# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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
_database_code_depnum_ccdc_archive 'CCDC 1410374'
_audit_update_record             
;
2016-04-21 deposited with the CCDC.
2016-06-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C19 H13 N2 O8 S Tb'
_chemical_formula_weight         588.29

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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                   10.5503(6)
_cell_length_b                   8.9330(5)
_cell_length_c                   20.1876(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.672(2)
_cell_angle_gamma                90.00
_cell_volume                     1902.47(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    956
_cell_measurement_theta_min      1.93
_cell_measurement_theta_max      25.10

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.054
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1144
_exptl_absorpt_coefficient_mu    3.881
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.4823
_exptl_absorpt_correction_T_max  0.5108
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'phi and omega scans'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            25838
_diffrn_reflns_av_R_equivalents  0.0747
_diffrn_reflns_av_sigmaI/netI    0.0320
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.93
_diffrn_reflns_theta_max         25.10
_reflns_number_total             3400
_reflns_number_gt                2766
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0373P)²+9.9953P] 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         3400
_refine_ls_number_parameters     280
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_gt           0.0349
_refine_ls_wR_factor_ref         0.0848
_refine_ls_wR_factor_gt          0.0785
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_restrained_S_all      1.058
_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
Tb1 Tb 0.16872(2) 0.74977(3) 0.202603(11) 0.01824(11) Uani 1 1 d . . .
N1 N 0.1481(4) 0.7817(5) 0.0775(2) 0.0195(10) Uani 1 1 d . . .
O1 O 0.3474(3) 0.6342(4) 0.15716(18) 0.0248(8) Uani 1 1 d . . .
C1 C 0.1222(5) 0.6697(7) 0.0359(3) 0.0266(13) Uani 1 1 d . . .
H1A H 0.1098 0.5746 0.0534 0.032 Uiso 1 1 calc R . .
S1 S 0.48416(13) 0.65456(16) 0.14469(7) 0.0253(3) Uani 1 1 d . . .
N2 N 0.2171(4) 1.0096(5) 0.1609(2) 0.0229(10) Uani 1 1 d . . .
O2 O 0.5420(4) 0.5198(5) 0.1217(2) 0.0450(12) Uani 1 1 d . . .
C2 C 0.1128(6) 0.6880(8) -0.0328(3) 0.0321(14) Uani 1 1 d . . .
H2A H 0.0960 0.6063 -0.0601 0.038 Uiso 1 1 calc R . .
C3 C 0.1284(6) 0.8266(7) -0.0591(3) 0.0309(14) Uani 1 1 d . . .
H3A H 0.1211 0.8407 -0.1047 0.037 Uiso 1 1 calc R . .
O3 O 0.5469(4) 0.7223(6) 0.2010(2) 0.0466(13) Uani 1 1 d . . .
C4 C 0.1556(5) 0.9489(7) -0.0173(3) 0.0241(12) Uani 1 1 d . . .
O4 O 0.3470(4) 0.8125(5) 0.2745(2) 0.0350(10) Uani 1 1 d . . .
H40B H 0.4203 0.7571 0.2611 0.053 Uiso 1 1 d R . .
H40C H 0.3640 0.9178 0.2712 0.053 Uiso 1 1 d R . .
C5 C 0.1743(5) 1.0975(7) -0.0418(3) 0.0317(15) Uani 1 1 d . . .
H5A H 0.1644 1.1166 -0.0868 0.038 Uiso 1 1 calc R . .
O5 O 0.0328(4) 0.3633(5) 0.31372(19) 0.0311(10) Uani 1 1 d . . .
C6 C 0.2059(6) 1.2092(7) -0.0007(3) 0.0333(15) Uani 1 1 d . . .
H6A H 0.2177 1.3049 -0.0177 0.040 Uiso 1 1 calc R . .
O6 O -0.0982(4) 0.3797(5) 0.20152(18) 0.0303(9) Uani 1 1 d . . .
C7 C 0.2218(5) 1.1844(7) 0.0687(3) 0.0262(12) Uani 1 1 d . . .
O7 O 0.0342(4) 0.5548(4) 0.16480(18) 0.0296(9) Uani 1 1 d . . .
C8 C 0.2607(6) 1.2972(7) 0.1127(3) 0.0318(14) Uani 1 1 d . . .
H8A H 0.2759 1.3935 0.0971 0.038 Uiso 1 1 calc R . .
O8 O 0.1543(4) 0.5540(4) 0.28090(18) 0.0280(9) Uani 1 1 d . . .
C9 C 0.2762(6) 1.2653(6) 0.1784(3) 0.0303(14) Uani 1 1 d . . .
H9A H 0.3022 1.3392 0.2081 0.036 Uiso 1 1 calc R . .
C10 C 0.2526(5) 1.1217(7) 0.2001(3) 0.0283(13) Uani 1 1 d . . .
H10A H 0.2622 1.1021 0.2451 0.034 Uiso 1 1 calc R . .
C11 C 0.2020(5) 1.0411(6) 0.0945(3) 0.0209(11) Uani 1 1 d . . .
C12 C 0.1667(5) 0.9197(6) 0.0512(2) 0.0197(12) Uani 1 1 d . . .
C13 C 0.4567(7) 0.8206(9) -0.0405(4) 0.0530(19) Uani 1 1 d . . .
H13 H 0.4365 0.7830 -0.0823 0.064 Uiso 1 1 calc R . .
C14 C 0.4597(7) 0.7314(10) 0.0138(4) 0.055(2) Uani 1 1 d . . .
H14A H 0.4413 0.6302 0.0086 0.066 Uiso 1 1 calc R . .
C15 C 0.4905(6) 0.7868(7) 0.0799(3) 0.0368(16) Uani 1 1 d . . .
C16 C 0.5170(6) 0.9311(9) 0.0878(4) 0.052(2) Uani 1 1 d D . .
H16 H 0.5368 0.9679 0.1298 0.062 Uiso 1 1 calc R . .
C17 C 0.5154(5) 1.0322(7) 0.0310(3) 0.0371(15) Uani 1 1 d D . .
C18 C -0.0056(5) 0.4646(6) 0.2070(3) 0.0221(12) Uani 1 1 d . . .
C19 C 0.0677(5) 0.4596(6) 0.2734(3) 0.0215(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
Tb1 O1 2.345(4) . ?
Tb1 O8 2.363(4) . ?
Tb1 O7 2.367(4) . ?
Tb1 O5 2.376(4) 2 ?
Tb1 O6 2.383(4) 2 ?
Tb1 O4 2.428(4) . ?
Tb1 N2 2.523(4) . ?
Tb1 N1 2.549(4) . ?
N1 C1 1.332(7) . ?
N1 C12 1.357(7) . ?
O1 S1 1.479(4) . ?
C1 C2 1.399(8) . ?
S1 O2 1.429(4) . ?
S1 O3 1.442(5) . ?
S1 C15 1.764(6) . ?
N2 C10 1.328(7) . ?
N2 C11 1.378(7) . ?
C2 C3 1.358(9) . ?
C3 C4 1.409(8) . ?
C4 C12 1.411(7) . ?
C4 C5 1.431(8) . ?
C5 C6 1.336(9) . ?
O5 C19 1.243(6) . ?
O5 Tb1 2.376(4) 2_545 ?
C6 C7 1.427(8) . ?
O6 C18 1.241(6) . ?
O6 Tb1 2.383(4) 2_545 ?
C7 C11 1.398(8) . ?
C7 C8 1.402(9) . ?
O7 C18 1.249(6) . ?
C8 C9 1.366(9) . ?
O8 C19 1.251(6) . ?
C9 C10 1.379(8) . ?
C11 C12 1.439(8) . ?
C13 C14 1.356(11) . ?
C13 C17 1.360(10) 3_675 ?
C14 C15 1.456(11) . ?
C15 C16 1.329(10) . ?
C16 C17 1.460(7) . ?
C17 C13 1.360(10) 3_675 ?
C17 C17 1.412(12) 3_675 ?
C18 C19 1.541(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
O1 Tb1 O8 89.67(13) . . ?
O1 Tb1 O7 91.81(13) . . ?
O8 Tb1 O7 68.18(13) . . ?
O1 Tb1 O5 148.86(13) . 2 ?
O8 Tb1 O5 110.14(14) . 2 ?
O7 Tb1 O5 74.76(14) . 2 ?
O1 Tb1 O6 142.36(13) . 2 ?
O8 Tb1 O6 78.11(13) . 2 ?
O7 Tb1 O6 115.37(14) . 2 ?
O5 Tb1 O6 67.51(13) 2 2 ?
O1 Tb1 O4 73.45(13) . . ?
O8 Tb1 O4 79.99(14) . . ?
O7 Tb1 O4 145.06(15) . . ?
O5 Tb1 O4 132.09(14) 2 . ?
O6 Tb1 O4 69.43(14) 2 . ?
O1 Tb1 N2 96.20(14) . . ?
O8 Tb1 N2 156.73(14) . . ?
O7 Tb1 N2 133.79(13) . . ?
O5 Tb1 N2 75.22(15) 2 . ?
O6 Tb1 N2 83.63(14) 2 . ?
O4 Tb1 N2 80.16(15) . . ?
O1 Tb1 N1 73.81(13) . . ?
O8 Tb1 N1 137.75(13) . . ?
O7 Tb1 N1 73.68(13) . . ?
O5 Tb1 N1 75.45(14) 2 . ?
O6 Tb1 N1 136.60(13) 2 . ?
O4 Tb1 N1 128.56(14) . . ?
N2 Tb1 N1 65.27(14) . . ?
C1 N1 C12 117.8(5) . . ?
C1 N1 Tb1 123.7(4) . . ?
C12 N1 Tb1 118.5(3) . . ?
S1 O1 Tb1 143.4(2) . . ?
N1 C1 C2 123.2(6) . . ?
O2 S1 O3 114.6(3) . . ?
O2 S1 O1 111.9(3) . . ?
O3 S1 O1 110.9(2) . . ?
O2 S1 C15 107.6(3) . . ?
O3 S1 C15 106.4(3) . . ?
O1 S1 C15 104.7(3) . . ?
C10 N2 C11 117.0(5) . . ?
C10 N2 Tb1 123.5(4) . . ?
C11 N2 Tb1 119.4(3) . . ?
C3 C2 C1 119.2(6) . . ?
C2 C3 C4 119.8(5) . . ?
C3 C4 C12 117.3(5) . . ?
C3 C4 C5 122.7(5) . . ?
C12 C4 C5 120.0(5) . . ?
C6 C5 C4 120.9(5) . . ?
C19 O5 Tb1 118.4(3) . 2_545 ?
C5 C6 C7 121.2(6) . . ?
C18 O6 Tb1 118.6(3) . 2_545 ?
C11 C7 C8 117.8(5) . . ?
C11 C7 C6 119.4(5) . . ?
C8 C7 C6 122.7(6) . . ?
C18 O7 Tb1 117.4(3) . . ?
C9 C8 C7 119.8(6) . . ?
C19 O8 Tb1 118.1(3) . . ?
C8 C9 C10 118.8(6) . . ?
N2 C10 C9 124.3(5) . . ?
N2 C11 C7 122.2(5) . . ?
N2 C11 C12 117.6(5) . . ?
C7 C11 C12 120.2(5) . . ?
N1 C12 C4 122.7(5) . . ?
N1 C12 C11 119.0(5) . . ?
C4 C12 C11 118.3(5) . . ?
C14 C13 C17 116.8(8) . 3_675 ?
C13 C14 C15 123.0(8) . . ?
C16 C15 C14 119.0(6) . . ?
C16 C15 S1 124.8(6) . . ?
C14 C15 S1 116.2(5) . . ?
C15 C16 C17 120.3(8) . . ?
C13 C17 C17 124.5(8) 3_675 3_675 ?
C13 C17 C16 119.1(7) 3_675 . ?
C17 C17 C16 116.4(8) 3_675 . ?
O6 C18 O7 127.2(5) . . ?
O6 C18 C19 116.5(5) . . ?
O7 C18 C19 116.2(5) . . ?
O5 C19 O8 127.5(5) . . ?
O5 C19 C18 116.1(5) . . ?
O8 C19 C18 116.4(5) . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.10
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         1.879
_refine_diff_density_min         -0.740
_refine_diff_density_rms         0.149
####################################################################### 
# 
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 1410375'
_audit_update_record             
;
2016-04-21 deposited with the CCDC.
2016-06-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C19 H15 N2 O9 S Sm'
_chemical_formula_weight         597.74

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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           triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.8357(8)
_cell_length_b                   10.6784(9)
_cell_length_c                   10.9831(9)
_cell_angle_alpha                80.877(2)
_cell_angle_beta                 69.329(2)
_cell_angle_gamma                88.555(2)
_cell_volume                     956.76(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3652
_cell_measurement_theta_min      3.00
_cell_measurement_theta_max      27.60

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.075
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             586
_exptl_absorpt_coefficient_mu    3.238
_exptl_absorpt_correction_type   Multi-SCAN
_exptl_absorpt_correction_T_min  0.5360
_exptl_absorpt_correction_T_max  0.5636
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku Saturn724 CCD'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19874
_diffrn_reflns_av_R_equivalents  0.1225
_diffrn_reflns_av_sigmaI/netI    0.0599
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.00
_diffrn_reflns_theta_max         27.60
_reflns_number_total             4431
_reflns_number_gt                4346
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0381P)²+1.5445P] 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         4431
_refine_ls_number_parameters     289
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0313
_refine_ls_R_factor_gt           0.0306
_refine_ls_wR_factor_ref         0.0800
_refine_ls_wR_factor_gt          0.0795
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      1.028
_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
Sm1 Sm 0.164383(15) 0.074474(12) 0.193666(12) 0.01321(7) Uani 1 1 d . . .
S1 S -0.08781(8) -0.18529(7) 0.47768(6) 0.01348(14) Uani 1 1 d . . .
O1 O 0.0204(3) -0.0793(2) 0.3968(2) 0.0188(4) Uani 1 1 d . . .
N1 N -0.1113(3) 0.1881(3) 0.2605(3) 0.0201(5) Uani 1 1 d . . .
C1 C 0.1802(4) -0.3112(3) 0.3596(3) 0.0210(6) Uani 1 1 d . . .
H1 H 0.2245 -0.2311 0.3170 0.025 Uiso 1 1 calc R . .
O2 O -0.2306(3) -0.1981(2) 0.4447(2) 0.0230(5) Uani 1 1 d . . .
N2 N 0.1671(3) 0.3248(3) 0.1140(3) 0.0200(5) Uani 1 1 d . . .
C2 C 0.0246(4) -0.3239(3) 0.4486(3) 0.0155(5) Uani 1 1 d . . .
O3 O -0.1302(3) -0.1818(2) 0.6183(2) 0.0208(5) Uani 1 1 d . . .
C3 C -0.0474(4) -0.4454(3) 0.5153(3) 0.0151(5) Uani 1 1 d . . .
C4 C -0.2084(4) -0.4625(3) 0.6083(3) 0.0198(6) Uani 1 1 d . . .
H4A H -0.2703 -0.3920 0.6291 0.024 Uiso 1 1 calc R . .
O4 O -0.1445(3) -0.1189(2) 0.0249(2) 0.0230(5) Uani 1 1 d . . .
O5 O -0.0283(3) -0.0664(2) 0.1615(2) 0.0217(5) Uani 1 1 d . . .
C5 C -0.2727(4) -0.5804(3) 0.6671(3) 0.0235(7) Uani 1 1 d . . .
H5 H -0.3791 -0.5897 0.7257 0.028 Uiso 1 1 calc R . .
O6 O 0.5632(3) -0.1432(2) -0.0548(2) 0.0267(5) Uani 1 1 d . . .
C6 C -0.0497(4) -0.0537(3) 0.0542(3) 0.0165(6) Uani 1 1 d . . .
O7 O 0.3222(3) -0.0923(2) 0.0800(2) 0.0233(5) Uani 1 1 d . . .
C7 C 0.4662(4) -0.0684(3) 0.0078(3) 0.0177(6) Uani 1 1 d . . .
C8 C -0.2483(4) 0.1216(4) 0.3299(4) 0.0277(7) Uani 1 1 d . . .
H8A H -0.2482 0.0338 0.3346 0.033 Uiso 1 1 calc R . .
O8 O 0.3527(3) -0.0107(3) 0.3141(3) 0.0320(6) Uani 1 1 d . . .
H80B H 0.4626 0.0110 0.2579 0.048 Uiso 1 1 d R . .
H80C H 0.3283 0.0259 0.3930 0.048 Uiso 1 1 d R . .
C9 C -0.3928(4) 0.1779(4) 0.3963(4) 0.0332(8) Uani 1 1 d . . .
H9A H -0.4859 0.1280 0.4443 0.040 Uiso 1 1 calc R . .
O9 O 0.4064(3) 0.1784(3) 0.7346(3) 0.0341(6) Uani 1 1 d . . .
H90D H 0.3964 0.2305 0.6583 0.051 Uiso 1 1 d R . .
H90C H 0.3034 0.1700 0.8052 0.051 Uiso 1 1 d R . .
C10 C -0.3953(4) 0.3061(4) 0.3897(4) 0.0314(8) Uani 1 1 d . . .
H10A H -0.4898 0.3446 0.4347 0.038 Uiso 1 1 calc R . .
C11 C -0.2544(4) 0.3804(3) 0.3145(3) 0.0243(7) Uani 1 1 d . . .
C12 C -0.2509(5) 0.5164(4) 0.2970(4) 0.0308(8) Uani 1 1 d . . .
H12A H -0.3426 0.5581 0.3413 0.037 Uiso 1 1 calc R . .
C13 C -0.1168(5) 0.5841(4) 0.2176(4) 0.0297(8) Uani 1 1 d . . .
H13A H -0.1175 0.6722 0.2064 0.036 Uiso 1 1 calc R . .
C14 C 0.0273(4) 0.5226(3) 0.1500(3) 0.0245(7) Uani 1 1 d . . .
C15 C 0.1668(5) 0.5909(3) 0.0626(4) 0.0310(8) Uani 1 1 d . . .
H15A H 0.1692 0.6792 0.0477 0.037 Uiso 1 1 calc R . .
C16 C 0.2988(5) 0.5267(4) -0.0001(4) 0.0309(8) Uani 1 1 d . . .
H16A H 0.3907 0.5703 -0.0617 0.037 Uiso 1 1 calc R . .
C17 C 0.2946(4) 0.3932(4) 0.0295(3) 0.0278(7) Uani 1 1 d . . .
H17A H 0.3867 0.3508 -0.0128 0.033 Uiso 1 1 calc R . .
C18 C 0.0319(4) 0.3892(3) 0.1703(3) 0.0186(6) Uani 1 1 d . . .
C19 C -0.1144(4) 0.3160(3) 0.2516(3) 0.0186(6) 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 O6 2.408(2) 2_655 ?
Sm1 O4 2.439(2) 2 ?
Sm1 O3 2.442(2) 2_556 ?
Sm1 O5 2.451(2) . ?
Sm1 O7 2.455(2) . ?
Sm1 O1 2.497(2) . ?
Sm1 O8 2.538(3) . ?
Sm1 N1 2.610(3) . ?
Sm1 N2 2.676(3) . ?
S1 O2 1.446(2) . ?
S1 O1 1.456(2) . ?
S1 O3 1.462(2) . ?
S1 C2 1.769(3) . ?
N1 C8 1.331(4) . ?
N1 C19 1.354(4) . ?
C1 C2 1.372(4) . ?
C1 C5 1.409(5) 2_546 ?
C1 H1 0.9300 . ?
N2 C17 1.324(4) . ?
N2 C18 1.361(4) . ?
C2 C3 1.427(4) . ?
O3 Sm1 2.442(2) 2_556 ?
C3 C4 1.424(4) . ?
C3 C3 1.432(6) 2_546 ?
C4 C5 1.358(5) . ?
C4 H4A 0.9300 . ?
O4 C6 1.257(4) . ?
O4 Sm1 2.439(2) 2 ?
O5 C6 1.245(4) . ?
C5 C1 1.409(5) 2_546 ?
C5 H5 0.9300 . ?
O6 C7 1.253(4) . ?
O6 Sm1 2.408(2) 2_655 ?
C6 C6 1.544(6) 2 ?
O7 C7 1.246(4) . ?
C7 C7 1.553(6) 2_655 ?
C8 C9 1.402(5) . ?
C8 H8A 0.9300 . ?
O8 H80B 0.9600 . ?
O8 H80C 0.9600 . ?
C9 C10 1.360(6) . ?
C9 H9A 0.9300 . ?
O9 H90D 0.9600 . ?
O9 H90C 0.9599 . ?
C10 C11 1.406(5) . ?
C10 H10A 0.9300 . ?
C11 C19 1.408(4) . ?
C11 C12 1.434(5) . ?
C12 C13 1.342(6) . ?
C12 H12A 0.9300 . ?
C13 C14 1.431(5) . ?
C13 H13A 0.9300 . ?
C14 C15 1.400(5) . ?
C14 C18 1.409(5) . ?
C15 C16 1.359(6) . ?
C15 H15A 0.9300 . ?
C16 C17 1.409(5) . ?
C16 H16A 0.9300 . ?
C17 H17A 0.9300 . ?
C18 C19 1.447(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O6 Sm1 O4 77.49(9) 2_655 2 ?
O6 Sm1 O3 100.68(9) 2_655 2_556 ?
O4 Sm1 O3 139.40(8) 2 2_556 ?
O6 Sm1 O5 130.67(8) 2_655 . ?
O4 Sm1 O5 66.01(7) 2 . ?
O3 Sm1 O5 128.64(8) 2_556 . ?
O6 Sm1 O7 66.63(8) 2_655 . ?
O4 Sm1 O7 76.36(9) 2 . ?
O3 Sm1 O7 140.83(8) 2_556 . ?
O5 Sm1 O7 73.15(8) . . ?
O6 Sm1 O1 139.25(8) 2_655 . ?
O4 Sm1 O1 133.43(8) 2 . ?
O3 Sm1 O1 72.94(7) 2_556 . ?
O5 Sm1 O1 67.48(7) . . ?
O7 Sm1 O1 92.63(7) . . ?
O6 Sm1 O8 71.92(9) 2_655 . ?
O4 Sm1 O8 142.64(8) 2 . ?
O3 Sm1 O8 68.66(9) 2_556 . ?
O5 Sm1 O8 121.18(9) . . ?
O7 Sm1 O8 72.17(9) . . ?
O1 Sm1 O8 68.32(8) . . ?
O6 Sm1 N1 133.60(8) 2_655 . ?
O4 Sm1 N1 82.60(9) 2 . ?
O3 Sm1 N1 69.45(9) 2_556 . ?
O5 Sm1 N1 74.38(9) . . ?
O7 Sm1 N1 146.34(9) . . ?
O1 Sm1 N1 83.00(8) . . ?
O8 Sm1 N1 134.42(9) . . ?
O6 Sm1 N2 71.80(8) 2_655 . ?
O4 Sm1 N2 69.35(8) 2 . ?
O3 Sm1 N2 71.64(8) 2_556 . ?
O5 Sm1 N2 120.08(8) . . ?
O7 Sm1 N2 130.50(8) . . ?
O1 Sm1 N2 136.86(8) . . ?
O8 Sm1 N2 118.64(9) . . ?
N1 Sm1 N2 61.99(9) . . ?
O2 S1 O1 113.89(13) . . ?
O2 S1 O3 111.31(14) . . ?
O1 S1 O3 111.69(13) . . ?
O2 S1 C2 107.84(15) . . ?
O1 S1 C2 106.15(14) . . ?
O3 S1 C2 105.38(13) . . ?
S1 O1 Sm1 157.08(14) . . ?
C8 N1 C19 117.8(3) . . ?
C8 N1 Sm1 120.2(2) . . ?
C19 N1 Sm1 120.3(2) . . ?
C2 C1 C5 119.9(3) . 2_546 ?
C2 C1 H1 120.0 . . ?
C5 C1 H1 120.0 2_546 . ?
C17 N2 C18 116.8(3) . . ?
C17 N2 Sm1 124.7(2) . . ?
C18 N2 Sm1 118.3(2) . . ?
C1 C2 C3 121.4(3) . . ?
C1 C2 S1 118.4(2) . . ?
C3 C2 S1 120.2(2) . . ?
S1 O3 Sm1 153.34(14) . 2_556 ?
C4 C3 C2 123.1(3) . . ?
C4 C3 C3 119.1(3) . 2_546 ?
C2 C3 C3 117.8(3) . 2_546 ?
C5 C4 C3 120.9(3) . . ?
C5 C4 H4A 119.5 . . ?
C3 C4 H4A 119.5 . . ?
C6 O4 Sm1 120.44(18) . 2 ?
C6 O5 Sm1 120.36(19) . . ?
C4 C5 C1 120.8(3) . 2_546 ?
C4 C5 H5 119.6 . . ?
C1 C5 H5 119.6 2_546 . ?
C7 O6 Sm1 121.1(2) . 2_655 ?
O5 C6 O4 126.8(3) . . ?
O5 C6 C6 116.7(3) . 2 ?
O4 C6 C6 116.5(3) . 2 ?
C7 O7 Sm1 119.0(2) . . ?
O7 C7 O6 126.8(3) . . ?
O7 C7 C7 117.2(3) . 2_655 ?
O6 C7 C7 116.0(3) . 2_655 ?
N1 C8 C9 122.9(3) . . ?
N1 C8 H8A 118.5 . . ?
C9 C8 H8A 118.5 . . ?
Sm1 O8 H80B 109.3 . . ?
Sm1 O8 H80C 109.6 . . ?
H80B O8 H80C 109.5 . . ?
C10 C9 C8 119.3(3) . . ?
C10 C9 H9A 120.4 . . ?
C8 C9 H9A 120.4 . . ?
H90D O9 H90C 109.5 . . ?
C9 C10 C11 119.7(3) . . ?
C9 C10 H10A 120.2 . . ?
C11 C10 H10A 120.2 . . ?
C10 C11 C19 117.3(3) . . ?
C10 C11 C12 122.6(3) . . ?
C19 C11 C12 120.1(3) . . ?
C13 C12 C11 120.8(3) . . ?
C13 C12 H12A 119.6 . . ?
C11 C12 H12A 119.6 . . ?
C12 C13 C14 121.0(3) . . ?
C12 C13 H13A 119.5 . . ?
C14 C13 H13A 119.5 . . ?
C15 C14 C18 117.8(3) . . ?
C15 C14 C13 122.2(3) . . ?
C18 C14 C13 120.0(3) . . ?
C16 C15 C14 119.2(3) . . ?
C16 C15 H15A 120.4 . . ?
C14 C15 H15A 120.4 . . ?
C15 C16 C17 119.1(3) . . ?
C15 C16 H16A 120.4 . . ?
C17 C16 H16A 120.4 . . ?
N2 C17 C16 123.8(4) . . ?
N2 C17 H17A 118.1 . . ?
C16 C17 H17A 118.1 . . ?
N2 C18 C14 123.1(3) . . ?
N2 C18 C19 117.9(3) . . ?
C14 C18 C19 119.0(3) . . ?
N1 C19 C11 123.0(3) . . ?
N1 C19 C18 118.0(3) . . ?
C11 C19 C18 119.0(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 S1 O1 Sm1 -34.9(4) . . . . ?
O3 S1 O1 Sm1 -162.1(3) . . . . ?
C2 S1 O1 Sm1 83.6(4) . . . . ?
O6 Sm1 O1 S1 -122.6(3) 2_655 . . . ?
O4 Sm1 O1 S1 7.3(4) 2 . . . ?
O3 Sm1 O1 S1 150.8(4) 2_556 . . . ?
O5 Sm1 O1 S1 4.2(3) . . . . ?
O7 Sm1 O1 S1 -66.3(4) . . . . ?
O8 Sm1 O1 S1 -135.9(4) . . . . ?
N1 Sm1 O1 S1 80.2(4) . . . . ?
N2 Sm1 O1 S1 114.8(4) . . . . ?
O6 Sm1 N1 C8 173.1(2) 2_655 . . . ?
O4 Sm1 N1 C8 108.2(3) 2 . . . ?
O3 Sm1 N1 C8 -101.7(3) 2_556 . . . ?
O5 Sm1 N1 C8 41.1(3) . . . . ?
O7 Sm1 N1 C8 56.8(3) . . . . ?
O1 Sm1 N1 C8 -27.4(3) . . . . ?
O8 Sm1 N1 C8 -77.5(3) . . . . ?
N2 Sm1 N1 C8 178.7(3) . . . . ?
O6 Sm1 N1 C19 -21.8(3) 2_655 . . . ?
O4 Sm1 N1 C19 -86.6(2) 2 . . . ?
O3 Sm1 N1 C19 63.4(2) 2_556 . . . ?
O5 Sm1 N1 C19 -153.7(2) . . . . ?
O7 Sm1 N1 C19 -138.0(2) . . . . ?
O1 Sm1 N1 C19 137.8(2) . . . . ?
O8 Sm1 N1 C19 87.7(3) . . . . ?
N2 Sm1 N1 C19 -16.1(2) . . . . ?
O6 Sm1 N2 C17 4.6(3) 2_655 . . . ?
O4 Sm1 N2 C17 -78.6(3) 2 . . . ?
O3 Sm1 N2 C17 112.9(3) 2_556 . . . ?
O5 Sm1 N2 C17 -122.5(3) . . . . ?
O7 Sm1 N2 C17 -29.4(3) . . . . ?
O1 Sm1 N2 C17 149.2(3) . . . . ?
O8 Sm1 N2 C17 61.1(3) . . . . ?
N1 Sm1 N2 C17 -171.1(3) . . . . ?
O6 Sm1 N2 C18 -170.7(2) 2_655 . . . ?
O4 Sm1 N2 C18 106.2(2) 2 . . . ?
O3 Sm1 N2 C18 -62.3(2) 2_556 . . . ?
O5 Sm1 N2 C18 62.3(2) . . . . ?
O7 Sm1 N2 C18 155.4(2) . . . . ?
O1 Sm1 N2 C18 -26.1(3) . . . . ?
O8 Sm1 N2 C18 -114.2(2) . . . . ?
N1 Sm1 N2 C18 13.6(2) . . . . ?
C5 C1 C2 C3 -0.3(5) 2_546 . . . ?
C5 C1 C2 S1 -179.3(3) 2_546 . . . ?
O2 S1 C2 C1 120.6(3) . . . . ?
O1 S1 C2 C1 -1.8(3) . . . . ?
O3 S1 C2 C1 -120.4(3) . . . . ?
O2 S1 C2 C3 -58.4(3) . . . . ?
O1 S1 C2 C3 179.2(2) . . . . ?
O3 S1 C2 C3 60.6(3) . . . . ?
O2 S1 O3 Sm1 -105.9(3) . . . 2_556 ?
O1 S1 O3 Sm1 22.6(4) . . . 2_556 ?
C2 S1 O3 Sm1 137.4(3) . . . 2_556 ?
C1 C2 C3 C4 180.0(3) . . . . ?
S1 C2 C3 C4 -1.0(4) . . . . ?
C1 C2 C3 C3 -1.1(5) . . . 2_546 ?
S1 C2 C3 C3 178.0(3) . . . 2_546 ?
C2 C3 C4 C5 178.5(3) . . . . ?
C3 C3 C4 C5 -0.4(5) 2_546 . . . ?
O6 Sm1 O5 C6 -46.0(3) 2_655 . . . ?
O4 Sm1 O5 C6 0.0(2) 2 . . . ?
O3 Sm1 O5 C6 135.1(2) 2_556 . . . ?
O7 Sm1 O5 C6 -82.2(2) . . . . ?
O1 Sm1 O5 C6 177.5(3) . . . . ?
O8 Sm1 O5 C6 -138.4(2) . . . . ?
N1 Sm1 O5 C6 88.7(2) . . . . ?
N2 Sm1 O5 C6 45.3(3) . . . . ?
C3 C4 C5 C1 1.8(5) . . . 2_546 ?
Sm1 O5 C6 O4 -179.8(3) . . . . ?
Sm1 O5 C6 C6 -0.2(5) . . . 2 ?
Sm1 O4 C6 O5 180.0(3) 2 . . . ?
Sm1 O4 C6 C6 0.3(5) 2 . . 2 ?
O6 Sm1 O7 C7 1.7(2) 2_655 . . . ?
O4 Sm1 O7 C7 83.7(2) 2 . . . ?
O3 Sm1 O7 C7 -76.2(3) 2_556 . . . ?
O5 Sm1 O7 C7 152.4(2) . . . . ?
O1 Sm1 O7 C7 -142.1(2) . . . . ?
O8 Sm1 O7 C7 -75.9(2) . . . . ?
N1 Sm1 O7 C7 136.6(2) . . . . ?
N2 Sm1 O7 C7 36.9(3) . . . . ?
Sm1 O7 C7 O6 178.7(3) . . . . ?
Sm1 O7 C7 C7 -1.7(4) . . . 2_655 ?
Sm1 O6 C7 O7 178.4(3) 2_655 . . . ?
Sm1 O6 C7 C7 -1.2(5) 2_655 . . 2_655 ?
C19 N1 C8 C9 -1.7(5) . . . . ?
Sm1 N1 C8 C9 163.8(3) . . . . ?
N1 C8 C9 C10 0.4(6) . . . . ?
C8 C9 C10 C11 1.3(6) . . . . ?
C9 C10 C11 C19 -1.6(5) . . . . ?
C9 C10 C11 C12 176.3(4) . . . . ?
C10 C11 C12 C13 -175.7(4) . . . . ?
C19 C11 C12 C13 2.2(6) . . . . ?
C11 C12 C13 C14 -1.1(6) . . . . ?
C12 C13 C14 C15 177.5(4) . . . . ?
C12 C13 C14 C18 -2.6(5) . . . . ?
C18 C14 C15 C16 1.1(5) . . . . ?
C13 C14 C15 C16 -179.0(4) . . . . ?
C14 C15 C16 C17 -3.2(6) . . . . ?
C18 N2 C17 C16 2.6(5) . . . . ?
Sm1 N2 C17 C16 -172.7(3) . . . . ?
C15 C16 C17 N2 1.4(6) . . . . ?
C17 N2 C18 C14 -4.9(5) . . . . ?
Sm1 N2 C18 C14 170.7(2) . . . . ?
C17 N2 C18 C19 173.3(3) . . . . ?
Sm1 N2 C18 C19 -11.1(4) . . . . ?
C15 C14 C18 N2 3.1(5) . . . . ?
C13 C14 C18 N2 -176.8(3) . . . . ?
C15 C14 C18 C19 -175.1(3) . . . . ?
C13 C14 C18 C19 5.0(5) . . . . ?
C8 N1 C19 C11 1.3(5) . . . . ?
Sm1 N1 C19 C11 -164.2(2) . . . . ?
C8 N1 C19 C18 -176.7(3) . . . . ?
Sm1 N1 C19 C18 17.9(4) . . . . ?
C10 C11 C19 N1 0.3(5) . . . . ?
C12 C11 C19 N1 -177.7(3) . . . . ?
C10 C11 C19 C18 178.3(3) . . . . ?
C12 C11 C19 C18 0.3(5) . . . . ?
N2 C18 C19 N1 -4.0(4) . . . . ?
C14 C18 C19 N1 174.2(3) . . . . ?
N2 C18 C19 C11 177.9(3) . . . . ?
C14 C18 C19 C11 -3.8(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.60
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.800
_refine_diff_density_min         -2.133
_refine_diff_density_rms         0.188
####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1475535'
_audit_update_record             
;
2016-04-21 deposited with the CCDC.
2016-06-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C19 H15 Eu N2 O9 S'
_chemical_formula_weight         599.35

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.8196(12)
_cell_length_b                   10.6527(14)
_cell_length_c                   10.9383(15)
_cell_angle_alpha                80.996(2)
_cell_angle_beta                 69.223(2)
_cell_angle_gamma                88.540(2)
_cell_volume                     948.5(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2836
_cell_measurement_theta_min      1.94
_cell_measurement_theta_max      25.25

_exptl_crystal_description       Block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.099
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             588
_exptl_absorpt_coefficient_mu    3.477
_exptl_absorpt_correction_type   Multi-SCAN
_exptl_absorpt_correction_T_min  0.6114
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku Saturn724 CCD'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            4905
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_av_sigmaI/netI    0.0737
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.94
_diffrn_reflns_theta_max         25.25
_reflns_number_total             3404
_reflns_number_gt                2946
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0542P)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         3404
_refine_ls_number_parameters     290
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_gt           0.0405
_refine_ls_wR_factor_ref         0.1109
_refine_ls_wR_factor_gt          0.0919
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_restrained_S_all      1.071
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001

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 0.16429(4) 0.57405(3) 0.19330(3) 0.01406(14) Uani 1 1 d . . .
S1 S -0.0873(2) 0.31529(17) 0.47772(17) 0.0144(4) Uani 1 1 d . . .
O1 O -0.1438(6) 0.3819(5) 0.0239(5) 0.0257(13) Uani 1 1 d . . .
O2 O 0.6772(6) 0.5926(5) -0.0786(5) 0.0249(13) Uani 1 1 d . . .
O3 O -0.0264(6) 0.4331(5) 0.1613(5) 0.0242(13) Uani 1 1 d . . .
O4 O 0.4367(6) 0.6431(5) 0.0534(5) 0.0243(13) Uani 1 1 d . . .
O5 O 0.3521(7) 0.4911(6) 0.3137(5) 0.0297(14) Uani 1 1 d . . .
H5WA H 0.4111 0.4384 0.2744 0.045 Uiso 1 1 calc R . .
H5WB H 0.2893 0.4483 0.4013 0.045 Uiso 1 1 d R . .
O6 O 0.0214(6) 0.4211(5) 0.3971(5) 0.0203(12) Uani 1 1 d . . .
O7 O -0.2302(6) 0.3013(5) 0.4437(5) 0.0238(12) Uani 1 1 d . . .
O8 O -0.1302(6) 0.3183(5) 0.6178(5) 0.0204(12) Uani 1 1 d . . .
O1W O 0.5924(7) 0.3200(6) 0.2639(6) 0.0329(14) Uani 1 1 d . . .
N1 N 0.1682(7) 0.8241(6) 0.1136(6) 0.0195(14) Uani 1 1 d . . .
N2 N -0.1113(7) 0.6860(6) 0.2609(6) 0.0181(14) Uani 1 1 d . . .
C1 C 0.2959(10) 0.8917(8) 0.0295(8) 0.0255(18) Uani 1 1 d . . .
H1A H 0.3892 0.8490 -0.0109 0.031 Uiso 1 1 calc R . .
C2 C 0.2994(10) 1.0248(8) -0.0027(9) 0.032(2) Uani 1 1 d . . .
H2A H 0.3898 1.0677 -0.0677 0.039 Uiso 1 1 calc R . .
C3 C 0.1670(11) 1.0909(8) 0.0633(8) 0.030(2) Uani 1 1 d . . .
H3A H 0.1708 1.1793 0.0495 0.036 Uiso 1 1 calc R . .
C4 C 0.0267(10) 1.0231(7) 0.1515(8) 0.0242(18) Uani 1 1 d . . .
C5 C -0.1175(11) 1.0812(8) 0.2165(9) 0.032(2) Uani 1 1 d . . .
H5A H -0.1204 1.1695 0.2036 0.038 Uiso 1 1 calc R . .
C6 C -0.2517(11) 1.0132(9) 0.2969(9) 0.034(2) Uani 1 1 d . . .
H6A H -0.3439 1.0555 0.3404 0.041 Uiso 1 1 calc R . .
C7 C -0.2557(10) 0.8805(8) 0.3164(8) 0.0245(18) Uani 1 1 d . . .
C8 C -0.3941(10) 0.8058(9) 0.3896(9) 0.033(2) Uani 1 1 d . . .
H8A H -0.4886 0.8437 0.4363 0.039 Uiso 1 1 calc R . .
C9 C -0.3926(10) 0.6759(8) 0.3936(9) 0.033(2) Uani 1 1 d . . .
H9A H -0.4869 0.6260 0.4375 0.040 Uiso 1 1 calc R . .
C10 C -0.2481(9) 0.6221(8) 0.3310(8) 0.0248(18) Uani 1 1 d . . .
H10A H -0.2469 0.5339 0.3388 0.030 Uiso 1 1 calc R . .
C11 C -0.1136(9) 0.8138(7) 0.2502(7) 0.0188(17) Uani 1 1 d . . .
C12 C 0.0309(9) 0.8866(7) 0.1701(7) 0.0189(16) Uani 1 1 d . . .
C13 C 0.5336(9) 0.5699(7) -0.0074(7) 0.0183(17) Uani 1 1 d . . .
C14 C -0.0494(8) 0.4470(7) 0.0544(7) 0.0152(16) Uani 1 1 d . . .
C15 C 0.0247(9) 0.1757(7) 0.4490(7) 0.0147(15) Uani 1 1 d . . .
C16 C 0.1803(8) 0.1896(7) 0.3611(7) 0.0165(16) Uani 1 1 d . . .
H16A H 0.2258 0.2703 0.3212 0.020 Uiso 1 1 calc R . .
C17 C 0.2730(9) 0.0792(8) 0.3307(8) 0.0252(19) Uani 1 1 d . . .
H17A H 0.3778 0.0882 0.2685 0.030 Uiso 1 1 calc R . .
C18 C 0.2097(9) -0.0383(7) 0.3916(7) 0.0195(17) Uani 1 1 d . . .
H18A H 0.2731 -0.1090 0.3734 0.023 Uiso 1 1 calc R . .
C19 C -0.0466(9) 0.0550(7) 0.5167(7) 0.0189(17) Uani 1 1 d . . .
H1WA H 0.6395 0.3066 0.3240 0.028 Uiso 1 1 d R . .
H1WB H 0.6598 0.3313 0.1858 0.028 Uiso 1 1 d R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Eu1 O4 2.405(5) . ?
Eu1 O1 2.418(5) 2_565 ?
Eu1 O3 2.432(5) . ?
Eu1 O8 2.441(5) 2_566 ?
Eu1 O2 2.451(5) 2_665 ?
Eu1 O6 2.487(5) . ?
Eu1 O5 2.524(6) . ?
Eu1 N2 2.594(6) . ?
Eu1 N1 2.667(7) . ?
Eu1 C13 3.222(7) . ?
Eu1 C13 3.242(7) 2_665 ?
Eu1 C14 3.240(7) . ?
S1 O7 1.452(6) . ?
S1 O8 1.448(5) . ?
S1 O6 1.453(5) . ?
S1 C15 1.771(7) . ?
O1 C14 1.258(9) . ?
O1 Eu1 2.418(5) 2_565 ?
O2 C13 1.236(8) . ?
O2 Eu1 2.451(5) 2_665 ?
O3 C14 1.243(9) . ?
O4 C13 1.227(8) . ?
O5 H5WA 0.8200 . ?
O5 H5WB 0.9656 . ?
O8 Eu1 2.441(5) 2_566 ?
O1W H1WA 0.8865 . ?
O1W H1WB 0.8419 . ?
N1 C1 1.316(10) . ?
N1 C12 1.360(9) . ?
N2 C10 1.315(10) . ?
N2 C11 1.348(10) . ?
C1 C2 1.405(11) . ?
C1 H1A 0.9300 . ?
C2 C3 1.378(12) . ?
C2 H2A 0.9300 . ?
C3 C4 1.402(12) . ?
C3 H3A 0.9300 . ?
C4 C5 1.401(12) . ?
C4 C12 1.437(11) . ?
C5 C6 1.343(13) . ?
C5 H5A 0.9300 . ?
C6 C7 1.396(12) . ?
C6 H6A 0.9300 . ?
C7 C8 1.386(12) . ?
C7 C11 1.439(10) . ?
C8 C9 1.378(12) . ?
C8 H8A 0.9300 . ?
C9 C10 1.374(11) . ?
C9 H9A 0.9300 . ?
C10 H10A 0.9300 . ?
C11 C12 1.428(11) . ?
C13 C13 1.581(15) 2_665 ?
C13 Eu1 3.242(7) 2_665 ?
C14 C14 1.531(14) 2_565 ?
C14 Eu1 3.251(7) 2_565 ?
C15 C16 1.364(10) . ?
C15 C19 1.418(10) . ?
C16 C17 1.429(10) . ?
C16 H16A 0.9300 . ?
C17 C18 1.354(11) . ?
C17 H17A 0.9300 . ?
C18 C19 1.429(10) 2_556 ?
C18 H18A 0.9300 . ?
C19 C18 1.429(10) 2_556 ?
C19 C19 1.433(14) 2_556 ?

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 O1 77.51(19) . 2_565 ?
O4 Eu1 O3 130.51(17) . . ?
O1 Eu1 O3 66.03(17) 2_565 . ?
O4 Eu1 O8 100.68(18) . 2_566 ?
O1 Eu1 O8 139.36(18) 2_565 2_566 ?
O3 Eu1 O8 128.79(17) . 2_566 ?
O4 Eu1 O2 66.59(17) . 2_665 ?
O1 Eu1 O2 76.42(19) 2_565 2_665 ?
O3 Eu1 O2 72.99(17) . 2_665 ?
O8 Eu1 O2 140.80(19) 2_566 2_665 ?
O4 Eu1 O6 139.22(18) . . ?
O1 Eu1 O6 133.64(17) 2_565 . ?
O3 Eu1 O6 67.69(17) . . ?
O8 Eu1 O6 72.71(17) 2_566 . ?
O2 Eu1 O6 92.83(17) 2_665 . ?
O4 Eu1 O5 71.97(19) . . ?
O1 Eu1 O5 143.01(18) 2_565 . ?
O3 Eu1 O5 121.39(19) . . ?
O8 Eu1 O5 68.18(17) 2_566 . ?
O2 Eu1 O5 72.62(18) 2_665 . ?
O6 Eu1 O5 68.27(18) . . ?
O4 Eu1 N2 133.78(18) . . ?
O1 Eu1 N2 82.50(19) 2_565 . ?
O3 Eu1 N2 74.37(18) . . ?
O8 Eu1 N2 69.62(18) 2_566 . ?
O2 Eu1 N2 146.17(19) 2_665 . ?
O6 Eu1 N2 82.82(18) . . ?
O5 Eu1 N2 134.13(18) . . ?
O4 Eu1 N1 71.44(18) . . ?
O1 Eu1 N1 69.35(18) 2_565 . ?
O3 Eu1 N1 120.53(18) . . ?
O8 Eu1 N1 71.68(17) 2_566 . ?
O2 Eu1 N1 130.22(17) 2_665 . ?
O6 Eu1 N1 136.92(17) . . ?
O5 Eu1 N1 117.99(19) . . ?
N2 Eu1 N1 62.54(19) . . ?
O4 Eu1 C13 18.94(18) . . ?
O1 Eu1 C13 75.92(18) 2_565 . ?
O3 Eu1 C13 115.25(18) . . ?
O8 Eu1 C13 114.47(18) 2_566 . ?
O2 Eu1 C13 47.67(18) 2_665 . ?
O6 Eu1 C13 128.23(18) . . ?
O5 Eu1 C13 68.39(19) . . ?
N2 Eu1 C13 148.92(19) . . ?
N1 Eu1 C13 88.75(19) . . ?
O4 Eu1 C13 47.24(18) . 2_665 ?
O1 Eu1 C13 75.42(19) 2_565 2_665 ?
O3 Eu1 C13 90.43(18) . 2_665 ?
O8 Eu1 C13 132.67(18) 2_566 2_665 ?
O2 Eu1 C13 19.37(18) 2_665 2_665 ?
O6 Eu1 C13 107.71(17) . 2_665 ?
O5 Eu1 C13 68.63(18) . 2_665 ?
N2 Eu1 C13 156.94(19) . 2_665 ?
N1 Eu1 C13 114.08(18) . 2_665 ?
C13 Eu1 C13 28.3(3) . 2_665 ?
O4 Eu1 C14 116.20(18) . . ?
O1 Eu1 C14 46.67(17) 2_565 . ?
O3 Eu1 C14 19.37(17) . . ?
O8 Eu1 C14 140.46(17) 2_566 . ?
O2 Eu1 C14 71.74(18) 2_665 . ?
O6 Eu1 C14 87.01(17) . . ?
O5 Eu1 C14 135.01(18) . . ?
N2 Eu1 C14 74.53(18) . . ?
N1 Eu1 C14 105.86(18) . . ?
C13 Eu1 C14 104.79(17) . . ?
C13 Eu1 C14 85.38(18) 2_665 . ?
O7 S1 O8 111.5(3) . . ?
O7 S1 O6 114.2(3) . . ?
O8 S1 O6 111.8(3) . . ?
O7 S1 C15 107.2(3) . . ?
O8 S1 C15 105.1(3) . . ?
O6 S1 C15 106.4(3) . . ?
C14 O1 Eu1 121.0(5) . 2_565 ?
C13 O2 Eu1 119.5(5) . 2_665 ?
C14 O3 Eu1 120.2(5) . . ?
C13 O4 Eu1 121.5(5) . . ?
Eu1 O5 H5WA 109.5 . . ?
Eu1 O5 H5WB 109.6 . . ?
H5WA O5 H5WB 107.2 . . ?
S1 O6 Eu1 156.6(3) . . ?
S1 O8 Eu1 153.1(3) . 2_566 ?
H1WA O1W H1WB 112.7 . . ?
C1 N1 C12 118.0(7) . . ?
C1 N1 Eu1 124.6(5) . . ?
C12 N1 Eu1 117.2(5) . . ?
C10 N2 C11 117.3(6) . . ?
C10 N2 Eu1 121.4(5) . . ?
C11 N2 Eu1 119.7(5) . . ?
N1 C1 C2 123.7(8) . . ?
N1 C1 H1A 118.1 . . ?
C2 C1 H1A 118.1 . . ?
C3 C2 C1 119.1(8) . . ?
C3 C2 H2A 120.4 . . ?
C1 C2 H2A 120.4 . . ?
C2 C3 C4 119.1(8) . . ?
C2 C3 H3A 120.5 . . ?
C4 C3 H3A 120.5 . . ?
C5 C4 C3 123.4(8) . . ?
C5 C4 C12 119.1(8) . . ?
C3 C4 C12 117.4(7) . . ?
C6 C5 C4 122.0(8) . . ?
C6 C5 H5A 119.0 . . ?
C4 C5 H5A 119.0 . . ?
C5 C6 C7 121.4(8) . . ?
C5 C6 H6A 119.3 . . ?
C7 C6 H6A 119.3 . . ?
C8 C7 C6 123.8(7) . . ?
C8 C7 C11 116.1(7) . . ?
C6 C7 C11 119.9(8) . . ?
C9 C8 C7 120.5(7) . . ?
C9 C8 H8A 119.8 . . ?
C7 C8 H8A 119.8 . . ?
C8 C9 C10 118.2(8) . . ?
C8 C9 H9A 120.9 . . ?
C10 C9 H9A 120.9 . . ?
N2 C10 C9 124.9(8) . . ?
N2 C10 H10A 117.6 . . ?
C9 C10 H10A 117.6 . . ?
N2 C11 C12 118.8(6) . . ?
N2 C11 C7 122.8(7) . . ?
C12 C11 C7 118.3(7) . . ?
N1 C12 C11 118.7(7) . . ?
N1 C12 C4 122.2(7) . . ?
C11 C12 C4 119.2(7) . . ?
O4 C13 O2 127.7(7) . . ?
O4 C13 C13 116.1(8) . 2_665 ?
O2 C13 C13 116.2(7) . 2_665 ?
O4 C13 Eu1 39.5(3) . . ?
O2 C13 Eu1 167.1(5) . . ?
C13 C13 Eu1 76.6(5) 2_665 . ?
O4 C13 Eu1 168.7(5) . 2_665 ?
O2 C13 Eu1 41.1(3) . 2_665 ?
C13 C13 Eu1 75.1(5) 2_665 2_665 ?
Eu1 C13 Eu1 151.7(3) . 2_665 ?
O3 C14 O1 127.2(7) . . ?
O3 C14 C14 117.2(8) . 2_565 ?
O1 C14 C14 115.6(8) . 2_565 ?
O3 C14 Eu1 40.4(4) . . ?
O1 C14 Eu1 167.7(5) . . ?
C14 C14 Eu1 76.7(5) 2_565 . ?
O3 C14 Eu1 166.8(5) . 2_565 ?
O1 C14 Eu1 39.6(3) . 2_565 ?
C14 C14 Eu1 76.0(5) 2_565 2_565 ?
Eu1 C14 Eu1 152.7(2) . 2_565 ?
C16 C15 C19 122.1(7) . . ?
C16 C15 S1 117.5(6) . . ?
C19 C15 S1 120.4(5) . . ?
C15 C16 C17 119.4(7) . . ?
C15 C16 H16A 120.3 . . ?
C17 C16 H16A 120.3 . . ?
C18 C17 C16 120.7(7) . . ?
C18 C17 H17A 119.6 . . ?
C16 C17 H17A 119.6 . . ?
C17 C18 C19 120.7(7) . 2_556 ?
C17 C18 H18A 119.7 . . ?
C19 C18 H18A 119.7 2_556 . ?
C15 C19 C18 122.9(7) . 2_556 ?
C15 C19 C19 117.8(8) . 2_556 ?
C18 C19 C19 119.1(8) 2_556 2_556 ?

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
O4 Eu1 O3 C14 -47.2(6) . . . . ?
O1 Eu1 O3 C14 -0.9(5) 2_565 . . . ?
O8 Eu1 O3 C14 134.2(5) 2_566 . . . ?
O2 Eu1 O3 C14 -83.3(5) 2_665 . . . ?
O6 Eu1 O3 C14 176.3(6) . . . . ?
O5 Eu1 O3 C14 -139.7(5) . . . . ?
N2 Eu1 O3 C14 87.7(5) . . . . ?
N1 Eu1 O3 C14 43.9(6) . . . . ?
C13 Eu1 O3 C14 -60.6(6) . . . . ?
C13 Eu1 O3 C14 -74.7(5) 2_665 . . . ?
O1 Eu1 O4 C13 -83.0(6) 2_565 . . . ?
O3 Eu1 O4 C13 -40.4(7) . . . . ?
O8 Eu1 O4 C13 138.5(6) 2_566 . . . ?
O2 Eu1 O4 C13 -2.5(6) 2_665 . . . ?
O6 Eu1 O4 C13 62.6(7) . . . . ?
O5 Eu1 O4 C13 75.8(6) . . . . ?
N2 Eu1 O4 C13 -149.6(6) . . . . ?
N1 Eu1 O4 C13 -155.1(6) . . . . ?
C13 Eu1 O4 C13 -1.4(7) 2_665 . . . ?
C14 Eu1 O4 C13 -56.1(6) . . . . ?
O7 S1 O6 Eu1 -33.8(8) . . . . ?
O8 S1 O6 Eu1 -161.7(7) . . . . ?
C15 S1 O6 Eu1 84.1(8) . . . . ?
O4 Eu1 O6 S1 -123.3(7) . . . . ?
O1 Eu1 O6 S1 7.1(9) 2_565 . . . ?
O3 Eu1 O6 S1 3.6(7) . . . . ?
O8 Eu1 O6 S1 150.4(8) 2_566 . . . ?
O2 Eu1 O6 S1 -66.8(8) 2_665 . . . ?
O5 Eu1 O6 S1 -136.8(8) . . . . ?
N2 Eu1 O6 S1 79.6(8) . . . . ?
N1 Eu1 O6 S1 115.0(7) . . . . ?
C13 Eu1 O6 S1 -101.7(8) . . . . ?
C13 Eu1 O6 S1 -79.4(8) 2_665 . . . ?
C14 Eu1 O6 S1 4.8(8) . . . . ?
O7 S1 O8 Eu1 -107.0(7) . . . 2_566 ?
O6 S1 O8 Eu1 22.3(8) . . . 2_566 ?
C15 S1 O8 Eu1 137.3(7) . . . 2_566 ?
O4 Eu1 N1 C1 4.2(6) . . . . ?
O1 Eu1 N1 C1 -79.0(6) 2_565 . . . ?
O3 Eu1 N1 C1 -122.5(6) . . . . ?
O8 Eu1 N1 C1 112.7(6) 2_566 . . . ?
O2 Eu1 N1 C1 -29.4(7) 2_665 . . . ?
O6 Eu1 N1 C1 148.4(6) . . . . ?
O5 Eu1 N1 C1 61.0(6) . . . . ?
N2 Eu1 N1 C1 -171.2(7) . . . . ?
C13 Eu1 N1 C1 -3.6(6) . . . . ?
C13 Eu1 N1 C1 -16.6(7) 2_665 . . . ?
C14 Eu1 N1 C1 -108.6(6) . . . . ?
O4 Eu1 N1 C12 -171.8(5) . . . . ?
O1 Eu1 N1 C12 104.9(5) 2_565 . . . ?
O3 Eu1 N1 C12 61.5(5) . . . . ?
O8 Eu1 N1 C12 -63.3(5) 2_566 . . . ?
O2 Eu1 N1 C12 154.6(5) 2_665 . . . ?
O6 Eu1 N1 C12 -27.6(6) . . . . ?
O5 Eu1 N1 C12 -115.0(5) . . . . ?
N2 Eu1 N1 C12 12.7(5) . . . . ?
C13 Eu1 N1 C12 -179.6(5) . . . . ?
C13 Eu1 N1 C12 167.4(5) 2_665 . . . ?
C14 Eu1 N1 C12 75.3(5) . . . . ?
O4 Eu1 N2 C10 173.6(5) . . . . ?
O1 Eu1 N2 C10 109.0(6) 2_565 . . . ?
O3 Eu1 N2 C10 41.8(6) . . . . ?
O8 Eu1 N2 C10 -101.1(6) 2_566 . . . ?
O2 Eu1 N2 C10 57.4(7) 2_665 . . . ?
O6 Eu1 N2 C10 -26.9(6) . . . . ?
O5 Eu1 N2 C10 -77.0(7) . . . . ?
N1 Eu1 N2 C10 179.5(7) . . . . ?
C13 Eu1 N2 C10 155.0(5) . . . . ?
C13 Eu1 N2 C10 92.2(7) 2_665 . . . ?
C14 Eu1 N2 C10 61.9(6) . . . . ?
O4 Eu1 N2 C11 -21.0(6) . . . . ?
O1 Eu1 N2 C11 -85.6(5) 2_565 . . . ?
O3 Eu1 N2 C11 -152.7(6) . . . . ?
O8 Eu1 N2 C11 64.3(5) 2_566 . . . ?
O2 Eu1 N2 C11 -137.2(5) 2_665 . . . ?
O6 Eu1 N2 C11 138.5(5) . . . . ?
O5 Eu1 N2 C11 88.4(6) . . . . ?
N1 Eu1 N2 C11 -15.0(5) . . . . ?
C13 Eu1 N2 C11 -39.6(7) . . . . ?
C13 Eu1 N2 C11 -102.4(7) 2_665 . . . ?
C14 Eu1 N2 C11 -132.6(6) . . . . ?
C12 N1 C1 C2 1.6(12) . . . . ?
Eu1 N1 C1 C2 -174.4(6) . . . . ?
N1 C1 C2 C3 4.9(13) . . . . ?
C1 C2 C3 C4 -6.1(13) . . . . ?
C2 C3 C4 C5 -175.6(8) . . . . ?
C2 C3 C4 C12 1.3(12) . . . . ?
C3 C4 C5 C6 177.6(9) . . . . ?
C12 C4 C5 C6 0.7(13) . . . . ?
C4 C5 C6 C7 -2.1(14) . . . . ?
C5 C6 C7 C8 -174.7(9) . . . . ?
C5 C6 C7 C11 0.3(13) . . . . ?
C6 C7 C8 C9 173.5(9) . . . . ?
C11 C7 C8 C9 -1.7(13) . . . . ?
C7 C8 C9 C10 4.4(14) . . . . ?
C11 N2 C10 C9 0.1(12) . . . . ?
Eu1 N2 C10 C9 165.9(7) . . . . ?
C8 C9 C10 N2 -3.8(14) . . . . ?
C10 N2 C11 C12 -177.3(7) . . . . ?
Eu1 N2 C11 C12 16.7(9) . . . . ?
C10 N2 C11 C7 2.9(11) . . . . ?
Eu1 N2 C11 C7 -163.1(6) . . . . ?
C8 C7 C11 N2 -2.1(12) . . . . ?
C6 C7 C11 N2 -177.5(7) . . . . ?
C8 C7 C11 C12 178.1(7) . . . . ?
C6 C7 C11 C12 2.7(11) . . . . ?
C1 N1 C12 C11 173.3(7) . . . . ?
Eu1 N1 C12 C11 -10.4(9) . . . . ?
C1 N1 C12 C4 -6.6(11) . . . . ?
Eu1 N1 C12 C4 169.7(6) . . . . ?
N2 C11 C12 N1 -3.7(11) . . . . ?
C7 C11 C12 N1 176.1(7) . . . . ?
N2 C11 C12 C4 176.2(7) . . . . ?
C7 C11 C12 C4 -4.0(11) . . . . ?
C5 C4 C12 N1 -177.7(7) . . . . ?
C3 C4 C12 N1 5.2(11) . . . . ?
C5 C4 C12 C11 2.4(11) . . . . ?
C3 C4 C12 C11 -174.7(7) . . . . ?
Eu1 O4 C13 O2 -177.5(6) . . . . ?
Eu1 O4 C13 C13 2.3(11) . . . 2_665 ?
Eu1 O4 C13 Eu1 175(3) . . . 2_665 ?
Eu1 O2 C13 O4 -177.7(6) 2_665 . . . ?
Eu1 O2 C13 C13 2.4(11) 2_665 . . 2_665 ?
Eu1 O2 C13 Eu1 175(2) 2_665 . . . ?
O1 Eu1 C13 O4 92.5(6) 2_565 . . . ?
O3 Eu1 C13 O4 147.0(6) . . . . ?
O8 Eu1 C13 O4 -45.7(6) 2_566 . . . ?
O2 Eu1 C13 O4 176.8(7) 2_665 . . . ?
O6 Eu1 C13 O4 -132.4(6) . . . . ?
O5 Eu1 C13 O4 -97.4(6) . . . . ?
N2 Eu1 C13 O4 45.1(8) . . . . ?
N1 Eu1 C13 O4 23.5(6) . . . . ?
C13 Eu1 C13 O4 177.8(10) 2_665 . . . ?
C14 Eu1 C13 O4 129.6(6) . . . . ?
O4 Eu1 C13 O2 9(2) . . . . ?
O1 Eu1 C13 O2 101(3) 2_565 . . . ?
O3 Eu1 C13 O2 156(3) . . . . ?
O8 Eu1 C13 O2 -37(3) 2_566 . . . ?
O2 Eu1 C13 O2 -174(3) 2_665 . . . ?
O6 Eu1 C13 O2 -124(3) . . . . ?
O5 Eu1 C13 O2 -89(3) . . . . ?
N2 Eu1 C13 O2 54(3) . . . . ?
N1 Eu1 C13 O2 32(3) . . . . ?
C13 Eu1 C13 O2 -173(3) 2_665 . . . ?
C14 Eu1 C13 O2 138(3) . . . . ?
O4 Eu1 C13 C13 -177.8(10) . . . 2_665 ?
O1 Eu1 C13 C13 -85.3(6) 2_565 . . 2_665 ?
O3 Eu1 C13 C13 -30.9(6) . . . 2_665 ?
O8 Eu1 C13 C13 136.5(5) 2_566 . . 2_665 ?
O2 Eu1 C13 C13 -1.0(5) 2_665 . . 2_665 ?
O6 Eu1 C13 C13 49.8(6) . . . 2_665 ?
O5 Eu1 C13 C13 84.8(6) . . . 2_665 ?
N2 Eu1 C13 C13 -132.7(5) . . . 2_665 ?
N1 Eu1 C13 C13 -154.3(6) . . . 2_665 ?
C14 Eu1 C13 C13 -48.3(6) . . . 2_665 ?
O4 Eu1 C13 Eu1 -177.8(10) . . . 2_665 ?
O1 Eu1 C13 Eu1 -85.3(6) 2_565 . . 2_665 ?
O3 Eu1 C13 Eu1 -30.9(6) . . . 2_665 ?
O8 Eu1 C13 Eu1 136.5(5) 2_566 . . 2_665 ?
O2 Eu1 C13 Eu1 -1.0(5) 2_665 . . 2_665 ?
O6 Eu1 C13 Eu1 49.8(6) . . . 2_665 ?
O5 Eu1 C13 Eu1 84.8(6) . . . 2_665 ?
N2 Eu1 C13 Eu1 -132.7(5) . . . 2_665 ?
N1 Eu1 C13 Eu1 -154.3(6) . . . 2_665 ?
C13 Eu1 C13 Eu1 0.004(1) 2_665 . . 2_665 ?
C14 Eu1 C13 Eu1 -48.3(6) . . . 2_665 ?
Eu1 O3 C14 O1 -179.9(5) . . . . ?
Eu1 O3 C14 C14 1.3(10) . . . 2_565 ?
Eu1 O3 C14 Eu1 177.6(19) . . . 2_565 ?
Eu1 O1 C14 O3 -179.1(6) 2_565 . . . ?
Eu1 O1 C14 C14 -0.2(10) 2_565 . . 2_565 ?
Eu1 O1 C14 Eu1 -180(2) 2_565 . . . ?
O4 Eu1 C14 O3 141.6(5) . . . . ?
O1 Eu1 C14 O3 178.9(6) 2_565 . . . ?
O8 Eu1 C14 O3 -61.4(6) 2_566 . . . ?
O2 Eu1 C14 O3 90.5(5) 2_665 . . . ?
O6 Eu1 C14 O3 -3.4(5) . . . . ?
O5 Eu1 C14 O3 51.3(6) . . . . ?
N2 Eu1 C14 O3 -86.8(5) . . . . ?
N1 Eu1 C14 O3 -141.6(5) . . . . ?
C13 Eu1 C14 O3 125.4(5) . . . . ?
C13 Eu1 C14 O3 104.6(5) 2_665 . . . ?
O4 Eu1 C14 O1 142(2) . . . . ?
O1 Eu1 C14 O1 179(2) 2_565 . . . ?
O3 Eu1 C14 O1 1(2) . . . . ?
O8 Eu1 C14 O1 -61(2) 2_566 . . . ?
O2 Eu1 C14 O1 91(2) 2_665 . . . ?
O6 Eu1 C14 O1 -3(2) . . . . ?
O5 Eu1 C14 O1 52(2) . . . . ?
N2 Eu1 C14 O1 -86(2) . . . . ?
N1 Eu1 C14 O1 -141(2) . . . . ?
C13 Eu1 C14 O1 126(2) . . . . ?
C13 Eu1 C14 O1 105(2) 2_665 . . . ?
O4 Eu1 C14 C14 -37.2(6) . . . 2_565 ?
O1 Eu1 C14 C14 0.1(4) 2_565 . . 2_565 ?
O3 Eu1 C14 C14 -178.8(9) . . . 2_565 ?
O8 Eu1 C14 C14 119.8(5) 2_566 . . 2_565 ?
O2 Eu1 C14 C14 -88.3(5) 2_665 . . 2_565 ?
O6 Eu1 C14 C14 177.8(5) . . . 2_565 ?
O5 Eu1 C14 C14 -127.4(5) . . . 2_565 ?
N2 Eu1 C14 C14 94.4(5) . . . 2_565 ?
N1 Eu1 C14 C14 39.6(5) . . . 2_565 ?
C13 Eu1 C14 C14 -53.4(5) . . . 2_565 ?
C13 Eu1 C14 C14 -74.2(5) 2_665 . . 2_565 ?
O4 Eu1 C14 Eu1 -37.2(6) . . . 2_565 ?
O1 Eu1 C14 Eu1 0.1(4) 2_565 . . 2_565 ?
O3 Eu1 C14 Eu1 -178.8(9) . . . 2_565 ?
O8 Eu1 C14 Eu1 119.8(5) 2_566 . . 2_565 ?
O2 Eu1 C14 Eu1 -88.3(5) 2_665 . . 2_565 ?
O6 Eu1 C14 Eu1 177.8(5) . . . 2_565 ?
O5 Eu1 C14 Eu1 -127.4(5) . . . 2_565 ?
N2 Eu1 C14 Eu1 94.4(5) . . . 2_565 ?
N1 Eu1 C14 Eu1 39.6(5) . . . 2_565 ?
C13 Eu1 C14 Eu1 -53.4(5) . . . 2_565 ?
C13 Eu1 C14 Eu1 -74.2(5) 2_665 . . 2_565 ?
O7 S1 C15 C16 121.3(6) . . . . ?
O8 S1 C15 C16 -120.0(6) . . . . ?
O6 S1 C15 C16 -1.3(7) . . . . ?
O7 S1 C15 C19 -59.2(7) . . . . ?
O8 S1 C15 C19 59.6(7) . . . . ?
O6 S1 C15 C19 178.3(6) . . . . ?
C19 C15 C16 C17 3.0(11) . . . . ?
S1 C15 C16 C17 -177.4(6) . . . . ?
C15 C16 C17 C18 -2.2(12) . . . . ?
C16 C17 C18 C19 2.6(12) . . . 2_556 ?
C16 C15 C19 C18 -179.6(7) . . . 2_556 ?
S1 C15 C19 C18 0.9(10) . . . 2_556 ?
C16 C15 C19 C19 -4.1(13) . . . 2_556 ?
S1 C15 C19 C19 176.3(7) . . . 2_556 ?

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        25.25
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         0.830
_refine_diff_density_min         -0.895
_refine_diff_density_rms         0.205
####################################################################### 
# 
# 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_2
_database_code_depnum_ccdc_archive 'CCDC 1475536'
_audit_update_record             
;
2016-04-21 deposited with the CCDC.
2016-06-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C19 H15 La N2 O9 S'
_chemical_formula_weight         586.30

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'
La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.8819(6)
_cell_length_b                   10.7645(7)
_cell_length_c                   11.2236(7)
_cell_angle_alpha                80.0930(10)
_cell_angle_beta                 69.8510(10)
_cell_angle_gamma                88.7400(10)
_cell_volume                     991.58(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    3023
_cell_measurement_theta_min      1.96
_cell_measurement_theta_max      25.25

_exptl_crystal_description       Block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.964
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             576
_exptl_absorpt_coefficient_mu    2.318
_exptl_absorpt_correction_type   Multi-SCAN
_exptl_absorpt_correction_T_min  0.6114
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku Saturn724 CCD'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            4972
_diffrn_reflns_av_R_equivalents  0.0213
_diffrn_reflns_av_sigmaI/netI    0.0458
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.96
_diffrn_reflns_theta_max         25.25
_reflns_number_total             3546
_reflns_number_gt                3227
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0542P)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         3546
_refine_ls_number_parameters     290
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0339
_refine_ls_R_factor_gt           0.0297
_refine_ls_wR_factor_ref         0.0763
_refine_ls_wR_factor_gt          0.0732
_refine_ls_goodness_of_fit_ref   0.896
_refine_ls_restrained_S_all      0.896
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
La1 La 0.16418(2) 0.577004(16) 0.196346(16) 0.01626(5) Uani 1 1 d . . .
S1 S -0.09037(9) 0.31204(7) 0.47798(7) 0.01736(17) Uani 1 1 d . . .
O1 O -0.1447(3) 0.3821(2) 0.0263(2) 0.0284(6) Uani 1 1 d . . .
O2 O 0.6756(3) 0.5923(2) -0.0848(2) 0.0285(6) Uani 1 1 d . . .
O3 O -0.0366(3) 0.4381(2) 0.1615(2) 0.0262(6) Uani 1 1 d . . .
O4 O 0.4425(3) 0.6441(2) 0.0495(2) 0.0318(6) Uani 1 1 d . . .
O5 O 0.3582(3) 0.4902(3) 0.3190(3) 0.0381(7) Uani 1 1 d . . .
H5WA H 0.4373 0.4626 0.2692 0.057 Uiso 1 1 calc R . .
H5WB H 0.2989 0.4357 0.3993 0.057 Uiso 1 1 d R . .
O6 O 0.0171(3) 0.4186(2) 0.3992(2) 0.0226(5) Uani 1 1 d . . .
O7 O -0.2316(3) 0.2995(2) 0.4443(2) 0.0273(6) Uani 1 1 d . . .
O8 O -0.1313(3) 0.3132(2) 0.6153(2) 0.0261(6) Uani 1 1 d . . .
O1W O 0.5972(3) 0.3253(3) 0.2660(2) 0.0386(7) Uani 1 1 d . . .
N1 N 0.1616(3) 0.8327(3) 0.1139(3) 0.0237(7) Uani 1 1 d . . .
N2 N -0.1164(3) 0.6963(3) 0.2610(3) 0.0245(7) Uani 1 1 d . . .
C1 C 0.2890(5) 0.9000(4) 0.0311(4) 0.0337(10) Uani 1 1 d . . .
H1A H 0.3787 0.8571 -0.0099 0.040 Uiso 1 1 calc R . .
C2 C 0.2970(5) 1.0323(4) 0.0014(4) 0.0390(10) Uani 1 1 d . . .
H2A H 0.3888 1.0754 -0.0588 0.047 Uiso 1 1 calc R . .
C3 C 0.1667(5) 1.0964(4) 0.0630(4) 0.0364(10) Uani 1 1 d . . .
H3A H 0.1704 1.1842 0.0476 0.044 Uiso 1 1 calc R . .
C4 C 0.0285(4) 1.0295(3) 0.1490(4) 0.0306(9) Uani 1 1 d . . .
C5 C -0.1133(5) 1.0902(4) 0.2157(4) 0.0381(10) Uani 1 1 d . . .
H5A H -0.1133 1.1779 0.2037 0.046 Uiso 1 1 calc R . .
C6 C -0.2458(5) 1.0228(4) 0.2951(4) 0.0382(10) Uani 1 1 d . . .
H6A H -0.3349 1.0645 0.3393 0.046 Uiso 1 1 calc R . .
C7 C -0.2526(4) 0.8885(3) 0.3129(3) 0.0299(9) Uani 1 1 d . . .
C8 C -0.3914(4) 0.8145(4) 0.3878(4) 0.0366(10) Uani 1 1 d . . .
H8A H -0.4840 0.8528 0.4317 0.044 Uiso 1 1 calc R . .
C9 C -0.3913(5) 0.6869(4) 0.3965(4) 0.0411(11) Uani 1 1 d . . .
H9A H -0.4833 0.6373 0.4457 0.049 Uiso 1 1 calc R . .
C10 C -0.2508(4) 0.6319(4) 0.3306(4) 0.0334(10) Uani 1 1 d . . .
H10A H -0.2521 0.5447 0.3362 0.040 Uiso 1 1 calc R . .
C11 C -0.1154(4) 0.8248(3) 0.2501(3) 0.0238(8) Uani 1 1 d . . .
C12 C 0.0284(4) 0.8951(3) 0.1701(3) 0.0237(8) Uani 1 1 d . . .
C13 C 0.5345(4) 0.5683(3) -0.0100(3) 0.0221(8) Uani 1 1 d . . .
C14 C -0.0522(4) 0.4487(3) 0.0553(3) 0.0202(7) Uani 1 1 d . . .
C15 C 0.0226(4) 0.1750(3) 0.4494(3) 0.0185(7) Uani 1 1 d . . .
C16 C 0.1760(4) 0.1902(3) 0.3626(3) 0.0252(8) Uani 1 1 d . . .
H16A H 0.2190 0.2705 0.3207 0.030 Uiso 1 1 calc R . .
C17 C 0.2677(4) 0.0840(3) 0.3371(3) 0.0288(9) Uani 1 1 d . . .
H17A H 0.3728 0.0948 0.2798 0.035 Uiso 1 1 calc R . .
C18 C 0.2061(4) -0.0343(3) 0.3945(3) 0.0237(8) Uani 1 1 d . . .
H18A H 0.2683 -0.1035 0.3743 0.028 Uiso 1 1 calc R . .
C19 C -0.0475(4) 0.0532(3) 0.5148(3) 0.0181(7) Uani 1 1 d . . .
H1WA H 0.6386 0.3048 0.3222 0.027 Uiso 1 1 d R . .
H1WB H 0.6590 0.3295 0.1840 0.027 Uiso 1 1 d R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
La1 O4 2.492(2) . ?
La1 O2 2.522(2) 2_665 ?
La1 O3 2.523(2) . ?
La1 O8 2.524(2) 2_566 ?
La1 O1 2.527(2) 2_565 ?
La1 O6 2.552(2) . ?
La1 O5 2.619(3) . ?
La1 N2 2.706(3) . ?
La1 N1 2.751(3) . ?
S1 O7 1.444(3) . ?
S1 O6 1.458(2) . ?
S1 O8 1.459(2) . ?
S1 C15 1.778(3) . ?
O1 C14 1.258(4) . ?
O1 La1 2.527(2) 2_565 ?
O2 C13 1.248(4) . ?
O2 La1 2.522(2) 2_665 ?
O3 C14 1.233(4) . ?
O4 C13 1.250(4) . ?
O5 H5WA 0.8200 . ?
O5 H5WB 0.9687 . ?
O8 La1 2.524(2) 2_566 ?
O1W H1WA 0.8309 . ?
O1W H1WB 0.8878 . ?
N1 C1 1.322(4) . ?
N1 C12 1.359(4) . ?
N2 C10 1.313(4) . ?
N2 C11 1.367(4) . ?
C1 C2 1.403(5) . ?
C1 H1A 0.9300 . ?
C2 C3 1.368(6) . ?
C2 H2A 0.9300 . ?
C3 C4 1.393(5) . ?
C3 H3A 0.9300 . ?
C4 C12 1.424(5) . ?
C4 C5 1.434(5) . ?
C5 C6 1.341(5) . ?
C5 H5A 0.9300 . ?
C6 C7 1.425(5) . ?
C6 H6A 0.9300 . ?
C7 C8 1.400(5) . ?
C7 C11 1.411(5) . ?
C8 C9 1.361(6) . ?
C8 H8A 0.9300 . ?
C9 C10 1.392(5) . ?
C9 H9A 0.9300 . ?
C10 H10A 0.9300 . ?
C11 C12 1.424(5) . ?
C13 C13 1.556(6) 2_665 ?
C14 C14 1.550(6) 2_565 ?
C15 C16 1.368(4) . ?
C15 C19 1.427(4) . ?
C16 C17 1.401(5) . ?
C16 H16A 0.9300 . ?
C17 C18 1.357(5) . ?
C17 H17A 0.9300 . ?
C18 C19 1.420(4) 2_556 ?
C18 H18A 0.9300 . ?
C19 C18 1.420(4) 2_556 ?
C19 C19 1.425(6) 2_556 ?

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 La1 O2 64.80(7) . 2_665 ?
O4 La1 O3 128.31(8) . . ?
O2 La1 O3 74.27(8) 2_665 . ?
O4 La1 O8 102.86(8) . 2_566 ?
O2 La1 O8 140.68(8) 2_665 2_566 ?
O3 La1 O8 128.81(7) . 2_566 ?
O4 La1 O1 75.62(8) . 2_565 ?
O2 La1 O1 75.09(8) 2_665 2_565 ?
O3 La1 O1 64.06(7) . 2_565 ?
O8 La1 O1 140.81(8) 2_566 2_565 ?
O4 La1 O6 140.11(8) . . ?
O2 La1 O6 92.40(7) 2_665 . ?
O3 La1 O6 68.08(7) . . ?
O8 La1 O6 73.59(7) 2_566 . ?
O1 La1 O6 132.14(7) 2_565 . ?
O4 La1 O5 72.87(8) . . ?
O2 La1 O5 72.06(8) 2_665 . ?
O3 La1 O5 123.05(8) . . ?
O8 La1 O5 68.61(8) 2_566 . ?
O1 La1 O5 141.65(8) 2_565 . ?
O6 La1 O5 68.93(8) . . ?
O4 La1 N2 133.48(8) . . ?
O2 La1 N2 147.11(9) 2_665 . ?
O3 La1 N2 73.95(8) . . ?
O8 La1 N2 69.12(9) 2_566 . ?
O1 La1 N2 83.62(8) 2_565 . ?
O6 La1 N2 83.50(8) . . ?
O5 La1 N2 134.42(8) . . ?
O4 La1 N1 73.60(8) . . ?
O2 La1 N1 130.99(8) 2_665 . ?
O3 La1 N1 117.40(8) . . ?
O8 La1 N1 71.76(8) 2_566 . ?
O1 La1 N1 70.34(8) 2_565 . ?
O6 La1 N1 136.61(7) . . ?
O5 La1 N1 119.43(9) . . ?
N2 La1 N1 60.22(8) . . ?
O7 S1 O6 113.76(14) . . ?
O7 S1 O8 111.82(14) . . ?
O6 S1 O8 111.62(14) . . ?
O7 S1 C15 107.91(15) . . ?
O6 S1 C15 105.80(14) . . ?
O8 S1 C15 105.30(14) . . ?
C14 O1 La1 121.15(19) . 2_565 ?
C13 O2 La1 120.1(2) . 2_665 ?
C14 O3 La1 120.8(2) . . ?
C13 O4 La1 121.3(2) . . ?
La1 O5 H5WA 109.5 . . ?
La1 O5 H5WB 110.1 . . ?
H5WA O5 H5WB 118.1 . . ?
S1 O6 La1 157.16(15) . . ?
S1 O8 La1 152.58(14) . 2_566 ?
H1WA O1W H1WB 118.2 . . ?
C1 N1 C12 118.0(3) . . ?
C1 N1 La1 123.1(2) . . ?
C12 N1 La1 118.5(2) . . ?
C10 N2 C11 118.2(3) . . ?
C10 N2 La1 119.9(2) . . ?
C11 N2 La1 119.9(2) . . ?
N1 C1 C2 124.0(3) . . ?
N1 C1 H1A 118.0 . . ?
C2 C1 H1A 118.0 . . ?
C3 C2 C1 118.4(3) . . ?
C3 C2 H2A 120.8 . . ?
C1 C2 H2A 120.8 . . ?
C2 C3 C4 119.6(4) . . ?
C2 C3 H3A 120.2 . . ?
C4 C3 H3A 120.2 . . ?
C3 C4 C12 118.3(3) . . ?
C3 C4 C5 122.7(3) . . ?
C12 C4 C5 119.0(3) . . ?
C6 C5 C4 121.1(3) . . ?
C6 C5 H5A 119.4 . . ?
C4 C5 H5A 119.4 . . ?
C5 C6 C7 121.2(3) . . ?
C5 C6 H6A 119.4 . . ?
C7 C6 H6A 119.4 . . ?
C8 C7 C11 117.2(3) . . ?
C8 C7 C6 123.3(3) . . ?
C11 C7 C6 119.5(3) . . ?
C9 C8 C7 120.2(3) . . ?
C9 C8 H8A 119.9 . . ?
C7 C8 H8A 119.9 . . ?
C8 C9 C10 118.8(4) . . ?
C8 C9 H9A 120.6 . . ?
C10 C9 H9A 120.6 . . ?
N2 C10 C9 123.6(4) . . ?
N2 C10 H10A 118.2 . . ?
C9 C10 H10A 118.2 . . ?
N2 C11 C7 122.0(3) . . ?
N2 C11 C12 118.2(3) . . ?
C7 C11 C12 119.8(3) . . ?
N1 C12 C11 119.3(3) . . ?
N1 C12 C4 121.4(3) . . ?
C11 C12 C4 119.2(3) . . ?
O2 C13 O4 126.2(3) . . ?
O2 C13 C13 117.1(3) . 2_665 ?
O4 C13 C13 116.7(3) . 2_665 ?
O3 C14 O1 126.1(3) . . ?
O3 C14 C14 118.1(4) . 2_565 ?
O1 C14 C14 115.7(4) . 2_565 ?
C16 C15 C19 121.7(3) . . ?
C16 C15 S1 118.2(2) . . ?
C19 C15 S1 120.1(2) . . ?
C15 C16 C17 119.6(3) . . ?
C15 C16 H16A 120.2 . . ?
C17 C16 H16A 120.2 . . ?
C18 C17 C16 121.3(3) . . ?
C18 C17 H17A 119.4 . . ?
C16 C17 H17A 119.4 . . ?
C17 C18 C19 120.5(3) . 2_556 ?
C17 C18 H18A 119.8 . . ?
C19 C18 H18A 119.8 2_556 . ?
C18 C19 C19 119.4(3) 2_556 2_556 ?
C18 C19 C15 123.1(3) 2_556 . ?
C19 C19 C15 117.5(3) 2_556 . ?

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
O4 La1 O3 C14 -40.8(3) . . . . ?
O2 La1 O3 C14 -79.0(2) 2_665 . . . ?
O8 La1 O3 C14 137.4(2) 2_566 . . . ?
O1 La1 O3 C14 1.8(2) 2_565 . . . ?
O6 La1 O3 C14 -178.2(3) . . . . ?
O5 La1 O3 C14 -134.6(2) . . . . ?
N2 La1 O3 C14 92.4(2) . . . . ?
N1 La1 O3 C14 49.4(3) . . . . ?
O2 La1 O4 C13 -0.9(3) 2_665 . . . ?
O3 La1 O4 C13 -42.1(3) . . . . ?
O8 La1 O4 C13 139.4(3) 2_566 . . . ?
O1 La1 O4 C13 -81.0(3) 2_565 . . . ?
O6 La1 O4 C13 59.7(3) . . . . ?
O5 La1 O4 C13 76.9(3) . . . . ?
N2 La1 O4 C13 -147.3(3) . . . . ?
N1 La1 O4 C13 -154.3(3) . . . . ?
O7 S1 O6 La1 -35.5(4) . . . . ?
O8 S1 O6 La1 -163.2(3) . . . . ?
C15 S1 O6 La1 82.8(4) . . . . ?
O4 La1 O6 S1 -117.9(3) . . . . ?
O2 La1 O6 S1 -65.8(4) 2_665 . . . ?
O3 La1 O6 S1 6.2(3) . . . . ?
O8 La1 O6 S1 151.6(4) 2_566 . . . ?
O1 La1 O6 S1 6.2(4) 2_565 . . . ?
O5 La1 O6 S1 -135.5(4) . . . . ?
N2 La1 O6 S1 81.5(4) . . . . ?
N1 La1 O6 S1 113.4(3) . . . . ?
O7 S1 O8 La1 -105.7(3) . . . 2_566 ?
O6 S1 O8 La1 23.0(4) . . . 2_566 ?
C15 S1 O8 La1 137.4(3) . . . 2_566 ?
O4 La1 N1 C1 2.0(3) . . . . ?
O2 La1 N1 C1 -30.5(3) 2_665 . . . ?
O3 La1 N1 C1 -123.1(3) . . . . ?
O8 La1 N1 C1 111.9(3) 2_566 . . . ?
O1 La1 N1 C1 -78.3(3) 2_565 . . . ?
O6 La1 N1 C1 150.5(3) . . . . ?
O5 La1 N1 C1 60.7(3) . . . . ?
N2 La1 N1 C1 -172.2(3) . . . . ?
O4 La1 N1 C12 -171.3(3) . . . . ?
O2 La1 N1 C12 156.2(2) 2_665 . . . ?
O3 La1 N1 C12 63.6(3) . . . . ?
O8 La1 N1 C12 -61.3(2) 2_566 . . . ?
O1 La1 N1 C12 108.5(3) 2_565 . . . ?
O6 La1 N1 C12 -22.7(3) . . . . ?
O5 La1 N1 C12 -112.5(2) . . . . ?
N2 La1 N1 C12 14.6(2) . . . . ?
O4 La1 N2 C10 171.7(3) . . . . ?
O2 La1 N2 C10 59.0(3) 2_665 . . . ?
O3 La1 N2 C10 43.7(3) . . . . ?
O8 La1 N2 C10 -100.2(3) 2_566 . . . ?
O1 La1 N2 C10 108.5(3) 2_565 . . . ?
O6 La1 N2 C10 -25.3(3) . . . . ?
O5 La1 N2 C10 -77.1(3) . . . . ?
N1 La1 N2 C10 179.5(3) . . . . ?
O4 La1 N2 C11 -24.6(3) . . . . ?
O2 La1 N2 C11 -137.3(2) 2_665 . . . ?
O3 La1 N2 C11 -152.7(3) . . . . ?
O8 La1 N2 C11 63.5(2) 2_566 . . . ?
O1 La1 N2 C11 -87.9(2) 2_565 . . . ?
O6 La1 N2 C11 138.3(3) . . . . ?
O5 La1 N2 C11 86.5(3) . . . . ?
N1 La1 N2 C11 -16.9(2) . . . . ?
C12 N1 C1 C2 2.5(6) . . . . ?
La1 N1 C1 C2 -170.8(3) . . . . ?
N1 C1 C2 C3 1.2(6) . . . . ?
C1 C2 C3 C4 -2.5(6) . . . . ?
C2 C3 C4 C12 0.2(6) . . . . ?
C2 C3 C4 C5 -179.2(4) . . . . ?
C3 C4 C5 C6 178.1(4) . . . . ?
C12 C4 C5 C6 -1.3(6) . . . . ?
C4 C5 C6 C7 -2.1(6) . . . . ?
C5 C6 C7 C8 -175.6(4) . . . . ?
C5 C6 C7 C11 2.7(6) . . . . ?
C11 C7 C8 C9 -0.9(6) . . . . ?
C6 C7 C8 C9 177.4(4) . . . . ?
C7 C8 C9 C10 0.5(6) . . . . ?
C11 N2 C10 C9 -1.6(6) . . . . ?
La1 N2 C10 C9 162.3(3) . . . . ?
C8 C9 C10 N2 0.8(7) . . . . ?
C10 N2 C11 C7 1.1(5) . . . . ?
La1 N2 C11 C7 -162.8(3) . . . . ?
C10 N2 C11 C12 -177.3(3) . . . . ?
La1 N2 C11 C12 18.8(4) . . . . ?
C8 C7 C11 N2 0.1(5) . . . . ?
C6 C7 C11 N2 -178.2(3) . . . . ?
C8 C7 C11 C12 178.5(3) . . . . ?
C6 C7 C11 C12 0.1(5) . . . . ?
C1 N1 C12 C11 174.1(3) . . . . ?
La1 N1 C12 C11 -12.3(4) . . . . ?
C1 N1 C12 C4 -4.8(5) . . . . ?
La1 N1 C12 C4 168.8(3) . . . . ?
N2 C11 C12 N1 -4.0(5) . . . . ?
C7 C11 C12 N1 177.6(3) . . . . ?
N2 C11 C12 C4 175.0(3) . . . . ?
C7 C11 C12 C4 -3.4(5) . . . . ?
C3 C4 C12 N1 3.5(5) . . . . ?
C5 C4 C12 N1 -177.0(4) . . . . ?
C3 C4 C12 C11 -175.4(4) . . . . ?
C5 C4 C12 C11 4.0(5) . . . . ?
La1 O2 C13 O4 -179.1(3) 2_665 . . . ?
La1 O2 C13 C13 0.2(5) 2_665 . . 2_665 ?
La1 O4 C13 O2 -179.6(3) . . . . ?
La1 O4 C13 C13 1.2(5) . . . 2_665 ?
La1 O3 C14 O1 177.7(2) . . . . ?
La1 O3 C14 C14 -1.2(5) . . . 2_565 ?
La1 O1 C14 O3 178.4(2) 2_565 . . . ?
La1 O1 C14 C14 -2.6(5) 2_565 . . 2_565 ?
O7 S1 C15 C16 120.0(3) . . . . ?
O6 S1 C15 C16 -2.1(3) . . . . ?
O8 S1 C15 C16 -120.5(3) . . . . ?
O7 S1 C15 C19 -59.2(3) . . . . ?
O6 S1 C15 C19 178.7(3) . . . . ?
O8 S1 C15 C19 60.4(3) . . . . ?
C19 C15 C16 C17 -0.3(5) . . . . ?
S1 C15 C16 C17 -179.5(3) . . . . ?
C15 C16 C17 C18 1.7(6) . . . . ?
C16 C17 C18 C19 -1.8(6) . . . 2_556 ?
C16 C15 C19 C18 180.0(3) . . . 2_556 ?
S1 C15 C19 C18 -0.9(5) . . . 2_556 ?
C16 C15 C19 C19 -0.9(6) . . . 2_556 ?
S1 C15 C19 C19 178.3(3) . . . 2_556 ?

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        25.25
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         0.534
_refine_diff_density_min         -0.535
_refine_diff_density_rms         0.107
####################################################################### 
# 
# 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_4
_database_code_depnum_ccdc_archive 'CCDC 1475537'
_audit_update_record             
;
2016-04-21 deposited with the CCDC.
2016-06-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C35 H24 La N4 O9 S2'
_chemical_formula_weight         847.61

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.2382(12)
_cell_length_b                   11.7405(11)
_cell_length_c                   14.0474(13)
_cell_angle_alpha                108.240(2)
_cell_angle_beta                 91.419(2)
_cell_angle_gamma                113.675(2)
_cell_volume                     1587.9(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    294(2)
_cell_measurement_reflns_used    1542
_cell_measurement_theta_min      2.01
_cell_measurement_theta_max      25.25

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.773
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             846
_exptl_absorpt_coefficient_mu    1.543
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.7903
_exptl_absorpt_correction_T_max  0.8865
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      294(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'phi and omega scans'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8255
_diffrn_reflns_av_R_equivalents  0.0348
_diffrn_reflns_av_sigmaI/netI    0.0752
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.01
_diffrn_reflns_theta_max         25.25
_reflns_number_total             5682
_reflns_number_gt                4808
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0296P)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         5682
_refine_ls_number_parameters     466
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0507
_refine_ls_R_factor_gt           0.0411
_refine_ls_wR_factor_ref         0.0833
_refine_ls_wR_factor_gt          0.0782
_refine_ls_goodness_of_fit_ref   0.976
_refine_ls_restrained_S_all      0.976
_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
C1 C 0.5750(5) 0.7189(5) 0.1075(4) 0.0330(12) Uani 1 1 d . . .
H1 H 0.5326 0.6332 0.1087 0.040 Uiso 1 1 calc R . .
C2 C 0.4967(5) 0.7798(5) 0.0906(4) 0.0382(13) Uani 1 1 d . . .
H2 H 0.4052 0.7357 0.0802 0.046 Uiso 1 1 calc R . .
C3 C 0.5578(5) 0.9054(5) 0.0899(4) 0.0382(13) Uani 1 1 d . . .
H3 H 0.5076 0.9486 0.0799 0.046 Uiso 1 1 calc R . .
C4 C 0.6955(5) 0.9708(5) 0.1040(3) 0.0296(11) Uani 1 1 d . . .
C5 C 0.7638(6) 1.1010(5) 0.1012(4) 0.0385(13) Uani 1 1 d . . .
H5 H 0.7166 1.1477 0.0930 0.046 Uiso 1 1 calc R . .
C6 C 0.8944(6) 1.1567(5) 0.1102(4) 0.0360(13) Uani 1 1 d . . .
H6 H 0.9372 1.2421 0.1085 0.043 Uiso 1 1 calc R . .
C7 C 0.9706(5) 1.0879(4) 0.1225(3) 0.0290(12) Uani 1 1 d . . .
C8 C 1.1079(5) 1.1421(5) 0.1280(3) 0.0326(12) Uani 1 1 d . . .
H8 H 1.1535 1.2265 0.1252 0.039 Uiso 1 1 calc R . .
C9 C 1.1735(5) 1.0701(5) 0.1375(3) 0.0328(12) Uani 1 1 d . . .
H9 H 1.2642 1.1035 0.1388 0.039 Uiso 1 1 calc R . .
C10 C 1.1039(5) 0.9454(4) 0.1453(3) 0.0277(11) Uani 1 1 d . . .
H10 H 1.1501 0.8975 0.1524 0.033 Uiso 1 1 calc R . .
C11 C 0.9073(5) 0.9609(4) 0.1288(3) 0.0233(10) Uani 1 1 d . . .
C12 C 0.7662(5) 0.9002(4) 0.1182(3) 0.0231(10) Uani 1 1 d . . .
C13 C 0.8338(5) 0.9074(5) 0.3638(4) 0.0405(14) Uani 1 1 d . . .
H13 H 0.8284 0.9369 0.3104 0.049 Uiso 1 1 calc R . .
C14 C 0.8350(6) 0.9870(5) 0.4608(4) 0.0461(15) Uani 1 1 d . . .
H14 H 0.8333 1.0686 0.4713 0.055 Uiso 1 1 calc R . .
C15 C 0.8385(6) 0.9454(6) 0.5405(4) 0.0500(16) Uani 1 1 d . . .
H15 H 0.8365 0.9963 0.6056 0.060 Uiso 1 1 calc R . .
C16 C 0.8451(5) 0.8252(6) 0.5223(4) 0.0422(14) Uani 1 1 d . . .
C17 C 0.8504(6) 0.7744(6) 0.6022(4) 0.0523(17) Uani 1 1 d . . .
H17 H 0.8516 0.8244 0.6685 0.063 Uiso 1 1 calc R . .
C18 C 0.8537(6) 0.6586(6) 0.5838(4) 0.0498(16) Uani 1 1 d . . .
H18 H 0.8585 0.6294 0.6375 0.060 Uiso 1 1 calc R . .
C19 C 0.8500(5) 0.5770(5) 0.4830(4) 0.0354(13) Uani 1 1 d . . .
C20 C 0.8479(5) 0.4511(5) 0.4588(4) 0.0399(14) Uani 1 1 d . . .
H20 H 0.8508 0.4176 0.5102 0.048 Uiso 1 1 calc R . .
C21 C 0.8417(5) 0.3778(5) 0.3617(4) 0.0399(14) Uani 1 1 d . . .
H21 H 0.8392 0.2936 0.3453 0.048 Uiso 1 1 calc R . .
C22 C 0.8393(5) 0.4315(5) 0.2868(4) 0.0319(12) Uani 1 1 d . . .
H22 H 0.8349 0.3806 0.2199 0.038 Uiso 1 1 calc R . .
C23 C 0.8465(4) 0.6227(5) 0.4017(3) 0.0254(11) Uani 1 1 d . . .
C24 C 0.8440(5) 0.7481(5) 0.4222(3) 0.0285(11) Uani 1 1 d . . .
C25 C 0.5042(5) 0.5751(5) 0.3507(4) 0.0398(14) Uani 1 1 d . . .
H25 H 0.5038 0.6200 0.3067 0.048 Uiso 1 1 calc R . .
C26 C 0.5107(5) 0.4528(5) 0.3139(3) 0.0260(11) Uani 1 1 d . . .
C27 C 0.5090(5) 0.3853(5) 0.3770(4) 0.0307(12) Uani 1 1 d . . .
H27 H 0.5124 0.3036 0.3515 0.037 Uiso 1 1 calc R . .
C28 C 0.5020(5) 0.4375(4) 0.4813(3) 0.0282(11) Uani 1 1 d . . .
C29 C 0.5015(5) 0.3715(5) 0.5498(4) 0.0394(14) Uani 1 1 d . . .
H29 H 0.5051 0.2898 0.5263 0.047 Uiso 1 1 calc R . .
C30 C 1.3487(5) 0.8402(4) 0.4514(3) 0.0267(11) Uani 1 1 d . . .
H30 H 1.2953 0.7741 0.4747 0.032 Uiso 1 1 calc R . .
C31 C 1.3186(4) 0.8292(4) 0.3539(3) 0.0241(11) Uani 1 1 d . . .
C32 C 1.3972(5) 0.9283(5) 0.3177(3) 0.0317(12) Uani 1 1 d . . .
H32 H 1.3753 0.9209 0.2510 0.038 Uiso 1 1 calc R . .
C33 C 1.5051(5) 1.0352(5) 0.3793(4) 0.0329(12) Uani 1 1 d . . .
H33 H 1.5569 1.1000 0.3542 0.039 Uiso 1 1 calc R . .
C34 C 1.5401(5) 1.0495(4) 0.4818(3) 0.0265(11) Uani 1 1 d . . .
C35 C 0.9628(4) 0.4367(4) 0.0123(3) 0.0233(11) Uani 1 1 d . . .
La1 La 0.85054(3) 0.64306(2) 0.150997(19) 0.01808(9) Uani 1 1 d . . .
N1 N 0.7056(4) 0.7746(4) 0.1220(3) 0.0258(9) Uani 1 1 d . . .
N2 N 0.9745(4) 0.8925(3) 0.1429(3) 0.0236(9) Uani 1 1 d . . .
N3 N 0.8400(4) 0.7928(4) 0.3428(3) 0.0265(9) Uani 1 1 d . . .
N4 N 0.8429(4) 0.5497(4) 0.3046(3) 0.0246(9) Uani 1 1 d . . .
O1 O 0.6203(3) 0.4939(3) 0.1608(2) 0.0328(8) Uani 1 1 d . . .
O2 O 0.5454(4) 0.2728(3) 0.1701(2) 0.0386(9) Uani 1 1 d . . .
O3 O 0.3899(3) 0.3511(3) 0.1287(2) 0.0376(9) Uani 1 1 d . . .
O4 O 1.0820(3) 0.7381(3) 0.2566(2) 0.0283(8) Uani 1 1 d . . .
O5 O 1.1371(3) 0.5946(3) 0.3234(3) 0.0412(9) Uani 1 1 d . . .
O6 O 1.2256(3) 0.6445(3) 0.1782(2) 0.0398(9) Uani 1 1 d . . .
O7 O 0.8812(3) 0.4399(3) 0.0725(2) 0.0305(8) Uani 1 1 d . . .
O8 O 0.9866(3) 0.3406(3) -0.0299(2) 0.0275(8) Uani 1 1 d . . .
O9 O 0.7300(4) 0.5478(4) -0.0334(2) 0.0363(9) Uani 1 1 d D . .
H9A H 0.687(5) 0.578(5) -0.060(3) 0.055 Uiso 1 1 d D . .
H9B H 0.752(5) 0.582(5) 0.0283(15) 0.055 Uiso 1 1 d D . .
S1 S 0.51770(11) 0.38514(12) 0.18298(9) 0.0261(3) Uani 1 1 d . . .
S2 S 1.17910(12) 0.68784(11) 0.27145(9) 0.0263(3) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.325(6) . ?
C1 C2 1.394(7) . ?
C1 H1 0.9300 . ?
C2 C3 1.358(7) . ?
C2 H2 0.9300 . ?
C3 C4 1.399(7) . ?
C3 H3 0.9300 . ?
C4 C12 1.409(6) . ?
C4 C5 1.422(6) . ?
C5 C6 1.329(7) . ?
C5 H5 0.9300 . ?
C6 C7 1.431(7) . ?
C6 H6 0.9300 . ?
C7 C8 1.402(7) . ?
C7 C11 1.404(6) . ?
C8 C9 1.358(7) . ?
C8 H8 0.9300 . ?
C9 C10 1.397(6) . ?
C9 H9 0.9300 . ?
C10 N2 1.327(6) . ?
C10 H10 0.9300 . ?
C11 N2 1.354(6) . ?
C11 C12 1.434(6) . ?
C12 N1 1.373(5) . ?
C13 N3 1.315(6) . ?
C13 C14 1.386(7) . ?
C13 H13 0.9300 . ?
C14 C15 1.360(7) . ?
C14 H14 0.9300 . ?
C15 C16 1.386(8) . ?
C15 H15 0.9300 . ?
C16 C24 1.411(6) . ?
C16 C17 1.436(7) . ?
C17 C18 1.318(8) . ?
C17 H17 0.9300 . ?
C18 C19 1.428(7) . ?
C18 H18 0.9300 . ?
C19 C20 1.400(7) . ?
C19 C23 1.410(6) . ?
C20 C21 1.348(7) . ?
C20 H20 0.9300 . ?
C21 C22 1.390(6) . ?
C21 H21 0.9300 . ?
C22 N4 1.315(6) . ?
C22 H22 0.9300 . ?
C23 N4 1.354(5) . ?
C23 C24 1.422(6) . ?
C24 N3 1.379(6) . ?
C25 C29 1.356(7) 2_666 ?
C25 C26 1.398(7) . ?
C25 H25 0.9300 . ?
C26 C27 1.358(6) . ?
C26 S1 1.778(5) . ?
C27 C28 1.417(6) . ?
C27 H27 0.9300 . ?
C28 C29 1.411(6) . ?
C28 C28 1.415(9) 2_666 ?
C29 C25 1.356(7) 2_666 ?
C29 H29 0.9300 . ?
C30 C31 1.355(6) . ?
C30 C34 1.415(6) 2_876 ?
C30 H30 0.9300 . ?
C31 C32 1.400(6) . ?
C31 S2 1.781(4) . ?
C32 C33 1.356(6) . ?
C32 H32 0.9300 . ?
C33 C34 1.422(6) . ?
C33 H33 0.9300 . ?
C34 C34 1.406(9) 2_876 ?
C34 C30 1.415(6) 2_876 ?
C35 O8 1.236(5) . ?
C35 O7 1.265(5) . ?
C35 C35 1.539(8) 2_765 ?
La1 O7 2.461(3) . ?
La1 O1 2.512(3) . ?
La1 O8 2.521(3) 2_765 ?
La1 O9 2.567(3) . ?
La1 O4 2.579(3) . ?
La1 N4 2.698(3) . ?
La1 N2 2.733(3) . ?
La1 N1 2.754(4) . ?
La1 N3 2.754(4) . ?
La1 H9B 1.79(2) . ?
O1 S1 1.464(3) . ?
O2 S1 1.433(3) . ?
O3 S1 1.448(3) . ?
O4 S2 1.472(3) . ?
O5 S2 1.434(3) . ?
O6 S2 1.441(3) . ?
O8 La1 2.521(3) 2_765 ?
O9 H9A 0.841(19) . ?
O9 H9B 0.815(19) . ?

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
N1 C1 C2 124.5(5) . . ?
N1 C1 H1 117.7 . . ?
C2 C1 H1 117.7 . . ?
C3 C2 C1 118.2(5) . . ?
C3 C2 H2 120.9 . . ?
C1 C2 H2 120.9 . . ?
C2 C3 C4 120.8(5) . . ?
C2 C3 H3 119.6 . . ?
C4 C3 H3 119.6 . . ?
C3 C4 C12 117.0(4) . . ?
C3 C4 C5 122.9(5) . . ?
C12 C4 C5 120.1(5) . . ?
C6 C5 C4 120.7(5) . . ?
C6 C5 H5 119.6 . . ?
C4 C5 H5 119.6 . . ?
C5 C6 C7 121.3(5) . . ?
C5 C6 H6 119.3 . . ?
C7 C6 H6 119.3 . . ?
C8 C7 C11 117.7(5) . . ?
C8 C7 C6 122.5(4) . . ?
C11 C7 C6 119.7(5) . . ?
C9 C8 C7 119.4(4) . . ?
C9 C8 H8 120.3 . . ?
C7 C8 H8 120.3 . . ?
C8 C9 C10 119.4(5) . . ?
C8 C9 H9 120.3 . . ?
C10 C9 H9 120.3 . . ?
N2 C10 C9 122.8(5) . . ?
N2 C10 H10 118.6 . . ?
C9 C10 H10 118.6 . . ?
N2 C11 C7 122.3(4) . . ?
N2 C11 C12 118.7(4) . . ?
C7 C11 C12 119.0(4) . . ?
N1 C12 C4 122.6(4) . . ?
N1 C12 C11 118.3(4) . . ?
C4 C12 C11 119.1(4) . . ?
N3 C13 C14 124.0(5) . . ?
N3 C13 H13 118.0 . . ?
C14 C13 H13 118.0 . . ?
C15 C14 C13 119.7(5) . . ?
C15 C14 H14 120.1 . . ?
C13 C14 H14 120.1 . . ?
C14 C15 C16 118.4(5) . . ?
C14 C15 H15 120.8 . . ?
C16 C15 H15 120.8 . . ?
C15 C16 C24 119.5(5) . . ?
C15 C16 C17 122.1(5) . . ?
C24 C16 C17 118.4(5) . . ?
C18 C17 C16 121.7(5) . . ?
C18 C17 H17 119.2 . . ?
C16 C17 H17 119.2 . . ?
C17 C18 C19 121.3(5) . . ?
C17 C18 H18 119.3 . . ?
C19 C18 H18 119.3 . . ?
C20 C19 C23 116.9(5) . . ?
C20 C19 C18 123.6(5) . . ?
C23 C19 C18 119.5(5) . . ?
C21 C20 C19 120.7(5) . . ?
C21 C20 H20 119.6 . . ?
C19 C20 H20 119.6 . . ?
C20 C21 C22 118.2(5) . . ?
C20 C21 H21 120.9 . . ?
C22 C21 H21 120.9 . . ?
N4 C22 C21 124.1(5) . . ?
N4 C22 H22 118.0 . . ?
C21 C22 H22 118.0 . . ?
N4 C23 C19 122.1(4) . . ?
N4 C23 C24 119.0(4) . . ?
C19 C23 C24 118.9(4) . . ?
N3 C24 C16 120.7(5) . . ?
N3 C24 C23 119.1(4) . . ?
C16 C24 C23 120.2(4) . . ?
C29 C25 C26 120.3(5) 2_666 . ?
C29 C25 H25 119.9 2_666 . ?
C26 C25 H25 119.9 . . ?
C27 C26 C25 120.3(4) . . ?
C27 C26 S1 120.4(4) . . ?
C25 C26 S1 119.3(4) . . ?
C26 C27 C28 121.0(4) . . ?
C26 C27 H27 119.5 . . ?
C28 C27 H27 119.5 . . ?
C29 C28 C28 118.5(5) . 2_666 ?
C29 C28 C27 122.9(4) . . ?
C28 C28 C27 118.6(5) 2_666 . ?
C25 C29 C28 121.3(5) 2_666 . ?
C25 C29 H29 119.4 2_666 . ?
C28 C29 H29 119.4 . . ?
C31 C30 C34 121.1(4) . 2_876 ?
C31 C30 H30 119.4 . . ?
C34 C30 H30 119.4 2_876 . ?
C30 C31 C32 120.2(4) . . ?
C30 C31 S2 119.9(4) . . ?
C32 C31 S2 119.9(3) . . ?
C33 C32 C31 120.3(4) . . ?
C33 C32 H32 119.8 . . ?
C31 C32 H32 119.8 . . ?
C32 C33 C34 120.9(4) . . ?
C32 C33 H33 119.5 . . ?
C34 C33 H33 119.5 . . ?
C34 C34 C30 118.9(5) 2_876 2_876 ?
C34 C34 C33 118.5(5) 2_876 . ?
C30 C34 C33 122.6(4) 2_876 . ?
O8 C35 O7 126.1(4) . . ?
O8 C35 C35 116.8(5) . 2_765 ?
O7 C35 C35 117.0(5) . 2_765 ?
O7 La1 O1 87.01(11) . . ?
O7 La1 O8 64.84(9) . 2_765 ?
O1 La1 O8 140.32(10) . 2_765 ?
O7 La1 O9 75.51(11) . . ?
O1 La1 O9 76.91(11) . . ?
O8 La1 O9 69.57(11) 2_765 . ?
O7 La1 O4 85.61(11) . . ?
O1 La1 O4 135.77(10) . . ?
O8 La1 O4 72.29(10) 2_765 . ?
O9 La1 O4 141.71(11) . . ?
O7 La1 N4 77.09(11) . . ?
O1 La1 N4 67.38(11) . . ?
O8 La1 N4 126.44(11) 2_765 . ?
O9 La1 N4 135.60(12) . . ?
O4 La1 N4 68.45(10) . . ?
O7 La1 N2 131.83(10) . . ?
O1 La1 N2 135.84(11) . . ?
O8 La1 N2 67.17(10) 2_765 . ?
O9 La1 N2 91.87(11) . . ?
O4 La1 N2 76.24(10) . . ?
N4 La1 N2 132.18(11) . . ?
O7 La1 N1 142.54(11) . . ?
O1 La1 N1 76.59(11) . . ?
O8 La1 N1 108.51(10) 2_765 . ?
O9 La1 N1 68.11(11) . . ?
O4 La1 N1 129.20(10) . . ?
N4 La1 N1 124.34(11) . . ?
N2 La1 N1 59.77(11) . . ?
O7 La1 N3 137.18(10) . . ?
O1 La1 N3 82.40(11) . . ?
O8 La1 N3 137.26(11) 2_765 . ?
O9 La1 N3 140.19(11) . . ?
O4 La1 N3 74.14(11) . . ?
N4 La1 N3 60.52(11) . . ?
N2 La1 N3 79.80(11) . . ?
N1 La1 N3 74.23(11) . . ?
O7 La1 H9B 80.5(14) . . ?
O1 La1 H9B 72.6(17) . . ?
O8 La1 H9B 75.5(17) 2_765 . ?
O9 La1 H9B 6.6(16) . . ?
O4 La1 H9B 147.7(17) . . ?
N4 La1 H9B 134.7(17) . . ?
N2 La1 H9B 91.6(16) . . ?
N1 La1 H9B 62.6(14) . . ?
N3 La1 H9B 133.7(15) . . ?
C1 N1 C12 116.8(4) . . ?
C1 N1 La1 122.1(3) . . ?
C12 N1 La1 121.0(3) . . ?
C10 N2 C11 118.2(4) . . ?
C10 N2 La1 119.4(3) . . ?
C11 N2 La1 122.3(3) . . ?
C13 N3 C24 117.5(4) . . ?
C13 N3 La1 123.3(3) . . ?
C24 N3 La1 119.1(3) . . ?
C22 N4 C23 118.0(4) . . ?
C22 N4 La1 119.9(3) . . ?
C23 N4 La1 122.1(3) . . ?
S1 O1 La1 156.6(2) . . ?
S2 O4 La1 136.74(18) . . ?
C35 O7 La1 121.1(3) . . ?
C35 O8 La1 120.2(3) . 2_765 ?
La1 O9 H9A 128(3) . . ?
La1 O9 H9B 15(4) . . ?
H9A O9 H9B 116(3) . . ?
O2 S1 O3 113.6(2) . . ?
O2 S1 O1 114.4(2) . . ?
O3 S1 O1 110.13(19) . . ?
O2 S1 C26 107.3(2) . . ?
O3 S1 C26 105.3(2) . . ?
O1 S1 C26 105.3(2) . . ?
O5 S2 O6 114.9(2) . . ?
O5 S2 O4 113.4(2) . . ?
O6 S2 O4 111.19(19) . . ?
O5 S2 C31 106.0(2) . . ?
O6 S2 C31 105.1(2) . . ?
O4 S2 C31 105.1(2) . . ?

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        25.25
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         0.635
_refine_diff_density_min         -0.620
_refine_diff_density_rms         0.115
####################################################################### 
# 
# 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_5
_database_code_depnum_ccdc_archive 'CCDC 1475538'
_audit_update_record             
;
2016-04-21 deposited with the CCDC.
2016-06-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C19 H11 Eu N2 O8 S'
_chemical_formula_weight         579.32

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   P2(1)/c

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                   10.5998(11)
_cell_length_b                   8.9530(9)
_cell_length_c                   20.265(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.979(2)
_cell_angle_gamma                90.00
_cell_volume                     1922.9(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1537
_cell_measurement_theta_min      2.49
_cell_measurement_theta_max      25.25

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.001
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1128
_exptl_absorpt_coefficient_mu    3.423
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.7259
_exptl_absorpt_correction_T_max  0.8752
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'phi and omega scans'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9417
_diffrn_reflns_av_R_equivalents  0.0805
_diffrn_reflns_av_sigmaI/netI    0.0976
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.49
_diffrn_reflns_theta_max         25.25
_reflns_number_total             3472
_reflns_number_gt                2015
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0309P)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         3472
_refine_ls_number_parameters     280
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0950
_refine_ls_R_factor_gt           0.0462
_refine_ls_wR_factor_ref         0.1026
_refine_ls_wR_factor_gt          0.0850
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_restrained_S_all      0.978
_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
C1 C 0.6214(9) 0.8275(11) 0.5343(5) 0.031(2) Uani 1 1 d . . .
H1 H 0.6089 0.9225 0.5516 0.037 Uiso 1 1 calc R . .
C2 C 0.6109(9) 0.8096(11) 0.4671(5) 0.031(3) Uani 1 1 d . . .
H2 H 0.5916 0.8907 0.4401 0.038 Uiso 1 1 calc R . .
C3 C 0.6292(9) 0.6704(12) 0.4404(4) 0.033(2) Uani 1 1 d . . .
H3 H 0.6244 0.6565 0.3949 0.040 Uiso 1 1 calc R . .
C4 C 0.6548(8) 0.5506(10) 0.4821(4) 0.026(2) Uani 1 1 d . . .
C5 C 0.6752(9) 0.4038(11) 0.4569(5) 0.036(3) Uani 1 1 d . . .
H5 H 0.6676 0.3857 0.4118 0.043 Uiso 1 1 calc R . .
C6 C 0.7054(9) 0.2916(10) 0.4986(5) 0.033(3) Uani 1 1 d . . .
H6 H 0.7148 0.1956 0.4818 0.039 Uiso 1 1 calc R . .
C7 C 0.7235(9) 0.3162(10) 0.5680(4) 0.028(2) Uani 1 1 d . . .
C8 C 0.7615(9) 0.2017(9) 0.6119(5) 0.029(2) Uani 1 1 d . . .
H8 H 0.7754 0.1054 0.5965 0.034 Uiso 1 1 calc R . .
C9 C 0.7773(8) 0.2335(10) 0.6763(5) 0.033(2) Uani 1 1 d . . .
H9 H 0.8051 0.1606 0.7058 0.039 Uiso 1 1 calc R . .
C10 C 0.7511(9) 0.3792(10) 0.6982(5) 0.036(3) Uani 1 1 d . . .
H10 H 0.7575 0.3986 0.7432 0.043 Uiso 1 1 calc R . .
C11 C 0.7022(8) 0.4585(10) 0.5938(4) 0.021(2) Uani 1 1 d . . .
C12 C 0.6659(8) 0.5794(11) 0.5497(4) 0.026(2) Uani 1 1 d . . .
C13 C 1.0193(10) 0.5678(15) 0.5917(7) 0.066(4) Uani 1 1 d . . .
H13 H 1.0398 0.5325 0.6337 0.079 Uiso 1 1 calc R . .
C14 C 0.9898(9) 0.7123(11) 0.5793(5) 0.037(3) Uani 1 1 d . . .
C15 C 0.9593(11) 0.7644(16) 0.5157(6) 0.069(4) Uani 1 1 d . . .
H15 H 0.9397 0.8651 0.5107 0.083 Uiso 1 1 calc R . .
C16 C 0.9567(11) 0.6732(16) 0.4586(7) 0.072(4) Uani 1 1 d . . .
H16 H 0.9375 0.7092 0.4166 0.086 Uiso 1 1 calc R . .
C17 C 0.9838(9) 0.5342(13) 0.4707(5) 0.041(3) Uani 1 1 d . . .
C18 C 0.5659(8) 1.0436(10) 0.7733(4) 0.023(2) Uani 1 1 d . . .
C19 C 0.4946(9) 1.0368(10) 0.7069(4) 0.024(2) Uani 1 1 d . . .
Eu1 Eu 0.67045(4) 0.75090(6) 0.702475(19) 0.02039(14) Uani 1 1 d . . .
N1 N 0.6486(7) 0.7167(7) 0.5764(3) 0.0222(19) Uani 1 1 d . . .
N2 N 0.7182(7) 0.4887(8) 0.6591(3) 0.0254(19) Uani 1 1 d . . .
O1 O 1.0492(6) 0.7778(7) 0.7005(3) 0.0438(19) Uani 1 1 d . . .
O2 O 1.0459(6) 0.9789(7) 0.6221(3) 0.0428(19) Uani 1 1 d . . .
O3 O 0.8505(6) 0.8646(6) 0.6564(3) 0.0273(15) Uani 1 1 d . . .
O4 O 0.4006(7) 1.1195(7) 0.7012(3) 0.0363(18) Uani 1 1 d . . .
O5 O 0.5348(6) 0.9474(7) 0.6644(3) 0.0308(16) Uani 1 1 d . . .
O6 O 0.6548(6) 0.9496(7) 0.7804(3) 0.0331(16) Uani 1 1 d . . .
O7 O 0.5321(6) 1.1380(7) 0.8135(3) 0.0333(16) Uani 1 1 d . . .
O8 O 0.8512(6) 0.6847(7) 0.7748(3) 0.0351(17) Uani 1 1 d . . .
S3 S 0.9867(2) 0.8442(3) 0.64455(13) 0.0292(6) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.335(10) . ?
C1 C2 1.374(12) . ?
C1 H1 0.9300 . ?
C2 C3 1.374(12) . ?
C2 H2 0.9300 . ?
C3 C4 1.390(12) . ?
C3 H3 0.9300 . ?
C4 C12 1.396(12) . ?
C4 C5 1.428(12) . ?
C5 C6 1.348(12) . ?
C5 H5 0.9300 . ?
C6 C7 1.434(12) . ?
C6 H6 0.9300 . ?
C7 C11 1.397(11) . ?
C7 C8 1.412(12) . ?
C8 C9 1.343(12) . ?
C8 H8 0.9300 . ?
C9 C10 1.408(12) . ?
C9 H9 0.9300 . ?
C10 N2 1.304(10) . ?
C10 H10 0.9300 . ?
C11 N2 1.358(10) . ?
C11 C12 1.451(12) . ?
C12 N1 1.357(10) . ?
C13 C14 1.353(14) . ?
C13 C17 1.559(16) 3_766 ?
C13 H13 0.9300 . ?
C14 C15 1.405(15) . ?
C14 S3 1.773(10) . ?
C15 C16 1.415(15) . ?
C15 H15 0.9300 . ?
C16 C17 1.299(15) . ?
C16 H16 0.9300 . ?
C17 C17 1.37(2) 3_766 ?
C17 C13 1.559(16) 3_766 ?
C18 O7 1.232(10) . ?
C18 O6 1.269(10) . ?
C18 C19 1.534(12) . ?
C18 Eu1 3.163(9) 2_656 ?
C18 Eu1 3.195(9) . ?
C19 O4 1.245(10) . ?
C19 O5 1.255(9) . ?
C19 Eu1 3.168(9) . ?
C19 Eu1 3.197(9) 2_656 ?
Eu1 O3 2.369(6) . ?
Eu1 O6 2.387(6) . ?
Eu1 O7 2.390(6) 2_646 ?
Eu1 O5 2.391(6) . ?
Eu1 O4 2.411(6) 2_646 ?
Eu1 O8 2.464(6) . ?
Eu1 N2 2.561(7) . ?
Eu1 N1 2.581(7) . ?
Eu1 C18 3.163(9) 2_646 ?
Eu1 C19 3.197(9) 2_646 ?
O1 S3 1.433(7) . ?
O2 S3 1.438(6) . ?
O3 S3 1.479(6) . ?
O4 Eu1 2.411(6) 2_656 ?
O7 Eu1 2.390(6) 2_656 ?

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
N1 C1 C2 123.9(9) . . ?
N1 C1 H1 118.0 . . ?
C2 C1 H1 118.0 . . ?
C3 C2 C1 119.2(9) . . ?
C3 C2 H2 120.4 . . ?
C1 C2 H2 120.4 . . ?
C2 C3 C4 119.2(8) . . ?
C2 C3 H3 120.4 . . ?
C4 C3 H3 120.4 . . ?
C3 C4 C12 117.8(9) . . ?
C3 C4 C5 121.4(9) . . ?
C12 C4 C5 120.7(9) . . ?
C6 C5 C4 119.8(9) . . ?
C6 C5 H5 120.1 . . ?
C4 C5 H5 120.1 . . ?
C5 C6 C7 121.8(9) . . ?
C5 C6 H6 119.1 . . ?
C7 C6 H6 119.1 . . ?
C11 C7 C8 118.2(8) . . ?
C11 C7 C6 119.1(9) . . ?
C8 C7 C6 122.6(9) . . ?
C9 C8 C7 119.2(8) . . ?
C9 C8 H8 120.4 . . ?
C7 C8 H8 120.4 . . ?
C8 C9 C10 118.7(9) . . ?
C8 C9 H9 120.7 . . ?
C10 C9 H9 120.7 . . ?
N2 C10 C9 123.9(9) . . ?
N2 C10 H10 118.1 . . ?
C9 C10 H10 118.1 . . ?
N2 C11 C7 121.8(8) . . ?
N2 C11 C12 118.6(8) . . ?
C7 C11 C12 119.5(8) . . ?
N1 C12 C4 123.2(9) . . ?
N1 C12 C11 117.8(8) . . ?
C4 C12 C11 118.9(8) . . ?
C14 C13 C17 114.1(12) . 3_766 ?
C14 C13 H13 122.9 . . ?
C17 C13 H13 122.9 3_766 . ?
C13 C14 C15 122.4(11) . . ?
C13 C14 S3 120.4(10) . . ?
C15 C14 S3 117.2(9) . . ?
C14 C15 C16 124.0(14) . . ?
C14 C15 H15 118.0 . . ?
C16 C15 H15 118.0 . . ?
C17 C16 C15 113.4(14) . . ?
C17 C16 H16 123.3 . . ?
C15 C16 H16 123.3 . . ?
C16 C17 C17 129.8(16) . 3_766 ?
C16 C17 C13 114.0(11) . 3_766 ?
C17 C17 C13 116.2(14) 3_766 3_766 ?
O7 C18 O6 127.1(9) . . ?
O7 C18 C19 117.6(8) . . ?
O6 C18 C19 115.3(8) . . ?
O7 C18 Eu1 41.8(4) . 2_656 ?
O6 C18 Eu1 163.6(6) . 2_656 ?
C19 C18 Eu1 77.3(5) . 2_656 ?
O7 C18 Eu1 165.3(7) . . ?
O6 C18 Eu1 41.0(4) . . ?
C19 C18 Eu1 75.1(5) . . ?
Eu1 C18 Eu1 146.4(3) 2_656 . ?
O4 C19 O5 126.7(9) . . ?
O4 C19 C18 116.0(8) . . ?
O5 C19 C18 117.3(8) . . ?
O4 C19 Eu1 161.5(7) . . ?
O5 C19 Eu1 42.1(4) . . ?
C18 C19 Eu1 77.0(5) . . ?
O4 C19 Eu1 41.5(4) . 2_656 ?
O5 C19 Eu1 166.4(7) . 2_656 ?
C18 C19 Eu1 74.8(5) . 2_656 ?
Eu1 C19 Eu1 145.9(3) . 2_656 ?
O3 Eu1 O6 90.3(2) . . ?
O3 Eu1 O7 148.9(2) . 2_646 ?
O6 Eu1 O7 109.4(2) . 2_646 ?
O3 Eu1 O5 92.3(2) . . ?
O6 Eu1 O5 67.5(2) . . ?
O7 Eu1 O5 74.5(2) 2_646 . ?
O3 Eu1 O4 142.5(2) . 2_646 ?
O6 Eu1 O4 78.6(2) . 2_646 ?
O7 Eu1 O4 67.1(2) 2_646 2_646 ?
O5 Eu1 O4 115.2(2) . 2_646 ?
O3 Eu1 O8 73.4(2) . . ?
O6 Eu1 O8 81.3(2) . . ?
O7 Eu1 O8 131.8(2) 2_646 . ?
O5 Eu1 O8 145.7(2) . . ?
O4 Eu1 O8 69.6(2) 2_646 . ?
O3 Eu1 N2 95.4(2) . . ?
O6 Eu1 N2 158.0(2) . . ?
O7 Eu1 N2 75.4(2) 2_646 . ?
O5 Eu1 N2 133.2(2) . . ?
O4 Eu1 N2 84.1(2) 2_646 . ?
O8 Eu1 N2 80.1(2) . . ?
O3 Eu1 N1 73.8(2) . . ?
O6 Eu1 N1 137.5(2) . . ?
O7 Eu1 N1 75.6(2) 2_646 . ?
O5 Eu1 N1 74.0(2) . . ?
O4 Eu1 N1 136.1(2) 2_646 . ?
O8 Eu1 N1 128.0(2) . . ?
N2 Eu1 N1 64.3(2) . . ?
O3 Eu1 C18 163.6(2) . 2_646 ?
O6 Eu1 C18 105.7(2) . 2_646 ?
O7 Eu1 C18 20.1(2) 2_646 2_646 ?
O5 Eu1 C18 90.5(2) . 2_646 ?
O4 Eu1 C18 47.8(2) 2_646 2_646 ?
O8 Eu1 C18 112.1(2) . 2_646 ?
N2 Eu1 C18 71.2(2) . 2_646 ?
N1 Eu1 C18 91.5(2) . 2_646 ?
O3 Eu1 C19 98.2(2) . . ?
O6 Eu1 C19 48.1(2) . . ?
O7 Eu1 C19 79.5(2) 2_646 . ?
O5 Eu1 C19 20.6(2) . . ?
O4 Eu1 C19 100.3(2) 2_646 . ?
O8 Eu1 C19 129.0(2) . . ?
N2 Eu1 C19 150.5(2) . . ?
N1 Eu1 C19 94.6(2) . . ?
C18 Eu1 C19 90.1(2) 2_646 . ?
O3 Eu1 C18 96.4(2) . . ?
O6 Eu1 C18 20.4(2) . . ?
O7 Eu1 C18 95.1(2) 2_646 . ?
O5 Eu1 C18 48.0(2) . . ?
O4 Eu1 C18 85.5(2) 2_646 . ?
O8 Eu1 C18 101.7(2) . . ?
N2 Eu1 C18 168.1(2) . . ?
N1 Eu1 C18 121.1(2) . . ?
C18 Eu1 C18 97.46(9) 2_646 . ?
C19 Eu1 C18 27.9(2) . . ?
O3 Eu1 C19 159.5(2) . 2_646 ?
O6 Eu1 C19 91.2(2) . 2_646 ?
O7 Eu1 C19 47.5(2) 2_646 2_646 ?
O5 Eu1 C19 107.1(2) . 2_646 ?
O4 Eu1 C19 20.0(2) 2_646 2_646 ?
O8 Eu1 C19 86.7(2) . 2_646 ?
N2 Eu1 C19 76.2(2) . 2_646 ?
N1 Eu1 C19 117.2(2) . 2_646 ?
C18 Eu1 C19 27.9(2) 2_646 2_646 ?
C19 Eu1 C19 98.07(8) . 2_646 ?
C18 Eu1 C19 92.1(2) . 2_646 ?
C1 N1 C12 116.6(8) . . ?
C1 N1 Eu1 123.9(6) . . ?
C12 N1 Eu1 119.4(5) . . ?
C10 N2 C11 118.1(8) . . ?
C10 N2 Eu1 122.2(6) . . ?
C11 N2 Eu1 119.7(6) . . ?
S3 O3 Eu1 143.7(4) . . ?
C19 O4 Eu1 118.4(6) . 2_656 ?
C19 O5 Eu1 117.2(6) . . ?
C18 O6 Eu1 118.6(6) . . ?
C18 O7 Eu1 118.1(6) . 2_656 ?
O1 S3 O2 113.6(4) . . ?
O1 S3 O3 111.2(4) . . ?
O2 S3 O3 112.4(4) . . ?
O1 S3 C14 107.4(5) . . ?
O2 S3 C14 108.0(4) . . ?
O3 S3 C14 103.5(4) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.25
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         1.498
_refine_diff_density_min         -0.735
_refine_diff_density_rms         0.165
####################################################################### 
# 
# 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
_database_code_depnum_ccdc_archive 'CCDC 1475539'
_audit_update_record             
;
2016-04-21 deposited with the CCDC.
2016-06-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C19 H13 Gd N2 O8 S'
_chemical_formula_weight         586.62

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'
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   P2(1)/c

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                   10.5700(10)
_cell_length_b                   8.9400(9)
_cell_length_c                   20.224(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.868(2)
_cell_angle_gamma                90.00
_cell_volume                     1910.9(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    3023
_cell_measurement_theta_min      2.01
_cell_measurement_theta_max      25.01

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.039
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1140
_exptl_absorpt_coefficient_mu    3.633
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.7259
_exptl_absorpt_correction_T_max  0.8752
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'phi and omega scans'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9131
_diffrn_reflns_av_R_equivalents  0.0583
_diffrn_reflns_av_sigmaI/netI    0.0730
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.01
_diffrn_reflns_theta_max         25.01
_reflns_number_total             3378
_reflns_number_gt                2089
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0273P)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         3378
_refine_ls_number_parameters     280
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0778
_refine_ls_R_factor_gt           0.0381
_refine_ls_wR_factor_ref         0.0839
_refine_ls_wR_factor_gt          0.0713
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_restrained_S_all      1.000
_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 0.83028(3) 0.25073(5) -0.202549(16) 0.02021(12) Uani 1 1 d . . .
S1 S 0.51436(19) 0.3446(2) -0.14449(10) 0.0285(5) Uani 1 1 d . . .
O1 O 0.6507(4) 0.3657(5) -0.1571(2) 0.0243(12) Uani 1 1 d . . .
O2 O 0.4529(5) 0.2768(7) -0.2008(3) 0.0473(17) Uani 1 1 d . . .
O3 O 0.4561(5) 0.4788(6) -0.1220(3) 0.0435(16) Uani 1 1 d . . .
O4 O 1.0330(4) 0.1380(6) -0.1866(2) 0.0321(13) Uani 1 1 d . . .
O1W O 0.6518(5) 0.1860(6) -0.2733(3) 0.0382(15) Uani 1 1 d . . .
O5 O 0.8448(5) 0.4482(6) -0.2810(2) 0.0286(13) Uani 1 1 d . . .
O6 O 0.9649(5) 0.4478(6) -0.1644(2) 0.0317(13) Uani 1 1 d . . .
O7 O 1.0999(5) 0.6202(6) -0.2011(2) 0.0306(13) Uani 1 1 d . . .
N1 N 0.7824(5) -0.0102(7) -0.1596(3) 0.0269(15) Uani 1 1 d . . .
N2 N 0.8516(5) 0.2165(6) -0.0769(3) 0.0240(16) Uani 1 1 d . . .
C1 C 0.7477(7) -0.1219(8) -0.2000(4) 0.032(2) Uani 1 1 d . . .
H1A H 0.7388 -0.1023 -0.2450 0.038 Uiso 1 1 calc R . .
C2 C 0.7246(7) -0.2663(9) -0.1775(4) 0.036(2) Uani 1 1 d . . .
H2A H 0.6999 -0.3412 -0.2069 0.043 Uiso 1 1 calc R . .
C3 C 0.7387(7) -0.2962(8) -0.1119(4) 0.033(2) Uani 1 1 d . . .
H3A H 0.7219 -0.3918 -0.0962 0.040 Uiso 1 1 calc R . .
C4 C 0.7779(7) -0.1853(8) -0.0680(4) 0.0263(18) Uani 1 1 d . . .
C5 C 0.7947(7) -0.2082(8) 0.0010(4) 0.033(2) Uani 1 1 d . . .
H5A H 0.7842 -0.3038 0.0181 0.040 Uiso 1 1 calc R . .
C6 C 0.8255(7) -0.0958(9) 0.0422(4) 0.034(2) Uani 1 1 d . . .
H6A H 0.8344 -0.1143 0.0873 0.040 Uiso 1 1 calc R . .
C7 C 0.8446(7) 0.0513(9) 0.0175(4) 0.0278(19) Uani 1 1 d . . .
C8 C 0.8719(7) 0.1725(10) 0.0587(4) 0.032(2) Uani 1 1 d . . .
H8A H 0.8784 0.1588 0.1042 0.038 Uiso 1 1 calc R . .
C9 C 0.8891(7) 0.3106(10) 0.0323(4) 0.034(2) Uani 1 1 d . . .
H9A H 0.9078 0.3919 0.0595 0.041 Uiso 1 1 calc R . .
C10 C 0.8784(7) 0.3294(10) -0.0364(4) 0.032(2) Uani 1 1 d . . .
H10A H 0.8904 0.4241 -0.0543 0.038 Uiso 1 1 calc R . .
C11 C 0.8331(6) 0.0785(9) -0.0503(3) 0.0216(17) Uani 1 1 d . . .
C12 C 0.7984(6) -0.0396(8) -0.0937(4) 0.0251(18) Uani 1 1 d . . .
C13 C 0.5097(8) 0.2134(9) -0.0798(4) 0.038(2) Uani 1 1 d . . .
C14 C 0.4813(7) 0.0702(11) -0.0914(6) 0.059(3) Uani 1 1 d . . .
H14A H 0.4621 0.0350 -0.1336 0.071 Uiso 1 1 calc R . .
C15 C 0.5401(8) 0.2647(14) -0.0151(5) 0.066(3) Uani 1 1 d U . .
H15A H 0.5595 0.3655 -0.0100 0.079 Uiso 1 1 calc R . .
C16 C 0.5433(8) 0.1743(13) 0.0422(5) 0.064(3) Uani 1 1 d U . .
H16A H 0.5616 0.2113 0.0842 0.077 Uiso 1 1 calc R . .
C17 C 0.5178(7) 0.0333(10) 0.0303(5) 0.042(2) Uani 1 1 d . . .
C18 C 1.0039(7) 0.5363(8) -0.2070(4) 0.0258(18) Uani 1 1 d . . .
C19 C 0.9329(7) 0.5412(8) -0.2731(4) 0.0241(18) Uani 1 1 d . . .
H1WB H 0.5744 0.2158 -0.2604 0.036 Uiso 1 1 d R . .
H1WA H 0.6429 0.1504 -0.3031 0.036 Uiso 1 1 d R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Gd1 O1 2.357(4) . ?
Gd1 O5 2.379(5) . ?
Gd1 O4 2.385(5) . ?
Gd1 O6 2.386(5) . ?
Gd1 O7 2.398(5) 2_744 ?
Gd1 O1W 2.421(5) . ?
Gd1 N1 2.543(6) . ?
Gd1 N2 2.566(6) . ?
S1 O3 1.426(5) . ?
S1 O2 1.437(6) . ?
S1 O1 1.479(5) . ?
S1 C13 1.759(8) . ?
O4 C19 1.247(8) 2_744 ?
O1W H1WB 0.9029 . ?
O1W H1WA 0.6863 . ?
O5 C19 1.257(8) . ?
O6 C18 1.245(8) . ?
O7 C18 1.265(8) . ?
O7 Gd1 2.398(5) 2_754 ?
N1 C1 1.339(9) . ?
N1 C12 1.366(9) . ?
N2 C10 1.327(9) . ?
N2 C11 1.362(8) . ?
C1 C2 1.392(10) . ?
C1 H1A 0.9300 . ?
C2 C3 1.360(10) . ?
C2 H2A 0.9300 . ?
C3 C4 1.390(10) . ?
C3 H3A 0.9300 . ?
C4 C5 1.418(10) . ?
C4 C12 1.421(10) . ?
C5 C6 1.342(10) . ?
C5 H5A 0.9300 . ?
C6 C7 1.422(10) . ?
C6 H6A 0.9300 . ?
C7 C8 1.394(11) . ?
C7 C11 1.396(10) . ?
C8 C9 1.359(11) . ?
C8 H8A 0.9300 . ?
C9 C10 1.403(10) . ?
C9 H9A 0.9300 . ?
C10 H10A 0.9300 . ?
C11 C12 1.418(10) . ?
C13 C14 1.335(11) . ?
C13 C15 1.419(13) . ?
C14 C17 1.544(13) 3_655 ?
C14 H14A 0.9300 . ?
C15 C16 1.412(13) . ?
C15 H15A 0.9300 . ?
C16 C17 1.311(12) . ?
C16 H16A 0.9300 . ?
C17 C17 1.408(17) 3_655 ?
C17 C14 1.544(13) 3_655 ?
C18 C19 1.523(10) . ?
C19 O4 1.247(8) 2_754 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Gd1 O5 89.80(16) . . ?
O1 Gd1 O4 149.14(17) . . ?
O5 Gd1 O4 109.69(17) . . ?
O1 Gd1 O6 91.83(17) . . ?
O5 Gd1 O6 67.90(16) . . ?
O4 Gd1 O6 74.79(18) . . ?
O1 Gd1 O7 142.06(17) . 2_744 ?
O5 Gd1 O7 78.20(18) . 2_744 ?
O4 Gd1 O7 67.52(17) . 2_744 ?
O6 Gd1 O7 115.64(17) . 2_744 ?
O1 Gd1 O1W 73.12(17) . . ?
O5 Gd1 O1W 80.83(18) . . ?
O4 Gd1 O1W 132.04(17) . . ?
O6 Gd1 O1W 145.43(18) . . ?
O7 Gd1 O1W 69.51(17) 2_744 . ?
O1 Gd1 N1 95.81(17) . . ?
O5 Gd1 N1 157.44(18) . . ?
O4 Gd1 N1 75.48(18) . . ?
O6 Gd1 N1 133.45(18) . . ?
O7 Gd1 N1 84.07(18) 2_744 . ?
O1W Gd1 N1 79.95(19) . . ?
O1 Gd1 N2 74.07(17) . . ?
O5 Gd1 N2 137.98(18) . . ?
O4 Gd1 N2 75.52(17) . . ?
O6 Gd1 N2 74.02(17) . . ?
O7 Gd1 N2 136.33(17) 2_744 . ?
O1W Gd1 N2 127.81(18) . . ?
N1 Gd1 N2 64.35(19) . . ?
O3 S1 O2 114.5(4) . . ?
O3 S1 O1 112.0(3) . . ?
O2 S1 O1 110.3(3) . . ?
O3 S1 C13 107.9(4) . . ?
O2 S1 C13 106.9(4) . . ?
O1 S1 C13 104.6(3) . . ?
S1 O1 Gd1 143.5(3) . . ?
C19 O4 Gd1 118.2(5) 2_744 . ?
Gd1 O1W H1WB 117.4 . . ?
Gd1 O1W H1WA 136.4 . . ?
H1WB O1W H1WA 106.2 . . ?
C19 O5 Gd1 117.5(4) . . ?
C18 O6 Gd1 116.6(5) . . ?
C18 O7 Gd1 117.8(5) . 2_754 ?
C1 N1 C12 118.8(7) . . ?
C1 N1 Gd1 122.0(5) . . ?
C12 N1 Gd1 119.2(5) . . ?
C10 N2 C11 118.4(7) . . ?
C10 N2 Gd1 122.3(5) . . ?
C11 N2 Gd1 119.3(5) . . ?
N1 C1 C2 122.7(8) . . ?
N1 C1 H1A 118.7 . . ?
C2 C1 H1A 118.7 . . ?
C3 C2 C1 118.9(8) . . ?
C3 C2 H2A 120.5 . . ?
C1 C2 H2A 120.5 . . ?
C2 C3 C4 120.7(7) . . ?
C2 C3 H3A 119.6 . . ?
C4 C3 H3A 119.6 . . ?
C3 C4 C5 123.9(7) . . ?
C3 C4 C12 117.8(7) . . ?
C5 C4 C12 118.3(7) . . ?
C6 C5 C4 121.9(7) . . ?
C6 C5 H5A 119.0 . . ?
C4 C5 H5A 119.0 . . ?
C5 C6 C7 120.6(7) . . ?
C5 C6 H6A 119.7 . . ?
C7 C6 H6A 119.7 . . ?
C8 C7 C11 117.8(7) . . ?
C8 C7 C6 122.6(7) . . ?
C11 C7 C6 119.7(7) . . ?
C9 C8 C7 119.9(7) . . ?
C9 C8 H8A 120.0 . . ?
C7 C8 H8A 120.0 . . ?
C8 C9 C10 119.3(8) . . ?
C8 C9 H9A 120.4 . . ?
C10 C9 H9A 120.4 . . ?
N2 C10 C9 122.2(8) . . ?
N2 C10 H10A 118.9 . . ?
C9 C10 H10A 118.9 . . ?
N2 C11 C7 122.4(7) . . ?
N2 C11 C12 117.8(6) . . ?
C7 C11 C12 119.8(7) . . ?
N1 C12 C11 119.2(7) . . ?
N1 C12 C4 121.1(7) . . ?
C11 C12 C4 119.7(7) . . ?
C14 C13 C15 121.3(9) . . ?
C14 C13 S1 121.1(8) . . ?
C15 C13 S1 117.6(8) . . ?
C13 C14 C17 115.8(10) . 3_655 ?
C13 C14 H14A 122.1 . . ?
C17 C14 H14A 122.1 3_655 . ?
C16 C15 C13 125.0(11) . . ?
C16 C15 H15A 117.5 . . ?
C13 C15 H15A 117.5 . . ?
C17 C16 C15 113.4(11) . . ?
C17 C16 H16A 123.3 . . ?
C15 C16 H16A 123.3 . . ?
C16 C17 C17 128.2(13) . 3_655 ?
C16 C17 C14 115.5(9) . 3_655 ?
C17 C17 C14 116.2(10) 3_655 3_655 ?
O6 C18 O7 125.7(7) . . ?
O6 C18 C19 117.5(7) . . ?
O7 C18 C19 116.8(7) . . ?
O4 C19 O5 126.7(7) 2_754 . ?
O4 C19 C18 116.8(7) 2_754 . ?
O5 C19 C18 116.5(7) . . ?

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 -170.8(4) . . . . ?
O2 S1 O1 Gd1 -42.0(6) . . . . ?
C13 S1 O1 Gd1 72.6(6) . . . . ?
O5 Gd1 O1 S1 118.7(5) . . . . ?
O4 Gd1 O1 S1 -110.7(5) . . . . ?
O6 Gd1 O1 S1 -173.4(5) . . . . ?
O7 Gd1 O1 S1 48.4(6) 2_744 . . . ?
O1W Gd1 O1 S1 38.2(5) . . . . ?
N1 Gd1 O1 S1 -39.4(5) . . . . ?
N2 Gd1 O1 S1 -100.6(5) . . . . ?
O1 Gd1 O4 C19 150.8(5) . . . 2_744 ?
O5 Gd1 O4 C19 -82.9(5) . . . 2_744 ?
O6 Gd1 O4 C19 -142.1(6) . . . 2_744 ?
O7 Gd1 O4 C19 -15.4(5) 2_744 . . 2_744 ?
O1W Gd1 O4 C19 12.5(7) . . . 2_744 ?
N1 Gd1 O4 C19 74.1(5) . . . 2_744 ?
N2 Gd1 O4 C19 140.8(6) . . . 2_744 ?
O1 Gd1 O5 C19 107.3(5) . . . . ?
O4 Gd1 O5 C19 -48.3(5) . . . . ?
O6 Gd1 O5 C19 15.2(5) . . . . ?
O7 Gd1 O5 C19 -109.0(5) 2_744 . . . ?
O1W Gd1 O5 C19 -179.8(5) . . . . ?
N1 Gd1 O5 C19 -147.9(5) . . . . ?
N2 Gd1 O5 C19 41.7(6) . . . . ?
O1 Gd1 O6 C18 -106.6(5) . . . . ?
O5 Gd1 O6 C18 -17.5(5) . . . . ?
O4 Gd1 O6 C18 101.6(5) . . . . ?
O7 Gd1 O6 C18 46.4(6) 2_744 . . . ?
O1W Gd1 O6 C18 -44.3(6) . . . . ?
N1 Gd1 O6 C18 153.7(5) . . . . ?
N2 Gd1 O6 C18 -179.4(5) . . . . ?
O1 Gd1 N1 C1 110.5(6) . . . . ?
O5 Gd1 N1 C1 6.9(8) . . . . ?
O4 Gd1 N1 C1 -99.6(6) . . . . ?
O6 Gd1 N1 C1 -151.4(5) . . . . ?
O7 Gd1 N1 C1 -31.4(5) 2_744 . . . ?
O1W Gd1 N1 C1 38.8(5) . . . . ?
N2 Gd1 N1 C1 179.7(6) . . . . ?
O1 Gd1 N1 C12 -72.8(5) . . . . ?
O5 Gd1 N1 C12 -176.5(5) . . . . ?
O4 Gd1 N1 C12 77.1(5) . . . . ?
O6 Gd1 N1 C12 25.3(6) . . . . ?
O7 Gd1 N1 C12 145.3(5) 2_744 . . . ?
O1W Gd1 N1 C12 -144.5(5) . . . . ?
N2 Gd1 N1 C12 -3.6(5) . . . . ?
O1 Gd1 N2 C10 -71.3(5) . . . . ?
O5 Gd1 N2 C10 -0.1(6) . . . . ?
O4 Gd1 N2 C10 103.3(5) . . . . ?
O6 Gd1 N2 C10 25.3(5) . . . . ?
O7 Gd1 N2 C10 135.9(5) 2_744 . . . ?
O1W Gd1 N2 C10 -124.2(5) . . . . ?
N1 Gd1 N2 C10 -176.1(6) . . . . ?
O1 Gd1 N2 C11 107.6(5) . . . . ?
O5 Gd1 N2 C11 178.8(4) . . . . ?
O4 Gd1 N2 C11 -77.7(5) . . . . ?
O6 Gd1 N2 C11 -155.7(5) . . . . ?
O7 Gd1 N2 C11 -45.1(6) 2_744 . . . ?
O1W Gd1 N2 C11 54.8(5) . . . . ?
N1 Gd1 N2 C11 2.9(5) . . . . ?
C12 N1 C1 C2 1.5(11) . . . . ?
Gd1 N1 C1 C2 178.2(5) . . . . ?
N1 C1 C2 C3 -0.6(12) . . . . ?
C1 C2 C3 C4 -1.2(12) . . . . ?
C2 C3 C4 C5 -180.0(7) . . . . ?
C2 C3 C4 C12 2.1(11) . . . . ?
C3 C4 C5 C6 -176.0(7) . . . . ?
C12 C4 C5 C6 2.0(11) . . . . ?
C4 C5 C6 C7 -1.1(12) . . . . ?
C5 C6 C7 C8 177.5(7) . . . . ?
C5 C6 C7 C11 -1.0(12) . . . . ?
C11 C7 C8 C9 -1.4(11) . . . . ?
C6 C7 C8 C9 -180.0(8) . . . . ?
C7 C8 C9 C10 0.3(12) . . . . ?
C11 N2 C10 C9 0.6(10) . . . . ?
Gd1 N2 C10 C9 179.5(5) . . . . ?
C8 C9 C10 N2 0.1(12) . . . . ?
C10 N2 C11 C7 -1.7(10) . . . . ?
Gd1 N2 C11 C7 179.3(5) . . . . ?
C10 N2 C11 C12 176.9(6) . . . . ?
Gd1 N2 C11 C12 -2.1(8) . . . . ?
C8 C7 C11 N2 2.2(11) . . . . ?
C6 C7 C11 N2 -179.2(7) . . . . ?
C8 C7 C11 C12 -176.5(7) . . . . ?
C6 C7 C11 C12 2.1(11) . . . . ?
C1 N1 C12 C11 -179.0(6) . . . . ?
Gd1 N1 C12 C11 4.2(9) . . . . ?
C1 N1 C12 C4 -0.5(10) . . . . ?
Gd1 N1 C12 C4 -177.3(5) . . . . ?
N2 C11 C12 N1 -1.4(10) . . . . ?
C7 C11 C12 N1 177.3(6) . . . . ?
N2 C11 C12 C4 -179.9(6) . . . . ?
C7 C11 C12 C4 -1.2(10) . . . . ?
C3 C4 C12 N1 -1.2(11) . . . . ?
C5 C4 C12 N1 -179.3(7) . . . . ?
C3 C4 C12 C11 177.3(7) . . . . ?
C5 C4 C12 C11 -0.8(10) . . . . ?
O3 S1 C13 C14 138.2(7) . . . . ?
O2 S1 C13 C14 14.5(8) . . . . ?
O1 S1 C13 C14 -102.4(7) . . . . ?
O3 S1 C13 C15 -43.3(7) . . . . ?
O2 S1 C13 C15 -166.9(6) . . . . ?
O1 S1 C13 C15 76.1(7) . . . . ?
C15 C13 C14 C17 0.8(12) . . . 3_655 ?
S1 C13 C14 C17 179.2(5) . . . 3_655 ?
C14 C13 C15 C16 -0.3(13) . . . . ?
S1 C13 C15 C16 -178.8(7) . . . . ?
C13 C15 C16 C17 1.6(13) . . . . ?
C15 C16 C17 C17 -3.7(16) . . . 3_655 ?
C15 C16 C17 C14 -179.5(7) . . . 3_655 ?
Gd1 O6 C18 O7 -159.6(6) . . . . ?
Gd1 O6 C18 C19 18.3(8) . . . . ?
Gd1 O7 C18 O6 170.8(6) 2_754 . . . ?
Gd1 O7 C18 C19 -7.1(8) 2_754 . . . ?
Gd1 O5 C19 O4 168.8(6) . . . 2_754 ?
Gd1 O5 C19 C18 -12.1(8) . . . . ?
O6 C18 C19 O4 174.8(6) . . . 2_754 ?
O7 C18 C19 O4 -7.1(10) . . . 2_754 ?
O6 C18 C19 O5 -4.3(10) . . . . ?
O7 C18 C19 O5 173.8(6) . . . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         1.370
_refine_diff_density_min         -0.795
_refine_diff_density_rms         0.142
