# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2013

#######################################################################
#
#                 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.
#
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#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
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#  data retrieval see:
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#  from this site to visualise CIF-encoded structures and 
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data_As(mnt)2
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H20 P, C8 As N4 S4'
_chemical_formula_sum            'C32 H20 As N4 P S4'
_chemical_formula_weight         694.69

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0020 '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'
As As 0.0500 2.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1020 0.0940 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1250 0.1230 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P21/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                   7.713(5)
_cell_length_b                   15.765(5)
_cell_length_c                   26.415(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.696(12)
_cell_angle_gamma                90.00
_cell_volume                     3166(2)
_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       needle
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1408
_exptl_absorpt_coefficient_mu    1.417
_exptl_absorpt_correction_type   Empirical
_exptl_absorpt_correction_T_min  0.758
_exptl_absorpt_correction_T_max  0.895
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART APEX'
_diffrn_measurement_method       /w-scans
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            20593
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_av_sigmaI/netI    0.0594
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         2.58
_diffrn_reflns_theta_max         28.31
_reflns_number_total             7815
_reflns_number_gt                5070
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART 5.628 (Bruker, 2003)'
_computing_cell_refinement       'SAINT 6.45 ( Bruker, 2003)'
_computing_data_reduction        'SAINT 6.45 (Bruker, 2003)'
_computing_structure_solution    SIR-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Diamond 3.1e, Ortep'
_computing_publication_material  ?

_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^)+(0.0929P)^2^+16.5004P] 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         7815
_refine_ls_number_parameters     379
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1252
_refine_ls_R_factor_gt           0.0791
_refine_ls_wR_factor_ref         0.2391
_refine_ls_wR_factor_gt          0.1920
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      1.028
_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
P1 P 0.43155(17) 0.47665(8) 0.32503(5) 0.0255(3) Uani 1 1 d . . .
C9 C 0.5468(6) 0.4170(3) 0.28358(18) 0.0257(10) Uani 1 1 d . . .
C10 C 0.5228(7) 0.3296(3) 0.27805(19) 0.0286(10) Uani 1 1 d . . .
H10 H 0.4482 0.3010 0.2964 0.034 Uiso 1 1 calc R . .
C11 C 0.6122(7) 0.2860(3) 0.2447(2) 0.0329(11) Uani 1 1 d . . .
H11 H 0.5991 0.2275 0.2411 0.039 Uiso 1 1 calc R . .
C12 C 0.7210(8) 0.3292(4) 0.2167(2) 0.0374(13) Uani 1 1 d . . .
H12 H 0.7789 0.2999 0.1939 0.045 Uiso 1 1 calc R . .
C13 C 0.7434(8) 0.4153(4) 0.2224(2) 0.0407(13) Uani 1 1 d . . .
H13 H 0.8163 0.4437 0.2034 0.049 Uiso 1 1 calc R . .
C14 C 0.6595(8) 0.4605(3) 0.2561(2) 0.0339(12) Uani 1 1 d . . .
H14 H 0.6774 0.5185 0.2605 0.041 Uiso 1 1 calc R . .
C15 C 0.2682(7) 0.5424(3) 0.2885(2) 0.0295(11) Uani 1 1 d . . .
C16 C 0.2557(8) 0.5525(3) 0.2357(2) 0.0329(11) Uani 1 1 d . . .
H16 H 0.3351 0.5252 0.2183 0.040 Uiso 1 1 calc R . .
C17 C 0.1247(8) 0.6032(4) 0.2092(2) 0.0402(13) Uani 1 1 d . . .
H17 H 0.1154 0.6095 0.1739 0.048 Uiso 1 1 calc R . .
C18 C 0.0070(8) 0.6446(4) 0.2350(3) 0.0422(14) Uani 1 1 d . . .
H18 H -0.0788 0.6797 0.2170 0.051 Uiso 1 1 calc R . .
C19 C 0.0165(7) 0.6341(3) 0.2873(3) 0.0390(13) Uani 1 1 d . . .
H19 H -0.0641 0.6611 0.3044 0.047 Uiso 1 1 calc R . .
C20 C 0.1468(7) 0.5832(3) 0.3141(2) 0.0353(12) Uani 1 1 d . . .
H20 H 0.1537 0.5759 0.3493 0.042 Uiso 1 1 calc R . .
C21 C 0.3179(7) 0.4089(3) 0.36326(19) 0.0279(10) Uani 1 1 d . . .
C22 C 0.1633(7) 0.3694(3) 0.3400(2) 0.0312(11) Uani 1 1 d . . .
H22 H 0.1215 0.3771 0.3052 0.037 Uiso 1 1 calc R . .
C23 C 0.0723(8) 0.3182(3) 0.3695(2) 0.0367(12) Uani 1 1 d . . .
H23 H -0.0317 0.2920 0.3545 0.044 Uiso 1 1 calc R . .
C24 C 0.1359(8) 0.3062(4) 0.4209(2) 0.0422(14) Uani 1 1 d . . .
H24 H 0.0746 0.2715 0.4402 0.051 Uiso 1 1 calc R . .
C25 C 0.2894(9) 0.3449(4) 0.4441(2) 0.0473(15) Uani 1 1 d . . .
H25 H 0.3315 0.3362 0.4788 0.057 Uiso 1 1 calc R . .
C26 C 0.3806(8) 0.3969(4) 0.4150(2) 0.0366(12) Uani 1 1 d . . .
H26 H 0.4837 0.4236 0.4303 0.044 Uiso 1 1 calc R . .
C27 C 0.5939(7) 0.5381(3) 0.3663(2) 0.0297(11) Uani 1 1 d . . .
C28 C 0.5633(8) 0.6223(3) 0.3784(2) 0.0359(12) Uani 1 1 d . . .
H28 H 0.4589 0.6491 0.3643 0.043 Uiso 1 1 calc R . .
C29 C 0.6919(9) 0.6655(4) 0.4120(2) 0.0449(15) Uani 1 1 d . . .
H29 H 0.6739 0.7218 0.4203 0.054 Uiso 1 1 calc R . .
C30 C 0.8455(9) 0.6251(4) 0.4331(2) 0.0453(15) Uani 1 1 d . . .
H30 H 0.9295 0.6543 0.4560 0.054 Uiso 1 1 calc R . .
C31 C 0.8767(8) 0.5429(4) 0.4209(2) 0.0430(14) Uani 1 1 d . . .
H31 H 0.9820 0.5169 0.4351 0.052 Uiso 1 1 calc R . .
C32 C 0.7512(8) 0.4982(4) 0.3875(2) 0.0370(12) Uani 1 1 d . . .
H32 H 0.7717 0.4421 0.3793 0.044 Uiso 1 1 calc R . .
As1 As 0.27314(13) 0.46338(5) 0.01495(3) 0.0646(3) Uani 1 1 d . . .
S1 S 0.3339(3) 0.44468(17) 0.11068(7) 0.0870(9) Uani 1 1 d . . .
S2 S 0.0274(2) 0.38094(9) 0.01370(5) 0.0457(4) Uani 1 1 d . . .
S3 S 0.4842(3) 0.36215(14) 0.01333(6) 0.0628(6) Uani 1 1 d . . .
S4 S 0.2119(3) 0.45661(10) -0.08250(6) 0.0559(5) Uani 1 1 d . . .
N1 N 0.1486(6) 0.3313(3) 0.21037(17) 0.0384(11) Uani 1 1 d . . .
N2 N -0.2044(7) 0.2484(3) 0.09451(19) 0.0443(12) Uani 1 1 d . . .
N3 N 0.7225(8) 0.2433(6) -0.0723(3) 0.086(2) Uani 1 1 d . . .
N4 N 0.4139(7) 0.3597(3) -0.18501(19) 0.0380(11) Uani 1 1 d . . .
C1 C 0.1596(8) 0.3799(3) 0.1173(2) 0.0356(12) Uani 1 1 d . . .
C2 C 0.1522(7) 0.3517(3) 0.1689(2) 0.0311(11) Uani 1 1 d . . .
C3 C 0.0345(7) 0.3535(3) 0.07832(19) 0.0292(10) Uani 1 1 d . . .
C4 C -0.0993(7) 0.2960(3) 0.08734(19) 0.0302(11) Uani 1 1 d . . .
C5 C 0.4896(8) 0.3497(4) -0.0524(2) 0.0453(15) Uani 1 1 d . . .
C6 C 0.6191(9) 0.2907(6) -0.0641(3) 0.061(2) Uani 1 1 d . . .
C7 C 0.3788(8) 0.3879(3) -0.0904(2) 0.0375(13) Uani 1 1 d . . .
C8 C 0.4000(8) 0.3713(3) -0.1428(2) 0.0337(12) Uani 1 1 d . . .

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
P1 0.0315(7) 0.0205(6) 0.0271(6) -0.0001(5) 0.0118(5) -0.0006(5)
C9 0.030(3) 0.022(2) 0.026(2) -0.0016(18) 0.0086(19) 0.0042(18)
C10 0.030(3) 0.026(2) 0.031(3) 0.002(2) 0.007(2) -0.0001(19)
C11 0.041(3) 0.024(2) 0.035(3) 0.001(2) 0.011(2) 0.005(2)
C12 0.045(3) 0.034(3) 0.036(3) -0.001(2) 0.017(2) 0.010(2)
C13 0.050(4) 0.036(3) 0.041(3) 0.006(2) 0.023(3) 0.001(3)
C14 0.046(3) 0.025(2) 0.036(3) 0.000(2) 0.023(2) -0.001(2)
C15 0.032(3) 0.024(2) 0.033(3) 0.002(2) 0.008(2) -0.004(2)
C16 0.044(3) 0.023(2) 0.034(3) 0.003(2) 0.011(2) -0.003(2)
C17 0.050(4) 0.036(3) 0.034(3) 0.005(2) 0.007(3) -0.003(3)
C18 0.036(3) 0.031(3) 0.057(4) 0.007(3) 0.001(3) 0.002(2)
C19 0.032(3) 0.025(3) 0.063(4) -0.001(2) 0.017(3) 0.000(2)
C20 0.040(3) 0.028(3) 0.041(3) 0.001(2) 0.017(2) 0.002(2)
C21 0.035(3) 0.022(2) 0.029(2) 0.0004(19) 0.013(2) 0.0004(19)
C22 0.037(3) 0.030(3) 0.030(3) -0.001(2) 0.012(2) 0.001(2)
C23 0.041(3) 0.029(3) 0.043(3) -0.005(2) 0.015(2) -0.006(2)
C24 0.046(3) 0.038(3) 0.049(3) 0.012(3) 0.028(3) 0.001(3)
C25 0.052(4) 0.058(4) 0.036(3) 0.015(3) 0.015(3) -0.006(3)
C26 0.039(3) 0.039(3) 0.033(3) 0.003(2) 0.009(2) -0.003(2)
C27 0.035(3) 0.026(2) 0.032(3) 0.001(2) 0.017(2) -0.002(2)
C28 0.044(3) 0.032(3) 0.034(3) -0.003(2) 0.014(2) -0.007(2)
C29 0.063(4) 0.029(3) 0.047(3) -0.011(2) 0.021(3) -0.017(3)
C30 0.047(4) 0.052(4) 0.038(3) -0.009(3) 0.010(3) -0.025(3)
C31 0.035(3) 0.051(4) 0.043(3) -0.001(3) 0.008(3) -0.011(3)
C32 0.041(3) 0.033(3) 0.039(3) -0.003(2) 0.010(2) -0.002(2)
As1 0.1189(7) 0.0477(4) 0.0380(4) -0.0171(3) 0.0445(4) -0.0485(4)
S1 0.1135(18) 0.1204(18) 0.0356(9) -0.0295(10) 0.0370(10) -0.0936(16)
S2 0.0818(12) 0.0328(7) 0.0239(6) -0.0015(5) 0.0131(7) -0.0178(7)
S3 0.0635(11) 0.0949(15) 0.0294(8) 0.0063(8) 0.0059(7) -0.0432(11)
S4 0.1090(15) 0.0316(7) 0.0361(8) 0.0032(6) 0.0385(9) 0.0109(8)
N1 0.044(3) 0.044(3) 0.027(2) -0.001(2) 0.007(2) -0.012(2)
N2 0.040(3) 0.056(3) 0.038(3) -0.001(2) 0.009(2) -0.012(2)
N3 0.034(3) 0.136(7) 0.088(5) 0.026(5) 0.016(3) 0.006(4)
N4 0.048(3) 0.029(2) 0.040(3) -0.0049(19) 0.016(2) -0.004(2)
C1 0.047(3) 0.034(3) 0.028(3) -0.007(2) 0.015(2) -0.011(2)
C2 0.031(3) 0.031(3) 0.033(3) -0.005(2) 0.008(2) -0.009(2)
C3 0.039(3) 0.022(2) 0.028(2) -0.0021(19) 0.009(2) -0.002(2)
C4 0.034(3) 0.031(3) 0.026(2) 0.003(2) 0.006(2) 0.000(2)
C5 0.040(3) 0.054(4) 0.043(3) 0.001(3) 0.013(3) -0.025(3)
C6 0.025(3) 0.101(6) 0.056(4) 0.016(4) 0.007(3) -0.010(4)
C7 0.054(4) 0.033(3) 0.028(3) -0.001(2) 0.014(2) -0.014(3)
C8 0.043(3) 0.023(2) 0.037(3) -0.002(2) 0.013(2) -0.007(2)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1 C15 1.784(5) . ?
P1 C9 1.789(5) . ?
P1 C27 1.799(6) . ?
P1 C21 1.797(5) . ?
C9 C10 1.395(7) . ?
C9 C14 1.401(7) . ?
C10 C11 1.390(7) . ?
C10 H10 0.9300 . ?
C11 C12 1.388(7) . ?
C11 H11 0.9300 . ?
C12 C13 1.373(8) . ?
C12 H12 0.9300 . ?
C13 C14 1.383(7) . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
C15 C16 1.391(7) . ?
C15 C20 1.399(7) . ?
C16 C17 1.383(8) . ?
C16 H16 0.9300 . ?
C17 C18 1.387(8) . ?
C17 H17 0.9300 . ?
C18 C19 1.380(9) . ?
C18 H18 0.9300 . ?
C19 C20 1.385(8) . ?
C19 H19 0.9300 . ?
C20 H20 0.9300 . ?
C21 C26 1.383(7) . ?
C21 C22 1.393(7) . ?
C22 C23 1.391(7) . ?
C22 H22 0.9300 . ?
C23 C24 1.376(8) . ?
C23 H23 0.9300 . ?
C24 C25 1.380(9) . ?
C24 H24 0.9300 . ?
C25 C26 1.394(8) . ?
C25 H25 0.9300 . ?
C26 H26 0.9300 . ?
C27 C28 1.394(7) . ?
C27 C32 1.397(8) . ?
C28 C29 1.392(8) . ?
C28 H28 0.9300 . ?
C29 C30 1.378(9) . ?
C29 H29 0.9300 . ?
C30 C31 1.366(9) . ?
C30 H30 0.9300 . ?
C31 C32 1.387(8) . ?
C31 H31 0.9300 . ?
C32 H32 0.9300 . ?
As1 S3 2.285(3) . ?
As1 S2 2.294(2) . ?
As1 S1 2.510(2) . ?
As1 S4 2.5397(18) . ?
S1 C1 1.721(6) . ?
S2 C3 1.753(5) . ?
S3 C5 1.755(6) . ?
S4 C7 1.722(6) . ?
N1 C2 1.147(7) . ?
N2 C4 1.144(7) . ?
N3 C6 1.140(11) . ?
N4 C8 1.152(7) . ?
C1 C3 1.353(8) . ?
C1 C2 1.443(7) . ?
C3 C4 1.423(7) . ?
C5 C7 1.345(9) . ?
C5 C6 1.436(11) . ?
C7 C8 1.446(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C15 P1 C9 110.7(2) . . ?
C15 P1 C27 111.8(2) . . ?
C9 P1 C27 106.7(2) . . ?
C15 P1 C21 106.4(2) . . ?
C9 P1 C21 111.8(2) . . ?
C27 P1 C21 109.6(2) . . ?
C10 C9 C14 120.8(4) . . ?
C10 C9 P1 120.8(4) . . ?
C14 C9 P1 118.4(4) . . ?
C11 C10 C9 119.0(5) . . ?
C11 C10 H10 120.5 . . ?
C9 C10 H10 120.5 . . ?
C12 C11 C10 120.2(5) . . ?
C12 C11 H11 119.9 . . ?
C10 C11 H11 119.9 . . ?
C13 C12 C11 120.2(5) . . ?
C13 C12 H12 119.9 . . ?
C11 C12 H12 119.9 . . ?
C12 C13 C14 121.1(5) . . ?
C12 C13 H13 119.5 . . ?
C14 C13 H13 119.5 . . ?
C13 C14 C9 118.7(5) . . ?
C13 C14 H14 120.7 . . ?
C9 C14 H14 120.7 . . ?
C16 C15 C20 119.5(5) . . ?
C16 C15 P1 122.1(4) . . ?
C20 C15 P1 118.3(4) . . ?
C17 C16 C15 119.6(5) . . ?
C17 C16 H16 120.2 . . ?
C15 C16 H16 120.2 . . ?
C16 C17 C18 120.4(5) . . ?
C16 C17 H17 119.8 . . ?
C18 C17 H17 119.8 . . ?
C19 C18 C17 120.4(5) . . ?
C19 C18 H18 119.8 . . ?
C17 C18 H18 119.8 . . ?
C18 C19 C20 119.5(5) . . ?
C18 C19 H19 120.3 . . ?
C20 C19 H19 120.3 . . ?
C19 C20 C15 120.5(5) . . ?
C19 C20 H20 119.8 . . ?
C15 C20 H20 119.8 . . ?
C26 C21 C22 120.4(5) . . ?
C26 C21 P1 120.9(4) . . ?
C22 C21 P1 118.7(4) . . ?
C23 C22 C21 119.1(5) . . ?
C23 C22 H22 120.4 . . ?
C21 C22 H22 120.4 . . ?
C24 C23 C22 120.2(5) . . ?
C24 C23 H23 119.9 . . ?
C22 C23 H23 119.9 . . ?
C23 C24 C25 120.9(5) . . ?
C23 C24 H24 119.5 . . ?
C25 C24 H24 119.5 . . ?
C24 C25 C26 119.3(6) . . ?
C24 C25 H25 120.3 . . ?
C26 C25 H25 120.3 . . ?
C21 C26 C25 120.0(6) . . ?
C21 C26 H26 120.0 . . ?
C25 C26 H26 120.0 . . ?
C28 C27 C32 120.4(5) . . ?
C28 C27 P1 121.6(4) . . ?
C32 C27 P1 118.0(4) . . ?
C29 C28 C27 118.8(6) . . ?
C29 C28 H28 120.6 . . ?
C27 C28 H28 120.6 . . ?
C30 C29 C28 120.2(5) . . ?
C30 C29 H29 119.9 . . ?
C28 C29 H29 119.9 . . ?
C31 C30 C29 121.1(6) . . ?
C31 C30 H30 119.4 . . ?
C29 C30 H30 119.4 . . ?
C30 C31 C32 120.0(6) . . ?
C30 C31 H31 120.0 . . ?
C32 C31 H31 120.0 . . ?
C31 C32 C27 119.5(5) . . ?
C31 C32 H32 120.3 . . ?
C27 C32 H32 120.3 . . ?
S3 As1 S2 101.17(8) . . ?
S3 As1 S1 85.65(9) . . ?
S2 As1 S1 87.80(6) . . ?
S3 As1 S4 87.89(6) . . ?
S2 As1 S4 87.10(6) . . ?
S1 As1 S4 170.85(8) . . ?
C1 S1 As1 99.0(2) . . ?
C3 S2 As1 103.63(19) . . ?
C5 S3 As1 103.4(3) . . ?
C7 S4 As1 97.7(2) . . ?
C3 C1 C2 119.2(5) . . ?
C3 C1 S1 125.0(4) . . ?
C2 C1 S1 115.8(4) . . ?
N1 C2 C1 178.1(6) . . ?
C1 C3 C4 120.8(5) . . ?
C1 C3 S2 124.5(4) . . ?
C4 C3 S2 114.6(4) . . ?
N2 C4 C3 178.5(6) . . ?
C7 C5 C6 120.4(6) . . ?
C7 C5 S3 124.7(5) . . ?
C6 C5 S3 114.8(5) . . ?
N3 C6 C5 178.5(8) . . ?
C5 C7 C8 118.3(6) . . ?
C5 C7 S4 125.8(5) . . ?
C8 C7 S4 115.9(4) . . ?
N4 C8 C7 178.3(6) . . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        28.31
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         0.984
_refine_diff_density_min         -0.827
_refine_diff_density_rms         0.135


_database_code_depnum_ccdc_archive 'CCDC 899118'
#######################################################################
#
#                 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_Sb(mnt)2
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H20 P, C8 N4 S4 Sb'
_chemical_formula_sum            'C32 H20 N4 P S4 Sb'
_chemical_formula_weight         741.48

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'
Sb Sb -0.5866 1.5461 '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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   P21212

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

_cell_length_a                   12.843(5)
_cell_length_b                   17.361(5)
_cell_length_c                   7.026(5)
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 90.000(5)
_cell_angle_gamma                90.000(5)
_cell_volume                     1566.6(13)
_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          0.04
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.572
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             740
_exptl_absorpt_coefficient_mu    1.228
_exptl_absorpt_correction_type   Empirical
_exptl_absorpt_correction_T_min  0.948
_exptl_absorpt_correction_T_max  0.969
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       /w-scans
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10253
_diffrn_reflns_av_R_equivalents  0.0395
_diffrn_reflns_av_sigmaI/netI    0.0479
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.83
_diffrn_reflns_theta_max         28.34
_reflns_number_total             3872
_reflns_number_gt                3473
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART 5.628 (Bruker, 2003)'
_computing_cell_refinement       'SAINT 6.45 ( Bruker, 2003)'
_computing_data_reduction        'SAINT 6.45 ( Bruker, 2003)'
_computing_structure_solution    SIR-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Diamond 3.1e, Ortep'
_computing_publication_material  ?

_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^)+(0.0127P)^2^+10.5106P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   1.03(4)
_refine_ls_number_reflns         3872
_refine_ls_number_parameters     191
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0631
_refine_ls_R_factor_gt           0.0420
_refine_ls_wR_factor_ref         0.1273
_refine_ls_wR_factor_gt          0.0878
_refine_ls_goodness_of_fit_ref   1.188
_refine_ls_restrained_S_all      1.188
_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
Sb1 Sb 0.0000 0.5000 0.81618(7) 0.02135(14) Uani 1 2 d S . .
P1 P -0.5000 0.5000 0.8590(2) 0.0175(3) Uani 1 2 d S . .
S1 S -0.10828(13) 0.57485(11) 1.0384(3) 0.0346(4) Uani 1 1 d . . .
S2 S 0.13708(12) 0.60949(9) 0.8863(3) 0.0264(3) Uani 1 1 d . . .
N1 N -0.1058(5) 0.7214(3) 1.4074(9) 0.0351(14) Uani 1 1 d . . .
N2 N 0.1853(5) 0.7617(3) 1.2385(10) 0.0354(15) Uani 1 1 d . . .
C1 C 0.0764(5) 0.6555(4) 1.0765(9) 0.0220(12) Uani 1 1 d . . .
C2 C -0.0223(5) 0.6429(4) 1.1346(9) 0.0252(14) Uani 1 1 d . . .
C3 C -0.0673(5) 0.6864(4) 1.2852(10) 0.0275(14) Uani 1 1 d . . .
C4 C 0.1359(5) 0.7155(3) 1.1694(10) 0.0257(13) Uani 1 1 d . . .
C5 C -0.4831(4) 0.5821(3) 1.0099(8) 0.0187(12) Uani 1 1 d . . .
C6 C -0.5603(5) 0.6381(4) 1.0303(9) 0.0221(12) Uani 1 1 d . . .
H6 H -0.6211 0.6350 0.9590 0.027 Uiso 1 1 calc R . .
C7 C -0.5457(5) 0.6987(3) 1.1580(10) 0.0243(13) Uani 1 1 d . . .
H7 H -0.5967 0.7364 1.1716 0.029 Uiso 1 1 calc R . .
C8 C -0.4548(5) 0.7027(4) 1.2644(10) 0.0242(13) Uani 1 1 d . . .
H8 H -0.4450 0.7431 1.3495 0.029 Uiso 1 1 calc R . .
C9 C -0.3784(5) 0.6466(4) 1.2446(9) 0.0261(13) Uani 1 1 d . . .
H9 H -0.3176 0.6496 1.3163 0.031 Uiso 1 1 calc R . .
C10 C -0.3923(5) 0.5865(3) 1.1193(9) 0.0231(12) Uani 1 1 d . . .
H10 H -0.3412 0.5488 1.1074 0.028 Uiso 1 1 calc R . .
C11 C -0.3890(4) 0.4880(4) 0.7065(8) 0.0210(12) Uani 1 1 d . . .
C12 C -0.3822(5) 0.4186(4) 0.6015(9) 0.0226(12) Uani 1 1 d . . .
H12 H -0.4324 0.3804 0.6156 0.027 Uiso 1 1 calc R . .
C13 C -0.2993(5) 0.4083(4) 0.4771(10) 0.0287(14) Uani 1 1 d . . .
H13 H -0.2939 0.3630 0.4071 0.034 Uiso 1 1 calc R . .
C14 C -0.2250(5) 0.4651(4) 0.4569(10) 0.0259(13) Uani 1 1 d . . .
H14 H -0.1688 0.4572 0.3758 0.031 Uiso 1 1 calc R . .
C15 C -0.2334(5) 0.5340(4) 0.5565(10) 0.0258(13) Uani 1 1 d . . .
H15 H -0.1845 0.5728 0.5378 0.031 Uiso 1 1 calc R . .
C16 C -0.3151(4) 0.5450(3) 0.6844(10) 0.0207(11) Uani 1 1 d . . .
H16 H -0.3198 0.5904 0.7542 0.025 Uiso 1 1 calc R . .

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 0.0223(2) 0.0214(2) 0.0204(2) 0.000 0.000 -0.0002(3)
P1 0.0169(8) 0.0159(8) 0.0196(9) 0.000 0.000 0.0005(10)
S1 0.0244(8) 0.0396(10) 0.0398(10) -0.0146(8) 0.0105(7) -0.0127(7)
S2 0.0235(7) 0.0229(7) 0.0328(8) -0.0001(6) 0.0071(7) -0.0012(6)
N1 0.040(3) 0.031(3) 0.034(3) -0.016(3) 0.007(3) -0.007(3)
N2 0.032(3) 0.026(3) 0.049(4) -0.004(3) -0.012(3) -0.006(2)
C1 0.021(3) 0.020(3) 0.025(3) 0.002(2) -0.004(2) -0.001(2)
C2 0.026(4) 0.023(3) 0.026(3) 0.004(2) -0.002(2) -0.001(2)
C3 0.026(3) 0.024(3) 0.032(4) 0.005(3) -0.003(3) -0.006(2)
C4 0.025(3) 0.021(3) 0.031(3) 0.009(3) -0.006(3) 0.005(2)
C5 0.018(3) 0.017(2) 0.021(2) 0.0004(19) 0.002(2) -0.004(2)
C6 0.018(3) 0.025(3) 0.023(3) 0.002(2) 0.000(2) 0.000(2)
C7 0.030(3) 0.015(3) 0.028(3) -0.001(2) 0.011(3) 0.006(2)
C8 0.032(3) 0.014(3) 0.027(3) -0.001(2) 0.000(3) -0.005(2)
C9 0.029(3) 0.025(3) 0.024(3) 0.003(2) -0.003(3) -0.006(3)
C10 0.027(3) 0.018(3) 0.024(3) 0.002(2) -0.003(3) 0.002(2)
C11 0.020(2) 0.027(3) 0.016(2) 0.002(2) -0.002(2) 0.002(2)
C12 0.022(3) 0.023(3) 0.022(3) -0.002(2) -0.002(2) 0.008(2)
C13 0.028(3) 0.035(4) 0.023(3) -0.002(3) -0.003(3) 0.005(3)
C14 0.020(3) 0.041(4) 0.016(3) 0.006(3) 0.001(2) 0.006(3)
C15 0.023(3) 0.032(3) 0.023(3) 0.006(3) -0.001(3) 0.004(3)
C16 0.021(3) 0.019(3) 0.023(3) 0.000(2) -0.004(3) 0.002(2)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sb1 S1 2.462(2) . ?
Sb1 S1 2.462(2) 2_565 ?
Sb1 S2 2.6373(17) . ?
Sb1 S2 2.6373(17) 2_565 ?
P1 C5 1.790(6) . ?
P1 C5 1.790(6) 2_465 ?
P1 C11 1.796(6) 2_465 ?
P1 C11 1.796(6) . ?
S1 C2 1.753(6) . ?
S2 C1 1.741(7) . ?
N1 C3 1.161(9) . ?
N2 C4 1.132(8) . ?
C1 C2 1.349(9) . ?
C1 C4 1.447(9) . ?
C2 C3 1.424(9) . ?
C5 C6 1.396(8) . ?
C5 C10 1.399(8) . ?
C6 C7 1.396(9) . ?
C7 C8 1.388(9) . ?
C8 C9 1.390(9) . ?
C9 C10 1.376(9) . ?
C11 C16 1.380(8) . ?
C11 C12 1.416(8) . ?
C12 C13 1.389(9) . ?
C13 C14 1.378(10) . ?
C14 C15 1.391(9) . ?
C15 C16 1.395(9) . ?

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
S1 Sb1 S1 101.26(11) . 2_565 ?
S1 Sb1 S2 83.00(6) . . ?
S1 Sb1 S2 83.39(6) 2_565 . ?
S1 Sb1 S2 83.39(6) . 2_565 ?
S1 Sb1 S2 83.00(6) 2_565 2_565 ?
S2 Sb1 S2 158.47(8) . 2_565 ?
C5 P1 C5 107.3(4) . 2_465 ?
C5 P1 C11 111.0(3) . 2_465 ?
C5 P1 C11 110.5(3) 2_465 2_465 ?
C5 P1 C11 110.5(3) . . ?
C5 P1 C11 111.0(3) 2_465 . ?
C11 P1 C11 106.7(4) 2_465 . ?
C2 S1 Sb1 104.1(2) . . ?
C1 S2 Sb1 100.1(2) . . ?
C2 C1 C4 118.5(6) . . ?
C2 C1 S2 125.3(5) . . ?
C4 C1 S2 116.1(5) . . ?
C1 C2 C3 121.4(6) . . ?
C1 C2 S1 125.8(5) . . ?
C3 C2 S1 112.8(5) . . ?
N1 C3 C2 178.8(7) . . ?
N2 C4 C1 177.6(8) . . ?
C6 C5 C10 119.8(5) . . ?
C6 C5 P1 122.0(4) . . ?
C10 C5 P1 118.1(4) . . ?
C5 C6 C7 119.8(6) . . ?
C8 C7 C6 119.7(6) . . ?
C7 C8 C9 120.4(6) . . ?
C10 C9 C8 120.2(6) . . ?
C9 C10 C5 120.1(6) . . ?
C16 C11 C12 120.6(5) . . ?
C16 C11 P1 122.0(5) . . ?
C12 C11 P1 117.3(4) . . ?
C13 C12 C11 119.0(6) . . ?
C14 C13 C12 120.3(6) . . ?
C13 C14 C15 120.6(6) . . ?
C14 C15 C16 120.0(6) . . ?
C11 C16 C15 119.4(6) . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        28.34
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         1.240
_refine_diff_density_min         -0.861
_refine_diff_density_rms         0.161


_database_code_depnum_ccdc_archive 'CCDC 899119'