# Supplementary Material (ESI) for Chemical Communications
# This journal is (c) The Royal Society of Chemistry 2010

data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182
loop_
_publ_author_name
_publ_author_address
C.Rotter
;
Department Chemie
Ludwig-Maximilians-University Munich
Butenandtstrasse 9 (Haus D)
D-81377 Munich
Germany
;
C.Evangelisti
;
Department Chemie
Ludwig-Maximilians-University Munich
Butenandtstrasse 9 (Haus D)
D-81377 Munich
Germany
;
S.Schonberger
;
Department Chemie
Ludwig-Maximilians-University Munich
Butenandtstrasse 9 (Haus D)
D-81377 Munich
Germany
;
T.M.Klapotke
;
Department Chemie
Ludwig-Maximilians-University Munich
Butenandtstrasse 9 (Haus D)
D-81377 Munich
Germany
;
;
K.Karaghiosoff
;
;
Department Chemie
Ludwig-Maximilians-University Munich
Butenandtstrasse 9 (Haus D)
D-81377 Munich
Germany
;

_publ_contact_author_name        'Karaghiosoff, Konstantin'
_publ_contact_author_email       klk@cup.uni-muenchen.de

_publ_section_title              
;
py2P2S7: A Bis(pyridine)adduct Stabilized Phosphorus Sulfide
;
loop_
_publ_contact_author_address
;
Department Chemie
Ludwig-Maximilians-University Munich
Butenandtstrasse 9 (Haus D)
D-81377 Munich
Germany
;
loop_
_publ_contact_author_fax
'+49 89 2180 77492'
loop_
_publ_contact_author_phone
'+49 89 2180 77426'

# Attachment 'Crystal-data.doc'

data_v1
_database_code_depnum_ccdc_archive 'CCDC 762680'
#TrackingRef 'Crystal-data.doc'

_audit_author_name               'Mayer, P.'
_audit_creation_date             01-09-2009
_audit_creation_method           SHELXL-97

_chemical_formula_moiety         'C10 H10 N2 P2 S7'
_chemical_formula_sum            ' C10 H10 N2 P2 S7'
_chemical_formula_weight         444.63
_publ_section_abstract           
;
The new phosphorus sulfide P2S7, stabilized as the bis(pyridinium) adduct
was obtained from the reaction of P4S10 and sulfur in pyridine, and could
be isolated in form of colourless blockshaped crystals which were
characterized using single crystal X-ray diffraction. Coordination of
pyridine is weak (d(P-N) = 187 pm) which is supported also by quantum
chemical calculations.
;

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'
Na Na 0.0362 0.0249 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/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                   13.000(3)
_cell_length_b                   8.0185(16)
_cell_length_c                   17.332(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.68(3)
_cell_angle_gamma                90.00
_cell_volume                     1790.5(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    6173

_cell_measurement_theta_min      3.134

_cell_measurement_theta_max      25.350

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.179

_exptl_crystal_size_mid          0.101

_exptl_crystal_size_min          0.043
_exptl_crystal_density_diffrn    1.649
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             904
_exptl_absorpt_coefficient_mu    1.051
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.880
_exptl_absorpt_correction_T_max  0.956

_diffrn_ambient_temperature      200(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  KappaCCD
_diffrn_measurement_method       ' 95mm CCD camera on \k-goniostat'
_diffrn_detector_area_resol_mean 9
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11002
_diffrn_reflns_av_R_equivalents  0.0617
_diffrn_reflns_av_sigmaI/netI    0.0528
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.14
_diffrn_reflns_theta_max         25.29
_reflns_number_total             3259
_reflns_number_gt                2316
_reflns_threshold_expression     >2\s(I)

_computing_data_collection       ?
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'

_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_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^ > 2\s(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^)+(0.0372P)^2^+1.1655P] 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         3259
_refine_ls_number_parameters     190
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0755
_refine_ls_R_factor_gt           0.0421
_refine_ls_wR_factor_ref         0.0980
_refine_ls_wR_factor_gt          0.0888
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.052
_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
P2 P 0.33236(7) 0.22115(13) 0.20630(5) 0.0349(2) Uani 1 1 d . . .
S5 S 0.20404(7) 0.07077(14) 0.22363(6) 0.0450(3) Uani 1 1 d . . .
S3 S 0.30611(7) -0.18613(13) 0.36287(6) 0.0443(3) Uani 1 1 d . . .
S7 S 0.26992(9) 0.43773(14) 0.18179(6) 0.0521(3) Uani 1 1 d . . .
S4 S 0.26495(9) -0.16218(13) 0.24424(6) 0.0518(3) Uani 1 1 d . . .
S2 S 0.22155(8) -0.33796(14) 0.51255(6) 0.0482(3) Uani 1 1 d . . .
P1 P 0.16955(7) -0.26182(13) 0.40838(6) 0.0361(2) Uani 1 1 d . . .
S1 S 0.07195(8) -0.37887(15) 0.33473(6) 0.0539(3) Uani 1 1 d . . .
S6 S 0.43214(8) 0.11378(15) 0.15033(6) 0.0511(3) Uani 1 1 d . . .
N1 N 0.1127(2) -0.0506(4) 0.41997(16) 0.0345(7) Uani 1 1 d . . .
N2 N 0.3923(2) 0.2313(4) 0.31011(15) 0.0316(7) Uani 1 1 d . . .
C1 C 0.0328(3) 0.0058(6) 0.3705(2) 0.0470(10) Uani 1 1 d . . .
H1 H 0.0025 -0.0633 0.3290 0.056 Uiso 1 1 calc R . .
C10 C 0.4804(3) 0.1492(5) 0.3340(2) 0.0381(9) Uani 1 1 d . . .
H10 H 0.5140 0.0893 0.2972 0.046 Uiso 1 1 calc R . .
C9 C 0.5229(3) 0.1499(5) 0.4102(2) 0.0484(11) Uani 1 1 d . . .
H9 H 0.5849 0.0895 0.4266 0.058 Uiso 1 1 calc R . .
C7 C 0.3854(3) 0.3234(6) 0.4382(2) 0.0507(11) Uani 1 1 d . . .
H7 H 0.3514 0.3854 0.4741 0.061 Uiso 1 1 calc R . .
C8 C 0.4751(3) 0.2389(6) 0.4632(2) 0.0509(11) Uani 1 1 d . . .
H8 H 0.5040 0.2416 0.5165 0.061 Uiso 1 1 calc R . .
C6 C 0.3449(3) 0.3182(5) 0.3613(2) 0.0414(9) Uani 1 1 d . . .
H6 H 0.2825 0.3768 0.3440 0.050 Uiso 1 1 calc R . .
C2 C -0.0058(3) 0.1627(6) 0.3791(3) 0.0593(12) Uani 1 1 d . . .
H2 H -0.0620 0.2026 0.3432 0.071 Uiso 1 1 calc R . .
C5 C 0.1545(3) 0.0473(5) 0.4792(2) 0.0487(10) Uani 1 1 d . . .
H5 H 0.2110 0.0065 0.5146 0.058 Uiso 1 1 calc R . .
C3 C 0.0361(3) 0.2618(6) 0.4391(3) 0.0543(11) Uani 1 1 d . . .
H3 H 0.0088 0.3700 0.4456 0.065 Uiso 1 1 calc R . .
C4 C 0.1173(3) 0.2040(6) 0.4896(3) 0.0565(11) Uani 1 1 d . . .
H4 H 0.1479 0.2716 0.5316 0.068 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
P2 0.0351(5) 0.0416(6) 0.0274(5) 0.0036(4) 0.0020(4) -0.0027(4)
S5 0.0328(5) 0.0567(7) 0.0444(6) 0.0067(5) 0.0005(4) -0.0083(4)
S3 0.0329(5) 0.0491(7) 0.0519(6) 0.0091(5) 0.0095(4) 0.0011(4)
S7 0.0621(7) 0.0442(7) 0.0468(6) 0.0130(5) -0.0041(5) 0.0042(5)
S4 0.0700(7) 0.0426(6) 0.0461(6) -0.0035(5) 0.0195(5) -0.0089(5)
S2 0.0520(6) 0.0490(7) 0.0425(6) 0.0100(5) 0.0027(5) 0.0096(5)
P1 0.0338(5) 0.0363(6) 0.0385(5) 0.0032(4) 0.0065(4) -0.0008(4)
S1 0.0557(7) 0.0545(7) 0.0503(7) -0.0052(5) 0.0024(5) -0.0168(5)
S6 0.0524(6) 0.0713(8) 0.0321(5) -0.0028(5) 0.0148(4) 0.0000(5)
N1 0.0307(15) 0.0364(19) 0.0370(18) 0.0063(15) 0.0062(13) 0.0025(13)
N2 0.0310(15) 0.0389(18) 0.0245(15) 0.0007(13) 0.0026(12) 0.0024(13)
C1 0.043(2) 0.056(3) 0.040(2) 0.004(2) -0.0008(18) 0.009(2)
C10 0.0332(19) 0.043(2) 0.038(2) -0.0025(18) 0.0037(16) 0.0032(17)
C9 0.039(2) 0.066(3) 0.036(2) -0.004(2) -0.0095(17) 0.015(2)
C7 0.056(3) 0.065(3) 0.032(2) -0.009(2) 0.0067(19) 0.011(2)
C8 0.055(3) 0.062(3) 0.032(2) -0.006(2) -0.0056(18) 0.006(2)
C6 0.038(2) 0.048(3) 0.039(2) -0.0004(18) 0.0069(17) 0.0085(18)
C2 0.054(3) 0.067(3) 0.056(3) 0.016(3) 0.004(2) 0.018(2)
C5 0.051(2) 0.046(3) 0.047(2) -0.002(2) -0.003(2) 0.001(2)
C3 0.064(3) 0.047(3) 0.057(3) 0.011(2) 0.026(2) 0.011(2)
C4 0.066(3) 0.047(3) 0.057(3) -0.008(2) 0.005(2) 0.004(2)

_geom_special_details            
;
All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell s.u.'s are taken
into account individually in the estimation of s.u.'s in distances, angles
and torsion angles; correlations between s.u.'s in cell parameters are
only
used when they are defined by crystal symmetry. An approximate
(isotropic)
treatment of cell s.u.'s is used for estimating s.u.'s 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
P2 N2 1.864(3) . ?
P2 S6 1.9239(14) . ?
P2 S7 1.9399(15) . ?
P2 S5 2.1121(13) . ?
S5 S4 2.0416(16) . ?
S3 S4 2.0633(16) . ?
S3 P1 2.1252(13) . ?
S2 P1 1.9398(15) . ?
P1 N1 1.869(3) . ?
P1 S1 1.9203(15) . ?
N1 C1 1.335(5) . ?
N1 C5 1.348(5) . ?
N2 C10 1.339(4) . ?
N2 C6 1.342(4) . ?
C1 C2 1.370(6) . ?
C1 H1 0.9500 . ?
C10 C9 1.361(5) . ?
C10 H10 0.9500 . ?
C9 C8 1.375(5) . ?
C9 H9 0.9500 . ?
C7 C6 1.365(5) . ?
C7 C8 1.369(5) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C6 H6 0.9500 . ?
C2 C3 1.363(6) . ?
C2 H2 0.9500 . ?
C5 C4 1.366(6) . ?
C5 H5 0.9500 . ?
C3 C4 1.360(6) . ?
C3 H3 0.9500 . ?
C4 H4 0.9500 . ?

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
N2 P2 S6 106.45(10) . . ?
N2 P2 S7 106.31(11) . . ?
S6 P2 S7 125.51(7) . . ?
N2 P2 S5 97.11(10) . . ?
S6 P2 S5 114.51(7) . . ?
S7 P2 S5 103.11(6) . . ?
S4 S5 P2 104.60(6) . . ?
S4 S3 P1 106.16(6) . . ?
S5 S4 S3 107.60(6) . . ?
N1 P1 S1 106.19(11) . . ?
N1 P1 S2 106.18(10) . . ?
S1 P1 S2 125.59(7) . . ?
N1 P1 S3 98.21(10) . . ?
S1 P1 S3 113.79(6) . . ?
S2 P1 S3 103.35(6) . . ?
C1 N1 C5 119.4(4) . . ?
C1 N1 P1 121.5(3) . . ?
C5 N1 P1 119.0(3) . . ?
C10 N2 C6 120.0(3) . . ?
C10 N2 P2 120.5(2) . . ?
C6 N2 P2 119.5(2) . . ?
N1 C1 C2 120.4(4) . . ?
N1 C1 H1 119.8 . . ?
C2 C1 H1 119.8 . . ?
N2 C10 C9 121.2(3) . . ?
N2 C10 H10 119.4 . . ?
C9 C10 H10 119.4 . . ?
C10 C9 C8 119.3(4) . . ?
C10 C9 H9 120.4 . . ?
C8 C9 H9 120.3 . . ?
C6 C7 C8 119.7(4) . . ?
C6 C7 H7 120.1 . . ?
C8 C7 H7 120.1 . . ?
C7 C8 C9 119.1(4) . . ?
C7 C8 H8 120.4 . . ?
C9 C8 H8 120.4 . . ?
N2 C6 C7 120.6(3) . . ?
N2 C6 H6 119.7 . . ?
C7 C6 H6 119.7 . . ?
C3 C2 C1 120.3(4) . . ?
C3 C2 H2 119.9 . . ?
C1 C2 H2 119.9 . . ?
N1 C5 C4 121.5(4) . . ?
N1 C5 H5 119.2 . . ?
C4 C5 H5 119.2 . . ?
C4 C3 C2 119.3(4) . . ?
C4 C3 H3 120.4 . . ?
C2 C3 H3 120.4 . . ?
C3 C4 C5 119.1(4) . . ?
C3 C4 H4 120.5 . . ?
C5 C4 H4 120.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 P2 S5 S4 -74.15(11) . . . . ?
S6 P2 S5 S4 37.60(8) . . . . ?
S7 P2 S5 S4 177.21(6) . . . . ?
P2 S5 S4 S3 90.88(7) . . . . ?
P1 S3 S4 S5 84.89(7) . . . . ?
S4 S3 P1 N1 -85.75(11) . . . . ?
S4 S3 P1 S1 26.06(9) . . . . ?
S4 S3 P1 S2 165.37(6) . . . . ?
S1 P1 N1 C1 -13.6(3) . . . . ?
S2 P1 N1 C1 -149.2(3) . . . . ?
S3 P1 N1 C1 104.2(3) . . . . ?
S1 P1 N1 C5 167.2(3) . . . . ?
S2 P1 N1 C5 31.5(3) . . . . ?
S3 P1 N1 C5 -75.0(3) . . . . ?
S6 P2 N2 C10 -9.7(3) . . . . ?
S7 P2 N2 C10 -145.5(3) . . . . ?
S5 P2 N2 C10 108.6(3) . . . . ?
S6 P2 N2 C6 172.1(3) . . . . ?
S7 P2 N2 C6 36.2(3) . . . . ?
S5 P2 N2 C6 -69.7(3) . . . . ?
C5 N1 C1 C2 0.9(5) . . . . ?
P1 N1 C1 C2 -178.4(3) . . . . ?
C6 N2 C10 C9 0.9(6) . . . . ?
P2 N2 C10 C9 -177.3(3) . . . . ?
N2 C10 C9 C8 -1.1(6) . . . . ?
C6 C7 C8 C9 0.0(7) . . . . ?
C10 C9 C8 C7 0.6(7) . . . . ?
C10 N2 C6 C7 -0.3(6) . . . . ?
P2 N2 C6 C7 177.9(3) . . . . ?
C8 C7 C6 N2 -0.1(6) . . . . ?
N1 C1 C2 C3 -1.0(6) . . . . ?
C1 N1 C5 C4 -0.5(6) . . . . ?
P1 N1 C5 C4 178.8(3) . . . . ?
C1 C2 C3 C4 0.8(6) . . . . ?
C2 C3 C4 C5 -0.5(6) . . . . ?
N1 C5 C4 C3 0.3(6) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.29
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.375
_refine_diff_density_min         -0.455
_refine_diff_density_rms         0.071

#===END