# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2003 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 loop_ _publ_author_name 'Michael P. Bubnov' 'Gleb A. Abakumov' 'Vladimir K. Cherkasov' 'Georgy K. Fukin' 'Konstantin A. Kozhanov' _publ_contact_author_name 'Dr Michael P Bubnov' _publ_contact_author_address ; G A Razuvaev Institute of organometallic chemistry of Russian Academy of Science 49 Tropinina str 603950 Nizhny Novgorod RUSSIAN FEDERATION ; _publ_contact_author_email BMP@IMOC.SINN.RU _publ_section_title ; EPR study of intramolecular dynamics in o-semiquinonic nickel complexes with di-phosphorous pincer ligand ; _publ_section_references ; Bruker (2000) SAINTPlus Data Reduction and Correction Program v. 6.02a, Bruker AXS, Madison, Wisconsin, USA. Bruker (2000) SMART. Bruker Molecular Analysis Research Tool, v. 5.625 Bruker AXS, Madison, Wisconsin, USA. Sheldrick G.M. (1998a). SADABS v.2.01, Bruker/Siemens Area Detector Absorption Correction Program, Bruker AXS, Madison, Wisconsin, USA. Sheldrick G.M. (2000). SHELXTL v. 6.12, Structure Determination Software Suite, Bruker AXS, Madison, Wisconsin, USA. ; data_nisqm _database_code_CSD 212481 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ; (2,6-bis-(diphenylphosphinomethyl)-phenyl) (3,6-di-tert-butyl- o-benzosemiquinono)nikel ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H47 Ni O2 P2' _chemical_formula_weight 752.49 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' O O 0.0106 0.0060 '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' 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 21.1434(16) _cell_length_b 9.4577(7) _cell_length_c 22.2619(16) _cell_angle_alpha 90.00 _cell_angle_beta 117.4680(10) _cell_angle_gamma 90.00 _cell_volume 3949.8(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 800 _cell_measurement_theta_min 2 _cell_measurement_theta_max 26 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.265 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1588 _exptl_absorpt_coefficient_mu 0.609 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8676 _exptl_absorpt_correction_T_max 0.9529 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1998a)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32601 _diffrn_reflns_av_R_equivalents 0.0512 _diffrn_reflns_av_sigmaI/netI 0.0448 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 26.00 _reflns_number_total 7748 _reflns_number_gt 6370 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0476P)^2^+0.6464P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7748 _refine_ls_number_parameters 648 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0481 _refine_ls_R_factor_gt 0.0355 _refine_ls_wR_factor_ref 0.0882 _refine_ls_wR_factor_gt 0.0840 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _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 0.073471(9) 0.15766(2) 0.810120(9) 0.01387(5) Uani 1 1 d . . . P1 P 0.05998(2) 0.26911(4) 0.888490(19) 0.01615(9) Uani 1 1 d . . . P2 P 0.145938(19) 0.01284(4) 0.795668(18) 0.01464(9) Uani 1 1 d . . . O1 O -0.00253(5) 0.02281(11) 0.78596(5) 0.0169(2) Uani 1 1 d . . . O2 O 0.00969(5) 0.22498(11) 0.71252(5) 0.0173(2) Uani 1 1 d . . . C1 C -0.04955(7) 0.02507(16) 0.72263(7) 0.0158(3) Uani 1 1 d . . . C2 C -0.04336(7) 0.13996(15) 0.68225(7) 0.0153(3) Uani 1 1 d . . . C3 C -0.09432(8) 0.15501(16) 0.61188(7) 0.0179(4) Uani 1 1 d . . . C4 C -0.14631(8) 0.05347(17) 0.58620(8) 0.0206(4) Uani 1 1 d . . . H4 H -0.1805(8) 0.0498(18) 0.5398(8) 0.023(5) Uiso 1 1 d . . . C5 C -0.15114(8) -0.06061(17) 0.62535(8) 0.0201(4) Uani 1 1 d . . . H5 H -0.1884(8) -0.1284(16) 0.6027(7) 0.012(4) Uiso 1 1 d . . . C6 C -0.10433(7) -0.07871(16) 0.69321(7) 0.0163(3) Uani 1 1 d . . . C7 C -0.08824(8) 0.28003(17) 0.57124(8) 0.0205(4) Uani 1 1 d . . . C8 C -0.09307(9) 0.41852(18) 0.60485(8) 0.0240(4) Uani 1 1 d . . . H8C H -0.1381(10) 0.424(2) 0.6042(9) 0.034(5) Uiso 1 1 d . . . H8B H -0.0883(9) 0.498(2) 0.5796(9) 0.033(5) Uiso 1 1 d . . . H8A H -0.0539(9) 0.4253(19) 0.6522(9) 0.028(5) Uiso 1 1 d . . . C9 C -0.01661(9) 0.27351(19) 0.56910(8) 0.0251(4) Uani 1 1 d . . . H9C H -0.0120(8) 0.1836(17) 0.5485(7) 0.013(4) Uiso 1 1 d . . . H9B H 0.0240(9) 0.2812(19) 0.6155(8) 0.027(5) Uiso 1 1 d . . . H9A H -0.0144(9) 0.349(2) 0.5404(9) 0.031(5) Uiso 1 1 d . . . C10 C -0.14799(10) 0.2792(2) 0.49800(8) 0.0299(5) Uani 1 1 d . . . H10C H -0.1460(9) 0.193(2) 0.4733(9) 0.028(5) Uiso 1 1 d . . . H10B H -0.1978(9) 0.2819(19) 0.4961(8) 0.028(5) Uiso 1 1 d . . . H10A H -0.1426(9) 0.3629(19) 0.4743(8) 0.027(5) Uiso 1 1 d . . . C11 C -0.10928(8) -0.20186(17) 0.73546(8) 0.0196(4) Uani 1 1 d . . . C12 C -0.03926(9) -0.28632(19) 0.76686(9) 0.0271(4) Uani 1 1 d . . . H12C H -0.0298(10) -0.324(2) 0.7313(9) 0.035(5) Uiso 1 1 d . . . H12B H -0.0424(10) -0.367(2) 0.7922(10) 0.043(6) Uiso 1 1 d . . . H12A H 0.0032(10) -0.226(2) 0.7995(10) 0.044(6) Uiso 1 1 d . . . C13 C -0.16858(9) -0.30578(18) 0.69286(9) 0.0241(4) Uani 1 1 d . . . H13C H -0.1684(9) -0.379(2) 0.7213(9) 0.030(5) Uiso 1 1 d . . . H13B H -0.2140(10) -0.260(2) 0.6724(9) 0.037(5) Uiso 1 1 d . . . H13A H -0.1638(9) -0.3481(18) 0.6550(8) 0.021(4) Uiso 1 1 d . . . C14 C -0.12490(9) -0.14359(19) 0.79164(9) 0.0273(4) Uani 1 1 d . . . H14C H -0.0885(10) -0.080(2) 0.8223(9) 0.040(6) Uiso 1 1 d . . . H14B H -0.1279(10) -0.226(2) 0.8197(9) 0.039(5) Uiso 1 1 d . . . H14A H -0.1721(10) -0.089(2) 0.7715(10) 0.045(6) Uiso 1 1 d . . . C15 C 0.15122(8) 0.28808(16) 0.83310(7) 0.0147(3) Uani 1 1 d . . . C16 C 0.15924(8) 0.41056(16) 0.87207(7) 0.0158(3) Uani 1 1 d . . . C17 C 0.21653(8) 0.50233(16) 0.88832(7) 0.0176(3) Uani 1 1 d . . . H17 H 0.2209(8) 0.5815(19) 0.9146(8) 0.023(5) Uiso 1 1 d . . . C18 C 0.26580(8) 0.47594(17) 0.86502(8) 0.0196(4) Uani 1 1 d . . . H18 H 0.3065(8) 0.5382(17) 0.8775(7) 0.014(4) Uiso 1 1 d . . . C19 C 0.25812(8) 0.35793(16) 0.82530(7) 0.0176(3) Uani 1 1 d . . . H19 H 0.2911(8) 0.3381(17) 0.8098(8) 0.016(4) Uiso 1 1 d . . . C20 C 0.20139(8) 0.26570(16) 0.80887(7) 0.0152(3) Uani 1 1 d . . . C21 C 0.10302(8) 0.43972(17) 0.89393(8) 0.0201(4) Uani 1 1 d . . . H21B H 0.1213(8) 0.4812(18) 0.9381(8) 0.020(4) Uiso 1 1 d . . . H21A H 0.0656(9) 0.4985(19) 0.8620(8) 0.027(5) Uiso 1 1 d . . . C22 C 0.10641(8) 0.18903(18) 0.97179(8) 0.0209(4) Uani 1 1 d . . . C23 C 0.17267(9) 0.2377(2) 1.02061(8) 0.0287(4) Uani 1 1 d . . . H23 H 0.1928(10) 0.328(2) 1.0115(9) 0.042(6) Uiso 1 1 d . . . C24 C 0.20956(11) 0.1653(2) 1.08083(9) 0.0397(5) Uani 1 1 d . . . H24 H 0.2545(10) 0.203(2) 1.1137(9) 0.034(5) Uiso 1 1 d . . . C25 C 0.18146(11) 0.0445(3) 1.09323(9) 0.0458(6) Uani 1 1 d . . . H25 H 0.2082(10) 0.000(2) 1.1354(10) 0.043(6) Uiso 1 1 d . . . C26 C 0.11623(11) -0.0056(2) 1.04588(10) 0.0439(5) Uani 1 1 d . . . H26 H 0.0947(11) -0.079(3) 1.0527(11) 0.057(7) Uiso 1 1 d . . . C27 C 0.07842(9) 0.0662(2) 0.98465(9) 0.0310(4) Uani 1 1 d . . . H27 H 0.0378(9) 0.0327(19) 0.9520(9) 0.027(5) Uiso 1 1 d . . . C28 C -0.02791(8) 0.31439(17) 0.87915(8) 0.0199(4) Uani 1 1 d . . . C29 C -0.08613(9) 0.30689(19) 0.81574(9) 0.0271(4) Uani 1 1 d . . . H29 H -0.0808(10) 0.268(2) 0.7780(10) 0.044(6) Uiso 1 1 d . . . C30 C -0.15222(9) 0.3544(2) 0.80557(9) 0.0323(5) Uani 1 1 d . . . H30 H -0.1941(10) 0.348(2) 0.7591(10) 0.045(6) Uiso 1 1 d . . . C31 C -0.16062(9) 0.4113(2) 0.85814(10) 0.0335(5) Uani 1 1 d . . . H31 H -0.2043(10) 0.448(2) 0.8505(9) 0.034(5) Uiso 1 1 d . . . C32 C -0.10330(10) 0.4157(2) 0.92182(10) 0.0433(5) Uani 1 1 d . . . H32 H -0.1091(11) 0.457(2) 0.9583(11) 0.052(6) Uiso 1 1 d . . . C33 C -0.03721(10) 0.3668(2) 0.93287(10) 0.0365(5) Uani 1 1 d . . . H33 H 0.0034(10) 0.369(2) 0.9772(10) 0.041(6) Uiso 1 1 d . . . C34 C 0.19201(8) 0.13618(16) 0.76599(8) 0.0180(3) Uani 1 1 d . . . H34B H 0.2348(8) 0.1024(17) 0.7681(7) 0.015(4) Uiso 1 1 d . . . H34A H 0.1589(8) 0.1526(17) 0.7179(8) 0.020(4) Uiso 1 1 d . . . C35 C 0.21643(8) -0.07055(16) 0.87000(7) 0.0168(3) Uani 1 1 d . . . C36 C 0.20781(8) -0.08584(17) 0.92805(8) 0.0201(4) Uani 1 1 d . . . H36 H 0.1666(8) -0.0557(18) 0.9274(8) 0.019(4) Uiso 1 1 d . . . C37 C 0.26052(9) -0.14950(17) 0.98557(8) 0.0236(4) Uani 1 1 d . . . H37 H 0.2530(9) -0.1581(19) 1.0234(9) 0.028(5) Uiso 1 1 d . . . C38 C 0.32235(9) -0.19705(18) 0.98580(8) 0.0247(4) Uani 1 1 d . . . H38 H 0.3584(10) -0.237(2) 1.0270(9) 0.033(5) Uiso 1 1 d . . . C39 C 0.33198(9) -0.18034(17) 0.92868(9) 0.0244(4) Uani 1 1 d . . . H39 H 0.3731(10) -0.212(2) 0.9284(9) 0.030(5) Uiso 1 1 d . . . C40 C 0.27953(8) -0.11849(17) 0.87118(8) 0.0211(4) Uani 1 1 d . . . H40 H 0.2860(9) -0.1072(19) 0.8323(9) 0.024(5) Uiso 1 1 d . . . C41 C 0.11035(7) -0.12714(16) 0.73277(7) 0.0157(3) Uani 1 1 d . . . C42 C 0.12387(8) -0.26947(17) 0.74950(8) 0.0209(4) Uani 1 1 d . . . H42 H 0.1516(8) -0.2977(18) 0.7955(8) 0.017(4) Uiso 1 1 d . . . C43 C 0.09619(9) -0.37302(18) 0.69973(9) 0.0263(4) Uani 1 1 d . . . H43 H 0.1062(9) -0.469(2) 0.7138(8) 0.027(5) Uiso 1 1 d . . . C44 C 0.05460(9) -0.33482(19) 0.63293(9) 0.0282(4) Uani 1 1 d . . . H44 H 0.0347(10) -0.406(2) 0.5981(9) 0.039(6) Uiso 1 1 d . . . C45 C 0.03916(9) -0.1932(2) 0.61571(8) 0.0257(4) Uani 1 1 d . . . H45 H 0.0085(9) -0.1648(18) 0.5695(9) 0.025(5) Uiso 1 1 d . . . C46 C 0.06655(8) -0.09003(18) 0.66536(8) 0.0201(4) Uani 1 1 d . . . H46 H 0.0561(8) 0.0033(18) 0.6537(8) 0.016(4) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.01433(9) 0.01163(9) 0.01529(8) -0.00177(7) 0.00653(7) -0.00125(7) P1 0.01566(17) 0.01547(19) 0.01787(17) -0.00283(15) 0.00821(14) -0.00053(15) P2 0.01611(17) 0.01196(18) 0.01572(17) -0.00150(14) 0.00723(14) -0.00011(15) O1 0.0175(5) 0.0153(5) 0.0161(5) -0.0004(4) 0.0062(4) -0.0019(4) O2 0.0176(5) 0.0145(5) 0.0175(5) -0.0011(4) 0.0060(4) -0.0028(4) C1 0.0143(6) 0.0139(7) 0.0193(7) -0.0020(6) 0.0078(5) 0.0025(6) C2 0.0154(6) 0.0124(7) 0.0182(7) -0.0031(6) 0.0077(5) 0.0008(6) C3 0.0179(7) 0.0158(8) 0.0181(7) -0.0012(6) 0.0066(6) 0.0021(6) C4 0.0181(7) 0.0206(8) 0.0167(7) -0.0022(6) 0.0028(6) -0.0005(6) C5 0.0181(7) 0.0179(8) 0.0219(7) -0.0054(6) 0.0072(6) -0.0034(6) C6 0.0158(6) 0.0147(7) 0.0207(7) -0.0023(6) 0.0104(6) -0.0004(6) C7 0.0207(7) 0.0169(8) 0.0182(7) 0.0012(6) 0.0041(6) -0.0012(6) C8 0.0246(8) 0.0163(8) 0.0267(8) 0.0026(7) 0.0081(7) 0.0020(7) C9 0.0311(8) 0.0223(9) 0.0233(8) 0.0022(7) 0.0137(7) -0.0019(7) C10 0.0350(9) 0.0259(9) 0.0182(8) 0.0053(7) 0.0033(7) -0.0049(8) C11 0.0177(7) 0.0175(8) 0.0234(7) 0.0002(6) 0.0092(6) -0.0024(6) C12 0.0241(8) 0.0183(8) 0.0356(9) 0.0058(7) 0.0109(7) 0.0014(7) C13 0.0239(8) 0.0171(8) 0.0294(8) 0.0009(7) 0.0107(7) -0.0030(7) C14 0.0309(8) 0.0280(9) 0.0265(8) -0.0027(7) 0.0162(7) -0.0084(7) C15 0.0146(6) 0.0134(7) 0.0129(6) 0.0021(6) 0.0037(5) -0.0004(6) C16 0.0173(7) 0.0140(7) 0.0144(7) 0.0023(6) 0.0058(5) 0.0024(6) C17 0.0211(7) 0.0103(7) 0.0184(7) -0.0005(6) 0.0066(6) 0.0002(6) C18 0.0186(7) 0.0160(8) 0.0213(7) 0.0024(6) 0.0067(6) -0.0027(6) C19 0.0183(7) 0.0167(8) 0.0196(7) 0.0044(6) 0.0102(6) 0.0026(6) C20 0.0183(7) 0.0125(7) 0.0140(6) 0.0019(5) 0.0067(5) 0.0003(6) C21 0.0220(7) 0.0147(8) 0.0243(7) -0.0033(6) 0.0114(6) 0.0004(6) C22 0.0226(7) 0.0236(8) 0.0210(7) -0.0005(6) 0.0140(6) 0.0062(6) C23 0.0241(8) 0.0356(10) 0.0253(8) -0.0037(7) 0.0104(7) 0.0078(8) C24 0.0354(10) 0.0562(13) 0.0240(9) -0.0006(9) 0.0106(8) 0.0160(9) C25 0.0467(10) 0.0686(14) 0.0282(9) 0.0172(9) 0.0225(8) 0.0367(10) C26 0.0564(10) 0.0423(12) 0.0529(10) 0.0210(9) 0.0421(8) 0.0194(10) C27 0.0295(8) 0.0327(10) 0.0348(9) 0.0065(8) 0.0183(7) 0.0049(8) C28 0.0176(7) 0.0167(8) 0.0275(8) -0.0035(6) 0.0122(6) -0.0001(6) C29 0.0244(8) 0.0290(9) 0.0285(8) -0.0059(7) 0.0127(7) 0.0023(7) C30 0.0223(8) 0.0342(10) 0.0361(9) -0.0019(8) 0.0099(7) 0.0035(8) C31 0.0198(8) 0.0312(10) 0.0530(10) -0.0083(8) 0.0198(7) 0.0007(7) C32 0.0312(9) 0.0582(13) 0.0467(10) -0.0218(10) 0.0233(8) 0.0003(9) C33 0.0249(8) 0.0491(12) 0.0352(9) -0.0158(9) 0.0137(7) -0.0006(8) C34 0.0204(7) 0.0161(8) 0.0213(7) -0.0017(6) 0.0129(6) -0.0008(6) C35 0.0184(7) 0.0095(7) 0.0191(7) -0.0035(6) 0.0057(6) -0.0011(6) C36 0.0235(7) 0.0146(8) 0.0216(7) -0.0031(6) 0.0099(6) 0.0012(6) C37 0.0316(8) 0.0158(8) 0.0203(7) -0.0017(6) 0.0093(7) 0.0001(7) C38 0.0225(8) 0.0155(8) 0.0220(8) -0.0021(6) -0.0017(7) -0.0018(7) C39 0.0173(7) 0.0170(8) 0.0332(9) -0.0044(7) 0.0069(7) 0.0009(6) C40 0.0212(7) 0.0163(8) 0.0259(8) -0.0036(6) 0.0109(6) -0.0017(6) C41 0.0147(6) 0.0148(7) 0.0201(7) -0.0038(6) 0.0102(5) -0.0013(6) C42 0.0201(7) 0.0184(8) 0.0261(8) -0.0018(6) 0.0125(6) -0.0019(6) C43 0.0303(8) 0.0151(8) 0.0361(9) -0.0041(7) 0.0175(7) -0.0029(7) C44 0.0303(8) 0.0248(9) 0.0318(8) -0.0152(7) 0.0162(7) -0.0089(7) C45 0.0231(8) 0.0328(10) 0.0200(8) -0.0046(7) 0.0090(6) -0.0017(7) C46 0.0194(7) 0.0183(8) 0.0230(7) -0.0008(6) 0.0100(6) 0.0011(6) _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 O1 1.9238(10) . ? Ni1 C15 1.9261(15) . ? Ni1 O2 2.0595(10) . ? Ni1 P1 2.1669(5) . ? Ni1 P2 2.1867(5) . ? P1 C22 1.8156(16) . ? P1 C28 1.8231(16) . ? P1 C21 1.8289(17) . ? P2 C35 1.8184(15) . ? P2 C41 1.8186(15) . ? P2 C34 1.8275(17) . ? O1 C1 1.2975(17) . ? O2 C2 1.2890(17) . ? C1 C6 1.426(2) . ? C1 C2 1.454(2) . ? C2 C3 1.442(2) . ? C3 C4 1.370(2) . ? C3 C7 1.530(2) . ? C4 C5 1.420(2) . ? C5 C6 1.383(2) . ? C6 C11 1.531(2) . ? C7 C10 1.534(2) . ? C7 C8 1.535(2) . ? C7 C9 1.538(2) . ? C11 C13 1.530(2) . ? C11 C14 1.536(2) . ? C11 C12 1.537(2) . ? C15 C16 1.410(2) . ? C15 C20 1.410(2) . ? C16 C17 1.395(2) . ? C16 C21 1.503(2) . ? C17 C18 1.384(2) . ? C18 C19 1.386(2) . ? C19 C20 1.389(2) . ? C20 C34 1.509(2) . ? C22 C27 1.392(3) . ? C22 C23 1.397(2) . ? C23 C24 1.382(3) . ? C24 C25 1.374(3) . ? C25 C26 1.377(3) . ? C26 C27 1.398(3) . ? C28 C29 1.382(2) . ? C28 C33 1.390(3) . ? C29 C30 1.383(3) . ? C30 C31 1.372(3) . ? C31 C32 1.377(3) . ? C32 C33 1.382(3) . ? C35 C36 1.393(2) . ? C35 C40 1.398(2) . ? C36 C37 1.388(2) . ? C37 C38 1.380(3) . ? C38 C39 1.387(3) . ? C39 C40 1.379(2) . ? C41 C42 1.391(2) . ? C41 C46 1.397(2) . ? C42 C43 1.390(2) . ? C43 C44 1.382(2) . ? C44 C45 1.390(3) . ? C45 C46 1.385(2) . ? 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 O1 Ni1 C15 177.96(6) . . ? O1 Ni1 O2 81.60(4) . . ? C15 Ni1 O2 98.37(5) . . ? O1 Ni1 P1 98.30(4) . . ? C15 Ni1 P1 83.56(5) . . ? O2 Ni1 P1 115.70(3) . . ? O1 Ni1 P2 95.47(3) . . ? C15 Ni1 P2 82.54(5) . . ? O2 Ni1 P2 101.58(3) . . ? P1 Ni1 P2 141.677(16) . . ? C22 P1 C28 104.90(8) . . ? C22 P1 C21 106.39(7) . . ? C28 P1 C21 104.49(7) . . ? C22 P1 Ni1 114.17(6) . . ? C28 P1 Ni1 121.89(5) . . ? C21 P1 Ni1 103.66(6) . . ? C35 P2 C41 105.03(7) . . ? C35 P2 C34 104.84(7) . . ? C41 P2 C34 106.65(7) . . ? C35 P2 Ni1 118.27(6) . . ? C41 P2 Ni1 120.01(5) . . ? C34 P2 Ni1 100.36(5) . . ? C1 O1 Ni1 114.55(10) . . ? C2 O2 Ni1 110.31(9) . . ? O1 C1 C6 122.71(14) . . ? O1 C1 C2 116.21(13) . . ? C6 C1 C2 121.07(12) . . ? O2 C2 C3 122.72(14) . . ? O2 C2 C1 116.59(12) . . ? C3 C2 C1 120.68(13) . . ? C4 C3 C2 115.96(14) . . ? C4 C3 C7 124.40(13) . . ? C2 C3 C7 119.63(13) . . ? C3 C4 C5 123.19(14) . . ? C6 C5 C4 123.15(14) . . ? C5 C6 C1 115.90(14) . . ? C5 C6 C11 123.24(13) . . ? C1 C6 C11 120.85(12) . . ? C3 C7 C10 111.82(13) . . ? C3 C7 C8 109.19(14) . . ? C10 C7 C8 108.37(13) . . ? C3 C7 C9 109.87(13) . . ? C10 C7 C9 107.86(14) . . ? C8 C7 C9 109.70(14) . . ? C13 C11 C6 112.14(12) . . ? C13 C11 C14 108.22(14) . . ? C6 C11 C14 109.19(13) . . ? C13 C11 C12 106.86(13) . . ? C6 C11 C12 110.51(14) . . ? C14 C11 C12 109.87(13) . . ? C16 C15 C20 117.42(14) . . ? C16 C15 Ni1 122.37(12) . . ? C20 C15 Ni1 120.17(11) . . ? C17 C16 C15 120.95(15) . . ? C17 C16 C21 121.56(14) . . ? C15 C16 C21 117.47(13) . . ? C18 C17 C16 120.27(14) . . ? C17 C18 C19 119.83(14) . . ? C18 C19 C20 120.44(15) . . ? C19 C20 C15 121.03(14) . . ? C19 C20 C34 121.48(15) . . ? C15 C20 C34 117.47(13) . . ? C16 C21 P1 105.09(11) . . ? C27 C22 C23 118.93(15) . . ? C27 C22 P1 118.50(12) . . ? C23 C22 P1 122.22(14) . . ? C24 C23 C22 120.44(19) . . ? C25 C24 C23 120.27(18) . . ? C24 C25 C26 120.37(18) . . ? C25 C26 C27 120.0(2) . . ? C22 C27 C26 120.00(17) . . ? C29 C28 C33 118.97(15) . . ? C29 C28 P1 119.04(13) . . ? C33 C28 P1 121.80(12) . . ? C28 C29 C30 120.48(17) . . ? C31 C30 C29 120.40(16) . . ? C30 C31 C32 119.43(17) . . ? C31 C32 C33 120.72(19) . . ? C32 C33 C28 119.93(16) . . ? C20 C34 P2 103.06(11) . . ? C36 C35 C40 118.75(14) . . ? C36 C35 P2 119.09(12) . . ? C40 C35 P2 122.16(13) . . ? C37 C36 C35 120.51(16) . . ? C38 C37 C36 120.05(17) . . ? C37 C38 C39 119.94(15) . . ? C40 C39 C38 120.28(16) . . ? C39 C40 C35 120.46(16) . . ? C42 C41 C46 118.91(14) . . ? C42 C41 P2 122.51(11) . . ? C46 C41 P2 118.56(12) . . ? C43 C42 C41 120.64(15) . . ? C44 C43 C42 119.92(16) . . ? C43 C44 C45 120.04(16) . . ? C46 C45 C44 120.02(15) . . ? C45 C46 C41 120.41(15) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.493 _refine_diff_density_min -0.257 _refine_diff_density_rms 0.060