Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Dr Jing-Min Shi' _publ_contact_author_address ; Department of Chemistry Shandong Normal University Jinan 250014 CHINA ; _publ_contact_author_email SHIJINGMIN@BEELINK.COM _publ_section_title ; Synthesis, crystal structure, magnetic property and theoretical studies on a one-dimensional polynuclear copper(II) complex [Cu2(?1,3-SCN)2(?'1,3-SCN)2(MPyO)2]n ; loop_ _publ_author_name 'Jing-Min Shi' 'Peng Cheng' 'Zhe Liu' 'Lian-Dong Liu' 'Wei Shi' ; You Min Sun ; data_41029bm _database_code_depnum_ccdc_archive 'CCDC 254314' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H28 Cu4 N12 O4 S8' _chemical_formula_weight 1155.30 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 5.624(4) _cell_length_b 17.691(11) _cell_length_c 11.076(7) _cell_angle_alpha 90.00 _cell_angle_beta 103.621(8) _cell_angle_gamma 90.00 _cell_volume 1071.0(12) _cell_formula_units_Z 1 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 1277 _cell_measurement_theta_min 2.2145 _cell_measurement_theta_max 24.617 _exptl_crystal_description rhombohedron _exptl_crystal_colour brown _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.791 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 580 _exptl_absorpt_coefficient_mu 2.402 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7146 _exptl_absorpt_correction_T_max 0.8311 _exptl_absorpt_process_details 'sadabs (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 '/f and /w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5763 _diffrn_reflns_av_R_equivalents 0.0492 _diffrn_reflns_av_sigmaI/netI 0.0603 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 26.00 _reflns_number_total 2087 _reflns_number_gt 1643 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART(Bruker, 1997)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT(Bruker, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL(Bruker, 2001)' _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^)+(0.0450P)^2^+0.0000P] 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 constru _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2087 _refine_ls_number_parameters 137 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0606 _refine_ls_R_factor_gt 0.0464 _refine_ls_wR_factor_ref 0.1022 _refine_ls_wR_factor_gt 0.0959 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _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 Cu1 Cu 0.27766(9) 0.47242(3) 0.33138(4) 0.02888(19) Uani 1 1 d . . . N1 N 0.5386(6) 0.41268(19) 0.2976(3) 0.0330(8) Uani 1 1 d . . . N2 N -0.0261(6) 0.46400(18) 0.6307(3) 0.0293(8) Uani 1 1 d . . . N3 N 0.1262(7) 0.5841(2) 0.1426(3) 0.0316(8) Uani 1 1 d . . . C1 C 0.2003(8) 0.6567(2) 0.1597(4) 0.0351(10) Uani 1 1 d . . . H1 H 0.3586 0.6678 0.2037 0.042 Uiso 1 1 calc R . . C2 C 0.0435(8) 0.7134(3) 0.1125(4) 0.0389(11) Uani 1 1 d . . . H2 H 0.0968 0.7632 0.1241 0.047 Uiso 1 1 calc R . . C3 C -0.1955(8) 0.6986(2) 0.0471(4) 0.0323(10) Uani 1 1 d . . . C4 C -0.3640(9) 0.7596(3) -0.0129(4) 0.0515(13) Uani 1 1 d . . . H4A H -0.5047 0.7376 -0.0679 0.077 Uiso 1 1 calc R . . H4B H -0.2812 0.7919 -0.0593 0.077 Uiso 1 1 calc R . . H4C H -0.4150 0.7886 0.0497 0.077 Uiso 1 1 calc R . . C5 C -0.2661(8) 0.6240(2) 0.0368(4) 0.0343(10) Uani 1 1 d . . . H5 H -0.4259 0.6117 -0.0035 0.041 Uiso 1 1 calc R . . C6 C -0.1051(8) 0.5674(2) 0.0849(4) 0.0335(10) Uani 1 1 d . . . H6 H -0.1565 0.5173 0.0776 0.040 Uiso 1 1 calc R . . C7 C 0.1273(7) 0.4406(2) 0.5886(3) 0.0250(9) Uani 1 1 d . . . C8 C 0.7000(7) 0.3913(2) 0.2585(3) 0.0261(9) Uani 1 1 d . . . O1 O 0.2897(5) 0.52918(16) 0.1802(2) 0.0354(7) Uani 1 1 d . . . S1 S 0.34673(19) 0.40772(6) 0.52782(9) 0.0289(3) Uani 1 1 d . . . S2 S 0.9271(2) 0.36167(7) 0.20373(10) 0.0401(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 Cu1 0.0261(3) 0.0331(3) 0.0309(3) 0.0030(2) 0.0137(2) 0.0080(2) N1 0.032(2) 0.032(2) 0.0380(19) 0.0021(17) 0.0148(17) 0.0054(17) N2 0.027(2) 0.033(2) 0.0307(18) 0.0066(16) 0.0138(16) 0.0050(16) N3 0.038(2) 0.037(2) 0.0232(16) 0.0059(16) 0.0138(15) 0.0059(18) C1 0.032(3) 0.038(3) 0.035(2) 0.000(2) 0.0088(19) -0.001(2) C2 0.045(3) 0.027(2) 0.047(3) -0.002(2) 0.015(2) -0.006(2) C3 0.032(3) 0.037(3) 0.028(2) -0.0005(19) 0.0073(18) 0.006(2) C4 0.055(3) 0.041(3) 0.057(3) 0.005(2) 0.010(3) 0.009(2) C5 0.031(3) 0.044(3) 0.028(2) -0.003(2) 0.0081(18) 0.000(2) C6 0.037(3) 0.029(2) 0.035(2) -0.0004(19) 0.010(2) 0.000(2) C7 0.026(2) 0.025(2) 0.0236(19) 0.0025(17) 0.0044(17) -0.0021(18) C8 0.024(2) 0.029(2) 0.0237(19) -0.0016(17) 0.0040(17) -0.0022(18) O1 0.0381(18) 0.0394(18) 0.0336(15) 0.0111(14) 0.0183(13) 0.0157(14) S1 0.0255(6) 0.0308(6) 0.0326(5) 0.0005(5) 0.0115(4) 0.0068(4) S2 0.0280(7) 0.0514(7) 0.0454(6) -0.0135(6) 0.0175(5) 0.0031(5) _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 Cu1 N1 1.915(4) . ? Cu1 N2 1.930(3) 3_566 ? Cu1 O1 1.967(3) . ? Cu1 S1 2.4077(16) . ? N1 C8 1.157(5) . ? N2 C7 1.150(5) . ? N2 Cu1 1.930(3) 3_566 ? N3 O1 1.335(4) . ? N3 C6 1.340(5) . ? N3 C1 1.349(5) . ? C1 C2 1.356(6) . ? C1 H1 0.9300 . ? C2 C3 1.393(6) . ? C2 H2 0.9300 . ? C3 C5 1.376(6) . ? C3 C4 1.485(6) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 C6 1.371(6) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 S1 1.645(4) . ? C8 S2 1.625(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 N1 Cu1 N2 177.31(14) . 3_566 ? N1 Cu1 O1 86.22(13) . . ? N2 Cu1 O1 93.54(13) 3_566 . ? N1 Cu1 S1 86.91(11) . . ? N2 Cu1 S1 92.91(10) 3_566 . ? O1 Cu1 S1 168.89(9) . . ? C8 N1 Cu1 163.3(3) . . ? C7 N2 Cu1 163.0(3) . 3_566 ? O1 N3 C6 120.6(4) . . ? O1 N3 C1 118.8(4) . . ? C6 N3 C1 120.6(4) . . ? N3 C1 C2 119.9(4) . . ? N3 C1 H1 120.0 . . ? C2 C1 H1 120.0 . . ? C1 C2 C3 121.5(4) . . ? C1 C2 H2 119.3 . . ? C3 C2 H2 119.3 . . ? C5 C3 C2 116.5(4) . . ? C5 C3 C4 121.2(4) . . ? C2 C3 C4 122.2(4) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C6 C5 C3 121.1(4) . . ? C6 C5 H5 119.4 . . ? C3 C5 H5 119.4 . . ? N3 C6 C5 120.2(4) . . ? N3 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? N2 C7 S1 179.6(4) . . ? N1 C8 S2 179.7(4) . . ? N3 O1 Cu1 118.6(2) . . ? C7 S1 Cu1 102.98(13) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Cu1 N1 C8 -69(3) 3_566 . . . ? O1 Cu1 N1 C8 16.1(11) . . . . ? S1 Cu1 N1 C8 -155.2(11) . . . . ? O1 N3 C1 C2 174.2(4) . . . . ? C6 N3 C1 C2 -3.5(6) . . . . ? N3 C1 C2 C3 0.6(7) . . . . ? C1 C2 C3 C5 2.2(6) . . . . ? C1 C2 C3 C4 -175.5(4) . . . . ? C2 C3 C5 C6 -2.3(6) . . . . ? C4 C3 C5 C6 175.5(4) . . . . ? O1 N3 C6 C5 -174.2(3) . . . . ? C1 N3 C6 C5 3.4(6) . . . . ? C3 C5 C6 N3 -0.4(6) . . . . ? Cu1 N2 C7 S1 -1(82) 3_566 . . . ? Cu1 N1 C8 S2 43(100) . . . . ? C6 N3 O1 Cu1 -76.7(4) . . . . ? C1 N3 O1 Cu1 105.6(4) . . . . ? N1 Cu1 O1 N3 176.8(3) . . . . ? N2 Cu1 O1 N3 -5.9(3) 3_566 . . . ? S1 Cu1 O1 N3 -131.3(4) . . . . ? N2 C7 S1 Cu1 -23(81) . . . . ? N1 Cu1 S1 C7 -175.72(17) . . . . ? N2 Cu1 S1 C7 6.98(17) 3_566 . . . ? O1 Cu1 S1 C7 132.4(5) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.434 _refine_diff_density_min -0.415 _refine_diff_density_rms 0.099