Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _audit_creation_date '2001-08-13' _audit_creation_method 'by teXsan v1.8' _audit_update_record ; 1997-02-04 - Report on C42 H52 Cl Cu2 Fe N14 O12 by David C. R. Hockless for Richard Parker and Leone Spiccia 2001-08-10 - A. David Rae fixes problems 2001-08-13 - Anthony C. Willis makes up cif 2001-03-13 - passes checkcif tests with minor warnings ; #------------------------------------------------------------------------------ _journal_coden_Cambridge 186 loop_ _publ_author_name _publ_author_address ' Richard J. Parker ' ; School of Chemistry PO Box 23 Monash University 3800 Australia ; ' Kevin D. Lu ' ; School of Chemistry PO Box 23 Monash University 3800 Australia ; ' Stuart R. Batten ' ; School of Chemistry PO Box 23 Monash University 3800 Australia ; ' Boujemaa Moubaraki ' ; School of Chemistry PO Box 23 Monash University 3800 Australia ; ' Keith S. Murray ' ; School of Chemistry PO Box 23 Monash University 3800 Australia ; ' Leone Spiccia ' ; School of Chemistry PO Box 23 Monash University 3800 Australia ; ' John D. Cashion ' ; School of Physics and Materials Engineering PO Box 27 Monash University 3800 Australia ; ' A. David Rae ' ; Research School of Chemistry, Institute of Advanced Studies, Australian National University, Canberra, A. C. T. 0200, Australia ; ' Anthony C. Willis ' ; Research School of Chemistry, Institute of Advanced Studies, Australian National University, Canberra, A. C. T. 0200, Australia ; _publ_contact_author_name 'Dr Leone Spiccia ' _publ_contact_author_address ; Dr Leone Spiccia School of Chemistry Monash University PO Box 23 Clayton Victoria 3800 AUSTRALIA ; _publ_contact_author_phone ' 61 3 9905 4526 ' _publ_contact_author_fax ' 61 3 9905 4597 ' _publ_contact_author_email ' leone.spiccia@sci.monash.edu.au ' _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Synthesis, X-ray Structures and Magnetic Properties of Linear and Bent Trinuclear Complexes Formed by Hexacyanometallates and Copper(II) Complexes ; _publ_section_references ; RAELS00, A.D. Rae (2000) Australian National University, Canberra, Australia. Rae, A.D. (1975) Acta Cryst. A31, 560-570, 570-574. Rae, A.D. (1996) Acta Cryst. A52, C44-C45. Molecular Structure Corporation. (1992-1997). teXsan. Single Crystal Structure Analysis Software. Version 1.7. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M. C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. ; data_PAR2 _database_code_CSD 187746 _audit_creation_date '2001-08-13' _audit_creation_method 'by teXsan v1.8' _audit_update_record ; 1997-02-04 - Report on C42 H52 Cl Cu2 Fe N14 O12 by David C. R. Hockless for Richard Parker and Leone Spiccia 2001-08-10 - A. David Rae fixes problems 2001-08-13 - Anthony C. Willis makes up cif 2001-03-13 - passes checkcif tests with minor warnings ; #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1992-1997)' _computing_structure_solution ; SIR92 (Altomare, et. al. 1994) ; _computing_structure_refinement 'RAELS00' _computing_publication_material 'teXsan (MSC, 1992-1997)' #------------------------------------------------------------------------------ _cell_length_a 12.665(2) _cell_length_b 12.665 _cell_length_c 27.860(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 3870(1) _cell_formula_units_Z 3 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 45.5 _cell_measurement_theta_max 49.7 #------------------------------------------------------------------------------ _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'P 32 ' _symmetry_Int_Tables_number 145 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -y,x-y,2/3+z 3 -x+y,-x,1/3+z #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _exptl_crystal_description 'prism' _exptl_crystal_colour 'green' _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 1.497 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 1163.35 _chemical_formula_analytical ? _chemical_formula_sum 'C42 H52 Cl Cu2 Fe N14 O12 ' _chemical_formula_moiety 'C42 H36 Cu2 Fe N14 +, Cl O4 -, 8(H2 O) ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1797.00 _exptl_absorpt_coefficient_mu 4.269 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details ; \y scans (North,Phillips & Matthews, 1968) ; _exptl_absorpt_correction_T_max .426 _exptl_absorpt_correction_T_min .309 _exptl_special_details ; The scan width was (1.30+0.30tan\q)\% with an \w scan speed of 32\% per minute (up to 5 scans to achieve I/\s(I) > 10). Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC6R' _diffrn_measurement_device_details ; Rigaku AFC6R diffractometer with extended arm and evacuated collimator and beam tunnel. Data cannot be collected beyond \y 60 deg in this configuration. ; _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -0.94 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? ? ? ? ? ? ? _diffrn_reflns_number 6212 _reflns_number_total 3845 _reflns_number_gt 3183 _reflns_threshold_expression I>3.00\s(I) _diffrn_reflns_av_R_equivalents 0.04747 _diffrn_reflns_av_sigmaI/netI 0.060 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 0.00 _diffrn_reflns_theta_max 60.05 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.04105 _diffrn_orient_matrix_UB_12 -0.04223 _diffrn_orient_matrix_UB_13 -0.03049 _diffrn_orient_matrix_UB_21 0.07519 _diffrn_orient_matrix_UB_22 -0.00130 _diffrn_orient_matrix_UB_23 -0.00997 _diffrn_orient_matrix_UB_31 -0.03120 _diffrn_orient_matrix_UB_32 -0.08079 _diffrn_orient_matrix_UB_33 0.01610 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 126 0.017 0.009 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 156 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Cl 0 3 0.348 0.702 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Cu 0 6 -2.019 0.589 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Fe 0 3 -1.179 3.204 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N 0 42 0.029 0.018 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 36 0.047 0.032 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_refinement_flags _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom CU1 0.3487(1) 0.3311(1) 0.6782(1) 1.0 0.0263(2) . Uani d ? CU2 0.3744(1) 0.3591(1) 0.3217(1) 1.0 0.0263(2) . Uani d ? FE1 0.3514(1) 0.3272(1) 0.5000 1.0 0.023(1) . Uani d ? C101 0.3324(6) 0.3255(6) 0.5685(2) 1.0 0.026(1) . Uani d ? N11 0.3296(6) 0.3238(6) 0.6092(2) 1.0 0.033(1) . Uani d ? C201 0.3689(6) 0.3288(6) 0.4314(2) 1.0 0.026(1) . Uani d ? N21 0.3748(6) 0.3355(6) 0.3903(2) 1.0 0.033(1) . Uani d ? C301 0.3112(7) 0.4561(7) 0.4906(3) 1.0 0.032(1) . Uani d ? N31 0.2897(8) 0.5315(7) 0.4833(3) 1.0 0.053(2) . Uani d ? C401 0.3886(7) 0.1977(7) 0.5115(3) 1.0 0.032(1) . Uani d ? N41 0.4088(8) 0.1227(7) 0.5208(3) 1.0 0.053(2) . Uani d ? C501 0.1809(7) 0.2080(7) 0.4918(3) 1.0 0.031(1) . Uani d ? N51 0.0798(7) 0.1385(7) 0.4858(3) 1.0 0.056(2) . Uani d ? C601 0.5212(7) 0.4458(6) 0.5063(3) 1.0 0.031(1) . Uani d ? N61 0.6233(7) 0.5187(7) 0.5097(3) 1.0 0.056(2) . Uani d ? N15 0.3687(5) 0.3437(5) 0.7501(2) 1.0 0.030(1) . Uani d ? N12 0.3354(4) 0.1613(3) 0.6903(1) 1.0 0.029(1) . Uani d ? C102 0.3493(4) 0.0903(4) 0.6586(2) 1.0 0.032(1) . Uani d ? C103 0.3583(5) -0.0098(4) 0.6726(2) 1.0 0.038(1) . Uani d ? C104 0.3525(5) -0.0368(4) 0.7210(2) 1.0 0.040(1) . Uani d ? C105 0.3381(5) 0.0370(4) 0.7537(2) 1.0 0.038(1) . Uani d ? C106 0.3299(3) 0.1350(4) 0.7372(2) 1.0 0.032(1) . Uani d ? C107 0.3141(6) 0.2205(5) 0.7698(2) 1.0 0.033(1) . Uani d ? N13 0.5274(3) 0.4750(3) 0.6785(2) 1.0 0.030(1) . Uani d ? C108 0.5823(4) 0.5533(4) 0.6426(2) 1.0 0.034(1) . Uani d ? C109 0.6816(4) 0.6683(4) 0.6501(2) 1.0 0.043(1) . Uani d ? C110 0.7249(5) 0.7027(4) 0.6964(2) 1.0 0.046(1) . Uani d ? C111 0.6678(4) 0.6213(4) 0.7335(2) 1.0 0.042(1) . Uani d ? C112 0.5696(3) 0.5086(4) 0.7233(2) 1.0 0.033(1) . Uani d ? C113 0.5013(5) 0.4138(5) 0.7611(2) 1.0 0.034(1) . Uani d ? N14 0.1994(3) 0.3462(4) 0.6942(1) 1.0 0.029(1) . Uani d ? C114 0.1022(4) 0.3143(5) 0.6665(2) 1.0 0.032(1) . Uani d ? C115 -0.0007(4) 0.3143(5) 0.6832(2) 1.0 0.039(1) . Uani d ? C116 -0.0023(4) 0.3486(5) 0.7302(2) 1.0 0.043(1) . Uani d ? C117 0.0986(5) 0.3816(5) 0.7589(2) 1.0 0.040(1) . Uani d ? C118 0.1975(4) 0.3794(3) 0.7398(2) 1.0 0.033(1) . Uani d ? C119 0.3114(5) 0.4136(6) 0.7679(2) 1.0 0.034(1) . Uani d ? N25 0.3778(5) 0.3839(5) 0.2502(2) 1.0 0.030(1) . Uani d ? N22 0.3796(4) 0.5279(3) 0.3222(1) 1.0 0.029(1) . Uani d ? C202 0.3435(5) 0.5742(4) 0.3573(2) 1.0 0.032(1) . Uani d ? C203 0.3228(5) 0.6703(4) 0.3496(2) 1.0 0.038(1) . Uani d ? C204 0.3401(5) 0.7195(4) 0.3040(2) 1.0 0.040(1) . Uani d ? C205 0.3775(5) 0.6713(4) 0.2677(2) 1.0 0.037(1) . Uani d ? C206 0.3964(3) 0.5758(3) 0.2780(2) 1.0 0.031(1) . Uani d ? C207 0.4370(5) 0.5170(5) 0.2411(2) 1.0 0.033(1) . Uani d ? N23 0.1946(3) 0.2285(4) 0.3084(1) 1.0 0.030(1) . Uani d ? C208 0.1195(4) 0.1430(4) 0.3391(2) 1.0 0.034(1) . Uani d ? C209 0.0096(4) 0.0448(4) 0.3245(2) 1.0 0.043(1) . Uani d ? C210 -0.0229(4) 0.0355(4) 0.2767(2) 1.0 0.047(1) . Uani d ? C211 0.0552(5) 0.1243(5) 0.2450(2) 1.0 0.042(1) . Uani d ? C212 0.1629(4) 0.2193(4) 0.2620(2) 1.0 0.034(1) . Uani d ? C213 0.2538(5) 0.3202(5) 0.2305(2) 1.0 0.034(1) . Uani d ? N24 0.5316(3) 0.3567(4) 0.3082(1) 1.0 0.029(1) . Uani d ? C214 0.6185(4) 0.3758(5) 0.3397(2) 1.0 0.032(1) . Uani d ? C215 0.7314(4) 0.3949(5) 0.3255(2) 1.0 0.039(1) . Uani d ? C216 0.7545(4) 0.3941(6) 0.2770(2) 1.0 0.043(1) . Uani d ? C217 0.6642(4) 0.3743(5) 0.2444(2) 1.0 0.040(1) . Uani d ? C218 0.5542(4) 0.3560(3) 0.2611(2) 1.0 0.033(1) . Uani d ? C219 0.4503(5) 0.3338(6) 0.2287(2) 1.0 0.034(1) . Uani d ? CL1 0.6802(2) 0.9592(3) 0.5838(1) 1.0 0.061(3) . Uani d ? O11 0.6965(10) 1.0463(9) 0.5512(4) 1.0 0.107(4) . Uani d ? O12 0.6443(14) 0.8497(10) 0.5608(4) 1.0 0.161(5) . Uani d ? O13 0.7818(12) 1.0018(17) 0.6117(4) 1.0 0.184(6) . Uani d ? O14 0.5779(10) 0.9387(11) 0.6133(4) 1.0 0.118(5) . Uani d ? O1 0.0035(9) -0.3832(10) 0.4478(4) 1.0 0.108(3) . Uani d ? O2 -0.0055(13) -0.2281(15) 0.3845(4) 1.0 0.165(5) . Uani d ? O3 -0.2371(9) -0.5860(10) 0.4462(3) 1.0 0.100(3) . Uani d ? O4 0.2644(7) 0.7352(7) 0.4644(2) 1.0 0.067(2) . Uani d ? O5 0.8146(6) 0.7689(5) 0.5196(3) 1.0 0.063(2) . Uani d ? O6 0.3738(6) -0.1076(5) 0.5440(3) 1.0 0.060(2) . Uani d ? O7 -0.0770(7) -0.0866(6) 0.4377(3) 1.0 0.074(2) . Uani d ? O8 -0.0295(8) 0.2585(7) 0.5556(3) 1.0 0.079(2) . Uani d ? H1C102 0.3535 0.1100 0.6237 1.0 0.034 . Uani d ? H1C103 0.3687 -0.0618 0.6481 1.0 0.043 . Uani d ? H1C104 0.3587 -0.1086 0.7321 1.0 0.047 . Uani d ? H1C105 0.3337 0.0194 0.7889 1.0 0.044 . Uani d ? H1C107 0.3535 0.2242 0.8014 1.0 0.038 . Uani d ? H2C107 0.2250 0.1885 0.7748 1.0 0.036 . Uani d ? H1C108 0.5508 0.5282 0.6092 1.0 0.035 . Uani d ? H1C109 0.7213 0.7255 0.6226 1.0 0.049 . Uani d ? H1C110 0.7965 0.7853 0.7029 1.0 0.056 . Uani d ? H1C111 0.6974 0.6441 0.7672 1.0 0.048 . Uani d ? H1C113 0.5134 0.4549 0.7929 1.0 0.039 . Uani d ? H2C113 0.5338 0.3563 0.7624 1.0 0.035 . Uani d ? H1C114 0.1037 0.2895 0.6325 1.0 0.033 . Uani d ? H1C115 -0.0724 0.2900 0.6617 1.0 0.044 . Uani d ? H1C116 -0.0754 0.3495 0.7433 1.0 0.050 . Uani d ? H1C117 0.0995 0.4068 0.7930 1.0 0.046 . Uani d ? H1C119 0.2902 0.3946 0.8026 1.0 0.040 . Uani d ? H2C119 0.3699 0.5028 0.7641 1.0 0.035 . Uani d ? H1C202 0.3310 0.5384 0.3902 1.0 0.034 . Uani d ? H1C203 0.2957 0.7035 0.3765 1.0 0.043 . Uani d ? H1C204 0.3259 0.7890 0.2974 1.0 0.046 . Uani d ? H1C205 0.3907 0.7053 0.2344 1.0 0.042 . Uani d ? H1C207 0.5275 0.5539 0.2429 1.0 0.035 . Uani d ? H2C207 0.4138 0.5311 0.2084 1.0 0.038 . Uani d ? H1C208 0.1432 0.1499 0.3736 1.0 0.035 . Uani d ? H1C209 -0.0452 -0.0182 0.3482 1.0 0.049 . Uani d ? H1C210 -0.1017 -0.0344 0.2651 1.0 0.056 . Uani d ? H1C211 0.0338 0.1196 0.2102 1.0 0.049 . Uani d ? H1C213 0.2262 0.3810 0.2260 1.0 0.035 . Uani d ? H2C213 0.2560 0.2846 0.1988 1.0 0.039 . Uani d ? H1C214 0.6015 0.3763 0.3747 1.0 0.033 . Uani d ? H1C215 0.7952 0.4090 0.3499 1.0 0.044 . Uani d ? H1C216 0.8353 0.4076 0.2657 1.0 0.051 . Uani d ? H1C217 0.6787 0.3733 0.2092 1.0 0.047 . Uani d ? H1C219 0.3967 0.2441 0.2237 1.0 0.036 . Uani d ? H2C219 0.4836 0.3742 0.1970 1.0 0.040 . Uani d ? H1O1 -0.0070 -0.3297 0.4242 1.0 0.108 . Uani d ? H2O1 0.0921 -0.3478 0.4553 1.0 0.108 . Uani d ? H1O2 -0.0323 -0.1746 0.4004 1.0 0.165 . Uani d ? H2O2 -0.0071 -0.2195 0.3489 1.0 0.165 . Uani d ? H1O3 -0.1504 -0.5184 0.4452 1.0 0.100 . Uani d ? H2O3 -0.2865 -0.5597 0.4656 1.0 0.100 . Uani d ? H1O4 0.2717 0.6611 0.4699 1.0 0.067 . Uani d ? H2O4 0.3021 0.7929 0.4919 1.0 0.067 . Uani d ? H1O5 0.7573 0.6799 0.5143 1.0 0.063 . Uani d ? H2O5 0.7688 0.8072 0.5334 1.0 0.063 . Uani d ? H1O6 0.3866 -0.0251 0.5360 1.0 0.060 . Uani d ? H2O6 0.4398 -0.0954 0.5669 1.0 0.060 . Uani d ? H1O7 -0.0194 -0.0043 0.4512 1.0 0.074 . Uani d ? H2O7 -0.1204 -0.1449 0.4645 1.0 0.074 . Uani d ? H1O8 0.0136 0.2287 0.5343 1.0 0.079 . Uani d ? H2O8 -0.1184 0.1966 0.5566 1.0 0.079 . Uani 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 CU1 0.0315(4) 0.0334(5) 0.0147(3) 0.0168(4) 0.0011(4) 0.0007(3) CU2 0.0315(4) 0.0334(5) 0.0147(3) 0.0168(4) 0.0011(4) 0.0007(3) FE1 0.028(1) 0.025(1) 0.014(1) 0.012(1) 0.000(1) 0.000(1) C101 0.025(3) 0.028(3) 0.022(3) 0.013(2) -0.004(2) 0.001(2) N11 0.042(3) 0.038(3) 0.021(2) 0.021(2) 0.000(2) 0.001(2) C201 0.025(3) 0.028(3) 0.022(3) 0.013(2) -0.004(2) 0.001(2) N21 0.042(3) 0.038(3) 0.021(2) 0.021(2) 0.000(2) 0.001(2) C301 0.043(3) 0.031(3) 0.021(3) 0.018(3) -0.002(2) -0.003(2) N31 0.086(5) 0.047(3) 0.037(3) 0.043(3) -0.006(3) -0.005(2) C401 0.043(3) 0.031(3) 0.021(3) 0.018(3) -0.002(2) -0.003(2) N41 0.086(5) 0.047(3) 0.037(3) 0.043(3) -0.006(3) -0.005(2) C501 0.037(4) 0.030(3) 0.022(3) 0.013(3) -0.002(2) 0.006(2) N51 0.042(4) 0.052(3) 0.053(3) 0.008(3) -0.008(3) 0.014(3) C601 0.037(4) 0.030(3) 0.022(3) 0.013(3) -0.002(2) 0.006(2) N61 0.042(4) 0.052(3) 0.053(3) 0.008(3) -0.008(3) 0.014(3) N15 0.037(1) 0.037(1) 0.018(1) 0.020(1) 0.000(1) 0.000(1) N12 0.032(1) 0.031(1) 0.023(1) 0.016(1) 0.001(1) 0.001(1) C102 0.037(1) 0.033(1) 0.028(1) 0.019(1) 0.000(1) -0.002(1) C103 0.043(1) 0.034(1) 0.040(1) 0.021(1) -0.001(1) -0.001(1) C104 0.045(1) 0.036(1) 0.043(2) 0.023(1) 0.001(1) 0.006(1) C105 0.044(1) 0.039(1) 0.034(1) 0.023(1) 0.003(1) 0.010(1) C106 0.037(1) 0.035(1) 0.024(1) 0.019(1) 0.003(1) 0.005(1) C107 0.042(1) 0.041(1) 0.020(1) 0.022(1) 0.004(1) 0.005(1) N13 0.030(1) 0.032(1) 0.026(1) 0.014(1) 0.001(1) 0.001(1) C108 0.032(1) 0.034(1) 0.034(1) 0.015(1) 0.005(1) 0.006(1) C109 0.033(1) 0.035(1) 0.054(2) 0.013(1) 0.005(1) 0.008(1) C110 0.034(1) 0.034(1) 0.063(2) 0.011(1) -0.005(1) -0.001(1) C111 0.037(1) 0.037(1) 0.048(1) 0.015(1) -0.011(1) -0.008(1) C112 0.033(1) 0.034(1) 0.031(1) 0.016(1) -0.006(1) -0.004(1) C113 0.040(1) 0.040(1) 0.023(1) 0.021(1) -0.006(1) -0.004(1) N14 0.031(1) 0.034(1) 0.023(1) 0.017(1) 0.002(1) 0.001(1) C114 0.031(1) 0.036(1) 0.031(1) 0.017(1) 0.000(1) 0.001(1) C115 0.032(1) 0.043(1) 0.044(1) 0.021(1) 0.003(1) 0.003(1) C116 0.039(1) 0.050(1) 0.045(2) 0.026(1) 0.011(1) 0.005(1) C117 0.044(1) 0.049(1) 0.033(1) 0.028(1) 0.011(1) 0.003(1) C118 0.038(1) 0.040(1) 0.024(1) 0.022(1) 0.006(1) 0.001(1) C119 0.043(1) 0.042(1) 0.019(1) 0.024(1) 0.002(1) -0.002(1) N25 0.037(1) 0.037(1) 0.018(1) 0.020(1) 0.001(1) 0.001(1) N22 0.033(1) 0.031(1) 0.023(1) 0.016(1) 0.001(1) 0.000(1) C202 0.038(1) 0.035(1) 0.027(1) 0.020(1) 0.000(1) -0.003(1) C203 0.044(1) 0.037(1) 0.038(1) 0.024(1) 0.000(1) -0.003(1) C204 0.044(1) 0.035(1) 0.043(2) 0.023(1) 0.000(1) 0.002(1) C205 0.042(1) 0.036(1) 0.036(1) 0.021(1) 0.002(1) 0.007(1) C206 0.036(1) 0.033(1) 0.026(1) 0.018(1) 0.002(1) 0.004(1) C207 0.039(1) 0.039(1) 0.022(1) 0.021(1) 0.005(1) 0.007(1) N23 0.030(1) 0.032(1) 0.026(1) 0.014(1) -0.001(1) 0.000(1) C208 0.031(1) 0.033(1) 0.036(1) 0.014(1) 0.003(1) 0.004(1) C209 0.031(1) 0.035(1) 0.055(2) 0.012(1) 0.000(1) 0.003(1) C210 0.035(1) 0.038(1) 0.061(2) 0.013(1) -0.011(1) -0.006(1) C211 0.039(1) 0.041(1) 0.044(1) 0.018(1) -0.014(1) -0.010(1) C212 0.035(1) 0.036(1) 0.028(1) 0.017(1) -0.007(1) -0.004(1) C213 0.041(1) 0.041(1) 0.021(1) 0.022(1) -0.005(1) -0.003(1) N24 0.031(1) 0.033(1) 0.023(1) 0.016(1) 0.002(1) 0.001(1) C214 0.031(1) 0.036(1) 0.030(1) 0.017(1) -0.001(1) 0.001(1) C215 0.032(1) 0.042(1) 0.045(1) 0.020(1) 0.001(1) 0.003(1) C216 0.036(1) 0.049(1) 0.048(2) 0.024(1) 0.011(1) 0.007(1) C217 0.041(1) 0.049(1) 0.036(1) 0.026(1) 0.013(1) 0.006(1) C218 0.036(1) 0.040(1) 0.025(1) 0.021(1) 0.007(1) 0.003(1) C219 0.043(1) 0.043(1) 0.019(1) 0.024(1) 0.004(1) 0.001(1) CL1 0.063(4) 0.071(4) 0.049(2) 0.035(2) 0.003(1) 0.011(1) O11 0.157(7) 0.091(5) 0.075(3) 0.063(4) 0.027(4) 0.037(3) O12 0.273(11) 0.087(5) 0.123(7) 0.089(6) 0.043(6) -0.001(3) O13 0.104(7) 0.319(13) 0.116(6) 0.097(7) -0.043(4) 0.002(7) O14 0.097(4) 0.160(8) 0.088(4) 0.058(5) 0.041(4) 0.021(4) O1 0.131(9) 0.112(8) 0.094(7) 0.072(7) 0.035(6) 0.021(6) O2 0.216(14) 0.262(15) 0.095(8) 0.179(13) 0.020(9) 0.038(9) O3 0.116(8) 0.132(8) 0.063(5) 0.072(7) -0.023(5) -0.035(5) O4 0.099(6) 0.079(5) 0.056(4) 0.068(5) 0.013(4) 0.007(4) O5 0.056(4) 0.035(3) 0.082(5) 0.012(3) -0.021(4) 0.000(3) O6 0.055(4) 0.029(3) 0.096(5) 0.021(3) -0.008(4) 0.003(3) O7 0.072(5) 0.053(4) 0.073(5) 0.015(4) -0.008(4) -0.012(4) O8 0.087(6) 0.066(5) 0.070(5) 0.029(4) 0.013(4) -0.011(4) H1C102 0.041 0.036 0.027 0.021 -0.001 -0.005 H1C103 0.050 0.037 0.047 0.026 -0.002 -0.005 H1C104 0.052 0.038 0.054 0.026 0.002 0.009 H1C105 0.053 0.047 0.035 0.028 0.005 0.015 H1C107 0.051 0.050 0.020 0.029 0.002 0.006 H2C107 0.043 0.043 0.023 0.023 0.008 0.009 H1C108 0.037 0.038 0.030 0.018 0.009 0.009 H1C109 0.037 0.039 0.065 0.014 0.012 0.015 H1C110 0.037 0.036 0.083 0.010 -0.009 -0.003 H1C111 0.045 0.043 0.053 0.019 -0.020 -0.015 H1C113 0.049 0.047 0.025 0.027 -0.011 -0.008 H2C113 0.040 0.041 0.025 0.022 -0.007 -0.002 H1C114 0.033 0.037 0.030 0.018 -0.005 -0.001 H1C115 0.033 0.047 0.056 0.022 -0.001 0.002 H1C116 0.043 0.059 0.058 0.032 0.016 0.008 H1C117 0.056 0.060 0.034 0.037 0.015 0.003 H1C119 0.054 0.052 0.019 0.032 0.004 -0.002 H2C119 0.045 0.041 0.023 0.024 -0.002 -0.006 H1C202 0.042 0.039 0.025 0.023 0.001 -0.004 H1C203 0.052 0.042 0.044 0.030 0.000 -0.007 H1C204 0.051 0.038 0.055 0.027 0.000 0.004 H1C205 0.049 0.041 0.040 0.025 0.004 0.013 H1C207 0.039 0.039 0.027 0.020 0.008 0.009 H2C207 0.049 0.047 0.023 0.027 0.005 0.009 H1C208 0.034 0.036 0.033 0.016 0.008 0.008 H1C209 0.033 0.038 0.069 0.011 0.006 0.009 H1C210 0.038 0.041 0.080 0.013 -0.018 -0.010 H1C211 0.049 0.049 0.047 0.024 -0.022 -0.015 H1C213 0.043 0.043 0.023 0.024 -0.006 -0.001 H2C213 0.052 0.050 0.021 0.029 -0.008 -0.006 H1C214 0.034 0.038 0.029 0.019 -0.005 -0.001 H1C215 0.033 0.047 0.055 0.021 -0.004 0.001 H1C216 0.039 0.057 0.063 0.028 0.016 0.010 H1C217 0.052 0.060 0.038 0.034 0.019 0.009 H1C219 0.047 0.044 0.020 0.026 0.000 -0.004 H2C219 0.053 0.053 0.020 0.031 0.008 0.004 H1O1 0.131 0.112 0.094 0.072 0.035 0.021 H2O1 0.131 0.112 0.094 0.072 0.035 0.021 H1O2 0.216 0.262 0.095 0.179 0.020 0.038 H2O2 0.216 0.262 0.095 0.179 0.020 0.038 H1O3 0.116 0.132 0.063 0.072 -0.023 -0.035 H2O3 0.116 0.132 0.063 0.072 -0.023 -0.035 H1O4 0.099 0.079 0.056 0.068 0.013 0.007 H2O4 0.099 0.079 0.056 0.068 0.013 0.007 H1O5 0.056 0.035 0.082 0.012 -0.021 0.000 H2O5 0.056 0.035 0.082 0.012 -0.021 0.000 H1O6 0.055 0.029 0.096 0.021 -0.008 0.003 H2O6 0.055 0.029 0.096 0.021 -0.008 0.003 H1O7 0.072 0.053 0.073 0.015 -0.008 -0.012 H2O7 0.072 0.053 0.073 0.015 -0.008 -0.012 H1O8 0.087 0.066 0.070 0.029 0.013 -0.011 H2O8 0.087 0.066 0.070 0.029 0.013 -0.011 #------------------------------------------------------------------------------ _refine_special_details ; The structure was solved and refined by "standards methods". However some features of the final version of that model were unsatisfactory. The asymmetric unit of the ordered structure contains a cation with pseudo P-3m symmetry situated at 0.3513, 0.3271, 0.5000 creating a pseudo rhombohedral R-3m symmetry. This symmetry is broken by the locations of the equatorial CN ligands of the cation and by the location of the anion and water molecules. However a pseudo inversion at 1/3, 1/3, 0 also relates the 32 screw related molecules at 2/3, 0, 2/3 and 0, 2/3, 1/3. This pseudo inversion symmetry creates sufficient refinement inconsistencies in an unconstrained refinement (mismatched distances and Uij parameters across the pseudo inversion centre) to justify a refinement with constraints and restraints. This clearly demonstrated that such features were artifacts of an unconstrained pseudo centrosymmetric structure refinement. The program RAELS00 was used for the constrained refinement and in the final cycle 260 variables were used to refine the 3290 (out of 3937 merged reflections) considered reliably observed with I > 3\s(I). All Cl and O atoms were refined as unrestrained isolated atoms. However, the pseudo centrosymmetric cation was constrained to have 6 identical planar fragments, [N12, C102 to C107] etc, using a common set of refineable local coordinates defined relative to 6 individually refineble local orthonormal axial systems (Rae, 1975). Remaining differences in pseudo centrosymmetrically related bonds in the cation were restrained to approach zero. A 15 parameter rigid body TLX thermal parametrisations, Rae (1975), were used for the perchlorate anion. Two 12 parameter TL parameterisations were used for the [N12 to N15, C102 to C119] and [N22 to N25, C202 to C219] fragments. These were centred on Cu1 and Cu2 respectively and constrained to have equal parameterisations, Rae (1996). Pairs of pseudo centrometrically related atoms in the cation that were not included in the TL parameterisations, were constrained to have equal isolated anisotropic atom parameterisations. The water O were refined as isolated anisotropic atoms. Hydrogen atoms were relocated in geometrically sensible positions after each refinement cycle and given the same thermal parameters as the atoms to which they are attached. Standard deviations are calculated using the inverse of the matrix used for the least squares and assume the correctness of the various constraints and restraints. Water hydrogens were inserted according to the following Hydrogen bonding pattern. O2--H-O1-H--O4*, O7--H-O2-H--O13*, O1--H-O3-H--N61*, N31--H-O4-H--O6*, N61--H-O5-H--O12, N41--H-O6-H--O14*, N51--H-O7-H--O5*, N51--H-O8-H--O11* References (1) RAELS00, A.D. Rae (2000) Australian National University, Canberra, Australia. (2) Rae, A.D. (1975) Acta Cryst. A31, 560-570, 570-574. (3) Rae, A.D. (1996) Acta Cryst. A52, C44-C45. Table 1. Refinement Statistics. Class** Number R(F) R(F2) wR Gof 1 3290 0.044 0.068 0.061 1.41 2 647 0.353 0.579 0.314 0.94 Refinement was on F. ** 1 Reflections with Io > 3\s(Io). 2 Remaining reflections. weighting scheme w =1/(var(|Fobs|) + (0.03|Fobs|2)). Final refinement cycle Maximum shift/sigma = 0.2 This is caused by highly correlated parameters being considered in isolation. 260 variables were used for a structure with 108 non Hydrogen atom sites per asymmetric unit. Final density map +0.563 to -0.536 e \%A^-^3. The enantiomorphic structure in P31 was tested , but refined to give R(F) = 0.068 and Gof =2.28 for the reflections in Class 1. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.0009|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3290 _refine_ls_number_parameters 260 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.057 _refine_ls_R_factor_gt 0.044 _refine_ls_wR_factor_all 0.063 _refine_ls_wR_factor_ref 0.061 _refine_ls_goodness_of_fit_all 1.35 _refine_ls_goodness_of_fit_ref 1.41 _refine_ls_shift/su_max 0.2 _refine_ls_shift/su_mean 0.03 _refine_diff_density_min -0.54 _refine_diff_density_max 0.56 #------------------------------------------------------------------------------ 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 CU1 N11 1.932(4) . . yes CU1 N15 2.017(4) . . yes CU1 N12 2.099(3) . . yes CU1 N13 2.079(3) . . yes CU1 N14 2.043(3) . . yes CU2 N21 1.933(4) . . yes CU2 N25 2.016(4) . . yes CU2 N22 2.105(3) . . yes CU2 N23 2.071(3) . . yes CU2 N24 2.042(3) . . yes FE1 C101 1.921(5) . . yes FE1 C201 1.922(5) . . yes FE1 C301 1.955(7) . . yes FE1 C401 1.947(7) . . yes FE1 C501 1.933(8) . . yes FE1 C601 1.918(7) . . yes C101 N11 1.136(7) . . yes C201 N21 1.149(7) . . yes C301 N31 1.134(9) . . yes C401 N41 1.130(9) . . yes C501 N51 1.147(9) . . yes C601 N61 1.158(9) . . yes N15 C107 1.461(7) . . yes N15 C113 1.486(7) . . yes N15 C119 1.483(7) . . yes N12 C102 1.333(4) . . yes N12 C106 1.342(4) . . yes C102 C103 1.384(4) . . yes C103 C104 1.383(5) . . yes C104 C105 1.382(5) . . yes C105 C106 1.374(4) . . yes C106 C107 1.502(4) . . yes N13 C108 1.333(4) . . yes N13 C112 1.342(4) . . yes C108 C109 1.384(4) . . yes C109 C110 1.383(5) . . yes C110 C111 1.382(5) . . yes C111 C112 1.374(4) . . yes C112 C113 1.502(4) . . yes N14 C114 1.333(4) . . yes N14 C118 1.342(4) . . yes C114 C115 1.384(4) . . yes C115 C116 1.383(5) . . yes C116 C117 1.382(5) . . yes C117 C118 1.374(4) . . yes C118 C119 1.502(4) . . yes N25 C207 1.484(7) . . yes N25 C213 1.466(7) . . yes N25 C219 1.479(7) . . yes N22 C202 1.333(4) . . yes N22 C206 1.342(4) . . yes C202 C203 1.384(4) . . yes C203 C204 1.383(5) . . yes C204 C205 1.382(5) . . yes C205 C206 1.374(4) . . yes C206 C207 1.502(4) . . yes N23 C208 1.333(4) . . yes N23 C212 1.342(4) . . yes C208 C209 1.384(4) . . yes C209 C210 1.383(5) . . yes C210 C211 1.382(5) . . yes C211 C212 1.374(4) . . yes C212 C213 1.502(4) . . yes N24 C214 1.333(4) . . yes N24 C218 1.342(4) . . yes C214 C215 1.384(4) . . yes C215 C216 1.383(5) . . yes C216 C217 1.382(5) . . yes C217 C218 1.374(4) . . yes C218 C219 1.502(4) . . yes CL1 O11 1.362(9) . . yes CL1 O12 1.383(10) . . yes CL1 O13 1.362(11) . . yes CL1 O14 1.444(9) . . yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag N31 O4 2.805(9) . . yes N41 O6 2.798(9) . . yes N51 O7 2.864(10) . . yes N51 O8 3.180(12) . . yes N61 O3 3.217(13) . 1_665 yes N61 O5 2.883(9) . . yes O11 O8 3.155(13) . 1_665 yes O12 O5 3.036(15) . . yes O13 O2 2.957(16) . 3_665 yes O14 O6 3.041(13) . 1_565 yes O1 O2 2.684(16) . . yes O1 O3 2.839(14) . . yes O1 O4 2.902(13) . 1_545 yes O2 O7 2.802(15) . . yes O3 N61 3.217(13) . 1_445 yes O4 O6 2.836(10) . 1_565 yes O5 O7 2.816(10) . 1_665 yes O2 O13 2.957(16) . 2_654 yes O4 O1 2.902(13) . 1_565 yes O6 O14 3.041(13) . 1_545 yes O6 O4 2.836(10) . 1_545 yes O7 O5 2.816(10) . 1_445 yes O8 O11 3.155(13) . 1_445 yes #------------------------------------------------------------------------------ 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 N11 CU1 N15 178.2(2) . . . yes N11 CU1 N12 99.6(2) . . . yes N11 CU1 N13 95.8(2) . . . yes N11 CU1 N14 97.0(2) . . . yes N15 CU1 N12 82.2(2) . . . yes N15 CU1 N13 83.6(2) . . . yes N15 CU1 N14 82.0(2) . . . yes N12 CU1 N13 113.1(2) . . . yes N12 CU1 N14 117.2(2) . . . yes N13 CU1 N14 124.8(2) . . . yes N21 CU2 N25 178.6(2) . . . yes N21 CU2 N22 98.6(2) . . . yes N21 CU2 N23 98.1(2) . . . yes N21 CU2 N24 95.9(2) . . . yes N25 CU2 N22 82.0(2) . . . yes N25 CU2 N23 82.9(2) . . . yes N25 CU2 N24 82.7(2) . . . yes N22 CU2 N23 106.0(2) . . . yes N22 CU2 N24 118.7(2) . . . yes N23 CU2 N24 130.2(2) . . . yes C101 FE1 C201 179.4(3) . . . yes C101 FE1 C301 93.4(3) . . . yes C101 FE1 C401 84.8(3) . . . yes C101 FE1 C501 91.4(3) . . . yes C101 FE1 C601 90.2(3) . . . yes C201 FE1 C301 86.2(3) . . . yes C201 FE1 C401 95.5(3) . . . yes C201 FE1 C501 88.2(3) . . . yes C201 FE1 C601 90.2(3) . . . yes C301 FE1 C401 178.1(3) . . . yes C301 FE1 C501 88.9(3) . . . yes C301 FE1 C601 91.0(3) . . . yes C401 FE1 C501 90.4(3) . . . yes C401 FE1 C601 89.8(3) . . . yes C501 FE1 C601 178.4(3) . . . yes FE1 C101 N11 174.3(7) . . . yes CU1 N11 C101 172.2(6) . . . yes FE1 C201 N21 174.4(7) . . . yes CU2 N21 C201 172.6(6) . . . yes FE1 C301 N31 177.2(7) . . . yes FE1 C401 N41 176.0(7) . . . yes FE1 C501 N51 178.3(7) . . . yes FE1 C601 N61 178.9(7) . . . yes CU1 N15 C107 108.4(3) . . . yes CU1 N15 C113 108.1(3) . . . yes CU1 N15 C119 107.4(3) . . . yes C107 N15 C113 110.6(4) . . . yes C107 N15 C119 113.6(4) . . . yes C113 N15 C119 108.6(4) . . . yes CU1 N12 C102 128.0(3) . . . yes CU1 N12 C106 112.2(3) . . . yes C102 N12 C106 119.0(3) . . . yes N12 C102 C103 122.1(3) . . . yes C102 C103 C104 118.8(3) . . . yes C103 C104 C105 119.0(3) . . . yes C104 C105 C106 119.0(3) . . . yes N12 C106 C105 122.1(3) . . . yes N12 C106 C107 114.8(3) . . . yes C105 C106 C107 123.1(3) . . . yes N15 C107 C106 112.4(3) . . . yes CU1 N13 C108 125.7(2) . . . yes CU1 N13 C112 111.6(2) . . . yes C108 N13 C112 119.0(3) . . . yes N13 C108 C109 122.1(3) . . . yes C108 C109 C110 118.8(3) . . . yes C109 C110 C111 119.0(3) . . . yes C110 C111 C112 119.0(3) . . . yes N13 C112 C111 122.1(3) . . . yes N13 C112 C113 114.8(3) . . . yes C111 C112 C113 123.1(3) . . . yes N15 C113 C112 111.2(3) . . . yes CU1 N14 C114 127.1(3) . . . yes CU1 N14 C118 113.5(2) . . . yes C114 N14 C118 119.0(3) . . . yes N14 C114 C115 122.1(3) . . . yes C114 C115 C116 118.8(3) . . . yes C115 C116 C117 119.0(3) . . . yes C116 C117 C118 119.0(3) . . . yes N14 C118 C117 122.1(3) . . . yes N14 C118 C119 114.8(3) . . . yes C117 C118 C119 123.1(3) . . . yes N15 C119 C118 109.9(3) . . . yes CU2 N25 C207 107.7(3) . . . yes CU2 N25 C213 110.4(3) . . . yes CU2 N25 C219 107.7(3) . . . yes C207 N25 C213 110.8(4) . . . yes C207 N25 C219 110.5(4) . . . yes C213 N25 C219 109.7(4) . . . yes CU2 N22 C202 127.4(2) . . . yes CU2 N22 C206 111.8(2) . . . yes C202 N22 C206 119.0(3) . . . yes N22 C202 C203 122.1(3) . . . yes C202 C203 C204 118.8(3) . . . yes C203 C204 C205 119.0(3) . . . yes C204 C205 C206 119.0(3) . . . yes N22 C206 C205 122.1(3) . . . yes N22 C206 C207 114.8(3) . . . yes C205 C206 C207 123.1(3) . . . yes N25 C207 C206 110.1(3) . . . yes CU2 N23 C208 126.0(3) . . . yes CU2 N23 C212 113.8(3) . . . yes C208 N23 C212 119.0(3) . . . yes N23 C208 C209 122.1(3) . . . yes C208 C209 C210 118.8(3) . . . yes C209 C210 C211 119.0(3) . . . yes C210 C211 C212 119.0(3) . . . yes N23 C212 C211 122.1(3) . . . yes N23 C212 C213 114.8(3) . . . yes C211 C212 C213 123.1(3) . . . yes N25 C213 C212 113.9(3) . . . yes CU2 N24 C214 126.8(3) . . . yes CU2 N24 C218 113.2(3) . . . yes C214 N24 C218 119.0(3) . . . yes N24 C214 C215 122.1(3) . . . yes C214 C215 C216 118.8(3) . . . yes C215 C216 C217 119.0(3) . . . yes C216 C217 C218 119.0(3) . . . yes N24 C218 C217 122.1(3) . . . yes N24 C218 C219 114.8(3) . . . yes C217 C218 C219 123.1(3) . . . yes N25 C219 C218 110.4(3) . . . yes O11 CL1 O12 110.1(7) . . . yes O11 CL1 O13 109.2(9) . . . yes O11 CL1 O14 106.5(6) . . . yes O12 CL1 O13 115.7(10) . . . yes O12 CL1 O14 105.6(8) . . . yes O13 CL1 O14 109.3(8) . . . yes C301 N31 O4 173.7(8) . . . no C401 N41 O6 160.8(7) . . . no C501 N51 O7 141.6(7) . . . no C501 N51 O8 97.5(7) . . . no O7 N51 O8 120.7(3) . . . no C601 N61 O5 151.0(7) . . . no C601 N61 O3 104.6(7) . . 1_665 no O5 N61 O3 100.0(3) . . 1_665 no CL1 O11 O8 108.7(6) . . 1_665 no CL1 O12 O5 125.5(9) . . . no CL1 O13 O2 123.7(8) . . 3_665 no CL1 O14 O6 105.8(6) . . 1_565 no O2 O1 O3 103.4(5) . . . no O2 O1 O4 100.4(4) . . 1_545 no O3 O1 O4 154.1(5) . . 1_545 no O13 O2 O1 132.5(6) 2_654 . . no O13 O2 O7 120.7(5) 2_654 . . no O1 O2 O7 105.5(5) . . . no N61 O3 O1 100.4(4) 1_445 . . no N31 O4 O1 100.3(4) . . 1_565 no N31 O4 O6 105.0(3) . . 1_565 no O1 O4 O6 121.2(3) 1_565 . 1_565 no N61 O5 O12 93.4(4) . . . no N61 O5 O7 120.3(3) . . 1_665 no O12 O5 O7 106.5(3) . . 1_665 no N41 O6 O14 105.6(3) . . 1_545 no N41 O6 O4 108.6(3) . . 1_545 no O14 O6 O4 134.6(3) 1_545 . 1_545 no N51 O7 O5 97.9(3) . . 1_445 no O2 O7 O5 102.8(4) . . 1_445 no N51 O8 O11 97.2(3) . . 1_445 no N51 O8 O11 97.2(3) . . 1_445 no #------------------------------------------------------------------------------ #===END data_kev _database_code_CSD 187747 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H62 Cu2 Fe N23 O6' _chemical_formula_weight 1120.04 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' _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 9.8849(1) _cell_length_b 11.4809(1) _cell_length_c 23.8906(3) _cell_angle_alpha 90.392(1) _cell_angle_beta 98.007(1) _cell_angle_gamma 107.933(1) _cell_volume 2550.85(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 41594 _cell_measurement_theta_min 2.10 _cell_measurement_theta_max 30.05 _exptl_crystal_description rod _exptl_crystal_colour green _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.075 _exptl_crystal_size_min 0.075 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.458 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1166 _exptl_absorpt_coefficient_mu 1.174 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41594 _diffrn_reflns_av_R_equivalents 0.0380 _diffrn_reflns_av_sigmaI/netI 0.0591 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 30.05 _reflns_number_total 13921 _reflns_number_gt 10336 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997a)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997b)' _computing_molecular_graphics 'ORTEP-III (Burnett and Johnson, 1996)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997b)' _publ_section_references ; Burnett, M. N. & Johnson, C. K. (1996). ORTEPIII. Report ORNL-6895. Oak Ridge National Laboratory, Tennessee, USA. Hooft, R. (1998). COLLECT Software. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods Enzymol. 276, 307--326. Sheldrick, G. M. (1997a). SHELXS97. Program for the Solution of Crystal Structures. University of Gottingen, Germany. Sheldrick, G. M. (1997b). SHELXL97. Program for the Refinement of Crystal Structures. University of Gottingen, Germany. Siemens (1994). XPREP. Version 5.03. Siemens Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. ; _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^)+(0.0671P)^2^+3.8989P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13921 _refine_ls_number_parameters 673 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0796 _refine_ls_R_factor_gt 0.0525 _refine_ls_wR_factor_ref 0.1466 _refine_ls_wR_factor_gt 0.1340 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.85321(4) 0.54548(3) 0.248926(17) 0.01712(10) Uani 1 1 d . . . Cu1 Cu 0.51365(4) 0.73301(3) 0.133460(16) 0.02124(10) Uani 1 1 d . . . Cu2 Cu 1.16124(4) 0.90597(3) 0.370414(15) 0.01837(9) Uani 1 1 d . . . C1 C 0.7202(3) 0.6279(3) 0.21666(14) 0.0237(6) Uani 1 1 d . . . N1 N 0.6424(3) 0.6757(3) 0.19461(14) 0.0344(7) Uani 1 1 d . . . C2 C 0.9943(3) 0.7022(3) 0.27245(12) 0.0192(5) Uani 1 1 d . . . N2 N 1.0762(3) 0.7961(2) 0.28806(11) 0.0245(5) Uani 1 1 d . . . C3 C 0.9914(3) 0.4636(3) 0.27710(15) 0.0277(7) Uani 1 1 d . . . N3 N 1.0744(3) 0.4148(3) 0.29267(16) 0.0414(8) Uani 1 1 d . . . C4 C 0.7076(3) 0.3892(3) 0.22634(13) 0.0223(6) Uani 1 1 d . . . N4 N 0.6205(3) 0.2970(2) 0.21203(12) 0.0280(6) Uani 1 1 d . . . C5 C 0.9144(3) 0.5476(3) 0.17552(15) 0.0299(7) Uani 1 1 d . . . N5 N 0.9487(4) 0.5494(3) 0.13085(14) 0.0480(9) Uani 1 1 d . . . C6 C 0.7895(3) 0.5446(3) 0.32213(14) 0.0236(6) Uani 1 1 d . . . N6 N 0.7511(3) 0.5448(3) 0.36572(13) 0.0361(7) Uani 1 1 d . . . N11 N 0.6571(3) 0.8974(2) 0.13666(12) 0.0256(6) Uani 1 1 d . . . C11 C 0.8050(3) 0.9204(3) 0.12504(19) 0.0401(9) Uani 1 1 d . . . H11A H 0.8464 0.8621 0.1459 0.048 Uiso 1 1 calc R . . H11B H 0.8019 0.9033 0.0841 0.048 Uiso 1 1 calc R . . C12 C 0.8977(6) 1.0417(4) 0.1402(4) 0.109(3) Uani 1 1 d . . . H12A H 0.9621 1.0360 0.1750 0.131 Uiso 1 1 calc R . . H12B H 0.9592 1.0645 0.1101 0.131 Uiso 1 1 calc R . . C13 C 0.8511(4) 1.1411(3) 0.1498(2) 0.0452(11) Uani 1 1 d . . . H13A H 0.8536 1.1892 0.1155 0.054 Uiso 1 1 calc R . . H13B H 0.9174 1.1949 0.1812 0.054 Uiso 1 1 calc R . . N12 N 0.7054(3) 1.1035(2) 0.16404(13) 0.0305(6) Uani 1 1 d . . . H12 H 0.6726 1.1584 0.1784 0.037 Uiso 1 1 calc R . . C14 C 0.6207(3) 0.9869(3) 0.15564(13) 0.0214(6) Uani 1 1 d . . . C15 C 0.4688(3) 0.9538(3) 0.16861(12) 0.0186(5) Uani 1 1 d . . . N13 N 0.3985(3) 0.8379(2) 0.16160(11) 0.0217(5) Uani 1 1 d . . . C16 C 0.2469(3) 0.7971(3) 0.16924(15) 0.0254(6) Uani 1 1 d . . . H16A H 0.2391 0.7705 0.2083 0.030 Uiso 1 1 calc R . . H16B H 0.1942 0.7256 0.1429 0.030 Uiso 1 1 calc R . . C17 C 0.1779(3) 0.8977(3) 0.15866(14) 0.0254(6) Uani 1 1 d . . . H17A H 0.0790 0.8703 0.1681 0.030 Uiso 1 1 calc R . . H17B H 0.1726 0.9167 0.1182 0.030 Uiso 1 1 calc R . . C18 C 0.2684(3) 1.0117(3) 0.19545(15) 0.0269(7) Uani 1 1 d . . . H18A H 0.2320 1.0813 0.1856 0.032 Uiso 1 1 calc R . . H18B H 0.2616 0.9963 0.2358 0.032 Uiso 1 1 calc R . . N14 N 0.4186(3) 1.0417(2) 0.18607(11) 0.0224(5) Uani 1 1 d . . . H14 H 0.4761 1.1177 0.1919 0.027 Uiso 1 1 calc R . . N21 N 0.4878(3) 0.6966(3) 0.04837(12) 0.0359(7) Uani 1 1 d . . . C21 C 0.5587(5) 0.7747(4) 0.00591(17) 0.0574(13) Uani 1 1 d . . . H21A H 0.6465 0.7544 0.0005 0.069 Uiso 1 1 calc R . . H21B H 0.5884 0.8615 0.0200 0.069 Uiso 1 1 calc R . . C22 C 0.4617(6) 0.7591(6) -0.0505(2) 0.083(2) Uani 1 1 d . . . H22A H 0.3827 0.7934 -0.0468 0.099 Uiso 1 1 calc R . . H22B H 0.5174 0.8048 -0.0791 0.099 Uiso 1 1 calc R . . C23 C 0.3995(6) 0.6255(6) -0.06968(19) 0.090(2) Uani 1 1 d . . . H23A H 0.3242 0.6150 -0.1030 0.108 Uiso 1 1 calc R . . H23B H 0.4757 0.5947 -0.0806 0.108 Uiso 1 1 calc R . . N22 N 0.3375(5) 0.5568(4) -0.02291(15) 0.0879(19) Uani 1 1 d . . . H22 H 0.2676 0.4870 -0.0305 0.105 Uiso 1 1 calc R . . C24 C 0.3847(4) 0.5976(4) 0.03099(15) 0.0460(11) Uani 1 1 d . . . C25 C 0.3153(4) 0.5242(3) 0.07721(15) 0.0366(8) Uani 1 1 d . . . N23 N 0.3628(3) 0.5733(2) 0.12762(11) 0.0253(5) Uani 1 1 d . . . C26 C 0.3073(4) 0.5054(3) 0.17587(14) 0.0294(7) Uani 1 1 d . . . H26A H 0.2291 0.5337 0.1867 0.035 Uiso 1 1 calc R . . H26B H 0.3852 0.5230 0.2086 0.035 Uiso 1 1 calc R . . C27 C 0.2508(4) 0.3686(3) 0.16195(17) 0.0399(9) Uani 1 1 d . . . H27A H 0.3316 0.3370 0.1577 0.048 Uiso 1 1 calc R . . H27B H 0.2022 0.3265 0.1931 0.048 Uiso 1 1 calc R . . C28 C 0.1470(5) 0.3432(4) 0.10813(18) 0.0511(12) Uani 1 1 d . . . H28A H 0.1171 0.2549 0.0966 0.061 Uiso 1 1 calc R . . H28B H 0.0602 0.3649 0.1138 0.061 Uiso 1 1 calc R . . N24 N 0.2156(4) 0.4156(3) 0.06406(14) 0.0561(11) Uani 1 1 d . . . H24 H 0.1910 0.3874 0.0285 0.067 Uiso 1 1 calc R . . N31 N 1.0077(3) 0.9831(2) 0.35494(10) 0.0194(5) Uani 1 1 d . . . C31 C 0.8527(3) 0.9176(3) 0.34937(14) 0.0247(6) Uani 1 1 d . . . H31A H 0.8179 0.9272 0.3855 0.030 Uiso 1 1 calc R . . H31B H 0.8355 0.8291 0.3413 0.030 Uiso 1 1 calc R . . C32 C 0.7695(3) 0.9667(3) 0.30211(14) 0.0276(7) Uani 1 1 d . . . H32A H 0.7959 0.9493 0.2652 0.033 Uiso 1 1 calc R . . H32B H 0.6649 0.9265 0.3010 0.033 Uiso 1 1 calc R . . C33 C 0.8058(3) 1.1035(3) 0.31315(15) 0.0298(7) Uani 1 1 d . . . H33A H 0.7576 1.1387 0.2816 0.036 Uiso 1 1 calc R . . H33B H 0.7723 1.1207 0.3486 0.036 Uiso 1 1 calc R . . N32 N 0.9620(3) 1.1580(2) 0.31806(12) 0.0258(6) Uani 1 1 d . . . H32 H 0.9989 1.2339 0.3086 0.031 Uiso 1 1 calc R . . C34 C 1.0491(3) 1.0926(3) 0.33701(12) 0.0192(5) Uani 1 1 d . . . C35 C 1.2086(3) 1.1455(3) 0.33476(12) 0.0196(6) Uani 1 1 d . . . N33 N 1.2807(2) 1.0699(2) 0.34756(10) 0.0187(5) Uani 1 1 d . . . C36 C 1.4371(3) 1.1117(3) 0.34623(13) 0.0222(6) Uani 1 1 d . . . H36A H 1.4561 1.0814 0.3102 0.027 Uiso 1 1 calc R . . H36B H 1.4852 1.0759 0.3775 0.027 Uiso 1 1 calc R . . C37 C 1.5008(3) 1.2503(3) 0.35173(14) 0.0265(7) Uani 1 1 d . . . H37A H 1.5025 1.2797 0.3909 0.032 Uiso 1 1 calc R . . H37B H 1.6009 1.2747 0.3436 0.032 Uiso 1 1 calc R . . C38 C 1.4120(3) 1.3084(3) 0.31075(17) 0.0315(7) Uani 1 1 d . . . H38A H 1.4456 1.3984 0.3182 0.038 Uiso 1 1 calc R . . H38B H 1.4237 1.2907 0.2714 0.038 Uiso 1 1 calc R . . N34 N 1.2602(3) 1.2587(2) 0.31782(12) 0.0245(5) Uani 1 1 d . . . H34 H 1.2030 1.3040 0.3108 0.029 Uiso 1 1 calc R . . N41 N 1.3059(3) 0.8184(2) 0.38262(11) 0.0205(5) Uani 1 1 d . . . C41 C 1.4091(3) 0.8157(3) 0.34455(14) 0.0250(6) Uani 1 1 d . . . H41A H 1.5064 0.8670 0.3618 0.030 Uiso 1 1 calc R . . H41B H 1.3836 0.8509 0.3084 0.030 Uiso 1 1 calc R . . C42 C 1.4107(4) 0.6855(3) 0.33273(14) 0.0299(7) Uani 1 1 d . . . H42A H 1.3167 0.6357 0.3118 0.036 Uiso 1 1 calc R . . H42B H 1.4862 0.6869 0.3093 0.036 Uiso 1 1 calc R . . C43 C 1.4405(4) 0.6302(4) 0.38866(16) 0.0382(8) Uani 1 1 d . . . H43A H 1.4294 0.5422 0.3823 0.046 Uiso 1 1 calc R . . H43B H 1.5403 0.6722 0.4069 0.046 Uiso 1 1 calc R . . N42 N 1.3387(3) 0.6442(3) 0.42519(12) 0.0319(6) Uani 1 1 d . . . H42 H 1.3162 0.5925 0.4519 0.038 Uiso 1 1 calc R . . C44 C 1.2796(3) 0.7340(3) 0.41863(13) 0.0215(6) Uani 1 1 d . . . C45 C 1.1653(3) 0.7380(3) 0.45402(12) 0.0208(6) Uani 1 1 d . . . N43 N 1.0915(3) 0.8093(2) 0.43623(10) 0.0205(5) Uani 1 1 d . . . C46 C 0.9811(3) 0.8207(3) 0.46930(13) 0.0248(6) Uani 1 1 d . . . H46A H 0.8870 0.7619 0.4531 0.030 Uiso 1 1 calc R . . H46B H 0.9730 0.9044 0.4665 0.030 Uiso 1 1 calc R . . C48 C 1.0429(4) 0.6739(3) 0.53566(14) 0.0299(7) Uani 1 1 d . . . H48A H 1.0797 0.6628 0.5753 0.036 Uiso 1 1 calc R . . H48B H 0.9517 0.6070 0.5239 0.036 Uiso 1 1 calc R . . C47 C 1.0160(4) 0.7963(3) 0.53149(14) 0.0292(7) Uani 1 1 d . . . H47A H 1.1025 0.8620 0.5495 0.035 Uiso 1 1 calc R . . H47B H 0.9348 0.7959 0.5516 0.035 Uiso 1 1 calc R . . N44 N 1.1482(3) 0.6687(2) 0.49892(11) 0.0265(6) Uani 1 1 d . . . H44 H 1.2006 0.6196 0.5065 0.032 Uiso 1 1 calc R . . N51 N 0.4047(6) 0.0515(5) 0.5100(3) 0.052(2) Uani 0.50 1 d PD . . O51 O 0.4974(8) 0.1024(7) 0.4830(3) 0.0583(17) Uani 0.50 1 d P . . O52 O 0.3935(8) -0.0493(6) 0.5298(3) 0.074(2) Uani 0.50 1 d P . . O53 O 0.3187(6) 0.1021(4) 0.5112(3) 0.0439(14) Uani 0.50 1 d PD . . N61 N 0.0000 0.0000 0.0000 0.105(3) Uani 1 2 d S . . O61 O 0.1296(9) 0.0601(8) 0.0330(4) 0.074(2) Uani 0.50 1 d P . . O62 O -0.037(2) -0.1059(10) -0.0010(6) 0.129(5) Uani 0.50 1 d P . . O63 O -0.0764(13) 0.0849(14) -0.0123(6) 0.159(8) Uani 0.50 1 d P . . O1 O 0.6621(2) 0.4796(2) 0.46744(10) 0.0285(5) Uani 1 1 d . . . O2 O 0.3739(3) 0.3366(3) 0.46748(12) 0.0459(7) Uani 1 1 d . . . O3 O 0.8925(6) 0.6978(4) 0.0444(2) 0.0685(14) Uani 0.70 1 d P . . O4 O 1.0163(14) 0.6624(13) 0.0301(4) 0.075(4) Uani 0.30 1 d P . . 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 0.0162(2) 0.01248(18) 0.0224(2) 0.00158(15) 0.00517(15) 0.00290(15) Cu1 0.01752(18) 0.01448(17) 0.0294(2) -0.00022(14) 0.00179(14) 0.00237(14) Cu2 0.01660(17) 0.01726(17) 0.02313(19) 0.00443(13) 0.00558(13) 0.00679(14) C1 0.0213(15) 0.0177(13) 0.0292(16) 0.0012(12) 0.0023(12) 0.0023(12) N1 0.0283(15) 0.0262(14) 0.0443(18) 0.0046(12) -0.0068(12) 0.0073(12) C2 0.0191(14) 0.0205(14) 0.0198(14) 0.0023(11) 0.0051(10) 0.0080(12) N2 0.0239(13) 0.0207(12) 0.0278(14) -0.0025(10) 0.0055(10) 0.0046(11) C3 0.0240(16) 0.0174(14) 0.0421(19) 0.0035(13) 0.0094(13) 0.0049(12) N3 0.0325(16) 0.0278(15) 0.070(2) 0.0160(15) 0.0126(15) 0.0163(13) C4 0.0246(15) 0.0178(14) 0.0271(15) 0.0009(11) 0.0105(12) 0.0077(12) N4 0.0279(14) 0.0176(12) 0.0366(16) -0.0037(11) 0.0127(11) 0.0011(11) C5 0.0230(16) 0.0263(16) 0.0341(18) -0.0025(13) 0.0088(13) -0.0032(13) N5 0.0394(18) 0.056(2) 0.0360(18) -0.0092(15) 0.0163(14) -0.0079(16) C6 0.0211(15) 0.0167(13) 0.0304(17) 0.0013(11) 0.0055(12) 0.0014(11) N6 0.0388(17) 0.0324(15) 0.0337(16) 0.0020(12) 0.0151(13) 0.0020(13) N11 0.0151(12) 0.0180(12) 0.0431(16) -0.0032(11) 0.0048(10) 0.0040(10) C11 0.0159(16) 0.0331(18) 0.070(3) -0.0131(18) 0.0105(16) 0.0042(14) C12 0.050(3) 0.025(2) 0.268(10) -0.002(3) 0.098(5) 0.001(2) C13 0.0192(17) 0.0289(18) 0.082(3) -0.0159(19) 0.0215(18) -0.0060(14) N12 0.0176(13) 0.0165(12) 0.0550(19) -0.0073(12) 0.0127(12) -0.0012(10) C14 0.0134(13) 0.0169(13) 0.0312(16) 0.0006(11) 0.0025(11) 0.0013(11) C15 0.0161(13) 0.0176(13) 0.0210(14) 0.0021(10) 0.0022(10) 0.0039(11) N13 0.0153(12) 0.0153(11) 0.0335(14) 0.0016(10) 0.0046(10) 0.0030(9) C16 0.0165(14) 0.0197(14) 0.0384(18) 0.0008(12) 0.0087(12) 0.0013(12) C17 0.0152(14) 0.0249(15) 0.0361(18) 0.0006(13) 0.0051(12) 0.0059(12) C18 0.0182(15) 0.0227(15) 0.0401(19) -0.0021(13) 0.0089(12) 0.0049(12) N14 0.0163(12) 0.0152(11) 0.0346(15) -0.0021(10) 0.0077(10) 0.0018(9) N21 0.0338(16) 0.0318(15) 0.0264(15) 0.0049(12) 0.0022(12) -0.0116(13) C21 0.051(3) 0.058(3) 0.034(2) 0.0139(19) 0.0017(18) -0.024(2) C22 0.067(3) 0.100(4) 0.037(3) 0.035(3) -0.005(2) -0.032(3) C23 0.079(4) 0.112(5) 0.023(2) 0.011(2) -0.002(2) -0.046(3) N22 0.093(3) 0.088(3) 0.0202(17) -0.0061(18) 0.0054(18) -0.061(3) C24 0.045(2) 0.044(2) 0.0245(18) 0.0029(15) 0.0020(15) -0.0202(18) C25 0.040(2) 0.0265(17) 0.0272(17) -0.0016(13) 0.0070(14) -0.0135(15) N23 0.0269(13) 0.0171(12) 0.0273(14) 0.0015(10) 0.0050(10) -0.0003(10) C26 0.0358(18) 0.0232(15) 0.0272(17) 0.0044(12) 0.0112(13) 0.0034(14) C27 0.051(2) 0.0220(16) 0.047(2) 0.0097(15) 0.0251(18) 0.0047(16) C28 0.062(3) 0.0285(19) 0.045(2) -0.0025(16) 0.024(2) -0.0191(19) N24 0.066(2) 0.0406(19) 0.0313(18) -0.0066(14) 0.0128(16) -0.0304(17) N31 0.0170(12) 0.0197(11) 0.0231(12) 0.0033(9) 0.0059(9) 0.0068(10) C31 0.0180(14) 0.0240(15) 0.0325(17) 0.0048(12) 0.0067(12) 0.0060(12) C32 0.0172(14) 0.0343(17) 0.0292(17) 0.0057(13) 0.0037(12) 0.0051(13) C33 0.0200(15) 0.0366(18) 0.0371(19) 0.0132(14) 0.0051(13) 0.0143(14) N32 0.0198(13) 0.0250(13) 0.0358(15) 0.0099(11) 0.0057(10) 0.0107(11) C34 0.0203(14) 0.0207(13) 0.0183(13) 0.0009(11) 0.0042(10) 0.0083(11) C35 0.0204(14) 0.0186(13) 0.0199(14) -0.0004(11) 0.0052(10) 0.0053(11) N33 0.0151(11) 0.0174(11) 0.0230(12) -0.0002(9) 0.0024(9) 0.0045(9) C36 0.0146(13) 0.0214(14) 0.0286(16) 0.0020(12) 0.0032(11) 0.0029(11) C37 0.0200(15) 0.0231(15) 0.0344(18) -0.0027(13) 0.0071(12) 0.0025(12) C38 0.0257(16) 0.0197(15) 0.052(2) 0.0067(14) 0.0185(15) 0.0057(13) N34 0.0212(13) 0.0175(12) 0.0377(15) 0.0071(10) 0.0111(11) 0.0071(10) N41 0.0181(12) 0.0227(12) 0.0236(13) 0.0054(10) 0.0055(9) 0.0093(10) C41 0.0252(15) 0.0276(15) 0.0267(16) 0.0054(12) 0.0091(12) 0.0123(13) C42 0.0343(18) 0.0333(17) 0.0295(17) 0.0021(13) 0.0133(13) 0.0174(15) C43 0.052(2) 0.043(2) 0.038(2) 0.0122(16) 0.0218(17) 0.0344(18) N42 0.0421(17) 0.0341(15) 0.0329(16) 0.0153(12) 0.0179(12) 0.0256(13) C44 0.0216(14) 0.0231(14) 0.0218(14) 0.0022(11) 0.0053(11) 0.0091(12) C45 0.0227(14) 0.0194(13) 0.0209(14) 0.0028(11) 0.0062(11) 0.0063(12) N43 0.0213(12) 0.0222(12) 0.0213(12) 0.0036(9) 0.0064(9) 0.0099(10) C46 0.0277(16) 0.0279(15) 0.0241(15) 0.0029(12) 0.0109(12) 0.0130(13) C48 0.0341(18) 0.0334(17) 0.0273(17) 0.0106(13) 0.0140(13) 0.0137(15) C47 0.0347(18) 0.0338(17) 0.0242(16) 0.0034(13) 0.0104(13) 0.0155(15) N44 0.0315(14) 0.0268(13) 0.0274(14) 0.0102(11) 0.0105(11) 0.0150(12) N51 0.071(5) 0.037(4) 0.016(3) -0.014(3) 0.004(3) -0.028(4) O51 0.072(4) 0.077(5) 0.032(3) 0.003(3) 0.004(3) 0.034(4) O52 0.072(5) 0.038(3) 0.088(5) 0.013(3) -0.035(4) 0.001(3) O53 0.041(3) 0.013(2) 0.067(4) 0.005(2) -0.016(3) 0.004(2) N61 0.141(9) 0.085(7) 0.067(5) 0.014(5) 0.050(6) -0.013(7) O61 0.063(5) 0.079(5) 0.073(5) 0.025(4) 0.011(4) 0.011(4) O62 0.182(15) 0.056(7) 0.136(11) 0.000(6) 0.037(11) 0.014(8) O63 0.105(9) 0.146(12) 0.141(11) 0.103(9) -0.062(8) -0.051(8) O1 0.0349(13) 0.0289(11) 0.0262(12) 0.0088(9) 0.0089(9) 0.0142(10) O2 0.0464(16) 0.0459(16) 0.0462(17) -0.0093(13) 0.0095(12) 0.0148(13) O3 0.078(4) 0.053(3) 0.054(3) -0.006(2) -0.016(3) 0.003(3) O4 0.076(8) 0.105(10) 0.021(5) 0.003(5) 0.000(5) 0.000(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 Fe1 C1 1.927(3) . ? Fe1 C2 1.929(3) . ? Fe1 C5 1.931(3) . ? Fe1 C3 1.935(3) . ? Fe1 C6 1.939(3) . ? Fe1 C4 1.940(3) . ? Cu1 N23 1.965(2) . ? Cu1 N11 1.975(3) . ? Cu1 N21 2.037(3) . ? Cu1 N1 2.049(3) . ? Cu1 N13 2.060(2) . ? Cu2 N31 1.975(2) . ? Cu2 N41 1.978(2) . ? Cu2 N43 2.008(2) . ? Cu2 N33 2.014(2) . ? Cu2 N2 2.241(3) . ? C1 N1 1.149(4) . ? C2 N2 1.153(4) . ? C3 N3 1.153(4) . ? C4 N4 1.153(4) . ? C5 N5 1.162(5) . ? C6 N6 1.157(4) . ? N11 C14 1.288(4) . ? N11 C11 1.469(4) . ? C11 C12 1.424(6) . ? C12 C13 1.385(6) . ? C13 N12 1.460(4) . ? N12 C14 1.339(4) . ? C14 C15 1.508(4) . ? C15 N13 1.294(4) . ? C15 N14 1.341(4) . ? N13 C16 1.464(4) . ? C16 C17 1.518(4) . ? C17 C18 1.526(4) . ? C18 N14 1.468(4) . ? N21 C24 1.291(4) . ? N21 C21 1.465(5) . ? C21 C22 1.516(6) . ? C22 C23 1.507(8) . ? C23 N22 1.467(6) . ? N22 C24 1.336(5) . ? C24 C25 1.506(5) . ? C25 N23 1.288(4) . ? C25 N24 1.333(4) . ? N23 C26 1.470(4) . ? C26 C27 1.514(5) . ? C27 C28 1.495(6) . ? C28 N24 1.457(5) . ? N31 C34 1.292(4) . ? N31 C31 1.471(4) . ? C31 C32 1.518(4) . ? C32 C33 1.511(5) . ? C33 N32 1.464(4) . ? N32 C34 1.343(4) . ? C34 C35 1.514(4) . ? C35 N33 1.296(4) . ? C35 N34 1.331(4) . ? N33 C36 1.476(4) . ? C36 C37 1.518(4) . ? C37 C38 1.517(5) . ? C38 N34 1.467(4) . ? N41 C44 1.290(4) . ? N41 C41 1.465(4) . ? C41 C42 1.524(4) . ? C42 C43 1.515(5) . ? C43 N42 1.464(4) . ? N42 C44 1.333(4) . ? C44 C45 1.514(4) . ? C45 N43 1.291(4) . ? C45 N44 1.338(4) . ? N43 C46 1.470(4) . ? C46 C47 1.526(4) . ? C48 N44 1.466(4) . ? C48 C47 1.510(5) . ? N51 O53 1.171(3) . ? N51 O51 1.198(9) . ? N51 O52 1.232(9) . ? O51 O52 1.457(11) 2_656 ? O52 O51 1.457(11) 2_656 ? N61 O62 1.156(11) 2 ? N61 O62 1.156(11) . ? N61 O61 1.381(8) . ? N61 O61 1.381(8) 2 ? N61 O63 1.415(17) . ? N61 O63 1.415(17) 2 ? O61 O62 1.344(19) 2 ? O61 O63 1.633(19) 2 ? O62 O63 1.072(18) 2 ? O62 O61 1.344(19) 2 ? O63 O62 1.072(18) 2 ? O63 O61 1.633(19) 2 ? O3 O4 1.483(15) . ? 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 C1 Fe1 C2 89.75(12) . . ? C1 Fe1 C5 87.42(15) . . ? C2 Fe1 C5 91.99(13) . . ? C1 Fe1 C3 176.58(14) . . ? C2 Fe1 C3 90.05(13) . . ? C5 Fe1 C3 89.18(15) . . ? C1 Fe1 C6 91.68(13) . . ? C2 Fe1 C6 88.03(12) . . ? C5 Fe1 C6 179.09(14) . . ? C3 Fe1 C6 91.72(14) . . ? C1 Fe1 C4 89.33(13) . . ? C2 Fe1 C4 178.43(12) . . ? C5 Fe1 C4 89.25(13) . . ? C3 Fe1 C4 90.94(13) . . ? C6 Fe1 C4 90.72(12) . . ? N23 Cu1 N11 176.65(11) . . ? N23 Cu1 N21 80.79(11) . . ? N11 Cu1 N21 97.77(11) . . ? N23 Cu1 N1 91.90(11) . . ? N11 Cu1 N1 91.38(11) . . ? N21 Cu1 N1 126.81(14) . . ? N23 Cu1 N13 98.04(10) . . ? N11 Cu1 N13 79.88(10) . . ? N21 Cu1 N13 117.08(12) . . ? N1 Cu1 N13 116.11(12) . . ? N31 Cu2 N41 175.95(11) . . ? N31 Cu2 N43 98.20(10) . . ? N41 Cu2 N43 81.42(10) . . ? N31 Cu2 N33 81.50(10) . . ? N41 Cu2 N33 101.17(10) . . ? N43 Cu2 N33 144.49(10) . . ? N31 Cu2 N2 89.05(10) . . ? N41 Cu2 N2 87.36(10) . . ? N43 Cu2 N2 111.84(10) . . ? N33 Cu2 N2 103.67(10) . . ? N1 C1 Fe1 176.3(3) . . ? C1 N1 Cu1 161.9(3) . . ? N2 C2 Fe1 177.7(3) . . ? C2 N2 Cu2 137.2(2) . . ? N3 C3 Fe1 178.5(3) . . ? N4 C4 Fe1 178.8(3) . . ? N5 C5 Fe1 178.6(4) . . ? N6 C6 Fe1 179.5(3) . . ? C14 N11 C11 119.1(3) . . ? C14 N11 Cu1 116.4(2) . . ? C11 N11 Cu1 124.1(2) . . ? C12 C11 N11 114.5(3) . . ? C13 C12 C11 124.4(4) . . ? C12 C13 N12 112.1(3) . . ? C14 N12 C13 121.2(3) . . ? N11 C14 N12 125.4(3) . . ? N11 C14 C15 115.4(2) . . ? N12 C14 C15 119.2(3) . . ? N13 C15 N14 126.0(3) . . ? N13 C15 C14 114.1(2) . . ? N14 C15 C14 119.8(2) . . ? C15 N13 C16 118.5(2) . . ? C15 N13 Cu1 114.03(19) . . ? C16 N13 Cu1 127.24(19) . . ? N13 C16 C17 111.9(2) . . ? C16 C17 C18 108.8(3) . . ? N14 C18 C17 109.1(2) . . ? C15 N14 C18 120.3(2) . . ? C24 N21 C21 118.2(3) . . ? C24 N21 Cu1 113.3(2) . . ? C21 N21 Cu1 128.1(2) . . ? N21 C21 C22 112.2(3) . . ? C23 C22 C21 110.6(5) . . ? N22 C23 C22 108.5(4) . . ? C24 N22 C23 121.5(4) . . ? N21 C24 N22 125.9(3) . . ? N21 C24 C25 114.9(3) . . ? N22 C24 C25 119.2(3) . . ? N23 C25 N24 125.4(3) . . ? N23 C25 C24 115.0(3) . . ? N24 C25 C24 119.6(3) . . ? C25 N23 C26 119.0(3) . . ? C25 N23 Cu1 115.8(2) . . ? C26 N23 Cu1 125.1(2) . . ? N23 C26 C27 111.7(3) . . ? C28 C27 C26 109.4(3) . . ? N24 C28 C27 109.2(3) . . ? C25 N24 C28 120.4(3) . . ? C34 N31 C31 118.7(2) . . ? C34 N31 Cu2 114.62(19) . . ? C31 N31 Cu2 125.03(19) . . ? N31 C31 C32 111.0(2) . . ? C33 C32 C31 108.4(3) . . ? N32 C33 C32 108.1(3) . . ? C34 N32 C33 120.3(3) . . ? N31 C34 N32 125.3(3) . . ? N31 C34 C35 115.5(2) . . ? N32 C34 C35 119.0(3) . . ? N33 C35 N34 126.5(3) . . ? N33 C35 C34 114.2(2) . . ? N34 C35 C34 119.2(3) . . ? C35 N33 C36 118.7(2) . . ? C35 N33 Cu2 113.96(19) . . ? C36 N33 Cu2 127.29(19) . . ? N33 C36 C37 112.5(2) . . ? C38 C37 C36 110.1(3) . . ? N34 C38 C37 109.4(3) . . ? C35 N34 C38 120.3(3) . . ? C44 N41 C41 117.6(2) . . ? C44 N41 Cu2 114.2(2) . . ? C41 N41 Cu2 125.63(19) . . ? N41 C41 C42 111.6(3) . . ? C43 C42 C41 108.6(3) . . ? N42 C43 C42 108.7(3) . . ? C44 N42 C43 121.1(3) . . ? N41 C44 N42 126.2(3) . . ? N41 C44 C45 114.7(3) . . ? N42 C44 C45 119.0(3) . . ? N43 C45 N44 126.5(3) . . ? N43 C45 C44 114.5(3) . . ? N44 C45 C44 119.0(3) . . ? C45 N43 C46 117.8(2) . . ? C45 N43 Cu2 113.72(19) . . ? C46 N43 Cu2 128.11(19) . . ? N43 C46 C47 112.0(3) . . ? N44 C48 C47 109.4(3) . . ? C48 C47 C46 109.3(3) . . ? C45 N44 C48 120.6(3) . . ? O53 N51 O51 112.9(7) . . ? O53 N51 O52 123.3(7) . . ? O51 N51 O52 123.4(7) . . ? N51 O51 O52 122.6(7) . 2_656 ? N51 O52 O51 114.0(8) . 2_656 ? O62 N61 O62 180(3) 2 . ? O62 N61 O61 63.3(9) 2 . ? O62 N61 O61 116.7(9) . . ? O62 N61 O61 116.7(9) 2 2 ? O62 N61 O61 63.3(9) . 2 ? O61 N61 O61 180.0(13) . 2 ? O62 N61 O63 48.0(9) 2 . ? O62 N61 O63 132.0(9) . . ? O61 N61 O63 108.5(6) . . ? O61 N61 O63 71.5(6) 2 . ? O62 N61 O63 132.0(9) 2 2 ? O62 N61 O63 48.0(9) . 2 ? O61 N61 O63 71.5(6) . 2 ? O61 N61 O63 108.5(6) 2 2 ? O63 N61 O63 180.0(10) . 2 ? O62 O61 N61 50.2(6) 2 . ? O62 O61 O63 103.9(8) 2 2 ? N61 O61 O63 55.2(5) . 2 ? O63 O62 N61 78.8(13) 2 . ? O63 O62 O61 139.6(15) 2 2 ? N61 O62 O61 66.5(9) . 2 ? O62 O63 N61 53.3(10) 2 . ? O62 O63 O61 104.2(17) 2 2 ? N61 O63 O61 53.3(7) . 2 ? _diffrn_measured_fraction_theta_max 0.933 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.976 _refine_diff_density_min -1.010 _refine_diff_density_rms 0.102 #===END OF CIF