Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Oksana Nesterova' _publ_contact_author_address ; Department of Inorganic Chemistry National Taras Shevchenko University Volodymyrska str. 64 Kyiv 01033 UKRAINE ; _publ_contact_author_email NESTEROVA@UNIV.KIEV.UA _publ_section_title ; Structural, Magnetic, High-Frequency and High-Field EPR Investigation of Double-Stranded Heterometallic [{Ni(en)2}2(u-NCS)4Cd(NCS)2] n.nCH3CN Polymer Self-Assembled from Cadmium Oxide, Nickel Thiocyanate and Ethylenediamine ; _publ_section_references ; Sheldrick, G M. (1996). SADABS. Program for Empirical Absorption Correction of Area Detector Data. University of Gottingen, Germany. Siemens (1995). SMART and SAINT. Area-Detector Control and Integration Software. Siemens Analytical X-ray Systems Inc., Madison, Wisconsin, USA. Hall, S.R., King, G.S.D., and Stewart., J.M. (1995). The Xtal 3.5 User's Manual. University of Western Australia, Lamb: Perth. ; loop_ _publ_author_name 'Oksana Nesterova' 'Julia Jezierska' 'Vladimir N. Kokozay' 'Wolfgang Linert' 'Andrew Ozarowski' ; S.Petrusenko ; 'Brian W. Skelton' #======================================================================= # Data block for single structure (one for each study in the paper) #======================================================================= data_po272 _database_code_depnum_ccdc_archive 'CCDC 610955' # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C16 H35 Cd1 N15 Ni2 S6' _chemical_formula_moiety 'C14 H32 Cd1 N14 Ni2 S6, C2 H3 N' _chemical_formula_weight 859.81 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_1_21/n_1 _symmetry_space_group_name_Hall -p_2yn loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 13.458(2) _cell_length_b 16.955(3) _cell_length_c 14.681(3) _cell_angle_alpha 90.00000 _cell_angle_beta 91.873(3) _cell_angle_gamma 90.00000 _cell_volume 3348.1(10) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.706 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 5052 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 27.83 _cell_measurement_temperature 150(2) _exptl_absorpt_coefficient_mu 2.152 _exptl_crystal_description prism _exptl_crystal_size_max .43 _exptl_crystal_size_mid .38 _exptl_crystal_size_min .21 _exptl_crystal_size_rad ? _exptl_crystal_colour mauve _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .74 _exptl_absorpt_correction_T_max 1 _diffrn_reflns_number 30952 _reflns_number_total 8289 _reflns_Friedel_coverage 0 _reflns_number_gt 8289 _reflns_threshold_expression 'I > 2.00 sig(I)' _diffrn_reflns_theta_max 28.5 _diffrn_reflns_theta_full 28.5 _diffrn_measured_fraction_theta_max 1.0 _diffrn_measured_fraction_theta_full 1.0 _diffrn_reflns_av_R_equivalents .041 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt .051 _refine_ls_wR_factor_ref .122 _refine_ls_goodness_of_fit_ref 1.198 _refine_ls_number_reflns 8289 _refine_ls_number_parameters 378 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .008 _refine_diff_density_min -1.009 _refine_diff_density_max 2.733 _refine_ls_extinction_method none _refine_ls_extinction_coef ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'Siemens SAINT' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 64 .002 .002 'IT Vol C. Table 6.1.1.4 Table 6.1.1.5' H ? 0 140 0 0 'IT Vol C. Table 6.1.1.4 Table 6.1.1.5' Cd ? 0 4 -1.005 1.202 'IT Vol C. Table 6.1.1.4 Table 6.1.1.5' N ? 0 60 .004 .003 'IT Vol C. Table 6.1.1.4 Table 6.1.1.5' Ni ? 0 8 .285 1.113 'IT Vol C. Table 6.1.1.4 Table 6.1.1.5' S ? 0 24 .11 .124 'IT Vol C. Table 6.1.1.4 Table 6.1.1.5' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cd1 .50879(3) .20794(2) .28180(2) .02068(17) Uani ? ? 1.00000 ? ? Ni1 .25473(5) .01267(4) .49249(4) .0195(3) Uani ? ? 1.00000 ? ? Ni2 .30151(5) -.02478(4) .00641(4) .0197(3) Uani ? ? 1.00000 ? ? S1 .71320(9) .20356(8) .28707(9) .0234(6) Uani ? ? 1.00000 ? ? C1 .7249(4) .1328(3) .3647(3) .022(2) Uani ? ? 1.00000 ? ? N1 .7320(3) .0827(3) .4179(3) .025(2) Uani ? ? 1.00000 ? ? S2 .30787(10) .20887(10) .26039(11) .0354(7) Uani ? ? 1.00000 ? ? C2 .2767(4) .1500(3) .3448(3) .021(2) Uani ? ? 1.00000 ? ? N2 .2524(3) .1095(3) .4022(3) .029(2) Uani ? ? 1.00000 ? ? S3 .52548(10) .04874(7) .25885(9) .0244(6) Uani ? ? 1.00000 ? ? C3 .4400(4) .0279(3) .1785(3) .023(2) Uani ? ? 1.00000 ? ? N3 .3826(3) .0116(3) .1216(3) .028(2) Uani ? ? 1.00000 ? ? S4 .51677(11) .24913(8) .10227(9) .0266(6) Uani ? ? 1.00000 ? ? C4 .5610(4) .1689(3) .0541(3) .023(2) Uani ? ? 1.00000 ? ? N4 .5929(3) .1139(3) .0186(3) .027(2) Uani ? ? 1.00000 ? ? S5 .57433(14) .24393(11) .60245(11) .0426(9) Uani ? ? 1.00000 ? ? C5 .5334(4) .2112(3) .5034(4) .028(3) Uani ? ? 1.00000 ? ? N5 .5054(3) .1860(3) .4355(3) .030(2) Uani ? ? 1.00000 ? ? S6 .48516(12) .50465(9) .31677(12) .0369(8) Uani ? ? 1.00000 ? ? C6 .5024(4) .4092(3) .3076(4) .027(3) Uani ? ? 1.00000 ? ? N6 .5131(4) .3422(3) .3006(3) .032(2) Uani ? ? 1.00000 ? ? N11 .1591(3) .0652(3) .5848(3) .023(2) Uani ? ? 1.00000 ? ? C11 .2216(5) .0934(4) .6625(4) .032(3) Uani ? ? 1.00000 ? ? C12 .3137(5) .1316(4) .6271(4) .037(3) Uani ? ? 1.00000 ? ? N12 .3645(3) .0746(3) .5687(3) .028(2) Uani ? ? 1.00000 ? ? N21 .3483(3) -.0435(3) .4019(3) .032(2) Uani ? ? 1.00000 ? ? C21 .2844(5) -.0741(4) .3241(4) .034(3) Uani ? ? 1.00000 ? ? C22 .1926(4) -.1085(3) .3630(4) .028(3) Uani ? ? 1.00000 ? ? N22 .1443(3) -.0467(3) .4160(3) .025(2) Uani ? ? 1.00000 ? ? N31 .3774(3) .0574(3) -.0718(3) .028(2) Uani ? ? 1.00000 ? ? C31 .3315(7) .1359(6) -.0567(10) .036(5) Uani ? ? .688(13) ? ? C31' .312(2) .1284(15) -.0916(16) .032(6) Uiso ? ? .312(13) ? ? C32 .2196(7) .1259(6) -.0517(7) .038(5) Uani ? ? .688(13) ? ? C32' .2626(14) .1454(10) -.0054(12) .026(4) Uiso ? ? .312(13) ? ? N32 .2023(4) .0707(3) .0212(4) .034(3) Uani ? ? 1.00000 ? ? N41 .2201(3) -.0725(3) -.1066(3) .030(2) Uani ? ? 1.00000 ? ? C41 .1777(8) -.1460(5) -.0780(6) .031(4) Uani ? ? .688(13) ? ? C41' .145(2) -.1290(18) -.052(2) .054(7) Uiso ? ? .312(13) ? ? C42 .1331(7) -.1326(5) .0157(6) .031(4) Uani ? ? .688(13) ? ? C42' .185(2) -.169(2) .027(2) .062(8) Uiso ? ? .312(13) ? ? N42 .2156(4) -.1035(3) .0807(3) .033(3) Uani ? ? 1.00000 ? ? N10 .4855(4) .4083(3) .9193(4) .040(3) Uani ? ? 1.00000 ? ? C10 .5018(4) .3531(4) .8795(4) .032(3) Uani ? ? 1.00000 ? ? C20 .5238(5) .2821(5) .8296(5) .052(4) Uani ? ? 1.00000 ? ? H11aN .11380 .02823 .60538 .02800 Uiso ? ? 1.00000 ? ? H11bN .12440 .10612 .55790 .02800 Uiso ? ? 1.00000 ? ? H11a .24115 .05092 .70053 .04400 Uiso ? ? 1.00000 ? ? H11b .18639 .13142 .69640 .04400 Uiso ? ? 1.00000 ? ? H12a .35615 .14633 .67784 .05000 Uiso ? ? 1.00000 ? ? H12b .29521 .17784 .59401 .05000 Uiso ? ? 1.00000 ? ? H12aN .40500 .10182 .52950 .03500 Uiso ? ? 1.00000 ? ? H12bN .40216 .04059 .60333 .03500 Uiso ? ? 1.00000 ? ? H21aN .38128 -.08466 .43148 .04200 Uiso ? ? 1.00000 ? ? H21bN .39504 -.00811 .38192 .04200 Uiso ? ? 1.00000 ? ? H21a .31985 -.11296 .29159 .04300 Uiso ? ? 1.00000 ? ? H21b .26744 -.03163 .28382 .04300 Uiso ? ? 1.00000 ? ? H22a .21023 -.15185 .40209 .03300 Uiso ? ? 1.00000 ? ? H22b .14876 -.12640 .31580 .03300 Uiso ? ? 1.00000 ? ? H22aN .11219 -.01204 .37744 .03300 Uiso ? ? 1.00000 ? ? H22bN .09981 -.06898 .45465 .03300 Uiso ? ? 1.00000 ? ? H31aN .37206 .04471 -.13296 .03800 Uiso ? ? .688(13) ? ? H31bN .44366 .05945 -.05415 .03800 Uiso ? ? .688(13) ? ? H31a .34485 .16990 -.10621 .04900 Uiso ? ? .688(13) ? ? H31b .35703 .15775 -.00171 .04900 Uiso ? ? .688(13) ? ? H32a .19321 .10656 -.10706 .05900 Uiso ? ? .688(13) ? ? H32b .19067 .17542 -.03760 .05900 Uiso ? ? .688(13) ? ? H32aN .21314 .09444 .07689 .04400 Uiso ? ? .688(13) ? ? H32bN .13750 .05299 .01649 .04400 Uiso ? ? .688(13) ? ? H31'aN .39594 .03422 -.12547 .03800 Uiso ? ? .312(13) ? ? H31'bN .43352 .07437 -.03986 .03800 Uiso ? ? .312(13) ? ? H31'a .26815 .11494 -.14164 .03900 Uiso ? ? .312(13) ? ? H31'b .35572 .17003 -.11294 .03900 Uiso ? ? .312(13) ? ? H32'a .22396 .18936 -.00893 .03800 Uiso ? ? .312(13) ? ? H32'b .31469 .15330 .04400 .03800 Uiso ? ? .312(13) ? ? H32'aN .18072 .07372 .07991 .04400 Uiso ? ? .312(13) ? ? H32'bN .14806 .06589 -.01851 .04400 Uiso ? ? .312(13) ? ? H41aN .26242 -.08253 -.15353 .03700 Uiso ? ? .688(13) ? ? H41bN .17168 -.03792 -.12615 .03700 Uiso ? ? .688(13) ? ? H41a .22447 -.18619 -.07392 .04500 Uiso ? ? .688(13) ? ? H41b .12350 -.16057 -.11858 .04500 Uiso ? ? .688(13) ? ? H42a .10886 -.18137 .03869 .04800 Uiso ? ? .688(13) ? ? H42b .08233 -.09505 .01266 .04800 Uiso ? ? .688(13) ? ? H42aN .18839 -.07836 .12952 .04100 Uiso ? ? .688(13) ? ? H42bN .25389 -.14527 .10148 .04100 Uiso ? ? .688(13) ? ? H41'aN .25867 -.10477 -.14190 .03700 Uiso ? ? .312(13) ? ? H41'bN .19080 -.03441 -.14277 .03700 Uiso ? ? .312(13) ? ? H41'a .10476 -.15935 -.08660 .05600 Uiso ? ? .312(13) ? ? H41'b .09198 -.08728 -.02294 .05600 Uiso ? ? .312(13) ? ? H42'a .14302 -.20161 .06110 .07300 Uiso ? ? .312(13) ? ? H42'b .24327 -.19848 .01196 .07300 Uiso ? ? .312(13) ? ? H42'aN .15901 -.07816 .09875 .04100 Uiso ? ? .312(13) ? ? H42'bN .25186 -.12007 .13140 .04100 Uiso ? ? .312(13) ? ? H20a .51405 .23685 .86902 .07800 Uiso ? ? 1.00000 ? ? H20b .48003 .27669 .77813 .07800 Uiso ? ? 1.00000 ? ? H20c .59161 .28138 .81206 .07800 Uiso ? ? 1.00000 ? ? 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 Cd1 .02330(18) .02034(17) .01840(17) .00080(13) .00052(12) .00017(13) Ni1 .0182(3) .0198(3) .0206(3) -.0006(2) -.0001(2) .0033(2) Ni2 .0188(3) .0213(3) .0192(3) -.0010(2) .0015(2) -.0020(2) S1 .0242(6) .0217(6) .0244(6) -.0017(5) -.0002(5) .0044(5) C1 .019(2) .019(2) .026(2) -.0023(18) -.0002(18) -.005(2) N1 .018(2) .028(2) .030(2) .0020(17) .0014(16) .0053(19) S2 .0248(7) .0424(8) .0390(8) -.0002(6) -.0005(6) .0239(7) C2 .018(2) .021(2) .026(2) .0004(18) -.0009(18) .0036(19) N2 .022(2) .036(3) .029(2) -.0012(19) -.0033(17) .007(2) S3 .0300(7) .0210(6) .0218(6) -.0036(5) -.0051(5) .0002(5) C3 .030(3) .021(2) .019(2) -.000(2) -.0007(19) .0001(18) N3 .032(2) .028(2) .024(2) -.0025(19) -.0018(18) -.0011(18) S4 .0383(7) .0206(6) .0210(6) .0063(5) .0033(5) .0026(5) C4 .018(2) .030(3) .019(2) -.003(2) -.0025(17) .006(2) N4 .026(2) .028(2) .029(2) .0007(18) .0043(18) .0015(19) S5 .0525(10) .0451(9) .0296(7) .0042(7) -.0090(7) -.0065(7) C5 .032(3) .030(3) .023(3) -.000(2) .006(2) -.002(2) N5 .030(2) .034(3) .026(2) .003(2) .0050(18) .001(2) S6 .0355(8) .0235(7) .0518(9) -.0006(6) .0032(7) -.0021(6) C6 .023(3) .032(3) .025(2) -.001(2) .002(2) -.002(2) N6 .035(3) .028(2) .033(3) .001(2) .002(2) -.008(2) N11 .025(2) .019(2) .027(2) .0008(16) .0012(17) .0033(17) C11 .039(3) .030(3) .028(3) .002(2) -.004(2) -.006(2) C12 .040(3) .032(3) .039(3) -.009(3) -.004(3) .002(3) N12 .024(2) .028(2) .031(2) -.0037(18) -.0031(18) .0038(19) N21 .027(2) .034(3) .034(3) .001(2) .007(2) .001(2) C21 .038(3) .040(3) .023(3) .002(3) .004(2) .000(2) C22 .031(3) .027(3) .027(3) .002(2) -.004(2) -.006(2) N22 .029(2) .025(2) .023(2) -.0001(17) -.0013(17) .0023(17) N31 .026(2) .031(2) .027(2) -.0004(18) .0006(17) .0019(19) C31 .020(4) .025(4) .063(8) -.002(3) -.006(5) .011(5) C32 .033(5) .033(5) .050(6) .010(4) .003(4) .015(4) N32 .028(2) .033(3) .042(3) .002(2) .010(2) -.001(2) N41 .029(2) .032(2) .028(2) -.000(2) -.0042(18) -.006(2) C41 .039(5) .032(4) .021(4) -.007(4) .004(4) -.012(3) C42 .031(5) .038(5) .025(4) -.013(4) .010(3) -.009(3) N42 .035(3) .034(3) .031(2) -.009(2) .008(2) -.004(2) N10 .036(3) .040(3) .046(3) .004(2) .005(2) .003(3) C10 .025(3) .046(4) .025(3) -.002(2) .001(2) .005(2) C20 .040(4) .064(5) .054(4) -.011(3) .014(3) -.022(4) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Cd1 S1 . . 2.7505(14) ? Cd1 S2 . . 2.7120(15) ? Cd1 S3 . . 2.7304(14) ? Cd1 S4 . . 2.7322(14) ? Cd1 N5 . . 2.289(5) ? Cd1 N6 . . 2.293(5) ? Ni1 N2 . . 2.110(5) ? Ni1 N11 . . 2.098(4) ? Ni1 N12 . . 2.104(5) ? Ni1 N21 . . 2.091(5) ? Ni1 N22 . . 2.092(4) ? Ni1 N1 . '3 656' 2.089(5) ? Ni2 N3 . . 2.077(5) ? Ni2 N31 . . 2.093(5) ? Ni2 N32 . . 2.114(5) ? Ni2 N41 . . 2.119(5) ? Ni2 N42 . . 2.095(5) ? Ni2 N4 . '3 655' 2.114(5) ? S1 C1 . . 1.658(5) ? C1 N1 . . 1.155(7) ? S2 C2 . . 1.655(5) ? C2 N2 . . 1.144(7) ? S3 C3 . . 1.658(5) ? C3 N3 . . 1.153(7) ? S4 C4 . . 1.653(5) ? C4 N4 . . 1.158(7) ? S5 C5 . . 1.635(6) ? C5 N5 . . 1.137(7) ? S6 C6 . . 1.642(6) ? C6 N6 . . 1.150(8) ? N11 C11 . . 1.474(7) ? N11 H11aN . . .932 ? N11 H11bN . . .918 ? C11 C12 . . 1.507(9) ? C11 H11a . . .944 ? C11 H11b . . .949 ? C12 N12 . . 1.476(8) ? C12 H12a . . .956 ? C12 H12b . . .951 ? N12 H12aN . . .928 ? N12 H12bN . . .911 ? N21 C21 . . 1.500(8) ? N21 H21aN . . .926 ? N21 H21bN . . .924 ? C21 C22 . . 1.496(8) ? C21 H21a . . .951 ? C21 H21b . . .955 ? C22 N22 . . 1.470(7) ? C22 H22a . . .957 ? C22 H22b . . .945 ? N22 H22aN . . .915 ? N22 H22bN . . .918 ? N31 C31 . . 1.487(11) ? N31 C31' . . 1.51(3) ? N31 H31aN . . .923 ? N31 H31bN . . .922 ? N31 H31'aN . . .922 ? N31 H31'bN . . .922 ? C31 C31' . . .58(3) ? C31 C32 . . 1.519(13) ? C31 H31a . . .949 ? C31 H31b . . .943 ? C31' C32' . . 1.48(3) ? C31' H31'a . . .96 ? C31' H31'b . . .98 ? C32 N32 . . 1.446(11) ? C32 H32a . . .935 ? C32 H32b . . .952 ? C32' N32 . . 1.561(19) ? C32' H32'a . . .909 ? C32' H32'b . . 1.001 ? N32 H32aN . . .919 ? N32 H32bN . . .922 ? N32 H32'aN . . .920 ? N32 H32'bN . . .923 ? N41 C41 . . 1.439(11) ? N41 C41' . . 1.63(3) ? N41 H41aN . . .923 ? N41 H41bN . . .916 ? N41 H41'aN . . .924 ? N41 H41'bN . . .917 ? C41 C42 . . 1.536(12) ? C41 H41a . . .928 ? C41 H41b . . .959 ? C41' C42' . . 1.42(4) ? C41' H41'a . . .89 ? C41' H41'b . . 1.10 ? C42 N42 . . 1.521(10) ? C42 H42a . . .955 ? C42 H42b . . .934 ? C42' N42 . . 1.41(3) ? C42' H42'a . . .95 ? C42' H42'b . . .97 ? N42 H42aN . . .920 ? N42 H42bN . . .922 ? N42 H42'aN . . .921 ? N42 H42'bN . . .921 ? N10 C10 . . 1.128(9) ? C10 C20 . . 1.446(10) ? C20 H20a . . .972 ? C20 H20b . . .947 ? C20 H20c . . .957 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published S1 Cd1 S2 . . . 174.82(4) ? S1 Cd1 S3 . . . 83.72(4) ? S1 Cd1 S4 . . . 87.89(4) ? S1 Cd1 N5 . . . 91.16(12) ? S1 Cd1 N6 . . . 90.11(13) ? S2 Cd1 S3 . . . 94.43(5) ? S2 Cd1 S4 . . . 87.55(5) ? S2 Cd1 N5 . . . 93.62(12) ? S2 Cd1 N6 . . . 91.69(13) ? S3 Cd1 S4 . . . 97.34(4) ? S3 Cd1 N5 . . . 88.03(13) ? S3 Cd1 N6 . . . 173.82(13) ? S4 Cd1 N5 . . . 174.41(13) ? S4 Cd1 N6 . . . 82.00(13) ? N5 Cd1 N6 . . . 92.49(18) ? N2 Ni1 N11 . . . 94.50(18) ? N2 Ni1 N12 . . . 86.64(18) ? N2 Ni1 N21 . . . 87.3(2) ? N2 Ni1 N22 . . . 92.42(18) ? N2 Ni1 N1 . . '3 656' 175.94(17) ? N11 Ni1 N12 . . . 83.07(17) ? N11 Ni1 N21 . . . 178.03(18) ? N11 Ni1 N22 . . . 96.39(17) ? N11 Ni1 N1 . . '3 656' 87.91(17) ? N12 Ni1 N21 . . . 97.94(18) ? N12 Ni1 N22 . . . 178.87(18) ? N12 Ni1 N1 . . '3 656' 90.42(18) ? N21 Ni1 N22 . . . 82.63(18) ? N21 Ni1 N1 . . '3 656' 90.39(19) ? N22 Ni1 N1 . . '3 656' 90.55(17) ? N3 Ni2 N31 . . . 89.81(18) ? N3 Ni2 N32 . . . 90.4(2) ? N3 Ni2 N41 . . . 174.8(2) ? N3 Ni2 N42 . . . 92.84(19) ? N3 Ni2 N4 . . '3 655' 90.87(18) ? N31 Ni2 N32 . . . 82.4(2) ? N31 Ni2 N41 . . . 94.20(18) ? N31 Ni2 N42 . . . 175.68(19) ? N31 Ni2 N4 . . '3 655' 92.19(18) ? N32 Ni2 N41 . . . 93.5(2) ? N32 Ni2 N42 . . . 94.2(2) ? N32 Ni2 N4 . . '3 655' 174.4(2) ? N41 Ni2 N42 . . . 83.36(19) ? N41 Ni2 N4 . . '3 655' 85.65(18) ? N42 Ni2 N4 . . '3 655' 91.2(2) ? Cd1 S1 C1 . . . 96.39(18) ? S1 C1 N1 . . . 178.9(5) ? C1 N1 Ni1 . . '3 656' 176.5(4) ? Cd1 S2 C2 . . . 100.69(18) ? S2 C2 N2 . . . 178.0(5) ? Ni1 N2 C2 . . . 158.7(4) ? Cd1 S3 C3 . . . 103.89(18) ? S3 C3 N3 . . . 177.8(5) ? Ni2 N3 C3 . . . 169.6(4) ? Cd1 S4 C4 . . . 103.23(18) ? S4 C4 N4 . . . 178.3(5) ? C4 N4 Ni2 . . '3 655' 156.2(4) ? S5 C5 N5 . . . 177.8(5) ? Cd1 N5 C5 . . . 141.8(5) ? S6 C6 N6 . . . 179.0(5) ? Cd1 N6 C6 . . . 171.2(5) ? Ni1 N11 C11 . . . 107.0(3) ? Ni1 N11 H11aN . . . 110.2 ? Ni1 N11 H11bN . . . 110.9 ? C11 N11 H11aN . . . 109.3 ? C11 N11 H11bN . . . 110.9 ? H11aN N11 H11bN . . . 108.5 ? N11 C11 C12 . . . 109.1(5) ? N11 C11 H11a . . . 110.5 ? N11 C11 H11b . . . 110.1 ? C12 C11 H11a . . . 108.4 ? C12 C11 H11b . . . 108.6 ? H11a C11 H11b . . . 110.1 ? C11 C12 N12 . . . 108.7(5) ? C11 C12 H12a . . . 108.7 ? C11 C12 H12b . . . 109.0 ? N12 C12 H12a . . . 110.3 ? N12 C12 H12b . . . 111.2 ? H12a C12 H12b . . . 108.9 ? Ni1 N12 C12 . . . 107.8(3) ? Ni1 N12 H12aN . . . 109.6 ? Ni1 N12 H12bN . . . 110.5 ? C12 N12 H12aN . . . 109.0 ? C12 N12 H12bN . . . 110.5 ? H12aN N12 H12bN . . . 109.5 ? Ni1 N21 C21 . . . 107.4(3) ? Ni1 N21 H21aN . . . 109.5 ? Ni1 N21 H21bN . . . 109.6 ? C21 N21 H21aN . . . 110.5 ? C21 N21 H21bN . . . 111.2 ? H21aN N21 H21bN . . . 108.5 ? N21 C21 C22 . . . 107.7(4) ? N21 C21 H21a . . . 109.7 ? N21 C21 H21b . . . 109.3 ? C22 C21 H21a . . . 110.8 ? C22 C21 H21b . . . 110.3 ? H21a C21 H21b . . . 109.0 ? C21 C22 N22 . . . 108.0(5) ? C21 C22 H22a . . . 109.7 ? C21 C22 H22b . . . 110.4 ? N22 C22 H22a . . . 109.5 ? N22 C22 H22b . . . 109.9 ? H22a C22 H22b . . . 109.3 ? Ni1 N22 C22 . . . 108.0(3) ? Ni1 N22 H22aN . . . 109.6 ? Ni1 N22 H22bN . . . 109.4 ? C22 N22 H22aN . . . 109.8 ? C22 N22 H22bN . . . 110.1 ? H22aN N22 H22bN . . . 110.0 ? Ni2 N31 C31 . . . 107.6(5) ? Ni2 N31 C31' . . . 110.2(10) ? Ni2 N31 H31aN . . . 110.7 ? Ni2 N31 H31bN . . . 110.8 ? Ni2 N31 H31'aN . . . 109.6 ? Ni2 N31 H31'bN . . . 109.5 ? C31 N31 H31aN . . . 109.6 ? C31 N31 H31bN . . . 109.1 ? C31' N31 H31'aN . . . 110.4 ? C31' N31 H31'bN . . . 108.1 ? H31aN N31 H31bN . . . 109.0 ? H31'aN N31 H31'bN . . . 109.1 ? N31 C31 C32 . . . 108.9(7) ? N31 C31 H31a . . . 109.8 ? N31 C31 H31b . . . 109.7 ? C32 C31 H31a . . . 108.6 ? C32 C31 H31b . . . 109.7 ? H31a C31 H31b . . . 110.2 ? N31 C31' C32' . . . 105.5 ? N31 C31' H31'a . . . 107 ? N31 C31' H31'b . . . 107 ? C32' C31' H31'a . . . 115 ? C32' C31' H31'b . . . 115 ? H31'a C31' H31'b . . . 107 ? C31 C32 N32 . . . 107.0(8) ? C31 C32 H32a . . . 110.2 ? C31 C32 H32b . . . 108.9 ? N32 C32 H32a . . . 110.5 ? N32 C32 H32b . . . 109.4 ? H32a C32 H32b . . . 110.6 ? C31' C32' H32'a . . . 112.6 ? C31' C32' H32'b . . . 108.7 ? N32 C32' H32'a . . . 112.3 ? N32 C32' H32'b . . . 106.6 ? H32'a C32' H32'b . . . 108.5 ? Ni2 N32 C32 . . . 107.6(5) ? Ni2 N32 C32' . . . 105.1(7) ? Ni2 N32 H32aN . . . 110.1 ? Ni2 N32 H32bN . . . 110.0 ? Ni2 N32 H32'aN . . . 111.0 ? Ni2 N32 H32'bN . . . 110.9 ? C32 N32 H32aN . . . 110.5 ? C32 N32 H32bN . . . 109.2 ? C32' N32 H32'aN . . . 111.8 ? C32' N32 H32'bN . . . 108.7 ? H32aN N32 H32bN . . . 109.4 ? H32'aN N32 H32'bN . . . 109.3 ? Ni2 N41 C41 . . . 107.6(4) ? Ni2 N41 C41' . . . 98.8(12) ? Ni2 N41 H41aN . . . 109.8 ? Ni2 N41 H41bN . . . 110.2 ? Ni2 N41 H41'aN . . . 112.3 ? Ni2 N41 H41'bN . . . 112.7 ? C41 N41 H41aN . . . 108.5 ? C41 N41 H41bN . . . 111.1 ? C41' N41 H41'aN . . . 107.3 ? C41' N41 H41'bN . . . 115.9 ? H41aN N41 H41bN . . . 109.5 ? H41'aN N41 H41'bN . . . 109.4 ? N41 C41 C42 . . . 107.7(7) ? N41 C41 H41a . . . 112.4 ? N41 C41 H41b . . . 110.0 ? C42 C41 H41a . . . 109.6 ? C42 C41 H41b . . . 106.4 ? H41a C41 H41b . . . 110.6 ? N41 C41' C42' . . . 117(2) ? N41 C41' H41'a . . . 116 ? N41 C41' H41'b . . . 104 ? C42' C41' H41'a . . . 113 ? C42' C41' H41'b . . . 103 ? H41'a C41' H41'b . . . 102 ? C41 C42 N42 . . . 108.1(7) ? C41 C42 H42a . . . 109.7 ? C41 C42 H42b . . . 111.4 ? N42 C42 H42a . . . 108.1 ? N42 C42 H42b . . . 109.1 ? H42a C42 H42b . . . 110.4 ? C41' C42' H42'a . . . 120 ? C41' C42' H42'b . . . 111 ? H42'a C42' H42'b . . . 108 ? Ni2 N42 C42 . . . 106.5(4) ? Ni2 N42 C42' . . . 111.2(13) ? Ni2 N42 H42aN . . . 110.5 ? Ni2 N42 H42bN . . . 110.5 ? Ni2 N42 H42'aN . . . 109.2 ? Ni2 N42 H42'bN . . . 109.2 ? C42 N42 H42aN . . . 109.8 ? C42 N42 H42bN . . . 110.3 ? C42' N42 H42'aN . . . 107.1 ? C42' N42 H42'bN . . . 110.8 ? H42aN N42 H42bN . . . 109.2 ? H42'aN N42 H42'bN . . . 109.3 ? N10 C10 C20 . . . 179.1(6) ? C10 C20 H20a . . . 108.8 ? C10 C20 H20b . . . 110.7 ? C10 C20 H20c . . . 111.1 ? H20a C20 H20b . . . 107.9 ? H20a C20 H20c . . . 107.4 ? H20b C20 H20c . . . 110.9 ? _exptl_crystal_F_000 1744 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 17 _reflns_limit_k_min 0 _reflns_limit_k_max 22 _reflns_limit_l_min -19 _reflns_limit_l_max 19 _reflns_number_observed ? _reflns_d_resolution_high .732 _reflns_d_resolution_low 11.071 _diffrn_reflns_av_sigmaI/netI .059 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 150(2) _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .068 _refine_ls_wR_factor_all .122 _refine_ls_goodness_of_fit_all 1.198 _refine_ls_shift/su_mean .001 #===END