# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 222 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Mary Rakowski DuBois' 'Morris Bullock' 'William G. Dougherty' 'Daniel DuBois' 'W. Scott Kassel' 'Brendan Twamley' 'Jenny Y. Yang' _publ_contact_author_name 'Mary Rakowski DuBois' _publ_contact_author_email MARY.RAKOWSKIDUBOIS@PNL.GOV _publ_section_title ; Reduction of Oxygen Catalyzed by Nickel Diphosphine Complexes with Positioned Pendant Amines ; # Attachment 'Complex_6.cif' data_pnl020 _database_code_depnum_ccdc_archive 'CCDC 751449' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H24 N2 Ni0.50 P2' _chemical_formula_weight 359.69 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 9.7763(2) _cell_length_b 19.7795(4) _cell_length_c 19.0291(3) _cell_angle_alpha 90.00 _cell_angle_beta 101.1210(10) _cell_angle_gamma 90.00 _cell_volume 3610.57(12) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7853 _cell_measurement_theta_min 4.47 _cell_measurement_theta_max 68.55 _exptl_crystal_description blade _exptl_crystal_colour yellow _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.323 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1520 _exptl_absorpt_coefficient_mu 2.685 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7370 _exptl_absorpt_correction_T_max 0.8642 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 10592 _diffrn_reflns_av_R_equivalents 0.0201 _diffrn_reflns_av_sigmaI/netI 0.0205 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 4.47 _diffrn_reflns_theta_max 69.10 _reflns_number_total 3181 _reflns_number_gt 2971 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0514P)^2^+3.2409P] 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 3181 _refine_ls_number_parameters 206 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0317 _refine_ls_R_factor_gt 0.0297 _refine_ls_wR_factor_ref 0.0804 _refine_ls_wR_factor_gt 0.0787 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.0000 0.291691(17) 0.2500 0.01380(12) Uani 1 2 d S . . N1 N 0.04996(15) 0.22782(7) 0.07301(7) 0.0197(3) Uani 1 1 d . . . N2 N 0.25515(13) 0.35957(7) 0.17533(7) 0.0171(3) Uani 1 1 d . . . P1 P 0.16220(4) 0.234944(19) 0.217864(19) 0.01451(12) Uani 1 1 d . . . P2 P -0.03202(4) 0.336634(19) 0.146621(19) 0.01406(11) Uani 1 1 d . . . C1 C 0.37418(17) 0.19737(9) 0.33183(9) 0.0220(3) Uani 1 1 d . . . H1A H 0.3764 0.2442 0.3432 0.026 Uiso 1 1 calc R . . C2 C 0.46493(18) 0.15329(9) 0.37467(9) 0.0261(4) Uani 1 1 d . . . H2A H 0.5300 0.1703 0.4144 0.031 Uiso 1 1 calc R . . C3 C 0.46101(19) 0.08476(10) 0.35979(10) 0.0297(4) Uani 1 1 d . . . H3A H 0.5230 0.0547 0.3891 0.036 Uiso 1 1 calc R . . C4 C 0.3663(2) 0.06043(10) 0.30188(10) 0.0332(4) Uani 1 1 d . . . H4A H 0.3626 0.0134 0.2916 0.040 Uiso 1 1 calc R . . C5 C 0.2762(2) 0.10459(9) 0.25863(9) 0.0273(4) Uani 1 1 d . . . H5A H 0.2112 0.0872 0.2191 0.033 Uiso 1 1 calc R . . C6 C 0.27975(16) 0.17380(8) 0.27226(8) 0.0182(3) Uani 1 1 d . . . C7 C 0.09706(17) 0.18438(8) 0.13545(8) 0.0195(3) Uani 1 1 d . . . H7A H 0.1725 0.1544 0.1259 0.023 Uiso 1 1 calc R . . H7B H 0.0187 0.1555 0.1434 0.023 Uiso 1 1 calc R . . C8 C 0.0252(2) 0.18665(9) 0.00809(9) 0.0306(4) Uani 1 1 d . . . H8A H 0.1101 0.1615 0.0047 0.046 Uiso 1 1 calc R . . H8B H -0.0004 0.2160 -0.0339 0.046 Uiso 1 1 calc R . . H8C H -0.0508 0.1548 0.0098 0.046 Uiso 1 1 calc R . . C9 C -0.07166(17) 0.27010(8) 0.07602(8) 0.0191(3) Uani 1 1 d . . . H9A H -0.1485 0.2412 0.0859 0.023 Uiso 1 1 calc R . . H9B H -0.1034 0.2920 0.0289 0.023 Uiso 1 1 calc R . . C10 C 0.29318(16) 0.28778(8) 0.18284(8) 0.0184(3) Uani 1 1 d . . . H10A H 0.3845 0.2836 0.2157 0.022 Uiso 1 1 calc R . . H10B H 0.3037 0.2700 0.1355 0.022 Uiso 1 1 calc R . . C11 C 0.37023(17) 0.39869(8) 0.15728(8) 0.0213(3) Uani 1 1 d . . . H11A H 0.4559 0.3887 0.1918 0.032 Uiso 1 1 calc R . . H11B H 0.3492 0.4470 0.1589 0.032 Uiso 1 1 calc R . . H11C H 0.3828 0.3866 0.1090 0.032 Uiso 1 1 calc R . . C12 C 0.12834(16) 0.37322(8) 0.12185(8) 0.0163(3) Uani 1 1 d . . . H12A H 0.1398 0.3542 0.0752 0.020 Uiso 1 1 calc R . . H12B H 0.1164 0.4227 0.1160 0.020 Uiso 1 1 calc R . . C13 C -0.16234(18) 0.42867(8) 0.03929(9) 0.0237(4) Uani 1 1 d . . . H13A H -0.1015 0.4115 0.0102 0.028 Uiso 1 1 calc R . . C14 C -0.25425(19) 0.48044(9) 0.01378(10) 0.0291(4) Uani 1 1 d . . . H14A H -0.2557 0.4989 -0.0324 0.035 Uiso 1 1 calc R . . C15 C -0.34438(18) 0.50527(9) 0.05601(11) 0.0295(4) Uani 1 1 d . . . H15A H -0.4068 0.5410 0.0388 0.035 Uiso 1 1 calc R . . C16 C -0.34321(17) 0.47794(8) 0.12294(10) 0.0262(4) Uani 1 1 d . . . H16A H -0.4062 0.4944 0.1512 0.031 Uiso 1 1 calc R . . C17 C -0.25003(16) 0.42620(8) 0.14939(9) 0.0209(3) Uani 1 1 d . . . H17A H -0.2491 0.4079 0.1956 0.025 Uiso 1 1 calc R . . C18 C -0.15865(16) 0.40156(8) 0.10771(8) 0.0177(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0139(2) 0.0152(2) 0.01237(19) 0.000 0.00257(14) 0.000 N1 0.0268(7) 0.0170(7) 0.0147(6) -0.0022(5) 0.0027(5) 0.0034(5) N2 0.0153(6) 0.0196(7) 0.0163(6) 0.0014(5) 0.0029(5) -0.0015(5) P1 0.0149(2) 0.0150(2) 0.0134(2) 0.00026(13) 0.00216(14) 0.00159(14) P2 0.0146(2) 0.0145(2) 0.01275(19) 0.00060(13) 0.00180(14) 0.00110(13) C1 0.0221(8) 0.0216(8) 0.0222(8) 0.0025(6) 0.0037(6) 0.0009(6) C2 0.0200(8) 0.0332(10) 0.0235(9) 0.0067(7) 0.0004(6) 0.0004(7) C3 0.0298(9) 0.0317(10) 0.0277(9) 0.0112(7) 0.0055(7) 0.0124(8) C4 0.0493(12) 0.0210(9) 0.0284(9) 0.0035(7) 0.0055(8) 0.0087(8) C5 0.0352(10) 0.0223(9) 0.0225(8) 0.0010(7) 0.0005(7) 0.0028(7) C6 0.0174(7) 0.0207(8) 0.0175(8) 0.0032(6) 0.0057(6) 0.0036(6) C7 0.0244(8) 0.0167(8) 0.0166(7) -0.0010(6) 0.0018(6) 0.0019(6) C8 0.0500(12) 0.0224(9) 0.0169(8) -0.0029(7) 0.0005(7) 0.0088(8) C9 0.0208(8) 0.0179(8) 0.0166(8) -0.0016(6) -0.0009(6) 0.0002(6) C10 0.0158(8) 0.0214(8) 0.0185(8) 0.0027(6) 0.0046(6) 0.0014(6) C11 0.0192(8) 0.0254(9) 0.0197(8) 0.0023(6) 0.0043(6) -0.0039(6) C12 0.0176(7) 0.0164(8) 0.0156(7) 0.0020(5) 0.0044(6) 0.0000(6) C13 0.0260(9) 0.0229(9) 0.0204(8) 0.0019(6) -0.0001(6) 0.0002(7) C14 0.0328(10) 0.0221(9) 0.0267(9) 0.0067(7) -0.0086(7) -0.0025(7) C15 0.0203(8) 0.0160(8) 0.0453(11) 0.0013(7) -0.0107(7) 0.0005(6) C16 0.0168(8) 0.0178(8) 0.0424(10) -0.0058(7) 0.0021(7) 0.0000(6) C17 0.0173(8) 0.0186(8) 0.0262(8) -0.0015(6) 0.0025(6) -0.0015(6) C18 0.0159(7) 0.0156(8) 0.0200(8) 0.0006(6) -0.0006(6) -0.0006(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 P2 2.1262(4) . ? Ni1 P2 2.1262(4) 2 ? Ni1 P1 2.1266(4) . ? Ni1 P1 2.1266(4) 2 ? N1 C8 1.460(2) . ? N1 C9 1.464(2) . ? N1 C7 1.467(2) . ? N2 C11 1.460(2) . ? N2 C10 1.468(2) . ? N2 C12 1.4693(19) . ? P1 C6 1.8428(16) . ? P1 C7 1.8654(16) . ? P1 C10 1.8723(16) . ? P2 C18 1.8375(15) . ? P2 C9 1.8671(16) . ? P2 C12 1.8679(15) . ? C1 C2 1.390(2) . ? C1 C6 1.397(2) . ? C2 C3 1.384(3) . ? C3 C4 1.382(3) . ? C4 C5 1.391(3) . ? C5 C6 1.392(2) . ? C13 C14 1.387(2) . ? C13 C18 1.402(2) . ? C14 C15 1.392(3) . ? C15 C16 1.381(3) . ? C16 C17 1.398(2) . ? C17 C18 1.392(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 P2 Ni1 P2 130.57(3) . 2 ? P2 Ni1 P1 86.532(14) . . ? P2 Ni1 P1 120.121(14) 2 . ? P2 Ni1 P1 120.123(14) . 2 ? P2 Ni1 P1 86.532(14) 2 2 ? P1 Ni1 P1 116.29(3) . 2 ? C8 N1 C9 110.38(13) . . ? C8 N1 C7 109.49(12) . . ? C9 N1 C7 115.69(13) . . ? C11 N2 C10 110.08(12) . . ? C11 N2 C12 108.98(12) . . ? C10 N2 C12 114.15(12) . . ? C6 P1 C7 101.25(7) . . ? C6 P1 C10 99.85(7) . . ? C7 P1 C10 98.40(7) . . ? C6 P1 Ni1 127.13(5) . . ? C7 P1 Ni1 111.84(5) . . ? C10 P1 Ni1 114.01(5) . . ? C18 P2 C9 99.93(7) . . ? C18 P2 C12 99.24(7) . . ? C9 P2 C12 99.16(7) . . ? C18 P2 Ni1 129.24(5) . . ? C9 P2 Ni1 110.13(5) . . ? C12 P2 Ni1 114.49(5) . . ? C2 C1 C6 120.91(16) . . ? C3 C2 C1 120.33(16) . . ? C2 C3 C4 119.48(16) . . ? C3 C4 C5 120.22(17) . . ? C6 C5 C4 121.13(17) . . ? C5 C6 C1 117.90(15) . . ? C5 C6 P1 123.39(13) . . ? C1 C6 P1 118.67(12) . . ? N1 C7 P1 111.72(11) . . ? N1 C9 P2 111.93(10) . . ? N2 C10 P1 113.38(10) . . ? N2 C12 P2 113.02(10) . . ? C14 C13 C18 120.42(16) . . ? C13 C14 C15 119.87(17) . . ? C16 C15 C14 120.05(15) . . ? C15 C16 C17 120.49(16) . . ? C18 C17 C16 119.76(16) . . ? C17 C18 C13 119.39(15) . . ? C17 C18 P2 118.14(12) . . ? C13 C18 P2 122.42(12) . . ? 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 P2 Ni1 P1 C6 177.86(7) . . . . ? P2 Ni1 P1 C6 41.95(7) 2 . . . ? P1 Ni1 P1 C6 -60.08(7) 2 . . . ? P2 Ni1 P1 C7 -57.58(6) . . . . ? P2 Ni1 P1 C7 166.51(6) 2 . . . ? P1 Ni1 P1 C7 64.48(6) 2 . . . ? P2 Ni1 P1 C10 52.95(6) . . . . ? P2 Ni1 P1 C10 -82.95(6) 2 . . . ? P1 Ni1 P1 C10 175.01(6) 2 . . . ? P2 Ni1 P2 C18 -51.87(6) 2 . . . ? P1 Ni1 P2 C18 -179.46(7) . . . . ? P1 Ni1 P2 C18 62.00(7) 2 . . . ? P2 Ni1 P2 C9 -174.32(6) 2 . . . ? P1 Ni1 P2 C9 58.10(6) . . . . ? P1 Ni1 P2 C9 -60.44(6) 2 . . . ? P2 Ni1 P2 C12 74.99(5) 2 . . . ? P1 Ni1 P2 C12 -52.60(6) . . . . ? P1 Ni1 P2 C12 -171.14(5) 2 . . . ? C6 C1 C2 C3 -1.4(3) . . . . ? C1 C2 C3 C4 0.1(3) . . . . ? C2 C3 C4 C5 0.4(3) . . . . ? C3 C4 C5 C6 0.3(3) . . . . ? C4 C5 C6 C1 -1.6(3) . . . . ? C4 C5 C6 P1 -179.23(14) . . . . ? C2 C1 C6 C5 2.1(2) . . . . ? C2 C1 C6 P1 179.90(13) . . . . ? C7 P1 C6 C5 -16.99(16) . . . . ? C10 P1 C6 C5 -117.69(15) . . . . ? Ni1 P1 C6 C5 111.80(13) . . . . ? C7 P1 C6 C1 165.37(12) . . . . ? C10 P1 C6 C1 64.67(13) . . . . ? Ni1 P1 C6 C1 -65.84(14) . . . . ? C8 N1 C7 P1 169.36(12) . . . . ? C9 N1 C7 P1 -65.18(15) . . . . ? C6 P1 C7 N1 -155.89(11) . . . . ? C10 P1 C7 N1 -54.01(12) . . . . ? Ni1 P1 C7 N1 66.13(12) . . . . ? C8 N1 C9 P2 -167.58(12) . . . . ? C7 N1 C9 P2 67.41(15) . . . . ? C18 P2 C9 N1 152.21(11) . . . . ? C12 P2 C9 N1 51.06(12) . . . . ? Ni1 P2 C9 N1 -69.36(11) . . . . ? C11 N2 C10 P1 172.30(10) . . . . ? C12 N2 C10 P1 -64.78(15) . . . . ? C6 P1 C10 N2 -144.97(11) . . . . ? C7 P1 C10 N2 111.98(12) . . . . ? Ni1 P1 C10 N2 -6.54(13) . . . . ? C11 N2 C12 P2 -171.13(10) . . . . ? C10 N2 C12 P2 65.35(14) . . . . ? C18 P2 C12 N2 146.51(11) . . . . ? C9 P2 C12 N2 -111.77(11) . . . . ? Ni1 P2 C12 N2 5.40(12) . . . . ? C18 C13 C14 C15 -0.6(3) . . . . ? C13 C14 C15 C16 -0.6(3) . . . . ? C14 C15 C16 C17 1.2(2) . . . . ? C15 C16 C17 C18 -0.6(2) . . . . ? C16 C17 C18 C13 -0.6(2) . . . . ? C16 C17 C18 P2 176.89(12) . . . . ? C14 C13 C18 C17 1.2(2) . . . . ? C14 C13 C18 P2 -176.16(13) . . . . ? C9 P2 C18 C17 125.83(13) . . . . ? C12 P2 C18 C17 -133.08(13) . . . . ? Ni1 P2 C18 C17 -0.62(16) . . . . ? C9 P2 C18 C13 -56.77(15) . . . . ? C12 P2 C18 C13 44.32(14) . . . . ? Ni1 P2 C18 C13 176.78(11) . . . . ? _diffrn_measured_fraction_theta_max 0.943 _diffrn_reflns_theta_full 67.00 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 0.487 _refine_diff_density_min -0.235 _refine_diff_density_rms 0.054 # Attachment 'Complex_8.cif' data_bt1146 _database_code_depnum_ccdc_archive 'CCDC 751450' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C62 H67 B2 F8 N5 Ni O4 P4' _chemical_formula_weight 1302.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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 _symmetry_space_group_name_Hall '-P 2yn' 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 24.8972(8) _cell_length_b 11.2331(3) _cell_length_c 25.3567(8) _cell_angle_alpha 90.00 _cell_angle_beta 113.3710(10) _cell_angle_gamma 90.00 _cell_volume 6509.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 9019 _cell_measurement_theta_min 2.44 _cell_measurement_theta_max 30.01 _exptl_crystal_description fragment _exptl_crystal_colour 'pale green' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.329 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2704 _exptl_absorpt_coefficient_mu 0.468 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8723 _exptl_absorpt_correction_T_max 0.9247 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(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 'Bruker/Siemens SMART APEX' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_reflns_number 69141 _diffrn_reflns_av_R_equivalents 0.0409 _diffrn_reflns_av_sigmaI/netI 0.0274 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 25.25 _reflns_number_total 11797 _reflns_number_gt 9766 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART v. 5.632 (Bruker, 2006)' _computing_cell_refinement 'SAINT+ v. 7.23a (Bruker, 2006)' _computing_data_reduction 'SAINT+ v. 7.23a (Bruker, 2006)' _computing_structure_solution 'XS, SHELXTL v. 6.14 (Bruker, 2003)' _computing_structure_refinement 'XL, SHELXTL v. 6.14 (Bruker, 2003)' _computing_molecular_graphics 'XP, SHELXTL v. 6.14 (Bruker, 2003)' _computing_publication_material 'XCIF, SHELXTL, v. 6.14 (Bruker, 2003)' _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^)+(0.0858P)^2^+2.9894P] 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 11797 _refine_ls_number_parameters 776 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0585 _refine_ls_R_factor_gt 0.0490 _refine_ls_wR_factor_ref 0.1373 _refine_ls_wR_factor_gt 0.1307 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.769399(14) 0.03243(3) 0.505662(13) 0.02240(10) Uani 1 1 d . . . B1 B 0.84830(16) 0.7250(3) 0.28993(14) 0.0382(8) Uani 1 1 d . . . B2 B 0.63116(18) 0.2974(3) 0.69236(18) 0.0479(9) Uani 1 1 d . . . F1 F 0.87137(16) 0.6145(2) 0.29595(11) 0.1234(14) Uani 1 1 d . . . F2 F 0.80539(10) 0.7344(2) 0.31132(10) 0.0744(7) Uani 1 1 d . . . F3 F 0.82434(9) 0.75108(19) 0.23245(7) 0.0595(5) Uani 1 1 d . . . F4 F 0.89139(8) 0.8076(2) 0.31839(8) 0.0569(5) Uani 1 1 d . . . F5 F 0.67539(14) 0.3145(3) 0.67299(14) 0.1212(13) Uani 1 1 d . . . F6 F 0.58333(17) 0.3746(3) 0.66556(14) 0.1234(13) Uani 1 1 d . . . F7 F 0.65173(9) 0.3161(3) 0.74968(10) 0.0883(9) Uani 1 1 d . . . F8 F 0.60927(8) 0.18765(16) 0.67705(8) 0.0513(5) Uani 1 1 d . . . N1 N 0.75715(9) 0.18557(18) 0.44978(8) 0.0235(4) Uani 1 1 d . . . N2 N 0.78491(9) 0.03666(18) 0.33713(8) 0.0224(4) Uani 1 1 d . . . N3 N 0.77926(9) -0.12434(18) 0.55942(8) 0.0232(4) Uani 1 1 d . . . N4 N 0.73530(9) 0.00527(19) 0.66389(8) 0.0225(4) Uani 1 1 d . . . N5 N 0.92294(18) 0.4041(4) 0.53686(19) 0.0926(13) Uani 1 1 d . . . O1 O 0.84897(7) 0.00279(15) 0.50243(7) 0.0245(4) Uani 1 1 d . . . O2 O 0.73367(7) -0.07039(15) 0.43316(7) 0.0244(4) Uani 1 1 d . . . O3 O 0.80222(8) 0.13087(15) 0.57988(7) 0.0261(4) Uani 1 1 d . . . O4 O 0.68780(7) 0.06354(15) 0.50453(7) 0.0257(4) Uani 1 1 d . . . P1 P 0.85559(3) 0.06862(6) 0.45326(3) 0.02216(15) Uani 1 1 d . . . P2 P 0.70074(3) -0.00086(6) 0.37912(3) 0.02273(15) Uani 1 1 d . . . P3 P 0.82674(3) 0.06049(6) 0.63487(3) 0.02302(15) Uani 1 1 d . . . P4 P 0.67444(3) -0.01620(6) 0.54579(3) 0.02201(15) Uani 1 1 d . . . C1 C 0.95018(12) 0.1711(2) 0.43605(12) 0.0323(6) Uani 1 1 d . . . H1A H 0.9250 0.1781 0.3966 0.039 Uiso 1 1 calc R . . C2 C 1.00681(13) 0.2121(3) 0.45531(13) 0.0394(7) Uani 1 1 d . . . H2A H 1.0208 0.2464 0.4289 0.047 Uiso 1 1 calc R . . C3 C 1.04367(12) 0.2039(3) 0.51284(13) 0.0392(7) Uani 1 1 d . . . H3A H 1.0827 0.2323 0.5257 0.047 Uiso 1 1 calc R . . C4 C 1.02345(12) 0.1543(3) 0.55159(12) 0.0370(7) Uani 1 1 d . . . H4A H 1.0485 0.1499 0.5912 0.044 Uiso 1 1 calc R . . C5 C 0.96683(12) 0.1113(2) 0.53262(11) 0.0306(6) Uani 1 1 d . . . H5A H 0.9532 0.0764 0.5591 0.037 Uiso 1 1 calc R . . C6 C 0.92980(11) 0.1190(2) 0.47464(11) 0.0261(5) Uani 1 1 d . . . C7 C 0.81173(11) 0.2039(2) 0.43988(10) 0.0240(5) Uani 1 1 d . . . H7A H 0.8352 0.2679 0.4655 0.029 Uiso 1 1 calc R . . H7B H 0.8013 0.2298 0.3997 0.029 Uiso 1 1 calc R . . C8 C 0.74460(12) 0.2971(2) 0.47664(11) 0.0272(6) Uani 1 1 d . . . H8A H 0.7097 0.2830 0.4853 0.033 Uiso 1 1 calc R . . H8B H 0.7781 0.3126 0.5135 0.033 Uiso 1 1 calc R . . C9 C 0.67795(14) 0.4357(3) 0.39988(13) 0.0396(7) Uani 1 1 d . . . H9A H 0.6457 0.3885 0.3983 0.048 Uiso 1 1 calc R . . C10 C 0.66845(16) 0.5328(3) 0.36309(14) 0.0487(8) Uani 1 1 d . . . H10A H 0.6300 0.5509 0.3364 0.058 Uiso 1 1 calc R . . C11 C 0.71469(16) 0.6022(3) 0.36545(13) 0.0448(8) Uani 1 1 d . . . H11A H 0.7083 0.6680 0.3402 0.054 Uiso 1 1 calc R . . C12 C 0.77025(16) 0.5763(3) 0.40443(14) 0.0441(8) Uani 1 1 d . . . H12A H 0.8022 0.6244 0.4060 0.053 Uiso 1 1 calc R . . C13 C 0.77981(13) 0.4801(2) 0.44153(13) 0.0351(6) Uani 1 1 d . . . H13A H 0.8182 0.4644 0.4690 0.042 Uiso 1 1 calc R . . C14 C 0.73402(12) 0.4068(2) 0.43901(11) 0.0291(6) Uani 1 1 d . . . C15 C 0.70514(11) 0.1579(2) 0.39605(10) 0.0243(5) Uani 1 1 d . . . H15A H 0.7076 0.2037 0.3637 0.029 Uiso 1 1 calc R . . H15B H 0.6691 0.1828 0.4007 0.029 Uiso 1 1 calc R . . C16 C 0.60710(12) -0.1500(2) 0.35913(12) 0.0316(6) Uani 1 1 d . . . H16A H 0.6351 -0.2032 0.3846 0.038 Uiso 1 1 calc R . . C17 C 0.54835(13) -0.1817(3) 0.33434(13) 0.0404(7) Uani 1 1 d . . . H17A H 0.5362 -0.2572 0.3424 0.048 Uiso 1 1 calc R . . C18 C 0.50758(12) -0.1032(3) 0.29796(13) 0.0394(7) Uani 1 1 d . . . H18A H 0.4674 -0.1250 0.2812 0.047 Uiso 1 1 calc R . . C19 C 0.52488(12) 0.0061(3) 0.28592(13) 0.0381(7) Uani 1 1 d . . . H19A H 0.4965 0.0596 0.2612 0.046 Uiso 1 1 calc R . . C20 C 0.58325(12) 0.0388(3) 0.30950(12) 0.0343(6) Uani 1 1 d . . . H20A H 0.5951 0.1140 0.3007 0.041 Uiso 1 1 calc R . . C21 C 0.62467(11) -0.0400(2) 0.34647(11) 0.0276(6) Uani 1 1 d . . . C22 C 0.72907(11) -0.0239(2) 0.32452(10) 0.0245(5) Uani 1 1 d . . . H22A H 0.7344 -0.1103 0.3206 0.029 Uiso 1 1 calc R . . H22B H 0.7000 0.0053 0.2873 0.029 Uiso 1 1 calc R . . C23 C 0.79614(11) 0.0434(2) 0.28376(10) 0.0260(5) Uani 1 1 d . . . H23A H 0.7597 0.0671 0.2512 0.031 Uiso 1 1 calc R . . H23B H 0.8076 -0.0362 0.2751 0.031 Uiso 1 1 calc R . . C24 C 0.83502(15) 0.2510(3) 0.29601(12) 0.0448(8) Uani 1 1 d . . . H24A H 0.7992 0.2773 0.2971 0.054 Uiso 1 1 calc R . . C25 C 0.87853(19) 0.3334(3) 0.30090(14) 0.0623(12) Uani 1 1 d . . . H25A H 0.8724 0.4156 0.3052 0.075 Uiso 1 1 calc R . . C26 C 0.9304(2) 0.2953(4) 0.29940(14) 0.0719(14) Uani 1 1 d . . . H26A H 0.9601 0.3514 0.3030 0.086 Uiso 1 1 calc R . . C27 C 0.93930(18) 0.1774(4) 0.29286(16) 0.0684(13) Uani 1 1 d . . . H27A H 0.9751 0.1522 0.2915 0.082 Uiso 1 1 calc R . . C28 C 0.89652(14) 0.0941(3) 0.28814(13) 0.0470(8) Uani 1 1 d . . . H28A H 0.9031 0.0120 0.2839 0.056 Uiso 1 1 calc R . . C29 C 0.84370(12) 0.1315(3) 0.28965(11) 0.0324(6) Uani 1 1 d . . . C30 C 0.83409(11) -0.0158(2) 0.38573(10) 0.0234(5) Uani 1 1 d . . . H30A H 0.8683 -0.0216 0.3753 0.028 Uiso 1 1 calc R . . H30B H 0.8233 -0.0976 0.3923 0.028 Uiso 1 1 calc R . . C31 C 0.92836(12) 0.1879(2) 0.65865(12) 0.0331(6) Uani 1 1 d . . . H31A H 0.9068 0.2302 0.6243 0.040 Uiso 1 1 calc R . . C32 C 0.98651(13) 0.2150(3) 0.69038(13) 0.0399(7) Uani 1 1 d . . . H32A H 1.0050 0.2760 0.6776 0.048 Uiso 1 1 calc R . . C33 C 1.01787(12) 0.1540(3) 0.74041(13) 0.0385(7) Uani 1 1 d . . . H33A H 1.0578 0.1735 0.7619 0.046 Uiso 1 1 calc R . . C34 C 0.99182(12) 0.0651(3) 0.75944(12) 0.0366(7) Uani 1 1 d . . . H34A H 1.0137 0.0236 0.7940 0.044 Uiso 1 1 calc R . . C35 C 0.93327(12) 0.0362(3) 0.72791(12) 0.0324(6) Uani 1 1 d . . . H35A H 0.9152 -0.0252 0.7408 0.039 Uiso 1 1 calc R . . C36 C 0.90151(11) 0.0978(2) 0.67742(11) 0.0261(5) Uani 1 1 d . . . C37 C 0.82485(10) -0.0971(2) 0.61731(10) 0.0232(5) Uani 1 1 d . . . H37A H 0.8636 -0.1213 0.6186 0.028 Uiso 1 1 calc R . . H37B H 0.8170 -0.1440 0.6465 0.028 Uiso 1 1 calc R . . C38 C 0.79866(12) -0.2321(2) 0.53553(11) 0.0269(6) Uani 1 1 d . . . H38A H 0.7681 -0.2512 0.4973 0.032 Uiso 1 1 calc R . . H38B H 0.8348 -0.2116 0.5301 0.032 Uiso 1 1 calc R . . C39 C 0.86611(17) -0.3687(3) 0.61129(16) 0.0612(10) Uani 1 1 d . . . H39A H 0.8978 -0.3197 0.6129 0.073 Uiso 1 1 calc R . . C40 C 0.8767(3) -0.4676(4) 0.64766(18) 0.0912(18) Uani 1 1 d . . . H40A H 0.9155 -0.4846 0.6740 0.109 Uiso 1 1 calc R . . C41 C 0.8318(3) -0.5396(4) 0.64549(17) 0.0831(17) Uani 1 1 d . . . H41A H 0.8391 -0.6058 0.6707 0.100 Uiso 1 1 calc R . . C42 C 0.7759(2) -0.5161(3) 0.6065(2) 0.0698(13) Uani 1 1 d . . . H42A H 0.7445 -0.5666 0.6046 0.084 Uiso 1 1 calc R . . C43 C 0.76517(16) -0.4188(3) 0.57016(15) 0.0472(8) Uani 1 1 d . . . H43A H 0.7266 -0.4044 0.5428 0.057 Uiso 1 1 calc R . . C44 C 0.81018(13) -0.3417(2) 0.57314(11) 0.0317(6) Uani 1 1 d . . . C45 C 0.72053(10) -0.1492(2) 0.55953(10) 0.0231(5) Uani 1 1 d . . . H45A H 0.7255 -0.1829 0.5973 0.028 Uiso 1 1 calc R . . H45B H 0.7005 -0.2096 0.5298 0.028 Uiso 1 1 calc R . . C46 C 0.58243(12) -0.1600(3) 0.54184(12) 0.0346(6) Uani 1 1 d . . . H46A H 0.6084 -0.1897 0.5781 0.042 Uiso 1 1 calc R . . C47 C 0.52643(13) -0.2045(3) 0.51622(14) 0.0432(7) Uani 1 1 d . . . H47A H 0.5138 -0.2651 0.5348 0.052 Uiso 1 1 calc R . . C48 C 0.48852(13) -0.1610(3) 0.46337(13) 0.0416(7) Uani 1 1 d . . . H48A H 0.4501 -0.1925 0.4456 0.050 Uiso 1 1 calc R . . C49 C 0.50633(12) -0.0722(3) 0.43646(12) 0.0387(7) Uani 1 1 d . . . H49A H 0.4799 -0.0419 0.4006 0.046 Uiso 1 1 calc R . . C50 C 0.56251(12) -0.0269(3) 0.46145(11) 0.0317(6) Uani 1 1 d . . . H50A H 0.5748 0.0338 0.4426 0.038 Uiso 1 1 calc R . . C51 C 0.60105(11) -0.0710(2) 0.51446(11) 0.0262(5) Uani 1 1 d . . . C52 C 0.68554(11) 0.0538(2) 0.61466(10) 0.0240(5) Uani 1 1 d . . . H52A H 0.6917 0.1402 0.6119 0.029 Uiso 1 1 calc R . . H52B H 0.6495 0.0438 0.6218 0.029 Uiso 1 1 calc R . . C53 C 0.71937(11) -0.0257(2) 0.71303(11) 0.0269(6) Uani 1 1 d . . . H53A H 0.7005 0.0436 0.7227 0.032 Uiso 1 1 calc R . . H53B H 0.7553 -0.0451 0.7471 0.032 Uiso 1 1 calc R . . C54 C 0.69751(12) -0.2425(2) 0.68868(11) 0.0315(6) Uani 1 1 d . . . H54A H 0.7368 -0.2524 0.6926 0.038 Uiso 1 1 calc R . . C55 C 0.65954(13) -0.3388(3) 0.67347(12) 0.0374(7) Uani 1 1 d . . . H55A H 0.6726 -0.4138 0.6660 0.045 Uiso 1 1 calc R . . C56 C 0.60253(14) -0.3259(3) 0.66919(13) 0.0424(7) Uani 1 1 d . . . H56A H 0.5766 -0.3921 0.6587 0.051 Uiso 1 1 calc R . . C57 C 0.58338(13) -0.2165(3) 0.68016(13) 0.0425(7) Uani 1 1 d . . . H57A H 0.5446 -0.2080 0.6780 0.051 Uiso 1 1 calc R . . C58 C 0.62121(12) -0.1189(3) 0.69442(12) 0.0353(6) Uani 1 1 d . . . H58A H 0.6079 -0.0438 0.7015 0.042 Uiso 1 1 calc R . . C59 C 0.67821(12) -0.1307(2) 0.69831(10) 0.0287(6) Uani 1 1 d . . . C60 C 0.78785(11) 0.0781(2) 0.68172(10) 0.0258(5) Uani 1 1 d . . . H60A H 0.8142 0.0560 0.7214 0.031 Uiso 1 1 calc R . . H60B H 0.7769 0.1628 0.6820 0.031 Uiso 1 1 calc R . . C61 C 1.0320(2) 0.4685(4) 0.5841(2) 0.0831(15) Uani 1 1 d . . . H61A H 1.0531 0.4161 0.6167 0.125 Uiso 1 1 calc R . . H61B H 1.0351 0.5510 0.5975 0.125 Uiso 1 1 calc R . . H61C H 1.0492 0.4618 0.5555 0.125 Uiso 1 1 calc R . . C62 C 0.9707(2) 0.4337(3) 0.55819(17) 0.0667(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.02808(19) 0.02438(19) 0.01619(17) 0.00204(12) 0.01032(14) 0.00394(13) B1 0.0445(19) 0.0361(18) 0.0288(17) -0.0071(14) 0.0088(15) -0.0005(15) B2 0.057(2) 0.039(2) 0.054(2) -0.0197(18) 0.029(2) -0.0104(18) F1 0.192(3) 0.0590(15) 0.0598(15) -0.0126(12) -0.0135(18) 0.0646(18) F2 0.0852(16) 0.0857(16) 0.0736(15) -0.0270(13) 0.0542(13) -0.0455(13) F3 0.0751(14) 0.0668(13) 0.0264(9) -0.0120(9) 0.0093(9) -0.0021(11) F4 0.0338(9) 0.0840(15) 0.0497(11) -0.0310(10) 0.0130(8) -0.0119(9) F5 0.142(2) 0.133(3) 0.144(3) -0.100(2) 0.115(2) -0.099(2) F6 0.199(4) 0.0699(18) 0.110(2) 0.0172(17) 0.071(2) 0.069(2) F7 0.0510(13) 0.149(3) 0.0619(14) -0.0618(16) 0.0196(11) -0.0119(14) F8 0.0580(11) 0.0447(11) 0.0611(12) -0.0219(9) 0.0340(10) -0.0200(9) N1 0.0297(11) 0.0249(11) 0.0169(10) -0.0016(8) 0.0101(9) 0.0034(9) N2 0.0251(11) 0.0266(11) 0.0151(10) 0.0002(8) 0.0075(8) 0.0013(9) N3 0.0264(11) 0.0254(11) 0.0179(10) -0.0015(8) 0.0091(9) 0.0046(9) N4 0.0226(10) 0.0306(11) 0.0147(10) 0.0012(8) 0.0079(8) 0.0025(9) N5 0.074(3) 0.083(3) 0.094(3) -0.027(2) 0.004(2) 0.023(2) O1 0.0274(9) 0.0279(9) 0.0184(8) 0.0023(7) 0.0092(7) 0.0039(7) O2 0.0292(9) 0.0258(9) 0.0187(8) 0.0006(7) 0.0100(7) 0.0031(7) O3 0.0343(10) 0.0250(9) 0.0199(9) -0.0001(7) 0.0116(8) 0.0022(7) O4 0.0305(9) 0.0281(9) 0.0196(9) 0.0055(7) 0.0111(7) 0.0063(7) P1 0.0249(3) 0.0245(3) 0.0168(3) 0.0005(2) 0.0080(3) 0.0020(3) P2 0.0248(3) 0.0257(3) 0.0178(3) -0.0001(3) 0.0086(3) 0.0018(3) P3 0.0257(3) 0.0265(3) 0.0177(3) 0.0005(2) 0.0095(3) 0.0016(3) P4 0.0245(3) 0.0251(3) 0.0167(3) 0.0017(2) 0.0084(3) 0.0045(3) C1 0.0308(14) 0.0337(15) 0.0292(14) 0.0045(12) 0.0085(12) 0.0003(12) C2 0.0371(16) 0.0365(16) 0.0452(17) 0.0066(13) 0.0169(14) -0.0035(13) C3 0.0282(14) 0.0336(16) 0.0486(18) -0.0046(14) 0.0075(13) -0.0014(12) C4 0.0323(15) 0.0383(16) 0.0306(15) -0.0054(12) 0.0022(12) 0.0056(12) C5 0.0330(14) 0.0323(15) 0.0244(13) -0.0027(11) 0.0091(11) 0.0045(12) C6 0.0289(13) 0.0212(13) 0.0264(13) -0.0021(10) 0.0089(11) 0.0018(10) C7 0.0286(13) 0.0235(13) 0.0202(12) -0.0008(10) 0.0100(10) 0.0010(10) C8 0.0362(14) 0.0264(13) 0.0207(12) -0.0008(10) 0.0128(11) 0.0057(11) C9 0.0446(17) 0.0295(15) 0.0385(17) 0.0014(13) 0.0098(14) 0.0041(13) C10 0.060(2) 0.0343(17) 0.0383(18) 0.0051(14) 0.0057(16) 0.0099(15) C11 0.073(2) 0.0290(15) 0.0299(16) 0.0041(12) 0.0174(16) 0.0050(15) C12 0.066(2) 0.0296(16) 0.0457(18) -0.0019(14) 0.0312(17) -0.0010(15) C13 0.0425(16) 0.0291(15) 0.0345(16) 0.0002(12) 0.0162(13) 0.0038(12) C14 0.0422(16) 0.0229(13) 0.0239(13) -0.0009(10) 0.0149(12) 0.0062(11) C15 0.0249(13) 0.0276(13) 0.0202(12) 0.0008(10) 0.0087(10) 0.0029(10) C16 0.0337(15) 0.0323(15) 0.0294(14) -0.0043(11) 0.0133(12) 0.0001(12) C17 0.0432(17) 0.0415(17) 0.0428(17) -0.0122(14) 0.0238(15) -0.0096(14) C18 0.0278(14) 0.055(2) 0.0369(16) -0.0161(14) 0.0145(13) -0.0075(14) C19 0.0273(15) 0.0490(18) 0.0325(15) -0.0067(13) 0.0060(12) 0.0068(13) C20 0.0309(15) 0.0355(16) 0.0322(15) -0.0016(12) 0.0081(12) 0.0038(12) C21 0.0274(13) 0.0326(14) 0.0232(13) -0.0045(11) 0.0106(11) 0.0021(11) C22 0.0270(13) 0.0290(14) 0.0172(12) -0.0013(10) 0.0085(10) -0.0005(10) C23 0.0322(14) 0.0295(14) 0.0173(12) 0.0009(10) 0.0109(11) 0.0002(11) C24 0.0552(19) 0.0392(17) 0.0222(14) 0.0076(13) -0.0035(13) -0.0086(15) C25 0.081(3) 0.044(2) 0.0323(18) 0.0161(15) -0.0092(18) -0.0263(19) C26 0.081(3) 0.100(4) 0.0273(17) 0.0015(19) 0.0131(18) -0.061(3) C27 0.066(2) 0.107(4) 0.048(2) -0.023(2) 0.0385(19) -0.044(2) C28 0.0482(18) 0.066(2) 0.0349(17) -0.0126(15) 0.0256(15) -0.0151(16) C29 0.0406(16) 0.0400(16) 0.0144(12) 0.0037(11) 0.0087(11) -0.0075(13) C30 0.0276(13) 0.0243(13) 0.0175(12) 0.0011(10) 0.0079(10) 0.0009(10) C31 0.0342(15) 0.0336(15) 0.0322(15) 0.0002(12) 0.0141(12) -0.0003(12) C32 0.0388(16) 0.0388(17) 0.0481(18) -0.0038(14) 0.0238(15) -0.0084(13) C33 0.0250(14) 0.0467(18) 0.0429(17) -0.0129(14) 0.0124(13) -0.0036(13) C34 0.0300(15) 0.0472(18) 0.0310(15) -0.0006(13) 0.0104(12) 0.0029(13) C35 0.0276(14) 0.0411(16) 0.0286(14) 0.0021(12) 0.0113(12) 0.0000(12) C36 0.0270(13) 0.0291(14) 0.0235(13) -0.0040(11) 0.0113(11) 0.0008(11) C37 0.0236(12) 0.0256(13) 0.0208(12) 0.0026(10) 0.0093(10) 0.0042(10) C38 0.0337(14) 0.0274(14) 0.0214(12) -0.0007(10) 0.0128(11) 0.0070(11) C39 0.059(2) 0.0374(18) 0.060(2) -0.0011(17) -0.0054(18) 0.0176(16) C40 0.124(4) 0.045(2) 0.048(2) 0.0018(19) -0.026(2) 0.033(3) C41 0.171(5) 0.034(2) 0.037(2) 0.0109(17) 0.034(3) 0.026(3) C42 0.124(4) 0.0289(18) 0.084(3) 0.0102(19) 0.071(3) 0.012(2) C43 0.063(2) 0.0266(15) 0.058(2) 0.0040(14) 0.0307(18) 0.0070(15) C44 0.0463(16) 0.0258(14) 0.0224(13) -0.0020(11) 0.0129(12) 0.0096(12) C45 0.0273(13) 0.0221(12) 0.0198(12) 0.0000(10) 0.0093(10) 0.0034(10) C46 0.0277(14) 0.0401(16) 0.0319(15) 0.0050(12) 0.0075(12) 0.0010(12) C47 0.0368(16) 0.0429(18) 0.0470(18) 0.0050(14) 0.0135(14) -0.0021(13) C48 0.0266(15) 0.0544(19) 0.0388(17) -0.0106(15) 0.0078(13) 0.0002(13) C49 0.0307(15) 0.061(2) 0.0239(14) -0.0012(13) 0.0103(12) 0.0105(14) C50 0.0287(14) 0.0452(17) 0.0199(13) -0.0007(12) 0.0081(11) 0.0074(12) C51 0.0271(13) 0.0302(14) 0.0210(12) -0.0017(10) 0.0094(11) 0.0059(11) C52 0.0267(13) 0.0269(13) 0.0186(12) 0.0004(10) 0.0093(10) 0.0034(10) C53 0.0304(14) 0.0339(15) 0.0188(12) 0.0027(11) 0.0125(11) 0.0042(11) C54 0.0351(15) 0.0375(15) 0.0216(13) 0.0106(11) 0.0108(11) 0.0040(12) C55 0.0463(17) 0.0367(16) 0.0270(14) 0.0104(12) 0.0121(13) 0.0016(13) C56 0.0495(19) 0.0446(18) 0.0331(16) 0.0075(13) 0.0163(14) -0.0107(15) C57 0.0379(16) 0.055(2) 0.0393(17) 0.0074(15) 0.0206(14) -0.0053(14) C58 0.0395(16) 0.0413(16) 0.0308(15) 0.0027(12) 0.0199(13) 0.0018(13) C59 0.0340(14) 0.0358(15) 0.0176(12) 0.0061(11) 0.0116(11) 0.0024(12) C60 0.0295(13) 0.0321(14) 0.0183(12) -0.0025(10) 0.0121(11) -0.0005(11) C61 0.087(3) 0.046(2) 0.076(3) -0.008(2) -0.011(2) -0.004(2) C62 0.074(3) 0.048(2) 0.053(2) -0.0103(18) -0.002(2) 0.014(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 O1 2.0423(17) . ? Ni1 O4 2.0504(17) . ? Ni1 O2 2.0512(17) . ? Ni1 O3 2.0523(17) . ? Ni1 N1 2.172(2) . ? Ni1 N3 2.180(2) . ? B1 F1 1.351(4) . ? B1 F3 1.370(4) . ? B1 F2 1.380(4) . ? B1 F4 1.385(4) . ? B2 F8 1.341(4) . ? B2 F7 1.352(4) . ? B2 F5 1.385(4) . ? B2 F6 1.411(5) . ? N1 C7 1.491(3) . ? N1 C15 1.493(3) . ? N1 C8 1.517(3) . ? N2 C22 1.464(3) . ? N2 C30 1.472(3) . ? N2 C23 1.488(3) . ? N3 C37 1.488(3) . ? N3 C45 1.490(3) . ? N3 C38 1.516(3) . ? N4 C60 1.454(3) . ? N4 C52 1.471(3) . ? N4 C53 1.491(3) . ? N5 C62 1.144(5) . ? O1 P1 1.5136(18) . ? O2 P2 1.5062(18) . ? O3 P3 1.5056(18) . ? O4 P4 1.5111(18) . ? P1 C6 1.798(3) . ? P1 C7 1.823(2) . ? P1 C30 1.841(2) . ? P2 C21 1.795(3) . ? P2 C22 1.804(2) . ? P2 C15 1.827(3) . ? P3 C36 1.792(3) . ? P3 C60 1.817(2) . ? P3 C37 1.821(3) . ? P4 C51 1.788(3) . ? P4 C45 1.831(2) . ? P4 C52 1.833(2) . ? C1 C2 1.376(4) . ? C1 C6 1.397(4) . ? C2 C3 1.384(4) . ? C3 C4 1.386(4) . ? C4 C5 1.384(4) . ? C5 C6 1.394(4) . ? C8 C14 1.516(4) . ? C9 C14 1.393(4) . ? C9 C10 1.393(4) . ? C10 C11 1.372(5) . ? C11 C12 1.375(5) . ? C12 C13 1.390(4) . ? C13 C14 1.387(4) . ? C16 C21 1.390(4) . ? C16 C17 1.390(4) . ? C17 C18 1.384(4) . ? C18 C19 1.375(5) . ? C19 C20 1.384(4) . ? C20 C21 1.400(4) . ? C23 C29 1.504(4) . ? C24 C29 1.380(4) . ? C24 C25 1.392(5) . ? C25 C26 1.374(6) . ? C26 C27 1.364(6) . ? C27 C28 1.387(5) . ? C28 C29 1.395(4) . ? C31 C32 1.383(4) . ? C31 C36 1.396(4) . ? C32 C33 1.380(4) . ? C33 C34 1.378(4) . ? C34 C35 1.395(4) . ? C35 C36 1.393(4) . ? C38 C44 1.514(4) . ? C39 C44 1.378(4) . ? C39 C40 1.400(6) . ? C40 C41 1.364(7) . ? C41 C42 1.376(7) . ? C42 C43 1.386(5) . ? C43 C44 1.394(4) . ? C46 C47 1.378(4) . ? C46 C51 1.397(4) . ? C47 C48 1.386(4) . ? C48 C49 1.377(5) . ? C49 C50 1.383(4) . ? C50 C51 1.396(4) . ? C53 C59 1.509(4) . ? C54 C55 1.387(4) . ? C54 C59 1.400(4) . ? C55 C56 1.387(4) . ? C56 C57 1.386(5) . ? C57 C58 1.397(4) . ? C58 C59 1.389(4) . ? C61 C62 1.455(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 Ni1 O4 177.12(7) . . ? O1 Ni1 O2 87.42(7) . . ? O4 Ni1 O2 90.48(7) . . ? O1 Ni1 O3 94.88(7) . . ? O4 Ni1 O3 87.30(7) . . ? O2 Ni1 O3 176.93(7) . . ? O1 Ni1 N1 89.45(7) . . ? O4 Ni1 N1 88.51(7) . . ? O2 Ni1 N1 87.85(7) . . ? O3 Ni1 N1 94.20(7) . . ? O1 Ni1 N3 91.32(7) . . ? O4 Ni1 N3 90.66(7) . . ? O2 Ni1 N3 90.39(7) . . ? O3 Ni1 N3 87.52(7) . . ? N1 Ni1 N3 178.05(8) . . ? F1 B1 F3 107.6(3) . . ? F1 B1 F2 112.7(3) . . ? F3 B1 F2 108.9(3) . . ? F1 B1 F4 110.5(3) . . ? F3 B1 F4 109.4(3) . . ? F2 B1 F4 107.7(2) . . ? F8 B2 F7 113.0(3) . . ? F8 B2 F5 108.3(3) . . ? F7 B2 F5 110.1(3) . . ? F8 B2 F6 104.9(3) . . ? F7 B2 F6 108.0(3) . . ? F5 B2 F6 112.5(4) . . ? C7 N1 C15 113.17(18) . . ? C7 N1 C8 108.99(19) . . ? C15 N1 C8 108.86(19) . . ? C7 N1 Ni1 108.51(14) . . ? C15 N1 Ni1 106.07(15) . . ? C8 N1 Ni1 111.23(14) . . ? C22 N2 C30 113.53(19) . . ? C22 N2 C23 109.25(19) . . ? C30 N2 C23 112.80(19) . . ? C37 N3 C45 113.69(18) . . ? C37 N3 C38 108.61(18) . . ? C45 N3 C38 108.65(19) . . ? C37 N3 Ni1 107.65(15) . . ? C45 N3 Ni1 106.58(14) . . ? C38 N3 Ni1 111.70(14) . . ? C60 N4 C52 114.0(2) . . ? C60 N4 C53 112.10(19) . . ? C52 N4 C53 112.45(19) . . ? P1 O1 Ni1 112.19(10) . . ? P2 O2 Ni1 114.17(10) . . ? P3 O3 Ni1 115.73(10) . . ? P4 O4 Ni1 112.22(9) . . ? O1 P1 C6 109.88(11) . . ? O1 P1 C7 107.92(10) . . ? C6 P1 C7 105.17(12) . . ? O1 P1 C30 115.34(11) . . ? C6 P1 C30 109.11(12) . . ? C7 P1 C30 108.92(11) . . ? O2 P2 C21 112.73(12) . . ? O2 P2 C22 112.73(11) . . ? C21 P2 C22 105.84(12) . . ? O2 P2 C15 109.39(11) . . ? C21 P2 C15 107.54(12) . . ? C22 P2 C15 108.36(12) . . ? O3 P3 C36 112.19(11) . . ? O3 P3 C60 115.02(11) . . ? C36 P3 C60 106.07(12) . . ? O3 P3 C37 108.79(10) . . ? C36 P3 C37 107.11(12) . . ? C60 P3 C37 107.26(12) . . ? O4 P4 C51 111.29(11) . . ? O4 P4 C45 108.78(11) . . ? C51 P4 C45 104.86(12) . . ? O4 P4 C52 114.45(11) . . ? C51 P4 C52 108.19(12) . . ? C45 P4 C52 108.81(11) . . ? C2 C1 C6 119.8(3) . . ? C1 C2 C3 120.6(3) . . ? C2 C3 C4 119.9(3) . . ? C5 C4 C3 120.0(3) . . ? C4 C5 C6 120.1(3) . . ? C5 C6 C1 119.5(2) . . ? C5 C6 P1 118.0(2) . . ? C1 C6 P1 122.4(2) . . ? N1 C7 P1 111.87(16) . . ? C14 C8 N1 113.84(19) . . ? C14 C9 C10 121.0(3) . . ? C11 C10 C9 119.9(3) . . ? C10 C11 C12 119.9(3) . . ? C11 C12 C13 120.3(3) . . ? C14 C13 C12 120.9(3) . . ? C13 C14 C9 117.9(3) . . ? C13 C14 C8 121.3(2) . . ? C9 C14 C8 120.8(3) . . ? N1 C15 P2 111.53(16) . . ? C21 C16 C17 119.6(3) . . ? C18 C17 C16 120.0(3) . . ? C19 C18 C17 120.3(3) . . ? C18 C19 C20 120.6(3) . . ? C19 C20 C21 119.3(3) . . ? C16 C21 C20 120.1(3) . . ? C16 C21 P2 118.9(2) . . ? C20 C21 P2 121.1(2) . . ? N2 C22 P2 113.08(17) . . ? N2 C23 C29 111.6(2) . . ? C29 C24 C25 120.3(4) . . ? C26 C25 C24 119.8(4) . . ? C27 C26 C25 120.4(3) . . ? C26 C27 C28 120.6(4) . . ? C27 C28 C29 119.6(4) . . ? C24 C29 C28 119.3(3) . . ? C24 C29 C23 119.9(3) . . ? C28 C29 C23 120.9(3) . . ? N2 C30 P1 114.27(17) . . ? C32 C31 C36 119.6(3) . . ? C33 C32 C31 120.4(3) . . ? C34 C33 C32 120.6(3) . . ? C33 C34 C35 119.9(3) . . ? C36 C35 C34 119.6(3) . . ? C35 C36 C31 120.0(2) . . ? C35 C36 P3 120.8(2) . . ? C31 C36 P3 119.2(2) . . ? N3 C37 P3 112.13(16) . . ? C44 C38 N3 114.11(19) . . ? C44 C39 C40 120.8(4) . . ? C41 C40 C39 120.4(4) . . ? C40 C41 C42 119.7(4) . . ? C41 C42 C43 120.1(4) . . ? C42 C43 C44 121.0(4) . . ? C39 C44 C43 117.9(3) . . ? C39 C44 C38 120.5(3) . . ? C43 C44 C38 121.6(3) . . ? N3 C45 P4 112.85(17) . . ? C47 C46 C51 119.9(3) . . ? C46 C47 C48 120.1(3) . . ? C49 C48 C47 120.3(3) . . ? C48 C49 C50 120.3(3) . . ? C49 C50 C51 119.6(3) . . ? C50 C51 C46 119.7(2) . . ? C50 C51 P4 119.8(2) . . ? C46 C51 P4 120.5(2) . . ? N4 C52 P4 114.04(16) . . ? N4 C53 C59 110.8(2) . . ? C55 C54 C59 120.3(3) . . ? C56 C55 C54 120.3(3) . . ? C57 C56 C55 120.0(3) . . ? C56 C57 C58 119.9(3) . . ? C59 C58 C57 120.6(3) . . ? C58 C59 C54 119.0(3) . . ? C58 C59 C53 121.2(3) . . ? C54 C59 C53 119.8(2) . . ? N4 C60 P3 112.50(17) . . ? N5 C62 C61 178.1(5) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.509 _refine_diff_density_min -0.756 _refine_diff_density_rms 0.074 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.500 0.000 0.500 275.4 38.8 2 0.000 0.500 1.000 275.4 38.8 _platon_squeeze_details ; Disordered solvent molecule Et2O removed. 78 electrons/cell ;