Electronic Supplementary Material for CrystEngComm This Journal is (c) The Royal Society of Chemistry 2007 data_global _journal_coden_Cambridge 1350 loop_ _publ_author_name 'A Nangia' 'Bipul Sarma' _publ_contact_author_name 'A. Nangia' _publ_contact_author_address ; School of Chemistry University of Hyderabad P O Central University 500046 Hyderabad INDIA ; _publ_contact_author_email ASHWINI_NANGIA@REDIFFMAIL.COM _publ_requested_journal CrystEngComm _publ_section_title ; Tetrakis(4-sulfophenyl)methane dodecahydrate. Reversible and selective water inclusion and release in an organic host ; data_an230_m _database_code_depnum_ccdc_archive 'CCDC 644921' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Tetrakis-(4-sulfonatophenyl)methane ; _chemical_name_common Tetrakis-(4-sulfonatophenyl)methane _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H32 O44 S8' _chemical_formula_weight 1593.24 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I4(1)/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 21.8492(12) _cell_length_b 21.8492(12) _cell_length_c 7.3635(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3515.2(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1085 _cell_measurement_theta_min 2.92 _cell_measurement_theta_max 19.50 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.505 _exptl_crystal_density_method ? _exptl_crystal_F_000 1624 _exptl_absorpt_coefficient_mu 0.357 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9320 _exptl_absorpt_correction_T_max 0.9720 _exptl_absorpt_process_details SADABS _exptl_special_details ; GM Sheldrick, University of Gottingen, Germany ; _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 area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9316 _diffrn_reflns_av_R_equivalents 0.0727 _diffrn_reflns_av_sigmaI/netI 0.0581 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.64 _diffrn_reflns_theta_max 26.07 _reflns_number_total 1696 _reflns_number_gt 1108 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1042P)^2^+2.0123P] 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 1696 _refine_ls_number_parameters 155 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1272 _refine_ls_R_factor_gt 0.0818 _refine_ls_wR_factor_ref 0.2067 _refine_ls_wR_factor_gt 0.1821 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.084 _refine_ls_shift/su_max 0.183 _refine_ls_shift/su_mean 0.001 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 0.10486(7) 0.43998(6) 0.10817(19) 0.0620(5) Uani 1 1 d . . . C7 C 0.0000 0.2500 0.6250 0.0301(17) Uani 1 4 d S . . C3 C -0.0073(2) 0.32400(19) 0.3629(6) 0.0370(10) Uani 1 1 d . . . C2 C 0.0148(2) 0.36685(19) 0.2442(6) 0.0381(10) Uani 1 1 d . . . O2 O 0.0636(2) 0.49047(15) 0.1149(5) 0.0755(18) Uani 1.000(13) 1 d . . . C6 C 0.1135(2) 0.3585(2) 0.3870(6) 0.0417(11) Uani 1 1 d . . . C5 C 0.0902(2) 0.3152(2) 0.5053(6) 0.0383(10) Uani 1 1 d . . . O4 O 0.0353(2) 0.47343(17) 0.6890(5) 0.0773(12) Uani 1 1 d . . . C4 C 0.02913(18) 0.29826(17) 0.4977(5) 0.0320(9) Uani 1 1 d . . . C1 C 0.0762(2) 0.38448(18) 0.2588(6) 0.0409(10) Uani 1 1 d . . . O1B O 0.1714(3) 0.4457(3) 0.1421(10) 0.083(2) Uani 0.70 1 d P . . O5 O 0.1098(3) 0.54172(19) 0.5391(6) 0.0963(15) Uani 1 1 d . . . O3 O 0.1053(2) 0.41219(18) -0.0701(5) 0.0927(16) Uani 1 1 d . . . O6A O 0.2266(9) 0.5081(11) 0.464(4) 0.092(8) Uani 0.25 1 d P A 1 O6B O 0.2097(10) 0.5134(11) 0.371(4) 0.085(7) Uani 0.25 1 d P B 2 H5 H 0.114(2) 0.301(2) 0.594(6) 0.041(12) Uiso 1 1 d . . . H6 H 0.157(2) 0.3734(18) 0.382(5) 0.036(11) Uiso 1 1 d . . . H3 H -0.047(2) 0.3169(18) 0.366(5) 0.030(11) Uiso 1 1 d . . . H2 H -0.010(2) 0.386(2) 0.164(7) 0.052(14) Uiso 1 1 d . . . O1A O 0.1492(5) 0.4750(5) 0.2345(16) 0.051(3) Uani 0.30 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 0.0660(10) 0.0497(8) 0.0701(10) 0.0239(7) -0.0019(7) -0.0170(7) C7 0.024(2) 0.024(2) 0.042(5) 0.000 0.000 0.000 C3 0.031(2) 0.039(2) 0.040(2) -0.0009(18) 0.0007(18) -0.0027(18) C2 0.040(2) 0.036(2) 0.039(2) -0.0025(19) -0.0038(19) 0.0016(19) O2 0.131(4) 0.035(2) 0.060(3) 0.0091(16) 0.009(2) 0.003(2) C6 0.035(2) 0.040(2) 0.049(3) 0.004(2) 0.001(2) -0.004(2) C5 0.035(2) 0.040(2) 0.040(3) -0.0027(19) 0.0012(19) 0.0007(18) O4 0.127(4) 0.048(2) 0.057(2) -0.0065(17) 0.000(2) 0.002(2) C4 0.036(2) 0.027(2) 0.033(2) -0.0051(16) 0.0020(17) 0.0024(16) C1 0.047(3) 0.030(2) 0.045(3) 0.0002(18) 0.005(2) -0.0088(19) O1B 0.071(4) 0.074(4) 0.103(5) 0.035(4) 0.027(4) -0.010(3) O5 0.151(5) 0.071(3) 0.067(3) -0.002(2) -0.002(3) 0.000(3) O3 0.153(4) 0.058(2) 0.067(3) 0.026(2) 0.047(3) 0.024(3) O6A 0.052(12) 0.093(16) 0.13(2) -0.051(17) -0.034(12) 0.026(10) O6B 0.058(14) 0.090(14) 0.106(19) 0.019(12) -0.034(12) 0.019(10) O1A 0.049(7) 0.053(7) 0.053(7) 0.016(6) -0.009(5) -0.025(6) _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 O2 1.425(4) . ? S1 O3 1.446(4) . ? S1 O1B 1.480(7) . ? S1 O1A 1.546(11) . ? S1 C1 1.759(4) . ? C7 C4 1.548(4) . ? C7 C4 1.548(4) 6_454 ? C7 C4 1.548(4) 15_556 ? C7 C4 1.548(4) 12_667 ? C3 C2 1.369(6) . ? C3 C4 1.391(6) . ? C3 H3 0.87(4) . ? C2 C1 1.400(6) . ? C2 H2 0.90(5) . ? C6 C1 1.370(6) . ? C6 C5 1.382(6) . ? C6 H6 1.01(4) . ? C5 C4 1.386(6) . ? C5 H5 0.89(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 O2 S1 O3 111.2(2) . . ? O2 S1 O1B 123.3(4) . . ? O3 S1 O1B 100.5(4) . . ? O2 S1 O1A 89.6(5) . . ? O3 S1 O1A 138.5(6) . . ? O1B S1 O1A 40.6(5) . . ? O2 S1 C1 106.7(2) . . ? O3 S1 C1 106.6(2) . . ? O1B S1 C1 107.5(3) . . ? O1A S1 C1 100.7(4) . . ? C4 C7 C4 105.5(3) . 6_454 ? C4 C7 C4 111.51(14) . 15_556 ? C4 C7 C4 111.51(14) 6_454 15_556 ? C4 C7 C4 111.51(14) . 12_667 ? C4 C7 C4 111.51(14) 6_454 12_667 ? C4 C7 C4 105.5(3) 15_556 12_667 ? C2 C3 C4 122.1(4) . . ? C2 C3 H3 119(3) . . ? C4 C3 H3 118(3) . . ? C3 C2 C1 118.4(4) . . ? C3 C2 H2 121(3) . . ? C1 C2 H2 120(3) . . ? C1 C6 C5 120.0(4) . . ? C1 C6 H6 114(2) . . ? C5 C6 H6 126(2) . . ? C6 C5 C4 120.8(4) . . ? C6 C5 H5 119(3) . . ? C4 C5 H5 120(3) . . ? C5 C4 C3 118.1(4) . . ? C5 C4 C7 123.6(3) . . ? C3 C4 C7 118.2(3) . . ? C6 C1 C2 120.6(4) . . ? C6 C1 S1 120.6(3) . . ? C2 C1 S1 118.8(3) . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 26.07 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 0.475 _refine_diff_density_min -0.264 _refine_diff_density_rms 0.079