# Supplementary Material (ESI) for ChemComm
# This journal is © The Royal Society of Chemistry 2000
# CCDC Number: 182/1565
# CIF-file generated for S4N4
#==============================================================================
data_global
#==============================================================================
# 0. AUDIT DETAILS
_audit_creation_date 'Thu Oct 14 09:39:32 1999'
_audit_creation_method 'PLATON
option'
_audit_update_record
;
26-Nov-99 Updated by the Author M.S.
;
#===============================================================================
# 1. SUBMISSION DETAILS
_publ_contact_author_name # Name of author for correspondence
;
Wolfgang Scherer
;
_publ_contact_author_address # address of author for correspondence
;
Anorganisch-chemisches Institut der
Technischen Universit\"at M\"unchen
Lichtenbergstrasse 4
D-85747 Garching bei M\"unchen
;
_publ_contact_author_email 'wolfgang.scherer@ch.tum.de'
_publ_contact_author_fax '089 289 13473'
_publ_contact_author_phone '089 289 14378'
_publ_requested_journal 'Chem.Comm.'
# Publication choise FI FM FO CI CM CO AD
_publ_requested_category ?
_publ_requested_coeditor_name ?
_publ_contact_letter # Include date of submission
;
Date of submission ?
;
#===============================================================================
# 2. PROCESSING SUMMARY (JOURNAL OFFICE ONLY)
_journal_date_recd_electronic ?
_journal_date_to_coeditor ?
_journal_date_from_coeditor ?
_journal_date_accepted ?
_journal_date_printers_first ?
_journal_date_printers_final ?
_journal_date_proofs_out ?
_journal_date_proofs_in ?
_journal_coeditor_name ?
_journal_coeditor_code ?
_journal_coeditor_notes
; ?
;
_journal_techeditor_code ?
_journal_techeditor_notes
; ?
;
_journal_coden_ASTM ?
_journal_name_full ?
_journal_year ?
_journal_volume ?
_journal_issue ?
_journal_page_first ?
_journal_page_last ?
_journal_suppl_publ_number ?
_journal_suppl_publ_pages ?
#===============================================================================
# 3. TITLE AND AUTHOR LIST
_publ_section_title
;
Molecular Recognition in the Solid State: Topology of Experimental and
Theoretical Charge Densities for S4N4
;
loop_
_publ_author_name
_publ_author_address
'Scherer W.'
;
Anorganisch-chemisches Institut der
Technischen Universit\"at M\"unchen
Lichtenbergstrasse 4
D-85747 Garching bei M\"unchen
;
'Spiegler M.'
;
Anorganisch-chemisches Institut der
Technischen Universit\"at M\"unchen
Lichtenbergstrasse 4
D-85747 Garching bei M\"unchen
;
'Pedersen B.'
;
Anorganisch-chemisches Institut der
Technischen Universit\"at M\"unchen
Lichtenbergstrasse 4
D-85747 Garching bei M\"unchen
;
'Tafipolsky M.'
;
Anorganisch-chemisches Institut der
Technischen Universit\"at M\"unchen
Lichtenbergstrasse 4
D-85747 Garching bei M\"unchen
;
'Hieringer W.'
;
Anorganisch-chemisches Institut der
Technischen Universit\"at M\"unchen
Lichtenbergstrasse 4
D-85747 Garching bei M\"unchen
;
'Reinhard B.'
;
Anorganisch-chemisches Institut der
Technischen Universit\"at M\"unchen
Lichtenbergstrasse 4
D-85747 Garching bei M\"unchen
;
'Mc Grady G. S.'
;
Department of Chemistry
King's College London
Strand
London, WC2R 2LS, UK
;
'Downs A. J.'
;
Inorganic Chemistry Laboratory
University of Oxford
South Parks Road
Oxford, OXI 3 QR, UK
;
# The loop structure below should contain the names and adresses of all
# authors, in the required order of publication. Repeat as necessary.
#===============================================================================
# 4. TEXT
_publ_section_synopsis
;
?
;
_publ_section_abstract
;
?
;
# Insert blank lines between paragraphs
_publ_section_comment
;
?
;
_publ_section_exptl_prep
;
?
;
_publ_section_exptl_refinement
;
?
;
# Insert blank lines between references
_publ_section_references
;
Blessing R. H., Cryst. Rev., 1987, 1, 3-57
;
_publ_section_figure_captions
;
?
;
_publ_section_acknowledgements
; View of the title compound with the atom numbering scheme
Displacement ellipsoids for non-H atoms are drawn at the 50% probability level
;
#===============================================================================
data_s4n4
#===============================================================================
# 5. CHEMICAL DATA
_chemical_name_systematic
;
Tetrasulfur tetranitride
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety
'N4 S4'
_chemical_formula_structural ?
_chemical_formula_sum
'N4 S4'
_chemical_formula_weight 184.32
_chemical_compound_source 'see text'
#===============================================================================
# 6. CRYSTAL DATA
_symmetry_cell_setting Monoclinic
_symmetry_space_group_name_Hall '-P 2yn'
_symmetry_space_group_name_H-M 'P 21/n'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
1/2-x,1/2+y,1/2-z
-x,-y,-z
1/2+x,1/2-y,1/2+z
_cell_length_a 8.7286(4)
_cell_length_b 7.0783(4)
_cell_length_c 8.6377(4)
_cell_angle_alpha 90
_cell_angle_beta 93.7219(18)
_cell_angle_gamma 90
_cell_volume 532.54(5)
_cell_formula_units_Z 4
_cell_measurement_temperature 100
_cell_measurement_reflns_used 30199
_cell_measurement_theta_min ?
_cell_measurement_theta_max ?
_cell_special_details
; ?
;
# values of the second crystal are included as remarks (#)
_exptl_crystal_description 'prism'
_exptl_crystal_colour 'orange'
_exptl_crystal_size_max 0.35 # 0.35
_exptl_crystal_size_mid 0.25 # 0.23
_exptl_crystal_size_min 0.20 # 0.20
_exptl_crystal_size_rad ?
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 2.299
_exptl_crystal_density_method 'Not Measured'
_exptl_crystal_F_000 368
_exptl_absorpt_coefficient_mu 1.66
_exptl_crystal_density_meas_temp ?
_exptl_absorpt_correction_type 'semiempirical'
_exptl_absorpt_process_details 'SORTAV (Blessing)'
_exptl_absorpt_correction_T_min 0.525 # 0.563
_exptl_absorpt_correction_T_max 0.647 # 0.681
#===============================================================================
# 7. EXPERIMENTAL DATA
_exptl_special_details
; ?
;
_diffrn_ambient_temperature 100
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_source 'FR591 rotating anode (Nonius)'
_diffrn_radiation_monochromator 'graphite'
_diffrn_measurement_device_type 'KappaCCD'
_diffrn_measurement_method 'CCD'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
? ? ?
# number of measured reflections (redundant set)
_diffrn_reflns_number 30199 # 22404
_diffrn_reflns_av_R_equivalents 0.0228
_diffrn_reflns_av_sigmaI/netI 0.0403
_diffrn_reflns_limit_h_min -19
_diffrn_reflns_limit_h_max 19
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_theta_min 3.22
_diffrn_reflns_theta_max 52.15
_diffrn_reflns_theta_full ?
_diffrn_measured_fraction_theta_max ?
_diffrn_measured_fraction_theta_full ?
_diffrn_reflns_reduction_process
;
?
;
# number of unique reflections
_reflns_number_total 6108
# number of observed reflections (> n sig(I))
_reflns_number_gt 4849
_reflns_threshold_expression >3sigma(i)
_computing_data_collection 'Collect (Nonius)'
_computing_cell_refinement 'Scalepack (HKL)'
_computing_data_reduction 'Denzo (Nonius)'
_computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement 'XD (Koritsanszky et al, 1995)'
_computing_molecular_graphics 'PLATON (Spek, 1990)'
_computing_publication_material 'PLATON (Spek, 1990)'
#===============================================================================
# 8. REFINEMENT DATA
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme 'calc w=1/[\'
_refine_ls_weighting_details
?
_refine_ls_hydrogen_treatment ?
_refine_ls_extinction_method none
_refine_ls_abs_structure_details none
_refine_ls_number_reflns 4849
_refine_ls_number_parameters 105
_refine_ls_number_restraints ?
_refine_ls_number_constraints ?
_refine_ls_R_factor_all 0.040
_refine_ls_R_factor_gt 0.025
_refine_ls_R_Fsqd_factor_ref 0.035
_refine_ls_R_Fsqd_factor_gt 0.033
_refine_ls_goodness_of_fit_ref 1.628
_refine_ls_restrained_S_all ?
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_diff_density_max 0.256 #sint/l<=0.8
_refine_diff_density_min -0.261 #sint/l<=0.8
_refine_diff_density_rms 0.088 #sint/l<=0.8
#===============================================================================
# 9. ATOMIC COORDINATES AND THERMAL PARAMETERS
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_thermal_displace_type
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_U_iso_or_equiv
S1 S Uani 0.00474(2) 0.92129(3) 0.30497(2) 1.000 0.0152(1)
S2 S Uani 0.15182(2) 0.70830(2) 0.09953(2) 1.000 0.0117(1)
S3 S Uani -0.14978(2) 0.79953(3) 0.05749(2) 1.000 0.0123(1)
S4 S Uani -0.04133(2) 0.54467(3) 0.27227(2) 1.000 0.0148(1)
N1 N Uani 0.01023(7) 0.76476(9) -0.02496(6) 1.000 0.0128(1)
N2 N Uani -0.02796(8) 0.72214(11) 0.39194(7) 1.000 0.0181(1)
N3 N Uani -0.18191(7) 0.60332(10) 0.14674(8) 1.000 0.0150(1)
N4 N Uani 0.16413(7) 0.88368(9) 0.22051(8) 1.000 0.0153(1)
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 0.0136(1) 0.0173(1) 0.0148(1) -0.0068(1) 0.0011(1) 0.0001(1)
S2 0.0087(1) 0.0139(1) 0.0126(1) -0.0010(1) 0.0010(1) 0.0018(1)
S3 0.0091(1) 0.0138(1) 0.0139(1) -0.0001(1) -0.0004(1) 0.0018(1)
S4 0.0156(1) 0.0158(1) 0.0131(1) 0.0029(1) 0.0010(1) -0.0009(1)
N1 0.0123(2) 0.0152(2) 0.0109(2) 0.0001(1) 0.0008(1) 0.0022(2)
N2 0.0190(2) 0.0250(3) 0.0106(2) -0.0013(2) 0.0022(2) 0.0006(2)
N3 0.0111(2) 0.0160(2) 0.0179(2) 0.0004(2) -0.0001(2) -0.0025(2)
N4 0.0107(2) 0.0167(2) 0.0183(2) -0.0043(2) -0.0003(2) -0.0018(2)
#===============================================================================
# 10. MOLECULAR GEOMETRY
_geom_special_details
;
Bond distances, angles etc. have been calculated using the
rounded fractional coordinates. All esds are estimated
from the variances of the (full) variance-covariance matrix.
The cell esds are taken into account in the estimation of
distances, angles and torsion angles
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 N2 1.6312(8) . . yes
S1 N4 1.6342(7) . . yes
S2 N1 1.6343(6) . . yes
S2 N4 1.6217(7) . . yes
S3 N1 1.6271(6) . . yes
S3 N3 1.6217(7) . . yes
S4 N2 1.6262(7) . . yes
S4 N3 1.6374(7) . . yes
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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 S1 N4 104.14(4) . . . yes
N1 S2 N4 104.62(3) . . . yes
N1 S3 N3 104.97(3) . . . yes
N2 S4 N3 104.17(4) . . . yes
S2 N1 S3 112.51(3) . . . yes
S1 N2 S4 112.48(4) . . . yes
S3 N3 S4 112.74(4) . . . yes
S1 N4 S2 112.93(4) . . . yes
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 N2 S4 -57.99(5) . . . . no
N2 S1 N4 S2 58.53(5) . . . . no
N4 S2 N1 S3 -58.15(5) . . . . no
N1 S2 N4 S1 57.88(5) . . . . no
N3 S3 N1 S2 -57.89(5) . . . . no
N1 S3 N3 S4 57.70(5) . . . . no
N3 S4 N2 S1 -58.23(5) . . . . no
N2 S4 N3 S3 58.92(5) . . . . no
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
S1 S3 2.5994(3) . . no
S1 N1 3.0609(6) . . no
S1 N3 3.0494(7) . . no
S1 S2 3.6706(3) . 2_555 no
S1 N3 3.1507(7) . 2_455 no
S1 S1 3.5548(3) . 3_576 no
S1 N1 3.2809(6) . 3_575 no
S2 S4 2.5955(3) . . no
S2 N2 3.0604(7) . . no
S2 N3 3.0591(7) . . no
S2 S1 3.6706(3) . 2_545 no
S2 N4 3.1548(7) . 2_545 no
S2 S3 3.7381(3) . 3_575 no
S2 S4 3.7481(3) . 3_565 no
S2 N3 3.0874(7) . 3_565 no
S2 N2 3.4526(7) . 4_564 no
S3 S1 2.5994(3) . . no
S3 N2 3.0623(7) . . no
S3 N4 3.0568(7) . . no
S3 S4 3.5996(3) . 2_455 no
S3 S2 3.7381(3) . 3_575 no
S3 N1 3.3345(7) . 3_575 no
S3 N4 3.2819(7) . 3_575 no
S3 N2 3.5146(7) . 4_464 no
S3 N4 3.4898(7) . 4_464 no
S4 S2 2.5955(3) . . no
S4 N1 3.0612(6) . . no
S4 N4 3.0460(7) . . no
S4 S3 3.5996(3) . 2_445 no
S4 N4 3.4808(7) . 2_545 no
S4 S2 3.7481(3) . 3_565 no
S4 N1 3.0837(6) . 3_565 no
S4 N2 3.4810(7) . 3_566 no
N1 S1 3.0609(6) . . no
N1 S4 3.0612(6) . . no
N1 S1 3.2809(6) . 3_575 no
N1 S3 3.3345(7) . 3_575 no
N1 S4 3.0837(6) . 3_565 no
N1 N3 3.2163(9) . 3_565 no
N2 S2 3.0604(7) . . no
N2 S3 3.0623(7) . . no
N2 S4 3.4810(7) . 3_566 no
N2 S2 3.4526(7) . 4_465 no
N2 S3 3.5145(7) . 4_565 no
N3 S1 3.0494(7) . . no
N3 S2 3.0591(7) . . no
N3 S1 3.1507(7) . 2_445 no
N3 S2 3.0874(7) . 3_565 no
N3 N1 3.2163(9) . 3_565 no
N4 S3 3.0568(7) . . no
N4 S4 3.0460(7) . . no
N4 S2 3.1548(7) . 2_555 no
N4 S4 3.4808(7) . 2_555 no
N4 S3 3.2819(7) . 3_575 no
N4 S3 3.4898(7) . 4_565 no
# End of Crystallographic Information File