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

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#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
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# 
#  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.
#
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#  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
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#  data retrieval see:
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#  from this site to visualise CIF-encoded structures and 
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data_compound1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C8 H5 K N4 O10.50 S2 La'
_chemical_formula_sum            'C8 H5 K La N4 O10.50 S2'
_chemical_formula_weight         567.29

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   c2/c

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

_cell_length_a                   18.175(3)
_cell_length_b                   8.3359(14)
_cell_length_c                   20.600(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.868(3)
_cell_angle_gamma                90.00
_cell_volume                     3119.3(9)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2777
_cell_measurement_theta_min      1.98
_cell_measurement_theta_max      25.16

_exptl_crystal_description       block
_exptl_crystal_colour            COLORLESS
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.19
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    2.416
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2184
_exptl_absorpt_coefficient_mu    3.341
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.3357
_exptl_absorpt_correction_T_max  0.4314
_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 9.00cm
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            7800
_diffrn_reflns_av_R_equivalents  0.0222
_diffrn_reflns_av_sigmaI/netI    0.0263
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.98
_diffrn_reflns_theta_max         25.16
_reflns_number_total             2777
_reflns_number_gt                2388
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXP-97
_computing_publication_material  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. Standard DFIX restraints were
used for the distance of the atoms, such as (o9 and h9a), (o9 and h9b),
(o2w and h2), (h9a and h9b), (o1w and h1a), (o1w and h1b), (h1a and h1b).
;

_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)+(0.0220P)²+4.9828P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    none
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2777
_refine_ls_number_parameters     255
_refine_ls_number_restraints     11
_refine_ls_R_factor_all          0.0253
_refine_ls_R_factor_gt           0.0210
_refine_ls_wR_factor_ref         0.0526
_refine_ls_wR_factor_gt          0.0499
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.117
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
La1 La 0.206582(9) 0.002569(19) 0.479426(8) 0.01392(8) Uani 1 1 d . . .
K1 K 0.00423(4) -0.00249(8) 0.59942(4) 0.02972(19) Uani 1 1 d D . .
S1 S 0.15595(6) -0.45248(13) 0.21038(5) 0.0381(2) Uani 1 1 d . . .
S2 S -0.02313(5) -0.50051(10) 0.62789(5) 0.0308(2) Uani 1 1 d . . .
O1 O 0.13052(12) -0.1194(3) 0.37817(11) 0.0252(5) Uani 1 1 d . . .
O2 O 0.25053(11) -0.1595(3) 0.38558(10) 0.0232(5) Uani 1 1 d . . .
O3 O 0.28223(14) -0.5261(3) 0.40126(12) 0.0280(6) Uani 1 1 d . . .
O4 O 0.36574(14) -0.4412(4) 0.33224(12) 0.0440(7) Uani 1 1 d . . .
O5 O 0.09919(12) -0.1602(2) 0.52012(11) 0.0261(5) Uani 1 1 d . . .
O6 O 0.17591(11) -0.3509(3) 0.49428(10) 0.0234(5) Uani 1 1 d . . .
O7 O 0.18465(11) -0.6849(2) 0.52055(11) 0.0214(5) Uani 1 1 d . . .
O8 O 0.08644(11) -0.8334(2) 0.50189(11) 0.0232(5) Uani 1 1 d . . .
O9 O 0.19044(15) 0.1997(3) 0.38565(12) 0.0362(6) Uani 1 1 d D . .
N1 N 0.13414(15) -0.3105(3) 0.26069(13) 0.0258(6) Uani 1 1 d . . .
N2 N 0.22998(18) -0.5183(3) 0.24867(15) 0.0338(8) Uani 1 1 d . . .
N3 N 0.02204(14) -0.3550(3) 0.59610(13) 0.0236(6) Uani 1 1 d . . .
N4 N 0.01826(14) -0.6494(3) 0.59410(14) 0.0244(6) Uani 1 1 d . . .
C1 C 0.18522(16) -0.3094(4) 0.30757(14) 0.0178(6) Uani 1 1 d . . .
C2 C 0.23977(17) -0.4287(4) 0.30050(15) 0.0198(7) Uani 1 1 d . . .
C3 C 0.18770(17) -0.1861(4) 0.36029(14) 0.0187(7) Uani 1 1 d . . .
C4 C 0.30269(19) -0.4659(4) 0.34820(16) 0.0220(7) Uani 1 1 d . . .
C5 C 0.07217(16) -0.4180(4) 0.55816(14) 0.0158(6) Uani 1 1 d . . .
C6 C 0.06993(16) -0.5890(4) 0.55736(15) 0.0168(6) Uani 1 1 d . . .
C7 C 0.11949(16) -0.3024(4) 0.52130(14) 0.0167(6) Uani 1 1 d . . .
C8 C 0.11661(16) -0.7093(4) 0.52294(15) 0.0172(7) Uani 1 1 d . . .
O1W O -0.08523(18) -0.1933(4) 0.71708(14) 0.0555(8) Uani 1 1 d D . .
O2W O 0.0000 0.1003(5) 0.7500 0.0733(16) Uani 1 2 d SD . .
H9A H 0.220(2) 0.292(4) 0.383(2) 0.080 Uiso 1 1 d D . .
H9B H 0.160(2) 0.192(5) 0.3481(16) 0.080 Uiso 1 1 d D . .
H1A H -0.104(2) -0.118(3) 0.7416(14) 0.080 Uiso 1 1 d D . .
H1B H -0.0507(14) -0.250(4) 0.7378(14) 0.080 Uiso 1 1 d D . .
H2 H -0.034(2) 0.179(4) 0.738(2) 0.080 Uiso 1 1 d 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
La1 O3 2.467(2) 7_546 ?
La1 O7 2.494(2) 7_546 ?
La1 O2 2.510(2) . ?
La1 O6 2.525(2) 7_546 ?
La1 O5 2.542(2) . ?
La1 O9 2.546(2) . ?
La1 O8 2.630(2) 1_565 ?
La1 O1 2.666(2) . ?
La1 O7 2.772(2) 1_565 ?
La1 C3 2.926(3) . ?
La1 O6 3.016(2) . ?
La1 C8 3.057(3) 1_565 ?
K1 O1 2.705(2) 5_556 ?
K1 O5 2.749(2) . ?
K1 O4 2.751(3) 7_546 ?
K1 O8 2.907(2) 1_565 ?
K1 O8 2.953(2) 5_546 ?
K1 N4 2.957(3) 1_565 ?
K1 N3 2.958(3) . ?
K1 O2W 3.2213(16) . ?
K1 O5 3.337(2) 5_556 ?
K1 O1W 3.362(3) . ?
K1 K1 4.0944(19) 5_556 ?
K1 La1 4.1125(10) 5_556 ?
S1 N1 1.631(3) . ?
S1 N2 1.632(3) . ?
S2 N3 1.615(3) . ?
S2 N4 1.620(3) . ?
O1 C3 1.245(4) . ?
O1 K1 2.705(2) 5_556 ?
O2 C3 1.259(4) . ?
O3 C4 1.269(4) . ?
O3 La1 2.467(2) 7_546 ?
O4 C4 1.220(4) . ?
O4 K1 2.751(3) 7_546 ?
O5 C7 1.242(4) . ?
O5 K1 3.337(2) 5_556 ?
O6 C7 1.250(4) . ?
O6 La1 2.525(2) 7_546 ?
O7 C8 1.256(4) . ?
O7 La1 2.494(2) 7_546 ?
O7 La1 2.772(2) 1_545 ?
O8 C8 1.242(4) . ?
O8 La1 2.630(2) 1_545 ?
O8 K1 2.907(2) 1_545 ?
O8 K1 2.953(2) 5_546 ?
O9 H9A 0.94(2) . ?
O9 H9B 0.93(2) . ?
N1 C1 1.318(4) . ?
N2 C2 1.310(4) . ?
N3 C5 1.328(4) . ?
N4 C6 1.324(4) . ?
N4 K1 2.957(3) 1_545 ?
C1 C2 1.415(4) . ?
C1 C3 1.495(4) . ?
C2 C4 1.515(4) . ?
C5 C6 1.427(4) . ?
C5 C7 1.512(4) . ?
C6 C8 1.505(4) . ?
C8 La1 3.057(3) 1_545 ?
O1W H1A 0.879(19) . ?
O1W H1B 0.884(18) . ?
O2W K1 3.2213(16) 2_556 ?
O2W H2 0.92(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 La1 O7 84.94(8) 7_546 7_546 ?
O3 La1 O2 142.37(7) 7_546 . ?
O7 La1 O2 93.21(7) 7_546 . ?
O3 La1 O6 77.55(8) 7_546 7_546 ?
O7 La1 O6 68.91(7) 7_546 7_546 ?
O2 La1 O6 66.90(7) . 7_546 ?
O3 La1 O5 75.70(8) 7_546 . ?
O7 La1 O5 160.50(8) 7_546 . ?
O2 La1 O5 103.53(7) . . ?
O6 La1 O5 108.38(7) 7_546 . ?
O3 La1 O9 135.09(8) 7_546 . ?
O7 La1 O9 71.24(8) 7_546 . ?
O2 La1 O9 78.16(8) . . ?
O6 La1 O9 124.17(8) 7_546 . ?
O5 La1 O9 121.61(8) . . ?
O3 La1 O8 79.94(8) 7_546 1_565 ?
O7 La1 O8 110.23(7) 7_546 1_565 ?
O2 La1 O8 134.60(7) . 1_565 ?
O6 La1 O8 157.47(7) 7_546 1_565 ?
O5 La1 O8 64.44(7) . 1_565 ?
O9 La1 O8 73.86(8) . 1_565 ?
O3 La1 O1 146.46(8) 7_546 . ?
O7 La1 O1 128.56(7) 7_546 . ?
O2 La1 O1 50.37(7) . . ?
O6 La1 O1 112.97(7) 7_546 . ?
O5 La1 O1 70.75(7) . . ?
O9 La1 O1 66.95(7) . . ?
O8 La1 O1 85.62(7) 1_565 . ?
O3 La1 O7 68.22(7) 7_546 1_565 ?
O7 La1 O7 63.20(7) 7_546 1_565 ?
O2 La1 O7 142.53(7) . 1_565 ?
O6 La1 O7 122.27(7) 7_546 1_565 ?
O5 La1 O7 106.33(6) . 1_565 ?
O9 La1 O7 67.11(8) . 1_565 ?
O8 La1 O7 47.87(6) 1_565 1_565 ?
O1 La1 O7 121.42(6) . 1_565 ?
O3 La1 C3 151.87(8) 7_546 . ?
O7 La1 C3 113.52(8) 7_546 . ?
O2 La1 C3 25.34(8) . . ?
O6 La1 C3 89.20(8) 7_546 . ?
O5 La1 C3 85.38(8) . . ?
O9 La1 C3 72.73(8) . . ?
O8 La1 C3 110.60(8) 1_565 . ?
O1 La1 C3 25.19(8) . . ?
O7 La1 C3 138.37(7) 1_565 . ?
O3 La1 O6 89.20(7) 7_546 . ?
O7 La1 O6 138.12(6) 7_546 . ?
O2 La1 O6 67.48(7) . . ?
O6 La1 O6 69.33(7) 7_546 . ?
O5 La1 O6 45.47(6) . . ?
O9 La1 O6 133.67(7) . . ?
O8 La1 O6 109.44(6) 1_565 . ?
O1 La1 O6 67.30(6) . . ?
O7 La1 O6 149.10(6) 1_565 . ?
C3 La1 O6 62.80(7) . . ?
O3 La1 C8 70.91(8) 7_546 1_565 ?
O7 La1 C8 87.29(7) 7_546 1_565 ?
O2 La1 C8 146.67(7) . 1_565 ?
O6 La1 C8 141.93(7) 7_546 1_565 ?
O5 La1 C8 84.19(7) . 1_565 ?
O9 La1 C8 70.47(8) . 1_565 ?
O8 La1 C8 23.75(7) 1_565 1_565 ?
O1 La1 C8 105.09(7) . 1_565 ?
O7 La1 C8 24.26(7) 1_565 1_565 ?
C3 La1 C8 128.26(8) . 1_565 ?
O6 La1 C8 129.46(7) . 1_565 ?
O1 K1 O5 150.50(8) 5_556 . ?
O1 K1 O4 138.08(8) 5_556 7_546 ?
O5 K1 O4 71.16(8) . 7_546 ?
O1 K1 O8 115.12(7) 5_556 1_565 ?
O5 K1 O8 58.30(7) . 1_565 ?
O4 K1 O8 89.08(7) 7_546 1_565 ?
O1 K1 O8 78.88(6) 5_556 5_546 ?
O5 K1 O8 72.85(7) . 5_546 ?
O4 K1 O8 137.13(8) 7_546 5_546 ?
O8 K1 O8 91.36(6) 1_565 5_546 ?
O1 K1 N4 73.27(7) 5_556 1_565 ?
O5 K1 N4 113.41(7) . 1_565 ?
O4 K1 N4 96.60(9) 7_546 1_565 ?
O8 K1 N4 56.27(7) 1_565 1_565 ?
O8 K1 N4 118.81(7) 5_546 1_565 ?
O1 K1 N3 118.52(7) 5_556 . ?
O5 K1 N3 55.94(7) . . ?
O4 K1 N3 75.50(9) 7_546 . ?
O8 K1 N3 114.00(7) 1_565 . ?
O8 K1 N3 65.31(7) 5_546 . ?
N4 K1 N3 168.14(8) 1_565 . ?
O1 K1 O2W 71.68(6) 5_556 . ?
O5 K1 O2W 137.26(7) . . ?
O4 K1 O2W 66.41(6) 7_546 . ?
O8 K1 O2W 124.43(8) 1_565 . ?
O8 K1 O2W 140.67(6) 5_546 . ?
N4 K1 O2W 77.04(10) 1_565 . ?
N3 K1 O2W 107.01(10) . . ?
O1 K1 O5 58.80(6) 5_556 5_556 ?
O5 K1 O5 96.04(6) . 5_556 ?
O4 K1 O5 154.24(8) 7_546 5_556 ?
O8 K1 O5 65.34(6) 1_565 5_556 ?
O8 K1 O5 51.59(6) 5_546 5_556 ?
N4 K1 O5 67.38(7) 1_565 5_556 ?
N3 K1 O5 116.50(7) . 5_556 ?
O2W K1 O5 124.89(7) . 5_556 ?
O1 K1 O1W 65.97(8) 5_556 . ?
O5 K1 O1W 122.00(8) . . ?
O4 K1 O1W 88.74(8) 7_546 . ?
O8 K1 O1W 177.51(7) 1_565 . ?
O8 K1 O1W 91.06(7) 5_546 . ?
N4 K1 O1W 122.82(8) 1_565 . ?
N3 K1 O1W 66.58(8) . . ?
O2W K1 O1W 53.44(8) . . ?
O5 K1 O1W 116.76(7) 5_556 . ?
O1 K1 K1 99.34(6) 5_556 5_556 ?
O5 K1 K1 54.14(5) . 5_556 ?
O4 K1 K1 121.14(6) 7_546 5_556 ?
O8 K1 K1 46.14(5) 1_565 5_556 ?
O8 K1 K1 45.23(5) 5_546 5_556 ?
N4 K1 K1 87.32(6) 1_565 5_556 ?
N3 K1 K1 89.28(6) . 5_556 ?
O2W K1 K1 163.61(8) . 5_556 ?
O5 K1 K1 41.90(4) 5_556 5_556 ?
O1W K1 K1 136.28(6) . 5_556 ?
O1 K1 La1 39.68(5) 5_556 5_556 ?
O5 K1 La1 111.10(5) . 5_556 ?
O4 K1 La1 167.35(7) 7_546 5_556 ?
O8 K1 La1 102.73(5) 1_565 5_556 ?
O8 K1 La1 39.60(4) 5_546 5_556 ?
N4 K1 La1 93.78(6) 1_565 5_556 ?
N3 K1 La1 95.28(5) . 5_556 ?
O2W K1 La1 109.22(2) . 5_556 ?
O5 K1 La1 38.13(4) 5_556 5_556 ?
O1W K1 La1 79.54(6) . 5_556 ?
K1 K1 La1 66.47(2) 5_556 5_556 ?
N1 S1 N2 98.65(14) . . ?
N3 S2 N4 98.71(15) . . ?
C3 O1 La1 89.15(18) . . ?
C3 O1 K1 170.9(2) . 5_556 ?
La1 O1 K1 99.94(7) . 5_556 ?
C3 O2 La1 96.11(18) . . ?
C4 O3 La1 144.1(2) . 7_546 ?
C4 O4 K1 129.2(2) . 7_546 ?
C7 O5 La1 106.57(19) . . ?
C7 O5 K1 129.6(2) . . ?
La1 O5 K1 116.39(8) . . ?
C7 O5 K1 124.21(19) . 5_556 ?
La1 O5 K1 87.70(7) . 5_556 ?
K1 O5 K1 83.96(6) . 5_556 ?
C7 O6 La1 140.08(19) . 7_546 ?
C7 O6 La1 83.47(18) . . ?
La1 O6 La1 110.67(7) 7_546 . ?
C8 O7 La1 151.7(2) . 7_546 ?
C8 O7 La1 90.65(18) . 1_545 ?
La1 O7 La1 116.80(7) 7_546 1_545 ?
C8 O8 La1 97.75(18) . 1_545 ?
C8 O8 K1 113.2(2) . 1_545 ?
La1 O8 K1 108.53(7) 1_545 1_545 ?
C8 O8 K1 149.6(2) . 5_546 ?
La1 O8 K1 94.71(7) 1_545 5_546 ?
K1 O8 K1 88.64(6) 1_545 5_546 ?
La1 O9 H9A 122(3) . . ?
La1 O9 H9B 129(3) . . ?
H9A O9 H9B 109(3) . . ?
C1 N1 S1 106.9(2) . . ?
C2 N2 S1 106.9(2) . . ?
C5 N3 S2 108.0(2) . . ?
C5 N3 K1 119.0(2) . . ?
S2 N3 K1 132.78(14) . . ?
C6 N4 S2 107.6(2) . . ?
C6 N4 K1 117.6(2) . 1_545 ?
S2 N4 K1 134.81(14) . 1_545 ?
N1 C1 C2 113.5(3) . . ?
N1 C1 C3 122.8(3) . . ?
C2 C1 C3 123.6(3) . . ?
N2 C2 C1 114.0(3) . . ?
N2 C2 C4 119.4(3) . . ?
C1 C2 C4 126.4(3) . . ?
O1 C3 O2 123.6(3) . . ?
O1 C3 C1 121.1(3) . . ?
O2 C3 C1 115.3(3) . . ?
O1 C3 La1 65.66(17) . . ?
O2 C3 La1 58.55(15) . . ?
C1 C3 La1 168.2(2) . . ?
O4 C4 O3 127.1(3) . . ?
O4 C4 C2 119.1(3) . . ?
O3 C4 C2 113.8(3) . . ?
N3 C5 C6 112.5(3) . . ?
N3 C5 C7 117.1(3) . . ?
C6 C5 C7 130.3(3) . . ?
N4 C6 C5 113.2(3) . . ?
N4 C6 C8 115.9(3) . . ?
C5 C6 C8 130.9(3) . . ?
O5 C7 O6 123.2(3) . . ?
O5 C7 C5 116.4(3) . . ?
O6 C7 C5 120.4(3) . . ?
O5 C7 La1 51.09(15) . . ?
O6 C7 La1 73.17(17) . . ?
C5 C7 La1 163.1(2) . . ?
O8 C8 O7 123.0(3) . . ?
O8 C8 C6 118.0(3) . . ?
O7 C8 C6 118.8(3) . . ?
O8 C8 La1 58.50(16) . 1_545 ?
O7 C8 La1 65.09(16) . 1_545 ?
C6 C8 La1 167.5(2) . 1_545 ?
K1 O1W H1A 106.4(13) . . ?
K1 O1W H1B 104.4(13) . . ?
H1A O1W H1B 113(3) . . ?
K1 O2W K1 149.16(16) . 2_556 ?
K1 O2W H2 89(3) . . ?
K1 O2W H2 114(3) 2_556 . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O9 H9A O3 0.94(2) 1.93(2) 2.842(3) 165(4) 1_565
O9 H9B O1W 0.93(2) 1.88(2) 2.806(4) 168(5) 5_556
O1W H1A O4 0.879(19) 2.03(2) 2.796(4) 146(2) 8_446
O1W H1B O1W 0.884(18) 2.65(3) 3.341(6) 135(3) 2_556
O2W H2 N1 0.92(2) 2.13(3) 3.005(4) 158(5) 5_556

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.16
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.400
_refine_diff_density_min         -0.459
_refine_diff_density_rms         0.092
_database_code_depnum_ccdc_archive 'CCDC 957579'
#######################################################################
#
#                 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_compound2

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C8 H5 Ce K N4 O10.50 S2'
_chemical_formula_sum            'C8 H5 Ce K N4 O10.50 S2'
_chemical_formula_weight         568.50

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   c2/c

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

_cell_length_a                   18.1735(7)
_cell_length_b                   8.3436(3)
_cell_length_c                   20.5557(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.6990(10)
_cell_angle_gamma                90.00
_cell_volume                     3115.5(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2748
_cell_measurement_theta_min      1.98
_cell_measurement_theta_max      25.06

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    2.424
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2192
_exptl_absorpt_coefficient_mu    3.525
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.3583
_exptl_absorpt_correction_T_max  0.4471
_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 9.00cm
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            7700
_diffrn_reflns_av_R_equivalents  0.0158
_diffrn_reflns_av_sigmaI/netI    0.0175
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.98
_diffrn_reflns_theta_max         25.06
_reflns_number_total             2748
_reflns_number_gt                2492
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXP-97
_computing_publication_material  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. Standard DFIX restraints were
used for the distance of the atoms, such as (o9 and h9a), (o9 and h9b),
(o2w and h2), (h9a and h9b), (o1w and h1a), (o1w and h1b), (h1a and h1b).
;

_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)+(0.0235P)²+5.6664P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2748
_refine_ls_number_parameters     255
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0210
_refine_ls_R_factor_gt           0.0187
_refine_ls_wR_factor_ref         0.0494
_refine_ls_wR_factor_gt          0.0475
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_restrained_S_all      1.098
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ce1 Ce 0.206832(7) 0.003757(15) 0.479582(7) 0.01498(7) Uani 1 1 d . . .
K1 K 0.00432(4) -0.00316(7) 0.59912(4) 0.03143(17) Uani 1 1 d D . .
S1 S 0.15570(5) -0.45069(11) 0.21074(4) 0.0407(2) Uani 1 1 d . . .
S2 S -0.02373(5) -0.49953(8) 0.62728(4) 0.03202(19) Uani 1 1 d . . .
O1 O 0.13074(10) -0.1173(2) 0.37917(9) 0.0262(4) Uani 1 1 d . . .
O2 O 0.25096(10) -0.1563(2) 0.38610(9) 0.0240(4) Uani 1 1 d . . .
O3 O 0.28187(12) -0.5254(2) 0.40199(10) 0.0287(5) Uani 1 1 d . . .
O4 O 0.36577(12) -0.4413(3) 0.33264(11) 0.0459(6) Uani 1 1 d . . .
O5 O 0.10132(10) -0.1609(2) 0.52023(10) 0.0272(4) Uani 1 1 d . . .
O6 O 0.17698(10) -0.3538(2) 0.49359(9) 0.0264(4) Uani 1 1 d . . .
O7 O 0.18551(9) -0.6855(2) 0.52119(9) 0.0234(4) Uani 1 1 d . . .
O8 O 0.08743(9) -0.8347(2) 0.50245(10) 0.0243(4) Uani 1 1 d . . .
O9 O 0.19070(13) 0.1996(3) 0.38643(10) 0.0375(5) Uani 1 1 d D . .
H9A H 0.218(2) 0.299(3) 0.3836(19) 0.080 Uiso 1 1 d D . .
H9B H 0.162(2) 0.183(5) 0.3470(14) 0.080 Uiso 1 1 d D . .
N1 N 0.13426(13) -0.3077(3) 0.26139(11) 0.0279(5) Uani 1 1 d . . .
N2 N 0.22968(17) -0.5170(3) 0.24895(14) 0.0368(7) Uani 1 1 d . . .
N3 N 0.02211(12) -0.3545(3) 0.59557(11) 0.0244(5) Uani 1 1 d . . .
N4 N 0.01789(12) -0.6492(3) 0.59375(12) 0.0254(5) Uani 1 1 d . . .
C1 C 0.18547(13) -0.3071(3) 0.30811(12) 0.0186(5) Uani 1 1 d . . .
C2 C 0.23965(14) -0.4276(3) 0.30107(12) 0.0213(6) Uani 1 1 d . . .
C3 C 0.18819(14) -0.1838(3) 0.36088(12) 0.0198(5) Uani 1 1 d . . .
C4 C 0.30249(15) -0.4657(3) 0.34863(13) 0.0226(6) Uani 1 1 d . . .
C5 C 0.07287(13) -0.4177(3) 0.55804(12) 0.0169(5) Uani 1 1 d . . .
C6 C 0.07003(13) -0.5891(3) 0.55719(12) 0.0178(5) Uani 1 1 d . . .
C7 C 0.12110(13) -0.3033(3) 0.52127(12) 0.0177(5) Uani 1 1 d . . .
C8 C 0.11719(13) -0.7097(3) 0.52336(12) 0.0170(5) Uani 1 1 d . . .
O1W O -0.08498(16) -0.1935(3) 0.71674(12) 0.0583(7) Uani 1 1 d D . .
O2W O 0.0000 0.0989(5) 0.7500 0.0791(14) Uani 1 2 d SD . .
H2 H 0.0376(18) 0.178(4) 0.758(2) 0.080 Uiso 1 1 d D . .
H1B H -0.1161(17) -0.132(3) 0.7488(13) 0.080 Uiso 1 1 d D . .
H1A H -0.0534(14) -0.271(4) 0.7449(14) 0.080 Uiso 1 1 d 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
Ce1 O3 2.444(2) 7_546 ?
Ce1 O7 2.4759(17) 7_546 ?
Ce1 O2 2.4921(17) . ?
Ce1 O6 2.5017(18) 7_546 ?
Ce1 O5 2.5215(18) . ?
Ce1 O9 2.528(2) . ?
Ce1 O8 2.6089(17) 1_565 ?
Ce1 O1 2.6501(18) . ?
Ce1 O7 2.7609(18) 1_565 ?
Ce1 C3 2.910(3) . ?
Ce1 C8 3.044(2) 1_565 ?
Ce1 K1 4.1199(7) 5_556 ?
K1 O1 2.7014(19) 5_556 ?
K1 O4 2.750(2) 7_546 ?
K1 O5 2.764(2) . ?
K1 O8 2.895(2) 1_565 ?
K1 N3 2.951(2) . ?
K1 O8 2.9599(19) 5_546 ?
K1 N4 2.966(2) 1_565 ?
K1 O2W 3.2195(13) . ?
K1 O1W 3.352(3) . ?
K1 O5 3.361(2) 5_556 ?
K1 K1 4.0735(16) 5_556 ?
K1 Ce1 4.1199(7) 5_556 ?
S1 N2 1.633(3) . ?
S1 N1 1.638(2) . ?
S2 N3 1.617(2) . ?
S2 N4 1.624(2) . ?
O1 C3 1.250(3) . ?
O1 K1 2.7014(19) 5_556 ?
O2 C3 1.260(3) . ?
O3 C4 1.271(4) . ?
O3 Ce1 2.444(2) 7_546 ?
O4 C4 1.222(4) . ?
O4 K1 2.750(2) 7_546 ?
O5 C7 1.241(3) . ?
O5 K1 3.361(2) 5_556 ?
O6 C7 1.252(3) . ?
O6 Ce1 2.5017(18) 7_546 ?
O7 C8 1.260(3) . ?
O7 Ce1 2.4759(17) 7_546 ?
O7 Ce1 2.7609(18) 1_545 ?
O8 C8 1.245(3) . ?
O8 Ce1 2.6089(17) 1_545 ?
O8 K1 2.895(2) 1_545 ?
O8 K1 2.9599(19) 5_546 ?
O9 H9A 0.970(18) . ?
O9 H9B 0.960(18) . ?
N1 C1 1.317(3) . ?
N2 C2 1.314(4) . ?
N3 C5 1.329(3) . ?
N4 C6 1.325(3) . ?
N4 K1 2.966(2) 1_545 ?
C1 C2 1.418(4) . ?
C1 C3 1.494(4) . ?
C2 C4 1.515(4) . ?
C5 C6 1.431(4) . ?
C5 C7 1.513(3) . ?
C6 C8 1.506(3) . ?
C8 Ce1 3.044(2) 1_545 ?
O1W H1B 1.018(17) . ?
O1W H1A 1.029(16) . ?
O2W K1 3.2195(13) 2_556 ?
O2W H2 0.961(19) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Ce1 O7 85.30(7) 7_546 7_546 ?
O3 Ce1 O2 142.03(6) 7_546 . ?
O7 Ce1 O2 92.92(6) 7_546 . ?
O3 Ce1 O6 76.82(7) 7_546 7_546 ?
O7 Ce1 O6 69.25(6) 7_546 7_546 ?
O2 Ce1 O6 67.24(6) . 7_546 ?
O3 Ce1 O5 75.67(7) 7_546 . ?
O7 Ce1 O5 160.86(7) 7_546 . ?
O2 Ce1 O5 103.22(6) . . ?
O6 Ce1 O5 107.44(6) 7_546 . ?
O3 Ce1 O9 135.34(7) 7_546 . ?
O7 Ce1 O9 70.92(7) 7_546 . ?
O2 Ce1 O9 78.18(7) . . ?
O6 Ce1 O9 124.64(7) 7_546 . ?
O5 Ce1 O9 122.08(7) . . ?
O3 Ce1 O8 80.11(6) 7_546 1_565 ?
O7 Ce1 O8 110.27(6) 7_546 1_565 ?
O2 Ce1 O8 134.76(6) . 1_565 ?
O6 Ce1 O8 156.88(6) 7_546 1_565 ?
O5 Ce1 O8 64.98(6) . 1_565 ?
O9 Ce1 O8 73.99(7) . 1_565 ?
O3 Ce1 O1 146.16(6) 7_546 . ?
O7 Ce1 O1 128.51(6) 7_546 . ?
O2 Ce1 O1 50.78(6) . . ?
O6 Ce1 O1 113.50(6) 7_546 . ?
O5 Ce1 O1 70.49(6) . . ?
O9 Ce1 O1 67.06(6) . . ?
O8 Ce1 O1 85.38(6) 1_565 . ?
O3 Ce1 O7 68.31(6) 7_546 1_565 ?
O7 Ce1 O7 62.93(6) 7_546 1_565 ?
O2 Ce1 O7 142.50(6) . 1_565 ?
O6 Ce1 O7 121.78(6) 7_546 1_565 ?
O5 Ce1 O7 107.09(5) . 1_565 ?
O9 Ce1 O7 67.26(6) . 1_565 ?
O8 Ce1 O7 48.24(5) 1_565 1_565 ?
O1 Ce1 O7 121.62(5) . 1_565 ?
O3 Ce1 C3 151.55(7) 7_546 . ?
O7 Ce1 C3 113.36(7) 7_546 . ?
O2 Ce1 C3 25.50(6) . . ?
O6 Ce1 C3 89.56(7) 7_546 . ?
O5 Ce1 C3 85.07(7) . . ?
O9 Ce1 C3 72.82(7) . . ?
O8 Ce1 C3 110.62(7) 1_565 . ?
O1 Ce1 C3 25.44(6) . . ?
O7 Ce1 C3 138.66(6) 1_565 . ?
O3 Ce1 C8 71.18(7) 7_546 1_565 ?
O7 Ce1 C8 87.18(6) 7_546 1_565 ?
O2 Ce1 C8 146.73(6) . 1_565 ?
O6 Ce1 C8 141.56(6) 7_546 1_565 ?
O5 Ce1 C8 84.90(6) . 1_565 ?
O9 Ce1 C8 70.44(7) . 1_565 ?
O8 Ce1 C8 23.90(6) 1_565 1_565 ?
O1 Ce1 C8 104.95(6) . 1_565 ?
O7 Ce1 C8 24.45(6) 1_565 1_565 ?
C3 Ce1 C8 128.33(7) . 1_565 ?
O3 Ce1 K1 116.17(5) 7_546 5_556 ?
O7 Ce1 K1 136.49(4) 7_546 5_556 ?
O2 Ce1 K1 90.79(4) . 5_556 ?
O6 Ce1 K1 148.89(5) 7_546 5_556 ?
O5 Ce1 K1 54.61(5) . 5_556 ?
O9 Ce1 K1 67.52(5) . 5_556 ?
O8 Ce1 K1 45.68(4) 1_565 5_556 ?
O1 Ce1 K1 40.12(4) . 5_556 ?
O7 Ce1 K1 89.15(4) 1_565 5_556 ?
C3 Ce1 K1 65.56(5) . 5_556 ?
C8 Ce1 K1 67.45(5) 1_565 5_556 ?
O1 K1 O4 138.50(7) 5_556 7_546 ?
O1 K1 O5 150.75(7) 5_556 . ?
O4 K1 O5 70.50(7) 7_546 . ?
O1 K1 O8 115.33(6) 5_556 1_565 ?
O4 K1 O8 88.53(6) 7_546 1_565 ?
O5 K1 O8 58.25(6) . 1_565 ?
O1 K1 N3 118.32(6) 5_556 . ?
O4 K1 N3 75.65(8) 7_546 . ?
O5 K1 N3 55.95(6) . . ?
O8 K1 N3 113.93(6) 1_565 . ?
O1 K1 O8 77.93(5) 5_556 5_546 ?
O4 K1 O8 137.74(7) 7_546 5_546 ?
O5 K1 O8 74.00(6) . 5_546 ?
O8 K1 O8 91.84(5) 1_565 5_546 ?
N3 K1 O8 65.70(6) . 5_546 ?
O1 K1 N4 73.31(6) 5_556 1_565 ?
O4 K1 N4 96.64(8) 7_546 1_565 ?
O5 K1 N4 113.40(6) . 1_565 ?
O8 K1 N4 56.32(6) 1_565 1_565 ?
N3 K1 N4 168.28(7) . 1_565 ?
O8 K1 N4 118.33(6) 5_546 1_565 ?
O1 K1 O2W 72.20(5) 5_556 . ?
O4 K1 O2W 66.30(6) 7_546 . ?
O5 K1 O2W 136.49(6) . . ?
O8 K1 O2W 124.12(7) 1_565 . ?
N3 K1 O2W 107.00(8) . . ?
O8 K1 O2W 140.44(5) 5_546 . ?
N4 K1 O2W 77.11(8) 1_565 . ?
O1 K1 O1W 66.13(7) 5_556 . ?
O4 K1 O1W 88.80(7) 7_546 . ?
O5 K1 O1W 121.90(7) . . ?
O8 K1 O1W 177.03(6) 1_565 . ?
N3 K1 O1W 66.60(7) . . ?
O8 K1 O1W 91.01(6) 5_546 . ?
N4 K1 O1W 122.76(7) 1_565 . ?
O2W K1 O1W 53.43(7) . . ?
O1 K1 O5 57.80(5) 5_556 5_556 ?
O4 K1 O5 154.71(7) 7_546 5_556 ?
O5 K1 O5 97.25(5) . 5_556 ?
O8 K1 O5 66.40(5) 1_565 5_556 ?
N3 K1 O5 116.57(6) . 5_556 ?
O8 K1 O5 51.23(5) 5_546 5_556 ?
N4 K1 O5 67.27(6) 1_565 5_556 ?
O2W K1 O5 124.45(6) . 5_556 ?
O1W K1 O5 116.18(6) . 5_556 ?
O1 K1 K1 98.76(5) 5_556 5_556 ?
O4 K1 K1 121.30(6) 7_546 5_556 ?
O5 K1 K1 54.95(5) . 5_556 ?
O8 K1 K1 46.57(4) 1_565 5_556 ?
N3 K1 K1 89.38(5) . 5_556 ?
O8 K1 K1 45.27(4) 5_546 5_556 ?
N4 K1 K1 87.17(5) 1_565 5_556 ?
O2W K1 K1 163.52(7) . 5_556 ?
O1W K1 K1 136.27(5) . 5_556 ?
O5 K1 K1 42.31(3) 5_556 5_556 ?
O1 K1 Ce1 39.20(4) 5_556 5_556 ?
O4 K1 Ce1 167.37(6) 7_546 5_556 ?
O5 K1 Ce1 111.83(5) . 5_556 ?
O8 K1 Ce1 103.29(4) 1_565 5_556 ?
N3 K1 Ce1 95.20(5) . 5_556 ?
O8 K1 Ce1 39.10(3) 5_546 5_556 ?
N4 K1 Ce1 93.68(5) 1_565 5_556 ?
O2W K1 Ce1 109.243(19) . 5_556 ?
O1W K1 Ce1 79.48(5) . 5_556 ?
O5 K1 Ce1 37.70(3) 5_556 5_556 ?
K1 K1 Ce1 66.387(18) 5_556 5_556 ?
N2 S1 N1 98.56(12) . . ?
N3 S2 N4 98.76(13) . . ?
C3 O1 Ce1 88.99(15) . . ?
C3 O1 K1 170.33(17) . 5_556 ?
Ce1 O1 K1 100.68(6) . 5_556 ?
C3 O2 Ce1 96.14(15) . . ?
C4 O3 Ce1 144.33(18) . 7_546 ?
C4 O4 K1 129.43(19) . 7_546 ?
C7 O5 Ce1 107.73(16) . . ?
C7 O5 K1 129.43(17) . . ?
Ce1 O5 K1 116.07(7) . . ?
C7 O5 K1 124.13(16) . 5_556 ?
Ce1 O5 K1 87.69(5) . 5_556 ?
K1 O5 K1 82.75(5) . 5_556 ?
C7 O6 Ce1 139.38(17) . 7_546 ?
C8 O7 Ce1 151.42(16) . 7_546 ?
C8 O7 Ce1 90.45(14) . 1_545 ?
Ce1 O7 Ce1 117.07(6) 7_546 1_545 ?
C8 O8 Ce1 98.03(14) . 1_545 ?
C8 O8 K1 113.55(16) . 1_545 ?
Ce1 O8 K1 109.06(6) 1_545 1_545 ?
C8 O8 K1 148.86(16) . 5_546 ?
Ce1 O8 K1 95.22(6) 1_545 5_546 ?
K1 O8 K1 88.16(5) 1_545 5_546 ?
Ce1 O9 H9A 123(2) . . ?
Ce1 O9 H9B 126(2) . . ?
H9A O9 H9B 110(2) . . ?
C1 N1 S1 106.86(19) . . ?
C2 N2 S1 107.0(2) . . ?
C5 N3 S2 108.19(18) . . ?
C5 N3 K1 119.13(16) . . ?
S2 N3 K1 132.48(12) . . ?
C6 N4 S2 107.41(18) . . ?
C6 N4 K1 117.37(17) . 1_545 ?
S2 N4 K1 135.21(12) . 1_545 ?
N1 C1 C2 113.6(2) . . ?
N1 C1 C3 122.6(2) . . ?
C2 C1 C3 123.6(2) . . ?
N2 C2 C1 114.0(2) . . ?
N2 C2 C4 119.3(2) . . ?
C1 C2 C4 126.6(2) . . ?
O1 C3 O2 123.3(2) . . ?
O1 C3 C1 120.9(2) . . ?
O2 C3 C1 115.7(2) . . ?
O1 C3 Ce1 65.57(14) . . ?
O2 C3 Ce1 58.36(13) . . ?
C1 C3 Ce1 168.29(17) . . ?
O4 C4 O3 126.9(3) . . ?
O4 C4 C2 119.3(3) . . ?
O3 C4 C2 113.8(2) . . ?
N3 C5 C6 112.2(2) . . ?
N3 C5 C7 117.5(2) . . ?
C6 C5 C7 130.2(2) . . ?
N4 C6 C5 113.4(2) . . ?
N4 C6 C8 115.8(2) . . ?
C5 C6 C8 130.8(2) . . ?
O5 C7 O6 123.6(2) . . ?
O5 C7 C5 116.1(2) . . ?
O6 C7 C5 120.3(2) . . ?
O8 C8 O7 122.7(2) . . ?
O8 C8 C6 118.2(2) . . ?
O7 C8 C6 119.0(2) . . ?
O8 C8 Ce1 58.07(13) . 1_545 ?
O7 C8 Ce1 65.09(13) . 1_545 ?
C6 C8 Ce1 168.13(17) . 1_545 ?
K1 O1W H1B 121.3(15) . . ?
K1 O1W H1A 115.4(13) . . ?
H1B O1W H1A 105.0(18) . . ?
K1 O2W K1 149.33(14) . 2_556 ?
K1 O2W H2 108(3) . . ?
K1 O2W H2 93(3) 2_556 . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O9 H9A O3 0.970(18) 1.899(19) 2.843(3) 164(3) 1_565
O9 H9B O1W 0.960(18) 1.89(2) 2.820(3) 162(4) 5_556
O2W H2 N1 0.961(19) 2.06(2) 3.002(3) 165(4) 6_556
O1W H1B O4 1.018(17) 1.87(2) 2.805(4) 152(3) 8_446

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.06
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.430
_refine_diff_density_min         -0.356
_refine_diff_density_rms         0.074
_database_code_depnum_ccdc_archive 'CCDC 957580'
#######################################################################
#
#                 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_compound3

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C8 H5 K N4 O10.50 Pr S2'
_chemical_formula_sum            'C8 H5 K N4 O10.50 Pr S2'
_chemical_formula_weight         569.29

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   c2/c

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

_cell_length_a                   18.1389(14)
_cell_length_b                   8.3629(6)
_cell_length_c                   20.4829(15)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.5050(10)
_cell_angle_gamma                90.00
_cell_volume                     3106.1(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2749
_cell_measurement_theta_min      1.99
_cell_measurement_theta_max      25.07

_exptl_crystal_description       block
_exptl_crystal_colour            COLORLESS
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.19
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    2.435
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2200
_exptl_absorpt_coefficient_mu    3.742
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.3357
_exptl_absorpt_correction_T_max  0.4314
_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 9.00cm
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            7705
_diffrn_reflns_av_R_equivalents  0.0164
_diffrn_reflns_av_sigmaI/netI    0.0186
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.99
_diffrn_reflns_theta_max         25.07
_reflns_number_total             2749
_reflns_number_gt                2457
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXP-97
_computing_publication_material  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. Standard DFIX restraints were
used for the distance of the atoms, such as (o9 and h9a), (o9 and h9b),
(o2w and h2), (h9a and h9b), (o1w and h1a), (o1w and h1b), (h1a and h1b).
;

_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)+(0.0168P)²+9.0801P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    none
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2749
_refine_ls_number_parameters     255
_refine_ls_number_restraints     11
_refine_ls_R_factor_all          0.0226
_refine_ls_R_factor_gt           0.0196
_refine_ls_wR_factor_ref         0.0446
_refine_ls_wR_factor_gt          0.0430
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_restrained_S_all      1.127
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pr1 Pr 0.207137(9) 0.006298(18) 0.479599(8) 0.01452(7) Uani 1 1 d . . .
K1 K 0.00474(4) -0.00451(9) 0.59897(4) 0.03020(18) Uani 1 1 d D . .
S1 S 0.15466(6) -0.44831(13) 0.21118(5) 0.0376(2) Uani 1 1 d . . .
S2 S -0.02442(5) -0.49862(10) 0.62711(5) 0.0304(2) Uani 1 1 d . . .
O1 O 0.13093(12) -0.1136(3) 0.38012(11) 0.0247(5) Uani 1 1 d . . .
O2 O 0.25161(12) -0.1542(3) 0.38693(10) 0.0224(5) Uani 1 1 d . . .
O3 O 0.28218(13) -0.5265(3) 0.40228(11) 0.0267(5) Uani 1 1 d . . .
O4 O 0.36572(14) -0.4394(4) 0.33255(12) 0.0429(7) Uani 1 1 d . . .
O5 O 0.10447(13) -0.1625(3) 0.52074(11) 0.0263(5) Uani 1 1 d . . .
O6 O 0.17754(12) -0.3595(3) 0.49250(11) 0.0260(5) Uani 1 1 d . . .
O7 O 0.18591(11) -0.6880(3) 0.52124(11) 0.0215(5) Uani 1 1 d . . .
O8 O 0.08706(12) -0.8361(2) 0.50226(11) 0.0229(5) Uani 1 1 d . . .
O9 O 0.19149(16) 0.1997(3) 0.38654(12) 0.0351(6) Uani 1 1 d D . .
N1 N 0.13378(15) -0.3046(3) 0.26174(13) 0.0253(6) Uani 1 1 d . . .
N2 N 0.22883(18) -0.5154(4) 0.24914(14) 0.0331(8) Uani 1 1 d . . .
N3 N 0.02258(15) -0.3543(3) 0.59530(13) 0.0233(6) Uani 1 1 d . . .
N4 N 0.01693(15) -0.6489(3) 0.59352(14) 0.0243(6) Uani 1 1 d . . .
C1 C 0.18559(17) -0.3048(4) 0.30887(15) 0.0182(7) Uani 1 1 d . . .
C2 C 0.23948(18) -0.4261(4) 0.30162(15) 0.0201(7) Uani 1 1 d . . .
C3 C 0.18857(17) -0.1811(4) 0.36180(15) 0.0184(7) Uani 1 1 d . . .
C4 C 0.30279(18) -0.4646(4) 0.34909(15) 0.0212(7) Uani 1 1 d . . .
C5 C 0.07319(16) -0.4187(4) 0.55755(14) 0.0161(6) Uani 1 1 d . . .
C6 C 0.06973(16) -0.5893(4) 0.55698(15) 0.0175(6) Uani 1 1 d . . .
C7 C 0.12221(17) -0.3063(4) 0.52078(14) 0.0175(7) Uani 1 1 d . . .
C8 C 0.11742(16) -0.7113(4) 0.52325(15) 0.0170(7) Uani 1 1 d . . .
O1W O -0.08534(18) -0.1956(4) 0.71620(14) 0.0538(8) Uani 1 1 d D . .
O2W O 0.0000 0.0955(6) 0.7500 0.0760(17) Uani 1 2 d SD . .
H9A H 0.218(2) 0.294(4) 0.388(2) 0.080 Uiso 1 1 d D . .
H9B H 0.161(2) 0.191(5) 0.3499(17) 0.080 Uiso 1 1 d D . .
H1A H -0.105(2) -0.123(3) 0.7416(15) 0.080 Uiso 1 1 d D . .
H1B H -0.0512(14) -0.252(4) 0.7380(15) 0.080 Uiso 1 1 d D . .
H2 H -0.039(2) 0.167(5) 0.745(3) 0.080 Uiso 1 1 d 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
Pr1 O3 2.428(2) 7_546 ?
Pr1 O7 2.465(2) 7_546 ?
Pr1 O2 2.477(2) . ?
Pr1 O6 2.479(2) 7_546 ?
Pr1 O5 2.501(2) . ?
Pr1 O9 2.511(2) . ?
Pr1 O8 2.598(2) 1_565 ?
Pr1 O1 2.631(2) . ?
Pr1 O7 2.726(2) 1_565 ?
Pr1 C3 2.889(3) . ?
Pr1 C8 3.017(3) 1_565 ?
Pr1 K1 4.1275(8) 5_556 ?
K1 O1 2.696(2) 5_556 ?
K1 O4 2.745(3) 7_546 ?
K1 O5 2.782(2) . ?
K1 O8 2.880(2) 1_565 ?
K1 O8 2.944(2) 5_546 ?
K1 N3 2.944(3) . ?
K1 N4 2.985(3) 1_565 ?
K1 O2W 3.2079(15) . ?
K1 O1W 3.346(3) . ?
K1 O5 3.411(3) 5_556 ?
K1 K1 4.0544(18) 5_556 ?
K1 Pr1 4.1275(8) 5_556 ?
S1 N2 1.635(3) . ?
S1 N1 1.637(3) . ?
S2 N3 1.624(3) . ?
S2 N4 1.625(3) . ?
O1 C3 1.254(4) . ?
O1 K1 2.696(2) 5_556 ?
O2 C3 1.262(4) . ?
O3 C4 1.271(4) . ?
O3 Pr1 2.428(2) 7_546 ?
O4 C4 1.218(4) . ?
O4 K1 2.745(3) 7_546 ?
O5 C7 1.245(4) . ?
O5 K1 3.411(3) 5_556 ?
O6 C7 1.253(4) . ?
O6 Pr1 2.479(2) 7_546 ?
O7 C8 1.259(4) . ?
O7 Pr1 2.465(2) 7_546 ?
O7 Pr1 2.726(2) 1_545 ?
O8 C8 1.251(4) . ?
O8 Pr1 2.598(2) 1_545 ?
O8 K1 2.880(2) 1_545 ?
O8 K1 2.944(2) 5_546 ?
O9 H9A 0.92(2) . ?
O9 H9B 0.92(2) . ?
N1 C1 1.329(4) . ?
N2 C2 1.319(4) . ?
N3 C5 1.329(4) . ?
N4 C6 1.328(4) . ?
N4 K1 2.985(3) 1_545 ?
C1 C2 1.419(4) . ?
C1 C3 1.499(4) . ?
C2 C4 1.520(4) . ?
C5 C6 1.429(4) . ?
C5 C7 1.509(4) . ?
C6 C8 1.516(4) . ?
C8 Pr1 3.017(3) 1_545 ?
O1W H1A 0.882(19) . ?
O1W H1B 0.891(19) . ?
O2W K1 3.2079(15) 2_556 ?
O2W H2 0.92(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Pr1 O7 85.51(8) 7_546 7_546 ?
O3 Pr1 O2 141.47(7) 7_546 . ?
O7 Pr1 O2 93.23(7) 7_546 . ?
O3 Pr1 O6 76.12(8) 7_546 7_546 ?
O7 Pr1 O6 69.35(7) 7_546 7_546 ?
O2 Pr1 O6 67.58(7) . 7_546 ?
O3 Pr1 O5 75.18(8) 7_546 . ?
O7 Pr1 O5 160.68(8) 7_546 . ?
O2 Pr1 O5 102.29(7) . . ?
O6 Pr1 O5 105.91(7) 7_546 . ?
O3 Pr1 O9 135.74(8) 7_546 . ?
O7 Pr1 O9 70.78(8) 7_546 . ?
O2 Pr1 O9 78.46(8) . . ?
O6 Pr1 O9 124.89(8) 7_546 . ?
O5 Pr1 O9 123.32(8) . . ?
O3 Pr1 O8 80.32(8) 7_546 1_565 ?
O7 Pr1 O8 110.62(7) 7_546 1_565 ?
O2 Pr1 O8 134.69(7) . 1_565 ?
O6 Pr1 O8 156.38(7) 7_546 1_565 ?
O5 Pr1 O8 65.85(7) . 1_565 ?
O9 Pr1 O8 74.35(8) . 1_565 ?
O3 Pr1 O1 145.59(8) 7_546 . ?
O7 Pr1 O1 128.85(7) 7_546 . ?
O2 Pr1 O1 51.31(7) . . ?
O6 Pr1 O1 114.38(7) 7_546 . ?
O5 Pr1 O1 70.43(7) . . ?
O9 Pr1 O1 67.10(8) . . ?
O8 Pr1 O1 84.60(7) 1_565 . ?
O3 Pr1 O7 68.35(7) 7_546 1_565 ?
O7 Pr1 O7 62.72(8) 7_546 1_565 ?
O2 Pr1 O7 143.09(7) . 1_565 ?
O6 Pr1 O7 121.17(7) 7_546 1_565 ?
O5 Pr1 O7 108.15(7) . 1_565 ?
O9 Pr1 O7 67.61(8) . 1_565 ?
O8 Pr1 O7 48.87(6) 1_565 1_565 ?
O1 Pr1 O7 121.62(7) . 1_565 ?
O3 Pr1 C3 150.98(8) 7_546 . ?
O7 Pr1 C3 113.77(8) 7_546 . ?
O2 Pr1 C3 25.76(8) . . ?
O6 Pr1 C3 90.18(8) 7_546 . ?
O5 Pr1 C3 84.48(8) . . ?
O9 Pr1 C3 72.96(8) . . ?
O8 Pr1 C3 110.15(8) 1_565 . ?
O1 Pr1 C3 25.72(8) . . ?
O7 Pr1 C3 139.08(7) 1_565 . ?
O3 Pr1 C8 71.32(8) 7_546 1_565 ?
O7 Pr1 C8 87.15(8) 7_546 1_565 ?
O2 Pr1 C8 147.17(8) . 1_565 ?
O6 Pr1 C8 141.05(8) 7_546 1_565 ?
O5 Pr1 C8 85.97(7) . 1_565 ?
O9 Pr1 C8 70.70(8) . 1_565 ?
O8 Pr1 C8 24.31(7) 1_565 1_565 ?
O1 Pr1 C8 104.56(7) . 1_565 ?
O7 Pr1 C8 24.67(7) 1_565 1_565 ?
C3 Pr1 C8 128.32(8) . 1_565 ?
O3 Pr1 K1 115.97(6) 7_546 5_556 ?
O7 Pr1 K1 136.43(5) 7_546 5_556 ?
O2 Pr1 K1 91.02(5) . 5_556 ?
O6 Pr1 K1 149.25(6) 7_546 5_556 ?
O5 Pr1 K1 55.62(6) . 5_556 ?
O9 Pr1 K1 67.71(6) . 5_556 ?
O8 Pr1 K1 45.18(5) 1_565 5_556 ?
O1 Pr1 K1 39.79(5) . 5_556 ?
O7 Pr1 K1 89.29(4) 1_565 5_556 ?
C3 Pr1 K1 65.51(6) . 5_556 ?
C8 Pr1 K1 67.32(6) 1_565 5_556 ?
O1 K1 O4 138.94(8) 5_556 7_546 ?
O1 K1 O5 151.11(8) 5_556 . ?
O4 K1 O5 69.65(8) 7_546 . ?
O1 K1 O8 114.96(7) 5_556 1_565 ?
O4 K1 O8 89.01(7) 7_546 1_565 ?
O5 K1 O8 58.62(6) . 1_565 ?
O1 K1 O8 77.06(7) 5_556 5_546 ?
O4 K1 O8 138.00(8) 7_546 5_546 ?
O5 K1 O8 75.14(7) . 5_546 ?
O8 K1 O8 91.77(6) 1_565 5_546 ?
O1 K1 N3 118.00(8) 5_556 . ?
O4 K1 N3 75.52(9) 7_546 . ?
O5 K1 N3 55.93(7) . . ?
O8 K1 N3 114.14(7) 1_565 . ?
O8 K1 N3 65.97(7) 5_546 . ?
O1 K1 N4 73.12(7) 5_556 1_565 ?
O4 K1 N4 97.25(9) 7_546 1_565 ?
O5 K1 N4 113.69(7) . 1_565 ?
O8 K1 N4 56.40(7) 1_565 1_565 ?
O8 K1 N4 117.76(7) 5_546 1_565 ?
N3 K1 N4 168.75(8) . 1_565 ?
O1 K1 O2W 72.76(6) 5_556 . ?
O4 K1 O2W 66.18(6) 7_546 . ?
O5 K1 O2W 135.54(7) . . ?
O8 K1 O2W 124.29(8) 1_565 . ?
O8 K1 O2W 140.20(6) 5_546 . ?
N3 K1 O2W 106.83(10) . . ?
N4 K1 O2W 77.30(10) 1_565 . ?
O1 K1 O1W 66.18(8) 5_556 . ?
O4 K1 O1W 88.81(8) 7_546 . ?
O5 K1 O1W 121.58(8) . . ?
O8 K1 O1W 177.52(7) 1_565 . ?
O8 K1 O1W 90.65(7) 5_546 . ?
N3 K1 O1W 66.42(8) . . ?
N4 K1 O1W 122.74(8) 1_565 . ?
O2W K1 O1W 53.60(9) . . ?
O1 K1 O5 56.56(6) 5_556 5_556 ?
O4 K1 O5 155.58(7) 7_546 5_556 ?
O5 K1 O5 98.89(6) . 5_556 ?
O8 K1 O5 66.86(6) 1_565 5_556 ?
O8 K1 O5 51.09(6) 5_546 5_556 ?
N3 K1 O5 116.78(7) . 5_556 ?
N4 K1 O5 66.87(7) 1_565 5_556 ?
O2W K1 O5 123.83(7) . 5_556 ?
O1W K1 O5 115.23(7) . 5_556 ?
O1 K1 K1 97.88(6) 5_556 5_556 ?
O4 K1 K1 121.83(6) 7_546 5_556 ?
O5 K1 K1 56.21(5) . 5_556 ?
O8 K1 K1 46.54(5) 1_565 5_556 ?
O8 K1 K1 45.23(5) 5_546 5_556 ?
N3 K1 K1 89.70(6) . 5_556 ?
N4 K1 K1 86.86(6) 1_565 5_556 ?
O2W K1 K1 163.33(9) . 5_556 ?
O1W K1 K1 135.88(6) . 5_556 ?
O5 K1 K1 42.68(4) 5_556 5_556 ?
O1 K1 Pr1 38.64(5) 5_556 5_556 ?
O4 K1 Pr1 167.00(7) 7_546 5_556 ?
O5 K1 Pr1 112.74(6) . 5_556 ?
O8 K1 Pr1 103.17(5) 1_565 5_556 ?
O8 K1 Pr1 38.75(4) 5_546 5_556 ?
N3 K1 Pr1 95.06(6) . 5_556 ?
N4 K1 Pr1 93.33(6) 1_565 5_556 ?
O2W K1 Pr1 109.19(2) . 5_556 ?
O1W K1 Pr1 79.10(6) . 5_556 ?
O5 K1 Pr1 37.24(4) 5_556 5_556 ?
K1 K1 Pr1 66.14(2) 5_556 5_556 ?
N2 S1 N1 98.76(14) . . ?
N3 S2 N4 98.72(14) . . ?
C3 O1 Pr1 88.74(18) . . ?
C3 O1 K1 169.7(2) . 5_556 ?
Pr1 O1 K1 101.57(7) . 5_556 ?
C3 O2 Pr1 95.70(18) . . ?
C4 O3 Pr1 143.9(2) . 7_546 ?
C4 O4 K1 128.6(2) . 7_546 ?
C7 O5 Pr1 110.53(19) . . ?
C7 O5 K1 129.09(19) . . ?
Pr1 O5 K1 115.30(8) . . ?
C7 O5 K1 122.77(19) . 5_556 ?
Pr1 O5 K1 87.14(6) . 5_556 ?
K1 O5 K1 81.11(6) . 5_556 ?
C7 O6 Pr1 138.6(2) . 7_546 ?
C8 O7 Pr1 150.8(2) . 7_546 ?
C8 O7 Pr1 90.72(17) . 1_545 ?
Pr1 O7 Pr1 117.28(8) 7_546 1_545 ?
C8 O8 Pr1 96.96(18) . 1_545 ?
C8 O8 K1 113.78(19) . 1_545 ?
Pr1 O8 K1 109.09(8) 1_545 1_545 ?
C8 O8 K1 148.8(2) . 5_546 ?
Pr1 O8 K1 96.07(7) 1_545 5_546 ?
K1 O8 K1 88.23(6) 1_545 5_546 ?
Pr1 O9 H9A 119(3) . . ?
Pr1 O9 H9B 128(3) . . ?
H9A O9 H9B 113(3) . . ?
C1 N1 S1 106.7(2) . . ?
C2 N2 S1 107.1(2) . . ?
C5 N3 S2 108.1(2) . . ?
C5 N3 K1 119.7(2) . . ?
S2 N3 K1 131.98(13) . . ?
C6 N4 S2 107.3(2) . . ?
C6 N4 K1 116.7(2) . 1_545 ?
S2 N4 K1 135.97(14) . 1_545 ?
N1 C1 C2 113.6(3) . . ?
N1 C1 C3 122.4(3) . . ?
C2 C1 C3 123.9(3) . . ?
N2 C2 C1 113.8(3) . . ?
N2 C2 C4 119.5(3) . . ?
C1 C2 C4 126.6(3) . . ?
O1 C3 O2 123.5(3) . . ?
O1 C3 C1 120.8(3) . . ?
O2 C3 C1 115.7(3) . . ?
O1 C3 Pr1 65.55(16) . . ?
O2 C3 Pr1 58.54(15) . . ?
C1 C3 Pr1 168.5(2) . . ?
O4 C4 O3 127.4(3) . . ?
O4 C4 C2 118.9(3) . . ?
O3 C4 C2 113.6(3) . . ?
N3 C5 C6 112.2(3) . . ?
N3 C5 C7 117.6(3) . . ?
C6 C5 C7 130.1(3) . . ?
N4 C6 C5 113.7(3) . . ?
N4 C6 C8 115.7(3) . . ?
C5 C6 C8 130.6(3) . . ?
O5 C7 O6 123.6(3) . . ?
O5 C7 C5 116.5(3) . . ?
O6 C7 C5 119.9(3) . . ?
O8 C8 O7 122.9(3) . . ?
O8 C8 C6 117.8(3) . . ?
O7 C8 C6 119.1(3) . . ?
O8 C8 Pr1 58.74(15) . 1_545 ?
O7 C8 Pr1 64.61(16) . 1_545 ?
C6 C8 Pr1 168.7(2) . 1_545 ?
K1 O1W H1A 107.7(14) . . ?
K1 O1W H1B 105.5(13) . . ?
H1A O1W H1B 111(3) . . ?
K1 O2W K1 149.77(17) 2_556 . ?
K1 O2W H2 104(3) 2_556 . ?
K1 O2W H2 95(3) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O9 H9A O3 0.92(2) 1.92(2) 2.832(3) 170(4) 1_565
O9 H9B O1W 0.92(2) 1.90(2) 2.815(4) 169(5) 5_556
O1W H1A O4 0.882(19) 2.02(2) 2.802(4) 147(3) 8_446
O2W H2 N1 0.92(2) 2.08(2) 2.995(4) 173(5) 5_556

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.07
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.596
_refine_diff_density_min         -0.377
_refine_diff_density_rms         0.076
_database_code_depnum_ccdc_archive 'CCDC 957581'
#######################################################################
#
#                 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_compound4

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C8 H5 K N4 Nd O10.50 S2'
_chemical_formula_sum            'C8 H5 K N4 Nd O10.50 S2'
_chemical_formula_weight         572.62

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   c2/c

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

_cell_length_a                   18.077(4)
_cell_length_b                   8.3675(17)
_cell_length_c                   20.380(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.14(3)
_cell_angle_gamma                90.00
_cell_volume                     3082.1(11)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    2.468
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2208
_exptl_absorpt_coefficient_mu    3.979
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.4141
_exptl_absorpt_correction_T_max  0.4516
_exptl_absorpt_process_details   Process-auto

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       omega-scan
_diffrn_detector_area_resol_mean 10.0
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            14640
_diffrn_reflns_av_R_equivalents  0.0400
_diffrn_reflns_av_sigmaI/netI    0.0344
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         3.36
_diffrn_reflns_theta_max         27.47
_reflns_number_total             3484
_reflns_number_gt                2948
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       Process-auto
_computing_cell_refinement       Process-auto
_computing_data_reduction        Process-auto
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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. Standard DFIX restraints were
used for the distance of the atoms, such as (o9 and h9a), (o9 and h9b),
(o2w and h2), (h9a and h9b), (o1w and h1a), (o1w and h1b), (h1a and h1b).To
 improve the parameters chemical more reasonable, ultimately restrain
 instructions OMIT were applied in the refinement.
;

_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)+(0.0000P)²+7.7402P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3484
_refine_ls_number_parameters     255
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0309
_refine_ls_R_factor_gt           0.0227
_refine_ls_wR_factor_ref         0.0464
_refine_ls_wR_factor_gt          0.0437
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.043
_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
Nd1 Nd 0.207443(8) 0.008762(17) 0.479673(7) 0.01389(5) Uani 1 1 d . . .
K1 K 0.00508(4) -0.00572(8) 0.59909(4) 0.03020(16) Uani 1 1 d . . .
S1 S 0.15383(5) -0.44626(11) 0.21171(4) 0.0374(2) Uani 1 1 d . . .
S2 S -0.02515(5) -0.49768(9) 0.62688(4) 0.02969(18) Uani 1 1 d . . .
O1 O 0.13123(11) -0.1108(2) 0.38100(10) 0.0238(5) Uani 1 1 d . . .
O2 O 0.25214(11) -0.1525(2) 0.38743(10) 0.0227(5) Uani 1 1 d . . .
O3 O 0.28239(12) -0.5276(2) 0.40225(10) 0.0258(5) Uani 1 1 d . . .
O4 O 0.36562(13) -0.4372(4) 0.33182(11) 0.0427(7) Uani 1 1 d . . .
O5 O 0.10752(12) -0.1636(2) 0.52132(11) 0.0254(5) Uani 1 1 d . . .
O6 O 0.17828(11) -0.3643(3) 0.49114(10) 0.0254(5) Uani 1 1 d . . .
O7 O 0.18593(11) -0.6898(2) 0.52137(10) 0.0209(4) Uani 1 1 d . . .
O8 O 0.08700(11) -0.8371(2) 0.50239(10) 0.0213(4) Uani 1 1 d . . .
O9 O 0.19207(15) 0.1994(3) 0.38681(11) 0.0334(6) Uani 1 1 d D . .
N1 N 0.13369(15) -0.3028(3) 0.26251(13) 0.0259(6) Uani 1 1 d . . .
N2 N 0.22778(16) -0.5148(3) 0.24951(13) 0.0332(7) Uani 1 1 d . . .
N3 N 0.02261(14) -0.3541(3) 0.59503(12) 0.0223(6) Uani 1 1 d . . .
N4 N 0.01607(14) -0.6483(3) 0.59335(13) 0.0247(6) Uani 1 1 d . . .
C1 C 0.18506(16) -0.3024(3) 0.30942(14) 0.0192(6) Uani 1 1 d . . .
C2 C 0.23931(17) -0.4245(3) 0.30219(14) 0.0194(6) Uani 1 1 d . . .
C3 C 0.18891(17) -0.1792(3) 0.36223(14) 0.0192(6) Uani 1 1 d . . .
C4 C 0.30227(16) -0.4643(3) 0.34867(14) 0.0199(6) Uani 1 1 d . . .
C5 C 0.07373(15) -0.4194(3) 0.55745(13) 0.0156(6) Uani 1 1 d . . .
C6 C 0.06947(15) -0.5906(3) 0.55690(14) 0.0165(6) Uani 1 1 d . . .
C7 C 0.12398(16) -0.3081(3) 0.52060(14) 0.0176(6) Uani 1 1 d . . .
C8 C 0.11723(15) -0.7120(3) 0.52324(14) 0.0155(6) Uani 1 1 d . . .
O1W O -0.08548(17) -0.1975(4) 0.71587(14) 0.0525(8) Uani 1 1 d D . .
O2W O 0.0000 0.0923(5) 0.7500 0.0744(16) Uani 1 2 d SD . .
H9A H 0.217(2) 0.298(4) 0.387(2) 0.080 Uiso 1 1 d D . .
H9B H 0.159(2) 0.192(5) 0.3511(17) 0.080 Uiso 1 1 d D . .
H1A H -0.0358(11) -0.202(6) 0.709(2) 0.080 Uiso 1 1 d D . .
H1B H -0.113(2) -0.171(6) 0.7522(16) 0.080 Uiso 1 1 d D . .
H2 H -0.0394(19) 0.161(5) 0.753(3) 0.080 Uiso 1 1 d 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
Nd1 O3 2.415(2) 7_546 ?
Nd1 O7 2.452(2) 7_546 ?
Nd1 O6 2.456(2) 7_546 ?
Nd1 O2 2.463(2) . ?
Nd1 O5 2.475(2) . ?
Nd1 O9 2.487(2) . ?
Nd1 O8 2.580(2) 1_565 ?
Nd1 O1 2.614(2) . ?
Nd1 O7 2.692(2) 1_565 ?
Nd1 C3 2.878(3) . ?
Nd1 C8 2.994(3) 1_565 ?
Nd1 K1 4.1341(13) 5_556 ?
K1 O1 2.688(2) 5_556 ?
K1 O4 2.747(3) 7_546 ?
K1 O5 2.793(2) . ?
K1 O8 2.861(2) 1_565 ?
K1 N3 2.934(3) . ?
K1 O8 2.940(2) 5_546 ?
K1 N4 3.000(3) 1_565 ?
K1 O2W 3.1862(15) . ?
K1 O1W 3.328(3) . ?
K1 K1 4.0405(18) 5_556 ?
K1 Nd1 4.1341(13) 5_556 ?
K1 H1A 2.88(5) . ?
S1 N1 1.631(3) . ?
S1 N2 1.633(3) . ?
S2 N4 1.622(3) . ?
S2 N3 1.622(3) . ?
O1 C3 1.256(3) . ?
O1 K1 2.688(2) 5_556 ?
O2 C3 1.264(4) . ?
O3 C4 1.272(4) . ?
O3 Nd1 2.415(2) 7_546 ?
O4 C4 1.223(4) . ?
O4 K1 2.747(3) 7_546 ?
O5 C7 1.245(3) . ?
O6 C7 1.253(4) . ?
O6 Nd1 2.456(2) 7_546 ?
O7 C8 1.257(3) . ?
O7 Nd1 2.452(2) 7_546 ?
O7 Nd1 2.692(2) 1_545 ?
O8 C8 1.252(3) . ?
O8 Nd1 2.580(2) 1_545 ?
O8 K1 2.861(2) 1_545 ?
O8 K1 2.940(2) 5_546 ?
O9 H9A 0.938(18) . ?
O9 H9B 0.938(18) . ?
N1 C1 1.319(4) . ?
N2 C2 1.326(4) . ?
N3 C5 1.329(4) . ?
N4 C6 1.321(4) . ?
N4 K1 3.000(3) 1_545 ?
C1 C2 1.426(4) . ?
C1 C3 1.491(4) . ?
C2 C4 1.504(4) . ?
C5 C6 1.434(4) . ?
C5 C7 1.511(4) . ?
C6 C8 1.507(4) . ?
C8 Nd1 2.994(3) 1_545 ?
O1W H1A 0.914(17) . ?
O1W H1B 0.930(18) . ?
O2W K1 3.1862(15) 2_556 ?
O2W H2 0.920(19) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Nd1 O7 85.64(8) 7_546 7_546 ?
O3 Nd1 O6 75.16(8) 7_546 7_546 ?
O7 Nd1 O6 69.44(7) 7_546 7_546 ?
O3 Nd1 O2 140.95(7) 7_546 . ?
O7 Nd1 O2 93.55(7) 7_546 . ?
O6 Nd1 O2 68.17(7) 7_546 . ?
O3 Nd1 O5 74.80(8) 7_546 . ?
O7 Nd1 O5 160.44(7) 7_546 . ?
O6 Nd1 O5 104.26(7) 7_546 . ?
O2 Nd1 O5 101.26(7) . . ?
O3 Nd1 O9 136.19(7) 7_546 . ?
O7 Nd1 O9 70.91(8) 7_546 . ?
O6 Nd1 O9 125.51(8) 7_546 . ?
O2 Nd1 O9 78.70(8) . . ?
O5 Nd1 O9 124.31(8) . . ?
O3 Nd1 O8 80.57(7) 7_546 1_565 ?
O7 Nd1 O8 111.03(6) 7_546 1_565 ?
O6 Nd1 O8 155.65(7) 7_546 1_565 ?
O2 Nd1 O8 134.55(7) . 1_565 ?
O5 Nd1 O8 66.76(7) . 1_565 ?
O9 Nd1 O8 74.57(8) . 1_565 ?
O3 Nd1 O1 145.10(7) 7_546 . ?
O7 Nd1 O1 129.21(7) 7_546 . ?
O6 Nd1 O1 115.20(7) 7_546 . ?
O2 Nd1 O1 51.62(7) . . ?
O5 Nd1 O1 70.35(7) . . ?
O9 Nd1 O1 67.10(7) . . ?
O8 Nd1 O1 84.01(7) 1_565 . ?
O3 Nd1 O7 68.46(7) 7_546 1_565 ?
O7 Nd1 O7 62.77(8) 7_546 1_565 ?
O6 Nd1 O7 120.71(7) 7_546 1_565 ?
O2 Nd1 O7 143.68(7) . 1_565 ?
O5 Nd1 O7 109.06(7) . 1_565 ?
O9 Nd1 O7 67.95(7) . 1_565 ?
O8 Nd1 O7 49.26(6) 1_565 1_565 ?
O1 Nd1 O7 121.61(6) . 1_565 ?
O3 Nd1 C3 150.43(7) 7_546 . ?
O7 Nd1 C3 114.14(8) 7_546 . ?
O6 Nd1 C3 90.91(8) 7_546 . ?
O2 Nd1 C3 25.91(8) . . ?
O5 Nd1 C3 83.87(8) . . ?
O9 Nd1 C3 73.04(8) . . ?
O8 Nd1 C3 109.74(8) 1_565 . ?
O1 Nd1 C3 25.87(7) . . ?
O7 Nd1 C3 139.41(7) 1_565 . ?
O3 Nd1 C8 71.61(7) 7_546 1_565 ?
O7 Nd1 C8 87.32(7) 7_546 1_565 ?
O6 Nd1 C8 140.59(7) 7_546 1_565 ?
O2 Nd1 C8 147.42(7) . 1_565 ?
O5 Nd1 C8 86.99(7) . 1_565 ?
O9 Nd1 C8 70.83(8) . 1_565 ?
O8 Nd1 C8 24.53(7) 1_565 1_565 ?
O1 Nd1 C8 104.18(7) . 1_565 ?
O7 Nd1 C8 24.81(6) 1_565 1_565 ?
C3 Nd1 C8 128.17(8) . 1_565 ?
O3 Nd1 K1 116.04(6) 7_546 5_556 ?
O7 Nd1 K1 136.47(5) 7_546 5_556 ?
O6 Nd1 K1 149.49(5) 7_546 5_556 ?
O2 Nd1 K1 90.96(5) . 5_556 ?
O5 Nd1 K1 56.67(5) . 5_556 ?
O9 Nd1 K1 67.64(6) . 5_556 ?
O8 Nd1 K1 44.92(5) 1_565 5_556 ?
O1 Nd1 K1 39.42(5) . 5_556 ?
O7 Nd1 K1 89.39(4) 1_565 5_556 ?
C3 Nd1 K1 65.28(7) . 5_556 ?
C8 Nd1 K1 67.21(5) 1_565 5_556 ?
O1 K1 O4 139.38(7) 5_556 7_546 ?
O1 K1 O5 151.30(7) 5_556 . ?
O4 K1 O5 68.99(7) 7_546 . ?
O1 K1 O8 114.44(7) 5_556 1_565 ?
O4 K1 O8 89.54(7) 7_546 1_565 ?
O5 K1 O8 58.95(6) . 1_565 ?
O1 K1 N3 117.67(7) 5_556 . ?
O4 K1 N3 75.54(8) 7_546 . ?
O5 K1 N3 56.01(6) . . ?
O8 K1 N3 114.39(7) 1_565 . ?
O1 K1 O8 76.14(6) 5_556 5_546 ?
O4 K1 O8 138.34(8) 7_546 5_546 ?
O5 K1 O8 76.22(7) . 5_546 ?
O8 K1 O8 91.70(6) 1_565 5_546 ?
N3 K1 O8 66.14(7) . 5_546 ?
O1 K1 N4 72.90(7) 5_556 1_565 ?
O4 K1 N4 97.88(8) 7_546 1_565 ?
O5 K1 N4 113.84(7) . 1_565 ?
O8 K1 N4 56.35(6) 1_565 1_565 ?
N3 K1 N4 169.21(7) . 1_565 ?
O8 K1 N4 117.11(7) 5_546 1_565 ?
O1 K1 O2W 73.55(6) 5_556 . ?
O4 K1 O2W 65.83(6) 7_546 . ?
O5 K1 O2W 134.55(6) . . ?
O8 K1 O2W 124.29(8) 1_565 . ?
N3 K1 O2W 106.75(10) . . ?
O8 K1 O2W 140.13(6) 5_546 . ?
N4 K1 O2W 77.54(10) 1_565 . ?
O1 K1 O1W 66.51(8) 5_556 . ?
O4 K1 O1W 88.58(8) 7_546 . ?
O5 K1 O1W 121.26(8) . . ?
O8 K1 O1W 177.82(7) 1_565 . ?
N3 K1 O1W 66.17(8) . . ?
O8 K1 O1W 90.44(7) 5_546 . ?
N4 K1 O1W 122.85(8) 1_565 . ?
O2W K1 O1W 53.82(8) . . ?
O1 K1 K1 96.82(6) 5_556 5_556 ?
O4 K1 K1 122.54(6) 7_546 5_556 ?
O5 K1 K1 57.42(5) . 5_556 ?
O8 K1 K1 46.65(4) 1_565 5_556 ?
N3 K1 K1 89.89(5) . 5_556 ?
O8 K1 K1 45.05(5) 5_546 5_556 ?
N4 K1 K1 86.51(6) 1_565 5_556 ?
O2W K1 K1 163.18(8) . 5_556 ?
O1W K1 K1 135.49(6) . 5_556 ?
O1 K1 Nd1 38.13(4) 5_556 5_556 ?
O4 K1 Nd1 166.60(6) 7_546 5_556 ?
O5 K1 Nd1 113.47(5) . 5_556 ?
O8 K1 Nd1 103.03(5) 1_565 5_556 ?
N3 K1 Nd1 94.76(5) . 5_556 ?
O8 K1 Nd1 38.30(4) 5_546 5_556 ?
N4 K1 Nd1 93.02(5) 1_565 5_556 ?
O2W K1 Nd1 109.39(3) . 5_556 ?
O1W K1 Nd1 78.94(6) . 5_556 ?
K1 K1 Nd1 65.71(3) 5_556 5_556 ?
O1 K1 Nd1 147.29(5) 5_556 . ?
O4 K1 Nd1 65.37(5) 7_546 . ?
O5 K1 Nd1 30.49(4) . . ?
O8 K1 Nd1 33.34(4) 1_565 . ?
N3 K1 Nd1 85.47(5) . . ?
O8 K1 Nd1 95.04(5) 5_546 . ?
N4 K1 Nd1 84.00(5) 1_565 . ?
O2W K1 Nd1 124.23(3) . . ?
O1W K1 Nd1 145.94(6) . . ?
K1 K1 Nd1 58.16(3) 5_556 . ?
Nd1 K1 Nd1 123.87(2) 5_556 . ?
O1 K1 H1A 80.8(6) 5_556 . ?
O4 K1 H1A 74.5(6) 7_546 . ?
O5 K1 H1A 110.7(7) . . ?
O8 K1 H1A 163.7(5) 1_565 . ?
N3 K1 H1A 59.0(9) . . ?
O8 K1 H1A 98.0(8) 5_546 . ?
N4 K1 H1A 128.1(9) 1_565 . ?
O2W K1 H1A 52.1(9) . . ?
O1W K1 H1A 14.8(5) . . ?
K1 K1 H1A 141.4(9) 5_556 . ?
Nd1 K1 H1A 92.7(6) 5_556 . ?
Nd1 K1 H1A 131.9(6) . . ?
N1 S1 N2 98.61(14) . . ?
N4 S2 N3 98.87(13) . . ?
C3 O1 Nd1 88.90(17) . . ?
C3 O1 K1 168.63(19) . 5_556 ?
Nd1 O1 K1 102.46(7) . 5_556 ?
C3 O2 Nd1 95.69(17) . . ?
C4 O3 Nd1 144.19(19) . 7_546 ?
C4 O4 K1 128.0(2) . 7_546 ?
C7 O5 Nd1 112.68(19) . . ?
C7 O5 K1 128.83(19) . . ?
Nd1 O5 K1 114.57(8) . . ?
C7 O6 Nd1 137.06(18) . 7_546 ?
C8 O7 Nd1 150.29(18) . 7_546 ?
C8 O7 Nd1 91.18(16) . 1_545 ?
Nd1 O7 Nd1 117.23(8) 7_546 1_545 ?
C8 O8 Nd1 96.60(17) . 1_545 ?
C8 O8 K1 114.03(18) . 1_545 ?
Nd1 O8 K1 109.11(7) 1_545 1_545 ?
C8 O8 K1 148.26(18) . 5_546 ?
Nd1 O8 K1 96.78(7) 1_545 5_546 ?
K1 O8 K1 88.30(6) 1_545 5_546 ?
Nd1 O9 H9A 121(3) . . ?
Nd1 O9 H9B 128(3) . . ?
H9A O9 H9B 111(3) . . ?
C1 N1 S1 107.4(2) . . ?
C2 N2 S1 107.2(2) . . ?
C5 N3 S2 107.9(2) . . ?
C5 N3 K1 120.08(18) . . ?
S2 N3 K1 131.75(13) . . ?
C6 N4 S2 107.4(2) . . ?
C6 N4 K1 115.85(18) . 1_545 ?
S2 N4 K1 136.63(13) . 1_545 ?
N1 C1 C2 113.5(3) . . ?
N1 C1 C3 123.2(3) . . ?
C2 C1 C3 123.2(3) . . ?
N2 C2 C1 113.2(3) . . ?
N2 C2 C4 119.3(3) . . ?
C1 C2 C4 127.4(3) . . ?
O1 C3 O2 123.0(3) . . ?
O1 C3 C1 120.5(3) . . ?
O2 C3 C1 116.4(3) . . ?
O1 C3 Nd1 65.24(15) . . ?
O2 C3 Nd1 58.40(14) . . ?
C1 C3 Nd1 168.9(2) . . ?
O4 C4 O3 126.9(3) . . ?
O4 C4 C2 118.9(3) . . ?
O3 C4 C2 114.2(3) . . ?
N3 C5 C6 112.1(3) . . ?
N3 C5 C7 117.7(2) . . ?
C6 C5 C7 130.1(3) . . ?
N4 C6 C5 113.6(3) . . ?
N4 C6 C8 116.2(2) . . ?
C5 C6 C8 130.2(3) . . ?
O5 C7 O6 124.1(3) . . ?
O5 C7 C5 116.5(3) . . ?
O6 C7 C5 119.4(3) . . ?
O8 C8 O7 122.5(3) . . ?
O8 C8 C6 117.9(2) . . ?
O7 C8 C6 119.3(2) . . ?
O8 C8 Nd1 58.87(14) . 1_545 ?
O7 C8 Nd1 64.00(15) . 1_545 ?
C6 C8 Nd1 168.89(19) . 1_545 ?
K1 O1W H1A 54(3) . . ?
K1 O1W H1B 137(3) . . ?
H1A O1W H1B 133(3) . . ?
K1 O2W K1 150.17(16) . 2_556 ?
K1 O2W H2 106(3) . . ?
K1 O2W H2 93(3) 2_556 . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O9 H9A O3 0.938(18) 1.901(19) 2.821(3) 166(4) 1_565
O9 H9B O1W 0.938(18) 1.88(2) 2.816(4) 173(5) 5_556
O1W H1A O1W 0.914(17) 2.65(3) 3.364(6) 135(3) 2_556
O1W H1B O4 0.930(18) 1.90(3) 2.778(4) 156(4) 8_446
O2W H2 N1 0.920(19) 2.10(2) 2.998(4) 166(5) 5_556

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        27.47
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         0.376
_refine_diff_density_min         -0.676
_refine_diff_density_rms         0.101
_database_code_depnum_ccdc_archive 'CCDC 957582'
#######################################################################
#
#                 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_compound5

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C8 H5 K N4 O10.50 S2 Sm'
_chemical_formula_sum            'C8 H5 K N4 O10.50 S2 Sm'
_chemical_formula_weight         578.73

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'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   c2/c

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

_cell_length_a                   18.0310(18)
_cell_length_b                   8.3836(8)
_cell_length_c                   20.254(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.9380(10)
_cell_angle_gamma                90.00
_cell_volume                     3061.3(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2725
_cell_measurement_theta_min      2.01
_cell_measurement_theta_max      25.15

_exptl_crystal_description       block
_exptl_crystal_colour            COLORLESS
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.19
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    2.511
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2224
_exptl_absorpt_coefficient_mu    4.450
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.3357
_exptl_absorpt_correction_T_max  0.4314
_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 9.00cm
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            7532
_diffrn_reflns_av_R_equivalents  0.0178
_diffrn_reflns_av_sigmaI/netI    0.0196
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.01
_diffrn_reflns_theta_max         25.15
_reflns_number_total             2725
_reflns_number_gt                2561
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXP-97
_computing_publication_material  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. Standard DFIX restraints were
used for the distance of the atoms, such as (o9 and h9a), (o9 and h9b),
(o2w and h2), (h9a and h9b), (o1w and h1a), (o1w and h1b), (h1a and h1b).
;

_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)+(0.0015P)²+42.9582P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    none
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2725
_refine_ls_number_parameters     255
_refine_ls_number_restraints     11
_refine_ls_R_factor_all          0.0299
_refine_ls_R_factor_gt           0.0280
_refine_ls_wR_factor_ref         0.0652
_refine_ls_wR_factor_gt          0.0645
_refine_ls_goodness_of_fit_ref   1.258
_refine_ls_restrained_S_all      1.344
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Sm1 Sm 0.207743(15) 0.01247(3) 0.479983(13) 0.01468(10) Uani 1 1 d . . .
K1 K 0.00562(7) -0.00756(17) 0.59919(8) 0.0304(3) Uani 1 1 d D . .
S1 S 0.15280(10) -0.4431(2) 0.21253(8) 0.0376(4) Uani 1 1 d . . .
S2 S -0.02607(9) -0.4955(2) 0.62637(8) 0.0297(4) Uani 1 1 d . . .
O1 O 0.1317(2) -0.1068(5) 0.3822(2) 0.0248(9) Uani 1 1 d . . .
O2 O 0.2523(2) -0.1486(5) 0.3887(2) 0.0226(9) Uani 1 1 d . . .
O3 O 0.2831(2) -0.5292(5) 0.40248(19) 0.0257(9) Uani 1 1 d . . .
O4 O 0.3657(2) -0.4341(7) 0.3320(2) 0.0440(14) Uani 1 1 d . . .
O5 O 0.1123(2) -0.1664(5) 0.5215(2) 0.0240(9) Uani 1 1 d . . .
O6 O 0.1792(2) -0.3722(5) 0.4898(2) 0.0240(9) Uani 1 1 d . . .
O7 O 0.1870(2) -0.6919(5) 0.5221(2) 0.0200(9) Uani 1 1 d . . .
O8 O 0.0870(2) -0.8395(4) 0.5032(2) 0.0200(9) Uani 1 1 d . . .
O9 O 0.1930(3) 0.1992(5) 0.3873(2) 0.0340(11) Uani 1 1 d D . .
N1 N 0.1331(3) -0.2984(6) 0.2634(3) 0.0262(12) Uani 1 1 d . . .
N2 N 0.2270(3) -0.5124(7) 0.2503(3) 0.0345(14) Uani 1 1 d . . .
N3 N 0.0231(3) -0.3541(6) 0.5947(3) 0.0230(11) Uani 1 1 d . . .
N4 N 0.0149(3) -0.6474(6) 0.5930(3) 0.0242(11) Uani 1 1 d . . .
C1 C 0.1859(3) -0.2988(7) 0.3103(3) 0.0184(12) Uani 1 1 d . . .
C2 C 0.2391(3) -0.4227(7) 0.3026(3) 0.0207(12) Uani 1 1 d . . .
C3 C 0.1890(3) -0.1746(7) 0.3637(3) 0.0192(12) Uani 1 1 d . . .
C4 C 0.3027(3) -0.4633(7) 0.3492(3) 0.0206(12) Uani 1 1 d . . .
C5 C 0.0745(3) -0.4199(7) 0.5571(3) 0.0161(11) Uani 1 1 d . . .
C6 C 0.0693(3) -0.5903(6) 0.5564(3) 0.0161(11) Uani 1 1 d . . .
C7 C 0.1269(3) -0.3118(7) 0.5200(3) 0.0189(12) Uani 1 1 d . . .
C8 C 0.1175(3) -0.7131(6) 0.5238(3) 0.0163(12) Uani 1 1 d . . .
O1W O -0.0852(3) -0.1988(7) 0.7147(3) 0.0514(15) Uani 1 1 d D . .
O2W O 0.0000 0.0903(11) 0.7500 0.072(3) Uani 1 2 d SD . .
H9A H 0.215(5) 0.302(5) 0.391(4) 0.080 Uiso 1 1 d D . .
H9B H 0.162(4) 0.195(9) 0.350(3) 0.080 Uiso 1 1 d D . .
H1A H -0.105(4) -0.128(3) 0.743(2) 0.080 Uiso 1 1 d D . .
H1B H -0.054(2) -0.266(7) 0.736(3) 0.080 Uiso 1 1 d D . .
H2 H -0.040(4) 0.158(9) 0.741(5) 0.080 Uiso 1 1 d D . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sm1 O3 2.388(4) 7_546 ?
Sm1 O6 2.423(4) 7_546 ?
Sm1 O7 2.423(4) 7_546 ?
Sm1 O2 2.437(4) . ?
Sm1 O5 2.442(4) . ?
Sm1 O9 2.455(4) . ?
Sm1 O8 2.556(4) 1_565 ?
Sm1 O1 2.592(4) . ?
Sm1 O7 2.650(4) 1_565 ?
Sm1 C3 2.845(6) . ?
Sm1 C8 2.963(6) 1_565 ?
Sm1 K1 4.1438(14) 5_556 ?
K1 O1 2.687(4) 5_556 ?
K1 O4 2.731(5) 7_546 ?
K1 O8 2.831(4) 1_565 ?
K1 O5 2.838(4) . ?
K1 N3 2.924(5) . ?
K1 O8 2.936(4) 5_546 ?
K1 N4 3.027(5) 1_565 ?
K1 O2W 3.166(3) . ?
K1 O1W 3.294(6) . ?
K1 K1 4.022(3) 5_556 ?
K1 Sm1 4.1438(14) 5_556 ?
S1 N1 1.634(5) . ?
S1 N2 1.636(5) . ?
S2 N3 1.619(5) . ?
S2 N4 1.625(5) . ?
O1 C3 1.242(7) . ?
O1 K1 2.687(4) 5_556 ?
O2 C3 1.261(7) . ?
O3 C4 1.268(7) . ?
O3 Sm1 2.388(4) 7_546 ?
O4 C4 1.219(7) . ?
O4 K1 2.731(5) 7_546 ?
O5 C7 1.247(7) . ?
O6 C7 1.240(7) . ?
O6 Sm1 2.423(4) 7_546 ?
O7 C8 1.267(7) . ?
O7 Sm1 2.423(4) 7_546 ?
O7 Sm1 2.650(4) 1_545 ?
O8 C8 1.261(7) . ?
O8 Sm1 2.556(4) 1_545 ?
O8 K1 2.831(4) 1_545 ?
O8 K1 2.936(4) 5_546 ?
O9 H9A 0.95(2) . ?
O9 H9B 0.94(2) . ?
N1 C1 1.333(7) . ?
N2 C2 1.315(8) . ?
N3 C5 1.328(7) . ?
N4 C6 1.328(7) . ?
N4 K1 3.027(5) 1_545 ?
C1 C2 1.425(8) . ?
C1 C3 1.503(8) . ?
C2 C4 1.511(8) . ?
C5 C6 1.431(8) . ?
C5 C7 1.518(8) . ?
C6 C8 1.506(8) . ?
C8 Sm1 2.963(6) 1_545 ?
O1W H1A 0.90(2) . ?
O1W H1B 0.90(2) . ?
O2W K1 3.166(3) 2_556 ?
O2W H2 0.94(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Sm1 O6 74.48(14) 7_546 7_546 ?
O3 Sm1 O7 86.51(14) 7_546 7_546 ?
O6 Sm1 O7 69.49(14) 7_546 7_546 ?
O3 Sm1 O2 140.42(14) 7_546 . ?
O6 Sm1 O2 68.65(14) 7_546 . ?
O7 Sm1 O2 93.58(13) 7_546 . ?
O3 Sm1 O5 74.39(14) 7_546 . ?
O6 Sm1 O5 102.10(14) 7_546 . ?
O7 Sm1 O5 160.71(14) 7_546 . ?
O2 Sm1 O5 99.44(14) . . ?
O3 Sm1 O9 136.85(15) 7_546 . ?
O6 Sm1 O9 125.62(16) 7_546 . ?
O7 Sm1 O9 70.48(15) 7_546 . ?
O2 Sm1 O9 78.81(15) . . ?
O5 Sm1 O9 125.92(15) . . ?
O3 Sm1 O8 80.43(14) 7_546 1_565 ?
O6 Sm1 O8 154.79(13) 7_546 1_565 ?
O7 Sm1 O8 111.80(12) 7_546 1_565 ?
O2 Sm1 O8 134.52(13) . 1_565 ?
O5 Sm1 O8 68.17(13) . 1_565 ?
O9 Sm1 O8 75.46(16) . 1_565 ?
O3 Sm1 O1 144.29(14) 7_546 . ?
O6 Sm1 O1 115.99(14) 7_546 . ?
O7 Sm1 O1 129.16(13) 7_546 . ?
O2 Sm1 O1 51.93(13) . . ?
O5 Sm1 O1 70.06(14) . . ?
O9 Sm1 O1 67.20(14) . . ?
O8 Sm1 O1 83.46(12) 1_565 . ?
O3 Sm1 O7 68.42(14) 7_546 1_565 ?
O6 Sm1 O7 119.71(13) 7_546 1_565 ?
O7 Sm1 O7 62.59(14) 7_546 1_565 ?
O2 Sm1 O7 144.34(13) . 1_565 ?
O5 Sm1 O7 111.08(13) . 1_565 ?
O9 Sm1 O7 68.61(14) . 1_565 ?
O8 Sm1 O7 50.30(11) 1_565 1_565 ?
O1 Sm1 O7 122.07(12) . 1_565 ?
O3 Sm1 C3 149.66(15) 7_546 . ?
O6 Sm1 C3 91.70(15) 7_546 . ?
O7 Sm1 C3 114.25(15) 7_546 . ?
O2 Sm1 C3 26.19(15) . . ?
O5 Sm1 C3 82.60(15) . . ?
O9 Sm1 C3 73.07(16) . . ?
O8 Sm1 C3 109.25(15) 1_565 . ?
O1 Sm1 C3 25.88(14) . . ?
O7 Sm1 C3 140.03(14) 1_565 . ?
O3 Sm1 C8 71.64(15) 7_546 1_565 ?
O6 Sm1 C8 139.93(15) 7_546 1_565 ?
O7 Sm1 C8 87.57(14) 7_546 1_565 ?
O2 Sm1 C8 147.93(14) . 1_565 ?
O5 Sm1 C8 88.86(14) . 1_565 ?
O9 Sm1 C8 71.40(16) . 1_565 ?
O8 Sm1 C8 25.05(14) 1_565 1_565 ?
O1 Sm1 C8 104.01(14) . 1_565 ?
O7 Sm1 C8 25.31(13) 1_565 1_565 ?
C3 Sm1 C8 128.14(16) . 1_565 ?
O3 Sm1 K1 115.80(10) 7_546 5_556 ?
O6 Sm1 K1 149.85(11) 7_546 5_556 ?
O7 Sm1 K1 136.24(9) 7_546 5_556 ?
O2 Sm1 K1 90.95(9) . 5_556 ?
O5 Sm1 K1 58.14(10) . 5_556 ?
O9 Sm1 K1 67.82(12) . 5_556 ?
O8 Sm1 K1 44.60(9) 1_565 5_556 ?
O1 Sm1 K1 39.10(9) . 5_556 ?
O7 Sm1 K1 89.92(8) 1_565 5_556 ?
C3 Sm1 K1 64.98(12) . 5_556 ?
C8 Sm1 K1 67.20(11) 1_565 5_556 ?
O1 K1 O4 140.28(15) 5_556 7_546 ?
O1 K1 O8 114.09(13) 5_556 1_565 ?
O4 K1 O8 89.65(13) 7_546 1_565 ?
O1 K1 O5 151.63(14) 5_556 . ?
O4 K1 O5 67.73(14) 7_546 . ?
O8 K1 O5 59.25(11) 1_565 . ?
O1 K1 N3 117.31(14) 5_556 . ?
O4 K1 N3 75.34(17) 7_546 . ?
O8 K1 N3 114.57(13) 1_565 . ?
O5 K1 N3 56.08(13) . . ?
O1 K1 O8 74.94(12) 5_556 5_546 ?
O4 K1 O8 138.67(15) 7_546 5_546 ?
O8 K1 O8 91.59(11) 1_565 5_546 ?
O5 K1 O8 77.66(12) . 5_546 ?
N3 K1 O8 66.69(13) . 5_546 ?
O1 K1 N4 72.66(14) 5_556 1_565 ?
O4 K1 N4 98.76(17) 7_546 1_565 ?
O8 K1 N4 56.31(13) 1_565 1_565 ?
O5 K1 N4 113.99(13) . 1_565 ?
N3 K1 N4 169.68(14) . 1_565 ?
O8 K1 N4 115.97(13) 5_546 1_565 ?
O1 K1 O2W 74.21(11) 5_556 . ?
O4 K1 O2W 66.07(12) 7_546 . ?
O8 K1 O2W 123.98(16) 1_565 . ?
O5 K1 O2W 133.59(12) . . ?
N3 K1 O2W 107.02(19) . . ?
O8 K1 O2W 140.14(11) 5_546 . ?
N4 K1 O2W 77.53(19) 1_565 . ?
O1 K1 O1W 66.68(14) 5_556 . ?
O4 K1 O1W 88.76(15) 7_546 . ?
O8 K1 O1W 178.09(13) 1_565 . ?
O5 K1 O1W 120.99(14) . . ?
N3 K1 O1W 66.02(15) . . ?
O8 K1 O1W 90.30(13) 5_546 . ?
N4 K1 O1W 122.92(15) 1_565 . ?
O2W K1 O1W 54.32(16) . . ?
O1 K1 K1 95.60(10) 5_556 5_556 ?
O4 K1 K1 122.95(11) 7_546 5_556 ?
O8 K1 K1 46.86(8) 1_565 5_556 ?
O5 K1 K1 58.94(9) . 5_556 ?
N3 K1 K1 90.22(11) . 5_556 ?
O8 K1 K1 44.73(8) 5_546 5_556 ?
N4 K1 K1 85.94(11) 1_565 5_556 ?
O2W K1 K1 162.52(17) . 5_556 ?
O1W K1 K1 135.03(11) . 5_556 ?
O1 K1 Sm1 37.47(9) 5_556 5_556 ?
O4 K1 Sm1 166.24(13) 7_546 5_556 ?
O8 K1 Sm1 103.16(9) 1_565 5_556 ?
O5 K1 Sm1 114.47(10) . 5_556 ?
N3 K1 Sm1 94.47(11) . 5_556 ?
O8 K1 Sm1 37.68(8) 5_546 5_556 ?
N4 K1 Sm1 92.63(10) 1_565 5_556 ?
O2W K1 Sm1 109.38(4) . 5_556 ?
O1W K1 Sm1 78.52(10) . 5_556 ?
K1 K1 Sm1 65.32(4) 5_556 5_556 ?
O1 K1 Sm1 146.64(11) 5_556 . ?
O4 K1 Sm1 65.36(10) 7_546 . ?
O8 K1 Sm1 33.09(8) 1_565 . ?
O5 K1 Sm1 30.67(8) . . ?
N3 K1 Sm1 86.01(10) . . ?
O8 K1 Sm1 95.50(9) 5_546 . ?
N4 K1 Sm1 83.82(10) 1_565 . ?
O2W K1 Sm1 123.95(5) . . ?
O1W K1 Sm1 146.37(11) . . ?
K1 K1 Sm1 58.67(3) 5_556 . ?
Sm1 K1 Sm1 123.99(4) 5_556 . ?
N1 S1 N2 98.8(3) . . ?
N3 S2 N4 98.8(2) . . ?
C3 O1 Sm1 88.5(3) . . ?
C3 O1 K1 168.0(4) . 5_556 ?
Sm1 O1 K1 103.44(14) . 5_556 ?
C3 O2 Sm1 95.3(3) . . ?
C4 O3 Sm1 143.8(4) . 7_546 ?
C4 O4 K1 127.3(4) . 7_546 ?
C7 O5 Sm1 116.2(4) . . ?
C7 O5 K1 128.1(4) . . ?
Sm1 O5 K1 112.98(15) . . ?
C7 O6 Sm1 135.8(4) . 7_546 ?
C8 O7 Sm1 149.7(4) . 7_546 ?
C8 O7 Sm1 91.3(3) . 1_545 ?
Sm1 O7 Sm1 117.41(14) 7_546 1_545 ?
C8 O8 Sm1 95.8(3) . 1_545 ?
C8 O8 K1 114.7(3) . 1_545 ?
Sm1 O8 K1 109.70(14) 1_545 1_545 ?
C8 O8 K1 147.2(4) . 5_546 ?
Sm1 O8 K1 97.73(13) 1_545 5_546 ?
K1 O8 K1 88.41(11) 1_545 5_546 ?
Sm1 O9 H9A 119(5) . . ?
Sm1 O9 H9B 131(5) . . ?
H9A O9 H9B 110(3) . . ?
C1 N1 S1 106.7(4) . . ?
C2 N2 S1 107.3(4) . . ?
C5 N3 S2 108.3(4) . . ?
C5 N3 K1 120.5(4) . . ?
S2 N3 K1 130.9(3) . . ?
C6 N4 S2 107.1(4) . . ?
C6 N4 K1 115.2(4) . 1_545 ?
S2 N4 K1 137.6(3) . 1_545 ?
N1 C1 C2 113.5(5) . . ?
N1 C1 C3 121.9(5) . . ?
C2 C1 C3 124.5(5) . . ?
N2 C2 C1 113.7(5) . . ?
N2 C2 C4 119.3(5) . . ?
C1 C2 C4 127.0(5) . . ?
O1 C3 O2 123.6(5) . . ?
O1 C3 C1 120.8(5) . . ?
O2 C3 C1 115.6(5) . . ?
O1 C3 Sm1 65.6(3) . . ?
O2 C3 Sm1 58.5(3) . . ?
C1 C3 Sm1 168.8(4) . . ?
O4 C4 O3 127.2(5) . . ?
O4 C4 C2 118.5(5) . . ?
O3 C4 C2 114.3(5) . . ?
N3 C5 C6 112.0(5) . . ?
N3 C5 C7 118.8(5) . . ?
C6 C5 C7 129.2(5) . . ?
N4 C6 C5 113.8(5) . . ?
N4 C6 C8 115.7(5) . . ?
C5 C6 C8 130.4(5) . . ?
O6 C7 O5 125.0(5) . . ?
O6 C7 C5 119.0(5) . . ?
O5 C7 C5 116.0(5) . . ?
O8 C8 O7 122.2(5) . . ?
O8 C8 C6 117.9(5) . . ?
O7 C8 C6 119.6(5) . . ?
O8 C8 Sm1 59.1(3) . 1_545 ?
O7 C8 Sm1 63.4(3) . 1_545 ?
C6 C8 Sm1 170.3(4) . 1_545 ?
K1 O1W H1A 109.8(15) . . ?
K1 O1W H1B 109.6(15) . . ?
H1A O1W H1B 111(3) . . ?
K1 O2W K1 150.0(3) . 2_556 ?
K1 O2W H2 91(6) . . ?
K1 O2W H2 108(6) 2_556 . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O9 H9A O3 0.95(2) 1.89(3) 2.811(6) 164(8) 1_565
O9 H9B O1W 0.94(2) 1.89(3) 2.815(7) 170(9) 5_556
O1W H1A O4 0.90(2) 1.96(3) 2.782(7) 151(4) 8_446
O1W H1B O1W 0.90(2) 2.74(6) 3.367(12) 127(5) 2_556
O2W H2 N1 0.94(2) 2.05(3) 2.976(7) 171(9) 5_556

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        25.15
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         1.291
_refine_diff_density_min         -0.951
_refine_diff_density_rms         0.128
_database_code_depnum_ccdc_archive 'CCDC 957583'
#######################################################################
#
#                 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_compound6

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C8 H5 Eu K N4 O10.50 S2'
_chemical_formula_sum            'C8 H5 Eu K N4 O10.50 S2'
_chemical_formula_weight         580.34

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'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   c2/c

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

_cell_length_a                   18.017(7)
_cell_length_b                   8.423(4)
_cell_length_c                   20.231(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.709(6)
_cell_angle_gamma                90.00
_cell_volume                     3070(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2691
_cell_measurement_theta_min      2.01
_cell_measurement_theta_max      24.99

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    2.511
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2232
_exptl_absorpt_coefficient_mu    4.698
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.3583
_exptl_absorpt_correction_T_max  0.4471
_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 9.00cm
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            7559
_diffrn_reflns_av_R_equivalents  0.0254
_diffrn_reflns_av_sigmaI/netI    0.0285
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.01
_diffrn_reflns_theta_max         24.99
_reflns_number_total             2691
_reflns_number_gt                2490
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXP-97
_computing_publication_material  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. Standard DFIX restraints were
used for the distance of the atoms, such as (o9 and h9a), (o9 and h9b),
(o2w and h2), (h9a and h9b), (o1w and h1a), (o1w and h1b), (h1a and h1b).
;

_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)+(0.0176P)²+3.0170P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2691
_refine_ls_number_parameters     255
_refine_ls_number_restraints     11
_refine_ls_R_factor_all          0.0212
_refine_ls_R_factor_gt           0.0193
_refine_ls_wR_factor_ref         0.0463
_refine_ls_wR_factor_gt          0.0452
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_restrained_S_all      1.181
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Eu1 Eu 0.207884(9) 0.014324(19) 0.480088(8) 0.01354(7) Uani 1 1 d . . .
K1 K 0.00603(5) -0.00826(9) 0.59919(5) 0.0296(2) Uani 1 1 d D . .
S1 S 0.15209(6) -0.44203(14) 0.21296(5) 0.0367(3) Uani 1 1 d . . .
S2 S -0.02641(6) -0.49415(11) 0.62620(6) 0.0282(2) Uani 1 1 d . . .
O1 O 0.13143(12) -0.1046(3) 0.38246(12) 0.0234(6) Uani 1 1 d . . .
O2 O 0.25235(13) -0.1476(3) 0.38930(11) 0.0213(6) Uani 1 1 d . . .
O3 O 0.28325(14) -0.5310(3) 0.40253(12) 0.0232(6) Uani 1 1 d . . .
O4 O 0.36563(15) -0.4326(4) 0.33185(14) 0.0406(8) Uani 1 1 d . . .
O5 O 0.11448(14) -0.1679(3) 0.52137(12) 0.0236(6) Uani 1 1 d . . .
O6 O 0.18018(13) -0.3752(3) 0.48898(12) 0.0235(6) Uani 1 1 d . . .
O7 O 0.18672(12) -0.6925(3) 0.52209(12) 0.0195(5) Uani 1 1 d . . .
O8 O 0.08766(12) -0.8396(3) 0.50323(12) 0.0196(5) Uani 1 1 d . . .
O9 O 0.19311(16) 0.1993(3) 0.38749(13) 0.0310(7) Uani 1 1 d D . .
N1 N 0.13312(16) -0.2965(4) 0.26379(15) 0.0250(7) Uani 1 1 d . . .
N2 N 0.2261(2) -0.5117(4) 0.25051(17) 0.0322(9) Uani 1 1 d . . .
N3 N 0.02313(16) -0.3542(3) 0.59403(15) 0.0215(7) Uani 1 1 d . . .
N4 N 0.01469(16) -0.6461(3) 0.59292(15) 0.0226(7) Uani 1 1 d . . .
C1 C 0.18526(18) -0.2973(4) 0.31052(16) 0.0169(7) Uani 1 1 d . . .
C2 C 0.23846(19) -0.4214(4) 0.30304(16) 0.0186(7) Uani 1 1 d . . .
C3 C 0.18893(19) -0.1735(4) 0.36398(17) 0.0186(8) Uani 1 1 d . . .
C4 C 0.3025(2) -0.4625(4) 0.34933(18) 0.0202(8) Uani 1 1 d . . .
C5 C 0.07475(17) -0.4202(4) 0.55677(16) 0.0145(7) Uani 1 1 d . . .
C6 C 0.06959(17) -0.5903(4) 0.55644(16) 0.0156(7) Uani 1 1 d . . .
C7 C 0.12780(18) -0.3130(4) 0.51973(17) 0.0164(7) Uani 1 1 d . . .
C8 C 0.11751(18) -0.7142(4) 0.52396(17) 0.0162(7) Uani 1 1 d . . .
O1W O -0.08455(19) -0.1992(4) 0.71438(14) 0.0502(9) Uani 1 1 d D . .
O2W O 0.0000 0.0886(6) 0.7500 0.0682(16) Uani 1 2 d SD . .
H9A H 0.220(2) 0.295(4) 0.383(2) 0.080 Uiso 1 1 d D . .
H9B H 0.159(2) 0.189(6) 0.3529(19) 0.080 Uiso 1 1 d D . .
H1A H -0.105(2) -0.138(3) 0.7455(15) 0.080 Uiso 1 1 d D . .
H1B H -0.0554(16) -0.271(4) 0.7362(17) 0.080 Uiso 1 1 d D . .
H2 H -0.039(2) 0.159(5) 0.743(3) 0.080 Uiso 1 1 d D . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Eu1 O3 2.382(3) 7_546 ?
Eu1 O6 2.409(2) 7_546 ?
Eu1 O7 2.421(2) 7_546 ?
Eu1 O2 2.431(2) . ?
Eu1 O5 2.433(2) . ?
Eu1 O9 2.449(3) . ?
Eu1 O8 2.540(2) 1_565 ?
Eu1 O1 2.595(2) . ?
Eu1 O7 2.640(2) 1_565 ?
Eu1 C3 2.849(4) . ?
Eu1 C8 2.951(3) 1_565 ?
Eu1 C7 3.218(3) . ?
K1 O1 2.683(3) 5_556 ?
K1 O4 2.731(3) 7_546 ?
K1 O8 2.832(3) 1_565 ?
K1 O5 2.860(3) . ?
K1 N3 2.932(3) . ?
K1 O8 2.949(3) 5_546 ?
K1 N4 3.057(3) 1_565 ?
K1 O2W 3.161(2) . ?
K1 O1W 3.283(4) . ?
K1 K1 4.019(3) 5_556 ?
K1 Eu1 4.1566(17) 5_556 ?
S1 N2 1.636(4) . ?
S1 N1 1.639(3) . ?
S2 N3 1.620(3) . ?
S2 N4 1.629(3) . ?
O1 C3 1.249(4) . ?
O1 K1 2.683(3) 5_556 ?
O2 C3 1.265(4) . ?
O3 C4 1.273(4) . ?
O3 Eu1 2.382(3) 7_546 ?
O4 C4 1.222(4) . ?
O4 K1 2.731(3) 7_546 ?
O5 C7 1.246(4) . ?
O6 C7 1.252(4) . ?
O6 Eu1 2.409(2) 7_546 ?
O7 C8 1.261(4) . ?
O7 Eu1 2.421(2) 7_546 ?
O7 Eu1 2.640(2) 1_545 ?
O8 C8 1.255(4) . ?
O8 Eu1 2.540(2) 1_545 ?
O8 K1 2.832(3) 1_545 ?
O8 K1 2.949(3) 5_546 ?
O9 H9A 0.94(2) . ?
O9 H9B 0.93(2) . ?
N1 C1 1.324(4) . ?
N2 C2 1.324(5) . ?
N3 C5 1.326(4) . ?
N4 C6 1.327(4) . ?
N4 K1 3.057(3) 1_545 ?
C1 C2 1.428(5) . ?
C1 C3 1.503(5) . ?
C2 C4 1.516(5) . ?
C5 C6 1.436(5) . ?
C5 C7 1.519(5) . ?
C6 C8 1.510(5) . ?
C8 Eu1 2.951(3) 1_545 ?
O1W H1A 0.900(19) . ?
O1W H1B 0.911(19) . ?
O2W K1 3.161(2) 2_556 ?
O2W H2 0.93(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Eu1 O6 73.99(8) 7_546 7_546 ?
O3 Eu1 O7 86.48(8) 7_546 7_546 ?
O6 Eu1 O7 69.64(9) 7_546 7_546 ?
O3 Eu1 O2 140.13(8) 7_546 . ?
O6 Eu1 O2 68.94(8) 7_546 . ?
O7 Eu1 O2 93.91(8) 7_546 . ?
O3 Eu1 O5 74.53(8) 7_546 . ?
O6 Eu1 O5 100.62(9) 7_546 . ?
O7 Eu1 O5 160.59(8) 7_546 . ?
O2 Eu1 O5 98.12(8) . . ?
O3 Eu1 O9 136.91(9) 7_546 . ?
O6 Eu1 O9 126.24(9) 7_546 . ?
O7 Eu1 O9 70.70(9) 7_546 . ?
O2 Eu1 O9 79.21(9) . . ?
O5 Eu1 O9 126.51(9) . . ?
O3 Eu1 O8 80.47(8) 7_546 1_565 ?
O6 Eu1 O8 154.31(8) 7_546 1_565 ?
O7 Eu1 O8 111.96(8) 7_546 1_565 ?
O2 Eu1 O8 134.48(8) . 1_565 ?
O5 Eu1 O8 69.34(8) . 1_565 ?
O9 Eu1 O8 75.39(9) . 1_565 ?
O3 Eu1 O1 144.09(8) 7_546 . ?
O6 Eu1 O1 116.41(8) 7_546 . ?
O7 Eu1 O1 129.38(8) 7_546 . ?
O2 Eu1 O1 52.07(8) . . ?
O5 Eu1 O1 69.81(8) . . ?
O9 Eu1 O1 67.15(9) . . ?
O8 Eu1 O1 83.18(8) 1_565 . ?
O3 Eu1 O7 68.42(8) 7_546 1_565 ?
O6 Eu1 O7 119.69(8) 7_546 1_565 ?
O7 Eu1 O7 62.78(9) 7_546 1_565 ?
O2 Eu1 O7 144.87(8) . 1_565 ?
O5 Eu1 O7 112.10(8) . 1_565 ?
O9 Eu1 O7 68.67(9) . 1_565 ?
O8 Eu1 O7 50.27(7) 1_565 1_565 ?
O1 Eu1 O7 121.90(7) . 1_565 ?
O3 Eu1 C3 149.37(9) 7_546 . ?
O6 Eu1 C3 92.02(9) 7_546 . ?
O7 Eu1 C3 114.54(9) 7_546 . ?
O2 Eu1 C3 26.23(9) . . ?
O5 Eu1 C3 81.74(9) . . ?
O9 Eu1 C3 73.26(10) . . ?
O8 Eu1 C3 109.10(9) 1_565 . ?
O1 Eu1 C3 25.99(8) . . ?
O7 Eu1 C3 140.20(9) 1_565 . ?
O3 Eu1 C8 71.63(9) 7_546 1_565 ?
O6 Eu1 C8 139.68(9) 7_546 1_565 ?
O7 Eu1 C8 87.75(9) 7_546 1_565 ?
O2 Eu1 C8 148.24(9) . 1_565 ?
O5 Eu1 C8 89.95(9) . 1_565 ?
O9 Eu1 C8 71.44(10) . 1_565 ?
O8 Eu1 C8 25.03(8) 1_565 1_565 ?
O1 Eu1 C8 103.79(8) . 1_565 ?
O7 Eu1 C8 25.30(8) 1_565 1_565 ?
C3 Eu1 C8 128.14(10) . 1_565 ?
O3 Eu1 C7 80.03(8) 7_546 . ?
O6 Eu1 C7 83.97(9) 7_546 . ?
O7 Eu1 C7 152.85(8) 7_546 . ?
O2 Eu1 C7 81.99(9) . . ?
O5 Eu1 C7 19.91(8) . . ?
O9 Eu1 C7 133.72(9) . . ?
O8 Eu1 C7 89.03(8) 1_565 . ?
O1 Eu1 C7 67.89(8) . . ?
O7 Eu1 C7 130.84(8) 1_565 . ?
C3 Eu1 C7 71.34(9) . . ?
C8 Eu1 C7 109.77(10) 1_565 . ?
O1 K1 O4 140.45(9) 5_556 7_546 ?
O1 K1 O8 113.91(8) 5_556 1_565 ?
O4 K1 O8 89.89(8) 7_546 1_565 ?
O1 K1 O5 151.73(8) 5_556 . ?
O4 K1 O5 67.40(9) 7_546 . ?
O8 K1 O5 59.63(7) 1_565 . ?
O1 K1 N3 117.03(8) 5_556 . ?
O4 K1 N3 75.43(10) 7_546 . ?
O8 K1 N3 114.73(8) 1_565 . ?
O5 K1 N3 55.97(7) . . ?
O1 K1 O8 74.32(7) 5_556 5_546 ?
O4 K1 O8 138.86(9) 7_546 5_546 ?
O8 K1 O8 91.94(7) 1_565 5_546 ?
O5 K1 O8 78.34(8) . 5_546 ?
N3 K1 O8 66.59(8) . 5_546 ?
O1 K1 N4 72.54(8) 5_556 1_565 ?
O4 K1 N4 99.20(9) 7_546 1_565 ?
O8 K1 N4 56.21(7) 1_565 1_565 ?
O5 K1 N4 114.25(8) . 1_565 ?
N3 K1 N4 169.96(9) . 1_565 ?
O8 K1 N4 115.68(8) 5_546 1_565 ?
O1 K1 O2W 74.47(6) 5_556 . ?
O4 K1 O2W 65.99(7) 7_546 . ?
O8 K1 O2W 123.82(9) 1_565 . ?
O5 K1 O2W 133.19(7) . . ?
N3 K1 O2W 107.20(11) . . ?
O8 K1 O2W 139.81(7) 5_546 . ?
N4 K1 O2W 77.58(11) 1_565 . ?
O1 K1 O1W 66.89(8) 5_556 . ?
O4 K1 O1W 88.47(9) 7_546 . ?
O8 K1 O1W 178.02(8) 1_565 . ?
O5 K1 O1W 120.62(8) . . ?
N3 K1 O1W 65.90(8) . . ?
O8 K1 O1W 90.03(8) 5_546 . ?
N4 K1 O1W 122.99(9) 1_565 . ?
O2W K1 O1W 54.41(10) . . ?
O1 K1 K1 95.01(6) 5_556 5_556 ?
O4 K1 K1 123.46(7) 7_546 5_556 ?
O8 K1 K1 47.17(5) 1_565 5_556 ?
O5 K1 K1 59.70(6) . 5_556 ?
N3 K1 K1 90.18(7) . 5_556 ?
O8 K1 K1 44.77(5) 5_546 5_556 ?
N4 K1 K1 85.77(6) 1_565 5_556 ?
O2W K1 K1 162.31(10) . 5_556 ?
O1W K1 K1 134.80(7) . 5_556 ?
O1 K1 Eu1 37.30(6) 5_556 5_556 ?
O4 K1 Eu1 165.90(7) 7_546 5_556 ?
O8 K1 Eu1 103.21(6) 1_565 5_556 ?
O5 K1 Eu1 114.72(6) . 5_556 ?
N3 K1 Eu1 94.09(6) . 5_556 ?
O8 K1 Eu1 37.22(4) 5_546 5_556 ?
N4 K1 Eu1 92.51(6) 1_565 5_556 ?
O2W K1 Eu1 109.44(3) . 5_556 ?
O1W K1 Eu1 78.53(6) . 5_556 ?
K1 K1 Eu1 64.95(3) 5_556 5_556 ?
O1 K1 Eu1 146.38(6) 5_556 . ?
O4 K1 Eu1 65.58(7) 7_546 . ?
O8 K1 Eu1 33.02(5) 1_565 . ?
O5 K1 Eu1 30.95(5) . . ?
N3 K1 Eu1 86.30(6) . . ?
O8 K1 Eu1 95.97(6) 5_546 . ?
N4 K1 Eu1 83.74(6) 1_565 . ?
O2W K1 Eu1 123.85(4) . . ?
O1W K1 Eu1 146.42(6) . . ?
K1 K1 Eu1 59.04(3) 5_556 . ?
Eu1 K1 Eu1 123.99(4) 5_556 . ?
N2 S1 N1 98.75(16) . . ?
N3 S2 N4 98.64(16) . . ?
C3 O1 Eu1 88.5(2) . . ?
C3 O1 K1 167.6(2) . 5_556 ?
Eu1 O1 K1 103.90(9) . 5_556 ?
C3 O2 Eu1 95.7(2) . . ?
C4 O3 Eu1 143.2(2) . 7_546 ?
C4 O4 K1 126.9(3) . 7_546 ?
C7 O5 Eu1 118.4(2) . . ?
C7 O5 K1 127.5(2) . . ?
Eu1 O5 K1 111.86(9) . . ?
C7 O6 Eu1 135.1(2) . 7_546 ?
C8 O7 Eu1 150.0(2) . 7_546 ?
C8 O7 Eu1 91.23(19) . 1_545 ?
Eu1 O7 Eu1 117.22(9) 7_546 1_545 ?
C8 O8 Eu1 96.1(2) . 1_545 ?
C8 O8 K1 114.6(2) . 1_545 ?
Eu1 O8 K1 109.55(9) 1_545 1_545 ?
C8 O8 K1 147.1(2) . 5_546 ?
Eu1 O8 K1 98.17(8) 1_545 5_546 ?
K1 O8 K1 88.06(7) 1_545 5_546 ?
Eu1 O9 H9A 125(3) . . ?
Eu1 O9 H9B 126(3) . . ?
H9A O9 H9B 110(3) . . ?
C1 N1 S1 107.0(2) . . ?
C2 N2 S1 107.1(3) . . ?
C5 N3 S2 108.5(2) . . ?
C5 N3 K1 120.8(2) . . ?
S2 N3 K1 130.55(15) . . ?
C6 N4 S2 107.3(2) . . ?
C6 N4 K1 114.5(2) . 1_545 ?
S2 N4 K1 138.03(15) . 1_545 ?
N1 C1 C2 113.5(3) . . ?
N1 C1 C3 122.3(3) . . ?
C2 C1 C3 124.1(3) . . ?
N2 C2 C1 113.6(3) . . ?
N2 C2 C4 118.9(3) . . ?
C1 C2 C4 127.5(3) . . ?
O1 C3 O2 123.1(3) . . ?
O1 C3 C1 120.6(3) . . ?
O2 C3 C1 116.3(3) . . ?
O1 C3 Eu1 65.56(19) . . ?
O2 C3 Eu1 58.12(17) . . ?
C1 C3 Eu1 169.2(2) . . ?
O4 C4 O3 127.0(3) . . ?
O4 C4 C2 118.6(3) . . ?
O3 C4 C2 114.4(3) . . ?
N3 C5 C6 112.0(3) . . ?
N3 C5 C7 118.8(3) . . ?
C6 C5 C7 129.2(3) . . ?
N4 C6 C5 113.5(3) . . ?
N4 C6 C8 115.6(3) . . ?
C5 C6 C8 130.8(3) . . ?
O5 C7 O6 124.8(3) . . ?
O5 C7 C5 116.6(3) . . ?
O6 C7 C5 118.6(3) . . ?
O5 C7 Eu1 41.71(17) . . ?
O6 C7 Eu1 83.8(2) . . ?
C5 C7 Eu1 156.8(2) . . ?
O8 C8 O7 122.1(3) . . ?
O8 C8 C6 118.8(3) . . ?
O7 C8 C6 119.0(3) . . ?
O8 C8 Eu1 58.86(17) . 1_545 ?
O7 C8 Eu1 63.47(17) . 1_545 ?
C6 C8 Eu1 170.8(2) . 1_545 ?
K1 O1W H1A 115.3(15) . . ?
K1 O1W H1B 112.3(14) . . ?
H1A O1W H1B 106(2) . . ?
K1 O2W K1 150.09(19) 2_556 . ?
K1 O2W H2 106(3) 2_556 . ?
K1 O2W H2 93(3) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O9 H9A O3 0.94(2) 1.90(2) 2.806(4) 161(4) 1_565
O9 H9B O1W 0.93(2) 1.90(2) 2.824(4) 171(5) 5_556
O1W H1A O4 0.900(19) 1.92(2) 2.782(4) 159(3) 8_446
O1W H1A O2W 0.900(19) 2.69(4) 2.948(6) 98(2) .
O1W H1B O1W 0.911(19) 2.77(4) 3.354(7) 123(3) 2_556
O2W H2 N1 0.93(2) 2.06(2) 2.980(4) 172(5) 5_556

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        24.99
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.441
_refine_diff_density_min         -0.596
_refine_diff_density_rms         0.096
_database_code_depnum_ccdc_archive 'CCDC 957584'
#######################################################################
#
#                 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_compound7

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C8 H5 Gd K N4 O10.50 S2'
_chemical_formula_sum            'C8 H5 Gd K N4 O10.50 S2'
_chemical_formula_weight         585.63

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'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   c2/c

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

_cell_length_a                   17.9598(11)
_cell_length_b                   8.3889(5)
_cell_length_c                   20.1191(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.6390(10)
_cell_angle_gamma                90.00
_cell_volume                     3031.0(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2691
_cell_measurement_theta_min      2.02
_cell_measurement_theta_max      25.09

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    2.567
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2240
_exptl_absorpt_coefficient_mu    4.996
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.3583
_exptl_absorpt_correction_T_max  0.4471
_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 9.00cm
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            7537
_diffrn_reflns_av_R_equivalents  0.0248
_diffrn_reflns_av_sigmaI/netI    0.0277
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.02
_diffrn_reflns_theta_max         25.09
_reflns_number_total             2691
_reflns_number_gt                2517
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXP-97
_computing_publication_material  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. Standard DFIX restraints were
used for the distance of the atoms, such as (o9 and h9a), (o9 and h9b),
(o2w and h2), (h9a and h9b), (o1w and h1a), (o1w and h1b), (h1a and h1b).
;

_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)+(0.0136P)²+5.9064P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2691
_refine_ls_number_parameters     255
_refine_ls_number_restraints     11
_refine_ls_R_factor_all          0.0198
_refine_ls_R_factor_gt           0.0181
_refine_ls_wR_factor_ref         0.0428
_refine_ls_wR_factor_gt          0.0420
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.112
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Gd1 Gd 0.207966(8) 0.015997(17) 0.480171(7) 0.01368(7) Uani 1 1 d . . .
K1 K 0.00642(4) -0.00850(9) 0.59930(5) 0.02978(19) Uani 1 1 d D . .
S1 S 0.15179(6) -0.44123(13) 0.21333(5) 0.0371(2) Uani 1 1 d . . .
S2 S -0.02656(5) -0.49308(10) 0.62588(5) 0.0281(2) Uani 1 1 d . . .
O1 O 0.13141(12) -0.1028(3) 0.38306(11) 0.0238(5) Uani 1 1 d . . .
O2 O 0.25238(12) -0.1462(3) 0.38969(11) 0.0222(5) Uani 1 1 d . . .
O3 O 0.28346(14) -0.5319(3) 0.40232(12) 0.0246(5) Uani 1 1 d . . .
O4 O 0.36570(14) -0.4310(4) 0.33167(13) 0.0422(7) Uani 1 1 d . . .
O5 O 0.11653(13) -0.1690(3) 0.52131(12) 0.0236(5) Uani 1 1 d . . .
O6 O 0.18084(12) -0.3782(3) 0.48843(11) 0.0227(5) Uani 1 1 d . . .
O7 O 0.18690(11) -0.6933(2) 0.52221(11) 0.0190(5) Uani 1 1 d . . .
O8 O 0.08757(12) -0.8400(2) 0.50344(11) 0.0203(5) Uani 1 1 d . . .
O9 O 0.19350(15) 0.1989(3) 0.38769(12) 0.0311(6) Uani 1 1 d D . .
N1 N 0.13321(15) -0.2956(3) 0.26439(14) 0.0252(7) Uani 1 1 d . . .
N2 N 0.2258(2) -0.5109(4) 0.25099(17) 0.0340(8) Uani 1 1 d . . .
N3 N 0.02372(15) -0.3533(3) 0.59409(14) 0.0216(6) Uani 1 1 d . . .
N4 N 0.01438(15) -0.6456(3) 0.59273(15) 0.0235(6) Uani 1 1 d . . .
C1 C 0.18513(17) -0.2960(4) 0.31112(16) 0.0183(7) Uani 1 1 d . . .
C2 C 0.23808(18) -0.4213(4) 0.30339(16) 0.0202(7) Uani 1 1 d . . .
C3 C 0.18888(18) -0.1726(4) 0.36422(16) 0.0192(7) Uani 1 1 d . . .
C4 C 0.30223(19) -0.4625(4) 0.34930(16) 0.0202(7) Uani 1 1 d . . .
C5 C 0.07529(17) -0.4207(4) 0.55658(15) 0.0158(6) Uani 1 1 d . . .
C6 C 0.06940(17) -0.5904(4) 0.55639(15) 0.0164(7) Uani 1 1 d . . .
C7 C 0.12891(17) -0.3140(4) 0.51938(16) 0.0172(7) Uani 1 1 d . . .
C8 C 0.11746(16) -0.7143(4) 0.52385(15) 0.0147(7) Uani 1 1 d . . .
O1W O -0.08460(18) -0.2001(4) 0.71393(14) 0.0507(8) Uani 1 1 d D . .
O2W O 0.0000 0.0879(6) 0.7500 0.0705(16) Uani 1 2 d SD . .
H9A H 0.222(2) 0.290(4) 0.387(2) 0.080 Uiso 1 1 d D . .
H9B H 0.162(2) 0.187(5) 0.3525(18) 0.080 Uiso 1 1 d D . .
H1A H -0.110(2) -0.135(3) 0.7408(15) 0.080 Uiso 1 1 d D . .
H1B H -0.0533(14) -0.261(4) 0.7385(16) 0.080 Uiso 1 1 d D . .
H2 H -0.038(2) 0.164(4) 0.746(3) 0.080 Uiso 1 1 d D . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Gd1 O3 2.371(2) 7_546 ?
Gd1 O6 2.386(2) 7_546 ?
Gd1 O7 2.405(2) 7_546 ?
Gd1 O5 2.413(2) . ?
Gd1 O2 2.415(2) . ?
Gd1 O9 2.424(2) . ?
Gd1 O8 2.525(2) 1_565 ?
Gd1 O1 2.577(2) . ?
Gd1 O7 2.610(2) 1_565 ?
Gd1 C3 2.836(3) . ?
Gd1 C8 2.927(3) 1_565 ?
Gd1 K1 4.1531(9) 5_556 ?
K1 O1 2.673(2) 5_556 ?
K1 O4 2.718(3) 7_546 ?
K1 O8 2.811(2) 1_565 ?
K1 O5 2.873(2) . ?
K1 N3 2.911(3) . ?
K1 O8 2.943(2) 5_546 ?
K1 N4 3.051(3) 1_565 ?
K1 O2W 3.1414(15) . ?
K1 O1W 3.265(3) . ?
K1 C8 3.527(3) 1_565 ?
K1 K1 4.0021(19) 5_556 ?
K1 Gd1 4.1531(9) 5_556 ?
S1 N2 1.631(3) . ?
S1 N1 1.633(3) . ?
S2 N3 1.616(3) . ?
S2 N4 1.623(3) . ?
O1 C3 1.249(4) . ?
O1 K1 2.673(2) 5_556 ?
O2 C3 1.265(4) . ?
O3 C4 1.264(4) . ?
O3 Gd1 2.371(2) 7_546 ?
O4 C4 1.226(4) . ?
O4 K1 2.718(3) 7_546 ?
O5 C7 1.237(4) . ?
O6 C7 1.249(4) . ?
O6 Gd1 2.386(2) 7_546 ?
O7 C8 1.260(4) . ?
O7 Gd1 2.405(2) 7_546 ?
O7 Gd1 2.610(2) 1_545 ?
O8 C8 1.251(4) . ?
O8 Gd1 2.525(2) 1_545 ?
O8 K1 2.811(2) 1_545 ?
O8 K1 2.943(2) 5_546 ?
O9 H9A 0.92(2) . ?
O9 H9B 0.91(2) . ?
N1 C1 1.317(4) . ?
N2 C2 1.311(4) . ?
N3 C5 1.328(4) . ?
N4 C6 1.320(4) . ?
N4 K1 3.051(3) 1_545 ?
C1 C2 1.427(4) . ?
C1 C3 1.488(4) . ?
C2 C4 1.509(5) . ?
C5 C6 1.428(5) . ?
C5 C7 1.518(4) . ?
C6 C8 1.505(4) . ?
C8 Gd1 2.927(3) 1_545 ?
C8 K1 3.527(3) 1_545 ?
O1W H1A 0.892(19) . ?
O1W H1B 0.901(18) . ?
O2W K1 3.1414(15) 2_556 ?
O2W H2 0.93(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Gd1 O6 73.65(8) 7_546 7_546 ?
O3 Gd1 O7 86.72(8) 7_546 7_546 ?
O6 Gd1 O7 69.51(7) 7_546 7_546 ?
O3 Gd1 O5 74.40(8) 7_546 . ?
O6 Gd1 O5 99.69(8) 7_546 . ?
O7 Gd1 O5 160.46(8) 7_546 . ?
O3 Gd1 O2 139.90(8) 7_546 . ?
O6 Gd1 O2 69.16(7) 7_546 . ?
O7 Gd1 O2 93.86(7) 7_546 . ?
O5 Gd1 O2 97.35(8) . . ?
O3 Gd1 O9 137.31(8) 7_546 . ?
O6 Gd1 O9 126.31(8) 7_546 . ?
O7 Gd1 O9 70.76(8) 7_546 . ?
O5 Gd1 O9 127.10(8) . . ?
O2 Gd1 O9 79.13(8) . . ?
O3 Gd1 O8 80.47(8) 7_546 1_565 ?
O6 Gd1 O8 153.94(7) 7_546 1_565 ?
O7 Gd1 O8 112.46(7) 7_546 1_565 ?
O5 Gd1 O8 69.91(7) . 1_565 ?
O2 Gd1 O8 134.42(7) . 1_565 ?
O9 Gd1 O8 75.81(8) . 1_565 ?
O3 Gd1 O1 143.69(8) 7_546 . ?
O6 Gd1 O1 116.82(8) 7_546 . ?
O7 Gd1 O1 129.53(7) 7_546 . ?
O5 Gd1 O1 69.63(8) . . ?
O2 Gd1 O1 52.31(7) . . ?
O9 Gd1 O1 67.11(8) . . ?
O8 Gd1 O1 82.81(7) 1_565 . ?
O3 Gd1 O7 68.43(7) 7_546 1_565 ?
O6 Gd1 O7 119.38(7) 7_546 1_565 ?
O7 Gd1 O7 62.95(8) 7_546 1_565 ?
O5 Gd1 O7 112.84(7) . 1_565 ?
O2 Gd1 O7 145.17(7) . 1_565 ?
O9 Gd1 O7 69.05(8) . 1_565 ?
O8 Gd1 O7 50.61(6) 1_565 1_565 ?
O1 Gd1 O7 121.93(7) . 1_565 ?
O3 Gd1 C3 149.02(8) 7_546 . ?
O6 Gd1 C3 92.33(9) 7_546 . ?
O7 Gd1 C3 114.61(8) 7_546 . ?
O5 Gd1 C3 81.19(8) . . ?
O2 Gd1 C3 26.34(8) . . ?
O9 Gd1 C3 73.19(9) . . ?
O8 Gd1 C3 108.87(8) 1_565 . ?
O1 Gd1 C3 26.12(8) . . ?
O7 Gd1 C3 140.45(8) 1_565 . ?
O3 Gd1 C8 71.78(8) 7_546 1_565 ?
O6 Gd1 C8 139.54(8) 7_546 1_565 ?
O7 Gd1 C8 88.09(8) 7_546 1_565 ?
O5 Gd1 C8 90.69(8) . 1_565 ?
O2 Gd1 C8 148.31(8) . 1_565 ?
O9 Gd1 C8 71.69(9) . 1_565 ?
O8 Gd1 C8 25.17(7) 1_565 1_565 ?
O1 Gd1 C8 103.49(8) . 1_565 ?
O7 Gd1 C8 25.49(7) 1_565 1_565 ?
C3 Gd1 C8 128.01(9) . 1_565 ?
O3 Gd1 K1 115.74(6) 7_546 5_556 ?
O6 Gd1 K1 149.78(6) 7_546 5_556 ?
O7 Gd1 K1 136.60(5) 7_546 5_556 ?
O5 Gd1 K1 59.38(6) . 5_556 ?
O2 Gd1 K1 90.79(5) . 5_556 ?
O9 Gd1 K1 67.86(6) . 5_556 ?
O8 Gd1 K1 44.48(5) 1_565 5_556 ?
O1 Gd1 K1 38.53(5) . 5_556 ?
O7 Gd1 K1 90.10(5) 1_565 5_556 ?
C3 Gd1 K1 64.65(7) . 5_556 ?
C8 Gd1 K1 67.15(6) 1_565 5_556 ?
O1 K1 O4 140.87(8) 5_556 7_546 ?
O1 K1 O8 113.79(7) 5_556 1_565 ?
O4 K1 O8 90.17(8) 7_546 1_565 ?
O1 K1 O5 151.68(8) 5_556 . ?
O4 K1 O5 66.97(8) 7_546 . ?
O8 K1 O5 59.72(6) 1_565 . ?
O1 K1 N3 116.82(8) 5_556 . ?
O4 K1 N3 75.10(9) 7_546 . ?
O8 K1 N3 114.74(7) 1_565 . ?
O5 K1 N3 55.96(7) . . ?
O1 K1 O8 73.70(7) 5_556 5_546 ?
O4 K1 O8 138.85(8) 7_546 5_546 ?
O8 K1 O8 91.89(6) 1_565 5_546 ?
O5 K1 O8 78.87(7) . 5_546 ?
N3 K1 O8 66.81(7) . 5_546 ?
O1 K1 N4 72.61(7) 5_556 1_565 ?
O4 K1 N4 99.72(9) 7_546 1_565 ?
O8 K1 N4 56.20(7) 1_565 1_565 ?
O5 K1 N4 114.28(7) . 1_565 ?
N3 K1 N4 170.04(8) . 1_565 ?
O8 K1 N4 115.30(7) 5_546 1_565 ?
O1 K1 O2W 74.80(6) 5_556 . ?
O4 K1 O2W 66.10(7) 7_546 . ?
O8 K1 O2W 123.89(8) 1_565 . ?
O5 K1 O2W 132.89(7) . . ?
N3 K1 O2W 107.19(10) . . ?
O8 K1 O2W 139.66(6) 5_546 . ?
N4 K1 O2W 77.71(10) 1_565 . ?
O1 K1 O1W 66.83(8) 5_556 . ?
O4 K1 O1W 88.50(8) 7_546 . ?
O8 K1 O1W 178.35(8) 1_565 . ?
O5 K1 O1W 120.53(8) . . ?
N3 K1 O1W 65.83(8) . . ?
O8 K1 O1W 89.76(7) 5_546 . ?
N4 K1 O1W 123.10(8) 1_565 . ?
O2W K1 O1W 54.61(9) . . ?
O1 K1 C8 109.97(7) 5_556 1_565 ?
O4 K1 C8 82.65(8) 7_546 1_565 ?
O8 K1 C8 18.75(6) 1_565 1_565 ?
O5 K1 C8 72.37(7) . 1_565 ?
N3 K1 C8 128.22(8) . 1_565 ?
O8 K1 C8 108.82(7) 5_546 1_565 ?
N4 K1 C8 41.93(7) 1_565 1_565 ?
O2W K1 C8 105.20(9) . 1_565 ?
O1W K1 C8 159.80(8) . 1_565 ?
O1 K1 K1 94.42(6) 5_556 5_556 ?
O4 K1 K1 123.76(7) 7_546 5_556 ?
O8 K1 K1 47.30(5) 1_565 5_556 ?
O5 K1 K1 60.26(5) . 5_556 ?
N3 K1 K1 90.26(6) . 5_556 ?
O8 K1 K1 44.59(5) 5_546 5_556 ?
N4 K1 K1 85.61(6) 1_565 5_556 ?
O2W K1 K1 162.19(9) . 5_556 ?
O1W K1 K1 134.35(6) . 5_556 ?
C8 K1 K1 64.66(5) 1_565 5_556 ?
O1 K1 Gd1 36.91(5) 5_556 5_556 ?
O4 K1 Gd1 165.51(7) 7_546 5_556 ?
O8 K1 Gd1 103.24(5) 1_565 5_556 ?
O5 K1 Gd1 115.05(5) . 5_556 ?
N3 K1 Gd1 94.01(6) . 5_556 ?
O8 K1 Gd1 36.96(4) 5_546 5_556 ?
N4 K1 Gd1 92.41(6) 1_565 5_556 ?
O2W K1 Gd1 109.36(2) . 5_556 ?
O1W K1 Gd1 78.18(6) . 5_556 ?
C8 K1 Gd1 111.79(5) 1_565 5_556 ?
K1 K1 Gd1 64.74(2) 5_556 5_556 ?
N2 S1 N1 98.45(15) . . ?
N3 S2 N4 98.73(15) . . ?
C3 O1 Gd1 88.60(19) . . ?
C3 O1 K1 166.8(2) . 5_556 ?
Gd1 O1 K1 104.55(8) . 5_556 ?
C3 O2 Gd1 95.74(19) . . ?
C4 O3 Gd1 143.2(2) . 7_546 ?
C4 O4 K1 126.5(2) . 7_546 ?
C7 O5 Gd1 119.9(2) . . ?
C7 O5 K1 127.1(2) . . ?
Gd1 O5 K1 111.17(8) . . ?
C7 O6 Gd1 134.7(2) . 7_546 ?
C8 O7 Gd1 149.8(2) . 7_546 ?
C8 O7 Gd1 91.44(18) . 1_545 ?
Gd1 O7 Gd1 117.05(8) 7_546 1_545 ?
C8 O8 Gd1 95.68(18) . 1_545 ?
C8 O8 K1 115.01(19) . 1_545 ?
Gd1 O8 K1 109.77(8) 1_545 1_545 ?
C8 O8 K1 146.66(19) . 5_546 ?
Gd1 O8 K1 98.56(7) 1_545 5_546 ?
K1 O8 K1 88.11(6) 1_545 5_546 ?
Gd1 O9 H9A 119(3) . . ?
Gd1 O9 H9B 126(3) . . ?
H9A O9 H9B 115(3) . . ?
C1 N1 S1 107.4(2) . . ?
C2 N2 S1 107.3(2) . . ?
C5 N3 S2 108.2(2) . . ?
C5 N3 K1 121.3(2) . . ?
S2 N3 K1 130.27(14) . . ?
C6 N4 S2 107.3(2) . . ?
C6 N4 K1 114.2(2) . 1_545 ?
S2 N4 K1 138.36(14) . 1_545 ?
N1 C1 C2 113.0(3) . . ?
N1 C1 C3 122.5(3) . . ?
C2 C1 C3 124.4(3) . . ?
N2 C2 C1 113.8(3) . . ?
N2 C2 C4 118.7(3) . . ?
C1 C2 C4 127.4(3) . . ?
O1 C3 O2 122.6(3) . . ?
O1 C3 C1 120.8(3) . . ?
O2 C3 C1 116.5(3) . . ?
O1 C3 Gd1 65.28(17) . . ?
O2 C3 Gd1 57.92(16) . . ?
C1 C3 Gd1 169.2(2) . . ?
O4 C4 O3 126.9(3) . . ?
O4 C4 C2 118.6(3) . . ?
O3 C4 C2 114.4(3) . . ?
N3 C5 C6 112.0(3) . . ?
N3 C5 C7 118.7(3) . . ?
C6 C5 C7 129.3(3) . . ?
N4 C6 C5 113.8(3) . . ?
N4 C6 C8 115.8(3) . . ?
C5 C6 C8 130.3(3) . . ?
O5 C7 O6 125.1(3) . . ?
O5 C7 C5 116.7(3) . . ?
O6 C7 C5 118.2(3) . . ?
O8 C8 O7 122.0(3) . . ?
O8 C8 C6 118.6(3) . . ?
O7 C8 C6 119.2(3) . . ?
O8 C8 Gd1 59.15(15) . 1_545 ?
O7 C8 Gd1 63.06(16) . 1_545 ?
C6 C8 Gd1 170.9(2) . 1_545 ?
O8 C8 K1 46.24(15) . 1_545 ?
O7 C8 K1 132.3(2) . 1_545 ?
C6 C8 K1 88.06(17) . 1_545 ?
Gd1 C8 K1 84.65(7) 1_545 1_545 ?
K1 O1W H1A 112.9(14) . . ?
K1 O1W H1B 110.5(13) . . ?
H1A O1W H1B 109(2) . . ?
K1 O2W K1 150.16(17) . 2_556 ?
K1 O2W H2 98(3) . . ?
K1 O2W H2 103(3) 2_556 . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O9 H9A O3 0.92(2) 1.88(2) 2.790(3) 169(4) 1_565
O9 H9B O1W 0.91(2) 1.91(2) 2.814(4) 168(5) 5_556
O1W H1A O4 0.892(19) 1.97(3) 2.769(4) 149(3) 8_446
O1W H1A O2W 0.892(19) 2.72(4) 2.941(5) 95(2) .
O1W H1B O1W 0.901(18) 2.69(3) 3.353(6) 131(3) 2_556
O2W H2 N1 0.93(2) 2.05(2) 2.971(4) 169(4) 5_556

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.09
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.423
_refine_diff_density_min         -0.361
_refine_diff_density_rms         0.085
_database_code_depnum_ccdc_archive 'CCDC 957585'
#######################################################################
#
#                 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_compound8

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C8 H5 K N4 O10.50 S2 Tb'
_chemical_formula_sum            'C8 H5 K N4 O10.50 S2 Tb'
_chemical_formula_weight         587.30

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   c2/c

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

_cell_length_a                   17.9851(18)
_cell_length_b                   8.4100(8)
_cell_length_c                   20.1083(19)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.563(2)
_cell_angle_gamma                90.00
_cell_volume                     3041.3(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2710
_cell_measurement_theta_min      2.03
_cell_measurement_theta_max      25.12

_exptl_crystal_description       block
_exptl_crystal_colour            COLORLESS
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.19
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    2.565
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2248
_exptl_absorpt_coefficient_mu    5.268
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.3357
_exptl_absorpt_correction_T_max  0.4314
_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 9.00cm
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            7574
_diffrn_reflns_av_R_equivalents  0.0257
_diffrn_reflns_av_sigmaI/netI    0.0290
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.03
_diffrn_reflns_theta_max         25.12
_reflns_number_total             2710
_reflns_number_gt                2610
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXP-97
_computing_publication_material  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. Standard DFIX restraints were
used for the distance of the atoms, such as (o9 and h9a), (o9 and h9b),
(o2w and h2), (h9a and h9b), (o1w and h1a), (o1w and h1b), (h1a and h1b).
;

_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)+(0.0151P)²+6.1929P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    none
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2710
_refine_ls_number_parameters     255
_refine_ls_number_restraints     11
_refine_ls_R_factor_all          0.0199
_refine_ls_R_factor_gt           0.0190
_refine_ls_wR_factor_ref         0.0461
_refine_ls_wR_factor_gt          0.0455
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_restrained_S_all      1.159
_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
Tb1 Tb 0.208050(8) 0.016858(17) 0.480321(7) 0.01310(7) Uani 1 1 d . . .
K1 K 0.00670(5) -0.00866(9) 0.59915(5) 0.0292(2) Uani 1 1 d D . .
S1 S 0.15157(6) -0.44077(13) 0.21356(5) 0.0362(2) Uani 1 1 d . . .
S2 S -0.02666(5) -0.49195(10) 0.62569(5) 0.0276(2) Uani 1 1 d . . .
O1 O 0.13114(12) -0.1012(3) 0.38308(12) 0.0241(5) Uani 1 1 d . . .
O2 O 0.25208(12) -0.1445(3) 0.39039(11) 0.0214(5) Uani 1 1 d . . .
O3 O 0.28383(14) -0.5323(3) 0.40274(12) 0.0239(5) Uani 1 1 d . . .
O4 O 0.36547(14) -0.4294(4) 0.33191(14) 0.0422(7) Uani 1 1 d . . .
O5 O 0.11795(13) -0.1689(3) 0.52119(12) 0.0227(5) Uani 1 1 d . . .
O6 O 0.18168(12) -0.3795(3) 0.48796(11) 0.0213(5) Uani 1 1 d . . .
O7 O 0.18731(11) -0.6931(3) 0.52262(11) 0.0185(5) Uani 1 1 d . . .
O8 O 0.08843(12) -0.8404(2) 0.50364(12) 0.0193(5) Uani 1 1 d . . .
O9 O 0.19350(15) 0.1986(3) 0.38805(12) 0.0300(6) Uani 1 1 d D . .
N1 N 0.13298(16) -0.2950(4) 0.26443(14) 0.0248(7) Uani 1 1 d . . .
N2 N 0.2256(2) -0.5107(4) 0.25149(18) 0.0317(8) Uani 1 1 d . . .
N3 N 0.02388(15) -0.3523(3) 0.59348(14) 0.0212(6) Uani 1 1 d . . .
N4 N 0.01421(16) -0.6449(3) 0.59239(15) 0.0232(6) Uani 1 1 d . . .
C1 C 0.18483(17) -0.2953(4) 0.31140(16) 0.0169(7) Uani 1 1 d . . .
C2 C 0.23798(18) -0.4203(4) 0.30350(16) 0.0189(7) Uani 1 1 d . . .
C3 C 0.18871(18) -0.1707(4) 0.36455(16) 0.0178(7) Uani 1 1 d . . .
C4 C 0.30233(19) -0.4611(4) 0.34967(17) 0.0197(7) Uani 1 1 d . . .
C5 C 0.07563(17) -0.4205(4) 0.55635(16) 0.0151(6) Uani 1 1 d . . .
C6 C 0.06971(17) -0.5907(4) 0.55605(16) 0.0156(7) Uani 1 1 d . . .
C7 C 0.12979(17) -0.3144(4) 0.51901(16) 0.0157(7) Uani 1 1 d . . .
C8 C 0.11794(17) -0.7143(4) 0.52377(16) 0.0153(7) Uani 1 1 d . . .
O1W O -0.08470(19) -0.1998(4) 0.71376(15) 0.0495(8) Uani 1 1 d D . .
O2W O 0.0000 0.0871(6) 0.7500 0.0657(16) Uani 1 2 d SD . .
H9A H 0.221(2) 0.292(4) 0.388(2) 0.080 Uiso 1 1 d D . .
H9B H 0.160(2) 0.193(6) 0.3525(18) 0.080 Uiso 1 1 d D . .
H1A H -0.103(2) -0.134(3) 0.7448(15) 0.080 Uiso 1 1 d D . .
H1B H -0.0550(17) -0.272(4) 0.7339(18) 0.080 Uiso 1 1 d D . .
H2 H -0.039(2) 0.160(5) 0.744(3) 0.080 Uiso 1 1 d D . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 O3 2.358(2) 7_546 ?
Tb1 O6 2.377(2) 7_546 ?
Tb1 O7 2.397(2) 7_546 ?
Tb1 O2 2.401(2) . ?
Tb1 O5 2.402(2) . ?
Tb1 O9 2.416(2) . ?
Tb1 O8 2.512(2) 1_565 ?
Tb1 O1 2.582(2) . ?
Tb1 O7 2.612(2) 1_565 ?
Tb1 C3 2.831(3) . ?
Tb1 C8 2.921(3) 1_565 ?
Tb1 K1 4.1658(10) 5_556 ?
K1 O1 2.673(2) 5_556 ?
K1 O4 2.723(3) 7_546 ?
K1 O8 2.812(2) 1_565 ?
K1 O5 2.888(2) . ?
K1 N3 2.909(3) . ?
K1 O8 2.957(2) 5_546 ?
K1 N4 3.065(3) 1_565 ?
K1 O2W 3.1418(16) . ?
K1 O1W 3.267(3) . ?
K1 C8 3.534(3) 1_565 ?
K1 K1 3.995(2) 5_556 ?
K1 Tb1 4.1658(10) 5_556 ?
S1 N1 1.634(3) . ?
S1 N2 1.637(4) . ?
S2 N3 1.624(3) . ?
S2 N4 1.629(3) . ?
O1 C3 1.249(4) . ?
O1 K1 2.673(2) 5_556 ?
O2 C3 1.267(4) . ?
O3 C4 1.271(4) . ?
O3 Tb1 2.358(2) 7_546 ?
O4 C4 1.223(4) . ?
O4 K1 2.723(3) 7_546 ?
O5 C7 1.243(4) . ?
O6 C7 1.254(4) . ?
O6 Tb1 2.377(2) 7_546 ?
O7 C8 1.261(4) . ?
O7 Tb1 2.397(2) 7_546 ?
O7 Tb1 2.612(2) 1_545 ?
O8 C8 1.252(4) . ?
O8 Tb1 2.512(2) 1_545 ?
O8 K1 2.812(2) 1_545 ?
O8 K1 2.957(2) 5_546 ?
O9 H9A 0.93(2) . ?
O9 H9B 0.93(2) . ?
N1 C1 1.321(4) . ?
N2 C2 1.310(5) . ?
N3 C5 1.329(4) . ?
N4 C6 1.324(4) . ?
N4 K1 3.065(3) 1_545 ?
C1 C2 1.431(4) . ?
C1 C3 1.498(4) . ?
C2 C4 1.516(5) . ?
C5 C6 1.435(5) . ?
C5 C7 1.524(4) . ?
C6 C8 1.505(4) . ?
C8 Tb1 2.921(3) 1_545 ?
C8 K1 3.534(3) 1_545 ?
O1W H1A 0.897(19) . ?
O1W H1B 0.901(19) . ?
O2W K1 3.1418(16) 2_556 ?
O2W H2 0.93(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Tb1 O6 73.50(8) 7_546 7_546 ?
O3 Tb1 O7 87.11(8) 7_546 7_546 ?
O6 Tb1 O7 69.75(8) 7_546 7_546 ?
O3 Tb1 O2 139.86(8) 7_546 . ?
O6 Tb1 O2 69.33(8) 7_546 . ?
O7 Tb1 O2 93.78(7) 7_546 . ?
O3 Tb1 O5 74.34(8) 7_546 . ?
O6 Tb1 O5 98.98(8) 7_546 . ?
O7 Tb1 O5 160.62(8) 7_546 . ?
O2 Tb1 O5 96.82(8) . . ?
O3 Tb1 O9 137.40(9) 7_546 . ?
O6 Tb1 O9 126.68(8) 7_546 . ?
O7 Tb1 O9 70.68(8) 7_546 . ?
O2 Tb1 O9 79.22(9) . . ?
O5 Tb1 O9 127.29(9) . . ?
O3 Tb1 O8 80.34(8) 7_546 1_565 ?
O6 Tb1 O8 153.65(8) 7_546 1_565 ?
O7 Tb1 O8 112.54(7) 7_546 1_565 ?
O2 Tb1 O8 134.43(8) . 1_565 ?
O5 Tb1 O8 70.42(7) . 1_565 ?
O9 Tb1 O8 75.79(9) . 1_565 ?
O3 Tb1 O1 143.48(8) 7_546 . ?
O6 Tb1 O1 117.10(8) 7_546 . ?
O7 Tb1 O1 129.34(8) 7_546 . ?
O2 Tb1 O1 52.47(7) . . ?
O5 Tb1 O1 69.56(8) . . ?
O9 Tb1 O1 66.95(8) . . ?
O8 Tb1 O1 82.63(7) 1_565 . ?
O3 Tb1 O7 68.37(8) 7_546 1_565 ?
O6 Tb1 O7 119.22(8) 7_546 1_565 ?
O7 Tb1 O7 62.94(8) 7_546 1_565 ?
O2 Tb1 O7 145.31(7) . 1_565 ?
O5 Tb1 O7 113.40(7) . 1_565 ?
O9 Tb1 O7 69.18(8) . 1_565 ?
O8 Tb1 O7 50.76(7) 1_565 1_565 ?
O1 Tb1 O7 121.90(7) . 1_565 ?
O3 Tb1 C3 148.95(8) 7_546 . ?
O6 Tb1 C3 92.60(9) 7_546 . ?
O7 Tb1 C3 114.49(8) 7_546 . ?
O2 Tb1 C3 26.44(8) . . ?
O5 Tb1 C3 80.86(8) . . ?
O9 Tb1 C3 73.10(9) . . ?
O8 Tb1 C3 108.74(8) 1_565 . ?
O1 Tb1 C3 26.17(8) . . ?
O7 Tb1 C3 140.49(8) 1_565 . ?
O3 Tb1 C8 71.83(9) 7_546 1_565 ?
O6 Tb1 C8 139.47(9) 7_546 1_565 ?
O7 Tb1 C8 88.10(8) 7_546 1_565 ?
O2 Tb1 C8 148.29(8) . 1_565 ?
O5 Tb1 C8 91.31(8) . 1_565 ?
O9 Tb1 C8 71.57(9) . 1_565 ?
O8 Tb1 C8 25.23(8) 1_565 1_565 ?
O1 Tb1 C8 103.26(8) . 1_565 ?
O7 Tb1 C8 25.57(8) 1_565 1_565 ?
C3 Tb1 C8 127.83(9) . 1_565 ?
O3 Tb1 K1 115.56(6) 7_546 5_556 ?
O6 Tb1 K1 149.64(6) 7_546 5_556 ?
O7 Tb1 K1 136.56(6) 7_546 5_556 ?
O2 Tb1 K1 90.75(5) . 5_556 ?
O5 Tb1 K1 59.62(6) . 5_556 ?
O9 Tb1 K1 67.84(7) . 5_556 ?
O8 Tb1 K1 44.52(5) 1_565 5_556 ?
O1 Tb1 K1 38.32(5) . 5_556 ?
O7 Tb1 K1 90.32(5) 1_565 5_556 ?
C3 Tb1 K1 64.49(7) . 5_556 ?
C8 Tb1 K1 67.20(6) 1_565 5_556 ?
O1 K1 O4 141.04(9) 5_556 7_546 ?
O1 K1 O8 114.15(7) 5_556 1_565 ?
O4 K1 O8 89.97(8) 7_546 1_565 ?
O1 K1 O5 151.93(8) 5_556 . ?
O4 K1 O5 66.49(8) 7_546 . ?
O8 K1 O5 59.62(6) 1_565 . ?
O1 K1 N3 116.59(8) 5_556 . ?
O4 K1 N3 74.96(10) 7_546 . ?
O8 K1 N3 114.63(7) 1_565 . ?
O5 K1 N3 55.99(7) . . ?
O1 K1 O8 73.19(7) 5_556 5_546 ?
O4 K1 O8 138.90(9) 7_546 5_546 ?
O8 K1 O8 92.37(6) 1_565 5_546 ?
O5 K1 O8 79.60(7) . 5_546 ?
N3 K1 O8 66.86(8) . 5_546 ?
O1 K1 N4 72.68(7) 5_556 1_565 ?
O4 K1 N4 100.14(10) 7_546 1_565 ?
O8 K1 N4 56.22(7) 1_565 1_565 ?
O5 K1 N4 114.24(7) . 1_565 ?
N3 K1 N4 170.09(8) . 1_565 ?
O8 K1 N4 115.02(8) 5_546 1_565 ?
O1 K1 O2W 74.81(6) 5_556 . ?
O4 K1 O2W 66.28(7) 7_546 . ?
O8 K1 O2W 123.76(9) 1_565 . ?
O5 K1 O2W 132.62(7) . . ?
N3 K1 O2W 107.31(11) . . ?
O8 K1 O2W 139.25(6) 5_546 . ?
N4 K1 O2W 77.83(11) 1_565 . ?
O1 K1 O1W 66.54(8) 5_556 . ?
O4 K1 O1W 88.56(9) 7_546 . ?
O8 K1 O1W 178.18(8) 1_565 . ?
O5 K1 O1W 120.64(8) . . ?
N3 K1 O1W 66.00(8) . . ?
O8 K1 O1W 89.44(7) 5_546 . ?
N4 K1 O1W 123.03(8) 1_565 . ?
O2W K1 O1W 54.59(9) . . ?
O1 K1 C8 110.18(7) 5_556 1_565 ?
O4 K1 C8 82.74(8) 7_546 1_565 ?
O8 K1 C8 18.66(7) 1_565 1_565 ?
O5 K1 C8 72.29(7) . 1_565 ?
N3 K1 C8 128.20(8) . 1_565 ?
O8 K1 C8 109.09(8) 5_546 1_565 ?
N4 K1 C8 41.96(7) 1_565 1_565 ?
O2W K1 C8 105.18(9) . 1_565 ?
O1W K1 C8 159.75(8) . 1_565 ?
O1 K1 K1 94.24(6) 5_556 5_556 ?
O4 K1 K1 123.87(7) 7_546 5_556 ?
O8 K1 K1 47.68(5) 1_565 5_556 ?
O5 K1 K1 60.69(5) . 5_556 ?
N3 K1 K1 90.14(6) . 5_556 ?
O8 K1 K1 44.69(5) 5_546 5_556 ?
N4 K1 K1 85.51(6) 1_565 5_556 ?
O2W K1 K1 162.14(9) . 5_556 ?
O1W K1 K1 134.13(7) . 5_556 ?
C8 K1 K1 64.86(6) 1_565 5_556 ?
O1 K1 Tb1 36.81(5) 5_556 5_556 ?
O4 K1 Tb1 165.24(7) 7_546 5_556 ?
O8 K1 Tb1 103.61(5) 1_565 5_556 ?
O5 K1 Tb1 115.39(6) . 5_556 ?
N3 K1 Tb1 93.84(6) . 5_556 ?
O8 K1 Tb1 36.56(4) 5_546 5_556 ?
N4 K1 Tb1 92.33(6) 1_565 5_556 ?
O2W K1 Tb1 109.29(2) . 5_556 ?
O1W K1 Tb1 77.96(6) . 5_556 ?
C8 K1 Tb1 111.94(6) 1_565 5_556 ?
K1 K1 Tb1 64.61(2) 5_556 5_556 ?
N1 S1 N2 98.54(16) . . ?
N3 S2 N4 98.65(15) . . ?
C3 O1 Tb1 88.1(2) . . ?
C3 O1 K1 167.0(2) . 5_556 ?
Tb1 O1 K1 104.87(8) . 5_556 ?
C3 O2 Tb1 96.04(18) . . ?
C4 O3 Tb1 142.9(2) . 7_546 ?
C4 O4 K1 126.2(2) . 7_546 ?
C7 O5 Tb1 120.8(2) . . ?
C7 O5 K1 126.8(2) . . ?
Tb1 O5 K1 110.84(8) . . ?
C7 O6 Tb1 134.6(2) . 7_546 ?
C8 O7 Tb1 149.9(2) . 7_546 ?
C8 O7 Tb1 91.05(18) . 1_545 ?
Tb1 O7 Tb1 117.06(8) 7_546 1_545 ?
C8 O8 Tb1 95.98(18) . 1_545 ?
C8 O8 K1 115.4(2) . 1_545 ?
Tb1 O8 K1 109.97(8) 1_545 1_545 ?
C8 O8 K1 146.2(2) . 5_546 ?
Tb1 O8 K1 98.92(7) 1_545 5_546 ?
K1 O8 K1 87.63(6) 1_545 5_546 ?
Tb1 O9 H9A 119(3) . . ?
Tb1 O9 H9B 129(3) . . ?
H9A O9 H9B 112(3) . . ?
C1 N1 S1 107.4(2) . . ?
C2 N2 S1 107.1(2) . . ?
C5 N3 S2 108.0(2) . . ?
C5 N3 K1 121.7(2) . . ?
S2 N3 K1 130.00(14) . . ?
C6 N4 S2 107.5(2) . . ?
C6 N4 K1 113.7(2) . 1_545 ?
S2 N4 K1 138.56(14) . 1_545 ?
N1 C1 C2 112.9(3) . . ?
N1 C1 C3 122.4(3) . . ?
C2 C1 C3 124.5(3) . . ?
N2 C2 C1 114.0(3) . . ?
N2 C2 C4 118.7(3) . . ?
C1 C2 C4 127.3(3) . . ?
O1 C3 O2 122.8(3) . . ?
O1 C3 C1 120.5(3) . . ?
O2 C3 C1 116.7(3) . . ?
O1 C3 Tb1 65.76(18) . . ?
O2 C3 Tb1 57.52(16) . . ?
C1 C3 Tb1 168.8(2) . . ?
O4 C4 O3 126.8(3) . . ?
O4 C4 C2 118.5(3) . . ?
O3 C4 C2 114.6(3) . . ?
N3 C5 C6 112.4(3) . . ?
N3 C5 C7 118.6(3) . . ?
C6 C5 C7 129.0(3) . . ?
N4 C6 C5 113.4(3) . . ?
N4 C6 C8 116.2(3) . . ?
C5 C6 C8 130.3(3) . . ?
O5 C7 O6 125.2(3) . . ?
O5 C7 C5 116.6(3) . . ?
O6 C7 C5 118.2(3) . . ?
O8 C8 O7 122.0(3) . . ?
O8 C8 C6 118.7(3) . . ?
O7 C8 C6 119.0(3) . . ?
O8 C8 Tb1 58.79(16) . 1_545 ?
O7 C8 Tb1 63.38(16) . 1_545 ?
C6 C8 Tb1 170.9(2) . 1_545 ?
O8 C8 K1 45.96(15) . 1_545 ?
O7 C8 K1 132.2(2) . 1_545 ?
C6 C8 K1 88.14(17) . 1_545 ?
Tb1 C8 K1 84.49(7) 1_545 1_545 ?
K1 O1W H1A 112.4(14) . . ?
K1 O1W H1B 110.4(14) . . ?
H1A O1W H1B 109(3) . . ?
K1 O2W K1 150.30(17) . 2_556 ?
K1 O2W H2 95(4) . . ?
K1 O2W H2 105(3) 2_556 . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O9 H9A O3 0.93(2) 1.88(2) 2.800(3) 170(5) 1_565
O9 H9B O1W 0.93(2) 1.90(2) 2.818(4) 172(5) 5_556
O1W H1A O4 0.897(19) 1.92(2) 2.769(4) 157(3) 8_446
O1W H1B O1W 0.901(19) 2.78(4) 3.364(7) 124(3) 2_556
O2W H2 N1 0.93(2) 2.05(2) 2.975(4) 172(5) 5_556

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.12
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.419
_refine_diff_density_min         -0.557
_refine_diff_density_rms         0.097


#===END
_database_code_depnum_ccdc_archive 'CCDC 957586'
#######################################################################
#
#                 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_compound9

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C16 H14 K2 La2 N4 O21 S2'
_chemical_formula_sum            'C16 H14 K2 La2 N4 O21 S2'
_chemical_formula_weight         1018.45

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'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   8.2691(6)
_cell_length_b                   10.3254(7)
_cell_length_c                   10.9614(12)
_cell_angle_alpha                102.7690(10)
_cell_angle_beta                 109.2740(10)
_cell_angle_gamma                111.5200(10)
_cell_volume                     756.93(11)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2667
_cell_measurement_theta_min      2.14
_cell_measurement_theta_max      25.10

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    2.234
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             490
_exptl_absorpt_coefficient_mu    3.292
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.4738
_exptl_absorpt_correction_T_max  0.6147
_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 9.00cm
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            3887
_diffrn_reflns_av_R_equivalents  0.0138
_diffrn_reflns_av_sigmaI/netI    0.0276
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.14
_diffrn_reflns_theta_max         25.10
_reflns_number_total             2667
_reflns_number_gt                2484
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXP-97
_computing_publication_material  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.Standard DFIX restraints were
used for the distance of the atoms, such as (o10 and h1a), (o10 and h1b),
(h1a and h1b), (o9 and h99), (o9 and h98), (h99 and h98). To improve the
 parameters chemical more reasonable, ultimately restrain instructions ISOR
 for (o11, o11') were applied in the refinement.
;

_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)+(0.0347P)²+0.7603P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    none
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2667
_refine_ls_number_parameters     240
_refine_ls_number_restraints     20
_refine_ls_R_factor_all          0.0261
_refine_ls_R_factor_gt           0.0234
_refine_ls_wR_factor_ref         0.0637
_refine_ls_wR_factor_gt          0.0622
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_restrained_S_all      1.089
_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
La1 La 0.32712(3) 1.11038(2) 1.06812(2) 0.01749(9) Uani 1 1 d . . .
K1 K 0.35519(15) 1.41867(11) 0.81638(11) 0.0343(2) Uani 1 1 d D . .
S1 S 0.81260(17) 1.41475(15) 0.73250(14) 0.0368(3) Uani 1 1 d . . .
O1 O 0.6493(5) 1.1351(3) 1.0073(3) 0.0328(7) Uani 1 1 d . . .
O2 O 0.5415(4) 1.2981(3) 0.9921(3) 0.0299(7) Uani 1 1 d . . .
O3 O 0.9617(4) 1.1090(3) 0.9620(3) 0.0273(6) Uani 1 1 d . . .
O4 O 1.2222(4) 1.3097(3) 1.0014(3) 0.0274(6) Uani 1 1 d . . .
O5 O 0.5185(4) 1.3698(3) 1.2828(3) 0.0328(7) Uani 1 1 d . . .
O6 O 0.2411(4) 1.2040(3) 1.2619(3) 0.0326(7) Uani 1 1 d . . .
O7 O 0.5322(5) 1.0873(4) 1.2681(3) 0.0415(8) Uani 1 1 d . . .
O8 O 0.7377(5) 1.0282(4) 1.3971(4) 0.0445(9) Uani 1 1 d . . .
O9 O 0.1397(5) 0.9886(4) 0.8046(3) 0.0359(8) Uani 1 1 d D . .
N1 N 0.6715(5) 1.3558(4) 0.8035(4) 0.0288(8) Uani 1 1 d . . .
N2 N 0.9735(5) 1.3650(4) 0.8047(4) 0.0308(8) Uani 1 1 d . . .
C1 C 0.7431(6) 1.2922(4) 0.8847(4) 0.0213(8) Uani 1 1 d . . .
C2 C 0.9169(6) 1.2964(4) 0.8835(4) 0.0212(8) Uani 1 1 d . . .
C3 C 0.6397(5) 1.2373(4) 0.9674(4) 0.0209(8) Uani 1 1 d . . .
C4 C 1.0422(6) 1.2351(4) 0.9564(4) 0.0215(8) Uani 1 1 d . . .
C5 C 0.4236(6) 1.4331(5) 1.4617(4) 0.0277(9) Uani 1 1 d . . .
H5 H 0.3293 1.4005 1.4924 0.080 Uiso 1 1 calc . . .
C6 C 0.3942(6) 1.3312(5) 1.3279(4) 0.0260(9) Uani 1 1 d . . .
C7 C 0.4801(6) 1.0239(5) 1.4495(5) 0.0298(10) Uani 1 1 d . . .
H7 H 0.3754 1.0438 1.4273 0.080 Uiso 1 1 calc . . .
C8 C 0.5924(6) 1.0483(5) 1.3674(4) 0.0272(9) Uani 1 1 d . . .
O10 O 0.1505(6) 1.1967(5) 0.5676(5) 0.0719(13) Uani 1 1 d D . .
O11 O 1.0955(17) 1.6204(15) 1.6611(13) 0.039(3) Uani 0.30 1 d PU . .
O11' O 1.083(3) 1.562(2) 1.620(2) 0.045(5) Uani 0.20 1 d PU . .
H1A H 0.029(4) 1.200(4) 0.532(3) 0.080 Uiso 1 1 d D . .
H1B H 0.128(7) 1.109(2) 0.588(3) 0.080 Uiso 1 1 d D . .
H99 H 0.184(5) 0.978(5) 0.745(3) 0.035(13) Uiso 1 1 d D . .
H98 H 0.025(3) 0.919(4) 0.772(4) 0.032(13) Uiso 1 1 d 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
La1 O7 2.411(3) . ?
La1 O3 2.475(3) 2_677 ?
La1 O9 2.517(3) . ?
La1 O6 2.559(3) . ?
La1 O1 2.586(3) 2_677 ?
La1 O2 2.600(3) . ?
La1 O5 2.620(3) . ?
La1 O4 2.661(3) 1_455 ?
La1 O3 2.851(3) 1_455 ?
La1 O1 2.890(3) . ?
La1 C6 2.963(4) . ?
La1 C3 3.107(4) . ?
K1 O10 2.627(5) . ?
K1 O5 2.677(3) 2_687 ?
K1 O2 2.821(3) 2_687 ?
K1 O2 2.854(3) . ?
K1 O4 2.857(3) 1_455 ?
K1 N2 2.950(4) 1_455 ?
K1 N1 2.955(4) . ?
K1 O4 3.129(3) 2_787 ?
K1 K1 3.529(2) 2_687 ?
K1 La1 4.2263(11) 2_687 ?
K1 H1A 3.00(2) . ?
K1 H1B 2.99(2) . ?
S1 N1 1.620(4) . ?
S1 N2 1.627(4) . ?
O1 C3 1.247(5) . ?
O1 La1 2.586(3) 2_677 ?
O2 C3 1.253(5) . ?
O2 K1 2.821(3) 2_687 ?
O3 C4 1.253(5) . ?
O3 La1 2.475(3) 2_677 ?
O3 La1 2.851(3) 1_655 ?
O4 C4 1.248(5) . ?
O4 La1 2.661(3) 1_655 ?
O4 K1 2.857(3) 1_655 ?
O4 K1 3.129(3) 2_787 ?
O5 C6 1.258(5) . ?
O5 K1 2.677(3) 2_687 ?
O6 C6 1.268(5) . ?
O7 C8 1.256(5) . ?
O8 C8 1.244(5) . ?
O9 H99 0.852(10) . ?
O9 H98 0.842(10) . ?
N1 C1 1.329(5) . ?
N2 C2 1.327(5) . ?
N2 K1 2.950(4) 1_655 ?
C1 C2 1.426(5) . ?
C1 C3 1.503(5) . ?
C2 C4 1.506(5) . ?
C4 La1 3.119(4) 1_655 ?
C5 C5 1.309(9) 2_688 ?
C5 C6 1.487(6) . ?
C5 H5 0.9300 . ?
C7 C7 1.303(9) 2_678 ?
C7 C8 1.488(6) . ?
C7 H7 0.9300 . ?
O10 H1A 0.972(19) . ?
O10 H1B 0.950(19) . ?
O11 O11' 0.62(2) . ?

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 La1 O3 90.38(11) . 2_677 ?
O7 La1 O9 142.58(12) . . ?
O3 La1 O9 79.55(10) 2_677 . ?
O7 La1 O6 75.68(11) . . ?
O3 La1 O6 73.54(9) 2_677 . ?
O9 La1 O6 133.22(10) . . ?
O7 La1 O1 69.12(11) . 2_677 ?
O3 La1 O1 69.31(9) 2_677 2_677 ?
O9 La1 O1 73.62(11) . 2_677 ?
O6 La1 O1 127.62(10) . 2_677 ?
O7 La1 O2 109.88(11) . . ?
O3 La1 O2 156.87(10) 2_677 . ?
O9 La1 O2 77.55(10) . . ?
O6 La1 O2 121.25(9) . . ?
O1 La1 O2 106.79(9) 2_677 . ?
O7 La1 O5 71.15(11) . . ?
O3 La1 O5 123.33(9) 2_677 . ?
O9 La1 O5 143.32(11) . . ?
O6 La1 O5 50.30(9) . . ?
O1 La1 O5 138.30(11) 2_677 . ?
O2 La1 O5 75.43(9) . . ?
O7 La1 O4 140.08(11) . 1_455 ?
O3 La1 O4 109.10(9) 2_677 1_455 ?
O9 La1 O4 76.63(11) . 1_455 ?
O6 La1 O4 77.06(10) . 1_455 ?
O1 La1 O4 149.98(10) 2_677 1_455 ?
O2 La1 O4 62.27(9) . 1_455 ?
O5 La1 O4 69.02(10) . 1_455 ?
O7 La1 O3 138.45(10) . 1_455 ?
O3 La1 O3 62.31(10) 2_677 1_455 ?
O9 La1 O3 66.58(10) . 1_455 ?
O6 La1 O3 67.13(9) . 1_455 ?
O1 La1 O3 121.07(9) 2_677 1_455 ?
O2 La1 O3 104.95(8) . 1_455 ?
O5 La1 O3 97.15(9) . 1_455 ?
O4 La1 O3 46.87(8) 1_455 1_455 ?
O7 La1 O1 78.78(10) . . ?
O3 La1 O1 132.50(9) 2_677 . ?
O9 La1 O1 81.90(10) . . ?
O6 La1 O1 143.49(10) . . ?
O1 La1 O1 63.58(10) 2_677 . ?
O2 La1 O1 46.56(8) . . ?
O5 La1 O1 96.77(9) . . ?
O4 La1 O1 108.44(8) 1_455 . ?
O3 La1 O1 142.77(8) 1_455 . ?
O7 La1 C6 71.04(12) . . ?
O3 La1 C6 98.43(11) 2_677 . ?
O9 La1 C6 145.79(11) . . ?
O6 La1 C6 25.21(10) . . ?
O1 La1 C6 138.00(10) 2_677 . ?
O2 La1 C6 98.67(11) . . ?
O5 La1 C6 25.10(10) . . ?
O4 La1 C6 71.82(10) 1_455 . ?
O3 La1 C6 82.11(10) 1_455 . ?
O1 La1 C6 120.34(11) . . ?
O7 La1 C3 96.78(11) . . ?
O3 La1 C3 148.09(10) 2_677 . ?
O9 La1 C3 75.93(10) . . ?
O6 La1 C3 138.36(10) . . ?
O1 La1 C3 84.28(10) 2_677 . ?
O2 La1 C3 23.25(9) . . ?
O5 La1 C3 88.27(10) . . ?
O4 La1 C3 84.79(9) 1_455 . ?
O3 La1 C3 123.23(9) 1_455 . ?
O1 La1 C3 23.64(9) . . ?
C6 La1 C3 113.33(11) . . ?
O10 K1 O5 93.88(13) . 2_687 ?
O10 K1 O2 152.48(13) . 2_687 ?
O5 K1 O2 70.94(9) 2_687 2_687 ?
O10 K1 O2 103.87(13) . . ?
O5 K1 O2 133.95(10) 2_687 . ?
O2 K1 O2 103.09(8) 2_687 . ?
O10 K1 O4 107.23(13) . 1_455 ?
O5 K1 O4 153.43(10) 2_687 1_455 ?
O2 K1 O4 83.15(9) 2_687 1_455 ?
O2 K1 O4 56.90(8) . 1_455 ?
O10 K1 N2 85.17(14) . 1_455 ?
O5 K1 N2 110.64(10) 2_687 1_455 ?
O2 K1 N2 79.36(10) 2_687 1_455 ?
O2 K1 N2 112.90(9) . 1_455 ?
O4 K1 N2 57.00(9) 1_455 1_455 ?
O10 K1 N1 82.19(13) . . ?
O5 K1 N1 86.25(10) 2_687 . ?
O2 K1 N1 118.23(10) 2_687 . ?
O2 K1 N1 55.51(9) . . ?
O4 K1 N1 111.99(9) 1_455 . ?
N2 K1 N1 159.57(11) 1_455 . ?
O10 K1 O4 138.39(13) . 2_787 ?
O5 K1 O4 61.45(9) 2_687 2_787 ?
O2 K1 O4 54.11(8) 2_687 2_787 ?
O2 K1 O4 77.92(8) . 2_787 ?
O4 K1 O4 107.91(7) 1_455 2_787 ?
N2 K1 O4 133.29(10) 1_455 2_787 ?
N1 K1 O4 64.42(9) . 2_787 ?
O10 K1 K1 154.52(12) . 2_687 ?
O5 K1 K1 107.47(8) 2_687 2_687 ?
O2 K1 K1 51.96(7) 2_687 2_687 ?
O2 K1 K1 51.13(7) . 2_687 ?
O4 K1 K1 57.53(7) 1_455 2_687 ?
N2 K1 K1 99.62(8) 1_455 2_687 ?
N1 K1 K1 85.43(8) . 2_687 ?
O4 K1 K1 50.37(6) 2_787 2_687 ?
O10 K1 La1 130.24(11) . 2_687 ?
O5 K1 La1 36.60(6) 2_687 2_687 ?
O2 K1 La1 36.94(6) 2_687 2_687 ?
O2 K1 La1 115.30(7) . 2_687 ?
O4 K1 La1 119.31(7) 1_455 2_687 ?
N2 K1 La1 105.16(8) 1_455 2_687 ?
N1 K1 La1 95.25(7) . 2_687 ?
O4 K1 La1 38.94(5) 2_787 2_687 ?
K1 K1 La1 72.94(3) 2_687 2_687 ?
O10 K1 H1A 18.4(5) . . ?
O5 K1 H1A 91.8(10) 2_687 . ?
O2 K1 H1A 135.6(5) 2_687 . ?
O2 K1 H1A 117.3(8) . . ?
O4 K1 H1A 103.1(11) 1_455 . ?
N2 K1 H1A 68.8(7) 1_455 . ?
N1 K1 H1A 100.3(6) . . ?
O4 K1 H1A 148.7(10) 2_787 . ?
K1 K1 H1A 160.3(11) 2_687 . ?
La1 K1 H1A 124.6(9) 2_687 . ?
O10 K1 H1B 18.0(5) . . ?
O5 K1 H1B 111.0(6) 2_687 . ?
O2 K1 H1B 163.0(10) 2_687 . ?
O2 K1 H1B 87.6(6) . . ?
O4 K1 H1B 92.0(8) 1_455 . ?
N2 K1 H1B 84.4(11) 1_455 . ?
N1 K1 H1B 78.7(10) . . ?
O4 K1 H1B 142.3(11) 2_787 . ?
K1 K1 H1B 137.0(5) 2_687 . ?
La1 K1 H1B 147.6(6) 2_687 . ?
H1A K1 H1B 30.2(4) . . ?
N1 S1 N2 98.48(18) . . ?
C3 O1 La1 141.5(3) . 2_677 ?
C3 O1 La1 88.0(2) . . ?
La1 O1 La1 116.42(10) 2_677 . ?
C3 O2 La1 101.7(2) . . ?
C3 O2 K1 132.8(3) . 2_687 ?
La1 O2 K1 102.37(10) . 2_687 ?
C3 O2 K1 125.0(3) . . ?
La1 O2 K1 116.67(10) . . ?
K1 O2 K1 76.91(8) 2_687 . ?
C4 O3 La1 152.0(3) . 2_677 ?
C4 O3 La1 90.3(2) . 1_655 ?
La1 O3 La1 117.69(10) 2_677 1_655 ?
C4 O4 La1 99.5(2) . 1_655 ?
C4 O4 K1 117.0(2) . 1_655 ?
La1 O4 K1 114.57(10) 1_655 1_655 ?
C4 O4 K1 158.4(3) . 2_787 ?
La1 O4 K1 93.40(8) 1_655 2_787 ?
K1 O4 K1 72.09(7) 1_655 2_787 ?
C6 O5 La1 92.9(2) . . ?
C6 O5 K1 134.9(3) . 2_687 ?
La1 O5 K1 105.85(10) . 2_687 ?
C6 O6 La1 95.5(2) . . ?
C8 O7 La1 163.5(3) . . ?
La1 O9 H99 128(3) . . ?
La1 O9 H98 116(3) . . ?
H99 O9 H98 110.2(18) . . ?
C1 N1 S1 108.3(3) . . ?
C1 N1 K1 120.4(3) . . ?
S1 N1 K1 130.22(17) . . ?
C2 N2 S1 107.4(3) . . ?
C2 N2 K1 117.5(3) . 1_655 ?
S1 N2 K1 134.76(18) . 1_655 ?
N1 C1 C2 112.2(3) . . ?
N1 C1 C3 117.0(3) . . ?
C2 C1 C3 130.7(3) . . ?
N2 C2 C1 113.5(3) . . ?
N2 C2 C4 116.4(3) . . ?
C1 C2 C4 130.1(3) . . ?
O1 C3 O2 122.0(4) . . ?
O1 C3 C1 121.5(3) . . ?
O2 C3 C1 116.5(3) . . ?
O1 C3 La1 68.4(2) . . ?
O2 C3 La1 55.01(19) . . ?
C1 C3 La1 164.2(3) . . ?
O4 C4 O3 123.1(4) . . ?
O4 C4 C2 117.7(3) . . ?
O3 C4 C2 119.1(4) . . ?
O4 C4 La1 57.3(2) . 1_655 ?
O3 C4 La1 66.0(2) . 1_655 ?
C2 C4 La1 170.1(3) . 1_655 ?
C5 C5 C6 122.9(5) 2_688 . ?
C5 C5 H5 118.5 2_688 . ?
C6 C5 H5 118.5 . . ?
O5 C6 O6 121.2(4) . . ?
O5 C6 C5 120.9(4) . . ?
O6 C6 C5 117.9(4) . . ?
O5 C6 La1 62.0(2) . . ?
O6 C6 La1 59.3(2) . . ?
C5 C6 La1 175.9(3) . . ?
C7 C7 C8 123.8(5) 2_678 . ?
C7 C7 H7 118.1 2_678 . ?
C8 C7 H7 118.1 . . ?
O8 C8 O7 122.8(4) . . ?
O8 C8 C7 120.0(4) . . ?
O7 C8 C7 117.2(4) . . ?
K1 O10 H1A 102.8(15) . . ?
K1 O10 H1B 103.4(16) . . ?
H1A O10 H1B 109(3) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O10 H1A O8 0.972(19) 2.12(3) 2.858(6) 132(3) 1_454
O10 H1B O8 0.950(19) 2.10(4) 2.851(6) 135(5) 2_677

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        25.10
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         0.962
_refine_diff_density_min         -0.472
_refine_diff_density_rms         0.105
_database_code_depnum_ccdc_archive 'CCDC 957587'
#######################################################################
#
#                 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_compound10

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C16 H14 Ce2 K2 N4 O21 S2'
_chemical_formula_sum            'C16 H14 Ce2 K2 N4 O21 S2'
_chemical_formula_weight         1020.87

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'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   8.2471(12)
_cell_length_b                   10.2753(14)
_cell_length_c                   10.915(2)
_cell_angle_alpha                102.534(3)
_cell_angle_beta                 109.195(3)
_cell_angle_gamma                112.160(2)
_cell_volume                     744.9(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2690
_cell_measurement_theta_min      2.15
_cell_measurement_theta_max      25.36

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    2.276
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             492
_exptl_absorpt_coefficient_mu    3.533
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.4738
_exptl_absorpt_correction_T_max  0.6147
_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 9.00cm
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            3910
_diffrn_reflns_av_R_equivalents  0.0271
_diffrn_reflns_av_sigmaI/netI    0.0582
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.15
_diffrn_reflns_theta_max         25.36
_reflns_number_total             2690
_reflns_number_gt                2378
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXP-97
_computing_publication_material  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. Standard DFIX restraints were
used for the distance of the atoms, such as (o10 and h1a), (o10 and h1b),
(h1a and h1b), (o9 and h99), (o9 and h98), (h99 and h98). To improve the
 parameters chemical more reasonable, ultimately restrain instructions ISOR
 for (o11) were applied in the refinement.
;

_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)+(0.0357P)²+0.9104P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    none
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2690
_refine_ls_number_parameters     229
_refine_ls_number_restraints     14
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0384
_refine_ls_wR_factor_ref         0.0852
_refine_ls_wR_factor_gt          0.0814
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_restrained_S_all      1.046
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ce1 Ce 0.32934(5) 1.11102(4) 1.06928(4) 0.01783(12) Uani 1 1 d . . .
K1 K 0.3591(2) 1.41561(18) 0.81665(17) 0.0342(4) Uani 1 1 d D . .
S1 S 0.8171(3) 1.4152(2) 0.7327(2) 0.0350(4) Uani 1 1 d . . .
O1 O 0.6540(7) 1.1363(5) 1.0105(5) 0.0332(11) Uani 1 1 d . . .
O2 O 0.5449(6) 1.2977(5) 0.9941(5) 0.0299(11) Uani 1 1 d . . .
O3 O 0.9608(6) 1.1078(5) 0.9609(5) 0.0262(10) Uani 1 1 d . . .
O4 O 1.2259(6) 1.3097(5) 1.0027(5) 0.0257(10) Uani 1 1 d . . .
O5 O 0.5232(6) 1.3693(5) 1.2839(5) 0.0303(11) Uani 1 1 d . . .
O6 O 0.2410(6) 1.2011(5) 1.2596(5) 0.0292(11) Uani 1 1 d . . .
O7 O 0.5284(7) 1.0838(6) 1.2646(5) 0.0402(13) Uani 1 1 d . . .
O8 O 0.7350(7) 1.0256(7) 1.3941(5) 0.0445(14) Uani 1 1 d . . .
O9 O 0.1423(7) 0.9937(6) 0.8076(5) 0.0338(11) Uani 1 1 d D . .
N1 N 0.6770(7) 1.3578(6) 0.8067(6) 0.0279(13) Uani 1 1 d . . .
N2 N 0.9783(7) 1.3659(6) 0.8051(6) 0.0292(13) Uani 1 1 d . . .
C1 C 0.7479(8) 1.2926(7) 0.8850(7) 0.0200(13) Uani 1 1 d . . .
C2 C 0.9210(8) 1.2973(7) 0.8843(7) 0.0201(13) Uani 1 1 d . . .
C3 C 0.6425(8) 1.2380(6) 0.9692(7) 0.0213(14) Uani 1 1 d . . .
C4 C 1.0448(9) 1.2348(7) 0.9563(6) 0.0198(13) Uani 1 1 d . . .
C5 C 0.4221(9) 1.4310(7) 1.4609(7) 0.0253(14) Uani 1 1 d . . .
H5 H 0.3263 1.3965 1.4908 0.080 Uiso 1 1 calc . . .
C6 C 0.3956(9) 1.3294(7) 1.3273(7) 0.0236(14) Uani 1 1 d . . .
C7 C 0.4805(10) 1.0236(8) 1.4484(7) 0.0296(15) Uani 1 1 d . . .
H7 H 0.3761 1.0440 1.4265 0.080 Uiso 1 1 calc . . .
C8 C 0.5896(10) 1.0469(8) 1.3641(7) 0.0278(15) Uani 1 1 d . . .
O10 O 0.1512(10) 1.1959(7) 0.5687(8) 0.076(2) Uani 1 1 d D . .
O11 O 1.087(3) 1.599(2) 1.639(2) 0.128(6) Uani 0.50 1 d PU . .
H1A H 0.041(6) 1.213(5) 0.523(4) 0.080 Uiso 1 1 d D . .
H1B H 0.097(9) 1.105(2) 0.584(3) 0.080 Uiso 1 1 d D . .
H99 H 0.190(10) 0.990(9) 0.749(6) 0.080 Uiso 1 1 d D . .
H98 H 0.036(7) 0.912(5) 0.776(8) 0.080 Uiso 1 1 d 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
Ce1 O7 2.371(4) . ?
Ce1 O3 2.448(4) 2_677 ?
Ce1 O9 2.489(5) . ?
Ce1 O6 2.524(4) . ?
Ce1 O2 2.566(4) . ?
Ce1 O1 2.573(4) 2_677 ?
Ce1 O5 2.593(4) . ?
Ce1 O4 2.640(4) 1_455 ?
Ce1 O3 2.860(4) 1_455 ?
Ce1 O1 2.886(4) . ?
Ce1 C6 2.930(6) . ?
Ce1 C3 3.082(6) . ?
K1 O10 2.596(7) . ?
K1 O5 2.677(5) 2_687 ?
K1 O2 2.835(5) . ?
K1 O4 2.835(5) 1_455 ?
K1 O2 2.845(5) 2_687 ?
K1 N1 2.928(5) . ?
K1 N2 2.940(5) 1_455 ?
K1 O4 3.071(5) 2_787 ?
K1 K1 3.501(3) 2_687 ?
K1 Ce1 4.2012(17) 2_687 ?
K1 H1A 2.99(2) . ?
K1 H1B 3.00(2) . ?
S1 N2 1.625(5) . ?
S1 N1 1.625(6) . ?
O1 C3 1.246(7) . ?
O1 Ce1 2.573(4) 2_677 ?
O2 C3 1.242(7) . ?
O2 K1 2.845(5) 2_687 ?
O3 C4 1.246(7) . ?
O3 Ce1 2.448(4) 2_677 ?
O3 Ce1 2.860(4) 1_655 ?
O4 C4 1.244(7) . ?
O4 Ce1 2.640(4) 1_655 ?
O4 K1 2.835(5) 1_655 ?
O4 K1 3.071(4) 2_787 ?
O5 C6 1.259(8) . ?
O5 K1 2.677(5) 2_687 ?
O6 C6 1.265(8) . ?
O7 C8 1.241(8) . ?
O8 C8 1.250(7) . ?
O9 H99 0.851(10) . ?
O9 H98 0.848(10) . ?
N1 C1 1.318(7) . ?
N2 C2 1.323(8) . ?
N2 K1 2.940(5) 1_655 ?
C1 C2 1.412(8) . ?
C1 C3 1.516(8) . ?
C2 C4 1.503(8) . ?
C5 C5 1.330(13) 2_688 ?
C5 C6 1.490(9) . ?
C5 H5 0.9300 . ?
C7 C7 1.313(13) 2_678 ?
C7 C8 1.480(9) . ?
C7 H7 0.9300 . ?
O10 H1A 0.99(2) . ?
O10 H1B 0.95(2) . ?

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 Ce1 O3 89.87(17) . 2_677 ?
O7 Ce1 O9 142.68(17) . . ?
O3 Ce1 O9 80.06(16) 2_677 . ?
O7 Ce1 O6 76.36(16) . . ?
O3 Ce1 O6 72.78(14) 2_677 . ?
O9 Ce1 O6 132.33(15) . . ?
O7 Ce1 O2 110.27(16) . . ?
O3 Ce1 O2 156.84(15) 2_677 . ?
O9 Ce1 O2 76.96(16) . . ?
O6 Ce1 O2 121.96(14) . . ?
O7 Ce1 O1 69.20(17) . 2_677 ?
O3 Ce1 O1 69.36(14) 2_677 2_677 ?
O9 Ce1 O1 73.63(16) . 2_677 ?
O6 Ce1 O1 127.90(14) . 2_677 ?
O2 Ce1 O1 106.33(13) . 2_677 ?
O7 Ce1 O5 71.70(17) . . ?
O3 Ce1 O5 123.08(14) 2_677 . ?
O9 Ce1 O5 142.73(16) . . ?
O6 Ce1 O5 50.86(14) . . ?
O2 Ce1 O5 75.78(14) . . ?
O1 Ce1 O5 138.86(15) 2_677 . ?
O7 Ce1 O4 141.10(17) . 1_455 ?
O3 Ce1 O4 108.62(13) 2_677 1_455 ?
O9 Ce1 O4 75.58(15) . 1_455 ?
O6 Ce1 O4 77.04(14) . 1_455 ?
O2 Ce1 O4 62.74(13) . 1_455 ?
O1 Ce1 O4 149.01(15) 2_677 1_455 ?
O5 Ce1 O4 69.53(14) . 1_455 ?
O7 Ce1 O3 138.63(15) . 1_455 ?
O3 Ce1 O3 61.97(15) 2_677 1_455 ?
O9 Ce1 O3 65.77(14) . 1_455 ?
O6 Ce1 O3 66.98(14) . 1_455 ?
O2 Ce1 O3 105.15(13) . 1_455 ?
O1 Ce1 O3 120.11(14) 2_677 1_455 ?
O5 Ce1 O3 97.70(13) . 1_455 ?
O4 Ce1 O3 46.75(12) 1_455 1_455 ?
O7 Ce1 O1 78.32(15) . . ?
O3 Ce1 O1 132.64(13) 2_677 . ?
O9 Ce1 O1 82.47(15) . . ?
O6 Ce1 O1 143.79(14) . . ?
O2 Ce1 O1 46.61(12) . . ?
O1 Ce1 O1 63.53(16) 2_677 . ?
O5 Ce1 O1 96.58(14) . . ?
O4 Ce1 O1 108.99(12) 1_455 . ?
O3 Ce1 O1 143.02(13) 1_455 . ?
O7 Ce1 C6 71.79(17) . . ?
O3 Ce1 C6 97.88(17) 2_677 . ?
O9 Ce1 C6 144.91(16) . . ?
O6 Ce1 C6 25.44(15) . . ?
O2 Ce1 C6 99.23(17) . . ?
O1 Ce1 C6 138.73(16) 2_677 . ?
O5 Ce1 C6 25.43(15) . . ?
O4 Ce1 C6 71.95(15) 1_455 . ?
O3 Ce1 C6 82.21(15) 1_455 . ?
O1 Ce1 C6 120.50(16) . . ?
O7 Ce1 C3 96.92(17) . . ?
O3 Ce1 C3 148.11(15) 2_677 . ?
O9 Ce1 C3 75.72(16) . . ?
O6 Ce1 C3 139.10(15) . . ?
O2 Ce1 C3 23.17(13) . . ?
O1 Ce1 C3 83.98(15) 2_677 . ?
O5 Ce1 C3 88.49(15) . . ?
O4 Ce1 C3 85.17(14) 1_455 . ?
O3 Ce1 C3 123.25(14) 1_455 . ?
O1 Ce1 C3 23.82(13) . . ?
C6 Ce1 C3 113.86(17) . . ?
O10 K1 O5 93.48(19) . 2_687 ?
O10 K1 O2 105.11(19) . . ?
O5 K1 O2 135.70(15) 2_687 . ?
O10 K1 O4 107.99(19) . 1_455 ?
O5 K1 O4 151.41(14) 2_687 1_455 ?
O2 K1 O4 57.11(12) . 1_455 ?
O10 K1 O2 150.19(19) . 2_687 ?
O5 K1 O2 69.95(13) 2_687 2_687 ?
O2 K1 O2 103.90(12) . 2_687 ?
O4 K1 O2 82.38(13) 1_455 2_687 ?
O10 K1 N1 83.5(2) . . ?
O5 K1 N1 87.98(15) 2_687 . ?
O2 K1 N1 55.72(14) . . ?
O4 K1 N1 112.50(14) 1_455 . ?
O2 K1 N1 119.10(15) 2_687 . ?
O10 K1 N2 85.2(2) . 1_455 ?
O5 K1 N2 107.67(15) 2_687 1_455 ?
O2 K1 N2 113.59(14) . 1_455 ?
O4 K1 N2 57.38(13) 1_455 1_455 ?
O2 K1 N2 77.11(14) 2_687 1_455 ?
N1 K1 N2 161.19(16) . 1_455 ?
O10 K1 O4 139.43(19) . 2_787 ?
O5 K1 O4 62.12(13) 2_687 2_787 ?
O2 K1 O4 78.50(13) . 2_787 ?
O4 K1 O4 107.41(11) 1_455 2_787 ?
O2 K1 O4 54.38(12) 2_687 2_787 ?
N1 K1 O4 64.99(14) . 2_787 ?
N2 K1 O4 131.35(15) 1_455 2_787 ?
O10 K1 K1 156.39(18) . 2_687 ?
O5 K1 K1 107.51(12) 2_687 2_687 ?
O2 K1 K1 52.08(10) . 2_687 ?
O4 K1 K1 56.81(10) 1_455 2_687 ?
O2 K1 K1 51.82(10) 2_687 2_687 ?
N1 K1 K1 86.51(13) . 2_687 ?
N2 K1 K1 98.21(13) 1_455 2_687 ?
O4 K1 K1 50.60(9) 2_787 2_687 ?
O10 K1 Ce1 129.71(17) . 2_687 ?
O5 K1 Ce1 36.45(9) 2_687 2_687 ?
O2 K1 Ce1 115.68(11) . 2_687 ?
O4 K1 Ce1 118.23(10) 1_455 2_687 ?
O2 K1 Ce1 36.72(9) 2_687 2_687 ?
N1 K1 Ce1 95.73(11) . 2_687 ?
N2 K1 Ce1 103.06(11) 1_455 2_687 ?
O4 K1 Ce1 38.80(8) 2_787 2_687 ?
K1 K1 Ce1 72.51(5) 2_687 2_687 ?
O10 K1 Ce1 96.56(17) . . ?
O5 K1 Ce1 164.96(11) 2_687 . ?
O2 K1 Ce1 30.06(9) . . ?
O4 K1 Ce1 31.74(8) 1_455 . ?
O2 K1 Ce1 105.20(10) 2_687 . ?
N1 K1 Ce1 82.08(11) . . ?
N2 K1 Ce1 84.38(11) 1_455 . ?
O4 K1 Ce1 103.25(9) 2_787 . ?
K1 K1 Ce1 60.81(4) 2_687 . ?
Ce1 K1 Ce1 133.32(4) 2_687 . ?
O10 K1 H1A 18.7(5) . . ?
O5 K1 H1A 86.8(13) 2_687 . ?
O2 K1 H1A 121.2(8) . . ?
O4 K1 H1A 107.5(15) 1_455 . ?
O2 K1 H1A 131.9(5) 2_687 . ?
N1 K1 H1A 100.7(8) . . ?
N2 K1 H1A 70.7(11) 1_455 . ?
O4 K1 H1A 145.1(15) 2_787 . ?
K1 K1 H1A 164.3(15) 2_687 . ?
Ce1 K1 H1A 120.0(11) 2_687 . ?
Ce1 K1 H1A 106.0(13) . . ?
O10 K1 H1B 17.8(5) . . ?
O5 K1 H1B 111.3(6) 2_687 . ?
O2 K1 H1B 91.1(9) . . ?
O4 K1 H1B 91.3(8) 1_455 . ?
O2 K1 H1B 156.6(14) 2_687 . ?
N1 K1 H1B 84.1(14) . . ?
N2 K1 H1B 80.5(14) 1_455 . ?
O4 K1 H1B 148.0(14) 2_787 . ?
K1 K1 H1B 139.6(6) 2_687 . ?
Ce1 K1 H1B 147.5(5) 2_687 . ?
Ce1 K1 H1B 79.0(5) . . ?
H1A K1 H1B 30.1(4) . . ?
N2 S1 N1 98.4(3) . . ?
C3 O1 Ce1 140.6(4) . 2_677 ?
C3 O1 Ce1 87.0(4) . . ?
Ce1 O1 Ce1 116.47(16) 2_677 . ?
C3 O2 Ce1 102.4(4) . . ?
C3 O2 K1 124.3(4) . . ?
Ce1 O2 K1 116.32(15) . . ?
C3 O2 K1 134.4(4) . 2_687 ?
Ce1 O2 K1 101.75(15) . 2_687 ?
K1 O2 K1 76.10(12) . 2_687 ?
C4 O3 Ce1 152.4(4) . 2_677 ?
C4 O3 Ce1 89.5(3) . 1_655 ?
Ce1 O3 Ce1 118.03(15) 2_677 1_655 ?
C4 O4 Ce1 100.1(3) . 1_655 ?
C4 O4 K1 116.1(4) . 1_655 ?
Ce1 O4 K1 113.87(15) 1_655 1_655 ?
C4 O4 K1 157.3(4) . 2_787 ?
Ce1 O4 K1 94.42(12) 1_655 2_787 ?
K1 O4 K1 72.59(11) 1_655 2_787 ?
C6 O5 Ce1 92.4(4) . . ?
C6 O5 K1 132.5(4) . 2_687 ?
Ce1 O5 K1 105.72(16) . 2_687 ?
C6 O6 Ce1 95.5(4) . . ?
C8 O7 Ce1 164.8(5) . . ?
Ce1 O9 H99 127(5) . . ?
Ce1 O9 H98 114(5) . . ?
H99 O9 H98 109.6(19) . . ?
C1 N1 S1 107.5(4) . . ?
C1 N1 K1 121.4(4) . . ?
S1 N1 K1 130.5(3) . . ?
C2 N2 S1 107.2(4) . . ?
C2 N2 K1 116.9(4) . 1_655 ?
S1 N2 K1 135.7(3) . 1_655 ?
N1 C1 C2 113.3(5) . . ?
N1 C1 C3 115.6(5) . . ?
C2 C1 C3 130.8(5) . . ?
N2 C2 C1 113.4(5) . . ?
N2 C2 C4 116.3(5) . . ?
C1 C2 C4 130.3(5) . . ?
O2 C3 O1 122.0(6) . . ?
O2 C3 C1 117.4(5) . . ?
O1 C3 C1 120.5(5) . . ?
O2 C3 Ce1 54.4(3) . . ?
O1 C3 Ce1 69.2(3) . . ?
C1 C3 Ce1 164.1(4) . . ?
O4 C4 O3 123.3(5) . . ?
O4 C4 C2 118.0(5) . . ?
O3 C4 C2 118.6(5) . . ?
C5 C5 C6 122.4(8) 2_688 . ?
C5 C5 H5 118.8 2_688 . ?
C6 C5 H5 118.8 . . ?
O5 C6 O6 121.2(6) . . ?
O5 C6 C5 121.3(6) . . ?
O6 C6 C5 117.6(6) . . ?
O5 C6 Ce1 62.2(3) . . ?
O6 C6 Ce1 59.0(3) . . ?
C5 C6 Ce1 175.8(5) . . ?
C7 C7 C8 125.2(8) 2_678 . ?
C7 C7 H7 117.4 2_678 . ?
C8 C7 H7 117.4 . . ?
O7 C8 O8 123.3(6) . . ?
O7 C8 C7 117.7(6) . . ?
O8 C8 C7 119.0(6) . . ?
K1 O10 H1A 103.9(16) . . ?
K1 O10 H1B 105.9(17) . . ?
H1A O10 H1B 107(3) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O10 H1A O8 0.99(2) 2.21(5) 2.863(8) 123(4) 1_454
O10 H1B O8 0.95(2) 2.25(6) 2.826(9) 118(5) 2_677

_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        25.36
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         0.945
_refine_diff_density_min         -1.186
_refine_diff_density_rms         0.158

#===END
_database_code_depnum_ccdc_archive 'CCDC 957588'
#######################################################################
#
#                 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_compound11

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C12 H4 La2 N6 O14 S3'
_chemical_formula_sum            'C12 H4 La2 N6 O14 S3'
_chemical_formula_weight         830.21

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   p2(1)

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

_cell_length_a                   7.0404(3)
_cell_length_b                   13.0015(6)
_cell_length_c                   13.7338(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 100.8810(10)
_cell_angle_gamma                90.00
_cell_volume                     1234.53(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    4896
_cell_measurement_theta_min      1.51
_cell_measurement_theta_max      28.37

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    2.233
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             784
_exptl_absorpt_coefficient_mu    3.744
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.3857
_exptl_absorpt_correction_T_max  0.5018
_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 9.00cm
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            7808
_diffrn_reflns_av_R_equivalents  0.0186
_diffrn_reflns_av_sigmaI/netI    0.0399
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.51
_diffrn_reflns_theta_max         28.37
_reflns_number_total             4896
_reflns_number_gt                4815
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXP-97
_computing_publication_material  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.  To improve the parameters 
 chemical more reasonable, ultimately restrain instructions ISOR for 
 (o2w) were applied in the refinement.
;

_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)+(0.0559P)²+1.7742P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   NONE
_refine_ls_hydrogen_treatment    NONE
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.006(18)
_refine_ls_number_reflns         4896
_refine_ls_number_parameters     352
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0283
_refine_ls_R_factor_gt           0.0279
_refine_ls_wR_factor_ref         0.0910
_refine_ls_wR_factor_gt          0.0908
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_restrained_S_all      1.102
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
La1 La 0.79235(5) 1.03844(3) -0.04226(2) 0.01053(9) Uani 1 1 d . . .
La2 La 0.58678(5) 0.96409(3) 0.44074(3) 0.01497(10) Uani 1 1 d . . .
S1 S 1.2581(3) 1.05736(16) 0.18774(13) 0.0245(4) Uani 1 1 d . . .
S2 S 0.6321(4) 1.29124(16) -0.20186(14) 0.0337(5) Uani 1 1 d . . .
S3 S 0.5953(2) 1.30682(14) 0.04923(14) 0.0207(4) Uani 1 1 d . . .
O1 O 0.6583(7) 0.9954(5) 0.1116(4) 0.0249(12) Uani 1 1 d . . .
O2 O 0.6411(8) 0.9933(6) 0.2695(4) 0.0352(16) Uani 1 1 d . . .
O3 O 0.9216(8) 0.9091(5) 0.4269(4) 0.0347(15) Uani 1 1 d . . .
O4 O 1.2423(8) 0.9124(5) 0.4607(4) 0.0296(13) Uani 1 1 d . . .
O5 O 0.7335(8) 0.9720(4) -0.2166(3) 0.0227(10) Uani 1 1 d . . .
O6 O 0.6730(10) 0.9794(5) -0.3803(4) 0.0391(16) Uani 1 1 d . . .
O7 O 0.4130(9) 1.1127(5) -0.5067(4) 0.0334(14) Uani 1 1 d . . .
O8 O 0.3825(8) 1.2829(4) -0.5059(4) 0.0268(12) Uani 1 1 d . . .
O9 O 0.4211(7) 1.0253(4) -0.0972(4) 0.0201(10) Uani 1 1 d . . .
O10 O 0.1143(7) 1.0590(4) -0.0912(5) 0.0273(13) Uani 1 1 d . . .
O11 O -0.0729(7) 1.2171(4) -0.0046(4) 0.0236(11) Uani 1 1 d . . .
O12 O 0.0004(7) 1.3825(4) -0.0076(5) 0.0254(12) Uani 1 1 d . . .
O13 O 0.8027(14) 1.1237(8) 0.4510(8) 0.077(3) Uani 1 1 d . . .
N1 N 1.0258(8) 1.0498(6) 0.1507(4) 0.0212(13) Uani 1 1 d . . .
N2 N 1.2690(8) 1.0100(5) 0.2987(4) 0.0214(13) Uani 1 1 d . . .
N3 N 0.6849(10) 1.1691(5) -0.1989(4) 0.0246(13) Uani 1 1 d . . .
N4 N 0.5365(10) 1.2979(5) -0.3166(5) 0.0246(13) Uani 1 1 d . . .
N5 N 0.5480(8) 1.1920(5) 0.0033(5) 0.0185(12) Uani 1 1 d . . .
N6 N 0.3716(8) 1.3401(5) 0.0440(4) 0.0168(12) Uani 1 1 d . . .
C1 C 0.9480(10) 1.0096(6) 0.2248(5) 0.0192(15) Uani 1 1 d . . .
C2 C 1.0906(9) 0.9861(6) 0.3110(5) 0.0181(14) Uani 1 1 d . . .
C3 C 0.7328(10) 0.9971(6) 0.2007(5) 0.0207(15) Uani 1 1 d . . .
C4 C 1.0790(10) 0.9311(6) 0.4076(5) 0.0194(14) Uani 1 1 d . . .
C5 C 0.6276(10) 1.1304(5) -0.2886(5) 0.0182(14) Uani 1 1 d . . .
C6 C 0.5407(11) 1.2051(6) -0.3582(5) 0.0217(15) Uani 1 1 d . . .
C7 C 0.6786(11) 1.0170(5) -0.2967(5) 0.0204(16) Uani 1 1 d . . .
C8 C 0.4413(10) 1.1987(6) -0.4658(5) 0.0207(14) Uani 1 1 d . . .
C9 C 0.3578(9) 1.1791(5) -0.0183(5) 0.0142(12) Uani 1 1 d . . .
C10 C 0.2558(9) 1.2650(5) 0.0075(5) 0.0148(12) Uani 1 1 d . . .
C11 C 0.2904(10) 1.0796(6) -0.0722(5) 0.0162(13) Uani 1 1 d . . .
C12 C 0.0434(8) 1.2879(5) -0.0032(5) 0.0137(13) Uani 1 1 d . . .
O1W O 0.832(2) 1.2511(15) 0.3470(11) 0.061(5) Uani 0.50 1 d P . .
O2W O 0.893(4) 0.747(2) 0.2493(19) 0.020(5) Uani 0.20 1 d PU . .
O3W O 0.617(4) 1.2603(18) 0.3075(13) 0.043(6) Uani 0.30 1 d P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
La1 O10 2.497(5) 1_655 ?
La1 O5 2.505(5) . ?
La1 O12 2.516(5) 2_645 ?
La1 O11 2.525(5) 1_655 ?
La1 O1 2.534(5) . ?
La1 O9 2.585(5) . ?
La1 N3 2.734(6) . ?
La1 N5 2.783(6) . ?
La1 N6 2.823(6) 2_645 ?
La1 N1 2.847(6) . ?
La2 O6 2.426(5) 1_556 ?
La2 O7 2.466(6) 1_556 ?
La2 O2 2.483(5) . ?
La2 O3 2.505(6) . ?
La2 O8 2.515(6) 2_645 ?
La2 O13 2.560(9) . ?
La2 O4 2.581(6) 1_455 ?
La2 N2 2.742(6) 1_455 ?
La2 N4 2.788(7) 2_645 ?
S1 N1 1.621(6) . ?
S1 N2 1.632(6) . ?
S2 N4 1.594(6) . ?
S2 N3 1.630(7) . ?
S3 N6 1.622(6) . ?
S3 N5 1.631(6) . ?
O1 C3 1.237(8) . ?
O2 C3 1.242(9) . ?
O3 C4 1.221(9) . ?
O4 C4 1.263(9) . ?
O4 La2 2.581(6) 1_655 ?
O5 C7 1.242(9) . ?
O6 C7 1.243(9) . ?
O6 La2 2.426(5) 1_554 ?
O7 C8 1.251(9) . ?
O7 La2 2.466(6) 1_554 ?
O8 C8 1.260(9) . ?
O8 La2 2.515(5) 2_655 ?
O9 C11 1.258(9) . ?
O10 C11 1.247(8) . ?
O10 La1 2.497(5) 1_455 ?
O11 C12 1.230(8) . ?
O11 La1 2.525(5) 1_455 ?
O12 C12 1.266(9) . ?
O12 La1 2.516(5) 2_655 ?
N1 C1 1.349(9) . ?
N2 C2 1.335(9) . ?
N2 La2 2.742(6) 1_655 ?
N3 C5 1.321(9) . ?
N4 C6 1.338(10) . ?
N4 La2 2.788(7) 2_655 ?
N5 C9 1.326(8) . ?
N6 C10 1.310(9) . ?
N6 La1 2.823(6) 2_655 ?
C1 C2 1.433(9) . ?
C1 C3 1.498(10) . ?
C2 C4 1.523(9) . ?
C5 C6 1.417(9) . ?
C5 C7 1.526(10) . ?
C6 C8 1.513(10) . ?
C9 C10 1.408(9) . ?
C9 C11 1.522(10) . ?
C10 C12 1.504(8) . ?
O1W O3W 1.51(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O10 La1 O5 76.96(18) 1_655 . ?
O10 La1 O12 69.54(18) 1_655 2_645 ?
O5 La1 O12 88.00(19) . 2_645 ?
O10 La1 O11 68.39(17) 1_655 1_655 ?
O5 La1 O11 120.06(18) . 1_655 ?
O12 La1 O11 120.61(18) 2_645 1_655 ?
O10 La1 O1 138.43(18) 1_655 . ?
O5 La1 O1 134.43(18) . . ?
O12 La1 O1 83.29(19) 2_645 . ?
O11 La1 O1 102.55(18) 1_655 . ?
O10 La1 O9 147.91(18) 1_655 . ?
O5 La1 O9 73.89(16) . . ?
O12 La1 O9 121.92(17) 2_645 . ?
O11 La1 O9 116.12(16) 1_655 . ?
O1 La1 O9 73.37(16) . . ?
O10 La1 N3 81.5(2) 1_655 . ?
O5 La1 N3 59.40(18) . . ?
O12 La1 N3 140.8(2) 2_645 . ?
O11 La1 N3 68.09(19) 1_655 . ?
O1 La1 N3 134.61(19) . . ?
O9 La1 N3 72.36(19) . . ?
O10 La1 N5 127.94(18) 1_655 . ?
O5 La1 N5 117.68(18) . . ?
O12 La1 N5 150.25(19) 2_645 . ?
O11 La1 N5 61.21(17) 1_655 . ?
O1 La1 N5 68.14(19) . . ?
O9 La1 N5 58.61(17) . . ?
N3 La1 N5 68.91(19) . . ?
O10 La1 N6 119.07(17) 1_655 2_645 ?
O5 La1 N6 71.53(17) . 2_645 ?
O12 La1 N6 58.78(17) 2_645 2_645 ?
O11 La1 N6 168.23(17) 1_655 2_645 ?
O1 La1 N6 65.75(18) . 2_645 ?
O9 La1 N6 63.14(17) . 2_645 ?
N3 La1 N6 120.59(19) . 2_645 ?
N5 La1 N6 112.83(17) . 2_645 ?
O10 La1 N1 81.45(18) 1_655 . ?
O5 La1 N1 150.46(19) . . ?
O12 La1 N1 65.5(2) 2_645 . ?
O11 La1 N1 68.5(2) 1_655 . ?
O1 La1 N1 58.38(16) . . ?
O9 La1 N1 130.50(16) . . ?
N3 La1 N1 136.5(2) . . ?
N5 La1 N1 91.50(19) . . ?
N6 La1 N1 102.64(19) 2_645 . ?
O6 La2 O7 71.50(19) 1_556 1_556 ?
O6 La2 O2 153.3(2) 1_556 . ?
O7 La2 O2 109.3(2) 1_556 . ?
O6 La2 O3 92.4(2) 1_556 . ?
O7 La2 O3 140.5(2) 1_556 . ?
O2 La2 O3 69.90(19) . . ?
O6 La2 O8 74.2(2) 1_556 2_645 ?
O7 La2 O8 130.1(2) 1_556 2_645 ?
O2 La2 O8 117.5(2) . 2_645 ?
O3 La2 O8 75.0(2) . 2_645 ?
O6 La2 O13 81.1(3) 1_556 . ?
O7 La2 O13 70.8(3) 1_556 . ?
O2 La2 O13 74.5(3) . . ?
O3 La2 O13 71.2(3) . . ?
O8 La2 O13 136.8(3) 2_645 . ?
O6 La2 O4 88.5(2) 1_556 1_455 ?
O7 La2 O4 69.2(2) 1_556 1_455 ?
O2 La2 O4 117.14(18) . 1_455 ?
O3 La2 O4 148.3(2) . 1_455 ?
O8 La2 O4 74.80(19) 2_645 1_455 ?
O13 La2 O4 139.9(3) . 1_455 ?
O6 La2 N2 135.8(2) 1_556 1_455 ?
O7 La2 N2 69.78(18) 1_556 1_455 ?
O2 La2 N2 62.84(18) . 1_455 ?
O3 La2 N2 131.40(18) . 1_455 ?
O8 La2 N2 117.43(18) 2_645 1_455 ?
O13 La2 N2 105.0(3) . 1_455 ?
O4 La2 N2 58.33(17) 1_455 1_455 ?
O6 La2 N4 132.3(2) 1_556 2_645 ?
O7 La2 N4 132.2(2) 1_556 2_645 ?
O2 La2 N4 68.0(2) . 2_645 ?
O3 La2 N4 85.5(2) . 2_645 ?
O8 La2 N4 59.16(17) 2_645 2_645 ?
O13 La2 N4 140.8(3) . 2_645 ?
O4 La2 N4 70.9(2) 1_455 2_645 ?
N2 La2 N4 67.4(2) 1_455 2_645 ?
N1 S1 N2 97.9(3) . . ?
N4 S2 N3 97.4(3) . . ?
N6 S3 N5 95.8(3) . . ?
C3 O1 La1 131.7(5) . . ?
C3 O2 La2 157.2(5) . . ?
C4 O3 La2 148.8(6) . . ?
C4 O4 La2 131.3(5) . 1_655 ?
C7 O5 La1 130.6(5) . . ?
C7 O6 La2 158.0(5) . 1_554 ?
C8 O7 La2 141.8(5) . 1_554 ?
C8 O8 La2 131.3(5) . 2_655 ?
C11 O9 La1 129.4(5) . . ?
C11 O10 La1 152.1(5) . 1_455 ?
C12 O11 La1 156.2(5) . 1_455 ?
C12 O12 La1 130.5(4) . 2_655 ?
C1 N1 S1 108.4(5) . . ?
C1 N1 La1 115.9(4) . . ?
S1 N1 La1 131.8(3) . . ?
C2 N2 S1 109.0(5) . . ?
C2 N2 La2 121.4(5) . 1_655 ?
S1 N2 La2 129.4(3) . 1_655 ?
C5 N3 S2 108.7(5) . . ?
C5 N3 La1 119.2(5) . . ?
S2 N3 La1 130.8(3) . . ?
C6 N4 S2 109.5(5) . . ?
C6 N4 La2 117.9(5) . 2_655 ?
S2 N4 La2 132.1(4) . 2_655 ?
C9 N5 S3 109.0(5) . . ?
C9 N5 La1 120.0(4) . . ?
S3 N5 La1 130.8(3) . . ?
C10 N6 S3 110.3(5) . . ?
C10 N6 La1 117.0(4) . 2_655 ?
S3 N6 La1 129.5(3) . 2_655 ?
N1 C1 C2 112.6(6) . . ?
N1 C1 C3 114.4(6) . . ?
C2 C1 C3 133.0(6) . . ?
N2 C2 C1 112.0(6) . . ?
N2 C2 C4 115.2(6) . . ?
C1 C2 C4 132.5(6) . . ?
O1 C3 O2 124.6(7) . . ?
O1 C3 C1 116.3(6) . . ?
O2 C3 C1 119.0(6) . . ?
O3 C4 O4 126.5(7) . . ?
O3 C4 C2 119.9(6) . . ?
O4 C4 C2 113.6(6) . . ?
N3 C5 C6 112.6(7) . . ?
N3 C5 C7 113.6(6) . . ?
C6 C5 C7 133.6(6) . . ?
N4 C6 C5 111.8(6) . . ?
N4 C6 C8 115.0(6) . . ?
C5 C6 C8 133.0(7) . . ?
O5 C7 O6 125.7(6) . . ?
O5 C7 C5 115.5(6) . . ?
O6 C7 C5 118.7(6) . . ?
O7 C8 O8 124.7(7) . . ?
O7 C8 C6 119.6(7) . . ?
O8 C8 C6 115.6(7) . . ?
N5 C9 C10 112.6(6) . . ?
N5 C9 C11 115.1(6) . . ?
C10 C9 C11 132.0(6) . . ?
N6 C10 C9 112.2(6) . . ?
N6 C10 C12 115.1(6) . . ?
C9 C10 C12 132.6(6) . . ?
O10 C11 O9 124.9(7) . . ?
O10 C11 C9 119.4(6) . . ?
O9 C11 C9 115.7(6) . . ?
O11 C12 O12 125.0(6) . . ?
O11 C12 C10 120.0(6) . . ?
O12 C12 C10 114.9(6) . . ?

_diffrn_measured_fraction_theta_max 0.971
_diffrn_reflns_theta_full        28.37
_diffrn_measured_fraction_theta_full 0.971
_refine_diff_density_max         2.360
_refine_diff_density_min         -0.805
_refine_diff_density_rms         0.201
_database_code_depnum_ccdc_archive 'CCDC 957589'
#######################################################################
#
#                 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_compound12

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C12 H4 Ce2 N6 O14 S3'
_chemical_formula_sum            'C12 H4 Ce2 N6 O14 S3'
_chemical_formula_weight         832.63

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'
Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   p2(1)

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

_cell_length_a                   6.975(5)
_cell_length_b                   12.901(8)
_cell_length_c                   13.551(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 100.729(11)
_cell_angle_gamma                90.00
_cell_volume                     1198.0(14)
_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            colourless
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    2.308
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             788
_exptl_absorpt_coefficient_mu    4.092
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.3857
_exptl_absorpt_correction_T_max  0.5018
_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 9.00cm
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            5916
_diffrn_reflns_av_R_equivalents  0.0895
_diffrn_reflns_av_sigmaI/netI    0.1099
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.06
_diffrn_reflns_theta_max         24.99
_reflns_number_total             3628
_reflns_number_gt                3248
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXP-97
_computing_publication_material  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. To improve the parameters 
 chemical more reasonable, ultimately restrain instructions ISOR for 
 (o6, n2, n4, c1, c4, c5, c7, c12, n3, o3, o5, o8, o1w, o2w, o4w, o3w), and 
 OMIT were applied in the refinement.
;

_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)+(0.1190P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   ?
_refine_ls_hydrogen_treatment    ?
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.03(4)
_refine_ls_number_reflns         3628
_refine_ls_number_parameters     361
_refine_ls_number_restraints     97
_refine_ls_R_factor_all          0.0766
_refine_ls_R_factor_gt           0.0718
_refine_ls_wR_factor_ref         0.1796
_refine_ls_wR_factor_gt          0.1759
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_restrained_S_all      0.995
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ce1 Ce 0.20663(13) -0.03988(7) 1.04123(6) 0.0139(3) Uani 1 1 d . . .
Ce2 Ce 0.41472(13) 0.03765(8) 0.55864(7) 0.0179(3) Uani 1 1 d . . .
S1 S -0.2583(7) -0.0586(5) 0.8117(3) 0.0282(13) Uani 1 1 d . . .
S2 S 0.3671(9) -0.2918(4) 1.2010(4) 0.0369(14) Uani 1 1 d . . .
S3 S 0.4031(6) -0.3074(4) 0.9477(4) 0.0261(11) Uani 1 1 d . . .
O1 O 0.3460(19) 0.0043(11) 0.8904(9) 0.027(3) Uani 1 1 d . . .
O2 O 0.3603(19) 0.0055(13) 0.7299(10) 0.037(4) Uani 1 1 d . . .
O3 O 0.078(2) 0.0928(12) 0.5730(11) 0.031(3) Uani 1 1 d U . .
O4 O -0.243(2) 0.0887(13) 0.5353(10) 0.034(4) Uani 1 1 d . . .
O5 O 0.2596(16) 0.0289(11) 1.2148(9) 0.020(3) Uani 1 1 d U . .
O6 O 0.329(2) 0.0249(13) 1.3799(11) 0.039(4) Uani 1 1 d U . .
O7 O 0.585(2) -0.1120(12) 1.5075(11) 0.038(4) Uani 1 1 d . . .
O8 O 0.6150(18) -0.2828(11) 1.5094(10) 0.027(3) Uani 1 1 d U . .
O9 O 0.5780(18) -0.0273(12) 1.0970(10) 0.025(3) Uani 1 1 d . . .
O10 O 0.8874(18) -0.0589(12) 1.0918(11) 0.029(3) Uani 1 1 d . . .
O11 O 1.0730(17) -0.2199(10) 1.0052(10) 0.022(3) Uani 1 1 d . . .
O12 O 1.0000(19) -0.3846(11) 1.0089(11) 0.029(3) Uani 1 1 d . . .
O13 O 0.195(3) -0.118(2) 0.5424(15) 0.083(8) Uani 1 1 d . . .
N1 N -0.025(2) -0.0475(18) 0.8496(13) 0.031(4) Uani 1 1 d . . .
N2 N -0.269(2) -0.0107(12) 0.7002(12) 0.020(3) Uani 1 1 d U . .
N3 N 0.314(2) -0.1679(14) 1.1988(12) 0.027(4) Uani 1 1 d U . .
N4 N 0.463(2) -0.2983(14) 1.3154(13) 0.027(4) Uani 1 1 d U . .
N5 N 0.453(2) -0.1937(14) 0.9949(13) 0.026(4) Uani 1 1 d . . .
N6 N 0.625(2) -0.3436(13) 0.9538(11) 0.018(4) Uani 1 1 d . . .
C1 C 0.045(3) -0.0131(14) 0.7739(14) 0.020(4) Uani 1 1 d U . .
C2 C -0.091(2) 0.0137(14) 0.6893(14) 0.019(4) Uani 1 1 d . . .
C3 C 0.262(2) 0.0020(15) 0.7973(13) 0.018(4) Uani 1 1 d . . .
C4 C -0.072(2) 0.0691(14) 0.5928(14) 0.018(4) Uani 1 1 d U . .
C5 C 0.373(2) -0.1285(14) 1.2873(12) 0.014(3) Uani 1 1 d U . .
C6 C 0.459(3) -0.2045(15) 1.3578(15) 0.023(4) Uani 1 1 d . . .
C7 C 0.323(2) -0.0194(13) 1.2967(13) 0.016(4) Uani 1 1 d U . .
C8 C 0.557(3) -0.1996(17) 1.4659(14) 0.025(4) Uani 1 1 d . . .
C9 C 0.644(3) -0.1799(15) 1.0156(13) 0.020(4) Uani 1 1 d . . .
C10 C 0.746(2) -0.2669(14) 0.9924(12) 0.015(4) Uani 1 1 d . . .
C11 C 0.713(3) -0.0799(15) 1.0721(14) 0.019(4) Uani 1 1 d . . .
C12 C 0.959(2) -0.2887(14) 1.0058(13) 0.014(4) Uani 1 1 d U . .
O1W O 0.161(6) -0.242(4) 0.646(3) 0.042(11) Uani 0.35 1 d PU . .
O2W O 0.118(10) 0.258(6) 0.755(5) 0.025(14) Uani 0.20 1 d PU . .
O3W O 0.192(13) 0.453(8) 0.677(6) 0.030(19) Uani 0.15 1 d PU . .
O4W O 0.396(7) -0.259(4) 0.703(4) 0.036(12) Uani 0.30 1 d PU . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ce1 O10 2.460(13) 1_455 ?
Ce1 O5 2.476(12) . ?
Ce1 O12 2.487(14) 2_657 ?
Ce1 O1 2.487(13) . ?
Ce1 O11 2.516(13) 1_455 ?
Ce1 O9 2.565(13) . ?
Ce1 N3 2.692(17) . ?
Ce1 N5 2.772(16) . ?
Ce1 N6 2.788(16) 2_657 ?
Ce1 N1 2.792(17) . ?
Ce2 O6 2.389(15) 1_554 ?
Ce2 O7 2.435(15) 1_554 ?
Ce2 O2 2.455(14) . ?
Ce2 O8 2.488(14) 2_657 ?
Ce2 O3 2.495(14) . ?
Ce2 O13 2.51(2) . ?
Ce2 O4 2.555(15) 1_655 ?
Ce2 N2 2.715(15) 1_655 ?
Ce2 N4 2.752(18) 2_657 ?
S1 N1 1.620(15) . ?
S1 N2 1.621(16) . ?
S2 N4 1.573(18) . ?
S2 N3 1.640(19) . ?
S3 N6 1.602(14) . ?
S3 N5 1.612(18) . ?
O1 C3 1.29(2) . ?
O2 C3 1.24(2) . ?
O3 C4 1.17(2) . ?
O4 C4 1.32(2) . ?
O4 Ce2 2.555(15) 1_455 ?
O5 C7 1.28(2) . ?
O6 C7 1.26(2) . ?
O6 Ce2 2.389(15) 1_556 ?
O7 C8 1.26(2) . ?
O7 Ce2 2.435(15) 1_556 ?
O8 C8 1.25(2) . ?
O8 Ce2 2.488(14) 2_647 ?
O9 C11 1.26(2) . ?
O10 C11 1.22(2) . ?
O10 Ce1 2.460(13) 1_655 ?
O11 C12 1.19(2) . ?
O11 Ce1 2.516(13) 1_655 ?
O12 C12 1.27(2) . ?
O12 Ce1 2.487(14) 2_647 ?
N1 C1 1.29(3) . ?
N2 C2 1.32(2) . ?
N2 Ce2 2.715(15) 1_455 ?
N3 C5 1.30(2) . ?
N4 C6 1.34(3) . ?
N4 Ce2 2.752(18) 2_647 ?
N5 C9 1.32(2) . ?
N6 C10 1.34(2) . ?
N6 Ce1 2.788(16) 2_647 ?
C1 C2 1.39(3) . ?
C1 C3 1.50(2) . ?
C2 C4 1.52(3) . ?
C5 C6 1.42(2) . ?
C5 C7 1.46(2) . ?
C6 C8 1.50(3) . ?
C9 C10 1.40(3) . ?
C9 C11 1.53(3) . ?
C10 C12 1.49(2) . ?
O1W O4W 1.69(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O10 Ce1 O5 75.8(4) 1_455 . ?
O10 Ce1 O12 69.4(5) 1_455 2_657 ?
O5 Ce1 O12 87.0(5) . 2_657 ?
O10 Ce1 O1 139.8(5) 1_455 . ?
O5 Ce1 O1 133.3(4) . . ?
O12 Ce1 O1 83.5(5) 2_657 . ?
O10 Ce1 O11 68.9(5) 1_455 1_455 ?
O5 Ce1 O11 120.0(4) . 1_455 ?
O12 Ce1 O11 121.0(5) 2_657 1_455 ?
O1 Ce1 O11 103.8(4) . 1_455 ?
O10 Ce1 O9 147.2(5) 1_455 . ?
O5 Ce1 O9 74.5(4) . . ?
O12 Ce1 O9 122.1(5) 2_657 . ?
O1 Ce1 O9 72.5(4) . . ?
O11 Ce1 O9 115.6(4) 1_455 . ?
O10 Ce1 N3 81.4(5) 1_455 . ?
O5 Ce1 N3 59.8(5) . . ?
O12 Ce1 N3 140.5(5) 2_657 . ?
O1 Ce1 N3 134.3(5) . . ?
O11 Ce1 N3 68.0(5) 1_455 . ?
O9 Ce1 N3 71.8(5) . . ?
O10 Ce1 N5 128.5(5) 1_455 . ?
O5 Ce1 N5 118.9(5) . . ?
O12 Ce1 N5 150.1(5) 2_657 . ?
O1 Ce1 N5 67.9(5) . . ?
O11 Ce1 N5 61.2(4) 1_455 . ?
O9 Ce1 N5 58.5(5) . . ?
N3 Ce1 N5 69.4(5) . . ?
O10 Ce1 N6 118.9(5) 1_455 2_657 ?
O5 Ce1 N6 70.4(4) . 2_657 ?
O12 Ce1 N6 59.7(5) 2_657 2_657 ?
O1 Ce1 N6 65.4(4) . 2_657 ?
O11 Ce1 N6 169.3(4) 1_455 2_657 ?
O9 Ce1 N6 62.4(5) . 2_657 ?
N3 Ce1 N6 119.0(5) . 2_657 ?
N5 Ce1 N6 112.3(5) . 2_657 ?
O10 Ce1 N1 81.9(4) 1_455 . ?
O5 Ce1 N1 148.6(5) . . ?
O12 Ce1 N1 64.5(6) 2_657 . ?
O1 Ce1 N1 59.4(4) . . ?
O11 Ce1 N1 70.0(5) 1_455 . ?
O9 Ce1 N1 130.8(4) . . ?
N3 Ce1 N1 138.0(6) . . ?
N5 Ce1 N1 92.3(6) . . ?
N6 Ce1 N1 102.9(6) 2_657 . ?
O6 Ce2 O7 72.6(5) 1_554 1_554 ?
O6 Ce2 O2 153.2(5) 1_554 . ?
O7 Ce2 O2 107.7(5) 1_554 . ?
O6 Ce2 O8 72.6(5) 1_554 2_657 ?
O7 Ce2 O8 130.1(5) 1_554 2_657 ?
O2 Ce2 O8 119.4(5) . 2_657 ?
O6 Ce2 O3 92.2(5) 1_554 . ?
O7 Ce2 O3 139.9(5) 1_554 . ?
O2 Ce2 O3 70.2(5) . . ?
O8 Ce2 O3 75.5(4) 2_657 . ?
O6 Ce2 O13 79.8(6) 1_554 . ?
O7 Ce2 O13 70.3(8) 1_554 . ?
O2 Ce2 O13 75.4(6) . . ?
O8 Ce2 O13 134.9(7) 2_657 . ?
O3 Ce2 O13 70.6(7) . . ?
O6 Ce2 O4 87.4(5) 1_554 1_655 ?
O7 Ce2 O4 69.6(5) 1_554 1_655 ?
O2 Ce2 O4 118.2(4) . 1_655 ?
O8 Ce2 O4 74.3(5) 2_657 1_655 ?
O3 Ce2 O4 148.4(5) . 1_655 ?
O13 Ce2 O4 139.9(7) . 1_655 ?
O6 Ce2 N2 135.8(5) 1_554 1_655 ?
O7 Ce2 N2 69.1(5) 1_554 1_655 ?
O2 Ce2 N2 62.7(4) . 1_655 ?
O8 Ce2 N2 118.5(4) 2_657 1_655 ?
O3 Ce2 N2 131.6(5) . 1_655 ?
O13 Ce2 N2 106.3(6) . 1_655 ?
O4 Ce2 N2 59.3(4) 1_655 1_655 ?
O6 Ce2 N4 132.2(5) 1_554 2_657 ?
O7 Ce2 N4 132.4(5) 1_554 2_657 ?
O2 Ce2 N4 68.2(5) . 2_657 ?
O8 Ce2 N4 60.6(5) 2_657 2_657 ?
O3 Ce2 N4 85.4(5) . 2_657 ?
O13 Ce2 N4 141.5(6) . 2_657 ?
O4 Ce2 N4 71.9(5) 1_655 2_657 ?
N2 Ce2 N4 67.7(5) 1_655 2_657 ?
N1 S1 N2 97.5(8) . . ?
N4 S2 N3 97.1(9) . . ?
N6 S3 N5 96.3(8) . . ?
C3 O1 Ce1 128.7(11) . . ?
C3 O2 Ce2 155.0(12) . . ?
C4 O3 Ce2 147.1(14) . . ?
C4 O4 Ce2 129.7(12) . 1_455 ?
C7 O5 Ce1 128.1(11) . . ?
C7 O6 Ce2 154.2(13) . 1_556 ?
C8 O7 Ce2 142.4(14) . 1_556 ?
C8 O8 Ce2 128.7(12) . 2_647 ?
C11 O9 Ce1 130.8(12) . . ?
C11 O10 Ce1 150.9(13) . 1_655 ?
C12 O11 Ce1 155.3(12) . 1_655 ?
C12 O12 Ce1 131.3(11) . 2_647 ?
C1 N1 S1 106.6(14) . . ?
C1 N1 Ce1 119.1(13) . . ?
S1 N1 Ce1 132.2(8) . . ?
C2 N2 S1 108.5(13) . . ?
C2 N2 Ce2 121.7(12) . 1_455 ?
S1 N2 Ce2 129.4(7) . 1_455 ?
C5 N3 S2 109.5(14) . . ?
C5 N3 Ce1 119.1(13) . . ?
S2 N3 Ce1 129.9(9) . . ?
C6 N4 S2 109.6(14) . . ?
C6 N4 Ce2 117.1(13) . 2_647 ?
S2 N4 Ce2 132.7(10) . 2_647 ?
C9 N5 S3 110.0(13) . . ?
C9 N5 Ce1 119.9(13) . . ?
S3 N5 Ce1 130.1(8) . . ?
C10 N6 S3 109.8(12) . . ?
C10 N6 Ce1 115.2(10) . 2_647 ?
S3 N6 Ce1 131.7(9) . 2_647 ?
N1 C1 C2 116.0(17) . . ?
N1 C1 C3 113.1(17) . . ?
C2 C1 C3 130.4(16) . . ?
N2 C2 C1 111.1(17) . . ?
N2 C2 C4 116.4(15) . . ?
C1 C2 C4 132.4(16) . . ?
O2 C3 O1 120.7(16) . . ?
O2 C3 C1 121.4(16) . . ?
O1 C3 C1 117.7(15) . . ?
O3 C4 O4 124.2(18) . . ?
O3 C4 C2 123.0(16) . . ?
O4 C4 C2 112.8(15) . . ?
N3 C5 C6 111.9(17) . . ?
N3 C5 C7 114.6(16) . . ?
C6 C5 C7 133.2(16) . . ?
N4 C6 C5 111.9(16) . . ?
N4 C6 C8 114.6(17) . . ?
C5 C6 C8 133.3(18) . . ?
O6 C7 O5 120.4(15) . . ?
O6 C7 C5 123.1(16) . . ?
O5 C7 C5 116.3(15) . . ?
O8 C8 O7 123.1(17) . . ?
O8 C8 C6 118.1(18) . . ?
O7 C8 C6 118.7(17) . . ?
N5 C9 C10 112.4(17) . . ?
N5 C9 C11 115.6(17) . . ?
C10 C9 C11 131.5(16) . . ?
N6 C10 C9 111.5(15) . . ?
N6 C10 C12 116.8(15) . . ?
C9 C10 C12 131.7(17) . . ?
O10 C11 O9 125.8(19) . . ?
O10 C11 C9 120.2(17) . . ?
O9 C11 C9 114.0(16) . . ?
O11 C12 O12 125.3(15) . . ?
O11 C12 C10 120.7(17) . . ?
O12 C12 C10 113.8(15) . . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        24.99
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         2.620
_refine_diff_density_min         -2.946
_refine_diff_density_rms         0.312


#===END
_database_code_depnum_ccdc_archive 'CCDC 957590'
