 116.15(19) . . ?
O6 C26 O5 126.3(2) . . ?
O6 C26 C27 117.49(19) . . ?
C26 C27 S3 121.37(16) . . ?
C26 C27 S3A 121.02(18) . . ?
C28 C27 S3 110.7(4) . . ?
C28 C27 C26 127.8(4) . . ?
C28A C27 C26 128.4(5) . . ?
C28A C27 S3A 110.0(5) . . ?
C27 C28 H28 122.2 . . ?
C27 C28 C29 115.6(7) . . ?
C29 C28 H28 122.2 . . ?
C28 C29 H29 126.0 . . ?
C30 C29 C28 108.0(9) . . ?
C30 C29 H29 126.0 . . ?
S3 C30 H30 122.4 . . ?
C29 C30 S3 115.2(8) . . ?
C29 C30 H30 122.4 . . ?
C17 S1A C20A 88.4(7) . . ?
C17 C18A H18A 122.4 . . ?
C17 C18A C19A 115.2(13) . . ?
C19A C18A H18A 122.4 . . ?
C18A C19A H19A 127.4 . . ?
C20A C19A C18A 105.3(17) . . ?
C20A C19A H19A 127.4 . . ?
S1A C20A H20A 121.0 . . ?
C19A C20A S1A 118.0(15) . . ?
C19A C20A H20A 121.0 . . ?
C22 S2A C25A 89.7(5) . . ?
C22 C23A H23A 121.8 . . ?
C22 C23A C24A 116.5(9) . . ?
C24A C23A H23A 121.8 . . ?
C23A C24A H24A 126.3 . . ?
C25A C24A C23A 107.4(13) . . ?
C25A C24A H24A 126.3 . . ?
S2A C25A H25A 121.9 . . ?
C24A C25A S2A 116.3(12) . . ?
C24A C25A H25A 121.9 . . ?
C27 S3A C30A 90.4(6) . . ?
C27 C28A H28A 121.6 . . ?
C27 C28A C29A 116.8(10) . . ?
C29A C28A H28A 121.6 . . ?
C28A C29A H29A 126.8 . . ?
C30A C29A C28A 106.3(14) . . ?
C30A C29A H29A 126.8 . . ?
S3A C30A H30A 121.9 . . ?
C29A C30A S3A 116.3(13) . . ?
C29A C30A H30A 121.9 . . ?

_olex2_submission_original_sample_id RJB392
_olex2_submission_special_instructions 'No special instructions were received'

####################################################################### 
# 
# 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_final_a_CCDC9
_database_code_depnum_ccdc_archive 'CCDC 1544445'
_audit_update_record             
;
2017-04-17 deposited with the CCDC.
2017-08-23 downloaded from the CCDC.
;
_audit_creation_date             2017-04-06
_audit_creation_method           
;
Olex2 1.2
(compiled Mar 28 2017 19:26:29 for OlexSys, GUI svn.r5335)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        RJB389
_chemical_formula_moiety         'C60 H44 Eu2 N6 O14 S6, 0.43(H2 O)'
_chemical_formula_sum            'C60 H44.86 Eu2 N6 O14.43 S6'
_chemical_formula_weight         1577.04
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Eu Eu -0.1578 3.6682 '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'

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

_cell_length_a                   11.9277(5)
_cell_length_b                   25.4424(10)
_cell_length_c                   9.7246(5)
_cell_angle_alpha                90
_cell_angle_beta                 97.836(2)
_cell_angle_gamma                90
_cell_volume                     2923.6(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9845
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      29.57
_cell_measurement_theta_min      2.26
_shelx_estimated_absorpt_T_max   0.590
_shelx_estimated_absorpt_T_min   0.353
_exptl_absorpt_coefficient_mu    2.415
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5132
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.0634 before and 0.0457 after correction.
The Ratio of minimum to maximum transmission is 0.5132.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.791
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       rhombohedral
_exptl_crystal_F_000             1569
_exptl_crystal_size_max          0.545
_exptl_crystal_size_mid          0.295
_exptl_crystal_size_min          0.244
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0254
_diffrn_reflns_av_unetI/netI     0.0239
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            26666
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.101
_diffrn_reflns_theta_min         2.261
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5847
_reflns_number_total             6437
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.399
_refine_diff_density_min         -0.937
_refine_diff_density_rms         0.078
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     532
_refine_ls_number_reflns         6437
_refine_ls_number_restraints     1002
_refine_ls_R_factor_all          0.0260
_refine_ls_R_factor_gt           0.0213
_refine_ls_restrained_S_all      1.047
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0128P)²+3.0236P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0428
_refine_ls_wR_factor_ref         0.0439
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O7-H7A = O7-H7B
 0.86 with sigma of 0.03
 O8-H8A = O8-H8B
 0.86 with sigma of 0.02
 H7B-H7A
 1.35 with sigma of 0.02
 H8A-H8B
 1.35 with sigma of 0.02
 S1A-C17 \\sim S1-C17 \\sim S2A-C22 \\sim S2-C22 \\sim S3-C27 \\sim S3A-C27
 with sigma of 0.01
 S1A-C20A \\sim S1-C20 \\sim S2A-C25A \\sim S2-C25 \\sim S3A-C30A \\sim S3-C30
 with sigma of 0.01
 C20A-C19A \\sim C20-C19 \\sim C25-C24 \\sim C25A-C24A \\sim C30A-C29A \\sim
C30-C29
 with sigma of 0.01
 C23A-C22 \\sim C23-C22 \\sim C18-C17 \\sim C18A-C17 \\sim C28-C27 \\sim
C28A-C27
 with sigma of 0.01
 C24A-C23A \\sim C24-C23 \\sim C19-C18 \\sim C19A-C18A \\sim C29A-C28A \\sim
C29-C28
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
S1 \\sim S1 \\sim S1 \\sim S1A \\sim S1A \\sim S1A \\sim C17 \\sim C17 \\sim
C17 \\sim C17 \\sim C17 \\sim C18 \\sim C18 \\sim C18 \\sim C18A \\sim C18A
\\sim C18A \\sim C19 \\sim C19 \\sim C19 \\sim C19A \\sim C19A \\sim C19A \\sim
C20 \\sim C20 \\sim C20 \\sim C20A \\sim C20A \\sim C20A: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02
S2 \\sim S2 \\sim S2 \\sim S2A \\sim S2A \\sim S2A \\sim C22 \\sim C22 \\sim
C22 \\sim C22 \\sim C22 \\sim C23 \\sim C23 \\sim C23 \\sim C23A \\sim C23A
\\sim C23A \\sim C24 \\sim C24 \\sim C24 \\sim C24A \\sim C24A \\sim C24A \\sim
C25 \\sim C25 \\sim C25 \\sim C25A \\sim C25A \\sim C25A: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02
S3 \\sim S3 \\sim S3 \\sim S3A \\sim S3A \\sim S3A \\sim C27 \\sim C27 \\sim
C27 \\sim C27 \\sim C27 \\sim C28 \\sim C28 \\sim C28 \\sim C28A \\sim C28A
\\sim C28A \\sim C29 \\sim C29 \\sim C29 \\sim C29A \\sim C29A \\sim C29A \\sim
C30 \\sim C30 \\sim C30 \\sim C30A \\sim C30A \\sim C30A: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(S1A)=Sof(C18A)=Sof(H18A)=Sof(C19A)=Sof(H19A)=Sof(C20A)=Sof(H20A)=1-FVAR(1)
 Sof(S1)=Sof(C18)=Sof(H18)=Sof(C19)=Sof(H19)=Sof(C20)=Sof(H20)=FVAR(1)
 Sof(S2A)=Sof(C23A)=Sof(H23A)=Sof(C24A)=Sof(H24A)=Sof(C25A)=Sof(H25A)=1-FVAR(2)
 Sof(S2)=Sof(C23)=Sof(H23)=Sof(C24)=Sof(H24)=Sof(C25)=Sof(H25)=FVAR(2)
 Sof(S3A)=Sof(C28A)=Sof(H28A)=Sof(C29A)=Sof(H29A)=Sof(C30A)=Sof(H30A)=1-FVAR(3)
 Sof(S3)=Sof(C28)=Sof(H28)=Sof(C29)=Sof(H29)=Sof(C30)=Sof(H30)=FVAR(3)
 Sof(O8)=Sof(H8A)=Sof(H8B)=FVAR(4)
6.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C12(H12), C13(H13),
 C14(H14), C15(H15), C18(H18), C18A(H18A), C19(H19), C19A(H19A), C20(H20),
 C20A(H20A), C23(H23), C23A(H23A), C24(H24), C24A(H24A), C25(H25), C25A(H25A),
 C28(H28), C28A(H28A), C29(H29), C29A(H29A), C30(H30), C30A(H30A)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Eu1 Eu 0.51641(2) 0.40186(2) 0.59814(2) 0.00977(4) Uani 1 1 d . U . . .
S1 S 0.24359(14) 0.44279(7) 1.00080(16) 0.0174(3) Uani 0.697(3) 1 d D U P A 1
S1A S 0.1425(4) 0.3626(2) 0.8136(5) 0.0145(8) Uani 0.303(3) 1 d D U P A 2
S2 S 0.13105(17) 0.53514(8) 0.2622(2) 0.0164(4) Uani 0.525(3) 1 d D U P B 1
S2A S 0.12333(18) 0.43828(9) 0.4290(3) 0.0157(5) Uani 0.475(3) 1 d D U P B 2
S3 S 0.88526(18) 0.29491(9) 0.6587(2) 0.0167(4) Uani 0.592(3) 1 d D U P C 1
S3A S 0.9659(3) 0.32411(17) 0.4033(3) 0.0239(7) Uani 0.408(3) 1 d D U P C 2
O1 O 0.41369(13) 0.44243(6) 0.79020(18) 0.0229(4) Uani 1 1 d . U . . .
O2 O 0.35376(13) 0.36640(6) 0.69696(16) 0.0162(3) Uani 1 1 d . U . . .
O3 O 0.38311(12) 0.51998(6) 0.34966(16) 0.0161(3) Uani 1 1 d . U . . .
O4 O 0.36450(12) 0.45251(6) 0.49105(17) 0.0169(3) Uani 1 1 d . U . . .
O5 O 0.70318(12) 0.37059(6) 0.56744(16) 0.0160(3) Uani 1 1 d . U . . .
O6 O 0.77276(13) 0.39871(6) 0.37769(16) 0.0179(3) Uani 1 1 d . U . . .
O7 O 0.55806(14) 0.43040(7) 0.36606(17) 0.0179(3) Uani 1 1 d D U . . .
H7A H 0.623(2) 0.4235(12) 0.361(3) 0.046(10) Uiso 1 1 d D . . . .
H7B H 0.535(3) 0.4583(11) 0.333(4) 0.077(14) Uiso 1 1 d D . . . .
O8 O 0.5035(8) 0.5313(4) 0.8981(9) 0.035(3) Uani 0.215(6) 1 d D U P . .
H8A H 0.472(12) 0.501(3) 0.878(13) 0.053 Uiso 0.215(6) 1 d DR . P . .
H8B H 0.529(12) 0.528(5) 0.985(4) 0.053 Uiso 0.215(6) 1 d DR . P . .
N1 N 0.62375(16) 0.38063(8) 0.8394(2) 0.0186(4) Uani 1 1 d . U . . .
N2 N 0.55058(14) 0.30315(7) 0.65920(19) 0.0118(4) Uani 1 1 d . U . . .
N3 N 0.41565(15) 0.33348(7) 0.42669(19) 0.0125(4) Uani 1 1 d . U . . .
C1 C 0.6568(2) 0.41978(11) 0.9281(3) 0.0294(6) Uani 1 1 d . U . . .
H1 H 0.6209 0.4530 0.9131 0.035 Uiso 1 1 calc R . . . .
C2 C 0.7405(2) 0.41413(11) 1.0402(3) 0.0345(7) Uani 1 1 d . U . . .
H2 H 0.7598 0.4424 1.1028 0.041 Uiso 1 1 calc R . . . .
C3 C 0.7951(2) 0.36664(12) 1.0589(3) 0.0310(6) Uani 1 1 d . U . . .
H3 H 0.8549 0.3620 1.1330 0.037 Uiso 1 1 calc R . . . .
C4 C 0.7623(2) 0.32562(11) 0.9690(3) 0.0255(6) Uani 1 1 d . U . . .
H4 H 0.7998 0.2926 0.9799 0.031 Uiso 1 1 calc R . . . .
C5 C 0.67324(18) 0.33340(9) 0.8621(2) 0.0173(5) Uani 1 1 d . U . . .
C6 C 0.62437(17) 0.28985(9) 0.7712(2) 0.0148(4) Uani 1 1 d . U . . .
C7 C 0.65002(19) 0.23749(9) 0.8045(3) 0.0201(5) Uani 1 1 d . U . . .
H7 H 0.7018 0.2290 0.8845 0.024 Uiso 1 1 calc R . . . .
C8 C 0.5996(2) 0.19819(9) 0.7206(3) 0.0216(5) Uani 1 1 d . U . . .
H8 H 0.6162 0.1623 0.7416 0.026 Uiso 1 1 calc R . . . .
C9 C 0.52471(19) 0.21177(9) 0.6054(2) 0.0175(5) Uani 1 1 d . U . . .
H9 H 0.4894 0.1853 0.5456 0.021 Uiso 1 1 calc R . . . .
C10 C 0.50118(17) 0.26476(8) 0.5773(2) 0.0131(4) Uani 1 1 d . U . . .
C11 C 0.42084(18) 0.28142(8) 0.4546(2) 0.0139(4) Uani 1 1 d . U . . .
C12 C 0.35705(19) 0.24529(9) 0.3702(2) 0.0170(5) Uani 1 1 d . U . . .
H12 H 0.3617 0.2089 0.3922 0.020 Uiso 1 1 calc R . . . .
C13 C 0.28684(19) 0.26236(9) 0.2543(3) 0.0195(5) Uani 1 1 d . U . . .
H13 H 0.2437 0.2379 0.1950 0.023 Uiso 1 1 calc R . . . .
C14 C 0.28028(19) 0.31550(9) 0.2259(3) 0.0201(5) Uani 1 1 d . U . . .
H14 H 0.2319 0.3285 0.1476 0.024 Uiso 1 1 calc R . . . .
C15 C 0.34591(18) 0.34945(9) 0.3144(2) 0.0167(5) Uani 1 1 d . U . . .
H15 H 0.3414 0.3860 0.2945 0.020 Uiso 1 1 calc R . . . .
C16 C 0.34516(18) 0.40459(9) 0.7779(2) 0.0152(4) Uani 1 1 d . U . . .
C17 C 0.24973(17) 0.40325(8) 0.8615(2) 0.0137(4) Uani 1 1 d D U . . .
C18 C 0.1554(6) 0.3716(3) 0.8387(9) 0.0142(14) Uani 0.697(3) 1 d D U P A 1
H18 H 0.1442 0.3469 0.7647 0.017 Uiso 0.697(3) 1 calc R . P A 1
C18A C 0.2363(14) 0.4333(6) 0.9765(14) 0.017(2) Uani 0.303(3) 1 d D U P A 2
H18A H 0.2909 0.4581 1.0163 0.020 Uiso 0.303(3) 1 calc R . P A 2
C19 C 0.0764(8) 0.3785(3) 0.9336(9) 0.0159(10) Uani 0.697(3) 1 d D U P A 1
H19 H 0.0075 0.3596 0.9321 0.019 Uiso 0.697(3) 1 calc R . P A 1
C19A C 0.1336(13) 0.4237(8) 1.029(2) 0.017(2) Uani 0.303(3) 1 d D U P A 2
H19A H 0.1092 0.4403 1.1075 0.021 Uiso 0.303(3) 1 calc R . P A 2
C20 C 0.1145(5) 0.4164(3) 1.0271(10) 0.0158(11) Uani 0.697(3) 1 d D U P A 1
H20 H 0.0741 0.4273 1.0999 0.019 Uiso 0.697(3) 1 calc R . P A 1
C20A C 0.0761(19) 0.3866(9) 0.948(2) 0.016(2) Uani 0.303(3) 1 d D U P A 2
H20A H 0.0036 0.3745 0.9641 0.019 Uiso 0.303(3) 1 calc R . P A 2
C21 C 0.32439(17) 0.48703(8) 0.4059(2) 0.0108(4) Uani 1 1 d . U . . .
C22 C 0.20017(17) 0.48779(8) 0.3687(2) 0.0119(4) Uani 1 1 d D U . . .
C23 C 0.1230(7) 0.4532(3) 0.4114(11) 0.0179(16) Uani 0.525(3) 1 d D U P B 1
H23 H 0.1453 0.4253 0.4741 0.022 Uiso 0.525(3) 1 calc R . P B 1
C23A C 0.1341(8) 0.5237(4) 0.2913(11) 0.0193(17) Uani 0.475(3) 1 d D U P B 2
H23A H 0.1638 0.5537 0.2507 0.023 Uiso 0.475(3) 1 calc R . P B 2
C24 C 0.0092(9) 0.4618(6) 0.356(2) 0.0179(15) Uani 0.525(3) 1 d D U P B 1
H24 H -0.0528 0.4401 0.3715 0.021 Uiso 0.525(3) 1 calc R . P B 1
C24A C 0.0177(10) 0.5121(6) 0.277(2) 0.0179(15) Uani 0.475(3) 1 d D U P B 2
H24A H -0.0404 0.5321 0.2244 0.021 Uiso 0.475(3) 1 calc R . P B 2
C25 C 0.0026(8) 0.5061(6) 0.2784(19) 0.0157(15) Uani 0.525(3) 1 d D U P B 1
H25 H -0.0674 0.5201 0.2358 0.019 Uiso 0.525(3) 1 calc R . P B 1
C25A C 0.0015(10) 0.4680(7) 0.350(2) 0.0158(17) Uani 0.475(3) 1 d D U P B 2
H25A H -0.0717 0.4545 0.3568 0.019 Uiso 0.475(3) 1 calc R . P B 2
C26 C 0.77633(17) 0.37147(8) 0.4844(2) 0.0124(4) Uani 1 1 d . U . . .
C27 C 0.87387(17) 0.33433(9) 0.5173(2) 0.0142(4) Uani 1 1 d D U . . .
C28 C 0.9597(8) 0.3243(5) 0.4397(8) 0.0217(16) Uani 0.592(3) 1 d D U P C 1
H28 H 0.9669 0.3430 0.3568 0.026 Uiso 0.592(3) 1 calc R . P C 1
C28A C 0.8938(11) 0.2993(5) 0.6261(11) 0.020(2) Uani 0.408(3) 1 d D U P C 2
H28A H 0.8462 0.2976 0.6967 0.024 Uiso 0.408(3) 1 calc R . P C 2
C29 C 1.0361(10) 0.2845(4) 0.4909(11) 0.0220(13) Uani 0.592(3) 1 d D U P C 1
H29 H 1.1003 0.2735 0.4503 0.026 Uiso 0.592(3) 1 calc R . P C 1
C29A C 0.9887(13) 0.2663(8) 0.6270(17) 0.0178(17) Uani 0.408(3) 1 d D U P C 2
H29A H 1.0172 0.2424 0.6983 0.021 Uiso 0.408(3) 1 calc R . P C 2
C30 C 1.0025(8) 0.2646(5) 0.6080(11) 0.0163(14) Uani 0.592(3) 1 d D U P C 1
H30 H 1.0404 0.2363 0.6581 0.020 Uiso 0.592(3) 1 calc R . P C 1
C30A C 1.0315(13) 0.2750(5) 0.5072(16) 0.0193(19) Uani 0.408(3) 1 d D U P C 2
H30A H 1.0934 0.2555 0.4819 0.023 Uiso 0.408(3) 1 calc R . P C 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Eu1 O1 2.5844(16) . ?
Eu1 O2 2.4514(15) . ?
Eu1 O3 2.3416(15) 3_666 ?
Eu1 O4 2.3481(14) . ?
Eu1 O5 2.4220(15) . ?
Eu1 O7 2.4846(16) . ?
Eu1 N1 2.5720(19) . ?
Eu1 N2 2.6000(17) . ?
Eu1 N3 2.5893(18) . ?
Eu1 C16 2.865(2) . ?
S1 C17 1.697(2) . ?
S1 C20 1.731(5) . ?
S1A C17 1.662(4) . ?
S1A C20A 1.729(9) . ?
S2 C22 1.724(3) . ?
S2 C25 1.727(7) . ?
S2A C22 1.708(3) . ?
S2A C25A 1.724(8) . ?
S3 C27 1.693(3) . ?
S3 C30 1.727(6) . ?
S3A C27 1.683(3) . ?
S3A C30A 1.726(8) . ?
O1 C16 1.258(3) . ?
O2 C16 1.263(3) . ?
O3 Eu1 2.3415(14) 3_666 ?
O3 C21 1.264(2) . ?
O4 C21 1.256(2) . ?
O5 C26 1.267(3) . ?
O6 C26 1.244(3) . ?
O7 H7A 0.81(2) . ?
O7 H7B 0.81(2) . ?
O8 H8A 0.86(2) . ?
O8 H8B 0.86(2) . ?
N1 C1 1.341(3) . ?
N1 C5 1.344(3) . ?
N2 C6 1.347(3) . ?
N2 C10 1.344(3) . ?
N3 C11 1.352(3) . ?
N3 C15 1.343(3) . ?
C1 H1 0.9500 . ?
C1 C2 1.382(4) . ?
C2 H2 0.9500 . ?
C2 C3 1.373(4) . ?
C3 H3 0.9500 . ?
C3 C4 1.383(4) . ?
C4 H4 0.9500 . ?
C4 C5 1.395(3) . ?
C5 C6 1.486(3) . ?
C6 C7 1.395(3) . ?
C7 H7 0.9500 . ?
C7 C8 1.376(4) . ?
C8 H8 0.9500 . ?
C8 C9 1.378(3) . ?
C9 H9 0.9500 . ?
C9 C10 1.396(3) . ?
C10 C11 1.487(3) . ?
C11 C12 1.388(3) . ?
C12 H12 0.9500 . ?
C12 C13 1.379(3) . ?
C13 H13 0.9500 . ?
C13 C14 1.380(3) . ?
C14 H14 0.9500 . ?
C14 C15 1.384(3) . ?
C15 H15 0.9500 . ?
C16 C17 1.487(3) . ?
C17 C18 1.377(6) . ?
C17 C18A 1.383(8) . ?
C18 H18 0.9500 . ?
C18 C19 1.417(8) . ?
C18A H18A 0.9500 . ?
C18A C19A 1.412(10) . ?
C19 H19 0.9500 . ?
C19 C20 1.361(5) . ?
C19A H19A 0.9500 . ?
C19A C20A 1.356(8) . ?
C20 H20 0.9500 . ?
C20A H20A 0.9500 . ?
C21 C22 1.477(3) . ?
C22 C23 1.377(6) . ?
C22 C23A 1.364(7) . ?
C23 H23 0.9500 . ?
C23 C24 1.406(9) . ?
C23A H23A 0.9500 . ?
C23A C24A 1.407(9) . ?
C24 H24 0.9500 . ?
C24 C25 1.356(6) . ?
C24A H24A 0.9500 . ?
C24A C25A 1.354(7) . ?
C25 H25 0.9500 . ?
C25A H25A 0.9500 . ?
C26 C27 1.499(3) . ?
C27 C28 1.376(6) . ?
C27 C28A 1.379(7) . ?
C28 H28 0.9500 . ?
C28 C29 1.406(9) . ?
C28A H28A 0.9500 . ?
C28A C29A 1.409(10) . ?
C29 H29 0.9500 . ?
C29 C30 1.356(6) . ?
C29A H29A 0.9500 . ?
C29A C30A 1.353(7) . ?
C30 H30 0.9500 . ?
C30A H30A 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 Eu1 N2 107.20(5) . . ?
O1 Eu1 N3 120.63(5) . . ?
O1 Eu1 C16 26.05(6) . . ?
O2 Eu1 O1 52.06(5) . . ?
O2 Eu1 O7 136.93(5) . . ?
O2 Eu1 N1 83.53(6) . . ?
O2 Eu1 N2 70.29(5) . . ?
O2 Eu1 N3 71.49(5) . . ?
O2 Eu1 C16 26.04(6) . . ?
O3 Eu1 O1 77.48(5) 3_666 . ?
O3 Eu1 O2 129.54(5) 3_666 . ?
O3 Eu1 O4 88.35(5) 3_666 . ?
O3 Eu1 O5 81.58(5) 3_666 . ?
O3 Eu1 O7 77.81(5) 3_666 . ?
O3 Eu1 N1 78.71(6) 3_666 . ?
O3 Eu1 N2 135.33(5) 3_666 . ?
O3 Eu1 N3 152.76(6) 3_666 . ?
O3 Eu1 C16 103.51(6) 3_666 . ?
O4 Eu1 O1 71.83(6) . . ?
O4 Eu1 O2 76.81(5) . . ?
O4 Eu1 O5 142.44(5) . . ?
O4 Eu1 O7 71.00(6) . . ?
O4 Eu1 N1 141.06(6) . . ?
O4 Eu1 N2 135.96(5) . . ?
O4 Eu1 N3 79.68(5) . . ?
O4 Eu1 C16 71.70(6) . . ?
O5 Eu1 O1 139.02(5) . . ?
O5 Eu1 O2 135.87(5) . . ?
O5 Eu1 O7 71.51(5) . . ?
O5 Eu1 N1 72.04(6) . . ?
O5 Eu1 N2 65.96(5) . . ?
O5 Eu1 N3 93.09(5) . . ?
O5 Eu1 C16 145.85(6) . . ?
O7 Eu1 O1 135.47(6) . . ?
O7 Eu1 N1 138.90(6) . . ?
O7 Eu1 N2 116.44(6) . . ?
O7 Eu1 N3 75.18(6) . . ?
O7 Eu1 C16 142.62(6) . . ?
N1 Eu1 O1 69.56(6) . . ?
N1 Eu1 N2 62.99(6) . . ?
N1 Eu1 N3 125.16(6) . . ?
N1 Eu1 C16 75.89(6) . . ?
N2 Eu1 C16 89.24(6) . . ?
N3 Eu1 N2 62.78(6) . . ?
N3 Eu1 C16 95.87(6) . . ?
C17 S1 C20 91.4(3) . . ?
C17 S1A C20A 89.0(8) . . ?
C22 S2 C25 90.2(5) . . ?
C22 S2A C25A 89.0(6) . . ?
C27 S3 C30 90.6(4) . . ?
C27 S3A C30A 90.6(6) . . ?
C16 O1 Eu1 89.51(13) . . ?
C16 O2 Eu1 95.57(13) . . ?
C21 O3 Eu1 140.08(14) . 3_666 ?
C21 O4 Eu1 151.36(14) . . ?
C26 O5 Eu1 142.90(14) . . ?
Eu1 O7 H7A 108(2) . . ?
Eu1 O7 H7B 121(3) . . ?
H7A O7 H7B 116(3) . . ?
H8A O8 H8B 103(3) . . ?
C1 N1 Eu1 119.80(16) . . ?
C1 N1 C5 118.3(2) . . ?
C5 N1 Eu1 119.39(15) . . ?
C6 N2 Eu1 119.48(14) . . ?
C10 N2 Eu1 121.60(14) . . ?
C10 N2 C6 118.81(19) . . ?
C11 N3 Eu1 121.64(14) . . ?
C15 N3 Eu1 120.15(14) . . ?
C15 N3 C11 117.79(19) . . ?
N1 C1 H1 118.4 . . ?
N1 C1 C2 123.2(3) . . ?
C2 C1 H1 118.4 . . ?
C1 C2 H2 120.8 . . ?
C3 C2 C1 118.3(3) . . ?
C3 C2 H2 120.8 . . ?
C2 C3 H3 120.3 . . ?
C2 C3 C4 119.5(2) . . ?
C4 C3 H3 120.3 . . ?
C3 C4 H4 120.5 . . ?
C3 C4 C5 119.0(3) . . ?
C5 C4 H4 120.5 . . ?
N1 C5 C4 121.5(2) . . ?
N1 C5 C6 116.16(19) . . ?
C4 C5 C6 122.3(2) . . ?
N2 C6 C5 117.00(19) . . ?
N2 C6 C7 121.8(2) . . ?
C7 C6 C5 121.2(2) . . ?
C6 C7 H7 120.3 . . ?
C8 C7 C6 119.4(2) . . ?
C8 C7 H7 120.3 . . ?
C7 C8 H8 120.6 . . ?
C7 C8 C9 118.8(2) . . ?
C9 C8 H8 120.6 . . ?
C8 C9 H9 120.3 . . ?
C8 C9 C10 119.4(2) . . ?
C10 C9 H9 120.3 . . ?
N2 C10 C9 121.7(2) . . ?
N2 C10 C11 116.80(18) . . ?
C9 C10 C11 121.5(2) . . ?
N3 C11 C10 116.58(19) . . ?
N3 C11 C12 121.6(2) . . ?
C12 C11 C10 121.8(2) . . ?
C11 C12 H12 120.1 . . ?
C13 C12 C11 119.8(2) . . ?
C13 C12 H12 120.1 . . ?
C12 C13 H13 120.5 . . ?
C12 C13 C14 118.9(2) . . ?
C14 C13 H13 120.5 . . ?
C13 C14 H14 120.8 . . ?
C13 C14 C15 118.4(2) . . ?
C15 C14 H14 120.8 . . ?
N3 C15 C14 123.5(2) . . ?
N3 C15 H15 118.2 . . ?
C14 C15 H15 118.2 . . ?
O1 C16 Eu1 64.44(12) . . ?
O1 C16 O2 122.7(2) . . ?
O1 C16 C17 120.1(2) . . ?
O2 C16 Eu1 58.40(11) . . ?
O2 C16 C17 117.16(19) . . ?
C17 C16 Eu1 174.86(15) . . ?
C16 C17 S1 122.87(16) . . ?
C16 C17 S1A 118.6(2) . . ?
C18 C17 S1 110.6(3) . . ?
C18 C17 C16 126.5(4) . . ?
C18A C17 S1A 113.7(7) . . ?
C18A C17 C16 127.7(7) . . ?
C17 C18 H18 122.5 . . ?
C17 C18 C19 115.1(6) . . ?
C19 C18 H18 122.5 . . ?
C17 C18A H18A 123.2 . . ?
C17 C18A C19A 113.5(14) . . ?
C19A C18A H18A 123.2 . . ?
C18 C19 H19 125.3 . . ?
C20 C19 C18 109.4(8) . . ?
C20 C19 H19 125.3 . . ?
C18A C19A H19A 126.1 . . ?
C20A C19A C18A 107.7(19) . . ?
C20A C19A H19A 126.1 . . ?
S1 C20 H20 123.3 . . ?
C19 C20 S1 113.5(7) . . ?
C19 C20 H20 123.3 . . ?
S1A C20A H20A 122.0 . . ?
C19A C20A S1A 116.0(17) . . ?
C19A C20A H20A 122.0 . . ?
O3 C21 C22 118.82(18) . . ?
O4 C21 O3 124.43(19) . . ?
O4 C21 C22 116.74(18) . . ?
C21 C22 S2 122.55(16) . . ?
C21 C22 S2A 118.28(16) . . ?
C23 C22 S2 110.0(4) . . ?
C23 C22 C21 127.4(4) . . ?
C23A C22 S2A 112.7(4) . . ?
C23A C22 C21 129.0(4) . . ?
C22 C23 H23 122.0 . . ?
C22 C23 C24 115.9(9) . . ?
C24 C23 H23 122.0 . . ?
C22 C23A H23A 123.1 . . ?
C22 C23A C24A 113.8(10) . . ?
C24A C23A H23A 123.1 . . ?
C23 C24 H24 125.7 . . ?
C25 C24 C23 108.7(13) . . ?
C25 C24 H24 125.7 . . ?
C23A C24A H24A 125.4 . . ?
C25A C24A C23A 109.3(14) . . ?
C25A C24A H24A 125.4 . . ?
S2 C25 H25 122.5 . . ?
C24 C25 S2 115.0(11) . . ?
C24 C25 H25 122.5 . . ?
S2A C25A H25A 122.4 . . ?
C24A C25A S2A 115.2(13) . . ?
C24A C25A H25A 122.4 . . ?
O5 C26 C27 115.79(19) . . ?
O6 C26 O5 126.4(2) . . ?
O6 C26 C27 117.78(19) . . ?
C26 C27 S3 121.36(16) . . ?
C26 C27 S3A 120.93(19) . . ?
C28 C27 S3 110.6(4) . . ?
C28 C27 C26 127.9(4) . . ?
C28A C27 S3A 110.2(5) . . ?
C28A C27 C26 128.2(5) . . ?
C27 C28 H28 122.1 . . ?
C27 C28 C29 115.8(8) . . ?
C29 C28 H28 122.1 . . ?
C27 C28A H28A 121.8 . . ?
C27 C28A C29A 116.4(11) . . ?
C29A C28A H28A 121.8 . . ?
C28 C29 H29 125.9 . . ?
C30 C29 C28 108.3(10) . . ?
C30 C29 H29 125.9 . . ?
C28A C29A H29A 126.5 . . ?
C30A C29A C28A 107.1(15) . . ?
C30A C29A H29A 126.5 . . ?
S3 C30 H30 122.7 . . ?
C29 C30 S3 114.7(9) . . ?
C29 C30 H30 122.7 . . ?
S3A C30A H30A 122.3 . . ?
C29A C30A S3A 115.4(13) . . ?
C29A C30A H30A 122.3 . . ?

_olex2_submission_original_sample_id RJB389
_olex2_submission_special_instructions 'No special instructions were received'

####################################################################### 
# 
# 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_final_a_CCDC10
_database_code_depnum_ccdc_archive 'CCDC 1544441'
_audit_update_record             
;
2017-04-17 deposited with the CCDC.
2017-08-23 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT417_final_a             
;
PROBLEM: Short Inter D-H..H-D       H7B    ..  H8B     ..       1.57 Ang.
RESPONSE: These hydrogens are water hydrogen atoms which were found in the difference map in good hydrogen bond locations. H8B is part of a partially occupied lattice water molecule which is only present 35% of the time
;
# Added during the CSD deposition process: Monday 17 April 2017 03:19 PM
# end Validation Reply Form



_audit_creation_date             2017-04-06
_audit_creation_method           
;
Olex2 1.2
(compiled Mar 28 2017 19:26:29 for OlexSys, GUI svn.r5335)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C60 H44 Ce2 N6 O14 S6, 0.69(H2 O)'
_chemical_formula_sum            'C60 H45.39 Ce2 N6 O14.69 S6'
_chemical_formula_weight         1558.14
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ce Ce -0.2486 2.6331 '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'

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

_cell_length_a                   12.0450(6)
_cell_length_b                   25.8165(12)
_cell_length_c                   9.6836(4)
_cell_angle_alpha                90
_cell_angle_beta                 98.2700(10)
_cell_angle_gamma                90
_cell_volume                     2979.9(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9800
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.14
_cell_measurement_theta_min      2.27
_shelx_estimated_absorpt_T_max   0.785
_shelx_estimated_absorpt_T_min   0.456
_exptl_absorpt_coefficient_mu    1.792
_exptl_absorpt_correction_T_max  0.8512
_exptl_absorpt_correction_T_min  0.5690
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1315 before and 0.0531 after correction.
The Ratio of minimum to maximum transmission is 0.6685.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.737
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       rhombohedral
_exptl_crystal_F_000             1554
_exptl_crystal_size_max          0.519
_exptl_crystal_size_mid          0.249
_exptl_crystal_size_min          0.142
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_av_unetI/netI     0.0292
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            34525
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.146
_diffrn_reflns_theta_min         2.326
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5802
_reflns_number_total             6588
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.385
_refine_diff_density_min         -0.644
_refine_diff_density_rms         0.084
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     530
_refine_ls_number_reflns         6588
_refine_ls_number_restraints     1002
_refine_ls_R_factor_all          0.0332
_refine_ls_R_factor_gt           0.0254
_refine_ls_restrained_S_all      1.044
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0153P)²+2.5824P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0472
_refine_ls_wR_factor_ref         0.0489
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O7-H7A = O7-H7B
 0.86 with sigma of 0.02
 O8-H8A = O8-H8B
 0.86 with sigma of 0.02
 H8A-H8B
 1.35 with sigma of 0.02
 H7B-H7A
 1.35 with sigma of 0.02
 S3A-C27 \\sim S3-C27 \\sim S2-C22 \\sim S2A-C22 \\sim S1A-C17 \\sim S1-C17
 with sigma of 0.01
 S3A-C30A \\sim S3-C30 \\sim S2-C25 \\sim S2A-C25A \\sim S1-C20 \\sim S1A-C20A
 with sigma of 0.01
 C20-C19 \\sim C20A-C19A \\sim C25-C24 \\sim C25A-C24A \\sim C30-C29 \\sim
C30A-C29A
 with sigma of 0.01
 C28-C27 \\sim C28A-C27 \\sim C23A-C22 \\sim C23-C22 \\sim C18A-C17 \\sim
C18-C17
 with sigma of 0.01
 C29A-C28A \\sim C29-C28 \\sim C24A-C23A \\sim C24-C23 \\sim C19A-C18A \\sim
C19-C18
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
S1 \\sim S1A \\sim C17 \\sim C18 \\sim C18A \\sim C19 \\sim C19A \\sim C20
\\sim C20A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
S2 \\sim S2A \\sim C22 \\sim C23 \\sim C23A \\sim C24 \\sim C24A \\sim C25
\\sim C25A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
S3 \\sim S3A \\sim C27 \\sim C28 \\sim C28A \\sim C29 \\sim C29A \\sim C30
\\sim C30A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(S1A)=Sof(C18A)=Sof(H18A)=Sof(C19A)=Sof(H19A)=Sof(C20A)=Sof(H20A)=1-FVAR(1)
 Sof(S1)=Sof(C18)=Sof(H18)=Sof(C19)=Sof(H19)=Sof(C20)=Sof(H20)=FVAR(1)
 Sof(S2A)=Sof(C23A)=Sof(H23A)=Sof(C24A)=Sof(H24A)=Sof(C25A)=Sof(H25A)=1-FVAR(2)
 Sof(S2)=Sof(C23)=Sof(H23)=Sof(C24)=Sof(H24)=Sof(C25)=Sof(H25)=FVAR(2)
 Sof(S3A)=Sof(C28A)=Sof(H28A)=Sof(C29A)=Sof(H29A)=Sof(C30A)=Sof(H30A)=1-FVAR(3)
 Sof(S3)=Sof(C28)=Sof(H28)=Sof(C29)=Sof(H29)=Sof(C30)=Sof(H30)=FVAR(3)
 Sof(O8)=Sof(H8A)=Sof(H8B)=FVAR(4)
6.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C12(H12), C13(H13),
 C14(H14), C15(H15), C18(H18), C18A(H18A), C19(H19), C19A(H19A), C20(H20),
 C20A(H20A), C23(H23), C23A(H23A), C24(H24), C24A(H24A), C25(H25), C25A(H25A),
 C28(H28), C28A(H28A), C29(H29), C29A(H29A), C30(H30), C30A(H30A)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ce1 Ce 0.51775(2) 0.59834(2) 0.59809(2) 0.01063(4) Uani 1 1 d . U . . .
S1 S 0.24216(14) 0.55674(7) 1.00340(16) 0.0181(3) Uani 0.693(3) 1 d D U P A 1
S1A S 0.1434(4) 0.6365(2) 0.8157(5) 0.0156(8) Uani 0.307(3) 1 d D U P A 2
S2 S 0.12281(19) 0.56213(9) 0.4270(3) 0.0169(5) Uani 0.458(3) 1 d D U P B 1
S2A S 0.12667(16) 0.46536(8) 0.2629(2) 0.0169(4) Uani 0.542(3) 1 d D U P B 2
S3 S 0.8881(2) 0.70460(9) 0.6604(2) 0.0187(4) Uani 0.571(3) 1 d D U P C 1
S3A S 0.9696(3) 0.67588(16) 0.4059(3) 0.0267(6) Uani 0.429(3) 1 d D U P C 2
O1 O 0.41579(14) 0.55982(6) 0.80094(18) 0.0253(4) Uani 1 1 d . U . . .
O2 O 0.35240(13) 0.63362(6) 0.70277(16) 0.0183(3) Uani 1 1 d . U . . .
O3 O 0.36298(13) 0.54737(6) 0.48516(17) 0.0203(4) Uani 1 1 d . U . . .
O4 O 0.37626(13) 0.47968(6) 0.34605(16) 0.0194(3) Uani 1 1 d . U . . .
O5 O 0.70717(12) 0.63104(6) 0.56656(16) 0.0179(3) Uani 1 1 d . U . . .
O6 O 0.77632(13) 0.60258(6) 0.37764(16) 0.0198(3) Uani 1 1 d . U . . .
O7 O 0.56272(14) 0.57074(7) 0.35952(17) 0.0219(4) Uani 1 1 d D U . . .
H7A H 0.6305(15) 0.5759(10) 0.354(3) 0.033 Uiso 1 1 d DR . . . .
H7B H 0.536(2) 0.5456(8) 0.320(3) 0.033 Uiso 1 1 d DR . . . .
O8 O 0.5021(4) 0.4708(2) 0.8993(5) 0.0270(18) Uani 0.349(6) 1 d D U P . .
H8A H 0.469(6) 0.4995(16) 0.907(8) 0.041 Uiso 0.349(6) 1 d DR . P . .
H8B H 0.460(5) 0.453(2) 0.841(7) 0.041 Uiso 0.349(6) 1 d DR . P . .
N1 N 0.41262(15) 0.66888(7) 0.42740(18) 0.0140(4) Uani 1 1 d . U . . .
N2 N 0.55087(14) 0.69927(7) 0.65947(18) 0.0126(4) Uani 1 1 d . U . . .
N3 N 0.62867(16) 0.62370(8) 0.84415(19) 0.0200(4) Uani 1 1 d . U . . .
C1 C 0.34157(19) 0.65310(9) 0.3150(2) 0.0186(5) Uani 1 1 d . U . . .
H1 H 0.3355 0.6170 0.2963 0.022 Uiso 1 1 calc R . . . .
C2 C 0.27715(19) 0.68648(9) 0.2256(2) 0.0209(5) Uani 1 1 d . U . . .
H2 H 0.2280 0.6737 0.1474 0.025 Uiso 1 1 calc R . . . .
C3 C 0.28583(19) 0.73890(9) 0.2524(2) 0.0213(5) Uani 1 1 d . U . . .
H3 H 0.2434 0.7630 0.1922 0.026 Uiso 1 1 calc R . . . .
C4 C 0.35695(19) 0.75586(9) 0.3678(2) 0.0186(5) Uani 1 1 d . U . . .
H4 H 0.3629 0.7918 0.3885 0.022 Uiso 1 1 calc R . . . .
C5 C 0.41993(18) 0.72029(8) 0.4539(2) 0.0136(4) Uani 1 1 d . U . . .
C6 C 0.50075(18) 0.73671(8) 0.5770(2) 0.0142(5) Uani 1 1 d . U . . .
C7 C 0.5232(2) 0.78908(9) 0.6041(2) 0.0188(5) Uani 1 1 d . U . . .
H7 H 0.4872 0.8149 0.5437 0.023 Uiso 1 1 calc R . . . .
C8 C 0.5982(2) 0.80284(9) 0.7195(3) 0.0232(5) Uani 1 1 d . U . . .
H8 H 0.6142 0.8383 0.7401 0.028 Uiso 1 1 calc R . . . .
C9 C 0.64942(19) 0.76459(9) 0.8042(2) 0.0216(5) Uani 1 1 d . U . . .
H9 H 0.7012 0.7733 0.8843 0.026 Uiso 1 1 calc R . . . .
C10 C 0.62490(18) 0.71303(9) 0.7718(2) 0.0164(5) Uani 1 1 d . U . . .
C11 C 0.67597(19) 0.67072(9) 0.8638(2) 0.0186(5) Uani 1 1 d . U . . .
C12 C 0.7662(2) 0.67914(11) 0.9688(2) 0.0283(6) Uani 1 1 d . U . . .
H12 H 0.8017 0.7121 0.9784 0.034 Uiso 1 1 calc R . . . .
C13 C 0.8036(2) 0.63938(12) 1.0582(3) 0.0341(7) Uani 1 1 d . U . . .
H13 H 0.8642 0.6449 1.1310 0.041 Uiso 1 1 calc R . . . .
C14 C 0.7530(2) 0.59199(12) 1.0418(3) 0.0361(7) Uani 1 1 d . U . . .
H14 H 0.7761 0.5643 1.1040 0.043 Uiso 1 1 calc R . . . .
C15 C 0.6669(2) 0.58546(10) 0.9316(2) 0.0291(6) Uani 1 1 d . U . . .
H15 H 0.6335 0.5522 0.9175 0.035 Uiso 1 1 calc R . . . .
C16 C 0.34539(19) 0.59623(9) 0.7851(2) 0.0170(5) Uani 1 1 d . U . . .
C17 C 0.24951(18) 0.59661(8) 0.8659(2) 0.0156(4) Uani 1 1 d D U . . .
C18 C 0.1562(6) 0.6279(4) 0.8419(9) 0.0154(14) Uani 0.693(3) 1 d D U P A 1
H18 H 0.1461 0.6528 0.7690 0.019 Uiso 0.693(3) 1 calc R . P A 1
C18A C 0.2349(14) 0.5663(6) 0.9791(14) 0.020(2) Uani 0.307(3) 1 d D U P A 2
H18A H 0.2888 0.5417 1.0187 0.024 Uiso 0.307(3) 1 calc R . P A 2
C19 C 0.0760(8) 0.6203(3) 0.9341(9) 0.0165(11) Uani 0.693(3) 1 d D U P A 1
H19 H 0.0073 0.6386 0.9312 0.020 Uiso 0.693(3) 1 calc R . P A 1
C19A C 0.1325(13) 0.5752(8) 1.031(2) 0.018(2) Uani 0.307(3) 1 d D U P A 2
H19A H 0.1078 0.5587 1.1092 0.022 Uiso 0.307(3) 1 calc R . P A 2
C20 C 0.1135(5) 0.5824(3) 1.0272(10) 0.0163(11) Uani 0.693(3) 1 d D U P A 1
H20 H 0.0727 0.5711 1.0987 0.020 Uiso 0.693(3) 1 calc R . P A 1
C20A C 0.0767(19) 0.6118(8) 0.948(2) 0.017(2) Uani 0.307(3) 1 d D U P A 2
H20A H 0.0043 0.6234 0.9620 0.020 Uiso 0.307(3) 1 calc R . P A 2
C21 C 0.32075(18) 0.51301(8) 0.4020(2) 0.0128(4) Uani 1 1 d . U . . .
C22 C 0.19726(17) 0.51258(8) 0.3675(2) 0.0128(4) Uani 1 1 d D U . . .
C23 C 0.1299(8) 0.4772(4) 0.2922(11) 0.0194(18) Uani 0.458(3) 1 d D U P B 1
H23 H 0.1588 0.4474 0.2521 0.023 Uiso 0.458(3) 1 calc R . P B 1
C23A C 0.1224(7) 0.5467(3) 0.4117(11) 0.0191(16) Uani 0.542(3) 1 d D U P B 2
H23A H 0.1460 0.5742 0.4743 0.023 Uiso 0.542(3) 1 calc R . P B 2
C24 C 0.0140(10) 0.4880(6) 0.278(2) 0.0183(16) Uani 0.458(3) 1 d D U P B 1
H24 H -0.0445 0.4679 0.2277 0.022 Uiso 0.458(3) 1 calc R . P B 1
C24A C 0.0080(9) 0.5387(6) 0.359(2) 0.0173(14) Uani 0.542(3) 1 d D U P B 2
H24A H -0.0529 0.5601 0.3751 0.021 Uiso 0.542(3) 1 calc R . P B 2
C25 C 0.0016(10) 0.5322(7) 0.349(2) 0.0158(18) Uani 0.458(3) 1 d D U P B 1
H25 H -0.0704 0.5461 0.3563 0.019 Uiso 0.458(3) 1 calc R . P B 1
C25A C 0.0010(8) 0.4949(5) 0.2808(18) 0.0163(15) Uani 0.542(3) 1 d D U P B 2
H25A H -0.0690 0.4813 0.2384 0.020 Uiso 0.542(3) 1 calc R . P B 2
C26 C 0.78015(18) 0.62975(8) 0.4848(2) 0.0143(4) Uani 1 1 d . U . . .
C27 C 0.87656(18) 0.66605(9) 0.5182(2) 0.0163(5) Uani 1 1 d D U . . .
C28 C 0.9617(8) 0.6753(5) 0.4416(9) 0.0255(17) Uani 0.571(3) 1 d D U P C 1
H28 H 0.9683 0.6570 0.3581 0.031 Uiso 0.571(3) 1 calc R . P C 1
C28A C 0.8961(11) 0.7001(5) 0.6279(11) 0.022(2) Uani 0.429(3) 1 d D U P C 2
H28A H 0.8496 0.7015 0.6991 0.027 Uiso 0.429(3) 1 calc R . P C 2
C29 C 1.0388(10) 0.7138(3) 0.4952(11) 0.0228(14) Uani 0.571(3) 1 d D U P C 1
H29 H 1.1032 0.7240 0.4558 0.027 Uiso 0.571(3) 1 calc R . P C 1
C29A C 0.9899(12) 0.7330(8) 0.6279(17) 0.0217(17) Uani 0.429(3) 1 d D U P C 2
H29A H 1.0175 0.7569 0.6994 0.026 Uiso 0.429(3) 1 calc R . P C 2
C30 C 1.0060(8) 0.7340(5) 0.6125(12) 0.0184(14) Uani 0.571(3) 1 d D U P C 1
H30 H 1.0443 0.7617 0.6635 0.022 Uiso 0.571(3) 1 calc R . P C 1
C30A C 1.0340(12) 0.7247(5) 0.5086(15) 0.0219(18) Uani 0.429(3) 1 d D U P C 2
H30A H 1.0951 0.7442 0.4839 0.026 Uiso 0.429(3) 1 calc R . P C 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ce1 O1 2.6551(16) . ?
Ce1 O2 2.5307(15) . ?
Ce1 O3 2.4116(15) . ?
Ce1 O4 2.4044(15) 3_666 ?
Ce1 O5 2.4924(15) . ?
Ce1 O7 2.5492(16) . ?
Ce1 N1 2.6551(18) . ?
Ce1 N2 2.6894(18) . ?
Ce1 N3 2.6411(18) . ?
Ce1 C16 2.945(2) . ?
S1 C17 1.696(2) . ?
S1 C20 1.731(5) . ?
S1A C17 1.659(4) . ?
S1A C20A 1.730(9) . ?
S2 C22 1.709(3) . ?
S2 C25 1.726(8) . ?
S2A C22 1.728(2) . ?
S2A C25A 1.726(7) . ?
S3 C27 1.689(3) . ?
S3 C30 1.731(6) . ?
S3A C27 1.689(3) . ?
S3A C30A 1.720(8) . ?
O1 C16 1.260(3) . ?
O2 C16 1.263(3) . ?
O3 C21 1.256(3) . ?
O4 Ce1 2.4045(15) 3_666 ?
O4 C21 1.259(3) . ?
O5 C26 1.265(3) . ?
O6 C26 1.248(3) . ?
O7 H7A 0.837(16) . ?
O7 H7B 0.797(16) . ?
O8 H8A 0.85(2) . ?
O8 H8B 0.84(2) . ?
N1 C1 1.348(3) . ?
N1 C5 1.352(3) . ?
N2 C6 1.341(3) . ?
N2 C10 1.351(3) . ?
N3 C11 1.343(3) . ?
N3 C15 1.339(3) . ?
C1 H1 0.9500 . ?
C1 C2 1.379(3) . ?
C2 H2 0.9500 . ?
C2 C3 1.379(3) . ?
C3 H3 0.9500 . ?
C3 C4 1.378(3) . ?
C4 H4 0.9500 . ?
C4 C5 1.390(3) . ?
C5 C6 1.488(3) . ?
C6 C7 1.396(3) . ?
C7 H7 0.9500 . ?
C7 C8 1.380(3) . ?
C8 H8 0.9500 . ?
C8 C9 1.372(4) . ?
C9 H9 0.9500 . ?
C9 C10 1.390(3) . ?
C10 C11 1.486(3) . ?
C11 C12 1.394(3) . ?
C12 H12 0.9500 . ?
C12 C13 1.376(4) . ?
C13 H13 0.9500 . ?
C13 C14 1.365(4) . ?
C14 H14 0.9500 . ?
C14 C15 1.387(4) . ?
C15 H15 0.9500 . ?
C16 C17 1.485(3) . ?
C17 C18 1.377(6) . ?
C17 C18A 1.378(8) . ?
C18 H18 0.9500 . ?
C18 C19 1.419(8) . ?
C18A H18A 0.9500 . ?
C18A C19A 1.417(10) . ?
C19 H19 0.9500 . ?
C19 C20 1.363(5) . ?
C19A H19A 0.9500 . ?
C19A C20A 1.356(7) . ?
C20 H20 0.9500 . ?
C20A H20A 0.9500 . ?
C21 C22 1.477(3) . ?
C22 C23 1.362(7) . ?
C22 C23A 1.373(6) . ?
C23 H23 0.9500 . ?
C23 C24 1.411(9) . ?
C23A H23A 0.9500 . ?
C23A C24A 1.414(9) . ?
C24 H24 0.9500 . ?
C24 C25 1.353(7) . ?
C24A H24A 0.9500 . ?
C24A C25A 1.355(6) . ?
C25 H25 0.9500 . ?
C25A H25A 0.9500 . ?
C26 C27 1.491(3) . ?
C27 C28 1.370(7) . ?
C27 C28A 1.374(7) . ?
C28 H28 0.9500 . ?
C28 C29 1.406(9) . ?
C28A H28A 0.9500 . ?
C28A C29A 1.414(10) . ?
C29 H29 0.9500 . ?
C29 C30 1.359(6) . ?
C29A H29A 0.9500 . ?
C29A C30A 1.356(7) . ?
C30 H30 0.9500 . ?
C30A H30A 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 Ce1 N1 119.18(5) . . ?
O1 Ce1 N2 105.61(5) . . ?
O1 Ce1 C16 25.33(6) . . ?
O2 Ce1 O1 50.51(5) . . ?
O2 Ce1 O7 138.22(5) . . ?
O2 Ce1 N1 70.74(5) . . ?
O2 Ce1 N2 70.31(5) . . ?
O2 Ce1 N3 82.79(5) . . ?
O2 Ce1 C16 25.23(6) . . ?
O3 Ce1 O1 73.83(6) . . ?
O3 Ce1 O2 77.08(5) . . ?
O3 Ce1 O5 142.26(5) . . ?
O3 Ce1 O7 71.80(5) . . ?
O3 Ce1 N1 79.84(5) . . ?
O3 Ce1 N2 135.18(5) . . ?
O3 Ce1 N3 143.33(6) . . ?
O3 Ce1 C16 72.63(6) . . ?
O4 Ce1 O1 78.87(5) 3_666 . ?
O4 Ce1 O2 129.37(5) 3_666 . ?
O4 Ce1 O3 89.75(5) 3_666 . ?
O4 Ce1 O5 81.11(5) 3_666 . ?
O4 Ce1 O7 78.14(5) 3_666 . ?
O4 Ce1 N1 154.81(5) 3_666 . ?
O4 Ce1 N2 134.81(5) 3_666 . ?
O4 Ce1 N3 79.71(6) 3_666 . ?
O4 Ce1 C16 104.16(6) 3_666 . ?
O5 Ce1 O1 138.28(5) . . ?
O5 Ce1 O2 135.58(5) . . ?
O5 Ce1 O7 70.49(5) . . ?
O5 Ce1 N1 93.12(5) . . ?
O5 Ce1 N2 65.77(5) . . ?
O5 Ce1 N3 70.93(6) . . ?
O5 Ce1 C16 145.11(5) . . ?
O7 Ce1 O1 138.33(6) . . ?
O7 Ce1 N1 76.83(5) . . ?
O7 Ce1 N2 115.28(5) . . ?
O7 Ce1 N3 137.82(6) . . ?
O7 Ce1 C16 144.35(6) . . ?
N1 Ce1 N2 61.01(5) . . ?
N1 Ce1 C16 94.61(6) . . ?
N2 Ce1 C16 88.70(6) . . ?
N3 Ce1 O1 69.71(6) . . ?
N3 Ce1 N1 121.71(6) . . ?
N3 Ce1 N2 61.36(6) . . ?
N3 Ce1 C16 76.09(6) . . ?
C17 S1 C20 91.2(3) . . ?
C17 S1A C20A 88.5(8) . . ?
C22 S2 C25 88.3(6) . . ?
C25A S2A C22 89.7(5) . . ?
C27 S3 C30 90.8(4) . . ?
C27 S3A C30A 91.4(6) . . ?
C16 O1 Ce1 90.32(13) . . ?
C16 O2 Ce1 96.07(13) . . ?
C21 O3 Ce1 153.10(14) . . ?
C21 O4 Ce1 140.67(14) . 3_666 ?
C26 O5 Ce1 142.98(14) . . ?
Ce1 O7 H7A 110.6(18) . . ?
Ce1 O7 H7B 122(2) . . ?
H7A O7 H7B 116(2) . . ?
H8A O8 H8B 107(3) . . ?
C1 N1 Ce1 119.09(14) . . ?
C1 N1 C5 117.81(19) . . ?
C5 N1 Ce1 122.88(14) . . ?
C6 N2 Ce1 121.80(14) . . ?
C6 N2 C10 118.58(19) . . ?
C10 N2 Ce1 119.50(14) . . ?
C11 N3 Ce1 120.09(14) . . ?
C15 N3 Ce1 118.12(16) . . ?
C15 N3 C11 118.5(2) . . ?
N1 C1 H1 118.2 . . ?
N1 C1 C2 123.6(2) . . ?
C2 C1 H1 118.2 . . ?
C1 C2 H2 120.9 . . ?
C1 C2 C3 118.3(2) . . ?
C3 C2 H2 120.9 . . ?
C2 C3 H3 120.5 . . ?
C4 C3 C2 119.1(2) . . ?
C4 C3 H3 120.5 . . ?
C3 C4 H4 120.1 . . ?
C3 C4 C5 119.9(2) . . ?
C5 C4 H4 120.1 . . ?
N1 C5 C4 121.3(2) . . ?
N1 C5 C6 116.66(19) . . ?
C4 C5 C6 122.0(2) . . ?
N2 C6 C5 117.28(19) . . ?
N2 C6 C7 121.9(2) . . ?
C7 C6 C5 120.8(2) . . ?
C6 C7 H7 120.4 . . ?
C8 C7 C6 119.2(2) . . ?
C8 C7 H7 120.4 . . ?
C7 C8 H8 120.5 . . ?
C9 C8 C7 119.0(2) . . ?
C9 C8 H8 120.5 . . ?
C8 C9 H9 120.3 . . ?
C8 C9 C10 119.5(2) . . ?
C10 C9 H9 120.3 . . ?
N2 C10 C9 121.9(2) . . ?
N2 C10 C11 117.3(2) . . ?
C9 C10 C11 120.8(2) . . ?
N3 C11 C10 116.67(19) . . ?
N3 C11 C12 121.0(2) . . ?
C12 C11 C10 122.3(2) . . ?
C11 C12 H12 120.3 . . ?
C13 C12 C11 119.5(3) . . ?
C13 C12 H12 120.3 . . ?
C12 C13 H13 120.2 . . ?
C14 C13 C12 119.7(2) . . ?
C14 C13 H13 120.2 . . ?
C13 C14 H14 121.0 . . ?
C13 C14 C15 118.1(3) . . ?
C15 C14 H14 121.0 . . ?
N3 C15 C14 123.2(3) . . ?
N3 C15 H15 118.4 . . ?
C14 C15 H15 118.4 . . ?
O1 C16 Ce1 64.35(12) . . ?
O1 C16 O2 122.8(2) . . ?
O1 C16 C17 120.1(2) . . ?
O2 C16 Ce1 58.69(11) . . ?
O2 C16 C17 117.1(2) . . ?
C17 C16 Ce1 173.74(15) . . ?
C16 C17 S1 122.82(17) . . ?
C16 C17 S1A 118.4(2) . . ?
C18 C17 S1 110.8(3) . . ?
C18 C17 C16 126.4(4) . . ?
C18A C17 S1A 113.8(7) . . ?
C18A C17 C16 127.8(7) . . ?
C17 C18 H18 122.4 . . ?
C17 C18 C19 115.2(6) . . ?
C19 C18 H18 122.4 . . ?
C17 C18A H18A 122.9 . . ?
C17 C18A C19A 114.2(14) . . ?
C19A C18A H18A 122.9 . . ?
C18 C19 H19 125.5 . . ?
C20 C19 C18 109.0(8) . . ?
C20 C19 H19 125.5 . . ?
C18A C19A H19A 126.8 . . ?
C20A C19A C18A 106(2) . . ?
C20A C19A H19A 126.8 . . ?
S1 C20 H20 123.1 . . ?
C19 C20 S1 113.8(7) . . ?
C19 C20 H20 123.1 . . ?
S1A C20A H20A 121.5 . . ?
C19A C20A S1A 117.0(17) . . ?
C19A C20A H20A 121.5 . . ?
O3 C21 O4 124.6(2) . . ?
O3 C21 C22 116.87(19) . . ?
O4 C21 C22 118.54(19) . . ?
C21 C22 S2 118.59(16) . . ?
C21 C22 S2A 122.15(16) . . ?
C23 C22 S2 112.4(4) . . ?
C23 C22 C21 129.0(5) . . ?
C23A C22 S2A 110.2(4) . . ?
C23A C22 C21 127.6(4) . . ?
C22 C23 H23 122.4 . . ?
C22 C23 C24 115.2(10) . . ?
C24 C23 H23 122.4 . . ?
C22 C23A H23A 121.9 . . ?
C22 C23A C24A 116.3(9) . . ?
C24A C23A H23A 121.9 . . ?
C23 C24 H24 126.4 . . ?
C25 C24 C23 107.2(14) . . ?
C25 C24 H24 126.4 . . ?
C23A C24A H24A 126.2 . . ?
C25A C24A C23A 107.7(12) . . ?
C25A C24A H24A 126.2 . . ?
S2 C25 H25 121.6 . . ?
C24 C25 S2 116.9(13) . . ?
C24 C25 H25 121.6 . . ?
S2A C25A H25A 122.0 . . ?
C24A C25A S2A 116.1(11) . . ?
C24A C25A H25A 122.0 . . ?
O5 C26 C27 115.95(19) . . ?
O6 C26 O5 126.1(2) . . ?
O6 C26 C27 117.89(19) . . ?
C26 C27 S3 121.15(17) . . ?
C26 C27 S3A 121.56(18) . . ?
C28 C27 S3 111.0(4) . . ?
C28 C27 C26 127.8(4) . . ?
C28A C27 S3A 110.2(5) . . ?
C28A C27 C26 127.7(5) . . ?
C27 C28 H28 122.3 . . ?
C27 C28 C29 115.5(8) . . ?
C29 C28 H28 122.3 . . ?
C27 C28A H28A 122.2 . . ?
C27 C28A C29A 115.7(11) . . ?
C29A C28A H28A 122.2 . . ?
C28 C29 H29 125.6 . . ?
C30 C29 C28 108.8(11) . . ?
C30 C29 H29 125.6 . . ?
C28A C29A H29A 125.8 . . ?
C30A C29A C28A 108.4(15) . . ?
C30A C29A H29A 125.8 . . ?
S3 C30 H30 123.1 . . ?
C29 C30 S3 113.9(9) . . ?
C29 C30 H30 123.1 . . ?
S3A C30A H30A 122.9 . . ?
C29A C30A S3A 114.2(13) . . ?
C29A C30A H30A 122.9 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ce1 O1 C16 O2 -5.4(2) . . . . ?
Ce1 O1 C16 C17 175.03(18) . . . . ?
Ce1 O2 C16 O1 5.7(2) . . . . ?
Ce1 O2 C16 C17 -174.72(16) . . . . ?
Ce1 O3 C21 O4 13.7(5) . . . . ?
Ce1 O3 C21 C22 -165.7(2) . . . . ?
Ce1 O4 C21 O3 73.9(3) 3_666 . . . ?
Ce1 O4 C21 C22 -106.7(2) 3_666 . . . ?
Ce1 O5 C26 O6 -5.9(4) . . . . ?
Ce1 O5 C26 C27 171.30(15) . . . . ?
Ce1 N1 C1 C2 175.32(18) . . . . ?
Ce1 N1 C5 C4 -174.93(15) . . . . ?
Ce1 N1 C5 C6 6.7(2) . . . . ?
Ce1 N2 C6 C5 3.7(2) . . . . ?
Ce1 N2 C6 C7 -175.96(15) . . . . ?
Ce1 N2 C10 C9 176.68(16) . . . . ?
Ce1 N2 C10 C11 -5.9(2) . . . . ?
Ce1 N3 C11 C10 25.8(2) . . . . ?
Ce1 N3 C11 C12 -156.12(17) . . . . ?
Ce1 N3 C15 C14 159.5(2) . . . . ?
S1 C17 C18 C19 -0.3(11) . . . . ?
S1A C17 C18A C19A 0(2) . . . . ?
S2 C22 C23 C24 0.0(15) . . . . ?
S2A C22 C23A C24A -3.4(14) . . . . ?
S3 C27 C28 C29 0.0(12) . . . . ?
S3A C27 C28A C29A -3.2(17) . . . . ?
O1 C16 C17 S1 12.5(3) . . . . ?
O1 C16 C17 S1A -165.5(3) . . . . ?
O1 C16 C17 C18 -167.3(6) . . . . ?
O1 C16 C17 C18A 12.8(11) . . . . ?
O2 C16 C17 S1 -167.06(18) . . . . ?
O2 C16 C17 S1A 14.9(4) . . . . ?
O2 C16 C17 C18 13.1(6) . . . . ?
O2 C16 C17 C18A -166.8(11) . . . . ?
O3 C21 C22 S2 6.9(3) . . . . ?
O3 C21 C22 S2A -176.08(18) . . . . ?
O3 C21 C22 C23 -173.1(7) . . . . ?
O3 C21 C22 C23A 2.7(7) . . . . ?
O4 C21 C22 S2 -172.5(2) . . . . ?
O4 C21 C22 S2A 4.5(3) . . . . ?
O4 C21 C22 C23 7.5(7) . . . . ?
O4 C21 C22 C23A -176.7(6) . . . . ?
O5 C26 C27 S3 2.1(3) . . . . ?
O5 C26 C27 S3A -170.1(2) . . . . ?
O5 C26 C27 C28 -174.5(7) . . . . ?
O5 C26 C27 C28A 0.9(9) . . . . ?
O6 C26 C27 S3 179.56(19) . . . . ?
O6 C26 C27 S3A 7.3(3) . . . . ?
O6 C26 C27 C28 2.9(7) . . . . ?
O6 C26 C27 C28A 178.3(9) . . . . ?
N1 C1 C2 C3 0.0(4) . . . . ?
N1 C5 C6 N2 -6.7(3) . . . . ?
N1 C5 C6 C7 173.0(2) . . . . ?
N2 C6 C7 C8 -0.6(3) . . . . ?
N2 C10 C11 N3 -12.7(3) . . . . ?
N2 C10 C11 C12 169.2(2) . . . . ?
N3 C11 C12 C13 -3.5(3) . . . . ?
C1 N1 C5 C4 -0.4(3) . . . . ?
C1 N1 C5 C6 -178.79(18) . . . . ?
C1 C2 C3 C4 -0.8(3) . . . . ?
C2 C3 C4 C5 1.0(3) . . . . ?
C3 C4 C5 N1 -0.4(3) . . . . ?
C3 C4 C5 C6 177.9(2) . . . . ?
C4 C5 C6 N2 174.9(2) . . . . ?
C4 C5 C6 C7 -5.4(3) . . . . ?
C5 N1 C1 C2 0.6(3) . . . . ?
C5 C6 C7 C8 179.73(19) . . . . ?
C6 N2 C10 C9 0.5(3) . . . . ?
C6 N2 C10 C11 177.90(18) . . . . ?
C6 C7 C8 C9 0.4(3) . . . . ?
C7 C8 C9 C10 0.2(3) . . . . ?
C8 C9 C10 N2 -0.7(3) . . . . ?
C8 C9 C10 C11 -178.0(2) . . . . ?
C9 C10 C11 N3 164.7(2) . . . . ?
C9 C10 C11 C12 -13.4(3) . . . . ?
C10 N2 C6 C5 179.80(18) . . . . ?
C10 N2 C6 C7 0.1(3) . . . . ?
C10 C11 C12 C13 174.4(2) . . . . ?
C11 N3 C15 C14 0.1(4) . . . . ?
C11 C12 C13 C14 1.1(4) . . . . ?
C12 C13 C14 C15 1.8(4) . . . . ?
C13 C14 C15 N3 -2.4(4) . . . . ?
C15 N3 C11 C10 -175.1(2) . . . . ?
C15 N3 C11 C12 2.9(3) . . . . ?
C16 C17 C18 C19 179.6(7) . . . . ?
C16 C17 C18A C19A -178.6(13) . . . . ?
C17 S1 C20 C19 0.0(7) . . . . ?
C17 S1A C20A C19A 1.4(19) . . . . ?
C17 C18 C19 C20 0.2(13) . . . . ?
C17 C18A C19A C20A 1(3) . . . . ?
C18 C19 C20 S1 -0.1(11) . . . . ?
C18A C19A C20A S1A -2(3) . . . . ?
C20 S1 C17 C16 -179.7(4) . . . . ?
C20 S1 C17 C18 0.2(6) . . . . ?
C20A S1A C17 C16 177.9(9) . . . . ?
C20A S1A C17 C18A -0.6(14) . . . . ?
C21 C22 C23 C24 179.9(11) . . . . ?
C21 C22 C23A C24A 177.7(11) . . . . ?
C22 S2 C25 C24 -1.8(16) . . . . ?
C22 S2A C25A C24A 1.0(13) . . . . ?
C22 C23 C24 C25 -1(2) . . . . ?
C22 C23A C24A C25A 4.0(19) . . . . ?
C23 C24 C25 S2 2(2) . . . . ?
C23A C24A C25A S2A -2.9(19) . . . . ?
C25 S2 C22 C21 -179.0(8) . . . . ?
C25 S2 C22 C23 1.0(10) . . . . ?
C25A S2A C22 C21 -179.7(6) . . . . ?
C25A S2A C22 C23A 1.4(8) . . . . ?
C26 C27 C28 C29 176.9(7) . . . . ?
C26 C27 C28A C29A -175.1(11) . . . . ?
C27 S3 C30 C29 -2.5(10) . . . . ?
C27 S3A C30A C29A 1.9(13) . . . . ?
C27 C28 C29 C30 -1.8(14) . . . . ?
C27 C28A C29A C30A 5(2) . . . . ?
C28 C29 C30 S3 2.8(14) . . . . ?
C28A C29A C30A S3A -4(2) . . . . ?
C30 S3 C27 C26 -175.8(5) . . . . ?
C30 S3 C27 C28 1.4(8) . . . . ?
C30A S3A C27 C26 173.2(6) . . . . ?
C30A S3A C27 C28A 0.7(9) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'


####################################################################### 
# 
# 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_final_a_CCDC11
_database_code_depnum_ccdc_archive 'CCDC 1544450'
_audit_update_record             
;
2017-04-17 deposited with the CCDC.
2017-08-23 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         'C55 H41 Ho2 N6 O12 S5, C5 H3 O2 S'
_chemical_formula_sum            'C60 H44 Ho2 N6 O14 S6'
_chemical_formula_weight         1595.23

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'
Ho Ho -0.2175 4.6783 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   25.5787(18)
_cell_length_b                   12.0144(8)
_cell_length_c                   40.596(3)
_cell_angle_alpha                90
_cell_angle_beta                 106.380(2)
_cell_angle_gamma                90
_cell_volume                     11969.2(14)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9155
_cell_measurement_theta_min      2.27
_cell_measurement_theta_max      25.38
_exptl_crystal_description       column
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.771
_exptl_crystal_F_000             6304
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.323
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    2.906
_shelx_estimated_absorpt_T_min   0.454
_shelx_estimated_absorpt_T_max   0.801
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.53027
_exptl_absorpt_correction_T_max  0.84842
_exptl_absorpt_process_details   'SADABS V2016/2 (Bruker, 2014)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_monochromator  'multilayer mirrors'
_diffrn_measurement_device       'Bruker D8 Quest/Photon 100'
_diffrn_measurement_method       'profile data from φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            175727
_diffrn_reflns_av_unetI/netI     0.0231
_diffrn_reflns_av_R_equivalents  0.0575
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_theta_min         2.197
_diffrn_reflns_theta_max         25.433
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             11021
_reflns_number_gt                10121
_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.
 
 _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       'APEX2 V2014.9-0 (Bruker, 2014)'
_computing_cell_refinement       'SAINT V8.37A (Bruker, 2005)'
_computing_data_reduction        
; 
SAINT V8.37A, XPREP v2014/2, SADABS V2016/2 (Bruker, 2014) 
;
_computing_structure_solution    'SHELX-2014-5 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELX-2014-7 (Sheldrick, 2015)'
_computing_molecular_graphics    'SHELXLE v817 (Hubschle, 2011)'
_computing_publication_material  'XCIF V2014-2 (Bruker, 2014)'

_refine_special_details          
; 
Structure was phased by direct methods (Sheldrick, 2015).  Systematic 
conditions suggested the ambiguous space group.  The space group choice 
was confirmed by successful convergence of the full-matrix least-squares 
refinement on F².  The final map had no significant features.  A final 
analysis of variance between observed and calculated structure factors 
showed some dependence on amplitude and little dependence on resolution. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0012P)²+10.0000P] 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         11021
_refine_ls_number_parameters     1036
_refine_ls_number_restraints     2233
_refine_ls_R_factor_all          0.0383
_refine_ls_R_factor_gt           0.0328
_refine_ls_wR_factor_ref         0.0491
_refine_ls_wR_factor_gt          0.0486
_refine_ls_goodness_of_fit_ref   1.868
_refine_ls_restrained_S_all      1.779
_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
Ho1 Ho 0.42206(2) 0.38238(2) 0.39010(2) 0.01290(4) Uani 1 1 d . U . . .
Ho2 Ho 0.23153(2) 0.17739(2) 0.35098(2) 0.01443(4) Uani 1 1 d . U . . .
N1 N 0.46067(11) 0.3206(2) 0.45108(7) 0.0207(7) Uani 1 1 d . U . . .
N2 N 0.50767(11) 0.4848(2) 0.42468(7) 0.0212(7) Uani 1 1 d . U . . .
N3 N 0.45676(11) 0.5346(2) 0.35905(8) 0.0221(7) Uani 1 1 d . U . . .
C1 C 0.43838(15) 0.2343(3) 0.46292(9) 0.0266(9) Uani 1 1 d . U . . .
H1 H 0.4048 0.2056 0.4490 0.032 Uiso 1 1 calc R U . . .
C2 C 0.46141(16) 0.1850(4) 0.49408(10) 0.0383(10) Uani 1 1 d . U . . .
H2 H 0.4446 0.1231 0.5015 0.046 Uiso 1 1 calc R U . . .
C3 C 0.50976(17) 0.2280(4) 0.51431(11) 0.0515(13) Uani 1 1 d . U . . .
H3 H 0.5274 0.1948 0.5358 0.062 Uiso 1 1 calc R U . . .
C4 C 0.53219(16) 0.3189(4) 0.50323(10) 0.0477(12) Uani 1 1 d . U . . .
H4 H 0.5647 0.3510 0.5174 0.057 Uiso 1 1 calc R U . . .
C5 C 0.50736(14) 0.3638(3) 0.47136(9) 0.0275(9) Uani 1 1 d . U . . .
C6 C 0.52987(14) 0.4603(3) 0.45769(9) 0.0267(9) Uani 1 1 d . U . . .
C7 C 0.57301(15) 0.5240(4) 0.47808(11) 0.0415(11) Uani 1 1 d . U . . .
H7 H 0.5884 0.5062 0.5016 0.050 Uiso 1 1 calc R U . . .
C8 C 0.59272(16) 0.6118(4) 0.46373(12) 0.0462(11) Uani 1 1 d . U . . .
H8 H 0.6216 0.6559 0.4773 0.055 Uiso 1 1 calc R U . . .
C9 C 0.57038(15) 0.6358(3) 0.42953(12) 0.0400(11) Uani 1 1 d . U . . .
H9 H 0.5836 0.6963 0.4191 0.048 Uiso 1 1 calc R U . . .
C10 C 0.52795(14) 0.5695(3) 0.41046(10) 0.0261(8) Uani 1 1 d . U . . .
C11 C 0.50350(14) 0.5890(3) 0.37353(10) 0.0268(9) Uani 1 1 d . U . . .
C12 C 0.52720(16) 0.6579(3) 0.35412(13) 0.0445(11) Uani 1 1 d . U . . .
H12 H 0.5606 0.6948 0.3647 0.053 Uiso 1 1 calc R U . . .
C13 C 0.50227(17) 0.6723(4) 0.31983(13) 0.0539(13) Uani 1 1 d . U . . .
H13 H 0.5183 0.7188 0.3064 0.065 Uiso 1 1 calc R U . . .
C14 C 0.45384(16) 0.6189(3) 0.30501(12) 0.0431(11) Uani 1 1 d . U . . .
H14 H 0.4354 0.6284 0.2814 0.052 Uiso 1 1 calc R U . . .
C15 C 0.43283(15) 0.5509(3) 0.32552(10) 0.0299(9) Uani 1 1 d . U . . .
H15 H 0.3995 0.5135 0.3153 0.036 Uiso 1 1 calc R U . . .
N4 N 0.27174(11) 0.1264(2) 0.30250(7) 0.0221(7) Uani 1 1 d . U . . .
N5 N 0.19240(11) 0.0075(2) 0.31636(8) 0.0253(7) Uani 1 1 d . U . . .
N6 N 0.19281(11) 0.0255(2) 0.38158(8) 0.0259(7) Uani 1 1 d . U . . .
C41 C 0.31655(14) 0.1753(3) 0.29870(9) 0.0249(8) Uani 1 1 d . U . . .
H41 H 0.3366 0.2235 0.3163 0.030 Uiso 1 1 calc R U . . .
C42 C 0.33503(17) 0.1585(3) 0.27011(10) 0.0345(10) Uani 1 1 d . U . . .
H42 H 0.3676 0.1927 0.2684 0.041 Uiso 1 1 calc R U . . .
C43 C 0.30518(19) 0.0913(4) 0.24433(10) 0.0441(11) Uani 1 1 d . U . . .
H43 H 0.3162 0.0806 0.2241 0.053 Uiso 1 1 calc R U . . .
C44 C 0.25925(18) 0.0395(4) 0.24796(10) 0.0403(11) Uani 1 1 d . U . . .
H44 H 0.2386 -0.0084 0.2305 0.048 Uiso 1 1 calc R U . . .
C45 C 0.24348(15) 0.0579(3) 0.27736(9) 0.0286(9) Uani 1 1 d . U . . .
C46 C 0.19585(15) 0.0018(3) 0.28415(10) 0.0310(9) Uani 1 1 d . U . . .
C47 C 0.15641(18) -0.0545(4) 0.25888(12) 0.0498(12) Uani 1 1 d . U . . .
H47 H 0.1596 -0.0608 0.2362 0.060 Uiso 1 1 calc R U . . .
C48 C 0.11279(19) -0.1010(4) 0.26751(14) 0.0590(14) Uani 1 1 d . U . . .
H48 H 0.0844 -0.1357 0.2503 0.071 Uiso 1 1 calc R U . . .
C49 C 0.11000(17) -0.0975(4) 0.30031(14) 0.0526(13) Uani 1 1 d . U . . .
H49 H 0.0805 -0.1318 0.3064 0.063 Uiso 1 1 calc R U . . .
C50 C 0.15113(15) -0.0428(3) 0.32519(11) 0.0328(9) Uani 1 1 d . U . . .
C51 C 0.15466(14) -0.0430(3) 0.36175(11) 0.0301(9) Uani 1 1 d . U . . .
C52 C 0.12332(16) -0.1128(3) 0.37637(14) 0.0427(11) Uani 1 1 d . U . . .
H52 H 0.0956 -0.1582 0.3621 0.051 Uiso 1 1 calc R U . . .
C53 C 0.13279(18) -0.1152(4) 0.41102(14) 0.0506(12) Uani 1 1 d . U . . .
H53 H 0.1118 -0.1625 0.4211 0.061 Uiso 1 1 calc R U . . .
C54 C 0.17256(17) -0.0496(3) 0.43129(13) 0.0436(11) Uani 1 1 d . U . . .
H54 H 0.1806 -0.0524 0.4556 0.052 Uiso 1 1 calc R U . . .
C55 C 0.20101(15) 0.0214(3) 0.41561(11) 0.0318(9) Uani 1 1 d . U . . .
H55 H 0.2276 0.0694 0.4297 0.038 Uiso 1 1 calc R U . . .
O1 O 0.43900(9) 0.30455(18) 0.33787(6) 0.0203(5) Uani 1 1 d . U . . .
O2 O 0.49987(9) 0.27589(19) 0.38797(6) 0.0214(5) Uani 1 1 d . U . . .
C16 C 0.48210(13) 0.2596(3) 0.35595(9) 0.0180(7) Uani 1 1 d D U . . .
S1 S 0.49837(6) 0.17697(14) 0.29580(4) 0.0381(5) Uani 0.875(4) 1 d D U P A 1
C17 C 0.51257(13) 0.1840(3) 0.33953(9) 0.0252(8) Uani 0.875(4) 1 d D U P A 1
C18 C 0.5510(3) 0.1077(8) 0.3555(2) 0.0366(15) Uani 0.875(4) 1 d D U P A 1
H18 H 0.5635 0.0989 0.3797 0.044 Uiso 0.875(4) 1 calc R U P A 1
C19 C 0.5701(3) 0.0432(6) 0.33207(17) 0.0472(15) Uani 0.875(4) 1 d D U P A 1
H19 H 0.5969 -0.0135 0.3387 0.057 Uiso 0.875(4) 1 calc R U P A 1
C20 C 0.5458(3) 0.0718(5) 0.29919(16) 0.0482(14) Uani 0.875(4) 1 d D U P A 1
H20 H 0.5539 0.0381 0.2800 0.058 Uiso 0.875(4) 1 calc R U P A 1
S1B S 0.5622(6) 0.0982(15) 0.3619(4) 0.036(2) Uani 0.125(4) 1 d D U P A 2
C17B C 0.51257(13) 0.1840(3) 0.33953(9) 0.0252(8) Uani 0.125(4) 1 d D U P A 2
C18B C 0.5075(17) 0.186(4) 0.3051(4) 0.034(3) Uani 0.125(4) 1 d D U P A 2
H18B H 0.4841 0.2357 0.2894 0.041 Uiso 0.125(4) 1 calc R U P A 2
C19B C 0.5412(18) 0.106(4) 0.2956(5) 0.041(3) Uani 0.125(4) 1 d D U P A 2
H19B H 0.5409 0.0903 0.2726 0.050 Uiso 0.125(4) 1 calc R U P A 2
C20B C 0.574(2) 0.055(4) 0.3236(6) 0.041(3) Uani 0.125(4) 1 d D U P A 2
H20B H 0.6006 0.0018 0.3225 0.049 Uiso 0.125(4) 1 calc R U P A 2
O3 O 0.39589(9) 0.54520(18) 0.41738(6) 0.0190(5) Uani 1 1 d . U . . .
O4 O 0.34813(8) 0.39320(18) 0.41882(6) 0.0182(5) Uani 1 1 d . U . . .
C21 C 0.35704(12) 0.4963(3) 0.42482(8) 0.0165(7) Uani 1 1 d D U . . .
S2 S 0.3236(2) 0.6976(3) 0.44221(14) 0.0290(8) Uani 0.551(4) 1 d D U P B 1
C22 C 0.32127(13) 0.5599(3) 0.44067(8) 0.0212(7) Uani 0.551(4) 1 d D U P B 1
C23 C 0.2762(7) 0.5195(12) 0.4514(4) 0.029(2) Uani 0.551(4) 1 d D U P B 1
H23 H 0.2630 0.4453 0.4502 0.035 Uiso 0.551(4) 1 calc R U P B 1
C24 C 0.2531(5) 0.6248(8) 0.4656(3) 0.031(2) Uani 0.551(4) 1 d D U P B 1
H24 H 0.2254 0.6246 0.4770 0.037 Uiso 0.551(4) 1 calc R U P B 1
C25 C 0.2794(5) 0.7156(10) 0.4588(4) 0.030(2) Uani 0.551(4) 1 d D U P B 1
H25 H 0.2699 0.7883 0.4644 0.036 Uiso 0.551(4) 1 calc R U P B 1
S2B S 0.2780(2) 0.4971(4) 0.45811(12) 0.0285(9) Uani 0.449(4) 1 d D U P B 2
C22B C 0.32127(13) 0.5599(3) 0.44067(8) 0.0212(7) Uani 0.449(4) 1 d D U P B 2
C23B C 0.3203(9) 0.6776(13) 0.4459(6) 0.026(2) Uani 0.449(4) 1 d D U P B 2
H23B H 0.3424 0.7323 0.4395 0.032 Uiso 0.449(4) 1 calc R U P B 2
C24B C 0.2743(6) 0.6974(11) 0.4646(4) 0.024(2) Uani 0.449(4) 1 d D U P B 2
H24B H 0.2612 0.7672 0.4698 0.029 Uiso 0.449(4) 1 calc R U P B 2
C25B C 0.2574(6) 0.5959(9) 0.4717(4) 0.026(2) Uani 0.449(4) 1 d D U P B 2
H25B H 0.2327 0.5886 0.4852 0.031 Uiso 0.449(4) 1 calc R U P B 2
O5 O 0.38484(9) 0.20724(17) 0.38578(5) 0.0167(5) Uani 1 1 d . U . . .
O6 O 0.31324(9) 0.09181(18) 0.37511(6) 0.0195(5) Uani 1 1 d . U . . .
C26 C 0.36376(13) 0.1120(3) 0.38397(8) 0.0147(7) Uani 1 1 d D U . . .
S3 S 0.37292(5) -0.11539(10) 0.39139(6) 0.0209(4) Uani 0.818(4) 1 d D U P C 1
C27 C 0.40006(12) 0.0143(2) 0.39234(8) 0.0151(7) Uani 0.818(4) 1 d D U P C 1
C28 C 0.4550(3) 0.0107(7) 0.3985(3) 0.0230(15) Uani 0.818(4) 1 d D U P C 1
H28 H 0.4770 0.0753 0.3999 0.028 Uiso 0.818(4) 1 calc R U P C 1
C29 C 0.4765(2) -0.0987(4) 0.4025(3) 0.0248(11) Uani 0.818(4) 1 d D U P C 1
H29 H 0.5142 -0.1159 0.4076 0.030 Uiso 0.818(4) 1 calc R U P C 1
C30 C 0.4359(2) -0.1768(5) 0.3982(2) 0.0229(13) Uani 0.818(4) 1 d D U P C 1
H30 H 0.4418 -0.2550 0.3988 0.027 Uiso 0.818(4) 1 calc R U P C 1
S3B S 0.4690(3) 0.0226(8) 0.4023(3) 0.0201(16) Uani 0.182(4) 1 d D U P C 2
C27B C 0.40006(12) 0.0143(2) 0.39234(8) 0.0151(7) Uani 0.182(4) 1 d D U P C 2
C28B C 0.3818(8) -0.0922(12) 0.3909(11) 0.020(3) Uani 0.182(4) 1 d D U P C 2
H28B H 0.3442 -0.1117 0.3847 0.024 Uiso 0.182(4) 1 calc R U P C 2
C29B C 0.4246(9) -0.1712(13) 0.3998(12) 0.022(3) Uani 0.182(4) 1 d D U P C 2
H29B H 0.4202 -0.2478 0.4042 0.026 Uiso 0.182(4) 1 calc R U P C 2
C30B C 0.4736(8) -0.1207(11) 0.4012(14) 0.022(3) Uani 0.182(4) 1 d D U P C 2
H30B H 0.5059 -0.1600 0.4014 0.026 Uiso 0.182(4) 1 calc R U P C 2
O7 O 0.34585(8) 0.43084(18) 0.34695(5) 0.0164(5) Uani 1 1 d . U . . .
O8 O 0.26887(9) 0.33975(18) 0.34412(6) 0.0176(5) Uani 1 1 d . U . . .
C31 C 0.29630(13) 0.4270(3) 0.34637(8) 0.0138(7) Uani 1 1 d D U . . .
S4 S 0.29949(6) 0.65693(12) 0.34537(6) 0.0245(4) Uani 0.773(4) 1 d D U P D 1
C32 C 0.26855(12) 0.5334(2) 0.34798(9) 0.0187(7) Uani 0.773(4) 1 d D U P D 1
C33 C 0.2186(3) 0.5480(7) 0.3549(2) 0.0257(16) Uani 0.773(4) 1 d D U P D 1
H33 H 0.1975 0.4905 0.3609 0.031 Uiso 0.773(4) 1 calc R U P D 1
C34 C 0.2039(3) 0.6663(5) 0.35155(15) 0.0324(15) Uani 0.773(4) 1 d D U P D 1
H34 H 0.1693 0.6945 0.3516 0.039 Uiso 0.773(4) 1 calc R U P D 1
C35 C 0.2458(3) 0.7303(5) 0.3484(2) 0.0326(17) Uani 0.773(4) 1 d D U P D 1
H35 H 0.2447 0.8093 0.3479 0.039 Uiso 0.773(4) 1 calc R U P D 1
S4B S 0.2035(2) 0.5305(6) 0.3491(2) 0.0260(15) Uani 0.227(4) 1 d D U P D 2
C32B C 0.26855(12) 0.5334(2) 0.34798(9) 0.0187(7) Uani 0.227(4) 1 d D U P D 2
C33B C 0.2866(9) 0.6429(12) 0.3467(9) 0.025(2) Uani 0.227(4) 1 d D U P D 2
H33B H 0.3184 0.6645 0.3407 0.030 Uiso 0.227(4) 1 calc R U P D 2
C34B C 0.2479(10) 0.7194(12) 0.3562(8) 0.029(3) Uani 0.227(4) 1 d D U P D 2
H34B H 0.2510 0.7982 0.3570 0.035 Uiso 0.227(4) 1 calc R U P D 2
C35B C 0.2072(8) 0.6607(13) 0.3636(6) 0.029(2) Uani 0.227(4) 1 d D U P D 2
H35B H 0.1836 0.6906 0.3757 0.035 Uiso 0.227(4) 1 calc R U P D 2
O9 O 0.17348(9) 0.23083(19) 0.29902(6) 0.0206(5) Uani 1 1 d . U . . .
O10 O 0.09664(9) 0.3158(2) 0.30008(6) 0.0255(6) Uani 1 1 d . U . . .
C36 C 0.13159(14) 0.2885(3) 0.28565(8) 0.0181(7) Uani 1 1 d D U . . .
S5 S 0.07075(9) 0.4032(2) 0.22874(5) 0.0285(6) Uani 0.673(4) 1 d D U P E 1
C37 C 0.12460(14) 0.3272(3) 0.25015(8) 0.0252(8) Uani 0.673(4) 1 d D U P E 1
C38 C 0.1593(5) 0.3144(12) 0.2299(4) 0.0282(19) Uani 0.673(4) 1 d D U P E 1
H38 H 0.1936 0.2780 0.2367 0.034 Uiso 0.673(4) 1 calc R U P E 1
C39 C 0.1349(3) 0.3660(9) 0.1959(2) 0.0421(18) Uani 0.673(4) 1 d D U P E 1
H39 H 0.1506 0.3647 0.1773 0.050 Uiso 0.673(4) 1 calc R U P E 1
C40 C 0.0876(4) 0.4146(10) 0.1952(2) 0.0440(19) Uani 0.673(4) 1 d D U P E 1
H40 H 0.0660 0.4532 0.1756 0.053 Uiso 0.673(4) 1 calc R U P E 1
S5B S 0.1703(3) 0.2959(7) 0.2304(2) 0.0380(14) Uani 0.327(4) 1 d D U P E 2
C37B C 0.12460(14) 0.3272(3) 0.25015(8) 0.0252(8) Uani 0.327(4) 1 d D U P E 2
C38B C 0.0840(7) 0.3891(18) 0.2266(4) 0.029(2) Uani 0.327(4) 1 d D U P E 2
H38B H 0.0501 0.4112 0.2298 0.034 Uiso 0.327(4) 1 calc R U P E 2
C39B C 0.1035(6) 0.415(2) 0.1952(4) 0.028(2) Uani 0.327(4) 1 d D U P E 2
H39B H 0.0840 0.4575 0.1759 0.034 Uiso 0.327(4) 1 calc R U P E 2
C40B C 0.1524(6) 0.3686(18) 0.1991(4) 0.030(2) Uani 0.327(4) 1 d D U P E 2
H40B H 0.1736 0.3803 0.1836 0.036 Uiso 0.327(4) 1 calc R U P E 2
O11 O 0.15511(9) 0.2570(2) 0.36217(6) 0.0206(6) Uani 1 1 d D U . . .
H11A H 0.1326(12) 0.281(3) 0.3440(7) 0.031 Uiso 1 1 d D U . . .
H11B H 0.1492(14) 0.292(3) 0.3789(7) 0.031 Uiso 1 1 d D U . . .
O12 O 0.26131(10) 0.2424(2) 0.40803(6) 0.0233(6) Uani 1 1 d D U . . .
H12A H 0.2401(13) 0.258(3) 0.4198(8) 0.035 Uiso 1 1 d D U . . .
H12B H 0.2862(12) 0.291(2) 0.4131(9) 0.035 Uiso 1 1 d D U . . .
O13 O 0.13165(11) 0.3769(2) 0.41097(7) 0.0368(7) Uani 1 1 d . U . . .
O14 O 0.19755(11) 0.2788(2) 0.44745(6) 0.0354(7) Uani 1 1 d . U . . .
C56 C 0.16138(16) 0.3528(3) 0.44052(10) 0.0305(9) Uani 1 1 d D U . . .
S6 S 0.11099(8) 0.52717(15) 0.46402(4) 0.0382(5) Uani 0.839(4) 1 d D U P F 1
C57 C 0.1541(2) 0.4146(4) 0.47096(11) 0.0248(11) Uani 0.839(4) 1 d D U P F 1
C58 C 0.1834(4) 0.3833(7) 0.5072(3) 0.0325(17) Uani 0.839(4) 1 d D U P F 1
H58 H 0.2078 0.3237 0.5159 0.039 Uiso 0.839(4) 1 calc R U P F 1
C59 C 0.1622(2) 0.4759(5) 0.52624(13) 0.0375(13) Uani 0.839(4) 1 d D U P F 1
H59 H 0.1740 0.4809 0.5506 0.045 Uiso 0.839(4) 1 calc R U P F 1
C60 C 0.1260(2) 0.5505(5) 0.50712(13) 0.0397(13) Uani 0.839(4) 1 d D U P F 1
H60 H 0.1107 0.6097 0.5168 0.048 Uiso 0.839(4) 1 calc R U P F 1
S6B S 0.1753(7) 0.4124(11) 0.5035(4) 0.044(2) Uani 0.161(4) 1 d D U P F 2
C57B C 0.1434(13) 0.440(2) 0.4613(4) 0.036(3) Uani 0.161(4) 1 d D U P F 2
C58B C 0.1071(17) 0.543(3) 0.4541(5) 0.036(3) Uani 0.161(4) 1 d D U P F 2
H58B H 0.0855 0.5732 0.4329 0.044 Uiso 0.161(4) 1 calc R U P F 2
C59B C 0.1157(11) 0.5851(18) 0.4913(5) 0.043(3) Uani 0.161(4) 1 d D U P F 2
H59B H 0.0972 0.6495 0.4957 0.051 Uiso 0.161(4) 1 calc R U P F 2
C60B C 0.1500(13) 0.528(2) 0.5174(5) 0.043(3) Uani 0.161(4) 1 d D U P F 2
H60B H 0.1588 0.5506 0.5408 0.051 Uiso 0.161(4) 1 calc R U P F 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

_exptl_special_details           
; 
One distinct cell was identified using APEX2 (Bruker, 2014).  Eight 
frame series were integrated and filtered for statistical outliers 
using SAINT (Bruker, 2014) then corrected for absorption by integration 
using SAINT/SADABS v2014/2 (Bruker, 2014) to sort, merge, and scale 
the combined data.  No decay correction was applied.    
;

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1.00 0.00 -1.00 0.0320
-1.00 0.00 1.00 0.0400
2.00 1.00 -2.00 0.0490
-2.00 -1.00 2.00 0.0310
1.00 0.00 3.00 0.1340
-1.00 0.00 -3.00 0.1550
1.00 3.00 0.00 0.0450
-1.00 -3.00 0.00 0.0300
2.00 -2.00 -3.00 0.0310
-2.00 2.00 3.00 0.0330

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
Ho1 O5 2.296(2) . ?
Ho1 O7 2.298(2) . ?
Ho1 O2 2.388(2) . ?
Ho1 O3 2.433(2) . ?
Ho1 O1 2.465(2) . ?
Ho1 O4 2.489(2) . ?
Ho1 N1 2.505(3) . ?
Ho1 N3 2.520(3) . ?
Ho1 N2 2.558(3) . ?
Ho1 C16 2.767(3) . ?
Ho1 C21 2.819(3) . ?
Ho2 O8 2.224(2) . ?
Ho2 O6 2.287(2) . ?
Ho2 O9 2.302(2) . ?
Ho2 O11 2.333(2) . ?
Ho2 O12 2.358(2) . ?
Ho2 N5 2.520(3) . ?
Ho2 N4 2.539(3) . ?
Ho2 N6 2.559(3) . ?
N1 C1 1.336(4) . ?
N1 C5 1.349(4) . ?
N2 C6 1.333(4) . ?
N2 C10 1.344(4) . ?
N3 C15 1.340(4) . ?
N3 C11 1.344(4) . ?
C1 C2 1.370(5) . ?
C1 H1 0.9500 . ?
C2 C3 1.378(6) . ?
C2 H2 0.9500 . ?
C3 C4 1.367(6) . ?
C3 H3 0.9500 . ?
C4 C5 1.380(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.472(5) . ?
C6 C7 1.404(5) . ?
C7 C8 1.368(6) . ?
C7 H7 0.9500 . ?
C8 C9 1.375(6) . ?
C8 H8 0.9500 . ?
C9 C10 1.392(5) . ?
C9 H9 0.9500 . ?
C10 C11 1.471(5) . ?
C11 C12 1.394(5) . ?
C12 C13 1.369(6) . ?
C12 H12 0.9500 . ?
C13 C14 1.374(6) . ?
C13 H13 0.9500 . ?
C14 C15 1.379(5) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
N4 C41 1.335(4) . ?
N4 C45 1.351(4) . ?
N5 C46 1.337(5) . ?
N5 C50 1.350(5) . ?
N6 C55 1.339(5) . ?
N6 C51 1.354(4) . ?
C41 C42 1.386(5) . ?
C41 H41 0.9500 . ?
C42 C43 1.371(6) . ?
C42 H42 0.9500 . ?
C43 C44 1.374(6) . ?
C43 H43 0.9500 . ?
C44 C45 1.382(5) . ?
C44 H44 0.9500 . ?
C45 C46 1.484(5) . ?
C46 C47 1.395(5) . ?
C47 C48 1.378(7) . ?
C47 H47 0.9500 . ?
C48 C49 1.354(7) . ?
C48 H48 0.9500 . ?
C49 C50 1.400(5) . ?
C49 H49 0.9500 . ?
C50 C51 1.461(6) . ?
C51 C52 1.403(5) . ?
C52 C53 1.359(6) . ?
C52 H52 0.9500 . ?
C53 C54 1.365(6) . ?
C53 H53 0.9500 . ?
C54 C55 1.387(5) . ?
C54 H54 0.9500 . ?
C55 H55 0.9500 . ?
O1 C16 1.261(4) . ?
O2 C16 1.265(4) . ?
C16 C17B 1.473(4) . ?
C16 C17 1.473(4) . ?
S1 C17 1.711(4) . ?
S1 C20 1.731(5) . ?
C17 C18 1.366(8) . ?
C18 C19 1.416(9) . ?
C18 H18 0.9500 . ?
C19 C20 1.348(7) . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?
S1B C17B 1.687(9) . ?
S1B C20B 1.743(11) . ?
C17B C18B 1.367(13) . ?
C18B C19B 1.416(14) . ?
C18B H18B 0.9500 . ?
C19B C20B 1.351(11) . ?
C19B H19B 0.9500 . ?
C20B H20B 0.9500 . ?
O3 C21 1.262(4) . ?
O4 C21 1.270(4) . ?
C21 C22B 1.472(4) . ?
C21 C22 1.472(4) . ?
S2 C25 1.486(10) . ?
S2 C22 1.656(4) . ?
C22 C23 1.428(14) . ?
C23 C24 1.572(16) . ?
C23 H23 0.9500 . ?
C24 C25 1.349(8) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
S2B C25B 1.468(11) . ?
S2B C22B 1.654(5) . ?
C22B C23B 1.432(15) . ?
C23B C24B 1.589(17) . ?
C23B H23B 0.9500 . ?
C24B C25B 1.352(8) . ?
C24B H24B 0.9500 . ?
C25B H25B 0.9500 . ?
O5 C26 1.258(4) . ?
O6 C26 1.263(4) . ?
C26 C27B 1.476(4) . ?
C26 C27 1.476(4) . ?
S3 C27 1.702(3) . ?
S3 C30 1.722(5) . ?
C27 C28 1.358(8) . ?
C28 C29 1.416(9) . ?
C28 H28 0.9500 . ?
C29 C30 1.375(6) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?
S3B C27B 1.698(7) . ?
S3B C30B 1.727(11) . ?
C27B C28B 1.358(12) . ?
C28B C29B 1.417(14) . ?
C28B H28B 0.9500 . ?
C29B C30B 1.379(10) . ?
C29B H29B 0.9500 . ?
C30B H30B 0.9500 . ?
O7 C31 1.262(4) . ?
O8 C31 1.250(4) . ?
C31 C32B 1.473(4) . ?
C31 C32 1.473(4) . ?
S4 C35 1.664(7) . ?
S4 C32 1.699(3) . ?
C32 C33 1.394(9) . ?
C33 C34 1.466(10) . ?
C33 H33 0.9500 . ?
C34 C35 1.354(6) . ?
C34 H34 0.9500 . ?
C35 H35 0.9500 . ?
S4B C35B 1.665(12) . ?
S4B C32B 1.678(6) . ?
C32B C33B 1.400(12) . ?
C33B C34B 1.480(14) . ?
C33B H33B 0.9500 . ?
C34B C35B 1.358(10) . ?
C34B H34B 0.9500 . ?
C35B H35B 0.9500 . ?
O9 C36 1.263(4) . ?
O10 C36 1.243(4) . ?
C36 C37B 1.476(4) . ?
C36 C37 1.476(4) . ?
S5 C40 1.547(9) . ?
S5 C37 1.676(4) . ?
C37 C38 1.377(12) . ?
C38 C39 1.482(13) . ?
C38 H38 0.9500 . ?
C39 C40 1.336(8) . ?
C39 H39 0.9500 . ?
C40 H40 0.9500 . ?
S5B C40B 1.502(12) . ?
S5B C37B 1.638(6) . ?
C37B C38B 1.409(14) . ?
C38B C39B 1.527(15) . ?
C38B H38B 0.9500 . ?
C39B C40B 1.336(10) . ?
C39B H39B 0.9500 . ?
C40B H40B 0.9500 . ?
O11 H11A 0.850(18) . ?
O11 H11B 0.847(18) . ?
O12 H12A 0.839(18) . ?
O12 H12B 0.843(19) . ?
O13 C56 1.259(5) . ?
O14 C56 1.257(5) . ?
C56 C57 1.497(5) . ?
C56 C57B 1.498(7) . ?
S6 C60 1.705(5) . ?
S6 C57 1.718(5) . ?
C57 C58 1.500(10) . ?
C58 C59 1.537(10) . ?
C58 H58 0.9500 . ?
C59 C60 1.363(7) . ?
C59 H59 0.9500 . ?
C60 H60 0.9500 . ?
S6B C60B 1.697(10) . ?
S6B C57B 1.711(10) . ?
C57B C58B 1.526(14) . ?
C58B C59B 1.546(13) . ?
C58B H58B 0.9500 . ?
C59B C60B 1.355(12) . ?
C59B H59B 0.9500 . ?
C60B H60B 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
O5 Ho1 O7 85.96(8) . . ?
O5 Ho1 O2 80.68(8) . . ?
O7 Ho1 O2 130.13(8) . . ?
O5 Ho1 O3 127.61(8) . . ?
O7 Ho1 O3 81.96(7) . . ?
O2 Ho1 O3 141.85(7) . . ?
O5 Ho1 O1 75.90(8) . . ?
O7 Ho1 O1 75.97(7) . . ?
O2 Ho1 O1 54.20(8) . . ?
O3 Ho1 O1 146.53(7) . . ?
O5 Ho1 O4 74.35(7) . . ?
O7 Ho1 O4 75.56(7) . . ?
O2 Ho1 O4 142.75(8) . . ?
O3 Ho1 O4 53.27(7) . . ?
O1 Ho1 O4 139.81(7) . . ?
O5 Ho1 N1 80.98(8) . . ?
O7 Ho1 N1 147.30(8) . . ?
O2 Ho1 N1 77.10(8) . . ?
O3 Ho1 N1 82.58(8) . . ?
O1 Ho1 N1 128.44(8) . . ?
O4 Ho1 N1 72.08(8) . . ?
O5 Ho1 N3 145.46(9) . . ?
O7 Ho1 N3 77.15(8) . . ?
O2 Ho1 N3 87.47(8) . . ?
O3 Ho1 N3 79.94(8) . . ?
O1 Ho1 N3 70.90(8) . . ?
O4 Ho1 N3 128.15(8) . . ?
N1 Ho1 N3 127.81(9) . . ?
O5 Ho1 N2 139.02(8) . . ?
O7 Ho1 N2 135.01(9) . . ?
O2 Ho1 N2 71.59(8) . . ?
O3 Ho1 N2 70.52(8) . . ?
O1 Ho1 N2 108.87(8) . . ?
O4 Ho1 N2 111.32(8) . . ?
N1 Ho1 N2 64.05(9) . . ?
N3 Ho1 N2 63.76(9) . . ?
O5 Ho1 C16 75.51(9) . . ?
O7 Ho1 C16 102.98(9) . . ?
O2 Ho1 C16 27.16(9) . . ?
O3 Ho1 C16 156.86(8) . . ?
O1 Ho1 C16 27.11(8) . . ?
O4 Ho1 C16 149.85(8) . . ?
N1 Ho1 C16 102.54(10) . . ?
N3 Ho1 C16 79.21(9) . . ?
N2 Ho1 C16 91.21(9) . . ?
O5 Ho1 C21 101.11(9) . . ?
O7 Ho1 C21 76.41(8) . . ?
O2 Ho1 C21 153.30(9) . . ?
O3 Ho1 C21 26.53(8) . . ?
O1 Ho1 C21 152.36(8) . . ?
O4 Ho1 C21 26.78(8) . . ?
N1 Ho1 C21 76.91(9) . . ?
N3 Ho1 C21 103.80(9) . . ?
N2 Ho1 C21 91.52(9) . . ?
C16 Ho1 C21 176.62(10) . . ?
O8 Ho2 O6 94.31(8) . . ?
O8 Ho2 O9 80.18(8) . . ?
O6 Ho2 O9 142.50(8) . . ?
O8 Ho2 O11 94.46(8) . . ?
O6 Ho2 O11 144.64(8) . . ?
O9 Ho2 O11 72.83(8) . . ?
O8 Ho2 O12 78.54(8) . . ?
O6 Ho2 O12 74.04(8) . . ?
O9 Ho2 O12 138.92(8) . . ?
O11 Ho2 O12 74.29(8) . . ?
O8 Ho2 N5 139.27(9) . . ?
O6 Ho2 N5 92.64(8) . . ?
O9 Ho2 N5 70.29(9) . . ?
O11 Ho2 N5 102.58(9) . . ?
O12 Ho2 N5 141.59(9) . . ?
O8 Ho2 N4 80.35(9) . . ?
O6 Ho2 N4 72.70(8) . . ?
O9 Ho2 N4 69.80(8) . . ?
O11 Ho2 N4 142.61(8) . . ?
O12 Ho2 N4 138.76(8) . . ?
N5 Ho2 N4 63.66(10) . . ?
O8 Ho2 N6 157.68(9) . . ?
O6 Ho2 N6 84.46(8) . . ?
O9 Ho2 N6 113.93(9) . . ?
O11 Ho2 N6 74.78(9) . . ?
O12 Ho2 N6 79.72(9) . . ?
N5 Ho2 N6 62.98(10) . . ?
N4 Ho2 N6 120.07(9) . . ?
C1 N1 C5 118.2(3) . . ?
C1 N1 Ho1 119.7(2) . . ?
C5 N1 Ho1 121.6(2) . . ?
C6 N2 C10 119.5(3) . . ?
C6 N2 Ho1 120.1(2) . . ?
C10 N2 Ho1 120.2(2) . . ?
C15 N3 C11 117.9(3) . . ?
C15 N3 Ho1 119.3(2) . . ?
C11 N3 Ho1 122.0(2) . . ?
N1 C1 C2 123.5(4) . . ?
N1 C1 H1 118.3 . . ?
C2 C1 H1 118.3 . . ?
C1 C2 C3 117.9(4) . . ?
C1 C2 H2 121.1 . . ?
C3 C2 H2 121.1 . . ?
C4 C3 C2 119.6(4) . . ?
C4 C3 H3 120.2 . . ?
C2 C3 H3 120.2 . . ?
C3 C4 C5 119.7(4) . . ?
C3 C4 H4 120.2 . . ?
C5 C4 H4 120.2 . . ?
N1 C5 C4 121.1(4) . . ?
N1 C5 C6 116.5(3) . . ?
C4 C5 C6 122.4(4) . . ?
N2 C6 C7 120.9(4) . . ?
N2 C6 C5 116.9(3) . . ?
C7 C6 C5 122.2(4) . . ?
C8 C7 C6 119.4(4) . . ?
C8 C7 H7 120.3 . . ?
C6 C7 H7 120.3 . . ?
C7 C8 C9 119.6(4) . . ?
C7 C8 H8 120.2 . . ?
C9 C8 H8 120.2 . . ?
C8 C9 C10 118.6(4) . . ?
C8 C9 H9 120.7 . . ?
C10 C9 H9 120.7 . . ?
N2 C10 C9 121.9(4) . . ?
N2 C10 C11 117.0(3) . . ?
C9 C10 C11 121.1(4) . . ?
N3 C11 C12 121.1(4) . . ?
N3 C11 C10 116.0(3) . . ?
C12 C11 C10 122.9(4) . . ?
C13 C12 C11 119.9(4) . . ?
C13 C12 H12 120.1 . . ?
C11 C12 H12 120.1 . . ?
C12 C13 C14 119.3(4) . . ?
C12 C13 H13 120.3 . . ?
C14 C13 H13 120.3 . . ?
C13 C14 C15 118.0(4) . . ?
C13 C14 H14 121.0 . . ?
C15 C14 H14 121.0 . . ?
N3 C15 C14 123.8(4) . . ?
N3 C15 H15 118.1 . . ?
C14 C15 H15 118.1 . . ?
C41 N4 C45 118.3(3) . . ?
C41 N4 Ho2 122.2(2) . . ?
C45 N4 Ho2 119.0(2) . . ?
C46 N5 C50 120.6(3) . . ?
C46 N5 Ho2 117.5(2) . . ?
C50 N5 Ho2 115.6(2) . . ?
C55 N6 C51 117.9(3) . . ?
C55 N6 Ho2 123.9(2) . . ?
C51 N6 Ho2 117.2(3) . . ?
N4 C41 C42 122.7(4) . . ?
N4 C41 H41 118.7 . . ?
C42 C41 H41 118.7 . . ?
C43 C42 C41 118.5(4) . . ?
C43 C42 H42 120.8 . . ?
C41 C42 H42 120.8 . . ?
C42 C43 C44 119.6(4) . . ?
C42 C43 H43 120.2 . . ?
C44 C43 H43 120.2 . . ?
C43 C44 C45 119.1(4) . . ?
C43 C44 H44 120.4 . . ?
C45 C44 H44 120.4 . . ?
N4 C45 C44 121.7(4) . . ?
N4 C45 C46 115.4(3) . . ?
C44 C45 C46 122.9(4) . . ?
N5 C46 C47 120.7(4) . . ?
N5 C46 C45 116.3(3) . . ?
C47 C46 C45 123.0(4) . . ?
C48 C47 C46 118.6(5) . . ?
C48 C47 H47 120.7 . . ?
C46 C47 H47 120.7 . . ?
C49 C48 C47 120.6(4) . . ?
C49 C48 H48 119.7 . . ?
C47 C48 H48 119.7 . . ?
C48 C49 C50 119.1(5) . . ?
C48 C49 H49 120.4 . . ?
C50 C49 H49 120.4 . . ?
N5 C50 C49 120.2(4) . . ?
N5 C50 C51 116.2(3) . . ?
C49 C50 C51 123.4(4) . . ?
N6 C51 C52 120.9(4) . . ?
N6 C51 C50 115.5(3) . . ?
C52 C51 C50 123.5(4) . . ?
C53 C52 C51 119.6(4) . . ?
C53 C52 H52 120.2 . . ?
C51 C52 H52 120.2 . . ?
C52 C53 C54 119.8(4) . . ?
C52 C53 H53 120.1 . . ?
C54 C53 H53 120.1 . . ?
C53 C54 C55 118.5(4) . . ?
C53 C54 H54 120.7 . . ?
C55 C54 H54 120.7 . . ?
N6 C55 C54 123.1(4) . . ?
N6 C55 H55 118.4 . . ?
C54 C55 H55 118.4 . . ?
C16 O1 Ho1 89.92(19) . . ?
C16 O2 Ho1 93.36(18) . . ?
O1 C16 O2 122.2(3) . . ?
O1 C16 C17B 119.2(3) . . ?
O2 C16 C17B 118.5(3) . . ?
O1 C16 C17 119.2(3) . . ?
O2 C16 C17 118.5(3) . . ?
O1 C16 Ho1 62.97(16) . . ?
O2 C16 Ho1 59.48(16) . . ?
C17B C16 Ho1 174.1(2) . . ?
C17 C16 Ho1 174.1(2) . . ?
C17 S1 C20 90.8(2) . . ?
C18 C17 C16 126.9(5) . . ?
C18 C17 S1 111.9(4) . . ?
C16 C17 S1 121.0(3) . . ?
C17 C18 C19 112.8(7) . . ?
C17 C18 H18 123.6 . . ?
C19 C18 H18 123.6 . . ?
C20 C19 C18 112.0(6) . . ?
C20 C19 H19 124.0 . . ?
C18 C19 H19 124.0 . . ?
C19 C20 S1 112.4(4) . . ?
C19 C20 H20 123.8 . . ?
S1 C20 H20 123.8 . . ?
C17B S1B C20B 89.5(7) . . ?
C18B C17B C16 122.8(11) . . ?
C18B C17B S1B 113.7(9) . . ?
C16 C17B S1B 123.1(6) . . ?
C17B C18B C19B 112.1(12) . . ?
C17B C18B H18B 123.9 . . ?
C19B C18B H18B 123.9 . . ?
C20B C19B C18B 110.9(12) . . ?
C20B C19B H19B 124.6 . . ?
C18B C19B H19B 124.6 . . ?
C19B C20B S1B 113.4(11) . . ?
C19B C20B H20B 123.3 . . ?
S1B C20B H20B 123.3 . . ?
C21 O3 Ho1 94.07(18) . . ?
C21 O4 Ho1 91.25(18) . . ?
O3 C21 O4 121.2(3) . . ?
O3 C21 C22B 119.4(3) . . ?
O4 C21 C22B 119.3(3) . . ?
O3 C21 C22 119.4(3) . . ?
O4 C21 C22 119.3(3) . . ?
O3 C21 Ho1 59.41(15) . . ?
O4 C21 Ho1 61.97(15) . . ?
C22B C21 Ho1 176.0(2) . . ?
C22 C21 Ho1 176.0(2) . . ?
C25 S2 C22 98.0(5) . . ?
C23 C22 C21 127.8(7) . . ?
C23 C22 S2 110.5(6) . . ?
C21 C22 S2 121.0(3) . . ?
C22 C23 C24 104.9(9) . . ?
C22 C23 H23 127.6 . . ?
C24 C23 H23 127.6 . . ?
C25 C24 C23 108.5(11) . . ?
C25 C24 H24 125.8 . . ?
C23 C24 H24 125.8 . . ?
C24 C25 S2 117.4(11) . . ?
C24 C25 H25 121.3 . . ?
S2 C25 H25 121.3 . . ?
C25B S2B C22B 98.5(5) . . ?
C23B C22B C21 128.0(7) . . ?
C23B C22B S2B 110.2(6) . . ?
C21 C22B S2B 121.6(3) . . ?
C22B C23B C24B 105.3(10) . . ?
C22B C23B H23B 127.3 . . ?
C24B C23B H23B 127.3 . . ?
C25B C24B C23B 107.0(12) . . ?
C25B C24B H24B 126.5 . . ?
C23B C24B H24B 126.5 . . ?
C24B C25B S2B 118.6(12) . . ?
C24B C25B H25B 120.7 . . ?
S2B C25B H25B 120.7 . . ?
C26 O5 Ho1 178.5(2) . . ?
C26 O6 Ho2 140.6(2) . . ?
O5 C26 O6 125.4(3) . . ?
O5 C26 C27B 118.6(3) . . ?
O6 C26 C27B 116.1(3) . . ?
O5 C26 C27 118.6(3) . . ?
O6 C26 C27 116.1(3) . . ?
C27 S3 C30 91.8(2) . . ?
C28 C27 C26 128.3(5) . . ?
C28 C27 S3 111.7(4) . . ?
C26 C27 S3 119.8(2) . . ?
C27 C28 C29 113.6(6) . . ?
C27 C28 H28 123.2 . . ?
C29 C28 H28 123.2 . . ?
C30 C29 C28 111.3(6) . . ?
C30 C29 H29 124.3 . . ?
C28 C29 H29 124.3 . . ?
C29 C30 S3 111.6(4) . . ?
C29 C30 H30 124.2 . . ?
S3 C30 H30 124.2 . . ?
C27B S3B C30B 90.5(7) . . ?
C28B C27B C26 123.6(9) . . ?
C28B C27B S3B 112.8(8) . . ?
C26 C27B S3B 123.5(4) . . ?
C27B C28B C29B 112.8(11) . . ?
C27B C28B H28B 123.6 . . ?
C29B C28B H28B 123.6 . . ?
C30B C29B C28B 110.1(14) . . ?
C30B C29B H29B 124.9 . . ?
C28B C29B H29B 124.9 . . ?
C29B C30B S3B 111.9(12) . . ?
C29B C30B H30B 124.1 . . ?
S3B C30B H30B 124.1 . . ?
C31 O7 Ho1 129.52(19) . . ?
C31 O8 Ho2 168.0(2) . . ?
O8 C31 O7 124.9(3) . . ?
O8 C31 C32B 117.6(3) . . ?
O7 C31 C32B 117.5(3) . . ?
O8 C31 C32 117.6(3) . . ?
O7 C31 C32 117.5(3) . . ?
C35 S4 C32 92.8(3) . . ?
C33 C32 C31 126.8(4) . . ?
C33 C32 S4 111.8(4) . . ?
C31 C32 S4 121.1(2) . . ?
C32 C33 C34 109.2(6) . . ?
C32 C33 H33 125.4 . . ?
C34 C33 H33 125.4 . . ?
C35 C34 C33 111.7(6) . . ?
C35 C34 H34 124.1 . . ?
C33 C34 H34 124.1 . . ?
C34 C35 S4 113.4(5) . . ?
C34 C35 H35 123.3 . . ?
S4 C35 H35 123.3 . . ?
C35B S4B C32B 91.8(7) . . ?
C33B C32B C31 130.2(8) . . ?
C33B C32B S4B 111.1(7) . . ?
C31 C32B S4B 118.5(3) . . ?
C32B C33B C34B 108.8(10) . . ?
C32B C33B H33B 125.6 . . ?
C34B C33B H33B 125.6 . . ?
C35B C34B C33B 110.2(12) . . ?
C35B C34B H34B 124.9 . . ?
C33B C34B H34B 124.9 . . ?
C34B C35B S4B 112.4(11) . . ?
C34B C35B H35B 123.8 . . ?
S4B C35B H35B 123.8 . . ?
C36 O9 Ho2 142.8(2) . . ?
O10 C36 O9 125.3(3) . . ?
O10 C36 C37B 118.1(3) . . ?
O9 C36 C37B 116.5(3) . . ?
O10 C36 C37 118.1(3) . . ?
O9 C36 C37 116.5(3) . . ?
C40 S5 C37 96.5(3) . . ?
C38 C37 C36 128.8(6) . . ?
C38 C37 S5 108.9(5) . . ?
C36 C37 S5 122.2(3) . . ?
C37 C38 C39 109.7(7) . . ?
C37 C38 H38 125.1 . . ?
C39 C38 H38 125.1 . . ?
C40 C39 C38 110.0(9) . . ?
C40 C39 H39 125.0 . . ?
C38 C39 H39 125.0 . . ?
C39 C40 S5 114.7(8) . . ?
C39 C40 H40 122.6 . . ?
S5 C40 H40 122.6 . . ?
C40B S5B C37B 101.0(6) . . ?
C38B C37B C36 133.7(7) . . ?
C38B C37B S5B 106.3(6) . . ?
C36 C37B S5B 120.0(3) . . ?
C37B C38B C39B 108.8(9) . . ?
C37B C38B H38B 125.6 . . ?
C39B C38B H38B 125.6 . . ?
C40B C39B C38B 109.3(12) . . ?
C40B C39B H39B 125.3 . . ?
C38B C39B H39B 125.3 . . ?
C39B C40B S5B 113.3(12) . . ?
C39B C40B H40B 123.4 . . ?
S5B C40B H40B 123.4 . . ?
Ho2 O11 H11A 112(3) . . ?
Ho2 O11 H11B 135(2) . . ?
H11A O11 H11B 107(4) . . ?
Ho2 O12 H12A 123(3) . . ?
Ho2 O12 H12B 119(3) . . ?
H12A O12 H12B 106(4) . . ?
O14 C56 O13 125.8(3) . . ?
O14 C56 C57 114.9(4) . . ?
O13 C56 C57 119.4(4) . . ?
O14 C56 C57B 133.9(8) . . ?
O13 C56 C57B 100.1(8) . . ?
C60 S6 C57 90.7(2) . . ?
C56 C57 C58 122.9(5) . . ?
C56 C57 S6 118.6(3) . . ?
C58 C57 S6 118.6(4) . . ?
C57 C58 C59 99.3(5) . . ?
C57 C58 H58 130.3 . . ?
C59 C58 H58 130.3 . . ?
C60 C59 C58 118.0(5) . . ?
C60 C59 H59 121.0 . . ?
C58 C59 H59 121.0 . . ?
C59 C60 S6 113.4(4) . . ?
C59 C60 H60 123.3 . . ?
S6 C60 H60 123.3 . . ?
C60B S6B C57B 93.1(6) . . ?
C56 C57B C58B 136.7(14) . . ?
C56 C57B S6B 106.9(11) . . ?
C58B C57B S6B 116.3(8) . . ?
C57B C58B C59B 99.5(9) . . ?
C57B C58B H58B 130.3 . . ?
C59B C58B H58B 130.3 . . ?
C60B C59B C58B 118.9(11) . . ?
C60B C59B H59B 120.5 . . ?
C58B C59B H59B 120.5 . . ?
C59B C60B S6B 112.1(10) . . ?
C59B C60B H60B 124.0 . . ?
S6B C60B H60B 124.0 . . ?

_refine_diff_density_max         0.811
_refine_diff_density_min         -1.621
_refine_diff_density_rms         0.098

####################################################################### 
# 
# 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_final_a_CCDC12
_database_code_depnum_ccdc_archive 'CCDC 1544447'
_audit_update_record             
;
2017-04-17 deposited with the CCDC.
2017-08-23 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT415_final_a             
;
PROBLEM: Short Inter D-H..H-X       H15    ..  H8B     ..       1.95 Ang.  
RESPONSE: H8A and H8B are water hydrogen atoms which were found in the
difference map in good hydrogen bond locations. H8A and H8B are part of a
partially occupied lattice water molecule which is only present 17% of the
time.
;
# end Validation Reply Form


_audit_creation_date             2017-04-06
_audit_creation_method           
;
Olex2 1.2
(compiled Mar 28 2017 19:26:29 for OlexSys, GUI svn.r5335)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        'Tb Dimer'
_chemical_formula_moiety         'C60 H44 N6 O14 S6 Tb2, 0.34(H2 O)'
_chemical_formula_sum            'C60 H44.74 N6 O14.37 S6 Tb2'
_chemical_formula_weight         1589.87
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   11.8918(8)
_cell_length_b                   25.3435(17)
_cell_length_c                   9.7176(6)
_cell_angle_alpha                90
_cell_angle_beta                 97.7600(10)
_cell_angle_gamma                90
_cell_volume                     2901.9(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9983
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      31.57
_cell_measurement_theta_min      2.36
_shelx_estimated_absorpt_T_max   0.713
_shelx_estimated_absorpt_T_min   0.401
_exptl_absorpt_coefficient_mu    2.708
_exptl_absorpt_correction_T_max  0.8237
_exptl_absorpt_correction_T_min  0.5234
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1349 before and 0.0430 after correction.
The Ratio of minimum to maximum transmission is 0.6354.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.820
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       rhombus
_exptl_crystal_F_000             1575
_exptl_crystal_size_max          0.413
_exptl_crystal_size_mid          0.184
_exptl_crystal_size_min          0.134
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0274
_diffrn_reflns_av_unetI/netI     0.0212
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            36952
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.281
_diffrn_reflns_theta_min         2.360
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_special_details          ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6530
_reflns_number_total             7185
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.525
_refine_diff_density_min         -0.590
_refine_diff_density_rms         0.076
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     530
_refine_ls_number_reflns         7185
_refine_ls_number_restraints     441
_refine_ls_R_factor_all          0.0235
_refine_ls_R_factor_gt           0.0191
_refine_ls_restrained_S_all      1.047
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0127P)²+2.7238P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0387
_refine_ls_wR_factor_ref         0.0398
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O8-H8A = O8-H8B
 0.86 with sigma of 0.02
 O7-H7A = O7-H7B
 0.86 with sigma of 0.02
 H8A-H8B
 1.35 with sigma of 0.02
 H7A-H7B
 1.35 with sigma of 0.02
 S1A-C17 \\sim S1-C17 \\sim S2-C22 \\sim S2A-C22 \\sim S3A-C27 \\sim S3-C27
 with sigma of 0.01
 S1A-C20A \\sim S1-C20 \\sim S2-C25 \\sim S2A-C25A \\sim S3A-C30A \\sim S3-C30
 with sigma of 0.01
 C20-C19 \\sim C20A-C19A \\sim C25A-C24A \\sim C25-C24 \\sim C30A-C29A \\sim
C30-C29
 with sigma of 0.01
 C19-C18 \\sim C19A-C18A \\sim C24A-C23A \\sim C24-C23 \\sim C29A-C28A \\sim
C29-C28
 with sigma of 0.01
 C18-C17 \\sim C18A-C17 \\sim C23A-C22 \\sim C23-C22 \\sim C28-C27 \\sim
C28A-C27
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
S1 \\sim C17 \\sim C18 \\sim C19 \\sim C20 \\sim S1A \\sim C18A \\sim C19A
\\sim C20A \\sim S1 \\sim C17 \\sim C18 \\sim C17 \\sim S1A \\sim C17 \\sim
C18A \\sim C17 \\sim S1 \\sim C20 \\sim C19 \\sim C18 \\sim S1A \\sim C20A
\\sim C19A \\sim C18A \\sim C20 \\sim C19 \\sim C20A \\sim C19A: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
S2 \\sim C22 \\sim C23 \\sim C24 \\sim C25 \\sim S2A \\sim C23A \\sim C24A
\\sim C25A \\sim S2 \\sim C22 \\sim C23 \\sim C22 \\sim S2A \\sim C22 \\sim
C23A \\sim C22 \\sim S2 \\sim C25 \\sim C24 \\sim C23 \\sim S2A \\sim C25A
\\sim C24A \\sim C23A \\sim C25 \\sim C24 \\sim C25A \\sim C24A: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
S3 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim S3A \\sim C28A \\sim C29A
\\sim C30A \\sim S3 \\sim C27 \\sim C28 \\sim C27 \\sim S3A \\sim C27 \\sim
C28A \\sim C27 \\sim S3 \\sim C30 \\sim C29 \\sim C28 \\sim S3A \\sim C30A
\\sim C29A \\sim C28A \\sim C30 \\sim C29 \\sim C30A \\sim C29A: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(S1A)=Sof(C18A)=Sof(H18A)=Sof(C19A)=Sof(H19A)=Sof(C20A)=Sof(H20A)=1-FVAR(1)
 Sof(S1)=Sof(C18)=Sof(H18)=Sof(C19)=Sof(H19)=Sof(C20)=Sof(H20)=FVAR(1)
 Sof(S2A)=Sof(C23A)=Sof(H23A)=Sof(C24A)=Sof(H24A)=Sof(C25A)=Sof(H25A)=1-FVAR(2)
 Sof(S2)=Sof(C23)=Sof(H23)=Sof(C24)=Sof(H24)=Sof(C25)=Sof(H25)=FVAR(2)
 Sof(S3A)=Sof(C28A)=Sof(H28A)=Sof(C29A)=Sof(H29A)=Sof(C30A)=Sof(H30A)=1-FVAR(3)
 Sof(S3)=Sof(C28)=Sof(H28)=Sof(C29)=Sof(H29)=Sof(C30)=Sof(H30)=FVAR(3)
 Sof(O8)=Sof(H8A)=Sof(H8B)=FVAR(4)
5.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C12(H12), C13(H13),
 C14(H14), C15(H15), C18(H18), C19(H19), C20(H20), C23(H23), C24(H24), C25(H25),
  C28(H28), C29(H29), C30(H30), C18A(H18A), C19A(H19A), C20A(H20A), C23A(H23A),
 C24A(H24A), C25A(H25A), C28A(H28A), C29A(H29A), C30A(H30A)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb 0.48393(2) 0.59803(2) 0.40156(2) 0.00924(3) Uani 1 1 d . . . . .
S1 S 0.75741(15) 0.55760(7) -0.00088(16) 0.0162(3) Uani 0.684(3) 1 d D U P A 1
S2 S 0.13310(17) 0.53528(8) 0.2618(2) 0.0152(4) Uani 0.519(3) 1 d D U P B 1
S3 S 0.11581(18) 0.70539(8) 0.34133(19) 0.0151(4) Uani 0.592(3) 1 d D U P C 1
O1 O 0.58752(12) 0.55619(6) 0.21071(15) 0.0214(3) Uani 1 1 d . . . . .
O2 O 0.64458(11) 0.63311(5) 0.30295(14) 0.0155(3) Uani 1 1 d . . . . .
O3 O 0.38514(11) 0.52030(5) 0.35125(14) 0.0157(3) Uani 1 1 d . . . . .
O4 O 0.36533(11) 0.45269(5) 0.49309(14) 0.0153(3) Uani 1 1 d . . . . .
O5 O 0.29807(11) 0.62913(5) 0.43173(14) 0.0154(3) Uani 1 1 d . . . . .
O6 O 0.22794(11) 0.60085(5) 0.62175(14) 0.0164(3) Uani 1 1 d . . . . .
O7 O 0.44292(12) 0.56954(6) 0.63098(14) 0.0162(3) Uani 1 1 d D . . . .
H7A H 0.3774(14) 0.5759(9) 0.639(3) 0.024 Uiso 1 1 d DR . . . .
H7B H 0.4632(18) 0.5399(7) 0.663(2) 0.024 Uiso 1 1 d DR . . . .
O8 O 0.4949(8) 0.4681(3) 0.1049(9) 0.024(3) Uani 0.169(5) 1 d D . P . .
H8A H 0.488(13) 0.465(5) 0.016(3) 0.036 Uiso 0.169(5) 1 d DR . P . .
H8B H 0.518(12) 0.500(2) 0.121(12) 0.036 Uiso 0.169(5) 1 d DR . P . .
N1 N 0.58434(13) 0.66572(6) 0.57234(16) 0.0122(3) Uani 1 1 d . . . . .
N2 N 0.45021(12) 0.69603(6) 0.34008(16) 0.0111(3) Uani 1 1 d . . . . .
N3 N 0.37834(14) 0.61802(7) 0.16129(17) 0.0182(3) Uani 1 1 d . . . . .
C1 C 0.65394(16) 0.64979(8) 0.6847(2) 0.0163(4) Uani 1 1 d . . . . .
H1 H 0.6583 0.6131 0.7046 0.020 Uiso 1 1 calc R . . . .
C2 C 0.71985(16) 0.68380(8) 0.7736(2) 0.0180(4) Uani 1 1 d . . . . .
H2 H 0.7681 0.6708 0.8522 0.022 Uiso 1 1 calc R . . . .
C3 C 0.71344(16) 0.73731(8) 0.7449(2) 0.0181(4) Uani 1 1 d . . . . .
H3 H 0.7566 0.7618 0.8043 0.022 Uiso 1 1 calc R . . . .
C4 C 0.64337(16) 0.75445(8) 0.6287(2) 0.0167(4) Uani 1 1 d . . . . .
H4 H 0.6389 0.7909 0.6063 0.020 Uiso 1 1 calc R . . . .
C5 C 0.57936(15) 0.71795(7) 0.54471(19) 0.0121(4) Uani 1 1 d . . . . .
C6 C 0.49918(15) 0.73459(7) 0.42154(19) 0.0122(4) Uani 1 1 d . . . . .
C7 C 0.47543(17) 0.78787(7) 0.3934(2) 0.0169(4) Uani 1 1 d . . . . .
H7 H 0.5107 0.8145 0.4532 0.020 Uiso 1 1 calc R . . . .
C8 C 0.40027(18) 0.80129(8) 0.2781(2) 0.0206(4) Uani 1 1 d . . . . .
H8 H 0.3834 0.8372 0.2567 0.025 Uiso 1 1 calc R . . . .
C9 C 0.34993(17) 0.76161(8) 0.1942(2) 0.0192(4) Uani 1 1 d . . . . .
H9 H 0.2979 0.7700 0.1141 0.023 Uiso 1 1 calc R . . . .
C10 C 0.37596(15) 0.70915(8) 0.22776(19) 0.0140(4) Uani 1 1 d . . . . .
C11 C 0.32784(16) 0.66519(8) 0.1377(2) 0.0171(4) Uani 1 1 d . . . . .
C12 C 0.23890(17) 0.67255(10) 0.0301(2) 0.0246(5) Uani 1 1 d . . . . .
H12 H 0.2004 0.7054 0.0188 0.029 Uiso 1 1 calc R . . . .
C13 C 0.20758(19) 0.63122(10) -0.0600(2) 0.0300(5) Uani 1 1 d . . . . .
H13 H 0.1477 0.6356 -0.1343 0.036 Uiso 1 1 calc R . . . .
C14 C 0.2637(2) 0.58383(10) -0.0412(2) 0.0329(6) Uani 1 1 d . . . . .
H14 H 0.2458 0.5555 -0.1044 0.039 Uiso 1 1 calc R . . . .
C15 C 0.3474(2) 0.57834(9) 0.0725(2) 0.0281(5) Uani 1 1 d . . . . .
H15 H 0.3842 0.5452 0.0880 0.034 Uiso 1 1 calc R . . . .
C16 C 0.65460(16) 0.59475(8) 0.2224(2) 0.0147(4) Uani 1 1 d . . . . .
C17 C 0.75085(15) 0.59677(7) 0.13931(19) 0.0133(3) Uani 1 1 d D U . . .
C18 C 0.8460(6) 0.6287(3) 0.1606(8) 0.0142(14) Uani 0.684(3) 1 d D U P A 1
H18 H 0.8572 0.6537 0.2341 0.017 Uiso 0.684(3) 1 calc R . P A 1
C19 C 0.9252(10) 0.6220(4) 0.0671(10) 0.0156(10) Uani 0.684(3) 1 d D U P A 1
H19 H 0.9943 0.6410 0.0691 0.019 Uiso 0.684(3) 1 calc R . P A 1
C20 C 0.8873(6) 0.5841(4) -0.0265(11) 0.0159(12) Uani 0.684(3) 1 d D U P A 1
H20 H 0.9281 0.5731 -0.0991 0.019 Uiso 0.684(3) 1 calc R . P A 1
C21 C 0.32595(15) 0.48734(7) 0.40777(18) 0.0106(3) Uani 1 1 d . . . . .
C22 C 0.20139(15) 0.48796(7) 0.36961(18) 0.0109(3) Uani 1 1 d D U . . .
C23 C 0.1234(7) 0.4533(3) 0.4136(11) 0.0185(17) Uani 0.519(3) 1 d D U P B 1
H23 H 0.1457 0.4251 0.4759 0.022 Uiso 0.519(3) 1 calc R . P B 1
C24 C 0.0100(9) 0.4623(6) 0.3605(17) 0.0144(14) Uani 0.519(3) 1 d D U P B 1
H24 H -0.0528 0.4416 0.3789 0.017 Uiso 0.519(3) 1 calc R . P B 1
C25 C 0.0047(8) 0.5057(6) 0.278(2) 0.0162(16) Uani 0.519(3) 1 d D U P B 1
H25 H -0.0653 0.5190 0.2327 0.019 Uiso 0.519(3) 1 calc R . P B 1
C26 C 0.22476(15) 0.62830(7) 0.51479(19) 0.0118(4) Uani 1 1 d . . . . .
C27 C 0.12736(15) 0.66573(7) 0.48248(18) 0.0132(4) Uani 1 1 d D U . . .
C28 C 0.0406(7) 0.6764(4) 0.5603(7) 0.0221(16) Uani 0.592(3) 1 d D U P C 1
H28 H 0.0329 0.6578 0.6435 0.027 Uiso 0.592(3) 1 calc R . P C 1
C29 C -0.0345(10) 0.7160(4) 0.5087(11) 0.0198(13) Uani 0.592(3) 1 d D U P C 1
H29 H -0.0988 0.7271 0.5494 0.024 Uiso 0.592(3) 1 calc R . P C 1
C30 C -0.0018(9) 0.7363(6) 0.3915(12) 0.0167(14) Uani 0.592(3) 1 d D U P C 1
H30 H -0.0399 0.7648 0.3415 0.020 Uiso 0.592(3) 1 calc R . P C 1
S1A S 0.8575(3) 0.63755(18) 0.1886(4) 0.0119(7) Uani 0.316(3) 1 d D U P A 2
C18A C 0.7675(13) 0.5667(6) 0.0238(13) 0.018(2) Uani 0.316(3) 1 d D U P A 2
H18A H 0.7150 0.5407 -0.0152 0.022 Uiso 0.316(3) 1 calc R . P A 2
C19A C 0.8682(14) 0.5781(9) -0.030(3) 0.016(2) Uani 0.316(3) 1 d D U P A 2
H19A H 0.8925 0.5625 -0.1096 0.020 Uiso 0.316(3) 1 calc R . P A 2
C20A C 0.925(2) 0.6154(10) 0.052(2) 0.016(2) Uani 0.316(3) 1 d D U P A 2
H20A H 0.9966 0.6286 0.0356 0.019 Uiso 0.316(3) 1 calc R . P A 2
S2A S 0.12388(18) 0.43845(8) 0.4297(3) 0.0147(4) Uani 0.481(3) 1 d D U P B 2
C23A C 0.1328(7) 0.5235(3) 0.2909(9) 0.0187(17) Uani 0.481(3) 1 d D U P B 2
H23A H 0.1624 0.5535 0.2496 0.022 Uiso 0.481(3) 1 calc R . P B 2
C24A C 0.0171(9) 0.5125(6) 0.276(2) 0.0156(15) Uani 0.481(3) 1 d D U P B 2
H24A H -0.0411 0.5330 0.2247 0.019 Uiso 0.481(3) 1 calc R . P B 2
C25A C 0.0017(9) 0.4674(7) 0.3461(19) 0.0150(18) Uani 0.481(3) 1 d D U P B 2
H25A H -0.0715 0.4528 0.3493 0.018 Uiso 0.481(3) 1 calc R . P B 2
S3A S 0.0350(3) 0.67552(17) 0.5969(3) 0.0223(6) Uani 0.408(3) 1 d D U P C 2
C28A C 0.1061(11) 0.7014(5) 0.3736(10) 0.020(2) Uani 0.408(3) 1 d D U P C 2
H28A H 0.1526 0.7033 0.3015 0.024 Uiso 0.408(3) 1 calc R . P C 2
C29A C 0.0123(14) 0.7341(8) 0.3764(19) 0.0184(17) Uani 0.408(3) 1 d D U P C 2
H29A H -0.0161 0.7586 0.3062 0.022 Uiso 0.408(3) 1 calc R . P C 2
C30A C -0.0316(15) 0.7254(5) 0.4956(17) 0.020(2) Uani 0.408(3) 1 d D U P C 2
H30A H -0.0936 0.7449 0.5214 0.024 Uiso 0.408(3) 1 calc R . P C 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 O1 2.5882(14) . ?
Tb1 O2 2.4193(13) . ?
Tb1 O3 2.3119(13) . ?
Tb1 O4 2.3277(13) 3_666 ?
Tb1 O5 2.4015(13) . ?
Tb1 O7 2.4542(13) . ?
Tb1 N1 2.5666(16) . ?
Tb1 N2 2.5732(15) . ?
Tb1 N3 2.5482(16) . ?
Tb1 C16 2.8482(18) . ?
S1 C17 1.696(2) . ?
S1 C20 1.732(5) . ?
S2 C22 1.722(2) . ?
S2 C25 1.728(8) . ?
S3 C27 1.691(2) . ?
S3 C30 1.729(7) . ?
O1 C16 1.257(2) . ?
O2 C16 1.264(2) . ?
O3 C21 1.265(2) . ?
O4 Tb1 2.3277(13) 3_666 ?
O4 C21 1.254(2) . ?
O5 C26 1.266(2) . ?
O6 C26 1.247(2) . ?
O7 H7A 0.809(15) . ?
O7 H7B 0.837(15) . ?
O8 H8A 0.86(2) . ?
O8 H8B 0.86(2) . ?
N1 C1 1.340(2) . ?
N1 C5 1.350(2) . ?
N2 C6 1.340(2) . ?
N2 C10 1.350(2) . ?
N3 C11 1.344(3) . ?
N3 C15 1.344(3) . ?
C1 H1 0.9500 . ?
C1 C2 1.386(3) . ?
C2 H2 0.9500 . ?
C2 C3 1.385(3) . ?
C3 H3 0.9500 . ?
C3 C4 1.380(3) . ?
C4 H4 0.9500 . ?
C4 C5 1.391(3) . ?
C5 C6 1.487(3) . ?
C6 C7 1.399(2) . ?
C7 H7 0.9500 . ?
C7 C8 1.379(3) . ?
C8 H8 0.9500 . ?
C8 C9 1.379(3) . ?
C9 H9 0.9500 . ?
C9 C10 1.394(3) . ?
C10 C11 1.483(3) . ?
C11 C12 1.396(3) . ?
C12 H12 0.9500 . ?
C12 C13 1.383(3) . ?
C13 H13 0.9500 . ?
C13 C14 1.374(4) . ?
C14 H14 0.9500 . ?
C14 C15 1.391(3) . ?
C15 H15 0.9500 . ?
C16 C17 1.488(2) . ?
C17 C18 1.384(6) . ?
C17 S1A 1.656(4) . ?
C17 C18A 1.393(8) . ?
C18 H18 0.9500 . ?
C18 C19 1.404(8) . ?
C19 H19 0.9500 . ?
C19 C20 1.358(5) . ?
C20 H20 0.9500 . ?
C21 C22 1.478(2) . ?
C22 C23 1.387(6) . ?
C22 S2A 1.706(3) . ?
C22 C23A 1.376(6) . ?
C23 H23 0.9500 . ?
C23 C24 1.397(9) . ?
C24 H24 0.9500 . ?
C24 C25 1.355(6) . ?
C25 H25 0.9500 . ?
C26 C27 1.497(3) . ?
C27 C28 1.386(6) . ?
C27 S3A 1.683(3) . ?
C27 C28A 1.388(7) . ?
C28 H28 0.9500 . ?
C28 C29 1.392(9) . ?
C29 H29 0.9500 . ?
C29 C30 1.353(6) . ?
C30 H30 0.9500 . ?
S1A C20A 1.733(9) . ?
C18A H18A 0.9500 . ?
C18A C19A 1.399(11) . ?
C19A H19A 0.9500 . ?
C19A C20A 1.354(7) . ?
C20A H20A 0.9500 . ?
S2A C25A 1.730(8) . ?
C23A H23A 0.9500 . ?
C23A C24A 1.392(10) . ?
C24A H24A 0.9500 . ?
C24A C25A 1.355(6) . ?
C25A H25A 0.9500 . ?
S3A C30A 1.727(8) . ?
C28A H28A 0.9500 . ?
C28A C29A 1.394(10) . ?
C29A H29A 0.9500 . ?
C29A C30A 1.352(7) . ?
C30A H30A 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Tb1 C16 26.18(5) . . ?
O2 Tb1 O1 52.34(4) . . ?
O2 Tb1 O7 137.08(5) . . ?
O2 Tb1 N1 71.77(5) . . ?
O2 Tb1 N2 70.12(4) . . ?
O2 Tb1 N3 83.21(5) . . ?
O2 Tb1 C16 26.18(5) . . ?
O3 Tb1 O1 77.10(4) . . ?
O3 Tb1 O2 129.44(5) . . ?
O3 Tb1 O4 87.80(5) . 3_666 ?
O3 Tb1 O5 81.70(5) . . ?
O3 Tb1 O7 77.51(5) . . ?
O3 Tb1 N1 152.25(5) . . ?
O3 Tb1 N2 135.61(5) . . ?
O3 Tb1 N3 78.59(5) . . ?
O3 Tb1 C16 103.27(5) . . ?
O4 Tb1 O1 71.10(5) 3_666 . ?
O4 Tb1 O2 76.98(5) 3_666 . ?
O4 Tb1 O5 142.60(5) 3_666 . ?
O4 Tb1 O7 70.95(5) 3_666 . ?
O4 Tb1 N1 79.71(5) 3_666 . ?
O4 Tb1 N2 136.20(5) 3_666 . ?
O4 Tb1 N3 140.15(5) 3_666 . ?
O4 Tb1 C16 71.50(5) 3_666 . ?
O5 Tb1 O1 139.19(5) . . ?
O5 Tb1 O2 135.79(4) . . ?
O5 Tb1 O7 71.74(5) . . ?
O5 Tb1 N1 93.28(5) . . ?
O5 Tb1 N2 66.08(4) . . ?
O5 Tb1 N3 72.47(5) . . ?
O5 Tb1 C16 145.87(5) . . ?
O7 Tb1 O1 134.63(5) . . ?
O7 Tb1 N1 75.02(5) . . ?
O7 Tb1 N2 116.81(5) . . ?
O7 Tb1 N3 139.21(5) . . ?
O7 Tb1 C16 142.38(5) . . ?
N1 Tb1 O1 120.81(5) . . ?
N1 Tb1 N2 63.21(5) . . ?
N1 Tb1 C16 96.15(5) . . ?
N2 Tb1 O1 107.66(5) . . ?
N2 Tb1 C16 89.30(5) . . ?
N3 Tb1 O1 69.40(5) . . ?
N3 Tb1 N1 126.03(5) . . ?
N3 Tb1 N2 63.47(5) . . ?
N3 Tb1 C16 75.48(5) . . ?
C17 S1 C20 91.6(4) . . ?
C22 S2 C25 89.5(5) . . ?
C27 S3 C30 91.2(4) . . ?
C16 O1 Tb1 88.53(11) . . ?
C16 O2 Tb1 96.21(11) . . ?
C21 O3 Tb1 140.15(12) . . ?
C21 O4 Tb1 150.93(12) . 3_666 ?
C26 O5 Tb1 142.84(12) . . ?
Tb1 O7 H7A 109.8(17) . . ?
Tb1 O7 H7B 121.3(16) . . ?
H7A O7 H7B 112(2) . . ?
H8A O8 H8B 104(3) . . ?
C1 N1 Tb1 120.51(12) . . ?
C1 N1 C5 117.57(16) . . ?
C5 N1 Tb1 121.51(12) . . ?
C6 N2 Tb1 121.66(12) . . ?
C6 N2 C10 118.86(16) . . ?
C10 N2 Tb1 119.35(12) . . ?
C11 N3 Tb1 119.15(13) . . ?
C15 N3 Tb1 119.86(14) . . ?
C15 N3 C11 118.61(18) . . ?
N1 C1 H1 118.1 . . ?
N1 C1 C2 123.75(18) . . ?
C2 C1 H1 118.1 . . ?
C1 C2 H2 120.9 . . ?
C3 C2 C1 118.19(19) . . ?
C3 C2 H2 120.9 . . ?
C2 C3 H3 120.5 . . ?
C4 C3 C2 118.95(19) . . ?
C4 C3 H3 120.5 . . ?
C3 C4 H4 120.2 . . ?
C3 C4 C5 119.56(18) . . ?
C5 C4 H4 120.2 . . ?
N1 C5 C4 121.97(18) . . ?
N1 C5 C6 116.36(16) . . ?
C4 C5 C6 121.64(17) . . ?
N2 C6 C5 116.68(16) . . ?
N2 C6 C7 121.89(18) . . ?
C7 C6 C5 121.43(17) . . ?
C6 C7 H7 120.4 . . ?
C8 C7 C6 119.24(19) . . ?
C8 C7 H7 120.4 . . ?
C7 C8 H8 120.6 . . ?
C7 C8 C9 118.87(18) . . ?
C9 C8 H8 120.6 . . ?
C8 C9 H9 120.3 . . ?
C8 C9 C10 119.47(19) . . ?
C10 C9 H9 120.3 . . ?
N2 C10 C9 121.66(19) . . ?
N2 C10 C11 116.77(17) . . ?
C9 C10 C11 121.50(18) . . ?
N3 C11 C10 116.08(17) . . ?
N3 C11 C12 121.5(2) . . ?
C12 C11 C10 122.33(19) . . ?
C11 C12 H12 120.5 . . ?
C13 C12 C11 119.0(2) . . ?
C13 C12 H12 120.5 . . ?
C12 C13 H13 120.2 . . ?
C14 C13 C12 119.6(2) . . ?
C14 C13 H13 120.2 . . ?
C13 C14 H14 120.8 . . ?
C13 C14 C15 118.4(2) . . ?
C15 C14 H14 120.8 . . ?
N3 C15 C14 122.7(2) . . ?
N3 C15 H15 118.7 . . ?
C14 C15 H15 118.7 . . ?
O1 C16 Tb1 65.29(10) . . ?
O1 C16 O2 122.84(17) . . ?
O1 C16 C17 120.21(17) . . ?
O2 C16 Tb1 57.61(9) . . ?
O2 C16 C17 116.96(16) . . ?
C17 C16 Tb1 174.01(14) . . ?
C16 C17 S1 122.54(15) . . ?
C16 C17 S1A 118.68(19) . . ?
C18 C17 S1 109.7(3) . . ?
C18 C17 C16 127.8(3) . . ?
C18A C17 C16 128.4(6) . . ?
C18A C17 S1A 112.8(6) . . ?
C17 C18 H18 122.0 . . ?
C17 C18 C19 116.0(6) . . ?
C19 C18 H18 122.0 . . ?
C18 C19 H19 125.4 . . ?
C20 C19 C18 109.2(9) . . ?
C20 C19 H19 125.4 . . ?
S1 C20 H20 123.2 . . ?
C19 C20 S1 113.5(8) . . ?
C19 C20 H20 123.2 . . ?
O3 C21 C22 118.81(16) . . ?
O4 C21 O3 124.72(17) . . ?
O4 C21 C22 116.45(15) . . ?
C21 C22 S2 122.31(14) . . ?
C21 C22 S2A 118.42(14) . . ?
C23 C22 S2 110.4(4) . . ?
C23 C22 C21 127.3(4) . . ?
C23A C22 C21 130.2(4) . . ?
C23A C22 S2A 111.4(4) . . ?
C22 C23 H23 122.1 . . ?
C22 C23 C24 115.7(8) . . ?
C24 C23 H23 122.1 . . ?
C23 C24 H24 125.8 . . ?
C25 C24 C23 108.5(12) . . ?
C25 C24 H24 125.7 . . ?
S2 C25 H25 122.1 . . ?
C24 C25 S2 115.8(11) . . ?
C24 C25 H25 122.1 . . ?
O5 C26 C27 115.84(16) . . ?
O6 C26 O5 126.50(17) . . ?
O6 C26 C27 117.63(16) . . ?
C26 C27 S3 121.50(14) . . ?
C26 C27 S3A 120.68(17) . . ?
C28 C27 S3 110.0(4) . . ?
C28 C27 C26 128.4(4) . . ?
C28A C27 C26 128.9(5) . . ?
C28A C27 S3A 109.9(5) . . ?
C27 C28 H28 122.2 . . ?
C27 C28 C29 115.6(7) . . ?
C29 C28 H28 122.2 . . ?
C28 C29 H29 125.2 . . ?
C30 C29 C28 109.5(10) . . ?
C30 C29 H29 125.2 . . ?
S3 C30 H30 123.2 . . ?
C29 C30 S3 113.6(9) . . ?
C29 C30 H30 123.2 . . ?
C17 S1A C20A 89.5(8) . . ?
C17 C18A H18A 122.9 . . ?
C17 C18A C19A 114.1(14) . . ?
C19A C18A H18A 122.9 . . ?
C18A C19A H19A 126.0 . . ?
C20A C19A C18A 108(2) . . ?
C20A C19A H19A 126.0 . . ?
S1A C20A H20A 122.2 . . ?
C19A C20A S1A 115.6(18) . . ?
C19A C20A H20A 122.2 . . ?
C22 S2A C25A 89.2(5) . . ?
C22 C23A H23A 122.3 . . ?
C22 C23A C24A 115.5(8) . . ?
C24A C23A H23A 122.3 . . ?
C23A C24A H24A 125.8 . . ?
C25A C24A C23A 108.4(12) . . ?
C25A C24A H24A 125.8 . . ?
S2A C25A H25A 122.2 . . ?
C24A C25A S2A 115.6(12) . . ?
C24A C25A H25A 122.2 . . ?
C27 S3A C30A 91.2(6) . . ?
C27 C28A H28A 122.1 . . ?
C27 C28A C29A 115.9(11) . . ?
C29A C28A H28A 122.1 . . ?
C28A C29A H29A 125.6 . . ?
C30A C29A C28A 108.8(16) . . ?
C30A C29A H29A 125.6 . . ?
S3A C30A H30A 123.0 . . ?
C29A C30A S3A 114.1(14) . . ?
C29A C30A H30A 123.0 . . ?

_olex2_submission_original_sample_id RJB391
_olex2_submission_special_instructions 'No special instructions were received'

####################################################################### 
# 
# 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_final_a_CCDC13
_database_code_depnum_ccdc_archive 'CCDC 1544446'
_audit_update_record             
;
2017-04-17 deposited with the CCDC.
2017-08-23 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT415_final_a             
;
PROBLEM: Short Inter D-H..H-X       H1     ..  H8A     ..       1.89 Ang.  
RESPONSE: H8A is a water hydrogen atom which was found in the
difference map in a good hydrogen bond location. H8A is part of a
partially occupied lattice water molecule which is only present 19% of the
time.
;
# end Validation Reply Form


_audit_creation_date             2017-04-06
_audit_creation_method           
;
Olex2 1.2
(compiled Mar 28 2017 19:26:29 for OlexSys, GUI svn.r5335)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        'Gd Dimer'
_chemical_formula_moiety         'C60 H44 Gd2 N6 O14 S6, 0.37(H2 O)'
_chemical_formula_sum            'C60 H44.74 Gd2 N6 O14.37 S6'
_chemical_formula_weight         1586.54
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Gd Gd -0.1653 3.9035 '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'

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

_cell_length_a                   11.9100(5)
_cell_length_b                   25.3890(10)
_cell_length_c                   9.7186(4)
_cell_angle_alpha                90
_cell_angle_beta                 97.852(2)
_cell_angle_gamma                90
_cell_volume                     2911.2(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9961
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      30.48
_cell_measurement_theta_min      2.26
_shelx_estimated_absorpt_T_max   0.836
_shelx_estimated_absorpt_T_min   0.807
_exptl_absorpt_coefficient_mu    2.548
_exptl_absorpt_correction_T_max  0.9166
_exptl_absorpt_correction_T_min  0.8219
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.0881 before and 0.0508 after correction.
The Ratio of minimum to maximum transmission is 0.8967.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.810
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       rhombus
_exptl_crystal_F_000             1571
_exptl_crystal_size_max          0.088
_exptl_crystal_size_mid          0.084
_exptl_crystal_size_min          0.073
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0362
_diffrn_reflns_av_unetI/netI     0.0369
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            26054
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.099
_diffrn_reflns_theta_min         2.262
_diffrn_ambient_temperature      100.01
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5388
_reflns_number_total             6426
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.444
_refine_diff_density_min         -0.528
_refine_diff_density_rms         0.091
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     530
_refine_ls_number_reflns         6426
_refine_ls_number_restraints     1045
_refine_ls_R_factor_all          0.0354
_refine_ls_R_factor_gt           0.0239
_refine_ls_restrained_S_all      1.003
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0155P)²+1.6699P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0424
_refine_ls_wR_factor_ref         0.0446
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O7-H7A = O7-H7B
 0.86 with sigma of 0.02
 O8-H8B = O8-H8A
 0.86 with sigma of 0.02
 H7A-H7B
 1.35 with sigma of 0.02
 H8B-H8A
 1.35 with sigma of 0.02
 S1-C17 \\sim S1A-C17 \\sim S2A-C22 \\sim S2-C22 \\sim S3-C27 \\sim S3A-C27
 with sigma of 0.01
 S1-C20 \\sim S1A-C20A \\sim S2A-C25A \\sim S2-C25 \\sim S3-C30 \\sim S3A-C30A
 with sigma of 0.01
 C30A-C29A \\sim C30-C29 \\sim C25-C24 \\sim C25A-C24A \\sim C20A-C19A \\sim
C20-C19
 with sigma of 0.01
 C18-C17 \\sim C18A-C17 \\sim C23-C22 \\sim C23A-C22 \\sim C28-C27 \\sim
C28A-C27
 with sigma of 0.01
 C24A-C23A \\sim C24-C23 \\sim C19-C18 \\sim C19A-C18A \\sim S3A-C30A \\sim
C29A-C28A
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
S1 \\sim C17 \\sim C18 \\sim C19 \\sim C20 \\sim S1A \\sim C18A \\sim C19A
\\sim C20A \\sim S1 \\sim C17 \\sim C18 \\sim C17 \\sim S1A \\sim C17 \\sim
C18A \\sim C17 \\sim S1 \\sim C20 \\sim C19 \\sim C18 \\sim S1A \\sim C20A
\\sim C19A \\sim C18A \\sim C20 \\sim C19 \\sim C20A \\sim C19A: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
S2 \\sim C22 \\sim C23 \\sim C24 \\sim C25 \\sim S2A \\sim C23A \\sim C24A
\\sim C25A \\sim S2 \\sim C22 \\sim C23 \\sim C22 \\sim S2A \\sim C22 \\sim
C23A \\sim C22 \\sim S2 \\sim C25 \\sim C24 \\sim C23 \\sim S2A \\sim C25A
\\sim C24A \\sim C23A \\sim C25 \\sim C24 \\sim C25A \\sim C24A: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
S3 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim S3A \\sim C28A \\sim C29A
\\sim C30A \\sim S3 \\sim C27 \\sim C28 \\sim C27 \\sim S3A \\sim C27 \\sim
C28A \\sim C27 \\sim S3 \\sim C30 \\sim C29 \\sim C28 \\sim S3A \\sim C30A
\\sim C29A \\sim C28A \\sim C30 \\sim C29 \\sim C30A \\sim C29A: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C28A) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C20A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(S1A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(S1A)=Sof(C18A)=Sof(H18A)=Sof(C19A)=Sof(H19A)=Sof(C20A)=Sof(H20A)=1-FVAR(1)
 Sof(S1)=Sof(C18)=Sof(H18)=Sof(C19)=Sof(H19)=Sof(C20)=Sof(H20)=FVAR(1)
 Sof(S2A)=Sof(C23A)=Sof(H23A)=Sof(C24A)=Sof(H24A)=Sof(C25A)=Sof(H25A)=1-FVAR(2)
 Sof(S2)=Sof(C23)=Sof(H23)=Sof(C24)=Sof(H24)=Sof(C25)=Sof(H25)=FVAR(2)
 Sof(S3A)=Sof(C28A)=Sof(H28A)=Sof(C29A)=Sof(H29A)=Sof(C30A)=Sof(H30A)=1-FVAR(3)
 Sof(S3)=Sof(C28)=Sof(H28)=Sof(C29)=Sof(H29)=Sof(C30)=Sof(H30)=FVAR(3)
 Sof(O8)=Sof(H8A)=Sof(H8B)=FVAR(4)
6.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C12(H12), C13(H13),
 C14(H14), C15(H15), C18(H18), C19(H19), C20(H20), C23(H23), C24(H24), C25(H25),
  C28(H28), C29(H29), C30(H30), C18A(H18A), C19A(H19A), C20A(H20A), C23A(H23A),
 C24A(H24A), C25A(H25A), C28A(H28A), C29A(H29A), C30A(H30A)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Gd1 Gd 0.51623(2) 0.40195(2) 0.59844(2) 0.00901(4) Uani 1 1 d . U . . .
S1 S 0.24393(13) 0.44259(6) 1.00063(15) 0.0147(3) Uani 0.692(3) 1 d D U P A 1
S2 S 0.13219(18) 0.53528(9) 0.2611(3) 0.0146(5) Uani 0.524(3) 1 d D U P B 1
S3 S 0.88458(17) 0.29484(8) 0.65928(19) 0.0143(4) Uani 0.589(3) 1 d D U P C 1
O1 O 0.41366(14) 0.44268(7) 0.78945(19) 0.0206(4) Uani 1 1 d . U . . .
O2 O 0.35366(13) 0.36635(6) 0.69617(17) 0.0143(4) Uani 1 1 d . U . . .
O3 O 0.38411(13) 0.51981(6) 0.34950(17) 0.0150(4) Uani 1 1 d . U . . .
O4 O 0.36431(13) 0.45244(6) 0.49180(18) 0.0152(4) Uani 1 1 d . U . . .
O5 O 0.70280(13) 0.37080(6) 0.56814(17) 0.0151(4) Uani 1 1 d . U . . .
O6 O 0.77260(13) 0.39896(7) 0.37820(17) 0.0164(4) Uani 1 1 d . U . . .
O7 O 0.55768(14) 0.43039(7) 0.36766(18) 0.0162(4) Uani 1 1 d D U . . .
H7A H 0.6254(15) 0.4242(10) 0.363(3) 0.024 Uiso 1 1 d DR . . . .
H7B H 0.536(2) 0.4585(8) 0.335(3) 0.024 Uiso 1 1 d DR . . . .
O8 O 0.5041(9) 0.5315(4) 0.8983(11) 0.027(4) Uani 0.186(6) 1 d D U P . .
H8A H 0.502(13) 0.531(5) 0.987(3) 0.041 Uiso 0.186(6) 1 d DR . P . .
H8B H 0.467(12) 0.504(4) 0.869(12) 0.041 Uiso 0.186(6) 1 d DR . P . .
N1 N 0.62287(18) 0.38138(8) 0.8392(2) 0.0171(5) Uani 1 1 d . U . . .
N2 N 0.55065(15) 0.30359(7) 0.6596(2) 0.0109(4) Uani 1 1 d . U . . .
N3 N 0.41619(16) 0.33389(7) 0.4269(2) 0.0110(4) Uani 1 1 d . U . . .
C1 C 0.6555(3) 0.42070(11) 0.9283(3) 0.0272(7) Uani 1 1 d . U . . .
H1 H 0.6195 0.4540 0.9129 0.033 Uiso 1 1 calc R . . . .
C2 C 0.7385(3) 0.41512(12) 1.0410(3) 0.0315(7) Uani 1 1 d . U . . .
H2 H 0.7569 0.4434 1.1041 0.038 Uiso 1 1 calc R . . . .
C3 C 0.7938(2) 0.36770(12) 1.0597(3) 0.0270(7) Uani 1 1 d . U . . .
H3 H 0.8536 0.3632 1.1342 0.032 Uiso 1 1 calc R . . . .
C4 C 0.7619(2) 0.32653(12) 0.9694(3) 0.0233(6) Uani 1 1 d . U . . .
H4 H 0.8002 0.2936 0.9803 0.028 Uiso 1 1 calc R . . . .
C5 C 0.6731(2) 0.33397(10) 0.8624(3) 0.0157(5) Uani 1 1 d . U . . .
C6 C 0.62468(19) 0.29034(10) 0.7719(2) 0.0133(5) Uani 1 1 d . U . . .
C7 C 0.6502(2) 0.23795(10) 0.8050(3) 0.0186(6) Uani 1 1 d . U . . .
H7 H 0.7022 0.2295 0.8850 0.022 Uiso 1 1 calc R . . . .
C8 C 0.5998(2) 0.19855(10) 0.7216(3) 0.0195(6) Uani 1 1 d . U . . .
H8 H 0.6162 0.1626 0.7431 0.023 Uiso 1 1 calc R . . . .
C9 C 0.5253(2) 0.21193(9) 0.6067(3) 0.0158(5) Uani 1 1 d . U . . .
H9 H 0.4903 0.1853 0.5469 0.019 Uiso 1 1 calc R . . . .
C10 C 0.50126(19) 0.26497(9) 0.5780(2) 0.0118(5) Uani 1 1 d . U . . .
C11 C 0.42109(19) 0.28173(9) 0.4551(2) 0.0118(5) Uani 1 1 d . U . . .
C12 C 0.3573(2) 0.24535(10) 0.3709(3) 0.0162(5) Uani 1 1 d . U . . .
H12 H 0.3620 0.2089 0.3932 0.019 Uiso 1 1 calc R . . . .
C13 C 0.2869(2) 0.26250(10) 0.2547(3) 0.0178(6) Uani 1 1 d . U . . .
H13 H 0.2436 0.2380 0.1954 0.021 Uiso 1 1 calc R . . . .
C14 C 0.2806(2) 0.31577(10) 0.2260(3) 0.0177(6) Uani 1 1 d . U . . .
H14 H 0.2322 0.3287 0.1474 0.021 Uiso 1 1 calc R . . . .
C15 C 0.3464(2) 0.34990(10) 0.3145(3) 0.0155(5) Uani 1 1 d . U . . .
H15 H 0.3419 0.3865 0.2945 0.019 Uiso 1 1 calc R . . . .
C16 C 0.3448(2) 0.40473(10) 0.7773(2) 0.0140(5) Uani 1 1 d . U . . .
C17 C 0.24940(19) 0.40306(9) 0.8611(2) 0.0124(5) Uani 1 1 d D U . . .
C18 C 0.1578(7) 0.3704(4) 0.8343(11) 0.0142(15) Uani 0.692(3) 1 d D U P A 1
H18 H 0.1457 0.3448 0.7624 0.017 Uiso 0.692(3) 1 calc R . P A 1
C19 C 0.0786(10) 0.3827(5) 0.9413(12) 0.0165(15) Uani 0.692(3) 1 d D U P A 1
H19 H 0.0076 0.3661 0.9450 0.020 Uiso 0.692(3) 1 calc R . P A 1
C20 C 0.1243(8) 0.4205(5) 1.0303(13) 0.0181(14) Uani 0.692(3) 1 d D U P A 1
H20 H 0.0876 0.4330 1.1049 0.022 Uiso 0.692(3) 1 calc R . P A 1
C21 C 0.32531(19) 0.48726(9) 0.4060(2) 0.0107(5) Uani 1 1 d . U . . .
C22 C 0.20061(19) 0.48791(8) 0.3692(2) 0.0103(5) Uani 1 1 d D U . . .
C23 C 0.1245(7) 0.4536(3) 0.4127(12) 0.0165(18) Uani 0.524(3) 1 d D U P B 1
H23 H 0.1436 0.4250 0.4746 0.020 Uiso 0.524(3) 1 calc R . P B 1
C24 C 0.0026(9) 0.4680(7) 0.347(2) 0.0151(18) Uani 0.524(3) 1 d D U P B 1
H24 H -0.0654 0.4499 0.3575 0.018 Uiso 0.524(3) 1 calc R . P B 1
C25 C 0.0130(8) 0.5117(7) 0.270(2) 0.0164(17) Uani 0.524(3) 1 d D U P B 1
H25 H -0.0526 0.5280 0.2220 0.020 Uiso 0.524(3) 1 calc R . P B 1
C26 C 0.77617(19) 0.37173(9) 0.4857(2) 0.0105(5) Uani 1 1 d . U . . .
C27 C 0.87333(19) 0.33429(9) 0.5175(2) 0.0126(5) Uani 1 1 d D U . . .
C28 C 0.9586(8) 0.3238(5) 0.4399(9) 0.0204(17) Uani 0.589(3) 1 d D U P C 1
H28 H 0.9721 0.3428 0.3596 0.025 Uiso 0.589(3) 1 calc R . P C 1
C29 C 1.0277(8) 0.2776(4) 0.5013(13) 0.0201(18) Uani 0.589(3) 1 d D U P C 1
H29 H 1.0862 0.2603 0.4613 0.024 Uiso 0.589(3) 1 calc R . P C 1
C30 C 0.9917(10) 0.2650(6) 0.6232(12) 0.0176(16) Uani 0.589(3) 1 d D U P C 1
H30 H 1.0295 0.2393 0.6838 0.021 Uiso 0.589(3) 1 calc R . P C 1
S1A S 0.1402(4) 0.3628(3) 0.8150(7) 0.0153(9) Uani 0.308(3) 1 d D U P A 2
C18A C 0.2279(12) 0.4313(6) 0.9766(13) 0.017(2) Uani 0.308(3) 1 d D U P A 2
H18A H 0.2762 0.4577 1.0215 0.020 Uiso 0.308(3) 1 calc R . P A 2
C19A C 0.1118(17) 0.4133(11) 1.023(3) 0.013(2) Uani 0.308(3) 1 d D U P A 2
H19A H 0.0785 0.4263 1.0997 0.015 Uiso 0.308(3) 1 calc R . P A 2
C20A C 0.069(2) 0.3759(12) 0.932(3) 0.013(2) Uani 0.308(3) 1 d D U P A 2
H20A H 0.0000 0.3585 0.9399 0.015 Uiso 0.308(3) 1 calc R . P A 2
S2A S 0.1229(2) 0.43832(10) 0.4287(3) 0.0143(5) Uani 0.476(3) 1 d D U P B 2
C23A C 0.1329(8) 0.5234(4) 0.2921(11) 0.0167(18) Uani 0.476(3) 1 d D U P B 2
H23A H 0.1586 0.5540 0.2496 0.020 Uiso 0.476(3) 1 calc R . P B 2
C24A C 0.0065(9) 0.5060(8) 0.285(2) 0.0150(18) Uani 0.476(3) 1 d D U P B 2
H24A H -0.0582 0.5232 0.2368 0.018 Uiso 0.476(3) 1 calc R . P B 2
C25A C 0.0086(9) 0.4615(7) 0.360(2) 0.0128(17) Uani 0.476(3) 1 d D U P B 2
H25A H -0.0604 0.4443 0.3720 0.015 Uiso 0.476(3) 1 calc R . P B 2
S3A S 0.9658(4) 0.3245(2) 0.4037(4) 0.0229(7) Uani 0.411(3) 1 d D U P C 2
C28A C 0.8966(10) 0.2988(5) 0.6256(10) 0.015(2) Uani 0.411(3) 1 d D U P C 2
H28A H 0.8546 0.2954 0.7015 0.019 Uiso 0.411(3) 1 calc R . P C 2
C29A C 1.0033(14) 0.2650(8) 0.6038(18) 0.0148(19) Uani 0.411(3) 1 d D U P C 2
H29A H 1.0336 0.2362 0.6592 0.018 Uiso 0.411(3) 1 calc R . P C 2
C30A C 1.0435(12) 0.2848(6) 0.4915(19) 0.0178(19) Uani 0.411(3) 1 d D U P C 2
H30A H 1.1153 0.2749 0.4678 0.021 Uiso 0.411(3) 1 calc R . P C 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Gd1 O1 2.5743(17) . ?
Gd1 O2 2.4435(16) . ?
Gd1 O3 2.3337(16) 3_666 ?
Gd1 O4 2.3407(15) . ?
Gd1 O5 2.4142(16) . ?
Gd1 O7 2.4694(17) . ?
Gd1 N1 2.559(2) . ?
Gd1 N2 2.5868(19) . ?
Gd1 N3 2.5772(19) . ?
Gd1 C16 2.858(2) . ?
S1 C17 1.695(2) . ?
S1 C20 1.594(5) . ?
S2 C22 1.726(3) . ?
S2 C25 1.555(6) . ?
S3 C27 1.694(3) . ?
S3 C30 1.565(6) . ?
O1 C16 1.260(3) . ?
O2 C16 1.267(3) . ?
O3 Gd1 2.3339(16) 3_666 ?
O3 C21 1.257(3) . ?
O4 C21 1.259(3) . ?
O5 C26 1.264(3) . ?
O6 C26 1.249(3) . ?
O7 H7A 0.829(16) . ?
O7 H7B 0.807(16) . ?
O8 H8A 0.86(2) . ?
O8 H8B 0.86(2) . ?
N1 C1 1.343(3) . ?
N1 C5 1.350(3) . ?
N2 C6 1.349(3) . ?
N2 C10 1.345(3) . ?
N3 C11 1.352(3) . ?
N3 C15 1.342(3) . ?
C1 H1 0.9500 . ?
C1 C2 1.379(4) . ?
C2 H2 0.9500 . ?
C2 C3 1.373(4) . ?
C3 H3 0.9500 . ?
C3 C4 1.384(4) . ?
C4 H4 0.9500 . ?
C4 C5 1.391(3) . ?
C5 C6 1.482(3) . ?
C6 C7 1.392(3) . ?
C7 H7 0.9500 . ?
C7 C8 1.373(4) . ?
C8 H8 0.9500 . ?
C8 C9 1.370(3) . ?
C9 H9 0.9500 . ?
C9 C10 1.397(3) . ?
C10 C11 1.486(3) . ?
C11 C12 1.389(3) . ?
C12 H12 0.9500 . ?
C12 C13 1.382(4) . ?
C13 H13 0.9500 . ?
C13 C14 1.381(3) . ?
C14 H14 0.9500 . ?
C14 C15 1.386(3) . ?
C15 H15 0.9500 . ?
C16 C17 1.486(3) . ?
C17 C18 1.366(6) . ?
C17 S1A 1.666(4) . ?
C17 C18A 1.385(8) . ?
C18 H18 0.9500 . ?
C18 C19 1.529(6) . ?
C19 H19 0.9500 . ?
C19 C20 1.356(5) . ?
C20 H20 0.9500 . ?
C21 C22 1.480(3) . ?
C22 C23 1.366(7) . ?
C22 S2A 1.710(3) . ?
C22 C23A 1.363(7) . ?
C23 H23 0.9500 . ?
C23 C24 1.550(7) . ?
C24 H24 0.9500 . ?
C24 C25 1.348(6) . ?
C25 H25 0.9500 . ?
C26 C27 1.497(3) . ?
C27 C28 1.371(7) . ?
C27 S3A 1.683(4) . ?
C27 C28A 1.383(7) . ?
C28 H28 0.9500 . ?
C28 C29 1.509(12) . ?
C29 H29 0.9500 . ?
C29 C30 1.352(6) . ?
C30 H30 0.9500 . ?
S1A C20A 1.542(8) . ?
C18A H18A 0.9500 . ?
C18A C19A 1.579(7) . ?
C19A H19A 0.9500 . ?
C19A C20A 1.348(7) . ?
C20A H20A 0.9500 . ?
S2A C25A 1.548(6) . ?
C23A H23A 0.9500 . ?
C23A C24A 1.561(7) . ?
C24A H24A 0.9500 . ?
C24A C25A 1.347(6) . ?
C25A H25A 0.9500 . ?
S3A C30A 1.545(8) . ?
C28A H28A 0.9500 . ?
C28A C29A 1.571(7) . ?
C29A H29A 0.9500 . ?
C29A C30A 1.347(7) . ?
C30A H30A 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 Gd1 N2 107.33(6) . . ?
O1 Gd1 N3 120.85(6) . . ?
O1 Gd1 C16 26.17(6) . . ?
O2 Gd1 O1 52.34(5) . . ?
O2 Gd1 O7 136.76(6) . . ?
O2 Gd1 N1 83.67(6) . . ?
O2 Gd1 N2 70.28(6) . . ?
O2 Gd1 N3 71.49(6) . . ?
O2 Gd1 C16 26.19(6) . . ?
O3 Gd1 O1 77.24(6) 3_666 . ?
O3 Gd1 O2 129.58(6) 3_666 . ?
O3 Gd1 O4 88.25(5) 3_666 . ?
O3 Gd1 O5 81.72(6) 3_666 . ?
O3 Gd1 O7 77.83(6) 3_666 . ?
O3 Gd1 N1 78.54(6) 3_666 . ?
O3 Gd1 N2 135.39(6) 3_666 . ?
O3 Gd1 N3 152.55(6) 3_666 . ?
O3 Gd1 C16 103.40(6) 3_666 . ?
O4 Gd1 O1 71.64(6) . . ?
O4 Gd1 O2 76.64(5) . . ?
O4 Gd1 O5 142.57(6) . . ?
O4 Gd1 O7 71.10(6) . . ?
O4 Gd1 N1 140.69(7) . . ?
O4 Gd1 N2 135.98(6) . . ?
O4 Gd1 N3 79.61(6) . . ?
O4 Gd1 C16 71.49(6) . . ?
O5 Gd1 O1 139.02(6) . . ?
O5 Gd1 O2 135.86(5) . . ?
O5 Gd1 O7 71.55(6) . . ?
O5 Gd1 N1 72.22(6) . . ?
O5 Gd1 N2 65.93(6) . . ?
O5 Gd1 N3 93.06(6) . . ?
O5 Gd1 C16 145.93(6) . . ?
O7 Gd1 O1 135.31(6) . . ?
O7 Gd1 N1 138.97(6) . . ?
O7 Gd1 N2 116.49(6) . . ?
O7 Gd1 N3 74.97(6) . . ?
O7 Gd1 C16 142.51(6) . . ?
N1 Gd1 O1 69.38(6) . . ?
N1 Gd1 N2 63.22(6) . . ?
N1 Gd1 N3 125.62(6) . . ?
N1 Gd1 C16 75.84(7) . . ?
N2 Gd1 C16 89.31(6) . . ?
N3 Gd1 N2 63.01(6) . . ?
N3 Gd1 C16 95.99(7) . . ?
C20 S1 C17 94.0(4) . . ?
C25 S2 C22 93.2(6) . . ?
C30 S3 C27 94.6(4) . . ?
C16 O1 Gd1 89.56(14) . . ?
C16 O2 Gd1 95.47(14) . . ?
C21 O3 Gd1 139.63(15) . 3_666 ?
C21 O4 Gd1 150.50(15) . . ?
C26 O5 Gd1 143.02(15) . . ?
Gd1 O7 H7A 107.9(19) . . ?
Gd1 O7 H7B 121(2) . . ?
H7A O7 H7B 114(2) . . ?
H8A O8 H8B 103(3) . . ?
C1 N1 Gd1 120.07(17) . . ?
C1 N1 C5 118.2(2) . . ?
C5 N1 Gd1 119.23(16) . . ?
C6 N2 Gd1 119.50(15) . . ?
C10 N2 Gd1 121.70(15) . . ?
C10 N2 C6 118.7(2) . . ?
C11 N3 Gd1 121.50(15) . . ?
C15 N3 Gd1 120.24(15) . . ?
C15 N3 C11 117.8(2) . . ?
N1 C1 H1 118.4 . . ?
N1 C1 C2 123.2(3) . . ?
C2 C1 H1 118.4 . . ?
C1 C2 H2 120.8 . . ?
C3 C2 C1 118.3(3) . . ?
C3 C2 H2 120.8 . . ?
C2 C3 H3 120.2 . . ?
C2 C3 C4 119.5(3) . . ?
C4 C3 H3 120.2 . . ?
C3 C4 H4 120.4 . . ?
C3 C4 C5 119.1(3) . . ?
C5 C4 H4 120.4 . . ?
N1 C5 C4 121.4(2) . . ?
N1 C5 C6 116.1(2) . . ?
C4 C5 C6 122.5(2) . . ?
N2 C6 C5 116.9(2) . . ?
N2 C6 C7 121.6(2) . . ?
C7 C6 C5 121.5(2) . . ?
C6 C7 H7 120.2 . . ?
C8 C7 C6 119.7(2) . . ?
C8 C7 H7 120.2 . . ?
C7 C8 H8 120.6 . . ?
C9 C8 C7 118.9(2) . . ?
C9 C8 H8 120.6 . . ?
C8 C9 H9 120.2 . . ?
C8 C9 C10 119.6(2) . . ?
C10 C9 H9 120.2 . . ?
N2 C10 C9 121.6(2) . . ?
N2 C10 C11 116.5(2) . . ?
C9 C10 C11 121.9(2) . . ?
N3 C11 C10 116.6(2) . . ?
N3 C11 C12 121.8(2) . . ?
C12 C11 C10 121.5(2) . . ?
C11 C12 H12 120.2 . . ?
C13 C12 C11 119.6(2) . . ?
C13 C12 H12 120.2 . . ?
C12 C13 H13 120.5 . . ?
C14 C13 C12 118.9(2) . . ?
C14 C13 H13 120.5 . . ?
C13 C14 H14 120.8 . . ?
C13 C14 C15 118.5(2) . . ?
C15 C14 H14 120.8 . . ?
N3 C15 C14 123.4(2) . . ?
N3 C15 H15 118.3 . . ?
C14 C15 H15 118.3 . . ?
O1 C16 Gd1 64.27(13) . . ?
O1 C16 O2 122.5(2) . . ?
O1 C16 C17 120.5(2) . . ?
O2 C16 Gd1 58.34(12) . . ?
O2 C16 C17 117.0(2) . . ?
C17 C16 Gd1 174.84(17) . . ?
C16 C17 S1 122.49(17) . . ?
C16 C17 S1A 119.8(3) . . ?
C18 C17 S1 113.3(4) . . ?
C18 C17 C16 124.2(4) . . ?
C18A C17 C16 132.0(6) . . ?
C18A C17 S1A 108.2(6) . . ?
C17 C18 H18 126.4 . . ?
C17 C18 C19 107.3(6) . . ?
C19 C18 H18 126.4 . . ?
C18 C19 H19 124.8 . . ?
C20 C19 C18 110.3(7) . . ?
C20 C19 H19 124.8 . . ?
S1 C20 H20 122.5 . . ?
C19 C20 S1 115.1(7) . . ?
C19 C20 H20 122.5 . . ?
O3 C21 O4 125.0(2) . . ?
O3 C21 C22 119.2(2) . . ?
O4 C21 C22 115.8(2) . . ?
C21 C22 S2 122.00(18) . . ?
C21 C22 S2A 118.79(18) . . ?
C23 C22 S2 110.8(4) . . ?
C23 C22 C21 127.2(4) . . ?
C23A C22 C21 129.8(4) . . ?
C23A C22 S2A 111.4(4) . . ?
C22 C23 H23 124.9 . . ?
C22 C23 C24 110.1(8) . . ?
C24 C23 H23 124.9 . . ?
C23 C24 H24 127.1 . . ?
C25 C24 C23 105.8(11) . . ?
C25 C24 H24 127.1 . . ?
S2 C25 H25 120.0 . . ?
C24 C25 S2 120.1(11) . . ?
C24 C25 H25 120.0 . . ?
O5 C26 C27 116.0(2) . . ?
O6 C26 O5 126.4(2) . . ?
O6 C26 C27 117.5(2) . . ?
C26 C27 S3 121.12(18) . . ?
C26 C27 S3A 121.0(2) . . ?
C28 C27 S3 110.5(5) . . ?
C28 C27 C26 128.3(5) . . ?
C28A C27 C26 129.8(5) . . ?
C28A C27 S3A 108.8(5) . . ?
C27 C28 H28 125.1 . . ?
C27 C28 C29 109.8(7) . . ?
C29 C28 H28 125.1 . . ?
C28 C29 H29 126.0 . . ?
C30 C29 C28 108.0(9) . . ?
C30 C29 H29 126.0 . . ?
S3 C30 H30 121.7 . . ?
C29 C30 S3 116.6(9) . . ?
C29 C30 H30 121.7 . . ?
C20A S1A C17 98.9(9) . . ?
C17 C18A H18A 124.8 . . ?
C17 C18A C19A 110.3(11) . . ?
C19A C18A H18A 124.8 . . ?
C18A C19A H19A 126.8 . . ?
C20A C19A C18A 106.3(17) . . ?
C20A C19A H19A 126.8 . . ?
S1A C20A H20A 121.9 . . ?
C19A C20A S1A 116.2(17) . . ?
C19A C20A H20A 121.9 . . ?
C25A S2A C22 93.4(6) . . ?
C22 C23A H23A 125.3 . . ?
C22 C23A C24A 109.5(8) . . ?
C24A C23A H23A 125.3 . . ?
C23A C24A H24A 127.3 . . ?
C25A C24A C23A 105.4(12) . . ?
C25A C24A H24A 127.3 . . ?
S2A C25A H25A 119.9 . . ?
C24A C25A S2A 120.2(12) . . ?
C24A C25A H25A 119.9 . . ?
C30A S3A C27 97.4(7) . . ?
C27 C28A H28A 125.2 . . ?
C27 C28A C29A 109.6(9) . . ?
C29A C28A H28A 125.2 . . ?
C28A C29A H29A 126.6 . . ?
C30A C29A C28A 106.8(13) . . ?
C30A C29A H29A 126.6 . . ?
S3A C30A H30A 122.0 . . ?
C29A C30A S3A 116.0(12) . . ?
C29A C30A H30A 122.0 . . ?

_olex2_submission_original_sample_id RJB390
_olex2_submission_special_instructions 'No special instructions were received'

