data_nelson_nii #---------------------------------------------------- #------------- BROMIDE.075THF---------------------- #--------------------------------------------------- _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C71 H62 Br2 Fe2 Ni2 O0.75 P4' _chemical_formula_weight 1440.03 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source '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' 'Fe' 'Fe' 0.3463 0.8444 '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' 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 24.0416(4) _cell_length_b 13.7277(2) _cell_length_c 18.7831(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.188(2) _cell_angle_gamma 90.00 _cell_volume 6197.76(17) _cell_formula_units_Z 4 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 5966 _cell_measurement_theta_min 2.9378 _cell_measurement_theta_max 29.3830 _exptl_crystal_description fragment _exptl_crystal_colour red _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.543 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2928 _exptl_absorpt_coefficient_mu 2.494 _exptl_absorpt_correction_T_min 0.88824 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 130(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 'Oxford Diffraction Xcalibur E' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15193 _diffrn_reflns_av_R_equivalents 0.0288 _diffrn_reflns_av_sigmaI/netI 0.0522 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 28.98 _reflns_number_total 7468 _reflns_number_gt 5781 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'CrysalisPro' _computing_cell_refinement 'CrysalisPro' _computing_data_reduction 'CrysalisPro' _computing_structure_solution 'SIR92' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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^ > 2\s(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^)+(0.0397P)^2^+11.7760P] 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 7468 _refine_ls_number_parameters 379 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0603 _refine_ls_R_factor_gt 0.0403 _refine_ls_wR_factor_ref 0.0972 _refine_ls_wR_factor_gt 0.0877 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.018 _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 0.247000(16) 0.13430(3) 0.03165(2) 0.01746(10) Uani 1 1 d . . . Br1 Br 0.254943(15) 0.20118(2) -0.088787(17) 0.02684(9) Uani 1 1 d . . . Fe1 Fe 0.260503(18) -0.08161(3) 0.18569(2) 0.01800(10) Uani 1 1 d . . . P1 P 0.32500(3) 0.07863(5) 0.08018(4) 0.01680(16) Uani 1 1 d . . . P2 P 0.18542(3) 0.01597(5) 0.04672(4) 0.01582(16) Uani 1 1 d . . . C1 C 0.31721(12) 0.0229(2) 0.16613(16) 0.0176(6) Uani 1 1 d . . . C2 C 0.34425(13) -0.0597(2) 0.19765(18) 0.0231(7) Uani 1 1 d . . . H2 H 0.3730 -0.0970 0.1770 0.028 Uiso 1 1 calc R . . C3 C 0.32058(14) -0.0761(2) 0.26499(18) 0.0285(8) Uani 1 1 d . . . H3 H 0.3306 -0.1271 0.2970 0.034 Uiso 1 1 calc R . . C4 C 0.27974(14) -0.0044(2) 0.27696(18) 0.0277(7) Uani 1 1 d . . . H4 H 0.2579 0.0016 0.3183 0.033 Uiso 1 1 calc R . . C5 C 0.27700(13) 0.0571(2) 0.21625(16) 0.0209(6) Uani 1 1 d . . . H5 H 0.2529 0.1114 0.2098 0.025 Uiso 1 1 calc R . . C6 C 0.20156(12) -0.0848(2) 0.10642(15) 0.0161(6) Uani 1 1 d . . . C7 C 0.24263(13) -0.1592(2) 0.09598(17) 0.0198(6) Uani 1 1 d . . . H7 H 0.2657 -0.1652 0.0558 0.024 Uiso 1 1 calc R . . C8 C 0.24292(14) -0.2219(2) 0.15588(18) 0.0259(7) Uani 1 1 d . . . H8 H 0.2662 -0.2772 0.1626 0.031 Uiso 1 1 calc R . . C9 C 0.20255(14) -0.1883(2) 0.20395(18) 0.0261(7) Uani 1 1 d . . . H9 H 0.1943 -0.2165 0.2487 0.031 Uiso 1 1 calc R . . C10 C 0.17659(13) -0.1044(2) 0.17323(17) 0.0220(7) Uani 1 1 d . . . H10 H 0.1475 -0.0677 0.1938 0.026 Uiso 1 1 calc R . . C11 C 0.36257(13) -0.0095(2) 0.02672(17) 0.0212(6) Uani 1 1 d . . . C12 C 0.33628(14) -0.0492(2) -0.03319(17) 0.0250(7) Uani 1 1 d . . . H12 H 0.2990 -0.0314 -0.0447 0.030 Uiso 1 1 calc R . . C13 C 0.36387(16) -0.1146(2) -0.07640(19) 0.0333(8) Uani 1 1 d . . . H13 H 0.3453 -0.1417 -0.1169 0.040 Uiso 1 1 calc R . . C14 C 0.41820(16) -0.1402(3) -0.0606(2) 0.0398(9) Uani 1 1 d . . . H14 H 0.4369 -0.1853 -0.0900 0.048 Uiso 1 1 calc R . . C15 C 0.44557(16) -0.0999(3) -0.0016(2) 0.0447(10) Uani 1 1 d . . . H15 H 0.4832 -0.1168 0.0090 0.054 Uiso 1 1 calc R . . C16 C 0.41781(14) -0.0351(3) 0.0418(2) 0.0333(8) Uani 1 1 d . . . H16 H 0.4365 -0.0079 0.0821 0.040 Uiso 1 1 calc R . . C17 C 0.37910(13) 0.1691(2) 0.09878(18) 0.0215(7) Uani 1 1 d . . . C18 C 0.40517(15) 0.2151(2) 0.0420(2) 0.0345(8) Uani 1 1 d . . . H18 H 0.3948 0.1988 -0.0056 0.041 Uiso 1 1 calc R . . C19 C 0.44586(16) 0.2841(3) 0.0548(3) 0.0465(11) Uani 1 1 d . . . H19 H 0.4633 0.3151 0.0160 0.056 Uiso 1 1 calc R . . C20 C 0.46167(16) 0.3087(3) 0.1247(3) 0.0474(12) Uani 1 1 d . . . H20 H 0.4903 0.3551 0.1334 0.057 Uiso 1 1 calc R . . C21 C 0.43553(16) 0.2651(3) 0.1804(2) 0.0410(10) Uani 1 1 d . . . H21 H 0.4455 0.2827 0.2279 0.049 Uiso 1 1 calc R . . C22 C 0.39462(14) 0.1954(2) 0.1679(2) 0.0286(8) Uani 1 1 d . . . H22 H 0.3770 0.1653 0.2070 0.034 Uiso 1 1 calc R . . C23 C 0.12105(12) 0.0614(2) 0.08525(16) 0.0188(6) Uani 1 1 d . . . C24 C 0.12410(14) 0.1442(2) 0.12763(18) 0.0266(7) Uani 1 1 d . . . H24 H 0.1590 0.1749 0.1361 0.032 Uiso 1 1 calc R . . C25 C 0.07672(15) 0.1826(3) 0.1577(2) 0.0326(8) Uani 1 1 d . . . H25 H 0.0794 0.2394 0.1865 0.039 Uiso 1 1 calc R . . C26 C 0.02589(15) 0.1392(3) 0.1463(2) 0.0335(8) Uani 1 1 d . . . H26 H -0.0063 0.1656 0.1676 0.040 Uiso 1 1 calc R . . C27 C 0.02154(14) 0.0570(3) 0.1039(2) 0.0316(8) Uani 1 1 d . . . H27 H -0.0137 0.0275 0.0952 0.038 Uiso 1 1 calc R . . C28 C 0.06924(13) 0.0178(2) 0.07394(18) 0.0249(7) Uani 1 1 d . . . H28 H 0.0664 -0.0393 0.0455 0.030 Uiso 1 1 calc R . . C29 C 0.15908(12) -0.0496(2) -0.03208(16) 0.0202(6) Uani 1 1 d . . . C30 C 0.14583(16) -0.1482(2) -0.0306(2) 0.0341(9) Uani 1 1 d . . . H30 H 0.1501 -0.1836 0.0126 0.041 Uiso 1 1 calc R . . C31 C 0.12662(17) -0.1952(3) -0.0911(2) 0.0470(11) Uani 1 1 d . . . H31 H 0.1173 -0.2624 -0.0893 0.056 Uiso 1 1 calc R . . C32 C 0.12092(16) -0.1454(4) -0.1538(2) 0.0502(12) Uani 1 1 d . . . H32 H 0.1088 -0.1784 -0.1958 0.060 Uiso 1 1 calc R . . C33 C 0.13273(17) -0.0475(4) -0.1560(2) 0.0575(14) Uani 1 1 d . . . H33 H 0.1276 -0.0127 -0.1994 0.069 Uiso 1 1 calc R . . C34 C 0.15211(15) 0.0015(3) -0.09526(19) 0.0389(9) Uani 1 1 d . . . H34 H 0.1604 0.0690 -0.0972 0.047 Uiso 1 1 calc R . . O1S O 0.4822(4) -0.1303(5) 0.2383(6) 0.063(2) Uani 0.38 1 d PU A -1 C1S C 0.5181(3) -0.0808(4) 0.1966(3) 0.0509(14) Uani 0.75 1 d PU A -1 H1S1 H 0.5078 -0.0900 0.1457 0.061 Uiso 0.75 1 calc PR A -1 H1S2 H 0.5565 -0.1052 0.2045 0.061 Uiso 0.75 1 calc PR A -1 C2S C 0.5149(2) 0.0272(3) 0.2161(3) 0.0418(12) Uani 0.75 1 d PU . . H2S1 H 0.5525 0.0557 0.2222 0.050 Uiso 0.75 1 calc PR A . H2S2 H 0.4940 0.0644 0.1791 0.050 Uiso 0.75 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0170(2) 0.01493(18) 0.0204(2) 0.00356(14) -0.00122(15) -0.00130(15) Br1 0.0457(2) 0.01676(15) 0.01818(16) -0.00049(12) 0.00433(14) -0.00381(14) Fe1 0.0170(2) 0.0191(2) 0.0179(2) 0.00413(16) -0.00108(17) -0.00287(17) P1 0.0150(4) 0.0172(3) 0.0182(4) 0.0016(3) 0.0007(3) -0.0017(3) P2 0.0147(4) 0.0148(3) 0.0179(4) 0.0011(3) -0.0008(3) -0.0008(3) C1 0.0140(14) 0.0196(14) 0.0191(15) 0.0003(12) -0.0010(12) -0.0030(12) C2 0.0172(16) 0.0237(15) 0.0283(17) 0.0023(13) -0.0047(13) -0.0038(13) C3 0.0262(18) 0.0346(18) 0.0244(17) 0.0097(14) -0.0101(14) -0.0076(15) C4 0.0281(18) 0.0366(18) 0.0182(16) -0.0026(14) -0.0025(13) -0.0114(15) C5 0.0212(16) 0.0194(14) 0.0222(16) -0.0032(12) 0.0000(12) -0.0034(13) C6 0.0152(15) 0.0146(13) 0.0185(15) 0.0008(11) -0.0012(11) -0.0036(11) C7 0.0192(16) 0.0171(14) 0.0231(16) -0.0023(12) -0.0006(12) -0.0007(12) C8 0.0246(18) 0.0183(15) 0.0346(19) 0.0067(13) -0.0067(14) -0.0037(13) C9 0.0228(17) 0.0270(16) 0.0285(18) 0.0109(13) -0.0022(14) -0.0092(14) C10 0.0178(16) 0.0248(15) 0.0233(17) 0.0026(13) 0.0005(13) -0.0055(13) C11 0.0194(16) 0.0218(15) 0.0225(16) 0.0008(12) 0.0041(12) -0.0019(13) C12 0.0240(17) 0.0273(16) 0.0236(17) -0.0010(13) 0.0008(13) -0.0030(14) C13 0.037(2) 0.0332(18) 0.030(2) -0.0085(15) 0.0021(16) -0.0048(16) C14 0.038(2) 0.039(2) 0.042(2) -0.0162(17) 0.0148(18) 0.0007(18) C15 0.0233(19) 0.052(2) 0.059(3) -0.018(2) 0.0048(18) 0.0085(18) C16 0.0213(18) 0.041(2) 0.037(2) -0.0128(16) -0.0009(15) 0.0005(16) C17 0.0161(15) 0.0162(14) 0.0321(18) 0.0033(12) -0.0018(13) -0.0030(12) C18 0.0254(19) 0.0328(19) 0.045(2) 0.0148(16) 0.0009(16) -0.0049(15) C19 0.028(2) 0.034(2) 0.078(3) 0.026(2) 0.002(2) -0.0075(17) C20 0.025(2) 0.0209(17) 0.096(4) 0.011(2) -0.012(2) -0.0101(16) C21 0.031(2) 0.0260(18) 0.065(3) -0.0122(18) -0.0155(19) -0.0043(16) C22 0.0222(18) 0.0205(15) 0.043(2) -0.0023(14) -0.0032(15) -0.0022(14) C23 0.0166(15) 0.0186(14) 0.0213(15) 0.0044(12) 0.0001(12) 0.0025(12) C24 0.0229(17) 0.0263(16) 0.0304(19) -0.0026(14) -0.0042(14) 0.0029(14) C25 0.033(2) 0.0312(18) 0.034(2) -0.0084(15) -0.0012(16) 0.0086(16) C26 0.0211(18) 0.041(2) 0.039(2) -0.0008(16) 0.0069(15) 0.0117(16) C27 0.0175(17) 0.0359(19) 0.041(2) 0.0047(16) 0.0030(15) -0.0033(15) C28 0.0214(17) 0.0225(15) 0.0310(18) 0.0001(13) 0.0018(14) -0.0028(13) C29 0.0133(14) 0.0287(16) 0.0187(15) -0.0027(12) 0.0008(12) 0.0011(13) C30 0.036(2) 0.0277(17) 0.038(2) -0.0076(15) -0.0136(17) 0.0021(16) C31 0.042(2) 0.044(2) 0.055(3) -0.030(2) -0.017(2) 0.0105(19) C32 0.023(2) 0.093(3) 0.035(2) -0.036(2) 0.0008(17) -0.008(2) C33 0.039(2) 0.119(4) 0.0150(18) 0.011(2) -0.0016(16) -0.029(3) C34 0.031(2) 0.059(2) 0.0258(19) 0.0118(17) -0.0052(15) -0.0196(19) O1S 0.065(6) 0.043(3) 0.081(6) -0.016(4) -0.024(4) -0.011(3) C1S 0.054(3) 0.036(3) 0.062(4) -0.010(2) -0.018(3) 0.033(2) C2S 0.043(3) 0.030(2) 0.051(3) -0.009(2) -0.014(2) 0.010(2) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 2.2048(8) . ? Ni1 P2 2.2199(8) . ? Ni1 Br1 2.4525(5) . ? Ni1 Br1 2.5014(5) 7 ? Br1 Ni1 2.5014(5) 7 ? Fe1 C1 2.018(3) . ? Fe1 C5 2.026(3) . ? Fe1 C7 2.032(3) . ? Fe1 C6 2.035(3) . ? Fe1 C2 2.044(3) . ? Fe1 C8 2.048(3) . ? Fe1 C10 2.050(3) . ? Fe1 C3 2.055(3) . ? Fe1 C9 2.055(3) . ? Fe1 C4 2.060(3) . ? P1 C1 1.800(3) . ? P1 C11 1.823(3) . ? P1 C17 1.826(3) . ? P2 C6 1.818(3) . ? P2 C23 1.831(3) . ? P2 C29 1.834(3) . ? C1 C2 1.430(4) . ? C1 C5 1.442(4) . ? C2 C3 1.416(5) . ? C2 H2 0.9500 . ? C3 C4 1.411(5) . ? C3 H3 0.9500 . ? C4 C5 1.420(4) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C10 1.428(4) . ? C6 C7 1.436(4) . ? C7 C8 1.417(4) . ? C7 H7 0.9500 . ? C8 C9 1.417(5) . ? C8 H8 0.9500 . ? C9 C10 1.426(4) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.391(4) . ? C11 C16 1.397(4) . ? C12 C13 1.388(5) . ? C12 H12 0.9500 . ? C13 C14 1.379(5) . ? C13 H13 0.9500 . ? C14 C15 1.392(5) . ? C14 H14 0.9500 . ? C15 C16 1.386(5) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 C22 1.391(5) . ? C17 C18 1.400(5) . ? C18 C19 1.379(5) . ? C18 H18 0.9500 . ? C19 C20 1.400(6) . ? C19 H19 0.9500 . ? C20 C21 1.369(6) . ? C20 H20 0.9500 . ? C21 C22 1.389(5) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C24 1.389(4) . ? C23 C28 1.394(4) . ? C24 C25 1.386(5) . ? C24 H24 0.9500 . ? C25 C26 1.372(5) . ? C25 H25 0.9500 . ? C26 C27 1.384(5) . ? C26 H26 0.9500 . ? C27 C28 1.395(5) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 C34 1.386(5) . ? C29 C30 1.391(4) . ? C30 C31 1.378(5) . ? C30 H30 0.9500 . ? C31 C32 1.365(6) . ? C31 H31 0.9500 . ? C32 C33 1.375(7) . ? C32 H32 0.9500 . ? C33 C34 1.396(6) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? O1S C1S 1.360(12) . ? C1S C2S 1.529(7) . ? C1S H1S1 0.9900 . ? C1S H1S2 0.9900 . ? C2S C2S 1.474(11) 2_655 ? C2S H2S1 0.9900 . ? C2S H2S2 0.9900 . ? 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 P2 104.92(3) . . ? P1 Ni1 Br1 115.42(3) . . ? P2 Ni1 Br1 117.16(3) . . ? P1 Ni1 Br1 99.14(3) . 7 ? P2 Ni1 Br1 125.98(3) . 7 ? Br1 Ni1 Br1 93.453(15) . 7 ? Ni1 Br1 Ni1 86.547(15) . 7 ? C1 Fe1 C5 41.78(12) . . ? C1 Fe1 C7 110.71(12) . . ? C5 Fe1 C7 139.85(12) . . ? C1 Fe1 C6 110.19(11) . . ? C5 Fe1 C6 110.92(12) . . ? C7 Fe1 C6 41.36(12) . . ? C1 Fe1 C2 41.21(12) . . ? C5 Fe1 C2 69.14(13) . . ? C7 Fe1 C2 111.06(13) . . ? C6 Fe1 C2 138.88(13) . . ? C1 Fe1 C8 139.06(13) . . ? C5 Fe1 C8 179.16(14) . . ? C7 Fe1 C8 40.65(12) . . ? C6 Fe1 C8 69.06(12) . . ? C2 Fe1 C8 111.46(13) . . ? C1 Fe1 C10 138.99(12) . . ? C5 Fe1 C10 111.23(13) . . ? C7 Fe1 C10 68.57(13) . . ? C6 Fe1 C10 40.92(12) . . ? C2 Fe1 C10 179.59(14) . . ? C8 Fe1 C10 68.16(13) . . ? C1 Fe1 C3 68.80(12) . . ? C5 Fe1 C3 68.25(13) . . ? C7 Fe1 C3 138.95(13) . . ? C6 Fe1 C3 178.97(13) . . ? C2 Fe1 C3 40.42(13) . . ? C8 Fe1 C3 111.78(13) . . ? C10 Fe1 C3 139.79(13) . . ? C1 Fe1 C9 179.11(13) . . ? C5 Fe1 C9 138.76(14) . . ? C7 Fe1 C9 68.44(13) . . ? C6 Fe1 C9 69.04(12) . . ? C2 Fe1 C9 139.15(13) . . ? C8 Fe1 C9 40.40(13) . . ? C10 Fe1 C9 40.65(12) . . ? C3 Fe1 C9 111.98(13) . . ? C1 Fe1 C4 69.19(13) . . ? C5 Fe1 C4 40.65(13) . . ? C7 Fe1 C4 179.07(13) . . ? C6 Fe1 C4 139.57(13) . . ? C2 Fe1 C4 68.23(14) . . ? C8 Fe1 C4 138.87(13) . . ? C10 Fe1 C4 112.15(13) . . ? C3 Fe1 C4 40.12(14) . . ? C9 Fe1 C4 111.66(14) . . ? C1 P1 C11 105.91(14) . . ? C1 P1 C17 101.80(14) . . ? C11 P1 C17 101.37(14) . . ? C1 P1 Ni1 114.50(10) . . ? C11 P1 Ni1 115.41(11) . . ? C17 P1 Ni1 116.08(10) . . ? C6 P2 C23 100.76(13) . . ? C6 P2 C29 100.94(14) . . ? C23 P2 C29 101.86(14) . . ? C6 P2 Ni1 120.08(10) . . ? C23 P2 Ni1 111.87(10) . . ? C29 P2 Ni1 118.45(10) . . ? C2 C1 C5 107.1(3) . . ? C2 C1 P1 130.8(2) . . ? C5 C1 P1 122.1(2) . . ? C2 C1 Fe1 70.36(17) . . ? C5 C1 Fe1 69.41(16) . . ? P1 C1 Fe1 123.29(15) . . ? C3 C2 C1 107.9(3) . . ? C3 C2 Fe1 70.21(18) . . ? C1 C2 Fe1 68.44(17) . . ? C3 C2 H2 126.0 . . ? C1 C2 H2 126.0 . . ? Fe1 C2 H2 126.9 . . ? C4 C3 C2 109.0(3) . . ? C4 C3 Fe1 70.15(18) . . ? C2 C3 Fe1 69.38(18) . . ? C4 C3 H3 125.5 . . ? C2 C3 H3 125.5 . . ? Fe1 C3 H3 126.6 . . ? C3 C4 C5 107.9(3) . . ? C3 C4 Fe1 69.73(19) . . ? C5 C4 Fe1 68.39(17) . . ? C3 C4 H4 126.0 . . ? C5 C4 H4 126.0 . . ? Fe1 C4 H4 127.4 . . ? C4 C5 C1 108.0(3) . . ? C4 C5 Fe1 70.96(18) . . ? C1 C5 Fe1 68.81(16) . . ? C4 C5 H5 126.0 . . ? C1 C5 H5 126.0 . . ? Fe1 C5 H5 125.8 . . ? C10 C6 C7 106.8(3) . . ? C10 C6 P2 126.7(2) . . ? C7 C6 P2 126.5(2) . . ? C10 C6 Fe1 70.13(17) . . ? C7 C6 Fe1 69.21(16) . . ? P2 C6 Fe1 124.84(15) . . ? C8 C7 C6 108.4(3) . . ? C8 C7 Fe1 70.29(18) . . ? C6 C7 Fe1 69.43(16) . . ? C8 C7 H7 125.8 . . ? C6 C7 H7 125.8 . . ? Fe1 C7 H7 126.1 . . ? C9 C8 C7 108.4(3) . . ? C9 C8 Fe1 70.07(18) . . ? C7 C8 Fe1 69.06(17) . . ? C9 C8 H8 125.8 . . ? C7 C8 H8 125.8 . . ? Fe1 C8 H8 126.6 . . ? C8 C9 C10 107.8(3) . . ? C8 C9 Fe1 69.53(18) . . ? C10 C9 Fe1 69.50(17) . . ? C8 C9 H9 126.1 . . ? C10 C9 H9 126.1 . . ? Fe1 C9 H9 126.4 . . ? C9 C10 C6 108.6(3) . . ? C9 C10 Fe1 69.85(18) . . ? C6 C10 Fe1 68.95(17) . . ? C9 C10 H10 125.7 . . ? C6 C10 H10 125.7 . . ? Fe1 C10 H10 127.1 . . ? C12 C11 C16 118.6(3) . . ? C12 C11 P1 118.9(2) . . ? C16 C11 P1 122.4(2) . . ? C13 C12 C11 120.8(3) . . ? C13 C12 H12 119.6 . . ? C11 C12 H12 119.6 . . ? C14 C13 C12 120.1(3) . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C13 C14 C15 120.0(3) . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C16 C15 C14 119.8(4) . . ? C16 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C15 C16 C11 120.7(3) . . ? C15 C16 H16 119.7 . . ? C11 C16 H16 119.7 . . ? C22 C17 C18 118.6(3) . . ? C22 C17 P1 122.1(3) . . ? C18 C17 P1 119.3(3) . . ? C19 C18 C17 120.3(4) . . ? C19 C18 H18 119.9 . . ? C17 C18 H18 119.9 . . ? C18 C19 C20 120.5(4) . . ? C18 C19 H19 119.8 . . ? C20 C19 H19 119.8 . . ? C21 C20 C19 119.4(3) . . ? C21 C20 H20 120.3 . . ? C19 C20 H20 120.3 . . ? C20 C21 C22 120.4(4) . . ? C20 C21 H21 119.8 . . ? C22 C21 H21 119.8 . . ? C21 C22 C17 120.8(4) . . ? C21 C22 H22 119.6 . . ? C17 C22 H22 119.6 . . ? C24 C23 C28 118.4(3) . . ? C24 C23 P2 118.0(2) . . ? C28 C23 P2 123.6(2) . . ? C25 C24 C23 120.7(3) . . ? C25 C24 H24 119.7 . . ? C23 C24 H24 119.7 . . ? C26 C25 C24 120.6(3) . . ? C26 C25 H25 119.7 . . ? C24 C25 H25 119.7 . . ? C25 C26 C27 120.0(3) . . ? C25 C26 H26 120.0 . . ? C27 C26 H26 120.0 . . ? C26 C27 C28 119.6(3) . . ? C26 C27 H27 120.2 . . ? C28 C27 H27 120.2 . . ? C23 C28 C27 120.8(3) . . ? C23 C28 H28 119.6 . . ? C27 C28 H28 119.6 . . ? C34 C29 C30 119.0(3) . . ? C34 C29 P2 118.4(3) . . ? C30 C29 P2 122.5(3) . . ? C31 C30 C29 120.8(4) . . ? C31 C30 H30 119.6 . . ? C29 C30 H30 119.6 . . ? C32 C31 C30 120.2(4) . . ? C32 C31 H31 119.9 . . ? C30 C31 H31 119.9 . . ? C31 C32 C33 119.9(4) . . ? C31 C32 H32 120.1 . . ? C33 C32 H32 120.1 . . ? C32 C33 C34 120.8(4) . . ? C32 C33 H33 119.6 . . ? C34 C33 H33 119.6 . . ? C29 C34 C33 119.3(4) . . ? C29 C34 H34 120.4 . . ? C33 C34 H34 120.4 . . ? O1S C1S C2S 108.1(6) . . ? O1S C1S H1S1 110.1 . . ? C2S C1S H1S1 110.1 . . ? O1S C1S H1S2 110.1 . . ? C2S C1S H1S2 110.1 . . ? H1S1 C1S H1S2 108.4 . . ? C2S C2S C1S 103.6(3) 2_655 . ? C2S C2S H2S1 111.0 2_655 . ? C1S C2S H2S1 111.0 . . ? C2S C2S H2S2 111.0 2_655 . ? C1S C2S H2S2 111.0 . . ? H2S1 C2S H2S2 109.0 . . ? 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 Br1 Ni1 -101.82(3) . . . 7 ? P2 Ni1 Br1 Ni1 133.83(3) . . . 7 ? Br1 Ni1 Br1 Ni1 0.0 7 . . 7 ? P2 Ni1 P1 C1 -45.68(11) . . . . ? Br1 Ni1 P1 C1 -176.20(10) . . . . ? Br1 Ni1 P1 C1 85.52(11) 7 . . . ? P2 Ni1 P1 C11 77.68(11) . . . . ? Br1 Ni1 P1 C11 -52.83(11) . . . . ? Br1 Ni1 P1 C11 -151.11(11) 7 . . . ? P2 Ni1 P1 C17 -163.92(12) . . . . ? Br1 Ni1 P1 C17 65.56(13) . . . . ? Br1 Ni1 P1 C17 -32.72(13) 7 . . . ? P1 Ni1 P2 C6 12.35(12) . . . . ? Br1 Ni1 P2 C6 141.84(11) . . . . ? Br1 Ni1 P2 C6 -101.02(11) 7 . . . ? P1 Ni1 P2 C23 130.07(11) . . . . ? Br1 Ni1 P2 C23 -100.44(11) . . . . ? Br1 Ni1 P2 C23 16.70(11) 7 . . . ? P1 Ni1 P2 C29 -111.93(11) . . . . ? Br1 Ni1 P2 C29 17.56(12) . . . . ? Br1 Ni1 P2 C29 134.70(11) 7 . . . ? C11 P1 C1 C2 14.8(3) . . . . ? C17 P1 C1 C2 -90.8(3) . . . . ? Ni1 P1 C1 C2 143.1(3) . . . . ? C11 P1 C1 C5 -162.4(2) . . . . ? C17 P1 C1 C5 92.0(3) . . . . ? Ni1 P1 C1 C5 -34.0(3) . . . . ? C11 P1 C1 Fe1 -77.2(2) . . . . ? C17 P1 C1 Fe1 177.14(17) . . . . ? Ni1 P1 C1 Fe1 51.08(19) . . . . ? C5 Fe1 C1 C2 117.8(3) . . . . ? C7 Fe1 C1 C2 -98.7(2) . . . . ? C6 Fe1 C1 C2 -142.98(19) . . . . ? C8 Fe1 C1 C2 -62.0(3) . . . . ? C10 Fe1 C1 C2 -179.5(2) . . . . ? C3 Fe1 C1 C2 37.20(19) . . . . ? C9 Fe1 C1 C2 -114(8) . . . . ? C4 Fe1 C1 C2 80.3(2) . . . . ? C7 Fe1 C1 C5 143.45(18) . . . . ? C6 Fe1 C1 C5 99.17(19) . . . . ? C2 Fe1 C1 C5 -117.8(3) . . . . ? C8 Fe1 C1 C5 -179.87(19) . . . . ? C10 Fe1 C1 C5 62.7(3) . . . . ? C3 Fe1 C1 C5 -80.6(2) . . . . ? C9 Fe1 C1 C5 128(8) . . . . ? C4 Fe1 C1 C5 -37.54(18) . . . . ? C5 Fe1 C1 P1 -115.6(3) . . . . ? C7 Fe1 C1 P1 27.9(2) . . . . ? C6 Fe1 C1 P1 -16.4(2) . . . . ? C2 Fe1 C1 P1 126.6(3) . . . . ? C8 Fe1 C1 P1 64.6(3) . . . . ? C10 Fe1 C1 P1 -52.9(3) . . . . ? C3 Fe1 C1 P1 163.8(2) . . . . ? C9 Fe1 C1 P1 13(8) . . . . ? C4 Fe1 C1 P1 -153.1(2) . . . . ? C5 C1 C2 C3 0.7(3) . . . . ? P1 C1 C2 C3 -176.8(2) . . . . ? Fe1 C1 C2 C3 -59.3(2) . . . . ? C5 C1 C2 Fe1 60.0(2) . . . . ? P1 C1 C2 Fe1 -117.5(3) . . . . ? C1 Fe1 C2 C3 119.6(3) . . . . ? C5 Fe1 C2 C3 80.5(2) . . . . ? C7 Fe1 C2 C3 -142.59(19) . . . . ? C6 Fe1 C2 C3 178.9(2) . . . . ? C8 Fe1 C2 C3 -98.8(2) . . . . ? C10 Fe1 C2 C3 -121(21) . . . . ? C9 Fe1 C2 C3 -61.6(3) . . . . ? C4 Fe1 C2 C3 36.77(19) . . . . ? C5 Fe1 C2 C1 -39.08(18) . . . . ? C7 Fe1 C2 C1 97.79(19) . . . . ? C6 Fe1 C2 C1 59.2(3) . . . . ? C8 Fe1 C2 C1 141.55(18) . . . . ? C10 Fe1 C2 C1 119(21) . . . . ? C3 Fe1 C2 C1 -119.6(3) . . . . ? C9 Fe1 C2 C1 178.8(2) . . . . ? C4 Fe1 C2 C1 -82.8(2) . . . . ? C1 C2 C3 C4 -0.9(4) . . . . ? Fe1 C2 C3 C4 -59.1(2) . . . . ? C1 C2 C3 Fe1 58.2(2) . . . . ? C1 Fe1 C3 C4 82.5(2) . . . . ? C5 Fe1 C3 C4 37.42(19) . . . . ? C7 Fe1 C3 C4 -179.9(2) . . . . ? C6 Fe1 C3 C4 73(8) . . . . ? C2 Fe1 C3 C4 120.4(3) . . . . ? C8 Fe1 C3 C4 -141.7(2) . . . . ? C10 Fe1 C3 C4 -60.2(3) . . . . ? C9 Fe1 C3 C4 -98.0(2) . . . . ? C1 Fe1 C3 C2 -37.90(18) . . . . ? C5 Fe1 C3 C2 -83.0(2) . . . . ? C7 Fe1 C3 C2 59.7(3) . . . . ? C6 Fe1 C3 C2 -47(8) . . . . ? C8 Fe1 C3 C2 98.0(2) . . . . ? C10 Fe1 C3 C2 179.46(19) . . . . ? C9 Fe1 C3 C2 141.64(19) . . . . ? C4 Fe1 C3 C2 -120.4(3) . . . . ? C2 C3 C4 C5 0.8(4) . . . . ? Fe1 C3 C4 C5 -57.9(2) . . . . ? C2 C3 C4 Fe1 58.6(2) . . . . ? C1 Fe1 C4 C3 -81.4(2) . . . . ? C5 Fe1 C4 C3 -120.0(3) . . . . ? C7 Fe1 C4 C3 3(9) . . . . ? C6 Fe1 C4 C3 -178.48(19) . . . . ? C2 Fe1 C4 C3 -37.04(19) . . . . ? C8 Fe1 C4 C3 61.1(3) . . . . ? C10 Fe1 C4 C3 142.80(19) . . . . ? C9 Fe1 C4 C3 98.8(2) . . . . ? C1 Fe1 C4 C5 38.55(18) . . . . ? C7 Fe1 C4 C5 123(9) . . . . ? C6 Fe1 C4 C5 -58.5(3) . . . . ? C2 Fe1 C4 C5 82.9(2) . . . . ? C8 Fe1 C4 C5 -178.9(2) . . . . ? C10 Fe1 C4 C5 -97.2(2) . . . . ? C3 Fe1 C4 C5 120.0(3) . . . . ? C9 Fe1 C4 C5 -141.21(19) . . . . ? C3 C4 C5 C1 -0.3(4) . . . . ? Fe1 C4 C5 C1 -59.0(2) . . . . ? C3 C4 C5 Fe1 58.7(2) . . . . ? C2 C1 C5 C4 -0.2(3) . . . . ? P1 C1 C5 C4 177.5(2) . . . . ? Fe1 C1 C5 C4 60.4(2) . . . . ? C2 C1 C5 Fe1 -60.6(2) . . . . ? P1 C1 C5 Fe1 117.2(2) . . . . ? C1 Fe1 C5 C4 -119.0(3) . . . . ? C7 Fe1 C5 C4 -178.8(2) . . . . ? C6 Fe1 C5 C4 143.69(19) . . . . ? C2 Fe1 C5 C4 -80.5(2) . . . . ? C8 Fe1 C5 C4 55(10) . . . . ? C10 Fe1 C5 C4 99.7(2) . . . . ? C3 Fe1 C5 C4 -37.0(2) . . . . ? C9 Fe1 C5 C4 62.0(3) . . . . ? C7 Fe1 C5 C1 -59.8(3) . . . . ? C6 Fe1 C5 C1 -97.28(19) . . . . ? C2 Fe1 C5 C1 38.56(18) . . . . ? C8 Fe1 C5 C1 174(100) . . . . ? C10 Fe1 C5 C1 -141.28(18) . . . . ? C3 Fe1 C5 C1 82.1(2) . . . . ? C9 Fe1 C5 C1 -178.94(19) . . . . ? C4 Fe1 C5 C1 119.0(3) . . . . ? C23 P2 C6 C10 -12.7(3) . . . . ? C29 P2 C6 C10 -117.1(3) . . . . ? Ni1 P2 C6 C10 110.6(3) . . . . ? C23 P2 C6 C7 168.5(3) . . . . ? C29 P2 C6 C7 64.1(3) . . . . ? Ni1 P2 C6 C7 -68.2(3) . . . . ? C23 P2 C6 Fe1 -102.76(19) . . . . ? C29 P2 C6 Fe1 152.77(18) . . . . ? Ni1 P2 C6 Fe1 20.5(2) . . . . ? C1 Fe1 C6 C10 -143.44(18) . . . . ? C5 Fe1 C6 C10 -98.69(19) . . . . ? C7 Fe1 C6 C10 117.8(2) . . . . ? C2 Fe1 C6 C10 179.46(19) . . . . ? C8 Fe1 C6 C10 80.41(19) . . . . ? C3 Fe1 C6 C10 -134(8) . . . . ? C9 Fe1 C6 C10 37.01(18) . . . . ? C4 Fe1 C6 C10 -62.2(2) . . . . ? C1 Fe1 C6 C7 98.77(18) . . . . ? C5 Fe1 C6 C7 143.53(18) . . . . ? C2 Fe1 C6 C7 61.7(2) . . . . ? C8 Fe1 C6 C7 -37.37(18) . . . . ? C10 Fe1 C6 C7 -117.8(2) . . . . ? C3 Fe1 C6 C7 108(8) . . . . ? C9 Fe1 C6 C7 -80.77(19) . . . . ? C4 Fe1 C6 C7 -180.0(2) . . . . ? C1 Fe1 C6 P2 -22.0(2) . . . . ? C5 Fe1 C6 P2 22.8(2) . . . . ? C7 Fe1 C6 P2 -120.8(3) . . . . ? C2 Fe1 C6 P2 -59.1(3) . . . . ? C8 Fe1 C6 P2 -158.1(2) . . . . ? C10 Fe1 C6 P2 121.5(3) . . . . ? C3 Fe1 C6 P2 -13(8) . . . . ? C9 Fe1 C6 P2 158.5(2) . . . . ? C4 Fe1 C6 P2 59.3(3) . . . . ? C10 C6 C7 C8 -0.7(3) . . . . ? P2 C6 C7 C8 178.3(2) . . . . ? Fe1 C6 C7 C8 59.7(2) . . . . ? C10 C6 C7 Fe1 -60.4(2) . . . . ? P2 C6 C7 Fe1 118.6(2) . . . . ? C1 Fe1 C7 C8 143.07(19) . . . . ? C5 Fe1 C7 C8 -179.0(2) . . . . ? C6 Fe1 C7 C8 -119.5(3) . . . . ? C2 Fe1 C7 C8 98.8(2) . . . . ? C10 Fe1 C7 C8 -81.0(2) . . . . ? C3 Fe1 C7 C8 62.0(3) . . . . ? C9 Fe1 C7 C8 -37.18(19) . . . . ? C4 Fe1 C7 C8 59(9) . . . . ? C1 Fe1 C7 C6 -97.41(18) . . . . ? C5 Fe1 C7 C6 -59.4(3) . . . . ? C2 Fe1 C7 C6 -141.66(17) . . . . ? C8 Fe1 C7 C6 119.5(3) . . . . ? C10 Fe1 C7 C6 38.50(17) . . . . ? C3 Fe1 C7 C6 -178.51(19) . . . . ? C9 Fe1 C7 C6 82.34(18) . . . . ? C4 Fe1 C7 C6 179(100) . . . . ? C6 C7 C8 C9 0.0(4) . . . . ? Fe1 C7 C8 C9 59.2(2) . . . . ? C6 C7 C8 Fe1 -59.2(2) . . . . ? C1 Fe1 C8 C9 -178.92(19) . . . . ? C5 Fe1 C8 C9 7(10) . . . . ? C7 Fe1 C8 C9 -119.9(3) . . . . ? C6 Fe1 C8 C9 -81.9(2) . . . . ? C2 Fe1 C8 C9 142.38(19) . . . . ? C10 Fe1 C8 C9 -37.78(19) . . . . ? C3 Fe1 C8 C9 98.8(2) . . . . ? C4 Fe1 C8 C9 61.3(3) . . . . ? C1 Fe1 C8 C7 -59.1(3) . . . . ? C5 Fe1 C8 C7 127(10) . . . . ? C6 Fe1 C8 C7 38.00(18) . . . . ? C2 Fe1 C8 C7 -97.7(2) . . . . ? C10 Fe1 C8 C7 82.1(2) . . . . ? C3 Fe1 C8 C7 -141.37(19) . . . . ? C9 Fe1 C8 C7 119.9(3) . . . . ? C4 Fe1 C8 C7 -178.8(2) . . . . ? C7 C8 C9 C10 0.6(4) . . . . ? Fe1 C8 C9 C10 59.2(2) . . . . ? C7 C8 C9 Fe1 -58.6(2) . . . . ? C1 Fe1 C9 C8 53(8) . . . . ? C5 Fe1 C9 C8 -179.8(2) . . . . ? C7 Fe1 C9 C8 37.40(18) . . . . ? C6 Fe1 C9 C8 81.9(2) . . . . ? C2 Fe1 C9 C8 -60.3(3) . . . . ? C10 Fe1 C9 C8 119.2(3) . . . . ? C3 Fe1 C9 C8 -98.2(2) . . . . ? C4 Fe1 C9 C8 -141.6(2) . . . . ? C1 Fe1 C9 C10 -66(8) . . . . ? C5 Fe1 C9 C10 61.0(3) . . . . ? C7 Fe1 C9 C10 -81.8(2) . . . . ? C6 Fe1 C9 C10 -37.25(18) . . . . ? C2 Fe1 C9 C10 -179.5(2) . . . . ? C8 Fe1 C9 C10 -119.2(3) . . . . ? C3 Fe1 C9 C10 142.6(2) . . . . ? C4 Fe1 C9 C10 99.2(2) . . . . ? C8 C9 C10 C6 -1.0(4) . . . . ? Fe1 C9 C10 C6 58.2(2) . . . . ? C8 C9 C10 Fe1 -59.2(2) . . . . ? C7 C6 C10 C9 1.0(3) . . . . ? P2 C6 C10 C9 -178.0(2) . . . . ? Fe1 C6 C10 C9 -58.7(2) . . . . ? C7 C6 C10 Fe1 59.77(19) . . . . ? P2 C6 C10 Fe1 -119.2(2) . . . . ? C1 Fe1 C10 C9 178.8(2) . . . . ? C5 Fe1 C10 C9 -141.8(2) . . . . ? C7 Fe1 C10 C9 81.4(2) . . . . ? C6 Fe1 C10 C9 120.3(3) . . . . ? C2 Fe1 C10 C9 60(21) . . . . ? C8 Fe1 C10 C9 37.6(2) . . . . ? C3 Fe1 C10 C9 -60.8(3) . . . . ? C4 Fe1 C10 C9 -97.9(2) . . . . ? C1 Fe1 C10 C6 58.4(3) . . . . ? C5 Fe1 C10 C6 97.85(19) . . . . ? C7 Fe1 C10 C6 -38.91(17) . . . . ? C2 Fe1 C10 C6 -60(21) . . . . ? C8 Fe1 C10 C6 -82.79(19) . . . . ? C3 Fe1 C10 C6 178.9(2) . . . . ? C9 Fe1 C10 C6 -120.3(3) . . . . ? C4 Fe1 C10 C6 141.74(17) . . . . ? C1 P1 C11 C12 116.3(3) . . . . ? C17 P1 C11 C12 -137.8(3) . . . . ? Ni1 P1 C11 C12 -11.5(3) . . . . ? C1 P1 C11 C16 -66.9(3) . . . . ? C17 P1 C11 C16 39.1(3) . . . . ? Ni1 P1 C11 C16 165.4(2) . . . . ? C16 C11 C12 C13 1.3(5) . . . . ? P1 C11 C12 C13 178.3(3) . . . . ? C11 C12 C13 C14 -0.6(5) . . . . ? C12 C13 C14 C15 -0.5(6) . . . . ? C13 C14 C15 C16 0.9(6) . . . . ? C14 C15 C16 C11 -0.2(6) . . . . ? C12 C11 C16 C15 -0.9(5) . . . . ? P1 C11 C16 C15 -177.8(3) . . . . ? C1 P1 C17 C22 -14.1(3) . . . . ? C11 P1 C17 C22 -123.2(3) . . . . ? Ni1 P1 C17 C22 110.9(2) . . . . ? C1 P1 C17 C18 167.2(3) . . . . ? C11 P1 C17 C18 58.1(3) . . . . ? Ni1 P1 C17 C18 -67.7(3) . . . . ? C22 C17 C18 C19 0.9(5) . . . . ? P1 C17 C18 C19 179.6(3) . . . . ? C17 C18 C19 C20 0.1(6) . . . . ? C18 C19 C20 C21 -1.4(6) . . . . ? C19 C20 C21 C22 1.5(6) . . . . ? C20 C21 C22 C17 -0.5(5) . . . . ? C18 C17 C22 C21 -0.7(5) . . . . ? P1 C17 C22 C21 -179.4(3) . . . . ? C6 P2 C23 C24 101.6(3) . . . . ? C29 P2 C23 C24 -154.7(3) . . . . ? Ni1 P2 C23 C24 -27.2(3) . . . . ? C6 P2 C23 C28 -78.9(3) . . . . ? C29 P2 C23 C28 24.8(3) . . . . ? Ni1 P2 C23 C28 152.3(2) . . . . ? C28 C23 C24 C25 -0.1(5) . . . . ? P2 C23 C24 C25 179.4(3) . . . . ? C23 C24 C25 C26 0.2(5) . . . . ? C24 C25 C26 C27 -0.7(6) . . . . ? C25 C26 C27 C28 1.1(5) . . . . ? C24 C23 C28 C27 0.6(5) . . . . ? P2 C23 C28 C27 -178.9(3) . . . . ? C26 C27 C28 C23 -1.1(5) . . . . ? C6 P2 C29 C34 -167.7(3) . . . . ? C23 P2 C29 C34 88.7(3) . . . . ? Ni1 P2 C29 C34 -34.5(3) . . . . ? C6 P2 C29 C30 12.4(3) . . . . ? C23 P2 C29 C30 -91.2(3) . . . . ? Ni1 P2 C29 C30 145.7(3) . . . . ? C34 C29 C30 C31 0.7(5) . . . . ? P2 C29 C30 C31 -179.4(3) . . . . ? C29 C30 C31 C32 0.7(6) . . . . ? C30 C31 C32 C33 -2.0(6) . . . . ? C31 C32 C33 C34 1.9(7) . . . . ? C30 C29 C34 C33 -0.9(5) . . . . ? P2 C29 C34 C33 179.3(3) . . . . ? C32 C33 C34 C29 -0.4(6) . . . . ? O1S C1S C2S C2S 14.0(8) . . . 2_655 ? _diffrn_measured_fraction_theta_max 0.908 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.866 _refine_diff_density_min -0.753 _refine_diff_density_rms 0.095 #===END #---------------------------------------------------- #------------- IODIDE------------------------------ #--------------------------------------------------- data_nelson_desperatefoo _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H56 Fe2 I2 Ni2 P4' _chemical_formula_weight 1479.93 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 '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' '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.853(2) _cell_length_b 13.508(3) _cell_length_c 14.046(4) _cell_angle_alpha 65.71(3) _cell_angle_beta 73.50(3) _cell_angle_gamma 72.75(2) _cell_volume 1436.6(6) _cell_formula_units_Z 1 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 1248 _cell_measurement_theta_min 3.1740 _cell_measurement_theta_max 21.9996 _exptl_crystal_description 'non-single sliver' _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.711 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 738 _exptl_absorpt_coefficient_mu 2.369 _exptl_absorpt_correction_T_min 0.93412 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 'Oxford Diffraction Xcalibur E' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6036 _diffrn_reflns_av_R_equivalents 0.0706 _diffrn_reflns_av_sigmaI/netI 0.1562 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.18 _diffrn_reflns_theta_max 22.05 _reflns_number_total 3515 _reflns_number_gt 2278 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'CrysalisPro' _computing_cell_refinement 'CrysalisPro' _computing_data_reduction 'CrysalisPro' _computing_structure_solution 'SIR92' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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^ > 2\s(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^)+(0.0299P)^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 3515 _refine_ls_number_parameters 352 _refine_ls_number_restraints 272 _refine_ls_R_factor_all 0.1191 _refine_ls_R_factor_gt 0.0678 _refine_ls_wR_factor_ref 0.1357 _refine_ls_wR_factor_gt 0.1143 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.024 _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 0.90534(18) 0.61293(13) -0.09411(13) 0.0193(4) Uani 1 1 d . . . Fe1 Fe 0.5158(2) 0.84610(15) -0.21846(14) 0.0212(5) Uani 1 1 d . . . I1 I 0.78847(10) 0.45388(8) 0.07344(7) 0.0257(3) Uani 1 1 d . . . P1 P 0.7832(4) 0.7643(3) -0.0569(3) 0.0199(9) Uani 1 1 d . . . P2 P 0.8619(4) 0.6583(3) -0.2572(3) 0.0195(9) Uani 1 1 d . . . C1 C 0.5758(14) 0.8149(11) -0.0803(9) 0.021(3) Uani 1 1 d U . . C2 C 0.4875(14) 0.9242(11) -0.1170(9) 0.026(3) Uani 1 1 d U . . H2 H 0.5260 0.9891 -0.1336 0.031 Uiso 1 1 calc R . . C3 C 0.3350(15) 0.9232(11) -0.1255(10) 0.029(3) Uani 1 1 d U . . H3 H 0.2525 0.9864 -0.1481 0.035 Uiso 1 1 calc R . . C4 C 0.3251(14) 0.8102(11) -0.0941(10) 0.026(3) Uani 1 1 d U . . H4 H 0.2353 0.7849 -0.0934 0.031 Uiso 1 1 calc R . . C5 C 0.4718(13) 0.7427(11) -0.0642(9) 0.023(3) Uani 1 1 d U . . H5 H 0.4975 0.6639 -0.0382 0.028 Uiso 1 1 calc R . . C6 C 0.8640(13) 0.8903(10) -0.1288(10) 0.019(3) Uani 1 1 d U . . C7 C 0.9745(13) 0.9018(10) -0.2251(10) 0.024(3) Uani 1 1 d U . . H7 H 1.0155 0.8406 -0.2485 0.028 Uiso 1 1 calc R . . C8 C 1.0248(14) 1.0009(10) -0.2863(10) 0.025(3) Uani 1 1 d U . . H8 H 1.0972 1.0077 -0.3522 0.030 Uiso 1 1 calc R . . C9 C 0.9715(15) 1.0875(11) -0.2530(10) 0.032(3) Uani 1 1 d U . . H9 H 1.0063 1.1551 -0.2962 0.038 Uiso 1 1 calc R . . C10 C 0.8672(14) 1.0805(11) -0.1572(11) 0.030(3) Uani 1 1 d U . . H10 H 0.8306 1.1424 -0.1347 0.036 Uiso 1 1 calc R . . C11 C 0.8171(14) 0.9818(10) -0.0949(10) 0.026(3) Uani 1 1 d U . . H11 H 0.7494 0.9754 -0.0275 0.031 Uiso 1 1 calc R . . C12 C 0.7596(13) 0.7503(10) 0.0807(9) 0.018(3) Uani 1 1 d U . . C13 C 0.6142(13) 0.7864(9) 0.1408(9) 0.018(3) Uani 1 1 d U . . H13 H 0.5205 0.8180 0.1098 0.022 Uiso 1 1 calc R . . C14 C 0.6035(14) 0.7773(10) 0.2423(10) 0.024(3) Uani 1 1 d U . . H14 H 0.5025 0.8029 0.2803 0.029 Uiso 1 1 calc R . . C15 C 0.7362(15) 0.7315(11) 0.2921(10) 0.030(3) Uani 1 1 d U . . H15 H 0.7271 0.7250 0.3634 0.035 Uiso 1 1 calc R . . C16 C 0.8829(14) 0.6956(10) 0.2339(10) 0.028(3) Uani 1 1 d U . . H16 H 0.9756 0.6634 0.2659 0.033 Uiso 1 1 calc R . . C17 C 0.8945(15) 0.7062(10) 0.1308(10) 0.027(3) Uani 1 1 d U . . H17 H 0.9965 0.6832 0.0921 0.033 Uiso 1 1 calc R . . C18 C 0.7040(13) 0.7763(10) -0.3105(9) 0.017(3) Uani 1 1 d U . . C19 C 0.6931(14) 0.8924(10) -0.3423(9) 0.022(3) Uani 1 1 d U . . H19 H 0.7735 0.9259 -0.3424 0.027 Uiso 1 1 calc R . . C20 C 0.5408(14) 0.9505(11) -0.3743(10) 0.028(3) Uani 1 1 d U . . H20 H 0.5040 1.0287 -0.4011 0.033 Uiso 1 1 calc R . . C21 C 0.4592(15) 0.8732(11) -0.3592(10) 0.030(3) Uani 1 1 d U . . H21 H 0.3535 0.8892 -0.3725 0.036 Uiso 1 1 calc R . . C22 C 0.5544(14) 0.7642(11) -0.3204(10) 0.031(3) Uani 1 1 d U . . H22 H 0.5241 0.6964 -0.3042 0.037 Uiso 1 1 calc R . . C23 C 1.0444(14) 0.6838(11) -0.3566(10) 0.021(3) Uani 1 1 d U . . C24 C 1.1789(14) 0.5985(11) -0.3397(10) 0.024(3) Uani 1 1 d U . . H24 H 1.1690 0.5301 -0.2828 0.029 Uiso 1 1 calc R . . C25 C 1.3279(13) 0.6120(11) -0.4050(9) 0.023(3) Uani 1 1 d U . . H25 H 1.4180 0.5518 -0.3941 0.028 Uiso 1 1 calc R . . C26 C 1.3457(15) 0.7122(12) -0.4855(10) 0.031(3) Uani 1 1 d U . . H26 H 1.4492 0.7233 -0.5262 0.037 Uiso 1 1 calc R . . C27 C 1.2112(15) 0.7965(12) -0.5064(10) 0.032(3) Uani 1 1 d U . . H27 H 1.2220 0.8639 -0.5646 0.038 Uiso 1 1 calc R . . C28 C 1.0626(14) 0.7836(11) -0.4438(10) 0.026(3) Uani 1 1 d U . . H28 H 0.9714 0.8421 -0.4592 0.031 Uiso 1 1 calc R . . C29 C 0.8060(12) 0.5513(10) -0.2824(10) 0.018(3) Uani 1 1 d U . . C30 C 0.8402(13) 0.5537(10) -0.3877(10) 0.023(3) Uani 1 1 d U . . H30 H 0.8958 0.6066 -0.4442 0.027 Uiso 1 1 calc R . . C31 C 0.7884(14) 0.4746(11) -0.4061(10) 0.027(3) Uani 1 1 d U . . H31 H 0.8110 0.4735 -0.4760 0.033 Uiso 1 1 calc R . . C32 C 0.7063(13) 0.3995(11) -0.3247(11) 0.028(3) Uani 1 1 d U . . H32 H 0.6744 0.3462 -0.3385 0.034 Uiso 1 1 calc R . . C33 C 0.6697(14) 0.4006(11) -0.2237(10) 0.027(3) Uani 1 1 d U . . H33 H 0.6105 0.3492 -0.1683 0.033 Uiso 1 1 calc R . . C34 C 0.7191(13) 0.4777(10) -0.2008(10) 0.023(3) Uani 1 1 d U . . H34 H 0.6931 0.4788 -0.1307 0.028 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 0.0199(10) 0.0190(11) 0.0208(11) -0.0086(9) -0.0052(7) -0.0030(8) Fe1 0.0209(11) 0.0238(13) 0.0220(12) -0.0108(10) -0.0078(9) -0.0013(10) I1 0.0214(5) 0.0286(6) 0.0261(6) -0.0070(5) -0.0043(4) -0.0080(4) P1 0.020(2) 0.021(2) 0.025(2) -0.0131(19) -0.0045(16) -0.0048(18) P2 0.0158(19) 0.021(2) 0.023(2) -0.0099(18) -0.0010(16) -0.0037(17) C1 0.023(6) 0.032(7) 0.013(7) -0.014(6) 0.000(5) -0.010(5) C2 0.027(7) 0.031(6) 0.020(7) -0.010(6) -0.002(6) -0.005(5) C3 0.027(6) 0.036(6) 0.031(8) -0.026(6) -0.004(6) 0.003(6) C4 0.011(6) 0.039(7) 0.031(8) -0.018(7) -0.001(5) -0.005(5) C5 0.016(6) 0.032(6) 0.025(7) -0.011(6) -0.009(5) -0.005(5) C6 0.012(6) 0.017(6) 0.028(7) -0.009(6) -0.007(5) 0.003(5) C7 0.013(7) 0.026(6) 0.039(8) -0.019(6) -0.001(5) -0.006(6) C8 0.019(7) 0.032(7) 0.037(7) -0.017(6) -0.006(5) -0.016(6) C9 0.041(8) 0.019(7) 0.036(8) -0.005(6) -0.010(6) -0.011(6) C10 0.037(8) 0.017(6) 0.044(8) -0.019(6) -0.007(6) -0.003(6) C11 0.031(7) 0.023(7) 0.028(7) -0.014(5) -0.008(5) 0.000(6) C12 0.014(6) 0.022(7) 0.024(7) -0.013(6) 0.000(4) -0.006(6) C13 0.019(6) 0.021(7) 0.027(6) -0.020(6) -0.004(5) -0.006(6) C14 0.024(6) 0.030(8) 0.022(6) -0.018(6) -0.002(5) -0.002(6) C15 0.033(7) 0.038(8) 0.026(7) -0.016(6) -0.013(5) -0.004(6) C16 0.029(6) 0.030(8) 0.033(7) -0.019(7) -0.010(6) -0.003(6) C17 0.030(6) 0.023(7) 0.034(7) -0.016(7) -0.013(5) 0.002(6) C18 0.012(6) 0.019(6) 0.024(7) -0.009(6) -0.008(5) -0.001(5) C19 0.030(6) 0.019(6) 0.024(7) -0.014(6) -0.006(6) -0.004(5) C20 0.035(7) 0.022(6) 0.021(7) -0.009(6) -0.011(6) 0.007(5) C21 0.024(6) 0.036(7) 0.029(8) -0.009(7) -0.019(6) 0.005(5) C22 0.028(7) 0.024(6) 0.043(8) -0.010(7) -0.013(6) -0.006(5) C23 0.017(6) 0.036(7) 0.020(7) -0.019(5) -0.002(5) -0.008(5) C24 0.025(6) 0.031(7) 0.020(7) -0.010(6) 0.000(5) -0.012(5) C25 0.012(5) 0.041(7) 0.021(7) -0.017(6) -0.007(5) -0.002(6) C26 0.016(6) 0.053(8) 0.025(8) -0.013(6) 0.003(6) -0.017(6) C27 0.035(7) 0.043(8) 0.015(7) -0.007(6) 0.002(5) -0.014(6) C28 0.018(6) 0.043(7) 0.021(7) -0.013(5) -0.004(5) -0.008(6) C29 0.004(6) 0.028(7) 0.025(6) -0.013(6) -0.005(5) -0.002(5) C30 0.017(6) 0.030(7) 0.025(6) -0.014(6) 0.003(5) -0.010(5) C31 0.025(7) 0.040(8) 0.025(7) -0.022(6) -0.004(6) -0.005(6) C32 0.022(7) 0.034(8) 0.040(7) -0.025(6) -0.002(6) -0.010(6) C33 0.028(7) 0.031(7) 0.031(6) -0.015(6) -0.005(6) -0.011(6) C34 0.026(7) 0.028(7) 0.020(6) -0.016(6) 0.005(5) -0.009(6) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 2.207(4) . ? Ni1 P2 2.231(4) . ? Ni1 I1 2.646(2) . ? Ni1 I1 2.6508(19) 2_765 ? Fe1 C1 2.001(11) . ? Fe1 C19 2.004(12) . ? Fe1 C2 2.021(12) . ? Fe1 C5 2.037(12) . ? Fe1 C21 2.038(12) . ? Fe1 C18 2.046(11) . ? Fe1 C22 2.047(12) . ? Fe1 C20 2.050(13) . ? Fe1 C4 2.062(12) . ? Fe1 C3 2.072(11) . ? I1 Ni1 2.6508(19) 2_765 ? P1 C12 1.819(12) . ? P1 C6 1.824(12) . ? P1 C1 1.833(12) . ? P2 C23 1.825(12) . ? P2 C18 1.828(12) . ? P2 C29 1.845(12) . ? C1 C2 1.406(16) . ? C1 C5 1.444(15) . ? C2 C3 1.393(16) . ? C2 H2 0.9500 . ? C3 C4 1.426(17) . ? C3 H3 0.9500 . ? C4 C5 1.409(15) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C7 1.406(15) . ? C6 C11 1.413(15) . ? C7 C8 1.384(16) . ? C7 H7 0.9500 . ? C8 C9 1.345(15) . ? C8 H8 0.9500 . ? C9 C10 1.382(15) . ? C9 H9 0.9500 . ? C10 C11 1.382(16) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 C13 1.399(14) . ? C12 C17 1.410(15) . ? C13 C14 1.357(14) . ? C13 H13 0.9500 . ? C14 C15 1.389(15) . ? C14 H14 0.9500 . ? C15 C16 1.393(15) . ? C15 H15 0.9500 . ? C16 C17 1.371(15) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 C19 1.424(16) . ? C18 C22 1.432(15) . ? C19 C20 1.436(16) . ? C19 H19 0.9500 . ? C20 C21 1.355(16) . ? C20 H20 0.9500 . ? C21 C22 1.428(16) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C24 1.387(16) . ? C23 C28 1.415(17) . ? C24 C25 1.390(15) . ? C24 H24 0.9500 . ? C25 C26 1.379(17) . ? C25 H25 0.9500 . ? C26 C27 1.385(16) . ? C26 H26 0.9500 . ? C27 C28 1.374(15) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 C34 1.382(15) . ? C29 C30 1.411(15) . ? C30 C31 1.416(15) . ? C30 H30 0.9500 . ? C31 C32 1.369(16) . ? C31 H31 0.9500 . ? C32 C33 1.368(15) . ? C32 H32 0.9500 . ? C33 C34 1.416(15) . ? C33 H33 0.9500 . ? C34 H34 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 P1 Ni1 P2 102.99(14) . . ? P1 Ni1 I1 103.27(11) . . ? P2 Ni1 I1 123.05(11) . . ? P1 Ni1 I1 113.45(10) . 2_765 ? P2 Ni1 I1 115.41(10) . 2_765 ? I1 Ni1 I1 98.50(7) . 2_765 ? C1 Fe1 C19 112.0(5) . . ? C1 Fe1 C2 40.9(4) . . ? C19 Fe1 C2 110.2(5) . . ? C1 Fe1 C5 41.9(4) . . ? C19 Fe1 C5 143.0(5) . . ? C2 Fe1 C5 68.6(5) . . ? C1 Fe1 C21 178.2(5) . . ? C19 Fe1 C21 67.6(5) . . ? C2 Fe1 C21 140.9(5) . . ? C5 Fe1 C21 137.5(5) . . ? C1 Fe1 C18 109.8(5) . . ? C19 Fe1 C18 41.1(4) . . ? C2 Fe1 C18 136.8(5) . . ? C5 Fe1 C18 113.2(5) . . ? C21 Fe1 C18 68.7(5) . . ? C1 Fe1 C22 137.3(5) . . ? C19 Fe1 C22 68.5(5) . . ? C2 Fe1 C22 177.6(5) . . ? C5 Fe1 C22 111.1(5) . . ? C21 Fe1 C22 40.9(5) . . ? C18 Fe1 C22 41.0(4) . . ? C1 Fe1 C20 142.0(5) . . ? C19 Fe1 C20 41.5(4) . . ? C2 Fe1 C20 112.7(5) . . ? C5 Fe1 C20 175.2(5) . . ? C21 Fe1 C20 38.7(5) . . ? C18 Fe1 C20 69.3(5) . . ? C22 Fe1 C20 67.8(5) . . ? C1 Fe1 C4 69.0(5) . . ? C19 Fe1 C4 175.9(5) . . ? C2 Fe1 C4 67.8(5) . . ? C5 Fe1 C4 40.2(4) . . ? C21 Fe1 C4 111.5(5) . . ? C18 Fe1 C4 142.7(5) . . ? C22 Fe1 C4 113.6(5) . . ? C20 Fe1 C4 135.4(5) . . ? C1 Fe1 C3 68.4(5) . . ? C19 Fe1 C3 135.9(5) . . ? C2 Fe1 C3 39.8(4) . . ? C5 Fe1 C3 67.9(5) . . ? C21 Fe1 C3 113.2(5) . . ? C18 Fe1 C3 176.2(5) . . ? C22 Fe1 C3 142.5(5) . . ? C20 Fe1 C3 109.9(5) . . ? C4 Fe1 C3 40.4(5) . . ? Ni1 I1 Ni1 81.50(7) . 2_765 ? C12 P1 C6 101.9(6) . . ? C12 P1 C1 102.8(5) . . ? C6 P1 C1 101.3(6) . . ? C12 P1 Ni1 115.8(4) . . ? C6 P1 Ni1 119.8(4) . . ? C1 P1 Ni1 113.0(4) . . ? C23 P2 C18 104.8(6) . . ? C23 P2 C29 102.6(5) . . ? C18 P2 C29 98.9(5) . . ? C23 P2 Ni1 111.1(4) . . ? C18 P2 Ni1 120.9(4) . . ? C29 P2 Ni1 116.3(4) . . ? C2 C1 C5 106.8(11) . . ? C2 C1 P1 129.8(10) . . ? C5 C1 P1 123.4(10) . . ? C2 C1 Fe1 70.3(7) . . ? C5 C1 Fe1 70.4(7) . . ? P1 C1 Fe1 123.5(6) . . ? C3 C2 C1 109.8(12) . . ? C3 C2 Fe1 72.1(7) . . ? C1 C2 Fe1 68.8(7) . . ? C3 C2 H2 125.1 . . ? C1 C2 H2 125.1 . . ? Fe1 C2 H2 125.5 . . ? C2 C3 C4 107.7(12) . . ? C2 C3 Fe1 68.1(7) . . ? C4 C3 Fe1 69.4(7) . . ? C2 C3 H3 126.1 . . ? C4 C3 H3 126.1 . . ? Fe1 C3 H3 127.9 . . ? C5 C4 C3 108.0(11) . . ? C5 C4 Fe1 68.9(7) . . ? C3 C4 Fe1 70.2(7) . . ? C5 C4 H4 126.0 . . ? C3 C4 H4 126.0 . . ? Fe1 C4 H4 126.4 . . ? C4 C5 C1 107.7(11) . . ? C4 C5 Fe1 70.8(7) . . ? C1 C5 Fe1 67.7(7) . . ? C4 C5 H5 126.2 . . ? C1 C5 H5 126.2 . . ? Fe1 C5 H5 126.8 . . ? C7 C6 C11 116.4(11) . . ? C7 C6 P1 120.2(9) . . ? C11 C6 P1 123.3(9) . . ? C8 C7 C6 121.1(11) . . ? C8 C7 H7 119.4 . . ? C6 C7 H7 119.4 . . ? C9 C8 C7 120.2(12) . . ? C9 C8 H8 119.9 . . ? C7 C8 H8 119.9 . . ? C8 C9 C10 121.6(13) . . ? C8 C9 H9 119.2 . . ? C10 C9 H9 119.2 . . ? C11 C10 C9 118.8(12) . . ? C11 C10 H10 120.6 . . ? C9 C10 H10 120.6 . . ? C10 C11 C6 121.6(12) . . ? C10 C11 H11 119.2 . . ? C6 C11 H11 119.2 . . ? C13 C12 C17 116.2(11) . . ? C13 C12 P1 123.8(9) . . ? C17 C12 P1 119.9(9) . . ? C14 C13 C12 121.7(11) . . ? C14 C13 H13 119.1 . . ? C12 C13 H13 119.1 . . ? C13 C14 C15 121.9(12) . . ? C13 C14 H14 119.1 . . ? C15 C14 H14 119.1 . . ? C14 C15 C16 117.7(12) . . ? C14 C15 H15 121.1 . . ? C16 C15 H15 121.1 . . ? C17 C16 C15 120.5(12) . . ? C17 C16 H16 119.7 . . ? C15 C16 H16 119.7 . . ? C16 C17 C12 122.0(12) . . ? C16 C17 H17 119.0 . . ? C12 C17 H17 119.0 . . ? C19 C18 C22 106.0(11) . . ? C19 C18 P2 130.6(9) . . ? C22 C18 P2 123.2(9) . . ? C19 C18 Fe1 67.9(6) . . ? C22 C18 Fe1 69.6(7) . . ? P2 C18 Fe1 123.8(6) . . ? C18 C19 C20 108.9(11) . . ? C18 C19 Fe1 71.0(7) . . ? C20 C19 Fe1 70.9(7) . . ? C18 C19 H19 125.5 . . ? C20 C19 H19 125.5 . . ? Fe1 C19 H19 124.1 . . ? C21 C20 C19 107.3(12) . . ? C21 C20 Fe1 70.2(8) . . ? C19 C20 Fe1 67.6(7) . . ? C21 C20 H20 126.3 . . ? C19 C20 H20 126.3 . . ? Fe1 C20 H20 127.5 . . ? C20 C21 C22 110.4(11) . . ? C20 C21 Fe1 71.1(7) . . ? C22 C21 Fe1 69.9(7) . . ? C20 C21 H21 124.8 . . ? C22 C21 H21 124.8 . . ? Fe1 C21 H21 125.8 . . ? C21 C22 C18 107.2(11) . . ? C21 C22 Fe1 69.2(7) . . ? C18 C22 Fe1 69.5(7) . . ? C21 C22 H22 126.4 . . ? C18 C22 H22 126.4 . . ? Fe1 C22 H22 126.5 . . ? C24 C23 C28 118.1(11) . . ? C24 C23 P2 115.7(10) . . ? C28 C23 P2 126.1(10) . . ? C23 C24 C25 120.8(13) . . ? C23 C24 H24 119.6 . . ? C25 C24 H24 119.6 . . ? C26 C25 C24 120.3(12) . . ? C26 C25 H25 119.8 . . ? C24 C25 H25 119.8 . . ? C25 C26 C27 119.4(12) . . ? C25 C26 H26 120.3 . . ? C27 C26 H26 120.3 . . ? C28 C27 C26 120.8(13) . . ? C28 C27 H27 119.6 . . ? C26 C27 H27 119.6 . . ? C27 C28 C23 120.4(13) . . ? C27 C28 H28 119.8 . . ? C23 C28 H28 119.8 . . ? C34 C29 C30 121.4(11) . . ? C34 C29 P2 119.8(9) . . ? C30 C29 P2 118.5(9) . . ? C29 C30 C31 117.6(12) . . ? C29 C30 H30 121.2 . . ? C31 C30 H30 121.2 . . ? C32 C31 C30 121.1(12) . . ? C32 C31 H31 119.5 . . ? C30 C31 H31 119.5 . . ? C33 C32 C31 120.6(12) . . ? C33 C32 H32 119.7 . . ? C31 C32 H32 119.7 . . ? C32 C33 C34 120.7(12) . . ? C32 C33 H33 119.7 . . ? C34 C33 H33 119.7 . . ? C29 C34 C33 118.6(11) . . ? C29 C34 H34 120.7 . . ? C33 C34 H34 120.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P1 Ni1 I1 Ni1 -116.66(11) . . . 2_765 ? P2 Ni1 I1 Ni1 127.94(13) . . . 2_765 ? I1 Ni1 I1 Ni1 0.0 2_765 . . 2_765 ? P2 Ni1 P1 C12 168.8(4) . . . . ? I1 Ni1 P1 C12 39.8(4) . . . . ? I1 Ni1 P1 C12 -65.8(4) 2_765 . . . ? P2 Ni1 P1 C6 -68.6(5) . . . . ? I1 Ni1 P1 C6 162.4(5) . . . . ? I1 Ni1 P1 C6 56.9(5) 2_765 . . . ? P2 Ni1 P1 C1 50.6(5) . . . . ? I1 Ni1 P1 C1 -78.4(4) . . . . ? I1 Ni1 P1 C1 176.0(4) 2_765 . . . ? P1 Ni1 P2 C23 106.0(5) . . . . ? I1 Ni1 P2 C23 -138.5(5) . . . . ? I1 Ni1 P2 C23 -18.2(5) 2_765 . . . ? P1 Ni1 P2 C18 -17.4(5) . . . . ? I1 Ni1 P2 C18 98.1(5) . . . . ? I1 Ni1 P2 C18 -141.6(4) 2_765 . . . ? P1 Ni1 P2 C29 -137.2(4) . . . . ? I1 Ni1 P2 C29 -21.7(4) . . . . ? I1 Ni1 P2 C29 98.6(4) 2_765 . . . ? C12 P1 C1 C2 89.4(11) . . . . ? C6 P1 C1 C2 -15.7(12) . . . . ? Ni1 P1 C1 C2 -145.1(10) . . . . ? C12 P1 C1 C5 -91.8(10) . . . . ? C6 P1 C1 C5 163.1(10) . . . . ? Ni1 P1 C1 C5 33.7(11) . . . . ? C12 P1 C1 Fe1 -179.2(7) . . . . ? C6 P1 C1 Fe1 75.7(8) . . . . ? Ni1 P1 C1 Fe1 -53.7(9) . . . . ? C19 Fe1 C1 C2 95.9(8) . . . . ? C5 Fe1 C1 C2 -116.9(10) . . . . ? C21 Fe1 C1 C2 173(16) . . . . ? C18 Fe1 C1 C2 140.0(7) . . . . ? C22 Fe1 C1 C2 177.6(7) . . . . ? C20 Fe1 C1 C2 58.6(10) . . . . ? C4 Fe1 C1 C2 -79.8(8) . . . . ? C3 Fe1 C1 C2 -36.4(7) . . . . ? C19 Fe1 C1 C5 -147.2(7) . . . . ? C2 Fe1 C1 C5 116.9(10) . . . . ? C21 Fe1 C1 C5 -70(17) . . . . ? C18 Fe1 C1 C5 -103.0(7) . . . . ? C22 Fe1 C1 C5 -65.5(9) . . . . ? C20 Fe1 C1 C5 175.6(7) . . . . ? C4 Fe1 C1 C5 37.1(7) . . . . ? C3 Fe1 C1 C5 80.5(7) . . . . ? C19 Fe1 C1 P1 -29.4(9) . . . . ? C2 Fe1 C1 P1 -125.3(12) . . . . ? C5 Fe1 C1 P1 117.7(11) . . . . ? C21 Fe1 C1 P1 47(17) . . . . ? C18 Fe1 C1 P1 14.7(9) . . . . ? C22 Fe1 C1 P1 52.3(11) . . . . ? C20 Fe1 C1 P1 -66.7(11) . . . . ? C4 Fe1 C1 P1 154.8(9) . . . . ? C3 Fe1 C1 P1 -161.7(9) . . . . ? C5 C1 C2 C3 -0.6(13) . . . . ? P1 C1 C2 C3 178.3(9) . . . . ? Fe1 C1 C2 C3 60.7(8) . . . . ? C5 C1 C2 Fe1 -61.3(8) . . . . ? P1 C1 C2 Fe1 117.7(10) . . . . ? C1 Fe1 C2 C3 -120.4(11) . . . . ? C19 Fe1 C2 C3 138.9(8) . . . . ? C5 Fe1 C2 C3 -80.7(8) . . . . ? C21 Fe1 C2 C3 59.9(12) . . . . ? C18 Fe1 C2 C3 177.6(8) . . . . ? C22 Fe1 C2 C3 -163(13) . . . . ? C20 Fe1 C2 C3 94.3(9) . . . . ? C4 Fe1 C2 C3 -37.3(8) . . . . ? C19 Fe1 C2 C1 -100.6(8) . . . . ? C5 Fe1 C2 C1 39.7(7) . . . . ? C21 Fe1 C2 C1 -179.6(8) . . . . ? C18 Fe1 C2 C1 -61.9(10) . . . . ? C22 Fe1 C2 C1 -43(13) . . . . ? C20 Fe1 C2 C1 -145.3(7) . . . . ? C4 Fe1 C2 C1 83.2(8) . . . . ? C3 Fe1 C2 C1 120.4(11) . . . . ? C1 C2 C3 C4 -0.4(14) . . . . ? Fe1 C2 C3 C4 58.3(8) . . . . ? C1 C2 C3 Fe1 -58.7(8) . . . . ? C1 Fe1 C3 C2 37.4(8) . . . . ? C19 Fe1 C3 C2 -62.3(11) . . . . ? C5 Fe1 C3 C2 82.7(8) . . . . ? C21 Fe1 C3 C2 -143.5(8) . . . . ? C18 Fe1 C3 C2 -25(8) . . . . ? C22 Fe1 C3 C2 178.9(9) . . . . ? C20 Fe1 C3 C2 -101.9(8) . . . . ? C4 Fe1 C3 C2 120.1(12) . . . . ? C1 Fe1 C3 C4 -82.7(8) . . . . ? C19 Fe1 C3 C4 177.6(7) . . . . ? C2 Fe1 C3 C4 -120.1(12) . . . . ? C5 Fe1 C3 C4 -37.4(7) . . . . ? C21 Fe1 C3 C4 96.4(9) . . . . ? C18 Fe1 C3 C4 -145(8) . . . . ? C22 Fe1 C3 C4 58.8(12) . . . . ? C20 Fe1 C3 C4 138.0(8) . . . . ? C2 C3 C4 C5 1.3(14) . . . . ? Fe1 C3 C4 C5 58.8(8) . . . . ? C2 C3 C4 Fe1 -57.5(8) . . . . ? C1 Fe1 C4 C5 -38.6(7) . . . . ? C19 Fe1 C4 C5 -144(7) . . . . ? C2 Fe1 C4 C5 -82.7(8) . . . . ? C21 Fe1 C4 C5 139.6(7) . . . . ? C18 Fe1 C4 C5 57.0(11) . . . . ? C22 Fe1 C4 C5 95.2(8) . . . . ? C20 Fe1 C4 C5 176.9(7) . . . . ? C3 Fe1 C4 C5 -119.4(11) . . . . ? C1 Fe1 C4 C3 80.8(8) . . . . ? C19 Fe1 C4 C3 -24(7) . . . . ? C2 Fe1 C4 C3 36.7(8) . . . . ? C5 Fe1 C4 C3 119.4(11) . . . . ? C21 Fe1 C4 C3 -101.0(8) . . . . ? C18 Fe1 C4 C3 176.4(8) . . . . ? C22 Fe1 C4 C3 -145.4(8) . . . . ? C20 Fe1 C4 C3 -63.7(10) . . . . ? C3 C4 C5 C1 -1.7(13) . . . . ? Fe1 C4 C5 C1 57.9(8) . . . . ? C3 C4 C5 Fe1 -59.5(8) . . . . ? C2 C1 C5 C4 1.4(13) . . . . ? P1 C1 C5 C4 -177.6(8) . . . . ? Fe1 C1 C5 C4 -59.8(8) . . . . ? C2 C1 C5 Fe1 61.2(8) . . . . ? P1 C1 C5 Fe1 -117.8(8) . . . . ? C1 Fe1 C5 C4 119.3(10) . . . . ? C19 Fe1 C5 C4 176.0(8) . . . . ? C2 Fe1 C5 C4 80.5(8) . . . . ? C21 Fe1 C5 C4 -63.2(10) . . . . ? C18 Fe1 C5 C4 -146.4(7) . . . . ? C22 Fe1 C5 C4 -102.1(8) . . . . ? C20 Fe1 C5 C4 -26(6) . . . . ? C3 Fe1 C5 C4 37.5(7) . . . . ? C19 Fe1 C5 C1 56.7(11) . . . . ? C2 Fe1 C5 C1 -38.8(6) . . . . ? C21 Fe1 C5 C1 177.5(7) . . . . ? C18 Fe1 C5 C1 94.3(7) . . . . ? C22 Fe1 C5 C1 138.6(7) . . . . ? C20 Fe1 C5 C1 -146(5) . . . . ? C4 Fe1 C5 C1 -119.3(10) . . . . ? C3 Fe1 C5 C1 -81.8(7) . . . . ? C12 P1 C6 C7 146.4(10) . . . . ? C1 P1 C6 C7 -107.7(10) . . . . ? Ni1 P1 C6 C7 17.2(11) . . . . ? C12 P1 C6 C11 -36.0(12) . . . . ? C1 P1 C6 C11 69.9(11) . . . . ? Ni1 P1 C6 C11 -165.2(9) . . . . ? C11 C6 C7 C8 -4.5(18) . . . . ? P1 C6 C7 C8 173.3(10) . . . . ? C6 C7 C8 C9 1.8(19) . . . . ? C7 C8 C9 C10 1(2) . . . . ? C8 C9 C10 C11 0(2) . . . . ? C9 C10 C11 C6 -3(2) . . . . ? C7 C6 C11 C10 5.0(19) . . . . ? P1 C6 C11 C10 -172.7(10) . . . . ? C6 P1 C12 C13 97.5(11) . . . . ? C1 P1 C12 C13 -7.2(12) . . . . ? Ni1 P1 C12 C13 -130.8(9) . . . . ? C6 P1 C12 C17 -79.1(11) . . . . ? C1 P1 C12 C17 176.2(10) . . . . ? Ni1 P1 C12 C17 52.6(11) . . . . ? C17 C12 C13 C14 -1.2(18) . . . . ? P1 C12 C13 C14 -177.9(9) . . . . ? C12 C13 C14 C15 -0.1(19) . . . . ? C13 C14 C15 C16 1(2) . . . . ? C14 C15 C16 C17 0.5(19) . . . . ? C15 C16 C17 C12 -2(2) . . . . ? C13 C12 C17 C16 2.2(19) . . . . ? P1 C12 C17 C16 179.1(10) . . . . ? C23 P2 C18 C19 -56.5(12) . . . . ? C29 P2 C18 C19 -162.2(11) . . . . ? Ni1 P2 C18 C19 69.8(12) . . . . ? C23 P2 C18 C22 128.4(10) . . . . ? C29 P2 C18 C22 22.8(11) . . . . ? Ni1 P2 C18 C22 -105.2(10) . . . . ? C23 P2 C18 Fe1 -145.2(7) . . . . ? C29 P2 C18 Fe1 109.2(7) . . . . ? Ni1 P2 C18 Fe1 -18.9(9) . . . . ? C1 Fe1 C18 C19 -101.1(8) . . . . ? C2 Fe1 C18 C19 -63.2(10) . . . . ? C5 Fe1 C18 C19 -146.1(7) . . . . ? C21 Fe1 C18 C19 80.0(8) . . . . ? C22 Fe1 C18 C19 118.0(11) . . . . ? C20 Fe1 C18 C19 38.4(7) . . . . ? C4 Fe1 C18 C19 177.8(8) . . . . ? C3 Fe1 C18 C19 -40(8) . . . . ? C1 Fe1 C18 C22 140.9(8) . . . . ? C19 Fe1 C18 C22 -118.0(11) . . . . ? C2 Fe1 C18 C22 178.8(8) . . . . ? C5 Fe1 C18 C22 95.8(8) . . . . ? C21 Fe1 C18 C22 -38.1(8) . . . . ? C20 Fe1 C18 C22 -79.7(8) . . . . ? C4 Fe1 C18 C22 59.7(11) . . . . ? C3 Fe1 C18 C22 -158(8) . . . . ? C1 Fe1 C18 P2 23.9(9) . . . . ? C19 Fe1 C18 P2 125.0(11) . . . . ? C2 Fe1 C18 P2 61.8(11) . . . . ? C5 Fe1 C18 P2 -21.1(8) . . . . ? C21 Fe1 C18 P2 -155.0(9) . . . . ? C22 Fe1 C18 P2 -117.0(11) . . . . ? C20 Fe1 C18 P2 163.4(9) . . . . ? C4 Fe1 C18 P2 -57.2(11) . . . . ? C3 Fe1 C18 P2 85(8) . . . . ? C22 C18 C19 C20 -1.7(13) . . . . ? P2 C18 C19 C20 -177.4(9) . . . . ? Fe1 C18 C19 C20 -61.1(8) . . . . ? C22 C18 C19 Fe1 59.4(8) . . . . ? P2 C18 C19 Fe1 -116.3(10) . . . . ? C1 Fe1 C19 C18 95.4(8) . . . . ? C2 Fe1 C19 C18 139.4(7) . . . . ? C5 Fe1 C19 C18 58.4(11) . . . . ? C21 Fe1 C19 C18 -82.7(8) . . . . ? C22 Fe1 C19 C18 -38.4(7) . . . . ? C20 Fe1 C19 C18 -118.8(10) . . . . ? C4 Fe1 C19 C18 -161(7) . . . . ? C3 Fe1 C19 C18 176.5(7) . . . . ? C1 Fe1 C19 C20 -145.8(7) . . . . ? C2 Fe1 C19 C20 -101.8(8) . . . . ? C5 Fe1 C19 C20 177.2(8) . . . . ? C21 Fe1 C19 C20 36.1(7) . . . . ? C18 Fe1 C19 C20 118.8(10) . . . . ? C22 Fe1 C19 C20 80.3(8) . . . . ? C4 Fe1 C19 C20 -42(7) . . . . ? C3 Fe1 C19 C20 -64.7(10) . . . . ? C18 C19 C20 C21 2.0(14) . . . . ? Fe1 C19 C20 C21 -59.1(9) . . . . ? C18 C19 C20 Fe1 61.2(8) . . . . ? C1 Fe1 C20 C21 177.4(8) . . . . ? C19 Fe1 C20 C21 119.5(10) . . . . ? C2 Fe1 C20 C21 -145.3(7) . . . . ? C5 Fe1 C20 C21 -40(6) . . . . ? C18 Fe1 C20 C21 81.4(8) . . . . ? C22 Fe1 C20 C21 37.2(7) . . . . ? C4 Fe1 C20 C21 -64.4(10) . . . . ? C3 Fe1 C20 C21 -102.6(8) . . . . ? C1 Fe1 C20 C19 57.9(10) . . . . ? C2 Fe1 C20 C19 95.3(7) . . . . ? C5 Fe1 C20 C19 -160(5) . . . . ? C21 Fe1 C20 C19 -119.5(10) . . . . ? C18 Fe1 C20 C19 -38.1(7) . . . . ? C22 Fe1 C20 C19 -82.2(7) . . . . ? C4 Fe1 C20 C19 176.1(7) . . . . ? C3 Fe1 C20 C19 138.0(7) . . . . ? C19 C20 C21 C22 -1.5(14) . . . . ? Fe1 C20 C21 C22 -59.0(9) . . . . ? C19 C20 C21 Fe1 57.5(8) . . . . ? C1 Fe1 C21 C20 -116(16) . . . . ? C19 Fe1 C21 C20 -38.6(7) . . . . ? C2 Fe1 C21 C20 56.3(11) . . . . ? C5 Fe1 C21 C20 175.4(7) . . . . ? C18 Fe1 C21 C20 -83.1(8) . . . . ? C22 Fe1 C21 C20 -121.2(11) . . . . ? C4 Fe1 C21 C20 137.1(8) . . . . ? C3 Fe1 C21 C20 93.3(8) . . . . ? C1 Fe1 C21 C22 5(17) . . . . ? C19 Fe1 C21 C22 82.6(8) . . . . ? C2 Fe1 C21 C22 177.5(8) . . . . ? C5 Fe1 C21 C22 -63.5(10) . . . . ? C18 Fe1 C21 C22 38.1(7) . . . . ? C20 Fe1 C21 C22 121.2(11) . . . . ? C4 Fe1 C21 C22 -101.7(8) . . . . ? C3 Fe1 C21 C22 -145.5(8) . . . . ? C20 C21 C22 C18 0.5(14) . . . . ? Fe1 C21 C22 C18 -59.3(8) . . . . ? C20 C21 C22 Fe1 59.7(9) . . . . ? C19 C18 C22 C21 0.8(13) . . . . ? P2 C18 C22 C21 176.9(8) . . . . ? Fe1 C18 C22 C21 59.1(8) . . . . ? C19 C18 C22 Fe1 -58.3(8) . . . . ? P2 C18 C22 Fe1 117.8(9) . . . . ? C1 Fe1 C22 C21 -179.8(8) . . . . ? C19 Fe1 C22 C21 -80.1(8) . . . . ? C2 Fe1 C22 C21 -139(13) . . . . ? C5 Fe1 C22 C21 139.6(7) . . . . ? C18 Fe1 C22 C21 -118.8(11) . . . . ? C20 Fe1 C22 C21 -35.3(7) . . . . ? C4 Fe1 C22 C21 96.1(8) . . . . ? C3 Fe1 C22 C21 58.9(12) . . . . ? C1 Fe1 C22 C18 -61.0(10) . . . . ? C19 Fe1 C22 C18 38.6(7) . . . . ? C2 Fe1 C22 C18 -20(13) . . . . ? C5 Fe1 C22 C18 -101.6(8) . . . . ? C21 Fe1 C22 C18 118.8(11) . . . . ? C20 Fe1 C22 C18 83.5(8) . . . . ? C4 Fe1 C22 C18 -145.2(7) . . . . ? C3 Fe1 C22 C18 177.6(9) . . . . ? C18 P2 C23 C24 -173.0(8) . . . . ? C29 P2 C23 C24 -70.1(10) . . . . ? Ni1 P2 C23 C24 54.8(9) . . . . ? C18 P2 C23 C28 11.2(12) . . . . ? C29 P2 C23 C28 114.1(11) . . . . ? Ni1 P2 C23 C28 -121.0(10) . . . . ? C28 C23 C24 C25 1.6(17) . . . . ? P2 C23 C24 C25 -174.5(9) . . . . ? C23 C24 C25 C26 2.5(18) . . . . ? C24 C25 C26 C27 -5.3(18) . . . . ? C25 C26 C27 C28 4.0(18) . . . . ? C26 C27 C28 C23 0.1(18) . . . . ? C24 C23 C28 C27 -2.9(17) . . . . ? P2 C23 C28 C27 172.8(9) . . . . ? C23 P2 C29 C34 153.0(10) . . . . ? C18 P2 C29 C34 -99.5(10) . . . . ? Ni1 P2 C29 C34 31.6(11) . . . . ? C23 P2 C29 C30 -33.0(10) . . . . ? C18 P2 C29 C30 74.4(10) . . . . ? Ni1 P2 C29 C30 -154.5(8) . . . . ? C34 C29 C30 C31 -2.8(17) . . . . ? P2 C29 C30 C31 -176.6(8) . . . . ? C29 C30 C31 C32 0.9(17) . . . . ? C30 C31 C32 C33 1.2(19) . . . . ? C31 C32 C33 C34 -1.4(19) . . . . ? C30 C29 C34 C33 2.6(17) . . . . ? P2 C29 C34 C33 176.3(9) . . . . ? C32 C33 C34 C29 -0.4(18) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 22.05 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.893 _refine_diff_density_min -0.734 _refine_diff_density_rms 0.176 #===END