# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_Compound _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C27 H28 Fe N3 O), 2(Cl O4), C4 H8 O' _chemical_formula_sum 'C58 H64 Cl2 Fe2 N6 O11' _chemical_formula_weight 1203.75 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pna21 _symmetry_space_group_name_Hall 'P 2c -2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 21.3524(9) _cell_length_b 9.1271(4) _cell_length_c 30.4606(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5936.3(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5413 _cell_measurement_theta_min 3.22 _cell_measurement_theta_max 31.42 _exptl_crystal_description prismatic _exptl_crystal_colour colourless _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.347 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2512 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_coefficient_mu 0.641 _exptl_absorpt_process_details ; Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.912 _exptl_absorpt_correction_T_max 0.941 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Ruby, Gemini' _diffrn_detector_area_resol_mean 10.2673 _diffrn_measurement_method '\w scans' _diffrn_standards_decay_% ? _diffrn_reflns_number 27977 _diffrn_reflns_av_R_equivalents 0.0705 _diffrn_reflns_av_sigmaI/netI 0.1045 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 3.23 _diffrn_reflns_theta_max 31.49 _reflns_number_total 14588 _reflns_number_gt 7255 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1279P)^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 none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _chemical_absolute_configuration ad _refine_ls_abs_structure_details ; 'Flack H D (1983), Acta Cryst. A39, 876-881' The Bijvoet coefficient for the strongest 100 Bijvoet pairs is B = 0.60(0.01) and its probability is 1.000 Dirdif (Beurskens et al. 1999) ; _refine_ls_abs_structure_Flack 0.10(3) _refine_ls_number_reflns 14588 _refine_ls_number_parameters 712 _refine_ls_number_restraints 26 _refine_ls_R_factor_all 0.1751 _refine_ls_R_factor_gt 0.0859 _refine_ls_wR_factor_ref 0.2631 _refine_ls_wR_factor_gt 0.1968 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.020 _refine_ls_shift/su_max 0.005 _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 0.99688(4) 0.81472(10) 0.12405(4) 0.0534(3) Uani 1 1 d . . . N1 N 0.8799(3) 0.6308(6) 0.11230(19) 0.0580(15) Uani 1 1 d . . . N2 N 1.0018(3) 0.8165(8) 0.0266(2) 0.0657(18) Uani 1 1 d . . . N3 N 0.9656(4) 0.5104(7) 0.1085(3) 0.081(2) Uani 1 1 d . . . H3 H 1.0048 0.4894 0.1080 0.098 Uiso 1 1 calc R . . O1 O 0.9074(3) 1.0513(6) 0.1237(2) 0.0831(16) Uani 1 1 d . . . C1 C 0.9391(3) 0.9521(7) 0.1229(3) 0.0561(15) Uani 1 1 d . . . C2 C 0.9432(3) 0.6428(7) 0.1167(2) 0.0558(16) Uani 1 1 d . . . C3 C 0.7983(5) 0.4380(12) 0.1000(4) 0.110(4) Uani 1 1 d . . . H3A H 0.7716 0.5208 0.1052 0.165 Uiso 1 1 calc R . . H3B H 0.7893 0.3627 0.1211 0.165 Uiso 1 1 calc R . . H3C H 0.7909 0.4010 0.0709 0.165 Uiso 1 1 calc R . . C4 C 0.9179(5) 0.4087(10) 0.1006(3) 0.088(3) Uani 1 1 d . . . H4 H 0.9229 0.3097 0.0942 0.106 Uiso 1 1 calc R . . C5 C 0.8632(5) 0.4823(10) 0.1041(3) 0.083(3) Uani 1 1 d . . . C6 C 1.0026(3) 0.8202(8) 0.0633(3) 0.059(2) Uani 1 1 d . . . C7 C 0.9955(3) 0.8136(10) -0.0196(3) 0.065(2) Uani 1 1 d . . . C8 C 0.9934(3) 0.6736(10) -0.0390(3) 0.073(2) Uani 1 1 d . . . C9 C 0.9861(4) 0.6755(13) -0.0853(3) 0.085(3) Uani 1 1 d . . . H9 H 0.9836 0.5874 -0.1005 0.102 Uiso 1 1 calc R . . C10 C 0.9828(5) 0.8042(15) -0.1079(3) 0.091(3) Uani 1 1 d . . . H10 H 0.9797 0.8026 -0.1383 0.109 Uiso 1 1 calc R . . C11 C 0.9840(4) 0.9358(13) -0.0863(3) 0.088(3) Uani 1 1 d . . . H11 H 0.9803 1.0220 -0.1024 0.106 Uiso 1 1 calc R . . C12 C 0.9904(3) 0.9436(9) -0.0421(3) 0.0621(19) Uani 1 1 d . . . C13 C 0.9930(5) 1.0878(11) -0.0193(4) 0.104(3) Uani 1 1 d . . . H13A H 0.9977 1.0722 0.0117 0.156 Uiso 1 1 calc R . . H13B H 0.9550 1.1409 -0.0247 0.156 Uiso 1 1 calc R . . H13C H 1.0280 1.1431 -0.0301 0.156 Uiso 1 1 calc R . . C14 C 0.9976(6) 0.5379(12) -0.0126(5) 0.112(4) Uani 1 1 d . . . H14A H 0.9954 0.4544 -0.0317 0.168 Uiso 1 1 calc R . . H14B H 0.9635 0.5347 0.0079 0.168 Uiso 1 1 calc R . . H14C H 1.0366 0.5366 0.0030 0.168 Uiso 1 1 calc R . . C15 C 0.8331(3) 0.7459(8) 0.1175(3) 0.0580(17) Uani 1 1 d . . . C16 C 0.8130(4) 0.8194(9) 0.0811(3) 0.070(2) Uani 1 1 d . . . C17 C 0.7689(4) 0.9316(10) 0.0878(4) 0.089(3) Uani 1 1 d . . . H17 H 0.7542 0.9847 0.0639 0.107 Uiso 1 1 calc R . . C18 C 0.7474(4) 0.9639(11) 0.1293(5) 0.099(3) Uani 1 1 d . . . H18 H 0.7184 1.0387 0.1333 0.119 Uiso 1 1 calc R . . C19 C 0.7684(4) 0.8867(12) 0.1641(4) 0.088(3) Uani 1 1 d . . . H19 H 0.7533 0.9098 0.1919 0.106 Uiso 1 1 calc R . . C20 C 0.8123(4) 0.7729(9) 0.1599(3) 0.071(2) Uani 1 1 d . . . C21 C 0.8360(5) 0.6916(10) 0.1993(3) 0.084(3) Uani 1 1 d . . . H21A H 0.8156 0.7280 0.2252 0.125 Uiso 1 1 calc R . . H21B H 0.8804 0.7057 0.2019 0.125 Uiso 1 1 calc R . . H21C H 0.8272 0.5890 0.1960 0.125 Uiso 1 1 calc R . . C22 C 0.8358(5) 0.7836(13) 0.0365(3) 0.097(3) Uani 1 1 d . . . H22A H 0.8157 0.8463 0.0155 0.145 Uiso 1 1 calc R . . H22B H 0.8263 0.6833 0.0298 0.145 Uiso 1 1 calc R . . H22C H 0.8803 0.7982 0.0352 0.145 Uiso 1 1 calc R . . C23 C 1.0885(4) 0.8943(12) 0.1324(4) 0.087(3) Uani 1 1 d . . . H23 H 1.1103 0.9484 0.1115 0.104 Uiso 1 1 calc R . . C24 C 1.0502(5) 0.9499(13) 0.1656(4) 0.098(3) Uani 1 1 d . . . H24 H 1.0427 1.0490 0.1704 0.118 Uiso 1 1 calc R . . C25 C 1.0250(5) 0.8393(15) 0.1901(3) 0.094(3) Uani 1 1 d . . . H25 H 0.9981 0.8498 0.2139 0.113 Uiso 1 1 calc R . . C26 C 1.0476(5) 0.7062(13) 0.1727(4) 0.098(4) Uani 1 1 d . . . H26 H 1.0379 0.6128 0.1829 0.118 Uiso 1 1 calc R . . C27 C 1.0879(4) 0.7399(13) 0.1367(4) 0.090(3) Uani 1 1 d . . . H27 H 1.1096 0.6731 0.1194 0.108 Uiso 1 1 calc R . . Fe1' Fe 0.35073(5) 0.29053(10) 0.28512(3) 0.0555(3) Uani 1 1 d . . . N1' N 0.2354(3) 0.0971(6) 0.2900(2) 0.0606(14) Uani 1 1 d . . . N2' N 0.3543(3) 0.3107(8) 0.3827(3) 0.0731(18) Uani 1 1 d . . . N3' N 0.3212(3) -0.0143(6) 0.3058(2) 0.0615(15) Uani 1 1 d . . . H3' H 0.3603 -0.0321 0.3101 0.074 Uiso 1 1 calc R . . O1' O 0.2596(3) 0.5247(7) 0.2823(3) 0.106(2) Uani 1 1 d . . . C1' C 0.2929(3) 0.4233(8) 0.2830(3) 0.0626(17) Uani 1 1 d . . . C2' C 0.2977(3) 0.1177(7) 0.2938(2) 0.0528(16) Uani 1 1 d . . . C3' C 0.1548(5) -0.1007(13) 0.2987(5) 0.126(5) Uani 1 1 d . . . H3D H 0.1281 -0.0212 0.2900 0.188 Uiso 1 1 calc R . . H3E H 0.1420 -0.1361 0.3270 0.188 Uiso 1 1 calc R . . H3F H 0.1517 -0.1784 0.2776 0.188 Uiso 1 1 calc R . . C4' C 0.2739(4) -0.1164(9) 0.3101(3) 0.081(2) Uani 1 1 d . . . H4' H 0.2789 -0.2141 0.3180 0.097 Uiso 1 1 calc R . . C5' C 0.2193(4) -0.0496(10) 0.3010(3) 0.080(2) Uani 1 1 d . . . C6' C 0.3541(3) 0.3049(9) 0.3446(3) 0.0597(19) Uani 1 1 d . . . C7' C 0.3482(3) 0.3149(10) 0.4285(2) 0.062(2) Uani 1 1 d . . . C8' C 0.3444(4) 0.1840(9) 0.4509(3) 0.072(2) Uani 1 1 d . . . C9' C 0.3379(5) 0.1942(14) 0.4972(4) 0.097(3) Uani 1 1 d . . . H9' H 0.3362 0.1085 0.5137 0.116 Uiso 1 1 calc R . . C10' C 0.3344(5) 0.3171(16) 0.5168(4) 0.098(3) Uani 1 1 d . . . H10' H 0.3279 0.3177 0.5470 0.118 Uiso 1 1 calc R . . C11' C 0.3396(4) 0.4470(13) 0.4957(4) 0.091(3) Uani 1 1 d . . . H11' H 0.3386 0.5341 0.5115 0.109 Uiso 1 1 calc R . . C12' C 0.3469(3) 0.4502(10) 0.4484(3) 0.073(2) Uani 1 1 d . . . C13' C 0.3504(6) 0.5891(12) 0.4236(4) 0.115(4) Uani 1 1 d . . . H13D H 0.3483 0.6701 0.4437 0.172 Uiso 1 1 calc R . . H13E H 0.3159 0.5945 0.4034 0.172 Uiso 1 1 calc R . . H13F H 0.3891 0.5929 0.4077 0.172 Uiso 1 1 calc R . . C14' C 0.3481(5) 0.0409(12) 0.4290(4) 0.111(4) Uani 1 1 d . . . H14D H 0.3439 -0.0356 0.4505 0.167 Uiso 1 1 calc R . . H14E H 0.3878 0.0319 0.4145 0.167 Uiso 1 1 calc R . . H14F H 0.3150 0.0329 0.4078 0.167 Uiso 1 1 calc R . . C15' C 0.1901(3) 0.2099(9) 0.2814(3) 0.066(2) Uani 1 1 d . . . C16' C 0.1629(3) 0.2845(9) 0.3154(3) 0.070(2) Uani 1 1 d . . . C17' C 0.1190(5) 0.3902(13) 0.3061(4) 0.102(3) Uani 1 1 d . . . H17' H 0.1004 0.4440 0.3285 0.122 Uiso 1 1 calc R . . C18' C 0.1027(5) 0.4152(15) 0.2622(5) 0.115(4) Uani 1 1 d . . . H18' H 0.0720 0.4844 0.2560 0.138 Uiso 1 1 calc R . . C19' C 0.1298(5) 0.3428(13) 0.2283(4) 0.097(3) Uani 1 1 d . . . H19' H 0.1192 0.3648 0.1994 0.117 Uiso 1 1 calc R . . C20' C 0.1741(4) 0.2346(10) 0.2376(3) 0.074(2) Uani 1 1 d . . . C21' C 0.2056(6) 0.1500(14) 0.2012(3) 0.108(3) Uani 1 1 d . . . H21D H 0.2346 0.0810 0.2136 0.161 Uiso 1 1 calc R . . H21E H 0.2278 0.2167 0.1824 0.161 Uiso 1 1 calc R . . H21F H 0.1746 0.0985 0.1844 0.161 Uiso 1 1 calc R . . C22' C 0.1811(5) 0.2564(13) 0.3623(4) 0.096(3) Uani 1 1 d . . . H22D H 0.1574 0.3195 0.3813 0.144 Uiso 1 1 calc R . . H22E H 0.2250 0.2758 0.3661 0.144 Uiso 1 1 calc R . . H22F H 0.1726 0.1561 0.3696 0.144 Uiso 1 1 calc R . . C23' C 0.4440(5) 0.2223(12) 0.2751(4) 0.092(3) Uani 1 1 d . . . H23' H 0.4673 0.1659 0.2945 0.110 Uiso 1 1 calc R . . C24' C 0.4087(6) 0.1684(15) 0.2417(5) 0.112(4) Uani 1 1 d . . . H24' H 0.4043 0.0703 0.2341 0.135 Uiso 1 1 calc R . . C25' C 0.3792(6) 0.292(2) 0.2201(3) 0.122(5) Uani 1 1 d . . . H25' H 0.3516 0.2885 0.1965 0.146 Uiso 1 1 calc R . . C26' C 0.4007(5) 0.4185(13) 0.2419(4) 0.101(4) Uani 1 1 d . . . H26' H 0.3905 0.5149 0.2351 0.121 Uiso 1 1 calc R . . C27' C 0.4401(4) 0.3721(10) 0.2758(4) 0.084(3) Uani 1 1 d . . . H27' H 0.4604 0.4331 0.2956 0.101 Uiso 1 1 calc R . . Cl1 Cl 0.96928(9) 0.70783(19) 0.32153(7) 0.0590(5) Uani 1 1 d D . . O2 O 0.9127(7) 0.7890(14) 0.3240(6) 0.240(7) Uani 1 1 d D . . O3 O 0.9540(7) 0.5695(15) 0.3385(5) 0.249(7) Uani 1 1 d D . . O4 O 0.9801(13) 0.6825(19) 0.2740(5) 0.84(8) Uani 1 1 d D . . O5 O 1.0204(9) 0.769(3) 0.3386(9) 0.56(4) Uani 1 1 d D . . Cl2 Cl 0.10593(9) 0.29839(17) 0.07930(7) 0.0616(5) Uani 1 1 d D . . O6 O 0.1251(10) 0.3285(18) 0.0337(5) 0.299(10) Uani 1 1 d D . . O7 O 0.1005(5) 0.4251(14) 0.1019(6) 0.266(10) Uani 1 1 d D . . O8 O 0.1565(4) 0.2124(11) 0.0940(4) 0.160(4) Uani 1 1 d D . . O9 O 0.0496(4) 0.2234(12) 0.0743(5) 0.189(5) Uani 1 1 d D . . O10 O 0.1789(14) 0.855(3) 0.4430(15) 0.315(15) Uani 1 1 d D . . C28 C 0.1905(15) 0.788(4) 0.4834(14) 0.242(14) Uani 1 1 d D . . H28A H 0.1689 0.8399 0.5067 0.290 Uiso 1 1 calc R . . H28B H 0.2351 0.7888 0.4897 0.290 Uiso 1 1 calc R . . C29 C 0.1679(13) 0.640(4) 0.4800(11) 0.239(14) Uani 1 1 d D . . H29A H 0.1979 0.5719 0.4923 0.287 Uiso 1 1 calc R . . H29B H 0.1284 0.6294 0.4954 0.287 Uiso 1 1 calc R . . C30 C 0.1597(17) 0.614(5) 0.4339(13) 0.30(2) Uani 1 1 d D . . H30A H 0.1168 0.5868 0.4277 0.364 Uiso 1 1 calc R . . H30B H 0.1871 0.5357 0.4242 0.364 Uiso 1 1 calc R . . C31 C 0.176(3) 0.751(5) 0.4116(10) 0.40(4) Uani 1 1 d D . . H31A H 0.2155 0.7419 0.3966 0.477 Uiso 1 1 calc R . . H31B H 0.1437 0.7758 0.3902 0.477 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0538(5) 0.0581(5) 0.0481(5) -0.0006(5) -0.0027(4) 0.0013(4) N1 0.061(3) 0.050(3) 0.063(4) 0.001(3) -0.004(3) -0.005(3) N2 0.053(3) 0.102(5) 0.043(4) 0.006(3) -0.002(3) 0.003(3) N3 0.090(5) 0.049(3) 0.105(6) 0.002(3) 0.012(4) 0.018(3) O1 0.085(3) 0.053(3) 0.111(5) -0.002(3) -0.004(4) 0.001(3) C1 0.064(4) 0.041(3) 0.064(4) 0.001(3) 0.006(4) -0.003(3) C2 0.066(4) 0.049(3) 0.052(4) 0.006(3) -0.005(3) -0.002(3) C3 0.119(8) 0.090(7) 0.120(8) -0.025(6) 0.028(6) -0.060(6) C4 0.113(7) 0.054(5) 0.098(7) 0.003(4) 0.012(6) -0.004(5) C5 0.105(7) 0.060(5) 0.084(6) -0.016(4) 0.007(5) -0.019(5) C6 0.050(4) 0.071(5) 0.057(5) 0.007(4) 0.008(3) -0.014(3) C7 0.050(4) 0.095(6) 0.050(5) -0.002(4) 0.006(3) -0.007(4) C8 0.053(4) 0.094(6) 0.073(6) -0.018(5) -0.004(4) -0.012(4) C9 0.077(5) 0.118(8) 0.061(6) -0.027(6) 0.002(4) 0.011(5) C10 0.072(5) 0.153(11) 0.048(5) -0.005(6) -0.004(4) -0.019(6) C11 0.069(5) 0.118(8) 0.078(7) 0.029(6) -0.002(4) -0.010(5) C12 0.056(4) 0.078(5) 0.052(5) 0.002(4) -0.010(3) 0.001(3) C13 0.111(8) 0.081(6) 0.119(10) -0.014(6) -0.026(6) 0.018(6) C14 0.116(8) 0.083(7) 0.137(11) 0.001(7) -0.019(7) -0.004(6) C15 0.057(4) 0.053(3) 0.064(5) -0.006(3) -0.007(4) -0.004(3) C16 0.059(4) 0.083(5) 0.069(6) -0.003(4) -0.013(4) -0.005(4) C17 0.073(5) 0.088(6) 0.107(8) -0.005(5) -0.045(5) 0.023(5) C18 0.058(5) 0.102(6) 0.137(10) -0.036(7) -0.018(6) 0.010(5) C19 0.053(4) 0.123(8) 0.088(7) -0.035(6) -0.014(5) 0.001(5) C20 0.062(4) 0.082(5) 0.069(6) -0.012(4) 0.000(4) -0.007(4) C21 0.093(6) 0.096(7) 0.061(5) 0.013(5) 0.001(4) -0.002(5) C22 0.087(6) 0.138(9) 0.066(6) 0.002(6) -0.016(5) -0.005(6) C23 0.067(5) 0.098(7) 0.096(8) 0.000(6) -0.008(5) -0.022(5) C24 0.094(7) 0.110(8) 0.091(8) -0.026(7) -0.035(6) -0.012(6) C25 0.081(6) 0.138(10) 0.064(6) -0.020(6) -0.008(5) 0.002(6) C26 0.094(7) 0.119(8) 0.083(7) 0.050(7) -0.036(6) -0.009(6) C27 0.058(5) 0.114(7) 0.098(8) -0.027(6) -0.024(5) 0.022(5) Fe1' 0.0581(5) 0.0607(5) 0.0477(5) 0.0055(5) 0.0000(5) -0.0103(4) N1' 0.061(3) 0.056(3) 0.065(4) 0.008(3) -0.009(3) -0.004(3) N2' 0.057(4) 0.098(5) 0.065(5) 0.003(4) -0.008(3) -0.013(3) N3' 0.059(3) 0.050(3) 0.075(4) 0.007(3) -0.004(3) 0.003(3) O1' 0.109(5) 0.069(3) 0.139(6) 0.019(4) 0.009(5) 0.009(4) C1' 0.067(4) 0.051(4) 0.069(5) 0.016(4) 0.004(4) -0.001(3) C2' 0.057(4) 0.061(4) 0.040(4) -0.006(3) -0.006(3) 0.002(3) C3' 0.097(7) 0.120(8) 0.160(13) 0.039(8) -0.022(7) -0.046(6) C4' 0.089(6) 0.058(5) 0.097(7) -0.008(4) -0.001(5) -0.009(4) C5' 0.081(6) 0.075(5) 0.085(6) -0.001(4) 0.000(4) -0.032(5) C6' 0.053(4) 0.087(5) 0.040(4) -0.001(4) -0.003(3) -0.007(3) C7' 0.046(4) 0.100(6) 0.040(4) -0.001(4) -0.007(3) -0.014(4) C8' 0.069(5) 0.082(5) 0.064(6) 0.005(4) -0.003(4) -0.027(4) C9' 0.080(6) 0.120(9) 0.091(8) 0.006(7) 0.007(5) -0.006(6) C10' 0.077(6) 0.147(11) 0.071(7) 0.009(7) 0.013(5) -0.008(6) C11' 0.072(5) 0.111(8) 0.089(7) -0.040(6) 0.007(5) -0.005(5) C12' 0.058(4) 0.083(6) 0.077(6) 0.003(5) 0.004(4) -0.012(4) C13' 0.120(9) 0.098(7) 0.125(10) -0.010(7) 0.009(7) -0.014(6) C14' 0.116(8) 0.106(8) 0.111(9) 0.009(7) 0.001(7) -0.044(7) C15' 0.036(3) 0.087(5) 0.074(5) 0.012(5) -0.006(4) -0.009(3) C16' 0.053(4) 0.090(6) 0.068(5) 0.018(5) 0.007(4) 0.008(4) C17' 0.075(6) 0.133(9) 0.097(8) 0.024(7) 0.035(6) 0.026(6) C18' 0.074(6) 0.148(10) 0.124(10) 0.056(8) 0.012(6) 0.028(6) C19' 0.068(5) 0.132(9) 0.092(8) 0.025(7) -0.008(5) 0.012(6) C20' 0.053(4) 0.087(6) 0.083(7) 0.025(5) -0.004(4) -0.004(4) C21' 0.124(8) 0.124(8) 0.075(7) 0.010(6) -0.036(6) 0.002(7) C22' 0.092(7) 0.116(7) 0.080(7) 0.007(6) 0.028(5) 0.016(6) C23' 0.080(6) 0.101(7) 0.095(8) 0.007(6) 0.027(6) 0.002(5) C24' 0.118(9) 0.129(9) 0.090(9) -0.034(8) 0.053(8) -0.035(8) C25' 0.079(7) 0.247(18) 0.040(5) 0.003(8) 0.012(5) -0.038(9) C26' 0.093(7) 0.107(8) 0.103(8) 0.055(7) 0.026(6) 0.017(6) C27' 0.062(4) 0.083(6) 0.106(8) -0.002(5) 0.001(5) -0.024(4) Cl1 0.0556(9) 0.0469(9) 0.0746(12) -0.0084(8) 0.0082(9) -0.0078(8) O2 0.251(17) 0.196(13) 0.27(2) 0.016(11) 0.054(14) 0.052(12) O3 0.249(17) 0.267(17) 0.231(18) 0.093(14) -0.007(11) -0.020(14) O4 0.40(5) 0.123(16) 2.0(2) 0.01(4) -0.37(9) 0.047(19) O5 0.35(3) 0.82(8) 0.51(6) -0.29(6) 0.01(3) -0.34(4) Cl2 0.0681(10) 0.0432(8) 0.0734(12) -0.0097(8) -0.0256(9) 0.0100(7) O6 0.34(3) 0.194(14) 0.36(3) 0.050(15) 0.03(2) 0.021(16) O7 0.117(7) 0.259(14) 0.42(2) -0.224(16) -0.059(10) 0.038(8) O8 0.134(8) 0.180(10) 0.166(11) -0.004(7) -0.045(7) 0.034(7) O9 0.131(8) 0.166(9) 0.271(16) -0.047(9) -0.027(9) -0.013(7) O10 0.23(2) 0.36(3) 0.35(4) 0.08(3) 0.09(3) 0.01(2) C28 0.20(3) 0.27(4) 0.25(4) -0.02(3) -0.03(3) 0.00(2) C29 0.23(3) 0.19(2) 0.30(4) 0.09(3) -0.07(2) -0.02(2) C30 0.27(3) 0.42(7) 0.22(3) -0.13(4) 0.02(3) -0.13(4) C31 0.47(8) 0.61(10) 0.11(2) 0.12(4) 0.02(3) 0.24(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 1.760(7) . ? Fe1 C6 1.855(9) . ? Fe1 C2 1.956(7) . ? Fe1 C26 2.087(8) . ? Fe1 C27 2.096(8) . ? Fe1 C24 2.103(9) . ? Fe1 C23 2.103(8) . ? Fe1 C25 2.113(10) . ? N1 C2 1.362(9) . ? N1 C5 1.424(10) . ? N1 C15 1.459(9) . ? N2 C6 1.118(10) . ? N2 C7 1.414(11) . ? N3 C2 1.324(9) . ? N3 C4 1.399(12) . ? N3 H3 0.8600 . ? O1 C1 1.130(8) . ? C3 C5 1.451(14) . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 C5 1.351(13) . ? C4 H4 0.9300 . ? C7 C12 1.375(11) . ? C7 C8 1.409(12) . ? C8 C9 1.418(13) . ? C8 C14 1.479(14) . ? C9 C10 1.363(15) . ? C9 H9 0.9300 . ? C10 C11 1.369(15) . ? C10 H10 0.9300 . ? C11 C12 1.354(12) . ? C11 H11 0.9300 . ? C12 C13 1.490(12) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C16 1.364(11) . ? C15 C20 1.389(11) . ? C16 C17 1.406(12) . ? C16 C22 1.481(13) . ? C17 C18 1.377(15) . ? C17 H17 0.9300 . ? C18 C19 1.349(15) . ? C18 H18 0.9300 . ? C19 C20 1.405(13) . ? C19 H19 0.9300 . ? C20 C21 1.499(12) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 C24 1.396(14) . ? C23 C27 1.416(14) . ? C23 H23 0.9300 . ? C24 C25 1.366(16) . ? C24 H24 0.9300 . ? C25 C26 1.410(16) . ? C25 H25 0.9300 . ? C26 C27 1.428(16) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? Fe1' C1' 1.731(8) . ? Fe1' C6' 1.819(8) . ? Fe1' C2' 1.959(7) . ? Fe1' C26' 2.057(9) . ? Fe1' C27' 2.067(8) . ? Fe1' C25' 2.072(10) . ? Fe1' C23' 2.109(10) . ? Fe1' C24' 2.127(11) . ? N1' C2' 1.350(9) . ? N1' C5' 1.422(10) . ? N1' C15' 1.436(9) . ? N2' C6' 1.160(10) . ? N2' C7' 1.402(11) . ? N3' C2' 1.355(8) . ? N3' C4' 1.380(10) . ? N3' H3' 0.8600 . ? O1' C1' 1.169(9) . ? C3' C5' 1.457(13) . ? C3' H3D 0.9600 . ? C3' H3E 0.9600 . ? C3' H3F 0.9600 . ? C4' C5' 1.344(13) . ? C4' H4' 0.9300 . ? C7' C12' 1.377(12) . ? C7' C8' 1.379(11) . ? C8' C9' 1.418(15) . ? C8' C14' 1.468(15) . ? C9' C10' 1.274(15) . ? C9' H9' 0.9300 . ? C10' C11' 1.354(15) . ? C10' H10' 0.9300 . ? C11' C12' 1.447(13) . ? C11' H11' 0.9300 . ? C12' C13' 1.477(14) . ? C13' H13D 0.9600 . ? C13' H13E 0.9600 . ? C13' H13F 0.9600 . ? C14' H14D 0.9600 . ? C14' H14E 0.9600 . ? C14' H14F 0.9600 . ? C15' C16' 1.369(12) . ? C15' C20' 1.395(13) . ? C16' C17' 1.375(12) . ? C16' C22' 1.503(14) . ? C17' C18' 1.400(15) . ? C17' H17' 0.9300 . ? C18' C19' 1.356(17) . ? C18' H18' 0.9300 . ? C19' C20' 1.396(13) . ? C19' H19' 0.9300 . ? C20' C21' 1.511(15) . ? C21' H21D 0.9600 . ? C21' H21E 0.9600 . ? C21' H21F 0.9600 . ? C22' H22D 0.9600 . ? C22' H22E 0.9600 . ? C22' H22F 0.9600 . ? C23' C24' 1.358(17) . ? C23' C27' 1.370(13) . ? C23' H23' 0.9300 . ? C24' C25' 1.450(19) . ? C24' H24' 0.9300 . ? C25' C26' 1.409(18) . ? C25' H25' 0.9300 . ? C26' C27' 1.397(14) . ? C26' H26' 0.9300 . ? C27' H27' 0.9300 . ? Cl1 O5 1.332(12) . ? Cl1 O3 1.403(12) . ? Cl1 O2 1.419(11) . ? Cl1 O4 1.485(14) . ? Cl2 O7 1.351(9) . ? Cl2 O9 1.392(8) . ? Cl2 O8 1.409(8) . ? Cl2 O6 1.475(12) . ? O10 C31 1.351(19) . ? O10 C28 1.395(18) . ? C28 C29 1.440(18) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C30 1.433(18) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 C31 1.462(19) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? 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 C6 90.4(4) . . ? C1 Fe1 C2 99.1(3) . . ? C6 Fe1 C2 86.9(3) . . ? C1 Fe1 C26 135.8(5) . . ? C6 Fe1 C26 133.4(5) . . ? C2 Fe1 C26 90.2(4) . . ? C1 Fe1 C27 152.4(4) . . ? C6 Fe1 C27 97.5(4) . . ? C2 Fe1 C27 107.6(4) . . ? C26 Fe1 C27 39.9(4) . . ? C1 Fe1 C24 88.5(4) . . ? C6 Fe1 C24 123.3(4) . . ? C2 Fe1 C24 148.9(4) . . ? C26 Fe1 C24 64.5(5) . . ? C27 Fe1 C24 65.1(4) . . ? C1 Fe1 C23 114.1(4) . . ? C6 Fe1 C23 92.9(4) . . ? C2 Fe1 C23 146.8(4) . . ? C26 Fe1 C23 66.1(4) . . ? C27 Fe1 C23 39.4(4) . . ? C24 Fe1 C23 38.8(4) . . ? C1 Fe1 C25 98.2(4) . . ? C6 Fe1 C25 158.2(4) . . ? C2 Fe1 C25 111.1(4) . . ? C26 Fe1 C25 39.2(4) . . ? C27 Fe1 C25 66.1(4) . . ? C24 Fe1 C25 37.8(4) . . ? C23 Fe1 C25 65.3(4) . . ? C2 N1 C5 110.0(6) . . ? C2 N1 C15 127.7(6) . . ? C5 N1 C15 122.2(7) . . ? C6 N2 C7 175.5(7) . . ? C2 N3 C4 112.1(7) . . ? C2 N3 H3 123.9 . . ? C4 N3 H3 123.9 . . ? O1 C1 Fe1 171.8(6) . . ? N3 C2 N1 105.4(6) . . ? N3 C2 Fe1 122.9(6) . . ? N1 C2 Fe1 131.1(5) . . ? C5 C3 H3A 109.5 . . ? C5 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C5 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C5 C4 N3 106.5(7) . . ? C5 C4 H4 126.7 . . ? N3 C4 H4 126.7 . . ? C4 C5 N1 105.7(8) . . ? C4 C5 C3 132.9(8) . . ? N1 C5 C3 121.3(9) . . ? N2 C6 Fe1 174.3(6) . . ? C12 C7 C8 124.8(8) . . ? C12 C7 N2 119.2(7) . . ? C8 C7 N2 116.0(8) . . ? C7 C8 C9 114.2(9) . . ? C7 C8 C14 122.0(9) . . ? C9 C8 C14 123.8(9) . . ? C10 C9 C8 121.2(9) . . ? C10 C9 H9 119.4 . . ? C8 C9 H9 119.4 . . ? C9 C10 C11 120.8(9) . . ? C9 C10 H10 119.6 . . ? C11 C10 H10 119.6 . . ? C12 C11 C10 121.7(10) . . ? C12 C11 H11 119.1 . . ? C10 C11 H11 119.1 . . ? C11 C12 C7 117.3(8) . . ? C11 C12 C13 121.0(9) . . ? C7 C12 C13 121.7(8) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C8 C14 H14A 109.5 . . ? C8 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C8 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 C20 124.6(7) . . ? C16 C15 N1 118.8(7) . . ? C20 C15 N1 116.6(7) . . ? C15 C16 C17 116.8(8) . . ? C15 C16 C22 122.2(8) . . ? C17 C16 C22 120.9(9) . . ? C18 C17 C16 120.9(9) . . ? C18 C17 H17 119.6 . . ? C16 C17 H17 119.6 . . ? C19 C18 C17 119.9(9) . . ? C19 C18 H18 120.1 . . ? C17 C18 H18 120.1 . . ? C18 C19 C20 122.4(9) . . ? C18 C19 H19 118.8 . . ? C20 C19 H19 118.8 . . ? C15 C20 C19 115.4(8) . . ? C15 C20 C21 123.3(8) . . ? C19 C20 C21 121.2(8) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C16 C22 H22A 109.5 . . ? C16 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C16 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 C27 106.8(9) . . ? C24 C23 Fe1 70.6(5) . . ? C27 C23 Fe1 70.0(5) . . ? C24 C23 H23 126.6 . . ? C27 C23 H23 126.6 . . ? Fe1 C23 H23 124.4 . . ? C25 C24 C23 111.0(10) . . ? C25 C24 Fe1 71.5(6) . . ? C23 C24 Fe1 70.6(5) . . ? C25 C24 H24 124.5 . . ? C23 C24 H24 124.5 . . ? Fe1 C24 H24 124.9 . . ? C24 C25 C26 107.3(10) . . ? C24 C25 Fe1 70.7(6) . . ? C26 C25 Fe1 69.4(5) . . ? C24 C25 H25 126.4 . . ? C26 C25 H25 126.4 . . ? Fe1 C25 H25 125.2 . . ? C25 C26 C27 108.0(9) . . ? C25 C26 Fe1 71.4(6) . . ? C27 C26 Fe1 70.4(5) . . ? C25 C26 H26 126.0 . . ? C27 C26 H26 126.0 . . ? Fe1 C26 H26 123.8 . . ? C23 C27 C26 106.9(9) . . ? C23 C27 Fe1 70.6(5) . . ? C26 C27 Fe1 69.7(5) . . ? C23 C27 H27 126.5 . . ? C26 C27 H27 126.5 . . ? Fe1 C27 H27 124.8 . . ? C1' Fe1' C6' 90.8(4) . . ? C1' Fe1' C2' 99.0(3) . . ? C6' Fe1' C2' 86.9(3) . . ? C1' Fe1' C26' 87.0(4) . . ? C6' Fe1' C26' 125.2(5) . . ? C2' Fe1' C26' 147.5(5) . . ? C1' Fe1' C27' 113.6(4) . . ? C6' Fe1' C27' 94.3(4) . . ? C2' Fe1' C27' 147.3(3) . . ? C26' Fe1' C27' 39.6(4) . . ? C1' Fe1' C25' 99.7(6) . . ? C6' Fe1' C25' 160.2(4) . . ? C2' Fe1' C25' 107.7(5) . . ? C26' Fe1' C25' 39.9(5) . . ? C27' Fe1' C25' 66.1(4) . . ? C1' Fe1' C23' 151.0(4) . . ? C6' Fe1' C23' 97.4(4) . . ? C2' Fe1' C23' 109.1(4) . . ? C26' Fe1' C23' 65.5(4) . . ? C27' Fe1' C23' 38.3(4) . . ? C25' Fe1' C23' 65.6(5) . . ? C1' Fe1' C24' 139.3(6) . . ? C6' Fe1' C24' 129.4(5) . . ? C2' Fe1' C24' 89.9(4) . . ? C26' Fe1' C24' 66.3(5) . . ? C27' Fe1' C24' 64.3(4) . . ? C25' Fe1' C24' 40.4(5) . . ? C23' Fe1' C24' 37.4(5) . . ? C2' N1' C5' 110.4(6) . . ? C2' N1' C15' 125.4(6) . . ? C5' N1' C15' 123.8(6) . . ? C6' N2' C7' 174.3(7) . . ? C2' N3' C4' 110.8(6) . . ? C2' N3' H3' 124.6 . . ? C4' N3' H3' 124.6 . . ? O1' C1' Fe1' 172.0(7) . . ? N1' C2' N3' 105.3(6) . . ? N1' C2' Fe1' 132.1(5) . . ? N3' C2' Fe1' 122.6(5) . . ? C5' C3' H3D 109.5 . . ? C5' C3' H3E 109.5 . . ? H3D C3' H3E 109.5 . . ? C5' C3' H3F 109.5 . . ? H3D C3' H3F 109.5 . . ? H3E C3' H3F 109.5 . . ? C5' C4' N3' 108.0(7) . . ? C5' C4' H4' 126.0 . . ? N3' C4' H4' 126.0 . . ? C4' C5' N1' 105.5(7) . . ? C4' C5' C3' 133.3(9) . . ? N1' C5' C3' 121.2(9) . . ? N2' C6' Fe1' 177.5(7) . . ? C12' C7' C8' 123.9(8) . . ? C12' C7' N2' 117.7(8) . . ? C8' C7' N2' 118.4(8) . . ? C7' C8' C9' 116.2(9) . . ? C7' C8' C14' 122.8(9) . . ? C9' C8' C14' 121.0(9) . . ? C10' C9' C8' 122.0(11) . . ? C10' C9' H9' 119.0 . . ? C8' C9' H9' 119.0 . . ? C9' C10' C11' 122.9(11) . . ? C9' C10' H10' 118.6 . . ? C11' C10' H10' 118.6 . . ? C10' C11' C12' 120.0(9) . . ? C10' C11' H11' 120.0 . . ? C12' C11' H11' 120.0 . . ? C7' C12' C11' 115.0(8) . . ? C7' C12' C13' 122.9(9) . . ? C11' C12' C13' 122.1(9) . . ? C12' C13' H13D 109.5 . . ? C12' C13' H13E 109.5 . . ? H13D C13' H13E 109.5 . . ? C12' C13' H13F 109.5 . . ? H13D C13' H13F 109.5 . . ? H13E C13' H13F 109.5 . . ? C8' C14' H14D 109.5 . . ? C8' C14' H14E 109.5 . . ? H14D C14' H14E 109.5 . . ? C8' C14' H14F 109.5 . . ? H14D C14' H14F 109.5 . . ? H14E C14' H14F 109.5 . . ? C16' C15' C20' 122.6(8) . . ? C16' C15' N1' 120.3(8) . . ? C20' C15' N1' 117.1(8) . . ? C15' C16' C17' 118.8(9) . . ? C15' C16' C22' 121.7(8) . . ? C17' C16' C22' 119.5(9) . . ? C16' C17' C18' 118.8(10) . . ? C16' C17' H17' 120.6 . . ? C18' C17' H17' 120.6 . . ? C19' C18' C17' 122.8(10) . . ? C19' C18' H18' 118.6 . . ? C17' C18' H18' 118.6 . . ? C18' C19' C20' 118.6(10) . . ? C18' C19' H19' 120.7 . . ? C20' C19' H19' 120.7 . . ? C15' C20' C19' 118.3(10) . . ? C15' C20' C21' 120.7(8) . . ? C19' C20' C21' 120.9(9) . . ? C20' C21' H21D 109.5 . . ? C20' C21' H21E 109.5 . . ? H21D C21' H21E 109.5 . . ? C20' C21' H21F 109.5 . . ? H21D C21' H21F 109.5 . . ? H21E C21' H21F 109.5 . . ? C16' C22' H22D 109.5 . . ? C16' C22' H22E 109.5 . . ? H22D C22' H22E 109.5 . . ? C16' C22' H22F 109.5 . . ? H22D C22' H22F 109.5 . . ? H22E C22' H22F 109.5 . . ? C24' C23' C27' 109.8(11) . . ? C24' C23' Fe1' 72.0(7) . . ? C27' C23' Fe1' 69.2(5) . . ? C24' C23' H23' 125.1 . . ? C27' C23' H23' 125.1 . . ? Fe1' C23' H23' 125.2 . . ? C23' C24' C25' 107.4(11) . . ? C23' C24' Fe1' 70.6(6) . . ? C25' C24' Fe1' 67.8(7) . . ? C23' C24' H24' 126.3 . . ? C25' C24' H24' 126.3 . . ? Fe1' C24' H24' 126.9 . . ? C26' C25' C24' 106.4(10) . . ? C26' C25' Fe1' 69.5(6) . . ? C24' C25' Fe1' 71.9(6) . . ? C26' C25' H25' 126.8 . . ? C24' C25' H25' 126.8 . . ? Fe1' C25' H25' 123.5 . . ? C27' C26' C25' 107.2(10) . . ? C27' C26' Fe1' 70.6(5) . . ? C25' C26' Fe1' 70.6(6) . . ? C27' C26' H26' 126.4 . . ? C25' C26' H26' 126.4 . . ? Fe1' C26' H26' 124.0 . . ? C23' C27' C26' 109.2(10) . . ? C23' C27' Fe1' 72.5(5) . . ? C26' C27' Fe1' 69.8(5) . . ? C23' C27' H27' 125.4 . . ? C26' C27' H27' 125.4 . . ? Fe1' C27' H27' 123.9 . . ? O5 Cl1 O3 115.0(13) . . ? O5 Cl1 O2 117.4(12) . . ? O3 Cl1 O2 104.6(8) . . ? O5 Cl1 O4 108.6(12) . . ? O3 Cl1 O4 104.9(10) . . ? O2 Cl1 O4 105.4(11) . . ? O7 Cl2 O9 113.8(7) . . ? O7 Cl2 O8 112.3(7) . . ? O9 Cl2 O8 115.1(7) . . ? O7 Cl2 O6 110.2(9) . . ? O9 Cl2 O6 103.2(9) . . ? O8 Cl2 O6 101.0(8) . . ? C31 O10 C28 109(3) . . ? O10 C28 C29 107(2) . . ? O10 C28 H28A 110.4 . . ? C29 C28 H28A 110.4 . . ? O10 C28 H28B 110.4 . . ? C29 C28 H28B 110.4 . . ? H28A C28 H28B 108.6 . . ? C30 C29 C28 105(2) . . ? C30 C29 H29A 110.7 . . ? C28 C29 H29A 110.7 . . ? C30 C29 H29B 110.7 . . ? C28 C29 H29B 110.7 . . ? H29A C29 H29B 108.8 . . ? C29 C30 C31 107(2) . . ? C29 C30 H30A 110.4 . . ? C31 C30 H30A 110.4 . . ? C29 C30 H30B 110.4 . . ? C31 C30 H30B 110.4 . . ? H30A C30 H30B 108.6 . . ? O10 C31 C30 107(3) . . ? O10 C31 H31A 110.4 . . ? C30 C31 H31A 110.4 . . ? O10 C31 H31B 110.4 . . ? C30 C31 H31B 110.4 . . ? H31A C31 H31B 108.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C4 N3 C2 N1 -2.8(9) . . . . ? C4 N3 C2 Fe1 -174.4(6) . . . . ? C5 N1 C2 N3 4.4(9) . . . . ? C15 N1 C2 N3 -179.3(7) . . . . ? C5 N1 C2 Fe1 175.0(6) . . . . ? C15 N1 C2 Fe1 -8.6(11) . . . . ? C1 Fe1 C2 N3 168.9(7) . . . . ? C6 Fe1 C2 N3 79.0(7) . . . . ? C26 Fe1 C2 N3 -54.5(8) . . . . ? C27 Fe1 C2 N3 -18.0(8) . . . . ? C24 Fe1 C2 N3 -88.7(10) . . . . ? C23 Fe1 C2 N3 -11.7(11) . . . . ? C25 Fe1 C2 N3 -88.5(8) . . . . ? C1 Fe1 C2 N1 -0.3(8) . . . . ? C6 Fe1 C2 N1 -90.3(7) . . . . ? C26 Fe1 C2 N1 136.2(8) . . . . ? C27 Fe1 C2 N1 172.8(7) . . . . ? C24 Fe1 C2 N1 102.0(9) . . . . ? C23 Fe1 C2 N1 179.1(7) . . . . ? C25 Fe1 C2 N1 102.2(7) . . . . ? C2 N3 C4 C5 0.1(11) . . . . ? N3 C4 C5 N1 2.5(10) . . . . ? N3 C4 C5 C3 -179.3(10) . . . . ? C2 N1 C5 C4 -4.3(10) . . . . ? C15 N1 C5 C4 179.1(7) . . . . ? C2 N1 C5 C3 177.2(8) . . . . ? C15 N1 C5 C3 0.6(13) . . . . ? C12 C7 C8 C9 0.8(11) . . . . ? N2 C7 C8 C9 179.1(6) . . . . ? C12 C7 C8 C14 -178.4(8) . . . . ? N2 C7 C8 C14 -0.1(11) . . . . ? C7 C8 C9 C10 1.1(12) . . . . ? C14 C8 C9 C10 -179.7(9) . . . . ? C8 C9 C10 C11 -2.5(15) . . . . ? C9 C10 C11 C12 2.0(15) . . . . ? C10 C11 C12 C7 -0.1(12) . . . . ? C10 C11 C12 C13 178.6(9) . . . . ? C8 C7 C12 C11 -1.3(11) . . . . ? N2 C7 C12 C11 -179.5(7) . . . . ? C8 C7 C12 C13 180.0(8) . . . . ? N2 C7 C12 C13 1.7(11) . . . . ? C2 N1 C15 C16 94.9(9) . . . . ? C5 N1 C15 C16 -89.2(9) . . . . ? C2 N1 C15 C20 -84.9(9) . . . . ? C5 N1 C15 C20 91.0(9) . . . . ? C20 C15 C16 C17 1.2(11) . . . . ? N1 C15 C16 C17 -178.6(7) . . . . ? C20 C15 C16 C22 -178.6(8) . . . . ? N1 C15 C16 C22 1.6(11) . . . . ? C15 C16 C17 C18 -0.4(12) . . . . ? C22 C16 C17 C18 179.5(9) . . . . ? C16 C17 C18 C19 -0.3(14) . . . . ? C17 C18 C19 C20 0.2(14) . . . . ? C16 C15 C20 C19 -1.4(11) . . . . ? N1 C15 C20 C19 178.4(7) . . . . ? C16 C15 C20 C21 -179.1(8) . . . . ? N1 C15 C20 C21 0.7(11) . . . . ? C18 C19 C20 C15 0.6(12) . . . . ? C18 C19 C20 C21 178.5(9) . . . . ? C1 Fe1 C23 C24 52.8(8) . . . . ? C6 Fe1 C23 C24 144.6(7) . . . . ? C2 Fe1 C23 C24 -126.5(8) . . . . ? C26 Fe1 C23 C24 -78.5(8) . . . . ? C27 Fe1 C23 C24 -117.0(9) . . . . ? C25 Fe1 C23 C24 -35.3(7) . . . . ? C1 Fe1 C23 C27 169.9(6) . . . . ? C6 Fe1 C23 C27 -98.4(6) . . . . ? C2 Fe1 C23 C27 -9.5(10) . . . . ? C26 Fe1 C23 C27 38.6(7) . . . . ? C24 Fe1 C23 C27 117.0(9) . . . . ? C25 Fe1 C23 C27 81.8(7) . . . . ? C27 C23 C24 C25 -0.6(11) . . . . ? Fe1 C23 C24 C25 60.4(7) . . . . ? C27 C23 C24 Fe1 -61.0(6) . . . . ? C1 Fe1 C24 C25 105.5(7) . . . . ? C6 Fe1 C24 C25 -165.0(6) . . . . ? C2 Fe1 C24 C25 0.3(12) . . . . ? C26 Fe1 C24 C25 -38.3(7) . . . . ? C27 Fe1 C24 C25 -82.6(7) . . . . ? C23 Fe1 C24 C25 -121.1(10) . . . . ? C1 Fe1 C24 C23 -133.3(7) . . . . ? C6 Fe1 C24 C23 -43.8(8) . . . . ? C2 Fe1 C24 C23 121.4(8) . . . . ? C26 Fe1 C24 C23 82.9(7) . . . . ? C27 Fe1 C24 C23 38.6(6) . . . . ? C25 Fe1 C24 C23 121.1(10) . . . . ? C23 C24 C25 C26 0.2(12) . . . . ? Fe1 C24 C25 C26 60.0(7) . . . . ? C23 C24 C25 Fe1 -59.8(7) . . . . ? C1 Fe1 C25 C24 -76.7(7) . . . . ? C6 Fe1 C25 C24 35.7(15) . . . . ? C2 Fe1 C25 C24 -179.8(6) . . . . ? C26 Fe1 C25 C24 117.9(10) . . . . ? C27 Fe1 C25 C24 79.5(7) . . . . ? C23 Fe1 C25 C24 36.2(6) . . . . ? C1 Fe1 C25 C26 165.4(7) . . . . ? C6 Fe1 C25 C26 -82.2(14) . . . . ? C2 Fe1 C25 C26 62.2(7) . . . . ? C27 Fe1 C25 C26 -38.4(6) . . . . ? C24 Fe1 C25 C26 -117.9(10) . . . . ? C23 Fe1 C25 C26 -81.8(7) . . . . ? C24 C25 C26 C27 0.4(11) . . . . ? Fe1 C25 C26 C27 61.2(6) . . . . ? C24 C25 C26 Fe1 -60.8(7) . . . . ? C1 Fe1 C26 C25 -21.0(9) . . . . ? C6 Fe1 C26 C25 149.6(7) . . . . ? C2 Fe1 C26 C25 -124.4(7) . . . . ? C27 Fe1 C26 C25 117.8(9) . . . . ? C24 Fe1 C26 C25 36.9(7) . . . . ? C23 Fe1 C26 C25 79.7(7) . . . . ? C1 Fe1 C26 C27 -138.8(6) . . . . ? C6 Fe1 C26 C27 31.8(9) . . . . ? C2 Fe1 C26 C27 117.9(7) . . . . ? C24 Fe1 C26 C27 -80.9(7) . . . . ? C23 Fe1 C26 C27 -38.1(6) . . . . ? C25 Fe1 C26 C27 -117.8(9) . . . . ? C24 C23 C27 C26 0.9(10) . . . . ? Fe1 C23 C27 C26 -60.5(6) . . . . ? C24 C23 C27 Fe1 61.4(6) . . . . ? C25 C26 C27 C23 -0.8(10) . . . . ? Fe1 C26 C27 C23 61.1(6) . . . . ? C25 C26 C27 Fe1 -61.9(7) . . . . ? C1 Fe1 C27 C23 -20.3(12) . . . . ? C6 Fe1 C27 C23 85.4(6) . . . . ? C2 Fe1 C27 C23 174.6(6) . . . . ? C26 Fe1 C27 C23 -117.4(9) . . . . ? C24 Fe1 C27 C23 -38.0(6) . . . . ? C25 Fe1 C27 C23 -79.6(7) . . . . ? C1 Fe1 C27 C26 97.1(11) . . . . ? C6 Fe1 C27 C26 -157.3(7) . . . . ? C2 Fe1 C27 C26 -68.1(7) . . . . ? C24 Fe1 C27 C26 79.4(8) . . . . ? C23 Fe1 C27 C26 117.4(9) . . . . ? C25 Fe1 C27 C26 37.7(7) . . . . ? C5' N1' C2' N3' 1.8(8) . . . . ? C15' N1' C2' N3' 174.5(7) . . . . ? C5' N1' C2' Fe1' -178.6(5) . . . . ? C15' N1' C2' Fe1' -5.8(11) . . . . ? C4' N3' C2' N1' -1.0(8) . . . . ? C4' N3' C2' Fe1' 179.3(6) . . . . ? C1' Fe1' C2' N1' 13.0(8) . . . . ? C6' Fe1' C2' N1' 103.4(7) . . . . ? C26' Fe1' C2' N1' -85.7(9) . . . . ? C27' Fe1' C2' N1' -163.5(7) . . . . ? C25' Fe1' C2' N1' -90.3(8) . . . . ? C23' Fe1' C2' N1' -159.8(7) . . . . ? C24' Fe1' C2' N1' -127.1(8) . . . . ? C1' Fe1' C2' N3' -167.3(6) . . . . ? C6' Fe1' C2' N3' -77.0(6) . . . . ? C26' Fe1' C2' N3' 94.0(8) . . . . ? C27' Fe1' C2' N3' 16.2(10) . . . . ? C25' Fe1' C2' N3' 89.4(7) . . . . ? C23' Fe1' C2' N3' 19.8(7) . . . . ? C24' Fe1' C2' N3' 52.5(7) . . . . ? C2' N3' C4' C5' -0.2(10) . . . . ? N3' C4' C5' N1' 1.2(10) . . . . ? N3' C4' C5' C3' 177.7(11) . . . . ? C2' N1' C5' C4' -1.9(10) . . . . ? C15' N1' C5' C4' -174.7(8) . . . . ? C2' N1' C5' C3' -178.9(9) . . . . ? C15' N1' C5' C3' 8.3(14) . . . . ? C12' C7' C8' C9' 0.8(12) . . . . ? N2' C7' C8' C9' -179.7(7) . . . . ? C12' C7' C8' C14' -177.8(8) . . . . ? N2' C7' C8' C14' 1.7(12) . . . . ? C7' C8' C9' C10' 1.6(14) . . . . ? C14' C8' C9' C10' -179.7(10) . . . . ? C8' C9' C10' C11' -3.4(18) . . . . ? C9' C10' C11' C12' 2.8(16) . . . . ? C8' C7' C12' C11' -1.3(11) . . . . ? N2' C7' C12' C11' 179.1(6) . . . . ? C8' C7' C12' C13' -179.2(9) . . . . ? N2' C7' C12' C13' 1.2(11) . . . . ? C10' C11' C12' C7' -0.4(12) . . . . ? C10' C11' C12' C13' 177.6(10) . . . . ? C2' N1' C15' C16' -89.2(9) . . . . ? C5' N1' C15' C16' 82.5(10) . . . . ? C2' N1' C15' C20' 93.1(9) . . . . ? C5' N1' C15' C20' -95.1(9) . . . . ? C20' C15' C16' C17' -1.4(12) . . . . ? N1' C15' C16' C17' -178.9(8) . . . . ? C20' C15' C16' C22' -179.8(8) . . . . ? N1' C15' C16' C22' 2.7(12) . . . . ? C15' C16' C17' C18' 1.4(15) . . . . ? C22' C16' C17' C18' 179.9(10) . . . . ? C16' C17' C18' C19' -2.1(19) . . . . ? C17' C18' C19' C20' 2.6(19) . . . . ? C16' C15' C20' C19' 1.9(12) . . . . ? N1' C15' C20' C19' 179.5(8) . . . . ? C16' C15' C20' C21' 179.7(9) . . . . ? N1' C15' C20' C21' -2.7(11) . . . . ? C18' C19' C20' C15' -2.5(15) . . . . ? C18' C19' C20' C21' 179.8(11) . . . . ? C1' Fe1' C23' C24' -102.5(11) . . . . ? C6' Fe1' C23' C24' 152.1(8) . . . . ? C2' Fe1' C23' C24' 62.9(8) . . . . ? C26' Fe1' C23' C24' -82.5(9) . . . . ? C27' Fe1' C23' C24' -120.3(10) . . . . ? C25' Fe1' C23' C24' -38.4(8) . . . . ? C1' Fe1' C23' C27' 17.8(13) . . . . ? C6' Fe1' C23' C27' -87.6(7) . . . . ? C2' Fe1' C23' C27' -176.8(6) . . . . ? C26' Fe1' C23' C27' 37.8(7) . . . . ? C25' Fe1' C23' C27' 81.9(8) . . . . ? C24' Fe1' C23' C27' 120.3(10) . . . . ? C27' C23' C24' C25' -1.2(12) . . . . ? Fe1' C23' C24' C25' 57.9(7) . . . . ? C27' C23' C24' Fe1' -59.1(7) . . . . ? C1' Fe1' C24' C23' 133.4(8) . . . . ? C6' Fe1' C24' C23' -36.9(9) . . . . ? C2' Fe1' C24' C23' -122.7(7) . . . . ? C26' Fe1' C24' C23' 80.1(8) . . . . ? C27' Fe1' C24' C23' 36.4(7) . . . . ? C25' Fe1' C24' C23' 119.1(10) . . . . ? C1' Fe1' C24' C25' 14.3(11) . . . . ? C6' Fe1' C24' C25' -156.0(7) . . . . ? C2' Fe1' C24' C25' 118.1(8) . . . . ? C26' Fe1' C24' C25' -39.0(7) . . . . ? C27' Fe1' C24' C25' -82.7(8) . . . . ? C23' Fe1' C24' C25' -119.1(10) . . . . ? C23' C24' C25' C26' 1.6(12) . . . . ? Fe1' C24' C25' C26' 61.3(7) . . . . ? C23' C24' C25' Fe1' -59.7(7) . . . . ? C1' Fe1' C25' C26' 73.3(8) . . . . ? C6' Fe1' C25' C26' -48(2) . . . . ? C2' Fe1' C25' C26' 176.1(7) . . . . ? C27' Fe1' C25' C26' -38.3(6) . . . . ? C23' Fe1' C25' C26' -80.4(7) . . . . ? C24' Fe1' C25' C26' -116.1(10) . . . . ? C1' Fe1' C25' C24' -170.6(7) . . . . ? C6' Fe1' C25' C24' 68(2) . . . . ? C2' Fe1' C25' C24' -67.8(8) . . . . ? C26' Fe1' C25' C24' 116.1(10) . . . . ? C27' Fe1' C25' C24' 77.7(7) . . . . ? C23' Fe1' C25' C24' 35.6(7) . . . . ? C24' C25' C26' C27' -1.4(12) . . . . ? Fe1' C25' C26' C27' 61.5(7) . . . . ? C24' C25' C26' Fe1' -62.8(7) . . . . ? C1' Fe1' C26' C27' 133.9(7) . . . . ? C6' Fe1' C26' C27' 44.9(8) . . . . ? C2' Fe1' C26' C27' -124.0(8) . . . . ? C25' Fe1' C26' C27' -117.1(10) . . . . ? C23' Fe1' C26' C27' -36.6(6) . . . . ? C24' Fe1' C26' C27' -77.7(7) . . . . ? C1' Fe1' C26' C25' -109.0(9) . . . . ? C6' Fe1' C26' C25' 162.1(8) . . . . ? C2' Fe1' C26' C25' -6.9(12) . . . . ? C27' Fe1' C26' C25' 117.1(10) . . . . ? C23' Fe1' C26' C25' 80.5(8) . . . . ? C24' Fe1' C26' C25' 39.5(8) . . . . ? C24' C23' C27' C26' 0.3(11) . . . . ? Fe1' C23' C27' C26' -60.5(7) . . . . ? C24' C23' C27' Fe1' 60.8(7) . . . . ? C25' C26' C27' C23' 0.7(11) . . . . ? Fe1' C26' C27' C23' 62.2(7) . . . . ? C25' C26' C27' Fe1' -61.5(7) . . . . ? C1' Fe1' C27' C23' -170.7(7) . . . . ? C6' Fe1' C27' C23' 96.5(7) . . . . ? C2' Fe1' C27' C23' 5.5(10) . . . . ? C26' Fe1' C27' C23' -118.9(10) . . . . ? C25' Fe1' C27' C23' -80.2(8) . . . . ? C24' Fe1' C27' C23' -35.6(7) . . . . ? C1' Fe1' C27' C26' -51.8(8) . . . . ? C6' Fe1' C27' C26' -144.6(7) . . . . ? C2' Fe1' C27' C26' 124.4(8) . . . . ? C25' Fe1' C27' C26' 38.6(8) . . . . ? C23' Fe1' C27' C26' 118.9(10) . . . . ? C24' Fe1' C27' C26' 83.3(9) . . . . ? C31 O10 C28 C29 -25(5) . . . . ? O10 C28 C29 C30 16(4) . . . . ? C28 C29 C30 C31 -2(5) . . . . ? C28 O10 C31 C30 23(6) . . . . ? C29 C30 C31 O10 -12(6) . . . . ? _diffrn_measured_fraction_theta_max 0.916 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.618 _refine_diff_density_min -0.415 _refine_diff_density_rms 0.077 _database_code_depnum_ccdc_archive 'CCDC 951023' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_Compound _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H50 Cl Fe N4 O Ru, F6 P, C4 H8 O' _chemical_formula_sum 'C48 H58 Cl F6 Fe N4 O2 P Ru' _chemical_formula_weight 1060.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Cl Cl 0.1484 0.1585 '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' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pna21 _symmetry_space_group_name_Hall 'P 2c -2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 25.0135(6) _cell_length_b 10.8950(3) _cell_length_c 17.0457(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4645.3(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150.0(1) _cell_measurement_reflns_used 4840 _cell_measurement_theta_min 3 _cell_measurement_theta_max 31 _exptl_crystal_description prismatic _exptl_crystal_colour orange _exptl_crystal_size_max 0.152 _exptl_crystal_size_mid 0.033 _exptl_crystal_size_min 0.030 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.516 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2184 _exptl_absorpt_correction_type refdelf _exptl_absorpt_coefficient_mu 0.797 _exptl_absorpt_process_details ; Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56 Cubic fit to sin(theta)/lambda - 24 parameters ; _exptl_absorpt_correction_T_min 0.961 _exptl_absorpt_correction_T_max 0.981 _exptl_special_details ; ? ; _diffrn_ambient_temperature 150.0(1) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Ruby, Gemini' _diffrn_detector_area_resol_mean 10.2673 _diffrn_measurement_method '\w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22674 _diffrn_reflns_av_R_equivalents 0.0587 _diffrn_reflns_av_sigmaI/netI 0.0984 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.26 _diffrn_reflns_theta_max 31.48 _reflns_number_total 11236 _reflns_number_gt 8454 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0264P)^2^+0.9010P] 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 ? _chemical_absolute_configuration ad _refine_ls_abs_structure_details ; 'Flack H D (1983), Acta Cryst. A39, 876-881' The Bijvoet coefficient for the strongest 100 Bijvoet pairs is B = 0.957(0.002) and its probability is 1.000 Dirdif (Beurskens et al. 1999) ; _refine_ls_abs_structure_Flack -0.01(2) _refine_ls_number_reflns 11236 _refine_ls_number_parameters 581 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0910 _refine_ls_R_factor_gt 0.0611 _refine_ls_wR_factor_ref 0.0998 _refine_ls_wR_factor_gt 0.0902 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _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 Ru1 Ru 0.095311(12) 0.01431(3) 0.999925(19) 0.01287(8) Uani 1 1 d . . . Fe1 Fe -0.09559(3) 0.00315(6) 1.05305(4) 0.01691(17) Uani 1 1 d . . . Cl1 Cl 0.08246(4) -0.06720(11) 1.13010(8) 0.0196(2) Uani 1 1 d . . . N1 N 0.01425(13) -0.0189(3) 0.9860(2) 0.0127(8) Uani 1 1 d . . . N2 N -0.14146(15) 0.2156(4) 0.9638(3) 0.0233(10) Uani 1 1 d . . . N3 N 0.00509(13) 0.1502(3) 1.0592(2) 0.0154(8) Uani 1 1 d . . . N4 N 0.08062(13) 0.2563(3) 1.0875(2) 0.0163(8) Uani 1 1 d . . . H4 H 0.0613 0.2945 1.1213 0.020 Uiso 1 1 calc R . . O1 O -0.13075(13) -0.1579(4) 0.9274(3) 0.0356(10) Uani 1 1 d . . . C1 C -0.11211(17) -0.0932(4) 0.9728(3) 0.0205(11) Uani 1 1 d . . . C2 C -0.02039(16) 0.0475(4) 1.0256(3) 0.0129(9) Uani 1 1 d . . . C3 C -0.02545(16) 0.2526(4) 1.0948(3) 0.0202(11) Uani 1 1 d . . . H3A H -0.0628 0.2323 1.0956 0.030 Uiso 1 1 calc R . . H3B H -0.0202 0.3258 1.0645 0.030 Uiso 1 1 calc R . . H3C H -0.0132 0.2661 1.1475 0.030 Uiso 1 1 calc R . . C4 C 0.05976(16) 0.1587(4) 1.0521(3) 0.0131(9) Uani 1 1 d . . . C6 C -0.12346(15) 0.1349(4) 1.0016(4) 0.0193(9) Uani 1 1 d . . . C7 C -0.16867(19) 0.2936(6) 0.9118(3) 0.0305(14) Uani 1 1 d . . . C8 C -0.1985(2) 0.2386(7) 0.8518(4) 0.0435(18) Uani 1 1 d . . . C9 C -0.2263(2) 0.3179(9) 0.8038(5) 0.068(3) Uani 1 1 d . . . H9 H -0.2476 0.2852 0.7643 0.082 Uiso 1 1 calc R . . C10 C -0.2238(3) 0.4436(11) 0.8120(5) 0.088(4) Uani 1 1 d . . . H10 H -0.2427 0.4946 0.7781 0.105 Uiso 1 1 calc R . . C11 C -0.1936(3) 0.4915(8) 0.8700(5) 0.069(3) Uani 1 1 d . . . H11 H -0.1921 0.5764 0.8751 0.083 Uiso 1 1 calc R . . C12 C -0.1648(2) 0.4206(6) 0.9221(4) 0.0421(17) Uani 1 1 d . . . C13 C -0.1308(3) 0.4738(5) 0.9852(5) 0.061(2) Uani 1 1 d . . . H13A H -0.1139 0.4088 1.0141 0.091 Uiso 1 1 calc R . . H13B H -0.1526 0.5217 1.0201 0.091 Uiso 1 1 calc R . . H13C H -0.1039 0.5253 0.9622 0.091 Uiso 1 1 calc R . . C14 C -0.1985(2) 0.1024(7) 0.8382(4) 0.057(2) Uani 1 1 d . . . H14A H -0.2214 0.0833 0.7947 0.085 Uiso 1 1 calc R . . H14B H -0.2114 0.0614 0.8843 0.085 Uiso 1 1 calc R . . H14C H -0.1628 0.0755 0.8269 0.085 Uiso 1 1 calc R . . C15 C -0.00403(15) -0.1058(4) 0.9282(3) 0.0116(9) Uani 1 1 d . . . C16 C -0.02141(16) -0.0575(4) 0.8562(3) 0.0148(10) Uani 1 1 d . . . C17 C -0.03699(16) -0.1396(4) 0.7979(3) 0.0199(11) Uani 1 1 d . . . H17 H -0.0484 -0.1098 0.7496 0.024 Uiso 1 1 calc R . . C18 C -0.03577(18) -0.2657(5) 0.8109(3) 0.0239(12) Uani 1 1 d . . . H18 H -0.0471 -0.3197 0.7721 0.029 Uiso 1 1 calc R . . C19 C -0.01766(19) -0.3095(5) 0.8815(3) 0.0226(11) Uani 1 1 d . . . H19 H -0.0162 -0.3939 0.8893 0.027 Uiso 1 1 calc R . . C20 C -0.00140(16) -0.2319(4) 0.9421(3) 0.0157(10) Uani 1 1 d . . . C21 C 0.01675(18) -0.2825(4) 1.0192(3) 0.0230(12) Uani 1 1 d . . . H21A H 0.0266 -0.2162 1.0534 0.035 Uiso 1 1 calc R . . H21B H 0.0471 -0.3350 1.0111 0.035 Uiso 1 1 calc R . . H21C H -0.0117 -0.3288 1.0426 0.035 Uiso 1 1 calc R . . C22 C -0.02555(18) 0.0788(4) 0.8407(3) 0.0217(11) Uani 1 1 d . . . H22A H -0.0136 0.1232 0.8861 0.033 Uiso 1 1 calc R . . H22B H -0.0621 0.0997 0.8297 0.033 Uiso 1 1 calc R . . H22C H -0.0036 0.0999 0.7965 0.033 Uiso 1 1 calc R . . C23 C -0.0924(3) 0.0446(6) 1.1740(3) 0.0379(15) Uani 1 1 d . . . H23 H -0.0787 0.1172 1.1945 0.045 Uiso 1 1 calc R . . C24 C -0.0636(2) -0.0626(6) 1.1585(3) 0.0370(16) Uani 1 1 d . . . H24 H -0.0273 -0.0744 1.1671 0.044 Uiso 1 1 calc R . . C25 C -0.0986(3) -0.1478(5) 1.1283(4) 0.0434(16) Uani 1 1 d . . . H25 H -0.0901 -0.2274 1.1133 0.052 Uiso 1 1 calc R . . C26 C -0.1492(2) -0.0938(7) 1.1242(4) 0.0448(18) Uani 1 1 d . . . H26 H -0.1802 -0.1305 1.1052 0.054 Uiso 1 1 calc R . . C27 C -0.1450(2) 0.0229(7) 1.1532(4) 0.0468(18) Uani 1 1 d . . . H27 H -0.1729 0.0787 1.1581 0.056 Uiso 1 1 calc R . . C28 C 0.13393(16) 0.3021(4) 1.0726(3) 0.0163(10) Uani 1 1 d . . . C29 C 0.17639(17) 0.2667(4) 1.1214(3) 0.0178(11) Uani 1 1 d . . . C30 C 0.22639(18) 0.3112(5) 1.1017(3) 0.0244(12) Uani 1 1 d . . . H30 H 0.2559 0.2879 1.1314 0.029 Uiso 1 1 calc R . . C31 C 0.23344(19) 0.3891(5) 1.0393(3) 0.0269(13) Uani 1 1 d . . . H31 H 0.2676 0.4165 1.0270 0.032 Uiso 1 1 calc R . . C32 C 0.19040(16) 0.4277(4) 0.9941(4) 0.0228(10) Uani 1 1 d . . . H32 H 0.1957 0.4811 0.9523 0.027 Uiso 1 1 calc R . . C33 C 0.13941(17) 0.3857(4) 1.0121(3) 0.0198(11) Uani 1 1 d . . . C34 C 0.09127(18) 0.4306(4) 0.9656(3) 0.0280(12) Uani 1 1 d . . . H34A H 0.1028 0.4879 0.9264 0.042 Uiso 1 1 calc R . . H34B H 0.0665 0.4701 1.0004 0.042 Uiso 1 1 calc R . . H34C H 0.0741 0.3620 0.9408 0.042 Uiso 1 1 calc R . . C35 C 0.16810(19) 0.1861(5) 1.1911(3) 0.0258(12) Uani 1 1 d . . . H35A H 0.1310 0.1639 1.1947 0.039 Uiso 1 1 calc R . . H35B H 0.1785 0.2293 1.2378 0.039 Uiso 1 1 calc R . . H35C H 0.1894 0.1133 1.1858 0.039 Uiso 1 1 calc R . . C36 C 0.16661(16) -0.1226(4) 0.9803(3) 0.0219(12) Uani 1 1 d . . . C37 C 0.18462(13) -0.0024(4) 1.0033(4) 0.0175(9) Uani 1 1 d . . . H37 H 0.2049 0.0076 1.0485 0.021 Uiso 1 1 calc R . . C38 C 0.17128(16) 0.1001(4) 0.9567(3) 0.0178(11) Uani 1 1 d . . . H38 H 0.1858 0.1763 0.9688 0.021 Uiso 1 1 calc R . . C39 C 0.13620(17) 0.0895(4) 0.8918(3) 0.0172(10) Uani 1 1 d . . . C40 C 0.11321(18) -0.0261(5) 0.8776(3) 0.0176(10) Uani 1 1 d . . . H40 H 0.0863 -0.0332 0.8402 0.021 Uiso 1 1 calc R . . C41 C 0.13028(17) -0.1330(4) 0.9194(3) 0.0177(11) Uani 1 1 d . . . H41 H 0.1169 -0.2097 0.9056 0.021 Uiso 1 1 calc R . . C42 C 0.18918(18) -0.2369(5) 1.0191(3) 0.0252(13) Uani 1 1 d . . . C43 C 0.23817(17) -0.2727(4) 0.9703(3) 0.0259(12) Uani 1 1 d . . . H43A H 0.2541 -0.3452 0.9920 0.039 Uiso 1 1 calc R . . H43B H 0.2637 -0.2068 0.9711 0.039 Uiso 1 1 calc R . . H43C H 0.2274 -0.2883 0.9172 0.039 Uiso 1 1 calc R . . C44 C 0.2037(2) -0.2251(5) 1.1048(4) 0.0390(16) Uani 1 1 d . . . H44A H 0.2172 -0.3023 1.1236 0.059 Uiso 1 1 calc R . . H44B H 0.1726 -0.2025 1.1344 0.059 Uiso 1 1 calc R . . H44C H 0.2307 -0.1632 1.1109 0.059 Uiso 1 1 calc R . . C45 C 0.12609(19) 0.1969(5) 0.8379(3) 0.0264(12) Uani 1 1 d . . . H45A H 0.1452 0.2674 0.8567 0.040 Uiso 1 1 calc R . . H45B H 0.0885 0.2147 0.8367 0.040 Uiso 1 1 calc R . . H45C H 0.1381 0.1769 0.7859 0.040 Uiso 1 1 calc R . . P1 P 0.34212(6) 0.08823(17) 0.23470(11) 0.0391(4) Uani 1 1 d . . . F1 F 0.29225(14) 0.0410(4) 0.1862(3) 0.0654(13) Uani 1 1 d . . . F2 F 0.39194(13) 0.1368(4) 0.2828(3) 0.0925(17) Uani 1 1 d . . . F3 F 0.30960(14) 0.2072(4) 0.2611(3) 0.0714(13) Uani 1 1 d . . . F4 F 0.37414(16) -0.0294(4) 0.2089(3) 0.097(2) Uani 1 1 d . . . F5 F 0.36309(19) 0.1590(4) 0.1606(3) 0.0917(17) Uani 1 1 d . . . F6 F 0.3208(2) 0.0194(5) 0.3098(3) 0.116(2) Uani 1 1 d . . . O2 O 0.04661(12) 0.4798(3) 0.1619(2) 0.0239(8) Uani 1 1 d . . . C46 C -0.00211(19) 0.5271(4) 0.1955(4) 0.0264(12) Uani 1 1 d . . . H46A H -0.0188 0.4655 0.2284 0.032 Uiso 1 1 calc R . . H46B H -0.0270 0.5498 0.1543 0.032 Uiso 1 1 calc R . . C47 C 0.0125(2) 0.6371(5) 0.2431(4) 0.0422(16) Uani 1 1 d . . . H47A H -0.0074 0.6390 0.2919 0.051 Uiso 1 1 calc R . . H47B H 0.0055 0.7121 0.2142 0.051 Uiso 1 1 calc R . . C48 C 0.0714(2) 0.6222(5) 0.2584(4) 0.0437(17) Uani 1 1 d . . . H48A H 0.0889 0.7012 0.2633 0.052 Uiso 1 1 calc R . . H48B H 0.0777 0.5749 0.3057 0.052 Uiso 1 1 calc R . . C49 C 0.0904(2) 0.5552(5) 0.1878(4) 0.0347(14) Uani 1 1 d . . . H49A H 0.1006 0.6127 0.1469 0.042 Uiso 1 1 calc R . . H49B H 0.1211 0.5048 0.2006 0.042 Uiso 1 1 calc R . . H42 H 0.159(2) -0.294(5) 1.003(5) 0.064(19) Uiso 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 Ru1 0.01231(14) 0.01487(15) 0.01143(16) -0.0013(2) 0.0003(2) 0.00200(13) Fe1 0.0134(3) 0.0208(4) 0.0165(4) -0.0003(3) 0.0005(3) -0.0003(3) Cl1 0.0195(5) 0.0256(6) 0.0136(6) 0.0015(5) 0.0000(5) 0.0026(5) N1 0.0151(15) 0.0127(15) 0.010(2) 0.0024(17) -0.0034(15) 0.0026(14) N2 0.022(2) 0.030(2) 0.018(3) 0.001(2) 0.0029(18) -0.0010(18) N3 0.0137(18) 0.0169(18) 0.016(2) -0.0049(17) 0.0017(17) 0.0013(15) N4 0.0122(17) 0.0188(19) 0.018(2) -0.0033(18) -0.0022(16) -0.0008(15) O1 0.0252(18) 0.045(2) 0.037(3) -0.012(2) 0.0019(18) -0.0131(18) C1 0.017(2) 0.025(2) 0.020(3) 0.001(2) 0.005(2) -0.0041(19) C2 0.0186(19) 0.0107(19) 0.010(2) 0.0001(18) -0.0038(18) 0.0025(16) C3 0.013(2) 0.019(2) 0.028(3) -0.010(2) 0.002(2) 0.0040(18) C4 0.013(2) 0.015(2) 0.011(2) 0.006(2) 0.0026(18) 0.0031(17) C6 0.0146(19) 0.029(2) 0.014(2) 0.001(3) -0.002(2) -0.0027(17) C7 0.017(2) 0.056(4) 0.019(3) 0.012(3) 0.004(2) 0.008(2) C8 0.019(3) 0.092(5) 0.020(3) 0.009(4) 0.004(2) 0.014(3) C9 0.028(3) 0.140(8) 0.037(4) 0.027(5) -0.001(3) 0.019(4) C10 0.062(5) 0.160(10) 0.041(5) 0.060(6) 0.026(4) 0.077(6) C11 0.090(6) 0.074(5) 0.043(5) 0.029(5) 0.025(4) 0.058(5) C12 0.063(4) 0.042(4) 0.021(3) 0.013(3) 0.016(3) 0.034(3) C13 0.104(5) 0.029(3) 0.049(6) 0.006(4) 0.018(4) 0.008(3) C14 0.036(3) 0.097(6) 0.037(4) -0.008(4) -0.006(3) -0.015(4) C15 0.0083(19) 0.014(2) 0.013(2) -0.001(2) 0.0016(17) 0.0013(16) C16 0.012(2) 0.017(2) 0.015(3) 0.004(2) -0.0008(18) -0.0015(18) C17 0.019(2) 0.030(3) 0.011(3) -0.001(2) -0.0041(19) 0.003(2) C18 0.026(2) 0.027(3) 0.019(3) -0.008(2) -0.002(2) 0.000(2) C19 0.027(2) 0.016(2) 0.025(3) -0.003(2) -0.001(2) -0.002(2) C20 0.014(2) 0.015(2) 0.018(3) 0.002(2) 0.0001(19) -0.0001(18) C21 0.030(2) 0.016(2) 0.023(3) 0.003(2) -0.004(2) -0.0025(18) C22 0.025(2) 0.019(2) 0.021(3) 0.005(2) 0.000(2) 0.004(2) C23 0.066(4) 0.033(3) 0.014(3) 0.002(3) 0.004(3) -0.015(3) C24 0.021(3) 0.069(4) 0.021(3) 0.020(3) 0.001(2) 0.006(3) C25 0.085(5) 0.021(3) 0.024(3) 0.003(3) 0.010(4) 0.009(3) C26 0.035(3) 0.077(5) 0.022(3) 0.013(4) -0.003(3) -0.033(3) C27 0.047(4) 0.066(5) 0.028(4) 0.017(4) 0.020(3) 0.032(3) C28 0.013(2) 0.016(2) 0.020(3) -0.007(2) 0.001(2) -0.0043(17) C29 0.017(2) 0.021(2) 0.016(3) -0.001(2) 0.005(2) -0.0031(19) C30 0.015(2) 0.026(3) 0.032(3) -0.001(3) -0.004(2) -0.005(2) C31 0.019(2) 0.028(3) 0.034(3) 0.001(3) 0.002(2) -0.005(2) C32 0.024(2) 0.019(2) 0.025(3) -0.001(3) 0.005(3) -0.0043(17) C33 0.023(2) 0.017(2) 0.019(3) -0.003(2) -0.004(2) 0.0005(17) C34 0.029(3) 0.023(2) 0.032(3) -0.001(2) 0.000(2) 0.012(2) C35 0.024(3) 0.033(3) 0.020(3) 0.006(3) -0.005(2) -0.004(2) C36 0.017(2) 0.021(2) 0.028(3) -0.002(2) 0.011(2) 0.0036(18) C37 0.0081(15) 0.024(2) 0.020(2) -0.005(3) -0.002(2) 0.0001(15) C38 0.016(2) 0.016(2) 0.022(3) -0.004(2) 0.005(2) -0.0001(18) C39 0.014(2) 0.024(3) 0.014(3) 0.001(2) 0.0079(19) 0.0018(19) C40 0.016(2) 0.027(3) 0.010(2) -0.007(2) 0.001(2) 0.002(2) C41 0.014(2) 0.018(2) 0.020(3) -0.002(2) 0.003(2) -0.0012(19) C42 0.017(2) 0.024(2) 0.035(4) 0.005(2) 0.003(2) 0.0046(19) C43 0.020(2) 0.020(2) 0.037(4) -0.002(2) 0.002(2) 0.0071(19) C44 0.035(3) 0.049(4) 0.033(4) 0.013(3) 0.004(3) 0.021(3) C45 0.030(3) 0.034(3) 0.015(3) 0.004(2) 0.003(2) 0.003(2) P1 0.0245(7) 0.0589(11) 0.0340(10) 0.0099(9) 0.0056(7) -0.0007(8) F1 0.042(2) 0.066(3) 0.088(4) 0.004(3) -0.019(2) -0.0129(19) F2 0.0377(19) 0.142(4) 0.098(4) -0.060(4) -0.018(3) 0.012(2) F3 0.059(2) 0.096(3) 0.059(3) -0.009(3) -0.012(2) 0.031(2) F4 0.046(3) 0.073(3) 0.173(6) -0.036(3) 0.001(3) 0.016(2) F5 0.137(4) 0.086(3) 0.053(3) -0.006(3) 0.044(3) -0.064(3) F6 0.109(4) 0.172(5) 0.068(4) 0.074(4) 0.021(3) 0.002(4) O2 0.0227(16) 0.0186(17) 0.031(2) -0.0080(17) 0.0059(15) -0.0023(14) C46 0.024(2) 0.023(2) 0.032(3) -0.004(3) 0.004(2) 0.006(2) C47 0.042(3) 0.036(3) 0.049(4) -0.020(3) 0.005(3) 0.002(3) C48 0.044(3) 0.044(4) 0.043(5) -0.025(3) -0.013(3) 0.010(3) C49 0.028(3) 0.030(3) 0.046(4) -0.013(3) -0.004(3) -0.009(2) _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 Ru1 C4 2.014(4) . ? Ru1 N1 2.073(3) . ? Ru1 C40 2.178(5) . ? Ru1 C37 2.242(3) . ? Ru1 C38 2.242(4) . ? Ru1 C39 2.262(5) . ? Ru1 C41 2.286(5) . ? Ru1 C36 2.349(4) . ? Ru1 Cl1 2.4116(13) . ? Fe1 C1 1.773(5) . ? Fe1 C6 1.821(5) . ? Fe1 C2 1.998(4) . ? Fe1 C25 2.087(6) . ? Fe1 C24 2.094(6) . ? Fe1 C26 2.095(6) . ? Fe1 C23 2.112(6) . ? Fe1 C27 2.118(6) . ? N1 C2 1.315(5) . ? N1 C15 1.441(6) . ? N2 C6 1.179(6) . ? N2 C7 1.404(7) . ? N3 C4 1.376(5) . ? N3 C2 1.410(5) . ? N3 C3 1.482(5) . ? N4 C4 1.329(6) . ? N4 C28 1.446(5) . ? N4 H4 0.8600 . ? O1 C1 1.146(6) . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C7 C12 1.398(8) . ? C7 C8 1.401(9) . ? C8 C9 1.378(9) . ? C8 C14 1.502(9) . ? C9 C10 1.378(12) . ? C9 H9 0.9300 . ? C10 C11 1.350(13) . ? C10 H10 0.9300 . ? C11 C12 1.380(9) . ? C11 H11 0.9300 . ? C12 C13 1.489(9) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C20 1.396(6) . ? C15 C16 1.404(6) . ? C16 C17 1.393(6) . ? C16 C22 1.512(6) . ? C17 C18 1.391(6) . ? C17 H17 0.9300 . ? C18 C19 1.372(7) . ? C18 H18 0.9300 . ? C19 C20 1.395(7) . ? C19 H19 0.9300 . ? C20 C21 1.496(7) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 C27 1.383(8) . ? C23 C24 1.397(8) . ? C23 H23 0.9300 . ? C24 C25 1.376(8) . ? C24 H24 0.9300 . ? C25 C26 1.398(8) . ? C25 H25 0.9300 . ? C26 C27 1.368(9) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 C33 1.382(7) . ? C28 C29 1.403(6) . ? C29 C30 1.383(6) . ? C29 C35 1.493(7) . ? C30 C31 1.372(7) . ? C30 H30 0.9300 . ? C31 C32 1.389(7) . ? C31 H31 0.9300 . ? C32 C33 1.389(6) . ? C32 H32 0.9300 . ? C33 C34 1.522(6) . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 C41 1.385(7) . ? C36 C37 1.439(6) . ? C36 C42 1.518(7) . ? C37 C38 1.410(7) . ? C37 H37 0.9300 . ? C38 C39 1.417(7) . ? C38 H38 0.9300 . ? C39 C40 1.405(6) . ? C39 C45 1.509(7) . ? C40 C41 1.431(7) . ? C40 H40 0.9300 . ? C41 H41 0.9300 . ? C42 C44 1.511(8) . ? C42 C43 1.532(6) . ? C42 H42 1.02(6) . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? P1 F5 1.570(4) . ? P1 F4 1.574(5) . ? P1 F6 1.577(5) . ? P1 F1 1.582(4) . ? P1 F2 1.583(4) . ? P1 F3 1.595(4) . ? O2 C49 1.439(6) . ? O2 C46 1.442(6) . ? C46 C47 1.493(7) . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C47 C48 1.504(7) . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C48 C49 1.485(8) . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? 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 C4 Ru1 N1 75.83(15) . . ? C4 Ru1 C40 132.17(19) . . ? N1 Ru1 C40 93.23(16) . . ? C4 Ru1 C37 119.49(17) . . ? N1 Ru1 C37 164.39(14) . . ? C40 Ru1 C37 78.6(2) . . ? C4 Ru1 C38 101.17(17) . . ? N1 Ru1 C38 149.78(16) . . ? C40 Ru1 C38 66.12(18) . . ? C37 Ru1 C38 36.66(17) . . ? C4 Ru1 C39 106.05(17) . . ? N1 Ru1 C39 114.36(16) . . ? C40 Ru1 C39 36.85(17) . . ? C37 Ru1 C39 66.4(2) . . ? C38 Ru1 C39 36.66(17) . . ? C4 Ru1 C41 169.26(19) . . ? N1 Ru1 C41 100.54(15) . . ? C40 Ru1 C41 37.29(18) . . ? C37 Ru1 C41 64.97(17) . . ? C38 Ru1 C41 76.76(17) . . ? C39 Ru1 C41 65.91(17) . . ? C4 Ru1 C36 153.39(18) . . ? N1 Ru1 C36 127.97(15) . . ? C40 Ru1 C36 65.13(18) . . ? C37 Ru1 C36 36.44(14) . . ? C38 Ru1 C36 64.82(16) . . ? C39 Ru1 C36 76.75(17) . . ? C41 Ru1 C36 34.73(17) . . ? C4 Ru1 Cl1 79.78(14) . . ? N1 Ru1 Cl1 84.86(10) . . ? C40 Ru1 Cl1 146.52(14) . . ? C37 Ru1 Cl1 94.57(16) . . ? C38 Ru1 Cl1 124.68(13) . . ? C39 Ru1 Cl1 160.67(12) . . ? C41 Ru1 Cl1 110.18(13) . . ? C36 Ru1 Cl1 89.89(13) . . ? C1 Fe1 C6 90.4(2) . . ? C1 Fe1 C2 100.47(19) . . ? C6 Fe1 C2 93.26(18) . . ? C1 Fe1 C25 90.0(2) . . ? C6 Fe1 C25 154.6(2) . . ? C2 Fe1 C25 111.7(2) . . ? C1 Fe1 C24 123.3(3) . . ? C6 Fe1 C24 146.0(3) . . ? C2 Fe1 C24 85.68(19) . . ? C25 Fe1 C24 38.4(2) . . ? C1 Fe1 C26 89.9(2) . . ? C6 Fe1 C26 115.5(2) . . ? C2 Fe1 C26 149.4(2) . . ? C25 Fe1 C26 39.1(2) . . ? C24 Fe1 C26 64.9(2) . . ? C1 Fe1 C23 152.7(2) . . ? C6 Fe1 C23 108.4(3) . . ? C2 Fe1 C23 98.1(2) . . ? C25 Fe1 C23 64.5(2) . . ? C24 Fe1 C23 38.8(2) . . ? C26 Fe1 C23 64.3(2) . . ? C1 Fe1 C27 123.1(3) . . ? C6 Fe1 C27 94.8(2) . . ? C2 Fe1 C27 135.5(3) . . ? C25 Fe1 C27 64.1(2) . . ? C24 Fe1 C27 64.3(2) . . ? C26 Fe1 C27 37.9(3) . . ? C23 Fe1 C27 38.2(2) . . ? C2 N1 C15 120.2(3) . . ? C2 N1 Ru1 119.3(3) . . ? C15 N1 Ru1 120.2(3) . . ? C6 N2 C7 168.9(5) . . ? C4 N3 C2 117.8(4) . . ? C4 N3 C3 119.9(4) . . ? C2 N3 C3 122.1(3) . . ? C4 N4 C28 123.9(4) . . ? C4 N4 H4 118.0 . . ? C28 N4 H4 118.0 . . ? O1 C1 Fe1 168.5(4) . . ? N1 C2 N3 110.3(3) . . ? N1 C2 Fe1 127.4(3) . . ? N3 C2 Fe1 121.5(3) . . ? N3 C3 H3A 109.5 . . ? N3 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N3 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N4 C4 N3 113.8(4) . . ? N4 C4 Ru1 130.7(3) . . ? N3 C4 Ru1 115.2(3) . . ? N2 C6 Fe1 175.5(5) . . ? C12 C7 C8 123.5(6) . . ? C12 C7 N2 119.0(5) . . ? C8 C7 N2 117.4(6) . . ? C9 C8 C7 115.7(7) . . ? C9 C8 C14 121.8(7) . . ? C7 C8 C14 122.4(6) . . ? C10 C9 C8 122.7(8) . . ? C10 C9 H9 118.7 . . ? C8 C9 H9 118.7 . . ? C11 C10 C9 118.9(7) . . ? C11 C10 H10 120.5 . . ? C9 C10 H10 120.5 . . ? C10 C11 C12 123.2(8) . . ? C10 C11 H11 118.4 . . ? C12 C11 H11 118.4 . . ? C11 C12 C7 115.9(7) . . ? C11 C12 C13 123.0(7) . . ? C7 C12 C13 121.1(5) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C8 C14 H14A 109.5 . . ? C8 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C8 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C20 C15 C16 122.1(4) . . ? C20 C15 N1 121.0(4) . . ? C16 C15 N1 116.8(4) . . ? C17 C16 C15 118.0(4) . . ? C17 C16 C22 119.1(4) . . ? C15 C16 C22 122.8(4) . . ? C18 C17 C16 120.9(5) . . ? C18 C17 H17 119.5 . . ? C16 C17 H17 119.5 . . ? C19 C18 C17 119.4(5) . . ? C19 C18 H18 120.3 . . ? C17 C18 H18 120.3 . . ? C18 C19 C20 122.3(5) . . ? C18 C19 H19 118.8 . . ? C20 C19 H19 118.8 . . ? C19 C20 C15 117.2(5) . . ? C19 C20 C21 121.0(4) . . ? C15 C20 C21 121.7(4) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C16 C22 H22A 109.5 . . ? C16 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C16 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C27 C23 C24 107.4(6) . . ? C27 C23 Fe1 71.1(4) . . ? C24 C23 Fe1 69.9(3) . . ? C27 C23 H23 126.3 . . ? C24 C23 H23 126.3 . . ? Fe1 C23 H23 124.3 . . ? C25 C24 C23 107.9(5) . . ? C25 C24 Fe1 70.5(3) . . ? C23 C24 Fe1 71.3(3) . . ? C25 C24 H24 126.1 . . ? C23 C24 H24 126.1 . . ? Fe1 C24 H24 123.8 . . ? C24 C25 C26 108.2(5) . . ? C24 C25 Fe1 71.1(3) . . ? C26 C25 Fe1 70.8(3) . . ? C24 C25 H25 125.9 . . ? C26 C25 H25 125.9 . . ? Fe1 C25 H25 123.9 . . ? C27 C26 C25 107.6(5) . . ? C27 C26 Fe1 72.0(3) . . ? C25 C26 Fe1 70.2(3) . . ? C27 C26 H26 126.2 . . ? C25 C26 H26 126.2 . . ? Fe1 C26 H26 123.3 . . ? C26 C27 C23 109.0(5) . . ? C26 C27 Fe1 70.1(3) . . ? C23 C27 Fe1 70.7(3) . . ? C26 C27 H27 125.5 . . ? C23 C27 H27 125.5 . . ? Fe1 C27 H27 125.3 . . ? C33 C28 C29 123.2(4) . . ? C33 C28 N4 116.7(4) . . ? C29 C28 N4 119.9(4) . . ? C30 C29 C28 116.4(5) . . ? C30 C29 C35 121.7(4) . . ? C28 C29 C35 121.9(4) . . ? C31 C30 C29 121.4(5) . . ? C31 C30 H30 119.3 . . ? C29 C30 H30 119.3 . . ? C30 C31 C32 121.1(5) . . ? C30 C31 H31 119.4 . . ? C32 C31 H31 119.4 . . ? C31 C32 C33 119.3(5) . . ? C31 C32 H32 120.3 . . ? C33 C32 H32 120.3 . . ? C28 C33 C32 118.2(4) . . ? C28 C33 C34 121.4(4) . . ? C32 C33 C34 120.4(5) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C29 C35 H35A 109.5 . . ? C29 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C29 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C41 C36 C37 118.9(4) . . ? C41 C36 C42 120.2(4) . . ? C37 C36 C42 120.8(4) . . ? C41 C36 Ru1 70.1(3) . . ? C37 C36 Ru1 67.7(2) . . ? C42 C36 Ru1 137.8(3) . . ? C38 C37 C36 119.6(5) . . ? C38 C37 Ru1 71.7(2) . . ? C36 C37 Ru1 75.8(2) . . ? C38 C37 H37 120.2 . . ? C36 C37 H37 120.2 . . ? Ru1 C37 H37 123.8 . . ? C37 C38 C39 121.5(4) . . ? C37 C38 Ru1 71.7(2) . . ? C39 C38 Ru1 72.4(3) . . ? C37 C38 H38 119.3 . . ? C39 C38 H38 119.3 . . ? Ru1 C38 H38 129.1 . . ? C40 C39 C38 117.4(4) . . ? C40 C39 C45 121.4(5) . . ? C38 C39 C45 121.1(4) . . ? C40 C39 Ru1 68.3(3) . . ? C38 C39 Ru1 70.9(3) . . ? C45 C39 Ru1 134.5(3) . . ? C39 C40 C41 121.4(4) . . ? C39 C40 Ru1 74.8(3) . . ? C41 C40 Ru1 75.4(3) . . ? C39 C40 H40 119.3 . . ? C41 C40 H40 119.3 . . ? Ru1 C40 H40 121.6 . . ? C36 C41 C40 120.2(4) . . ? C36 C41 Ru1 75.1(3) . . ? C40 C41 Ru1 67.3(3) . . ? C36 C41 H41 119.9 . . ? C40 C41 H41 119.9 . . ? Ru1 C41 H41 130.2 . . ? C44 C42 C36 116.2(4) . . ? C44 C42 C43 110.7(4) . . ? C36 C42 C43 105.6(4) . . ? C44 C42 H42 119(4) . . ? C36 C42 H42 96(3) . . ? C43 C42 H42 107(4) . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C42 C44 H44A 109.5 . . ? C42 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C42 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C39 C45 H45A 109.5 . . ? C39 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C39 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? F5 P1 F4 90.3(3) . . ? F5 P1 F6 179.0(3) . . ? F4 P1 F6 90.7(3) . . ? F5 P1 F1 90.2(3) . . ? F4 P1 F1 89.5(3) . . ? F6 P1 F1 90.1(3) . . ? F5 P1 F2 89.4(3) . . ? F4 P1 F2 90.9(2) . . ? F6 P1 F2 90.2(3) . . ? F1 P1 F2 179.4(3) . . ? F5 P1 F3 89.9(3) . . ? F4 P1 F3 179.8(3) . . ? F6 P1 F3 89.1(3) . . ? F1 P1 F3 90.6(2) . . ? F2 P1 F3 89.1(2) . . ? C49 O2 C46 108.5(4) . . ? O2 C46 C47 107.2(4) . . ? O2 C46 H46A 110.3 . . ? C47 C46 H46A 110.3 . . ? O2 C46 H46B 110.3 . . ? C47 C46 H46B 110.3 . . ? H46A C46 H46B 108.5 . . ? C46 C47 C48 104.4(4) . . ? C46 C47 H47A 110.9 . . ? C48 C47 H47A 110.9 . . ? C46 C47 H47B 110.9 . . ? C48 C47 H47B 110.9 . . ? H47A C47 H47B 108.9 . . ? C49 C48 C47 103.1(5) . . ? C49 C48 H48A 111.2 . . ? C47 C48 H48A 111.2 . . ? C49 C48 H48B 111.2 . . ? C47 C48 H48B 111.2 . . ? H48A C48 H48B 109.1 . . ? O2 C49 C48 106.6(4) . . ? O2 C49 H49A 110.4 . . ? C48 C49 H49A 110.4 . . ? O2 C49 H49B 110.4 . . ? C48 C49 H49B 110.4 . . ? H49A C49 H49B 108.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C4 Ru1 N1 C2 -11.8(3) . . . . ? C40 Ru1 N1 C2 -144.6(4) . . . . ? C37 Ru1 N1 C2 157.5(7) . . . . ? C38 Ru1 N1 C2 -99.8(4) . . . . ? C39 Ru1 N1 C2 -113.3(3) . . . . ? C41 Ru1 N1 C2 178.5(3) . . . . ? C36 Ru1 N1 C2 154.7(3) . . . . ? Cl1 Ru1 N1 C2 68.9(3) . . . . ? C4 Ru1 N1 C15 162.3(3) . . . . ? C40 Ru1 N1 C15 29.5(3) . . . . ? C37 Ru1 N1 C15 -28.4(9) . . . . ? C38 Ru1 N1 C15 74.4(4) . . . . ? C39 Ru1 N1 C15 60.8(3) . . . . ? C41 Ru1 N1 C15 -7.4(3) . . . . ? C36 Ru1 N1 C15 -31.1(4) . . . . ? Cl1 Ru1 N1 C15 -117.0(3) . . . . ? C6 Fe1 C1 O1 -89(2) . . . . ? C2 Fe1 C1 O1 177(2) . . . . ? C25 Fe1 C1 O1 65(2) . . . . ? C24 Fe1 C1 O1 86(2) . . . . ? C26 Fe1 C1 O1 26(2) . . . . ? C23 Fe1 C1 O1 45(3) . . . . ? C27 Fe1 C1 O1 7(2) . . . . ? C15 N1 C2 N3 -161.5(4) . . . . ? Ru1 N1 C2 N3 12.7(5) . . . . ? C15 N1 C2 Fe1 28.6(6) . . . . ? Ru1 N1 C2 Fe1 -157.3(2) . . . . ? C4 N3 C2 N1 -5.5(6) . . . . ? C3 N3 C2 N1 168.8(4) . . . . ? C4 N3 C2 Fe1 165.1(3) . . . . ? C3 N3 C2 Fe1 -20.5(6) . . . . ? C1 Fe1 C2 N1 -29.8(5) . . . . ? C6 Fe1 C2 N1 -120.7(4) . . . . ? C25 Fe1 C2 N1 64.4(5) . . . . ? C24 Fe1 C2 N1 93.3(5) . . . . ? C26 Fe1 C2 N1 78.3(7) . . . . ? C23 Fe1 C2 N1 130.1(4) . . . . ? C27 Fe1 C2 N1 139.0(4) . . . . ? C1 Fe1 C2 N3 161.3(4) . . . . ? C6 Fe1 C2 N3 70.3(4) . . . . ? C25 Fe1 C2 N3 -104.5(4) . . . . ? C24 Fe1 C2 N3 -75.6(4) . . . . ? C26 Fe1 C2 N3 -90.6(6) . . . . ? C23 Fe1 C2 N3 -38.8(4) . . . . ? C27 Fe1 C2 N3 -30.0(5) . . . . ? C28 N4 C4 N3 -164.0(4) . . . . ? C28 N4 C4 Ru1 23.0(7) . . . . ? C2 N3 C4 N4 -178.1(4) . . . . ? C3 N3 C4 N4 7.5(6) . . . . ? C2 N3 C4 Ru1 -4.0(5) . . . . ? C3 N3 C4 Ru1 -178.4(3) . . . . ? N1 Ru1 C4 N4 -179.3(5) . . . . ? C40 Ru1 C4 N4 -98.0(5) . . . . ? C37 Ru1 C4 N4 4.0(5) . . . . ? C38 Ru1 C4 N4 -30.2(5) . . . . ? C39 Ru1 C4 N4 -67.6(5) . . . . ? C41 Ru1 C4 N4 -107.9(9) . . . . ? C36 Ru1 C4 N4 24.8(7) . . . . ? Cl1 Ru1 C4 N4 93.5(4) . . . . ? N1 Ru1 C4 N3 7.8(3) . . . . ? C40 Ru1 C4 N3 89.1(4) . . . . ? C37 Ru1 C4 N3 -168.9(3) . . . . ? C38 Ru1 C4 N3 156.9(3) . . . . ? C39 Ru1 C4 N3 119.5(3) . . . . ? C41 Ru1 C4 N3 79.2(10) . . . . ? C36 Ru1 C4 N3 -148.1(3) . . . . ? Cl1 Ru1 C4 N3 -79.4(3) . . . . ? C6 N2 C7 C12 170(2) . . . . ? C6 N2 C7 C8 -10(3) . . . . ? C12 C7 C8 C9 -2.3(8) . . . . ? N2 C7 C8 C9 177.6(5) . . . . ? C12 C7 C8 C14 175.1(6) . . . . ? N2 C7 C8 C14 -5.0(8) . . . . ? C7 C8 C9 C10 2.1(10) . . . . ? C14 C8 C9 C10 -175.3(7) . . . . ? C8 C9 C10 C11 -0.9(12) . . . . ? C9 C10 C11 C12 -0.1(12) . . . . ? C10 C11 C12 C7 -0.1(10) . . . . ? C10 C11 C12 C13 179.0(7) . . . . ? C8 C7 C12 C11 1.4(9) . . . . ? N2 C7 C12 C11 -178.5(5) . . . . ? C8 C7 C12 C13 -177.7(6) . . . . ? N2 C7 C12 C13 2.3(8) . . . . ? C2 N1 C15 C20 -107.8(5) . . . . ? Ru1 N1 C15 C20 78.1(4) . . . . ? C2 N1 C15 C16 75.8(5) . . . . ? Ru1 N1 C15 C16 -98.2(4) . . . . ? C20 C15 C16 C17 0.8(6) . . . . ? N1 C15 C16 C17 177.1(4) . . . . ? C20 C15 C16 C22 178.8(4) . . . . ? N1 C15 C16 C22 -5.0(6) . . . . ? C15 C16 C17 C18 0.5(6) . . . . ? C22 C16 C17 C18 -177.5(4) . . . . ? C16 C17 C18 C19 -1.7(7) . . . . ? C17 C18 C19 C20 1.5(7) . . . . ? C18 C19 C20 C15 -0.2(7) . . . . ? C18 C19 C20 C21 178.3(4) . . . . ? C16 C15 C20 C19 -1.0(6) . . . . ? N1 C15 C20 C19 -177.1(4) . . . . ? C16 C15 C20 C21 -179.5(4) . . . . ? N1 C15 C20 C21 4.4(6) . . . . ? C1 Fe1 C23 C27 -57.5(7) . . . . ? C6 Fe1 C23 C27 73.8(4) . . . . ? C2 Fe1 C23 C27 170.0(4) . . . . ? C25 Fe1 C23 C27 -79.8(4) . . . . ? C24 Fe1 C23 C27 -117.4(5) . . . . ? C26 Fe1 C23 C27 -36.3(4) . . . . ? C1 Fe1 C23 C24 60.0(6) . . . . ? C6 Fe1 C23 C24 -168.8(3) . . . . ? C2 Fe1 C23 C24 -72.6(4) . . . . ? C25 Fe1 C23 C24 37.6(3) . . . . ? C26 Fe1 C23 C24 81.1(4) . . . . ? C27 Fe1 C23 C24 117.4(5) . . . . ? C27 C23 C24 C25 0.3(7) . . . . ? Fe1 C23 C24 C25 -61.4(4) . . . . ? C27 C23 C24 Fe1 61.6(4) . . . . ? C1 Fe1 C24 C25 -34.0(4) . . . . ? C6 Fe1 C24 C25 136.9(4) . . . . ? C2 Fe1 C24 C25 -133.7(4) . . . . ? C26 Fe1 C24 C25 37.9(4) . . . . ? C23 Fe1 C24 C25 117.6(5) . . . . ? C27 Fe1 C24 C25 80.1(4) . . . . ? C1 Fe1 C24 C23 -151.6(3) . . . . ? C6 Fe1 C24 C23 19.3(5) . . . . ? C2 Fe1 C24 C23 108.7(4) . . . . ? C25 Fe1 C24 C23 -117.6(5) . . . . ? C26 Fe1 C24 C23 -79.7(4) . . . . ? C27 Fe1 C24 C23 -37.5(4) . . . . ? C23 C24 C25 C26 0.5(7) . . . . ? Fe1 C24 C25 C26 -61.4(4) . . . . ? C23 C24 C25 Fe1 61.9(4) . . . . ? C1 Fe1 C25 C24 152.1(4) . . . . ? C6 Fe1 C25 C24 -117.2(6) . . . . ? C2 Fe1 C25 C24 50.9(4) . . . . ? C26 Fe1 C25 C24 -117.9(5) . . . . ? C23 Fe1 C25 C24 -38.0(3) . . . . ? C27 Fe1 C25 C24 -80.5(4) . . . . ? C1 Fe1 C25 C26 -89.9(4) . . . . ? C6 Fe1 C25 C26 0.8(8) . . . . ? C2 Fe1 C25 C26 168.8(4) . . . . ? C24 Fe1 C25 C26 117.9(5) . . . . ? C23 Fe1 C25 C26 80.0(4) . . . . ? C27 Fe1 C25 C26 37.4(4) . . . . ? C24 C25 C26 C27 -1.1(7) . . . . ? Fe1 C25 C26 C27 -62.6(4) . . . . ? C24 C25 C26 Fe1 61.6(4) . . . . ? C1 Fe1 C26 C27 -152.9(4) . . . . ? C6 Fe1 C26 C27 -62.5(4) . . . . ? C2 Fe1 C26 C27 96.3(6) . . . . ? C25 Fe1 C26 C27 117.1(5) . . . . ? C24 Fe1 C26 C27 79.7(4) . . . . ? C23 Fe1 C26 C27 36.6(4) . . . . ? C1 Fe1 C26 C25 90.0(4) . . . . ? C6 Fe1 C26 C25 -179.6(4) . . . . ? C2 Fe1 C26 C25 -20.8(7) . . . . ? C24 Fe1 C26 C25 -37.3(4) . . . . ? C23 Fe1 C26 C25 -80.5(4) . . . . ? C27 Fe1 C26 C25 -117.1(5) . . . . ? C25 C26 C27 C23 1.2(7) . . . . ? Fe1 C26 C27 C23 -60.2(4) . . . . ? C25 C26 C27 Fe1 61.5(4) . . . . ? C24 C23 C27 C26 -0.9(7) . . . . ? Fe1 C23 C27 C26 59.9(4) . . . . ? C24 C23 C27 Fe1 -60.8(4) . . . . ? C1 Fe1 C27 C26 32.9(5) . . . . ? C6 Fe1 C27 C26 126.5(4) . . . . ? C2 Fe1 C27 C26 -133.8(4) . . . . ? C25 Fe1 C27 C26 -38.6(4) . . . . ? C24 Fe1 C27 C26 -81.5(4) . . . . ? C23 Fe1 C27 C26 -119.6(5) . . . . ? C1 Fe1 C27 C23 152.5(4) . . . . ? C6 Fe1 C27 C23 -113.9(4) . . . . ? C2 Fe1 C27 C23 -14.2(5) . . . . ? C25 Fe1 C27 C23 81.0(4) . . . . ? C24 Fe1 C27 C23 38.1(4) . . . . ? C26 Fe1 C27 C23 119.6(5) . . . . ? C4 N4 C28 C33 88.2(6) . . . . ? C4 N4 C28 C29 -95.4(6) . . . . ? C33 C28 C29 C30 -5.9(7) . . . . ? N4 C28 C29 C30 178.0(4) . . . . ? C33 C28 C29 C35 173.6(5) . . . . ? N4 C28 C29 C35 -2.5(7) . . . . ? C28 C29 C30 C31 2.1(7) . . . . ? C35 C29 C30 C31 -177.5(5) . . . . ? C29 C30 C31 C32 1.0(8) . . . . ? C30 C31 C32 C33 -0.6(8) . . . . ? C29 C28 C33 C32 6.4(7) . . . . ? N4 C28 C33 C32 -177.4(4) . . . . ? C29 C28 C33 C34 -174.2(4) . . . . ? N4 C28 C33 C34 2.1(7) . . . . ? C31 C32 C33 C28 -3.0(7) . . . . ? C31 C32 C33 C34 177.6(5) . . . . ? C4 Ru1 C36 C41 -166.1(4) . . . . ? N1 Ru1 C36 C41 44.1(4) . . . . ? C40 Ru1 C36 C41 -29.5(3) . . . . ? C37 Ru1 C36 C41 -134.7(5) . . . . ? C38 Ru1 C36 C41 -103.5(3) . . . . ? C39 Ru1 C36 C41 -66.6(3) . . . . ? Cl1 Ru1 C36 C41 127.5(3) . . . . ? C4 Ru1 C36 C37 -31.4(6) . . . . ? N1 Ru1 C36 C37 178.8(3) . . . . ? C40 Ru1 C36 C37 105.2(4) . . . . ? C38 Ru1 C36 C37 31.2(3) . . . . ? C39 Ru1 C36 C37 68.0(3) . . . . ? C41 Ru1 C36 C37 134.7(5) . . . . ? Cl1 Ru1 C36 C37 -97.9(3) . . . . ? C4 Ru1 C36 C42 80.4(6) . . . . ? N1 Ru1 C36 C42 -69.4(6) . . . . ? C40 Ru1 C36 C42 -143.0(6) . . . . ? C37 Ru1 C36 C42 111.8(7) . . . . ? C38 Ru1 C36 C42 143.0(6) . . . . ? C39 Ru1 C36 C42 179.8(6) . . . . ? C41 Ru1 C36 C42 -113.5(6) . . . . ? Cl1 Ru1 C36 C42 13.9(5) . . . . ? C41 C36 C37 C38 -9.1(7) . . . . ? C42 C36 C37 C38 167.6(4) . . . . ? Ru1 C36 C37 C38 -58.9(3) . . . . ? C41 C36 C37 Ru1 49.8(4) . . . . ? C42 C36 C37 Ru1 -133.5(4) . . . . ? C4 Ru1 C37 C38 -67.2(4) . . . . ? N1 Ru1 C37 C38 124.7(6) . . . . ? C40 Ru1 C37 C38 65.1(3) . . . . ? C39 Ru1 C37 C38 28.5(3) . . . . ? C41 Ru1 C37 C38 101.8(4) . . . . ? C36 Ru1 C37 C38 128.3(5) . . . . ? Cl1 Ru1 C37 C38 -148.1(3) . . . . ? C4 Ru1 C37 C36 164.4(3) . . . . ? N1 Ru1 C37 C36 -3.6(9) . . . . ? C40 Ru1 C37 C36 -63.3(3) . . . . ? C38 Ru1 C37 C36 -128.3(5) . . . . ? C39 Ru1 C37 C36 -99.8(4) . . . . ? C41 Ru1 C37 C36 -26.6(3) . . . . ? Cl1 Ru1 C37 C36 83.6(3) . . . . ? C36 C37 C38 C39 6.2(7) . . . . ? Ru1 C37 C38 C39 -54.9(4) . . . . ? C36 C37 C38 Ru1 61.0(4) . . . . ? C4 Ru1 C38 C37 125.1(3) . . . . ? N1 Ru1 C38 C37 -153.9(3) . . . . ? C40 Ru1 C38 C37 -103.5(3) . . . . ? C39 Ru1 C38 C37 -133.0(4) . . . . ? C41 Ru1 C38 C37 -65.7(3) . . . . ? C36 Ru1 C38 C37 -31.0(3) . . . . ? Cl1 Ru1 C38 C37 39.9(3) . . . . ? C4 Ru1 C38 C39 -101.9(3) . . . . ? N1 Ru1 C38 C39 -21.0(5) . . . . ? C40 Ru1 C38 C39 29.4(3) . . . . ? C37 Ru1 C38 C39 133.0(4) . . . . ? C41 Ru1 C38 C39 67.3(3) . . . . ? C36 Ru1 C38 C39 102.0(3) . . . . ? Cl1 Ru1 C38 C39 172.8(2) . . . . ? C37 C38 C39 C40 2.8(7) . . . . ? Ru1 C38 C39 C40 -51.7(4) . . . . ? C37 C38 C39 C45 -174.4(4) . . . . ? Ru1 C38 C39 C45 131.1(4) . . . . ? C37 C38 C39 Ru1 54.5(4) . . . . ? C4 Ru1 C39 C40 -141.3(3) . . . . ? N1 Ru1 C39 C40 -59.9(3) . . . . ? C37 Ru1 C39 C40 103.0(3) . . . . ? C38 Ru1 C39 C40 131.5(4) . . . . ? C41 Ru1 C39 C40 31.1(3) . . . . ? C36 Ru1 C39 C40 66.0(3) . . . . ? Cl1 Ru1 C39 C40 113.4(4) . . . . ? C4 Ru1 C39 C38 87.2(3) . . . . ? N1 Ru1 C39 C38 168.6(2) . . . . ? C40 Ru1 C39 C38 -131.5(4) . . . . ? C37 Ru1 C39 C38 -28.5(3) . . . . ? C41 Ru1 C39 C38 -100.4(3) . . . . ? C36 Ru1 C39 C38 -65.4(3) . . . . ? Cl1 Ru1 C39 C38 -18.0(6) . . . . ? C4 Ru1 C39 C45 -28.0(5) . . . . ? N1 Ru1 C39 C45 53.4(5) . . . . ? C40 Ru1 C39 C45 113.3(6) . . . . ? C37 Ru1 C39 C45 -143.7(5) . . . . ? C38 Ru1 C39 C45 -115.2(6) . . . . ? C41 Ru1 C39 C45 144.4(5) . . . . ? C36 Ru1 C39 C45 179.4(5) . . . . ? Cl1 Ru1 C39 C45 -133.2(4) . . . . ? C38 C39 C40 C41 -9.0(7) . . . . ? C45 C39 C40 C41 168.2(4) . . . . ? Ru1 C39 C40 C41 -61.9(4) . . . . ? C38 C39 C40 Ru1 52.9(4) . . . . ? C45 C39 C40 Ru1 -129.9(4) . . . . ? C4 Ru1 C40 C39 54.1(4) . . . . ? N1 Ru1 C40 C39 127.8(3) . . . . ? C37 Ru1 C40 C39 -65.6(3) . . . . ? C38 Ru1 C40 C39 -29.3(3) . . . . ? C41 Ru1 C40 C39 -129.0(4) . . . . ? C36 Ru1 C40 C39 -101.4(3) . . . . ? Cl1 Ru1 C40 C39 -146.6(2) . . . . ? C4 Ru1 C40 C41 -177.0(2) . . . . ? N1 Ru1 C40 C41 -103.2(3) . . . . ? C37 Ru1 C40 C41 63.4(3) . . . . ? C38 Ru1 C40 C41 99.7(3) . . . . ? C39 Ru1 C40 C41 129.0(4) . . . . ? C36 Ru1 C40 C41 27.6(2) . . . . ? Cl1 Ru1 C40 C41 -17.6(4) . . . . ? C37 C36 C41 C40 3.2(7) . . . . ? C42 C36 C41 C40 -173.6(4) . . . . ? Ru1 C36 C41 C40 51.9(4) . . . . ? C37 C36 C41 Ru1 -48.7(4) . . . . ? C42 C36 C41 Ru1 134.5(4) . . . . ? C39 C40 C41 C36 6.1(7) . . . . ? Ru1 C40 C41 C36 -55.5(4) . . . . ? C39 C40 C41 Ru1 61.6(4) . . . . ? C4 Ru1 C41 C36 144.7(8) . . . . ? N1 Ru1 C41 C36 -146.1(3) . . . . ? C40 Ru1 C41 C36 132.5(4) . . . . ? C37 Ru1 C41 C36 27.8(3) . . . . ? C38 Ru1 C41 C36 64.7(3) . . . . ? C39 Ru1 C41 C36 101.8(3) . . . . ? Cl1 Ru1 C41 C36 -57.8(3) . . . . ? C4 Ru1 C41 C40 12.2(10) . . . . ? N1 Ru1 C41 C40 81.4(3) . . . . ? C37 Ru1 C41 C40 -104.7(3) . . . . ? C38 Ru1 C41 C40 -67.8(3) . . . . ? C39 Ru1 C41 C40 -30.7(3) . . . . ? C36 Ru1 C41 C40 -132.5(4) . . . . ? Cl1 Ru1 C41 C40 169.7(2) . . . . ? C41 C36 C42 C44 -149.5(5) . . . . ? C37 C36 C42 C44 33.8(6) . . . . ? Ru1 C36 C42 C44 -56.2(7) . . . . ? C41 C36 C42 C43 87.3(5) . . . . ? C37 C36 C42 C43 -89.4(6) . . . . ? Ru1 C36 C42 C43 -179.4(4) . . . . ? C49 O2 C46 C47 0.7(6) . . . . ? O2 C46 C47 C48 -19.9(6) . . . . ? C46 C47 C48 C49 30.7(6) . . . . ? C46 O2 C49 C48 19.3(6) . . . . ? C47 C48 C49 O2 -31.0(6) . . . . ? _diffrn_measured_fraction_theta_max 0.912 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.532 _refine_diff_density_min -0.779 _refine_diff_density_rms 0.111 _database_code_depnum_ccdc_archive 'CCDC 951024'