Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2001 data_global #============================================================================== _journal_coden_Cambridge 186 # 1. SUBMISSION DETAILS _publ_contact_author 'Dr R. Cannon' _publ_contact_author_address ; Dr R Cannon School of Chemical Sciences University of East Anglia Norwich Norfolk NR4 7TJ UNITED KINGDOM ; _publ_contact_author_email 'R.CANNON@UEA.AC.UK' _publ_requested_journal 'Dalton Transactions' _publ_requested_coeditor_name ? _publ_contact_letter ; Here you find the crystallographic data of the publication Electron Transfer in a Trinuclear Oxo-Centered Mixed-Valence Iron Complex: Evidence of Strong Exchange-Coupling' which is submitted to the journal 'Dalton Trans.. Sincerely Regine Herbst-Irmer ; #============================================================================== # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Electron Transfer in a Trinuclear Oxo-Centered Mixed-Valence Iron Complex: Evidence of Strong Exchange-Coupling ; loop_ _publ_author_name _publ_author_address 'Stadler, Christian' ; Dipartimanto de Biocatalisis Instituto de catalisis y Petroquimica (CSIC) Campus Universidad Autonoma Cantoblanco 28049 Madrid Spain ; 'Daub, Jorg' ; Institut f\"ur Organische Chemie Universit\"at Regensburg Universit\"atsstr. 31 D-93053 Regensburg Germany ; 'Kohler, Jurgen' ; Institut f\"ur Organische Chemie Universit\"at Erlangen-N\"urnberg Henkestr. 42 D-91054 Erlangen Germany ; 'Sallfrank, Rolf W.' ; Institut f\"ur Organische Chemie Universit\"at Erlangen-N\"urnberg Henkestr. 42 D-91054 Erlangen Germany ; 'Coropceanu, Veaceslav' ; Institut f\"ur Physik Medizinische Universit\"at L\"ubeck Ratzeburger Allee 160 D-23538 L\"ubeck Germany ; 'Volker Sch\"unemann' ; Institut f\"ur Physik Medizinische Universit\"at L\"ubeck Ratzeburger Allee 160 D-23538 L\"ubeck Germany ; 'Ober, Claudia' ; Institut f\"ur Physik Medizinische Universit\"at L\"ubeck Ratzeburger Allee 160 D-23538 L\"ubeck Germany ; 'Trautwein, Alfred X.' ; Institut f\"ur Physik Medizinische Universit\"at L\"ubeck Ratzeburger Allee 160 D-23538 L\"ubeck Germany ; 'Parker, Stewart F.' ; Rutherford Appleton Laboratory Chilton Didcot OX11 0qx UK ; 'Poyraz, Mehmet' ; School of Chemical Sciences University of East Anglia Norwich NR4 7TJ UK ; 'Inomata, Tomohiko' ; School of Chemical Sciences University of East Anglia Norwich NR4 7TJ UK ; 'Cannon, Roderick D.' ; School of Chemical Sciences University of East Anglia Norwich NR4 7TJ UK ; #============================================================================== data_chausey _database_code_CSD 165605 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43.20 H49.80 Cl3.60 Fe2 N33 Ni O7' _chemical_formula_weight 1441.39 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' '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' 'Ni' 'Ni' 0.3393 1.1124 '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' _symmetry_cell_setting rhombohedral _symmetry_space_group_name_H-M R-3c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+5/6' 'x-y+2/3, -y+1/3, -z+5/6' '-x+2/3, -x+y+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+7/6' 'x-y+1/3, -y+2/3, -z+7/6' '-x+1/3, -x+y+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-y+2/3, -x+1/3, z-1/6' '-x+y+2/3, y+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-y+1/3, -x+2/3, z+1/6' '-x+y+1/3, y+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' _cell_length_a 23.184(3) _cell_length_b 23.184(3) _cell_length_c 22.634(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 10536(2) _cell_formula_units_Z 6 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 42133 _cell_measurement_theta_min 1.76 _cell_measurement_theta_max 28.28 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.50 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.363 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4423 _exptl_absorpt_coefficient_mu 0.877 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5406 _exptl_absorpt_correction_T_max 0.6683 _exptl_absorpt_process_details ? _exptl_special_details ; Intensities were measured with a Siemens CCD area detector ; _diffrn_ambient_temperature 133(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 'Stoe-Siemens-Huber four circle diffractometer' _diffrn_measurement_method 'phi scan' _diffrn_detector_area_resol_mean '8.192 pixels/mm' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42133 _diffrn_reflns_av_R_equivalents 0.0332 _diffrn_reflns_av_sigmaI/netI 0.0178 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 28.28 _reflns_number_total 2902 _reflns_number_gt 2452 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART (V. 4.202, Siemens 1996)' _computing_cell_refinement 'Siemens SAINT (V. 4.050, Siemens 1996)' _computing_data_reduction 'Siemens SAINT (V. 4.050, Siemens 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker AXS SHELXTL (V. 5.10)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0552P)^2^+19.7318P] 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 SHELXL _refine_ls_extinction_coef 0.00016(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2902 _refine_ls_number_parameters 245 _refine_ls_number_restraints 248 _refine_ls_R_factor_all 0.0484 _refine_ls_R_factor_gt 0.0371 _refine_ls_wR_factor_ref 0.1047 _refine_ls_wR_factor_gt 0.0981 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.070 _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 0.0000 0.081733(14) 0.2500 0.02096(12) Uani 0.67 2 d SP . 1 Ni1 Ni 0.0000 0.081733(14) 0.2500 0.02096(12) Uani 0.33 2 d SP . 2 O1 O 0.0000 0.0000 0.2500 0.0209(6) Uani 1 6 d S . . O2 O 0.14564(8) 0.25140(7) 0.33549(8) 0.0423(4) Uani 1 1 d . . . N1 N 0.11575(8) 0.06430(8) 0.32602(7) 0.0265(3) Uani 1 1 d . . . N2 N 0.14113(10) 0.04906(9) 0.37398(9) 0.0413(5) Uani 1 1 d . . . N3 N 0.14849(11) 0.08814(10) 0.41718(9) 0.0473(5) Uani 1 1 d . . . N4 N 0.12771(9) 0.13052(9) 0.39808(8) 0.0350(4) Uani 1 1 d . . . N5 N 0.07912(7) 0.14159(7) 0.30604(7) 0.0240(3) Uani 1 1 d . . . N6 N 0.0000 0.16974(9) 0.2500 0.0275(5) Uani 1 2 d S . . C1 C 0.0000 0.28680(13) 0.2500 0.0597(11) Uani 1 2 d S . . H1 H 0.0000 0.3278 0.2500 0.072 Uiso 1 2 calc SR . . C2 C 0.05064(12) 0.28253(10) 0.27898(13) 0.0492(7) Uani 1 1 d . . . H2 H 0.0857 0.3201 0.2983 0.059 Uiso 1 1 calc R . . C3 C 0.04823(10) 0.22164(9) 0.27864(10) 0.0324(4) Uani 1 1 d . . . C4 C 0.09684(9) 0.20705(9) 0.31024(9) 0.0298(4) Uani 1 1 d . . . C5 C 0.10799(9) 0.11579(9) 0.34147(8) 0.0250(4) Uani 1 1 d . . . C6 C 0.12153(15) 0.17486(14) 0.44033(11) 0.0530(7) Uani 1 1 d . . . H6A H 0.1590 0.2203 0.4353 0.079 Uiso 1 1 calc R . . H6B H 0.1219 0.1596 0.4806 0.079 Uiso 1 1 calc R . . H6C H 0.0796 0.1744 0.4334 0.079 Uiso 1 1 calc R . . C1S C 0.3358(3) 0.2280(5) 0.2880(7) 0.074(3) Uani 0.20 1 d PDU A -1 H1S H 0.3312 0.2040 0.2500 0.089 Uiso 0.20 1 calc PR A -1 Cl1S Cl 0.3440(4) 0.1821(4) 0.3448(3) 0.1109(19) Uani 0.20 1 d PDU A -1 Cl2S Cl 0.4030(2) 0.3087(3) 0.2809(3) 0.1049(18) Uani 0.20 1 d PDU A -1 Cl3S Cl 0.26377(18) 0.2325(2) 0.2981(2) 0.0774(12) Uani 0.20 1 d PDU A -1 C1P C 0.2890(14) 0.2038(12) 0.3256(13) 0.110(7) Uani 0.15 1 d PDU B -2 H1P1 H 0.3027 0.1959 0.3643 0.165 Uiso 0.15 1 calc PR B -2 H1P2 H 0.2702 0.1629 0.3021 0.165 Uiso 0.15 1 calc PR B -2 H1P3 H 0.2553 0.2171 0.3310 0.165 Uiso 0.15 1 calc PR B -2 C2P C 0.3478(11) 0.2579(12) 0.2945(12) 0.111(6) Uani 0.15 1 d PDU B -2 H2P1 H 0.3636 0.2382 0.2642 0.134 Uiso 0.15 1 calc PR B -2 H2P2 H 0.3844 0.2825 0.3231 0.134 Uiso 0.15 1 calc PR B -2 C3P C 0.3301(11) 0.3051(10) 0.2655(11) 0.114(6) Uani 0.15 1 d PDU B -2 H3P1 H 0.3049 0.2852 0.2287 0.136 Uiso 0.15 1 calc PR B -2 H3P2 H 0.3018 0.3142 0.2923 0.136 Uiso 0.15 1 calc PR B -2 C4P C 0.3932(14) 0.3684(12) 0.2519(18) 0.143(10) Uani 0.15 1 d PDU B -2 H4P1 H 0.4169 0.3893 0.2891 0.171 Uiso 0.15 1 calc PR B -2 H4P2 H 0.4225 0.3585 0.2274 0.171 Uiso 0.15 1 calc PR B -2 C5P C 0.378(3) 0.4156(15) 0.2195(18) 0.190(15) Uani 0.15 1 d PDU B -2 H5P1 H 0.4037 0.4295 0.1827 0.285 Uiso 0.15 1 calc PR B -2 H5P2 H 0.3903 0.4547 0.2443 0.285 Uiso 0.15 1 calc PR B -2 H5P3 H 0.3304 0.3934 0.2105 0.285 Uiso 0.15 1 calc PR B -2 C1Q C 0.3311(13) 0.2179(15) 0.3068(10) 0.074(5) Uani 0.15 1 d PDU C -3 H1Q1 H 0.2906 0.2190 0.3172 0.111 Uiso 0.15 1 calc PR C -3 H1Q2 H 0.3189 0.1763 0.2859 0.111 Uiso 0.15 1 calc PR C -3 H1Q3 H 0.3591 0.2559 0.2812 0.111 Uiso 0.15 1 calc PR C -3 C2Q C 0.3686(10) 0.2219(17) 0.3617(11) 0.101(7) Uani 0.15 1 d PDU C -3 H2Q1 H 0.3861 0.1908 0.3587 0.121 Uiso 0.15 1 calc PR C -3 H2Q2 H 0.4069 0.2675 0.3663 0.121 Uiso 0.15 1 calc PR C -3 C3Q C 0.3239(12) 0.2043(13) 0.4142(9) 0.092(7) Uani 0.15 1 d PDU C -3 H3Q1 H 0.2770 0.1769 0.4015 0.110 Uiso 0.15 1 calc PR C -3 H3Q2 H 0.3294 0.2455 0.4325 0.110 Uiso 0.15 1 calc PR C -3 C4Q C 0.3401(14) 0.1665(13) 0.4585(12) 0.116(8) Uani 0.15 1 d PDU C -3 H4Q1 H 0.3772 0.1609 0.4439 0.139 Uiso 0.15 1 calc PR C -3 H4Q2 H 0.3008 0.1218 0.4649 0.139 Uiso 0.15 1 calc PR C -3 C5Q C 0.3595(14) 0.205(2) 0.5151(11) 0.128(12) Uani 0.15 1 d PDU C -3 H5Q1 H 0.3220 0.1848 0.5429 0.192 Uiso 0.15 1 calc PR C -3 H5Q2 H 0.3712 0.2512 0.5073 0.192 Uiso 0.15 1 calc PR C -3 H5Q3 H 0.3979 0.2043 0.5323 0.192 Uiso 0.15 1 calc PR C -3 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 0.01801(18) 0.01790(14) 0.0270(2) -0.00107(6) -0.00213(12) 0.00901(9) Ni1 0.01801(18) 0.01790(14) 0.0270(2) -0.00107(6) -0.00213(12) 0.00901(9) O1 0.0190(8) 0.0190(8) 0.0246(16) 0.000 0.000 0.0095(4) O2 0.0347(8) 0.0227(7) 0.0626(11) -0.0093(7) -0.0186(7) 0.0091(6) N1 0.0280(7) 0.0244(7) 0.0283(8) 0.0002(6) -0.0064(6) 0.0140(6) N2 0.0508(11) 0.0362(9) 0.0403(11) -0.0014(8) -0.0188(9) 0.0243(9) N3 0.0647(13) 0.0426(10) 0.0349(11) -0.0010(8) -0.0179(9) 0.0270(10) N4 0.0430(10) 0.0340(9) 0.0262(9) -0.0036(7) -0.0062(7) 0.0178(8) N5 0.0219(7) 0.0192(7) 0.0294(8) -0.0015(6) -0.0037(6) 0.0093(6) N6 0.0245(10) 0.0202(7) 0.0393(13) -0.0021(5) -0.0042(9) 0.0123(5) C1 0.057(2) 0.0277(10) 0.104(3) -0.0148(11) -0.030(2) 0.0287(11) C2 0.0420(12) 0.0223(9) 0.0841(19) -0.0124(11) -0.0217(12) 0.0167(9) C3 0.0275(9) 0.0201(8) 0.0494(13) -0.0037(8) -0.0060(8) 0.0119(7) C4 0.0258(9) 0.0212(8) 0.0399(11) -0.0028(8) -0.0045(8) 0.0100(7) C5 0.0220(8) 0.0229(8) 0.0258(9) -0.0001(7) -0.0009(7) 0.0080(7) C6 0.0694(17) 0.0537(15) 0.0332(12) -0.0140(11) -0.0012(11) 0.0288(13) C1S 0.046(6) 0.075(7) 0.092(9) -0.032(7) 0.011(7) 0.023(5) Cl1S 0.090(4) 0.169(6) 0.093(4) -0.007(4) 0.006(3) 0.079(4) Cl2S 0.0453(19) 0.084(3) 0.156(5) -0.061(3) 0.003(2) 0.0104(19) Cl3S 0.0430(16) 0.068(2) 0.113(4) -0.032(2) 0.0014(19) 0.0209(16) C1P 0.074(13) 0.107(12) 0.133(15) -0.049(10) 0.026(11) 0.033(10) C2P 0.091(10) 0.103(10) 0.126(12) -0.050(9) 0.039(9) 0.037(8) C3P 0.123(12) 0.114(10) 0.103(13) -0.057(9) 0.040(10) 0.060(9) C4P 0.160(17) 0.119(12) 0.126(18) -0.036(12) 0.038(16) 0.053(12) C5P 0.29(4) 0.18(2) 0.10(3) 0.00(2) 0.06(3) 0.12(2) C1Q 0.050(11) 0.064(11) 0.111(10) -0.021(11) -0.007(9) 0.031(9) C2Q 0.067(12) 0.102(15) 0.114(13) 0.008(13) -0.006(8) 0.028(12) C3Q 0.048(13) 0.076(11) 0.116(10) -0.004(12) -0.011(9) 0.004(9) C4Q 0.061(13) 0.118(17) 0.143(16) 0.044(14) 0.029(13) 0.025(12) C5Q 0.038(13) 0.16(3) 0.130(16) 0.044(17) -0.009(15) 0.009(18) _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 O1 1.8949(4) . y Fe1 N6 2.040(2) . y Fe1 N5 2.0865(15) 6 ? Fe1 N5 2.0865(15) . y Fe1 N1 2.1515(16) 2 y Fe1 N1 2.1515(16) 4 ? O1 Ni1 1.8949(4) 2 ? O1 Fe1 1.8949(4) 2 ? O1 Ni1 1.8949(4) 3 ? O1 Fe1 1.8949(4) 3 ? O2 C4 1.225(2) . y N1 C5 1.339(2) . y N1 N2 1.363(2) . y N1 Ni1 2.1514(16) 3 ? N1 Fe1 2.1514(16) 3 ? N2 N3 1.285(3) . y N3 N4 1.363(3) . y N4 C5 1.346(2) . y N4 C6 1.463(3) . y N5 C5 1.360(2) . y N5 C4 1.363(2) . y N6 C3 1.331(2) . y N6 C3 1.331(2) 6 y C1 C2 1.391(3) 6 y C1 C2 1.391(3) . ? C2 C3 1.384(3) . y C3 C4 1.509(3) . y C1S Cl1S 1.740(7) . ? C1S Cl3S 1.741(7) . ? C1S Cl2S 1.743(7) . ? C1P C2P 1.490(7) . ? C2P C3P 1.498(7) . ? C3P C4P 1.498(7) . ? C4P C5P 1.496(7) . ? C1Q C2Q 1.494(7) . ? C2Q C3Q 1.493(7) . ? C3Q C4Q 1.497(7) . ? C4Q C5Q 1.498(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Fe1 N6 180.0 . . y O1 Fe1 N5 103.04(4) . 6 y N6 Fe1 N5 76.96(4) . 6 y O1 Fe1 N5 103.04(4) . . ? N6 Fe1 N5 76.96(4) . . ? N5 Fe1 N5 153.93(8) 6 . y O1 Fe1 N1 91.16(4) . 2 y N6 Fe1 N1 88.84(4) . 2 y N5 Fe1 N1 91.42(6) 6 2 y N5 Fe1 N1 88.06(6) . 2 y O1 Fe1 N1 91.16(4) . 4 ? N6 Fe1 N1 88.84(4) . 4 ? N5 Fe1 N1 88.06(6) 6 4 ? N5 Fe1 N1 91.42(6) . 4 ? N1 Fe1 N1 177.69(8) 2 4 y Fe1 O1 Ni1 120.0 . 2 ? Fe1 O1 Fe1 120.0 . 2 ? Ni1 O1 Fe1 0.00(3) 2 2 ? Fe1 O1 Ni1 120.0 . 3 ? Ni1 O1 Ni1 120.0 2 3 ? Fe1 O1 Ni1 120.0 2 3 ? Fe1 O1 Fe1 120.0 . 3 ? Ni1 O1 Fe1 120.0 2 3 ? Fe1 O1 Fe1 120.0 2 3 ? Ni1 O1 Fe1 0.0 3 3 ? C5 N1 N2 106.91(16) . . y C5 N1 Ni1 131.32(12) . 3 y N2 N1 Ni1 120.90(12) . 3 y C5 N1 Fe1 131.32(12) . 3 ? N2 N1 Fe1 120.90(12) . 3 ? Ni1 N1 Fe1 0.000(17) 3 3 ? N3 N2 N1 110.21(17) . . y N2 N3 N4 107.28(17) . . y C5 N4 N3 108.45(17) . . y C5 N4 C6 131.3(2) . . y N3 N4 C6 119.58(19) . . y C5 N5 C4 120.54(16) . . y C5 N5 Fe1 121.89(12) . . y C4 N5 Fe1 117.28(12) . . y C3 N6 C3 122.1(2) . 6 y C3 N6 Fe1 118.93(11) . . y C3 N6 Fe1 118.93(11) 6 . ? C2 C1 C2 120.9(3) 6 . y C3 C2 C1 117.7(2) . . y N6 C3 C2 120.77(19) . . y N6 C3 C4 114.33(16) . . y C2 C3 C4 124.89(18) . . y O2 C4 N5 127.22(18) . . y O2 C4 C3 120.85(17) . . y N5 C4 C3 111.93(15) . . y N1 C5 N4 107.15(17) . . y N1 C5 N5 123.58(17) . . y N4 C5 N5 128.99(18) . . y Cl1S C1S Cl3S 109.9(6) . . ? Cl1S C1S Cl2S 114.3(8) . . ? Cl3S C1S Cl2S 108.5(6) . . ? C1P C2P C3P 110.5(10) . . ? C4P C3P C2P 108.5(10) . . ? C5P C4P C3P 110.3(10) . . ? C3Q C2Q C1Q 110.0(10) . . ? C2Q C3Q C4Q 110.5(10) . . ? C3Q C4Q C5Q 108.2(10) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.388 _refine_diff_density_min -0.267 _refine_diff_density_rms 0.065 ### END ### data_jk01_2 _database_code_CSD 153559 #----------------------------------------------------------------------- #4 Chemical and physical data _chemical_name_systematic '?' _chemical_name_common '?' _chemical_formula_moiety '?' _chemical_formula_sum 'C39 H33 Cl18 Cu Fe2 N33 O7' _chemical_formula_weight 1889.32 _chemical_melting_point ? _ccdc_compound_id '?' _ccdc_biological_activity '?' _ccdc_polymorph '?' _ccdc_chemdiag_type '?' loop_ _ccdc_chemdiag_records ? _exptl_crystal_density_diffrn ? _exptl_crystal_colour 'orange' #------------------------------------------------------------------------- #5 Other data relating to the structure determination and refinement _diffrn_radiation_type 'Mo-Ka' _diffrn_measurement_device 'Nonius KappaCCD' _ccdc_temp_data_collection 173 _ccdc_ls_R_squared ? _refine_ls_abs_structure_details '?' _ccdc_disorder '?' _ccdc_comments '?' #------------------------------------------------------------------------- #6 Include your "standard" CIF file here _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H33 Cl18 Cu Fe2 N33 O7' _chemical_formula_weight 1889.32 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' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 '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' _symmetry_cell_setting Rhombohedral _symmetry_space_group_name_H-M R-3c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+5/6' 'x-y+2/3, -y+1/3, -z+5/6' '-x+2/3, -x+y+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+7/6' 'x-y+1/3, -y+2/3, -z+7/6' '-x+1/3, -x+y+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-y+2/3, -x+1/3, z-1/6' '-x+y+2/3, y+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-y+1/3, -x+2/3, z+1/6' '-x+y+1/3, y+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' _cell_length_a 23.314(3) _cell_length_b 23.314(3) _cell_length_c 22.811(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 10738(2) _cell_formula_units_Z 6 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 28436 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 27.48 _exptl_crystal_description blocks _exptl_crystal_colour orange _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.753 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5646 _exptl_absorpt_coefficient_mu 1.436 _exptl_absorpt_correction_type Scalepack _exptl_absorpt_correction_T_min 0.6333 _exptl_absorpt_correction_T_max 0.6725 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23307 _diffrn_reflns_av_R_equivalents 0.0357 _diffrn_reflns_av_sigmaI/netI 0.0253 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 27.51 _reflns_number_total 2751 _reflns_number_gt 2316 _reflns_threshold_expression >2sigma(I) _computing_data_collection Collect _computing_cell_refinement Denzo-SMN _computing_data_reduction Denzo-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0675P)^2^+50.4738P] 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 SHELXL _refine_ls_extinction_coef 0.00020(7) _refine_ls_extinction_expression 'Fc^*^==kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2751 _refine_ls_number_parameters 192 _refine_ls_number_restraints 78 _refine_ls_R_factor_all 0.0629 _refine_ls_R_factor_gt 0.0465 _refine_ls_wR_factor_ref 0.1347 _refine_ls_wR_factor_gt 0.1263 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.112 _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 0.08140(2) 0.2500 0.02266(19) Uani 0.67 2 d SP . 1 Cu1 Cu 0.0000 0.08140(2) 0.2500 0.02266(19) Uani 0.33 2 d SP . 2 O1 O 0.0000 0.0000 0.2500 0.0170(8) Uani 1 6 d S . . O2 O 0.14432(11) 0.24986(10) 0.33482(10) 0.0380(5) Uani 1 1 d . . . N1 N 0.11674(13) 0.06600(12) 0.32639(11) 0.0295(5) Uani 1 1 d . . . N2 N 0.14291(15) 0.05145(15) 0.37378(12) 0.0407(7) Uani 1 1 d . . . N3 N 0.14778(16) 0.08835(15) 0.41666(12) 0.0436(7) Uani 1 1 d . . . N4 N 0.12479(14) 0.12869(14) 0.39849(11) 0.0342(6) Uani 1 1 d . . . N5 N 0.07712(11) 0.14026(11) 0.30690(10) 0.0227(5) Uani 1 1 d . . . N6 N 0.0000 0.16870(13) 0.2500 0.0228(6) Uani 1 2 d S . . C1 C 0.0000 0.28520(19) 0.2500 0.0445(12) Uani 1 2 d S . . H1 H 0.0000 0.3259 0.2500 0.053 Uiso 1 2 calc SR . . C2 C 0.04968(17) 0.28057(15) 0.27932(15) 0.0374(7) Uani 1 1 d . . . H2 H 0.0841 0.3176 0.2992 0.045 Uiso 1 1 calc R . . C3 C 0.04730(14) 0.22012(13) 0.27865(13) 0.0266(6) Uani 1 1 d . . . C4 C 0.09541(13) 0.20546(13) 0.31041(12) 0.0258(6) Uani 1 1 d . . . C5 C 0.10653(13) 0.11510(14) 0.34218(12) 0.0246(6) Uani 1 1 d . . . C6 C 0.1178(2) 0.1725(2) 0.43984(16) 0.0524(10) Uani 1 1 d . . . H6A H 0.1540 0.2180 0.4340 0.079 Uiso 1 1 calc R . . H6B H 0.1194 0.1584 0.4800 0.079 Uiso 1 1 calc R . . H6C H 0.0753 0.1706 0.4333 0.079 Uiso 1 1 calc R . . C1S C 0.3321(2) 0.2262(3) 0.2930(2) 0.0610(15) Uani 0.801(7) 1 d PDU A 1 H1S H 0.3213 0.2068 0.2526 0.073 Uiso 0.801(7) 1 calc PR A 1 Cl1 Cl 0.34461(17) 0.1712(2) 0.33803(12) 0.1064(12) Uani 0.801(7) 1 d PDU A 1 Cl2 Cl 0.40069(14) 0.30300(19) 0.2876(2) 0.1146(15) Uani 0.801(7) 1 d PDU A 1 Cl3 Cl 0.26323(12) 0.22954(16) 0.31896(13) 0.0853(8) Uani 0.801(7) 1 d PDU A 1 C1S' C 0.3531(10) 0.2832(13) 0.3362(12) 0.148(10) Uani 0.199(7) 1 d PDU A 2 H1S' H 0.3672 0.3153 0.3696 0.178 Uiso 0.199(7) 1 calc PR A 2 Cl1' Cl 0.3665(7) 0.2176(9) 0.3504(4) 0.123(4) Uani 0.199(7) 1 d PDU A 2 Cl2' Cl 0.3962(9) 0.3202(8) 0.2715(6) 0.123(6) Uani 0.199(7) 1 d PDU A 2 Cl3' Cl 0.2671(7) 0.2385(9) 0.3280(12) 0.252(12) Uani 0.199(7) 1 d PDU A 2 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 0.0214(3) 0.0221(2) 0.0242(3) -0.00085(9) -0.00170(19) 0.01068(15) Cu1 0.0214(3) 0.0221(2) 0.0242(3) -0.00085(9) -0.00170(19) 0.01068(15) O1 0.0145(12) 0.0145(12) 0.022(2) 0.000 0.000 0.0073(6) O2 0.0309(11) 0.0239(10) 0.0548(14) -0.0076(9) -0.0172(10) 0.0104(9) N1 0.0349(13) 0.0306(13) 0.0289(12) 0.0021(10) -0.0040(10) 0.0209(11) N2 0.0493(17) 0.0412(16) 0.0396(15) 0.0031(12) -0.0114(12) 0.0287(14) N3 0.0536(18) 0.0441(16) 0.0363(15) 0.0049(12) -0.0120(13) 0.0267(14) N4 0.0380(14) 0.0390(15) 0.0264(13) -0.0010(10) -0.0043(10) 0.0200(12) N5 0.0214(11) 0.0207(11) 0.0268(11) -0.0011(8) -0.0030(8) 0.0111(9) N6 0.0207(15) 0.0184(11) 0.0299(17) -0.0012(6) -0.0023(12) 0.0104(7) C1 0.049(3) 0.0258(15) 0.066(3) -0.0077(12) -0.015(2) 0.0247(14) C2 0.0377(17) 0.0231(14) 0.0523(19) -0.0082(13) -0.0124(14) 0.0157(13) C3 0.0259(14) 0.0198(13) 0.0340(15) -0.0011(11) -0.0018(11) 0.0113(11) C4 0.0227(13) 0.0206(13) 0.0324(14) -0.0025(11) -0.0036(11) 0.0096(11) C5 0.0209(13) 0.0253(13) 0.0254(13) 0.0018(10) 0.0003(10) 0.0099(11) C6 0.069(3) 0.062(2) 0.0318(17) -0.0143(16) -0.0057(16) 0.037(2) C1S 0.041(3) 0.070(3) 0.070(4) -0.030(3) -0.004(2) 0.025(2) Cl1 0.1064(19) 0.172(3) 0.0779(14) 0.0232(17) 0.0296(13) 0.098(2) Cl2 0.0400(10) 0.0827(17) 0.199(4) -0.045(2) 0.0143(15) 0.0140(10) Cl3 0.0393(10) 0.0729(16) 0.133(2) -0.0240(12) 0.0064(9) 0.0198(9) C1S' 0.104(12) 0.16(2) 0.15(2) 0.05(2) 0.015(19) 0.041(18) Cl1' 0.152(10) 0.140(11) 0.065(5) -0.008(6) 0.014(5) 0.065(9) Cl2' 0.118(10) 0.106(10) 0.076(6) -0.035(5) 0.007(5) 0.004(7) Cl3' 0.067(7) 0.081(7) 0.58(3) -0.140(12) 0.081(10) 0.017(5) _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 O1 1.8977(6) . ? Fe1 N6 2.035(3) . ? Fe1 N5 2.082(2) 6 ? Fe1 N5 2.082(2) . ? Fe1 N1 2.194(3) 4 ? Fe1 N1 2.194(3) 2 ? O1 Cu1 1.8977(6) 2 ? O1 Fe1 1.8977(6) 2 ? O1 Cu1 1.8977(6) 3 ? O1 Fe1 1.8977(6) 3 ? O2 C4 1.225(3) . ? N1 C5 1.330(4) . ? N1 N2 1.365(3) . ? N1 Cu1 2.194(3) 3 ? N1 Fe1 2.194(3) 3 ? N2 N3 1.270(4) . ? N3 N4 1.359(4) . ? N4 C5 1.340(4) . ? N4 C6 1.459(4) . ? N5 C4 1.360(3) . ? N5 C5 1.365(3) . ? N6 C3 1.326(3) 6 ? N6 C3 1.326(3) . ? C1 C2 1.388(4) 6 ? C1 C2 1.388(4) . ? C2 C3 1.382(4) . ? C3 C4 1.511(4) . ? C1S Cl2 1.707(6) . ? C1S Cl3 1.750(5) . ? C1S Cl1 1.779(6) . ? C1S' Cl1' 1.738(17) . ? C1S' Cl3' 1.746(16) . ? C1S' Cl2' 1.752(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Fe1 N6 180.0 . . ? O1 Fe1 N5 103.14(6) . 6 ? N6 Fe1 N5 76.86(6) . 6 ? O1 Fe1 N5 103.14(6) . . ? N6 Fe1 N5 76.86(6) . . ? N5 Fe1 N5 153.72(12) 6 . ? O1 Fe1 N1 91.43(7) . 4 ? N6 Fe1 N1 88.57(7) . 4 ? N5 Fe1 N1 87.34(9) 6 4 ? N5 Fe1 N1 92.02(9) . 4 ? O1 Fe1 N1 91.43(7) . 2 ? N6 Fe1 N1 88.57(7) . 2 ? N5 Fe1 N1 92.02(9) 6 2 ? N5 Fe1 N1 87.34(9) . 2 ? N1 Fe1 N1 177.15(13) 4 2 ? Cu1 O1 Fe1 0.00(5) 2 2 ? Cu1 O1 Cu1 120.0 2 3 ? Fe1 O1 Cu1 120.0 2 3 ? Cu1 O1 Fe1 120.0 2 3 ? Fe1 O1 Fe1 120.0 2 3 ? Cu1 O1 Fe1 0.0 3 3 ? Cu1 O1 Fe1 120.0 2 . ? Fe1 O1 Fe1 120.0 2 . ? Cu1 O1 Fe1 120.0 3 . ? Fe1 O1 Fe1 120.0 3 . ? C5 N1 N2 107.1(2) . . ? C5 N1 Cu1 130.73(19) . 3 ? N2 N1 Cu1 120.83(19) . 3 ? C5 N1 Fe1 130.73(19) . 3 ? N2 N1 Fe1 120.83(19) . 3 ? Cu1 N1 Fe1 0.00(3) 3 3 ? N3 N2 N1 110.0(3) . . ? N2 N3 N4 107.5(2) . . ? C5 N4 N3 108.5(3) . . ? C5 N4 C6 130.7(3) . . ? N3 N4 C6 120.6(3) . . ? C4 N5 C5 120.1(2) . . ? C4 N5 Fe1 117.27(18) . . ? C5 N5 Fe1 122.55(18) . . ? C3 N6 C3 121.5(3) 6 . ? C3 N6 Fe1 119.23(16) 6 . ? C3 N6 Fe1 119.23(16) . . ? C2 C1 C2 120.7(4) 6 . ? C3 C2 C1 117.7(3) . . ? N6 C3 C2 121.2(3) . . ? N6 C3 C4 114.1(2) . . ? C2 C3 C4 124.7(3) . . ? O2 C4 N5 127.6(3) . . ? O2 C4 C3 120.6(2) . . ? N5 C4 C3 111.8(2) . . ? N1 C5 N4 106.9(3) . . ? N1 C5 N5 123.7(3) . . ? N4 C5 N5 129.2(3) . . ? Cl2 C1S Cl3 112.1(3) . . ? Cl2 C1S Cl1 113.1(3) . . ? Cl3 C1S Cl1 108.7(3) . . ? Cl1' C1S' Cl3' 98.8(14) . . ? Cl1' C1S' Cl2' 106.2(14) . . ? Cl3' C1S' Cl2' 114.1(17) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.556 _refine_diff_density_min -0.662 _refine_diff_density_rms 0.157