# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_general_ _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 #TrackingRef '9192_web_deposit_cif_file_0_Md.AlamgirHossain_1327327776.Br_10069_Jan22.cif' _publ_contact_author ; Md. Alamgir Hossain Department of Chemistry and Biochemistry Jackson State University Jackson 1325 Lynch Street Jackson, MS 39212, USA ; _publ_contact_author_email alamgir.hossain@jsums.edu _publ_contact_author_fax 601-979-3674 _publ_contact_author_phone 601-979-3748 loop_ _publ_author_name _publ_author_address 'Musabbir A. Saeed' ; Department of Chemistry and Biochemistry Jackson State University Jackson 1325 Lynch Street Jackson, MS 39212, USA ; 'Syed Ataul Haque' ; Department of Chemistry University of Kansas Lawrence, KS 66045, USA ; 'Avijit Pramanik' '' 'Bryan M. Wong' '' 'Douglas R. Powell' '' 'Dillip Kumar Chand' '' ; Md.A.Hossain ; '' _publ_section_title ; Self-assembly of Ordered Water Tetramers in an Encapsulated [Br(H2O)12]-Complex ; _publ_section_acknowledgements ; National Science Foundation is acknowledged for a CAREER award (CHE-1056927) to MAH. The work was supported by the National Institute of health (G12RR013459). The NMR instrument used for this work was funded by the National Science Foundation (CHE-0821357). The authors thank the National Science Foundation (CHE-0130835) and the University of Oklahoma for funds to acquire the diffractometer used in this work. ; #============================================================ data_10069 _database_code_depnum_ccdc_archive 'CCDC 864063' #TrackingRef '9192_web_deposit_cif_file_0_Md.AlamgirHossain_1327327776.Br_10069_Jan22.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H54 N8 S3, 6Br, 12(H2 O)' _chemical_formula_sum 'C30 H78 Br6 N8 O12 S3' _chemical_formula_weight 1318.64 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' O O 0.0106 0.0060 '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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Cubic _symmetry_space_group_name_H-M 'P 21 3' _symmetry_space_group_name_Hall 'P 2ac 2ab 3' 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' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' _cell_length_a 17.7890(9) _cell_length_b 17.7890(9) _cell_length_c 17.7890(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5629.3(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8258 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 28.46 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.58 _exptl_crystal_size_mid 0.54 _exptl_crystal_size_min 0.36 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.556 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2672 _exptl_absorpt_coefficient_mu 4.444 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1826 _exptl_absorpt_correction_T_max 0.2976 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2001)' _exptl_special_details ; The sample exhibited racemic twinning. The intensity data were truncated to 0.86 \%A resolution because data in higher resolution shells all had < 2. ; _diffrn_ambient_temperature 100(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 'CCD Bruker APEX' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% . _diffrn_reflns_number 73811 _diffrn_reflns_av_R_equivalents 0.1045 _diffrn_reflns_av_sigmaI/netI 0.0332 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 24.38 _reflns_number_total 3105 _reflns_number_gt 2791 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART (Bruker, 2007)' _computing_cell_refinement 'SMART (Bruker, 2007)' _computing_data_reduction 'SMART (Bruker, 2007)' _computing_structure_solution 'SHELXTL (Sheldrick, 2008)' _computing_structure_refinement 'SHELXTL (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _refine_special_details ; ; _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^)+(0.1800P)^2^+120.0000P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.12(5) _refine_ls_number_reflns 3105 _refine_ls_number_parameters 179 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1269 _refine_ls_R_factor_gt 0.1191 _refine_ls_wR_factor_ref 0.3510 _refine_ls_wR_factor_gt 0.3460 _refine_ls_goodness_of_fit_ref 1.244 _refine_ls_restrained_S_all 1.244 _refine_ls_shift/su_max 0.012 _refine_ls_shift/su_mean 0.003 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 Br1 Br 0.60834(15) 0.22364(16) 1.10883(17) 0.0611(9) Uani 1 1 d . . . Br2 Br 0.76026(10) 0.23974(10) 0.73974(10) 0.0302(8) Uani 1 3 d S . . Br3 Br 0.92847(12) 0.92847(12) 0.92847(12) 0.0386(9) Uani 1 3 d S . . Br4 Br 0.9432(2) 0.4432(2) 1.0568(2) 0.0784(16) Uani 1 3 d S . . S1 S 0.8879(2) 0.2597(2) 0.9236(3) 0.0250(9) Uani 1 1 d . . . N1 N 0.5751(8) 0.4249(8) 0.9249(8) 0.024(5) Uani 1 3 d S . . C2 C 0.5901(12) 0.4089(11) 1.0047(10) 0.033(5) Uani 1 1 d . . . H2A H 0.5657 0.3605 1.0176 0.039 Uiso 1 1 calc R . . H2B H 0.5656 0.4484 1.0353 0.039 Uiso 1 1 calc R . . C3 C 0.6712(10) 0.4044(11) 1.0276(9) 0.026(4) Uani 1 1 d . . . H3A H 0.6749 0.3992 1.0829 0.031 Uiso 1 1 calc R . . H3B H 0.6975 0.4511 1.0127 0.031 Uiso 1 1 calc R . . N4 N 0.7083(9) 0.3372(9) 0.9897(9) 0.027(3) Uani 1 1 d . . . H4A H 0.6756 0.2971 0.9909 0.033 Uiso 1 1 calc R . . H4B H 0.7172 0.3487 0.9401 0.033 Uiso 1 1 calc R . . C5 C 0.7817(9) 0.3141(13) 1.0263(10) 0.031(5) Uani 1 1 d . . . H5A H 0.8176 0.3565 1.0236 0.038 Uiso 1 1 calc R . . H5B H 0.7725 0.3028 1.0800 0.038 Uiso 1 1 calc R . . C6 C 0.8156(10) 0.2473(10) 0.9897(10) 0.024(4) Uani 1 1 d . . . C7 C 0.7973(9) 0.1789(11) 0.9961(10) 0.026(4) Uani 1 1 d . . . H7 H 0.7582 0.1633 1.0290 0.031 Uiso 1 1 calc R . . C8 C 0.8393(11) 0.1249(10) 0.9502(9) 0.026(4) Uani 1 1 d . . . H8 H 0.8324 0.0720 0.9497 0.032 Uiso 1 1 calc R . . C9 C 0.8910(10) 0.1648(9) 0.9077(9) 0.020(4) Uani 1 1 d . . . C10 C 0.9466(9) 0.1319(10) 0.8552(8) 0.017(3) Uani 1 1 d . . . H10A H 0.9615 0.0814 0.8733 0.021 Uiso 1 1 calc R . . H10B H 0.9921 0.1639 0.8540 0.021 Uiso 1 1 calc R . . N11 N 0.9149(10) 0.1254(9) 0.7770(8) 0.036(4) Uani 1 1 d . . . H11A H 0.8682 0.1032 0.7793 0.043 Uiso 1 1 calc R . . H11B H 0.9090 0.1727 0.7570 0.043 Uiso 1 1 calc R . . C12 C 0.9652(11) 0.0798(13) 0.7267(13) 0.041(5) Uani 1 1 d . . . H12A H 0.9838 0.0358 0.7553 0.049 Uiso 1 1 calc R . . H12B H 1.0093 0.1108 0.7127 0.049 Uiso 1 1 calc R . . C13 C 0.9263(16) 0.0516(16) 0.6537(13) 0.053(6) Uani 1 1 d . . . H13A H 0.9645 0.0270 0.6215 0.064 Uiso 1 1 calc R . . H13B H 0.8885 0.0131 0.6674 0.064 Uiso 1 1 calc R . . N14 N 0.8895(7) 0.1105(7) 0.6105(7) 0.020(5) Uani 1 3 d S . . O1S O 0.6057(11) 0.1091(11) 0.9654(10) 0.061(5) Uani 1 1 d . . . H1SA H 0.6067 0.1388 1.0028 0.073 Uiso 1 1 d R . . H1SB H 0.5607 0.0944 0.9593 0.073 Uiso 1 1 d R . . O2S O 0.7849(11) 0.0380(9) 0.7700(9) 0.050(4) Uani 1 1 d . . . H2SA H 0.7572 0.0375 0.8089 0.060 Uiso 1 1 d R . . H2SB H 0.7792 0.0848 0.7627 0.060 Uiso 1 1 d R . . O3S O 0.7651(8) 0.3845(8) 0.8539(8) 0.038(3) Uani 1 1 d . . . H3SA H 0.7637 0.3470 0.8243 0.046 Uiso 1 1 d R . . H3SB H 0.8036 0.4097 0.8668 0.046 Uiso 1 1 d R . . O4S O 0.6952(11) 0.0125(9) 0.8947(9) 0.055(5) Uani 1 1 d . . . H4SA H 0.6662 0.0431 0.9172 0.066 Uiso 1 1 d R . . H4SB H 0.6733 -0.0179 0.8651 0.066 Uiso 1 1 d 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 Br1 0.0496(14) 0.0620(16) 0.0716(18) 0.0156(13) 0.0282(13) -0.0003(12) Br2 0.0302(8) 0.0302(8) 0.0302(8) -0.0022(7) 0.0022(7) 0.0022(7) Br3 0.0386(9) 0.0386(9) 0.0386(9) 0.0005(9) 0.0005(9) 0.0005(9) Br4 0.0784(16) 0.0784(16) 0.0784(16) 0.0023(17) 0.0023(17) -0.0023(17) S1 0.023(2) 0.021(2) 0.031(2) 0.0034(18) -0.0005(18) -0.0006(17) N1 0.024(5) 0.024(5) 0.024(5) 0.000(6) 0.000(6) 0.000(6) C2 0.051(12) 0.036(11) 0.011(8) 0.001(7) 0.018(8) 0.011(9) C3 0.027(9) 0.036(10) 0.014(8) 0.003(7) 0.005(7) 0.008(8) N4 0.029(8) 0.028(8) 0.025(8) -0.001(6) -0.017(7) 0.002(7) C5 0.006(7) 0.071(14) 0.017(8) -0.014(9) -0.006(7) 0.004(8) C6 0.023(9) 0.025(9) 0.025(9) 0.010(7) -0.011(7) -0.007(7) C7 0.013(8) 0.044(12) 0.021(9) 0.001(8) -0.004(7) 0.012(8) C8 0.041(11) 0.026(10) 0.011(7) 0.002(7) -0.010(7) 0.009(8) C9 0.026(8) 0.014(7) 0.021(9) 0.003(6) -0.019(7) 0.000(7) C10 0.011(7) 0.033(9) 0.008(7) 0.003(6) 0.003(6) 0.003(6) N11 0.049(10) 0.035(9) 0.023(8) -0.011(7) -0.019(7) 0.029(8) C12 0.030(10) 0.043(12) 0.050(13) -0.002(10) 0.009(9) 0.032(9) C13 0.056(15) 0.068(16) 0.036(12) -0.014(11) 0.008(11) 0.002(13) N14 0.020(5) 0.020(5) 0.020(5) -0.006(6) 0.006(6) 0.006(6) O1S 0.071(12) 0.062(11) 0.050(10) 0.003(9) 0.012(9) 0.003(10) O2S 0.079(12) 0.040(8) 0.032(8) 0.005(7) 0.009(8) 0.000(8) O3S 0.046(8) 0.031(7) 0.038(7) -0.004(6) -0.009(6) 0.013(7) O4S 0.088(13) 0.043(9) 0.034(8) 0.000(7) -0.018(8) -0.031(9) _geom_special_details ; ; 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 C9 1.713(16) . ? S1 C6 1.757(19) . ? N1 C2 1.47(2) . ? N1 C2 1.47(2) 7_665 ? N1 C2 1.47(2) 10_646 ? C2 C3 1.50(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 N4 1.52(2) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? N4 C5 1.52(2) . ? N4 H4A 0.9200 . ? N4 H4B 0.9200 . ? C5 C6 1.48(3) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.26(3) . ? C7 C8 1.47(3) . ? C7 H7 0.9500 . ? C8 C9 1.39(3) . ? C8 H8 0.9500 . ? C9 C10 1.48(2) . ? C10 N11 1.50(2) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? N11 C12 1.50(2) . ? N11 H11A 0.9200 . ? N11 H11B 0.9200 . ? C12 C13 1.55(3) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 N14 1.46(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? N14 C13 1.46(3) 7_665 ? N14 C13 1.46(3) 10_646 ? O1S H1SA 0.8500 . ? O1S H1SB 0.8498 . ? O2S H2SA 0.8499 . ? O2S H2SB 0.8501 . ? O3S H3SA 0.8500 . ? O3S H3SB 0.8500 . ? O4S H4SA 0.8500 . ? O4S H4SB 0.8499 . ? 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 C9 S1 C6 90.6(9) . . ? C2 N1 C2 109.0(12) . 7_665 ? C2 N1 C2 109.0(12) . 10_646 ? C2 N1 C2 109.0(12) 7_665 10_646 ? N1 C2 C3 116.4(15) . . ? N1 C2 H2A 108.2 . . ? C3 C2 H2A 108.2 . . ? N1 C2 H2B 108.2 . . ? C3 C2 H2B 108.2 . . ? H2A C2 H2B 107.3 . . ? C2 C3 N4 109.8(15) . . ? C2 C3 H3A 109.7 . . ? N4 C3 H3A 109.7 . . ? C2 C3 H3B 109.7 . . ? N4 C3 H3B 109.7 . . ? H3A C3 H3B 108.2 . . ? C5 N4 C3 113.4(14) . . ? C5 N4 H4A 108.9 . . ? C3 N4 H4A 108.9 . . ? C5 N4 H4B 108.9 . . ? C3 N4 H4B 108.9 . . ? H4A N4 H4B 107.7 . . ? C6 C5 N4 112.3(14) . . ? C6 C5 H5A 109.1 . . ? N4 C5 H5A 109.1 . . ? C6 C5 H5B 109.1 . . ? N4 C5 H5B 109.1 . . ? H5A C5 H5B 107.9 . . ? C7 C6 C5 128.8(18) . . ? C7 C6 S1 111.7(15) . . ? C5 C6 S1 119.4(14) . . ? C6 C7 C8 116.6(18) . . ? C6 C7 H7 121.7 . . ? C8 C7 H7 121.7 . . ? C9 C8 C7 107.9(16) . . ? C9 C8 H8 126.0 . . ? C7 C8 H8 126.0 . . ? C8 C9 C10 125.8(15) . . ? C8 C9 S1 113.1(14) . . ? C10 C9 S1 121.0(13) . . ? C9 C10 N11 111.2(13) . . ? C9 C10 H10A 109.4 . . ? N11 C10 H10A 109.4 . . ? C9 C10 H10B 109.4 . . ? N11 C10 H10B 109.4 . . ? H10A C10 H10B 108.0 . . ? C12 N11 C10 111.6(14) . . ? C12 N11 H11A 109.3 . . ? C10 N11 H11A 109.3 . . ? C12 N11 H11B 109.3 . . ? C10 N11 H11B 109.3 . . ? H11A N11 H11B 108.0 . . ? N11 C12 C13 114.0(17) . . ? N11 C12 H12A 108.8 . . ? C13 C12 H12A 108.8 . . ? N11 C12 H12B 108.7 . . ? C13 C12 H12B 108.8 . . ? H12A C12 H12B 107.6 . . ? N14 C13 C12 114(2) . . ? N14 C13 H13A 108.7 . . ? C12 C13 H13A 108.7 . . ? N14 C13 H13B 108.7 . . ? C12 C13 H13B 108.7 . . ? H13A C13 H13B 107.6 . . ? C13 N14 C13 107.1(13) 7_665 . ? C13 N14 C13 107.1(13) 7_665 10_646 ? C13 N14 C13 107.1(13) . 10_646 ? H1SA O1S H1SB 108.0 . . ? H2SA O2S H2SB 93.7 . . ? H3SA O3S H3SB 127.1 . . ? H4SA O4S H4SB 114.9 . . ? 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 C2 N1 C2 C3 166.9(17) 7_665 . . . ? C2 N1 C2 C3 -74(3) 10_646 . . . ? N1 C2 C3 N4 -66(2) . . . . ? C2 C3 N4 C5 -162.6(16) . . . . ? C3 N4 C5 C6 178.4(15) . . . . ? N4 C5 C6 C7 -77(2) . . . . ? N4 C5 C6 S1 98.8(17) . . . . ? C9 S1 C6 C7 -0.9(14) . . . . ? C9 S1 C6 C5 -177.4(13) . . . . ? C5 C6 C7 C8 177.4(16) . . . . ? S1 C6 C7 C8 1(2) . . . . ? C6 C7 C8 C9 -1(2) . . . . ? C7 C8 C9 C10 178.0(15) . . . . ? C7 C8 C9 S1 0.3(17) . . . . ? C6 S1 C9 C8 0.2(13) . . . . ? C6 S1 C9 C10 -177.6(13) . . . . ? C8 C9 C10 N11 90.3(19) . . . . ? S1 C9 C10 N11 -92.1(16) . . . . ? C9 C10 N11 C12 -169.8(16) . . . . ? C10 N11 C12 C13 163.3(19) . . . . ? N11 C12 C13 N14 52(3) . . . . ? C12 C13 N14 C13 -171.0(18) . . . 7_665 ? C12 C13 N14 C13 74(3) . . . 10_646 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N4 H4B O3S 0.92 1.87 2.75(2) 160.6 . N4 H4A O3S 0.92 2.25 2.83(2) 120.5 7_665 N4 H4A Br1 0.92 2.75 3.425(17) 131.5 . N11 H11A O2S 0.92 1.89 2.79(3) 165.4 . N11 H11B O2S 0.92 2.11 2.92(2) 146.9 10_646 N11 H11B Br2 0.92 2.92 3.484(15) 121.2 . O1S H1SA Br1 0.85 2.42 3.265(19) 179.6 . O1S H1SB Br4 0.85 2.21 3.06(2) 179.8 4_457 O2S H2SA O4S 0.85 1.93 2.77(2) 167.3 . O2S H2SB Br2 0.85 2.81 3.656(16) 179.5 . O3S H3SA Br2 0.85 2.43 3.281(14) 179.8 . O3S H3SB O1S 0.85 1.91 2.76(2) 179.0 10_646 O4S H4SA O1S 0.85 1.81 2.66(3) 179.1 . O4S H4SB Br1 0.85 2.53 3.378(15) 179.6 6_456 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.38 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.268 _refine_diff_density_min -2.225 _refine_diff_density_rms 0.318 _iucr_refine_instruction_details ; TITL 10069 in P2(1)3 CELL 0.71073 17.7890 17.7890 17.7890 90.000 90.000 90.000 ZERR 4.00 0.0009 0.0009 0.0009 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 SYMM Z, X, Y SYMM 0.5+Z, 0.5-X, -Y SYMM 0.5-Z, -X, 0.5+Y SYMM -Z, 0.5+X, 0.5-Y SYMM Y, Z, X SYMM -Y, 0.5+Z, 0.5-X SYMM 0.5+Y, 0.5-Z, -X SYMM 0.5-Y, -Z, 0.5+X SFAC C H N O S BR UNIT 120 312 32 48 12 24 TEMP -173 SIZE 0.36 0.54 0.58 shel 10 0.86 acta 50 conf wpdb -2 eqiv $1 -z+3/2, -x+1, y+1/2 eqiv $2 -y+1, z-1/2, -x+3/2 eqiv $3 x-1/2, -y+1/2, -z+2 eqiv $4 z-1/2, -x+1/2, -y+1 htab n4 o3s htab n4 o3s_$1 htab n4 br1 htab n11 o2s htab n11 o2s_$2 htab n11 br2 htab o1s br1 htab o1s br4_$3 htab o2s o4s htab o2s br2 htab o3s br2 htab o3s o1s_$2 htab o4s o1s htab o4s br1_$4 htab L.S. 4 BOND $h FMAP 2 PLAN 20 twin WGHT 0.180000 120.000000 BASF 0.11902 FVAR 0.18732 BR1 6 0.608337 0.223644 1.108830 11.00000 0.04956 0.06204 = 0.07160 0.01564 0.02816 -0.00025 BR2 6 0.760259 0.239741 0.739742 10.33333 0.03020 0.03020 = 0.03020 -0.00223 0.00223 0.00223 BR3 6 0.928466 0.928466 0.928466 10.33333 0.03863 0.03863 = 0.03863 0.00051 0.00051 0.00051 BR4 6 0.943171 0.443171 1.056829 10.33333 0.07841 0.07841 = 0.07841 0.00233 0.00233 -0.00233 S1 5 0.887940 0.259696 0.923640 11.00000 0.02318 0.02111 = 0.03076 0.00336 -0.00053 -0.00064 N1 3 0.575149 0.424851 0.924851 10.33333 0.02434 0.02434 = 0.02434 0.00022 -0.00022 -0.00022 C2 1 0.590095 0.408852 1.004748 11.00000 0.05055 0.03573 = 0.01122 0.00072 0.01797 0.01091 AFIX 23 H2A 2 0.565730 0.360506 1.017639 11.00000 -1.20000 H2B 2 0.565613 0.448428 1.035268 11.00000 -1.20000 AFIX 0 C3 1 0.671245 0.404382 1.027582 11.00000 0.02713 0.03558 = 0.01444 0.00260 0.00549 0.00767 AFIX 23 H3A 2 0.674928 0.399170 1.082867 11.00000 -1.20000 H3B 2 0.697522 0.451143 1.012746 11.00000 -1.20000 AFIX 0 N4 3 0.708318 0.337187 0.989723 11.00000 0.02888 0.02822 = 0.02521 -0.00147 -0.01746 0.00167 AFIX 23 H4A 2 0.675630 0.297128 0.990948 11.00000 -1.20000 H4B 2 0.717233 0.348728 0.940104 11.00000 -1.20000 AFIX 0 C5 1 0.781683 0.314053 1.026276 11.00000 0.00558 0.07125 = 0.01725 -0.01392 -0.00639 0.00433 AFIX 23 H5A 2 0.817571 0.356505 1.023614 11.00000 -1.20000 H5B 2 0.772536 0.302778 1.080001 11.00000 -1.20000 AFIX 0 C6 1 0.815604 0.247280 0.989745 11.00000 0.02279 0.02515 = 0.02468 0.00972 -0.01059 -0.00667 C7 1 0.797278 0.178894 0.996132 11.00000 0.01261 0.04365 = 0.02136 0.00093 -0.00407 0.01181 AFIX 43 H7 2 0.758228 0.163279 1.029045 11.00000 -1.20000 AFIX 0 C8 1 0.839310 0.124943 0.950210 11.00000 0.04110 0.02630 = 0.01134 0.00154 -0.01014 0.00890 AFIX 43 H8 2 0.832354 0.071997 0.949689 11.00000 -1.20000 AFIX 0 C9 1 0.890993 0.164790 0.907681 11.00000 0.02601 0.01375 = 0.02145 0.00331 -0.01917 0.00043 C10 1 0.946589 0.131903 0.855183 11.00000 0.01085 0.03306 = 0.00773 0.00342 0.00278 0.00329 AFIX 23 H10A 2 0.961499 0.081439 0.873300 11.00000 -1.20000 H10B 2 0.992102 0.163911 0.854045 11.00000 -1.20000 AFIX 0 N11 3 0.914857 0.125435 0.777043 11.00000 0.04894 0.03528 = 0.02251 -0.01068 -0.01867 0.02855 AFIX 23 H11A 2 0.868229 0.103178 0.779308 11.00000 -1.20000 H11B 2 0.908990 0.172746 0.756996 11.00000 -1.20000 AFIX 0 C12 1 0.965193 0.079811 0.726748 11.00000 0.02964 0.04337 = 0.04958 -0.00248 0.00874 0.03208 AFIX 23 H12A 2 0.983848 0.035810 0.755262 11.00000 -1.20000 H12B 2 1.009274 0.110754 0.712725 11.00000 -1.20000 AFIX 0 C13 1 0.926316 0.051559 0.653733 11.00000 0.05580 0.06836 = 0.03613 -0.01358 0.00826 0.00231 AFIX 23 H13A 2 0.964474 0.026955 0.621549 11.00000 -1.20000 H13B 2 0.888454 0.013121 0.667379 11.00000 -1.20000 AFIX 0 N14 3 0.889518 0.110482 0.610482 10.33333 0.01976 0.01976 = 0.01976 -0.00623 0.00623 0.00623 O1S 4 0.605731 0.109068 0.965445 11.00000 0.07094 0.06244 = 0.04984 0.00307 0.01203 0.00343 AFIX 3 H1SA 2 0.606661 0.138817 1.002825 11.00000 -1.20000 H1SB 2 0.560671 0.094438 0.959295 11.00000 -1.20000 AFIX 0 O2S 4 0.784917 0.037978 0.769981 11.00000 0.07885 0.03975 = 0.03191 0.00536 0.00892 0.00007 AFIX 3 H2SA 2 0.757167 0.037508 0.808871 11.00000 -1.20000 H2SB 2 0.779167 0.084848 0.762651 11.00000 -1.20000 AFIX 0 O3S 4 0.765118 0.384546 0.853854 11.00000 0.04580 0.03069 = 0.03778 -0.00379 -0.00940 0.01341 AFIX 3 H3SA 2 0.763718 0.347046 0.824274 11.00000 -1.20000 H3SB 2 0.803648 0.409676 0.866784 11.00000 -1.20000 AFIX 0 O4S 4 0.695246 0.012496 0.894681 11.00000 0.08846 0.04293 = 0.03393 -0.00021 -0.01787 -0.03094 AFIX 3 H4SA 2 0.666246 0.043096 0.917171 11.00000 -1.20000 H4SB 2 0.673336 -0.017924 0.865061 11.00000 -1.20000 HKLF 4 REM 10069 in P2(1)3 REM R1 = 0.1191 for 2791 Fo > 4sig(Fo) and 0.1269 for all 3105 data REM 179 parameters refined using 0 restraints END WGHT 0.1581 175.3251 REM Highest difference peak 2.268, deepest hole -2.225, 1-sigma level 0.318 Q1 1 0.7214 0.2786 0.7786 10.33333 0.05 2.27 Q2 1 0.9252 0.4442 1.0025 11.00000 0.05 2.19 Q3 1 0.7804 0.2804 1.2196 10.33333 0.05 1.97 Q4 1 1.1050 0.1956 0.7321 11.00000 0.05 1.63 Q5 1 0.7375 0.2723 1.2018 11.00000 0.05 1.47 Q6 1 0.8542 -0.0916 0.7633 11.00000 0.05 1.40 Q7 1 0.9100 0.4100 1.0900 10.33333 0.05 1.40 Q8 1 0.8565 0.0295 0.6068 11.00000 0.05 1.36 Q9 1 0.8941 1.0076 0.9266 11.00000 0.05 1.20 Q10 1 0.5616 0.1821 1.1160 11.00000 0.05 1.15 Q11 1 0.8914 0.8914 0.8914 10.33333 0.05 1.06 Q12 1 0.7651 0.1986 0.7932 11.00000 0.05 1.03 Q13 1 0.6015 0.1517 1.0652 11.00000 0.05 1.00 Q14 1 0.6170 0.1224 1.0663 11.00000 0.05 0.94 Q15 1 0.7745 0.2583 0.6907 11.00000 0.05 0.93 Q16 1 0.7640 0.4397 1.0978 11.00000 0.05 0.90 Q17 1 0.9974 0.1317 0.8756 11.00000 0.05 0.90 Q18 1 0.7730 0.4376 1.0701 11.00000 0.05 0.88 Q19 1 0.9744 0.4070 1.1010 11.00000 0.05 0.86 Q20 1 0.6758 0.4364 1.0552 11.00000 0.05 0.85 #===END ;