Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_sean24a _database_code_CSD 188681 _journal_coden_Cambridge 182 loop_ _publ_author_name 'Shimizu, George' 'Dalrymple, Sean A.' _publ_contact_author_name 'Prof George Shimizu' _publ_contact_author_address ; Chemistry University of Calgary 2500 University Drive N.W. Calgary Alberta T2N 1N4 CANADA ; _publ_contact_author_email 'GSHIMIZU@UCALGARY.CA' _publ_requested_journal 'Chemical Communications' _publ_section_title ; An open channel coordination framework sustained by cooperative primary and secondary sphere interactions ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H24 Al2 O38.33 S6' _chemical_formula_weight 1027.97 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Al' 'Al' 0.0645 0.0514 '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 Trigonal _symmetry_space_group_name_H-M R-3m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z' 'x-y, -y, -z' '-x, -x+y, -z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+1/3' 'x-y+2/3, -y+1/3, -z+1/3' '-x+2/3, -x+y+1/3, -z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+2/3' 'x-y+1/3, -y+2/3, -z+2/3' '-x+1/3, -x+y+2/3, -z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z' '-x+y, y, z' 'x, x-y, z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-y+2/3, -x+1/3, z+1/3' '-x+y+2/3, y+1/3, z+1/3' 'x+2/3, x-y+1/3, z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-y+1/3, -x+2/3, z+2/3' '-x+y+1/3, y+2/3, z+2/3' 'x+1/3, x-y+2/3, z+2/3' _cell_length_a 11.9858(17) _cell_length_b 11.9858(17) _cell_length_c 24.641(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3065.7(9) _cell_formula_units_Z 3 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.670 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1574 _exptl_absorpt_coefficient_mu 0.494 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.8864 _exptl_absorpt_correction_T_max 0.9296 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'omega - phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5856 _diffrn_reflns_av_R_equivalents 0.0575 _diffrn_reflns_av_sigmaI/netI 0.0433 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.85 _diffrn_reflns_theta_max 27.47 _reflns_number_total 877 _reflns_number_gt 650 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_cell_refinement 'DENZO (Nonius, 1998)' _computing_data_reduction 'DENZO (Nonius, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'DIAMOND 2.1 (Crystal Impact)' _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^)+(0.1139P)^2^+12.9772P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 877 _refine_ls_number_parameters 63 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0884 _refine_ls_R_factor_gt 0.0663 _refine_ls_wR_factor_ref 0.1978 _refine_ls_wR_factor_gt 0.1805 _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_restrained_S_all 1.094 _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 0.50937(6) 0.01874(12) 0.09991(4) 0.0267(5) Uani 1 2 d S . . Al1 Al 0.6667 0.3333 0.04674(13) 0.0436(9) Uani 1 6 d S . . O1 O 0.5888(3) -0.0248(3) 0.07281(10) 0.0369(8) Uani 1 1 d . . . O2 O 0.57882(18) 0.1576(4) 0.10893(15) 0.0408(11) Uani 1 2 d S . . O3 O 0.7612(2) 0.2388(2) -0.00739(16) 0.0407(10) Uani 1 2 d S . . H1A H 0.7030 0.1907 -0.0373 0.061 Uiso 0.50 1 calc PR . . H1B H 0.7765 0.1800 0.0149 0.061 Uiso 0.50 1 calc PR . . H1C H 0.8433 0.3066 -0.0221 0.061 Uiso 0.00 1 calc PR . . C1 C 0.4013(2) -0.1975(4) 0.16635(16) 0.0149(9) Uani 1 2 d S . . C2 C 0.4749(2) -0.0501(4) 0.16640(18) 0.0218(10) Uani 1 2 d S . . H2A H 0.5570 -0.0193 0.1862 0.033 Uiso 0.50 1 calc PR . . H2B H 0.4236 -0.0193 0.1862 0.033 Uiso 0.50 1 calc PR . . O4S O 0.8167(3) 0.1833(3) 0.07720(17) 0.0474(12) Uani 1 2 d S . . O5S O 0.8100(5) 0.1900(5) 0.1690(5) 0.062(3) Uiso 0.50 2 d SP . . O6S O 0.9166(9) 0.0834(9) 0.0406(7) 0.060(4) Uiso 0.30 2 d SP . . O7S O 0.6933(7) 0.3067(7) 0.2165(7) 0.061(5) Uiso 0.30 2 d SP . . O8S O 0.7351(19) 0.0464(17) 0.0073(8) 0.041(5) Uiso 0.15 1 d P . . 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 0.0364(7) 0.0171(7) 0.0202(6) 0.0019(4) 0.0009(2) 0.0086(3) Al1 0.0461(13) 0.0461(13) 0.0386(17) 0.000 0.000 0.0230(6) O1 0.0495(18) 0.0333(15) 0.0252(13) 0.0031(11) 0.0086(11) 0.0187(13) O2 0.061(2) 0.0161(19) 0.030(2) 0.0051(14) 0.0025(7) 0.0080(9) O3 0.0450(18) 0.0450(18) 0.034(2) -0.0027(9) 0.0027(9) 0.024(2) C1 0.0160(16) 0.014(2) 0.0142(18) 0.0003(15) 0.0002(7) 0.0068(10) C2 0.0270(19) 0.013(2) 0.020(2) -0.0014(17) -0.0007(8) 0.0067(11) O4S 0.0431(18) 0.0431(18) 0.040(2) 0.0069(11) -0.0069(11) 0.009(2) _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 O1 1.457(3) 23_655 ? S1 O1 1.457(3) . ? S1 O2 1.459(4) . ? S1 C2 1.788(5) . ? Al1 O3 2.374(5) . ? Al1 O3 2.374(5) 3_665 ? Al1 O3 2.374(5) 2_655 ? Al1 O2 2.382(4) 2_655 ? Al1 O2 2.382(4) . ? Al1 O2 2.382(4) 3_665 ? C1 C1 1.410(4) 26 ? C1 C1 1.410(4) 27_445 ? C1 C2 1.530(6) . ? O5S O5S 0.973(19) 25_655 ? O7S O7S 0.96(3) 2_655 ? O7S O7S 0.96(3) 3_665 ? O8S O8S 1.03(3) 5 ? 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 O1 S1 O1 112.8(2) 23_655 . ? O1 S1 O2 112.12(14) 23_655 . ? O1 S1 O2 112.12(14) . . ? O1 S1 C2 107.22(13) 23_655 . ? O1 S1 C2 107.22(13) . . ? O2 S1 C2 104.8(2) . . ? O3 Al1 O3 91.51(17) . 3_665 ? O3 Al1 O3 91.51(17) . 2_655 ? O3 Al1 O3 91.51(17) 3_665 2_655 ? O3 Al1 O2 92.57(10) . 2_655 ? O3 Al1 O2 174.15(19) 3_665 2_655 ? O3 Al1 O2 92.57(10) 2_655 2_655 ? O3 Al1 O2 92.57(10) . . ? O3 Al1 O2 92.57(10) 3_665 . ? O3 Al1 O2 174.15(19) 2_655 . ? O2 Al1 O2 83.06(16) 2_655 . ? O3 Al1 O2 174.15(19) . 3_665 ? O3 Al1 O2 92.57(10) 3_665 3_665 ? O3 Al1 O2 92.57(10) 2_655 3_665 ? O2 Al1 O2 83.06(16) 2_655 3_665 ? O2 Al1 O2 83.06(16) . 3_665 ? S1 O2 Al1 131.2(2) . . ? C1 C1 C1 119.989(14) 26 27_445 ? C1 C1 C2 119.997(6) 26 . ? C1 C1 C2 119.995(6) 27_445 . ? C1 C2 S1 113.5(3) . . ? O7S O7S O7S 60.000(4) 2_655 3_665 ? 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 O1 S1 O2 Al1 -64.03(15) 23_655 . . . ? O1 S1 O2 Al1 64.03(15) . . . . ? C2 S1 O2 Al1 180.0 . . . . ? O3 Al1 O2 S1 -45.81(8) . . . . ? O3 Al1 O2 S1 45.81(8) 3_665 . . . ? O3 Al1 O2 S1 180.000(5) 2_655 . . . ? O2 Al1 O2 S1 -138.09(7) 2_655 . . . ? O2 Al1 O2 S1 138.09(7) 3_665 . . . ? C1 C1 C2 S1 90.8(5) 26 . . . ? C1 C1 C2 S1 -90.8(5) 27_445 . . . ? O1 S1 C2 C1 60.69(14) 23_655 . . . ? O1 S1 C2 C1 -60.69(14) . . . . ? O2 S1 C2 C1 180.0 . . . . ? 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 O3 H1A O1 0.98 1.93 2.787(4) 144.2 5 O3 H1B O8S 0.98 1.43 2.196(19) 130.1 . O3 H1B O4S 0.98 1.60 2.381(6) 132.9 . O3 H1B O8S 0.98 2.43 3.076(18) 122.9 5 O3 H1B O6S 0.98 2.55 3.436(19) 150.2 . O3 H1C O1 0.98 1.86 2.787(4) 156.6 20_665 O3 H1C O8S 0.98 2.43 3.076(19) 122.7 20_665 _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 1.172 _refine_diff_density_min -0.730 _refine_diff_density_rms 0.122