Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 loop_ _publ_author_name 'Douglas W. Stephan' 'Jason D. Masuda' 'Pingrong Wei' _publ_contact_author_name 'Prof Douglas W. Stephan' _publ_contact_author_address ; Department of Chemistry & Biochemistry University of Windsor 401 Sunset Windsor Ontario N9B3P4 CANADA ; _publ_contact_author_email STEPHAN@UWINDSOR.CA _publ_section_title ; Ni and Pd Phosphinimine-Imine Ligand Complexes ; data_(C6H3i-Pr2)NC(Me)CH2PPh2 _database_code_CSD 211491 _audit_creation_method SHELXL-97 _chemical_formula_sum 'C54 H64 N2 P2' _chemical_formula_weight 803.01 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 21.355(12) _cell_length_b 17.586(10) _cell_length_c 13.052(7) _cell_angle_alpha 90.00 _cell_angle_beta 98.315(12) _cell_angle_gamma 90.00 _cell_volume 4850(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.25 _exptl_crystal_density_diffrn 1.100 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1728 _exptl_absorpt_coefficient_mu 0.125 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.306829 _exptl_absorpt_correction_T_max 0.488921 _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 20418 _diffrn_reflns_av_R_equivalents 0.0407 _diffrn_reflns_av_sigmaI/netI 0.0516 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 23.26 _reflns_number_total 6888 _reflns_number_gt 4287 _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^)+(0.0595P)^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 6888 _refine_ls_number_parameters 523 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0766 _refine_ls_R_factor_gt 0.0390 _refine_ls_wR_factor_ref 0.1028 _refine_ls_wR_factor_gt 0.0925 _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 P1 P 0.64730(3) 0.41182(3) 0.92687(4) 0.04631(17) Uani 1 1 d . . . P2 P 0.12799(3) 1.08842(4) 1.17339(5) 0.0570(2) Uani 1 1 d . . . N1 N 0.50849(7) 0.52013(10) 0.80407(12) 0.0415(4) Uani 1 1 d . . . N2 N -0.02351(8) 0.99206(10) 1.20738(13) 0.0488(5) Uani 1 1 d . . . C1 C 0.65808(10) 0.49990(12) 1.00264(16) 0.0441(6) Uani 1 1 d . . . C2 C 0.71961(11) 0.52851(14) 1.0218(2) 0.0641(7) Uani 1 1 d . . . H2A H 0.7520 0.5031 0.9954 0.077 Uiso 1 1 calc R . . C3 C 0.73319(14) 0.59392(17) 1.0793(2) 0.0810(9) Uani 1 1 d . . . H3A H 0.7746 0.6117 1.0919 0.097 Uiso 1 1 calc R . . C4 C 0.68605(16) 0.63295(16) 1.1180(2) 0.0766(8) Uani 1 1 d . . . H4A H 0.6953 0.6771 1.1565 0.092 Uiso 1 1 calc R . . C5 C 0.62522(13) 0.60612(14) 1.0992(2) 0.0684(7) Uani 1 1 d . . . H5A H 0.5930 0.6325 1.1247 0.082 Uiso 1 1 calc R . . C6 C 0.61118(11) 0.54019(13) 1.04256(18) 0.0580(6) Uani 1 1 d . . . H6A H 0.5697 0.5226 1.0311 0.070 Uiso 1 1 calc R . . C7 C 0.65595(9) 0.33977(11) 1.02983(16) 0.0433(5) Uani 1 1 d . . . C8 C 0.62422(11) 0.34125(13) 1.11563(17) 0.0533(6) Uani 1 1 d . . . H8A H 0.5957 0.3802 1.1227 0.064 Uiso 1 1 calc R . . C9 C 0.63468(12) 0.28523(15) 1.19069(18) 0.0646(7) Uani 1 1 d . . . H9A H 0.6131 0.2868 1.2477 0.078 Uiso 1 1 calc R . . C10 C 0.67687(13) 0.22710(15) 1.1814(2) 0.0693(8) Uani 1 1 d . . . H10A H 0.6840 0.1898 1.2322 0.083 Uiso 1 1 calc R . . C11 C 0.70830(13) 0.22444(14) 1.0969(2) 0.0712(8) Uani 1 1 d . . . H11A H 0.7365 0.1851 1.0901 0.085 Uiso 1 1 calc R . . C12 C 0.69790(10) 0.28046(13) 1.02175(19) 0.0581(6) Uani 1 1 d . . . H12A H 0.7194 0.2783 0.9648 0.070 Uiso 1 1 calc R . . C13 C 0.55998(9) 0.40871(11) 0.88368(16) 0.0458(6) Uani 1 1 d . . . H13A H 0.5474 0.3570 0.8646 0.055 Uiso 1 1 calc R . . H13B H 0.5381 0.4240 0.9404 0.055 Uiso 1 1 calc R . . C14 C 0.54109(10) 0.46085(12) 0.79198(16) 0.0443(5) Uani 1 1 d . . . C15 C 0.56441(14) 0.43746(16) 0.69335(18) 0.0814(9) Uani 1 1 d . . . H15A H 0.5511 0.4742 0.6403 0.122 Uiso 1 1 calc R . . H15B H 0.5473 0.3886 0.6721 0.122 Uiso 1 1 calc R . . H15C H 0.6098 0.4347 0.7047 0.122 Uiso 1 1 calc R . . C16 C 0.49217(10) 0.57215(11) 0.71888(16) 0.0420(5) Uani 1 1 d . . . C17 C 0.52744(10) 0.63941(12) 0.71775(17) 0.0500(6) Uani 1 1 d . . . C18 C 0.50987(12) 0.69105(13) 0.63729(19) 0.0620(7) Uani 1 1 d . . . H18A H 0.5334 0.7352 0.6341 0.074 Uiso 1 1 calc R . . C19 C 0.45851(12) 0.67795(14) 0.56271(18) 0.0610(7) Uani 1 1 d . . . H19A H 0.4475 0.7131 0.5099 0.073 Uiso 1 1 calc R . . C20 C 0.42362(11) 0.61258(14) 0.56678(17) 0.0561(6) Uani 1 1 d . . . H20A H 0.3886 0.6046 0.5167 0.067 Uiso 1 1 calc R . . C21 C 0.43912(10) 0.55777(12) 0.64366(16) 0.0460(6) Uani 1 1 d . . . C22 C 0.39830(10) 0.48670(13) 0.64452(18) 0.0573(6) Uani 1 1 d . . . H22A H 0.4175 0.4543 0.7017 0.069 Uiso 1 1 calc R . . C23 C 0.33119(12) 0.50730(17) 0.6643(2) 0.0853(9) Uani 1 1 d . . . H23A H 0.3335 0.5354 0.7278 0.128 Uiso 1 1 calc R . . H23B H 0.3073 0.4616 0.6694 0.128 Uiso 1 1 calc R . . H23C H 0.3108 0.5378 0.6081 0.128 Uiso 1 1 calc R . . C24 C 0.39504(14) 0.44058(15) 0.5439(2) 0.0857(9) Uani 1 1 d . . . H24A H 0.4371 0.4276 0.5323 0.129 Uiso 1 1 calc R . . H24B H 0.3748 0.4704 0.4869 0.129 Uiso 1 1 calc R . . H24C H 0.3711 0.3949 0.5497 0.129 Uiso 1 1 calc R . . C25 C 0.58361(12) 0.65618(14) 0.8011(2) 0.0664(7) Uani 1 1 d . . . H25A H 0.5841 0.6170 0.8546 0.080 Uiso 1 1 calc R . . C26 C 0.57698(16) 0.73268(19) 0.8527(3) 0.1297(14) Uani 1 1 d . . . H26A H 0.5375 0.7344 0.8795 0.195 Uiso 1 1 calc R . . H26B H 0.5781 0.7726 0.8027 0.195 Uiso 1 1 calc R . . H26C H 0.6112 0.7393 0.9083 0.195 Uiso 1 1 calc R . . C27 C 0.64613(15) 0.6514(3) 0.7593(3) 0.1507(16) Uani 1 1 d . . . H27A H 0.6501 0.6021 0.7291 0.226 Uiso 1 1 calc R . . H27B H 0.6803 0.6590 0.8148 0.226 Uiso 1 1 calc R . . H27C H 0.6476 0.6899 0.7076 0.226 Uiso 1 1 calc R . . C28 C 0.14209(10) 0.98801(14) 1.1412(2) 0.0570(6) Uani 1 1 d . . . C29 C 0.11435(14) 0.95231(16) 1.0509(2) 0.0775(8) Uani 1 1 d . . . H29A H 0.0874 0.9799 1.0022 0.093 Uiso 1 1 calc R . . C30 C 0.12606(17) 0.87673(18) 1.0320(3) 0.0983(10) Uani 1 1 d . . . H30A H 0.1063 0.8536 0.9718 0.118 Uiso 1 1 calc R . . C31 C 0.16693(19) 0.8356(2) 1.1021(4) 0.1080(12) Uani 1 1 d . . . H31A H 0.1751 0.7848 1.0891 0.130 Uiso 1 1 calc R . . C32 C 0.19573(14) 0.8698(2) 1.1915(4) 0.1021(12) Uani 1 1 d . . . H32A H 0.2237 0.8423 1.2389 0.123 Uiso 1 1 calc R . . C33 C 0.18297(11) 0.94541(17) 1.2109(2) 0.0789(8) Uani 1 1 d . . . H33A H 0.2022 0.9679 1.2719 0.095 Uiso 1 1 calc R . . C34 C 0.14769(10) 1.13846(12) 1.05841(18) 0.0523(6) Uani 1 1 d . . . C35 C 0.10690(12) 1.15222(14) 0.96746(19) 0.0656(7) Uani 1 1 d . . . H35A H 0.0653 1.1352 0.9612 0.079 Uiso 1 1 calc R . . C36 C 0.12731(13) 1.19107(15) 0.8856(2) 0.0711(8) Uani 1 1 d . . . H36A H 0.0993 1.2003 0.8255 0.085 Uiso 1 1 calc R . . C37 C 0.18890(14) 1.21589(15) 0.8934(2) 0.0763(8) Uani 1 1 d . . . H37A H 0.2027 1.2412 0.8382 0.092 Uiso 1 1 calc R . . C38 C 0.22974(13) 1.20320(16) 0.9827(3) 0.0848(9) Uani 1 1 d . . . H38A H 0.2714 1.2199 0.9879 0.102 Uiso 1 1 calc R . . C39 C 0.20961(11) 1.16571(14) 1.0654(2) 0.0693(7) Uani 1 1 d . . . H39A H 0.2376 1.1586 1.1262 0.083 Uiso 1 1 calc R . . C40 C 0.04023(10) 1.09103(13) 1.15077(18) 0.0534(6) Uani 1 1 d . . . H40A H 0.0264 1.1436 1.1480 0.064 Uiso 1 1 calc R . . H40B H 0.0253 1.0680 1.0842 0.064 Uiso 1 1 calc R . . C41 C 0.01076(11) 1.04993(13) 1.23386(18) 0.0522(6) Uani 1 1 d . . . C42 C 0.02472(14) 1.08179(17) 1.3418(2) 0.0879(9) Uani 1 1 d . . . H42A H 0.0042 1.0512 1.3880 0.132 Uiso 1 1 calc R . . H42B H 0.0093 1.1330 1.3422 0.132 Uiso 1 1 calc R . . H42C H 0.0696 1.0814 1.3640 0.132 Uiso 1 1 calc R . . C43 C -0.05385(11) 0.94990(13) 1.28068(16) 0.0489(6) Uani 1 1 d . . . C44 C -0.02149(11) 0.88982(13) 1.33663(18) 0.0543(6) Uani 1 1 d . . . C45 C -0.05435(13) 0.84616(15) 1.39989(19) 0.0669(7) Uani 1 1 d . . . H45A H -0.0336 0.8067 1.4382 0.080 Uiso 1 1 calc R . . C46 C -0.11728(14) 0.86014(16) 1.4070(2) 0.0744(8) Uani 1 1 d . . . H46A H -0.1385 0.8301 1.4496 0.089 Uiso 1 1 calc R . . C47 C -0.14854(12) 0.91884(16) 1.3508(2) 0.0692(7) Uani 1 1 d . . . H47A H -0.1908 0.9279 1.3562 0.083 Uiso 1 1 calc R . . C48 C -0.11825(11) 0.96465(14) 1.28615(18) 0.0563(6) Uani 1 1 d . . . C49 C -0.15391(11) 1.02778(15) 1.22260(19) 0.0641(7) Uani 1 1 d . . . H49A H -0.1286 1.0418 1.1686 0.077 Uiso 1 1 calc R . . C50 C -0.16028(15) 1.09915(17) 1.2868(3) 0.1107(12) Uani 1 1 d . . . H50A H -0.1193 1.1140 1.3212 0.166 Uiso 1 1 calc R . . H50B H -0.1876 1.0888 1.3373 0.166 Uiso 1 1 calc R . . H50C H -0.1779 1.1395 1.2421 0.166 Uiso 1 1 calc R . . C51 C -0.21869(13) 1.00379(18) 1.1679(3) 0.1079(12) Uani 1 1 d . . . H51A H -0.2144 0.9591 1.1273 0.162 Uiso 1 1 calc R . . H51B H -0.2365 1.0441 1.1234 0.162 Uiso 1 1 calc R . . H51C H -0.2460 0.9930 1.2184 0.162 Uiso 1 1 calc R . . C52 C 0.04698(11) 0.87016(15) 1.3273(2) 0.0662(7) Uani 1 1 d . . . H52A H 0.0613 0.9063 1.2784 0.079 Uiso 1 1 calc R . . C53 C 0.05263(16) 0.79054(19) 1.2830(3) 0.1268(14) Uani 1 1 d . . . H53B H 0.0260 0.7867 1.2173 0.190 Uiso 1 1 calc R . . H53C H 0.0397 0.7536 1.3299 0.190 Uiso 1 1 calc R . . H53D H 0.0958 0.7812 1.2739 0.190 Uiso 1 1 calc R . . C54 C 0.09083(14) 0.8785(2) 1.4298(3) 0.1360(15) Uani 1 1 d . . . H54B H 0.0873 0.9290 1.4562 0.204 Uiso 1 1 calc R . . H54C H 0.1337 0.8694 1.4191 0.204 Uiso 1 1 calc R . . H54D H 0.0791 0.8423 1.4788 0.204 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 P1 0.0479(3) 0.0473(4) 0.0436(3) 0.0032(3) 0.0060(3) 0.0061(3) P2 0.0522(4) 0.0617(4) 0.0561(4) 0.0023(3) 0.0044(3) -0.0064(3) N1 0.0433(10) 0.0405(11) 0.0399(10) 0.0045(8) 0.0032(8) 0.0010(9) N2 0.0480(11) 0.0512(12) 0.0480(11) 0.0039(10) 0.0094(9) -0.0004(9) C1 0.0437(13) 0.0447(14) 0.0437(13) 0.0092(10) 0.0051(11) -0.0024(11) C2 0.0537(16) 0.0606(17) 0.0784(18) 0.0027(14) 0.0111(13) -0.0066(13) C3 0.0696(19) 0.071(2) 0.098(2) -0.0017(18) -0.0023(17) -0.0270(16) C4 0.104(2) 0.0565(18) 0.0679(18) -0.0088(14) 0.0065(17) -0.0220(17) C5 0.084(2) 0.0541(17) 0.0699(18) -0.0104(14) 0.0198(15) -0.0037(14) C6 0.0561(15) 0.0526(15) 0.0664(16) -0.0056(13) 0.0131(13) -0.0051(12) C7 0.0432(13) 0.0407(13) 0.0434(14) -0.0030(10) -0.0024(11) 0.0035(10) C8 0.0624(16) 0.0481(15) 0.0482(15) -0.0004(12) 0.0044(13) 0.0031(11) C9 0.0789(18) 0.0617(18) 0.0514(16) 0.0093(13) 0.0027(14) -0.0111(15) C10 0.0807(19) 0.0513(17) 0.0667(19) 0.0194(14) -0.0206(16) -0.0138(15) C11 0.0752(19) 0.0524(17) 0.080(2) 0.0093(15) -0.0089(17) 0.0175(13) C12 0.0588(15) 0.0538(16) 0.0608(16) 0.0008(13) 0.0057(12) 0.0124(12) C13 0.0544(14) 0.0362(13) 0.0443(13) 0.0018(10) -0.0010(11) -0.0003(10) C14 0.0495(13) 0.0415(14) 0.0406(13) 0.0026(11) 0.0017(11) 0.0024(11) C15 0.113(2) 0.085(2) 0.0465(16) 0.0059(14) 0.0138(15) 0.0465(17) C16 0.0482(13) 0.0381(13) 0.0407(13) 0.0058(10) 0.0097(11) 0.0099(10) C17 0.0581(15) 0.0415(14) 0.0508(14) 0.0058(11) 0.0085(12) 0.0062(11) C18 0.0789(18) 0.0414(15) 0.0671(17) 0.0125(13) 0.0148(15) 0.0046(12) C19 0.0787(18) 0.0527(16) 0.0514(15) 0.0174(12) 0.0084(14) 0.0194(14) C20 0.0604(15) 0.0606(17) 0.0457(14) 0.0059(12) 0.0021(12) 0.0146(13) C21 0.0479(13) 0.0489(14) 0.0411(13) 0.0057(11) 0.0061(11) 0.0098(10) C22 0.0517(15) 0.0660(17) 0.0513(15) 0.0095(13) -0.0024(12) 0.0014(12) C23 0.0611(18) 0.103(2) 0.092(2) -0.0049(17) 0.0116(15) -0.0107(15) C24 0.098(2) 0.071(2) 0.086(2) -0.0108(17) 0.0081(17) -0.0063(16) C25 0.0710(18) 0.0496(16) 0.0732(17) 0.0132(13) -0.0073(14) -0.0123(12) C26 0.142(3) 0.103(3) 0.128(3) -0.046(2) -0.035(2) 0.005(2) C27 0.063(2) 0.228(5) 0.154(4) -0.017(3) -0.007(2) -0.001(2) C28 0.0441(13) 0.0628(16) 0.0658(17) 0.0156(14) 0.0134(13) 0.0057(12) C29 0.098(2) 0.0618(19) 0.072(2) 0.0055(15) 0.0130(17) 0.0123(15) C30 0.135(3) 0.066(2) 0.099(2) -0.0036(19) 0.033(2) 0.010(2) C31 0.109(3) 0.069(2) 0.159(4) 0.019(3) 0.065(3) 0.024(2) C32 0.064(2) 0.087(3) 0.159(4) 0.051(3) 0.027(2) 0.0285(18) C33 0.0487(16) 0.088(2) 0.099(2) 0.0262(18) 0.0055(15) 0.0044(15) C34 0.0503(15) 0.0464(14) 0.0602(16) -0.0020(12) 0.0084(12) -0.0050(11) C35 0.0656(16) 0.0671(17) 0.0632(17) 0.0016(14) 0.0066(14) -0.0208(13) C36 0.087(2) 0.0687(19) 0.0565(17) 0.0021(14) 0.0060(15) -0.0231(15) C37 0.092(2) 0.0626(18) 0.079(2) 0.0053(15) 0.0279(18) -0.0174(16) C38 0.0590(17) 0.086(2) 0.113(3) 0.0217(19) 0.0233(18) -0.0168(15) C39 0.0533(16) 0.0639(17) 0.089(2) 0.0134(15) 0.0036(14) -0.0063(13) C40 0.0541(14) 0.0460(14) 0.0613(15) 0.0072(12) 0.0129(12) 0.0019(11) C41 0.0525(14) 0.0505(15) 0.0549(15) -0.0010(12) 0.0126(12) 0.0038(12) C42 0.106(2) 0.094(2) 0.0696(19) -0.0231(16) 0.0305(17) -0.0302(17) C43 0.0550(15) 0.0512(15) 0.0418(13) -0.0024(11) 0.0110(12) -0.0034(12) C44 0.0562(15) 0.0563(16) 0.0512(14) 0.0064(12) 0.0105(12) -0.0033(12) C45 0.0729(19) 0.0659(18) 0.0632(17) 0.0144(14) 0.0141(14) -0.0033(14) C46 0.082(2) 0.078(2) 0.0675(18) 0.0131(16) 0.0271(16) -0.0128(16) C47 0.0583(16) 0.085(2) 0.0689(17) 0.0032(16) 0.0243(14) -0.0037(15) C48 0.0529(16) 0.0636(16) 0.0540(15) -0.0007(13) 0.0133(12) -0.0039(13) C49 0.0547(15) 0.0742(18) 0.0653(17) 0.0072(14) 0.0143(13) 0.0063(13) C50 0.122(3) 0.079(2) 0.119(3) -0.008(2) -0.023(2) 0.0175(19) C51 0.085(2) 0.097(3) 0.128(3) -0.007(2) -0.032(2) 0.0070(17) C52 0.0597(17) 0.0665(18) 0.0725(18) 0.0185(14) 0.0096(14) 0.0031(13) C53 0.104(3) 0.079(2) 0.209(4) -0.006(3) 0.066(3) 0.0073(19) C54 0.075(2) 0.218(5) 0.106(3) 0.015(3) -0.014(2) 0.018(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 P1 C1 1.834(2) . ? P1 C7 1.837(2) . ? P1 C13 1.869(2) . ? P2 C34 1.840(3) . ? P2 C28 1.850(3) . ? P2 C40 1.855(2) . ? N1 C14 1.276(3) . ? N1 C16 1.443(2) . ? N2 C41 1.272(3) . ? N2 C43 1.437(3) . ? C1 C6 1.388(3) . ? C1 C2 1.396(3) . ? C2 C3 1.381(4) . ? C3 C4 1.373(4) . ? C4 C5 1.371(4) . ? C5 C6 1.384(3) . ? C7 C12 1.389(3) . ? C7 C8 1.391(3) . ? C8 C9 1.385(3) . ? C9 C10 1.380(4) . ? C10 C11 1.372(4) . ? C11 C12 1.385(3) . ? C13 C14 1.515(3) . ? C14 C15 1.503(3) . ? C16 C17 1.403(3) . ? C16 C21 1.411(3) . ? C17 C18 1.398(3) . ? C17 C25 1.527(3) . ? C18 C19 1.377(3) . ? C19 C20 1.375(3) . ? C20 C21 1.396(3) . ? C21 C22 1.525(3) . ? C22 C24 1.536(3) . ? C22 C23 1.536(3) . ? C25 C27 1.516(4) . ? C25 C26 1.520(4) . ? C28 C33 1.386(3) . ? C28 C29 1.390(3) . ? C29 C30 1.381(4) . ? C30 C31 1.375(4) . ? C31 C32 1.376(5) . ? C32 C33 1.388(4) . ? C34 C35 1.388(3) . ? C34 C39 1.397(3) . ? C35 C36 1.390(3) . ? C36 C37 1.376(3) . ? C37 C38 1.369(4) . ? C38 C39 1.385(4) . ? C40 C41 1.514(3) . ? C41 C42 1.505(3) . ? C43 C44 1.408(3) . ? C43 C48 1.411(3) . ? C44 C45 1.390(3) . ? C44 C52 1.524(3) . ? C45 C46 1.383(3) . ? C46 C47 1.382(3) . ? C47 C48 1.392(3) . ? C48 C49 1.522(3) . ? C49 C51 1.522(3) . ? C49 C50 1.526(4) . ? C52 C54 1.525(4) . ? C52 C53 1.526(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 C1 P1 C7 101.34(10) . . ? C1 P1 C13 103.26(10) . . ? C7 P1 C13 101.00(9) . . ? C34 P2 C28 101.97(11) . . ? C34 P2 C40 101.72(10) . . ? C28 P2 C40 100.45(10) . . ? C14 N1 C16 119.87(18) . . ? C41 N2 C43 121.95(19) . . ? C6 C1 C2 117.4(2) . . ? C6 C1 P1 126.32(17) . . ? C2 C1 P1 116.27(18) . . ? C3 C2 C1 121.1(2) . . ? C4 C3 C2 120.6(2) . . ? C5 C4 C3 119.2(3) . . ? C4 C5 C6 120.7(3) . . ? C5 C6 C1 121.0(2) . . ? C12 C7 C8 118.0(2) . . ? C12 C7 P1 117.41(18) . . ? C8 C7 P1 124.55(16) . . ? C9 C8 C7 120.6(2) . . ? C10 C9 C8 120.4(2) . . ? C11 C10 C9 119.9(2) . . ? C10 C11 C12 119.9(2) . . ? C11 C12 C7 121.3(2) . . ? C14 C13 P1 111.13(14) . . ? N1 C14 C15 125.70(19) . . ? N1 C14 C13 118.98(19) . . ? C15 C14 C13 115.31(19) . . ? C17 C16 C21 121.46(18) . . ? C17 C16 N1 118.18(18) . . ? C21 C16 N1 120.19(18) . . ? C18 C17 C16 118.0(2) . . ? C18 C17 C25 120.5(2) . . ? C16 C17 C25 121.52(19) . . ? C19 C18 C17 121.5(2) . . ? C20 C19 C18 119.6(2) . . ? C19 C20 C21 122.1(2) . . ? C20 C21 C16 117.4(2) . . ? C20 C21 C22 119.7(2) . . ? C16 C21 C22 122.97(18) . . ? C21 C22 C24 112.4(2) . . ? C21 C22 C23 110.9(2) . . ? C24 C22 C23 109.9(2) . . ? C27 C25 C26 110.6(3) . . ? C27 C25 C17 112.0(2) . . ? C26 C25 C17 111.9(2) . . ? C33 C28 C29 117.6(3) . . ? C33 C28 P2 118.3(2) . . ? C29 C28 P2 124.08(19) . . ? C30 C29 C28 121.3(3) . . ? C31 C30 C29 120.1(3) . . ? C30 C31 C32 119.8(3) . . ? C31 C32 C33 119.8(3) . . ? C28 C33 C32 121.3(3) . . ? C35 C34 C39 117.8(2) . . ? C35 C34 P2 126.27(18) . . ? C39 C34 P2 115.90(18) . . ? C34 C35 C36 121.0(2) . . ? C37 C36 C35 120.1(3) . . ? C38 C37 C36 119.7(3) . . ? C37 C38 C39 120.6(3) . . ? C38 C39 C34 120.7(2) . . ? C41 C40 P2 112.91(16) . . ? N2 C41 C42 125.5(2) . . ? N2 C41 C40 118.0(2) . . ? C42 C41 C40 116.5(2) . . ? C44 C43 C48 121.4(2) . . ? C44 C43 N2 119.9(2) . . ? C48 C43 N2 118.4(2) . . ? C45 C44 C43 118.1(2) . . ? C45 C44 C52 119.6(2) . . ? C43 C44 C52 122.2(2) . . ? C46 C45 C44 121.4(2) . . ? C47 C46 C45 119.8(2) . . ? C46 C47 C48 121.6(2) . . ? C47 C48 C43 117.8(2) . . ? C47 C48 C49 120.8(2) . . ? C43 C48 C49 121.4(2) . . ? C51 C49 C48 113.8(2) . . ? C51 C49 C50 109.8(2) . . ? C48 C49 C50 112.2(2) . . ? C44 C52 C54 112.5(2) . . ? C44 C52 C53 111.6(2) . . ? C54 C52 C53 110.4(3) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.265 _refine_diff_density_min -0.208 _refine_diff_density_rms 0.035 #===end data_[Li(THF)][(C6H3i-Pr2)NC(Me)CHPPh2(NC6H3i-Pr2)] _database_code_CSD 211492 _audit_creation_method SHELXL-97 _chemical_formula_sum 'C43 H55 Li N2 O P' _chemical_formula_weight 653.80 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' Li Li -0.0003 0.0001 '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' O O 0.0106 0.0060 '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 10.687(7) _cell_length_b 19.406(12) _cell_length_c 19.757(12) _cell_angle_alpha 90.00 _cell_angle_beta 98.359(13) _cell_angle_gamma 90.00 _cell_volume 4054(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 50.0 _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.23 _exptl_crystal_density_diffrn 1.071 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1412 _exptl_absorpt_coefficient_mu 0.100 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.310565 _exptl_absorpt_correction_T_max 0.488950 _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 17063 _diffrn_reflns_av_R_equivalents 0.0415 _diffrn_reflns_av_sigmaI/netI 0.0850 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 23.33 _reflns_number_total 5785 _reflns_number_gt 2723 _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^)+(0.0471P)^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 5785 _refine_ls_number_parameters 433 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1125 _refine_ls_R_factor_gt 0.0498 _refine_ls_wR_factor_ref 0.1176 _refine_ls_wR_factor_gt 0.1085 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _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 Li1 Li 1.0072(5) 0.7874(3) 0.8071(3) 0.0683(15) Uani 1 1 d . . . P1 P 0.95615(8) 0.92533(4) 0.86533(4) 0.0550(3) Uani 1 1 d . . . N1 N 0.9562(2) 0.88240(11) 0.79640(12) 0.0497(6) Uani 1 1 d . . . N2 N 1.0522(2) 0.76863(13) 0.90268(12) 0.0496(6) Uani 1 1 d . . . O1 O 0.9998(3) 0.72219(13) 0.73532(13) 0.1097(9) Uani 1 1 d . . . C1 C 0.9567(3) 0.90948(14) 0.72944(16) 0.0513(8) Uani 1 1 d . . . C2 C 0.8433(3) 0.91370(15) 0.68268(17) 0.0597(9) Uani 1 1 d . . . C3 C 0.8493(4) 0.93470(19) 0.6162(2) 0.0933(12) Uani 1 1 d . . . H3A H 0.7748 0.9383 0.5856 0.112 Uiso 1 1 calc R . . C4 C 0.9612(5) 0.9503(2) 0.5943(2) 0.1104(15) Uani 1 1 d . . . H4A H 0.9628 0.9639 0.5492 0.133 Uiso 1 1 calc R . . C5 C 1.0708(4) 0.94576(19) 0.6391(2) 0.0926(12) Uani 1 1 d . . . H5A H 1.1470 0.9565 0.6242 0.111 Uiso 1 1 calc R . . C6 C 1.0711(3) 0.92545(16) 0.70657(17) 0.0616(9) Uani 1 1 d . . . C7 C 1.2740(3) 0.9863(2) 0.7567(2) 0.1145(14) Uani 1 1 d . . . H7A H 1.2238 1.0234 0.7704 0.172 Uiso 1 1 calc R . . H7B H 1.2969 0.9961 0.7125 0.172 Uiso 1 1 calc R . . H7C H 1.3491 0.9813 0.7894 0.172 Uiso 1 1 calc R . . C8 C 1.2760(4) 0.8587(2) 0.7332(2) 0.1286(16) Uani 1 1 d . . . H8A H 1.2273 0.8172 0.7330 0.193 Uiso 1 1 calc R . . H8B H 1.3517 0.8544 0.7657 0.193 Uiso 1 1 calc R . . H8C H 1.2982 0.8665 0.6885 0.193 Uiso 1 1 calc R . . C9 C 1.1979(3) 0.9196(2) 0.75320(18) 0.0824(11) Uani 1 1 d . . . H9A H 1.1792 0.9103 0.7995 0.099 Uiso 1 1 calc R . . C10 C 0.7175(3) 0.89591(19) 0.70480(18) 0.0795(11) Uani 1 1 d . . . H10A H 0.7329 0.8908 0.7547 0.095 Uiso 1 1 calc R . . C11 C 0.6185(4) 0.9514(3) 0.6893(4) 0.229(4) Uani 1 1 d . . . H11A H 0.5419 0.9371 0.7052 0.343 Uiso 1 1 calc R . . H11B H 0.6023 0.9592 0.6408 0.343 Uiso 1 1 calc R . . H11C H 0.6484 0.9933 0.7120 0.343 Uiso 1 1 calc R . . C12 C 0.6651(5) 0.8294(3) 0.6769(3) 0.211(3) Uani 1 1 d . . . H12A H 0.7276 0.7940 0.6871 0.316 Uiso 1 1 calc R . . H12B H 0.6423 0.8332 0.6282 0.316 Uiso 1 1 calc R . . H12C H 0.5916 0.8180 0.6973 0.316 Uiso 1 1 calc R . . C13 C 1.0044(3) 1.01444(15) 0.85926(17) 0.0576(9) Uani 1 1 d . . . C14 C 0.9434(3) 1.05723(18) 0.80855(17) 0.0713(10) Uani 1 1 d . . . H14A H 0.8758 1.0400 0.7783 0.086 Uiso 1 1 calc R . . C15 C 0.9808(4) 1.1249(2) 0.8019(2) 0.0916(13) Uani 1 1 d . . . H15A H 0.9384 1.1526 0.7675 0.110 Uiso 1 1 calc R . . C16 C 1.0801(5) 1.1508(2) 0.8459(3) 0.0990(14) Uani 1 1 d . . . H16A H 1.1054 1.1962 0.8414 0.119 Uiso 1 1 calc R . . C17 C 1.1427(4) 1.1101(2) 0.8967(2) 0.0977(13) Uani 1 1 d . . . H17A H 1.2093 1.1282 0.9270 0.117 Uiso 1 1 calc R . . C18 C 1.1064(4) 1.04128(19) 0.90285(18) 0.0787(10) Uani 1 1 d . . . H18A H 1.1509 1.0134 0.9364 0.094 Uiso 1 1 calc R . . C19 C 0.7961(3) 0.93295(19) 0.88738(15) 0.0619(9) Uani 1 1 d . . . C20 C 0.7479(4) 0.9913(2) 0.91356(17) 0.0838(11) Uani 1 1 d . . . H20A H 0.7958 1.0315 0.9180 0.101 Uiso 1 1 calc R . . C21 C 0.6274(5) 0.9909(3) 0.9336(2) 0.1137(16) Uani 1 1 d . . . H21A H 0.5959 1.0304 0.9517 0.136 Uiso 1 1 calc R . . C22 C 0.5568(5) 0.9321(4) 0.9263(3) 0.1283(19) Uani 1 1 d . . . H22A H 0.4761 0.9320 0.9386 0.154 Uiso 1 1 calc R . . C23 C 0.6032(5) 0.8738(3) 0.9011(2) 0.1222(16) Uani 1 1 d . . . H23A H 0.5547 0.8338 0.8968 0.147 Uiso 1 1 calc R . . C24 C 0.7222(4) 0.8740(2) 0.88215(19) 0.0943(13) Uani 1 1 d . . . H24A H 0.7536 0.8337 0.8655 0.113 Uiso 1 1 calc R . . C25 C 1.0778(3) 0.69848(15) 0.92149(14) 0.0498(8) Uani 1 1 d . . . C26 C 0.9791(3) 0.65554(17) 0.93609(15) 0.0594(9) Uani 1 1 d . . . C27 C 1.0002(3) 0.58513(18) 0.94424(17) 0.0735(10) Uani 1 1 d . . . H27A H 0.9350 0.5566 0.9537 0.088 Uiso 1 1 calc R . . C28 C 1.1173(4) 0.55694(17) 0.93839(16) 0.0727(10) Uani 1 1 d . . . H28A H 1.1302 0.5097 0.9430 0.087 Uiso 1 1 calc R . . C29 C 1.2127(3) 0.59869(18) 0.92588(16) 0.0641(9) Uani 1 1 d . . . H29A H 1.2915 0.5795 0.9229 0.077 Uiso 1 1 calc R . . C30 C 1.1969(3) 0.66909(16) 0.91733(14) 0.0532(8) Uani 1 1 d . . . C31 C 1.3092(3) 0.71327(16) 0.90447(17) 0.0673(9) Uani 1 1 d . . . H31A H 1.2814 0.7614 0.9006 0.081 Uiso 1 1 calc R . . C32 C 1.4165(3) 0.7078(2) 0.9641(2) 0.1113(14) Uani 1 1 d . . . H32A H 1.3867 0.7220 1.0055 0.167 Uiso 1 1 calc R . . H32B H 1.4851 0.7371 0.9557 0.167 Uiso 1 1 calc R . . H32C H 1.4453 0.6610 0.9687 0.167 Uiso 1 1 calc R . . C33 C 1.3573(3) 0.6934(2) 0.83827(19) 0.1106(14) Uani 1 1 d . . . H33A H 1.2901 0.6981 0.8006 0.166 Uiso 1 1 calc R . . H33B H 1.3861 0.6465 0.8412 0.166 Uiso 1 1 calc R . . H33C H 1.4261 0.7232 0.8312 0.166 Uiso 1 1 calc R . . C34 C 0.8491(3) 0.68537(18) 0.9422(2) 0.0814(11) Uani 1 1 d . . . H34A H 0.8575 0.7357 0.9423 0.098 Uiso 1 1 calc R . . C35 C 0.8034(4) 0.6653(3) 1.0091(2) 0.163(2) Uani 1 1 d . . . H35A H 0.7226 0.6861 1.0112 0.244 Uiso 1 1 calc R . . H35B H 0.8632 0.6810 1.0470 0.244 Uiso 1 1 calc R . . H35C H 0.7957 0.6161 1.0113 0.244 Uiso 1 1 calc R . . C36 C 0.7540(4) 0.6666(3) 0.8813(3) 0.157(2) Uani 1 1 d . . . H36A H 0.7842 0.6814 0.8402 0.235 Uiso 1 1 calc R . . H36B H 0.6750 0.6890 0.8848 0.235 Uiso 1 1 calc R . . H36C H 0.7420 0.6176 0.8800 0.235 Uiso 1 1 calc R . . C37 C 1.0429(3) 0.88735(16) 0.93608(15) 0.0633(9) Uani 1 1 d . . . H37A H 1.0757 0.9177 0.9706 0.076 Uiso 1 1 calc R . . C38 C 1.0714(3) 0.81782(17) 0.94923(16) 0.0532(8) Uani 1 1 d . . . C39 C 1.1248(3) 0.80007(16) 1.02322(15) 0.0813(11) Uani 1 1 d . . . H39A H 1.1413 0.7515 1.0269 0.122 Uiso 1 1 calc R . . H39B H 1.0646 0.8126 1.0527 0.122 Uiso 1 1 calc R . . H39C H 1.2021 0.8250 1.0364 0.122 Uiso 1 1 calc R . . C40 C 0.9886(5) 0.7347(3) 0.6633(2) 0.153(2) Uani 1 1 d . . . H40A H 0.9103 0.7590 0.6478 0.183 Uiso 1 1 calc R . . H40B H 1.0584 0.7632 0.6535 0.183 Uiso 1 1 calc R . . C41 C 0.9896(7) 0.6739(3) 0.6300(3) 0.214(3) Uani 1 1 d . . . H41A H 1.0620 0.6710 0.6056 0.256 Uiso 1 1 calc R . . H41B H 0.9129 0.6680 0.5977 0.256 Uiso 1 1 calc R . . C42 C 0.9978(9) 0.6225(3) 0.6841(4) 0.317(6) Uani 1 1 d . . . H42A H 0.9251 0.5921 0.6754 0.380 Uiso 1 1 calc R . . H42B H 1.0730 0.5948 0.6831 0.380 Uiso 1 1 calc R . . C43 C 1.0018(5) 0.6491(2) 0.7444(3) 0.143(2) Uani 1 1 d . . . H43A H 1.0054 0.6253 0.7855 0.172 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 Li1 0.093(4) 0.057(3) 0.057(4) 0.002(3) 0.015(3) 0.005(3) P1 0.0719(6) 0.0468(5) 0.0470(5) 0.0020(5) 0.0107(4) 0.0069(5) N1 0.0660(16) 0.0463(15) 0.0375(16) 0.0019(13) 0.0096(12) 0.0028(12) N2 0.0619(16) 0.0418(16) 0.0448(16) 0.0022(15) 0.0063(13) 0.0038(13) O1 0.201(3) 0.064(2) 0.065(2) -0.0138(15) 0.0205(18) 0.0083(17) C1 0.064(2) 0.042(2) 0.048(2) -0.0013(17) 0.0077(19) 0.0019(16) C2 0.079(3) 0.055(2) 0.044(2) 0.0041(18) 0.0032(19) 0.0003(19) C3 0.108(3) 0.106(3) 0.060(3) 0.014(2) -0.006(2) -0.004(3) C4 0.147(4) 0.137(4) 0.049(3) 0.025(3) 0.020(3) -0.019(3) C5 0.105(3) 0.108(3) 0.069(3) 0.014(3) 0.029(3) -0.016(3) C6 0.075(3) 0.064(2) 0.048(2) 0.0033(19) 0.0151(19) -0.0047(19) C7 0.087(3) 0.114(4) 0.142(4) -0.016(3) 0.013(3) -0.016(3) C8 0.092(3) 0.105(3) 0.189(5) 0.003(3) 0.024(3) 0.015(3) C9 0.070(2) 0.095(3) 0.086(3) 0.009(2) 0.023(2) -0.007(2) C10 0.070(2) 0.093(3) 0.072(3) 0.001(2) 0.001(2) -0.003(2) C11 0.099(4) 0.159(5) 0.437(11) 0.092(6) 0.067(5) 0.045(4) C12 0.165(5) 0.171(5) 0.317(8) -0.126(6) 0.105(5) -0.096(4) C13 0.080(2) 0.049(2) 0.046(2) -0.0012(19) 0.0156(18) 0.0051(19) C14 0.099(3) 0.056(3) 0.061(3) 0.002(2) 0.017(2) 0.004(2) C15 0.140(4) 0.058(3) 0.083(3) 0.015(2) 0.036(3) 0.011(3) C16 0.145(4) 0.061(3) 0.102(4) -0.005(3) 0.056(3) -0.021(3) C17 0.122(4) 0.082(3) 0.092(4) -0.015(3) 0.024(3) -0.030(3) C18 0.106(3) 0.065(3) 0.066(3) 0.002(2) 0.016(2) -0.004(2) C19 0.083(2) 0.057(2) 0.048(2) 0.0060(19) 0.0172(18) 0.012(2) C20 0.098(3) 0.088(3) 0.069(3) -0.005(2) 0.024(2) 0.019(2) C21 0.126(4) 0.137(5) 0.087(3) -0.001(3) 0.046(3) 0.048(4) C22 0.106(4) 0.181(6) 0.110(4) 0.020(4) 0.057(3) 0.010(5) C23 0.128(4) 0.123(4) 0.129(4) 0.009(3) 0.062(3) -0.020(3) C24 0.101(3) 0.083(3) 0.110(3) 0.021(3) 0.056(3) 0.006(3) C25 0.058(2) 0.047(2) 0.044(2) 0.0028(16) 0.0075(16) 0.0021(18) C26 0.056(2) 0.058(2) 0.065(2) 0.0111(19) 0.0104(17) 0.0011(19) C27 0.075(3) 0.062(3) 0.086(3) 0.015(2) 0.020(2) -0.012(2) C28 0.087(3) 0.049(2) 0.082(3) 0.0100(19) 0.011(2) 0.005(2) C29 0.063(2) 0.060(3) 0.070(2) 0.0035(19) 0.0116(18) 0.008(2) C30 0.060(2) 0.051(2) 0.049(2) 0.0039(17) 0.0100(16) 0.0022(19) C31 0.058(2) 0.064(2) 0.084(3) 0.008(2) 0.021(2) 0.0054(19) C32 0.078(3) 0.138(4) 0.115(3) 0.003(3) 0.006(3) -0.024(3) C33 0.111(3) 0.131(4) 0.100(3) -0.001(3) 0.049(3) -0.013(3) C34 0.057(2) 0.076(3) 0.115(3) 0.028(2) 0.023(2) 0.002(2) C35 0.118(4) 0.228(6) 0.161(5) 0.061(4) 0.082(4) 0.052(4) C36 0.078(3) 0.219(6) 0.164(5) -0.022(4) -0.015(3) 0.028(3) C37 0.089(2) 0.053(2) 0.043(2) -0.0043(17) -0.0074(17) 0.0043(18) C38 0.058(2) 0.058(2) 0.044(2) 0.008(2) 0.0093(16) 0.0075(17) C39 0.111(3) 0.076(3) 0.053(2) 0.002(2) -0.006(2) 0.022(2) C40 0.291(7) 0.100(4) 0.064(3) -0.014(3) 0.015(4) -0.006(4) C41 0.375(9) 0.142(5) 0.099(4) -0.043(5) -0.047(5) 0.101(6) C42 0.686(18) 0.100(5) 0.113(5) -0.011(5) -0.117(8) 0.105(7) C43 0.282(6) 0.059(3) 0.089(4) -0.008(3) 0.027(4) -0.009(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 Li1 O1 1.894(6) . ? Li1 N2 1.914(6) . ? Li1 N1 1.925(6) . ? Li1 P1 2.995(5) . ? P1 N1 1.597(2) . ? P1 C37 1.727(3) . ? P1 C13 1.813(3) . ? P1 C19 1.831(3) . ? N1 C1 1.424(3) . ? N2 C38 1.321(3) . ? N2 C25 1.427(3) . ? O1 C40 1.431(4) . ? O1 C43 1.430(4) . ? C1 C6 1.399(4) . ? C1 C2 1.416(4) . ? C2 C3 1.385(4) . ? C2 C10 1.513(4) . ? C3 C4 1.364(5) . ? C4 C5 1.365(5) . ? C5 C6 1.389(4) . ? C6 C9 1.528(4) . ? C7 C9 1.525(4) . ? C8 C9 1.530(4) . ? C10 C12 1.480(5) . ? C10 C11 1.509(5) . ? C13 C18 1.389(4) . ? C13 C14 1.389(4) . ? C14 C15 1.384(5) . ? C15 C16 1.367(5) . ? C16 C17 1.373(5) . ? C17 C18 1.401(5) . ? C19 C20 1.376(4) . ? C19 C24 1.386(4) . ? C20 C21 1.401(5) . ? C21 C22 1.364(6) . ? C22 C23 1.359(6) . ? C23 C24 1.377(5) . ? C25 C30 1.408(4) . ? C25 C26 1.407(4) . ? C26 C27 1.391(4) . ? C26 C34 1.525(4) . ? C27 C28 1.386(4) . ? C28 C29 1.353(4) . ? C29 C30 1.384(4) . ? C30 C31 1.526(4) . ? C31 C33 1.523(4) . ? C31 C32 1.523(4) . ? C34 C36 1.502(5) . ? C34 C35 1.525(5) . ? C37 C38 1.399(4) . ? C38 C39 1.529(4) . ? C40 C41 1.351(5) . ? C41 C42 1.457(7) . ? C42 C43 1.292(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Li1 N2 126.1(3) . . ? O1 Li1 N1 125.2(3) . . ? N2 Li1 N1 108.5(3) . . ? O1 Li1 P1 153.5(3) . . ? N2 Li1 P1 79.93(18) . . ? N1 Li1 P1 28.59(11) . . ? N1 P1 C37 113.64(14) . . ? N1 P1 C13 113.94(13) . . ? C37 P1 C13 109.64(17) . . ? N1 P1 C19 111.19(14) . . ? C37 P1 C19 104.61(15) . . ? C13 P1 C19 102.91(16) . . ? N1 P1 Li1 35.24(13) . . ? C37 P1 Li1 79.80(15) . . ? C13 P1 Li1 139.24(14) . . ? C19 P1 Li1 113.08(16) . . ? C1 N1 P1 126.89(19) . . ? C1 N1 Li1 114.6(2) . . ? P1 N1 Li1 116.2(2) . . ? C38 N2 C25 120.2(2) . . ? C38 N2 Li1 122.7(3) . . ? C25 N2 Li1 116.7(2) . . ? C40 O1 C43 106.9(3) . . ? C40 O1 Li1 128.3(3) . . ? C43 O1 Li1 124.8(3) . . ? C6 C1 C2 118.8(3) . . ? C6 C1 N1 120.2(3) . . ? C2 C1 N1 120.6(3) . . ? C3 C2 C1 118.8(3) . . ? C3 C2 C10 120.5(3) . . ? C1 C2 C10 120.7(3) . . ? C4 C3 C2 122.1(4) . . ? C5 C4 C3 119.2(4) . . ? C4 C5 C6 121.6(4) . . ? C5 C6 C1 119.5(3) . . ? C5 C6 C9 118.5(3) . . ? C1 C6 C9 121.9(3) . . ? C6 C9 C7 112.6(3) . . ? C6 C9 C8 111.8(3) . . ? C7 C9 C8 111.0(3) . . ? C12 C10 C2 113.3(3) . . ? C12 C10 C11 109.3(4) . . ? C2 C10 C11 113.8(3) . . ? C18 C13 C14 117.8(3) . . ? C18 C13 P1 121.5(3) . . ? C14 C13 P1 120.6(3) . . ? C15 C14 C13 121.6(4) . . ? C16 C15 C14 119.8(4) . . ? C15 C16 C17 120.3(4) . . ? C16 C17 C18 120.1(4) . . ? C13 C18 C17 120.4(4) . . ? C20 C19 C24 117.8(3) . . ? C20 C19 P1 124.7(3) . . ? C24 C19 P1 117.2(3) . . ? C19 C20 C21 120.7(4) . . ? C22 C21 C20 119.5(4) . . ? C23 C22 C21 120.7(5) . . ? C22 C23 C24 119.8(5) . . ? C23 C24 C19 121.4(4) . . ? C30 C25 C26 118.9(3) . . ? C30 C25 N2 120.8(3) . . ? C26 C25 N2 119.8(3) . . ? C27 C26 C25 119.5(3) . . ? C27 C26 C34 119.9(3) . . ? C25 C26 C34 120.7(3) . . ? C28 C27 C26 120.8(3) . . ? C29 C28 C27 119.5(3) . . ? C28 C29 C30 122.1(3) . . ? C29 C30 C25 119.2(3) . . ? C29 C30 C31 119.3(3) . . ? C25 C30 C31 121.5(3) . . ? C33 C31 C32 109.6(3) . . ? C33 C31 C30 111.9(3) . . ? C32 C31 C30 110.7(3) . . ? C36 C34 C35 111.6(3) . . ? C36 C34 C26 111.3(3) . . ? C35 C34 C26 112.4(3) . . ? C38 C37 P1 129.7(2) . . ? N2 C38 C37 124.1(3) . . ? N2 C38 C39 120.1(3) . . ? C37 C38 C39 115.8(3) . . ? C41 C40 O1 109.3(4) . . ? C40 C41 C42 104.1(5) . . ? C43 C42 C41 113.2(5) . . ? C42 C43 O1 106.4(5) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 23.33 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.225 _refine_diff_density_min -0.232 _refine_diff_density_rms 0.033 #===end data_[Ni((C6H3i-Pr2)NC(Me)CHPPh2(NC6H3i-Pr2))(?-Br)2Li(THF)2] _database_code_CSD 211493 _audit_creation_method SHELXL-97 _chemical_formula_sum 'C47 H64 Br2 Li N2 Ni O2 P' _chemical_formula_weight 945.44 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.284(6) _cell_length_b 13.404(7) _cell_length_c 18.234(10) _cell_angle_alpha 81.631(10) _cell_angle_beta 74.457(12) _cell_angle_gamma 67.997(9) _cell_volume 2460(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 50.0 _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.18 _exptl_crystal_density_diffrn 1.276 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 984 _exptl_absorpt_coefficient_mu 2.086 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.111712 _exptl_absorpt_correction_T_max 0.256594 _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 10205 _diffrn_reflns_av_R_equivalents 0.0782 _diffrn_reflns_av_sigmaI/netI 0.1749 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 23.27 _reflns_number_total 6993 _reflns_number_gt 3057 _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^)+(0.0972P)^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 6993 _refine_ls_number_parameters 501 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1780 _refine_ls_R_factor_gt 0.0671 _refine_ls_wR_factor_ref 0.1909 _refine_ls_wR_factor_gt 0.1485 _refine_ls_goodness_of_fit_ref 0.906 _refine_ls_restrained_S_all 0.906 _refine_ls_shift/su_max 0.185 _refine_ls_shift/su_mean 0.006 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 0.47790(12) 0.32260(9) 0.25210(6) 0.0462(4) Uani 1 1 d . . . Br1 Br 0.59965(11) 0.43335(8) 0.26807(6) 0.0668(4) Uani 1 1 d . . . Br2 Br 0.46210(12) 0.38840(10) 0.12165(6) 0.0759(4) Uani 1 1 d . . . P1 P 0.5740(3) 0.09693(19) 0.33561(13) 0.0504(7) Uani 1 1 d . . . N1 N 0.5710(7) 0.1628(5) 0.2534(3) 0.0389(18) Uani 1 1 d . . . N2 N 0.3362(7) 0.3369(6) 0.3465(4) 0.050(2) Uani 1 1 d . . . O1 O 0.3764(9) 0.6692(7) 0.1498(5) 0.105(3) Uani 1 1 d . . . O2 O 0.6726(10) 0.5851(7) 0.0934(4) 0.108(3) Uani 1 1 d . . . Li1 Li 0.532(2) 0.5345(14) 0.1480(10) 0.083(6) Uani 1 1 d . . . C1 C 0.7175(11) 0.0812(8) 0.3707(5) 0.057(3) Uani 1 1 d . . . C2 C 0.8143(14) -0.0158(10) 0.3854(7) 0.094(4) Uani 1 1 d . . . H2A H 0.8067 -0.0802 0.3782 0.112 Uiso 1 1 calc R . . C3 C 0.9193(17) -0.0190(13) 0.4100(9) 0.137(6) Uani 1 1 d . . . H3A H 0.9811 -0.0853 0.4198 0.164 Uiso 1 1 calc R . . C4 C 0.9361(16) 0.0742(16) 0.4205(8) 0.119(5) Uani 1 1 d . . . H4A H 1.0109 0.0715 0.4343 0.143 Uiso 1 1 calc R . . C5 C 0.8368(17) 0.1742(12) 0.4099(7) 0.096(4) Uani 1 1 d . . . H5A H 0.8431 0.2380 0.4196 0.115 Uiso 1 1 calc R . . C6 C 0.7320(13) 0.1762(9) 0.3854(6) 0.077(4) Uani 1 1 d . . . H6A H 0.6677 0.2423 0.3781 0.092 Uiso 1 1 calc R . . C7 C 0.5889(10) -0.0425(7) 0.3319(5) 0.055(3) Uani 1 1 d . . . C8 C 0.4965(12) -0.0831(9) 0.3812(6) 0.090(4) Uani 1 1 d . . . H8A H 0.4260 -0.0387 0.4155 0.108 Uiso 1 1 calc R . . C9 C 0.5117(19) -0.1907(11) 0.3784(9) 0.121(6) Uani 1 1 d . . . H9A H 0.4488 -0.2169 0.4099 0.146 Uiso 1 1 calc R . . C10 C 0.6172(17) -0.2586(10) 0.3303(9) 0.106(5) Uani 1 1 d . . . H10A H 0.6283 -0.3310 0.3308 0.128 Uiso 1 1 calc R . . C11 C 0.7055(12) -0.2188(8) 0.2817(7) 0.078(3) Uani 1 1 d . . . H11A H 0.7747 -0.2638 0.2471 0.093 Uiso 1 1 calc R . . C12 C 0.6946(10) -0.1140(8) 0.2827(6) 0.062(3) Uani 1 1 d . . . H12A H 0.7584 -0.0897 0.2502 0.075 Uiso 1 1 calc R . . C13 C 0.5717(10) 0.0632(7) 0.1502(5) 0.052(3) Uani 1 1 d . . . C14 C 0.6402(12) 0.0060(8) 0.0847(6) 0.073(3) Uani 1 1 d . . . H14A H 0.5991 -0.0279 0.0640 0.088 Uiso 1 1 calc R . . C15 C 0.7689(14) -0.0017(10) 0.0495(6) 0.092(4) Uani 1 1 d . . . H15A H 0.8127 -0.0391 0.0052 0.110 Uiso 1 1 calc R . . C16 C 0.8293(11) 0.0459(9) 0.0804(6) 0.077(4) Uani 1 1 d . . . H16A H 0.9151 0.0405 0.0563 0.092 Uiso 1 1 calc R . . C17 C 0.7686(10) 0.1030(7) 0.1470(5) 0.054(3) Uani 1 1 d . . . C18 C 0.6344(10) 0.1095(7) 0.1833(5) 0.046(3) Uani 1 1 d . . . C19 C 0.4279(10) 0.0728(8) 0.1830(5) 0.058(3) Uani 1 1 d . . . H19A H 0.3964 0.1083 0.2314 0.069 Uiso 1 1 calc R . . C20 C 0.3447(12) 0.1417(9) 0.1287(6) 0.089(4) Uani 1 1 d . . . H20A H 0.3547 0.2107 0.1194 0.134 Uiso 1 1 calc R . . H20B H 0.2540 0.1511 0.1508 0.134 Uiso 1 1 calc R . . H20C H 0.3725 0.1068 0.0814 0.134 Uiso 1 1 calc R . . C21 C 0.4046(12) -0.0351(9) 0.1969(7) 0.094(4) Uani 1 1 d . . . H21A H 0.4544 -0.0808 0.2319 0.141 Uiso 1 1 calc R . . H21B H 0.4319 -0.0695 0.1495 0.141 Uiso 1 1 calc R . . H21C H 0.3128 -0.0222 0.2179 0.141 Uiso 1 1 calc R . . C22 C 0.8399(10) 0.1592(8) 0.1758(5) 0.059(3) Uani 1 1 d . . . H22A H 0.7828 0.1940 0.2227 0.070 Uiso 1 1 calc R . . C23 C 0.8677(11) 0.2462(9) 0.1174(6) 0.088(4) Uani 1 1 d . . . H23A H 0.7867 0.2958 0.1064 0.132 Uiso 1 1 calc R . . H23B H 0.9258 0.2134 0.0715 0.132 Uiso 1 1 calc R . . H23C H 0.9080 0.2843 0.1377 0.132 Uiso 1 1 calc R . . C24 C 0.9685(12) 0.0804(10) 0.1941(7) 0.095(4) Uani 1 1 d . . . H24A H 0.9505 0.0264 0.2314 0.143 Uiso 1 1 calc R . . H24B H 1.0090 0.1188 0.2139 0.143 Uiso 1 1 calc R . . H24C H 1.0268 0.0467 0.1485 0.143 Uiso 1 1 calc R . . C25 C 0.2279(10) 0.4371(8) 0.3515(5) 0.049(3) Uani 1 1 d . . . C26 C 0.1355(11) 0.4536(9) 0.3097(6) 0.063(3) Uani 1 1 d . . . C27 C 0.0304(12) 0.5513(11) 0.3141(6) 0.079(3) Uani 1 1 d . . . H27A H -0.0318 0.5628 0.2862 0.094 Uiso 1 1 calc R . . C28 C 0.0160(12) 0.6324(10) 0.3595(7) 0.078(4) Uani 1 1 d . . . H28A H -0.0545 0.6972 0.3617 0.093 Uiso 1 1 calc R . . C29 C 0.1085(12) 0.6141(10) 0.4007(6) 0.066(3) Uani 1 1 d . . . H29A H 0.0987 0.6678 0.4313 0.079 Uiso 1 1 calc R . . C30 C 0.2164(11) 0.5186(8) 0.3987(5) 0.050(3) Uani 1 1 d . . . C31 C 0.3112(11) 0.5088(8) 0.4462(5) 0.065(3) Uani 1 1 d . . . H31A H 0.3834 0.4396 0.4364 0.078 Uiso 1 1 calc R . . C32 C 0.3703(11) 0.5977(8) 0.4259(6) 0.076(3) Uani 1 1 d . . . H32A H 0.4131 0.5968 0.3728 0.114 Uiso 1 1 calc R . . H32B H 0.4332 0.5858 0.4558 0.114 Uiso 1 1 calc R . . H32C H 0.3017 0.6664 0.4366 0.114 Uiso 1 1 calc R . . C33 C 0.2476(13) 0.5103(10) 0.5328(6) 0.097(4) Uani 1 1 d . . . H33A H 0.2123 0.4534 0.5473 0.146 Uiso 1 1 calc R . . H33B H 0.1782 0.5784 0.5442 0.146 Uiso 1 1 calc R . . H33C H 0.3129 0.4999 0.5606 0.146 Uiso 1 1 calc R . . C34 C 0.1427(11) 0.3668(10) 0.2617(6) 0.078(3) Uani 1 1 d . . . H34A H 0.2359 0.3233 0.2445 0.094 Uiso 1 1 calc R . . C35 C 0.0744(16) 0.2907(13) 0.3104(8) 0.152(7) Uani 1 1 d . . . H35A H 0.1106 0.2627 0.3543 0.228 Uiso 1 1 calc R . . H35B H 0.0881 0.2322 0.2806 0.228 Uiso 1 1 calc R . . H35C H -0.0181 0.3298 0.3265 0.228 Uiso 1 1 calc R . . C36 C 0.0888(13) 0.4114(12) 0.1898(8) 0.124(5) Uani 1 1 d . . . H36A H 0.1322 0.4587 0.1605 0.185 Uiso 1 1 calc R . . H36B H -0.0040 0.4505 0.2044 0.185 Uiso 1 1 calc R . . H36C H 0.1045 0.3528 0.1596 0.185 Uiso 1 1 calc R . . C37 C 0.3378(11) 0.2603(8) 0.4024(5) 0.061(3) Uani 1 1 d . . . C38 C 0.4358(11) 0.1606(8) 0.4042(5) 0.075(4) Uani 1 1 d . . . H38A H 0.4257 0.1208 0.4502 0.090 Uiso 1 1 calc R . . C39 C 0.2195(11) 0.2800(8) 0.4711(5) 0.089(4) Uani 1 1 d . . . H39A H 0.1568 0.3509 0.4656 0.134 Uiso 1 1 calc R . . H39B H 0.2485 0.2738 0.5171 0.134 Uiso 1 1 calc R . . H39C H 0.1792 0.2275 0.4737 0.134 Uiso 1 1 calc R . . C40 C 0.275(2) 0.6968(16) 0.2121(9) 0.171(8) Uani 1 1 d . . . H40A H 0.2914 0.7379 0.2453 0.206 Uiso 1 1 calc R . . H40B H 0.2631 0.6328 0.2405 0.206 Uiso 1 1 calc R . . C41 C 0.160(3) 0.761(3) 0.1840(16) 0.30(2) Uani 1 1 d . . . H41A H 0.0896 0.7327 0.2064 0.356 Uiso 1 1 calc R . . H41B H 0.1302 0.8345 0.1987 0.356 Uiso 1 1 calc R . . C42 C 0.186(3) 0.759(3) 0.1125(16) 0.237(13) Uani 1 1 d . . . H42A H 0.1522 0.8315 0.0907 0.285 Uiso 1 1 calc R . . H42B H 0.1435 0.7161 0.0982 0.285 Uiso 1 1 calc R . . C43 C 0.326(3) 0.7135(17) 0.0829(10) 0.215(12) Uani 1 1 d . . . H43A H 0.3478 0.6577 0.0480 0.258 Uiso 1 1 calc R . . H43B H 0.3606 0.7686 0.0567 0.258 Uiso 1 1 calc R . . C44B C 0.713(3) 0.638(3) 0.1360(17) 0.118(9) Uiso 0.50 1 d P . . C44A C 0.638(4) 0.703(3) 0.0697(19) 0.149(12) Uiso 0.50 1 d P . . C45B C 0.803(4) 0.697(3) 0.0911(19) 0.123(11) Uiso 0.50 1 d P . . C45A C 0.862(3) 0.627(3) 0.0783(17) 0.106(9) Uiso 0.50 1 d P . . C46A C 0.844(3) 0.632(3) 0.0155(16) 0.101(8) Uiso 0.50 1 d P . . C46B C 0.773(4) 0.710(3) 0.033(2) 0.131(11) Uiso 0.50 1 d P . . C47B C 0.744(4) 0.573(3) 0.0171(19) 0.121(12) Uiso 0.50 1 d P . . C47A C 0.793(4) 0.534(4) 0.043(3) 0.153(16) 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 Ni1 0.0470(8) 0.0361(7) 0.0438(6) 0.0028(5) 0.0063(6) -0.0148(7) Br1 0.0733(9) 0.0557(7) 0.0708(7) 0.0017(6) -0.0027(6) -0.0336(7) Br2 0.0919(10) 0.0798(9) 0.0587(6) 0.0182(6) -0.0171(6) -0.0415(8) P1 0.0616(19) 0.0341(15) 0.0456(13) 0.0041(12) -0.0019(13) -0.0156(15) N1 0.043(5) 0.024(4) 0.040(4) -0.004(3) -0.001(4) -0.007(4) N2 0.035(5) 0.042(5) 0.049(4) -0.004(4) 0.019(4) -0.008(5) O1 0.092(7) 0.092(7) 0.092(6) 0.017(6) 0.000(6) -0.012(6) O2 0.147(9) 0.094(7) 0.082(5) 0.007(5) 0.018(6) -0.078(7) Li1 0.109(17) 0.054(12) 0.086(12) 0.028(10) -0.021(12) -0.042(13) C1 0.084(9) 0.054(7) 0.045(5) 0.008(5) -0.023(6) -0.035(7) C2 0.132(12) 0.052(8) 0.126(10) 0.017(7) -0.097(10) -0.028(9) C3 0.174(17) 0.107(13) 0.182(15) 0.041(11) -0.146(14) -0.054(13) C4 0.135(15) 0.151(16) 0.117(11) 0.034(11) -0.079(11) -0.083(14) C5 0.144(14) 0.093(11) 0.090(9) 0.005(8) -0.049(9) -0.076(11) C6 0.121(11) 0.064(8) 0.078(7) 0.012(6) -0.040(8) -0.063(8) C7 0.065(8) 0.041(6) 0.056(6) 0.015(5) -0.012(6) -0.025(6) C8 0.088(10) 0.060(8) 0.099(9) 0.020(7) 0.002(7) -0.026(8) C9 0.197(19) 0.067(10) 0.137(12) 0.035(9) -0.040(12) -0.101(12) C10 0.153(16) 0.032(8) 0.146(13) 0.018(8) -0.068(12) -0.032(10) C11 0.087(10) 0.029(7) 0.111(9) -0.009(6) -0.032(8) -0.006(7) C12 0.059(8) 0.045(7) 0.072(7) -0.007(6) -0.001(6) -0.015(6) C13 0.072(8) 0.044(6) 0.043(5) -0.003(5) -0.003(5) -0.030(6) C14 0.090(10) 0.064(8) 0.070(7) -0.017(6) -0.010(7) -0.033(8) C15 0.108(11) 0.093(10) 0.073(7) -0.040(7) 0.027(8) -0.055(9) C16 0.068(8) 0.084(9) 0.068(7) -0.019(7) 0.022(6) -0.036(8) C17 0.056(7) 0.045(6) 0.047(5) -0.003(5) 0.013(5) -0.017(6) C18 0.058(7) 0.034(6) 0.041(5) 0.003(4) -0.004(5) -0.017(6) C19 0.051(7) 0.067(8) 0.063(6) -0.012(6) -0.022(6) -0.019(6) C20 0.089(10) 0.086(9) 0.092(8) -0.026(7) -0.025(8) -0.018(8) C21 0.093(10) 0.100(10) 0.107(9) -0.003(8) -0.022(8) -0.057(9) C22 0.050(7) 0.054(7) 0.056(6) -0.007(5) 0.010(5) -0.015(7) C23 0.068(8) 0.079(9) 0.096(8) -0.012(7) 0.020(7) -0.028(8) C24 0.079(10) 0.094(10) 0.101(9) -0.017(8) -0.008(8) -0.023(9) C25 0.035(7) 0.045(7) 0.050(6) 0.005(5) 0.013(5) -0.015(6) C26 0.042(7) 0.051(8) 0.074(7) -0.002(6) 0.004(6) -0.006(7) C27 0.059(9) 0.081(10) 0.076(8) 0.004(7) -0.010(7) -0.010(9) C28 0.050(8) 0.058(8) 0.080(8) -0.001(7) 0.010(7) 0.011(7) C29 0.060(8) 0.064(9) 0.058(6) -0.010(6) 0.011(6) -0.018(8) C30 0.050(7) 0.037(7) 0.058(6) -0.001(5) 0.001(6) -0.019(7) C31 0.068(8) 0.046(7) 0.068(6) -0.005(5) 0.005(6) -0.019(6) C32 0.077(9) 0.070(8) 0.083(7) -0.014(6) 0.002(6) -0.038(7) C33 0.136(12) 0.089(9) 0.073(7) 0.008(7) -0.022(8) -0.052(10) C34 0.049(8) 0.092(9) 0.090(8) -0.022(8) -0.002(7) -0.024(7) C35 0.175(17) 0.176(16) 0.142(12) -0.052(11) 0.031(11) -0.133(15) C36 0.094(11) 0.134(13) 0.135(12) -0.053(11) -0.037(10) -0.007(10) C37 0.078(9) 0.048(7) 0.045(5) -0.007(5) 0.024(5) -0.033(7) C38 0.088(9) 0.043(7) 0.052(6) 0.007(5) 0.024(6) -0.008(7) C39 0.094(9) 0.060(7) 0.068(7) 0.000(6) 0.046(7) -0.021(7) C40 0.166(19) 0.147(17) 0.094(11) 0.025(11) 0.027(13) 0.013(15) C41 0.14(2) 0.31(4) 0.23(3) 0.14(3) 0.05(2) 0.05(2) C42 0.15(2) 0.30(4) 0.21(3) 0.02(3) -0.06(2) 0.00(3) C43 0.24(3) 0.17(2) 0.089(12) 0.005(12) -0.015(16) 0.06(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 Ni1 N2 1.987(6) . ? Ni1 N1 2.001(6) . ? Ni1 Br2 2.4426(19) . ? Ni1 Br1 2.4586(18) . ? Br1 Li1 2.543(19) . ? Br2 Li1 2.515(18) . ? P1 N1 1.627(6) . ? P1 C38 1.730(10) . ? P1 C7 1.822(9) . ? P1 C1 1.826(11) . ? N1 C18 1.432(10) . ? N2 C37 1.336(11) . ? N2 C25 1.433(11) . ? O1 C40 1.359(16) . ? O1 C43 1.440(19) . ? O1 Li1 1.99(2) . ? O2 C44B 1.38(3) . ? O2 C47A 1.41(4) . ? O2 C47B 1.41(3) . ? O2 C44A 1.51(4) . ? O2 Li1 1.930(19) . ? C1 C2 1.395(14) . ? C1 C6 1.414(13) . ? C2 C3 1.360(16) . ? C3 C4 1.379(18) . ? C4 C5 1.415(19) . ? C5 C6 1.362(15) . ? C7 C12 1.403(12) . ? C7 C8 1.405(12) . ? C8 C9 1.394(15) . ? C9 C10 1.370(18) . ? C10 C11 1.360(16) . ? C11 C12 1.365(13) . ? C13 C18 1.384(12) . ? C13 C14 1.393(13) . ? C13 C19 1.534(13) . ? C14 C15 1.393(14) . ? C15 C16 1.351(14) . ? C16 C17 1.402(13) . ? C17 C18 1.456(12) . ? C17 C22 1.513(13) . ? C19 C20 1.516(13) . ? C19 C21 1.539(13) . ? C22 C23 1.525(12) . ? C22 C24 1.530(14) . ? C25 C26 1.385(14) . ? C25 C30 1.435(13) . ? C26 C27 1.394(15) . ? C26 C34 1.521(14) . ? C27 C28 1.396(15) . ? C28 C29 1.375(15) . ? C29 C30 1.394(14) . ? C30 C31 1.507(14) . ? C31 C32 1.528(12) . ? C31 C33 1.550(13) . ? C34 C36 1.542(16) . ? C34 C35 1.543(14) . ? C37 C38 1.382(14) . ? C37 C39 1.535(11) . ? C40 C41 1.44(3) . ? C41 C42 1.26(3) . ? C42 C43 1.44(3) . ? C44B C45B 1.51(4) . ? C44B C44A 1.62(4) . ? C44B C45A 1.70(4) . ? C44A C46B 1.53(4) . ? C44A C47B 1.92(5) . ? C44A C45B 1.97(5) . ? C45B C45A 0.94(4) . ? C45B C46B 1.16(4) . ? C45B C46A 1.60(4) . ? C45A C46A 1.21(3) . ? C45A C46B 1.51(5) . ? C45A C47A 1.95(5) . ? C46A C46B 1.08(4) . ? C46A C47A 1.60(5) . ? C46A C47B 1.60(4) . ? C47B C47A 0.82(5) . ? 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 100.9(3) . . ? N2 Ni1 Br2 129.5(2) . . ? N1 Ni1 Br2 108.72(19) . . ? N2 Ni1 Br1 105.6(2) . . ? N1 Ni1 Br1 117.1(2) . . ? Br2 Ni1 Br1 96.11(5) . . ? Ni1 Br1 Li1 83.8(4) . . ? Ni1 Br2 Li1 84.7(4) . . ? N1 P1 C38 111.0(5) . . ? N1 P1 C7 112.7(4) . . ? C38 P1 C7 109.7(5) . . ? N1 P1 C1 113.6(4) . . ? C38 P1 C1 107.5(5) . . ? C7 P1 C1 102.1(5) . . ? C18 N1 P1 121.7(5) . . ? C18 N1 Ni1 120.1(5) . . ? P1 N1 Ni1 118.2(3) . . ? C37 N2 C25 120.7(7) . . ? C37 N2 Ni1 124.1(7) . . ? C25 N2 Ni1 115.2(5) . . ? C40 O1 C43 108.2(13) . . ? C40 O1 Li1 122.5(11) . . ? C43 O1 Li1 121.8(12) . . ? C44B O2 C47A 100(2) . . ? C44B O2 C47B 114.4(19) . . ? C47A O2 C47B 34(2) . . ? C44B O2 C44A 68.1(17) . . ? C47A O2 C44A 105(2) . . ? C47B O2 C44A 82.5(19) . . ? C44B O2 Li1 115.6(14) . . ? C47A O2 Li1 131.4(19) . . ? C47B O2 Li1 130.0(16) . . ? C44A O2 Li1 118.1(17) . . ? O2 Li1 O1 101.1(8) . . ? O2 Li1 Br2 131.6(10) . . ? O1 Li1 Br2 105.4(9) . . ? O2 Li1 Br1 106.1(10) . . ? O1 Li1 Br1 123.1(9) . . ? Br2 Li1 Br1 92.2(5) . . ? C2 C1 C6 116.3(10) . . ? C2 C1 P1 126.4(8) . . ? C6 C1 P1 117.2(9) . . ? C3 C2 C1 122.0(12) . . ? C2 C3 C4 121.2(15) . . ? C3 C4 C5 118.5(13) . . ? C6 C5 C4 119.6(12) . . ? C5 C6 C1 122.2(12) . . ? C12 C7 C8 117.6(9) . . ? C12 C7 P1 121.9(7) . . ? C8 C7 P1 120.4(8) . . ? C9 C8 C7 119.4(12) . . ? C10 C9 C8 121.4(13) . . ? C11 C10 C9 119.2(11) . . ? C10 C11 C12 121.3(12) . . ? C11 C12 C7 121.1(10) . . ? C18 C13 C14 119.5(10) . . ? C18 C13 C19 122.3(8) . . ? C14 C13 C19 118.2(10) . . ? C13 C14 C15 121.5(10) . . ? C16 C15 C14 119.2(10) . . ? C15 C16 C17 123.0(10) . . ? C16 C17 C18 117.0(9) . . ? C16 C17 C22 119.9(9) . . ? C18 C17 C22 123.0(8) . . ? C13 C18 N1 121.6(8) . . ? C13 C18 C17 119.7(8) . . ? N1 C18 C17 118.7(8) . . ? C20 C19 C13 109.8(8) . . ? C20 C19 C21 106.7(9) . . ? C13 C19 C21 114.7(9) . . ? C17 C22 C23 110.3(9) . . ? C17 C22 C24 112.1(8) . . ? C23 C22 C24 109.7(9) . . ? C26 C25 N2 118.7(9) . . ? C26 C25 C30 121.0(11) . . ? N2 C25 C30 120.3(10) . . ? C25 C26 C27 118.8(11) . . ? C25 C26 C34 121.9(11) . . ? C27 C26 C34 119.2(12) . . ? C26 C27 C28 121.8(12) . . ? C29 C28 C27 118.4(12) . . ? C28 C29 C30 122.9(11) . . ? C29 C30 C25 117.1(10) . . ? C29 C30 C31 117.7(10) . . ? C25 C30 C31 125.2(10) . . ? C30 C31 C32 112.7(9) . . ? C30 C31 C33 112.7(9) . . ? C32 C31 C33 107.9(9) . . ? C26 C34 C36 113.8(11) . . ? C26 C34 C35 110.8(9) . . ? C36 C34 C35 110.8(11) . . ? N2 C37 C38 126.2(8) . . ? N2 C37 C39 118.9(9) . . ? C38 C37 C39 114.9(8) . . ? C37 C38 P1 131.1(7) . . ? O1 C40 C41 106.4(16) . . ? C42 C41 C40 110(3) . . ? C41 C42 C43 110(3) . . ? O1 C43 C42 103.9(16) . . ? O2 C44B C45B 116(2) . . ? O2 C44B C44A 59.7(18) . . ? C45B C44B C44A 78(2) . . ? O2 C44B C45A 99(2) . . ? C45B C44B C45A 33.5(16) . . ? C44A C44B C45A 92(2) . . ? O2 C44A C46B 102(3) . . ? O2 C44A C44B 52.2(17) . . ? C46B C44A C44B 81(2) . . ? O2 C44A C47B 46.4(15) . . ? C46B C44A C47B 72(2) . . ? C44B C44A C47B 82(2) . . ? O2 C44A C45B 88(2) . . ? C46B C44A C45B 36.0(16) . . ? C44B C44A C45B 48.5(17) . . ? C47B C44A C45B 85(2) . . ? C45A C45B C46B 91(4) . . ? C45A C45B C44B 84(3) . . ? C46B C45B C44B 99(3) . . ? C45A C45B C46A 48(3) . . ? C46B C45B C46A 43(2) . . ? C44B C45B C46A 95(2) . . ? C45A C45B C44A 105(4) . . ? C46B C45B C44A 51(2) . . ? C44B C45B C44A 53.7(18) . . ? C46A C45B C44A 74(2) . . ? C45B C45A C46A 96(4) . . ? C45B C45A C46B 50(3) . . ? C46A C45A C46B 45(2) . . ? C45B C45A C44B 62(3) . . ? C46A C45A C44B 103(3) . . ? C46B C45A C44B 79(2) . . ? C45B C45A C47A 116(4) . . ? C46A C45A C47A 55(2) . . ? C46B C45A C47A 81(2) . . ? C44B C45A C47A 71.2(19) . . ? C46B C46A C45A 82(3) . . ? C46B C46A C47A 115(3) . . ? C45A C46A C47A 87(3) . . ? C46B C46A C47B 99(3) . . ? C45A C46A C47B 110(3) . . ? C47A C46A C47B 29.6(19) . . ? C46B C46A C45B 46(2) . . ? C45A C46A C45B 36(2) . . ? C47A C46A C45B 104(2) . . ? C47B C46A C45B 111(2) . . ? C46A C46B C45B 91(4) . . ? C46A C46B C45A 52(2) . . ? C45B C46B C45A 39(2) . . ? C46A C46B C44A 111(3) . . ? C45B C46B C44A 93(3) . . ? C45A C46B C44A 104(3) . . ? C47A C47B O2 73(4) . . ? C47A C47B C46A 75(4) . . ? O2 C47B C46A 101(2) . . ? C47A C47B C44A 108(5) . . ? O2 C47B C44A 51.1(15) . . ? C46A C47B C44A 75(2) . . ? C47B C47A O2 73(5) . . ? C47B C47A C46A 75(5) . . ? O2 C47A C46A 101(3) . . ? C47B C47A C45A 105(5) . . ? O2 C47A C45A 87(2) . . ? C46A C47A C45A 38.0(15) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 23.28 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.203 _refine_diff_density_min -0.654 _refine_diff_density_rms 0.094 #===end data_PdBr((C6H3i-Pr2)NC(Me)CHPPh2(NC6H3i-Pr2))(PPh3) _database_code_CSD 211494 _audit_creation_method SHELXL-97 _chemical_formula_sum 'C64 H71 Cl N2 P2 Pd' _chemical_formula_weight 1072.02 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 '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 10.367(7) _cell_length_b 26.477(17) _cell_length_c 23.410(15) _cell_angle_alpha 90.00 _cell_angle_beta 96.274(13) _cell_angle_gamma 90.00 _cell_volume 6387(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 50.0 _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.21 _exptl_crystal_density_diffrn 1.115 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2248 _exptl_absorpt_coefficient_mu 0.418 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.086523 _exptl_absorpt_correction_T_max 0.191252 _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 27188 _diffrn_reflns_av_R_equivalents 0.0979 _diffrn_reflns_av_sigmaI/netI 0.1004 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 23.35 _reflns_number_total 9140 _reflns_number_gt 5585 _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^)+(0.0603P)^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 9140 _refine_ls_number_parameters 631 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0856 _refine_ls_R_factor_gt 0.0541 _refine_ls_wR_factor_ref 0.1475 _refine_ls_wR_factor_gt 0.1415 _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_restrained_S_all 1.098 _refine_ls_shift/su_max 0.114 _refine_ls_shift/su_mean 0.002 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 Pd1 Pd 1.05058(3) 0.744829(16) 0.261683(17) 0.03864(16) Uani 1 1 d . . . Cl1 Cl 1.24274(12) 0.74950(7) 0.32355(6) 0.0635(5) Uani 1 1 d . . . P1 P 0.99296(12) 0.77948(5) 0.15353(6) 0.0391(4) Uani 1 1 d . . . P2 P 0.93631(13) 0.73796(6) 0.33879(6) 0.0441(4) Uani 1 1 d . . . N1 N 1.1321(4) 0.76944(16) 0.18751(18) 0.0400(11) Uani 1 1 d . . . N2 N 0.9726(4) 0.65804(17) 0.1553(2) 0.0449(12) Uani 1 1 d . . . C1 C 0.9162(5) 0.8416(2) 0.1623(3) 0.0496(15) Uani 1 1 d . . . C2 C 0.8860(6) 0.8560(2) 0.2165(3) 0.0625(17) Uani 1 1 d . . . H2A H 0.9064 0.8348 0.2479 0.075 Uiso 1 1 calc R . . C3 C 0.8254(7) 0.9020(3) 0.2237(4) 0.084(2) Uani 1 1 d . . . H3A H 0.8070 0.9115 0.2602 0.100 Uiso 1 1 calc R . . C4 C 0.7928(8) 0.9332(3) 0.1791(4) 0.095(3) Uani 1 1 d . . . H4A H 0.7490 0.9632 0.1843 0.115 Uiso 1 1 calc R . . C5 C 0.8262(9) 0.9195(3) 0.1243(4) 0.106(3) Uani 1 1 d . . . H5A H 0.8077 0.9415 0.0936 0.127 Uiso 1 1 calc R . . C6 C 0.8859(7) 0.8740(2) 0.1158(3) 0.074(2) Uani 1 1 d . . . H6A H 0.9058 0.8651 0.0794 0.089 Uiso 1 1 calc R . . C7 C 0.9819(5) 0.7735(2) 0.0762(2) 0.0456(14) Uani 1 1 d . . . C8 C 0.8631(6) 0.7615(2) 0.0446(3) 0.0620(17) Uani 1 1 d . . . H8A H 0.7918 0.7536 0.0638 0.074 Uiso 1 1 calc R . . C9 C 1.0854(6) 0.7863(3) 0.0459(3) 0.0685(19) Uani 1 1 d . . . H9A H 1.1650 0.7947 0.0659 0.082 Uiso 1 1 calc R . . C10 C 1.0713(7) 0.7865(3) -0.0141(3) 0.091(3) Uani 1 1 d . . . H10A H 1.1410 0.7957 -0.0338 0.110 Uiso 1 1 calc R . . C11 C 0.9563(7) 0.7733(3) -0.0440(3) 0.086(2) Uani 1 1 d . . . H11A H 0.9484 0.7723 -0.0839 0.103 Uiso 1 1 calc R . . C12 C 0.8510(7) 0.7614(3) -0.0149(3) 0.076(2) Uani 1 1 d . . . H12A H 0.7718 0.7533 -0.0355 0.092 Uiso 1 1 calc R . . C13 C 1.2628(5) 0.7835(2) 0.1791(2) 0.0420(14) Uani 1 1 d . . . C14 C 1.3370(4) 0.7494(2) 0.1480(2) 0.0442(13) Uani 1 1 d . . . C15 C 1.4635(5) 0.7640(3) 0.1412(3) 0.0579(17) Uani 1 1 d . . . H15A H 1.5130 0.7428 0.1206 0.069 Uiso 1 1 calc R . . C16 C 1.5185(6) 0.8070(3) 0.1628(3) 0.0639(18) Uani 1 1 d . . . H16A H 1.6036 0.8149 0.1571 0.077 Uiso 1 1 calc R . . C17 C 1.4473(6) 0.8393(3) 0.1936(3) 0.0678(19) Uani 1 1 d . . . H17A H 1.4860 0.8688 0.2085 0.081 Uiso 1 1 calc R . . C18 C 1.3175(5) 0.8288(2) 0.2032(3) 0.0504(15) Uani 1 1 d . . . C19 C 1.2830(5) 0.6995(2) 0.1265(3) 0.0545(16) Uani 1 1 d . . . H19A H 1.1886 0.7034 0.1200 0.065 Uiso 1 1 calc R . . C20 C 1.3098(6) 0.6587(2) 0.1712(3) 0.076(2) Uani 1 1 d . . . H20A H 1.2785 0.6693 0.2064 0.114 Uiso 1 1 calc R . . H20B H 1.4016 0.6527 0.1777 0.114 Uiso 1 1 calc R . . H20C H 1.2664 0.6282 0.1578 0.114 Uiso 1 1 calc R . . C21 C 1.3286(8) 0.6824(3) 0.0684(3) 0.099(3) Uani 1 1 d . . . H21A H 1.3087 0.7083 0.0401 0.149 Uiso 1 1 calc R . . H21B H 1.2847 0.6518 0.0559 0.149 Uiso 1 1 calc R . . H21C H 1.4206 0.6766 0.0734 0.149 Uiso 1 1 calc R . . C22 C 1.2456(6) 0.8647(2) 0.2369(3) 0.0685(19) Uani 1 1 d . . . H22A H 1.1658 0.8478 0.2454 0.082 Uiso 1 1 calc R . . C23 C 1.3230(8) 0.8788(3) 0.2952(4) 0.110(3) Uani 1 1 d . . . H23A H 1.3441 0.8487 0.3170 0.165 Uiso 1 1 calc R . . H23B H 1.2714 0.9006 0.3163 0.165 Uiso 1 1 calc R . . H23C H 1.4015 0.8959 0.2883 0.165 Uiso 1 1 calc R . . C24 C 1.2042(8) 0.9134(3) 0.2004(4) 0.109(3) Uani 1 1 d . . . H24A H 1.1544 0.9035 0.1652 0.164 Uiso 1 1 calc R . . H24B H 1.2804 0.9312 0.1919 0.164 Uiso 1 1 calc R . . H24C H 1.1528 0.9349 0.2219 0.164 Uiso 1 1 calc R . . C25 C 0.8993(4) 0.73721(19) 0.1923(2) 0.0357(12) Uani 1 1 d . . . H25A H 0.8178 0.7525 0.2011 0.043 Uiso 1 1 calc R . . C26 C 0.8832(5) 0.6833(2) 0.1759(2) 0.0383(13) Uani 1 1 d . . . C27 C 0.7512(5) 0.6602(2) 0.1847(3) 0.0607(18) Uani 1 1 d . . . H27A H 0.7493 0.6255 0.1730 0.091 Uiso 1 1 calc R . . H27B H 0.6837 0.6785 0.1621 0.091 Uiso 1 1 calc R . . H27C H 0.7378 0.6624 0.2246 0.091 Uiso 1 1 calc R . . C28 C 0.9576(5) 0.6050(2) 0.1427(3) 0.0531(16) Uani 1 1 d . . . C29 C 0.9827(5) 0.5690(2) 0.1862(3) 0.0570(17) Uani 1 1 d . . . C30 C 0.9752(7) 0.5185(3) 0.1712(4) 0.077(2) Uani 1 1 d . . . H30A H 0.9932 0.4943 0.1997 0.092 Uiso 1 1 calc R . . C31 C 0.9418(7) 0.5029(3) 0.1151(4) 0.089(3) Uani 1 1 d . . . H31A H 0.9361 0.4687 0.1062 0.107 Uiso 1 1 calc R . . C32 C 0.9176(6) 0.5383(3) 0.0733(3) 0.072(2) Uani 1 1 d . . . H32A H 0.8946 0.5279 0.0356 0.086 Uiso 1 1 calc R . . C33 C 0.9260(5) 0.5896(2) 0.0850(3) 0.0556(16) Uani 1 1 d . . . C34 C 1.0227(6) 0.5835(2) 0.2496(3) 0.0666(18) Uani 1 1 d . . . H34A H 1.0196 0.6204 0.2527 0.080 Uiso 1 1 calc R . . C35 C 1.1620(6) 0.5661(3) 0.2699(3) 0.086(2) Uani 1 1 d . . . H35A H 1.2210 0.5806 0.2456 0.130 Uiso 1 1 calc R . . H35B H 1.1666 0.5300 0.2680 0.130 Uiso 1 1 calc R . . H35C H 1.1853 0.5770 0.3088 0.130 Uiso 1 1 calc R . . C36 C 0.9295(7) 0.5610(3) 0.2898(3) 0.096(3) Uani 1 1 d . . . H36A H 0.8423 0.5715 0.2773 0.145 Uiso 1 1 calc R . . H36B H 0.9536 0.5726 0.3283 0.145 Uiso 1 1 calc R . . H36C H 0.9344 0.5248 0.2888 0.145 Uiso 1 1 calc R . . C37 C 0.8993(6) 0.6279(3) 0.0375(3) 0.0700(19) Uani 1 1 d . . . H37A H 0.9264 0.6608 0.0538 0.084 Uiso 1 1 calc R . . C38 C 0.7545(8) 0.6320(4) 0.0168(4) 0.121(3) Uani 1 1 d . . . H38A H 0.7070 0.6385 0.0490 0.182 Uiso 1 1 calc R . . H38B H 0.7249 0.6009 -0.0012 0.182 Uiso 1 1 calc R . . H38C H 0.7406 0.6591 -0.0103 0.182 Uiso 1 1 calc R . . C39 C 0.9806(11) 0.6181(4) -0.0128(4) 0.149(4) Uani 1 1 d . . . H39A H 1.0710 0.6169 0.0014 0.224 Uiso 1 1 calc R . . H39B H 0.9661 0.6448 -0.0405 0.224 Uiso 1 1 calc R . . H39C H 0.9553 0.5865 -0.0307 0.224 Uiso 1 1 calc R . . C40 C 1.0096(5) 0.7009(2) 0.3997(2) 0.0516(15) Uani 1 1 d . . . C41 C 1.0899(6) 0.6608(2) 0.3919(3) 0.0621(17) Uani 1 1 d . . . H41A H 1.1150 0.6547 0.3556 0.075 Uiso 1 1 calc R . . C42 C 1.1336(7) 0.6298(3) 0.4367(4) 0.088(2) Uani 1 1 d . . . H42A H 1.1862 0.6023 0.4306 0.106 Uiso 1 1 calc R . . C43 C 1.0993(10) 0.6396(4) 0.4912(4) 0.105(3) Uani 1 1 d . . . H43A H 1.1297 0.6187 0.5217 0.126 Uiso 1 1 calc R . . C44 C 1.0214(9) 0.6796(4) 0.5005(3) 0.101(3) Uani 1 1 d . . . H44A H 0.9996 0.6859 0.5373 0.121 Uiso 1 1 calc R . . C45 C 0.9748(6) 0.7106(3) 0.4560(3) 0.073(2) Uani 1 1 d . . . H45A H 0.9211 0.7377 0.4624 0.088 Uiso 1 1 calc R . . C46 C 0.9133(6) 0.8018(2) 0.3669(3) 0.0554(16) Uani 1 1 d . . . C47 C 1.0133(6) 0.8369(3) 0.3664(3) 0.0680(19) Uani 1 1 d . . . H47A H 1.0914 0.8273 0.3535 0.082 Uiso 1 1 calc R . . C48 C 0.9976(8) 0.8865(3) 0.3851(3) 0.088(2) Uani 1 1 d . . . H48A H 1.0640 0.9100 0.3844 0.106 Uiso 1 1 calc R . . C49 C 0.8793(10) 0.9000(3) 0.4050(3) 0.100(3) Uani 1 1 d . . . H49A H 0.8659 0.9330 0.4165 0.120 Uiso 1 1 calc R . . C50 C 0.7850(8) 0.8652(3) 0.4075(4) 0.095(3) Uani 1 1 d . . . H50A H 0.7085 0.8744 0.4221 0.114 Uiso 1 1 calc R . . C51 C 0.7991(7) 0.8177(3) 0.3894(3) 0.077(2) Uani 1 1 d . . . H51A H 0.7321 0.7947 0.3917 0.092 Uiso 1 1 calc R . . C52 C 0.7731(5) 0.7123(2) 0.3284(2) 0.0456(14) Uani 1 1 d . . . C53 C 0.6726(5) 0.7389(3) 0.2967(2) 0.0583(17) Uani 1 1 d . . . H53A H 0.6897 0.7703 0.2814 0.070 Uiso 1 1 calc R . . C54 C 0.5476(6) 0.7191(3) 0.2878(3) 0.0689(19) Uani 1 1 d . . . H54A H 0.4813 0.7375 0.2675 0.083 Uiso 1 1 calc R . . C55 C 0.5228(6) 0.6722(3) 0.3090(3) 0.075(2) Uani 1 1 d . . . H55A H 0.4391 0.6592 0.3032 0.090 Uiso 1 1 calc R . . C57 C 0.7458(6) 0.6650(3) 0.3492(3) 0.0601(17) Uani 1 1 d . . . H57A H 0.8113 0.6467 0.3702 0.072 Uiso 1 1 calc R . . C56 C 0.6198(6) 0.6440(3) 0.3390(3) 0.074(2) Uani 1 1 d . . . H56A H 0.6026 0.6118 0.3522 0.089 Uiso 1 1 calc R . . C58 C 1.0223(14) 1.0281(4) 0.3394(8) 0.157(6) Uani 1 1 d . . . C59 C 1.1419(11) 1.0169(3) 0.3509(5) 0.102(3) Uani 1 1 d . . . H59A H 1.1876 1.0074 0.3206 0.123 Uiso 1 1 calc R . . C60 C 1.2133(12) 1.0181(5) 0.4099(10) 0.179(7) Uani 1 1 d . . . H60A H 1.3015 1.0111 0.4166 0.215 Uiso 1 1 calc R . . C61 C 1.1472(17) 1.0291(6) 0.4500(9) 0.222(9) Uani 1 1 d . . . H61A H 1.1868 1.0283 0.4876 0.266 Uiso 1 1 calc R . . C62 C 1.0166(17) 1.0424(6) 0.4403(10) 0.198(9) Uani 1 1 d . . . H62A H 0.9748 1.0524 0.4716 0.238 Uiso 1 1 calc R . . C63 C 0.9470(17) 1.0415(5) 0.3877(8) 0.157(7) Uani 1 1 d . . . H63A H 0.8587 1.0488 0.3823 0.189 Uiso 1 1 calc R . . C64 C 0.9470(16) 1.0288(5) 0.2884(7) 0.227(9) Uani 1 1 d . . . H64A H 0.9986 1.0202 0.2582 0.341 Uiso 1 1 calc R . . H64B H 0.9111 1.0620 0.2817 0.341 Uiso 1 1 calc R . . H64C H 0.8780 1.0048 0.2892 0.341 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 Pd1 0.0356(2) 0.0542(3) 0.0270(2) -0.0033(2) 0.00730(15) 0.0028(2) Cl1 0.0415(7) 0.1083(13) 0.0399(9) 0.0011(9) 0.0010(6) 0.0027(8) P1 0.0404(8) 0.0470(9) 0.0302(9) -0.0015(7) 0.0060(6) 0.0009(6) P2 0.0443(8) 0.0583(10) 0.0308(9) -0.0032(7) 0.0091(6) 0.0044(7) N1 0.037(2) 0.055(3) 0.029(3) -0.001(2) 0.0095(19) -0.0025(19) N2 0.043(3) 0.045(3) 0.049(3) -0.012(2) 0.015(2) -0.002(2) C1 0.053(3) 0.048(4) 0.047(4) -0.003(3) 0.001(3) 0.001(3) C2 0.074(4) 0.060(4) 0.055(5) -0.003(4) 0.016(3) 0.016(3) C3 0.098(5) 0.075(5) 0.080(6) -0.015(5) 0.024(5) 0.020(4) C4 0.114(6) 0.075(6) 0.093(7) -0.016(5) -0.011(5) 0.038(5) C5 0.153(8) 0.071(6) 0.082(7) -0.002(5) -0.039(6) 0.034(5) C6 0.102(5) 0.058(5) 0.059(5) -0.004(4) -0.011(4) 0.024(4) C7 0.046(3) 0.058(4) 0.032(3) 0.000(3) 0.002(3) 0.003(3) C8 0.067(4) 0.080(5) 0.038(4) 0.000(3) -0.002(3) 0.002(3) C9 0.054(4) 0.111(6) 0.041(4) 0.012(4) 0.009(3) 0.003(4) C10 0.073(5) 0.165(8) 0.039(5) 0.023(5) 0.017(4) 0.010(5) C11 0.089(5) 0.134(7) 0.035(4) 0.002(4) 0.005(4) 0.016(5) C12 0.086(5) 0.095(5) 0.043(5) -0.007(4) -0.018(4) 0.004(4) C13 0.039(3) 0.055(4) 0.033(3) 0.008(3) 0.003(2) -0.003(3) C14 0.042(3) 0.058(4) 0.033(3) 0.005(3) 0.006(2) 0.003(3) C15 0.048(3) 0.081(5) 0.049(4) 0.008(4) 0.020(3) 0.010(3) C16 0.049(4) 0.083(5) 0.061(5) 0.008(4) 0.015(3) -0.012(4) C17 0.062(4) 0.076(5) 0.065(5) 0.002(4) 0.004(4) -0.030(4) C18 0.049(3) 0.056(4) 0.047(4) 0.002(3) 0.008(3) -0.008(3) C19 0.053(3) 0.067(4) 0.047(4) -0.009(3) 0.017(3) 0.012(3) C20 0.084(5) 0.067(5) 0.077(6) 0.000(4) 0.009(4) 0.004(4) C21 0.115(6) 0.108(6) 0.084(6) -0.033(5) 0.050(5) -0.006(5) C22 0.075(4) 0.058(4) 0.075(5) -0.025(4) 0.022(4) -0.019(3) C23 0.122(6) 0.123(7) 0.090(7) -0.051(6) 0.034(5) -0.045(5) C24 0.102(6) 0.071(6) 0.154(9) -0.013(6) 0.007(6) 0.004(4) C25 0.028(2) 0.054(4) 0.025(3) -0.002(3) 0.006(2) -0.001(2) C26 0.041(3) 0.048(4) 0.027(3) -0.003(3) 0.006(2) 0.001(2) C27 0.046(3) 0.066(4) 0.075(5) -0.019(4) 0.027(3) -0.007(3) C28 0.041(3) 0.053(4) 0.068(5) -0.010(4) 0.021(3) -0.001(3) C29 0.061(4) 0.045(4) 0.067(5) -0.010(4) 0.014(3) 0.000(3) C30 0.089(5) 0.065(5) 0.078(6) -0.005(4) 0.016(4) 0.001(4) C31 0.096(6) 0.057(5) 0.115(8) -0.031(6) 0.019(5) -0.011(4) C32 0.080(5) 0.071(6) 0.067(5) -0.025(5) 0.021(4) -0.012(4) C33 0.056(4) 0.062(5) 0.050(5) -0.021(4) 0.016(3) -0.005(3) C34 0.081(5) 0.056(4) 0.063(5) 0.002(4) 0.011(4) 0.006(3) C35 0.084(5) 0.101(6) 0.075(6) 0.002(5) 0.012(4) 0.009(4) C36 0.110(6) 0.101(6) 0.085(6) -0.005(5) 0.040(5) -0.003(5) C37 0.079(5) 0.082(5) 0.053(5) -0.022(4) 0.022(4) -0.019(4) C38 0.100(6) 0.155(9) 0.101(8) 0.022(7) -0.020(5) -0.019(6) C39 0.194(10) 0.152(9) 0.121(9) 0.006(7) 0.104(8) 0.013(8) C40 0.051(3) 0.074(4) 0.030(4) 0.003(3) 0.004(3) -0.006(3) C41 0.065(4) 0.071(5) 0.050(5) 0.010(4) 0.007(3) 0.008(3) C42 0.092(5) 0.083(6) 0.086(7) 0.018(5) -0.006(5) 0.011(4) C43 0.119(7) 0.119(8) 0.070(7) 0.039(6) -0.028(6) -0.023(6) C44 0.130(7) 0.136(8) 0.035(5) 0.021(5) 0.005(5) -0.005(6) C45 0.081(5) 0.091(5) 0.048(5) 0.007(4) 0.010(4) 0.002(4) C46 0.068(4) 0.061(4) 0.039(4) 0.001(3) 0.017(3) 0.004(3) C47 0.071(4) 0.078(5) 0.057(5) -0.017(4) 0.016(3) -0.003(4) C48 0.131(7) 0.062(5) 0.074(6) -0.018(4) 0.021(5) -0.020(4) C49 0.150(8) 0.076(6) 0.083(6) -0.021(5) 0.049(6) 0.031(6) C50 0.115(6) 0.066(6) 0.116(7) -0.020(5) 0.072(5) 0.001(5) C51 0.086(5) 0.074(5) 0.078(6) -0.010(4) 0.046(4) 0.007(4) C52 0.047(3) 0.060(4) 0.034(4) 0.000(3) 0.017(3) 0.008(3) C53 0.049(3) 0.089(5) 0.040(4) 0.002(3) 0.016(3) 0.012(3) C54 0.046(4) 0.113(6) 0.051(4) 0.006(4) 0.018(3) 0.010(4) C55 0.044(4) 0.125(7) 0.058(5) -0.007(5) 0.015(3) -0.007(4) C57 0.053(4) 0.077(5) 0.050(4) 0.000(4) 0.008(3) 0.003(3) C56 0.072(5) 0.093(5) 0.059(5) 0.002(4) 0.013(4) -0.027(4) C58 0.120(9) 0.096(8) 0.241(19) 0.063(10) -0.043(11) -0.015(7) C59 0.106(8) 0.069(5) 0.134(10) 0.021(6) 0.022(7) 0.011(5) C60 0.103(9) 0.122(9) 0.32(2) 0.078(12) 0.055(13) 0.027(7) C61 0.151(13) 0.170(13) 0.37(3) -0.022(14) 0.129(15) 0.040(10) C62 0.177(17) 0.128(11) 0.32(3) 0.058(16) 0.142(17) 0.039(10) C63 0.191(16) 0.086(8) 0.218(18) 0.039(11) 0.129(15) 0.033(9) C64 0.275(18) 0.135(11) 0.239(19) -0.046(11) -0.120(16) 0.019(10) _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 Pd1 N1 2.115(4) . ? Pd1 C25 2.141(5) . ? Pd1 P2 2.2720(18) . ? Pd1 Cl1 2.3347(18) . ? Pd1 P1 2.698(2) . ? P1 N1 1.592(4) . ? P1 C25 1.791(5) . ? P1 C7 1.808(6) . ? P1 C1 1.848(6) . ? P2 C52 1.815(6) . ? P2 C40 1.828(6) . ? P2 C46 1.839(6) . ? N1 C13 1.439(6) . ? N2 C26 1.279(6) . ? N2 C28 1.441(7) . ? C1 C6 1.395(9) . ? C1 C2 1.395(8) . ? C2 C3 1.390(9) . ? C3 C4 1.345(10) . ? C4 C5 1.411(11) . ? C5 C6 1.379(10) . ? C7 C9 1.391(8) . ? C7 C8 1.403(7) . ? C8 C12 1.386(9) . ? C9 C10 1.396(9) . ? C10 C11 1.360(9) . ? C11 C12 1.383(10) . ? C13 C18 1.417(8) . ? C13 C14 1.436(7) . ? C14 C15 1.393(7) . ? C14 C19 1.499(8) . ? C15 C16 1.347(8) . ? C16 C17 1.381(9) . ? C17 C18 1.416(8) . ? C18 C22 1.488(8) . ? C19 C20 1.507(8) . ? C19 C21 1.556(9) . ? C22 C23 1.551(10) . ? C22 C24 1.578(10) . ? C25 C26 1.483(7) . ? C26 C27 1.533(7) . ? C28 C29 1.397(9) . ? C28 C33 1.414(8) . ? C29 C30 1.382(9) . ? C29 C34 1.545(9) . ? C30 C31 1.384(10) . ? C31 C32 1.361(10) . ? C32 C33 1.385(9) . ? C33 C37 1.508(9) . ? C34 C35 1.541(8) . ? C34 C36 1.542(9) . ? C37 C38 1.530(9) . ? C37 C39 1.544(10) . ? C40 C41 1.372(8) . ? C40 C45 1.426(9) . ? C41 C42 1.370(10) . ? C42 C43 1.387(12) . ? C43 C44 1.364(12) . ? C44 C45 1.372(10) . ? C46 C47 1.394(8) . ? C46 C51 1.411(8) . ? C47 C48 1.398(9) . ? C48 C49 1.405(10) . ? C49 C50 1.349(11) . ? C50 C51 1.339(9) . ? C52 C57 1.385(8) . ? C52 C53 1.401(7) . ? C53 C54 1.393(8) . ? C54 C55 1.371(10) . ? C55 C56 1.381(9) . ? C57 C56 1.416(8) . ? C58 C59 1.275(13) . ? C58 C64 1.353(15) . ? C58 C63 1.49(2) . ? C59 C60 1.494(18) . ? C60 C61 1.26(2) . ? C61 C62 1.393(19) . ? C62 C63 1.36(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pd1 C25 74.40(17) . . ? N1 Pd1 P2 165.15(12) . . ? C25 Pd1 P2 101.15(14) . . ? N1 Pd1 Cl1 95.89(12) . . ? C25 Pd1 Cl1 168.63(13) . . ? P2 Pd1 Cl1 89.71(7) . . ? N1 Pd1 P1 36.12(11) . . ? C25 Pd1 P1 41.49(13) . . ? P2 Pd1 P1 133.76(6) . . ? Cl1 Pd1 P1 130.58(5) . . ? N1 P1 C25 98.9(2) . . ? N1 P1 C7 116.1(2) . . ? C25 P1 C7 118.3(3) . . ? N1 P1 C1 118.1(2) . . ? C25 P1 C1 103.7(3) . . ? C7 P1 C1 102.0(3) . . ? N1 P1 Pd1 51.57(15) . . ? C25 P1 Pd1 52.36(15) . . ? C7 P1 Pd1 153.27(19) . . ? C1 P1 Pd1 104.6(2) . . ? C52 P2 C40 101.9(3) . . ? C52 P2 C46 103.7(3) . . ? C40 P2 C46 105.9(3) . . ? C52 P2 Pd1 118.85(19) . . ? C40 P2 Pd1 117.0(2) . . ? C46 P2 Pd1 108.1(2) . . ? C13 N1 P1 134.7(4) . . ? C13 N1 Pd1 131.2(3) . . ? P1 N1 Pd1 92.31(18) . . ? C26 N2 C28 121.4(4) . . ? C6 C1 C2 119.2(6) . . ? C6 C1 P1 121.7(5) . . ? C2 C1 P1 119.1(5) . . ? C3 C2 C1 120.0(7) . . ? C4 C3 C2 121.5(8) . . ? C3 C4 C5 118.8(7) . . ? C6 C5 C4 121.0(8) . . ? C5 C6 C1 119.4(7) . . ? C9 C7 C8 117.9(6) . . ? C9 C7 P1 121.4(4) . . ? C8 C7 P1 120.2(4) . . ? C12 C8 C7 120.6(6) . . ? C7 C9 C10 120.8(6) . . ? C11 C10 C9 120.4(7) . . ? C10 C11 C12 120.0(7) . . ? C11 C12 C8 120.3(6) . . ? C18 C13 C14 121.4(5) . . ? C18 C13 N1 120.4(5) . . ? C14 C13 N1 118.1(5) . . ? C15 C14 C13 116.5(5) . . ? C15 C14 C19 121.9(5) . . ? C13 C14 C19 121.5(4) . . ? C16 C15 C14 123.9(6) . . ? C15 C16 C17 119.3(6) . . ? C16 C17 C18 122.2(6) . . ? C17 C18 C13 116.7(5) . . ? C17 C18 C22 119.9(5) . . ? C13 C18 C22 123.4(5) . . ? C14 C19 C20 111.4(5) . . ? C14 C19 C21 114.3(5) . . ? C20 C19 C21 110.3(6) . . ? C18 C22 C23 112.3(6) . . ? C18 C22 C24 110.9(6) . . ? C23 C22 C24 111.3(6) . . ? C26 C25 P1 121.5(4) . . ? C26 C25 Pd1 109.8(3) . . ? P1 C25 Pd1 86.15(19) . . ? N2 C26 C25 122.3(4) . . ? N2 C26 C27 122.5(5) . . ? C25 C26 C27 115.2(4) . . ? C29 C28 C33 120.3(6) . . ? C29 C28 N2 120.5(6) . . ? C33 C28 N2 119.0(6) . . ? C30 C29 C28 118.2(6) . . ? C30 C29 C34 119.1(6) . . ? C28 C29 C34 122.7(5) . . ? C29 C30 C31 122.1(7) . . ? C32 C31 C30 118.9(7) . . ? C31 C32 C33 122.0(7) . . ? C32 C33 C28 118.3(7) . . ? C32 C33 C37 120.6(6) . . ? C28 C33 C37 121.0(6) . . ? C35 C34 C36 108.9(6) . . ? C35 C34 C29 111.5(6) . . ? C36 C34 C29 111.7(6) . . ? C33 C37 C38 112.1(6) . . ? C33 C37 C39 112.2(7) . . ? C38 C37 C39 111.6(7) . . ? C41 C40 C45 118.8(6) . . ? C41 C40 P2 121.1(5) . . ? C45 C40 P2 119.9(5) . . ? C42 C41 C40 121.0(7) . . ? C41 C42 C43 119.8(8) . . ? C44 C43 C42 120.5(8) . . ? C43 C44 C45 120.6(8) . . ? C44 C45 C40 119.3(7) . . ? C47 C46 C51 117.3(6) . . ? C47 C46 P2 119.0(5) . . ? C51 C46 P2 123.7(5) . . ? C46 C47 C48 120.7(6) . . ? C47 C48 C49 118.6(7) . . ? C50 C49 C48 120.3(7) . . ? C51 C50 C49 121.5(7) . . ? C50 C51 C46 121.5(7) . . ? C57 C52 C53 118.2(5) . . ? C57 C52 P2 121.0(4) . . ? C53 C52 P2 120.7(5) . . ? C54 C53 C52 121.0(6) . . ? C55 C54 C53 119.6(6) . . ? C54 C55 C56 121.3(6) . . ? C52 C57 C56 121.0(6) . . ? C55 C56 C57 118.7(7) . . ? C59 C58 C64 130(2) . . ? C59 C58 C63 118.4(15) . . ? C64 C58 C63 111.6(16) . . ? C58 C59 C60 124.2(14) . . ? C61 C60 C59 116.1(14) . . ? C60 C61 C62 122(2) . . ? C63 C62 C61 124(2) . . ? C62 C63 C58 115.0(17) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 23.35 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.975 _refine_diff_density_min -1.339 _refine_diff_density_rms 0.097 #===end data_NiBr((C6H3i-Pr2)NC(Me)CHPPh2(NC6H3i-Pr2))(PPh3) _database_code_CSD 211495 _audit_creation_method SHELXL-97 _chemical_formula_sum 'C59 H70 Br Cl4 N2 Ni P2' _chemical_formula_weight 1149.53 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 23.05(3) _cell_length_b 10.399(15) _cell_length_c 24.60(3) _cell_angle_alpha 90.00 _cell_angle_beta 104.11(3) _cell_angle_gamma 90.00 _cell_volume 5719(14) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 50.0 _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.21 _exptl_crystal_density_diffrn 1.335 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2396 _exptl_absorpt_coefficient_mu 1.319 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.097503 _exptl_absorpt_correction_T_max 0.191327 _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 19576 _diffrn_reflns_av_R_equivalents 0.2008 _diffrn_reflns_av_sigmaI/netI 0.1384 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 23.59 _reflns_number_total 8239 _reflns_number_gt 4880 _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^)+(0.1656P)^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 8239 _refine_ls_number_parameters 597 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1321 _refine_ls_R_factor_gt 0.0784 _refine_ls_wR_factor_ref 0.2251 _refine_ls_wR_factor_gt 0.1903 _refine_ls_goodness_of_fit_ref 1.160 _refine_ls_restrained_S_all 1.168 _refine_ls_shift/su_max 0.004 _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 0.22208(5) 0.72900(8) 0.43420(3) 0.0390(3) Uani 1 1 d . . . Br1 Br 0.20656(5) 0.50976(7) 0.41426(3) 0.0643(3) Uani 1 1 d . . . Cl1 Cl 0.1941(3) 0.2843(5) 0.00435(18) 0.1571(16) Uiso 1 1 d D . . Cl2 Cl 0.1101(3) 0.2452(6) 0.0707(2) 0.211(2) Uiso 1 1 d D . . Cl3 Cl 0.5060(7) 1.2299(17) 0.2274(6) 0.442(8) Uiso 1 1 d D . . Cl4 Cl 0.5261(9) 1.4239(17) 0.3146(8) 0.507(10) Uiso 1 1 d D . . P1 P 0.18514(9) 0.92804(17) 0.37370(7) 0.0378(5) Uani 1 1 d . . . P2 P 0.23864(10) 0.68927(18) 0.52457(7) 0.0425(5) Uani 1 1 d . . . N1 N 0.1884(3) 0.7813(5) 0.3571(2) 0.0449(16) Uani 1 1 d . . . N2 N 0.3287(3) 0.9055(5) 0.4035(2) 0.0430(16) Uani 1 1 d . . . H2A H 0.3075 0.8609 0.3764 0.052 Uiso 1 1 calc R . . C1 C 0.1928(4) 1.0444(7) 0.3215(3) 0.0441(19) Uani 1 1 d . . . C2 C 0.1755(4) 1.0131(7) 0.2653(3) 0.055(2) Uani 1 1 d . . . H2B H 0.1655 0.9286 0.2546 0.066 Uiso 1 1 calc R . . C3 C 0.1729(5) 1.1066(8) 0.2245(3) 0.071(3) Uani 1 1 d . . . H3A H 0.1614 1.0850 0.1867 0.085 Uiso 1 1 calc R . . C4 C 0.1875(5) 1.2322(8) 0.2407(4) 0.074(3) Uani 1 1 d . . . H4A H 0.1870 1.2947 0.2135 0.089 Uiso 1 1 calc R . . C5 C 0.2027(5) 1.2657(8) 0.2963(3) 0.064(3) Uani 1 1 d . . . H5A H 0.2111 1.3509 0.3068 0.077 Uiso 1 1 calc R . . C6 C 0.2055(4) 1.1719(7) 0.3368(3) 0.052(2) Uani 1 1 d . . . H6A H 0.2159 1.1944 0.3746 0.063 Uiso 1 1 calc R . . C7 C 0.1168(4) 0.9824(7) 0.3905(3) 0.049(2) Uani 1 1 d . . . C8 C 0.0797(4) 1.0784(8) 0.3611(3) 0.060(2) Uani 1 1 d . . . H8A H 0.0904 1.1205 0.3316 0.072 Uiso 1 1 calc R . . C9 C 0.0274(5) 1.1116(9) 0.3754(4) 0.071(3) Uani 1 1 d . . . H9A H 0.0039 1.1778 0.3562 0.086 Uiso 1 1 calc R . . C10 C 0.0097(4) 1.0490(10) 0.4171(4) 0.072(3) Uani 1 1 d . . . H10A H -0.0262 1.0711 0.4257 0.086 Uiso 1 1 calc R . . C11 C 0.0441(4) 0.9548(9) 0.4460(3) 0.063(2) Uani 1 1 d . . . H11A H 0.0321 0.9127 0.4748 0.076 Uiso 1 1 calc R . . C12 C 0.0968(4) 0.9206(8) 0.4332(3) 0.056(2) Uani 1 1 d . . . H12A H 0.1197 0.8549 0.4534 0.067 Uiso 1 1 calc R . . C13 C 0.3896(4) 0.9269(8) 0.4036(3) 0.047(2) Uani 1 1 d . . . C14 C 0.4315(4) 0.8353(8) 0.4261(3) 0.051(2) Uani 1 1 d . . . C15 C 0.4911(4) 0.8538(10) 0.4235(4) 0.071(3) Uani 1 1 d . . . H15A H 0.5196 0.7927 0.4395 0.085 Uiso 1 1 calc R . . C16 C 0.5081(5) 0.9573(10) 0.3985(4) 0.073(3) Uani 1 1 d . . . H16A H 0.5478 0.9684 0.3974 0.088 Uiso 1 1 calc R . . C17 C 0.4652(5) 1.0462(10) 0.3747(4) 0.074(3) Uani 1 1 d . . . H17A H 0.4768 1.1174 0.3570 0.088 Uiso 1 1 calc R . . C18 C 0.4053(4) 1.0348(8) 0.3760(3) 0.055(2) Uani 1 1 d . . . C19 C 0.4169(5) 0.7159(8) 0.4575(4) 0.066(2) Uani 1 1 d . . . H19A H 0.3733 0.7091 0.4509 0.079 Uiso 1 1 calc R . . C20 C 0.4403(6) 0.5924(9) 0.4375(4) 0.087(3) Uani 1 1 d . . . H20A H 0.4229 0.5814 0.3982 0.130 Uiso 1 1 calc R . . H20B H 0.4296 0.5208 0.4577 0.130 Uiso 1 1 calc R . . H20C H 0.4830 0.5971 0.4440 0.130 Uiso 1 1 calc R . . C21 C 0.4434(6) 0.7297(10) 0.5202(4) 0.093(4) Uani 1 1 d . . . H21A H 0.4282 0.8065 0.5334 0.139 Uiso 1 1 calc R . . H21B H 0.4861 0.7351 0.5274 0.139 Uiso 1 1 calc R . . H21C H 0.4325 0.6565 0.5393 0.139 Uiso 1 1 calc R . . C22 C 0.3596(4) 1.1357(8) 0.3498(3) 0.064(2) Uani 1 1 d . . . H22A H 0.3202 1.1055 0.3526 0.077 Uiso 1 1 calc R . . C23 C 0.3572(6) 1.1574(12) 0.2874(4) 0.106(4) Uani 1 1 d . . . H23A H 0.3488 1.0773 0.2676 0.159 Uiso 1 1 calc R . . H23B H 0.3949 1.1902 0.2836 0.159 Uiso 1 1 calc R . . H23C H 0.3262 1.2181 0.2719 0.159 Uiso 1 1 calc R . . C24 C 0.3724(6) 1.2627(10) 0.3814(4) 0.100(4) Uani 1 1 d . . . H24A H 0.3729 1.2492 0.4201 0.149 Uiso 1 1 calc R . . H24B H 0.3417 1.3238 0.3654 0.149 Uiso 1 1 calc R . . H24C H 0.4105 1.2951 0.3786 0.149 Uiso 1 1 calc R . . C25 C 0.3034(4) 0.9470(6) 0.4402(3) 0.042(2) Uani 1 1 d . . . C26 C 0.3374(4) 1.0275(8) 0.4889(3) 0.063(3) Uani 1 1 d . . . H26A H 0.3778 1.0392 0.4859 0.095 Uiso 1 1 calc R . . H26B H 0.3376 0.9845 0.5235 0.095 Uiso 1 1 calc R . . H26C H 0.3183 1.1098 0.4883 0.095 Uiso 1 1 calc R . . C27 C 0.2396(3) 0.9200(6) 0.4385(3) 0.0355(17) Uani 1 1 d . . . H27A H 0.2264 0.9621 0.4691 0.043 Uiso 1 1 calc R . . C28 C 0.1660(4) 0.7067(6) 0.3071(2) 0.0396(19) Uani 1 1 d . . . C29 C 0.2072(4) 0.6780(6) 0.2737(3) 0.0433(19) Uani 1 1 d . . . C30 C 0.1878(4) 0.6060(7) 0.2259(3) 0.050(2) Uani 1 1 d . . . H30A H 0.2138 0.5891 0.2033 0.060 Uiso 1 1 calc R . . C31 C 0.1309(5) 0.5587(8) 0.2110(3) 0.062(2) Uani 1 1 d . . . H31A H 0.1189 0.5102 0.1784 0.074 Uiso 1 1 calc R . . C32 C 0.0901(5) 0.5823(8) 0.2441(3) 0.069(3) Uani 1 1 d . . . H32A H 0.0768 0.4997 0.2548 0.083 Uiso 1 1 calc R . . H32B H 0.0554 0.6243 0.2205 0.083 Uiso 1 1 calc R . . C33 C 0.1088(4) 0.6564(7) 0.2932(3) 0.049(2) Uani 1 1 d . . . C34 C 0.2715(4) 0.7190(8) 0.2903(3) 0.058(2) Uani 1 1 d . . . H34A H 0.2766 0.7755 0.3230 0.070 Uiso 1 1 calc R . . C35 C 0.2919(5) 0.7934(10) 0.2440(4) 0.084(3) Uani 1 1 d . . . H35A H 0.2656 0.8650 0.2320 0.127 Uiso 1 1 calc R . . H35B H 0.2908 0.7373 0.2128 0.127 Uiso 1 1 calc R . . H35C H 0.3319 0.8242 0.2585 0.127 Uiso 1 1 calc R . . C36 C 0.3125(6) 0.6035(11) 0.3070(4) 0.100(4) Uani 1 1 d . . . H36A H 0.3005 0.5559 0.3359 0.150 Uiso 1 1 calc R . . H36B H 0.3530 0.6325 0.3208 0.150 Uiso 1 1 calc R . . H36C H 0.3100 0.5491 0.2750 0.150 Uiso 1 1 calc R . . C37 C 0.0628(5) 0.6810(9) 0.3269(3) 0.064(2) Uani 1 1 d . . . H37A H 0.0843 0.7207 0.3622 0.077 Uiso 1 1 calc R . . C38 C 0.0168(5) 0.7755(12) 0.2987(4) 0.095(3) Uani 1 1 d . . . H38A H 0.0361 0.8519 0.2900 0.142 Uiso 1 1 calc R . . H38B H -0.0085 0.7970 0.3232 0.142 Uiso 1 1 calc R . . H38C H -0.0071 0.7387 0.2648 0.142 Uiso 1 1 calc R . . C39 C 0.0364(6) 0.5570(12) 0.3423(4) 0.104(4) Uani 1 1 d . . . H39A H 0.0681 0.5004 0.3605 0.156 Uiso 1 1 calc R . . H39B H 0.0132 0.5167 0.3090 0.156 Uiso 1 1 calc R . . H39C H 0.0113 0.5753 0.3672 0.156 Uiso 1 1 calc R . . C40 C 0.3602(5) 0.3958(8) 0.5472(4) 0.078(3) Uani 1 1 d . . . H40A H 0.3884 0.3657 0.5290 0.094 Uiso 1 1 calc R . . C41 C 0.3552(5) 0.3396(9) 0.5969(4) 0.081(3) Uani 1 1 d . . . H41A H 0.3795 0.2705 0.6117 0.097 Uiso 1 1 calc R . . C42 C 0.3150(5) 0.3853(9) 0.6237(4) 0.075(3) Uani 1 1 d . . . H42A H 0.3113 0.3463 0.6567 0.090 Uiso 1 1 calc R . . C43 C 0.2789(5) 0.4905(8) 0.6024(3) 0.065(3) Uani 1 1 d . . . H43A H 0.2520 0.5221 0.6219 0.078 Uiso 1 1 calc R . . C44 C 0.2825(4) 0.5483(7) 0.5526(3) 0.0432(19) Uani 1 1 d . . . C45 C 0.3231(4) 0.4967(8) 0.5249(3) 0.060(2) Uani 1 1 d . . . H45A H 0.3253 0.5310 0.4905 0.072 Uiso 1 1 calc R . . C46 C 0.1665(4) 0.6657(7) 0.5427(3) 0.0439(19) Uani 1 1 d . . . C47 C 0.1599(4) 0.6887(7) 0.5974(3) 0.054(2) Uani 1 1 d . . . H47A H 0.1923 0.7174 0.6251 0.064 Uiso 1 1 calc R . . C48 C 0.1059(5) 0.6690(8) 0.6098(4) 0.062(2) Uani 1 1 d . . . H48A H 0.1022 0.6804 0.6463 0.074 Uiso 1 1 calc R . . C49 C 0.0556(5) 0.6311(8) 0.5673(4) 0.073(3) Uani 1 1 d . . . H49A H 0.0408 0.5514 0.5793 0.087 Uiso 1 1 calc R . . H49B H 0.0247 0.6953 0.5658 0.087 Uiso 1 1 calc R . . C50 C 0.0611(4) 0.6132(8) 0.5139(4) 0.064(2) Uani 1 1 d . . . H50A H 0.0278 0.5903 0.4858 0.077 Uiso 1 1 calc R . . C51 C 0.1158(4) 0.6288(8) 0.5014(3) 0.053(2) Uani 1 1 d . . . H51A H 0.1191 0.6146 0.4650 0.064 Uiso 1 1 calc R . . C52 C 0.2728(4) 0.8135(7) 0.5745(3) 0.046(2) Uani 1 1 d . . . C53 C 0.3310(5) 0.8025(8) 0.6058(3) 0.061(2) Uani 1 1 d . . . H53A H 0.3529 0.7292 0.6021 0.073 Uiso 1 1 calc R . . C54 C 0.3582(5) 0.8998(9) 0.6434(3) 0.072(3) Uani 1 1 d . . . H54A H 0.3975 0.8914 0.6643 0.087 Uiso 1 1 calc R . . C55 C 0.3253(6) 1.0070(9) 0.6486(4) 0.075(3) Uani 1 1 d . . . H55A H 0.3425 1.0713 0.6736 0.090 Uiso 1 1 calc R . . C56 C 0.2674(6) 1.0211(8) 0.6173(4) 0.072(3) Uani 1 1 d . . . H56A H 0.2460 1.0951 0.6209 0.086 Uiso 1 1 calc R . . C57 C 0.2411(4) 0.9251(7) 0.5804(3) 0.048(2) Uani 1 1 d . . . H57A H 0.2019 0.9350 0.5593 0.057 Uiso 1 1 calc R . . C58 C 0.1325(7) 0.2209(18) 0.0056(7) 0.218(11) Uani 1 1 d D . . H58A H 0.1349 0.1293 -0.0008 0.262 Uiso 1 1 calc R . . H58B H 0.1018 0.2559 -0.0250 0.262 Uiso 1 1 calc R . . C59 C 0.5172(18) 1.375(3) 0.2510(12) 0.36(2) Uiso 1 1 d D . . H59B H 0.5523 1.4051 0.2396 0.434 Uiso 1 1 calc R . . H59A H 0.4839 1.4250 0.2293 0.434 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 0.0560(7) 0.0327(5) 0.0297(5) 0.0002(3) 0.0133(4) -0.0004(5) Br1 0.1091(9) 0.0377(4) 0.0440(5) -0.0024(3) 0.0145(5) -0.0041(5) P1 0.0493(14) 0.0347(9) 0.0308(9) 0.0009(7) 0.0125(9) 0.0046(9) P2 0.0600(16) 0.0371(10) 0.0321(9) 0.0036(8) 0.0144(9) -0.0014(10) N1 0.068(5) 0.042(3) 0.026(3) -0.001(2) 0.013(3) 0.005(3) N2 0.051(5) 0.043(3) 0.037(3) -0.012(3) 0.015(3) -0.005(3) C1 0.055(6) 0.041(4) 0.040(4) 0.006(3) 0.018(4) 0.003(4) C2 0.076(7) 0.044(4) 0.046(4) 0.002(4) 0.015(4) 0.000(4) C3 0.112(9) 0.057(6) 0.041(4) 0.010(4) 0.014(5) 0.019(6) C4 0.116(10) 0.048(5) 0.063(5) 0.024(4) 0.032(6) 0.013(5) C5 0.081(8) 0.042(5) 0.069(6) 0.011(4) 0.017(5) -0.002(5) C6 0.068(7) 0.045(4) 0.048(4) -0.001(4) 0.021(4) -0.003(4) C7 0.068(7) 0.039(4) 0.046(4) -0.004(3) 0.025(4) 0.003(4) C8 0.075(7) 0.057(5) 0.046(4) 0.003(4) 0.010(4) 0.025(5) C9 0.066(7) 0.080(6) 0.064(5) 0.004(5) 0.007(5) 0.039(6) C10 0.050(7) 0.105(7) 0.063(5) -0.007(5) 0.019(5) 0.020(6) C11 0.053(6) 0.085(6) 0.057(5) 0.011(5) 0.023(5) 0.013(5) C12 0.068(7) 0.050(5) 0.057(5) 0.000(4) 0.028(5) 0.006(4) C13 0.048(6) 0.053(5) 0.045(4) -0.015(4) 0.021(4) -0.011(4) C14 0.044(6) 0.050(5) 0.060(5) -0.004(4) 0.013(4) 0.002(4) C15 0.035(6) 0.085(7) 0.090(6) 0.005(5) 0.010(5) 0.009(5) C16 0.049(7) 0.079(7) 0.093(7) 0.017(6) 0.021(5) -0.004(6) C17 0.075(8) 0.072(6) 0.079(6) 0.008(5) 0.028(6) -0.033(6) C18 0.057(7) 0.053(5) 0.059(5) -0.004(4) 0.024(5) -0.002(4) C19 0.060(7) 0.058(5) 0.083(6) 0.010(4) 0.025(5) -0.003(5) C20 0.102(10) 0.067(6) 0.087(7) 0.006(5) 0.014(6) 0.007(6) C21 0.129(11) 0.076(7) 0.082(7) 0.002(5) 0.043(7) -0.020(7) C22 0.063(7) 0.057(5) 0.075(6) 0.017(4) 0.022(5) 0.000(5) C23 0.113(11) 0.127(10) 0.069(6) 0.009(6) 0.003(6) 0.007(9) C24 0.132(12) 0.076(7) 0.087(7) 0.002(5) 0.018(7) 0.014(7) C25 0.066(6) 0.024(3) 0.037(4) 0.001(3) 0.013(4) -0.004(4) C26 0.079(7) 0.068(5) 0.047(4) -0.014(4) 0.024(5) -0.031(5) C27 0.036(5) 0.033(4) 0.039(4) -0.002(3) 0.013(3) -0.011(3) C28 0.063(6) 0.028(4) 0.025(3) 0.000(3) 0.006(3) -0.001(4) C29 0.060(6) 0.034(4) 0.035(4) -0.001(3) 0.009(4) 0.006(4) C30 0.067(7) 0.044(4) 0.038(4) -0.005(3) 0.010(4) 0.006(4) C31 0.078(8) 0.063(5) 0.037(4) -0.017(4) -0.001(4) 0.017(5) C32 0.108(9) 0.047(5) 0.048(5) 0.005(4) 0.008(5) 0.002(5) C33 0.063(7) 0.041(4) 0.033(4) -0.003(3) -0.005(4) -0.005(4) C34 0.059(6) 0.075(6) 0.044(4) -0.022(4) 0.020(4) -0.009(5) C35 0.090(9) 0.083(7) 0.094(7) 0.001(5) 0.048(6) 0.001(6) C36 0.082(9) 0.122(10) 0.093(7) 0.042(7) 0.013(6) 0.025(8) C37 0.066(7) 0.075(6) 0.051(5) -0.004(4) 0.014(5) -0.014(5) C38 0.086(9) 0.112(9) 0.082(7) -0.008(6) 0.013(6) 0.015(8) C39 0.104(11) 0.129(10) 0.083(7) -0.013(7) 0.032(7) -0.067(9) C40 0.098(9) 0.053(6) 0.094(7) 0.017(5) 0.042(6) 0.021(6) C41 0.082(9) 0.055(6) 0.099(7) 0.018(5) 0.010(6) 0.023(6) C42 0.092(9) 0.066(6) 0.062(5) 0.020(5) 0.009(6) 0.014(6) C43 0.094(8) 0.051(5) 0.052(5) 0.012(4) 0.025(5) 0.007(5) C44 0.051(6) 0.037(4) 0.036(4) 0.003(3) 0.001(4) -0.007(4) C45 0.071(7) 0.055(5) 0.057(5) 0.005(4) 0.022(5) 0.005(5) C46 0.057(6) 0.040(4) 0.040(4) 0.007(3) 0.021(4) 0.001(4) C47 0.059(6) 0.054(5) 0.047(4) 0.004(4) 0.011(4) -0.001(4) C48 0.068(7) 0.062(5) 0.066(5) -0.002(4) 0.037(5) -0.004(5) C49 0.081(9) 0.049(5) 0.099(7) 0.006(5) 0.044(7) -0.004(5) C50 0.060(7) 0.067(6) 0.066(5) -0.007(4) 0.016(5) -0.017(5) C51 0.063(7) 0.055(5) 0.040(4) -0.002(3) 0.009(4) -0.019(5) C52 0.069(7) 0.046(4) 0.025(3) 0.004(3) 0.013(4) -0.014(4) C53 0.081(8) 0.055(5) 0.047(4) 0.007(4) 0.016(5) -0.015(5) C54 0.089(8) 0.078(7) 0.043(5) 0.008(4) 0.002(5) -0.045(6) C55 0.119(11) 0.060(6) 0.050(5) -0.007(4) 0.030(6) -0.033(7) C56 0.123(11) 0.053(5) 0.048(5) -0.003(4) 0.038(6) -0.017(6) C57 0.064(6) 0.044(4) 0.039(4) -0.002(3) 0.019(4) -0.005(4) C58 0.100(15) 0.28(2) 0.26(2) -0.19(2) 0.022(13) 0.027(15) _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 1.944(6) . ? Ni1 C27 2.024(7) . ? Ni1 P2 2.201(3) . ? Ni1 Br1 2.341(3) . ? Ni1 P1 2.570(3) . ? Cl1 C58 1.574(14) . ? Cl2 C58 1.818(13) . ? Cl3 C59 1.618(18) . ? Cl4 C59 1.609(18) . ? P1 N1 1.587(6) . ? P1 C27 1.774(7) . ? P1 C1 1.804(7) . ? P1 C7 1.813(8) . ? P2 C44 1.819(8) . ? P2 C52 1.824(8) . ? P2 C46 1.840(8) . ? N1 C28 1.439(8) . ? N2 C25 1.267(8) . ? N2 C13 1.419(10) . ? C1 C2 1.382(10) . ? C1 C6 1.391(10) . ? C2 C3 1.388(10) . ? C3 C4 1.383(12) . ? C4 C5 1.374(11) . ? C5 C6 1.384(10) . ? C7 C8 1.396(11) . ? C7 C12 1.402(10) . ? C8 C9 1.380(13) . ? C9 C10 1.361(12) . ? C10 C11 1.348(12) . ? C11 C12 1.374(12) . ? C13 C14 1.374(11) . ? C13 C18 1.405(11) . ? C14 C15 1.403(12) . ? C14 C19 1.542(11) . ? C15 C16 1.344(13) . ? C16 C17 1.376(14) . ? C17 C18 1.394(13) . ? C18 C22 1.514(12) . ? C19 C20 1.519(13) . ? C19 C21 1.520(12) . ? C22 C24 1.525(13) . ? C22 C23 1.539(12) . ? C25 C27 1.488(11) . ? C25 C26 1.514(10) . ? C28 C33 1.382(11) . ? C28 C29 1.431(10) . ? C29 C30 1.373(10) . ? C29 C34 1.499(12) . ? C30 C31 1.365(12) . ? C31 C32 1.407(13) . ? C32 C33 1.409(10) . ? C33 C37 1.518(12) . ? C34 C36 1.523(13) . ? C34 C35 1.542(12) . ? C37 C38 1.488(14) . ? C37 C39 1.512(13) . ? C40 C45 1.380(12) . ? C40 C41 1.384(12) . ? C41 C42 1.347(14) . ? C42 C43 1.398(12) . ? C43 C44 1.385(10) . ? C44 C45 1.394(12) . ? C46 C51 1.402(11) . ? C46 C47 1.411(9) . ? C47 C48 1.367(13) . ? C48 C49 1.415(13) . ? C49 C50 1.362(11) . ? C50 C51 1.379(12) . ? C52 C53 1.380(12) . ? C52 C57 1.399(11) . ? C53 C54 1.410(12) . ? C54 C55 1.370(14) . ? C55 C56 1.377(15) . ? C56 C57 1.386(12) . ? 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 C27 78.7(2) . . ? N1 Ni1 P2 165.4(2) . . ? C27 Ni1 P2 98.51(18) . . ? N1 Ni1 Br1 93.63(18) . . ? C27 Ni1 Br1 169.99(17) . . ? P2 Ni1 Br1 90.50(7) . . ? N1 Ni1 P1 38.07(17) . . ? C27 Ni1 P1 43.4(2) . . ? P2 Ni1 P1 133.42(8) . . ? Br1 Ni1 P1 130.60(9) . . ? N1 P1 C27 96.8(3) . . ? N1 P1 C1 116.3(3) . . ? C27 P1 C1 120.0(4) . . ? N1 P1 C7 117.2(4) . . ? C27 P1 C7 105.9(3) . . ? C1 P1 C7 101.2(3) . . ? N1 P1 Ni1 49.1(2) . . ? C27 P1 Ni1 51.7(2) . . ? C1 P1 Ni1 151.2(3) . . ? C7 P1 Ni1 107.6(2) . . ? C44 P2 C52 101.9(4) . . ? C44 P2 C46 104.6(3) . . ? C52 P2 C46 101.5(3) . . ? C44 P2 Ni1 118.6(2) . . ? C52 P2 Ni1 119.2(2) . . ? C46 P2 Ni1 109.0(2) . . ? C28 N1 P1 135.2(5) . . ? C28 N1 Ni1 131.2(4) . . ? P1 N1 Ni1 92.9(3) . . ? C25 N2 C13 124.9(6) . . ? C2 C1 C6 119.1(6) . . ? C2 C1 P1 120.0(6) . . ? C6 C1 P1 119.8(5) . . ? C1 C2 C3 120.7(7) . . ? C4 C3 C2 119.3(7) . . ? C5 C4 C3 120.8(7) . . ? C4 C5 C6 119.7(8) . . ? C5 C6 C1 120.4(7) . . ? C8 C7 C12 116.3(8) . . ? C8 C7 P1 124.2(6) . . ? C12 C7 P1 119.4(6) . . ? C9 C8 C7 120.7(8) . . ? C10 C9 C8 121.0(8) . . ? C11 C10 C9 119.9(9) . . ? C10 C11 C12 120.5(8) . . ? C11 C12 C7 121.6(8) . . ? C14 C13 C18 120.6(8) . . ? C14 C13 N2 119.4(7) . . ? C18 C13 N2 119.7(8) . . ? C13 C14 C15 119.1(8) . . ? C13 C14 C19 122.8(8) . . ? C15 C14 C19 118.0(8) . . ? C16 C15 C14 121.9(9) . . ? C15 C16 C17 118.3(10) . . ? C16 C17 C18 123.1(8) . . ? C17 C18 C13 116.9(8) . . ? C17 C18 C22 121.4(8) . . ? C13 C18 C22 121.6(8) . . ? C20 C19 C21 108.8(8) . . ? C20 C19 C14 112.4(7) . . ? C21 C19 C14 110.4(8) . . ? C18 C22 C24 110.8(8) . . ? C18 C22 C23 112.2(8) . . ? C24 C22 C23 109.7(8) . . ? N2 C25 C27 122.7(6) . . ? N2 C25 C26 120.9(8) . . ? C27 C25 C26 116.4(6) . . ? C25 C27 P1 119.6(4) . . ? C25 C27 Ni1 111.7(5) . . ? P1 C27 Ni1 84.9(3) . . ? C33 C28 C29 120.5(6) . . ? C33 C28 N1 122.4(6) . . ? C29 C28 N1 117.0(7) . . ? C30 C29 C28 118.7(8) . . ? C30 C29 C34 118.9(7) . . ? C28 C29 C34 122.3(6) . . ? C31 C30 C29 121.3(8) . . ? C30 C31 C32 121.0(7) . . ? C31 C32 C33 118.9(9) . . ? C28 C33 C32 119.5(8) . . ? C28 C33 C37 123.6(6) . . ? C32 C33 C37 116.8(8) . . ? C29 C34 C36 110.9(8) . . ? C29 C34 C35 113.6(8) . . ? C36 C34 C35 108.3(8) . . ? C38 C37 C39 113.3(10) . . ? C38 C37 C33 111.8(7) . . ? C39 C37 C33 111.7(8) . . ? C45 C40 C41 119.7(9) . . ? C42 C41 C40 119.9(9) . . ? C41 C42 C43 120.7(8) . . ? C44 C43 C42 120.8(9) . . ? C43 C44 C45 117.4(8) . . ? C43 C44 P2 122.5(6) . . ? C45 C44 P2 120.1(5) . . ? C40 C45 C44 121.4(8) . . ? C51 C46 C47 118.1(7) . . ? C51 C46 P2 120.3(5) . . ? C47 C46 P2 121.5(6) . . ? C48 C47 C46 120.2(8) . . ? C47 C48 C49 120.3(8) . . ? C50 C49 C48 119.9(9) . . ? C49 C50 C51 120.2(9) . . ? C50 C51 C46 121.2(7) . . ? C53 C52 C57 118.3(7) . . ? C53 C52 P2 121.3(7) . . ? C57 C52 P2 120.4(7) . . ? C52 C53 C54 121.5(9) . . ? C55 C54 C53 118.5(10) . . ? C54 C55 C56 121.2(9) . . ? C55 C56 C57 120.0(10) . . ? C56 C57 C52 120.6(9) . . ? Cl1 C58 Cl2 114.3(8) . . ? Cl4 C59 Cl3 128(2) . . ? _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 23.59 _diffrn_measured_fraction_theta_full 0.964 _refine_diff_density_max 0.919 _refine_diff_density_min -1.082 _refine_diff_density_rms 0.104 #===end data_NiBr2((C6H3i-Pr2)NC(Me)CH2PPh2(NC6H3i-Pr2)) _database_code_CSD 211496 _audit_creation_method SHELXL-97 _chemical_formula_sum 'C46 H57 Br2 N2 Ni O0 P' _chemical_formula_weight 887.44 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.932(7) _cell_length_b 13.976(7) _cell_length_c 23.942(12) _cell_angle_alpha 90.00 _cell_angle_beta 105.303(9) _cell_angle_gamma 90.00 _cell_volume 4497(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 50.0 _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.24 _exptl_crystal_density_diffrn 1.311 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1840 _exptl_absorpt_coefficient_mu 2.276 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.143924 _exptl_absorpt_correction_T_max 0.256582 _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 18638 _diffrn_reflns_av_R_equivalents 0.0482 _diffrn_reflns_av_sigmaI/netI 0.0660 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 23.29 _reflns_number_total 6404 _reflns_number_gt 3965 _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^)+(0.0354P)^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 6404 _refine_ls_number_parameters 457 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0782 _refine_ls_R_factor_gt 0.0369 _refine_ls_wR_factor_ref 0.0823 _refine_ls_wR_factor_gt 0.0747 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.000 _refine_ls_shift/su_max 0.034 _refine_ls_shift/su_mean 0.002 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 0.23533(4) 0.75439(4) 0.233883(19) 0.03857(15) Uani 1 1 d . . . Br1 Br 0.12857(4) 0.82609(4) 0.28179(2) 0.07508(18) Uani 1 1 d . . . Br2 Br 0.37778(4) 0.84628(3) 0.22508(2) 0.07052(17) Uani 1 1 d . . . P1 P 0.21789(7) 0.62333(7) 0.12619(4) 0.0338(3) Uani 1 1 d . . . N1 N 0.1616(2) 0.6997(2) 0.15637(11) 0.0318(7) Uani 1 1 d . . . N2 N 0.3118(2) 0.6347(2) 0.26807(12) 0.0357(8) Uani 1 1 d . . . C1 C 0.1712(3) 0.5015(3) 0.11622(15) 0.0403(10) Uani 1 1 d . . . C2 C 0.1689(4) 0.4483(3) 0.06667(18) 0.0671(14) Uani 1 1 d . . . H2A H 0.1844 0.4774 0.0353 0.080 Uiso 1 1 calc R . . C3 C 0.1437(4) 0.3526(4) 0.0639(2) 0.0912(18) Uani 1 1 d . . . H3A H 0.1419 0.3185 0.0303 0.109 Uiso 1 1 calc R . . C4 C 0.1214(4) 0.3071(3) 0.1089(2) 0.0807(16) Uani 1 1 d . . . H4A H 0.1051 0.2424 0.1064 0.097 Uiso 1 1 calc R . . C5 C 0.1232(3) 0.3575(3) 0.1579(2) 0.0634(13) Uani 1 1 d . . . H5A H 0.1079 0.3270 0.1890 0.076 Uiso 1 1 calc R . . C6 C 0.1475(3) 0.4539(3) 0.16171(17) 0.0505(11) Uani 1 1 d . . . H6A H 0.1480 0.4874 0.1954 0.061 Uiso 1 1 calc R . . C7 C 0.2341(3) 0.6572(3) 0.05659(14) 0.0359(10) Uani 1 1 d . . . C8 C 0.3271(3) 0.6761(3) 0.04819(17) 0.0537(12) Uani 1 1 d . . . H8A H 0.3834 0.6737 0.0794 0.064 Uiso 1 1 calc R . . C9 C 0.3364(4) 0.6987(3) -0.00674(19) 0.0667(14) Uani 1 1 d . . . H9A H 0.3989 0.7118 -0.0120 0.080 Uiso 1 1 calc R . . C10 C 0.2546(4) 0.7018(3) -0.05299(19) 0.0645(14) Uani 1 1 d . . . H10A H 0.2617 0.7153 -0.0897 0.077 Uiso 1 1 calc R . . C11 C 0.1615(4) 0.6848(3) -0.04534(17) 0.0566(12) Uani 1 1 d . . . H11A H 0.1058 0.6888 -0.0768 0.068 Uiso 1 1 calc R . . C12 C 0.1504(3) 0.6620(3) 0.00902(16) 0.0491(11) Uani 1 1 d . . . H12A H 0.0874 0.6499 0.0138 0.059 Uiso 1 1 calc R . . C13 C 0.0702(3) 0.7455(3) 0.12151(13) 0.0320(9) Uani 1 1 d . . . C14 C 0.0759(3) 0.8310(3) 0.09069(15) 0.0384(10) Uani 1 1 d . . . C15 C -0.0110(3) 0.8697(3) 0.05553(16) 0.0504(11) Uani 1 1 d . . . H15A H -0.0069 0.9245 0.0343 0.060 Uiso 1 1 calc R . . C16 C -0.1030(3) 0.8296(3) 0.05112(17) 0.0500(11) Uani 1 1 d . . . H16A H -0.1600 0.8556 0.0264 0.060 Uiso 1 1 calc R . . C17 C -0.1087(3) 0.7501(3) 0.08405(15) 0.0448(10) Uani 1 1 d . . . H17A H -0.1709 0.7242 0.0825 0.054 Uiso 1 1 calc R . . C18 C -0.0241(3) 0.7072(3) 0.11970(15) 0.0349(9) Uani 1 1 d . . . C19 C 0.1725(3) 0.8879(3) 0.09840(16) 0.0476(11) Uani 1 1 d . . . H19A H 0.2275 0.8475 0.1198 0.057 Uiso 1 1 calc R . . C20 C 0.1689(3) 0.9770(3) 0.13555(18) 0.0650(13) Uani 1 1 d . . . H20A H 0.1563 0.9578 0.1715 0.098 Uiso 1 1 calc R . . H20B H 0.1166 1.0187 0.1151 0.098 Uiso 1 1 calc R . . H20C H 0.2314 1.0100 0.1432 0.098 Uiso 1 1 calc R . . C21 C 0.1955(3) 0.9176(3) 0.04162(18) 0.0697(14) Uani 1 1 d . . . H21A H 0.1987 0.8617 0.0189 0.105 Uiso 1 1 calc R . . H21B H 0.2582 0.9505 0.0501 0.105 Uiso 1 1 calc R . . H21C H 0.1439 0.9593 0.0203 0.105 Uiso 1 1 calc R . . C22 C -0.0392(3) 0.6208(3) 0.15485(16) 0.0459(11) Uani 1 1 d . . . H22A H 0.0263 0.5997 0.1781 0.055 Uiso 1 1 calc R . . C23 C -0.0871(3) 0.5372(3) 0.11550(18) 0.0655(13) Uani 1 1 d . . . H23A H -0.0465 0.5210 0.0901 0.098 Uiso 1 1 calc R . . H23B H -0.1522 0.5556 0.0929 0.098 Uiso 1 1 calc R . . H23C H -0.0926 0.4827 0.1389 0.098 Uiso 1 1 calc R . . C24 C -0.1019(3) 0.6478(4) 0.19669(18) 0.0708(14) Uani 1 1 d . . . H24A H -0.0701 0.6993 0.2213 0.106 Uiso 1 1 calc R . . H24B H -0.1078 0.5934 0.2200 0.106 Uiso 1 1 calc R . . H24C H -0.1670 0.6678 0.1749 0.106 Uiso 1 1 calc R . . C25 C 0.3406(3) 0.6085(3) 0.17419(14) 0.0381(10) Uani 1 1 d . . . H25A H 0.3757 0.5612 0.1574 0.046 Uiso 1 1 calc R . . H25B H 0.3760 0.6686 0.1756 0.046 Uiso 1 1 calc R . . C26 C 0.3466(3) 0.5783(3) 0.23570(15) 0.0383(10) Uani 1 1 d . . . C27 C 0.3982(3) 0.4838(3) 0.25479(16) 0.0609(13) Uani 1 1 d . . . H27A H 0.3971 0.4706 0.2940 0.091 Uiso 1 1 calc R . . H27B H 0.4659 0.4874 0.2526 0.091 Uiso 1 1 calc R . . H27C H 0.3643 0.4336 0.2299 0.091 Uiso 1 1 calc R . . C28 C 0.3319(3) 0.6116(3) 0.32995(15) 0.0399(10) Uani 1 1 d . . . C29 C 0.2591(3) 0.5709(3) 0.35190(16) 0.0443(11) Uani 1 1 d . . . C30 C 0.2843(4) 0.5467(3) 0.41058(18) 0.0619(13) Uani 1 1 d . . . H30A H 0.2373 0.5175 0.4262 0.074 Uiso 1 1 calc R . . C31 C 0.3776(4) 0.5654(4) 0.44554(19) 0.0720(15) Uani 1 1 d . . . H31A H 0.3929 0.5483 0.4844 0.086 Uiso 1 1 calc R . . C32 C 0.4490(4) 0.6090(3) 0.42401(18) 0.0650(14) Uani 1 1 d . . . H32A H 0.5117 0.6212 0.4485 0.078 Uiso 1 1 calc R . . C33 C 0.4277(3) 0.6352(3) 0.36546(16) 0.0482(11) Uani 1 1 d . . . C34 C 0.0744(3) 0.5864(4) 0.34191(19) 0.0862(17) Uani 1 1 d . . . H34A H 0.0824 0.6543 0.3470 0.129 Uiso 1 1 calc R . . H34B H 0.0798 0.5568 0.3788 0.129 Uiso 1 1 calc R . . H34C H 0.0101 0.5729 0.3164 0.129 Uiso 1 1 calc R . . C35 C 0.1427(4) 0.4384(3) 0.30596(18) 0.0870(17) Uani 1 1 d . . . H35A H 0.1932 0.4147 0.2889 0.130 Uiso 1 1 calc R . . H35B H 0.0782 0.4255 0.2805 0.130 Uiso 1 1 calc R . . H35C H 0.1486 0.4071 0.3424 0.130 Uiso 1 1 calc R . . C36 C 0.1558(3) 0.5467(3) 0.31562(17) 0.0551(12) Uani 1 1 d . . . H36A H 0.1472 0.5768 0.2776 0.066 Uiso 1 1 calc R . . C37 C 0.5080(3) 0.6878(4) 0.34535(18) 0.0616(13) Uani 1 1 d . . . H37A H 0.4837 0.6966 0.3034 0.074 Uiso 1 1 calc R . . C38 C 0.6056(3) 0.6300(4) 0.3572(2) 0.0973(19) Uani 1 1 d . . . H38A H 0.5925 0.5683 0.3391 0.146 Uiso 1 1 calc R . . H38B H 0.6323 0.6220 0.3982 0.146 Uiso 1 1 calc R . . H38C H 0.6528 0.6637 0.3416 0.146 Uiso 1 1 calc R . . C39 C 0.5275(4) 0.7865(4) 0.3728(2) 0.0990(19) Uani 1 1 d . . . H39A H 0.4664 0.8221 0.3646 0.148 Uiso 1 1 calc R . . H39B H 0.5749 0.8197 0.3572 0.148 Uiso 1 1 calc R . . H39C H 0.5535 0.7800 0.4139 0.148 Uiso 1 1 calc R . . C40 C 0.5841(11) 0.8106(11) 0.1031(7) 0.356(10) Uani 1 1 d . . . H40A H 0.5843 0.8163 0.0632 0.534 Uiso 1 1 calc R . . H40B H 0.6356 0.8503 0.1264 0.534 Uiso 1 1 calc R . . H40C H 0.5207 0.8307 0.1077 0.534 Uiso 1 1 calc R . . C41 C 0.6223(5) 0.5770(11) 0.0754(5) 0.409(16) Uani 1 1 d G . . H41A H 0.6279 0.5418 0.0435 0.491 Uiso 1 1 calc R . . C42 C 0.6290(5) 0.5314(5) 0.1279(7) 0.406(15) Uani 1 1 d G . . H42A H 0.6390 0.4656 0.1310 0.487 Uiso 1 1 calc R . . C43 C 0.6207(5) 0.5841(10) 0.1756(4) 0.325(12) Uani 1 1 d G . . H43A H 0.6251 0.5535 0.2107 0.390 Uiso 1 1 calc R . . C44 C 0.6057(4) 0.6824(9) 0.1709(4) 0.168(4) Uani 1 1 d G . . H44A H 0.6001 0.7176 0.2028 0.201 Uiso 1 1 calc R . . C45 C 0.5990(4) 0.7280(5) 0.1184(6) 0.198(7) Uani 1 1 d G . . C46 C 0.6074(5) 0.6753(11) 0.0707(3) 0.228(8) Uani 1 1 d G . . H46A H 0.6029 0.7059 0.0356 0.273 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 0.0414(3) 0.0325(3) 0.0407(3) -0.0039(2) 0.0089(2) 0.0026(3) Br1 0.0870(4) 0.0815(4) 0.0664(3) -0.0098(3) 0.0373(3) 0.0246(3) Br2 0.0547(3) 0.0542(3) 0.0930(4) 0.0096(3) 0.0024(3) -0.0179(3) P1 0.0348(6) 0.0350(6) 0.0331(5) 0.0000(5) 0.0114(5) 0.0017(5) N1 0.0276(18) 0.0334(18) 0.0345(17) -0.0011(14) 0.0085(15) 0.0026(16) N2 0.039(2) 0.038(2) 0.0313(17) 0.0023(15) 0.0106(15) 0.0052(17) C1 0.047(3) 0.037(2) 0.037(2) -0.002(2) 0.011(2) 0.003(2) C2 0.107(4) 0.048(3) 0.049(3) -0.010(2) 0.025(3) -0.006(3) C3 0.153(6) 0.053(4) 0.075(4) -0.030(3) 0.043(4) -0.018(4) C4 0.117(5) 0.041(3) 0.086(4) -0.016(3) 0.030(4) -0.018(3) C5 0.075(4) 0.049(3) 0.071(3) 0.004(3) 0.027(3) -0.007(3) C6 0.062(3) 0.038(3) 0.055(3) -0.006(2) 0.022(2) -0.001(2) C7 0.041(3) 0.037(2) 0.031(2) -0.0007(18) 0.011(2) 0.004(2) C8 0.048(3) 0.073(3) 0.042(2) 0.005(2) 0.015(2) 0.000(3) C9 0.065(4) 0.090(4) 0.056(3) 0.013(3) 0.036(3) -0.003(3) C10 0.092(4) 0.069(3) 0.040(3) 0.008(2) 0.028(3) 0.003(3) C11 0.074(4) 0.053(3) 0.038(3) 0.004(2) 0.006(2) -0.004(3) C12 0.052(3) 0.053(3) 0.043(3) 0.000(2) 0.013(2) -0.009(2) C13 0.035(2) 0.032(2) 0.0299(19) -0.0021(19) 0.0104(18) 0.001(2) C14 0.041(3) 0.037(2) 0.039(2) 0.000(2) 0.013(2) 0.003(2) C15 0.055(3) 0.043(3) 0.050(3) 0.012(2) 0.009(2) 0.010(3) C16 0.042(3) 0.049(3) 0.049(3) -0.001(2) -0.006(2) 0.011(3) C17 0.035(2) 0.049(3) 0.049(2) -0.009(2) 0.009(2) -0.002(3) C18 0.034(3) 0.037(2) 0.034(2) -0.0056(19) 0.009(2) -0.002(2) C19 0.047(3) 0.041(3) 0.058(3) 0.011(2) 0.019(2) 0.004(2) C20 0.061(3) 0.051(3) 0.087(3) -0.009(3) 0.025(3) -0.012(3) C21 0.077(4) 0.064(3) 0.082(3) 0.024(3) 0.045(3) 0.005(3) C22 0.036(3) 0.051(3) 0.049(2) 0.005(2) 0.008(2) -0.004(2) C23 0.067(3) 0.049(3) 0.079(3) 0.005(3) 0.015(3) -0.017(3) C24 0.063(3) 0.095(4) 0.062(3) 0.011(3) 0.031(3) -0.007(3) C25 0.037(2) 0.040(2) 0.039(2) 0.0001(19) 0.013(2) 0.009(2) C26 0.035(2) 0.041(3) 0.038(2) 0.003(2) 0.009(2) 0.004(2) C27 0.076(3) 0.055(3) 0.051(2) 0.006(2) 0.013(2) 0.028(3) C28 0.048(3) 0.039(2) 0.030(2) -0.0010(19) 0.006(2) 0.012(2) C29 0.050(3) 0.048(3) 0.038(2) 0.004(2) 0.016(2) 0.003(2) C30 0.075(4) 0.071(3) 0.042(3) 0.008(2) 0.019(3) 0.002(3) C31 0.092(4) 0.084(4) 0.036(3) 0.010(3) 0.011(3) 0.017(4) C32 0.063(3) 0.080(4) 0.042(3) -0.003(3) -0.002(3) 0.011(3) C33 0.045(3) 0.058(3) 0.039(3) -0.002(2) 0.008(2) 0.014(2) C34 0.062(3) 0.131(5) 0.073(3) 0.020(3) 0.031(3) -0.004(3) C35 0.125(5) 0.072(4) 0.059(3) 0.006(3) 0.016(3) -0.036(4) C36 0.062(3) 0.067(3) 0.040(2) 0.012(2) 0.020(2) -0.015(3) C37 0.043(3) 0.084(4) 0.053(3) -0.002(3) 0.004(2) 0.002(3) C38 0.052(3) 0.135(5) 0.102(4) 0.002(4) 0.016(3) 0.014(4) C39 0.121(5) 0.088(4) 0.083(4) -0.022(3) 0.019(4) -0.028(4) C40 0.291(18) 0.29(2) 0.45(3) 0.003(18) 0.031(16) -0.108(17) C41 0.040(6) 0.206(16) 0.94(5) 0.00(2) 0.048(14) -0.003(9) C42 0.119(11) 0.270(18) 0.85(4) 0.00(3) 0.16(2) -0.036(11) C43 0.069(7) 0.314(19) 0.60(3) 0.32(2) 0.095(11) 0.040(10) C44 0.068(5) 0.236(13) 0.195(9) 0.057(8) 0.026(6) -0.002(7) C45 0.076(6) 0.166(11) 0.337(18) 0.133(14) 0.026(10) 0.011(7) C46 0.042(5) 0.41(3) 0.213(10) -0.034(13) -0.001(6) 0.013(10) _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 2.019(3) . ? Ni1 N2 2.036(3) . ? Ni1 Br1 2.3309(10) . ? Ni1 Br2 2.4193(11) . ? P1 N1 1.605(3) . ? P1 C7 1.803(4) . ? P1 C25 1.803(4) . ? P1 C1 1.816(4) . ? N1 C13 1.473(4) . ? N2 C26 1.286(4) . ? N2 C28 1.469(4) . ? C1 C6 1.388(5) . ? C1 C2 1.393(5) . ? C2 C3 1.379(6) . ? C3 C4 1.357(6) . ? C4 C5 1.363(6) . ? C5 C6 1.387(6) . ? C7 C8 1.388(5) . ? C7 C12 1.400(5) . ? C8 C9 1.391(5) . ? C9 C10 1.364(6) . ? C10 C11 1.377(6) . ? C11 C12 1.388(5) . ? C13 C18 1.408(5) . ? C13 C14 1.418(5) . ? C14 C15 1.389(5) . ? C14 C19 1.532(5) . ? C15 C16 1.378(5) . ? C16 C17 1.377(5) . ? C17 C18 1.396(5) . ? C18 C22 1.518(5) . ? C19 C21 1.533(5) . ? C19 C20 1.538(5) . ? C22 C23 1.538(5) . ? C22 C24 1.540(5) . ? C25 C26 1.513(5) . ? C26 C27 1.515(5) . ? C28 C29 1.383(5) . ? C28 C33 1.419(5) . ? C29 C30 1.397(5) . ? C29 C36 1.510(5) . ? C30 C31 1.373(6) . ? C31 C32 1.377(6) . ? C32 C33 1.403(5) . ? C33 C37 1.518(6) . ? C34 C36 1.538(6) . ? C35 C36 1.535(6) . ? C37 C39 1.521(6) . ? C37 C38 1.543(6) . ? C40 C45 1.212(14) . ? C41 C42 1.3900 . ? C41 C46 1.3900 . ? C42 C43 1.3900 . ? C43 C44 1.3900 . ? C44 C45 1.3900 . ? C45 C46 1.3900 . ? 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 98.26(12) . . ? N1 Ni1 Br1 112.29(9) . . ? N2 Ni1 Br1 119.33(9) . . ? N1 Ni1 Br2 110.53(8) . . ? N2 Ni1 Br2 96.71(9) . . ? Br1 Ni1 Br2 117.35(4) . . ? N1 P1 C7 115.88(16) . . ? N1 P1 C25 106.46(16) . . ? C7 P1 C25 106.88(17) . . ? N1 P1 C1 118.85(17) . . ? C7 P1 C1 104.63(17) . . ? C25 P1 C1 102.86(18) . . ? C13 N1 P1 119.1(2) . . ? C13 N1 Ni1 120.7(2) . . ? P1 N1 Ni1 118.39(16) . . ? C26 N2 C28 118.2(3) . . ? C26 N2 Ni1 120.1(2) . . ? C28 N2 Ni1 121.7(2) . . ? C6 C1 C2 117.1(4) . . ? C6 C1 P1 119.8(3) . . ? C2 C1 P1 122.6(3) . . ? C3 C2 C1 120.5(4) . . ? C4 C3 C2 121.6(4) . . ? C3 C4 C5 119.1(5) . . ? C4 C5 C6 120.5(4) . . ? C5 C6 C1 121.2(4) . . ? C8 C7 C12 118.8(3) . . ? C8 C7 P1 122.2(3) . . ? C12 C7 P1 119.0(3) . . ? C7 C8 C9 120.2(4) . . ? C10 C9 C8 120.6(4) . . ? C9 C10 C11 120.0(4) . . ? C10 C11 C12 120.4(4) . . ? C11 C12 C7 119.9(4) . . ? C18 C13 C14 119.0(3) . . ? C18 C13 N1 120.9(3) . . ? C14 C13 N1 120.1(3) . . ? C15 C14 C13 118.9(4) . . ? C15 C14 C19 117.9(4) . . ? C13 C14 C19 122.9(3) . . ? C16 C15 C14 122.2(4) . . ? C17 C16 C15 118.5(4) . . ? C16 C17 C18 122.0(4) . . ? C17 C18 C13 119.1(3) . . ? C17 C18 C22 117.5(4) . . ? C13 C18 C22 123.4(3) . . ? C14 C19 C21 114.6(3) . . ? C14 C19 C20 109.1(3) . . ? C21 C19 C20 109.9(3) . . ? C18 C22 C23 111.5(3) . . ? C18 C22 C24 110.5(3) . . ? C23 C22 C24 110.8(3) . . ? C26 C25 P1 116.8(3) . . ? N2 C26 C25 118.9(3) . . ? N2 C26 C27 125.2(3) . . ? C25 C26 C27 115.9(3) . . ? C29 C28 C33 122.5(3) . . ? C29 C28 N2 120.7(4) . . ? C33 C28 N2 116.9(3) . . ? C28 C29 C30 117.8(4) . . ? C28 C29 C36 123.9(3) . . ? C30 C29 C36 118.2(4) . . ? C31 C30 C29 120.9(4) . . ? C30 C31 C32 121.2(4) . . ? C31 C32 C33 120.4(4) . . ? C32 C33 C28 117.1(4) . . ? C32 C33 C37 117.7(4) . . ? C28 C33 C37 125.3(3) . . ? C29 C36 C35 111.3(4) . . ? C29 C36 C34 112.2(3) . . ? C35 C36 C34 110.3(4) . . ? C33 C37 C39 111.4(4) . . ? C33 C37 C38 112.1(4) . . ? C39 C37 C38 110.3(4) . . ? C42 C41 C46 120.0 . . ? C41 C42 C43 120.0 . . ? C42 C43 C44 120.0 . . ? C45 C44 C43 120.0 . . ? C40 C45 C46 107.5(13) . . ? C40 C45 C44 132.4(13) . . ? C46 C45 C44 120.0 . . ? C45 C46 C41 120.0 . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 23.29 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.549 _refine_diff_density_min -0.467 _refine_diff_density_rms 0.059 #===end