Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Ashutosh Ghosh' _publ_contact_author_address ; Department of Science University of Calcutta 92 APC Road Kolkata 700 009 INDIA ; _publ_contact_author_email 'GHOSH 59@YAHOO.COM' _publ_section_title ; The first metamagnetic thiocyanato-bridged one-dimensional nickel(II) complex ; _publ_section_references ; Oxford Diffraction Ltd, Crysalis Program (2005) Oxford Diffraction Ltd, Abspack Program (2005) Sheldrick, G.M. (1997) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (2004) PLATON program, Utrecht University, The Netherlands ; loop_ _publ_author_name 'Ghosh Ashutosh' 'Shouvik Chattopadhyay' 'Carmen Diaz' 'M. Drew' data_x _database_code_depnum_ccdc_archive 'CCDC 626916' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H15 N5 Ni S2' _chemical_formula_weight 352.12 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P212121 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' _cell_length_a 7.7083(7) _cell_length_b 12.2654(6) _cell_length_c 15.8917(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1502.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour black _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.557 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 728 _exptl_absorpt_coefficient_mu 1.565 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'ABSPACK, Oxford Diffraction Ltd' _exptl_absorpt_correction_T_min 0.879 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_standards_number ? _diffrn_measurement_device 'Oxford Diffaction X-Calibur System' _diffrn_measurement_method '321 frames, counting time 10 s.' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9754 _diffrn_reflns_av_R_equivalents 0.0411 _diffrn_reflns_av_sigmaI/netI 0.0583 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 29.98 _reflns_number_total 4281 _reflns_number_gt 3712 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Crysalis, Oxford Diffraction' _computing_cell_refinement 'Crysalis, Oxford Diffraction' _computing_data_reduction 'Crysalis, Oxford Diffraction' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics PLATON(Spek,2004) _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 ; w=1/[\s^2^(Fo^2^)+(0.0327P)^2^+1.2643P] 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 SHELXL _refine_ls_extinction_coef 0.0003(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.039(17) _refine_ls_number_reflns 4281 _refine_ls_number_parameters 183 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0609 _refine_ls_R_factor_gt 0.0479 _refine_ls_wR_factor_ref 0.0893 _refine_ls_wR_factor_gt 0.0837 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _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 N22 N 0.3969(4) 0.3296(2) 0.86395(19) 0.0249(7) Uani 1 1 d . . . H22A H 0.3425 0.2653 0.8710 0.030 Uiso 1 1 calc R . . H22B H 0.4531 0.3445 0.9123 0.030 Uiso 1 1 calc R . . N11 N 0.7521(3) 0.3013(2) 0.67075(17) 0.0172(5) Uani 1 1 d . . . C17 C 0.5485(5) 0.4317(2) 0.6175(2) 0.0216(7) Uani 1 1 d . . . C19 C 0.2865(5) 0.4578(3) 0.6948(3) 0.0258(8) Uani 1 1 d . . . H19A H 0.2206 0.4526 0.6429 0.031 Uiso 1 1 calc R . . H19B H 0.3027 0.5346 0.7072 0.031 Uiso 1 1 calc R . . C16 C 0.7150(5) 0.3711(2) 0.6074(2) 0.0177(7) Uani 1 1 d . . . C20 C 0.1833(5) 0.4063(3) 0.7649(3) 0.0316(9) Uani 1 1 d . . . H20A H 0.0695 0.4400 0.7663 0.038 Uiso 1 1 calc R . . H20B H 0.1671 0.3298 0.7519 0.038 Uiso 1 1 calc R . . C12 C 0.8911(5) 0.2370(3) 0.6643(2) 0.0229(8) Uani 1 1 d . . . H12 H 0.9157 0.1886 0.7078 0.027 Uiso 1 1 calc R . . C14 C 0.9650(5) 0.3133(3) 0.5316(2) 0.0283(8) Uani 1 1 d . . . H14 H 1.0374 0.3176 0.4849 0.034 Uiso 1 1 calc R . . C21 C 0.2623(5) 0.4149(3) 0.8512(3) 0.0312(9) Uani 1 1 d . . . H21A H 0.3142 0.4864 0.8581 0.037 Uiso 1 1 calc R . . H21B H 0.1723 0.4068 0.8934 0.037 Uiso 1 1 calc R . . C13 C 1.0000(5) 0.2400(3) 0.5951(2) 0.0289(9) Uani 1 1 d . . . H13 H 1.0949 0.1934 0.5915 0.035 Uiso 1 1 calc R . . C15 C 0.8212(5) 0.3803(3) 0.5378(2) 0.0230(8) Uani 1 1 d . . . H15 H 0.7964 0.4307 0.4958 0.028 Uiso 1 1 calc R . . N18 N 0.4569(4) 0.4071(2) 0.68216(19) 0.0191(6) Uani 1 1 d . . . Ni1 Ni 0.57927(5) 0.31051(3) 0.77092(3) 0.01727(10) Uani 1 1 d . . . S100 S 0.26708(12) -0.01166(6) 0.67239(6) 0.02072(18) Uani 1 1 d . . . S200 S 1.04743(14) 0.15243(9) 0.92791(7) 0.0387(3) Uani 1 1 d . . . C200 C 0.8746(5) 0.2034(3) 0.8837(2) 0.0214(7) Uani 1 1 d . . . N100 N 0.4562(4) 0.1689(2) 0.7309(2) 0.0247(6) Uani 1 1 d . . . C100 C 0.3774(4) 0.0950(2) 0.7073(2) 0.0201(7) Uani 1 1 d . . . N200 N 0.7519(4) 0.2371(2) 0.85042(19) 0.0220(6) Uani 1 1 d . . . C171 C 0.4955(5) 0.5140(3) 0.5524(3) 0.0329(9) Uani 1 1 d . . . H17A H 0.4273 0.5701 0.5785 0.039 Uiso 1 1 calc R . . H17B H 0.4281 0.4787 0.5095 0.039 Uiso 1 1 calc R . . H17C H 0.5972 0.5457 0.5277 0.039 Uiso 1 1 calc 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 N22 0.0228(16) 0.0241(14) 0.0277(16) -0.0018(12) 0.0055(13) -0.0041(12) N11 0.0184(14) 0.0163(11) 0.0168(13) -0.0001(11) -0.0049(11) -0.0006(11) C17 0.025(2) 0.0187(14) 0.0209(17) -0.0041(13) -0.0081(15) 0.0001(13) C19 0.0205(19) 0.0199(15) 0.037(2) -0.0028(15) -0.0075(16) 0.0057(13) C16 0.0218(17) 0.0169(14) 0.0142(16) -0.0025(12) -0.0001(14) 0.0003(12) C20 0.0183(18) 0.0329(18) 0.044(3) -0.0092(19) 0.0002(18) 0.0023(14) C12 0.024(2) 0.0177(14) 0.0272(19) -0.0042(14) -0.0049(16) 0.0050(13) C14 0.031(2) 0.0347(17) 0.0196(17) -0.0030(16) 0.0073(14) -0.0024(17) C21 0.027(2) 0.0313(18) 0.035(2) -0.0025(17) 0.0101(18) 0.0033(17) C13 0.0242(19) 0.0303(18) 0.032(2) -0.0044(16) -0.0006(17) 0.0088(15) C15 0.0247(19) 0.0252(16) 0.0193(19) 0.0012(14) -0.0016(15) -0.0041(14) N18 0.0176(15) 0.0161(11) 0.0235(15) -0.0026(11) -0.0058(12) 0.0006(10) Ni1 0.01623(19) 0.01590(17) 0.0197(2) 0.00019(17) -0.00034(19) 0.00017(16) S100 0.0206(4) 0.0180(3) 0.0235(4) 0.0024(3) -0.0048(3) -0.0021(3) S200 0.0256(6) 0.0507(6) 0.0397(6) 0.0179(5) -0.0042(5) 0.0050(4) C200 0.0273(19) 0.0177(15) 0.0191(17) 0.0027(13) 0.0019(14) -0.0034(13) N100 0.0239(15) 0.0178(12) 0.0325(16) 0.0029(13) -0.0014(14) -0.0001(10) C100 0.0221(18) 0.0163(14) 0.0219(18) 0.0037(13) 0.0005(13) 0.0040(12) N200 0.0227(16) 0.0206(12) 0.0226(15) 0.0010(11) -0.0004(13) -0.0003(12) C171 0.038(2) 0.0287(18) 0.032(2) 0.0053(17) -0.0037(18) 0.0100(17) _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 N22 C21 1.488(5) . ? N22 Ni1 2.053(3) . ? N11 C12 1.334(4) . ? N11 C16 1.352(4) . ? N11 Ni1 2.079(3) . ? C17 N18 1.283(4) . ? C17 C16 1.493(5) . ? C17 C171 1.501(5) . ? C19 N18 1.468(4) . ? C19 C20 1.508(6) . ? C16 C15 1.380(5) . ? C20 C21 1.504(6) . ? C12 C13 1.385(5) . ? C14 C13 1.378(5) . ? C14 C15 1.383(5) . ? N18 Ni1 2.069(3) . ? Ni1 N200 2.043(3) . ? Ni1 N100 2.079(3) . ? Ni1 S100 2.6404(9) 3_656 ? S100 C100 1.656(3) . ? S100 Ni1 2.6404(9) 3_646 ? S200 C200 1.631(4) . ? C200 N200 1.160(4) . ? N100 C100 1.154(4) . ? 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 C21 N22 Ni1 117.4(2) . . ? C12 N11 C16 119.2(3) . . ? C12 N11 Ni1 127.2(2) . . ? C16 N11 Ni1 113.6(2) . . ? N18 C17 C16 116.2(3) . . ? N18 C17 C171 124.1(3) . . ? C16 C17 C171 119.7(3) . . ? N18 C19 C20 113.3(3) . . ? N11 C16 C15 121.5(3) . . ? N11 C16 C17 114.7(3) . . ? C15 C16 C17 123.7(3) . . ? C21 C20 C19 115.5(3) . . ? N11 C12 C13 122.1(3) . . ? C13 C14 C15 119.4(3) . . ? N22 C21 C20 110.9(3) . . ? C14 C13 C12 118.8(3) . . ? C14 C15 C16 118.9(3) . . ? C17 N18 C19 120.1(3) . . ? C17 N18 Ni1 115.5(2) . . ? C19 N18 Ni1 123.9(2) . . ? N200 Ni1 N22 92.90(12) . . ? N200 Ni1 N100 96.81(11) . . ? N22 Ni1 N100 90.18(12) . . ? N200 Ni1 N11 91.85(11) . . ? N22 Ni1 N11 175.02(11) . . ? N100 Ni1 N11 90.73(11) . . ? N200 Ni1 N18 165.98(12) . . ? N22 Ni1 N18 96.52(12) . . ? N100 Ni1 N18 93.53(11) . . ? N11 Ni1 N18 78.54(11) . . ? N200 Ni1 S100 82.00(8) . 3_656 ? N22 Ni1 S100 88.12(8) . 3_656 ? N100 Ni1 S100 177.87(9) . 3_656 ? N11 Ni1 S100 91.07(7) . 3_656 ? N18 Ni1 S100 87.94(8) . 3_656 ? C100 S100 Ni1 107.93(12) . 3_646 ? N200 C200 S200 177.9(3) . . ? C100 N100 Ni1 175.0(3) . . ? N100 C100 S100 179.0(3) . . ? C200 N200 Ni1 165.9(3) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 29.98 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.434 _refine_diff_density_min -0.569 _refine_diff_density_rms 0.089 _publ_section_references ; Oxford Diffraction Ltd, Crysalis Program (2005) Oxford Diffraction Ltd, Abspack Program (2005) Sheldrick, G.M. (1997) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (2004) PLATON program, Utrecht University, The Netherlands ; #===END