# Electronic Supplementary Material (ESI) for CrystEngComm
# This journal is © The Royal Society of Chemistry 2012


data_global
_journal_name_full               CrystEngComm
_journal_coden_cambridge         1350
_journal_year                    ?
_journal_volume                  ?
_journal_page_first              ?
loop_
_publ_author_name
W.Bensch
B.Seidlhofer
C.Nather
_publ_contact_author_name        'W. Bensch'
_publ_contact_author_email       WBENSCH@AC.UNI-KIEL.DE

data_chris
_database_code_depnum_ccdc_archive 'CCDC 865203'
#TrackingRef '- BeS938.CIF'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            '[Ni(en)(tren)]4Sb14S25'
_chemical_melting_point          ?
_chemical_formula_moiety         'S25 Sb14, 4(C8 H26 N6 Ni)'
_chemical_formula_sum            'C32 H104 N24 Ni4 S25 Sb14'
_chemical_formula_weight         3566.23

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   16.5428(3)
_cell_length_b                   25.8974(4)
_cell_length_c                   22.5225(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 98.8810(10)
_cell_angle_gamma                90.00
_cell_volume                     9533.3(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    15953
_cell_measurement_theta_min      1.25
_cell_measurement_theta_max      24.63

_exptl_crystal_description       rhombohedrons
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.485
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             6760
_exptl_absorpt_coefficient_mu    5.252
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.4033
_exptl_absorpt_correction_T_max  0.5230
_exptl_absorpt_process_details   'X-Shape (STOE & CIE, 1998)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Stoe Imaging Plate Diffraction System'
_diffrn_measurement_method       '\f scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        none
_diffrn_reflns_number            63078
_diffrn_reflns_av_R_equivalents  0.0342
_diffrn_reflns_av_sigmaI/netI    0.0272
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.25
_diffrn_reflns_theta_max         24.63
_reflns_number_total             15953
_reflns_number_gt                13509
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'STOE-IPDS Program Package'
_computing_cell_refinement       'STOE-IPDS Program Package'
_computing_data_reduction        'STOE-IPDS Program Package'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0406P)^2^+18.6590P] where P=(Fo^2^+2Fc^2^)/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         15953
_refine_ls_number_parameters     894
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0469
_refine_ls_R_factor_gt           0.0357
_refine_ls_wR_factor_ref         0.0800
_refine_ls_wR_factor_gt          0.0763
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_restrained_S_all      1.050
_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
Sb1 Sb 0.47267(3) 0.423077(17) 0.23697(2) 0.04006(10) Uani 1 1 d . . .
Sb2 Sb 0.32329(3) 0.690885(17) -0.00416(2) 0.03978(10) Uani 1 1 d . . .
Sb3 Sb 0.10940(2) 0.715485(17) 0.033677(19) 0.03772(10) Uani 1 1 d . . .
Sb4 Sb 0.09377(3) 0.548306(18) 0.23336(2) 0.04285(11) Uani 1 1 d . . .
Sb5 Sb 0.20275(3) 0.609248(17) 0.12176(2) 0.04052(10) Uani 1 1 d . . .
Sb6 Sb 0.69036(3) 0.468780(18) 0.25557(2) 0.04193(11) Uani 1 1 d . . .
Sb7 Sb 0.26813(2) 0.468311(16) 0.264584(19) 0.03770(10) Uani 1 1 d . . .
Sb8 Sb -0.13347(3) 0.953229(18) -0.26312(2) 0.04469(11) Uani 1 1 d . . .
Sb9 Sb -0.04435(3) 0.822311(18) 0.00749(2) 0.04400(11) Uani 1 1 d . . .
Sb10 Sb 0.52536(3) 0.725379(17) -0.01111(2) 0.04134(11) Uani 1 1 d . . .
Sb11 Sb 0.71870(3) 0.806346(19) 0.02147(2) 0.04739(12) Uani 1 1 d . . .
Sb12 Sb 0.60593(3) 0.381998(18) 0.12995(2) 0.04335(11) Uani 1 1 d . . .
Sb13 Sb 0.38620(3) 0.376169(17) 0.37044(2) 0.04062(10) Uani 1 1 d . . .
Sb14 Sb -0.11720(3) 0.885548(19) -0.13035(2) 0.04762(12) Uani 1 1 d . . .
Ni1 Ni 0.23572(5) 0.95789(3) 0.01050(4) 0.03839(19) Uani 1 1 d . . .
Ni2 Ni 0.07828(5) 0.70233(3) -0.23113(4) 0.03501(17) Uani 1 1 d . . .
Ni3 Ni 0.56785(5) 0.81434(3) -0.24817(4) 0.03861(18) Uani 1 1 d . E .
Ni4 Ni 0.25104(5) 0.43451(3) -0.02451(4) 0.04038(19) Uani 1 1 d . F .
S1 S 0.07827(11) 0.62367(7) 0.16746(8) 0.0484(4) Uani 1 1 d . . .
S2 S 0.15050(12) 0.60178(7) 0.01893(8) 0.0517(4) Uani 1 1 d . . .
S3 S 0.41454(10) 0.76100(7) 0.03877(8) 0.0473(4) Uani 1 1 d . . .
S4 S 0.64146(11) 0.74095(7) 0.07269(9) 0.0507(4) Uani 1 1 d . . .
S5 S 0.23458(10) 0.55984(7) 0.28949(8) 0.0431(4) Uani 1 1 d . . .
S6 S 0.49830(11) 0.63822(7) 0.01267(9) 0.0499(4) Uani 1 1 d . . .
S7 S 0.66549(11) 0.37052(7) 0.23572(8) 0.0480(4) Uani 1 1 d . . .
S8 S 0.56965(10) 0.48941(7) 0.18541(9) 0.0500(4) Uani 1 1 d . . .
S9 S 0.38730(10) 0.46956(6) 0.35710(8) 0.0412(4) Uani 1 1 d . . .
S10 S 0.08854(10) 0.80614(7) 0.07064(8) 0.0458(4) Uani 1 1 d . . .
S11 S 0.35255(11) 0.35946(7) 0.26338(8) 0.0478(4) Uani 1 1 d . . .
S12 S 0.14009(11) 0.48923(7) 0.16573(9) 0.0523(4) Uani 1 1 d . . .
S13 S 0.01219(11) 0.88330(8) -0.06105(9) 0.0550(5) Uani 1 1 d . . .
S14 S 0.19805(10) 0.74521(7) -0.03630(7) 0.0415(4) Uani 1 1 d . . .
S15 S 0.22572(10) 0.70519(7) 0.11674(8) 0.0452(4) Uani 1 1 d . . .
S16 S -0.09976(13) 0.97795(7) -0.15660(9) 0.0567(5) Uani 1 1 d . . .
S17 S 0.80515(11) 0.45768(7) 0.20237(9) 0.0502(4) Uani 1 1 d . . .
S18 S 0.72928(11) 0.57251(7) 0.23941(11) 0.0571(5) Uani 1 1 d . . .
S19 S -0.08195(13) 0.85321(8) -0.22055(9) 0.0593(5) Uani 1 1 d . . .
S20 S 0.46661(10) 0.36485(8) 0.14998(8) 0.0498(4) Uani 1 1 d . . .
S21 S 0.35723(11) 0.70744(7) -0.10664(8) 0.0471(4) Uani 1 1 d . . .
S22 S 0.75392(10) 0.86276(8) 0.11011(9) 0.0523(4) Uani 1 1 d . . .
S23 S -0.05770(14) 0.75053(8) -0.05457(10) 0.0634(5) Uani 1 1 d . . .
S24 S 0.36525(10) 0.48522(7) 0.19568(8) 0.0456(4) Uani 1 1 d . . .
S25 S 0.61156(15) 0.85346(10) -0.03199(11) 0.0732(6) Uani 1 1 d . . .
N11 N 0.3568(3) 0.9317(2) 0.0216(3) 0.0431(13) Uani 1 1 d . . .
N12 N 0.2906(4) 1.0211(2) 0.0658(3) 0.0532(15) Uani 1 1 d . . .
H12A H 0.2809 1.0512 0.0459 0.064 Uiso 1 1 calc R . .
H12B H 0.2687 1.0229 0.0999 0.064 Uiso 1 1 calc R . .
N13 N 0.2189(3) 0.8922(2) -0.0501(3) 0.0487(14) Uani 1 1 d . . .
H13A H 0.1867 0.8686 -0.0360 0.058 Uiso 1 1 calc R . .
H13B H 0.1940 0.9025 -0.0865 0.058 Uiso 1 1 calc R . .
N14 N 0.2290(4) 0.9094(2) 0.0847(3) 0.0544(15) Uani 1 1 d . . .
H14A H 0.2350 0.9282 0.1187 0.065 Uiso 1 1 calc R . .
H14B H 0.1798 0.8938 0.0804 0.065 Uiso 1 1 calc R . .
N15 N 0.2297(3) 1.0043(2) -0.0682(3) 0.0503(14) Uani 1 1 d . . .
H15A H 0.2568 1.0342 -0.0595 0.060 Uiso 1 1 calc R . .
H15B H 0.2525 0.9876 -0.0965 0.060 Uiso 1 1 calc R . .
N16 N 0.1149(3) 0.9852(2) 0.0057(3) 0.0506(15) Uani 1 1 d . . .
H16A H 0.0795 0.9593 -0.0054 0.061 Uiso 1 1 calc R . .
H16B H 0.1068 0.9965 0.0421 0.061 Uiso 1 1 calc R . .
N21 N -0.0292(3) 0.6608(2) -0.2274(2) 0.0412(12) Uani 1 1 d . . .
N22 N -0.0005(3) 0.7435(2) -0.3009(3) 0.0483(14) Uani 1 1 d . . .
H22A H -0.0004 0.7774 -0.2919 0.058 Uiso 1 1 calc R . .
H22B H 0.0183 0.7398 -0.3361 0.058 Uiso 1 1 calc R . .
N23 N 0.1240(4) 0.6562(2) -0.1542(3) 0.0470(13) Uani 1 1 d . . .
H23A H 0.1645 0.6355 -0.1627 0.056 Uiso 1 1 calc R . .
H23B H 0.1445 0.6767 -0.1232 0.056 Uiso 1 1 calc R . .
N24 N 0.0990(3) 0.6419(2) -0.2903(3) 0.0471(13) Uani 1 1 d . . .
H24A H 0.1222 0.6547 -0.3208 0.057 Uiso 1 1 calc R . .
H24B H 0.1334 0.6185 -0.2706 0.057 Uiso 1 1 calc R . .
N25 N 0.0658(3) 0.7654(2) -0.1722(3) 0.0415(12) Uani 1 1 d . . .
H25A H 0.0138 0.7768 -0.1779 0.050 Uiso 1 1 calc R . .
H25B H 0.0788 0.7552 -0.1337 0.050 Uiso 1 1 calc R . .
N26 N 0.1863(3) 0.7412(2) -0.2405(3) 0.0478(14) Uani 1 1 d . . .
H26A H 0.2287 0.7192 -0.2339 0.057 Uiso 1 1 calc R . .
H26B H 0.1829 0.7533 -0.2783 0.057 Uiso 1 1 calc R . .
N31 N 0.4446(3) 0.8226(2) -0.2433(3) 0.0463(13) Uani 1 1 d . E .
N32 N 0.5411(5) 0.8622(3) -0.3239(3) 0.067(2) Uani 1 1 d . . .
H32A H 0.5808 0.8860 -0.3233 0.080 Uiso 0.70 1 calc PR A 1
H32B H 0.5400 0.8431 -0.3574 0.080 Uiso 0.70 1 calc PR A 1
H32C H 0.5554 0.8951 -0.3149 0.080 Uiso 0.30 1 calc PR A 2
H32D H 0.5668 0.8513 -0.3540 0.080 Uiso 0.30 1 calc PR A 2
N33 N 0.5760(3) 0.8808(2) -0.1883(3) 0.0473(14) Uani 1 1 d . . .
H33A H 0.6073 0.8730 -0.1531 0.057 Uiso 1 1 calc R E .
H33B H 0.5994 0.9075 -0.2048 0.057 Uiso 1 1 calc R . .
N34 N 0.5252(4) 0.7474(2) -0.2981(3) 0.0526(15) Uani 1 1 d . . .
H34A H 0.5327 0.7513 -0.3366 0.063 Uiso 1 1 calc R E .
H34B H 0.5541 0.7197 -0.2829 0.063 Uiso 1 1 calc R . .
N35 N 0.6902(4) 0.8027(3) -0.2578(5) 0.088(3) Uani 1 1 d . . .
H35A H 0.6923 0.7901 -0.2948 0.106 Uiso 1 1 calc R E .
H35B H 0.7163 0.8333 -0.2547 0.106 Uiso 1 1 calc R . .
N36 N 0.6059(5) 0.7690(3) -0.1685(4) 0.080(2) Uani 1 1 d . . .
H36A H 0.5847 0.7815 -0.1369 0.096 Uiso 1 1 calc R E .
H36B H 0.5914 0.7357 -0.1743 0.096 Uiso 1 1 calc R . .
N41 N 0.1456(4) 0.3991(2) -0.0032(3) 0.0515(15) Uani 1 1 d . . .
N42 N 0.1639(4) 0.4887(3) -0.0677(3) 0.0641(18) Uani 1 1 d . . .
H42A H 0.1738 0.5200 -0.0509 0.077 Uiso 1 1 calc R . .
H42B H 0.1688 0.4911 -0.1068 0.077 Uiso 1 1 calc R . .
N43 N 0.3095(4) 0.3788(3) 0.0356(3) 0.0699(19) Uani 1 1 d . . .
H43A H 0.3389 0.3573 0.0158 0.084 Uiso 1 1 calc R . .
H43B H 0.3441 0.3946 0.0647 0.084 Uiso 1 1 calc R . .
N44 N 0.2377(5) 0.3793(3) -0.0947(3) 0.0647(18) Uani 1 1 d . . .
H44A H 0.2489 0.3939 -0.1288 0.078 Uiso 1 1 calc R . .
H44B H 0.2728 0.3530 -0.0850 0.078 Uiso 1 1 calc R . .
N45 N 0.3574(5) 0.4654(3) -0.0502(4) 0.077(2) Uani 1 1 d D . .
H45A H 0.3911 0.4399 -0.0584 0.092 Uiso 0.50 1 calc PR B 1
H45B H 0.3448 0.4851 -0.0833 0.092 Uiso 0.50 1 calc PR B 1
H45C H 0.4008 0.4453 -0.0369 0.092 Uiso 0.50 1 calc PR B 2
H45D H 0.3522 0.4675 -0.0905 0.092 Uiso 0.50 1 calc PR B 2
N46 N 0.2771(4) 0.4905(3) 0.0458(3) 0.0560(16) Uani 1 1 d D . .
H46A H 0.2306 0.5072 0.0502 0.067 Uiso 0.50 1 calc PR C 1
H46B H 0.2954 0.4742 0.0806 0.067 Uiso 0.50 1 calc PR C 1
H46C H 0.2433 0.5179 0.0391 0.067 Uiso 0.50 1 calc PR C 2
H46D H 0.2726 0.4767 0.0818 0.067 Uiso 0.50 1 calc PR C 2
C11 C 0.4083(4) 0.9785(3) 0.0333(4) 0.0514(18) Uani 1 1 d . . .
H11A H 0.4067 0.9979 -0.0037 0.062 Uiso 1 1 calc R . .
H11B H 0.4646 0.9684 0.0469 0.062 Uiso 1 1 calc R . .
C12 C 0.3792(5) 1.0124(3) 0.0802(4) 0.060(2) Uani 1 1 d . . .
H12C H 0.3918 0.9960 0.1193 0.072 Uiso 1 1 calc R . .
H12D H 0.4076 1.0453 0.0821 0.072 Uiso 1 1 calc R . .
C13 C 0.3680(4) 0.9063(3) -0.0350(3) 0.0496(17) Uani 1 1 d . . .
H13C H 0.4198 0.8880 -0.0294 0.060 Uiso 1 1 calc R . .
H13D H 0.3697 0.9323 -0.0658 0.060 Uiso 1 1 calc R . .
C14 C 0.2992(4) 0.8686(3) -0.0556(3) 0.0509(17) Uani 1 1 d . . .
H14C H 0.3002 0.8590 -0.0971 0.061 Uiso 1 1 calc R . .
H14D H 0.3068 0.8375 -0.0313 0.061 Uiso 1 1 calc R . .
C15 C 0.3715(4) 0.8955(3) 0.0741(3) 0.0508(17) Uani 1 1 d . . .
H15C H 0.3974 0.9144 0.1091 0.061 Uiso 1 1 calc R . .
H15D H 0.4091 0.8687 0.0656 0.061 Uiso 1 1 calc R . .
C16 C 0.2939(5) 0.8705(3) 0.0884(4) 0.0569(19) Uani 1 1 d . . .
H16C H 0.2773 0.8428 0.0601 0.068 Uiso 1 1 calc R . .
H16D H 0.3038 0.8558 0.1285 0.068 Uiso 1 1 calc R . .
C17 C 0.1422(4) 1.0147(3) -0.0902(4) 0.0577(19) Uani 1 1 d . . .
H17A H 0.1170 0.9845 -0.1109 0.069 Uiso 1 1 calc R . .
H17B H 0.1371 1.0433 -0.1183 0.069 Uiso 1 1 calc R . .
C18 C 0.1005(5) 1.0275(3) -0.0381(4) 0.063(2) Uani 1 1 d . . .
H18A H 0.1220 1.0595 -0.0197 0.076 Uiso 1 1 calc R . .
H18B H 0.0422 1.0317 -0.0513 0.076 Uiso 1 1 calc R . .
C21 C -0.0973(4) 0.6965(3) -0.2479(4) 0.0573(19) Uani 1 1 d . . .
H21A H -0.1007 0.7223 -0.2172 0.069 Uiso 1 1 calc R . .
H21B H -0.1484 0.6775 -0.2544 0.069 Uiso 1 1 calc R . .
C22 C -0.0844(4) 0.7231(3) -0.3063(4) 0.0566(19) Uani 1 1 d . . .
H22C H -0.0937 0.6985 -0.3392 0.068 Uiso 1 1 calc R . .
H22D H -0.1233 0.7511 -0.3151 0.068 Uiso 1 1 calc R . .
C23 C -0.0258(5) 0.6464(3) -0.1632(3) 0.0491(17) Uani 1 1 d . . .
H23C H -0.0677 0.6209 -0.1596 0.059 Uiso 1 1 calc R . .
H23D H -0.0368 0.6766 -0.1404 0.059 Uiso 1 1 calc R . .
C24 C 0.0568(5) 0.6247(3) -0.1378(3) 0.0571(19) Uani 1 1 d . . .
H24C H 0.0617 0.6231 -0.0943 0.069 Uiso 1 1 calc R . .
H24D H 0.0613 0.5898 -0.1525 0.069 Uiso 1 1 calc R . .
C25 C -0.0329(5) 0.6133(3) -0.2649(3) 0.0518(17) Uani 1 1 d . . .
H25C H -0.0891 0.6073 -0.2832 0.062 Uiso 1 1 calc R . .
H25D H -0.0153 0.5840 -0.2393 0.062 Uiso 1 1 calc R . .
C26 C 0.0206(5) 0.6171(3) -0.3140(3) 0.0559(19) Uani 1 1 d . . .
H26C H 0.0305 0.5828 -0.3286 0.067 Uiso 1 1 calc R . .
H26D H -0.0074 0.6371 -0.3474 0.067 Uiso 1 1 calc R . .
C27 C 0.2002(4) 0.7844(3) -0.1978(3) 0.0501(17) Uani 1 1 d . . .
H27A H 0.2310 0.8113 -0.2144 0.060 Uiso 1 1 calc R . .
H27B H 0.2322 0.7725 -0.1606 0.060 Uiso 1 1 calc R . .
C28 C 0.1205(4) 0.8061(3) -0.1852(4) 0.0481(17) Uani 1 1 d . . .
H28A H 0.1308 0.8294 -0.1511 0.058 Uiso 1 1 calc R . .
H28B H 0.0948 0.8257 -0.2197 0.058 Uiso 1 1 calc R . .
C31 C 0.4058(5) 0.8536(3) -0.2958(5) 0.075(3) Uani 1 1 d . . .
H31A H 0.3659 0.8768 -0.2829 0.090 Uiso 0.70 1 calc PR D 1
H31B H 0.3768 0.8305 -0.3257 0.090 Uiso 0.70 1 calc PR D 1
H31C H 0.3507 0.8404 -0.3073 0.090 Uiso 0.30 1 calc PR D 2
H31D H 0.4006 0.8887 -0.2818 0.090 Uiso 0.30 1 calc PR D 2
C32A C 0.4691(9) 0.8860(6) -0.3255(6) 0.076(4) Uani 0.70 1 d P E 1
H32E H 0.4463 0.8931 -0.3670 0.092 Uiso 0.70 1 calc PR E 1
H32F H 0.4779 0.9188 -0.3047 0.092 Uiso 0.70 1 calc PR E 1
C32B C 0.4376(16) 0.8562(12) -0.3424(13) 0.054(6) Uiso 0.30 1 d P E 2
H32G H 0.4157 0.8856 -0.3662 0.065 Uiso 0.30 1 calc PR E 2
H32H H 0.4247 0.8252 -0.3663 0.065 Uiso 0.30 1 calc PR E 2
C33 C 0.4385(5) 0.8487(3) -0.1858(4) 0.064(2) Uani 1 1 d . . .
H33C H 0.4543 0.8249 -0.1528 0.077 Uiso 1 1 calc R E .
H33D H 0.3822 0.8590 -0.1852 0.077 Uiso 1 1 calc R . .
C34 C 0.4929(5) 0.8955(3) -0.1778(4) 0.061(2) Uani 1 1 d . E .
H34C H 0.4711 0.9221 -0.2060 0.073 Uiso 1 1 calc R . .
H34D H 0.4952 0.9090 -0.1374 0.073 Uiso 1 1 calc R . .
C35 C 0.4116(5) 0.7695(3) -0.2449(4) 0.063(2) Uani 1 1 d . . .
H35C H 0.3524 0.7707 -0.2501 0.076 Uiso 1 1 calc R E .
H35D H 0.4309 0.7524 -0.2071 0.076 Uiso 1 1 calc R . .
C36 C 0.4381(5) 0.7391(3) -0.2956(4) 0.0585(19) Uani 1 1 d . E .
H36C H 0.4283 0.7026 -0.2899 0.070 Uiso 1 1 calc R . .
H36D H 0.4060 0.7496 -0.3334 0.070 Uiso 1 1 calc R . .
C37 C 0.7313(7) 0.7685(4) -0.2148(8) 0.123(6) Uani 1 1 d . E .
H37A H 0.7896 0.7753 -0.2091 0.148 Uiso 1 1 calc R . .
H37B H 0.7223 0.7331 -0.2286 0.148 Uiso 1 1 calc R . .
C38 C 0.7005(7) 0.7755(5) -0.1593(6) 0.106(4) Uani 1 1 d . E .
H38A H 0.7150 0.8098 -0.1437 0.127 Uiso 1 1 calc R . .
H38B H 0.7256 0.7505 -0.1302 0.127 Uiso 1 1 calc R . .
C41 C 0.0842(5) 0.4404(4) -0.0053(5) 0.081(3) Uani 1 1 d . . .
H41A H 0.0976 0.4625 0.0296 0.098 Uiso 1 1 calc R . .
H41B H 0.0308 0.4253 -0.0040 0.098 Uiso 1 1 calc R . .
C42 C 0.0808(6) 0.4727(4) -0.0621(5) 0.089(3) Uani 1 1 d . . .
H42C H 0.0577 0.4525 -0.0969 0.106 Uiso 1 1 calc R . .
H42D H 0.0465 0.5028 -0.0598 0.106 Uiso 1 1 calc R . .
C43 C 0.1702(6) 0.3780(4) 0.0580(4) 0.072(3) Uani 1 1 d . . .
H43C H 0.1278 0.3551 0.0677 0.086 Uiso 1 1 calc R . .
H43D H 0.1762 0.4061 0.0868 0.086 Uiso 1 1 calc R . .
C44 C 0.2493(6) 0.3490(3) 0.0625(4) 0.074(3) Uani 1 1 d . . .
H44C H 0.2703 0.3423 0.1045 0.089 Uiso 1 1 calc R . .
H44D H 0.2400 0.3161 0.0421 0.089 Uiso 1 1 calc R . .
C45 C 0.1193(6) 0.3559(4) -0.0467(4) 0.076(3) Uani 1 1 d . . .
H45E H 0.1358 0.3232 -0.0276 0.091 Uiso 1 1 calc R . .
H45F H 0.0601 0.3559 -0.0564 0.091 Uiso 1 1 calc R . .
C46 C 0.1550(7) 0.3606(4) -0.1034(4) 0.087(3) Uani 1 1 d . . .
H46E H 0.1535 0.3269 -0.1225 0.105 Uiso 1 1 calc R . .
H46F H 0.1211 0.3837 -0.1305 0.105 Uiso 1 1 calc R . .
C47A C 0.3982(11) 0.4977(8) 0.0020(9) 0.083(6) Uiso 0.50 1 d PD F 1
H47A H 0.4365 0.5212 -0.0125 0.100 Uiso 0.50 1 calc PR F 1
H47B H 0.4294 0.4750 0.0313 0.100 Uiso 0.50 1 calc PR F 1
C48A C 0.3395(10) 0.5289(6) 0.0331(8) 0.060(4) Uiso 0.50 1 d PD F 1
H48A H 0.3674 0.5440 0.0701 0.073 Uiso 0.50 1 calc PR F 1
H48B H 0.3143 0.5563 0.0072 0.073 Uiso 0.50 1 calc PR F 1
C47B C 0.3684(13) 0.5166(6) -0.0236(8) 0.075(5) Uiso 0.50 1 d PD F 2
H47C H 0.3247 0.5397 -0.0405 0.090 Uiso 0.50 1 calc PR F 2
H47D H 0.4206 0.5313 -0.0292 0.090 Uiso 0.50 1 calc PR F 2
C48B C 0.3653(9) 0.5057(8) 0.0423(7) 0.067(5) Uiso 0.50 1 d PD F 2
H48C H 0.3806 0.5363 0.0664 0.081 Uiso 0.50 1 calc PR F 2
H48D H 0.4024 0.4779 0.0568 0.081 Uiso 0.50 1 calc PR F 2

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Sb1 0.0391(2) 0.0442(3) 0.0364(2) -0.00415(19) 0.00411(17) 0.00436(18)
Sb2 0.0413(2) 0.0395(2) 0.0382(2) -0.00002(19) 0.00533(18) 0.00280(18)
Sb3 0.0364(2) 0.0391(2) 0.0375(2) -0.00089(18) 0.00516(17) -0.00065(17)
Sb4 0.0362(2) 0.0493(3) 0.0434(3) 0.0061(2) 0.00729(19) 0.00161(18)
Sb5 0.0394(2) 0.0421(2) 0.0382(2) 0.00029(19) 0.00018(18) 0.00220(18)
Sb6 0.0424(2) 0.0488(3) 0.0352(2) -0.00146(19) 0.00800(18) -0.00023(19)
Sb7 0.0372(2) 0.0382(2) 0.0382(2) 0.00050(18) 0.00737(17) 0.00017(17)
Sb8 0.0412(2) 0.0486(3) 0.0451(3) -0.0026(2) 0.00930(19) 0.00224(19)
Sb9 0.0415(2) 0.0434(3) 0.0480(3) -0.0027(2) 0.00971(19) 0.00341(19)
Sb10 0.0412(2) 0.0425(2) 0.0414(3) 0.00022(19) 0.00988(18) 0.00025(18)
Sb11 0.0472(3) 0.0478(3) 0.0498(3) -0.0065(2) 0.0160(2) -0.0036(2)
Sb12 0.0429(2) 0.0440(3) 0.0447(3) -0.0036(2) 0.01188(19) 0.00046(19)
Sb13 0.0358(2) 0.0426(2) 0.0432(3) 0.00460(19) 0.00519(18) 0.00391(18)
Sb14 0.0425(2) 0.0460(3) 0.0535(3) -0.0012(2) 0.0046(2) 0.00045(19)
Ni1 0.0387(4) 0.0396(5) 0.0380(5) -0.0039(4) 0.0096(3) -0.0062(3)
Ni2 0.0370(4) 0.0348(4) 0.0334(4) 0.0009(3) 0.0060(3) 0.0018(3)
Ni3 0.0344(4) 0.0382(4) 0.0433(5) -0.0024(4) 0.0063(3) -0.0006(3)
Ni4 0.0415(4) 0.0429(5) 0.0381(5) 0.0048(4) 0.0104(4) 0.0047(4)
S1 0.0477(9) 0.0495(10) 0.0483(10) 0.0059(8) 0.0082(8) 0.0119(8)
S2 0.0644(11) 0.0500(11) 0.0380(10) -0.0047(8) -0.0009(8) -0.0015(8)
S3 0.0434(9) 0.0468(10) 0.0511(11) -0.0126(8) 0.0057(8) 0.0046(7)
S4 0.0466(9) 0.0514(11) 0.0517(11) 0.0086(8) 0.0006(8) -0.0044(8)
S5 0.0432(9) 0.0424(9) 0.0422(9) -0.0047(7) 0.0017(7) 0.0040(7)
S6 0.0505(10) 0.0393(9) 0.0614(12) 0.0037(8) 0.0135(8) 0.0034(7)
S7 0.0550(10) 0.0412(9) 0.0456(10) 0.0008(8) 0.0011(8) -0.0042(8)
S8 0.0400(9) 0.0503(10) 0.0580(11) 0.0078(9) 0.0025(8) 0.0015(7)
S9 0.0421(8) 0.0408(9) 0.0403(9) -0.0036(7) 0.0049(7) -0.0010(7)
S10 0.0474(9) 0.0464(10) 0.0421(9) -0.0085(8) 0.0022(7) 0.0050(7)
S11 0.0577(10) 0.0416(10) 0.0451(10) -0.0067(8) 0.0108(8) -0.0031(8)
S12 0.0542(10) 0.0492(11) 0.0506(11) -0.0103(8) -0.0004(8) 0.0009(8)
S13 0.0493(10) 0.0531(11) 0.0588(12) 0.0082(9) -0.0040(8) -0.0127(8)
S14 0.0403(8) 0.0488(10) 0.0362(9) 0.0055(7) 0.0086(7) 0.0070(7)
S15 0.0492(9) 0.0419(9) 0.0407(9) 0.0007(7) -0.0049(7) -0.0041(7)
S16 0.0776(13) 0.0445(10) 0.0464(11) -0.0048(8) 0.0046(9) 0.0025(9)
S17 0.0508(10) 0.0405(10) 0.0639(12) -0.0047(8) 0.0236(9) 0.0028(7)
S18 0.0441(9) 0.0385(10) 0.0902(15) -0.0017(10) 0.0152(9) 0.0026(7)
S19 0.0680(12) 0.0529(11) 0.0541(12) -0.0078(9) -0.0001(9) 0.0200(9)
S20 0.0404(9) 0.0614(11) 0.0488(10) -0.0193(9) 0.0109(7) -0.0053(8)
S21 0.0559(10) 0.0494(10) 0.0371(9) 0.0013(8) 0.0108(8) 0.0127(8)
S22 0.0375(9) 0.0572(11) 0.0612(12) -0.0160(9) 0.0048(8) -0.0019(8)
S23 0.0771(13) 0.0524(12) 0.0611(13) -0.0127(10) 0.0115(10) -0.0181(10)
S24 0.0430(9) 0.0535(10) 0.0425(9) 0.0103(8) 0.0130(7) 0.0102(7)
S25 0.0858(15) 0.0715(15) 0.0581(13) 0.0177(11) -0.0022(11) 0.0046(12)
N11 0.043(3) 0.041(3) 0.044(3) 0.001(3) 0.005(2) -0.005(2)
N12 0.060(4) 0.047(4) 0.052(4) -0.008(3) 0.008(3) -0.005(3)
N13 0.045(3) 0.051(4) 0.049(4) -0.008(3) 0.004(3) -0.002(3)
N14 0.064(4) 0.055(4) 0.046(4) -0.003(3) 0.015(3) -0.018(3)
N15 0.047(3) 0.052(4) 0.055(4) 0.008(3) 0.019(3) 0.005(3)
N16 0.045(3) 0.056(4) 0.054(4) -0.013(3) 0.019(3) -0.004(3)
N21 0.044(3) 0.039(3) 0.041(3) -0.006(2) 0.007(2) 0.001(2)
N22 0.056(3) 0.044(3) 0.042(3) 0.003(3) 0.000(3) 0.002(3)
N23 0.057(3) 0.036(3) 0.046(3) -0.001(3) 0.004(3) 0.007(3)
N24 0.056(3) 0.049(3) 0.037(3) 0.004(3) 0.010(3) 0.005(3)
N25 0.041(3) 0.042(3) 0.043(3) 0.002(2) 0.008(2) 0.005(2)
N26 0.050(3) 0.049(3) 0.047(3) 0.002(3) 0.013(3) 0.001(3)
N31 0.039(3) 0.046(3) 0.053(4) -0.003(3) 0.007(3) -0.001(2)
N32 0.095(6) 0.062(4) 0.045(4) 0.002(3) 0.013(4) -0.031(4)
N33 0.045(3) 0.052(4) 0.045(3) -0.005(3) 0.008(3) -0.007(3)
N34 0.054(3) 0.048(4) 0.057(4) -0.007(3) 0.015(3) -0.002(3)
N35 0.055(4) 0.057(5) 0.156(9) -0.038(5) 0.028(5) -0.004(4)
N36 0.102(6) 0.052(4) 0.075(5) 0.011(4) -0.021(4) -0.002(4)
N41 0.050(3) 0.055(4) 0.051(4) -0.018(3) 0.012(3) -0.013(3)
N42 0.079(5) 0.064(4) 0.046(4) -0.007(3) -0.003(3) 0.025(4)
N43 0.071(4) 0.075(5) 0.063(5) 0.019(4) 0.011(4) 0.020(4)
N44 0.092(5) 0.054(4) 0.051(4) 0.006(3) 0.021(4) 0.022(4)
N45 0.074(5) 0.076(5) 0.090(6) 0.011(4) 0.043(4) 0.002(4)
N46 0.051(3) 0.068(4) 0.046(4) 0.006(3) 0.001(3) -0.009(3)
C11 0.043(4) 0.051(4) 0.058(5) 0.006(4) 0.000(3) -0.011(3)
C12 0.065(5) 0.050(5) 0.060(5) -0.006(4) -0.006(4) -0.019(4)
C13 0.047(4) 0.055(4) 0.048(4) -0.003(3) 0.010(3) 0.008(3)
C14 0.055(4) 0.053(4) 0.044(4) -0.015(3) 0.006(3) 0.007(3)
C15 0.057(4) 0.045(4) 0.047(4) 0.007(3) -0.002(3) -0.009(3)
C16 0.071(5) 0.053(5) 0.047(4) 0.012(4) 0.008(4) -0.008(4)
C17 0.044(4) 0.066(5) 0.062(5) 0.010(4) 0.002(3) 0.004(3)
C18 0.052(4) 0.056(5) 0.083(6) -0.007(4) 0.018(4) 0.007(4)
C21 0.045(4) 0.055(5) 0.073(5) 0.001(4) 0.013(4) -0.006(3)
C22 0.047(4) 0.054(5) 0.062(5) 0.007(4) -0.010(3) 0.005(3)
C23 0.066(4) 0.045(4) 0.040(4) -0.006(3) 0.020(3) -0.007(3)
C24 0.082(5) 0.052(5) 0.037(4) 0.006(3) 0.008(4) 0.001(4)
C25 0.064(5) 0.043(4) 0.048(4) -0.004(3) 0.009(3) -0.006(3)
C26 0.074(5) 0.049(4) 0.045(4) -0.001(3) 0.011(4) -0.001(4)
C27 0.045(4) 0.051(4) 0.053(4) -0.002(3) 0.006(3) -0.005(3)
C28 0.049(4) 0.040(4) 0.057(5) 0.002(3) 0.013(3) -0.010(3)
C31 0.063(5) 0.059(5) 0.089(7) -0.010(5) -0.031(5) 0.009(4)
C32A 0.092(10) 0.069(9) 0.063(8) 0.020(7) -0.002(7) 0.004(8)
C33 0.048(4) 0.080(6) 0.068(5) -0.024(5) 0.021(4) -0.009(4)
C34 0.059(5) 0.062(5) 0.061(5) -0.024(4) 0.007(4) 0.003(4)
C35 0.055(4) 0.065(5) 0.073(6) -0.010(4) 0.025(4) -0.021(4)
C36 0.066(5) 0.054(5) 0.056(5) -0.002(4) 0.010(4) -0.014(4)
C37 0.059(6) 0.056(6) 0.246(19) -0.025(9) -0.005(9) 0.000(5)
C38 0.085(7) 0.102(9) 0.109(9) -0.025(7) -0.052(7) 0.051(6)
C41 0.040(4) 0.097(7) 0.111(8) -0.037(6) 0.023(5) -0.005(4)
C42 0.061(6) 0.092(7) 0.101(8) -0.029(6) -0.025(5) 0.027(5)
C43 0.089(6) 0.081(6) 0.053(5) -0.013(4) 0.032(5) -0.041(5)
C44 0.106(7) 0.058(5) 0.052(5) 0.014(4) -0.003(5) -0.015(5)
C45 0.081(6) 0.075(6) 0.070(6) -0.018(5) 0.005(5) -0.030(5)
C46 0.122(9) 0.077(7) 0.063(6) -0.029(5) 0.015(6) -0.014(6)

_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
Sb1 S20 2.4621(18) . ?
Sb1 S24 2.4704(17) . ?
Sb1 S11 2.7170(18) . ?
Sb1 S8 2.7293(18) . ?
Sb2 S3 2.4618(18) . ?
Sb2 S21 2.4953(17) . ?
Sb2 S14 2.5165(16) . ?
Sb3 S14 2.4374(16) . ?
Sb3 S15 2.4824(17) . ?
Sb3 S10 2.5323(17) . ?
Sb4 S12 2.3682(19) . ?
Sb4 S1 2.4415(18) . ?
Sb4 S5 2.4908(17) . ?
Sb5 S2 2.3517(19) . ?
Sb5 S1 2.4686(17) . ?
Sb5 S15 2.5187(18) . ?
Sb6 S8 2.4075(18) . ?
Sb6 S17 2.4138(17) . ?
Sb6 S7 2.6052(18) . ?
Sb6 S18 2.7992(19) . ?
Sb7 S24 2.4394(16) . ?
Sb7 S5 2.5175(17) . ?
Sb7 S9 2.6382(17) . ?
Sb7 S12 2.878(2) . ?
Sb8 S18 2.3753(18) 4_475 ?
Sb8 S16 2.462(2) . ?
Sb8 S17 2.5912(19) 4_475 ?
Sb8 S19 2.847(2) . ?
Sb9 S23 2.316(2) . ?
Sb9 S10 2.4628(18) . ?
Sb9 S13 2.4897(19) . ?
Sb10 S6 2.3781(18) . ?
Sb10 S3 2.4719(17) . ?
Sb10 S4 2.5087(19) . ?
Sb11 S25 2.328(2) . ?
Sb11 S22 2.4697(19) . ?
Sb11 S4 2.5073(18) . ?
Sb12 S7 2.4514(19) . ?
Sb12 S20 2.4563(17) . ?
Sb12 S21 2.4719(18) 3_665 ?
Sb13 S11 2.4285(19) . ?
Sb13 S9 2.4375(17) . ?
Sb13 S22 2.4493(17) 2_645 ?
Sb14 S19 2.353(2) . ?
Sb14 S13 2.4473(19) . ?
Sb14 S16 2.492(2) . ?
Ni1 N11 2.093(6) . ?
Ni1 N16 2.106(6) . ?
Ni1 N14 2.107(6) . ?
Ni1 N15 2.131(6) . ?
Ni1 N12 2.170(6) . ?
Ni1 N13 2.172(6) . ?
Ni2 N26 2.090(5) . ?
Ni2 N21 2.091(5) . ?
Ni2 N24 2.117(6) . ?
Ni2 N25 2.135(5) . ?
Ni2 N23 2.145(6) . ?
Ni2 N22 2.161(6) . ?
Ni3 N31 2.071(5) . ?
Ni3 N35 2.091(7) . ?
Ni3 N32 2.100(7) . ?
Ni3 N34 2.127(6) . ?
Ni3 N36 2.155(7) . ?
Ni3 N33 2.179(6) . ?
Ni4 N41 2.091(6) . ?
Ni4 N45 2.095(6) . ?
Ni4 N43 2.109(7) . ?
Ni4 N44 2.118(7) . ?
Ni4 N42 2.135(6) . ?
Ni4 N46 2.141(6) . ?
S17 Sb8 2.5912(19) 4_676 ?
S18 Sb8 2.3753(18) 4_676 ?
S21 Sb12 2.4719(18) 3_665 ?
S22 Sb13 2.4493(17) 2_655 ?
N11 C13 1.471(9) . ?
N11 C11 1.483(9) . ?
N11 C15 1.497(9) . ?
N12 C12 1.469(10) . ?
N13 C14 1.484(9) . ?
N14 C16 1.467(10) . ?
N15 C17 1.480(9) . ?
N16 C18 1.468(10) . ?
N21 C21 1.476(9) . ?
N21 C23 1.485(9) . ?
N21 C25 1.486(9) . ?
N22 C22 1.473(9) . ?
N23 C24 1.471(9) . ?
N24 C26 1.472(10) . ?
N25 C28 1.448(8) . ?
N26 C27 1.470(9) . ?
N31 C33 1.478(9) . ?
N31 C35 1.479(9) . ?
N31 C31 1.490(10) . ?
N32 C32A 1.336(15) . ?
N32 C32B 1.71(3) . ?
N33 C34 1.479(9) . ?
N34 C36 1.467(9) . ?
N35 C37 1.408(16) . ?
N36 C38 1.556(13) . ?
N41 C41 1.471(11) . ?
N41 C43 1.480(11) . ?
N41 C45 1.506(10) . ?
N42 C42 1.459(12) . ?
N43 C44 1.463(11) . ?
N44 C46 1.437(12) . ?
N45 C47B 1.455(16) . ?
N45 C47A 1.515(17) . ?
N46 C48A 1.492(14) . ?
N46 C48B 1.526(14) . ?
C11 C12 1.508(11) . ?
C13 C14 1.518(10) . ?
C15 C16 1.516(10) . ?
C17 C18 1.489(11) . ?
C21 C22 1.528(11) . ?
C23 C24 1.506(11) . ?
C25 C26 1.522(10) . ?
C27 C28 1.500(9) . ?
C31 C32B 1.25(3) . ?
C31 C32A 1.570(17) . ?
C33 C34 1.504(11) . ?
C35 C36 1.506(11) . ?
C37 C38 1.432(18) . ?
C41 C42 1.522(15) . ?
C43 C44 1.498(13) . ?
C45 C46 1.493(13) . ?
C47A C48A 1.517(17) . ?
C47B C48B 1.520(18) . ?

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
S20 Sb1 S24 99.26(7) . . ?
S20 Sb1 S11 82.04(6) . . ?
S24 Sb1 S11 88.25(6) . . ?
S20 Sb1 S8 90.08(6) . . ?
S24 Sb1 S8 82.28(5) . . ?
S11 Sb1 S8 166.57(6) . . ?
S3 Sb2 S21 91.42(6) . . ?
S3 Sb2 S14 97.37(6) . . ?
S21 Sb2 S14 86.03(5) . . ?
S14 Sb3 S15 92.72(6) . . ?
S14 Sb3 S10 92.63(6) . . ?
S15 Sb3 S10 88.91(6) . . ?
S12 Sb4 S1 98.02(7) . . ?
S12 Sb4 S5 91.94(6) . . ?
S1 Sb4 S5 102.41(6) . . ?
S2 Sb5 S1 102.69(7) . . ?
S2 Sb5 S15 94.13(6) . . ?
S1 Sb5 S15 90.62(6) . . ?
S8 Sb6 S17 109.69(7) . . ?
S8 Sb6 S7 90.64(6) . . ?
S17 Sb6 S7 85.07(6) . . ?
S8 Sb6 S18 83.44(6) . . ?
S17 Sb6 S18 80.52(6) . . ?
S7 Sb6 S18 161.51(6) . . ?
S24 Sb7 S5 99.34(6) . . ?
S24 Sb7 S9 90.86(6) . . ?
S5 Sb7 S9 88.63(5) . . ?
S24 Sb7 S12 87.27(6) . . ?
S5 Sb7 S12 80.44(5) . . ?
S9 Sb7 S12 168.45(6) . . ?
S18 Sb8 S16 97.07(8) 4_475 . ?
S18 Sb8 S17 85.72(6) 4_475 4_475 ?
S16 Sb8 S17 94.59(7) . 4_475 ?
S18 Sb8 S19 88.52(7) 4_475 . ?
S16 Sb8 S19 84.11(6) . . ?
S17 Sb8 S19 173.89(6) 4_475 . ?
S23 Sb9 S10 101.86(7) . . ?
S23 Sb9 S13 98.34(7) . . ?
S10 Sb9 S13 94.51(6) . . ?
S6 Sb10 S3 94.20(6) . . ?
S6 Sb10 S4 97.59(7) . . ?
S3 Sb10 S4 97.67(6) . . ?
S25 Sb11 S22 100.01(8) . . ?
S25 Sb11 S4 100.99(8) . . ?
S22 Sb11 S4 95.80(7) . . ?
S7 Sb12 S20 92.72(6) . . ?
S7 Sb12 S21 91.00(6) . 3_665 ?
S20 Sb12 S21 97.97(6) . 3_665 ?
S11 Sb13 S9 93.40(6) . . ?
S11 Sb13 S22 94.25(7) . 2_645 ?
S9 Sb13 S22 100.84(6) . 2_645 ?
S19 Sb14 S13 103.49(7) . . ?
S19 Sb14 S16 94.80(7) . . ?
S13 Sb14 S16 92.99(7) . . ?
N11 Ni1 N16 176.1(2) . . ?
N11 Ni1 N14 83.0(2) . . ?
N16 Ni1 N14 94.3(2) . . ?
N11 Ni1 N15 101.7(2) . . ?
N16 Ni1 N15 81.1(2) . . ?
N14 Ni1 N15 173.9(2) . . ?
N11 Ni1 N12 82.4(2) . . ?
N16 Ni1 N12 95.0(2) . . ?
N14 Ni1 N12 93.6(2) . . ?
N15 Ni1 N12 90.8(2) . . ?
N11 Ni1 N13 81.3(2) . . ?
N16 Ni1 N13 101.7(2) . . ?
N14 Ni1 N13 90.8(2) . . ?
N15 Ni1 N13 86.2(2) . . ?
N12 Ni1 N13 162.4(2) . . ?
N26 Ni2 N21 176.0(2) . . ?
N26 Ni2 N24 93.9(2) . . ?
N21 Ni2 N24 82.3(2) . . ?
N26 Ni2 N25 82.0(2) . . ?
N21 Ni2 N25 101.8(2) . . ?
N24 Ni2 N25 175.9(2) . . ?
N26 Ni2 N23 98.6(2) . . ?
N21 Ni2 N23 82.9(2) . . ?
N24 Ni2 N23 91.4(2) . . ?
N25 Ni2 N23 88.8(2) . . ?
N26 Ni2 N22 96.7(2) . . ?
N21 Ni2 N22 82.1(2) . . ?
N24 Ni2 N22 92.6(2) . . ?
N25 Ni2 N22 88.3(2) . . ?
N23 Ni2 N22 163.8(2) . . ?
N31 Ni3 N35 176.3(3) . . ?
N31 Ni3 N32 84.0(3) . . ?
N35 Ni3 N32 95.0(4) . . ?
N31 Ni3 N34 82.2(2) . . ?
N35 Ni3 N34 94.3(3) . . ?
N32 Ni3 N34 92.3(3) . . ?
N31 Ni3 N36 100.1(3) . . ?
N35 Ni3 N36 81.1(4) . . ?
N32 Ni3 N36 174.7(3) . . ?
N34 Ni3 N36 91.6(3) . . ?
N31 Ni3 N33 81.5(2) . . ?
N35 Ni3 N33 102.1(3) . . ?
N32 Ni3 N33 91.2(3) . . ?
N34 Ni3 N33 162.9(2) . . ?
N36 Ni3 N33 86.1(3) . . ?
N41 Ni4 N45 175.7(3) . . ?
N41 Ni4 N43 82.5(3) . . ?
N45 Ni4 N43 96.7(3) . . ?
N41 Ni4 N44 83.2(3) . . ?
N45 Ni4 N44 92.7(3) . . ?
N43 Ni4 N44 90.1(3) . . ?
N41 Ni4 N42 82.2(3) . . ?
N45 Ni4 N42 99.2(3) . . ?
N43 Ni4 N42 162.3(3) . . ?
N44 Ni4 N42 96.8(3) . . ?
N41 Ni4 N46 102.0(2) . . ?
N45 Ni4 N46 82.2(3) . . ?
N43 Ni4 N46 88.2(3) . . ?
N44 Ni4 N46 174.4(3) . . ?
N42 Ni4 N46 86.4(3) . . ?
Sb4 S1 Sb5 96.69(6) . . ?
Sb2 S3 Sb10 89.94(6) . . ?
Sb11 S4 Sb10 98.50(7) . . ?
Sb4 S5 Sb7 89.72(6) . . ?
Sb12 S7 Sb6 94.45(6) . . ?
Sb6 S8 Sb1 93.64(6) . . ?
Sb13 S9 Sb7 93.81(6) . . ?
Sb9 S10 Sb3 97.04(6) . . ?
Sb13 S11 Sb1 92.64(6) . . ?
Sb4 S12 Sb7 84.06(6) . . ?
Sb14 S13 Sb9 92.02(6) . . ?
Sb3 S14 Sb2 100.85(6) . . ?
Sb3 S15 Sb5 92.01(6) . . ?
Sb8 S16 Sb14 87.96(6) . . ?
Sb6 S17 Sb8 92.69(6) . 4_676 ?
Sb8 S18 Sb6 88.49(6) 4_676 . ?
Sb14 S19 Sb8 82.28(6) . . ?
Sb12 S20 Sb1 96.39(6) . . ?
Sb12 S21 Sb2 97.68(6) 3_665 . ?
Sb13 S22 Sb11 96.70(6) 2_655 . ?
Sb7 S24 Sb1 98.61(6) . . ?
C13 N11 C11 112.0(5) . . ?
C13 N11 C15 112.2(6) . . ?
C11 N11 C15 110.6(5) . . ?
C13 N11 Ni1 106.7(4) . . ?
C11 N11 Ni1 105.6(4) . . ?
C15 N11 Ni1 109.4(4) . . ?
C12 N12 Ni1 109.0(4) . . ?
C14 N13 Ni1 110.3(4) . . ?
C16 N14 Ni1 109.1(4) . . ?
C17 N15 Ni1 107.4(4) . . ?
C18 N16 Ni1 109.9(4) . . ?
C21 N21 C23 112.0(5) . . ?
C21 N21 C25 112.2(6) . . ?
C23 N21 C25 109.7(5) . . ?
C21 N21 Ni2 106.1(4) . . ?
C23 N21 Ni2 105.3(4) . . ?
C25 N21 Ni2 111.3(4) . . ?
C22 N22 Ni2 109.7(4) . . ?
C24 N23 Ni2 109.0(4) . . ?
C26 N24 Ni2 109.3(4) . . ?
C28 N25 Ni2 107.9(4) . . ?
C27 N26 Ni2 110.5(4) . . ?
C33 N31 C35 111.9(6) . . ?
C33 N31 C31 111.8(7) . . ?
C35 N31 C31 111.7(6) . . ?
C33 N31 Ni3 107.1(4) . . ?
C35 N31 Ni3 105.3(4) . . ?
C31 N31 Ni3 108.7(5) . . ?
C32A N32 C32B 34.9(11) . . ?
C32A N32 Ni3 111.6(7) . . ?
C32B N32 Ni3 102.8(10) . . ?
C34 N33 Ni3 109.3(4) . . ?
C36 N34 Ni3 110.3(4) . . ?
C37 N35 Ni3 113.1(8) . . ?
C38 N36 Ni3 102.1(6) . . ?
C41 N41 C43 112.8(7) . . ?
C41 N41 C45 113.0(7) . . ?
C43 N41 C45 110.0(7) . . ?
C41 N41 Ni4 105.7(5) . . ?
C43 N41 Ni4 104.8(4) . . ?
C45 N41 Ni4 110.1(5) . . ?
C42 N42 Ni4 110.7(6) . . ?
C44 N43 Ni4 110.7(5) . . ?
C46 N44 Ni4 108.5(5) . . ?
C47B N45 C47A 33.3(10) . . ?
C47B N45 Ni4 106.9(8) . . ?
C47A N45 Ni4 106.7(9) . . ?
C48A N46 C48B 28.7(8) . . ?
C48A N46 Ni4 112.1(7) . . ?
C48B N46 Ni4 102.9(8) . . ?
N11 C11 C12 111.3(6) . . ?
N12 C12 C11 110.5(6) . . ?
N11 C13 C14 111.3(5) . . ?
N13 C14 C13 110.3(6) . . ?
N11 C15 C16 113.3(6) . . ?
N14 C16 C15 109.3(6) . . ?
N15 C17 C18 108.9(7) . . ?
N16 C18 C17 108.5(6) . . ?
N21 C21 C22 110.5(6) . . ?
N22 C22 C21 110.2(6) . . ?
N21 C23 C24 111.1(5) . . ?
N23 C24 C23 111.9(6) . . ?
N21 C25 C26 112.5(6) . . ?
N24 C26 C25 110.0(6) . . ?
N26 C27 C28 110.9(6) . . ?
N25 C28 C27 111.1(6) . . ?
C32B C31 N31 120.8(15) . . ?
C32B C31 C32A 38.5(14) . . ?
N31 C31 C32A 113.1(8) . . ?
N32 C32A C31 113.1(10) . . ?
C31 C32B N32 110(2) . . ?
N31 C33 C34 110.6(6) . . ?
N33 C34 C33 109.2(6) . . ?
N31 C35 C36 110.9(6) . . ?
N34 C36 C35 110.8(6) . . ?
N35 C37 C38 108.7(9) . . ?
C37 C38 N36 110.8(9) . . ?
N41 C41 C42 111.2(7) . . ?
N42 C42 C41 108.4(7) . . ?
N41 C43 C44 111.2(6) . . ?
N43 C44 C43 110.5(7) . . ?
C46 C45 N41 112.6(7) . . ?
N44 C46 C45 113.9(8) . . ?
N45 C47A C48A 114.4(13) . . ?
N46 C48A C47A 104.1(13) . . ?
N45 C47B C48B 102.4(13) . . ?
C47B C48B N46 105.9(12) . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        24.63
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         0.884
_refine_diff_density_min         -0.773
_refine_diff_density_rms         0.117