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

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#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
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# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  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
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#  data retrieval see:
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#  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.
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data_1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H38 Ho N8, 0.5(Se6 Sn2), Cl'
_chemical_formula_sum            'C12 H38 Cl Ho N8 Se3 Sn'
_chemical_formula_weight         850.45

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Ho Ho -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

_cell_length_a                   10.1839(4)
_cell_length_b                   14.1303(5)
_cell_length_c                   18.0100(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.5710(10)
_cell_angle_gamma                90.00
_cell_volume                     2529.54(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            YELLOW
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.233
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1608
_exptl_absorpt_coefficient_mu    8.529
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.2555
_exptl_absorpt_correction_T_max  0.3611
_exptl_absorpt_process_details   'optimized using Stoe X-shape'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(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            18668
_diffrn_reflns_av_R_equivalents  0.0308
_diffrn_reflns_av_sigmaI/netI    0.0268
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.85
_diffrn_reflns_theta_max         25.10
_reflns_number_total             4453
_reflns_number_gt                4010
_reflns_threshold_expression     >2sigma(I)

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

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

_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)+(0.0211P)²+6.7254P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4453
_refine_ls_number_parameters     239
_refine_ls_number_restraints     324
_refine_ls_R_factor_all          0.0296
_refine_ls_R_factor_gt           0.0251
_refine_ls_wR_factor_ref         0.0583
_refine_ls_wR_factor_gt          0.0566
_refine_ls_goodness_of_fit_ref   1.143
_refine_ls_restrained_S_all      1.186
_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
Ho1 Ho 0.56157(2) 0.263984(16) 0.135637(12) 0.01440(7) Uani 1 1 d . . .
Sn1 Sn 0.09897(3) 0.56517(2) 0.077949(17) 0.01459(9) Uani 1 1 d . . .
Se1 Se 0.34726(5) 0.57717(4) 0.09173(3) 0.01994(12) Uani 1 1 d . . .
Se3 Se 0.01549(5) 0.64777(4) 0.17732(3) 0.02133(12) Uani 1 1 d . . .
Se2 Se 0.02407(5) 0.38972(4) 0.05881(3) 0.02074(12) Uani 1 1 d . . .
Cl1 Cl 0.44960(14) 0.93996(10) 0.12686(9) 0.0346(3) Uani 1 1 d . . .
N1 N 0.4604(5) 0.1670(3) 0.2253(3) 0.0288(10) Uani 1 1 d U . .
H1A H 0.4158 0.1181 0.1994 0.035 Uiso 1 1 calc R . .
H1B H 0.5274 0.1430 0.2614 0.035 Uiso 1 1 calc R . .
N2 N 0.3990(4) 0.3561(3) 0.1920(2) 0.0258(9) Uani 1 1 d U . .
H2A H 0.4454 0.3909 0.2309 0.031 Uiso 1 1 calc R . .
H2B H 0.3545 0.3964 0.1567 0.031 Uiso 1 1 calc R . .
N3 N 0.6426(4) 0.4285(3) 0.1218(2) 0.0229(9) Uani 1 1 d U . .
H3A H 0.6911 0.4288 0.0855 0.027 Uiso 1 1 calc R . .
H3B H 0.5709 0.4664 0.1060 0.027 Uiso 1 1 calc R . .
N4 N 0.7221(4) 0.3148(3) 0.2540(2) 0.0232(9) Uani 1 1 d U . .
H4A H 0.6756 0.3346 0.2883 0.028 Uiso 1 1 calc R . .
H4B H 0.7729 0.2651 0.2741 0.028 Uiso 1 1 calc R . .
N5 N 0.6984(5) 0.1164(3) 0.1680(2) 0.0270(9) Uani 1 1 d U . .
H5A H 0.7461 0.1209 0.2162 0.032 Uiso 1 1 calc R . .
H5B H 0.6422 0.0668 0.1658 0.032 Uiso 1 1 calc R . .
N6 N 0.7232(5) 0.2422(3) 0.0512(3) 0.0305(10) Uani 1 1 d U . .
H6A H 0.6764 0.2389 0.0027 0.037 Uiso 1 1 calc R . .
H6B H 0.7764 0.2936 0.0552 0.037 Uiso 1 1 calc R . .
N7 N 0.4329(5) 0.1482(4) 0.0459(3) 0.0381(11) Uani 1 1 d U . .
H7A H 0.4783 0.1332 0.0099 0.046 Uiso 1 1 calc R . .
H7B H 0.4194 0.0950 0.0706 0.046 Uiso 1 1 calc R . .
N8 N 0.4197(5) 0.3412(4) 0.0199(3) 0.0361(11) Uani 1 1 d U . .
H8A H 0.3667 0.3846 0.0354 0.043 Uiso 1 1 calc R . .
H8B H 0.4746 0.3723 -0.0047 0.043 Uiso 1 1 calc R . .
C1 C 0.3662(7) 0.2198(5) 0.2635(4) 0.0446(15) Uani 1 1 d U . .
H1C H 0.2976 0.1766 0.2728 0.053 Uiso 1 1 calc R . .
H1D H 0.4158 0.2427 0.3124 0.053 Uiso 1 1 calc R . .
C2 C 0.3016(6) 0.2989(4) 0.2198(4) 0.0385(13) Uani 1 1 d U . .
H2 H 0.2454 0.2707 0.1740 0.046 Uiso 1 1 calc R . .
C3 C 0.2053(5) 0.3515(4) 0.2566(3) 0.0278(12) Uani 1 1 d U . .
H3C H 0.1457 0.3074 0.2729 0.042 Uiso 1 1 calc R . .
H3D H 0.1540 0.3950 0.2207 0.042 Uiso 1 1 calc R . .
H3E H 0.2546 0.3859 0.2997 0.042 Uiso 1 1 calc R . .
C4 C 0.7258(6) 0.4676(4) 0.1926(3) 0.0303(12) Uani 1 1 d U . .
H4C H 0.6677 0.4957 0.2227 0.036 Uiso 1 1 calc R . .
H4D H 0.7834 0.5170 0.1801 0.036 Uiso 1 1 calc R . .
C5 C 0.8108(5) 0.3924(4) 0.2385(3) 0.0292(12) Uani 1 1 d U . .
H5 H 0.8712 0.3666 0.2080 0.035 Uiso 1 1 calc R . .
C6 C 0.8964(6) 0.4343(5) 0.3108(3) 0.0377(14) Uani 1 1 d U . .
H6C H 0.8389 0.4594 0.3417 0.057 Uiso 1 1 calc R . .
H6D H 0.9515 0.4840 0.2978 0.057 Uiso 1 1 calc R . .
H6E H 0.9527 0.3858 0.3384 0.057 Uiso 1 1 calc R . .
C7 C 0.7896(8) 0.0979(6) 0.1189(4) 0.0589(16) Uani 1 1 d U . .
H7 H 0.8371 0.0412 0.1238 0.071 Uiso 1 1 calc R . .
C8 C 0.8068(9) 0.1598(6) 0.0672(5) 0.0659(17) Uani 1 1 d U . .
C9 C 0.8996(7) 0.1423(5) 0.0145(5) 0.0514(18) Uani 1 1 d U . .
H9A H 0.9518 0.0864 0.0302 0.077 Uiso 1 1 calc R . .
H9B H 0.9587 0.1955 0.0158 0.077 Uiso 1 1 calc R . .
H9C H 0.8477 0.1339 -0.0364 0.077 Uiso 1 1 calc R . .
C10 C 0.3349(6) 0.2784(4) -0.0339(3) 0.0340(13) Uani 1 1 d U . .
H10A H 0.3823 0.2577 -0.0722 0.041 Uiso 1 1 calc R . .
H10B H 0.2537 0.3112 -0.0592 0.041 Uiso 1 1 calc R . .
C11 C 0.2991(6) 0.1938(5) 0.0098(4) 0.0404(14) Uani 1 1 d U . .
H11 H 0.2573 0.2169 0.0505 0.048 Uiso 1 1 calc R . .
C12 C 0.2069(7) 0.1286(6) -0.0372(4) 0.0572(19) Uani 1 1 d U . .
H12A H 0.2489 0.1021 -0.0753 0.086 Uiso 1 1 calc R . .
H12B H 0.1268 0.1619 -0.0614 0.086 Uiso 1 1 calc R . .
H12C H 0.1840 0.0788 -0.0060 0.086 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
Ho1 N7 2.467(5) . ?
Ho1 N2 2.490(4) . ?
Ho1 N6 2.491(4) . ?
Ho1 N4 2.493(4) . ?
Ho1 N3 2.497(4) . ?
Ho1 N1 2.504(4) . ?
Ho1 N5 2.506(4) . ?
Ho1 N8 2.513(5) . ?
Sn1 Se3 2.4393(6) . ?
Sn1 Se1 2.4921(6) . ?
Sn1 Se2 2.5884(6) 3_565 ?
Sn1 Se2 2.5947(6) . ?
Se2 Sn1 2.5884(6) 3_565 ?
N1 C1 1.496(7) . ?
N1 H1A 0.9000 . ?
N1 H1B 0.9000 . ?
N2 C2 1.449(7) . ?
N2 H2A 0.9000 . ?
N2 H2B 0.9000 . ?
N3 C4 1.477(7) . ?
N3 H3A 0.9000 . ?
N3 H3B 0.9000 . ?
N4 C5 1.486(7) . ?
N4 H4A 0.9000 . ?
N4 H4B 0.9000 . ?
N5 C7 1.438(8) . ?
N5 H5A 0.9000 . ?
N5 H5B 0.9000 . ?
N6 C8 1.435(8) . ?
N6 H6A 0.9000 . ?
N6 H6B 0.9000 . ?
N7 C11 1.519(8) . ?
N7 H7A 0.9000 . ?
N7 H7B 0.9000 . ?
N8 C10 1.452(7) . ?
N8 H8A 0.9000 . ?
N8 H8B 0.9000 . ?
C1 C2 1.441(9) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C2 C3 1.495(8) . ?
C2 H2 0.9800 . ?
C3 H3C 0.9600 . ?
C3 H3D 0.9600 . ?
C3 H3E 0.9600 . ?
C4 C5 1.500(8) . ?
C4 H4C 0.9700 . ?
C4 H4D 0.9700 . ?
C5 C6 1.519(8) . ?
C5 H5 0.9800 . ?
C6 H6C 0.9600 . ?
C6 H6D 0.9600 . ?
C6 H6E 0.9600 . ?
C7 C8 1.317(10) . ?
C7 H7 0.9300 . ?
C8 C9 1.499(9) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 C11 1.519(9) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C12 1.449(9) . ?
C11 H11 0.9800 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?

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
N7 Ho1 N2 107.97(17) . . ?
N7 Ho1 N6 81.10(17) . . ?
N2 Ho1 N6 154.16(15) . . ?
N7 Ho1 N4 155.14(15) . . ?
N2 Ho1 N4 82.59(15) . . ?
N6 Ho1 N4 99.23(16) . . ?
N7 Ho1 N3 133.76(15) . . ?
N2 Ho1 N3 79.50(14) . . ?
N6 Ho1 N3 77.13(15) . . ?
N4 Ho1 N3 69.40(14) . . ?
N7 Ho1 N1 79.95(17) . . ?
N2 Ho1 N1 67.63(14) . . ?
N6 Ho1 N1 138.19(15) . . ?
N4 Ho1 N1 83.75(15) . . ?
N3 Ho1 N1 139.91(15) . . ?
N7 Ho1 N5 77.85(16) . . ?
N2 Ho1 N5 136.54(14) . . ?
N6 Ho1 N5 68.36(15) . . ?
N4 Ho1 N5 79.22(15) . . ?
N3 Ho1 N5 128.24(15) . . ?
N1 Ho1 N5 71.38(15) . . ?
N7 Ho1 N8 67.47(16) . . ?
N2 Ho1 N8 78.35(16) . . ?
N6 Ho1 N8 83.35(16) . . ?
N4 Ho1 N8 137.39(16) . . ?
N3 Ho1 N8 69.85(16) . . ?
N1 Ho1 N8 121.99(16) . . ?
N5 Ho1 N8 138.14(15) . . ?
Se3 Sn1 Se1 113.73(2) . . ?
Se3 Sn1 Se2 113.99(2) . 3_565 ?
Se1 Sn1 Se2 110.40(2) . 3_565 ?
Se3 Sn1 Se2 114.54(2) . . ?
Se1 Sn1 Se2 109.93(2) . . ?
Se2 Sn1 Se2 92.378(18) 3_565 . ?
Sn1 Se2 Sn1 87.622(18) 3_565 . ?
C1 N1 Ho1 114.7(3) . . ?
C1 N1 H1A 108.6 . . ?
Ho1 N1 H1A 108.6 . . ?
C1 N1 H1B 108.6 . . ?
Ho1 N1 H1B 108.6 . . ?
H1A N1 H1B 107.6 . . ?
C2 N2 Ho1 114.5(3) . . ?
C2 N2 H2A 108.6 . . ?
Ho1 N2 H2A 108.6 . . ?
C2 N2 H2B 108.6 . . ?
Ho1 N2 H2B 108.6 . . ?
H2A N2 H2B 107.6 . . ?
C4 N3 Ho1 113.7(3) . . ?
C4 N3 H3A 108.8 . . ?
Ho1 N3 H3A 108.8 . . ?
C4 N3 H3B 108.8 . . ?
Ho1 N3 H3B 108.8 . . ?
H3A N3 H3B 107.7 . . ?
C5 N4 Ho1 111.4(3) . . ?
C5 N4 H4A 109.4 . . ?
Ho1 N4 H4A 109.4 . . ?
C5 N4 H4B 109.4 . . ?
Ho1 N4 H4B 109.4 . . ?
H4A N4 H4B 108.0 . . ?
C7 N5 Ho1 114.2(4) . . ?
C7 N5 H5A 108.7 . . ?
Ho1 N5 H5A 108.7 . . ?
C7 N5 H5B 108.7 . . ?
Ho1 N5 H5B 108.7 . . ?
H5A N5 H5B 107.6 . . ?
C8 N6 Ho1 114.8(4) . . ?
C8 N6 H6A 108.6 . . ?
Ho1 N6 H6A 108.6 . . ?
C8 N6 H6B 108.6 . . ?
Ho1 N6 H6B 108.6 . . ?
H6A N6 H6B 107.5 . . ?
C11 N7 Ho1 107.3(4) . . ?
C11 N7 H7A 110.2 . . ?
Ho1 N7 H7A 110.2 . . ?
C11 N7 H7B 110.2 . . ?
Ho1 N7 H7B 110.2 . . ?
H7A N7 H7B 108.5 . . ?
C10 N8 Ho1 116.1(4) . . ?
C10 N8 H8A 108.3 . . ?
Ho1 N8 H8A 108.3 . . ?
C10 N8 H8B 108.3 . . ?
Ho1 N8 H8B 108.3 . . ?
H8A N8 H8B 107.4 . . ?
C2 C1 N1 113.5(5) . . ?
C2 C1 H1C 108.9 . . ?
N1 C1 H1C 108.9 . . ?
C2 C1 H1D 108.9 . . ?
N1 C1 H1D 108.9 . . ?
H1C C1 H1D 107.7 . . ?
C1 C2 N2 110.8(5) . . ?
C1 C2 C3 114.1(5) . . ?
N2 C2 C3 116.1(5) . . ?
C1 C2 H2 104.8 . . ?
N2 C2 H2 104.8 . . ?
C3 C2 H2 104.8 . . ?
C2 C3 H3C 109.5 . . ?
C2 C3 H3D 109.5 . . ?
H3C C3 H3D 109.5 . . ?
C2 C3 H3E 109.5 . . ?
H3C C3 H3E 109.5 . . ?
H3D C3 H3E 109.5 . . ?
N3 C4 C5 111.4(5) . . ?
N3 C4 H4C 109.3 . . ?
C5 C4 H4C 109.3 . . ?
N3 C4 H4D 109.3 . . ?
C5 C4 H4D 109.3 . . ?
H4C C4 H4D 108.0 . . ?
N4 C5 C4 108.9(4) . . ?
N4 C5 C6 112.7(5) . . ?
C4 C5 C6 110.5(5) . . ?
N4 C5 H5 108.2 . . ?
C4 C5 H5 108.2 . . ?
C6 C5 H5 108.2 . . ?
C5 C6 H6C 109.5 . . ?
C5 C6 H6D 109.5 . . ?
H6C C6 H6D 109.5 . . ?
C5 C6 H6E 109.5 . . ?
H6C C6 H6E 109.5 . . ?
H6D C6 H6E 109.5 . . ?
C8 C7 N5 121.1(6) . . ?
C8 C7 H7 119.4 . . ?
N5 C7 H7 119.4 . . ?
C7 C8 N6 121.1(6) . . ?
C7 C8 C9 122.5(7) . . ?
N6 C8 C9 115.8(6) . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N8 C10 C11 108.1(5) . . ?
N8 C10 H10A 110.1 . . ?
C11 C10 H10A 110.1 . . ?
N8 C10 H10B 110.1 . . ?
C11 C10 H10B 110.1 . . ?
H10A C10 H10B 108.4 . . ?
C12 C11 N7 112.8(6) . . ?
C12 C11 C10 113.3(5) . . ?
N7 C11 C10 105.1(5) . . ?
C12 C11 H11 108.5 . . ?
N7 C11 H11 108.5 . . ?
C10 C11 H11 108.5 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        25.10
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         1.572
_refine_diff_density_min         -1.709
_refine_diff_density_rms         0.127
_database_code_depnum_ccdc_archive 'CCDC 988893'
#######################################################################
#
#                 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_2

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H54 Ho2 N12 O2, Se6 Sn2'
_chemical_formula_sum            'C16 H54 Ho2 N12 O2 Se6 Sn2'
_chemical_formula_weight         1487.75

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn '
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   12.0096(6)
_cell_length_b                   11.7181(6)
_cell_length_c                   13.7717(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.1380(10)
_cell_angle_gamma                90.00
_cell_volume                     1913.49(17)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            YELLOW
_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    2.586
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1376
_exptl_absorpt_coefficient_mu    11.121
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.1808
_exptl_absorpt_correction_T_max  0.3313
_exptl_absorpt_process_details   'optimized using Stoe X-shape'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(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            13479
_diffrn_reflns_av_R_equivalents  0.0391
_diffrn_reflns_av_sigmaI/netI    0.0327
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.09
_diffrn_reflns_theta_max         25.09
_reflns_number_total             3364
_reflns_number_gt                3057
_reflns_threshold_expression     >2sigma(I)

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

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

_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)+(0.0280P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3364
_refine_ls_number_parameters     185
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0249
_refine_ls_R_factor_gt           0.0215
_refine_ls_wR_factor_ref         0.0529
_refine_ls_wR_factor_gt          0.0514
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.034
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ho1 Ho 0.475756(14) 0.418188(15) 0.611311(12) 0.01238(7) Uani 1 1 d . . .
Sn1 Sn 0.50550(2) 0.02112(2) 0.872515(18) 0.01444(8) Uani 1 1 d . . .
Se1 Se 0.66822(3) 0.12188(4) 0.82328(3) 0.01895(11) Uani 1 1 d . . .
Se2 Se 0.42335(3) 0.13921(3) 1.00535(3) 0.01823(10) Uani 1 1 d . . .
Se3 Se 0.36123(3) -0.02355(3) 0.73035(3) 0.01900(11) Uani 1 1 d . . .
O1W O 0.4190(2) 0.4486(2) 0.45120(19) 0.0172(6) Uani 1 1 d D . .
N1 N 0.2726(3) 0.3525(3) 0.5833(2) 0.0175(7) Uani 1 1 d . . .
H1A H 0.2403 0.3743 0.6350 0.021 Uiso 1 1 calc R . .
H1B H 0.2359 0.3880 0.5296 0.021 Uiso 1 1 calc R . .
N2 N 0.4578(3) 0.2075(3) 0.5664(2) 0.0161(7) Uani 1 1 d . . .
H2C H 0.4717 0.1650 0.6223 0.019 Uiso 1 1 calc R . .
N3 N 0.6625(3) 0.3122(3) 0.6225(2) 0.0207(8) Uani 1 1 d . . .
H3A H 0.7129 0.3594 0.6018 0.025 Uiso 1 1 calc R . .
H3B H 0.6874 0.2966 0.6862 0.025 Uiso 1 1 calc R . .
N4 N 0.4488(3) 0.3290(3) 0.7738(2) 0.0210(8) Uani 1 1 d . . .
H4A H 0.3760 0.3084 0.7697 0.025 Uiso 1 1 calc R . .
H4B H 0.4905 0.2649 0.7824 0.025 Uiso 1 1 calc R . .
N5 N 0.5895(3) 0.5204(3) 0.7614(2) 0.0179(7) Uani 1 1 d . . .
H5C H 0.6623 0.5221 0.7506 0.022 Uiso 1 1 calc R . .
N6 N 0.3692(3) 0.5836(3) 0.6647(3) 0.0199(8) Uani 1 1 d . . .
H6A H 0.3522 0.6310 0.6130 0.024 Uiso 1 1 calc R . .
H6B H 0.3036 0.5572 0.6797 0.024 Uiso 1 1 calc R . .
C1 C 0.2576(3) 0.2281(3) 0.5699(3) 0.0200(9) Uani 1 1 d . . .
H1C H 0.1826 0.2125 0.5347 0.024 Uiso 1 1 calc R . .
H1D H 0.2647 0.1914 0.6337 0.024 Uiso 1 1 calc R . .
C2 C 0.3438(3) 0.1803(4) 0.5137(3) 0.0194(9) Uani 1 1 d . . .
H2A H 0.3347 0.0983 0.5074 0.023 Uiso 1 1 calc R . .
H2B H 0.3338 0.2131 0.4482 0.023 Uiso 1 1 calc R . .
C3 C 0.5459(3) 0.1843(4) 0.5056(3) 0.0203(9) Uani 1 1 d . . .
H3C H 0.5357 0.2343 0.4487 0.024 Uiso 1 1 calc R . .
H3D H 0.5398 0.1060 0.4825 0.024 Uiso 1 1 calc R . .
C4 C 0.6611(3) 0.2040(4) 0.5660(3) 0.0210(9) Uani 1 1 d . . .
H4C H 0.6798 0.1408 0.6111 0.025 Uiso 1 1 calc R . .
H4D H 0.7174 0.2074 0.5228 0.025 Uiso 1 1 calc R . .
C5 C 0.4787(4) 0.4015(4) 0.8614(3) 0.0229(9) Uani 1 1 d . . .
H5A H 0.4851 0.3552 0.9205 0.028 Uiso 1 1 calc R . .
H5B H 0.4205 0.4583 0.8639 0.028 Uiso 1 1 calc R . .
C6 C 0.5907(4) 0.4599(4) 0.8560(3) 0.0234(10) Uani 1 1 d . . .
H6C H 0.6069 0.5141 0.9096 0.028 Uiso 1 1 calc R . .
H6D H 0.6503 0.4033 0.8638 0.028 Uiso 1 1 calc R . .
C7 C 0.5520(3) 0.6409(4) 0.7610(3) 0.0215(9) Uani 1 1 d . . .
H7A H 0.5786 0.6810 0.7075 0.026 Uiso 1 1 calc R . .
H7B H 0.5855 0.6770 0.8221 0.026 Uiso 1 1 calc R . .
C8 C 0.4253(4) 0.6516(4) 0.7494(3) 0.0231(9) Uani 1 1 d . . .
H8A H 0.3998 0.6254 0.8090 0.028 Uiso 1 1 calc R . .
H8B H 0.4041 0.7312 0.7397 0.028 Uiso 1 1 calc R . .
H1W H 0.354(2) 0.433(4) 0.425(3) 0.026(13) Uiso 1 1 d D . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ho1 O1W 2.231(3) . ?
Ho1 O1W 2.263(3) 3_666 ?
Ho1 N6 2.497(3) . ?
Ho1 N1 2.529(3) . ?
Ho1 N4 2.537(3) . ?
Ho1 N2 2.545(3) . ?
Ho1 N3 2.547(3) . ?
Ho1 N5 2.584(3) . ?
Ho1 Ho1 3.7393(4) 3_666 ?
Sn1 Se3 2.4560(5) . ?
Sn1 Se1 2.4685(5) . ?
Sn1 Se2 2.5754(5) 3_657 ?
Sn1 Se2 2.6092(5) . ?
Se2 Sn1 2.5754(5) 3_657 ?
O1W Ho1 2.263(3) 3_666 ?
O1W H1W 0.831(19) . ?
N1 C1 1.476(5) . ?
N1 H1A 0.9000 . ?
N1 H1B 0.9000 . ?
N2 C3 1.474(5) . ?
N2 C2 1.479(5) . ?
N2 H2C 0.9100 . ?
N3 C4 1.486(5) . ?
N3 H3A 0.9000 . ?
N3 H3B 0.9000 . ?
N4 C5 1.473(5) . ?
N4 H4A 0.9000 . ?
N4 H4B 0.9000 . ?
N5 C6 1.480(5) . ?
N5 C7 1.481(5) . ?
N5 H5C 0.9100 . ?
N6 C8 1.483(5) . ?
N6 H6A 0.9000 . ?
N6 H6B 0.9000 . ?
C1 C2 1.497(5) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.515(6) . ?
C3 H3C 0.9700 . ?
C3 H3D 0.9700 . ?
C4 H4C 0.9700 . ?
C4 H4D 0.9700 . ?
C5 C6 1.521(6) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 H6C 0.9700 . ?
C6 H6D 0.9700 . ?
C7 C8 1.510(6) . ?
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 Ho1 O1W 67.36(11) . 3_666 ?
O1W Ho1 N6 94.38(11) . . ?
O1W Ho1 N6 85.39(11) 3_666 . ?
O1W Ho1 N1 76.23(10) . . ?
O1W Ho1 N1 137.35(10) 3_666 . ?
N6 Ho1 N1 75.76(11) . . ?
O1W Ho1 N4 151.16(10) . . ?
O1W Ho1 N4 141.01(10) 3_666 . ?
N6 Ho1 N4 85.25(12) . . ?
N1 Ho1 N4 75.75(11) . . ?
O1W Ho1 N2 85.06(10) . . ?
O1W Ho1 N2 127.39(10) 3_666 . ?
N6 Ho1 N2 142.84(11) . . ?
N1 Ho1 N2 68.01(10) . . ?
N4 Ho1 N2 78.28(11) . . ?
O1W Ho1 N3 105.40(11) . . ?
O1W Ho1 N3 79.62(11) 3_666 . ?
N6 Ho1 N3 148.04(11) . . ?
N1 Ho1 N3 132.82(11) . . ?
N4 Ho1 N3 88.87(11) . . ?
N2 Ho1 N3 65.25(11) . . ?
O1W Ho1 N5 139.14(10) . . ?
O1W Ho1 N5 74.24(10) 3_666 . ?
N6 Ho1 N5 68.60(11) . . ?
N1 Ho1 N5 129.63(11) . . ?
N4 Ho1 N5 67.10(11) . . ?
N2 Ho1 N5 131.11(10) . . ?
N3 Ho1 N5 80.17(11) . . ?
O1W Ho1 Ho1 33.95(7) . 3_666 ?
O1W Ho1 Ho1 33.41(7) 3_666 3_666 ?
N6 Ho1 Ho1 89.83(8) . 3_666 ?
N1 Ho1 Ho1 107.64(7) . 3_666 ?
N4 Ho1 Ho1 173.17(8) . 3_666 ?
N2 Ho1 Ho1 108.43(7) . 3_666 ?
N3 Ho1 Ho1 92.83(8) . 3_666 ?
N5 Ho1 Ho1 106.67(7) . 3_666 ?
Se3 Sn1 Se1 111.841(17) . . ?
Se3 Sn1 Se2 118.951(17) . 3_657 ?
Se1 Sn1 Se2 109.467(16) . 3_657 ?
Se3 Sn1 Se2 111.995(17) . . ?
Se1 Sn1 Se2 110.054(17) . . ?
Se2 Sn1 Se2 92.990(15) 3_657 . ?
Sn1 Se2 Sn1 87.010(15) 3_657 . ?
Ho1 O1W Ho1 112.64(11) . 3_666 ?
Ho1 O1W H1W 121(3) . . ?
Ho1 O1W H1W 122(3) 3_666 . ?
C1 N1 Ho1 114.5(2) . . ?
C1 N1 H1A 108.6 . . ?
Ho1 N1 H1A 108.6 . . ?
C1 N1 H1B 108.6 . . ?
Ho1 N1 H1B 108.6 . . ?
H1A N1 H1B 107.6 . . ?
C3 N2 C2 111.9(3) . . ?
C3 N2 Ho1 106.0(2) . . ?
C2 N2 Ho1 111.4(2) . . ?
C3 N2 H2C 109.2 . . ?
C2 N2 H2C 109.2 . . ?
Ho1 N2 H2C 109.2 . . ?
C4 N3 Ho1 116.6(2) . . ?
C4 N3 H3A 108.1 . . ?
Ho1 N3 H3A 108.1 . . ?
C4 N3 H3B 108.1 . . ?
Ho1 N3 H3B 108.1 . . ?
H3A N3 H3B 107.3 . . ?
C5 N4 Ho1 115.8(2) . . ?
C5 N4 H4A 108.3 . . ?
Ho1 N4 H4A 108.3 . . ?
C5 N4 H4B 108.3 . . ?
Ho1 N4 H4B 108.3 . . ?
H4A N4 H4B 107.4 . . ?
C6 N5 C7 114.9(3) . . ?
C6 N5 Ho1 114.3(2) . . ?
C7 N5 Ho1 108.5(2) . . ?
C6 N5 H5C 106.2 . . ?
C7 N5 H5C 106.2 . . ?
Ho1 N5 H5C 106.2 . . ?
C8 N6 Ho1 117.3(2) . . ?
C8 N6 H6A 108.0 . . ?
Ho1 N6 H6A 108.0 . . ?
C8 N6 H6B 108.0 . . ?
Ho1 N6 H6B 108.0 . . ?
H6A N6 H6B 107.2 . . ?
N1 C1 C2 110.7(3) . . ?
N1 C1 H1C 109.5 . . ?
C2 C1 H1C 109.5 . . ?
N1 C1 H1D 109.5 . . ?
C2 C1 H1D 109.5 . . ?
H1C C1 H1D 108.1 . . ?
N2 C2 C1 109.1(3) . . ?
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 109.6(3) . . ?
N2 C3 H3C 109.8 . . ?
C4 C3 H3C 109.8 . . ?
N2 C3 H3D 109.8 . . ?
C4 C3 H3D 109.8 . . ?
H3C C3 H3D 108.2 . . ?
N3 C4 C3 110.6(3) . . ?
N3 C4 H4C 109.5 . . ?
C3 C4 H4C 109.5 . . ?
N3 C4 H4D 109.5 . . ?
C3 C4 H4D 109.5 . . ?
H4C C4 H4D 108.1 . . ?
N4 C5 C6 108.8(3) . . ?
N4 C5 H5A 109.9 . . ?
C6 C5 H5A 109.9 . . ?
N4 C5 H5B 109.9 . . ?
C6 C5 H5B 109.9 . . ?
H5A C5 H5B 108.3 . . ?
N5 C6 C5 112.0(3) . . ?
N5 C6 H6C 109.2 . . ?
C5 C6 H6C 109.2 . . ?
N5 C6 H6D 109.2 . . ?
C5 C6 H6D 109.2 . . ?
H6C C6 H6D 107.9 . . ?
N5 C7 C8 112.4(3) . . ?
N5 C7 H7A 109.1 . . ?
C8 C7 H7A 109.1 . . ?
N5 C7 H7B 109.1 . . ?
C8 C7 H7B 109.1 . . ?
H7A C7 H7B 107.9 . . ?
N6 C8 C7 111.3(3) . . ?
N6 C8 H8A 109.4 . . ?
C7 C8 H8A 109.4 . . ?
N6 C8 H8B 109.4 . . ?
C7 C8 H8B 109.4 . . ?
H8A C8 H8B 108.0 . . ?

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        25.09
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         1.256
_refine_diff_density_min         -0.970
_refine_diff_density_rms         0.143
_database_code_depnum_ccdc_archive 'CCDC 988894'
#######################################################################
#
#                 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_3

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C16 H48 Cl2 Ho2 N10 O2), Se10 Sn4, 4(H2 O)'
_chemical_formula_sum            'C32 H104 Cl4 Ho4 N20 O8 Se10 Sn4'
_chemical_formula_weight         2963.20

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

_symmetry_cell_setting           Tetragonal
_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                   28.0757(12)
_cell_length_b                   28.0757(12)
_cell_length_c                   10.9479(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     8629.6(9)
_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          0.11
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.281
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5408
_exptl_absorpt_coefficient_mu    9.144
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.2006
_exptl_absorpt_correction_T_max  0.3014
_exptl_absorpt_process_details   'optimized using Stoe X-shape'

_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            15679
_diffrn_reflns_av_R_equivalents  0.0390
_diffrn_reflns_av_sigmaI/netI    0.0339
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.47
_diffrn_reflns_theta_max         25.09
_reflns_number_total             3821
_reflns_number_gt                3291
_reflns_threshold_expression     >2sigma(I)

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

_refine_special_details          
; 
 Structure 3 contains large solvent-accessible voids, 
which are filled by the free disorded H₂O molecules, 
but parts of H₂O molecules are difficult to locate in 
the final structural refinement. 
The numbers of free H₂O molecules is further confirmed 
by elemental analyses and TGA analysis. 
So the chemical formula of 3 is [Ho₂(tepa)₂(OH)₂Cl₂]₂[Sn₄Se₁₀].4H₂O.
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)+(0.0330P)²+71.7375P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3821
_refine_ls_number_parameters     199
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.0348
_refine_ls_R_factor_gt           0.0273
_refine_ls_wR_factor_ref         0.0741
_refine_ls_wR_factor_gt          0.0704
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.058
_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
Ho1 Ho 0.445979(9) 0.526521(9) 0.56707(2) 0.01447(9) Uani 1 1 d . . .
Sn1 Sn 0.454082(14) 0.307611(13) 0.74604(3) 0.01387(11) Uani 1 1 d . . .
Se1 Se 0.41137(2) 0.36378(2) 0.61554(5) 0.01671(14) Uani 1 1 d . . .
Se2 Se 0.39393(2) 0.26217(2) 0.87553(5) 0.01817(15) Uani 1 1 d . . .
Se3 Se 0.5000 0.2500 0.61071(7) 0.01617(18) Uani 1 2 d S . .
Cl1 Cl 0.38815(6) 0.47450(6) 0.41676(15) 0.0280(4) Uani 1 1 d . . .
O1W O 0.51028(14) 0.54171(14) 0.4552(4) 0.0163(9) Uani 1 1 d D . .
N1 N 0.36301(19) 0.5508(2) 0.6450(5) 0.0267(12) Uani 1 1 d . . .
H1A H 0.3617 0.5828 0.6495 0.032 Uiso 1 1 calc R . .
H1B H 0.3411 0.5413 0.5902 0.032 Uiso 1 1 calc R . .
N2 N 0.41780(19) 0.47573(18) 0.7450(5) 0.0227(12) Uani 1 1 d . . .
H2C H 0.4228 0.4450 0.7216 0.027 Uiso 1 1 calc R . .
N3 N 0.50438(18) 0.52869(17) 0.7426(4) 0.0191(11) Uani 1 1 d . . .
H3C H 0.5336 0.5248 0.7080 0.023 Uiso 1 1 calc R . .
N4 N 0.45882(18) 0.61006(17) 0.6440(5) 0.0187(11) Uani 1 1 d . . .
H4C H 0.4347 0.6162 0.6973 0.022 Uiso 1 1 calc R . .
N5 N 0.41527(19) 0.58876(19) 0.4164(5) 0.0248(12) Uani 1 1 d . . .
H5A H 0.4345 0.5892 0.3506 0.030 Uiso 1 1 calc R . .
H5B H 0.3860 0.5801 0.3910 0.030 Uiso 1 1 calc R . .
C1 C 0.3505(3) 0.5309(2) 0.7651(7) 0.0313(16) Uani 1 1 d . . .
H1C H 0.3164 0.5331 0.7779 0.038 Uiso 1 1 calc R . .
H1D H 0.3663 0.5488 0.8292 0.038 Uiso 1 1 calc R . .
C2 C 0.3660(2) 0.4794(2) 0.7691(7) 0.0303(16) Uani 1 1 d . . .
H2A H 0.3589 0.4660 0.8488 0.036 Uiso 1 1 calc R . .
H2B H 0.3486 0.4613 0.7082 0.036 Uiso 1 1 calc R . .
C3 C 0.4464(2) 0.4822(2) 0.8580(6) 0.0265(15) Uani 1 1 d . . .
H3A H 0.4424 0.4548 0.9110 0.032 Uiso 1 1 calc R . .
H3B H 0.4355 0.5102 0.9016 0.032 Uiso 1 1 calc R . .
C4 C 0.4984(2) 0.4878(2) 0.8252(6) 0.0261(15) Uani 1 1 d . . .
H4A H 0.5170 0.4927 0.8988 0.031 Uiso 1 1 calc R . .
H4B H 0.5098 0.4590 0.7856 0.031 Uiso 1 1 calc R . .
C5 C 0.5066(2) 0.5752(2) 0.8073(6) 0.0227(14) Uani 1 1 d . . .
H5C H 0.5362 0.5776 0.8528 0.027 Uiso 1 1 calc R . .
H5D H 0.4803 0.5778 0.8644 0.027 Uiso 1 1 calc R . .
C6 C 0.5038(2) 0.6147(2) 0.7139(6) 0.0197(13) Uani 1 1 d . . .
H6A H 0.5048 0.6453 0.7546 0.024 Uiso 1 1 calc R . .
H6B H 0.5308 0.6127 0.6588 0.024 Uiso 1 1 calc R . .
C7 C 0.4557(2) 0.6467(2) 0.5463(6) 0.0227(14) Uani 1 1 d . . .
H7A H 0.4842 0.6457 0.4963 0.027 Uiso 1 1 calc R . .
H7B H 0.4534 0.6781 0.5826 0.027 Uiso 1 1 calc R . .
C8 C 0.4128(2) 0.6375(2) 0.4683(6) 0.0250(14) Uani 1 1 d . . .
H8A H 0.3841 0.6407 0.5170 0.030 Uiso 1 1 calc R . .
H8B H 0.4115 0.6607 0.4027 0.030 Uiso 1 1 calc R . .
O2W O 0.2854(8) 0.4523(8) 1.030(2) 0.050(6) Uani 0.25 1 d PU A 1
O2W' O 0.2626(7) 0.5597(8) 0.3718(18) 0.042(5) Uani 0.25 1 d PU B 2
H1W H 0.532(3) 0.562(3) 0.440(9) 0.08(3) Uiso 1 1 d D . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ho1 O1W 2.223(4) . ?
Ho1 O1W 2.288(4) 9_666 ?
Ho1 N4 2.518(5) . ?
Ho1 N3 2.527(5) . ?
Ho1 N2 2.541(5) . ?
Ho1 N5 2.553(5) . ?
Ho1 N1 2.573(5) . ?
Ho1 Cl1 2.7344(16) . ?
Ho1 Ho1 3.6845(5) 9_666 ?
Sn1 Se1 2.4426(7) . ?
Sn1 Se3 2.5443(6) . ?
Sn1 Se2 2.5470(7) 11_667 ?
Sn1 Se2 2.5474(7) . ?
Se2 Sn1 2.5470(7) 16_657 ?
Se3 Sn1 2.5443(6) 6_554 ?
O1W Ho1 2.288(4) 9_666 ?
O1W H1W 0.85(2) . ?
N1 C1 1.470(9) . ?
N1 H1A 0.9000 . ?
N1 H1B 0.9000 . ?
N2 C2 1.481(8) . ?
N2 C3 1.486(8) . ?
N2 H2C 0.9100 . ?
N3 C4 1.472(8) . ?
N3 C5 1.487(8) . ?
N3 H3C 0.9100 . ?
N4 C6 1.482(8) . ?
N4 C7 1.487(8) . ?
N4 H4C 0.9100 . ?
N5 C8 1.483(8) . ?
N5 H5A 0.9000 . ?
N5 H5B 0.9000 . ?
C1 C2 1.512(9) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.512(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 1.500(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
O1W Ho1 O1W 70.49(17) . 9_666 ?
O1W Ho1 N4 83.65(15) . . ?
O1W Ho1 N4 137.59(15) 9_666 . ?
O1W Ho1 N3 83.54(16) . . ?
O1W Ho1 N3 75.69(15) 9_666 . ?
N4 Ho1 N3 68.29(16) . . ?
O1W Ho1 N2 141.55(16) . . ?
O1W Ho1 N2 77.23(16) 9_666 . ?
N4 Ho1 N2 108.10(16) . . ?
N3 Ho1 N2 68.43(17) . . ?
O1W Ho1 N5 77.69(16) . . ?
O1W Ho1 N5 133.27(16) 9_666 . ?
N4 Ho1 N5 68.10(17) . . ?
N3 Ho1 N5 133.95(17) . . ?
N2 Ho1 N5 140.76(18) . . ?
O1W Ho1 N1 150.15(16) . . ?
O1W Ho1 N1 137.98(16) 9_666 . ?
N4 Ho1 N1 76.82(17) . . ?
N3 Ho1 N1 109.20(17) . . ?
N2 Ho1 N1 67.19(17) . . ?
N5 Ho1 N1 74.17(18) . . ?
O1W Ho1 Cl1 104.66(11) . . ?
O1W Ho1 Cl1 78.90(11) 9_666 . ?
N4 Ho1 Cl1 141.62(12) . . ?
N3 Ho1 Cl1 148.85(12) . . ?
N2 Ho1 Cl1 88.67(12) . . ?
N5 Ho1 Cl1 77.07(13) . . ?
N1 Ho1 Cl1 78.67(13) . . ?
O1W Ho1 Ho1 35.83(10) . 9_666 ?
O1W Ho1 Ho1 34.66(10) 9_666 9_666 ?
N4 Ho1 Ho1 113.07(11) . 9_666 ?
N3 Ho1 Ho1 77.21(11) . 9_666 ?
N2 Ho1 Ho1 109.58(12) . 9_666 ?
N5 Ho1 Ho1 107.28(12) . 9_666 ?
N1 Ho1 Ho1 169.96(13) . 9_666 ?
Cl1 Ho1 Ho1 91.90(4) . 9_666 ?
Se1 Sn1 Se3 108.58(2) . . ?
Se1 Sn1 Se2 107.00(2) . 11_667 ?
Se3 Sn1 Se2 109.67(2) . 11_667 ?
Se1 Sn1 Se2 108.86(2) . . ?
Se3 Sn1 Se2 109.97(2) . . ?
Se2 Sn1 Se2 112.632(18) 11_667 . ?
Sn1 Se2 Sn1 105.89(3) 16_657 . ?
Sn1 Se3 Sn1 108.77(3) . 6_554 ?
Ho1 O1W Ho1 109.51(17) . 9_666 ?
Ho1 O1W H1W 146(7) . . ?
Ho1 O1W H1W 98(7) 9_666 . ?
C1 N1 Ho1 114.3(4) . . ?
C1 N1 H1A 108.7 . . ?
Ho1 N1 H1A 108.7 . . ?
C1 N1 H1B 108.7 . . ?
Ho1 N1 H1B 108.7 . . ?
H1A N1 H1B 107.6 . . ?
C2 N2 C3 112.0(5) . . ?
C2 N2 Ho1 113.8(4) . . ?
C3 N2 Ho1 113.7(4) . . ?
C2 N2 H2C 105.5 . . ?
C3 N2 H2C 105.5 . . ?
Ho1 N2 H2C 105.5 . . ?
C4 N3 C5 113.4(5) . . ?
C4 N3 Ho1 112.0(4) . . ?
C5 N3 Ho1 114.3(4) . . ?
C4 N3 H3C 105.4 . . ?
C5 N3 H3C 105.4 . . ?
Ho1 N3 H3C 105.4 . . ?
C6 N4 C7 111.2(5) . . ?
C6 N4 Ho1 112.1(4) . . ?
C7 N4 Ho1 113.2(4) . . ?
C6 N4 H4C 106.6 . . ?
C7 N4 H4C 106.6 . . ?
Ho1 N4 H4C 106.6 . . ?
C8 N5 Ho1 113.6(4) . . ?
C8 N5 H5A 108.9 . . ?
Ho1 N5 H5A 108.9 . . ?
C8 N5 H5B 108.9 . . ?
Ho1 N5 H5B 108.9 . . ?
H5A N5 H5B 107.7 . . ?
N1 C1 C2 108.7(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 110.1(5) . . ?
N2 C2 H2A 109.6 . . ?
C1 C2 H2A 109.6 . . ?
N2 C2 H2B 109.6 . . ?
C1 C2 H2B 109.6 . . ?
H2A C2 H2B 108.2 . . ?
N2 C3 C4 109.7(5) . . ?
N2 C3 H3A 109.7 . . ?
C4 C3 H3A 109.7 . . ?
N2 C3 H3B 109.7 . . ?
C4 C3 H3B 109.7 . . ?
H3A C3 H3B 108.2 . . ?
N3 C4 C3 109.7(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 108.6(5) . . ?
N3 C5 H5C 110.0 . . ?
C6 C5 H5C 110.0 . . ?
N3 C5 H5D 110.0 . . ?
C6 C5 H5D 110.0 . . ?
H5C C5 H5D 108.3 . . ?
N4 C6 C5 109.3(5) . . ?
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 . . ?
N4 C7 C8 109.8(5) . . ?
N4 C7 H7A 109.7 . . ?
C8 C7 H7A 109.7 . . ?
N4 C7 H7B 109.7 . . ?
C8 C7 H7B 109.7 . . ?
H7A C7 H7B 108.2 . . ?
N5 C8 C7 109.8(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 0.994
_diffrn_reflns_theta_full        25.09
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         2.124
_refine_diff_density_min         -0.568
_refine_diff_density_rms         0.158
_database_code_depnum_ccdc_archive 'CCDC 988895'
