Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_1 _database_code_CSD 179243 _journal_coden_Cambridge 186 loop_ _publ_author_name 'Xiao Ming Ren' 'Youcun Chen' 'Cheng He' 'Song Gao' _publ_contact_author_name 'Dr Xiao Ming Ren' _publ_contact_author_address ; Chemicalservice Group Max-Planck-Institut fur Festkorperforschung Heisenbergstrasse 1 Stuttgart 800665 GERMANY ; _publ_contact_author_email 'X.REN@FKF.MPG.DE' _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Spontaneous magnetization below 7.7 K based on a novel 3-D H-bonding network material: Synthesis, crystal structure and magnetic property ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H7 N6 Ni S4' _chemical_formula_weight 434.20 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' '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 'Monoclinic' _symmetry_space_group_name_H-M 'C2/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 41.3120(10) _cell_length_b 6.4570(10) _cell_length_c 12.9580(10) _cell_angle_alpha 90.00 _cell_angle_beta 93.730(10) _cell_angle_gamma 90.00 _cell_volume 3449.2(6) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Plate _exptl_crystal_colour Brown _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.672 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1752 _exptl_absorpt_coefficient_mu 1.616 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.99 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ? _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 '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 8385 _diffrn_reflns_av_R_equivalents 0.0626 _diffrn_reflns_av_sigmaI/netI 0.0447 _diffrn_reflns_limit_h_min -48 _diffrn_reflns_limit_h_max 48 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 24.99 _reflns_number_total 3034 _reflns_number_gt 2698 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1000P)^2^+1.9900P] 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 3034 _refine_ls_number_parameters 220 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0543 _refine_ls_R_factor_gt 0.0510 _refine_ls_wR_factor_ref 0.1525 _refine_ls_wR_factor_gt 0.1496 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.092 _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 Ni1 Ni 0.2500 0.2500 0.5000 0.0446(2) Uani 1 2 d S . . Ni2 Ni 0.5000 0.0000 0.5000 0.0511(2) Uani 1 2 d S . . S1 S 0.26434(2) 0.41952(15) 0.36797(7) 0.0539(3) Uani 1 1 d . . . S2 S 0.27574(2) -0.02210(15) 0.45816(8) 0.0560(3) Uani 1 1 d . . . S3 S 0.46926(3) 0.13521(18) 0.60917(7) 0.0625(3) Uani 1 1 d . . . S4 S 0.48843(2) 0.23435(16) 0.38628(8) 0.0574(3) Uani 1 1 d . . . N1 N 0.31543(9) 0.3557(5) 0.1437(3) 0.0627(9) Uani 1 1 d . . . N2 N 0.32984(8) -0.2088(6) 0.2598(3) 0.0599(8) Uani 1 1 d . . . N3 N 0.41434(8) 0.5872(6) 0.6324(3) 0.0635(9) Uani 1 1 d . . . N4 N 0.43666(9) 0.7021(6) 0.3488(3) 0.0622(8) Uani 1 1 d . . . N5 N 0.35037(8) 0.2931(6) 0.5428(3) 0.0596(8) Uani 1 1 d . . . H5A H 0.3394 0.3323 0.5934 0.071 Uiso 1 1 calc R . . N6 N 0.40293(7) 0.1102(5) 0.3043(2) 0.0575(8) Uani 1 1 d . . . H6A H 0.4128 -0.0070 0.3072 0.069 Uiso 1 1 calc R . . H6B H 0.4043 0.1890 0.2512 0.069 Uiso 1 1 calc R . . C1 C 0.30282(10) 0.3070(7) 0.2161(3) 0.0576(9) Uani 1 1 d . . . C2 C 0.28767(10) 0.2426(6) 0.3074(3) 0.0537(9) Uani 1 1 d . . . C3 C 0.29280(9) 0.0490(6) 0.3472(3) 0.0536(9) Uani 1 1 d . . . C4 C 0.31312(10) -0.0961(6) 0.2984(3) 0.0563(9) Uani 1 1 d . . . C5 C 0.43202(10) 0.4805(7) 0.5945(3) 0.0594(10) Uani 1 1 d . . . C6 C 0.45376(9) 0.3501(6) 0.5439(3) 0.0564(9) Uani 1 1 d . . . C7 C 0.46221(9) 0.3937(6) 0.4461(3) 0.0560(9) Uani 1 1 d . . . C8 C 0.44847(9) 0.5669(7) 0.3910(3) 0.0585(9) Uani 1 1 d . . . C9 C 0.35256(9) 0.4193(7) 0.4609(3) 0.0582(9) Uani 1 1 d . . . H9 H 0.3420 0.5465 0.4598 0.070 Uiso 1 1 calc R . . C10 C 0.36977(9) 0.3646(6) 0.3805(3) 0.0565(9) Uani 1 1 d . . . H10 H 0.3713 0.4542 0.3248 0.068 Uiso 1 1 calc R . . C11 C 0.38567(10) 0.1690(7) 0.3810(3) 0.0565(9) Uani 1 1 d . . . C12 C 0.38276(10) 0.0448(7) 0.4696(3) 0.0589(10) Uani 1 1 d . . . H12 H 0.3932 -0.0827 0.4750 0.071 Uiso 1 1 calc R . . C13 C 0.36465(9) 0.1118(7) 0.5472(3) 0.0596(10) Uani 1 1 d . . . H13 H 0.3624 0.0272 0.6043 0.071 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 Ni1 0.0407(4) 0.0549(4) 0.0389(4) 0.0028(2) 0.0077(3) 0.0017(2) Ni2 0.0494(4) 0.0688(5) 0.0358(4) -0.0063(3) 0.0088(3) 0.0072(3) S1 0.0602(6) 0.0559(6) 0.0466(6) 0.0079(4) 0.0121(4) 0.0085(4) S2 0.0624(6) 0.0562(6) 0.0517(6) 0.0067(4) 0.0206(5) 0.0071(4) S3 0.0672(6) 0.0844(7) 0.0375(6) -0.0003(4) 0.0150(4) 0.0205(5) S4 0.0584(6) 0.0761(7) 0.0393(6) -0.0036(4) 0.0151(4) 0.0096(4) N1 0.069(2) 0.071(2) 0.049(2) -0.0025(15) 0.0116(17) -0.0078(17) N2 0.063(2) 0.0661(19) 0.052(2) -0.0041(15) 0.0138(16) 0.0023(16) N3 0.0628(19) 0.079(2) 0.049(2) -0.0088(16) 0.0082(16) 0.0101(18) N4 0.061(2) 0.075(2) 0.051(2) -0.0043(17) 0.0078(16) 0.0101(18) N5 0.0580(19) 0.076(2) 0.045(2) 0.0004(15) 0.0064(15) -0.0016(17) N6 0.0597(18) 0.072(2) 0.0416(18) 0.0061(14) 0.0080(14) 0.0016(15) C1 0.063(2) 0.066(2) 0.045(2) -0.0032(18) 0.0100(18) -0.0047(19) C2 0.057(2) 0.062(2) 0.043(2) -0.0046(15) 0.0103(17) -0.0032(16) C3 0.056(2) 0.060(2) 0.046(2) -0.0035(16) 0.0115(16) -0.0006(17) C4 0.059(2) 0.062(2) 0.048(2) -0.0040(17) 0.0119(17) -0.0001(19) C5 0.059(2) 0.075(3) 0.045(2) -0.0089(18) 0.0084(18) 0.0082(19) C6 0.055(2) 0.071(2) 0.043(2) -0.0089(17) 0.0084(16) 0.0075(18) C7 0.054(2) 0.070(2) 0.044(2) -0.0088(17) 0.0088(17) 0.0075(18) C8 0.057(2) 0.072(3) 0.047(2) -0.0065(19) 0.0093(18) 0.009(2) C9 0.057(2) 0.073(2) 0.045(2) 0.0009(18) 0.0046(17) -0.0006(19) C10 0.056(2) 0.071(2) 0.043(2) 0.0033(16) 0.0047(16) -0.0008(18) C11 0.057(2) 0.071(2) 0.042(2) 0.0046(17) 0.0069(16) -0.0002(18) C12 0.059(2) 0.073(2) 0.044(2) 0.0052(17) 0.0070(18) -0.0003(19) C13 0.060(2) 0.075(3) 0.044(2) 0.0041(17) 0.0068(18) -0.002(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 Ni1 S2 2.1416(9) . ? Ni1 S2 2.1416(9) 7_556 ? Ni1 S1 2.1466(9) 7_556 ? Ni1 S1 2.1466(9) . ? Ni2 S4 2.1443(10) 5_656 ? Ni2 S4 2.1443(10) . ? Ni2 S3 2.1471(9) . ? Ni2 S3 2.1471(9) 5_656 ? S1 C2 1.717(4) . ? S2 C3 1.704(4) . ? S3 C6 1.726(4) . ? S4 C7 1.715(4) . ? N1 C1 1.146(5) . ? N2 C4 1.141(5) . ? N3 C5 1.138(5) . ? N4 C8 1.124(5) . ? N5 C13 1.310(5) . ? N5 C9 1.346(5) . ? N5 H5A 0.8600 . ? N6 C11 1.317(5) . ? N6 H6A 0.8600 . ? N6 H6B 0.8600 . ? C1 C2 1.435(6) . ? C2 C3 1.364(5) . ? C3 C4 1.432(5) . ? C5 C6 1.423(5) . ? C6 C7 1.366(6) . ? C7 C8 1.424(6) . ? C9 C10 1.346(6) . ? C9 H9 0.9300 . ? C10 C11 1.423(6) . ? C10 H10 0.9300 . ? C11 C12 1.412(6) . ? C12 C13 1.362(6) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? 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 S2 Ni1 S2 180.00(6) . 7_556 ? S2 Ni1 S1 87.18(4) . 7_556 ? S2 Ni1 S1 92.82(4) 7_556 7_556 ? S2 Ni1 S1 92.82(4) . . ? S2 Ni1 S1 87.18(4) 7_556 . ? S1 Ni1 S1 180.00(5) 7_556 . ? S4 Ni2 S4 180.00(5) 5_656 . ? S4 Ni2 S3 87.08(4) 5_656 . ? S4 Ni2 S3 92.92(4) . . ? S4 Ni2 S3 92.92(4) 5_656 5_656 ? S4 Ni2 S3 87.08(4) . 5_656 ? S3 Ni2 S3 180.00(5) . 5_656 ? C2 S1 Ni1 102.55(14) . . ? C3 S2 Ni1 103.42(14) . . ? C6 S3 Ni2 102.72(13) . . ? C7 S4 Ni2 103.42(15) . . ? C13 N5 C9 121.4(4) . . ? C13 N5 H5A 119.3 . . ? C9 N5 H5A 119.3 . . ? C11 N6 H6A 120.0 . . ? C11 N6 H6B 120.0 . . ? H6A N6 H6B 120.0 . . ? N1 C1 C2 178.6(5) . . ? C3 C2 C1 120.8(3) . . ? C3 C2 S1 121.0(3) . . ? C1 C2 S1 118.2(3) . . ? C2 C3 C4 120.9(4) . . ? C2 C3 S2 120.2(3) . . ? C4 C3 S2 118.9(3) . . ? N2 C4 C3 178.6(4) . . ? N3 C5 C6 178.1(5) . . ? C7 C6 C5 120.9(4) . . ? C7 C6 S3 120.8(3) . . ? C5 C6 S3 118.4(3) . . ? C6 C7 C8 120.6(3) . . ? C6 C7 S4 120.2(3) . . ? C8 C7 S4 119.2(3) . . ? N4 C8 C7 177.7(4) . . ? C10 C9 N5 121.2(4) . . ? C10 C9 H9 119.4 . . ? N5 C9 H9 119.4 . . ? C9 C10 C11 119.7(4) . . ? C9 C10 H10 120.1 . . ? C11 C10 H10 120.1 . . ? N6 C11 C12 122.0(4) . . ? N6 C11 C10 121.6(4) . . ? C12 C11 C10 116.4(4) . . ? C13 C12 C11 120.0(4) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? N5 C13 C12 121.3(4) . . ? N5 C13 H13 119.4 . . ? C12 C13 H13 119.4 . . ? 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 N5 H5A N1 0.86 2.35 3.030(5) 135.7 6_566 N5 H5A N2 0.86 2.36 3.039(5) 136.6 6_556 N6 H6A N4 0.86 2.17 3.019(5) 168.1 1_545 N6 H6B N3 0.86 2.17 3.023(5) 170.4 6_565 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.558 _refine_diff_density_min -0.570 _refine_diff_density_rms 0.088