Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Beer, P. D.' 'Bernhardt, P.' _publ_contact_author_name 'Dr P Bernhardt' _publ_contact_author_address ; Dr P Bernhardt Department of Chemistry University of Queensland Brisbane 4072 AUSTRALIA ; _publ_contact_author_email 'bernhardt@chemistry.uq.edu.au' data_pb65073 _database_code_CSD 156422 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H50 Fe2 N6' _chemical_formula_weight 654.50 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' _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 7.679(4) _cell_length_b 10.914(4) _cell_length_c 11.027(5) _cell_angle_alpha 115.07(3) _cell_angle_beta 100.90(4) _cell_angle_gamma 99.74(3) _cell_volume 789.0(6) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10 _cell_measurement_theta_max 14 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.377 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 348 _exptl_absorpt_coefficient_mu 0.953 _exptl_absorpt_correction_type '\y-scans' _exptl_absorpt_correction_T_min 0.5986 _exptl_absorpt_correction_T_max 0.8106 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CAD4' _diffrn_measurement_method '\w-2\q scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 7200 _diffrn_standards_decay_% 'less than 5%' _diffrn_reflns_number 2988 _diffrn_reflns_av_R_equivalents 0.0477 _diffrn_reflns_av_sigmaI/netI 0.0249 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 24.97 _reflns_number_total 2762 _reflns_number_gt 2428 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4' _computing_cell_refinement 'SET4 in CAD4' _computing_data_reduction 'XCAD4' _computing_structure_solution 'SHELXS' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON' _computing_publication_material 'WINGX' _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^)+(0.1061P)^2^+0.2383P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary PAtterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2762 _refine_ls_number_parameters 190 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0594 _refine_ls_R_factor_gt 0.0526 _refine_ls_wR_factor_ref 0.1456 _refine_ls_wR_factor_gt 0.1395 _refine_ls_goodness_of_fit_ref 1.109 _refine_ls_restrained_S_all 1.109 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.49990(5) 0.28077(4) 0.07162(4) 0.0303(2) Uani 1 1 d . . . C1A C 0.2491(4) 0.2804(3) 0.1125(3) 0.0331(7) Uani 1 1 d . . . C2A C 0.3104(4) 0.3933(3) 0.0841(4) 0.0381(7) Uani 1 1 d . . . H2AA H 0.3326 0.4886 0.1446 0.046 Uiso 1 1 calc R . . C3A C 0.3320(5) 0.3361(4) -0.0515(4) 0.0432(8) Uani 1 1 d . . . H3AA H 0.3704 0.3868 -0.0960 0.052 Uiso 1 1 calc R . . C4A C 0.2847(5) 0.1876(4) -0.1079(4) 0.0430(8) Uani 1 1 d . . . H4AA H 0.2869 0.1236 -0.1959 0.052 Uiso 1 1 calc R . . C5A C 0.2337(4) 0.1541(3) -0.0065(4) 0.0386(7) Uani 1 1 d . . . H5AA H 0.1963 0.0638 -0.0167 0.046 Uiso 1 1 calc R . . C1B C 0.7633(5) 0.3389(4) 0.0619(4) 0.0426(8) Uani 1 1 d . . . H1BB H 0.7981 0.3765 0.0057 0.051 Uiso 1 1 calc R . . C2B C 0.7093(5) 0.1934(4) 0.0238(4) 0.0458(8) Uani 1 1 d . . . H2BB H 0.7025 0.1191 -0.0614 0.055 Uiso 1 1 calc R . . C3B C 0.6676(5) 0.1820(4) 0.1391(4) 0.0433(8) Uani 1 1 d . . . H3BB H 0.6279 0.0986 0.1429 0.052 Uiso 1 1 calc R . . C4B C 0.6968(4) 0.3196(4) 0.2474(4) 0.0395(7) Uani 1 1 d . . . H4BB H 0.6805 0.3427 0.3351 0.047 Uiso 1 1 calc R . . C5B C 0.7553(4) 0.4163(4) 0.1990(4) 0.0390(7) Uani 1 1 d . . . H5BB H 0.7834 0.5139 0.2492 0.047 Uiso 1 1 calc R . . N1 N 0.0520(3) 0.2148(3) 0.5677(3) 0.0344(6) Uani 1 1 d . . . H1N H 0.0699 0.1346 0.5656 0.041 Uiso 1 1 d R . . N2 N 0.1291(3) -0.0580(3) 0.3183(3) 0.0343(6) Uani 1 1 d . . . H2N H 0.0993 -0.0587 0.2350 0.041 Uiso 1 1 d R . . N3 N 0.2507(4) 0.1823(3) 0.2746(3) 0.0341(6) Uani 1 1 d . . . H3N H 0.3612 0.1745 0.2612 0.041 Uiso 1 1 d R . . C1 C 0.1283(4) -0.2239(3) 0.4143(4) 0.0368(7) Uani 1 1 d . . . H1C H 0.1399 -0.3171 0.3945 0.044 Uiso 1 1 calc R . . H1D H 0.2236 -0.1557 0.5000 0.044 Uiso 1 1 calc R . . C2 C 0.0704(4) 0.2164(3) 0.4395(3) 0.0339(7) Uani 1 1 d . . . H2C H 0.0567 0.3048 0.4438 0.041 Uiso 1 1 calc R . . H2D H -0.0282 0.1408 0.3608 0.041 Uiso 1 1 calc R . . C3 C 0.2567(4) 0.1992(3) 0.4150(3) 0.0316(6) Uani 1 1 d . . . C4 C 0.2871(4) 0.0621(3) 0.4113(3) 0.0343(7) Uani 1 1 d . . . H4A H 0.3952 0.0459 0.3805 0.041 Uiso 1 1 calc R . . H4B H 0.3103 0.0720 0.5050 0.041 Uiso 1 1 calc R . . C5 C 0.1535(5) -0.1951(3) 0.2947(4) 0.0383(7) Uani 1 1 d . . . H5A H 0.2763 -0.1978 0.2857 0.046 Uiso 1 1 calc R . . H5B H 0.0644 -0.2681 0.2078 0.046 Uiso 1 1 calc R . . C6 C 0.4151(4) 0.3228(3) 0.5320(4) 0.0403(7) Uani 1 1 d . . . H6A H 0.3973 0.4096 0.5370 0.060 Uiso 1 1 calc R . . H6B H 0.5303 0.3129 0.5128 0.060 Uiso 1 1 calc R . . H6C H 0.4173 0.3235 0.6197 0.060 Uiso 1 1 calc R . . C7 C 0.2074(4) 0.2944(3) 0.2443(4) 0.0370(7) Uani 1 1 d . . . H7A H 0.2797 0.3855 0.3217 0.044 Uiso 1 1 calc R . . H7B H 0.0777 0.2890 0.2344 0.044 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 Fe1 0.0308(3) 0.0329(3) 0.0372(3) 0.0227(2) 0.0108(2) 0.0152(2) C1A 0.0262(14) 0.0372(16) 0.0470(17) 0.0289(14) 0.0074(13) 0.0147(12) C2A 0.0365(17) 0.0398(17) 0.0511(19) 0.0315(15) 0.0105(14) 0.0180(14) C3A 0.0421(18) 0.054(2) 0.050(2) 0.0399(17) 0.0096(15) 0.0172(16) C4A 0.0390(18) 0.0504(19) 0.0402(17) 0.0247(16) 0.0038(14) 0.0137(15) C5A 0.0328(16) 0.0381(17) 0.0495(18) 0.0270(15) 0.0068(14) 0.0094(13) C1B 0.0346(17) 0.053(2) 0.055(2) 0.0329(17) 0.0212(15) 0.0182(15) C2B 0.048(2) 0.0455(19) 0.053(2) 0.0238(16) 0.0227(16) 0.0264(16) C3B 0.0386(18) 0.0461(19) 0.060(2) 0.0345(17) 0.0160(16) 0.0216(15) C4B 0.0313(16) 0.0546(19) 0.0442(17) 0.0305(16) 0.0103(13) 0.0213(15) C5B 0.0310(16) 0.0379(16) 0.0481(18) 0.0199(15) 0.0089(13) 0.0135(13) N1 0.0310(13) 0.0415(14) 0.0472(15) 0.0304(12) 0.0163(11) 0.0187(11) N2 0.0335(13) 0.0391(14) 0.0427(14) 0.0273(12) 0.0128(11) 0.0168(11) N3 0.0342(13) 0.0391(14) 0.0472(15) 0.0299(12) 0.0189(11) 0.0203(11) C1 0.0382(17) 0.0381(16) 0.0522(18) 0.0298(15) 0.0204(14) 0.0232(14) C2 0.0298(15) 0.0391(16) 0.0454(17) 0.0275(14) 0.0128(13) 0.0174(13) C3 0.0270(14) 0.0355(15) 0.0434(17) 0.0255(13) 0.0121(12) 0.0148(12) C4 0.0276(15) 0.0431(17) 0.0480(17) 0.0315(15) 0.0122(13) 0.0194(13) C5 0.0392(17) 0.0389(16) 0.0499(18) 0.0248(15) 0.0231(15) 0.0206(14) C6 0.0329(17) 0.0413(17) 0.0485(18) 0.0225(15) 0.0104(14) 0.0124(14) C7 0.0357(17) 0.0417(17) 0.0516(19) 0.0316(15) 0.0184(14) 0.0219(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C3B 2.040(3) . ? Fe1 C3A 2.041(3) . ? Fe1 C4A 2.043(4) . ? Fe1 C2A 2.045(3) . ? Fe1 C2B 2.046(3) . ? Fe1 C5A 2.050(3) . ? Fe1 C4B 2.050(3) . ? Fe1 C1B 2.052(3) . ? Fe1 C5B 2.055(4) . ? Fe1 C1A 2.059(3) . ? C1A C5A 1.411(5) . ? C1A C2A 1.423(4) . ? C1A C7 1.497(5) . ? C2A C3A 1.411(5) . ? C3A C4A 1.416(5) . ? C4A C5A 1.415(5) . ? C1B C5B 1.405(5) . ? C1B C2B 1.419(5) . ? C2B C3B 1.418(5) . ? C3B C4B 1.413(5) . ? C4B C5B 1.417(5) . ? N1 C1 1.449(4) 2_556 ? N1 C2 1.454(4) . ? N2 C4 1.447(4) . ? N2 C5 1.458(4) . ? N3 C7 1.469(4) . ? N3 C3 1.470(4) . ? C1 N1 1.449(4) 2_556 ? C1 C5 1.518(5) . ? C2 C3 1.533(4) . ? C3 C6 1.530(4) . ? C3 C4 1.538(4) . ? 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 C3B Fe1 C3A 163.23(15) . . ? C3B Fe1 C4A 126.09(15) . . ? C3A Fe1 C4A 40.57(14) . . ? C3B Fe1 C2A 155.02(15) . . ? C3A Fe1 C2A 40.40(14) . . ? C4A Fe1 C2A 68.01(15) . . ? C3B Fe1 C2B 40.62(15) . . ? C3A Fe1 C2B 125.64(16) . . ? C4A Fe1 C2B 107.02(15) . . ? C2A Fe1 C2B 163.36(14) . . ? C3B Fe1 C5A 108.31(14) . . ? C3A Fe1 C5A 67.99(14) . . ? C4A Fe1 C5A 40.46(14) . . ? C2A Fe1 C5A 67.76(14) . . ? C2B Fe1 C5A 119.53(15) . . ? C3B Fe1 C4B 40.43(14) . . ? C3A Fe1 C4B 154.58(15) . . ? C4A Fe1 C4B 164.08(14) . . ? C2A Fe1 C4B 121.05(14) . . ? C2B Fe1 C4B 67.98(15) . . ? C5A Fe1 C4B 127.56(14) . . ? C3B Fe1 C1B 68.06(15) . . ? C3A Fe1 C1B 107.55(15) . . ? C4A Fe1 C1B 119.12(15) . . ? C2A Fe1 C1B 126.68(14) . . ? C2B Fe1 C1B 40.52(14) . . ? C5A Fe1 C1B 153.68(15) . . ? C4B Fe1 C1B 67.64(15) . . ? C3B Fe1 C5B 68.04(14) . . ? C3A Fe1 C5B 119.77(14) . . ? C4A Fe1 C5B 153.46(15) . . ? C2A Fe1 C5B 109.00(14) . . ? C2B Fe1 C5B 67.89(15) . . ? C5A Fe1 C5B 165.02(14) . . ? C4B Fe1 C5B 40.39(14) . . ? C1B Fe1 C5B 40.01(14) . . ? C3B Fe1 C1A 120.33(13) . . ? C3A Fe1 C1A 68.19(13) . . ? C4A Fe1 C1A 68.07(14) . . ? C2A Fe1 C1A 40.57(12) . . ? C2B Fe1 C1A 154.07(14) . . ? C5A Fe1 C1A 40.18(13) . . ? C4B Fe1 C1A 109.38(13) . . ? C1B Fe1 C1A 164.48(14) . . ? C5B Fe1 C1A 127.93(14) . . ? C5A C1A C2A 107.3(3) . . ? C5A C1A C7 126.8(3) . . ? C2A C1A C7 126.0(3) . . ? C5A C1A Fe1 69.55(19) . . ? C2A C1A Fe1 69.16(18) . . ? C7 C1A Fe1 126.9(2) . . ? C3A C2A C1A 108.4(3) . . ? C3A C2A Fe1 69.66(19) . . ? C1A C2A Fe1 70.26(17) . . ? C2A C3A C4A 107.9(3) . . ? C2A C3A Fe1 69.93(18) . . ? C4A C3A Fe1 69.77(19) . . ? C5A C4A C3A 107.8(3) . . ? C5A C4A Fe1 70.04(19) . . ? C3A C4A Fe1 69.66(19) . . ? C1A C5A C4A 108.6(3) . . ? C1A C5A Fe1 70.28(18) . . ? C4A C5A Fe1 69.50(19) . . ? C5B C1B C2B 108.4(3) . . ? C5B C1B Fe1 70.1(2) . . ? C2B C1B Fe1 69.5(2) . . ? C3B C2B C1B 107.6(3) . . ? C3B C2B Fe1 69.46(19) . . ? C1B C2B Fe1 69.97(19) . . ? C4B C3B C2B 107.9(3) . . ? C4B C3B Fe1 70.16(19) . . ? C2B C3B Fe1 69.9(2) . . ? C3B C4B C5B 108.1(3) . . ? C3B C4B Fe1 69.41(19) . . ? C5B C4B Fe1 70.01(19) . . ? C1B C5B C4B 108.0(3) . . ? C1B C5B Fe1 69.9(2) . . ? C4B C5B Fe1 69.60(19) . . ? C1 N1 C2 112.0(2) 2_556 . ? C4 N2 C5 115.8(2) . . ? C7 N3 C3 117.1(2) . . ? N1 C1 C5 110.0(3) 2_556 . ? N1 C2 C3 112.7(2) . . ? N3 C3 C6 113.6(3) . . ? N3 C3 C2 108.1(2) . . ? C6 C3 C2 110.5(3) . . ? N3 C3 C4 105.2(2) . . ? C6 C3 C4 108.3(3) . . ? C2 C3 C4 111.0(2) . . ? N2 C4 C3 111.8(2) . . ? N2 C5 C1 111.1(3) . . ? N3 C7 C1A 110.7(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.073 _refine_diff_density_min -1.417 _refine_diff_density_rms 0.117 #=END data_pb66076 _database_code_CSD 156423 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H56 Cl2 Fe2 N6 O2' _chemical_formula_weight 763.45 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' 'Cl' 'Cl' 0.1484 0.1585 '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 ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 14.967(5) _cell_length_b 7.4043(8) _cell_length_c 33.060(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.55(2) _cell_angle_gamma 90.00 _cell_volume 3663.5(17) _cell_formula_units_Z 4 _cell_measurement_temperature 569(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.50 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.384 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1616 _exptl_absorpt_coefficient_mu 0.977 _exptl_absorpt_correction_type '\y-scans' _exptl_absorpt_correction_T_min 0.5919 _exptl_absorpt_correction_T_max 0.6409 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 569(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 'CAD4' _diffrn_measurement_method '\w-2\q scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 7200 _diffrn_standards_decay_% 'less than 5%' _diffrn_reflns_number 3337 _diffrn_reflns_av_R_equivalents 0.0528 _diffrn_reflns_av_sigmaI/netI 0.0232 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 2.46 _diffrn_reflns_theta_max 24.98 _reflns_number_total 3204 _reflns_number_gt 2509 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4' _computing_cell_refinement 'SET4 in CAD4' _computing_data_reduction 'XCAD4' _computing_structure_solution 'SHELXS' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON' _computing_publication_material 'WINGX' _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^)+(0.0645P)^2^+5.5712P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3204 _refine_ls_number_parameters 208 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0576 _refine_ls_R_factor_gt 0.0386 _refine_ls_wR_factor_ref 0.1191 _refine_ls_wR_factor_gt 0.1033 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.36840(3) 0.34625(6) 0.196015(13) 0.03904(17) Uani 1 1 d . . . C1A C 0.4650(2) 0.4138(4) 0.15499(9) 0.0422(7) Uani 1 1 d . . . C2A C 0.3792(2) 0.4634(4) 0.14027(10) 0.0482(8) Uani 1 1 d . . . H2A H 0.3525 0.4233 0.1164 0.058 Uiso 1 1 calc R . . C3A C 0.3414(3) 0.5857(5) 0.16856(12) 0.0571(9) Uani 1 1 d . . . H3A H 0.2854 0.6393 0.1663 0.069 Uiso 1 1 calc R . . C4A C 0.4028(3) 0.6120(4) 0.20051(11) 0.0550(9) Uani 1 1 d . . . H4A H 0.3945 0.6856 0.2230 0.066 Uiso 1 1 calc R . . C5A C 0.4792(2) 0.5069(4) 0.19242(10) 0.0482(8) Uani 1 1 d . . . H5A H 0.5301 0.4993 0.2087 0.058 Uiso 1 1 calc R . . C1B C 0.3802(2) 0.1718(5) 0.24397(10) 0.0511(8) Uani 1 1 d . . . H1B H 0.4273 0.1660 0.2625 0.061 Uiso 1 1 calc R . . C2B C 0.3738(3) 0.0769(5) 0.20714(12) 0.0605(10) Uani 1 1 d . . . H2B H 0.4162 -0.0022 0.1969 0.073 Uiso 1 1 calc R . . C3B C 0.2924(3) 0.1221(6) 0.18860(11) 0.0683(12) Uani 1 1 d . . . H3B H 0.2712 0.0784 0.1640 0.082 Uiso 1 1 calc R . . C4B C 0.2483(2) 0.2461(6) 0.21399(12) 0.0620(10) Uani 1 1 d . . . H4B H 0.1927 0.2981 0.2091 0.074 Uiso 1 1 calc R . . C5B C 0.3027(2) 0.2766(5) 0.24768(10) 0.0510(8) Uani 1 1 d . . . H5B H 0.2898 0.3537 0.2691 0.061 Uiso 1 1 calc R . . N1 N 0.57571(14) 0.1320(3) 0.03807(7) 0.0363(5) Uani 1 1 d . . . H1A H 0.5397 0.2232 0.0455 0.044 Uiso 1 1 d R . . N2 N 0.43778(15) -0.1075(3) 0.05129(7) 0.0381(6) Uani 1 1 d . . . H2C H 0.4733 -0.0447 0.0346 0.046 Uiso 1 1 calc R . . H2D H 0.3933 -0.0338 0.0590 0.046 Uiso 1 1 calc R . . N3 N 0.48986(16) 0.1413(3) 0.11475(7) 0.0388(6) Uani 1 1 d . . . H3C H 0.4453 0.1000 0.1303 0.047 Uiso 1 1 d R . . C1 C 0.6432(2) 0.2002(5) 0.01030(10) 0.0453(8) Uani 1 1 d . . . H1D H 0.6861 0.1055 0.0048 0.054 Uiso 1 1 calc R . . H1E H 0.6749 0.3000 0.0229 0.054 Uiso 1 1 calc R . . C2 C 0.61752(19) 0.0530(4) 0.07401(9) 0.0408(7) Uani 1 1 d . . . H2E H 0.6565 0.1418 0.0866 0.049 Uiso 1 1 calc R . . H2F H 0.6540 -0.0490 0.0660 0.049 Uiso 1 1 calc R . . C3 C 0.54843(19) -0.0105(4) 0.10491(9) 0.0390(7) Uani 1 1 d . . . C4 C 0.4902(2) -0.1616(4) 0.08741(9) 0.0435(7) Uani 1 1 d . . . H4C H 0.5283 -0.2626 0.0803 0.052 Uiso 1 1 calc R . . H4D H 0.4495 -0.2026 0.1081 0.052 Uiso 1 1 calc R . . C5 C 0.3988(2) -0.2626(4) 0.02873(9) 0.0467(8) Uani 1 1 d . . . H5C H 0.3540 -0.3211 0.0452 0.056 Uiso 1 1 calc R . . H5D H 0.4452 -0.3501 0.0231 0.056 Uiso 1 1 calc R . . C6 C 0.5982(2) -0.0949(5) 0.14101(10) 0.0568(9) Uani 1 1 d . . . H6A H 0.6357 -0.0056 0.1536 0.085 Uiso 1 1 calc R . . H6B H 0.6342 -0.1937 0.1318 0.085 Uiso 1 1 calc R . . H6C H 0.5557 -0.1384 0.1603 0.085 Uiso 1 1 calc R . . C7 C 0.5323(2) 0.2940(5) 0.13539(10) 0.0481(8) Uani 1 1 d . . . H7A H 0.5662 0.3637 0.1160 0.058 Uiso 1 1 calc R . . H7B H 0.5736 0.2490 0.1558 0.058 Uiso 1 1 calc R . . Cl1 Cl 0.25364(6) 0.08623(17) 0.07172(3) 0.0742(3) Uani 1 1 d . . . O1 O 0.1213(2) 0.1951(4) -0.00426(11) 0.0924(10) Uani 1 1 d . . . H1 H 0.1517 0.1681 0.0145 0.111 Uiso 1 1 d R . . H2 H 0.1525 0.1964 -0.0261 0.111 Uiso 1 1 d 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 Fe1 0.0443(3) 0.0302(2) 0.0429(3) 0.00324(18) 0.01440(18) -0.00049(18) C1A 0.0471(17) 0.0377(16) 0.0422(16) 0.0042(13) 0.0157(13) -0.0062(14) C2A 0.0562(19) 0.0438(18) 0.0447(18) 0.0143(15) 0.0102(15) -0.0007(15) C3A 0.061(2) 0.0377(17) 0.073(2) 0.0164(17) 0.0197(18) 0.0071(16) C4A 0.071(2) 0.0294(16) 0.065(2) -0.0030(15) 0.0286(19) -0.0059(16) C5A 0.0555(19) 0.0365(17) 0.0528(19) -0.0063(14) 0.0142(15) -0.0097(15) C1B 0.0529(19) 0.0493(19) 0.0513(19) 0.0175(16) 0.0105(15) 0.0028(15) C2B 0.081(3) 0.0288(17) 0.073(2) 0.0087(16) 0.036(2) 0.0019(17) C3B 0.095(3) 0.064(3) 0.046(2) 0.0058(18) 0.007(2) -0.042(2) C4B 0.0453(18) 0.070(3) 0.070(3) 0.031(2) 0.0098(17) -0.0056(18) C5B 0.059(2) 0.0451(18) 0.049(2) 0.0043(15) 0.0242(16) -0.0003(16) N1 0.0279(11) 0.0412(14) 0.0400(13) -0.0044(11) 0.0100(10) -0.0035(10) N2 0.0354(12) 0.0364(13) 0.0428(13) -0.0003(11) 0.0090(10) -0.0078(10) N3 0.0353(12) 0.0425(14) 0.0386(13) -0.0023(11) 0.0099(10) -0.0023(11) C1 0.0363(15) 0.0513(19) 0.0485(18) -0.0082(15) 0.0112(13) -0.0197(14) C2 0.0317(14) 0.0479(18) 0.0428(16) -0.0058(14) 0.0048(12) -0.0001(13) C3 0.0375(15) 0.0416(17) 0.0380(16) 0.0012(13) 0.0026(12) 0.0004(13) C4 0.0492(17) 0.0383(16) 0.0432(17) 0.0040(14) 0.0053(13) -0.0036(14) C5 0.0498(18) 0.0424(18) 0.0482(19) -0.0044(14) 0.0101(14) -0.0198(15) C6 0.059(2) 0.059(2) 0.052(2) 0.0065(17) -0.0051(16) 0.0040(18) C7 0.0430(17) 0.0497(19) 0.0520(19) -0.0069(15) 0.0135(14) -0.0073(14) Cl1 0.0569(5) 0.0895(8) 0.0763(7) -0.0276(6) -0.0007(5) 0.0143(5) O1 0.0695(19) 0.080(2) 0.127(3) -0.007(2) -0.0125(18) -0.0019(16) _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 C3B 2.025(4) . ? Fe1 C2B 2.030(3) . ? Fe1 C3A 2.030(3) . ? Fe1 C4B 2.038(3) . ? Fe1 C4A 2.039(3) . ? Fe1 C2A 2.045(3) . ? Fe1 C5A 2.045(3) . ? Fe1 C5B 2.045(3) . ? Fe1 C1B 2.051(3) . ? Fe1 C1A 2.054(3) . ? Fe1 Fe1 14.518(4) 5_655 ? C1A C2A 1.417(5) . ? C1A C5A 1.430(4) . ? C1A C7 1.494(4) . ? C2A C3A 1.423(5) . ? C3A C4A 1.407(5) . ? C4A C5A 1.411(5) . ? C1B C5B 1.402(5) . ? C1B C2B 1.409(5) . ? C2B C3B 1.398(6) . ? C3B C4B 1.412(6) . ? C4B C5B 1.392(5) . ? N1 C2 1.460(4) . ? N1 C1 1.461(4) . ? N2 C4 1.478(4) . ? N2 C5 1.486(4) . ? N3 C7 1.462(4) . ? N3 C3 1.464(4) . ? C1 C5 1.502(5) 5_655 ? C2 C3 1.534(4) . ? C3 C4 1.528(4) . ? C3 C6 1.534(4) . ? C5 C1 1.502(5) 5_655 ? 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 C3B Fe1 C2B 40.34(17) . . ? C3B Fe1 C3A 123.53(18) . . ? C2B Fe1 C3A 161.15(17) . . ? C3B Fe1 C4B 40.66(17) . . ? C2B Fe1 C4B 67.85(16) . . ? C3A Fe1 C4B 106.02(15) . . ? C3B Fe1 C4A 160.16(18) . . ? C2B Fe1 C4A 157.77(18) . . ? C3A Fe1 C4A 40.44(15) . . ? C4B Fe1 C4A 123.55(16) . . ? C3B Fe1 C2A 106.73(15) . . ? C2B Fe1 C2A 125.23(15) . . ? C3A Fe1 C2A 40.88(14) . . ? C4B Fe1 C2A 119.66(15) . . ? C4A Fe1 C2A 68.53(15) . . ? C3B Fe1 C5A 157.54(17) . . ? C2B Fe1 C5A 123.47(15) . . ? C3A Fe1 C5A 67.92(15) . . ? C4B Fe1 C5A 161.16(16) . . ? C4A Fe1 C5A 40.42(14) . . ? C2A Fe1 C5A 68.25(14) . . ? C3B Fe1 C5B 67.71(15) . . ? C2B Fe1 C5B 67.63(14) . . ? C3A Fe1 C5B 119.89(14) . . ? C4B Fe1 C5B 39.87(15) . . ? C4A Fe1 C5B 107.79(14) . . ? C2A Fe1 C5B 154.51(14) . . ? C5A Fe1 C5B 126.28(14) . . ? C3B Fe1 C1B 67.76(16) . . ? C2B Fe1 C1B 40.38(15) . . ? C3A Fe1 C1B 155.58(15) . . ? C4B Fe1 C1B 67.36(14) . . ? C4A Fe1 C1B 122.12(16) . . ? C2A Fe1 C1B 163.09(14) . . ? C5A Fe1 C1B 110.33(15) . . ? C5B Fe1 C1B 40.02(13) . . ? C3B Fe1 C1A 121.18(15) . . ? C2B Fe1 C1A 109.40(13) . . ? C3A Fe1 C1A 68.31(14) . . ? C4B Fe1 C1A 155.44(15) . . ? C4A Fe1 C1A 68.54(13) . . ? C2A Fe1 C1A 40.45(13) . . ? C5A Fe1 C1A 40.85(13) . . ? C5B Fe1 C1A 163.77(14) . . ? C1B Fe1 C1A 127.44(13) . . ? C3B Fe1 Fe1 76.08(12) . 5_655 ? C2B Fe1 Fe1 78.70(10) . 5_655 ? C3A Fe1 Fe1 87.93(11) . 5_655 ? C4B Fe1 Fe1 112.29(13) . 5_655 ? C4A Fe1 Fe1 109.59(10) . 5_655 ? C2A Fe1 Fe1 47.21(10) . 5_655 ? C5A Fe1 Fe1 85.78(9) . 5_655 ? C5B Fe1 Fe1 142.50(10) . 5_655 ? C1B Fe1 Fe1 116.46(10) . 5_655 ? C1A Fe1 Fe1 45.39(9) . 5_655 ? C2A C1A C5A 107.4(3) . . ? C2A C1A C7 128.1(3) . . ? C5A C1A C7 124.5(3) . . ? C2A C1A Fe1 69.43(17) . . ? C5A C1A Fe1 69.24(17) . . ? C7 C1A Fe1 128.6(2) . . ? C1A C2A C3A 107.7(3) . . ? C1A C2A Fe1 70.12(17) . . ? C3A C2A Fe1 69.02(19) . . ? C4A C3A C2A 108.7(3) . . ? C4A C3A Fe1 70.1(2) . . ? C2A C3A Fe1 70.10(18) . . ? C3A C4A C5A 107.8(3) . . ? C3A C4A Fe1 69.45(19) . . ? C5A C4A Fe1 70.01(18) . . ? C4A C5A C1A 108.4(3) . . ? C4A C5A Fe1 69.57(19) . . ? C1A C5A Fe1 69.91(17) . . ? C5B C1B C2B 107.6(3) . . ? C5B C1B Fe1 69.75(19) . . ? C2B C1B Fe1 68.99(19) . . ? C3B C2B C1B 108.1(3) . . ? C3B C2B Fe1 69.7(2) . . ? C1B C2B Fe1 70.64(19) . . ? C2B C3B C4B 107.8(3) . . ? C2B C3B Fe1 70.0(2) . . ? C4B C3B Fe1 70.2(2) . . ? C5B C4B C3B 107.9(3) . . ? C5B C4B Fe1 70.32(19) . . ? C3B C4B Fe1 69.2(2) . . ? C4B C5B C1B 108.6(3) . . ? C4B C5B Fe1 69.82(19) . . ? C1B C5B Fe1 70.24(18) . . ? C2 N1 C1 110.9(2) . . ? C4 N2 C5 113.5(2) . . ? C7 N3 C3 116.1(2) . . ? N1 C1 C5 111.1(2) . 5_655 ? N1 C2 C3 112.2(2) . . ? N3 C3 C4 107.8(2) . . ? N3 C3 C6 115.3(3) . . ? C4 C3 C6 105.5(3) . . ? N3 C3 C2 108.8(2) . . ? C4 C3 C2 110.9(2) . . ? C6 C3 C2 108.5(3) . . ? N2 C4 C3 113.8(2) . . ? N2 C5 C1 110.6(3) . 5_655 ? N3 C7 C1A 111.7(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.423 _refine_diff_density_min -0.472 _refine_diff_density_rms 0.071 #=END