Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Pedro Valerga' _publ_contact_author_address ; Ciencia de Mat. e I.M. y Quimica Inorganica Universidad de Cadiz Facultad de Ciencias Campus Rio San Pedro Puerto Real Cadiz 11500 SPAIN ; _publ_contact_author_email PEDRO.VALERGA@UCA.ES _publ_section_title ; Oligomerization and Regioselective Hydrosilylation of Styrenes Catalyzed by Cationic Allyl Nickel Complexes Bearing Allylphosphine Ligands ; loop_ _publ_author_name 'Pedro Valerga' 'Iqbal Hyder' 'Manuel Jimenez-Tenorio' 'M. Puerta' data_pv0516 _database_code_depnum_ccdc_archive 'CCDC 638224' _audit_creation_method SHELXL-97 _chemical_name_systematic 'trihapto-allyl-bromide-allyldiphenylphosphine-nickel (II)' _chemical_name_common 'trihapto-allyl-bromide-allyldiphenylphosphine-nickel (ii)' _chemical_melting_point ? _chemical_formula_moiety 'C18 H20 Br Ni P' _chemical_formula_sum 'C18 H20 Br Ni P' _chemical_formula_weight 405.93 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_int_tables_number 61 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 11.461(2) _cell_length_b 16.298(3) _cell_length_c 18.029(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3367.8(12) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5554 _cell_measurement_theta_min 2.254 _cell_measurement_theta_max 24.898 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.601 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1648 _exptl_absorpt_coefficient_mu 3.611 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.754 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details '(SADABS; Sheldrick, 2004)' _exptl_special_details ; Bruker SMART APEX 3-circle diffractometer with CCD area detector, sealed X-ray tube, graphite monochromator. A hemisphere of the reciprocal space up to theta(max) = 25.16 deg was measured by omega scan frames with delta(omega) = 0.30 deg and 10 sec per frame, 1700 frames were recorded using program SMART (Bruker). Frame data evaluation and integration were done with program SAINT+(Bruker); Lattice parameters by least-squares refinement of the geometric parameters of the strongest reflections with program SAINT + (Bruker). Correction for absorption and crystal decay (insignificant) were applied by semi-empirical method from equivalents using program SADABS (G.M. Sheldrick, version of 2001, Univ. of Goettingen, Germany). Data reduction was done with program XPREP (BRUKER). ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_source_type 'Bruker SMART APEX' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD area detector' _diffrn_measurement_method '1700 omega scan frames, 0.3 deg, 10 sec' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% -0.0188 _diffrn_reflns_number 21191 _diffrn_reflns_av_R_equivalents 0.0552 _diffrn_reflns_av_sigmaI/netI 0.0339 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 25.16 _reflns_number_total 2992 _reflns_number_gt 2580 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SAINT (Bruker, 2001)' _computing_data_reduction 'SAINT (Bruker, 2001)' _computing_structure_solution 'SHELXTL (Sheldrick, 2001)' _computing_structure_refinement 'SHELXTL (Sheldrick, 2001)' _computing_molecular_graphics 'ORTEP-3 vers. 1.08 (Faruggia, 2005)' _computing_publication_material 'SHELXTL (Sheldrick, 2001)' _refine_special_details ; 1) 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. 2) All non hydrogen atoms were anisotropically refined. All hydrogen atoms were isotropically refined with thermal parameters related to their parent bonded atoms. ; _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^)+(0.0443P)^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_extinction_coef ? _refine_ls_number_reflns 2992 _refine_ls_number_parameters 250 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0468 _refine_ls_R_factor_gt 0.0341 _refine_ls_wR_factor_ref 0.0773 _refine_ls_wR_factor_gt 0.0732 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.93341(3) 0.17186(2) 0.35059(2) 0.01705(12) Uani 1 1 d . . . Br1 Br 0.74361(2) 0.122061(19) 0.353519(18) 0.02541(12) Uani 1 1 d . . . P1 P 0.89458(6) 0.29385(5) 0.30543(4) 0.01619(18) Uani 1 1 d . . . C1 C 1.1052(3) 0.1912(2) 0.3588(2) 0.0284(8) Uani 1 1 d . . . H1A H 1.102(3) 0.197(2) 0.405(2) 0.034 Uiso 1 1 d . . . H1B H 1.148(3) 0.221(2) 0.3302(19) 0.034 Uiso 1 1 d . . . C2 C 1.0812(3) 0.1067(2) 0.3494(2) 0.0310(8) Uani 1 1 d . . . H2 H 1.102(3) 0.083(2) 0.297(2) 0.037 Uiso 1 1 d . . . C3 C 1.0059(3) 0.0673(2) 0.39613(19) 0.0241(7) Uani 1 1 d . . . H3A H 0.978(3) 0.011(2) 0.3853(18) 0.029 Uiso 1 1 d . . . H3B H 0.996(3) 0.082(2) 0.4448(18) 0.029 Uiso 1 1 d . . . C4 C 0.7492(2) 0.3367(2) 0.32724(18) 0.0200(7) Uani 1 1 d . . . H4A H 0.745(2) 0.3900(19) 0.308(2) 0.024 Uiso 1 1 d . . . H4B H 0.695(3) 0.2997(19) 0.3033(18) 0.024 Uiso 1 1 d . . . C5 C 0.7259(2) 0.3397(2) 0.40842(17) 0.0202(7) Uani 1 1 d . . . H5 H 0.715(3) 0.288(2) 0.4300(18) 0.024 Uiso 1 1 d . . . C6 C 0.7248(3) 0.4074(2) 0.4479(2) 0.0291(8) Uani 1 1 d . . . H6A H 0.739(3) 0.458(2) 0.423(2) 0.035 Uiso 1 1 d . . . H6B H 0.705(3) 0.407(2) 0.497(2) 0.035 Uiso 1 1 d . . . C7 C 0.8971(2) 0.29061(18) 0.20449(16) 0.0166(6) Uani 1 1 d . . . C8 C 0.9567(2) 0.22713(19) 0.17022(17) 0.0195(7) Uani 1 1 d . . . H8 H 0.997(3) 0.1861(19) 0.1981(18) 0.023 Uiso 1 1 d . . . C9 C 0.9594(3) 0.2207(2) 0.09399(18) 0.0236(7) Uani 1 1 d . . . H9 H 0.997(3) 0.179(2) 0.0725(18) 0.028 Uiso 1 1 d . . . C10 C 0.9026(3) 0.2785(2) 0.05136(19) 0.0240(7) Uani 1 1 d . . . H10 H 0.902(3) 0.2739(19) 0.004(2) 0.029 Uiso 1 1 d . . . C11 C 0.8439(2) 0.3429(2) 0.08417(18) 0.0237(7) Uani 1 1 d . . . H11 H 0.809(3) 0.3820(18) 0.0566(19) 0.028 Uiso 1 1 d . . . C12 C 0.8401(3) 0.34907(19) 0.16033(18) 0.0222(7) Uani 1 1 d . . . H12 H 0.796(3) 0.3953(19) 0.1836(18) 0.027 Uiso 1 1 d . . . C13 C 0.9896(2) 0.37894(17) 0.33139(17) 0.0167(6) Uani 1 1 d . . . C14 C 1.0183(2) 0.3890(2) 0.40589(17) 0.0209(7) Uani 1 1 d . . . H14 H 0.995(3) 0.3526(19) 0.4403(18) 0.025 Uiso 1 1 d . . . C15 C 1.0843(2) 0.45442(19) 0.42940(18) 0.0229(7) Uani 1 1 d . . . H15 H 1.102(2) 0.4578(19) 0.4789(19) 0.028 Uiso 1 1 d . . . C16 C 1.1242(3) 0.5117(2) 0.37896(19) 0.0252(7) Uani 1 1 d . . . H16 H 1.167(3) 0.556(2) 0.3926(18) 0.030 Uiso 1 1 d . . . C17 C 1.0976(3) 0.5017(2) 0.3045(2) 0.0265(7) Uani 1 1 d . . . H17 H 1.128(3) 0.536(2) 0.2703(18) 0.032 Uiso 1 1 d . . . C18 C 1.0307(2) 0.43634(19) 0.28107(17) 0.0201(7) Uani 1 1 d . . . H18 H 1.012(2) 0.430(2) 0.2327(17) 0.024 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0175(2) 0.0187(2) 0.0150(2) 0.00183(16) -0.00061(14) 0.00167(15) Br1 0.01948(18) 0.0216(2) 0.0352(2) 0.00041(14) 0.00036(13) -0.00083(12) P1 0.0167(4) 0.0188(4) 0.0131(4) 0.0005(3) -0.0004(3) 0.0008(3) C1 0.0194(16) 0.030(2) 0.036(2) -0.0014(17) -0.0045(15) 0.0026(14) C2 0.0253(17) 0.034(2) 0.033(2) 0.0032(16) -0.0058(14) 0.0073(15) C3 0.0279(16) 0.0212(18) 0.023(2) 0.0017(15) -0.0036(14) 0.0061(14) C4 0.0204(15) 0.0195(17) 0.0202(18) 0.0015(14) -0.0008(12) 0.0011(13) C5 0.0162(14) 0.0239(18) 0.0204(19) 0.0022(15) 0.0024(12) -0.0006(13) C6 0.0269(17) 0.034(2) 0.026(2) -0.0025(18) 0.0030(14) 0.0011(15) C7 0.0171(13) 0.0194(16) 0.0133(16) -0.0005(13) -0.0011(11) -0.0031(12) C8 0.0209(15) 0.0204(17) 0.0173(18) -0.0007(13) -0.0007(12) 0.0013(13) C9 0.0306(17) 0.0201(17) 0.0200(19) -0.0033(14) 0.0038(13) 0.0036(14) C10 0.0268(16) 0.0313(19) 0.0138(17) -0.0015(15) 0.0002(13) -0.0071(14) C11 0.0222(16) 0.0284(19) 0.021(2) 0.0059(14) -0.0040(13) 0.0049(14) C12 0.0216(16) 0.0253(18) 0.0197(19) -0.0013(14) -0.0002(12) 0.0049(14) C13 0.0152(14) 0.0178(16) 0.0171(17) -0.0001(12) 0.0010(11) 0.0030(12) C14 0.0212(15) 0.0255(18) 0.0161(18) 0.0026(14) 0.0045(12) -0.0003(13) C15 0.0229(15) 0.0264(19) 0.0195(19) -0.0062(14) 0.0010(12) 0.0026(13) C16 0.0213(16) 0.0233(18) 0.031(2) -0.0072(15) -0.0032(14) 0.0025(13) C17 0.0257(16) 0.0200(18) 0.034(2) 0.0085(15) 0.0018(14) 0.0002(14) C18 0.0210(15) 0.0208(17) 0.0184(18) 0.0010(14) -0.0001(13) 0.0030(13) _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 C1 1.999(3) . ? Ni1 C2 2.000(3) . ? Ni1 C3 2.066(3) . ? Ni1 P1 2.1941(9) . ? Ni1 Br1 2.3224(6) . ? P1 C7 1.821(3) . ? P1 C13 1.824(3) . ? P1 C4 1.849(3) . ? C1 C2 1.414(5) . ? C1 H1A 0.83(4) . ? C1 H1B 0.86(4) . ? C2 C3 1.366(5) . ? C2 H2 1.06(3) . ? C3 H3A 0.99(3) . ? C3 H3B 0.92(3) . ? C4 C5 1.489(4) . ? C4 H4A 0.94(3) . ? C4 H4B 0.97(3) . ? C5 C6 1.313(5) . ? C5 H5 0.94(3) . ? C6 H6A 0.96(4) . ? C6 H6B 0.92(4) . ? C7 C8 1.385(4) . ? C7 C12 1.403(4) . ? C8 C9 1.379(4) . ? C8 H8 0.96(3) . ? C9 C10 1.379(5) . ? C9 H9 0.89(3) . ? C10 C11 1.380(4) . ? C10 H10 0.85(4) . ? C11 C12 1.378(4) . ? C11 H11 0.90(3) . ? C12 H12 1.00(3) . ? C13 C18 1.386(4) . ? C13 C14 1.393(4) . ? C14 C15 1.374(4) . ? C14 H14 0.90(3) . ? C15 C16 1.381(5) . ? C15 H15 0.92(3) . ? C16 C17 1.386(5) . ? C16 H16 0.91(3) . ? C17 C18 1.379(4) . ? C17 H17 0.90(3) . ? C18 H18 0.90(3) . ? 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 Ni1 C2 41.43(15) . . ? C1 Ni1 C3 72.80(14) . . ? C2 Ni1 C3 39.22(13) . . ? C1 Ni1 P1 94.86(11) . . ? C2 Ni1 P1 130.49(11) . . ? C3 Ni1 P1 167.55(9) . . ? C1 Ni1 Br1 167.34(11) . . ? C2 Ni1 Br1 127.45(11) . . ? C3 Ni1 Br1 94.55(9) . . ? P1 Ni1 Br1 97.76(3) . . ? C7 P1 C13 105.61(13) . . ? C7 P1 C4 103.74(14) . . ? C13 P1 C4 101.30(14) . . ? C7 P1 Ni1 109.97(10) . . ? C13 P1 Ni1 118.20(10) . . ? C4 P1 Ni1 116.51(11) . . ? C2 C1 Ni1 69.31(19) . . ? C2 C1 H1A 103(3) . . ? Ni1 C1 H1A 93(2) . . ? C2 C1 H1B 126(2) . . ? Ni1 C1 H1B 127(2) . . ? H1A C1 H1B 124(4) . . ? C3 C2 C1 120.4(3) . . ? C3 C2 Ni1 73.01(19) . . ? C1 C2 Ni1 69.26(19) . . ? C3 C2 H2 121.8(19) . . ? C1 C2 H2 115.0(19) . . ? Ni1 C2 H2 113.6(18) . . ? C2 C3 Ni1 67.77(19) . . ? C2 C3 H3A 121.0(19) . . ? Ni1 C3 H3A 123.8(19) . . ? C2 C3 H3B 123(2) . . ? Ni1 C3 H3B 97(2) . . ? H3A C3 H3B 113(3) . . ? C5 C4 P1 112.5(2) . . ? C5 C4 H4A 109(2) . . ? P1 C4 H4A 108.3(18) . . ? C5 C4 H4B 110.1(19) . . ? P1 C4 H4B 104.4(17) . . ? H4A C4 H4B 112(3) . . ? C6 C5 C4 124.2(3) . . ? C6 C5 H5 122(2) . . ? C4 C5 H5 114(2) . . ? C5 C6 H6A 118(2) . . ? C5 C6 H6B 122(2) . . ? H6A C6 H6B 120(3) . . ? C8 C7 C12 118.9(3) . . ? C8 C7 P1 118.4(2) . . ? C12 C7 P1 122.7(2) . . ? C9 C8 C7 120.8(3) . . ? C9 C8 H8 117.4(19) . . ? C7 C8 H8 121.7(19) . . ? C8 C9 C10 119.5(3) . . ? C8 C9 H9 120(2) . . ? C10 C9 H9 120(2) . . ? C9 C10 C11 120.7(3) . . ? C9 C10 H10 120(2) . . ? C11 C10 H10 119(2) . . ? C12 C11 C10 119.9(3) . . ? C12 C11 H11 119(2) . . ? C10 C11 H11 121(2) . . ? C11 C12 C7 120.1(3) . . ? C11 C12 H12 119.3(19) . . ? C7 C12 H12 120.6(19) . . ? C18 C13 C14 118.1(3) . . ? C18 C13 P1 123.3(2) . . ? C14 C13 P1 118.5(2) . . ? C15 C14 C13 121.3(3) . . ? C15 C14 H14 118(2) . . ? C13 C14 H14 121(2) . . ? C14 C15 C16 120.2(3) . . ? C14 C15 H15 117.8(19) . . ? C16 C15 H15 122(2) . . ? C15 C16 C17 119.1(3) . . ? C15 C16 H16 123(2) . . ? C17 C16 H16 118(2) . . ? C18 C17 C16 120.6(3) . . ? C18 C17 H17 119(2) . . ? C16 C17 H17 121(2) . . ? C17 C18 C13 120.7(3) . . ? C17 C18 H18 121(2) . . ? C13 C18 H18 118(2) . . ? 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 C1 Ni1 P1 C7 92.12(15) . . . . ? C2 Ni1 P1 C7 68.60(17) . . . . ? C3 Ni1 P1 C7 99.5(5) . . . . ? Br1 Ni1 P1 C7 -88.84(9) . . . . ? C1 Ni1 P1 C13 -29.20(16) . . . . ? C2 Ni1 P1 C13 -52.72(18) . . . . ? C3 Ni1 P1 C13 -21.8(5) . . . . ? Br1 Ni1 P1 C13 149.85(11) . . . . ? C1 Ni1 P1 C4 -150.25(17) . . . . ? C2 Ni1 P1 C4 -173.78(18) . . . . ? C3 Ni1 P1 C4 -142.8(5) . . . . ? Br1 Ni1 P1 C4 28.79(12) . . . . ? C3 Ni1 C1 C2 29.0(2) . . . . ? P1 Ni1 C1 C2 -152.7(2) . . . . ? Br1 Ni1 C1 C2 31.6(6) . . . . ? Ni1 C1 C2 C3 -54.2(3) . . . . ? C1 Ni1 C2 C3 133.0(3) . . . . ? P1 Ni1 C2 C3 169.91(17) . . . . ? Br1 Ni1 C2 C3 -38.7(3) . . . . ? C3 Ni1 C2 C1 -133.0(3) . . . . ? P1 Ni1 C2 C1 36.9(3) . . . . ? Br1 Ni1 C2 C1 -171.68(18) . . . . ? C1 C2 C3 Ni1 52.5(3) . . . . ? C1 Ni1 C3 C2 -30.5(2) . . . . ? P1 Ni1 C3 C2 -38.2(6) . . . . ? Br1 Ni1 C3 C2 150.1(2) . . . . ? C7 P1 C4 C5 176.3(2) . . . . ? C13 P1 C4 C5 -74.3(3) . . . . ? Ni1 P1 C4 C5 55.3(3) . . . . ? P1 C4 C5 C6 107.3(3) . . . . ? C13 P1 C7 C8 107.9(2) . . . . ? C4 P1 C7 C8 -146.0(2) . . . . ? Ni1 P1 C7 C8 -20.7(2) . . . . ? C13 P1 C7 C12 -72.9(3) . . . . ? C4 P1 C7 C12 33.2(3) . . . . ? Ni1 P1 C7 C12 158.5(2) . . . . ? C12 C7 C8 C9 -0.6(4) . . . . ? P1 C7 C8 C9 178.6(2) . . . . ? C7 C8 C9 C10 0.4(4) . . . . ? C8 C9 C10 C11 0.4(5) . . . . ? C9 C10 C11 C12 -1.0(4) . . . . ? C10 C11 C12 C7 0.8(4) . . . . ? C8 C7 C12 C11 0.1(4) . . . . ? P1 C7 C12 C11 -179.2(2) . . . . ? C7 P1 C13 C18 12.1(3) . . . . ? C4 P1 C13 C18 -95.8(3) . . . . ? Ni1 P1 C13 C18 135.6(2) . . . . ? C7 P1 C13 C14 -170.8(2) . . . . ? C4 P1 C13 C14 81.3(2) . . . . ? Ni1 P1 C13 C14 -47.3(2) . . . . ? C18 C13 C14 C15 0.8(4) . . . . ? P1 C13 C14 C15 -176.5(2) . . . . ? C13 C14 C15 C16 -0.3(4) . . . . ? C14 C15 C16 C17 -0.6(4) . . . . ? C15 C16 C17 C18 1.0(4) . . . . ? C16 C17 C18 C13 -0.5(4) . . . . ? C14 C13 C18 C17 -0.4(4) . . . . ? P1 C13 C18 C17 176.7(2) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.16 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.898 _refine_diff_density_min -0.346 _refine_diff_density_rms 0.086 #=== END #=== pv0613 ====== Compound 2 in the text data_pv0613 _database_code_depnum_ccdc_archive 'CCDC 638225' _audit_creation_method SHELXL-97 _chemical_name_systematic 'trihapto-allyl-allyldiisopropylphosphine-bromo-nickel (II)' _chemical_name_common 'trihapto-allyl-allyldiisopropylphosphine-bromo-nickel (ii)' _chemical_melting_point ? _chemical_formula_moiety 'C12 H24 Br Ni P' _chemical_formula_sum 'C12 H24 Br Ni P' _chemical_formula_weight 337.90 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' 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 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_int_tables_number 14 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 12.436(3) _cell_length_b 7.4524(16) _cell_length_c 15.775(4) _cell_angle_alpha 90.00 _cell_angle_beta 96.071(4) _cell_angle_gamma 90.00 _cell_volume 1453.8(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3238 _cell_measurement_theta_min 2.597 _cell_measurement_theta_max 24.997 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.49 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.544 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 696 _exptl_absorpt_coefficient_mu 4.164 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.667 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details '(SADABS; Sheldrick, 2004)' _exptl_special_details ; Bruker SMART APEX 3-circle diffractometer with CCD area detector, sealed X-ray tube, graphite monochromator. A hemisphere of the reciprocal space up to theta(max) = 25.02 deg was measured by omega scan frames with delta(omega) = 0.30 deg and 10 sec per frame, 1700 frames were recorded using program SMART (Bruker). Frame data evaluation and integration were done with program SAINT+(Bruker); Lattice parameters by least-squares refinement of the geometric parameters of the strongest reflections with program SAINT + (Bruker). Correction for absorption and crystal decay (insignificant) were applied by semi-empirical method from equivalents using program SADABS (G.M. Sheldrick, version of 2001, Univ. of Goettingen, Germany). Data reduction was done with program XPREP (BRUKER). ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_source_type 'Bruker SMART APEX' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD area detector' _diffrn_measurement_method '1700 omega scan frames, 0.3 deg, 10 sec' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.0001 _diffrn_reflns_number 5722 _diffrn_reflns_av_R_equivalents 0.0591 _diffrn_reflns_av_sigmaI/netI 0.0651 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.60 _diffrn_reflns_theta_max 25.02 _reflns_number_total 2508 _reflns_number_gt 2143 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SAINT (Bruker, 2001)' _computing_data_reduction 'SAINT (Bruker, 2001)' _computing_structure_solution 'SHELXTL (Sheldrick, 2001)' _computing_structure_refinement 'SHELXTL (Sheldrick, 2001)' _computing_molecular_graphics 'ORTEP-3 vers. 1.08 (Faruggia, 2005)' _computing_publication_material 'SHELXTL (Sheldrick, 2001)' _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^)+(0.0342P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2508 _refine_ls_number_parameters 140 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0403 _refine_ls_R_factor_gt 0.0345 _refine_ls_wR_factor_ref 0.0804 _refine_ls_wR_factor_gt 0.0783 _refine_ls_goodness_of_fit_ref 0.932 _refine_ls_restrained_S_all 0.932 _refine_ls_shift/su_max 0.000 _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 0.36536(3) 0.78357(6) 0.15244(3) 0.01628(14) Uani 1 1 d . . . Br1 Br 0.33546(3) 1.07875(4) 0.10675(2) 0.02176(13) Uani 1 1 d . . . P1 P 0.22601(7) 0.75073(12) 0.22533(6) 0.0157(2) Uani 1 1 d . . . C1 C 0.5042(3) 0.7578(5) 0.0932(3) 0.0245(9) Uani 1 1 d . . . H1A H 0.5020 0.8040 0.0342 0.029 Uiso 1 1 calc R . . H1B H 0.5736 0.7801 0.1285 0.029 Uiso 1 1 calc R . . C2 C 0.4546(3) 0.5940(5) 0.1039(3) 0.0261(9) Uani 1 1 d . . . H2 H 0.4242 0.5234 0.0531 0.031 Uiso 1 1 calc R . . C3 C 0.4310(3) 0.5453(5) 0.1849(2) 0.0249(9) Uani 1 1 d . . . H3A H 0.4920 0.5451 0.2306 0.030 Uiso 1 1 calc R . . H3B H 0.3803 0.4437 0.1884 0.030 Uiso 1 1 calc R . . C4 C 0.1626(3) 0.9602(5) 0.2578(2) 0.0193(8) Uani 1 1 d . . . H4A H 0.1406 1.0323 0.2061 0.023 Uiso 1 1 calc R . . H4B H 0.0963 0.9293 0.2842 0.023 Uiso 1 1 calc R . . C5 C 0.2335(3) 1.0731(4) 0.3190(2) 0.0218(9) Uani 1 1 d . . . H5 H 0.3015 1.1093 0.3025 0.026 Uiso 1 1 calc R . . C6 C 0.2083(3) 1.1263(5) 0.3943(2) 0.0277(9) Uani 1 1 d . . . H6A H 0.1410 1.0928 0.4130 0.033 Uiso 1 1 calc R . . H6B H 0.2576 1.1980 0.4298 0.033 Uiso 1 1 calc R . . C7 C 0.1111(3) 0.6502(5) 0.1573(2) 0.0191(8) Uani 1 1 d . . . H7 H 0.0442 0.6673 0.1864 0.023 Uiso 1 1 calc R . . C8 C 0.0952(3) 0.7469(5) 0.0718(2) 0.0284(9) Uani 1 1 d . . . H8A H 0.0838 0.8752 0.0813 0.043 Uiso 1 1 calc R . . H8B H 0.0320 0.6972 0.0374 0.043 Uiso 1 1 calc R . . H8C H 0.1596 0.7307 0.0418 0.043 Uiso 1 1 calc R . . C9 C 0.1268(3) 0.4480(5) 0.1443(3) 0.0296(10) Uani 1 1 d . . . H9A H 0.0655 0.4006 0.1067 0.044 Uiso 1 1 calc R . . H9B H 0.1308 0.3868 0.1995 0.044 Uiso 1 1 calc R . . H9C H 0.1939 0.4277 0.1183 0.044 Uiso 1 1 calc R . . C10 C 0.2417(3) 0.6107(5) 0.3218(2) 0.0176(8) Uani 1 1 d . . . H10 H 0.2612 0.4878 0.3029 0.021 Uiso 1 1 calc R . . C11 C 0.1375(3) 0.5898(5) 0.3647(2) 0.0245(9) Uani 1 1 d . . . H11A H 0.1507 0.5096 0.4140 0.037 Uiso 1 1 calc R . . H11B H 0.0807 0.5389 0.3240 0.037 Uiso 1 1 calc R . . H11C H 0.1144 0.7075 0.3838 0.037 Uiso 1 1 calc R . . C12 C 0.3363(3) 0.6739(5) 0.3853(2) 0.0242(8) Uani 1 1 d . . . H12A H 0.3196 0.7924 0.4075 0.036 Uiso 1 1 calc R . . H12B H 0.4021 0.6816 0.3563 0.036 Uiso 1 1 calc R . . H12C H 0.3476 0.5882 0.4325 0.036 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 0.0172(2) 0.0176(3) 0.0150(3) 0.0000(2) 0.00595(19) 0.00035(18) Br1 0.0280(2) 0.0187(2) 0.0200(2) 0.00278(16) 0.00910(16) 0.00096(15) P1 0.0175(5) 0.0169(5) 0.0133(5) -0.0004(4) 0.0042(4) -0.0005(4) C1 0.0167(18) 0.033(2) 0.025(2) 0.0045(19) 0.0084(17) 0.0050(16) C2 0.026(2) 0.025(2) 0.028(2) -0.0043(18) 0.0078(18) 0.0076(16) C3 0.025(2) 0.024(2) 0.027(2) 0.0050(18) 0.0081(17) 0.0061(16) C4 0.0204(18) 0.0195(19) 0.0193(19) 0.0003(17) 0.0078(15) 0.0007(15) C5 0.0223(19) 0.019(2) 0.025(2) 0.0006(17) 0.0064(17) 0.0015(15) C6 0.031(2) 0.024(2) 0.029(2) -0.0051(19) 0.0031(18) -0.0006(17) C7 0.0178(17) 0.027(2) 0.0134(18) -0.0009(17) 0.0037(15) -0.0043(15) C8 0.028(2) 0.041(2) 0.016(2) 0.0006(19) 0.0015(17) -0.0066(18) C9 0.033(2) 0.029(2) 0.027(2) -0.0070(19) 0.0027(18) -0.0053(17) C10 0.0241(18) 0.0144(18) 0.0152(18) -0.0015(16) 0.0070(15) 0.0029(14) C11 0.028(2) 0.031(2) 0.0159(19) 0.0018(17) 0.0096(17) -0.0004(16) C12 0.032(2) 0.026(2) 0.0148(19) 0.0017(17) 0.0021(16) 0.0038(17) _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 C2 1.998(4) . ? Ni1 C3 1.998(3) . ? Ni1 C1 2.058(3) . ? Ni1 P1 2.1924(10) . ? Ni1 Br1 2.3324(7) . ? P1 C10 1.838(3) . ? P1 C4 1.846(3) . ? P1 C7 1.853(3) . ? C1 C2 1.386(5) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.389(5) . ? C2 H2 1.0000 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.496(5) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.321(5) . ? C5 H5 0.9500 . ? C6 H6A 0.9500 . ? C6 H6B 0.9500 . ? C7 C8 1.523(5) . ? C7 C9 1.536(5) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.533(5) . ? C10 C12 1.536(5) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? 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 C2 Ni1 C3 40.69(15) . . ? C2 Ni1 C1 39.92(14) . . ? C3 Ni1 C1 72.17(15) . . ? C2 Ni1 P1 128.60(11) . . ? C3 Ni1 P1 95.18(11) . . ? C1 Ni1 P1 167.33(11) . . ? C2 Ni1 Br1 128.70(12) . . ? C3 Ni1 Br1 164.75(11) . . ? C1 Ni1 Br1 93.55(10) . . ? P1 Ni1 Br1 99.11(3) . . ? C10 P1 C4 105.18(16) . . ? C10 P1 C7 104.94(16) . . ? C4 P1 C7 100.19(16) . . ? C10 P1 Ni1 118.48(11) . . ? C4 P1 Ni1 115.82(12) . . ? C7 P1 Ni1 110.20(12) . . ? C2 C1 Ni1 67.7(2) . . ? C2 C1 H1A 116.9 . . ? Ni1 C1 H1A 116.9 . . ? C2 C1 H1B 116.9 . . ? Ni1 C1 H1B 116.9 . . ? H1A C1 H1B 113.9 . . ? C1 C2 C3 118.9(4) . . ? C1 C2 Ni1 72.4(2) . . ? C3 C2 Ni1 69.7(2) . . ? C1 C2 H2 120.1 . . ? C3 C2 H2 120.1 . . ? Ni1 C2 H2 120.1 . . ? C2 C3 Ni1 69.7(2) . . ? C2 C3 H3A 116.7 . . ? Ni1 C3 H3A 116.7 . . ? C2 C3 H3B 116.7 . . ? Ni1 C3 H3B 116.7 . . ? H3A C3 H3B 113.7 . . ? C5 C4 P1 114.5(2) . . ? C5 C4 H4A 108.6 . . ? P1 C4 H4A 108.6 . . ? C5 C4 H4B 108.6 . . ? P1 C4 H4B 108.6 . . ? H4A C4 H4B 107.6 . . ? C6 C5 C4 124.8(3) . . ? C6 C5 H5 117.6 . . ? C4 C5 H5 117.6 . . ? C5 C6 H6A 120.0 . . ? C5 C6 H6B 120.0 . . ? H6A C6 H6B 120.0 . . ? C8 C7 C9 110.7(3) . . ? C8 C7 P1 110.0(2) . . ? C9 C7 P1 111.9(2) . . ? C8 C7 H7 108.1 . . ? C9 C7 H7 108.1 . . ? P1 C7 H7 108.1 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 C12 111.6(3) . . ? C11 C10 P1 113.8(2) . . ? C12 C10 P1 111.8(2) . . ? C11 C10 H10 106.4 . . ? C12 C10 H10 106.4 . . ? P1 C10 H10 106.4 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? 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 C2 Ni1 P1 C10 54.7(2) . . . . ? C3 Ni1 P1 C10 29.15(17) . . . . ? C1 Ni1 P1 C10 32.1(5) . . . . ? Br1 Ni1 P1 C10 -145.50(13) . . . . ? C2 Ni1 P1 C4 -178.86(19) . . . . ? C3 Ni1 P1 C4 155.55(17) . . . . ? C1 Ni1 P1 C4 158.5(5) . . . . ? Br1 Ni1 P1 C4 -19.10(13) . . . . ? C2 Ni1 P1 C7 -66.07(19) . . . . ? C3 Ni1 P1 C7 -91.66(17) . . . . ? C1 Ni1 P1 C7 -88.7(5) . . . . ? Br1 Ni1 P1 C7 93.69(13) . . . . ? C3 Ni1 C1 C2 31.0(2) . . . . ? P1 Ni1 C1 C2 27.9(6) . . . . ? Br1 Ni1 C1 C2 -154.4(2) . . . . ? Ni1 C1 C2 C3 -53.7(3) . . . . ? C3 Ni1 C2 C1 -131.2(4) . . . . ? P1 Ni1 C2 C1 -172.45(18) . . . . ? Br1 Ni1 C2 C1 33.5(3) . . . . ? C1 Ni1 C2 C3 131.2(4) . . . . ? P1 Ni1 C2 C3 -41.3(3) . . . . ? Br1 Ni1 C2 C3 164.67(18) . . . . ? C1 C2 C3 Ni1 55.0(3) . . . . ? C1 Ni1 C3 C2 -30.5(2) . . . . ? P1 Ni1 C3 C2 148.8(2) . . . . ? Br1 Ni1 C3 C2 -51.7(5) . . . . ? C10 P1 C4 C5 68.1(3) . . . . ? C7 P1 C4 C5 176.8(3) . . . . ? Ni1 P1 C4 C5 -64.7(3) . . . . ? P1 C4 C5 C6 -123.7(3) . . . . ? C10 P1 C7 C8 -175.8(3) . . . . ? C4 P1 C7 C8 75.3(3) . . . . ? Ni1 P1 C7 C8 -47.2(3) . . . . ? C10 P1 C7 C9 -52.4(3) . . . . ? C4 P1 C7 C9 -161.3(3) . . . . ? Ni1 P1 C7 C9 76.2(3) . . . . ? C4 P1 C10 C11 51.6(3) . . . . ? C7 P1 C10 C11 -53.6(3) . . . . ? Ni1 P1 C10 C11 -177.0(2) . . . . ? C4 P1 C10 C12 -75.9(3) . . . . ? C7 P1 C10 C12 178.9(2) . . . . ? Ni1 P1 C10 C12 55.4(3) . . . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.855 _refine_diff_density_min -0.542 _refine_diff_density_rms 0.105 #=== END #=== pv0616 ====== Compound 3b in the text data_pv0616 _database_code_depnum_ccdc_archive 'CCDC 638226' _audit_creation_method SHELXL-97 _chemical_name_systematic 'dibromo-bis(allyldiisopropylphosphine)-nickel (II)' _chemical_name_common 'dibromo-bis(allyldiisopropylphosphine)-nickel (ii)' _chemical_melting_point ? _chemical_formula_moiety 'C18 H38 Br2 Ni P2' _chemical_formula_sum 'C18 H38 Br2 Ni P2' _chemical_formula_weight 534.95 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' 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 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_int_tables_number 14 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 8.2979(17) _cell_length_b 15.238(3) _cell_length_c 9.3390(19) _cell_angle_alpha 90.00 _cell_angle_beta 104.40(3) _cell_angle_gamma 90.00 _cell_volume 1143.8(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5182 _cell_measurement_theta_min 2.618 _cell_measurement_theta_max 25.044 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.553 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 548 _exptl_absorpt_coefficient_mu 4.480 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.696 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details '(SADABS; Sheldrick, 2004)' _exptl_special_details ; Bruker SMART APEX 3-circle diffractometer with CCD area detector, sealed X-ray tube, graphite monochromator. A hemisphere of the reciprocal space up to theta(max) = 25.04 deg was measured by omega scan frames with delta(omega) = 0.30 deg and 10 sec per frame, 1700 frames were recorded using program SMART (Bruker). Frame data evaluation and integration were done with program SAINT+(Bruker); Lattice parameters by least-squares refinement of the geometric parameters of the strongest reflections with program SAINT + (Bruker). Correction for absorption and crystal decay (insignificant) were applied by semi-empirical method from equivalents using program SADABS (G.M. Sheldrick, version of 2001, Univ. of Goettingen, Germany). Data reduction was done with program XPREP (BRUKER). ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_source_type 'Bruker SMART APEX' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD area detector' _diffrn_measurement_method '1700 omega scan frames, 0.3 deg, 10 sec' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.0009 _diffrn_reflns_number 7892 _diffrn_reflns_av_R_equivalents 0.0278 _diffrn_reflns_av_sigmaI/netI 0.0236 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.62 _diffrn_reflns_theta_max 25.04 _reflns_number_total 2015 _reflns_number_gt 1979 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SAINT (Bruker, 2001)' _computing_data_reduction 'SAINT (Bruker, 2001)' _computing_structure_solution 'SHELXTL (Sheldrick, 2001)' _computing_structure_refinement 'SHELXTL (Sheldrick, 2001)' _computing_molecular_graphics 'ORTEP-3 vers. 1.08 (Faruggia, 2005)' _computing_publication_material 'SHELXTL (Sheldrick, 2001)' _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^)+(0.0203P)^2^+2.2780P] 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 2015 _refine_ls_number_parameters 110 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0272 _refine_ls_R_factor_gt 0.0265 _refine_ls_wR_factor_ref 0.0592 _refine_ls_wR_factor_gt 0.0588 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _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 0.5000 1.0000 0.01301(12) Uani 1 2 d S . . Br1 Br 0.09304(4) 0.588271(18) 1.20394(3) 0.02182(10) Uani 1 1 d . . . P1 P 0.07445(8) 0.60484(4) 0.85788(7) 0.01395(15) Uani 1 1 d . . . C1 C 0.1050(4) 0.57114(18) 0.6769(3) 0.0191(6) Uani 1 1 d . . . H1A H -0.0003 0.5458 0.6173 0.023 Uiso 1 1 calc R . . H1B H 0.1299 0.6239 0.6244 0.023 Uiso 1 1 calc R . . C2 C 0.2418(4) 0.50547(19) 0.6855(3) 0.0218(6) Uani 1 1 d . . . H2 H 0.2409 0.4544 0.7438 0.026 Uiso 1 1 calc R . . C3 C 0.3625(4) 0.5134(2) 0.6185(3) 0.0281(7) Uani 1 1 d . . . H3A H 0.3674 0.5635 0.5593 0.034 Uiso 1 1 calc R . . H3B H 0.4449 0.4689 0.6292 0.034 Uiso 1 1 calc R . . C4 C -0.0967(3) 0.68519(18) 0.8011(3) 0.0203(6) Uani 1 1 d . . . H4 H -0.0729 0.7218 0.7198 0.024 Uiso 1 1 calc R . . C5 C -0.2620(4) 0.6386(2) 0.7400(3) 0.0264(7) Uani 1 1 d . . . H5A H -0.2868 0.6008 0.8167 0.040 Uiso 1 1 calc R . . H5B H -0.2548 0.6028 0.6546 0.040 Uiso 1 1 calc R . . H5C H -0.3506 0.6822 0.7093 0.040 Uiso 1 1 calc R . . C6 C -0.1103(5) 0.7468(2) 0.9264(4) 0.0412(9) Uani 1 1 d . . . H6A H -0.2038 0.7872 0.8914 0.062 Uiso 1 1 calc R . . H6B H -0.0070 0.7805 0.9589 0.062 Uiso 1 1 calc R . . H6C H -0.1289 0.7124 1.0095 0.062 Uiso 1 1 calc R . . C7 C 0.2600(3) 0.67128(18) 0.9419(3) 0.0184(6) Uani 1 1 d . . . H7 H 0.2344 0.7032 1.0272 0.022 Uiso 1 1 calc R . . C8 C 0.4112(4) 0.6138(2) 1.0056(3) 0.0242(6) Uani 1 1 d . . . H8A H 0.4435 0.5828 0.9251 0.036 Uiso 1 1 calc R . . H8B H 0.3836 0.5711 1.0742 0.036 Uiso 1 1 calc R . . H8C H 0.5038 0.6507 1.0584 0.036 Uiso 1 1 calc R . . C9 C 0.3000(4) 0.7413(2) 0.8386(3) 0.0321(7) Uani 1 1 d . . . H9A H 0.3897 0.7791 0.8939 0.048 Uiso 1 1 calc R . . H9B H 0.2007 0.7768 0.7984 0.048 Uiso 1 1 calc R . . H9C H 0.3355 0.7128 0.7575 0.048 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 0.0141(2) 0.0118(2) 0.0133(2) -0.00025(17) 0.00375(18) -0.00115(18) Br1 0.03031(18) 0.01933(16) 0.01725(15) -0.00519(10) 0.00863(12) -0.00922(11) P1 0.0143(3) 0.0129(3) 0.0142(3) 0.0008(3) 0.0027(3) -0.0006(3) C1 0.0235(15) 0.0203(14) 0.0142(13) -0.0005(11) 0.0061(11) -0.0037(12) C2 0.0256(16) 0.0204(15) 0.0204(14) -0.0028(11) 0.0076(12) -0.0017(12) C3 0.0266(17) 0.0330(17) 0.0267(16) -0.0033(13) 0.0103(13) -0.0013(14) C4 0.0200(14) 0.0180(14) 0.0206(14) 0.0025(11) 0.0005(11) 0.0030(12) C5 0.0157(14) 0.0270(16) 0.0349(17) 0.0007(13) 0.0033(12) 0.0035(13) C6 0.044(2) 0.0323(19) 0.0364(18) -0.0086(15) -0.0099(15) 0.0268(16) C7 0.0168(14) 0.0182(14) 0.0189(13) -0.0013(11) 0.0023(11) -0.0056(11) C8 0.0178(15) 0.0294(16) 0.0243(15) -0.0026(12) 0.0035(12) -0.0013(12) C9 0.0334(18) 0.0306(17) 0.0304(17) 0.0047(14) 0.0043(14) -0.0148(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 P1 2.2590(8) . ? Ni1 P1 2.2590(7) 3_567 ? Ni1 Br1 2.3025(5) 3_567 ? Ni1 Br1 2.3025(5) . ? P1 C1 1.843(3) . ? P1 C7 1.847(3) . ? P1 C4 1.850(3) . ? C1 C2 1.500(4) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.312(4) . ? C2 H2 0.9500 . ? C3 H3A 0.9500 . ? C3 H3B 0.9500 . ? C4 C5 1.523(4) . ? C4 C6 1.527(4) . ? C4 H4 1.0000 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.525(4) . ? C7 C9 1.529(4) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? 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 P1 Ni1 P1 180.0 . 3_567 ? P1 Ni1 Br1 89.34(2) 3_567 3_567 ? P1 Ni1 Br1 89.34(2) . . ? P1 Ni1 Br1 90.66(2) 3_567 . ? Br1 Ni1 Br1 180.0 3_567 . ? C1 P1 C7 104.62(13) . . ? C1 P1 C4 101.07(13) . . ? C7 P1 C4 104.97(13) . . ? C1 P1 Ni1 117.50(9) . . ? C7 P1 Ni1 117.31(9) . . ? C4 P1 Ni1 109.51(10) . . ? C2 C1 P1 114.28(19) . . ? C2 C1 H1A 108.7 . . ? P1 C1 H1A 108.7 . . ? C2 C1 H1B 108.7 . . ? P1 C1 H1B 108.7 . . ? H1A C1 H1B 107.6 . . ? C3 C2 C1 124.8(3) . . ? C3 C2 H2 117.6 . . ? C1 C2 H2 117.6 . . ? C2 C3 H3A 120.0 . . ? C2 C3 H3B 120.0 . . ? H3A C3 H3B 120.0 . . ? C5 C4 C6 110.0(3) . . ? C5 C4 P1 110.7(2) . . ? C6 C4 P1 112.65(19) . . ? C5 C4 H4 107.7 . . ? C6 C4 H4 107.7 . . ? P1 C4 H4 107.7 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 C9 111.1(2) . . ? C8 C7 P1 111.67(19) . . ? C9 C7 P1 113.8(2) . . ? C8 C7 H7 106.6 . . ? C9 C7 H7 106.6 . . ? P1 C7 H7 106.6 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? 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 P1 Ni1 P1 C1 92(100) 3_567 . . . ? Br1 Ni1 P1 C1 -20.22(11) 3_567 . . . ? Br1 Ni1 P1 C1 159.78(11) . . . . ? P1 Ni1 P1 C7 -34(100) 3_567 . . . ? Br1 Ni1 P1 C7 -146.31(10) 3_567 . . . ? Br1 Ni1 P1 C7 33.69(10) . . . . ? P1 Ni1 P1 C4 -153(100) 3_567 . . . ? Br1 Ni1 P1 C4 94.25(10) 3_567 . . . ? Br1 Ni1 P1 C4 -85.75(10) . . . . ? C7 P1 C1 C2 70.1(2) . . . . ? C4 P1 C1 C2 178.9(2) . . . . ? Ni1 P1 C1 C2 -62.0(2) . . . . ? P1 C1 C2 C3 -129.2(3) . . . . ? C1 P1 C4 C5 75.8(2) . . . . ? C7 P1 C4 C5 -175.6(2) . . . . ? Ni1 P1 C4 C5 -48.8(2) . . . . ? C1 P1 C4 C6 -160.5(2) . . . . ? C7 P1 C4 C6 -51.9(3) . . . . ? Ni1 P1 C4 C6 74.9(2) . . . . ? C1 P1 C7 C8 -78.3(2) . . . . ? C4 P1 C7 C8 175.77(19) . . . . ? Ni1 P1 C7 C8 53.9(2) . . . . ? C1 P1 C7 C9 48.5(2) . . . . ? C4 P1 C7 C9 -57.5(2) . . . . ? Ni1 P1 C7 C9 -179.31(19) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.438 _refine_diff_density_min -0.371 _refine_diff_density_rms 0.080 #==== END #=== pv0611 ====== Compound 5b in the text data_pv0611 _database_code_depnum_ccdc_archive 'CCDC 638227' _audit_creation_method SHELXL-97 _chemical_name_systematic ; (Trihapto-2-methyl-allyl)-bis(diisopropyl-allyl-phosphino)-nickel (II) tetrakis{3,5-bis(trifluoromethyl)phenyl}borate ; _chemical_name_common ; (Trihapto-2-methyl-allyl)-bis(diisopropyl-allyl-phosphino)- nickel (ii) tetrakis(3,5-bis(trifluoromethyl)phenyl)borate ; _chemical_melting_point ? _chemical_formula_moiety 'C22 H45 Ni P2 1+; C32 H12 B F24 1-' _chemical_formula_sum 'C54 H57 B F24 Ni P2' _chemical_formula_weight 1293.46 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' 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_int_tables_number 14 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 12.799(3) _cell_length_b 11.980(2) _cell_length_c 37.938(8) _cell_angle_alpha 90.00 _cell_angle_beta 99.13(3) _cell_angle_gamma 90.00 _cell_volume 5743(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8763 _cell_measurement_theta_min 2.175 _cell_measurement_theta_max 24.965 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.496 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2640 _exptl_absorpt_coefficient_mu 0.508 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.851 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details '(SADABS; Sheldrick, 2004)' _exptl_special_details ; Bruker SMART APEX 3-circle diffractometer with CCD area detector, sealed X-ray tube, graphite monochromator. A hemisphere of the reciprocal space up to theta(max) = 25.01 deg was measured by omega scan frames with delta(omega) = 0.30 deg and 10 sec per frame, 1700 frames were recorded using program SMART (Bruker). Frame data evaluation and integration were done with program SAINT+(Bruker); Lattice parameters by least-squares refinement of the geometric parameters of the strongest reflections with program SAINT + (Bruker). Correction for absorption and crystal decay (insignificant) were applied by semi-empirical method from equivalents using program SADABS (G.M. Sheldrick, version of 2001, Univ. of Goettingen, Germany). Data reduction was done with program XPREP (BRUKER). ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_source_type 'Bruker SMART APEX' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method '1700 omega scan frames, 0.3 deg, 10 sec' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.0001 _diffrn_reflns_number 35584 _diffrn_reflns_av_R_equivalents 0.0479 _diffrn_reflns_av_sigmaI/netI 0.0486 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -44 _diffrn_reflns_limit_l_max 45 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 25.01 _reflns_number_total 10098 _reflns_number_gt 9238 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SAINT (Bruker, 2001)' _computing_data_reduction 'SAINT (Bruker, 2001)' _computing_structure_solution 'SHELXTL (Sheldrick, 2001)' _computing_structure_refinement 'SHELXTL (Sheldrick, 2001)' _computing_molecular_graphics 'ORTEP-3 vers. 1.08 (Faruggia, 2005)' _computing_publication_material 'SHELXTL (Sheldrick, 2001)' _refine_special_details ; 1) 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. 2) Two of CF~3~ groups were splitted and refined with complementary ocuppation factors. ; _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^)+(0.0435P)^2^+26.3846P] 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 10098 _refine_ls_number_parameters 768 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0860 _refine_ls_R_factor_gt 0.0770 _refine_ls_wR_factor_ref 0.1594 _refine_ls_wR_factor_gt 0.1540 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.071 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.78122(4) 0.39740(5) 0.136310(15) 0.01839(15) Uani 1 1 d . . . P1 P 0.90873(9) 0.43305(9) 0.10443(3) 0.0185(2) Uani 1 1 d . . . P2 P 0.77004(9) 0.53450(10) 0.17564(3) 0.0228(3) Uani 1 1 d . . . C1 C 0.7624(4) 0.2427(4) 0.11308(13) 0.0268(11) Uani 1 1 d . . . H1A H 0.7753 0.2370 0.0881 0.032 Uiso 1 1 calc R . . H1B H 0.7897 0.1784 0.1282 0.032 Uiso 1 1 calc R . . C2 C 0.6644(3) 0.2859(4) 0.11826(13) 0.0254(10) Uani 1 1 d . . . C3 C 0.6560(4) 0.3183(4) 0.15305(14) 0.0296(11) Uani 1 1 d . . . H3A H 0.6732 0.2611 0.1719 0.036 Uiso 1 1 calc R . . H3B H 0.5944 0.3654 0.1560 0.036 Uiso 1 1 calc R . . C4 C 0.5826(4) 0.3171(4) 0.08703(15) 0.0353(12) Uani 1 1 d . . . H4A H 0.5267 0.2604 0.0837 0.053 Uiso 1 1 calc R . . H4B H 0.6157 0.3216 0.0655 0.053 Uiso 1 1 calc R . . H4C H 0.5519 0.3897 0.0915 0.053 Uiso 1 1 calc R . . C5 C 0.8485(3) 0.4355(4) 0.05675(11) 0.0224(10) Uani 1 1 d . . . H5 H 0.8159 0.3604 0.0511 0.027 Uiso 1 1 calc R . . C6 C 0.7582(4) 0.5208(4) 0.05086(12) 0.0280(11) Uani 1 1 d . . . H6A H 0.7873 0.5963 0.0546 0.042 Uiso 1 1 calc R . . H6B H 0.7093 0.5066 0.0678 0.042 Uiso 1 1 calc R . . H6C H 0.7201 0.5141 0.0264 0.042 Uiso 1 1 calc R . . C7 C 0.9248(4) 0.4556(4) 0.03002(12) 0.0292(11) Uani 1 1 d . . . H7A H 0.8886 0.4397 0.0058 0.044 Uiso 1 1 calc R . . H7B H 0.9863 0.4064 0.0357 0.044 Uiso 1 1 calc R . . H7C H 0.9482 0.5336 0.0315 0.044 Uiso 1 1 calc R . . C8 C 1.0213(3) 0.3341(4) 0.10885(13) 0.0249(10) Uani 1 1 d . . . H8 H 1.0795 0.3715 0.0986 0.030 Uiso 1 1 calc R . . C9 C 0.9994(4) 0.2227(4) 0.08939(14) 0.0325(12) Uani 1 1 d . . . H9A H 1.0661 0.1823 0.0896 0.049 Uiso 1 1 calc R . . H9B H 0.9664 0.2364 0.0647 0.049 Uiso 1 1 calc R . . H9C H 0.9516 0.1778 0.1014 0.049 Uiso 1 1 calc R . . C10 C 1.0613(4) 0.3159(4) 0.14862(13) 0.0333(12) Uani 1 1 d . . . H10A H 1.0031 0.2891 0.1603 0.050 Uiso 1 1 calc R . . H10B H 1.0882 0.3866 0.1595 0.050 Uiso 1 1 calc R . . H10C H 1.1183 0.2604 0.1515 0.050 Uiso 1 1 calc R . . C11 C 0.9765(4) 0.5701(4) 0.11241(13) 0.0248(10) Uani 1 1 d . . . H11A H 0.9268 0.6281 0.1013 0.030 Uiso 1 1 calc R . . H11B H 0.9879 0.5837 0.1385 0.030 Uiso 1 1 calc R . . C12 C 1.0795(4) 0.5891(4) 0.09978(15) 0.0332(12) Uani 1 1 d . . . H12 H 1.0824 0.5796 0.0751 0.040 Uiso 1 1 calc R . . C13 C 1.1662(4) 0.6181(4) 0.12098(15) 0.0354(12) Uani 1 1 d . . . H13A H 1.1654 0.6281 0.1458 0.042 Uiso 1 1 calc R . . H13B H 1.2299 0.6292 0.1116 0.042 Uiso 1 1 calc R . . C14 C 0.7399(4) 0.4780(4) 0.21850(13) 0.0323(11) Uani 1 1 d . . . H14 H 0.6703 0.4386 0.2131 0.039 Uiso 1 1 calc R . . C15 C 0.8222(5) 0.3907(5) 0.23369(16) 0.0455(14) Uani 1 1 d . . . H15A H 0.8903 0.4275 0.2415 0.068 Uiso 1 1 calc R . . H15B H 0.8301 0.3356 0.2152 0.068 Uiso 1 1 calc R . . H15C H 0.7990 0.3531 0.2540 0.068 Uiso 1 1 calc R . . C16 C 0.7291(5) 0.5659(5) 0.24692(14) 0.0428(14) Uani 1 1 d . . . H16A H 0.7055 0.5300 0.2675 0.064 Uiso 1 1 calc R . . H16B H 0.6772 0.6222 0.2369 0.064 Uiso 1 1 calc R . . H16C H 0.7978 0.6018 0.2545 0.064 Uiso 1 1 calc R . . C17 C 0.6638(4) 0.6393(4) 0.16086(13) 0.0285(11) Uani 1 1 d . . . H17 H 0.6624 0.6921 0.1812 0.034 Uiso 1 1 calc R . . C18 C 0.5552(4) 0.5883(4) 0.15229(16) 0.0396(13) Uani 1 1 d . . . H18A H 0.5022 0.6477 0.1475 0.059 Uiso 1 1 calc R . . H18B H 0.5409 0.5435 0.1726 0.059 Uiso 1 1 calc R . . H18C H 0.5518 0.5404 0.1312 0.059 Uiso 1 1 calc R . . C19 C 0.6884(5) 0.7082(4) 0.12924(14) 0.0405(13) Uani 1 1 d . . . H19A H 0.6885 0.6594 0.1085 0.061 Uiso 1 1 calc R . . H19B H 0.7581 0.7432 0.1355 0.061 Uiso 1 1 calc R . . H19C H 0.6345 0.7662 0.1235 0.061 Uiso 1 1 calc R . . C20 C 0.8801(4) 0.6314(4) 0.19030(14) 0.0316(11) Uani 1 1 d . . . H20A H 0.8950 0.6729 0.1691 0.038 Uiso 1 1 calc R . . H20B H 0.8558 0.6865 0.2067 0.038 Uiso 1 1 calc R . . C21 C 0.9806(4) 0.5831(5) 0.20834(15) 0.0405(13) Uani 1 1 d . . . H21 H 1.0066 0.5177 0.1985 0.049 Uiso 1 1 calc R . . C22 C 1.0357(5) 0.6261(6) 0.23724(18) 0.0577(18) Uani 1 1 d . . . H22A H 1.0113 0.6915 0.2475 0.069 Uiso 1 1 calc R . . H22B H 1.0999 0.5919 0.2479 0.069 Uiso 1 1 calc R . . F1 F 0.6350(2) 1.1038(2) 0.03420(8) 0.0398(7) Uani 1 1 d . . . F2 F 0.6818(3) 0.9592(3) 0.00790(8) 0.0493(9) Uani 1 1 d . . . F3 F 0.7421(2) 0.9884(3) 0.06291(8) 0.0462(8) Uani 1 1 d . . . F4 F 0.3407(3) 0.6396(3) 0.01922(13) 0.0813(14) Uani 1 1 d . . . F5 F 0.4974(4) 0.6080(4) 0.01585(19) 0.143(3) Uani 1 1 d . . . F6 F 0.4372(5) 0.5766(3) 0.06286(12) 0.1021(19) Uani 1 1 d . . . F7 F 0.2249(2) 1.4362(2) 0.04750(7) 0.0401(8) Uani 1 1 d . . . F8 F 0.3491(3) 1.3518(3) 0.02817(8) 0.0511(9) Uani 1 1 d . . . F9 F 0.1975(4) 1.2768(3) 0.02352(9) 0.0773(14) Uani 1 1 d . . . F10 F 0.2973(2) 1.3001(2) 0.20194(7) 0.0325(7) Uani 1 1 d . . . F11 F 0.4497(2) 1.3607(2) 0.19512(7) 0.0295(6) Uani 1 1 d . . . F12 F 0.3108(3) 1.4551(2) 0.17471(7) 0.0399(8) Uani 1 1 d . . . F13A F 0.0259(14) 1.0467(8) 0.1775(4) 0.082(3) Uani 0.740(16) 1 d PD A 1 F14A F -0.0074(8) 0.8673(11) 0.1797(4) 0.064(3) Uani 0.740(16) 1 d PD A 1 F15A F -0.1047(4) 0.9900(11) 0.14766(19) 0.082(3) Uani 0.740(16) 1 d PD A 1 F16A F -0.0636(10) 0.9178(10) 0.0194(3) 0.046(2) Uani 0.745(19) 1 d PD B 1 F17A F 0.0745(6) 0.8412(11) 0.0069(2) 0.072(3) Uani 0.745(19) 1 d PD B 1 F18A F -0.0328(10) 0.7433(8) 0.0347(3) 0.104(4) Uani 0.745(19) 1 d PD B 1 F19 F 0.3881(3) 0.7438(3) 0.25845(7) 0.0450(8) Uani 1 1 d . . . F20 F 0.3002(2) 0.6765(2) 0.21095(8) 0.0371(7) Uani 1 1 d . . . F21 F 0.4579(2) 0.6212(3) 0.22910(10) 0.0496(9) Uani 1 1 d . . . F22 F 0.7617(2) 0.8913(3) 0.20153(10) 0.0477(9) Uani 1 1 d . . . F23 F 0.7123(2) 1.0597(3) 0.19265(9) 0.0503(9) Uani 1 1 d . . . F24 F 0.7109(2) 0.9841(3) 0.24315(7) 0.0422(8) Uani 1 1 d . . . F13B F 0.039(5) 1.019(3) 0.1839(11) 0.082(3) Uani 0.260(16) 1 d PD A 2 F14B F 0.023(3) 0.880(4) 0.1812(14) 0.064(3) Uani 0.260(16) 1 d PD A 2 F15B F -0.1034(14) 0.920(3) 0.1469(6) 0.082(3) Uani 0.260(16) 1 d PD A 2 F16B F -0.062(3) 0.904(3) 0.0101(8) 0.046(2) Uani 0.255(19) 1 d PD B 2 F17B F 0.0636(19) 0.785(3) 0.0186(7) 0.072(3) Uani 0.255(19) 1 d PD B 2 F18B F -0.069(3) 0.779(2) 0.0409(9) 0.104(4) Uani 0.255(19) 1 d PD B 2 C23 C 0.4205(3) 0.9234(3) 0.08461(11) 0.0173(9) Uani 1 1 d . . . C24 C 0.5026(3) 0.9802(4) 0.07206(11) 0.0167(9) Uani 1 1 d . . . H24 H 0.5171 1.0551 0.0794 0.020 Uiso 1 1 calc R . . C25 C 0.5638(3) 0.9312(4) 0.04920(11) 0.0199(9) Uani 1 1 d . . . C26 C 0.5449(4) 0.8226(4) 0.03751(12) 0.0248(10) Uani 1 1 d . . . H26 H 0.5865 0.7891 0.0217 0.030 Uiso 1 1 calc R . . C27 C 0.4639(4) 0.7637(4) 0.04934(12) 0.0233(10) Uani 1 1 d . . . C28 C 0.4054(3) 0.8126(4) 0.07276(11) 0.0197(9) Uani 1 1 d . . . H28 H 0.3524 0.7693 0.0813 0.024 Uiso 1 1 calc R . . C29 C 0.6550(4) 0.9946(4) 0.03830(12) 0.0272(11) Uani 1 1 d . . . C30 C 0.4379(4) 0.6479(4) 0.03658(14) 0.0332(12) Uani 1 1 d . . . C31 C 0.3494(3) 1.1104(3) 0.11412(11) 0.0147(8) Uani 1 1 d . . . C32 C 0.3179(3) 1.1664(3) 0.08196(11) 0.0168(9) Uani 1 1 d . . . H32 H 0.3094 1.1251 0.0603 0.020 Uiso 1 1 calc R . . C33 C 0.2987(3) 1.2808(3) 0.08054(11) 0.0166(9) Uani 1 1 d . . . C34 C 0.3102(3) 1.3440(4) 0.11167(11) 0.0188(9) Uani 1 1 d . . . H34 H 0.2978 1.4222 0.1109 0.023 Uiso 1 1 calc R . . C35 C 0.3404(3) 1.2893(4) 0.14392(11) 0.0185(9) Uani 1 1 d . . . C36 C 0.3606(3) 1.1752(3) 0.14498(11) 0.0154(8) Uani 1 1 d . . . H36 H 0.3827 1.1404 0.1674 0.018 Uiso 1 1 calc R . . C37 C 0.2669(4) 1.3353(4) 0.04514(12) 0.0233(10) Uani 1 1 d . . . C38 C 0.3496(3) 1.3519(4) 0.17855(12) 0.0216(10) Uani 1 1 d . . . C39 C 0.2282(3) 0.9396(3) 0.10731(12) 0.0187(9) Uani 1 1 d . . . C40 C 0.1654(3) 0.9559(4) 0.13408(13) 0.0231(10) Uani 1 1 d . . . H40 H 0.1984 0.9804 0.1570 0.028 Uiso 1 1 calc R . . C41 C 0.0571(4) 0.9376(4) 0.12844(15) 0.0320(12) Uani 1 1 d . A . C42 C 0.0063(4) 0.9021(4) 0.09563(16) 0.0371(13) Uani 1 1 d . . . H42 H -0.0678 0.8885 0.0918 0.044 Uiso 1 1 calc R . . C43 C 0.0650(4) 0.8866(4) 0.06824(15) 0.0331(12) Uani 1 1 d . B . C44 C 0.1738(4) 0.9057(4) 0.07409(13) 0.0244(10) Uani 1 1 d . . . H44 H 0.2123 0.8954 0.0549 0.029 Uiso 1 1 calc R . . C45 C -0.0050(4) 0.9550(5) 0.15805(17) 0.0435(15) Uani 1 1 d D . . C46 C 0.0093(5) 0.8460(5) 0.03290(17) 0.0472(16) Uani 1 1 d D . . C47 C 0.4164(3) 0.9259(3) 0.15272(11) 0.0153(9) Uani 1 1 d . . . C48 C 0.3789(3) 0.8425(3) 0.17284(11) 0.0178(9) Uani 1 1 d . . . H48 H 0.3105 0.8124 0.1651 0.021 Uiso 1 1 calc R . . C49 C 0.4390(3) 0.8016(3) 0.20415(11) 0.0167(9) Uani 1 1 d . . . C50 C 0.5391(3) 0.8426(3) 0.21619(11) 0.0185(9) Uani 1 1 d . . . H50 H 0.5795 0.8152 0.2376 0.022 Uiso 1 1 calc R . . C51 C 0.5793(3) 0.9249(3) 0.19626(11) 0.0156(9) Uani 1 1 d . . . C52 C 0.5196(3) 0.9651(3) 0.16525(11) 0.0170(9) Uani 1 1 d . . . H52 H 0.5490 1.0209 0.1520 0.020 Uiso 1 1 calc R . . C53 C 0.3961(3) 0.7117(4) 0.22553(12) 0.0226(10) Uani 1 1 d . . . C54 C 0.6904(3) 0.9649(4) 0.20835(12) 0.0221(10) Uani 1 1 d . . . B1 B 0.3544(4) 0.9736(4) 0.11464(13) 0.0159(10) 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 0.0173(3) 0.0165(3) 0.0220(3) 0.0000(2) 0.0053(2) -0.0020(2) P1 0.0160(5) 0.0199(6) 0.0198(6) 0.0015(5) 0.0032(4) -0.0016(4) P2 0.0245(6) 0.0218(6) 0.0224(6) -0.0012(5) 0.0043(5) -0.0011(5) C1 0.030(3) 0.015(2) 0.037(3) -0.003(2) 0.011(2) -0.0033(19) C2 0.020(2) 0.014(2) 0.043(3) -0.008(2) 0.010(2) -0.0102(18) C3 0.029(3) 0.017(2) 0.047(3) -0.001(2) 0.021(2) -0.008(2) C4 0.022(2) 0.027(3) 0.056(3) -0.009(2) 0.002(2) -0.004(2) C5 0.025(2) 0.021(2) 0.020(2) -0.0026(18) 0.0003(19) -0.0027(19) C6 0.032(3) 0.029(3) 0.021(2) 0.000(2) 0.000(2) -0.002(2) C7 0.035(3) 0.032(3) 0.021(2) -0.002(2) 0.007(2) -0.001(2) C8 0.016(2) 0.027(3) 0.033(3) 0.004(2) 0.007(2) 0.0024(19) C9 0.028(3) 0.029(3) 0.042(3) 0.003(2) 0.010(2) 0.007(2) C10 0.021(2) 0.037(3) 0.040(3) 0.007(2) 0.001(2) 0.008(2) C11 0.022(2) 0.023(2) 0.029(3) 0.003(2) 0.002(2) -0.0046(19) C12 0.032(3) 0.028(3) 0.041(3) 0.006(2) 0.012(2) -0.001(2) C13 0.023(3) 0.030(3) 0.052(3) 0.005(2) 0.004(2) -0.008(2) C14 0.035(3) 0.036(3) 0.028(3) 0.005(2) 0.009(2) 0.000(2) C15 0.052(4) 0.042(3) 0.041(3) 0.013(3) 0.002(3) 0.002(3) C16 0.047(3) 0.048(3) 0.033(3) -0.002(3) 0.007(3) 0.004(3) C17 0.038(3) 0.022(2) 0.026(3) -0.006(2) 0.006(2) 0.006(2) C18 0.035(3) 0.029(3) 0.052(3) -0.009(3) -0.002(3) 0.010(2) C19 0.056(4) 0.029(3) 0.035(3) 0.003(2) 0.002(3) 0.014(3) C20 0.032(3) 0.027(3) 0.033(3) -0.006(2) 0.000(2) -0.003(2) C21 0.031(3) 0.047(3) 0.043(3) 0.006(3) 0.003(2) 0.003(2) C22 0.039(3) 0.060(4) 0.066(4) -0.005(3) -0.017(3) 0.000(3) F1 0.0351(16) 0.0341(17) 0.0536(19) 0.0030(14) 0.0176(14) -0.0055(13) F2 0.053(2) 0.057(2) 0.0455(19) -0.0228(16) 0.0318(16) -0.0174(17) F3 0.0227(15) 0.066(2) 0.0482(19) 0.0098(17) -0.0013(14) -0.0085(15) F4 0.076(3) 0.037(2) 0.112(4) -0.027(2) -0.042(3) -0.0040(19) F5 0.139(5) 0.072(3) 0.256(7) -0.116(4) 0.149(5) -0.059(3) F6 0.196(6) 0.0206(19) 0.073(3) -0.0005(19) -0.032(3) -0.021(3) F7 0.0537(19) 0.0369(17) 0.0303(16) 0.0158(13) 0.0086(14) 0.0235(15) F8 0.055(2) 0.069(2) 0.0347(17) 0.0262(16) 0.0252(16) 0.0305(18) F9 0.117(3) 0.049(2) 0.044(2) 0.0205(17) -0.056(2) -0.041(2) F10 0.0300(15) 0.0442(17) 0.0249(14) -0.0110(13) 0.0093(12) -0.0059(13) F11 0.0237(14) 0.0399(16) 0.0234(14) -0.0108(12) -0.0015(11) -0.0056(12) F12 0.060(2) 0.0259(16) 0.0293(15) -0.0093(12) -0.0061(14) 0.0190(14) F13A 0.115(6) 0.035(6) 0.123(6) -0.009(5) 0.098(5) -0.007(6) F14A 0.075(7) 0.047(4) 0.081(3) 0.027(3) 0.043(6) -0.006(5) F15A 0.036(2) 0.132(9) 0.085(3) 0.049(5) 0.031(2) 0.052(4) F16A 0.049(2) 0.049(4) 0.030(5) 0.000(4) -0.019(4) 0.008(2) F17A 0.053(3) 0.100(7) 0.052(5) -0.044(5) -0.029(3) 0.019(4) F18A 0.159(8) 0.017(4) 0.099(5) 0.013(4) -0.095(6) -0.034(4) F19 0.066(2) 0.0483(19) 0.0245(16) -0.0064(14) 0.0188(15) -0.0278(17) F20 0.0376(17) 0.0348(16) 0.0352(16) 0.0115(13) -0.0060(13) -0.0159(13) F21 0.0449(18) 0.0324(17) 0.077(2) 0.0321(17) 0.0255(17) 0.0142(15) F22 0.0201(14) 0.0430(19) 0.079(2) -0.0308(17) 0.0065(15) 0.0021(13) F23 0.0342(17) 0.0451(19) 0.064(2) 0.0272(17) -0.0169(16) -0.0176(15) F24 0.0334(16) 0.065(2) 0.0259(15) -0.0107(15) -0.0018(13) -0.0146(15) F13B 0.115(6) 0.035(6) 0.123(6) -0.009(5) 0.098(5) -0.007(6) F14B 0.075(7) 0.047(4) 0.081(3) 0.027(3) 0.043(6) -0.006(5) F15B 0.036(2) 0.132(9) 0.085(3) 0.049(5) 0.031(2) 0.052(4) F16B 0.049(2) 0.049(4) 0.030(5) 0.000(4) -0.019(4) 0.008(2) F17B 0.053(3) 0.100(7) 0.052(5) -0.044(5) -0.029(3) 0.019(4) F18B 0.159(8) 0.017(4) 0.099(5) 0.013(4) -0.095(6) -0.034(4) C23 0.016(2) 0.016(2) 0.017(2) 0.0013(17) -0.0047(17) 0.0029(17) C24 0.016(2) 0.017(2) 0.016(2) -0.0023(17) -0.0034(17) -0.0001(17) C25 0.022(2) 0.021(2) 0.016(2) -0.0015(18) -0.0022(18) 0.0012(18) C26 0.023(2) 0.028(3) 0.022(2) -0.006(2) -0.0017(19) 0.009(2) C27 0.024(2) 0.019(2) 0.024(2) -0.0034(19) -0.0039(19) 0.0047(19) C28 0.020(2) 0.019(2) 0.020(2) 0.0001(18) 0.0000(18) 0.0013(18) C29 0.030(3) 0.031(3) 0.021(2) -0.002(2) 0.005(2) 0.004(2) C30 0.035(3) 0.024(3) 0.040(3) -0.013(2) 0.001(2) 0.000(2) C31 0.0084(18) 0.018(2) 0.018(2) 0.0015(17) 0.0007(16) -0.0017(16) C32 0.013(2) 0.019(2) 0.017(2) -0.0017(17) 0.0022(17) -0.0033(17) C33 0.0103(19) 0.020(2) 0.019(2) 0.0038(17) 0.0000(17) -0.0023(16) C34 0.015(2) 0.014(2) 0.026(2) 0.0012(18) 0.0016(18) 0.0018(17) C35 0.011(2) 0.022(2) 0.022(2) -0.0021(18) 0.0008(17) 0.0004(17) C36 0.015(2) 0.016(2) 0.014(2) 0.0008(16) 0.0001(16) 0.0017(16) C37 0.025(2) 0.020(2) 0.023(2) 0.0008(19) -0.002(2) 0.0009(19) C38 0.021(2) 0.019(2) 0.024(2) -0.0002(19) 0.0002(19) 0.0000(18) C39 0.017(2) 0.011(2) 0.026(2) 0.0073(17) -0.0025(18) 0.0009(17) C40 0.020(2) 0.017(2) 0.031(3) 0.0055(19) 0.002(2) 0.0022(18) C41 0.023(2) 0.022(2) 0.050(3) 0.015(2) 0.004(2) 0.000(2) C42 0.017(2) 0.027(3) 0.064(4) 0.015(3) -0.005(2) 0.000(2) C43 0.031(3) 0.011(2) 0.051(3) 0.001(2) -0.013(2) -0.001(2) C44 0.022(2) 0.016(2) 0.031(3) 0.0014(19) -0.007(2) 0.0030(18) C45 0.022(3) 0.050(4) 0.061(4) 0.020(3) 0.015(3) 0.004(2) C46 0.039(3) 0.030(3) 0.061(4) -0.004(3) -0.027(3) -0.001(3) C47 0.017(2) 0.015(2) 0.014(2) -0.0030(16) 0.0014(17) 0.0040(16) C48 0.015(2) 0.015(2) 0.024(2) -0.0038(18) 0.0026(18) 0.0001(17) C49 0.023(2) 0.010(2) 0.017(2) -0.0008(17) 0.0058(18) 0.0032(17) C50 0.023(2) 0.016(2) 0.016(2) -0.0029(17) 0.0003(18) 0.0017(18) C51 0.018(2) 0.014(2) 0.014(2) -0.0058(16) 0.0011(17) 0.0035(17) C52 0.017(2) 0.016(2) 0.018(2) -0.0023(17) 0.0042(17) 0.0021(17) C53 0.020(2) 0.024(2) 0.022(2) -0.0008(19) -0.0015(19) 0.0013(19) C54 0.024(2) 0.022(2) 0.020(2) 0.0002(19) 0.0030(19) 0.0037(19) B1 0.015(2) 0.015(2) 0.017(2) -0.0012(19) 0.0006(19) -0.0039(19) _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 C2 2.040(4) . ? Ni1 C3 2.047(4) . ? Ni1 C1 2.049(4) . ? Ni1 P1 2.2215(13) . ? Ni1 P2 2.2386(13) . ? P1 C5 1.850(4) . ? P1 C8 1.853(5) . ? P1 C11 1.859(5) . ? P2 C20 1.842(5) . ? P2 C14 1.858(5) . ? P2 C17 1.870(5) . ? C1 C2 1.399(6) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.396(7) . ? C2 C4 1.499(7) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.533(6) . ? C5 C7 1.534(6) . ? C5 H5 1.0000 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.530(7) . ? C8 C10 1.530(7) . ? C8 H8 1.0000 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.489(6) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.310(7) . ? C12 H12 0.9500 . ? C13 H13A 0.9500 . ? C13 H13B 0.9500 . ? C14 C16 1.529(7) . ? C14 C15 1.531(7) . ? C14 H14 1.0000 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.506(7) . ? C17 C19 1.530(7) . ? C17 H17 1.0000 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.475(7) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.311(8) . ? C21 H21 0.9500 . ? C22 H22A 0.9500 . ? C22 H22B 0.9500 . ? F1 C29 1.338(6) . ? F2 C29 1.324(5) . ? F3 C29 1.337(5) . ? F4 C30 1.315(6) . ? F5 C30 1.271(6) . ? F6 C30 1.314(7) . ? F7 C37 1.332(5) . ? F8 C37 1.332(5) . ? F9 C37 1.312(5) . ? F10 C38 1.345(5) . ? F11 C38 1.339(5) . ? F12 C38 1.332(5) . ? F13A C45 1.347(13) . ? F14A C45 1.338(12) . ? F15A C45 1.341(8) . ? F16A C46 1.313(11) . ? F17A C46 1.389(11) . ? F18A C46 1.350(10) . ? F19 C53 1.326(5) . ? F20 C53 1.332(5) . ? F21 C53 1.337(5) . ? F22 C54 1.324(5) . ? F23 C54 1.333(5) . ? F24 C54 1.325(5) . ? F13B C45 1.30(4) . ? F14B C45 1.27(3) . ? F15B C45 1.33(2) . ? F16B C46 1.35(3) . ? F17B C46 1.19(2) . ? F18B C46 1.35(3) . ? C23 C24 1.397(6) . ? C23 C28 1.406(6) . ? C23 B1 1.638(6) . ? C24 C25 1.388(6) . ? C24 H24 0.9500 . ? C25 C26 1.383(6) . ? C25 C29 1.504(6) . ? C26 C27 1.386(7) . ? C26 H26 0.9500 . ? C27 C28 1.380(6) . ? C27 C30 1.490(6) . ? C28 H28 0.9500 . ? C31 C36 1.393(6) . ? C31 C32 1.395(6) . ? C31 B1 1.640(6) . ? C32 C33 1.392(6) . ? C32 H32 0.9500 . ? C33 C34 1.391(6) . ? C33 C37 1.491(6) . ? C34 C35 1.388(6) . ? C34 H34 0.9500 . ? C35 C36 1.390(6) . ? C35 C38 1.501(6) . ? C36 H36 0.9500 . ? C39 C44 1.400(6) . ? C39 C40 1.405(6) . ? C39 B1 1.646(6) . ? C40 C41 1.386(6) . ? C40 H40 0.9500 . ? C41 C42 1.377(8) . ? C41 C45 1.491(8) . ? C42 C43 1.389(8) . ? C42 H42 0.9500 . ? C43 C44 1.393(7) . ? C43 C46 1.496(7) . ? C44 H44 0.9500 . ? C47 C48 1.387(6) . ? C47 C52 1.412(6) . ? C47 B1 1.637(6) . ? C48 C49 1.397(6) . ? C48 H48 0.9500 . ? C49 C50 1.380(6) . ? C49 C53 1.503(6) . ? C50 C51 1.390(6) . ? C50 H50 0.9500 . ? C51 C52 1.384(6) . ? C51 C54 1.501(6) . ? C52 H52 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 C2 Ni1 C3 39.94(19) . . ? C2 Ni1 C1 40.02(18) . . ? C3 Ni1 C1 70.78(19) . . ? C2 Ni1 P1 120.37(14) . . ? C3 Ni1 P1 159.49(14) . . ? C1 Ni1 P1 89.19(13) . . ? C2 Ni1 P2 125.66(13) . . ? C3 Ni1 P2 89.82(14) . . ? C1 Ni1 P2 159.12(14) . . ? P1 Ni1 P2 110.61(5) . . ? C5 P1 C8 107.2(2) . . ? C5 P1 C11 104.9(2) . . ? C8 P1 C11 102.4(2) . . ? C5 P1 Ni1 107.90(15) . . ? C8 P1 Ni1 117.11(15) . . ? C11 P1 Ni1 116.45(15) . . ? C20 P2 C14 102.7(2) . . ? C20 P2 C17 98.8(2) . . ? C14 P2 C17 105.4(2) . . ? C20 P2 Ni1 122.47(17) . . ? C14 P2 Ni1 111.11(17) . . ? C17 P2 Ni1 114.39(16) . . ? C2 C1 Ni1 69.6(3) . . ? C2 C1 H1A 116.7 . . ? Ni1 C1 H1A 116.7 . . ? C2 C1 H1B 116.7 . . ? Ni1 C1 H1B 116.7 . . ? H1A C1 H1B 113.7 . . ? C3 C2 C1 116.2(5) . . ? C3 C2 C4 121.9(4) . . ? C1 C2 C4 120.7(4) . . ? C3 C2 Ni1 70.3(3) . . ? C1 C2 Ni1 70.3(3) . . ? C4 C2 Ni1 119.0(3) . . ? C2 C3 Ni1 69.7(3) . . ? C2 C3 H3A 116.7 . . ? Ni1 C3 H3A 116.7 . . ? C2 C3 H3B 116.7 . . ? Ni1 C3 H3B 116.7 . . ? H3A C3 H3B 113.7 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C6 C5 C7 110.1(4) . . ? C6 C5 P1 109.9(3) . . ? C7 C5 P1 116.0(3) . . ? C6 C5 H5 106.8 . . ? C7 C5 H5 106.8 . . ? P1 C5 H5 106.8 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 C10 111.0(4) . . ? C9 C8 P1 115.7(3) . . ? C10 C8 P1 108.3(3) . . ? C9 C8 H8 107.1 . . ? C10 C8 H8 107.1 . . ? P1 C8 H8 107.1 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 P1 119.8(4) . . ? C12 C11 H11A 107.4 . . ? P1 C11 H11A 107.4 . . ? C12 C11 H11B 107.4 . . ? P1 C11 H11B 107.4 . . ? H11A C11 H11B 106.9 . . ? C13 C12 C11 123.3(5) . . ? C13 C12 H12 118.3 . . ? C11 C12 H12 118.3 . . ? C12 C13 H13A 120.0 . . ? C12 C13 H13B 120.0 . . ? H13A C13 H13B 120.0 . . ? C16 C14 C15 109.8(4) . . ? C16 C14 P2 114.9(4) . . ? C15 C14 P2 110.6(4) . . ? C16 C14 H14 107.1 . . ? C15 C14 H14 107.1 . . ? P2 C14 H14 107.1 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 C19 110.3(4) . . ? C18 C17 P2 113.3(3) . . ? C19 C17 P2 111.5(3) . . ? C18 C17 H17 107.1 . . ? C19 C17 H17 107.1 . . ? P2 C17 H17 107.1 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 P2 117.5(4) . . ? C21 C20 H20A 107.9 . . ? P2 C20 H20A 107.9 . . ? C21 C20 H20B 107.9 . . ? P2 C20 H20B 107.9 . . ? H20A C20 H20B 107.2 . . ? C22 C21 C20 123.2(6) . . ? C22 C21 H21 118.4 . . ? C20 C21 H21 118.4 . . ? C21 C22 H22A 120.0 . . ? C21 C22 H22B 120.0 . . ? H22A C22 H22B 120.0 . . ? C24 C23 C28 115.1(4) . . ? C24 C23 B1 124.0(4) . . ? C28 C23 B1 120.6(4) . . ? C25 C24 C23 122.5(4) . . ? C25 C24 H24 118.8 . . ? C23 C24 H24 118.8 . . ? C26 C25 C24 120.7(4) . . ? C26 C25 C29 119.4(4) . . ? C24 C25 C29 119.9(4) . . ? C25 C26 C27 118.4(4) . . ? C25 C26 H26 120.8 . . ? C27 C26 H26 120.8 . . ? C28 C27 C26 120.2(4) . . ? C28 C27 C30 119.2(4) . . ? C26 C27 C30 120.6(4) . . ? C27 C28 C23 123.0(4) . . ? C27 C28 H28 118.5 . . ? C23 C28 H28 118.5 . . ? F2 C29 F3 106.8(4) . . ? F2 C29 F1 106.4(4) . . ? F3 C29 F1 104.9(4) . . ? F2 C29 C25 113.4(4) . . ? F3 C29 C25 112.2(4) . . ? F1 C29 C25 112.5(4) . . ? F4 C30 F6 102.2(5) . . ? F4 C30 F5 105.9(5) . . ? F6 C30 F5 107.5(6) . . ? F4 C30 C27 112.2(4) . . ? F6 C30 C27 112.8(4) . . ? F5 C30 C27 115.2(5) . . ? C36 C31 C32 116.4(4) . . ? C36 C31 B1 123.3(4) . . ? C32 C31 B1 119.8(4) . . ? C33 C32 C31 122.2(4) . . ? C33 C32 H32 118.9 . . ? C31 C32 H32 118.9 . . ? C32 C33 C34 120.6(4) . . ? C32 C33 C37 119.2(4) . . ? C34 C33 C37 120.2(4) . . ? C35 C34 C33 118.0(4) . . ? C35 C34 H34 121.0 . . ? C33 C34 H34 121.0 . . ? C34 C35 C36 120.9(4) . . ? C34 C35 C38 120.6(4) . . ? C36 C35 C38 118.5(4) . . ? C35 C36 C31 122.0(4) . . ? C35 C36 H36 119.0 . . ? C31 C36 H36 119.0 . . ? F9 C37 F8 106.6(4) . . ? F9 C37 F7 106.6(4) . . ? F8 C37 F7 104.9(4) . . ? F9 C37 C33 112.9(4) . . ? F8 C37 C33 112.2(4) . . ? F7 C37 C33 113.1(4) . . ? F12 C38 F11 106.9(4) . . ? F12 C38 F10 106.5(4) . . ? F11 C38 F10 105.4(3) . . ? F12 C38 C35 113.1(4) . . ? F11 C38 C35 112.8(4) . . ? F10 C38 C35 111.7(4) . . ? C44 C39 C40 115.5(4) . . ? C44 C39 B1 124.0(4) . . ? C40 C39 B1 120.1(4) . . ? C41 C40 C39 122.6(5) . . ? C41 C40 H40 118.7 . . ? C39 C40 H40 118.7 . . ? C42 C41 C40 120.4(5) . . ? C42 C41 C45 119.5(5) . . ? C40 C41 C45 120.1(5) . . ? C41 C42 C43 118.9(5) . . ? C41 C42 H42 120.5 . . ? C43 C42 H42 120.5 . . ? C42 C43 C44 120.3(5) . . ? C42 C43 C46 118.5(5) . . ? C44 C43 C46 121.2(5) . . ? C43 C44 C39 122.2(5) . . ? C43 C44 H44 118.9 . . ? C39 C44 H44 118.9 . . ? F14A C45 F14B 18.0(18) . . ? F14A C45 F15A 108.2(6) . . ? F14B C45 F15A 125.2(16) . . ? F14A C45 F13A 109.7(11) . . ? F14B C45 F13A 100(3) . . ? F15A C45 F13A 95.1(10) . . ? F14A C45 F13B 93(2) . . ? F14B C45 F13B 82(3) . . ? F15A C45 F13B 108(3) . . ? F13A C45 F13B 19(2) . . ? F14A C45 F15B 80.6(11) . . ? F14B C45 F15B 98.5(19) . . ? F15A C45 F15B 36.5(10) . . ? F13A C45 F15B 127.7(16) . . ? F13B C45 F15B 134(3) . . ? F14A C45 C41 114.9(8) . . ? F14B C45 C41 107(2) . . ? F15A C45 C41 114.7(5) . . ? F13A C45 C41 112.4(8) . . ? F13B C45 C41 116(3) . . ? F15B C45 C41 107.9(11) . . ? F16A C46 F16B 16.9(15) . . ? F16A C46 F17A 102.7(7) . . ? F16B C46 F17A 89.2(18) . . ? F16A C46 F17B 130.7(14) . . ? F16B C46 F17B 114.1(18) . . ? F17A C46 F17B 36.5(16) . . ? F16A C46 F18A 110.6(10) . . ? F16B C46 F18A 106(2) . . ? F17A C46 F18A 106.7(7) . . ? F17B C46 F18A 74.3(15) . . ? F16A C46 F18B 88.4(15) . . ? F16B C46 F18B 90(3) . . ? F17A C46 F18B 133.0(15) . . ? F17B C46 F18B 104.0(18) . . ? F18A C46 F18B 29.9(14) . . ? F16A C46 C43 110.2(6) . . ? F16B C46 C43 125.8(15) . . ? F17A C46 C43 113.2(5) . . ? F17B C46 C43 112.1(11) . . ? F18A C46 C43 112.9(6) . . ? F18B C46 C43 104.8(15) . . ? C48 C47 C52 116.2(4) . . ? C48 C47 B1 125.1(4) . . ? C52 C47 B1 118.5(4) . . ? C47 C48 C49 121.9(4) . . ? C47 C48 H48 119.0 . . ? C49 C48 H48 119.0 . . ? C50 C49 C48 120.9(4) . . ? C50 C49 C53 118.4(4) . . ? C48 C49 C53 120.7(4) . . ? C49 C50 C51 118.5(4) . . ? C49 C50 H50 120.8 . . ? C51 C50 H50 120.8 . . ? C52 C51 C50 120.5(4) . . ? C52 C51 C54 121.1(4) . . ? C50 C51 C54 118.3(4) . . ? C51 C52 C47 122.1(4) . . ? C51 C52 H52 119.0 . . ? C47 C52 H52 119.0 . . ? F19 C53 F20 106.2(4) . . ? F19 C53 F21 105.8(4) . . ? F20 C53 F21 106.1(4) . . ? F19 C53 C49 113.0(4) . . ? F20 C53 C49 113.2(4) . . ? F21 C53 C49 112.0(4) . . ? F22 C54 F24 106.0(4) . . ? F22 C54 F23 106.3(4) . . ? F24 C54 F23 105.9(4) . . ? F22 C54 C51 112.1(4) . . ? F24 C54 C51 112.9(4) . . ? F23 C54 C51 113.1(4) . . ? C23 B1 C47 104.7(3) . . ? C23 B1 C31 112.4(3) . . ? C47 B1 C31 111.8(3) . . ? C23 B1 C39 113.2(3) . . ? C47 B1 C39 112.8(3) . . ? C31 B1 C39 102.1(3) . . ? 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 C2 Ni1 P1 C5 38.5(2) . . . . ? C3 Ni1 P1 C5 52.6(5) . . . . ? C1 Ni1 P1 C5 64.9(2) . . . . ? P2 Ni1 P1 C5 -121.92(16) . . . . ? C2 Ni1 P1 C8 -82.5(2) . . . . ? C3 Ni1 P1 C8 -68.3(5) . . . . ? C1 Ni1 P1 C8 -56.1(2) . . . . ? P2 Ni1 P1 C8 117.11(18) . . . . ? C2 Ni1 P1 C11 156.0(2) . . . . ? C3 Ni1 P1 C11 170.1(5) . . . . ? C1 Ni1 P1 C11 -177.6(2) . . . . ? P2 Ni1 P1 C11 -4.43(18) . . . . ? C2 Ni1 P2 C20 -179.9(3) . . . . ? C3 Ni1 P2 C20 161.2(3) . . . . ? C1 Ni1 P2 C20 139.9(4) . . . . ? P1 Ni1 P2 C20 -20.8(2) . . . . ? C2 Ni1 P2 C14 58.4(3) . . . . ? C3 Ni1 P2 C14 39.4(2) . . . . ? C1 Ni1 P2 C14 18.1(4) . . . . ? P1 Ni1 P2 C14 -142.48(18) . . . . ? C2 Ni1 P2 C17 -60.8(3) . . . . ? C3 Ni1 P2 C17 -79.7(2) . . . . ? C1 Ni1 P2 C17 -101.0(4) . . . . ? P1 Ni1 P2 C17 98.39(18) . . . . ? C3 Ni1 C1 C2 32.1(3) . . . . ? P1 Ni1 C1 C2 -143.4(3) . . . . ? P2 Ni1 C1 C2 54.7(5) . . . . ? Ni1 C1 C2 C3 -55.0(4) . . . . ? Ni1 C1 C2 C4 112.8(4) . . . . ? C1 Ni1 C2 C3 128.7(4) . . . . ? P1 Ni1 C2 C3 172.4(2) . . . . ? P2 Ni1 C2 C3 -30.4(3) . . . . ? C3 Ni1 C2 C1 -128.7(4) . . . . ? P1 Ni1 C2 C1 43.7(3) . . . . ? P2 Ni1 C2 C1 -159.0(2) . . . . ? C3 Ni1 C2 C4 116.4(5) . . . . ? C1 Ni1 C2 C4 -115.0(5) . . . . ? P1 Ni1 C2 C4 -71.3(4) . . . . ? P2 Ni1 C2 C4 86.0(4) . . . . ? C1 C2 C3 Ni1 55.0(4) . . . . ? C4 C2 C3 Ni1 -112.6(4) . . . . ? C1 Ni1 C3 C2 -32.1(3) . . . . ? P1 Ni1 C3 C2 -19.1(6) . . . . ? P2 Ni1 C3 C2 155.8(3) . . . . ? C8 P1 C5 C6 -177.0(3) . . . . ? C11 P1 C5 C6 -68.7(3) . . . . ? Ni1 P1 C5 C6 56.1(3) . . . . ? C8 P1 C5 C7 -51.3(4) . . . . ? C11 P1 C5 C7 57.0(4) . . . . ? Ni1 P1 C5 C7 -178.3(3) . . . . ? C5 P1 C8 C9 -45.6(4) . . . . ? C11 P1 C8 C9 -155.6(4) . . . . ? Ni1 P1 C8 C9 75.7(4) . . . . ? C5 P1 C8 C10 -170.9(3) . . . . ? C11 P1 C8 C10 79.0(4) . . . . ? Ni1 P1 C8 C10 -49.6(4) . . . . ? C5 P1 C11 C12 -76.8(4) . . . . ? C8 P1 C11 C12 35.0(4) . . . . ? Ni1 P1 C11 C12 164.1(3) . . . . ? P1 C11 C12 C13 -122.5(5) . . . . ? C20 P2 C14 C16 48.2(4) . . . . ? C17 P2 C14 C16 -54.7(4) . . . . ? Ni1 P2 C14 C16 -179.2(3) . . . . ? C20 P2 C14 C15 -76.8(4) . . . . ? C17 P2 C14 C15 -179.7(4) . . . . ? Ni1 P2 C14 C15 55.9(4) . . . . ? C20 P2 C17 C18 -170.8(4) . . . . ? C14 P2 C17 C18 -64.9(4) . . . . ? Ni1 P2 C17 C18 57.5(4) . . . . ? C20 P2 C17 C19 64.1(4) . . . . ? C14 P2 C17 C19 169.9(4) . . . . ? Ni1 P2 C17 C19 -67.7(4) . . . . ? C14 P2 C20 C21 65.1(5) . . . . ? C17 P2 C20 C21 173.2(4) . . . . ? Ni1 P2 C20 C21 -60.4(5) . . . . ? P2 C20 C21 C22 -135.7(6) . . . . ? C28 C23 C24 C25 0.8(6) . . . . ? B1 C23 C24 C25 173.6(4) . . . . ? C23 C24 C25 C26 0.6(6) . . . . ? C23 C24 C25 C29 -176.5(4) . . . . ? C24 C25 C26 C27 -0.4(6) . . . . ? C29 C25 C26 C27 176.7(4) . . . . ? C25 C26 C27 C28 -1.2(6) . . . . ? C25 C26 C27 C30 177.9(4) . . . . ? C26 C27 C28 C23 2.7(7) . . . . ? C30 C27 C28 C23 -176.4(4) . . . . ? C24 C23 C28 C27 -2.4(6) . . . . ? B1 C23 C28 C27 -175.6(4) . . . . ? C26 C25 C29 F2 26.0(6) . . . . ? C24 C25 C29 F2 -156.8(4) . . . . ? C26 C25 C29 F3 -95.0(5) . . . . ? C24 C25 C29 F3 82.1(5) . . . . ? C26 C25 C29 F1 146.9(4) . . . . ? C24 C25 C29 F1 -36.0(6) . . . . ? C28 C27 C30 F4 60.6(6) . . . . ? C26 C27 C30 F4 -118.5(5) . . . . ? C28 C27 C30 F6 -54.2(6) . . . . ? C26 C27 C30 F6 126.8(5) . . . . ? C28 C27 C30 F5 -178.2(6) . . . . ? C26 C27 C30 F5 2.8(8) . . . . ? C36 C31 C32 C33 0.0(6) . . . . ? B1 C31 C32 C33 171.2(4) . . . . ? C31 C32 C33 C34 0.0(6) . . . . ? C31 C32 C33 C37 179.0(4) . . . . ? C32 C33 C34 C35 -0.6(6) . . . . ? C37 C33 C34 C35 -179.7(4) . . . . ? C33 C34 C35 C36 1.3(6) . . . . ? C33 C34 C35 C38 -177.3(4) . . . . ? C34 C35 C36 C31 -1.4(6) . . . . ? C38 C35 C36 C31 177.2(4) . . . . ? C32 C31 C36 C35 0.7(6) . . . . ? B1 C31 C36 C35 -170.2(4) . . . . ? C32 C33 C37 F9 42.5(6) . . . . ? C34 C33 C37 F9 -138.4(4) . . . . ? C32 C33 C37 F8 -78.0(5) . . . . ? C34 C33 C37 F8 101.1(5) . . . . ? C32 C33 C37 F7 163.6(4) . . . . ? C34 C33 C37 F7 -17.3(6) . . . . ? C34 C35 C38 F12 9.8(6) . . . . ? C36 C35 C38 F12 -168.8(4) . . . . ? C34 C35 C38 F11 -111.6(4) . . . . ? C36 C35 C38 F11 69.7(5) . . . . ? C34 C35 C38 F10 129.9(4) . . . . ? C36 C35 C38 F10 -48.7(5) . . . . ? C44 C39 C40 C41 1.3(6) . . . . ? B1 C39 C40 C41 174.5(4) . . . . ? C39 C40 C41 C42 -0.1(7) . . . . ? C39 C40 C41 C45 179.3(4) . . . . ? C40 C41 C42 C43 -0.9(7) . . . . ? C45 C41 C42 C43 179.8(5) . . . . ? C41 C42 C43 C44 0.6(7) . . . . ? C41 C42 C43 C46 178.9(4) . . . . ? C42 C43 C44 C39 0.7(7) . . . . ? C46 C43 C44 C39 -177.5(4) . . . . ? C40 C39 C44 C43 -1.6(6) . . . . ? B1 C39 C44 C43 -174.6(4) . . . . ? C42 C41 C45 F14A 93.8(9) . . . . ? C40 C41 C45 F14A -85.5(9) . . . . ? C42 C41 C45 F14B 111(2) . . . . ? C40 C41 C45 F14B -68(2) . . . . ? C42 C41 C45 F15A -32.5(9) . . . . ? C40 C41 C45 F15A 148.1(7) . . . . ? C42 C41 C45 F13A -139.8(8) . . . . ? C40 C41 C45 F13A 40.9(9) . . . . ? C42 C41 C45 F13B -160(2) . . . . ? C40 C41 C45 F13B 21(2) . . . . ? C42 C41 C45 F15B 6.1(14) . . . . ? C40 C41 C45 F15B -173.3(13) . . . . ? C42 C43 C46 F16A 61.3(9) . . . . ? C44 C43 C46 F16A -120.4(9) . . . . ? C42 C43 C46 F16B 69(3) . . . . ? C44 C43 C46 F16B -113(3) . . . . ? C42 C43 C46 F17A 175.7(7) . . . . ? C44 C43 C46 F17A -6.0(9) . . . . ? C42 C43 C46 F17B -145(2) . . . . ? C44 C43 C46 F17B 34(2) . . . . ? C42 C43 C46 F18A -62.9(10) . . . . ? C44 C43 C46 F18A 115.4(9) . . . . ? C42 C43 C46 F18B -32.5(16) . . . . ? C44 C43 C46 F18B 145.8(15) . . . . ? C52 C47 C48 C49 1.4(6) . . . . ? B1 C47 C48 C49 176.3(4) . . . . ? C47 C48 C49 C50 -0.4(6) . . . . ? C47 C48 C49 C53 179.6(4) . . . . ? C48 C49 C50 C51 -0.6(6) . . . . ? C53 C49 C50 C51 179.4(4) . . . . ? C49 C50 C51 C52 0.6(6) . . . . ? C49 C50 C51 C54 -176.7(4) . . . . ? C50 C51 C52 C47 0.5(6) . . . . ? C54 C51 C52 C47 177.8(4) . . . . ? C48 C47 C52 C51 -1.5(6) . . . . ? B1 C47 C52 C51 -176.7(4) . . . . ? C50 C49 C53 F19 60.9(5) . . . . ? C48 C49 C53 F19 -119.1(4) . . . . ? C50 C49 C53 F20 -178.4(4) . . . . ? C48 C49 C53 F20 1.6(6) . . . . ? C50 C49 C53 F21 -58.5(5) . . . . ? C48 C49 C53 F21 121.5(4) . . . . ? C52 C51 C54 F22 -102.8(5) . . . . ? C50 C51 C54 F22 74.5(5) . . . . ? C52 C51 C54 F24 137.5(4) . . . . ? C50 C51 C54 F24 -45.2(5) . . . . ? C52 C51 C54 F23 17.2(6) . . . . ? C50 C51 C54 F23 -165.5(4) . . . . ? C24 C23 B1 C47 -93.1(4) . . . . ? C28 C23 B1 C47 79.4(4) . . . . ? C24 C23 B1 C31 28.5(5) . . . . ? C28 C23 B1 C31 -159.0(4) . . . . ? C24 C23 B1 C39 143.6(4) . . . . ? C28 C23 B1 C39 -43.9(5) . . . . ? C48 C47 B1 C23 -107.2(4) . . . . ? C52 C47 B1 C23 67.5(4) . . . . ? C48 C47 B1 C31 130.8(4) . . . . ? C52 C47 B1 C31 -54.5(5) . . . . ? C48 C47 B1 C39 16.3(6) . . . . ? C52 C47 B1 C39 -168.9(4) . . . . ? C36 C31 B1 C23 -139.1(4) . . . . ? C32 C31 B1 C23 50.3(5) . . . . ? C36 C31 B1 C47 -21.6(5) . . . . ? C32 C31 B1 C47 167.8(3) . . . . ? C36 C31 B1 C39 99.3(4) . . . . ? C32 C31 B1 C39 -71.3(4) . . . . ? C44 C39 B1 C23 -20.5(6) . . . . ? C40 C39 B1 C23 166.9(4) . . . . ? C44 C39 B1 C47 -139.2(4) . . . . ? C40 C39 B1 C47 48.2(5) . . . . ? C44 C39 B1 C31 100.6(4) . . . . ? C40 C39 B1 C31 -72.0(5) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.813 _refine_diff_density_min -0.458 _refine_diff_density_rms 0.080 #=== END #=== END OF GLOBAL CIF ====