Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_t _database_code_CSD 169414 _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Meng, Qingjin' 'Ren, Xiao-Ming' 'Song, You' 'Xie, Jingli' 'Zhou, Yang' _publ_contact_author_name 'Prof Qingjin Meng' _publ_contact_author_address ; Coordination Chemistry Institute 22 Hankou Road Nanjing City Jiangsu 210093 CHINA ; _publ_contact_author_email 'NJUXJL@263.NET' _publ_section_title ; Synthesis, crystal structure and magnetic property of a novel one-dimensional nickel(III) chain complex showing ferromagnetic ordering in low temperature ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H10 Br F N5 Ni S4' _chemical_formula_weight 606.19 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' 'F' 'F' 0.0171 0.0103 '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' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.989(2) _cell_length_b 26.363(5) _cell_length_c 7.4860(15) _cell_angle_alpha 90.00 _cell_angle_beta 101.63(3) _cell_angle_gamma 90.00 _cell_volume 2317.5(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 3.56 _cell_measurement_theta_max 13.50 _exptl_crystal_description needle _exptl_crystal_colour dark _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.737 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1204 _exptl_absorpt_coefficient_mu 2.949 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.684 _exptl_absorpt_correction_T_max 0.782 _exptl_absorpt_process_details '(North, et.al, 1984)' _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 'CAD 4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 3.60 _diffrn_reflns_number 4353 _diffrn_reflns_av_R_equivalents 0.0470 _diffrn_reflns_av_sigmaI/netI 0.0536 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 24.97 _reflns_number_total 4022 _reflns_number_gt 2493 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD-4 Software (Enraf-Nonius 1990)' _computing_cell_refinement 'CAD-4 Software (Enraf-Nonius 1990)' _computing_data_reduction 'CAD-4 Software (Enraf-Nonius 1990)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXS-97 (Sheldrick, 1990)' _computing_publication_material 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.2000P)^2^+22.5000P] 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 SHELXL _refine_ls_extinction_coef 0.0080(17) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4022 _refine_ls_number_parameters 290 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1506 _refine_ls_R_factor_gt 0.0793 _refine_ls_wR_factor_ref 0.3529 _refine_ls_wR_factor_gt 0.2233 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.083 _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 0.25984(14) 0.72565(6) 1.0428(2) 0.0446(6) Uani 1 1 d . . . S1 S 0.1539(3) 0.66183(13) 0.9432(5) 0.0527(9) Uani 1 1 d . . . S2 S 0.4014(3) 0.67808(13) 1.1556(5) 0.0542(9) Uani 1 1 d . . . S3 S 0.3762(3) 0.78676(13) 1.1283(5) 0.0519(9) Uani 1 1 d . . . S4 S 0.1234(3) 0.77624(13) 0.9340(5) 0.0516(9) Uani 1 1 d . . . N1 N 0.1690(14) 0.5226(5) 0.881(2) 0.084(4) Uani 1 1 d . . . N2 N 0.5070(14) 0.5479(6) 1.167(2) 0.091(5) Uani 1 1 d . . . N3 N 0.3975(13) 0.9256(5) 1.111(2) 0.082(4) Uani 1 1 d . . . N4 N 0.0634(11) 0.9114(6) 0.865(2) 0.082(4) Uani 1 1 d . . . C1 C 0.2057(14) 0.5604(6) 0.938(2) 0.064(4) Uani 1 1 d . . . C2 C 0.2436(12) 0.6116(5) 0.9952(17) 0.052(3) Uani 1 1 d . . . C3 C 0.3561(12) 0.6188(5) 1.0888(18) 0.053(3) Uani 1 1 d . . . C4 C 0.4371(13) 0.5781(5) 1.1313(19) 0.057(4) Uani 1 1 d . . . C5 C 0.3533(12) 0.8883(5) 1.0908(19) 0.051(3) Uani 1 1 d . . . C6 C 0.2959(9) 0.8388(5) 1.0547(16) 0.040(3) Uani 1 1 d . . . C7 C 0.1845(12) 0.8341(4) 0.9717(18) 0.048(3) Uani 1 1 d . . . C8 C 0.1151(12) 0.8793(5) 0.910(2) 0.054(3) Uani 1 1 d . . . Br1 Br 0.7231(2) 0.83193(6) 1.0010(2) 0.0823(7) Uani 1 1 d . . . F1 F 0.5781(7) 0.6481(3) 0.9037(13) 0.071(2) Uani 1 1 d . . . N5 N 0.7783(10) 0.5727(4) 0.8830(15) 0.051(3) Uani 1 1 d . . . C9 C 0.6845(16) 0.5540(5) 0.784(2) 0.068(4) Uani 1 1 d . . . H9A H 0.6176 0.5567 0.8279 0.081 Uiso 1 1 calc R . . C10 C 0.6796(16) 0.5310(6) 0.619(2) 0.078(5) Uani 1 1 d . . . H10A H 0.6117 0.5187 0.5502 0.093 Uiso 1 1 calc R . . C11 C 0.784(2) 0.5270(6) 0.560(3) 0.088(6) Uani 1 1 d . . . H11A H 0.7859 0.5108 0.4505 0.106 Uiso 1 1 calc R . . C12 C 0.8795(17) 0.5461(6) 0.661(3) 0.077(5) Uani 1 1 d . . . H12A H 0.9484 0.5431 0.6227 0.092 Uiso 1 1 calc R . . C13 C 0.8739(13) 0.5699(6) 0.818(3) 0.075(5) Uani 1 1 d . . . H13A H 0.9395 0.5850 0.8841 0.090 Uiso 1 1 calc R . . C14 C 0.7803(12) 0.5991(5) 1.057(2) 0.057(3) Uani 1 1 d . . . H14A H 0.8509 0.5914 1.1414 0.068 Uiso 1 1 calc R . . H14B H 0.7179 0.5870 1.1104 0.068 Uiso 1 1 calc R . . C15 C 0.7700(12) 0.6563(5) 1.0312(17) 0.051(3) Uani 1 1 d . . . C16 C 0.6686(13) 0.6779(5) 0.9655(19) 0.054(3) Uani 1 1 d . . . C17 C 0.6516(13) 0.7304(5) 0.9534(19) 0.058(4) Uani 1 1 d . . . H17A H 0.5800 0.7439 0.9071 0.069 Uiso 1 1 calc R . . C18 C 0.7415(11) 0.7607(6) 1.0104(18) 0.055(3) Uani 1 1 d . . . C19 C 0.8511(14) 0.7397(6) 1.078(2) 0.066(4) Uani 1 1 d . . . H19A H 0.9144 0.7606 1.1116 0.079 Uiso 1 1 calc R . . C20 C 0.8609(14) 0.6879(6) 1.091(2) 0.068(4) Uani 1 1 d . . . H20A H 0.9311 0.6738 1.1425 0.081 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 0.0426(10) 0.0474(10) 0.0429(10) 0.0034(7) 0.0062(7) -0.0016(7) S1 0.0475(18) 0.0505(18) 0.058(2) -0.0007(14) 0.0054(15) -0.0048(14) S2 0.0511(19) 0.0542(19) 0.054(2) -0.0006(15) 0.0033(15) 0.0018(15) S3 0.0431(18) 0.0500(18) 0.057(2) 0.0032(14) -0.0042(15) -0.0024(14) S4 0.0406(17) 0.0527(19) 0.056(2) -0.0004(14) -0.0030(15) -0.0013(14) N1 0.098(11) 0.065(9) 0.090(10) 0.002(8) 0.025(9) -0.020(8) N2 0.077(10) 0.077(10) 0.110(13) -0.011(9) -0.003(9) 0.026(8) N3 0.071(9) 0.061(9) 0.108(12) -0.002(8) 0.000(8) 0.001(7) N4 0.046(7) 0.083(10) 0.115(12) -0.008(9) 0.009(8) 0.006(7) C1 0.059(9) 0.068(10) 0.060(9) -0.010(7) 0.003(7) -0.010(7) C2 0.069(9) 0.040(7) 0.048(7) 0.011(5) 0.010(7) -0.005(6) C3 0.066(9) 0.047(7) 0.053(8) 0.013(6) 0.030(7) 0.001(6) C4 0.063(9) 0.057(8) 0.053(8) 0.016(6) 0.016(7) 0.009(7) C5 0.055(8) 0.042(7) 0.056(8) 0.005(6) 0.008(6) 0.000(6) C6 0.029(6) 0.048(7) 0.042(7) 0.000(5) 0.005(5) -0.002(5) C7 0.061(8) 0.038(6) 0.046(7) 0.000(5) 0.014(6) 0.010(6) C8 0.055(8) 0.037(7) 0.067(9) 0.010(6) 0.004(7) 0.011(6) Br1 0.1308(18) 0.0570(10) 0.0613(10) -0.0073(7) 0.0247(10) -0.0131(9) F1 0.046(4) 0.062(5) 0.097(7) -0.009(5) -0.004(4) -0.003(4) N5 0.054(7) 0.045(6) 0.049(6) 0.002(5) -0.003(5) 0.005(5) C9 0.087(11) 0.042(7) 0.074(10) -0.011(7) 0.016(9) -0.012(7) C10 0.091(13) 0.051(9) 0.076(11) -0.020(8) -0.016(10) -0.006(8) C11 0.131(19) 0.051(9) 0.087(13) 0.013(9) 0.030(13) 0.006(11) C12 0.078(12) 0.064(10) 0.099(14) 0.007(9) 0.044(11) 0.001(9) C13 0.049(9) 0.076(10) 0.108(14) -0.030(10) 0.033(9) -0.010(7) C14 0.050(8) 0.064(9) 0.059(8) 0.016(7) 0.017(7) 0.006(6) C15 0.061(8) 0.055(8) 0.035(7) -0.004(5) 0.006(6) 0.007(6) C16 0.060(8) 0.054(8) 0.051(8) -0.003(6) 0.016(7) -0.009(7) C17 0.058(8) 0.051(8) 0.056(8) -0.007(6) -0.007(7) 0.015(6) C18 0.046(8) 0.074(9) 0.046(7) -0.003(6) 0.009(6) -0.001(7) C19 0.066(10) 0.069(10) 0.067(10) 0.007(7) 0.023(8) -0.010(8) C20 0.059(9) 0.077(11) 0.068(10) -0.010(8) 0.015(8) 0.010(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 Ni1 S4 2.140(4) . ? Ni1 S2 2.142(4) . ? Ni1 S3 2.143(4) . ? Ni1 S1 2.149(4) . ? S1 C2 1.702(14) . ? S2 C3 1.696(14) . ? S3 C6 1.702(12) . ? S4 C7 1.690(13) . ? N1 C1 1.137(19) . ? N2 C4 1.146(19) . ? N3 C5 1.112(18) . ? N4 C8 1.063(18) . ? C1 C2 1.46(2) . ? C2 C3 1.40(2) . ? C3 C4 1.440(19) . ? C5 C6 1.476(18) . ? C6 C7 1.360(18) . ? C7 C8 1.475(17) . ? Br1 C18 1.891(16) . ? F1 C16 1.342(16) . ? N5 C9 1.312(19) . ? N5 C13 1.334(19) . ? N5 C14 1.475(18) . ? C9 C10 1.36(2) . ? C10 C11 1.41(3) . ? C11 C12 1.34(3) . ? C12 C13 1.35(2) . ? C14 C15 1.52(2) . ? C15 C16 1.34(2) . ? C15 C20 1.37(2) . ? C16 C17 1.402(19) . ? C17 C18 1.34(2) . ? C18 C19 1.42(2) . ? C19 C20 1.37(2) . ? 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 S4 Ni1 S2 177.28(15) . . ? S4 Ni1 S3 92.67(14) . . ? S2 Ni1 S3 84.62(14) . . ? S4 Ni1 S1 90.16(14) . . ? S2 Ni1 S1 92.55(15) . . ? S3 Ni1 S1 174.88(16) . . ? C2 S1 Ni1 103.2(5) . . ? C3 S2 Ni1 104.0(5) . . ? C6 S3 Ni1 102.6(4) . . ? C7 S4 Ni1 103.1(5) . . ? N1 C1 C2 173.7(18) . . ? C3 C2 C1 118.9(13) . . ? C3 C2 S1 120.5(10) . . ? C1 C2 S1 120.5(11) . . ? C2 C3 C4 123.1(13) . . ? C2 C3 S2 119.4(10) . . ? C4 C3 S2 117.4(11) . . ? N2 C4 C3 175.6(17) . . ? N3 C5 C6 177.2(16) . . ? C7 C6 C5 122.9(11) . . ? C7 C6 S3 120.9(9) . . ? C5 C6 S3 116.2(9) . . ? C6 C7 C8 120.6(11) . . ? C6 C7 S4 120.8(9) . . ? C8 C7 S4 118.6(11) . . ? N4 C8 C7 178.7(17) . . ? C9 N5 C13 118.3(14) . . ? C9 N5 C14 122.5(13) . . ? C13 N5 C14 119.1(12) . . ? N5 C9 C10 123.7(17) . . ? C9 C10 C11 115.9(16) . . ? C12 C11 C10 120.6(18) . . ? C11 C12 C13 118.6(18) . . ? N5 C13 C12 122.8(16) . . ? N5 C14 C15 111.7(11) . . ? C16 C15 C20 117.7(14) . . ? C16 C15 C14 120.7(13) . . ? C20 C15 C14 121.3(13) . . ? C15 C16 F1 119.3(13) . . ? C15 C16 C17 123.4(14) . . ? F1 C16 C17 117.2(13) . . ? C18 C17 C16 118.1(14) . . ? C17 C18 C19 120.6(16) . . ? C17 C18 Br1 119.9(11) . . ? C19 C18 Br1 119.5(12) . . ? C20 C19 C18 118.2(15) . . ? C15 C20 C19 121.9(15) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.035 _refine_diff_density_min -1.200 _refine_diff_density_rms 0.260