# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full J.Mater.Chem. _journal_coden_cambridge 1145 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Prof Canadell Enric' _publ_contact_author_email CANADELL@ICMAB.ES loop_ _publ_author_name C.Enric L.I.Buravov A.D.Dubrovskii O.A.Dyachenko V.N.Laukhin ; G.V.Shilov ; N.G.Spitsina E.B.Yagubskii data_dybr3 _database_code_depnum_ccdc_archive 'CCDC 243316' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ; tetra(bis(ethylenedioxo)tetrathiafulvalene) tetracyano-nickel acetonitrile solvate ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H22 N4 Ni0.50 O8 S8' _chemical_formula_weight 804.31 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni -3.0029 0.5091 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.1270(10) _cell_length_b 19.098(4) _cell_length_c 12.535(3) _cell_angle_alpha 87.03(3) _cell_angle_beta 71.53(3) _cell_angle_gamma 87.70(3) _cell_volume 1615.6(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.65 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.653 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 824 _exptl_absorpt_coefficient_mu 5.895 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.0750 _exptl_absorpt_correction_T_max 0.5240 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'KM-4 (Kuma Diffraction)' _diffrn_measurement_method 'omega/2 teta' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 6631 _diffrn_reflns_av_R_equivalents 0.0524 _diffrn_reflns_av_sigmaI/netI 0.0815 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 4.47 _diffrn_reflns_theta_max 80.56 _reflns_number_total 6479 _reflns_number_gt 2629 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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^)+(0.1414P)^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 6479 _refine_ls_number_parameters 479 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.1958 _refine_ls_R_factor_gt 0.0748 _refine_ls_wR_factor_ref 0.2091 _refine_ls_wR_factor_gt 0.1832 _refine_ls_goodness_of_fit_ref 0.842 _refine_ls_restrained_S_all 0.841 _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 S1A S 0.19296(16) 0.05877(5) 0.01298(9) 0.0276(3) Uani 1 1 d . . . S2A S 0.42520(16) 0.09867(5) -0.22130(9) 0.0274(3) Uani 1 1 d . . . S3A S 0.32385(16) -0.10158(5) -0.02981(9) 0.0281(3) Uani 1 1 d . . . S4A S 0.55708(16) -0.06320(5) -0.26512(9) 0.0271(3) Uani 1 1 d . . . O1A O 0.0921(5) 0.19206(15) 0.0499(3) 0.0369(8) Uani 1 1 d . . . O2A O 0.3215(5) 0.23171(15) -0.1801(3) 0.0368(8) Uani 1 1 d . . . O3A O 0.4279(5) -0.23478(16) -0.0693(3) 0.0368(8) Uani 1 1 d . . . O4A O 0.6568(5) -0.19710(15) -0.2991(3) 0.0362(8) Uani 1 1 d . . . C1A C 0.3493(6) 0.0328(2) -0.1183(4) 0.0234(10) Uani 1 1 d . . . C2A C 0.4031(6) -0.0365(2) -0.1354(4) 0.0252(10) Uani 1 1 d . . . C3A C 0.1965(6) 0.1471(2) -0.0271(4) 0.0272(10) Uani 1 1 d . . . C4A C 0.3026(6) 0.1647(2) -0.1355(4) 0.0259(10) Uani 1 1 d . . . C5A C 0.4490(6) -0.1685(2) -0.1156(4) 0.0258(10) Uani 1 1 d . . . C6A C 0.5526(6) -0.1509(2) -0.2233(4) 0.0267(10) Uani 1 1 d . . . C7A C 0.0647(8) 0.2593(2) -0.0042(5) 0.0402(13) Uani 1 1 d D . . C8A C 0.2534(8) 0.2811(2) -0.0904(5) 0.0411(13) Uani 1 1 d D . . C9A C 0.4932(8) -0.2854(3) -0.1565(5) 0.0439(13) Uani 1 1 d . . . H5A H 0.3909 -0.2900 -0.1913 0.061(18) Uiso 1 1 calc R . . H6A H 0.5138 -0.3308 -0.1229 0.068(19) Uiso 1 1 calc R . . C10A C 0.6819(8) -0.2640(2) -0.2450(5) 0.0397(13) Uani 1 1 d D . . H1A H 0.025(6) 0.2921(17) 0.057(2) 0.022(12) Uiso 1 1 d D . . H2A H -0.042(4) 0.2572(19) -0.038(3) 0.008(10) Uiso 1 1 d D . . H3A H 0.248(9) 0.3320(8) -0.107(5) 0.09(2) Uiso 1 1 d D . . H4A H 0.366(5) 0.292(3) -0.065(4) 0.056(17) Uiso 1 1 d D . . H7A H 0.729(6) -0.2991(16) -0.302(2) 0.022(11) Uiso 1 1 d D . . H8A H 0.776(5) -0.265(2) -0.202(3) 0.039(14) Uiso 1 1 d D . . S1B S -0.06199(16) 0.05930(5) -0.23642(9) 0.0267(3) Uani 1 1 d . . . S2B S 0.17675(16) 0.10016(5) -0.46940(9) 0.0273(3) Uani 1 1 d . . . S3B S 0.07051(16) -0.10061(5) -0.27960(9) 0.0283(3) Uani 1 1 d . . . S4B S 0.30911(16) -0.06154(5) -0.51354(9) 0.0267(3) Uani 1 1 d . . . O1B O -0.1671(5) 0.19240(16) -0.2001(3) 0.0377(8) Uani 1 1 d . . . O2B O 0.0692(5) 0.23291(15) -0.4270(3) 0.0366(8) Uani 1 1 d . . . O3B O 0.1759(5) -0.23365(15) -0.3194(3) 0.0377(8) Uani 1 1 d . . . O4B O 0.4090(5) -0.19554(16) -0.5473(3) 0.0365(8) Uani 1 1 d . . . C1B C 0.0958(6) 0.0337(2) -0.3659(4) 0.0249(10) Uani 1 1 d . . . C2B C 0.1526(6) -0.0353(2) -0.3845(3) 0.0220(10) Uani 1 1 d . . . C3B C -0.0586(6) 0.1479(2) -0.2764(4) 0.0246(10) Uani 1 1 d . . . C4B C 0.0494(6) 0.1661(2) -0.3835(4) 0.0274(11) Uani 1 1 d . . . C5B C 0.1958(6) -0.1680(2) -0.3639(4) 0.0275(11) Uani 1 1 d . . . C6B C 0.3043(7) -0.1498(2) -0.4714(4) 0.0271(10) Uani 1 1 d . . . C7B C -0.1964(7) 0.2592(2) -0.2535(5) 0.0369(12) Uani 1 1 d D . . C8B C -0.0058(8) 0.2824(2) -0.3381(5) 0.0398(13) Uani 1 1 d D . . C9B C 0.2430(9) -0.2841(2) -0.4080(5) 0.0414(13) Uani 1 1 d D . . C10B C 0.4345(9) -0.2626(3) -0.4939(5) 0.0449(14) Uani 1 1 d D . . H1B H -0.246(7) 0.291(2) -0.191(3) 0.046(15) Uiso 1 1 d D . . H2B H -0.302(5) 0.255(2) -0.288(3) 0.038(14) Uiso 1 1 d D . . H3B H -0.023(10) 0.3325(10) -0.354(6) 0.11(3) Uiso 1 1 d D . . H4B H 0.100(5) 0.290(3) -0.306(4) 0.053(16) Uiso 1 1 d D . . H5B H 0.244(7) -0.3278(15) -0.364(4) 0.063(18) Uiso 1 1 d D . . H6B H 0.134(5) -0.287(3) -0.440(4) 0.055(17) Uiso 1 1 d D . . H7B H 0.530(5) -0.260(2) -0.453(3) 0.036(13) Uiso 1 1 d D . . H8B H 0.472(7) -0.297(2) -0.552(3) 0.054(17) Uiso 1 1 d D . . Ni1 Ni 0.0000 0.5000 0.0000 0.0462(5) Uani 1 2 d S . . C1 C 0.0342(9) 0.4342(3) 0.1085(5) 0.0569(17) Uani 1 1 d . . . N1 N 0.0600(12) 0.3939(3) 0.1733(6) 0.106(3) Uani 1 1 d . . . C2 C -0.0971(11) 0.4313(3) -0.0639(6) 0.072(2) Uani 1 1 d . . . N2 N -0.1602(13) 0.3883(3) -0.0988(7) 0.129(3) Uani 1 1 d . . . N1' N -0.3923(16) 0.4023(4) -0.3362(9) 0.139(4) Uani 1 1 d . . . C1' C -0.4344(13) 0.4458(5) -0.2658(9) 0.102(3) Uani 1 1 d . . . C2' C -0.4758(12) 0.5002(4) -0.1867(7) 0.111(3) Uani 1 1 d . . . N2' N -0.6919(15) 0.4034(4) -0.5503(8) 0.130(3) Uani 1 1 d . . . C3' C 0.7483(14) -0.4434(4) -0.5196(8) 0.093(3) Uani 1 1 d . . . C4' C -0.1631(13) 0.5051(4) 0.3912(7) 0.121(4) 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 S1A 0.0292(7) 0.0244(5) 0.0265(7) -0.0015(5) -0.0053(6) 0.0033(5) S2A 0.0261(7) 0.0273(5) 0.0265(7) 0.0002(5) -0.0057(6) 0.0042(5) S3A 0.0289(7) 0.0264(5) 0.0267(7) 0.0000(5) -0.0060(6) 0.0036(5) S4A 0.0276(7) 0.0264(5) 0.0249(7) -0.0027(5) -0.0056(6) 0.0055(5) O1A 0.042(2) 0.0253(15) 0.038(2) -0.0114(15) -0.0057(17) 0.0093(14) O2A 0.038(2) 0.0266(16) 0.043(2) 0.0022(15) -0.0101(17) 0.0041(15) O3A 0.039(2) 0.0308(16) 0.037(2) 0.0033(15) -0.0081(17) 0.0035(15) O4A 0.040(2) 0.0281(16) 0.037(2) -0.0086(15) -0.0066(17) 0.0094(15) C1A 0.020(2) 0.024(2) 0.029(3) -0.0033(18) -0.011(2) 0.0013(18) C2A 0.021(2) 0.029(2) 0.029(3) -0.003(2) -0.013(2) -0.0009(19) C3A 0.024(3) 0.026(2) 0.031(3) -0.006(2) -0.008(2) 0.0033(19) C4A 0.023(3) 0.022(2) 0.033(3) 0.001(2) -0.010(2) 0.0014(19) C5A 0.025(3) 0.020(2) 0.035(3) -0.0020(19) -0.013(2) 0.0036(18) C6A 0.028(3) 0.026(2) 0.020(3) -0.0032(19) -0.001(2) 0.0099(19) C7A 0.039(3) 0.027(3) 0.057(4) -0.014(2) -0.019(3) 0.008(2) C8A 0.043(4) 0.021(2) 0.063(4) -0.004(2) -0.021(3) 0.002(2) C9A 0.053(4) 0.028(3) 0.050(4) -0.003(2) -0.018(3) 0.004(2) C10A 0.048(4) 0.025(2) 0.046(4) -0.005(2) -0.017(3) 0.015(2) S1B 0.0276(7) 0.0247(5) 0.0249(7) -0.0028(5) -0.0044(6) 0.0036(5) S2B 0.0260(7) 0.0269(5) 0.0258(7) 0.0009(5) -0.0045(6) 0.0034(5) S3B 0.0277(7) 0.0270(5) 0.0278(7) 0.0003(5) -0.0060(6) 0.0034(5) S4B 0.0264(7) 0.0271(5) 0.0238(7) -0.0034(5) -0.0044(6) 0.0048(5) O1B 0.042(2) 0.0294(16) 0.037(2) -0.0109(15) -0.0051(17) 0.0073(15) O2B 0.039(2) 0.0235(15) 0.043(2) 0.0029(15) -0.0083(18) 0.0006(15) O3B 0.047(2) 0.0201(15) 0.045(2) 0.0044(14) -0.0140(18) 0.0009(15) O4B 0.040(2) 0.0301(16) 0.035(2) -0.0103(15) -0.0052(17) 0.0065(15) C1B 0.021(2) 0.030(2) 0.025(3) -0.0052(19) -0.010(2) 0.0056(19) C2B 0.019(2) 0.025(2) 0.024(3) -0.0028(18) -0.010(2) 0.0053(18) C3B 0.025(3) 0.026(2) 0.021(3) -0.0027(19) -0.004(2) 0.0016(19) C4B 0.023(3) 0.025(2) 0.034(3) -0.003(2) -0.009(2) 0.0022(19) C5B 0.026(3) 0.024(2) 0.034(3) 0.000(2) -0.012(2) 0.0018(19) C6B 0.027(3) 0.027(2) 0.028(3) -0.005(2) -0.009(2) 0.0045(19) C7B 0.028(3) 0.028(2) 0.052(4) -0.008(2) -0.008(3) 0.006(2) C8B 0.044(3) 0.023(2) 0.061(4) -0.012(2) -0.027(3) 0.003(2) C9B 0.054(4) 0.020(2) 0.055(4) -0.001(2) -0.026(3) 0.001(2) C10B 0.047(4) 0.026(3) 0.068(4) -0.005(3) -0.028(4) 0.008(2) Ni1 0.0617(10) 0.0333(7) 0.0540(9) -0.0068(6) -0.0333(8) 0.0093(6) C1 0.088(5) 0.032(3) 0.064(4) -0.012(3) -0.042(4) 0.006(3) N1 0.190(7) 0.050(3) 0.114(5) 0.010(4) -0.103(5) -0.001(4) C2 0.114(6) 0.039(3) 0.105(5) 0.007(3) -0.095(5) -0.009(4) N2 0.218(8) 0.038(3) 0.211(8) -0.009(4) -0.184(7) 0.011(4) N1' 0.199(9) 0.086(5) 0.181(9) -0.030(6) -0.130(8) 0.035(6) C1' 0.094(7) 0.082(6) 0.148(10) 0.029(6) -0.070(7) 0.006(5) C2' 0.121(7) 0.091(6) 0.124(7) -0.065(6) -0.043(6) 0.044(5) N2' 0.196(9) 0.066(5) 0.154(9) 0.000(5) -0.092(8) -0.001(6) C3' 0.121(7) 0.063(5) 0.110(8) 0.020(5) -0.062(7) -0.010(5) C4' 0.121(7) 0.125(8) 0.131(8) -0.068(7) -0.054(7) 0.041(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 S1A C3A 1.733(4) . ? S1A C1A 1.753(4) . ? S2A C4A 1.723(4) . ? S2A C1A 1.727(4) . ? S3A C5A 1.740(4) . ? S3A C2A 1.741(4) . ? S4A C6A 1.728(4) . ? S4A C2A 1.737(5) . ? O1A C3A 1.343(5) . ? O1A C7A 1.456(5) . ? O2A C4A 1.363(5) . ? O2A C8A 1.456(6) . ? O3A C5A 1.359(5) . ? O3A C9A 1.448(6) . ? O4A C6A 1.349(5) . ? O4A C10A 1.447(5) . ? C1A C2A 1.372(6) . ? C3A C4A 1.361(6) . ? C5A C6A 1.350(6) . ? C7A C8A 1.493(7) . ? C9A C10A 1.503(7) . ? S1B C1B 1.738(4) . ? S1B C3B 1.739(4) . ? S2B C4B 1.732(4) . ? S2B C1B 1.744(4) . ? S3B C5B 1.738(5) . ? S3B C2B 1.740(4) . ? S4B C2B 1.734(4) . ? S4B C6B 1.739(4) . ? O1B C3B 1.341(5) . ? O1B C7B 1.449(5) . ? O2B C4B 1.356(5) . ? O2B C8B 1.453(6) . ? O3B C5B 1.339(5) . ? O3B C9B 1.459(6) . ? O4B C6B 1.345(5) . ? O4B C10B 1.446(5) . ? C1B C2B 1.373(5) . ? C3B C4B 1.354(6) . ? C5B C6B 1.359(6) . ? C7B C8B 1.501(7) . ? C9B C10B 1.503(8) . ? Ni1 C2 1.837(6) . ? Ni1 C2 1.837(6) 2_565 ? Ni1 C1 1.870(6) 2_565 ? Ni1 C1 1.870(6) . ? C1 N1 1.142(7) . ? C2 N2 1.122(7) . ? N1' C1' 1.203(11) . ? C1' C2' 1.431(12) . ? N2' C3' 1.155(10) 2_554 ? C3' N2' 1.155(11) 2_554 ? C3' C4' 1.495(11) 1_644 ? C4' C3' 1.495(11) 1_466 ? 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 C3A S1A C1A 94.3(2) . . ? C4A S2A C1A 94.5(2) . . ? C5A S3A C2A 93.7(2) . . ? C6A S4A C2A 94.2(2) . . ? C3A O1A C7A 110.4(4) . . ? C4A O2A C8A 109.9(4) . . ? C5A O3A C9A 110.3(3) . . ? C6A O4A C10A 111.3(3) . . ? C2A C1A S2A 123.5(4) . . ? C2A C1A S1A 120.3(3) . . ? S2A C1A S1A 116.2(2) . . ? C1A C2A S4A 120.9(3) . . ? C1A C2A S3A 122.4(4) . . ? S4A C2A S3A 116.7(2) . . ? O1A C3A C4A 125.5(4) . . ? O1A C3A S1A 117.8(3) . . ? C4A C3A S1A 116.8(3) . . ? C3A C4A O2A 124.1(4) . . ? C3A C4A S2A 118.1(3) . . ? O2A C4A S2A 117.7(3) . . ? C6A C5A O3A 125.3(4) . . ? C6A C5A S3A 117.7(3) . . ? O3A C5A S3A 116.9(3) . . ? O4A C6A C5A 124.2(4) . . ? O4A C6A S4A 118.1(3) . . ? C5A C6A S4A 117.6(3) . . ? O1A C7A C8A 110.5(4) . . ? O2A C8A C7A 112.0(4) . . ? O3A C9A C10A 111.6(4) . . ? O4A C10A C9A 111.2(4) . . ? C1B S1B C3B 94.4(2) . . ? C4B S2B C1B 94.1(2) . . ? C5B S3B C2B 94.3(2) . . ? C2B S4B C6B 94.0(2) . . ? C3B O1B C7B 110.9(3) . . ? C4B O2B C8B 110.5(4) . . ? C5B O3B C9B 110.4(4) . . ? C6B O4B C10B 111.3(4) . . ? C2B C1B S1B 121.2(3) . . ? C2B C1B S2B 122.4(3) . . ? S1B C1B S2B 116.4(2) . . ? C1B C2B S4B 121.6(3) . . ? C1B C2B S3B 121.5(3) . . ? S4B C2B S3B 116.9(2) . . ? O1B C3B C4B 125.3(4) . . ? O1B C3B S1B 117.6(3) . . ? C4B C3B S1B 117.1(3) . . ? C3B C4B O2B 124.3(4) . . ? C3B C4B S2B 117.9(3) . . ? O2B C4B S2B 117.7(3) . . ? O3B C5B C6B 124.9(4) . . ? O3B C5B S3B 118.1(4) . . ? C6B C5B S3B 116.9(3) . . ? O4B C6B C5B 124.4(4) . . ? O4B C6B S4B 117.7(3) . . ? C5B C6B S4B 117.9(3) . . ? O1B C7B C8B 110.3(4) . . ? O2B C8B C7B 111.9(4) . . ? O3B C9B C10B 111.3(4) . . ? O4B C10B C9B 110.3(4) . . ? C2 Ni1 C2 180.000(1) . 2_565 ? C2 Ni1 C1 90.2(2) . 2_565 ? C2 Ni1 C1 89.8(2) 2_565 2_565 ? C2 Ni1 C1 89.8(2) . . ? C2 Ni1 C1 90.2(2) 2_565 . ? C1 Ni1 C1 180.0(4) 2_565 . ? N1 C1 Ni1 178.3(7) . . ? N2 C2 Ni1 177.3(8) . . ? N1' C1' C2' 176.6(11) . . ? N2' C3' C4' 175.5(10) 2_554 1_644 ? _diffrn_measured_fraction_theta_max 0.917 _diffrn_reflns_theta_full 80.56 _diffrn_measured_fraction_theta_full 0.917 _refine_diff_density_max 1.471 _refine_diff_density_min -0.711 _refine_diff_density_rms 0.165 data_dybr4 _database_code_depnum_ccdc_archive 'CCDC 249303' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ; penta(bis(ethylenedioxo)tetrathiafulvalene) tetracyano-nickel ethylene glycol solvate ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H29 N2 Ni0.50 O13 S10' _chemical_formula_weight 975.51 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni -3.0029 0.5091 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 17.542(4) _cell_length_b 10.415(2) _cell_length_c 10.928(2) _cell_angle_alpha 71.94(3) _cell_angle_beta 84.40(3) _cell_angle_gamma 88.88(3) _cell_volume 1889.0(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.715 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1002 _exptl_absorpt_coefficient_mu 6.257 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.0915 _exptl_absorpt_correction_T_max 0.5501 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'KM-4 (Kuma Diffraction)' _diffrn_measurement_method 'omega/2 teta' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 8196 _diffrn_reflns_av_R_equivalents 0.0171 _diffrn_reflns_av_sigmaI/netI 0.0316 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.53 _diffrn_reflns_theta_max 80.47 _reflns_number_total 7790 _reflns_number_gt 4214 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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^)+(0.1574P)^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 7790 _refine_ls_number_parameters 582 _refine_ls_number_restraints 62 _refine_ls_R_factor_all 0.1270 _refine_ls_R_factor_gt 0.0674 _refine_ls_wR_factor_ref 0.2099 _refine_ls_wR_factor_gt 0.1864 _refine_ls_goodness_of_fit_ref 0.907 _refine_ls_restrained_S_all 0.903 _refine_ls_shift/su_max 0.001 _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 S1A S 0.60978(4) 0.65602(8) 1.08186(8) 0.0339(2) Uani 1 1 d . . . S2A S 0.56664(4) 0.56678(8) 1.36590(8) 0.0336(2) Uani 1 1 d . . . S3A S 0.43314(4) 0.63293(8) 1.03519(8) 0.0333(2) Uani 1 1 d . . . S4A S 0.39195(4) 0.54383(8) 1.31974(8) 0.0337(2) Uani 1 1 d . . . O1A O 0.75498(13) 0.6689(3) 1.1259(3) 0.0461(6) Uani 1 1 d . . . O2A O 0.71215(14) 0.5835(3) 1.4034(3) 0.0459(6) Uani 1 1 d . . . O3A O 0.28693(13) 0.6174(3) 1.0013(2) 0.0434(6) Uani 1 1 d . . . O4A O 0.24639(13) 0.5325(3) 1.2794(3) 0.0427(6) Uani 1 1 d . . . C1A C 0.53814(16) 0.6045(3) 1.2101(3) 0.0302(6) Uani 1 1 d . . . C2A C 0.46300(16) 0.5956(3) 1.1902(3) 0.0293(6) Uani 1 1 d . . . C3A C 0.68275(16) 0.6400(3) 1.1829(4) 0.0366(7) Uani 1 1 d . . . C4A C 0.66278(16) 0.6002(3) 1.3121(3) 0.0332(7) Uani 1 1 d . . . C5A C 0.33688(16) 0.5999(3) 1.0915(3) 0.0318(7) Uani 1 1 d . . . C6A C 0.31848(16) 0.5598(3) 1.2205(3) 0.0333(7) Uani 1 1 d . . . C7A C 0.80952(19) 0.6197(4) 1.2216(5) 0.0529(10) Uani 1 1 d D . . C8A C 0.7843(2) 0.6517(4) 1.3446(5) 0.0503(10) Uani 1 1 d D . . C9A C 0.21403(19) 0.5549(4) 1.0612(4) 0.0468(9) Uani 1 1 d D . . C10A C 0.19176(18) 0.5876(4) 1.1864(4) 0.0465(9) Uani 1 1 d D . . H1A H 0.815(3) 0.526(2) 1.233(4) 0.060(13) Uiso 1 1 d D . . H2A H 0.8588(16) 0.648(4) 1.181(4) 0.060(13) Uiso 1 1 d D . . H3A H 0.782(2) 0.747(2) 1.321(4) 0.057(12) Uiso 1 1 d D . . H4A H 0.8250(19) 0.629(4) 1.398(4) 0.052(12) Uiso 1 1 d D . . H5A H 0.1758(19) 0.583(4) 1.003(3) 0.043(10) Uiso 1 1 d D . . H6A H 0.206(2) 0.461(2) 1.076(4) 0.053(12) Uiso 1 1 d D . . H7A H 0.1423(15) 0.559(4) 1.231(4) 0.047(11) Uiso 1 1 d D . . H8A H 0.188(2) 0.681(2) 1.179(4) 0.041(10) Uiso 1 1 d D . . S1B S 0.60504(4) 0.85646(8) 0.48315(8) 0.0333(2) Uani 1 1 d . . . S2B S 0.56202(4) 0.76405(8) 0.76712(8) 0.0329(2) Uani 1 1 d . . . S3B S 0.43010(4) 0.83266(8) 0.43419(8) 0.0338(2) Uani 1 1 d . . . S4B S 0.38652(4) 0.74164(8) 0.71819(8) 0.0340(2) Uani 1 1 d . . . O1B O 0.74988(13) 0.8717(3) 0.5275(3) 0.0437(6) Uani 1 1 d . . . O2B O 0.70754(13) 0.7799(3) 0.8048(3) 0.0438(6) Uani 1 1 d . . . O3B O 0.28450(14) 0.8178(3) 0.3957(3) 0.0464(6) Uani 1 1 d . . . O4B O 0.24100(13) 0.7305(3) 0.6725(3) 0.0447(6) Uani 1 1 d . . . C1B C 0.53334(15) 0.8035(3) 0.6112(3) 0.0281(6) Uani 1 1 d . . . C2B C 0.45839(16) 0.7944(3) 0.5906(3) 0.0302(6) Uani 1 1 d . . . C3B C 0.67758(17) 0.8414(3) 0.5836(3) 0.0346(7) Uani 1 1 d . . . C4B C 0.65819(17) 0.7991(3) 0.7128(3) 0.0335(7) Uani 1 1 d . . . C5B C 0.33403(17) 0.7996(3) 0.4868(3) 0.0348(7) Uani 1 1 d . . . C6B C 0.31373(17) 0.7585(3) 0.6164(4) 0.0354(7) Uani 1 1 d . . . C7B C 0.80399(18) 0.8169(4) 0.6211(4) 0.0468(9) Uani 1 1 d D . . C8B C 0.77985(19) 0.8447(4) 0.7475(4) 0.0461(9) Uani 1 1 d D . . C9B C 0.2115(2) 0.7551(4) 0.4535(4) 0.0494(10) Uani 1 1 d D . . C10B C 0.18733(19) 0.7855(4) 0.5779(4) 0.0495(10) Uani 1 1 d D . . H1B H 0.807(2) 0.724(3) 0.627(4) 0.057(12) Uiso 1 1 d D . . H2B H 0.8525(16) 0.842(4) 0.576(4) 0.056(12) Uiso 1 1 d D . . H3B H 0.783(3) 0.940(2) 0.730(5) 0.070(14) Uiso 1 1 d D . . H4B H 0.817(2) 0.822(5) 0.807(4) 0.065(13) Uiso 1 1 d D . . H5B H 0.173(2) 0.784(5) 0.396(4) 0.066(13) Uiso 1 1 d D . . H6B H 0.211(2) 0.662(2) 0.467(4) 0.048(11) Uiso 1 1 d D . . H7B H 0.186(2) 0.878(2) 0.572(4) 0.035(9) Uiso 1 1 d D . . H8B H 0.1376(14) 0.761(4) 0.617(4) 0.041(10) Uiso 1 1 d D . . S1C S 0.61029(4) 1.05384(8) -0.11460(8) 0.0352(2) Uani 1 1 d . . . S2C S 0.56409(4) 0.96600(8) 0.16820(8) 0.0352(2) Uani 1 1 d . . . O1C O 0.75461(14) 1.0651(3) -0.0659(3) 0.0461(6) Uani 1 1 d . . . O2C O 0.70864(14) 0.9815(3) 0.2103(3) 0.0461(6) Uani 1 1 d . . . C1C C 0.53761(16) 1.0039(3) 0.0113(3) 0.0317(7) Uani 1 1 d . . . C2C C 0.68198(18) 1.0364(3) -0.0107(3) 0.0359(7) Uani 1 1 d . . . C3C C 0.66042(18) 0.9981(3) 0.1174(3) 0.0342(7) Uani 1 1 d . . . C4C C 0.8078(2) 1.0163(4) 0.0309(5) 0.0505(10) Uani 1 1 d D . . C5C C 0.7813(2) 1.0481(4) 0.1542(4) 0.0479(9) Uani 1 1 d D . . H1C H 0.812(2) 0.922(3) 0.038(4) 0.051(11) Uiso 1 1 d D . . H2C H 0.8576(16) 1.045(4) -0.012(4) 0.044(10) Uiso 1 1 d D . . H3C H 0.773(3) 1.142(3) 0.139(5) 0.088(17) Uiso 1 1 d D . . H4C H 0.818(2) 1.026(4) 0.217(4) 0.061(13) Uiso 1 1 d D . . Ni1 Ni 0.0000 0.5000 1.0000 0.0494(3) Uani 1 2 d S . . C1 C 0.0144(2) 0.6536(4) 1.0482(4) 0.0564(10) Uani 1 1 d . . . N1 N 0.0254(3) 0.7464(4) 1.0815(4) 0.0847(13) Uani 1 1 d . . . C2 C 0.0175(3) 0.3951(4) 1.1653(5) 0.0613(11) Uani 1 1 d . . . N2 N 0.0304(3) 0.3329(4) 1.2680(5) 0.0934(15) Uani 1 1 d . . . C1' C 0.0340(3) 1.0025(5) 1.2146(6) 0.0872(16) Uani 1 1 d . . . C2' C -0.0272(4) 0.0116(7) 1.3041(10) 0.146(3) Uani 1 1 d . . . O1' O 0.07303(16) 0.8761(3) 1.2506(3) 0.0750(9) Uani 1 1 d . . . O2' O 0.91590(18) 0.9150(4) 0.3419(4) 0.1088(15) Uani 1 1 d . . . C3' C -0.0055(3) 0.4285(4) 1.5407(5) 0.0746(13) Uani 1 1 d . . . O3' O 0.05410(18) 0.3467(3) 1.5104(3) 0.0744(9) 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 S1A 0.0279(4) 0.0408(4) 0.0300(5) -0.0075(4) 0.0015(3) -0.0052(3) S2A 0.0260(4) 0.0424(4) 0.0298(5) -0.0072(3) -0.0022(3) -0.0032(3) S3A 0.0254(4) 0.0424(4) 0.0291(5) -0.0069(3) -0.0011(3) -0.0031(3) S4A 0.0268(4) 0.0416(4) 0.0298(5) -0.0075(4) 0.0010(3) -0.0049(3) O1A 0.0246(11) 0.0582(15) 0.0513(17) -0.0130(12) 0.0056(10) -0.0094(10) O2A 0.0316(12) 0.0585(16) 0.0465(17) -0.0125(12) -0.0106(11) -0.0029(10) O3A 0.0266(11) 0.0617(16) 0.0393(16) -0.0112(12) -0.0058(10) -0.0019(10) O4A 0.0260(11) 0.0536(14) 0.0437(16) -0.0102(12) 0.0051(10) -0.0079(10) C1A 0.0256(14) 0.0311(14) 0.0309(18) -0.0059(12) -0.0004(11) 0.0003(10) C2A 0.0250(13) 0.0307(14) 0.0287(18) -0.0046(12) 0.0002(11) -0.0026(10) C3A 0.0218(13) 0.0382(16) 0.048(2) -0.0127(15) 0.0006(13) -0.0033(11) C4A 0.0235(13) 0.0417(17) 0.034(2) -0.0099(14) -0.0049(12) -0.0005(11) C5A 0.0250(13) 0.0373(15) 0.0325(19) -0.0094(13) -0.0051(12) -0.0012(11) C6A 0.0238(13) 0.0358(15) 0.039(2) -0.0104(14) 0.0015(12) -0.0035(11) C7A 0.0235(15) 0.057(2) 0.074(3) -0.016(2) -0.0010(16) 0.0019(14) C8A 0.0322(17) 0.053(2) 0.065(3) -0.014(2) -0.0158(17) -0.0039(15) C9A 0.0295(16) 0.060(2) 0.052(3) -0.0164(19) -0.0103(15) -0.0058(15) C10A 0.0253(15) 0.048(2) 0.062(3) -0.0102(18) -0.0038(15) -0.0009(13) S1B 0.0280(4) 0.0395(4) 0.0292(5) -0.0067(3) 0.0015(3) -0.0046(3) S2B 0.0248(4) 0.0424(4) 0.0281(5) -0.0063(3) -0.0007(3) -0.0033(3) S3B 0.0271(4) 0.0419(4) 0.0303(5) -0.0077(3) -0.0026(3) -0.0028(3) S4B 0.0275(4) 0.0411(4) 0.0303(5) -0.0074(3) 0.0007(3) -0.0041(3) O1B 0.0246(11) 0.0558(15) 0.0467(16) -0.0119(12) 0.0050(10) -0.0075(10) O2B 0.0281(11) 0.0613(16) 0.0387(15) -0.0098(12) -0.0049(10) -0.0033(10) O3B 0.0328(12) 0.0630(16) 0.0439(17) -0.0149(13) -0.0109(11) 0.0001(11) O4B 0.0257(11) 0.0562(15) 0.0508(17) -0.0165(12) 0.0036(10) -0.0053(10) C1B 0.0241(13) 0.0312(14) 0.0266(17) -0.0060(12) -0.0004(11) 0.0010(10) C2B 0.0277(13) 0.0287(14) 0.0320(19) -0.0059(12) -0.0040(12) 0.0008(10) C3B 0.0262(14) 0.0359(16) 0.038(2) -0.0064(14) -0.0010(12) -0.0045(11) C4B 0.0270(14) 0.0394(16) 0.033(2) -0.0082(14) -0.0051(12) -0.0001(12) C5B 0.0260(14) 0.0436(17) 0.035(2) -0.0115(14) -0.0058(12) 0.0015(12) C6B 0.0237(13) 0.0375(16) 0.044(2) -0.0116(14) -0.0016(13) -0.0017(11) C7B 0.0231(14) 0.050(2) 0.062(3) -0.0124(19) 0.0013(15) 0.0016(14) C8B 0.0293(16) 0.053(2) 0.054(3) -0.0122(18) -0.0077(15) -0.0051(14) C9B 0.0345(17) 0.052(2) 0.063(3) -0.016(2) -0.0169(17) -0.0045(15) C10B 0.0263(15) 0.052(2) 0.069(3) -0.017(2) -0.0034(16) -0.0008(14) S1C 0.0320(4) 0.0411(4) 0.0295(5) -0.0074(4) 0.0008(3) -0.0044(3) S2C 0.0304(4) 0.0439(5) 0.0280(5) -0.0063(3) -0.0017(3) -0.0012(3) O1C 0.0313(12) 0.0586(15) 0.0453(17) -0.0131(12) 0.0037(10) -0.0088(10) O2C 0.0361(13) 0.0617(16) 0.0383(15) -0.0112(12) -0.0069(11) -0.0023(11) C1C 0.0311(15) 0.0329(15) 0.0272(18) -0.0047(12) 0.0005(12) -0.0008(11) C2C 0.0300(15) 0.0397(17) 0.036(2) -0.0094(14) -0.0004(13) -0.0051(12) C3C 0.0328(15) 0.0410(17) 0.0285(19) -0.0090(14) -0.0073(13) 0.0023(12) C4C 0.0297(16) 0.051(2) 0.067(3) -0.012(2) -0.0025(16) -0.0007(15) C5C 0.0360(18) 0.056(2) 0.053(3) -0.0150(19) -0.0124(16) -0.0016(16) Ni1 0.0417(5) 0.0520(6) 0.0579(7) -0.0204(5) -0.0099(4) -0.0034(4) C1 0.058(2) 0.051(2) 0.059(3) -0.015(2) -0.0095(19) 0.0026(18) N1 0.113(3) 0.056(2) 0.097(3) -0.036(2) -0.029(3) -0.003(2) C2 0.072(3) 0.050(2) 0.064(3) -0.015(2) -0.024(2) -0.0034(19) N2 0.146(4) 0.062(2) 0.078(3) -0.022(2) -0.035(3) -0.006(3) C1' 0.064(3) 0.062(3) 0.133(5) -0.035(3) 0.023(3) -0.008(2) C2' 0.080(4) 0.104(5) 0.247(10) -0.068(5) 0.065(5) -0.006(3) O1' 0.0528(17) 0.085(2) 0.087(3) -0.0253(19) -0.0120(16) 0.0105(15) O2' 0.0481(18) 0.098(3) 0.131(3) 0.028(2) 0.0129(19) 0.0107(17) C3' 0.065(3) 0.061(3) 0.090(4) -0.015(3) 0.004(2) 0.005(2) O3' 0.079(2) 0.0649(19) 0.083(2) -0.0234(17) -0.0293(18) 0.0297(16) _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 S1A C3A 1.744(3) . ? S1A C1A 1.746(3) . ? S2A C4A 1.736(3) . ? S2A C1A 1.745(3) . ? S3A C5A 1.742(3) . ? S3A C2A 1.747(3) . ? S4A C6A 1.737(3) . ? S4A C2A 1.749(3) . ? O1A C3A 1.352(4) . ? O1A C7A 1.454(5) . ? O2A C4A 1.353(4) . ? O2A C8A 1.453(4) . ? O3A C5A 1.350(4) . ? O3A C9A 1.447(4) . ? O4A C6A 1.355(4) . ? O4A C10A 1.444(4) . ? C1A C2A 1.366(4) . ? C3A C4A 1.354(5) . ? C5A C6A 1.348(5) . ? C7A C8A 1.508(7) . ? C9A C10A 1.524(6) . ? S1B C3B 1.734(3) . ? S1B C1B 1.746(3) . ? S2B C4B 1.739(3) . ? S2B C1B 1.746(3) . ? S3B C5B 1.732(3) . ? S3B C2B 1.749(3) . ? S4B C2B 1.745(3) . ? S4B C6B 1.745(3) . ? O1B C3B 1.352(4) . ? O1B C7B 1.442(4) . ? O2B C4B 1.356(4) . ? O2B C8B 1.440(4) . ? O3B C5B 1.352(4) . ? O3B C9B 1.444(4) . ? O4B C6B 1.356(4) . ? O4B C10B 1.444(5) . ? C1B C2B 1.366(4) . ? C3B C4B 1.353(5) . ? C5B C6B 1.359(5) . ? C7B C8B 1.516(6) . ? C9B C10B 1.509(6) . ? S1C C1C 1.740(3) . ? S1C C2C 1.745(3) . ? S2C C3C 1.732(3) . ? S2C C1C 1.744(3) . ? O1C C2C 1.353(4) . ? O1C C4C 1.445(5) . ? O2C C3C 1.352(4) . ? O2C C5C 1.449(4) . ? C1C C1C 1.375(6) 2_675 ? C2C C3C 1.348(5) . ? C4C C5C 1.512(6) . ? Ni1 C2 1.850(5) 2_567 ? Ni1 C2 1.850(5) . ? Ni1 C1 1.861(4) . ? Ni1 C1 1.861(4) 2_567 ? C1 N1 1.159(5) . ? C2 N2 1.150(6) . ? C1' C2' 1.403(8) 1_565 ? C1' O1' 1.433(6) . ? C2' O2' 1.371(7) 1_446 ? C2' C1' 1.403(8) 1_545 ? O2' C2' 1.371(7) 1_664 ? C3' O3' 1.415(5) . ? C3' C3' 1.484(9) 2_568 ? 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 C3A S1A C1A 93.71(16) . . ? C4A S2A C1A 93.85(15) . . ? C5A S3A C2A 93.81(15) . . ? C6A S4A C2A 93.75(15) . . ? C3A O1A C7A 109.8(3) . . ? C4A O2A C8A 109.7(3) . . ? C5A O3A C9A 109.9(3) . . ? C6A O4A C10A 109.6(3) . . ? C2A C1A S2A 121.2(3) . . ? C2A C1A S1A 121.9(3) . . ? S2A C1A S1A 116.89(16) . . ? C1A C2A S3A 122.0(3) . . ? C1A C2A S4A 121.3(3) . . ? S3A C2A S4A 116.68(16) . . ? O1A C3A C4A 125.1(3) . . ? O1A C3A S1A 117.3(3) . . ? C4A C3A S1A 117.6(2) . . ? O2A C4A C3A 125.0(3) . . ? O2A C4A S2A 117.0(3) . . ? C3A C4A S2A 117.9(2) . . ? C6A C5A O3A 125.6(3) . . ? C6A C5A S3A 117.7(2) . . ? O3A C5A S3A 116.8(2) . . ? C5A C6A O4A 124.9(3) . . ? C5A C6A S4A 118.1(2) . . ? O4A C6A S4A 117.0(3) . . ? O1A C7A C8A 111.3(3) . . ? O2A C8A C7A 110.3(3) . . ? O3A C9A C10A 110.4(3) . . ? O4A C10A C9A 110.9(3) . . ? C3B S1B C1B 93.86(15) . . ? C4B S2B C1B 93.73(15) . . ? C5B S3B C2B 94.03(16) . . ? C2B S4B C6B 93.76(15) . . ? C3B O1B C7B 110.0(3) . . ? C4B O2B C8B 109.8(3) . . ? C5B O3B C9B 110.3(3) . . ? C6B O4B C10B 109.9(3) . . ? C2B C1B S2B 121.6(3) . . ? C2B C1B S1B 121.7(3) . . ? S2B C1B S1B 116.76(16) . . ? C1B C2B S4B 121.8(3) . . ? C1B C2B S3B 121.4(3) . . ? S4B C2B S3B 116.77(16) . . ? O1B C3B C4B 124.3(3) . . ? O1B C3B S1B 117.8(3) . . ? C4B C3B S1B 117.9(2) . . ? C3B C4B O2B 125.6(3) . . ? C3B C4B S2B 117.8(2) . . ? O2B C4B S2B 116.6(2) . . ? O3B C5B C6B 124.7(3) . . ? O3B C5B S3B 117.5(3) . . ? C6B C5B S3B 117.8(2) . . ? O4B C6B C5B 124.9(3) . . ? O4B C6B S4B 117.6(3) . . ? C5B C6B S4B 117.6(2) . . ? O1B C7B C8B 111.1(3) . . ? O2B C8B C7B 110.8(3) . . ? O3B C9B C10B 111.1(3) . . ? O4B C10B C9B 110.9(3) . . ? C1C S1C C2C 93.54(16) . . ? C3C S2C C1C 93.68(15) . . ? C2C O1C C4C 109.7(3) . . ? C3C O2C C5C 110.0(3) . . ? C1C C1C S1C 121.8(3) 2_675 . ? C1C C1C S2C 121.1(3) 2_675 . ? S1C C1C S2C 117.09(17) . . ? C3C C2C O1C 125.5(3) . . ? C3C C2C S1C 117.6(2) . . ? O1C C2C S1C 117.0(3) . . ? C2C C3C O2C 124.9(3) . . ? C2C C3C S2C 118.1(2) . . ? O2C C3C S2C 117.0(3) . . ? O1C C4C C5C 111.7(3) . . ? O2C C5C C4C 110.4(3) . . ? C2 Ni1 C2 180.000(2) 2_567 . ? C2 Ni1 C1 91.04(18) 2_567 . ? C2 Ni1 C1 88.96(18) . . ? C2 Ni1 C1 88.96(18) 2_567 2_567 ? C2 Ni1 C1 91.04(18) . 2_567 ? C1 Ni1 C1 180.000(1) . 2_567 ? N1 C1 Ni1 177.3(4) . . ? N2 C2 Ni1 177.6(4) . . ? C2' C1' O1' 113.8(5) 1_565 . ? O2' C2' C1' 120.2(6) 1_446 1_545 ? O3' C3' C3' 111.2(5) . 2_568 ? _diffrn_measured_fraction_theta_max 0.941 _diffrn_reflns_theta_full 80.47 _diffrn_measured_fraction_theta_full 0.941 _refine_diff_density_max 1.799 _refine_diff_density_min -0.574 _refine_diff_density_rms 0.193