# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C34 H21 N5 O14 S2 Sm2'
_chemical_formula_weight         1088.38

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                   9.6304(7)
_cell_length_b                   9.6386(7)
_cell_length_c                   10.0130(7)
_cell_angle_alpha                85.4430(10)
_cell_angle_beta                 72.7850(10)
_cell_angle_gamma                72.7610(10)
_cell_volume                     847.89(11)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2436
_cell_measurement_theta_min      3.06
_cell_measurement_theta_max      27.65

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.132
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             528
_exptl_absorpt_coefficient_mu    3.635
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.4516
_exptl_absorpt_correction_T_max  0.8682
_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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            4228
_diffrn_reflns_av_R_equivalents  0.0197
_diffrn_reflns_av_sigmaI/netI    0.0401
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.21
_diffrn_reflns_theta_max         25.00
_reflns_number_total             2957
_reflns_number_gt                2725
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_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)+(0.0331P)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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2957
_refine_ls_number_parameters     277
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.0280
_refine_ls_R_factor_gt           0.0253
_refine_ls_wR_factor_ref         0.0624
_refine_ls_wR_factor_gt          0.0607
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.032
_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
C1 C 0.4769(6) 0.3275(6) 0.5735(5) 0.0367(12) Uani 1 1 d . . .
H1A H 0.4940 0.3209 0.4775 0.044 Uiso 1 1 calc R . .
C2 C 0.5877(6) 0.3545(6) 0.6219(6) 0.0457(15) Uani 1 1 d . . .
H2A H 0.6782 0.3618 0.5591 0.055 Uiso 1 1 calc R . .
C3 C 0.5635(6) 0.3699(6) 0.7602(6) 0.0417(13) Uani 1 1 d . . .
H3A H 0.6373 0.3881 0.7930 0.050 Uiso 1 1 calc R . .
C4 C 0.4277(6) 0.3586(5) 0.8541(5) 0.0298(11) Uani 1 1 d . . .
C5 C 0.3903(6) 0.3729(5) 1.0028(5) 0.0355(12) Uani 1 1 d . . .
H5A H 0.4614 0.3881 1.0413 0.043 Uiso 1 1 calc R . .
C6 C 0.2572(7) 0.3650(5) 1.0879(5) 0.0381(13) Uani 1 1 d . . .
H6A H 0.2354 0.3794 1.1836 0.046 Uiso 1 1 calc R . .
C7 C 0.1473(6) 0.3346(5) 1.0336(5) 0.0293(11) Uani 1 1 d . . .
C8 C 0.0079(7) 0.3202(6) 1.1187(5) 0.0420(14) Uani 1 1 d . . .
H8A H -0.0175 0.3324 1.2150 0.050 Uiso 1 1 calc R . .
C9 C -0.0902(6) 0.2887(6) 1.0608(5) 0.0441(14) Uani 1 1 d . . .
H9A H -0.1836 0.2803 1.1161 0.053 Uiso 1 1 calc R . .
C10 C -0.0471(6) 0.2690(6) 0.9160(5) 0.0345(12) Uani 1 1 d . . .
H10A H -0.1151 0.2482 0.8769 0.041 Uiso 1 1 calc R . .
C11 C 0.1801(5) 0.3135(4) 0.8895(4) 0.0223(10) Uani 1 1 d . . .
C12 C 0.3211(5) 0.3276(4) 0.7978(5) 0.0228(10) Uani 1 1 d . . .
C13 C 0.0197(5) 0.0243(5) 0.4228(4) 0.0208(9) Uani 1 1 d . . .
C14 C 0.6234(12) -0.0127(12) 0.8740(11) 0.019(4) Uani 0.50 1 d PGU A -1
H14 H 0.7003 -0.0223 0.7902 0.023 Uiso 0.50 1 calc PR A -1
C15 C 0.4856(13) -0.0329(13) 0.8768(13) 0.012(3) Uani 0.50 1 d PGU A -1
C16 C 0.3706(13) -0.0185(15) 1.0020(14) 0.029(4) Uani 0.50 1 d PGU A -1
C17 C 0.3936(12) 0.0161(15) 1.1245(13) 0.027(4) Uani 0.50 1 d PGU A -1
H17 H 0.3167 0.0258 1.2083 0.032 Uiso 0.50 1 calc PR A -1
C18 C 0.5315(13) 0.0363(14) 1.1216(11) 0.024(4) Uani 0.50 1 d PGU . -1
C19 C 0.6464(12) 0.0219(12) 0.9964(11) 0.009(3) Uani 0.50 1 d PGU A -1
H19 H 0.7387 0.0354 0.9945 0.010 Uiso 0.50 1 calc PR A -1
C20 C -0.0745(4) 0.4896(4) 0.5497(4) 0.0170(9) Uani 1 1 d . . .
N1 N 0.3473(4) 0.3107(4) 0.6581(4) 0.0251(9) Uani 1 1 d . A .
N2 N 0.0835(4) 0.2782(4) 0.8316(4) 0.0275(9) Uani 1 1 d . A .
N3 N 0.2213(9) -0.0337(9) 1.0130(8) 0.035(2) Uani 0.50 1 d P A -1
H3B H 0.1529 -0.0214 1.0924 0.042 Uiso 0.50 1 calc PR A -1
H3C H 0.2018 -0.0551 0.9400 0.042 Uiso 0.50 1 calc PR A -1
O1 O 0.0930(4) 0.1171(3) 0.3962(3) 0.0260(7) Uani 1 1 d . A .
O2 O -0.0216(4) -0.0305(3) 0.3392(3) 0.0276(7) Uani 1 1 d . . .
O3 O 0.3229(3) 0.0095(3) 0.6987(3) 0.0260(7) Uani 1 1 d . A .
O4 O 0.5932(3) -0.0963(3) 0.6130(3) 0.0266(7) Uani 1 1 d . . .
O5 O 0.4341(4) -0.2380(3) 0.7559(3) 0.0305(8) Uani 1 1 d . A .
O6 O -0.0649(3) 0.3690(3) 0.6102(3) 0.0275(7) Uani 1 1 d . A .
O7 O -0.1911(3) 0.5941(3) 0.5631(3) 0.0254(7) Uani 1 1 d . . .
S1 S 0.45627(12) -0.09608(11) 0.72566(10) 0.0192(2) Uani 1 1 d . . .
Sm1 Sm 0.18129(2) 0.19157(2) 0.57435(2) 0.01585(9) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.332(6) . ?
C1 C2 1.390(7) . ?
C1 H1A 0.9300 . ?
C2 C3 1.347(7) . ?
C2 H2A 0.9300 . ?
C3 C4 1.396(7) . ?
C3 H3A 0.9300 . ?
C4 C12 1.418(6) . ?
C4 C5 1.433(7) . ?
C5 C6 1.333(8) . ?
C5 H5A 0.9300 . ?
C6 C7 1.433(7) . ?
C6 H6A 0.9300 . ?
C7 C8 1.400(7) . ?
C7 C11 1.400(6) . ?
C8 C9 1.358(8) . ?
C8 H8A 0.9300 . ?
C9 C10 1.396(7) . ?
C9 H9A 0.9300 . ?
C10 N2 1.315(6) . ?
C10 H10A 0.9300 . ?
C11 N2 1.362(5) . ?
C11 C12 1.434(6) . ?
C12 N1 1.360(6) . ?
C13 O2 1.236(5) . ?
C13 O1 1.263(5) . ?
C13 C13 1.548(8) 2_556 ?
C14 C15 1.3900 . ?
C14 C19 1.3900 . ?
C14 H14 0.9300 . ?
C15 C16 1.3900 . ?
C15 S1 1.800(11) . ?
C16 C17 1.3900 . ?
C16 N3 1.460(13) . ?
C17 C18 1.3900 . ?
C17 H17 0.9300 . ?
C18 C19 1.3900 . ?
C18 S1 1.724(11) 2_657 ?
C19 H19 0.9300 . ?
C20 O7 1.248(5) . ?
C20 O6 1.258(5) . ?
C20 C20 1.543(8) 2_566 ?
N1 Sm1 2.572(3) . ?
N2 Sm1 2.580(4) . ?
N3 H3B 0.8600 . ?
N3 H3C 0.8600 . ?
O1 Sm1 2.426(3) . ?
O2 Sm1 2.437(3) 2_556 ?
O3 S1 1.464(3) . ?
O3 Sm1 2.394(3) . ?
O4 S1 1.460(3) . ?
O4 Sm1 2.399(3) 2_656 ?
O5 S1 1.442(3) . ?
O6 Sm1 2.422(3) . ?
O7 Sm1 2.399(3) 2_566 ?
S1 C18 1.723(11) 2_657 ?
Sm1 O7 2.399(3) 2_566 ?
Sm1 O4 2.399(3) 2_656 ?
Sm1 O2 2.437(3) 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
N1 C1 C2 123.1(5) . . ?
N1 C1 H1A 118.5 . . ?
C2 C1 H1A 118.5 . . ?
C3 C2 C1 119.7(5) . . ?
C3 C2 H2A 120.1 . . ?
C1 C2 H2A 120.1 . . ?
C2 C3 C4 119.9(5) . . ?
C2 C3 H3A 120.0 . . ?
C4 C3 H3A 120.0 . . ?
C3 C4 C12 117.4(4) . . ?
C3 C4 C5 124.6(5) . . ?
C12 C4 C5 118.0(5) . . ?
C6 C5 C4 122.3(5) . . ?
C6 C5 H5A 118.8 . . ?
C4 C5 H5A 118.8 . . ?
C5 C6 C7 120.6(4) . . ?
C5 C6 H6A 119.7 . . ?
C7 C6 H6A 119.7 . . ?
C8 C7 C11 117.4(5) . . ?
C8 C7 C6 123.0(5) . . ?
C11 C7 C6 119.6(5) . . ?
C9 C8 C7 120.1(5) . . ?
C9 C8 H8A 120.0 . . ?
C7 C8 H8A 120.0 . . ?
C8 C9 C10 118.3(5) . . ?
C8 C9 H9A 120.8 . . ?
C10 C9 H9A 120.8 . . ?
N2 C10 C9 124.1(5) . . ?
N2 C10 H10A 117.9 . . ?
C9 C10 H10A 117.9 . . ?
N2 C11 C7 122.6(4) . . ?
N2 C11 C12 117.9(4) . . ?
C7 C11 C12 119.5(4) . . ?
N1 C12 C4 122.2(4) . . ?
N1 C12 C11 118.0(4) . . ?
C4 C12 C11 119.8(4) . . ?
O2 C13 O1 126.9(4) . . ?
O2 C13 C13 118.2(5) . 2_556 ?
O1 C13 C13 114.9(5) . 2_556 ?
C15 C14 C19 120.0 . . ?
C15 C14 H14 120.0 . . ?
C19 C14 H14 120.0 . . ?
C16 C15 C14 120.0 . . ?
C16 C15 S1 117.8(5) . . ?
C14 C15 S1 121.9(5) . . ?
C17 C16 C15 120.0 . . ?
C17 C16 N3 116.7(7) . . ?
C15 C16 N3 123.3(7) . . ?
C16 C17 C18 120.0 . . ?
C16 C17 H17 120.0 . . ?
C18 C17 H17 120.0 . . ?
C19 C18 C17 120.0 . . ?
C19 C18 S1 122.9(4) . 2_657 ?
C17 C18 S1 116.8(4) . 2_657 ?
C18 C19 C14 120.0 . . ?
C18 C19 H19 120.0 . . ?
C14 C19 H19 120.0 . . ?
O7 C20 O6 126.8(4) . . ?
O7 C20 C20 116.9(4) . 2_566 ?
O6 C20 C20 116.3(4) . 2_566 ?
C1 N1 C12 117.6(4) . . ?
C1 N1 Sm1 122.0(3) . . ?
C12 N1 Sm1 118.8(3) . . ?
C10 N2 C11 117.4(4) . . ?
C10 N2 Sm1 123.0(3) . . ?
C11 N2 Sm1 118.8(3) . . ?
C16 N3 H3B 120.0 . . ?
C16 N3 H3C 120.0 . . ?
H3B N3 H3C 120.0 . . ?
C13 O1 Sm1 120.6(3) . . ?
C13 O2 Sm1 119.3(3) . 2_556 ?
S1 O3 Sm1 157.46(19) . . ?
S1 O4 Sm1 158.0(2) . 2_656 ?
C20 O6 Sm1 119.3(3) . . ?
C20 O7 Sm1 120.2(3) . 2_566 ?
O5 S1 O4 113.62(19) . . ?
O5 S1 O3 111.89(19) . . ?
O4 S1 O3 110.85(18) . . ?
O5 S1 C18 105.7(4) . 2_657 ?
O4 S1 C18 109.5(4) . 2_657 ?
O3 S1 C18 104.7(4) . 2_657 ?
O5 S1 C15 108.2(4) . . ?
O4 S1 C15 104.5(4) . . ?
O3 S1 C15 107.3(4) . . ?
C18 S1 C15 5.0(8) 2_657 . ?
O3 Sm1 O7 142.37(10) . 2_566 ?
O3 Sm1 O4 80.47(10) . 2_656 ?
O7 Sm1 O4 79.50(10) 2_566 2_656 ?
O3 Sm1 O6 140.50(10) . . ?
O7 Sm1 O6 67.13(10) 2_566 . ?
O4 Sm1 O6 138.92(10) 2_656 . ?
O3 Sm1 O1 119.11(11) . . ?
O7 Sm1 O1 85.73(10) 2_566 . ?
O4 Sm1 O1 75.16(10) 2_656 . ?
O6 Sm1 O1 79.01(11) . . ?
O3 Sm1 O2 76.26(10) . 2_556 ?
O7 Sm1 O2 141.34(10) 2_566 2_556 ?
O4 Sm1 O2 115.75(11) 2_656 2_556 ?
O6 Sm1 O2 81.06(10) . 2_556 ?
O1 Sm1 O2 66.45(9) . 2_556 ?
O3 Sm1 N1 73.31(11) . . ?
O7 Sm1 N1 73.40(11) 2_566 . ?
O4 Sm1 N1 84.72(11) 2_656 . ?
O6 Sm1 N1 106.75(12) . . ?
O1 Sm1 N1 153.35(11) . . ?
O2 Sm1 N1 139.58(11) 2_556 . ?
O3 Sm1 N2 74.01(11) . . ?
O7 Sm1 N2 105.71(11) 2_566 . ?
O4 Sm1 N2 143.60(11) 2_656 . ?
O6 Sm1 N2 71.45(11) . . ?
O1 Sm1 N2 140.35(11) . . ?
O2 Sm1 N2 83.04(11) 2_556 . ?
N1 Sm1 N2 63.48(12) . . ?

_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         0.773
_refine_diff_density_min         -0.650
_refine_diff_density_rms         0.113
_database_code_depnum_ccdc_archive 'CCDC 981691'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C31 H21 Eu N5 O8 S2'
_chemical_formula_weight         807.61

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'
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                   10.551(2)
_cell_length_b                   10.620(2)
_cell_length_c                   15.094(4)
_cell_angle_alpha                74.956(18)
_cell_angle_beta                 69.597(11)
_cell_angle_gamma                72.234(11)
_cell_volume                     1487.2(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.803
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             802
_exptl_absorpt_coefficient_mu    2.312
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5819
_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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            15738
_diffrn_reflns_av_R_equivalents  0.1132
_diffrn_reflns_av_sigmaI/netI    0.1330
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.04
_diffrn_reflns_theta_max         25.00
_reflns_number_total             5226
_reflns_number_gt                3960
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_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          
; Restraints: DELU,SIMU and ISOR restraints for the disordered H2N-BDS ligand,
 to control the displacement parameters of overlapping components. Such
 restraints are often required for disorder components that interpenetrate each
 other, since the electron density of the disordered atoms strongly overlap and
 can not be resolved satisfactorily in free refinement. Restraints are gentler
 and more flexible than rigid constraints. ; 
;

_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)+(0.0463P)²+1.3125P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5226
_refine_ls_number_parameters     463
_refine_ls_number_restraints     204
_refine_ls_R_factor_all          0.0879
_refine_ls_R_factor_gt           0.0568
_refine_ls_wR_factor_ref         0.1412
_refine_ls_wR_factor_gt          0.1280
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_restrained_S_all      1.066
_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
Eu1 Eu 0.13140(5) 0.12513(4) 0.29193(3) 0.02969(16) Uani 1 1 d . . .
S1 S 0.3740(2) -0.13782(19) 0.40050(16) 0.0359(5) Uani 1 1 d . . .
S3 S -0.1095(3) 0.2038(3) 0.14426(19) 0.0530(7) Uani 1 1 d . . .
O1 O 0.2580(7) -0.1828(5) 0.4729(5) 0.0472(16) Uani 1 1 d . A .
O2 O 0.3298(6) -0.0262(5) 0.3268(4) 0.0364(14) Uani 1 1 d . A .
O3 O 0.4843(7) -0.2430(5) 0.3552(5) 0.0517(17) Uani 1 1 d . A .
O4 O -0.0369(7) 0.1436(6) 0.2173(4) 0.0497(17) Uani 1 1 d . B .
O5 O -0.0711(10) 0.3276(7) 0.0906(6) 0.084(3) Uani 1 1 d . B .
O6 O -0.2558(8) 0.2120(10) 0.1842(7) 0.100(3) Uani 1 1 d . B .
O7 O -0.0038(6) 0.0318(5) 0.6089(4) 0.0340(13) Uani 1 1 d . . .
O8 O 0.0821(7) 0.1321(5) 0.4583(4) 0.0378(14) Uani 1 1 d . . .
N1 N 0.2422(7) -0.0315(6) 0.1679(5) 0.0361(17) Uani 1 1 d . . .
N2 N 0.2429(8) 0.2331(7) 0.1184(5) 0.0435(19) Uani 1 1 d . . .
N3 N 0.2444(7) 0.2975(6) 0.3091(5) 0.0327(16) Uani 1 1 d . . .
N4 N -0.0324(7) 0.3540(6) 0.3221(5) 0.0333(16) Uani 1 1 d . . .
C1 C 0.2474(11) -0.1635(8) 0.1930(7) 0.050(3) Uani 1 1 d . . .
H1A H 0.2183 -0.1999 0.2577 0.060 Uiso 1 1 calc R . .
C2 C 0.2955(13) -0.2483(10) 0.1246(9) 0.068(3) Uani 1 1 d . . .
H2A H 0.2977 -0.3393 0.1442 0.082 Uiso 1 1 calc R . .
C3 C 0.3384(12) -0.1976(12) 0.0302(9) 0.064(3) Uani 1 1 d . . .
H3A H 0.3673 -0.2528 -0.0154 0.077 Uiso 1 1 calc R . .
C4 C 0.3389(10) -0.0626(11) 0.0019(7) 0.052(3) Uani 1 1 d . . .
C5 C 0.3832(11) -0.0026(14) -0.0949(8) 0.068(3) Uani 1 1 d . . .
H5A H 0.4141 -0.0552 -0.1423 0.082 Uiso 1 1 calc R . .
C6 C 0.3823(13) 0.1315(14) -0.1214(8) 0.072(3) Uani 1 1 d . . .
H6A H 0.4138 0.1677 -0.1859 0.086 Uiso 1 1 calc R . .
C7 C 0.3332(12) 0.2159(12) -0.0504(7) 0.060(3) Uani 1 1 d . . .
C8 C 0.3223(13) 0.3555(13) -0.0719(9) 0.075(4) Uani 1 1 d . . .
H8A H 0.3462 0.3970 -0.1357 0.090 Uiso 1 1 calc R . .
C9 C 0.2787(15) 0.4292(12) -0.0031(9) 0.076(4) Uani 1 1 d . . .
H9A H 0.2760 0.5204 -0.0181 0.092 Uiso 1 1 calc R . .
C10 C 0.2368(12) 0.3655(10) 0.0929(8) 0.062(3) Uani 1 1 d . . .
H10A H 0.1805 0.4350 0.1335 0.075 Uiso 1 1 d R . .
C11 C 0.2897(9) 0.1596(9) 0.0465(6) 0.041(2) Uani 1 1 d . . .
C12 C 0.2914(9) 0.0177(9) 0.0736(6) 0.040(2) Uani 1 1 d . . .
C13 C 0.3775(9) 0.2710(8) 0.3035(7) 0.045(2) Uani 1 1 d . . .
H13A H 0.4364 0.1934 0.2812 0.054 Uiso 1 1 calc R . .
C14 C 0.4337(11) 0.3542(9) 0.3294(8) 0.060(3) Uani 1 1 d . . .
H14A H 0.5278 0.3309 0.3254 0.072 Uiso 1 1 calc R . .
C15 C 0.3499(11) 0.4702(9) 0.3609(7) 0.051(3) Uani 1 1 d . . .
H15A H 0.3865 0.5272 0.3774 0.061 Uiso 1 1 calc R . .
C16 C 0.2062(10) 0.5023(8) 0.3681(6) 0.041(2) Uani 1 1 d . . .
C17 C 0.1116(11) 0.6191(8) 0.4026(6) 0.043(2) Uani 1 1 d . . .
H17A H 0.1498 0.6879 0.4028 0.052 Uiso 1 1 d R . .
C18 C -0.0223(11) 0.6509(8) 0.4050(7) 0.045(2) Uani 1 1 d . . .
H18A H -0.0812 0.7299 0.4252 0.054 Uiso 1 1 calc R . .
C19 C -0.0748(10) 0.5637(8) 0.3767(6) 0.040(2) Uani 1 1 d . . .
C20 C -0.2150(10) 0.5902(8) 0.3818(7) 0.049(3) Uani 1 1 d . . .
H20A H -0.2763 0.6690 0.4009 0.059 Uiso 1 1 calc R . .
C21 C -0.2617(10) 0.5001(9) 0.3588(8) 0.053(3) Uani 1 1 d . . .
H21A H -0.3543 0.5168 0.3607 0.063 Uiso 1 1 calc R . .
C22 C -0.1657(10) 0.3804(8) 0.3318(7) 0.043(2) Uani 1 1 d . . .
H22A H -0.1992 0.3154 0.3052 0.051 Uiso 1 1 d R . .
C23 C 0.0132(9) 0.4432(7) 0.3460(6) 0.0316(19) Uani 1 1 d . . .
C24 C 0.1577(9) 0.4140(7) 0.3417(6) 0.0322(19) Uani 1 1 d . . .
C25 C 0.454(3) -0.078(2) 0.4555(19) 0.029(4) Uani 0.50 1 d PGU A -1
C26 C 0.381(3) -0.051(2) 0.5476(19) 0.032(5) Uani 0.50 1 d PGU A -1
H26 H 0.2969 -0.0755 0.5796 0.039 Uiso 0.50 1 calc PR A -1
C27 C 0.433(3) 0.013(2) 0.5917(19) 0.038(5) Uani 0.50 1 d PGU A -1
H27 H 0.3844 0.0312 0.6533 0.046 Uiso 0.50 1 calc PR A -1
C28 C 0.559(3) 0.050(2) 0.5438(19) 0.028(4) Uani 0.50 1 d PGU . -1
C29 C 0.632(3) 0.023(2) 0.4518(19) 0.036(5) Uani 0.50 1 d PGU A -1
H29 H 0.7159 0.0476 0.4198 0.043 Uiso 0.50 1 calc PR A -1
C30 C 0.580(3) -0.041(2) 0.4077(19) 0.029(4) Uani 0.50 1 d PGU A -1
N5 N 0.6474(18) -0.0501(15) 0.3203(10) 0.052(4) Uani 0.50 1 d PU A -1
H5B H 0.7199 -0.0178 0.2930 0.062 Uiso 0.50 1 calc PR A -1
H5C H 0.6206 -0.0885 0.2887 0.062 Uiso 0.50 1 calc PR A -1
C31 C 0.0241(9) 0.0488(7) 0.5197(6) 0.0317(19) Uani 1 1 d U . .
C32 C -0.045(2) 0.0729(16) 0.0668(15) 0.028(4) Uani 0.50 1 d PGU B -2
C33 C -0.001(2) 0.1183(16) -0.0314(15) 0.040(4) Uani 0.50 1 d PGU B -2
H33 H -0.0001 0.2083 -0.0545 0.048 Uiso 0.50 1 calc PR B -2
C34 C 0.042(3) 0.0293(18) -0.0952(15) 0.049(5) Uani 0.50 1 d PGU B -2
C35 C 0.041(3) -0.1052(18) -0.0607(16) 0.049(5) Uani 0.50 1 d PGU . -2
C36 C -0.004(3) -0.1506(15) 0.0375(17) 0.042(5) Uani 0.50 1 d PGU B -2
H36 H -0.0047 -0.2406 0.0606 0.050 Uiso 0.50 1 calc PR B -2
C37 C -0.047(2) -0.0615(16) 0.1012(15) 0.038(5) Uani 0.50 1 d PGU B -2
H37 H -0.0766 -0.0919 0.1670 0.046 Uiso 0.50 1 calc PR B -2
N6 N 0.085(2) 0.101(2) -0.1986(14) 0.089(6) Uani 0.50 1 d PU B -2
H6B H 0.0806 0.1854 -0.2106 0.107 Uiso 0.50 1 calc PR B -2
H6C H 0.1138 0.0564 -0.2450 0.107 Uiso 0.50 1 calc PR B -2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Eu1 O7 2.345(5) 2_556 ?
Eu1 O2 2.349(5) . ?
Eu1 O4 2.351(6) . ?
Eu1 O8 2.396(5) . ?
Eu1 N1 2.557(6) . ?
Eu1 N4 2.562(6) . ?
Eu1 N3 2.575(6) . ?
Eu1 N2 2.583(7) . ?
Eu1 C31 3.171(9) 2_556 ?
Eu1 C31 3.187(9) . ?
S1 O1 1.440(7) . ?
S1 O3 1.455(6) . ?
S1 O2 1.483(5) . ?
S1 C25 1.70(3) . ?
S1 C28 1.82(3) 2_656 ?
S3 O6 1.432(9) . ?
S3 O5 1.447(8) . ?
S3 O4 1.461(6) . ?
S3 C35 1.67(2) 2 ?
S3 C32 1.864(19) . ?
O7 C31 1.250(9) . ?
O7 Eu1 2.345(5) 2_556 ?
O8 C31 1.235(10) . ?
N1 C1 1.343(10) . ?
N1 C12 1.354(11) . ?
N2 C10 1.346(11) . ?
N2 C11 1.365(11) . ?
N3 C13 1.322(11) . ?
N3 C24 1.386(10) . ?
N4 C22 1.310(11) . ?
N4 C23 1.355(9) . ?
C1 C2 1.405(12) . ?
C1 H1A 0.9300 . ?
C2 C3 1.350(16) . ?
C2 H2A 0.9300 . ?
C3 C4 1.386(15) . ?
C3 H3A 0.9300 . ?
C4 C5 1.408(15) . ?
C4 C12 1.411(12) . ?
C5 C6 1.373(16) . ?
C5 H5A 0.9300 . ?
C6 C7 1.431(15) . ?
C6 H6A 0.9300 . ?
C7 C11 1.397(13) . ?
C7 C8 1.410(15) . ?
C8 C9 1.331(16) . ?
C8 H8A 0.9300 . ?
C9 C10 1.407(14) . ?
C9 H9A 0.9300 . ?
C10 H10A 0.9936 . ?
C11 C12 1.451(12) . ?
C13 C14 1.395(12) . ?
C13 H13A 0.9300 . ?
C14 C15 1.368(13) . ?
C14 H14A 0.9300 . ?
C15 C16 1.419(13) . ?
C15 H15A 0.9300 . ?
C16 C24 1.388(11) . ?
C16 C17 1.423(12) . ?
C17 C18 1.338(13) . ?
C17 H17A 0.9374 . ?
C18 C19 1.425(12) . ?
C18 H18A 0.9300 . ?
C19 C20 1.397(13) . ?
C19 C23 1.413(11) . ?
C20 C21 1.364(12) . ?
C20 H20A 0.9300 . ?
C21 C22 1.414(11) . ?
C21 H21A 0.9300 . ?
C22 H22A 1.0752 . ?
C23 C24 1.441(12) . ?
C25 C26 1.3900 . ?
C25 C30 1.3900 . ?
C26 C27 1.3900 . ?
C26 H26 0.9300 . ?
C27 C28 1.3900 . ?
C27 H27 0.9300 . ?
C28 C29 1.3900 . ?
C28 S1 1.82(3) 2_656 ?
C29 C30 1.3900 . ?
C29 H29 0.9300 . ?
C30 N5 1.28(3) . ?
N5 H5B 0.8600 . ?
N5 H5C 0.8600 . ?
C31 C31 1.592(14) 2_556 ?
C31 Eu1 3.171(9) 2_556 ?
C32 C33 1.3900 . ?
C32 C37 1.3900 . ?
C33 C34 1.3900 . ?
C33 H33 0.9300 . ?
C34 C35 1.3900 . ?
C34 N6 1.52(3) . ?
C35 C36 1.3900 . ?
C35 S3 1.67(2) 2 ?
C36 C37 1.3900 . ?
C36 H36 0.9300 . ?
C37 H37 0.9300 . ?
N6 H6B 0.8600 . ?
N6 H6C 0.8600 . ?

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
O7 Eu1 O2 87.53(19) 2_556 . ?
O7 Eu1 O4 75.7(2) 2_556 . ?
O2 Eu1 O4 140.81(19) . . ?
O7 Eu1 O8 68.45(17) 2_556 . ?
O2 Eu1 O8 78.6(2) . . ?
O4 Eu1 O8 124.7(2) . . ?
O7 Eu1 N1 88.7(2) 2_556 . ?
O2 Eu1 N1 71.5(2) . . ?
O4 Eu1 N1 72.9(2) . . ?
O8 Eu1 N1 143.0(2) . . ?
O7 Eu1 N4 104.8(2) 2_556 . ?
O2 Eu1 N4 141.8(2) . . ?
O4 Eu1 N4 77.3(2) . . ?
O8 Eu1 N4 73.0(2) . . ?
N1 Eu1 N4 143.0(2) . . ?
O7 Eu1 N3 138.53(19) 2_556 . ?
O2 Eu1 N3 82.18(19) . . ?
O4 Eu1 N3 132.9(2) . . ?
O8 Eu1 N3 70.15(19) . . ?
N1 Eu1 N3 124.8(2) . . ?
N4 Eu1 N3 64.5(2) . . ?
O7 Eu1 N2 146.7(2) 2_556 . ?
O2 Eu1 N2 100.0(2) . . ?
O4 Eu1 N2 78.3(2) . . ?
O8 Eu1 N2 144.8(2) . . ?
N1 Eu1 N2 63.8(2) . . ?
N4 Eu1 N2 89.3(2) . . ?
N3 Eu1 N2 74.8(2) . . ?
O7 Eu1 C31 19.80(17) 2_556 2_556 ?
O2 Eu1 C31 82.4(2) . 2_556 ?
O4 Eu1 C31 91.4(2) . 2_556 ?
O8 Eu1 C31 48.73(18) . 2_556 ?
N1 Eu1 C31 105.0(2) . 2_556 ?
N4 Eu1 C31 97.1(2) . 2_556 ?
N3 Eu1 C31 118.7(2) . 2_556 ?
N2 Eu1 C31 166.5(2) . 2_556 ?
O7 Eu1 C31 48.78(18) 2_556 . ?
O2 Eu1 C31 78.2(2) . . ?
O4 Eu1 C31 112.9(2) . . ?
O8 Eu1 C31 19.77(17) . . ?
N1 Eu1 C31 128.5(2) . . ?
N4 Eu1 C31 83.2(2) . . ?
N3 Eu1 C31 89.8(2) . . ?
N2 Eu1 C31 164.5(2) . . ?
C31 Eu1 C31 29.0(2) 2_556 . ?
O1 S1 O3 115.0(4) . . ?
O1 S1 O2 112.5(4) . . ?
O3 S1 O2 110.5(4) . . ?
O1 S1 C25 107.7(9) . . ?
O3 S1 C25 103.4(8) . . ?
O2 S1 C25 107.0(8) . . ?
O1 S1 C28 107.2(8) . 2_656 ?
O3 S1 C28 110.8(8) . 2_656 ?
O2 S1 C28 99.8(7) . 2_656 ?
C25 S1 C28 8.6(14) . 2_656 ?
O6 S3 O5 115.7(6) . . ?
O6 S3 O4 111.3(5) . . ?
O5 S3 O4 110.7(5) . . ?
O6 S3 C35 110.0(8) . 2 ?
O5 S3 C35 101.8(7) . 2 ?
O4 S3 C35 106.6(8) . 2 ?
O6 S3 C32 104.5(7) . . ?
O5 S3 C32 111.1(7) . . ?
O4 S3 C32 102.7(7) . . ?
C35 S3 C32 9.3(12) 2 . ?
S1 O2 Eu1 142.2(4) . . ?
S3 O4 Eu1 153.5(4) . . ?
C31 O7 Eu1 120.7(5) . 2_556 ?
C31 O8 Eu1 119.2(5) . . ?
C1 N1 C12 117.7(7) . . ?
C1 N1 Eu1 121.5(6) . . ?
C12 N1 Eu1 120.7(5) . . ?
C10 N2 C11 117.3(8) . . ?
C10 N2 Eu1 122.3(7) . . ?
C11 N2 Eu1 119.5(5) . . ?
C13 N3 C24 118.0(7) . . ?
C13 N3 Eu1 123.0(5) . . ?
C24 N3 Eu1 118.1(5) . . ?
C22 N4 C23 117.3(7) . . ?
C22 N4 Eu1 122.5(5) . . ?
C23 N4 Eu1 119.2(5) . . ?
N1 C1 C2 122.1(10) . . ?
N1 C1 H1A 119.0 . . ?
C2 C1 H1A 119.0 . . ?
C3 C2 C1 120.0(10) . . ?
C3 C2 H2A 120.0 . . ?
C1 C2 H2A 120.0 . . ?
C2 C3 C4 119.5(9) . . ?
C2 C3 H3A 120.3 . . ?
C4 C3 H3A 120.3 . . ?
C3 C4 C5 122.9(10) . . ?
C3 C4 C12 118.2(10) . . ?
C5 C4 C12 118.9(10) . . ?
C6 C5 C4 121.9(10) . . ?
C6 C5 H5A 119.0 . . ?
C4 C5 H5A 119.0 . . ?
C5 C6 C7 120.5(10) . . ?
C5 C6 H6A 119.7 . . ?
C7 C6 H6A 119.7 . . ?
C11 C7 C8 116.8(10) . . ?
C11 C7 C6 119.2(11) . . ?
C8 C7 C6 124.0(11) . . ?
C9 C8 C7 121.7(11) . . ?
C9 C8 H8A 119.2 . . ?
C7 C8 H8A 119.2 . . ?
C8 C9 C10 118.3(11) . . ?
C8 C9 H9A 120.9 . . ?
C10 C9 H9A 120.9 . . ?
N2 C10 C9 123.1(11) . . ?
N2 C10 H10A 126.0 . . ?
C9 C10 H10A 108.8 . . ?
N2 C11 C7 122.7(9) . . ?
N2 C11 C12 117.5(7) . . ?
C7 C11 C12 119.8(9) . . ?
N1 C12 C4 122.4(9) . . ?
N1 C12 C11 117.9(7) . . ?
C4 C12 C11 119.7(9) . . ?
N3 C13 C14 123.0(8) . . ?
N3 C13 H13A 118.5 . . ?
C14 C13 H13A 118.5 . . ?
C15 C14 C13 119.7(9) . . ?
C15 C14 H14A 120.1 . . ?
C13 C14 H14A 120.1 . . ?
C14 C15 C16 119.0(8) . . ?
C14 C15 H15A 120.5 . . ?
C16 C15 H15A 120.5 . . ?
C24 C16 C15 117.9(8) . . ?
C24 C16 C17 119.6(9) . . ?
C15 C16 C17 122.4(8) . . ?
C18 C17 C16 121.7(8) . . ?
C18 C17 H17A 117.9 . . ?
C16 C17 H17A 117.1 . . ?
C17 C18 C19 120.0(8) . . ?
C17 C18 H18A 120.0 . . ?
C19 C18 H18A 120.0 . . ?
C20 C19 C23 117.4(7) . . ?
C20 C19 C18 121.8(8) . . ?
C23 C19 C18 120.7(9) . . ?
C21 C20 C19 119.6(8) . . ?
C21 C20 H20A 120.2 . . ?
C19 C20 H20A 120.2 . . ?
C20 C21 C22 118.4(9) . . ?
C20 C21 H21A 120.8 . . ?
C22 C21 H21A 120.8 . . ?
N4 C22 C21 124.0(8) . . ?
N4 C22 H22A 116.7 . . ?
C21 C22 H22A 118.3 . . ?
N4 C23 C19 123.1(8) . . ?
N4 C23 C24 119.0(7) . . ?
C19 C23 C24 117.8(7) . . ?
N3 C24 C16 122.3(8) . . ?
N3 C24 C23 117.6(6) . . ?
C16 C24 C23 120.1(7) . . ?
C26 C25 C30 120.0 . . ?
C26 C25 S1 117.3(9) . . ?
C30 C25 S1 122.2(9) . . ?
C27 C26 C25 120.0 . . ?
C27 C26 H26 120.0 . . ?
C25 C26 H26 120.0 . . ?
C26 C27 C28 120.0 . . ?
C26 C27 H27 120.0 . . ?
C28 C27 H27 120.0 . . ?
C29 C28 C27 120.0 . . ?
C29 C28 S1 119.6(9) . 2_656 ?
C27 C28 S1 120.4(9) . 2_656 ?
C30 C29 C28 120.0 . . ?
C30 C29 H29 120.0 . . ?
C28 C29 H29 120.0 . . ?
N5 C30 C29 115.1(14) . . ?
N5 C30 C25 124.5(14) . . ?
C29 C30 C25 120.0 . . ?
C30 N5 H5B 120.0 . . ?
C30 N5 H5C 120.0 . . ?
H5B N5 H5C 120.0 . . ?
O8 C31 O7 128.7(7) . . ?
O8 C31 C31 115.8(9) . 2_556 ?
O7 C31 C31 115.4(9) . 2_556 ?
O8 C31 Eu1 167.7(5) . 2_556 ?
O7 C31 Eu1 39.5(4) . 2_556 ?
C31 C31 Eu1 76.0(6) 2_556 2_556 ?
O8 C31 Eu1 41.0(4) . . ?
O7 C31 Eu1 169.4(6) . . ?
C31 C31 Eu1 75.0(6) 2_556 . ?
Eu1 C31 Eu1 151.0(2) 2_556 . ?
C33 C32 C37 120.0 . . ?
C33 C32 S3 115.8(7) . . ?
C37 C32 S3 124.1(7) . . ?
C32 C33 C34 120.0 . . ?
C32 C33 H33 120.0 . . ?
C34 C33 H33 120.0 . . ?
C33 C34 C35 120.0 . . ?
C33 C34 N6 111.0(12) . . ?
C35 C34 N6 129.0(12) . . ?
C36 C35 C34 120.0 . . ?
C36 C35 S3 124.8(9) . 2 ?
C34 C35 S3 115.0(9) . 2 ?
C37 C36 C35 120.0 . . ?
C37 C36 H36 120.0 . . ?
C35 C36 H36 120.0 . . ?
C36 C37 C32 120.0 . . ?
C36 C37 H37 120.0 . . ?
C32 C37 H37 120.0 . . ?
C34 N6 H6B 120.0 . . ?
C34 N6 H6C 120.0 . . ?
H6B N6 H6C 120.0 . . ?

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
O1 S1 O2 Eu1 9.4(6) . . . . ?
O3 S1 O2 Eu1 139.4(5) . . . . ?
C25 S1 O2 Eu1 -108.7(10) . . . . ?
C28 S1 O2 Eu1 -103.9(9) 2_656 . . . ?
O7 Eu1 O2 S1 -25.5(5) 2_556 . . . ?
O4 Eu1 O2 S1 -89.1(6) . . . . ?
O8 Eu1 O2 S1 43.0(5) . . . . ?
N1 Eu1 O2 S1 -114.9(5) . . . . ?
N4 Eu1 O2 S1 85.5(6) . . . . ?
N3 Eu1 O2 S1 114.3(5) . . . . ?
N2 Eu1 O2 S1 -172.8(5) . . . . ?
C31 Eu1 O2 S1 -6.3(5) 2_556 . . . ?
C31 Eu1 O2 S1 22.9(5) . . . . ?
O6 S3 O4 Eu1 -140.9(8) . . . . ?
O5 S3 O4 Eu1 -10.7(10) . . . . ?
C35 S3 O4 Eu1 99.1(10) 2 . . . ?
C32 S3 O4 Eu1 107.9(10) . . . . ?
O7 Eu1 O4 S3 175.3(9) 2_556 . . . ?
O2 Eu1 O4 S3 -117.3(8) . . . . ?
O8 Eu1 O4 S3 124.9(8) . . . . ?
N1 Eu1 O4 S3 -91.6(9) . . . . ?
N4 Eu1 O4 S3 66.2(8) . . . . ?
N3 Eu1 O4 S3 30.3(10) . . . . ?
N2 Eu1 O4 S3 -25.8(8) . . . . ?
C31 Eu1 O4 S3 163.1(8) 2_556 . . . ?
C31 Eu1 O4 S3 143.1(8) . . . . ?
O7 Eu1 O8 C31 5.1(6) 2_556 . . . ?
O2 Eu1 O8 C31 -86.8(6) . . . . ?
O4 Eu1 O8 C31 58.5(7) . . . . ?
N1 Eu1 O8 C31 -50.5(8) . . . . ?
N4 Eu1 O8 C31 119.1(7) . . . . ?
N3 Eu1 O8 C31 -172.5(7) . . . . ?
N2 Eu1 O8 C31 -177.9(6) . . . . ?
C31 Eu1 O8 C31 3.0(7) 2_556 . . . ?
O7 Eu1 N1 C1 -22.4(7) 2_556 . . . ?
O2 Eu1 N1 C1 65.4(7) . . . . ?
O4 Eu1 N1 C1 -97.8(7) . . . . ?
O8 Eu1 N1 C1 27.7(8) . . . . ?
N4 Eu1 N1 C1 -135.6(6) . . . . ?
N3 Eu1 N1 C1 131.4(7) . . . . ?
N2 Eu1 N1 C1 177.0(7) . . . . ?
C31 Eu1 N1 C1 -11.0(7) 2_556 . . . ?
C31 Eu1 N1 C1 8.3(8) . . . . ?
O7 Eu1 N1 C12 154.2(6) 2_556 . . . ?
O2 Eu1 N1 C12 -118.0(7) . . . . ?
O4 Eu1 N1 C12 78.8(6) . . . . ?
O8 Eu1 N1 C12 -155.7(6) . . . . ?
N4 Eu1 N1 C12 41.0(8) . . . . ?
N3 Eu1 N1 C12 -52.0(7) . . . . ?
N2 Eu1 N1 C12 -6.4(6) . . . . ?
C31 Eu1 N1 C12 165.6(6) 2_556 . . . ?
C31 Eu1 N1 C12 -175.1(6) . . . . ?
O7 Eu1 N2 C10 139.2(7) 2_556 . . . ?
O2 Eu1 N2 C10 -120.0(8) . . . . ?
O4 Eu1 N2 C10 99.9(8) . . . . ?
O8 Eu1 N2 C10 -35.8(9) . . . . ?
N1 Eu1 N2 C10 176.4(8) . . . . ?
N4 Eu1 N2 C10 22.7(8) . . . . ?
N3 Eu1 N2 C10 -41.0(7) . . . . ?
C31 Eu1 N2 C10 141.2(9) 2_556 . . . ?
C31 Eu1 N2 C10 -38.4(13) . . . . ?
O7 Eu1 N2 C11 -29.8(9) 2_556 . . . ?
O2 Eu1 N2 C11 71.0(7) . . . . ?
O4 Eu1 N2 C11 -69.1(7) . . . . ?
O8 Eu1 N2 C11 155.3(6) . . . . ?
N1 Eu1 N2 C11 7.5(6) . . . . ?
N4 Eu1 N2 C11 -146.3(7) . . . . ?
N3 Eu1 N2 C11 150.0(7) . . . . ?
C31 Eu1 N2 C11 -27.7(14) 2_556 . . . ?
C31 Eu1 N2 C11 152.6(7) . . . . ?
O7 Eu1 N3 C13 96.1(7) 2_556 . . . ?
O2 Eu1 N3 C13 18.9(7) . . . . ?
O4 Eu1 N3 C13 -141.1(7) . . . . ?
O8 Eu1 N3 C13 99.5(7) . . . . ?
N1 Eu1 N3 C13 -42.1(8) . . . . ?
N4 Eu1 N3 C13 179.6(8) . . . . ?
N2 Eu1 N3 C13 -83.7(7) . . . . ?
C31 Eu1 N3 C13 95.7(7) 2_556 . . . ?
C31 Eu1 N3 C13 97.0(7) . . . . ?
O7 Eu1 N3 C24 -72.5(6) 2_556 . . . ?
O2 Eu1 N3 C24 -149.8(6) . . . . ?
O4 Eu1 N3 C24 50.2(7) . . . . ?
O8 Eu1 N3 C24 -69.1(6) . . . . ?
N1 Eu1 N3 C24 149.3(5) . . . . ?
N4 Eu1 N3 C24 11.0(5) . . . . ?
N2 Eu1 N3 C24 107.6(6) . . . . ?
C31 Eu1 N3 C24 -73.0(6) 2_556 . . . ?
C31 Eu1 N3 C24 -71.7(6) . . . . ?
O7 Eu1 N4 C22 -40.4(7) 2_556 . . . ?
O2 Eu1 N4 C22 -145.6(7) . . . . ?
O4 Eu1 N4 C22 30.9(7) . . . . ?
O8 Eu1 N4 C22 -101.8(7) . . . . ?
N1 Eu1 N4 C22 67.8(8) . . . . ?
N3 Eu1 N4 C22 -177.5(8) . . . . ?
N2 Eu1 N4 C22 109.1(7) . . . . ?
C31 Eu1 N4 C22 -59.0(7) 2_556 . . . ?
C31 Eu1 N4 C22 -84.5(7) . . . . ?
O7 Eu1 N4 C23 127.4(6) 2_556 . . . ?
O2 Eu1 N4 C23 22.2(8) . . . . ?
O4 Eu1 N4 C23 -161.3(6) . . . . ?
O8 Eu1 N4 C23 66.0(6) . . . . ?
N1 Eu1 N4 C23 -124.4(6) . . . . ?
N3 Eu1 N4 C23 -9.7(5) . . . . ?
N2 Eu1 N4 C23 -83.1(6) . . . . ?
C31 Eu1 N4 C23 108.8(6) 2_556 . . . ?
C31 Eu1 N4 C23 83.3(6) . . . . ?
C12 N1 C1 C2 -3.1(14) . . . . ?
Eu1 N1 C1 C2 173.6(8) . . . . ?
N1 C1 C2 C3 0.1(17) . . . . ?
C1 C2 C3 C4 2.1(18) . . . . ?
C2 C3 C4 C5 179.4(11) . . . . ?
C2 C3 C4 C12 -1.3(16) . . . . ?
C3 C4 C5 C6 179.7(11) . . . . ?
C12 C4 C5 C6 0.4(16) . . . . ?
C4 C5 C6 C7 -1.1(17) . . . . ?
C5 C6 C7 C11 1.7(17) . . . . ?
C5 C6 C7 C8 -176.7(11) . . . . ?
C11 C7 C8 C9 2.9(17) . . . . ?
C6 C7 C8 C9 -178.6(12) . . . . ?
C7 C8 C9 C10 -3(2) . . . . ?
C11 N2 C10 C9 -1.3(16) . . . . ?
Eu1 N2 C10 C9 -170.5(9) . . . . ?
C8 C9 C10 N2 2.2(19) . . . . ?
C10 N2 C11 C7 1.4(14) . . . . ?
Eu1 N2 C11 C7 170.8(7) . . . . ?
C10 N2 C11 C12 -177.7(9) . . . . ?
Eu1 N2 C11 C12 -8.2(11) . . . . ?
C8 C7 C11 N2 -2.1(15) . . . . ?
C6 C7 C11 N2 179.3(9) . . . . ?
C8 C7 C11 C12 176.9(9) . . . . ?
C6 C7 C11 C12 -1.6(15) . . . . ?
C1 N1 C12 C4 4.0(13) . . . . ?
Eu1 N1 C12 C4 -172.7(6) . . . . ?
C1 N1 C12 C11 -178.2(8) . . . . ?
Eu1 N1 C12 C11 5.0(10) . . . . ?
C3 C4 C12 N1 -1.9(14) . . . . ?
C5 C4 C12 N1 177.5(9) . . . . ?
C3 C4 C12 C11 -179.6(9) . . . . ?
C5 C4 C12 C11 -0.3(14) . . . . ?
N2 C11 C12 N1 2.2(12) . . . . ?
C7 C11 C12 N1 -176.9(9) . . . . ?
N2 C11 C12 C4 -180.0(8) . . . . ?
C7 C11 C12 C4 0.9(13) . . . . ?
C24 N3 C13 C14 0.5(14) . . . . ?
Eu1 N3 C13 C14 -168.2(7) . . . . ?
N3 C13 C14 C15 -1.1(16) . . . . ?
C13 C14 C15 C16 1.1(16) . . . . ?
C14 C15 C16 C24 -0.5(15) . . . . ?
C14 C15 C16 C17 178.3(10) . . . . ?
C24 C16 C17 C18 -4.1(14) . . . . ?
C15 C16 C17 C18 177.1(10) . . . . ?
C16 C17 C18 C19 2.9(15) . . . . ?
C17 C18 C19 C20 177.4(10) . . . . ?
C17 C18 C19 C23 0.1(14) . . . . ?
C23 C19 C20 C21 0.8(14) . . . . ?
C18 C19 C20 C21 -176.5(9) . . . . ?
C19 C20 C21 C22 1.2(15) . . . . ?
C23 N4 C22 C21 4.8(14) . . . . ?
Eu1 N4 C22 C21 172.9(7) . . . . ?
C20 C21 C22 N4 -4.2(16) . . . . ?
C22 N4 C23 C19 -2.6(12) . . . . ?
Eu1 N4 C23 C19 -171.0(6) . . . . ?
C22 N4 C23 C24 176.4(8) . . . . ?
Eu1 N4 C23 C24 8.0(10) . . . . ?
C20 C19 C23 N4 -0.2(13) . . . . ?
C18 C19 C23 N4 177.2(8) . . . . ?
C20 C19 C23 C24 -179.2(8) . . . . ?
C18 C19 C23 C24 -1.8(12) . . . . ?
C13 N3 C24 C16 0.1(12) . . . . ?
Eu1 N3 C24 C16 169.3(6) . . . . ?
C13 N3 C24 C23 179.0(8) . . . . ?
Eu1 N3 C24 C23 -11.8(9) . . . . ?
C15 C16 C24 N3 -0.1(13) . . . . ?
C17 C16 C24 N3 -178.9(8) . . . . ?
C15 C16 C24 C23 -178.9(8) . . . . ?
C17 C16 C24 C23 2.2(12) . . . . ?
N4 C23 C24 N3 2.7(11) . . . . ?
C19 C23 C24 N3 -178.3(7) . . . . ?
N4 C23 C24 C16 -178.5(7) . . . . ?
C19 C23 C24 C16 0.6(12) . . . . ?
O1 S1 C25 C26 -15.6(8) . . . . ?
O3 S1 C25 C26 -137.7(6) . . . . ?
O2 S1 C25 C26 105.6(7) . . . . ?
C28 S1 C25 C26 73(11) 2_656 . . . ?
O1 S1 C25 C30 172.3(6) . . . . ?
O3 S1 C25 C30 50.1(8) . . . . ?
O2 S1 C25 C30 -66.5(8) . . . . ?
C28 S1 C25 C30 -99(11) 2_656 . . . ?
C30 C25 C26 C27 0.0 . . . . ?
S1 C25 C26 C27 -172.3(10) . . . . ?
C25 C26 C27 C28 0.0 . . . . ?
C26 C27 C28 C29 0.0 . . . . ?
C26 C27 C28 S1 178.3(11) . . . 2_656 ?
C27 C28 C29 C30 0.0 . . . . ?
S1 C28 C29 C30 -178.3(11) 2_656 . . . ?
C28 C29 C30 N5 173.8(15) . . . . ?
C28 C29 C30 C25 0.0 . . . . ?
C26 C25 C30 N5 -173.1(16) . . . . ?
S1 C25 C30 N5 -1.2(12) . . . . ?
C26 C25 C30 C29 0.0 . . . . ?
S1 C25 C30 C29 171.9(11) . . . . ?
Eu1 O8 C31 O7 176.0(7) . . . . ?
Eu1 O8 C31 C31 -5.0(12) . . . 2_556 ?
Eu1 O8 C31 Eu1 -169(3) . . . 2_556 ?
Eu1 O7 C31 O8 175.1(7) 2_556 . . . ?
Eu1 O7 C31 C31 -3.8(12) 2_556 . . 2_556 ?
Eu1 O7 C31 Eu1 -171(3) 2_556 . . . ?
O7 Eu1 C31 O8 -173.7(7) 2_556 . . . ?
O2 Eu1 C31 O8 89.1(6) . . . . ?
O4 Eu1 C31 O8 -130.4(6) . . . . ?
N1 Eu1 C31 O8 143.6(6) . . . . ?
N4 Eu1 C31 O8 -57.3(6) . . . . ?
N3 Eu1 C31 O8 7.0(7) . . . . ?
N2 Eu1 C31 O8 4.5(13) . . . . ?
C31 Eu1 C31 O8 -175.3(11) 2_556 . . . ?
O7 Eu1 C31 O7 169(3) 2_556 . . . ?
O2 Eu1 C31 O7 72(3) . . . . ?
O4 Eu1 C31 O7 -147(3) . . . . ?
O8 Eu1 C31 O7 -17(3) . . . . ?
N1 Eu1 C31 O7 127(3) . . . . ?
N4 Eu1 C31 O7 -74(3) . . . . ?
N3 Eu1 C31 O7 -10(3) . . . . ?
N2 Eu1 C31 O7 -12(4) . . . . ?
C31 Eu1 C31 O7 168(4) 2_556 . . . ?
O7 Eu1 C31 C31 1.6(5) 2_556 . . 2_556 ?
O2 Eu1 C31 C31 -95.6(6) . . . 2_556 ?
O4 Eu1 C31 C31 44.9(6) . . . 2_556 ?
O8 Eu1 C31 C31 175.3(11) . . . 2_556 ?
N1 Eu1 C31 C31 -41.1(7) . . . 2_556 ?
N4 Eu1 C31 C31 118.0(6) . . . 2_556 ?
N3 Eu1 C31 C31 -177.6(6) . . . 2_556 ?
N2 Eu1 C31 C31 179.8(6) . . . 2_556 ?
O7 Eu1 C31 Eu1 1.6(5) 2_556 . . 2_556 ?
O2 Eu1 C31 Eu1 -95.6(6) . . . 2_556 ?
O4 Eu1 C31 Eu1 44.9(6) . . . 2_556 ?
O8 Eu1 C31 Eu1 175.3(11) . . . 2_556 ?
N1 Eu1 C31 Eu1 -41.1(7) . . . 2_556 ?
N4 Eu1 C31 Eu1 118.0(6) . . . 2_556 ?
N3 Eu1 C31 Eu1 -177.6(6) . . . 2_556 ?
N2 Eu1 C31 Eu1 179.8(6) . . . 2_556 ?
C31 Eu1 C31 Eu1 0.0 2_556 . . 2_556 ?
O6 S3 C32 C33 111.4(7) . . . . ?
O5 S3 C32 C33 -14.0(8) . . . . ?
O4 S3 C32 C33 -132.3(5) . . . . ?
C35 S3 C32 C33 -16(8) 2 . . . ?
O6 S3 C32 C37 -65.2(9) . . . . ?
O5 S3 C32 C37 169.3(6) . . . . ?
O4 S3 C32 C37 51.0(8) . . . . ?
C35 S3 C32 C37 167(9) 2 . . . ?
C37 C32 C33 C34 0.0 . . . . ?
S3 C32 C33 C34 -176.8(9) . . . . ?
C32 C33 C34 C35 0.0 . . . . ?
C32 C33 C34 N6 179.6(16) . . . . ?
C33 C34 C35 C36 0.0 . . . . ?
N6 C34 C35 C36 -180(2) . . . . ?
C33 C34 C35 S3 -174.3(13) . . . 2 ?
N6 C34 C35 S3 6.1(14) . . . 2 ?
C34 C35 C36 C37 0.0 . . . . ?
S3 C35 C36 C37 173.7(15) 2 . . . ?
C35 C36 C37 C32 0.0 . . . . ?
C33 C32 C37 C36 0.0 . . . . ?
S3 C32 C37 C36 176.6(9) . . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.604
_refine_diff_density_min         -1.217
_refine_diff_density_rms         0.168


_database_code_depnum_ccdc_archive 'CCDC 981692'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C31 H21 Gd N5 O8 S2'
_chemical_formula_weight         812.90

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   10.5440(14)
_cell_length_b                   10.5785(15)
_cell_length_c                   15.068(2)
_cell_angle_alpha                92.469(3)
_cell_angle_beta                 110.420(2)
_cell_angle_gamma                107.942(3)
_cell_volume                     1476.9(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.828
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             804
_exptl_absorpt_coefficient_mu    2.450
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.5997
_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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7454
_diffrn_reflns_av_R_equivalents  0.0480
_diffrn_reflns_av_sigmaI/netI    0.1086
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.12
_diffrn_reflns_theta_max         25.25
_reflns_number_total             5313
_reflns_number_gt                4036
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_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          
;
 Restraints: DELU,SIMU and ISOR restraints for the disordered H2N-BDS ligand,
 to control the displacement parameters of overlapping components. Such
 restraints are often required for disorder components that interpenetrate each
 other, since the electron density of the disordered atoms strongly overlap and
 can not be resolved satisfactorily in free refinement. Restraints are gentler
 and more flexible than rigid constraints. 
;

_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)+(0.0473P)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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5313
_refine_ls_number_parameters     463
_refine_ls_number_restraints     198
_refine_ls_R_factor_all          0.0827
_refine_ls_R_factor_gt           0.0568
_refine_ls_wR_factor_ref         0.1215
_refine_ls_wR_factor_gt          0.1091
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_restrained_S_all      0.997
_refine_ls_shift/su_max          0.004
_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 0.4580(8) 0.0483(8) -0.0195(6) 0.0230(18) Uani 1 1 d . . .
C2 C 0.8362(10) 0.3806(9) 0.1684(6) 0.039(2) Uani 1 1 d . . .
H2A H 0.8830 0.3181 0.1820 0.047 Uiso 1 1 calc R . .
C3 C 0.9034(10) 0.4995(10) 0.1397(7) 0.051(3) Uani 1 1 d . . .
H3A H 0.9935 0.5161 0.1366 0.061 Uiso 1 1 calc R . .
C4 C 0.8339(10) 0.5897(9) 0.1166(7) 0.046(3) Uani 1 1 d . . .
H4A H 0.8751 0.6680 0.0961 0.055 Uiso 1 1 calc R . .
C5 C 0.6987(9) 0.5631(8) 0.1241(6) 0.034(2) Uani 1 1 d . . .
C6 C 0.6183(10) 0.6486(9) 0.0965(6) 0.042(2) Uani 1 1 d . . .
H6A H 0.6584 0.7277 0.0763 0.050 Uiso 1 1 calc R . .
C7 C 0.4871(10) 0.6215(9) 0.0978(7) 0.043(2) Uani 1 1 d . . .
H7A H 0.4361 0.6795 0.0774 0.051 Uiso 1 1 calc R . .
C8 C 0.4257(9) 0.5023(8) 0.1309(6) 0.035(2) Uani 1 1 d . . .
C9 C 0.2899(10) 0.4685(10) 0.1394(7) 0.046(3) Uani 1 1 d . . .
H9A H 0.2363 0.5251 0.1223 0.055 Uiso 1 1 calc R . .
C10 C 0.2385(10) 0.3563(10) 0.1715(7) 0.047(3) Uani 1 1 d . . .
H10A H 0.1503 0.3355 0.1782 0.056 Uiso 1 1 calc R . .
C11 C 0.3190(10) 0.2692(9) 0.1955(7) 0.041(2) Uani 1 1 d . . .
H11A H 0.2801 0.1898 0.2158 0.049 Uiso 1 1 calc R . .
C12 C 0.5028(9) 0.4136(8) 0.1596(5) 0.0271(19) Uani 1 1 d . . .
C13 C 0.6404(8) 0.4435(8) 0.1527(6) 0.0290(19) Uani 1 1 d . . .
C14 C 0.6720(11) 0.3649(10) 0.4060(8) 0.059(3) Uani 1 1 d . . .
H14A H 0.6581 0.4173 0.3579 0.071 Uiso 1 1 calc R . .
C15 C 0.7247(12) 0.4268(12) 0.5010(9) 0.074(4) Uani 1 1 d . . .
H15A H 0.7434 0.5185 0.5162 0.089 Uiso 1 1 calc R . .
C16 C 0.7484(12) 0.3502(15) 0.5716(8) 0.074(4) Uani 1 1 d . . .
H16A H 0.7862 0.3910 0.6356 0.089 Uiso 1 1 calc R . .
C17 C 0.7172(11) 0.2123(13) 0.5496(7) 0.055(3) Uani 1 1 d . . .
C18 C 0.7377(11) 0.1276(15) 0.6198(7) 0.070(4) Uani 1 1 d . . .
H18A H 0.7706 0.1641 0.6844 0.084 Uiso 1 1 calc R . .
C19 C 0.7108(12) -0.0019(15) 0.5953(8) 0.067(3) Uani 1 1 d . . .
H19A H 0.7262 -0.0552 0.6428 0.080 Uiso 1 1 calc R . .
C20 C 0.6588(10) -0.0607(11) 0.4976(6) 0.043(2) Uani 1 1 d . . .
C21 C 0.6304(11) -0.1962(12) 0.4697(7) 0.055(3) Uani 1 1 d . . .
H21A H 0.6474 -0.2508 0.5161 0.066 Uiso 1 1 calc R . .
C22 C 0.5772(11) -0.2507(11) 0.3742(8) 0.059(3) Uani 1 1 d . . .
H22A H 0.5535 -0.3425 0.3549 0.071 Uiso 1 1 calc R . .
C23 C 0.5595(10) -0.1634(10) 0.3059(7) 0.047(3) Uani 1 1 d . . .
H23A H 0.5266 -0.1982 0.2411 0.056 Uiso 1 1 calc R . .
C24 C 0.6358(8) 0.0167(9) 0.4258(6) 0.032(2) Uani 1 1 d . . .
C25 C 0.6635(9) 0.1566(10) 0.4526(6) 0.038(2) Uani 1 1 d . . .
C26 C 0.096(3) -0.052(2) 0.0474(19) 0.018(4) Uani 0.50 1 d PGU A -1
C27 C 0.019(3) -0.015(2) 0.0957(19) 0.027(5) Uani 0.50 1 d PGU A -1
C28 C -0.077(3) 0.049(2) 0.052(2) 0.029(5) Uani 0.50 1 d PGU A -1
H28 H -0.1294 0.0735 0.0843 0.035 Uiso 0.50 1 calc PR A -1
C29 C -0.096(3) 0.077(2) -0.040(2) 0.030(5) Uani 0.50 1 d PGU . -1
C30 C -0.019(3) 0.041(2) -0.0883(19) 0.022(5) Uani 0.50 1 d PGU A -1
H30 H -0.0310 0.0600 -0.1499 0.027 Uiso 0.50 1 calc PR A -1
C31 C 0.078(3) -0.024(2) -0.0446(19) 0.021(4) Uani 0.50 1 d PGU A -1
H31 H 0.1297 -0.0479 -0.0769 0.025 Uiso 0.50 1 calc PR A -1
N5 N 0.0334(15) -0.0451(15) 0.1807(10) 0.042(4) Uani 0.50 1 d PU A -1
H5A H 0.0911 -0.0872 0.2071 0.051 Uiso 0.50 1 calc PR A -1
H5B H -0.0147 -0.0226 0.2105 0.051 Uiso 0.50 1 calc PR A -1
C32 C 0.982(2) 0.1072(17) 0.4411(15) 0.036(5) Uani 0.50 1 d PGU B -1
C33 C 0.948(3) -0.0279(18) 0.4065(15) 0.047(5) Uani 0.50 1 d PGU B -1
C34 C 0.968(2) -0.1177(16) 0.4703(16) 0.039(5) Uani 0.50 1 d PGU B -1
H34 H 0.9454 -0.2081 0.4471 0.047 Uiso 0.50 1 calc PR B -1
C35 C 1.023(2) -0.0723(15) 0.5686(16) 0.028(4) Uani 0.50 1 d PGU . -1
C36 C 1.057(2) 0.0628(16) 0.6032(14) 0.030(4) Uani 0.50 1 d PGU B -1
H36 H 1.0934 0.0931 0.6690 0.037 Uiso 0.50 1 calc PR B -1
C37 C 1.037(2) 0.1525(15) 0.5394(15) 0.033(4) Uani 0.50 1 d PGU B -1
H37 H 1.0594 0.2429 0.5626 0.039 Uiso 0.50 1 calc PR B -1
N6 N 0.885(2) -0.105(2) 0.3004(14) 0.089(6) Uani 0.50 1 d PU B -1
H6B H 0.8681 -0.1899 0.2896 0.107 Uiso 0.50 1 calc PR B -1
H6C H 0.8664 -0.0616 0.2531 0.107 Uiso 0.50 1 calc PR B -1
Gd1 Gd 0.57691(4) 0.12488(4) 0.20741(3) 0.02373(14) Uani 1 1 d . . .
N1 N 0.7093(7) 0.3523(6) 0.1772(5) 0.0310(17) Uani 1 1 d . . .
N2 N 0.4475(7) 0.2956(6) 0.1905(5) 0.0294(16) Uani 1 1 d . . .
N3 N 0.6406(7) 0.2329(7) 0.3811(5) 0.0378(18) Uani 1 1 d . . .
N4 N 0.5886(7) -0.0322(7) 0.3321(5) 0.0324(17) Uani 1 1 d . . .
O1 O 0.4604(6) 0.1335(5) 0.0416(4) 0.0290(13) Uani 1 1 d . . .
O2 O 0.3960(6) 0.0323(5) -0.1091(4) 0.0311(13) Uani 1 1 d . . .
O3 O 0.3442(5) -0.0244(5) 0.1730(4) 0.0316(13) Uani 1 1 d . A .
O4 O 0.1613(6) -0.2414(6) 0.1452(5) 0.0437(16) Uani 1 1 d . A .
O5 O 0.2692(6) -0.1834(6) 0.0275(4) 0.0409(15) Uani 1 1 d . A .
O6 O 0.8190(6) 0.1428(6) 0.2810(4) 0.0411(16) Uani 1 1 d . B .
O7 O 0.9799(9) 0.3268(7) 0.4089(5) 0.081(3) Uani 1 1 d . B .
O8 O 1.0717(8) 0.2121(10) 0.3146(6) 0.090(3) Uani 1 1 d . B .
S1 S 0.2259(2) -0.1375(2) 0.09971(16) 0.0316(5) Uani 1 1 d . . .
S2 S 0.9645(3) 0.2029(3) 0.35451(19) 0.0496(7) 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 O1 1.248(9) . ?
C1 O2 1.255(9) . ?
C1 C1 1.556(14) 2_655 ?
C2 N1 1.333(10) . ?
C2 C3 1.409(12) . ?
C2 H2A 0.9300 . ?
C3 C4 1.359(12) . ?
C3 H3A 0.9300 . ?
C4 C5 1.412(12) . ?
C4 H4A 0.9300 . ?
C5 C13 1.386(11) . ?
C5 C6 1.402(12) . ?
C6 C7 1.331(12) . ?
C6 H6A 0.9300 . ?
C7 C8 1.427(12) . ?
C7 H7A 0.9300 . ?
C8 C12 1.410(11) . ?
C8 C9 1.417(12) . ?
C9 C10 1.331(12) . ?
C9 H9A 0.9300 . ?
C10 C11 1.413(12) . ?
C10 H10A 0.9300 . ?
C11 N2 1.327(10) . ?
C11 H11A 0.9300 . ?
C12 N2 1.381(10) . ?
C12 C13 1.428(11) . ?
C13 N1 1.368(9) . ?
C14 N3 1.335(11) . ?
C14 C15 1.388(14) . ?
C14 H14A 0.9300 . ?
C15 C16 1.366(16) . ?
C15 H15A 0.9300 . ?
C16 C17 1.389(15) . ?
C16 H16A 0.9300 . ?
C17 C25 1.396(12) . ?
C17 C18 1.418(15) . ?
C18 C19 1.318(16) . ?
C18 H18A 0.9300 . ?
C19 C20 1.416(14) . ?
C19 H19A 0.9300 . ?
C20 C24 1.384(11) . ?
C20 C21 1.384(14) . ?
C21 C22 1.373(14) . ?
C21 H21A 0.9300 . ?
C22 C23 1.415(12) . ?
C22 H22A 0.9300 . ?
C23 N4 1.334(11) . ?
C23 H23A 0.9300 . ?
C24 N4 1.340(10) . ?
C24 C25 1.428(12) . ?
C25 N3 1.372(11) . ?
C26 C27 1.3900 . ?
C26 C31 1.3900 . ?
C26 S1 1.84(2) . ?
C27 N5 1.30(3) . ?
C27 C28 1.3900 . ?
C28 C29 1.3900 . ?
C28 H28 0.9300 . ?
C29 C30 1.3900 . ?
C29 S1 1.68(2) 2 ?
C30 C31 1.3900 . ?
C30 H30 0.9300 . ?
C31 H31 0.9300 . ?
N5 H5A 0.8600 . ?
N5 H5B 0.8600 . ?
C32 C33 1.3900 . ?
C32 C37 1.3900 . ?
C32 S2 1.68(2) . ?
C33 C34 1.3900 . ?
C33 N6 1.57(3) . ?
C34 C35 1.3900 . ?
C34 H34 0.9300 . ?
C35 C36 1.3900 . ?
C35 S2 1.847(19) 2_756 ?
C36 C37 1.3900 . ?
C36 H36 0.9300 . ?
C37 H37 0.9300 . ?
N6 H6B 0.8600 . ?
N6 H6C 0.8600 . ?
Gd1 O2 2.327(5) 2_655 ?
Gd1 O3 2.332(5) . ?
Gd1 O6 2.343(5) . ?
Gd1 O1 2.389(5) . ?
Gd1 N1 2.532(6) . ?
Gd1 N2 2.550(7) . ?
Gd1 N4 2.558(7) . ?
Gd1 N3 2.579(7) . ?
O2 Gd1 2.327(5) 2_655 ?
O3 S1 1.487(5) . ?
O4 S1 1.439(6) . ?
O5 S1 1.437(6) . ?
O6 S2 1.462(6) . ?
O7 S2 1.449(8) . ?
O8 S2 1.436(7) . ?
S1 C29 1.68(2) 2 ?
S2 C35 1.85(2) 2_756 ?

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 C1 O2 127.2(7) . . ?
O1 C1 C1 116.6(9) . 2_655 ?
O2 C1 C1 116.2(8) . 2_655 ?
N1 C2 C3 123.8(8) . . ?
N1 C2 H2A 118.1 . . ?
C3 C2 H2A 118.1 . . ?
C4 C3 C2 118.7(9) . . ?
C4 C3 H3A 120.7 . . ?
C2 C3 H3A 120.7 . . ?
C3 C4 C5 119.3(8) . . ?
C3 C4 H4A 120.3 . . ?
C5 C4 H4A 120.3 . . ?
C13 C5 C6 119.7(8) . . ?
C13 C5 C4 118.1(8) . . ?
C6 C5 C4 122.0(8) . . ?
C7 C6 C5 122.9(9) . . ?
C7 C6 H6A 118.5 . . ?
C5 C6 H6A 118.5 . . ?
C6 C7 C8 119.2(8) . . ?
C6 C7 H7A 120.4 . . ?
C8 C7 H7A 120.4 . . ?
C12 C8 C9 117.0(8) . . ?
C12 C8 C7 119.8(8) . . ?
C9 C8 C7 123.2(8) . . ?
C10 C9 C8 120.5(8) . . ?
C10 C9 H9A 119.7 . . ?
C8 C9 H9A 119.7 . . ?
C9 C10 C11 119.5(9) . . ?
C9 C10 H10A 120.2 . . ?
C11 C10 H10A 120.2 . . ?
N2 C11 C10 123.0(8) . . ?
N2 C11 H11A 118.5 . . ?
C10 C11 H11A 118.5 . . ?
N2 C12 C8 122.3(8) . . ?
N2 C12 C13 118.5(7) . . ?
C8 C12 C13 119.1(8) . . ?
N1 C13 C5 123.3(7) . . ?
N1 C13 C12 117.5(7) . . ?
C5 C13 C12 119.1(7) . . ?
N3 C14 C15 122.4(11) . . ?
N3 C14 H14A 118.8 . . ?
C15 C14 H14A 118.8 . . ?
C16 C15 C14 118.6(11) . . ?
C16 C15 H15A 120.7 . . ?
C14 C15 H15A 120.7 . . ?
C15 C16 C17 121.2(10) . . ?
C15 C16 H16A 119.4 . . ?
C17 C16 H16A 119.4 . . ?
C16 C17 C25 117.1(11) . . ?
C16 C17 C18 123.6(11) . . ?
C25 C17 C18 119.3(11) . . ?
C19 C18 C17 121.3(11) . . ?
C19 C18 H18A 119.4 . . ?
C17 C18 H18A 119.4 . . ?
C18 C19 C20 120.7(11) . . ?
C18 C19 H19A 119.7 . . ?
C20 C19 H19A 119.7 . . ?
C24 C20 C21 117.3(9) . . ?
C24 C20 C19 120.7(10) . . ?
C21 C20 C19 122.0(10) . . ?
C22 C21 C20 120.5(9) . . ?
C22 C21 H21A 119.7 . . ?
C20 C21 H21A 119.7 . . ?
C21 C22 C23 118.2(10) . . ?
C21 C22 H22A 120.9 . . ?
C23 C22 H22A 120.9 . . ?
N4 C23 C22 121.7(10) . . ?
N4 C23 H23A 119.1 . . ?
C22 C23 H23A 119.1 . . ?
N4 C24 C20 123.7(9) . . ?
N4 C24 C25 117.8(7) . . ?
C20 C24 C25 118.4(8) . . ?
N3 C25 C17 122.2(10) . . ?
N3 C25 C24 118.2(8) . . ?
C17 C25 C24 119.6(9) . . ?
C27 C26 C31 120.0 . . ?
C27 C26 S1 122.9(9) . . ?
C31 C26 S1 117.1(9) . . ?
N5 C27 C26 120.0(13) . . ?
N5 C27 C28 120.0(14) . . ?
C26 C27 C28 120.0 . . ?
C27 C28 C29 120.0 . . ?
C27 C28 H28 120.0 . . ?
C29 C28 H28 120.0 . . ?
C30 C29 C28 120.0 . . ?
C30 C29 S1 118.7(12) . 2 ?
C28 C29 S1 120.9(12) . 2 ?
C31 C30 C29 120.0 . . ?
C31 C30 H30 120.0 . . ?
C29 C30 H30 120.0 . . ?
C30 C31 C26 120.0 . . ?
C30 C31 H31 120.0 . . ?
C26 C31 H31 120.0 . . ?
C27 N5 H5A 120.0 . . ?
C27 N5 H5B 120.0 . . ?
H5A N5 H5B 120.0 . . ?
C33 C32 C37 120.0 . . ?
C33 C32 S2 113.3(8) . . ?
C37 C32 S2 126.4(8) . . ?
C34 C33 C32 120.0 . . ?
C34 C33 N6 109.7(13) . . ?
C32 C33 N6 130.3(13) . . ?
C35 C34 C33 120.0 . . ?
C35 C34 H34 120.0 . . ?
C33 C34 H34 120.0 . . ?
C34 C35 C36 120.0 . . ?
C34 C35 S2 115.8(8) . 2_756 ?
C36 C35 S2 124.1(8) . 2_756 ?
C37 C36 C35 120.0 . . ?
C37 C36 H36 120.0 . . ?
C35 C36 H36 120.0 . . ?
C36 C37 C32 120.0 . . ?
C36 C37 H37 120.0 . . ?
C32 C37 H37 120.0 . . ?
C33 N6 H6B 120.0 . . ?
C33 N6 H6C 120.0 . . ?
H6B N6 H6C 120.0 . . ?
O2 Gd1 O3 87.66(19) 2_655 . ?
O2 Gd1 O6 75.5(2) 2_655 . ?
O3 Gd1 O6 141.3(2) . . ?
O2 Gd1 O1 68.89(18) 2_655 . ?
O3 Gd1 O1 78.52(18) . . ?
O6 Gd1 O1 124.51(19) . . ?
O2 Gd1 N1 105.1(2) 2_655 . ?
O3 Gd1 N1 141.3(2) . . ?
O6 Gd1 N1 77.4(2) . . ?
O1 Gd1 N1 72.7(2) . . ?
O2 Gd1 N2 138.66(19) 2_655 . ?
O3 Gd1 N2 81.4(2) . . ?
O6 Gd1 N2 133.2(2) . . ?
O1 Gd1 N2 69.88(19) . . ?
N1 Gd1 N2 64.7(2) . . ?
O2 Gd1 N4 88.8(2) 2_655 . ?
O3 Gd1 N4 71.7(2) . . ?
O6 Gd1 N4 73.3(2) . . ?
O1 Gd1 N4 143.4(2) . . ?
N1 Gd1 N4 143.1(2) . . ?
N2 Gd1 N4 124.3(2) . . ?
O2 Gd1 N3 146.3(2) 2_655 . ?
O3 Gd1 N3 100.1(2) . . ?
O6 Gd1 N3 78.3(2) . . ?
O1 Gd1 N3 144.7(2) . . ?
N1 Gd1 N3 89.2(2) . . ?
N2 Gd1 N3 75.0(2) . . ?
N4 Gd1 N3 63.5(2) . . ?
C2 N1 C13 116.6(7) . . ?
C2 N1 Gd1 122.7(5) . . ?
C13 N1 Gd1 119.7(5) . . ?
C11 N2 C12 117.5(7) . . ?
C11 N2 Gd1 123.5(5) . . ?
C12 N2 Gd1 118.1(5) . . ?
C14 N3 C25 118.5(8) . . ?
C14 N3 Gd1 122.0(7) . . ?
C25 N3 Gd1 118.8(6) . . ?
C23 N4 C24 118.5(8) . . ?
C23 N4 Gd1 120.3(6) . . ?
C24 N4 Gd1 120.9(6) . . ?
C1 O1 Gd1 118.0(5) . . ?
C1 O2 Gd1 120.1(5) . 2_655 ?
S1 O3 Gd1 142.2(3) . . ?
S2 O6 Gd1 153.1(4) . . ?
O5 S1 O4 115.0(4) . . ?
O5 S1 O3 112.4(3) . . ?
O4 S1 O3 110.6(4) . . ?
O5 S1 C29 104.8(10) . 2 ?
O4 S1 C29 105.9(9) . 2 ?
O3 S1 C29 107.4(8) . 2 ?
O5 S1 C26 110.0(9) . . ?
O4 S1 C26 107.7(8) . . ?
O3 S1 C26 99.9(7) . . ?
C29 S1 C26 7.7(15) 2 . ?
O8 S2 O7 115.7(5) . . ?
O8 S2 O6 111.2(5) . . ?
O7 S2 O6 110.8(4) . . ?
O8 S2 C32 110.2(9) . . ?
O7 S2 C32 99.8(7) . . ?
O6 S2 C32 108.3(8) . . ?
O8 S2 C35 104.7(8) . 2_756 ?
O7 S2 C35 110.7(7) . 2_756 ?
O6 S2 C35 102.8(7) . 2_756 ?
C32 S2 C35 10.8(12) . 2_756 ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        25.25
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         1.393
_refine_diff_density_min         -0.693
_refine_diff_density_rms         0.165

_database_code_depnum_ccdc_archive 'CCDC 981693'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C31 H21 N5 O8 S2 Tb'
_chemical_formula_weight         814.57

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'
Tb Tb -0.1723 4.1537 '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                   10.5381(14)
_cell_length_b                   10.5712(13)
_cell_length_c                   15.041(2)
_cell_angle_alpha                75.114(4)
_cell_angle_beta                 69.497(2)
_cell_angle_gamma                72.006(2)
_cell_volume                     1471.7(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    745
_cell_measurement_theta_min      0.00
_cell_measurement_theta_max      0.00

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.838
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             806
_exptl_absorpt_coefficient_mu    2.608
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.6235
_exptl_absorpt_correction_T_max  0.9259
_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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            7270
_diffrn_reflns_av_R_equivalents  0.0531
_diffrn_reflns_av_sigmaI/netI    0.1173
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.05
_diffrn_reflns_theta_max         25.00
_reflns_number_total             5147
_reflns_number_gt                3802
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Restraints: DELU,SIMU and ISOR restraints for the disordered H2N-BDS ligand,
 to control the displacement parameters of overlapping components. Such
 restraints are often required for disorder components that interpenetrate each
 other, since the electron density of the disordered atoms strongly overlap and
 can not be resolved satisfactorily in free refinement. Restraints are gentler
 and more flexible than rigid constraints.  
;

_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)+(0.0533P)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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5147
_refine_ls_number_parameters     463
_refine_ls_number_restraints     204
_refine_ls_R_factor_all          0.0875
_refine_ls_R_factor_gt           0.0583
_refine_ls_wR_factor_ref         0.1308
_refine_ls_wR_factor_gt          0.1155
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_restrained_S_all      0.983
_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 0.12934(5) 0.12487(5) 0.29327(3) 0.02364(15) Uani 1 1 d . . 4
S1 S 0.3733(2) -0.1369(2) 0.39967(17) 0.0304(6) Uani 1 1 d . A 4
S3 S -0.1100(3) 0.2031(3) 0.1464(2) 0.0495(8) Uani 1 1 d . B 4
O1 O 0.2575(7) -0.1836(6) 0.4728(5) 0.0395(17) Uani 1 1 d . A 4
O2 O 0.3272(6) -0.0241(6) 0.3274(4) 0.0300(15) Uani 1 1 d . A 4
O3 O 0.4836(7) -0.2405(7) 0.3525(5) 0.0430(18) Uani 1 1 d . A 4
O4 O -0.0372(6) 0.1433(7) 0.2188(5) 0.0395(17) Uani 1 1 d . B 4
O5 O -0.0733(10) 0.3285(9) 0.0927(6) 0.078(3) Uani 1 1 d . B 4
O6 O -0.2559(8) 0.2118(10) 0.1859(6) 0.086(3) Uani 1 1 d . B 4
O7 O -0.0055(6) 0.0322(6) 0.6100(4) 0.0317(15) Uani 1 1 d . . 4
O8 O 0.0805(6) 0.1337(6) 0.4587(4) 0.0278(14) Uani 1 1 d . . 4
N1 N 0.2411(7) -0.0316(8) 0.1694(5) 0.0296(18) Uani 1 1 d . C 4
N2 N 0.2378(8) 0.2330(9) 0.1207(6) 0.039(2) Uani 1 1 d . C 4
N3 N 0.2444(8) 0.2951(7) 0.3100(5) 0.0291(18) Uani 1 1 d . D 4
N4 N -0.0336(7) 0.3521(7) 0.3241(5) 0.0256(17) Uani 1 1 d . D 4
C1 C 0.2469(12) -0.1627(11) 0.1943(8) 0.049(3) Uani 1 1 d . C 4
H1A H 0.2190 -0.1981 0.2595 0.059 Uiso 1 1 calc R C 4
C2 C 0.2928(12) -0.2508(12) 0.1278(9) 0.055(3) Uani 1 1 d . C 4
H2A H 0.2909 -0.3412 0.1481 0.066 Uiso 1 1 calc R C 4
C3 C 0.3408(12) -0.2000(14) 0.0318(9) 0.060(4) Uani 1 1 d . C 4
H3A H 0.3757 -0.2569 -0.0136 0.072 Uiso 1 1 calc R C 4
C4 C 0.3370(10) -0.0620(14) 0.0025(7) 0.046(3) Uani 1 1 d . C 4
C5 C 0.3851(11) -0.0012(16) -0.0934(9) 0.060(4) Uani 1 1 d . C 4
H5A H 0.4203 -0.0540 -0.1416 0.073 Uiso 1 1 calc R C 4
C6 C 0.3820(12) 0.1296(17) -0.1177(9) 0.067(4) Uani 1 1 d . C 4
H6A H 0.4150 0.1662 -0.1822 0.081 Uiso 1 1 calc R C 4
C7 C 0.3296(11) 0.2134(15) -0.0477(8) 0.053(3) Uani 1 1 d . C 4
C8 C 0.3197(14) 0.3535(17) -0.0691(10) 0.076(4) Uani 1 1 d . C 4
H8A H 0.3449 0.3942 -0.1332 0.091 Uiso 1 1 calc R C 4
C9 C 0.2754(15) 0.4304(15) -0.0005(10) 0.075(4) Uani 1 1 d . C 4
H9A H 0.2716 0.5222 -0.0152 0.090 Uiso 1 1 calc R C 4
C10 C 0.2350(12) 0.3633(12) 0.0951(8) 0.055(3) Uani 1 1 d . C 4
H10A H 0.1787 0.4328 0.1357 0.066 Uiso 1 1 d R C 4
C11 C 0.2863(9) 0.1587(11) 0.0493(7) 0.038(3) Uani 1 1 d . C 4
C12 C 0.2879(9) 0.0188(10) 0.0759(7) 0.033(2) Uani 1 1 d . C 4
C13 C 0.3766(9) 0.2688(10) 0.3036(7) 0.035(2) Uani 1 1 d . D 4
H13A H 0.4351 0.1898 0.2821 0.042 Uiso 1 1 calc R D 4
C14 C 0.4339(11) 0.3520(11) 0.3270(9) 0.055(3) Uani 1 1 d . D 4
H14A H 0.5289 0.3294 0.3205 0.066 Uiso 1 1 calc R D 4
C15 C 0.3493(11) 0.4684(11) 0.3601(8) 0.045(3) Uani 1 1 d . D 4
H15A H 0.3862 0.5253 0.3767 0.054 Uiso 1 1 calc R D 4
C16 C 0.2052(10) 0.5009(9) 0.3688(6) 0.031(2) Uani 1 1 d . D 4
C17 C 0.1090(10) 0.6192(10) 0.4045(7) 0.038(3) Uani 1 1 d . D 4
H17A H 0.1473 0.6880 0.4047 0.046 Uiso 1 1 d R D 4
C18 C -0.0225(11) 0.6508(10) 0.4046(7) 0.040(3) Uani 1 1 d . D 4
H18A H -0.0807 0.7320 0.4228 0.049 Uiso 1 1 calc R D 4
C19 C -0.0775(10) 0.5641(9) 0.3777(6) 0.030(2) Uani 1 1 d . D 4
C20 C -0.2170(11) 0.5881(10) 0.3831(7) 0.041(3) Uani 1 1 d . D 4
H20A H -0.2790 0.6672 0.4023 0.049 Uiso 1 1 calc R D 4
C21 C -0.2644(11) 0.4983(11) 0.3608(8) 0.048(3) Uani 1 1 d . D 4
H21A H -0.3580 0.5149 0.3645 0.057 Uiso 1 1 calc R D 4
C22 C -0.1691(10) 0.3798(10) 0.3320(7) 0.035(2) Uani 1 1 d . D 4
H22A H -0.2026 0.3147 0.3054 0.041 Uiso 1 1 d R D 4
C23 C 0.0120(9) 0.4429(9) 0.3468(6) 0.026(2) Uani 1 1 d . D 4
C24 C 0.1579(9) 0.4111(9) 0.3417(6) 0.028(2) Uani 1 1 d . D 4
C25 C 0.444(3) -0.076(3) 0.458(2) 0.030(5) Uani 0.50 1 d PGU E -1
C26 C 0.370(3) -0.047(2) 0.550(2) 0.031(5) Uani 0.50 1 d PGU E -1
H26 H 0.2847 -0.0698 0.5816 0.037 Uiso 0.50 1 calc PR E -1
C27 C 0.422(3) 0.017(2) 0.594(2) 0.023(5) Uani 0.50 1 d PGU E -1
H27 H 0.3729 0.0371 0.6552 0.028 Uiso 0.50 1 calc PR E -1
C28 C 0.549(3) 0.052(2) 0.546(2) 0.022(5) Uani 0.50 1 d PGU E -1
C29 C 0.623(3) 0.022(2) 0.454(2) 0.030(5) Uani 0.50 1 d PGU E -1
H29 H 0.7083 0.0456 0.4221 0.035 Uiso 0.50 1 calc PR E -1
C30 C 0.570(3) -0.042(3) 0.410(2) 0.031(6) Uani 0.50 1 d PGU E -1
N5 N 0.6456(17) -0.0522(17) 0.3201(11) 0.045(4) Uani 0.50 1 d PU E -1
H5B H 0.7190 -0.0209 0.2949 0.053 Uiso 0.50 1 calc PR E -1
H5C H 0.6211 -0.0904 0.2868 0.053 Uiso 0.50 1 calc PR E -1
C31 C 0.0223(9) 0.0485(9) 0.5187(7) 0.028(2) Uani 1 1 d U . .
C32 C -0.046(2) 0.0716(16) 0.0715(15) 0.025(4) Uani 0.50 1 d PGU F -2
C33 C -0.002(3) 0.1180(17) -0.0269(15) 0.033(5) Uani 0.50 1 d PGU F -2
H33 H -0.0015 0.2085 -0.0494 0.040 Uiso 0.50 1 calc PR F -2
C34 C 0.042(3) 0.0291(19) -0.0916(14) 0.045(5) Uani 0.50 1 d PGU F -2
C35 C 0.042(3) -0.1062(19) -0.0580(15) 0.035(5) Uani 0.50 1 d PGU F -2
C36 C -0.002(2) -0.1526(16) 0.0404(15) 0.035(5) Uani 0.50 1 d PGU F -2
H36 H -0.0025 -0.2432 0.0629 0.042 Uiso 0.50 1 calc PR F -2
C37 C -0.046(2) -0.0637(17) 0.1051(14) 0.029(5) Uani 0.50 1 d PGU F -2
H37 H -0.0755 -0.0948 0.1709 0.035 Uiso 0.50 1 calc PR F -2
N6 N 0.085(2) 0.102(2) -0.1975(15) 0.085(6) Uani 0.50 1 d PU F -2
H6B H 0.1136 0.0574 -0.2441 0.101 Uiso 0.50 1 calc PR F -2
H6C H 0.0810 0.1871 -0.2094 0.101 Uiso 0.50 1 calc PR F -2


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

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 O7 2.312(6) 2_556 ?
Tb1 O2 2.324(6) . ?
Tb1 O4 2.329(6) . ?
Tb1 O8 2.378(6) . ?
Tb1 N4 2.530(7) . ?
Tb1 N1 2.537(7) . ?
Tb1 N2 2.561(8) . ?
Tb1 N3 2.562(7) . ?
S1 O3 1.446(6) . ?
S1 O1 1.448(7) . ?
S1 O2 1.478(6) . ?
S3 O6 1.423(8) . ?
S3 O5 1.451(9) . ?
S3 O4 1.452(6) . ?
O7 C31 1.277(10) . ?
O7 Tb1 2.312(6) 2_556 ?
O8 C31 1.240(10) . ?
N1 C1 1.328(12) . ?
N1 C12 1.340(11) . ?
N2 C10 1.325(13) . ?
N2 C11 1.353(12) . ?
N3 C13 1.307(11) . ?
N3 C24 1.367(10) . ?
N4 C22 1.334(11) . ?
N4 C23 1.356(10) . ?
C1 C2 1.400(14) . ?
C1 H1A 0.9300 . ?
C2 C3 1.373(16) . ?
C2 H2A 0.9300 . ?
C3 C4 1.403(16) . ?
C3 H3A 0.9300 . ?
C4 C5 1.401(16) . ?
C4 C12 1.424(13) . ?
C5 C6 1.329(17) . ?
C5 H5A 0.9300 . ?
C6 C7 1.403(16) . ?
C6 H6A 0.9300 . ?
C7 C11 1.390(14) . ?
C7 C8 1.411(17) . ?
C8 C9 1.342(18) . ?
C8 H8A 0.9300 . ?
C9 C10 1.409(16) . ?
C9 H9A 0.9300 . ?
C10 H10A 0.9862 . ?
C11 C12 1.426(14) . ?
C13 C14 1.377(13) . ?
C13 H13A 0.9300 . ?
C14 C15 1.373(13) . ?
C14 H14A 0.9300 . ?
C15 C16 1.415(13) . ?
C15 H15A 0.9300 . ?
C16 C24 1.396(12) . ?
C16 C17 1.436(12) . ?
C17 C18 1.321(13) . ?
C17 H17A 0.9352 . ?
C18 C19 1.423(13) . ?
C18 H18A 0.9300 . ?
C19 C20 1.389(13) . ?
C19 C23 1.413(11) . ?
C20 C21 1.355(13) . ?
C20 H20A 0.9300 . ?
C21 C22 1.401(12) . ?
C21 H21A 0.9300 . ?
C22 H22A 1.0717 . ?
C23 C24 1.447(12) . ?
C25 C26 1.3900 . ?
C25 C30 1.3900 . ?
C26 C27 1.3900 . ?
C26 H26 0.9300 . ?
C27 C28 1.3900 . ?
C27 H27 0.9300 . ?
C28 C29 1.3900 . ?
C29 C30 1.3900 . ?
C29 H29 0.9300 . ?
C30 N5 1.32(3) . ?
N5 H5B 0.8600 . ?
N5 H5C 0.8600 . ?
C31 C31 1.538(18) 2_556 ?
C32 C33 1.3900 . ?
C32 C37 1.3900 . ?
C33 C34 1.3900 . ?
C33 H33 0.9300 . ?
C34 C35 1.3900 . ?
C34 N6 1.55(3) . ?
C35 C36 1.3900 . ?
C36 C37 1.3900 . ?
C36 H36 0.9300 . ?
C37 H37 0.9300 . ?
N6 H6B 0.8600 . ?
N6 H6C 0.8600 . ?

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
O7 Tb1 O2 87.6(2) 2_556 . ?
O7 Tb1 O4 75.7(2) 2_556 . ?
O2 Tb1 O4 141.2(2) . . ?
O7 Tb1 O8 69.4(2) 2_556 . ?
O2 Tb1 O8 78.5(2) . . ?
O4 Tb1 O8 125.0(2) . . ?
O7 Tb1 N4 105.3(2) 2_556 . ?
O2 Tb1 N4 141.2(2) . . ?
O4 Tb1 N4 77.5(2) . . ?
O8 Tb1 N4 72.6(2) . . ?
O7 Tb1 N1 88.1(2) 2_556 . ?
O2 Tb1 N1 71.7(2) . . ?
O4 Tb1 N1 73.0(2) . . ?
O8 Tb1 N1 143.3(2) . . ?
N4 Tb1 N1 143.3(2) . . ?
O7 Tb1 N2 146.0(2) 2_556 . ?
O2 Tb1 N2 100.3(2) . . ?
O4 Tb1 N2 77.8(2) . . ?
O8 Tb1 N2 144.5(2) . . ?
N4 Tb1 N2 89.1(3) . . ?
N1 Tb1 N2 63.8(3) . . ?
O7 Tb1 N3 139.2(2) 2_556 . ?
O2 Tb1 N3 81.0(2) . . ?
O4 Tb1 N3 133.4(2) . . ?
O8 Tb1 N3 70.0(2) . . ?
N4 Tb1 N3 65.2(2) . . ?
N1 Tb1 N3 124.0(2) . . ?
N2 Tb1 N3 74.8(2) . . ?
O3 S1 O1 115.2(4) . . ?
O3 S1 O2 110.3(4) . . ?
O1 S1 O2 112.4(4) . . ?
O6 S3 O5 115.0(6) . . ?
O6 S3 O4 111.8(5) . . ?
O5 S3 O4 110.9(5) . . ?
S1 O2 Tb1 142.6(4) . . ?
S3 O4 Tb1 153.8(5) . . ?
C31 O7 Tb1 119.6(5) . 2_556 ?
C31 O8 Tb1 117.3(5) . . ?
C1 N1 C12 118.5(8) . . ?
C1 N1 Tb1 121.3(6) . . ?
C12 N1 Tb1 120.1(6) . . ?
C10 N2 C11 117.2(10) . . ?
C10 N2 Tb1 123.2(7) . . ?
C11 N2 Tb1 119.2(7) . . ?
C13 N3 C24 118.4(8) . . ?
C13 N3 Tb1 123.7(6) . . ?
C24 N3 Tb1 117.1(5) . . ?
C22 N4 C23 117.8(7) . . ?
C22 N4 Tb1 122.2(6) . . ?
C23 N4 Tb1 119.4(6) . . ?
N1 C1 C2 123.6(11) . . ?
N1 C1 H1A 118.2 . . ?
C2 C1 H1A 118.2 . . ?
C3 C2 C1 118.2(11) . . ?
C3 C2 H2A 120.9 . . ?
C1 C2 H2A 120.9 . . ?
C2 C3 C4 119.9(10) . . ?
C2 C3 H3A 120.0 . . ?
C4 C3 H3A 120.0 . . ?
C5 C4 C3 124.1(11) . . ?
C5 C4 C12 118.5(12) . . ?
C3 C4 C12 117.3(10) . . ?
C6 C5 C4 122.0(11) . . ?
C6 C5 H5A 119.0 . . ?
C4 C5 H5A 119.0 . . ?
C5 C6 C7 121.1(13) . . ?
C5 C6 H6A 119.5 . . ?
C7 C6 H6A 119.5 . . ?
C11 C7 C6 120.0(13) . . ?
C11 C7 C8 116.2(11) . . ?
C6 C7 C8 123.8(13) . . ?
C9 C8 C7 122.6(13) . . ?
C9 C8 H8A 118.7 . . ?
C7 C8 H8A 118.7 . . ?
C8 C9 C10 115.8(13) . . ?
C8 C9 H9A 122.1 . . ?
C10 C9 H9A 122.1 . . ?
N2 C10 C9 125.0(12) . . ?
N2 C10 H10A 125.1 . . ?
C9 C10 H10A 107.3 . . ?
N2 C11 C7 123.1(11) . . ?
N2 C11 C12 117.7(9) . . ?
C7 C11 C12 119.2(10) . . ?
N1 C12 C4 122.3(10) . . ?
N1 C12 C11 118.6(8) . . ?
C4 C12 C11 119.1(10) . . ?
N3 C13 C14 123.6(9) . . ?
N3 C13 H13A 118.2 . . ?
C14 C13 H13A 118.2 . . ?
C15 C14 C13 119.3(10) . . ?
C15 C14 H14A 120.3 . . ?
C13 C14 H14A 120.3 . . ?
C14 C15 C16 119.2(9) . . ?
C14 C15 H15A 120.4 . . ?
C16 C15 H15A 120.4 . . ?
C24 C16 C15 117.0(8) . . ?
C24 C16 C17 120.2(9) . . ?
C15 C16 C17 122.8(8) . . ?
C18 C17 C16 120.7(9) . . ?
C18 C17 H17A 118.4 . . ?
C16 C17 H17A 116.9 . . ?
C17 C18 C19 121.8(9) . . ?
C17 C18 H18A 119.1 . . ?
C19 C18 H18A 119.1 . . ?
C20 C19 C23 116.8(8) . . ?
C20 C19 C18 124.0(9) . . ?
C23 C19 C18 119.2(9) . . ?
C21 C20 C19 121.2(9) . . ?
C21 C20 H20A 119.4 . . ?
C19 C20 H20A 119.4 . . ?
C20 C21 C22 118.4(9) . . ?
C20 C21 H21A 120.8 . . ?
C22 C21 H21A 120.8 . . ?
N4 C22 C21 123.1(9) . . ?
N4 C22 H22A 117.6 . . ?
C21 C22 H22A 118.7 . . ?
N4 C23 C19 122.7(8) . . ?
N4 C23 C24 117.9(7) . . ?
C19 C23 C24 119.3(8) . . ?
N3 C24 C16 122.4(8) . . ?
N3 C24 C23 119.0(8) . . ?
C16 C24 C23 118.6(8) . . ?
C26 C25 C30 120.0 . . ?
C27 C26 C25 120.0 . . ?
C27 C26 H26 120.0 . . ?
C25 C26 H26 120.0 . . ?
C26 C27 C28 120.0 . . ?
C26 C27 H27 120.0 . . ?
C28 C27 H27 120.0 . . ?
C27 C28 C29 120.0 . . ?
C30 C29 C28 120.0 . . ?
C30 C29 H29 120.0 . . ?
C28 C29 H29 120.0 . . ?
N5 C30 C29 113.1(15) . . ?
N5 C30 C25 126.6(15) . . ?
C29 C30 C25 120.0 . . ?
C30 N5 H5B 120.0 . . ?
C30 N5 H5C 120.0 . . ?
H5B N5 H5C 120.0 . . ?
O8 C31 O7 126.5(8) . . ?
O8 C31 C31 117.9(10) . 2_556 ?
O7 C31 C31 115.5(10) . 2_556 ?
C33 C32 C37 120.0 . . ?
C32 C33 C34 120.0 . . ?
C32 C33 H33 120.0 . . ?
C34 C33 H33 120.0 . . ?
C35 C34 C33 120.0 . . ?
C35 C34 N6 128.5(13) . . ?
C33 C34 N6 111.5(13) . . ?
C34 C35 C36 120.0 . . ?
C37 C36 C35 120.0 . . ?
C37 C36 H36 120.0 . . ?
C35 C36 H36 120.0 . . ?
C36 C37 C32 120.0 . . ?
C36 C37 H37 120.0 . . ?
C32 C37 H37 120.0 . . ?
C34 N6 H6B 120.0 . . ?
C34 N6 H6C 120.0 . . ?
H6B N6 H6C 120.0 . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         1.282
_refine_diff_density_min         -1.258
_refine_diff_density_rms         0.177

_database_code_depnum_ccdc_archive 'CCDC 981694'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C31 H21 Er N5 O8 S2'
_chemical_formula_weight         822.91

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   10.542(3)
_cell_length_b                   10.561(3)
_cell_length_c                   14.961(4)
_cell_angle_alpha                75.527(6)
_cell_angle_beta                 69.711(6)
_cell_angle_gamma                71.721(6)
_cell_volume                     1464.7(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.866
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             812
_exptl_absorpt_coefficient_mu    3.071
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.5787
_exptl_absorpt_correction_T_max  0.9135
_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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7307
_diffrn_reflns_av_R_equivalents  0.0927
_diffrn_reflns_av_sigmaI/netI    0.2143
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.06
_diffrn_reflns_theta_max         25.00
_reflns_number_total             5136
_reflns_number_gt                2991
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_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          
; 
 Restraints: DELU,SIMU and ISOR restraints for the disordered H2N-BDS ligand,
 to control the displacement parameters of overlapping components. Such
 restraints are often required for disorder components that interpenetrate each
 other, since the electron density of the disordered atoms strongly overlap and
 can not be resolved satisfactorily in free refinement. Restraints are gentler
 and more flexible than rigid constraints.  
;


_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)+(0.0569P)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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5136
_refine_ls_number_parameters     463
_refine_ls_number_restraints     210
_refine_ls_R_factor_all          0.1437
_refine_ls_R_factor_gt           0.0818
_refine_ls_wR_factor_ref         0.1837
_refine_ls_wR_factor_gt          0.1494
_refine_ls_goodness_of_fit_ref   0.956
_refine_ls_restrained_S_all      0.938
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Er1 Er 0.12658(6) 0.12423(6) 0.29546(4) 0.02707(15) Uani 1 1 d . . 4
S1 S 0.3718(3) -0.1350(3) 0.3990(2) 0.0338(8) Uani 1 1 d . A 4
S3 S -0.1132(3) 0.2013(4) 0.1498(2) 0.0501(10) Uani 1 1 d . B 4
O1 O 0.2573(8) -0.1841(9) 0.4712(6) 0.041(2) Uani 1 1 d . A 4
O2 O 0.3243(7) -0.0216(8) 0.3282(5) 0.037(2) Uani 1 1 d . A 4
O3 O 0.4820(8) -0.2364(9) 0.3498(6) 0.047(3) Uani 1 1 d . A 4
O4 O -0.0393(7) 0.1407(8) 0.2240(6) 0.041(2) Uani 1 1 d . B 4
O5 O -0.0811(12) 0.3239(11) 0.0977(7) 0.080(4) Uani 1 1 d . B 4
O6 O -0.2605(9) 0.2086(13) 0.1914(8) 0.099(4) Uani 1 1 d . B 4
O7 O -0.0087(8) 0.0328(8) 0.6113(5) 0.033(2) Uani 1 1 d . . 4
O8 O 0.0799(7) 0.1322(7) 0.4594(5) 0.030(2) Uani 1 1 d . . 4
N1 N 0.2376(9) -0.0337(10) 0.1746(7) 0.036(3) Uani 1 1 d . C 4
N2 N 0.2285(11) 0.2378(11) 0.1276(8) 0.047(3) Uani 1 1 d . C 4
N3 N 0.2392(9) 0.2895(10) 0.3139(7) 0.032(3) Uani 1 1 d . D 4
N4 N -0.0390(8) 0.3478(9) 0.3258(6) 0.026(3) Uani 1 1 d . D 4
C1 C 0.2442(12) -0.1631(13) 0.1954(9) 0.044(4) Uani 1 1 d . C 4
H1A H 0.2092 -0.1976 0.2601 0.053 Uiso 1 1 calc R C 4
C2 C 0.2989(13) -0.2554(15) 0.1297(11) 0.058(4) Uani 1 1 d . C 4
H2A H 0.3063 -0.3475 0.1494 0.069 Uiso 1 1 calc R C 4
C3 C 0.3403(12) -0.1998(17) 0.0351(10) 0.066(5) Uani 1 1 d . C 4
H3A H 0.3718 -0.2543 -0.0122 0.079 Uiso 1 1 calc R C 4
C4 C 0.3362(12) -0.0619(15) 0.0077(8) 0.044(4) Uani 1 1 d . C 4
C5 C 0.3850(12) -0.0019(16) -0.0901(9) 0.052(4) Uani 1 1 d . C 4
H5A H 0.4228 -0.0569 -0.1375 0.063 Uiso 1 1 calc R C 4
C6 C 0.3789(15) 0.1249(18) -0.1157(10) 0.067(5) Uani 1 1 d . C 4
H6A H 0.4082 0.1605 -0.1807 0.080 Uiso 1 1 calc R C 4
C7 C 0.3283(14) 0.2090(18) -0.0459(9) 0.058(5) Uani 1 1 d . C 4
C8 C 0.3141(15) 0.3551(18) -0.0643(11) 0.071(6) Uani 1 1 d . C 4
H8A H 0.3400 0.3987 -0.1276 0.085 Uiso 1 1 calc R C 4
C9 C 0.2659(16) 0.4256(16) 0.0064(10) 0.067(5) Uani 1 1 d . C 4
H9A H 0.2582 0.5181 -0.0071 0.080 Uiso 1 1 calc R C 4
C10 C 0.2258(15) 0.3619(15) 0.1027(10) 0.055(4) Uani 1 1 d . C 4
H10A H 0.1695 0.4314 0.1433 0.067 Uiso 1 1 d R C 4
C11 C 0.2793(11) 0.1584(14) 0.0543(8) 0.034(3) Uani 1 1 d . C 4
C12 C 0.2849(12) 0.0182(14) 0.0785(9) 0.040(4) Uani 1 1 d . C 4
C13 C 0.3710(13) 0.2673(14) 0.3059(9) 0.047(4) Uani 1 1 d . D 4
H13A H 0.4301 0.1876 0.2848 0.056 Uiso 1 1 calc R D 4
C14 C 0.4306(14) 0.3524(15) 0.3262(10) 0.052(4) Uani 1 1 d . D 4
H14A H 0.5263 0.3313 0.3171 0.063 Uiso 1 1 calc R D 4
C15 C 0.3450(12) 0.4678(14) 0.3598(9) 0.042(4) Uani 1 1 d . D 4
H15A H 0.3818 0.5255 0.3758 0.050 Uiso 1 1 calc R D 4
C16 C 0.2041(12) 0.4995(14) 0.3701(9) 0.045(4) Uani 1 1 d . D 4
C17 C 0.1042(14) 0.6193(13) 0.4034(9) 0.048(4) Uani 1 1 d . D 4
H17A H 0.1425 0.6881 0.4036 0.058 Uiso 1 1 d R D 4
C18 C -0.0278(12) 0.6499(13) 0.4046(9) 0.043(4) Uani 1 1 d . D 4
H18A H -0.0879 0.7303 0.4239 0.051 Uiso 1 1 calc R D 4
C19 C -0.0781(12) 0.5620(12) 0.3768(9) 0.036(3) Uani 1 1 d . D 4
C20 C -0.2187(12) 0.5853(12) 0.3828(9) 0.040(3) Uani 1 1 d . D 4
H20A H -0.2799 0.6659 0.4012 0.048 Uiso 1 1 calc R D 4
C21 C -0.2699(13) 0.4962(13) 0.3632(9) 0.048(4) Uani 1 1 d . D 4
H21A H -0.3634 0.5145 0.3660 0.057 Uiso 1 1 calc R D 4
C22 C -0.1732(12) 0.3735(12) 0.3380(9) 0.038(3) Uani 1 1 d . D 4
H22A H -0.2067 0.3084 0.3113 0.046 Uiso 1 1 d R D 4
C23 C 0.0062(12) 0.4367(13) 0.3509(8) 0.032(3) Uani 1 1 d . D 4
C24 C 0.1536(11) 0.4070(12) 0.3455(9) 0.035(3) Uani 1 1 d . D 4
C25 C 0.451(2) -0.0779(16) 0.4540(15) 0.028(4) Uani 0.50 1 d PGU E -1
C26 C 0.378(2) -0.0476(17) 0.5464(15) 0.027(4) Uani 0.50 1 d PGU E -1
H26 H 0.2928 -0.0694 0.5785 0.032 Uiso 0.50 1 calc PR E -1
C27 C 0.432(2) 0.0152(19) 0.5907(15) 0.024(4) Uani 0.50 1 d PGU E -1
H27 H 0.3837 0.0355 0.6525 0.029 Uiso 0.50 1 calc PR E -1
C28 C 0.560(2) 0.0478(19) 0.5427(16) 0.0182(11) Uani 0.50 1 d PGU E -1
C29 C 0.632(2) 0.0176(19) 0.4503(16) 0.027(4) Uani 0.50 1 d PGU E -1
H29 H 0.7176 0.0394 0.4182 0.033 Uiso 0.50 1 calc PR E -1
C30 C 0.578(2) -0.0453(17) 0.4060(15) 0.023(4) Uani 0.50 1 d PGU E -1
N5 N 0.6490(18) -0.0459(19) 0.3143(13) 0.034(4) Uani 0.50 1 d PU E -1
H5B H 0.7190 -0.0102 0.2897 0.041 Uiso 0.50 1 calc PR E -1
H5C H 0.6254 -0.0821 0.2789 0.041 Uiso 0.50 1 calc PR E -1
C31 C 0.0237(10) 0.0474(12) 0.5193(8) 0.027(3) Uani 1 1 d U . .
C32 C -0.043(2) 0.0718(17) 0.0727(16) 0.029(4) Uani 0.50 1 d PGU F -2
C33 C 0.001(3) 0.1188(17) -0.0256(17) 0.045(4) Uani 0.50 1 d PGU F -2
H33 H 0.0018 0.2093 -0.0471 0.053 Uiso 0.50 1 calc PR F -2
C34 C 0.045(3) 0.031(2) -0.0917(16) 0.041(4) Uani 0.50 1 d PGU F -2
C35 C 0.045(3) -0.105(2) -0.0596(16) 0.033(4) Uani 0.50 1 d PGU F -2
C36 C 0.000(3) -0.1517(17) 0.0387(16) 0.032(4) Uani 0.50 1 d PGU F -2
H36 H -0.0004 -0.2422 0.0602 0.038 Uiso 0.50 1 calc PR F -2
C37 C -0.044(2) -0.0635(17) 0.1048(15) 0.033(4) Uani 0.50 1 d PGU F -2
H37 H -0.0740 -0.0949 0.1706 0.039 Uiso 0.50 1 calc PR F -2
N6 N 0.082(2) 0.108(3) -0.1956(16) 0.068(5) Uani 0.50 1 d PU F -2
H6B H 0.0729 0.1938 -0.2053 0.081 Uiso 0.50 1 calc PR F -2
H6C H 0.1105 0.0656 -0.2439 0.081 Uiso 0.50 1 calc PR F -2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Er1 O7 2.275(8) 2_556 ?
Er1 O4 2.289(8) . ?
Er1 O2 2.297(7) . ?
Er1 O8 2.346(8) . ?
Er1 N4 2.496(8) . ?
Er1 N1 2.497(10) . ?
Er1 N3 2.510(11) . ?
Er1 N2 2.516(10) . ?
S1 O3 1.436(8) . ?
S1 O1 1.449(8) . ?
S1 O2 1.471(8) . ?
S3 O5 1.409(12) . ?
S3 O6 1.443(9) . ?
S3 O4 1.477(8) . ?
O7 C31 1.279(13) . ?
O7 Er1 2.275(8) 2_556 ?
O8 C31 1.233(13) . ?
N1 C1 1.309(16) . ?
N1 C12 1.377(15) . ?
N2 C10 1.263(17) . ?
N2 C11 1.401(16) . ?
N3 C13 1.301(15) . ?
N3 C24 1.369(14) . ?
N4 C22 1.310(14) . ?
N4 C23 1.352(16) . ?
C1 C2 1.408(18) . ?
C1 H1A 0.9300 . ?
C2 C3 1.361(19) . ?
C2 H2A 0.9300 . ?
C3 C4 1.40(2) . ?
C3 H3A 0.9300 . ?
C4 C12 1.375(18) . ?
C4 C5 1.423(17) . ?
C5 C6 1.28(2) . ?
C5 H5A 0.9300 . ?
C6 C7 1.39(2) . ?
C6 H6A 0.9300 . ?
C7 C11 1.427(16) . ?
C7 C8 1.47(2) . ?
C8 C9 1.31(2) . ?
C8 H8A 0.9300 . ?
C9 C10 1.407(19) . ?
C9 H9A 0.9300 . ?
C10 H10A 0.9798 . ?
C11 C12 1.421(18) . ?
C13 C14 1.38(2) . ?
C13 H13A 0.9300 . ?
C14 C15 1.362(17) . ?
C14 H14A 0.9300 . ?
C15 C16 1.376(16) . ?
C15 H15A 0.9300 . ?
C16 C24 1.420(18) . ?
C16 C17 1.440(17) . ?
C17 C18 1.322(17) . ?
C17 H17A 0.9362 . ?
C18 C19 1.404(18) . ?
C18 H18A 0.9300 . ?
C19 C20 1.398(16) . ?
C19 C23 1.404(16) . ?
C20 C21 1.353(18) . ?
C20 H20A 0.9300 . ?
C21 C22 1.418(16) . ?
C21 H21A 0.9300 . ?
C22 H22A 1.0686 . ?
C23 C24 1.463(16) . ?
C25 C26 1.3900 . ?
C25 C30 1.3900 . ?
C26 C27 1.3900 . ?
C26 H26 0.9300 . ?
C27 C28 1.3900 . ?
C27 H27 0.9300 . ?
C28 C29 1.3900 . ?
C29 C30 1.3900 . ?
C29 H29 0.9300 . ?
C30 N5 1.32(3) . ?
N5 H5B 0.8600 . ?
N5 H5C 0.8600 . ?
C31 C31 1.54(2) 2_556 ?
C32 C33 1.3900 . ?
C32 C37 1.3900 . ?
C33 C34 1.3900 . ?
C33 H33 0.9300 . ?
C34 C35 1.3900 . ?
C34 N6 1.54(3) . ?
C35 C36 1.3900 . ?
C36 C37 1.3900 . ?
C36 H36 0.9300 . ?
C37 H37 0.9300 . ?
N6 H6B 0.8600 . ?
N6 H6C 0.8600 . ?

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
O7 Er1 O4 74.9(3) 2_556 . ?
O7 Er1 O2 87.6(3) 2_556 . ?
O4 Er1 O2 141.5(3) . . ?
O7 Er1 O8 69.9(3) 2_556 . ?
O4 Er1 O8 124.5(3) . . ?
O2 Er1 O8 78.3(2) . . ?
O7 Er1 N4 105.6(3) 2_556 . ?
O4 Er1 N4 76.4(3) . . ?
O2 Er1 N4 142.0(3) . . ?
O8 Er1 N4 73.6(3) . . ?
O7 Er1 N1 86.5(3) 2_556 . ?
O4 Er1 N1 73.7(3) . . ?
O2 Er1 N1 71.2(3) . . ?
O8 Er1 N1 142.0(3) . . ?
N4 Er1 N1 143.4(3) . . ?
O7 Er1 N3 139.4(3) 2_556 . ?
O4 Er1 N3 134.4(3) . . ?
O2 Er1 N3 80.0(3) . . ?
O8 Er1 N3 69.7(3) . . ?
N4 Er1 N3 66.7(3) . . ?
N1 Er1 N3 124.3(3) . . ?
O7 Er1 N2 146.9(3) 2_556 . ?
O4 Er1 N2 78.9(3) . . ?
O2 Er1 N2 100.9(3) . . ?
O8 Er1 N2 143.1(3) . . ?
N4 Er1 N2 87.3(3) . . ?
N1 Er1 N2 66.7(4) . . ?
N3 Er1 N2 73.8(4) . . ?
O3 S1 O1 114.9(6) . . ?
O3 S1 O2 109.8(5) . . ?
O1 S1 O2 112.5(5) . . ?
O5 S3 O6 114.8(7) . . ?
O5 S3 O4 112.0(7) . . ?
O6 S3 O4 110.5(6) . . ?
S1 O2 Er1 142.4(5) . . ?
S3 O4 Er1 152.9(6) . . ?
C31 O7 Er1 120.0(8) . 2_556 ?
C31 O8 Er1 117.8(8) . . ?
C1 N1 C12 116.7(11) . . ?
C1 N1 Er1 124.1(8) . . ?
C12 N1 Er1 119.0(8) . . ?
C10 N2 C11 117.5(12) . . ?
C10 N2 Er1 125.8(9) . . ?
C11 N2 Er1 116.3(8) . . ?
C13 N3 C24 116.5(12) . . ?
C13 N3 Er1 125.5(9) . . ?
C24 N3 Er1 117.6(8) . . ?
C22 N4 C23 117.4(10) . . ?
C22 N4 Er1 123.4(8) . . ?
C23 N4 Er1 117.8(7) . . ?
N1 C1 C2 126.5(13) . . ?
N1 C1 H1A 116.8 . . ?
C2 C1 H1A 116.8 . . ?
C3 C2 C1 115.1(14) . . ?
C3 C2 H2A 122.5 . . ?
C1 C2 H2A 122.5 . . ?
C2 C3 C4 121.3(13) . . ?
C2 C3 H3A 119.4 . . ?
C4 C3 H3A 119.4 . . ?
C12 C4 C3 118.6(12) . . ?
C12 C4 C5 118.8(14) . . ?
C3 C4 C5 122.7(13) . . ?
C6 C5 C4 122.9(14) . . ?
C6 C5 H5A 118.6 . . ?
C4 C5 H5A 118.6 . . ?
C5 C6 C7 120.0(15) . . ?
C5 C6 H6A 120.0 . . ?
C7 C6 H6A 120.0 . . ?
C6 C7 C11 121.5(16) . . ?
C6 C7 C8 126.0(13) . . ?
C11 C7 C8 112.4(13) . . ?
C9 C8 C7 121.5(14) . . ?
C9 C8 H8A 119.3 . . ?
C7 C8 H8A 119.3 . . ?
C8 C9 C10 120.3(16) . . ?
C8 C9 H9A 119.9 . . ?
C10 C9 H9A 119.9 . . ?
N2 C10 C9 124.2(15) . . ?
N2 C10 H10A 124.6 . . ?
C9 C10 H10A 108.5 . . ?
N2 C11 C12 119.8(11) . . ?
N2 C11 C7 124.0(13) . . ?
C12 C11 C7 116.2(12) . . ?
C4 C12 N1 121.8(13) . . ?
C4 C12 C11 120.6(12) . . ?
N1 C12 C11 117.6(11) . . ?
N3 C13 C14 125.5(13) . . ?
N3 C13 H13A 117.2 . . ?
C14 C13 H13A 117.2 . . ?
C15 C14 C13 118.1(13) . . ?
C15 C14 H14A 121.0 . . ?
C13 C14 H14A 121.0 . . ?
C14 C15 C16 120.3(14) . . ?
C14 C15 H15A 119.9 . . ?
C16 C15 H15A 119.9 . . ?
C15 C16 C24 117.3(12) . . ?
C15 C16 C17 125.2(14) . . ?
C24 C16 C17 117.5(11) . . ?
C18 C17 C16 122.5(14) . . ?
C18 C17 H17A 119.0 . . ?
C16 C17 H17A 115.3 . . ?
C17 C18 C19 120.6(11) . . ?
C17 C18 H18A 119.7 . . ?
C19 C18 H18A 119.7 . . ?
C20 C19 C18 122.7(11) . . ?
C20 C19 C23 114.7(12) . . ?
C18 C19 C23 122.2(11) . . ?
C21 C20 C19 123.1(11) . . ?
C21 C20 H20A 118.5 . . ?
C19 C20 H20A 118.5 . . ?
C20 C21 C22 116.3(12) . . ?
C20 C21 H21A 121.9 . . ?
C22 C21 H21A 121.9 . . ?
N4 C22 C21 123.9(13) . . ?
N4 C22 H22A 116.8 . . ?
C21 C22 H22A 117.7 . . ?
N4 C23 C19 124.1(11) . . ?
N4 C23 C24 119.2(10) . . ?
C19 C23 C24 116.6(12) . . ?
N3 C24 C16 122.3(11) . . ?
N3 C24 C23 117.3(12) . . ?
C16 C24 C23 120.4(10) . . ?
C26 C25 C30 120.0 . . ?
C27 C26 C25 120.0 . . ?
C27 C26 H26 120.0 . . ?
C25 C26 H26 120.0 . . ?
C26 C27 C28 120.0 . . ?
C26 C27 H27 120.0 . . ?
C28 C27 H27 120.0 . . ?
C27 C28 C29 120.0 . . ?
C30 C29 C28 120.0 . . ?
C30 C29 H29 120.0 . . ?
C28 C29 H29 120.0 . . ?
N5 C30 C29 111.2(14) . . ?
N5 C30 C25 127.9(15) . . ?
C29 C30 C25 120.0 . . ?
C30 N5 H5B 120.0 . . ?
C30 N5 H5C 120.0 . . ?
H5B N5 H5C 120.0 . . ?
O8 C31 O7 127.8(12) . . ?
O8 C31 C31 117.2(13) . 2_556 ?
O7 C31 C31 114.8(13) . 2_556 ?
C33 C32 C37 120.0 . . ?
C32 C33 C34 120.0 . . ?
C32 C33 H33 120.0 . . ?
C34 C33 H33 120.0 . . ?
C33 C34 C35 120.0 . . ?
C33 C34 N6 110.1(15) . . ?
C35 C34 N6 129.8(15) . . ?
C36 C35 C34 120.0 . . ?
C37 C36 C35 120.0 . . ?
C37 C36 H36 120.0 . . ?
C35 C36 H36 120.0 . . ?
C36 C37 C32 120.0 . . ?
C36 C37 H37 120.0 . . ?
C32 C37 H37 120.0 . . ?
C34 N6 H6B 120.0 . . ?
C34 N6 H6C 120.0 . . ?
H6B N6 H6C 120.0 . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         1.363
_refine_diff_density_min         -1.226
_refine_diff_density_rms         0.237


_database_code_depnum_ccdc_archive 'CCDC 981695'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_130505c_0m

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C31 H21 N5 O8 S2 Yb'
_chemical_formula_weight         828.69

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   10.5522(9)
_cell_length_b                   10.5726(10)
_cell_length_c                   14.9134(13)
_cell_angle_alpha                75.774(2)
_cell_angle_beta                 69.8350(10)
_cell_angle_gamma                71.5590(10)
_cell_volume                     1464.1(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.880
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             816
_exptl_absorpt_coefficient_mu    3.400
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.5496
_exptl_absorpt_correction_T_max  0.9049
_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  ?
_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            7222
_diffrn_reflns_av_R_equivalents  0.0226
_diffrn_reflns_av_sigmaI/netI    0.0476
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.05
_diffrn_reflns_theta_max         25.00
_reflns_number_total             5119
_reflns_number_gt                4529
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_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          
; 
 Restraints: DELU,SIMU and ISOR restraints for the disordered H2N-BDS ligand,
 to control the displacement parameters of overlapping components. Such
 restraints are often required for disorder components that interpenetrate each
 other, since the electron density of the disordered atoms strongly overlap and
 can not be resolved satisfactorily in free refinement. Restraints are gentler
 and more flexible than rigid constraints.  
;


_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)+(0.0533P)²+0.3202P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5119
_refine_ls_number_parameters     463
_refine_ls_number_restraints     210
_refine_ls_R_factor_all          0.0393
_refine_ls_R_factor_gt           0.0333
_refine_ls_wR_factor_ref         0.0849
_refine_ls_wR_factor_gt          0.0811
_refine_ls_goodness_of_fit_ref   0.980
_refine_ls_restrained_S_all      0.963
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Yb1 Yb 0.12449(2) 0.12389(2) 0.296799(15) 0.02123(9) Uani 1 1 d . . 4
S1 S 0.37124(14) -0.13423(13) 0.39768(10) 0.0276(3) Uani 1 1 d . A 4
S3 S -0.11413(16) 0.20058(17) 0.15108(12) 0.0439(4) Uani 1 1 d . B 4
O1 O 0.2586(4) -0.1821(4) 0.4708(3) 0.0386(10) Uani 1 1 d . A 4
O2 O 0.3202(4) -0.0191(4) 0.3281(3) 0.0290(8) Uani 1 1 d . A 4
O3 O 0.4803(4) -0.2365(4) 0.3481(3) 0.0401(10) Uani 1 1 d . A 4
O4 O -0.0387(4) 0.1415(4) 0.2237(3) 0.0384(10) Uani 1 1 d . B 4
O5 O -0.0848(7) 0.3259(5) 0.1004(4) 0.0757(17) Uani 1 1 d . B 4
O6 O -0.2594(5) 0.2056(7) 0.1923(4) 0.083(2) Uani 1 1 d . B 4
O7 O -0.0081(4) 0.0333(3) 0.6106(2) 0.0247(8) Uani 1 1 d . . 4
O8 O 0.0783(4) 0.1330(3) 0.4600(2) 0.0256(8) Uani 1 1 d . . 4
N1 N 0.2340(5) -0.0333(5) 0.1757(3) 0.0314(10) Uani 1 1 d . C 4
N2 N 0.2264(5) 0.2325(5) 0.1286(3) 0.0366(11) Uani 1 1 d . C 4
N3 N 0.2366(4) 0.2878(4) 0.3142(3) 0.0240(9) Uani 1 1 d . D 4
N4 N -0.0395(4) 0.3445(4) 0.3284(3) 0.0261(9) Uani 1 1 d . D 4
C1 C 0.2422(7) -0.1647(6) 0.1990(5) 0.0428(15) Uani 1 1 d . C 4
H1A H 0.2115 -0.2003 0.2639 0.051 Uiso 1 1 calc R C 4
C2 C 0.2945(8) -0.2513(7) 0.1308(6) 0.0574(19) Uani 1 1 d . C 4
H2A H 0.2980 -0.3427 0.1498 0.069 Uiso 1 1 calc R C 4
C3 C 0.3402(7) -0.2010(8) 0.0364(5) 0.057(2) Uani 1 1 d . C 4
H3A H 0.3741 -0.2577 -0.0100 0.068 Uiso 1 1 calc R C 4
C4 C 0.3368(6) -0.0660(8) 0.0088(4) 0.0462(17) Uani 1 1 d . C 4
C5 C 0.3856(7) -0.0046(9) -0.0899(5) 0.060(2) Uani 1 1 d . C 4
H5A H 0.4220 -0.0577 -0.1387 0.072 Uiso 1 1 calc R C 4
C6 C 0.3797(7) 0.1263(9) -0.1128(5) 0.061(2) Uani 1 1 d . C 4
H6A H 0.4137 0.1619 -0.1772 0.073 Uiso 1 1 calc R C 4
C7 C 0.3236(7) 0.2133(8) -0.0424(4) 0.0501(18) Uani 1 1 d . C 4
C8 C 0.3139(9) 0.3492(9) -0.0638(6) 0.067(2) Uani 1 1 d . C 4
H8A H 0.3443 0.3890 -0.1277 0.081 Uiso 1 1 calc R C 4
C9 C 0.2595(9) 0.4263(8) 0.0087(6) 0.071(2) Uani 1 1 d . C 4
H9A H 0.2510 0.5188 -0.0054 0.085 Uiso 1 1 calc R C 4
C10 C 0.2174(8) 0.3643(7) 0.1036(5) 0.0515(18) Uani 1 1 d . C 4
H10A H 0.1611 0.4338 0.1443 0.062 Uiso 1 1 d R C 4
C11 C 0.2777(6) 0.1565(7) 0.0565(4) 0.0366(14) Uani 1 1 d . C 4
C12 C 0.2823(5) 0.0159(6) 0.0813(4) 0.0304(13) Uani 1 1 d . C 4
C13 C 0.3704(6) 0.2634(6) 0.3058(4) 0.0341(13) Uani 1 1 d . D 4
H13A H 0.4298 0.1838 0.2842 0.041 Uiso 1 1 calc R D 4
C14 C 0.4283(6) 0.3504(7) 0.3277(5) 0.0455(16) Uani 1 1 d . D 4
H14A H 0.5235 0.3290 0.3205 0.055 Uiso 1 1 calc R D 4
C15 C 0.3424(6) 0.4665(7) 0.3594(5) 0.0442(15) Uani 1 1 d . D 4
H15A H 0.3787 0.5251 0.3749 0.053 Uiso 1 1 calc R D 4
C16 C 0.2013(6) 0.4983(5) 0.3689(4) 0.0303(12) Uani 1 1 d . D 4
C17 C 0.1046(6) 0.6197(6) 0.4017(4) 0.0372(14) Uani 1 1 d . D 4
H17A H 0.1428 0.6885 0.4019 0.045 Uiso 1 1 d R D 4
C18 C -0.0296(6) 0.6496(5) 0.4050(4) 0.0363(14) Uani 1 1 d . D 4
H18A H -0.0894 0.7300 0.4249 0.044 Uiso 1 1 calc R D 4
C19 C -0.0832(6) 0.5600(5) 0.3783(4) 0.0323(12) Uani 1 1 d . D 4
C20 C -0.2245(6) 0.5871(6) 0.3841(5) 0.0430(15) Uani 1 1 d . D 4
H20A H -0.2864 0.6683 0.4010 0.052 Uiso 1 1 calc R D 4
C21 C -0.2689(6) 0.4924(6) 0.3645(5) 0.0450(16) Uani 1 1 d . D 4
H21A H -0.3626 0.5081 0.3689 0.054 Uiso 1 1 calc R D 4
C22 C -0.1758(6) 0.3725(6) 0.3381(4) 0.0336(13) Uani 1 1 d . D 4
H22A H -0.2093 0.3075 0.3115 0.040 Uiso 1 1 d R D 4
C23 C 0.0064(5) 0.4366(5) 0.3503(4) 0.0256(11) Uani 1 1 d . D 4
C24 C 0.1515(5) 0.4064(5) 0.3437(4) 0.0257(11) Uani 1 1 d . D 4
C25 C 0.450(3) -0.067(3) 0.4486(15) 0.031(4) Uani 0.50 1 d PGU E -1
C26 C 0.377(3) -0.038(3) 0.5416(15) 0.033(5) Uani 0.50 1 d PGU E -1
H26 H 0.2931 -0.0607 0.5735 0.040 Uiso 0.50 1 calc PR E -1
C27 C 0.430(3) 0.026(3) 0.5868(15) 0.031(5) Uani 0.50 1 d PGU E -1
H27 H 0.3814 0.0449 0.6490 0.038 Uiso 0.50 1 calc PR E -1
C28 C 0.556(3) 0.060(3) 0.5390(14) 0.019(3) Uani 0.50 1 d PGU E -1
C29 C 0.629(3) 0.031(3) 0.4461(14) 0.023(3) Uani 0.50 1 d PGU E -1
H29 H 0.7135 0.0541 0.4141 0.028 Uiso 0.50 1 calc PR E -1
C30 C 0.576(3) -0.032(3) 0.4008(14) 0.023(3) Uani 0.50 1 d PGU E -1
N5 N 0.6460(10) -0.0510(11) 0.3183(7) 0.042(2) Uani 0.50 1 d PU E -1
H5B H 0.7222 -0.0255 0.2921 0.050 Uiso 0.50 1 calc PR E -1
H5C H 0.6188 -0.0897 0.2864 0.050 Uiso 0.50 1 calc PR E -1
C31 C 0.0206(5) 0.0489(5) 0.5208(4) 0.0222(11) Uani 1 1 d U . .
C32 C -0.049(2) 0.0749(16) 0.0713(14) 0.027(3) Uani 0.50 1 d PGU F -2
C33 C -0.005(2) 0.1225(16) -0.0269(14) 0.034(4) Uani 0.50 1 d PGU F -2
H33 H -0.0064 0.2132 -0.0479 0.041 Uiso 0.50 1 calc PR F -2
C34 C 0.041(2) 0.0345(18) -0.0938(14) 0.038(4) Uani 0.50 1 d PGU F -2
C35 C 0.043(2) -0.1011(17) -0.0624(14) 0.035(4) Uani 0.50 1 d PGU F -2
C36 C -0.001(2) -0.1487(16) 0.0359(14) 0.036(4) Uani 0.50 1 d PGU F -2
H36 H 0.0007 -0.2395 0.0569 0.044 Uiso 0.50 1 calc PR F -2
C37 C -0.047(2) -0.0607(16) 0.1027(14) 0.029(3) Uani 0.50 1 d PGU F -2
H37 H -0.0763 -0.0925 0.1685 0.034 Uiso 0.50 1 calc PR F -2
N6 N 0.0880(15) 0.1069(14) -0.1993(9) 0.076(4) Uani 0.50 1 d PU F -2
H6B H 0.1200 0.0618 -0.2467 0.092 Uiso 0.50 1 calc PR F -2
H6C H 0.0820 0.1921 -0.2103 0.092 Uiso 0.50 1 calc PR F -2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Yb1 O2 2.261(3) . ?
Yb1 O7 2.274(3) 2_556 ?
Yb1 O4 2.275(4) . ?
Yb1 O8 2.332(3) . ?
Yb1 N4 2.466(4) . ?
Yb1 N1 2.486(4) . ?
Yb1 N3 2.490(4) . ?
Yb1 N2 2.504(5) . ?
Yb1 C31 3.088(5) 2_556 ?
Yb1 C31 3.117(5) . ?
S1 O3 1.435(4) . ?
S1 O1 1.440(4) . ?
S1 O2 1.483(4) . ?
S3 O5 1.424(6) . ?
S3 O6 1.430(5) . ?
S3 O4 1.465(4) . ?
O7 C31 1.248(6) . ?
O7 Yb1 2.274(3) 2_556 ?
O8 C31 1.245(6) . ?
N1 C1 1.329(7) . ?
N1 C12 1.350(7) . ?
N2 C10 1.333(8) . ?
N2 C11 1.358(8) . ?
N3 C13 1.319(7) . ?
N3 C24 1.363(6) . ?
N4 C22 1.336(7) . ?
N4 C23 1.361(6) . ?
C1 C2 1.389(9) . ?
C1 H1A 0.9300 . ?
C2 C3 1.349(10) . ?
C2 H2A 0.9300 . ?
C3 C4 1.378(10) . ?
C3 H3A 0.9300 . ?
C4 C12 1.403(8) . ?
C4 C5 1.440(10) . ?
C5 C6 1.328(11) . ?
C5 H5A 0.9300 . ?
C6 C7 1.414(10) . ?
C6 H6A 0.9300 . ?
C7 C8 1.372(11) . ?
C7 C11 1.423(8) . ?
C8 C9 1.369(11) . ?
C8 H8A 0.9300 . ?
C9 C10 1.388(10) . ?
C9 H9A 0.9300 . ?
C10 H10A 0.9770 . ?
C11 C12 1.430(8) . ?
C13 C14 1.402(8) . ?
C13 H13A 0.9300 . ?
C14 C15 1.356(9) . ?
C14 H14A 0.9300 . ?
C15 C16 1.383(8) . ?
C15 H15A 0.9300 . ?
C16 C24 1.415(7) . ?
C16 C17 1.436(8) . ?
C17 C18 1.335(8) . ?
C17 H17A 0.9380 . ?
C18 C19 1.434(8) . ?
C18 H18A 0.9300 . ?
C19 C20 1.402(8) . ?
C19 C23 1.409(7) . ?
C20 C21 1.358(8) . ?
C20 H20A 0.9300 . ?
C21 C22 1.384(8) . ?
C21 H21A 0.9300 . ?
C22 H22A 1.0679 . ?
C23 C24 1.435(7) . ?
C25 C26 1.3900 . ?
C25 C30 1.3900 . ?
C26 C27 1.3900 . ?
C26 H26 0.9300 . ?
C27 C28 1.3900 . ?
C27 H27 0.9300 . ?
C28 C29 1.3900 . ?
C29 C30 1.3900 . ?
C29 H29 0.9300 . ?
C30 N5 1.22(2) . ?
N5 H5B 0.8600 . ?
N5 H5C 0.8600 . ?
C31 C31 1.558(10) 2_556 ?
C31 Yb1 3.088(5) 2_556 ?
C32 C33 1.3900 . ?
C32 C37 1.3900 . ?
C33 C34 1.3900 . ?
C33 H33 0.9300 . ?
C34 C35 1.3900 . ?
C34 N6 1.56(2) . ?
C35 C36 1.3900 . ?
C36 C37 1.3900 . ?
C36 H36 0.9300 . ?
C37 H37 0.9300 . ?
N6 H6B 0.8600 . ?
N6 H6C 0.8600 . ?

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
O2 Yb1 O7 87.73(13) . 2_556 ?
O2 Yb1 O4 141.51(14) . . ?
O7 Yb1 O4 75.62(13) 2_556 . ?
O2 Yb1 O8 78.63(13) . . ?
O7 Yb1 O8 70.23(11) 2_556 . ?
O4 Yb1 O8 125.11(13) . . ?
O2 Yb1 N4 141.78(13) . . ?
O7 Yb1 N4 105.74(13) 2_556 . ?
O4 Yb1 N4 76.66(14) . . ?
O8 Yb1 N4 73.04(13) . . ?
O2 Yb1 N1 71.33(13) . . ?
O7 Yb1 N1 86.19(14) 2_556 . ?
O4 Yb1 N1 73.11(14) . . ?
O8 Yb1 N1 142.38(14) . . ?
N4 Yb1 N1 143.48(14) . . ?
O2 Yb1 N3 79.89(13) . . ?
O7 Yb1 N3 139.96(12) 2_556 . ?
O4 Yb1 N3 133.82(14) . . ?
O8 Yb1 N3 70.04(12) . . ?
N4 Yb1 N3 66.71(13) . . ?
N1 Yb1 N3 124.18(14) . . ?
O2 Yb1 N2 100.15(14) . . ?
O7 Yb1 N2 145.87(14) 2_556 . ?
O4 Yb1 N2 77.88(15) . . ?
O8 Yb1 N2 143.79(14) . . ?
N4 Yb1 N2 88.46(15) . . ?
N1 Yb1 N2 65.65(16) . . ?
N3 Yb1 N2 74.11(15) . . ?
O2 Yb1 C31 82.78(13) . 2_556 ?
O7 Yb1 C31 20.57(12) 2_556 2_556 ?
O4 Yb1 C31 91.55(14) . 2_556 ?
O8 Yb1 C31 49.71(12) . 2_556 ?
N4 Yb1 C31 97.42(13) . 2_556 ?
N1 Yb1 C31 103.36(14) . 2_556 ?
N3 Yb1 C31 119.43(13) . 2_556 ?
N2 Yb1 C31 166.44(14) . 2_556 ?
O2 Yb1 C31 78.80(13) . . ?
O7 Yb1 C31 49.63(12) 2_556 . ?
O4 Yb1 C31 112.72(13) . . ?
O8 Yb1 C31 20.64(12) . . ?
N4 Yb1 C31 83.28(13) . . ?
N1 Yb1 C31 127.30(14) . . ?
N3 Yb1 C31 90.48(13) . . ?
N2 Yb1 C31 164.44(14) . . ?
C31 Yb1 C31 29.08(17) 2_556 . ?
O3 S1 O1 114.8(3) . . ?
O3 S1 O2 110.9(2) . . ?
O1 S1 O2 112.0(2) . . ?
O5 S3 O6 114.7(4) . . ?
O5 S3 O4 111.1(3) . . ?
O6 S3 O4 111.2(3) . . ?
S1 O2 Yb1 143.2(2) . . ?
S3 O4 Yb1 154.4(3) . . ?
C31 O7 Yb1 119.6(3) . 2_556 ?
C31 O8 Yb1 118.0(3) . . ?
C1 N1 C12 117.7(5) . . ?
C1 N1 Yb1 122.7(4) . . ?
C12 N1 Yb1 119.5(4) . . ?
C10 N2 C11 117.6(5) . . ?
C10 N2 Yb1 123.7(4) . . ?
C11 N2 Yb1 118.2(4) . . ?
C13 N3 C24 117.4(4) . . ?
C13 N3 Yb1 124.8(3) . . ?
C24 N3 Yb1 117.5(3) . . ?
C22 N4 C23 117.4(4) . . ?
C22 N4 Yb1 123.6(3) . . ?
C23 N4 Yb1 118.4(3) . . ?
N1 C1 C2 122.9(6) . . ?
N1 C1 H1A 118.6 . . ?
C2 C1 H1A 118.6 . . ?
C3 C2 C1 119.1(7) . . ?
C3 C2 H2A 120.4 . . ?
C1 C2 H2A 120.4 . . ?
C2 C3 C4 120.2(6) . . ?
C2 C3 H3A 119.9 . . ?
C4 C3 H3A 119.9 . . ?
C3 C4 C12 117.8(6) . . ?
C3 C4 C5 123.8(6) . . ?
C12 C4 C5 118.4(7) . . ?
C6 C5 C4 121.4(6) . . ?
C6 C5 H5A 119.3 . . ?
C4 C5 H5A 119.3 . . ?
C5 C6 C7 122.2(7) . . ?
C5 C6 H6A 118.9 . . ?
C7 C6 H6A 118.9 . . ?
C8 C7 C6 123.6(7) . . ?
C8 C7 C11 118.0(7) . . ?
C6 C7 C11 118.4(7) . . ?
C9 C8 C7 120.1(7) . . ?
C9 C8 H8A 120.0 . . ?
C7 C8 H8A 120.0 . . ?
C8 C9 C10 119.0(7) . . ?
C8 C9 H9A 120.5 . . ?
C10 C9 H9A 120.5 . . ?
N2 C10 C9 123.4(7) . . ?
N2 C10 H10A 126.2 . . ?
C9 C10 H10A 108.7 . . ?
N2 C11 C7 122.0(6) . . ?
N2 C11 C12 118.4(5) . . ?
C7 C11 C12 119.6(6) . . ?
N1 C12 C4 122.3(6) . . ?
N1 C12 C11 117.7(5) . . ?
C4 C12 C11 119.9(5) . . ?
N3 C13 C14 123.8(5) . . ?
N3 C13 H13A 118.1 . . ?
C14 C13 H13A 118.1 . . ?
C15 C14 C13 118.5(5) . . ?
C15 C14 H14A 120.8 . . ?
C13 C14 H14A 120.8 . . ?
C14 C15 C16 120.5(5) . . ?
C14 C15 H15A 119.8 . . ?
C16 C15 H15A 119.8 . . ?
C15 C16 C24 117.6(5) . . ?
C15 C16 C17 123.4(5) . . ?
C24 C16 C17 119.0(5) . . ?
C18 C17 C16 121.3(5) . . ?
C18 C17 H17A 119.3 . . ?
C16 C17 H17A 116.7 . . ?
C17 C18 C19 121.2(5) . . ?
C17 C18 H18A 119.4 . . ?
C19 C18 H18A 119.4 . . ?
C20 C19 C23 118.2(5) . . ?
C20 C19 C18 122.2(5) . . ?
C23 C19 C18 119.5(5) . . ?
C21 C20 C19 118.6(5) . . ?
C21 C20 H20A 120.7 . . ?
C19 C20 H20A 120.7 . . ?
C20 C21 C22 120.4(5) . . ?
C20 C21 H21A 119.8 . . ?
C22 C21 H21A 119.8 . . ?
N4 C22 C21 123.0(5) . . ?
N4 C22 H22A 117.2 . . ?
C21 C22 H22A 118.8 . . ?
N4 C23 C19 122.3(5) . . ?
N4 C23 C24 118.3(5) . . ?
C19 C23 C24 119.4(5) . . ?
N3 C24 C16 122.2(5) . . ?
N3 C24 C23 118.2(4) . . ?
C16 C24 C23 119.6(5) . . ?
C26 C25 C30 120.0 . . ?
C25 C26 C27 120.0 . . ?
C25 C26 H26 120.0 . . ?
C27 C26 H26 120.0 . . ?
C28 C27 C26 120.0 . . ?
C28 C27 H27 120.0 . . ?
C26 C27 H27 120.0 . . ?
C27 C28 C29 120.0 . . ?
C30 C29 C28 120.0 . . ?
C30 C29 H29 120.0 . . ?
C28 C29 H29 120.0 . . ?
N5 C30 C29 115.6(13) . . ?
N5 C30 C25 124.4(13) . . ?
C29 C30 C25 120.0 . . ?
C30 N5 H5B 120.0 . . ?
C30 N5 H5C 120.0 . . ?
H5B N5 H5C 120.0 . . ?
O8 C31 O7 128.0(5) . . ?
O8 C31 C31 115.7(5) . 2_556 ?
O7 C31 C31 116.2(5) . 2_556 ?
O8 C31 Yb1 167.6(3) . 2_556 ?
O7 C31 Yb1 39.8(2) . 2_556 ?
C31 C31 Yb1 76.5(4) 2_556 2_556 ?
O8 C31 Yb1 41.4(2) . . ?
O7 C31 Yb1 169.2(3) . . ?
C31 C31 Yb1 74.4(4) 2_556 . ?
Yb1 C31 Yb1 150.92(17) 2_556 . ?
C33 C32 C37 120.0 . . ?
C32 C33 C34 120.0 . . ?
C32 C33 H33 120.0 . . ?
C34 C33 H33 120.0 . . ?
C35 C34 C33 120.0 . . ?
C35 C34 N6 128.1(10) . . ?
C33 C34 N6 111.9(10) . . ?
C34 C35 C36 120.0 . . ?
C37 C36 C35 120.0 . . ?
C37 C36 H36 120.0 . . ?
C35 C36 H36 120.0 . . ?
C36 C37 C32 120.0 . . ?
C36 C37 H37 120.0 . . ?
C32 C37 H37 120.0 . . ?
C34 N6 H6B 120.0 . . ?
C34 N6 H6C 120.0 . . ?
H6B N6 H6C 120.0 . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         1.353
_refine_diff_density_min         -0.820
_refine_diff_density_rms         0.122


_database_code_depnum_ccdc_archive 'CCDC 981696'
