# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_shelxl _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H24 Fe N6 Pt' _chemical_formula_weight 815.57 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 '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 7.2452(2) _cell_length_b 13.9706(5) _cell_length_c 16.3779(7) _cell_angle_alpha 73.531(3) _cell_angle_beta 83.678(3) _cell_angle_gamma 89.998(3) _cell_volume 1579.24(10) _cell_formula_units_Z 2 _cell_measurement_temperature 120(1) _cell_measurement_reflns_used 100 _cell_measurement_theta_min 12 _cell_measurement_theta_max 20 _exptl_crystal_description prismatic _exptl_crystal_colour red _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.715 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 796 _exptl_absorpt_coefficient_mu 4.921 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5897 _exptl_absorpt_correction_T_max 0.6942 _exptl_absorpt_process_details 'Empirical absorption correction:XABS2' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(1) _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30408 _diffrn_reflns_av_R_equivalents 0.0403 _diffrn_reflns_av_sigmaI/netI 0.0461 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.95 _diffrn_reflns_theta_max 32.51 _reflns_number_total 10484 _reflns_number_gt 9658 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement 'HKL DENZO' _computing_data_reduction 'HKL DENZO and SCALEPACK' _computing_structure_solution SHELXS-97 _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^ > 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^)+(0.0656P)^2^+23.2445P] 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 10484 _refine_ls_number_parameters 418 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0553 _refine_ls_R_factor_gt 0.0505 _refine_ls_wR_factor_ref 0.1281 _refine_ls_wR_factor_gt 0.1240 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _refine_ls_shift/su_max 0.022 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt Pt 0.49309(2) 0.237530(12) 0.032574(11) 0.00550(6) Uani 1 1 d . . . Fe2 Fe 0.0000 0.5000 0.0000 0.00436(16) Uani 1 2 d S . . Fe1 Fe 0.0000 0.0000 0.0000 0.00428(16) Uani 1 2 d S . . N1 N 0.0223(6) 0.0943(4) -0.1184(3) 0.0133(8) Uani 1 1 d . . . N2 N 0.1813(6) 0.0837(3) 0.0281(3) 0.0098(7) Uani 1 1 d . . . N3 N 0.8116(6) 0.3952(3) 0.0199(3) 0.0101(8) Uani 1 1 d . . . N4 N 0.1934(6) 0.4030(3) 0.0081(3) 0.0126(8) Uani 1 1 d . . . N5 N -0.0075(7) 0.4804(4) 0.1259(3) 0.0182(9) Uani 1 1 d . . . N6 N 0.7990(6) 0.0794(3) 0.0317(3) 0.0100(7) Uani 1 1 d . . . C1 C 0.0450(8) 0.0605(4) -0.1876(4) 0.0164(10) Uani 1 1 d . . . H1 H 0.0544 -0.0079 -0.1794 0.020 Uiso 1 1 calc R . . C2 C 0.0552(9) 0.1229(5) -0.2708(4) 0.0204(11) Uani 1 1 d . . . H2 H 0.0738 0.0968 -0.3173 0.024 Uiso 1 1 calc R . . C3 C 0.0369(10) 0.2257(5) -0.2836(4) 0.0219(12) Uani 1 1 d . . . C4 C 0.0172(10) 0.2622(5) -0.2129(4) 0.0244(13) Uani 1 1 d . . . H4 H 0.0081 0.3304 -0.2199 0.029 Uiso 1 1 calc R . . C5 C 0.0114(9) 0.1957(4) -0.1315(4) 0.0179(11) Uani 1 1 d . . . H5 H -0.0003 0.2206 -0.0842 0.022 Uiso 1 1 calc R . . C6 C 0.0334(10) 0.2899(6) -0.3693(5) 0.0274(14) Uani 1 1 d . . . C7 C 0.0239(11) 0.3361(6) -0.4430(5) 0.0285(14) Uani 1 1 d . . . C8 C 0.2953(7) 0.1390(4) 0.0334(3) 0.0095(8) Uani 1 1 d . . . C9 C 0.6939(7) 0.3368(4) 0.0266(3) 0.0103(8) Uani 1 1 d . . . C10 C 0.3041(7) 0.3427(4) 0.0183(4) 0.0111(9) Uani 1 1 d . . . C11 C 0.6842(7) 0.1348(4) 0.0376(4) 0.0112(9) Uani 1 1 d . . . C12 C 0.1507(10) 0.4846(5) 0.1623(4) 0.0224(12) Uani 1 1 d . . . H12 H 0.2618 0.5011 0.1265 0.027 Uiso 1 1 calc R . . C13 C 0.1564(11) 0.4658(5) 0.2498(5) 0.0268(14) Uani 1 1 d . . . H13 H 0.2678 0.4718 0.2716 0.032 Uiso 1 1 calc R . . C14 C -0.0079(11) 0.4377(5) 0.3044(5) 0.0261(13) Uani 1 1 d . . . C15 C -0.1727(11) 0.4332(5) 0.2686(5) 0.0264(13) Uani 1 1 d . . . H15 H -0.2848 0.4155 0.3035 0.032 Uiso 1 1 calc R . . C16 C -0.1670(9) 0.4554(5) 0.1796(4) 0.0209(11) Uani 1 1 d . . . H16 H -0.2776 0.4531 0.1562 0.025 Uiso 1 1 calc R . . C17 C -0.0036(12) 0.4101(6) 0.3962(5) 0.0309(15) Uani 1 1 d . . . C18 C 0.0111(12) 0.3792(6) 0.4714(5) 0.0287(14) Uani 1 1 d . . . C19 C 0.0315(11) 0.1485(6) 0.3844(5) 0.0296(15) Uani 1 1 d . . . C20 C 0.0879(13) 0.1290(6) 0.4681(5) 0.0344(17) Uani 1 1 d . . . H20 H 0.0059 0.0955 0.5154 0.041 Uiso 1 1 calc R . . C21 C 0.2595(13) 0.1585(7) 0.4801(5) 0.0383(18) Uani 1 1 d . . . H21 H 0.2937 0.1444 0.5353 0.046 Uiso 1 1 calc R . . C22 C 0.3849(12) 0.2099(6) 0.4100(6) 0.0343(16) Uani 1 1 d . . . H22 H 0.5012 0.2304 0.4190 0.041 Uiso 1 1 calc R . . C23 C 0.3378(12) 0.2303(6) 0.3284(6) 0.0351(17) Uani 1 1 d . . . H23 H 0.4228 0.2639 0.2824 0.042 Uiso 1 1 calc R . . C24 C 0.1613(10) 0.2007(5) 0.3135(5) 0.0258(13) Uani 1 1 d . . . C25 C 0.1066(14) 0.2202(6) 0.2298(5) 0.0364(18) Uani 1 1 d . . . H25 H 0.1891 0.2541 0.1828 0.044 Uiso 1 1 calc R . . C26 C -0.0631(13) 0.1904(6) 0.2168(5) 0.0338(17) Uani 1 1 d . . . H26 H -0.0950 0.2036 0.1613 0.041 Uiso 1 1 calc R . . C27 C -0.1920(13) 0.1393(7) 0.2871(7) 0.041(2) Uani 1 1 d . . . H27 H -0.3082 0.1190 0.2779 0.049 Uiso 1 1 calc R . . C28 C -0.1446(12) 0.1201(7) 0.3689(6) 0.0355(17) Uani 1 1 d . . . H28 H -0.2306 0.0877 0.4150 0.043 Uiso 1 1 calc R . . C29 C 0.5724(9) 0.2129(5) 0.6627(4) 0.0234(12) Uani 1 1 d . . . C30 C 0.6197(12) 0.1416(6) 0.6177(5) 0.0323(16) Uani 1 1 d . . . H30 H 0.6383 0.1622 0.5581 0.039 Uiso 1 1 calc R . . C31 C 0.6386(12) 0.0432(7) 0.6600(6) 0.0360(17) Uani 1 1 d . . . H31 H 0.6725 -0.0020 0.6293 0.043 Uiso 1 1 calc R . . C32 C 0.6062(12) 0.0101(6) 0.7508(6) 0.0361(17) Uani 1 1 d . . . H32 H 0.6169 -0.0570 0.7794 0.043 Uiso 1 1 calc R . . C33 C 0.5590(10) 0.0771(6) 0.7968(5) 0.0278(14) Uani 1 1 d . . . H33 H 0.5375 0.0546 0.8563 0.033 Uiso 1 1 calc R . . C34 C 0.5430(10) 0.1798(6) 0.7542(5) 0.0255(13) Uani 1 1 d . . . C35 C 0.4949(12) 0.2503(7) 0.7996(6) 0.0373(18) Uani 1 1 d . . . H35 H 0.4751 0.2297 0.8592 0.045 Uiso 1 1 calc R . . C36 C 0.4772(13) 0.3492(8) 0.7563(7) 0.044(2) Uani 1 1 d . . . H36 H 0.4483 0.3953 0.7867 0.053 Uiso 1 1 calc R . . C37 C 0.5027(13) 0.3811(7) 0.6654(7) 0.042(2) Uani 1 1 d . . . H37 H 0.4852 0.4476 0.6367 0.050 Uiso 1 1 calc R . . C38 C 0.5525(13) 0.3159(6) 0.6196(6) 0.0374(18) Uani 1 1 d . . . H38 H 0.5736 0.3385 0.5602 0.045 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 Pt 0.00319(8) 0.00362(8) 0.01013(9) -0.00234(6) -0.00156(5) 0.00053(5) Fe2 0.0027(4) 0.0024(4) 0.0082(4) -0.0014(3) -0.0017(3) 0.0008(3) Fe1 0.0029(4) 0.0024(4) 0.0078(4) -0.0015(3) -0.0017(3) 0.0005(3) N1 0.0096(18) 0.017(2) 0.010(2) 0.0015(16) -0.0015(15) -0.0001(16) N2 0.0094(18) 0.0061(17) 0.015(2) -0.0048(15) -0.0021(15) 0.0008(14) N3 0.0059(17) 0.0073(17) 0.017(2) -0.0031(15) -0.0027(15) 0.0011(14) N4 0.0098(18) 0.0069(18) 0.023(2) -0.0061(16) -0.0066(16) 0.0023(14) N5 0.020(2) 0.022(2) 0.013(2) -0.0059(18) 0.0002(18) 0.0003(19) N6 0.0071(17) 0.0099(18) 0.015(2) -0.0075(15) -0.0016(15) 0.0016(14) C1 0.018(2) 0.010(2) 0.021(3) -0.0047(19) 0.000(2) 0.0016(18) C2 0.025(3) 0.021(3) 0.015(3) -0.003(2) -0.002(2) 0.002(2) C3 0.026(3) 0.021(3) 0.016(3) -0.001(2) -0.003(2) 0.001(2) C4 0.033(3) 0.017(3) 0.020(3) 0.000(2) -0.004(3) 0.002(2) C5 0.023(3) 0.013(2) 0.017(3) -0.004(2) -0.005(2) 0.003(2) C6 0.028(3) 0.027(3) 0.026(3) -0.004(3) -0.005(3) 0.001(3) C7 0.034(4) 0.026(3) 0.024(3) -0.005(3) -0.004(3) 0.004(3) C8 0.0072(19) 0.009(2) 0.013(2) -0.0041(17) -0.0025(16) 0.0019(15) C9 0.0058(19) 0.011(2) 0.015(2) -0.0037(17) -0.0028(16) 0.0013(16) C10 0.0075(19) 0.0050(19) 0.022(3) -0.0043(17) -0.0058(18) 0.0015(15) C11 0.0061(19) 0.010(2) 0.020(2) -0.0079(18) -0.0011(17) -0.0018(16) C12 0.026(3) 0.022(3) 0.019(3) -0.005(2) -0.006(2) 0.002(2) C13 0.037(4) 0.021(3) 0.022(3) -0.003(2) -0.013(3) 0.001(3) C14 0.038(4) 0.016(3) 0.024(3) -0.005(2) -0.009(3) 0.007(3) C15 0.030(3) 0.024(3) 0.023(3) -0.004(2) 0.001(3) 0.006(3) C16 0.020(3) 0.024(3) 0.017(3) -0.004(2) -0.001(2) 0.001(2) C17 0.042(4) 0.025(3) 0.026(3) -0.007(3) -0.007(3) 0.003(3) C18 0.040(4) 0.024(3) 0.022(3) -0.004(2) -0.005(3) 0.003(3) C19 0.035(4) 0.025(3) 0.026(3) -0.004(3) -0.002(3) 0.012(3) C20 0.043(4) 0.036(4) 0.021(3) -0.004(3) 0.001(3) 0.011(3) C21 0.044(5) 0.047(5) 0.027(4) -0.012(3) -0.010(3) 0.013(4) C22 0.031(4) 0.031(4) 0.041(4) -0.008(3) -0.009(3) 0.003(3) C23 0.030(4) 0.033(4) 0.040(4) -0.008(3) 0.002(3) 0.003(3) C24 0.032(3) 0.019(3) 0.025(3) -0.004(2) -0.002(3) 0.009(2) C25 0.054(5) 0.023(3) 0.031(4) -0.008(3) -0.001(3) 0.012(3) C26 0.050(5) 0.028(4) 0.028(4) -0.011(3) -0.016(3) 0.011(3) C27 0.039(4) 0.040(5) 0.053(5) -0.020(4) -0.022(4) 0.012(4) C28 0.037(4) 0.034(4) 0.035(4) -0.008(3) -0.004(3) 0.006(3) C29 0.021(3) 0.028(3) 0.022(3) -0.008(2) -0.002(2) 0.002(2) C30 0.041(4) 0.034(4) 0.024(3) -0.011(3) -0.007(3) 0.003(3) C31 0.037(4) 0.037(4) 0.038(4) -0.016(3) -0.009(3) 0.007(3) C32 0.039(4) 0.031(4) 0.037(4) -0.005(3) -0.012(3) 0.002(3) C33 0.023(3) 0.030(3) 0.025(3) 0.001(3) -0.003(2) -0.002(3) C34 0.020(3) 0.028(3) 0.026(3) -0.005(3) -0.003(2) 0.000(2) C35 0.033(4) 0.052(5) 0.030(4) -0.017(4) -0.002(3) 0.004(4) C36 0.038(5) 0.050(5) 0.049(5) -0.025(4) 0.001(4) 0.002(4) C37 0.040(5) 0.035(4) 0.051(5) -0.010(4) -0.011(4) 0.006(4) C38 0.046(5) 0.026(4) 0.034(4) 0.001(3) -0.005(4) -0.001(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N1 2.001(5) . ? Fe1 N1 2.001(5) 2 ? Fe1 N2 1.934(4) 2 ? Fe1 N2 1.934(4) . ? Fe1 N6 1.944(4) 2_655 ? Fe1 N6 1.944(4) 1_455 ? Fe2 N3 1.935(4) 1_455 ? Fe2 N3 1.935(4) 2_665 ? Fe2 N4 1.938(4) . ? Fe2 N4 1.938(4) 2_565 ? Fe2 N5 1.996(5) 2_565 ? Fe2 N5 1.996(5) . ? Pt C8 1.984(5) . ? Pt C9 1.985(5) . ? Pt C10 1.990(5) . ? Pt C11 1.986(5) . ? N1 C1 1.340(8) . ? N1 C5 1.374(7) . ? N2 C8 1.158(7) . ? N3 C9 1.155(7) . ? N3 Fe2 1.935(4) 1_655 ? N4 C10 1.155(7) . ? N5 C16 1.354(8) . ? N5 C12 1.358(8) . ? N6 C11 1.151(7) . ? N6 Fe1 1.944(4) 1_655 ? C1 C2 1.389(8) . ? C2 C3 1.400(9) . ? C3 C4 1.386(10) . ? C3 C6 1.439(9) . ? C4 C5 1.389(9) . ? C6 C7 1.206(10) . ? C7 C18 1.373(10) 1_554 ? C12 C13 1.388(9) . ? C13 C14 1.392(11) . ? C14 C15 1.396(11) . ? C14 C17 1.447(10) . ? C15 C16 1.397(9) . ? C17 C18 1.201(10) . ? C18 C7 1.373(10) 1_556 ? C19 C28 1.406(12) . ? C19 C20 1.426(11) . ? C19 C24 1.430(11) . ? C20 C21 1.361(13) . ? C21 C22 1.402(13) . ? C22 C23 1.367(12) . ? C23 C24 1.412(12) . ? C24 C25 1.421(11) . ? C25 C26 1.355(13) . ? C26 C27 1.417(14) . ? C27 C28 1.372(13) . ? C29 C30 1.419(10) . ? C29 C34 1.430(10) . ? C29 C38 1.427(11) . ? C30 C31 1.366(12) . ? C31 C32 1.419(13) . ? C32 C33 1.380(12) . ? C33 C34 1.418(10) . ? C34 C35 1.415(11) . ? C35 C36 1.376(14) . ? C36 C37 1.418(14) . ? C37 C38 1.360(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Fe1 N1 180.0(3) . 2 ? N2 Fe1 N1 88.24(19) . . ? N2 Fe1 N1 91.76(19) 2 . ? N2 Fe1 N1 88.24(19) 2 2 ? N2 Fe1 N1 91.76(19) . 2 ? N6 Fe1 N1 91.8(2) 2_655 . ? N6 Fe1 N1 88.2(2) 1_455 . ? N6 Fe1 N1 88.2(2) 2_655 2 ? N6 Fe1 N1 91.8(2) 1_455 2 ? N2 Fe1 N2 180.0(3) 2 . ? N2 Fe1 N6 90.93(18) 2 2_655 ? N2 Fe1 N6 89.07(18) . 2_655 ? N2 Fe1 N6 89.07(18) 2 1_455 ? N2 Fe1 N6 90.93(18) . 1_455 ? N6 Fe1 N6 180.0(3) 2_655 1_455 ? N3 Fe2 N3 180.00(19) 1_455 2_665 ? N3 Fe2 N4 90.54(18) 1_455 . ? N3 Fe2 N4 89.46(18) 2_665 . ? N3 Fe2 N4 89.46(18) 1_455 2_565 ? N3 Fe2 N4 90.54(18) 2_665 2_565 ? N4 Fe2 N4 180.000(1) . 2_565 ? N3 Fe2 N5 89.3(2) 1_455 2_565 ? N3 Fe2 N5 90.7(2) 2_665 2_565 ? N4 Fe2 N5 91.2(2) . 2_565 ? N4 Fe2 N5 88.8(2) 2_565 2_565 ? N3 Fe2 N5 90.7(2) 1_455 . ? N3 Fe2 N5 89.3(2) 2_665 . ? N4 Fe2 N5 88.8(2) . . ? N4 Fe2 N5 91.2(2) 2_565 . ? N5 Fe2 N5 180.000(1) 2_565 . ? C8 Pt C9 177.6(2) . . ? C8 Pt C11 90.8(2) . . ? C9 Pt C11 88.8(2) . . ? C8 Pt C10 89.0(2) . . ? C9 Pt C10 91.2(2) . . ? C11 Pt C10 175.8(2) . . ? C1 N1 C5 117.8(5) . . ? C1 N1 Fe1 121.0(4) . . ? C5 N1 Fe1 121.2(4) . . ? C8 N2 Fe1 171.0(4) . . ? C9 N3 Fe2 175.0(5) . 1_655 ? C10 N4 Fe2 175.6(5) . . ? C16 N5 C12 116.8(6) . . ? C16 N5 Fe2 122.0(4) . . ? C12 N5 Fe2 121.0(4) . . ? C11 N6 Fe1 169.6(5) . 1_655 ? N1 C1 C2 123.0(5) . . ? C1 C2 C3 118.9(6) . . ? C4 C3 C2 118.8(6) . . ? C4 C3 C6 121.9(6) . . ? C2 C3 C6 119.2(6) . . ? C3 C4 C5 119.2(6) . . ? N1 C5 C4 122.2(6) . . ? C7 C6 C3 173.8(8) . . ? C6 C7 C18 174.0(8) . 1_554 ? N2 C8 Pt 175.5(5) . . ? N3 C9 Pt 177.6(5) . . ? N4 C10 Pt 178.1(5) . . ? N6 C11 Pt 173.1(5) . . ? N5 C12 C13 123.9(7) . . ? C14 C13 C12 118.6(7) . . ? C13 C14 C15 118.6(7) . . ? C13 C14 C17 119.7(7) . . ? C15 C14 C17 121.6(7) . . ? C14 C15 C16 119.2(7) . . ? N5 C16 C15 122.9(6) . . ? C18 C17 C14 173.2(8) . . ? C17 C18 C7 175.3(9) . 1_556 ? C28 C19 C20 123.3(8) . . ? C28 C19 C24 119.1(7) . . ? C20 C19 C24 117.6(8) . . ? C21 C20 C19 121.3(8) . . ? C20 C21 C22 120.5(8) . . ? C23 C22 C21 120.5(8) . . ? C22 C23 C24 120.5(8) . . ? C23 C24 C25 122.4(8) . . ? C23 C24 C19 119.6(7) . . ? C25 C24 C19 118.0(7) . . ? C26 C25 C24 121.5(8) . . ? C25 C26 C27 120.5(8) . . ? C28 C27 C26 119.6(8) . . ? C27 C28 C19 121.2(9) . . ? C30 C29 C34 118.5(7) . . ? C30 C29 C38 122.2(7) . . ? C34 C29 C38 119.2(7) . . ? C31 C30 C29 121.5(7) . . ? C30 C31 C32 119.9(8) . . ? C33 C32 C31 120.4(8) . . ? C32 C33 C34 120.5(7) . . ? C33 C34 C35 121.9(7) . . ? C33 C34 C29 119.1(7) . . ? C35 C34 C29 118.9(7) . . ? C36 C35 C34 120.5(8) . . ? C35 C36 C37 120.2(9) . . ? C38 C37 C36 121.0(9) . . ? C37 C38 C29 120.1(8) . . ? _diffrn_measured_fraction_theta_max 0.918 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.241 _refine_diff_density_min -2.266 _refine_diff_density_rms 0.314 _database_code_depnum_ccdc_archive 'CCDC 971021' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_shelxl _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H24 Fe N6 Pt' _chemical_formula_weight 815.57 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 '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 7.3635(2) _cell_length_b 14.1112(4) _cell_length_c 16.3906(5) _cell_angle_alpha 74.663(3) _cell_angle_beta 82.349(2) _cell_angle_gamma 89.878(2) _cell_volume 1626.86(8) _cell_formula_units_Z 2 _cell_measurement_temperature 195(1) _cell_measurement_reflns_used 100 _cell_measurement_theta_min 12 _cell_measurement_theta_max 25 _exptl_crystal_description prismatic _exptl_crystal_colour red _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.665 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 796 _exptl_absorpt_coefficient_mu 4.777 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5979 _exptl_absorpt_correction_T_max 0.7011 _exptl_absorpt_process_details 'Empirical absorption correction:XABS2' _exptl_special_details ; ? ; _diffrn_ambient_temperature 195(1) _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31373 _diffrn_reflns_av_R_equivalents 0.0342 _diffrn_reflns_av_sigmaI/netI 0.0412 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 32.64 _reflns_number_total 10926 _reflns_number_gt 9980 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement 'HKL DENZO' _computing_data_reduction 'HKL DENZO and SCALEPACK' _computing_structure_solution SHELXS-97 _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^ > 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^)+(0.0273P)^2^+1.3390P] 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 10926 _refine_ls_number_parameters 418 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0289 _refine_ls_R_factor_gt 0.0239 _refine_ls_wR_factor_ref 0.0550 _refine_ls_wR_factor_gt 0.0519 _refine_ls_goodness_of_fit_ref 0.902 _refine_ls_restrained_S_all 0.902 _refine_ls_shift/su_max 0.035 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt Pt 0.491722(10) 0.228367(6) 0.034498(5) 0.01073(3) Uani 1 1 d . . . Fe2 Fe 0.0000 0.5000 0.0000 0.01096(8) Uani 1 2 d S . . Fe1 Fe 0.0000 0.0000 0.0000 0.00939(8) Uani 1 2 d S . . N1 N 0.0213(3) 0.09424(14) -0.11615(12) 0.0137(3) Uani 1 1 d . . . N2 N 0.1789(3) 0.08126(14) 0.02915(12) 0.0137(3) Uani 1 1 d . . . N3 N 0.7992(3) 0.38447(15) 0.02452(14) 0.0197(4) Uani 1 1 d . . . N4 N 0.2108(3) 0.39621(15) 0.00416(14) 0.0206(4) Uani 1 1 d . . . N5 N -0.0054(3) 0.48017(16) 0.13980(13) 0.0215(4) Uani 1 1 d . . . N6 N 0.7986(3) 0.07500(14) 0.03587(12) 0.0137(3) Uani 1 1 d . . . C1 C 0.0421(4) 0.06127(19) -0.18635(16) 0.0210(5) Uani 1 1 d . . . H1 H 0.0528 -0.0059 -0.1798 0.025 Uiso 1 1 calc R . . C2 C 0.0485(4) 0.1221(2) -0.26765(17) 0.0283(6) Uani 1 1 d . . . H2 H 0.0638 0.0961 -0.3146 0.034 Uiso 1 1 calc R . . C3 C 0.0318(4) 0.2225(2) -0.27904(16) 0.0255(5) Uani 1 1 d . . . C4 C 0.0141(4) 0.2568(2) -0.20700(17) 0.0253(5) Uani 1 1 d . . . H4 H 0.0051 0.3238 -0.2122 0.030 Uiso 1 1 calc R . . C5 C 0.0097(3) 0.19184(18) -0.12746(15) 0.0189(4) Uani 1 1 d . . . H5 H -0.0018 0.2164 -0.0798 0.023 Uiso 1 1 calc R . . C6 C 0.0288(4) 0.2863(2) -0.36299(18) 0.0318(6) Uani 1 1 d . . . C7 C 0.0210(5) 0.3319(2) -0.43472(19) 0.0361(7) Uani 1 1 d . . . C8 C 0.2942(3) 0.13261(16) 0.03515(14) 0.0141(4) Uani 1 1 d . . . C9 C 0.6861(3) 0.32595(17) 0.02987(15) 0.0153(4) Uani 1 1 d . . . C10 C 0.3132(3) 0.33441(16) 0.01620(15) 0.0149(4) Uani 1 1 d . . . C11 C 0.6802(3) 0.12674(16) 0.04247(14) 0.0129(4) Uani 1 1 d . . . C12 C 0.1454(4) 0.4927(2) 0.17307(18) 0.0307(6) Uani 1 1 d . . . H12 H 0.2523 0.5160 0.1360 0.037 Uiso 1 1 calc R . . C13 C 0.1512(5) 0.4729(2) 0.25948(19) 0.0394(8) Uani 1 1 d . . . H13 H 0.2594 0.4835 0.2797 0.047 Uiso 1 1 calc R . . C14 C -0.0060(5) 0.4371(2) 0.31613(18) 0.0340(7) Uani 1 1 d . . . C15 C -0.1638(5) 0.4248(3) 0.28215(19) 0.0377(7) Uani 1 1 d . . . H15 H -0.2726 0.4017 0.3178 0.045 Uiso 1 1 calc R . . C16 C -0.1572(4) 0.4474(2) 0.19444(18) 0.0315(6) Uani 1 1 d . . . H16 H -0.2643 0.4393 0.1723 0.038 Uiso 1 1 calc R . . C17 C -0.0016(6) 0.4086(2) 0.40690(19) 0.0408(8) Uani 1 1 d . . . C18 C 0.0084(5) 0.3769(2) 0.48072(19) 0.0385(7) Uani 1 1 d . . . C19 C 0.0318(5) 0.1487(3) 0.3843(2) 0.0419(8) Uani 1 1 d . . . C20 C 0.0858(6) 0.1289(3) 0.4668(2) 0.0530(10) Uani 1 1 d . . . H20 H 0.0051 0.0950 0.5141 0.064 Uiso 1 1 calc R . . C21 C 0.2531(6) 0.1586(4) 0.4776(3) 0.0627(12) Uani 1 1 d . . . H21 H 0.2869 0.1451 0.5321 0.075 Uiso 1 1 calc R . . C22 C 0.3747(7) 0.2091(4) 0.4076(3) 0.0630(12) Uani 1 1 d . . . H22 H 0.4893 0.2292 0.4161 0.076 Uiso 1 1 calc R . . C23 C 0.3314(6) 0.2298(3) 0.3278(3) 0.0608(11) Uani 1 1 d . . . H23 H 0.4161 0.2635 0.2821 0.073 Uiso 1 1 calc R . . C24 C 0.1550(5) 0.2001(3) 0.3128(2) 0.0433(8) Uani 1 1 d . . . C25 C 0.1039(7) 0.2197(3) 0.2316(2) 0.0606(12) Uani 1 1 d . . . H25 H 0.1849 0.2541 0.1846 0.073 Uiso 1 1 calc R . . C26 C -0.0606(8) 0.1897(3) 0.2205(3) 0.0651(13) Uani 1 1 d . . . H26 H -0.0921 0.2035 0.1655 0.078 Uiso 1 1 calc R . . C27 C -0.1870(7) 0.1377(4) 0.2895(4) 0.0679(14) Uani 1 1 d . . . H27 H -0.3004 0.1171 0.2802 0.082 Uiso 1 1 calc R . . C28 C -0.1423(6) 0.1173(3) 0.3716(3) 0.0565(10) Uani 1 1 d . . . H28 H -0.2255 0.0834 0.4178 0.068 Uiso 1 1 calc R . . C29 C 0.5634(5) 0.2118(3) 0.6619(2) 0.0394(7) Uani 1 1 d . . . C30 C 0.6138(6) 0.1404(3) 0.6189(2) 0.0507(9) Uani 1 1 d . . . H30 H 0.6349 0.1585 0.5595 0.061 Uiso 1 1 calc R . . C31 C 0.6326(6) 0.0457(3) 0.6618(3) 0.0563(10) Uani 1 1 d . . . H31 H 0.6649 -0.0007 0.6318 0.068 Uiso 1 1 calc R . . C32 C 0.6035(5) 0.0171(3) 0.7511(3) 0.0538(10) Uani 1 1 d . . . H32 H 0.6155 -0.0484 0.7801 0.065 Uiso 1 1 calc R . . C33 C 0.5581(5) 0.0837(3) 0.7957(2) 0.0477(9) Uani 1 1 d . . . H33 H 0.5408 0.0639 0.8551 0.057 Uiso 1 1 calc R . . C34 C 0.5366(4) 0.1831(3) 0.7529(2) 0.0385(7) Uani 1 1 d . . . C35 C 0.4906(5) 0.2537(3) 0.7971(3) 0.0514(10) Uani 1 1 d . . . H35 H 0.4749 0.2355 0.8565 0.062 Uiso 1 1 calc R . . C36 C 0.4685(6) 0.3485(4) 0.7546(3) 0.0634(12) Uani 1 1 d . . . H36 H 0.4377 0.3945 0.7851 0.076 Uiso 1 1 calc R . . C37 C 0.4916(6) 0.3776(3) 0.6657(3) 0.0641(12) Uani 1 1 d . . . H37 H 0.4747 0.4428 0.6373 0.077 Uiso 1 1 calc R . . C38 C 0.5387(6) 0.3112(3) 0.6201(3) 0.0551(10) Uani 1 1 d . . . H38 H 0.5548 0.3316 0.5608 0.066 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 Pt 0.00770(4) 0.00815(4) 0.01726(4) -0.00433(3) -0.00309(3) 0.00101(3) Fe2 0.00943(18) 0.00759(18) 0.0164(2) -0.00299(15) -0.00424(15) 0.00102(15) Fe1 0.00740(17) 0.00741(18) 0.01378(19) -0.00284(15) -0.00294(14) 0.00093(14) N1 0.0135(8) 0.0121(9) 0.0155(9) -0.0035(7) -0.0022(7) -0.0006(7) N2 0.0117(8) 0.0102(8) 0.0197(9) -0.0041(7) -0.0039(7) 0.0010(7) N3 0.0163(9) 0.0162(10) 0.0272(11) -0.0050(8) -0.0067(8) -0.0009(8) N4 0.0180(10) 0.0151(9) 0.0294(11) -0.0061(8) -0.0052(8) 0.0038(8) N5 0.0271(11) 0.0195(10) 0.0182(10) -0.0046(8) -0.0059(8) 0.0020(9) N6 0.0125(8) 0.0115(8) 0.0183(9) -0.0043(7) -0.0050(7) 0.0016(7) C1 0.0264(12) 0.0176(11) 0.0201(11) -0.0060(9) -0.0048(9) 0.0040(10) C2 0.0371(15) 0.0311(15) 0.0162(12) -0.0053(10) -0.0043(10) 0.0020(12) C3 0.0260(13) 0.0290(14) 0.0175(11) 0.0018(10) -0.0054(9) -0.0014(11) C4 0.0316(14) 0.0179(12) 0.0237(12) 0.0001(10) -0.0058(10) 0.0015(10) C5 0.0230(12) 0.0136(10) 0.0199(11) -0.0032(8) -0.0047(9) 0.0010(9) C6 0.0397(16) 0.0307(15) 0.0216(13) -0.0002(11) -0.0059(11) -0.0010(13) C7 0.0473(19) 0.0329(16) 0.0239(14) 0.0011(12) -0.0079(12) 0.0027(14) C8 0.0122(9) 0.0117(10) 0.0189(10) -0.0046(8) -0.0033(8) 0.0024(8) C9 0.0136(10) 0.0131(10) 0.0204(11) -0.0053(8) -0.0050(8) 0.0029(8) C10 0.0119(9) 0.0119(10) 0.0222(11) -0.0059(8) -0.0035(8) 0.0002(8) C11 0.0127(9) 0.0101(9) 0.0156(10) -0.0029(7) -0.0020(7) -0.0009(7) C12 0.0341(15) 0.0326(15) 0.0240(13) -0.0014(11) -0.0116(11) -0.0067(12) C13 0.055(2) 0.0359(17) 0.0277(15) -0.0017(12) -0.0216(14) -0.0056(15) C14 0.057(2) 0.0235(14) 0.0210(13) -0.0023(11) -0.0101(13) 0.0071(13) C15 0.0421(18) 0.0460(19) 0.0215(14) -0.0058(13) 0.0018(12) 0.0050(15) C16 0.0289(14) 0.0421(17) 0.0235(13) -0.0084(12) -0.0042(11) 0.0038(13) C17 0.070(2) 0.0281(16) 0.0242(14) -0.0042(12) -0.0112(14) 0.0075(16) C18 0.058(2) 0.0308(16) 0.0258(14) -0.0031(12) -0.0126(14) 0.0036(15) C19 0.053(2) 0.0375(18) 0.0349(17) -0.0109(14) -0.0029(15) 0.0150(16) C20 0.065(3) 0.050(2) 0.0373(19) -0.0047(16) 0.0011(17) 0.010(2) C21 0.062(3) 0.072(3) 0.058(3) -0.021(2) -0.015(2) 0.013(2) C22 0.055(3) 0.063(3) 0.075(3) -0.020(2) -0.016(2) 0.006(2) C23 0.061(3) 0.050(2) 0.063(3) -0.007(2) 0.008(2) 0.004(2) C24 0.058(2) 0.0295(16) 0.0391(18) -0.0067(13) 0.0013(15) 0.0152(16) C25 0.100(4) 0.046(2) 0.0342(19) -0.0088(16) -0.005(2) 0.028(2) C26 0.106(4) 0.049(3) 0.054(3) -0.027(2) -0.033(3) 0.029(3) C27 0.066(3) 0.057(3) 0.103(4) -0.047(3) -0.039(3) 0.020(2) C28 0.053(2) 0.051(2) 0.066(3) -0.020(2) -0.004(2) 0.007(2) C29 0.0334(16) 0.0440(19) 0.0403(18) -0.0085(15) -0.0081(13) -0.0034(14) C30 0.054(2) 0.061(3) 0.0394(19) -0.0146(18) -0.0126(16) 0.005(2) C31 0.059(3) 0.057(3) 0.058(2) -0.021(2) -0.014(2) 0.005(2) C32 0.047(2) 0.047(2) 0.061(2) -0.0001(19) -0.0146(18) 0.0000(18) C33 0.0374(18) 0.056(2) 0.0393(18) 0.0056(17) -0.0062(14) -0.0093(17) C34 0.0234(14) 0.056(2) 0.0357(16) -0.0113(15) -0.0040(12) -0.0058(14) C35 0.0376(19) 0.073(3) 0.048(2) -0.025(2) 0.0006(16) -0.0037(19) C36 0.050(2) 0.067(3) 0.084(3) -0.039(3) -0.009(2) 0.002(2) C37 0.056(3) 0.045(2) 0.095(4) -0.023(2) -0.013(2) 0.004(2) C38 0.052(2) 0.056(3) 0.052(2) -0.0031(19) -0.0100(18) 0.002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N1 1.9998(19) 2 ? Fe1 N1 1.9998(19) . ? Fe1 N2 1.9346(19) . ? Fe1 N2 1.9346(19) 2 ? Fe1 N6 1.9378(18) 1_455 ? Fe1 N6 1.9378(18) 2_655 ? Fe2 N3 2.124(2) 2_665 ? Fe2 N3 2.124(2) 1_455 ? Fe2 N4 2.127(2) 2_565 ? Fe2 N4 2.127(2) . ? Fe2 N5 2.229(2) . ? Fe2 N5 2.229(2) 2_565 ? Pt C8 1.985(2) . ? Pt C9 1.968(2) . ? Pt C10 1.979(2) . ? Pt C11 1.985(2) . ? N1 C1 1.342(3) . ? N1 C5 1.344(3) . ? N2 C8 1.148(3) . ? N3 C9 1.153(3) . ? N3 Fe2 2.124(2) 1_655 ? N4 C10 1.146(3) . ? N5 C16 1.335(4) . ? N5 C12 1.332(3) . ? N6 C11 1.149(3) . ? N6 Fe1 1.9378(18) 1_655 ? C1 C2 1.376(4) . ? C2 C3 1.386(4) . ? C3 C4 1.381(4) . ? C3 C6 1.435(4) . ? C4 C5 1.378(3) . ? C6 C7 1.190(4) . ? C7 C18 1.379(4) 1_554 ? C12 C13 1.376(4) . ? C13 C14 1.388(5) . ? C14 C15 1.384(5) . ? C14 C17 1.440(4) . ? C15 C16 1.382(4) . ? C17 C18 1.186(4) . ? C18 C7 1.379(4) 1_556 ? C19 C24 1.412(5) . ? C19 C28 1.417(6) . ? C19 C20 1.417(5) . ? C20 C21 1.350(6) . ? C21 C22 1.387(6) . ? C22 C23 1.343(6) . ? C23 C24 1.438(6) . ? C24 C25 1.388(5) . ? C25 C26 1.335(7) . ? C26 C27 1.403(7) . ? C27 C28 1.382(6) . ? C29 C30 1.398(5) . ? C29 C34 1.424(5) . ? C29 C38 1.412(5) . ? C30 C31 1.353(6) . ? C31 C32 1.399(6) . ? C32 C33 1.352(6) . ? C33 C34 1.412(5) . ? C34 C35 1.395(5) . ? C35 C36 1.355(6) . ? C36 C37 1.392(7) . ? C37 C38 1.363(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Fe1 N1 180.00(19) 2 . ? N2 Fe1 N1 91.38(8) . 2 ? N2 Fe1 N1 88.62(8) 2 2 ? N6 Fe1 N1 91.67(8) 1_455 2 ? N6 Fe1 N1 88.33(8) 2_655 2 ? N2 Fe1 N1 88.62(8) . . ? N2 Fe1 N1 91.38(8) 2 . ? N6 Fe1 N1 88.33(8) 1_455 . ? N6 Fe1 N1 91.67(8) 2_655 . ? N2 Fe1 N2 180.00(11) . 2 ? N2 Fe1 N6 92.13(8) . 1_455 ? N2 Fe1 N6 87.87(8) 2 1_455 ? N2 Fe1 N6 87.87(8) . 2_655 ? N2 Fe1 N6 92.13(8) 2 2_655 ? N6 Fe1 N6 180.00(9) 1_455 2_655 ? N4 Fe2 N4 180.0 2_565 . ? N4 Fe2 N3 89.95(8) 2_565 2_665 ? N4 Fe2 N3 90.05(8) . 2_665 ? N4 Fe2 N3 90.05(8) 2_565 1_455 ? N4 Fe2 N3 89.95(8) . 1_455 ? N3 Fe2 N3 180.0 2_665 1_455 ? N4 Fe2 N5 91.01(8) 2_565 . ? N4 Fe2 N5 88.99(8) . . ? N3 Fe2 N5 89.60(8) 2_665 . ? N3 Fe2 N5 90.41(8) 1_455 . ? N4 Fe2 N5 88.99(8) 2_565 2_565 ? N4 Fe2 N5 91.01(8) . 2_565 ? N3 Fe2 N5 90.40(8) 2_665 2_565 ? N3 Fe2 N5 89.59(8) 1_455 2_565 ? N5 Fe2 N5 180.0 . 2_565 ? C8 Pt C11 92.23(9) . . ? C9 Pt C10 89.71(9) . . ? C9 Pt C8 178.01(9) . . ? C10 Pt C8 89.22(9) . . ? C9 Pt C11 88.71(9) . . ? C10 Pt C11 175.08(9) . . ? C1 N1 C5 117.3(2) . . ? C1 N1 Fe1 120.53(16) . . ? C5 N1 Fe1 122.15(16) . . ? C8 N2 Fe1 170.91(19) . . ? C9 N3 Fe2 173.2(2) . 1_655 ? C10 N4 Fe2 171.5(2) . . ? C16 N5 C12 117.1(2) . . ? C16 N5 Fe2 121.06(18) . . ? C12 N5 Fe2 121.64(19) . . ? C11 N6 Fe1 168.30(18) . 1_655 ? N1 C1 C2 123.1(2) . . ? C1 C2 C3 119.5(2) . . ? C4 C3 C2 117.5(2) . . ? C4 C3 C6 122.3(3) . . ? C2 C3 C6 120.1(3) . . ? C5 C4 C3 120.0(2) . . ? N1 C5 C4 122.5(2) . . ? C7 C6 C3 173.9(4) . . ? C6 C7 C18 174.9(4) . 1_554 ? N2 C8 Pt 174.7(2) . . ? N3 C9 Pt 177.9(2) . . ? N4 C10 Pt 178.8(2) . . ? N6 C11 Pt 170.60(19) . . ? N5 C12 C13 123.4(3) . . ? C12 C13 C14 119.4(3) . . ? C15 C14 C13 117.7(3) . . ? C15 C14 C17 121.4(3) . . ? C13 C14 C17 120.9(3) . . ? C16 C15 C14 119.0(3) . . ? N5 C16 C15 123.5(3) . . ? C18 C17 C14 173.8(4) . . ? C17 C18 C7 174.9(4) . 1_556 ? C24 C19 C28 119.0(4) . . ? C24 C19 C20 119.4(4) . . ? C28 C19 C20 121.7(4) . . ? C21 C20 C19 120.7(4) . . ? C20 C21 C22 120.2(4) . . ? C23 C22 C21 121.8(5) . . ? C22 C23 C24 120.4(4) . . ? C25 C24 C19 119.9(4) . . ? C25 C24 C23 122.5(4) . . ? C19 C24 C23 117.6(4) . . ? C26 C25 C24 120.5(4) . . ? C25 C26 C27 121.6(4) . . ? C28 C27 C26 119.8(4) . . ? C27 C28 C19 119.2(4) . . ? C30 C29 C34 118.4(3) . . ? C30 C29 C38 123.6(4) . . ? C34 C29 C38 118.0(4) . . ? C31 C30 C29 121.4(4) . . ? C30 C31 C32 120.3(4) . . ? C33 C32 C31 120.5(4) . . ? C32 C33 C34 120.6(4) . . ? C35 C34 C33 121.9(4) . . ? C35 C34 C29 119.3(4) . . ? C33 C34 C29 118.7(3) . . ? C36 C35 C34 120.9(4) . . ? C35 C36 C37 120.7(4) . . ? C38 C37 C36 120.3(4) . . ? C37 C38 C29 120.8(4) . . ? _diffrn_measured_fraction_theta_max 0.918 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.819 _refine_diff_density_min -0.797 _refine_diff_density_rms 0.121 _database_code_depnum_ccdc_archive 'CCDC 971022' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_shelxl _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H24 Fe N6 Pt' _chemical_formula_weight 815.57 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 '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 7.5174(2) _cell_length_b 14.3676(7) _cell_length_c 16.350(2) _cell_angle_alpha 76.831(8) _cell_angle_beta 84.282(6) _cell_angle_gamma 89.965(3) _cell_volume 1710.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 250(1) _cell_measurement_reflns_used 150 _cell_measurement_theta_min 12 _cell_measurement_theta_max 20 _exptl_crystal_description prismatic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.584 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 796 _exptl_absorpt_coefficient_mu 4.544 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6116 _exptl_absorpt_correction_T_max 0.7126 _exptl_absorpt_process_details 'Empirical absorption correction:XABS2' _exptl_special_details ; ? ; _diffrn_ambient_temperature 250(1) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17337 _diffrn_reflns_av_R_equivalents 0.0703 _diffrn_reflns_av_sigmaI/netI 0.1059 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 29.05 _reflns_number_total 7909 _reflns_number_gt 6281 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement 'HKL DENZO' _computing_data_reduction 'HKL DENZO and SCALEPACK' _computing_structure_solution SHELXS-97 _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^ > 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^)+(0.1516P)^2^+49.4900P] 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 7909 _refine_ls_number_parameters 418 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1160 _refine_ls_R_factor_gt 0.0921 _refine_ls_wR_factor_ref 0.2144 _refine_ls_wR_factor_gt 0.1786 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.015 _refine_ls_shift/su_mean 0.006 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt Pt 0.49365(7) 0.23890(4) 0.03256(4) 0.0172(2) Uani 1 1 d . . . Fe2 Fe 0.0000 0.5000 0.0000 0.0130(6) Uani 1 2 d S . . Fe1 Fe 0.0000 0.0000 0.0000 0.0128(6) Uani 1 2 d S . . N1 N 0.020(2) 0.1004(13) -0.1238(11) 0.039(4) Uani 1 1 d . . . N2 N 0.191(2) 0.0865(11) 0.0353(11) 0.035(3) Uani 1 1 d . . . N3 N 0.799(2) 0.3907(11) 0.0201(11) 0.037(4) Uani 1 1 d . . . N4 N 0.204(2) 0.3979(11) 0.0070(12) 0.041(4) Uani 1 1 d . . . N5 N -0.007(3) 0.4760(18) 0.1374(14) 0.060(6) Uani 1 1 d . . . N6 N 0.788(2) 0.0823(11) 0.0387(11) 0.034(3) Uani 1 1 d . . . C1 C 0.043(3) 0.0657(18) -0.1908(16) 0.058(5) Uani 1 1 d . . . H1 H 0.0538 0.0002 -0.1855 0.070 Uiso 1 1 calc R . . C2 C 0.053(3) 0.1283(16) -0.2721(15) 0.049(5) Uani 1 1 d . . . H2 H 0.0744 0.1034 -0.3198 0.059 Uiso 1 1 calc R . . C3 C 0.030(4) 0.2285(18) -0.2817(15) 0.058(6) Uani 1 1 d . . . C4 C 0.013(4) 0.2617(16) -0.2084(14) 0.053(6) Uani 1 1 d . . . H4 H 0.0057 0.3269 -0.2110 0.064 Uiso 1 1 calc R . . C5 C 0.006(3) 0.1976(14) -0.1318(14) 0.045(5) Uani 1 1 d . . . H5 H -0.0088 0.2209 -0.0830 0.054 Uiso 1 1 calc R . . C6 C 0.031(4) 0.293(2) -0.3649(18) 0.073(7) Uani 1 1 d . . . C7 C 0.016(4) 0.334(2) -0.4366(17) 0.072(7) Uani 1 1 d . . . C8 C 0.301(2) 0.1422(12) 0.0375(12) 0.027(4) Uani 1 1 d . . . C9 C 0.688(2) 0.3364(12) 0.0259(12) 0.031(4) Uani 1 1 d . . . C10 C 0.310(2) 0.3406(11) 0.0181(12) 0.027(3) Uani 1 1 d . . . C11 C 0.680(2) 0.1383(11) 0.0412(12) 0.025(3) Uani 1 1 d . . . C12 C 0.148(4) 0.487(2) 0.1719(18) 0.071(7) Uani 1 1 d . . . H12 H 0.2525 0.5065 0.1365 0.085 Uiso 1 1 calc R . . C13 C 0.153(4) 0.468(2) 0.2617(18) 0.074(8) Uani 1 1 d . . . H13 H 0.2580 0.4754 0.2854 0.089 Uiso 1 1 calc R . . C14 C -0.010(4) 0.436(2) 0.3132(16) 0.064(7) Uani 1 1 d . . . C15 C -0.163(4) 0.432(2) 0.2773(19) 0.070(7) Uani 1 1 d . . . H15 H -0.2707 0.4169 0.3113 0.084 Uiso 1 1 calc R . . C16 C -0.162(4) 0.451(2) 0.1875(16) 0.069(7) Uani 1 1 d . . . H16 H -0.2675 0.4471 0.1635 0.083 Uiso 1 1 calc R . . C17 C -0.005(4) 0.407(2) 0.4045(19) 0.070(7) Uani 1 1 d . . . C18 C 0.006(4) 0.3814(19) 0.4777(17) 0.067(7) Uani 1 1 d . . . C19 C 0.043(5) 0.151(2) 0.381(2) 0.088(9) Uani 1 1 d . . . C20 C 0.091(6) 0.129(3) 0.467(2) 0.119(12) Uani 1 1 d . . . H20 H 0.0137 0.0963 0.5124 0.143 Uiso 1 1 calc R . . C21 C 0.261(6) 0.160(3) 0.475(3) 0.134(13) Uani 1 1 d . . . H21 H 0.3014 0.1459 0.5282 0.161 Uiso 1 1 calc R . . C22 C 0.376(6) 0.213(3) 0.407(3) 0.121(11) Uani 1 1 d . . . H22 H 0.4842 0.2357 0.4185 0.145 Uiso 1 1 calc R . . C23 C 0.339(6) 0.232(3) 0.325(3) 0.127(12) Uani 1 1 d . . . H23 H 0.4208 0.2637 0.2813 0.153 Uiso 1 1 calc R . . C24 C 0.149(5) 0.198(2) 0.308(2) 0.098(9) Uani 1 1 d . . . C25 C 0.105(7) 0.220(3) 0.232(3) 0.113(15) Uani 1 1 d . . . H25 H 0.1820 0.2550 0.1877 0.175 Uiso 1 1 calc R . . C26 C -0.057(6) 0.189(2) 0.219(3) 0.103(10) Uani 1 1 d . . . H26 H -0.0878 0.2020 0.1638 0.124 Uiso 1 1 calc R . . C27 C -0.188(6) 0.138(3) 0.286(3) 0.123(13) Uani 1 1 d . . . H27 H -0.2976 0.1189 0.2731 0.147 Uiso 1 1 calc R . . C28 C -0.146(6) 0.117(3) 0.375(3) 0.130(12) Uani 1 1 d . . . H28 H -0.2250 0.0877 0.4215 0.157 Uiso 1 1 calc R . . C29 C 0.563(4) 0.210(2) 0.6615(17) 0.062(6) Uani 1 1 d . . . C30 C 0.611(5) 0.139(2) 0.619(2) 0.089(9) Uani 1 1 d . . . H30 H 0.6316 0.1546 0.5607 0.107 Uiso 1 1 calc R . . C31 C 0.627(5) 0.048(3) 0.662(3) 0.110(11) Uani 1 1 d . . . H31 H 0.6611 0.0029 0.6313 0.132 Uiso 1 1 calc R . . C32 C 0.596(5) 0.017(3) 0.751(2) 0.109(10) Uani 1 1 d . . . H32 H 0.6014 -0.0477 0.7781 0.131 Uiso 1 1 calc R . . C33 C 0.559(4) 0.085(2) 0.795(2) 0.075(7) Uani 1 1 d . . . H33 H 0.5478 0.0669 0.8541 0.090 Uiso 1 1 calc R . . C34 C 0.538(3) 0.181(2) 0.7558(19) 0.071(7) Uani 1 1 d . . . C35 C 0.491(4) 0.254(3) 0.797(2) 0.105(11) Uani 1 1 d . . . H35 H 0.4707 0.2388 0.8557 0.126 Uiso 1 1 calc R . . C36 C 0.471(5) 0.352(3) 0.754(3) 0.126(13) Uani 1 1 d . . . H36 H 0.4446 0.3992 0.7831 0.151 Uiso 1 1 calc R . . C37 C 0.495(5) 0.372(3) 0.664(3) 0.132(14) Uani 1 1 d . . . H37 H 0.4765 0.4337 0.6351 0.159 Uiso 1 1 calc R . . C38 C 0.540(5) 0.311(3) 0.622(3) 0.102(10) Uani 1 1 d . . . H38 H 0.5580 0.3302 0.5635 0.122 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 Pt 0.0107(3) 0.0095(3) 0.0328(3) -0.0066(2) -0.0041(2) 0.00072(19) Fe2 0.0094(12) 0.0060(12) 0.0242(15) -0.0039(11) -0.0036(10) 0.0006(10) Fe1 0.0087(12) 0.0056(12) 0.0245(15) -0.0036(11) -0.0028(10) 0.0004(10) N1 0.027(7) 0.053(11) 0.034(8) -0.003(8) -0.002(6) 0.001(7) N2 0.027(7) 0.018(7) 0.061(10) -0.013(7) -0.004(7) -0.002(6) N3 0.023(7) 0.019(7) 0.062(10) 0.005(7) -0.005(7) -0.005(6) N4 0.027(8) 0.020(8) 0.078(12) -0.013(7) -0.018(7) 0.004(6) N5 0.050(11) 0.085(17) 0.049(12) -0.017(11) -0.017(9) 0.010(11) N6 0.022(7) 0.029(8) 0.055(10) -0.016(7) -0.017(7) 0.006(6) C1 0.048(12) 0.056(13) 0.064(15) 0.001(11) -0.010(10) 0.002(10) C2 0.068(13) 0.039(12) 0.042(12) -0.011(9) -0.006(10) -0.001(10) C3 0.078(15) 0.048(13) 0.042(12) 0.001(10) -0.007(11) 0.003(11) C4 0.090(17) 0.028(11) 0.036(12) 0.003(9) -0.006(11) 0.002(11) C5 0.073(13) 0.022(9) 0.039(11) -0.006(8) 0.001(9) -0.002(9) C6 0.099(19) 0.056(16) 0.055(15) 0.003(12) 0.001(13) 0.010(14) C7 0.11(2) 0.059(16) 0.047(14) 0.003(12) -0.020(13) 0.004(14) C8 0.022(8) 0.013(8) 0.049(10) -0.013(7) -0.012(7) 0.007(6) C9 0.018(7) 0.021(8) 0.052(10) -0.006(7) -0.008(7) -0.002(6) C10 0.020(7) 0.009(7) 0.051(10) -0.004(7) -0.012(7) 0.010(6) C11 0.022(7) 0.012(7) 0.042(10) -0.011(7) 0.000(7) 0.001(6) C12 0.064(16) 0.084(18) 0.060(16) -0.002(13) -0.016(12) -0.007(13) C13 0.072(17) 0.087(19) 0.052(16) 0.017(14) -0.026(13) -0.007(14) C14 0.10(2) 0.061(15) 0.033(13) -0.011(11) -0.013(13) 0.011(14) C15 0.072(16) 0.076(17) 0.064(16) -0.025(14) 0.003(13) 0.013(13) C16 0.054(14) 0.11(2) 0.042(13) -0.013(13) 0.011(10) -0.027(13) C17 0.10(2) 0.051(15) 0.060(16) -0.003(12) -0.022(14) 0.006(14) C18 0.10(2) 0.049(14) 0.044(14) 0.006(11) -0.007(13) -0.002(13) C19 0.13(2) 0.073(18) 0.065(18) -0.014(14) -0.026(16) 0.041(17) C20 0.16(3) 0.13(3) 0.07(2) -0.038(19) -0.01(2) 0.02(2) C21 0.12(3) 0.16(4) 0.12(3) -0.03(3) -0.03(2) 0.03(3) C22 0.15(3) 0.11(3) 0.12(3) -0.05(2) -0.02(2) 0.01(2) C23 0.12(3) 0.13(3) 0.13(3) -0.04(2) -0.03(2) 0.05(2) C24 0.16(3) 0.058(16) 0.07(2) -0.018(14) -0.002(18) 0.048(17) C25 0.16(5) 0.09(2) 0.09(3) -0.04(2) 0.00(3) 0.05(3) C26 0.12(3) 0.08(2) 0.12(2) -0.038(18) -0.04(2) -0.011(19) C27 0.13(3) 0.12(3) 0.14(3) -0.07(3) -0.05(3) 0.01(2) C28 0.14(3) 0.14(3) 0.12(3) -0.04(2) -0.01(2) 0.02(2) C29 0.063(14) 0.070(16) 0.054(14) -0.015(12) -0.004(11) -0.006(12) C30 0.13(2) 0.066(19) 0.071(19) -0.015(15) -0.007(17) 0.019(17) C31 0.12(3) 0.10(3) 0.12(3) -0.04(2) -0.03(2) 0.03(2) C32 0.11(3) 0.12(3) 0.09(2) -0.02(2) -0.010(19) 0.00(2) C33 0.079(17) 0.058(16) 0.077(17) 0.010(13) -0.010(13) -0.009(13) C34 0.055(14) 0.089(19) 0.079(17) -0.040(15) -0.001(12) -0.014(13) C35 0.068(19) 0.18(4) 0.07(2) -0.05(2) -0.003(15) 0.00(2) C36 0.14(3) 0.12(3) 0.14(3) -0.06(3) 0.00(2) 0.06(3) C37 0.12(3) 0.14(3) 0.17(4) -0.08(3) -0.04(3) 0.06(3) C38 0.13(3) 0.08(2) 0.11(2) -0.029(18) -0.04(2) 0.03(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N1 2.193(17) . ? Fe1 N1 2.193(17) 2 ? Fe1 N2 2.104(15) 2 ? Fe1 N2 2.104(15) . ? Fe1 N6 2.113(15) 2_655 ? Fe1 N6 2.113(15) 1_455 ? Fe2 N4 2.113(16) . ? Fe2 N4 2.113(16) 2_565 ? Fe2 N5 2.19(2) 2_565 ? Fe2 N5 2.19(2) . ? Fe2 N3 2.129(16) 1_455 ? Fe2 N3 2.129(16) 2_665 ? Pt C8 1.990(17) . ? Pt C11 2.005(16) . ? Pt C9 2.000(17) . ? Pt C10 2.000(15) . ? N1 C1 1.30(3) . ? N1 C5 1.38(3) . ? N2 C8 1.16(2) . ? N3 C9 1.13(2) . ? N3 Fe2 2.129(16) 1_655 ? N4 C10 1.14(2) . ? N5 C12 1.37(3) . ? N5 C16 1.35(3) . ? N6 C11 1.15(2) . ? N6 Fe1 2.113(15) 1_655 ? C1 C2 1.42(3) . ? C2 C3 1.43(3) . ? C3 C4 1.38(3) . ? C3 C6 1.46(4) . ? C4 C5 1.37(3) . ? C6 C7 1.21(4) . ? C7 C18 1.42(4) 1_554 ? C12 C13 1.43(4) . ? C13 C14 1.43(4) . ? C14 C15 1.35(4) . ? C14 C17 1.46(4) . ? C15 C16 1.43(4) . ? C17 C18 1.18(4) . ? C18 C7 1.42(4) 1_556 ? C19 C20 1.45(5) . ? C19 C28 1.52(5) . ? C19 C24 1.39(5) . ? C20 C21 1.39(6) . ? C21 C22 1.41(6) . ? C22 C23 1.36(6) . ? C23 C24 1.58(5) . ? C24 C25 1.29(5) . ? C25 C26 1.35(6) . ? C26 C27 1.46(6) . ? C27 C28 1.49(6) . ? C29 C30 1.39(4) . ? C29 C34 1.49(4) . ? C29 C38 1.45(4) . ? C30 C31 1.35(5) . ? C31 C32 1.42(5) . ? C32 C33 1.35(5) . ? C33 C34 1.40(4) . ? C34 C35 1.41(5) . ? C35 C36 1.43(6) . ? C36 C37 1.42(6) . ? C37 C38 1.26(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Fe1 N1 180.0(12) . 2 ? N2 Fe1 N1 87.8(7) . . ? N6 Fe1 N1 92.2(6) 2_655 . ? N6 Fe1 N1 87.8(6) 1_455 . ? N2 Fe1 N1 87.8(7) 2 2 ? N2 Fe1 N1 92.2(7) . 2 ? N6 Fe1 N1 87.8(6) 2_655 2 ? N6 Fe1 N1 92.2(6) 1_455 2 ? N2 Fe1 N2 180.0(9) 2 . ? N2 Fe1 N6 91.4(6) 2 2_655 ? N2 Fe1 N6 88.6(6) . 2_655 ? N2 Fe1 N6 88.6(6) 2 1_455 ? N2 Fe1 N6 91.4(6) . 1_455 ? N6 Fe1 N6 180.0(10) 2_655 1_455 ? N2 Fe1 N1 92.2(7) 2 . ? N4 Fe2 N4 180.000(2) . 2_565 ? N4 Fe2 N5 93.3(8) . 2_565 ? N4 Fe2 N5 86.7(8) 2_565 2_565 ? N4 Fe2 N5 86.7(8) . . ? N4 Fe2 N5 93.3(8) 2_565 . ? N5 Fe2 N5 180.00(18) 2_565 . ? N4 Fe2 N3 91.2(6) . 1_455 ? N4 Fe2 N3 88.8(6) 2_565 1_455 ? N5 Fe2 N3 92.3(8) 2_565 1_455 ? N5 Fe2 N3 87.7(8) . 1_455 ? N4 Fe2 N3 88.8(6) . 2_665 ? N4 Fe2 N3 91.2(6) 2_565 2_665 ? N5 Fe2 N3 87.7(8) 2_565 2_665 ? N5 Fe2 N3 92.3(8) . 2_665 ? N3 Fe2 N3 180.000(2) 1_455 2_665 ? C8 Pt C11 91.3(6) . . ? C8 Pt C9 179.2(8) . . ? C11 Pt C9 88.7(7) . . ? C8 Pt C10 89.0(7) . . ? C11 Pt C10 177.3(8) . . ? C9 Pt C10 91.0(7) . . ? C1 N1 C5 120.0(19) . . ? C1 N1 Fe1 118.1(16) . . ? C5 N1 Fe1 121.9(14) . . ? C8 N2 Fe1 166.2(16) . . ? C9 N3 Fe2 175.3(16) . 1_655 ? C10 N4 Fe2 174.2(18) . . ? C12 N5 C16 120(2) . . ? C12 N5 Fe2 118.8(18) . . ? C16 N5 Fe2 120.9(17) . . ? C11 N6 Fe1 164.6(16) . 1_655 ? N1 C1 C2 120(2) . . ? C3 C2 C1 121(2) . . ? C4 C3 C2 116(2) . . ? C4 C3 C6 122(2) . . ? C2 C3 C6 121(2) . . ? C3 C4 C5 119(2) . . ? N1 C5 C4 123(2) . . ? C7 C6 C3 169(3) . . ? C6 C7 C18 177(4) . 1_554 ? N2 C8 Pt 176.1(17) . . ? N3 C9 Pt 178.0(19) . . ? N4 C10 Pt 177.4(18) . . ? N6 C11 Pt 174.1(17) . . ? N5 C12 C13 121(3) . . ? C12 C13 C14 117(3) . . ? C15 C14 C13 120(3) . . ? C15 C14 C17 122(3) . . ? C13 C14 C17 118(3) . . ? C16 C15 C14 121(3) . . ? N5 C16 C15 120(3) . . ? C18 C17 C14 177(4) . . ? C17 C18 C7 170(3) . 1_556 ? C20 C19 C28 112(4) . . ? C20 C19 C24 127(4) . . ? C28 C19 C24 121(3) . . ? C21 C20 C19 114(4) . . ? C20 C21 C22 124(4) . . ? C23 C22 C21 124(4) . . ? C22 C23 C24 117(4) . . ? C25 C24 C23 118(4) . . ? C25 C24 C19 127(4) . . ? C23 C24 C19 114(3) . . ? C26 C25 C24 117(5) . . ? C25 C26 C27 124(4) . . ? C28 C27 C26 120(4) . . ? C27 C28 C19 110(4) . . ? C30 C29 C34 116(3) . . ? C30 C29 C38 126(3) . . ? C34 C29 C38 118(3) . . ? C29 C30 C31 121(3) . . ? C32 C31 C30 124(4) . . ? C33 C32 C31 117(4) . . ? C32 C33 C34 122(3) . . ? C35 C34 C29 115(3) . . ? C35 C34 C33 126(3) . . ? C29 C34 C33 119(3) . . ? C34 C35 C36 124(4) . . ? C35 C36 C37 116(4) . . ? C38 C37 C36 124(5) . . ? C37 C38 C29 122(4) . . ? _diffrn_measured_fraction_theta_max 0.863 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.501 _refine_diff_density_min -0.421 _refine_diff_density_rms 0.451 _database_code_depnum_ccdc_archive 'CCDC 971023' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_shelxl _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H18 Fe N8 O4 Pt' _chemical_formula_weight 805.46 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' N N 0.0061 0.0033 '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' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.2443(4) _cell_length_b 13.8127(8) _cell_length_c 15.4746(9) _cell_angle_alpha 80.352(5) _cell_angle_beta 87.669(5) _cell_angle_gamma 89.842(5) _cell_volume 1525.26(15) _cell_formula_units_Z 2 _cell_measurement_temperature 120(1) _cell_measurement_reflns_used 100 _cell_measurement_theta_min 12 _cell_measurement_theta_max 20 _exptl_crystal_description prismatic _exptl_crystal_colour red _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.754 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 780 _exptl_absorpt_coefficient_mu 5.105 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6855 _exptl_absorpt_correction_T_max 0.7493 _exptl_absorpt_process_details 'Empirical absorption correction:XABS2' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(1) _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15916 _diffrn_reflns_av_R_equivalents 0.0523 _diffrn_reflns_av_sigmaI/netI 0.0828 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.48 _diffrn_reflns_theta_max 30.69 _reflns_number_total 8232 _reflns_number_gt 7031 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement 'HKL DENZO' _computing_data_reduction 'HKL DENZO and SCALEPACK' _computing_structure_solution SHELXS-97 _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^ > 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^)+(0.0580P)^2^+4.6644P] 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 8232 _refine_ls_number_parameters 388 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0634 _refine_ls_R_factor_gt 0.0511 _refine_ls_wR_factor_ref 0.1295 _refine_ls_wR_factor_gt 0.1178 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.072 _refine_ls_shift/su_max 0.036 _refine_ls_shift/su_mean 0.014 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 Pt1 Pt 0.00288(3) 0.260609(15) 0.462873(15) 0.00885(8) Uani 1 1 d . . . Fe1 Fe -0.5000 0.5000 0.5000 0.0071(2) Uani 1 2 d S . . Fe2 Fe 0.5000 0.0000 0.5000 0.0073(2) Uani 1 2 d S . . N1 N -0.4918(7) 0.5895(4) 0.3840(4) 0.0110(10) Uani 1 1 d . . . N2 N -0.3063(7) 0.4189(3) 0.4610(4) 0.0098(10) Uani 1 1 d . . . N3 N 0.3110(7) 0.0999(4) 0.4899(4) 0.0109(10) Uani 1 1 d . . . N4 N -0.3101(7) 0.1005(4) 0.4861(4) 0.0108(10) Uani 1 1 d . . . N5 N 0.5033(8) 0.0068(4) 0.3700(4) 0.0140(11) Uani 1 1 d . . . N6 N 0.3125(7) 0.4185(4) 0.4625(4) 0.0114(10) Uani 1 1 d . . . N7 N -0.0102(12) 0.1562(7) 0.7904(8) 0.057(3) Uani 1 1 d . . . N8 N 0.460(2) 0.388(2) 0.0272(7) 0.79(9) Uani 1 1 d D . . O1 O -0.0035(12) 0.1181(6) 0.7240(7) 0.067(2) Uani 1 1 d . . . O2 O -0.0091(16) 0.1094(7) 0.8647(7) 0.089(3) Uani 1 1 d . . . O3 O 0.301(3) 0.3983(18) 0.0007(10) 0.36(3) Uani 1 1 d D . . O4 O 0.600(3) 0.4056(13) -0.0190(6) 0.263(15) Uani 1 1 d D . . C1 C -0.4853(9) 0.5538(5) 0.3068(4) 0.0146(12) Uani 1 1 d . . . H1 H -0.4818 0.4861 0.3091 0.017 Uiso 1 1 calc R . . C2 C -0.4837(11) 0.6122(5) 0.2270(5) 0.0221(15) Uani 1 1 d . . . H2 H -0.4798 0.5844 0.1762 0.027 Uiso 1 1 calc R . . C3 C -0.4879(11) 0.7149(5) 0.2214(5) 0.0238(15) Uani 1 1 d . . . C4 C -0.4925(11) 0.7519(5) 0.3002(5) 0.0209(14) Uani 1 1 d . . . H4 H -0.4940 0.8194 0.2993 0.025 Uiso 1 1 calc R . . C5 C -0.4948(8) 0.6890(4) 0.3788(5) 0.0133(12) Uani 1 1 d . . . H5 H -0.4985 0.7152 0.4305 0.016 Uiso 1 1 calc R . . C6 C -0.4890(13) 0.7783(6) 0.1375(5) 0.0300(18) Uani 1 1 d . . . C7 C -0.4925(14) 0.8261(6) 0.0660(5) 0.035(2) Uani 1 1 d . . . C8 C -0.4985(15) 0.8763(6) -0.0185(5) 0.036(2) Uani 1 1 d . . . C9 C -0.1918(9) 0.3632(4) 0.4549(4) 0.0137(12) Uani 1 1 d . . . C10 C 0.3448(10) 0.0145(5) 0.3262(5) 0.0175(13) Uani 1 1 d . . . H10 H 0.2331 0.0056 0.3584 0.021 Uiso 1 1 calc R . . C11 C 0.3413(12) 0.0350(5) 0.2357(5) 0.0240(15) Uani 1 1 d . . . H11 H 0.2293 0.0385 0.2080 0.029 Uiso 1 1 calc R . . C12 C 0.5065(12) 0.0503(5) 0.1864(5) 0.0259(17) Uani 1 1 d . . . C13 C 0.6702(12) 0.0368(5) 0.2300(5) 0.0249(16) Uani 1 1 d . . . H13 H 0.7830 0.0421 0.1986 0.030 Uiso 1 1 calc R . . C14 C 0.6641(10) 0.0149(5) 0.3219(5) 0.0210(14) Uani 1 1 d . . . H14 H 0.7745 0.0057 0.3507 0.025 Uiso 1 1 calc R . . C15 C 0.5029(14) 0.0849(6) 0.0934(5) 0.0332(19) Uani 1 1 d . . . C16 C 0.1966(9) 0.1580(4) 0.4799(4) 0.0122(12) Uani 1 1 d . . . C17 C -0.1945(8) 0.1585(4) 0.4772(4) 0.0104(11) Uani 1 1 d . . . C18 C 0.1965(8) 0.3628(4) 0.4570(4) 0.0119(12) Uani 1 1 d . . . C19 C -0.0141(12) 0.2646(7) 0.7796(6) 0.0353(19) Uani 1 1 d . . . C20 C -0.0173(15) 0.3086(8) 0.8525(7) 0.050(3) Uani 1 1 d . . . H20 H -0.0186 0.2715 0.9085 0.061 Uiso 1 1 calc R . . C21 C -0.0185(15) 0.4102(9) 0.8402(9) 0.057(3) Uani 1 1 d . . . H21 H -0.0198 0.4426 0.8882 0.069 Uiso 1 1 calc R . . C22 C -0.0179(14) 0.4642(7) 0.7542(8) 0.046(2) Uani 1 1 d . . . H22 H -0.0200 0.5324 0.7460 0.055 Uiso 1 1 calc R . . C23 C -0.0144(12) 0.4174(7) 0.6827(7) 0.040(2) Uani 1 1 d . . . H23 H -0.0122 0.4533 0.6262 0.048 Uiso 1 1 calc R . . C24 C -0.0141(12) 0.3165(7) 0.6962(6) 0.036(2) Uani 1 1 d . . . H24 H -0.0138 0.2834 0.6486 0.043 Uiso 1 1 calc R . . C25 C 0.4823(17) 0.3504(6) 0.1161(4) 0.120(10) Uani 1 1 d GD . . C26 C 0.6566(14) 0.3397(7) 0.1509(5) 0.123(9) Uani 1 1 d GD . . C27 C 0.6744(11) 0.3016(6) 0.2391(5) 0.073(4) Uani 1 1 d G . . C28 C 0.5180(13) 0.2742(5) 0.2926(4) 0.047(3) Uani 1 1 d G . . C29 C 0.3438(11) 0.2850(7) 0.2578(6) 0.085(5) Uani 1 1 d G . . C30 C 0.3260(13) 0.3231(7) 0.1696(6) 0.30(3) Uani 1 1 d GD . . 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 Pt1 0.00549(12) 0.00302(11) 0.01841(14) -0.00243(8) -0.00239(8) 0.00103(7) Fe1 0.0046(5) 0.0021(5) 0.0145(6) -0.0005(4) -0.0021(4) 0.0011(4) Fe2 0.0054(5) 0.0018(5) 0.0144(6) -0.0001(4) -0.0017(4) 0.0004(4) N1 0.007(2) 0.007(2) 0.018(3) 0.0017(19) -0.0048(19) 0.0028(18) N2 0.007(2) 0.002(2) 0.020(3) -0.0012(18) -0.0027(19) 0.0041(18) N5 0.024(3) 0.001(2) 0.016(3) 0.0030(18) -0.003(2) 0.001(2) N3 0.007(2) 0.004(2) 0.022(3) -0.0036(19) -0.003(2) -0.0014(18) N4 0.007(2) 0.005(2) 0.020(3) -0.0027(19) -0.0021(19) -0.0005(18) N6 0.008(2) 0.005(2) 0.021(3) -0.0021(19) -0.003(2) 0.0011(19) N7 0.029(4) 0.035(5) 0.104(9) -0.006(5) -0.002(5) 0.003(4) N8 2.0(2) 0.09(2) 0.22(4) -0.03(2) 0.60(8) -0.07(6) O1 0.066(5) 0.037(4) 0.101(7) -0.027(5) 0.004(5) 0.003(4) O2 0.117(9) 0.057(6) 0.079(7) 0.024(5) 0.002(6) 0.009(6) O3 0.34(3) 0.19(2) 0.62(6) -0.19(3) -0.36(4) 0.11(2) O4 0.60(5) 0.128(15) 0.057(10) -0.014(10) -0.005(18) -0.05(2) C1 0.018(3) 0.011(3) 0.014(3) -0.003(2) 0.000(2) 0.001(2) C2 0.037(4) 0.014(3) 0.017(4) -0.008(3) -0.001(3) 0.003(3) C3 0.031(4) 0.019(3) 0.021(4) 0.000(3) 0.001(3) -0.003(3) C4 0.033(4) 0.010(3) 0.019(4) 0.001(2) -0.004(3) 0.003(3) C5 0.008(3) 0.008(3) 0.023(3) -0.001(2) -0.003(2) 0.000(2) C6 0.049(5) 0.020(4) 0.021(4) -0.003(3) -0.001(3) 0.000(3) C7 0.062(6) 0.021(4) 0.020(4) 0.000(3) -0.004(4) 0.000(4) C8 0.071(7) 0.021(4) 0.016(4) 0.000(3) -0.004(4) -0.001(4) C9 0.016(3) 0.008(3) 0.017(3) -0.003(2) 0.000(2) -0.007(2) C10 0.021(3) 0.007(3) 0.025(4) -0.002(2) -0.005(3) 0.001(2) C11 0.039(4) 0.018(3) 0.016(4) -0.003(3) -0.007(3) -0.003(3) C12 0.050(5) 0.010(3) 0.018(4) -0.005(3) 0.000(3) 0.001(3) C13 0.040(4) 0.019(3) 0.015(4) -0.003(3) 0.008(3) -0.001(3) C14 0.024(4) 0.014(3) 0.024(4) -0.002(3) 0.004(3) 0.001(3) C15 0.061(6) 0.019(4) 0.019(4) -0.002(3) 0.001(4) 0.000(4) C16 0.012(3) 0.004(2) 0.021(3) -0.004(2) 0.000(2) -0.003(2) C17 0.007(3) 0.004(2) 0.020(3) -0.002(2) -0.005(2) 0.005(2) C18 0.011(3) 0.009(3) 0.016(3) -0.002(2) -0.003(2) 0.010(2) C19 0.030(4) 0.031(4) 0.044(5) -0.002(4) -0.007(4) 0.004(4) C20 0.056(7) 0.056(7) 0.039(6) -0.007(5) -0.005(5) 0.002(5) C21 0.053(7) 0.057(7) 0.071(8) -0.040(7) -0.005(6) 0.005(6) C22 0.049(6) 0.029(5) 0.063(7) -0.016(5) -0.009(5) 0.000(4) C23 0.033(5) 0.037(5) 0.048(6) 0.002(4) -0.001(4) -0.001(4) C24 0.031(4) 0.036(5) 0.042(5) -0.010(4) 0.001(4) 0.002(4) C25 0.27(3) 0.041(7) 0.066(10) -0.033(7) -0.106(14) 0.051(12) C26 0.23(2) 0.063(10) 0.079(12) -0.033(9) 0.071(14) -0.053(13) C27 0.097(11) 0.064(8) 0.066(9) -0.033(7) -0.003(8) -0.012(8) C28 0.066(7) 0.023(4) 0.055(7) -0.011(4) -0.012(5) -0.001(4) C29 0.117(13) 0.071(10) 0.080(11) -0.040(9) -0.043(10) 0.034(9) C30 0.37(5) 0.10(2) 0.45(6) -0.18(3) 0.26(5) -0.07(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 C18 1.981(6) . ? Pt1 C16 1.985(6) . ? Pt1 C17 1.991(6) . ? Pt1 C9 1.990(7) . ? Fe1 N2 1.933(5) 2_466 ? Fe1 N2 1.933(5) . ? Fe1 N1 2.000(5) 2_466 ? Fe1 N1 2.000(5) . ? Fe2 N3 1.934(5) . ? Fe2 N3 1.934(5) 2_656 ? Fe2 N4 1.937(5) 1_655 ? Fe2 N4 1.937(5) 2_556 ? Fe2 N5 1.997(6) 2_656 ? Fe2 N5 1.997(6) . ? Fe1 N6 1.934(5) 2_566 ? Fe1 N6 1.934(5) 1_455 ? N1 C5 1.363(8) . ? N1 C1 1.366(8) . ? N2 C9 1.142(8) . ? N5 C14 1.351(9) . ? N5 C10 1.352(9) . ? N3 C16 1.149(8) . ? N4 C17 1.149(8) . ? N4 Fe2 1.937(5) 1_455 ? N6 C18 1.156(8) . ? N6 Fe1 1.934(5) 1_655 ? N7 O2 1.222(14) . ? N7 O1 1.229(13) . ? N7 C19 1.480(12) . ? N8 O4 1.221(8) . ? N8 O3 1.236(8) . ? N8 C25 1.402(6) . ? C1 C2 1.357(10) . ? C2 C3 1.407(10) . ? C3 C4 1.398(10) . ? C3 C6 1.441(11) . ? C4 C5 1.371(9) . ? C6 C7 1.190(11) . ? C7 C8 1.376(11) . ? C8 C15 1.194(11) 2_565 ? C10 C11 1.383(10) . ? C11 C12 1.390(11) . ? C12 C13 1.385(12) . ? C12 C15 1.440(11) . ? C13 C14 1.402(10) . ? C15 C8 1.194(11) 2_565 ? C19 C20 1.367(14) . ? C19 C24 1.367(13) . ? C20 C21 1.383(15) . ? C21 C22 1.411(17) . ? C22 C23 1.371(14) . ? C23 C24 1.375(13) . ? C25 C26 1.3900 . ? C25 C30 1.3900 . ? C26 C27 1.3900 . ? C27 C28 1.3900 . ? C28 C29 1.3900 . ? C29 C30 1.3900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C18 Pt1 C16 89.4(2) . . ? C18 Pt1 C17 176.2(2) . . ? C16 Pt1 C17 91.0(2) . . ? C18 Pt1 C9 90.3(2) . . ? C16 Pt1 C9 176.0(3) . . ? C17 Pt1 C9 89.0(2) . . ? N2 Fe1 N1 91.6(2) 2_466 2_466 ? N2 Fe1 N1 88.4(2) . 2_466 ? N2 Fe1 N2 180.0(3) 2_466 . ? N6 Fe1 N1 91.8(2) 2_566 2_466 ? N6 Fe1 N1 88.2(2) 1_455 2_466 ? N2 Fe1 N1 88.4(2) 2_466 . ? N2 Fe1 N1 91.6(2) . . ? N6 Fe1 N1 88.2(2) 2_566 . ? N6 Fe1 N1 91.8(2) 1_455 . ? N1 Fe1 N1 180.000(1) 2_466 . ? N2 Fe1 N6 91.1(2) 2_466 2_566 ? N2 Fe1 N6 88.9(2) . 2_566 ? N2 Fe1 N6 88.9(2) 2_466 1_455 ? N2 Fe1 N6 91.1(2) . 1_455 ? N6 Fe1 N6 180.000(1) 2_566 1_455 ? N3 Fe2 N3 180.000(1) . 2_656 ? N3 Fe2 N4 90.3(2) . 1_655 ? N3 Fe2 N4 89.7(2) 2_656 1_655 ? N3 Fe2 N4 89.7(2) . 2_556 ? N3 Fe2 N4 90.3(2) 2_656 2_556 ? N4 Fe2 N4 180.000(1) 1_655 2_556 ? N3 Fe2 N5 90.8(2) . 2_656 ? N3 Fe2 N5 89.2(2) 2_656 2_656 ? N4 Fe2 N5 90.2(2) 1_655 2_656 ? N4 Fe2 N5 89.8(2) 2_556 2_656 ? N3 Fe2 N5 89.2(2) . . ? N3 Fe2 N5 90.8(2) 2_656 . ? N4 Fe2 N5 89.8(2) 1_655 . ? N4 Fe2 N5 90.2(2) 2_556 . ? N5 Fe2 N5 180.000(1) 2_656 . ? C5 N1 C1 117.1(5) . . ? C5 N1 Fe1 121.2(4) . . ? C1 N1 Fe1 121.6(4) . . ? C9 N2 Fe1 166.6(5) . . ? C14 N5 C10 117.5(6) . . ? C14 N5 Fe2 121.1(5) . . ? C10 N5 Fe2 121.1(5) . . ? C16 N3 Fe2 176.6(5) . . ? C17 N4 Fe2 178.3(5) . 1_455 ? C18 N6 Fe1 166.8(5) . 1_655 ? O2 N7 O1 123.6(10) . . ? O2 N7 C19 118.2(11) . . ? O1 N7 C19 118.2(10) . . ? O4 N8 O3 124.7(8) . . ? O4 N8 C25 116.8(8) . . ? O3 N8 C25 118.4(8) . . ? C2 C1 N1 123.3(6) . . ? C1 C2 C3 119.7(6) . . ? C4 C3 C2 117.3(7) . . ? C4 C3 C6 121.9(7) . . ? C2 C3 C6 120.7(7) . . ? C5 C4 C3 120.2(6) . . ? N1 C5 C4 122.4(6) . . ? C7 C6 C3 176.2(8) . . ? C6 C7 C8 176.7(9) . . ? C15 C8 C7 176.4(9) 2_565 . ? N2 C9 Pt1 171.7(6) . . ? N5 C10 C11 123.0(7) . . ? C10 C11 C12 119.5(7) . . ? C13 C12 C11 118.2(7) . . ? C13 C12 C15 122.1(8) . . ? C11 C12 C15 119.6(8) . . ? C12 C13 C14 119.3(7) . . ? N5 C14 C13 122.3(7) . . ? C8 C15 C12 172.7(9) 2_565 . ? N3 C16 Pt1 178.8(5) . . ? N4 C17 Pt1 178.9(6) . . ? N6 C18 Pt1 173.0(6) . . ? C20 C19 C24 122.9(9) . . ? C20 C19 N7 119.3(10) . . ? C24 C19 N7 117.8(9) . . ? C19 C20 C21 117.8(11) . . ? C20 C21 C22 119.6(10) . . ? C23 C22 C21 120.9(9) . . ? C22 C23 C24 118.7(10) . . ? C19 C24 C23 120.1(9) . . ? C26 C25 C30 120.0 . . ? C26 C25 N8 121.5(5) . . ? C30 C25 N8 118.5(5) . . ? C27 C26 C25 120.0 . . ? C26 C27 C28 120.0 . . ? C29 C28 C27 120.0 . . ? C28 C29 C30 120.0 . . ? C29 C30 C25 120.0 . . ? _diffrn_measured_fraction_theta_max 0.869 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.403 _refine_diff_density_min -1.502 _refine_diff_density_rms 0.284 _database_code_depnum_ccdc_archive 'CCDC 971024' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_shelxl _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H18 Fe N8 O4 Pt' _chemical_formula_weight 805.46 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' N N 0.0061 0.0033 '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' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.4872(7) _cell_length_b 14.3024(7) _cell_length_c 15.0203(15) _cell_angle_alpha 86.393(6) _cell_angle_beta 84.502(8) _cell_angle_gamma 89.936(5) _cell_volume 1597.9(2) _cell_formula_units_Z 2 _cell_measurement_temperature 250(1) _cell_measurement_reflns_used 100 _cell_measurement_theta_min 12 _cell_measurement_theta_max 20 _exptl_crystal_description prismatic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.674 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 780 _exptl_absorpt_coefficient_mu 4.873 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6965 _exptl_absorpt_correction_T_max 0.7586 _exptl_absorpt_process_details 'Empirical absorption correction:XABS2' _exptl_special_details ; ? ; _diffrn_ambient_temperature 250(1) _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14808 _diffrn_reflns_av_R_equivalents 0.0772 _diffrn_reflns_av_sigmaI/netI 0.1054 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 30.63 _reflns_number_total 8591 _reflns_number_gt 6945 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement 'HKL DENZO' _computing_data_reduction 'HKL DENZO and SCALEPACK' _computing_structure_solution SHELXS-97 _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^ > 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^)+(0.0621P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8591 _refine_ls_number_parameters 178 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.1249 _refine_ls_R_factor_gt 0.0995 _refine_ls_wR_factor_ref 0.2111 _refine_ls_wR_factor_gt 0.1844 _refine_ls_goodness_of_fit_ref 1.161 _refine_ls_restrained_S_all 1.162 _refine_ls_shift/su_max 0.042 _refine_ls_shift/su_mean 0.017 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 N7 N -0.021(8) 0.173(2) 0.801(3) 0.23(2) Uiso 1 1 d D . . N8 N 0.406(5) 0.381(7) 0.035(3) 0.68(11) Uiso 1 1 d D . . C19 C -0.024(4) 0.268(2) 0.7918(18) 0.081(7) Uiso 1 1 d D . . C20 C -0.045(5) 0.320(2) 0.869(2) 0.099(9) Uiso 1 1 d . . . C21 C -0.030(6) 0.414(3) 0.856(3) 0.127(13) Uiso 1 1 d . . . C22 C -0.045(5) 0.458(3) 0.768(3) 0.111(11) Uiso 1 1 d . . . C23 C -0.034(5) 0.406(3) 0.697(2) 0.113(11) Uiso 1 1 d . . . C24 C -0.031(4) 0.313(2) 0.7052(19) 0.083(7) Uiso 1 1 d . . . C25 C 0.461(3) 0.347(2) 0.1160(16) 0.133(14) Uiso 1 1 d GD . . C26 C 0.642(3) 0.346(2) 0.1296(17) 0.134(13) Uiso 1 1 d GD . . C27 C 0.697(3) 0.308(2) 0.2099(19) 0.143(14) Uiso 1 1 d G . . C28 C 0.571(4) 0.270(2) 0.2766(16) 0.111(10) Uiso 1 1 d G . . C29 C 0.390(4) 0.272(2) 0.2630(17) 0.172(19) Uiso 1 1 d G . . C30 C 0.335(3) 0.310(2) 0.183(2) 0.25(3) Uiso 1 1 d GD . . Pt1 Pt 0.00681(5) 0.25891(2) 0.46230(3) 0.02121(19) Uani 1 1 d . . . Fe1 Fe -0.5000 0.5000 0.5000 0.0220(5) Uani 1 2 d S . . Fe2 Fe 0.5000 0.0000 0.5000 0.0215(5) Uani 1 2 d S . . N1 N -0.4814(16) 0.5941(8) 0.3779(8) 0.032(2) Uiso 1 1 d . . . N2 N -0.2834(17) 0.4147(8) 0.4436(8) 0.029(2) Uiso 1 1 d . . . N5 N 0.512(2) -0.0007(11) 0.3510(10) 0.049(3) Uiso 1 1 d . . . N3 N 0.2953(17) 0.1065(9) 0.4969(8) 0.029(2) Uiso 1 1 d . . . N4 N -0.2940(18) 0.1054(9) 0.4871(8) 0.032(2) Uiso 1 1 d . . . N6 N 0.3063(16) 0.4133(8) 0.4484(7) 0.028(2) Uiso 1 1 d . . . O1 O -0.023(5) 0.121(3) 0.733(2) 0.167(12) Uiso 1 1 d D . . O2 O -0.011(7) 0.123(3) 0.876(3) 0.25(2) Uiso 1 1 d D . . O3 O 0.246(7) 0.414(3) 0.029(3) 0.27(2) Uiso 1 1 d D . . O4 O 0.516(7) 0.390(8) -0.038(2) 0.97(13) Uiso 1 1 d D . . C1 C -0.468(2) 0.5527(12) 0.2924(11) 0.040(3) Uiso 1 1 d . . . C2 C -0.465(3) 0.6134(14) 0.2181(13) 0.053(4) Uiso 1 1 d . . . C3 C -0.475(3) 0.7101(15) 0.2210(13) 0.057(4) Uiso 1 1 d . . . C4 C -0.476(3) 0.7470(14) 0.3035(13) 0.052(4) Uiso 1 1 d . . . C5 C -0.483(2) 0.6868(11) 0.3798(10) 0.036(3) Uiso 1 1 d . . . C6 C -0.472(4) 0.766(2) 0.1419(19) 0.082(7) Uiso 1 1 d . . . C7 C -0.486(4) 0.8148(19) 0.0709(17) 0.074(6) Uiso 1 1 d . . . C8 C -0.503(4) 0.868(2) -0.0036(19) 0.077(7) Uiso 1 1 d . . . C9 C -0.1775(16) 0.3573(8) 0.4456(7) 0.019(2) Uiso 1 1 d . . . C10 C 0.362(3) 0.0092(15) 0.3111(14) 0.058(5) Uiso 1 1 d . . . C11 C 0.364(3) 0.0338(17) 0.2195(16) 0.070(6) Uiso 1 1 d . . . C12 C 0.513(4) 0.0480(18) 0.1690(17) 0.072(6) Uiso 1 1 d . . . C13 C 0.663(3) 0.0406(17) 0.2042(15) 0.066(5) Uiso 1 1 d . . . C14 C 0.670(3) 0.0085(17) 0.2992(16) 0.068(6) Uiso 1 1 d . . . C15 C 0.507(5) 0.089(3) 0.075(2) 0.105(10) Uiso 1 1 d . . . C16 C 0.1926(17) 0.1626(9) 0.4839(8) 0.022(2) Uiso 1 1 d . . . C17 C -0.1865(16) 0.1625(9) 0.4796(7) 0.020(2) Uiso 1 1 d . . . C18 C 0.1979(17) 0.3571(9) 0.4485(8) 0.022(2) 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 Pt1 0.0107(2) 0.0097(2) 0.0432(3) -0.00096(17) -0.00336(17) 0.00032(15) Fe1 0.0135(10) 0.0109(10) 0.0414(13) 0.0018(9) -0.0038(9) 0.0003(8) Fe2 0.0114(10) 0.0105(10) 0.0418(14) 0.0036(9) -0.0021(9) -0.0005(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N7 O1 1.303(10) . ? N7 O2 1.304(11) . ? N7 C19 1.360(10) . ? N8 O4 1.299(12) . ? N8 O3 1.298(12) . ? N8 C25 1.389(7) . ? C19 C20 1.42(4) . ? C19 C24 1.42(4) . ? C20 C21 1.36(5) . ? C21 C22 1.44(6) . ? C22 C23 1.33(5) . ? C23 C24 1.34(4) . ? C25 C26 1.3900 . ? C25 C30 1.3900 . ? C26 C27 1.3900 . ? C27 C28 1.3900 . ? C28 C29 1.3900 . ? C29 C30 1.3900 . ? Pt1 C18 1.994(13) . ? Pt1 C9 1.991(12) . ? Pt1 C17 1.987(12) . ? Pt1 C16 1.991(13) . ? Fe1 N6 2.141(12) 1_455 ? Fe1 N6 2.141(12) 2_566 ? Fe1 N2 2.167(12) . ? Fe1 N2 2.167(12) 2_466 ? Fe1 N1 2.199(12) 2_466 ? Fe1 N1 2.199(12) . ? Fe2 N4 2.144(13) 2_556 ? Fe2 N4 2.144(13) 1_655 ? Fe2 N3 2.161(12) 2_656 ? Fe2 N3 2.161(12) . ? Fe2 N5 2.232(15) . ? Fe2 N5 2.232(15) 2_656 ? N1 C5 1.328(19) . ? N1 C1 1.443(19) . ? N2 C9 1.142(17) . ? N5 C10 1.33(3) . ? N5 C14 1.35(3) . ? N3 C16 1.132(18) . ? N4 C17 1.141(19) . ? N4 Fe2 2.144(13) 1_455 ? N6 C18 1.142(18) . ? N6 Fe1 2.141(12) 1_655 ? C1 C2 1.37(3) . ? C2 C3 1.39(3) . ? C3 C6 1.39(3) . ? C3 C4 1.38(3) . ? C4 C5 1.39(2) . ? C6 C7 1.25(4) . ? C7 C8 1.33(4) . ? C8 C15 1.20(4) 2_565 ? C10 C11 1.40(3) . ? C11 C12 1.30(4) . ? C12 C13 1.28(3) . ? C12 C15 1.50(4) . ? C13 C14 1.48(3) . ? C15 C8 1.20(4) 2_565 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 N7 O2 112(4) . . ? O1 N7 C19 122(4) . . ? O2 N7 C19 126(4) . . ? O4 N8 O3 116.7(11) . . ? O4 N8 C25 122.1(16) . . ? O3 N8 C25 121(3) . . ? C20 C19 N7 119(3) . . ? C20 C19 C24 121(3) . . ? N7 C19 C24 119(3) . . ? C19 C20 C21 116(3) . . ? C22 C21 C20 120(4) . . ? C23 C22 C21 119(4) . . ? C22 C23 C24 122(4) . . ? C23 C24 C19 118(3) . . ? C26 C25 C30 120.0 . . ? C26 C25 N8 120.4(6) . . ? C30 C25 N8 119.6(6) . . ? C27 C26 C25 120.0 . . ? C28 C27 C26 120.0 . . ? C29 C28 C27 120.0 . . ? C28 C29 C30 120.0 . . ? C29 C30 C25 120.0 . . ? C18 Pt1 C9 89.9(5) . . ? C18 Pt1 C17 178.3(4) . . ? C9 Pt1 C17 89.5(5) . . ? C18 Pt1 C16 89.2(5) . . ? C9 Pt1 C16 177.6(4) . . ? C17 Pt1 C16 91.3(5) . . ? N6 Fe1 N6 180.0(9) 1_455 2_566 ? N6 Fe1 N2 90.7(5) 1_455 . ? N6 Fe1 N2 89.3(5) 2_566 . ? N6 Fe1 N2 89.3(5) 1_455 2_466 ? N6 Fe1 N2 90.7(5) 2_566 2_466 ? N2 Fe1 N2 180.000(3) . 2_466 ? N6 Fe1 N1 88.4(4) 1_455 2_466 ? N6 Fe1 N1 91.6(4) 2_566 2_466 ? N2 Fe1 N1 89.0(4) . 2_466 ? N2 Fe1 N1 91.0(4) 2_466 2_466 ? N6 Fe1 N1 91.6(4) 1_455 . ? N6 Fe1 N1 88.4(4) 2_566 . ? N2 Fe1 N1 91.0(4) . . ? N2 Fe1 N1 89.0(4) 2_466 . ? N1 Fe1 N1 180.000(2) 2_466 . ? N4 Fe2 N4 180.000(1) 2_556 1_655 ? N4 Fe2 N3 90.8(5) 2_556 2_656 ? N4 Fe2 N3 89.2(5) 1_655 2_656 ? N4 Fe2 N3 89.2(5) 2_556 . ? N4 Fe2 N3 90.8(5) 1_655 . ? N3 Fe2 N3 180.000(2) 2_656 . ? N4 Fe2 N5 90.2(5) 2_556 . ? N4 Fe2 N5 89.8(5) 1_655 . ? N3 Fe2 N5 90.7(5) 2_656 . ? N3 Fe2 N5 89.3(5) . . ? N4 Fe2 N5 89.8(5) 2_556 2_656 ? N4 Fe2 N5 90.2(5) 1_655 2_656 ? N3 Fe2 N5 89.3(5) 2_656 2_656 ? N3 Fe2 N5 90.7(5) . 2_656 ? N5 Fe2 N5 180.000(2) . 2_656 ? C5 N1 C1 119.0(13) . . ? C5 N1 Fe1 122.8(9) . . ? C1 N1 Fe1 118.1(10) . . ? C9 N2 Fe1 154.9(10) . . ? C10 N5 C14 117.9(18) . . ? C10 N5 Fe2 119.2(13) . . ? C14 N5 Fe2 121.4(14) . . ? C16 N3 Fe2 171.3(11) . . ? C17 N4 Fe2 178.8(13) . 1_455 ? C18 N6 Fe1 158.4(10) . 1_655 ? C2 C1 N1 116.4(15) . . ? C3 C2 C1 124.1(17) . . ? C2 C3 C6 120(2) . . ? C2 C3 C4 117.6(19) . . ? C6 C3 C4 122(2) . . ? C5 C4 C3 119.2(18) . . ? N1 C5 C4 123.5(14) . . ? C7 C6 C3 174(3) . . ? C6 C7 C8 179(3) . . ? C15 C8 C7 174(3) 2_565 . ? N2 C9 Pt1 174.2(10) . . ? N5 C10 C11 122(2) . . ? C12 C11 C10 122(2) . . ? C11 C12 C13 119(3) . . ? C11 C12 C15 119(3) . . ? C13 C12 C15 121(3) . . ? C12 C13 C14 122(2) . . ? N5 C14 C13 117(2) . . ? C8 C15 C12 172(4) 2_565 . ? N3 C16 Pt1 178.4(13) . . ? N4 C17 Pt1 177.5(12) . . ? N6 C18 Pt1 174.1(10) . . ? _diffrn_measured_fraction_theta_max 0.871 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.213 _refine_diff_density_min -1.285 _refine_diff_density_rms 0.569 _database_code_depnum_ccdc_archive 'CCDC 971025'