# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1752 #Nickel(II) complexes with dithiadiiminoamine and #dithiabis(thiosemicarbazone) ligands. #Vitaly V. Pavlishchuk, Sergey V. Kolotilov, Anthony W. Addison, Raymond J. #Butcher and Ekkehard Sinn data_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H27 Cl2 N4 Ni O8.50 S2' _chemical_formula_weight 557.11 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' 'Cl' 'Cl' 0.1484 0.1585 '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 Pccn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y, z-1/2' _cell_length_a 16.888(2) _cell_length_b 19.831(3) _cell_length_c 13.2864(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4449.7(10) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 37 _cell_measurement_theta_min 4.96 _cell_measurement_theta_max 12.51 _exptl_crystal_description needle _exptl_crystal_colour pale_purple _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.74 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.663 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2312 _exptl_absorpt_coefficient_mu 1.348 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4107 _exptl_absorpt_correction_T_max 0.4374 _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 ? _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_% ? _diffrn_reflns_number 5007 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0725 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5007 _reflns_number_gt 2991 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens 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^)+(0.0474P)^2^+4.0131P] 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 5007 _refine_ls_number_parameters 335 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.1116 _refine_ls_R_factor_gt 0.0546 _refine_ls_wR_factor_ref 0.1329 _refine_ls_wR_factor_gt 0.1092 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0.301 _refine_ls_shift/su_mean 0.023 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 Ni Ni 0.07264(3) 0.38334(3) 0.16815(4) 0.03310(16) Uani 1 1 d . . . Cl1 Cl 0.19452(8) 0.59502(7) 0.08197(12) 0.0603(4) Uani 1 1 d . . . Cl2 Cl 0.37728(7) 0.35729(6) 0.09202(10) 0.0496(3) Uani 1 1 d D . . S1A S -0.02288(7) 0.47690(6) 0.16860(9) 0.0470(3) Uani 1 1 d . . . S1B S -0.01114(7) 0.32634(7) 0.29028(9) 0.0487(3) Uani 1 1 d . . . O1W O 0.2500 0.7500 0.2259(9) 0.178(4) Uani 1 2 d S . . O11 O 0.1330(3) 0.5726(2) 0.0202(4) 0.117(2) Uani 1 1 d . . . O12 O 0.2374(3) 0.5384(2) 0.1168(4) 0.1099(18) Uani 1 1 d . . . O13 O 0.1583(4) 0.6316(3) 0.1611(4) 0.1218(19) Uani 1 1 d . . . O14 O 0.2459(3) 0.6392(2) 0.0313(5) 0.130(2) Uani 1 1 d . . . O21 O 0.4031(3) 0.3339(2) 0.1859(3) 0.1058(17) Uani 1 1 d D A . O22 O 0.3176(6) 0.3149(5) 0.0568(6) 0.087(5) Uani 0.57(3) 1 d PD A 1 O23 O 0.4385(4) 0.3609(9) 0.0246(6) 0.128(6) Uani 0.57(3) 1 d PD A 1 O24 O 0.3468(10) 0.4220(4) 0.1032(7) 0.113(6) Uani 0.57(3) 1 d PD A 1 O22A O 0.4392(8) 0.3845(13) 0.0387(10) 0.136(10) Uani 0.43(3) 1 d PD A 2 O23A O 0.3159(12) 0.4004(14) 0.1015(13) 0.223(16) Uani 0.43(3) 1 d PD A 2 O24A O 0.350(2) 0.2984(9) 0.0377(12) 0.168(12) Uani 0.43(3) 1 d PD A 2 N1A N 0.1667(3) 0.3174(2) 0.2021(4) 0.0430(10) Uani 1 1 d . . . H1NA H 0.146(3) 0.277(3) 0.203(4) 0.067(19) Uiso 1 1 d . . . H2NA H 0.195(3) 0.321(3) 0.163(4) 0.048(19) Uiso 1 1 d . . . N2A N 0.1264(2) 0.4416(2) 0.2744(3) 0.0423(9) Uani 1 1 d . . . N1B N 0.1282(3) 0.4159(2) 0.0359(3) 0.0438(10) Uani 1 1 d . . . H1NB H 0.105(3) 0.458(3) 0.012(4) 0.08(2) Uiso 1 1 d . . . H2NB H 0.174(3) 0.424(3) 0.046(4) 0.059(18) Uiso 1 1 d . . . N2B N 0.0105(2) 0.32448(17) 0.0699(3) 0.0359(8) Uani 1 1 d . . . C1A C 0.1965(3) 0.3363(3) 0.3022(4) 0.0521(13) Uani 1 1 d . . . H1AA H 0.2486 0.3168 0.3124 0.056(14) Uiso 1 1 calc R . . H1AB H 0.1614 0.3187 0.3537 0.037(12) Uiso 1 1 calc R . . C2A C 0.2014(3) 0.4123(3) 0.3107(4) 0.0544(14) Uani 1 1 d . . . H2AA H 0.2102 0.4252 0.3802 0.050(14) Uiso 1 1 calc R . . H2AB H 0.2452 0.4291 0.2706 0.057(15) Uiso 1 1 calc R . . C3A C 0.1012(3) 0.4976(2) 0.3081(4) 0.0490(12) Uani 1 1 d . . . C31A C 0.1409(5) 0.5405(3) 0.3866(5) 0.0800(19) Uani 1 1 d . . . H31D H 0.1880 0.5184 0.4098 0.20(5) Uiso 1 1 calc R . . H31E H 0.1054 0.5472 0.4421 0.16(4) Uiso 1 1 calc R . . H31F H 0.1545 0.5834 0.3578 0.21(5) Uiso 1 1 calc R . . C4A C 0.0256(3) 0.5260(3) 0.2650(4) 0.0583(14) Uani 1 1 d . . . H4AA H 0.0372 0.5702 0.2374 0.077(18) Uiso 1 1 calc R . . H4AB H -0.0116 0.5324 0.3199 0.062(16) Uiso 1 1 calc R . . C5A C -0.1038(3) 0.4388(3) 0.2374(4) 0.0604(15) Uani 1 1 d . . . H5AA H -0.1370 0.4745 0.2643 0.064(16) Uiso 1 1 calc R . . H5AB H -0.1358 0.4129 0.1907 0.043(13) Uiso 1 1 calc R . . C1B C 0.1178(3) 0.3620(2) -0.0383(3) 0.0469(12) Uani 1 1 d . . . H1BA H 0.1542 0.3254 -0.0237 0.028(11) Uiso 1 1 calc R . . H1BB H 0.1298 0.3790 -0.1050 0.042(12) Uiso 1 1 calc R . . C2B C 0.0336(3) 0.3361(3) -0.0355(3) 0.0453(12) Uani 1 1 d . . . H2BA H -0.0016 0.3688 -0.0661 0.054(14) Uiso 1 1 calc R . . H2BB H 0.0298 0.2943 -0.0732 0.09(2) Uiso 1 1 calc R . . C3B C -0.0467(3) 0.2860(2) 0.0926(4) 0.0417(11) Uani 1 1 d . . . C31B C -0.0964(3) 0.2455(3) 0.0215(5) 0.0621(15) Uani 1 1 d . . . H31A H -0.0802 0.2545 -0.0464 0.17(4) Uiso 1 1 calc R . . H31B H -0.1511 0.2576 0.0296 0.14(3) Uiso 1 1 calc R . . H31C H -0.0898 0.1984 0.0358 0.13(3) Uiso 1 1 calc R . . C4B C -0.0671(3) 0.2760(3) 0.2020(4) 0.0576(14) Uani 1 1 d . . . H4BA H -0.0592 0.2288 0.2186 0.11(2) Uiso 1 1 calc R . . H4BB H -0.1229 0.2858 0.2112 0.073(17) Uiso 1 1 calc R . . C5B C -0.0791(3) 0.3928(3) 0.3236(4) 0.0625(15) Uani 1 1 d . . . H5BA H -0.1263 0.3726 0.3522 0.064(17) Uiso 1 1 calc R . . H5BB H -0.0548 0.4203 0.3756 0.08(2) 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 Ni 0.0319(3) 0.0355(3) 0.0319(3) -0.0026(3) 0.0005(2) 0.0023(2) Cl1 0.0463(7) 0.0528(8) 0.0818(10) 0.0063(7) -0.0036(7) -0.0011(6) Cl2 0.0463(7) 0.0477(7) 0.0550(7) -0.0041(6) 0.0022(6) -0.0001(6) S1A 0.0457(7) 0.0473(7) 0.0479(7) 0.0009(6) -0.0011(6) 0.0128(5) S1B 0.0473(7) 0.0578(8) 0.0411(6) 0.0083(6) 0.0064(6) 0.0004(6) O1W 0.099(6) 0.186(9) 0.250(11) 0.000 0.000 -0.014(7) O11 0.104(4) 0.086(3) 0.162(5) -0.029(3) -0.078(4) 0.023(3) O12 0.073(3) 0.076(3) 0.180(5) 0.038(3) -0.046(3) 0.006(2) O13 0.155(5) 0.122(4) 0.088(3) -0.023(3) 0.029(4) 0.000(4) O14 0.097(3) 0.077(3) 0.217(6) 0.047(4) 0.067(4) 0.010(3) O21 0.136(4) 0.108(4) 0.073(3) 0.014(3) -0.036(3) -0.038(3) O22 0.068(6) 0.129(12) 0.063(5) -0.011(5) -0.012(4) -0.057(6) O23 0.053(7) 0.222(15) 0.109(10) -0.040(9) 0.029(6) 0.002(9) O24 0.157(12) 0.047(5) 0.135(10) -0.020(6) 0.004(9) 0.038(6) O22A 0.118(16) 0.22(2) 0.071(10) 0.017(11) 0.021(9) -0.115(15) O23A 0.134(14) 0.161(18) 0.38(4) 0.16(2) 0.180(19) 0.110(14) O24A 0.36(3) 0.043(8) 0.101(12) 0.000(8) -0.065(17) -0.037(15) N1A 0.041(2) 0.041(3) 0.046(3) -0.006(2) -0.003(2) 0.006(2) N2A 0.043(2) 0.044(2) 0.040(2) -0.0063(18) -0.0046(18) 0.0028(18) N1B 0.041(2) 0.047(3) 0.044(2) -0.004(2) 0.006(2) -0.004(2) N2B 0.0324(18) 0.037(2) 0.038(2) -0.0002(16) -0.0020(16) 0.0026(16) C1A 0.047(3) 0.056(3) 0.054(3) -0.003(3) -0.010(2) 0.013(3) C2A 0.049(3) 0.058(3) 0.056(3) -0.013(3) -0.014(3) 0.003(3) C3A 0.063(3) 0.044(3) 0.040(3) -0.009(2) -0.002(2) 0.004(2) C31A 0.108(5) 0.064(4) 0.068(4) -0.028(3) -0.022(4) 0.004(4) C4A 0.069(4) 0.046(3) 0.060(3) -0.008(3) 0.001(3) 0.007(3) C5A 0.042(3) 0.072(4) 0.067(4) -0.002(3) 0.009(3) 0.013(3) C1B 0.047(3) 0.058(3) 0.036(3) 0.000(2) 0.004(2) 0.006(2) C2B 0.045(3) 0.055(3) 0.037(2) -0.006(2) -0.003(2) -0.002(2) C3B 0.033(2) 0.036(2) 0.056(3) -0.004(2) -0.005(2) 0.003(2) C31B 0.050(3) 0.057(4) 0.080(4) -0.018(3) -0.011(3) -0.011(3) C4B 0.049(3) 0.065(4) 0.058(3) 0.003(3) 0.012(3) -0.017(3) C5B 0.053(3) 0.078(4) 0.056(3) -0.001(3) 0.020(3) 0.011(3) _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 Ni N2A 2.037(4) . ? Ni N2B 2.042(3) . ? Ni N1B 2.094(4) . ? Ni N1A 2.106(4) . ? Ni S1B 2.4317(13) . ? Ni S1A 2.4586(13) . ? Cl1 O11 1.397(4) . ? Cl1 O14 1.405(5) . ? Cl1 O12 1.414(4) . ? Cl1 O13 1.416(5) . ? Cl2 O23A 1.350(11) . ? Cl2 O23 1.370(5) . ? Cl2 O22A 1.374(10) . ? Cl2 O24 1.391(5) . ? Cl2 O22 1.393(5) . ? Cl2 O21 1.400(4) . ? Cl2 O24A 1.446(10) . ? S1A C4A 1.806(5) . ? S1A C5A 1.810(5) . ? S1B C5B 1.803(5) . ? S1B C4B 1.807(5) . ? N1A C1A 1.470(6) . ? N2A C3A 1.270(6) . ? N2A C2A 1.473(6) . ? N1B C1B 1.464(6) . ? N2B C3B 1.267(5) . ? N2B C2B 1.472(5) . ? C1A C2A 1.515(7) . ? C3A C31A 1.504(7) . ? C3A C4A 1.510(7) . ? C5A C5B 1.522(7) . ? C1B C2B 1.513(6) . ? C3B C31B 1.498(6) . ? C3B C4B 1.507(7) . ? 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 N2A Ni N2B 175.03(15) . . ? N2A Ni N1B 101.94(16) . . ? N2B Ni N1B 82.52(16) . . ? N2A Ni N1A 82.37(16) . . ? N2B Ni N1A 99.78(16) . . ? N1B Ni N1A 91.9(2) . . ? N2A Ni S1B 93.49(11) . . ? N2B Ni S1B 82.05(11) . . ? N1B Ni S1B 164.57(13) . . ? N1A Ni S1B 90.42(16) . . ? N2A Ni S1A 82.13(11) . . ? N2B Ni S1A 95.49(10) . . ? N1B Ni S1A 93.65(14) . . ? N1A Ni S1A 164.31(13) . . ? S1B Ni S1A 88.13(5) . . ? O11 Cl1 O14 112.2(4) . . ? O11 Cl1 O12 108.7(3) . . ? O14 Cl1 O12 109.6(3) . . ? O11 Cl1 O13 106.2(4) . . ? O14 Cl1 O13 107.6(3) . . ? O12 Cl1 O13 112.6(4) . . ? O23A Cl2 O23 127.4(9) . . ? O23A Cl2 O22A 112.6(6) . . ? O23 Cl2 O22A 21.2(13) . . ? O23A Cl2 O24 28.5(11) . . ? O23 Cl2 O24 107.5(8) . . ? O22A Cl2 O24 88.6(10) . . ? O23A Cl2 O22 81.8(13) . . ? O23 Cl2 O22 111.0(4) . . ? O22A Cl2 O22 127.9(10) . . ? O24 Cl2 O22 109.0(4) . . ? O23A Cl2 O21 111.4(7) . . ? O23 Cl2 O21 111.4(4) . . ? O22A Cl2 O21 110.6(6) . . ? O24 Cl2 O21 109.0(3) . . ? O22 Cl2 O21 108.9(3) . . ? O23A Cl2 O24A 108.5(6) . . ? O23 Cl2 O24A 87.2(15) . . ? O22A Cl2 O24A 107.3(7) . . ? O24 Cl2 O24A 133.1(11) . . ? O22 Cl2 O24A 28.2(14) . . ? O21 Cl2 O24A 105.9(5) . . ? C4A S1A C5A 102.1(3) . . ? C4A S1A Ni 96.42(17) . . ? C5A S1A Ni 100.48(18) . . ? C5B S1B C4B 103.4(3) . . ? C5B S1B Ni 101.19(18) . . ? C4B S1B Ni 97.37(16) . . ? C1A N1A Ni 107.1(3) . . ? C3A N2A C2A 121.1(4) . . ? C3A N2A Ni 126.2(3) . . ? C2A N2A Ni 112.7(3) . . ? C1B N1B Ni 106.6(3) . . ? C3B N2B C2B 121.5(4) . . ? C3B N2B Ni 125.7(3) . . ? C2B N2B Ni 112.5(3) . . ? N1A C1A C2A 109.8(4) . . ? N2A C2A C1A 108.7(4) . . ? N2A C3A C31A 126.2(5) . . ? N2A C3A C4A 118.5(4) . . ? C31A C3A C4A 115.3(5) . . ? C3A C4A S1A 116.8(3) . . ? C5B C5A S1A 115.0(4) . . ? N1B C1B C2B 110.1(4) . . ? N2B C2B C1B 109.0(4) . . ? N2B C3B C31B 126.9(5) . . ? N2B C3B C4B 118.9(4) . . ? C31B C3B C4B 114.2(4) . . ? C3B C4B S1B 115.7(3) . . ? C5A C5B S1B 115.3(4) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.488 _refine_diff_density_min -0.375 _refine_diff_density_rms 0.080 #===END data_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H20 Cl2 N6 Ni O9 S4' _chemical_formula_weight 626.17 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' 'Cl' 'Cl' 0.1484 0.1585 '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 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 7.6487(16) _cell_length_b 14.789(3) _cell_length_c 21.618(5) _cell_angle_alpha 90.00 _cell_angle_beta 97.399(16) _cell_angle_gamma 90.00 _cell_volume 2425.1(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 40 _cell_measurement_theta_min 2.94 _cell_measurement_theta_max 12.53 _exptl_crystal_description long_needle _exptl_crystal_colour pale_purple _exptl_crystal_size_max 0.02 _exptl_crystal_size_mid 0.95 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.715 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1280 _exptl_absorpt_coefficient_mu 1.417 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.8300 _exptl_absorpt_correction_T_max 0.9558 _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 ? _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_% ? _diffrn_reflns_number 4607 _diffrn_reflns_av_R_equivalents 0.0331 _diffrn_reflns_av_sigmaI/netI 0.0618 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4267 _reflns_number_gt 3038 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens 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^)+(0.0509P)^2^+4.5244P] 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 4267 _refine_ls_number_parameters 374 _refine_ls_number_restraints 38 _refine_ls_R_factor_all 0.0818 _refine_ls_R_factor_gt 0.0508 _refine_ls_wR_factor_ref 0.1281 _refine_ls_wR_factor_gt 0.1127 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.086 _refine_ls_shift/su_max 0.128 _refine_ls_shift/su_mean 0.002 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 Ni Ni 0.93093(9) 0.77559(4) 0.05236(3) 0.0324(2) Uani 1 1 d . . . Cl1 Cl 0.6687(2) 1.05974(13) 0.17702(10) 0.0713(5) Uani 1 1 d D . . Cl2 Cl 1.0488(3) 0.93349(14) 0.35999(8) 0.0765(6) Uani 1 1 d D . . S1A S 0.7774(2) 0.90527(10) 0.00454(7) 0.0417(4) Uani 1 1 d . . . S2A S 1.0985(2) 0.64201(10) 0.07663(6) 0.0442(4) Uani 1 1 d . . . S1B S 0.65291(19) 0.69459(10) 0.04000(7) 0.0423(4) Uani 1 1 d . . . S2B S 1.17722(19) 0.87027(10) 0.08581(7) 0.0419(4) Uani 1 1 d . . . O1W O 1.0385(8) 0.5495(4) -0.1566(2) 0.0812(15) Uani 1 1 d . . . O11 O 0.5671(8) 0.9894(4) 0.1483(3) 0.106(2) Uani 1 1 d D A . O12 O 0.547(2) 1.1228(14) 0.1951(13) 0.233(16) Uani 0.49 1 d PD A 1 O13 O 0.781(2) 1.0340(10) 0.2265(6) 0.121(7) Uani 0.49 1 d PD A 1 O14 O 0.755(3) 1.1010(18) 0.1317(7) 0.27(2) Uani 0.49 1 d PD A 1 O12A O 0.6257(19) 1.1421(5) 0.1513(6) 0.089(5) Uani 0.51 1 d PD A 2 O13A O 0.645(4) 1.0617(10) 0.2401(4) 0.190(11) Uani 0.51 1 d PD A 2 O14A O 0.8461(11) 1.0411(9) 0.1740(13) 0.188(12) Uani 0.51 1 d PD A 2 O21 O 1.1827(7) 0.9070(4) 0.4073(2) 0.0842(16) Uani 1 1 d D B . O22 O 0.9213(12) 0.9861(6) 0.3834(4) 0.112(4) Uani 0.69 1 d PD B 1 O23 O 1.1436(10) 1.0023(5) 0.3205(3) 0.084(2) Uani 0.69 1 d PD B 1 O24 O 0.9972(12) 0.8678(5) 0.3182(3) 0.100(3) Uani 0.69 1 d PD B 1 O22A O 0.9045(15) 0.8603(9) 0.3709(7) 0.088(5) Uiso 0.31 1 d PD B 2 O23A O 1.072(2) 0.9205(13) 0.3002(4) 0.114(8) Uiso 0.31 1 d PD B 2 O24A O 0.963(2) 1.0125(8) 0.3754(8) 0.087(8) Uiso 0.31 1 d PD B 2 N1A N 0.9711(6) 0.7463(3) -0.03764(19) 0.0328(10) Uani 1 1 d . . . N2A N 1.0586(6) 0.6668(3) -0.0470(2) 0.0372(11) Uani 1 1 d . . . N3A N 1.2093(8) 0.5422(4) -0.0111(3) 0.0506(14) Uani 1 1 d . . . N1B N 0.8657(6) 0.8009(3) 0.13961(19) 0.0344(10) Uani 1 1 d . . . N2B N 0.9837(7) 0.8511(4) 0.1789(2) 0.0458(13) Uani 1 1 d . . . N3B N 1.2307(10) 0.9354(5) 0.1990(3) 0.0691(19) Uani 1 1 d . . . C1A C 0.5496(7) 0.8727(4) 0.0044(3) 0.0486(15) Uani 1 1 d . . . H1AA H 0.5141 0.8878 0.0447 0.049(17) Uiso 1 1 calc R . . H1AB H 0.4774 0.9082 -0.0268 0.07(2) Uiso 1 1 calc R . . C2A C 0.8181(8) 0.8810(4) -0.0747(3) 0.0477(15) Uani 1 1 d . . . H2AA H 0.7057 0.8813 -0.1012 0.07(2) Uiso 1 1 calc R . . H2AB H 0.8880 0.9300 -0.0885 0.026(13) Uiso 1 1 calc R . . C3A C 0.9096(7) 0.7937(4) -0.0852(2) 0.0374(13) Uani 1 1 d . . . C4A C 0.9239(11) 0.7701(5) -0.1516(3) 0.0573(18) Uani 1 1 d . . . H4AA H 1.0409 0.7488 -0.1550 0.20(6) Uiso 1 1 calc R . . H4AB H 0.8999 0.8227 -0.1773 0.09(3) Uiso 1 1 calc R . . H4AC H 0.8402 0.7236 -0.1653 0.17(5) Uiso 1 1 calc R . . C5A C 1.1235(7) 0.6151(4) 0.0019(3) 0.0383(13) Uani 1 1 d . . . C1B C 0.5120(8) 0.7734(4) -0.0084(3) 0.0517(15) Uani 1 1 d . . . H1BA H 0.5238 0.7613 -0.0518 0.07(2) Uiso 1 1 calc R . . H1BB H 0.3904 0.7614 -0.0027 0.060(19) Uiso 1 1 calc R . . C2B C 0.5976(8) 0.7166(4) 0.1176(3) 0.0489(15) Uani 1 1 d . . . H2BA H 0.4838 0.7464 0.1135 0.09(3) Uiso 1 1 calc R . . H2BB H 0.5842 0.6589 0.1378 0.042(15) Uiso 1 1 calc R . . C3B C 0.7244(7) 0.7724(4) 0.1597(2) 0.0355(12) Uani 1 1 d . . . C4B C 0.6767(9) 0.7888(5) 0.2234(3) 0.0583(18) Uani 1 1 d . . . H4BA H 0.6727 0.8527 0.2309 0.11(3) Uiso 1 1 calc R . . H4BB H 0.7635 0.7614 0.2538 0.10(3) Uiso 1 1 calc R . . H4BC H 0.5633 0.7627 0.2267 0.12(3) Uiso 1 1 calc R . . C5B C 1.1280(7) 0.8868(4) 0.1587(3) 0.0409(13) Uani 1 1 d . . . H1NA H 1.250(7) 0.510(4) 0.018(2) 0.024(15) Uiso 1 1 d . . . H1B H 0.968(7) 0.860(4) 0.212(2) 0.027(15) Uiso 1 1 d . . . H1NB H 1.216(9) 0.947(4) 0.235(3) 0.06(2) Uiso 1 1 d . . . H1A H 1.071(7) 0.650(4) -0.083(3) 0.038(16) Uiso 1 1 d . . . H2NB H 1.320(9) 0.953(5) 0.191(3) 0.05(2) Uiso 1 1 d . . . H2NA H 1.225(8) 0.534(4) -0.048(3) 0.05(2) Uiso 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 Ni 0.0355(4) 0.0339(4) 0.0294(3) -0.0025(3) 0.0102(3) -0.0006(3) Cl1 0.0613(11) 0.0619(11) 0.0849(13) 0.0138(10) -0.0122(10) -0.0130(10) Cl2 0.0779(13) 0.0986(15) 0.0474(10) -0.0292(10) -0.0129(9) 0.0304(11) S1A 0.0471(8) 0.0365(8) 0.0434(8) 0.0013(6) 0.0137(7) 0.0041(7) S2A 0.0552(9) 0.0423(8) 0.0350(7) -0.0017(6) 0.0055(6) 0.0076(7) S1B 0.0434(8) 0.0433(8) 0.0414(8) -0.0041(6) 0.0093(6) -0.0070(7) S2B 0.0381(8) 0.0484(8) 0.0423(8) -0.0074(7) 0.0166(6) -0.0077(7) O1W 0.102(4) 0.076(4) 0.070(3) -0.013(3) 0.027(3) -0.001(3) O11 0.105(5) 0.093(4) 0.117(5) -0.016(4) 0.002(4) -0.040(4) O12 0.17(2) 0.20(3) 0.31(4) -0.14(3) -0.08(2) 0.06(2) O13 0.091(11) 0.174(16) 0.081(10) -0.031(11) -0.052(9) 0.036(12) O14 0.23(3) 0.36(5) 0.19(2) 0.13(3) -0.05(2) -0.22(3) O12A 0.116(13) 0.050(6) 0.091(10) 0.025(6) -0.028(8) 0.007(8) O13A 0.38(4) 0.132(16) 0.070(10) 0.026(10) 0.059(17) -0.04(2) O14A 0.046(8) 0.110(12) 0.41(4) 0.047(19) 0.057(15) 0.004(8) O21 0.089(4) 0.098(4) 0.060(3) 0.007(3) -0.014(3) 0.005(3) O22 0.134(9) 0.082(6) 0.142(9) 0.027(6) 0.102(8) 0.033(6) O23 0.116(7) 0.090(6) 0.048(4) 0.013(4) 0.019(4) -0.024(5) O24 0.143(8) 0.093(6) 0.059(5) -0.024(4) -0.007(5) -0.042(6) N1A 0.035(2) 0.033(2) 0.031(2) -0.0016(19) 0.0102(19) -0.0007(19) N2A 0.042(3) 0.040(3) 0.031(3) -0.005(2) 0.011(2) 0.006(2) N3A 0.063(4) 0.047(3) 0.044(3) -0.001(3) 0.012(3) 0.016(3) N1B 0.037(2) 0.038(2) 0.029(2) -0.0031(19) 0.0096(19) -0.004(2) N2B 0.053(3) 0.059(3) 0.028(3) -0.007(2) 0.013(2) -0.017(3) N3B 0.072(4) 0.095(5) 0.043(3) -0.020(3) 0.014(3) -0.042(4) C1A 0.040(3) 0.058(4) 0.049(4) 0.004(3) 0.011(3) 0.008(3) C2A 0.059(4) 0.048(4) 0.039(3) 0.010(3) 0.014(3) 0.005(3) C3A 0.044(3) 0.036(3) 0.034(3) 0.001(2) 0.012(2) -0.006(3) C4A 0.089(5) 0.057(4) 0.029(3) 0.004(3) 0.019(3) 0.002(4) C5A 0.034(3) 0.041(3) 0.039(3) -0.007(3) 0.005(2) -0.002(3) C1B 0.038(3) 0.069(4) 0.048(4) 0.003(3) 0.004(3) -0.002(3) C2B 0.050(4) 0.058(4) 0.042(3) 0.006(3) 0.017(3) -0.010(3) C3B 0.041(3) 0.034(3) 0.034(3) 0.002(2) 0.012(2) 0.000(3) C4B 0.062(4) 0.078(5) 0.040(3) 0.000(3) 0.024(3) -0.008(4) C5B 0.046(3) 0.040(3) 0.038(3) 0.000(3) 0.010(3) -0.007(3) _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 Ni N1B 2.047(4) . ? Ni N1A 2.054(4) . ? Ni S2A 2.3763(17) . ? Ni S2B 2.3835(16) . ? Ni S1A 2.4111(16) . ? Ni S1B 2.4253(16) . ? Cl1 O13 1.338(8) . ? Cl1 O12A 1.361(7) . ? Cl1 O14 1.388(10) . ? Cl1 O14A 1.394(8) . ? Cl1 O11 1.395(5) . ? Cl1 O13A 1.399(9) . ? Cl1 O12 1.410(10) . ? Cl2 O23A 1.341(9) . ? Cl2 O24 1.352(6) . ? Cl2 O22 1.393(6) . ? Cl2 O24A 1.402(9) . ? Cl2 O21 1.407(4) . ? Cl2 O23 1.565(6) . ? Cl2 O22A 1.585(9) . ? S1A C1A 1.807(6) . ? S1A C2A 1.816(6) . ? S2A C5A 1.699(5) . ? S1B C2B 1.812(6) . ? S1B C1B 1.823(6) . ? S2B C5B 1.684(5) . ? N1A C3A 1.283(7) . ? N1A N2A 1.381(6) . ? N2A C5A 1.347(7) . ? N3A C5A 1.310(7) . ? N1B C3B 1.287(6) . ? N1B N2B 1.374(6) . ? N2B C5B 1.347(7) . ? N3B C5B 1.310(8) . ? C1A C1B 1.516(8) . ? C2A C3A 1.500(8) . ? C3A C4A 1.495(7) . ? C2B C3B 1.491(8) . ? C3B C4B 1.489(7) . ? 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 N1B Ni N1A 174.35(17) . . ? N1B Ni S2A 97.87(13) . . ? N1A Ni S2A 83.79(12) . . ? N1B Ni S2B 83.68(12) . . ? N1A Ni S2B 101.68(12) . . ? S2A Ni S2B 92.22(6) . . ? N1B Ni S1A 94.97(13) . . ? N1A Ni S1A 83.43(12) . . ? S2A Ni S1A 167.15(5) . . ? S2B Ni S1A 89.15(6) . . ? N1B Ni S1B 82.97(13) . . ? N1A Ni S1B 91.56(12) . . ? S2A Ni S1B 93.09(6) . . ? S2B Ni S1B 166.19(5) . . ? S1A Ni S1B 88.50(6) . . ? O13 Cl1 O12A 132.7(8) . . ? O13 Cl1 O14 112.1(8) . . ? O12A Cl1 O14 55.3(12) . . ? O13 Cl1 O14A 56.8(9) . . ? O12A Cl1 O14A 110.1(7) . . ? O14 Cl1 O14A 60.2(10) . . ? O13 Cl1 O11 114.0(6) . . ? O12A Cl1 O11 113.2(5) . . ? O14 Cl1 O11 107.5(7) . . ? O14A Cl1 O11 108.8(7) . . ? O13 Cl1 O13A 51.5(8) . . ? O12A Cl1 O13A 109.0(7) . . ? O14 Cl1 O13A 144.2(10) . . ? O14A Cl1 O13A 107.4(7) . . ? O11 Cl1 O13A 108.3(7) . . ? O13 Cl1 O12 110.3(8) . . ? O12A Cl1 O12 52.2(11) . . ? O14 Cl1 O12 107.1(8) . . ? O14A Cl1 O12 145.8(10) . . ? O11 Cl1 O12 105.4(7) . . ? O13A Cl1 O12 62.8(10) . . ? O23A Cl2 O24 46.8(8) . . ? O23A Cl2 O22 128.0(9) . . ? O24 Cl2 O22 119.2(6) . . ? O23A Cl2 O24A 118.2(7) . . ? O24 Cl2 O24A 130.9(8) . . ? O22 Cl2 O24A 22.6(8) . . ? O23A Cl2 O21 119.2(7) . . ? O24 Cl2 O21 114.1(4) . . ? O22 Cl2 O21 111.7(5) . . ? O24A Cl2 O21 112.2(7) . . ? O23A Cl2 O23 55.9(8) . . ? O24 Cl2 O23 102.7(4) . . ? O22 Cl2 O23 103.3(5) . . ? O24A Cl2 O23 81.4(8) . . ? O21 Cl2 O23 103.4(4) . . ? O23A Cl2 O22A 103.1(7) . . ? O24 Cl2 O22A 57.3(6) . . ? O22 Cl2 O22A 78.1(7) . . ? O24A Cl2 O22A 100.2(7) . . ? O21 Cl2 O22A 99.0(5) . . ? O23 Cl2 O22A 155.0(6) . . ? C1A S1A C2A 103.2(3) . . ? C1A S1A Ni 101.8(2) . . ? C2A S1A Ni 96.6(2) . . ? C5A S2A Ni 96.2(2) . . ? C2B S1B C1B 103.0(3) . . ? C2B S1B Ni 96.6(2) . . ? C1B S1B Ni 101.1(2) . . ? C5B S2B Ni 96.1(2) . . ? C3A N1A N2A 118.8(4) . . ? C3A N1A Ni 124.1(4) . . ? N2A N1A Ni 116.9(3) . . ? C5A N2A N1A 120.3(4) . . ? C3B N1B N2B 118.7(4) . . ? C3B N1B Ni 124.5(4) . . ? N2B N1B Ni 116.7(3) . . ? C5B N2B N1B 120.8(5) . . ? C1B C1A S1A 114.7(4) . . ? C3A C2A S1A 116.9(4) . . ? N1A C3A C4A 125.3(5) . . ? N1A C3A C2A 118.6(5) . . ? C4A C3A C2A 116.1(5) . . ? N3A C5A N2A 116.3(5) . . ? N3A C5A S2A 121.1(5) . . ? N2A C5A S2A 122.6(4) . . ? C1A C1B S1B 115.5(4) . . ? C3B C2B S1B 117.0(4) . . ? N1B C3B C4B 125.1(5) . . ? N1B C3B C2B 118.9(5) . . ? C4B C3B C2B 115.9(5) . . ? N3B C5B N2B 116.5(6) . . ? N3B C5B S2B 121.0(5) . . ? N2B C5B S2B 122.5(4) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.726 _refine_diff_density_min -0.688 _refine_diff_density_rms 0.083 #===END data_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H18 N6 Ni S4' _chemical_formula_weight 409.25 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 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 8.7734(8) _cell_length_b 7.7896(9) _cell_length_c 25.061(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.209(5) _cell_angle_gamma 90.00 _cell_volume 1690.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 71 _cell_measurement_theta_min 0.12 _cell_measurement_theta_max 12.48 _exptl_crystal_description needle _exptl_crystal_colour purple _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.6 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.608 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 848 _exptl_absorpt_coefficient_mu 1.642 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.7989 _exptl_absorpt_correction_T_max 0.8992 _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 'Bruker P4' _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_% ? _diffrn_reflns_number 3894 _diffrn_reflns_av_R_equivalents 0.0393 _diffrn_reflns_av_sigmaI/netI 0.0777 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 27.50 _reflns_number_total 3646 _reflns_number_gt 2185 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.0343P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3646 _refine_ls_number_parameters 234 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0944 _refine_ls_R_factor_gt 0.0445 _refine_ls_wR_factor_ref 0.1101 _refine_ls_wR_factor_gt 0.0887 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.005 _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 Ni Ni 0.86505(6) 0.32319(7) 0.12864(2) 0.02746(16) Uani 1 1 d . A . S1A S 1.01027(13) 0.16956(15) 0.20083(5) 0.0359(3) Uani 1 1 d . A . S2A S 0.75468(15) 0.53424(18) 0.06210(6) 0.0508(4) Uani 1 1 d D . . S1B S 0.92799(13) 0.15086(16) 0.05878(5) 0.0388(3) Uani 1 1 d . . . S2B S 0.74458(14) 0.47545(16) 0.19461(5) 0.0434(3) Uani 1 1 d D . . N1A N 1.2618(5) 0.3049(6) 0.25607(17) 0.0408(10) Uani 1 1 d . A . H6N1 H 1.267(5) 0.216(6) 0.2730(17) 0.032(14) Uiso 1 1 d . . . H6N2 H 1.331(5) 0.392(6) 0.2622(18) 0.042(14) Uiso 1 1 d . . . N2A N 1.1684(4) 0.4633(5) 0.18284(14) 0.0305(8) Uani 1 1 d . A . N3A N 1.0477(4) 0.4859(4) 0.14009(13) 0.0265(8) Uani 1 1 d . . . N1B N 0.7124(5) -0.0212(6) -0.00499(16) 0.0411(10) Uani 1 1 d . . . H5N1 H 0.614(5) -0.059(6) -0.0184(18) 0.041(14) Uiso 1 1 d . . . H5N2 H 0.789(6) -0.043(6) -0.0202(18) 0.040(15) Uiso 1 1 d . . . N2B N 0.6247(4) 0.0946(5) 0.06737(14) 0.0318(9) Uani 1 1 d . . . N3B N 0.6614(4) 0.1953(4) 0.11369(14) 0.0292(8) Uani 1 1 d . A . C1A C 1.1529(5) 0.3255(5) 0.21230(16) 0.0288(9) Uani 1 1 d . . . C2A C 1.0602(5) 0.6097(6) 0.10719(18) 0.0346(10) Uani 1 1 d . A . C3A C 1.1976(6) 0.7248(8) 0.1097(2) 0.0598(17) Uani 1 1 d . . . H12A H 1.2800 0.6820 0.1362 0.09(2) Uiso 1 1 calc R A . H12B H 1.1705 0.8386 0.1195 0.16(4) Uiso 1 1 calc R . . H12C H 1.2305 0.7277 0.0750 0.08(2) Uiso 1 1 calc R . . C4A C 0.9298(6) 0.6524(7) 0.0631(2) 0.0488(14) Uani 1 1 d . A . H1A H 0.9650 0.6351 0.0287 0.11(2) Uiso 1 1 calc R . . H1B H 0.9064 0.7735 0.0658 0.074(19) Uiso 1 1 calc R . . C5A C 0.6217(9) 0.6420(10) 0.0943(3) 0.055(2) Uani 0.69 1 d PD A 1 H5AA H 0.6004 0.7531 0.0772 0.037(18) Uiso 0.69 1 calc PR A 1 H5AB H 0.5259 0.5775 0.0893 0.07(3) Uiso 0.69 1 calc PR A 1 C5B C 0.6760(12) 0.6688(11) 0.1548(4) 0.069(3) Uani 0.69 1 d PD A 1 H5BA H 0.5914 0.7183 0.1702 0.06(2) Uiso 0.69 1 calc PR A 1 H5BD H 0.7591 0.7524 0.1591 0.06(3) Uiso 0.69 1 calc PR A 1 C5AA C 0.707(3) 0.700(2) 0.1132(8) 0.064(6) Uiso 0.31 1 d PD A 2 H5AC H 0.8021 0.7491 0.1319 0.076 Uiso 0.31 1 calc PR A 2 H5AD H 0.6466 0.7915 0.0940 0.076 Uiso 0.31 1 calc PR A 2 C5BB C 0.617(2) 0.623(3) 0.1548(8) 0.051(7) Uiso 0.31 1 d PD A 2 H5BB H 0.5256 0.5635 0.1368 0.062 Uiso 0.31 1 calc PR A 2 H5BC H 0.5847 0.7124 0.1774 0.062 Uiso 0.31 1 calc PR A 2 C1B C 0.7412(5) 0.0741(5) 0.04062(17) 0.0323(10) Uani 1 1 d . A . C2B C 0.5590(5) 0.2082(6) 0.14435(19) 0.0402(12) Uani 1 1 d . . . C3B C 0.4093(7) 0.1140(9) 0.1376(3) 0.073(2) Uani 1 1 d . A . H11A H 0.4181 0.0095 0.1180 0.062(17) Uiso 1 1 calc R . . H11B H 0.3295 0.1843 0.1180 0.15(4) Uiso 1 1 calc R . . H11C H 0.3837 0.0873 0.1725 0.071(19) Uiso 1 1 calc R . . C4B C 0.5886(6) 0.3277(8) 0.1923(2) 0.0615(17) Uani 1 1 d . A . H3A H 0.6071 0.2582 0.2248 0.051(16) Uiso 1 1 calc R . . H3B H 0.4951 0.3931 0.1935 0.10(2) 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 Ni 0.0246(3) 0.0249(3) 0.0329(3) 0.0022(3) 0.0046(2) -0.0016(3) S1A 0.0321(6) 0.0308(6) 0.0428(7) 0.0106(5) -0.0006(5) -0.0060(5) S2A 0.0365(7) 0.0486(8) 0.0642(9) 0.0237(7) -0.0017(6) -0.0013(6) S1B 0.0292(6) 0.0486(7) 0.0408(7) -0.0094(6) 0.0124(5) -0.0057(6) S2B 0.0374(7) 0.0417(7) 0.0510(8) -0.0149(6) 0.0071(6) 0.0000(6) N1A 0.042(2) 0.038(3) 0.039(2) 0.010(2) -0.0069(19) -0.012(2) N2A 0.026(2) 0.033(2) 0.0309(19) 0.0025(17) -0.0011(15) -0.0066(16) N3A 0.0263(19) 0.0267(18) 0.0271(18) 0.0011(15) 0.0066(15) -0.0024(16) N1B 0.036(3) 0.052(3) 0.035(2) -0.013(2) 0.005(2) -0.003(2) N2B 0.028(2) 0.034(2) 0.033(2) -0.0040(17) 0.0059(16) -0.0056(17) N3B 0.0231(19) 0.0289(19) 0.036(2) -0.0009(16) 0.0075(15) -0.0046(16) C1A 0.028(2) 0.030(2) 0.029(2) 0.000(2) 0.0059(18) 0.001(2) C2A 0.034(3) 0.032(2) 0.038(3) 0.006(2) 0.007(2) -0.006(2) C3A 0.047(3) 0.066(4) 0.064(4) 0.025(3) -0.001(3) -0.028(3) C4A 0.043(3) 0.051(3) 0.049(3) 0.018(3) -0.001(2) -0.013(3) C5A 0.035(5) 0.042(5) 0.090(7) 0.011(4) 0.013(4) 0.008(4) C5B 0.045(6) 0.045(5) 0.113(9) -0.038(6) -0.001(6) 0.018(5) C1B 0.036(3) 0.027(2) 0.033(2) 0.007(2) 0.006(2) 0.003(2) C2B 0.036(3) 0.045(3) 0.043(3) -0.010(2) 0.014(2) -0.012(2) C3B 0.060(4) 0.090(5) 0.079(4) -0.043(4) 0.041(4) -0.037(4) C4B 0.046(3) 0.080(4) 0.063(4) -0.035(4) 0.023(3) -0.023(3) _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 Ni N3A 2.027(3) . ? Ni N3B 2.028(3) . ? Ni S1B 2.3414(13) . ? Ni S1A 2.3644(12) . ? Ni S2B 2.4117(14) . ? Ni S2A 2.4299(14) . ? S1A C1A 1.735(4) . ? S2A C5A 1.737(7) . ? S2A C4A 1.788(5) . ? S2A C5AA 1.910(16) . ? S1B C1B 1.735(5) . ? S2B C4B 1.782(5) . ? S2B C5BB 1.793(16) . ? S2B C5B 1.853(9) . ? N1A C1A 1.344(5) . ? N2A C1A 1.322(5) . ? N2A N3A 1.391(4) . ? N3A C2A 1.284(5) . ? N1B C1B 1.352(6) . ? N2B C1B 1.319(5) . ? N2B N3B 1.395(5) . ? N3B C2B 1.276(5) . ? C2A C4A 1.496(6) . ? C2A C3A 1.496(6) . ? C5A C5B 1.529(11) . ? C5AA C5BB 1.527(19) . ? C2B C3B 1.490(7) . ? C2B C4B 1.510(6) . ? 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 N3A Ni N3B 170.61(14) . . ? N3A Ni S1B 100.87(10) . . ? N3B Ni S1B 83.48(10) . . ? N3A Ni S1A 83.75(10) . . ? N3B Ni S1A 104.11(10) . . ? S1B Ni S1A 96.85(5) . . ? N3A Ni S2B 91.08(10) . . ? N3B Ni S2B 84.17(10) . . ? S1B Ni S2B 167.49(5) . . ? S1A Ni S2B 88.05(5) . . ? N3A Ni S2A 83.87(10) . . ? N3B Ni S2A 87.88(10) . . ? S1B Ni S2A 89.45(5) . . ? S1A Ni S2A 166.98(5) . . ? S2B Ni S2A 88.14(5) . . ? C1A S1A Ni 93.35(14) . . ? C5A S2A C4A 112.6(4) . . ? C5A S2A C5AA 29.2(6) . . ? C4A S2A C5AA 85.6(6) . . ? C5A S2A Ni 103.4(3) . . ? C4A S2A Ni 95.26(16) . . ? C5AA S2A Ni 95.9(7) . . ? C1B S1B Ni 93.88(16) . . ? C4B S2B C5BB 89.3(7) . . ? C4B S2B C5B 109.0(4) . . ? C5BB S2B C5B 19.8(7) . . ? C4B S2B Ni 94.53(17) . . ? C5BB S2B Ni 103.7(7) . . ? C5B S2B Ni 99.8(3) . . ? C1A N2A N3A 113.5(3) . . ? C2A N3A N2A 117.1(4) . . ? C2A N3A Ni 121.7(3) . . ? N2A N3A Ni 121.1(2) . . ? C1B N2B N3B 113.4(3) . . ? C2B N3B N2B 117.0(4) . . ? C2B N3B Ni 122.3(3) . . ? N2B N3B Ni 120.6(3) . . ? N2A C1A N1A 115.4(4) . . ? N2A C1A S1A 127.7(3) . . ? N1A C1A S1A 116.8(3) . . ? N3A C2A C4A 120.5(4) . . ? N3A C2A C3A 125.0(4) . . ? C4A C2A C3A 114.4(4) . . ? C2A C4A S2A 116.7(3) . . ? C5B C5A S2A 113.6(6) . . ? C5A C5B S2B 116.5(6) . . ? C5BB C5AA S2A 112.7(14) . . ? C5AA C5BB S2B 106.6(14) . . ? N2B C1B N1B 116.2(4) . . ? N2B C1B S1B 127.0(3) . . ? N1B C1B S1B 116.8(4) . . ? N3B C2B C3B 125.8(4) . . ? N3B C2B C4B 118.7(4) . . ? C3B C2B C4B 115.5(4) . . ? C2B C4B S2B 117.2(4) . . ? _diffrn_measured_fraction_theta_max 0.939 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.939 _refine_diff_density_max 0.484 _refine_diff_density_min -0.467 _refine_diff_density_rms 0.097 #===END data_4 #============================================================================== _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution ? _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan for Windows (MSC, 1997)' #------------------------------------------------------------------------------ _cell_length_a 22.046(9) _cell_length_b 11.339(4) _cell_length_c 21.319(9) _cell_angle_alpha 90 _cell_angle_beta 117.363(2) _cell_angle_gamma 90 _cell_volume 4733(3) _cell_formula_units_Z 8 _cell_measurement_temperature 291.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 4.8 _cell_measurement_theta_max 13.4 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c ' _symmetry_Int_Tables_number 15 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' +x, +y, +z' ' -x, +y,1/2-z' ' -x, +y,1/2-z' ' -x, -y, -z' ' -x, -y, -z' ' +x, -y,1/2+z' ' +x, -y,1/2+z' '1/2+x,1/2+y, +z' '1/2+x,1/2+y, +z' '1/2-x,1/2+y,1/2-z' '1/2-x,1/2+y,1/2-z' '1/2-x,1/2-y, -z' '1/2-x,1/2-y, -z' '1/2+x,1/2-y,1/2+z' '1/2+x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'rhombic' _exptl_crystal_colour 'purple' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.25 _exptl_crystal_density_diffrn 1.594 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 568.08 _chemical_formula_analytical ? _chemical_formula_sum 'C13 H25 Cl2 N3.50 O9 Ni S2 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 2348.00 _exptl_absorpt_coefficient_mu 1.270 _exptl_absorpt_correction_type none _exptl_special_details ; The scan width was (1.24+0.30tan\q)\% with an \w scan speed of 2\% per minute (up to 5 scans to achieve I/\s(I) > 10). Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. ; #============================================================================== # EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 291.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'Rigaku AFC6S ' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -2.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? ? ? ? ? ? ? _diffrn_reflns_number 5063 _reflns_number_total 4928 _reflns_number_gt 1584 _reflns_threshold_expression I>1.70\s(I) _diffrn_reflns_av_R_equivalents 0.11836 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 100 _diffrn_reflns_limit_h_max -100 _diffrn_reflns_limit_k_min 100 _diffrn_reflns_limit_k_max -100 _diffrn_reflns_limit_l_min 100 _diffrn_reflns_limit_l_max -100 _diffrn_reflns_theta_min 0.00 _diffrn_reflns_theta_max 27.70 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.03122 _diffrn_orient_matrix_UB_12 -0.00724 _diffrn_orient_matrix_UB_13 -0.02209 _diffrn_orient_matrix_UB_21 0.02783 _diffrn_orient_matrix_UB_22 0.06749 _diffrn_orient_matrix_UB_23 0.02934 _diffrn_orient_matrix_UB_31 0.02932 _diffrn_orient_matrix_UB_32 -0.05631 _diffrn_orient_matrix_UB_33 0.03796 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ni 0 8 0.285 1.113 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Cl 0 16 0.132 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; S 0 16 0.110 0.124 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; O 0 72 0.008 0.006 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N 0 28 0.004 0.003 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; C 0 104 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; H 0 200 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Ni(0) 0.1186(1) 0.1901(2) 0.5903(1) 0.0455(7) 1.000 . Uani d ? Cl(1) 0.3751(3) 0.5332(5) 0.6002(3) 0.080(2) 1.000 . Uani d ? Cl(2) 0.1219(3) 0.6034(5) 0.6615(3) 0.079(2) 1.000 . Uani d ? S(1) 0.0807(3) -0.0102(4) 0.5909(2) 0.060(2) 1.000 . Uani d ? S(2) 0.1511(3) 0.2130(4) 0.7128(2) 0.058(2) 1.000 . Uani d ? O(1) 0.0240(7) 0.2682(9) 0.5712(6) 0.065(5) 1.000 . Uani d ? O(11) 0.4136(7) 0.559(1) 0.5670(7) 0.097(6) 1.000 . Uani d ? O(13) 0.427(2) 0.513(3) 0.672(2) 0.10(1) 0.500 S Uiso d ? O(12) 0.308(2) 0.593(3) 0.566(2) 0.10(1) 0.500 S Uiso d ? O(14) 0.348(2) 0.411(3) 0.578(2) 0.10(1) 0.440 S Uiso d ? O(15) 0.395(2) 0.420(3) 0.634(2) 0.10(1) 0.420 S Uiso d ? O(16) 0.417(2) 0.602(3) 0.664(2) 0.10(1) 0.410 S Uiso d ? O(17) 0.341(2) 0.631(3) 0.611(2) 0.10(1) 0.370 S Uiso d ? O(18) 0.309(2) 0.489(4) 0.548(2) 0.10(1) 0.360 S Uiso d ? O(21) 0.153(1) 0.502(2) 0.701(1) 0.140(7) 0.910 S Uiso d ? O(22) 0.151(1) 0.614(2) 0.619(1) 0.139(8) 0.790 S Uiso d ? O(23) 0.165(2) 0.687(3) 0.710(1) 0.14(1) 0.620 S Uiso d ? O(24) 0.096(2) 0.695(3) 0.683(2) 0.14(1) 0.490 S Uiso d ? O(25) 0.058(2) 0.558(4) 0.604(2) 0.15(2) 0.460 S Uiso d ? O(26) 0.050(4) 0.631(6) 0.646(4) 0.15(2) 0.290 S Uiso d ? O(27) 0.083(4) 0.500(7) 0.661(4) 0.14(2) 0.240 S Uiso d ? O(28) 0.070(5) 0.649(9) 0.589(5) 0.16(3) 0.200 S Uiso d ? N(1) 0.2099(7) 0.109(1) 0.6125(7) 0.049(5) 1.000 . Uani d ? N(2) 0.1731(9) 0.341(1) 0.5952(8) 0.067(6) 1.000 . Uani d ? N(3) 0.0709(7) 0.207(1) 0.4825(6) 0.055(5) 1.000 . Uani d ? N(4) 0.5000 0.036(3) 0.7500 0.18(2) 0.500 S Uiso d ? C(1) 0.012(1) 0.289(2) 0.619(1) 0.061(7) 1.000 . Uani d ? C(2) 0.064(1) 0.261(1) 0.6930(9) 0.061(7) 1.000 . Uani d ? C(3) 0.1558(9) 0.056(1) 0.7355(8) 0.062(7) 1.000 . Uani d ? C(4) 0.093(1) -0.019(1) 0.678(1) 0.067(7) 1.000 . Uani d ? C(5) 0.160(1) -0.083(2) 0.6046(9) 0.068(7) 1.000 . Uani d ? C(6) 0.219(1) -0.002(2) 0.6148(8) 0.057(7) 1.000 . Uani d ? C(7) 0.264(1) 0.191(2) 0.619(1) 0.084(8) 1.000 . Uani d ? C(8) 0.250(1) 0.314(2) 0.6378(9) 0.075(8) 1.000 . Uani d ? C(9) 0.132(2) 0.388(3) 0.517(2) 0.05(1) 0.550 S Uiso d ? C(9) 0.165(2) 0.367(4) 0.528(2) 0.05(1) 0.450 S Uiso d ? C(10) 0.119(2) 0.284(3) 0.469(2) 0.06(1) 0.550 S Uiso d ? C(10) 0.090(2) 0.332(4) 0.473(2) 0.07(1) 0.450 S Uiso d ? C(11) -0.056(1) 0.346(2) 0.600(1) 0.092(9) 1.000 . Uani d ? C(12) 0.284(1) -0.064(2) 0.623(1) 0.085(8) 1.000 . Uani d ? C(21) 0.5000 0.248(3) 0.7500 0.10(1) 0.500 S Uiso d ? C(22) 0.5000 0.127(3) 0.7500 0.11(1) 0.500 S Uiso d ? H(2) 0.1607 0.3977 0.6218 0.081 0.550 S Uiso d ? H(21) 0.0447 0.1973 0.7071 0.072 1.000 . Uiso c ? H(2) 0.1571 0.4089 0.6126 0.081 0.450 S Uiso d ? H(22) 0.0683 0.3279 0.7197 0.072 1.000 . Uiso c ? H(31) 0.1977 0.0281 0.7387 0.075 1.000 . Uiso c ? H(3) 0.0647 0.1327 0.4589 0.064 0.550 S Uiso d ? H(32) 0.1569 0.0524 0.7803 0.075 1.000 . Uiso c ? H(3) 0.0263 0.2429 0.4652 0.064 0.550 S Uiso d ? H(3) 0.0865 0.1512 0.4597 0.064 0.450 S Uiso d ? H(3) 0.0218 0.1983 0.4625 0.064 0.450 S Uiso d ? H(41) 0.0531 0.0082 0.6798 0.085 1.000 . Uiso c ? H(42) 0.1018 -0.0983 0.6935 0.085 1.000 . Uiso c ? H(51) 0.1781 -0.1265 0.6466 0.096 1.000 . Uiso c ? H(52) 0.1535 -0.1276 0.5657 0.096 1.000 . Uiso c ? H(71) 0.3057 0.1679 0.6558 0.096 1.000 . Uiso c ? H(72) 0.2666 0.1932 0.5754 0.096 1.000 . Uiso c ? H(81) 0.2695 0.3720 0.6226 0.106 1.000 . Uiso c ? H(82) 0.2563 0.3197 0.6825 0.106 1.000 . Uiso c ? H(91) 0.0850 0.4227 0.5067 0.051 0.550 S Uiso d ? H(92) 0.1527 0.4515 0.5042 0.051 0.550 S Uiso d ? H(93) 0.1702 0.4515 0.5201 0.042 0.450 S Uiso d ? H(94) 0.1950 0.3254 0.5161 0.042 0.450 S Uiso d ? H(101) 0.1598 0.2471 0.4795 0.057 0.550 S Uiso d ? H(102) 0.0976 0.3083 0.4188 0.057 0.550 S Uiso d ? H(103) 0.0840 0.3397 0.4243 0.071 0.450 S Uiso d ? H(104) 0.0579 0.3862 0.4760 0.071 0.450 S Uiso d ? H(111) -0.0664 0.3628 0.6392 0.093 1.000 . Uiso c ? H(112) -0.0643 0.4229 0.5748 0.093 1.000 . Uiso c ? H(113) -0.0973 0.2994 0.5666 0.093 1.000 . Uiso c ? H(121) 0.2820 -0.1485 0.6249 0.096 1.000 . Uiso c ? H(122) 0.2960 -0.0470 0.5844 0.096 1.000 . Uiso c ? H(123) 0.3261 -0.0413 0.6660 0.096 1.000 . Uiso c ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ni(0) 0.060(2) 0.040(1) 0.049(1) -0.003(1) 0.035(1) 0.003(1) Cl(1) 0.092(5) 0.091(4) 0.080(4) -0.009(4) 0.061(4) -0.002(4) Cl(2) 0.094(5) 0.054(4) 0.098(5) 0.002(3) 0.051(4) -0.003(3) S(1) 0.075(4) 0.051(3) 0.054(3) -0.013(3) 0.028(3) -0.001(3) S(2) 0.079(4) 0.055(3) 0.057(3) -0.007(3) 0.047(3) 0.001(3) O(1) 0.08(1) 0.046(8) 0.081(9) 0.012(7) 0.053(9) 0.012(7) O(11) 0.14(1) 0.09(1) 0.11(1) -0.01(1) 0.10(1) -0.001(9) N(1) 0.07(1) 0.042(9) 0.048(9) -0.012(9) 0.036(9) -0.007(8) N(2) 0.11(1) 0.05(1) 0.07(1) -0.01(1) 0.06(1) -0.012(8) N(3) 0.08(1) 0.046(9) 0.057(9) -0.019(9) 0.041(9) -0.004(8) C(1) 0.08(2) 0.05(1) 0.07(1) 0.01(1) 0.05(1) 0.01(1) C(2) 0.10(2) 0.05(1) 0.07(1) 0.01(1) 0.06(1) 0.00(1) C(3) 0.10(2) 0.06(1) 0.05(1) 0.02(1) 0.06(1) 0.01(1) C(4) 0.10(2) 0.03(1) 0.11(2) -0.01(1) 0.08(1) 0.02(1) C(5) 0.10(2) 0.06(1) 0.06(1) 0.02(1) 0.05(1) 0.02(1) C(6) 0.08(2) 0.06(1) 0.04(1) 0.01(1) 0.03(1) 0.00(1) C(7) 0.09(2) 0.10(2) 0.09(2) -0.01(2) 0.06(1) -0.00(2) C(8) 0.10(2) 0.08(1) 0.07(1) -0.04(2) 0.05(1) -0.02(1) C(11) 0.10(2) 0.06(1) 0.15(2) 0.03(1) 0.09(2) 0.01(1) C(12) 0.10(2) 0.08(2) 0.08(1) 0.04(1) 0.05(1) 0.01(1) #============================================================================== # REFINEMENT DATA _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00002|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 1584 _refine_ls_number_parameters 263 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all ? _refine_ls_R_factor_gt 0.0924 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.0650 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 2.237 _refine_ls_shift/su_max 0.0244 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_min -0.64 _refine_diff_density_max 0.00 #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni S(1) 2.422(5) . . ? Ni S(2) 2.382(6) . . ? Ni O(1) 2.13(1) . . ? Ni N(1) 2.06(2) . . ? Ni N(2) 2.06(2) . . ? Ni N(3) 2.05(1) . . ? Cl(1) O(11) 1.36(2) . . ? Cl(1) O(13) 1.45(3) . . ? Cl(1) O(12) 1.48(3) . . ? Cl(1) O(14) 1.50(3) . . ? Cl(1) O(15) 1.44(4) . . ? Cl(1) O(16) 1.47(3) . . ? Cl(1) O(17) 1.42(5) . . ? Cl(1) O(18) 1.46(4) . . ? Cl(2) O(21) 1.40(2) . . ? Cl(2) O(22) 1.35(3) . . ? Cl(2) O(23) 1.40(3) . . ? Cl(2) O(24) 1.37(5) . . ? Cl(2) O(25) 1.47(4) . . ? Cl(2) O(26) 1.50(8) . . ? Cl(2) O(27) 1.44(8) . . ? Cl(2) O(28) 1.53(9) . . ? S(1) C(4) 1.74(2) . . ? S(1) C(5) 1.83(2) . . ? S(2) C(2) 1.85(2) . . ? S(2) C(3) 1.83(2) . . ? O(1) C(1) 1.18(3) . . ? O(13) O(15) 1.31(5) . . ? O(13) O(16) 1.03(5) . . ? O(12) O(17) 1.01(5) . . ? O(12) O(18) 1.25(6) . . ? O(14) O(15) 1.17(5) . . ? O(14) O(18) 1.19(5) . . ? O(16) O(17) 1.55(5) . . ? O(21) O(27) 1.38(8) . . ? O(22) O(28) 1.6(1) . . ? O(23) O(24) 1.36(6) . . ? O(24) O(26) 1.22(8) . . ? O(25) O(26) 1.3(1) . . ? O(25) O(27) 1.25(9) . . ? O(25) O(28) 1.1(1) . . ? O(26) O(27) 1.6(1) . . ? O(26) O(28) 1.5(2) . . ? N(1) C(6) 1.27(2) . . ? N(1) C(7) 1.47(3) . . ? N(2) C(8) 1.55(3) . . ? N(2) C(9a) 1.58(4) . . ? N(2) C(9b) 1.38(5) . . ? N(2) H(2n1) 0.98 . . no N(2) H(2n2) 0.99 . . no N(3) C(10a) 1.49(5) . . ? N(3) C(10b) 1.51(5) . . ? N(3) H(3n1) 0.96 . . no N(3) H(3n2) 0.97 . . no N(3) H(3n3) 0.95 . . no N(3) H(3n4) 0.97 . . no N(4) C(22) 1.04(5) . . ? C(1) C(2) 1.50(2) . . ? C(1) C(11) 1.51(3) . . ? C(2) H(21) 0.95 . . no C(2) H(22) 0.93 . . no C(3) C(4) 1.61(2) . . ? C(3) H(31) 0.95 . . no C(3) H(32) 0.94 . . no C(4) H(41) 0.96 . . no C(4) H(42) 0.95 . . no C(5) C(6) 1.53(3) . . ? C(5) H(51) 0.93 . . no C(5) H(52) 0.92 . . no C(6) C(12) 1.53(3) . . ? C(7) C(8) 1.52(3) . . ? C(7) H(71) 0.93 . . no C(7) H(72) 0.96 . . no C(8) H(81) 0.92 . . no C(8) H(82) 0.90 . . no C(9a) C(9b) 0.70(6) . . ? C(9a) C(10a) 1.51(5) . . ? C(9a) C(10b) 1.16(5) . . ? C(9a) H(91) 1.02 . . no C(9a) H(92) 0.96 . . no C(9a) H(93) 1.09 . . no C(9b) C(10a) 1.54(5) . . ? C(9b) C(10b) 1.59(6) . . ? C(9b) H(92) 1.06 . . no C(9b) H(93) 0.99 . . no C(9b) H(94) 0.95 . . no C(10a) C(10b) 0.87(7) . . ? C(10a) H(101) 0.93 . . no C(10a) H(102) 0.99 . . no C(10a) H(103) 1.11 . . no C(10b) H(91) 1.29 . . no C(10b) H(102) 1.27 . . no C(10b) H(103) 0.98 . . no C(10b) H(104) 0.96 . . no C(11) H(111) 0.98 . . no C(11) H(112) 0.99 . . no C(11) H(113) 1.01 . . no C(12) H(121) 0.96 . . no C(12) H(122) 0.99 . . no C(12) H(123) 0.98 . . no C(21) C(22) 1.37(5) . . ? #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S(1) Ni S(2) 91.6(2) . . . ? S(1) Ni O(1) 94.7(4) . . . ? S(1) Ni N(1) 83.3(4) . . . ? S(1) Ni N(2) 166.0(5) . . . ? S(1) Ni N(3) 95.4(4) . . . ? S(2) Ni O(1) 86.5(4) . . . ? S(2) Ni N(1) 91.6(4) . . . ? S(2) Ni N(2) 88.8(5) . . . ? S(2) Ni N(3) 163.6(4) . . . ? O(1) Ni N(1) 177.2(6) . . . ? O(1) Ni N(2) 99.3(6) . . . ? O(1) Ni N(3) 78.1(6) . . . ? N(1) Ni N(2) 82.8(6) . . . ? N(1) Ni N(3) 104.0(6) . . . ? N(2) Ni N(3) 88.0(6) . . . ? O(11) Cl(1) O(13) 102(2) . . . ? O(11) Cl(1) O(12) 111(2) . . . ? O(11) Cl(1) O(14) 107(2) . . . ? O(11) Cl(1) O(15) 110(2) . . . ? O(11) Cl(1) O(16) 96(2) . . . ? O(11) Cl(1) O(17) 115(2) . . . ? O(11) Cl(1) O(18) 108(2) . . . ? O(13) Cl(1) O(12) 136(2) . . . ? O(13) Cl(1) O(14) 101(2) . . . ? O(13) Cl(1) O(17) 100(2) . . . ? O(12) Cl(1) O(14) 96(2) . . . ? O(12) Cl(1) O(15) 131(2) . . . ? O(12) Cl(1) O(16) 106(2) . . . ? O(14) Cl(1) O(17) 128(3) . . . ? O(15) Cl(1) O(16) 95(2) . . . ? O(15) Cl(1) O(17) 132(3) . . . ? O(15) Cl(1) O(18) 92(2) . . . ? O(17) Cl(1) O(18) 89(3) . . . ? O(21) Cl(2) O(22) 103(2) . . . ? O(21) Cl(2) O(23) 98(1) . . . ? O(21) Cl(2) O(24) 126(2) . . . ? O(21) Cl(2) O(25) 103(2) . . . ? O(21) Cl(2) O(26) 119(3) . . . ? O(22) Cl(2) O(23) 93(2) . . . ? O(22) Cl(2) O(24) 125(2) . . . ? O(22) Cl(2) O(25) 93(3) . . . ? O(22) Cl(2) O(26) 129(3) . . . ? O(22) Cl(2) O(27) 122(4) . . . ? O(23) Cl(2) O(26) 109(3) . . . ? O(23) Cl(2) O(28) 117(4) . . . ? O(24) Cl(2) O(25) 99(3) . . . ? O(24) Cl(2) O(27) 107(4) . . . ? O(27) Cl(2) O(28) 95(5) . . . ? Ni S(1) C(4) 99.9(5) . . . ? Ni S(1) C(5) 96.9(6) . . . ? C(4) S(1) C(5) 97.5(9) . . . ? Ni S(2) C(2) 91.4(6) . . . ? Ni S(2) C(3) 97.9(6) . . . ? C(2) S(2) C(3) 105.7(9) . . . ? Ni O(1) C(1) 120(1) . . . ? Ni N(1) C(6) 125(1) . . . ? Ni N(1) C(7) 114(1) . . . ? C(6) N(1) C(7) 121(2) . . . ? Ni N(2) C(8) 109(1) . . . ? Ni N(2) C(9a) 101(2) . . . ? Ni N(2) C(9b) 109(2) . . . ? Ni N(2) H(2n1) 105.3 . . . no Ni N(2) H(2n2) 111.4 . . . no C(8) N(2) C(9a) 129(2) . . . ? C(8) N(2) C(9b) 104(3) . . . ? C(8) N(2) H(2n1) 108.4 . . . no C(8) N(2) H(2n2) 114.8 . . . no C(9a) N(2) H(2n1) 102.1 . . . no C(9b) N(2) H(2n2) 108.6 . . . no H(2n1) N(2) H(2n2) 12.6 . . . no Ni N(3) C(10a) 103(1) . . . ? Ni N(3) C(10b) 102(2) . . . ? Ni N(3) H(3n1) 112.4 . . . no Ni N(3) H(3n2) 111.9 . . . no Ni N(3) H(3n3) 113.0 . . . no Ni N(3) H(3n4) 112.1 . . . no C(10a) N(3) H(3n1) 110.7 . . . no C(10a) N(3) H(3n2) 111.5 . . . no C(10b) N(3) H(3n3) 111.4 . . . no C(10b) N(3) H(3n4) 110.8 . . . no H(3n1) N(3) H(3n2) 107.1 . . . no H(3n3) N(3) H(3n4) 107.4 . . . no O(1) C(1) C(2) 120(2) . . . ? O(1) C(1) C(11) 117(2) . . . ? C(2) C(1) C(11) 124(2) . . . ? S(2) C(2) C(1) 121(2) . . . ? S(2) C(2) H(21) 106.0 . . . no S(2) C(2) H(22) 107.2 . . . no C(1) C(2) H(21) 105.1 . . . no C(1) C(2) H(22) 106.3 . . . no H(21) C(2) H(22) 111.1 . . . no S(2) C(3) C(4) 113(1) . . . ? S(2) C(3) H(31) 106.2 . . . no S(2) C(3) H(32) 106.5 . . . no C(4) C(3) H(31) 109.9 . . . no C(4) C(3) H(32) 111.4 . . . no H(31) C(3) H(32) 109.9 . . . no S(1) C(4) C(3) 116(2) . . . ? S(1) C(4) H(41) 109.4 . . . no S(1) C(4) H(42) 109.9 . . . no C(3) C(4) H(41) 106.3 . . . no C(3) C(4) H(42) 105.8 . . . no H(41) C(4) H(42) 108.8 . . . no S(1) C(5) C(6) 116(1) . . . ? S(1) C(5) H(51) 110.2 . . . no S(1) C(5) H(52) 111.0 . . . no C(6) C(5) H(51) 102.7 . . . no C(6) C(5) H(52) 103.1 . . . no H(51) C(5) H(52) 113.5 . . . no N(1) C(6) C(5) 118(2) . . . ? N(1) C(6) C(12) 126(2) . . . ? C(5) C(6) C(12) 115(2) . . . ? N(1) C(7) C(8) 111(2) . . . ? N(1) C(7) H(71) 109.9 . . . no N(1) C(7) H(72) 109.1 . . . no C(8) C(7) H(71) 106.3 . . . no C(8) C(7) H(72) 110.1 . . . no H(71) C(7) H(72) 110.7 . . . no N(2) C(8) C(7) 109(1) . . . ? N(2) C(8) H(81) 102.5 . . . no N(2) C(8) H(82) 101.2 . . . no C(7) C(8) H(81) 112.4 . . . no C(7) C(8) H(82) 113.0 . . . no H(81) C(8) H(82) 117.1 . . . no N(2) C(9a) C(10a) 107(2) . . . ? N(2) C(9a) H(91) 113.2 . . . no N(2) C(9a) H(92) 115.5 . . . no N(2) C(9a) H(93) 95.8 . . . no C(10a) C(9a) H(91) 107.2 . . . no C(10a) C(9a) H(92) 111.1 . . . no H(91) C(9a) H(92) 102.7 . . . no N(2) C(9b) C(10b) 108(4) . . . ? N(2) C(9b) H(93) 114.9 . . . no N(2) C(9b) H(94) 113.5 . . . no C(10b) C(9b) H(93) 106.3 . . . no C(10b) C(9b) H(94) 107.0 . . . no H(93) C(9b) H(94) 106.3 . . . no N(3) C(10a) C(9a) 105(3) . . . ? N(3) C(10a) H(101) 113.0 . . . no N(3) C(10a) H(102) 110.7 . . . no N(3) C(10a) H(103) 103.5 . . . no C(9a) C(10a) H(101) 109.0 . . . no C(9a) C(10a) H(102) 111.2 . . . no H(101) C(10a) H(102) 108.0 . . . no N(3) C(10b) C(9b) 113(3) . . . ? N(3) C(10b) H(103) 108.6 . . . no N(3) C(10b) H(104) 109.6 . . . no C(9b) C(10b) H(103) 110.2 . . . no C(9b) C(10b) H(104) 109.2 . . . no H(103) C(10b) H(104) 106.1 . . . no C(1) C(11) H(111) 116.6 . . . no C(1) C(11) H(112) 115.2 . . . no C(1) C(11) H(113) 115.1 . . . no H(111) C(11) H(112) 103.7 . . . no H(111) C(11) H(113) 102.7 . . . no H(112) C(11) H(113) 101.6 . . . no C(6) C(12) H(121) 113.5 . . . no C(6) C(12) H(122) 113.2 . . . no C(6) C(12) H(123) 114.4 . . . no H(121) C(12) H(122) 105.3 . . . no H(121) C(12) H(123) 106.0 . . . no H(122) C(12) H(123) 103.5 . . . no N(4) C(22) C(21) 180.00 . . . ? #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Ni N(3) 2.05(1) . . no Ni N(1) 2.06(2) . . no Ni N(2) 2.06(2) . . no Ni C(10b) 2.80(5) . . no Ni C(10a) 2.80(4) . . no Ni C(9a) 2.82(4) . . no Ni C(9b) 2.84(5) . . no Ni C(1) 2.91(2) . . no Ni C(8) 2.96(2) . . no Ni C(7) 2.98(2) . . no Ni C(6) 2.98(2) . . no Ni C(2) 3.05(3) . . no Cl(2) O(24) 1.37(5) . . no Cl(2) O(27) 1.44(8) . . no Cl(2) O(25) 1.47(4) . . no Cl(2) O(26) 1.50(8) . . no Cl(2) O(28) 1.53(9) . . no S(1) C(4) 1.74(2) . . no S(1) C(5) 1.83(2) . . no S(1) C(3) 2.85(2) . . no S(1) C(6) 2.86(2) . . no S(1) N(1) 2.99(2) . . no S(2) C(3) 1.83(2) . . no S(2) C(2) 1.85(2) . . no S(2) C(4) 2.87(2) . . no S(2) C(1) 2.92(2) . . no S(2) N(2) 3.12(2) . . no O(1) C(1) 1.18(3) . . no O(1) C(11) 2.30(3) . . no O(1) C(2) 2.33(2) . . no O(1) N(3) 2.63(2) . . no O(1) C(10b) 3.13(6) . . no O(1) O(27) 3.16(7) . . no O(14) C(10a) 2.67(6) . 7_556 no O(14) N(3) 2.97(5) . 7_556 no O(14) C(8) 3.15(6) . . no O(15) C(10a) 3.12(6) . 7_556 no O(15) C(21) 3.17(4) . . no O(21) O(27) 1.38(8) . . no O(21) O(25) 2.25(4) . . no O(21) O(24) 2.46(4) . . no O(21) O(26) 2.49(7) . . no O(21) O(28) 2.79(9) . . no O(21) N(2) 3.08(3) . . no O(22) O(28) 1.6(1) . . no O(22) O(25) 2.04(6) . . no O(22) O(24) 2.41(6) . . no O(22) O(27) 2.4(1) . . no O(22) O(26) 2.6(1) . . no O(23) O(24) 1.36(6) . . no O(23) O(26) 2.36(7) . . no O(23) O(28) 2.50(9) . . no O(23) O(27) 2.67(8) . . no O(23) O(25) 2.81(5) . . no O(24) O(26) 1.22(8) . . no O(24) O(28) 1.9(1) . . no O(24) O(25) 2.16(6) . . no O(24) O(27) 2.25(8) . . no O(24) C(21) 3.10(6) . 5_455 no O(24) C(22) 3.14(6) . 5_455 no O(25) O(28) 1.1(1) . . no O(25) O(27) 1.25(9) . . no O(25) O(26) 1.3(1) . . no O(25) C(10b) 3.14(6) . 3_566 no O(26) O(28) 1.5(2) . . no O(26) O(27) 1.6(1) . . no O(26) C(22) 2.9(1) . 5_455 no O(26) C(10b) 2.97(7) . 3_566 no O(26) N(4) 3.09(9) . 5_455 no O(27) O(28) 2.2(1) . . no O(27) C(1) 2.77(8) . . no O(27) C(2) 2.88(8) . . no O(28) C(10b) 3.1(1) . 3_566 no N(1) C(6) 1.27(2) . . no N(1) C(7) 1.47(3) . . no N(1) C(5) 2.41(2) . . no N(1) C(8) 2.46(3) . . no N(1) C(12) 2.50(3) . . no N(1) N(2) 2.73(2) . . no N(2) C(9b) 1.38(5) . . no N(2) C(8) 1.55(3) . . no N(2) C(9a) 1.58(4) . . no N(2) C(10b) 2.41(4) . . no N(2) C(10a) 2.48(4) . . no N(2) C(7) 2.50(3) . . no N(2) N(3) 2.86(2) . . no N(3) C(10a) 1.49(5) . . no N(3) C(10b) 1.51(5) . . no N(3) C(9a) 2.37(4) . . no N(3) C(9b) 2.58(5) . . no N(4) C(22) 1.04(5) . . no N(4) C(21) 2.41(5) . . no C(1) C(2) 1.50(2) . . no C(1) C(11) 1.51(3) . . no C(2) C(11) 2.66(2) . . no C(2) C(3) 2.93(2) . . no C(3) C(4) 1.61(2) . . no C(4) C(5) 2.69(4) . . no C(5) C(6) 1.53(3) . . no C(5) C(12) 2.59(3) . . no C(6) C(12) 1.53(3) . . no C(6) C(7) 2.39(3) . . no C(7) C(8) 1.52(3) . . no C(7) C(12) 2.93(3) . . no C(7) C(9b) 2.94(4) . . no C(8) C(9b) 2.31(4) . . no C(8) C(9a) 2.83(3) . . no C(9a) C(10b) 1.16(5) . . no C(9a) C(10a) 1.51(5) . . no C(9b) C(10b) 1.59(6) . . no C(21) C(22) 1.37(5) . . no #------------------------------------------------------------------------------