Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _publ_contact_author_email I.DANCE@UNSW.EDU.AU _publ_contact_author_name 'Prof Ian Dance' _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name I.Dance D.Craig P.A.W.Dean K.J.Fisher M.C.Jennings ; O.Ohene-Fianko ; M.Scudder G.D.Willett data_00016 _database_code_CSD 200409 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety (Ph4P)3[Fe(CN)6](H2O)(BuOH)(hexane) _chemical_formula_sum 'C88 H86 Fe N6 O2 P3' _chemical_formula_weight 1408.39 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pccn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y, z-1/2' _cell_length_a 15.8694(3) _cell_length_b 17.6413(3) _cell_length_c 26.4893(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7415.9(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.261 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2972 _exptl_absorpt_coefficient_mu 0.322 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.9124 _exptl_absorpt_correction_T_max 0.9384 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Nonius Kappa-CCD' _diffrn_measurement_method 'phi/omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43239 _diffrn_reflns_av_R_equivalents 0.056 _diffrn_reflns_av_sigmaI/netI 0.0420 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 25.03 _reflns_number_total 6540 _reflns_number_gt 4877 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement 'Nonius DENZO' _computing_data_reduction 'Nonius DENZOL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0971P)^2^+13.9546P] 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 6540 _refine_ls_number_parameters 368 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0899 _refine_ls_R_factor_gt 0.0646 _refine_ls_wR_factor_ref 0.1949 _refine_ls_wR_factor_gt 0.1768 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.067 _refine_ls_shift/su_max 0.071 _refine_ls_shift/su_mean 0.003 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 Fe Fe 0.0000 0.0000 0.5000 0.0233(2) Uani 1 2 d S . . C1 C 0.0848(3) 0.0454(2) 0.45651(15) 0.0344(9) Uani 1 1 d . . . N1 N 0.1370(3) 0.0704(2) 0.43120(16) 0.0571(11) Uani 1 1 d . . . C2 C -0.0457(2) -0.0579(2) 0.44409(14) 0.0308(9) Uani 1 1 d . . . N2 N -0.0709(2) -0.0954(2) 0.41184(14) 0.0491(10) Uani 1 1 d . . . C3 C -0.0789(2) 0.0838(2) 0.49161(13) 0.0268(8) Uani 1 1 d . . . N3 N -0.1262(2) 0.13384(19) 0.48862(12) 0.0343(8) Uani 1 1 d . . . P1 P 0.7500 0.2500 0.24852(5) 0.0281(3) Uani 1 2 d S . . P2 P 0.03670(6) 0.45989(5) 0.38875(4) 0.0272(3) Uani 1 1 d . . . C11 C 0.83093(14) 0.20829(15) 0.28686(9) 0.0337(9) Uani 1 1 d G . . C12 C 0.81300(16) 0.17677(16) 0.33374(9) 0.0456(11) Uani 1 1 d G . . H12A H 0.7570 0.1777 0.3464 0.055 Uiso 1 1 calc R . . C13 C 0.8770(2) 0.14386(17) 0.36208(8) 0.0624(15) Uani 1 1 d G . . H13A H 0.8647 0.1223 0.3941 0.075 Uiso 1 1 calc R . . C14 C 0.95892(19) 0.14246(17) 0.34354(12) 0.0645(16) Uani 1 1 d G . . H14A H 1.0027 0.1200 0.3629 0.077 Uiso 1 1 calc R . . C15 C 0.97686(13) 0.17397(18) 0.29666(13) 0.0592(14) Uani 1 1 d G . . H15A H 1.0329 0.1730 0.2840 0.071 Uiso 1 1 calc R . . C16 C 0.91286(16) 0.20689(16) 0.26832(9) 0.0462(11) Uani 1 1 d G . . H16A H 0.9251 0.2284 0.2363 0.055 Uiso 1 1 calc R . . C21 C 0.70154(16) 0.17941(13) 0.20993(9) 0.0325(9) Uani 1 1 d G . . C22 C 0.69816(17) 0.10501(14) 0.22707(9) 0.0432(10) Uani 1 1 d G . . H22A H 0.7269 0.0910 0.2571 0.052 Uiso 1 1 calc R . . C23 C 0.6527(2) 0.05102(11) 0.20024(11) 0.0555(13) Uani 1 1 d G . . H23A H 0.6504 0.0002 0.2120 0.067 Uiso 1 1 calc R . . C24 C 0.61066(18) 0.07144(15) 0.15627(11) 0.0551(13) Uani 1 1 d G . . H24A H 0.5796 0.0345 0.1379 0.066 Uiso 1 1 calc R . . C25 C 0.61404(18) 0.14585(17) 0.13912(8) 0.0525(13) Uani 1 1 d G . . H25A H 0.5853 0.1598 0.1091 0.063 Uiso 1 1 calc R . . C26 C 0.65948(18) 0.19983(13) 0.16595(9) 0.0450(11) Uani 1 1 d G . . H26A H 0.6618 0.2507 0.1542 0.054 Uiso 1 1 calc R . . C31 C 0.06519(15) 0.38032(11) 0.42740(9) 0.0303(8) Uani 1 1 d G . . C32 C 0.13594(15) 0.38244(12) 0.45830(11) 0.0407(10) Uani 1 1 d G . . H32A H 0.1684 0.4276 0.4607 0.049 Uiso 1 1 calc R . . C33 C 0.15925(15) 0.31854(15) 0.48564(11) 0.0536(12) Uani 1 1 d G . . H33A H 0.2076 0.3200 0.5068 0.064 Uiso 1 1 calc R . . C34 C 0.11180(18) 0.25252(12) 0.48208(11) 0.0480(11) Uani 1 1 d G . . H34A H 0.1277 0.2089 0.5008 0.058 Uiso 1 1 calc R . . C35 C 0.04105(17) 0.25041(11) 0.45118(11) 0.0439(10) Uani 1 1 d G . . H35A H 0.0086 0.2053 0.4487 0.053 Uiso 1 1 calc R . . C36 C 0.01774(14) 0.31431(14) 0.42384(9) 0.0361(9) Uani 1 1 d G . . H36A H -0.0306 0.3129 0.4027 0.043 Uiso 1 1 calc R . . C41 C -0.07524(11) 0.47059(15) 0.39071(9) 0.0316(9) Uani 1 1 d G . . C42 C -0.11932(15) 0.45887(16) 0.43538(8) 0.0425(10) Uani 1 1 d G . . H42A H -0.0912 0.4388 0.4641 0.051 Uiso 1 1 calc R . . C43 C -0.20455(15) 0.47657(18) 0.43807(9) 0.0531(12) Uani 1 1 d G . . H43A H -0.2347 0.4686 0.4686 0.064 Uiso 1 1 calc R . . C44 C -0.24570(12) 0.50598(18) 0.39610(12) 0.0541(13) Uani 1 1 d G . . H44A H -0.3040 0.5181 0.3979 0.065 Uiso 1 1 calc R . . C45 C -0.20162(15) 0.51770(17) 0.35143(10) 0.0527(12) Uani 1 1 d G . . H45A H -0.2297 0.5378 0.3227 0.063 Uiso 1 1 calc R . . C46 C -0.11639(15) 0.50000(16) 0.34874(8) 0.0403(10) Uani 1 1 d G . . H46A H -0.0863 0.5080 0.3182 0.048 Uiso 1 1 calc R . . C51 C 0.08366(14) 0.54638(11) 0.41100(10) 0.0299(8) Uani 1 1 d G . . C52 C 0.17067(13) 0.55407(13) 0.41413(10) 0.0379(10) Uani 1 1 d G . . H52A H 0.2063 0.5136 0.4038 0.046 Uiso 1 1 calc R . . C53 C 0.20563(12) 0.62089(15) 0.43241(11) 0.0466(11) Uani 1 1 d G . . H53A H 0.2651 0.6261 0.4346 0.056 Uiso 1 1 calc R . . C54 C 0.15358(17) 0.68003(12) 0.44757(10) 0.0486(12) Uani 1 1 d G . . H54A H 0.1775 0.7257 0.4601 0.058 Uiso 1 1 calc R . . C55 C 0.06656(16) 0.67235(12) 0.44444(10) 0.0448(11) Uani 1 1 d G . . H55A H 0.0310 0.7128 0.4548 0.054 Uiso 1 1 calc R . . C56 C 0.03160(11) 0.60552(13) 0.42615(10) 0.0349(9) Uani 1 1 d G . . H56A H -0.0279 0.6003 0.4240 0.042 Uiso 1 1 calc R . . C61 C 0.06518(17) 0.44613(13) 0.32367(7) 0.0306(8) Uani 1 1 d G . . C62 C 0.04661(18) 0.37731(12) 0.30066(9) 0.0419(10) Uani 1 1 d G . . H62A H 0.0258 0.3363 0.3202 0.050 Uiso 1 1 calc R . . C63 C 0.05854(19) 0.36854(12) 0.24901(9) 0.0487(11) Uani 1 1 d G . . H63A H 0.0459 0.3215 0.2333 0.058 Uiso 1 1 calc R . . C64 C 0.08905(18) 0.42858(15) 0.22036(7) 0.0418(10) Uani 1 1 d G . . H64A H 0.0972 0.4226 0.1851 0.050 Uiso 1 1 calc R . . C65 C 0.10762(18) 0.49739(13) 0.24337(9) 0.0412(10) Uani 1 1 d G . . H65A H 0.1285 0.5384 0.2238 0.049 Uiso 1 1 calc R . . C66 C 0.09568(17) 0.50617(11) 0.29502(9) 0.0374(9) Uani 1 1 d G . . H66A H 0.1084 0.5532 0.3107 0.045 Uiso 1 1 calc R . . C71 C -0.0633(5) 0.7683(4) 0.3513(3) 0.109(2) Uiso 1 1 d D . . H71A H -0.0802 0.8210 0.3455 0.164 Uiso 1 1 calc R . . H71B H -0.0329 0.7494 0.3217 0.164 Uiso 1 1 calc R . . H71C H -0.0267 0.7656 0.3810 0.164 Uiso 1 1 calc R . . C72 C -0.1341(4) 0.7244(4) 0.3593(3) 0.091(2) Uiso 1 1 d D . . H72A H -0.1303 0.7000 0.3928 0.109 Uiso 1 1 calc R . . H72B H -0.1366 0.6839 0.3334 0.109 Uiso 1 1 calc R . . C73 C -0.2122(4) 0.7709(4) 0.3567(3) 0.103(2) Uiso 1 1 d D . . H73A H -0.2129 0.8060 0.3858 0.124 Uiso 1 1 calc R . . H73B H -0.2102 0.8021 0.3256 0.124 Uiso 1 1 calc R . . C81 C 0.237(2) 0.3880(16) 0.3611(9) 0.286(18) Uiso 0.50 1 d PD A -1 H81A H 0.2368 0.4430 0.3563 0.429 Uiso 0.50 1 calc PR A -1 H81B H 0.2731 0.3750 0.3899 0.429 Uiso 0.50 1 calc PR A -1 H81C H 0.1795 0.3703 0.3676 0.429 Uiso 0.50 1 calc PR A -1 C82 C 0.2693(8) 0.3517(6) 0.3159(5) 0.069(3) Uiso 0.50 1 d PD A -1 H82A H 0.3305 0.3625 0.3145 0.082 Uiso 0.50 1 calc PR A -1 H82B H 0.2434 0.3779 0.2868 0.082 Uiso 0.50 1 calc PR A -1 C83 C 0.259(3) 0.2692(9) 0.3072(8) 0.212(11) Uiso 0.50 1 d PD A -1 H83A H 0.2243 0.2647 0.2763 0.254 Uiso 0.50 1 calc PR A -1 H83B H 0.3158 0.2503 0.2981 0.254 Uiso 0.50 1 calc PR A -1 C84 C 0.2246(14) 0.2135(9) 0.3429(7) 0.142(7) Uiso 0.50 1 d PD A -1 H84A H 0.2724 0.2003 0.3652 0.171 Uiso 0.50 1 calc PR A -1 H84B H 0.1848 0.2427 0.3642 0.171 Uiso 0.50 1 calc PR A -1 O85 O 0.1831(12) 0.1436(9) 0.3335(8) 0.199(7) Uiso 0.50 1 d PD A -1 H85A H 0.1325 0.1469 0.3425 0.299 Uiso 0.50 1 calc PR A -1 O91 O -0.2500 0.2500 0.4366(2) 0.134(4) Uani 1 2 d SD . . H91 H -0.213(4) 0.233(5) 0.456(2) 0.161 Uiso 1 1 d 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 Fe 0.0212(4) 0.0282(4) 0.0205(4) -0.0010(3) -0.0001(3) 0.0021(3) C1 0.039(2) 0.029(2) 0.036(2) -0.0051(17) 0.0063(18) 0.0005(17) N1 0.064(3) 0.042(2) 0.066(3) -0.003(2) 0.033(2) -0.010(2) C2 0.0223(18) 0.040(2) 0.030(2) -0.0027(17) -0.0011(16) 0.0084(16) N2 0.037(2) 0.067(3) 0.043(2) -0.021(2) -0.0083(17) 0.0094(19) C3 0.0249(18) 0.0328(19) 0.0228(19) 0.0002(15) -0.0015(14) -0.0015(17) N3 0.0301(17) 0.0376(18) 0.0350(19) 0.0027(15) 0.0012(14) 0.0043(16) P1 0.0283(7) 0.0356(7) 0.0203(7) 0.000 0.000 -0.0024(6) P2 0.0225(5) 0.0308(5) 0.0284(5) 0.0012(4) -0.0006(4) -0.0032(4) C11 0.039(2) 0.031(2) 0.031(2) -0.0037(17) -0.0105(17) -0.0044(17) C12 0.062(3) 0.045(2) 0.029(2) -0.0021(19) -0.008(2) 0.008(2) C13 0.104(5) 0.050(3) 0.033(3) -0.007(2) -0.027(3) 0.014(3) C14 0.077(4) 0.045(3) 0.072(4) -0.007(3) -0.046(3) 0.005(3) C15 0.042(3) 0.046(3) 0.090(4) 0.006(3) -0.024(3) -0.002(2) C16 0.035(2) 0.044(2) 0.060(3) 0.008(2) -0.010(2) -0.008(2) C21 0.0277(19) 0.046(2) 0.0234(19) -0.0076(17) 0.0011(15) -0.0022(17) C22 0.040(2) 0.044(2) 0.046(3) -0.008(2) -0.012(2) 0.001(2) C23 0.057(3) 0.046(3) 0.064(3) -0.017(2) -0.010(3) -0.004(2) C24 0.044(3) 0.072(3) 0.050(3) -0.025(3) -0.002(2) -0.017(2) C25 0.041(2) 0.089(4) 0.028(2) -0.004(2) -0.0055(19) -0.022(2) C26 0.041(2) 0.065(3) 0.029(2) 0.002(2) -0.0031(18) -0.015(2) C31 0.031(2) 0.032(2) 0.028(2) 0.0021(16) 0.0007(16) 0.0005(16) C32 0.036(2) 0.039(2) 0.048(3) 0.004(2) -0.0092(19) -0.0010(18) C33 0.047(3) 0.050(3) 0.063(3) 0.011(2) -0.017(2) 0.007(2) C34 0.056(3) 0.038(2) 0.050(3) 0.010(2) 0.001(2) 0.009(2) C35 0.053(3) 0.034(2) 0.045(3) 0.0021(19) 0.007(2) -0.005(2) C36 0.038(2) 0.037(2) 0.033(2) 0.0018(18) 0.0009(17) -0.0042(18) C41 0.0243(18) 0.0312(19) 0.039(2) -0.0025(17) 0.0000(17) -0.0024(16) C42 0.032(2) 0.054(3) 0.042(2) 0.001(2) 0.0050(19) -0.003(2) C43 0.035(2) 0.064(3) 0.060(3) -0.005(2) 0.013(2) -0.006(2) C44 0.025(2) 0.060(3) 0.078(4) -0.007(3) 0.001(2) 0.005(2) C45 0.031(2) 0.059(3) 0.068(3) 0.001(2) -0.015(2) 0.006(2) C46 0.033(2) 0.045(2) 0.043(3) 0.000(2) -0.0028(18) 0.0001(19) C51 0.0296(19) 0.032(2) 0.028(2) 0.0038(16) -0.0032(16) -0.0068(16) C52 0.031(2) 0.045(2) 0.037(2) 0.0028(19) -0.0017(18) -0.0065(19) C53 0.042(2) 0.057(3) 0.041(2) 0.008(2) -0.005(2) -0.024(2) C54 0.067(3) 0.046(3) 0.032(2) 0.000(2) -0.004(2) -0.023(2) C55 0.063(3) 0.037(2) 0.034(2) -0.0048(18) 0.006(2) -0.004(2) C56 0.038(2) 0.035(2) 0.031(2) -0.0008(17) 0.0035(17) -0.0042(18) C61 0.0234(18) 0.039(2) 0.030(2) 0.0009(17) -0.0006(15) -0.0013(16) C62 0.049(3) 0.042(2) 0.035(2) -0.0016(19) 0.0073(19) -0.013(2) C63 0.061(3) 0.050(3) 0.036(2) -0.008(2) 0.005(2) -0.016(2) C64 0.033(2) 0.062(3) 0.030(2) 0.002(2) 0.0004(18) -0.002(2) C65 0.043(2) 0.047(2) 0.033(2) 0.0084(19) 0.0021(18) -0.004(2) C66 0.039(2) 0.035(2) 0.038(2) 0.0009(18) 0.0021(18) -0.0059(18) O91 0.226(10) 0.145(6) 0.032(3) 0.000 0.000 0.121(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 Fe C2 1.940(4) 5_556 ? Fe C2 1.940(4) . ? Fe C1 1.944(4) . ? Fe C1 1.944(4) 5_556 ? Fe C3 1.950(4) . ? Fe C3 1.950(4) 5_556 ? C1 N1 1.154(5) . ? C2 N2 1.152(5) . ? C3 N3 1.161(5) . ? P1 C21 1.7853(19) 2_655 ? P1 C21 1.7853(19) . ? P1 C11 1.795(2) . ? P1 C11 1.795(2) 2_655 ? P2 C41 1.787(2) . ? P2 C31 1.7952(19) . ? P2 C51 1.7975(19) . ? P2 C61 1.799(2) . ? C11 C12 1.3900 . ? C11 C16 1.3900 . ? C12 C13 1.3900 . ? C13 C14 1.3900 . ? C14 C15 1.3900 . ? C15 C16 1.3900 . ? C21 C22 1.3900 . ? C21 C26 1.3900 . ? C22 C23 1.3900 . ? C23 C24 1.3900 . ? C24 C25 1.3900 . ? C25 C26 1.3900 . ? C31 C32 1.3900 . ? C31 C36 1.3900 . ? C32 C33 1.3900 . ? C33 C34 1.3900 . ? C34 C35 1.3900 . ? C35 C36 1.3900 . ? C41 C42 1.3900 . ? C41 C46 1.3900 . ? C42 C43 1.3900 . ? C43 C44 1.3900 . ? C44 C45 1.3900 . ? C45 C46 1.3900 . ? C51 C52 1.3900 . ? C51 C56 1.3900 . ? C52 C53 1.3900 . ? C53 C54 1.3900 . ? C54 C55 1.3900 . ? C55 C56 1.3900 . ? C61 C62 1.3900 . ? C61 C66 1.3900 . ? C62 C63 1.3900 . ? C63 C64 1.3900 . ? C64 C65 1.3900 . ? C65 C66 1.3900 . ? C71 C72 1.380(7) . ? C72 C73 1.488(7) . ? C73 C73 1.409(13) 2_465 ? C81 C82 1.450(10) . ? C82 C83 1.482(9) . ? C83 C84 1.470(9) . ? C84 O85 1.419(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Fe C2 180.000(1) 5_556 . ? C2 Fe C1 88.65(16) 5_556 . ? C2 Fe C1 91.35(16) . . ? C2 Fe C1 91.35(16) 5_556 5_556 ? C2 Fe C1 88.65(16) . 5_556 ? C1 Fe C1 180.0(2) . 5_556 ? C2 Fe C3 85.87(15) 5_556 . ? C2 Fe C3 94.13(15) . . ? C1 Fe C3 93.68(15) . . ? C1 Fe C3 86.32(15) 5_556 . ? C2 Fe C3 94.13(15) 5_556 5_556 ? C2 Fe C3 85.87(15) . 5_556 ? C1 Fe C3 86.32(15) . 5_556 ? C1 Fe C3 93.68(15) 5_556 5_556 ? C3 Fe C3 180.000(1) . 5_556 ? N1 C1 Fe 177.5(4) . . ? N2 C2 Fe 176.6(4) . . ? N3 C3 Fe 177.4(3) . . ? C21 P1 C21 110.13(18) 2_655 . ? C21 P1 C11 107.56(12) 2_655 . ? C21 P1 C11 110.26(12) . . ? C21 P1 C11 110.26(12) 2_655 2_655 ? C21 P1 C11 107.56(12) . 2_655 ? C11 P1 C11 111.09(18) . 2_655 ? C41 P2 C31 108.44(12) . . ? C41 P2 C51 108.23(12) . . ? C31 P2 C51 111.86(12) . . ? C41 P2 C61 106.97(13) . . ? C31 P2 C61 112.20(13) . . ? C51 P2 C61 108.94(12) . . ? C12 C11 C16 120.0 . . ? C12 C11 P1 121.52(15) . . ? C16 C11 P1 118.47(15) . . ? C11 C12 C13 120.0 . . ? C14 C13 C12 120.0 . . ? C13 C14 C15 120.0 . . ? C16 C15 C14 120.0 . . ? C15 C16 C11 120.0 . . ? C22 C21 C26 120.0 . . ? C22 C21 P1 119.23(14) . . ? C26 C21 P1 120.39(14) . . ? C23 C22 C21 120.0 . . ? C22 C23 C24 120.0 . . ? C25 C24 C23 120.0 . . ? C26 C25 C24 120.0 . . ? C25 C26 C21 120.0 . . ? C32 C31 C36 120.0 . . ? C32 C31 P2 121.22(13) . . ? C36 C31 P2 118.68(14) . . ? C33 C32 C31 120.0 . . ? C32 C33 C34 120.0 . . ? C33 C34 C35 120.0 . . ? C36 C35 C34 120.0 . . ? C35 C36 C31 120.0 . . ? C42 C41 C46 120.0 . . ? C42 C41 P2 120.62(14) . . ? C46 C41 P2 118.89(14) . . ? C43 C42 C41 120.0 . . ? C44 C43 C42 120.0 . . ? C43 C44 C45 120.0 . . ? C46 C45 C44 120.0 . . ? C45 C46 C41 120.0 . . ? C52 C51 C56 120.0 . . ? C52 C51 P2 120.94(13) . . ? C56 C51 P2 119.04(13) . . ? C51 C52 C53 120.0 . . ? C54 C53 C52 120.0 . . ? C53 C54 C55 120.0 . . ? C54 C55 C56 120.0 . . ? C55 C56 C51 120.0 . . ? C62 C61 C66 120.0 . . ? C62 C61 P2 119.00(13) . . ? C66 C61 P2 120.53(14) . . ? C63 C62 C61 120.0 . . ? C62 C63 C64 120.0 . . ? C63 C64 C65 120.0 . . ? C66 C65 C64 120.0 . . ? C65 C66 C61 120.0 . . ? C71 C72 C73 111.2(6) . . ? C73 C73 C72 114.9(8) 2_465 . ? C81 C82 C83 121.5(13) . . ? C84 C83 C82 126.7(13) . . ? O85 C84 C83 129.9(15) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.166 _refine_diff_density_min -0.712 _refine_diff_density_rms 0.074 data_DID117 _database_code_CSD 200410 _audit_creation_method 'RAELSPUB and manual entry' # TEXT _publ_section_abstract ? _publ_section_comment ? _publ_section_acknowledgements ? _publ_section_references ; Altomare, A., Burla, M.C., Camalli, M., Cascarano, G., Giacovazzo, C., Guagliardi, A., Polidori, G., J. Appl. Cryst., 1994, 27, 435. De Meulenaer, J. and Tompa, H. Acta Cryst., 1965, 19, 1014. Ibers, J.A. and Hamilton, W.C., (Eds) International Tables for X-Ray Crystallography Vol. 4 , Kynoch Press, Birmingham, 1974. Johnson, C.K.,'ORTEP-II', Oak Ridge National Laboratory, Tennessee, U.S.A., 1976. Rae, A.D., RAELS. A comprehensive Constrained Least Squares Refinement Program, University of New South Wales, 1989. ; _publ_section_figure_captions ? _publ_section_exptl_prep ? _publ_section_exptl_refinement ? _computing_data_collection 'CAD4 Version 5.0, 1989' _computing_cell_refinement 'CAD4 Version 5.0, 1989' _computing_data_reduction 'Local program' _computing_structure_solution 'SIR92 (Altomare et al, 1994)' _computing_structure_refinement 'RAELS, (Rae, 1989)' _computing_molecular_graphics 'ORTEP-II, (Johnson, 1976)' _computing_publication_material 'Local programs' # CHEMICAL DATA _chemical_name_systematic ? _chemical_formula_moiety 'C19 H18 P 1+,0.5(C5 Fe N6 O 2-),H2 O' _chemical_formula_sum 'C21.5 H20 Fe0.5 N3 O1.5 P1' _chemical_formula_iupac ? _chemical_formula_weight 403.3 # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,1/2+y,1/2-z 3 -x,-y,-z 4 x,1/2-y,1/2+z _cell_length_a 9.805(6) _cell_length_b 12.026(3) _cell_length_c 17.229(11) _cell_angle_alpha 90 _cell_angle_beta 90.27(3) _cell_angle_gamma 90 _cell_volume 2032(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 10 _cell_measurement_theta_min 12 _cell_measurement_theta_max 13 _cell_measurement_temperature 294 _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.08 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.32 _exptl_crystal_F_000 840.0 _exptl_absorpt_coefficient_mu 0.492 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details '(DeMeulenaer & Tompa, 1965)' _exptl_absorpt_correction_T_min 0.90 _exptl_absorpt_correction_T_max 0.97 # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'Nonius CAD-4' _diffrn_measurement_method \w--2\q _diffrn_reflns_number 3699 _diffrn_reflns_av_R_equivalents 0.010 _diffrn_reflns_theta_max 25 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_standards_number 1 _diffrn_standards_interval_time 30min _diffrn_standards_decay_% 0 # REFINEMENT DATA _refine_special_details ? _reflns_number_total 3569 _reflns_number_gt 2758 _reflns_threshold_expression I>2\s(I) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.041 _refine_ls_wR_factor_ref 0.057 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 2758 _refine_ls_number_parameters 147 _refine_ls_goodness_of_fit_ref 1.85 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(F) + 0.0004F^2^]' _refine_ls_shift/su_max 0.009 _refine_diff_density_max 0.31 _refine_diff_density_min -0.70 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _atom_type_scat_source 'International Tables for X-ray Crystallography, Vol. IV' # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_type_symbol _atom_type_description C/N 0.5C+0.5N N/O 0.5N+0.5O loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_type_symbol _atom_site_occupancy P 0.07819(6) 0.12070(5) 0.75423(3) 0.0407(2) Uani P 1.0 C1 0.18561(17) 0.23809(13) 0.77358(9) 0.0415(5) Uani C 1.0 C2 0.20905(17) 0.31309(15) 0.71377(9) 0.0484(4) Uani C 1.0 C3 0.2859(2) 0.4072(1) 0.7278(1) 0.0594(6) Uani C 1.0 C4 0.3389(2) 0.4266(2) 0.8007(1) 0.0651(6) Uani C 1.0 C5 0.3159(2) 0.3524(2) 0.8602(1) 0.0642(4) Uani C 1.0 C6 0.2393(2) 0.2580(1) 0.8470(1) 0.0517(4) Uani C 1.0 C7 -0.09054(17) 0.17220(15) 0.73692(9) 0.0431(6) Uani C 1.0 C8 -0.17884(18) 0.18539(16) 0.79908(9) 0.0568(6) Uani C 1.0 C9 -0.3068(2) 0.2299(2) 0.7867(1) 0.0714(9) Uani C 1.0 C10 -0.3467(2) 0.2610(2) 0.7131(1) 0.0716(8) Uani C 1.0 C11 -0.2595(2) 0.2481(2) 0.6513(1) 0.0694(6) Uani C 1.0 C12 -0.1312(2) 0.2037(2) 0.6628(1) 0.0557(6) Uani C 1.0 C13 0.1365(2) 0.0471(1) 0.6705(1) 0.0463(6) Uani C 1.0 C14 0.0487(2) -0.0279(2) 0.6347(1) 0.0603(6) Uani C 1.0 C15 0.0941(3) -0.0902(2) 0.5727(1) 0.0777(7) Uani C 1.0 C16 0.2257(2) -0.0780(2) 0.5465(1) 0.0814(9) Uani C 1.0 C17 0.3131(2) -0.0038(2) 0.5818(1) 0.079(1) Uani C 1.0 C18 0.2693(2) 0.0591(2) 0.6439(1) 0.0619(6) Uani C 1.0 C19 0.0772(3) 0.0274(2) 0.8348(2) 0.0556(7) Uani C 1.0 Fe 0.5000 0.5000 0.5000 0.0782(3) Uani Fe 1.0 C1Cy1 0.4615(3) 0.3487(3) 0.5215(2) 0.0675(8) Uani C 1.0 N1Cy1 0.4408(4) 0.2575(3) 0.5343(2) 0.102(1) Uani N 1.0 C1Cy2 0.3115(3) 0.5360(3) 0.5155(2) 0.0635(8) Uani C 1.0 N1Cy2 0.1989(3) 0.5562(3) 0.5228(2) 0.0866(9) Uani N 1.0 C/N 0.5376(2) 0.5246(2) 0.6028(2) 0.0588(7) Uani C/N 1.0 N/O 0.5643(2) 0.5397(2) 0.6664(1) 0.0763(7) Uani N/O 1.0 OW 0.0575(3) 0.3236(3) 0.5217(2) 0.1165(9) Uani O 1.0 HC2 0.1705 0.2990 0.6608 0.053 Uani H 1.0 HC3 0.3030 0.4614 0.6849 0.072 Uani H 1.0 HC4 0.3945 0.4949 0.8106 0.079 Uani H 1.0 HC5 0.3548 0.3671 0.9129 0.081 Uani H 1.0 HC6 0.2226 0.2041 0.8902 0.058 Uani H 1.0 HC8 -0.1498 0.1628 0.8525 0.069 Uani H 1.0 HC9 -0.3708 0.2396 0.8312 0.095 Uani H 1.0 HC10 -0.4396 0.2932 0.7044 0.088 Uani H 1.0 HC11 -0.2892 0.2709 0.5980 0.091 Uani H 1.0 HC12 -0.0678 0.1943 0.6179 0.068 Uani H 1.0 HC14 -0.0469 -0.0368 0.6538 0.073 Uani H 1.0 HC15 0.0313 -0.1443 0.5467 0.102 Uani H 1.0 HC16 0.2581 -0.1234 0.5015 0.102 Uani H 1.0 HC17 0.4086 0.0046 0.5624 0.106 Uani H 1.0 HC18 0.3326 0.1131 0.6695 0.075 Uani H 1.0 H1C19 0.0167 -0.0373 0.8227 0.076 Uani H 1.0 H2C19 0.1721 0.0004 0.8450 0.076 Uani H 1.0 H3C19 0.0423 0.0669 0.8817 0.076 Uani H 1.0 H1OW 0.1194 0.3895 0.5250 0.116 Uani H 1.0 H2OW -0.0364 0.3486 0.5069 0.116 Uani H 1.0 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol P 0.0448(4) 0.0379(3) 0.0395(3) -0.0006(3) -0.0002(2) 0.0031(3) P C1 0.0400(9) 0.0426(7) 0.0419(8) 0.0040(6) 0.0004(6) 0.0017(5) C C2 0.0482(8) 0.0455(7) 0.0514(7) 0.0003(6) 0.0042(7) 0.0068(6) C C3 0.055(1) 0.0480(7) 0.075(1) -0.0047(7) 0.0034(9) 0.0074(7) C C4 0.057(1) 0.0503(7) 0.088(1) -0.0059(7) -0.0081(9) -0.0022(7) C C5 0.065(1) 0.0557(9) 0.0716(9) -0.0049(8) -0.017(1) -0.0062(7) C C6 0.0550(9) 0.0507(7) 0.0494(8) 0.0001(6) -0.0098(7) -0.0017(6) C C7 0.0487(7) 0.035(1) 0.0456(8) -0.0016(6) 0.0019(5) 0.0006(7) C C8 0.0526(7) 0.059(1) 0.0585(8) 0.0054(7) 0.0107(6) 0.0007(8) C C9 0.0538(7) 0.074(1) 0.087(1) 0.0111(7) 0.0105(7) -0.002(1) C C10 0.0548(7) 0.061(1) 0.099(1) 0.0093(7) -0.0076(7) -0.001(1) C C11 0.0646(8) 0.066(1) 0.077(1) 0.0103(8) -0.0159(8) 0.006(1) C C12 0.0599(7) 0.055(1) 0.0520(8) 0.0052(7) -0.0066(6) 0.0053(8) C C13 0.0539(9) 0.0391(9) 0.0458(8) 0.0018(7) -0.0022(7) 0.0017(7) C C14 0.0722(9) 0.052(1) 0.0571(9) -0.0049(8) -0.0050(7) -0.0114(7) C C15 0.104(2) 0.065(1) 0.064(1) 0.001(1) -0.003(1) -0.0214(9) C C16 0.109(2) 0.073(1) 0.062(1) 0.018(1) 0.009(1) -0.015(1) C C17 0.083(1) 0.086(2) 0.069(1) 0.013(1) 0.019(1) -0.0110(9) C C18 0.0597(9) 0.065(1) 0.0610(9) 0.0022(7) 0.0099(8) -0.0048(7) C C19 0.061(2) 0.051(2) 0.054(2) -0.004(1) -0.003(1) 0.015(1) C Fe 0.0426(3) 0.0807(5) 0.1111(6) -0.0121(3) -0.0075(3) 0.0273(4) Fe C1Cy1 0.069(2) 0.079(2) 0.055(2) -0.024(2) -0.016(1) 0.011(2) C N1Cy1 0.136(3) 0.083(2) 0.086(2) -0.047(2) -0.029(2) 0.019(2) N C1Cy2 0.053(2) 0.089(2) 0.049(2) -0.013(2) -0.006(1) 0.003(2) C N1Cy2 0.057(2) 0.137(3) 0.066(2) -0.004(2) 0.000(1) -0.016(2) N C/N 0.048(1) 0.073(2) 0.056(2) -0.016(1) -0.007(1) 0.011(1) C N/O 0.068(2) 0.095(2) 0.065(2) -0.018(1) -0.007(1) 0.008(1) N OW 0.125(2) 0.126(2) 0.099(2) -0.040(2) 0.012(2) -0.002(2) O # MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag P C1 1.792(2) 1_555 1_555 no P C7 1.790(2) 1_555 1_555 no P C13 1.789(2) 1_555 1_555 no P C19 1.785(3) 1_555 1_555 no C1 C2 1.389(1) 1_555 1_555 no C1 C6 1.389(1) 1_555 1_555 no C2 C3 1.380(2) 1_555 1_555 no C3 C4 1.377(2) 1_555 1_555 no C4 C5 1.377(2) 1_555 1_555 no C5 C6 1.380(2) 1_555 1_555 no Fe C1Cy1 1.895(3) 1_555 1_555 no Fe C1Cy1 1.895(3) 1_555 3_666 no Fe C1Cy2 1.919(3) 1_555 1_555 no Fe C1Cy2 1.919(3) 1_555 3_666 no Fe C/N 1.831(3) 1_555 1_555 no Fe C/N 1.831(3) 1_555 3_666 no C1Cy1 N1Cy1 1.137(4) 1_555 1_555 no C1Cy2 N1Cy2 1.137(4) 1_555 1_555 no C/N N/O 1.140(3) 1_555 1_555 no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 P C7 107.48(8) 1_555 1_555 1_555 no C1 P C13 110.49(8) 1_555 1_555 1_555 no C1 P C19 110.8(1) 1_555 1_555 1_555 no C7 P C13 109.61(8) 1_555 1_555 1_555 no C7 P C19 109.8(1) 1_555 1_555 1_555 no C13 P C19 108.6(1) 1_555 1_555 1_555 no P C1 C2 118.2(1) 1_555 1_555 1_555 no P C1 C6 121.7(1) 1_555 1_555 1_555 no C2 C1 C6 120.0(1) 1_555 1_555 1_555 no C1 C2 C3 119.6(1) 1_555 1_555 1_555 no C2 C3 C4 120.1(1) 1_555 1_555 1_555 no C3 C4 C5 120.4(2) 1_555 1_555 1_555 no C4 C5 C6 120.1(1) 1_555 1_555 1_555 no C1 C6 C5 119.6(1) 1_555 1_555 1_555 no P C7 C8 119.3(1) 1_555 1_555 1_555 no P C7 C12 120.6(1) 1_555 1_555 1_555 no P C13 C14 118.7(1) 1_555 1_555 1_555 no P C13 C18 121.2(1) 1_555 1_555 1_555 no C1Cy1 Fe C1Cy1 180.0(2) 1_555 1_555 3_666 no C1Cy1 Fe C1Cy2 89.8(1) 1_555 1_555 1_555 no C1Cy1 Fe C1Cy2 90.2(1) 1_555 1_555 3_666 no C1Cy1 Fe C/N 90.3(1) 1_555 1_555 1_555 no C1Cy1 Fe C/N 89.7(1) 1_555 1_555 3_666 no C1Cy2 Fe C1Cy2 180.0(3) 1_555 1_555 3_666 no C1Cy2 Fe C/N 91.0(1) 1_555 1_555 1_555 no C1Cy2 Fe C/N 89.0(1) 1_555 1_555 3_666 no C/N Fe C/N 180.0(2) 1_555 1_555 3_666 no Fe C1Cy1 N1Cy1 178.8(4) 1_555 1_555 1_555 no Fe C1Cy2 N1Cy2 178.1(3) 1_555 1_555 1_555 no Fe C/N N/O 178.3(3) 1_555 1_555 1_555 no data_DID112 _database_code_CSD 200411 _audit_creation_method 'RAELSPUB and manual entry' # TEXT _publ_section_abstract ? _publ_section_comment ? _publ_section_acknowledgements ? _publ_section_references ; Altomare, A., Burla, M.C., Camalli, M., Cascarano, G., Giacovazzo, C., Guagliardi, A., Polidori, G., J. Appl. Cryst., 1994, 27, 435. De Meulenaer, J. and Tompa, H. Acta Cryst., 1965, 19, 1014. Ibers, J.A. and Hamilton, W.C., (Eds) International Tables for X-Ray Crystallography Vol. 4 , Kynoch Press, Birmingham, 1974. Johnson, C.K.,'ORTEP-II', Oak Ridge National Laboratory, Tennessee, U.S.A., 1976. Rae, A.D., RAELS. A comprehensive Constrained Least Squares Refinement Program, University of New South Wales, 1989. ; _publ_section_figure_captions ? _publ_section_exptl_prep ? _publ_section_exptl_refinement ? _computing_data_collection 'CAD4 Version 5.0, 1989' _computing_cell_refinement 'CAD4 Version 5.0, 1989' _computing_data_reduction 'Local program' _computing_structure_solution 'SIR92 (Altomare et al, 1994)' _computing_structure_refinement 'RAELS, (Rae, 1989)' _computing_molecular_graphics 'ORTEP-II, (Johnson, 1976)' _computing_publication_material 'Local programs' # CHEMICAL DATA _chemical_name_systematic ? _chemical_formula_moiety '2(C24 H20 P 1+),C5 Fe N6 O 2-' _chemical_formula_sum 'C53 H40 Fe1 N6 O1 P2' _chemical_formula_iupac ? _chemical_formula_weight 894.7 # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,1/2+y,1/2-z 3 -x,-y,-z 4 x,1/2-y,1/2+z _cell_length_a 8.993(7) _cell_length_b 21.378(8) _cell_length_c 24.324(18) _cell_angle_alpha 90 _cell_angle_beta 104.57(3) _cell_angle_gamma 90 _cell_volume 4526(4) _cell_formula_units_Z 4 _cell_measurement_reflns_used 10 _cell_measurement_theta_min 10 _cell_measurement_theta_max 11 _cell_measurement_temperature 294 _exptl_crystal_description multifacetted _exptl_crystal_colour brown _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.17 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.31 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1856.0 _exptl_absorpt_coefficient_mu 0.445 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details '(DeMeulenaer & Tompa, 1965)' _exptl_absorpt_correction_T_min 0.92 _exptl_absorpt_correction_T_max 0.95 # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'Nonius CAD-4' _diffrn_measurement_method \w--2\q _diffrn_reflns_number 6054 _diffrn_reflns_av_R_equivalents 0.009 _diffrn_reflns_theta_max 23 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 26 _diffrn_standards_number 1 _diffrn_standards_interval_time 30min _diffrn_standards_decay_% 0 # REFINEMENT DATA _refine_special_details ? _reflns_number_total 5892 _reflns_number_gt 4598 _reflns_threshold_expression I>2\s(I) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.033 _refine_ls_wR_factor_ref 0.045 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 4598 _refine_ls_number_parameters 285 _refine_ls_goodness_of_fit_ref 1.49 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(F) + 0.0004F^2^]' _refine_ls_shift/su_max 0.013 _refine_diff_density_max 0.35 _refine_diff_density_min -0.34 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _atom_type_scat_source 'International Tables for X-ray Crystallography, Vol. IV' # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_type_symbol _atom_site_occupancy P1A 0.62862(8) 0.37622(3) 0.54969(3) 0.0365(2) Uani P 1.0 C1A 0.75152(21) 0.44101(8) 0.57978(7) 0.0416(7) Uani C 1.0 C2A 0.79633(23) 0.48600(10) 0.54603(7) 0.0509(6) Uani C 1.0 C3A 0.88921(24) 0.53494(9) 0.57140(10) 0.0601(9) Uani C 1.0 C4A 0.93673(23) 0.53903(9) 0.62945(10) 0.0630(8) Uani C 1.0 C5A 0.89280(24) 0.49471(11) 0.66298(7) 0.0665(7) Uani C 1.0 C6A 0.79996(24) 0.44537(9) 0.63854(8) 0.0545(7) Uani C 1.0 C7A 0.45708(19) 0.38099(8) 0.57420(8) 0.0379(7) Uani C 1.0 C8A 0.41127(22) 0.43743(8) 0.59295(9) 0.0531(8) Uani C 1.0 C9A 0.27485(25) 0.44043(9) 0.60932(10) 0.067(1) Uani C 1.0 C10A 0.1854(2) 0.3881(1) 0.6071(1) 0.0663(9) Uani C 1.0 C11A 0.2301(2) 0.3322(1) 0.5886(1) 0.0682(8) Uani C 1.0 C12A 0.36612(23) 0.32811(8) 0.57199(9) 0.0537(7) Uani C 1.0 C13A 0.71993(22) 0.30273(8) 0.57279(7) 0.0380(8) Uani C 1.0 C14A 0.74379(26) 0.28585(9) 0.62947(7) 0.0553(8) Uani C 1.0 C15A 0.80921(28) 0.22848(10) 0.64752(7) 0.069(1) Uani C 1.0 C16A 0.85026(27) 0.18852(9) 0.60974(8) 0.062(1) Uani C 1.0 C17A 0.82695(27) 0.20497(9) 0.55372(8) 0.0620(9) Uani C 1.0 C18A 0.76170(25) 0.26210(9) 0.53472(6) 0.0515(8) Uani C 1.0 C19A 0.58057(20) 0.37893(9) 0.47345(6) 0.0419(9) Uani C 1.0 C20A 0.42840(20) 0.37317(10) 0.44292(8) 0.0546(9) Uani C 1.0 C21A 0.39251(21) 0.37470(11) 0.38420(8) 0.070(1) Uani C 1.0 C22A 0.50631(26) 0.38184(11) 0.35630(7) 0.068(1) Uani C 1.0 C23A 0.65678(25) 0.38755(10) 0.38625(8) 0.059(1) Uani C 1.0 C24A 0.69535(18) 0.38615(10) 0.44499(8) 0.0480(8) Uani C 1.0 P1B 0.32168(8) 0.07944(3) 0.63319(3) 0.0339(2) Uani P 1.0 C1B 0.14275(17) 0.03884(8) 0.61998(7) 0.0356(7) Uani C 1.0 C2B 0.03163(21) 0.04556(8) 0.56912(7) 0.0416(7) Uani C 1.0 C3B -0.10667(19) 0.01421(10) 0.56133(8) 0.0514(8) Uani C 1.0 C4B -0.13393(19) -0.02325(9) 0.60351(9) 0.056(1) Uani C 1.0 C5B -0.02456(23) -0.03005(9) 0.65382(8) 0.054(1) Uani C 1.0 C6B 0.11457(20) 0.00085(9) 0.66255(7) 0.0434(7) Uani C 1.0 C7B 0.46935(19) 0.02736(8) 0.66975(7) 0.0371(6) Uani C 1.0 C8B 0.45904(19) -0.03594(8) 0.65657(8) 0.0459(6) Uani C 1.0 C9B 0.57228(24) -0.07629(7) 0.68542(9) 0.0569(5) Uani C 1.0 C10B 0.69387(21) -0.05396(9) 0.72674(9) 0.0610(8) Uani C 1.0 C11B 0.70459(19) 0.00852(10) 0.73992(8) 0.0622(8) Uani C 1.0 C12B 0.59270(22) 0.04972(7) 0.71163(8) 0.0494(5) Uani C 1.0 C13B 0.31686(21) 0.14759(8) 0.67575(8) 0.0385(6) Uani C 1.0 C14B 0.42474(22) 0.19449(9) 0.67746(9) 0.0519(6) Uani C 1.0 C15B 0.42463(24) 0.24646(8) 0.71133(10) 0.0642(6) Uani C 1.0 C16B 0.31879(25) 0.25166(9) 0.74301(9) 0.0613(7) Uani C 1.0 C17B 0.21199(23) 0.20547(10) 0.74147(9) 0.0589(7) Uani C 1.0 C18B 0.20995(20) 0.15309(9) 0.70790(9) 0.0487(5) Uani C 1.0 C19B 0.36235(20) 0.10563(8) 0.56858(7) 0.0360(8) Uani C 1.0 C20B 0.47930(21) 0.07880(9) 0.54861(8) 0.0498(8) Uani C 1.0 C21B 0.50700(23) 0.10017(11) 0.49843(8) 0.063(1) Uani C 1.0 C22B 0.41964(24) 0.14749(10) 0.46859(8) 0.059(1) Uani C 1.0 C23B 0.30400(23) 0.17415(9) 0.48812(8) 0.0536(9) Uani C 1.0 C24B 0.27425(20) 0.15353(9) 0.53820(8) 0.0437(7) Uani C 1.0 Fe 0.85512(4) 0.22378(2) 0.35590(2) 0.0361(1) Uani Fe 1.0 C1Cy1 0.8725(3) 0.1538(1) 0.4082(1) 0.0412(7) Uani C 1.0 N1Cy1 0.8674(3) 0.1152(1) 0.4402(1) 0.0572(7) Uani N 1.0 C1Cy2 0.9661(3) 0.2769(1) 0.4174(1) 0.0421(7) Uani C 1.0 N1Cy2 1.0319(3) 0.3098(1) 0.4521(1) 0.0628(8) Uani N 1.0 C1Cy3 0.7854(4) 0.1686(1) 0.2911(1) 0.0459(7) Uani C 1.0 N1Cy3 0.7425(3) 0.1366(1) 0.2527(1) 0.0639(8) Uani N 1.0 C1Cy4 1.0579(4) 0.2010(1) 0.3480(1) 0.0418(7) Uani C 1.0 N1Cy4 1.1764(3) 0.1874(1) 0.3429(1) 0.0605(8) Uani N 1.0 C1Cy5 0.8612(3) 0.2946(2) 0.3059(1) 0.0420(7) Uani C 1.0 N1Cy5 0.8622(3) 0.3387(1) 0.2797(1) 0.0589(7) Uani N 1.0 N1 0.6809(3) 0.2362(1) 0.3633(1) 0.0433(6) Uani N 1.0 O1 0.5591(3) 0.2393(1) 0.3696(1) 0.0715(7) Uani O 1.0 HC2A 0.7617 0.4831 0.5037 0.063 Uani H 1.0 HC3A 0.9218 0.5675 0.5473 0.076 Uani H 1.0 HC4A 1.0039 0.5746 0.6475 0.075 Uani H 1.0 HC5A 0.9280 0.4981 0.7053 0.089 Uani H 1.0 HC6A 0.7680 0.4131 0.6630 0.067 Uani H 1.0 HC8A 0.4764 0.4756 0.5946 0.071 Uani H 1.0 HC9A 0.2413 0.4809 0.6229 0.094 Uani H 1.0 HC10A 0.0870 0.3906 0.6190 0.083 Uani H 1.0 HC11A 0.1642 0.2943 0.5871 0.097 Uani H 1.0 HC12A 0.3987 0.2874 0.5585 0.071 Uani H 1.0 HC14A 0.7139 0.3150 0.6570 0.075 Uani H 1.0 HC15A 0.8267 0.2161 0.6883 0.100 Uani H 1.0 HC16A 0.8975 0.1471 0.6231 0.076 Uani H 1.0 HC17A 0.8572 0.1755 0.5265 0.086 Uani H 1.0 HC18A 0.7447 0.2741 0.4939 0.070 Uani H 1.0 HC20A 0.3454 0.3680 0.4632 0.062 Uani H 1.0 HC21A 0.2831 0.3706 0.3620 0.090 Uani H 1.0 HC22A 0.4794 0.3829 0.3138 0.084 Uani H 1.0 HC23A 0.7390 0.3927 0.3655 0.070 Uani H 1.0 HC24A 0.8051 0.3903 0.4668 0.053 Uani H 1.0 HC2B 0.0514 0.0729 0.5383 0.045 Uani H 1.0 HC3B -0.1871 0.0189 0.5248 0.061 Uani H 1.0 HC4B -0.2342 -0.0458 0.5975 0.068 Uani H 1.0 HC5B -0.0455 -0.0575 0.6843 0.068 Uani H 1.0 HC6B 0.1943 -0.0041 0.6992 0.048 Uani H 1.0 HC8B 0.3704 -0.0523 0.6264 0.055 Uani H 1.0 HC9B 0.5654 -0.1219 0.6761 0.073 Uani H 1.0 HC10B 0.7752 -0.0834 0.7474 0.075 Uani H 1.0 HC11B 0.7937 0.0244 0.7701 0.083 Uani H 1.0 HC12B 0.6006 0.0953 0.7213 0.060 Uani H 1.0 HC14B 0.5019 0.1907 0.6544 0.065 Uani H 1.0 HC15B 0.5021 0.2804 0.7127 0.088 Uani H 1.0 HC16B 0.3195 0.2894 0.7674 0.074 Uani H 1.0 HC17B 0.1353 0.2097 0.7647 0.077 Uani H 1.0 HC18B 0.1320 0.1194 0.7068 0.061 Uani H 1.0 HC20B 0.5430 0.0443 0.5703 0.062 Uani H 1.0 HC21B 0.5911 0.0810 0.4838 0.086 Uani H 1.0 HC22B 0.4404 0.1627 0.4323 0.072 Uani H 1.0 HC23B 0.2409 0.2086 0.4661 0.068 Uani H 1.0 HC24B 0.1899 0.1730 0.5524 0.053 Uani H 1.0 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol P1A 0.0372(4) 0.0367(4) 0.0358(4) 0.0043(3) 0.0097(3) -0.0003(3) P C1A 0.035(1) 0.0420(9) 0.047(1) 0.0048(8) 0.0088(8) 0.0014(7) C C2A 0.046(1) 0.045(1) 0.0633(8) -0.0011(8) 0.0163(9) 0.0043(8) C C3A 0.047(1) 0.046(1) 0.090(1) -0.0027(8) 0.021(1) -0.0027(9) C C4A 0.041(1) 0.052(1) 0.093(1) -0.0004(9) 0.012(1) -0.017(1) C C5A 0.058(1) 0.067(1) 0.0676(9) -0.006(1) 0.003(1) -0.017(1) C C6A 0.052(1) 0.058(1) 0.049(1) -0.0027(8) 0.0044(9) -0.0049(8) C C7A 0.0378(9) 0.040(1) 0.034(1) 0.0041(7) 0.0055(8) -0.0003(9) C C8A 0.0545(9) 0.0467(9) 0.063(1) 0.0092(7) 0.0239(9) -0.005(1) C C9A 0.061(1) 0.068(1) 0.079(2) 0.017(1) 0.034(1) -0.001(1) C C10A 0.0487(9) 0.086(2) 0.069(2) 0.0092(9) 0.025(1) 0.004(2) C C11A 0.052(1) 0.076(1) 0.083(2) -0.009(1) 0.029(1) -0.005(1) C C12A 0.0482(9) 0.0512(9) 0.065(1) -0.0071(8) 0.0206(9) -0.006(1) C C13A 0.036(1) 0.0431(9) 0.0337(9) 0.0041(8) 0.0069(9) -0.0021(7) C C14A 0.074(1) 0.0552(9) 0.0371(9) 0.0206(9) 0.0139(9) 0.0057(7) C C15A 0.097(2) 0.061(1) 0.0479(9) 0.030(1) 0.017(1) 0.0120(9) C C16A 0.075(2) 0.0517(9) 0.056(1) 0.021(1) 0.009(1) 0.0046(8) C C17A 0.078(2) 0.0531(9) 0.052(1) 0.025(1) 0.011(1) -0.0031(8) C C18A 0.063(1) 0.0506(9) 0.0404(8) 0.0177(9) 0.0115(9) -0.0035(7) C C19A 0.048(1) 0.038(2) 0.0411(7) 0.011(1) 0.0134(6) 0.0018(7) C C20A 0.0512(9) 0.064(1) 0.0454(7) 0.020(1) 0.0055(7) -0.0057(8) C C21A 0.075(1) 0.082(2) 0.0450(7) 0.033(1) 0.0011(8) -0.0069(9) C C22A 0.102(2) 0.061(2) 0.0412(7) 0.030(2) 0.0149(6) 0.0027(7) C C23A 0.095(1) 0.044(1) 0.0467(7) 0.010(1) 0.0309(8) 0.0030(9) C C24A 0.0642(9) 0.039(1) 0.0465(7) 0.005(1) 0.0250(7) 0.0007(8) C P1B 0.0350(4) 0.0337(4) 0.0326(4) 0.0003(3) 0.0079(3) -0.0022(3) P C1B 0.0351(7) 0.034(1) 0.0377(9) 0.0049(7) 0.0093(6) -0.0047(8) C C2B 0.0364(7) 0.040(1) 0.0445(9) 0.0054(7) 0.0034(7) -0.0075(7) C C3B 0.0366(7) 0.047(1) 0.066(1) 0.0027(7) 0.0040(7) -0.0138(9) C C4B 0.0405(8) 0.049(1) 0.082(2) -0.0037(8) 0.0177(7) -0.013(1) C C5B 0.0494(9) 0.049(1) 0.070(1) -0.0059(9) 0.0244(8) -0.004(1) C C6B 0.0444(8) 0.041(1) 0.0475(9) -0.0001(7) 0.0166(6) -0.0010(8) C C7B 0.0356(9) 0.0417(8) 0.034(1) -0.0002(7) 0.0094(7) -0.0001(7) C C8B 0.0426(9) 0.0399(9) 0.055(1) 0.0017(7) 0.0124(7) 0.0015(7) C C9B 0.051(1) 0.0477(8) 0.073(2) 0.0093(8) 0.0165(9) 0.0110(8) C C10B 0.052(1) 0.067(1) 0.062(1) 0.017(1) 0.0101(9) 0.015(1) C C11B 0.0498(9) 0.074(1) 0.054(1) 0.0136(9) -0.0041(8) 0.001(1) C C12B 0.0418(9) 0.0566(8) 0.043(1) 0.0044(7) -0.0009(7) -0.0050(8) C C13B 0.038(1) 0.0405(9) 0.036(1) 0.0010(7) 0.0067(9) -0.0028(8) C C14B 0.060(1) 0.0453(9) 0.053(1) -0.0118(8) 0.0185(9) -0.0108(8) C C15B 0.079(2) 0.0489(9) 0.066(2) -0.0132(9) 0.021(1) -0.0186(9) C C16B 0.068(2) 0.054(1) 0.058(1) 0.0046(9) 0.010(1) -0.020(1) C C17B 0.053(1) 0.067(1) 0.056(1) 0.0054(9) 0.013(1) -0.023(1) C C18B 0.043(1) 0.058(1) 0.047(1) 0.0001(7) 0.0135(8) -0.0141(8) C C19B 0.037(1) 0.032(1) 0.0372(8) -0.0017(9) 0.0065(7) -0.0013(7) C C20B 0.048(1) 0.059(1) 0.0459(8) 0.0089(8) 0.0173(8) 0.0045(8) C C21B 0.060(1) 0.083(2) 0.051(1) 0.007(1) 0.025(1) 0.0090(9) C C22B 0.064(2) 0.069(2) 0.0449(9) -0.008(1) 0.0166(9) 0.0085(9) C C23B 0.065(2) 0.050(1) 0.0444(9) -0.0023(9) 0.0106(8) 0.0102(9) C C24B 0.051(1) 0.037(1) 0.0416(8) 0.0024(7) 0.0080(7) 0.0051(7) C Fe 0.0414(3) 0.0343(2) 0.0328(2) 0.0050(2) 0.0100(2) 0.0016(2) Fe C1Cy1 0.051(2) 0.041(2) 0.033(2) 0.007(1) 0.013(1) -0.002(2) C N1Cy1 0.079(2) 0.049(2) 0.048(2) 0.010(2) 0.023(1) 0.007(1) N C1Cy2 0.045(2) 0.042(2) 0.039(2) 0.006(2) 0.011(1) 0.001(2) C N1Cy2 0.067(2) 0.059(2) 0.056(2) 0.003(2) 0.004(2) -0.011(2) N C1Cy3 0.058(2) 0.042(2) 0.038(2) 0.005(2) 0.012(2) 0.007(2) C N1Cy3 0.089(2) 0.056(2) 0.043(2) -0.004(2) 0.009(2) -0.007(2) N C1Cy4 0.052(2) 0.039(2) 0.037(2) 0.005(2) 0.015(2) 0.007(1) C N1Cy4 0.060(2) 0.067(2) 0.063(2) 0.017(2) 0.031(2) 0.018(2) N C1Cy5 0.047(2) 0.042(2) 0.037(2) 0.006(1) 0.010(1) -0.004(2) C N1Cy5 0.087(2) 0.043(2) 0.047(2) 0.007(2) 0.019(2) 0.008(1) N N1 0.046(2) 0.039(2) 0.045(2) 0.001(1) 0.013(1) 0.003(1) N O1 0.050(2) 0.070(2) 0.101(2) 0.003(1) 0.032(1) 0.006(1) O # MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1A C1A 1.808(2) 1_555 1_555 no P1A C7A 1.791(2) 1_555 1_555 no P1A C13A 1.796(2) 1_555 1_555 no P1A C19A 1.796(2) 1_555 1_555 no C1A C2A 1.388(1) 1_555 1_555 no C1A C6A 1.388(1) 1_555 1_555 no C2A C3A 1.383(1) 1_555 1_555 no C3A C4A 1.371(1) 1_555 1_555 no C4A C5A 1.371(1) 1_555 1_555 no C5A C6A 1.383(1) 1_555 1_555 no P1B C1B 1.785(2) 1_555 1_555 no P1B C7B 1.789(2) 1_555 1_555 no P1B C13B 1.794(2) 1_555 1_555 no P1B C19B 1.791(2) 1_555 1_555 no Fe C1Cy1 1.944(3) 1_555 1_555 no Fe C1Cy2 1.941(3) 1_555 1_555 no Fe C1Cy3 1.942(3) 1_555 1_555 no Fe C1Cy4 1.944(3) 1_555 1_555 no Fe C1Cy5 1.952(3) 1_555 1_555 no Fe N1 1.644(3) 1_555 1_555 no C1Cy1 N1Cy1 1.144(3) 1_555 1_555 no C1Cy2 N1Cy2 1.145(4) 1_555 1_555 no C1Cy3 N1Cy3 1.144(4) 1_555 1_555 no C1Cy4 N1Cy4 1.141(3) 1_555 1_555 no C1Cy5 N1Cy5 1.140(4) 1_555 1_555 no N1 O1 1.145(3) 1_555 1_555 no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1A P1A C7A 108.16(9) 1_555 1_555 1_555 no C1A P1A C13A 111.02(9) 1_555 1_555 1_555 no C1A P1A C19A 110.91(9) 1_555 1_555 1_555 no C7A P1A C13A 108.06(9) 1_555 1_555 1_555 no C7A P1A C19A 109.76(9) 1_555 1_555 1_555 no C13A P1A C19A 108.87(9) 1_555 1_555 1_555 no P1A C1A C2A 122.0(1) 1_555 1_555 1_555 no P1A C1A C6A 118.0(1) 1_555 1_555 1_555 no C2A C1A C6A 119.97(9) 1_555 1_555 1_555 no C1A C2A C3A 119.52(8) 1_555 1_555 1_555 no C2A C3A C4A 120.28(8) 1_555 1_555 1_555 no C3A C4A C5A 120.4(1) 1_555 1_555 1_555 no C4A C5A C6A 120.28(8) 1_555 1_555 1_555 no C1A C6A C5A 119.52(8) 1_555 1_555 1_555 no P1A C7A C8A 120.7(1) 1_555 1_555 1_555 no P1A C7A C12A 119.3(1) 1_555 1_555 1_555 no P1A C13A C14A 118.8(1) 1_555 1_555 1_555 no P1A C13A C18A 121.2(1) 1_555 1_555 1_555 no P1A C19A C20A 119.9(1) 1_555 1_555 1_555 no P1A C19A C24A 120.2(1) 1_555 1_555 1_555 no C1B P1B C7B 108.05(9) 1_555 1_555 1_555 no C1B P1B C13B 110.32(9) 1_555 1_555 1_555 no C1B P1B C19B 111.59(9) 1_555 1_555 1_555 no C7B P1B C13B 109.95(9) 1_555 1_555 1_555 no C7B P1B C19B 109.93(9) 1_555 1_555 1_555 no C13B P1B C19B 107.01(9) 1_555 1_555 1_555 no P1B C1B C2B 121.6(1) 1_555 1_555 1_555 no P1B C1B C6B 118.4(1) 1_555 1_555 1_555 no P1B C7B C8B 119.6(1) 1_555 1_555 1_555 no P1B C7B C12B 120.4(1) 1_555 1_555 1_555 no P1B C13B C14B 119.1(1) 1_555 1_555 1_555 no P1B C13B C18B 121.0(1) 1_555 1_555 1_555 no P1B C19B C20B 121.2(1) 1_555 1_555 1_555 no P1B C19B C24B 118.8(1) 1_555 1_555 1_555 no C1Cy1 Fe C1Cy2 90.3(1) 1_555 1_555 1_555 no C1Cy1 Fe C1Cy3 91.2(1) 1_555 1_555 1_555 no C1Cy1 Fe C1Cy4 87.1(1) 1_555 1_555 1_555 no C1Cy1 Fe C1Cy5 174.0(1) 1_555 1_555 1_555 no C1Cy1 Fe N1 88.5(1) 1_555 1_555 1_555 no C1Cy2 Fe C1Cy3 168.1(1) 1_555 1_555 1_555 no C1Cy2 Fe C1Cy4 84.8(1) 1_555 1_555 1_555 no C1Cy2 Fe C1Cy5 86.4(1) 1_555 1_555 1_555 no C1Cy2 Fe N1 98.1(1) 1_555 1_555 1_555 no C1Cy3 Fe C1Cy4 83.5(1) 1_555 1_555 1_555 no C1Cy3 Fe C1Cy5 91.1(1) 1_555 1_555 1_555 no C1Cy3 Fe N1 93.8(1) 1_555 1_555 1_555 no C1Cy4 Fe C1Cy5 87.6(1) 1_555 1_555 1_555 no C1Cy4 Fe N1 174.8(1) 1_555 1_555 1_555 no C1Cy5 Fe N1 96.9(1) 1_555 1_555 1_555 no Fe C1Cy1 N1Cy1 172.0(3) 1_555 1_555 1_555 no Fe C1Cy2 N1Cy2 177.4(3) 1_555 1_555 1_555 no Fe C1Cy3 N1Cy3 179.0(3) 1_555 1_555 1_555 no Fe C1Cy4 N1Cy4 179.4(3) 1_555 1_555 1_555 no Fe C1Cy5 N1Cy5 174.9(3) 1_555 1_555 1_555 no Fe N1 O1 173.9(2) 1_555 1_555 1_555 no data_00061b _database_code_CSD 200412 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety (Me2Ph2P)3[Fe(CN)6](H2O)2 _chemical_formula_sum 'C48 H52 Fe N6 O2 P3' _chemical_formula_weight 893.72 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 24.8172(4) _cell_length_b 9.1563(2) _cell_length_c 21.3197(4) _cell_angle_alpha 90.00 _cell_angle_beta 107.7030(10) _cell_angle_gamma 90.00 _cell_volume 4615.14(15) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.286 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1876 _exptl_absorpt_coefficient_mu 0.476 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.8289 _exptl_absorpt_correction_T_max 0.8985 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Nonius Kappa-CCD' _diffrn_measurement_method 'phi/omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 51650 _diffrn_reflns_av_R_equivalents 0.0510 _diffrn_reflns_av_sigmaI/netI 0.0646 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.58 _diffrn_reflns_theta_max 30.03 _reflns_number_total 13480 _reflns_number_gt 7763 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement 'Nonius DENZO' _computing_data_reduction 'Nonius DENZO' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0707P)^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 13480 _refine_ls_number_parameters 482 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0908 _refine_ls_R_factor_gt 0.0458 _refine_ls_wR_factor_ref 0.1374 _refine_ls_wR_factor_gt 0.1246 _refine_ls_goodness_of_fit_ref 0.978 _refine_ls_restrained_S_all 0.977 _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 Fe1 Fe 0.0000 0.62815(4) 0.7500 0.01678(9) Uani 1 2 d S . . C11 C -0.06908(8) 0.62866(19) 0.67597(9) 0.0208(4) Uani 1 1 d . . . N11 N -0.11149(7) 0.62908(18) 0.63467(8) 0.0292(4) Uani 1 1 d . . . C12 C -0.03486(7) 0.4759(2) 0.78870(9) 0.0207(4) Uani 1 1 d . . . N12 N -0.05689(7) 0.38504(18) 0.80919(8) 0.0287(4) Uani 1 1 d . . . C13 C -0.03488(7) 0.7829(2) 0.78672(9) 0.0201(4) Uani 1 1 d . . . N13 N -0.05597(7) 0.87824(17) 0.80539(9) 0.0279(4) Uani 1 1 d . . . Fe2 Fe -0.5000 -0.13738(4) -0.2500 0.01773(9) Uani 1 2 d S . . C21 C -0.42907(8) -0.14155(19) -0.17794(10) 0.0213(4) Uani 1 1 d . . . N21 N -0.38656(7) -0.14726(18) -0.13716(9) 0.0298(4) Uani 1 1 d . . . C22 C -0.46921(7) 0.0165(2) -0.29216(9) 0.0215(4) Uani 1 1 d . . . N22 N -0.45169(7) 0.11082(18) -0.31596(9) 0.0285(4) Uani 1 1 d . . . C23 C -0.46635(7) -0.2907(2) -0.28846(9) 0.0206(4) Uani 1 1 d . . . N23 N -0.44485(7) -0.38415(17) -0.30835(8) 0.0276(4) Uani 1 1 d . . . P1 P -0.407770(19) -0.58036(5) -0.07636(2) 0.01984(11) Uani 1 1 d . . . C1A C -0.33348(3) -0.54917(14) -0.06211(6) 0.0224(4) Uani 1 1 d G . . C1B C -0.29365(5) -0.60888(14) -0.00749(6) 0.0291(5) Uani 1 1 d G . . H1BA H -0.3055 -0.6690 0.0222 0.035 Uiso 1 1 calc R . . C1C C -0.23646(4) -0.58067(15) 0.00376(6) 0.0363(5) Uani 1 1 d G . . H1CA H -0.2092 -0.6215 0.0411 0.044 Uiso 1 1 calc R . . C1D C -0.21908(4) -0.49273(16) -0.03962(7) 0.0379(6) Uani 1 1 d G . . H1DA H -0.1800 -0.4734 -0.0319 0.046 Uiso 1 1 calc R . . C1E C -0.25890(5) -0.43301(15) -0.09425(7) 0.0382(6) Uani 1 1 d G . . H1EA H -0.2470 -0.3729 -0.1239 0.046 Uiso 1 1 calc R . . C1F C -0.31610(4) -0.46123(14) -0.10550(6) 0.0305(5) Uani 1 1 d G . . H1FA H -0.3433 -0.4204 -0.1428 0.037 Uiso 1 1 calc R . . C1G C -0.41661(5) -0.73435(10) -0.02876(5) 0.0204(4) Uani 1 1 d G . . C1H C -0.41629(5) -0.71751(10) 0.03615(6) 0.0279(4) Uani 1 1 d G . . H1HA H -0.4119 -0.6231 0.0556 0.033 Uiso 1 1 calc R . . C1I C -0.42241(6) -0.83874(14) 0.07264(5) 0.0324(5) Uani 1 1 d G . . H1IA H -0.4222 -0.8272 0.1170 0.039 Uiso 1 1 calc R . . C1J C -0.42886(5) -0.97681(11) 0.04421(6) 0.0291(5) Uani 1 1 d G . . H1JA H -0.4330 -1.0597 0.0691 0.035 Uiso 1 1 calc R . . C1K C -0.42919(5) -0.99364(10) -0.02070(6) 0.0295(5) Uani 1 1 d G . . H1KA H -0.4336 -1.0880 -0.0401 0.035 Uiso 1 1 calc R . . C1L C -0.42306(5) -0.87242(13) -0.05719(5) 0.0247(4) Uani 1 1 d G . . H1LA H -0.4233 -0.8839 -0.1015 0.030 Uiso 1 1 calc R . . C1M C -0.43964(8) -0.6128(2) -0.16226(9) 0.0245(4) Uani 1 1 d . . . H1MA H -0.4803 -0.6300 -0.1711 0.037 Uiso 1 1 calc R . . H1MB H -0.4222 -0.6988 -0.1755 0.037 Uiso 1 1 calc R . . H1MC H -0.4339 -0.5275 -0.1873 0.037 Uiso 1 1 calc R . . C1N C -0.43846(8) -0.4223(2) -0.05187(10) 0.0267(4) Uani 1 1 d . . . H1NA H -0.4209 -0.4052 -0.0047 0.040 Uiso 1 1 calc R . . H1NB H -0.4792 -0.4376 -0.0608 0.040 Uiso 1 1 calc R . . H1NC H -0.4321 -0.3373 -0.0767 0.040 Uiso 1 1 calc R . . P2 P -0.08884(2) 1.07516(5) 0.57525(2) 0.02144(12) Uani 1 1 d . . . C2A C -0.16284(3) 1.04428(14) 0.56376(6) 0.0236(4) Uani 1 1 d G . . C2B C -0.20428(5) 1.11765(13) 0.51523(6) 0.0284(5) Uani 1 1 d G . . H2BA H -0.1937 1.1852 0.4872 0.034 Uiso 1 1 calc R . . C2C C -0.26112(4) 1.09217(15) 0.50769(6) 0.0348(5) Uani 1 1 d G . . H2CA H -0.2894 1.1423 0.4745 0.042 Uiso 1 1 calc R . . C2D C -0.27652(4) 0.99332(16) 0.54867(7) 0.0371(6) Uani 1 1 d G . . H2DA H -0.3154 0.9759 0.5435 0.045 Uiso 1 1 calc R . . C2E C -0.23509(5) 0.91994(14) 0.59720(7) 0.0367(5) Uani 1 1 d G . . H2EA H -0.2456 0.8524 0.6252 0.044 Uiso 1 1 calc R . . C2F C -0.17825(5) 0.94542(14) 0.60474(6) 0.0303(5) Uani 1 1 d G . . H2FA H -0.1499 0.8953 0.6379 0.036 Uiso 1 1 calc R . . C2G C -0.08119(5) 1.22823(11) 0.52676(6) 0.0220(4) Uani 1 1 d G . . C2H C -0.08939(5) 1.21250(11) 0.45965(6) 0.0291(5) Uani 1 1 d G . . H2HA H -0.0978 1.1191 0.4396 0.035 Uiso 1 1 calc R . . C2I C -0.08537(6) 1.33336(14) 0.42187(5) 0.0333(5) Uani 1 1 d G . . H2IA H -0.0910 1.3226 0.3760 0.040 Uiso 1 1 calc R . . C2J C -0.07315(5) 1.46996(12) 0.45121(6) 0.0309(5) Uani 1 1 d G . . H2JA H -0.0704 1.5526 0.4254 0.037 Uiso 1 1 calc R . . C2K C -0.06494(5) 1.48569(10) 0.51832(6) 0.0294(5) Uani 1 1 d G . . H2KA H -0.0566 1.5791 0.5384 0.035 Uiso 1 1 calc R . . C2L C -0.06896(5) 1.36483(13) 0.55609(4) 0.0247(4) Uani 1 1 d G . . H2LA H -0.0633 1.3756 0.6020 0.030 Uiso 1 1 calc R . . C2M C -0.05543(8) 1.1100(2) 0.66062(9) 0.0273(4) Uani 1 1 d . . . H2MA H -0.0150 1.1271 0.6683 0.041 Uiso 1 1 calc R . . H2MB H -0.0605 1.0256 0.6865 0.041 Uiso 1 1 calc R . . H2MC H -0.0724 1.1966 0.6740 0.041 Uiso 1 1 calc R . . C2N C -0.05879(8) 0.9162(2) 0.55063(10) 0.0290(5) Uani 1 1 d . . . H2NA H -0.0773 0.8976 0.5037 0.043 Uiso 1 1 calc R . . H2NB H -0.0644 0.8320 0.5764 0.043 Uiso 1 1 calc R . . H2NC H -0.0182 0.9316 0.5583 0.043 Uiso 1 1 calc R . . P3 P -0.24679(2) 0.37872(6) -0.30364(3) 0.02703(13) Uani 1 1 d . . . C3A C -0.25999(5) 0.27231(14) -0.23987(6) 0.0276(5) Uani 1 1 d G . . C3B C -0.21726(4) 0.25515(15) -0.18057(7) 0.0393(6) Uani 1 1 d G . . H3BA H -0.1805 0.2927 -0.1757 0.047 Uiso 1 1 calc R . . C3C C -0.22828(6) 0.18304(16) -0.12842(5) 0.0490(7) Uani 1 1 d G . . H3CA H -0.1991 0.1713 -0.0879 0.059 Uiso 1 1 calc R . . C3D C -0.28203(7) 0.12811(15) -0.13555(6) 0.0456(6) Uani 1 1 d G . . H3DA H -0.2896 0.0788 -0.0999 0.055 Uiso 1 1 calc R . . C3E C -0.32476(5) 0.14527(14) -0.19485(7) 0.0342(5) Uani 1 1 d G . . H3EA H -0.3615 0.1077 -0.1997 0.041 Uiso 1 1 calc R . . C3F C -0.31374(4) 0.21737(14) -0.24701(5) 0.0292(5) Uani 1 1 d G . . H3FA H -0.3429 0.2291 -0.2875 0.035 Uiso 1 1 calc R . . C3G C -0.24703(5) 0.56647(11) -0.28126(7) 0.0268(4) Uani 1 1 d G . . C3H C -0.29786(4) 0.63080(14) -0.28163(7) 0.0310(5) Uani 1 1 d G . . H3HA H -0.3322 0.5775 -0.2972 0.037 Uiso 1 1 calc R . . C3I C -0.29845(4) 0.77315(14) -0.25920(8) 0.0381(6) Uani 1 1 d G . . H3IA H -0.3332 0.8171 -0.2595 0.046 Uiso 1 1 calc R . . C3J C -0.24822(5) 0.85118(11) -0.23641(7) 0.0370(5) Uani 1 1 d G . . H3JA H -0.2486 0.9485 -0.2211 0.044 Uiso 1 1 calc R . . C3K C -0.19739(4) 0.78685(13) -0.23604(7) 0.0350(5) Uani 1 1 d G . . H3KA H -0.1631 0.8402 -0.2205 0.042 Uiso 1 1 calc R . . C3L C -0.19680(4) 0.64450(14) -0.25847(7) 0.0305(5) Uani 1 1 d G . . H3LA H -0.1621 0.6005 -0.2582 0.037 Uiso 1 1 calc R . . C3M C -0.30044(8) 0.3447(2) -0.37932(10) 0.0348(5) Uani 1 1 d . . . H3MA H -0.3374 0.3714 -0.3749 0.052 Uiso 1 1 calc R . . H3MB H -0.3004 0.2409 -0.3904 0.052 Uiso 1 1 calc R . . H3MC H -0.2931 0.4032 -0.4143 0.052 Uiso 1 1 calc R . . C3N C -0.18047(8) 0.3306(2) -0.31392(12) 0.0380(6) Uani 1 1 d . . . H3NA H -0.1811 0.2275 -0.3265 0.057 Uiso 1 1 calc R . . H3NB H -0.1503 0.3465 -0.2725 0.057 Uiso 1 1 calc R . . H3NC H -0.1735 0.3914 -0.3485 0.057 Uiso 1 1 calc R . . O1 O -0.43100(7) -0.62852(15) -0.38409(8) 0.0312(3) Uani 1 1 d D . . H1A H -0.4338(10) -0.566(2) -0.3563(10) 0.047 Uiso 1 1 d D . . H1B H -0.4368(9) -0.702(2) -0.3655(11) 0.047 Uiso 1 1 d D . . O2 O -0.07629(8) 0.12374(16) 0.88250(8) 0.0392(4) Uani 1 1 d D . . H2A H -0.0760(11) 0.063(2) 0.8535(11) 0.059 Uiso 1 1 d D . . H2B H -0.0764(10) 0.199(2) 0.8600(12) 0.059 Uiso 1 1 d 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 Fe1 0.01762(18) 0.01598(19) 0.0166(2) 0.000 0.00496(14) 0.000 C11 0.0242(9) 0.0174(9) 0.0214(10) -0.0001(8) 0.0077(8) 0.0000(7) N11 0.0257(9) 0.0331(10) 0.0263(10) -0.0026(8) 0.0043(7) 0.0029(7) C12 0.0210(9) 0.0213(10) 0.0184(10) -0.0006(8) 0.0038(8) 0.0031(7) N12 0.0326(9) 0.0250(9) 0.0297(10) 0.0025(8) 0.0110(8) -0.0024(7) C13 0.0185(9) 0.0209(10) 0.0215(10) 0.0007(8) 0.0071(8) -0.0024(7) N13 0.0275(9) 0.0235(9) 0.0347(10) -0.0034(8) 0.0123(8) -0.0026(7) Fe2 0.02063(19) 0.01531(19) 0.0180(2) 0.000 0.00697(15) 0.000 C21 0.0283(10) 0.0150(9) 0.0226(10) -0.0008(8) 0.0107(8) 0.0001(7) N21 0.0315(9) 0.0293(10) 0.0272(10) -0.0018(8) 0.0069(8) 0.0025(7) C22 0.0226(9) 0.0218(10) 0.0204(10) -0.0009(8) 0.0072(8) 0.0018(8) N22 0.0338(9) 0.0240(9) 0.0301(10) 0.0021(8) 0.0133(8) -0.0005(7) C23 0.0206(9) 0.0202(10) 0.0220(10) -0.0004(8) 0.0077(8) -0.0035(7) N23 0.0299(9) 0.0232(9) 0.0310(10) -0.0031(8) 0.0113(8) -0.0021(7) P1 0.0197(2) 0.0188(3) 0.0207(3) -0.0002(2) 0.00556(19) 0.00094(19) C1A 0.0214(9) 0.0193(10) 0.0251(11) -0.0019(8) 0.0052(8) 0.0008(7) C1B 0.0268(10) 0.0292(11) 0.0293(12) -0.0007(9) 0.0057(9) 0.0019(8) C1C 0.0240(10) 0.0383(13) 0.0405(14) -0.0051(11) 0.0007(9) 0.0025(9) C1D 0.0214(10) 0.0355(13) 0.0564(16) -0.0124(11) 0.0112(10) -0.0045(9) C1E 0.0323(12) 0.0340(13) 0.0524(16) 0.0017(11) 0.0193(11) -0.0068(10) C1F 0.0280(10) 0.0287(11) 0.0360(13) 0.0031(9) 0.0117(9) -0.0010(9) C1G 0.0187(9) 0.0208(10) 0.0212(10) 0.0006(8) 0.0052(7) 0.0004(7) C1H 0.0357(11) 0.0255(11) 0.0244(11) -0.0057(9) 0.0121(9) -0.0007(9) C1I 0.0394(12) 0.0362(12) 0.0269(12) 0.0008(10) 0.0178(9) 0.0019(10) C1J 0.0294(10) 0.0280(11) 0.0339(13) 0.0075(9) 0.0156(9) 0.0009(9) C1K 0.0348(11) 0.0208(10) 0.0348(13) -0.0021(9) 0.0132(9) -0.0034(9) C1L 0.0301(10) 0.0224(10) 0.0232(11) -0.0027(8) 0.0106(8) -0.0013(8) C1M 0.0226(9) 0.0295(11) 0.0200(10) 0.0008(8) 0.0042(8) 0.0017(8) C1N 0.0297(10) 0.0210(10) 0.0297(12) -0.0012(8) 0.0092(9) 0.0050(8) P2 0.0229(2) 0.0202(3) 0.0213(3) -0.0002(2) 0.0068(2) 0.00280(19) C2A 0.0241(9) 0.0216(10) 0.0256(11) -0.0036(8) 0.0083(8) 0.0007(8) C2B 0.0286(10) 0.0280(11) 0.0273(11) -0.0019(9) 0.0067(9) 0.0017(8) C2C 0.0254(11) 0.0389(13) 0.0358(13) -0.0060(10) 0.0029(9) 0.0051(9) C2D 0.0270(11) 0.0418(14) 0.0448(15) -0.0163(11) 0.0140(10) -0.0060(10) C2E 0.0368(12) 0.0347(13) 0.0421(14) -0.0049(11) 0.0171(10) -0.0083(10) C2F 0.0306(11) 0.0256(11) 0.0347(13) -0.0001(9) 0.0098(9) -0.0023(9) C2G 0.0215(9) 0.0219(10) 0.0225(10) -0.0003(8) 0.0068(8) 0.0013(7) C2H 0.0372(11) 0.0270(11) 0.0248(11) -0.0055(9) 0.0116(9) 0.0005(9) C2I 0.0412(12) 0.0381(13) 0.0252(12) 0.0003(10) 0.0167(9) 0.0020(10) C2J 0.0307(11) 0.0319(12) 0.0355(13) 0.0089(10) 0.0181(9) 0.0041(9) C2K 0.0297(11) 0.0234(11) 0.0366(13) -0.0015(9) 0.0123(9) -0.0031(8) C2L 0.0247(10) 0.0243(11) 0.0245(11) -0.0018(8) 0.0068(8) -0.0011(8) C2M 0.0244(10) 0.0330(12) 0.0235(11) 0.0012(9) 0.0058(8) 0.0033(8) C2N 0.0313(11) 0.0243(11) 0.0329(12) 0.0011(9) 0.0121(9) 0.0076(8) P3 0.0254(3) 0.0253(3) 0.0322(3) -0.0030(2) 0.0114(2) -0.0001(2) C3A 0.0309(11) 0.0213(10) 0.0284(12) -0.0034(9) 0.0058(9) 0.0043(8) C3B 0.0402(12) 0.0313(13) 0.0377(14) -0.0038(10) -0.0009(11) 0.0012(10) C3C 0.0695(18) 0.0382(14) 0.0278(14) 0.0001(11) -0.0021(12) 0.0068(13) C3D 0.0749(18) 0.0310(13) 0.0353(14) 0.0080(11) 0.0232(13) 0.0121(12) C3E 0.0421(12) 0.0280(12) 0.0387(14) 0.0043(10) 0.0214(10) 0.0074(9) C3F 0.0294(11) 0.0274(11) 0.0326(12) 0.0017(9) 0.0122(9) 0.0042(8) C3G 0.0251(10) 0.0261(11) 0.0305(12) 0.0015(9) 0.0104(8) 0.0005(8) C3H 0.0251(10) 0.0289(12) 0.0398(13) -0.0003(10) 0.0113(9) 0.0001(8) C3I 0.0313(11) 0.0411(14) 0.0453(15) 0.0033(11) 0.0169(10) 0.0095(10) C3J 0.0410(13) 0.0283(12) 0.0418(14) -0.0035(10) 0.0128(11) 0.0036(10) C3K 0.0304(11) 0.0352(13) 0.0394(14) 0.0003(10) 0.0105(10) -0.0048(9) C3L 0.0241(10) 0.0277(11) 0.0419(13) 0.0010(10) 0.0132(9) 0.0005(8) C3M 0.0400(12) 0.0388(13) 0.0269(12) -0.0026(10) 0.0118(10) -0.0073(10) C3N 0.0299(11) 0.0332(12) 0.0548(16) -0.0095(11) 0.0184(11) 0.0017(9) O1 0.0460(9) 0.0220(8) 0.0313(9) -0.0002(6) 0.0203(7) -0.0002(7) O2 0.0651(11) 0.0259(9) 0.0346(10) 0.0013(7) 0.0270(8) 0.0009(8) _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 C13 1.9447(19) . ? Fe1 C13 1.9447(19) 2_556 ? Fe1 C11 1.9454(19) 2_556 ? Fe1 C11 1.9454(19) . ? Fe1 C12 1.9509(19) 2_556 ? Fe1 C12 1.951(2) . ? C11 N11 1.149(2) . ? C12 N12 1.152(2) . ? C13 N13 1.149(2) . ? Fe2 C23 1.9386(19) . ? Fe2 C23 1.9386(19) 2_454 ? Fe2 C22 1.9483(19) 2_454 ? Fe2 C22 1.9483(19) . ? Fe2 C21 1.9533(19) . ? Fe2 C21 1.9533(19) 2_454 ? C21 N21 1.146(2) . ? C22 N22 1.151(2) . ? C23 N23 1.155(2) . ? P1 C1M 1.7853(19) . ? P1 C1N 1.7858(18) . ? P1 C1G 1.7893 . ? P1 C1A 1.7980 . ? C1A C1B 1.3900 . ? C1A C1F 1.3900 . ? C1B C1C 1.3900 . ? C1C C1D 1.3900 . ? C1D C1E 1.3900 . ? C1E C1F 1.3900 . ? C1G C1H 1.3900 . ? C1G C1L 1.3900 . ? C1H C1I 1.3900 . ? C1I C1J 1.3900 . ? C1J C1K 1.3900 . ? C1K C1L 1.3900 . ? P2 C2M 1.785(2) . ? P2 C2N 1.7857(19) . ? P2 C2G 1.7857 . ? P2 C2A 1.7997 . ? C2A C2B 1.3900 . ? C2A C2F 1.3900 . ? C2B C2C 1.3900 . ? C2C C2D 1.3900 . ? C2D C2E 1.3900 . ? C2E C2F 1.3900 . ? C2G C2H 1.3900 . ? C2G C2L 1.3900 . ? C2H C2I 1.3900 . ? C2I C2J 1.3900 . ? C2J C2K 1.3900 . ? C2K C2L 1.3900 . ? P3 C3M 1.779(2) . ? P3 C3N 1.7804(19) . ? P3 C3A 1.7822(11) . ? P3 C3G 1.7846(11) . ? C3A C3B 1.3900 . ? C3A C3F 1.3900 . ? C3B C3C 1.3900 . ? C3C C3D 1.3900 . ? C3D C3E 1.3900 . ? C3E C3F 1.3900 . ? C3G C3H 1.3900 . ? C3G C3L 1.3900 . ? C3H C3I 1.3900 . ? C3I C3J 1.3900 . ? C3J C3K 1.3900 . ? C3K C3L 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 C13 Fe1 C13 86.46(11) . 2_556 ? C13 Fe1 C11 93.55(7) . 2_556 ? C13 Fe1 C11 86.25(7) 2_556 2_556 ? C13 Fe1 C11 86.25(7) . . ? C13 Fe1 C11 93.55(7) 2_556 . ? C11 Fe1 C11 179.72(11) 2_556 . ? C13 Fe1 C12 178.60(8) . 2_556 ? C13 Fe1 C12 92.37(7) 2_556 2_556 ? C11 Fe1 C12 87.14(7) 2_556 2_556 ? C11 Fe1 C12 93.06(7) . 2_556 ? C13 Fe1 C12 92.37(8) . . ? C13 Fe1 C12 178.60(8) 2_556 . ? C11 Fe1 C12 93.06(7) 2_556 . ? C11 Fe1 C12 87.14(7) . . ? C12 Fe1 C12 88.81(11) 2_556 . ? N11 C11 Fe1 176.29(17) . . ? N12 C12 Fe1 177.37(17) . . ? N13 C13 Fe1 176.44(17) . . ? C23 Fe2 C23 87.17(11) . 2_454 ? C23 Fe2 C22 177.40(7) . 2_454 ? C23 Fe2 C22 92.81(8) 2_454 2_454 ? C23 Fe2 C22 92.81(8) . . ? C23 Fe2 C22 177.40(7) 2_454 . ? C22 Fe2 C22 87.33(11) 2_454 . ? C23 Fe2 C21 85.26(7) . . ? C23 Fe2 C21 93.11(7) 2_454 . ? C22 Fe2 C21 92.14(7) 2_454 . ? C22 Fe2 C21 89.48(7) . . ? C23 Fe2 C21 93.11(7) . 2_454 ? C23 Fe2 C21 85.26(7) 2_454 2_454 ? C22 Fe2 C21 89.48(7) 2_454 2_454 ? C22 Fe2 C21 92.14(7) . 2_454 ? C21 Fe2 C21 177.76(10) . 2_454 ? N21 C21 Fe2 177.33(18) . . ? N22 C22 Fe2 177.77(18) . . ? N23 C23 Fe2 176.71(17) . . ? C1M P1 C1N 109.86(9) . . ? C1M P1 C1G 110.98(8) . . ? C1N P1 C1G 109.63(8) . . ? C1M P1 C1A 108.15(8) . . ? C1N P1 C1A 109.18(8) . . ? C1G P1 C1A 109.01(6) . . ? C1B C1A C1F 120.0 . . ? C1B C1A P1 120.69(7) . . ? C1F C1A P1 119.29(7) . . ? C1C C1B C1A 120.0 . . ? C1B C1C C1D 120.0 . . ? C1C C1D C1E 120.0 . . ? C1D C1E C1F 120.0 . . ? C1E C1F C1A 120.0 . . ? C1H C1G C1L 120.0 . . ? C1H C1G P1 120.85(7) . . ? C1L C1G P1 119.15(7) . . ? C1G C1H C1I 120.0 . . ? C1H C1I C1J 120.0 . . ? C1K C1J C1I 120.0 . . ? C1J C1K C1L 120.0 . . ? C1K C1L C1G 120.0 . . ? C2M P2 C2N 109.85(9) . . ? C2M P2 C2G 110.60(8) . . ? C2N P2 C2G 110.01(8) . . ? C2M P2 C2A 107.78(8) . . ? C2N P2 C2A 109.40(8) . . ? C2G P2 C2A 109.17(6) . . ? C2B C2A C2F 120.0 . . ? C2B C2A P2 121.24(7) . . ? C2F C2A P2 118.76(7) . . ? C2C C2B C2A 120.0 . . ? C2B C2C C2D 120.0 . . ? C2E C2D C2C 120.0 . . ? C2F C2E C2D 120.0 . . ? C2E C2F C2A 120.0 . . ? C2H C2G C2L 120.0 . . ? C2H C2G P2 120.43(7) . . ? C2L C2G P2 119.53(7) . . ? C2G C2H C2I 120.0 . . ? C2H C2I C2J 120.0 . . ? C2K C2J C2I 120.0 . . ? C2J C2K C2L 120.0 . . ? C2K C2L C2G 120.0 . . ? C3M P3 C3N 108.06(11) . . ? C3M P3 C3A 109.61(8) . . ? C3N P3 C3A 110.48(9) . . ? C3M P3 C3G 110.39(9) . . ? C3N P3 C3G 110.46(8) . . ? C3A P3 C3G 107.84(7) . . ? C3B C3A C3F 120.0 . . ? C3B C3A P3 119.29(8) . . ? C3F C3A P3 120.48(8) . . ? C3C C3B C3A 120.0 . . ? C3B C3C C3D 120.0 . . ? C3E C3D C3C 120.0 . . ? C3D C3E C3F 120.0 . . ? C3E C3F C3A 120.0 . . ? C3H C3G C3L 120.0 . . ? C3H C3G P3 118.92(7) . . ? C3L C3G P3 120.86(7) . . ? C3G C3H C3I 120.0 . . ? C3J C3I C3H 120.0 . . ? C3K C3J C3I 120.0 . . ? C3J C3K C3L 120.0 . . ? C3K C3L C3G 120.0 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.911 _refine_diff_density_min -0.449 _refine_diff_density_rms 0.069