# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1779 data_mf196fac _publ_contact_letter ; please find in the following the CIF file corresponding to two structures described in a Communication to be considered for Chem Commun. entitled: [Ni(edt-CN)2]-, a novel paramagnetic nickel dithiolene complex analog of Ni(mnt)2- with two cyano groups only. by M. Fourmigu and J. N. Bertran which has been sent by air mail the 29th of July to the Cambridge Office With best regards Marc Fourmigue ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis(tetraphenylphosphonium) bis(1-cyano-1,2-dithioethylene)nickelate ; _chemical_name_common '(PPh4)2(Ni(edt-CN)2)' _chemical_melting_point ? _chemical_formula_moiety '(C24 H20 P)2, C6 H2 N2 Ni S4' _chemical_formula_sum 'C54 H42 N2 Ni P2 S4' _chemical_formula_weight 967.79 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' 'P' 'P' 0.1023 0.0942 '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 20.523(4) _cell_length_b 11.220(2) _cell_length_c 21.304(4) _cell_angle_alpha 90.00 _cell_angle_beta 107.33(3) _cell_angle_gamma 90.00 _cell_volume 4682.9(16) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.9 _exptl_crystal_description 'plate' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.373 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2008 _exptl_absorpt_coefficient_mu 0.701 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.7837 _exptl_absorpt_correction_T_max 0.9471 _exptl_absorpt_process_details 'FACEIT, Stoe IPDS' _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 'area_detector' _diffrn_measurement_device_type 'Stoe-IPDS' _diffrn_measurement_method 'oscillation, phin incr. 1.1 deg' _diffrn_detector_area_resol_mean 6.66 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35954 _diffrn_reflns_av_R_equivalents 0.0612 _diffrn_reflns_av_sigmaI/netI 0.0577 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 25.95 _reflns_number_total 9096 _reflns_number_gt 5396 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'EXPOSE, Stoe-IPDS' _computing_cell_refinement 'CELL, Stoe-IPDS' _computing_data_reduction 'INTEGRATE, Stoe-IPDS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0724P)^2^+3.0661P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9096 _refine_ls_number_parameters 571 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0996 _refine_ls_R_factor_gt 0.0581 _refine_ls_wR_factor_ref 0.1628 _refine_ls_wR_factor_gt 0.1491 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _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 Ni1 Ni 0.5000 0.0000 0.0000 0.0407(2) Uani 1 2 d S . . S1 S 0.50077(7) -0.19483(12) 0.00592(6) 0.0527(3) Uani 1 1 d . . . S2 S 0.52947(6) -0.00340(13) -0.09046(6) 0.0522(3) Uani 1 1 d . . . N1 N 0.5231(3) -0.4582(5) -0.0960(2) 0.0706(13) Uani 1 1 d . . . C3 C 0.5208(3) -0.3596(5) -0.0823(2) 0.0553(12) Uani 1 1 d . . . C1 C 0.5185(2) -0.2362(5) -0.0668(2) 0.0478(11) Uani 1 1 d . . . C2 C 0.5311(2) -0.1529(5) -0.1070(2) 0.0541(12) Uani 1 1 d . . . H2 H 0.5410 -0.1770 -0.1449 0.065 Uiso 1 1 calc R . . Ni2 Ni 0.0000 0.5000 0.0000 0.0464(2) Uani 1 2 d S . . S3 S -0.09925(7) 0.50516(13) 0.01855(6) 0.0565(3) Uani 1 1 d . . . S4 S 0.00502(6) 0.30588(13) 0.00993(7) 0.0590(4) Uani 1 1 d . . . N2 N -0.1011(3) 0.0505(6) 0.0366(3) 0.0815(15) Uani 1 1 d . . . C4 C -0.1175(3) 0.3570(5) 0.0263(2) 0.0563(13) Uani 1 1 d . . . H4 H -0.1588 0.3363 0.0331 0.068 Uiso 1 1 calc R . . C5 C -0.0734(2) 0.2708(5) 0.0227(2) 0.0553(13) Uani 1 1 d . . . C6 C -0.0889(3) 0.1488(6) 0.0303(3) 0.0632(14) Uani 1 1 d . . . P1 P 0.26886(5) 0.48238(11) 0.18070(5) 0.0385(3) Uani 1 1 d . . . C7 C 0.3401(2) 0.4656(4) 0.2529(2) 0.0402(10) Uani 1 1 d . . . C8 C 0.3605(2) 0.3523(5) 0.2789(2) 0.0530(12) Uani 1 1 d . . . H8 H 0.3411 0.2844 0.2557 0.064 Uiso 1 1 calc R . . C9 C 0.4101(3) 0.3419(5) 0.3396(3) 0.0631(14) Uani 1 1 d . . . H9 H 0.4236 0.2668 0.3572 0.076 Uiso 1 1 calc R . . C10 C 0.4390(2) 0.4421(6) 0.3735(3) 0.0604(14) Uani 1 1 d . . . H10 H 0.4720 0.4348 0.4141 0.073 Uiso 1 1 calc R . . C11 C 0.4194(2) 0.5529(5) 0.3477(2) 0.0573(13) Uani 1 1 d . . . H11 H 0.4394 0.6203 0.3710 0.069 Uiso 1 1 calc R . . C12 C 0.3703(2) 0.5654(5) 0.2874(2) 0.0517(12) Uani 1 1 d . . . H12 H 0.3577 0.6410 0.2702 0.062 Uiso 1 1 calc R . . C13 C 0.2853(2) 0.6137(4) 0.1393(2) 0.0414(10) Uani 1 1 d . . . C14 C 0.2377(2) 0.7034(5) 0.1202(2) 0.0513(12) Uani 1 1 d . . . H14 H 0.1954 0.6957 0.1272 0.062 Uiso 1 1 calc R . . C15 C 0.2527(3) 0.8047(5) 0.0905(3) 0.0661(15) Uani 1 1 d . . . H15 H 0.2208 0.8657 0.0781 0.079 Uiso 1 1 calc R . . C16 C 0.3149(3) 0.8153(6) 0.0793(2) 0.0671(16) Uani 1 1 d . . . H16 H 0.3247 0.8833 0.0588 0.081 Uiso 1 1 calc R . . C17 C 0.3627(3) 0.7265(6) 0.0979(3) 0.0684(16) Uani 1 1 d . . . H17 H 0.4048 0.7346 0.0902 0.082 Uiso 1 1 calc R . . C18 C 0.3486(3) 0.6260(5) 0.1277(3) 0.0574(13) Uani 1 1 d . . . H18 H 0.3810 0.5658 0.1402 0.069 Uiso 1 1 calc R . . C19 C 0.1932(2) 0.5024(4) 0.20655(18) 0.0377(9) Uani 1 1 d . . . C20 C 0.1292(2) 0.5090(5) 0.1593(2) 0.0499(11) Uani 1 1 d . . . H20 H 0.1255 0.5038 0.1148 0.060 Uiso 1 1 calc R . . C21 C 0.0718(2) 0.5233(5) 0.1792(2) 0.0607(14) Uani 1 1 d . . . H21 H 0.0291 0.5292 0.1480 0.073 Uiso 1 1 calc R . . C22 C 0.0773(3) 0.5289(5) 0.2451(3) 0.0583(14) Uani 1 1 d . . . H22 H 0.0381 0.5352 0.2583 0.070 Uiso 1 1 calc R . . C23 C 0.1402(3) 0.5252(5) 0.2914(2) 0.0600(14) Uani 1 1 d . . . H23 H 0.1435 0.5321 0.3357 0.072 Uiso 1 1 calc R . . C24 C 0.1990(2) 0.5113(5) 0.2727(2) 0.0537(12) Uani 1 1 d . . . H24 H 0.2416 0.5080 0.3041 0.064 Uiso 1 1 calc R . . C25 C 0.2585(2) 0.3551(4) 0.1273(2) 0.0425(10) Uani 1 1 d . . . C26 C 0.3040(3) 0.3321(6) 0.0938(3) 0.087(2) Uani 1 1 d . . . H26 H 0.3423 0.3804 0.1007 0.105 Uiso 1 1 calc R . . C27 C 0.2947(4) 0.2379(7) 0.0496(4) 0.095(2) Uani 1 1 d . . . H27 H 0.3273 0.2215 0.0285 0.114 Uiso 1 1 calc R . . C28 C 0.2373(3) 0.1701(5) 0.0374(3) 0.0666(15) Uani 1 1 d . . . H28 H 0.2295 0.1098 0.0061 0.080 Uiso 1 1 calc R . . C29 C 0.1920(3) 0.1902(5) 0.0707(3) 0.0758(17) Uani 1 1 d . . . H29 H 0.1535 0.1422 0.0631 0.091 Uiso 1 1 calc R . . C30 C 0.2024(3) 0.2810(5) 0.1158(3) 0.0706(16) Uani 1 1 d . . . H30 H 0.1711 0.2929 0.1390 0.085 Uiso 1 1 calc R . . P2 P 0.82262(5) 0.51104(11) 0.23014(5) 0.0405(3) Uani 1 1 d . . . C31 C 0.7932(2) 0.5275(4) 0.3014(2) 0.0419(10) Uani 1 1 d . . . C32 C 0.8395(2) 0.5289(5) 0.3638(2) 0.0506(12) Uani 1 1 d . . . H32 H 0.8860 0.5200 0.3694 0.061 Uiso 1 1 calc R . . C33 C 0.8160(2) 0.5437(5) 0.4173(2) 0.0568(13) Uani 1 1 d . . . H33 H 0.8467 0.5420 0.4594 0.068 Uiso 1 1 calc R . . C34 C 0.7478(3) 0.5609(5) 0.4093(2) 0.0552(13) Uani 1 1 d . . . H34 H 0.7328 0.5732 0.4459 0.066 Uiso 1 1 calc R . . C35 C 0.7018(2) 0.5599(5) 0.3475(2) 0.0536(12) Uani 1 1 d . . . H35 H 0.6556 0.5704 0.3426 0.064 Uiso 1 1 calc R . . C36 C 0.7233(2) 0.5436(5) 0.2925(2) 0.0487(12) Uani 1 1 d . . . H36 H 0.6921 0.5433 0.2507 0.058 Uiso 1 1 calc R . . C37 C 0.7506(2) 0.4906(4) 0.15875(19) 0.0420(10) Uani 1 1 d . . . C38 C 0.7294(3) 0.3769(5) 0.1358(3) 0.0589(14) Uani 1 1 d . . . H38 H 0.7545 0.3104 0.1550 0.071 Uiso 1 1 calc R . . C39 C 0.6703(3) 0.3642(6) 0.0838(3) 0.0713(16) Uani 1 1 d . . . H39 H 0.6560 0.2884 0.0680 0.086 Uiso 1 1 calc R . . C40 C 0.6331(3) 0.4602(6) 0.0555(3) 0.0703(17) Uani 1 1 d . . . H40 H 0.5932 0.4498 0.0210 0.084 Uiso 1 1 calc R . . C41 C 0.6539(3) 0.5721(6) 0.0776(3) 0.0672(16) Uani 1 1 d . . . H41 H 0.6284 0.6378 0.0577 0.081 Uiso 1 1 calc R . . C42 C 0.7128(3) 0.5884(5) 0.1294(3) 0.0630(14) Uani 1 1 d . . . H42 H 0.7269 0.6648 0.1443 0.076 Uiso 1 1 calc R . . C43 C 0.8651(2) 0.6457(4) 0.2171(2) 0.0457(11) Uani 1 1 d . . . C44 C 0.8863(3) 0.7306(5) 0.2657(2) 0.0561(13) Uani 1 1 d . . . H44 H 0.8791 0.7191 0.3064 0.067 Uiso 1 1 calc R . . C45 C 0.9186(3) 0.8334(5) 0.2539(3) 0.0668(15) Uani 1 1 d . . . H45 H 0.9328 0.8910 0.2865 0.080 Uiso 1 1 calc R . . C46 C 0.9294(3) 0.8496(6) 0.1939(3) 0.0714(16) Uani 1 1 d . . . H46 H 0.9513 0.9181 0.1862 0.086 Uiso 1 1 calc R . . C47 C 0.9082(3) 0.7666(6) 0.1457(3) 0.0769(17) Uani 1 1 d . . . H47 H 0.9160 0.7783 0.1053 0.092 Uiso 1 1 calc R . . C48 C 0.8753(3) 0.6649(5) 0.1565(3) 0.0663(15) Uani 1 1 d . . . H48 H 0.8599 0.6092 0.1230 0.080 Uiso 1 1 calc R . . C49 C 0.8793(2) 0.3854(4) 0.2417(2) 0.0429(10) Uani 1 1 d . . . C50 C 0.8884(3) 0.3070(5) 0.2935(3) 0.0568(13) Uani 1 1 d . . . H50 H 0.8641 0.3173 0.3237 0.068 Uiso 1 1 calc R . . C51 C 0.9338(3) 0.2128(5) 0.3007(3) 0.0645(15) Uani 1 1 d . . . H51 H 0.9398 0.1604 0.3358 0.077 Uiso 1 1 calc R . . C52 C 0.9694(3) 0.1963(5) 0.2574(3) 0.0619(14) Uani 1 1 d . . . H52 H 1.0001 0.1334 0.2631 0.074 Uiso 1 1 calc R . . C53 C 0.9604(3) 0.2725(5) 0.2045(3) 0.0671(15) Uani 1 1 d . . . H53 H 0.9842 0.2598 0.1742 0.081 Uiso 1 1 calc R . . C54 C 0.9159(3) 0.3678(5) 0.1968(2) 0.0591(14) Uani 1 1 d . . . H54 H 0.9104 0.4200 0.1617 0.071 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 Ni1 0.0323(4) 0.0493(5) 0.0391(4) 0.0040(4) 0.0086(3) -0.0048(4) S1 0.0620(7) 0.0508(8) 0.0482(7) 0.0074(6) 0.0207(5) -0.0002(6) S2 0.0542(6) 0.0571(8) 0.0498(6) 0.0038(6) 0.0226(5) -0.0092(6) N1 0.080(3) 0.062(3) 0.066(3) -0.003(3) 0.017(2) 0.006(3) C3 0.057(3) 0.058(4) 0.051(3) 0.004(3) 0.016(2) 0.004(3) C1 0.038(2) 0.057(3) 0.049(3) 0.003(2) 0.013(2) 0.000(2) C2 0.051(3) 0.068(4) 0.048(3) -0.004(3) 0.021(2) -0.005(2) Ni2 0.0477(4) 0.0556(5) 0.0324(4) -0.0056(4) 0.0064(3) 0.0000(4) S3 0.0600(7) 0.0655(9) 0.0469(6) -0.0042(7) 0.0202(5) 0.0062(7) S4 0.0496(7) 0.0579(9) 0.0668(9) -0.0031(7) 0.0130(6) -0.0010(6) N2 0.071(3) 0.074(4) 0.102(4) 0.004(3) 0.028(3) -0.006(3) C4 0.057(3) 0.069(4) 0.041(3) -0.003(2) 0.011(2) -0.005(3) C5 0.052(3) 0.066(4) 0.045(3) -0.005(3) 0.009(2) -0.005(3) C6 0.049(3) 0.073(4) 0.066(3) -0.001(3) 0.014(2) -0.002(3) P1 0.0383(5) 0.0410(7) 0.0374(5) -0.0002(5) 0.0132(4) -0.0016(5) C7 0.036(2) 0.043(3) 0.045(2) 0.000(2) 0.0163(18) -0.0001(18) C8 0.046(3) 0.051(3) 0.057(3) 0.001(2) 0.008(2) -0.002(2) C9 0.050(3) 0.064(4) 0.067(3) 0.014(3) 0.005(2) 0.002(3) C10 0.043(3) 0.084(4) 0.052(3) 0.004(3) 0.011(2) -0.006(3) C11 0.047(3) 0.073(4) 0.050(3) -0.009(3) 0.012(2) -0.011(3) C12 0.052(3) 0.049(3) 0.053(3) 0.001(2) 0.014(2) 0.000(2) C13 0.042(2) 0.045(3) 0.039(2) -0.001(2) 0.0140(18) -0.0039(19) C14 0.048(3) 0.052(3) 0.053(3) 0.003(2) 0.014(2) -0.004(2) C15 0.067(3) 0.056(4) 0.064(3) 0.013(3) 0.003(3) -0.004(3) C16 0.082(4) 0.067(4) 0.047(3) 0.009(3) 0.013(3) -0.030(3) C17 0.066(3) 0.076(4) 0.073(4) 0.001(3) 0.036(3) -0.021(3) C18 0.056(3) 0.056(3) 0.068(3) 0.007(3) 0.031(3) 0.001(2) C19 0.042(2) 0.042(2) 0.0314(19) 0.002(2) 0.0144(16) -0.004(2) C20 0.048(2) 0.068(3) 0.034(2) -0.002(2) 0.0125(18) -0.003(2) C21 0.039(2) 0.091(4) 0.050(3) -0.006(3) 0.010(2) -0.005(3) C22 0.048(3) 0.074(4) 0.058(3) -0.002(3) 0.025(2) -0.001(2) C23 0.060(3) 0.084(4) 0.040(2) -0.002(3) 0.021(2) 0.005(3) C24 0.046(2) 0.075(4) 0.040(2) 0.000(3) 0.0128(19) 0.001(2) C25 0.040(2) 0.046(3) 0.040(2) -0.005(2) 0.0096(18) -0.002(2) C26 0.064(3) 0.100(5) 0.115(5) -0.057(4) 0.054(4) -0.034(3) C27 0.096(5) 0.101(6) 0.114(5) -0.053(5) 0.071(4) -0.030(4) C28 0.079(4) 0.057(4) 0.063(3) -0.022(3) 0.020(3) -0.001(3) C29 0.075(4) 0.056(4) 0.102(5) -0.030(3) 0.036(3) -0.024(3) C30 0.082(4) 0.060(4) 0.088(4) -0.020(3) 0.054(3) -0.021(3) P2 0.0385(5) 0.0468(7) 0.0364(5) -0.0025(5) 0.0112(4) 0.0020(5) C31 0.035(2) 0.050(3) 0.042(2) -0.004(2) 0.0138(18) -0.0003(18) C32 0.035(2) 0.072(4) 0.045(2) -0.003(2) 0.0112(19) 0.000(2) C33 0.049(3) 0.086(4) 0.032(2) -0.002(2) 0.007(2) 0.004(3) C34 0.060(3) 0.066(3) 0.046(3) 0.000(2) 0.026(2) -0.001(3) C35 0.041(2) 0.066(3) 0.059(3) -0.003(3) 0.023(2) -0.002(2) C36 0.035(2) 0.062(3) 0.045(2) 0.010(2) 0.0052(19) 0.005(2) C37 0.046(2) 0.047(3) 0.032(2) 0.000(2) 0.0110(17) 0.004(2) C38 0.058(3) 0.050(3) 0.057(3) 0.002(3) -0.001(2) 0.002(2) C39 0.067(3) 0.068(4) 0.062(3) -0.001(3) -0.007(3) -0.010(3) C40 0.050(3) 0.101(5) 0.048(3) 0.005(3) -0.003(2) -0.003(3) C41 0.056(3) 0.085(5) 0.048(3) 0.011(3) -0.005(2) 0.018(3) C42 0.068(3) 0.057(4) 0.055(3) -0.005(3) 0.006(3) 0.007(3) C43 0.045(2) 0.044(3) 0.050(3) -0.004(2) 0.017(2) 0.004(2) C44 0.060(3) 0.058(3) 0.049(3) -0.003(3) 0.014(2) -0.002(3) C45 0.066(3) 0.057(4) 0.070(4) -0.012(3) 0.010(3) -0.009(3) C46 0.068(4) 0.056(4) 0.097(5) -0.002(3) 0.035(3) -0.007(3) C47 0.098(4) 0.072(4) 0.080(4) 0.004(4) 0.056(4) -0.006(4) C48 0.086(4) 0.064(4) 0.061(3) -0.012(3) 0.041(3) -0.011(3) C49 0.037(2) 0.048(3) 0.043(2) -0.003(2) 0.0101(18) 0.0000(19) C50 0.059(3) 0.056(3) 0.059(3) 0.003(3) 0.023(2) 0.007(2) C51 0.067(3) 0.053(3) 0.065(3) 0.011(3) 0.007(3) 0.008(3) C52 0.049(3) 0.057(4) 0.072(4) -0.008(3) 0.006(3) 0.011(2) C53 0.057(3) 0.076(4) 0.071(4) -0.012(3) 0.023(3) 0.018(3) C54 0.060(3) 0.069(4) 0.049(3) 0.002(3) 0.018(2) 0.013(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 Ni1 S2 2.1852(12) . ? Ni1 S2 2.1854(12) 3_655 ? Ni1 S1 2.1894(14) . ? Ni1 S1 2.1894(14) 3_655 ? S1 C1 1.756(5) . ? S2 C2 1.716(6) . ? N1 C3 1.149(7) . ? C3 C1 1.426(8) . ? C1 C2 1.343(7) . ? Ni2 S4 2.1877(15) 3_565 ? Ni2 S4 2.1877(15) . ? Ni2 S3 2.1880(13) 3_565 ? Ni2 S3 2.1881(13) . ? S3 C4 1.723(6) . ? S4 C5 1.755(5) . ? N2 C6 1.147(7) . ? C4 C5 1.342(7) . ? C5 C6 1.425(8) . ? P1 C7 1.788(4) . ? P1 C25 1.798(5) . ? P1 C13 1.800(5) . ? P1 C19 1.809(4) . ? C7 C12 1.381(7) . ? C7 C8 1.401(7) . ? C8 C9 1.392(7) . ? C9 C10 1.373(8) . ? C10 C11 1.369(8) . ? C11 C12 1.383(7) . ? C13 C14 1.377(7) . ? C13 C18 1.399(6) . ? C14 C15 1.379(7) . ? C15 C16 1.371(8) . ? C16 C17 1.372(8) . ? C17 C18 1.366(8) . ? C19 C24 1.382(6) . ? C19 C20 1.399(6) . ? C20 C21 1.376(6) . ? C21 C22 1.375(7) . ? C22 C23 1.373(7) . ? C23 C24 1.388(7) . ? C25 C26 1.359(7) . ? C25 C30 1.381(7) . ? C26 C27 1.391(8) . ? C27 C28 1.360(8) . ? C28 C29 1.345(8) . ? C29 C30 1.374(8) . ? P2 C37 1.792(4) . ? P2 C49 1.797(5) . ? P2 C31 1.802(4) . ? P2 C43 1.807(5) . ? C31 C32 1.386(6) . ? C31 C36 1.402(6) . ? C32 C33 1.374(6) . ? C33 C34 1.372(7) . ? C34 C35 1.374(7) . ? C35 C36 1.381(7) . ? C37 C42 1.381(7) . ? C37 C38 1.389(7) . ? C38 C39 1.385(7) . ? C39 C40 1.354(8) . ? C40 C41 1.364(8) . ? C41 C42 1.385(7) . ? C43 C44 1.379(7) . ? C43 C48 1.385(7) . ? C44 C45 1.390(8) . ? C45 C46 1.372(8) . ? C46 C47 1.359(8) . ? C47 C48 1.379(8) . ? C49 C50 1.381(7) . ? C49 C54 1.394(7) . ? C50 C51 1.387(7) . ? C51 C52 1.349(8) . ? C52 C53 1.382(8) . ? C53 C54 1.383(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 S2 Ni1 S2 180.0 . 3_655 ? S2 Ni1 S1 91.96(5) . . ? S2 Ni1 S1 88.04(5) 3_655 . ? S2 Ni1 S1 88.05(5) . 3_655 ? S2 Ni1 S1 91.95(5) 3_655 3_655 ? S1 Ni1 S1 179.996(1) . 3_655 ? C1 S1 Ni1 102.31(18) . . ? C2 S2 Ni1 103.01(17) . . ? N1 C3 C1 178.3(6) . . ? C2 C1 C3 120.2(5) . . ? C2 C1 S1 120.5(4) . . ? C3 C1 S1 119.4(4) . . ? C1 C2 S2 122.1(4) . . ? S4 Ni2 S4 180.0 3_565 . ? S4 Ni2 S3 91.63(5) 3_565 3_565 ? S4 Ni2 S3 88.37(5) . 3_565 ? S4 Ni2 S3 88.37(5) 3_565 . ? S4 Ni2 S3 91.63(5) . . ? S3 Ni2 S3 180.0 3_565 . ? C4 S3 Ni2 103.44(19) . . ? C5 S4 Ni2 102.7(2) . . ? C5 C4 S3 121.3(4) . . ? C4 C5 C6 120.5(5) . . ? C4 C5 S4 120.8(4) . . ? C6 C5 S4 118.7(4) . . ? N2 C6 C5 179.7(6) . . ? C7 P1 C25 111.9(2) . . ? C7 P1 C13 106.4(2) . . ? C25 P1 C13 110.2(2) . . ? C7 P1 C19 107.90(19) . . ? C25 P1 C19 109.9(2) . . ? C13 P1 C19 110.5(2) . . ? C12 C7 C8 119.4(4) . . ? C12 C7 P1 119.7(4) . . ? C8 C7 P1 120.5(3) . . ? C9 C8 C7 119.6(5) . . ? C10 C9 C8 120.1(5) . . ? C11 C10 C9 120.3(5) . . ? C10 C11 C12 120.7(5) . . ? C7 C12 C11 120.0(5) . . ? C14 C13 C18 119.3(4) . . ? C14 C13 P1 121.6(3) . . ? C18 C13 P1 119.1(4) . . ? C13 C14 C15 120.2(5) . . ? C16 C15 C14 119.8(5) . . ? C15 C16 C17 120.6(5) . . ? C18 C17 C16 120.1(5) . . ? C17 C18 C13 120.0(5) . . ? C24 C19 C20 120.5(4) . . ? C24 C19 P1 119.9(3) . . ? C20 C19 P1 119.7(3) . . ? C21 C20 C19 119.5(4) . . ? C22 C21 C20 120.1(4) . . ? C23 C22 C21 120.4(5) . . ? C22 C23 C24 120.6(4) . . ? C19 C24 C23 118.9(4) . . ? C26 C25 C30 117.3(5) . . ? C26 C25 P1 120.8(4) . . ? C30 C25 P1 121.8(4) . . ? C25 C26 C27 121.5(5) . . ? C28 C27 C26 119.4(6) . . ? C29 C28 C27 120.1(5) . . ? C28 C29 C30 120.3(5) . . ? C29 C30 C25 121.2(5) . . ? C37 P2 C49 110.6(2) . . ? C37 P2 C31 109.18(19) . . ? C49 P2 C31 109.3(2) . . ? C37 P2 C43 106.9(2) . . ? C49 P2 C43 110.8(2) . . ? C31 P2 C43 110.0(2) . . ? C32 C31 C36 120.6(4) . . ? C32 C31 P2 120.2(3) . . ? C36 C31 P2 119.1(3) . . ? C33 C32 C31 119.2(4) . . ? C34 C33 C32 120.7(4) . . ? C33 C34 C35 120.2(4) . . ? C34 C35 C36 120.7(4) . . ? C35 C36 C31 118.4(4) . . ? C42 C37 C38 119.7(4) . . ? C42 C37 P2 119.5(4) . . ? C38 C37 P2 120.6(4) . . ? C39 C38 C37 118.9(5) . . ? C40 C39 C38 121.2(6) . . ? C39 C40 C41 120.1(5) . . ? C40 C41 C42 120.3(5) . . ? C37 C42 C41 119.7(5) . . ? C44 C43 C48 119.4(5) . . ? C44 C43 P2 121.4(4) . . ? C48 C43 P2 119.2(4) . . ? C43 C44 C45 119.9(5) . . ? C46 C45 C44 119.8(5) . . ? C47 C46 C45 120.6(6) . . ? C46 C47 C48 120.2(6) . . ? C47 C48 C43 120.1(5) . . ? C50 C49 C54 119.1(4) . . ? C50 C49 P2 122.5(4) . . ? C54 C49 P2 118.4(4) . . ? C49 C50 C51 120.0(5) . . ? C52 C51 C50 120.8(5) . . ? C51 C52 C53 120.3(5) . . ? C52 C53 C54 119.9(5) . . ? C53 C54 C49 120.0(5) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.95 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.643 _refine_diff_density_min -0.265 _refine_diff_density_rms 0.066 #===END data_mf207psi _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis(2-cyano-1,2-ethylenedithiolate)Nickelate, tetraphenylphosphonium ; _chemical_name_common 'PPh4, Ni(edt-CN)2' _chemical_melting_point ? _chemical_formula_moiety 'C24 H20 P, C6 H2 N2 Ni S4' _chemical_formula_sum 'C30 H22 N2 Ni P S4' _chemical_formula_weight 628.42 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' 'P' 'P' 0.1023 0.0942 '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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.3940(12) _cell_length_b 11.5100(11) _cell_length_c 12.8262(13) _cell_angle_alpha 64.264(10) _cell_angle_beta 72.777(12) _cell_angle_gamma 83.074(12) _cell_volume 1447.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7773 _cell_measurement_theta_min 1.85 _cell_measurement_theta_max 25.8 _exptl_crystal_description ? _exptl_crystal_colour brown _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.442 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 646 _exptl_absorpt_coefficient_mu 1.037 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.82077 _exptl_absorpt_correction_T_max 0.92026 _exptl_absorpt_process_details 'SHELXL PSI-SCAN' _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 'Stoe-IPDS' _diffrn_measurement_method 'oscillation, phi incr. 1.8' _diffrn_detector_area_resol_mean 6.66 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14189 _diffrn_reflns_av_R_equivalents 0.0427 _diffrn_reflns_av_sigmaI/netI 0.0514 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 25.97 _reflns_number_total 5232 _reflns_number_gt 3582 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'EXPOSE, Stoe-IPDS' _computing_cell_refinement 'CELL, Stoe-IPDS' _computing_data_reduction 'INTEGRATE, Stoe-IPDS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0347P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5232 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0608 _refine_ls_R_factor_gt 0.0343 _refine_ls_wR_factor_ref 0.0713 _refine_ls_wR_factor_gt 0.0655 _refine_ls_goodness_of_fit_ref 0.893 _refine_ls_restrained_S_all 0.893 _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 Ni1 Ni 0.62099(3) 0.61272(3) 0.72517(3) 0.04443(10) Uani 1 1 d . . . P1 P 0.25415(5) 1.09642(6) 0.80097(5) 0.03516(15) Uani 1 1 d . . . S1 S 0.77945(6) 0.73527(7) 0.65267(6) 0.05322(19) Uani 1 1 d . . . S2 S 0.70257(6) 0.50973(8) 0.61621(7) 0.0591(2) Uani 1 1 d . . . S3 S 0.54285(7) 0.71108(7) 0.83878(7) 0.0593(2) Uani 1 1 d . . . S4 S 0.46334(7) 0.48801(8) 0.80120(6) 0.0588(2) Uani 1 1 d . . . N1 N 1.0923(3) 0.7851(3) 0.4500(2) 0.0888(9) Uani 1 1 d . . . N2 N 0.1645(3) 0.4189(3) 1.0361(2) 0.0792(8) Uani 1 1 d . . . C1 C 0.8779(2) 0.6785(3) 0.5530(2) 0.0492(7) Uani 1 1 d . . . C2 C 0.8430(2) 0.5823(3) 0.5362(2) 0.0543(7) Uani 1 1 d . . . H2 H 0.8955 0.5549 0.4805 0.065 Uiso 1 1 calc R . . C3 C 0.9971(3) 0.7374(3) 0.4942(2) 0.0612(8) Uani 1 1 d . . . C4 C 0.3697(2) 0.5373(3) 0.9081(2) 0.0505(7) Uani 1 1 d . . . C5 C 0.4058(2) 0.6338(3) 0.9238(2) 0.0548(7) Uani 1 1 d . . . H5 H 0.3553 0.6590 0.9820 0.066 Uiso 1 1 calc R . . C6 C 0.2562(3) 0.4708(3) 0.9802(2) 0.0570(7) Uani 1 1 d . . . C7 C 0.2843(2) 1.0289(2) 0.94604(19) 0.0372(5) Uani 1 1 d . . . C8 C 0.3705(2) 0.9324(3) 0.9699(2) 0.0484(6) Uani 1 1 d . . . H8 H 0.4169 0.9088 0.9092 0.058 Uiso 1 1 calc R . . C9 C 0.3878(3) 0.8711(3) 1.0835(3) 0.0605(8) Uani 1 1 d . . . H9 H 0.4450 0.8054 1.0994 0.073 Uiso 1 1 calc R . . C10 C 0.3210(3) 0.9066(3) 1.1726(2) 0.0669(9) Uani 1 1 d . . . H10 H 0.3321 0.8645 1.2493 0.080 Uiso 1 1 calc R . . C11 C 0.2383(3) 1.0038(4) 1.1486(2) 0.0730(10) Uani 1 1 d . . . H11 H 0.1948 1.0290 1.2090 0.088 Uiso 1 1 calc R . . C12 C 0.2180(3) 1.0654(3) 1.0364(2) 0.0592(8) Uani 1 1 d . . . H12 H 0.1603 1.1308 1.0215 0.071 Uiso 1 1 calc R . . C13 C 0.3947(2) 1.1463(2) 0.6822(2) 0.0382(6) Uani 1 1 d . . . C14 C 0.4371(3) 1.2716(3) 0.6228(2) 0.0574(7) Uani 1 1 d . . . H14 H 0.3916 1.3356 0.6424 0.069 Uiso 1 1 calc R . . C15 C 0.5477(3) 1.3025(3) 0.5340(3) 0.0685(9) Uani 1 1 d . . . H15 H 0.5755 1.3876 0.4940 0.082 Uiso 1 1 calc R . . C16 C 0.6157(3) 1.2114(3) 0.5043(2) 0.0648(9) Uani 1 1 d . . . H16 H 0.6895 1.2337 0.4440 0.078 Uiso 1 1 calc R . . C17 C 0.5755(3) 1.0861(3) 0.5634(3) 0.0718(9) Uani 1 1 d . . . H17 H 0.6228 1.0229 0.5440 0.086 Uiso 1 1 calc R . . C18 C 0.4652(2) 1.0527(3) 0.6517(2) 0.0585(8) Uani 1 1 d . . . H18 H 0.4381 0.9674 0.6909 0.070 Uiso 1 1 calc R . . C19 C 0.1852(2) 0.9748(2) 0.78544(19) 0.0363(5) Uani 1 1 d . . . C20 C 0.1357(2) 0.8626(2) 0.8829(2) 0.0440(6) Uani 1 1 d . . . H20 H 0.1435 0.8448 0.9586 0.053 Uiso 1 1 calc R . . C21 C 0.0744(2) 0.7767(3) 0.8680(3) 0.0542(7) Uani 1 1 d . . . H21 H 0.0420 0.7005 0.9334 0.065 Uiso 1 1 calc R . . C22 C 0.0612(2) 0.8038(3) 0.7563(3) 0.0564(7) Uani 1 1 d . . . H22 H 0.0183 0.7467 0.7470 0.068 Uiso 1 1 calc R . . C23 C 0.1110(3) 0.9143(3) 0.6588(3) 0.0563(7) Uani 1 1 d . . . H23 H 0.1026 0.9313 0.5836 0.068 Uiso 1 1 calc R . . C24 C 0.1736(2) 1.0007(3) 0.6715(2) 0.0476(6) Uani 1 1 d . . . H24 H 0.2078 1.0755 0.6052 0.057 Uiso 1 1 calc R . . C25 C 0.1469(2) 1.2261(2) 0.79165(19) 0.0391(6) Uani 1 1 d . . . C26 C 0.1771(3) 1.3363(3) 0.7986(2) 0.0556(7) Uani 1 1 d . . . H26 H 0.2540 1.3441 0.8064 0.067 Uiso 1 1 calc R . . C27 C 0.0924(3) 1.4333(3) 0.7938(3) 0.0676(9) Uani 1 1 d . . . H27 H 0.1128 1.5070 0.7975 0.081 Uiso 1 1 calc R . . C28 C -0.0226(3) 1.4219(3) 0.7835(2) 0.0640(9) Uani 1 1 d . . . H28 H -0.0795 1.4876 0.7805 0.077 Uiso 1 1 calc R . . C29 C -0.0523(3) 1.3136(3) 0.7778(2) 0.0577(8) Uani 1 1 d . . . H29 H -0.1299 1.3058 0.7714 0.069 Uiso 1 1 calc R . . C30 C 0.0313(2) 1.2161(3) 0.7814(2) 0.0431(6) Uani 1 1 d . . . H30 H 0.0102 1.1431 0.7769 0.052 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 Ni1 0.04297(18) 0.0466(2) 0.04076(18) -0.01735(15) -0.00950(14) 0.00195(15) P1 0.0380(3) 0.0353(4) 0.0340(3) -0.0165(3) -0.0101(3) 0.0023(3) S1 0.0532(4) 0.0541(5) 0.0464(4) -0.0203(3) -0.0041(3) -0.0058(3) S2 0.0520(4) 0.0726(6) 0.0639(4) -0.0415(4) -0.0116(3) 0.0004(4) S3 0.0563(4) 0.0495(5) 0.0694(5) -0.0327(4) 0.0007(4) -0.0046(3) S4 0.0532(4) 0.0708(5) 0.0583(4) -0.0372(4) -0.0030(3) -0.0113(4) N1 0.0588(17) 0.137(3) 0.0729(18) -0.0505(19) -0.0033(15) -0.0206(18) N2 0.0631(17) 0.106(2) 0.0714(17) -0.0453(16) 0.0000(14) -0.0252(16) C1 0.0438(15) 0.061(2) 0.0335(13) -0.0130(13) -0.0103(11) 0.0033(13) C2 0.0482(16) 0.074(2) 0.0432(14) -0.0303(15) -0.0119(12) 0.0121(14) C3 0.0531(18) 0.085(2) 0.0444(15) -0.0286(15) -0.0103(14) 0.0003(16) C4 0.0410(15) 0.058(2) 0.0460(15) -0.0195(14) -0.0066(12) -0.0003(13) C5 0.0528(16) 0.0524(19) 0.0559(16) -0.0278(15) -0.0035(13) 0.0037(14) C6 0.0537(18) 0.070(2) 0.0529(16) -0.0317(15) -0.0114(14) -0.0030(15) C7 0.0393(13) 0.0392(16) 0.0366(12) -0.0173(11) -0.0124(10) -0.0011(11) C8 0.0517(16) 0.0501(18) 0.0511(15) -0.0254(13) -0.0207(12) 0.0067(13) C9 0.0646(18) 0.055(2) 0.0655(18) -0.0171(15) -0.0372(15) 0.0048(15) C10 0.071(2) 0.084(3) 0.0404(15) -0.0128(15) -0.0238(15) -0.0119(18) C11 0.070(2) 0.109(3) 0.0438(16) -0.0381(18) -0.0156(15) 0.011(2) C12 0.0571(17) 0.077(2) 0.0468(15) -0.0309(15) -0.0167(13) 0.0159(15) C13 0.0389(13) 0.0407(16) 0.0360(12) -0.0168(11) -0.0113(10) 0.0019(11) C14 0.0584(17) 0.0455(19) 0.0593(17) -0.0197(14) -0.0058(14) -0.0032(14) C15 0.064(2) 0.059(2) 0.0646(18) -0.0164(16) 0.0002(16) -0.0207(16) C16 0.0474(17) 0.087(3) 0.0502(16) -0.0264(17) 0.0015(13) -0.0122(17) C17 0.0565(19) 0.078(3) 0.074(2) -0.0417(19) 0.0045(16) 0.0055(17) C18 0.0584(17) 0.0509(19) 0.0567(16) -0.0244(14) 0.0010(14) -0.0006(14) C19 0.0366(13) 0.0379(15) 0.0366(12) -0.0188(11) -0.0095(10) 0.0039(11) C20 0.0429(14) 0.0459(17) 0.0409(13) -0.0172(12) -0.0086(11) -0.0027(12) C21 0.0472(16) 0.0446(18) 0.0631(17) -0.0182(14) -0.0086(13) -0.0063(13) C22 0.0536(17) 0.056(2) 0.078(2) -0.0426(17) -0.0213(15) 0.0001(14) C23 0.0672(18) 0.061(2) 0.0566(16) -0.0348(15) -0.0247(14) 0.0013(15) C24 0.0577(16) 0.0462(17) 0.0404(13) -0.0195(12) -0.0129(12) -0.0006(13) C25 0.0428(14) 0.0405(16) 0.0347(12) -0.0175(11) -0.0113(10) 0.0062(11) C26 0.0639(18) 0.052(2) 0.0677(18) -0.0368(15) -0.0276(14) 0.0117(14) C27 0.100(3) 0.051(2) 0.0666(19) -0.0359(16) -0.0346(18) 0.0218(18) C28 0.082(2) 0.065(2) 0.0416(15) -0.0246(15) -0.0240(15) 0.0385(17) C29 0.0504(16) 0.075(2) 0.0440(15) -0.0248(15) -0.0151(12) 0.0198(15) C30 0.0453(14) 0.0463(17) 0.0371(13) -0.0181(12) -0.0118(11) 0.0060(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 S1 2.1437(9) . ? Ni1 S4 2.1463(9) . ? Ni1 S3 2.1492(8) . ? Ni1 S2 2.1508(8) . ? P1 C19 1.794(2) . ? P1 C25 1.797(2) . ? P1 C13 1.797(2) . ? P1 C7 1.801(2) . ? S1 C1 1.737(3) . ? S2 C2 1.708(3) . ? S3 C5 1.703(3) . ? S4 C4 1.733(3) . ? N1 C3 1.143(4) . ? N2 C6 1.139(3) . ? C1 C2 1.340(4) . ? C1 C3 1.430(4) . ? C4 C5 1.341(4) . ? C4 C6 1.424(4) . ? C7 C8 1.382(3) . ? C7 C12 1.385(3) . ? C8 C9 1.379(4) . ? C9 C10 1.366(4) . ? C10 C11 1.361(4) . ? C11 C12 1.378(4) . ? C13 C14 1.375(4) . ? C13 C18 1.390(3) . ? C14 C15 1.385(4) . ? C15 C16 1.350(4) . ? C16 C17 1.367(4) . ? C17 C18 1.380(4) . ? C19 C20 1.380(3) . ? C19 C24 1.402(3) . ? C20 C21 1.383(4) . ? C21 C22 1.379(4) . ? C22 C23 1.370(4) . ? C23 C24 1.380(4) . ? C25 C30 1.385(3) . ? C25 C26 1.398(3) . ? C26 C27 1.376(4) . ? C27 C28 1.382(4) . ? C28 C29 1.368(4) . ? C29 C30 1.376(3) . ? 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 S1 Ni1 S4 178.82(4) . . ? S1 Ni1 S3 87.65(3) . . ? S4 Ni1 S3 91.95(3) . . ? S1 Ni1 S2 92.17(3) . . ? S4 Ni1 S2 88.19(3) . . ? S3 Ni1 S2 177.93(4) . . ? C19 P1 C25 108.04(11) . . ? C19 P1 C13 107.09(10) . . ? C25 P1 C13 112.51(11) . . ? C19 P1 C7 109.06(11) . . ? C25 P1 C7 109.21(11) . . ? C13 P1 C7 110.83(11) . . ? C1 S1 Ni1 102.87(10) . . ? C2 S2 Ni1 103.75(10) . . ? C5 S3 Ni1 103.69(10) . . ? C4 S4 Ni1 103.21(10) . . ? C2 C1 C3 122.9(2) . . ? C2 C1 S1 120.7(2) . . ? C3 C1 S1 116.4(2) . . ? C1 C2 S2 120.47(19) . . ? N1 C3 C1 178.0(3) . . ? C5 C4 C6 121.3(2) . . ? C5 C4 S4 120.1(2) . . ? C6 C4 S4 118.5(2) . . ? C4 C5 S3 121.0(2) . . ? N2 C6 C4 178.7(4) . . ? C8 C7 C12 119.3(2) . . ? C8 C7 P1 118.90(17) . . ? C12 C7 P1 121.6(2) . . ? C9 C8 C7 120.2(2) . . ? C10 C9 C8 120.2(3) . . ? C11 C10 C9 119.8(3) . . ? C10 C11 C12 121.2(3) . . ? C11 C12 C7 119.3(3) . . ? C14 C13 C18 118.6(2) . . ? C14 C13 P1 123.16(19) . . ? C18 C13 P1 118.17(19) . . ? C13 C14 C15 120.0(3) . . ? C16 C15 C14 121.2(3) . . ? C15 C16 C17 119.6(3) . . ? C16 C17 C18 120.5(3) . . ? C17 C18 C13 120.1(3) . . ? C20 C19 C24 119.8(2) . . ? C20 C19 P1 122.04(17) . . ? C24 C19 P1 117.98(18) . . ? C19 C20 C21 119.9(2) . . ? C22 C21 C20 120.1(3) . . ? C23 C22 C21 120.4(3) . . ? C22 C23 C24 120.4(3) . . ? C23 C24 C19 119.4(3) . . ? C30 C25 C26 119.1(2) . . ? C30 C25 P1 120.05(19) . . ? C26 C25 P1 120.8(2) . . ? C27 C26 C25 119.7(3) . . ? C26 C27 C28 120.5(3) . . ? C29 C28 C27 119.7(3) . . ? C28 C29 C30 120.7(3) . . ? C29 C30 C25 120.2(3) . . ? _diffrn_measured_fraction_theta_max 0.925 _diffrn_reflns_theta_full 25.97 _diffrn_measured_fraction_theta_full 0.925 _refine_diff_density_max 0.296 _refine_diff_density_min -0.196 _refine_diff_density_rms 0.047