Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'P Braunstein' 'Anthony Kermagoret' _publ_contact_author_name 'P. Braunstein' _publ_contact_author_address ; Laboratoire de Chimie de Coordn. UMR 7177 CNRS Universite Louis Pasteur 4 rue Blaise Pascal Strasbourg Cedex 67070 FRANCE ; _publ_contact_author_email BRAUNSTEIN@CHIMIE.U-STRASBG.FR _publ_requested_journal 'Dalton Transactions' _publ_section_title ; SHOP-type nickel complexes with alkyl substituents on phosphorus, synthesis and catalytic ethylene oligomerization ; data_shelxl _database_code_depnum_ccdc_archive 'CCDC 659315' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C45 H38 Ni O2 P2' _chemical_formula_sum 'C45 H38 Ni O2 P2' _chemical_formula_weight 731.40 _chemical_absolute_configuration . loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.61300(10) _cell_length_b 13.4690(2) _cell_length_c 14.0310(3) _cell_angle_alpha 76.3300(8) _cell_angle_beta 82.2130(8) _cell_angle_gamma 74.8470(12) _cell_volume 1875.29(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6336 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 30.034 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.295 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 764 _exptl_absorpt_coefficient_mu 0.639 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15910 _diffrn_reflns_av_R_equivalents 0.0210 _diffrn_reflns_av_sigmaI/netI 0.0520 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 30.01 _reflns_number_total 10885 _reflns_number_gt 8098 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo (Nonius B.V., 1998)' _computing_data_reduction 'Denzo (Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON 98 (Spek, 1998)' _computing_publication_material '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^)+(0.0376P)^2^+0.4901P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10885 _refine_ls_number_parameters 451 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0628 _refine_ls_R_factor_gt 0.0392 _refine_ls_wR_factor_ref 0.0993 _refine_ls_wR_factor_gt 0.0895 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni Ni 0.026008(17) 0.271400(16) 0.747235(13) 0.02164(6) Uani 1 1 d . . . P1 P -0.08958(4) 0.27790(3) 0.62468(3) 0.02224(9) Uani 1 1 d . . . P2 P 0.14695(4) 0.24427(3) 0.86780(3) 0.02151(9) Uani 1 1 d . . . O1 O 0.14359(11) 0.14944(10) 0.71289(8) 0.0307(3) Uani 1 1 d . . . O2 O 0.39532(13) -0.08658(11) 0.89357(11) 0.0467(3) Uani 1 1 d . . . C1 C 0.25894(15) 0.12600(13) 0.85035(12) 0.0266(3) Uani 1 1 d . . . H1 H 0.3273 0.0892 0.8920 0.032 Uiso 1 1 calc . . . C2 C 0.23650(14) 0.09342(13) 0.77069(11) 0.0250(3) Uani 1 1 d . . . C3 C 0.31014(15) -0.00613(14) 0.73926(13) 0.0299(4) Uani 1 1 d . . . C4 C 0.29835(19) -0.01342(17) 0.64315(15) 0.0433(5) Uani 1 1 d . . . H4 H 0.2494 0.0455 0.6004 0.052 Uiso 1 1 calc . . . C5 C 0.3564(2) -0.1044(2) 0.60881(19) 0.0611(6) Uani 1 1 d . . . H5 H 0.3472 -0.1075 0.5432 0.073 Uiso 1 1 calc . . . C6 C 0.4273(2) -0.1902(2) 0.6698(2) 0.0661(7) Uani 1 1 d . . . H6 H 0.4665 -0.2528 0.6465 0.079 Uiso 1 1 calc . . . C7 C 0.4417(2) -0.18577(17) 0.7643(2) 0.0538(6) Uani 1 1 d . . . H7 H 0.4911 -0.2454 0.8059 0.065 Uiso 1 1 calc . . . C8 C 0.38454(16) -0.09466(15) 0.79987(15) 0.0373(4) Uani 1 1 d . . . C9 C 0.4585(3) -0.1774(2) 0.9607(2) 0.0879(10) Uani 1 1 d . . . H9A H 0.4128 -0.2335 0.9677 0.132 Uiso 1 1 calc . . . H9B H 0.4566 -0.1598 1.0249 0.132 Uiso 1 1 calc . . . H9C H 0.5496 -0.2012 0.9356 0.132 Uiso 1 1 calc . . . C10 C -0.09623(14) 0.38366(13) 0.79173(11) 0.0241(3) Uani 1 1 d . . . C11 C -0.19344(16) 0.36242(14) 0.86714(12) 0.0304(4) Uani 1 1 d . . . H11 H -0.1967 0.2914 0.8939 0.036 Uiso 1 1 calc . . . C12 C -0.28441(18) 0.44154(17) 0.90358(14) 0.0411(4) Uani 1 1 d . . . H12 H -0.3489 0.4241 0.9543 0.049 Uiso 1 1 calc . . . C13 C -0.2820(2) 0.54458(17) 0.86698(16) 0.0464(5) Uani 1 1 d . . . H13 H -0.3434 0.5986 0.8931 0.056 Uiso 1 1 calc . . . C14 C -0.1907(2) 0.56959(15) 0.79244(17) 0.0463(5) Uani 1 1 d . . . H14 H -0.1898 0.6412 0.7662 0.056 Uiso 1 1 calc . . . C15 C -0.09778(18) 0.48933(15) 0.75441(14) 0.0363(4) Uani 1 1 d . . . H15 H -0.0353 0.5078 0.7025 0.044 Uiso 1 1 calc . . . C16 C 0.06902(14) 0.21653(13) 0.99190(11) 0.0248(3) Uani 1 1 d . . . C17 C -0.00551(17) 0.14173(14) 1.00947(12) 0.0315(4) Uani 1 1 d . . . H17 H -0.0111 0.1082 0.9583 0.038 Uiso 1 1 calc . . . C18 C -0.07131(17) 0.11570(15) 1.10026(13) 0.0368(4) Uani 1 1 d . . . H18 H -0.1218 0.0648 1.1111 0.044 Uiso 1 1 calc . . . C19 C -0.06348(19) 0.16382(17) 1.17502(13) 0.0403(4) Uani 1 1 d . . . H19 H -0.1094 0.1467 1.2373 0.048 Uiso 1 1 calc . . . C20 C 0.0111(2) 0.23686(17) 1.15933(13) 0.0410(4) Uani 1 1 d . . . H20 H 0.0174 0.2691 1.2113 0.049 Uiso 1 1 calc . . . C21 C 0.07736(17) 0.26374(15) 1.06795(12) 0.0326(4) Uani 1 1 d . . . H21 H 0.1282 0.3144 1.0577 0.039 Uiso 1 1 calc . . . C22 C 0.23695(15) 0.34298(13) 0.86405(11) 0.0248(3) Uani 1 1 d . . . C23 C 0.37096(16) 0.32081(15) 0.83560(12) 0.0320(4) Uani 1 1 d . . . H23 H 0.4149 0.2533 0.8236 0.038 Uiso 1 1 calc . . . C24 C 0.43990(19) 0.39823(19) 0.82491(15) 0.0447(5) Uani 1 1 d . . . H24 H 0.5313 0.3830 0.8065 0.054 Uiso 1 1 calc . . . C25 C 0.3771(2) 0.49591(18) 0.84076(16) 0.0503(6) Uani 1 1 d . . . H25 H 0.4249 0.5483 0.8328 0.060 Uiso 1 1 calc . . . C26 C 0.2444(2) 0.51899(16) 0.86826(15) 0.0438(5) Uani 1 1 d . . . H26 H 0.2013 0.5872 0.8789 0.053 Uiso 1 1 calc . . . C27 C 0.17397(17) 0.44260(14) 0.88030(13) 0.0327(4) Uani 1 1 d . . . H27 H 0.0829 0.4584 0.8996 0.039 Uiso 1 1 calc . . . C28 C 0.01719(16) 0.22273(14) 0.52729(11) 0.0282(3) Uani 1 1 d . . . C29 C 0.13207(18) 0.25736(16) 0.49764(14) 0.0389(4) Uani 1 1 d . . . H29 H 0.1500 0.3085 0.5269 0.047 Uiso 1 1 calc . . . C30 C 0.2196(2) 0.2176(2) 0.42606(16) 0.0534(6) Uani 1 1 d . . . H30 H 0.2974 0.2419 0.4058 0.064 Uiso 1 1 calc . . . C31 C 0.1950(2) 0.1430(2) 0.38381(15) 0.0585(6) Uani 1 1 d . . . H31 H 0.2564 0.1150 0.3354 0.070 Uiso 1 1 calc . . . C32 C 0.0822(3) 0.10895(17) 0.41136(15) 0.0532(6) Uani 1 1 d . . . H32 H 0.0652 0.0579 0.3815 0.064 Uiso 1 1 calc . . . C33 C -0.00830(19) 0.14899(15) 0.48335(13) 0.0385(4) Uani 1 1 d . . . H33 H -0.0869 0.1257 0.5020 0.046 Uiso 1 1 calc . . . C34 C -0.20144(15) 0.19202(13) 0.67293(12) 0.0269(3) Uani 1 1 d . . . C35 C -0.16660(17) 0.11140(15) 0.75430(13) 0.0345(4) Uani 1 1 d . . . H35 H -0.0849 0.1007 0.7804 0.041 Uiso 1 1 calc . . . C36 C -0.2500(2) 0.04640(16) 0.79765(14) 0.0424(5) Uani 1 1 d . . . H36 H -0.2251 -0.0087 0.8529 0.051 Uiso 1 1 calc . . . C37 C -0.36910(18) 0.06173(16) 0.76052(16) 0.0430(5) Uani 1 1 d . . . H37 H -0.4272 0.0184 0.7912 0.052 Uiso 1 1 calc . . . C38 C -0.40373(17) 0.14020(17) 0.67863(16) 0.0446(5) Uani 1 1 d . . . H38 H -0.4847 0.1494 0.6520 0.053 Uiso 1 1 calc . . . C39 C -0.32101(17) 0.20576(15) 0.63500(14) 0.0367(4) Uani 1 1 d . . . H39 H -0.3460 0.2601 0.5792 0.044 Uiso 1 1 calc . . . C40 C -0.19351(15) 0.39783(13) 0.55815(12) 0.0266(3) Uani 1 1 d . . . C41 C -0.17304(18) 0.43181(17) 0.45667(13) 0.0401(4) Uani 1 1 d . . . H41 H -0.1030 0.3926 0.4209 0.048 Uiso 1 1 calc . . . C42 C -0.2543(2) 0.52235(19) 0.40777(15) 0.0515(6) Uani 1 1 d . . . H42 H -0.2390 0.5452 0.3387 0.062 Uiso 1 1 calc . . . C43 C -0.3564(2) 0.57928(17) 0.45804(16) 0.0480(5) Uani 1 1 d . . . H43 H -0.4118 0.6413 0.4240 0.058 Uiso 1 1 calc . . . C44 C -0.37861(18) 0.54620(16) 0.55838(16) 0.0424(5) Uani 1 1 d . . . H44 H -0.4504 0.5849 0.5932 0.051 Uiso 1 1 calc . . . C45 C -0.29675(17) 0.45704(15) 0.60846(13) 0.0336(4) Uani 1 1 d . . . H45 H -0.3111 0.4360 0.6778 0.040 Uiso 1 1 calc . . . 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 Ni 0.02006(10) 0.02277(11) 0.02143(10) -0.00572(8) -0.00350(7) -0.00202(8) P1 0.02090(18) 0.0249(2) 0.02043(19) -0.00447(15) -0.00289(14) -0.00427(15) P2 0.02145(18) 0.0214(2) 0.02157(19) -0.00446(15) -0.00405(14) -0.00387(15) O1 0.0284(6) 0.0315(7) 0.0305(6) -0.0128(5) -0.0091(5) 0.0049(5) O2 0.0487(8) 0.0257(7) 0.0580(9) 0.0008(6) -0.0183(7) 0.0033(6) C1 0.0235(7) 0.0230(8) 0.0314(8) -0.0049(6) -0.0065(6) -0.0005(6) C2 0.0206(7) 0.0219(8) 0.0301(8) -0.0051(6) 0.0005(6) -0.0026(6) C3 0.0214(7) 0.0259(9) 0.0428(10) -0.0124(7) 0.0018(7) -0.0040(6) C4 0.0410(10) 0.0434(12) 0.0478(11) -0.0237(9) 0.0029(8) -0.0044(9) C5 0.0585(14) 0.0619(17) 0.0703(16) -0.0446(14) 0.0067(12) -0.0055(12) C6 0.0473(13) 0.0491(15) 0.107(2) -0.0485(15) 0.0083(13) 0.0017(11) C7 0.0385(11) 0.0300(11) 0.0905(18) -0.0190(11) -0.0065(11) 0.0027(8) C8 0.0251(8) 0.0264(9) 0.0587(12) -0.0096(8) -0.0021(8) -0.0035(7) C9 0.116(2) 0.0410(15) 0.084(2) 0.0073(14) -0.0399(18) 0.0203(15) C10 0.0227(7) 0.0249(8) 0.0264(8) -0.0077(6) -0.0070(6) -0.0038(6) C11 0.0278(8) 0.0316(9) 0.0292(8) -0.0077(7) -0.0042(6) -0.0006(7) C12 0.0328(9) 0.0487(13) 0.0384(10) -0.0174(9) -0.0016(8) 0.0030(8) C13 0.0424(11) 0.0432(12) 0.0541(12) -0.0265(10) -0.0141(9) 0.0086(9) C14 0.0578(12) 0.0213(9) 0.0632(13) -0.0086(9) -0.0294(11) -0.0033(9) C15 0.0372(9) 0.0282(10) 0.0444(10) -0.0037(8) -0.0089(8) -0.0099(8) C16 0.0242(7) 0.0242(8) 0.0233(7) -0.0020(6) -0.0035(6) -0.0032(6) C17 0.0365(9) 0.0309(10) 0.0294(8) -0.0058(7) -0.0048(7) -0.0111(7) C18 0.0354(9) 0.0361(11) 0.0372(10) -0.0001(8) 0.0008(7) -0.0139(8) C19 0.0414(10) 0.0458(12) 0.0293(9) -0.0023(8) 0.0057(7) -0.0120(9) C20 0.0521(11) 0.0484(12) 0.0260(9) -0.0122(8) 0.0020(8) -0.0165(10) C21 0.0371(9) 0.0360(10) 0.0283(8) -0.0081(7) -0.0026(7) -0.0138(8) C22 0.0288(8) 0.0250(8) 0.0211(7) -0.0017(6) -0.0072(6) -0.0074(6) C23 0.0301(8) 0.0371(10) 0.0296(8) -0.0050(7) -0.0037(7) -0.0103(7) C24 0.0378(10) 0.0579(14) 0.0439(11) -0.0067(10) 0.0000(8) -0.0261(10) C25 0.0611(13) 0.0480(14) 0.0513(12) -0.0007(10) -0.0122(10) -0.0344(11) C26 0.0601(13) 0.0278(10) 0.0476(11) -0.0062(8) -0.0174(10) -0.0125(9) C27 0.0377(9) 0.0291(9) 0.0330(9) -0.0070(7) -0.0089(7) -0.0075(7) C28 0.0313(8) 0.0297(9) 0.0214(7) -0.0061(6) -0.0017(6) -0.0030(7) C29 0.0354(9) 0.0449(12) 0.0362(10) -0.0125(8) 0.0045(7) -0.0096(8) C30 0.0477(12) 0.0629(16) 0.0425(11) -0.0133(11) 0.0169(9) -0.0092(11) C31 0.0741(15) 0.0511(14) 0.0339(11) -0.0112(10) 0.0180(10) 0.0043(12) C32 0.0916(17) 0.0336(12) 0.0326(10) -0.0140(9) 0.0003(11) -0.0084(11) C33 0.0534(11) 0.0335(10) 0.0289(9) -0.0082(8) -0.0032(8) -0.0096(9) C34 0.0247(7) 0.0279(9) 0.0293(8) -0.0093(7) -0.0002(6) -0.0061(6) C35 0.0356(9) 0.0335(10) 0.0354(9) -0.0035(7) -0.0056(7) -0.0118(8) C36 0.0477(11) 0.0350(11) 0.0426(11) -0.0008(8) 0.0015(9) -0.0158(9) C37 0.0369(10) 0.0358(11) 0.0592(12) -0.0146(9) 0.0129(9) -0.0176(8) C38 0.0252(8) 0.0451(12) 0.0675(14) -0.0157(10) -0.0033(8) -0.0122(8) C39 0.0287(8) 0.0370(11) 0.0442(10) -0.0063(8) -0.0077(7) -0.0071(8) C40 0.0245(7) 0.0270(9) 0.0277(8) -0.0022(6) -0.0072(6) -0.0058(6) C41 0.0365(9) 0.0444(12) 0.0304(9) 0.0011(8) -0.0034(7) -0.0014(8) C42 0.0473(11) 0.0547(14) 0.0387(11) 0.0124(10) -0.0118(9) -0.0036(10) C43 0.0433(11) 0.0359(11) 0.0570(13) 0.0059(10) -0.0212(10) -0.0013(9) C44 0.0333(9) 0.0354(11) 0.0562(12) -0.0136(9) -0.0108(8) 0.0033(8) C45 0.0328(9) 0.0342(10) 0.0321(9) -0.0070(7) -0.0055(7) -0.0037(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni C10 1.8869(16) . ? Ni O1 1.9046(12) . ? Ni P2 2.1665(4) . ? Ni P1 2.2167(4) . ? P1 C28 1.8231(17) . ? P1 C40 1.8253(16) . ? P1 C34 1.8265(16) . ? P2 C1 1.7680(17) . ? P2 C22 1.8167(16) . ? P2 C16 1.8218(15) . ? O1 C2 1.3182(19) . ? O2 C8 1.367(2) . ? O2 C9 1.425(3) . ? C1 C2 1.363(2) . ? C1 H1 0.9500 . ? C2 C3 1.497(2) . ? C3 C4 1.400(3) . ? C3 C8 1.407(2) . ? C4 C5 1.385(3) . ? C4 H4 0.9500 . ? C5 C6 1.373(4) . ? C5 H5 0.9500 . ? C6 C7 1.372(4) . ? C6 H6 0.9500 . ? C7 C8 1.393(3) . ? C7 H7 0.9500 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C15 1.392(2) . ? C10 C11 1.408(2) . ? C11 C12 1.384(2) . ? C11 H11 0.9500 . ? C12 C13 1.367(3) . ? C12 H12 0.9500 . ? C13 C14 1.370(3) . ? C13 H13 0.9500 . ? C14 C15 1.414(3) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C21 1.388(2) . ? C16 C17 1.396(2) . ? C17 C18 1.382(2) . ? C17 H17 0.9500 . ? C18 C19 1.379(3) . ? C18 H18 0.9500 . ? C19 C20 1.379(3) . ? C19 H19 0.9500 . ? C20 C21 1.392(2) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 C27 1.390(2) . ? C22 C23 1.397(2) . ? C23 C24 1.393(3) . ? C23 H23 0.9500 . ? C24 C25 1.366(3) . ? C24 H24 0.9500 . ? C25 C26 1.381(3) . ? C25 H25 0.9500 . ? C26 C27 1.390(3) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 C33 1.384(2) . ? C28 C29 1.395(2) . ? C29 C30 1.378(3) . ? C29 H29 0.9500 . ? C30 C31 1.376(3) . ? C30 H30 0.9500 . ? C31 C32 1.367(3) . ? C31 H31 0.9500 . ? C32 C33 1.399(3) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 C35 1.392(2) . ? C34 C39 1.393(2) . ? C35 C36 1.389(2) . ? C35 H35 0.9500 . ? C36 C37 1.379(3) . ? C36 H36 0.9500 . ? C37 C38 1.382(3) . ? C37 H37 0.9500 . ? C38 C39 1.389(3) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 C45 1.391(2) . ? C40 C41 1.394(2) . ? C41 C42 1.384(3) . ? C41 H41 0.9500 . ? C42 C43 1.369(3) . ? C42 H42 0.9500 . ? C43 C44 1.380(3) . ? C43 H43 0.9500 . ? C44 C45 1.383(3) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? 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 C10 Ni O1 174.58(6) . . ? C10 Ni P2 92.36(5) . . ? O1 Ni P2 85.78(3) . . ? C10 Ni P1 93.67(5) . . ? O1 Ni P1 87.88(3) . . ? P2 Ni P1 172.899(18) . . ? C28 P1 C40 103.54(7) . . ? C28 P1 C34 106.48(8) . . ? C40 P1 C34 103.82(7) . . ? C28 P1 Ni 110.21(5) . . ? C40 P1 Ni 124.52(6) . . ? C34 P1 Ni 106.98(5) . . ? C1 P2 C22 109.12(7) . . ? C1 P2 C16 106.45(7) . . ? C22 P2 C16 107.15(7) . . ? C1 P2 Ni 99.92(5) . . ? C22 P2 Ni 116.43(5) . . ? C16 P2 Ni 116.93(5) . . ? C2 O1 Ni 119.95(10) . . ? C8 O2 C9 118.95(18) . . ? C2 C1 P2 112.62(11) . . ? C2 C1 H1 123.7 . . ? P2 C1 H1 123.7 . . ? O1 C2 C1 121.42(15) . . ? O1 C2 C3 113.08(14) . . ? C1 C2 C3 125.50(14) . . ? C4 C3 C8 117.47(17) . . ? C4 C3 C2 117.11(16) . . ? C8 C3 C2 125.34(16) . . ? C5 C4 C3 121.6(2) . . ? C5 C4 H4 119.2 . . ? C3 C4 H4 119.2 . . ? C6 C5 C4 119.8(2) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? C7 C6 C5 120.3(2) . . ? C7 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? C6 C7 C8 120.7(2) . . ? C6 C7 H7 119.7 . . ? C8 C7 H7 119.7 . . ? O2 C8 C7 122.86(18) . . ? O2 C8 C3 116.92(16) . . ? C7 C8 C3 120.21(19) . . ? O2 C9 H9A 109.5 . . ? O2 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? O2 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C15 C10 C11 116.18(16) . . ? C15 C10 Ni 124.05(13) . . ? C11 C10 Ni 119.76(12) . . ? C12 C11 C10 122.24(17) . . ? C12 C11 H11 118.9 . . ? C10 C11 H11 118.9 . . ? C13 C12 C11 120.34(18) . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C12 C13 C14 119.72(18) . . ? C12 C13 H13 120.1 . . ? C14 C13 H13 120.1 . . ? C13 C14 C15 120.32(18) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C10 C15 C14 121.16(17) . . ? C10 C15 H15 119.4 . . ? C14 C15 H15 119.4 . . ? C21 C16 C17 118.71(14) . . ? C21 C16 P2 125.54(12) . . ? C17 C16 P2 115.74(12) . . ? C18 C17 C16 120.98(16) . . ? C18 C17 H17 119.5 . . ? C16 C17 H17 119.5 . . ? C19 C18 C17 119.86(16) . . ? C19 C18 H18 120.1 . . ? C17 C18 H18 120.1 . . ? C18 C19 C20 119.92(16) . . ? C18 C19 H19 120.0 . . ? C20 C19 H19 120.0 . . ? C19 C20 C21 120.54(17) . . ? C19 C20 H20 119.7 . . ? C21 C20 H20 119.7 . . ? C16 C21 C20 119.97(16) . . ? C16 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C27 C22 C23 119.41(15) . . ? C27 C22 P2 121.65(12) . . ? C23 C22 P2 118.70(13) . . ? C24 C23 C22 119.68(18) . . ? C24 C23 H23 120.2 . . ? C22 C23 H23 120.2 . . ? C25 C24 C23 120.46(18) . . ? C25 C24 H24 119.8 . . ? C23 C24 H24 119.8 . . ? C24 C25 C26 120.40(17) . . ? C24 C25 H25 119.8 . . ? C26 C25 H25 119.8 . . ? C25 C26 C27 120.10(19) . . ? C25 C26 H26 120.0 . . ? C27 C26 H26 120.0 . . ? C26 C27 C22 119.96(17) . . ? C26 C27 H27 120.0 . . ? C22 C27 H27 120.0 . . ? C33 C28 C29 119.26(16) . . ? C33 C28 P1 124.17(13) . . ? C29 C28 P1 116.57(14) . . ? C30 C29 C28 120.22(19) . . ? C30 C29 H29 119.9 . . ? C28 C29 H29 119.9 . . ? C31 C30 C29 120.3(2) . . ? C31 C30 H30 119.8 . . ? C29 C30 H30 119.8 . . ? C32 C31 C30 120.19(19) . . ? C32 C31 H31 119.9 . . ? C30 C31 H31 119.9 . . ? C31 C32 C33 120.3(2) . . ? C31 C32 H32 119.9 . . ? C33 C32 H32 119.9 . . ? C28 C33 C32 119.72(18) . . ? C28 C33 H33 120.1 . . ? C32 C33 H33 120.1 . . ? C35 C34 C39 118.86(15) . . ? C35 C34 P1 117.65(12) . . ? C39 C34 P1 123.45(13) . . ? C36 C35 C34 120.66(16) . . ? C36 C35 H35 119.7 . . ? C34 C35 H35 119.7 . . ? C37 C36 C35 120.03(18) . . ? C37 C36 H36 120.0 . . ? C35 C36 H36 120.0 . . ? C36 C37 C38 119.86(16) . . ? C36 C37 H37 120.1 . . ? C38 C37 H37 120.1 . . ? C37 C38 C39 120.45(17) . . ? C37 C38 H38 119.8 . . ? C39 C38 H38 119.8 . . ? C38 C39 C34 120.12(17) . . ? C38 C39 H39 119.9 . . ? C34 C39 H39 119.9 . . ? C45 C40 C41 118.44(16) . . ? C45 C40 P1 120.07(12) . . ? C41 C40 P1 121.48(14) . . ? C42 C41 C40 120.35(18) . . ? C42 C41 H41 119.8 . . ? C40 C41 H41 119.8 . . ? C43 C42 C41 120.60(18) . . ? C43 C42 H42 119.7 . . ? C41 C42 H42 119.7 . . ? C42 C43 C44 119.73(18) . . ? C42 C43 H43 120.1 . . ? C44 C43 H43 120.1 . . ? C43 C44 C45 120.29(19) . . ? C43 C44 H44 119.9 . . ? C45 C44 H44 119.9 . . ? C44 C45 C40 120.56(17) . . ? C44 C45 H45 119.7 . . ? C40 C45 H45 119.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C10 Ni P1 C28 155.56(8) . . . . ? O1 Ni P1 C28 -29.65(7) . . . . ? P2 Ni P1 C28 -56.41(15) . . . . ? C10 Ni P1 C40 31.79(8) . . . . ? O1 Ni P1 C40 -153.41(7) . . . . ? P2 Ni P1 C40 179.83(14) . . . . ? C10 Ni P1 C34 -89.08(7) . . . . ? O1 Ni P1 C34 85.72(7) . . . . ? P2 Ni P1 C34 58.96(15) . . . . ? C10 Ni P2 C1 171.67(7) . . . . ? O1 Ni P2 C1 -3.22(6) . . . . ? P1 Ni P2 C1 23.59(15) . . . . ? C10 Ni P2 C22 -71.06(8) . . . . ? O1 Ni P2 C22 114.04(7) . . . . ? P1 Ni P2 C22 140.86(14) . . . . ? C10 Ni P2 C16 57.39(8) . . . . ? O1 Ni P2 C16 -117.50(7) . . . . ? P1 Ni P2 C16 -90.69(15) . . . . ? C10 Ni O1 C2 -64.6(6) . . . . ? P2 Ni O1 C2 5.54(11) . . . . ? P1 Ni O1 C2 -171.26(11) . . . . ? C22 P2 C1 C2 -121.28(12) . . . . ? C16 P2 C1 C2 123.39(12) . . . . ? Ni P2 C1 C2 1.32(12) . . . . ? Ni O1 C2 C1 -6.3(2) . . . . ? Ni O1 C2 C3 173.38(10) . . . . ? P2 C1 C2 O1 2.7(2) . . . . ? P2 C1 C2 C3 -176.94(12) . . . . ? O1 C2 C3 C4 16.9(2) . . . . ? C1 C2 C3 C4 -163.36(16) . . . . ? O1 C2 C3 C8 -159.62(15) . . . . ? C1 C2 C3 C8 20.1(2) . . . . ? C8 C3 C4 C5 0.6(3) . . . . ? C2 C3 C4 C5 -176.22(18) . . . . ? C3 C4 C5 C6 0.1(3) . . . . ? C4 C5 C6 C7 -0.5(4) . . . . ? C5 C6 C7 C8 0.2(4) . . . . ? C9 O2 C8 C7 -5.2(3) . . . . ? C9 O2 C8 C3 173.8(2) . . . . ? C6 C7 C8 O2 179.56(19) . . . . ? C6 C7 C8 C3 0.6(3) . . . . ? C4 C3 C8 O2 -179.99(16) . . . . ? C2 C3 C8 O2 -3.4(2) . . . . ? C4 C3 C8 C7 -1.0(3) . . . . ? C2 C3 C8 C7 175.60(16) . . . . ? O1 Ni C10 C15 168.1(5) . . . . ? P2 Ni C10 C15 98.27(14) . . . . ? P1 Ni C10 C15 -85.49(14) . . . . ? O1 Ni C10 C11 -12.0(6) . . . . ? P2 Ni C10 C11 -81.81(12) . . . . ? P1 Ni C10 C11 94.44(12) . . . . ? C15 C10 C11 C12 -1.0(2) . . . . ? Ni C10 C11 C12 179.08(13) . . . . ? C10 C11 C12 C13 -0.3(3) . . . . ? C11 C12 C13 C14 1.4(3) . . . . ? C12 C13 C14 C15 -1.0(3) . . . . ? C11 C10 C15 C14 1.3(2) . . . . ? Ni C10 C15 C14 -178.76(13) . . . . ? C13 C14 C15 C10 -0.3(3) . . . . ? C1 P2 C16 C21 117.16(15) . . . . ? C22 P2 C16 C21 0.51(17) . . . . ? Ni P2 C16 C21 -132.27(13) . . . . ? C1 P2 C16 C17 -63.37(14) . . . . ? C22 P2 C16 C17 179.99(13) . . . . ? Ni P2 C16 C17 47.20(14) . . . . ? C21 C16 C17 C18 0.8(3) . . . . ? P2 C16 C17 C18 -178.73(14) . . . . ? C16 C17 C18 C19 -0.1(3) . . . . ? C17 C18 C19 C20 -0.7(3) . . . . ? C18 C19 C20 C21 0.9(3) . . . . ? C17 C16 C21 C20 -0.6(3) . . . . ? P2 C16 C21 C20 178.89(15) . . . . ? C19 C20 C21 C16 -0.3(3) . . . . ? C1 P2 C22 C27 -176.96(13) . . . . ? C16 P2 C22 C27 -62.09(14) . . . . ? Ni P2 C22 C27 70.97(14) . . . . ? C1 P2 C22 C23 8.75(15) . . . . ? C16 P2 C22 C23 123.61(13) . . . . ? Ni P2 C22 C23 -103.33(12) . . . . ? C27 C22 C23 C24 0.7(2) . . . . ? P2 C22 C23 C24 175.10(14) . . . . ? C22 C23 C24 C25 -0.9(3) . . . . ? C23 C24 C25 C26 0.4(3) . . . . ? C24 C25 C26 C27 0.2(3) . . . . ? C25 C26 C27 C22 -0.4(3) . . . . ? C23 C22 C27 C26 0.0(2) . . . . ? P2 C22 C27 C26 -174.30(14) . . . . ? C40 P1 C28 C33 -93.28(16) . . . . ? C34 P1 C28 C33 15.83(17) . . . . ? Ni P1 C28 C33 131.52(14) . . . . ? C40 P1 C28 C29 87.67(15) . . . . ? C34 P1 C28 C29 -163.23(14) . . . . ? Ni P1 C28 C29 -47.54(15) . . . . ? C33 C28 C29 C30 -0.7(3) . . . . ? P1 C28 C29 C30 178.45(16) . . . . ? C28 C29 C30 C31 -0.5(3) . . . . ? C29 C30 C31 C32 1.1(4) . . . . ? C30 C31 C32 C33 -0.6(3) . . . . ? C29 C28 C33 C32 1.1(3) . . . . ? P1 C28 C33 C32 -177.89(15) . . . . ? C31 C32 C33 C28 -0.5(3) . . . . ? C28 P1 C34 C35 93.63(15) . . . . ? C40 P1 C34 C35 -157.46(14) . . . . ? Ni P1 C34 C35 -24.20(15) . . . . ? C28 P1 C34 C39 -88.95(17) . . . . ? C40 P1 C34 C39 19.96(17) . . . . ? Ni P1 C34 C39 153.22(14) . . . . ? C39 C34 C35 C36 -0.7(3) . . . . ? P1 C34 C35 C36 176.88(15) . . . . ? C34 C35 C36 C37 -0.4(3) . . . . ? C35 C36 C37 C38 1.6(3) . . . . ? C36 C37 C38 C39 -1.8(3) . . . . ? C37 C38 C39 C34 0.8(3) . . . . ? C35 C34 C39 C38 0.5(3) . . . . ? P1 C34 C39 C38 -176.92(15) . . . . ? C28 P1 C40 C45 174.22(14) . . . . ? C34 P1 C40 C45 63.14(15) . . . . ? Ni P1 C40 C45 -59.15(15) . . . . ? C28 P1 C40 C41 -5.09(16) . . . . ? C34 P1 C40 C41 -116.17(15) . . . . ? Ni P1 C40 C41 121.55(14) . . . . ? C45 C40 C41 C42 -0.1(3) . . . . ? P1 C40 C41 C42 179.19(16) . . . . ? C40 C41 C42 C43 -0.6(3) . . . . ? C41 C42 C43 C44 0.1(3) . . . . ? C42 C43 C44 C45 1.2(3) . . . . ? C43 C44 C45 C40 -1.9(3) . . . . ? C41 C40 C45 C44 1.4(3) . . . . ? P1 C40 C45 C44 -177.96(14) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 30.01 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.648 _refine_diff_density_min -0.402 _refine_diff_density_rms 0.060