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

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

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H24 N5 O Se3 Sn Y'
_chemical_formula_sum            'C8 H24 N5 O Se3 Sn Y'
_chemical_formula_weight         650.82

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   Pbca
_symmetry_space_group_name_Hall  '-P 2ac 2ab '

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

_cell_length_a                   12.4190(4)
_cell_length_b                   13.6062(6)
_cell_length_c                   20.6569(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3490.5(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    10676
_cell_measurement_theta_min      3.55
_cell_measurement_theta_max      28.94

_exptl_crystal_description       sheet
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.467
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2448
_exptl_absorpt_coefficient_mu    10.996
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3776
_exptl_absorpt_correction_T_max  0.6094
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 7.31
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8993
_diffrn_reflns_av_R_equivalents  0.0272
_diffrn_reflns_av_unetI/netI     0.0299
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         3.55
_diffrn_reflns_theta_max         25.09
_reflns_number_total             3097
_reflns_number_gt                2629
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)'
_computing_cell_refinement       'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)'
_computing_data_reduction        
'CrystalStructure, Ver. 3.60 (Rigaku/MSC, 2004)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL97

_refine_special_details          
; 
SIMU restraint prevents the thermal ellipsoids of all adjacent 
C and N atoms from adopting different orientations, and DFIX 
restraint makes all the C-C and C-N distances approximately equal. 
Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0725P)²+71.5505P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3097
_refine_ls_number_parameters     172
_refine_ls_number_restraints     234
_refine_ls_R_factor_all          0.0677
_refine_ls_R_factor_gt           0.0570
_refine_ls_wR_factor_ref         0.1524
_refine_ls_wR_factor_gt          0.1457
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_restrained_S_all      1.069
_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
Sn1 Sn 0.08779(5) 0.53360(5) 0.56225(3) 0.0228(2) Uani 1 1 d . . .
Y1 Y 0.45472(7) 0.52088(6) 0.58448(4) 0.0146(2) Uani 1 1 d . . .
Se1 Se 0.25709(9) 0.61758(9) 0.53135(5) 0.0303(3) Uani 1 1 d . . .
Se2 Se 0.07103(9) 0.37613(8) 0.49218(6) 0.0305(3) Uani 1 1 d . . .
Se3 Se 0.07239(10) 0.50460(10) 0.67945(6) 0.0385(3) Uani 1 1 d . . .
O1W O 0.4926(5) 0.4076(5) 0.5100(3) 0.0218(15) Uani 1 1 d . . .
H1WA H 0.5486 0.3762 0.5215 0.033 Uiso 1 1 d R . .
N1 N 0.3625(8) 0.5592(7) 0.6912(5) 0.0381(17) Uani 1 1 d DU . .
H1A H 0.2914 0.5485 0.6862 0.046 Uiso 1 1 calc R . .
H1B H 0.3864 0.5161 0.7210 0.046 Uiso 1 1 calc R . .
N2 N 0.4931(7) 0.6944(7) 0.6210(5) 0.0375(18) Uani 1 1 d DU . .
H2C H 0.4892 0.7336 0.5854 0.045 Uiso 1 1 calc R . .
N3 N 0.6570(7) 0.5514(6) 0.6022(4) 0.0329(16) Uani 1 1 d DU . .
H3C H 0.6883 0.5347 0.5639 0.039 Uiso 1 1 calc R . .
N4 N 0.5430(6) 0.3965(6) 0.6595(5) 0.0310(16) Uani 1 1 d DU . .
H4C H 0.5337 0.4190 0.7006 0.037 Uiso 1 1 calc R . .
N5 N 0.3270(8) 0.3787(6) 0.6139(4) 0.0311(17) Uani 1 1 d DU . .
H5A H 0.2643 0.4042 0.6279 0.037 Uiso 1 1 calc R . .
H5B H 0.3130 0.3438 0.5779 0.037 Uiso 1 1 calc R . .
C1 C 0.3767(12) 0.6577(7) 0.7171(6) 0.050(2) Uani 1 1 d DU . .
H1C H 0.4298 0.6558 0.7515 0.060 Uiso 1 1 calc R . .
H1D H 0.3092 0.6798 0.7358 0.060 Uiso 1 1 calc R . .
C2 C 0.4119(11) 0.7295(9) 0.6670(6) 0.056(2) Uani 1 1 d DU . .
H2A H 0.3490 0.7502 0.6427 0.067 Uiso 1 1 calc R . .
H2B H 0.4404 0.7870 0.6888 0.067 Uiso 1 1 calc R . .
C3 C 0.5982(8) 0.7092(11) 0.6496(7) 0.052(2) Uani 1 1 d DU . .
H3A H 0.5982 0.6849 0.6938 0.062 Uiso 1 1 calc R . .
H3B H 0.6147 0.7789 0.6507 0.062 Uiso 1 1 calc R . .
C4 C 0.6827(10) 0.6558(7) 0.6108(7) 0.045(2) Uani 1 1 d DU . .
H4A H 0.6893 0.6866 0.5686 0.054 Uiso 1 1 calc R . .
H4B H 0.7516 0.6616 0.6326 0.054 Uiso 1 1 calc R . .
C5 C 0.7094(9) 0.4887(7) 0.6501(6) 0.0389(19) Uani 1 1 d DU . .
H5C H 0.7014 0.5173 0.6928 0.047 Uiso 1 1 calc R . .
H5D H 0.7857 0.4840 0.6406 0.047 Uiso 1 1 calc R . .
C6 C 0.6595(7) 0.3876(7) 0.6490(6) 0.0347(18) Uani 1 1 d DU . .
H6A H 0.6732 0.3564 0.6076 0.042 Uiso 1 1 calc R . .
H6B H 0.6911 0.3472 0.6827 0.042 Uiso 1 1 calc R . .
C7 C 0.4890(7) 0.3004(7) 0.6558(6) 0.0346(19) Uani 1 1 d DU . .
H7A H 0.5168 0.2576 0.6895 0.042 Uiso 1 1 calc R . .
H7B H 0.5043 0.2701 0.6143 0.042 Uiso 1 1 calc R . .
C8 C 0.3687(8) 0.3115(8) 0.6638(5) 0.037(2) Uani 1 1 d DU . .
H8A H 0.3342 0.2479 0.6598 0.045 Uiso 1 1 calc R . .
H8B H 0.3528 0.3375 0.7065 0.045 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sn1 Se3 2.4602(14) . ?
Sn1 Se1 2.4766(13) . ?
Sn1 Se2 2.5813(13) 5_566 ?
Sn1 Se2 2.5941(13) . ?
Y1 O1W 2.228(7) . ?
Y1 O1W 2.277(7) 5_666 ?
Y1 N2 2.524(9) . ?
Y1 N1 2.539(9) . ?
Y1 N4 2.543(9) . ?
Y1 N3 2.573(9) . ?
Y1 N5 2.575(9) . ?
Y1 Se1 2.9932(14) . ?
Y1 Y1 3.7106(17) 5_666 ?
Se2 Sn1 2.5813(13) 5_566 ?
O1W Y1 2.277(6) 5_666 ?
O1W H1WA 0.8500 . ?
N1 C1 1.454(9) . ?
N1 H1A 0.9000 . ?
N1 H1B 0.9000 . ?
N2 C3 1.447(9) . ?
N2 C2 1.465(9) . ?
N2 H2C 0.9100 . ?
N3 C5 1.459(9) . ?
N3 C4 1.466(8) . ?
N3 H3C 0.9100 . ?
N4 C6 1.468(8) . ?
N4 C7 1.471(8) . ?
N4 H4C 0.9100 . ?
N5 C8 1.472(8) . ?
N5 H5A 0.9000 . ?
N5 H5B 0.9000 . ?
C1 C2 1.489(9) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.507(9) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.510(9) . ?
C5 H5C 0.9700 . ?
C5 H5D 0.9700 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C8 1.510(9) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?

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
Se3 Sn1 Se1 113.18(5) . . ?
Se3 Sn1 Se2 116.46(5) . 5_566 ?
Se1 Sn1 Se2 108.47(5) . 5_566 ?
Se3 Sn1 Se2 114.23(5) . . ?
Se1 Sn1 Se2 107.78(5) . . ?
Se2 Sn1 Se2 95.08(4) 5_566 . ?
O1W Y1 O1W 69.1(3) . 5_666 ?
O1W Y1 N2 144.5(3) . . ?
O1W Y1 N2 78.6(3) 5_666 . ?
O1W Y1 N1 146.8(3) . . ?
O1W Y1 N1 141.8(3) 5_666 . ?
N2 Y1 N1 68.5(3) . . ?
O1W Y1 N4 82.5(3) . . ?
O1W Y1 N4 133.1(3) 5_666 . ?
N2 Y1 N4 111.0(3) . . ?
N1 Y1 N4 78.6(3) . . ?
O1W Y1 N3 90.2(3) . . ?
O1W Y1 N3 76.8(3) 5_666 . ?
N2 Y1 N3 67.8(3) . . ?
N1 Y1 N3 106.5(3) . . ?
N4 Y1 N3 66.4(3) . . ?
O1W Y1 N5 76.9(3) . . ?
O1W Y1 N5 134.5(3) 5_666 . ?
N2 Y1 N5 138.4(3) . . ?
N1 Y1 N5 70.8(3) . . ?
N4 Y1 N5 67.8(3) . . ?
N3 Y1 N5 133.6(3) . . ?
O1W Y1 Se1 102.93(18) . . ?
O1W Y1 Se1 74.56(17) 5_666 . ?
N2 Y1 Se1 81.6(2) . . ?
N1 Y1 Se1 81.8(2) . . ?
N4 Y1 Se1 150.38(18) . . ?
N3 Y1 Se1 141.45(19) . . ?
N5 Y1 Se1 84.94(19) . . ?
O1W Y1 Y1 34.98(17) . 5_666 ?
O1W Y1 Y1 34.12(17) 5_666 5_666 ?
N2 Y1 Y1 111.6(2) . 5_666 ?
N1 Y1 Y1 170.1(2) . 5_666 ?
N4 Y1 Y1 109.9(2) . 5_666 ?
N3 Y1 Y1 82.1(2) . 5_666 ?
N5 Y1 Y1 107.1(2) . 5_666 ?
Se1 Y1 Y1 88.34(4) . 5_666 ?
Sn1 Se1 Y1 113.50(5) . . ?
Sn1 Se2 Sn1 84.92(4) 5_566 . ?
Y1 O1W Y1 110.9(3) . 5_666 ?
Y1 O1W H1WA 109.1 . . ?
Y1 O1W H1WA 102.6 5_666 . ?
C1 N1 Y1 117.0(7) . . ?
C1 N1 H1A 108.0 . . ?
Y1 N1 H1A 108.0 . . ?
C1 N1 H1B 108.0 . . ?
Y1 N1 H1B 108.0 . . ?
H1A N1 H1B 107.3 . . ?
C3 N2 C2 108.1(10) . . ?
C3 N2 Y1 115.0(7) . . ?
C2 N2 Y1 111.7(7) . . ?
C3 N2 H2C 107.2 . . ?
C2 N2 H2C 107.2 . . ?
Y1 N2 H2C 107.2 . . ?
C5 N3 C4 112.7(9) . . ?
C5 N3 Y1 116.0(7) . . ?
C4 N3 Y1 112.7(7) . . ?
C5 N3 H3C 104.7 . . ?
C4 N3 H3C 104.7 . . ?
Y1 N3 H3C 104.7 . . ?
C6 N4 C7 111.6(8) . . ?
C6 N4 Y1 112.9(6) . . ?
C7 N4 Y1 111.3(6) . . ?
C6 N4 H4C 106.9 . . ?
C7 N4 H4C 106.9 . . ?
Y1 N4 H4C 106.9 . . ?
C8 N5 Y1 114.5(7) . . ?
C8 N5 H5A 108.6 . . ?
Y1 N5 H5A 108.6 . . ?
C8 N5 H5B 108.6 . . ?
Y1 N5 H5B 108.6 . . ?
H5A N5 H5B 107.6 . . ?
N1 C1 C2 112.6(10) . . ?
N1 C1 H1C 109.1 . . ?
C2 C1 H1C 109.1 . . ?
N1 C1 H1D 109.1 . . ?
C2 C1 H1D 109.1 . . ?
H1C C1 H1D 107.8 . . ?
N2 C2 C1 116.1(11) . . ?
N2 C2 H2A 108.3 . . ?
C1 C2 H2A 108.3 . . ?
N2 C2 H2B 108.3 . . ?
C1 C2 H2B 108.3 . . ?
H2A C2 H2B 107.4 . . ?
N2 C3 C4 110.1(10) . . ?
N2 C3 H3A 109.6 . . ?
C4 C3 H3A 109.6 . . ?
N2 C3 H3B 109.6 . . ?
C4 C3 H3B 109.6 . . ?
H3A C3 H3B 108.2 . . ?
N3 C4 C3 112.3(10) . . ?
N3 C4 H4A 109.1 . . ?
C3 C4 H4A 109.1 . . ?
N3 C4 H4B 109.1 . . ?
C3 C4 H4B 109.1 . . ?
H4A C4 H4B 107.9 . . ?
N3 C5 C6 109.8(9) . . ?
N3 C5 H5C 109.7 . . ?
C6 C5 H5C 109.7 . . ?
N3 C5 H5D 109.7 . . ?
C6 C5 H5D 109.7 . . ?
H5C C5 H5D 108.2 . . ?
N4 C6 C5 109.1(9) . . ?
N4 C6 H6A 109.9 . . ?
C5 C6 H6A 109.9 . . ?
N4 C6 H6B 109.9 . . ?
C5 C6 H6B 109.9 . . ?
H6A C6 H6B 108.3 . . ?
N4 C7 C8 110.8(8) . . ?
N4 C7 H7A 109.5 . . ?
C8 C7 H7A 109.5 . . ?
N4 C7 H7B 109.5 . . ?
C8 C7 H7B 109.5 . . ?
H7A C7 H7B 108.1 . . ?
N5 C8 C7 109.5(9) . . ?
N5 C8 H8A 109.8 . . ?
C7 C8 H8A 109.8 . . ?
N5 C8 H8B 109.8 . . ?
C7 C8 H8B 109.8 . . ?
H8A C8 H8B 108.2 . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        25.09
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         3.464
_refine_diff_density_min         -1.654
_refine_diff_density_rms         0.254
_database_code_depnum_ccdc_archive 'CCDC 1027991'
#######################################################################
#
#                 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_Ib

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H24 N5 O Pr Se3 Sn'
_chemical_formula_sum            'C8 H24 N5 O Pr Se3 Sn'
_chemical_formula_weight         702.82

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sn Sn -0.6537 1.4246 '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           orthorhombic
_symmetry_space_group_name_H-M   Pbca
_symmetry_space_group_name_Hall  '-P 2ac 2ab '

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

_cell_length_a                   12.450(2)
_cell_length_b                   13.617(2)
_cell_length_c                   21.005(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3561.0(10)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    12508
_cell_measurement_theta_min      2.5372
_cell_measurement_theta_max      28.2994

_exptl_crystal_description       sheet
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.622
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2608
_exptl_absorpt_coefficient_mu    10.239
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3088
_exptl_absorpt_correction_T_max  0.5786
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 7.31
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13495
_diffrn_reflns_av_R_equivalents  0.0330
_diffrn_reflns_av_unetI/netI     0.0299
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.42
_diffrn_reflns_theta_max         25.09
_reflns_number_total             3077
_reflns_number_gt                2577
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)'
_computing_cell_refinement       'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)'
_computing_data_reduction        
'CrystalStructure, Ver. 3.60 (Rigaku/MSC, 2004)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL97

_refine_special_details          
; 
 SIMU restraint prevents the thermal ellipsoids of all adjacent 
C and N atoms from adopting different orientations, and DFIX 
restraint makes all the C-C and C-N distances approximately equal.
Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1091P)²+80.0492P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3077
_refine_ls_number_parameters     172
_refine_ls_number_restraints     234
_refine_ls_R_factor_all          0.0615
_refine_ls_R_factor_gt           0.0500
_refine_ls_wR_factor_ref         0.1741
_refine_ls_wR_factor_gt          0.1595
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_restrained_S_all      0.992
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pr1 Pr 0.44959(5) 0.52330(4) 0.41473(3) 0.0206(2) Uani 1 1 d . . .
Sn1 Sn 0.08555(6) 0.53546(6) 0.43807(4) 0.0253(3) Uani 1 1 d . . .
Se3 Se -0.07596(10) 0.62097(9) 0.49180(6) 0.0328(3) Uani 1 1 d . . .
Se1 Se 0.25022(10) 0.62735(10) 0.46722(6) 0.0340(3) Uani 1 1 d . . .
Se2 Se 0.06894(12) 0.50411(12) 0.32284(6) 0.0432(4) Uani 1 1 d . . .
O1W O 0.4879(7) 0.4022(6) 0.4900(3) 0.0306(18) Uani 1 1 d . . .
H1WA H 0.5430 0.3702 0.4782 0.046 Uiso 1 1 d R . .
N1 N 0.3607(10) 0.5716(8) 0.3044(5) 0.0425(19) Uani 1 1 d DU . .
H1A H 0.3915 0.5368 0.2729 0.051 Uiso 1 1 calc R . .
H1B H 0.2902 0.5567 0.3052 0.051 Uiso 1 1 calc R . .
N2 N 0.5011(9) 0.7020(9) 0.3771(5) 0.045(2) Uani 1 1 d DU . .
H2C H 0.4583 0.7435 0.3997 0.054 Uiso 1 1 calc R . .
N3 N 0.6601(9) 0.5538(7) 0.3922(5) 0.0411(18) Uani 1 1 d DU . .
H3C H 0.6932 0.5433 0.4303 0.049 Uiso 1 1 calc R . .
N4 N 0.5443(7) 0.3939(7) 0.3384(5) 0.0361(17) Uani 1 1 d DU . .
H4C H 0.5370 0.4148 0.2974 0.043 Uiso 1 1 calc R . .
N5 N 0.3206(9) 0.3738(8) 0.3800(5) 0.038(2) Uani 1 1 d DU . .
H5A H 0.3037 0.3384 0.4147 0.046 Uiso 1 1 calc R . .
H5B H 0.2593 0.3985 0.3639 0.046 Uiso 1 1 calc R . .
C1 C 0.3739(11) 0.6760(9) 0.2920(8) 0.056(2) Uani 1 1 d DU . .
H1C H 0.3169 0.7107 0.3140 0.067 Uiso 1 1 calc R . .
H1D H 0.3634 0.6867 0.2468 0.067 Uiso 1 1 calc R . .
C2 C 0.4798(12) 0.7228(12) 0.3107(6) 0.057(2) Uani 1 1 d DU . .
H2A H 0.5373 0.6967 0.2845 0.069 Uiso 1 1 calc R . .
H2B H 0.4763 0.7932 0.3040 0.069 Uiso 1 1 calc R . .
C3 C 0.6117(9) 0.7305(10) 0.3921(8) 0.057(2) Uani 1 1 d DU . .
H3A H 0.6176 0.7430 0.4374 0.068 Uiso 1 1 calc R . .
H3B H 0.6287 0.7910 0.3699 0.068 Uiso 1 1 calc R . .
C4 C 0.6916(11) 0.6526(8) 0.3734(8) 0.051(2) Uani 1 1 d DU . .
H4A H 0.7010 0.6542 0.3276 0.061 Uiso 1 1 calc R . .
H4B H 0.7604 0.6680 0.3927 0.061 Uiso 1 1 calc R . .
C5 C 0.7109(11) 0.4854(8) 0.3481(7) 0.044(2) Uani 1 1 d DU . .
H5C H 0.7868 0.4799 0.3581 0.053 Uiso 1 1 calc R . .
H5D H 0.7044 0.5102 0.3050 0.053 Uiso 1 1 calc R . .
C6 C 0.6583(8) 0.3845(9) 0.3526(7) 0.043(2) Uani 1 1 d DU . .
H6A H 0.6917 0.3398 0.3226 0.052 Uiso 1 1 calc R . .
H6B H 0.6677 0.3580 0.3951 0.052 Uiso 1 1 calc R . .
C7 C 0.4897(8) 0.2995(8) 0.3450(7) 0.040(2) Uani 1 1 d DU . .
H7A H 0.5013 0.2743 0.3876 0.048 Uiso 1 1 calc R . .
H7B H 0.5202 0.2530 0.3150 0.048 Uiso 1 1 calc R . .
C8 C 0.3692(8) 0.3089(10) 0.3328(6) 0.042(2) Uani 1 1 d DU . .
H8A H 0.3572 0.3350 0.2904 0.050 Uiso 1 1 calc R . .
H8B H 0.3360 0.2445 0.3351 0.050 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pr1 O1W 2.333(8) . ?
Pr1 O1W 2.375(8) 5_666 ?
Pr1 N2 2.637(11) . ?
Pr1 N1 2.651(11) . ?
Pr1 N4 2.659(10) . ?
Pr1 N5 2.694(11) . ?
Pr1 N3 2.695(11) . ?
Pr1 Se1 3.0633(14) . ?
Pr1 Pr1 3.8483(13) 5_666 ?
Sn1 Se2 2.4663(15) . ?
Sn1 Se1 2.4787(15) . ?
Sn1 Se3 2.5832(15) . ?
Sn1 Se3 2.5927(15) 5_566 ?
Se3 Sn1 2.5927(15) 5_566 ?
O1W Pr1 2.375(8) 5_666 ?
O1W H1WA 0.8500 . ?
N1 C1 1.455(9) . ?
N1 H1A 0.9000 . ?
N1 H1B 0.9000 . ?
N2 C2 1.449(9) . ?
N2 C3 1.465(9) . ?
N2 H2C 0.9100 . ?
N3 C5 1.458(9) . ?
N3 C4 1.458(9) . ?
N3 H3C 0.9100 . ?
N4 C6 1.456(9) . ?
N4 C7 1.461(9) . ?
N4 H4C 0.9100 . ?
N5 C8 1.459(9) . ?
N5 H5A 0.9000 . ?
N5 H5B 0.9000 . ?
C1 C2 1.516(9) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.507(9) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.526(9) . ?
C5 H5C 0.9700 . ?
C5 H5D 0.9700 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C8 1.527(9) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?

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
O1W Pr1 O1W 70.4(3) . 5_666 ?
O1W Pr1 N2 143.6(3) . . ?
O1W Pr1 N2 77.2(3) 5_666 . ?
O1W Pr1 N1 148.5(3) . . ?
O1W Pr1 N1 140.1(3) 5_666 . ?
N2 Pr1 N1 67.1(3) . . ?
O1W Pr1 N4 81.4(3) . . ?
O1W Pr1 N4 130.3(3) 5_666 . ?
N2 Pr1 N4 108.8(3) . . ?
N1 Pr1 N4 79.7(3) . . ?
O1W Pr1 N5 76.8(3) . . ?
O1W Pr1 N5 138.3(3) 5_666 . ?
N2 Pr1 N5 139.6(3) . . ?
N1 Pr1 N5 72.6(3) . . ?
N4 Pr1 N5 66.4(3) . . ?
O1W Pr1 N3 91.6(3) . . ?
O1W Pr1 N3 76.3(3) 5_666 . ?
N2 Pr1 N3 64.5(3) . . ?
N1 Pr1 N3 102.4(4) . . ?
N4 Pr1 N3 64.2(3) . . ?
N5 Pr1 N3 130.4(3) . . ?
O1W Pr1 Se1 104.4(2) . . ?
O1W Pr1 Se1 76.4(2) 5_666 . ?
N2 Pr1 Se1 83.0(3) . . ?
N1 Pr1 Se1 82.0(3) . . ?
N4 Pr1 Se1 152.0(2) . . ?
N5 Pr1 Se1 87.9(2) . . ?
N3 Pr1 Se1 141.2(2) . . ?
O1W Pr1 Pr1 35.54(19) . 5_666 ?
O1W Pr1 Pr1 34.82(19) 5_666 5_666 ?
N2 Pr1 Pr1 110.6(2) . 5_666 ?
N1 Pr1 Pr1 172.2(3) . 5_666 ?
N4 Pr1 Pr1 107.9(2) . 5_666 ?
N5 Pr1 Pr1 108.8(2) . 5_666 ?
N3 Pr1 Pr1 82.6(2) . 5_666 ?
Se1 Pr1 Pr1 90.32(3) . 5_666 ?
Se2 Sn1 Se1 113.53(5) . . ?
Se2 Sn1 Se3 116.20(6) . . ?
Se1 Sn1 Se3 107.96(5) . . ?
Se2 Sn1 Se3 114.30(6) . 5_566 ?
Se1 Sn1 Se3 108.21(5) . 5_566 ?
Se3 Sn1 Se3 94.94(5) . 5_566 ?
Sn1 Se3 Sn1 85.06(5) . 5_566 ?
Sn1 Se1 Pr1 110.35(5) . . ?
Pr1 O1W Pr1 109.6(3) . 5_666 ?
Pr1 O1W H1WA 109.3 . . ?
Pr1 O1W H1WA 101.5 5_666 . ?
C1 N1 Pr1 110.6(8) . . ?
C1 N1 H1A 109.5 . . ?
Pr1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
Pr1 N1 H1B 109.5 . . ?
H1A N1 H1B 108.1 . . ?
C2 N2 C3 109.0(11) . . ?
C2 N2 Pr1 115.1(9) . . ?
C3 N2 Pr1 114.1(8) . . ?
C2 N2 H2C 105.9 . . ?
C3 N2 H2C 105.9 . . ?
Pr1 N2 H2C 105.9 . . ?
C5 N3 C4 107.4(10) . . ?
C5 N3 Pr1 115.8(8) . . ?
C4 N3 Pr1 116.8(8) . . ?
C5 N3 H3C 105.2 . . ?
C4 N3 H3C 105.2 . . ?
Pr1 N3 H3C 105.2 . . ?
C6 N4 C7 110.8(9) . . ?
C6 N4 Pr1 111.5(8) . . ?
C7 N4 Pr1 108.6(7) . . ?
C6 N4 H4C 108.6 . . ?
C7 N4 H4C 108.6 . . ?
Pr1 N4 H4C 108.6 . . ?
C8 N5 Pr1 113.3(7) . . ?
C8 N5 H5A 108.9 . . ?
Pr1 N5 H5A 108.9 . . ?
C8 N5 H5B 108.9 . . ?
Pr1 N5 H5B 108.9 . . ?
H5A N5 H5B 107.7 . . ?
N1 C1 C2 117.6(12) . . ?
N1 C1 H1C 107.9 . . ?
C2 C1 H1C 107.9 . . ?
N1 C1 H1D 107.9 . . ?
C2 C1 H1D 107.9 . . ?
H1C C1 H1D 107.2 . . ?
N2 C2 C1 109.0(11) . . ?
N2 C2 H2A 109.9 . . ?
C1 C2 H2A 109.9 . . ?
N2 C2 H2B 109.9 . . ?
C1 C2 H2B 109.9 . . ?
H2A C2 H2B 108.3 . . ?
N2 C3 C4 112.3(12) . . ?
N2 C3 H3A 109.2 . . ?
C4 C3 H3A 109.2 . . ?
N2 C3 H3B 109.2 . . ?
C4 C3 H3B 109.2 . . ?
H3A C3 H3B 107.9 . . ?
N3 C4 C3 113.7(11) . . ?
N3 C4 H4A 108.8 . . ?
C3 C4 H4A 108.8 . . ?
N3 C4 H4B 108.8 . . ?
C3 C4 H4B 108.8 . . ?
H4A C4 H4B 107.7 . . ?
N3 C5 C6 110.4(10) . . ?
N3 C5 H5C 109.6 . . ?
C6 C5 H5C 109.6 . . ?
N3 C5 H5D 109.6 . . ?
C6 C5 H5D 109.6 . . ?
H5C C5 H5D 108.1 . . ?
N4 C6 C5 109.1(10) . . ?
N4 C6 H6A 109.9 . . ?
C5 C6 H6A 109.9 . . ?
N4 C6 H6B 109.9 . . ?
C5 C6 H6B 109.9 . . ?
H6A C6 H6B 108.3 . . ?
N4 C7 C8 111.6(10) . . ?
N4 C7 H7A 109.3 . . ?
C8 C7 H7A 109.3 . . ?
N4 C7 H7B 109.3 . . ?
C8 C7 H7B 109.3 . . ?
H7A C7 H7B 108.0 . . ?
N5 C8 C7 110.1(10) . . ?
N5 C8 H8A 109.6 . . ?
C7 C8 H8A 109.6 . . ?
N5 C8 H8B 109.6 . . ?
C7 C8 H8B 109.6 . . ?
H8A C8 H8B 108.1 . . ?

_diffrn_measured_fraction_theta_max 0.971
_diffrn_reflns_theta_full        25.09
_diffrn_measured_fraction_theta_full 0.971
_refine_diff_density_max         2.775
_refine_diff_density_min         -1.736
_refine_diff_density_rms         0.313
_database_code_depnum_ccdc_archive 'CCDC 1022709'
#######################################################################
#
#                 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_Ic

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H24 Dy N5 O Se3 Sn'
_chemical_formula_sum            'C8 H24 Dy N5 O Se3 Sn'
_chemical_formula_weight         724.41

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'
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   Pbca
_symmetry_space_group_name_Hall  '-P 2ac 2ab '

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

_cell_length_a                   12.4132(3)
_cell_length_b                   13.5901(4)
_cell_length_c                   20.6722(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3487.33(17)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    11694
_cell_measurement_theta_min      2.970
_cell_measurement_theta_max      28.949

_exptl_crystal_description       sheet
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.759
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2664
_exptl_absorpt_coefficient_mu    11.947
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2223
_exptl_absorpt_correction_T_max  0.5865
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 7.31
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9935
_diffrn_reflns_av_R_equivalents  0.0349
_diffrn_reflns_av_unetI/netI     0.0379
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.97
_diffrn_reflns_theta_max         25.10
_reflns_number_total             3104
_reflns_number_gt                2650
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)'
_computing_cell_refinement       'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)'
_computing_data_reduction        
'CrystalStructure, Ver. 3.60 (Rigaku/MSC, 2004)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL97

_refine_special_details          
; 
 SIMU restraint prevents the thermal ellipsoids of all adjacent 
C and N atoms from adopting different orientations, and 
DFIX restraint makes all the C-C and C-N distances approximately 
equal.Refinement of F² against ALL reflections.  
The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0689P)²+106.6697P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3104
_refine_ls_number_parameters     172
_refine_ls_number_restraints     234
_refine_ls_R_factor_all          0.0658
_refine_ls_R_factor_gt           0.0570
_refine_ls_wR_factor_ref         0.1506
_refine_ls_wR_factor_gt          0.1444
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_restrained_S_all      1.050
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.54600(4) 0.52119(4) 0.41530(3) 0.0177(2) Uani 1 1 d . . .
Sn1 Sn 0.91229(7) 0.53376(7) 0.43794(4) 0.0236(2) Uani 1 1 d . . .
Se1 Se 0.74330(10) 0.61860(11) 0.46858(7) 0.0312(3) Uani 1 1 d . . .
Se2 Se 0.92808(13) 0.50477(13) 0.32086(7) 0.0400(4) Uani 1 1 d . . .
Se3 Se 1.07142(11) 0.62392(10) 0.49206(7) 0.0311(3) Uani 1 1 d . . .
O1W O 0.4941(7) 0.5944(6) 0.5099(4) 0.0241(18) Uani 1 1 d . . .
H1WA H 0.4275 0.5836 0.5162 0.036 Uiso 1 1 d R . .
N1 N 0.6372(10) 0.5596(8) 0.3079(6) 0.0404(19) Uani 1 1 d DU . .
H1A H 0.7083 0.5488 0.3127 0.049 Uiso 1 1 calc R . .
H1B H 0.6129 0.5162 0.2784 0.049 Uiso 1 1 calc R . .
N2 N 0.5073(8) 0.6959(9) 0.3781(6) 0.041(2) Uani 1 1 d DU . .
H2C H 0.5103 0.7354 0.4136 0.050 Uiso 1 1 calc R . .
N3 N 0.3429(9) 0.5522(8) 0.3974(6) 0.0377(19) Uani 1 1 d DU . .
H3C H 0.3117 0.5352 0.4356 0.045 Uiso 1 1 calc R . .
N4 N 0.4567(8) 0.3970(8) 0.3400(6) 0.0345(18) Uani 1 1 d DU . .
H4C H 0.4657 0.4193 0.2988 0.041 Uiso 1 1 calc R . .
N5 N 0.6739(9) 0.3766(8) 0.3859(5) 0.035(2) Uani 1 1 d DU . .
H5A H 0.7371 0.4014 0.3722 0.042 Uiso 1 1 calc R . .
H5B H 0.6869 0.3410 0.4217 0.042 Uiso 1 1 calc R . .
C1 C 0.6234(14) 0.6576(9) 0.2815(7) 0.051(3) Uani 1 1 d DU . .
H1C H 0.5687 0.6561 0.2480 0.061 Uiso 1 1 calc R . .
H1D H 0.6904 0.6790 0.2619 0.061 Uiso 1 1 calc R . .
C2 C 0.5909(12) 0.7294(11) 0.3331(7) 0.054(2) Uani 1 1 d DU . .
H2A H 0.6544 0.7466 0.3579 0.065 Uiso 1 1 calc R . .
H2B H 0.5656 0.7890 0.3122 0.065 Uiso 1 1 calc R . .
C3 C 0.4017(9) 0.7080(13) 0.3495(8) 0.051(2) Uani 1 1 d DU . .
H3A H 0.4019 0.6812 0.3060 0.062 Uiso 1 1 calc R . .
H3B H 0.3847 0.7776 0.3465 0.062 Uiso 1 1 calc R . .
C4 C 0.3163(11) 0.6565(9) 0.3893(8) 0.046(2) Uani 1 1 d DU . .
H4A H 0.3112 0.6876 0.4315 0.055 Uiso 1 1 calc R . .
H4B H 0.2470 0.6627 0.3681 0.055 Uiso 1 1 calc R . .
C5 C 0.2892(12) 0.4897(9) 0.3493(7) 0.042(2) Uani 1 1 d DU . .
H5C H 0.2970 0.5180 0.3065 0.050 Uiso 1 1 calc R . .
H5D H 0.2130 0.4846 0.3591 0.050 Uiso 1 1 calc R . .
C6 C 0.3410(8) 0.3886(9) 0.3514(7) 0.038(2) Uani 1 1 d DU . .
H6A H 0.3284 0.3587 0.3934 0.046 Uiso 1 1 calc R . .
H6B H 0.3089 0.3467 0.3187 0.046 Uiso 1 1 calc R . .
C7 C 0.5103(9) 0.3013(9) 0.3443(7) 0.037(2) Uani 1 1 d DU . .
H7A H 0.4819 0.2578 0.3112 0.044 Uiso 1 1 calc R . .
H7B H 0.4953 0.2720 0.3862 0.044 Uiso 1 1 calc R . .
C8 C 0.6307(9) 0.3115(11) 0.3357(6) 0.039(2) Uani 1 1 d DU . .
H8A H 0.6646 0.2473 0.3388 0.047 Uiso 1 1 calc R . .
H8B H 0.6463 0.3385 0.2933 0.047 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 O1W 2.259(8) 5_666 ?
Dy1 O1W 2.288(8) . ?
Dy1 N2 2.541(12) . ?
Dy1 N1 2.546(12) . ?
Dy1 N4 2.550(11) . ?
Dy1 N3 2.583(11) . ?
Dy1 N5 2.598(11) . ?
Dy1 Se1 2.9938(14) . ?
Dy1 Dy1 3.7281(11) 5_666 ?
Sn1 Se2 2.4599(17) . ?
Sn1 Se1 2.4761(15) . ?
Sn1 Se3 2.5797(16) . ?
Sn1 Se3 2.5936(16) 5_766 ?
Se3 Sn1 2.5936(16) 5_766 ?
O1W Dy1 2.259(8) 5_666 ?
O1W H1WA 0.8500 . ?
N1 C1 1.450(9) . ?
N1 H1A 0.9000 . ?
N1 H1B 0.9000 . ?
N2 C3 1.448(9) . ?
N2 C2 1.466(9) . ?
N2 H2C 0.9100 . ?
N3 C4 1.465(9) . ?
N3 C5 1.468(9) . ?
N3 H3C 0.9100 . ?
N4 C6 1.461(9) . ?
N4 C7 1.464(9) . ?
N4 H4C 0.9100 . ?
N5 C8 1.464(9) . ?
N5 H5A 0.9000 . ?
N5 H5B 0.9000 . ?
C1 C2 1.501(9) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.514(9) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.517(9) . ?
C5 H5C 0.9700 . ?
C5 H5D 0.9700 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C8 1.512(9) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?

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
O1W Dy1 O1W 69.8(4) 5_666 . ?
O1W Dy1 N2 144.6(3) 5_666 . ?
O1W Dy1 N2 78.4(4) . . ?
O1W Dy1 N1 146.8(3) 5_666 . ?
O1W Dy1 N1 141.4(3) . . ?
N2 Dy1 N1 68.2(4) . . ?
O1W Dy1 N4 82.0(3) 5_666 . ?
O1W Dy1 N4 133.5(3) . . ?
N2 Dy1 N4 110.6(4) . . ?
N1 Dy1 N4 78.2(4) . . ?
O1W Dy1 N3 89.8(3) 5_666 . ?
O1W Dy1 N3 77.1(3) . . ?
N2 Dy1 N3 67.7(3) . . ?
N1 Dy1 N3 106.0(4) . . ?
N4 Dy1 N3 66.2(3) . . ?
O1W Dy1 N5 76.6(3) 5_666 . ?
O1W Dy1 N5 134.5(3) . . ?
N2 Dy1 N5 138.7(4) . . ?
N1 Dy1 N5 71.3(4) . . ?
N4 Dy1 N5 67.8(3) . . ?
N3 Dy1 N5 133.3(3) . . ?
O1W Dy1 Se1 103.7(2) 5_666 . ?
O1W Dy1 Se1 73.9(2) . . ?
N2 Dy1 Se1 81.5(3) . . ?
N1 Dy1 Se1 82.3(3) . . ?
N4 Dy1 Se1 150.8(2) . . ?
N3 Dy1 Se1 141.2(2) . . ?
N5 Dy1 Se1 85.5(2) . . ?
O1W Dy1 Dy1 35.2(2) 5_666 5_666 ?
O1W Dy1 Dy1 34.7(2) . 5_666 ?
N2 Dy1 Dy1 111.8(3) . 5_666 ?
N1 Dy1 Dy1 170.7(3) . 5_666 ?
N4 Dy1 Dy1 109.8(3) . 5_666 ?
N3 Dy1 Dy1 82.0(3) . 5_666 ?
N5 Dy1 Dy1 106.9(3) . 5_666 ?
Se1 Dy1 Dy1 88.48(3) . 5_666 ?
Se2 Sn1 Se1 113.19(6) . . ?
Se2 Sn1 Se3 116.21(6) . . ?
Se1 Sn1 Se3 108.46(6) . . ?
Se2 Sn1 Se3 114.23(6) . 5_766 ?
Se1 Sn1 Se3 107.94(6) . 5_766 ?
Se3 Sn1 Se3 95.21(5) . 5_766 ?
Sn1 Se1 Dy1 113.14(5) . . ?
Sn1 Se3 Sn1 84.79(5) . 5_766 ?
Dy1 O1W Dy1 110.2(4) 5_666 . ?
Dy1 O1W H1WA 63.9 5_666 . ?
Dy1 O1W H1WA 109.2 . . ?
C1 N1 Dy1 117.6(9) . . ?
C1 N1 H1A 107.9 . . ?
Dy1 N1 H1A 107.9 . . ?
C1 N1 H1B 107.9 . . ?
Dy1 N1 H1B 107.9 . . ?
H1A N1 H1B 107.2 . . ?
C3 N2 C2 110.2(11) . . ?
C3 N2 Dy1 113.7(9) . . ?
C2 N2 Dy1 110.4(9) . . ?
C3 N2 H2C 107.4 . . ?
C2 N2 H2C 107.4 . . ?
Dy1 N2 H2C 107.4 . . ?
C4 N3 C5 112.4(11) . . ?
C4 N3 Dy1 113.2(8) . . ?
C5 N3 Dy1 116.5(8) . . ?
C4 N3 H3C 104.4 . . ?
C5 N3 H3C 104.4 . . ?
Dy1 N3 H3C 104.4 . . ?
C6 N4 C7 111.5(9) . . ?
C6 N4 Dy1 112.3(8) . . ?
C7 N4 Dy1 110.7(8) . . ?
C6 N4 H4C 107.3 . . ?
C7 N4 H4C 107.3 . . ?
Dy1 N4 H4C 107.3 . . ?
C8 N5 Dy1 113.5(8) . . ?
C8 N5 H5A 108.9 . . ?
Dy1 N5 H5A 108.9 . . ?
C8 N5 H5B 108.9 . . ?
Dy1 N5 H5B 108.9 . . ?
H5A N5 H5B 107.7 . . ?
N1 C1 C2 111.2(12) . . ?
N1 C1 H1C 109.4 . . ?
C2 C1 H1C 109.4 . . ?
N1 C1 H1D 109.4 . . ?
C2 C1 H1D 109.4 . . ?
H1C C1 H1D 108.0 . . ?
N2 C2 C1 116.0(13) . . ?
N2 C2 H2A 108.3 . . ?
C1 C2 H2A 108.3 . . ?
N2 C2 H2B 108.3 . . ?
C1 C2 H2B 108.3 . . ?
H2A C2 H2B 107.4 . . ?
N2 C3 C4 111.0(11) . . ?
N2 C3 H3A 109.4 . . ?
C4 C3 H3A 109.4 . . ?
N2 C3 H3B 109.4 . . ?
C4 C3 H3B 109.4 . . ?
H3A C3 H3B 108.0 . . ?
N3 C4 C3 110.6(12) . . ?
N3 C4 H4A 109.5 . . ?
C3 C4 H4A 109.5 . . ?
N3 C4 H4B 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 108.1 . . ?
N3 C5 C6 108.2(11) . . ?
N3 C5 H5C 110.1 . . ?
C6 C5 H5C 110.1 . . ?
N3 C5 H5D 110.1 . . ?
C6 C5 H5D 110.1 . . ?
H5C C5 H5D 108.4 . . ?
N4 C6 C5 109.9(11) . . ?
N4 C6 H6A 109.7 . . ?
C5 C6 H6A 109.7 . . ?
N4 C6 H6B 109.7 . . ?
C5 C6 H6B 109.7 . . ?
H6A C6 H6B 108.2 . . ?
N4 C7 C8 111.1(10) . . ?
N4 C7 H7A 109.4 . . ?
C8 C7 H7A 109.4 . . ?
N4 C7 H7B 109.4 . . ?
C8 C7 H7B 109.4 . . ?
H7A C7 H7B 108.0 . . ?
N5 C8 C7 109.5(10) . . ?
N5 C8 H8A 109.8 . . ?
C7 C8 H8A 109.8 . . ?
N5 C8 H8B 109.8 . . ?
C7 C8 H8B 109.8 . . ?
H8A C8 H8B 108.2 . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.10
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         6.600
_refine_diff_density_min         -1.767
_refine_diff_density_rms         0.313
_database_code_depnum_ccdc_archive 'CCDC 1022710'
#######################################################################
#
#                 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_Id

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H24 Er N5 O Se3 Sn'
_chemical_formula_sum            'C8 H24 Er N5 O Se3 Sn'
_chemical_formula_weight         729.17

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'
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   Pbca
_symmetry_space_group_name_Hall  '-P 2ac 2ab '

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

_cell_length_a                   12.4182(10)
_cell_length_b                   13.6053(11)
_cell_length_c                   20.6357(17)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3486.5(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    11606
_cell_measurement_theta_min      3.1531
_cell_measurement_theta_max      28.2812

_exptl_crystal_description       sheet
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.778
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2680
_exptl_absorpt_coefficient_mu    12.477
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3407
_exptl_absorpt_correction_T_max  0.4351
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 7.31
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13101
_diffrn_reflns_av_R_equivalents  0.0416
_diffrn_reflns_av_unetI/netI     0.0389
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.43
_diffrn_reflns_theta_max         25.09
_reflns_number_total             3016
_reflns_number_gt                2520
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)'
_computing_cell_refinement       'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)'
_computing_data_reduction        
'CrystalStructure, Ver. 3.60 (Rigaku/MSC, 2004)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL97

_refine_special_details          
; 
SIMU restraint prevents the thermal ellipsoids of all adjacent C and 
N atoms from adopting different orientations, and 
DFIX restraint makes all the C-C and C-N distances 
approximately equal. Refinement of F² against ALL reflections.  
The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1342P)²+162.8718P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3016
_refine_ls_number_parameters     172
_refine_ls_number_restraints     228
_refine_ls_R_factor_all          0.0858
_refine_ls_R_factor_gt           0.0702
_refine_ls_wR_factor_ref         0.2337
_refine_ls_wR_factor_gt          0.1938
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_restrained_S_all      1.077
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Er1 Er 0.04504(6) 0.02088(5) 0.58449(4) 0.0182(3) Uani 1 1 d . . .
Sn1 Sn 0.41199(10) 0.03351(9) 0.56225(6) 0.0254(4) Uani 1 1 d . . .
Se3 Se 0.57012(16) 0.12427(13) 0.50761(10) 0.0324(5) Uani 1 1 d . . .
Se1 Se 0.24162(15) 0.11634(14) 0.53127(9) 0.0327(5) Uani 1 1 d . . .
Se2 Se 0.42703(19) 0.00525(17) 0.67965(10) 0.0401(5) Uani 1 1 d . . .
O1W O 0.0086(10) -0.0922(8) 0.5105(5) 0.025(2) Uani 1 1 d . . .
H1WA H -0.0474 -0.1237 0.5218 0.037 Uiso 1 1 d R . .
N1 N 0.1381(14) 0.0585(11) 0.6922(9) 0.041(2) Uani 1 1 d DU . .
H1A H 0.1171 0.0129 0.7212 0.049 Uiso 1 1 calc R . .
H1B H 0.2095 0.0513 0.6865 0.049 Uiso 1 1 calc R . .
N2 N 0.0088(10) 0.1955(13) 0.6217(8) 0.040(2) Uani 1 1 d DU . .
H2C H 0.0120 0.2348 0.5861 0.049 Uiso 1 1 calc R . .
N3 N -0.1558(12) 0.0529(10) 0.6015(8) 0.037(2) Uani 1 1 d DU . .
H3C H -0.1863 0.0351 0.5632 0.044 Uiso 1 1 calc R . .
N4 N -0.0435(10) -0.1035(10) 0.6595(9) 0.036(2) Uani 1 1 d DU . .
H4C H -0.0332 -0.0820 0.7008 0.044 Uiso 1 1 calc R . .
N5 N 0.1707(12) -0.1214(11) 0.6127(8) 0.034(2) Uani 1 1 d DU . .
H5A H 0.1830 -0.1563 0.5764 0.041 Uiso 1 1 calc R . .
H5B H 0.2342 -0.0962 0.6256 0.041 Uiso 1 1 calc R . .
C1 C 0.1193(18) 0.1553(11) 0.7207(9) 0.047(3) Uani 1 1 d DU . .
H1C H 0.1826 0.1766 0.7444 0.056 Uiso 1 1 calc R . .
H1D H 0.0591 0.1525 0.7505 0.056 Uiso 1 1 calc R . .
C2 C 0.0950(15) 0.2271(14) 0.6658(9) 0.048(3) Uani 1 1 d DU . .
H2A H 0.0752 0.2899 0.6845 0.057 Uiso 1 1 calc R . .
H2B H 0.1602 0.2370 0.6407 0.057 Uiso 1 1 calc R . .
C3 C -0.0972(11) 0.2086(17) 0.6505(10) 0.047(2) Uani 1 1 d DU . .
H3A H -0.1138 0.2780 0.6542 0.057 Uiso 1 1 calc R . .
H3B H -0.0990 0.1797 0.6934 0.057 Uiso 1 1 calc R . .
C4 C -0.1789(15) 0.1581(11) 0.6066(11) 0.043(2) Uani 1 1 d DU . .
H4A H -0.2508 0.1673 0.6240 0.052 Uiso 1 1 calc R . .
H4B H -0.1766 0.1876 0.5638 0.052 Uiso 1 1 calc R . .
C5 C -0.2124(16) -0.0072(12) 0.6496(10) 0.041(3) Uani 1 1 d DU . .
H5C H -0.2882 -0.0123 0.6386 0.049 Uiso 1 1 calc R . .
H5D H -0.2062 0.0222 0.6922 0.049 Uiso 1 1 calc R . .
C6 C -0.1598(11) -0.1094(12) 0.6490(11) 0.039(2) Uani 1 1 d DU . .
H6A H -0.1919 -0.1496 0.6827 0.047 Uiso 1 1 calc R . .
H6B H -0.1738 -0.1408 0.6077 0.047 Uiso 1 1 calc R . .
C7 C 0.0108(11) -0.1985(11) 0.6539(11) 0.037(3) Uani 1 1 d DU . .
H7A H -0.0038 -0.2263 0.6115 0.044 Uiso 1 1 calc R . .
H7B H -0.0177 -0.2432 0.6862 0.044 Uiso 1 1 calc R . .
C8 C 0.1324(12) -0.1890(14) 0.6630(9) 0.040(3) Uani 1 1 d DU . .
H8A H 0.1487 -0.1631 0.7057 0.048 Uiso 1 1 calc R . .
H8B H 0.1669 -0.2526 0.6585 0.048 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Er1 O1W 2.214(11) . ?
Er1 O1W 2.286(11) 5_556 ?
Er1 N2 2.538(16) . ?
Er1 N4 2.544(16) . ?
Er1 N5 2.553(15) . ?
Er1 N3 2.556(15) . ?
Er1 N1 2.558(17) . ?
Er1 Se1 2.975(2) . ?
Er1 Er1 3.7058(15) 5_556 ?
Sn1 Se2 2.460(2) . ?
Sn1 Se1 2.481(2) . ?
Sn1 Se3 2.579(2) . ?
Sn1 Se3 2.595(2) 5_656 ?
Se3 Sn1 2.595(2) 5_656 ?
O1W Er1 2.286(11) 5_556 ?
O1W H1WA 0.8501 . ?
N1 C1 1.459(9) . ?
N1 H1A 0.9000 . ?
N1 H1B 0.9000 . ?
N2 C3 1.455(9) . ?
N2 C2 1.468(9) . ?
N2 H2C 0.9100 . ?
N3 C4 1.463(9) . ?
N3 C5 1.465(9) . ?
N3 H3C 0.9100 . ?
N4 C7 1.463(9) . ?
N4 C6 1.463(9) . ?
N4 H4C 0.9100 . ?
N5 C8 1.466(9) . ?
N5 H5A 0.9000 . ?
N5 H5B 0.9000 . ?
C1 C2 1.526(10) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.524(9) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.535(9) . ?
C5 H5C 0.9700 . ?
C5 H5D 0.9700 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C8 1.527(9) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?

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
O1W Er1 O1W 69.1(5) . 5_556 ?
O1W Er1 N2 145.4(5) . . ?
O1W Er1 N2 79.1(5) 5_556 . ?
O1W Er1 N4 82.5(5) . . ?
O1W Er1 N4 132.7(4) 5_556 . ?
N2 Er1 N4 111.2(5) . . ?
O1W Er1 N5 75.8(5) . . ?
O1W Er1 N5 134.0(5) 5_556 . ?
N2 Er1 N5 138.5(5) . . ?
N4 Er1 N5 67.7(4) . . ?
O1W Er1 N3 90.8(5) . . ?
O1W Er1 N3 76.2(5) 5_556 . ?
N2 Er1 N3 68.0(4) . . ?
N4 Er1 N3 66.9(4) . . ?
N5 Er1 N3 134.0(4) . . ?
O1W Er1 N1 146.2(5) . . ?
O1W Er1 N1 142.4(5) 5_556 . ?
N2 Er1 N1 68.2(5) . . ?
N4 Er1 N1 78.4(5) . . ?
N5 Er1 N1 71.2(5) . . ?
N3 Er1 N1 106.7(5) . . ?
O1W Er1 Se1 102.5(3) . . ?
O1W Er1 Se1 74.8(3) 5_556 . ?
N2 Er1 Se1 81.3(3) . . ?
N4 Er1 Se1 150.4(3) . . ?
N5 Er1 Se1 85.0(3) . . ?
N3 Er1 Se1 141.0(3) . . ?
N1 Er1 Se1 82.1(4) . . ?
O1W Er1 Er1 35.2(3) . 5_556 ?
O1W Er1 Er1 33.9(3) 5_556 5_556 ?
N2 Er1 Er1 112.0(4) . 5_556 ?
N4 Er1 Er1 109.9(4) . 5_556 ?
N5 Er1 Er1 106.4(4) . 5_556 ?
N3 Er1 Er1 82.0(4) . 5_556 ?
N1 Er1 Er1 170.1(4) . 5_556 ?
Se1 Er1 Er1 88.12(5) . 5_556 ?
Se2 Sn1 Se1 112.92(8) . . ?
Se2 Sn1 Se3 116.59(9) . . ?
Se1 Sn1 Se3 108.61(8) . . ?
Se2 Sn1 Se3 114.29(8) . 5_656 ?
Se1 Sn1 Se3 107.79(8) . 5_656 ?
Se3 Sn1 Se3 95.05(7) . 5_656 ?
Sn1 Se3 Sn1 84.95(7) . 5_656 ?
Sn1 Se1 Er1 113.97(7) . . ?
Er1 O1W Er1 110.9(5) . 5_556 ?
Er1 O1W H1WA 109.2 . . ?
Er1 O1W H1WA 102.2 5_556 . ?
C1 N1 Er1 117.2(12) . . ?
C1 N1 H1A 108.0 . . ?
Er1 N1 H1A 108.0 . . ?
C1 N1 H1B 108.0 . . ?
Er1 N1 H1B 108.0 . . ?
H1A N1 H1B 107.2 . . ?
C3 N2 C2 111.8(15) . . ?
C3 N2 Er1 113.5(12) . . ?
C2 N2 Er1 109.4(12) . . ?
C3 N2 H2C 107.3 . . ?
C2 N2 H2C 107.3 . . ?
Er1 N2 H2C 107.3 . . ?
C4 N3 C5 113.8(15) . . ?
C4 N3 Er1 111.6(11) . . ?
C5 N3 Er1 117.8(11) . . ?
C4 N3 H3C 103.9 . . ?
C5 N3 H3C 103.9 . . ?
Er1 N3 H3C 103.9 . . ?
C7 N4 C6 113.3(12) . . ?
C7 N4 Er1 109.9(11) . . ?
C6 N4 Er1 111.9(11) . . ?
C7 N4 H4C 107.1 . . ?
C6 N4 H4C 107.1 . . ?
Er1 N4 H4C 107.1 . . ?
C8 N5 Er1 116.0(11) . . ?
C8 N5 H5A 108.3 . . ?
Er1 N5 H5A 108.3 . . ?
C8 N5 H5B 108.3 . . ?
Er1 N5 H5B 108.3 . . ?
H5A N5 H5B 107.4 . . ?
N1 C1 C2 108.1(16) . . ?
N1 C1 H1C 110.1 . . ?
C2 C1 H1C 110.1 . . ?
N1 C1 H1D 110.1 . . ?
C2 C1 H1D 110.1 . . ?
H1C C1 H1D 108.4 . . ?
N2 C2 C1 114.6(16) . . ?
N2 C2 H2A 108.6 . . ?
C1 C2 H2A 108.6 . . ?
N2 C2 H2B 108.6 . . ?
C1 C2 H2B 108.6 . . ?
H2A C2 H2B 107.6 . . ?
N2 C3 C4 107.8(14) . . ?
N2 C3 H3A 110.2 . . ?
C4 C3 H3A 110.2 . . ?
N2 C3 H3B 110.2 . . ?
C4 C3 H3B 110.2 . . ?
H3A C3 H3B 108.5 . . ?
N3 C4 C3 110.7(16) . . ?
N3 C4 H4A 109.5 . . ?
C3 C4 H4A 109.5 . . ?
N3 C4 H4B 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 108.1 . . ?
N3 C5 C6 107.2(14) . . ?
N3 C5 H5C 110.3 . . ?
C6 C5 H5C 110.3 . . ?
N3 C5 H5D 110.3 . . ?
C6 C5 H5D 110.3 . . ?
H5C C5 H5D 108.5 . . ?
N4 C6 C5 111.7(14) . . ?
N4 C6 H6A 109.3 . . ?
C5 C6 H6A 109.3 . . ?
N4 C6 H6B 109.3 . . ?
C5 C6 H6B 109.3 . . ?
H6A C6 H6B 107.9 . . ?
N4 C7 C8 111.8(13) . . ?
N4 C7 H7A 109.3 . . ?
C8 C7 H7A 109.3 . . ?
N4 C7 H7B 109.3 . . ?
C8 C7 H7B 109.3 . . ?
H7A C7 H7B 107.9 . . ?
N5 C8 C7 106.6(13) . . ?
N5 C8 H8A 110.4 . . ?
C7 C8 H8A 110.4 . . ?
N5 C8 H8B 110.4 . . ?
C7 C8 H8B 110.4 . . ?
H8A C8 H8B 108.6 . . ?

_diffrn_measured_fraction_theta_max 0.972
_diffrn_reflns_theta_full        25.09
_diffrn_measured_fraction_theta_full 0.972
_refine_diff_density_max         6.800
_refine_diff_density_min         -2.308
_refine_diff_density_rms         0.532
_database_code_depnum_ccdc_archive 'CCDC 1022711'
#######################################################################
#
#                 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_Ie

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H24 N5 O Se3 Sn Tm'
_chemical_formula_sum            'C8 H24 N5 O Se3 Sn Tm'
_chemical_formula_weight         730.84

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tm Tm -0.3139 5.2483 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   Pbca
_symmetry_space_group_name_Hall  '-P 2ac 2ab '

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

_cell_length_a                   12.399(3)
_cell_length_b                   13.518(4)
_cell_length_c                   20.504(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3436.7(17)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       sheet
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.820
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2678
_exptl_absorpt_coefficient_mu    12.937
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.303
_exptl_absorpt_correction_T_max  0.465
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 7.31
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14156
_diffrn_reflns_av_R_equivalents  0.0473
_diffrn_reflns_av_unetI/netI     0.0383
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.99
_diffrn_reflns_theta_max         25.10
_reflns_number_total             3036
_reflns_number_gt                2825
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)'
_computing_cell_refinement       'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)'
_computing_data_reduction        
'CrystalStructure, Ver. 3.60 (Rigaku/MSC, 2004)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL97

_refine_special_details          
; 
SIMU restraint prevents the thermal ellipsoids of all adjacent C and N 
atoms from adopting different orientations, and DFIX restraint makes all 
the C-C and C-N distances approximately equal. 
Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0640P)²+208.8991P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3036
_refine_ls_number_parameters     172
_refine_ls_number_restraints     234
_refine_ls_R_factor_all          0.0661
_refine_ls_R_factor_gt           0.0626
_refine_ls_wR_factor_ref         0.1581
_refine_ls_wR_factor_gt          0.1559
_refine_ls_goodness_of_fit_ref   1.144
_refine_ls_restrained_S_all      1.107
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Tm1 Tm 0.54500(4) 0.52043(4) 0.58461(3) 0.0073(2) Uani 1 1 d . . 1
Sn1 Sn 0.91152(7) 0.53406(7) 0.56232(5) 0.0132(3) Uani 1 1 d . . 1
Se1 Se 0.74131(11) 0.61760(11) 0.53106(7) 0.0163(3) Uani 1 1 d . A 1
Se2 Se 0.92615(13) 0.50528(12) 0.68052(7) 0.0217(4) Uani 1 1 d . B 1
Se3 Se 1.07090(12) 0.62509(11) 0.50793(7) 0.0173(3) Uani 1 1 d . . 1
O1W O 0.5061(7) 0.4076(7) 0.5099(4) 0.0124(19) Uani 1 1 d . . 1
H1WA H 0.4501 0.3759 0.5215 0.019 Uiso 1 1 d R . 1
N3 N 0.3438(10) 0.5526(8) 0.6009(6) 0.0200(19) Uani 1 1 d DU C 1
H3C H 0.3133 0.5348 0.5622 0.024 Uiso 1 1 calc R C 1
N5 N 0.6713(10) 0.3797(9) 0.6124(6) 0.019(2) Uani 1 1 d DU C 1
H5A H 0.6836 0.3444 0.5760 0.023 Uiso 1 1 calc R C 1
H5B H 0.7348 0.4055 0.6253 0.023 Uiso 1 1 calc R C 1
N4 N 0.4573(8) 0.3964(8) 0.6597(6) 0.0200(18) Uani 1 1 d DU C 1
H4C H 0.4672 0.4189 0.7011 0.024 Uiso 1 1 calc R C 1
N1 N 0.6373(11) 0.5580(9) 0.6917(6) 0.0241(19) Uani 1 1 d DU C 1
H1A H 0.6143 0.5137 0.7213 0.029 Uiso 1 1 calc R C 1
H1B H 0.7086 0.5483 0.6864 0.029 Uiso 1 1 calc R C 1
N2 N 0.5106(9) 0.6948(10) 0.6208(6) 0.025(2) Uani 1 1 d DU C 1
H2C H 0.5138 0.7337 0.5846 0.030 Uiso 1 1 calc R C 1
C6 C 0.3410(9) 0.3881(10) 0.6497(8) 0.022(2) Uani 1 1 d DU C 1
H6A H 0.3096 0.3485 0.6843 0.026 Uiso 1 1 calc R C 1
H6B H 0.3268 0.3553 0.6085 0.026 Uiso 1 1 calc R C 1
C7 C 0.5115(9) 0.3006(9) 0.6556(8) 0.022(2) Uani 1 1 d DU C 1
H7A H 0.4959 0.2703 0.6137 0.026 Uiso 1 1 calc R C 1
H7B H 0.4842 0.2572 0.6895 0.026 Uiso 1 1 calc R C 1
C8 C 0.6325(10) 0.3124(11) 0.6633(7) 0.023(2) Uani 1 1 d DU C 1
H8A H 0.6490 0.3392 0.7061 0.027 Uiso 1 1 calc R C 1
H8B H 0.6678 0.2487 0.6592 0.027 Uiso 1 1 calc R C 1
C5 C 0.2897(12) 0.4903(9) 0.6494(7) 0.024(2) Uani 1 1 d DU C 1
H5C H 0.2136 0.4848 0.6389 0.029 Uiso 1 1 calc R C 1
H5D H 0.2961 0.5201 0.6922 0.029 Uiso 1 1 calc R C 1
C4 C 0.3190(12) 0.6580(9) 0.6072(8) 0.027(2) Uani 1 1 d DU C 1
H4A H 0.2486 0.6662 0.6271 0.033 Uiso 1 1 calc R C 1
H4B H 0.3174 0.6885 0.5644 0.033 Uiso 1 1 calc R C 1
C1 C 0.6220(14) 0.6568(9) 0.7191(7) 0.032(2) Uani 1 1 d DU C 1
H1C H 0.6872 0.6776 0.7414 0.038 Uiso 1 1 calc R C 1
H1D H 0.5637 0.6556 0.7506 0.038 Uiso 1 1 calc R C 1
C2 C 0.5958(12) 0.7287(11) 0.6652(7) 0.032(2) Uani 1 1 d DU C 1
H2A H 0.5737 0.7910 0.6846 0.039 Uiso 1 1 calc R C 1
H2B H 0.6607 0.7410 0.6401 0.039 Uiso 1 1 calc R C 1
C3 C 0.4039(9) 0.7077(13) 0.6490(7) 0.030(2) Uani 1 1 d DU C 1
H3A H 0.3879 0.7777 0.6526 0.036 Uiso 1 1 calc R C 1
H3B H 0.4026 0.6794 0.6925 0.036 Uiso 1 1 calc R C 1


_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
Tm1 O1W 2.216(9) . ?
Tm1 O1W 2.259(9) 5_666 ?
Tm1 N2 2.508(13) . ?
Tm1 N4 2.522(12) . ?
Tm1 N1 2.528(12) . ?
Tm1 N5 2.529(12) . ?
Tm1 N3 2.554(12) . ?
Tm1 Se1 2.9758(16) . ?
Tm1 Tm1 3.6864(14) 5_666 ?
Sn1 Se2 2.4614(18) . ?
Sn1 Se1 2.4780(17) . ?
Sn1 Se3 2.5813(17) . ?
Sn1 Se3 2.5982(18) 5_766 ?
Se3 Sn1 2.5982(18) 5_766 ?
O1W Tm1 2.259(9) 5_666 ?
O1W H1WA 0.8500 . ?
N3 C4 1.463(9) . ?
N3 C5 1.467(9) . ?
N3 H3C 0.9100 . ?
N5 C8 1.466(9) . ?
N5 H5A 0.9000 . ?
N5 H5B 0.9000 . ?
N4 C6 1.461(9) . ?
N4 C7 1.461(9) . ?
N4 H4C 0.9100 . ?
N1 C1 1.460(9) . ?
N1 H1A 0.9000 . ?
N1 H1B 0.9000 . ?
N2 C3 1.454(9) . ?
N2 C2 1.468(9) . ?
N2 H2C 0.9100 . ?
C6 C5 1.521(9) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C8 1.518(9) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C5 H5C 0.9700 . ?
C5 H5D 0.9700 . ?
C4 C3 1.514(9) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C1 C2 1.507(9) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?

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
O1W Tm1 O1W 69.1(4) . 5_666 ?
O1W Tm1 N2 144.6(4) . . ?
O1W Tm1 N2 78.5(4) 5_666 . ?
O1W Tm1 N4 82.6(4) . . ?
O1W Tm1 N4 133.5(3) 5_666 . ?
N2 Tm1 N4 111.8(4) . . ?
O1W Tm1 N1 146.9(4) . . ?
O1W Tm1 N1 141.8(4) 5_666 . ?
N2 Tm1 N1 68.3(4) . . ?
N4 Tm1 N1 78.4(4) . . ?
O1W Tm1 N5 76.9(4) . . ?
O1W Tm1 N5 133.7(4) 5_666 . ?
N2 Tm1 N5 138.2(4) . . ?
N4 Tm1 N5 68.2(3) . . ?
N1 Tm1 N5 71.0(4) . . ?
O1W Tm1 N3 89.7(4) . . ?
O1W Tm1 N3 76.4(3) 5_666 . ?
N2 Tm1 N3 68.6(3) . . ?
N4 Tm1 N3 67.2(3) . . ?
N1 Tm1 N3 107.1(4) . . ?
N5 Tm1 N3 134.7(3) . . ?
O1W Tm1 Se1 103.1(2) . . ?
O1W Tm1 Se1 73.9(2) 5_666 . ?
N2 Tm1 Se1 80.4(3) . . ?
N4 Tm1 Se1 150.6(2) . . ?
N1 Tm1 Se1 82.0(3) . . ?
N5 Tm1 Se1 84.8(3) . . ?
N3 Tm1 Se1 140.5(2) . . ?
O1W Tm1 Tm1 34.9(2) . 5_666 ?
O1W Tm1 Tm1 34.1(2) 5_666 5_666 ?
N2 Tm1 Tm1 111.6(3) . 5_666 ?
N4 Tm1 Tm1 110.1(3) . 5_666 ?
N1 Tm1 Tm1 170.0(3) . 5_666 ?
N5 Tm1 Tm1 106.7(3) . 5_666 ?
N3 Tm1 Tm1 81.5(3) . 5_666 ?
Se1 Tm1 Tm1 88.08(4) . 5_666 ?
Se2 Sn1 Se1 112.92(6) . . ?
Se2 Sn1 Se3 116.38(6) . . ?
Se1 Sn1 Se3 108.85(6) . . ?
Se2 Sn1 Se3 114.13(6) . 5_766 ?
Se1 Sn1 Se3 107.78(6) . 5_766 ?
Se3 Sn1 Se3 95.22(5) . 5_766 ?
Sn1 Se1 Tm1 113.58(6) . . ?
Sn1 Se3 Sn1 84.78(5) . 5_766 ?
Tm1 O1W Tm1 110.9(4) . 5_666 ?
Tm1 O1W H1WA 109.3 . . ?
Tm1 O1W H1WA 103.3 5_666 . ?
C4 N3 C5 113.8(11) . . ?
C4 N3 Tm1 112.5(8) . . ?
C5 N3 Tm1 116.0(8) . . ?
C4 N3 H3C 104.3 . . ?
C5 N3 H3C 104.3 . . ?
Tm1 N3 H3C 104.3 . . ?
C8 N5 Tm1 115.1(8) . . ?
C8 N5 H5A 108.5 . . ?
Tm1 N5 H5A 108.5 . . ?
C8 N5 H5B 108.5 . . ?
Tm1 N5 H5B 108.5 . . ?
H5A N5 H5B 107.5 . . ?
C6 N4 C7 112.2(10) . . ?
C6 N4 Tm1 113.0(8) . . ?
C7 N4 Tm1 110.9(8) . . ?
C6 N4 H4C 106.8 . . ?
C7 N4 H4C 106.8 . . ?
Tm1 N4 H4C 106.8 . . ?
C1 N1 Tm1 117.3(9) . . ?
C1 N1 H1A 108.0 . . ?
Tm1 N1 H1A 108.0 . . ?
C1 N1 H1B 108.0 . . ?
Tm1 N1 H1B 108.0 . . ?
H1A N1 H1B 107.2 . . ?
C3 N2 C2 111.8(11) . . ?
C3 N2 Tm1 112.6(9) . . ?
C2 N2 Tm1 110.8(9) . . ?
C3 N2 H2C 107.1 . . ?
C2 N2 H2C 107.1 . . ?
Tm1 N2 H2C 107.1 . . ?
N4 C6 C5 110.1(11) . . ?
N4 C6 H6A 109.6 . . ?
C5 C6 H6A 109.6 . . ?
N4 C6 H6B 109.6 . . ?
C5 C6 H6B 109.6 . . ?
H6A C6 H6B 108.1 . . ?
N4 C7 C8 110.8(11) . . ?
N4 C7 H7A 109.5 . . ?
C8 C7 H7A 109.5 . . ?
N4 C7 H7B 109.5 . . ?
C8 C7 H7B 109.5 . . ?
H7A C7 H7B 108.1 . . ?
N5 C8 C7 108.4(11) . . ?
N5 C8 H8A 110.0 . . ?
C7 C8 H8A 110.0 . . ?
N5 C8 H8B 110.0 . . ?
C7 C8 H8B 110.0 . . ?
H8A C8 H8B 108.4 . . ?
N3 C5 C6 109.4(11) . . ?
N3 C5 H5C 109.8 . . ?
C6 C5 H5C 109.8 . . ?
N3 C5 H5D 109.8 . . ?
C6 C5 H5D 109.8 . . ?
H5C C5 H5D 108.2 . . ?
N3 C4 C3 109.6(12) . . ?
N3 C4 H4A 109.7 . . ?
C3 C4 H4A 109.7 . . ?
N3 C4 H4B 109.7 . . ?
C3 C4 H4B 109.7 . . ?
H4A C4 H4B 108.2 . . ?
N1 C1 C2 109.6(12) . . ?
N1 C1 H1C 109.7 . . ?
C2 C1 H1C 109.7 . . ?
N1 C1 H1D 109.7 . . ?
C2 C1 H1D 109.7 . . ?
H1C C1 H1D 108.2 . . ?
N2 C2 C1 114.1(13) . . ?
N2 C2 H2A 108.7 . . ?
C1 C2 H2A 108.7 . . ?
N2 C2 H2B 108.7 . . ?
C1 C2 H2B 108.7 . . ?
H2A C2 H2B 107.6 . . ?
N2 C3 C4 110.8(12) . . ?
N2 C3 H3A 109.5 . . ?
C4 C3 H3A 109.5 . . ?
N2 C3 H3B 109.5 . . ?
C4 C3 H3B 109.5 . . ?
H3A C3 H3B 108.1 . . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        25.10
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         6.900
_refine_diff_density_min         -1.546
_refine_diff_density_rms         0.415
_database_code_depnum_ccdc_archive 'CCDC 1027992'
#######################################################################
#
#                 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_IIa

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C16 H48 Cl2 N10 O2 Y2),Se10 Sn4,4(H2 O)'
_chemical_formula_sum            'C32 H104 Cl4 N20 O8 Se10 Sn4 Y4'
_chemical_formula_weight         2659.10

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'
Cl Cl 0.1484 0.1585 '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'
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Tetragona
_symmetry_space_group_name_H-M   I41/a
_symmetry_space_group_name_Hall  '-I 4ad '

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'

_cell_length_a                   28.236(11)
_cell_length_b                   28.236(11)
_cell_length_c                   10.940(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     8722(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    12814
_cell_measurement_theta_min      3.1991
_cell_measurement_theta_max      28.2005

_exptl_crystal_description       sheet
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.025
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4896
_exptl_absorpt_coefficient_mu    8.090
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4194
_exptl_absorpt_correction_T_max  0.6878
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 7.31
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14694
_diffrn_reflns_av_R_equivalents  0.0582
_diffrn_reflns_av_unetI/netI     0.0528
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.46
_diffrn_reflns_theta_max         25.10
_reflns_number_total             3854
_reflns_number_gt                3191
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)'
_computing_cell_refinement       'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)'
_computing_data_reduction        
'CrystalStructure, Ver. 3.60 (Rigaku/MSC, 2004)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL97

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0730P)²+72.0969P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3854
_refine_ls_number_parameters     178
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0565
_refine_ls_R_factor_gt           0.0470
_refine_ls_wR_factor_ref         0.1392
_refine_ls_wR_factor_gt          0.1336
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_restrained_S_all      1.096
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Sn1 Sn 0.057044(15) 0.795904(16) 0.00418(4) 0.01769(18) Uani 1 1 d . . .
Se2 Se 0.0000 0.7500 0.14048(9) 0.0209(3) Uani 1 2 d S . .
Se1 Se 0.10551(2) 0.73881(3) -0.12556(7) 0.0246(2) Uani 1 1 d . . .
Se3 Se 0.11335(2) 0.83871(3) 0.13312(7) 0.0220(2) Uani 1 1 d . . .
Y1 Y 0.22333(2) 0.69630(2) 0.31662(6) 0.0189(2) Uani 1 1 d . . .
Cl1 Cl 0.27478(7) 0.63797(7) 0.1664(2) 0.0339(5) Uani 1 1 d . . .
O1W O 0.20846(16) 0.76072(17) 0.2062(4) 0.0214(11) Uani 1 1 d . . .
H1WA H 0.1925 0.7801 0.2488 0.032 Uiso 1 1 d R . .
N2 N 0.1407(2) 0.7099(2) 0.3960(6) 0.0252(14) Uani 1 1 d . . .
H2C H 0.1345 0.6859 0.4493 0.030 Uiso 1 1 calc R . .
N3 N 0.2212(2) 0.7543(2) 0.4940(6) 0.0242(14) Uani 1 1 d . . .
H3C H 0.2249 0.7834 0.4598 0.029 Uiso 1 1 calc R . .
N4 N 0.2737(2) 0.6667(2) 0.4943(6) 0.0303(15) Uani 1 1 d . . .
H4C H 0.3042 0.6714 0.4703 0.036 Uiso 1 1 calc R . .
N5 N 0.1985(2) 0.6138(2) 0.3939(7) 0.0368(17) Uani 1 1 d . . .
H5A H 0.1667 0.6129 0.3992 0.044 Uiso 1 1 calc R . .
H5B H 0.2074 0.5920 0.3384 0.044 Uiso 1 1 calc R . .
N1 N 0.1610(2) 0.6667(3) 0.1668(7) 0.0343(16) Uani 1 1 d . . .
H1A H 0.1609 0.6859 0.1011 0.041 Uiso 1 1 calc R . .
H1B H 0.1693 0.6376 0.1412 0.041 Uiso 1 1 calc R . .
C1 C 0.1125(3) 0.6646(3) 0.2175(9) 0.035(2) Uani 1 1 d . . .
H1C H 0.1087 0.6358 0.2647 0.043 Uiso 1 1 calc R . .
H1D H 0.0897 0.6642 0.1514 0.043 Uiso 1 1 calc R . .
C3 C 0.1362(3) 0.7539(3) 0.4654(7) 0.0280(17) Uani 1 1 d . . .
H3A H 0.1058 0.7550 0.5062 0.034 Uiso 1 1 calc R . .
H3B H 0.1383 0.7809 0.4106 0.034 Uiso 1 1 calc R . .
C4 C 0.1756(3) 0.7562(3) 0.5587(7) 0.0317(18) Uani 1 1 d . . .
H4A H 0.1733 0.7853 0.6054 0.038 Uiso 1 1 calc R . .
H4B H 0.1730 0.7297 0.6149 0.038 Uiso 1 1 calc R . .
C2 C 0.1038(3) 0.7070(3) 0.2979(8) 0.0301(18) Uani 1 1 d . . .
H2A H 0.1045 0.7356 0.2489 0.036 Uiso 1 1 calc R . .
H2B H 0.0726 0.7045 0.3350 0.036 Uiso 1 1 calc R . .
C6 C 0.2682(3) 0.6950(3) 0.6075(7) 0.0303(18) Uani 1 1 d . . .
H6A H 0.2957 0.6907 0.6595 0.036 Uiso 1 1 calc R . .
H6B H 0.2404 0.6845 0.6520 0.036 Uiso 1 1 calc R . .
C5 C 0.2630(3) 0.7475(3) 0.5739(8) 0.0343(19) Uani 1 1 d . . .
H5C H 0.2593 0.7662 0.6477 0.041 Uiso 1 1 calc R . .
H5D H 0.2912 0.7583 0.5319 0.041 Uiso 1 1 calc R . .
C7 C 0.2696(3) 0.6150(3) 0.5163(9) 0.039(2) Uani 1 1 d . . .
H7A H 0.2830 0.6072 0.5954 0.047 Uiso 1 1 calc R . .
H7B H 0.2871 0.5978 0.4541 0.047 Uiso 1 1 calc R . .
C8 C 0.2185(3) 0.6009(3) 0.5126(9) 0.039(2) Uani 1 1 d . . .
H8A H 0.2156 0.5670 0.5251 0.047 Uiso 1 1 calc R . .
H8B H 0.2013 0.6168 0.5774 0.047 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sn1 Se3 2.4449(11) . ?
Sn1 Se1 2.5468(11) . ?
Sn1 Se1 2.5472(12) 16_665 ?
Sn1 Se2 2.5490(10) . ?
Se2 Sn1 2.5490(11) 6_464 ?
Se1 Sn1 2.5472(11) 11_565 ?
Y1 O1W 2.224(5) . ?
Y1 O1W 2.290(5) 13_565 ?
Y1 N2 2.520(6) . ?
Y1 N3 2.539(6) . ?
Y1 N1 2.545(7) . ?
Y1 N4 2.549(7) . ?
Y1 N5 2.575(7) . ?
Y1 Cl1 2.743(2) . ?
Y1 Y1 3.6865(18) 13_565 ?
O1W Y1 2.290(5) 13_565 ?
O1W H1WA 0.8500 . ?
N2 C3 1.463(10) . ?
N2 C2 1.498(10) . ?
N2 H2C 0.9100 . ?
N3 C4 1.471(10) . ?
N3 C5 1.480(10) . ?
N3 H3C 0.9100 . ?
N4 C6 1.482(10) . ?
N4 C7 1.484(11) . ?
N4 H4C 0.9100 . ?
N5 C8 1.463(12) . ?
N5 H5A 0.9000 . ?
N5 H5B 0.9000 . ?
N1 C1 1.479(10) . ?
N1 H1A 0.9000 . ?
N1 H1B 0.9000 . ?
C1 C2 1.505(13) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C3 C4 1.510(11) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C6 C5 1.534(12) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C5 H5C 0.9700 . ?
C5 H5D 0.9700 . ?
C7 C8 1.499(12) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?

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
Se3 Sn1 Se1 106.56(3) . . ?
Se3 Sn1 Se1 108.82(3) . 16_665 ?
Se1 Sn1 Se1 112.55(4) . 16_665 ?
Se3 Sn1 Se2 108.95(4) . . ?
Se1 Sn1 Se2 110.10(3) . . ?
Se1 Sn1 Se2 109.75(3) 16_665 . ?
Sn1 Se2 Sn1 108.40(5) 6_464 . ?
Sn1 Se1 Sn1 105.94(3) . 11_565 ?
O1W Y1 O1W 70.49(19) . 13_565 ?
O1W Y1 N2 83.57(19) . . ?
O1W Y1 N2 137.37(19) 13_565 . ?
O1W Y1 N3 83.31(19) . . ?
O1W Y1 N3 76.22(19) 13_565 . ?
N2 Y1 N3 67.4(2) . . ?
O1W Y1 N1 77.7(2) . . ?
O1W Y1 N1 133.2(2) 13_565 . ?
N2 Y1 N1 68.4(2) . . ?
N3 Y1 N1 133.4(2) . . ?
O1W Y1 N4 142.0(2) . . ?
O1W Y1 N4 77.72(19) 13_565 . ?
N2 Y1 N4 107.7(2) . . ?
N3 Y1 N4 69.0(2) . . ?
N1 Y1 N4 140.3(2) . . ?
O1W Y1 N5 150.1(2) . . ?
O1W Y1 N5 138.1(2) 13_565 . ?
N2 Y1 N5 76.8(2) . . ?
N3 Y1 N5 109.0(2) . . ?
N1 Y1 N5 74.1(2) . . ?
N4 Y1 N5 66.8(2) . . ?
O1W Y1 Cl1 105.39(14) . . ?
O1W Y1 Cl1 78.91(13) 13_565 . ?
N2 Y1 Cl1 142.05(15) . . ?
N3 Y1 Cl1 149.04(14) . . ?
N1 Y1 Cl1 77.48(17) . . ?
N4 Y1 Cl1 87.98(16) . . ?
N5 Y1 Cl1 78.35(17) . . ?
O1W Y1 Y1 35.84(12) . 13_565 ?
O1W Y1 Y1 34.66(12) 13_565 13_565 ?
N2 Y1 Y1 112.92(14) . 13_565 ?
N3 Y1 Y1 77.39(14) . 13_565 ?
N1 Y1 Y1 107.30(17) . 13_565 ?
N4 Y1 Y1 110.06(15) . 13_565 ?
N5 Y1 Y1 170.12(16) . 13_565 ?
Cl1 Y1 Y1 92.33(5) . 13_565 ?
Y1 O1W Y1 109.51(19) . 13_565 ?
Y1 O1W H1WA 109.2 . . ?
Y1 O1W H1WA 99.5 13_565 . ?
C3 N2 C2 111.0(6) . . ?
C3 N2 Y1 112.8(4) . . ?
C2 N2 Y1 112.9(5) . . ?
C3 N2 H2C 106.5 . . ?
C2 N2 H2C 106.5 . . ?
Y1 N2 H2C 106.5 . . ?
C4 N3 C5 114.7(6) . . ?
C4 N3 Y1 114.4(5) . . ?
C5 N3 Y1 110.5(5) . . ?
C4 N3 H3C 105.4 . . ?
C5 N3 H3C 105.4 . . ?
Y1 N3 H3C 105.4 . . ?
C6 N4 C7 112.8(7) . . ?
C6 N4 Y1 113.7(5) . . ?
C7 N4 Y1 113.7(5) . . ?
C6 N4 H4C 105.2 . . ?
C7 N4 H4C 105.2 . . ?
Y1 N4 H4C 105.2 . . ?
C8 N5 Y1 114.3(5) . . ?
C8 N5 H5A 108.7 . . ?
Y1 N5 H5A 108.7 . . ?
C8 N5 H5B 108.7 . . ?
Y1 N5 H5B 108.7 . . ?
H5A N5 H5B 107.6 . . ?
C1 N1 Y1 114.3(5) . . ?
C1 N1 H1A 108.7 . . ?
Y1 N1 H1A 108.7 . . ?
C1 N1 H1B 108.7 . . ?
Y1 N1 H1B 108.7 . . ?
H1A N1 H1B 107.6 . . ?
N1 C1 C2 109.9(7) . . ?
N1 C1 H1C 109.7 . . ?
C2 C1 H1C 109.7 . . ?
N1 C1 H1D 109.7 . . ?
C2 C1 H1D 109.7 . . ?
H1C C1 H1D 108.2 . . ?
N2 C3 C4 108.8(6) . . ?
N2 C3 H3A 109.9 . . ?
C4 C3 H3A 109.9 . . ?
N2 C3 H3B 109.9 . . ?
C4 C3 H3B 109.9 . . ?
H3A C3 H3B 108.3 . . ?
N3 C4 C3 108.5(6) . . ?
N3 C4 H4A 110.0 . . ?
C3 C4 H4A 110.0 . . ?
N3 C4 H4B 110.0 . . ?
C3 C4 H4B 110.0 . . ?
H4A C4 H4B 108.4 . . ?
N2 C2 C1 110.3(6) . . ?
N2 C2 H2A 109.6 . . ?
C1 C2 H2A 109.6 . . ?
N2 C2 H2B 109.6 . . ?
C1 C2 H2B 109.6 . . ?
H2A C2 H2B 108.1 . . ?
N4 C6 C5 109.3(6) . . ?
N4 C6 H6A 109.8 . . ?
C5 C6 H6A 109.8 . . ?
N4 C6 H6B 109.8 . . ?
C5 C6 H6B 109.8 . . ?
H6A C6 H6B 108.3 . . ?
N3 C5 C6 110.0(6) . . ?
N3 C5 H5C 109.7 . . ?
C6 C5 H5C 109.7 . . ?
N3 C5 H5D 109.7 . . ?
C6 C5 H5D 109.7 . . ?
H5C C5 H5D 108.2 . . ?
N4 C7 C8 109.4(7) . . ?
N4 C7 H7A 109.8 . . ?
C8 C7 H7A 109.8 . . ?
N4 C7 H7B 109.8 . . ?
C8 C7 H7B 109.8 . . ?
H7A C7 H7B 108.2 . . ?
N5 C8 C7 109.2(7) . . ?
N5 C8 H8A 109.8 . . ?
C7 C8 H8A 109.8 . . ?
N5 C8 H8B 109.8 . . ?
C7 C8 H8B 109.8 . . ?
H8A C8 H8B 108.3 . . ?

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        25.10
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         1.054
_refine_diff_density_min         -0.982
_refine_diff_density_rms         0.220

# SQUEEZE RESULTS (APPEND TO CIF)
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.250 0.500 0.130 453.0 91.0
2 0.250 1.000 0.864 453.0 91.0
3 0.750 0.500 0.364 453.0 91.0
4 0.750 1.000 0.630 453.0 91.0
_platon_squeeze_details          
;
;

########End
_database_code_depnum_ccdc_archive 'CCDC 1022712'
#######################################################################
#
#                 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_IIb

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C16 H48 Cl2 Dy2 N10 O2), Se10 Sn4, 4(H2 O) '
_chemical_formula_sum            'C32 H104 Cl4 Dy4 N20 O8 Se10 Sn4'
_chemical_formula_weight         2953.48

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Tetragona
_symmetry_space_group_name_H-M   I41/a
_symmetry_space_group_name_Hall  '-I 4ad '

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'

_cell_length_a                   28.2390(2)
_cell_length_b                   28.2390(2)
_cell_length_c                   11.0380(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     8802.16(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       sheet
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.229
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5328
_exptl_absorpt_coefficient_mu    8.762
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4195
_exptl_absorpt_correction_T_max  0.6685
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 7.31
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10394
_diffrn_reflns_av_R_equivalents  0.0299
_diffrn_reflns_av_unetI/netI     0.0410
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.19
_diffrn_reflns_theta_max         25.09
_reflns_number_total             3911
_reflns_number_gt                3241
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)'
_computing_cell_refinement       'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)'
_computing_data_reduction        
'CrystalStructure, Ver. 3.60 (Rigaku/MSC, 2004)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL97

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0243P)²+10.6460P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3911
_refine_ls_number_parameters     178
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0405
_refine_ls_R_factor_gt           0.0295
_refine_ls_wR_factor_ref         0.0676
_refine_ls_wR_factor_gt          0.0641
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_restrained_S_all      1.085
_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
Sn1 Sn 0.454448(13) 0.307277(13) 0.24679(3) 0.02705(11) Uani 1 1 d . . .
Dy1 Dy 0.445975(9) 0.526534(9) 0.06663(2) 0.02533(9) Uani 1 1 d . . .
Se1 Se 0.39483(2) 0.26187(2) 0.37485(6) 0.03906(18) Uani 1 1 d . . .
Se2 Se 0.41200(2) 0.36328(2) 0.11802(6) 0.03482(16) Uani 1 1 d . . .
Se3 Se 0.5000 0.2500 0.11220(7) 0.0334(2) Uani 1 2 d S . .
Cl1 Cl 0.38776(6) 0.47550(6) -0.08327(16) 0.0522(5) Uani 1 1 d . . .
O1W O 0.51044(13) 0.54175(12) -0.0445(3) 0.0283(9) Uani 1 1 d . . .
H1WA H 0.5300 0.5576 -0.0025 0.042 Uiso 1 1 d R . .
N1 N 0.36311(17) 0.55068(19) 0.1447(5) 0.0485(14) Uani 1 1 d . . .
H1A H 0.3618 0.5825 0.1499 0.058 Uiso 1 1 calc R . .
H1B H 0.3413 0.5414 0.0902 0.058 Uiso 1 1 calc R . .
N2 N 0.41707(17) 0.47624(17) 0.2451(4) 0.0385(13) Uani 1 1 d . . .
H2C H 0.4216 0.4457 0.2219 0.046 Uiso 1 1 calc R . .
N3 N 0.50374(16) 0.52880(16) 0.2423(4) 0.0327(12) Uani 1 1 d . . .
H3C H 0.5329 0.5249 0.2086 0.039 Uiso 1 1 calc R . .
N4 N 0.45915(16) 0.60952(15) 0.1451(4) 0.0326(12) Uani 1 1 d . . .
H4C H 0.4352 0.6154 0.1981 0.039 Uiso 1 1 calc R . .
N5 N 0.41617(19) 0.58964(17) -0.0820(5) 0.0440(14) Uani 1 1 d . . .
H5A H 0.4356 0.5902 -0.1467 0.053 Uiso 1 1 calc R . .
H5B H 0.3872 0.5812 -0.1083 0.053 Uiso 1 1 calc R . .
C1 C 0.3510(3) 0.5304(3) 0.2634(7) 0.060(2) Uani 1 1 d . . .
H1C H 0.3171 0.5323 0.2762 0.072 Uiso 1 1 calc R . .
H1D H 0.3666 0.5482 0.3271 0.072 Uiso 1 1 calc R . .
C2 C 0.3662(2) 0.4804(2) 0.2680(7) 0.060(2) Uani 1 1 d . . .
H2A H 0.3489 0.4623 0.2078 0.071 Uiso 1 1 calc R . .
H2B H 0.3589 0.4673 0.3471 0.071 Uiso 1 1 calc R . .
C3 C 0.4463(2) 0.4824(2) 0.3544(5) 0.0458(17) Uani 1 1 d . . .
H3A H 0.4423 0.4551 0.4067 0.055 Uiso 1 1 calc R . .
H3B H 0.4355 0.5101 0.3984 0.055 Uiso 1 1 calc R . .
C4 C 0.4974(2) 0.4881(2) 0.3242(5) 0.0441(17) Uani 1 1 d . . .
H4A H 0.5155 0.4930 0.3978 0.053 Uiso 1 1 calc R . .
H4B H 0.5090 0.4595 0.2854 0.053 Uiso 1 1 calc R . .
C5 C 0.5057(2) 0.5747(2) 0.3058(6) 0.0442(16) Uani 1 1 d . . .
H5C H 0.5349 0.5770 0.3519 0.053 Uiso 1 1 calc R . .
H5D H 0.4793 0.5773 0.3618 0.053 Uiso 1 1 calc R . .
C6 C 0.5034(2) 0.6139(2) 0.2147(6) 0.0398(16) Uani 1 1 d . . .
H6A H 0.5043 0.6443 0.2556 0.048 Uiso 1 1 calc R . .
H6B H 0.5304 0.6120 0.1605 0.048 Uiso 1 1 calc R . .
C7 C 0.4555(2) 0.6461(2) 0.0489(6) 0.0459(17) Uani 1 1 d . . .
H7A H 0.4841 0.6459 0.0003 0.055 Uiso 1 1 calc R . .
H7B H 0.4526 0.6771 0.0860 0.055 Uiso 1 1 calc R . .
C8 C 0.4134(2) 0.6374(2) -0.0312(6) 0.0475(18) Uani 1 1 d . . .
H8A H 0.3845 0.6407 0.0154 0.057 Uiso 1 1 calc R . .
H8B H 0.4129 0.6605 -0.0962 0.057 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sn1 Se2 2.4409(7) . ?
Sn1 Se1 2.5427(7) 11_666 ?
Sn1 Se1 2.5449(7) . ?
Sn1 Se3 2.5452(6) . ?
Dy1 O1W 2.237(3) . ?
Dy1 O1W 2.301(3) 9_665 ?
Dy1 N4 2.526(4) . ?
Dy1 N3 2.535(4) . ?
Dy1 N2 2.562(5) . ?
Dy1 N5 2.564(5) . ?
Dy1 N1 2.585(5) . ?
Dy1 Cl1 2.7418(16) . ?
Dy1 Dy1 3.7040(5) 9_665 ?
Se1 Sn1 2.5427(7) 16_656 ?
Se3 Sn1 2.5452(6) 6_554 ?
O1W Dy1 2.301(3) 9_665 ?
O1W H1WA 0.8499 . ?
N1 C1 1.471(8) . ?
N1 H1A 0.9000 . ?
N1 H1B 0.9000 . ?
N2 C2 1.463(8) . ?
N2 C3 1.471(7) . ?
N2 H2C 0.9100 . ?
N3 C4 1.474(7) . ?
N3 C5 1.475(7) . ?
N3 H3C 0.9100 . ?
N4 C6 1.472(7) . ?
N4 C7 1.485(7) . ?
N4 H4C 0.9100 . ?
N5 C8 1.462(7) . ?
N5 H5A 0.9000 . ?
N5 H5B 0.9000 . ?
C1 C2 1.475(9) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.490(8) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.496(8) . ?
C5 H5C 0.9700 . ?
C5 H5D 0.9700 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C8 1.500(9) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?

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
Se2 Sn1 Se1 107.04(2) . 11_666 ?
Se2 Sn1 Se1 108.97(2) . . ?
Se1 Sn1 Se1 112.353(17) 11_666 . ?
Se2 Sn1 Se3 108.67(3) . . ?
Se1 Sn1 Se3 109.93(2) 11_666 . ?
Se1 Sn1 Se3 109.78(2) . . ?
O1W Dy1 O1W 70.58(14) . 9_665 ?
O1W Dy1 N4 83.68(14) . . ?
O1W Dy1 N4 137.32(14) 9_665 . ?
O1W Dy1 N3 83.75(14) . . ?
O1W Dy1 N3 76.00(14) 9_665 . ?
N4 Dy1 N3 67.63(15) . . ?
O1W Dy1 N2 141.95(14) . . ?
O1W Dy1 N2 77.72(14) 9_665 . ?
N4 Dy1 N2 107.31(15) . . ?
N3 Dy1 N2 68.33(15) . . ?
O1W Dy1 N5 77.44(15) . . ?
O1W Dy1 N5 133.64(14) 9_665 . ?
N4 Dy1 N5 67.85(16) . . ?
N3 Dy1 N5 133.09(16) . . ?
N2 Dy1 N5 140.59(16) . . ?
O1W Dy1 N1 150.31(15) . . ?
O1W Dy1 N1 137.79(15) 9_665 . ?
N4 Dy1 N1 76.96(16) . . ?
N3 Dy1 N1 108.72(16) . . ?
N2 Dy1 N1 66.52(16) . . ?
N5 Dy1 N1 74.51(17) . . ?
O1W Dy1 Cl1 104.95(10) . . ?
O1W Dy1 Cl1 79.41(10) 9_665 . ?
N4 Dy1 Cl1 141.52(11) . . ?
N3 Dy1 Cl1 149.41(11) . . ?
N2 Dy1 Cl1 88.95(12) . . ?
N5 Dy1 Cl1 77.43(12) . . ?
N1 Dy1 Cl1 78.29(13) . . ?
O1W Dy1 Dy1 35.86(8) . 9_665 ?
O1W Dy1 Dy1 34.72(9) 9_665 9_665 ?
N4 Dy1 Dy1 112.97(11) . 9_665 ?
N3 Dy1 Dy1 77.52(10) . 9_665 ?
N2 Dy1 Dy1 110.09(11) . 9_665 ?
N5 Dy1 Dy1 107.30(12) . 9_665 ?
N1 Dy1 Dy1 169.97(12) . 9_665 ?
Cl1 Dy1 Dy1 92.39(4) . 9_665 ?
Sn1 Se1 Sn1 106.20(3) 16_656 . ?
Sn1 Se3 Sn1 108.58(3) 6_554 . ?
Dy1 O1W Dy1 109.42(14) . 9_665 ?
Dy1 O1W H1WA 109.4 . . ?
Dy1 O1W H1WA 98.7 9_665 . ?
C1 N1 Dy1 113.9(4) . . ?
C1 N1 H1A 108.8 . . ?
Dy1 N1 H1A 108.8 . . ?
C1 N1 H1B 108.8 . . ?
Dy1 N1 H1B 108.8 . . ?
H1A N1 H1B 107.7 . . ?
C2 N2 C3 113.5(5) . . ?
C2 N2 Dy1 113.6(4) . . ?
C3 N2 Dy1 112.7(3) . . ?
C2 N2 H2C 105.3 . . ?
C3 N2 H2C 105.3 . . ?
Dy1 N2 H2C 105.3 . . ?
C4 N3 C5 113.5(4) . . ?
C4 N3 Dy1 111.8(3) . . ?
C5 N3 Dy1 114.2(4) . . ?
C4 N3 H3C 105.4 . . ?
C5 N3 H3C 105.4 . . ?
Dy1 N3 H3C 105.4 . . ?
C6 N4 C7 112.0(5) . . ?
C6 N4 Dy1 112.4(3) . . ?
C7 N4 Dy1 113.0(3) . . ?
C6 N4 H4C 106.3 . . ?
C7 N4 H4C 106.3 . . ?
Dy1 N4 H4C 106.3 . . ?
C8 N5 Dy1 114.4(4) . . ?
C8 N5 H5A 108.7 . . ?
Dy1 N5 H5A 108.7 . . ?
C8 N5 H5B 108.7 . . ?
Dy1 N5 H5B 108.7 . . ?
H5A N5 H5B 107.6 . . ?
N1 C1 C2 109.6(6) . . ?
N1 C1 H1C 109.8 . . ?
C2 C1 H1C 109.8 . . ?
N1 C1 H1D 109.8 . . ?
C2 C1 H1D 109.8 . . ?
H1C C1 H1D 108.2 . . ?
C1 C2 N2 111.0(5) . . ?
C1 C2 H2A 109.4 . . ?
N2 C2 H2A 109.4 . . ?
C1 C2 H2B 109.4 . . ?
N2 C2 H2B 109.4 . . ?
H2A C2 H2B 108.0 . . ?
N2 C3 C4 111.8(5) . . ?
N2 C3 H3A 109.2 . . ?
C4 C3 H3A 109.2 . . ?
N2 C3 H3B 109.2 . . ?
C4 C3 H3B 109.2 . . ?
H3A C3 H3B 107.9 . . ?
N3 C4 C3 109.8(5) . . ?
N3 C4 H4A 109.7 . . ?
C3 C4 H4A 109.7 . . ?
N3 C4 H4B 109.7 . . ?
C3 C4 H4B 109.7 . . ?
H4A C4 H4B 108.2 . . ?
N3 C5 C6 109.2(5) . . ?
N3 C5 H5C 109.8 . . ?
C6 C5 H5C 109.8 . . ?
N3 C5 H5D 109.8 . . ?
C6 C5 H5D 109.8 . . ?
H5C C5 H5D 108.3 . . ?
N4 C6 C5 109.0(5) . . ?
N4 C6 H6A 109.9 . . ?
C5 C6 H6A 109.9 . . ?
N4 C6 H6B 109.9 . . ?
C5 C6 H6B 109.9 . . ?
H6A C6 H6B 108.3 . . ?
N4 C7 C8 111.2(5) . . ?
N4 C7 H7A 109.4 . . ?
C8 C7 H7A 109.4 . . ?
N4 C7 H7B 109.4 . . ?
C8 C7 H7B 109.4 . . ?
H7A C7 H7B 108.0 . . ?
N5 C8 C7 109.6(5) . . ?
N5 C8 H8A 109.7 . . ?
C7 C8 H8A 109.7 . . ?
N5 C8 H8B 109.7 . . ?
C7 C8 H8B 109.7 . . ?
H8A C8 H8B 108.2 . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.09
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.677
_refine_diff_density_min         -0.602
_refine_diff_density_rms         0.123

# SQUEEZE RESULTS (APPEND TO CIF)
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.250 0.500 0.126 467.0 95.3
2 0.250 1.000 0.870 467.0 95.3
3 0.750 0.500 0.370 467.0 95.3
4 0.750 1.000 0.626 467.0 95.3
_platon_squeeze_details          
;
;

########End
_database_code_depnum_ccdc_archive 'CCDC 1022713'
#######################################################################
#
#                 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_IIc

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C16 H48 Cl2 Er2 N10 O2), Se10 Sn4, 4(H2 O)'
_chemical_formula_sum            'C32 H104 Cl4 Er4 N20 O8 Se10 Sn4'
_chemical_formula_weight         2972.52

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'
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Tetragona
_symmetry_space_group_name_H-M   I41/a
_symmetry_space_group_name_Hall  '-I 4ad '

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'

_cell_length_a                   28.1622(3)
_cell_length_b                   28.1622(3)
_cell_length_c                   11.0089(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     8731.3(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    12637
_cell_measurement_theta_min      3.198
_cell_measurement_theta_max      29.045

_exptl_crystal_description       sheet
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.261
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5360
_exptl_absorpt_coefficient_mu    9.254
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4292
_exptl_absorpt_correction_T_max  0.6547
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 7.31
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10732
_diffrn_reflns_av_R_equivalents  0.0254
_diffrn_reflns_av_unetI/netI     0.0299
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.20
_diffrn_reflns_theta_max         25.09
_reflns_number_total             3877
_reflns_number_gt                3398
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)'
_computing_cell_refinement       'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)'
_computing_data_reduction        
'CrystalStructure, Ver. 3.60 (Rigaku/MSC, 2004)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL97

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0303P)²+9.2627P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3877
_refine_ls_number_parameters     178
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0300
_refine_ls_R_factor_gt           0.0244
_refine_ls_wR_factor_ref         0.0630
_refine_ls_wR_factor_gt          0.0606
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_restrained_S_all      1.060
_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
Sn1 Sn 0.442731(11) 0.704186(11) 0.99647(3) 0.02544(10) Uani 1 1 d . . .
Er1 Er 0.446579(7) 0.526605(7) 0.567569(18) 0.02413(8) Uani 1 1 d . . .
Cl1 Cl 0.38824(5) 0.47596(5) 0.41960(13) 0.0489(4) Uani 1 1 d . . .
O1W O 0.51032(11) 0.54101(10) 0.4565(3) 0.0273(7) Uani 1 1 d . . .
H1WA H 0.5301 0.5569 0.4983 0.041 Uiso 1 1 d R . .
N1 N 0.36414(15) 0.55105(17) 0.6456(4) 0.0469(12) Uani 1 1 d . . .
H1A H 0.3630 0.5829 0.6509 0.056 Uiso 1 1 calc R . .
H1B H 0.3422 0.5420 0.5908 0.056 Uiso 1 1 calc R . .
N2 N 0.41781(15) 0.47630(15) 0.7434(4) 0.0386(11) Uani 1 1 d . . .
H2C H 0.4227 0.4458 0.7195 0.046 Uiso 1 1 calc R . .
N3 N 0.50407(14) 0.52877(14) 0.7416(3) 0.0306(9) Uani 1 1 d . . .
H3C H 0.5332 0.5250 0.7072 0.037 Uiso 1 1 calc R . .
N4 N 0.45971(14) 0.60941(13) 0.6445(3) 0.0315(9) Uani 1 1 d . . .
H4C H 0.4357 0.6154 0.6975 0.038 Uiso 1 1 calc R . .
N5 N 0.41668(16) 0.58862(15) 0.4186(4) 0.0414(11) Uani 1 1 d . . .
H5A H 0.4359 0.5889 0.3534 0.050 Uiso 1 1 calc R . .
H5B H 0.3875 0.5801 0.3931 0.050 Uiso 1 1 calc R . .
C1 C 0.3516(2) 0.5311(2) 0.7630(6) 0.0591(17) Uani 1 1 d . . .
H1C H 0.3176 0.5335 0.7758 0.071 Uiso 1 1 calc R . .
H1D H 0.3675 0.5484 0.8272 0.071 Uiso 1 1 calc R . .
C2 C 0.3665(2) 0.4797(2) 0.7658(6) 0.0530(16) Uani 1 1 d . . .
H2A H 0.3590 0.4661 0.8444 0.064 Uiso 1 1 calc R . .
H2B H 0.3494 0.4621 0.7041 0.064 Uiso 1 1 calc R . .
C3 C 0.4463(2) 0.4819(2) 0.8543(5) 0.0510(16) Uani 1 1 d . . .
H3A H 0.4422 0.4543 0.9060 0.061 Uiso 1 1 calc R . .
H3B H 0.4354 0.5096 0.8988 0.061 Uiso 1 1 calc R . .
C4 C 0.4983(2) 0.4876(2) 0.8227(4) 0.0436(14) Uani 1 1 d . . .
H4A H 0.5167 0.4923 0.8962 0.052 Uiso 1 1 calc R . .
H4B H 0.5097 0.4592 0.7827 0.052 Uiso 1 1 calc R . .
C5 C 0.5066(2) 0.57430(19) 0.8061(5) 0.0420(13) Uani 1 1 d . . .
H5C H 0.5361 0.5764 0.8514 0.050 Uiso 1 1 calc R . .
H5D H 0.4804 0.5769 0.8629 0.050 Uiso 1 1 calc R . .
C6 C 0.50404(19) 0.61366(19) 0.7143(5) 0.0406(13) Uani 1 1 d . . .
H6A H 0.5050 0.6441 0.7553 0.049 Uiso 1 1 calc R . .
H6B H 0.5311 0.6118 0.6599 0.049 Uiso 1 1 calc R . .
C7 C 0.4562(2) 0.64573(18) 0.5487(5) 0.0434(14) Uani 1 1 d . . .
H7A H 0.4848 0.6453 0.4997 0.052 Uiso 1 1 calc R . .
H7B H 0.4536 0.6769 0.5857 0.052 Uiso 1 1 calc R . .
C8 C 0.4142(2) 0.63727(19) 0.4692(5) 0.0450(14) Uani 1 1 d . . .
H8A H 0.3852 0.6410 0.5159 0.054 Uiso 1 1 calc R . .
H8B H 0.4138 0.6603 0.4036 0.054 Uiso 1 1 calc R . .
Se1 Se 0.48832(2) 0.644601(17) 1.12505(5) 0.03749(14) Uani 1 1 d . . .
Se2 Se 0.5000 0.7500 0.86179(6) 0.03195(17) Uani 1 2 d S . .
Se3 Se 0.386926(17) 0.661568(19) 0.86705(4) 0.03299(13) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sn1 Se3 2.4373(5) . ?
Sn1 Se1 2.5416(6) 15_567 ?
Sn1 Se2 2.5425(5) . ?
Sn1 Se1 2.5432(6) . ?
Er1 O1W 2.209(3) . ?
Er1 O1W 2.274(3) 9_666 ?
Er1 N4 2.508(4) . ?
Er1 N3 2.509(4) . ?
Er1 N2 2.532(4) . ?
Er1 N5 2.539(4) . ?
Er1 N1 2.569(4) . ?
Er1 Cl1 2.7179(13) . ?
Er1 Er1 3.6759(4) 9_666 ?
O1W Er1 2.274(3) 9_666 ?
O1W H1WA 0.8499 . ?
N1 C1 1.453(7) . ?
N1 H1A 0.9000 . ?
N1 H1B 0.9000 . ?
N2 C2 1.468(7) . ?
N2 C3 1.470(7) . ?
N2 H2C 0.9100 . ?
N3 C4 1.471(6) . ?
N3 C5 1.467(6) . ?
N3 H3C 0.9100 . ?
N4 C6 1.471(6) . ?
N4 C7 1.472(6) . ?
N4 H4C 0.9100 . ?
N5 C8 1.480(6) . ?
N5 H5A 0.9000 . ?
N5 H5B 0.9000 . ?
C1 C2 1.506(8) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.513(8) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.502(7) . ?
C5 H5C 0.9700 . ?
C5 H5D 0.9700 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C8 1.490(8) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
Se1 Sn1 2.5416(6) 12_768 ?
Se2 Sn1 2.5425(5) 6_564 ?

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
Se3 Sn1 Se1 107.167(19) . 15_567 ?
Se3 Sn1 Se2 108.54(2) . . ?
Se1 Sn1 Se2 109.851(18) 15_567 . ?
Se3 Sn1 Se1 109.03(2) . . ?
Se1 Sn1 Se1 112.321(14) 15_567 . ?
Se2 Sn1 Se1 109.826(18) . . ?
O1W Er1 O1W 69.85(12) . 9_666 ?
O1W Er1 N4 84.04(12) . . ?
O1W Er1 N4 137.67(12) 9_666 . ?
O1W Er1 N3 83.91(12) . . ?
O1W Er1 N3 76.41(12) 9_666 . ?
N4 Er1 N3 67.95(13) . . ?
O1W Er1 N2 141.80(13) . . ?
O1W Er1 N2 77.96(12) 9_666 . ?
N4 Er1 N2 108.03(13) . . ?
N3 Er1 N2 68.68(14) . . ?
O1W Er1 N5 77.63(13) . . ?
O1W Er1 N5 132.67(12) 9_666 . ?
N4 Er1 N5 68.12(13) . . ?
N3 Er1 N5 133.65(14) . . ?
N2 Er1 N5 140.57(15) . . ?
O1W Er1 N1 150.45(13) . . ?
O1W Er1 N1 138.23(13) 9_666 . ?
N4 Er1 N1 76.78(14) . . ?
N3 Er1 N1 108.73(14) . . ?
N2 Er1 N1 66.74(14) . . ?
N5 Er1 N1 74.45(15) . . ?
O1W Er1 Cl1 104.82(9) . . ?
O1W Er1 Cl1 79.24(8) 9_666 . ?
N4 Er1 Cl1 141.19(10) . . ?
N3 Er1 Cl1 149.37(10) . . ?
N2 Er1 Cl1 88.34(10) . . ?
N5 Er1 Cl1 76.91(11) . . ?
N1 Er1 Cl1 78.16(11) . . ?
O1W Er1 Er1 35.50(7) . 9_666 ?
O1W Er1 Er1 34.35(8) 9_666 9_666 ?
N4 Er1 Er1 113.26(9) . 9_666 ?
N3 Er1 Er1 77.93(9) . 9_666 ?
N2 Er1 Er1 110.08(10) . 9_666 ?
N5 Er1 Er1 106.89(10) . 9_666 ?
N1 Er1 Er1 169.79(11) . 9_666 ?
Cl1 Er1 Er1 92.19(3) . 9_666 ?
Er1 O1W Er1 110.15(12) . 9_666 ?
Er1 O1W H1WA 109.3 . . ?
Er1 O1W H1WA 98.9 9_666 . ?
C1 N1 Er1 114.4(3) . . ?
C1 N1 H1A 108.7 . . ?
Er1 N1 H1A 108.7 . . ?
C1 N1 H1B 108.7 . . ?
Er1 N1 H1B 108.7 . . ?
H1A N1 H1B 107.6 . . ?
C2 N2 C3 112.9(4) . . ?
C2 N2 Er1 114.0(3) . . ?
C3 N2 Er1 113.6(3) . . ?
C2 N2 H2C 105.0 . . ?
C3 N2 H2C 105.0 . . ?
Er1 N2 H2C 105.0 . . ?
C4 N3 C5 113.6(4) . . ?
C4 N3 Er1 111.8(3) . . ?
C5 N3 Er1 114.9(3) . . ?
C4 N3 H3C 105.1 . . ?
C5 N3 H3C 105.1 . . ?
Er1 N3 H3C 105.1 . . ?
C6 N4 C7 112.1(4) . . ?
C6 N4 Er1 112.2(3) . . ?
C7 N4 Er1 113.2(3) . . ?
C6 N4 H4C 106.3 . . ?
C7 N4 H4C 106.3 . . ?
Er1 N4 H4C 106.3 . . ?
C8 N5 Er1 114.2(3) . . ?
C8 N5 H5A 108.7 . . ?
Er1 N5 H5A 108.7 . . ?
C8 N5 H5B 108.7 . . ?
Er1 N5 H5B 108.7 . . ?
H5A N5 H5B 107.6 . . ?
N1 C1 C2 108.8(5) . . ?
N1 C1 H1C 109.9 . . ?
C2 C1 H1C 109.9 . . ?
N1 C1 H1D 109.9 . . ?
C2 C1 H1D 109.9 . . ?
H1C C1 H1D 108.3 . . ?
N2 C2 C1 109.5(5) . . ?
N2 C2 H2A 109.8 . . ?
C1 C2 H2A 109.8 . . ?
N2 C2 H2B 109.8 . . ?
C1 C2 H2B 109.8 . . ?
H2A C2 H2B 108.2 . . ?
N2 C3 C4 110.3(4) . . ?
N2 C3 H3A 109.6 . . ?
C4 C3 H3A 109.6 . . ?
N2 C3 H3B 109.6 . . ?
C4 C3 H3B 109.6 . . ?
H3A C3 H3B 108.1 . . ?
N3 C4 C3 109.3(4) . . ?
N3 C4 H4A 109.8 . . ?
C3 C4 H4A 109.8 . . ?
N3 C4 H4B 109.8 . . ?
C3 C4 H4B 109.8 . . ?
H4A C4 H4B 108.3 . . ?
N3 C5 C6 108.5(4) . . ?
N3 C5 H5C 110.0 . . ?
C6 C5 H5C 110.0 . . ?
N3 C5 H5D 110.0 . . ?
C6 C5 H5D 110.0 . . ?
H5C C5 H5D 108.4 . . ?
N4 C6 C5 109.4(4) . . ?
N4 C6 H6A 109.8 . . ?
C5 C6 H6A 109.8 . . ?
N4 C6 H6B 109.8 . . ?
C5 C6 H6B 109.8 . . ?
H6A C6 H6B 108.2 . . ?
N4 C7 C8 111.3(4) . . ?
N4 C7 H7A 109.4 . . ?
C8 C7 H7A 109.4 . . ?
N4 C7 H7B 109.4 . . ?
C8 C7 H7B 109.4 . . ?
H7A C7 H7B 108.0 . . ?
N5 C8 C7 109.3(4) . . ?
N5 C8 H8A 109.8 . . ?
C7 C8 H8A 109.8 . . ?
N5 C8 H8B 109.8 . . ?
C7 C8 H8B 109.8 . . ?
H8A C8 H8B 108.3 . . ?
Sn1 Se1 Sn1 106.23(2) 12_768 . ?
Sn1 Se2 Sn1 108.65(3) 6_564 . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.09
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.586
_refine_diff_density_min         -0.884
_refine_diff_density_rms         0.110

# SQUEEZE RESULTS (APPEND TO CIF)
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.250 0.500 0.625 462.0 95.1
2 0.250 1.000 0.370 462.0 95.1
3 0.750 0.500 0.870 462.0 95.1
4 0.750 1.000 0.125 462.0 95.1
_platon_squeeze_details          
;
;

########End
_database_code_depnum_ccdc_archive 'CCDC 1022860'
#######################################################################
#
#                 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_IId

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C16 H48 Cl2 N10 O2 Tm2), Se10 Sn4, 4(H2 O)'
_chemical_formula_sum            'C32 H104 Cl4 N20 O8 Se10 Sn4 Tm4'
_chemical_formula_weight         2979.22

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'
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tm Tm -0.3139 5.2483 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Tetragona
_symmetry_space_group_name_H-M   I41/a
_symmetry_space_group_name_Hall  '-I 4ad '

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'

_cell_length_a                   28.2080(3)
_cell_length_b                   28.2080(3)
_cell_length_c                   11.0142(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     8763.9(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    10987
_cell_measurement_theta_min      3.194
_cell_measurement_theta_max      28.947

_exptl_crystal_description       sheet
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.258
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5376
_exptl_absorpt_coefficient_mu    9.439
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3971
_exptl_absorpt_correction_T_max  0.6013
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 7.31
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9361
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_unetI/netI     0.0472
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.19
_diffrn_reflns_theta_max         25.10
_reflns_number_total             3897
_reflns_number_gt                3287
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)'
_computing_cell_refinement       'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)'
_computing_data_reduction        
'CrystalStructure, Ver. 3.60 (Rigaku/MSC, 2004)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL97

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0286P)²+8.6356P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.000070(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         3897
_refine_ls_number_parameters     179
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0388
_refine_ls_R_factor_gt           0.0301
_refine_ls_wR_factor_ref         0.0773
_refine_ls_wR_factor_gt          0.0735
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_restrained_S_all      1.092
_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
Tm1 Tm 0.446890(9) 0.526610(9) 0.06777(3) 0.02517(11) Uani 1 1 d . . .
Sn1 Sn 0.454020(14) 0.307170(14) 0.24623(4) 0.02725(14) Uani 1 1 d . . .
Se3 Se 0.5000 0.2500 0.11145(9) 0.0334(2) Uani 1 2 d S . .
Se2 Se 0.39453(2) 0.26150(2) 0.37500(7) 0.0391(2) Uani 1 1 d . . .
Se1 Se 0.41127(2) 0.36299(2) 0.11651(6) 0.03468(19) Uani 1 1 d . . .
Cl1 Cl 0.38830(6) 0.47570(6) -0.07931(18) 0.0494(5) Uani 1 1 d . . .
O1W O 0.51064(13) 0.54117(13) -0.0429(4) 0.0260(10) Uani 1 1 d . . .
H1WA H 0.5304 0.5571 -0.0013 0.039 Uiso 1 1 d R . .
N4 N 0.46018(18) 0.60911(17) 0.1438(5) 0.0339(13) Uani 1 1 d . . .
H4C H 0.4362 0.6151 0.1970 0.041 Uiso 1 1 calc R . .
N3 N 0.50450(17) 0.52871(18) 0.2418(5) 0.0327(13) Uani 1 1 d . . .
H3C H 0.5336 0.5250 0.2073 0.039 Uiso 1 1 calc R . .
N2 N 0.41795(19) 0.47573(19) 0.2422(5) 0.0397(14) Uani 1 1 d . . .
H2C H 0.4228 0.4452 0.2184 0.048 Uiso 1 1 calc R . .
N5 N 0.41721(19) 0.58791(18) -0.0798(5) 0.0414(15) Uani 1 1 d . . .
H5A H 0.4365 0.5881 -0.1448 0.050 Uiso 1 1 calc R . .
H5B H 0.3882 0.5791 -0.1055 0.050 Uiso 1 1 calc R . .
N1 N 0.36489(18) 0.55143(19) 0.1451(6) 0.0450(16) Uani 1 1 d . . .
H1A H 0.3640 0.5833 0.1507 0.054 Uiso 1 1 calc R . .
H1B H 0.3430 0.5427 0.0899 0.054 Uiso 1 1 calc R . .
C7 C 0.4564(3) 0.6454(2) 0.0489(7) 0.0456(19) Uani 1 1 d . . .
H7A H 0.4851 0.6453 0.0003 0.055 Uiso 1 1 calc R . .
H7B H 0.4533 0.6763 0.0863 0.055 Uiso 1 1 calc R . .
C5 C 0.5068(3) 0.5743(2) 0.3060(6) 0.0420(18) Uani 1 1 d . . .
H5C H 0.5362 0.5764 0.3515 0.050 Uiso 1 1 calc R . .
H5D H 0.4806 0.5769 0.3625 0.050 Uiso 1 1 calc R . .
C1 C 0.3518(3) 0.5314(3) 0.2625(8) 0.056(2) Uani 1 1 d . . .
H1C H 0.3179 0.5341 0.2748 0.067 Uiso 1 1 calc R . .
H1D H 0.3678 0.5484 0.3272 0.067 Uiso 1 1 calc R . .
C6 C 0.5043(2) 0.6137(2) 0.2134(6) 0.0394(17) Uani 1 1 d . . .
H6A H 0.5052 0.6442 0.2541 0.047 Uiso 1 1 calc R . .
H6B H 0.5314 0.6119 0.1592 0.047 Uiso 1 1 calc R . .
C8 C 0.4141(2) 0.6363(2) -0.0323(7) 0.048(2) Uani 1 1 d . . .
H8A H 0.3850 0.6402 0.0136 0.058 Uiso 1 1 calc R . .
H8B H 0.4139 0.6589 -0.0988 0.058 Uiso 1 1 calc R . .
C4 C 0.4987(3) 0.4873(3) 0.3222(6) 0.0446(19) Uani 1 1 d . . .
H4A H 0.5169 0.4917 0.3960 0.053 Uiso 1 1 calc R . .
H4B H 0.5101 0.4589 0.2818 0.053 Uiso 1 1 calc R . .
C2 C 0.3664(3) 0.4798(2) 0.2634(8) 0.052(2) Uani 1 1 d . . .
H2A H 0.3585 0.4657 0.3412 0.063 Uiso 1 1 calc R . .
H2B H 0.3494 0.4628 0.2006 0.063 Uiso 1 1 calc R . .
C3 C 0.4462(3) 0.4818(3) 0.3529(6) 0.050(2) Uani 1 1 d . . .
H3A H 0.4419 0.4545 0.4054 0.060 Uiso 1 1 calc R . .
H3B H 0.4354 0.5097 0.3964 0.060 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tm1 O1W 2.211(4) . ?
Tm1 O1W 2.273(4) 9_665 ?
Tm1 N4 2.501(5) . ?
Tm1 N3 2.514(5) . ?
Tm1 N5 2.516(5) . ?
Tm1 N2 2.533(5) . ?
Tm1 N1 2.562(5) . ?
Tm1 Cl1 2.7236(17) . ?
Tm1 Tm1 3.6688(5) 9_665 ?
Sn1 Se1 2.4443(7) . ?
Sn1 Se3 2.5469(7) . ?
Sn1 Se2 2.5470(8) . ?
Sn1 Se2 2.5489(8) 11_666 ?
Se3 Sn1 2.5469(7) 6_554 ?
Se2 Sn1 2.5489(8) 16_656 ?
O1W Tm1 2.273(4) 9_665 ?
O1W H1WA 0.8500 . ?
N4 C7 1.466(8) . ?
N4 C6 1.469(8) . ?
N4 H4C 0.9100 . ?
N3 C5 1.469(7) . ?
N3 C4 1.476(8) . ?
N3 H3C 0.9100 . ?
N2 C3 1.467(9) . ?
N2 C2 1.476(8) . ?
N2 H2C 0.9100 . ?
N5 C8 1.466(8) . ?
N5 H5A 0.9000 . ?
N5 H5B 0.9000 . ?
N1 C1 1.458(9) . ?
N1 H1A 0.9000 . ?
N1 H1B 0.9000 . ?
C7 C8 1.513(10) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C5 C6 1.510(9) . ?
C5 H5C 0.9700 . ?
C5 H5D 0.9700 . ?
C1 C2 1.514(9) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C4 C3 1.526(10) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?

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
O1W Tm1 O1W 70.19(15) . 9_665 ?
O1W Tm1 N4 83.67(15) . . ?
O1W Tm1 N4 138.07(16) 9_665 . ?
O1W Tm1 N3 83.70(16) . . ?
O1W Tm1 N3 76.76(15) 9_665 . ?
N4 Tm1 N3 68.04(17) . . ?
O1W Tm1 N5 77.70(16) . . ?
O1W Tm1 N5 132.50(16) 9_665 . ?
N4 Tm1 N5 68.07(18) . . ?
N3 Tm1 N5 133.74(17) . . ?
O1W Tm1 N2 141.76(16) . . ?
O1W Tm1 N2 77.57(16) 9_665 . ?
N4 Tm1 N2 108.76(17) . . ?
N3 Tm1 N2 69.10(17) . . ?
N5 Tm1 N2 140.52(18) . . ?
O1W Tm1 N1 150.08(16) . . ?
O1W Tm1 N1 138.22(16) 9_665 . ?
N4 Tm1 N1 76.70(17) . . ?
N3 Tm1 N1 108.89(18) . . ?
N5 Tm1 N1 74.13(19) . . ?
N2 Tm1 N1 67.16(18) . . ?
O1W Tm1 Cl1 105.28(11) . . ?
O1W Tm1 Cl1 78.73(11) 9_665 . ?
N4 Tm1 Cl1 141.31(13) . . ?
N3 Tm1 Cl1 149.12(12) . . ?
N5 Tm1 Cl1 77.08(13) . . ?
N2 Tm1 Cl1 87.53(13) . . ?
N1 Tm1 Cl1 78.11(14) . . ?
O1W Tm1 Tm1 35.65(9) . 9_665 ?
O1W Tm1 Tm1 34.54(9) 9_665 9_665 ?
N4 Tm1 Tm1 113.23(12) . 9_665 ?
N3 Tm1 Tm1 77.99(11) . 9_665 ?
N5 Tm1 Tm1 106.87(13) . 9_665 ?
N2 Tm1 Tm1 109.88(12) . 9_665 ?
N1 Tm1 Tm1 169.83(13) . 9_665 ?
Cl1 Tm1 Tm1 92.17(4) . 9_665 ?
Se1 Sn1 Se3 108.57(3) . . ?
Se1 Sn1 Se2 109.04(3) . . ?
Se3 Sn1 Se2 109.87(2) . . ?
Se1 Sn1 Se2 107.14(2) . 11_666 ?
Se3 Sn1 Se2 109.81(2) . 11_666 ?
Se2 Sn1 Se2 112.31(2) . 11_666 ?
Sn1 Se3 Sn1 108.69(4) 6_554 . ?
Sn1 Se2 Sn1 106.23(3) . 16_656 ?
Tm1 O1W Tm1 109.81(15) . 9_665 ?
Tm1 O1W H1WA 109.5 . . ?
Tm1 O1W H1WA 99.5 9_665 . ?
C7 N4 C6 111.9(5) . . ?
C7 N4 Tm1 113.6(4) . . ?
C6 N4 Tm1 112.6(4) . . ?
C7 N4 H4C 106.0 . . ?
C6 N4 H4C 106.0 . . ?
Tm1 N4 H4C 106.0 . . ?
C5 N3 C4 114.2(5) . . ?
C5 N3 Tm1 114.6(4) . . ?
C4 N3 Tm1 111.5(4) . . ?
C5 N3 H3C 105.1 . . ?
C4 N3 H3C 105.1 . . ?
Tm1 N3 H3C 105.1 . . ?
C3 N2 C2 113.2(6) . . ?
C3 N2 Tm1 112.9(4) . . ?
C2 N2 Tm1 113.2(4) . . ?
C3 N2 H2C 105.6 . . ?
C2 N2 H2C 105.6 . . ?
Tm1 N2 H2C 105.6 . . ?
C8 N5 Tm1 115.5(4) . . ?
C8 N5 H5A 108.4 . . ?
Tm1 N5 H5A 108.4 . . ?
C8 N5 H5B 108.4 . . ?
Tm1 N5 H5B 108.4 . . ?
H5A N5 H5B 107.5 . . ?
C1 N1 Tm1 114.7(4) . . ?
C1 N1 H1A 108.6 . . ?
Tm1 N1 H1A 108.6 . . ?
C1 N1 H1B 108.6 . . ?
Tm1 N1 H1B 108.6 . . ?
H1A N1 H1B 107.6 . . ?
N4 C7 C8 111.2(6) . . ?
N4 C7 H7A 109.4 . . ?
C8 C7 H7A 109.4 . . ?
N4 C7 H7B 109.4 . . ?
C8 C7 H7B 109.4 . . ?
H7A C7 H7B 108.0 . . ?
N3 C5 C6 108.5(5) . . ?
N3 C5 H5C 110.0 . . ?
C6 C5 H5C 110.0 . . ?
N3 C5 H5D 110.0 . . ?
C6 C5 H5D 110.0 . . ?
H5C C5 H5D 108.4 . . ?
N1 C1 C2 108.1(6) . . ?
N1 C1 H1C 110.1 . . ?
C2 C1 H1C 110.1 . . ?
N1 C1 H1D 110.1 . . ?
C2 C1 H1D 110.1 . . ?
H1C C1 H1D 108.4 . . ?
N4 C6 C5 109.1(5) . . ?
N4 C6 H6A 109.9 . . ?
C5 C6 H6A 109.9 . . ?
N4 C6 H6B 109.9 . . ?
C5 C6 H6B 109.9 . . ?
H6A C6 H6B 108.3 . . ?
N5 C8 C7 108.7(5) . . ?
N5 C8 H8A 110.0 . . ?
C7 C8 H8A 110.0 . . ?
N5 C8 H8B 110.0 . . ?
C7 C8 H8B 110.0 . . ?
H8A C8 H8B 108.3 . . ?
N3 C4 C3 108.7(6) . . ?
N3 C4 H4A 109.9 . . ?
C3 C4 H4A 109.9 . . ?
N3 C4 H4B 109.9 . . ?
C3 C4 H4B 109.9 . . ?
H4A C4 H4B 108.3 . . ?
N2 C2 C1 110.0(5) . . ?
N2 C2 H2A 109.7 . . ?
C1 C2 H2A 109.7 . . ?
N2 C2 H2B 109.7 . . ?
C1 C2 H2B 109.7 . . ?
H2A C2 H2B 108.2 . . ?
N2 C3 C4 110.7(5) . . ?
N2 C3 H3A 109.5 . . ?
C4 C3 H3A 109.5 . . ?
N2 C3 H3B 109.5 . . ?
C4 C3 H3B 109.5 . . ?
H3A C3 H3B 108.1 . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.10
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.826
_refine_diff_density_min         -0.748
_refine_diff_density_rms         0.137

# SQUEEZE RESULTS (APPEND TO CIF)
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.250 0.500 0.122 470.0 98.1
2 0.250 1.000 0.871 470.0 98.1
3 0.750 0.500 0.371 470.0 98.1
4 0.750 1.000 0.622 470.0 98.1
_platon_squeeze_details          
;
;

########End
_database_code_depnum_ccdc_archive 'CCDC 1022861'
