Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'D. W. Stephan' _publ_contact_author_address ; Dept of Chemistry & Biochemistry University of Windsor Windsor Ontario N9P 3P4 CANADA ; _publ_contact_author_email STEPHAN@UWINDSOR.CA _publ_section_title ; P-H and P-P Bond Activation by Ni(I) and Fe(I) ?-diketiminato-Complexes ; loop_ _publ_author_name 'D. W. Stephan' 'Guangcai Bai.' 'Anjan K. Das' 'Pingrong Wei.' data_(NacNac)Ni(PH2Ph) _database_code_depnum_ccdc_archive 'CCDC 284029' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C35 H48 N2 Ni P' _chemical_formula_weight 586.43 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 15.6612(18) _cell_length_b 16.3201(19) _cell_length_c 26.832(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6858.1(14) _cell_formula_units_Z 8 _cell_measurement_temperature 273(2) _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_diffrn 1.136 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2520 _exptl_absorpt_coefficient_mu 0.636 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.837188 _exptl_absorpt_correction_T_max 1.000000 _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 62484 _diffrn_reflns_av_R_equivalents 0.1356 _diffrn_reflns_av_sigmaI/netI 0.0660 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6036 _reflns_number_gt 3204 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0795P)^2^+5.9078P] 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_number_reflns 6036 _refine_ls_number_parameters 354 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1385 _refine_ls_R_factor_gt 0.0633 _refine_ls_wR_factor_ref 0.1896 _refine_ls_wR_factor_gt 0.1411 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _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 0.90103(4) 0.18524(4) 0.38692(2) 0.0553(3) Uani 1 1 d . . . P1 P 1.02992(10) 0.19180(15) 0.41524(8) 0.1047(8) Uani 1 1 d . . . H10B H 1.0464 0.2491 0.4164 0.126 Uiso 1 1 calc R . . H10C H 1.0295 0.1718 0.4493 0.126 Uiso 1 1 calc R . . N1 N 0.8233(2) 0.2313(2) 0.43423(13) 0.0420(9) Uani 1 1 d . . . N2 N 0.8199(2) 0.1553(2) 0.33911(12) 0.0366(9) Uani 1 1 d . . . C1 C 0.8605(3) 0.2632(3) 0.47912(17) 0.0464(12) Uani 1 1 d . . . C2 C 0.8741(4) 0.2127(4) 0.51971(19) 0.0624(16) Uani 1 1 d . . . C3 C 0.9209(4) 0.2432(5) 0.5601(2) 0.083(2) Uani 1 1 d . . . H3A H 0.9313 0.2100 0.5876 0.100 Uiso 1 1 calc R . . C4 C 0.9516(4) 0.3222(6) 0.5593(3) 0.093(2) Uani 1 1 d . . . H4A H 0.9836 0.3417 0.5860 0.111 Uiso 1 1 calc R . . C5 C 0.9359(4) 0.3713(5) 0.5203(3) 0.086(2) Uani 1 1 d . . . H5A H 0.9569 0.4246 0.5207 0.103 Uiso 1 1 calc R . . C6 C 0.8896(4) 0.3455(4) 0.4795(2) 0.0618(15) Uani 1 1 d . . . C7 C 0.8383(5) 0.1261(4) 0.5217(2) 0.089(2) Uani 1 1 d . . . H7A H 0.8036 0.1190 0.4916 0.107 Uiso 1 1 calc R . . C8 C 0.7789(8) 0.1136(5) 0.5658(3) 0.163(4) Uani 1 1 d . . . H8A H 0.7577 0.0584 0.5656 0.245 Uiso 1 1 calc R . . H8B H 0.7318 0.1511 0.5635 0.245 Uiso 1 1 calc R . . H8C H 0.8095 0.1233 0.5962 0.245 Uiso 1 1 calc R . . C9 C 0.9066(7) 0.0611(5) 0.5201(4) 0.173(5) Uani 1 1 d . . . H9A H 0.9431 0.0704 0.4920 0.260 Uiso 1 1 calc R . . H9B H 0.8804 0.0081 0.5172 0.260 Uiso 1 1 calc R . . H9C H 0.9397 0.0633 0.5502 0.260 Uiso 1 1 calc R . . C10 C 0.8693(5) 0.4050(4) 0.4379(3) 0.096(2) Uani 1 1 d . . . H10A H 0.8296 0.3774 0.4152 0.115 Uiso 1 1 calc R . . C11 C 0.9493(7) 0.4261(6) 0.4077(3) 0.160(4) Uani 1 1 d . . . H11A H 0.9346 0.4639 0.3816 0.239 Uiso 1 1 calc R . . H11B H 0.9725 0.3770 0.3933 0.239 Uiso 1 1 calc R . . H11C H 0.9911 0.4507 0.4292 0.239 Uiso 1 1 calc R . . C12 C 0.8261(6) 0.4819(5) 0.4559(3) 0.136(3) Uani 1 1 d . . . H12A H 0.7762 0.4676 0.4748 0.204 Uiso 1 1 calc R . . H12B H 0.8098 0.5148 0.4278 0.204 Uiso 1 1 calc R . . H12C H 0.8648 0.5123 0.4766 0.204 Uiso 1 1 calc R . . C13 C 0.7399(3) 0.2334(3) 0.42770(16) 0.0408(11) Uani 1 1 d . . . C14 C 0.6830(3) 0.2680(4) 0.46750(18) 0.0647(15) Uani 1 1 d . . . H14A H 0.6877 0.2353 0.4971 0.097 Uiso 1 1 calc R . . H14B H 0.6249 0.2676 0.4561 0.097 Uiso 1 1 calc R . . H14C H 0.6999 0.3232 0.4748 0.097 Uiso 1 1 calc R . . C15 C 0.7002(3) 0.2035(3) 0.38458(16) 0.0444(12) Uani 1 1 d . . . H15A H 0.6411 0.2088 0.3838 0.053 Uiso 1 1 calc R . . C16 C 0.7365(3) 0.1673(3) 0.34296(16) 0.0400(11) Uani 1 1 d . . . C17 C 0.6783(3) 0.1419(4) 0.3008(2) 0.0675(16) Uani 1 1 d . . . H17A H 0.6950 0.1697 0.2709 0.101 Uiso 1 1 calc R . . H17B H 0.6205 0.1561 0.3090 0.101 Uiso 1 1 calc R . . H17C H 0.6825 0.0838 0.2959 0.101 Uiso 1 1 calc R . . C18 C 0.8567(3) 0.1169(3) 0.29609(16) 0.0371(11) Uani 1 1 d . . . C19 C 0.8891(3) 0.1652(3) 0.25756(18) 0.0471(12) Uani 1 1 d . . . C20 C 0.9344(3) 0.1273(4) 0.21979(19) 0.0570(14) Uani 1 1 d . . . H20A H 0.9569 0.1589 0.1941 0.068 Uiso 1 1 calc R . . C21 C 0.9470(3) 0.0440(4) 0.2194(2) 0.0618(15) Uani 1 1 d . . . H21A H 0.9779 0.0196 0.1938 0.074 Uiso 1 1 calc R . . C22 C 0.9137(3) -0.0025(3) 0.2569(2) 0.0570(14) Uani 1 1 d . . . H22A H 0.9225 -0.0589 0.2564 0.068 Uiso 1 1 calc R . . C23 C 0.8676(3) 0.0313(3) 0.29524(17) 0.0424(11) Uani 1 1 d . . . C24 C 0.8754(4) 0.2575(3) 0.2566(2) 0.0708(18) Uani 1 1 d . . . H24A H 0.8354 0.2707 0.2835 0.085 Uiso 1 1 calc R . . C25 C 0.9585(6) 0.3014(4) 0.2680(4) 0.157(4) Uani 1 1 d . . . H25A H 0.9492 0.3596 0.2673 0.235 Uiso 1 1 calc R . . H25B H 1.0006 0.2870 0.2436 0.235 Uiso 1 1 calc R . . H25C H 0.9783 0.2856 0.3005 0.235 Uiso 1 1 calc R . . C26 C 0.8351(7) 0.2859(4) 0.2085(3) 0.155(4) Uani 1 1 d . . . H26A H 0.8276 0.3443 0.2094 0.232 Uiso 1 1 calc R . . H26B H 0.7805 0.2599 0.2044 0.232 Uiso 1 1 calc R . . H26C H 0.8714 0.2716 0.1810 0.232 Uiso 1 1 calc R . . C27 C 0.8317(4) -0.0232(3) 0.3358(2) 0.0651(16) Uani 1 1 d . . . H27A H 0.7956 0.0108 0.3573 0.078 Uiso 1 1 calc R . . C28 C 0.7763(5) -0.0913(4) 0.3149(3) 0.107(3) Uani 1 1 d . . . H28A H 0.7549 -0.1244 0.3417 0.160 Uiso 1 1 calc R . . H28B H 0.8098 -0.1247 0.2928 0.160 Uiso 1 1 calc R . . H28C H 0.7293 -0.0679 0.2968 0.160 Uiso 1 1 calc R . . C29 C 0.9020(6) -0.0592(5) 0.3680(3) 0.127(3) Uani 1 1 d . . . H29A H 0.9366 -0.0158 0.3811 0.190 Uiso 1 1 calc R . . H29B H 0.9367 -0.0951 0.3482 0.190 Uiso 1 1 calc R . . H29C H 0.8770 -0.0896 0.3949 0.190 Uiso 1 1 calc R . . C30 C 1.1118(3) 0.1364(4) 0.38142(19) 0.0604(15) Uani 1 1 d . . . C31 C 1.1966(4) 0.1383(4) 0.3944(2) 0.0680(16) Uani 1 1 d . . . H31A H 1.2145 0.1707 0.4209 0.082 Uiso 1 1 calc R . . C32 C 1.2547(4) 0.0927(4) 0.3684(2) 0.0775(19) Uani 1 1 d . . . H32A H 1.3121 0.0946 0.3772 0.093 Uiso 1 1 calc R . . C33 C 1.2289(4) 0.0444(4) 0.3297(2) 0.0710(17) Uani 1 1 d . . . H33A H 1.2686 0.0129 0.3124 0.085 Uiso 1 1 calc R . . C34 C 1.1455(4) 0.0426(4) 0.3164(2) 0.0650(15) Uani 1 1 d . . . H34A H 1.1279 0.0102 0.2898 0.078 Uiso 1 1 calc R . . C35 C 1.0872(4) 0.0880(3) 0.3420(2) 0.0629(15) Uani 1 1 d . . . H35A H 1.0300 0.0863 0.3327 0.075 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 0.0355(4) 0.0790(5) 0.0513(4) -0.0284(3) -0.0022(3) 0.0026(4) P1 0.0458(9) 0.168(2) 0.1002(14) -0.0804(14) -0.0146(9) 0.0124(11) N1 0.044(2) 0.046(2) 0.036(2) -0.0115(17) 0.0010(18) 0.0022(19) N2 0.037(2) 0.038(2) 0.034(2) -0.0064(16) -0.0002(17) -0.0020(17) C1 0.040(3) 0.058(3) 0.041(3) -0.015(2) 0.002(2) 0.009(3) C2 0.070(4) 0.066(4) 0.051(3) -0.005(3) -0.009(3) 0.024(3) C3 0.089(5) 0.110(6) 0.050(4) -0.012(4) -0.017(3) 0.040(5) C4 0.069(5) 0.138(7) 0.071(5) -0.048(5) -0.017(4) 0.018(5) C5 0.087(5) 0.094(5) 0.077(5) -0.033(4) -0.012(4) -0.015(4) C6 0.060(4) 0.070(4) 0.055(3) -0.019(3) -0.005(3) -0.013(3) C7 0.128(6) 0.070(5) 0.069(4) 0.004(3) -0.012(4) 0.028(4) C8 0.254(13) 0.115(7) 0.121(7) 0.024(6) 0.051(8) -0.031(8) C9 0.213(12) 0.094(7) 0.212(11) 0.003(7) -0.035(9) 0.071(7) C10 0.136(7) 0.077(5) 0.075(5) -0.005(4) -0.015(5) -0.044(5) C11 0.228(12) 0.125(7) 0.126(7) 0.002(6) 0.069(8) -0.046(8) C12 0.167(9) 0.084(6) 0.157(8) 0.001(6) -0.027(7) 0.008(6) C13 0.040(3) 0.039(3) 0.043(3) -0.001(2) 0.007(2) 0.005(2) C14 0.060(4) 0.083(4) 0.051(3) -0.017(3) 0.009(3) 0.011(3) C15 0.034(2) 0.050(3) 0.049(3) -0.008(2) 0.002(2) -0.005(2) C16 0.035(3) 0.045(3) 0.039(3) -0.004(2) 0.001(2) 0.000(2) C17 0.038(3) 0.096(4) 0.068(4) -0.030(3) -0.007(3) 0.004(3) C18 0.030(2) 0.043(3) 0.038(3) -0.010(2) -0.003(2) -0.001(2) C19 0.048(3) 0.043(3) 0.050(3) -0.009(2) 0.006(2) -0.005(2) C20 0.049(3) 0.070(4) 0.052(3) -0.006(3) 0.014(3) -0.009(3) C21 0.048(3) 0.076(4) 0.061(4) -0.026(3) 0.007(3) 0.012(3) C22 0.055(3) 0.052(3) 0.064(3) -0.014(3) -0.003(3) 0.011(3) C23 0.041(3) 0.041(3) 0.045(3) -0.010(2) -0.004(2) 0.000(2) C24 0.104(5) 0.038(3) 0.070(4) -0.001(3) 0.026(3) -0.010(3) C25 0.158(9) 0.080(6) 0.232(11) -0.034(6) 0.061(8) -0.069(6) C26 0.302(14) 0.075(5) 0.088(5) 0.021(4) 0.011(7) 0.055(7) C27 0.088(4) 0.044(3) 0.063(3) -0.002(3) 0.007(3) -0.009(3) C28 0.137(7) 0.075(5) 0.108(6) 0.003(4) 0.011(5) -0.045(5) C29 0.150(8) 0.119(7) 0.111(6) 0.065(5) -0.030(6) -0.015(6) C30 0.038(3) 0.085(4) 0.058(3) -0.018(3) 0.001(3) -0.004(3) C31 0.047(3) 0.097(5) 0.060(4) -0.017(3) -0.004(3) -0.009(3) C32 0.039(3) 0.119(6) 0.075(4) 0.003(4) 0.006(3) -0.001(4) C33 0.062(4) 0.081(4) 0.069(4) -0.003(3) 0.017(3) 0.008(3) C34 0.060(4) 0.076(4) 0.059(3) -0.007(3) 0.005(3) -0.002(3) C35 0.046(3) 0.080(4) 0.063(4) -0.011(3) -0.003(3) 0.000(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 N2 1.871(3) . ? Ni1 N1 1.912(4) . ? Ni1 P1 2.1596(17) . ? P1 C30 1.813(5) . ? N1 C13 1.318(6) . ? N1 C1 1.435(5) . ? N2 C16 1.325(5) . ? N2 C18 1.434(5) . ? C1 C2 1.382(7) . ? C1 C6 1.418(7) . ? C2 C3 1.401(8) . ? C2 C7 1.520(9) . ? C3 C4 1.376(10) . ? C4 C5 1.342(9) . ? C5 C6 1.378(8) . ? C6 C10 1.514(9) . ? C7 C9 1.507(10) . ? C7 C8 1.520(10) . ? C10 C12 1.505(10) . ? C10 C11 1.530(10) . ? C13 C15 1.401(6) . ? C13 C14 1.502(6) . ? C15 C16 1.386(6) . ? C16 C17 1.510(6) . ? C18 C19 1.396(6) . ? C18 C23 1.408(6) . ? C19 C20 1.383(6) . ? C19 C24 1.522(7) . ? C20 C21 1.373(7) . ? C21 C22 1.364(7) . ? C22 C23 1.374(6) . ? C23 C27 1.514(7) . ? C24 C26 1.509(9) . ? C24 C25 1.517(10) . ? C27 C29 1.517(9) . ? C27 C28 1.518(8) . ? C30 C31 1.373(7) . ? C30 C35 1.375(7) . ? C31 C32 1.366(8) . ? C32 C33 1.366(8) . ? C33 C34 1.355(8) . ? C34 C35 1.362(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 N2 Ni1 N1 97.24(16) . . ? N2 Ni1 P1 152.76(12) . . ? N1 Ni1 P1 109.98(12) . . ? C30 P1 Ni1 117.42(18) . . ? C13 N1 C1 120.3(4) . . ? C13 N1 Ni1 123.5(3) . . ? C1 N1 Ni1 116.2(3) . . ? C16 N2 C18 121.6(4) . . ? C16 N2 Ni1 125.3(3) . . ? C18 N2 Ni1 113.1(3) . . ? C2 C1 C6 120.6(5) . . ? C2 C1 N1 120.5(5) . . ? C6 C1 N1 118.7(5) . . ? C1 C2 C3 118.6(6) . . ? C1 C2 C7 121.7(5) . . ? C3 C2 C7 119.7(6) . . ? C4 C3 C2 120.3(6) . . ? C5 C4 C3 120.5(6) . . ? C4 C5 C6 122.2(7) . . ? C5 C6 C1 117.7(6) . . ? C5 C6 C10 119.9(6) . . ? C1 C6 C10 122.3(5) . . ? C9 C7 C8 111.2(7) . . ? C9 C7 C2 113.1(7) . . ? C8 C7 C2 112.3(6) . . ? C12 C10 C6 113.1(6) . . ? C12 C10 C11 110.5(7) . . ? C6 C10 C11 111.3(7) . . ? N1 C13 C15 122.8(4) . . ? N1 C13 C14 120.3(4) . . ? C15 C13 C14 117.0(4) . . ? C16 C15 C13 129.2(4) . . ? N2 C16 C15 122.1(4) . . ? N2 C16 C17 119.7(4) . . ? C15 C16 C17 118.2(4) . . ? C19 C18 C23 120.3(4) . . ? C19 C18 N2 119.7(4) . . ? C23 C18 N2 119.6(4) . . ? C20 C19 C18 118.4(4) . . ? C20 C19 C24 120.2(5) . . ? C18 C19 C24 121.4(4) . . ? C21 C20 C19 121.5(5) . . ? C22 C21 C20 119.4(5) . . ? C21 C22 C23 122.0(5) . . ? C22 C23 C18 118.3(5) . . ? C22 C23 C27 119.9(5) . . ? C18 C23 C27 121.8(4) . . ? C26 C24 C25 112.8(7) . . ? C26 C24 C19 112.2(5) . . ? C25 C24 C19 110.1(6) . . ? C23 C27 C29 111.5(5) . . ? C23 C27 C28 112.0(5) . . ? C29 C27 C28 110.0(6) . . ? C31 C30 C35 118.6(5) . . ? C31 C30 P1 123.1(4) . . ? C35 C30 P1 118.2(4) . . ? C32 C31 C30 120.2(5) . . ? C31 C32 C33 120.3(6) . . ? C34 C33 C32 119.8(6) . . ? C33 C34 C35 120.2(6) . . ? C34 C35 C30 120.8(5) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.578 _refine_diff_density_min -0.582 _refine_diff_density_rms 0.071 #===end data_(NacNac)Ni(PHPh2) _database_code_depnum_ccdc_archive 'CCDC 284030' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C41 H52 N2 Ni P' _chemical_formula_weight 662.53 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' 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 13.3110(16) _cell_length_b 20.471(2) _cell_length_c 14.5076(17) _cell_angle_alpha 90.00 _cell_angle_beta 101.689(2) _cell_angle_gamma 90.00 _cell_volume 3871.2(8) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.21 _exptl_crystal_density_diffrn 1.137 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1420 _exptl_absorpt_coefficient_mu 0.571 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.865586 _exptl_absorpt_correction_T_max 1.00000 _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 36847 _diffrn_reflns_av_R_equivalents 0.0770 _diffrn_reflns_av_sigmaI/netI 0.0625 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6799 _reflns_number_gt 3732 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1014P)^2^+3.7878P] 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_number_reflns 6799 _refine_ls_number_parameters 418 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1294 _refine_ls_R_factor_gt 0.0649 _refine_ls_wR_factor_ref 0.1950 _refine_ls_wR_factor_gt 0.1504 _refine_ls_goodness_of_fit_ref 0.967 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.003 _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 1.02268(5) 0.79345(3) 0.81040(4) 0.0609(3) Uani 1 1 d . . . P1 P 0.92289(14) 0.73913(8) 0.69849(12) 0.0647(5) Uani 0.86 1 d PD . . H30A H 0.8313 0.7336 0.7062 0.091(19) Uiso 0.86 1 d P . . P1A P 1.0205(11) 0.7390(5) 0.6928(7) 0.091(4) Uani 0.14 1 d PD . . N1 N 0.9981(3) 0.77311(18) 0.9330(3) 0.0555(10) Uani 1 1 d . . . N2 N 1.1106(3) 0.86517(18) 0.8461(3) 0.0589(10) Uani 1 1 d . . . C1 C 0.9187(4) 0.7262(2) 0.9369(3) 0.0588(13) Uani 1 1 d . . . C2 C 0.9429(4) 0.6603(2) 0.9543(4) 0.0682(14) Uani 1 1 d . . . C3 C 0.8615(6) 0.6161(3) 0.9469(4) 0.0889(18) Uani 1 1 d . . . H3A H 0.8754 0.5718 0.9565 0.107 Uiso 1 1 calc R . . C4 C 0.7625(5) 0.6368(4) 0.9260(5) 0.098(2) Uani 1 1 d . . . H4A H 0.7095 0.6066 0.9215 0.118 Uiso 1 1 calc R . . C5 C 0.7403(5) 0.7015(4) 0.9114(4) 0.0875(18) Uani 1 1 d . . . H5A H 0.6721 0.7147 0.8980 0.105 Uiso 1 1 calc R . . C6 C 0.8165(4) 0.7478(3) 0.9161(4) 0.0695(14) Uani 1 1 d . . . C7 C 1.0530(5) 0.6365(3) 0.9819(5) 0.0886(18) Uani 1 1 d . . . H7A H 1.0978 0.6749 0.9873 0.106 Uiso 1 1 calc R . . C8 C 1.0819(6) 0.5918(4) 0.9076(6) 0.133(3) Uani 1 1 d . . . H8A H 1.0688 0.6136 0.8478 0.199 Uiso 1 1 calc R . . H8B H 1.0417 0.5525 0.9033 0.199 Uiso 1 1 calc R . . H8C H 1.1534 0.5809 0.9249 0.199 Uiso 1 1 calc R . . C9 C 1.0742(7) 0.6017(4) 1.0771(6) 0.146(3) Uani 1 1 d . . . H9A H 1.0561 0.6299 1.1240 0.219 Uiso 1 1 calc R . . H9B H 1.1457 0.5908 1.0942 0.219 Uiso 1 1 calc R . . H9C H 1.0339 0.5624 1.0728 0.219 Uiso 1 1 calc R . . C10 C 0.7898(4) 0.8188(3) 0.9023(5) 0.0890(18) Uani 1 1 d . . . H10A H 0.8526 0.8422 0.8971 0.107 Uiso 1 1 calc R . . C11 C 0.7102(7) 0.8335(4) 0.8144(6) 0.168(4) Uani 1 1 d . . . H11A H 0.7321 0.8155 0.7606 0.252 Uiso 1 1 calc R . . H11B H 0.7023 0.8799 0.8070 0.252 Uiso 1 1 calc R . . H11C H 0.6458 0.8143 0.8199 0.252 Uiso 1 1 calc R . . C12 C 0.7513(10) 0.8478(4) 0.9829(6) 0.195(5) Uani 1 1 d . . . H12A H 0.7998 0.8395 1.0404 0.293 Uiso 1 1 calc R . . H12B H 0.6865 0.8284 0.9866 0.293 Uiso 1 1 calc R . . H12C H 0.7428 0.8940 0.9738 0.293 Uiso 1 1 calc R . . C13 C 1.0229(5) 0.7847(3) 1.1055(4) 0.096(2) Uani 1 1 d . . . H13A H 0.9580 0.8027 1.1118 0.143 Uiso 1 1 calc R . . H13B H 1.0760 0.8015 1.1547 0.143 Uiso 1 1 calc R . . H13C H 1.0207 0.7380 1.1101 0.143 Uiso 1 1 calc R . . C14 C 1.0450(4) 0.8036(2) 1.0113(4) 0.0629(13) Uani 1 1 d . . . C15 C 1.1142(4) 0.8541(3) 1.0104(4) 0.0692(14) Uani 1 1 d . . . H15A H 1.1460 0.8698 1.0693 0.083 Uiso 1 1 calc R . . C16 C 1.1430(4) 0.8848(2) 0.9334(4) 0.0663(14) Uani 1 1 d . . . C17 C 1.2121(6) 0.9440(3) 0.9542(5) 0.114(3) Uani 1 1 d . . . H17A H 1.2809 0.9320 0.9504 0.172 Uiso 1 1 calc R . . H17B H 1.2112 0.9597 1.0163 0.172 Uiso 1 1 calc R . . H17C H 1.1881 0.9776 0.9090 0.172 Uiso 1 1 calc R . . C18 C 1.1335(4) 0.9021(2) 0.7692(4) 0.0656(14) Uani 1 1 d . . . C19 C 1.2224(5) 0.8872(3) 0.7349(4) 0.0768(16) Uani 1 1 d . . . C20 C 1.2410(6) 0.9237(4) 0.6593(5) 0.105(2) Uani 1 1 d . . . H20A H 1.2995 0.9150 0.6357 0.126 Uiso 1 1 calc R . . C21 C 1.1771(8) 0.9711(4) 0.6193(5) 0.120(3) Uani 1 1 d . . . H21A H 1.1926 0.9950 0.5694 0.144 Uiso 1 1 calc R . . C22 C 1.0881(7) 0.9846(3) 0.6518(5) 0.111(2) Uani 1 1 d . . . H22A H 1.0435 1.0168 0.6226 0.133 Uiso 1 1 calc R . . C23 C 1.0655(5) 0.9504(3) 0.7275(4) 0.0836(17) Uani 1 1 d . . . C24 C 1.2920(4) 0.8325(3) 0.7741(5) 0.0930(19) Uani 1 1 d . . . H24A H 1.2670 0.8146 0.8279 0.112 Uiso 1 1 calc R . . C25 C 1.2864(8) 0.7784(4) 0.7019(6) 0.158(4) Uani 1 1 d . . . H25A H 1.2163 0.7655 0.6804 0.238 Uiso 1 1 calc R . . H25B H 1.3257 0.7416 0.7301 0.238 Uiso 1 1 calc R . . H25C H 1.3139 0.7938 0.6496 0.238 Uiso 1 1 calc R . . C26 C 1.4030(7) 0.8518(6) 0.8086(10) 0.234(6) Uani 1 1 d . . . H26A H 1.4071 0.8859 0.8545 0.351 Uiso 1 1 calc R . . H26B H 1.4310 0.8670 0.7565 0.351 Uiso 1 1 calc R . . H26C H 1.4413 0.8145 0.8365 0.351 Uiso 1 1 calc R . . C27 C 0.9662(6) 0.9653(3) 0.7612(6) 0.112(2) Uani 1 1 d . . . H27A H 0.9608 0.9344 0.8116 0.135 Uiso 1 1 calc R . . C28 C 0.8724(7) 0.9572(5) 0.6839(8) 0.166(4) Uani 1 1 d . . . H28A H 0.8121 0.9671 0.7081 0.249 Uiso 1 1 calc R . . H28B H 0.8687 0.9130 0.6614 0.249 Uiso 1 1 calc R . . H28C H 0.8766 0.9864 0.6331 0.249 Uiso 1 1 calc R . . C29 C 0.9660(10) 1.0336(5) 0.8003(8) 0.216(6) Uani 1 1 d . . . H29A H 0.9025 1.0412 0.8202 0.324 Uiso 1 1 calc R . . H29B H 0.9734 1.0646 0.7525 0.324 Uiso 1 1 calc R . . H29C H 1.0220 1.0383 0.8532 0.324 Uiso 1 1 calc R . . C36 C 0.9104(5) 0.7767(2) 0.5838(4) 0.0728(15) Uani 1 1 d D . . C37 C 0.8207(5) 0.7700(3) 0.5179(5) 0.0903(19) Uani 1 1 d . . . H37A H 0.7691 0.7433 0.5317 0.108 Uiso 1 1 calc R . . C41 C 0.9846(5) 0.8166(3) 0.5578(5) 0.0905(18) Uani 1 1 d D . . H41A H 1.0461 0.8230 0.6005 0.109 Uiso 1 1 calc R . . C40 C 0.9707(6) 0.8467(3) 0.4722(5) 0.0945(19) Uani 1 1 d . . . H40A H 1.0228 0.8718 0.4562 0.113 Uiso 1 1 calc R . . C30 C 0.9473(7) 0.6545(3) 0.6743(5) 0.104(2) Uani 1 1 d D . . C38 C 0.8053(6) 0.8009(3) 0.4340(5) 0.101(2) Uani 1 1 d . . . H38A H 0.7432 0.7960 0.3916 0.122 Uiso 1 1 calc R . . C39 C 0.8804(7) 0.8394(3) 0.4113(5) 0.099(2) Uani 1 1 d . . . H39A H 0.8693 0.8606 0.3534 0.119 Uiso 1 1 calc R . . C35 C 1.0169(9) 0.6298(5) 0.6319(8) 0.168(4) Uani 1 1 d D . . H35A H 1.0597 0.6592 0.6095 0.202 Uiso 1 1 calc R . . C31 C 0.8810(7) 0.6085(4) 0.7013(6) 0.133(3) Uani 1 1 d . . . H31A H 0.8275 0.6226 0.7289 0.160 Uiso 1 1 calc R . . C33 C 0.9712(15) 0.5253(7) 0.6457(11) 0.198(9) Uani 1 1 d . . . H33A H 0.9814 0.4810 0.6363 0.238 Uiso 1 1 calc R . . C34 C 1.0320(16) 0.5660(7) 0.6178(11) 0.242(9) Uani 1 1 d . . . H34A H 1.0846 0.5519 0.5890 0.290 Uiso 1 1 calc R . . C32 C 0.8938(12) 0.5423(6) 0.6875(10) 0.185(6) Uani 1 1 d . . . H32A H 0.8510 0.5113 0.7063 0.222 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 0.0659(4) 0.0541(4) 0.0678(4) -0.0124(3) 0.0256(3) -0.0117(3) P1 0.0718(11) 0.0578(10) 0.0696(11) -0.0112(8) 0.0266(9) -0.0176(9) P1A 0.137(12) 0.055(7) 0.079(8) -0.005(5) 0.019(8) -0.009(7) N1 0.052(2) 0.049(2) 0.067(3) -0.0010(19) 0.016(2) -0.0009(18) N2 0.063(3) 0.050(2) 0.069(3) -0.007(2) 0.026(2) -0.0071(19) C1 0.061(3) 0.056(3) 0.062(3) 0.002(2) 0.020(3) -0.007(2) C2 0.070(4) 0.054(3) 0.082(4) 0.002(3) 0.020(3) -0.011(3) C3 0.107(5) 0.066(4) 0.100(5) -0.002(3) 0.035(4) -0.020(4) C4 0.075(5) 0.108(6) 0.115(5) -0.002(4) 0.028(4) -0.038(4) C5 0.064(4) 0.106(5) 0.095(5) 0.007(4) 0.023(3) -0.007(4) C6 0.061(3) 0.081(4) 0.070(4) 0.005(3) 0.021(3) -0.008(3) C7 0.088(4) 0.052(3) 0.124(5) -0.003(3) 0.019(4) 0.003(3) C8 0.111(6) 0.122(6) 0.164(8) -0.024(6) 0.026(5) 0.036(5) C9 0.154(8) 0.134(7) 0.131(7) 0.017(6) -0.017(6) 0.024(6) C10 0.061(4) 0.092(4) 0.114(5) 0.026(4) 0.018(3) 0.016(3) C11 0.199(10) 0.150(8) 0.139(7) 0.011(6) -0.003(7) 0.083(7) C12 0.344(16) 0.119(7) 0.127(7) -0.007(6) 0.060(9) 0.085(9) C13 0.119(5) 0.108(5) 0.065(4) -0.001(3) 0.029(4) -0.027(4) C14 0.061(3) 0.065(3) 0.064(3) 0.001(3) 0.016(3) -0.002(3) C15 0.073(3) 0.068(3) 0.066(3) -0.012(3) 0.012(3) -0.012(3) C16 0.071(3) 0.053(3) 0.078(4) -0.010(3) 0.023(3) -0.012(3) C17 0.140(6) 0.108(5) 0.098(5) -0.028(4) 0.031(4) -0.070(5) C18 0.075(4) 0.053(3) 0.077(4) -0.007(3) 0.036(3) -0.016(3) C19 0.081(4) 0.070(4) 0.087(4) -0.007(3) 0.034(3) -0.023(3) C20 0.115(6) 0.097(5) 0.118(6) 0.002(5) 0.061(5) -0.026(5) C21 0.171(8) 0.096(6) 0.111(6) 0.014(5) 0.071(6) -0.036(6) C22 0.158(7) 0.058(4) 0.125(6) 0.021(4) 0.049(5) -0.005(4) C23 0.116(5) 0.050(3) 0.094(4) 0.002(3) 0.043(4) -0.001(3) C24 0.064(4) 0.112(5) 0.112(5) -0.003(4) 0.040(4) -0.006(4) C25 0.231(11) 0.132(7) 0.122(7) -0.005(6) 0.060(7) 0.077(7) C26 0.090(7) 0.247(14) 0.341(18) 0.051(12) -0.015(8) -0.025(8) C27 0.120(6) 0.086(5) 0.142(7) 0.029(5) 0.053(6) 0.034(4) C28 0.125(8) 0.139(8) 0.240(12) 0.008(8) 0.051(8) 0.035(6) C29 0.222(12) 0.185(11) 0.252(14) -0.089(10) 0.073(10) 0.049(10) C36 0.097(4) 0.049(3) 0.071(4) -0.008(3) 0.013(3) -0.006(3) C37 0.104(5) 0.072(4) 0.100(5) -0.011(4) 0.033(4) -0.028(4) C41 0.078(4) 0.086(4) 0.100(5) -0.006(4) 0.002(4) -0.014(3) C40 0.104(5) 0.086(5) 0.096(5) 0.019(4) 0.028(4) -0.015(4) C30 0.178(8) 0.048(4) 0.084(5) 0.001(3) 0.016(5) -0.017(4) C38 0.098(5) 0.093(5) 0.105(6) -0.006(4) 0.001(4) 0.000(4) C39 0.130(6) 0.079(5) 0.083(5) 0.013(4) 0.008(5) 0.004(4) C35 0.242(12) 0.104(7) 0.188(10) 0.000(7) 0.114(9) 0.020(7) C31 0.165(8) 0.099(6) 0.120(6) 0.018(5) -0.010(5) -0.004(6) C33 0.30(2) 0.084(8) 0.181(13) -0.027(8) -0.026(13) 0.042(11) C34 0.41(3) 0.114(10) 0.243(15) -0.011(11) 0.164(16) 0.059(13) C32 0.224(15) 0.094(9) 0.195(13) 0.055(8) -0.058(10) -0.058(8) _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 N2 1.884(4) . ? Ni1 N1 1.919(4) . ? Ni1 P1A 2.034(11) . ? Ni1 P1 2.1824(18) . ? P1 P1A 1.319(14) . ? P1 C30 1.809(7) . ? P1 C36 1.810(6) . ? P1A C30 1.976(11) . ? P1A C36 2.075(12) . ? N1 C14 1.335(6) . ? N1 C1 1.437(6) . ? N2 C16 1.317(6) . ? N2 C18 1.429(6) . ? C1 C2 1.397(7) . ? C1 C6 1.404(7) . ? C2 C3 1.399(7) . ? C2 C7 1.520(8) . ? C3 C4 1.359(9) . ? C4 C5 1.364(8) . ? C5 C6 1.381(8) . ? C6 C10 1.499(8) . ? C7 C8 1.521(9) . ? C7 C9 1.530(9) . ? C10 C12 1.492(10) . ? C10 C11 1.513(9) . ? C13 C14 1.506(7) . ? C14 C15 1.386(7) . ? C15 C16 1.402(7) . ? C16 C17 1.513(7) . ? C18 C23 1.393(8) . ? C18 C19 1.408(7) . ? C19 C20 1.389(8) . ? C19 C24 1.489(8) . ? C20 C21 1.342(10) . ? C21 C22 1.389(10) . ? C22 C23 1.386(8) . ? C23 C27 1.529(9) . ? C24 C26 1.513(10) . ? C24 C25 1.516(9) . ? C27 C28 1.508(11) . ? C27 C29 1.509(11) . ? C36 C37 1.377(8) . ? C36 C41 1.390(8) . ? C37 C38 1.350(9) . ? C41 C40 1.365(8) . ? C40 C39 1.349(9) . ? C30 C35 1.314(11) . ? C30 C31 1.399(11) . ? C38 C39 1.365(9) . ? C35 C34 1.344(13) . ? C31 C32 1.385(14) . ? C33 C34 1.284(19) . ? C33 C32 1.344(18) . ? 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 N2 Ni1 N1 97.35(17) . . ? N2 Ni1 P1A 124.1(4) . . ? N1 Ni1 P1A 133.1(3) . . ? N2 Ni1 P1 148.45(14) . . ? N1 Ni1 P1 112.74(13) . . ? P1A Ni1 P1 36.2(4) . . ? P1A P1 C30 76.6(5) . . ? P1A P1 C36 81.5(5) . . ? C30 P1 C36 102.4(3) . . ? P1A P1 Ni1 65.7(4) . . ? C30 P1 Ni1 121.7(3) . . ? C36 P1 Ni1 113.3(2) . . ? P1 P1A C30 63.0(5) . . ? P1 P1A Ni1 78.0(6) . . ? C30 P1A Ni1 121.1(7) . . ? P1 P1A C36 59.6(5) . . ? C30 P1A C36 88.3(5) . . ? Ni1 P1A C36 108.8(6) . . ? C14 N1 C1 120.0(4) . . ? C14 N1 Ni1 123.3(3) . . ? C1 N1 Ni1 116.5(3) . . ? C16 N2 C18 120.6(4) . . ? C16 N2 Ni1 124.5(3) . . ? C18 N2 Ni1 114.6(3) . . ? C2 C1 C6 121.4(5) . . ? C2 C1 N1 120.5(4) . . ? C6 C1 N1 117.9(4) . . ? C1 C2 C3 117.7(5) . . ? C1 C2 C7 122.1(5) . . ? C3 C2 C7 120.2(5) . . ? C4 C3 C2 121.1(6) . . ? C3 C4 C5 120.5(6) . . ? C4 C5 C6 121.7(6) . . ? C5 C6 C1 117.6(5) . . ? C5 C6 C10 120.5(5) . . ? C1 C6 C10 121.9(5) . . ? C2 C7 C8 112.0(5) . . ? C2 C7 C9 112.2(6) . . ? C8 C7 C9 109.4(6) . . ? C12 C10 C6 113.0(6) . . ? C12 C10 C11 106.8(7) . . ? C6 C10 C11 114.3(6) . . ? N1 C14 C15 122.6(5) . . ? N1 C14 C13 120.6(5) . . ? C15 C14 C13 116.9(5) . . ? C14 C15 C16 129.2(5) . . ? N2 C16 C15 122.7(5) . . ? N2 C16 C17 120.2(5) . . ? C15 C16 C17 117.0(5) . . ? C23 C18 C19 121.3(5) . . ? C23 C18 N2 119.5(5) . . ? C19 C18 N2 119.2(5) . . ? C20 C19 C18 117.3(6) . . ? C20 C19 C24 120.6(6) . . ? C18 C19 C24 122.0(5) . . ? C21 C20 C19 122.1(7) . . ? C20 C21 C22 120.4(7) . . ? C23 C22 C21 120.3(7) . . ? C22 C23 C18 118.5(6) . . ? C22 C23 C27 119.5(6) . . ? C18 C23 C27 122.0(5) . . ? C19 C24 C26 114.9(7) . . ? C19 C24 C25 110.2(6) . . ? C26 C24 C25 109.0(8) . . ? C28 C27 C29 108.4(8) . . ? C28 C27 C23 112.3(7) . . ? C29 C27 C23 111.9(7) . . ? C37 C36 C41 115.7(5) . . ? C37 C36 P1 120.1(5) . . ? C41 C36 P1 124.1(5) . . ? C37 C36 P1A 150.6(5) . . ? C41 C36 P1A 89.7(5) . . ? P1 C36 P1A 38.9(4) . . ? C38 C37 C36 122.1(6) . . ? C40 C41 C36 122.6(6) . . ? C39 C40 C41 119.0(6) . . ? C35 C30 C31 114.6(7) . . ? C35 C30 P1 129.1(7) . . ? C31 C30 P1 116.3(7) . . ? C35 C30 P1A 91.4(7) . . ? C31 C30 P1A 150.8(7) . . ? P1 C30 P1A 40.5(4) . . ? C37 C38 C39 120.2(7) . . ? C40 C39 C38 120.3(7) . . ? C30 C35 C34 125.9(11) . . ? C32 C31 C30 121.0(11) . . ? C34 C33 C32 124.3(16) . . ? C33 C34 C35 117.4(16) . . ? C33 C32 C31 116.6(13) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.576 _refine_diff_density_min -0.365 _refine_diff_density_rms 0.057 #===end data_(NacNac)Fe(CH2CPh2) _database_code_depnum_ccdc_archive 'CCDC 284031' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C43 H53 Fe N2' _chemical_formula_weight 653.72 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' Fe Fe 0.3463 0.8444 '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 11.970(4) _cell_length_b 22.830(8) _cell_length_c 13.765(5) _cell_angle_alpha 90.00 _cell_angle_beta 97.209(9) _cell_angle_gamma 90.00 _cell_volume 3732(2) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.19 _exptl_crystal_density_diffrn 1.163 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1404 _exptl_absorpt_coefficient_mu 0.435 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.473791 _exptl_absorpt_correction_T_max 1.0000 _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 17836 _diffrn_reflns_av_R_equivalents 0.0299 _diffrn_reflns_av_sigmaI/netI 0.0307 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 23.50 _reflns_number_total 5380 _reflns_number_gt 4403 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0633P)^2^+0.9372P] 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_number_reflns 5380 _refine_ls_number_parameters 417 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0577 _refine_ls_R_factor_gt 0.0397 _refine_ls_wR_factor_ref 0.1082 _refine_ls_wR_factor_gt 0.0983 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.002 _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 Fe1 Fe 0.92239(2) 0.908495(13) 0.75667(2) 0.05340(13) Uani 1 1 d . . . N1 N 0.97484(14) 0.86757(8) 0.64507(14) 0.0553(4) Uani 1 1 d . . . N2 N 0.75845(14) 0.89895(8) 0.70905(14) 0.0563(5) Uani 1 1 d . . . C1 C 1.08999(17) 0.84786(10) 0.65652(18) 0.0606(6) Uani 1 1 d . . . C2 C 1.11467(19) 0.79236(11) 0.6954(2) 0.0715(7) Uani 1 1 d . . . C3 C 1.2274(2) 0.77519(13) 0.7107(3) 0.0952(10) Uani 1 1 d . . . H3A H 1.2467 0.7387 0.7377 0.114 Uiso 1 1 calc R . . C4 C 1.3097(2) 0.81215(16) 0.6859(3) 0.1083(12) Uani 1 1 d . . . H4A H 1.3845 0.8001 0.6953 0.130 Uiso 1 1 calc R . . C5 C 1.2835(2) 0.86605(15) 0.6479(3) 0.0944(9) Uani 1 1 d . . . H5A H 1.3411 0.8900 0.6315 0.113 Uiso 1 1 calc R . . C6 C 1.17396(19) 0.88632(12) 0.6328(2) 0.0723(7) Uani 1 1 d . . . C7 C 1.1481(2) 0.94725(12) 0.5933(2) 0.0810(8) Uani 1 1 d . . . H7A H 1.0791 0.9600 0.6186 0.097 Uiso 1 1 calc R . . C8 C 1.1242(4) 0.94827(19) 0.4833(3) 0.1361(15) Uani 1 1 d . . . H8A H 1.0681 0.9194 0.4620 0.204 Uiso 1 1 calc R . . H8B H 1.1921 0.9397 0.4556 0.204 Uiso 1 1 calc R . . H8C H 1.0973 0.9864 0.4621 0.204 Uiso 1 1 calc R . . C9 C 1.2377(3) 0.99222(15) 0.6263(3) 0.1108(11) Uani 1 1 d . . . H9A H 1.2528 0.9919 0.6964 0.166 Uiso 1 1 calc R . . H9B H 1.2118 1.0304 0.6045 0.166 Uiso 1 1 calc R . . H9C H 1.3054 0.9829 0.5988 0.166 Uiso 1 1 calc R . . C10 C 1.0252(2) 0.75027(11) 0.7219(2) 0.0800(8) Uani 1 1 d . . . H10A H 0.9521 0.7683 0.7001 0.096 Uiso 1 1 calc R . . C11 C 1.0272(3) 0.69179(15) 0.6696(3) 0.1270(14) Uani 1 1 d . . . H11A H 0.9691 0.6669 0.6889 0.191 Uiso 1 1 calc R . . H11B H 1.0991 0.6735 0.6867 0.191 Uiso 1 1 calc R . . H11C H 1.0144 0.6980 0.6001 0.191 Uiso 1 1 calc R . . C12 C 1.0307(3) 0.74115(17) 0.8296(3) 0.1283(14) Uani 1 1 d . . . H12A H 1.0288 0.7784 0.8617 0.192 Uiso 1 1 calc R . . H12B H 1.0993 0.7212 0.8533 0.192 Uiso 1 1 calc R . . H12C H 0.9676 0.7180 0.8432 0.192 Uiso 1 1 calc R . . C13 C 0.90620(19) 0.85082(10) 0.56626(18) 0.0605(6) Uani 1 1 d . . . C14 C 0.79133(19) 0.85947(10) 0.55435(18) 0.0635(6) Uani 1 1 d . . . H14A H 0.7552 0.8514 0.4920 0.076 Uiso 1 1 calc R . . C15 C 0.72157(18) 0.87834(11) 0.62088(18) 0.0616(6) Uani 1 1 d . . . C16 C 0.5965(2) 0.87290(15) 0.5876(2) 0.0909(9) Uani 1 1 d . . . H16A H 0.5564 0.9011 0.6216 0.136 Uiso 1 1 calc R . . H16B H 0.5717 0.8342 0.6016 0.136 Uiso 1 1 calc R . . H16C H 0.5822 0.8800 0.5184 0.136 Uiso 1 1 calc R . . C17 C 0.9522(2) 0.81747(13) 0.4856(2) 0.0835(8) Uani 1 1 d . . . H17A H 1.0245 0.8330 0.4760 0.125 Uiso 1 1 calc R . . H17B H 0.9015 0.8213 0.4260 0.125 Uiso 1 1 calc R . . H17C H 0.9597 0.7769 0.5032 0.125 Uiso 1 1 calc R . . C18 C 0.67647(18) 0.91100(11) 0.77423(18) 0.0639(6) Uani 1 1 d . . . C19 C 0.6272(2) 0.96647(13) 0.7745(2) 0.0763(7) Uani 1 1 d . . . C20 C 0.5459(2) 0.97542(17) 0.8359(3) 0.1017(10) Uani 1 1 d . . . H20A H 0.5104 1.0116 0.8363 0.122 Uiso 1 1 calc R . . C21 C 0.5171(3) 0.9318(2) 0.8960(3) 0.1094(11) Uani 1 1 d . . . H21A H 0.4615 0.9384 0.9362 0.131 Uiso 1 1 calc R . . C22 C 0.5692(2) 0.87890(17) 0.8975(2) 0.0952(9) Uani 1 1 d . . . H22A H 0.5492 0.8500 0.9397 0.114 Uiso 1 1 calc R . . C23 C 0.6519(2) 0.86685(12) 0.8376(2) 0.0729(7) Uani 1 1 d . . . C24 C 0.6581(2) 1.01637(13) 0.7115(3) 0.0905(9) Uani 1 1 d . . . H24A H 0.7199 1.0029 0.6767 0.109 Uiso 1 1 calc R . . C25 C 0.6998(3) 1.07011(15) 0.7708(3) 0.1248(14) Uani 1 1 d . . . H25A H 0.7621 1.0594 0.8183 0.187 Uiso 1 1 calc R . . H25B H 0.6400 1.0854 0.8037 0.187 Uiso 1 1 calc R . . H25C H 0.7235 1.0994 0.7278 0.187 Uiso 1 1 calc R . . C26 C 0.5619(3) 1.03527(19) 0.6344(3) 0.1394(15) Uani 1 1 d . . . H26A H 0.5350 1.0020 0.5957 0.209 Uiso 1 1 calc R . . H26B H 0.5885 1.0645 0.5928 0.209 Uiso 1 1 calc R . . H26C H 0.5017 1.0512 0.6662 0.209 Uiso 1 1 calc R . . C27 C 0.7107(2) 0.80830(13) 0.8437(2) 0.0861(8) Uani 1 1 d . . . H27A H 0.7768 0.8121 0.8087 0.103 Uiso 1 1 calc R . . C28 C 0.7530(3) 0.78925(16) 0.9474(3) 0.1151(11) Uani 1 1 d . . . H28A H 0.8000 0.8194 0.9794 0.173 Uiso 1 1 calc R . . H28B H 0.7958 0.7538 0.9455 0.173 Uiso 1 1 calc R . . H28C H 0.6901 0.7825 0.9828 0.173 Uiso 1 1 calc R . . C29 C 0.6391(4) 0.75982(18) 0.7946(3) 0.1541(19) Uani 1 1 d . . . H29A H 0.6127 0.7709 0.7285 0.231 Uiso 1 1 calc R . . H29B H 0.5760 0.7530 0.8297 0.231 Uiso 1 1 calc R . . H29C H 0.6832 0.7247 0.7944 0.231 Uiso 1 1 calc R . . C30 C 0.90673(18) 0.94816(10) 0.88341(17) 0.0612(6) Uani 1 1 d . . . H30A H 0.8734 0.9870 0.8789 0.073 Uiso 1 1 calc R . . H30B H 0.8799 0.9240 0.9336 0.073 Uiso 1 1 calc R . . C31 C 1.02322(17) 0.94515(9) 0.87610(16) 0.0557(5) Uani 1 1 d . . . C32 C 1.08010(19) 0.99990(10) 0.84902(18) 0.0615(6) Uani 1 1 d . . . C33 C 1.0240(2) 1.03912(11) 0.7823(2) 0.0778(7) Uani 1 1 d . . . H33A H 0.9536 1.0291 0.7501 0.093 Uiso 1 1 calc R . . C34 C 1.0700(3) 1.09209(13) 0.7632(3) 0.1034(11) Uani 1 1 d . . . H34A H 1.0306 1.1177 0.7188 0.124 Uiso 1 1 calc R . . C35 C 1.1739(4) 1.10753(16) 0.8093(3) 0.1192(13) Uani 1 1 d . . . H35A H 1.2049 1.1437 0.7967 0.143 Uiso 1 1 calc R . . C36 C 1.2317(3) 1.06969(15) 0.8739(3) 0.1020(10) Uani 1 1 d . . . H36A H 1.3027 1.0799 0.9045 0.122 Uiso 1 1 calc R . . C37 C 1.1855(2) 1.01650(12) 0.8941(2) 0.0756(7) Uani 1 1 d . . . H37A H 1.2256 0.9913 0.9386 0.091 Uiso 1 1 calc R . . C38 C 1.09312(19) 0.89878(10) 0.93147(18) 0.0608(6) Uani 1 1 d . . . C39 C 1.1930(2) 0.87853(11) 0.9014(2) 0.0745(7) Uani 1 1 d . . . H39A H 1.2179 0.8941 0.8455 0.089 Uiso 1 1 calc R . . C40 C 1.2554(3) 0.83548(14) 0.9537(3) 0.0953(10) Uani 1 1 d . . . H40A H 1.3224 0.8227 0.9332 0.114 Uiso 1 1 calc R . . C41 C 1.2196(3) 0.81152(15) 1.0353(3) 0.1073(11) Uani 1 1 d . . . H41A H 1.2614 0.7822 1.0699 0.129 Uiso 1 1 calc R . . C42 C 1.1223(3) 0.83099(14) 1.0654(2) 0.0987(10) Uani 1 1 d . . . H42A H 1.0973 0.8148 1.1208 0.118 Uiso 1 1 calc R . . C43 C 1.0607(2) 0.87448(12) 1.0143(2) 0.0765(7) Uani 1 1 d . . . H43A H 0.9950 0.8877 1.0367 0.092 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 Fe1 0.04364(19) 0.0618(2) 0.0542(2) -0.00563(14) 0.00381(14) -0.00112(13) N1 0.0454(9) 0.0634(11) 0.0577(12) -0.0052(8) 0.0092(8) -0.0034(8) N2 0.0431(9) 0.0689(12) 0.0567(12) -0.0044(9) 0.0053(8) 0.0002(8) C1 0.0467(12) 0.0708(15) 0.0652(16) -0.0139(11) 0.0113(10) 0.0007(10) C2 0.0570(14) 0.0670(15) 0.091(2) -0.0116(13) 0.0101(13) 0.0039(11) C3 0.0685(17) 0.0815(19) 0.135(3) -0.0091(18) 0.0124(17) 0.0180(15) C4 0.0470(15) 0.118(3) 0.161(4) -0.013(2) 0.0174(17) 0.0095(16) C5 0.0543(16) 0.107(2) 0.125(3) -0.005(2) 0.0236(16) -0.0052(15) C6 0.0529(14) 0.0857(17) 0.0804(19) -0.0110(14) 0.0166(12) -0.0059(12) C7 0.0651(15) 0.0909(19) 0.090(2) 0.0052(15) 0.0204(14) -0.0115(13) C8 0.168(4) 0.137(3) 0.098(3) 0.011(2) -0.003(3) -0.030(3) C9 0.115(3) 0.101(2) 0.119(3) -0.003(2) 0.025(2) -0.033(2) C10 0.0712(16) 0.0646(15) 0.105(2) -0.0003(14) 0.0136(15) 0.0051(12) C11 0.131(3) 0.093(2) 0.163(4) -0.036(2) 0.038(3) -0.029(2) C12 0.150(3) 0.122(3) 0.114(3) 0.000(2) 0.021(3) -0.046(2) C13 0.0594(14) 0.0668(14) 0.0565(15) -0.0042(11) 0.0119(11) -0.0087(11) C14 0.0565(14) 0.0815(16) 0.0512(14) -0.0049(11) 0.0016(11) -0.0046(11) C15 0.0473(12) 0.0734(15) 0.0622(16) -0.0009(12) -0.0006(11) -0.0038(10) C16 0.0495(14) 0.138(3) 0.081(2) -0.0157(18) -0.0052(13) -0.0033(15) C17 0.0743(17) 0.108(2) 0.0705(19) -0.0244(15) 0.0178(14) -0.0074(15) C18 0.0399(11) 0.0871(17) 0.0637(16) -0.0117(12) 0.0032(10) -0.0012(11) C19 0.0498(13) 0.094(2) 0.084(2) -0.0207(15) 0.0043(12) 0.0059(13) C20 0.0714(19) 0.123(3) 0.112(3) -0.028(2) 0.0196(18) 0.0175(18) C21 0.0711(19) 0.163(4) 0.099(3) -0.027(2) 0.0317(18) 0.015(2) C22 0.0697(18) 0.139(3) 0.080(2) -0.0045(19) 0.0235(15) -0.0102(18) C23 0.0531(14) 0.099(2) 0.0687(18) -0.0065(14) 0.0135(12) -0.0061(13) C24 0.0703(17) 0.0829(19) 0.118(3) -0.0109(18) 0.0082(16) 0.0121(14) C25 0.108(3) 0.082(2) 0.175(4) -0.019(2) -0.019(3) 0.0183(19) C26 0.128(3) 0.150(3) 0.128(4) 0.021(3) -0.031(3) -0.002(3) C27 0.0820(18) 0.099(2) 0.081(2) 0.0092(16) 0.0238(15) -0.0091(15) C28 0.124(3) 0.113(3) 0.104(3) 0.012(2) -0.006(2) -0.010(2) C29 0.209(5) 0.118(3) 0.120(4) -0.034(3) -0.038(3) 0.013(3) C30 0.0580(13) 0.0709(14) 0.0541(14) -0.0074(11) 0.0054(10) 0.0003(11) C31 0.0519(12) 0.0599(13) 0.0532(14) -0.0044(10) -0.0013(10) -0.0022(10) C32 0.0664(14) 0.0606(14) 0.0567(15) -0.0070(11) 0.0042(11) -0.0078(11) C33 0.0932(19) 0.0665(16) 0.0713(18) 0.0019(13) 0.0011(14) -0.0074(13) C34 0.145(3) 0.075(2) 0.088(2) 0.0120(16) 0.008(2) -0.0134(19) C35 0.157(4) 0.081(2) 0.122(3) 0.005(2) 0.024(3) -0.047(2) C36 0.105(2) 0.098(2) 0.104(3) -0.016(2) 0.0142(19) -0.048(2) C37 0.0750(16) 0.0782(17) 0.0726(18) -0.0087(13) 0.0054(13) -0.0168(13) C38 0.0583(13) 0.0600(14) 0.0608(15) -0.0025(11) -0.0058(11) -0.0052(10) C39 0.0600(15) 0.0780(16) 0.0824(19) -0.0036(14) -0.0037(13) 0.0028(12) C40 0.0729(18) 0.093(2) 0.113(3) -0.0061(19) -0.0151(18) 0.0184(16) C41 0.114(3) 0.085(2) 0.112(3) 0.013(2) -0.029(2) 0.0162(19) C42 0.120(3) 0.091(2) 0.079(2) 0.0191(17) -0.0064(19) 0.003(2) C43 0.0811(17) 0.0787(17) 0.0673(18) 0.0061(13) 0.0002(14) -0.0005(14) _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 Fe1 N1 1.9669(19) . ? Fe1 C30 1.995(2) . ? Fe1 N2 2.0014(18) . ? Fe1 C31 2.089(2) . ? N1 C13 1.332(3) . ? N1 C1 1.440(3) . ? N2 C15 1.325(3) . ? N2 C18 1.437(3) . ? C1 C2 1.392(3) . ? C1 C6 1.404(3) . ? C2 C3 1.395(3) . ? C2 C10 1.517(4) . ? C3 C4 1.372(4) . ? C4 C5 1.358(5) . ? C5 C6 1.382(4) . ? C6 C7 1.511(4) . ? C7 C8 1.506(5) . ? C7 C9 1.512(4) . ? C10 C12 1.490(5) . ? C10 C11 1.519(4) . ? C13 C14 1.378(3) . ? C13 C17 1.507(3) . ? C14 C15 1.383(3) . ? C15 C16 1.514(3) . ? C18 C23 1.389(4) . ? C18 C19 1.397(4) . ? C19 C20 1.381(4) . ? C19 C24 1.506(4) . ? C20 C21 1.367(5) . ? C21 C22 1.358(5) . ? C22 C23 1.392(4) . ? C23 C27 1.508(4) . ? C24 C25 1.523(4) . ? C24 C26 1.527(5) . ? C27 C29 1.507(5) . ? C27 C28 1.517(4) . ? C30 C31 1.412(3) . ? C31 C32 1.493(3) . ? C31 C38 1.497(3) . ? C32 C37 1.386(3) . ? C32 C33 1.393(3) . ? C33 C34 1.368(4) . ? C34 C35 1.370(5) . ? C35 C36 1.364(5) . ? C36 C37 1.377(4) . ? C38 C43 1.367(4) . ? C38 C39 1.393(4) . ? C39 C40 1.381(4) . ? C40 C41 1.366(5) . ? C41 C42 1.358(5) . ? C42 C43 1.377(4) . ? 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 N1 Fe1 C30 166.58(8) . . ? N1 Fe1 N2 95.08(8) . . ? C30 Fe1 N2 98.04(8) . . ? N1 Fe1 C31 126.55(8) . . ? C30 Fe1 C31 40.38(9) . . ? N2 Fe1 C31 138.37(8) . . ? C13 N1 C1 118.92(19) . . ? C13 N1 Fe1 123.21(15) . . ? C1 N1 Fe1 117.26(14) . . ? C15 N2 C18 117.71(19) . . ? C15 N2 Fe1 122.62(15) . . ? C18 N2 Fe1 119.54(15) . . ? C2 C1 C6 122.3(2) . . ? C2 C1 N1 118.7(2) . . ? C6 C1 N1 118.9(2) . . ? C1 C2 C3 117.9(2) . . ? C1 C2 C10 123.1(2) . . ? C3 C2 C10 118.9(3) . . ? C4 C3 C2 120.0(3) . . ? C5 C4 C3 121.0(3) . . ? C4 C5 C6 122.0(3) . . ? C5 C6 C1 116.7(3) . . ? C5 C6 C7 120.7(2) . . ? C1 C6 C7 122.6(2) . . ? C8 C7 C6 112.3(3) . . ? C8 C7 C9 109.2(3) . . ? C6 C7 C9 114.3(3) . . ? C12 C10 C2 112.6(3) . . ? C12 C10 C11 110.3(3) . . ? C2 C10 C11 112.9(3) . . ? N1 C13 C14 124.0(2) . . ? N1 C13 C17 120.0(2) . . ? C14 C13 C17 115.8(2) . . ? C13 C14 C15 129.9(2) . . ? N2 C15 C14 123.9(2) . . ? N2 C15 C16 120.6(2) . . ? C14 C15 C16 115.5(2) . . ? C23 C18 C19 122.2(2) . . ? C23 C18 N2 117.9(2) . . ? C19 C18 N2 119.8(2) . . ? C20 C19 C18 117.7(3) . . ? C20 C19 C24 118.9(3) . . ? C18 C19 C24 123.4(2) . . ? C21 C20 C19 120.9(3) . . ? C22 C21 C20 120.5(3) . . ? C21 C22 C23 121.7(3) . . ? C18 C23 C22 116.8(3) . . ? C18 C23 C27 122.9(2) . . ? C22 C23 C27 120.3(3) . . ? C19 C24 C25 112.9(3) . . ? C19 C24 C26 113.3(3) . . ? C25 C24 C26 108.2(3) . . ? C29 C27 C23 113.0(3) . . ? C29 C27 C28 108.4(3) . . ? C23 C27 C28 113.9(3) . . ? C31 C30 Fe1 73.36(13) . . ? C30 C31 C32 117.5(2) . . ? C30 C31 C38 119.5(2) . . ? C32 C31 C38 118.42(19) . . ? C30 C31 Fe1 66.25(12) . . ? C32 C31 Fe1 112.06(16) . . ? C38 C31 Fe1 110.38(15) . . ? C37 C32 C33 117.1(2) . . ? C37 C32 C31 122.3(2) . . ? C33 C32 C31 120.4(2) . . ? C34 C33 C32 121.5(3) . . ? C33 C34 C35 120.1(3) . . ? C36 C35 C34 119.7(3) . . ? C35 C36 C37 120.4(3) . . ? C36 C37 C32 121.1(3) . . ? C43 C38 C39 117.2(2) . . ? C43 C38 C31 120.8(2) . . ? C39 C38 C31 121.9(2) . . ? C40 C39 C38 120.6(3) . . ? C41 C40 C39 120.6(3) . . ? C42 C41 C40 119.3(3) . . ? C41 C42 C43 120.4(3) . . ? C38 C43 C42 121.9(3) . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 23.50 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 0.252 _refine_diff_density_min -0.164 _refine_diff_density_rms 0.038 #===end data_[(NacNac)Fe(??-PPh)]2.Toluene _database_code_depnum_ccdc_archive 'CCDC 284032' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C38.50 H50 Fe N2 P' _chemical_formula_weight 627.63 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' Fe Fe 0.3463 0.8444 '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 13.1127(6) _cell_length_b 14.2879(7) _cell_length_c 19.5668(9) _cell_angle_alpha 90.00 _cell_angle_beta 92.8560(10) _cell_angle_gamma 90.00 _cell_volume 3661.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.18 _exptl_crystal_density_diffrn 1.055 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1244 _exptl_absorpt_coefficient_mu 0.477 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.737894 _exptl_absorpt_correction_T_max 1.00000 _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 17870 _diffrn_reflns_av_R_equivalents 0.0491 _diffrn_reflns_av_sigmaI/netI 0.0498 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 23.26 _reflns_number_total 5262 _reflns_number_gt 3522 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0866P)^2^+1.8524P] 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_number_reflns 5262 _refine_ls_number_parameters 374 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0838 _refine_ls_R_factor_gt 0.0486 _refine_ls_wR_factor_ref 0.1446 _refine_ls_wR_factor_gt 0.1179 _refine_ls_goodness_of_fit_ref 0.905 _refine_ls_restrained_S_all 0.905 _refine_ls_shift/su_max 0.002 _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 Fe1 Fe 0.10644(4) 0.40743(3) 0.01114(3) 0.0450(2) Uani 1 1 d . . . P1 P 0.07854(8) 0.57713(7) 0.01374(5) 0.0524(3) Uani 1 1 d . . . N1 N 0.1503(2) 0.3392(2) 0.09780(14) 0.0458(7) Uani 1 1 d . . . N2 N 0.2262(2) 0.3648(2) -0.04118(15) 0.0501(8) Uani 1 1 d . . . C1 C 0.0788(3) 0.3243(3) 0.15079(19) 0.0511(9) Uani 1 1 d . . . C2 C 0.0222(3) 0.2406(3) 0.1495(2) 0.0635(11) Uani 1 1 d . . . C3 C -0.0427(4) 0.2250(4) 0.2020(3) 0.0869(16) Uani 1 1 d . . . H3A H -0.0784 0.1688 0.2033 0.104 Uiso 1 1 calc R . . C4 C -0.0554(4) 0.2906(5) 0.2521(3) 0.0914(17) Uani 1 1 d . . . H4A H -0.0993 0.2787 0.2869 0.110 Uiso 1 1 calc R . . C5 C -0.0034(4) 0.3736(4) 0.2507(2) 0.0775(14) Uani 1 1 d . . . H5A H -0.0140 0.4181 0.2843 0.093 Uiso 1 1 calc R . . C6 C 0.0649(3) 0.3930(3) 0.20024(19) 0.0580(10) Uani 1 1 d . . . C7 C 0.0300(4) 0.1690(3) 0.0923(3) 0.0775(13) Uani 1 1 d . . . H7A H 0.0472 0.2038 0.0513 0.093 Uiso 1 1 calc R . . C8 C -0.0701(5) 0.1179(4) 0.0747(3) 0.118(2) Uani 1 1 d . . . H8A H -0.1235 0.1627 0.0654 0.177 Uiso 1 1 calc R . . H8B H -0.0874 0.0793 0.1127 0.177 Uiso 1 1 calc R . . H8C H -0.0625 0.0793 0.0351 0.177 Uiso 1 1 calc R . . C9 C 0.1147(5) 0.0979(4) 0.1062(4) 0.130(2) Uani 1 1 d . . . H9A H 0.1773 0.1299 0.1186 0.195 Uiso 1 1 calc R . . H9B H 0.1235 0.0613 0.0657 0.195 Uiso 1 1 calc R . . H9C H 0.0970 0.0574 0.1429 0.195 Uiso 1 1 calc R . . C10 C 0.1208(3) 0.4849(3) 0.2005(2) 0.0656(12) Uani 1 1 d . . . H10A H 0.1581 0.4877 0.1583 0.079 Uiso 1 1 calc R . . C11 C 0.0493(5) 0.5678(4) 0.2000(3) 0.1037(18) Uani 1 1 d . . . H11A H 0.0003 0.5624 0.1620 0.156 Uiso 1 1 calc R . . H11B H 0.0878 0.6245 0.1956 0.156 Uiso 1 1 calc R . . H11C H 0.0144 0.5692 0.2419 0.156 Uiso 1 1 calc R . . C12 C 0.1990(5) 0.4939(4) 0.2602(3) 0.110(2) Uani 1 1 d . . . H12A H 0.2449 0.4415 0.2602 0.164 Uiso 1 1 calc R . . H12B H 0.1646 0.4949 0.3024 0.164 Uiso 1 1 calc R . . H12C H 0.2369 0.5509 0.2557 0.164 Uiso 1 1 calc R . . C13 C 0.2828(3) 0.2753(3) 0.1800(2) 0.0731(13) Uani 1 1 d . . . H13A H 0.3174 0.3242 0.2055 0.110 Uiso 1 1 calc R . . H13B H 0.3288 0.2238 0.1744 0.110 Uiso 1 1 calc R . . H13C H 0.2251 0.2544 0.2041 0.110 Uiso 1 1 calc R . . C14 C 0.2467(3) 0.3121(3) 0.11014(19) 0.0522(10) Uani 1 1 d . . . C15 C 0.3195(3) 0.3134(3) 0.0606(2) 0.0617(11) Uani 1 1 d . . . H15A H 0.3856 0.2999 0.0772 0.074 Uiso 1 1 calc R . . C16 C 0.3103(3) 0.3313(3) -0.0093(2) 0.0566(10) Uani 1 1 d . . . C17 C 0.4034(3) 0.3055(4) -0.0484(2) 0.0816(14) Uani 1 1 d . . . H17A H 0.4154 0.2394 -0.0446 0.122 Uiso 1 1 calc R . . H17B H 0.4618 0.3389 -0.0296 0.122 Uiso 1 1 calc R . . H17C H 0.3917 0.3219 -0.0957 0.122 Uiso 1 1 calc R . . C18 C 0.2241(3) 0.3736(3) -0.1149(2) 0.0557(10) Uani 1 1 d . . . C19 C 0.2634(3) 0.4526(3) -0.1455(2) 0.0664(12) Uani 1 1 d . . . C20 C 0.2595(4) 0.4573(5) -0.2161(3) 0.0910(16) Uani 1 1 d . . . H20A H 0.2860 0.5096 -0.2373 0.109 Uiso 1 1 calc R . . C21 C 0.2184(5) 0.3882(6) -0.2550(3) 0.103(2) Uani 1 1 d . . . H21A H 0.2175 0.3932 -0.3024 0.123 Uiso 1 1 calc R . . C22 C 0.1777(4) 0.3104(5) -0.2257(3) 0.0919(17) Uani 1 1 d . . . H22A H 0.1494 0.2632 -0.2534 0.110 Uiso 1 1 calc R . . C23 C 0.1783(3) 0.3014(3) -0.1546(2) 0.0675(12) Uani 1 1 d . . . C24 C 0.3103(4) 0.5326(4) -0.1053(3) 0.0902(16) Uani 1 1 d . . . H24A H 0.2960 0.5234 -0.0571 0.108 Uiso 1 1 calc R . . C25 C 0.2662(5) 0.6278(4) -0.1280(3) 0.123(2) Uani 1 1 d . . . H25A H 0.1935 0.6274 -0.1241 0.185 Uiso 1 1 calc R . . H25B H 0.2815 0.6393 -0.1747 0.185 Uiso 1 1 calc R . . H25C H 0.2959 0.6762 -0.0994 0.185 Uiso 1 1 calc R . . C26 C 0.4279(5) 0.5375(6) -0.1107(4) 0.163(3) Uani 1 1 d . . . H26A H 0.4579 0.4796 -0.0951 0.245 Uiso 1 1 calc R . . H26B H 0.4548 0.5879 -0.0828 0.245 Uiso 1 1 calc R . . H26C H 0.4436 0.5480 -0.1575 0.245 Uiso 1 1 calc R . . C27 C 0.1320(4) 0.2156(3) -0.1221(3) 0.0862(15) Uani 1 1 d . . . H27A H 0.1024 0.2366 -0.0798 0.103 Uiso 1 1 calc R . . C28 C 0.2110(5) 0.1411(4) -0.1022(4) 0.135(2) Uani 1 1 d . . . H28A H 0.2654 0.1687 -0.0744 0.202 Uiso 1 1 calc R . . H28B H 0.2380 0.1150 -0.1427 0.202 Uiso 1 1 calc R . . H28C H 0.1794 0.0924 -0.0768 0.202 Uiso 1 1 calc R . . C29 C 0.0454(4) 0.1707(4) -0.1662(3) 0.117(2) Uani 1 1 d . . . H29A H 0.0188 0.1180 -0.1425 0.176 Uiso 1 1 calc R . . H29B H 0.0711 0.1504 -0.2089 0.176 Uiso 1 1 calc R . . H29C H -0.0080 0.2158 -0.1750 0.176 Uiso 1 1 calc R . . C30 C 0.1753(3) 0.6523(3) 0.0568(2) 0.0566(10) Uani 1 1 d . . . C31 C 0.1559(4) 0.7452(3) 0.0680(3) 0.0849(15) Uani 1 1 d . . . H31A H 0.0942 0.7708 0.0516 0.102 Uiso 1 1 calc R . . C32 C 0.2261(5) 0.8013(4) 0.1030(4) 0.122(2) Uani 1 1 d . . . H32A H 0.2119 0.8642 0.1101 0.146 Uiso 1 1 calc R . . C33 C 0.3160(5) 0.7642(5) 0.1271(3) 0.119(2) Uani 1 1 d . . . H33A H 0.3634 0.8019 0.1509 0.143 Uiso 1 1 calc R . . C34 C 0.3373(4) 0.6723(4) 0.1168(3) 0.0923(16) Uani 1 1 d . . . H34A H 0.3992 0.6475 0.1335 0.111 Uiso 1 1 calc R . . C35 C 0.2673(3) 0.6158(3) 0.0817(2) 0.0697(12) Uani 1 1 d . . . H35A H 0.2821 0.5529 0.0747 0.084 Uiso 1 1 calc R . . C36 C 0.4043(14) -0.0989(12) -0.0479(9) 0.283(7) Uiso 1 1 d . . . C37 C 0.3865(17) -0.0220(16) 0.0055(12) 0.167(7) Uiso 0.50 1 d P . . C38 C 0.4364(13) 0.0312(10) 0.0379(7) 0.212(4) Uiso 1 1 d . . . C39 C 0.540(2) 0.0373(17) 0.0174(13) 0.188(8) Uiso 0.50 1 d P . . C40 C 0.5042(17) 0.0917(13) 0.0785(10) 0.165(6) Uiso 0.50 1 d P . . 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 Fe1 0.0429(3) 0.0442(3) 0.0482(3) 0.0010(2) 0.0044(2) 0.0011(2) P1 0.0475(6) 0.0444(6) 0.0644(7) -0.0036(5) -0.0055(5) -0.0024(4) N1 0.0437(19) 0.0487(18) 0.0454(18) 0.0030(14) 0.0050(14) -0.0002(14) N2 0.048(2) 0.0494(18) 0.053(2) 0.0015(15) 0.0106(15) 0.0019(15) C1 0.043(2) 0.059(2) 0.051(2) 0.0133(19) 0.0012(18) -0.0004(19) C2 0.056(3) 0.074(3) 0.061(3) 0.022(2) 0.001(2) -0.009(2) C3 0.071(3) 0.103(4) 0.086(4) 0.038(3) 0.000(3) -0.025(3) C4 0.066(3) 0.145(5) 0.065(3) 0.027(3) 0.015(3) -0.014(4) C5 0.063(3) 0.117(4) 0.053(3) 0.003(3) 0.010(2) 0.007(3) C6 0.052(2) 0.075(3) 0.047(2) 0.004(2) 0.0023(19) 0.008(2) C7 0.086(3) 0.059(3) 0.087(3) 0.010(2) -0.003(3) -0.017(3) C8 0.116(5) 0.109(4) 0.125(5) 0.012(4) -0.029(4) -0.047(4) C9 0.136(6) 0.090(4) 0.160(6) -0.028(4) -0.036(5) 0.016(4) C10 0.075(3) 0.065(3) 0.057(3) -0.006(2) 0.004(2) 0.010(2) C11 0.131(5) 0.089(4) 0.093(4) 0.001(3) 0.016(3) 0.038(4) C12 0.124(5) 0.085(4) 0.115(5) -0.012(3) -0.037(4) -0.009(3) C13 0.063(3) 0.090(3) 0.065(3) 0.013(2) -0.004(2) 0.012(2) C14 0.050(3) 0.054(2) 0.052(2) 0.0037(18) -0.0005(19) 0.0013(19) C15 0.041(2) 0.075(3) 0.069(3) 0.007(2) 0.003(2) 0.006(2) C16 0.044(2) 0.061(3) 0.065(3) 0.002(2) 0.008(2) 0.002(2) C17 0.052(3) 0.115(4) 0.080(3) 0.010(3) 0.022(2) 0.020(3) C18 0.049(2) 0.066(3) 0.053(2) 0.001(2) 0.0132(19) 0.013(2) C19 0.058(3) 0.083(3) 0.060(3) 0.016(2) 0.015(2) 0.005(2) C20 0.073(3) 0.131(5) 0.070(4) 0.028(3) 0.019(3) 0.008(3) C21 0.086(4) 0.169(6) 0.055(3) 0.011(4) 0.021(3) 0.032(4) C22 0.081(4) 0.131(5) 0.065(3) -0.038(3) 0.011(3) 0.021(4) C23 0.064(3) 0.079(3) 0.060(3) -0.014(2) 0.013(2) 0.014(2) C24 0.088(4) 0.093(4) 0.091(4) 0.026(3) 0.014(3) -0.023(3) C25 0.158(6) 0.088(4) 0.127(5) 0.035(4) 0.041(4) -0.011(4) C26 0.105(6) 0.152(7) 0.231(9) 0.028(6) -0.016(6) -0.046(5) C27 0.097(4) 0.072(3) 0.090(4) -0.031(3) 0.015(3) -0.008(3) C28 0.151(6) 0.083(4) 0.166(7) 0.011(4) -0.026(5) -0.004(4) C29 0.099(4) 0.104(4) 0.148(5) -0.050(4) 0.006(4) -0.009(4) C30 0.050(3) 0.059(3) 0.061(3) -0.002(2) 0.0020(19) -0.009(2) C31 0.074(3) 0.066(3) 0.114(4) -0.020(3) -0.010(3) -0.011(3) C32 0.099(5) 0.087(4) 0.176(6) -0.045(4) -0.024(4) -0.017(4) C33 0.086(4) 0.123(5) 0.145(6) -0.051(4) -0.020(4) -0.029(4) C34 0.049(3) 0.124(5) 0.102(4) -0.018(4) -0.009(3) -0.008(3) C35 0.047(3) 0.086(3) 0.076(3) -0.004(2) 0.001(2) -0.003(2) _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 Fe1 N2 2.012(3) . ? Fe1 N1 2.015(3) . ? Fe1 P1 2.4530(11) . ? Fe1 P1 2.4599(11) 3_565 ? P1 C30 1.836(4) . ? P1 Fe1 2.4599(11) 3_565 ? N1 C14 1.333(5) . ? N1 C1 1.448(4) . ? N2 C16 1.329(5) . ? N2 C18 1.447(5) . ? C1 C6 1.397(5) . ? C1 C2 1.406(5) . ? C2 C3 1.384(6) . ? C2 C7 1.523(6) . ? C3 C4 1.372(7) . ? C4 C5 1.368(7) . ? C5 C6 1.394(6) . ? C6 C10 1.503(6) . ? C7 C9 1.520(7) . ? C7 C8 1.527(7) . ? C10 C11 1.510(6) . ? C10 C12 1.522(6) . ? C13 C14 1.517(5) . ? C14 C15 1.393(5) . ? C15 C16 1.392(5) . ? C16 C17 1.517(5) . ? C18 C19 1.388(6) . ? C18 C23 1.408(6) . ? C19 C20 1.382(6) . ? C19 C24 1.501(7) . ? C20 C21 1.343(8) . ? C21 C22 1.371(8) . ? C22 C23 1.397(6) . ? C23 C27 1.520(6) . ? C24 C25 1.535(7) . ? C24 C26 1.552(8) . ? C27 C28 1.523(7) . ? C27 C29 1.533(7) . ? C30 C31 1.371(6) . ? C30 C35 1.380(6) . ? C31 C32 1.376(7) . ? C32 C33 1.355(8) . ? C33 C34 1.359(8) . ? C34 C35 1.381(6) . ? C36 C39 1.28(2) 3_655 ? C36 C40 1.37(2) 3_655 ? C36 C37 1.54(3) . ? C37 C39 1.11(3) 3_655 ? C37 C38 1.17(2) . ? C38 C39 1.43(2) . ? C38 C40 1.45(2) . ? C38 C39 1.50(3) 3_655 ? C39 C37 1.11(3) 3_655 ? C39 C36 1.28(2) 3_655 ? C39 C38 1.50(3) 3_655 ? C39 C40 1.52(3) . ? C39 C39 1.61(5) 3_655 ? C40 C36 1.37(2) 3_655 ? 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 N2 Fe1 N1 94.83(12) . . ? N2 Fe1 P1 115.54(9) . . ? N1 Fe1 P1 119.84(9) . . ? N2 Fe1 P1 135.53(9) . 3_565 ? N1 Fe1 P1 116.57(9) . 3_565 ? P1 Fe1 P1 76.64(4) . 3_565 ? C30 P1 Fe1 119.19(14) . . ? C30 P1 Fe1 133.69(14) . 3_565 ? Fe1 P1 Fe1 103.36(4) . 3_565 ? C14 N1 C1 118.0(3) . . ? C14 N1 Fe1 121.4(2) . . ? C1 N1 Fe1 120.4(2) . . ? C16 N2 C18 118.3(3) . . ? C16 N2 Fe1 121.4(3) . . ? C18 N2 Fe1 120.3(2) . . ? C6 C1 C2 121.5(4) . . ? C6 C1 N1 120.3(3) . . ? C2 C1 N1 118.2(3) . . ? C3 C2 C1 117.9(4) . . ? C3 C2 C7 120.2(4) . . ? C1 C2 C7 121.9(4) . . ? C4 C3 C2 121.3(5) . . ? C5 C4 C3 120.0(4) . . ? C4 C5 C6 121.6(5) . . ? C5 C6 C1 117.5(4) . . ? C5 C6 C10 120.2(4) . . ? C1 C6 C10 122.4(3) . . ? C9 C7 C2 113.2(4) . . ? C9 C7 C8 109.4(4) . . ? C2 C7 C8 113.5(5) . . ? C6 C10 C11 112.5(4) . . ? C6 C10 C12 112.7(4) . . ? C11 C10 C12 109.5(4) . . ? N1 C14 C15 123.1(3) . . ? N1 C14 C13 120.9(3) . . ? C15 C14 C13 115.9(3) . . ? C16 C15 C14 131.1(4) . . ? N2 C16 C15 123.8(4) . . ? N2 C16 C17 121.4(4) . . ? C15 C16 C17 114.8(4) . . ? C19 C18 C23 121.0(4) . . ? C19 C18 N2 120.8(4) . . ? C23 C18 N2 118.2(4) . . ? C20 C19 C18 118.3(5) . . ? C20 C19 C24 118.7(5) . . ? C18 C19 C24 123.0(4) . . ? C21 C20 C19 121.7(5) . . ? C20 C21 C22 120.8(5) . . ? C21 C22 C23 120.6(5) . . ? C22 C23 C18 117.6(5) . . ? C22 C23 C27 120.5(5) . . ? C18 C23 C27 121.9(4) . . ? C19 C24 C25 112.6(5) . . ? C19 C24 C26 112.4(5) . . ? C25 C24 C26 107.6(5) . . ? C23 C27 C28 113.0(5) . . ? C23 C27 C29 113.7(5) . . ? C28 C27 C29 109.1(4) . . ? C31 C30 C35 118.5(4) . . ? C31 C30 P1 120.6(3) . . ? C35 C30 P1 120.8(3) . . ? C30 C31 C32 121.2(5) . . ? C33 C32 C31 119.6(6) . . ? C32 C33 C34 120.5(5) . . ? C33 C34 C35 120.1(5) . . ? C30 C35 C34 120.1(5) . . ? C39 C36 C40 69.8(18) 3_655 3_655 ? C39 C36 C37 45.2(14) 3_655 . ? C40 C36 C37 114.1(17) 3_655 . ? C39 C37 C38 83(2) 3_655 . ? C39 C37 C36 54.6(17) 3_655 . ? C38 C37 C36 137(2) . . ? C37 C38 C39 114(2) . . ? C37 C38 C40 176(2) . . ? C39 C38 C40 63.5(14) . . ? C37 C38 C39 47.1(13) . 3_655 ? C39 C38 C39 66.6(19) . 3_655 ? C40 C38 C39 130(2) . 3_655 ? C37 C39 C36 80(2) 3_655 3_655 ? C37 C39 C38 163(3) 3_655 . ? C36 C39 C38 116(3) 3_655 . ? C37 C39 C38 50.3(17) 3_655 3_655 ? C36 C39 C38 130(3) 3_655 3_655 ? C38 C39 C38 113.4(19) . 3_655 ? C37 C39 C40 137(3) 3_655 . ? C36 C39 C40 58.0(15) 3_655 . ? C38 C39 C40 58.8(16) . . ? C38 C39 C40 170(2) 3_655 . ? C37 C39 C39 105(3) 3_655 3_655 ? C36 C39 C39 175(4) 3_655 3_655 ? C38 C39 C39 58.8(18) . 3_655 ? C38 C39 C39 54.6(15) 3_655 3_655 ? C40 C39 C39 117(3) . 3_655 ? C36 C40 C38 109.4(16) 3_655 . ? C36 C40 C39 52.2(13) 3_655 . ? C38 C40 C39 57.7(11) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.489 _refine_diff_density_min -0.178 _refine_diff_density_rms 0.054 #===end data_[((NacNac)Ni)2(??-(PPh)2)] _database_code_depnum_ccdc_archive 'CCDC 284033' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C80.50 H103.50 N4 Ni2 P2' _chemical_formula_weight 1306.53 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' 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 23.028(6) _cell_length_b 13.781(4) _cell_length_c 24.031(7) _cell_angle_alpha 90.00 _cell_angle_beta 106.742(8) _cell_angle_gamma 90.00 _cell_volume 7303(4) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.14 _exptl_crystal_density_diffrn 1.188 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2802 _exptl_absorpt_coefficient_mu 0.604 _exptl_absorpt_correction_type none _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 15842 _diffrn_reflns_av_R_equivalents 0.1620 _diffrn_reflns_av_sigmaI/netI 0.1913 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 23.40 _reflns_number_total 9532 _reflns_number_gt 4529 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1000P)^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_number_reflns 9532 _refine_ls_number_parameters 806 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1636 _refine_ls_R_factor_gt 0.0803 _refine_ls_wR_factor_ref 0.2182 _refine_ls_wR_factor_gt 0.1813 _refine_ls_goodness_of_fit_ref 0.905 _refine_ls_restrained_S_all 0.905 _refine_ls_shift/su_max 0.002 _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 0.24232(5) 0.29153(7) 0.40835(4) 0.0394(3) Uani 1 1 d . . . Ni2 Ni 0.28881(5) 0.43444(7) 0.53963(4) 0.0449(3) Uani 1 1 d . . . P1 P 0.20680(10) 0.37594(16) 0.47084(9) 0.0449(6) Uani 1 1 d . . . P2 P 0.28147(11) 0.28185(16) 0.50600(8) 0.0471(6) Uani 1 1 d . . . N1 N 0.3027(3) 0.2573(4) 0.3739(3) 0.0457(18) Uani 1 1 d . . . N2 N 0.1771(3) 0.2936(5) 0.3373(2) 0.0427(17) Uani 1 1 d . . . N3 N 0.3524(3) 0.4279(5) 0.6111(3) 0.0530(19) Uani 1 1 d . . . N4 N 0.2892(4) 0.5736(5) 0.5311(3) 0.058(2) Uani 1 1 d . . . C1 C 0.3624(4) 0.2212(6) 0.4060(4) 0.050(2) Uani 1 1 d . . . C2 C 0.4109(4) 0.2851(7) 0.4289(4) 0.054(2) Uani 1 1 d . . . C3 C 0.4683(5) 0.2499(9) 0.4548(5) 0.078(3) Uani 1 1 d . . . H3A H 0.4998 0.2929 0.4705 0.093 Uiso 1 1 calc R . . C4 C 0.4794(5) 0.1508(10) 0.4578(5) 0.092(4) Uani 1 1 d . . . H4A H 0.5187 0.1278 0.4735 0.110 Uiso 1 1 calc R . . C5 C 0.4324(6) 0.0869(8) 0.4375(5) 0.082(3) Uani 1 1 d . . . H5A H 0.4399 0.0206 0.4411 0.098 Uiso 1 1 calc R . . C6 C 0.3738(5) 0.1197(7) 0.4118(4) 0.062(3) Uani 1 1 d . . . C7 C 0.4024(4) 0.3971(6) 0.4249(4) 0.060(3) Uani 1 1 d . . . H7A H 0.3596 0.4116 0.4059 0.073 Uiso 1 1 calc R . . C8 C 0.4205(4) 0.4419(7) 0.4856(4) 0.068(3) Uani 1 1 d . . . H8A H 0.3952 0.4159 0.5076 0.103 Uiso 1 1 calc R . . H8B H 0.4154 0.5110 0.4826 0.103 Uiso 1 1 calc R . . H8C H 0.4621 0.4268 0.5049 0.103 Uiso 1 1 calc R . . C9 C 0.4405(5) 0.4427(8) 0.3895(4) 0.100(4) Uani 1 1 d . . . H9A H 0.4288 0.4161 0.3509 0.150 Uiso 1 1 calc R . . H9B H 0.4826 0.4291 0.4077 0.150 Uiso 1 1 calc R . . H9C H 0.4343 0.5117 0.3875 0.150 Uiso 1 1 calc R . . C10 C 0.3220(5) 0.0490(7) 0.3907(4) 0.074(3) Uani 1 1 d . . . H10A H 0.2859 0.0792 0.3969 0.089 Uiso 1 1 calc R . . C11 C 0.3073(6) 0.0261(8) 0.3248(5) 0.116(4) Uani 1 1 d . . . H11A H 0.2995 0.0855 0.3031 0.173 Uiso 1 1 calc R . . H11B H 0.2721 -0.0149 0.3133 0.173 Uiso 1 1 calc R . . H11C H 0.3412 -0.0065 0.3175 0.173 Uiso 1 1 calc R . . C12 C 0.3330(5) -0.0481(7) 0.4251(6) 0.106(4) Uani 1 1 d . . . H12A H 0.3408 -0.0349 0.4658 0.159 Uiso 1 1 calc R . . H12B H 0.3672 -0.0808 0.4186 0.159 Uiso 1 1 calc R . . H12C H 0.2977 -0.0885 0.4121 0.159 Uiso 1 1 calc R . . C13 C 0.1173(5) 0.2706(7) 0.3386(3) 0.054(2) Uani 1 1 d . . . C14 C 0.0731(5) 0.3430(8) 0.3409(4) 0.061(3) Uani 1 1 d . . . C15 C 0.0167(5) 0.3145(9) 0.3384(5) 0.084(3) Uani 1 1 d . . . H15A H -0.0117 0.3617 0.3398 0.101 Uiso 1 1 calc R . . C16 C -0.0011(6) 0.2191(12) 0.3339(6) 0.106(4) Uani 1 1 d . . . H16A H -0.0409 0.2023 0.3314 0.127 Uiso 1 1 calc R . . C17 C 0.0409(6) 0.1492(9) 0.3332(5) 0.090(4) Uani 1 1 d . . . H17A H 0.0295 0.0843 0.3315 0.108 Uiso 1 1 calc R . . C18 C 0.0981(5) 0.1719(8) 0.3349(4) 0.067(3) Uani 1 1 d . . . C19 C 0.0894(5) 0.4509(7) 0.3463(4) 0.069(3) Uani 1 1 d . . . H19A H 0.1323 0.4553 0.3685 0.083 Uiso 1 1 calc R . . C20 C 0.0831(6) 0.4990(8) 0.2874(5) 0.121(5) Uani 1 1 d . . . H20A H 0.0945 0.5660 0.2932 0.181 Uiso 1 1 calc R . . H20B H 0.0417 0.4944 0.2638 0.181 Uiso 1 1 calc R . . H20C H 0.1090 0.4666 0.2683 0.181 Uiso 1 1 calc R . . C21 C 0.0550(5) 0.5097(8) 0.3781(5) 0.106(4) Uani 1 1 d . . . H21A H 0.0682 0.5760 0.3799 0.159 Uiso 1 1 calc R . . H21B H 0.0623 0.4847 0.4168 0.159 Uiso 1 1 calc R . . H21C H 0.0125 0.5062 0.3581 0.159 Uiso 1 1 calc R . . C22 C 0.1444(5) 0.0892(7) 0.3352(5) 0.080(3) Uani 1 1 d . . . H22A H 0.1833 0.1190 0.3360 0.096 Uiso 1 1 calc R . . C23 C 0.1540(6) 0.0262(9) 0.3865(6) 0.123(5) Uani 1 1 d . . . H23A H 0.1693 0.0642 0.4211 0.185 Uiso 1 1 calc R . . H23B H 0.1828 -0.0235 0.3853 0.185 Uiso 1 1 calc R . . H23C H 0.1163 -0.0032 0.3867 0.185 Uiso 1 1 calc R . . C24 C 0.1219(7) 0.0292(10) 0.2784(6) 0.164(7) Uani 1 1 d . . . H24A H 0.1506 -0.0213 0.2782 0.247 Uiso 1 1 calc R . . H24B H 0.1179 0.0709 0.2455 0.247 Uiso 1 1 calc R . . H24C H 0.0833 0.0007 0.2762 0.247 Uiso 1 1 calc R . . C25 C 0.3515(4) 0.2586(7) 0.2924(4) 0.072(3) Uani 1 1 d . . . H25A H 0.3740 0.2018 0.3092 0.108 Uiso 1 1 calc R . . H25B H 0.3774 0.3145 0.3015 0.108 Uiso 1 1 calc R . . H25C H 0.3370 0.2510 0.2509 0.108 Uiso 1 1 calc R . . C26 C 0.2975(5) 0.2719(6) 0.3171(4) 0.051(2) Uani 1 1 d . . . C27 C 0.2419(5) 0.2950(6) 0.2768(4) 0.057(2) Uani 1 1 d . . . H27A H 0.2432 0.3117 0.2396 0.068 Uiso 1 1 calc R . . C28 C 0.1869(4) 0.2956(6) 0.2860(3) 0.050(2) Uani 1 1 d . . . C29 C 0.1317(4) 0.2909(7) 0.2305(3) 0.072(3) Uani 1 1 d . . . H29A H 0.1181 0.2249 0.2236 0.108 Uiso 1 1 calc R . . H29B H 0.1435 0.3145 0.1978 0.108 Uiso 1 1 calc R . . H29C H 0.0994 0.3303 0.2359 0.108 Uiso 1 1 calc R . . C30 C 0.3521(5) 0.3490(8) 0.6506(3) 0.058(3) Uani 1 1 d . . . C31 C 0.3888(5) 0.2667(8) 0.6503(4) 0.066(3) Uani 1 1 d . . . C32 C 0.3893(5) 0.1937(9) 0.6911(4) 0.096(4) Uani 1 1 d . . . H32A H 0.4130 0.1386 0.6925 0.116 Uiso 1 1 calc R . . C33 C 0.3553(7) 0.2028(12) 0.7285(5) 0.108(5) Uani 1 1 d . . . H33A H 0.3551 0.1522 0.7541 0.130 Uiso 1 1 calc R . . C34 C 0.3218(7) 0.2823(12) 0.7300(5) 0.107(5) Uani 1 1 d . . . H34A H 0.3004 0.2879 0.7573 0.128 Uiso 1 1 calc R . . C35 C 0.3199(5) 0.3575(9) 0.6891(4) 0.073(3) Uani 1 1 d . . . C36 C 0.4258(5) 0.2523(8) 0.6097(5) 0.081(3) Uani 1 1 d . . . H36A H 0.4039 0.2857 0.5738 0.097 Uiso 1 1 calc R . . C37 C 0.4320(6) 0.1454(10) 0.5921(6) 0.128(5) Uani 1 1 d . . . H37A H 0.3925 0.1164 0.5788 0.192 Uiso 1 1 calc R . . H37B H 0.4562 0.1101 0.6252 0.192 Uiso 1 1 calc R . . H37C H 0.4512 0.1435 0.5616 0.192 Uiso 1 1 calc R . . C38 C 0.4873(6) 0.2983(10) 0.6287(7) 0.142(6) Uani 1 1 d . . . H38A H 0.4834 0.3651 0.6383 0.213 Uiso 1 1 calc R . . H38B H 0.5059 0.2943 0.5978 0.213 Uiso 1 1 calc R . . H38C H 0.5121 0.2649 0.6622 0.213 Uiso 1 1 calc R . . C39 C 0.2805(7) 0.4468(11) 0.6912(5) 0.109(4) Uani 1 1 d . . . H39A H 0.2825 0.4892 0.6591 0.131 Uiso 1 1 calc R . . C40 C 0.2162(7) 0.4223(12) 0.6820(7) 0.157(6) Uani 1 1 d . . . H40A H 0.2013 0.3878 0.6460 0.236 Uiso 1 1 calc R . . H40B H 0.1933 0.4809 0.6805 0.236 Uiso 1 1 calc R . . H40C H 0.2122 0.3824 0.7134 0.236 Uiso 1 1 calc R . . C41 C 0.3046(9) 0.5067(14) 0.7480(7) 0.222(10) Uani 1 1 d . . . H41A H 0.2791 0.5622 0.7466 0.333 Uiso 1 1 calc R . . H41B H 0.3453 0.5278 0.7516 0.333 Uiso 1 1 calc R . . H41C H 0.3043 0.4670 0.7807 0.333 Uiso 1 1 calc R . . C42 C 0.2389(5) 0.6267(6) 0.4929(4) 0.056(2) Uani 1 1 d . . . C43 C 0.2380(5) 0.6390(7) 0.4349(4) 0.064(3) Uani 1 1 d . . . C44 C 0.1925(5) 0.6998(8) 0.4006(6) 0.090(3) Uani 1 1 d . . . H44A H 0.1910 0.7106 0.3620 0.108 Uiso 1 1 calc R . . C45 C 0.1509(6) 0.7430(9) 0.4226(7) 0.105(4) Uani 1 1 d . . . H45A H 0.1215 0.7834 0.3991 0.126 Uiso 1 1 calc R . . C46 C 0.1519(6) 0.7277(8) 0.4783(7) 0.103(4) Uani 1 1 d . . . H46A H 0.1230 0.7582 0.4924 0.124 Uiso 1 1 calc R . . C47 C 0.1953(5) 0.6671(7) 0.5161(5) 0.066(3) Uani 1 1 d . . . C48 C 0.2836(4) 0.5947(7) 0.4088(4) 0.063(3) Uani 1 1 d . . . H48A H 0.3071 0.5470 0.4365 0.076 Uiso 1 1 calc R . . C49 C 0.2530(5) 0.5404(7) 0.3511(4) 0.089(3) Uani 1 1 d . . . H49A H 0.2249 0.4934 0.3577 0.133 Uiso 1 1 calc R . . H49B H 0.2835 0.5080 0.3378 0.133 Uiso 1 1 calc R . . H49C H 0.2318 0.5861 0.3223 0.133 Uiso 1 1 calc R . . C50 C 0.3285(5) 0.6690(8) 0.3973(5) 0.111(4) Uani 1 1 d . . . H50A H 0.3483 0.7024 0.4328 0.167 Uiso 1 1 calc R . . H50B H 0.3071 0.7150 0.3687 0.167 Uiso 1 1 calc R . . H50C H 0.3583 0.6361 0.3833 0.167 Uiso 1 1 calc R . . C51 C 0.1933(5) 0.6511(8) 0.5768(5) 0.090(4) Uani 1 1 d . . . H51A H 0.2089 0.5855 0.5876 0.108 Uiso 1 1 calc R . . C52 C 0.1312(6) 0.6554(9) 0.5863(6) 0.128(5) Uani 1 1 d . . . H52A H 0.1044 0.6109 0.5604 0.192 Uiso 1 1 calc R . . H52B H 0.1153 0.7200 0.5789 0.192 Uiso 1 1 calc R . . H52C H 0.1343 0.6379 0.6258 0.192 Uiso 1 1 calc R . . C53 C 0.2367(6) 0.7229(10) 0.6214(6) 0.138(6) Uani 1 1 d . . . H53A H 0.2768 0.7193 0.6171 0.207 Uiso 1 1 calc R . . H53B H 0.2379 0.7048 0.6603 0.207 Uiso 1 1 calc R . . H53C H 0.2216 0.7880 0.6139 0.207 Uiso 1 1 calc R . . C54 C 0.4386(5) 0.4947(8) 0.6904(4) 0.097(4) Uani 1 1 d . . . H54A H 0.4198 0.5030 0.7209 0.146 Uiso 1 1 calc R . . H54B H 0.4683 0.5448 0.6931 0.146 Uiso 1 1 calc R . . H54C H 0.4581 0.4325 0.6943 0.146 Uiso 1 1 calc R . . C55 C 0.3903(4) 0.5009(8) 0.6313(4) 0.066(3) Uani 1 1 d . . . C56 C 0.3854(5) 0.5912(7) 0.6032(4) 0.070(3) Uani 1 1 d . . . H56A H 0.4184 0.6325 0.6160 0.084 Uiso 1 1 calc R . . C57 C 0.3368(5) 0.6268(6) 0.5581(4) 0.060(3) Uani 1 1 d . . . C58 C 0.3428(5) 0.7342(6) 0.5428(5) 0.086(3) Uani 1 1 d . . . H58A H 0.3071 0.7539 0.5130 0.129 Uiso 1 1 calc R . . H58B H 0.3777 0.7422 0.5290 0.129 Uiso 1 1 calc R . . H58C H 0.3473 0.7735 0.5768 0.129 Uiso 1 1 calc R . . C59 C 0.1429(4) 0.3461(6) 0.4941(3) 0.052(2) Uani 1 1 d . . . C60 C 0.1192(5) 0.4127(9) 0.5240(5) 0.092(4) Uani 1 1 d . . . H60A H 0.1377 0.4732 0.5313 0.110 Uiso 1 1 calc R . . C61 C 0.0716(6) 0.3960(11) 0.5431(6) 0.118(5) Uani 1 1 d . . . H61A H 0.0601 0.4423 0.5660 0.142 Uiso 1 1 calc R . . C62 C 0.0380(6) 0.3097(12) 0.5292(6) 0.108(4) Uani 1 1 d . . . H62A H 0.0031 0.2988 0.5403 0.129 Uiso 1 1 calc R . . C63 C 0.0601(5) 0.2423(9) 0.4982(5) 0.087(4) Uani 1 1 d . . . H63A H 0.0406 0.1827 0.4895 0.105 Uiso 1 1 calc R . . C64 C 0.1083(4) 0.2605(7) 0.4807(4) 0.060(3) Uani 1 1 d . . . H64A H 0.1201 0.2139 0.4582 0.072 Uiso 1 1 calc R . . C65 C 0.2593(4) 0.1791(6) 0.5432(3) 0.052(2) Uani 1 1 d . . . C66 C 0.2706(5) 0.0864(7) 0.5256(5) 0.095(4) Uani 1 1 d . . . H66A H 0.2868 0.0772 0.4948 0.114 Uiso 1 1 calc R . . C67 C 0.2565(7) 0.0064(9) 0.5567(7) 0.129(5) Uani 1 1 d . . . H67A H 0.2630 -0.0563 0.5457 0.155 Uiso 1 1 calc R . . C68 C 0.2343(7) 0.0195(10) 0.6008(6) 0.112(5) Uani 1 1 d . . . H68A H 0.2261 -0.0344 0.6206 0.135 Uiso 1 1 calc R . . C69 C 0.2233(5) 0.1072(10) 0.6179(4) 0.093(4) Uani 1 1 d . . . H69A H 0.2069 0.1144 0.6488 0.112 Uiso 1 1 calc R . . C70 C 0.2366(4) 0.1894(7) 0.5892(4) 0.068(3) Uani 1 1 d . . . H70A H 0.2297 0.2511 0.6016 0.081 Uiso 1 1 calc R . . C71 C 0.0610(15) -0.0341(18) 0.512(3) 0.186(10) Uani 1 1 d . . . H71A H 0.1006 -0.0554 0.5176 0.223 Uiso 1 1 calc R . . C72 C 0.041(3) -0.003(3) 0.5563(15) 0.192(12) Uani 1 1 d . . . C73 C -0.020(3) 0.0329(19) 0.542(2) 0.172(10) Uani 1 1 d . . . H73A H -0.0331 0.0574 0.5727 0.207 Uiso 1 1 calc R . . C74 C -0.043(2) 0.728(2) 0.2639(11) 0.189(11) Uani 1 1 d . . . C75 C -0.0918(17) 0.679(3) 0.254(2) 0.28(3) Uani 1 1 d . . . H75A H -0.1158 0.6908 0.2783 0.340 Uiso 1 1 calc R . . C76 C -0.112(2) 0.614(4) 0.213(3) 0.31(3) Uani 1 1 d . . . H76A H -0.1468 0.5763 0.2091 0.375 Uiso 1 1 calc R . . C77 C -0.073(2) 0.609(2) 0.1720(12) 0.206(15) Uani 1 1 d . . . H77A H -0.0817 0.5669 0.1403 0.248 Uiso 1 1 calc R . . C78 C -0.0182(15) 0.675(3) 0.186(2) 0.210(15) Uani 1 1 d . . . H78A H 0.0086 0.6760 0.1637 0.252 Uiso 1 1 calc R . . C79 C -0.0110(13) 0.730(2) 0.2320(16) 0.208(16) Uani 1 1 d . . . H79A H 0.0211 0.7736 0.2405 0.250 Uiso 1 1 calc R . . C80 C -0.0295(14) 0.7938(16) 0.3115(10) 0.312(19) Uani 1 1 d . . . H80A H 0.0069 0.8289 0.3130 0.468 Uiso 1 1 calc R . . H80B H -0.0239 0.7581 0.3470 0.468 Uiso 1 1 calc R . . H80C H -0.0625 0.8385 0.3068 0.468 Uiso 1 1 calc R . . C81 C 0.076(3) -0.005(4) 0.606(2) 0.28(4) Uani 0.50 1 d P . . H81A H 0.1146 -0.0308 0.6042 0.415 Uiso 0.50 1 calc PR . . H81B H 0.0599 -0.0458 0.6298 0.415 Uiso 0.50 1 calc PR . . H81C H 0.0820 0.0594 0.6215 0.415 Uiso 0.50 1 calc PR . . 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 0.0565(7) 0.0319(6) 0.0234(5) -0.0013(5) 0.0011(5) -0.0039(5) Ni2 0.0658(8) 0.0394(6) 0.0241(5) -0.0036(5) 0.0042(6) -0.0109(6) P1 0.0581(16) 0.0392(13) 0.0307(11) -0.0032(10) 0.0023(12) -0.0048(12) P2 0.0708(17) 0.0396(13) 0.0245(10) 0.0029(10) 0.0036(12) -0.0082(12) N1 0.061(5) 0.030(4) 0.024(4) -0.001(3) -0.024(4) -0.006(3) N2 0.059(5) 0.040(4) 0.024(3) -0.003(3) 0.005(4) -0.007(4) N3 0.062(5) 0.061(5) 0.025(4) -0.005(4) -0.005(4) -0.023(4) N4 0.092(6) 0.033(4) 0.046(4) -0.010(4) 0.016(5) -0.015(5) C1 0.066(7) 0.043(6) 0.038(5) -0.005(5) 0.013(5) 0.004(5) C2 0.056(7) 0.055(6) 0.047(5) 0.010(5) 0.007(5) 0.009(6) C3 0.067(8) 0.079(8) 0.076(7) -0.001(6) 0.004(7) 0.009(6) C4 0.072(9) 0.101(10) 0.089(9) 0.005(8) 0.004(8) 0.039(8) C5 0.094(9) 0.054(7) 0.095(9) 0.017(7) 0.023(8) 0.028(7) C6 0.076(8) 0.049(6) 0.057(6) -0.005(5) 0.016(6) 0.013(6) C7 0.069(7) 0.047(6) 0.061(6) -0.004(5) 0.011(6) -0.013(5) C8 0.088(7) 0.058(6) 0.052(5) 0.000(5) 0.008(6) -0.018(6) C9 0.154(11) 0.076(8) 0.067(7) -0.007(6) 0.027(8) -0.044(7) C10 0.097(8) 0.044(6) 0.081(7) -0.003(6) 0.024(7) 0.006(6) C11 0.190(13) 0.059(8) 0.096(9) -0.032(7) 0.038(10) -0.018(8) C12 0.133(10) 0.039(6) 0.149(12) 0.016(7) 0.044(9) 0.011(6) C13 0.069(7) 0.059(7) 0.027(4) 0.004(4) 0.004(5) -0.006(6) C14 0.053(7) 0.070(7) 0.051(6) 0.008(5) -0.003(6) -0.005(6) C15 0.068(9) 0.092(10) 0.084(8) 0.015(7) 0.007(7) 0.001(7) C16 0.069(9) 0.125(13) 0.110(10) 0.022(10) 0.003(8) -0.037(9) C17 0.076(9) 0.077(9) 0.099(9) 0.003(8) -0.005(8) -0.035(8) C18 0.074(8) 0.065(7) 0.052(6) -0.001(5) 0.000(6) -0.030(6) C19 0.072(7) 0.067(8) 0.060(6) 0.014(6) 0.005(6) 0.011(6) C20 0.181(13) 0.078(9) 0.090(9) 0.029(8) 0.019(9) 0.017(9) C21 0.114(10) 0.088(9) 0.117(10) -0.003(8) 0.034(9) 0.023(8) C22 0.084(8) 0.053(7) 0.087(8) -0.018(6) -0.002(7) -0.024(6) C23 0.147(12) 0.107(11) 0.107(10) 0.036(9) 0.024(10) 0.010(9) C24 0.218(16) 0.101(11) 0.132(12) -0.069(10) -0.016(12) 0.012(11) C25 0.092(8) 0.073(7) 0.052(6) -0.009(5) 0.023(6) -0.011(6) C26 0.078(7) 0.032(5) 0.041(5) -0.006(4) 0.016(6) -0.009(5) C27 0.089(8) 0.052(6) 0.028(5) -0.002(4) 0.014(6) -0.012(6) C28 0.072(7) 0.044(5) 0.031(5) 0.002(4) 0.007(5) -0.004(5) C29 0.086(7) 0.083(8) 0.032(5) -0.004(5) -0.007(6) 0.004(6) C30 0.073(7) 0.072(7) 0.020(4) 0.002(5) -0.002(5) -0.033(6) C31 0.058(7) 0.091(9) 0.036(5) 0.020(6) -0.008(5) -0.025(6) C32 0.109(10) 0.109(10) 0.051(6) 0.037(7) -0.010(7) -0.028(8) C33 0.126(12) 0.127(13) 0.052(7) 0.043(9) -0.004(8) -0.034(10) C34 0.138(13) 0.148(14) 0.040(6) -0.002(9) 0.035(8) -0.037(10) C35 0.079(8) 0.100(9) 0.031(5) -0.001(6) 0.005(6) -0.029(7) C36 0.073(8) 0.081(8) 0.073(7) 0.027(7) -0.005(7) 0.004(6) C37 0.144(12) 0.123(13) 0.114(10) 0.013(10) 0.032(10) 0.006(10) C38 0.092(10) 0.161(14) 0.158(14) -0.027(12) 0.013(10) -0.042(10) C39 0.145(13) 0.146(14) 0.053(7) -0.013(8) 0.056(8) -0.005(11) C40 0.134(13) 0.176(17) 0.159(15) 0.007(13) 0.036(12) 0.002(12) C41 0.27(2) 0.26(2) 0.149(15) -0.128(16) 0.081(15) -0.037(18) C42 0.076(7) 0.028(5) 0.054(6) -0.006(5) 0.004(6) -0.010(5) C43 0.085(8) 0.040(6) 0.062(6) 0.003(5) 0.009(6) -0.002(5) C44 0.100(9) 0.061(8) 0.093(9) 0.008(7) 0.004(8) 0.013(7) C45 0.131(12) 0.060(8) 0.108(11) 0.021(8) 0.010(10) 0.025(8) C46 0.122(11) 0.053(8) 0.134(12) -0.010(8) 0.036(10) 0.027(7) C47 0.068(7) 0.049(6) 0.082(7) -0.021(6) 0.022(7) -0.009(6) C48 0.089(8) 0.052(6) 0.044(5) 0.011(5) 0.011(6) -0.007(6) C49 0.137(10) 0.055(7) 0.059(6) -0.003(6) 0.006(7) 0.007(6) C50 0.139(11) 0.095(9) 0.107(9) -0.007(8) 0.046(9) -0.040(8) C51 0.133(11) 0.060(7) 0.089(8) -0.027(7) 0.049(8) -0.006(7) C52 0.141(11) 0.118(11) 0.152(12) -0.037(10) 0.087(11) 0.010(9) C53 0.177(14) 0.119(12) 0.136(12) -0.064(10) 0.075(11) -0.042(10) C54 0.110(9) 0.109(10) 0.046(6) -0.005(6) -0.020(7) -0.042(7) C55 0.064(7) 0.086(8) 0.037(5) -0.010(6) -0.003(6) -0.017(6) C56 0.085(8) 0.060(7) 0.058(6) -0.014(6) 0.008(7) -0.030(6) C57 0.083(8) 0.036(6) 0.053(6) -0.013(5) 0.007(6) -0.011(6) C58 0.118(9) 0.039(6) 0.088(8) -0.012(6) 0.009(7) -0.032(6) C59 0.062(6) 0.047(6) 0.036(5) 0.000(4) -0.003(5) 0.001(5) C60 0.087(8) 0.092(9) 0.112(9) -0.039(8) 0.053(8) -0.033(7) C61 0.110(10) 0.111(11) 0.156(13) -0.051(10) 0.075(10) -0.025(9) C62 0.087(9) 0.151(14) 0.095(9) 0.015(10) 0.042(8) -0.008(10) C63 0.091(9) 0.083(9) 0.084(8) 0.013(7) 0.020(8) -0.037(7) C64 0.066(7) 0.066(7) 0.050(5) 0.007(5) 0.020(6) -0.019(5) C65 0.068(7) 0.041(6) 0.038(5) 0.009(4) 0.000(5) -0.008(5) C66 0.169(12) 0.043(7) 0.093(8) 0.013(6) 0.069(9) 0.007(7) C67 0.214(16) 0.058(8) 0.135(13) 0.009(9) 0.083(12) 0.014(9) C68 0.183(14) 0.064(9) 0.095(10) 0.019(8) 0.047(10) -0.024(9) C69 0.126(10) 0.098(10) 0.055(6) 0.023(7) 0.024(7) -0.024(8) C70 0.089(8) 0.064(7) 0.045(5) 0.016(5) 0.012(6) -0.016(6) C71 0.21(3) 0.097(14) 0.28(4) -0.02(2) 0.11(4) -0.040(17) C72 0.26(6) 0.098(16) 0.26(4) 0.00(2) 0.15(4) -0.05(2) C73 0.21(3) 0.090(14) 0.27(4) -0.03(2) 0.15(3) -0.06(2) C74 0.23(3) 0.19(3) 0.125(18) 0.060(19) 0.02(2) 0.09(3) C75 0.14(2) 0.28(5) 0.42(8) 0.11(4) 0.08(3) -0.05(3) C76 0.27(5) 0.26(5) 0.36(7) 0.15(5) 0.02(5) -0.05(3) C77 0.29(4) 0.113(18) 0.15(2) 0.041(16) -0.04(2) 0.07(2) C78 0.25(3) 0.17(3) 0.26(4) 0.14(3) 0.14(3) 0.13(3) C79 0.26(3) 0.21(3) 0.20(3) 0.12(3) 0.14(3) 0.18(3) C80 0.53(5) 0.17(2) 0.131(17) -0.007(18) -0.07(2) 0.09(3) C81 0.29(7) 0.31(7) 0.19(5) 0.00(5) 0.02(5) -0.17(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 N1 1.872(7) . ? Ni1 N2 1.922(6) . ? Ni1 P1 2.233(2) . ? Ni1 P2 2.262(2) . ? Ni2 N3 1.911(6) . ? Ni2 N4 1.929(7) . ? Ni2 P2 2.242(2) . ? Ni2 P1 2.270(2) . ? P1 C59 1.766(9) . ? P1 P2 2.125(3) . ? P2 C65 1.824(8) . ? N1 C26 1.352(10) . ? N1 C1 1.456(10) . ? N2 C28 1.316(9) . ? N2 C13 1.421(10) . ? N3 C55 1.330(11) . ? N3 C30 1.443(10) . ? N4 C57 1.323(10) . ? N4 C42 1.452(11) . ? C1 C2 1.404(11) . ? C1 C6 1.423(12) . ? C2 C3 1.377(12) . ? C2 C7 1.556(12) . ? C3 C4 1.388(14) . ? C4 C5 1.370(14) . ? C5 C6 1.389(13) . ? C6 C10 1.510(13) . ? C7 C9 1.523(12) . ? C7 C8 1.529(12) . ? C10 C11 1.552(14) . ? C10 C12 1.555(13) . ? C13 C18 1.426(12) . ? C13 C14 1.437(12) . ? C14 C15 1.342(12) . ? C14 C19 1.530(13) . ? C15 C16 1.373(15) . ? C16 C17 1.369(15) . ? C17 C18 1.342(13) . ? C18 C22 1.560(14) . ? C19 C21 1.488(13) . ? C19 C20 1.530(14) . ? C22 C23 1.472(14) . ? C22 C24 1.552(14) . ? C25 C26 1.537(11) . ? C26 C27 1.400(12) . ? C27 C28 1.350(11) . ? C28 C29 1.557(11) . ? C30 C35 1.347(12) . ? C30 C31 1.416(13) . ? C31 C32 1.402(13) . ? C31 C36 1.482(13) . ? C32 C33 1.357(16) . ? C33 C34 1.346(16) . ? C34 C35 1.421(15) . ? C35 C39 1.537(16) . ? C36 C38 1.498(14) . ? C36 C37 1.551(15) . ? C39 C40 1.471(15) . ? C39 C41 1.553(17) . ? C42 C43 1.397(12) . ? C42 C47 1.398(12) . ? C43 C44 1.407(13) . ? C43 C48 1.502(12) . ? C44 C45 1.359(15) . ? C45 C46 1.348(16) . ? C46 C47 1.413(15) . ? C47 C51 1.488(14) . ? C48 C50 1.535(12) . ? C48 C49 1.553(12) . ? C51 C52 1.515(13) . ? C51 C53 1.583(15) . ? C54 C55 1.534(13) . ? C55 C56 1.404(13) . ? C56 C57 1.402(12) . ? C57 C58 1.542(12) . ? C59 C60 1.371(12) . ? C59 C64 1.409(11) . ? C60 C61 1.326(13) . ? C61 C62 1.405(16) . ? C62 C63 1.376(15) . ? C63 C64 1.320(12) . ? C65 C70 1.360(11) . ? C65 C66 1.394(12) . ? C66 C67 1.421(14) . ? C67 C68 1.315(16) . ? C68 C69 1.325(15) . ? C69 C70 1.405(13) . ? C71 C72 1.35(4) . ? C71 C73 1.37(3) 3_556 ? C72 C81 1.23(5) . ? C72 C73 1.44(4) . ? C73 C71 1.37(3) 3_556 ? C74 C79 1.20(3) . ? C74 C75 1.28(4) . ? C74 C80 1.42(3) . ? C75 C76 1.32(6) . ? C76 C77 1.52(6) . ? C77 C78 1.51(4) . ? C78 C79 1.31(4) . ? 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 N1 Ni1 N2 95.8(3) . . ? N1 Ni1 P1 153.0(2) . . ? N2 Ni1 P1 104.2(2) . . ? N1 Ni1 P2 108.6(2) . . ? N2 Ni1 P2 153.9(2) . . ? P1 Ni1 P2 56.41(9) . . ? N3 Ni2 N4 96.7(3) . . ? N3 Ni2 P2 103.8(2) . . ? N4 Ni2 P2 153.7(2) . . ? N3 Ni2 P1 154.0(2) . . ? N4 Ni2 P1 107.7(3) . . ? P2 Ni2 P1 56.19(9) . . ? C59 P1 P2 112.6(3) . . ? C59 P1 Ni1 126.3(3) . . ? P2 P1 Ni1 62.50(9) . . ? C59 P1 Ni2 116.5(3) . . ? P2 P1 Ni2 61.24(9) . . ? Ni1 P1 Ni2 106.61(10) . . ? C65 P2 P1 111.1(3) . . ? C65 P2 Ni2 123.7(3) . . ? P1 P2 Ni2 62.57(9) . . ? C65 P2 Ni1 118.0(3) . . ? P1 P2 Ni1 61.09(8) . . ? Ni2 P2 Ni1 106.55(9) . . ? C26 N1 C1 112.4(7) . . ? C26 N1 Ni1 123.2(6) . . ? C1 N1 Ni1 124.1(5) . . ? C28 N2 C13 116.9(7) . . ? C28 N2 Ni1 122.1(6) . . ? C13 N2 Ni1 119.5(5) . . ? C55 N3 C30 117.2(7) . . ? C55 N3 Ni2 123.0(6) . . ? C30 N3 Ni2 118.7(5) . . ? C57 N4 C42 115.4(7) . . ? C57 N4 Ni2 121.8(7) . . ? C42 N4 Ni2 122.8(6) . . ? C2 C1 C6 118.4(9) . . ? C2 C1 N1 121.1(7) . . ? C6 C1 N1 120.4(8) . . ? C3 C2 C1 120.5(9) . . ? C3 C2 C7 117.7(9) . . ? C1 C2 C7 121.8(8) . . ? C2 C3 C4 120.6(11) . . ? C5 C4 C3 119.9(10) . . ? C4 C5 C6 121.1(10) . . ? C5 C6 C1 119.4(9) . . ? C5 C6 C10 120.8(9) . . ? C1 C6 C10 119.8(9) . . ? C9 C7 C8 109.0(7) . . ? C9 C7 C2 111.3(8) . . ? C8 C7 C2 110.2(8) . . ? C6 C10 C11 113.1(9) . . ? C6 C10 C12 112.6(9) . . ? C11 C10 C12 108.7(9) . . ? N2 C13 C18 119.8(9) . . ? N2 C13 C14 123.1(8) . . ? C18 C13 C14 117.0(9) . . ? C15 C14 C13 118.8(10) . . ? C15 C14 C19 119.9(10) . . ? C13 C14 C19 121.3(9) . . ? C14 C15 C16 123.2(11) . . ? C17 C16 C15 118.6(11) . . ? C18 C17 C16 121.8(11) . . ? C17 C18 C13 120.6(10) . . ? C17 C18 C22 119.6(10) . . ? C13 C18 C22 119.8(9) . . ? C21 C19 C14 114.7(9) . . ? C21 C19 C20 108.4(9) . . ? C14 C19 C20 112.8(9) . . ? C23 C22 C24 110.8(10) . . ? C23 C22 C18 111.9(10) . . ? C24 C22 C18 109.4(10) . . ? N1 C26 C27 122.1(8) . . ? N1 C26 C25 121.8(9) . . ? C27 C26 C25 116.1(8) . . ? C28 C27 C26 127.0(8) . . ? N2 C28 C27 125.3(8) . . ? N2 C28 C29 119.0(8) . . ? C27 C28 C29 115.6(8) . . ? C35 C30 C31 121.3(10) . . ? C35 C30 N3 119.5(10) . . ? C31 C30 N3 119.0(8) . . ? C32 C31 C30 117.2(10) . . ? C32 C31 C36 118.3(11) . . ? C30 C31 C36 124.5(9) . . ? C33 C32 C31 120.4(13) . . ? C34 C33 C32 122.4(13) . . ? C33 C34 C35 118.7(12) . . ? C30 C35 C34 119.9(12) . . ? C30 C35 C39 122.6(10) . . ? C34 C35 C39 117.5(11) . . ? C31 C36 C38 114.6(11) . . ? C31 C36 C37 114.9(10) . . ? C38 C36 C37 109.3(10) . . ? C40 C39 C35 112.9(12) . . ? C40 C39 C41 110.1(12) . . ? C35 C39 C41 112.9(13) . . ? C43 C42 C47 122.9(10) . . ? C43 C42 N4 118.2(9) . . ? C47 C42 N4 118.9(9) . . ? C42 C43 C44 116.9(10) . . ? C42 C43 C48 123.8(9) . . ? C44 C43 C48 119.2(9) . . ? C45 C44 C43 121.4(12) . . ? C46 C45 C44 120.3(13) . . ? C45 C46 C47 122.6(12) . . ? C42 C47 C46 115.7(10) . . ? C42 C47 C51 124.1(10) . . ? C46 C47 C51 120.2(11) . . ? C43 C48 C50 113.1(8) . . ? C43 C48 C49 112.1(8) . . ? C50 C48 C49 108.5(8) . . ? C47 C51 C52 116.1(11) . . ? C47 C51 C53 112.4(9) . . ? C52 C51 C53 108.2(9) . . ? N3 C55 C56 122.8(9) . . ? N3 C55 C54 121.4(9) . . ? C56 C55 C54 115.6(9) . . ? C57 C56 C55 128.2(9) . . ? N4 C57 C56 123.3(9) . . ? N4 C57 C58 122.2(9) . . ? C56 C57 C58 114.5(9) . . ? C60 C59 C64 113.3(9) . . ? C60 C59 P1 120.2(8) . . ? C64 C59 P1 126.2(7) . . ? C61 C60 C59 124.0(11) . . ? C60 C61 C62 121.2(12) . . ? C63 C62 C61 115.9(11) . . ? C64 C63 C62 121.3(11) . . ? C63 C64 C59 124.0(10) . . ? C70 C65 C66 119.4(9) . . ? C70 C65 P2 123.0(7) . . ? C66 C65 P2 117.4(7) . . ? C65 C66 C67 117.4(10) . . ? C68 C67 C66 121.3(12) . . ? C67 C68 C69 121.8(13) . . ? C68 C69 C70 119.8(11) . . ? C65 C70 C69 120.3(10) . . ? C72 C71 C73 117(4) . 3_556 ? C81 C72 C71 118(8) . . ? C81 C72 C73 125(7) . . ? C71 C72 C73 117(3) . . ? C71 C73 C72 126(3) 3_556 . ? C79 C74 C75 123(4) . . ? C79 C74 C80 118(5) . . ? C75 C74 C80 118(5) . . ? C74 C75 C76 128(6) . . ? C75 C76 C77 111(5) . . ? C78 C77 C76 116(3) . . ? C79 C78 C77 116(3) . . ? C74 C79 C78 125(4) . . ? _diffrn_measured_fraction_theta_max 0.894 _diffrn_reflns_theta_full 23.40 _diffrn_measured_fraction_theta_full 0.894 _refine_diff_density_max 0.983 _refine_diff_density_min -1.226 _refine_diff_density_rms 0.092 #===end