# Electronic Supplementary Material (ESI) for Dalton Transactions.
# 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_6-Sm
_database_code_depnum_ccdc_archive 'CCDC 1549869'
_audit_update_record             
;
2017-05-13 deposited with the CCDC.
2017-11-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C19 H13 N2 O7 S Sm'
_chemical_formula_sum            'C19 H13 N2 O7 S Sm'
_chemical_formula_weight         563.72

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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   11.9619(3)
_cell_length_b                   8.48361(18)
_cell_length_c                   17.9950(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 103.186(2)
_cell_angle_gamma                90.00
_cell_volume                     1777.99(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    3164
_cell_measurement_theta_min      3.21
_cell_measurement_theta_max      27.56

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.106
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1100
_exptl_absorpt_coefficient_mu    3.470
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5294
_exptl_absorpt_correction_T_max  0.6067
_exptl_absorpt_process_details   
; 
CrysAlis Pro (Agilent, 2013)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1954
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6593
_diffrn_reflns_av_R_equivalents  0.0301
_diffrn_reflns_av_sigmaI/netI    0.0542
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.21
_diffrn_reflns_theta_max         27.56
_reflns_number_total             4054
_reflns_number_gt                3286
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_cell_refinement       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_data_reduction        
;
CrysAlis Pro (Agilent, 2013)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    '(K. Brandenburg, Diamond 3.1, 2009)'
_computing_publication_material  '(K. Brandenburg, Diamond 3.1, 2009)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0140P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4054
_refine_ls_number_parameters     277
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0302
_refine_ls_wR_factor_ref         0.0581
_refine_ls_wR_factor_gt          0.0534
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_restrained_S_all      1.018
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Sm1 Sm 0.880827(16) 0.96137(2) 0.199729(11) 0.01397(6) Uani 1 1 d . . .
S1 S 0.81957(8) 1.37244(12) 0.17142(5) 0.0166(2) Uani 1 1 d . . .
O1 O 0.7711(2) 1.2172(3) 0.18059(15) 0.0207(6) Uani 1 1 d . . .
O1W O 0.8467(2) 0.7310(3) 0.27698(16) 0.0247(7) Uani 1 1 d D . .
H1W1 H 0.900(3) 0.692(4) 0.3114(17) 0.037 Uiso 1 1 d D . .
H1W2 H 0.813(3) 0.658(3) 0.2479(19) 0.037 Uiso 1 1 d D . .
O2 O 0.7367(2) 1.4983(3) 0.16687(16) 0.0241(7) Uani 1 1 d . . .
O3 O 0.9230(2) 1.4026(3) 0.23050(14) 0.0228(7) Uani 1 1 d . . .
O4 O 0.9602(2) 1.1199(3) 0.12291(14) 0.0185(6) Uani 1 1 d . . .
O5 O 1.0378(2) 1.2388(3) -0.13405(15) 0.0222(6) Uani 1 1 d . . .
O6 O 0.9044(2) 1.4172(3) -0.18285(15) 0.0245(7) Uani 1 1 d . . .
N1 N 0.7309(3) 0.8954(4) 0.07303(19) 0.0220(8) Uani 1 1 d . . .
N2 N 0.6645(3) 0.9333(4) 0.20632(19) 0.0239(8) Uani 1 1 d . . .
C1 C 0.8603(3) 1.3612(5) 0.0838(2) 0.0136(8) Uani 1 1 d . . .
C2 C 0.9247(3) 1.2303(5) 0.0700(2) 0.0157(8) Uani 1 1 d . . .
C3 C 0.9502(3) 1.2209(5) -0.0018(2) 0.0179(8) Uani 1 1 d . . .
H3 H 0.9891 1.1329 -0.0137 0.022 Uiso 1 1 calc R . .
C4 C 0.9192(3) 1.3389(5) -0.0560(2) 0.0154(8) Uani 1 1 d . . .
C5 C 0.8559(3) 1.4678(5) -0.0407(2) 0.0175(8) Uani 1 1 d . . .
H5 H 0.8339 1.5465 -0.0770 0.021 Uiso 1 1 calc R . .
C6 C 0.8263(3) 1.4777(5) 0.0287(2) 0.0171(8) Uani 1 1 d . . .
H6 H 0.7832 1.5629 0.0389 0.021 Uiso 1 1 calc R . .
C7 C 0.9569(3) 1.3292(5) -0.1299(2) 0.0169(8) Uani 1 1 d . . .
C8 C 0.7607(4) 0.8866(6) 0.0072(2) 0.0302(11) Uani 1 1 d . . .
H8 H 0.8348 0.9169 0.0054 0.036 Uiso 1 1 calc R . .
C9 C 0.6869(4) 0.8337(6) -0.0608(3) 0.0406(13) Uani 1 1 d . . .
H9 H 0.7112 0.8290 -0.1063 0.049 Uiso 1 1 calc R . .
C10 C 0.5794(4) 0.7899(6) -0.0576(3) 0.0432(14) Uani 1 1 d . . .
H10 H 0.5295 0.7523 -0.1014 0.052 Uiso 1 1 calc R . .
C11 C 0.5419(4) 0.8001(5) 0.0101(3) 0.0331(12) Uani 1 1 d . . .
C12 C 0.4286(4) 0.7624(7) 0.0164(3) 0.0537(16) Uani 1 1 d . . .
H12 H 0.3769 0.7217 -0.0258 0.064 Uiso 1 1 calc R . .
C13 C 0.3950(4) 0.7835(7) 0.0805(3) 0.0533(16) Uani 1 1 d . . .
H13 H 0.3201 0.7574 0.0822 0.064 Uiso 1 1 calc R . .
C14 C 0.4711(4) 0.8459(6) 0.1479(3) 0.0345(12) Uani 1 1 d . . .
C15 C 0.4372(4) 0.8846(6) 0.2148(3) 0.0436(14) Uani 1 1 d . . .
H15 H 0.3622 0.8656 0.2188 0.052 Uiso 1 1 calc R . .
C16 C 0.5140(4) 0.9502(6) 0.2740(3) 0.0386(12) Uani 1 1 d . . .
H16 H 0.4914 0.9814 0.3179 0.046 Uiso 1 1 calc R . .
C17 C 0.6273(4) 0.9701(6) 0.2680(3) 0.0306(10) Uani 1 1 d . . .
H17 H 0.6797 1.0115 0.3097 0.037 Uiso 1 1 calc R . .
C18 C 0.5855(3) 0.8770(5) 0.1452(2) 0.0232(9) Uani 1 1 d . . .
C19 C 0.6220(3) 0.8549(5) 0.0754(2) 0.0232(9) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sm1 O4 2.284(3) . ?
Sm1 O6 2.309(3) 4_586 ?
Sm1 O5 2.399(3) 3_775 ?
Sm1 O3 2.447(2) 2_745 ?
Sm1 O1W 2.486(3) . ?
Sm1 O1 2.519(3) . ?
Sm1 N1 2.620(3) . ?
Sm1 N2 2.628(3) . ?
S1 O2 1.446(3) . ?
S1 O3 1.459(3) . ?
S1 O1 1.463(3) . ?
S1 C1 1.756(4) . ?
O1W H1W1 0.85(4) . ?
O1W H1W2 0.85(4) . ?
O3 Sm1 2.447(2) 2_755 ?
O4 C2 1.334(4) . ?
O5 C7 1.250(4) . ?
O5 Sm1 2.399(3) 3_775 ?
O6 C7 1.259(4) . ?
O6 Sm1 2.309(3) 4_585 ?
N1 C8 1.315(5) . ?
N1 C19 1.357(5) . ?
N2 C17 1.324(5) . ?
N2 C18 1.362(5) . ?
C1 C6 1.393(5) . ?
C1 C2 1.406(5) . ?
C2 C3 1.396(5) . ?
C3 C4 1.387(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.393(5) . ?
C4 C7 1.502(5) . ?
C5 C6 1.375(5) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C8 C9 1.409(6) . ?
C8 H8 0.9300 . ?
C9 C10 1.352(7) . ?
C9 H9 0.9300 . ?
C10 C11 1.393(7) . ?
C10 H10 0.9300 . ?
C11 C19 1.414(5) . ?
C11 C12 1.422(7) . ?
C12 C13 1.317(8) . ?
C12 H12 0.9300 . ?
C13 C14 1.442(7) . ?
C13 H13 0.9300 . ?
C14 C15 1.394(7) . ?
C14 C18 1.406(6) . ?
C15 C16 1.358(7) . ?
C15 H15 0.9300 . ?
C16 C17 1.394(6) . ?
C16 H16 0.9300 . ?
C17 H17 0.9300 . ?
C18 C19 1.433(6) . ?

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 Sm1 O6 108.07(10) . 4_586 ?
O4 Sm1 O5 81.21(10) . 3_775 ?
O6 Sm1 O5 141.98(9) 4_586 3_775 ?
O4 Sm1 O3 87.04(9) . 2_745 ?
O6 Sm1 O3 73.65(9) 4_586 2_745 ?
O5 Sm1 O3 70.06(9) 3_775 2_745 ?
O4 Sm1 O1W 160.95(9) . . ?
O6 Sm1 O1W 80.82(10) 4_586 . ?
O5 Sm1 O1W 81.70(10) 3_775 . ?
O3 Sm1 O1W 79.25(9) 2_745 . ?
O4 Sm1 O1 71.68(9) . . ?
O6 Sm1 O1 72.07(9) 4_586 . ?
O5 Sm1 O1 143.13(9) 3_775 . ?
O3 Sm1 O1 130.89(9) 2_745 . ?
O1W Sm1 O1 127.37(9) . . ?
O4 Sm1 N1 84.01(10) . . ?
O6 Sm1 N1 143.92(10) 4_586 . ?
O5 Sm1 N1 72.20(9) 3_775 . ?
O3 Sm1 N1 142.10(10) 2_745 . ?
O1W Sm1 N1 98.70(10) . . ?
O1 Sm1 N1 80.40(10) . . ?
O4 Sm1 N2 129.05(10) . . ?
O6 Sm1 N2 85.14(10) 4_586 . ?
O5 Sm1 N2 118.20(10) 3_775 . ?
O3 Sm1 N2 142.86(10) 2_745 . ?
O1W Sm1 N2 67.32(10) . . ?
O1 Sm1 N2 66.21(10) . . ?
N1 Sm1 N2 62.23(11) . . ?
O2 S1 O3 111.61(17) . . ?
O2 S1 O1 112.77(17) . . ?
O3 S1 O1 111.57(16) . . ?
O2 S1 C1 108.42(17) . . ?
O3 S1 C1 107.53(16) . . ?
O1 S1 C1 104.52(17) . . ?
S1 O1 Sm1 125.69(15) . . ?
Sm1 O1W H1W1 122(3) . . ?
Sm1 O1W H1W2 110(3) . . ?
H1W1 O1W H1W2 109.7(17) . . ?
S1 O3 Sm1 164.74(18) . 2_755 ?
C2 O4 Sm1 137.4(2) . . ?
C7 O5 Sm1 150.5(2) . 3_775 ?
C7 O6 Sm1 153.2(3) . 4_585 ?
C8 N1 C19 118.3(4) . . ?
C8 N1 Sm1 121.5(3) . . ?
C19 N1 Sm1 119.9(3) . . ?
C17 N2 C18 117.1(4) . . ?
C17 N2 Sm1 122.6(3) . . ?
C18 N2 Sm1 120.2(3) . . ?
C6 C1 C2 121.2(4) . . ?
C6 C1 S1 120.3(3) . . ?
C2 C1 S1 118.5(3) . . ?
O4 C2 C3 121.3(3) . . ?
O4 C2 C1 121.8(3) . . ?
C3 C2 C1 116.9(3) . . ?
C4 C3 C2 122.0(4) . . ?
C4 C3 H3 119.0 . . ?
C2 C3 H3 119.0 . . ?
C3 C4 C5 119.8(4) . . ?
C3 C4 C7 119.8(3) . . ?
C5 C4 C7 120.3(3) . . ?
C6 C5 C4 119.4(4) . . ?
C6 C5 H5 120.3 . . ?
C4 C5 H5 120.3 . . ?
C5 C6 C1 120.6(4) . . ?
C5 C6 H6 119.7 . . ?
C1 C6 H6 119.7 . . ?
O5 C7 O6 125.3(4) . . ?
O5 C7 C4 118.6(3) . . ?
O6 C7 C4 116.1(3) . . ?
N1 C8 C9 123.7(4) . . ?
N1 C8 H8 118.2 . . ?
C9 C8 H8 118.2 . . ?
C10 C9 C8 117.7(5) . . ?
C10 C9 H9 121.2 . . ?
C8 C9 H9 121.2 . . ?
C9 C10 C11 121.3(4) . . ?
C9 C10 H10 119.4 . . ?
C11 C10 H10 119.4 . . ?
C10 C11 C19 117.1(4) . . ?
C10 C11 C12 123.9(4) . . ?
C19 C11 C12 119.0(5) . . ?
C13 C12 C11 121.7(5) . . ?
C13 C12 H12 119.1 . . ?
C11 C12 H12 119.1 . . ?
C12 C13 C14 121.8(5) . . ?
C12 C13 H13 119.1 . . ?
C14 C13 H13 119.1 . . ?
C15 C14 C18 117.6(4) . . ?
C15 C14 C13 124.1(5) . . ?
C18 C14 C13 118.2(5) . . ?
C16 C15 C14 119.7(5) . . ?
C16 C15 H15 120.2 . . ?
C14 C15 H15 120.2 . . ?
C15 C16 C17 119.0(5) . . ?
C15 C16 H16 120.5 . . ?
C17 C16 H16 120.5 . . ?
N2 C17 C16 123.7(4) . . ?
N2 C17 H17 118.2 . . ?
C16 C17 H17 118.2 . . ?
N2 C18 C14 122.6(4) . . ?
N2 C18 C19 117.4(4) . . ?
C14 C18 C19 119.9(4) . . ?
N1 C19 C11 122.0(4) . . ?
N1 C19 C18 118.7(3) . . ?
C11 C19 C18 119.2(4) . . ?

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
O2 S1 O1 Sm1 -175.88(16) . . . . ?
O3 S1 O1 Sm1 -49.3(2) . . . . ?
C1 S1 O1 Sm1 66.6(2) . . . . ?
O4 Sm1 O1 S1 -33.29(18) . . . . ?
O6 Sm1 O1 S1 83.50(19) 4_586 . . . ?
O5 Sm1 O1 S1 -78.1(2) 3_775 . . . ?
O3 Sm1 O1 S1 35.7(2) 2_745 . . . ?
O1W Sm1 O1 S1 146.23(16) . . . . ?
N1 Sm1 O1 S1 -120.1(2) . . . . ?
N2 Sm1 O1 S1 176.1(2) . . . . ?
O2 S1 O3 Sm1 -111.0(7) . . . 2_755 ?
O1 S1 O3 Sm1 121.9(7) . . . 2_755 ?
C1 S1 O3 Sm1 7.8(8) . . . 2_755 ?
O6 Sm1 O4 C2 -95.7(3) 4_586 . . . ?
O5 Sm1 O4 C2 122.3(3) 3_775 . . . ?
O3 Sm1 O4 C2 -167.5(3) 2_745 . . . ?
O1W Sm1 O4 C2 148.8(3) . . . . ?
O1 Sm1 O4 C2 -32.4(3) . . . . ?
N1 Sm1 O4 C2 49.4(3) . . . . ?
N2 Sm1 O4 C2 2.9(4) . . . . ?
O4 Sm1 N1 C8 35.2(3) . . . . ?
O6 Sm1 N1 C8 147.9(3) 4_586 . . . ?
O5 Sm1 N1 C8 -47.5(3) 3_775 . . . ?
O3 Sm1 N1 C8 -42.2(4) 2_745 . . . ?
O1W Sm1 N1 C8 -125.8(3) . . . . ?
O1 Sm1 N1 C8 107.5(4) . . . . ?
N2 Sm1 N1 C8 175.6(4) . . . . ?
O4 Sm1 N1 C19 -151.0(3) . . . . ?
O6 Sm1 N1 C19 -38.3(4) 4_586 . . . ?
O5 Sm1 N1 C19 126.3(3) 3_775 . . . ?
O3 Sm1 N1 C19 131.7(3) 2_745 . . . ?
O1W Sm1 N1 C19 48.0(3) . . . . ?
O1 Sm1 N1 C19 -78.6(3) . . . . ?
N2 Sm1 N1 C19 -10.5(3) . . . . ?
O4 Sm1 N2 C17 -116.8(3) . . . . ?
O6 Sm1 N2 C17 -7.4(3) 4_586 . . . ?
O5 Sm1 N2 C17 141.0(3) 3_775 . . . ?
O3 Sm1 N2 C17 47.2(4) 2_745 . . . ?
O1W Sm1 N2 C17 74.7(3) . . . . ?
O1 Sm1 N2 C17 -79.9(3) . . . . ?
N1 Sm1 N2 C17 -171.4(4) . . . . ?
O4 Sm1 N2 C18 64.2(3) . . . . ?
O6 Sm1 N2 C18 173.6(3) 4_586 . . . ?
O5 Sm1 N2 C18 -38.0(3) 3_775 . . . ?
O3 Sm1 N2 C18 -131.9(3) 2_745 . . . ?
O1W Sm1 N2 C18 -104.4(3) . . . . ?
O1 Sm1 N2 C18 101.0(3) . . . . ?
N1 Sm1 N2 C18 9.6(3) . . . . ?
O2 S1 C1 C6 9.2(3) . . . . ?
O3 S1 C1 C6 -111.7(3) . . . . ?
O1 S1 C1 C6 129.7(3) . . . . ?
O2 S1 C1 C2 -169.0(3) . . . . ?
O3 S1 C1 C2 70.2(3) . . . . ?
O1 S1 C1 C2 -48.5(3) . . . . ?
Sm1 O4 C2 C3 -127.6(3) . . . . ?
Sm1 O4 C2 C1 52.5(5) . . . . ?
C6 C1 C2 O4 178.3(3) . . . . ?
S1 C1 C2 O4 -3.5(5) . . . . ?
C6 C1 C2 C3 -1.6(5) . . . . ?
S1 C1 C2 C3 176.6(3) . . . . ?
O4 C2 C3 C4 -176.5(3) . . . . ?
C1 C2 C3 C4 3.4(5) . . . . ?
C2 C3 C4 C5 -3.2(6) . . . . ?
C2 C3 C4 C7 175.1(3) . . . . ?
C3 C4 C5 C6 1.0(6) . . . . ?
C7 C4 C5 C6 -177.3(3) . . . . ?
C4 C5 C6 C1 0.8(6) . . . . ?
C2 C1 C6 C5 -0.5(6) . . . . ?
S1 C1 C6 C5 -178.6(3) . . . . ?
Sm1 O5 C7 O6 -48.3(7) 3_775 . . . ?
Sm1 O5 C7 C4 133.2(4) 3_775 . . . ?
Sm1 O6 C7 O5 -11.1(8) 4_585 . . . ?
Sm1 O6 C7 C4 167.4(4) 4_585 . . . ?
C3 C4 C7 O5 -17.7(5) . . . . ?
C5 C4 C7 O5 160.6(3) . . . . ?
C3 C4 C7 O6 163.7(3) . . . . ?
C5 C4 C7 O6 -18.1(5) . . . . ?
C19 N1 C8 C9 -1.6(7) . . . . ?
Sm1 N1 C8 C9 172.3(4) . . . . ?
N1 C8 C9 C10 0.0(8) . . . . ?
C8 C9 C10 C11 1.4(8) . . . . ?
C9 C10 C11 C19 -1.3(7) . . . . ?
C9 C10 C11 C12 177.2(5) . . . . ?
C10 C11 C12 C13 -175.5(6) . . . . ?
C19 C11 C12 C13 2.9(8) . . . . ?
C11 C12 C13 C14 0.0(10) . . . . ?
C12 C13 C14 C15 173.6(6) . . . . ?
C12 C13 C14 C18 -3.2(8) . . . . ?
C18 C14 C15 C16 0.2(7) . . . . ?
C13 C14 C15 C16 -176.7(5) . . . . ?
C14 C15 C16 C17 -3.3(7) . . . . ?
C18 N2 C17 C16 1.8(7) . . . . ?
Sm1 N2 C17 C16 -177.3(3) . . . . ?
C15 C16 C17 N2 2.4(8) . . . . ?
C17 N2 C18 C14 -5.1(6) . . . . ?
Sm1 N2 C18 C14 174.0(3) . . . . ?
C17 N2 C18 C19 172.7(4) . . . . ?
Sm1 N2 C18 C19 -8.2(5) . . . . ?
C15 C14 C18 N2 4.2(7) . . . . ?
C13 C14 C18 N2 -178.8(4) . . . . ?
C15 C14 C18 C19 -173.5(4) . . . . ?
C13 C14 C18 C19 3.5(7) . . . . ?
C8 N1 C19 C11 1.8(6) . . . . ?
Sm1 N1 C19 C11 -172.2(3) . . . . ?
C8 N1 C19 C18 -174.7(4) . . . . ?
Sm1 N1 C19 C18 11.3(5) . . . . ?
C10 C11 C19 N1 -0.4(7) . . . . ?
C12 C11 C19 N1 -178.9(4) . . . . ?
C10 C11 C19 C18 176.1(4) . . . . ?
C12 C11 C19 C18 -2.5(7) . . . . ?
N2 C18 C19 N1 -2.0(6) . . . . ?
C14 C18 C19 N1 175.8(4) . . . . ?
N2 C18 C19 C11 -178.6(4) . . . . ?
C14 C18 C19 C11 -0.7(6) . . . . ?

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
O1W H1W1 O4 0.85(4) 1.915(13) 2.752(4) 169(5) 2_745
O1W H1W2 O2 0.85(4) 2.049(12) 2.892(4) 173(4) 1_545
O1W H1W2 O3 0.85(4) 2.59(3) 3.106(4) 120(3) 1_545

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        27.56
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         0.872
_refine_diff_density_min         -0.755
_refine_diff_density_rms         0.131
####################################################################### 
# 
# 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_7-Yb
_database_code_depnum_ccdc_archive 'CCDC 1549875'
_audit_update_record             
;
2017-05-13 deposited with the CCDC.
2017-11-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C31 H20 N5 O9 S Yb'
_chemical_formula_sum            'C31 H20 N5 O9 S Yb'
_chemical_formula_weight         811.62

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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   11.60661(19)
_cell_length_b                   14.8753(2)
_cell_length_c                   17.4492(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 104.6085(17)
_cell_angle_gamma                90.00
_cell_volume                     2915.24(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    4488
_cell_measurement_theta_min      3.29
_cell_measurement_theta_max      27.56

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.849
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1596
_exptl_absorpt_coefficient_mu    3.347
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5264
_exptl_absorpt_correction_T_max  0.6337
_exptl_absorpt_process_details   
; 
CrysAlis Pro (Agilent, 2013)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1954
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10988
_diffrn_reflns_av_R_equivalents  0.0261
_diffrn_reflns_av_sigmaI/netI    0.0518
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         3.29
_diffrn_reflns_theta_max         27.56
_reflns_number_total             6653
_reflns_number_gt                5398
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_cell_refinement       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_data_reduction        
;
CrysAlis Pro (Agilent, 2013)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    '(K. Brandenburg, Diamond 3.1, 2009)'
_computing_publication_material  '(K. Brandenburg, Diamond 3.1, 2009)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0229P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6653
_refine_ls_number_parameters     430
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0344
_refine_ls_wR_factor_ref         0.0688
_refine_ls_wR_factor_gt          0.0631
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.034
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Yb1 Yb 0.310613(14) 0.390254(11) 0.747142(10) 0.02290(6) Uani 1 1 d . . .
S1 S 0.31429(9) 0.60867(7) 0.67280(6) 0.0282(2) Uani 1 1 d . . .
O1 O 0.3731(2) 0.52938(18) 0.71517(17) 0.0325(7) Uani 1 1 d . . .
O1W O 0.3903(3) 0.24863(18) 0.7743(2) 0.0401(8) Uani 1 1 d D . .
H1W1 H 0.4605(14) 0.229(3) 0.786(3) 0.060 Uiso 1 1 d D . .
H1W2 H 0.343(3) 0.211(2) 0.746(3) 0.060 Uiso 1 1 d D . .
O2 O 0.2627(3) 0.5903(2) 0.59047(18) 0.0482(9) Uani 1 1 d . . .
O3 O 0.3915(3) 0.68602(19) 0.6857(2) 0.0520(9) Uani 1 1 d . . .
O4 O 0.1688(2) 0.48388(18) 0.75560(17) 0.0321(7) Uani 1 1 d . . .
O5 O -0.0927(3) 0.4753(2) 0.7551(3) 0.0636(11) Uani 1 1 d . . .
O6 O -0.0039(3) 0.5175(3) 0.8737(2) 0.0728(12) Uani 1 1 d . . .
O7 O -0.1947(3) 0.6515(2) 0.7887(2) 0.0438(8) Uani 1 1 d . . .
O8 O -0.1554(2) 0.79302(18) 0.76411(18) 0.0353(7) Uani 1 1 d . . .
N1 N 0.2077(3) 0.3871(2) 0.6057(2) 0.0348(9) Uani 1 1 d . . .
N2 N 0.4450(3) 0.3642(2) 0.6533(2) 0.0326(8) Uani 1 1 d . . .
N3 N 0.5045(3) 0.4244(2) 0.8476(2) 0.0323(8) Uani 1 1 d . . .
N4 N 0.3049(3) 0.3727(2) 0.8881(2) 0.0342(8) Uani 1 1 d . . .
N5 N -0.0276(3) 0.5253(3) 0.8017(3) 0.0423(10) Uani 1 1 d . . .
C1 C 0.1960(3) 0.6352(3) 0.7150(2) 0.0256(9) Uani 1 1 d . . .
C2 C 0.1364(3) 0.5675(3) 0.7473(2) 0.0220(8) Uani 1 1 d . . .
C3 C 0.0339(3) 0.5974(2) 0.7697(2) 0.0245(9) Uani 1 1 d . . .
C4 C -0.0090(3) 0.6847(3) 0.7619(2) 0.0268(9) Uani 1 1 d . . .
C5 C 0.0576(4) 0.7483(3) 0.7334(3) 0.0382(11) Uani 1 1 d . . .
H5 H 0.0344 0.8084 0.7306 0.046 Uiso 1 1 calc R . .
C6 C 0.1573(3) 0.7237(3) 0.7095(3) 0.0330(10) Uani 1 1 d . . .
H6 H 0.1994 0.7671 0.6893 0.040 Uiso 1 1 calc R . .
C7 C -0.1294(4) 0.7111(3) 0.7740(2) 0.0291(9) Uani 1 1 d . . .
C8 C 0.0898(4) 0.3895(3) 0.5813(3) 0.0509(13) Uani 1 1 d . . .
H8 H 0.0460 0.3876 0.6192 0.061 Uiso 1 1 calc R . .
C9 C 0.0280(5) 0.3947(3) 0.5012(4) 0.0664(18) Uani 1 1 d . . .
H9 H -0.0548 0.3938 0.4860 0.080 Uiso 1 1 calc R . .
C10 C 0.0924(6) 0.4010(4) 0.4466(3) 0.0684(19) Uani 1 1 d . . .
H10 H 0.0531 0.4064 0.3933 0.082 Uiso 1 1 calc R . .
C11 C 0.2160(5) 0.3997(3) 0.4689(3) 0.0503(14) Uani 1 1 d . . .
C12 C 0.2886(7) 0.4049(4) 0.4143(3) 0.0667(18) Uani 1 1 d . . .
H12 H 0.2529 0.4139 0.3608 0.080 Uiso 1 1 calc R . .
C13 C 0.4066(7) 0.3970(3) 0.4381(3) 0.0650(17) Uani 1 1 d . . .
H13 H 0.4515 0.4006 0.4009 0.078 Uiso 1 1 calc R . .
C14 C 0.4654(5) 0.3832(3) 0.5193(3) 0.0478(13) Uani 1 1 d . . .
C15 C 0.5881(5) 0.3697(3) 0.5458(4) 0.0574(15) Uani 1 1 d . . .
H15 H 0.6361 0.3734 0.5106 0.069 Uiso 1 1 calc R . .
C16 C 0.6367(5) 0.3512(3) 0.6235(3) 0.0541(14) Uani 1 1 d . . .
H16 H 0.7182 0.3416 0.6423 0.065 Uiso 1 1 calc R . .
C17 C 0.5616(4) 0.3470(3) 0.6742(3) 0.0408(11) Uani 1 1 d . . .
H17 H 0.5952 0.3310 0.7266 0.049 Uiso 1 1 calc R . .
C18 C 0.3976(4) 0.3812(3) 0.5755(3) 0.0342(10) Uani 1 1 d . . .
C19 C 0.2715(4) 0.3902(3) 0.5503(2) 0.0359(11) Uani 1 1 d . . .
C20 C 0.6004(4) 0.4579(3) 0.8301(3) 0.0445(12) Uani 1 1 d . . .
H20 H 0.5931 0.4799 0.7792 0.053 Uiso 1 1 calc R . .
C21 C 0.7126(4) 0.4617(3) 0.8842(4) 0.0566(15) Uani 1 1 d . . .
H21 H 0.7786 0.4834 0.8688 0.068 Uiso 1 1 calc R . .
C22 C 0.7226(5) 0.4332(4) 0.9591(4) 0.0588(16) Uani 1 1 d . . .
H22 H 0.7969 0.4328 0.9952 0.071 Uiso 1 1 calc R . .
C23 C 0.6228(5) 0.4046(3) 0.9830(3) 0.0474(13) Uani 1 1 d . . .
C24 C 0.6230(6) 0.3824(3) 1.0625(3) 0.0653(18) Uani 1 1 d . . .
H24 H 0.6945 0.3837 1.1013 0.078 Uiso 1 1 calc R . .
C25 C 0.5235(7) 0.3599(4) 1.0825(3) 0.0656(18) Uani 1 1 d . . .
H25 H 0.5266 0.3470 1.1351 0.079 Uiso 1 1 calc R . .
C26 C 0.4132(5) 0.3552(3) 1.0254(3) 0.0492(14) Uani 1 1 d . . .
C27 C 0.3058(6) 0.3355(3) 1.0444(3) 0.0646(18) Uani 1 1 d . . .
H27 H 0.3051 0.3222 1.0963 0.078 Uiso 1 1 calc R . .
C28 C 0.2027(6) 0.3357(3) 0.9866(3) 0.0607(16) Uani 1 1 d . . .
H28 H 0.1308 0.3232 0.9988 0.073 Uiso 1 1 calc R . .
C29 C 0.2054(5) 0.3549(3) 0.9085(3) 0.0468(12) Uani 1 1 d . . .
H29 H 0.1340 0.3552 0.8694 0.056 Uiso 1 1 calc R . .
C30 C 0.4082(5) 0.3740(3) 0.9459(3) 0.0378(11) Uani 1 1 d . . .
C31 C 0.5141(4) 0.3993(3) 0.9235(3) 0.0338(10) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Yb1 O4 2.189(3) . ?
Yb1 O8 2.280(3) 2_546 ?
Yb1 O1W 2.301(3) . ?
Yb1 O1 2.307(3) . ?
Yb1 N1 2.456(3) . ?
Yb1 N4 2.491(4) . ?
Yb1 N3 2.531(3) . ?
Yb1 N2 2.559(4) . ?
Yb1 H1W2 2.69(3) . ?
S1 O2 1.436(3) . ?
S1 O3 1.441(3) . ?
S1 O1 1.466(3) . ?
S1 C1 1.758(4) . ?
O1W H1W1 0.85(4) . ?
O1W H1W2 0.85(4) . ?
O4 C2 1.297(4) . ?
O5 N5 1.215(5) . ?
O6 N5 1.222(5) . ?
O7 C7 1.235(5) . ?
O8 C7 1.256(4) . ?
O8 Yb1 2.280(3) 2_556 ?
N1 C8 1.327(6) . ?
N1 C19 1.358(6) . ?
N2 C17 1.335(5) . ?
N2 C18 1.354(5) . ?
N3 C20 1.324(5) . ?
N3 C31 1.354(5) . ?
N4 C29 1.318(6) . ?
N4 C30 1.360(6) . ?
N5 C3 1.474(5) . ?
C1 C6 1.387(5) . ?
C1 C2 1.417(5) . ?
C2 C3 1.414(5) . ?
C3 C4 1.385(5) . ?
C4 C5 1.391(6) . ?
C4 C7 1.517(5) . ?
C5 C6 1.376(6) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C8 C9 1.404(7) . ?
C8 H8 0.9300 . ?
C9 C10 1.354(9) . ?
C9 H9 0.9300 . ?
C10 C11 1.390(8) . ?
C10 H10 0.9300 . ?
C11 C19 1.412(6) . ?
C11 C12 1.424(8) . ?
C12 C13 1.332(8) . ?
C12 H12 0.9300 . ?
C13 C14 1.424(7) . ?
C13 H13 0.9300 . ?
C14 C15 1.396(7) . ?
C14 C18 1.404(6) . ?
C15 C16 1.359(7) . ?
C15 H15 0.9300 . ?
C16 C17 1.392(6) . ?
C16 H16 0.9300 . ?
C17 H17 0.9300 . ?
C18 C19 1.424(6) . ?
C20 C21 1.404(6) . ?
C20 H20 0.9300 . ?
C21 C22 1.352(7) . ?
C21 H21 0.9300 . ?
C22 C23 1.393(7) . ?
C22 H22 0.9300 . ?
C23 C31 1.420(6) . ?
C23 C24 1.424(8) . ?
C24 C25 1.332(8) . ?
C24 H24 0.9300 . ?
C25 C26 1.411(8) . ?
C25 H25 0.9300 . ?
C26 C30 1.400(6) . ?
C26 C27 1.400(8) . ?
C27 C28 1.356(8) . ?
C27 H27 0.9300 . ?
C28 C29 1.401(7) . ?
C28 H28 0.9300 . ?
C29 H29 0.9300 . ?
C30 C31 1.431(7) . ?

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 Yb1 O8 79.52(10) . 2_546 ?
O4 Yb1 O1W 146.97(11) . . ?
O8 Yb1 O1W 72.83(10) 2_546 . ?
O4 Yb1 O1 74.52(9) . . ?
O8 Yb1 O1 146.92(9) 2_546 . ?
O1W Yb1 O1 137.42(10) . . ?
O4 Yb1 N1 84.08(11) . . ?
O8 Yb1 N1 74.21(11) 2_546 . ?
O1W Yb1 N1 104.91(12) . . ?
O1 Yb1 N1 82.95(10) . . ?
O4 Yb1 N4 78.01(11) . . ?
O8 Yb1 N4 78.53(11) 2_546 . ?
O1W Yb1 N4 79.07(12) . . ?
O1 Yb1 N4 114.90(11) . . ?
N1 Yb1 N4 149.64(12) . . ?
O4 Yb1 N3 112.20(11) . . ?
O8 Yb1 N3 137.09(11) 2_546 . ?
O1W Yb1 N3 78.49(11) . . ?
O1 Yb1 N3 73.05(10) . . ?
N1 Yb1 N3 145.26(12) . . ?
N4 Yb1 N3 65.03(12) . . ?
O4 Yb1 N2 136.80(10) . . ?
O8 Yb1 N2 116.41(11) 2_546 . ?
O1W Yb1 N2 73.45(11) . . ?
O1 Yb1 N2 72.64(10) . . ?
N1 Yb1 N2 64.82(12) . . ?
N4 Yb1 N2 142.02(11) . . ?
N3 Yb1 N2 83.94(11) . . ?
O4 Yb1 H1W2 137.7(8) . . ?
O8 Yb1 H1W2 58.7(7) 2_546 . ?
O1W Yb1 H1W2 17.3(5) . . ?
O1 Yb1 H1W2 146.5(10) . . ?
N1 Yb1 H1W2 90.5(8) . . ?
N4 Yb1 H1W2 86.5(10) . . ?
N3 Yb1 H1W2 95.8(5) . . ?
N2 Yb1 H1W2 74.8(10) . . ?
O2 S1 O3 113.2(2) . . ?
O2 S1 O1 112.03(18) . . ?
O3 S1 O1 111.81(18) . . ?
O2 S1 C1 106.79(19) . . ?
O3 S1 C1 106.04(19) . . ?
O1 S1 C1 106.44(18) . . ?
S1 O1 Yb1 135.13(16) . . ?
Yb1 O1W H1W1 133(3) . . ?
Yb1 O1W H1W2 109(3) . . ?
H1W1 O1W H1W2 110.8(17) . . ?
C2 O4 Yb1 143.6(2) . . ?
C7 O8 Yb1 141.6(3) . 2_556 ?
C8 N1 C19 118.3(4) . . ?
C8 N1 Yb1 121.5(3) . . ?
C19 N1 Yb1 120.0(3) . . ?
C17 N2 C18 115.9(4) . . ?
C17 N2 Yb1 126.4(3) . . ?
C18 N2 Yb1 117.0(3) . . ?
C20 N3 C31 117.6(4) . . ?
C20 N3 Yb1 124.6(3) . . ?
C31 N3 Yb1 117.5(3) . . ?
C29 N4 C30 118.1(4) . . ?
C29 N4 Yb1 122.1(3) . . ?
C30 N4 Yb1 119.6(3) . . ?
O5 N5 O6 124.7(5) . . ?
O5 N5 C3 118.1(4) . . ?
O6 N5 C3 117.0(4) . . ?
C6 C1 C2 121.3(4) . . ?
C6 C1 S1 117.2(3) . . ?
C2 C1 S1 121.2(3) . . ?
O4 C2 C3 120.8(4) . . ?
O4 C2 C1 124.7(4) . . ?
C3 C2 C1 114.5(3) . . ?
C4 C3 C2 125.1(4) . . ?
C4 C3 N5 121.5(4) . . ?
C2 C3 N5 113.4(3) . . ?
C3 C4 C5 117.1(4) . . ?
C3 C4 C7 123.4(4) . . ?
C5 C4 C7 119.2(3) . . ?
C6 C5 C4 120.9(4) . . ?
C6 C5 H5 119.6 . . ?
C4 C5 H5 119.6 . . ?
C5 C6 C1 121.0(4) . . ?
C5 C6 H6 119.5 . . ?
C1 C6 H6 119.5 . . ?
O7 C7 O8 125.9(4) . . ?
O7 C7 C4 118.5(4) . . ?
O8 C7 C4 115.5(4) . . ?
N1 C8 C9 123.2(6) . . ?
N1 C8 H8 118.4 . . ?
C9 C8 H8 118.4 . . ?
C10 C9 C8 118.1(6) . . ?
C10 C9 H9 121.0 . . ?
C8 C9 H9 121.0 . . ?
C9 C10 C11 121.1(5) . . ?
C9 C10 H10 119.4 . . ?
C11 C10 H10 119.4 . . ?
C10 C11 C19 117.3(5) . . ?
C10 C11 C12 123.8(5) . . ?
C19 C11 C12 118.9(5) . . ?
C13 C12 C11 121.5(5) . . ?
C13 C12 H12 119.3 . . ?
C11 C12 H12 119.3 . . ?
C12 C13 C14 121.3(5) . . ?
C12 C13 H13 119.4 . . ?
C14 C13 H13 119.4 . . ?
C15 C14 C18 118.0(5) . . ?
C15 C14 C13 122.9(5) . . ?
C18 C14 C13 119.1(5) . . ?
C16 C15 C14 119.5(5) . . ?
C16 C15 H15 120.3 . . ?
C14 C15 H15 120.3 . . ?
C15 C16 C17 118.3(5) . . ?
C15 C16 H16 120.9 . . ?
C17 C16 H16 120.9 . . ?
N2 C17 C16 125.0(5) . . ?
N2 C17 H17 117.5 . . ?
C16 C17 H17 117.5 . . ?
N2 C18 C14 123.2(5) . . ?
N2 C18 C19 116.9(4) . . ?
C14 C18 C19 119.7(4) . . ?
N1 C19 C11 121.9(5) . . ?
N1 C19 C18 118.6(4) . . ?
C11 C19 C18 119.5(5) . . ?
N3 C20 C21 123.5(5) . . ?
N3 C20 H20 118.3 . . ?
C21 C20 H20 118.3 . . ?
C22 C21 C20 118.4(5) . . ?
C22 C21 H21 120.8 . . ?
C20 C21 H21 120.8 . . ?
C21 C22 C23 120.7(5) . . ?
C21 C22 H22 119.6 . . ?
C23 C22 H22 119.6 . . ?
C22 C23 C31 116.8(5) . . ?
C22 C23 C24 124.4(5) . . ?
C31 C23 C24 118.8(5) . . ?
C25 C24 C23 121.6(5) . . ?
C25 C24 H24 119.2 . . ?
C23 C24 H24 119.2 . . ?
C24 C25 C26 121.3(5) . . ?
C24 C25 H25 119.4 . . ?
C26 C25 H25 119.4 . . ?
C30 C26 C27 117.3(5) . . ?
C30 C26 C25 119.5(6) . . ?
C27 C26 C25 123.1(5) . . ?
C28 C27 C26 119.7(5) . . ?
C28 C27 H27 120.2 . . ?
C26 C27 H27 120.2 . . ?
C27 C28 C29 119.4(5) . . ?
C27 C28 H28 120.3 . . ?
C29 C28 H28 120.3 . . ?
N4 C29 C28 122.7(5) . . ?
N4 C29 H29 118.7 . . ?
C28 C29 H29 118.7 . . ?
N4 C30 C26 122.7(5) . . ?
N4 C30 C31 117.3(4) . . ?
C26 C30 C31 119.9(5) . . ?
N3 C31 C23 122.6(5) . . ?
N3 C31 C30 118.4(4) . . ?
C23 C31 C30 118.7(4) . . ?

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
O2 S1 O1 Yb1 -65.5(3) . . . . ?
O3 S1 O1 Yb1 166.3(2) . . . . ?
C1 S1 O1 Yb1 50.9(3) . . . . ?
O4 Yb1 O1 S1 -35.8(2) . . . . ?
O8 Yb1 O1 S1 3.7(4) 2_546 . . . ?
O1W Yb1 O1 S1 154.3(2) . . . . ?
N1 Yb1 O1 S1 49.9(2) . . . . ?
N4 Yb1 O1 S1 -104.4(2) . . . . ?
N3 Yb1 O1 S1 -155.5(3) . . . . ?
N2 Yb1 O1 S1 115.7(3) . . . . ?
O8 Yb1 O4 C2 -158.7(4) 2_546 . . . ?
O1W Yb1 O4 C2 167.9(4) . . . . ?
O1 Yb1 O4 C2 0.5(4) . . . . ?
N1 Yb1 O4 C2 -83.8(4) . . . . ?
N4 Yb1 O4 C2 120.9(4) . . . . ?
N3 Yb1 O4 C2 64.4(4) . . . . ?
N2 Yb1 O4 C2 -41.1(5) . . . . ?
O4 Yb1 N1 C8 -37.4(3) . . . . ?
O8 Yb1 N1 C8 43.3(3) 2_546 . . . ?
O1W Yb1 N1 C8 110.2(3) . . . . ?
O1 Yb1 N1 C8 -112.5(3) . . . . ?
N4 Yb1 N1 C8 16.4(4) . . . . ?
N3 Yb1 N1 C8 -158.6(3) . . . . ?
N2 Yb1 N1 C8 173.4(4) . . . . ?
O4 Yb1 N1 C19 137.1(3) . . . . ?
O8 Yb1 N1 C19 -142.1(3) 2_546 . . . ?
O1W Yb1 N1 C19 -75.2(3) . . . . ?
O1 Yb1 N1 C19 62.1(3) . . . . ?
N4 Yb1 N1 C19 -169.0(3) . . . . ?
N3 Yb1 N1 C19 16.0(4) . . . . ?
N2 Yb1 N1 C19 -12.0(3) . . . . ?
O4 Yb1 N2 C17 136.4(3) . . . . ?
O8 Yb1 N2 C17 -120.2(3) 2_546 . . . ?
O1W Yb1 N2 C17 -59.6(3) . . . . ?
O1 Yb1 N2 C17 94.2(3) . . . . ?
N1 Yb1 N2 C17 -175.5(4) . . . . ?
N4 Yb1 N2 C17 -14.2(4) . . . . ?
N3 Yb1 N2 C17 20.1(3) . . . . ?
O4 Yb1 N2 C18 -34.2(3) . . . . ?
O8 Yb1 N2 C18 69.2(3) 2_546 . . . ?
O1W Yb1 N2 C18 129.8(3) . . . . ?
O1 Yb1 N2 C18 -76.3(3) . . . . ?
N1 Yb1 N2 C18 13.9(3) . . . . ?
N4 Yb1 N2 C18 175.2(2) . . . . ?
N3 Yb1 N2 C18 -150.4(3) . . . . ?
O4 Yb1 N3 C20 -109.3(3) . . . . ?
O8 Yb1 N3 C20 152.0(3) 2_546 . . . ?
O1W Yb1 N3 C20 103.4(4) . . . . ?
O1 Yb1 N3 C20 -44.5(3) . . . . ?
N1 Yb1 N3 C20 3.8(5) . . . . ?
N4 Yb1 N3 C20 -173.4(4) . . . . ?
N2 Yb1 N3 C20 29.1(3) . . . . ?
O4 Yb1 N3 C31 76.8(3) . . . . ?
O8 Yb1 N3 C31 -21.8(4) 2_546 . . . ?
O1W Yb1 N3 C31 -70.4(3) . . . . ?
O1 Yb1 N3 C31 141.6(3) . . . . ?
N1 Yb1 N3 C31 -170.0(3) . . . . ?
N4 Yb1 N3 C31 12.8(3) . . . . ?
N2 Yb1 N3 C31 -144.7(3) . . . . ?
O4 Yb1 N4 C29 52.5(3) . . . . ?
O8 Yb1 N4 C29 -29.1(3) 2_546 . . . ?
O1W Yb1 N4 C29 -103.6(4) . . . . ?
O1 Yb1 N4 C29 118.9(3) . . . . ?
N1 Yb1 N4 C29 -2.7(5) . . . . ?
N3 Yb1 N4 C29 174.1(4) . . . . ?
N2 Yb1 N4 C29 -147.6(3) . . . . ?
O4 Yb1 N4 C30 -133.1(3) . . . . ?
O8 Yb1 N4 C30 145.3(3) 2_546 . . . ?
O1W Yb1 N4 C30 70.8(3) . . . . ?
O1 Yb1 N4 C30 -66.7(3) . . . . ?
N1 Yb1 N4 C30 171.7(3) . . . . ?
N3 Yb1 N4 C30 -11.5(3) . . . . ?
N2 Yb1 N4 C30 26.8(4) . . . . ?
O2 S1 C1 C6 -85.5(3) . . . . ?
O3 S1 C1 C6 35.5(4) . . . . ?
O1 S1 C1 C6 154.7(3) . . . . ?
O2 S1 C1 C2 89.4(3) . . . . ?
O3 S1 C1 C2 -149.6(3) . . . . ?
O1 S1 C1 C2 -30.4(3) . . . . ?
Yb1 O4 C2 C3 -172.7(3) . . . . ?
Yb1 O4 C2 C1 8.4(6) . . . . ?
C6 C1 C2 O4 -178.7(4) . . . . ?
S1 C1 C2 O4 6.6(5) . . . . ?
C6 C1 C2 C3 2.4(5) . . . . ?
S1 C1 C2 C3 -172.3(3) . . . . ?
O4 C2 C3 C4 -178.8(4) . . . . ?
C1 C2 C3 C4 0.2(6) . . . . ?
O4 C2 C3 N5 -0.1(5) . . . . ?
C1 C2 C3 N5 178.9(3) . . . . ?
O5 N5 C3 C4 98.7(5) . . . . ?
O6 N5 C3 C4 -85.2(5) . . . . ?
O5 N5 C3 C2 -80.0(5) . . . . ?
O6 N5 C3 C2 96.1(4) . . . . ?
C2 C3 C4 C5 -3.4(6) . . . . ?
N5 C3 C4 C5 178.0(4) . . . . ?
C2 C3 C4 C7 169.8(4) . . . . ?
N5 C3 C4 C7 -8.8(6) . . . . ?
C3 C4 C5 C6 4.1(6) . . . . ?
C7 C4 C5 C6 -169.3(4) . . . . ?
C4 C5 C6 C1 -1.7(7) . . . . ?
C2 C1 C6 C5 -1.7(6) . . . . ?
S1 C1 C6 C5 173.2(3) . . . . ?
Yb1 O8 C7 O7 -6.9(7) 2_556 . . . ?
Yb1 O8 C7 C4 169.5(3) 2_556 . . . ?
C3 C4 C7 O7 -2.9(6) . . . . ?
C5 C4 C7 O7 170.2(4) . . . . ?
C3 C4 C7 O8 -179.5(4) . . . . ?
C5 C4 C7 O8 -6.5(6) . . . . ?
C19 N1 C8 C9 0.3(7) . . . . ?
Yb1 N1 C8 C9 175.0(3) . . . . ?
N1 C8 C9 C10 -2.6(8) . . . . ?
C8 C9 C10 C11 1.9(9) . . . . ?
C9 C10 C11 C19 0.8(8) . . . . ?
C9 C10 C11 C12 179.1(5) . . . . ?
C10 C11 C12 C13 -175.3(5) . . . . ?
C19 C11 C12 C13 3.0(8) . . . . ?
C11 C12 C13 C14 -0.1(9) . . . . ?
C12 C13 C14 C15 176.4(5) . . . . ?
C12 C13 C14 C18 -2.4(8) . . . . ?
C18 C14 C15 C16 3.0(7) . . . . ?
C13 C14 C15 C16 -175.8(5) . . . . ?
C14 C15 C16 C17 -0.5(8) . . . . ?
C18 N2 C17 C16 4.4(7) . . . . ?
Yb1 N2 C17 C16 -166.2(4) . . . . ?
C15 C16 C17 N2 -3.5(8) . . . . ?
C17 N2 C18 C14 -1.5(6) . . . . ?
Yb1 N2 C18 C14 170.0(3) . . . . ?
C17 N2 C18 C19 173.5(4) . . . . ?
Yb1 N2 C18 C19 -15.0(5) . . . . ?
C15 C14 C18 N2 -2.1(7) . . . . ?
C13 C14 C18 N2 176.8(4) . . . . ?
C15 C14 C18 C19 -176.9(4) . . . . ?
C13 C14 C18 C19 1.9(7) . . . . ?
C8 N1 C19 C11 2.7(6) . . . . ?
Yb1 N1 C19 C11 -172.1(3) . . . . ?
C8 N1 C19 C18 -175.6(4) . . . . ?
Yb1 N1 C19 C18 9.7(5) . . . . ?
C10 C11 C19 N1 -3.3(7) . . . . ?
C12 C11 C19 N1 178.4(4) . . . . ?
C10 C11 C19 C18 175.0(4) . . . . ?
C12 C11 C19 C18 -3.4(7) . . . . ?
N2 C18 C19 N1 4.1(6) . . . . ?
C14 C18 C19 N1 179.2(4) . . . . ?
N2 C18 C19 C11 -174.2(4) . . . . ?
C14 C18 C19 C11 0.9(6) . . . . ?
C31 N3 C20 C21 5.3(7) . . . . ?
Yb1 N3 C20 C21 -168.5(3) . . . . ?
N3 C20 C21 C22 -2.8(8) . . . . ?
C20 C21 C22 C23 -2.9(8) . . . . ?
C21 C22 C23 C31 5.4(7) . . . . ?
C21 C22 C23 C24 -173.2(5) . . . . ?
C22 C23 C24 C25 176.4(5) . . . . ?
C31 C23 C24 C25 -2.2(8) . . . . ?
C23 C24 C25 C26 1.3(9) . . . . ?
C24 C25 C26 C30 0.5(8) . . . . ?
C24 C25 C26 C27 -177.3(5) . . . . ?
C30 C26 C27 C28 -0.4(7) . . . . ?
C25 C26 C27 C28 177.4(5) . . . . ?
C26 C27 C28 C29 0.6(8) . . . . ?
C30 N4 C29 C28 -1.3(7) . . . . ?
Yb1 N4 C29 C28 173.2(4) . . . . ?
C27 C28 C29 N4 0.3(8) . . . . ?
C29 N4 C30 C26 1.5(6) . . . . ?
Yb1 N4 C30 C26 -173.2(3) . . . . ?
C29 N4 C30 C31 -175.9(4) . . . . ?
Yb1 N4 C30 C31 9.5(5) . . . . ?
C27 C26 C30 N4 -0.6(7) . . . . ?
C25 C26 C30 N4 -178.5(4) . . . . ?
C27 C26 C30 C31 176.7(4) . . . . ?
C25 C26 C30 C31 -1.2(7) . . . . ?
C20 N3 C31 C23 -2.4(6) . . . . ?
Yb1 N3 C31 C23 171.9(3) . . . . ?
C20 N3 C31 C30 172.1(4) . . . . ?
Yb1 N3 C31 C30 -13.6(5) . . . . ?
C22 C23 C31 N3 -2.9(6) . . . . ?
C24 C23 C31 N3 175.8(4) . . . . ?
C22 C23 C31 C30 -177.3(4) . . . . ?
C24 C23 C31 C30 1.4(6) . . . . ?
N4 C30 C31 N3 3.0(6) . . . . ?
C26 C30 C31 N3 -174.4(4) . . . . ?
N4 C30 C31 C23 177.7(4) . . . . ?
C26 C30 C31 C23 0.3(6) . . . . ?

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
O1W H1W1 O3 0.85(4) 1.779(11) 2.622(4) 179(5) 2_646
O1W H1W2 O7 0.85(4) 1.90(2) 2.682(4) 154(4) 2_546

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        27.56
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         0.991
_refine_diff_density_min         -0.682
_refine_diff_density_rms         0.112
####################################################################### 
# 
# 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_7-Lu
_database_code_depnum_ccdc_archive 'CCDC 1549876'
_audit_update_record             
;
2017-05-13 deposited with the CCDC.
2017-11-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C31 H20 Lu N5 O9 S'
_chemical_formula_sum            'C31 H20 Lu N5 O9 S'
_chemical_formula_weight         813.55

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'
Lu Lu -0.4720 5.8584 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   11.6033(3)
_cell_length_b                   14.8669(4)
_cell_length_c                   17.4306(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 104.603(3)
_cell_angle_gamma                90.00
_cell_volume                     2909.72(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    3730
_cell_measurement_theta_min      3.29
_cell_measurement_theta_max      27.56

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.857
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1600
_exptl_absorpt_coefficient_mu    3.532
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5689
_exptl_absorpt_correction_T_max  0.6766
_exptl_absorpt_process_details   
; 
CrysAlis Pro (Agilent, 2013)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1954
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8913
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_av_sigmaI/netI    0.0533
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.29
_diffrn_reflns_theta_max         25.01
_reflns_number_total             5095
_reflns_number_gt                4379
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_cell_refinement       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_data_reduction        
;
CrysAlis Pro (Agilent, 2013)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    '(K. Brandenburg, Diamond 3.1, 2009)'
_computing_publication_material  '(K. Brandenburg, Diamond 3.1, 2009)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1020P)²+201.3370P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5095
_refine_ls_number_parameters     370
_refine_ls_number_restraints     74
_refine_ls_R_factor_all          0.0889
_refine_ls_R_factor_gt           0.0809
_refine_ls_wR_factor_ref         0.2405
_refine_ls_wR_factor_gt          0.2351
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.037
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Lu1 Lu 1.31032(6) 1.10960(4) 0.24739(4) 0.0230(3) Uani 1 1 d . . .
S1 S 1.3139(4) 0.8918(3) 0.1730(3) 0.0271(9) Uani 1 1 d . . .
O1 O 1.3733(10) 0.9705(8) 0.2139(8) 0.035(3) Uani 1 1 d . . .
O1W O 1.3910(11) 1.2510(9) 0.2753(10) 0.043(3) Uani 1 1 d D . .
H1W1 H 1.346(14) 1.288(10) 0.244(12) 0.065 Uiso 1 1 d D . .
H1W2 H 1.457(10) 1.277(11) 0.297(12) 0.065 Uiso 1 1 d D . .
O2 O 1.3907(11) 0.8157(9) 0.1861(11) 0.053(4) Uani 1 1 d . . .
O3 O 1.2630(14) 0.9096(11) 0.0902(8) 0.050(4) Uani 1 1 d . . .
O4 O 1.1681(10) 1.0170(8) 0.2562(7) 0.033(3) Uani 1 1 d . . .
O5 O 0.9969(15) 0.9828(14) 0.3735(10) 0.071(5) Uani 1 1 d . . .
O6 O 0.9077(15) 1.0246(10) 0.2560(11) 0.063(5) Uani 1 1 d . . .
O7 O 0.8045(12) 0.8480(10) 0.2883(9) 0.047(4) Uani 1 1 d . . .
O8 O 0.8444(11) 0.7061(8) 0.2635(8) 0.038(3) Uani 1 1 d . . .
N2 N 1.5040(13) 1.0759(10) 0.3467(9) 0.033(3) Uani 1 1 d . . .
N3 N 1.4445(13) 1.1343(10) 0.1555(9) 0.033(3) Uani 1 1 d . . .
N4 N 1.2071(13) 1.1130(10) 0.1060(9) 0.037(4) Uani 1 1 d . . .
N5 N 0.9722(14) 0.9747(11) 0.3017(10) 0.040(4) Uani 1 1 d . . .
C1 C 1.1946(15) 0.8639(12) 0.2151(11) 0.031(4) Uani 1 1 d . . .
C2 C 1.1367(14) 0.9330(11) 0.2475(10) 0.024(3) Uani 1 1 d . . .
C3 C 1.0344(14) 0.9025(11) 0.2708(10) 0.025(3) Uani 1 1 d . . .
C4 C 0.9924(14) 0.8150(12) 0.2621(10) 0.028(4) Uani 1 1 d . . .
C5 C 1.0582(15) 0.7510(12) 0.2317(11) 0.033(4) Uani 1 1 d . . .
H5 H 1.0330 0.6914 0.2264 0.040 Uiso 1 1 calc R . .
C6 C 1.1580(17) 0.7755(13) 0.2101(12) 0.037(4) Uani 1 1 d . . .
H6 H 1.2022 0.7321 0.1916 0.045 Uiso 1 1 calc R . .
C7 C 0.8708(15) 0.7890(12) 0.2738(10) 0.030(4) Uani 1 1 d . . .
N1 N 1.3039(16) 1.1264(11) 0.3899(9) 0.039(4) Uani 1 1 d . . .
C8 C 1.205(2) 1.1445(15) 0.4091(13) 0.048(5) Uani 1 1 d U . .
H8 H 1.1338 1.1451 0.3696 0.058 Uiso 1 1 calc R . .
C9 C 1.201(2) 1.1631(16) 0.4874(12) 0.060(3) Uani 1 1 d DU . .
H9 H 1.1298 1.1751 0.5002 0.073 Uiso 1 1 calc R . .
C10 C 1.3075(17) 1.1630(16) 0.5446(13) 0.060(3) Uani 1 1 d DU . .
H10 H 1.3089 1.1753 0.5972 0.073 Uiso 1 1 calc R . .
C11 C 1.412(2) 1.1445(16) 0.5234(14) 0.060(3) Uani 1 1 d DU . .
C12 C 1.531(2) 1.1363(16) 0.5812(15) 0.060(3) Uani 1 1 d . . .
H12 H 1.5350 1.1466 0.6345 0.073 Uiso 1 1 calc R . .
C13 C 1.626(3) 1.1163(16) 0.5621(15) 0.060(3) Uani 1 1 d . . .
H13 H 1.6971 1.1148 0.6011 0.073 Uiso 1 1 calc R . .
C14 C 1.626(2) 1.0957(15) 0.4816(13) 0.050(5) Uani 1 1 d . . .
C15 C 1.720(2) 1.067(2) 0.4615(16) 0.071(8) Uani 1 1 d . . .
H15 H 1.7939 1.0658 0.4983 0.085 Uiso 1 1 calc R . .
C16 C 1.7084(18) 1.0383(17) 0.3837(17) 0.061(7) Uani 1 1 d . . .
H16 H 1.7748 1.0170 0.3686 0.073 Uiso 1 1 calc R . .
C17 C 1.6003(18) 1.0412(15) 0.3293(13) 0.045(5) Uani 1 1 d . . .
H17 H 1.5939 1.0183 0.2788 0.054 Uiso 1 1 calc R . .
C18 C 1.5107(19) 1.1010(12) 0.4210(11) 0.040(5) Uani 1 1 d . . .
C19 C 1.4086(17) 1.1266(12) 0.4458(11) 0.036(4) Uani 1 1 d . . .
C20 C 1.562(2) 1.1532(13) 0.1755(13) 0.047(5) Uani 1 1 d . . .
H20 H 1.5951 1.1717 0.2273 0.056 Uiso 1 1 calc R . .
C21 C 1.637(2) 1.1471(16) 0.1249(15) 0.056(6) Uani 1 1 d . . .
H21 H 1.7191 1.1548 0.1437 0.067 Uiso 1 1 calc R . .
C22 C 1.587(2) 1.1293(16) 0.0463(14) 0.055(6) Uani 1 1 d . . .
H22 H 1.6349 1.1258 0.0112 0.066 Uiso 1 1 calc R . .
C23 C 1.468(2) 1.1169(15) 0.0192(10) 0.052(2) Uani 1 1 d DU . .
C24 C 1.4175(16) 1.1038(14) -0.0607(10) 0.052(2) Uani 1 1 d DU . .
H24 H 1.4641 1.0962 -0.0964 0.062 Uiso 1 1 calc R . .
C25 C 1.2962(16) 1.1026(14) -0.0846(12) 0.052(2) Uani 1 1 d DU . .
H25 H 1.2605 1.1046 -0.1387 0.062 Uiso 1 1 calc R . .
C26 C 1.223(2) 1.0987(15) -0.0327(12) 0.052(2) Uani 1 1 d DU . .
C27 C 1.107(2) 1.0958(15) -0.0478(14) 0.052(2) Uani 1 1 d U . .
H27 H 1.0666 1.0855 -0.1003 0.062 Uiso 1 1 calc R . .
C28 C 1.037(2) 1.1063(14) 0.0057(13) 0.052(2) Uani 1 1 d U . .
H28 H 0.9550 1.1108 -0.0124 0.062 Uiso 1 1 calc R . .
C29 C 1.084(2) 1.1097(14) 0.0764(13) 0.052(2) Uani 1 1 d U . .
H29 H 1.0365 1.1099 0.1119 0.062 Uiso 1 1 calc R . .
C30 C 1.2683(18) 1.1098(12) 0.0520(11) 0.034(4) Uani 1 1 d . . .
C31 C 1.397(2) 1.1195(12) 0.0762(11) 0.040(5) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Lu1 O4 2.184(11) . ?
Lu1 O8 2.269(12) 2_755 ?
Lu1 O1W 2.303(12) . ?
Lu1 O1 2.317(12) . ?
Lu1 N4 2.455(15) . ?
Lu1 N1 2.515(15) . ?
Lu1 N2 2.517(16) . ?
Lu1 N3 2.525(14) . ?
S1 O2 1.422(14) . ?
S1 O3 1.440(14) . ?
S1 O1 1.450(12) . ?
S1 C1 1.772(18) . ?
O1W H1W1 0.85(5) . ?
O1W H1W2 0.85(5) . ?
O4 C2 1.30(2) . ?
O5 N5 1.22(2) . ?
O6 N5 1.20(2) . ?
O7 C7 1.23(2) . ?
O8 C7 1.27(2) . ?
O8 Lu1 2.269(12) 2_745 ?
N2 C17 1.33(2) . ?
N2 C18 1.33(2) . ?
N3 C20 1.35(3) . ?
N3 C31 1.37(2) . ?
N4 C30 1.31(2) . ?
N4 C29 1.39(3) . ?
N5 C3 1.47(2) . ?
C1 C6 1.38(2) . ?
C1 C2 1.42(2) . ?
C2 C3 1.42(2) . ?
C3 C4 1.39(2) . ?
C4 C5 1.40(2) . ?
C4 C7 1.53(2) . ?
C5 C6 1.36(3) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
N1 C8 1.31(3) . ?
N1 C19 1.35(3) . ?
C8 C9 1.40(3) . ?
C8 H8 0.9300 . ?
C9 C10 1.376(10) . ?
C9 H9 0.9300 . ?
C10 C11 1.383(10) . ?
C10 H10 0.9300 . ?
C11 C19 1.37(3) . ?
C11 C12 1.49(3) . ?
C12 C13 1.27(4) . ?
C12 H12 0.9300 . ?
C13 C14 1.44(3) . ?
C13 H13 0.9300 . ?
C14 C15 1.30(4) . ?
C14 C18 1.48(3) . ?
C15 C16 1.40(4) . ?
C15 H15 0.9300 . ?
C16 C17 1.37(3) . ?
C16 H16 0.9300 . ?
C17 H17 0.9300 . ?
C18 C19 1.41(3) . ?
C20 C21 1.39(3) . ?
C20 H20 0.9300 . ?
C21 C22 1.37(3) . ?
C21 H21 0.9300 . ?
C22 C23 1.35(3) . ?
C22 H22 0.9300 . ?
C23 C24 1.381(10) . ?
C23 C31 1.44(3) . ?
C24 C25 1.363(10) . ?
C24 H24 0.9300 . ?
C25 C26 1.391(10) . ?
C25 H25 0.9300 . ?
C26 C27 1.30(3) . ?
C26 C30 1.45(3) . ?
C27 C28 1.39(3) . ?
C27 H27 0.9300 . ?
C28 C29 1.22(3) . ?
C28 H28 0.9300 . ?
C29 H29 0.9300 . ?
C30 C31 1.45(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 Lu1 O8 79.0(5) . 2_755 ?
O4 Lu1 O1W 146.6(5) . . ?
O8 Lu1 O1W 73.2(5) 2_755 . ?
O4 Lu1 O1 75.3(4) . . ?
O8 Lu1 O1 146.8(4) 2_755 . ?
O1W Lu1 O1 137.0(4) . . ?
O4 Lu1 N4 84.1(5) . . ?
O8 Lu1 N4 74.2(5) 2_755 . ?
O1W Lu1 N4 105.2(5) . . ?
O1 Lu1 N4 82.6(5) . . ?
O4 Lu1 N1 77.4(5) . . ?
O8 Lu1 N1 78.5(5) 2_755 . ?
O1W Lu1 N1 79.2(6) . . ?
O1 Lu1 N1 115.3(5) . . ?
N4 Lu1 N1 149.4(6) . . ?
O4 Lu1 N2 112.7(5) . . ?
O8 Lu1 N2 137.2(5) 2_755 . ?
O1W Lu1 N2 78.0(5) . . ?
O1 Lu1 N2 73.2(5) . . ?
N4 Lu1 N2 145.1(5) . . ?
N1 Lu1 N2 65.4(5) . . ?
O4 Lu1 N3 137.2(5) . . ?
O8 Lu1 N3 117.1(5) 2_755 . ?
O1W Lu1 N3 73.6(5) . . ?
O1 Lu1 N3 71.7(5) . . ?
N4 Lu1 N3 65.4(5) . . ?
N1 Lu1 N3 142.0(5) . . ?
N2 Lu1 N3 83.0(5) . . ?
O2 S1 O3 112.9(10) . . ?
O2 S1 O1 111.2(8) . . ?
O3 S1 O1 111.6(9) . . ?
O2 S1 C1 105.7(8) . . ?
O3 S1 C1 107.0(9) . . ?
O1 S1 C1 108.0(8) . . ?
S1 O1 Lu1 134.7(7) . . ?
Lu1 O1W H1W1 107(10) . . ?
Lu1 O1W H1W2 141(10) . . ?
H1W1 O1W H1W2 109.8(19) . . ?
C2 O4 Lu1 142.5(11) . . ?
C7 O8 Lu1 141.5(11) . 2_745 ?
C17 N2 C18 118.9(18) . . ?
C17 N2 Lu1 125.1(13) . . ?
C18 N2 Lu1 115.8(12) . . ?
C20 N3 C31 114.7(17) . . ?
C20 N3 Lu1 127.6(13) . . ?
C31 N3 Lu1 117.5(12) . . ?
C30 N4 C29 115.0(17) . . ?
C30 N4 Lu1 120.2(12) . . ?
C29 N4 Lu1 124.6(14) . . ?
O6 N5 O5 124.5(19) . . ?
O6 N5 C3 119.2(16) . . ?
O5 N5 C3 116.1(18) . . ?
C6 C1 C2 123.1(16) . . ?
C6 C1 S1 117.2(14) . . ?
C2 C1 S1 119.5(13) . . ?
O4 C2 C3 120.2(14) . . ?
O4 C2 C1 126.5(15) . . ?
C3 C2 C1 113.3(14) . . ?
C4 C3 C2 124.3(15) . . ?
C4 C3 N5 122.3(14) . . ?
C2 C3 N5 113.3(14) . . ?
C3 C4 C5 117.9(15) . . ?
C3 C4 C7 122.3(15) . . ?
C5 C4 C7 119.2(15) . . ?
C6 C5 C4 120.5(17) . . ?
C6 C5 H5 119.7 . . ?
C4 C5 H5 119.7 . . ?
C5 C6 C1 120.6(18) . . ?
C5 C6 H6 119.7 . . ?
C1 C6 H6 119.7 . . ?
O7 C7 O8 125.3(16) . . ?
O7 C7 C4 119.6(15) . . ?
O8 C7 C4 115.1(15) . . ?
C8 N1 C19 120.2(17) . . ?
C8 N1 Lu1 121.4(14) . . ?
C19 N1 Lu1 117.9(13) . . ?
N1 C8 C9 122(2) . . ?
N1 C8 H8 118.9 . . ?
C9 C8 H8 118.9 . . ?
C10 C9 C8 118(2) . . ?
C10 C9 H9 121.1 . . ?
C8 C9 H9 121.1 . . ?
C9 C10 C11 119(2) . . ?
C9 C10 H10 120.3 . . ?
C11 C10 H10 120.3 . . ?
C19 C11 C10 120(2) . . ?
C19 C11 C12 116(2) . . ?
C10 C11 C12 124(2) . . ?
C13 C12 C11 124(2) . . ?
C13 C12 H12 118.0 . . ?
C11 C12 H12 118.0 . . ?
C12 C13 C14 121(3) . . ?
C12 C13 H13 119.3 . . ?
C14 C13 H13 119.3 . . ?
C15 C14 C13 123(2) . . ?
C15 C14 C18 120(2) . . ?
C13 C14 C18 117(2) . . ?
C14 C15 C16 119(2) . . ?
C14 C15 H15 120.7 . . ?
C16 C15 H15 120.7 . . ?
C17 C16 C15 121(2) . . ?
C17 C16 H16 119.6 . . ?
C15 C16 H16 119.6 . . ?
N2 C17 C16 122(2) . . ?
N2 C17 H17 119.0 . . ?
C16 C17 H17 119.0 . . ?
N2 C18 C19 121.7(17) . . ?
N2 C18 C14 120(2) . . ?
C19 C18 C14 118.2(19) . . ?
N1 C19 C11 120.7(19) . . ?
N1 C19 C18 116.7(17) . . ?
C11 C19 C18 122.4(19) . . ?
N3 C20 C21 125(2) . . ?
N3 C20 H20 117.4 . . ?
C21 C20 H20 117.4 . . ?
C22 C21 C20 118(2) . . ?
C22 C21 H21 121.1 . . ?
C20 C21 H21 121.1 . . ?
C23 C22 C21 121(2) . . ?
C23 C22 H22 119.4 . . ?
C21 C22 H22 119.4 . . ?
C22 C23 C24 120(2) . . ?
C22 C23 C31 117.6(18) . . ?
C24 C23 C31 122(2) . . ?
C25 C24 C23 117(2) . . ?
C25 C24 H24 121.6 . . ?
C23 C24 H24 121.6 . . ?
C24 C25 C26 124(2) . . ?
C24 C25 H25 118.1 . . ?
C26 C25 H25 118.1 . . ?
C27 C26 C25 130(2) . . ?
C27 C26 C30 107.6(18) . . ?
C25 C26 C30 122(2) . . ?
C26 C27 C28 127(2) . . ?
C26 C27 H27 116.3 . . ?
C28 C27 H27 116.3 . . ?
C29 C28 C27 120(3) . . ?
C29 C28 H28 120.1 . . ?
C27 C28 H28 120.1 . . ?
C28 C29 N4 122(2) . . ?
C28 C29 H29 118.8 . . ?
N4 C29 H29 118.8 . . ?
N4 C30 C31 119.4(16) . . ?
N4 C30 C26 127.6(18) . . ?
C31 C30 C26 113.0(16) . . ?
N3 C31 C23 123(2) . . ?
N3 C31 C30 115.5(16) . . ?
C23 C31 C30 121.3(17) . . ?

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
O2 S1 O1 Lu1 -164.8(11) . . . . ?
O3 S1 O1 Lu1 68.1(13) . . . . ?
C1 S1 O1 Lu1 -49.3(13) . . . . ?
O4 Lu1 O1 S1 34.1(11) . . . . ?
O8 Lu1 O1 S1 -6.3(17) 2_755 . . . ?
O1W Lu1 O1 S1 -156.1(10) . . . . ?
N4 Lu1 O1 S1 -51.7(11) . . . . ?
N1 Lu1 O1 S1 102.3(12) . . . . ?
N2 Lu1 O1 S1 153.8(12) . . . . ?
N3 Lu1 O1 S1 -118.1(12) . . . . ?
O8 Lu1 O4 C2 158.6(19) 2_755 . . . ?
O1W Lu1 O4 C2 -167.5(17) . . . . ?
O1 Lu1 O4 C2 -0.2(18) . . . . ?
N4 Lu1 O4 C2 83.7(19) . . . . ?
N1 Lu1 O4 C2 -120.8(19) . . . . ?
N2 Lu1 O4 C2 -64.5(19) . . . . ?
N3 Lu1 O4 C2 40(2) . . . . ?
O4 Lu1 N2 C17 108.7(15) . . . . ?
O8 Lu1 N2 C17 -152.9(14) 2_755 . . . ?
O1W Lu1 N2 C17 -104.5(16) . . . . ?
O1 Lu1 N2 C17 43.1(15) . . . . ?
N4 Lu1 N2 C17 -5(2) . . . . ?
N1 Lu1 N2 C17 172.0(17) . . . . ?
N3 Lu1 N2 C17 -29.9(15) . . . . ?
O4 Lu1 N2 C18 -76.1(13) . . . . ?
O8 Lu1 N2 C18 22.3(16) 2_755 . . . ?
O1W Lu1 N2 C18 70.6(13) . . . . ?
O1 Lu1 N2 C18 -141.7(13) . . . . ?
N4 Lu1 N2 C18 170.1(12) . . . . ?
N1 Lu1 N2 C18 -12.9(12) . . . . ?
N3 Lu1 N2 C18 145.3(13) . . . . ?
O4 Lu1 N3 C20 -137.6(15) . . . . ?
O8 Lu1 N3 C20 118.7(16) 2_755 . . . ?
O1W Lu1 N3 C20 57.9(16) . . . . ?
O1 Lu1 N3 C20 -96.1(16) . . . . ?
N4 Lu1 N3 C20 173.8(17) . . . . ?
N1 Lu1 N3 C20 12(2) . . . . ?
N2 Lu1 N3 C20 -21.5(16) . . . . ?
O4 Lu1 N3 C31 36.2(16) . . . . ?
O8 Lu1 N3 C31 -67.5(14) 2_755 . . . ?
O1W Lu1 N3 C31 -128.3(14) . . . . ?
O1 Lu1 N3 C31 77.6(13) . . . . ?
N4 Lu1 N3 C31 -12.5(12) . . . . ?
N1 Lu1 N3 C31 -174.5(12) . . . . ?
N2 Lu1 N3 C31 152.2(13) . . . . ?
O4 Lu1 N4 C30 -137.4(14) . . . . ?
O8 Lu1 N4 C30 142.4(14) 2_755 . . . ?
O1W Lu1 N4 C30 75.3(14) . . . . ?
O1 Lu1 N4 C30 -61.5(14) . . . . ?
N1 Lu1 N4 C30 169.8(12) . . . . ?
N2 Lu1 N4 C30 -15.5(19) . . . . ?
N3 Lu1 N4 C30 11.8(13) . . . . ?
O4 Lu1 N4 C29 36.2(15) . . . . ?
O8 Lu1 N4 C29 -44.0(15) 2_755 . . . ?
O1W Lu1 N4 C29 -111.2(15) . . . . ?
O1 Lu1 N4 C29 112.1(15) . . . . ?
N1 Lu1 N4 C29 -17(2) . . . . ?
N2 Lu1 N4 C29 158.1(14) . . . . ?
N3 Lu1 N4 C29 -174.7(16) . . . . ?
O2 S1 C1 C6 -34.9(18) . . . . ?
O3 S1 C1 C6 85.7(17) . . . . ?
O1 S1 C1 C6 -154.0(15) . . . . ?
O2 S1 C1 C2 149.0(15) . . . . ?
O3 S1 C1 C2 -90.4(16) . . . . ?
O1 S1 C1 C2 29.9(17) . . . . ?
Lu1 O4 C2 C3 172.2(13) . . . . ?
Lu1 O4 C2 C1 -8(3) . . . . ?
C6 C1 C2 O4 177.9(18) . . . . ?
S1 C1 C2 O4 -6(3) . . . . ?
C6 C1 C2 C3 -3(3) . . . . ?
S1 C1 C2 C3 173.2(13) . . . . ?
O4 C2 C3 C4 178.3(16) . . . . ?
C1 C2 C3 C4 -1(3) . . . . ?
O4 C2 C3 N5 1(2) . . . . ?
C1 C2 C3 N5 -178.0(15) . . . . ?
O6 N5 C3 C4 -98(2) . . . . ?
O5 N5 C3 C4 87(2) . . . . ?
O6 N5 C3 C2 79(2) . . . . ?
O5 N5 C3 C2 -96.3(19) . . . . ?
C2 C3 C4 C5 3(3) . . . . ?
N5 C3 C4 C5 179.8(16) . . . . ?
C2 C3 C4 C7 -168.7(16) . . . . ?
N5 C3 C4 C7 8(3) . . . . ?
C3 C4 C5 C6 -2(3) . . . . ?
C7 C4 C5 C6 170.6(18) . . . . ?
C4 C5 C6 C1 -2(3) . . . . ?
C2 C1 C6 C5 4(3) . . . . ?
S1 C1 C6 C5 -171.6(15) . . . . ?
Lu1 O8 C7 O7 6(3) 2_745 . . . ?
Lu1 O8 C7 C4 -170.3(13) 2_745 . . . ?
C3 C4 C7 O7 3(3) . . . . ?
C5 C4 C7 O7 -168.5(17) . . . . ?
C3 C4 C7 O8 179.8(16) . . . . ?
C5 C4 C7 O8 8(2) . . . . ?
O4 Lu1 N1 C8 -52.6(16) . . . . ?
O8 Lu1 N1 C8 28.5(16) 2_755 . . . ?
O1W Lu1 N1 C8 103.3(16) . . . . ?
O1 Lu1 N1 C8 -119.5(16) . . . . ?
N4 Lu1 N1 C8 2(2) . . . . ?
N2 Lu1 N1 C8 -175.1(17) . . . . ?
N3 Lu1 N1 C8 148.1(15) . . . . ?
O4 Lu1 N1 C19 134.9(14) . . . . ?
O8 Lu1 N1 C19 -144.0(14) 2_755 . . . ?
O1W Lu1 N1 C19 -69.1(13) . . . . ?
O1 Lu1 N1 C19 68.0(14) . . . . ?
N4 Lu1 N1 C19 -170.8(12) . . . . ?
N2 Lu1 N1 C19 12.5(12) . . . . ?
N3 Lu1 N1 C19 -24.3(17) . . . . ?
C19 N1 C8 C9 -1(3) . . . . ?
Lu1 N1 C8 C9 -173.4(17) . . . . ?
N1 C8 C9 C10 1(3) . . . . ?
C8 C9 C10 C11 0(4) . . . . ?
C9 C10 C11 C19 0(4) . . . . ?
C9 C10 C11 C12 -176(2) . . . . ?
C19 C11 C12 C13 2(4) . . . . ?
C10 C11 C12 C13 177(3) . . . . ?
C11 C12 C13 C14 -3(4) . . . . ?
C12 C13 C14 C15 -174(3) . . . . ?
C12 C13 C14 C18 1(3) . . . . ?
C13 C14 C15 C16 172(2) . . . . ?
C18 C14 C15 C16 -3(4) . . . . ?
C14 C15 C16 C17 1(4) . . . . ?
C18 N2 C17 C16 -6(3) . . . . ?
Lu1 N2 C17 C16 168.9(16) . . . . ?
C15 C16 C17 N2 4(3) . . . . ?
C17 N2 C18 C19 -171.2(18) . . . . ?
Lu1 N2 C18 C19 13(2) . . . . ?
C17 N2 C18 C14 4(3) . . . . ?
Lu1 N2 C18 C14 -171.6(14) . . . . ?
C15 C14 C18 N2 1(3) . . . . ?
C13 C14 C18 N2 -174.7(19) . . . . ?
C15 C14 C18 C19 176(2) . . . . ?
C13 C14 C18 C19 1(3) . . . . ?
C8 N1 C19 C11 1(3) . . . . ?
Lu1 N1 C19 C11 173.4(16) . . . . ?
C8 N1 C19 C18 176.3(18) . . . . ?
Lu1 N1 C19 C18 -11(2) . . . . ?
C10 C11 C19 N1 0(3) . . . . ?
C12 C11 C19 N1 175.6(19) . . . . ?
C10 C11 C19 C18 -175(2) . . . . ?
C12 C11 C19 C18 0(3) . . . . ?
N2 C18 C19 N1 -2(3) . . . . ?
C14 C18 C19 N1 -176.8(17) . . . . ?
N2 C18 C19 C11 173.8(19) . . . . ?
C14 C18 C19 C11 -1(3) . . . . ?
C31 N3 C20 C21 -9(3) . . . . ?
Lu1 N3 C20 C21 165.3(18) . . . . ?
N3 C20 C21 C22 7(4) . . . . ?
C20 C21 C22 C23 -1(4) . . . . ?
C21 C22 C23 C24 177(2) . . . . ?
C21 C22 C23 C31 -2(3) . . . . ?
C22 C23 C24 C25 -172(2) . . . . ?
C31 C23 C24 C25 7(3) . . . . ?
C23 C24 C25 C26 -11(3) . . . . ?
C24 C25 C26 C27 -179(2) . . . . ?
C24 C25 C26 C30 10(3) . . . . ?
C25 C26 C27 C28 -169(2) . . . . ?
C30 C26 C27 C28 3(3) . . . . ?
C26 C27 C28 C29 -8(4) . . . . ?
C27 C28 C29 N4 7(3) . . . . ?
C30 N4 C29 C28 -2(3) . . . . ?
Lu1 N4 C29 C28 -175.7(17) . . . . ?
C29 N4 C30 C31 175.5(17) . . . . ?
Lu1 N4 C30 C31 -10(2) . . . . ?
C29 N4 C30 C26 -3(3) . . . . ?
Lu1 N4 C30 C26 170.7(15) . . . . ?
C27 C26 C30 N4 3(3) . . . . ?
C25 C26 C30 N4 175(2) . . . . ?
C27 C26 C30 C31 -176.5(18) . . . . ?
C25 C26 C30 C31 -4(3) . . . . ?
C20 N3 C31 C23 5(3) . . . . ?
Lu1 N3 C31 C23 -169.7(15) . . . . ?
C20 N3 C31 C30 -172.9(16) . . . . ?
Lu1 N3 C31 C30 13(2) . . . . ?
C22 C23 C31 N3 0(3) . . . . ?
C24 C23 C31 N3 -178.6(19) . . . . ?
C22 C23 C31 C30 178.0(19) . . . . ?
C24 C23 C31 C30 -1(3) . . . . ?
N4 C30 C31 N3 -2(2) . . . . ?
C26 C30 C31 N3 177.2(16) . . . . ?
N4 C30 C31 C23 -179.7(18) . . . . ?
C26 C30 C31 C23 -1(3) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H1W1 O7 0.85(5) 1.91(12) 2.681(19) 149(21) 2_755
O1W H1W2 O2 0.85(5) 1.81(8) 2.633(18) 161(24) 2_855

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         3.118
_refine_diff_density_min         -2.973
_refine_diff_density_rms         0.276

# start Validation Reply Form
_vrf_PLAT430_3-Yb                
;
PROBLEM: Short Inter D...A Contact  O10W   ..  O10W    ..       1.90 Ang.  
RESPONSE: Owing to the disorder of the O10w, the H atoms were not added, 
which then leads to such alert.
;
####################################################################### 
# 
# 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_6-Eu
_database_code_depnum_ccdc_archive 'CCDC 1549870'
_audit_update_record             
;
2017-05-13 deposited with the CCDC.
2017-11-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C19 H13 Eu N2 O7 S'
_chemical_formula_sum            'C19 H13 Eu N2 O7 S'
_chemical_formula_weight         565.33

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'
Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   11.9548(2)
_cell_length_b                   8.47498(17)
_cell_length_c                   17.9413(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 103.253(2)
_cell_angle_gamma                90.00
_cell_volume                     1769.34(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    2846
_cell_measurement_theta_min      3.34
_cell_measurement_theta_max      27.56

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.122
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1104
_exptl_absorpt_coefficient_mu    3.713
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5094
_exptl_absorpt_correction_T_max  0.5880
_exptl_absorpt_process_details   
; 
CrysAlis Pro (Agilent, 2013)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1954
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6279
_diffrn_reflns_av_R_equivalents  0.0315
_diffrn_reflns_av_sigmaI/netI    0.0599
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         3.34
_diffrn_reflns_theta_max         27.56
_reflns_number_total             4025
_reflns_number_gt                3335
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_cell_refinement       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_data_reduction        
;
CrysAlis Pro (Agilent, 2013)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    '(K. Brandenburg, Diamond 3.1, 2009)'
_computing_publication_material  '(K. Brandenburg, Diamond 3.1, 2009)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0187P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4025
_refine_ls_number_parameters     277
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_gt           0.0348
_refine_ls_wR_factor_ref         0.0679
_refine_ls_wR_factor_gt          0.0629
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_restrained_S_all      1.015
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Eu1 Eu 0.380889(17) 0.46162(3) 0.199596(12) 0.01271(7) Uani 1 1 d . . .
S1 S 0.31992(9) 0.87268(14) 0.17173(6) 0.0149(2) Uani 1 1 d . . .
O1 O 0.2716(2) 0.7171(4) 0.18136(18) 0.0189(7) Uani 1 1 d . . .
O1W O 0.3474(3) 0.2328(4) 0.2767(2) 0.0219(7) Uani 1 1 d D . .
H1W1 H 0.302(3) 0.164(4) 0.254(2) 0.033 Uiso 1 1 d D . .
H1W2 H 0.403(3) 0.192(4) 0.308(2) 0.033 Uiso 1 1 d D . .
O2 O 0.2366(3) 0.9983(4) 0.16702(19) 0.0207(7) Uani 1 1 d . . .
O3 O 0.4236(2) 0.9030(4) 0.23125(18) 0.0218(7) Uani 1 1 d . . .
O4 O 0.4606(2) 0.6197(4) 0.12320(17) 0.0173(7) Uani 1 1 d . . .
O5 O 0.4060(3) 0.9174(4) -0.18348(18) 0.0219(7) Uani 1 1 d . . .
O6 O 0.5386(2) 0.7383(4) -0.13397(18) 0.0199(7) Uani 1 1 d . . .
N1 N 0.2311(3) 0.3957(5) 0.0736(2) 0.0203(9) Uani 1 1 d . . .
N2 N 0.1646(3) 0.4347(5) 0.2064(2) 0.0207(9) Uani 1 1 d . . .
C1 C 0.3602(4) 0.8620(5) 0.0833(2) 0.0144(9) Uani 1 1 d . . .
C2 C 0.4250(3) 0.7304(5) 0.0699(3) 0.0139(9) Uani 1 1 d . . .
C3 C 0.4507(4) 0.7203(5) -0.0017(3) 0.0168(10) Uani 1 1 d . . .
H3 H 0.4899 0.6323 -0.0133 0.020 Uiso 1 1 calc R . .
C4 C 0.4194(3) 0.8379(5) -0.0563(3) 0.0152(9) Uani 1 1 d . . .
C5 C 0.3558(3) 0.9685(5) -0.0414(2) 0.0153(9) Uani 1 1 d . . .
H5 H 0.3339 1.0475 -0.0778 0.018 Uiso 1 1 calc R . .
C6 C 0.3264(3) 0.9768(5) 0.0287(2) 0.0152(9) Uani 1 1 d . . .
H6 H 0.2831 1.0616 0.0391 0.018 Uiso 1 1 calc R . .
C7 C 0.4578(4) 0.8298(5) -0.1302(3) 0.0162(9) Uani 1 1 d . . .
C8 C 0.2612(4) 0.3864(6) 0.0068(3) 0.0284(12) Uani 1 1 d . . .
H8 H 0.3353 0.4164 0.0049 0.034 Uiso 1 1 calc R . .
C9 C 0.1875(5) 0.3340(7) -0.0605(3) 0.0389(14) Uani 1 1 d . . .
H9 H 0.2124 0.3288 -0.1059 0.047 Uiso 1 1 calc R . .
C10 C 0.0788(5) 0.2908(7) -0.0587(3) 0.0412(15) Uani 1 1 d . . .
H10 H 0.0284 0.2549 -0.1029 0.049 Uiso 1 1 calc R . .
C11 C 0.0435(4) 0.3006(6) 0.0096(3) 0.0319(13) Uani 1 1 d . . .
C12 C -0.0706(5) 0.2619(8) 0.0160(4) 0.0509(18) Uani 1 1 d . . .
H12 H -0.1221 0.2196 -0.0261 0.061 Uiso 1 1 calc R . .
C13 C -0.1048(5) 0.2856(7) 0.0815(4) 0.0482(17) Uani 1 1 d . . .
H13 H -0.1799 0.2613 0.0835 0.058 Uiso 1 1 calc R . .
C14 C -0.0286(4) 0.3470(6) 0.1478(4) 0.0318(13) Uani 1 1 d . . .
C15 C -0.0622(4) 0.3857(7) 0.2148(4) 0.0385(15) Uani 1 1 d . . .
H15 H -0.1374 0.3676 0.2186 0.046 Uiso 1 1 calc R . .
C16 C 0.0153(5) 0.4504(7) 0.2749(3) 0.0378(15) Uani 1 1 d . . .
H16 H -0.0068 0.4805 0.3192 0.045 Uiso 1 1 calc R . .
C17 C 0.1289(4) 0.4703(6) 0.2683(3) 0.0311(12) Uani 1 1 d . . .
H17 H 0.1820 0.5111 0.3101 0.037 Uiso 1 1 calc R . .
C18 C 0.0867(4) 0.3775(5) 0.1452(3) 0.0201(10) Uani 1 1 d . . .
C19 C 0.1219(4) 0.3557(6) 0.0751(3) 0.0219(11) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Eu1 O4 2.276(3) . ?
Eu1 O5 2.292(3) 4_576 ?
Eu1 O6 2.388(3) 3_665 ?
Eu1 O3 2.433(3) 2_645 ?
Eu1 O1W 2.467(3) . ?
Eu1 O1 2.511(3) . ?
Eu1 N1 2.603(4) . ?
Eu1 N2 2.626(4) . ?
S1 O2 1.447(3) . ?
S1 O3 1.462(3) . ?
S1 O1 1.466(3) . ?
S1 C1 1.763(4) . ?
O1W H1W1 0.85(5) . ?
O1W H1W2 0.85(5) . ?
O3 Eu1 2.433(3) 2_655 ?
O4 C2 1.338(5) . ?
O5 C7 1.256(5) . ?
O5 Eu1 2.292(3) 4_575 ?
O6 C7 1.253(5) . ?
O6 Eu1 2.388(3) 3_665 ?
N1 C8 1.330(6) . ?
N1 C19 1.355(5) . ?
N2 C17 1.313(6) . ?
N2 C18 1.357(6) . ?
C1 C6 1.373(6) . ?
C1 C2 1.410(6) . ?
C2 C3 1.390(6) . ?
C3 C4 1.388(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.403(6) . ?
C4 C7 1.500(6) . ?
C5 C6 1.383(6) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C8 C9 1.394(7) . ?
C8 H8 0.9300 . ?
C9 C10 1.358(7) . ?
C9 H9 0.9300 . ?
C10 C11 1.387(8) . ?
C10 H10 0.9300 . ?
C11 C19 1.404(7) . ?
C11 C12 1.433(7) . ?
C12 C13 1.346(9) . ?
C12 H12 0.9300 . ?
C13 C14 1.420(8) . ?
C13 H13 0.9300 . ?
C14 C15 1.390(8) . ?
C14 C18 1.415(6) . ?
C15 C16 1.365(8) . ?
C15 H15 0.9300 . ?
C16 C17 1.400(7) . ?
C16 H16 0.9300 . ?
C17 H17 0.9300 . ?
C18 C19 1.426(7) . ?

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 Eu1 O5 107.61(11) . 4_576 ?
O4 Eu1 O6 81.33(11) . 3_665 ?
O5 Eu1 O6 141.78(11) 4_576 3_665 ?
O4 Eu1 O3 86.64(10) . 2_645 ?
O5 Eu1 O3 73.47(11) 4_576 2_645 ?
O6 Eu1 O3 70.01(10) 3_665 2_645 ?
O4 Eu1 O1W 160.80(10) . . ?
O5 Eu1 O1W 80.94(11) 4_576 . ?
O6 Eu1 O1W 81.62(11) 3_665 . ?
O3 Eu1 O1W 79.27(10) 2_645 . ?
O4 Eu1 O1 72.01(10) . . ?
O5 Eu1 O1 71.85(11) 4_576 . ?
O6 Eu1 O1 143.51(10) 3_665 . ?
O3 Eu1 O1 130.75(11) 2_645 . ?
O1W Eu1 O1 127.17(10) . . ?
O4 Eu1 N1 84.43(11) . . ?
O5 Eu1 N1 144.18(11) 4_576 . ?
O6 Eu1 N1 72.18(11) 3_665 . ?
O3 Eu1 N1 142.03(11) 2_645 . ?
O1W Eu1 N1 98.67(12) . . ?
O1 Eu1 N1 80.69(11) . . ?
O4 Eu1 N2 129.19(11) . . ?
O5 Eu1 N2 85.42(11) 4_576 . ?
O6 Eu1 N2 118.26(11) 3_665 . ?
O3 Eu1 N2 143.07(11) 2_645 . ?
O1W Eu1 N2 67.52(11) . . ?
O1 Eu1 N2 65.96(11) . . ?
N1 Eu1 N2 62.18(12) . . ?
O2 S1 O3 111.73(19) . . ?
O2 S1 O1 112.60(18) . . ?
O3 S1 O1 111.31(19) . . ?
O2 S1 C1 108.1(2) . . ?
O3 S1 C1 107.81(19) . . ?
O1 S1 C1 104.8(2) . . ?
S1 O1 Eu1 125.71(16) . . ?
Eu1 O1W H1W1 116(3) . . ?
Eu1 O1W H1W2 120(3) . . ?
H1W1 O1W H1W2 111.7(18) . . ?
S1 O3 Eu1 164.42(19) . 2_655 ?
C2 O4 Eu1 137.3(2) . . ?
C7 O5 Eu1 154.1(3) . 4_575 ?
C7 O6 Eu1 150.3(3) . 3_665 ?
C8 N1 C19 117.6(4) . . ?
C8 N1 Eu1 121.4(3) . . ?
C19 N1 Eu1 120.7(3) . . ?
C17 N2 C18 118.1(4) . . ?
C17 N2 Eu1 122.3(3) . . ?
C18 N2 Eu1 119.6(3) . . ?
C6 C1 C2 121.5(4) . . ?
C6 C1 S1 120.6(3) . . ?
C2 C1 S1 117.9(3) . . ?
O4 C2 C3 121.1(4) . . ?
O4 C2 C1 122.0(4) . . ?
C3 C2 C1 116.9(4) . . ?
C4 C3 C2 121.8(4) . . ?
C4 C3 H3 119.1 . . ?
C2 C3 H3 119.1 . . ?
C3 C4 C5 120.1(4) . . ?
C3 C4 C7 120.2(4) . . ?
C5 C4 C7 119.6(4) . . ?
C6 C5 C4 118.4(4) . . ?
C6 C5 H5 120.8 . . ?
C4 C5 H5 120.8 . . ?
C1 C6 C5 121.2(4) . . ?
C1 C6 H6 119.4 . . ?
C5 C6 H6 119.4 . . ?
O6 C7 O5 125.2(4) . . ?
O6 C7 C4 118.2(4) . . ?
O5 C7 C4 116.7(4) . . ?
N1 C8 C9 123.5(5) . . ?
N1 C8 H8 118.3 . . ?
C9 C8 H8 118.3 . . ?
C10 C9 C8 118.9(5) . . ?
C10 C9 H9 120.6 . . ?
C8 C9 H9 120.6 . . ?
C9 C10 C11 119.5(5) . . ?
C9 C10 H10 120.3 . . ?
C11 C10 H10 120.3 . . ?
C10 C11 C19 118.6(5) . . ?
C10 C11 C12 123.0(5) . . ?
C19 C11 C12 118.3(5) . . ?
C13 C12 C11 121.4(6) . . ?
C13 C12 H12 119.3 . . ?
C11 C12 H12 119.3 . . ?
C12 C13 C14 121.4(5) . . ?
C12 C13 H13 119.3 . . ?
C14 C13 H13 119.3 . . ?
C15 C14 C18 117.5(5) . . ?
C15 C14 C13 123.6(5) . . ?
C18 C14 C13 118.8(5) . . ?
C16 C15 C14 119.9(5) . . ?
C16 C15 H15 120.0 . . ?
C14 C15 H15 120.0 . . ?
C15 C16 C17 118.6(5) . . ?
C15 C16 H16 120.7 . . ?
C17 C16 H16 120.7 . . ?
N2 C17 C16 123.6(5) . . ?
N2 C17 H17 118.2 . . ?
C16 C17 H17 118.2 . . ?
N2 C18 C14 122.1(4) . . ?
N2 C18 C19 118.3(4) . . ?
C14 C18 C19 119.5(5) . . ?
N1 C19 C11 121.8(4) . . ?
N1 C19 C18 117.7(4) . . ?
C11 C19 C18 120.4(4) . . ?

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
O2 S1 O1 Eu1 -176.54(19) . . . . ?
O3 S1 O1 Eu1 -50.2(3) . . . . ?
C1 S1 O1 Eu1 66.1(3) . . . . ?
O4 Eu1 O1 S1 -32.5(2) . . . . ?
O5 Eu1 O1 S1 83.6(2) 4_576 . . . ?
O6 Eu1 O1 S1 -77.7(3) 3_665 . . . ?
O3 Eu1 O1 S1 36.3(3) 2_645 . . . ?
O1W Eu1 O1 S1 146.48(19) . . . . ?
N1 Eu1 O1 S1 -119.7(2) . . . . ?
N2 Eu1 O1 S1 176.7(3) . . . . ?
O2 S1 O3 Eu1 -111.3(8) . . . 2_655 ?
O1 S1 O3 Eu1 121.8(8) . . . 2_655 ?
C1 S1 O3 Eu1 7.4(8) . . . 2_655 ?
O5 Eu1 O4 C2 -96.4(4) 4_576 . . . ?
O6 Eu1 O4 C2 121.8(4) 3_665 . . . ?
O3 Eu1 O4 C2 -167.9(4) 2_645 . . . ?
O1W Eu1 O4 C2 149.5(4) . . . . ?
O1 Eu1 O4 C2 -32.9(4) . . . . ?
N1 Eu1 O4 C2 49.1(4) . . . . ?
N2 Eu1 O4 C2 2.3(5) . . . . ?
O4 Eu1 N1 C8 35.2(4) . . . . ?
O5 Eu1 N1 C8 147.8(3) 4_576 . . . ?
O6 Eu1 N1 C8 -47.5(4) 3_665 . . . ?
O3 Eu1 N1 C8 -42.0(5) 2_645 . . . ?
O1W Eu1 N1 C8 -125.7(4) . . . . ?
O1 Eu1 N1 C8 107.8(4) . . . . ?
N2 Eu1 N1 C8 175.5(4) . . . . ?
O4 Eu1 N1 C19 -150.8(3) . . . . ?
O5 Eu1 N1 C19 -38.2(4) 4_576 . . . ?
O6 Eu1 N1 C19 126.5(4) 3_665 . . . ?
O3 Eu1 N1 C19 132.0(3) 2_645 . . . ?
O1W Eu1 N1 C19 48.3(3) . . . . ?
O1 Eu1 N1 C19 -78.2(3) . . . . ?
N2 Eu1 N1 C19 -10.5(3) . . . . ?
O4 Eu1 N2 C17 -117.1(4) . . . . ?
O5 Eu1 N2 C17 -8.1(4) 4_576 . . . ?
O6 Eu1 N2 C17 140.3(4) 3_665 . . . ?
O3 Eu1 N2 C17 46.4(5) 2_645 . . . ?
O1W Eu1 N2 C17 74.0(4) . . . . ?
O1 Eu1 N2 C17 -80.2(4) . . . . ?
N1 Eu1 N2 C17 -172.2(4) . . . . ?
O4 Eu1 N2 C18 65.0(4) . . . . ?
O5 Eu1 N2 C18 174.1(3) 4_576 . . . ?
O6 Eu1 N2 C18 -37.5(4) 3_665 . . . ?
O3 Eu1 N2 C18 -131.5(3) 2_645 . . . ?
O1W Eu1 N2 C18 -103.9(3) . . . . ?
O1 Eu1 N2 C18 101.9(3) . . . . ?
N1 Eu1 N2 C18 9.9(3) . . . . ?
O2 S1 C1 C6 9.4(4) . . . . ?
O3 S1 C1 C6 -111.6(4) . . . . ?
O1 S1 C1 C6 129.7(4) . . . . ?
O2 S1 C1 C2 -169.0(3) . . . . ?
O3 S1 C1 C2 70.1(4) . . . . ?
O1 S1 C1 C2 -48.6(4) . . . . ?
Eu1 O4 C2 C3 -127.4(4) . . . . ?
Eu1 O4 C2 C1 52.7(6) . . . . ?
C6 C1 C2 O4 178.4(4) . . . . ?
S1 C1 C2 O4 -3.3(6) . . . . ?
C6 C1 C2 C3 -1.5(6) . . . . ?
S1 C1 C2 C3 176.8(3) . . . . ?
O4 C2 C3 C4 -176.7(4) . . . . ?
C1 C2 C3 C4 3.2(6) . . . . ?
C2 C3 C4 C5 -2.8(6) . . . . ?
C2 C3 C4 C7 174.5(4) . . . . ?
C3 C4 C5 C6 0.5(6) . . . . ?
C7 C4 C5 C6 -176.8(4) . . . . ?
C2 C1 C6 C5 -0.7(7) . . . . ?
S1 C1 C6 C5 -178.9(3) . . . . ?
C4 C5 C6 C1 1.2(6) . . . . ?
Eu1 O6 C7 O5 -47.6(8) 3_665 . . . ?
Eu1 O6 C7 C4 132.9(5) 3_665 . . . ?
Eu1 O5 C7 O6 -11.2(10) 4_575 . . . ?
Eu1 O5 C7 C4 168.3(5) 4_575 . . . ?
C3 C4 C7 O6 -16.5(6) . . . . ?
C5 C4 C7 O6 160.8(4) . . . . ?
C3 C4 C7 O5 164.0(4) . . . . ?
C5 C4 C7 O5 -18.7(6) . . . . ?
C19 N1 C8 C9 -1.8(7) . . . . ?
Eu1 N1 C8 C9 172.4(4) . . . . ?
N1 C8 C9 C10 0.4(8) . . . . ?
C8 C9 C10 C11 0.4(8) . . . . ?
C9 C10 C11 C19 0.2(8) . . . . ?
C9 C10 C11 C12 178.1(6) . . . . ?
C10 C11 C12 C13 -174.2(6) . . . . ?
C19 C11 C12 C13 3.7(9) . . . . ?
C11 C12 C13 C14 -1.3(10) . . . . ?
C12 C13 C14 C15 174.5(6) . . . . ?
C12 C13 C14 C18 -2.6(9) . . . . ?
C18 C14 C15 C16 -0.1(8) . . . . ?
C13 C14 C15 C16 -177.2(6) . . . . ?
C14 C15 C16 C17 -2.5(9) . . . . ?
C18 N2 C17 C16 1.0(7) . . . . ?
Eu1 N2 C17 C16 -177.0(4) . . . . ?
C15 C16 C17 N2 2.2(8) . . . . ?
C17 N2 C18 C14 -3.8(7) . . . . ?
Eu1 N2 C18 C14 174.2(3) . . . . ?
C17 N2 C18 C19 172.9(4) . . . . ?
Eu1 N2 C18 C19 -9.1(6) . . . . ?
C15 C14 C18 N2 3.4(7) . . . . ?
C13 C14 C18 N2 -179.4(5) . . . . ?
C15 C14 C18 C19 -173.3(5) . . . . ?
C13 C14 C18 C19 4.0(7) . . . . ?
C8 N1 C19 C11 2.3(7) . . . . ?
Eu1 N1 C19 C11 -171.9(4) . . . . ?
C8 N1 C19 C18 -175.1(4) . . . . ?
Eu1 N1 C19 C18 10.6(5) . . . . ?
C10 C11 C19 N1 -1.6(8) . . . . ?
C12 C11 C19 N1 -179.6(5) . . . . ?
C10 C11 C19 C18 175.8(5) . . . . ?
C12 C11 C19 C18 -2.2(8) . . . . ?
N2 C18 C19 N1 -0.9(7) . . . . ?
C14 C18 C19 N1 175.9(4) . . . . ?
N2 C18 C19 C11 -178.4(5) . . . . ?
C14 C18 C19 C11 -1.6(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
O1W H1W1 O2 0.85(5) 2.11(2) 2.895(5) 156(5) 1_545
O1W H1W2 O4 0.85(5) 1.903(11) 2.742(4) 173(4) 2_645

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        27.56
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         1.476
_refine_diff_density_min         -1.007
_refine_diff_density_rms         0.152
####################################################################### 
# 
# 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_7-Gd
_database_code_depnum_ccdc_archive 'CCDC 1549871'
_audit_update_record             
;
2017-05-13 deposited with the CCDC.
2017-11-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C31 H20 Gd N5 O9 S'
_chemical_formula_sum            'C31 H20 Gd N5 O9 S'
_chemical_formula_weight         795.83

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'
Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   11.6131(3)
_cell_length_b                   14.8734(4)
_cell_length_c                   17.5855(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 104.818(3)
_cell_angle_gamma                90.00
_cell_volume                     2936.46(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    3525
_cell_measurement_theta_min      2.99
_cell_measurement_theta_max      27.56

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.800
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1572
_exptl_absorpt_coefficient_mu    2.396
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6331
_exptl_absorpt_correction_T_max  0.7151
_exptl_absorpt_process_details   
; 
CrysAlis Pro (Agilent, 2013)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1954
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10807
_diffrn_reflns_av_R_equivalents  0.0346
_diffrn_reflns_av_sigmaI/netI    0.0731
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.99
_diffrn_reflns_theta_max         27.56
_reflns_number_total             6699
_reflns_number_gt                4901
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_cell_refinement       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_data_reduction        
;
CrysAlis Pro (Agilent, 2013)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    '(K. Brandenburg, Diamond 3.1, 2009)'
_computing_publication_material  '(K. Brandenburg, Diamond 3.1, 2009)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0141P)²+19.0694P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6699
_refine_ls_number_parameters     430
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0818
_refine_ls_R_factor_gt           0.0531
_refine_ls_wR_factor_ref         0.1144
_refine_ls_wR_factor_gt          0.1059
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_restrained_S_all      1.095
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Gd1 Gd 0.31557(3) 0.39350(2) 0.74428(2) 0.02553(10) Uani 1 1 d . . .
S1 S 0.30991(14) 0.61556(13) 0.67234(11) 0.0304(4) Uani 1 1 d . . .
O1 O 0.3762(4) 0.5404(3) 0.7166(3) 0.0375(13) Uani 1 1 d . . .
O1W O 0.3957(4) 0.2460(3) 0.7670(4) 0.0466(15) Uani 1 1 d D . .
H1W1 H 0.347(5) 0.203(3) 0.753(6) 0.070 Uiso 1 1 d D . .
H1W2 H 0.466(2) 0.226(5) 0.783(5) 0.070 Uiso 1 1 d D . .
O2 O 0.2554(5) 0.5910(4) 0.5921(3) 0.0485(15) Uani 1 1 d . . .
O3 O 0.3816(5) 0.6955(4) 0.6802(4) 0.0520(16) Uani 1 1 d . . .
O4 O 0.1667(4) 0.4875(3) 0.7512(3) 0.0375(13) Uani 1 1 d . . .
O5 O -0.0946(6) 0.4766(4) 0.7532(5) 0.069(2) Uani 1 1 d . . .
O6 O -0.0006(6) 0.5151(6) 0.8714(4) 0.079(2) Uani 1 1 d . . .
O7 O -0.1960(5) 0.6504(4) 0.7915(4) 0.0507(16) Uani 1 1 d . . .
O8 O -0.1574(4) 0.7930(3) 0.7701(3) 0.0433(14) Uani 1 1 d . . .
N1 N 0.2150(5) 0.3878(4) 0.5991(4) 0.0370(14) Uani 1 1 d . . .
N2 N 0.4542(5) 0.3702(4) 0.6495(4) 0.0340(14) Uani 1 1 d . . .
N3 N 0.5119(5) 0.4265(4) 0.8500(4) 0.0352(14) Uani 1 1 d . . .
N4 N 0.3111(6) 0.3729(4) 0.8879(4) 0.0378(15) Uani 1 1 d . . .
N5 N -0.0269(6) 0.5255(5) 0.8011(5) 0.0457(18) Uani 1 1 d . . .
C1 C 0.1927(6) 0.6406(5) 0.7163(4) 0.0298(16) Uani 1 1 d . . .
C2 C 0.1341(6) 0.5716(5) 0.7460(4) 0.0266(15) Uani 1 1 d . . .
C3 C 0.0322(6) 0.5991(5) 0.7703(4) 0.0303(15) Uani 1 1 d . . .
C4 C -0.0111(6) 0.6867(5) 0.7650(4) 0.0315(16) Uani 1 1 d . . .
C5 C 0.0540(7) 0.7520(5) 0.7370(5) 0.042(2) Uani 1 1 d . . .
H5 H 0.0297 0.8118 0.7349 0.051 Uiso 1 1 calc R . .
C6 C 0.1533(6) 0.7293(5) 0.7126(5) 0.0391(19) Uani 1 1 d . . .
H6 H 0.1949 0.7736 0.6934 0.047 Uiso 1 1 calc R . .
C7 C -0.1306(7) 0.7108(5) 0.7783(5) 0.0363(18) Uani 1 1 d . . .
C8 C 0.0959(8) 0.3911(6) 0.5728(6) 0.054(2) Uani 1 1 d . . .
H8 H 0.0507 0.3896 0.6095 0.065 Uiso 1 1 calc R . .
C9 C 0.0398(8) 0.3964(7) 0.4976(6) 0.061(3) Uani 1 1 d . . .
H9 H -0.0429 0.3945 0.4818 0.074 Uiso 1 1 calc R . .
C10 C 0.1066(9) 0.4048(8) 0.4416(6) 0.071(3) Uani 1 1 d . . .
H10 H 0.0675 0.4124 0.3888 0.086 Uiso 1 1 calc R . .
C11 C 0.2282(9) 0.4018(6) 0.4637(5) 0.056(2) Uani 1 1 d . . .
C12 C 0.3046(8) 0.4015(6) 0.4103(4) 0.0410(19) Uani 1 1 d . . .
H12 H 0.2707 0.4062 0.3565 0.049 Uiso 1 1 calc R . .
C13 C 0.4150(12) 0.3951(7) 0.4350(5) 0.074(3) Uani 1 1 d . . .
H13 H 0.4604 0.3982 0.3985 0.088 Uiso 1 1 calc R . .
C14 C 0.4762(9) 0.3834(6) 0.5162(5) 0.051(2) Uani 1 1 d . . .
C15 C 0.5977(9) 0.3702(6) 0.5444(6) 0.059(3) Uani 1 1 d . . .
H15 H 0.6459 0.3710 0.5095 0.071 Uiso 1 1 calc R . .
C16 C 0.6478(8) 0.3560(6) 0.6227(6) 0.056(3) Uani 1 1 d . . .
H16 H 0.7295 0.3483 0.6421 0.067 Uiso 1 1 calc R . .
C17 C 0.5712(7) 0.3535(6) 0.6727(5) 0.046(2) Uani 1 1 d . . .
H17 H 0.6037 0.3392 0.7253 0.055 Uiso 1 1 calc R . .
C18 C 0.4066(7) 0.3831(5) 0.5722(4) 0.0389(18) Uani 1 1 d . . .
C19 C 0.2796(7) 0.3914(5) 0.5451(4) 0.0383(17) Uani 1 1 d . . .
C20 C 0.6083(7) 0.4602(6) 0.8349(6) 0.049(2) Uani 1 1 d . . .
H20 H 0.6022 0.4830 0.7848 0.059 Uiso 1 1 calc R . .
C21 C 0.7186(8) 0.4640(7) 0.8890(7) 0.064(3) Uani 1 1 d . . .
H21 H 0.7847 0.4866 0.8747 0.077 Uiso 1 1 calc R . .
C22 C 0.7280(9) 0.4340(7) 0.9631(7) 0.069(3) Uani 1 1 d . . .
H22 H 0.8022 0.4329 0.9991 0.083 Uiso 1 1 calc R . .
C23 C 0.6309(8) 0.4057(6) 0.9852(5) 0.054(2) Uani 1 1 d . . .
C24 C 0.6269(11) 0.3831(7) 1.0617(6) 0.070(3) Uani 1 1 d . . .
H24 H 0.6979 0.3850 1.1009 0.084 Uiso 1 1 calc R . .
C25 C 0.5285(13) 0.3589(7) 1.0828(6) 0.081(4) Uani 1 1 d . . .
H25 H 0.5326 0.3450 1.1350 0.097 Uiso 1 1 calc R . .
C26 C 0.4165(10) 0.3546(6) 1.0245(5) 0.054(2) Uani 1 1 d . . .
C27 C 0.3103(11) 0.3354(7) 1.0434(6) 0.068(3) Uani 1 1 d . . .
H27 H 0.3091 0.3242 1.0953 0.081 Uiso 1 1 calc R . .
C28 C 0.2084(11) 0.3332(6) 0.9850(6) 0.068(3) Uani 1 1 d . . .
H28 H 0.1364 0.3190 0.9959 0.082 Uiso 1 1 calc R . .
C29 C 0.2128(8) 0.3528(6) 0.9075(6) 0.052(2) Uani 1 1 d . . .
H29 H 0.1421 0.3514 0.8681 0.062 Uiso 1 1 calc R . .
C30 C 0.4143(8) 0.3742(5) 0.9462(5) 0.0390(19) Uani 1 1 d . . .
C31 C 0.5189(7) 0.4006(6) 0.9251(4) 0.0411(19) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Gd1 O4 2.251(5) . ?
Gd1 O8 2.331(5) 2_546 ?
Gd1 O1W 2.376(5) . ?
Gd1 O1 2.383(5) . ?
Gd1 N1 2.523(6) . ?
Gd1 N4 2.559(6) . ?
Gd1 N3 2.594(6) . ?
Gd1 N2 2.620(6) . ?
S1 O3 1.438(5) . ?
S1 O2 1.438(6) . ?
S1 O1 1.464(5) . ?
S1 C1 1.768(7) . ?
O1W H1W1 0.85(8) . ?
O1W H1W2 0.85(8) . ?
O4 C2 1.302(8) . ?
O5 N5 1.232(9) . ?
O6 N5 1.204(9) . ?
O7 C7 1.236(9) . ?
O8 C7 1.262(9) . ?
O8 Gd1 2.331(5) 2_556 ?
N1 C8 1.342(10) . ?
N1 C19 1.354(9) . ?
N2 C17 1.338(9) . ?
N2 C18 1.344(9) . ?
N3 C20 1.313(10) . ?
N3 C31 1.358(9) . ?
N4 C29 1.307(10) . ?
N4 C30 1.364(10) . ?
N5 C3 1.467(10) . ?
C1 C6 1.393(10) . ?
C1 C2 1.404(10) . ?
C2 C3 1.418(9) . ?
C3 C4 1.391(10) . ?
C4 C5 1.395(10) . ?
C4 C7 1.508(10) . ?
C5 C6 1.373(10) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C8 C9 1.319(12) . ?
C8 H8 0.9300 . ?
C9 C10 1.407(14) . ?
C9 H9 0.9300 . ?
C10 C11 1.366(13) . ?
C10 H10 0.9300 . ?
C11 C19 1.411(11) . ?
C11 C12 1.447(12) . ?
C12 C13 1.247(13) . ?
C12 H12 0.9300 . ?
C13 C14 1.434(13) . ?
C13 H13 0.9300 . ?
C14 C15 1.384(13) . ?
C14 C18 1.425(10) . ?
C15 C16 1.368(13) . ?
C15 H15 0.9300 . ?
C16 C17 1.402(11) . ?
C16 H16 0.9300 . ?
C17 H17 0.9300 . ?
C18 C19 1.434(11) . ?
C20 C21 1.388(12) . ?
C20 H20 0.9300 . ?
C21 C22 1.354(14) . ?
C21 H21 0.9300 . ?
C22 C23 1.351(14) . ?
C22 H22 0.9300 . ?
C23 C24 1.399(14) . ?
C23 C31 1.453(10) . ?
C24 C25 1.337(16) . ?
C24 H24 0.9300 . ?
C25 C26 1.437(15) . ?
C25 H25 0.9300 . ?
C26 C27 1.387(14) . ?
C26 C30 1.401(11) . ?
C27 C28 1.355(14) . ?
C27 H27 0.9300 . ?
C28 C29 1.407(12) . ?
C28 H28 0.9300 . ?
C29 H29 0.9300 . ?
C30 C31 1.413(11) . ?

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 Gd1 O8 79.00(18) . 2_546 ?
O4 Gd1 O1W 146.87(19) . . ?
O8 Gd1 O1W 71.95(18) 2_546 . ?
O4 Gd1 O1 73.31(17) . . ?
O8 Gd1 O1 146.22(18) 2_546 . ?
O1W Gd1 O1 139.21(17) . . ?
O4 Gd1 N1 85.0(2) . . ?
O8 Gd1 N1 73.8(2) 2_546 . ?
O1W Gd1 N1 101.5(2) . . ?
O1 Gd1 N1 84.7(2) . . ?
O4 Gd1 N4 79.1(2) . . ?
O8 Gd1 N4 79.4(2) 2_546 . ?
O1W Gd1 N4 80.2(2) . . ?
O1 Gd1 N4 113.17(19) . . ?
N1 Gd1 N4 150.9(2) . . ?
O4 Gd1 N3 113.0(2) . . ?
O8 Gd1 N3 136.3(2) 2_546 . ?
O1W Gd1 N3 79.6(2) . . ?
O1 Gd1 N3 73.82(19) . . ?
N1 Gd1 N3 145.73(19) . . ?
N4 Gd1 N3 63.3(2) . . ?
O4 Gd1 N2 136.21(19) . . ?
O8 Gd1 N2 116.21(19) 2_546 . ?
O1W Gd1 N2 73.0(2) . . ?
O1 Gd1 N2 74.30(17) . . ?
N1 Gd1 N2 63.41(19) . . ?
N4 Gd1 N2 141.6(2) . . ?
N3 Gd1 N2 84.88(19) . . ?
O3 S1 O2 113.8(4) . . ?
O3 S1 O1 111.6(3) . . ?
O2 S1 O1 111.6(3) . . ?
O3 S1 C1 106.0(3) . . ?
O2 S1 C1 106.7(3) . . ?
O1 S1 C1 106.7(3) . . ?
S1 O1 Gd1 131.8(3) . . ?
Gd1 O1W H1W1 117(5) . . ?
Gd1 O1W H1W2 133(5) . . ?
H1W1 O1W H1W2 110.3(18) . . ?
C2 O4 Gd1 143.7(5) . . ?
C7 O8 Gd1 143.0(5) . 2_556 ?
C8 N1 C19 117.7(7) . . ?
C8 N1 Gd1 121.1(6) . . ?
C19 N1 Gd1 120.8(5) . . ?
C17 N2 C18 117.2(7) . . ?
C17 N2 Gd1 124.9(5) . . ?
C18 N2 Gd1 117.7(5) . . ?
C20 N3 C31 117.5(7) . . ?
C20 N3 Gd1 124.4(6) . . ?
C31 N3 Gd1 117.8(5) . . ?
C29 N4 C30 117.7(7) . . ?
C29 N4 Gd1 121.8(6) . . ?
C30 N4 Gd1 120.3(5) . . ?
O6 N5 O5 125.2(8) . . ?
O6 N5 C3 117.0(8) . . ?
O5 N5 C3 117.7(7) . . ?
C6 C1 C2 121.7(6) . . ?
C6 C1 S1 117.3(6) . . ?
C2 C1 S1 120.6(5) . . ?
O4 C2 C1 124.6(6) . . ?
O4 C2 C3 120.4(6) . . ?
C1 C2 C3 115.0(6) . . ?
C4 C3 C2 124.4(7) . . ?
C4 C3 N5 121.9(6) . . ?
C2 C3 N5 113.7(6) . . ?
C3 C4 C5 117.2(6) . . ?
C3 C4 C7 122.9(7) . . ?
C5 C4 C7 119.5(7) . . ?
C6 C5 C4 120.9(7) . . ?
C6 C5 H5 119.6 . . ?
C4 C5 H5 119.6 . . ?
C5 C6 C1 120.7(7) . . ?
C5 C6 H6 119.6 . . ?
C1 C6 H6 119.6 . . ?
O7 C7 O8 125.5(7) . . ?
O7 C7 C4 119.4(7) . . ?
O8 C7 C4 115.0(7) . . ?
C9 C8 N1 123.3(9) . . ?
C9 C8 H8 118.4 . . ?
N1 C8 H8 118.4 . . ?
C8 C9 C10 119.2(8) . . ?
C8 C9 H9 120.4 . . ?
C10 C9 H9 120.4 . . ?
C11 C10 C9 120.8(9) . . ?
C11 C10 H10 119.6 . . ?
C9 C10 H10 119.6 . . ?
C10 C11 C19 115.5(9) . . ?
C10 C11 C12 125.2(9) . . ?
C19 C11 C12 119.1(8) . . ?
C13 C12 C11 121.4(8) . . ?
C13 C12 H12 119.3 . . ?
C11 C12 H12 119.3 . . ?
C12 C13 C14 124.0(9) . . ?
C12 C13 H13 118.0 . . ?
C14 C13 H13 118.0 . . ?
C15 C14 C18 117.4(8) . . ?
C15 C14 C13 125.0(9) . . ?
C18 C14 C13 117.6(9) . . ?
C16 C15 C14 120.9(8) . . ?
C16 C15 H15 119.5 . . ?
C14 C15 H15 119.5 . . ?
C15 C16 C17 117.4(8) . . ?
C15 C16 H16 121.3 . . ?
C17 C16 H16 121.3 . . ?
N2 C17 C16 124.2(8) . . ?
N2 C17 H17 117.9 . . ?
C16 C17 H17 117.9 . . ?
N2 C18 C14 122.7(8) . . ?
N2 C18 C19 118.1(7) . . ?
C14 C18 C19 119.2(7) . . ?
N1 C19 C11 123.3(8) . . ?
N1 C19 C18 118.1(6) . . ?
C11 C19 C18 118.6(7) . . ?
N3 C20 C21 124.2(9) . . ?
N3 C20 H20 117.9 . . ?
C21 C20 H20 117.9 . . ?
C22 C21 C20 118.6(10) . . ?
C22 C21 H21 120.7 . . ?
C20 C21 H21 120.7 . . ?
C23 C22 C21 120.8(9) . . ?
C23 C22 H22 119.6 . . ?
C21 C22 H22 119.6 . . ?
C22 C23 C24 126.0(10) . . ?
C22 C23 C31 117.7(9) . . ?
C24 C23 C31 116.3(10) . . ?
C25 C24 C23 124.9(10) . . ?
C25 C24 H24 117.5 . . ?
C23 C24 H24 117.5 . . ?
C24 C25 C26 119.7(10) . . ?
C24 C25 H25 120.1 . . ?
C26 C25 H25 120.1 . . ?
C27 C26 C30 119.0(9) . . ?
C27 C26 C25 122.4(10) . . ?
C30 C26 C25 118.5(10) . . ?
C28 C27 C26 118.7(9) . . ?
C28 C27 H27 120.6 . . ?
C26 C27 H27 120.6 . . ?
C27 C28 C29 119.3(10) . . ?
C27 C28 H28 120.4 . . ?
C29 C28 H28 120.4 . . ?
N4 C29 C28 123.5(10) . . ?
N4 C29 H29 118.2 . . ?
C28 C29 H29 118.2 . . ?
N4 C30 C26 121.8(8) . . ?
N4 C30 C31 117.2(7) . . ?
C26 C30 C31 121.0(8) . . ?
N3 C31 C30 119.5(7) . . ?
N3 C31 C23 120.8(8) . . ?
C30 C31 C23 119.6(8) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O3 S1 O1 Gd1 172.4(4) . . . . ?
O2 S1 O1 Gd1 -59.1(5) . . . . ?
C1 S1 O1 Gd1 57.0(5) . . . . ?
O4 Gd1 O1 S1 -38.2(4) . . . . ?
O8 Gd1 O1 S1 -1.9(6) 2_546 . . . ?
O1W Gd1 O1 S1 149.6(4) . . . . ?
N1 Gd1 O1 S1 48.1(4) . . . . ?
N4 Gd1 O1 S1 -108.2(4) . . . . ?
N3 Gd1 O1 S1 -158.9(5) . . . . ?
N2 Gd1 O1 S1 111.9(4) . . . . ?
O8 Gd1 O4 C2 -162.6(9) 2_546 . . . ?
O1W Gd1 O4 C2 168.5(7) . . . . ?
O1 Gd1 O4 C2 -2.2(8) . . . . ?
N1 Gd1 O4 C2 -88.2(9) . . . . ?
N4 Gd1 O4 C2 116.3(9) . . . . ?
N3 Gd1 O4 C2 61.6(9) . . . . ?
N2 Gd1 O4 C2 -46.0(10) . . . . ?
O4 Gd1 N1 C8 -35.2(7) . . . . ?
O8 Gd1 N1 C8 44.7(7) 2_546 . . . ?
O1W Gd1 N1 C8 111.9(7) . . . . ?
O1 Gd1 N1 C8 -108.9(7) . . . . ?
N4 Gd1 N1 C8 21.5(9) . . . . ?
N3 Gd1 N1 C8 -159.7(6) . . . . ?
N2 Gd1 N1 C8 176.0(7) . . . . ?
O4 Gd1 N1 C19 137.4(6) . . . . ?
O8 Gd1 N1 C19 -142.6(6) 2_546 . . . ?
O1W Gd1 N1 C19 -75.4(6) . . . . ?
O1 Gd1 N1 C19 63.8(6) . . . . ?
N4 Gd1 N1 C19 -165.9(5) . . . . ?
N3 Gd1 N1 C19 13.0(8) . . . . ?
N2 Gd1 N1 C19 -11.3(6) . . . . ?
O4 Gd1 N2 C17 137.8(6) . . . . ?
O8 Gd1 N2 C17 -120.3(6) 2_546 . . . ?
O1W Gd1 N2 C17 -61.1(6) . . . . ?
O1 Gd1 N2 C17 94.2(6) . . . . ?
N1 Gd1 N2 C17 -173.8(7) . . . . ?
N4 Gd1 N2 C17 -13.5(8) . . . . ?
N3 Gd1 N2 C17 19.6(6) . . . . ?
O4 Gd1 N2 C18 -36.6(6) . . . . ?
O8 Gd1 N2 C18 65.3(6) 2_546 . . . ?
O1W Gd1 N2 C18 124.5(6) . . . . ?
O1 Gd1 N2 C18 -80.2(5) . . . . ?
N1 Gd1 N2 C18 11.8(5) . . . . ?
N4 Gd1 N2 C18 172.1(5) . . . . ?
N3 Gd1 N2 C18 -154.8(5) . . . . ?
O4 Gd1 N3 C20 -110.0(6) . . . . ?
O8 Gd1 N3 C20 151.8(6) 2_546 . . . ?
O1W Gd1 N3 C20 102.2(7) . . . . ?
O1 Gd1 N3 C20 -46.6(6) . . . . ?
N1 Gd1 N3 C20 6.9(8) . . . . ?
N4 Gd1 N3 C20 -173.7(7) . . . . ?
N2 Gd1 N3 C20 28.6(6) . . . . ?
O4 Gd1 N3 C31 75.6(6) . . . . ?
O8 Gd1 N3 C31 -22.6(7) 2_546 . . . ?
O1W Gd1 N3 C31 -72.2(6) . . . . ?
O1 Gd1 N3 C31 139.1(6) . . . . ?
N1 Gd1 N3 C31 -167.5(5) . . . . ?
N4 Gd1 N3 C31 11.9(5) . . . . ?
N2 Gd1 N3 C31 -145.8(6) . . . . ?
O4 Gd1 N4 C29 52.6(6) . . . . ?
O8 Gd1 N4 C29 -28.1(6) 2_546 . . . ?
O1W Gd1 N4 C29 -101.4(7) . . . . ?
O1 Gd1 N4 C29 119.0(6) . . . . ?
N1 Gd1 N4 C29 -5.4(9) . . . . ?
N3 Gd1 N4 C29 175.4(7) . . . . ?
N2 Gd1 N4 C29 -147.2(6) . . . . ?
O4 Gd1 N4 C30 -133.6(6) . . . . ?
O8 Gd1 N4 C30 145.7(6) 2_546 . . . ?
O1W Gd1 N4 C30 72.4(5) . . . . ?
O1 Gd1 N4 C30 -67.2(6) . . . . ?
N1 Gd1 N4 C30 168.4(5) . . . . ?
N3 Gd1 N4 C30 -10.9(5) . . . . ?
N2 Gd1 N4 C30 26.5(7) . . . . ?
O3 S1 C1 C6 31.2(7) . . . . ?
O2 S1 C1 C6 -90.4(7) . . . . ?
O1 S1 C1 C6 150.2(6) . . . . ?
O3 S1 C1 C2 -155.4(6) . . . . ?
O2 S1 C1 C2 83.0(7) . . . . ?
O1 S1 C1 C2 -36.3(7) . . . . ?
Gd1 O4 C2 C1 12.7(13) . . . . ?
Gd1 O4 C2 C3 -168.2(6) . . . . ?
C6 C1 C2 O4 -179.8(7) . . . . ?
S1 C1 C2 O4 7.0(10) . . . . ?
C6 C1 C2 C3 1.0(11) . . . . ?
S1 C1 C2 C3 -172.1(5) . . . . ?
O4 C2 C3 C4 -178.2(7) . . . . ?
C1 C2 C3 C4 1.0(11) . . . . ?
O4 C2 C3 N5 0.8(10) . . . . ?
C1 C2 C3 N5 -180.0(6) . . . . ?
O6 N5 C3 C4 -85.6(9) . . . . ?
O5 N5 C3 C4 98.1(9) . . . . ?
O6 N5 C3 C2 95.4(8) . . . . ?
O5 N5 C3 C2 -81.0(9) . . . . ?
C2 C3 C4 C5 -2.9(12) . . . . ?
N5 C3 C4 C5 178.1(7) . . . . ?
C2 C3 C4 C7 169.3(7) . . . . ?
N5 C3 C4 C7 -9.6(12) . . . . ?
C3 C4 C5 C6 2.9(12) . . . . ?
C7 C4 C5 C6 -169.7(8) . . . . ?
C4 C5 C6 C1 -1.0(13) . . . . ?
C2 C1 C6 C5 -1.1(12) . . . . ?
S1 C1 C6 C5 172.3(6) . . . . ?
Gd1 O8 C7 O7 -10.0(15) 2_556 . . . ?
Gd1 O8 C7 C4 165.8(6) 2_556 . . . ?
C3 C4 C7 O7 -3.0(12) . . . . ?
C5 C4 C7 O7 169.1(8) . . . . ?
C3 C4 C7 O8 -179.0(7) . . . . ?
C5 C4 C7 O8 -6.9(11) . . . . ?
C19 N1 C8 C9 0.9(14) . . . . ?
Gd1 N1 C8 C9 173.8(8) . . . . ?
N1 C8 C9 C10 -4.2(17) . . . . ?
C8 C9 C10 C11 4.1(17) . . . . ?
C9 C10 C11 C19 -0.9(16) . . . . ?
C9 C10 C11 C12 174.0(10) . . . . ?
C10 C11 C12 C13 -177.1(12) . . . . ?
C19 C11 C12 C13 -2.3(15) . . . . ?
C11 C12 C13 C14 3.0(17) . . . . ?
C12 C13 C14 C15 175.5(11) . . . . ?
C12 C13 C14 C18 -2.9(16) . . . . ?
C18 C14 C15 C16 1.1(14) . . . . ?
C13 C14 C15 C16 -177.3(10) . . . . ?
C14 C15 C16 C17 1.3(15) . . . . ?
C18 N2 C17 C16 5.5(13) . . . . ?
Gd1 N2 C17 C16 -168.9(7) . . . . ?
C15 C16 C17 N2 -4.8(14) . . . . ?
C17 N2 C18 C14 -2.8(11) . . . . ?
Gd1 N2 C18 C14 172.0(6) . . . . ?
C17 N2 C18 C19 173.3(7) . . . . ?
Gd1 N2 C18 C19 -11.8(9) . . . . ?
C15 C14 C18 N2 -0.4(13) . . . . ?
C13 C14 C18 N2 178.2(8) . . . . ?
C15 C14 C18 C19 -176.5(8) . . . . ?
C13 C14 C18 C19 2.1(12) . . . . ?
C8 N1 C19 C11 2.6(13) . . . . ?
Gd1 N1 C19 C11 -170.3(7) . . . . ?
C8 N1 C19 C18 -176.7(8) . . . . ?
Gd1 N1 C19 C18 10.4(10) . . . . ?
C10 C11 C19 N1 -2.5(14) . . . . ?
C12 C11 C19 N1 -177.7(8) . . . . ?
C10 C11 C19 C18 176.8(9) . . . . ?
C12 C11 C19 C18 1.5(13) . . . . ?
N2 C18 C19 N1 1.5(11) . . . . ?
C14 C18 C19 N1 177.8(7) . . . . ?
N2 C18 C19 C11 -177.8(7) . . . . ?
C14 C18 C19 C11 -1.6(12) . . . . ?
C31 N3 C20 C21 5.6(13) . . . . ?
Gd1 N3 C20 C21 -168.8(7) . . . . ?
N3 C20 C21 C22 -2.3(15) . . . . ?
C20 C21 C22 C23 -3.7(16) . . . . ?
C21 C22 C23 C24 -172.2(10) . . . . ?
C21 C22 C23 C31 5.7(15) . . . . ?
C22 C23 C24 C25 177.0(11) . . . . ?
C31 C23 C24 C25 -1.0(15) . . . . ?
C23 C24 C25 C26 0.2(17) . . . . ?
C24 C25 C26 C27 -175.9(10) . . . . ?
C24 C25 C26 C30 1.3(14) . . . . ?
C30 C26 C27 C28 2.2(15) . . . . ?
C25 C26 C27 C28 179.5(9) . . . . ?
C26 C27 C28 C29 -1.6(16) . . . . ?
C30 N4 C29 C28 0.4(13) . . . . ?
Gd1 N4 C29 C28 174.3(7) . . . . ?
C27 C28 C29 N4 0.3(15) . . . . ?
C29 N4 C30 C26 0.3(11) . . . . ?
Gd1 N4 C30 C26 -173.7(6) . . . . ?
C29 N4 C30 C31 -176.8(7) . . . . ?
Gd1 N4 C30 C31 9.2(9) . . . . ?
C27 C26 C30 N4 -1.6(12) . . . . ?
C25 C26 C30 N4 -178.9(8) . . . . ?
C27 C26 C30 C31 175.3(8) . . . . ?
C25 C26 C30 C31 -2.0(12) . . . . ?
C20 N3 C31 C30 172.4(7) . . . . ?
Gd1 N3 C31 C30 -12.8(10) . . . . ?
C20 N3 C31 C23 -3.2(12) . . . . ?
Gd1 N3 C31 C23 171.6(6) . . . . ?
N4 C30 C31 N3 2.6(11) . . . . ?
C26 C30 C31 N3 -174.4(7) . . . . ?
N4 C30 C31 C23 178.3(7) . . . . ?
C26 C30 C31 C23 1.2(12) . . . . ?
C22 C23 C31 N3 -2.3(13) . . . . ?
C24 C23 C31 N3 175.8(8) . . . . ?
C22 C23 C31 C30 -177.9(8) . . . . ?
C24 C23 C31 C30 0.2(12) . . . . ?

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
O1W H1W1 O7 0.85(8) 1.90(3) 2.689(8) 155(7) 2_546
O1W H1W2 O3 0.85(8) 1.779(13) 2.625(7) 175(7) 2_646

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        27.56
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         1.950
_refine_diff_density_min         -1.584
_refine_diff_density_rms         0.140
####################################################################### 
# 
# 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_7-Er
_database_code_depnum_ccdc_archive 'CCDC 1549874'
_audit_update_record             
;
2017-05-13 deposited with the CCDC.
2017-11-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C31 H20 Er N5 O9 S'
_chemical_formula_sum            'C31 H20 Er N5 O9 S'
_chemical_formula_weight         805.84

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'
Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   11.6194(3)
_cell_length_b                   14.8842(3)
_cell_length_c                   17.4773(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 104.617(2)
_cell_angle_gamma                90.00
_cell_volume                     2924.80(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    4276
_cell_measurement_theta_min      3.28
_cell_measurement_theta_max      27.56

_exptl_crystal_description       block
_exptl_crystal_colour            pink
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.830
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1588
_exptl_absorpt_coefficient_mu    3.008
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5988
_exptl_absorpt_correction_T_max  0.6782
_exptl_absorpt_process_details   
; 
CrysAlis Pro (Agilent, 2013)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1954
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10651
_diffrn_reflns_av_R_equivalents  0.0340
_diffrn_reflns_av_sigmaI/netI    0.0686
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.28
_diffrn_reflns_theta_max         27.56
_reflns_number_total             6682
_reflns_number_gt                5057
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_cell_refinement       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_data_reduction        
;
CrysAlis Pro (Agilent, 2013)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    '(K. Brandenburg, Diamond 3.1, 2009)'
_computing_publication_material  '(K. Brandenburg, Diamond 3.1, 2009)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0135P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6682
_refine_ls_number_parameters     430
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0607
_refine_ls_R_factor_gt           0.0390
_refine_ls_wR_factor_ref         0.0677
_refine_ls_wR_factor_gt          0.0610
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_restrained_S_all      1.002
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Er1 Er 0.811902(18) 0.608983(13) 0.746162(11) 0.02434(6) Uani 1 1 d . . .
S1 S 0.81257(10) 0.38957(8) 0.67258(7) 0.0298(3) Uani 1 1 d . . .
O1 O 0.8741(3) 0.4678(2) 0.71508(17) 0.0333(8) Uani 1 1 d . . .
O1W O 0.8923(3) 0.7524(2) 0.7718(2) 0.0418(9) Uani 1 1 d D . .
H1W1 H 0.9596(18) 0.777(3) 0.787(3) 0.063 Uiso 1 1 d D . .
H1W2 H 0.840(3) 0.791(2) 0.750(3) 0.063 Uiso 1 1 d D . .
O2 O 0.7599(3) 0.4098(2) 0.59057(17) 0.0487(10) Uani 1 1 d . . .
O3 O 0.8873(3) 0.3112(2) 0.6837(2) 0.0531(10) Uani 1 1 d . . .
O4 O 0.6675(3) 0.51506(19) 0.75376(18) 0.0332(8) Uani 1 1 d . . .
O5 O 0.4062(4) 0.5245(3) 0.7542(3) 0.0742(13) Uani 1 1 d . . .
O6 O 0.4971(4) 0.4841(3) 0.8736(2) 0.0846(15) Uani 1 1 d . . .
O7 O 0.3045(3) 0.3491(2) 0.7905(2) 0.0455(9) Uani 1 1 d . . .
O8 O 0.3437(3) 0.2072(2) 0.76615(19) 0.0384(8) Uani 1 1 d . . .
N1 N 0.7102(3) 0.6125(3) 0.6039(2) 0.0346(9) Uani 1 1 d . . .
N2 N 0.9473(4) 0.6336(2) 0.6521(2) 0.0324(9) Uani 1 1 d . . .
N3 N 1.0056(4) 0.5751(3) 0.8476(2) 0.0330(9) Uani 1 1 d . . .
N4 N 0.8072(4) 0.6274(3) 0.8881(2) 0.0366(10) Uani 1 1 d . . .
N5 N 0.4728(4) 0.4745(3) 0.8011(3) 0.0476(12) Uani 1 1 d . . .
C1 C 0.6947(4) 0.3633(3) 0.7156(2) 0.0249(10) Uani 1 1 d . . .
C2 C 0.6360(4) 0.4320(3) 0.7465(2) 0.0254(10) Uani 1 1 d . . .
C3 C 0.5344(4) 0.4024(3) 0.7697(2) 0.0256(10) Uani 1 1 d . . .
C4 C 0.4914(4) 0.3143(3) 0.7631(2) 0.0278(10) Uani 1 1 d . . .
C5 C 0.5569(4) 0.2500(3) 0.7346(3) 0.0376(12) Uani 1 1 d . . .
H5 H 0.5332 0.1901 0.7313 0.045 Uiso 1 1 calc R . .
C6 C 0.6567(4) 0.2752(3) 0.7113(3) 0.0354(12) Uani 1 1 d . . .
H6 H 0.6997 0.2317 0.6921 0.043 Uiso 1 1 calc R . .
C7 C 0.3709(4) 0.2894(3) 0.7759(3) 0.0310(11) Uani 1 1 d . . .
C8 C 0.5930(5) 0.6098(4) 0.5789(3) 0.0500(14) Uani 1 1 d . . .
H8 H 0.5488 0.6115 0.6164 0.060 Uiso 1 1 calc R . .
C9 C 0.5321(6) 0.6045(4) 0.4995(4) 0.0642(17) Uani 1 1 d . . .
H9 H 0.4495 0.6056 0.4841 0.077 Uiso 1 1 calc R . .
C10 C 0.5970(7) 0.5979(4) 0.4454(3) 0.068(2) Uani 1 1 d . . .
H10 H 0.5578 0.5918 0.3922 0.081 Uiso 1 1 calc R . .
C11 C 0.7199(6) 0.6001(4) 0.4669(3) 0.0515(15) Uani 1 1 d . . .
C12 C 0.7926(7) 0.5961(4) 0.4128(3) 0.0624(19) Uani 1 1 d . . .
H12 H 0.7576 0.5877 0.3593 0.075 Uiso 1 1 calc R . .
C13 C 0.9085(7) 0.6039(4) 0.4372(3) 0.0638(18) Uani 1 1 d . . .
H13 H 0.9533 0.6003 0.4001 0.077 Uiso 1 1 calc R . .
C14 C 0.9688(6) 0.6178(3) 0.5182(3) 0.0477(15) Uani 1 1 d . . .
C15 C 1.0918(6) 0.6303(4) 0.5461(3) 0.0543(16) Uani 1 1 d . . .
H15 H 1.1406 0.6265 0.5115 0.065 Uiso 1 1 calc R . .
C16 C 1.1386(5) 0.6479(4) 0.6229(3) 0.0526(15) Uani 1 1 d . . .
H16 H 1.2199 0.6577 0.6420 0.063 Uiso 1 1 calc R . .
C17 C 1.0636(5) 0.6511(3) 0.6734(3) 0.0418(13) Uani 1 1 d . . .
H17 H 1.0969 0.6666 0.7259 0.050 Uiso 1 1 calc R . .
C18 C 0.8994(5) 0.6185(3) 0.5741(3) 0.0357(12) Uani 1 1 d . . .
C19 C 0.7746(5) 0.6093(3) 0.5489(3) 0.0386(12) Uani 1 1 d . . .
C20 C 1.1026(5) 0.5410(4) 0.8309(3) 0.0463(14) Uani 1 1 d . . .
H20 H 1.0958 0.5185 0.7804 0.056 Uiso 1 1 calc R . .
C21 C 1.2138(5) 0.5372(4) 0.8850(4) 0.0586(16) Uani 1 1 d . . .
H21 H 1.2798 0.5159 0.8696 0.070 Uiso 1 1 calc R . .
C22 C 1.2240(6) 0.5648(4) 0.9596(4) 0.0641(18) Uani 1 1 d . . .
H22 H 1.2979 0.5637 0.9958 0.077 Uiso 1 1 calc R . .
C23 C 1.1251(6) 0.5947(3) 0.9830(3) 0.0493(15) Uani 1 1 d . . .
C24 C 1.1237(7) 0.6170(4) 1.0624(3) 0.070(2) Uani 1 1 d . . .
H24 H 1.1944 0.6152 1.1018 0.084 Uiso 1 1 calc R . .
C25 C 1.0235(8) 0.6404(4) 1.0815(3) 0.069(2) Uani 1 1 d . . .
H25 H 1.0266 0.6536 1.1340 0.083 Uiso 1 1 calc R . .
C26 C 0.9132(6) 0.6457(3) 1.0249(3) 0.0502(16) Uani 1 1 d . . .
C27 C 0.8070(7) 0.6653(4) 1.0432(4) 0.065(2) Uani 1 1 d . . .
H27 H 0.8064 0.6784 1.0951 0.078 Uiso 1 1 calc R . .
C28 C 0.7049(7) 0.6656(4) 0.9863(4) 0.0664(19) Uani 1 1 d . . .
H28 H 0.6332 0.6783 0.9986 0.080 Uiso 1 1 calc R . .
C29 C 0.7073(5) 0.6465(3) 0.9083(3) 0.0507(15) Uani 1 1 d . . .
H29 H 0.6362 0.6473 0.8691 0.061 Uiso 1 1 calc R . .
C30 C 0.9099(5) 0.6260(3) 0.9453(3) 0.0389(13) Uani 1 1 d . . .
C31 C 1.0163(5) 0.6001(3) 0.9241(3) 0.0361(12) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Er1 O4 2.214(3) . ?
Er1 O8 2.293(3) 2_656 ?
Er1 O1W 2.328(3) . ?
Er1 O1 2.331(3) . ?
Er1 N1 2.469(4) . ?
Er1 N4 2.509(4) . ?
Er1 N3 2.540(4) . ?
Er1 N2 2.573(4) . ?
S1 O3 1.438(3) . ?
S1 O2 1.441(3) . ?
S1 O1 1.467(3) . ?
S1 C1 1.765(4) . ?
O1W H1W1 0.85(5) . ?
O1W H1W2 0.85(5) . ?
O4 C2 1.287(5) . ?
O5 N5 1.227(6) . ?
O6 N5 1.235(5) . ?
O7 C7 1.244(5) . ?
O8 C7 1.265(5) . ?
O8 Er1 2.293(3) 2_646 ?
N1 C8 1.321(6) . ?
N1 C19 1.360(6) . ?
N2 C17 1.334(6) . ?
N2 C18 1.354(6) . ?
N3 C20 1.333(6) . ?
N3 C31 1.363(5) . ?
N4 C29 1.327(6) . ?
N4 C30 1.350(6) . ?
N5 C3 1.470(6) . ?
C1 C6 1.379(6) . ?
C1 C2 1.410(6) . ?
C2 C3 1.412(6) . ?
C3 C4 1.398(6) . ?
C4 C5 1.391(6) . ?
C4 C7 1.519(6) . ?
C5 C6 1.375(6) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C8 C9 1.392(7) . ?
C8 H8 0.9300 . ?
C9 C10 1.354(8) . ?
C9 H9 0.9300 . ?
C10 C11 1.382(8) . ?
C10 H10 0.9300 . ?
C11 C12 1.419(8) . ?
C11 C19 1.421(6) . ?
C12 C13 1.311(8) . ?
C12 H12 0.9300 . ?
C13 C14 1.428(8) . ?
C13 H13 0.9300 . ?
C14 C15 1.401(8) . ?
C14 C18 1.415(6) . ?
C15 C16 1.340(7) . ?
C15 H15 0.9300 . ?
C16 C17 1.389(6) . ?
C16 H16 0.9300 . ?
C17 H17 0.9300 . ?
C18 C19 1.411(7) . ?
C20 C21 1.396(7) . ?
C20 H20 0.9300 . ?
C21 C22 1.343(7) . ?
C21 H21 0.9300 . ?
C22 C23 1.386(8) . ?
C22 H22 0.9300 . ?
C23 C31 1.417(7) . ?
C23 C24 1.432(8) . ?
C24 C25 1.335(9) . ?
C24 H24 0.9300 . ?
C25 C26 1.410(9) . ?
C25 H25 0.9300 . ?
C26 C27 1.381(8) . ?
C26 C30 1.413(6) . ?
C27 C28 1.342(8) . ?
C27 H27 0.9300 . ?
C28 C29 1.401(7) . ?
C28 H28 0.9300 . ?
C29 H29 0.9300 . ?
C30 C31 1.429(7) . ?

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 Er1 O8 79.43(11) . 2_656 ?
O4 Er1 O1W 147.24(11) . . ?
O8 Er1 O1W 72.66(12) 2_656 . ?
O4 Er1 O1 74.28(10) . . ?
O8 Er1 O1 146.80(11) 2_656 . ?
O1W Er1 O1 137.62(11) . . ?
O4 Er1 N1 84.06(12) . . ?
O8 Er1 N1 74.10(12) 2_656 . ?
O1W Er1 N1 103.94(13) . . ?
O1 Er1 N1 83.25(12) . . ?
O4 Er1 N4 78.68(12) . . ?
O8 Er1 N4 79.04(12) 2_656 . ?
O1W Er1 N4 79.49(13) . . ?
O1 Er1 N4 114.46(12) . . ?
N1 Er1 N4 150.28(14) . . ?
O4 Er1 N3 112.61(12) . . ?
O8 Er1 N3 136.98(12) 2_656 . ?
O1W Er1 N3 78.81(12) . . ?
O1 Er1 N3 73.22(11) . . ?
N1 Er1 N3 145.27(13) . . ?
N4 Er1 N3 64.42(13) . . ?
O4 Er1 N2 136.34(11) . . ?
O8 Er1 N2 116.36(12) 2_656 . ?
O1W Er1 N2 73.25(12) . . ?
O1 Er1 N2 72.77(11) . . ?
N1 Er1 N2 64.41(13) . . ?
N4 Er1 N2 141.76(13) . . ?
N3 Er1 N2 84.11(12) . . ?
O3 S1 O2 113.2(2) . . ?
O3 S1 O1 112.0(2) . . ?
O2 S1 O1 111.6(2) . . ?
O3 S1 C1 105.6(2) . . ?
O2 S1 C1 106.8(2) . . ?
O1 S1 C1 107.00(19) . . ?
S1 O1 Er1 133.90(18) . . ?
Er1 O1W H1W1 139(3) . . ?
Er1 O1W H1W2 109(3) . . ?
H1W1 O1W H1W2 110.4(17) . . ?
C2 O4 Er1 143.3(3) . . ?
C7 O8 Er1 142.5(3) . 2_646 ?
C8 N1 C19 118.0(4) . . ?
C8 N1 Er1 121.6(3) . . ?
C19 N1 Er1 120.1(3) . . ?
C17 N2 C18 116.3(4) . . ?
C17 N2 Er1 126.1(3) . . ?
C18 N2 Er1 117.2(3) . . ?
C20 N3 C31 116.5(4) . . ?
C20 N3 Er1 124.9(3) . . ?
C31 N3 Er1 118.4(3) . . ?
C29 N4 C30 118.4(4) . . ?
C29 N4 Er1 121.7(4) . . ?
C30 N4 Er1 119.6(3) . . ?
O5 N5 O6 123.9(5) . . ?
O5 N5 C3 118.5(4) . . ?
O6 N5 C3 117.5(5) . . ?
C6 C1 C2 122.1(4) . . ?
C6 C1 S1 117.4(3) . . ?
C2 C1 S1 120.3(3) . . ?
O4 C2 C1 125.6(4) . . ?
O4 C2 C3 120.6(4) . . ?
C1 C2 C3 113.9(4) . . ?
C4 C3 C2 125.2(4) . . ?
C4 C3 N5 121.2(4) . . ?
C2 C3 N5 113.7(4) . . ?
C5 C4 C3 117.3(4) . . ?
C5 C4 C7 119.6(4) . . ?
C3 C4 C7 122.7(4) . . ?
C6 C5 C4 119.8(4) . . ?
C6 C5 H5 120.1 . . ?
C4 C5 H5 120.1 . . ?
C5 C6 C1 121.7(4) . . ?
C5 C6 H6 119.2 . . ?
C1 C6 H6 119.2 . . ?
O7 C7 O8 124.8(4) . . ?
O7 C7 C4 119.9(4) . . ?
O8 C7 C4 115.1(4) . . ?
N1 C8 C9 123.6(6) . . ?
N1 C8 H8 118.2 . . ?
C9 C8 H8 118.2 . . ?
C10 C9 C8 117.9(6) . . ?
C10 C9 H9 121.0 . . ?
C8 C9 H9 121.0 . . ?
C9 C10 C11 121.8(5) . . ?
C9 C10 H10 119.1 . . ?
C11 C10 H10 119.1 . . ?
C10 C11 C12 124.5(5) . . ?
C10 C11 C19 116.5(5) . . ?
C12 C11 C19 119.0(6) . . ?
C13 C12 C11 121.0(5) . . ?
C13 C12 H12 119.5 . . ?
C11 C12 H12 119.5 . . ?
C12 C13 C14 122.8(6) . . ?
C12 C13 H13 118.6 . . ?
C14 C13 H13 118.6 . . ?
C15 C14 C18 117.9(5) . . ?
C15 C14 C13 124.5(5) . . ?
C18 C14 C13 117.6(6) . . ?
C16 C15 C14 119.7(5) . . ?
C16 C15 H15 120.1 . . ?
C14 C15 H15 120.1 . . ?
C15 C16 C17 118.8(6) . . ?
C15 C16 H16 120.6 . . ?
C17 C16 H16 120.6 . . ?
N2 C17 C16 124.7(5) . . ?
N2 C17 H17 117.6 . . ?
C16 C17 H17 117.6 . . ?
N2 C18 C19 117.4(4) . . ?
N2 C18 C14 122.3(5) . . ?
C19 C18 C14 120.2(4) . . ?
N1 C19 C18 118.7(4) . . ?
N1 C19 C11 122.0(5) . . ?
C18 C19 C11 119.2(5) . . ?
N3 C20 C21 123.8(5) . . ?
N3 C20 H20 118.1 . . ?
C21 C20 H20 118.1 . . ?
C22 C21 C20 118.9(6) . . ?
C22 C21 H21 120.5 . . ?
C20 C21 H21 120.5 . . ?
C21 C22 C23 120.6(6) . . ?
C21 C22 H22 119.7 . . ?
C23 C22 H22 119.7 . . ?
C22 C23 C31 117.2(5) . . ?
C22 C23 C24 125.0(6) . . ?
C31 C23 C24 117.7(6) . . ?
C25 C24 C23 121.8(6) . . ?
C25 C24 H24 119.1 . . ?
C23 C24 H24 119.1 . . ?
C24 C25 C26 122.3(6) . . ?
C24 C25 H25 118.8 . . ?
C26 C25 H25 118.8 . . ?
C27 C26 C25 123.8(6) . . ?
C27 C26 C30 117.9(6) . . ?
C25 C26 C30 118.2(6) . . ?
C28 C27 C26 120.3(6) . . ?
C28 C27 H27 119.9 . . ?
C26 C27 H27 119.9 . . ?
C27 C28 C29 119.3(6) . . ?
C27 C28 H28 120.4 . . ?
C29 C28 H28 120.4 . . ?
N4 C29 C28 122.5(6) . . ?
N4 C29 H29 118.8 . . ?
C28 C29 H29 118.8 . . ?
N4 C30 C26 121.7(5) . . ?
N4 C30 C31 118.3(4) . . ?
C26 C30 C31 120.0(5) . . ?
N3 C31 C23 122.7(5) . . ?
N3 C31 C30 117.2(4) . . ?
C23 C31 C30 119.9(5) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O3 S1 O1 Er1 -167.6(2) . . . . ?
O2 S1 O1 Er1 64.3(3) . . . . ?
C1 S1 O1 Er1 -52.3(3) . . . . ?
O4 Er1 O1 S1 35.7(2) . . . . ?
O8 Er1 O1 S1 -3.2(4) 2_656 . . . ?
O1W Er1 O1 S1 -153.3(2) . . . . ?
N1 Er1 O1 S1 -50.0(2) . . . . ?
N4 Er1 O1 S1 105.1(3) . . . . ?
N3 Er1 O1 S1 155.8(3) . . . . ?
N2 Er1 O1 S1 -115.3(3) . . . . ?
O8 Er1 O4 C2 160.3(5) 2_656 . . . ?
O1W Er1 O4 C2 -167.9(4) . . . . ?
O1 Er1 O4 C2 0.8(5) . . . . ?
N1 Er1 O4 C2 85.4(5) . . . . ?
N4 Er1 O4 C2 -118.9(5) . . . . ?
N3 Er1 O4 C2 -62.9(5) . . . . ?
N2 Er1 O4 C2 43.0(5) . . . . ?
O4 Er1 N1 C8 36.8(4) . . . . ?
O8 Er1 N1 C8 -43.9(4) 2_656 . . . ?
O1W Er1 N1 C8 -110.9(4) . . . . ?
O1 Er1 N1 C8 111.6(4) . . . . ?
N4 Er1 N1 C8 -17.8(6) . . . . ?
N3 Er1 N1 C8 158.6(4) . . . . ?
N2 Er1 N1 C8 -174.3(4) . . . . ?
O4 Er1 N1 C19 -137.3(4) . . . . ?
O8 Er1 N1 C19 142.0(4) 2_656 . . . ?
O1W Er1 N1 C19 75.0(4) . . . . ?
O1 Er1 N1 C19 -62.5(3) . . . . ?
N4 Er1 N1 C19 168.1(3) . . . . ?
N3 Er1 N1 C19 -15.5(5) . . . . ?
N2 Er1 N1 C19 11.6(3) . . . . ?
O4 Er1 N2 C17 -137.3(4) . . . . ?
O8 Er1 N2 C17 119.8(4) 2_656 . . . ?
O1W Er1 N2 C17 59.6(4) . . . . ?
O1 Er1 N2 C17 -94.7(4) . . . . ?
N1 Er1 N2 C17 174.6(4) . . . . ?
N4 Er1 N2 C17 13.2(5) . . . . ?
N3 Er1 N2 C17 -20.5(4) . . . . ?
O4 Er1 N2 C18 35.4(4) . . . . ?
O8 Er1 N2 C18 -67.4(3) 2_656 . . . ?
O1W Er1 N2 C18 -127.7(3) . . . . ?
O1 Er1 N2 C18 78.1(3) . . . . ?
N1 Er1 N2 C18 -12.6(3) . . . . ?
N4 Er1 N2 C18 -174.1(3) . . . . ?
N3 Er1 N2 C18 152.3(3) . . . . ?
O4 Er1 N3 C20 109.1(4) . . . . ?
O8 Er1 N3 C20 -151.9(4) 2_656 . . . ?
O1W Er1 N3 C20 -103.1(4) . . . . ?
O1 Er1 N3 C20 44.7(4) . . . . ?
N1 Er1 N3 C20 -4.7(5) . . . . ?
N4 Er1 N3 C20 173.3(4) . . . . ?
N2 Er1 N3 C20 -29.0(4) . . . . ?
O4 Er1 N3 C31 -76.7(3) . . . . ?
O8 Er1 N3 C31 22.2(4) 2_656 . . . ?
O1W Er1 N3 C31 71.1(3) . . . . ?
O1 Er1 N3 C31 -141.1(3) . . . . ?
N1 Er1 N3 C31 169.5(3) . . . . ?
N4 Er1 N3 C31 -12.5(3) . . . . ?
N2 Er1 N3 C31 145.2(3) . . . . ?
O4 Er1 N4 C29 -52.8(4) . . . . ?
O8 Er1 N4 C29 28.5(4) 2_656 . . . ?
O1W Er1 N4 C29 102.6(4) . . . . ?
O1 Er1 N4 C29 -119.5(4) . . . . ?
N1 Er1 N4 C29 2.9(5) . . . . ?
N3 Er1 N4 C29 -174.8(4) . . . . ?
N2 Er1 N4 C29 147.5(3) . . . . ?
O4 Er1 N4 C30 133.4(4) . . . . ?
O8 Er1 N4 C30 -145.4(4) 2_656 . . . ?
O1W Er1 N4 C30 -71.2(3) . . . . ?
O1 Er1 N4 C30 66.6(4) . . . . ?
N1 Er1 N4 C30 -170.9(3) . . . . ?
N3 Er1 N4 C30 11.3(3) . . . . ?
N2 Er1 N4 C30 -26.4(4) . . . . ?
O3 S1 C1 C6 -33.4(4) . . . . ?
O2 S1 C1 C6 87.4(4) . . . . ?
O1 S1 C1 C6 -153.0(4) . . . . ?
O3 S1 C1 C2 152.1(4) . . . . ?
O2 S1 C1 C2 -87.1(4) . . . . ?
O1 S1 C1 C2 32.5(4) . . . . ?
Er1 O4 C2 C1 -9.9(8) . . . . ?
Er1 O4 C2 C3 170.7(3) . . . . ?
C6 C1 C2 O4 178.7(4) . . . . ?
S1 C1 C2 O4 -7.1(6) . . . . ?
C6 C1 C2 C3 -1.9(6) . . . . ?
S1 C1 C2 C3 172.3(3) . . . . ?
O4 C2 C3 C4 178.8(4) . . . . ?
C1 C2 C3 C4 -0.7(6) . . . . ?
O4 C2 C3 N5 0.1(6) . . . . ?
C1 C2 C3 N5 -179.4(4) . . . . ?
O5 N5 C3 C4 -98.8(6) . . . . ?
O6 N5 C3 C4 85.5(6) . . . . ?
O5 N5 C3 C2 80.0(6) . . . . ?
O6 N5 C3 C2 -95.8(5) . . . . ?
C2 C3 C4 C5 3.0(7) . . . . ?
N5 C3 C4 C5 -178.4(4) . . . . ?
C2 C3 C4 C7 -169.4(4) . . . . ?
N5 C3 C4 C7 9.2(7) . . . . ?
C3 C4 C5 C6 -2.7(7) . . . . ?
C7 C4 C5 C6 169.9(4) . . . . ?
C4 C5 C6 C1 0.3(8) . . . . ?
C2 C1 C6 C5 2.2(7) . . . . ?
S1 C1 C6 C5 -172.2(4) . . . . ?
Er1 O8 C7 O7 7.6(8) 2_646 . . . ?
Er1 O8 C7 C4 -168.5(3) 2_646 . . . ?
C5 C4 C7 O7 -169.8(4) . . . . ?
C3 C4 C7 O7 2.3(7) . . . . ?
C5 C4 C7 O8 6.5(6) . . . . ?
C3 C4 C7 O8 178.6(4) . . . . ?
C19 N1 C8 C9 -0.6(8) . . . . ?
Er1 N1 C8 C9 -174.8(4) . . . . ?
N1 C8 C9 C10 3.0(9) . . . . ?
C8 C9 C10 C11 -2.7(10) . . . . ?
C9 C10 C11 C12 -178.1(6) . . . . ?
C9 C10 C11 C19 0.2(9) . . . . ?
C10 C11 C12 C13 175.8(7) . . . . ?
C19 C11 C12 C13 -2.4(9) . . . . ?
C11 C12 C13 C14 -0.7(11) . . . . ?
C12 C13 C14 C15 -177.1(6) . . . . ?
C12 C13 C14 C18 3.1(9) . . . . ?
C18 C14 C15 C16 -4.0(8) . . . . ?
C13 C14 C15 C16 176.2(5) . . . . ?
C14 C15 C16 C17 1.5(9) . . . . ?
C18 N2 C17 C16 -5.2(7) . . . . ?
Er1 N2 C17 C16 167.6(4) . . . . ?
C15 C16 C17 N2 3.4(8) . . . . ?
C17 N2 C18 C19 -173.5(4) . . . . ?
Er1 N2 C18 C19 13.0(5) . . . . ?
C17 N2 C18 C14 2.3(7) . . . . ?
Er1 N2 C18 C14 -171.1(4) . . . . ?
C15 C14 C18 N2 2.1(8) . . . . ?
C13 C14 C18 N2 -178.1(5) . . . . ?
C15 C14 C18 C19 177.8(5) . . . . ?
C13 C14 C18 C19 -2.4(7) . . . . ?
C8 N1 C19 C18 175.6(5) . . . . ?
Er1 N1 C19 C18 -10.1(6) . . . . ?
C8 N1 C19 C11 -2.2(7) . . . . ?
Er1 N1 C19 C11 172.1(4) . . . . ?
N2 C18 C19 N1 -2.4(7) . . . . ?
C14 C18 C19 N1 -178.4(4) . . . . ?
N2 C18 C19 C11 175.4(4) . . . . ?
C14 C18 C19 C11 -0.6(7) . . . . ?
C10 C11 C19 N1 2.3(8) . . . . ?
C12 C11 C19 N1 -179.2(5) . . . . ?
C10 C11 C19 C18 -175.4(5) . . . . ?
C12 C11 C19 C18 3.0(8) . . . . ?
C31 N3 C20 C21 -5.7(8) . . . . ?
Er1 N3 C20 C21 168.6(4) . . . . ?
N3 C20 C21 C22 3.7(9) . . . . ?
C20 C21 C22 C23 1.4(9) . . . . ?
C21 C22 C23 C31 -3.8(8) . . . . ?
C21 C22 C23 C24 173.5(6) . . . . ?
C22 C23 C24 C25 -175.9(6) . . . . ?
C31 C23 C24 C25 1.4(9) . . . . ?
C23 C24 C25 C26 -0.8(10) . . . . ?
C24 C25 C26 C27 176.7(6) . . . . ?
C24 C25 C26 C30 -0.5(9) . . . . ?
C25 C26 C27 C28 -177.3(6) . . . . ?
C30 C26 C27 C28 -0.2(9) . . . . ?
C26 C27 C28 C29 -0.5(9) . . . . ?
C30 N4 C29 C28 0.3(8) . . . . ?
Er1 N4 C29 C28 -173.7(4) . . . . ?
C27 C28 C29 N4 0.5(9) . . . . ?
C29 N4 C30 C26 -1.0(7) . . . . ?
Er1 N4 C30 C26 173.1(3) . . . . ?
C29 N4 C30 C31 176.3(4) . . . . ?
Er1 N4 C30 C31 -9.7(6) . . . . ?
C27 C26 C30 N4 0.9(7) . . . . ?
C25 C26 C30 N4 178.3(5) . . . . ?
C27 C26 C30 C31 -176.3(5) . . . . ?
C25 C26 C30 C31 1.0(7) . . . . ?
C20 N3 C31 C23 2.9(7) . . . . ?
Er1 N3 C31 C23 -171.8(4) . . . . ?
C20 N3 C31 C30 -172.3(4) . . . . ?
Er1 N3 C31 C30 13.1(5) . . . . ?
C22 C23 C31 N3 1.7(8) . . . . ?
C24 C23 C31 N3 -175.8(5) . . . . ?
C22 C23 C31 C30 176.8(5) . . . . ?
C24 C23 C31 C30 -0.8(7) . . . . ?
N4 C30 C31 N3 -2.4(7) . . . . ?
C26 C30 C31 N3 174.9(4) . . . . ?
N4 C30 C31 C23 -177.7(4) . . . . ?
C26 C30 C31 C23 -0.4(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
O1W H1W1 O3 0.85(5) 1.795(12) 2.631(5) 170(5) 2_756
O1W H1W2 O7 0.85(5) 1.864(15) 2.688(5) 163(4) 2_656

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        27.56
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         0.875
_refine_diff_density_min         -0.686
_refine_diff_density_rms         0.117
####################################################################### 
# 
# 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_7-Tb
_database_code_depnum_ccdc_archive 'CCDC 1549872'
_audit_update_record             
;
2017-05-13 deposited with the CCDC.
2017-11-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C31 H20 N5 O9 S Tb'
_chemical_formula_sum            'C31 H20 N5 O9 S Tb'
_chemical_formula_weight         797.50

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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   11.5956(5)
_cell_length_b                   14.8563(5)
_cell_length_c                   17.5154(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 104.709(4)
_cell_angle_gamma                90.00
_cell_volume                     2918.5(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    3555
_cell_measurement_theta_min      3.61
_cell_measurement_theta_max      28.99

_exptl_crystal_description       prism
_exptl_crystal_colour            deepred
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.815
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1576
_exptl_absorpt_coefficient_mu    2.562
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6026
_exptl_absorpt_correction_T_max  0.7156
_exptl_absorpt_process_details   
; 
CrysAlis Pro (Agilent, 2013)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1954
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10769
_diffrn_reflns_av_R_equivalents  0.0318
_diffrn_reflns_av_sigmaI/netI    0.0621
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         3.34
_diffrn_reflns_theta_max         27.56
_reflns_number_total             6692
_reflns_number_gt                5353
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_cell_refinement       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_data_reduction        
;
CrysAlis Pro (Agilent, 2013)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    '(K. Brandenburg, Diamond 3.1, 2009)'
_computing_publication_material  '(K. Brandenburg, Diamond 3.1, 2009)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0790P)²+27.6214P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6692
_refine_ls_number_parameters     430
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0696
_refine_ls_R_factor_gt           0.0542
_refine_ls_wR_factor_ref         0.1714
_refine_ls_wR_factor_gt          0.1615
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.023
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb 0.68559(3) 0.89266(2) 0.75505(2) 0.02324(13) Uani 1 1 d . . .
S2 S 1.31075(16) 0.61398(13) 0.67225(12) 0.0276(4) Uani 1 1 d . . .
O1 O 1.3760(5) 0.5377(4) 0.7158(4) 0.0358(13) Uani 1 1 d . . .
O1W O 0.6061(5) 0.7462(4) 0.7315(4) 0.0421(15) Uani 1 1 d D . .
H1W1 H 0.655(6) 0.706(5) 0.755(6) 0.063 Uiso 1 1 d D . .
H1W2 H 0.535(3) 0.727(6) 0.724(6) 0.063 Uiso 1 1 d D . .
O2 O 1.3838(5) 0.6939(5) 0.6807(5) 0.0507(18) Uani 1 1 d . . .
O3 O 1.2560(6) 0.5906(5) 0.5921(4) 0.0445(16) Uani 1 1 d . . .
O4 O 1.1672(5) 0.4865(4) 0.7521(3) 0.0343(13) Uani 1 1 d . . .
O5 O 0.9061(8) 0.4760(5) 0.7538(6) 0.069(2) Uani 1 1 d . . .
O6 O 0.9994(8) 0.5146(7) 0.8719(5) 0.078(3) Uani 1 1 d . . .
O7 O 0.8428(5) 0.7927(4) 0.7686(4) 0.0403(15) Uani 1 1 d . . .
O8 O 0.8046(6) 0.6508(5) 0.7913(4) 0.0452(16) Uani 1 1 d . . .
N1 N 0.9727(7) 0.5257(6) 0.8009(5) 0.0441(19) Uani 1 1 d . . .
N2 N 0.6897(7) 0.8720(5) 0.6115(4) 0.0365(17) Uani 1 1 d . . .
N3 N 0.4889(6) 0.9261(5) 0.6502(4) 0.0330(15) Uani 1 1 d . . .
N4 N 0.5483(6) 0.8687(5) 0.8494(4) 0.0340(16) Uani 1 1 d . . .
N5 N 0.7866(6) 0.8872(5) 0.8994(4) 0.0340(16) Uani 1 1 d . . .
C1 C 1.1942(7) 0.6401(6) 0.7155(5) 0.0278(16) Uani 1 1 d . . .
C2 C 1.1345(6) 0.5705(5) 0.7459(4) 0.0241(15) Uani 1 1 d . . .
C3 C 1.0330(7) 0.5990(5) 0.7703(5) 0.0275(16) Uani 1 1 d . . .
C4 C 0.9893(7) 0.6859(6) 0.7638(5) 0.0287(16) Uani 1 1 d . . .
C5 C 1.0542(7) 0.7512(6) 0.7364(6) 0.039(2) Uani 1 1 d . . .
H5 H 1.0303 0.8111 0.7344 0.046 Uiso 1 1 calc R . .
C6 C 1.1539(7) 0.7273(6) 0.7124(5) 0.0345(18) Uani 1 1 d . . .
H6 H 1.1955 0.7718 0.6932 0.041 Uiso 1 1 calc R . .
C7 C 0.8707(7) 0.7107(6) 0.7776(5) 0.0331(18) Uani 1 1 d . . .
C8 C 0.7892(10) 0.8533(8) 0.5926(6) 0.050(2) Uani 1 1 d . . .
H8 H 0.8602 0.8524 0.6319 0.060 Uiso 1 1 calc R . .
C9 C 0.7917(14) 0.8343(8) 0.5139(8) 0.070(4) Uani 1 1 d . . .
H9 H 0.8637 0.8225 0.5016 0.085 Uiso 1 1 calc R . .
C10 C 0.6890(14) 0.8334(8) 0.4569(7) 0.063(3) Uani 1 1 d . . .
H10 H 0.6891 0.8177 0.4055 0.076 Uiso 1 1 calc R . .
C11 C 0.5821(11) 0.8563(7) 0.4754(6) 0.051(3) Uani 1 1 d . . .
C12 C 0.4706(17) 0.8592(9) 0.4172(7) 0.079(5) Uani 1 1 d . . .
H12 H 0.4666 0.8440 0.3651 0.095 Uiso 1 1 calc R . .
C13 C 0.3750(16) 0.8835(8) 0.4377(7) 0.069(4) Uani 1 1 d . . .
H13 H 0.3042 0.8864 0.3982 0.083 Uiso 1 1 calc R . .
C14 C 0.3704(10) 0.9056(7) 0.5148(6) 0.051(3) Uani 1 1 d . . .
C15 C 0.2739(11) 0.9350(9) 0.5370(8) 0.069(4) Uani 1 1 d . . .
H15 H 0.2000 0.9354 0.5006 0.083 Uiso 1 1 calc R . .
C16 C 0.2830(9) 0.9645(8) 0.6125(7) 0.060(3) Uani 1 1 d . . .
H16 H 0.2168 0.9871 0.6270 0.072 Uiso 1 1 calc R . .
C17 C 0.3929(8) 0.9599(7) 0.6666(6) 0.047(2) Uani 1 1 d . . .
H17 H 0.3994 0.9818 0.7172 0.056 Uiso 1 1 calc R . .
C18 C 0.4816(9) 0.8998(6) 0.5752(5) 0.040(2) Uani 1 1 d . . .
C19 C 0.5859(9) 0.8746(6) 0.5540(5) 0.037(2) Uani 1 1 d . . .
C20 C 0.4304(8) 0.8521(7) 0.8270(6) 0.041(2) Uani 1 1 d . . .
H20 H 0.3968 0.8381 0.7743 0.050 Uiso 1 1 calc R . .
C21 C 0.3558(10) 0.8546(8) 0.8777(7) 0.052(3) Uani 1 1 d . . .
H21 H 0.2741 0.8457 0.8589 0.062 Uiso 1 1 calc R . .
C22 C 0.4051(11) 0.8704(8) 0.9550(7) 0.053(3) Uani 1 1 d . . .
H22 H 0.3565 0.8727 0.9898 0.064 Uiso 1 1 calc R . .
C23 C 0.5253(11) 0.8830(7) 0.9829(6) 0.049(3) Uani 1 1 d . . .
C24 C 0.5873(15) 0.8966(8) 1.0658(6) 0.070(4) Uani 1 1 d . . .
H24 H 0.5422 0.9027 1.1025 0.084 Uiso 1 1 calc R . .
C25 C 0.6978(10) 0.9002(6) 1.0894(4) 0.039(2) Uani 1 1 d . . .
H25 H 0.7324 0.9024 1.1434 0.047 Uiso 1 1 calc R . .
C26 C 0.7737(11) 0.9011(7) 1.0365(6) 0.051(3) Uani 1 1 d . . .
C27 C 0.8947(11) 0.9029(10) 1.0573(8) 0.074(4) Uani 1 1 d . . .
H27 H 0.9340 0.9089 1.1103 0.089 Uiso 1 1 calc R . .
C28 C 0.9619(10) 0.8963(8) 1.0025(9) 0.066(4) Uani 1 1 d . . .
H28 H 1.0448 0.8963 1.0184 0.079 Uiso 1 1 calc R . .
C29 C 0.9047(10) 0.8899(7) 0.9261(7) 0.052(3) Uani 1 1 d . . .
H29 H 0.9503 0.8873 0.8895 0.063 Uiso 1 1 calc R . .
C30 C 0.7229(9) 0.8919(6) 0.9536(5) 0.0359(19) Uani 1 1 d . . .
C31 C 0.5962(9) 0.8822(6) 0.9273(5) 0.037(2) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 O4 2.232(6) 2_756 ?
Tb1 O7 2.316(6) . ?
Tb1 O1W 2.359(6) . ?
Tb1 O1 2.366(6) 2_756 ?
Tb1 N5 2.503(7) . ?
Tb1 N2 2.546(7) . ?
Tb1 N3 2.587(7) . ?
Tb1 N4 2.594(7) . ?
S2 O3 1.429(7) . ?
S2 O2 1.444(7) . ?
S2 O1 1.465(6) . ?
S2 C1 1.753(8) . ?
O1 Tb1 2.366(6) 2_746 ?
O1W H1W1 0.85(4) . ?
O1W H1W2 0.85(4) . ?
O4 C2 1.301(9) . ?
O4 Tb1 2.232(5) 2_746 ?
O5 N1 1.224(12) . ?
O6 N1 1.215(11) . ?
O7 C7 1.260(10) . ?
O8 C7 1.237(11) . ?
N1 C3 1.468(11) . ?
N2 C8 1.309(12) . ?
N2 C19 1.359(12) . ?
N3 C17 1.318(12) . ?
N3 C18 1.352(12) . ?
N4 C20 1.345(11) . ?
N4 C31 1.352(11) . ?
N5 C29 1.331(13) . ?
N5 C30 1.345(12) . ?
C1 C6 1.374(12) . ?
C1 C2 1.420(11) . ?
C2 C3 1.415(11) . ?
C3 C4 1.381(11) . ?
C4 C5 1.386(12) . ?
C4 C7 1.500(11) . ?
C5 C6 1.374(12) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C8 C9 1.415(15) . ?
C8 H8 0.9300 . ?
C9 C10 1.345(19) . ?
C9 H9 0.9300 . ?
C10 C11 1.401(17) . ?
C10 H10 0.9300 . ?
C11 C19 1.392(13) . ?
C11 C12 1.429(19) . ?
C12 C13 1.30(2) . ?
C12 H12 0.9300 . ?
C13 C14 1.404(17) . ?
C13 H13 0.9300 . ?
C14 C15 1.347(19) . ?
C14 C18 1.449(13) . ?
C15 C16 1.372(19) . ?
C15 H15 0.9300 . ?
C16 C17 1.383(14) . ?
C16 H16 0.9300 . ?
C17 H17 0.9300 . ?
C18 C19 1.404(15) . ?
C20 C21 1.389(13) . ?
C20 H20 0.9300 . ?
C21 C22 1.349(15) . ?
C21 H21 0.9300 . ?
C22 C23 1.368(17) . ?
C22 H22 0.9300 . ?
C23 C31 1.424(13) . ?
C23 C24 1.462(16) . ?
C24 C25 1.243(18) . ?
C24 H24 0.9300 . ?
C25 C26 1.431(15) . ?
C25 H25 0.9300 . ?
C26 C27 1.357(17) . ?
C26 C30 1.429(13) . ?
C27 C28 1.39(2) . ?
C27 H27 0.9300 . ?
C28 C29 1.336(18) . ?
C28 H28 0.9300 . ?
C29 H29 0.9300 . ?
C30 C31 1.431(14) . ?

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 Tb1 O7 79.2(2) 2_756 . ?
O4 Tb1 O1W 146.8(2) 2_756 . ?
O7 Tb1 O1W 71.9(2) . . ?
O4 Tb1 O1 73.7(2) 2_756 2_756 ?
O7 Tb1 O1 146.6(2) . 2_756 ?
O1W Tb1 O1 138.8(2) . 2_756 ?
O4 Tb1 N5 84.7(2) 2_756 . ?
O7 Tb1 N5 73.8(2) . . ?
O1W Tb1 N5 102.1(2) . . ?
O1 Tb1 N5 84.3(2) 2_756 . ?
O4 Tb1 N2 79.3(2) 2_756 . ?
O7 Tb1 N2 79.2(2) . . ?
O1W Tb1 N2 79.7(3) . . ?
O1 Tb1 N2 113.9(2) 2_756 . ?
N5 Tb1 N2 150.7(3) . . ?
O4 Tb1 N3 112.9(2) 2_756 . ?
O7 Tb1 N3 136.5(2) . . ?
O1W Tb1 N3 79.5(2) . . ?
O1 Tb1 N3 73.7(2) 2_756 . ?
N5 Tb1 N3 145.6(2) . . ?
N2 Tb1 N3 63.6(2) . . ?
O4 Tb1 N4 136.3(2) 2_756 . ?
O7 Tb1 N4 116.2(2) . . ?
O1W Tb1 N4 73.1(2) . . ?
O1 Tb1 N4 73.7(2) 2_756 . ?
N5 Tb1 N4 63.8(2) . . ?
N2 Tb1 N4 141.4(2) . . ?
N3 Tb1 N4 84.6(2) . . ?
O3 S2 O2 113.8(4) . . ?
O3 S2 O1 111.4(4) . . ?
O2 S2 O1 111.7(4) . . ?
O3 S2 C1 106.2(4) . . ?
O2 S2 C1 105.7(4) . . ?
O1 S2 C1 107.4(4) . . ?
S2 O1 Tb1 132.3(3) . 2_746 ?
Tb1 O1W H1W1 112(7) . . ?
Tb1 O1W H1W2 131(7) . . ?
H1W1 O1W H1W2 109.6(18) . . ?
C2 O4 Tb1 143.7(5) . 2_746 ?
C7 O7 Tb1 143.5(6) . . ?
O6 N1 O5 124.2(10) . . ?
O6 N1 C3 116.9(9) . . ?
O5 N1 C3 118.6(8) . . ?
C8 N2 C19 119.3(8) . . ?
C8 N2 Tb1 121.0(7) . . ?
C19 N2 Tb1 119.6(6) . . ?
C17 N3 C18 118.3(8) . . ?
C17 N3 Tb1 124.0(6) . . ?
C18 N3 Tb1 117.4(6) . . ?
C20 N4 C31 116.6(8) . . ?
C20 N4 Tb1 125.6(6) . . ?
C31 N4 Tb1 117.5(6) . . ?
C29 N5 C30 116.8(8) . . ?
C29 N5 Tb1 122.1(7) . . ?
C30 N5 Tb1 120.7(6) . . ?
C6 C1 C2 120.6(7) . . ?
C6 C1 S2 118.9(6) . . ?
C2 C1 S2 120.2(6) . . ?
O4 C2 C1 124.7(7) . . ?
O4 C2 C3 120.6(7) . . ?
C1 C2 C3 114.6(7) . . ?
C4 C3 C2 124.9(7) . . ?
C4 C3 N1 121.6(7) . . ?
C2 C3 N1 113.5(7) . . ?
C3 C4 C5 117.5(7) . . ?
C3 C4 C7 123.3(8) . . ?
C5 C4 C7 119.0(7) . . ?
C6 C5 C4 119.9(8) . . ?
C6 C5 H5 120.1 . . ?
C4 C5 H5 120.1 . . ?
C5 C6 C1 122.4(8) . . ?
C5 C6 H6 118.8 . . ?
C1 C6 H6 118.8 . . ?
O8 C7 O7 124.5(8) . . ?
O8 C7 C4 119.6(8) . . ?
O7 C7 C4 115.7(8) . . ?
N2 C8 C9 121.8(11) . . ?
N2 C8 H8 119.1 . . ?
C9 C8 H8 119.1 . . ?
C10 C9 C8 119.5(12) . . ?
C10 C9 H9 120.3 . . ?
C8 C9 H9 120.3 . . ?
C9 C10 C11 119.6(10) . . ?
C9 C10 H10 120.2 . . ?
C11 C10 H10 120.2 . . ?
C19 C11 C10 117.9(11) . . ?
C19 C11 C12 119.7(12) . . ?
C10 C11 C12 122.3(11) . . ?
C13 C12 C11 119.4(11) . . ?
C13 C12 H12 120.3 . . ?
C11 C12 H12 120.3 . . ?
C12 C13 C14 125.0(12) . . ?
C12 C13 H13 117.5 . . ?
C14 C13 H13 117.5 . . ?
C15 C14 C13 126.2(12) . . ?
C15 C14 C18 117.3(10) . . ?
C13 C14 C18 116.4(12) . . ?
C14 C15 C16 121.1(10) . . ?
C14 C15 H15 119.5 . . ?
C16 C15 H15 119.5 . . ?
C15 C16 C17 118.4(11) . . ?
C15 C16 H16 120.8 . . ?
C17 C16 H16 120.8 . . ?
N3 C17 C16 123.5(11) . . ?
N3 C17 H17 118.2 . . ?
C16 C17 H17 118.2 . . ?
N3 C18 C19 119.3(8) . . ?
N3 C18 C14 121.1(10) . . ?
C19 C18 C14 119.3(9) . . ?
N2 C19 C11 121.8(10) . . ?
N2 C19 C18 118.1(8) . . ?
C11 C19 C18 120.0(9) . . ?
N4 C20 C21 124.1(9) . . ?
N4 C20 H20 118.0 . . ?
C21 C20 H20 118.0 . . ?
C22 C21 C20 118.2(10) . . ?
C22 C21 H21 120.9 . . ?
C20 C21 H21 120.9 . . ?
C21 C22 C23 121.0(9) . . ?
C21 C22 H22 119.5 . . ?
C23 C22 H22 119.5 . . ?
C22 C23 C31 117.9(9) . . ?
C22 C23 C24 125.0(11) . . ?
C31 C23 C24 117.2(11) . . ?
C25 C24 C23 122.8(11) . . ?
C25 C24 H24 118.6 . . ?
C23 C24 H24 118.6 . . ?
C24 C25 C26 122.5(9) . . ?
C24 C25 H25 118.8 . . ?
C26 C25 H25 118.8 . . ?
C27 C26 C30 113.9(11) . . ?
C27 C26 C25 126.2(11) . . ?
C30 C26 C25 119.7(10) . . ?
C26 C27 C28 122.6(11) . . ?
C26 C27 H27 118.7 . . ?
C28 C27 H27 118.7 . . ?
C29 C28 C27 118.3(10) . . ?
C29 C28 H28 120.8 . . ?
C27 C28 H28 120.8 . . ?
C28 C29 N5 124.0(11) . . ?
C28 C29 H29 118.0 . . ?
N5 C29 H29 118.0 . . ?
N5 C30 C26 124.3(9) . . ?
N5 C30 C31 118.1(7) . . ?
C26 C30 C31 117.5(9) . . ?
N4 C31 C23 122.0(9) . . ?
N4 C31 C30 117.7(8) . . ?
C23 C31 C30 120.2(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
O3 S2 O1 Tb1 -60.6(6) . . . 2_746 ?
O2 S2 O1 Tb1 170.9(5) . . . 2_746 ?
C1 S2 O1 Tb1 55.4(6) . . . 2_746 ?
O4 Tb1 O7 C7 -179.6(11) 2_756 . . . ?
O1W Tb1 O7 C7 -16.1(10) . . . . ?
O1 Tb1 O7 C7 144.0(9) 2_756 . . . ?
N5 Tb1 O7 C7 92.8(11) . . . . ?
N2 Tb1 O7 C7 -98.6(10) . . . . ?
N3 Tb1 O7 C7 -67.6(11) . . . . ?
N4 Tb1 O7 C7 43.8(11) . . . . ?
O4 Tb1 N2 C8 51.8(8) 2_756 . . . ?
O7 Tb1 N2 C8 -29.2(8) . . . . ?
O1W Tb1 N2 C8 -102.5(8) . . . . ?
O1 Tb1 N2 C8 118.5(8) 2_756 . . . ?
N5 Tb1 N2 C8 -6.3(11) . . . . ?
N3 Tb1 N2 C8 174.2(9) . . . . ?
N4 Tb1 N2 C8 -147.9(7) . . . . ?
O4 Tb1 N2 C19 -132.6(7) 2_756 . . . ?
O7 Tb1 N2 C19 146.4(7) . . . . ?
O1W Tb1 N2 C19 73.1(6) . . . . ?
O1 Tb1 N2 C19 -65.9(7) 2_756 . . . ?
N5 Tb1 N2 C19 169.4(6) . . . . ?
N3 Tb1 N2 C19 -10.2(6) . . . . ?
N4 Tb1 N2 C19 27.8(8) . . . . ?
O4 Tb1 N3 C17 -109.6(7) 2_756 . . . ?
O7 Tb1 N3 C17 151.7(7) . . . . ?
O1W Tb1 N3 C17 102.6(8) . . . . ?
O1 Tb1 N3 C17 -45.8(7) 2_756 . . . ?
N5 Tb1 N3 C17 6.6(10) . . . . ?
N2 Tb1 N3 C17 -173.8(8) . . . . ?
N4 Tb1 N3 C17 28.8(8) . . . . ?
O4 Tb1 N3 C18 76.4(6) 2_756 . . . ?
O7 Tb1 N3 C18 -22.3(8) . . . . ?
O1W Tb1 N3 C18 -71.4(6) . . . . ?
O1 Tb1 N3 C18 140.2(6) 2_756 . . . ?
N5 Tb1 N3 C18 -167.5(6) . . . . ?
N2 Tb1 N3 C18 12.1(6) . . . . ?
N4 Tb1 N3 C18 -145.2(6) . . . . ?
O4 Tb1 N4 C20 137.1(7) 2_756 . . . ?
O7 Tb1 N4 C20 -120.5(7) . . . . ?
O1W Tb1 N4 C20 -61.3(7) . . . . ?
O1 Tb1 N4 C20 93.8(7) 2_756 . . . ?
N5 Tb1 N4 C20 -174.5(8) . . . . ?
N2 Tb1 N4 C20 -14.3(9) . . . . ?
N3 Tb1 N4 C20 19.3(7) . . . . ?
O4 Tb1 N4 C31 -36.2(7) 2_756 . . . ?
O7 Tb1 N4 C31 66.1(6) . . . . ?
O1W Tb1 N4 C31 125.3(6) . . . . ?
O1 Tb1 N4 C31 -79.5(6) 2_756 . . . ?
N5 Tb1 N4 C31 12.1(6) . . . . ?
N2 Tb1 N4 C31 172.3(5) . . . . ?
N3 Tb1 N4 C31 -154.1(6) . . . . ?
O4 Tb1 N5 C29 -35.9(7) 2_756 . . . ?
O7 Tb1 N5 C29 44.4(7) . . . . ?
O1W Tb1 N5 C29 111.3(7) . . . . ?
O1 Tb1 N5 C29 -110.0(8) 2_756 . . . ?
N2 Tb1 N5 C29 21.0(10) . . . . ?
N3 Tb1 N5 C29 -159.8(7) . . . . ?
N4 Tb1 N5 C29 175.3(8) . . . . ?
O4 Tb1 N5 C30 136.4(6) 2_756 . . . ?
O7 Tb1 N5 C30 -143.3(7) . . . . ?
O1W Tb1 N5 C30 -76.5(6) . . . . ?
O1 Tb1 N5 C30 62.2(6) 2_756 . . . ?
N2 Tb1 N5 C30 -166.8(6) . . . . ?
N3 Tb1 N5 C30 12.5(9) . . . . ?
N4 Tb1 N5 C30 -12.4(6) . . . . ?
O3 S2 C1 C6 -89.5(8) . . . . ?
O2 S2 C1 C6 31.7(8) . . . . ?
O1 S2 C1 C6 151.2(7) . . . . ?
O3 S2 C1 C2 83.9(7) . . . . ?
O2 S2 C1 C2 -154.8(7) . . . . ?
O1 S2 C1 C2 -35.4(7) . . . . ?
Tb1 O4 C2 C1 11.0(14) 2_746 . . . ?
Tb1 O4 C2 C3 -168.8(6) 2_746 . . . ?
C6 C1 C2 O4 -179.0(8) . . . . ?
S2 C1 C2 O4 7.6(11) . . . . ?
C6 C1 C2 C3 0.8(11) . . . . ?
S2 C1 C2 C3 -172.5(6) . . . . ?
O4 C2 C3 C4 -178.0(7) . . . . ?
C1 C2 C3 C4 2.2(12) . . . . ?
O4 C2 C3 N1 -0.5(11) . . . . ?
C1 C2 C3 N1 179.6(7) . . . . ?
O6 N1 C3 C4 -87.3(11) . . . . ?
O5 N1 C3 C4 97.9(11) . . . . ?
O6 N1 C3 C2 95.1(10) . . . . ?
O5 N1 C3 C2 -79.7(10) . . . . ?
C2 C3 C4 C5 -4.6(12) . . . . ?
N1 C3 C4 C5 178.2(8) . . . . ?
C2 C3 C4 C7 169.4(7) . . . . ?
N1 C3 C4 C7 -7.8(12) . . . . ?
C3 C4 C5 C6 4.0(13) . . . . ?
C7 C4 C5 C6 -170.3(8) . . . . ?
C4 C5 C6 C1 -1.2(14) . . . . ?
C2 C1 C6 C5 -1.3(14) . . . . ?
S2 C1 C6 C5 172.1(7) . . . . ?
Tb1 O7 C7 O8 -8.8(17) . . . . ?
Tb1 O7 C7 C4 166.3(7) . . . . ?
C3 C4 C7 O8 -3.9(13) . . . . ?
C5 C4 C7 O8 170.0(8) . . . . ?
C3 C4 C7 O7 -179.3(8) . . . . ?
C5 C4 C7 O7 -5.3(12) . . . . ?
C19 N2 C8 C9 -0.9(16) . . . . ?
Tb1 N2 C8 C9 174.7(8) . . . . ?
N2 C8 C9 C10 -1.5(18) . . . . ?
C8 C9 C10 C11 3.6(18) . . . . ?
C9 C10 C11 C19 -3.4(16) . . . . ?
C9 C10 C11 C12 178.1(11) . . . . ?
C19 C11 C12 C13 3.4(18) . . . . ?
C10 C11 C12 C13 -178.0(12) . . . . ?
C11 C12 C13 C14 -2(2) . . . . ?
C12 C13 C14 C15 176.5(13) . . . . ?
C12 C13 C14 C18 -0.4(18) . . . . ?
C13 C14 C15 C16 -172.3(12) . . . . ?
C18 C14 C15 C16 4.6(17) . . . . ?
C14 C15 C16 C17 -2.6(18) . . . . ?
C18 N3 C17 C16 4.4(15) . . . . ?
Tb1 N3 C17 C16 -169.6(8) . . . . ?
C15 C16 C17 N3 -2.2(17) . . . . ?
C17 N3 C18 C19 171.8(9) . . . . ?
Tb1 N3 C18 C19 -13.9(10) . . . . ?
C17 N3 C18 C14 -2.1(13) . . . . ?
Tb1 N3 C18 C14 172.3(7) . . . . ?
C15 C14 C18 N3 -2.3(14) . . . . ?
C13 C14 C18 N3 174.9(9) . . . . ?
C15 C14 C18 C19 -176.2(10) . . . . ?
C13 C14 C18 C19 1.1(14) . . . . ?
C8 N2 C19 C11 1.2(14) . . . . ?
Tb1 N2 C19 C11 -174.5(7) . . . . ?
C8 N2 C19 C18 -176.5(9) . . . . ?
Tb1 N2 C19 C18 7.8(10) . . . . ?
C10 C11 C19 N2 1.0(14) . . . . ?
C12 C11 C19 N2 179.6(9) . . . . ?
C10 C11 C19 C18 178.6(9) . . . . ?
C12 C11 C19 C18 -2.8(14) . . . . ?
N3 C18 C19 N2 4.3(12) . . . . ?
C14 C18 C19 N2 178.3(8) . . . . ?
N3 C18 C19 C11 -173.4(8) . . . . ?
C14 C18 C19 C11 0.6(13) . . . . ?
C31 N4 C20 C21 4.8(14) . . . . ?
Tb1 N4 C20 C21 -168.6(8) . . . . ?
N4 C20 C21 C22 -3.3(17) . . . . ?
C20 C21 C22 C23 -0.4(17) . . . . ?
C21 C22 C23 C31 2.2(16) . . . . ?
C21 C22 C23 C24 -177.2(11) . . . . ?
C22 C23 C24 C25 173.8(12) . . . . ?
C31 C23 C24 C25 -5.7(17) . . . . ?
C23 C24 C25 C26 6.9(18) . . . . ?
C24 C25 C26 C27 -178.5(13) . . . . ?
C24 C25 C26 C30 -4.0(16) . . . . ?
C30 C26 C27 C28 -0.1(18) . . . . ?
C25 C26 C27 C28 174.6(12) . . . . ?
C26 C27 C28 C29 2(2) . . . . ?
C27 C28 C29 N5 -1.8(18) . . . . ?
C30 N5 C29 C28 0.5(15) . . . . ?
Tb1 N5 C29 C28 173.0(9) . . . . ?
C29 N5 C30 C26 1.2(13) . . . . ?
Tb1 N5 C30 C26 -171.4(7) . . . . ?
C29 N5 C30 C31 -175.3(8) . . . . ?
Tb1 N5 C30 C31 12.1(10) . . . . ?
C27 C26 C30 N5 -1.3(15) . . . . ?
C25 C26 C30 N5 -176.4(8) . . . . ?
C27 C26 C30 C31 175.2(10) . . . . ?
C25 C26 C30 C31 0.1(13) . . . . ?
C20 N4 C31 C23 -2.8(13) . . . . ?
Tb1 N4 C31 C23 171.2(7) . . . . ?
C20 N4 C31 C30 174.5(8) . . . . ?
Tb1 N4 C31 C30 -11.5(10) . . . . ?
C22 C23 C31 N4 -0.6(14) . . . . ?
C24 C23 C31 N4 178.9(9) . . . . ?
C22 C23 C31 C30 -177.8(9) . . . . ?
C24 C23 C31 C30 1.7(13) . . . . ?
N5 C30 C31 N4 0.2(12) . . . . ?
C26 C30 C31 N4 -176.6(8) . . . . ?
N5 C30 C31 C23 177.5(8) . . . . ?
C26 C30 C31 C23 0.8(12) . . . . ?

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
O1W H1W1 O8 0.85(4) 1.88(4) 2.680(9) 156(9) .
O1W H1W2 O2 0.85(4) 1.80(3) 2.622(9) 164(10) 1_455

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         2.850
_refine_diff_density_min         -1.789
_refine_diff_density_rms         0.158
####################################################################### 
# 
# 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_7-Ho
_database_code_depnum_ccdc_archive 'CCDC 1549873'
_audit_update_record             
;
2017-05-13 deposited with the CCDC.
2017-11-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C31 H20 Ho N5 O9 S'
_chemical_formula_sum            'C31 H20 Ho N5 O9 S'
_chemical_formula_weight         803.51

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'
Ho Ho -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   11.6315(2)
_cell_length_b                   14.8756(3)
_cell_length_c                   17.5103(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 104.705(2)
_cell_angle_gamma                90.00
_cell_volume                     2930.49(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    4239
_cell_measurement_theta_min      3.28
_cell_measurement_theta_max      27.56

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.821
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1584
_exptl_absorpt_coefficient_mu    2.838
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5871
_exptl_absorpt_correction_T_max  0.6595
_exptl_absorpt_process_details   
; 
CrysAlis Pro (Agilent, 2013)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1954
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10615
_diffrn_reflns_av_R_equivalents  0.0291
_diffrn_reflns_av_sigmaI/netI    0.0607
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         3.28
_diffrn_reflns_theta_max         27.56
_reflns_number_total             6712
_reflns_number_gt                5224
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_cell_refinement       
;
CrysAlis Pro (Agilent, 2013)
;
_computing_data_reduction        
;
CrysAlis Pro (Agilent, 2013)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    '(K. Brandenburg, Diamond 3.1, 2009)'
_computing_publication_material  '(K. Brandenburg, Diamond 3.1, 2009)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0161P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6712
_refine_ls_number_parameters     430
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0558
_refine_ls_R_factor_gt           0.0366
_refine_ls_wR_factor_ref         0.0647
_refine_ls_wR_factor_gt          0.0585
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_restrained_S_all      1.007
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ho1 Ho 0.312865(16) 0.391713(11) 0.745967(11) 0.02297(6) Uani 1 1 d . . .
S1 S 0.31162(9) 0.61179(7) 0.67218(6) 0.0284(2) Uani 1 1 d . . .
O1 O 0.3745(2) 0.53418(17) 0.71575(16) 0.0325(7) Uani 1 1 d . . .
O1W O 0.3932(3) 0.24722(18) 0.7714(2) 0.0417(8) Uani 1 1 d D . .
H1W1 H 0.345(3) 0.207(2) 0.749(3) 0.063 Uiso 1 1 d D . .
H1W2 H 0.4622(16) 0.226(2) 0.789(3) 0.063 Uiso 1 1 d D . .
O2 O 0.2590(3) 0.5904(2) 0.59078(17) 0.0479(8) Uani 1 1 d . . .
O3 O 0.3859(3) 0.69017(18) 0.6830(2) 0.0499(9) Uani 1 1 d . . .
O4 O 0.1676(2) 0.48548(17) 0.75362(16) 0.0337(7) Uani 1 1 d . . .
O5 O -0.0936(3) 0.4759(2) 0.7545(2) 0.0609(10) Uani 1 1 d . . .
O6 O -0.0024(3) 0.5163(3) 0.8728(2) 0.0719(12) Uani 1 1 d . . .
O7 O -0.1954(3) 0.65117(19) 0.79042(19) 0.0424(8) Uani 1 1 d . . .
O8 O -0.1566(2) 0.79330(17) 0.76673(17) 0.0371(7) Uani 1 1 d . . .
N1 N 0.2119(3) 0.3873(2) 0.6031(2) 0.0347(8) Uani 1 1 d . . .
N2 N 0.4504(3) 0.3672(2) 0.6521(2) 0.0312(8) Uani 1 1 d . . .
N3 N 0.5076(3) 0.4261(2) 0.8488(2) 0.0320(8) Uani 1 1 d . . .
N4 N 0.3075(3) 0.3723(2) 0.8879(2) 0.0347(9) Uani 1 1 d . . .
N5 N -0.0270(3) 0.5252(2) 0.8016(3) 0.0391(9) Uani 1 1 d . . .
C1 C 0.1930(3) 0.6372(2) 0.7150(2) 0.0230(8) Uani 1 1 d . . .
C2 C 0.1347(3) 0.5692(3) 0.7463(2) 0.0239(8) Uani 1 1 d . . .
C3 C 0.0331(3) 0.5982(3) 0.7695(2) 0.0249(9) Uani 1 1 d . . .
C4 C -0.0100(4) 0.6853(3) 0.7630(2) 0.0270(9) Uani 1 1 d . . .
C5 C 0.0551(4) 0.7501(3) 0.7348(3) 0.0356(10) Uani 1 1 d . . .
H5 H 0.0309 0.8099 0.7320 0.043 Uiso 1 1 calc R . .
C6 C 0.1555(4) 0.7262(3) 0.7111(3) 0.0341(10) Uani 1 1 d . . .
H6 H 0.1985 0.7700 0.6924 0.041 Uiso 1 1 calc R . .
C7 C -0.1297(4) 0.7106(3) 0.7761(2) 0.0298(9) Uani 1 1 d . . .
C8 C 0.0953(4) 0.3901(3) 0.5778(3) 0.0483(12) Uani 1 1 d . . .
H8 H 0.0511 0.3884 0.6152 0.058 Uiso 1 1 calc R . .
C9 C 0.0336(5) 0.3957(3) 0.4979(3) 0.0639(16) Uani 1 1 d . . .
H9 H -0.0491 0.3947 0.4823 0.077 Uiso 1 1 calc R . .
C10 C 0.0992(6) 0.4026(4) 0.4442(3) 0.0659(17) Uani 1 1 d . . .
H10 H 0.0607 0.4091 0.3910 0.079 Uiso 1 1 calc R . .
C11 C 0.2221(5) 0.4004(3) 0.4667(3) 0.0492(13) Uani 1 1 d . . .
C12 C 0.2941(6) 0.4045(4) 0.4124(3) 0.0653(17) Uani 1 1 d . . .
H12 H 0.2584 0.4130 0.3590 0.078 Uiso 1 1 calc R . .
C13 C 0.4133(6) 0.3964(4) 0.4367(3) 0.0644(16) Uani 1 1 d . . .
H13 H 0.4586 0.3990 0.4000 0.077 Uiso 1 1 calc R . .
C14 C 0.4707(5) 0.3838(3) 0.5183(3) 0.0457(12) Uani 1 1 d . . .
C15 C 0.5935(5) 0.3699(3) 0.5454(3) 0.0562(15) Uani 1 1 d . . .
H15 H 0.6419 0.3725 0.5105 0.067 Uiso 1 1 calc R . .
C16 C 0.6411(5) 0.3525(3) 0.6231(3) 0.0526(14) Uani 1 1 d . . .
H16 H 0.7222 0.3424 0.6424 0.063 Uiso 1 1 calc R . .
C17 C 0.5654(4) 0.3501(3) 0.6735(3) 0.0407(11) Uani 1 1 d . . .
H17 H 0.5986 0.3354 0.7261 0.049 Uiso 1 1 calc R . .
C18 C 0.4013(4) 0.3817(3) 0.5737(2) 0.0346(10) Uani 1 1 d . . .
C19 C 0.2753(4) 0.3913(3) 0.5480(2) 0.0368(10) Uani 1 1 d . . .
C20 C 0.6046(4) 0.4593(3) 0.8320(3) 0.0432(12) Uani 1 1 d . . .
H20 H 0.5982 0.4810 0.7813 0.052 Uiso 1 1 calc R . .
C21 C 0.7150(4) 0.4634(3) 0.8861(4) 0.0567(14) Uani 1 1 d . . .
H21 H 0.7809 0.4856 0.8712 0.068 Uiso 1 1 calc R . .
C22 C 0.7249(5) 0.4347(3) 0.9607(4) 0.0629(16) Uani 1 1 d . . .
H22 H 0.7988 0.4349 0.9970 0.075 Uiso 1 1 calc R . .
C23 C 0.6250(5) 0.4046(3) 0.9837(3) 0.0465(13) Uani 1 1 d . . .
C24 C 0.6255(6) 0.3825(3) 1.0633(3) 0.0669(18) Uani 1 1 d . . .
H24 H 0.6966 0.3844 1.1024 0.080 Uiso 1 1 calc R . .
C25 C 0.5254(7) 0.3594(3) 1.0823(3) 0.0658(18) Uani 1 1 d . . .
H25 H 0.5287 0.3460 1.1347 0.079 Uiso 1 1 calc R . .
C26 C 0.4143(5) 0.3544(3) 1.0256(3) 0.0475(13) Uani 1 1 d . . .
C27 C 0.3066(7) 0.3340(3) 1.0427(3) 0.0645(18) Uani 1 1 d . . .
H27 H 0.3054 0.3199 1.0942 0.077 Uiso 1 1 calc R . .
C28 C 0.2041(6) 0.3345(3) 0.9855(3) 0.0629(17) Uani 1 1 d . . .
H28 H 0.1321 0.3221 0.9973 0.075 Uiso 1 1 calc R . .
C29 C 0.2082(5) 0.3539(3) 0.9091(3) 0.0484(13) Uani 1 1 d . . .
H29 H 0.1370 0.3540 0.8700 0.058 Uiso 1 1 calc R . .
C30 C 0.4099(4) 0.3742(2) 0.9457(2) 0.0335(10) Uani 1 1 d . . .
C31 C 0.5171(4) 0.4005(3) 0.9247(2) 0.0348(10) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ho1 O4 2.221(3) . ?
Ho1 O8 2.300(3) 2_546 ?
Ho1 O1 2.340(3) . ?
Ho1 O1W 2.341(3) . ?
Ho1 N1 2.479(3) . ?
Ho1 N4 2.519(3) . ?
Ho1 N3 2.562(3) . ?
Ho1 N2 2.594(3) . ?
S1 O3 1.435(3) . ?
S1 O2 1.437(3) . ?
S1 O1 1.472(3) . ?
S1 C1 1.770(4) . ?
O1W H1W1 0.85(4) . ?
O1W H1W2 0.85(4) . ?
O4 C2 1.300(4) . ?
O5 N5 1.222(5) . ?
O6 N5 1.214(5) . ?
O7 C7 1.235(5) . ?
O8 C7 1.270(4) . ?
O8 Ho1 2.300(3) 2_556 ?
N1 C8 1.316(5) . ?
N1 C19 1.357(5) . ?
N2 C17 1.319(5) . ?
N2 C18 1.364(5) . ?
N3 C20 1.332(5) . ?
N3 C31 1.360(5) . ?
N4 C29 1.328(5) . ?
N4 C30 1.354(5) . ?
N5 C3 1.477(5) . ?
C1 C6 1.389(5) . ?
C1 C2 1.405(5) . ?
C2 C3 1.411(5) . ?
C3 C4 1.383(5) . ?
C4 C5 1.392(5) . ?
C4 C7 1.515(5) . ?
C5 C6 1.382(5) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C8 C9 1.405(6) . ?
C8 H8 0.9300 . ?
C9 C10 1.358(8) . ?
C9 H9 0.9300 . ?
C10 C11 1.383(8) . ?
C10 H10 0.9300 . ?
C11 C19 1.408(6) . ?
C11 C12 1.420(7) . ?
C12 C13 1.349(8) . ?
C12 H12 0.9300 . ?
C13 C14 1.427(7) . ?
C13 H13 0.9300 . ?
C14 C15 1.402(7) . ?
C14 C18 1.410(6) . ?
C15 C16 1.358(7) . ?
C15 H15 0.9300 . ?
C16 C17 1.395(6) . ?
C16 H16 0.9300 . ?
C17 H17 0.9300 . ?
C18 C19 1.426(6) . ?
C20 C21 1.390(6) . ?
C20 H20 0.9300 . ?
C21 C22 1.351(7) . ?
C21 H21 0.9300 . ?
C22 C23 1.397(7) . ?
C22 H22 0.9300 . ?
C23 C31 1.409(6) . ?
C23 C24 1.432(7) . ?
C24 C25 1.334(8) . ?
C24 H24 0.9300 . ?
C25 C26 1.418(8) . ?
C25 H25 0.9300 . ?
C26 C27 1.393(8) . ?
C26 C30 1.418(6) . ?
C27 C28 1.348(8) . ?
C27 H27 0.9300 . ?
C28 C29 1.382(6) . ?
C28 H28 0.9300 . ?
C29 H29 0.9300 . ?
C30 C31 1.441(6) . ?

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 Ho1 O8 79.11(9) . 2_546 ?
O4 Ho1 O1 74.11(9) . . ?
O8 Ho1 O1 146.54(10) 2_546 . ?
O4 Ho1 O1W 146.95(10) . . ?
O8 Ho1 O1W 72.62(10) 2_546 . ?
O1 Ho1 O1W 138.08(10) . . ?
O4 Ho1 N1 84.53(11) . . ?
O8 Ho1 N1 74.05(11) 2_546 . ?
O1 Ho1 N1 83.68(10) . . ?
O1W Ho1 N1 103.36(12) . . ?
O4 Ho1 N4 78.62(11) . . ?
O8 Ho1 N4 78.78(11) 2_546 . ?
O1 Ho1 N4 114.37(10) . . ?
O1W Ho1 N4 79.39(12) . . ?
N1 Ho1 N4 150.26(12) . . ?
O4 Ho1 N3 112.50(10) . . ?
O8 Ho1 N3 136.95(10) 2_546 . ?
O1 Ho1 N3 73.23(10) . . ?
O1W Ho1 N3 79.09(11) . . ?
N1 Ho1 N3 145.32(12) . . ?
N4 Ho1 N3 64.41(11) . . ?
O4 Ho1 N2 136.69(10) . . ?
O8 Ho1 N2 116.65(10) 2_546 . ?
O1 Ho1 N2 73.19(9) . . ?
O1W Ho1 N2 73.17(11) . . ?
N1 Ho1 N2 64.39(11) . . ?
N4 Ho1 N2 141.51(11) . . ?
N3 Ho1 N2 84.03(11) . . ?
O3 S1 O2 113.7(2) . . ?
O3 S1 O1 111.44(18) . . ?
O2 S1 O1 111.79(18) . . ?
O3 S1 C1 106.16(18) . . ?
O2 S1 C1 106.60(19) . . ?
O1 S1 C1 106.65(17) . . ?
S1 O1 Ho1 133.40(16) . . ?
Ho1 O1W H1W1 112(3) . . ?
Ho1 O1W H1W2 135(3) . . ?
H1W1 O1W H1W2 111.4(17) . . ?
C2 O4 Ho1 143.6(2) . . ?
C7 O8 Ho1 142.4(3) . 2_556 ?
C8 N1 C19 117.3(4) . . ?
C8 N1 Ho1 121.5(3) . . ?
C19 N1 Ho1 120.8(3) . . ?
C17 N2 C18 116.8(4) . . ?
C17 N2 Ho1 126.3(3) . . ?
C18 N2 Ho1 116.6(3) . . ?
C20 N3 C31 117.2(4) . . ?
C20 N3 Ho1 124.5(3) . . ?
C31 N3 Ho1 118.0(3) . . ?
C29 N4 C30 117.3(4) . . ?
C29 N4 Ho1 122.7(3) . . ?
C30 N4 Ho1 119.8(3) . . ?
O6 N5 O5 124.9(4) . . ?
O6 N5 C3 117.4(4) . . ?
O5 N5 C3 117.7(4) . . ?
C6 C1 C2 121.9(4) . . ?
C6 C1 S1 116.9(3) . . ?
C2 C1 S1 121.1(3) . . ?
O4 C2 C1 124.7(3) . . ?
O4 C2 C3 120.7(4) . . ?
C1 C2 C3 114.5(3) . . ?
C4 C3 C2 125.1(4) . . ?
C4 C3 N5 121.5(3) . . ?
C2 C3 N5 113.4(3) . . ?
C3 C4 C5 117.4(4) . . ?
C3 C4 C7 123.2(4) . . ?
C5 C4 C7 119.0(4) . . ?
C6 C5 C4 120.4(4) . . ?
C6 C5 H5 119.8 . . ?
C4 C5 H5 119.8 . . ?
C5 C6 C1 120.6(4) . . ?
C5 C6 H6 119.7 . . ?
C1 C6 H6 119.7 . . ?
O7 C7 O8 125.1(4) . . ?
O7 C7 C4 119.5(4) . . ?
O8 C7 C4 115.3(4) . . ?
N1 C8 C9 124.0(5) . . ?
N1 C8 H8 118.0 . . ?
C9 C8 H8 118.0 . . ?
C10 C9 C8 117.4(5) . . ?
C10 C9 H9 121.3 . . ?
C8 C9 H9 121.3 . . ?
C9 C10 C11 121.5(5) . . ?
C9 C10 H10 119.3 . . ?
C11 C10 H10 119.3 . . ?
C10 C11 C19 116.7(5) . . ?
C10 C11 C12 123.4(5) . . ?
C19 C11 C12 119.9(5) . . ?
C13 C12 C11 121.2(5) . . ?
C13 C12 H12 119.4 . . ?
C11 C12 H12 119.4 . . ?
C12 C13 C14 120.7(5) . . ?
C12 C13 H13 119.7 . . ?
C14 C13 H13 119.7 . . ?
C15 C14 C18 118.5(5) . . ?
C15 C14 C13 122.3(5) . . ?
C18 C14 C13 119.2(5) . . ?
C16 C15 C14 119.2(5) . . ?
C16 C15 H15 120.4 . . ?
C14 C15 H15 120.4 . . ?
C15 C16 C17 118.5(5) . . ?
C15 C16 H16 120.8 . . ?
C17 C16 H16 120.8 . . ?
N2 C17 C16 125.0(5) . . ?
N2 C17 H17 117.5 . . ?
C16 C17 H17 117.5 . . ?
N2 C18 C14 121.9(4) . . ?
N2 C18 C19 117.8(4) . . ?
C14 C18 C19 120.2(4) . . ?
N1 C19 C11 123.0(5) . . ?
N1 C19 C18 118.2(4) . . ?
C11 C19 C18 118.8(4) . . ?
N3 C20 C21 123.7(5) . . ?
N3 C20 H20 118.2 . . ?
C21 C20 H20 118.2 . . ?
C22 C21 C20 118.8(5) . . ?
C22 C21 H21 120.6 . . ?
C20 C21 H21 120.6 . . ?
C21 C22 C23 120.5(5) . . ?
C21 C22 H22 119.8 . . ?
C23 C22 H22 119.8 . . ?
C22 C23 C31 117.0(5) . . ?
C22 C23 C24 123.8(5) . . ?
C31 C23 C24 119.1(5) . . ?
C25 C24 C23 120.9(5) . . ?
C25 C24 H24 119.5 . . ?
C23 C24 H24 119.5 . . ?
C24 C25 C26 122.5(5) . . ?
C24 C25 H25 118.8 . . ?
C26 C25 H25 118.8 . . ?
C27 C26 C25 124.8(5) . . ?
C27 C26 C30 116.6(5) . . ?
C25 C26 C30 118.6(5) . . ?
C28 C27 C26 120.8(5) . . ?
C28 C27 H27 119.6 . . ?
C26 C27 H27 119.6 . . ?
C27 C28 C29 118.7(5) . . ?
C27 C28 H28 120.7 . . ?
C29 C28 H28 120.7 . . ?
N4 C29 C28 124.0(5) . . ?
N4 C29 H29 118.0 . . ?
C28 C29 H29 118.0 . . ?
N4 C30 C26 122.5(5) . . ?
N4 C30 C31 118.0(4) . . ?
C26 C30 C31 119.4(5) . . ?
N3 C31 C23 122.7(4) . . ?
N3 C31 C30 117.6(4) . . ?
C23 C31 C30 119.5(4) . . ?

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
O3 S1 O1 Ho1 168.8(2) . . . . ?
O2 S1 O1 Ho1 -62.8(3) . . . . ?
C1 S1 O1 Ho1 53.4(3) . . . . ?
O4 Ho1 O1 S1 -36.9(2) . . . . ?
O8 Ho1 O1 S1 1.2(3) 2_546 . . . ?
O1W Ho1 O1 S1 152.2(2) . . . . ?
N1 Ho1 O1 S1 49.2(2) . . . . ?
N4 Ho1 O1 S1 -106.2(2) . . . . ?
N3 Ho1 O1 S1 -157.0(2) . . . . ?
N2 Ho1 O1 S1 114.3(2) . . . . ?
O8 Ho1 O4 C2 -159.9(4) 2_546 . . . ?
O1 Ho1 O4 C2 -0.2(4) . . . . ?
O1W Ho1 O4 C2 168.7(4) . . . . ?
N1 Ho1 O4 C2 -85.2(4) . . . . ?
N4 Ho1 O4 C2 119.5(4) . . . . ?
N3 Ho1 O4 C2 63.5(4) . . . . ?
N2 Ho1 O4 C2 -42.4(5) . . . . ?
O4 Ho1 N1 C8 -36.2(4) . . . . ?
O8 Ho1 N1 C8 44.0(3) 2_546 . . . ?
O1 Ho1 N1 C8 -110.8(4) . . . . ?
O1W Ho1 N1 C8 111.2(4) . . . . ?
N4 Ho1 N1 C8 19.2(5) . . . . ?
N3 Ho1 N1 C8 -158.7(3) . . . . ?
N2 Ho1 N1 C8 174.9(4) . . . . ?
O4 Ho1 N1 C19 136.8(3) . . . . ?
O8 Ho1 N1 C19 -143.0(3) 2_546 . . . ?
O1 Ho1 N1 C19 62.3(3) . . . . ?
O1W Ho1 N1 C19 -75.8(3) . . . . ?
N4 Ho1 N1 C19 -167.7(3) . . . . ?
N3 Ho1 N1 C19 14.3(4) . . . . ?
N2 Ho1 N1 C19 -12.1(3) . . . . ?
O4 Ho1 N2 C17 137.1(3) . . . . ?
O8 Ho1 N2 C17 -119.9(3) 2_546 . . . ?
O1 Ho1 N2 C17 94.7(3) . . . . ?
O1W Ho1 N2 C17 -60.0(3) . . . . ?
N1 Ho1 N2 C17 -174.4(4) . . . . ?
N4 Ho1 N2 C17 -13.6(4) . . . . ?
N3 Ho1 N2 C17 20.4(3) . . . . ?
O4 Ho1 N2 C18 -36.2(3) . . . . ?
O8 Ho1 N2 C18 66.7(3) 2_546 . . . ?
O1 Ho1 N2 C18 -78.7(3) . . . . ?
O1W Ho1 N2 C18 126.7(3) . . . . ?
N1 Ho1 N2 C18 12.3(3) . . . . ?
N4 Ho1 N2 C18 173.1(2) . . . . ?
N3 Ho1 N2 C18 -152.9(3) . . . . ?
O4 Ho1 N3 C20 -110.3(3) . . . . ?
O8 Ho1 N3 C20 151.5(3) 2_546 . . . ?
O1 Ho1 N3 C20 -46.0(3) . . . . ?
O1W Ho1 N3 C20 102.2(3) . . . . ?
N1 Ho1 N3 C20 4.4(4) . . . . ?
N4 Ho1 N3 C20 -174.5(4) . . . . ?
N2 Ho1 N3 C20 28.2(3) . . . . ?
O4 Ho1 N3 C31 76.7(3) . . . . ?
O8 Ho1 N3 C31 -21.6(3) 2_546 . . . ?
O1 Ho1 N3 C31 140.9(3) . . . . ?
O1W Ho1 N3 C31 -70.9(3) . . . . ?
N1 Ho1 N3 C31 -168.7(3) . . . . ?
N4 Ho1 N3 C31 12.4(3) . . . . ?
N2 Ho1 N3 C31 -144.9(3) . . . . ?
O4 Ho1 N4 C29 51.9(3) . . . . ?
O8 Ho1 N4 C29 -29.1(3) 2_546 . . . ?
O1 Ho1 N4 C29 118.4(3) . . . . ?
O1W Ho1 N4 C29 -103.3(3) . . . . ?
N1 Ho1 N4 C29 -4.9(5) . . . . ?
N3 Ho1 N4 C29 173.8(4) . . . . ?
N2 Ho1 N4 C29 -148.1(3) . . . . ?
O4 Ho1 N4 C30 -132.9(3) . . . . ?
O8 Ho1 N4 C30 146.2(3) 2_546 . . . ?
O1 Ho1 N4 C30 -66.3(3) . . . . ?
O1W Ho1 N4 C30 72.0(3) . . . . ?
N1 Ho1 N4 C30 170.4(3) . . . . ?
N3 Ho1 N4 C30 -10.9(3) . . . . ?
N2 Ho1 N4 C30 27.1(4) . . . . ?
O3 S1 C1 C6 32.5(4) . . . . ?
O2 S1 C1 C6 -88.9(3) . . . . ?
O1 S1 C1 C6 151.5(3) . . . . ?
O3 S1 C1 C2 -151.7(3) . . . . ?
O2 S1 C1 C2 86.8(3) . . . . ?
O1 S1 C1 C2 -32.8(4) . . . . ?
Ho1 O4 C2 C1 10.0(7) . . . . ?
Ho1 O4 C2 C3 -170.8(3) . . . . ?
C6 C1 C2 O4 -177.8(4) . . . . ?
S1 C1 C2 O4 6.7(5) . . . . ?
C6 C1 C2 C3 2.9(6) . . . . ?
S1 C1 C2 C3 -172.6(3) . . . . ?
O4 C2 C3 C4 -179.1(4) . . . . ?
C1 C2 C3 C4 0.3(6) . . . . ?
O4 C2 C3 N5 0.2(5) . . . . ?
C1 C2 C3 N5 179.5(3) . . . . ?
O6 N5 C3 C4 -84.8(5) . . . . ?
O5 N5 C3 C4 98.4(5) . . . . ?
O6 N5 C3 C2 95.9(4) . . . . ?
O5 N5 C3 C2 -80.9(5) . . . . ?
C2 C3 C4 C5 -3.1(6) . . . . ?
N5 C3 C4 C5 177.6(4) . . . . ?
C2 C3 C4 C7 169.8(4) . . . . ?
N5 C3 C4 C7 -9.4(6) . . . . ?
C3 C4 C5 C6 2.9(6) . . . . ?
C7 C4 C5 C6 -170.3(4) . . . . ?
C4 C5 C6 C1 0.0(7) . . . . ?
C2 C1 C6 C5 -3.1(6) . . . . ?
S1 C1 C6 C5 172.6(3) . . . . ?
Ho1 O8 C7 O7 -8.2(7) 2_556 . . . ?
Ho1 O8 C7 C4 167.7(3) 2_556 . . . ?
C3 C4 C7 O7 -2.8(6) . . . . ?
C5 C4 C7 O7 170.0(4) . . . . ?
C3 C4 C7 O8 -179.0(4) . . . . ?
C5 C4 C7 O8 -6.2(6) . . . . ?
C19 N1 C8 C9 1.0(7) . . . . ?
Ho1 N1 C8 C9 174.2(3) . . . . ?
N1 C8 C9 C10 -3.1(8) . . . . ?
C8 C9 C10 C11 2.8(8) . . . . ?
C9 C10 C11 C19 -0.6(8) . . . . ?
C9 C10 C11 C12 177.9(5) . . . . ?
C10 C11 C12 C13 -175.8(6) . . . . ?
C19 C11 C12 C13 2.7(8) . . . . ?
C11 C12 C13 C14 -0.3(9) . . . . ?
C12 C13 C14 C15 176.2(5) . . . . ?
C12 C13 C14 C18 -1.3(8) . . . . ?
C18 C14 C15 C16 1.8(7) . . . . ?
C13 C14 C15 C16 -175.7(4) . . . . ?
C14 C15 C16 C17 -0.7(7) . . . . ?
C18 N2 C17 C16 5.0(6) . . . . ?
Ho1 N2 C17 C16 -168.3(3) . . . . ?
C15 C16 C17 N2 -2.9(7) . . . . ?
C17 N2 C18 C14 -3.6(6) . . . . ?
Ho1 N2 C18 C14 170.4(3) . . . . ?
C17 N2 C18 C19 173.8(4) . . . . ?
Ho1 N2 C18 C19 -12.2(5) . . . . ?
C15 C14 C18 N2 0.4(6) . . . . ?
C13 C14 C18 N2 178.0(4) . . . . ?
C15 C14 C18 C19 -177.0(4) . . . . ?
C13 C14 C18 C19 0.6(6) . . . . ?
C8 N1 C19 C11 1.5(6) . . . . ?
Ho1 N1 C19 C11 -171.8(3) . . . . ?
C8 N1 C19 C18 -175.5(4) . . . . ?
Ho1 N1 C19 C18 11.2(5) . . . . ?
C10 C11 C19 N1 -1.7(7) . . . . ?
C12 C11 C19 N1 179.7(4) . . . . ?
C10 C11 C19 C18 175.3(4) . . . . ?
C12 C11 C19 C18 -3.3(7) . . . . ?
N2 C18 C19 N1 1.3(6) . . . . ?
C14 C18 C19 N1 178.8(4) . . . . ?
N2 C18 C19 C11 -175.8(4) . . . . ?
C14 C18 C19 C11 1.7(6) . . . . ?
C31 N3 C20 C21 4.4(6) . . . . ?
Ho1 N3 C20 C21 -168.8(3) . . . . ?
N3 C20 C21 C22 -1.9(8) . . . . ?
C20 C21 C22 C23 -2.4(8) . . . . ?
C21 C22 C23 C31 4.0(7) . . . . ?
C21 C22 C23 C24 -172.8(5) . . . . ?
C22 C23 C24 C25 175.9(5) . . . . ?
C31 C23 C24 C25 -0.8(8) . . . . ?
C23 C24 C25 C26 0.6(9) . . . . ?
C24 C25 C26 C27 -177.4(5) . . . . ?
C24 C25 C26 C30 0.4(8) . . . . ?
C25 C26 C27 C28 177.1(5) . . . . ?
C30 C26 C27 C28 -0.7(7) . . . . ?
C26 C27 C28 C29 1.3(8) . . . . ?
C30 N4 C29 C28 -1.7(7) . . . . ?
Ho1 N4 C29 C28 173.7(3) . . . . ?
C27 C28 C29 N4 -0.1(8) . . . . ?
C29 N4 C30 C26 2.3(6) . . . . ?
Ho1 N4 C30 C26 -173.2(3) . . . . ?
C29 N4 C30 C31 -175.6(4) . . . . ?
Ho1 N4 C30 C31 8.9(5) . . . . ?
C27 C26 C30 N4 -1.1(6) . . . . ?
C25 C26 C30 N4 -179.1(4) . . . . ?
C27 C26 C30 C31 176.7(4) . . . . ?
C25 C26 C30 C31 -1.2(6) . . . . ?
C20 N3 C31 C23 -2.6(6) . . . . ?
Ho1 N3 C31 C23 171.0(3) . . . . ?
C20 N3 C31 C30 173.0(4) . . . . ?
Ho1 N3 C31 C30 -13.4(5) . . . . ?
C22 C23 C31 N3 -1.4(6) . . . . ?
C24 C23 C31 N3 175.5(4) . . . . ?
C22 C23 C31 C30 -176.9(4) . . . . ?
C24 C23 C31 C30 0.0(6) . . . . ?
N4 C30 C31 N3 3.3(5) . . . . ?
C26 C30 C31 N3 -174.7(3) . . . . ?
N4 C30 C31 C23 179.0(4) . . . . ?
C26 C30 C31 C23 1.0(6) . . . . ?

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
O1W H1W1 O7 0.85(4) 1.896(17) 2.690(4) 157(4) 2_546
O1W H1W2 O3 0.85(4) 1.791(12) 2.631(4) 172(5) 2_646

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        27.56
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         0.743
_refine_diff_density_min         -0.655
_refine_diff_density_rms         0.115
