data_arc _publ_requested_journal 'Organometallics' _publ_contact_author_name 'Prof. A. R. Chakravarty' _publ_contact_author_address ;Department of Inorganic and Physical Chemistry Indian Institute of Science Bangalore 560 012. INDIA ; _publ_contact_author_email arc@ipc.iisc.ernet.in _publ_contact_author_phone 91-080-22932533 _publ_contact_author_fax 91-080-23600683 _publ_author_name ; Tridib K. Goswami, Sudarshan Gadadhar, Mithun Roy, Munirathinam Nethaji, Anjali A. Karande, Akhil R. Chakravarty ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H28 Cu1 F6 Fe1 N3 O2 P1 S1' _chemical_formula_sum 'C28 H28 Cu1 F6 Fe1 N3 O2 P1 S1' _chemical_absolute_configuration 'rm' _chemical_formula_weight 734.97 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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 10.790(5) _cell_length_b 11.048(5) _cell_length_c 14.823(5) _cell_angle_alpha 68.657(5) _cell_angle_beta 85.234(5) _cell_angle_gamma 64.677(5) _cell_volume 1482.1(11) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'block' _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.647 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 746 _exptl_absorpt_coefficient_mu 1.401 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.8388 _exptl_absorpt_correction_T_max 0.8726 _exptl_absorpt_process_details 'SADABS(Sheldrick,1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Bruker Smart CCD Area Detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20179 _diffrn_reflns_av_R_equivalents 0.0415 _diffrn_reflns_av_sigmaI/netI 0.0709 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9267 _reflns_number_gt 7444 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Smart' _computing_cell_refinement 'Bruker Smart' _computing_data_reduction 'Bruker Saint' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0904P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _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 0.000(16) _refine_ls_number_reflns 9267 _refine_ls_number_parameters 775 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0712 _refine_ls_R_factor_gt 0.0538 _refine_ls_wR_factor_ref 0.1457 _refine_ls_wR_factor_gt 0.1333 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _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 Cu1 Cu 0.34347(7) 1.45712(7) 0.95776(5) 0.0338(2) Uani 1 1 d . . . Fe1 Fe 0.84174(10) 1.20520(11) 0.98664(8) 0.0437(3) Uani 1 1 d . . . S1 S 0.0908(2) 1.5647(3) 0.86984(16) 0.0515(5) Uani 1 1 d . . . O1 O 0.3811(5) 1.6120(5) 0.8620(4) 0.0364(11) Uani 1 1 d . . . O2 O 0.4462(5) 1.6783(5) 0.7109(3) 0.0434(11) Uani 1 1 d . . . N1 N 0.2981(6) 1.5506(7) 1.0566(5) 0.0401(15) Uani 1 1 d . . . N2 N 0.3206(7) 1.2965(7) 1.0722(5) 0.0413(15) Uani 1 1 d . . . N3 N 0.4170(6) 1.3562(6) 0.8650(4) 0.0344(13) Uani 1 1 d . . . H3 H 0.3665 1.3085 0.8637 0.041 Uiso 1 1 calc R . . C1 C 0.2995(10) 1.6725(9) 1.0496(7) 0.062(2) Uani 1 1 d . . . H1 H 0.3347 1.7201 0.9963 0.074 Uiso 1 1 calc R . . C2 C 0.2469(10) 1.7329(10) 1.1241(7) 0.065(3) Uani 1 1 d . . . H2 H 0.2507 1.8174 1.1195 0.078 Uiso 1 1 calc R . . C3 C 0.1919(11) 1.6657(10) 1.2003(6) 0.068(3) Uani 1 1 d . . . H3A H 0.1530 1.7066 1.2466 0.081 Uiso 1 1 calc R . . C4 C 0.1942(9) 1.5323(10) 1.2092(6) 0.054(2) Uani 1 1 d . . . C5 C 0.1431(11) 1.4545(14) 1.2889(7) 0.083(4) Uani 1 1 d . . . H5 H 0.1010 1.4920 1.3361 0.100 Uiso 1 1 calc R . . C6 C 0.1578(11) 1.3177(16) 1.2951(7) 0.082(4) Uani 1 1 d . . . H6 H 0.1247 1.2653 1.3473 0.099 Uiso 1 1 calc R . . C7 C 0.2214(9) 1.2591(11) 1.2240(6) 0.055(2) Uani 1 1 d . . . C8 C 0.2484(12) 1.1174(13) 1.2316(7) 0.078(3) Uani 1 1 d . . . H8 H 0.2247 1.0573 1.2852 0.093 Uiso 1 1 calc R . . C9 C 0.3085(11) 1.0735(10) 1.1599(6) 0.060(2) Uani 1 1 d . . . H9 H 0.3282 0.9812 1.1636 0.072 Uiso 1 1 calc R . . C10 C 0.3414(9) 1.1637(9) 1.0810(6) 0.0475(19) Uani 1 1 d . . . H10 H 0.3802 1.1314 1.0310 0.057 Uiso 1 1 calc R . . C11 C 0.2622(7) 1.3412(9) 1.1438(5) 0.0387(18) Uani 1 1 d . . . C12 C 0.2504(7) 1.4828(9) 1.1350(6) 0.0421(19) Uani 1 1 d . . . C13 C 0.4128(7) 1.5960(7) 0.7802(5) 0.0327(16) Uani 1 1 d . . . C14 C 0.3967(7) 1.4708(7) 0.7697(5) 0.0301(15) Uani 1 1 d . . . H14 H 0.4671 1.4314 0.7290 0.036 Uiso 1 1 calc R . . C15 C 0.2548(6) 1.5293(7) 0.7175(5) 0.0356(15) Uani 1 1 d . . . H15A H 0.2606 1.5722 0.6483 0.043 Uiso 1 1 calc R . . H15B H 0.2335 1.4487 0.7274 0.043 Uiso 1 1 calc R . . C16 C 0.1364(8) 1.6389(8) 0.7476(6) 0.0437(19) Uani 1 1 d . . . H16A H 0.0567 1.6805 0.7020 0.052 Uiso 1 1 calc R . . H16B H 0.1603 1.7156 0.7440 0.052 Uiso 1 1 calc R . . C17 C 0.0033(10) 1.7298(12) 0.8952(8) 0.078(3) Uani 1 1 d . . . H17A H -0.0269 1.7079 0.9595 0.117 Uiso 1 1 calc R . . H17B H -0.0749 1.7956 0.8487 0.117 Uiso 1 1 calc R . . H17C H 0.0655 1.7727 0.8906 0.117 Uiso 1 1 calc R . . C18 C 0.5653(7) 1.2511(7) 0.8927(5) 0.0377(15) Uani 1 1 d . . . H18A H 0.5714 1.1660 0.9470 0.045 Uiso 1 1 calc R . . H18B H 0.6038 1.2221 0.8385 0.045 Uiso 1 1 calc R . . C19 C 0.6473(7) 1.3138(7) 0.9202(5) 0.0327(15) Uani 1 1 d . . . C20 C 0.6469(8) 1.3343(8) 1.0091(6) 0.0466(18) Uani 1 1 d . . . H20 H 0.5962 1.3096 1.0608 0.056 Uiso 1 1 calc R . . C21 C 0.7363(9) 1.3987(10) 1.0062(8) 0.065(2) Uani 1 1 d . . . H21 H 0.7558 1.4230 1.0554 0.078 Uiso 1 1 calc R . . C22 C 0.7910(9) 1.4194(9) 0.9139(8) 0.069(3) Uani 1 1 d . . . H22 H 0.8521 1.4610 0.8926 0.083 Uiso 1 1 calc R . . C23 C 0.7396(7) 1.3681(8) 0.8608(5) 0.0454(18) Uani 1 1 d . . . H23 H 0.7603 1.3684 0.7986 0.055 Uiso 1 1 calc R . . C24 C 0.8981(10) 0.9886(10) 1.0168(8) 0.078(3) Uani 1 1 d . . . H24 H 0.8436 0.9482 1.0058 0.094 Uiso 1 1 calc R . . C25 C 0.9840(9) 1.0376(10) 0.9528(7) 0.070(3) Uani 1 1 d . . . H25 H 0.9960 1.0333 0.8911 0.084 Uiso 1 1 calc R . . C26 C 1.0495(10) 1.0938(11) 0.9930(8) 0.067(3) Uani 1 1 d . . . H26 H 1.1105 1.1324 0.9633 0.080 Uiso 1 1 calc R . . C27 C 1.0047(11) 1.0806(13) 1.0891(8) 0.082(3) Uani 1 1 d . . . H27 H 1.0302 1.1090 1.1337 0.098 Uiso 1 1 calc R . . C28 C 0.9116(9) 1.0135(11) 1.1014(8) 0.078(3) Uani 1 1 d . . . H28 H 0.8672 0.9902 1.1572 0.093 Uiso 1 1 calc R . . Cu2 Cu 0.42380(7) 1.09912(7) 0.61525(5) 0.0338(2) Uani 1 1 d . . . Fe2 Fe -0.07577(10) 1.32400(11) 0.58405(7) 0.0405(3) Uani 1 1 d . . . S2 S 0.6750(2) 0.9282(2) 0.70814(15) 0.0471(5) Uani 1 1 d . . . O3 O 0.3824(5) 1.1888(5) 0.7126(4) 0.0366(12) Uani 1 1 d . . . O4 O 0.3218(5) 1.1524(5) 0.8651(3) 0.0427(12) Uani 1 1 d . . . N4 N 0.4447(6) 1.2657(6) 0.5133(4) 0.0317(13) Uani 1 1 d . . . N5 N 0.4716(7) 1.0206(7) 0.5064(5) 0.0418(15) Uani 1 1 d . . . N6 N 0.3418(5) 0.9691(5) 0.7042(4) 0.0280(12) Uani 1 1 d . . . H6A H 0.3896 0.8782 0.7045 0.034 Uiso 1 1 calc R . . C29 C 0.4118(9) 1.3946(8) 0.5141(6) 0.0452(19) Uani 1 1 d . . . H29 H 0.3719 1.4156 0.5678 0.054 Uiso 1 1 calc R . . C30 C 0.4342(10) 1.5021(9) 0.4373(6) 0.054(2) Uani 1 1 d . . . H30 H 0.4064 1.5933 0.4390 0.065 Uiso 1 1 calc R . . C31 C 0.4988(9) 1.4686(10) 0.3589(6) 0.058(2) Uani 1 1 d . . . H31 H 0.5205 1.5352 0.3090 0.070 Uiso 1 1 calc R . . C32 C 0.5305(8) 1.3351(9) 0.3563(5) 0.0452(19) Uani 1 1 d . . . C33 C 0.5920(11) 1.2905(11) 0.2771(8) 0.070(3) Uani 1 1 d . . . H33 H 0.6181 1.3519 0.2261 0.084 Uiso 1 1 calc R . . C34 C 0.6134(12) 1.1605(12) 0.2745(7) 0.075(3) Uani 1 1 d . . . H34 H 0.6535 1.1341 0.2226 0.090 Uiso 1 1 calc R . . C35 C 0.5732(10) 1.0652(10) 0.3530(7) 0.057(2) Uani 1 1 d . . . C36 C 0.5835(12) 0.9311(10) 0.3531(7) 0.070(3) Uani 1 1 d . . . H36 H 0.6221 0.8998 0.3027 0.084 Uiso 1 1 calc R . . C37 C 0.5370(11) 0.8516(9) 0.4266(7) 0.063(3) Uani 1 1 d . . . H37 H 0.5433 0.7646 0.4273 0.076 Uiso 1 1 calc R . . C38 C 0.4789(9) 0.8998(8) 0.5023(6) 0.049(2) Uani 1 1 d . . . H38 H 0.4442 0.8450 0.5515 0.059 Uiso 1 1 calc R . . C39 C 0.5155(8) 1.1037(8) 0.4319(5) 0.0318(16) Uani 1 1 d . . . C40 C 0.4974(8) 1.2362(8) 0.4360(6) 0.0396(18) Uani 1 1 d . . . C41 C 0.3531(7) 1.1143(7) 0.7943(5) 0.0291(15) Uani 1 1 d . . . C42 C 0.3609(6) 0.9713(7) 0.8015(4) 0.0246(14) Uani 1 1 d . . . H42 H 0.2882 0.9540 0.8407 0.030 Uiso 1 1 calc R . . C43 C 0.5019(7) 0.8515(7) 0.8530(5) 0.0377(15) Uani 1 1 d . . . H43A H 0.4946 0.8241 0.9225 0.045 Uiso 1 1 calc R . . H43B H 0.5194 0.7683 0.8369 0.045 Uiso 1 1 calc R . . C44 C 0.6272(9) 0.8842(9) 0.8307(6) 0.046(2) Uani 1 1 d . . . H44A H 0.7055 0.8013 0.8717 0.056 Uiso 1 1 calc R . . H44B H 0.6116 0.9638 0.8505 0.056 Uiso 1 1 calc R . . C45 C 0.7316(9) 0.7601(9) 0.6926(7) 0.063(2) Uani 1 1 d . . . H45A H 0.7617 0.7694 0.6287 0.095 Uiso 1 1 calc R . . H45B H 0.6569 0.7327 0.7006 0.095 Uiso 1 1 calc R . . H45C H 0.8065 0.6879 0.7403 0.095 Uiso 1 1 calc R . . C46 C 0.1964(7) 1.0243(7) 0.6709(5) 0.0349(14) Uani 1 1 d . . . H46A H 0.1523 0.9767 0.7220 0.042 Uiso 1 1 calc R . . H46B H 0.1919 1.0004 0.6148 0.042 Uiso 1 1 calc R . . C47 C 0.1181(7) 1.1851(7) 0.6439(5) 0.0341(15) Uani 1 1 d . . . C48 C 0.1218(7) 1.2898(8) 0.5554(6) 0.0452(18) Uani 1 1 d . . . H48 H 0.1655 1.2720 0.5018 0.054 Uiso 1 1 calc R . . C49 C 0.0489(9) 1.4248(9) 0.5621(8) 0.066(3) Uani 1 1 d . . . H49 H 0.0334 1.5124 0.5129 0.080 Uiso 1 1 calc R . . C50 C 0.0028(8) 1.4066(9) 0.6548(7) 0.057(2) Uani 1 1 d . . . H50 H -0.0474 1.4799 0.6781 0.069 Uiso 1 1 calc R . . C51 C 0.0448(7) 1.2598(8) 0.7069(5) 0.0416(16) Uani 1 1 d . . . H51 H 0.0282 1.2180 0.7708 0.050 Uiso 1 1 calc R . . C52 C -0.2357(11) 1.4538(14) 0.4805(9) 0.084(3) Uani 1 1 d . . . H52 H -0.2453 1.5415 0.4341 0.101 Uiso 1 1 calc R . . C53 C -0.2843(9) 1.4334(11) 0.5733(8) 0.068(3) Uani 1 1 d . . . H53 H -0.3329 1.5045 0.5988 0.081 Uiso 1 1 calc R . . C54 C -0.2452(9) 1.2846(12) 0.6205(8) 0.072(3) Uani 1 1 d . . . H54 H -0.2632 1.2400 0.6833 0.086 Uiso 1 1 calc R . . C55 C -0.1755(9) 1.2159(12) 0.5576(8) 0.077(3) Uani 1 1 d . . . H55 H -0.1383 1.1175 0.5711 0.092 Uiso 1 1 calc R . . C56 C -0.1706(8) 1.3210(14) 0.4694(7) 0.075(3) Uani 1 1 d . . . H56 H -0.1314 1.3047 0.4142 0.090 Uiso 1 1 calc R . . P1 P 1.0568(4) 1.8765(3) 0.4316(2) 0.0828(9) Uani 1 1 d . . . F1 F 1.1591(12) 1.8609(10) 0.3486(8) 0.166(5) Uani 1 1 d . . . F2 F 1.1043(13) 1.7184(9) 0.4787(8) 0.178(5) Uani 1 1 d . . . F3 F 0.9544(13) 1.882(2) 0.3652(10) 0.281(10) Uani 1 1 d . . . F4 F 1.015(2) 2.0327(11) 0.3871(14) 0.317(13) Uani 1 1 d . . . F5 F 1.156(3) 1.875(3) 0.4927(15) 0.382(16) Uani 1 1 d . . . F6 F 0.955(2) 1.8916(15) 0.5041(14) 0.312(13) Uani 1 1 d . . . P2 P 0.6901(3) 1.7104(3) 1.1518(2) 0.0714(8) Uani 1 1 d . . . F7 F 0.5892(15) 1.681(2) 1.1103(8) 0.231(7) Uani 1 1 d . . . F8 F 0.7801(14) 1.6951(13) 1.0659(7) 0.183(5) Uani 1 1 d . . . F9 F 0.7886(15) 1.7289(18) 1.2032(10) 0.213(6) Uani 1 1 d . . . F10 F 0.5909(10) 1.7321(9) 1.2359(6) 0.119(3) Uani 1 1 d . . . F11 F 0.6289(13) 1.8713(9) 1.1023(11) 0.243(9) Uani 1 1 d . . . F12 F 0.7539(11) 1.5459(11) 1.2128(8) 0.170(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0403(5) 0.0356(4) 0.0323(5) -0.0162(4) 0.0113(4) -0.0206(4) Fe1 0.0314(6) 0.0515(6) 0.0399(6) -0.0091(5) 0.0017(5) -0.0165(5) S1 0.0406(11) 0.0694(13) 0.0542(12) -0.0254(11) 0.0123(9) -0.0312(10) O1 0.043(3) 0.033(3) 0.047(3) -0.026(2) 0.014(2) -0.022(2) O2 0.056(3) 0.029(2) 0.047(3) -0.012(2) 0.017(2) -0.024(2) N1 0.036(4) 0.052(4) 0.041(4) -0.028(3) 0.012(3) -0.019(3) N2 0.042(4) 0.051(4) 0.039(4) -0.017(3) 0.011(3) -0.027(3) N3 0.038(3) 0.033(3) 0.040(3) -0.015(3) 0.006(3) -0.021(3) C1 0.067(6) 0.054(5) 0.077(7) -0.038(5) 0.011(5) -0.027(4) C2 0.079(7) 0.050(5) 0.061(6) -0.038(5) -0.008(5) -0.005(5) C3 0.074(6) 0.066(6) 0.029(4) -0.023(4) 0.004(4) 0.006(5) C4 0.050(5) 0.072(6) 0.027(4) -0.023(4) 0.005(4) -0.013(4) C5 0.067(6) 0.116(10) 0.036(5) -0.031(6) 0.021(4) -0.011(6) C6 0.065(7) 0.140(11) 0.030(5) -0.024(6) 0.029(5) -0.044(7) C7 0.056(5) 0.083(6) 0.032(4) -0.017(4) 0.010(4) -0.040(5) C8 0.094(8) 0.112(9) 0.048(6) -0.012(6) 0.017(5) -0.078(7) C9 0.085(6) 0.061(5) 0.047(5) -0.008(4) 0.012(5) -0.053(5) C10 0.064(5) 0.050(4) 0.037(4) -0.016(4) 0.016(4) -0.033(4) C11 0.023(4) 0.061(5) 0.025(4) -0.013(4) 0.009(3) -0.015(4) C12 0.022(4) 0.056(5) 0.041(4) -0.024(4) 0.009(3) -0.007(3) C13 0.032(4) 0.030(3) 0.041(4) -0.016(3) -0.004(3) -0.013(3) C14 0.037(4) 0.026(3) 0.026(4) -0.009(3) 0.002(3) -0.012(3) C15 0.035(4) 0.045(4) 0.033(4) -0.014(3) 0.000(3) -0.023(3) C16 0.034(4) 0.036(4) 0.053(5) -0.009(4) -0.003(4) -0.013(3) C17 0.043(5) 0.105(8) 0.084(7) -0.054(7) 0.014(5) -0.015(5) C18 0.042(4) 0.026(3) 0.038(4) -0.010(3) 0.003(3) -0.009(3) C19 0.026(3) 0.034(3) 0.036(4) -0.011(3) 0.002(3) -0.012(3) C20 0.042(4) 0.053(5) 0.045(4) -0.023(4) 0.006(3) -0.016(4) C21 0.053(5) 0.069(6) 0.086(7) -0.041(5) 0.003(5) -0.025(4) C22 0.046(5) 0.055(5) 0.102(8) -0.007(5) -0.019(5) -0.032(4) C23 0.042(4) 0.054(5) 0.040(4) -0.011(4) 0.004(3) -0.026(4) C24 0.079(7) 0.058(6) 0.094(8) -0.026(5) 0.044(6) -0.034(5) C25 0.055(5) 0.059(6) 0.064(6) -0.007(5) 0.004(5) -0.009(4) C26 0.040(5) 0.078(7) 0.071(7) -0.019(5) 0.019(5) -0.024(5) C27 0.054(7) 0.093(8) 0.065(7) -0.021(6) -0.020(6) -0.003(6) C28 0.045(5) 0.066(6) 0.074(7) 0.004(5) 0.016(5) -0.008(4) Cu2 0.0433(5) 0.0319(4) 0.0307(5) -0.0132(4) 0.0104(4) -0.0199(4) Fe2 0.0308(6) 0.0428(6) 0.0404(6) -0.0136(5) -0.0009(5) -0.0097(5) S2 0.0377(10) 0.0437(10) 0.0539(12) -0.0108(9) 0.0009(9) -0.0173(9) O3 0.048(3) 0.030(2) 0.042(3) -0.018(2) 0.011(2) -0.023(2) O4 0.066(3) 0.053(3) 0.037(3) -0.031(2) 0.017(2) -0.041(3) N4 0.038(3) 0.032(3) 0.025(3) -0.007(2) 0.001(3) -0.018(3) N5 0.044(4) 0.047(4) 0.033(4) -0.017(3) 0.005(3) -0.017(3) N6 0.029(3) 0.019(2) 0.038(3) -0.013(2) -0.001(2) -0.009(2) C29 0.055(5) 0.041(4) 0.035(4) -0.011(3) 0.004(3) -0.019(4) C30 0.067(5) 0.039(4) 0.058(5) -0.011(4) 0.003(4) -0.030(4) C31 0.065(6) 0.060(5) 0.033(5) 0.016(4) -0.005(4) -0.039(4) C32 0.046(4) 0.058(5) 0.028(4) 0.001(4) 0.010(3) -0.033(4) C33 0.079(7) 0.065(6) 0.058(6) -0.005(5) 0.011(5) -0.040(5) C34 0.073(7) 0.093(8) 0.041(6) -0.027(6) 0.023(5) -0.019(6) C35 0.065(6) 0.055(5) 0.043(5) -0.022(4) 0.009(4) -0.016(4) C36 0.109(8) 0.054(5) 0.040(5) -0.025(4) 0.024(5) -0.025(5) C37 0.090(7) 0.040(4) 0.061(6) -0.021(4) 0.002(5) -0.025(5) C38 0.067(6) 0.040(4) 0.038(4) -0.014(3) 0.006(4) -0.022(4) C39 0.034(4) 0.037(4) 0.014(3) -0.005(3) 0.000(3) -0.010(3) C40 0.030(4) 0.039(4) 0.034(4) -0.005(3) 0.001(3) -0.008(3) C41 0.023(3) 0.035(4) 0.032(4) -0.013(3) 0.005(3) -0.016(3) C42 0.026(3) 0.030(3) 0.017(3) -0.004(3) 0.006(3) -0.016(3) C43 0.035(4) 0.036(4) 0.038(4) -0.006(3) -0.003(3) -0.016(3) C44 0.050(5) 0.044(4) 0.040(4) -0.007(4) -0.006(4) -0.020(4) C45 0.055(5) 0.054(5) 0.069(6) -0.031(5) 0.001(4) -0.005(4) C46 0.041(4) 0.026(3) 0.040(4) -0.015(3) -0.001(3) -0.014(3) C47 0.027(4) 0.041(4) 0.041(4) -0.019(3) 0.007(3) -0.018(3) C48 0.027(4) 0.044(4) 0.048(4) -0.004(4) 0.006(3) -0.011(3) C49 0.053(5) 0.039(5) 0.089(7) -0.002(5) -0.006(5) -0.019(4) C50 0.048(5) 0.048(5) 0.077(6) -0.034(4) -0.012(4) -0.008(4) C51 0.041(4) 0.050(4) 0.034(4) -0.020(3) 0.000(3) -0.014(3) C52 0.050(7) 0.106(9) 0.083(9) -0.030(7) -0.016(6) -0.020(6) C53 0.024(5) 0.076(7) 0.087(8) -0.032(6) -0.010(5) -0.001(4) C54 0.051(5) 0.096(8) 0.083(7) -0.045(6) 0.011(5) -0.036(5) C55 0.062(6) 0.101(8) 0.104(8) -0.070(7) 0.020(6) -0.042(6) C56 0.036(4) 0.135(9) 0.062(6) -0.061(7) 0.006(4) -0.023(5) P1 0.111(3) 0.0562(15) 0.0627(17) -0.0076(13) 0.0077(17) -0.0313(16) F1 0.229(12) 0.121(7) 0.186(9) -0.088(7) 0.113(9) -0.098(8) F2 0.222(12) 0.074(5) 0.181(10) 0.017(6) 0.014(9) -0.067(6) F3 0.129(10) 0.44(3) 0.149(10) -0.016(13) -0.070(8) -0.072(12) F4 0.42(2) 0.075(6) 0.34(2) -0.050(9) 0.271(19) -0.062(10) F5 0.57(4) 0.52(4) 0.265(19) -0.10(2) -0.09(2) -0.43(4) F6 0.46(3) 0.188(13) 0.31(2) -0.126(13) 0.30(2) -0.181(17) P2 0.099(2) 0.0795(18) 0.0516(14) -0.0223(13) 0.0154(14) -0.0555(17) F7 0.224(13) 0.48(2) 0.142(8) -0.154(12) 0.050(8) -0.255(15) F8 0.239(12) 0.213(11) 0.121(7) -0.081(8) 0.119(8) -0.121(10) F9 0.240(14) 0.341(19) 0.205(11) -0.153(13) 0.038(10) -0.213(15) F10 0.161(7) 0.103(5) 0.100(5) -0.040(4) 0.050(5) -0.067(5) F11 0.191(11) 0.077(6) 0.280(15) 0.036(7) 0.138(11) -0.002(6) F12 0.146(8) 0.133(8) 0.154(8) 0.004(7) 0.037(7) -0.043(6) _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 Cu1 O1 1.959(5) . ? Cu1 N3 1.985(6) . ? Cu1 N1 2.001(6) . ? Cu1 N2 2.050(6) . ? Cu1 S1 2.690(3) . ? Fe1 C23 2.033(7) . ? Fe1 C26 2.034(10) . ? Fe1 C19 2.035(7) . ? Fe1 C27 2.036(10) . ? Fe1 C25 2.038(10) . ? Fe1 C28 2.042(9) . ? Fe1 C22 2.048(9) . ? Fe1 C20 2.057(8) . ? Fe1 C21 2.065(9) . ? Fe1 C24 2.078(9) . ? S1 C16 1.820(9) . ? S1 C17 1.823(10) . ? O1 C13 1.287(9) . ? O2 C13 1.245(9) . ? N1 C1 1.318(10) . ? N1 C12 1.332(10) . ? N2 C11 1.331(10) . ? N2 C10 1.343(10) . ? N3 C14 1.469(9) . ? N3 C18 1.501(9) . ? N3 H3 0.9100 . ? C1 C2 1.447(12) . ? C1 H1 0.9300 . ? C2 C3 1.355(14) . ? C2 H2 0.9300 . ? C3 C4 1.421(14) . ? C3 H3A 0.9300 . ? C4 C12 1.385(11) . ? C4 C5 1.414(15) . ? C5 C6 1.420(16) . ? C5 H5 0.9300 . ? C6 C7 1.413(14) . ? C6 H6 0.9300 . ? C7 C11 1.378(12) . ? C7 C8 1.426(14) . ? C8 C9 1.333(14) . ? C8 H8 0.9300 . ? C9 C10 1.368(12) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.471(12) . ? C13 C14 1.528(9) . ? C14 C15 1.533(9) . ? C14 H14 0.9800 . ? C15 C16 1.508(10) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C19 1.489(9) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.416(10) . ? C19 C23 1.451(10) . ? C20 C21 1.414(12) . ? C20 H20 0.9300 . ? C21 C22 1.423(13) . ? C21 H21 0.9300 . ? C22 C23 1.384(12) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 C25 1.401(13) . ? C24 C28 1.408(16) . ? C24 H24 0.9300 . ? C25 C26 1.397(14) . ? C25 H25 0.9300 . ? C26 C27 1.442(15) . ? C26 H26 0.9300 . ? C27 C28 1.449(17) . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? Cu2 O3 1.953(5) . ? Cu2 N4 1.999(6) . ? Cu2 N6 2.025(5) . ? Cu2 N5 2.030(6) . ? Cu2 S2 2.675(2) . ? Fe2 C47 2.022(7) . ? Fe2 C49 2.024(8) . ? Fe2 C52 2.027(11) . ? Fe2 C53 2.035(9) . ? Fe2 C48 2.036(7) . ? Fe2 C50 2.039(8) . ? Fe2 C54 2.042(9) . ? Fe2 C51 2.043(7) . ? Fe2 C55 2.061(9) . ? Fe2 C56 2.072(8) . ? S2 C45 1.786(8) . ? S2 C44 1.794(9) . ? O3 C41 1.295(8) . ? O4 C41 1.238(8) . ? N4 C29 1.317(9) . ? N4 C40 1.323(10) . ? N5 C38 1.327(10) . ? N5 C39 1.354(10) . ? N6 C46 1.472(8) . ? N6 C42 1.485(8) . ? N6 H6A 0.9100 . ? C29 C30 1.408(12) . ? C29 H29 0.9300 . ? C30 C31 1.390(13) . ? C30 H30 0.9300 . ? C31 C32 1.380(12) . ? C31 H31 0.9300 . ? C32 C40 1.429(10) . ? C32 C33 1.439(14) . ? C33 C34 1.369(15) . ? C33 H33 0.9300 . ? C34 C35 1.437(15) . ? C34 H34 0.9300 . ? C35 C39 1.398(11) . ? C35 C36 1.436(13) . ? C36 C37 1.341(13) . ? C36 H36 0.9300 . ? C37 C38 1.404(12) . ? C37 H37 0.9300 . ? C38 H38 0.9300 . ? C39 C40 1.415(10) . ? C41 C42 1.509(9) . ? C42 C43 1.544(9) . ? C42 H42 0.9800 . ? C43 C44 1.524(10) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? C46 C47 1.512(9) . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C47 C48 1.410(10) . ? C47 C51 1.434(9) . ? C48 C49 1.393(11) . ? C48 H48 0.9300 . ? C49 C50 1.396(13) . ? C49 H49 0.9300 . ? C50 C51 1.396(11) . ? C50 H50 0.9300 . ? C51 H51 0.9300 . ? C52 C56 1.396(16) . ? C52 C53 1.405(16) . ? C52 H52 0.9300 . ? C53 C54 1.410(14) . ? C53 H53 0.9300 . ? C54 C55 1.387(13) . ? C54 H54 0.9300 . ? C55 C56 1.413(15) . ? C55 H55 0.9300 . ? C56 H56 0.9300 . ? P1 F5 1.454(14) . ? P1 F6 1.471(12) . ? P1 F4 1.474(10) . ? P1 F2 1.486(8) . ? P1 F3 1.506(14) . ? P1 F1 1.590(10) . ? P2 F9 1.480(10) . ? P2 F7 1.490(10) . ? P2 F11 1.504(8) . ? P2 F8 1.550(9) . ? P2 F12 1.560(10) . ? P2 F10 1.592(8) . ? 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 Cu1 N3 85.1(2) . . ? O1 Cu1 N1 93.0(2) . . ? N3 Cu1 N1 171.6(3) . . ? O1 Cu1 N2 171.7(2) . . ? N3 Cu1 N2 99.8(2) . . ? N1 Cu1 N2 81.2(3) . . ? O1 Cu1 S1 91.74(16) . . ? N3 Cu1 S1 88.20(18) . . ? N1 Cu1 S1 100.01(19) . . ? N2 Cu1 S1 95.04(19) . . ? C23 Fe1 C26 119.1(4) . . ? C23 Fe1 C19 41.8(3) . . ? C26 Fe1 C19 154.4(4) . . ? C23 Fe1 C27 154.2(4) . . ? C26 Fe1 C27 41.5(4) . . ? C19 Fe1 C27 162.5(4) . . ? C23 Fe1 C25 108.3(3) . . ? C26 Fe1 C25 40.1(4) . . ? C19 Fe1 C25 120.3(4) . . ? C27 Fe1 C25 68.2(4) . . ? C23 Fe1 C28 162.3(4) . . ? C26 Fe1 C28 68.6(4) . . ? C19 Fe1 C28 124.7(4) . . ? C27 Fe1 C28 41.6(5) . . ? C25 Fe1 C28 66.4(4) . . ? C23 Fe1 C22 39.6(3) . . ? C26 Fe1 C22 108.5(4) . . ? C19 Fe1 C22 68.0(3) . . ? C27 Fe1 C22 120.8(4) . . ? C25 Fe1 C22 127.1(4) . . ? C28 Fe1 C22 156.9(5) . . ? C23 Fe1 C20 68.7(3) . . ? C26 Fe1 C20 163.8(4) . . ? C19 Fe1 C20 40.5(3) . . ? C27 Fe1 C20 125.6(4) . . ? C25 Fe1 C20 154.7(4) . . ? C28 Fe1 C20 108.4(4) . . ? C22 Fe1 C20 67.6(4) . . ? C23 Fe1 C21 68.1(4) . . ? C26 Fe1 C21 126.8(4) . . ? C19 Fe1 C21 68.1(3) . . ? C27 Fe1 C21 107.9(4) . . ? C25 Fe1 C21 164.1(4) . . ? C28 Fe1 C21 121.7(5) . . ? C22 Fe1 C21 40.5(4) . . ? C20 Fe1 C21 40.1(3) . . ? C23 Fe1 C24 125.2(4) . . ? C26 Fe1 C24 68.6(4) . . ? C19 Fe1 C24 106.5(4) . . ? C27 Fe1 C24 69.5(5) . . ? C25 Fe1 C24 39.8(4) . . ? C28 Fe1 C24 40.0(4) . . ? C22 Fe1 C24 162.3(5) . . ? C20 Fe1 C24 120.0(3) . . ? C21 Fe1 C24 155.0(4) . . ? C16 S1 C17 99.2(4) . . ? C16 S1 Cu1 95.5(3) . . ? C17 S1 Cu1 101.3(3) . . ? C13 O1 Cu1 114.2(4) . . ? C1 N1 C12 118.4(7) . . ? C1 N1 Cu1 128.5(6) . . ? C12 N1 Cu1 112.9(5) . . ? C11 N2 C10 117.1(7) . . ? C11 N2 Cu1 111.8(5) . . ? C10 N2 Cu1 130.7(5) . . ? C14 N3 C18 112.2(5) . . ? C14 N3 Cu1 105.2(4) . . ? C18 N3 Cu1 111.7(4) . . ? C14 N3 H3 109.2 . . ? C18 N3 H3 109.2 . . ? Cu1 N3 H3 109.2 . . ? N1 C1 C2 120.8(9) . . ? N1 C1 H1 119.6 . . ? C2 C1 H1 119.6 . . ? C3 C2 C1 119.6(9) . . ? C3 C2 H2 120.2 . . ? C1 C2 H2 120.2 . . ? C2 C3 C4 119.5(8) . . ? C2 C3 H3A 120.2 . . ? C4 C3 H3A 120.2 . . ? C12 C4 C5 122.0(10) . . ? C12 C4 C3 115.8(8) . . ? C5 C4 C3 122.1(9) . . ? C4 C5 C6 118.3(9) . . ? C4 C5 H5 120.8 . . ? C6 C5 H5 120.8 . . ? C7 C6 C5 121.6(10) . . ? C7 C6 H6 119.2 . . ? C5 C6 H6 119.2 . . ? C11 C7 C6 118.8(10) . . ? C11 C7 C8 117.8(8) . . ? C6 C7 C8 123.4(10) . . ? C9 C8 C7 118.3(8) . . ? C9 C8 H8 120.9 . . ? C7 C8 H8 120.9 . . ? C8 C9 C10 120.3(9) . . ? C8 C9 H9 119.9 . . ? C10 C9 H9 119.9 . . ? N2 C10 C9 123.3(8) . . ? N2 C10 H10 118.4 . . ? C9 C10 H10 118.4 . . ? N2 C11 C7 123.2(8) . . ? N2 C11 C12 115.5(7) . . ? C7 C11 C12 121.2(7) . . ? N1 C12 C4 125.8(8) . . ? N1 C12 C11 116.4(7) . . ? C4 C12 C11 117.8(8) . . ? O2 C13 O1 124.8(6) . . ? O2 C13 C14 120.5(6) . . ? O1 C13 C14 114.6(6) . . ? N3 C14 C13 110.8(5) . . ? N3 C14 C15 112.5(6) . . ? C13 C14 C15 108.3(5) . . ? N3 C14 H14 108.4 . . ? C13 C14 H14 108.4 . . ? C15 C14 H14 108.4 . . ? C16 C15 C14 116.6(6) . . ? C16 C15 H15A 108.1 . . ? C14 C15 H15A 108.1 . . ? C16 C15 H15B 108.1 . . ? C14 C15 H15B 108.1 . . ? H15A C15 H15B 107.3 . . ? C15 C16 S1 113.5(5) . . ? C15 C16 H16A 108.9 . . ? S1 C16 H16A 108.9 . . ? C15 C16 H16B 108.9 . . ? S1 C16 H16B 108.9 . . ? H16A C16 H16B 107.7 . . ? S1 C17 H17A 109.5 . . ? S1 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? S1 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 N3 111.8(5) . . ? C19 C18 H18A 109.3 . . ? N3 C18 H18A 109.3 . . ? C19 C18 H18B 109.3 . . ? N3 C18 H18B 109.3 . . ? H18A C18 H18B 107.9 . . ? C20 C19 C23 107.2(6) . . ? C20 C19 C18 125.9(6) . . ? C23 C19 C18 126.8(6) . . ? C20 C19 Fe1 70.6(4) . . ? C23 C19 Fe1 69.0(4) . . ? C18 C19 Fe1 126.6(5) . . ? C21 C20 C19 108.5(7) . . ? C21 C20 Fe1 70.3(5) . . ? C19 C20 Fe1 68.9(4) . . ? C21 C20 H20 125.7 . . ? C19 C20 H20 125.7 . . ? Fe1 C20 H20 126.7 . . ? C20 C21 C22 107.2(7) . . ? C20 C21 Fe1 69.6(5) . . ? C22 C21 Fe1 69.1(5) . . ? C20 C21 H21 126.4 . . ? C22 C21 H21 126.4 . . ? Fe1 C21 H21 126.4 . . ? C23 C22 C21 109.7(7) . . ? C23 C22 Fe1 69.6(5) . . ? C21 C22 Fe1 70.4(5) . . ? C23 C22 H22 125.2 . . ? C21 C22 H22 125.2 . . ? Fe1 C22 H22 126.4 . . ? C22 C23 C19 107.3(7) . . ? C22 C23 Fe1 70.8(5) . . ? C19 C23 Fe1 69.2(4) . . ? C22 C23 H23 126.3 . . ? C19 C23 H23 126.3 . . ? Fe1 C23 H23 125.3 . . ? C25 C24 C28 105.4(10) . . ? C25 C24 Fe1 68.6(6) . . ? C28 C24 Fe1 68.7(6) . . ? C25 C24 H24 127.3 . . ? C28 C24 H24 127.3 . . ? Fe1 C24 H24 127.0 . . ? C26 C25 C24 111.9(10) . . ? C26 C25 Fe1 69.8(6) . . ? C24 C25 Fe1 71.7(6) . . ? C26 C25 H25 124.1 . . ? C24 C25 H25 124.1 . . ? Fe1 C25 H25 126.1 . . ? C25 C26 C27 107.2(9) . . ? C25 C26 Fe1 70.1(6) . . ? C27 C26 Fe1 69.3(6) . . ? C25 C26 H26 126.4 . . ? C27 C26 H26 126.4 . . ? Fe1 C26 H26 125.8 . . ? C26 C27 C28 105.2(10) . . ? C26 C27 Fe1 69.2(6) . . ? C28 C27 Fe1 69.4(6) . . ? C26 C27 H27 127.4 . . ? C28 C27 H27 127.4 . . ? Fe1 C27 H27 125.6 . . ? C24 C28 C27 110.4(9) . . ? C24 C28 Fe1 71.4(6) . . ? C27 C28 Fe1 69.0(6) . . ? C24 C28 H28 124.8 . . ? C27 C28 H28 124.8 . . ? Fe1 C28 H28 126.4 . . ? O3 Cu2 N4 93.1(2) . . ? O3 Cu2 N6 85.1(2) . . ? N4 Cu2 N6 162.6(2) . . ? O3 Cu2 N5 174.7(2) . . ? N4 Cu2 N5 81.8(3) . . ? N6 Cu2 N5 100.1(2) . . ? O3 Cu2 S2 87.90(16) . . ? N4 Cu2 S2 104.58(17) . . ? N6 Cu2 S2 92.66(16) . . ? N5 Cu2 S2 92.50(19) . . ? C47 Fe2 C49 68.3(3) . . ? C47 Fe2 C52 159.1(4) . . ? C49 Fe2 C52 106.1(5) . . ? C47 Fe2 C53 159.6(4) . . ? C49 Fe2 C53 121.8(4) . . ? C52 Fe2 C53 40.5(4) . . ? C47 Fe2 C48 40.7(3) . . ? C49 Fe2 C48 40.1(3) . . ? C52 Fe2 C48 122.3(4) . . ? C53 Fe2 C48 157.7(4) . . ? C47 Fe2 C50 68.4(3) . . ? C49 Fe2 C50 40.2(4) . . ? C52 Fe2 C50 121.2(4) . . ? C53 Fe2 C50 106.9(4) . . ? C48 Fe2 C50 67.6(3) . . ? C47 Fe2 C54 124.7(4) . . ? C49 Fe2 C54 159.0(4) . . ? C52 Fe2 C54 67.5(5) . . ? C53 Fe2 C54 40.5(4) . . ? C48 Fe2 C54 160.2(4) . . ? C50 Fe2 C54 124.5(4) . . ? C47 Fe2 C51 41.3(3) . . ? C49 Fe2 C51 67.7(4) . . ? C52 Fe2 C51 157.1(4) . . ? C53 Fe2 C51 122.5(4) . . ? C48 Fe2 C51 68.2(3) . . ? C50 Fe2 C51 40.0(3) . . ? C54 Fe2 C51 109.9(4) . . ? C47 Fe2 C55 110.2(4) . . ? C49 Fe2 C55 158.4(4) . . ? C52 Fe2 C55 67.1(5) . . ? C53 Fe2 C55 67.3(4) . . ? C48 Fe2 C55 124.6(3) . . ? C50 Fe2 C55 161.0(4) . . ? C54 Fe2 C55 39.5(4) . . ? C51 Fe2 C55 126.4(4) . . ? C47 Fe2 C56 124.7(3) . . ? C49 Fe2 C56 121.8(5) . . ? C52 Fe2 C56 39.8(4) . . ? C53 Fe2 C56 67.4(4) . . ? C48 Fe2 C56 108.5(3) . . ? C50 Fe2 C56 156.6(4) . . ? C54 Fe2 C56 66.9(4) . . ? C51 Fe2 C56 162.2(4) . . ? C55 Fe2 C56 40.0(4) . . ? C45 S2 C44 101.4(4) . . ? C45 S2 Cu2 107.6(3) . . ? C44 S2 Cu2 98.8(3) . . ? C41 O3 Cu2 113.7(4) . . ? C29 N4 C40 119.0(6) . . ? C29 N4 Cu2 128.8(5) . . ? C40 N4 Cu2 112.1(5) . . ? C38 N5 C39 118.5(6) . . ? C38 N5 Cu2 130.8(5) . . ? C39 N5 Cu2 110.3(5) . . ? C46 N6 C42 113.3(5) . . ? C46 N6 Cu2 109.8(4) . . ? C42 N6 Cu2 103.9(4) . . ? C46 N6 H6A 109.9 . . ? C42 N6 H6A 109.9 . . ? Cu2 N6 H6A 109.9 . . ? N4 C29 C30 122.9(7) . . ? N4 C29 H29 118.5 . . ? C30 C29 H29 118.5 . . ? C31 C30 C29 118.4(8) . . ? C31 C30 H30 120.8 . . ? C29 C30 H30 120.8 . . ? C32 C31 C30 119.0(7) . . ? C32 C31 H31 120.5 . . ? C30 C31 H31 120.5 . . ? C31 C32 C40 118.0(7) . . ? C31 C32 C33 124.0(7) . . ? C40 C32 C33 118.0(8) . . ? C34 C33 C32 122.0(9) . . ? C34 C33 H33 119.0 . . ? C32 C33 H33 119.0 . . ? C33 C34 C35 119.3(9) . . ? C33 C34 H34 120.4 . . ? C35 C34 H34 120.4 . . ? C39 C35 C36 116.7(8) . . ? C39 C35 C34 120.3(9) . . ? C36 C35 C34 122.9(8) . . ? C37 C36 C35 119.4(8) . . ? C37 C36 H36 120.3 . . ? C35 C36 H36 120.3 . . ? C36 C37 C38 119.9(8) . . ? C36 C37 H37 120.0 . . ? C38 C37 H37 120.0 . . ? N5 C38 C37 122.4(8) . . ? N5 C38 H38 118.8 . . ? C37 C38 H38 118.8 . . ? N5 C39 C35 123.0(7) . . ? N5 C39 C40 116.6(6) . . ? C35 C39 C40 120.4(7) . . ? N4 C40 C39 117.7(7) . . ? N4 C40 C32 122.4(7) . . ? C39 C40 C32 119.9(7) . . ? O4 C41 O3 124.3(6) . . ? O4 C41 C42 119.5(6) . . ? O3 C41 C42 116.2(6) . . ? N6 C42 C41 111.5(5) . . ? N6 C42 C43 110.1(5) . . ? C41 C42 C43 108.9(5) . . ? N6 C42 H42 108.8 . . ? C41 C42 H42 108.8 . . ? C43 C42 H42 108.8 . . ? C44 C43 C42 117.8(6) . . ? C44 C43 H43A 107.9 . . ? C42 C43 H43A 107.9 . . ? C44 C43 H43B 107.9 . . ? C42 C43 H43B 107.9 . . ? H43A C43 H43B 107.2 . . ? C43 C44 S2 118.8(5) . . ? C43 C44 H44A 107.6 . . ? S2 C44 H44A 107.6 . . ? C43 C44 H44B 107.6 . . ? S2 C44 H44B 107.6 . . ? H44A C44 H44B 107.0 . . ? S2 C45 H45A 109.5 . . ? S2 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? S2 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? N6 C46 C47 113.1(5) . . ? N6 C46 H46A 109.0 . . ? C47 C46 H46A 109.0 . . ? N6 C46 H46B 109.0 . . ? C47 C46 H46B 109.0 . . ? H46A C46 H46B 107.8 . . ? C48 C47 C51 107.0(6) . . ? C48 C47 C46 125.3(6) . . ? C51 C47 C46 127.1(6) . . ? C48 C47 Fe2 70.2(4) . . ? C51 C47 Fe2 70.1(4) . . ? C46 C47 Fe2 131.9(5) . . ? C49 C48 C47 108.3(7) . . ? C49 C48 Fe2 69.5(5) . . ? C47 C48 Fe2 69.1(4) . . ? C49 C48 H48 125.9 . . ? C47 C48 H48 125.9 . . ? Fe2 C48 H48 127.1 . . ? C48 C49 C50 108.7(7) . . ? C48 C49 Fe2 70.4(5) . . ? C50 C49 Fe2 70.5(5) . . ? C48 C49 H49 125.7 . . ? C50 C49 H49 125.7 . . ? Fe2 C49 H49 125.1 . . ? C49 C50 C51 108.5(7) . . ? C49 C50 Fe2 69.3(5) . . ? C51 C50 Fe2 70.2(4) . . ? C49 C50 H50 125.7 . . ? C51 C50 H50 125.7 . . ? Fe2 C50 H50 126.4 . . ? C50 C51 C47 107.5(7) . . ? C50 C51 Fe2 69.8(4) . . ? C47 C51 Fe2 68.6(4) . . ? C50 C51 H51 126.2 . . ? C47 C51 H51 126.2 . . ? Fe2 C51 H51 126.9 . . ? C56 C52 C53 109.0(11) . . ? C56 C52 Fe2 71.9(6) . . ? C53 C52 Fe2 70.1(6) . . ? C56 C52 H52 125.5 . . ? C53 C52 H52 125.5 . . ? Fe2 C52 H52 124.1 . . ? C52 C53 C54 106.9(10) . . ? C52 C53 Fe2 69.5(6) . . ? C54 C53 Fe2 70.0(5) . . ? C52 C53 H53 126.5 . . ? C54 C53 H53 126.5 . . ? Fe2 C53 H53 125.5 . . ? C55 C54 C53 108.6(10) . . ? C55 C54 Fe2 71.0(5) . . ? C53 C54 Fe2 69.5(6) . . ? C55 C54 H54 125.7 . . ? C53 C54 H54 125.7 . . ? Fe2 C54 H54 125.4 . . ? C54 C55 C56 108.3(10) . . ? C54 C55 Fe2 69.5(5) . . ? C56 C55 Fe2 70.4(6) . . ? C54 C55 H55 125.8 . . ? C56 C55 H55 125.8 . . ? Fe2 C55 H55 125.8 . . ? C52 C56 C55 107.2(9) . . ? C52 C56 Fe2 68.4(6) . . ? C55 C56 Fe2 69.6(5) . . ? C52 C56 H56 126.4 . . ? C55 C56 H56 126.4 . . ? Fe2 C56 H56 127.2 . . ? F5 P1 F6 91.6(14) . . ? F5 P1 F4 85.4(14) . . ? F6 P1 F4 93.1(7) . . ? F5 P1 F2 92.0(11) . . ? F6 P1 F2 87.5(7) . . ? F4 P1 F2 177.4(13) . . ? F5 P1 F3 177.9(12) . . ? F6 P1 F3 89.7(12) . . ? F4 P1 F3 92.9(12) . . ? F2 P1 F3 89.7(10) . . ? F5 P1 F1 92.2(12) . . ? F6 P1 F1 176.2(12) . . ? F4 P1 F1 87.1(6) . . ? F2 P1 F1 92.5(6) . . ? F3 P1 F1 86.5(8) . . ? F9 P2 F7 173.8(8) . . ? F9 P2 F11 85.2(10) . . ? F7 P2 F11 99.0(11) . . ? F9 P2 F8 93.9(7) . . ? F7 P2 F8 90.6(7) . . ? F11 P2 F8 89.7(6) . . ? F9 P2 F12 90.7(8) . . ? F7 P2 F12 84.7(9) . . ? F11 P2 F12 174.3(8) . . ? F8 P2 F12 94.6(6) . . ? F9 P2 F10 88.1(6) . . ? F7 P2 F10 87.6(6) . . ? F11 P2 F10 88.2(5) . . ? F8 P2 F10 177.0(7) . . ? F12 P2 F10 87.6(5) . . ? _diffrn_measured_fraction_theta_max 0.958 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.958 _refine_diff_density_max 0.979 _refine_diff_density_min -0.391 _refine_diff_density_rms 0.087 #===END data_tg2_0m _publ_requested_journal 'Organometallics' _publ_contact_author_name 'Prof. A. R. Chakravarty' _publ_contact_author_address ;Department of Inorganic and Physical Chemistry Indian Institute of Science Bangalore 560 012. INDIA ; _publ_contact_author_email arc@ipc.iisc.ernet.in _publ_contact_author_phone 91-080-22932533 _publ_contact_author_fax 91-080-23600683 _publ_author_name ; Tridib K. Goswami, Sudarshan Gadadhar, Mithun Roy, Munirathinam Nethaji, Anjali A. Karande, Akhil R. Chakravarty ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H24 Cl Cu N3 O6 S' _chemical_formula_sum 'C24 H24 Cl Cu N3 O6 S' _chemical_formula_weight 581.51 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' 'S' 'S' 0.1246 0.1234 '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' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 7.4256(7) _cell_length_b 11.2727(10) _cell_length_c 29.133(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2438.6(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'needle' _exptl_crystal_colour 'blue' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.584 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1196 _exptl_absorpt_coefficient_mu 1.137 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.6916 _exptl_absorpt_correction_T_max 0.8044 _exptl_absorpt_process_details 'SADABS(Sheldrick,1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Bruker Smart CCD Area Detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20731 _diffrn_reflns_av_R_equivalents 0.0630 _diffrn_reflns_av_sigmaI/netI 0.1260 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.40 _diffrn_reflns_theta_max 30.59 _reflns_number_total 7357 _reflns_number_gt 3580 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker Smart' _computing_cell_refinement 'Bruker Smart' _computing_data_reduction 'Bruker Saint' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^ > 2\s(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^)+(0.1095P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(2) _refine_ls_number_reflns 7357 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1552 _refine_ls_R_factor_gt 0.0613 _refine_ls_wR_factor_ref 0.1905 _refine_ls_wR_factor_gt 0.1449 _refine_ls_goodness_of_fit_ref 0.861 _refine_ls_restrained_S_all 0.861 _refine_ls_shift/su_max 0.006 _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 Cu1 Cu 0.39587(7) 0.74415(6) 0.920393(19) 0.03585(18) Uani 1 1 d . . . S1 S 0.4439(2) 0.35936(13) 0.96024(6) 0.0586(5) Uani 1 1 d . . . O1 O 0.2748(5) 0.8201(3) 0.97127(12) 0.0396(8) Uani 1 1 d . . . O2 O 0.1416(5) 0.7838(3) 1.03755(13) 0.0433(9) Uani 1 1 d . . . N1 N 0.4631(6) 0.8975(4) 0.88896(15) 0.0395(10) Uani 1 1 d . . . N2 N 0.5220(6) 0.6733(4) 0.86653(15) 0.0400(10) Uani 1 1 d . . . N3 N 0.2207(6) 0.6105(4) 0.93568(15) 0.0378(10) Uani 1 1 d . . . H3 H 0.2728 0.5393 0.9293 0.045 Uiso 1 1 calc R . . C1 C 0.4317(8) 1.0085(5) 0.9021(2) 0.0500(15) Uani 1 1 d . . . H1 H 0.3811 1.0224 0.9308 0.060 Uiso 1 1 calc R . . C2 C 0.4740(9) 1.1076(6) 0.8730(3) 0.0620(18) Uani 1 1 d . . . H2 H 0.4538 1.1851 0.8827 0.074 Uiso 1 1 calc R . . C3 C 0.5457(9) 1.0838(6) 0.8302(2) 0.0605(18) Uani 1 1 d . . . H3A H 0.5723 1.1465 0.8105 0.073 Uiso 1 1 calc R . . C4 C 0.5790(8) 0.9684(6) 0.81596(19) 0.0490(15) Uani 1 1 d . . . C5 C 0.6479(9) 0.9358(7) 0.7723(2) 0.0608(18) Uani 1 1 d . . . H5 H 0.6724 0.9955 0.7512 0.073 Uiso 1 1 calc R . . C6 C 0.6795(8) 0.8229(7) 0.7600(2) 0.0567(17) Uani 1 1 d . . . H6 H 0.7256 0.8058 0.7311 0.068 Uiso 1 1 calc R . . C7 C 0.6417(7) 0.7285(6) 0.79187(19) 0.0461(14) Uani 1 1 d . . . C8 C 0.6785(8) 0.6100(6) 0.7831(2) 0.0530(16) Uani 1 1 d . . . H8 H 0.7296 0.5875 0.7553 0.064 Uiso 1 1 calc R . . C9 C 0.6393(9) 0.5261(6) 0.8157(2) 0.0598(18) Uani 1 1 d . . . H9 H 0.6653 0.4465 0.8104 0.072 Uiso 1 1 calc R . . C10 C 0.5605(8) 0.5610(5) 0.8567(2) 0.0511(15) Uani 1 1 d . . . H10 H 0.5334 0.5031 0.8784 0.061 Uiso 1 1 calc R . . C11 C 0.5665(5) 0.7562(5) 0.83455(16) 0.0361(10) Uani 1 1 d . . . C12 C 0.5341(7) 0.8782(5) 0.84724(19) 0.0387(12) Uani 1 1 d . . . C13 C 0.1080(9) 0.6395(6) 0.8236(2) 0.0546(15) Uani 1 1 d . . . H13 H 0.1190 0.5574 0.8222 0.066 Uiso 1 1 calc R . . C14 C 0.1295(10) 0.7054(8) 0.7846(2) 0.067(2) Uani 1 1 d . . . H14 H 0.1587 0.6678 0.7572 0.081 Uiso 1 1 calc R . . C15 C 0.1086(11) 0.8265(9) 0.7853(4) 0.092(3) Uani 1 1 d . . . H15 H 0.1205 0.8699 0.7584 0.110 Uiso 1 1 calc R . . C16 C 0.0702(11) 0.8834(7) 0.8256(4) 0.079(3) Uani 1 1 d . . . H16 H 0.0570 0.9654 0.8261 0.095 Uiso 1 1 calc R . . C17 C 0.0510(9) 0.8181(6) 0.8659(3) 0.068(2) Uani 1 1 d . . . H17 H 0.0256 0.8566 0.8934 0.081 Uiso 1 1 calc R . . C18 C 0.0703(8) 0.6934(6) 0.8649(2) 0.0462(14) Uani 1 1 d . . . C19 C 0.0476(8) 0.6231(6) 0.9085(2) 0.0563(17) Uani 1 1 d . . . H19A H 0.0029 0.5447 0.9009 0.068 Uiso 1 1 calc R . . H19B H -0.0420 0.6617 0.9276 0.068 Uiso 1 1 calc R . . C20 C 0.1841(7) 0.6193(5) 0.98560(18) 0.0368(11) Uani 1 1 d . . . H20 H 0.0611 0.5917 0.9916 0.044 Uiso 1 1 calc R . . C21 C 0.1986(6) 0.7505(6) 0.99941(16) 0.0352(10) Uani 1 1 d . . . C22 C 0.3147(8) 0.5479(5) 1.0153(2) 0.0435(13) Uani 1 1 d . . . H22A H 0.4363 0.5751 1.0092 0.052 Uiso 1 1 calc R . . H22B H 0.2888 0.5640 1.0473 0.052 Uiso 1 1 calc R . . C23 C 0.3074(9) 0.4143(5) 1.0076(2) 0.0541(16) Uani 1 1 d . . . H23A H 0.1831 0.3919 1.0022 0.065 Uiso 1 1 calc R . . H23B H 0.3461 0.3751 1.0356 0.065 Uiso 1 1 calc R . . C24 C 0.6669(9) 0.3939(6) 0.9804(3) 0.076(2) Uani 1 1 d . . . H24A H 0.7537 0.3696 0.9579 0.114 Uiso 1 1 calc R . . H24B H 0.6891 0.3527 1.0087 0.114 Uiso 1 1 calc R . . H24C H 0.6768 0.4778 0.9854 0.114 Uiso 1 1 calc R . . Cl1 Cl 0.0119(3) 1.2656(2) 0.86447(7) 0.0768(5) Uani 1 1 d . . . O3 O 0.1565(15) 1.3393(9) 0.8556(4) 0.190(4) Uani 1 1 d . . . O4 O 0.024(2) 1.1983(11) 0.8266(4) 0.250(7) Uani 1 1 d . . . O5 O 0.0408(14) 1.1976(15) 0.8985(4) 0.301(9) Uani 1 1 d . . . O6 O -0.1539(14) 1.3119(9) 0.8645(5) 0.241(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0398(3) 0.0374(3) 0.0303(3) -0.0011(3) 0.0039(2) 0.0005(3) S1 0.0770(12) 0.0375(8) 0.0614(10) -0.0066(8) -0.0080(8) 0.0022(7) O1 0.048(2) 0.0334(19) 0.038(2) 0.0022(17) 0.0108(16) -0.0008(16) O2 0.047(2) 0.045(2) 0.038(2) -0.0038(16) 0.0072(16) -0.0036(16) N1 0.041(2) 0.039(3) 0.039(3) -0.002(2) 0.0005(19) 0.0019(19) N2 0.038(2) 0.046(3) 0.036(3) -0.002(2) -0.006(2) 0.006(2) N3 0.045(2) 0.034(2) 0.034(2) -0.0061(19) 0.0030(19) 0.0043(19) C1 0.063(4) 0.041(3) 0.045(3) -0.006(3) 0.005(3) 0.004(3) C2 0.067(4) 0.048(4) 0.071(5) 0.012(3) 0.004(4) 0.003(3) C3 0.071(4) 0.055(4) 0.055(4) 0.023(3) 0.001(3) -0.007(3) C4 0.047(4) 0.063(4) 0.038(3) 0.016(3) -0.003(3) -0.007(3) C5 0.055(4) 0.078(5) 0.049(4) 0.015(4) 0.008(3) -0.004(3) C6 0.049(3) 0.097(5) 0.024(3) 0.010(3) 0.003(2) -0.001(3) C7 0.036(3) 0.062(4) 0.040(3) -0.002(3) -0.002(2) 0.006(3) C8 0.060(4) 0.072(5) 0.027(3) -0.011(3) 0.008(3) 0.006(3) C9 0.058(4) 0.057(4) 0.065(5) -0.020(3) -0.004(3) 0.012(3) C10 0.060(4) 0.044(3) 0.049(4) -0.007(3) 0.002(3) 0.000(3) C11 0.030(2) 0.047(3) 0.031(2) -0.003(3) -0.0015(17) 0.002(3) C12 0.029(2) 0.051(3) 0.036(3) 0.007(3) -0.005(2) -0.001(2) C13 0.050(3) 0.068(4) 0.046(4) 0.003(3) -0.006(3) 0.011(3) C14 0.054(4) 0.107(6) 0.041(4) 0.003(4) 0.009(3) 0.014(4) C15 0.054(5) 0.119(8) 0.102(8) 0.044(7) -0.022(5) -0.009(5) C16 0.072(5) 0.060(5) 0.105(7) 0.013(5) -0.041(5) -0.002(4) C17 0.058(5) 0.059(4) 0.086(6) -0.027(4) -0.024(4) -0.002(3) C18 0.041(3) 0.057(4) 0.040(3) -0.004(3) -0.010(3) 0.000(3) C19 0.046(3) 0.077(5) 0.046(4) -0.005(3) -0.005(3) -0.011(3) C20 0.040(3) 0.040(3) 0.031(3) -0.001(2) 0.001(2) -0.001(2) C21 0.032(2) 0.040(3) 0.033(2) 0.002(3) -0.0019(19) 0.007(3) C22 0.055(3) 0.039(3) 0.037(3) 0.000(3) 0.001(3) -0.003(2) C23 0.059(4) 0.041(3) 0.062(4) 0.009(3) 0.004(3) 0.000(3) C24 0.073(5) 0.051(4) 0.104(6) -0.009(4) 0.001(4) 0.011(3) Cl1 0.0844(12) 0.0754(13) 0.0706(12) 0.0106(11) -0.0022(9) 0.0130(12) O3 0.176(9) 0.158(8) 0.236(11) 0.037(8) -0.016(8) -0.062(7) O4 0.331(18) 0.225(11) 0.193(11) -0.072(10) 0.063(12) -0.037(12) O5 0.165(8) 0.58(2) 0.158(9) 0.229(13) 0.022(7) 0.048(13) O6 0.155(8) 0.153(8) 0.416(19) 0.036(10) -0.025(10) 0.095(7) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Cu1 O1 1.934(3) . ? Cu1 N2 1.994(5) . ? Cu1 N1 2.019(5) . ? Cu1 N3 2.039(4) . ? Cu1 O2 2.220(4) 3_567 ? S1 C24 1.799(7) . ? S1 C23 1.822(6) . ? O1 C21 1.269(6) . ? O2 C21 1.247(6) . ? O2 Cu1 2.220(4) 3_467 ? N1 C1 1.329(7) . ? N1 C12 1.343(7) . ? N2 C10 1.329(7) . ? N2 C11 1.360(7) . ? N3 C20 1.483(7) . ? N3 C19 1.516(7) . ? C1 C2 1.437(8) . ? C2 C3 1.382(9) . ? C3 C4 1.388(9) . ? C4 C12 1.406(8) . ? C4 C5 1.420(9) . ? C5 C6 1.342(9) . ? C6 C7 1.439(9) . ? C7 C8 1.388(9) . ? C7 C11 1.398(7) . ? C8 C9 1.372(9) . ? C9 C10 1.387(8) . ? C11 C12 1.444(8) . ? C13 C14 1.368(9) . ? C13 C18 1.377(8) . ? C14 C15 1.374(11) . ? C15 C16 1.367(12) . ? C16 C17 1.392(11) . ? C17 C18 1.414(8) . ? C18 C19 1.507(8) . ? C20 C22 1.529(7) . ? C20 C21 1.536(9) . ? C22 C23 1.523(7) . ? Cl1 O5 1.271(9) . ? Cl1 O6 1.337(9) . ? Cl1 O4 1.342(11) . ? Cl1 O3 1.381(10) . ? 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 Cu1 N2 177.30(18) . . ? O1 Cu1 N1 94.78(16) . . ? N2 Cu1 N1 82.54(18) . . ? O1 Cu1 N3 82.15(16) . . ? N2 Cu1 N3 100.10(18) . . ? N1 Cu1 N3 152.76(18) . . ? O1 Cu1 O2 91.25(15) . 3_567 ? N2 Cu1 O2 89.51(16) . 3_567 ? N1 Cu1 O2 99.70(16) . 3_567 ? N3 Cu1 O2 107.40(16) . 3_567 ? C24 S1 C23 101.0(3) . . ? C21 O1 Cu1 115.4(4) . . ? C21 O2 Cu1 136.7(3) . 3_467 ? C1 N1 C12 118.8(5) . . ? C1 N1 Cu1 129.2(4) . . ? C12 N1 Cu1 111.6(4) . . ? C10 N2 C11 117.1(5) . . ? C10 N2 Cu1 130.7(4) . . ? C11 N2 Cu1 112.2(3) . . ? C20 N3 C19 110.5(4) . . ? C20 N3 Cu1 106.4(3) . . ? C19 N3 Cu1 111.0(3) . . ? N1 C1 C2 121.6(6) . . ? C3 C2 C1 117.7(6) . . ? C2 C3 C4 121.3(6) . . ? C3 C4 C12 116.3(6) . . ? C3 C4 C5 125.1(6) . . ? C12 C4 C5 118.6(6) . . ? C6 C5 C4 123.2(6) . . ? C5 C6 C7 119.7(6) . . ? C8 C7 C11 117.2(6) . . ? C8 C7 C6 123.7(6) . . ? C11 C7 C6 119.1(6) . . ? C9 C8 C7 119.7(5) . . ? C8 C9 C10 119.4(6) . . ? N2 C10 C9 123.1(6) . . ? N2 C11 C7 123.6(5) . . ? N2 C11 C12 116.0(4) . . ? C7 C11 C12 120.4(5) . . ? N1 C12 C4 124.2(6) . . ? N1 C12 C11 116.9(5) . . ? C4 C12 C11 118.9(5) . . ? C14 C13 C18 120.7(7) . . ? C13 C14 C15 120.9(8) . . ? C16 C15 C14 120.2(9) . . ? C15 C16 C17 119.8(8) . . ? C16 C17 C18 119.9(7) . . ? C13 C18 C17 118.5(7) . . ? C13 C18 C19 121.9(6) . . ? C17 C18 C19 119.7(7) . . ? C18 C19 N3 113.2(5) . . ? N3 C20 C22 113.8(4) . . ? N3 C20 C21 108.0(4) . . ? C22 C20 C21 108.3(4) . . ? O2 C21 O1 122.8(6) . . ? O2 C21 C20 120.0(5) . . ? O1 C21 C20 117.2(4) . . ? C23 C22 C20 114.5(5) . . ? C22 C23 S1 115.3(4) . . ? O5 Cl1 O6 113.0(8) . . ? O5 Cl1 O4 106.7(10) . . ? O6 Cl1 O4 106.4(10) . . ? O5 Cl1 O3 112.2(8) . . ? O6 Cl1 O3 118.8(7) . . ? O4 Cl1 O3 97.6(8) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 30.59 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.705 _refine_diff_density_min -0.421 _refine_diff_density_rms 0.082