# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Qin-Yu Zhu' _publ_contact_author_email zhuqinyu@suda.edu.cn loop_ _publ_author_name 'Zheng Shi' 'Qiong-Hua Han' 'Xin-Yu Li' 'Ming-Yan Shao' 'Qin-Yu Zhu' 'Jie Dai' data_3 _database_code_depnum_ccdc_archive 'CCDC 814567' #TrackingRef '- 3-4-R.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H48 N8 O20 S6' _chemical_formula_weight 889.00 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall '-P 1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.991(8) _cell_length_b 9.925(14) _cell_length_c 15.346(19) _cell_angle_alpha 105.01(4) _cell_angle_beta 90.24(3) _cell_angle_gamma 107.12(3) _cell_volume 979(2) _cell_formula_units_Z 1 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 4112 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description Block _exptl_crystal_colour Red _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.508 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 468 _exptl_absorpt_coefficient_mu 0.433 _exptl_absorpt_correction_type ?multi-scan _exptl_absorpt_correction_T_min 0.7813 _exptl_absorpt_correction_T_max 0.9379 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7030 _diffrn_reflns_av_R_equivalents 0.1261 _diffrn_reflns_av_sigmaI/netI 0.2344 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3309 _reflns_number_gt 1042 _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^)+(0.0010P)^2^+1.5000P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3309 _refine_ls_number_parameters 238 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2747 _refine_ls_R_factor_gt 0.1337 _refine_ls_wR_factor_ref 0.2342 _refine_ls_wR_factor_gt 0.1866 _refine_ls_goodness_of_fit_ref 1.195 _refine_ls_restrained_S_all 1.195 _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 N1 N 0.3622(14) -0.1279(12) 0.2916(7) 0.085(3) Uani 1 1 d . . . H1 H 0.4447 -0.1789 0.2904 0.102 Uiso 1 1 calc R . . N2 N 0.2318(13) -0.0492(10) 0.1238(5) 0.077(3) Uani 1 1 d . . . H2A H 0.1254 -0.0158 0.1230 0.116 Uiso 1 1 calc R . . H2B H 0.2849 -0.0555 0.0701 0.116 Uiso 1 1 calc R . . H2C H 0.3249 0.0129 0.1681 0.116 Uiso 1 1 calc R . . N3 N 0.6887(12) 0.3541(10) 0.3513(7) 0.072(3) Uani 1 1 d . . . H3 H 0.7103 0.2918 0.3039 0.086 Uiso 1 1 calc R . . N4 N 0.2679(14) 0.3543(10) 0.3313(7) 0.095(3) Uani 1 1 d . . . H4A H 0.2860 0.2706 0.3366 0.143 Uiso 1 1 calc R . . H4B H 0.1489 0.3338 0.3000 0.143 Uiso 1 1 calc R . . H4C H 0.2694 0.4139 0.3867 0.143 Uiso 1 1 calc R . . C1 C 0.6281(16) 0.0556(13) 0.3984(8) 0.069(3) Uani 1 1 d . . . C2 C 0.7448(14) 0.1889(14) 0.4365(7) 0.065(3) Uani 1 1 d . . . C3 C 0.9335(14) 0.0268(12) 0.4826(6) 0.060(3) Uani 1 1 d . . . C4 C 0.4181(19) 0.0096(16) 0.3423(9) 0.085(4) Uani 1 1 d . . . C5 C 0.7040(17) 0.3356(14) 0.4350(9) 0.078(4) Uani 1 1 d . . . C6 C 0.1634(16) -0.2000(15) 0.2361(8) 0.092(4) Uani 1 1 d . . . H6A H 0.0652 -0.1541 0.2653 0.111 Uiso 1 1 calc R . . H6B H 0.1170 -0.3034 0.2359 0.111 Uiso 1 1 calc R . . C7 C 0.1686(17) -0.1910(11) 0.1396(8) 0.078(4) Uani 1 1 d . . . H7A H 0.2577 -0.2454 0.1098 0.093 Uiso 1 1 calc R . . H7B H 0.0334 -0.2424 0.1093 0.093 Uiso 1 1 calc R . . C8 C 0.6339(16) 0.4840(14) 0.3428(9) 0.087(4) Uani 1 1 d . . . H8A H 0.7409 0.5459 0.3165 0.104 Uiso 1 1 calc R . . H8B H 0.6160 0.5422 0.4026 0.104 Uiso 1 1 calc R . . C9 C 0.4365(18) 0.4298(15) 0.2811(8) 0.084(4) Uani 1 1 d . . . H9A H 0.4073 0.5128 0.2668 0.101 Uiso 1 1 calc R . . H9B H 0.4485 0.3609 0.2243 0.101 Uiso 1 1 calc R . . O1 O 0.3196(11) 0.0934(9) 0.3516(5) 0.084(3) Uani 1 1 d . . . O2 O 0.7149(13) 0.4282(10) 0.5102(5) 0.099(3) Uani 1 1 d . . . O3 O 0.7770(19) 0.1491(15) 0.0635(7) 0.179(6) Uani 1 1 d . . . O4 O 0.7812(18) -0.0603(11) 0.1093(7) 0.151(4) Uani 1 1 d . . . O5 O 0.6303(11) 0.1201(9) 0.1988(5) 0.099(3) Uani 1 1 d . . . O6 O 0.9958(12) 0.1832(13) 0.1921(6) 0.142(4) Uani 1 1 d . . . O7 O 0.6252(13) -0.2800(10) 0.1869(6) 0.115(3) Uani 1 1 d . . . O8 O 0.7219(17) 0.4957(12) 0.0634(8) 0.164(5) Uani 1 1 d . . . O9 O 0.5825(14) -0.2390(13) -0.0475(8) 0.157(5) Uani 1 1 d . . . O10 O 1.124(3) 0.4472(15) 0.1043(12) 0.313(11) Uani 1 1 d . . . S1 S 0.7067(5) -0.0912(4) 0.4171(2) 0.0833(11) Uani 1 1 d . . . S2 S 0.9583(5) 0.2169(4) 0.5076(2) 0.0844(11) Uani 1 1 d . . . S3 S 0.7961(5) 0.1001(4) 0.1402(2) 0.0856(12) 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 N1 0.058(6) 0.096(9) 0.116(9) 0.038(7) -0.014(6) 0.040(6) N2 0.068(6) 0.099(8) 0.063(6) -0.001(5) -0.024(5) 0.044(6) N3 0.070(6) 0.082(7) 0.076(7) 0.016(6) 0.004(5) 0.048(6) N4 0.084(8) 0.087(8) 0.108(8) -0.012(6) -0.027(6) 0.049(6) C1 0.049(7) 0.079(8) 0.103(9) 0.042(8) 0.011(6) 0.043(7) C2 0.039(6) 0.092(9) 0.058(7) 0.004(6) -0.020(5) 0.025(6) C3 0.055(7) 0.074(8) 0.047(6) 0.004(6) -0.003(5) 0.024(6) C4 0.058(9) 0.091(11) 0.096(10) 0.018(9) 0.003(7) 0.015(8) C5 0.075(9) 0.083(9) 0.079(9) -0.002(8) -0.013(6) 0.051(7) C6 0.063(8) 0.137(12) 0.077(8) 0.010(8) -0.020(6) 0.048(8) C7 0.070(8) 0.032(6) 0.092(9) 0.006(6) 0.021(6) -0.033(5) C8 0.060(8) 0.087(9) 0.115(10) 0.010(8) -0.022(7) 0.042(7) C9 0.080(9) 0.121(11) 0.080(8) 0.055(8) 0.012(7) 0.049(8) O1 0.053(5) 0.113(7) 0.109(6) 0.030(5) 0.000(4) 0.061(5) O2 0.116(7) 0.121(7) 0.078(6) -0.011(5) -0.015(5) 0.094(6) O3 0.223(13) 0.295(16) 0.137(9) 0.149(11) 0.119(9) 0.175(12) O4 0.198(11) 0.099(7) 0.157(10) -0.017(7) 0.052(8) 0.090(7) O5 0.069(5) 0.142(8) 0.078(6) -0.015(5) -0.011(4) 0.057(5) O6 0.056(5) 0.203(11) 0.122(8) -0.026(7) -0.022(5) 0.036(6) O7 0.099(7) 0.132(8) 0.119(7) -0.005(6) 0.006(5) 0.074(6) O8 0.141(10) 0.142(10) 0.193(11) -0.025(8) -0.003(8) 0.083(8) O9 0.108(8) 0.185(12) 0.173(10) 0.064(9) -0.011(7) 0.025(8) O10 0.44(3) 0.106(10) 0.31(2) 0.042(11) -0.208(18) -0.019(13) S1 0.070(2) 0.093(3) 0.085(2) 0.0036(18) -0.0267(16) 0.0395(19) S2 0.070(2) 0.097(3) 0.088(2) 0.0057(19) -0.0242(16) 0.046(2) S3 0.062(2) 0.123(3) 0.073(2) 0.004(2) -0.0020(16) 0.049(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 N1 C4 1.324(14) . ? N1 C6 1.502(13) . ? N1 H1 0.8700 . ? N2 C7 1.431(12) . ? N2 H2A 0.9000 . ? N2 H2B 0.9000 . ? N2 H2C 0.9000 . ? N3 C5 1.351(13) . ? N3 C8 1.485(14) . ? N3 H3 0.8700 . ? N4 C9 1.526(13) . ? N4 H4A 0.9000 . ? N4 H4B 0.9000 . ? N4 H4C 0.9000 . ? C1 C2 1.311(14) . ? C1 C4 1.580(16) . ? C1 S1 1.787(11) . ? C2 C5 1.569(16) . ? C2 S2 1.755(9) . ? C3 C3 1.365(19) 2_756 ? C3 S2 1.781(11) . ? C3 S1 1.783(10) . ? C4 O1 1.210(14) . ? C5 O2 1.262(12) . ? C6 C7 1.507(14) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C8 C9 1.542(14) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? O3 S3 1.404(10) . ? O4 S3 1.510(10) . ? O5 S3 1.498(8) . ? O6 S3 1.496(8) . ? 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 C4 N1 C6 123.2(11) . . ? C4 N1 H1 118.4 . . ? C6 N1 H1 118.4 . . ? C7 N2 H2A 109.5 . . ? C7 N2 H2B 109.5 . . ? H2A N2 H2B 109.5 . . ? C7 N2 H2C 109.5 . . ? H2A N2 H2C 109.5 . . ? H2B N2 H2C 109.5 . . ? C5 N3 C8 118.0(10) . . ? C5 N3 H3 121.0 . . ? C8 N3 H3 121.0 . . ? C9 N4 H4A 109.5 . . ? C9 N4 H4B 109.5 . . ? H4A N4 H4B 109.5 . . ? C9 N4 H4C 109.5 . . ? H4A N4 H4C 109.5 . . ? H4B N4 H4C 109.5 . . ? C2 C1 C4 127.2(11) . . ? C2 C1 S1 116.8(9) . . ? C4 C1 S1 115.9(9) . . ? C1 C2 C5 126.7(9) . . ? C1 C2 S2 120.0(10) . . ? C5 C2 S2 112.9(8) . . ? C3 C3 S2 123.4(10) 2_756 . ? C3 C3 S1 121.8(11) 2_756 . ? S2 C3 S1 114.5(5) . . ? O1 C4 N1 126.0(12) . . ? O1 C4 C1 120.7(12) . . ? N1 C4 C1 113.1(12) . . ? O2 C5 N3 127.8(12) . . ? O2 C5 C2 117.2(11) . . ? N3 C5 C2 114.3(10) . . ? N1 C6 C7 114.2(10) . . ? N1 C6 H6A 108.7 . . ? C7 C6 H6A 108.7 . . ? N1 C6 H6B 108.7 . . ? C7 C6 H6B 108.7 . . ? H6A C6 H6B 107.6 . . ? N2 C7 C6 118.4(9) . . ? N2 C7 H7A 107.7 . . ? C6 C7 H7A 107.7 . . ? N2 C7 H7B 107.7 . . ? C6 C7 H7B 107.7 . . ? H7A C7 H7B 107.1 . . ? N3 C8 C9 108.3(10) . . ? N3 C8 H8A 110.0 . . ? C9 C8 H8A 110.0 . . ? N3 C8 H8B 110.0 . . ? C9 C8 H8B 110.0 . . ? H8A C8 H8B 108.4 . . ? N4 C9 C8 108.2(9) . . ? N4 C9 H9A 110.1 . . ? C8 C9 H9A 110.1 . . ? N4 C9 H9B 110.1 . . ? C8 C9 H9B 110.1 . . ? H9A C9 H9B 108.4 . . ? C3 S1 C1 94.2(5) . . ? C2 S2 C3 93.8(5) . . ? O3 S3 O6 110.4(8) . . ? O3 S3 O5 109.2(6) . . ? O6 S3 O5 110.2(5) . . ? O3 S3 O4 108.6(8) . . ? O6 S3 O4 108.7(7) . . ? O5 S3 O4 109.8(6) . . ? 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 C4 C1 C2 C5 0(2) . . . . ? S1 C1 C2 C5 -176.4(9) . . . . ? C4 C1 C2 S2 172.2(9) . . . . ? S1 C1 C2 S2 -3.7(14) . . . . ? C6 N1 C4 O1 1(2) . . . . ? C6 N1 C4 C1 176.5(10) . . . . ? C2 C1 C4 O1 -22(2) . . . . ? S1 C1 C4 O1 154.2(11) . . . . ? C2 C1 C4 N1 162.3(12) . . . . ? S1 C1 C4 N1 -21.8(14) . . . . ? C8 N3 C5 O2 -14.7(17) . . . . ? C8 N3 C5 C2 175.2(9) . . . . ? C1 C2 C5 O2 127.2(13) . . . . ? S2 C2 C5 O2 -45.9(14) . . . . ? C1 C2 C5 N3 -61.5(16) . . . . ? S2 C2 C5 N3 125.3(9) . . . . ? C4 N1 C6 C7 93.2(15) . . . . ? N1 C6 C7 N2 -58.7(15) . . . . ? C5 N3 C8 C9 -120.0(12) . . . . ? N3 C8 C9 N4 68.3(13) . . . . ? C3 C3 S1 C1 -179.3(12) 2_756 . . . ? S2 C3 S1 C1 6.5(7) . . . . ? C2 C1 S1 C3 -1.9(10) . . . . ? C4 C1 S1 C3 -178.3(9) . . . . ? C1 C2 S2 C3 7.1(11) . . . . ? C5 C2 S2 C3 -179.2(9) . . . . ? C3 C3 S2 C2 178.0(12) 2_756 . . . ? S1 C3 S2 C2 -7.9(7) . . . . ? _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.960 _refine_diff_density_max 0.479 _refine_diff_density_min -0.381 _refine_diff_density_rms 0.087 ########End data_4 _database_code_depnum_ccdc_archive 'CCDC 814568' #TrackingRef '- 3-4-R.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H38 N10 Ni2 O6 S4' _chemical_formula_weight 808.30 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' 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 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc ' 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 8.3195(9) _cell_length_b 13.0986(14) _cell_length_c 15.951(2) _cell_angle_alpha 90.00 _cell_angle_beta 105.181(3) _cell_angle_gamma 90.00 _cell_volume 1677.6(3) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 4944 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description Block _exptl_crystal_colour Red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.600 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 840 _exptl_absorpt_coefficient_mu 1.426 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6743 _exptl_absorpt_correction_T_max 0.8706 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6416 _diffrn_reflns_av_R_equivalents 0.0521 _diffrn_reflns_av_sigmaI/netI 0.0750 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2868 _reflns_number_gt 2083 _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^)+(0.0002P)^2^+10.3501P] 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 2868 _refine_ls_number_parameters 222 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1035 _refine_ls_R_factor_gt 0.0720 _refine_ls_wR_factor_ref 0.1309 _refine_ls_wR_factor_gt 0.1200 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.001 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 -0.14695(10) 0.58605(6) 0.14173(6) 0.0336(3) Uani 1 1 d . . . N1 N -0.0880(6) 0.7075(4) 0.2040(4) 0.0353(14) Uani 1 1 d . . . N2 N 0.0899(7) 0.5660(5) 0.1603(5) 0.0426(16) Uani 1 1 d . . . H2A H 0.127(10) 0.505(7) 0.186(6) 0.08(3) Uiso 1 1 d . . . H2B H 0.107(8) 0.570(5) 0.110(4) 0.03(2) Uiso 1 1 d . . . N3 N -0.3802(6) 0.5941(4) 0.1240(4) 0.0347(13) Uani 1 1 d . . . N4 N -0.1908(8) 0.4472(5) 0.1059(5) 0.0470(18) Uani 1 1 d D . . H4A H -0.099(6) 0.415(6) 0.130(5) 0.08(3) Uiso 1 1 d D . . H4B H -0.216(9) 0.442(6) 0.054(5) 0.05(3) Uiso 1 1 d . . . N9 N 0.1748(9) 0.2070(5) 0.0802(5) 0.0607(19) Uani 1 1 d . . . C1 C -0.3015(7) 0.8276(4) 0.1327(4) 0.0313(15) Uani 1 1 d . . . C2 C -0.4331(7) 0.7743(4) 0.0869(4) 0.0315(15) Uani 1 1 d . . . C3 C -0.4785(8) 0.9594(4) 0.0267(5) 0.0348(16) Uani 1 1 d . . . C4 C -0.1502(8) 0.7993(5) 0.2019(5) 0.0358(17) Uani 1 1 d . . . C5 C -0.4883(8) 0.6659(5) 0.0908(4) 0.0328(16) Uani 1 1 d . . . C6 C 0.0766(8) 0.6901(5) 0.2658(5) 0.0436(19) Uani 1 1 d . . . H6A H 0.0682 0.6401 0.3102 0.052 Uiso 1 1 calc R . . H6B H 0.1219 0.7539 0.2946 0.052 Uiso 1 1 calc R . . C7 C 0.1836(8) 0.6504(5) 0.2111(5) 0.045(2) Uani 1 1 d . . . H7A H 0.2050 0.7040 0.1726 0.053 Uiso 1 1 calc R . . H7B H 0.2904 0.6260 0.2477 0.053 Uiso 1 1 calc R . . C8 C -0.4593(8) 0.4924(5) 0.1228(5) 0.047(2) Uani 1 1 d . . . H8A H -0.5330 0.4783 0.0652 0.057 Uiso 1 1 calc R . . H8B H -0.5252 0.4899 0.1655 0.057 Uiso 1 1 calc R . . C9 C -0.3206(9) 0.4154(5) 0.1450(5) 0.053(2) Uani 1 1 d . . . H9A H -0.2765 0.4109 0.2082 0.064 Uiso 1 1 calc R . . H9B H -0.3625 0.3480 0.1231 0.064 Uiso 1 1 calc R . . C10 C 0.206(2) 0.3070(13) 0.0838(11) 0.144(6) Uiso 1 1 d . . . H10 H 0.3048 0.3288 0.1233 0.172 Uiso 1 1 calc R . . C11 C 0.039(2) 0.175(2) 0.0226(12) 0.276(15) Uani 1 1 d . . . H11A H -0.0512 0.2223 0.0204 0.414 Uiso 1 1 calc R . . H11B H 0.0088 0.1078 0.0394 0.414 Uiso 1 1 calc R . . H11C H 0.0609 0.1706 -0.0342 0.414 Uiso 1 1 calc R . . C12 C 0.286(2) 0.1525(19) 0.1346(11) 0.309(18) Uani 1 1 d . . . H12A H 0.3556 0.1969 0.1778 0.464 Uiso 1 1 calc R . . H12B H 0.3541 0.1165 0.1034 0.464 Uiso 1 1 calc R . . H12C H 0.2303 0.1035 0.1631 0.464 Uiso 1 1 calc R . . O1 O -0.0852(6) 0.8719(3) 0.2532(3) 0.0507(14) Uani 1 1 d . . . O2 O -0.6432(5) 0.6523(3) 0.0604(3) 0.0429(13) Uani 1 1 d . . . O3 O 0.1189(9) 0.3722(5) 0.0409(5) 0.092(2) Uani 1 1 d . . . S1 S -0.3018(2) 0.96030(12) 0.11536(13) 0.0431(5) Uani 1 1 d . . . S2 S -0.5906(2) 0.84472(12) 0.01417(13) 0.0415(5) 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 Ni1 0.0303(4) 0.0272(4) 0.0385(5) -0.0008(4) 0.0007(4) 0.0032(4) N1 0.033(3) 0.027(3) 0.039(4) 0.000(2) -0.003(3) 0.002(2) N2 0.036(3) 0.046(4) 0.045(5) 0.008(3) 0.009(3) 0.005(3) N3 0.033(3) 0.028(3) 0.038(4) 0.002(3) 0.002(3) 0.000(2) N4 0.042(4) 0.034(3) 0.053(5) -0.009(3) -0.008(4) 0.002(3) N9 0.061(4) 0.061(4) 0.065(5) -0.017(4) 0.026(4) -0.012(4) C1 0.030(3) 0.028(3) 0.034(4) -0.004(3) 0.003(3) 0.001(3) C2 0.031(3) 0.027(3) 0.035(4) 0.002(3) 0.007(3) 0.005(3) C3 0.031(3) 0.029(3) 0.042(4) -0.004(3) 0.005(3) 0.003(3) C4 0.033(3) 0.031(3) 0.040(4) -0.002(3) 0.003(3) -0.003(3) C5 0.033(3) 0.030(3) 0.033(4) -0.005(3) 0.004(3) -0.003(3) C6 0.037(4) 0.035(4) 0.049(5) -0.002(3) -0.005(4) -0.003(3) C7 0.031(3) 0.042(4) 0.053(5) 0.015(4) -0.002(4) 0.000(3) C8 0.040(4) 0.027(3) 0.067(6) 0.004(3) -0.001(4) -0.003(3) C9 0.050(4) 0.028(3) 0.069(6) 0.000(4) -0.009(4) -0.001(4) C11 0.153(15) 0.56(4) 0.152(18) -0.15(2) 0.115(14) -0.13(2) C12 0.27(2) 0.58(4) 0.125(15) 0.16(2) 0.138(16) 0.33(3) O1 0.052(3) 0.038(3) 0.048(3) -0.011(2) -0.011(3) 0.002(2) O2 0.030(2) 0.033(2) 0.059(4) -0.003(2) 0.000(2) -0.003(2) O3 0.115(6) 0.085(5) 0.082(5) 0.020(4) 0.036(4) 0.032(4) S1 0.0414(10) 0.0247(8) 0.0510(12) -0.0011(8) -0.0095(9) -0.0001(7) S2 0.0341(9) 0.0276(8) 0.0526(13) 0.0016(8) -0.0067(8) 0.0003(7) _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 N1 1.871(5) . ? Ni1 N3 1.889(5) . ? Ni1 N4 1.913(6) . ? Ni1 N2 1.932(6) . ? N1 C4 1.306(7) . ? N1 C6 1.480(8) . ? N2 C7 1.467(9) . ? N2 H2A 0.91(9) . ? N2 H2B 0.85(7) . ? N3 C5 1.313(8) . ? N3 C8 1.484(8) . ? N4 C9 1.443(10) . ? N4 H4A 0.86(2) . ? N4 H4B 0.81(8) . ? N9 C12 1.302(15) . ? N9 C10 1.333(16) . ? N9 C11 1.323(17) . ? C1 C2 1.342(8) . ? C1 C4 1.487(8) . ? C1 S1 1.760(6) . ? C2 C5 1.499(8) . ? C2 S2 1.765(6) . ? C3 C3 1.352(12) 3_475 ? C3 S2 1.751(6) . ? C3 S1 1.753(6) . ? C4 O1 1.279(7) . ? C5 O2 1.265(7) . ? C6 C7 1.494(10) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C8 C9 1.503(9) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C10 O3 1.210(15) . ? C10 H10 0.9400 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C11 H11C 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C12 H12C 0.9700 . ? 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 Ni1 N3 98.5(2) . . ? N1 Ni1 N4 165.9(3) . . ? N3 Ni1 N4 84.3(3) . . ? N1 Ni1 N2 85.3(3) . . ? N3 Ni1 N2 175.4(3) . . ? N4 Ni1 N2 91.4(3) . . ? C4 N1 C6 116.8(5) . . ? C4 N1 Ni1 136.2(4) . . ? C6 N1 Ni1 106.9(4) . . ? C7 N2 Ni1 110.8(5) . . ? C7 N2 H2A 110(5) . . ? Ni1 N2 H2A 114(5) . . ? C7 N2 H2B 106(4) . . ? Ni1 N2 H2B 105(4) . . ? H2A N2 H2B 111(7) . . ? C5 N3 C8 112.5(5) . . ? C5 N3 Ni1 131.9(4) . . ? C8 N3 Ni1 112.7(4) . . ? C9 N4 Ni1 104.5(5) . . ? C9 N4 H4A 110(6) . . ? Ni1 N4 H4A 104(6) . . ? C9 N4 H4B 114(6) . . ? Ni1 N4 H4B 112(6) . . ? H4A N4 H4B 112(8) . . ? C12 N9 C10 114.4(15) . . ? C12 N9 C11 127.9(18) . . ? C10 N9 C11 117.6(16) . . ? C2 C1 C4 133.3(6) . . ? C2 C1 S1 117.4(5) . . ? C4 C1 S1 109.2(4) . . ? C1 C2 C5 133.2(6) . . ? C1 C2 S2 116.5(5) . . ? C5 C2 S2 109.9(4) . . ? C3 C3 S2 123.9(6) 3_475 . ? C3 C3 S1 122.0(6) 3_475 . ? S2 C3 S1 114.0(3) . . ? O1 C4 N1 124.7(6) . . ? O1 C4 C1 115.1(5) . . ? N1 C4 C1 120.1(6) . . ? O2 C5 N3 125.1(6) . . ? O2 C5 C2 114.2(5) . . ? N3 C5 C2 120.7(5) . . ? N1 C6 C7 104.7(6) . . ? N1 C6 H6A 110.8 . . ? C7 C6 H6A 110.8 . . ? N1 C6 H6B 110.8 . . ? C7 C6 H6B 110.8 . . ? H6A C6 H6B 108.9 . . ? N2 C7 C6 105.9(6) . . ? N2 C7 H7A 110.6 . . ? C6 C7 H7A 110.6 . . ? N2 C7 H7B 110.6 . . ? C6 C7 H7B 110.6 . . ? H7A C7 H7B 108.7 . . ? N3 C8 C9 106.8(5) . . ? N3 C8 H8A 110.4 . . ? C9 C8 H8A 110.4 . . ? N3 C8 H8B 110.4 . . ? C9 C8 H8B 110.4 . . ? H8A C8 H8B 108.6 . . ? N4 C9 C8 108.7(6) . . ? N4 C9 H9A 110.0 . . ? C8 C9 H9A 110.0 . . ? N4 C9 H9B 110.0 . . ? C8 C9 H9B 110.0 . . ? H9A C9 H9B 108.3 . . ? O3 C10 N9 126.1(15) . . ? O3 C10 H10 117.0 . . ? N9 C10 H10 117.0 . . ? N9 C11 H11A 109.5 . . ? N9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N9 C12 H12A 109.5 . . ? N9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C3 S1 C1 94.9(3) . . ? C3 S2 C2 95.2(3) . . ? 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 N3 Ni1 N1 C4 -37.0(8) . . . . ? N4 Ni1 N1 C4 -137.6(11) . . . . ? N2 Ni1 N1 C4 145.5(8) . . . . ? N3 Ni1 N1 C6 147.7(5) . . . . ? N4 Ni1 N1 C6 47.2(13) . . . . ? N2 Ni1 N1 C6 -29.8(5) . . . . ? N1 Ni1 N2 C7 0.8(5) . . . . ? N3 Ni1 N2 C7 -146(3) . . . . ? N4 Ni1 N2 C7 -165.5(6) . . . . ? N1 Ni1 N3 C5 53.6(7) . . . . ? N4 Ni1 N3 C5 -140.3(7) . . . . ? N2 Ni1 N3 C5 -160(4) . . . . ? N1 Ni1 N3 C8 -147.2(5) . . . . ? N4 Ni1 N3 C8 18.9(5) . . . . ? N2 Ni1 N3 C8 0(4) . . . . ? N1 Ni1 N4 C9 63.4(13) . . . . ? N3 Ni1 N4 C9 -38.9(5) . . . . ? N2 Ni1 N4 C9 139.6(5) . . . . ? C4 C1 C2 C5 5.2(14) . . . . ? S1 C1 C2 C5 -171.2(6) . . . . ? C4 C1 C2 S2 176.6(7) . . . . ? S1 C1 C2 S2 0.2(8) . . . . ? C6 N1 C4 O1 -5.3(11) . . . . ? Ni1 N1 C4 O1 179.8(6) . . . . ? C6 N1 C4 C1 170.6(6) . . . . ? Ni1 N1 C4 C1 -4.4(11) . . . . ? C2 C1 C4 O1 -154.1(8) . . . . ? S1 C1 C4 O1 22.5(8) . . . . ? C2 C1 C4 N1 29.7(12) . . . . ? S1 C1 C4 N1 -153.7(6) . . . . ? C8 N3 C5 O2 -0.1(10) . . . . ? Ni1 N3 C5 O2 159.1(5) . . . . ? C8 N3 C5 C2 179.4(6) . . . . ? Ni1 N3 C5 C2 -21.3(10) . . . . ? C1 C2 C5 O2 155.6(8) . . . . ? S2 C2 C5 O2 -16.3(8) . . . . ? C1 C2 C5 N3 -24.0(12) . . . . ? S2 C2 C5 N3 164.2(6) . . . . ? C4 N1 C6 C7 -124.1(7) . . . . ? Ni1 N1 C6 C7 52.3(6) . . . . ? Ni1 N2 C7 C6 27.9(7) . . . . ? N1 C6 C7 N2 -51.0(7) . . . . ? C5 N3 C8 C9 168.7(7) . . . . ? Ni1 N3 C8 C9 5.3(8) . . . . ? Ni1 N4 C9 C8 51.4(7) . . . . ? N3 C8 C9 N4 -36.9(8) . . . . ? C12 N9 C10 O3 -178.4(15) . . . . ? C11 N9 C10 O3 2(2) . . . . ? C3 C3 S1 C1 -166.3(8) 3_475 . . . ? S2 C3 S1 C1 13.4(4) . . . . ? C2 C1 S1 C3 -8.3(6) . . . . ? C4 C1 S1 C3 174.5(5) . . . . ? C3 C3 S2 C2 166.3(9) 3_475 . . . ? S1 C3 S2 C2 -13.3(4) . . . . ? C1 C2 S2 C3 8.0(6) . . . . ? C5 C2 S2 C3 -178.7(5) . . . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 1.204 _refine_diff_density_min -0.573 _refine_diff_density_rms 0.097 ########End