# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2011


data_global
_journal_name_full               'Dalton Trans.'
_journal_coden_cambridge         0222
_publ_contact_author_name        'R.T. Boere'
_publ_contact_author_address     
;
Department of Chemistry and Biochemistry
University of Lethbridge
Lethbridge, AB Canada
T1K 3M4
;
_publ_contact_author_email       boere@uleth.ca
_publ_contact_author_phone       +1-403-329-2045
_publ_contact_author_fax         +1-403-329-2057
_publ_author_address             
;
Department of Chemistry and Biochemistry
University of Lethbridge
Lethbridge, AB Canada
T1K 3M4
;
loop_
_publ_author_name
R.T.Boere
'Ken Wong'
'Klaus Moock'

data_H2C2N4S2
_database_code_depnum_ccdc_archive 'CCDC 836600'
#TrackingRef '- Dalton01.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
1,5,2,4,6,8-dithiatetrazocine
;
_chemical_name_common            1,5,2,4,6,8-dithiatetrazocine
_chemical_melting_point          393
_chemical_formula_moiety         'C2 H2 N4 S2'
_chemical_formula_sum            'C2 H2 N4 S2'
_chemical_formula_weight         146.20
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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pbca
_symmetry_int_tables_number      61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'

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

_cell_length_a                   5.979(3)
_cell_length_b                   7.217(3)
_cell_length_c                   12.281(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     530.0(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    2599
_cell_measurement_theta_min      3.31
_cell_measurement_theta_max      28.37
_exptl_crystal_description       Plate
_exptl_crystal_colour            Yellow
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.08
_exptl_crystal_density_diffrn    1.832
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             296
_exptl_absorpt_coefficient_mu    0.880
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5724
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   
;
SADABS (Bruker, 2008)
;
_exptl_special_details           
;
A crystal coated in Paratone (TM) oil was mounted on the end of a thin glass
capillary and cooled in the gas stream of the diffractometer Kryoflex device.
;
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0.00 1.00 -1.00 0.0600
1.00 1.00 2.00 0.0600
2.00 2.00 1.00 0.0700
-2.00 -2.00 -1.00 0.0900
-1.00 -2.00 1.00 0.0800
1.00 2.00 -1.00 0.0700
-1.00 -2.00 2.00 0.0800
-2.00 1.00 0.00 0.0800
2.00 -1.00 -2.00 0.0800
-1.00 2.00 1.00 0.0600
0.00 -1.00 0.00 0.0900
0.00 1.00 0.00 0.0600
0.00 0.00 1.00 0.0300
0.00 0.00 -1.00 0.0300

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Bruker D8'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  
;
Bruker ApexII CCD area-detector diffractometer
;
_diffrn_measurement_method       'phi and omega scans'
_diffrn_reflns_number            5237
_diffrn_reflns_av_R_equivalents  0.0551
_diffrn_reflns_av_sigmaI/netI    0.0295
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.32
_diffrn_reflns_theta_max         27.54
_reflns_number_total             609
_reflns_number_gt                505
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker, 2006)'
_computing_cell_refinement       'SAINT-Plus (Bruker, 2006)'
_computing_data_reduction        SAINT-Plus
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
# if use Dual Space, write: 'SHELXD (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_molecular_graphics    'Mercury (Macrae <i>et al.</i>, 2006)'
_computing_publication_material  'publCIF (Westrip, 2007)'
# Bruker (2008). APEX2, SAINT-Plus and SADABS. Bruker AXS Inc., Madison
# Wisconsin, USA.
# Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
# Macrae, D. F., Edgington, P. R., McCabe, P., Pidcock, E., Shields, G. P.,
# Taylor, R., Towler, M. & van de Streek, J. (2006). J. Appl. Cryst. 39,
# 453-457.
# Westrip, S. J. (2009). publCIF. In preparation.

_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^)+(0.0628P)^2^+0.1620P] 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_number_reflns         609
_refine_ls_number_parameters     50
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0481
_refine_ls_R_factor_gt           0.0389
_refine_ls_wR_factor_ref         0.1117
_refine_ls_wR_factor_gt          0.1042
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_restrained_S_all      1.109
_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
S1 S 0.1969(6) 0.3961(5) -0.1058(3) 0.0320(4) Uani 0.75 1 d P A 1
N1 N -0.0137(14) 0.5047(16) -0.1518(8) 0.0301(11) Uani 0.75 1 d P . 1
N2 N 0.2612(7) 0.3608(5) 0.0165(2) 0.0305(7) Uani 0.75 1 d P A 1
C1 C 0.177(3) 0.406(3) 0.1105(19) 0.0321(9) Uani 0.75 1 d P . 1
H1 H 0.2664 0.3547 0.1670 0.039 Uiso 0.75 1 calc PR . 1
S2 S 0.200(2) 0.3989(19) 0.1099(14) 0.0321(9) Uani 0.25 1 d P . 2
N3 N 0.024(5) 0.494(5) -0.141(3) 0.0301(11) Uani 0.25 1 d PD . 2
N4 N 0.249(3) 0.376(2) -0.0163(10) 0.0305(7) Uani 0.25 1 d PD B 2
C2 C 0.180(8) 0.404(7) -0.108(4) 0.0320(4) Uani 0.25 1 d PD B 2
H2 H 0.2651 0.3450 -0.1635 0.038 Uiso 0.25 1 calc PR B 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
S1 0.0290(8) 0.0332(6) 0.0337(5) -0.0010(3) 0.0083(4) 0.0041(5)
N1 0.034(3) 0.0327(17) 0.024(2) 0.0016(14) -0.0062(17) -0.002(2)
N2 0.0242(10) 0.0307(12) 0.037(2) 0.0091(14) -0.0073(16) 0.0033(9)
C1 0.027(3) 0.0338(10) 0.0357(7) 0.0022(7) -0.0119(15) 0.0039(13)
S2 0.027(3) 0.0338(10) 0.0357(7) 0.0022(7) -0.0119(15) 0.0039(13)
N3 0.034(3) 0.0327(17) 0.024(2) 0.0016(14) -0.0062(17) -0.002(2)
N4 0.0242(10) 0.0307(12) 0.037(2) 0.0091(14) -0.0073(16) 0.0033(9)
C2 0.0290(8) 0.0332(6) 0.0337(5) -0.0010(3) 0.0083(4) 0.0041(5)

_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
S1 N2 1.571(4) . ?
S1 N1 1.588(6) . ?
N1 C1 1.28(2) 5_565 ?
N2 C1 1.30(2) . ?
C1 H1 0.9500 . ?
S2 N4 1.59(2) . ?
S2 N3 1.59(4) 5_565 ?
N3 C2 1.21(3) . ?
N4 C2 1.22(3) . ?
C2 H2 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 S1 N1 127.9(6) . . ?
C1 N1 S1 135.7(13) 5_565 . ?
C1 N2 S1 135.6(10) . . ?
N1 C1 N2 141(2) 5_565 . ?
N1 C1 H1 109.6 5_565 . ?
N2 C1 H1 109.6 . . ?
N4 S2 N3 116.2(16) . 5_565 ?
C2 N3 S2 146(4) . 5_565 ?
C2 N4 S2 146(3) . . ?
N3 C2 N4 131(6) . . ?
N3 C2 H2 114.3 . . ?
N4 C2 H2 114.3 . . ?

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 S1 N1 C1 3(2) . . . 5_565 ?
N1 S1 N2 C1 -1.3(13) . . . . ?
S1 N2 C1 N1 -1(3) . . . 5_565 ?
N3 S2 N4 C2 -3(5) 5_565 . . . ?
S2 N3 C2 N4 -12(12) 5_565 . . . ?
S2 N4 C2 N3 9(9) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.25
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.440
_refine_diff_density_min         -0.337
_refine_diff_density_rms         0.087
_iucr_refine_instruction_details 
;
TITL C2H2N4S2 in Pbca
CELL 0.71073 5.9794 7.2174 12.2812 90.000 90.000 90.000
ZERR 4.00 0.0026 0.0032 0.0054 0.000 0.000 0.000
LATT 1
SYMM 0.5-X, -Y, 0.5+Z
SYMM -X, 0.5+Y, 0.5-Z
SYMM 0.5+X, 0.5-Y, -Z
SFAC C H N S
UNIT 8 8 16 8
SIZE 0.08 0.18 0.20
TEMP -100
EADP S1 C2
EADP S2 C1
SADI 0.01 N3 C2 N4 C2
EADP N1 N3
EADP N2 N4
L.S. 12
MPLA 5 S1 N1 N2 C1 H1
BOND $H
ACTA 50.5
CONF
WGHT 0.062800 0.162000
FVAR 0.23172
PART 1
S1 4 0.196948 0.396064 -0.105848 10.75000 0.02900 0.03323 =
0.03372 -0.00103 0.00834 0.00412
N1 3 -0.013697 0.504736 -0.151806 10.75000 0.03412 0.03266 =
0.02354 0.00160 -0.00620 -0.00198
N2 3 0.261163 0.360842 0.016457 10.75000 0.02421 0.03066 =
0.03674 0.00911 -0.00728 0.00328
C1 1 0.176956 0.405559 0.110454 10.75000 0.02680 0.03380 =
0.03572 0.00224 -0.01195 0.00386
AFIX 43
H1 2 0.266359 0.354743 0.166997 10.75000 -1.20000
AFIX 0
PART 2
S2 4 0.199945 0.398880 0.109931 10.25000 0.02680 0.03380 =
0.03572 0.00224 -0.01195 0.00386
N3 3 0.023543 0.493983 -0.141451 10.25000 0.03412 0.03266 =
0.02354 0.00160 -0.00620 -0.00198
N4 3 0.248559 0.376179 -0.016326 10.25000 0.02421 0.03066 =
0.03674 0.00911 -0.00728 0.00328
C2 1 0.180324 0.404142 -0.108068 10.25000 0.02900 0.03323 =
0.03372 -0.00103 0.00834 0.00412
AFIX 43
H2 2 0.265058 0.344987 -0.163504 10.25000 -1.20000
PART 0
HKLF 4
END
;

data_S4N4
_database_code_depnum_ccdc_archive 'CCDC 836601'
#TrackingRef '- Dalton01.cif'

# Results very similar to the re-determination at 100 K reported by
# W. Scherer e.a., Chemm. Commun. (2000), 635.

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
tetranitrogen tetrasulfide
;
_chemical_name_common            'tetranitrogen tetrasulfide'
_chemical_melting_point          ?
_chemical_formula_moiety         'N4 S4'
_chemical_formula_sum            'N4 S4'
_chemical_formula_weight         184.28

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/n
_symmetry_int_tables_number      14
_symmetry_space_group_name_Hall  -P2yn

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                   8.647(3)
_cell_length_b                   7.101(3)
_cell_length_c                   8.732(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.402(4)
_cell_angle_gamma                90.00
_cell_volume                     535.2(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    2555
_cell_measurement_theta_min      3.22
_cell_measurement_theta_max      27.44
_exptl_crystal_recrystallization_method 'Slow cooling'
_diffrn_ambient_pressure         101
_exptl_crystal_description       Needle
_exptl_crystal_colour            Yellow
_exptl_crystal_size_max          0.287
_exptl_crystal_size_mid          0.095
_exptl_crystal_size_min          0.030
_exptl_crystal_density_diffrn    2.287
_exptl_crystal_F_000             368
_exptl_absorpt_coefficient_mu    1.649
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.610
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_process_details   
;
SADABS (Bruker, 2006)
;
_exptl_special_details           
;
A crystal coated in Paratone (TM) oil was mounted on the end of a thin glass
capillary and cooled in the gas stream of the diffractometer Kryoflex device.
;
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Bruker D8'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  
;
Bruker ApexII CCD area-detector diffractometer
;
_diffrn_measurement_method       'phi and omega scans'
_diffrn_reflns_number            5966
_diffrn_reflns_av_R_equivalents  0.0561
_diffrn_reflns_av_sigmaI/netI    0.0517
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         3.22
_diffrn_reflns_theta_max         27.48
_reflns_number_total             1228
_reflns_number_gt                958
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'APEX2 (Bruker, 2006)'
_computing_cell_refinement       'SAINT-Plus (Bruker, 2006)'
_computing_data_reduction        SAINT-Plus
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
# if use Dual Space, write: 'SHELXD (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_molecular_graphics    'Mercury (Macrae <i>et al.</i>, 2006)'
_computing_publication_material  'publCIF (Westrip, 2007)'
# Bruker (2006). APEX2, SAINT-Plus and SADABS. Bruker AXS Inc., Madison
# Wisconsin, USA.
# Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
# Macrae, D. F., Edgington, P. R., McCabe, P., Pidcock, E., Shields, G. P.,
# Taylor, R., Towler, M. & van de Streek, J. (2006). J. Appl. Cryst. 39,
# 453-457.
# Westrip, S. P. (2010). J. Appl. Cryst. 43, 920-925.
_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^)+(0.0241P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_number_reflns         1228
_refine_ls_number_parameters     73
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0299
_refine_ls_wR_factor_ref         0.0611
_refine_ls_wR_factor_gt          0.0580
_refine_ls_goodness_of_fit_ref   0.941
_refine_ls_restrained_S_all      0.941
_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
S1 S 0.59822(8) 0.20860(10) 1.15140(8) 0.02104(18) Uani 1 1 d . . .
S3 S 0.55930(8) 0.29842(10) 0.85055(8) 0.02218(18) Uani 1 1 d . . .
S2 S 0.77366(8) 0.04704(10) 0.95985(8) 0.02674(19) Uani 1 1 d . . .
S4 S 0.80358(8) 0.42187(10) 1.00614(8) 0.02741(19) Uani 1 1 d . . .
N1 N 0.7178(3) 0.3838(3) 1.1648(2) 0.0249(6) Uani 1 1 d . . .
N2 N 0.8921(3) 0.2242(3) 0.9741(3) 0.0307(6) Uani 1 1 d . . .
N3 N 0.6494(3) 0.1043(3) 0.8190(2) 0.0249(6) Uani 1 1 d . . .
N4 N 0.4759(3) 0.2631(3) 1.0097(2) 0.0213(5) 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
S1 0.0246(4) 0.0226(4) 0.0160(3) 0.0031(3) 0.0011(3) -0.0014(3)
S3 0.0267(4) 0.0228(4) 0.0167(4) 0.0029(3) -0.0010(3) -0.0002(3)
S2 0.0250(4) 0.0276(4) 0.0277(4) -0.0014(3) 0.0019(3) 0.0055(3)
S4 0.0280(4) 0.0296(4) 0.0246(4) 0.0000(3) 0.0010(3) -0.0123(3)
N1 0.0317(14) 0.0257(13) 0.0169(12) -0.0016(10) -0.0010(10) -0.0076(11)
N2 0.0183(13) 0.0408(16) 0.0333(15) 0.0009(12) 0.0045(11) -0.0025(11)
N3 0.0314(14) 0.0233(13) 0.0197(12) -0.0056(10) -0.0002(11) 0.0013(11)
N4 0.0201(12) 0.0218(13) 0.0222(13) 0.0032(10) 0.0025(10) 0.0000(10)

_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
S1 N1 1.617(2) . ?
S1 N4 1.626(2) . ?
S3 N3 1.615(2) . ?
S3 N4 1.623(2) . ?
S2 N2 1.622(2) . ?
S2 N3 1.636(2) . ?
S4 N2 1.631(3) . ?
S4 N1 1.632(2) . ?

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
N1 S1 N4 104.83(12) . . ?
N3 S3 N4 104.91(12) . . ?
N2 S2 N3 104.39(13) . . ?
N2 S4 N1 104.18(12) . . ?
S1 N1 S4 112.76(13) . . ?
S2 N2 S4 112.31(14) . . ?
S3 N3 S2 112.71(13) . . ?
S3 N4 S1 112.72(14) . . ?

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
N4 S1 N1 S4 -57.71(16) . . . . ?
N2 S4 N1 S1 -58.69(17) . . . . ?
N3 S2 N2 S4 58.11(17) . . . . ?
N1 S4 N2 S2 58.16(17) . . . . ?
N4 S3 N3 S2 -57.74(16) . . . . ?
N2 S2 N3 S3 -58.85(17) . . . . ?
N3 S3 N4 S1 58.07(15) . . . . ?
N1 S1 N4 S3 58.14(16) . . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.25
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.333
_refine_diff_density_min         -0.394
_refine_diff_density_rms         0.081
_iucr_refine_instruction_details 
;
TITL S4N4 from H-8MR synthesis in P2(1)/n
CELL 0.71073 8.6469 7.1006 8.7323 90.000 93.402 90.000
ZERR 4.00 0.0031 0.0025 0.0031 0.000 0.004 0.000
LATT 1
SYMM 0.5-X, 0.5+Y, 0.5-Z
SFAC N S
UNIT 16 16
L.S. 18
BOND
CONF
ACTA 50.5
MPLA 4 S1 > S4
MPLA 4 N1 > N4
FMAP 2
PLAN 5
TEMP -100.000
WGHT 0.024100
FVAR 0.57262
S1 2 0.598220 0.208597 1.151404 11.00000 0.02455 0.02259 =
0.01598 0.00310 0.00114 -0.00142
S3 2 0.559298 0.298420 0.850554 11.00000 0.02673 0.02284 =
0.01670 0.00294 -0.00095 -0.00020
S2 2 0.773662 0.047040 0.959846 11.00000 0.02502 0.02755 =
0.02770 -0.00145 0.00194 0.00550
S4 2 0.803575 0.421865 1.006142 11.00000 0.02804 0.02957 =
0.02455 0.00003 0.00104 -0.01233
N1 1 0.717775 0.383812 1.164764 11.00000 0.03173 0.02573 =
0.01690 -0.00162 -0.00098 -0.00757
N2 1 0.892119 0.224151 0.974051 11.00000 0.01827 0.04081 =
0.03331 0.00088 0.00446 -0.00245
N3 1 0.649352 0.104298 0.819049 11.00000 0.03143 0.02327 =
0.01967 -0.00564 -0.00019 0.00130
N4 1 0.475881 0.263088 1.009706 11.00000 0.02005 0.02182 =
0.02223 0.00324 0.00249 -0.00002
HKLF 4
END
;