# 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