# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' # Attachment 'Cpds_1-4_R.cif' _journal_coden_Cambridge 0222 #===================================================================== # 1. TITLE AND AUTHOR LIST _publ_section_title ; Water-Induced Reversible Structural Phase Transformatiom with Chromic Behavior of Metal Supramolecular Frameworks Containing Aminopyrazine with Sulfate Anion ; loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Jaursup Boonmak' . ; Department of Chemistry Faculty of Science Khon Kaen University Khon Kaen 40002 Thailand ; 'Motohiro Nakano' . ; Division of Applied Chemistry Graduate School of Engineering Osaka University Suita, Osaka 565-0871 Japan ; 'Narongsak Chaichit' . ; Department of Physics Faculty of Science and Technology Thammasat University, Rangsit Pathumthani 12121 Thailand ; 'Sujittra Youngme' . ; Department of Chemistry Faculty of Science Khon Kaen University Khon Kaen 40002 Thailand ; _publ_contact_author_name 'Sujittra Youngme' _publ_contact_author_email sujittra@kku.ac.th #============================================================================ data_1_Co _database_code_depnum_ccdc_archive 'CCDC 752993' #TrackingRef 'Cpds_1-4_R.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; di(2-aminopyrazine)-tetraaqua cobalt(II) hexaaqua cobalt(II) disulfate dihydrate ; _chemical_name_common ;di(2-aminopyrazine)-tetraaqua cobalt(ii) hexaaqua cobalt(ii) disulfate dihydrate ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H34 Co2 N6 O20 S2' _chemical_formula_weight 716.39 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.5697(4) _cell_length_b 8.3236(5) _cell_length_c 13.2130(8) _cell_angle_alpha 75.8320(10) _cell_angle_beta 78.6140(10) _cell_angle_gamma 78.8290(10) _cell_volume 678.68(7) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.61 _cell_measurement_theta_max 26.87 _exptl_crystal_description rectangular _exptl_crystal_colour orange _exptl_crystal_size_max 0.53 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.753 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 370 _exptl_absorpt_coefficient_mu 1.468 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.715035 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ; Siemens SMART CCD area detector diffractometer ; _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3734 _diffrn_reflns_av_R_equivalents 0.0127 _diffrn_reflns_av_sigmaI/netI 0.0152 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 26.87 _reflns_number_total 2796 _reflns_number_gt 2531 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement 'SAINT (Bruker, 2000)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material 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^)+(0.0574P)^2^+0.0338P] 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 2796 _refine_ls_number_parameters 243 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0299 _refine_ls_R_factor_gt 0.0266 _refine_ls_wR_factor_ref 0.0769 _refine_ls_wR_factor_gt 0.0750 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _refine_ls_shift/su_max 0.001 _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 Co1 Co 0.0000 0.5000 0.5000 0.01936(10) Uani 1 2 d S . . Co2 Co 0.0000 1.0000 0.0000 0.02450(11) Uani 1 2 d S . . O1 O 0.0212(2) 0.46546(17) 0.66028(10) 0.0296(3) Uani 1 1 d . . . O2 O 0.0409(3) 0.73861(17) 0.05513(13) 0.0405(4) Uani 1 1 d . . . O3 O 0.2839(2) 0.9733(2) -0.09960(12) 0.0414(4) Uani 1 1 d . . . O4 O 0.1434(2) 1.0249(2) 0.12380(12) 0.0374(3) Uani 1 1 d . . . O5 O 0.5370(2) 0.20927(16) 0.79952(13) 0.0423(3) Uani 1 1 d . . . O6 O 0.41342(19) 0.48178(16) 0.70010(9) 0.0297(3) Uani 1 1 d . . . O7 O 0.66757(19) 0.45122(16) 0.81454(10) 0.0301(3) Uani 1 1 d . . . O8 O 0.3094(2) 0.4154(2) 0.88794(10) 0.0398(3) Uani 1 1 d . . . O9 O 0.2818(2) 0.58598(17) 0.46633(11) 0.0283(3) Uani 1 1 d . . . O10 O 0.3828(2) 0.28007(18) 0.08787(13) 0.0383(3) Uani 1 1 d . . . C1 C 0.1514(3) 0.1277(2) 0.59253(14) 0.0274(4) Uani 1 1 d . . . C2 C 0.2191(3) -0.0449(2) 0.59685(14) 0.0271(4) Uani 1 1 d . . . C4 C 0.2376(3) 0.1826(2) 0.41256(14) 0.0291(4) Uani 1 1 d . . . C3 C 0.2981(3) 0.0144(2) 0.41670(15) 0.0295(4) Uani 1 1 d . . . N1 N 0.1583(2) 0.24018(17) 0.50181(11) 0.0252(3) Uani 1 1 d . . . N2 N 0.2877(2) -0.10210(18) 0.50782(12) 0.0284(3) Uani 1 1 d . . . N3 N 0.2129(3) -0.1555(2) 0.69061(14) 0.0401(4) Uani 1 1 d . . . S1 S 0.48103(6) 0.38825(5) 0.80072(3) 0.02246(11) Uani 1 1 d . . . H1 H 0.099(3) 0.166(2) 0.6588(16) 0.026(5) Uiso 1 1 d . . . H1A H 0.135(5) 0.474(3) 0.673(2) 0.052(8) Uiso 1 1 d . . . H1B H -0.066(4) 0.465(3) 0.707(2) 0.047(7) Uiso 1 1 d . . . H2 H 0.246(3) 0.256(3) 0.3496(17) 0.034(5) Uiso 1 1 d . . . H2A H -0.037(5) 0.688(4) 0.072(2) 0.063(9) Uiso 1 1 d . . . H2B H 0.140(5) 0.667(4) 0.095(2) 0.060(8) Uiso 1 1 d . . . H3 H 0.353(3) -0.021(3) 0.3452(18) 0.034(5) Uiso 1 1 d . . . H3A H 0.162(4) -0.124(3) 0.750(2) 0.053(8) Uiso 1 1 d . . . H3B H 0.259(4) -0.267(3) 0.6961(18) 0.041(6) Uiso 1 1 d . . . H3C H 0.372(4) 0.885(3) -0.0929(18) 0.044(7) Uiso 1 1 d . . . H3D H 0.345(4) 1.051(3) -0.125(2) 0.051(7) Uiso 1 1 d . . . H4 H 0.194(4) 1.122(3) 0.1115(19) 0.048(7) Uiso 1 1 d . . . H4A H 0.233(4) 0.942(3) 0.149(2) 0.052(8) Uiso 1 1 d . . . H9 H 0.293(4) 0.679(3) 0.4757(17) 0.037(6) Uiso 1 1 d . . . H9A H 0.376(4) 0.562(3) 0.425(2) 0.045(7) Uiso 1 1 d . . . H10 H 0.366(4) 0.353(4) 0.121(2) 0.058(9) Uiso 1 1 d . . . H10A H 0.374(5) 0.334(4) 0.027(3) 0.071(10) Uiso 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 Co1 0.01752(17) 0.01876(16) 0.02157(16) -0.00400(11) -0.00322(11) -0.00248(12) Co2 0.01817(18) 0.02380(18) 0.02991(18) -0.00044(12) -0.00552(12) -0.00436(13) O1 0.0226(7) 0.0428(8) 0.0240(6) -0.0077(5) -0.0044(5) -0.0053(6) O2 0.0296(8) 0.0283(7) 0.0604(9) 0.0080(6) -0.0168(7) -0.0091(6) O3 0.0242(7) 0.0313(8) 0.0588(9) -0.0003(6) 0.0048(6) -0.0043(7) O4 0.0355(8) 0.0338(8) 0.0457(8) -0.0027(6) -0.0193(6) -0.0059(7) O5 0.0404(8) 0.0238(6) 0.0601(9) -0.0008(6) -0.0131(7) -0.0040(6) O6 0.0270(7) 0.0329(7) 0.0269(6) -0.0022(5) -0.0090(5) 0.0001(5) O7 0.0213(6) 0.0382(7) 0.0335(6) -0.0088(5) -0.0051(5) -0.0089(5) O8 0.0264(7) 0.0603(9) 0.0310(7) -0.0082(6) 0.0037(5) -0.0131(6) O9 0.0222(6) 0.0276(7) 0.0370(7) -0.0137(5) 0.0026(5) -0.0072(5) O10 0.0472(9) 0.0316(7) 0.0387(8) -0.0096(6) -0.0110(6) -0.0050(6) C1 0.0285(9) 0.0228(8) 0.0307(9) -0.0069(6) -0.0044(7) -0.0020(7) C2 0.0222(8) 0.0230(8) 0.0364(9) -0.0055(6) -0.0065(6) -0.0036(7) C4 0.0270(9) 0.0295(9) 0.0294(8) -0.0047(7) -0.0049(7) -0.0024(7) C3 0.0260(9) 0.0317(9) 0.0334(9) -0.0137(7) -0.0059(7) -0.0006(7) N1 0.0209(7) 0.0225(7) 0.0320(7) -0.0057(5) -0.0048(5) -0.0023(5) N2 0.0247(8) 0.0225(7) 0.0407(8) -0.0108(6) -0.0080(6) -0.0017(6) N3 0.0537(12) 0.0245(9) 0.0372(9) -0.0039(7) -0.0060(8) 0.0012(8) S1 0.0189(2) 0.0247(2) 0.02304(19) -0.00073(14) -0.00504(14) -0.00532(16) _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 Co1 O9 2.0421(12) . ? Co1 O9 2.0421(12) 2_566 ? Co1 O1 2.0953(13) . ? Co1 O1 2.0953(13) 2_566 ? Co1 N1 2.2072(14) 2_566 ? Co1 N1 2.2072(14) . ? Co2 O3 2.0672(14) 2_575 ? Co2 O3 2.0672(14) . ? Co2 O2 2.1003(14) 2_575 ? Co2 O2 2.1003(14) . ? Co2 O4 2.1110(14) . ? Co2 O4 2.1110(14) 2_575 ? O1 H1A 0.81(3) . ? O1 H1B 0.75(3) . ? O2 H2A 0.70(3) . ? O2 H2B 0.94(3) . ? O3 H3C 0.84(3) . ? O3 H3D 0.80(3) . ? O4 H4 0.90(3) . ? O4 H4A 0.86(3) . ? O5 S1 1.4669(14) . ? O6 S1 1.4709(12) . ? O7 S1 1.4812(12) . ? O8 S1 1.4717(13) . ? O9 H9 0.83(2) . ? O9 H9A 0.77(3) . ? O10 H10 0.81(3) . ? O10 H10A 0.83(3) . ? C1 N1 1.327(2) . ? C1 C2 1.410(3) . ? C1 H1 0.98(2) . ? C2 N2 1.340(2) . ? C2 N3 1.349(2) . ? C4 N1 1.353(2) . ? C4 C3 1.370(3) . ? C4 H2 0.90(2) . ? C3 N2 1.348(2) . ? C3 H3 1.04(2) . ? N3 H3A 0.87(3) . ? N3 H3B 0.91(3) . ? 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 O9 Co1 O9 180 . 2_566 ? O9 Co1 O1 87.45(5) . . ? O9 Co1 O1 92.55(5) 2_566 . ? O9 Co1 O1 92.55(5) . 2_566 ? O9 Co1 O1 87.45(5) 2_566 2_566 ? O1 Co1 O1 180 . 2_566 ? O9 Co1 N1 88.63(5) . 2_566 ? O9 Co1 N1 91.37(5) 2_566 2_566 ? O1 Co1 N1 90.17(5) . 2_566 ? O1 Co1 N1 89.83(5) 2_566 2_566 ? O9 Co1 N1 91.37(5) . . ? O9 Co1 N1 88.63(5) 2_566 . ? O1 Co1 N1 89.83(5) . . ? O1 Co1 N1 90.17(5) 2_566 . ? N1 Co1 N1 180 2_566 . ? O3 Co2 O3 180 2_575 . ? O3 Co2 O2 88.85(6) 2_575 2_575 ? O3 Co2 O2 91.15(6) . 2_575 ? O3 Co2 O2 91.15(6) 2_575 . ? O3 Co2 O2 88.85(6) . . ? O2 Co2 O2 180 2_575 . ? O3 Co2 O4 87.31(6) 2_575 . ? O3 Co2 O4 92.69(6) . . ? O2 Co2 O4 89.95(6) 2_575 . ? O2 Co2 O4 90.05(6) . . ? O3 Co2 O4 92.69(6) 2_575 2_575 ? O3 Co2 O4 87.31(6) . 2_575 ? O2 Co2 O4 90.05(6) 2_575 2_575 ? O2 Co2 O4 89.95(6) . 2_575 ? O4 Co2 O4 180 . 2_575 ? Co1 O1 H1A 115.5(19) . . ? Co1 O1 H1B 129(2) . . ? H1A O1 H1B 114(3) . . ? Co2 O2 H2A 127(3) . . ? Co2 O2 H2B 130.8(17) . . ? H2A O2 H2B 96(3) . . ? Co2 O3 H3C 123.2(16) . . ? Co2 O3 H3D 120.5(19) . . ? H3C O3 H3D 109(2) . . ? Co2 O4 H4 114.0(16) . . ? Co2 O4 H4A 117.9(17) . . ? H4 O4 H4A 110(2) . . ? Co1 O9 H9 122.0(16) . . ? Co1 O9 H9A 126(2) . . ? H9 O9 H9A 107(2) . . ? H10 O10 H10A 103(3) . . ? N1 C1 C2 122.14(17) . . ? N1 C1 H1 118.8(11) . . ? C2 C1 H1 119.0(11) . . ? N2 C2 N3 118.92(16) . . ? N2 C2 C1 120.53(16) . . ? N3 C2 C1 120.55(17) . . ? N1 C4 C3 120.70(16) . . ? N1 C4 H2 119.1(13) . . ? C3 C4 H2 120.2(13) . . ? N2 C3 C4 123.11(17) . . ? N2 C3 H3 120.3(12) . . ? C4 C3 H3 116.6(12) . . ? C1 N1 C4 117.03(15) . . ? C1 N1 Co1 119.50(12) . . ? C4 N1 Co1 122.80(11) . . ? C2 N2 C3 116.37(15) . . ? C2 N3 H3A 121.8(17) . . ? C2 N3 H3B 122.7(15) . . ? H3A N3 H3B 115(2) . . ? O5 S1 O6 109.82(8) . . ? O5 S1 O8 110.65(9) . . ? O6 S1 O8 108.98(8) . . ? O5 S1 O7 109.05(8) . . ? O6 S1 O7 109.09(7) . . ? O8 S1 O7 109.24(8) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.87 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.315 _refine_diff_density_min -0.444 _refine_diff_density_rms 0.067 #======= END data_2_Fe _database_code_depnum_ccdc_archive 'CCDC 752994' #TrackingRef 'Cpds_1-4_R.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; di(2-aminopyrazine)-tetraaqua iron(II) hexaaqua iron(II) disulfate dihydrate ; _chemical_name_common ;di(2-aminopyrazine)-tetraaqua iron(ii) hexaaqua iron(ii) disulfate dihydrate ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H34 Fe2 N6 O20 S2' _chemical_formula_weight 710.23 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.5726(4) _cell_length_b 8.3984(5) _cell_length_c 13.2221(8) _cell_angle_alpha 75.6230(10) _cell_angle_beta 78.3380(10) _cell_angle_gamma 78.7860(10) _cell_volume 684.35(7) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.61 _cell_measurement_theta_max 17.67 _exptl_crystal_description rectangular _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.723 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 368 _exptl_absorpt_coefficient_mu 1.304 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.577038 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ; Siemens SMART CCD area detector diffractometer ; _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 999 _diffrn_reflns_av_R_equivalents 0.0106 _diffrn_reflns_av_sigmaI/netI 0.0170 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 3 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 17.67 _reflns_number_total 874 _reflns_number_gt 804 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement 'SAINT (Bruker, 2000)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material 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^)+(0.0583P)^2^+0.3044P] 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 874 _refine_ls_number_parameters 243 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0286 _refine_ls_R_factor_gt 0.0254 _refine_ls_wR_factor_ref 0.0731 _refine_ls_wR_factor_gt 0.0676 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _refine_ls_shift/su_max 0.001 _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 Fe1 Fe 0.0000 0.5000 0.5000 0.0253(5) Uani 1 2 d S . . Fe2 Fe 0.0000 1.0000 0.0000 0.0296(6) Uani 1 2 d S . . O1 O 0.0233(7) 0.4624(5) 0.6598(3) 0.0341(14) Uani 1 1 d . . . O2 O 0.0392(10) 0.7409(7) 0.0573(4) 0.0485(18) Uani 1 1 d . . . O3 O 0.2858(7) 0.9718(9) -0.1045(4) 0.0471(18) Uani 1 1 d . . . O4 O 0.1465(7) 1.0247(9) 0.1257(4) 0.0421(16) Uani 1 1 d . . . O5 O 0.5376(5) 0.2098(5) 0.8001(3) 0.0441(13) Uani 1 1 d . . . O6 O 0.4080(5) 0.4819(5) 0.7017(3) 0.0309(13) Uani 1 1 d . . . O7 O 0.6669(5) 0.4498(4) 0.8140(3) 0.0307(12) Uani 1 1 d . . . O8 O 0.3116(5) 0.4108(5) 0.8907(3) 0.0426(13) Uani 1 1 d . . . O9 O 0.2859(6) 0.5896(5) 0.4660(3) 0.0364(14) Uani 1 1 d . . . O10 O 0.3833(6) 0.2798(6) 0.0903(5) 0.0452(17) Uani 1 1 d . . . C1 C 0.1549(8) 0.1244(12) 0.5928(8) 0.028(3) Uani 1 1 d . . . C2 C 0.2197(8) -0.0443(12) 0.5962(8) 0.027(2) Uani 1 1 d . . . C4 C 0.2373(9) 0.1787(12) 0.4143(7) 0.034(3) Uani 1 1 d . . . C3 C 0.2961(8) 0.0153(13) 0.4167(8) 0.028(2) Uani 1 1 d . . . N1 N 0.1601(6) 0.2373(8) 0.5035(6) 0.0277(19) Uani 1 1 d . . . N2 N 0.2887(6) -0.1011(8) 0.5064(6) 0.0284(19) Uani 1 1 d . . . N3 N 0.2138(9) -0.1550(11) 0.6885(8) 0.046(3) Uani 1 1 d . . . S1 S 0.47918(19) 0.3878(2) 0.80134(15) 0.0273(7) Uani 1 1 d . . . H1 H 0.099(7) 0.151(6) 0.660(4) 0.032(15) Uiso 1 1 d . . . H1A H 0.145(11) 0.476(8) 0.682(5) 0.09(3) Uiso 1 1 d . . . H1B H -0.064(8) 0.451(7) 0.704(4) 0.03(2) Uiso 1 1 d . . . H2 H 0.250(7) 0.246(7) 0.353(4) 0.001(17) Uiso 1 1 d . . . H2A H -0.039(11) 0.696(9) 0.072(5) 0.07(3) Uiso 1 1 d . . . H2B H 0.142(10) 0.678(9) 0.089(6) 0.07(3) Uiso 1 1 d . . . H3 H 0.354(7) -0.030(6) 0.351(4) 0.035(15) Uiso 1 1 d . . . H3A H 0.177(9) -0.110(8) 0.746(5) 0.07(2) Uiso 1 1 d . . . H3B H 0.262(6) -0.252(7) 0.699(4) 0.000(16) Uiso 1 1 d . . . H3C H 0.363(10) 0.886(9) -0.094(6) 0.07(4) Uiso 1 1 d . . . H3D H 0.340(9) 1.039(8) -0.113(5) 0.03(2) Uiso 1 1 d . . . H4 H 0.190(9) 1.106(9) 0.112(5) 0.05(3) Uiso 1 1 d . . . H4A H 0.245(9) 0.936(9) 0.151(5) 0.05(3) Uiso 1 1 d . . . H9 H 0.292(10) 0.699(10) 0.475(5) 0.10(3) Uiso 1 1 d . . . H9A H 0.373(7) 0.568(6) 0.426(4) 0.014(16) Uiso 1 1 d . . . H10 H 0.364(7) 0.342(6) 0.117(4) 0.008(18) Uiso 1 1 d . . . H10A H 0.386(11) 0.315(10) 0.018(7) 0.09(3) Uiso 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 Fe1 0.0250(6) 0.0239(11) 0.0284(10) -0.0089(9) -0.0002(5) -0.0075(6) Fe2 0.0252(6) 0.0282(11) 0.0355(10) -0.0059(9) -0.0015(6) -0.0089(6) O1 0.030(2) 0.046(4) 0.028(3) -0.011(3) 0.002(2) -0.013(2) O2 0.035(3) 0.034(4) 0.075(5) 0.003(4) -0.017(3) -0.012(3) O3 0.030(3) 0.037(5) 0.070(4) -0.011(4) 0.007(2) -0.013(4) O4 0.040(3) 0.034(4) 0.057(4) -0.007(4) -0.015(2) -0.011(3) O5 0.042(2) 0.016(3) 0.071(3) -0.003(3) -0.010(2) -0.004(2) O6 0.031(2) 0.036(4) 0.023(3) 0.002(3) -0.010(2) -0.003(2) O7 0.0251(18) 0.036(3) 0.034(3) -0.009(3) -0.0046(17) -0.0110(18) O8 0.034(2) 0.064(4) 0.031(3) -0.011(3) 0.0049(19) -0.020(2) O9 0.028(2) 0.034(4) 0.049(3) -0.022(3) 0.010(2) -0.009(2) O10 0.058(3) 0.037(4) 0.048(4) -0.023(4) -0.004(3) -0.011(2) C1 0.032(3) 0.009(8) 0.043(7) -0.009(7) -0.001(4) -0.002(4) C2 0.026(3) 0.016(8) 0.036(7) 0.009(7) -0.011(4) -0.010(4) C4 0.038(4) 0.039(8) 0.021(6) -0.006(6) 0.005(4) -0.011(4) C3 0.032(3) 0.020(7) 0.034(7) -0.010(7) -0.010(4) 0.003(4) N1 0.022(2) 0.024(6) 0.035(4) -0.001(5) -0.003(3) -0.009(3) N2 0.031(3) 0.026(5) 0.031(4) -0.009(5) -0.008(3) -0.005(3) N3 0.064(4) 0.009(7) 0.058(7) -0.006(7) -0.007(4) 0.006(4) S1 0.0238(8) 0.0260(17) 0.0320(16) -0.0058(15) -0.0008(8) -0.0081(8) _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 Fe1 O9 2.083(3) 2_566 ? Fe1 O9 2.083(3) . ? Fe1 O1 2.089(4) 2_566 ? Fe1 O1 2.089(4) . ? Fe1 N1 2.246(6) . ? Fe1 N1 2.246(6) 2_566 ? Fe2 O2 2.102(5) . ? Fe2 O2 2.102(5) 2_575 ? Fe2 O3 2.106(4) . ? Fe2 O3 2.106(4) 2_575 ? Fe2 O4 2.151(5) 2_575 ? Fe2 O4 2.151(5) . ? O1 H1A 0.94(7) . ? O1 H1B 0.73(5) . ? O2 H2A 0.66(7) . ? O2 H2B 0.88(7) . ? O3 H3C 0.80(7) . ? O3 H3D 0.70(5) . ? O4 H4 0.75(7) . ? O4 H4A 0.93(7) . ? O5 S1 1.473(4) . ? O6 S1 1.472(4) . ? O7 S1 1.482(3) . ? O8 S1 1.466(3) . ? O9 H9 0.96(8) . ? O9 H9A 0.73(4) . ? O10 H10 0.68(4) . ? O10 H10A 0.92(9) . ? C1 N1 1.317(8) . ? C1 C2 1.390(9) . ? C1 H1 0.95(5) . ? C2 N3 1.337(8) . ? C2 N2 1.350(8) . ? C4 C3 1.346(9) . ? C4 N1 1.356(8) . ? C4 H2 0.86(5) . ? C3 N2 1.335(7) . ? C3 H3 1.01(5) . ? N3 H3A 0.90(6) . ? N3 H3B 0.80(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 O9 Fe1 O9 180 2_566 . ? O9 Fe1 O1 87.04(17) 2_566 2_566 ? O9 Fe1 O1 92.96(17) . 2_566 ? O9 Fe1 O1 92.96(17) 2_566 . ? O9 Fe1 O1 87.04(17) . . ? O1 Fe1 O1 180 2_566 . ? O9 Fe1 N1 87.81(16) 2_566 . ? O9 Fe1 N1 92.19(16) . . ? O1 Fe1 N1 91.4(2) 2_566 . ? O1 Fe1 N1 88.6(2) . . ? O9 Fe1 N1 92.19(16) 2_566 2_566 ? O9 Fe1 N1 87.81(16) . 2_566 ? O1 Fe1 N1 88.6(2) 2_566 2_566 ? O1 Fe1 N1 91.4(2) . 2_566 ? N1 Fe1 N1 180 . 2_566 ? O2 Fe2 O2 180 . 2_575 ? O2 Fe2 O3 89.2(3) . . ? O2 Fe2 O3 90.8(3) 2_575 . ? O2 Fe2 O3 90.8(3) . 2_575 ? O2 Fe2 O3 89.2(3) 2_575 2_575 ? O3 Fe2 O3 180 . 2_575 ? O2 Fe2 O4 90.4(2) . 2_575 ? O2 Fe2 O4 89.6(2) 2_575 2_575 ? O3 Fe2 O4 86.07(18) . 2_575 ? O3 Fe2 O4 93.93(18) 2_575 2_575 ? O2 Fe2 O4 89.6(2) . . ? O2 Fe2 O4 90.4(2) 2_575 . ? O3 Fe2 O4 93.93(18) . . ? O3 Fe2 O4 86.07(18) 2_575 . ? O4 Fe2 O4 180 2_575 . ? Fe1 O1 H1A 122(4) . . ? Fe1 O1 H1B 125(4) . . ? H1A O1 H1B 112(6) . . ? Fe2 O2 H2A 124(7) . . ? Fe2 O2 H2B 128(5) . . ? H2A O2 H2B 104(9) . . ? Fe2 O3 H3C 118(6) . . ? Fe2 O3 H3D 112(5) . . ? H3C O3 H3D 111(7) . . ? Fe2 O4 H4 111(5) . . ? Fe2 O4 H4A 117(3) . . ? H4 O4 H4A 111(7) . . ? Fe1 O9 H9 121(4) . . ? Fe1 O9 H9A 125(4) . . ? H9 O9 H9A 108(5) . . ? H10 O10 H10A 114(7) . . ? N1 C1 C2 122.7(7) . . ? N1 C1 H1 123(3) . . ? C2 C1 H1 115(3) . . ? N3 C2 N2 118.1(7) . . ? N3 C2 C1 120.9(7) . . ? N2 C2 C1 121.0(8) . . ? C3 C4 N1 122.2(8) . . ? C3 C4 H2 117(3) . . ? N1 C4 H2 121(3) . . ? N2 C3 C4 123.0(7) . . ? N2 C3 H3 114(3) . . ? C4 C3 H3 123(3) . . ? C1 N1 C4 115.6(6) . . ? C1 N1 Fe1 121.0(4) . . ? C4 N1 Fe1 122.6(6) . . ? C3 N2 C2 115.5(6) . . ? C2 N3 H3A 115(4) . . ? C2 N3 H3B 128(4) . . ? H3A N3 H3B 116(6) . . ? O8 S1 O6 109.6(2) . . ? O8 S1 O5 110.0(2) . . ? O6 S1 O5 110.5(2) . . ? O8 S1 O7 109.02(19) . . ? O6 S1 O7 109.4(2) . . ? O5 S1 O7 108.2(2) . . ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 17.67 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 0.183 _refine_diff_density_min -0.250 _refine_diff_density_rms 0.051 #======= END data_3_CoFe _database_code_depnum_ccdc_archive 'CCDC 752995' #TrackingRef 'Cpds_1-4_R.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; di(2-aminopyrazine)-tetraaqua cobalt(II) hexaaqua iron(II) disulfate dihydrate ; _chemical_name_common ;di(2-aminopyrazine)-tetraaqua cobalt(ii) hexaaqua iron(ii) disulfate dihydrate ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H34 Co Fe N6 O20 S2' _chemical_formula_weight 713.31 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.5742(4) _cell_length_b 8.3548(5) _cell_length_c 13.2410(8) _cell_angle_alpha 75.6760(10) _cell_angle_beta 78.5020(10) _cell_angle_gamma 78.8140(10) _cell_volume 682.46(7) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.61 _cell_measurement_theta_max 27.45 _exptl_crystal_description rectangular _exptl_crystal_colour 'yellowish orange' _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.736 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 369 _exptl_absorpt_coefficient_mu 1.384 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.695703 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ; Siemens SMART CCD area detector diffractometer ; _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4208 _diffrn_reflns_av_R_equivalents 0.0129 _diffrn_reflns_av_sigmaI/netI 0.0130 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 27.45 _reflns_number_total 3016 _reflns_number_gt 2832 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement 'SAINT (Bruker, 2000)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material 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^)+(0.0550P)^2^+0.2470P] 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 3016 _refine_ls_number_parameters 243 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0285 _refine_ls_R_factor_gt 0.0267 _refine_ls_wR_factor_ref 0.0849 _refine_ls_wR_factor_gt 0.0779 _refine_ls_goodness_of_fit_ref 1.102 _refine_ls_restrained_S_all 1.102 _refine_ls_shift/su_max 0.001 _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 Co1 Co 0.0000 0.5000 0.5000 0.02144(10) Uani 1 2 d S . . Fe1 Fe 0.0000 1.0000 0.0000 0.02430(11) Uani 1 2 d S . . O1 O 0.0219(2) 0.46371(18) 0.66007(11) 0.0304(3) Uani 1 1 d . . . O2 O 0.0395(3) 0.73867(19) 0.05735(14) 0.0413(4) Uani 1 1 d . . . O3 O 0.2849(2) 0.9724(2) -0.10194(15) 0.0429(4) Uani 1 1 d . . . O4 O 0.1448(2) 1.0258(2) 0.12482(13) 0.0389(3) Uani 1 1 d . . . O5 O 0.5366(3) 0.20957(17) 0.79948(14) 0.0428(4) Uani 1 1 d . . . O6 O 0.4116(2) 0.48171(17) 0.70075(10) 0.0310(3) Uani 1 1 d . . . O7 O 0.6681(2) 0.45099(17) 0.81391(11) 0.0306(3) Uani 1 1 d . . . O8 O 0.3105(2) 0.4144(2) 0.88858(12) 0.0407(3) Uani 1 1 d . . . O9 O 0.2834(2) 0.58721(17) 0.46589(12) 0.0292(3) Uani 1 1 d . . . O10 O 0.3828(3) 0.28106(19) 0.08889(14) 0.0389(3) Uani 1 1 d . . . C1 C 0.1518(3) 0.1269(2) 0.59251(16) 0.0293(4) Uani 1 1 d . . . C2 C 0.2197(3) -0.0462(2) 0.59682(16) 0.0283(4) Uani 1 1 d . . . C4 C 0.2372(3) 0.1834(2) 0.41284(16) 0.0306(4) Uani 1 1 d . . . C3 C 0.2981(3) 0.0148(2) 0.41650(16) 0.0320(4) Uani 1 1 d . . . N1 N 0.1586(2) 0.23885(18) 0.50237(13) 0.0264(3) Uani 1 1 d . . . N2 N 0.2878(2) -0.10136(19) 0.50713(14) 0.0302(3) Uani 1 1 d . . . N3 N 0.2131(3) -0.1563(2) 0.69000(16) 0.0432(4) Uani 1 1 d . . . S1 S 0.48062(6) 0.38816(5) 0.80094(3) 0.02330(11) Uani 1 1 d . . . H1 H 0.103(4) 0.157(3) 0.6599(19) 0.031(6) Uiso 1 1 d . . . H1A H 0.126(5) 0.465(4) 0.680(2) 0.048(8) Uiso 1 1 d . . . H1B H -0.070(5) 0.456(3) 0.710(2) 0.044(7) Uiso 1 1 d . . . H2 H 0.245(4) 0.267(3) 0.346(2) 0.038(6) Uiso 1 1 d . . . H2A H -0.046(6) 0.682(4) 0.075(3) 0.062(10) Uiso 1 1 d . . . H2B H 0.136(5) 0.676(4) 0.090(2) 0.049(8) Uiso 1 1 d . . . H3 H 0.353(4) -0.022(3) 0.3439(19) 0.031(6) Uiso 1 1 d . . . H3A H 0.159(5) -0.127(4) 0.757(3) 0.063(9) Uiso 1 1 d . . . H3B H 0.254(5) -0.258(4) 0.695(2) 0.052(8) Uiso 1 1 d . . . H3C H 0.365(5) 0.891(4) -0.092(2) 0.057(9) Uiso 1 1 d . . . H3D H 0.341(5) 1.046(4) -0.125(3) 0.059(10) Uiso 1 1 d . . . H4 H 0.195(5) 1.121(4) 0.113(2) 0.045(7) Uiso 1 1 d . . . H4A H 0.239(5) 0.941(4) 0.149(2) 0.058(9) Uiso 1 1 d . . . H9 H 0.300(4) 0.674(4) 0.475(2) 0.047(7) Uiso 1 1 d . . . H9A H 0.383(4) 0.565(3) 0.424(2) 0.034(6) Uiso 1 1 d . . . H10 H 0.371(5) 0.360(4) 0.117(3) 0.060(9) Uiso 1 1 d . . . H10A H 0.375(6) 0.338(5) 0.024(3) 0.068(10) Uiso 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 Co1 0.01963(17) 0.02063(16) 0.02326(18) -0.00429(12) -0.00280(12) -0.00242(11) Fe1 0.01819(18) 0.02325(17) 0.0293(2) -0.00060(13) -0.00426(13) -0.00401(12) O1 0.0247(7) 0.0426(7) 0.0240(7) -0.0072(5) -0.0032(6) -0.0063(5) O2 0.0306(8) 0.0283(7) 0.0612(10) 0.0067(7) -0.0163(7) -0.0073(6) O3 0.0259(7) 0.0320(8) 0.0610(11) -0.0009(7) 0.0048(7) -0.0048(6) O4 0.0358(8) 0.0355(7) 0.0476(9) -0.0036(6) -0.0181(7) -0.0060(6) O5 0.0407(8) 0.0231(6) 0.0623(10) -0.0017(6) -0.0131(7) -0.0038(5) O6 0.0281(7) 0.0348(7) 0.0279(7) -0.0024(5) -0.0088(5) -0.0006(5) O7 0.0222(6) 0.0388(7) 0.0330(7) -0.0079(5) -0.0049(5) -0.0090(5) O8 0.0270(7) 0.0623(10) 0.0315(7) -0.0096(7) 0.0037(6) -0.0132(6) O9 0.0217(6) 0.0296(6) 0.0378(7) -0.0140(5) 0.0033(5) -0.0071(5) O10 0.0480(9) 0.0311(7) 0.0392(8) -0.0100(6) -0.0092(7) -0.0040(6) C1 0.0298(9) 0.0240(8) 0.0331(10) -0.0081(7) -0.0032(7) -0.0009(6) C2 0.0239(8) 0.0233(8) 0.0379(10) -0.0067(7) -0.0060(7) -0.0031(6) C4 0.0288(9) 0.0297(9) 0.0316(9) -0.0069(7) -0.0033(7) -0.0014(7) C3 0.0299(9) 0.0322(9) 0.0355(10) -0.0138(7) -0.0052(7) 0.0003(7) N1 0.0222(7) 0.0222(6) 0.0337(8) -0.0062(6) -0.0033(6) -0.0019(5) N2 0.0263(8) 0.0248(7) 0.0415(9) -0.0117(6) -0.0064(6) -0.0018(5) N3 0.0559(12) 0.0255(8) 0.0413(10) -0.0031(7) -0.0051(8) 0.0017(7) S1 0.0200(2) 0.0249(2) 0.0240(2) -0.00137(15) -0.00433(15) -0.00515(14) _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 Co1 O9 2.0578(13) 2_566 ? Co1 O9 2.0578(13) . ? Co1 O1 2.0957(14) . ? Co1 O1 2.0957(14) 2_566 ? Co1 N1 2.2237(14) 2_566 ? Co1 N1 2.2237(14) . ? Fe1 O3 2.0886(16) 2_575 ? Fe1 O3 2.0886(16) . ? Fe1 O2 2.1094(15) 2_575 ? Fe1 O2 2.1094(15) . ? Fe1 O4 2.1372(15) . ? Fe1 O4 2.1372(15) 2_575 ? O1 H1A 0.78(3) . ? O1 H1B 0.80(3) . ? O2 H2A 0.77(4) . ? O2 H2B 0.86(3) . ? O3 H3C 0.78(3) . ? O3 H3D 0.75(4) . ? O4 H4 0.89(3) . ? O4 H4A 0.88(3) . ? O5 S1 1.4699(14) . ? O6 S1 1.4717(13) . ? O7 S1 1.4844(13) . ? O8 S1 1.4692(15) . ? O9 H9 0.79(3) . ? O9 H9A 0.79(3) . ? O10 H10 0.82(4) . ? O10 H10A 0.87(4) . ? C1 N1 1.321(2) . ? C1 C2 1.418(2) . ? C1 H1 0.97(2) . ? C2 N2 1.342(3) . ? C2 N3 1.343(3) . ? C4 N1 1.350(2) . ? C4 C3 1.379(2) . ? C4 H2 0.99(3) . ? C3 N2 1.343(3) . ? C3 H3 1.05(2) . ? N3 H3A 0.96(3) . ? N3 H3B 0.83(3) . ? 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 O9 Co1 O9 180 2_566 . ? O9 Co1 O1 92.54(6) 2_566 . ? O9 Co1 O1 87.46(6) . . ? O9 Co1 O1 87.46(6) 2_566 2_566 ? O9 Co1 O1 92.54(6) . 2_566 ? O1 Co1 O1 180 . 2_566 ? O9 Co1 N1 91.70(5) 2_566 2_566 ? O9 Co1 N1 88.30(5) . 2_566 ? O1 Co1 N1 90.63(6) . 2_566 ? O1 Co1 N1 89.37(6) 2_566 2_566 ? O9 Co1 N1 88.30(5) 2_566 . ? O9 Co1 N1 91.70(5) . . ? O1 Co1 N1 89.37(6) . . ? O1 Co1 N1 90.63(6) 2_566 . ? N1 Co1 N1 180 2_566 . ? O3 Fe1 O3 180 2_575 . ? O3 Fe1 O2 89.24(7) 2_575 2_575 ? O3 Fe1 O2 90.76(7) . 2_575 ? O3 Fe1 O2 90.76(7) 2_575 . ? O3 Fe1 O2 89.24(7) . . ? O2 Fe1 O2 180 2_575 . ? O3 Fe1 O4 86.57(7) 2_575 . ? O3 Fe1 O4 93.43(7) . . ? O2 Fe1 O4 90.20(6) 2_575 . ? O2 Fe1 O4 89.80(6) . . ? O3 Fe1 O4 93.43(7) 2_575 2_575 ? O3 Fe1 O4 86.57(7) . 2_575 ? O2 Fe1 O4 89.80(6) 2_575 2_575 ? O2 Fe1 O4 90.20(6) . 2_575 ? O4 Fe1 O4 180 . 2_575 ? Co1 O1 H1A 123(2) . . ? Co1 O1 H1B 128(2) . . ? H1A O1 H1B 108(3) . . ? Fe1 O2 H2A 128(3) . . ? Fe1 O2 H2B 129(2) . . ? H2A O2 H2B 99(3) . . ? Fe1 O3 H3C 120(2) . . ? Fe1 O3 H3D 119(3) . . ? H3C O3 H3D 111(3) . . ? Fe1 O4 H4 114.7(18) . . ? Fe1 O4 H4A 117.0(19) . . ? H4 O4 H4A 109(3) . . ? Co1 O9 H9 125(2) . . ? Co1 O9 H9A 128.9(19) . . ? H9 O9 H9A 103(3) . . ? H10 O10 H10A 98(3) . . ? N1 C1 C2 122.20(17) . . ? N1 C1 H1 122.3(14) . . ? C2 C1 H1 115.5(14) . . ? N2 C2 N3 119.46(16) . . ? N2 C2 C1 119.95(18) . . ? N3 C2 C1 120.58(18) . . ? N1 C4 C3 120.43(18) . . ? N1 C4 H2 117.7(14) . . ? C3 C4 H2 121.9(14) . . ? N2 C3 C4 122.93(18) . . ? N2 C3 H3 119.9(13) . . ? C4 C3 H3 117.2(13) . . ? C1 N1 C4 117.50(15) . . ? C1 N1 Co1 119.78(12) . . ? C4 N1 Co1 122.06(12) . . ? C2 N2 C3 116.87(15) . . ? C2 N3 H3A 124.3(19) . . ? C2 N3 H3B 123(2) . . ? H3A N3 H3B 113(3) . . ? O8 S1 O5 110.66(10) . . ? O8 S1 O6 109.07(9) . . ? O5 S1 O6 109.72(9) . . ? O8 S1 O7 109.23(8) . . ? O5 S1 O7 109.01(8) . . ? O6 S1 O7 109.14(8) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.454 _refine_diff_density_min -0.545 _refine_diff_density_rms 0.068 #======= END data_4_Cd _database_code_depnum_ccdc_archive 'CCDC 752996' #TrackingRef 'Cpds_1-4_R.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; mu-2-aminopyrazine-diaqua-mu-sulfato cadmium(II) monohydrate ; _chemical_name_common 'mu-2-aminopyrazine-diaqua-mu-sulfato cadmium(ii) monohydrate' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H10 Cd N3 O6 S' _chemical_formula_weight 340.61 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M c2/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 19.4038(4) _cell_length_b 7.3913(4) _cell_length_c 6.6216(3) _cell_angle_alpha 90.00 _cell_angle_beta 106.7190(10) _cell_angle_gamma 90.00 _cell_volume 909.52(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 25.29 _exptl_crystal_description rod _exptl_crystal_colour colorless _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.487 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 668 _exptl_absorpt_coefficient_mu 2.647 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.727363 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ; Siemens SMART CCD area detector diffractometer ; _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1729 _diffrn_reflns_av_R_equivalents 0.0207 _diffrn_reflns_av_sigmaI/netI 0.0149 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 25.29 _reflns_number_total 859 _reflns_number_gt 850 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement 'SAINT (Bruker, 2000)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material 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^)+(0.0682P)^2^+3.9868P] 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_number_reflns 859 _refine_ls_number_parameters 82 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0336 _refine_ls_R_factor_gt 0.0334 _refine_ls_wR_factor_ref 0.1104 _refine_ls_wR_factor_gt 0.1102 _refine_ls_goodness_of_fit_ref 1.264 _refine_ls_restrained_S_all 1.264 _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 Cd1 Cd 0.41072(2) 0.0000 0.25127(7) 0.0234(3) Uani 1 2 d S . . C1 C 0.4626(3) 0.4073(7) 0.2454(7) 0.0248(11) Uani 1 1 d . . . H1 H 0.5004 0.3460 0.2158 0.030 Uiso 1 1 calc R . . C2 C 0.3558(3) 0.4051(8) 0.3263(8) 0.0308(12) Uani 1 1 d . . . N1 N 0.4090(2) 0.3113(6) 0.2872(6) 0.0249(9) Uani 1 1 d . . . N2 N 0.2945(5) 0.3401(10) 0.3530(13) 0.0257(18) Uani 0.50 1 d P . . H2A H 0.2863 0.2255 0.3453 0.031 Uiso 0.50 1 calc PR . . H2B H 0.2633 0.4129 0.3778 0.031 Uiso 0.50 1 calc PR . . O1 O 0.3389(3) 0.0000 0.5564(8) 0.0313(12) Uani 1 2 d S . . O2 O 0.4658(3) 0.0000 0.6565(8) 0.0309(12) Uani 1 2 d S . . O3 O 0.4034(3) 0.1597(10) 0.8699(9) 0.084(2) Uani 1 1 d . . . O4 O 0.2898(3) 0.0000 0.0739(9) 0.0443(15) Uani 1 2 d S . . O5 O 0.1727(4) 0.0000 0.2108(11) 0.064(2) Uani 1 2 d S . . S1 S 0.40238(9) 0.0000 0.7401(2) 0.0265(5) Uani 1 2 d S . . 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 Cd1 0.0226(4) 0.0229(3) 0.0244(4) 0.000 0.0066(2) 0.000 C1 0.024(2) 0.031(3) 0.019(2) 0.0008(18) 0.0055(19) 0.0009(19) C2 0.026(3) 0.046(3) 0.019(2) 0.001(2) 0.005(2) -0.006(2) N1 0.030(2) 0.024(2) 0.0186(17) 0.0013(15) 0.0041(17) -0.0023(15) N2 0.029(4) 0.020(4) 0.035(5) -0.001(3) 0.019(4) 0.000(3) O1 0.028(3) 0.034(3) 0.025(2) 0.000 -0.003(2) 0.000 O2 0.027(3) 0.040(3) 0.031(3) 0.000 0.016(2) 0.000 O3 0.039(3) 0.139(6) 0.083(4) -0.087(4) 0.032(3) -0.027(3) O4 0.029(3) 0.069(4) 0.032(3) 0.000 0.005(3) 0.000 O5 0.032(4) 0.125(7) 0.035(3) 0.000 0.012(3) 0.000 S1 0.0178(8) 0.0477(12) 0.0148(8) 0.000 0.0061(7) 0.000 _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 Cd1 O2 2.297(5) 5_656 ? Cd1 O4 2.303(6) . ? Cd1 N1 2.315(4) . ? Cd1 N1 2.315(4) 6 ? Cd1 O2 2.587(5) . ? C1 N1 1.352(7) . ? C1 C1 1.370(10) 6_565 ? C1 H1 0.9300 . ? C2 N1 1.330(7) . ? C2 N2 1.341(10) . ? C2 C2 1.403(12) 6_565 ? N2 H2A 0.8600 . ? N2 H2B 0.8600 . ? O1 S1 1.461(5) . ? O2 S1 1.487(6) . ? O2 Cd1 2.297(5) 5_656 ? O3 S1 1.457(5) . ? S1 O3 1.457(5) 6 ? 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 Cd1 O4 165.5(2) 5_656 . ? O2 Cd1 N1 91.00(10) 5_656 . ? O4 Cd1 N1 90.55(10) . . ? O2 Cd1 N1 91.00(10) 5_656 6 ? O4 Cd1 N1 90.55(10) . 6 ? N1 Cd1 N1 167.6(2) . 6 ? O2 Cd1 O2 68.7(2) 5_656 . ? O4 Cd1 O2 125.8(2) . . ? N1 Cd1 O2 84.68(10) . . ? N1 Cd1 O2 84.68(10) 6 . ? N1 C1 C1 121.7(3) . 6_565 ? N1 C1 H1 119.2 . . ? C1 C1 H1 119.2 6_565 . ? N1 C2 N2 127.4(6) . . ? N1 C2 C2 121.4(3) . 6_565 ? N2 C2 C2 111.0(4) . 6_565 ? C2 N1 C1 116.9(5) . . ? C2 N1 Cd1 125.0(4) . . ? C1 N1 Cd1 117.8(3) . . ? C2 N2 H2A 120.0 . . ? C2 N2 H2B 120.0 . . ? H2A N2 H2B 120.0 . . ? S1 O2 Cd1 144.4(3) . 5_656 ? S1 O2 Cd1 104.3(3) . . ? Cd1 O2 Cd1 111.3(2) 5_656 . ? O3 S1 O3 108.2(6) . 6 ? O3 S1 O1 110.8(3) . . ? O3 S1 O1 110.8(3) 6 . ? O3 S1 O2 110.3(3) . . ? O3 S1 O2 110.3(3) 6 . ? O1 S1 O2 106.3(3) . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 25.29 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.750 _refine_diff_density_min -0.663 _refine_diff_density_rms 0.187