# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Prof Matthias Wagner' _publ_contact_author_address ; Inst. fuer Anorganische Chemie Goethe-Universitaet Frankfurt Marie Curie-Strasse 11 Frankfurt 60439 ; _publ_contact_author_email MATTHIAS.WAGNER@CHEMIE.UNI-FRANKFURT.DE _publ_section_title ; Solvent-Free Methylthiomethyllithium [LiCH2SMe] : Solid State Structure and Thermal Decomposition. ; loop_ _publ_author_name 'Matthias Wagner' 'Edith Alig' 'Robert E. Dinnebier' 'Hans-Wolfram Lerner' 'Kai Ruth' 'Ingebororg Sanger' ; S.Tonnes ; data_CH3SCH2LI _database_code_depnum_ccdc_archive 'CCDC 267441' _pd_block_id 2005-03-29T16:19|C2SLI_ANISO_R|R.E.D.|D8 _audit_creation_method 'from EXP file using GSAS2CIF' _audit_creation_date 2005-03-29T16:19 _audit_author_name R.E.D. _audit_update_record ; 2005-03-29T16:19 Initial CIF as created by GSAS2CIF ; #============================================================================= # this information describes the project, paper etc. for the CIF # # Acta Cryst. Section C papers and editorial correspondence is generated # # from the information in this section # # # # (from) CIF submission form for Rietveld refinements (Acta Cryst. C) # # Version 14 December 1998 # #============================================================================= _publ_section_comment ; The crystal structure of CH3SCH2LI was solved from powder diffraction data ; # The following items are used to identify the programs used. _computing_molecular_graphics ? _computing_publication_material ? _refine_ls_weighting_scheme ? _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_number_constraints ? _refine_ls_restrained_S_all ? _refine_ls_restrained_S_obs ? #============================================================================== # 5. SAMPLE PREPARATION DATA # (In the unusual case where multiple samples are used in a single # Rietveld study, this information should be moved into the phase # blocks) # The following three fields describe the preparation of the material. # The cooling rate is in K/min. The pressure at which the sample was # prepared is in kPa. The temperature of preparation is in K. _pd_prep_cool_rate ? _pd_prep_pressure ? _pd_prep_temperature ? _pd_char_colour ? # use ICDD colour descriptions _refine_ls_shift/su_max 0.34 _refine_ls_shift/su_mean 0.03 _computing_structure_refinement GSAS _refine_ls_number_parameters 47 _refine_ls_goodness_of_fit_all 2.14 _refine_ls_number_restraints 17 _refine_ls_matrix_type full #============================================================================== # 6. CHEMICAL, STRUCTURAL AND CRYSTAL DATA _pd_char_particle_morphology ? _chemical_name_systematic ; ? ; _chemical_name_common Methylthiomethyllithium _chemical_formula_moiety ? _chemical_formula_structural LiCH2SCH3 _chemical_formula_analytical ? _chemical_melting_point ? _chemical_compound_source ? # for minerals and # natural products _symmetry_space_group_name_Hall ? _exptl_crystal_F_000 ? _exptl_crystal_density_diffrn ? _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _cell_measurement_temperature ? _cell_special_details ; ? ; _geom_special_details ? # The following item identifies the program(s) used (if appropriate). _computing_structure_solution ? #============================================================================== # 7. Phase information from GSAS _pd_phase_name CH3SCH2Li _cell_length_a 8.32854(34) _cell_length_b 5.03756(13) _cell_length_c 9.82453(23) _cell_angle_alpha 90.0 _cell_angle_beta 100.3750(13) _cell_angle_gamma 90.0 _cell_volume 405.454(30) _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +x,+y,+z 2 -x,+y+1/2,-z+1/2 -1 -x,-y,-z -2 +x,-y+1/2,+z+1/2 # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_thermal_displace_type _atom_site_U_iso_or_equiv _atom_site_symmetry_multiplicity Li LI1 0.4882(18) 0.6545(22) 0.0837(13) 1.0 Uiso 0.076(7) 4 S S2 0.64226(17) 0.5475(4) 0.33936(20) 1.0 Uiso 0.0650(8) 4 C C3 0.6825(5) 0.8156(8) 0.4632(5) 1.0 Uiso 0.0650(8) 4 C C4 0.84000(28) 0.4261(8) 0.31514(34) 1.0 Uiso 0.0650(8) 4 H H5 0.7988(22) 0.894(5) 0.4616(30) 1.0 Uiso 0.0650(8) 4 H H6 0.678(5) 0.7423(23) 0.5626(9) 1.0 Uiso 0.0650(8) 4 H H7 0.8246(9) 0.279(5) 0.2384(24) 1.0 Uiso 0.0650(8) 4 H H8 0.9025(15) 0.346(6) 0.4084(11) 1.0 Uiso 0.0650(8) 4 H H9 0.9082(12) 0.5834(24) 0.285(4) 1.0 Uiso 0.0650(8) 4 # If you change Z, be sure to change all 3 of the following _chemical_formula_sum 'C2 H5 Li S' _chemical_formula_weight 68.06 _cell_formula_units_Z 4 # MOLECULAR GEOMETRY 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 LI1 LI1 2.298(21) . -1_665 N LI1 S2 2.662(12) . 1_555 N LI1 S2 2.443(13) . 2_655 N LI1 C3 2.216(12) . 2_645 N LI1 C3 2.175(13) . -2_564 N LI1 H5 2.692(28) . 2_645 N LI1 H6 2.753(28) . 2_645 N LI1 H6 1.71(4) . -2_564 N S2 LI1 2.662(12) . 1_555 N S2 LI1 2.443(10) . 2_645 N S2 C3 1.8086(8) . 1_555 N S2 C4 1.8120(8) . 1_555 N S2 H5 2.373(4) . 1_555 N S2 H6 2.372(4) . 1_555 N S2 H6 2.983(6) . -2_564 N S2 H7 2.381(4) . 1_555 N S2 H8 2.3793(32) . 1_555 N S2 H9 2.379(4) . 1_555 N C3 LI1 2.216(12) . 2_655 N C3 LI1 2.175(13) . -2_565 N C3 S2 1.8086(8) . 1_555 N C3 C4 2.8939(29) . 1_555 N C3 H5 1.0501(8) . 1_555 N C3 H6 1.0499(8) . 1_555 N C4 S2 1.8120(8) . 1_555 N C4 C3 2.8939(29) . 1_555 N C4 H5 2.816(9) . 1_555 N C4 H7 1.0501(8) . 1_555 N C4 H8 1.0500(8) . 1_555 N C4 H9 1.0502(8) . 1_555 N H5 LI1 2.692(28) . 2_655 N H5 S2 2.373(4) . 1_555 N H5 C3 1.0501(8) . 1_555 N H5 C4 2.816(9) . 1_555 N H5 H6 1.7143(25) . 1_555 N H5 H7 2.96(4) . 1_565 N H5 H8 2.97(4) . 1_555 N H5 H8 2.52(4) . 1_565 N H5 H8 2.853(33) . -1_766 N H5 H9 2.623(28) . 1_555 N H6 LI1 2.753(28) . 2_655 N H6 LI1 1.71(4) . -2_565 N H6 S2 2.372(4) . 1_555 N H6 S2 2.983(6) . -2_565 N H6 C3 1.0499(8) . 1_555 N H6 H5 1.7143(25) . 1_555 N H6 H9 2.773(31) . -2_565 N H7 S2 2.381(4) . 1_555 N H7 C4 1.0501(8) . 1_555 N H7 H5 2.96(4) . 1_545 N H7 H8 1.7124(30) . 1_555 N H7 H9 1.7131(23) . 1_555 N H7 H9 2.479(8) . 2_745 N H8 S2 2.3793(32) . 1_555 N H8 C4 1.0500(8) . 1_555 N H8 H5 2.52(4) . 1_545 N H8 H5 2.97(4) . 1_555 N H8 H5 2.853(33) . -1_766 N H8 H7 1.7124(30) . 1_555 N H8 H8 2.69(6) . -1_766 N H8 H9 1.7144(21) . 1_555 N H8 H9 2.983(7) . 2_745 N H9 S2 2.379(4) . 1_555 N H9 C4 1.0502(8) . 1_555 N H9 H5 2.623(28) . 1_555 N H9 H6 2.773(31) . -2_564 N H9 H7 1.7131(23) . 1_555 N H9 H7 2.479(8) . 2_755 N H9 H8 1.7144(21) . 1_555 N H9 H8 2.983(7) . 2_755 N 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 LI1 LI1 S2 116.7(8) -1_665 . 1_555 N LI1 LI1 S2 150.5(10) -1_665 . 2_655 N LI1 LI1 C3 57.6(5) -1_665 . 2_645 N LI1 LI1 C3 59.3(6) -1_665 . -2_575 N LI1 LI1 H5 74.9(8) -1_665 . 2_645 N LI1 LI1 H6 38.3(7) -1_665 . 2_645 N LI1 LI1 H6 85.4(8) -1_665 . -2_575 N S2 LI1 S2 92.2(4) 1_555 . 2_655 N S2 LI1 C3 102.8(5) 1_555 . 2_645 N S2 LI1 C3 104.4(6) 1_555 . -2_575 N S2 LI1 H5 108.7(7) 1_555 . 2_645 N S2 LI1 H6 116.8(4) 1_555 . 2_645 N S2 LI1 H6 82.9(7) 1_555 . -2_575 N S2 LI1 C3 112.6(6) 2_655 . 2_645 N S2 LI1 C3 121.9(6) 2_655 . -2_575 N S2 LI1 H5 90.8(7) 2_655 . 2_645 N S2 LI1 H6 124.2(9) 2_655 . 2_645 N S2 LI1 H6 105.3(7) 2_655 . -2_575 N C3 LI1 C3 116.9(5) 2_645 . -2_575 N C3 LI1 H5 22.1(4) 2_645 . 2_645 N C3 LI1 H6 21.0(5) 2_645 . 2_645 N C3 LI1 H6 141.3(6) 2_645 . -2_575 N C3 LI1 H5 132.0(9) -2_575 . 2_645 N C3 LI1 H6 97.0(8) -2_575 . 2_645 N C3 LI1 H6 28.3(4) -2_575 . -2_575 N H5 LI1 H6 36.68(17) 2_645 . 2_645 N H5 LI1 H6 160.0(11) 2_645 . -2_575 N H6 LI1 H6 123.7(10) 2_645 . -2_575 N LI1 S2 LI1 106.9(4) 1_555 . 2_645 N LI1 S2 C3 118.89(33) 1_555 . 1_555 N LI1 S2 C4 103.85(32) 1_555 . 1_555 N LI1 S2 H5 117.1(10) 1_555 . 1_555 N LI1 S2 H6 138.4(8) 1_555 . 1_555 N LI1 S2 H6 34.8(7) 1_555 . -2_575 N LI1 S2 H7 87.6(6) 1_555 . 1_555 N LI1 S2 H8 127.9(4) 1_555 . 1_555 N LI1 S2 H9 94.7(8) 1_555 . 1_555 N LI1 S2 C3 115.8(4) 2_645 . 1_555 N LI1 S2 C4 103.5(4) 2_645 . 1_555 N LI1 S2 H5 132.4(8) 2_645 . 1_555 N LI1 S2 H6 92.2(4) 2_645 . 1_555 N LI1 S2 H6 133.9(7) 2_645 . -2_575 N LI1 S2 H7 91.2(8) 2_645 . 1_555 N LI1 S2 H8 89.9(8) 2_645 . 1_555 N LI1 S2 H9 128.0(4) 2_645 . 1_555 N C3 S2 C4 106.12(15) 1_555 . 1_555 N C3 S2 H5 24.67(9) 1_555 . 1_555 N C3 S2 H6 24.70(8) 1_555 . 1_555 N C3 S2 H6 108.15(25) 1_555 . -2_575 N C3 S2 H7 130.58(22) 1_555 . 1_555 N C3 S2 H8 94.5(7) 1_555 . 1_555 N C3 S2 H9 91.6(7) 1_555 . 1_555 N C4 S2 H5 83.4(4) 1_555 . 1_555 N C4 S2 H6 107.1(10) 1_555 . 1_555 N C4 S2 H6 75.9(6) 1_555 . -2_575 N C4 S2 H7 24.53(9) 1_555 . 1_555 N C4 S2 H8 24.57(7) 1_555 . 1_555 N C4 S2 H9 24.58(10) 1_555 . 1_555 N H5 S2 H6 42.36(7) 1_555 . 1_555 N H5 S2 H6 93.7(13) 1_555 . -2_575 N H5 S2 H7 107.2(4) 1_555 . 1_555 N H5 S2 H8 77.4(12) 1_555 . 1_555 N H5 S2 H9 67.0(7) 1_555 . 1_555 N H6 S2 H6 132.8(4) 1_555 . -2_575 N H6 S2 H7 129.6(9) 1_555 . 1_555 N H6 S2 H8 87.5(9) 1_555 . 1_555 N H6 S2 H9 102.1(14) 1_555 . 1_555 N H6 S2 H7 69.3(9) -2_575 . 1_555 N H6 S2 H8 100.1(6) -2_575 . 1_555 N H6 S2 H9 61.1(9) -2_575 . 1_555 N H7 S2 H8 42.17(12) 1_555 . 1_555 N H7 S2 H9 42.19(7) 1_555 . 1_555 N H8 S2 H9 42.24(7) 1_555 . 1_555 N LI1 C3 LI1 63.1(5) 2_655 . -2_565 N LI1 C3 S2 113.66(34) 2_655 . 1_555 N LI1 C3 C4 138.6(4) 2_655 . 1_555 N LI1 C3 H5 105.4(19) 2_655 . 1_555 N LI1 C3 H6 109.7(18) 2_655 . 1_555 N LI1 C3 S2 110.6(4) -2_576 . 1_555 N LI1 C3 C4 140.3(4) -2_576 . 1_555 N LI1 C3 H5 139.6(6) -2_576 . 1_555 N LI1 C3 H6 50.6(22) -2_576 . 1_555 N S2 C3 C4 36.98(8) 1_555 . 1_555 N S2 C3 H5 109.37(29) 1_555 . 1_555 N S2 C3 H6 109.25(26) 1_555 . 1_555 N C4 C3 H5 75.2(4) 1_555 . 1_555 N C4 C3 H6 108.9(13) 1_555 . 1_555 N H5 C3 H6 109.44(22) 1_555 . 1_555 N S2 C4 C3 36.90(7) 1_555 . 1_555 N S2 C4 H5 56.85(28) 1_555 . 1_555 N S2 C4 H7 109.69(29) 1_555 . 1_555 N S2 C4 H8 109.58(23) 1_555 . 1_555 N S2 C4 H9 109.55(32) 1_555 . 1_555 N C3 C4 H5 21.138(34) 1_555 . 1_555 N C3 C4 H7 146.44(21) 1_555 . 1_555 N C3 C4 H8 91.2(11) 1_555 . 1_555 N C3 C4 H9 87.1(12) 1_555 . 1_555 N H5 C4 H7 161.7(14) 1_555 . 1_555 N H5 C4 H8 88.0(19) 1_555 . 1_555 N H5 C4 H9 68.7(16) 1_555 . 1_555 N H7 C4 H8 109.26(27) 1_555 . 1_555 N H7 C4 H9 109.31(20) 1_555 . 1_555 N H8 C4 H9 109.43(18) 1_555 . 1_555 N LI1 H5 S2 83.3(7) 2_655 . 1_555 N LI1 H5 C3 52.5(14) 2_655 . 1_555 N LI1 H5 C4 120.6(8) 2_655 . 1_555 N LI1 H5 H6 73.6(17) 2_655 . 1_555 N LI1 H5 H7 75.0(10) 2_655 . 1_565 N LI1 H5 H8 134.5(5) 2_655 . 1_555 N LI1 H5 H8 81.6(10) 2_655 . 1_565 N LI1 H5 H8 163.2(10) 2_655 . -1_766 N LI1 H5 H9 125.8(14) 2_655 . 1_555 N S2 H5 C3 45.96(20) 1_555 . 1_555 N S2 H5 C4 39.73(12) 1_555 . 1_555 N S2 H5 H6 68.77(19) 1_555 . 1_555 N S2 H5 H7 102.3(11) 1_555 . 1_565 N S2 H5 H8 51.4(5) 1_555 . 1_555 N S2 H5 H8 137.5(15) 1_555 . 1_565 N S2 H5 H8 105.7(10) 1_555 . -1_766 N S2 H5 H9 56.60(33) 1_555 . 1_555 N C3 H5 C4 83.6(4) 1_555 . 1_555 N C3 H5 H6 35.28(11) 1_555 . 1_555 N C3 H5 H7 116.7(26) 1_555 . 1_565 N C3 H5 H8 87.1(12) 1_555 . 1_555 N C3 H5 H8 134.1(24) 1_555 . 1_565 N C3 H5 H8 124.5(25) 1_555 . -1_766 N C3 H5 H9 102.5(4) 1_555 . 1_555 N C4 H5 H6 93.4(10) 1_555 . 1_555 N C4 H5 H7 97.9(6) 1_555 . 1_565 N C4 H5 H8 20.69(25) 1_555 . 1_555 N C4 H5 H8 124.9(6) 1_555 . 1_565 N C4 H5 H8 72.4(8) 1_555 . -1_766 N C4 H5 H9 21.90(7) 1_555 . 1_555 N H6 H5 H7 148.1(27) 1_555 . 1_565 N H6 H5 H8 84.6(17) 1_555 . 1_555 N H6 H5 H8 141.4(10) 1_555 . 1_565 N H6 H5 H8 96.1(27) 1_555 . -1_766 N H6 H5 H9 115.2(11) 1_555 . 1_555 N H7 H5 H8 114.6(5) 1_565 . 1_555 N H7 H5 H8 35.3(5) 1_565 . 1_565 N H7 H5 H8 115.8(5) 1_565 . -1_766 N H7 H5 H9 79.6(7) 1_565 . 1_555 N H8 H5 H8 132.99(30) 1_555 . 1_565 N H8 H5 H8 55.0(10) 1_555 . -1_766 N H8 H5 H9 35.00(35) 1_555 . 1_555 N H8 H5 H8 99.9(7) 1_565 . -1_766 N H8 H5 H9 103.2(6) 1_565 . 1_555 N H8 H5 H9 70.4(6) -1_766 . 1_555 N LI1 H6 LI1 56.3(10) 2_655 . -2_565 N LI1 H6 S2 82.1(6) 2_655 . 1_555 N LI1 H6 S2 94.8(8) 2_655 . -2_576 N LI1 H6 C3 49.3(13) 2_655 . 1_555 N LI1 H6 H5 69.7(16) 2_655 . 1_555 N LI1 H6 H9 112.5(5) 2_655 . -2_576 N LI1 H6 S2 105.8(15) -2_576 . 1_555 N LI1 H6 S2 62.3(5) -2_576 . -2_576 N LI1 H6 C3 101.1(26) -2_576 . 1_555 N LI1 H6 H5 125.8(24) -2_576 . 1_555 N LI1 H6 H9 109.3(5) -2_576 . -2_576 N S2 H6 S2 166.7(15) 1_555 . -2_576 N S2 H6 C3 46.05(18) 1_555 . 1_555 N S2 H6 H5 68.87(21) 1_555 . 1_555 N S2 H6 H9 144.3(16) 1_555 . -2_576 N S2 H6 C3 138.4(9) -2_576 . 1_555 N S2 H6 H5 122.3(7) -2_576 . 1_555 N S2 H6 H9 48.65(27) -2_576 . -2_576 N C3 H6 H5 35.29(11) 1_555 . 1_555 N C3 H6 H9 119.0(19) 1_555 . -2_576 N H5 H6 H9 85.4(20) 1_555 . -2_576 N S2 H7 C4 45.77(20) 1_555 . 1_555 N S2 H7 H5 85.8(9) 1_555 . 1_545 N S2 H7 H8 68.87(12) 1_555 . 1_555 N S2 H7 H9 68.85(25) 1_555 . 1_555 N S2 H7 H9 156.0(5) 1_555 . 2_745 N C4 H7 H5 86.9(18) 1_555 . 1_545 N C4 H7 H8 35.37(14) 1_555 . 1_555 N C4 H7 H9 35.35(10) 1_555 . 1_555 N C4 H7 H9 110.5(7) 1_555 . 2_745 N H5 H7 H8 58.1(19) 1_545 . 1_555 N H5 H7 H9 118.0(19) 1_545 . 1_555 N H5 H7 H9 89.7(4) 1_545 . 2_745 N H8 H7 H9 60.06(11) 1_555 . 1_555 N H8 H7 H9 88.8(5) 1_555 . 2_745 N H9 H7 H9 92.9(7) 1_555 . 2_745 N S2 H8 C4 45.85(16) 1_555 . 1_555 N S2 H8 H5 96.7(9) 1_555 . 1_545 N S2 H8 H5 51.2(6) 1_555 . 1_555 N S2 H8 H5 170.0(6) 1_555 . -1_766 N S2 H8 H7 68.96(15) 1_555 . 1_555 N S2 H8 H8 110.6(13) 1_555 . -1_766 N S2 H8 H9 68.87(22) 1_555 . 1_555 N S2 H8 H9 124.52(27) 1_555 . 2_745 N C4 H8 H5 113.3(20) 1_555 . 1_545 N C4 H8 H5 71.3(17) 1_555 . 1_555 N C4 H8 H5 144.1(6) 1_555 . -1_766 N C4 H8 H7 35.37(14) 1_555 . 1_555 N C4 H8 H8 120.3(26) 1_555 . -1_766 N C4 H8 H9 35.29(9) 1_555 . 1_555 N C4 H8 H9 81.52(29) 1_555 . 2_745 N H5 H8 H5 132.99(30) 1_545 . 1_555 N H5 H8 H5 80.1(7) 1_545 . -1_766 N H5 H8 H7 86.6(23) 1_545 . 1_555 N H5 H8 H8 124.8(8) 1_545 . -1_766 N H5 H8 H9 146.3(23) 1_545 . 1_555 N H5 H8 H9 88.4(12) 1_545 . 2_745 N H5 H8 H5 125.0(10) 1_555 . -1_766 N H5 H8 H7 106.5(15) 1_555 . 1_555 N H5 H8 H8 60.3(10) 1_555 . -1_766 N H5 H8 H9 61.4(19) 1_555 . 1_555 N H5 H8 H9 136.7(13) 1_555 . 2_745 N H5 H8 H7 120.0(11) -1_766 . 1_555 N H5 H8 H8 64.71(15) -1_766 . -1_766 N H5 H8 H9 118.7(9) -1_766 . 1_555 N H5 H8 H9 65.1(9) -1_766 . 2_745 N H7 H8 H8 147.4(25) 1_555 . -1_766 N H7 H8 H9 59.99(13) 1_555 . 1_555 N H7 H8 H9 56.2(4) 1_555 . 2_745 N H8 H8 H9 88.9(27) -1_766 . 1_555 N H8 H8 H9 110.88(23) -1_766 . 2_745 N H9 H8 H9 76.9(4) 1_555 . 2_745 N S2 H9 C4 45.87(22) 1_555 . 1_555 N S2 H9 H5 56.4(4) 1_555 . 1_555 N S2 H9 H6 70.3(6) 1_555 . -2_575 N S2 H9 H7 68.96(23) 1_555 . 1_555 N S2 H9 H7 159.73(34) 1_555 . 2_755 N S2 H9 H8 68.89(20) 1_555 . 1_555 N S2 H9 H8 142.92(32) 1_555 . 2_755 N C4 H9 H5 89.4(16) 1_555 . 1_555 N C4 H9 H6 97.5(14) 1_555 . -2_575 N C4 H9 H7 35.34(10) 1_555 . 1_555 N C4 H9 H7 150.0(10) 1_555 . 2_755 N C4 H9 H8 35.28(9) 1_555 . 1_555 N C4 H9 H8 153.0(27) 1_555 . 2_755 N H5 H9 H6 93.4(6) 1_555 . -2_575 N H5 H9 H7 122.5(12) 1_555 . 1_555 N H5 H9 H7 104.36(25) 1_555 . 2_755 N H5 H9 H8 83.6(22) 1_555 . 1_555 N H5 H9 H8 116.3(9) 1_555 . 2_755 N H6 H9 H7 83.4(18) -2_575 . 1_555 N H6 H9 H7 107.9(9) -2_575 . 2_755 N H6 H9 H8 132.5(13) -2_575 . 1_555 N H6 H9 H8 74.3(7) -2_575 . 2_755 N H7 H9 H7 131.3(6) 1_555 . 2_755 N H7 H9 H8 59.95(15) 1_555 . 1_555 N H7 H9 H8 117.7(27) 1_555 . 2_755 N H7 H9 H8 118.8(14) 2_755 . 1_555 N H7 H9 H8 35.03(12) 2_755 . 2_755 N H8 H9 H8 147.8(5) 1_555 . 2_755 N # Powder diffraction data for histogram 1 #============================================================================== # 8. INSTRUMENT CHARACTERIZATION _exptl_special_details ; ? ; # if regions of the data are excluded, the reason(s) are supplied here: _pd_proc_info_excluded_regions ; ? ; # The following item is used to identify the equipment used to record # the powder pattern when the diffractogram was measured at a laboratory # other than the authors' home institution, e.g. when neutron or synchrotron # radiation is used. _pd_instr_location ; ? ; _pd_calibration_special_details # description of the method used # to calibrate the instrument ; ? ; _diffrn_ambient_temperature ? _diffrn_source ? _diffrn_source_target ? _diffrn_source_type ? _diffrn_measurement_device_type ? _diffrn_detector ? _diffrn_detector_type ? # make or model of detector _pd_meas_scan_method ? # options are 'step', 'cont', # 'tof', 'fixed' or # 'disp' (= dispersive) _pd_meas_special_details ; ? ; # The following two items identify the program(s) used (if appropriate). _computing_data_collection ? _computing_data_reduction ? # Describe any processing performed on the data, prior to refinement. # For example: a manual Lp correction or a precomputed absorption correction _pd_proc_info_data_reduction ? # The following item is used for angular dispersive measurements only. _diffrn_radiation_monochromator ? # The following items are used to define the size of the instrument. # Not all distances are appropriate for all instrument types. _pd_instr_dist_src/mono ? _pd_instr_dist_mono/spec ? _pd_instr_dist_src/spec ? _pd_instr_dist_spec/anal ? _pd_instr_dist_anal/detc ? _pd_instr_dist_spec/detc ? # 10. Specimen size and mounting information # The next three fields give the specimen dimensions in mm. The equatorial # plane contains the incident and diffracted beam. _pd_spec_size_axial ? # perpendicular to # equatorial plane _pd_spec_size_equat ? # parallel to # scattering vector # in transmission _pd_spec_size_thick ? # parallel to # scattering vector # in reflection _pd_spec_mounting # This field should be # used to give details of the # container. ; ? ; _pd_spec_mount_mode ? # options are 'reflection' # or 'transmission' _pd_spec_shape ? # options are 'cylinder' # 'flat_sheet' or 'irregular' loop_ _atom_type_symbol _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source Li 4.0 0.000 0.000 1.12820 3.95460 0.75080 1.05240 0.61750 85.3905 0.46530 168.261 0.03770 International_Tables_Vol_C S 4.0 0.000 0.000 6.90530 1.46790 5.20340 22.2151 1.43790 0.25360 1.58630 56.1720 0.86690 International_Tables_Vol_C C 8.0 0.000 0.000 2.31000 20.8439 1.02000 10.2075 1.58860 0.56870 0.86500 51.6512 0.21560 International_Tables_Vol_C H 20.0 0.000 0.000 0.49300 10.5109 0.32291 26.1257 0.14019 3.14236 0.04081 57.7997 0.00304 International_Tables_Vol_C _diffrn_radiation_probe x-ray _diffrn_radiation_polarisn_ratio ? _diffrn_radiation_wavelength 1.54056 _diffrn_radiation_type ? _pd_proc_ls_prof_R_factor 0.0352 _pd_proc_ls_prof_wR_factor 0.0485 _pd_proc_ls_prof_wR_expected 0.0229 _refine_ls_R_Fsqd_factor 0.11648 _pd_proc_ls_background_function ; GSAS Background function number 2 with 4 terms. Cosine Fourier series 1: 0.00000 2: 0.00000 3: 0.00000 4: 0.00000 ; _exptl_absorpt_process_details ; GSAS Absorption/surface roughness correction: function number 0 No correction is applied. ; _exptl_absorpt_correction_T_min 1.00000 _exptl_absorpt_correction_T_max 1.00000 # Extinction correction _gsas_exptl_extinct_corr_T_min 1.00000 _gsas_exptl_extinct_corr_T_max 1.00000 _pd_proc_ls_profile_function ; CW Profile function number 4 with 21 terms Pseudovoigt profile coefficients as parameterized in P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. Asymmetry correction of L.W. Finger, D.E. Cox & A. P. Jephcoat (1994). J. Appl. Cryst.,27,892-900. Microstrain broadening by P.W. Stephens, (1999). J. Appl. Cryst.,32,281-289. #1(GU) = 0.000 #2(GV) = 0.000 #3(GW) = 0.000 #4(GP) = 1.713 #5(LX) = 0.000 #6(ptec) = 0.00 #7(trns) = 0.00 #8(shft) = 0.0000 #9(sfec) = 0.00 #10(S/L) = 0.0222 #11(H/L) = 0.0300 #12(eta) = 0.7402 #13(S400 ) = 7.9E-01 #14(S040 ) = 5.7E+00 #15(S004 ) = 1.3E-01 #16(S220 ) = -3.3E-01 #17(S202 ) = 1.8E-01 #18(S022 ) = 5.5E-01 #19(S301 ) = 3.9E-01 #20(S103 ) = 4.7E-02 #21(S121 ) = 1.3E-01 Peak tails are ignored where the intensity is below 0.0010 times the peak Aniso. broadening axis 0.0 0.0 1.0 ; _pd_proc_ls_peak_cutoff 0.00100 _pd_proc_info_datetime 2005-03-29T16:19:26 _pd_calc_method 'Rietveld Refinement' #---- raw/calc data loop ----- _pd_meas_2theta_range_min 8.0 _pd_meas_2theta_range_max 68.21779 _pd_meas_2theta_range_inc 0.01721 _pd_proc_2theta_range_min 8.0235 _pd_proc_2theta_range_max 68.24129 _pd_proc_2theta_range_inc 0.01721 _reflns_number_total 162 _reflns_limit_h_min 0 _reflns_limit_h_max 6 _reflns_limit_k_min 0 _reflns_limit_k_max 3 _reflns_limit_l_min -6 _reflns_limit_l_max 6 _reflns_d_resolution_high 1.377 _reflns_d_resolution_low 8.192 #--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--#