Supplementary Material for CrystEngComm This journal is © The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 1350 loop_ _publ_author_name 'Lars Ohrstrom' 'Krister Larsson' _publ_contact_author_name 'Dr Lars Ohrstrom' _publ_contact_author_address ; Dept. of Materials and Surface Chemistry Chalmers Tekniska Högskola Inorganic Chemistry Göteborg SE-412 96 SWEDEN ; _publ_contact_author_email OHRSTROM@INOC.CHALMERS.SE _publ_requested_journal 'Cryst Eng. Comm.' _publ_section_title ; A (10,3)-b Net by Sulphate Hydrogen-Bonded Biimidazolate Complexes ; _ccdc_compound_id ? _ccdc_biological_activity ? _ccdc_polymorph ? _ccdc_chemdiag_type ? _ccdc_chemdiag_records ; ? ; data_crbiim2 _database_code_CSD 206283 _audit_creation_date 2002-10-25T13:01:44-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C18 H15 Cr1 N12' _chemical_formula_sum 'C18 H15 Cr N12 O4 S' _chemical_formula_weight 547.48 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'I 41' _symmetry_space_group_name_Hall 'I 4bw' _symmetry_Int_Tables_number 80 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x+1/2, z+1/4' 'y, -x+1/2, z+1/4' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-y+1/2, x+1, z+3/4' 'y+1/2, -x+1, z+3/4' _cell_length_a 12.8274(7) _cell_length_b 12.8274(7) _cell_length_c 14.2567(7) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2345.8(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5528 _cell_measurement_theta_min 2.75 _cell_measurement_theta_max 36.99 _cell_measurement_wavelength 0.924 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description rod _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.06 _exptl_crystal_density_diffrn 1.55 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1116 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.251 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Shape and scale corrections using equivalent reflections. Shape function based on spherical harmonics. Highest even and odd order for spherical harmonics: 4 and 1 Laue group: 4/m Friedel opposites are equivalent. ; _exptl_absorpt_correction_T_min 0.2811 _exptl_absorpt_correction_T_max 1.0000 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.9240 _diffrn_radiation_monochromator 'Si (111) single crystal' _diffrn_radiation_probe x-ray _diffrn_radiation_type synchrotron _diffrn_reflns_av_sigmaI/netI 0.009 _diffrn_reflns_av_R_equivalents 0.120 _diffrn_reflns_number 6527 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 36.6 _diffrn_reflns_theta_full 36.6 _diffrn_measured_fraction_theta_full 0.9044 _diffrn_measured_fraction_theta_max 0.8746 _reflns_number_total 1966 _reflns_number_gt 1870 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'Twinsolve (Rigaku, 1998-2002)' _computing_data_reduction 'Twinsolve (Rigaku, 1998-2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; Ortep-3 for Windows (Farrugia, 1997) DIAMOND - Visual Crystal Structure Information System CRYSTAL IMPACT, Postfach 1251, D-53002 Bonn ; #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.1640P)^2^+0.6264P] 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_number_reflns 1966 _refine_ls_number_parameters 164 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0707 _refine_ls_R_factor_gt 0.0692 _refine_ls_wR_factor_ref 0.2001 _refine_ls_wR_factor_gt 0.1969 _refine_ls_goodness_of_fit_ref 1.100 _refine_ls_restrained_S_all 1.100 _refine_ls_abs_structure_details ; Flack H D (1983), Acta Cryst. A39, 876-881 ; _refine_ls_abs_structure_Flack 0.00(3) _refine_diff_density_max 1.089 _refine_diff_density_min -0.400 _refine_diff_density_rms 0.070 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0052 0.0029 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0095 0.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr 0.3307 1.0133 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1722 0.2093 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0084 0.0063 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Cr Cr 0.5000 0.5000 0.83326(9) 0.0430(3) Uani 1 2 d S . . C12 C 0.5609(4) 0.2935(4) 0.7583(4) 0.0573(11) Uani 1 1 d . . . N12 N 0.4138(3) 0.2689(3) 0.6407(4) 0.0622(11) Uani 1 1 d . . . N11 N 0.6012(4) 0.3613(3) 0.8157(4) 0.0692(12) Uani 1 1 d . . . N20 N 0.5969(4) 0.5414(4) 0.9531(4) 0.0687(12) Uani 1 1 d . . . C13 C 0.4653(4) 0.3196(3) 0.7089(4) 0.0557(10) Uani 1 1 d . . . C22 C 0.5522(4) 0.5189(4) 1.0336(4) 0.0620(12) Uani 1 1 d . . . C10 C 0.6894(5) 0.3164(5) 0.8495(5) 0.0805(17) Uani 1 1 d . . . H10 H 0.7345 0.3466 0.8927 0.097 Uiso 1 1 calc R . . C11 C 0.7016(5) 0.2206(5) 0.8104(5) 0.0791(17) Uani 1 1 d . . . H11 H 0.7560 0.1743 0.8212 0.095 Uiso 1 1 calc R . . C20 C 0.6973(4) 0.5691(5) 0.9787(6) 0.0764(19) Uani 1 1 d . . . H20 H 0.7487 0.5890 0.9363 0.092 Uiso 1 1 calc R . . N13 N 0.6183(3) 0.2057(4) 0.7522(4) 0.0650(11) Uani 1 1 d . . . N10 N 0.4154(3) 0.4074(3) 0.7327(3) 0.0604(10) Uani 1 1 d . . . C15 C 0.3294(4) 0.4118(4) 0.6770(5) 0.0687(14) Uani 1 1 d . . . H15 H 0.2792 0.4641 0.6783 0.082 Uiso 1 1 calc R . . C14 C 0.3286(4) 0.3272(4) 0.6192(5) 0.0708(14) Uani 1 1 d . . . H14 H 0.2790 0.3122 0.5736 0.085 Uiso 1 1 calc R . . N21 N 0.6186(3) 0.5319(4) 1.1057(4) 0.0703(13) Uani 1 1 d . . . C21 C 0.7113(4) 0.5641(5) 1.0682(6) 0.0794(18) Uani 1 1 d . . . H21 H 0.7723 0.5794 1.1007 0.095 Uiso 1 1 calc R . . S1 S 0.5000 0.5000 1.35841(17) 0.0678(9) Uani 1 2 d S . . O101 O 0.5890(3) 0.5245(4) 1.2980(4) 0.0826(13) Uani 1 1 d . . . O100 O 0.5874(5) 0.0225(5) 0.6665(5) 0.119(3) Uani 1 1 d . . . 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 Cr 0.0588(5) 0.0480(4) 0.0221(7) 0.000 0.000 -0.0087(3) C12 0.072(2) 0.064(2) 0.036(3) 0.0073(18) 0.000(2) -0.0024(18) N12 0.078(2) 0.0605(19) 0.049(3) -0.0013(18) -0.005(2) 0.0048(16) N11 0.083(2) 0.071(2) 0.053(3) 0.003(2) -0.013(2) -0.0042(18) N20 0.075(2) 0.082(3) 0.049(3) -0.005(2) 0.004(2) -0.0143(19) C13 0.069(2) 0.0551(18) 0.042(3) 0.0007(18) 0.0015(19) -0.0032(15) C22 0.069(3) 0.071(3) 0.046(4) -0.001(2) 0.005(2) -0.0057(19) C10 0.091(3) 0.090(3) 0.061(5) 0.005(3) -0.025(3) -0.009(3) C11 0.078(3) 0.101(4) 0.059(4) 0.014(3) -0.018(3) 0.007(3) C20 0.063(3) 0.091(3) 0.075(6) 0.000(3) 0.012(3) -0.017(2) N13 0.069(2) 0.080(2) 0.046(3) 0.017(2) -0.0029(19) 0.0034(18) N10 0.071(2) 0.065(2) 0.046(3) -0.0009(17) 0.0001(18) -0.0012(16) C15 0.073(3) 0.068(2) 0.065(4) 0.000(2) -0.010(2) 0.011(2) C14 0.075(3) 0.072(3) 0.065(4) 0.001(2) -0.014(2) 0.003(2) N21 0.068(2) 0.083(3) 0.060(4) -0.007(2) -0.008(2) -0.0046(18) C21 0.067(3) 0.098(4) 0.073(6) -0.004(3) -0.009(3) -0.013(2) S1 0.0683(9) 0.0810(10) 0.054(3) 0.000 0.000 -0.0160(6) O101 0.0635(19) 0.129(3) 0.055(3) -0.012(3) -0.0014(18) -0.014(2) O100 0.118(4) 0.133(5) 0.107(6) -0.045(4) -0.040(4) 0.049(4) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Cr N10 2.155(5) . ? Cr N10 2.155(5) 2_665 ? Cr N20 2.179(6) . ? Cr N20 2.179(6) 2_665 ? Cr N11 2.217(5) . ? Cr N11 2.217(5) 2_665 ? C12 N11 1.302(7) . ? C12 N13 1.348(7) . ? C12 C13 1.453(7) . ? N12 C13 1.343(7) . ? N12 C14 1.360(7) . ? N11 C10 1.358(8) . ? N20 C22 1.314(8) . ? N20 C20 1.385(7) . ? C13 N10 1.340(6) . ? C22 N21 1.347(8) . ? C22 C22 1.423(10) 2_665 ? C10 C11 1.358(11) . ? C11 N13 1.367(8) . ? C20 C21 1.290(11) . ? N10 C15 1.360(7) . ? C15 C14 1.363(9) . ? N21 C21 1.368(8) . ? S1 O100 1.423(6) 8 ? S1 O100 1.423(6) 7_545 ? S1 O101 1.464(5) 2_665 ? S1 O101 1.464(5) . ? O100 S1 1.423(6) 3_644 ? 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 N10 Cr N10 96.6(3) . 2_665 ? N10 Cr N20 160.64(18) . . ? N10 Cr N20 95.77(18) 2_665 . ? N10 Cr N20 95.77(18) . 2_665 ? N10 Cr N20 160.64(18) 2_665 2_665 ? N20 Cr N20 76.7(3) . 2_665 ? N10 Cr N11 77.14(17) . . ? N10 Cr N11 94.12(18) 2_665 . ? N20 Cr N11 87.14(19) . . ? N20 Cr N11 103.1(2) 2_665 . ? N10 Cr N11 94.12(18) . 2_665 ? N10 Cr N11 77.14(17) 2_665 2_665 ? N20 Cr N11 103.1(2) . 2_665 ? N20 Cr N11 87.14(19) 2_665 2_665 ? N11 Cr N11 167.0(3) . 2_665 ? N11 C12 N13 112.5(5) . . ? N11 C12 C13 119.1(5) . . ? N13 C12 C13 128.5(5) . . ? C13 N12 C14 107.0(5) . . ? C12 N11 C10 105.7(5) . . ? C12 N11 Cr 112.0(3) . . ? C10 N11 Cr 142.0(4) . . ? C22 N20 C20 103.5(6) . . ? C22 N20 Cr 112.5(4) . . ? C20 N20 Cr 143.1(5) . . ? N10 C13 N12 110.8(4) . . ? N10 C13 C12 118.3(5) . . ? N12 C13 C12 130.8(4) . . ? N20 C22 N21 111.3(5) . . ? N20 C22 C22 119.0(3) . 2_665 ? N21 C22 C22 129.6(3) . 2_665 ? N11 C10 C11 109.5(5) . . ? C10 C11 N13 106.6(5) . . ? C21 C20 N20 112.2(6) . . ? C12 N13 C11 105.7(5) . . ? C13 N10 C15 106.0(4) . . ? C13 N10 Cr 113.0(3) . . ? C15 N10 Cr 140.7(4) . . ? N10 C15 C14 109.0(5) . . ? N12 C14 C15 107.2(5) . . ? C22 N21 C21 106.8(6) . . ? C20 C21 N21 106.3(5) . . ? O100 S1 O100 108.8(7) 8 7_545 ? O100 S1 O101 109.4(3) 8 2_665 ? O100 S1 O101 110.7(3) 7_545 2_665 ? O100 S1 O101 110.7(3) 8 . ? O100 S1 O101 109.4(3) 7_545 . ? O101 S1 O101 107.9(4) 2_665 . ?