# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 222 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Andy Hor' 'Christopher Corkery' 'Qingchun Ge.' 'Mark Humphrey' 'Marek Samoc' _publ_contact_author_name 'T. S. Andy Hor' _publ_contact_author_email ANDYHOR@NUS.EDU.SG _publ_section_title ; Organobimetallic RuII-ReI 4-Ethynylpyridyl Complexes: Structures & Non-Linear Optical Properties ; # Attachment 'all_cif.txt' data_7281a _database_code_depnum_ccdc_archive 'CCDC 721189' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C63 H52 F6 Fe N4 O3 P3 Re Ru' _chemical_formula_weight 1463.12 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' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.2310 '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 Pna2(1) 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 16.5888(12) _cell_length_b 14.2533(9) _cell_length_c 24.6169(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5820.5(7) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.670 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2904 _exptl_absorpt_coefficient_mu 2.728 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.4083 _exptl_absorpt_correction_T_max 0.9475 _exptl_absorpt_process_details 'Sadabs, (Sheldrick 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42083 _diffrn_reflns_av_R_equivalents 0.0947 _diffrn_reflns_av_sigmaI/netI 0.1060 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 0.83 _diffrn_reflns_theta_max 27.49 _reflns_number_total 12734 _reflns_number_gt 9841 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0331P)^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 0.00(8) _refine_ls_number_reflns 12734 _refine_ls_number_parameters 729 _refine_ls_number_restraints 110 _refine_ls_R_factor_all 0.0921 _refine_ls_R_factor_gt 0.0651 _refine_ls_wR_factor_ref 0.1107 _refine_ls_wR_factor_gt 0.1020 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.072 _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 Re1 Re 0.41196(2) 0.09785(2) 0.089159(18) 0.03063(9) Uani 1 1 d . . . Ru1 Ru 0.47363(4) 0.46976(5) 0.41144(3) 0.02736(16) Uani 1 1 d . . . Fe1 Fe 0.69307(8) 0.33099(8) 0.35463(5) 0.0321(3) Uani 1 1 d . . . P1 P 0.55066(16) 0.36291(19) 0.45691(10) 0.0327(6) Uani 1 1 d . . . P2 P 0.57443(14) 0.53183(16) 0.35960(10) 0.0272(5) Uani 1 1 d . . . O1 O 0.4297(5) 0.2783(6) 0.0233(3) 0.062(2) Uani 1 1 d . . . O2 O 0.3872(5) -0.0120(6) -0.0156(4) 0.076(3) Uani 1 1 d . . . O3 O 0.5961(4) 0.0827(5) 0.0782(4) 0.057(2) Uani 1 1 d . . . N1 N 0.4196(4) 0.1761(5) 0.1663(3) 0.0288(18) Uani 1 1 d . . . N2 N 0.2831(4) 0.1038(4) 0.1029(2) 0.0249(17) Uani 1 1 d . . . N3 N 0.3885(5) -0.0163(5) 0.1447(3) 0.0310(19) Uani 1 1 d . . . C1 C 0.4160(6) 0.5286(10) 0.4854(5) 0.060(3) Uani 1 1 d . . . H1 H 0.4349 0.5187 0.5231 0.072 Uiso 1 1 calc R . . C2 C 0.4367(6) 0.6032(8) 0.4526(5) 0.057(4) Uani 1 1 d . . . H2 H 0.4724 0.6562 0.4624 0.069 Uiso 1 1 calc R . . C3 C 0.3903(7) 0.5942(7) 0.4039(5) 0.049(3) Uani 1 1 d . . . H3 H 0.3900 0.6395 0.3734 0.059 Uiso 1 1 calc R . . C4 C 0.3444(6) 0.5155(6) 0.4069(5) 0.042(2) Uani 1 1 d . . . H4 H 0.3048 0.4947 0.3793 0.050 Uiso 1 1 calc R . . C5 C 0.3588(6) 0.4713(7) 0.4574(5) 0.046(3) Uani 1 1 d . . . H5 H 0.3300 0.4162 0.4723 0.055 Uiso 1 1 calc R . . C6 C 0.4557(5) 0.3747(6) 0.3544(4) 0.029(2) Uani 1 1 d . . . C7 C 0.4412(6) 0.3205(6) 0.3163(4) 0.031(2) Uani 1 1 d . . . C8 C 0.3697(5) 0.2454(5) 0.1807(4) 0.026(2) Uani 1 1 d . . . H8 H 0.3289 0.2619 0.1560 0.031 Uiso 1 1 calc R . . C9 C 0.3732(5) 0.2947(6) 0.2288(4) 0.028(2) Uani 1 1 d . . . H9 H 0.3362 0.3429 0.2361 0.033 Uiso 1 1 calc R . . C10 C 0.4333(5) 0.2713(6) 0.2668(4) 0.027(2) Uani 1 1 d . . . C11 C 0.4864(6) 0.1990(6) 0.2522(4) 0.038(2) Uani 1 1 d . . . H11 H 0.5278 0.1810 0.2761 0.046 Uiso 1 1 calc R . . C12 C 0.4780(6) 0.1543(6) 0.2031(4) 0.030(2) Uani 1 1 d . . . H12 H 0.5145 0.1062 0.1944 0.036 Uiso 1 1 calc R . . C13 C 0.2319(6) 0.1628(6) 0.0796(4) 0.037(2) Uani 1 1 d . . . H13 H 0.2525 0.2049 0.0537 0.044 Uiso 1 1 calc R . . C14 C 0.1509(5) 0.1666(5) 0.0906(5) 0.038(2) Uani 1 1 d . . . H14 H 0.1181 0.2107 0.0728 0.046 Uiso 1 1 calc R . . C15 C 0.1177(5) 0.1055(6) 0.1280(3) 0.027(2) Uani 1 1 d . . . C16 C 0.1706(5) 0.0437(6) 0.1527(4) 0.031(2) Uani 1 1 d . . . H16 H 0.1504 0.0006 0.1783 0.038 Uiso 1 1 calc R . . C17 C 0.2520(6) 0.0433(6) 0.1410(3) 0.030(2) Uani 1 1 d . . . C18 C 0.3122(5) -0.0203(6) 0.1666(4) 0.030(2) Uani 1 1 d . . . C19 C 0.2952(6) -0.0769(6) 0.2099(4) 0.035(2) Uani 1 1 d . . . H19 H 0.2429 -0.0763 0.2246 0.042 Uiso 1 1 calc R . . C20 C 0.3530(7) -0.1352(6) 0.2328(5) 0.048(3) Uani 1 1 d . . . C21 C 0.4267(6) -0.1291(7) 0.2112(5) 0.045(3) Uani 1 1 d . . . H21 H 0.4687 -0.1642 0.2268 0.054 Uiso 1 1 calc R . . C22 C 0.4435(6) -0.0735(6) 0.1668(5) 0.044(3) Uani 1 1 d . . . H22 H 0.4954 -0.0758 0.1515 0.053 Uiso 1 1 calc R . . C23 C 0.0285(6) 0.1066(7) 0.1418(5) 0.051(3) Uani 1 1 d . . . H23A H -0.0010 0.0711 0.1147 0.077 Uiso 1 1 calc R . . H23B H 0.0092 0.1708 0.1423 0.077 Uiso 1 1 calc R . . H23C H 0.0204 0.0784 0.1773 0.077 Uiso 1 1 calc R . . C24 C 0.3332(7) -0.1931(8) 0.2817(5) 0.060(3) Uani 1 1 d . . . H24A H 0.3800 -0.2298 0.2920 0.091 Uiso 1 1 calc R . . H24B H 0.2888 -0.2348 0.2733 0.091 Uiso 1 1 calc R . . H24C H 0.3181 -0.1521 0.3115 0.091 Uiso 1 1 calc R . . C25 C 0.4228(6) 0.2084(8) 0.0477(4) 0.043(3) Uani 1 1 d . . . C26 C 0.5261(6) 0.0861(6) 0.0819(5) 0.043(3) Uani 1 1 d . . . C27 C 0.3970(7) 0.0292(8) 0.0246(4) 0.046(3) Uani 1 1 d . . . C28 C 0.6292(6) 0.2949(7) 0.4219(4) 0.039(2) Uani 1 1 d . . . C29 C 0.7134(7) 0.2986(7) 0.4334(4) 0.045(3) Uani 1 1 d . . . H29 H 0.7392 0.3404 0.4604 0.054 Uiso 1 1 calc R . . C30 C 0.7537(7) 0.2345(7) 0.4002(5) 0.054(3) Uani 1 1 d . . . H30 H 0.8127 0.2239 0.3996 0.065 Uiso 1 1 calc R . . C31 C 0.6976(8) 0.1895(7) 0.3672(4) 0.049(3) Uani 1 1 d . . . H31 H 0.7092 0.1409 0.3395 0.058 Uiso 1 1 calc R . . C32 C 0.6214(7) 0.2253(7) 0.3808(4) 0.044(3) Uani 1 1 d . . . H32 H 0.5700 0.2063 0.3636 0.053 Uiso 1 1 calc R . . C33 C 0.6536(5) 0.4587(6) 0.3291(3) 0.029(2) Uani 1 1 d . . . C34 C 0.7392(6) 0.4600(7) 0.3359(4) 0.041(2) Uani 1 1 d . . . H34 H 0.7699 0.5015 0.3606 0.049 Uiso 1 1 calc R . . C35 C 0.7720(6) 0.3902(6) 0.3009(4) 0.041(3) Uani 1 1 d . . . H35 H 0.8299 0.3743 0.2976 0.049 Uiso 1 1 calc R . . C36 C 0.7073(6) 0.3437(7) 0.2731(4) 0.042(3) Uani 1 1 d . . . H36 H 0.7123 0.2919 0.2465 0.050 Uiso 1 1 calc R . . C37 C 0.6351(7) 0.3871(6) 0.2903(4) 0.035(2) Uani 1 1 d . . . H37 H 0.5802 0.3698 0.2781 0.042 Uiso 1 1 calc R . . C1A C 0.4856(5) 0.2736(5) 0.4883(3) 0.053(3) Uani 1 1 d GU . . C2A C 0.4488(5) 0.2952(5) 0.5375(3) 0.079(3) Uani 1 1 d GU . . H2A H 0.4583 0.3536 0.5540 0.095 Uiso 1 1 calc R . . C3A C 0.3980(5) 0.2304(6) 0.5622(3) 0.085(3) Uani 1 1 d GU . . H3A H 0.3732 0.2451 0.5955 0.102 Uiso 1 1 calc R . . C4A C 0.3840(5) 0.1441(5) 0.5378(4) 0.074(3) Uani 1 1 d GU . . H4A H 0.3496 0.1003 0.5545 0.088 Uiso 1 1 calc R . . C5A C 0.4208(5) 0.1225(5) 0.4886(4) 0.090(3) Uani 1 1 d GU . . H5A H 0.4113 0.0641 0.4720 0.108 Uiso 1 1 calc R . . C6A C 0.4716(5) 0.1872(6) 0.4639(3) 0.075(3) Uani 1 1 d GU . . H6A H 0.4964 0.1726 0.4306 0.090 Uiso 1 1 calc R . . C1B C 0.6056(6) 0.4034(9) 0.5172(4) 0.047(3) Uani 1 1 d . . . C2B C 0.6153(6) 0.4964(9) 0.5279(4) 0.050(3) Uani 1 1 d . . . H2B H 0.5904 0.5407 0.5051 0.061 Uiso 1 1 calc R . . C3B C 0.6610(7) 0.5275(10) 0.5712(5) 0.072(4) Uani 1 1 d . . . H3B H 0.6684 0.5921 0.5770 0.086 Uiso 1 1 calc R . . C4B C 0.6951(7) 0.4644(11) 0.6055(5) 0.074(4) Uani 1 1 d . . . H4B H 0.7259 0.4861 0.6350 0.088 Uiso 1 1 calc R . . C5B C 0.6857(7) 0.3700(10) 0.5979(5) 0.063(3) Uani 1 1 d . . . H5B H 0.7080 0.3267 0.6225 0.075 Uiso 1 1 calc R . . C6B C 0.6416(7) 0.3392(9) 0.5522(4) 0.058(3) Uani 1 1 d . . . H6B H 0.6364 0.2746 0.5454 0.069 Uiso 1 1 calc R . . C1C C 0.6326(5) 0.6263(6) 0.3905(4) 0.030(2) Uani 1 1 d U . . C2C C 0.6965(6) 0.6042(7) 0.4263(4) 0.044(2) Uani 1 1 d U . . H2C H 0.7082 0.5412 0.4345 0.052 Uiso 1 1 calc R . . C3C C 0.7424(7) 0.6763(9) 0.4495(4) 0.058(3) Uani 1 1 d DU . . H3C H 0.7839 0.6620 0.4742 0.069 Uiso 1 1 calc R . . C4C C 0.7270(7) 0.7652(8) 0.4366(5) 0.067(4) Uani 1 1 d DU . . H4C H 0.7608 0.8127 0.4501 0.080 Uiso 1 1 calc R . . C5C C 0.6637(7) 0.7891(8) 0.4045(5) 0.059(3) Uani 1 1 d DU . . H5C H 0.6519 0.8527 0.3981 0.071 Uiso 1 1 calc R . . C6C C 0.6168(7) 0.7201(7) 0.3812(4) 0.044(3) Uani 1 1 d U . . H6C H 0.5734 0.7371 0.3587 0.053 Uiso 1 1 calc R . . C1D C 0.5394(5) 0.5849(6) 0.2944(4) 0.028(2) Uani 1 1 d . . . C2D C 0.5906(6) 0.6402(6) 0.2638(4) 0.041(2) Uani 1 1 d . . . H2D H 0.6412 0.6573 0.2778 0.049 Uiso 1 1 calc R . . C3D C 0.5679(6) 0.6702(7) 0.2130(4) 0.043(3) Uani 1 1 d . . . H3D H 0.6027 0.7091 0.1930 0.052 Uiso 1 1 calc R . . C4D C 0.4967(8) 0.6447(7) 0.1915(5) 0.055(3) Uani 1 1 d . . . H4D H 0.4833 0.6633 0.1561 0.066 Uiso 1 1 calc R . . C5D C 0.4429(8) 0.5910(7) 0.2214(5) 0.052(3) Uani 1 1 d . . . H5D H 0.3923 0.5752 0.2069 0.062 Uiso 1 1 calc R . . C6D C 0.4648(6) 0.5607(6) 0.2735(4) 0.034(2) Uani 1 1 d . . . H6D H 0.4290 0.5242 0.2942 0.041 Uiso 1 1 calc R . . P3 P 0.17162(17) 0.5448(2) 0.24957(12) 0.0436(7) Uani 1 1 d . . . F6 F 0.2098(6) 0.5468(8) 0.3065(4) 0.137(4) Uani 1 1 d . . . F1 F 0.2259(6) 0.6237(6) 0.2258(5) 0.132(4) Uani 1 1 d . . . F2 F 0.1121(6) 0.6232(5) 0.2694(4) 0.107(3) Uani 1 1 d . . . F5 F 0.1320(5) 0.5426(8) 0.1922(4) 0.128(4) Uani 1 1 d . . . F3 F 0.1123(7) 0.4676(7) 0.2696(4) 0.152(5) Uani 1 1 d . . . F4 F 0.2331(6) 0.4723(7) 0.2300(4) 0.129(4) Uani 1 1 d . . . C1S C 0.9859(11) 0.5185(13) 0.3645(7) 0.128(7) Uani 1 1 d . . . H1S1 H 1.0418 0.5003 0.3697 0.191 Uiso 1 1 calc R . . H1S2 H 0.9792 0.5451 0.3286 0.191 Uiso 1 1 calc R . . H1S3 H 0.9516 0.4638 0.3683 0.191 Uiso 1 1 calc R . . C2S C 0.9634(10) 0.5892(14) 0.4059(9) 0.101(7) Uani 1 1 d . . . N1S N 0.9456(11) 0.6388(13) 0.4384(9) 0.139(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 Re1 0.03057(17) 0.03330(16) 0.02803(17) -0.0085(2) 0.0057(2) -0.00665(16) Ru1 0.0211(3) 0.0351(4) 0.0259(4) -0.0111(3) 0.0006(3) 0.0006(3) Fe1 0.0311(7) 0.0331(7) 0.0321(8) 0.0038(6) 0.0045(6) 0.0080(6) P1 0.0276(14) 0.0452(16) 0.0254(14) -0.0001(12) 0.0011(11) 0.0003(12) P2 0.0245(12) 0.0287(12) 0.0284(13) -0.0046(10) -0.0022(10) 0.0014(10) O1 0.076(6) 0.065(5) 0.045(5) 0.012(4) -0.004(4) -0.029(5) O2 0.081(7) 0.085(6) 0.062(6) -0.040(5) 0.000(5) -0.023(5) O3 0.039(4) 0.066(5) 0.067(7) -0.023(4) 0.008(4) -0.003(4) N1 0.018(4) 0.030(4) 0.038(5) -0.006(4) 0.005(3) -0.001(3) N2 0.038(4) 0.027(3) 0.010(4) -0.004(3) -0.002(3) -0.003(3) N3 0.035(5) 0.022(4) 0.036(5) -0.013(4) 0.002(4) 0.002(4) C1 0.036(6) 0.106(10) 0.038(7) -0.031(7) 0.003(5) 0.012(7) C2 0.034(6) 0.056(7) 0.081(10) -0.043(7) 0.022(6) -0.012(5) C3 0.051(7) 0.038(6) 0.058(8) -0.010(6) 0.017(6) 0.012(5) C4 0.034(5) 0.038(5) 0.054(7) -0.023(5) -0.006(5) 0.015(5) C5 0.034(6) 0.045(6) 0.059(7) -0.018(6) 0.011(5) 0.006(5) C6 0.022(5) 0.031(5) 0.032(5) -0.003(4) 0.002(4) 0.004(4) C7 0.033(5) 0.034(5) 0.025(5) -0.004(4) 0.005(4) 0.003(4) C8 0.022(5) 0.026(5) 0.030(5) 0.003(4) -0.002(4) -0.004(4) C9 0.020(5) 0.026(5) 0.038(6) -0.005(4) 0.006(4) -0.003(4) C10 0.029(5) 0.028(5) 0.025(5) -0.005(4) 0.008(4) -0.005(4) C11 0.041(6) 0.042(6) 0.031(6) -0.010(4) -0.008(4) 0.000(5) C12 0.033(5) 0.023(5) 0.033(5) -0.008(4) 0.005(4) 0.006(4) C13 0.052(6) 0.031(5) 0.028(7) 0.004(4) -0.001(5) -0.010(4) C14 0.040(5) 0.035(4) 0.039(5) -0.013(6) -0.011(6) 0.000(4) C15 0.033(5) 0.029(5) 0.018(4) -0.005(4) -0.005(4) -0.009(4) C16 0.032(5) 0.032(5) 0.031(5) -0.007(4) 0.004(4) -0.001(4) C17 0.036(5) 0.035(5) 0.019(5) -0.010(4) -0.005(4) -0.003(4) C18 0.029(5) 0.027(5) 0.033(5) -0.013(4) 0.000(4) -0.002(4) C19 0.044(6) 0.030(5) 0.031(6) 0.008(4) 0.003(5) 0.003(4) C20 0.047(7) 0.021(5) 0.077(9) 0.007(5) 0.002(6) -0.003(5) C21 0.035(6) 0.032(5) 0.069(8) 0.002(5) -0.011(5) 0.000(5) C22 0.029(5) 0.031(5) 0.071(8) 0.002(5) -0.002(5) -0.003(4) C23 0.031(6) 0.064(7) 0.058(8) 0.005(6) -0.001(5) 0.005(5) C24 0.073(9) 0.051(7) 0.058(8) 0.021(6) -0.013(7) 0.011(6) C25 0.034(6) 0.066(7) 0.029(6) -0.001(5) -0.002(5) -0.014(5) C26 0.052(6) 0.040(5) 0.036(7) -0.018(5) -0.002(6) -0.011(4) C27 0.052(7) 0.051(7) 0.035(7) -0.014(6) 0.014(5) -0.003(6) C28 0.037(6) 0.052(6) 0.029(6) 0.015(5) 0.006(4) 0.017(5) C29 0.057(7) 0.055(6) 0.024(5) 0.016(5) -0.009(5) 0.007(6) C30 0.054(7) 0.053(6) 0.055(8) 0.024(6) 0.022(6) 0.021(6) C31 0.073(9) 0.034(6) 0.038(7) -0.001(5) 0.016(6) 0.004(6) C32 0.057(7) 0.037(6) 0.038(6) 0.012(5) 0.010(5) 0.005(5) C33 0.033(5) 0.030(5) 0.023(5) -0.003(4) 0.007(4) 0.005(4) C34 0.031(6) 0.047(6) 0.044(6) -0.007(5) 0.005(5) 0.003(5) C35 0.040(6) 0.045(6) 0.038(6) 0.019(5) 0.016(5) 0.009(5) C36 0.044(6) 0.047(6) 0.035(6) 0.006(5) 0.019(5) 0.019(5) C37 0.050(7) 0.033(5) 0.021(5) 0.001(4) -0.002(5) 0.007(5) C1A 0.045(5) 0.060(5) 0.055(5) 0.011(4) 0.007(4) -0.008(4) C2A 0.075(6) 0.093(6) 0.068(5) 0.003(5) 0.011(5) -0.028(5) C3A 0.081(6) 0.102(6) 0.071(6) 0.012(5) 0.012(5) -0.020(5) C4A 0.069(5) 0.072(5) 0.080(6) 0.024(5) 0.018(5) 0.000(5) C5A 0.087(6) 0.074(5) 0.108(6) 0.009(5) 0.030(5) -0.005(5) C6A 0.069(5) 0.066(5) 0.090(6) -0.001(5) 0.033(5) -0.003(5) C1B 0.026(6) 0.093(9) 0.022(5) 0.002(6) 0.004(4) 0.006(6) C2B 0.028(6) 0.086(9) 0.037(7) -0.015(6) -0.001(5) -0.001(6) C3B 0.036(7) 0.103(10) 0.076(10) -0.036(8) -0.006(6) 0.004(7) C4B 0.039(7) 0.134(12) 0.049(9) -0.029(8) -0.003(6) -0.011(8) C5B 0.042(6) 0.121(10) 0.025(8) 0.015(7) -0.005(5) 0.005(7) C6B 0.042(7) 0.104(10) 0.028(6) 0.007(6) -0.001(5) -0.009(7) C1C 0.021(4) 0.041(5) 0.026(4) -0.009(4) 0.004(4) -0.005(4) C2C 0.039(5) 0.059(5) 0.033(5) -0.008(5) 0.004(4) -0.002(5) C3C 0.036(6) 0.091(7) 0.046(6) -0.019(6) -0.003(5) -0.013(5) C4C 0.065(7) 0.076(7) 0.060(7) -0.014(6) 0.011(6) -0.041(6) C5C 0.078(7) 0.049(5) 0.051(6) 0.005(5) 0.010(6) -0.019(5) C6C 0.053(6) 0.041(5) 0.038(5) -0.006(4) 0.002(5) -0.014(5) C1D 0.029(5) 0.022(5) 0.033(5) -0.002(4) -0.001(4) 0.014(4) C2D 0.051(7) 0.037(5) 0.034(6) 0.002(4) 0.015(5) 0.018(5) C3D 0.045(7) 0.043(6) 0.041(6) 0.002(5) 0.002(5) 0.007(5) C4D 0.091(10) 0.035(6) 0.039(7) 0.007(5) -0.016(7) 0.014(6) C5D 0.060(8) 0.043(7) 0.052(8) -0.009(6) -0.023(6) 0.011(6) C6D 0.043(6) 0.028(5) 0.030(5) -0.008(4) -0.009(5) 0.001(4) P3 0.0351(16) 0.0525(17) 0.0432(17) -0.0010(14) -0.0001(13) 0.0027(14) F6 0.145(9) 0.200(10) 0.067(6) -0.033(6) -0.035(6) 0.070(8) F1 0.121(9) 0.105(7) 0.170(10) 0.009(6) 0.051(7) -0.037(6) F2 0.129(8) 0.090(5) 0.104(7) 0.000(5) 0.016(6) 0.044(5) F5 0.088(7) 0.212(10) 0.083(7) -0.029(7) -0.029(5) 0.024(7) F3 0.186(11) 0.138(8) 0.133(9) -0.026(7) 0.068(8) -0.091(8) F4 0.151(10) 0.132(7) 0.104(7) 0.008(6) 0.038(6) 0.093(7) C1S 0.123(16) 0.162(17) 0.098(15) 0.037(13) 0.052(12) 0.044(14) C2S 0.055(10) 0.129(16) 0.119(17) 0.068(14) 0.026(11) 0.025(11) N1S 0.093(13) 0.146(16) 0.18(2) 0.012(13) 0.033(12) 0.019(11) _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 Re1 C27 1.882(11) . ? Re1 C25 1.886(11) . ? Re1 C26 1.910(11) . ? Re1 N3 2.160(8) . ? Re1 N2 2.165(7) . ? Re1 N1 2.206(7) . ? Ru1 C6 1.974(9) . ? Ru1 C5 2.215(10) . ? Ru1 C1 2.220(10) . ? Ru1 C2 2.240(10) . ? Ru1 C4 2.243(9) . ? Ru1 C3 2.256(10) . ? Ru1 P1 2.282(3) . ? Ru1 P2 2.282(2) . ? Fe1 C37 2.017(9) . ? Fe1 C29 2.021(9) . ? Fe1 C32 2.025(10) . ? Fe1 C36 2.030(10) . ? Fe1 C28 2.032(9) . ? Fe1 C33 2.033(8) . ? Fe1 C30 2.040(10) . ? Fe1 C31 2.042(10) . ? Fe1 C35 2.043(9) . ? Fe1 C34 2.044(10) . ? P1 C1B 1.834(11) . ? P1 C28 1.839(10) . ? P1 C1A 1.839(6) . ? P2 C1C 1.822(9) . ? P2 C33 1.838(9) . ? P2 C1D 1.867(9) . ? O1 C25 1.168(12) . ? O2 C27 1.163(12) . ? O3 C26 1.165(11) . ? N1 C8 1.337(10) . ? N1 C12 1.361(11) . ? N2 C13 1.326(11) . ? N2 C17 1.375(10) . ? N3 C22 1.339(12) . ? N3 C18 1.378(11) . ? C1 C2 1.378(16) . ? C1 C5 1.428(14) . ? C2 C3 1.432(16) . ? C3 C4 1.357(13) . ? C4 C5 1.415(14) . ? C6 C7 1.238(12) . ? C7 C10 1.412(12) . ? C8 C9 1.378(11) . ? C9 C10 1.407(12) . ? C10 C11 1.402(12) . ? C11 C12 1.374(12) . ? C13 C14 1.372(12) . ? C14 C15 1.381(13) . ? C15 C16 1.384(12) . ? C15 C23 1.518(13) . ? C16 C17 1.381(12) . ? C17 C18 1.488(12) . ? C18 C19 1.366(12) . ? C19 C20 1.389(13) . ? C20 C21 1.336(14) . ? C20 C24 1.496(14) . ? C21 C22 1.377(15) . ? C28 C32 1.422(14) . ? C28 C29 1.426(14) . ? C29 C30 1.397(13) . ? C30 C31 1.393(15) . ? C31 C32 1.405(15) . ? C33 C37 1.429(12) . ? C33 C34 1.429(12) . ? C34 C35 1.424(13) . ? C35 C36 1.436(14) . ? C36 C37 1.414(13) . ? C1A C2A 1.3900 . ? C1A C6A 1.3900 . ? C2A C3A 1.3900 . ? C3A C4A 1.3900 . ? C4A C5A 1.3900 . ? C5A C6A 1.3900 . ? C1B C2B 1.362(15) . ? C1B C6B 1.392(14) . ? C2B C3B 1.382(15) . ? C3B C4B 1.356(16) . ? C4B C5B 1.368(16) . ? C5B C6B 1.412(15) . ? C1C C6C 1.382(13) . ? C1C C2C 1.415(13) . ? C2C C3C 1.401(13) . ? C3C C4C 1.331(12) . ? C4C C5C 1.357(13) . ? C5C C6C 1.380(14) . ? C1D C2D 1.382(13) . ? C1D C6D 1.384(12) . ? C2D C3D 1.374(13) . ? C3D C4D 1.345(15) . ? C4D C5D 1.386(16) . ? C5D C6D 1.400(14) . ? P3 F4 1.530(8) . ? P3 F6 1.538(9) . ? P3 F1 1.555(9) . ? P3 F3 1.557(9) . ? P3 F5 1.558(9) . ? P3 F2 1.568(8) . ? C1S C2S 1.48(2) . ? C2S N1S 1.11(2) . ? 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 C27 Re1 C25 89.5(4) . . ? C27 Re1 C26 90.4(5) . . ? C25 Re1 C26 85.8(4) . . ? C27 Re1 N3 96.8(4) . . ? C25 Re1 N3 171.4(4) . . ? C26 Re1 N3 99.9(4) . . ? C27 Re1 N2 91.2(4) . . ? C25 Re1 N2 98.4(4) . . ? C26 Re1 N2 175.5(4) . . ? N3 Re1 N2 75.7(3) . . ? C27 Re1 N1 175.6(4) . . ? C25 Re1 N1 92.2(4) . . ? C26 Re1 N1 93.9(4) . . ? N3 Re1 N1 81.2(3) . . ? N2 Re1 N1 84.4(2) . . ? C6 Ru1 C5 103.9(4) . . ? C6 Ru1 C1 141.0(4) . . ? C5 Ru1 C1 37.6(4) . . ? C6 Ru1 C2 149.7(4) . . ? C5 Ru1 C2 61.7(4) . . ? C1 Ru1 C2 36.0(4) . . ? C6 Ru1 C4 91.1(4) . . ? C5 Ru1 C4 37.0(4) . . ? C1 Ru1 C4 61.3(4) . . ? C2 Ru1 C4 61.0(4) . . ? C6 Ru1 C3 112.8(4) . . ? C5 Ru1 C3 60.5(4) . . ? C1 Ru1 C3 60.5(5) . . ? C2 Ru1 C3 37.1(4) . . ? C4 Ru1 C3 35.1(3) . . ? C6 Ru1 P1 88.6(3) . . ? C5 Ru1 P1 103.7(3) . . ? C1 Ru1 P1 95.2(3) . . ? C2 Ru1 P1 119.8(4) . . ? C4 Ru1 P1 138.9(3) . . ? C3 Ru1 P1 155.3(3) . . ? C6 Ru1 P2 88.8(3) . . ? C5 Ru1 P2 155.8(3) . . ? C1 Ru1 P2 128.9(4) . . ? C2 Ru1 P2 97.1(3) . . ? C4 Ru1 P2 124.0(3) . . ? C3 Ru1 P2 95.6(3) . . ? P1 Ru1 P2 97.05(9) . . ? C37 Fe1 C29 157.3(4) . . ? C37 Fe1 C32 105.3(4) . . ? C29 Fe1 C32 67.8(4) . . ? C37 Fe1 C36 40.9(4) . . ? C29 Fe1 C36 161.8(4) . . ? C32 Fe1 C36 116.7(4) . . ? C37 Fe1 C28 119.4(4) . . ? C29 Fe1 C28 41.2(4) . . ? C32 Fe1 C28 41.0(4) . . ? C36 Fe1 C28 152.8(4) . . ? C37 Fe1 C33 41.3(3) . . ? C29 Fe1 C33 123.7(4) . . ? C32 Fe1 C33 125.1(4) . . ? C36 Fe1 C33 69.6(4) . . ? C28 Fe1 C33 108.1(4) . . ? C37 Fe1 C30 159.0(4) . . ? C29 Fe1 C30 40.2(4) . . ? C32 Fe1 C30 67.2(5) . . ? C36 Fe1 C30 123.1(4) . . ? C28 Fe1 C30 68.8(4) . . ? C33 Fe1 C30 158.8(4) . . ? C37 Fe1 C31 121.9(4) . . ? C29 Fe1 C31 67.9(4) . . ? C32 Fe1 C31 40.4(4) . . ? C36 Fe1 C31 103.5(4) . . ? C28 Fe1 C31 69.3(4) . . ? C33 Fe1 C31 160.5(4) . . ? C30 Fe1 C31 39.9(4) . . ? C37 Fe1 C35 68.5(4) . . ? C29 Fe1 C35 127.5(4) . . ? C32 Fe1 C35 152.8(4) . . ? C36 Fe1 C35 41.3(4) . . ? C28 Fe1 C35 165.1(4) . . ? C33 Fe1 C35 68.7(4) . . ? C30 Fe1 C35 108.5(4) . . ? C31 Fe1 C35 118.8(4) . . ? C37 Fe1 C34 69.2(4) . . ? C29 Fe1 C34 111.1(4) . . ? C32 Fe1 C34 163.9(4) . . ? C36 Fe1 C34 69.7(4) . . ? C28 Fe1 C34 127.4(4) . . ? C33 Fe1 C34 41.0(4) . . ? C30 Fe1 C34 123.1(5) . . ? C31 Fe1 C34 155.3(4) . . ? C35 Fe1 C34 40.8(4) . . ? C1B P1 C28 101.1(5) . . ? C1B P1 C1A 99.7(5) . . ? C28 P1 C1A 104.3(4) . . ? C1B P1 Ru1 117.7(4) . . ? C28 P1 Ru1 121.3(3) . . ? C1A P1 Ru1 109.9(3) . . ? C1C P2 C33 102.2(4) . . ? C1C P2 C1D 102.9(4) . . ? C33 P2 C1D 95.8(4) . . ? C1C P2 Ru1 116.2(3) . . ? C33 P2 Ru1 122.2(3) . . ? C1D P2 Ru1 114.2(3) . . ? C8 N1 C12 115.6(8) . . ? C8 N1 Re1 124.5(6) . . ? C12 N1 Re1 119.9(6) . . ? C13 N2 C17 116.8(8) . . ? C13 N2 Re1 126.2(6) . . ? C17 N2 Re1 116.9(6) . . ? C22 N3 C18 116.2(8) . . ? C22 N3 Re1 126.4(7) . . ? C18 N3 Re1 116.4(6) . . ? C2 C1 C5 109.0(11) . . ? C2 C1 Ru1 72.8(6) . . ? C5 C1 Ru1 71.1(6) . . ? C1 C2 C3 106.7(10) . . ? C1 C2 Ru1 71.2(6) . . ? C3 C2 Ru1 72.0(6) . . ? C4 C3 C2 109.3(11) . . ? C4 C3 Ru1 71.9(5) . . ? C2 C3 Ru1 70.8(6) . . ? C3 C4 C5 108.7(10) . . ? C3 C4 Ru1 73.0(6) . . ? C5 C4 Ru1 70.4(5) . . ? C4 C5 C1 106.3(10) . . ? C4 C5 Ru1 72.6(6) . . ? C1 C5 Ru1 71.4(6) . . ? C7 C6 Ru1 174.9(8) . . ? C6 C7 C10 168.9(10) . . ? N1 C8 C9 125.3(8) . . ? C8 C9 C10 118.8(8) . . ? C11 C10 C9 116.6(8) . . ? C11 C10 C7 121.9(9) . . ? C9 C10 C7 121.5(8) . . ? C12 C11 C10 120.2(9) . . ? N1 C12 C11 123.5(8) . . ? N2 C13 C14 124.6(9) . . ? C13 C14 C15 119.8(9) . . ? C14 C15 C16 116.2(9) . . ? C14 C15 C23 122.1(8) . . ? C16 C15 C23 121.7(8) . . ? C17 C16 C15 122.0(9) . . ? N2 C17 C16 120.5(8) . . ? N2 C17 C18 114.8(8) . . ? C16 C17 C18 124.7(9) . . ? C19 C18 N3 121.3(9) . . ? C19 C18 C17 123.5(9) . . ? N3 C18 C17 115.2(8) . . ? C18 C19 C20 121.8(10) . . ? C21 C20 C19 115.6(10) . . ? C21 C20 C24 123.9(10) . . ? C19 C20 C24 120.3(10) . . ? C20 C21 C22 122.5(10) . . ? N3 C22 C21 122.4(10) . . ? O1 C25 Re1 178.2(9) . . ? O3 C26 Re1 177.2(8) . . ? O2 C27 Re1 179.0(11) . . ? C32 C28 C29 104.9(9) . . ? C32 C28 P1 129.5(8) . . ? C29 C28 P1 125.5(8) . . ? C32 C28 Fe1 69.2(5) . . ? C29 C28 Fe1 69.0(5) . . ? P1 C28 Fe1 128.2(5) . . ? C30 C29 C28 109.2(10) . . ? C30 C29 Fe1 70.6(6) . . ? C28 C29 Fe1 69.8(5) . . ? C31 C30 C29 108.8(10) . . ? C31 C30 Fe1 70.1(6) . . ? C29 C30 Fe1 69.2(5) . . ? C30 C31 C32 107.1(9) . . ? C30 C31 Fe1 70.0(6) . . ? C32 C31 Fe1 69.1(6) . . ? C31 C32 C28 110.0(10) . . ? C31 C32 Fe1 70.5(6) . . ? C28 C32 Fe1 69.8(6) . . ? C37 C33 C34 107.6(8) . . ? C37 C33 P2 121.6(7) . . ? C34 C33 P2 130.8(7) . . ? C37 C33 Fe1 68.7(5) . . ? C34 C33 Fe1 69.9(5) . . ? P2 C33 Fe1 127.7(5) . . ? C35 C34 C33 107.4(9) . . ? C35 C34 Fe1 69.6(5) . . ? C33 C34 Fe1 69.1(5) . . ? C34 C35 C36 109.0(9) . . ? C34 C35 Fe1 69.6(5) . . ? C36 C35 Fe1 68.9(5) . . ? C37 C36 C35 106.7(9) . . ? C37 C36 Fe1 69.1(5) . . ? C35 C36 Fe1 69.9(6) . . ? C36 C37 C33 109.3(9) . . ? C36 C37 Fe1 70.0(6) . . ? C33 C37 Fe1 69.9(5) . . ? C2A C1A C6A 120.0 . . ? C2A C1A P1 118.0(5) . . ? C6A C1A P1 121.9(5) . . ? C1A C2A C3A 120.0 . . ? C4A C3A C2A 120.0 . . ? C3A C4A C5A 120.0 . . ? C6A C5A C4A 120.0 . . ? C5A C6A C1A 120.0 . . ? C2B C1B C6B 118.0(10) . . ? C2B C1B P1 121.5(9) . . ? C6B C1B P1 120.5(10) . . ? C1B C2B C3B 121.8(12) . . ? C4B C3B C2B 119.8(13) . . ? C3B C4B C5B 121.3(12) . . ? C4B C5B C6B 118.3(11) . . ? C1B C6B C5B 120.8(12) . . ? C6C C1C C2C 117.4(9) . . ? C6C C1C P2 123.1(7) . . ? C2C C1C P2 119.5(7) . . ? C3C C2C C1C 119.9(10) . . ? C4C C3C C2C 119.7(11) . . ? C3C C4C C5C 121.9(11) . . ? C4C C5C C6C 119.9(11) . . ? C5C C6C C1C 121.0(11) . . ? C2D C1D C6D 119.3(9) . . ? C2D C1D P2 120.5(7) . . ? C6D C1D P2 119.8(7) . . ? C3D C2D C1D 120.3(10) . . ? C4D C3D C2D 120.9(11) . . ? C3D C4D C5D 120.4(11) . . ? C4D C5D C6D 119.3(11) . . ? C1D C6D C5D 119.7(10) . . ? F4 P3 F6 91.4(5) . . ? F4 P3 F1 89.1(6) . . ? F6 P3 F1 95.3(6) . . ? F4 P3 F3 92.5(6) . . ? F6 P3 F3 89.1(6) . . ? F1 P3 F3 175.3(7) . . ? F4 P3 F5 89.0(5) . . ? F6 P3 F5 179.3(6) . . ? F1 P3 F5 85.3(6) . . ? F3 P3 F5 90.3(6) . . ? F4 P3 F2 177.0(6) . . ? F6 P3 F2 87.9(5) . . ? F1 P3 F2 88.1(5) . . ? F3 P3 F2 90.4(6) . . ? F5 P3 F2 91.7(5) . . ? N1S C2S C1S 177(2) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.174 _refine_diff_density_min -1.108 _refine_diff_density_rms 0.136 #===end data_7253 _database_code_depnum_ccdc_archive 'CCDC 721190' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C62 H51 Cl6 F6 Fe N3 O3 P3 Re Ru' _chemical_formula_weight 1648.79 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' P P 0.1023 0.0942 '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' Re Re -1.0185 7.2310 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.3707(6) _cell_length_b 16.6896(8) _cell_length_c 17.4696(9) _cell_angle_alpha 74.4360(10) _cell_angle_beta 83.0730(10) _cell_angle_gamma 82.1490(10) _cell_volume 3151.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.738 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1628 _exptl_absorpt_coefficient_mu 2.776 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5104 _exptl_absorpt_correction_T_max 0.7688 _exptl_absorpt_process_details 'Sadabs, (Sheldrick 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41593 _diffrn_reflns_av_R_equivalents 0.0609 _diffrn_reflns_av_sigmaI/netI 0.0719 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 27.47 _reflns_number_total 14407 _reflns_number_gt 11547 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0594P)^2^+5.0419P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14407 _refine_ls_number_parameters 782 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0761 _refine_ls_R_factor_gt 0.0588 _refine_ls_wR_factor_ref 0.1382 _refine_ls_wR_factor_gt 0.1308 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.54311(4) 0.09047(3) 0.28250(3) 0.02420(12) Uani 1 1 d . . . Re1 Re 0.52248(2) 0.312354(15) 0.736296(14) 0.02837(8) Uani 1 1 d . . . Fe1 Fe 0.39390(8) 0.35006(5) 0.19536(5) 0.02704(19) Uani 1 1 d . . . P1 P 0.63773(13) 0.19711(10) 0.20059(9) 0.0243(3) Uani 1 1 d . . . P2 P 0.35513(13) 0.13969(9) 0.24825(9) 0.0247(3) Uani 1 1 d . . . O1 O 0.7510(5) 0.1928(4) 0.7689(3) 0.0614(16) Uani 1 1 d . . . O2 O 0.5373(6) 0.3616(3) 0.8915(3) 0.0618(17) Uani 1 1 d . . . O3 O 0.3877(6) 0.1694(3) 0.8426(3) 0.0599(15) Uani 1 1 d . . . N1 N 0.5159(4) 0.2751(3) 0.6260(3) 0.0273(11) Uani 1 1 d . . . N2 N 0.5993(5) 0.4198(3) 0.6569(3) 0.0308(12) Uani 1 1 d . . . N3 N 0.3718(5) 0.4034(3) 0.6967(3) 0.0324(12) Uani 1 1 d . . . C1 C 0.7021(7) -0.0062(4) 0.2981(5) 0.049(2) Uani 1 1 d . . . H1 H 0.7865 0.0052 0.2905 0.059 Uiso 1 1 calc R . . C2 C 0.6363(7) -0.0191(4) 0.2394(5) 0.0476(19) Uani 1 1 d . . . H2 H 0.6666 -0.0182 0.1836 0.057 Uiso 1 1 calc R . . C3 C 0.5226(6) -0.0381(4) 0.2756(5) 0.0391(16) Uani 1 1 d . . . H3 H 0.4594 -0.0535 0.2495 0.047 Uiso 1 1 calc R . . C4 C 0.5174(7) -0.0386(4) 0.3573(5) 0.0455(18) Uani 1 1 d . . . H4 H 0.4507 -0.0546 0.3982 0.055 Uiso 1 1 calc R . . C5 C 0.6293(7) -0.0185(4) 0.3706(5) 0.052(2) Uani 1 1 d . . . H5 H 0.6539 -0.0173 0.4228 0.063 Uiso 1 1 calc R . . C6 C 0.5198(5) 0.1543(4) 0.3641(3) 0.0242(12) Uani 1 1 d . . . C7 C 0.5129(6) 0.1838(4) 0.4220(4) 0.0321(14) Uani 1 1 d . . . C8 C 0.4141(6) 0.2572(4) 0.6042(4) 0.0292(13) Uani 1 1 d . . . H8 H 0.3428 0.2643 0.6362 0.035 Uiso 1 1 calc R . . C9 C 0.4102(6) 0.2291(4) 0.5376(4) 0.0298(13) Uani 1 1 d . . . H9 H 0.3368 0.2185 0.5249 0.036 Uiso 1 1 calc R . . C10 C 0.5139(6) 0.2160(4) 0.4881(4) 0.0299(13) Uani 1 1 d . . . C11 C 0.6185(6) 0.2347(4) 0.5108(4) 0.0322(14) Uani 1 1 d . . . H11 H 0.6909 0.2282 0.4798 0.039 Uiso 1 1 calc R . . C12 C 0.6162(5) 0.2627(4) 0.5782(4) 0.0289(13) Uani 1 1 d . . . H12 H 0.6885 0.2738 0.5920 0.035 Uiso 1 1 calc R . . C13 C 0.2562(7) 0.3914(5) 0.7194(5) 0.0475(18) Uani 1 1 d . . . H13 H 0.2385 0.3408 0.7556 0.057 Uiso 1 1 calc R . . C14 C 0.1649(7) 0.4491(6) 0.6922(5) 0.063(2) Uani 1 1 d . . . H14 H 0.0858 0.4377 0.7086 0.076 Uiso 1 1 calc R . . C15 C 0.1884(8) 0.5245(6) 0.6406(6) 0.065(3) Uani 1 1 d . . . H15 H 0.1261 0.5657 0.6219 0.079 Uiso 1 1 calc R . . C16 C 0.3052(7) 0.5379(5) 0.6171(5) 0.0502(19) Uani 1 1 d . . . H16 H 0.3236 0.5890 0.5822 0.060 Uiso 1 1 calc R . . C17 C 0.3953(6) 0.4768(4) 0.6445(4) 0.0351(15) Uani 1 1 d . . . C18 C 0.5244(6) 0.4851(4) 0.6219(4) 0.0342(14) Uani 1 1 d . . . C19 C 0.5668(7) 0.5551(4) 0.5692(4) 0.0455(18) Uani 1 1 d . . . H19 H 0.5130 0.6003 0.5453 0.055 Uiso 1 1 calc R . . C20 C 0.6882(7) 0.5588(5) 0.5514(5) 0.0504(19) Uani 1 1 d . . . H20 H 0.7178 0.6063 0.5162 0.060 Uiso 1 1 calc R . . C21 C 0.7643(7) 0.4915(5) 0.5865(4) 0.0438(17) Uani 1 1 d . . . H21 H 0.8472 0.4919 0.5752 0.053 Uiso 1 1 calc R . . C22 C 0.7183(6) 0.4240(4) 0.6379(4) 0.0366(15) Uani 1 1 d . . . H22 H 0.7713 0.3782 0.6615 0.044 Uiso 1 1 calc R . . C23 C 0.6655(7) 0.2382(4) 0.7571(4) 0.0395(16) Uani 1 1 d . . . C24 C 0.4377(6) 0.2223(4) 0.8015(4) 0.0382(16) Uani 1 1 d . . . C25 C 0.5321(7) 0.3452(4) 0.8319(4) 0.0400(16) Uani 1 1 d . . . C26 C 0.2975(5) 0.2500(4) 0.2359(3) 0.0252(12) Uani 1 1 d . . . C27 C 0.2529(5) 0.3052(4) 0.1654(4) 0.0334(14) Uani 1 1 d . . . H27 H 0.2479 0.2907 0.1146 0.040 Uiso 1 1 calc R . . C28 C 0.2167(6) 0.3846(4) 0.1809(5) 0.0400(16) Uani 1 1 d . . . H28 H 0.1826 0.4352 0.1427 0.048 Uiso 1 1 calc R . . C29 C 0.2392(6) 0.3792(4) 0.2600(4) 0.0410(16) Uani 1 1 d . . . H29 H 0.2238 0.4256 0.2864 0.049 Uiso 1 1 calc R . . C30 C 0.2911(5) 0.2974(4) 0.2941(4) 0.0316(14) Uani 1 1 d . . . H30 H 0.3165 0.2761 0.3488 0.038 Uiso 1 1 calc R . . C31 C 0.5677(5) 0.3054(4) 0.1772(4) 0.0276(13) Uani 1 1 d . . . C32 C 0.5529(5) 0.3527(4) 0.2346(4) 0.0294(13) Uani 1 1 d . . . H32 H 0.5732 0.3317 0.2906 0.035 Uiso 1 1 calc R . . C33 C 0.5036(6) 0.4354(4) 0.1986(4) 0.0367(15) Uani 1 1 d . . . H33 H 0.4836 0.4819 0.2248 0.044 Uiso 1 1 calc R . . C34 C 0.4884(6) 0.4392(4) 0.1187(4) 0.0354(15) Uani 1 1 d . . . H34 H 0.4542 0.4888 0.0795 0.042 Uiso 1 1 calc R . . C35 C 0.5271(6) 0.3598(4) 0.1045(4) 0.0304(13) Uani 1 1 d . . . H35 H 0.5255 0.3444 0.0537 0.037 Uiso 1 1 calc R . . C1A C 0.7744(5) 0.2188(4) 0.2347(4) 0.0297(13) Uani 1 1 d . . . C2A C 0.8109(6) 0.1774(5) 0.3100(4) 0.0384(16) Uani 1 1 d . . . H2A H 0.7696 0.1339 0.3431 0.046 Uiso 1 1 calc R . . C3A C 0.9088(7) 0.2011(6) 0.3355(5) 0.055(2) Uani 1 1 d . . . H3A H 0.9322 0.1746 0.3868 0.066 Uiso 1 1 calc R . . C4A C 0.9710(6) 0.2622(5) 0.2870(5) 0.0496(19) Uani 1 1 d . . . H4A H 1.0382 0.2767 0.3045 0.060 Uiso 1 1 calc R . . C5A C 0.9362(6) 0.3027(5) 0.2128(5) 0.0466(18) Uani 1 1 d . . . H5A H 0.9792 0.3453 0.1797 0.056 Uiso 1 1 calc R . . C6A C 0.8384(6) 0.2813(5) 0.1867(4) 0.0405(16) Uani 1 1 d . . . H6A H 0.8148 0.3094 0.1357 0.049 Uiso 1 1 calc R . . C1B C 0.6914(5) 0.1760(4) 0.1038(3) 0.0284(13) Uani 1 1 d . . . C2B C 0.8050(6) 0.1372(4) 0.0913(4) 0.0321(14) Uani 1 1 d . . . H2B H 0.8597 0.1293 0.1297 0.038 Uiso 1 1 calc R . . C3B C 0.8392(6) 0.1097(4) 0.0231(4) 0.0405(16) Uani 1 1 d . . . H3B H 0.9160 0.0822 0.0162 0.049 Uiso 1 1 calc R . . C4B C 0.7623(7) 0.1223(4) -0.0341(4) 0.0409(17) Uani 1 1 d . . . H4B H 0.7862 0.1044 -0.0808 0.049 Uiso 1 1 calc R . . C5B C 0.6500(7) 0.1612(4) -0.0229(4) 0.0389(16) Uani 1 1 d . . . H5B H 0.5966 0.1695 -0.0621 0.047 Uiso 1 1 calc R . . C6B C 0.6139(6) 0.1883(4) 0.0450(4) 0.0291(13) Uani 1 1 d . . . H6B H 0.5366 0.2152 0.0516 0.035 Uiso 1 1 calc R . . C1C C 0.3054(5) 0.1204(4) 0.1588(4) 0.0281(13) Uani 1 1 d . . . C2C C 0.3853(6) 0.0849(4) 0.1073(4) 0.0350(15) Uani 1 1 d . . . H2C H 0.4655 0.0702 0.1184 0.042 Uiso 1 1 calc R . . C3C C 0.3483(7) 0.0710(5) 0.0400(4) 0.0470(18) Uani 1 1 d . . . H3C H 0.4028 0.0461 0.0060 0.056 Uiso 1 1 calc R . . C4C C 0.2321(8) 0.0937(5) 0.0228(5) 0.051(2) Uani 1 1 d . . . H4C H 0.2072 0.0854 -0.0237 0.061 Uiso 1 1 calc R . . C5C C 0.1507(7) 0.1291(5) 0.0742(5) 0.0476(19) Uani 1 1 d . . . H5C H 0.0711 0.1446 0.0623 0.057 Uiso 1 1 calc R . . C6C C 0.1866(6) 0.1413(4) 0.1423(4) 0.0372(15) Uani 1 1 d . . . H6C H 0.1311 0.1637 0.1776 0.045 Uiso 1 1 calc R . . C1D C 0.2519(5) 0.0819(4) 0.3261(4) 0.0317(14) Uani 1 1 d . . . C2D C 0.2170(6) 0.0084(5) 0.3172(5) 0.0476(19) Uani 1 1 d . . . H2D H 0.2330 -0.0047 0.2676 0.057 Uiso 1 1 calc R . . C3D C 0.1589(8) -0.0458(5) 0.3803(6) 0.062(2) Uani 1 1 d . . . H3D H 0.1363 -0.0954 0.3735 0.075 Uiso 1 1 calc R . . C4D C 0.1345(7) -0.0267(6) 0.4527(6) 0.062(3) Uani 1 1 d . . . H4D H 0.0961 -0.0637 0.4958 0.075 Uiso 1 1 calc R . . C5D C 0.1664(7) 0.0474(6) 0.4624(4) 0.055(2) Uani 1 1 d . . . H5D H 0.1481 0.0609 0.5116 0.067 Uiso 1 1 calc R . . C6D C 0.2261(6) 0.1018(5) 0.3985(4) 0.0400(16) Uani 1 1 d . . . H6D H 0.2485 0.1516 0.4051 0.048 Uiso 1 1 calc R . . C1S C 0.9532(8) 0.8534(6) 0.2369(5) 0.070(3) Uani 1 1 d . . . H1S1 H 1.0180 0.8174 0.2655 0.083 Uiso 1 1 calc R . . H1S2 H 0.8864 0.8609 0.2763 0.083 Uiso 1 1 calc R . . C2S C 0.8470(16) 0.3372(10) 0.9121(8) 0.132(6) Uani 1 1 d . . . H2S1 H 0.9226 0.3017 0.9216 0.159 Uiso 0.588(7) 1 calc PR A 1 H2S2 H 0.7833 0.3003 0.9260 0.159 Uiso 0.588(7) 1 calc PR A 1 C3S C 0.253(2) 0.4191(10) 0.9470(11) 0.186(8) Uani 1 1 d DU . . H3S1 H 0.2145 0.4260 0.9985 0.223 Uiso 0.588(7) 1 calc PR A 1 H3S2 H 0.3365 0.4286 0.9445 0.223 Uiso 0.588(7) 1 calc PR A 1 Cl1A Cl 0.9091(4) 0.8053(3) 0.1723(3) 0.1477(17) Uani 1 1 d . . . Cl1B Cl 1.0020(3) 0.95114(16) 0.18866(19) 0.0942(10) Uani 1 1 d . . . Cl2A Cl 0.8487(5) 0.3844(3) 0.8164(3) 0.1579(18) Uani 1 1 d . A . Cl3A Cl 0.2478(6) 0.3197(3) 0.9442(3) 0.193(3) Uani 1 1 d U A . Cl2B Cl 0.8273(12) 0.3991(4) 0.9729(4) 0.191(5) Uani 0.588(7) 1 d P A 1 Cl3B Cl 0.1911(14) 0.4891(6) 0.8781(6) 0.245(7) Uani 0.588(7) 1 d PD A 1 Cl2C Cl 0.9516(19) 0.3508(14) 0.9529(12) 0.250 Uiso 0.412(7) 1 d P A 2 Cl3C Cl 0.1495(18) 0.4901(13) 0.9624(13) 0.250 Uiso 0.412(7) 1 d P A 2 P3 P 0.98031(18) 0.70312(14) 0.45798(13) 0.0487(5) Uani 1 1 d . . . F1 F 0.8979(7) 0.6994(5) 0.5374(4) 0.108(2) Uani 1 1 d . . . F2 F 0.9858(7) 0.6054(4) 0.4774(5) 0.121(3) Uani 1 1 d . . . F3 F 1.0615(5) 0.7064(5) 0.3783(3) 0.112(3) Uani 1 1 d . . . F4 F 0.9727(8) 0.7987(4) 0.4377(6) 0.150(4) Uani 1 1 d . . . F5 F 0.8661(5) 0.7102(5) 0.4134(4) 0.110(2) Uani 1 1 d . . . F6 F 1.0962(7) 0.6898(6) 0.5005(5) 0.152(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 Ru1 0.0252(2) 0.0228(2) 0.0245(2) -0.00599(19) -0.00280(19) -0.00179(19) Re1 0.03948(16) 0.02387(13) 0.02148(13) -0.00553(9) -0.00599(10) -0.00010(10) Fe1 0.0294(5) 0.0236(4) 0.0287(5) -0.0077(4) -0.0032(4) -0.0024(4) P1 0.0236(8) 0.0275(8) 0.0224(7) -0.0069(6) -0.0028(6) -0.0031(6) P2 0.0248(8) 0.0235(8) 0.0259(8) -0.0058(6) -0.0016(6) -0.0045(6) O1 0.058(4) 0.062(4) 0.049(3) 0.001(3) -0.010(3) 0.020(3) O2 0.116(5) 0.035(3) 0.037(3) -0.015(2) -0.021(3) 0.005(3) O3 0.086(4) 0.047(3) 0.048(3) -0.008(3) 0.002(3) -0.026(3) N1 0.033(3) 0.023(3) 0.025(3) -0.005(2) -0.003(2) -0.001(2) N2 0.041(3) 0.022(3) 0.029(3) -0.007(2) -0.008(2) 0.001(2) N3 0.041(3) 0.032(3) 0.023(3) -0.008(2) -0.002(2) 0.002(2) C1 0.033(4) 0.032(4) 0.081(6) -0.017(4) -0.015(4) 0.013(3) C2 0.052(5) 0.033(4) 0.058(5) -0.020(4) 0.002(4) 0.004(3) C3 0.043(4) 0.017(3) 0.059(5) -0.010(3) -0.016(3) 0.001(3) C4 0.044(4) 0.029(4) 0.052(5) 0.007(3) -0.005(3) 0.000(3) C5 0.061(5) 0.031(4) 0.060(5) -0.005(4) -0.026(4) 0.017(4) C6 0.026(3) 0.023(3) 0.021(3) -0.001(2) -0.002(2) -0.003(2) C7 0.036(4) 0.032(3) 0.027(3) -0.006(3) -0.003(3) -0.002(3) C8 0.032(3) 0.030(3) 0.025(3) -0.007(3) -0.001(3) -0.004(3) C9 0.035(3) 0.026(3) 0.029(3) -0.007(3) -0.007(3) -0.004(3) C10 0.038(4) 0.025(3) 0.023(3) -0.001(2) -0.003(3) -0.003(3) C11 0.030(3) 0.038(4) 0.029(3) -0.010(3) 0.001(3) -0.002(3) C12 0.028(3) 0.031(3) 0.028(3) -0.006(3) -0.008(3) -0.002(3) C13 0.044(4) 0.047(4) 0.048(5) -0.008(4) 0.002(3) -0.007(3) C14 0.036(4) 0.082(7) 0.063(6) -0.008(5) -0.006(4) 0.001(4) C15 0.045(5) 0.069(6) 0.072(6) -0.007(5) -0.019(4) 0.020(4) C16 0.054(5) 0.042(4) 0.046(4) 0.000(3) -0.015(4) 0.009(4) C17 0.035(4) 0.034(4) 0.035(4) -0.009(3) -0.002(3) -0.001(3) C18 0.042(4) 0.031(3) 0.031(3) -0.011(3) -0.008(3) 0.000(3) C19 0.062(5) 0.028(4) 0.041(4) 0.002(3) -0.011(4) -0.002(3) C20 0.058(5) 0.035(4) 0.055(5) -0.002(3) 0.003(4) -0.016(4) C21 0.045(4) 0.041(4) 0.045(4) -0.011(3) -0.003(3) -0.007(3) C22 0.038(4) 0.033(4) 0.039(4) -0.005(3) -0.013(3) -0.004(3) C23 0.051(4) 0.040(4) 0.026(3) -0.007(3) -0.008(3) 0.004(3) C24 0.047(4) 0.036(4) 0.032(4) -0.012(3) 0.001(3) -0.002(3) C25 0.063(5) 0.030(4) 0.032(4) -0.011(3) -0.013(3) -0.004(3) C26 0.022(3) 0.024(3) 0.027(3) -0.002(2) -0.001(2) -0.004(2) C27 0.030(3) 0.028(3) 0.041(4) -0.003(3) -0.013(3) -0.002(3) C28 0.031(4) 0.026(3) 0.060(5) -0.004(3) -0.010(3) 0.002(3) C29 0.037(4) 0.038(4) 0.050(4) -0.019(3) 0.004(3) -0.002(3) C30 0.029(3) 0.032(3) 0.034(3) -0.011(3) 0.003(3) -0.004(3) C31 0.025(3) 0.025(3) 0.032(3) -0.006(3) -0.002(2) -0.005(2) C32 0.036(3) 0.026(3) 0.031(3) -0.010(3) -0.004(3) -0.009(3) C33 0.041(4) 0.032(4) 0.040(4) -0.013(3) -0.004(3) -0.009(3) C34 0.041(4) 0.024(3) 0.039(4) -0.002(3) -0.005(3) -0.008(3) C35 0.037(4) 0.026(3) 0.028(3) -0.006(3) -0.002(3) -0.005(3) C1A 0.026(3) 0.038(4) 0.026(3) -0.011(3) 0.000(2) -0.003(3) C2A 0.030(3) 0.049(4) 0.035(4) -0.005(3) -0.007(3) -0.008(3) C3A 0.039(4) 0.081(6) 0.043(4) -0.003(4) -0.021(3) -0.015(4) C4A 0.026(4) 0.065(5) 0.062(5) -0.017(4) -0.007(3) -0.015(3) C5A 0.030(4) 0.054(5) 0.056(5) -0.007(4) -0.001(3) -0.020(3) C6A 0.039(4) 0.049(4) 0.033(4) -0.003(3) -0.009(3) -0.011(3) C1B 0.034(3) 0.028(3) 0.023(3) -0.006(2) 0.001(2) -0.008(3) C2B 0.029(3) 0.041(4) 0.029(3) -0.015(3) 0.001(3) -0.005(3) C3B 0.034(4) 0.046(4) 0.044(4) -0.022(3) 0.000(3) 0.005(3) C4B 0.056(5) 0.041(4) 0.029(4) -0.017(3) 0.006(3) -0.008(3) C5B 0.052(4) 0.039(4) 0.028(3) -0.010(3) -0.009(3) -0.006(3) C6B 0.034(3) 0.026(3) 0.026(3) -0.005(2) 0.000(3) -0.004(3) C1C 0.025(3) 0.027(3) 0.033(3) -0.006(3) -0.004(3) -0.008(2) C2C 0.038(4) 0.031(3) 0.037(4) -0.007(3) -0.006(3) -0.010(3) C3C 0.061(5) 0.051(5) 0.036(4) -0.023(3) -0.007(4) -0.008(4) C4C 0.066(5) 0.058(5) 0.036(4) -0.014(4) -0.013(4) -0.020(4) C5C 0.043(4) 0.050(5) 0.056(5) -0.013(4) -0.022(4) -0.013(4) C6C 0.040(4) 0.035(4) 0.040(4) -0.010(3) -0.008(3) -0.012(3) C1D 0.022(3) 0.035(3) 0.033(3) -0.001(3) 0.002(3) -0.004(3) C2D 0.037(4) 0.043(4) 0.056(5) -0.002(4) 0.003(3) -0.009(3) C3D 0.057(5) 0.041(5) 0.079(7) 0.004(4) 0.010(5) -0.019(4) C4D 0.044(5) 0.054(5) 0.068(6) 0.021(4) 0.007(4) -0.016(4) C5D 0.039(4) 0.085(7) 0.031(4) -0.001(4) 0.005(3) -0.003(4) C6D 0.026(3) 0.057(5) 0.036(4) -0.009(3) 0.000(3) -0.008(3) C1S 0.063(6) 0.069(6) 0.059(6) 0.003(5) 0.000(5) 0.010(5) C2S 0.175(15) 0.132(13) 0.091(10) -0.001(9) -0.034(10) -0.059(11) C3S 0.25(2) 0.103(12) 0.201(18) -0.065(13) 0.005(15) 0.018(13) Cl1A 0.164(4) 0.169(4) 0.124(3) -0.023(3) -0.033(3) -0.078(3) Cl1B 0.0793(18) 0.0585(15) 0.116(2) 0.0040(15) 0.0227(16) 0.0113(13) Cl2A 0.195(5) 0.167(4) 0.119(3) -0.023(3) -0.044(3) -0.044(4) Cl3A 0.319(8) 0.142(4) 0.126(4) -0.051(3) 0.034(4) -0.068(5) Cl2B 0.400(16) 0.086(4) 0.062(4) -0.003(3) 0.000(6) 0.005(6) Cl3B 0.47(2) 0.131(7) 0.150(9) -0.061(6) -0.096(11) 0.046(10) P3 0.0424(11) 0.0521(12) 0.0465(12) -0.0037(9) 0.0034(9) -0.0119(9) F1 0.131(6) 0.131(6) 0.060(4) -0.024(4) 0.028(4) -0.035(5) F2 0.118(6) 0.067(4) 0.154(7) -0.011(4) 0.029(5) 0.001(4) F3 0.067(4) 0.156(6) 0.064(4) 0.016(4) 0.019(3) 0.042(4) F4 0.195(9) 0.062(4) 0.187(9) -0.038(5) 0.055(7) -0.039(5) F5 0.049(3) 0.181(7) 0.102(5) -0.038(5) -0.016(3) -0.006(4) F6 0.094(5) 0.237(10) 0.111(6) 0.021(6) -0.049(4) -0.072(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 Ru1 C6 1.972(6) . ? Ru1 C3 2.227(6) . ? Ru1 C4 2.237(7) . ? Ru1 C5 2.239(7) . ? Ru1 C1 2.243(7) . ? Ru1 C2 2.247(7) . ? Ru1 P1 2.2711(16) . ? Ru1 P2 2.2730(16) . ? Re1 C25 1.911(7) . ? Re1 C23 1.913(7) . ? Re1 C24 1.923(7) . ? Re1 N2 2.170(5) . ? Re1 N3 2.176(5) . ? Re1 N1 2.190(5) . ? Fe1 C32 2.020(6) . ? Fe1 C30 2.024(6) . ? Fe1 C33 2.033(6) . ? Fe1 C31 2.034(6) . ? Fe1 C27 2.035(6) . ? Fe1 C26 2.042(6) . ? Fe1 C34 2.045(6) . ? Fe1 C28 2.045(7) . ? Fe1 C29 2.047(7) . ? Fe1 C35 2.047(6) . ? P1 C31 1.832(6) . ? P1 C1B 1.835(6) . ? P1 C1A 1.842(6) . ? P2 C26 1.832(6) . ? P2 C1D 1.838(6) . ? P2 C1C 1.843(6) . ? O1 C23 1.151(8) . ? O2 C25 1.155(8) . ? O3 C24 1.147(8) . ? N1 C8 1.355(8) . ? N1 C12 1.356(8) . ? N2 C18 1.342(8) . ? N2 C22 1.360(8) . ? N3 C13 1.352(9) . ? N3 C17 1.355(8) . ? C1 C5 1.410(11) . ? C1 C2 1.417(11) . ? C2 C3 1.407(10) . ? C3 C4 1.419(10) . ? C4 C5 1.420(11) . ? C6 C7 1.228(8) . ? C7 C10 1.400(9) . ? C8 C9 1.374(8) . ? C9 C10 1.403(9) . ? C10 C11 1.397(9) . ? C11 C12 1.374(8) . ? C13 C14 1.352(11) . ? C14 C15 1.375(13) . ? C15 C16 1.372(11) . ? C16 C17 1.374(9) . ? C17 C18 1.488(9) . ? C18 C19 1.384(9) . ? C19 C20 1.384(11) . ? C20 C21 1.370(11) . ? C21 C22 1.362(10) . ? C26 C27 1.427(8) . ? C26 C30 1.437(8) . ? C27 C28 1.419(9) . ? C28 C29 1.412(10) . ? C29 C30 1.413(9) . ? C31 C32 1.417(8) . ? C31 C35 1.436(8) . ? C32 C33 1.422(9) . ? C33 C34 1.410(9) . ? C34 C35 1.415(9) . ? C1A C6A 1.383(9) . ? C1A C2A 1.395(9) . ? C2A C3A 1.389(9) . ? C3A C4A 1.359(11) . ? C4A C5A 1.370(11) . ? C5A C6A 1.376(9) . ? C1B C2B 1.385(8) . ? C1B C6B 1.388(8) . ? C2B C3B 1.382(9) . ? C3B C4B 1.362(10) . ? C4B C5B 1.368(10) . ? C5B C6B 1.379(9) . ? C1C C2C 1.389(9) . ? C1C C6C 1.393(9) . ? C2C C3C 1.380(9) . ? C3C C4C 1.371(11) . ? C4C C5C 1.395(11) . ? C5C C6C 1.377(9) . ? C1D C6D 1.381(9) . ? C1D C2D 1.392(10) . ? C2D C3D 1.386(10) . ? C3D C4D 1.374(13) . ? C4D C5D 1.392(12) . ? C5D C6D 1.405(10) . ? C1S Cl1A 1.705(11) . ? C1S Cl1B 1.753(10) . ? C2S Cl2C 1.53(2) . ? C2S Cl2A 1.645(14) . ? C2S Cl2B 1.647(17) . ? C3S Cl3B 1.591(15) . ? C3S Cl3C 1.60(2) . ? C3S Cl3A 1.681(17) . ? P3 F4 1.531(7) . ? P3 F6 1.551(7) . ? P3 F3 1.567(6) . ? P3 F5 1.568(6) . ? P3 F1 1.569(6) . ? P3 F2 1.569(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 Ru1 C3 137.7(3) . . ? C6 Ru1 C4 101.3(3) . . ? C3 Ru1 C4 37.1(3) . . ? C6 Ru1 C5 89.1(3) . . ? C3 Ru1 C5 61.6(3) . . ? C4 Ru1 C5 37.0(3) . . ? C6 Ru1 C1 113.0(3) . . ? C3 Ru1 C1 61.4(3) . . ? C4 Ru1 C1 61.6(3) . . ? C5 Ru1 C1 36.7(3) . . ? C6 Ru1 C2 148.9(3) . . ? C3 Ru1 C2 36.6(3) . . ? C4 Ru1 C2 61.6(3) . . ? C5 Ru1 C2 61.3(3) . . ? C1 Ru1 C2 36.8(3) . . ? C6 Ru1 P1 87.89(17) . . ? C3 Ru1 P1 133.5(2) . . ? C4 Ru1 P1 158.8(2) . . ? C5 Ru1 P1 125.5(2) . . ? C1 Ru1 P1 97.2(2) . . ? C2 Ru1 P1 101.1(2) . . ? C6 Ru1 P2 89.44(17) . . ? C3 Ru1 P2 92.57(18) . . ? C4 Ru1 P2 101.5(2) . . ? C5 Ru1 P2 136.7(2) . . ? C1 Ru1 P2 153.5(2) . . ? C2 Ru1 P2 118.3(2) . . ? P1 Ru1 P2 97.68(6) . . ? C25 Re1 C23 89.4(3) . . ? C25 Re1 C24 87.0(3) . . ? C23 Re1 C24 87.0(3) . . ? C25 Re1 N2 95.4(2) . . ? C23 Re1 N2 99.0(3) . . ? C24 Re1 N2 173.5(3) . . ? C25 Re1 N3 95.4(2) . . ? C23 Re1 N3 172.3(2) . . ? C24 Re1 N3 99.3(3) . . ? N2 Re1 N3 74.5(2) . . ? C25 Re1 N1 178.7(3) . . ? C23 Re1 N1 89.7(2) . . ? C24 Re1 N1 94.0(2) . . ? N2 Re1 N1 83.79(18) . . ? N3 Re1 N1 85.43(18) . . ? C32 Fe1 C30 105.0(3) . . ? C32 Fe1 C33 41.1(2) . . ? C30 Fe1 C33 120.6(3) . . ? C32 Fe1 C31 40.9(2) . . ? C30 Fe1 C31 121.3(3) . . ? C33 Fe1 C31 69.1(3) . . ? C32 Fe1 C27 160.5(2) . . ? C30 Fe1 C27 69.3(3) . . ? C33 Fe1 C27 157.9(3) . . ? C31 Fe1 C27 125.1(3) . . ? C32 Fe1 C26 122.6(2) . . ? C30 Fe1 C26 41.4(2) . . ? C33 Fe1 C26 158.4(3) . . ? C31 Fe1 C26 107.9(2) . . ? C27 Fe1 C26 41.0(2) . . ? C32 Fe1 C34 68.4(3) . . ? C30 Fe1 C34 157.5(3) . . ? C33 Fe1 C34 40.4(3) . . ? C31 Fe1 C34 68.6(3) . . ? C27 Fe1 C34 123.9(3) . . ? C26 Fe1 C34 160.1(3) . . ? C32 Fe1 C28 156.2(3) . . ? C30 Fe1 C28 68.7(3) . . ? C33 Fe1 C28 121.0(3) . . ? C31 Fe1 C28 161.9(3) . . ? C27 Fe1 C28 40.7(3) . . ? C26 Fe1 C28 68.6(2) . . ? C34 Fe1 C28 108.3(3) . . ? C32 Fe1 C29 120.1(3) . . ? C30 Fe1 C29 40.6(3) . . ? C33 Fe1 C29 105.3(3) . . ? C31 Fe1 C29 156.6(3) . . ? C27 Fe1 C29 68.4(3) . . ? C26 Fe1 C29 68.5(3) . . ? C34 Fe1 C29 122.7(3) . . ? C28 Fe1 C29 40.4(3) . . ? C32 Fe1 C35 68.8(3) . . ? C30 Fe1 C35 159.2(2) . . ? C33 Fe1 C35 68.6(3) . . ? C31 Fe1 C35 41.2(2) . . ? C27 Fe1 C35 109.7(3) . . ? C26 Fe1 C35 124.1(2) . . ? C34 Fe1 C35 40.5(2) . . ? C28 Fe1 C35 125.0(3) . . ? C29 Fe1 C35 159.8(3) . . ? C31 P1 C1B 105.3(3) . . ? C31 P1 C1A 96.2(3) . . ? C1B P1 C1A 102.4(3) . . ? C31 P1 Ru1 122.1(2) . . ? C1B P1 Ru1 111.8(2) . . ? C1A P1 Ru1 116.2(2) . . ? C26 P2 C1D 104.8(3) . . ? C26 P2 C1C 100.4(3) . . ? C1D P2 C1C 100.4(3) . . ? C26 P2 Ru1 121.75(19) . . ? C1D P2 Ru1 107.3(2) . . ? C1C P2 Ru1 119.5(2) . . ? C8 N1 C12 115.9(5) . . ? C8 N1 Re1 122.6(4) . . ? C12 N1 Re1 121.4(4) . . ? C18 N2 C22 117.9(6) . . ? C18 N2 Re1 117.8(4) . . ? C22 N2 Re1 124.2(4) . . ? C13 N3 C17 117.6(6) . . ? C13 N3 Re1 124.7(5) . . ? C17 N3 Re1 117.7(4) . . ? C5 C1 C2 108.0(7) . . ? C5 C1 Ru1 71.5(4) . . ? C2 C1 Ru1 71.8(4) . . ? C3 C2 C1 107.9(7) . . ? C3 C2 Ru1 70.9(4) . . ? C1 C2 Ru1 71.5(4) . . ? C2 C3 C4 108.6(7) . . ? C2 C3 Ru1 72.5(4) . . ? C4 C3 Ru1 71.8(4) . . ? C3 C4 C5 107.2(7) . . ? C3 C4 Ru1 71.1(4) . . ? C5 C4 Ru1 71.6(4) . . ? C1 C5 C4 108.3(7) . . ? C1 C5 Ru1 71.8(4) . . ? C4 C5 Ru1 71.4(4) . . ? C7 C6 Ru1 170.7(5) . . ? C6 C7 C10 176.0(7) . . ? N1 C8 C9 123.1(6) . . ? C8 C9 C10 121.1(6) . . ? C11 C10 C7 122.3(6) . . ? C11 C10 C9 115.5(6) . . ? C7 C10 C9 122.1(6) . . ? C12 C11 C10 120.4(6) . . ? N1 C12 C11 124.0(6) . . ? N3 C13 C14 122.9(8) . . ? C13 C14 C15 119.8(8) . . ? C16 C15 C14 118.2(7) . . ? C15 C16 C17 120.3(8) . . ? N3 C17 C16 121.3(7) . . ? N3 C17 C18 114.5(6) . . ? C16 C17 C18 124.2(7) . . ? N2 C18 C19 121.1(6) . . ? N2 C18 C17 115.5(6) . . ? C19 C18 C17 123.4(6) . . ? C18 C19 C20 120.2(7) . . ? C21 C20 C19 118.5(7) . . ? C22 C21 C20 119.1(7) . . ? N2 C22 C21 123.2(6) . . ? O1 C23 Re1 178.9(7) . . ? O3 C24 Re1 177.7(6) . . ? O2 C25 Re1 177.1(6) . . ? C27 C26 C30 107.3(5) . . ? C27 C26 P2 126.0(5) . . ? C30 C26 P2 126.7(5) . . ? C27 C26 Fe1 69.3(3) . . ? C30 C26 Fe1 68.6(3) . . ? P2 C26 Fe1 126.3(3) . . ? C28 C27 C26 108.0(6) . . ? C28 C27 Fe1 70.0(4) . . ? C26 C27 Fe1 69.8(3) . . ? C29 C28 C27 108.2(6) . . ? C29 C28 Fe1 69.9(4) . . ? C27 C28 Fe1 69.3(4) . . ? C28 C29 C30 108.6(6) . . ? C28 C29 Fe1 69.8(4) . . ? C30 C29 Fe1 68.8(4) . . ? C29 C30 C26 107.8(6) . . ? C29 C30 Fe1 70.5(4) . . ? C26 C30 Fe1 70.0(3) . . ? C32 C31 C35 107.3(5) . . ? C32 C31 P1 121.0(5) . . ? C35 C31 P1 131.6(5) . . ? C32 C31 Fe1 69.0(3) . . ? C35 C31 Fe1 69.9(4) . . ? P1 C31 Fe1 129.3(3) . . ? C31 C32 C33 108.6(6) . . ? C31 C32 Fe1 70.1(3) . . ? C33 C32 Fe1 69.9(4) . . ? C34 C33 C32 107.6(6) . . ? C34 C33 Fe1 70.2(4) . . ? C32 C33 Fe1 69.0(4) . . ? C33 C34 C35 108.9(6) . . ? C33 C34 Fe1 69.3(4) . . ? C35 C34 Fe1 69.9(4) . . ? C34 C35 C31 107.6(6) . . ? C34 C35 Fe1 69.7(4) . . ? C31 C35 Fe1 68.9(3) . . ? C6A C1A C2A 119.0(6) . . ? C6A C1A P1 119.3(5) . . ? C2A C1A P1 121.6(5) . . ? C3A C2A C1A 119.3(7) . . ? C4A C3A C2A 120.7(7) . . ? C3A C4A C5A 120.3(7) . . ? C4A C5A C6A 120.0(7) . . ? C5A C6A C1A 120.6(6) . . ? C2B C1B C6B 118.0(6) . . ? C2B C1B P1 120.9(5) . . ? C6B C1B P1 120.5(5) . . ? C3B C2B C1B 120.8(6) . . ? C4B C3B C2B 120.5(6) . . ? C3B C4B C5B 119.4(6) . . ? C4B C5B C6B 121.0(6) . . ? C5B C6B C1B 120.2(6) . . ? C2C C1C C6C 119.2(6) . . ? C2C C1C P2 120.7(5) . . ? C6C C1C P2 120.1(5) . . ? C3C C2C C1C 120.7(7) . . ? C4C C3C C2C 119.9(7) . . ? C3C C4C C5C 120.0(7) . . ? C6C C5C C4C 120.3(7) . . ? C5C C6C C1C 119.8(7) . . ? C6D C1D C2D 119.4(6) . . ? C6D C1D P2 120.7(5) . . ? C2D C1D P2 118.9(5) . . ? C3D C2D C1D 121.0(8) . . ? C4D C3D C2D 119.8(8) . . ? C3D C4D C5D 120.1(7) . . ? C4D C5D C6D 120.0(8) . . ? C1D C6D C5D 119.7(7) . . ? Cl1A C1S Cl1B 112.6(5) . . ? Cl2C C2S Cl2A 114.7(13) . . ? Cl2C C2S Cl2B 59.5(10) . . ? Cl2A C2S Cl2B 115.7(10) . . ? Cl3B C3S Cl3C 55.8(10) . . ? Cl3B C3S Cl3A 115.6(13) . . ? Cl3C C3S Cl3A 131.5(17) . . ? F4 P3 F6 94.0(6) . . ? F4 P3 F3 88.2(4) . . ? F6 P3 F3 87.4(4) . . ? F4 P3 F5 89.7(5) . . ? F6 P3 F5 175.8(5) . . ? F3 P3 F5 90.7(4) . . ? F4 P3 F1 92.1(4) . . ? F6 P3 F1 93.1(4) . . ? F3 P3 F1 179.3(5) . . ? F5 P3 F1 88.7(4) . . ? F4 P3 F2 178.6(6) . . ? F6 P3 F2 87.3(5) . . ? F3 P3 F2 91.6(4) . . ? F5 P3 F2 89.0(4) . . ? F1 P3 F2 88.1(4) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.614 _refine_diff_density_min -1.247 _refine_diff_density_rms 0.150 #===end data_7257 _database_code_depnum_ccdc_archive 'CCDC 721191' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C67 H57 F6 Fe N3 O4.50 P3 Re Ru' _chemical_formula_weight 1526.19 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' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.2310 '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' P P 0.1023 0.0942 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.9936(4) _cell_length_b 15.0032(5) _cell_length_c 19.5116(6) _cell_angle_alpha 76.8370(10) _cell_angle_beta 87.3760(10) _cell_angle_gamma 76.4780(10) _cell_volume 3046.71(18) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.664 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1520 _exptl_absorpt_coefficient_mu 2.611 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.4533 _exptl_absorpt_correction_T_max 0.7446 _exptl_absorpt_process_details 'Sadabs, (Sheldrick 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19681 _diffrn_reflns_av_R_equivalents 0.0675 _diffrn_reflns_av_sigmaI/netI 0.1380 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 26.00 _reflns_number_total 11983 _reflns_number_gt 7840 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0621P)^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_number_reflns 11983 _refine_ls_number_parameters 761 _refine_ls_number_restraints 66 _refine_ls_R_factor_all 0.1197 _refine_ls_R_factor_gt 0.0737 _refine_ls_wR_factor_ref 0.1652 _refine_ls_wR_factor_gt 0.1459 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.021 _refine_ls_shift/su_mean 0.001 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 0.15067(7) 0.29204(5) 0.82220(4) 0.0278(2) Uani 1 1 d . . . Re1 Re 0.62062(4) -0.27415(3) 0.69691(2) 0.02898(14) Uani 1 1 d . . . Fe1 Fe 0.53915(13) 0.30738(10) 0.78397(8) 0.0354(4) Uani 1 1 d . . . P1 P 0.2946(2) 0.29502(17) 0.90192(14) 0.0283(6) Uani 1 1 d . . . P2 P 0.2324(3) 0.37582(18) 0.72684(14) 0.0312(6) Uani 1 1 d . . . N1 N 0.5168(8) -0.1450(5) 0.7253(4) 0.032(2) Uani 1 1 d . . . N2 N 0.4823(8) -0.2443(6) 0.6141(4) 0.037(2) Uani 1 1 d . . . O1 O 0.7736(8) -0.4552(5) 0.6603(4) 0.052(2) Uani 1 1 d . . . O2 O 0.8249(8) -0.3061(6) 0.8074(4) 0.058(2) Uani 1 1 d . . . O3 O 0.4956(8) -0.4016(5) 0.8097(4) 0.050(2) Uani 1 1 d . . . C1 C -0.0471(10) 0.3342(9) 0.7807(7) 0.053(3) Uani 1 1 d . . . H1 H -0.0737 0.3623 0.7312 0.063 Uiso 1 1 calc R . . C2 C -0.0393(9) 0.3843(8) 0.8338(6) 0.043(3) Uani 1 1 d . . . H2 H -0.0593 0.4535 0.8277 0.052 Uiso 1 1 calc R . . C3 C -0.0049(9) 0.3181(8) 0.8967(6) 0.045(3) Uani 1 1 d . . . H3 H 0.0021 0.3325 0.9432 0.053 Uiso 1 1 calc R . . C4 C 0.0051(10) 0.2277(8) 0.8842(6) 0.047(3) Uani 1 1 d . . . H4 H 0.0209 0.1680 0.9203 0.056 Uiso 1 1 calc R . . C5 C -0.0198(10) 0.2377(9) 0.8133(7) 0.051(3) Uani 1 1 d . . . H5 H -0.0238 0.1860 0.7903 0.062 Uiso 1 1 calc R . . C6 C 0.2622(8) 0.1764(6) 0.8027(5) 0.027(2) Uani 1 1 d . . . C7 C 0.3210(9) 0.1040(7) 0.7883(5) 0.032(2) Uani 1 1 d . . . C8 C 0.3909(9) -0.1235(7) 0.7326(5) 0.034(2) Uani 1 1 d . . . H8 H 0.3458 -0.1656 0.7235 0.041 Uiso 1 1 calc R . . C9 C 0.3254(9) -0.0438(7) 0.7526(5) 0.034(2) Uani 1 1 d . . . H9 H 0.2378 -0.0328 0.7565 0.041 Uiso 1 1 calc R . . C10 C 0.3874(10) 0.0210(6) 0.7672(5) 0.031(2) Uani 1 1 d . . . C11 C 0.5170(9) -0.0007(7) 0.7594(5) 0.032(2) Uani 1 1 d . . . H11 H 0.5641 0.0398 0.7692 0.039 Uiso 1 1 calc R . . C12 C 0.5753(10) -0.0786(7) 0.7382(5) 0.034(2) Uani 1 1 d . . . H12 H 0.6623 -0.0887 0.7318 0.041 Uiso 1 1 calc R . . N4 N 0.6875(8) -0.1810(5) 0.6083(5) 0.037(2) Uani 1 1 d . . . C14 C 0.3762(12) -0.2746(9) 0.6173(6) 0.057(4) Uani 1 1 d . . . H14 H 0.3593 -0.3142 0.6596 0.069 Uiso 1 1 calc R . . C15 C 0.2918(14) -0.2528(10) 0.5646(7) 0.083(5) Uani 1 1 d . . . H15 H 0.2180 -0.2751 0.5711 0.100 Uiso 1 1 calc R . . C16 C 0.3155(13) -0.1975(10) 0.5012(7) 0.070(4) Uani 1 1 d . . . H16 H 0.2582 -0.1826 0.4637 0.084 Uiso 1 1 calc R . . C17 C 0.4261(11) -0.1628(8) 0.4921(6) 0.046(3) Uani 1 1 d . . . C18 C 0.4639(13) -0.1091(9) 0.4306(6) 0.061(4) Uani 1 1 d . . . H18 H 0.4132 -0.0940 0.3902 0.074 Uiso 1 1 calc R . . C19 C 0.5688(12) -0.0779(8) 0.4262(6) 0.051(3) Uani 1 1 d . . . H19 H 0.5902 -0.0412 0.3836 0.061 Uiso 1 1 calc R . . C20 C 0.6479(11) -0.1004(7) 0.4862(6) 0.041(3) Uani 1 1 d . . . C21 C 0.7615(12) -0.0724(8) 0.4845(6) 0.051(3) Uani 1 1 d . . . H21 H 0.7898 -0.0395 0.4422 0.062 Uiso 1 1 calc R . . C22 C 0.8302(12) -0.0936(8) 0.5450(7) 0.051(3) Uani 1 1 d . . . H22 H 0.9034 -0.0716 0.5458 0.061 Uiso 1 1 calc R . . C23 C 0.7916(10) -0.1467(7) 0.6039(6) 0.040(3) Uani 1 1 d . . . H23 H 0.8409 -0.1607 0.6447 0.048 Uiso 1 1 calc R . . C24 C 0.5060(10) -0.1886(7) 0.5527(5) 0.032(2) Uani 1 1 d . . . C25 C 0.6174(10) -0.1558(7) 0.5475(5) 0.033(2) Uani 1 1 d . . . C26 C 0.7151(10) -0.3854(6) 0.6714(5) 0.033(2) Uani 1 1 d . . . C27 C 0.5415(10) -0.3510(7) 0.7667(5) 0.036(3) Uani 1 1 d . . . C28 C 0.7466(12) -0.2923(7) 0.7652(6) 0.047(3) Uani 1 1 d . . . C29 C 0.4616(9) 0.2778(7) 0.8818(5) 0.033(2) Uani 1 1 d . . . C30 C 0.5353(10) 0.3458(7) 0.8759(5) 0.041(3) Uani 1 1 d . . . H30 H 0.5041 0.4106 0.8826 0.050 Uiso 1 1 calc R . . C31 C 0.6566(10) 0.3067(8) 0.8614(6) 0.049(3) Uani 1 1 d . . . H31 H 0.7273 0.3383 0.8557 0.059 Uiso 1 1 calc R . . C32 C 0.6625(11) 0.2141(8) 0.8545(6) 0.043(3) Uani 1 1 d . . . H32 H 0.7378 0.1688 0.8435 0.051 Uiso 1 1 calc R . . C33 C 0.5416(10) 0.1981(7) 0.8663(6) 0.038(3) Uani 1 1 d . . . H33 H 0.5172 0.1392 0.8645 0.045 Uiso 1 1 calc R . . C34 C 0.3999(10) 0.3589(7) 0.7120(5) 0.036(3) Uani 1 1 d . . . C35 C 0.4748(9) 0.2733(7) 0.7003(5) 0.033(2) Uani 1 1 d . . . H35 H 0.4454 0.2155 0.7012 0.040 Uiso 1 1 calc R . . C36 C 0.5982(10) 0.2839(8) 0.6874(6) 0.047(3) Uani 1 1 d . . . H36 H 0.6705 0.2346 0.6785 0.057 Uiso 1 1 calc R . . C37 C 0.6021(12) 0.3756(8) 0.6914(6) 0.052(3) Uani 1 1 d . . . H37 H 0.6768 0.4028 0.6851 0.062 Uiso 1 1 calc R . . C38 C 0.4805(9) 0.4217(7) 0.7042(6) 0.046(3) Uani 1 1 d . . . H38 H 0.4552 0.4875 0.7097 0.055 Uiso 1 1 calc R . . C1A C 0.2873(9) 0.2003(7) 0.9807(5) 0.032(2) Uani 1 1 d . . . C2A C 0.3360(11) 0.1065(7) 0.9777(6) 0.044(3) Uani 1 1 d . . . H2A H 0.3792 0.0917 0.9376 0.053 Uiso 1 1 calc R . . C3A C 0.3203(11) 0.0358(8) 1.0342(6) 0.048(3) Uani 1 1 d . . . H3A H 0.3544 -0.0273 1.0325 0.057 Uiso 1 1 calc R . . C4A C 0.2557(12) 0.0557(8) 1.0930(6) 0.053(3) Uani 1 1 d . . . H4A H 0.2439 0.0067 1.1305 0.063 Uiso 1 1 calc R . . C5A C 0.2091(12) 0.1464(9) 1.0964(6) 0.054(3) Uani 1 1 d . . . H5A H 0.1651 0.1605 1.1365 0.065 Uiso 1 1 calc R . . C6A C 0.2256(10) 0.2171(7) 1.0420(6) 0.042(3) Uani 1 1 d . . . H6A H 0.1943 0.2796 1.0459 0.050 Uiso 1 1 calc R . . C1B C 0.2705(10) 0.3968(7) 0.9425(5) 0.032(2) Uani 1 1 d . . . C2B C 0.3492(10) 0.3984(7) 0.9961(5) 0.040(3) Uani 1 1 d . . . H2B H 0.4158 0.3463 1.0119 0.048 Uiso 1 1 calc R . . C3B C 0.3313(11) 0.4740(8) 1.0260(6) 0.046(3) Uani 1 1 d . . . H3B H 0.3872 0.4740 1.0610 0.055 Uiso 1 1 calc R . . C4B C 0.2355(11) 0.5486(8) 1.0064(6) 0.048(3) Uani 1 1 d . . . H4B H 0.2246 0.6000 1.0278 0.057 Uiso 1 1 calc R . . C5B C 0.1542(11) 0.5498(7) 0.9557(6) 0.047(3) Uani 1 1 d . . . H5B H 0.0868 0.6017 0.9413 0.056 Uiso 1 1 calc R . . C6B C 0.1730(9) 0.4728(7) 0.9258(5) 0.035(2) Uani 1 1 d . . . H6B H 0.1150 0.4729 0.8918 0.042 Uiso 1 1 calc R . . C1C C 0.1787(9) 0.5028(7) 0.7194(5) 0.031(2) Uani 1 1 d . . . C2C C 0.2324(9) 0.5458(6) 0.7618(5) 0.033(2) Uani 1 1 d . . . H2C H 0.3003 0.5102 0.7911 0.040 Uiso 1 1 calc R . . C3C C 0.1888(10) 0.6396(8) 0.7619(6) 0.043(3) Uani 1 1 d . . . H3C H 0.2262 0.6670 0.7917 0.052 Uiso 1 1 calc R . . C4C C 0.0901(11) 0.6938(8) 0.7185(6) 0.052(3) Uani 1 1 d . . . H4C H 0.0598 0.7580 0.7180 0.062 Uiso 1 1 calc R . . C5C C 0.0377(11) 0.6508(8) 0.6759(7) 0.055(3) Uani 1 1 d . . . H5C H -0.0283 0.6864 0.6452 0.066 Uiso 1 1 calc R . . C6C C 0.0798(11) 0.5584(8) 0.6777(6) 0.051(3) Uani 1 1 d . . . H6C H 0.0399 0.5309 0.6491 0.061 Uiso 1 1 calc R . . C1D C 0.1848(11) 0.3602(8) 0.6411(6) 0.047(3) Uani 1 1 d . . . C2D C 0.2101(14) 0.4173(9) 0.5794(7) 0.082(5) Uani 1 1 d . . . H2D H 0.2541 0.4638 0.5802 0.098 Uiso 1 1 calc R . . C3D C 0.1713(14) 0.4071(10) 0.5162(7) 0.095(6) Uani 1 1 d . . . H3D H 0.1825 0.4500 0.4745 0.114 Uiso 1 1 calc R . . C4D C 0.1180(17) 0.3367(12) 0.5137(9) 0.088(5) Uani 1 1 d . . . H4D H 0.0989 0.3273 0.4698 0.106 Uiso 1 1 calc R . . C5D C 0.0915(14) 0.2797(11) 0.5722(7) 0.073(4) Uani 1 1 d . . . H5D H 0.0484 0.2332 0.5700 0.088 Uiso 1 1 calc R . . C6D C 0.1280(11) 0.2896(8) 0.6364(6) 0.045(3) Uani 1 1 d . . . H6D H 0.1136 0.2470 0.6777 0.054 Uiso 1 1 calc R . . P3 P 0.9297(3) 0.0388(2) 0.6854(2) 0.0639(11) Uani 1 1 d D . . O1S O 0.2443(11) 0.7785(7) 0.8651(6) 0.084(3) Uani 1 1 d . . . C1S C 0.3508(16) 0.7630(10) 0.9081(8) 0.084(5) Uani 1 1 d . . . H1S1 H 0.3607 0.7027 0.9423 0.101 Uiso 1 1 calc R . . H1S2 H 0.4262 0.7612 0.8791 0.101 Uiso 1 1 calc R . . C2S C 0.3338(19) 0.8371(11) 0.9434(9) 0.104(6) Uani 1 1 d . . . H2S1 H 0.3843 0.8817 0.9213 0.124 Uiso 1 1 calc R . . H2S2 H 0.3599 0.8125 0.9927 0.124 Uiso 1 1 calc R . . C3S C 0.204(2) 0.8828(14) 0.9389(10) 0.124(7) Uani 1 1 d . . . H3S1 H 0.1932 0.9496 0.9164 0.148 Uiso 1 1 calc R . . H3S2 H 0.1677 0.8773 0.9860 0.148 Uiso 1 1 calc R . . C4S C 0.1434(18) 0.8341(15) 0.8955(12) 0.121(7) Uani 1 1 d . . . H4S1 H 0.0930 0.7946 0.9251 0.146 Uiso 1 1 calc R . . H4S2 H 0.0894 0.8801 0.8589 0.146 Uiso 1 1 calc R . . O1Y O 0.628(2) 0.5025(19) 0.5514(11) 0.200 Uiso 0.50 1 d PD A -1 C1Y C 0.645(3) 0.424(2) 0.518(2) 0.200 Uiso 0.50 1 d PD A -1 H1Y1 H 0.6279 0.3684 0.5508 0.240 Uiso 0.50 1 calc PR A -1 H1Y2 H 0.7298 0.4084 0.4998 0.240 Uiso 0.50 1 calc PR A -1 C2Y C 0.552(2) 0.4584(14) 0.4599(10) 0.200 Uiso 0.50 1 d PD A -1 H2Y1 H 0.5085 0.4093 0.4567 0.240 Uiso 0.50 1 calc PR A -1 H2Y2 H 0.5926 0.4767 0.4150 0.240 Uiso 0.50 1 calc PR A -1 C3Y C 0.461(3) 0.542(2) 0.4772(12) 0.200 Uiso 0.50 1 d PD A -1 H3Y1 H 0.4238 0.5859 0.4341 0.240 Uiso 0.50 1 calc PR A -1 H3Y2 H 0.3935 0.5220 0.5071 0.240 Uiso 0.50 1 calc PR A -1 C4Y C 0.535(2) 0.586(2) 0.5147(18) 0.200 Uiso 0.50 1 d PD A -1 H4Y1 H 0.4837 0.6184 0.5481 0.240 Uiso 0.50 1 calc PR A -1 H4Y2 H 0.5748 0.6303 0.4820 0.240 Uiso 0.50 1 calc PR A -1 F1 F 0.8783(13) 0.1468(7) 0.6812(10) 0.109(5) Uiso 0.574(13) 1 d PD B 1 F2 F 0.7978(9) 0.0240(10) 0.6802(8) 0.099(5) Uiso 0.574(13) 1 d PD B 1 F3 F 0.9942(14) -0.0638(7) 0.6829(9) 0.109(5) Uiso 0.574(13) 1 d PD B 1 F4 F 1.0649(9) 0.0631(9) 0.6791(9) 0.099(5) Uiso 0.574(13) 1 d PD B 1 F5 F 0.9381(16) 0.0584(12) 0.6011(5) 0.110(5) Uiso 0.574(13) 1 d PD B 1 F6 F 0.9366(16) 0.0211(11) 0.7648(5) 0.110(5) Uiso 0.574(13) 1 d PD B 1 F7 F 0.8334(18) 0.0698(12) 0.7435(9) 0.114(7) Uiso 0.426(13) 1 d PD B 2 F8 F 0.9175(18) -0.0669(8) 0.7209(9) 0.097(6) Uiso 0.426(13) 1 d PD B 2 F9 F 1.0295(16) 0.0014(14) 0.6366(9) 0.114(7) Uiso 0.426(13) 1 d PD B 2 F11 F 0.8200(17) 0.0413(13) 0.6358(10) 0.098(6) Uiso 0.426(13) 1 d PD B 2 F10 F 0.9115(19) 0.1435(7) 0.6479(9) 0.097(6) Uiso 0.426(13) 1 d PD B 2 F12 F 1.0215(17) 0.0284(13) 0.7456(8) 0.098(6) Uiso 0.426(13) 1 d PD B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0198(4) 0.0299(4) 0.0359(5) -0.0157(4) -0.0013(4) -0.0018(4) Re1 0.0340(3) 0.0230(2) 0.0301(2) -0.00809(16) -0.00062(17) -0.00458(18) Fe1 0.0227(8) 0.0317(8) 0.0520(10) -0.0154(7) 0.0039(7) -0.0017(7) P1 0.0245(14) 0.0266(14) 0.0371(16) -0.0140(12) -0.0026(12) -0.0049(12) P2 0.0288(15) 0.0297(14) 0.0357(16) -0.0139(12) -0.0002(12) -0.0016(12) N1 0.039(5) 0.024(4) 0.036(5) -0.010(4) -0.003(4) -0.010(4) N2 0.043(6) 0.038(5) 0.038(5) -0.015(4) -0.001(4) -0.016(5) O1 0.060(6) 0.041(5) 0.058(5) -0.021(4) 0.001(4) -0.010(4) O2 0.051(5) 0.069(6) 0.051(5) -0.015(4) -0.012(4) -0.004(5) O3 0.060(6) 0.046(5) 0.044(5) -0.002(4) 0.005(4) -0.022(4) C1 0.021(6) 0.078(10) 0.064(9) -0.026(7) -0.012(6) -0.011(6) C2 0.023(6) 0.037(6) 0.069(9) -0.018(6) 0.000(6) 0.000(5) C3 0.025(6) 0.061(8) 0.053(8) -0.023(6) 0.003(5) -0.012(6) C4 0.026(6) 0.051(7) 0.059(8) -0.007(6) 0.003(5) -0.005(6) C5 0.030(7) 0.065(9) 0.072(9) -0.038(7) 0.000(6) -0.013(6) C6 0.016(5) 0.028(5) 0.035(6) -0.013(4) 0.004(4) 0.002(4) C7 0.026(6) 0.038(6) 0.032(6) -0.016(5) 0.002(4) -0.002(5) C8 0.028(6) 0.030(6) 0.047(7) -0.012(5) -0.003(5) -0.011(5) C9 0.021(6) 0.037(6) 0.047(7) -0.014(5) 0.006(5) -0.011(5) C10 0.040(6) 0.023(5) 0.029(6) -0.008(4) 0.002(5) -0.003(5) C11 0.021(5) 0.034(6) 0.047(7) -0.024(5) -0.002(5) 0.001(5) C12 0.029(6) 0.038(6) 0.034(6) -0.006(5) -0.005(5) -0.006(5) N4 0.037(5) 0.018(4) 0.053(6) -0.015(4) 0.011(4) 0.004(4) C14 0.059(9) 0.074(9) 0.045(8) 0.001(6) -0.009(6) -0.040(8) C15 0.092(12) 0.111(13) 0.059(10) 0.011(9) -0.032(9) -0.072(11) C16 0.056(9) 0.103(12) 0.055(9) -0.009(8) -0.023(7) -0.030(9) C17 0.053(8) 0.038(7) 0.045(7) -0.008(6) -0.001(6) -0.006(6) C18 0.069(10) 0.071(9) 0.035(7) -0.004(7) 0.001(7) -0.007(8) C19 0.065(9) 0.049(7) 0.031(7) 0.003(5) 0.008(6) -0.012(7) C20 0.048(7) 0.035(6) 0.037(7) -0.006(5) -0.009(6) -0.002(6) C21 0.066(9) 0.056(8) 0.041(8) -0.017(6) 0.013(6) -0.028(7) C22 0.059(8) 0.043(7) 0.062(9) -0.017(6) 0.018(7) -0.029(6) C23 0.029(6) 0.035(6) 0.059(8) -0.020(6) 0.006(5) -0.006(5) C24 0.034(6) 0.032(6) 0.034(6) -0.010(5) 0.001(5) -0.010(5) C25 0.037(6) 0.023(5) 0.038(6) -0.010(5) 0.002(5) -0.003(5) C26 0.053(7) 0.017(5) 0.030(6) -0.014(4) 0.000(5) -0.004(5) C27 0.039(7) 0.033(6) 0.032(6) -0.012(5) -0.006(5) 0.005(5) C28 0.052(8) 0.034(6) 0.058(8) -0.030(6) -0.003(6) 0.004(6) C29 0.032(6) 0.032(6) 0.042(6) -0.013(5) 0.002(5) -0.014(5) C30 0.040(7) 0.036(6) 0.054(8) -0.018(5) 0.002(6) -0.012(5) C31 0.023(6) 0.066(8) 0.066(9) -0.029(7) 0.002(6) -0.014(6) C32 0.041(7) 0.044(7) 0.044(7) -0.019(5) -0.008(5) -0.003(6) C33 0.032(6) 0.027(6) 0.049(7) -0.007(5) -0.012(5) 0.002(5) C34 0.037(6) 0.038(6) 0.030(6) -0.006(5) 0.000(5) -0.005(5) C35 0.031(6) 0.041(6) 0.027(6) -0.009(5) 0.011(4) -0.009(5) C36 0.027(6) 0.055(8) 0.060(8) -0.022(6) 0.020(5) -0.005(6) C37 0.052(8) 0.047(7) 0.059(8) -0.007(6) 0.004(6) -0.020(6) C38 0.032(7) 0.030(6) 0.069(9) -0.003(6) 0.009(6) -0.004(5) C1A 0.025(6) 0.031(6) 0.045(7) -0.010(5) -0.001(5) -0.013(5) C2A 0.054(8) 0.037(6) 0.040(7) -0.009(5) -0.011(6) -0.006(6) C3A 0.063(8) 0.030(6) 0.051(8) -0.007(6) -0.012(6) -0.013(6) C4A 0.078(10) 0.038(7) 0.039(7) 0.009(6) -0.016(7) -0.020(7) C5A 0.073(9) 0.053(8) 0.037(7) -0.015(6) 0.008(6) -0.013(7) C6A 0.040(7) 0.047(7) 0.046(7) -0.028(6) 0.002(5) -0.008(6) C1B 0.040(6) 0.027(5) 0.034(6) -0.013(5) 0.006(5) -0.011(5) C2B 0.037(7) 0.037(6) 0.046(7) -0.012(5) -0.003(5) -0.007(5) C3B 0.055(8) 0.049(7) 0.045(7) -0.024(6) -0.004(6) -0.023(7) C4B 0.052(8) 0.043(7) 0.063(8) -0.031(6) 0.005(6) -0.020(6) C5B 0.047(7) 0.032(6) 0.060(8) -0.022(6) 0.012(6) 0.001(5) C6B 0.028(6) 0.038(6) 0.041(6) -0.015(5) 0.008(5) -0.007(5) C1C 0.025(6) 0.030(5) 0.039(6) -0.012(5) 0.004(5) -0.004(5) C2C 0.028(6) 0.028(5) 0.043(7) -0.012(5) 0.005(5) 0.000(5) C3C 0.042(7) 0.047(7) 0.044(7) -0.012(6) 0.000(6) -0.016(6) C4C 0.056(8) 0.031(6) 0.066(9) -0.015(6) 0.001(7) -0.002(6) C5C 0.044(8) 0.047(7) 0.067(9) -0.011(7) -0.015(7) 0.007(6) C6C 0.058(8) 0.040(7) 0.059(8) -0.020(6) -0.020(7) -0.005(6) C1D 0.061(8) 0.048(7) 0.026(6) -0.017(5) -0.004(6) 0.005(6) C2D 0.145(16) 0.064(9) 0.048(9) -0.025(7) -0.006(9) -0.036(10) C3D 0.171(19) 0.061(10) 0.040(9) -0.011(7) -0.005(10) 0.001(11) C4D 0.123(15) 0.084(12) 0.065(11) -0.046(10) -0.018(10) -0.007(11) C5D 0.093(12) 0.084(11) 0.049(9) -0.040(8) -0.008(8) -0.008(9) C6D 0.058(8) 0.044(7) 0.036(7) -0.018(5) -0.011(6) -0.007(6) P3 0.045(2) 0.060(2) 0.092(3) -0.033(2) -0.025(2) -0.0006(18) O1S 0.095(9) 0.077(7) 0.087(8) -0.011(6) -0.036(7) -0.032(7) C1S 0.104(14) 0.087(12) 0.066(11) -0.023(9) 0.004(10) -0.026(10) C2S 0.124(17) 0.098(14) 0.087(13) -0.037(11) -0.021(12) -0.001(13) C3S 0.15(2) 0.119(17) 0.110(16) -0.069(14) 0.021(15) -0.010(16) C4S 0.087(15) 0.115(17) 0.15(2) -0.002(15) 0.010(14) -0.028(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C6 1.980(9) . ? Ru1 C3 2.216(11) . ? Ru1 C4 2.229(11) . ? Ru1 C5 2.240(11) . ? Ru1 C1 2.251(10) . ? Ru1 C2 2.253(10) . ? Ru1 P2 2.271(3) . ? Ru1 P1 2.284(3) . ? Re1 C27 1.894(12) . ? Re1 C28 1.896(12) . ? Re1 C26 1.906(9) . ? Re1 N2 2.168(8) . ? Re1 N4 2.178(9) . ? Re1 N1 2.182(8) . ? Fe1 C30 2.000(10) . ? Fe1 C33 2.013(11) . ? Fe1 C34 2.015(10) . ? Fe1 C35 2.021(10) . ? Fe1 C32 2.024(11) . ? Fe1 C31 2.028(11) . ? Fe1 C38 2.034(10) . ? Fe1 C37 2.041(12) . ? Fe1 C36 2.045(11) . ? Fe1 C29 2.052(10) . ? P1 C29 1.830(10) . ? P1 C1B 1.836(9) . ? P1 C1A 1.854(10) . ? P2 C34 1.818(11) . ? P2 C1C 1.832(10) . ? P2 C1D 1.856(10) . ? N1 C8 1.354(12) . ? N1 C12 1.379(12) . ? N2 C14 1.342(13) . ? N2 C24 1.349(13) . ? O1 C26 1.153(11) . ? O2 C28 1.168(12) . ? O3 C27 1.176(12) . ? C1 C5 1.409(16) . ? C1 C2 1.428(15) . ? C2 C3 1.395(15) . ? C3 C4 1.410(15) . ? C4 C5 1.390(15) . ? C6 C7 1.213(12) . ? C7 C10 1.427(12) . ? C8 C9 1.373(13) . ? C9 C10 1.394(13) . ? C10 C11 1.395(13) . ? C11 C12 1.339(13) . ? N4 C23 1.353(13) . ? N4 C25 1.374(12) . ? C14 C15 1.348(15) . ? C15 C16 1.375(18) . ? C16 C17 1.420(17) . ? C17 C18 1.390(16) . ? C17 C24 1.430(14) . ? C18 C19 1.334(16) . ? C19 C20 1.419(15) . ? C20 C25 1.370(14) . ? C20 C21 1.404(16) . ? C21 C22 1.367(16) . ? C22 C23 1.352(15) . ? C24 C25 1.415(14) . ? C29 C33 1.394(13) . ? C29 C30 1.427(13) . ? C30 C31 1.371(14) . ? C31 C32 1.412(15) . ? C32 C33 1.405(15) . ? C34 C35 1.415(13) . ? C34 C38 1.417(14) . ? C35 C36 1.408(14) . ? C36 C37 1.406(15) . ? C37 C38 1.394(15) . ? C1A C6A 1.391(14) . ? C1A C2A 1.397(13) . ? C2A C3A 1.381(15) . ? C3A C4A 1.375(16) . ? C4A C5A 1.352(15) . ? C5A C6A 1.358(15) . ? C1B C6B 1.359(13) . ? C1B C2B 1.396(13) . ? C2B C3B 1.361(13) . ? C3B C4B 1.340(15) . ? C4B C5B 1.359(15) . ? C5B C6B 1.379(13) . ? C1C C6C 1.375(14) . ? C1C C2C 1.383(13) . ? C2C C3C 1.378(13) . ? C3C C4C 1.383(15) . ? C4C C5C 1.378(15) . ? C5C C6C 1.347(14) . ? C1D C2D 1.368(17) . ? C1D C6D 1.371(15) . ? C2D C3D 1.374(17) . ? C3D C4D 1.333(19) . ? C4D C5D 1.33(2) . ? C5D C6D 1.383(15) . ? P3 F9 1.511(9) . ? P3 F6 1.513(9) . ? P3 F2 1.529(9) . ? P3 F12 1.541(9) . ? P3 F10 1.545(9) . ? P3 F3 1.547(9) . ? P3 F11 1.569(9) . ? P3 F1 1.572(9) . ? P3 F7 1.589(9) . ? P3 F4 1.604(9) . ? P3 F5 1.605(9) . ? P3 F8 1.613(9) . ? O1S C1S 1.415(16) . ? O1S C4S 1.42(2) . ? C1S C2S 1.408(12) . ? C2S C3S 1.42(2) . ? C3S C4S 1.51(2) . ? O1Y C1Y 1.444(18) . ? O1Y C4Y 1.481(19) . ? C1Y C2Y 1.478(17) . ? C2Y C3Y 1.503(18) . ? C3Y C4Y 1.470(18) . ? 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 C6 Ru1 C3 133.5(4) . . ? C6 Ru1 C4 98.8(4) . . ? C3 Ru1 C4 37.0(4) . . ? C6 Ru1 C5 91.7(4) . . ? C3 Ru1 C5 61.2(4) . . ? C4 Ru1 C5 36.2(4) . . ? C6 Ru1 C1 118.6(4) . . ? C3 Ru1 C1 61.3(4) . . ? C4 Ru1 C1 61.0(4) . . ? C5 Ru1 C1 36.6(4) . . ? C6 Ru1 C2 152.7(4) . . ? C3 Ru1 C2 36.4(4) . . ? C4 Ru1 C2 61.0(4) . . ? C5 Ru1 C2 61.1(4) . . ? C1 Ru1 C2 37.0(4) . . ? C6 Ru1 P2 88.4(3) . . ? C3 Ru1 P2 137.6(3) . . ? C4 Ru1 P2 156.2(3) . . ? C5 Ru1 P2 121.5(3) . . ? C1 Ru1 P2 95.7(4) . . ? C2 Ru1 P2 103.7(3) . . ? C6 Ru1 P1 88.9(3) . . ? C3 Ru1 P1 91.9(3) . . ? C4 Ru1 P1 106.3(3) . . ? C5 Ru1 P1 142.0(3) . . ? C1 Ru1 P1 150.1(3) . . ? C2 Ru1 P1 113.4(3) . . ? P2 Ru1 P1 96.49(10) . . ? C27 Re1 C28 86.7(5) . . ? C27 Re1 C26 88.4(4) . . ? C28 Re1 C26 87.2(4) . . ? C27 Re1 N2 97.6(4) . . ? C28 Re1 N2 175.5(4) . . ? C26 Re1 N2 94.2(4) . . ? C27 Re1 N4 172.0(4) . . ? C28 Re1 N4 101.1(5) . . ? C26 Re1 N4 93.5(4) . . ? N2 Re1 N4 74.6(3) . . ? C27 Re1 N1 92.9(4) . . ? C28 Re1 N1 92.1(4) . . ? C26 Re1 N1 178.4(4) . . ? N2 Re1 N1 86.5(3) . . ? N4 Re1 N1 85.2(3) . . ? C30 Fe1 C33 68.2(4) . . ? C30 Fe1 C34 123.3(4) . . ? C33 Fe1 C34 124.2(4) . . ? C30 Fe1 C35 158.5(4) . . ? C33 Fe1 C35 106.7(4) . . ? C34 Fe1 C35 41.1(4) . . ? C30 Fe1 C32 68.0(4) . . ? C33 Fe1 C32 40.7(4) . . ? C34 Fe1 C32 160.2(4) . . ? C35 Fe1 C32 122.7(4) . . ? C30 Fe1 C31 39.8(4) . . ? C33 Fe1 C31 68.3(5) . . ? C34 Fe1 C31 157.9(5) . . ? C35 Fe1 C31 159.7(4) . . ? C32 Fe1 C31 40.8(4) . . ? C30 Fe1 C38 110.6(4) . . ? C33 Fe1 C38 162.8(4) . . ? C34 Fe1 C38 41.0(4) . . ? C35 Fe1 C38 67.8(4) . . ? C32 Fe1 C38 156.1(5) . . ? C31 Fe1 C38 122.6(5) . . ? C30 Fe1 C37 125.2(5) . . ? C33 Fe1 C37 155.0(5) . . ? C34 Fe1 C37 69.1(5) . . ? C35 Fe1 C37 68.3(4) . . ? C32 Fe1 C37 119.8(5) . . ? C31 Fe1 C37 107.4(5) . . ? C38 Fe1 C37 40.0(4) . . ? C30 Fe1 C36 160.4(4) . . ? C33 Fe1 C36 120.1(5) . . ? C34 Fe1 C36 68.8(4) . . ? C35 Fe1 C36 40.5(4) . . ? C32 Fe1 C36 105.8(5) . . ? C31 Fe1 C36 123.6(5) . . ? C38 Fe1 C36 67.1(4) . . ? C37 Fe1 C36 40.3(4) . . ? C30 Fe1 C29 41.2(4) . . ? C33 Fe1 C29 40.1(4) . . ? C34 Fe1 C29 108.5(4) . . ? C35 Fe1 C29 121.5(4) . . ? C32 Fe1 C29 68.1(4) . . ? C31 Fe1 C29 68.1(4) . . ? C38 Fe1 C29 127.7(4) . . ? C37 Fe1 C29 163.3(4) . . ? C36 Fe1 C29 155.7(4) . . ? C29 P1 C1B 100.9(5) . . ? C29 P1 C1A 104.0(5) . . ? C1B P1 C1A 100.4(4) . . ? C29 P1 Ru1 122.0(3) . . ? C1B P1 Ru1 119.0(3) . . ? C1A P1 Ru1 107.8(3) . . ? C34 P2 C1C 103.8(5) . . ? C34 P2 C1D 98.7(5) . . ? C1C P2 C1D 103.0(5) . . ? C34 P2 Ru1 122.5(3) . . ? C1C P2 Ru1 112.0(3) . . ? C1D P2 Ru1 114.4(4) . . ? C8 N1 C12 114.3(8) . . ? C8 N1 Re1 123.6(6) . . ? C12 N1 Re1 122.2(7) . . ? C14 N2 C24 116.6(9) . . ? C14 N2 Re1 127.4(8) . . ? C24 N2 Re1 116.0(7) . . ? C5 C1 C2 107.3(11) . . ? C5 C1 Ru1 71.3(6) . . ? C2 C1 Ru1 71.6(6) . . ? C3 C2 C1 107.6(10) . . ? C3 C2 Ru1 70.4(6) . . ? C1 C2 Ru1 71.4(6) . . ? C2 C3 C4 108.4(10) . . ? C2 C3 Ru1 73.3(7) . . ? C4 C3 Ru1 72.0(7) . . ? C5 C4 C3 108.2(11) . . ? C5 C4 Ru1 72.3(7) . . ? C3 C4 Ru1 71.0(7) . . ? C4 C5 C1 108.5(11) . . ? C4 C5 Ru1 71.4(6) . . ? C1 C5 Ru1 72.1(6) . . ? C7 C6 Ru1 174.0(8) . . ? C6 C7 C10 176.6(11) . . ? N1 C8 C9 123.9(9) . . ? C8 C9 C10 120.6(9) . . ? C9 C10 C11 115.7(9) . . ? C9 C10 C7 121.4(9) . . ? C11 C10 C7 122.8(9) . . ? C12 C11 C10 120.9(9) . . ? C11 C12 N1 124.6(10) . . ? C23 N4 C25 114.9(9) . . ? C23 N4 Re1 128.9(8) . . ? C25 N4 Re1 116.2(7) . . ? N2 C14 C15 125.2(12) . . ? C14 C15 C16 118.8(13) . . ? C15 C16 C17 120.3(11) . . ? C18 C17 C16 126.5(12) . . ? C18 C17 C24 118.3(12) . . ? C16 C17 C24 115.3(11) . . ? C19 C18 C17 123.1(12) . . ? C18 C19 C20 119.7(11) . . ? C25 C20 C21 117.7(10) . . ? C25 C20 C19 119.7(11) . . ? C21 C20 C19 122.5(11) . . ? C22 C21 C20 119.1(11) . . ? C23 C22 C21 119.1(12) . . ? C22 C23 N4 125.0(11) . . ? N2 C24 C25 118.0(9) . . ? N2 C24 C17 123.6(10) . . ? C25 C24 C17 118.3(10) . . ? C20 C25 N4 124.0(10) . . ? C20 C25 C24 120.9(10) . . ? N4 C25 C24 115.1(9) . . ? O1 C26 Re1 175.8(9) . . ? O3 C27 Re1 177.5(9) . . ? O2 C28 Re1 178.2(9) . . ? C33 C29 C30 105.9(9) . . ? C33 C29 P1 127.7(8) . . ? C30 C29 P1 126.4(7) . . ? C33 C29 Fe1 68.5(6) . . ? C30 C29 Fe1 67.5(6) . . ? P1 C29 Fe1 126.5(5) . . ? C31 C30 C29 109.6(9) . . ? C31 C30 Fe1 71.2(6) . . ? C29 C30 Fe1 71.4(6) . . ? C30 C31 C32 107.9(10) . . ? C30 C31 Fe1 69.0(6) . . ? C32 C31 Fe1 69.4(6) . . ? C33 C32 C31 107.3(10) . . ? C33 C32 Fe1 69.2(6) . . ? C31 C32 Fe1 69.8(6) . . ? C29 C33 C32 109.3(9) . . ? C29 C33 Fe1 71.5(6) . . ? C32 C33 Fe1 70.0(6) . . ? C35 C34 C38 105.9(9) . . ? C35 C34 P2 122.3(8) . . ? C38 C34 P2 131.7(8) . . ? C35 C34 Fe1 69.7(6) . . ? C38 C34 Fe1 70.2(6) . . ? P2 C34 Fe1 128.0(6) . . ? C36 C35 C34 108.6(10) . . ? C36 C35 Fe1 70.7(6) . . ? C34 C35 Fe1 69.2(6) . . ? C37 C36 C35 108.3(10) . . ? C37 C36 Fe1 69.7(7) . . ? C35 C36 Fe1 68.8(6) . . ? C38 C37 C36 107.1(10) . . ? C38 C37 Fe1 69.7(7) . . ? C36 C37 Fe1 70.0(7) . . ? C37 C38 C34 109.9(10) . . ? C37 C38 Fe1 70.3(6) . . ? C34 C38 Fe1 68.8(6) . . ? C6A C1A C2A 117.2(10) . . ? C6A C1A P1 123.0(8) . . ? C2A C1A P1 119.6(8) . . ? C3A C2A C1A 119.5(11) . . ? C4A C3A C2A 121.3(11) . . ? C5A C4A C3A 119.5(11) . . ? C4A C5A C6A 120.2(12) . . ? C5A C6A C1A 122.4(10) . . ? C6B C1B C2B 115.4(9) . . ? C6B C1B P1 123.3(8) . . ? C2B C1B P1 121.2(8) . . ? C3B C2B C1B 121.1(10) . . ? C4B C3B C2B 121.4(11) . . ? C3B C4B C5B 120.0(10) . . ? C4B C5B C6B 118.2(11) . . ? C1B C6B C5B 123.8(10) . . ? C6C C1C C2C 116.6(9) . . ? C6C C1C P2 123.7(8) . . ? C2C C1C P2 119.5(7) . . ? C3C C2C C1C 121.5(9) . . ? C2C C3C C4C 120.3(10) . . ? C5C C4C C3C 117.9(10) . . ? C6C C5C C4C 121.0(11) . . ? C5C C6C C1C 122.7(10) . . ? C2D C1D C6D 117.3(10) . . ? C2D C1D P2 120.6(10) . . ? C6D C1D P2 122.0(9) . . ? C1D C2D C3D 120.2(12) . . ? C4D C3D C2D 120.6(14) . . ? C5D C4D C3D 121.0(14) . . ? C4D C5D C6D 119.2(15) . . ? C1D C6D C5D 121.3(12) . . ? F9 P3 F6 127.3(9) . . ? F9 P3 F2 118.9(10) . . ? F6 P3 F2 97.4(7) . . ? F9 P3 F12 94.9(8) . . ? F6 P3 F12 38.6(8) . . ? F2 P3 F12 135.7(9) . . ? F9 P3 F10 96.2(8) . . ? F6 P3 F10 113.7(10) . . ? F2 P3 F10 101.1(10) . . ? F12 P3 F10 102.8(11) . . ? F9 P3 F3 49.9(9) . . ? F6 P3 F3 94.3(7) . . ? F2 P3 F3 93.8(8) . . ? F12 P3 F3 86.8(10) . . ? F10 P3 F3 145.8(8) . . ? F9 P3 F11 93.3(12) . . ? F6 P3 F11 130.5(10) . . ? F2 P3 F11 33.2(8) . . ? F12 P3 F11 168.8(11) . . ? F10 P3 F11 83.8(11) . . ? F3 P3 F11 92.7(10) . . ? F9 P3 F1 122.7(10) . . ? F6 P3 F1 89.9(9) . . ? F2 P3 F1 91.8(6) . . ? F12 P3 F1 92.7(10) . . ? F10 P3 F1 27.3(8) . . ? F3 P3 F1 172.4(8) . . ? F11 P3 F1 89.3(10) . . ? F9 P3 F7 173.7(10) . . ? F6 P3 F7 46.6(9) . . ? F2 P3 F7 63.7(9) . . ? F12 P3 F7 80.1(11) . . ? F10 P3 F7 88.6(7) . . ? F3 P3 F7 125.5(8) . . ? F11 P3 F7 91.2(12) . . ? F1 P3 F7 61.7(8) . . ? F9 P3 F4 57.4(9) . . ? F6 P3 F4 90.4(8) . . ? F2 P3 F4 171.5(8) . . ? F12 P3 F4 52.5(8) . . ? F10 P3 F4 72.6(9) . . ? F3 P3 F4 88.7(6) . . ? F11 P3 F4 138.7(11) . . ? F1 P3 F4 84.9(6) . . ? F7 P3 F4 120.8(10) . . ? F9 P3 F5 48.0(8) . . ? F6 P3 F5 173.7(8) . . ? F2 P3 F5 88.8(6) . . ? F12 P3 F5 135.2(9) . . ? F10 P3 F5 65.2(9) . . ? F3 P3 F5 84.7(9) . . ? F11 P3 F5 55.7(9) . . ? F1 P3 F5 90.3(9) . . ? F7 P3 F5 138.2(10) . . ? F4 P3 F5 83.4(8) . . ? F9 P3 F8 90.3(11) . . ? F6 P3 F8 69.5(9) . . ? F2 P3 F8 66.7(8) . . ? F12 P3 F8 86.9(7) . . ? F10 P3 F8 167.8(10) . . ? F3 P3 F8 40.7(8) . . ? F11 P3 F8 85.5(7) . . ? F1 P3 F8 146.9(9) . . ? F7 P3 F8 85.7(7) . . ? F4 P3 F8 119.5(8) . . ? F5 P3 F8 112.9(9) . . ? C1S O1S C4S 107.1(12) . . ? C2S C1S O1S 108.1(14) . . ? C1S C2S C3S 107.7(16) . . ? C2S C3S C4S 106.3(15) . . ? O1S C4S C3S 104.8(15) . . ? C1Y O1Y C4Y 112.7(13) . . ? O1Y C1Y C2Y 103.5(13) . . ? C1Y C2Y C3Y 106.2(11) . . ? C4Y C3Y C2Y 105.3(13) . . ? C3Y C4Y O1Y 100.9(13) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.301 _refine_diff_density_min -0.915 _refine_diff_density_rms 0.172 #===end data_7263 _database_code_depnum_ccdc_archive 'CCDC 721192' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H64 F6 Fe N4 O5 P3 Re Ru' _chemical_formula_weight 1615.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.2310 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.7232(4) _cell_length_b 16.4535(5) _cell_length_c 37.8595(12) _cell_angle_alpha 90.00 _cell_angle_beta 93.8910(10) _cell_angle_gamma 90.00 _cell_volume 6664.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 2883 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 20.08 _exptl_crystal_description Block _exptl_crystal_colour Orange _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas 'Not Measured' _exptl_crystal_density_diffrn 1.610 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3232 _exptl_absorpt_coefficient_mu 2.394 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.4795 _exptl_absorpt_correction_T_max 0.7621 _exptl_absorpt_process_details 'Sadabs, (Sheldrick 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38909 _diffrn_reflns_av_R_equivalents 0.0797 _diffrn_reflns_av_sigmaI/netI 0.0829 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -45 _diffrn_reflns_limit_l_max 45 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11738 _reflns_number_gt 8372 _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, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0420P)^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_number_reflns 11738 _refine_ls_number_parameters 838 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.0790 _refine_ls_R_factor_gt 0.0490 _refine_ls_wR_factor_ref 0.1093 _refine_ls_wR_factor_gt 0.0989 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re 0.52349(3) -0.236621(16) 0.070649(7) 0.02939(9) Uani 1 1 d . . . Ru1 Ru 0.40029(5) 0.27102(3) 0.181518(13) 0.02446(13) Uani 1 1 d . . . Fe1 Fe 0.80097(8) 0.29484(6) 0.16748(2) 0.0301(2) Uani 1 1 d . . . P1 P 0.49706(16) 0.35211(10) 0.14290(4) 0.0281(4) Uani 1 1 d . . . P2 P 0.56231(15) 0.25423(10) 0.22312(4) 0.0251(4) Uani 1 1 d . . . O1 O 0.2706(5) -0.2610(3) 0.10178(14) 0.0526(14) Uani 1 1 d . . . O2 O 0.5310(5) -0.4179(3) 0.05103(13) 0.0516(14) Uani 1 1 d . . . O3 O 0.6543(5) -0.2822(3) 0.14270(13) 0.0496(14) Uani 1 1 d . . . N1 N 0.5195(5) -0.1079(3) 0.08650(13) 0.0280(12) Uani 1 1 d . . . N2 N 0.4372(5) -0.1912(3) 0.02164(14) 0.0345(14) Uani 1 1 d . . . N3 N 0.6801(5) -0.1947(3) 0.04033(13) 0.0322(13) Uani 1 1 d . . . N4 N 0.8048(6) -0.3390(4) 0.07071(15) 0.0418(15) Uani 1 1 d . . . C1 C 0.2336(6) 0.2169(4) 0.20446(19) 0.0364(17) Uani 1 1 d . . . H1 H 0.2306 0.1632 0.2162 0.044 Uiso 1 1 calc R . . C2 C 0.2601(6) 0.2920(4) 0.22177(19) 0.0355(17) Uani 1 1 d . . . H2 H 0.2792 0.2995 0.2475 0.043 Uiso 1 1 calc R . . C3 C 0.2459(6) 0.3547(4) 0.19620(19) 0.0361(17) Uani 1 1 d . . . H3 H 0.2527 0.4139 0.2007 0.043 Uiso 1 1 calc R . . C4 C 0.2113(6) 0.3160(5) 0.1629(2) 0.0426(19) Uani 1 1 d . . . H4 H 0.1903 0.3445 0.1402 0.051 Uiso 1 1 calc R . . C5 C 0.2041(6) 0.2322(4) 0.16828(19) 0.0403(18) Uani 1 1 d . . . H5 H 0.1763 0.1913 0.1503 0.048 Uiso 1 1 calc R . . C6 C 0.4645(6) 0.1771(4) 0.15638(17) 0.0284(15) Uani 1 1 d . . . C7 C 0.4929(6) 0.1175(4) 0.13955(17) 0.0292(15) Uani 1 1 d . . . C8 C 0.6226(6) -0.0695(4) 0.10080(17) 0.0320(16) Uani 1 1 d . . . H8 H 0.7005 -0.0950 0.0993 0.038 Uiso 1 1 calc R . . C9 C 0.6194(6) 0.0046(4) 0.11732(16) 0.0295(15) Uani 1 1 d . . . H9 H 0.6940 0.0291 0.1264 0.035 Uiso 1 1 calc R . . C10 C 0.5051(6) 0.0437(4) 0.12062(16) 0.0283(15) Uani 1 1 d . . . C11 C 0.3997(7) 0.0055(4) 0.10420(17) 0.0357(17) Uani 1 1 d . . . H11 H 0.3212 0.0309 0.1042 0.043 Uiso 1 1 calc R . . C12 C 0.4100(6) -0.0677(4) 0.08824(17) 0.0347(17) Uani 1 1 d . . . H12 H 0.3371 -0.0918 0.0778 0.042 Uiso 1 1 calc R . . C13 C 0.3160(7) -0.2000(5) 0.0109(2) 0.048(2) Uani 1 1 d . . . H13 H 0.2655 -0.2330 0.0244 0.058 Uiso 1 1 calc R . . C14 C 0.2631(8) -0.1630(5) -0.0188(2) 0.061(2) Uani 1 1 d . . . H14 H 0.1774 -0.1696 -0.0252 0.073 Uiso 1 1 calc R . . C15 C 0.3347(9) -0.1170(6) -0.0390(2) 0.071(3) Uani 1 1 d . . . H15 H 0.2999 -0.0915 -0.0596 0.085 Uiso 1 1 calc R . . C16 C 0.4590(8) -0.1080(5) -0.0288(2) 0.056(2) Uani 1 1 d . . . H16 H 0.5099 -0.0758 -0.0424 0.067 Uiso 1 1 calc R . . C17 C 0.5101(7) -0.1461(4) 0.00142(17) 0.0375(17) Uani 1 1 d . . . C18 C 0.6443(7) -0.1444(4) 0.01257(18) 0.0395(18) Uani 1 1 d . . . C19 C 0.7295(7) -0.0981(4) -0.00436(18) 0.0442(19) Uani 1 1 d . . . H19 H 0.7024 -0.0638 -0.0232 0.053 Uiso 1 1 calc R . . C20 C 0.8547(8) -0.1023(4) 0.0065(2) 0.050(2) Uani 1 1 d . . . H20 H 0.9127 -0.0685 -0.0038 0.060 Uiso 1 1 calc R . . C21 C 0.8944(7) -0.1565(4) 0.03284(19) 0.046(2) Uani 1 1 d . . . H21 H 0.9798 -0.1625 0.0396 0.055 Uiso 1 1 calc R . . C22 C 0.8042(7) -0.2024(4) 0.04921(17) 0.0337(17) Uani 1 1 d . . . C23 C 0.8483(7) -0.2631(4) 0.07644(18) 0.0372(17) Uani 1 1 d . . . C24 C 0.9331(7) -0.2417(5) 0.1040(2) 0.0455(19) Uani 1 1 d . . . H24 H 0.9627 -0.1881 0.1065 0.055 Uiso 1 1 calc R . . C25 C 0.9733(8) -0.3018(6) 0.1279(2) 0.063(2) Uani 1 1 d . . . H25 H 1.0309 -0.2899 0.1471 0.076 Uiso 1 1 calc R . . C26 C 0.9269(8) -0.3788(5) 0.1230(2) 0.061(2) Uani 1 1 d . . . H26 H 0.9506 -0.4202 0.1392 0.073 Uiso 1 1 calc R . . C27 C 0.8461(8) -0.3951(5) 0.0944(2) 0.057(2) Uani 1 1 d . . . H27 H 0.8177 -0.4488 0.0911 0.069 Uiso 1 1 calc R . . C28 C 0.5277(7) -0.3497(4) 0.05745(17) 0.0366(17) Uani 1 1 d . . . C29 C 0.3690(7) -0.2538(4) 0.09071(18) 0.0368(17) Uani 1 1 d . . . C30 C 0.6086(7) -0.2652(4) 0.1152(2) 0.0401(18) Uani 1 1 d . . . C31 C 0.6639(6) 0.3492(4) 0.13651(15) 0.0266(15) Uani 1 1 d . . . C32 C 0.7187(6) 0.2838(4) 0.11810(17) 0.0374(17) Uani 1 1 d . . . H32 H 0.6744 0.2352 0.1083 0.045 Uiso 1 1 calc R . . C33 C 0.8478(6) 0.3004(4) 0.11679(18) 0.0403(18) Uani 1 1 d . . . H33 H 0.9094 0.2650 0.1060 0.048 Uiso 1 1 calc R . . C34 C 0.8739(7) 0.3752(4) 0.13302(18) 0.0402(19) Uani 1 1 d . . . H34 H 0.9572 0.4011 0.1361 0.048 Uiso 1 1 calc R . . C35 C 0.7620(6) 0.4068(4) 0.14516(18) 0.0369(17) Uani 1 1 d . . . H35 H 0.7534 0.4585 0.1582 0.044 Uiso 1 1 calc R . . C36 C 0.7224(6) 0.2471(4) 0.21018(16) 0.0289(15) Uani 1 1 d . . . C37 C 0.8235(6) 0.2984(4) 0.22192(17) 0.0318(16) Uani 1 1 d . . . H37 H 0.8171 0.3476 0.2368 0.038 Uiso 1 1 calc R . . C38 C 0.9338(6) 0.2692(4) 0.20780(18) 0.0388(18) Uani 1 1 d . . . H38 H 1.0180 0.2938 0.2112 0.047 Uiso 1 1 calc R . . C39 C 0.9012(6) 0.1976(4) 0.18743(18) 0.0357(17) Uani 1 1 d . . . H39 H 0.9593 0.1639 0.1744 0.043 Uiso 1 1 calc R . . C40 C 0.7709(6) 0.1852(4) 0.18849(17) 0.0334(16) Uani 1 1 d . . . H40 H 0.7222 0.1404 0.1768 0.040 Uiso 1 1 calc R . . C1A C 0.4387(6) 0.3409(4) 0.09617(17) 0.0323(16) Uani 1 1 d . . . C2A C 0.4844(7) 0.3919(4) 0.07064(18) 0.0435(19) Uani 1 1 d . . . H2A H 0.5503 0.4277 0.0771 0.052 Uiso 1 1 calc R . . C3A C 0.4352(8) 0.3908(5) 0.03635(19) 0.051(2) Uani 1 1 d . . . H3A H 0.4666 0.4255 0.0194 0.061 Uiso 1 1 calc R . . C4A C 0.3375(8) 0.3373(5) 0.0270(2) 0.053(2) Uani 1 1 d . . . H4A H 0.3015 0.3371 0.0037 0.063 Uiso 1 1 calc R . . C5A C 0.2939(7) 0.2856(4) 0.05125(19) 0.0440(19) Uani 1 1 d . . . H5A H 0.2292 0.2490 0.0445 0.053 Uiso 1 1 calc R . . C6A C 0.3452(6) 0.2867(4) 0.08610(18) 0.0373(17) Uani 1 1 d . . . H6A H 0.3158 0.2503 0.1028 0.045 Uiso 1 1 calc R . . C1B C 0.4610(6) 0.4596(4) 0.14998(17) 0.0315(16) Uani 1 1 d . . . C2B C 0.3555(7) 0.4956(4) 0.1331(2) 0.047(2) Uani 1 1 d . . . H2B H 0.3104 0.4666 0.1151 0.057 Uiso 1 1 calc R . . C3B C 0.3155(8) 0.5702(5) 0.1416(2) 0.056(2) Uani 1 1 d . . . H3B H 0.2429 0.5916 0.1298 0.068 Uiso 1 1 calc R . . C4B C 0.3801(9) 0.6156(5) 0.1674(3) 0.066(3) Uani 1 1 d . . . H4B H 0.3540 0.6685 0.1728 0.080 Uiso 1 1 calc R . . C5B C 0.4838(8) 0.5818(5) 0.1852(2) 0.055(2) Uani 1 1 d . . . H5B H 0.5279 0.6114 0.2033 0.067 Uiso 1 1 calc R . . C6B C 0.5238(7) 0.5041(4) 0.17672(19) 0.0434(19) Uani 1 1 d . . . H6B H 0.5943 0.4816 0.1892 0.052 Uiso 1 1 calc R . . C1C C 0.5800(6) 0.3312(4) 0.25844(16) 0.0280(15) Uani 1 1 d . . . C2C C 0.5244(6) 0.4061(4) 0.25319(17) 0.0346(17) Uani 1 1 d . . . H2C H 0.4727 0.4155 0.2325 0.042 Uiso 1 1 calc R . . C3C C 0.5434(7) 0.4682(4) 0.27800(19) 0.0447(19) Uani 1 1 d . . . H3C H 0.5069 0.5196 0.2739 0.054 Uiso 1 1 calc R . . C4C C 0.6164(8) 0.4533(5) 0.3087(2) 0.052(2) Uani 1 1 d . . . H4C H 0.6293 0.4945 0.3258 0.062 Uiso 1 1 calc R . . C5C C 0.6703(7) 0.3781(5) 0.31438(19) 0.049(2) Uani 1 1 d . . . H5C H 0.7192 0.3682 0.3355 0.059 Uiso 1 1 calc R . . C6C C 0.6537(7) 0.3168(4) 0.28939(18) 0.0403(18) Uani 1 1 d . . . H6C H 0.6920 0.2659 0.2934 0.048 Uiso 1 1 calc R . . C1D C 0.5503(6) 0.1613(4) 0.24966(17) 0.0320(16) Uani 1 1 d . . . C2D C 0.6413(7) 0.1008(4) 0.25176(19) 0.0445(19) Uani 1 1 d . . . H2D H 0.7151 0.1083 0.2401 0.053 Uiso 1 1 calc R . . C3D C 0.6256(8) 0.0296(4) 0.2707(2) 0.053(2) Uani 1 1 d . . . H3D H 0.6883 -0.0104 0.2715 0.063 Uiso 1 1 calc R . . C4D C 0.5194(8) 0.0172(5) 0.2882(2) 0.053(2) Uani 1 1 d . . . H4D H 0.5080 -0.0316 0.3005 0.064 Uiso 1 1 calc R . . C5D C 0.4302(7) 0.0765(5) 0.2875(2) 0.048(2) Uani 1 1 d . . . H5D H 0.3578 0.0689 0.2998 0.058 Uiso 1 1 calc R . . C6D C 0.4458(6) 0.1486(4) 0.26863(18) 0.0414(18) Uani 1 1 d . . . H6D H 0.3842 0.1892 0.2688 0.050 Uiso 1 1 calc R . . P3 P 0.01192(18) 0.04310(12) 0.09138(5) 0.0382(5) Uani 1 1 d . . . F1 F 0.0833(5) 0.0415(4) 0.12890(13) 0.0930(18) Uani 1 1 d . . . F2 F 0.1071(5) -0.0166(4) 0.07576(16) 0.0983(19) Uani 1 1 d . . . F3 F -0.0600(5) 0.0451(3) 0.05348(12) 0.0802(16) Uani 1 1 d . . . F4 F -0.0885(5) 0.1009(3) 0.10658(16) 0.0945(18) Uani 1 1 d . . . F5 F 0.0950(6) 0.1166(4) 0.08162(16) 0.121(2) Uani 1 1 d . . . F6 F -0.0717(5) -0.0313(3) 0.10101(13) 0.0797(16) Uani 1 1 d . . . O1S O 0.2908(7) 0.8081(4) 0.19011(15) 0.0745(18) Uani 1 1 d D . . C1S C 0.2196(8) 0.8770(5) 0.1767(2) 0.072(3) Uani 1 1 d D . . H1S1 H 0.1338 0.8746 0.1840 0.086 Uiso 1 1 calc R . . H1S2 H 0.2171 0.8788 0.1508 0.086 Uiso 1 1 calc R . . C2S C 0.2896(9) 0.9530(5) 0.1931(2) 0.083(3) Uani 1 1 d D . . H2S1 H 0.2871 0.9983 0.1763 0.100 Uiso 1 1 calc R . . H2S2 H 0.2527 0.9706 0.2148 0.100 Uiso 1 1 calc R . . C3S C 0.4262(10) 0.9221(6) 0.2012(3) 0.107(4) Uani 1 1 d D . . H3S1 H 0.4832 0.9489 0.1857 0.128 Uiso 1 1 calc R . . H3S2 H 0.4545 0.9333 0.2259 0.128 Uiso 1 1 calc R . . C4S C 0.4228(9) 0.8314(7) 0.1943(3) 0.107(4) Uani 1 1 d D . . H4S1 H 0.4648 0.8184 0.1729 0.129 Uiso 1 1 calc R . . H4S2 H 0.4649 0.8021 0.2143 0.129 Uiso 1 1 calc R . . O2S O 0.1000(14) 0.6349(13) 0.0311(4) 0.244(8) Uani 1 1 d D . . C5S C 0.0691(17) 0.6671(9) -0.0025(6) 0.173(9) Uani 1 1 d D . . H5S1 H 0.1023 0.7223 -0.0044 0.207 Uiso 1 1 calc R . . H5S2 H -0.0219 0.6688 -0.0073 0.207 Uiso 1 1 calc R . . C6S C 0.130(2) 0.6088(10) -0.0289(3) 0.176(8) Uani 1 1 d D . . H6S1 H 0.0658 0.5781 -0.0429 0.211 Uiso 1 1 calc R . . H6S2 H 0.1802 0.6394 -0.0450 0.211 Uiso 1 1 calc R . . C8S C 0.1829(19) 0.5643(12) 0.0327(5) 0.246(13) Uani 1 1 d D . . H8S1 H 0.1410 0.5164 0.0418 0.295 Uiso 1 1 calc R . . H8S2 H 0.2593 0.5751 0.0477 0.295 Uiso 1 1 calc R . . C7S C 0.2115(14) 0.5525(10) -0.0057(5) 0.173(7) Uani 1 1 d D . . H7S1 H 0.2998 0.5644 -0.0086 0.208 Uiso 1 1 calc R . . H7S2 H 0.1953 0.4960 -0.0128 0.208 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 Re1 0.03686(17) 0.02414(16) 0.02723(15) 0.00017(12) 0.00269(12) -0.00254(13) Ru1 0.0182(3) 0.0252(3) 0.0302(3) -0.0022(2) 0.0028(2) 0.0007(2) Fe1 0.0221(5) 0.0313(6) 0.0375(6) -0.0013(4) 0.0070(4) -0.0007(4) P1 0.0277(10) 0.0255(10) 0.0313(10) 0.0005(7) 0.0023(8) 0.0018(7) P2 0.0207(9) 0.0257(10) 0.0290(9) -0.0013(7) 0.0019(7) 0.0000(7) O1 0.048(4) 0.056(4) 0.055(3) 0.013(3) 0.011(3) -0.008(3) O2 0.082(4) 0.025(3) 0.049(3) -0.003(2) 0.007(3) -0.005(3) O3 0.050(3) 0.062(4) 0.037(3) 0.010(3) -0.004(3) -0.003(3) N1 0.028(3) 0.028(3) 0.028(3) 0.000(2) 0.002(3) 0.000(3) N2 0.044(4) 0.028(3) 0.031(3) -0.003(2) -0.003(3) -0.005(3) N3 0.043(4) 0.026(3) 0.028(3) -0.006(2) 0.011(3) -0.001(3) N4 0.045(4) 0.035(4) 0.045(4) -0.002(3) 0.003(3) 0.001(3) C1 0.022(4) 0.036(5) 0.053(5) -0.002(3) 0.012(3) -0.001(3) C2 0.024(4) 0.039(4) 0.045(4) -0.007(3) 0.010(3) 0.000(3) C3 0.019(4) 0.036(4) 0.054(5) -0.008(4) 0.004(3) 0.010(3) C4 0.020(4) 0.057(5) 0.051(5) 0.013(4) 0.003(3) 0.006(3) C5 0.023(4) 0.050(5) 0.049(5) -0.013(4) 0.004(3) -0.006(3) C6 0.021(4) 0.025(4) 0.040(4) 0.005(3) 0.000(3) -0.005(3) C7 0.022(4) 0.028(4) 0.037(4) -0.001(3) -0.004(3) 0.002(3) C8 0.030(4) 0.026(4) 0.041(4) 0.004(3) 0.009(3) 0.000(3) C9 0.024(4) 0.028(4) 0.036(4) -0.003(3) -0.004(3) 0.001(3) C10 0.031(4) 0.026(4) 0.028(4) 0.002(3) 0.002(3) 0.000(3) C11 0.037(4) 0.031(4) 0.040(4) -0.004(3) 0.007(3) 0.005(3) C12 0.026(4) 0.038(4) 0.040(4) -0.001(3) 0.002(3) -0.007(3) C13 0.044(5) 0.053(5) 0.047(5) 0.005(4) -0.006(4) -0.013(4) C14 0.054(6) 0.073(6) 0.053(5) 0.023(5) -0.014(5) -0.009(5) C15 0.061(7) 0.095(8) 0.055(6) 0.032(5) -0.006(5) 0.000(5) C16 0.059(6) 0.063(6) 0.046(5) 0.024(4) 0.003(4) -0.003(4) C17 0.046(5) 0.039(4) 0.027(4) 0.009(3) 0.000(3) 0.003(3) C18 0.052(5) 0.034(4) 0.034(4) -0.001(3) 0.011(4) -0.003(4) C19 0.058(6) 0.041(5) 0.035(4) 0.007(3) 0.012(4) -0.009(4) C20 0.060(6) 0.042(5) 0.050(5) 0.001(4) 0.021(4) -0.013(4) C21 0.048(5) 0.040(5) 0.051(5) -0.004(4) 0.009(4) -0.002(4) C22 0.042(5) 0.027(4) 0.033(4) -0.005(3) 0.009(3) -0.007(3) C23 0.034(4) 0.039(4) 0.041(4) 0.001(3) 0.013(3) 0.003(3) C24 0.040(5) 0.044(5) 0.052(5) -0.008(4) 0.001(4) -0.002(4) C25 0.054(6) 0.080(7) 0.053(6) 0.007(5) -0.011(4) 0.012(5) C26 0.065(6) 0.054(6) 0.063(6) 0.015(5) 0.000(5) 0.013(5) C27 0.064(6) 0.047(5) 0.061(6) -0.002(4) 0.005(5) 0.003(4) C28 0.045(5) 0.033(5) 0.032(4) 0.000(3) -0.003(3) -0.002(3) C29 0.046(5) 0.033(4) 0.031(4) 0.000(3) -0.001(3) -0.004(3) C30 0.054(5) 0.025(4) 0.042(5) -0.004(3) 0.008(4) -0.008(4) C31 0.028(4) 0.029(4) 0.023(4) 0.003(3) 0.006(3) -0.001(3) C32 0.041(5) 0.039(5) 0.032(4) 0.000(3) 0.005(3) 0.004(3) C33 0.036(4) 0.043(5) 0.044(4) 0.005(4) 0.022(4) 0.007(4) C34 0.041(5) 0.038(5) 0.044(4) 0.011(3) 0.025(4) -0.001(3) C35 0.038(4) 0.027(4) 0.047(5) 0.006(3) 0.010(4) -0.002(3) C36 0.028(4) 0.027(4) 0.032(4) -0.003(3) 0.004(3) 0.004(3) C37 0.022(4) 0.035(4) 0.038(4) -0.005(3) -0.002(3) -0.003(3) C38 0.016(4) 0.049(5) 0.052(5) -0.003(4) 0.002(3) 0.003(3) C39 0.020(4) 0.041(4) 0.047(4) 0.002(3) 0.008(3) 0.009(3) C40 0.024(4) 0.031(4) 0.045(4) 0.001(3) 0.007(3) 0.001(3) C1A 0.033(4) 0.032(4) 0.031(4) -0.004(3) 0.002(3) 0.003(3) C2A 0.051(5) 0.040(5) 0.039(5) -0.003(3) 0.001(4) 0.000(4) C3A 0.073(6) 0.046(5) 0.034(5) 0.007(4) 0.006(4) 0.005(4) C4A 0.069(6) 0.052(5) 0.035(5) -0.012(4) -0.008(4) 0.003(4) C5A 0.046(5) 0.045(5) 0.041(5) -0.009(4) 0.001(4) -0.001(4) C6A 0.041(4) 0.039(4) 0.032(4) -0.003(3) -0.001(3) 0.002(3) C1B 0.031(4) 0.027(4) 0.038(4) 0.004(3) 0.014(3) 0.004(3) C2B 0.047(5) 0.042(5) 0.053(5) 0.011(4) 0.010(4) 0.004(4) C3B 0.058(6) 0.034(5) 0.079(7) 0.011(4) 0.020(5) 0.020(4) C4B 0.086(8) 0.034(5) 0.083(7) 0.006(5) 0.040(6) 0.014(5) C5B 0.071(6) 0.037(5) 0.062(6) -0.012(4) 0.028(5) -0.012(4) C6B 0.054(5) 0.035(5) 0.042(5) -0.003(3) 0.012(4) -0.005(4) C1C 0.027(4) 0.027(4) 0.031(4) -0.004(3) 0.007(3) -0.003(3) C2C 0.036(4) 0.036(4) 0.031(4) -0.004(3) 0.001(3) -0.004(3) C3C 0.056(5) 0.032(4) 0.047(5) -0.014(3) 0.004(4) 0.002(4) C4C 0.069(6) 0.049(5) 0.038(5) -0.021(4) 0.014(4) -0.008(4) C5C 0.053(5) 0.061(6) 0.032(4) -0.009(4) -0.010(4) -0.002(4) C6C 0.045(5) 0.037(4) 0.038(4) -0.006(3) -0.002(4) 0.000(3) C1D 0.035(4) 0.026(4) 0.035(4) 0.005(3) -0.001(3) -0.006(3) C2D 0.045(5) 0.037(5) 0.050(5) 0.009(4) -0.003(4) 0.009(4) C3D 0.066(6) 0.034(5) 0.058(5) 0.015(4) 0.004(5) 0.013(4) C4D 0.064(6) 0.051(6) 0.044(5) 0.017(4) 0.000(4) -0.015(5) C5D 0.043(5) 0.053(5) 0.050(5) 0.011(4) 0.007(4) -0.011(4) C6D 0.034(4) 0.049(5) 0.042(4) 0.011(4) 0.007(4) 0.005(4) P3 0.0328(11) 0.0428(12) 0.0388(11) -0.0026(9) 0.0008(9) -0.0057(9) F1 0.083(4) 0.137(5) 0.055(3) -0.003(3) -0.021(3) -0.002(3) F2 0.045(3) 0.127(5) 0.122(5) -0.049(4) 0.003(3) 0.020(3) F3 0.083(4) 0.103(4) 0.052(3) 0.008(3) -0.018(3) 0.003(3) F4 0.074(4) 0.084(4) 0.125(5) -0.042(3) 0.000(3) 0.022(3) F5 0.151(6) 0.108(5) 0.108(5) -0.003(4) 0.036(4) -0.083(4) F6 0.094(4) 0.067(3) 0.081(4) -0.002(3) 0.027(3) -0.030(3) O1S 0.101(6) 0.060(4) 0.064(4) -0.009(3) 0.014(4) 0.008(4) C1S 0.079(7) 0.072(7) 0.066(6) -0.008(5) 0.013(5) 0.012(6) C2S 0.110(10) 0.079(8) 0.061(6) -0.002(5) 0.015(6) -0.001(7) C3S 0.111(11) 0.096(10) 0.108(10) 0.005(7) -0.030(8) -0.011(8) C4S 0.093(10) 0.114(11) 0.115(10) -0.013(8) 0.007(8) 0.028(8) O2S 0.162(14) 0.32(2) 0.247(18) -0.114(16) 0.022(13) 0.036(14) C5S 0.158(17) 0.098(12) 0.27(3) 0.076(16) 0.087(19) 0.022(11) C6S 0.29(3) 0.133(14) 0.109(13) 0.009(11) 0.041(15) 0.002(15) C8S 0.114(17) 0.31(3) 0.32(3) -0.13(3) 0.027(19) 0.006(17) C7S 0.134(15) 0.171(17) 0.22(2) 0.034(16) 0.042(15) 0.035(12) _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 Re1 C29 1.890(8) . ? Re1 C30 1.923(8) . ? Re1 C28 1.927(7) . ? Re1 N2 2.151(5) . ? Re1 N1 2.202(5) . ? Re1 N3 2.208(5) . ? Ru1 C6 1.964(7) . ? Ru1 C5 2.223(7) . ? Ru1 C1 2.226(6) . ? Ru1 C4 2.226(7) . ? Ru1 C2 2.239(6) . ? Ru1 C3 2.252(6) . ? Ru1 P1 2.2805(17) . ? Ru1 P2 2.2814(17) . ? Fe1 C40 2.007(6) . ? Fe1 C33 2.019(6) . ? Fe1 C32 2.021(7) . ? Fe1 C31 2.026(6) . ? Fe1 C36 2.031(6) . ? Fe1 C39 2.043(7) . ? Fe1 C34 2.049(6) . ? Fe1 C35 2.058(6) . ? Fe1 C38 2.060(7) . ? Fe1 C37 2.060(6) . ? P1 C31 1.822(6) . ? P1 C1B 1.833(6) . ? P1 C1A 1.845(7) . ? P2 C36 1.821(6) . ? P2 C1D 1.839(6) . ? P2 C1C 1.842(6) . ? O1 C29 1.168(8) . ? O2 C28 1.149(7) . ? O3 C30 1.153(8) . ? N1 C12 1.354(8) . ? N1 C8 1.354(8) . ? N2 C13 1.343(9) . ? N2 C17 1.352(8) . ? N3 C22 1.357(8) . ? N3 C18 1.371(8) . ? N4 C27 1.341(9) . ? N4 C23 1.345(8) . ? C1 C5 1.407(10) . ? C1 C2 1.417(9) . ? C2 C3 1.416(9) . ? C3 C4 1.438(10) . ? C4 C5 1.398(9) . ? C6 C7 1.220(8) . ? C7 C10 1.421(9) . ? C8 C9 1.372(8) . ? C9 C10 1.397(8) . ? C10 C11 1.401(9) . ? C11 C12 1.355(9) . ? C13 C14 1.368(10) . ? C14 C15 1.352(10) . ? C15 C16 1.370(11) . ? C16 C17 1.383(9) . ? C17 C18 1.473(10) . ? C18 C19 1.381(9) . ? C19 C20 1.379(10) . ? C20 C21 1.382(10) . ? C21 C22 1.404(9) . ? C22 C23 1.489(10) . ? C23 C24 1.382(10) . ? C24 C25 1.389(10) . ? C25 C26 1.370(11) . ? C26 C27 1.367(11) . ? C31 C32 1.431(8) . ? C31 C35 1.437(9) . ? C32 C33 1.415(9) . ? C33 C34 1.394(10) . ? C34 C35 1.413(9) . ? C36 C37 1.421(9) . ? C36 C40 1.428(8) . ? C37 C38 1.415(9) . ? C38 C39 1.437(9) . ? C39 C40 1.416(9) . ? C1A C6A 1.376(9) . ? C1A C2A 1.393(9) . ? C2A C3A 1.368(10) . ? C3A C4A 1.395(10) . ? C4A C5A 1.357(10) . ? C5A C6A 1.395(9) . ? C1B C6B 1.387(9) . ? C1B C2B 1.392(9) . ? C2B C3B 1.347(10) . ? C3B C4B 1.379(12) . ? C4B C5B 1.378(12) . ? C5B C6B 1.393(10) . ? C1C C2C 1.378(9) . ? C1C C6C 1.388(9) . ? C2C C3C 1.394(9) . ? C3C C4C 1.378(10) . ? C4C C5C 1.377(10) . ? C5C C6C 1.386(9) . ? C1D C6D 1.387(9) . ? C1D C2D 1.392(9) . ? C2D C3D 1.390(9) . ? C3D C4D 1.370(10) . ? C4D C5D 1.366(10) . ? C5D C6D 1.400(9) . ? P3 F5 1.561(5) . ? P3 F2 1.562(5) . ? P3 F1 1.568(5) . ? P3 F4 1.574(5) . ? P3 F6 1.575(5) . ? P3 F3 1.582(5) . ? O1S C1S 1.441(9) . ? O1S C4S 1.464(10) . ? C1S C2S 1.565(10) . ? C2S C3S 1.562(11) . ? C3S C4S 1.515(11) . ? O2S C5S 1.397(13) . ? O2S C8S 1.462(14) . ? C5S C6S 1.560(14) . ? C6S C7S 1.512(14) . ? C8S C7S 1.521(14) . ? 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 C29 Re1 C30 89.3(3) . . ? C29 Re1 C28 89.8(3) . . ? C30 Re1 C28 88.5(3) . . ? C29 Re1 N2 93.5(3) . . ? C30 Re1 N2 173.5(2) . . ? C28 Re1 N2 97.4(2) . . ? C29 Re1 N1 90.0(2) . . ? C30 Re1 N1 90.7(2) . . ? C28 Re1 N1 179.2(2) . . ? N2 Re1 N1 83.42(19) . . ? C29 Re1 N3 166.9(3) . . ? C30 Re1 N3 101.6(3) . . ? C28 Re1 N3 97.8(2) . . ? N2 Re1 N3 75.0(2) . . ? N1 Re1 N3 82.56(18) . . ? C6 Ru1 C5 91.3(3) . . ? C6 Ru1 C1 101.1(2) . . ? C5 Ru1 C1 36.9(2) . . ? C6 Ru1 C4 116.7(3) . . ? C5 Ru1 C4 36.6(2) . . ? C1 Ru1 C4 61.2(3) . . ? C6 Ru1 C2 136.4(2) . . ? C5 Ru1 C2 61.9(2) . . ? C1 Ru1 C2 37.0(2) . . ? C4 Ru1 C2 61.7(3) . . ? C6 Ru1 C3 152.7(3) . . ? C5 Ru1 C3 62.0(2) . . ? C1 Ru1 C3 61.6(2) . . ? C4 Ru1 C3 37.5(2) . . ? C2 Ru1 C3 36.8(2) . . ? C6 Ru1 P1 87.71(18) . . ? C5 Ru1 P1 119.2(2) . . ? C1 Ru1 P1 153.73(19) . . ? C4 Ru1 P1 92.65(19) . . ? C2 Ru1 P1 134.60(18) . . ? C3 Ru1 P1 100.06(19) . . ? C6 Ru1 P2 87.92(19) . . ? C5 Ru1 P2 141.8(2) . . ? C1 Ru1 P2 106.0(2) . . ? C4 Ru1 P2 153.2(2) . . ? C2 Ru1 P2 93.65(19) . . ? C3 Ru1 P2 116.22(19) . . ? P1 Ru1 P2 98.92(6) . . ? C40 Fe1 C33 118.4(3) . . ? C40 Fe1 C32 102.4(3) . . ? C33 Fe1 C32 41.0(3) . . ? C40 Fe1 C31 119.8(3) . . ? C33 Fe1 C31 69.3(3) . . ? C32 Fe1 C31 41.4(2) . . ? C40 Fe1 C36 41.4(2) . . ? C33 Fe1 C36 156.6(3) . . ? C32 Fe1 C36 121.5(3) . . ? C31 Fe1 C36 107.9(2) . . ? C40 Fe1 C39 40.9(2) . . ? C33 Fe1 C39 103.2(3) . . ? C32 Fe1 C39 117.2(3) . . ? C31 Fe1 C39 154.5(3) . . ? C36 Fe1 C39 68.8(2) . . ? C40 Fe1 C34 155.6(3) . . ? C33 Fe1 C34 40.1(3) . . ? C32 Fe1 C34 68.3(3) . . ? C31 Fe1 C34 68.9(3) . . ? C36 Fe1 C34 162.4(3) . . ? C39 Fe1 C34 121.8(3) . . ? C40 Fe1 C35 159.1(3) . . ? C33 Fe1 C35 68.0(3) . . ? C32 Fe1 C35 68.7(3) . . ? C31 Fe1 C35 41.2(2) . . ? C36 Fe1 C35 126.1(3) . . ? C39 Fe1 C35 160.0(3) . . ? C34 Fe1 C35 40.2(2) . . ? C40 Fe1 C38 69.1(3) . . ? C33 Fe1 C38 120.7(3) . . ? C32 Fe1 C38 154.7(3) . . ? C31 Fe1 C38 163.3(3) . . ? C36 Fe1 C38 68.5(3) . . ? C39 Fe1 C38 41.0(3) . . ? C34 Fe1 C38 109.2(3) . . ? C35 Fe1 C38 126.8(3) . . ? C40 Fe1 C37 68.9(3) . . ? C33 Fe1 C37 158.5(3) . . ? C32 Fe1 C37 160.5(3) . . ? C31 Fe1 C37 126.7(2) . . ? C36 Fe1 C37 40.6(2) . . ? C39 Fe1 C37 68.3(3) . . ? C34 Fe1 C37 126.5(3) . . ? C35 Fe1 C37 113.1(3) . . ? C38 Fe1 C37 40.2(2) . . ? C31 P1 C1B 105.3(3) . . ? C31 P1 C1A 98.2(3) . . ? C1B P1 C1A 100.1(3) . . ? C31 P1 Ru1 124.3(2) . . ? C1B P1 Ru1 111.1(2) . . ? C1A P1 Ru1 114.6(2) . . ? C36 P2 C1D 101.3(3) . . ? C36 P2 C1C 100.8(3) . . ? C1D P2 C1C 100.5(3) . . ? C36 P2 Ru1 120.6(2) . . ? C1D P2 Ru1 113.5(2) . . ? C1C P2 Ru1 117.0(2) . . ? C12 N1 C8 116.0(5) . . ? C12 N1 Re1 121.1(4) . . ? C8 N1 Re1 121.8(4) . . ? C13 N2 C17 118.3(6) . . ? C13 N2 Re1 125.0(5) . . ? C17 N2 Re1 116.6(5) . . ? C22 N3 C18 117.7(6) . . ? C22 N3 Re1 127.6(4) . . ? C18 N3 Re1 113.9(5) . . ? C27 N4 C23 115.9(7) . . ? C5 C1 C2 108.6(6) . . ? C5 C1 Ru1 71.4(4) . . ? C2 C1 Ru1 72.0(4) . . ? C3 C2 C1 108.0(7) . . ? C3 C2 Ru1 72.1(4) . . ? C1 C2 Ru1 71.0(4) . . ? C2 C3 C4 106.6(6) . . ? C2 C3 Ru1 71.1(4) . . ? C4 C3 Ru1 70.3(4) . . ? C5 C4 C3 108.8(6) . . ? C5 C4 Ru1 71.5(4) . . ? C3 C4 Ru1 72.2(4) . . ? C4 C5 C1 107.9(6) . . ? C4 C5 Ru1 71.8(4) . . ? C1 C5 Ru1 71.7(4) . . ? C7 C6 Ru1 173.9(6) . . ? C6 C7 C10 170.4(7) . . ? N1 C8 C9 123.5(6) . . ? C8 C9 C10 119.9(6) . . ? C9 C10 C11 116.1(6) . . ? C9 C10 C7 123.4(6) . . ? C11 C10 C7 120.5(6) . . ? C12 C11 C10 120.6(6) . . ? N1 C12 C11 123.6(6) . . ? N2 C13 C14 122.6(7) . . ? C15 C14 C13 119.7(8) . . ? C14 C15 C16 118.6(8) . . ? C15 C16 C17 120.5(7) . . ? N2 C17 C16 120.3(7) . . ? N2 C17 C18 116.1(6) . . ? C16 C17 C18 123.6(7) . . ? N3 C18 C19 122.0(7) . . ? N3 C18 C17 115.2(6) . . ? C19 C18 C17 122.8(7) . . ? C20 C19 C18 119.6(7) . . ? C19 C20 C21 119.6(7) . . ? C20 C21 C22 118.6(7) . . ? N3 C22 C21 122.2(6) . . ? N3 C22 C23 119.7(6) . . ? C21 C22 C23 118.1(7) . . ? N4 C23 C24 124.1(7) . . ? N4 C23 C22 114.9(7) . . ? C24 C23 C22 120.9(7) . . ? C23 C24 C25 118.1(8) . . ? C26 C25 C24 118.4(8) . . ? C27 C26 C25 119.7(8) . . ? N4 C27 C26 123.8(8) . . ? O2 C28 Re1 177.2(6) . . ? O1 C29 Re1 176.1(6) . . ? O3 C30 Re1 176.8(6) . . ? C32 C31 C35 106.8(6) . . ? C32 C31 P1 121.6(5) . . ? C35 C31 P1 131.5(5) . . ? C32 C31 Fe1 69.1(4) . . ? C35 C31 Fe1 70.6(4) . . ? P1 C31 Fe1 128.0(3) . . ? C33 C32 C31 107.8(6) . . ? C33 C32 Fe1 69.4(4) . . ? C31 C32 Fe1 69.5(4) . . ? C34 C33 C32 108.8(6) . . ? C34 C33 Fe1 71.1(4) . . ? C32 C33 Fe1 69.6(4) . . ? C33 C34 C35 108.6(6) . . ? C33 C34 Fe1 68.8(4) . . ? C35 C34 Fe1 70.2(4) . . ? C34 C35 C31 108.0(6) . . ? C34 C35 Fe1 69.6(4) . . ? C31 C35 Fe1 68.2(4) . . ? C37 C36 C40 107.7(6) . . ? C37 C36 P2 126.2(5) . . ? C40 C36 P2 126.0(5) . . ? C37 C36 Fe1 70.8(4) . . ? C40 C36 Fe1 68.4(3) . . ? P2 C36 Fe1 129.7(3) . . ? C38 C37 C36 108.6(6) . . ? C38 C37 Fe1 69.9(4) . . ? C36 C37 Fe1 68.6(4) . . ? C37 C38 C39 107.6(6) . . ? C37 C38 Fe1 69.9(4) . . ? C39 C38 Fe1 68.9(4) . . ? C40 C39 C38 107.9(6) . . ? C40 C39 Fe1 68.2(4) . . ? C38 C39 Fe1 70.1(4) . . ? C39 C40 C36 108.1(6) . . ? C39 C40 Fe1 70.9(4) . . ? C36 C40 Fe1 70.2(4) . . ? C6A C1A C2A 118.8(7) . . ? C6A C1A P1 121.6(5) . . ? C2A C1A P1 119.5(5) . . ? C3A C2A C1A 121.3(7) . . ? C2A C3A C4A 118.9(7) . . ? C5A C4A C3A 120.8(7) . . ? C4A C5A C6A 119.9(7) . . ? C1A C6A C5A 120.3(7) . . ? C6B C1B C2B 116.7(7) . . ? C6B C1B P1 121.3(6) . . ? C2B C1B P1 121.1(6) . . ? C3B C2B C1B 122.8(8) . . ? C2B C3B C4B 120.7(9) . . ? C5B C4B C3B 118.5(8) . . ? C4B C5B C6B 120.6(8) . . ? C1B C6B C5B 120.7(8) . . ? C2C C1C C6C 119.3(6) . . ? C2C C1C P2 119.2(5) . . ? C6C C1C P2 121.4(5) . . ? C1C C2C C3C 121.1(7) . . ? C4C C3C C2C 119.1(7) . . ? C5C C4C C3C 120.0(7) . . ? C4C C5C C6C 120.9(7) . . ? C5C C6C C1C 119.5(7) . . ? C6D C1D C2D 116.8(6) . . ? C6D C1D P2 119.8(5) . . ? C2D C1D P2 123.4(5) . . ? C3D C2D C1D 121.5(7) . . ? C4D C3D C2D 120.6(7) . . ? C5D C4D C3D 119.2(7) . . ? C4D C5D C6D 120.5(7) . . ? C1D C6D C5D 121.3(7) . . ? F5 P3 F2 90.0(4) . . ? F5 P3 F1 88.6(3) . . ? F2 P3 F1 92.3(3) . . ? F5 P3 F4 92.0(4) . . ? F2 P3 F4 177.6(3) . . ? F1 P3 F4 89.0(3) . . ? F5 P3 F6 179.7(3) . . ? F2 P3 F6 89.8(3) . . ? F1 P3 F6 91.6(3) . . ? F4 P3 F6 88.3(3) . . ? F5 P3 F3 91.2(3) . . ? F2 P3 F3 87.7(3) . . ? F1 P3 F3 179.8(3) . . ? F4 P3 F3 90.9(3) . . ? F6 P3 F3 88.6(3) . . ? C1S O1S C4S 108.5(6) . . ? O1S C1S C2S 105.1(7) . . ? C3S C2S C1S 103.6(6) . . ? C4S C3S C2S 106.0(7) . . ? O1S C4S C3S 106.8(7) . . ? C5S O2S C8S 116.5(10) . . ? O2S C5S C6S 105.4(9) . . ? C7S C6S C5S 104.8(9) . . ? O2S C8S C7S 102.9(10) . . ? C6S C7S C8S 109.3(9) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.087 _refine_diff_density_min -0.533 _refine_diff_density_rms 0.120 #===end data_7316 _database_code_depnum_ccdc_archive 'CCDC 721193' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H11 Br N3 O3 Re' _chemical_formula_weight 583.41 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 31.1691(16) _cell_length_b 7.1260(4) _cell_length_c 16.8518(8) _cell_angle_alpha 90.00 _cell_angle_beta 110.967(2) _cell_angle_gamma 90.00 _cell_volume 3495.1(3) _cell_formula_units_Z 8 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 6806 _cell_measurement_theta_min 2.46 _cell_measurement_theta_max 27.43 _exptl_crystal_description Yellow _exptl_crystal_colour Block _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.217 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2192 _exptl_absorpt_coefficient_mu 9.263 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.1968 _exptl_absorpt_correction_T_max 0.4577 _exptl_absorpt_process_details 'Sadabs, (Sheldrick 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11888 _diffrn_reflns_av_R_equivalents 0.0225 _diffrn_reflns_av_sigmaI/netI 0.0258 _diffrn_reflns_limit_h_min -40 _diffrn_reflns_limit_h_max 40 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.46 _diffrn_reflns_theta_max 27.47 _reflns_number_total 3994 _reflns_number_gt 3613 _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, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0185P)^2^+1.5520P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3994 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0204 _refine_ls_R_factor_gt 0.0177 _refine_ls_wR_factor_ref 0.0423 _refine_ls_wR_factor_gt 0.0415 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.003 _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 Re1 Re 0.902943(3) 0.392793(14) 0.805437(6) 0.02686(4) Uani 1 1 d . . . Br1 Br 0.846729(9) 0.67882(4) 0.745780(17) 0.03602(7) Uani 1 1 d . . . N1 N 0.86473(7) 0.3449(3) 0.88911(13) 0.0287(4) Uani 1 1 d . . . N2 N 0.84108(7) 0.2300(3) 0.72802(13) 0.0306(5) Uani 1 1 d . . . N3 N 0.85655(8) 0.1906(3) 0.53050(14) 0.0381(5) Uani 1 1 d . . . O1 O 0.96461(8) 0.0551(3) 0.87473(14) 0.0513(6) Uani 1 1 d . . . O2 O 0.94989(7) 0.4626(3) 0.67584(13) 0.0494(5) Uani 1 1 d . . . O3 O 0.97883(8) 0.6419(3) 0.92465(15) 0.0541(6) Uani 1 1 d . . . C1 C 0.88078(11) 0.3810(4) 0.97337(17) 0.0346(6) Uani 1 1 d . . . H1 H 0.9105 0.4311 0.9988 0.041 Uiso 1 1 calc R . . C2 C 0.85483(11) 0.3463(4) 1.02313(18) 0.0394(7) Uani 1 1 d . . . H2 H 0.8666 0.3747 1.0815 0.047 Uiso 1 1 calc R . . C3 C 0.81219(10) 0.2711(4) 0.98743(18) 0.0409(7) Uani 1 1 d . . . H3 H 0.7945 0.2452 1.0210 0.049 Uiso 1 1 calc R . . C4 C 0.79496(10) 0.2327(4) 0.90103(18) 0.0387(6) Uani 1 1 d . . . H4 H 0.7656 0.1800 0.8752 0.046 Uiso 1 1 calc R . . C5 C 0.82231(9) 0.2741(4) 0.85328(16) 0.0309(5) Uani 1 1 d . . . C6 C 0.80718(9) 0.2349(4) 0.76135(16) 0.0317(5) Uani 1 1 d . . . C7 C 0.76157(9) 0.2082(4) 0.71264(18) 0.0384(6) Uani 1 1 d . . . H7 H 0.7391 0.2152 0.7377 0.046 Uiso 1 1 calc R . . C8 C 0.74888(10) 0.1711(4) 0.62664(18) 0.0405(6) Uani 1 1 d . . . H8 H 0.7178 0.1618 0.5914 0.049 Uiso 1 1 calc R . . C9 C 0.78369(10) 0.1483(4) 0.59464(18) 0.0376(6) Uani 1 1 d . . . H9 H 0.7763 0.1140 0.5374 0.045 Uiso 1 1 calc R . . C10 C 0.82946(10) 0.1753(4) 0.64605(16) 0.0320(5) Uani 1 1 d . . . C13 C 0.86565(10) 0.1332(4) 0.61096(16) 0.0317(6) Uani 1 1 d . . . C14 C 0.90384(9) 0.0272(4) 0.65657(17) 0.0345(6) Uani 1 1 d . . . H14 H 0.9079 -0.0162 0.7115 0.041 Uiso 1 1 calc R . . C15 C 0.93582(10) -0.0133(4) 0.61923(19) 0.0427(7) Uani 1 1 d . . . H15 H 0.9624 -0.0826 0.6487 0.051 Uiso 1 1 calc R . . C16 C 0.92772(11) 0.0506(5) 0.5377(2) 0.0469(7) Uani 1 1 d . . . H16 H 0.9491 0.0279 0.5112 0.056 Uiso 1 1 calc R . . C17 C 0.88827(12) 0.1471(5) 0.49606(19) 0.0458(8) Uani 1 1 d . . . H17 H 0.8828 0.1857 0.4400 0.055 Uiso 1 1 calc R . . C18 C 0.94130(9) 0.1837(4) 0.84866(16) 0.0340(6) Uani 1 1 d . . . C19 C 0.93194(10) 0.4339(4) 0.72366(17) 0.0347(6) Uani 1 1 d . . . C20 C 0.95005(10) 0.5498(4) 0.87971(17) 0.0351(6) 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 Re1 0.02210(6) 0.03645(7) 0.02289(6) 0.00221(4) 0.00909(4) 0.00025(4) Br1 0.03279(15) 0.04177(15) 0.03730(15) 0.00931(12) 0.01719(12) 0.00614(11) N1 0.0295(12) 0.0348(11) 0.0233(10) 0.0048(9) 0.0112(9) 0.0021(9) N2 0.0265(11) 0.0403(12) 0.0262(11) 0.0019(9) 0.0109(9) -0.0021(9) N3 0.0433(14) 0.0482(14) 0.0251(11) -0.0008(10) 0.0149(10) -0.0070(11) O1 0.0486(14) 0.0581(13) 0.0496(13) 0.0135(11) 0.0204(11) 0.0198(11) O2 0.0411(12) 0.0756(14) 0.0385(11) 0.0062(11) 0.0228(10) -0.0092(11) O3 0.0494(14) 0.0527(13) 0.0519(14) -0.0096(11) 0.0079(11) -0.0133(11) C1 0.0369(15) 0.0402(15) 0.0273(14) 0.0016(11) 0.0122(12) 0.0028(11) C2 0.0516(18) 0.0456(16) 0.0251(13) 0.0045(12) 0.0188(13) 0.0068(13) C3 0.0481(18) 0.0480(16) 0.0383(16) 0.0063(13) 0.0299(14) 0.0050(13) C4 0.0345(15) 0.0499(16) 0.0383(15) 0.0049(13) 0.0210(13) -0.0023(13) C5 0.0300(13) 0.0373(14) 0.0295(13) 0.0028(10) 0.0155(11) 0.0022(11) C6 0.0284(13) 0.0388(14) 0.0294(13) 0.0038(11) 0.0122(11) 0.0001(11) C7 0.0273(14) 0.0511(17) 0.0397(15) 0.0004(13) 0.0153(12) -0.0045(12) C8 0.0266(14) 0.0522(16) 0.0383(16) 0.0007(13) 0.0063(12) -0.0056(12) C9 0.0371(16) 0.0441(15) 0.0290(14) -0.0028(11) 0.0087(12) -0.0035(12) C10 0.0363(15) 0.0328(13) 0.0261(13) 0.0013(11) 0.0102(11) -0.0037(11) C13 0.0364(15) 0.0369(14) 0.0239(13) -0.0031(10) 0.0132(11) -0.0085(11) C14 0.0328(14) 0.0441(15) 0.0282(13) -0.0030(11) 0.0126(11) -0.0049(12) C15 0.0377(16) 0.0514(18) 0.0432(17) -0.0071(14) 0.0197(13) -0.0022(13) C16 0.0467(19) 0.0627(19) 0.0421(17) -0.0133(15) 0.0290(15) -0.0134(16) C17 0.054(2) 0.0619(19) 0.0279(15) -0.0070(13) 0.0223(14) -0.0154(16) C18 0.0299(14) 0.0454(15) 0.0283(13) 0.0015(12) 0.0125(11) 0.0014(12) C19 0.0279(14) 0.0448(15) 0.0288(14) 0.0035(11) 0.0068(11) -0.0031(11) C20 0.0326(15) 0.0415(14) 0.0319(14) 0.0041(12) 0.0124(12) 0.0011(12) _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 Re1 C18 1.886(3) . ? Re1 C20 1.913(3) . ? Re1 C19 1.922(3) . ? Re1 N1 2.174(2) . ? Re1 N2 2.228(2) . ? Re1 Br1 2.6409(3) . ? N1 C5 1.340(3) . ? N1 C1 1.351(3) . ? N2 C10 1.354(3) . ? N2 C6 1.363(3) . ? N3 C13 1.345(3) . ? N3 C17 1.349(4) . ? O1 C18 1.154(3) . ? O2 C19 1.152(3) . ? O3 C20 1.150(3) . ? C1 C2 1.380(4) . ? C2 C3 1.358(4) . ? C3 C4 1.387(4) . ? C4 C5 1.397(3) . ? C5 C6 1.476(3) . ? C6 C7 1.377(4) . ? C7 C8 1.384(4) . ? C8 C9 1.383(4) . ? C9 C10 1.392(4) . ? C10 C13 1.480(4) . ? C13 C14 1.387(4) . ? C14 C15 1.386(4) . ? C15 C16 1.383(4) . ? C16 C17 1.364(5) . ? 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 C18 Re1 C20 88.70(12) . . ? C18 Re1 C19 90.10(11) . . ? C20 Re1 C19 86.11(12) . . ? C18 Re1 N1 92.54(9) . . ? C20 Re1 N1 97.92(10) . . ? C19 Re1 N1 175.23(10) . . ? C18 Re1 N2 96.38(10) . . ? C20 Re1 N2 171.25(10) . . ? C19 Re1 N2 100.96(10) . . ? N1 Re1 N2 74.80(8) . . ? C18 Re1 Br1 177.89(8) . . ? C20 Re1 Br1 92.69(9) . . ? C19 Re1 Br1 91.57(8) . . ? N1 Re1 Br1 85.71(6) . . ? N2 Re1 Br1 82.05(6) . . ? C5 N1 C1 118.7(2) . . ? C5 N1 Re1 116.62(16) . . ? C1 N1 Re1 124.71(18) . . ? C10 N2 C6 117.6(2) . . ? C10 N2 Re1 127.35(17) . . ? C6 N2 Re1 112.43(17) . . ? C13 N3 C17 116.2(3) . . ? N1 C1 C2 121.9(3) . . ? C3 C2 C1 119.7(3) . . ? C2 C3 C4 119.5(2) . . ? C3 C4 C5 118.4(3) . . ? N1 C5 C4 121.8(2) . . ? N1 C5 C6 116.0(2) . . ? C4 C5 C6 122.2(2) . . ? N2 C6 C7 122.6(2) . . ? N2 C6 C5 115.7(2) . . ? C7 C6 C5 121.7(2) . . ? C6 C7 C8 119.9(2) . . ? C9 C8 C7 117.4(3) . . ? C8 C9 C10 120.9(3) . . ? N2 C10 C9 121.0(2) . . ? N2 C10 C13 120.1(2) . . ? C9 C10 C13 118.8(2) . . ? N3 C13 C14 123.6(2) . . ? N3 C13 C10 115.2(2) . . ? C14 C13 C10 121.0(2) . . ? C15 C14 C13 118.4(3) . . ? C16 C15 C14 118.5(3) . . ? C17 C16 C15 119.2(3) . . ? N3 C17 C16 124.0(3) . . ? O1 C18 Re1 179.6(3) . . ? O2 C19 Re1 178.2(3) . . ? O3 C20 Re1 178.9(3) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.595 _refine_diff_density_min -0.547 _refine_diff_density_rms 0.119 #===end data_7302 _database_code_depnum_ccdc_archive 'CCDC 721194' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H63 Cl2 F6 Fe N3 O3 P3 Re Ru' _chemical_formula_weight 1591.14 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' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.8417(3) _cell_length_b 10.4494(3) _cell_length_c 54.2177(16) _cell_angle_alpha 90.00 _cell_angle_beta 93.1280(10) _cell_angle_gamma 90.00 _cell_volume 6698.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.578 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3176 _exptl_absorpt_coefficient_mu 2.454 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.4891 _exptl_absorpt_correction_T_max 0.8278 _exptl_absorpt_process_details 'Sadabs, (Sheldrick 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38509 _diffrn_reflns_av_R_equivalents 0.0833 _diffrn_reflns_av_sigmaI/netI 0.0855 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -64 _diffrn_reflns_limit_l_max 64 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11798 _reflns_number_gt 10045 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0479P)^2^+20.0000P] 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_number_reflns 11798 _refine_ls_number_parameters 810 _refine_ls_number_restraints 97 _refine_ls_R_factor_all 0.1056 _refine_ls_R_factor_gt 0.0886 _refine_ls_wR_factor_ref 0.1796 _refine_ls_wR_factor_gt 0.1738 _refine_ls_goodness_of_fit_ref 1.446 _refine_ls_restrained_S_all 1.447 _refine_ls_shift/su_max 0.014 _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 0.12254(8) 1.08860(9) 0.071447(16) 0.0274(2) Uani 1 1 d . . . Re1 Re 0.03848(3) 0.68182(4) 0.228327(7) 0.01884(13) Uani 1 1 d . . . Fe1 Fe 0.45972(15) 0.93023(16) 0.08725(3) 0.0340(4) Uani 1 1 d . . . P1 P 0.2090(3) 0.9278(3) 0.05127(5) 0.0261(7) Uani 1 1 d . . . P2 P 0.2839(3) 1.1961(3) 0.08349(6) 0.0323(7) Uani 1 1 d . . . O1 O -0.1606(7) 0.8682(8) 0.23218(16) 0.037(2) Uani 1 1 d . . . O2 O 0.2024(7) 0.8677(8) 0.25542(15) 0.043(2) Uani 1 1 d . . . O3 O -0.0244(7) 0.5724(8) 0.27855(13) 0.035(2) Uani 1 1 d . . . N1 N 0.0730(8) 0.7633(8) 0.19213(17) 0.027(2) Uani 1 1 d . . . N2 N -0.0524(6) 0.5354(8) 0.20756(15) 0.0195(19) Uani 1 1 d . . . N3 N 0.1638(7) 0.5356(8) 0.22130(14) 0.0182(19) Uani 1 1 d . . . C1 C 0.0067(13) 1.2588(14) 0.0704(3) 0.052(4) Uani 1 1 d . . . H1 H 0.0214 1.3427 0.0784 0.063 Uiso 1 1 calc R . . C2 C 0.0280(12) 1.2249(13) 0.0458(3) 0.047(4) Uani 1 1 d . . . H2 H 0.0616 1.2810 0.0334 0.056 Uiso 1 1 calc R . . C3 C -0.0121(10) 1.1022(14) 0.0418(2) 0.045(4) Uani 1 1 d . . . H3 H -0.0113 1.0565 0.0258 0.053 Uiso 1 1 calc R . . C4 C -0.0600(11) 1.0545(16) 0.0627(3) 0.055(4) Uani 1 1 d . . . H4 H -0.1011 0.9726 0.0642 0.066 Uiso 1 1 calc R . . C5 C -0.0483(11) 1.1519(16) 0.0806(3) 0.056(4) Uani 1 1 d . . . H5 H -0.0787 1.1489 0.0973 0.067 Uiso 1 1 calc R . . C6 C 0.1359(10) 0.9930(11) 0.1037(2) 0.033(3) Uani 1 1 d . . . C7 C 0.1303(10) 0.9450(11) 0.1234(2) 0.031(3) Uani 1 1 d . . . C8 C -0.0099(10) 0.8099(13) 0.1765(2) 0.042(3) Uani 1 1 d . . . H8 H -0.0848 0.8017 0.1812 0.051 Uiso 1 1 calc R . . C9 C 0.0064(11) 0.8672(13) 0.1548(2) 0.040(3) Uani 1 1 d . . . H9 H -0.0566 0.8962 0.1451 0.048 Uiso 1 1 calc R . . C10 C 0.1134(10) 0.8846(11) 0.1464(2) 0.029(3) Uani 1 1 d . . . C11 C 0.2009(10) 0.8395(13) 0.1632(2) 0.037(3) Uani 1 1 d . . . H11 H 0.2767 0.8486 0.1592 0.044 Uiso 1 1 calc R . . C12 C 0.1774(10) 0.7848(11) 0.1844(2) 0.034(3) Uani 1 1 d . . . H12 H 0.2390 0.7590 0.1949 0.041 Uiso 1 1 calc R . . C13 C -0.1641(8) 0.5438(11) 0.20001(19) 0.023(2) Uani 1 1 d . . . H13 H -0.2049 0.6177 0.2039 0.028 Uiso 1 1 calc R . . C14 C -0.2194(9) 0.4458(11) 0.1867(2) 0.029(3) Uani 1 1 d . . . H14 H -0.2969 0.4532 0.1822 0.034 Uiso 1 1 calc R . . C15 C -0.1618(9) 0.3399(11) 0.1803(2) 0.027(3) Uani 1 1 d . . . C16 C -0.0480(9) 0.3318(10) 0.18820(19) 0.025(2) Uani 1 1 d . . . H16 H -0.0065 0.2586 0.1843 0.030 Uiso 1 1 calc R . . C17 C 0.0046(9) 0.4276(10) 0.20149(18) 0.019(2) Uani 1 1 d . . . C18 C 0.1237(9) 0.4274(10) 0.20950(19) 0.021(2) Uani 1 1 d . . . C19 C 0.1941(9) 0.3254(11) 0.2069(2) 0.027(2) Uani 1 1 d . . . H19 H 0.1648 0.2515 0.1990 0.032 Uiso 1 1 calc R . . C20 C 0.3078(9) 0.3255(11) 0.2154(2) 0.029(3) Uani 1 1 d . . . C21 C 0.3464(9) 0.4403(12) 0.2259(2) 0.031(3) Uani 1 1 d . . . H21 H 0.4231 0.4502 0.2309 0.038 Uiso 1 1 calc R . . C22 C 0.2723(9) 0.5380(11) 0.2287(2) 0.030(3) Uani 1 1 d . . . H22 H 0.3002 0.6127 0.2366 0.036 Uiso 1 1 calc R . . C23 C -0.2185(9) 0.2283(12) 0.1658(2) 0.035(3) Uani 1 1 d . . . C24 C -0.1498(11) 0.1950(14) 0.1434(2) 0.050(4) Uani 1 1 d . . . H24A H -0.0754 0.1649 0.1491 0.075 Uiso 1 1 calc R . . H24B H -0.1422 0.2707 0.1333 0.075 Uiso 1 1 calc R . . H24C H -0.1886 0.1286 0.1337 0.075 Uiso 1 1 calc R . . C25 C -0.3412(11) 0.2656(15) 0.1567(3) 0.061(4) Uani 1 1 d . . . H25A H -0.3781 0.1925 0.1487 0.091 Uiso 1 1 calc R . . H25B H -0.3385 0.3356 0.1450 0.091 Uiso 1 1 calc R . . H25C H -0.3833 0.2921 0.1707 0.091 Uiso 1 1 calc R . . C26 C -0.2259(13) 0.1145(14) 0.1828(3) 0.057(4) Uani 1 1 d . . . H26A H -0.1504 0.0838 0.1874 0.085 Uiso 1 1 calc R . . H26B H -0.2690 0.0470 0.1744 0.085 Uiso 1 1 calc R . . H26C H -0.2633 0.1397 0.1975 0.085 Uiso 1 1 calc R . . C27 C 0.3820(10) 0.2081(13) 0.2124(2) 0.042(3) Uani 1 1 d . . . C28 C 0.3346(12) 0.0954(13) 0.2271(3) 0.061(5) Uani 1 1 d . . . H28A H 0.3406 0.1154 0.2446 0.092 Uiso 1 1 calc R . . H28B H 0.3776 0.0186 0.2241 0.092 Uiso 1 1 calc R . . H28C H 0.2559 0.0817 0.2219 0.092 Uiso 1 1 calc R . . C29 C 0.5039(10) 0.2312(15) 0.2222(3) 0.055(4) Uani 1 1 d . . . H29A H 0.5342 0.3054 0.2140 0.082 Uiso 1 1 calc R . . H29B H 0.5495 0.1567 0.2188 0.082 Uiso 1 1 calc R . . H29C H 0.5054 0.2462 0.2398 0.082 Uiso 1 1 calc R . . C30 C 0.3824(11) 0.1725(15) 0.1849(2) 0.055(4) Uani 1 1 d . . . H30A H 0.3060 0.1528 0.1787 0.082 Uiso 1 1 calc R . . H30B H 0.4303 0.0983 0.1829 0.082 Uiso 1 1 calc R . . H30C H 0.4113 0.2438 0.1757 0.082 Uiso 1 1 calc R . . C31 C -0.0848(9) 0.7983(9) 0.23097(18) 0.021(2) Uani 1 1 d . . . C32 C 0.1401(9) 0.7994(11) 0.2456(2) 0.027(3) Uani 1 1 d . . . C33 C 0.0004(9) 0.6106(10) 0.2593(2) 0.025(2) Uani 1 1 d . . . C34 C 0.3361(10) 0.8513(10) 0.0644(2) 0.033(3) Uani 1 1 d U . . C35 C 0.4459(10) 0.8443(11) 0.0537(2) 0.035(3) Uani 1 1 d U . . H35 H 0.4661 0.8824 0.0379 0.042 Uiso 1 1 calc R . . C36 C 0.5182(12) 0.7718(12) 0.0700(3) 0.044(3) Uani 1 1 d U . . H36 H 0.5985 0.7517 0.0676 0.053 Uiso 1 1 calc R . . C37 C 0.4572(13) 0.7404(12) 0.0915(3) 0.051(3) Uani 1 1 d U . . H37 H 0.4876 0.6925 0.1061 0.062 Uiso 1 1 calc R . . C38 C 0.3466(11) 0.7842(11) 0.0875(2) 0.040(3) Uani 1 1 d U . . H38 H 0.2860 0.7751 0.0992 0.048 Uiso 1 1 calc R . . C39 C 0.4125(11) 1.1139(10) 0.0937(2) 0.031(3) Uani 1 1 d . . . C40 C 0.4220(12) 1.0413(12) 0.1162(2) 0.042(3) Uani 1 1 d . . . H40 H 0.3599 1.0254 0.1274 0.050 Uiso 1 1 calc R . . C41 C 0.5334(13) 0.9935(14) 0.1196(2) 0.051(4) Uani 1 1 d . . . H41 H 0.5626 0.9392 0.1335 0.061 Uiso 1 1 calc R . . C42 C 0.5965(12) 1.0380(13) 0.0997(3) 0.049(4) Uani 1 1 d . . . H42 H 0.6771 1.0201 0.0971 0.059 Uiso 1 1 calc R . . C43 C 0.5212(10) 1.1105(11) 0.0841(2) 0.034(3) Uani 1 1 d . . . H43 H 0.5411 1.1508 0.0684 0.041 Uiso 1 1 calc R . . C1A C 0.1098(10) 0.7896(10) 0.0466(2) 0.032(3) Uani 1 1 d . . . C2A C 0.0668(11) 0.7512(12) 0.0242(2) 0.042(3) Uani 1 1 d . . . H2A H 0.0872 0.7950 0.0100 0.050 Uiso 1 1 calc R . . C3A C -0.0068(13) 0.6486(14) 0.0219(3) 0.062(5) Uani 1 1 d . . . H3A H -0.0351 0.6228 0.0061 0.075 Uiso 1 1 calc R . . C4A C -0.0387(12) 0.5840(14) 0.0425(3) 0.062(5) Uani 1 1 d . . . H4A H -0.0869 0.5126 0.0410 0.075 Uiso 1 1 calc R . . C5A C 0.0018(12) 0.6269(14) 0.0655(3) 0.055(4) Uani 1 1 d . . . H5A H -0.0214 0.5856 0.0798 0.066 Uiso 1 1 calc R . . C6A C 0.0754(11) 0.7286(13) 0.0680(3) 0.044(3) Uani 1 1 d . . . H6A H 0.1022 0.7568 0.0837 0.053 Uiso 1 1 calc R . . C1B C 0.2483(10) 0.9569(12) 0.0193(2) 0.031(3) Uani 1 1 d . . . C2B C 0.2275(10) 1.0749(12) 0.0086(2) 0.036(3) Uani 1 1 d . . . H2B H 0.1932 1.1400 0.0176 0.043 Uiso 1 1 calc R . . C3B C 0.2579(10) 1.0969(13) -0.0158(2) 0.038(3) Uani 1 1 d . . . H3B H 0.2450 1.1779 -0.0229 0.046 Uiso 1 1 calc R . . C4B C 0.3066(11) 1.0016(16) -0.0294(2) 0.051(4) Uani 1 1 d . . . H4B H 0.3257 1.0170 -0.0457 0.061 Uiso 1 1 calc R . . C5B C 0.3266(11) 0.8847(16) -0.0188(2) 0.052(4) Uani 1 1 d . . . H5B H 0.3610 0.8193 -0.0276 0.062 Uiso 1 1 calc R . . C6B C 0.2956(11) 0.8631(13) 0.0053(2) 0.044(3) Uani 1 1 d . . . H6B H 0.3074 0.7814 0.0122 0.052 Uiso 1 1 calc R . . C1C C 0.3279(11) 1.3054(12) 0.0598(2) 0.036(3) Uani 1 1 d . . . C2C C 0.3829(10) 1.2627(12) 0.0396(2) 0.034(3) Uani 1 1 d . . . H2C H 0.4053 1.1764 0.0390 0.041 Uiso 1 1 calc R . . C3C C 0.4065(11) 1.3412(15) 0.0201(2) 0.050(4) Uani 1 1 d . . . H3C H 0.4456 1.3101 0.0067 0.060 Uiso 1 1 calc R . . C4C C 0.3707(13) 1.4679(15) 0.0208(3) 0.059(4) Uani 1 1 d . . . H4C H 0.3852 1.5227 0.0076 0.071 Uiso 1 1 calc R . . C5C C 0.3157(14) 1.5141(12) 0.0401(3) 0.063(5) Uani 1 1 d . . . H5C H 0.2929 1.6002 0.0403 0.076 Uiso 1 1 calc R . . C6C C 0.2927(12) 1.4344(12) 0.0597(3) 0.046(3) Uani 1 1 d . . . H6C H 0.2536 1.4665 0.0730 0.056 Uiso 1 1 calc R . . C1D C 0.2764(12) 1.3038(12) 0.1103(2) 0.040(3) Uani 1 1 d U . . C2D C 0.3688(13) 1.3821(14) 0.1175(3) 0.055(4) Uani 1 1 d U . . H2D H 0.4353 1.3785 0.1088 0.066 Uiso 1 1 calc R . . C3D C 0.3622(16) 1.4650(16) 0.1376(3) 0.072(5) Uani 1 1 d U . . H3D H 0.4253 1.5146 0.1428 0.087 Uiso 1 1 calc R . . C4D C 0.2666(15) 1.4743(16) 0.1494(3) 0.064(4) Uani 1 1 d U . . H4D H 0.2616 1.5333 0.1624 0.077 Uiso 1 1 calc R . . C5D C 0.1758(14) 1.3986(15) 0.1428(3) 0.058(4) Uani 1 1 d U . . H5D H 0.1096 1.4034 0.1516 0.070 Uiso 1 1 calc R . . C6D C 0.1817(12) 1.3157(14) 0.1233(3) 0.050(4) Uani 1 1 d U . . H6D H 0.1182 1.2653 0.1187 0.060 Uiso 1 1 calc R . . P3 P 0.5447(3) 0.7464(4) 0.18777(8) 0.0567(11) Uani 1 1 d D . . F1 F 0.4988(15) 0.8473(16) 0.1687(3) 0.099(3) Uiso 0.50 1 d PD A 1 F2 F 0.5907(16) 0.6434(17) 0.2071(4) 0.099(3) Uiso 0.50 1 d PD A 1 F3 F 0.5303(15) 0.8418(16) 0.2086(3) 0.099(3) Uiso 0.50 1 d PD A 1 F4 F 0.5665(15) 0.6472(16) 0.1659(3) 0.099(3) Uiso 0.50 1 d PD A 1 F5 F 0.4246(11) 0.6889(17) 0.1886(3) 0.099(3) Uiso 0.50 1 d PD A 1 F6 F 0.6689(11) 0.7956(19) 0.1843(4) 0.099(3) Uiso 0.50 1 d PD A 1 F7 F 0.4652(14) 0.7493(19) 0.1635(3) 0.103(3) Uiso 0.50 1 d PD A 2 F8 F 0.6219(14) 0.7441(19) 0.2117(3) 0.103(3) Uiso 0.50 1 d PD A 2 F9 F 0.4396(13) 0.758(2) 0.2041(3) 0.103(3) Uiso 0.50 1 d PD A 2 F10 F 0.6510(13) 0.742(2) 0.1723(3) 0.103(3) Uiso 0.50 1 d PD A 2 F11 F 0.5383(15) 0.5983(12) 0.1883(4) 0.103(3) Uiso 0.50 1 d PD A 2 F12 F 0.5444(18) 0.8965(13) 0.1864(4) 0.103(3) Uiso 0.50 1 d PD A 2 C1S C 0.786(3) 0.634(4) 0.1269(6) 0.087(13) Uani 0.50 1 d P . . H1S1 H 0.7334 0.5691 0.1201 0.105 Uiso 0.50 1 calc PR . . H1S2 H 0.7602 0.6609 0.1429 0.105 Uiso 0.50 1 calc PR . . Cl1 Cl 0.9236(9) 0.5626(9) 0.13150(16) 0.081(3) Uani 0.50 1 d P . . Cl2 Cl 0.7848(9) 0.7555(12) 0.1084(2) 0.111(4) Uani 0.50 1 d P . . C2S C 0.636(3) 0.457(2) 0.0662(4) 0.059(8) Uani 0.50 1 d PDU . . H2S1 H 0.5977 0.5253 0.0751 0.071 Uiso 0.50 1 calc PR . . H2S2 H 0.5765 0.3953 0.0613 0.071 Uiso 0.50 1 calc PR . . Cl3 Cl 0.6704(9) 0.5191(15) 0.0420(2) 0.123(5) Uani 0.50 1 d PDU . . Cl4 Cl 0.7102(12) 0.3894(16) 0.0857(3) 0.173(8) Uani 0.50 1 d PDU . . 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 0.0356(6) 0.0265(5) 0.0205(5) 0.0036(4) 0.0058(4) 0.0010(4) Re1 0.0224(2) 0.0177(2) 0.0166(2) 0.00033(19) 0.00271(15) 0.00056(19) Fe1 0.0416(11) 0.0282(10) 0.0315(10) 0.0012(8) -0.0051(8) -0.0013(8) P1 0.0315(17) 0.0267(16) 0.0206(15) -0.0005(12) 0.0054(12) -0.0023(13) P2 0.0440(19) 0.0255(17) 0.0282(16) -0.0005(14) 0.0084(14) -0.0014(14) O1 0.032(5) 0.030(5) 0.050(6) -0.013(4) 0.006(4) 0.009(4) O2 0.046(6) 0.042(5) 0.039(5) -0.010(4) -0.001(4) -0.015(4) O3 0.050(5) 0.037(5) 0.018(4) 0.010(4) 0.010(4) 0.000(4) N1 0.028(5) 0.019(5) 0.035(6) 0.000(4) 0.006(4) 0.003(4) N2 0.011(4) 0.028(5) 0.020(5) 0.001(4) 0.002(3) -0.001(4) N3 0.015(5) 0.022(5) 0.018(4) 0.002(4) 0.002(3) 0.003(4) C1 0.072(11) 0.039(8) 0.046(9) 0.005(7) 0.002(7) 0.025(8) C2 0.051(9) 0.043(8) 0.046(9) 0.018(7) 0.000(7) 0.023(7) C3 0.028(7) 0.065(10) 0.039(8) 0.011(7) -0.010(6) 0.012(7) C4 0.034(8) 0.074(11) 0.057(10) -0.005(9) -0.007(7) -0.004(8) C5 0.041(8) 0.087(12) 0.039(8) 0.002(8) 0.008(6) 0.010(8) C6 0.038(7) 0.030(7) 0.030(7) -0.005(5) 0.005(5) 0.000(5) C7 0.041(7) 0.030(7) 0.023(6) 0.003(5) 0.006(5) -0.005(6) C8 0.022(6) 0.065(9) 0.038(7) 0.021(7) -0.003(5) -0.009(6) C9 0.039(8) 0.051(8) 0.029(7) 0.014(6) -0.001(6) 0.002(6) C10 0.035(7) 0.026(6) 0.028(6) -0.011(5) 0.015(5) -0.002(5) C11 0.022(6) 0.055(9) 0.035(7) 0.008(6) 0.013(5) -0.002(6) C12 0.028(7) 0.037(7) 0.037(7) 0.014(6) -0.005(5) 0.005(5) C13 0.019(6) 0.026(6) 0.026(6) 0.004(5) 0.004(5) 0.001(5) C14 0.022(6) 0.036(7) 0.028(6) 0.003(5) -0.006(5) 0.001(5) C15 0.029(6) 0.025(6) 0.028(6) 0.004(5) 0.004(5) -0.007(5) C16 0.029(6) 0.021(6) 0.028(6) 0.006(5) 0.013(5) 0.009(5) C17 0.025(6) 0.017(6) 0.017(5) 0.001(4) 0.005(4) -0.004(5) C18 0.026(6) 0.014(5) 0.022(6) -0.002(4) 0.004(4) -0.003(4) C19 0.022(6) 0.025(6) 0.033(6) 0.000(5) 0.005(5) 0.001(5) C20 0.027(6) 0.033(7) 0.029(6) 0.014(6) 0.006(5) 0.015(5) C21 0.018(6) 0.037(7) 0.039(7) 0.006(6) 0.001(5) 0.001(5) C22 0.029(7) 0.030(7) 0.031(7) 0.007(5) 0.001(5) -0.006(5) C23 0.022(6) 0.047(8) 0.036(7) -0.010(6) 0.006(5) -0.014(5) C24 0.036(8) 0.063(10) 0.052(9) -0.032(8) 0.012(6) -0.014(7) C25 0.036(8) 0.069(11) 0.074(11) -0.027(9) -0.018(7) -0.017(7) C26 0.063(10) 0.049(9) 0.058(10) -0.013(8) -0.005(8) -0.023(8) C27 0.034(7) 0.044(8) 0.049(8) 0.007(6) 0.019(6) 0.014(6) C28 0.048(9) 0.041(9) 0.097(13) 0.031(8) 0.022(8) 0.017(7) C29 0.029(8) 0.069(10) 0.067(10) -0.009(8) 0.006(7) 0.031(7) C30 0.041(8) 0.067(10) 0.057(9) -0.014(8) 0.004(7) 0.028(8) C31 0.038(7) 0.011(5) 0.014(5) -0.004(4) 0.001(4) -0.003(5) C32 0.028(6) 0.026(7) 0.030(6) 0.000(5) 0.008(5) -0.007(5) C33 0.028(6) 0.018(6) 0.027(6) -0.003(5) 0.001(5) 0.005(5) C34 0.045(6) 0.017(6) 0.037(6) -0.006(5) 0.004(5) -0.001(5) C35 0.030(6) 0.028(7) 0.046(7) -0.003(5) 0.001(5) 0.003(5) C36 0.044(7) 0.033(7) 0.055(8) -0.012(6) -0.009(5) 0.004(6) C37 0.073(9) 0.026(7) 0.053(8) -0.002(6) -0.013(6) 0.009(7) C38 0.047(7) 0.025(7) 0.046(7) 0.005(5) -0.008(5) -0.007(5) C39 0.053(8) 0.020(6) 0.018(6) -0.004(5) -0.004(5) -0.010(6) C40 0.053(9) 0.041(8) 0.030(7) -0.006(6) -0.005(6) -0.003(7) C41 0.071(10) 0.052(9) 0.027(7) -0.009(6) -0.017(7) 0.002(8) C42 0.039(8) 0.046(9) 0.059(10) -0.009(7) -0.017(7) 0.000(7) C43 0.040(8) 0.024(6) 0.038(7) 0.003(5) -0.004(6) 0.000(5) C1A 0.034(7) 0.019(6) 0.043(7) -0.002(5) 0.002(5) 0.001(5) C2A 0.050(8) 0.035(8) 0.039(8) 0.004(6) -0.009(6) -0.014(6) C3A 0.072(11) 0.043(9) 0.067(11) 0.001(8) -0.039(9) -0.017(8) C4A 0.052(10) 0.036(8) 0.097(13) 0.020(9) -0.022(9) -0.016(7) C5A 0.053(9) 0.052(9) 0.061(10) 0.000(8) 0.018(8) -0.013(8) C6A 0.044(8) 0.040(8) 0.048(8) -0.002(6) 0.003(6) -0.015(6) C1B 0.036(7) 0.037(7) 0.022(6) -0.008(5) 0.005(5) -0.007(6) C2B 0.039(7) 0.036(7) 0.035(7) -0.002(6) 0.010(6) -0.006(6) C3B 0.043(8) 0.045(8) 0.027(7) 0.004(6) -0.006(6) -0.018(6) C4B 0.039(8) 0.086(12) 0.030(7) 0.010(8) 0.019(6) 0.007(8) C5B 0.046(9) 0.081(12) 0.029(8) -0.006(7) 0.014(6) 0.016(8) C6B 0.047(8) 0.049(8) 0.034(7) -0.003(6) -0.006(6) 0.013(7) C1C 0.050(8) 0.028(7) 0.032(7) 0.004(6) 0.013(6) -0.008(6) C2C 0.041(8) 0.028(7) 0.035(7) -0.001(5) 0.001(6) -0.010(6) C3C 0.047(9) 0.063(11) 0.040(8) 0.004(7) 0.005(6) -0.014(7) C4C 0.068(11) 0.051(10) 0.061(10) 0.026(8) 0.021(8) -0.010(8) C5C 0.109(13) 0.015(7) 0.068(11) 0.007(7) 0.034(10) -0.002(8) C6C 0.056(9) 0.034(8) 0.050(9) 0.008(7) 0.013(7) -0.002(7) C1D 0.063(8) 0.031(7) 0.026(6) -0.005(5) 0.009(6) -0.006(6) C2D 0.060(9) 0.057(9) 0.050(8) -0.027(7) 0.006(7) -0.008(7) C3D 0.103(12) 0.064(10) 0.050(9) -0.031(8) 0.013(9) -0.018(9) C4D 0.100(11) 0.062(10) 0.033(8) -0.012(7) 0.022(8) 0.003(9) C5D 0.073(10) 0.064(10) 0.040(8) -0.006(7) 0.019(7) 0.000(8) C6D 0.059(8) 0.043(8) 0.050(8) -0.013(7) 0.013(7) -0.008(7) P3 0.033(2) 0.055(3) 0.083(3) 0.016(2) 0.0050(19) 0.0147(18) C1S 0.05(2) 0.15(4) 0.07(2) 0.02(2) 0.035(17) 0.02(2) Cl1 0.114(8) 0.073(6) 0.057(5) 0.013(5) 0.009(5) 0.010(5) Cl2 0.096(8) 0.131(10) 0.098(8) -0.030(7) -0.057(6) 0.061(7) C2S 0.083(19) 0.018(12) 0.077(19) 0.009(13) 0.005(16) 0.003(13) Cl3 0.084(7) 0.192(14) 0.095(8) -0.019(9) 0.028(6) -0.026(8) Cl4 0.118(10) 0.186(15) 0.204(15) 0.100(12) -0.088(10) -0.065(10) _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 C6 2.012(12) . ? Ru1 C3 2.207(12) . ? Ru1 C5 2.212(14) . ? Ru1 C4 2.216(13) . ? Ru1 C1 2.245(13) . ? Ru1 C2 2.247(12) . ? Ru1 P1 2.278(3) . ? Ru1 P2 2.281(3) . ? Re1 C31 1.912(11) . ? Re1 C33 1.914(11) . ? Re1 C32 1.926(11) . ? Re1 N2 2.153(8) . ? Re1 N3 2.177(8) . ? Re1 N1 2.198(9) . ? Fe1 C37 1.997(13) . ? Fe1 C40 2.023(13) . ? Fe1 C35 2.025(12) . ? Fe1 C41 2.028(12) . ? Fe1 C43 2.030(12) . ? Fe1 C38 2.031(12) . ? Fe1 C39 2.035(12) . ? Fe1 C34 2.040(12) . ? Fe1 C36 2.041(13) . ? Fe1 C42 2.056(13) . ? P1 C34 1.815(13) . ? P1 C1B 1.846(11) . ? P1 C1A 1.870(12) . ? P2 C39 1.809(13) . ? P2 C1C 1.817(12) . ? P2 C1D 1.845(12) . ? O1 C31 1.162(12) . ? O2 C32 1.138(12) . ? O3 C33 1.169(12) . ? N1 C12 1.345(14) . ? N1 C8 1.351(14) . ? N2 C17 1.363(13) . ? N2 C13 1.366(12) . ? N3 C22 1.326(13) . ? N3 C18 1.372(13) . ? C1 C2 1.418(18) . ? C1 C5 1.42(2) . ? C2 C3 1.381(19) . ? C3 C4 1.389(19) . ? C4 C5 1.41(2) . ? C6 C7 1.188(15) . ? C7 C10 1.420(15) . ? C8 C9 1.345(16) . ? C9 C10 1.381(16) . ? C10 C11 1.421(16) . ? C11 C12 1.329(15) . ? C13 C14 1.395(15) . ? C14 C15 1.356(16) . ? C15 C16 1.394(15) . ? C15 C23 1.539(15) . ? C16 C17 1.364(15) . ? C17 C18 1.452(14) . ? C18 C19 1.365(15) . ? C19 C20 1.399(15) . ? C20 C21 1.394(17) . ? C20 C27 1.523(16) . ? C21 C22 1.360(16) . ? C23 C26 1.509(18) . ? C23 C24 1.539(16) . ? C23 C25 1.560(17) . ? C27 C29 1.530(18) . ? C27 C30 1.536(18) . ? C27 C28 1.545(18) . ? C34 C38 1.434(16) . ? C34 C35 1.453(17) . ? C35 C36 1.415(17) . ? C36 C37 1.44(2) . ? C37 C38 1.393(18) . ? C39 C43 1.415(17) . ? C39 C40 1.437(16) . ? C40 C41 1.412(19) . ? C41 C42 1.43(2) . ? C42 C43 1.414(17) . ? C1A C2A 1.350(16) . ? C1A C6A 1.402(17) . ? C2A C3A 1.383(18) . ? C3A C4A 1.38(2) . ? C4A C5A 1.39(2) . ? C5A C6A 1.376(18) . ? C1B C2B 1.377(17) . ? C1B C6B 1.378(17) . ? C2B C3B 1.409(16) . ? C3B C4B 1.385(19) . ? C4B C5B 1.37(2) . ? C5B C6B 1.390(17) . ? C1C C2C 1.380(16) . ? C1C C6C 1.411(17) . ? C2C C3C 1.378(17) . ? C3C C4C 1.39(2) . ? C4C C5C 1.35(2) . ? C5C C6C 1.388(18) . ? C1D C6D 1.362(18) . ? C1D C2D 1.405(18) . ? C2D C3D 1.396(19) . ? C3D C4D 1.33(2) . ? C4D C5D 1.37(2) . ? C5D C6D 1.372(18) . ? P3 F3 1.524(12) . ? P3 F8 1.545(12) . ? P3 F5 1.547(12) . ? P3 F11 1.550(13) . ? P3 F10 1.551(13) . ? P3 F1 1.555(12) . ? P3 F12 1.571(14) . ? P3 F9 1.572(13) . ? P3 F7 1.574(12) . ? P3 F6 1.579(13) . ? P3 F2 1.579(14) . ? P3 F4 1.605(13) . ? C1S Cl2 1.62(4) . ? C1S Cl1 1.79(3) . ? C2S Cl4 1.515(18) . ? C2S Cl3 1.541(18) . ? 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 C6 Ru1 C3 133.2(5) . . ? C6 Ru1 C5 89.0(5) . . ? C3 Ru1 C5 60.8(5) . . ? C6 Ru1 C4 97.8(5) . . ? C3 Ru1 C4 36.6(5) . . ? C5 Ru1 C4 37.1(5) . . ? C6 Ru1 C1 115.7(5) . . ? C3 Ru1 C1 61.0(5) . . ? C5 Ru1 C1 37.2(5) . . ? C4 Ru1 C1 62.3(6) . . ? C6 Ru1 C2 150.0(5) . . ? C3 Ru1 C2 36.1(5) . . ? C5 Ru1 C2 61.2(5) . . ? C4 Ru1 C2 61.5(6) . . ? C1 Ru1 C2 36.8(5) . . ? C6 Ru1 P1 92.0(3) . . ? C3 Ru1 P1 91.3(4) . . ? C5 Ru1 P1 140.3(4) . . ? C4 Ru1 P1 103.7(4) . . ? C1 Ru1 P1 149.6(4) . . ? C2 Ru1 P1 113.1(4) . . ? C6 Ru1 P2 88.3(3) . . ? C3 Ru1 P2 137.5(4) . . ? C5 Ru1 P2 123.4(4) . . ? C4 Ru1 P2 158.8(4) . . ? C1 Ru1 P2 96.8(4) . . ? C2 Ru1 P2 104.3(4) . . ? P1 Ru1 P2 96.27(11) . . ? C31 Re1 C33 88.0(4) . . ? C31 Re1 C32 91.0(4) . . ? C33 Re1 C32 89.6(5) . . ? C31 Re1 N2 97.4(4) . . ? C33 Re1 N2 92.7(4) . . ? C32 Re1 N2 171.4(4) . . ? C31 Re1 N3 171.9(4) . . ? C33 Re1 N3 94.4(4) . . ? C32 Re1 N3 96.8(4) . . ? N2 Re1 N3 74.7(3) . . ? C31 Re1 N1 90.0(4) . . ? C33 Re1 N1 177.1(4) . . ? C32 Re1 N1 92.6(4) . . ? N2 Re1 N1 85.4(3) . . ? N3 Re1 N1 87.3(3) . . ? C37 Fe1 C40 118.4(6) . . ? C37 Fe1 C35 70.2(5) . . ? C40 Fe1 C35 160.2(5) . . ? C37 Fe1 C41 103.5(6) . . ? C40 Fe1 C41 40.8(5) . . ? C35 Fe1 C41 158.6(5) . . ? C37 Fe1 C43 159.8(6) . . ? C40 Fe1 C43 68.2(5) . . ? C35 Fe1 C43 110.4(5) . . ? C41 Fe1 C43 68.3(5) . . ? C37 Fe1 C38 40.5(5) . . ? C40 Fe1 C38 104.6(6) . . ? C35 Fe1 C38 69.6(5) . . ? C41 Fe1 C38 119.5(6) . . ? C43 Fe1 C38 159.6(5) . . ? C37 Fe1 C39 155.7(6) . . ? C40 Fe1 C39 41.5(5) . . ? C35 Fe1 C39 124.3(4) . . ? C41 Fe1 C39 69.7(5) . . ? C43 Fe1 C39 40.7(5) . . ? C38 Fe1 C39 121.4(5) . . ? C37 Fe1 C34 69.7(5) . . ? C40 Fe1 C34 121.5(5) . . ? C35 Fe1 C34 41.9(5) . . ? C41 Fe1 C34 156.7(6) . . ? C43 Fe1 C34 125.0(5) . . ? C38 Fe1 C34 41.3(5) . . ? C39 Fe1 C34 106.9(5) . . ? C37 Fe1 C36 41.8(6) . . ? C40 Fe1 C36 156.3(5) . . ? C35 Fe1 C36 40.7(5) . . ? C41 Fe1 C36 121.4(6) . . ? C43 Fe1 C36 125.6(6) . . ? C38 Fe1 C36 68.5(6) . . ? C39 Fe1 C36 161.3(5) . . ? C34 Fe1 C36 69.1(5) . . ? C37 Fe1 C42 121.5(6) . . ? C40 Fe1 C42 68.6(6) . . ? C35 Fe1 C42 124.1(6) . . ? C41 Fe1 C42 40.8(6) . . ? C43 Fe1 C42 40.5(5) . . ? C38 Fe1 C42 156.6(5) . . ? C39 Fe1 C42 69.3(5) . . ? C34 Fe1 C42 161.3(5) . . ? C36 Fe1 C42 108.3(6) . . ? C34 P1 C1B 101.2(6) . . ? C34 P1 C1A 102.3(5) . . ? C1B P1 C1A 100.9(5) . . ? C34 P1 Ru1 121.4(4) . . ? C1B P1 Ru1 118.2(4) . . ? C1A P1 Ru1 109.9(4) . . ? C39 P2 C1C 104.3(6) . . ? C39 P2 C1D 97.2(6) . . ? C1C P2 C1D 101.7(6) . . ? C39 P2 Ru1 122.1(4) . . ? C1C P2 Ru1 112.0(4) . . ? C1D P2 Ru1 116.7(4) . . ? C12 N1 C8 113.2(10) . . ? C12 N1 Re1 124.1(7) . . ? C8 N1 Re1 122.3(8) . . ? C17 N2 C13 117.7(9) . . ? C17 N2 Re1 118.2(6) . . ? C13 N2 Re1 124.0(7) . . ? C22 N3 C18 117.5(9) . . ? C22 N3 Re1 126.3(7) . . ? C18 N3 Re1 116.0(6) . . ? C2 C1 C5 106.3(13) . . ? C2 C1 Ru1 71.7(7) . . ? C5 C1 Ru1 70.1(8) . . ? C3 C2 C1 107.6(13) . . ? C3 C2 Ru1 70.4(7) . . ? C1 C2 Ru1 71.5(7) . . ? C2 C3 C4 110.9(14) . . ? C2 C3 Ru1 73.5(7) . . ? C4 C3 Ru1 72.0(7) . . ? C3 C4 C5 106.0(14) . . ? C3 C4 Ru1 71.4(8) . . ? C5 C4 Ru1 71.3(8) . . ? C4 C5 C1 109.2(13) . . ? C4 C5 Ru1 71.6(8) . . ? C1 C5 Ru1 72.7(8) . . ? C7 C6 Ru1 170.9(11) . . ? C6 C7 C10 174.8(13) . . ? C9 C8 N1 125.1(11) . . ? C8 C9 C10 121.7(12) . . ? C9 C10 C7 121.6(11) . . ? C9 C10 C11 113.3(11) . . ? C7 C10 C11 125.1(10) . . ? C12 C11 C10 121.2(11) . . ? C11 C12 N1 125.5(11) . . ? N2 C13 C14 121.8(10) . . ? C15 C14 C13 120.2(10) . . ? C14 C15 C16 117.5(10) . . ? C14 C15 C23 122.5(10) . . ? C16 C15 C23 119.9(10) . . ? C17 C16 C15 121.6(10) . . ? N2 C17 C16 121.1(9) . . ? N2 C17 C18 114.5(9) . . ? C16 C17 C18 124.4(10) . . ? C19 C18 N3 119.6(9) . . ? C19 C18 C17 124.0(10) . . ? N3 C18 C17 116.4(9) . . ? C18 C19 C20 123.2(11) . . ? C21 C20 C19 115.0(10) . . ? C21 C20 C27 124.0(10) . . ? C19 C20 C27 121.0(11) . . ? C22 C21 C20 119.6(10) . . ? N3 C22 C21 124.9(11) . . ? C26 C23 C24 110.8(12) . . ? C26 C23 C15 108.9(10) . . ? C24 C23 C15 109.8(9) . . ? C26 C23 C25 107.8(11) . . ? C24 C23 C25 109.2(11) . . ? C15 C23 C25 110.2(10) . . ? C20 C27 C29 112.0(11) . . ? C20 C27 C30 109.4(10) . . ? C29 C27 C30 108.7(10) . . ? C20 C27 C28 109.3(10) . . ? C29 C27 C28 107.7(11) . . ? C30 C27 C28 109.8(13) . . ? O1 C31 Re1 178.8(9) . . ? O2 C32 Re1 178.2(11) . . ? O3 C33 Re1 177.1(9) . . ? C38 C34 C35 106.6(11) . . ? C38 C34 P1 126.0(10) . . ? C35 C34 P1 127.4(9) . . ? C38 C34 Fe1 69.0(7) . . ? C35 C34 Fe1 68.5(7) . . ? P1 C34 Fe1 127.7(6) . . ? C36 C35 C34 107.7(12) . . ? C36 C35 Fe1 70.2(7) . . ? C34 C35 Fe1 69.6(7) . . ? C35 C36 C37 108.2(12) . . ? C35 C36 Fe1 69.1(7) . . ? C37 C36 Fe1 67.5(7) . . ? C38 C37 C36 108.0(12) . . ? C38 C37 Fe1 71.1(7) . . ? C36 C37 Fe1 70.7(8) . . ? C37 C38 C34 109.4(12) . . ? C37 C38 Fe1 68.4(8) . . ? C34 C38 Fe1 69.7(7) . . ? C43 C39 C40 105.6(11) . . ? C43 C39 P2 131.9(9) . . ? C40 C39 P2 122.4(10) . . ? C43 C39 Fe1 69.5(7) . . ? C40 C39 Fe1 68.8(7) . . ? P2 C39 Fe1 129.0(6) . . ? C41 C40 C39 109.0(12) . . ? C41 C40 Fe1 69.8(7) . . ? C39 C40 Fe1 69.7(7) . . ? C40 C41 C42 108.1(12) . . ? C40 C41 Fe1 69.4(7) . . ? C42 C41 Fe1 70.7(7) . . ? C43 C42 C41 106.7(12) . . ? C43 C42 Fe1 68.8(7) . . ? C41 C42 Fe1 68.5(8) . . ? C42 C43 C39 110.6(12) . . ? C42 C43 Fe1 70.8(7) . . ? C39 C43 Fe1 69.8(7) . . ? C2A C1A C6A 119.7(12) . . ? C2A C1A P1 123.7(10) . . ? C6A C1A P1 116.6(9) . . ? C1A C2A C3A 121.2(13) . . ? C4A C3A C2A 120.2(13) . . ? C3A C4A C5A 118.4(13) . . ? C6A C5A C4A 121.5(14) . . ? C5A C6A C1A 118.9(13) . . ? C2B C1B C6B 118.3(11) . . ? C2B C1B P1 119.5(9) . . ? C6B C1B P1 122.1(10) . . ? C1B C2B C3B 119.4(12) . . ? C4B C3B C2B 121.3(13) . . ? C5B C4B C3B 119.0(12) . . ? C4B C5B C6B 119.5(13) . . ? C1B C6B C5B 122.4(13) . . ? C2C C1C C6C 117.3(11) . . ? C2C C1C P2 121.6(9) . . ? C6C C1C P2 120.5(10) . . ? C3C C2C C1C 122.7(13) . . ? C2C C3C C4C 118.0(13) . . ? C5C C4C C3C 121.5(13) . . ? C4C C5C C6C 120.0(13) . . ? C5C C6C C1C 120.4(13) . . ? C6D C1D C2D 117.0(12) . . ? C6D C1D P2 122.7(10) . . ? C2D C1D P2 120.3(10) . . ? C3D C2D C1D 120.2(14) . . ? C4D C3D C2D 120.2(16) . . ? C3D C4D C5D 120.6(15) . . ? C4D C5D C6D 119.7(14) . . ? C1D C6D C5D 122.3(14) . . ? F3 P3 F8 58.2(9) . . ? F3 P3 F5 95.2(8) . . ? F8 P3 F5 118.1(9) . . ? F3 P3 F11 129.1(10) . . ? F8 P3 F11 89.7(8) . . ? F5 P3 F11 64.2(9) . . ? F3 P3 F10 123.4(10) . . ? F8 P3 F10 89.6(8) . . ? F5 P3 F10 141.1(10) . . ? F11 P3 F10 91.1(9) . . ? F3 P3 F1 90.0(8) . . ? F8 P3 F1 137.6(10) . . ? F5 P3 F1 89.7(8) . . ? F11 P3 F1 132.4(9) . . ? F10 P3 F1 85.8(10) . . ? F3 P3 F12 51.9(9) . . ? F8 P3 F12 93.2(8) . . ? F5 P3 F12 112.9(11) . . ? F11 P3 F12 176.7(10) . . ? F10 P3 F12 90.4(12) . . ? F1 P3 F12 44.8(8) . . ? F3 P3 F9 53.7(9) . . ? F8 P3 F9 88.8(8) . . ? F5 P3 F9 41.8(8) . . ? F11 P3 F9 91.3(9) . . ? F10 P3 F9 177.0(11) . . ? F1 P3 F9 93.8(10) . . ? F12 P3 F9 87.3(12) . . ? F3 P3 F7 121.4(9) . . ? F8 P3 F7 179.5(10) . . ? F5 P3 F7 61.6(9) . . ? F11 P3 F7 90.4(8) . . ? F10 P3 F7 90.9(8) . . ? F1 P3 F7 42.3(8) . . ? F12 P3 F7 86.6(8) . . ? F9 P3 F7 90.8(8) . . ? F3 P3 F6 91.0(8) . . ? F8 P3 F6 65.9(9) . . ? F5 P3 F6 173.7(9) . . ? F11 P3 F6 112.0(10) . . ? F10 P3 F6 32.6(8) . . ? F1 P3 F6 89.7(9) . . ? F12 P3 F6 70.7(11) . . ? F9 P3 F6 144.5(10) . . ? F7 P3 F6 114.4(10) . . ? F3 P3 F2 90.1(9) . . ? F8 P3 F2 42.7(9) . . ? F5 P3 F2 90.0(8) . . ? F11 P3 F2 47.3(9) . . ? F10 P3 F2 94.4(11) . . ? F1 P3 F2 179.7(11) . . ? F12 P3 F2 135.5(10) . . ? F9 P3 F2 86.1(11) . . ? F7 P3 F2 137.4(10) . . ? F6 P3 F2 90.6(10) . . ? F3 P3 F4 177.2(9) . . ? F8 P3 F4 119.8(10) . . ? F5 P3 F4 87.5(8) . . ? F11 P3 F4 51.6(9) . . ? F10 P3 F4 54.0(9) . . ? F1 P3 F4 90.7(8) . . ? F12 P3 F4 127.5(11) . . ? F9 P3 F4 129.0(10) . . ? F7 P3 F4 60.7(9) . . ? F6 P3 F4 86.2(8) . . ? F2 P3 F4 89.2(10) . . ? Cl2 C1S Cl1 113.2(18) . . ? Cl4 C2S Cl3 128(2) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.545 _refine_diff_density_min -3.600 _refine_diff_density_rms 0.184