# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_3-acetone _database_code_depnum_ccdc_archive 'CCDC 914947' #TrackingRef 'CrystallographicData.cif' #============================================================================== _audit_creation_date 08-09-04 _audit_creation_method CRYSTALS_ver_12.86 _oxford_structure_analysis_title 5966 _chemical_name_systematic . _chemical_melting_point 'not measured' _cell_length_a 13.4126(2) _cell_length_b 16.0697(2) _cell_length_c 18.8013(2) _cell_angle_alpha 90 _cell_angle_beta 91.9500(5) _cell_angle_gamma 90 _cell_volume 4050.02(9) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1 ' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y+1/2,-z+1/2 x,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' F 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4' S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Re -1.0185 7.2310 28.7621 1.6719 15.7189 9.0923 14.5564 0.3505 5.4417 52.0861 10.4720 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Ru -1.2594 0.8363 19.2674 0.8085 12.9182 8.4347 4.8634 24.7997 1.5676 94.2928 5.3787 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C9 H15 F9 N6 O14 Re1 Ru1 S3 # Dc = 1.62 Fooo = 2268.00 Mu = 36.03 M = 985.70 # Found Formula = C18 H33 F9 N6 O17 Re1 Ru1 S3 # Dc = 1.90 FOOO = 2268.00 Mu = 36.24 M = 1159.94 _chemical_formula_sum 'C18 H33 F9 N6 O17 Re1 Ru1 S3' _chemical_formula_moiety 'C6 H15 N6 O5 Re Ru, 3(C3 H6 O), 3(C F3 O3 S)' _chemical_compound_source . _chemical_formula_weight 1159.94 _cell_measurement_reflns_used 9459 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description needle _exptl_crystal_colour clear_pale_yellow _exptl_crystal_size_min 0.11 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_max 0.28 _exptl_crystal_density_diffrn 1.902 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 2268 _exptl_absorpt_coefficient_mu 3.624 # Sheldrick geometric approximatio 0.65 0.67 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.53 _exptl_absorpt_correction_T_max 0.67 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device 'Nonius KappaCCD' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% . _diffrn_ambient_temperature 150 _diffrn_reflns_number 58795 _reflns_number_total 9202 _diffrn_reflns_av_R_equivalents 0.021 # Number of reflections with Friedels Law is 9202 # Number of reflections without Friedels Law is 18288 # Theoretical number of reflections is about 9274 _diffrn_reflns_theta_min 5.119 _diffrn_reflns_theta_max 27.468 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.919 _diffrn_measured_fraction_theta_full 0.993 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _reflns_limit_h_min -17 _reflns_limit_h_max 17 _reflns_limit_k_min 0 _reflns_limit_k_max 20 _reflns_limit_l_min 0 _reflns_limit_l_max 24 _oxford_diffrn_Wilson_B_factor 1.89 _oxford_diffrn_Wilson_scale 55.20 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.04 _refine_diff_density_max 1.50 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-3.0\s(I) _refine_ls_number_reflns 9200 _refine_ls_number_restraints 418 _refine_ls_number_parameters 497 _oxford_refine_ls_R_factor_ref 0.0398 _refine_ls_wR_factor_ref 0.0646 _refine_ls_goodness_of_fit_ref 0.9899 _refine_ls_shift/su_max 0.001382 # The values computed from all data _oxford_reflns_number_all 9201 _refine_ls_R_factor_all 0.0398 _refine_ls_wR_factor_all 0.0646 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 7734 _refine_ls_R_factor_gt 0.0291 _refine_ls_wR_factor_gt 0.0612 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.02P)^2^ + 7.85P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Insert your own references if required - in alphabetical order 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Ru1 Ru 0.463531(16) 0.410266(14) 0.216784(13) 0.0191 1.0000 Uani . U . . . . . Re1 Re 0.070372(8) 0.402055(8) 0.208510(7) 0.0252 1.0000 Uani . U . . . . . C1 C 0.2275(2) 0.41182(19) 0.20826(17) 0.0247 1.0000 Uani . U . . . . . C2 C 0.0891(3) 0.3039(2) 0.2749(2) 0.0384 1.0000 Uani . U . . . . . C3 C 0.0671(2) 0.4810(2) 0.2920(2) 0.0321 1.0000 Uani . U . . . . . C4 C 0.0592(2) 0.4990(2) 0.1409(2) 0.0327 1.0000 Uani . U . . . . . C5 C 0.0731(2) 0.3233(2) 0.1256(2) 0.0330 1.0000 Uani . U . . . . . C6 C -0.0773(2) 0.3938(2) 0.2083(2) 0.0328 1.0000 Uani . U . . . . . O1 O 0.1039(3) 0.2489(2) 0.31061(17) 0.0646 1.0000 Uani . U . . . . . O2 O 0.0634(2) 0.52563(18) 0.33795(15) 0.0465 1.0000 Uani . U . . . . . O3 O 0.0508(2) 0.55262(18) 0.10280(16) 0.0496 1.0000 Uani . U . . . . . O4 O 0.0722(2) 0.27890(18) 0.07966(15) 0.0504 1.0000 Uani . U . . . . . O5 O -0.16132(18) 0.39112(19) 0.20703(18) 0.0525 1.0000 Uani . U . . . . . N1 N 0.31237(19) 0.41471(16) 0.20979(14) 0.0241 1.0000 Uani . U . . . . . N2 N 0.47510(19) 0.52335(16) 0.16155(14) 0.0265 1.0000 Uani . U . . . . . N3 N 0.46115(19) 0.47561(16) 0.31334(14) 0.0258 1.0000 Uani . U . . . . . N4 N 0.45238(19) 0.29517(16) 0.26975(14) 0.0254 1.0000 Uani . U . . . . . N5 N 0.46448(19) 0.34270(17) 0.12053(14) 0.0261 1.0000 Uani . U . . . . . N6 N 0.61877(17) 0.40562(16) 0.22752(14) 0.0229 1.0000 Uani . U . . . . . F1 F 0.85950(19) 0.6017(2) 0.27598(16) 0.0786 1.0000 Uani . U . . . . . F2 F 0.85923(16) 0.60568(15) 0.38939(13) 0.0516 1.0000 Uani . U . . . . . F3 F 0.8078(2) 0.49837(15) 0.33355(17) 0.0708 1.0000 Uani . U . . . . . F4 F 0.14301(15) 0.54311(15) -0.05050(13) 0.0496 1.0000 Uani . U . . . . . F5 F 0.16296(18) 0.42410(16) 0.00059(15) 0.0569 1.0000 Uani . U . . . . . F6 F 0.20217(18) 0.44022(17) -0.10815(13) 0.0582 1.0000 Uani . U . . . . . F7 F 0.7691(2) 0.25535(15) 0.29444(13) 0.0599 1.0000 Uani . U . . . . . F8 F 0.87023(17) 0.19972(18) 0.22221(19) 0.0785 1.0000 Uani . U . . . . . F9 F 0.7949(3) 0.12295(17) 0.29708(18) 0.0884 1.0000 Uani . U . . . . . S1 S 0.68250(6) 0.62201(5) 0.32735(5) 0.0328 1.0000 Uani . U . . . . . S2 S 0.32894(6) 0.50743(5) -0.01585(4) 0.0297 1.0000 Uani . U . . . . . S3 S 0.68186(6) 0.17234(5) 0.19054(5) 0.0295 1.0000 Uani . U . . . . . O6 O 0.6975(2) 0.71050(16) 0.32910(17) 0.0515 1.0000 Uani . U . . . . . O7 O 0.6421(2) 0.59019(16) 0.26091(15) 0.0444 1.0000 Uani . U . . . . . O8 O 0.6385(2) 0.5879(2) 0.38922(17) 0.0604 1.0000 Uani . U . . . . . O9 O 0.31314(19) 0.54743(18) 0.05099(13) 0.0434 1.0000 Uani . U . . . . . O10 O 0.35953(19) 0.56073(18) -0.07228(14) 0.0434 1.0000 Uani . U . . . . . O11 O 0.3827(2) 0.42948(18) -0.01135(16) 0.0480 1.0000 Uani . U . . . . . O12 O 0.6784(2) 0.24767(15) 0.14941(14) 0.0401 1.0000 Uani . U . . . . . O13 O 0.5972(2) 0.16123(17) 0.23526(17) 0.0501 1.0000 Uani . U . . . . . O14 O 0.71070(19) 0.09852(15) 0.15369(15) 0.0412 1.0000 Uani . U . . . . . C7 C 0.8094(3) 0.5802(2) 0.3315(2) 0.0371 1.0000 Uani . U . . . . . C8 C 0.2029(3) 0.4773(2) -0.0452(2) 0.0364 1.0000 Uani . U . . . . . C9 C 0.7843(3) 0.1887(2) 0.2543(2) 0.0464 1.0000 Uani . U . . . . . O15 O 0.3680(2) 0.34765(19) 0.40298(16) 0.0529 1.0000 Uani . U . . . . . O16 O 0.6120(2) 0.35338(17) 0.38017(14) 0.0423 1.0000 Uani . U . . . . . O17 O 0.9789(4) 0.3474(4) 0.4061(3) 0.1277 1.0000 Uani . U . . . . . C10 C 0.2302(3) 0.4189(3) 0.4475(3) 0.0517 1.0000 Uani . U . . . . . C11 C 0.2924(3) 0.3445(2) 0.43693(19) 0.0346 1.0000 Uani . U . . . . . C12 C 0.2616(3) 0.2648(2) 0.4712(2) 0.0480 1.0000 Uani . U . . . . . C13 C 0.5751(4) 0.3940(4) 0.4963(2) 0.0674 1.0000 Uani . U . . . . . C14 C 0.5928(3) 0.3319(3) 0.4395(2) 0.0414 1.0000 Uani . U . . . . . C15 C 0.5858(4) 0.2418(3) 0.4581(3) 0.0725 1.0000 Uani . U . . . . . C16 C 0.8840(7) 0.3948(4) 0.4951(4) 0.1140 1.0000 Uani . U . . . . . C17 C 0.9203(3) 0.3305(3) 0.4492(3) 0.0547 1.0000 Uani . U . . . . . C18 C 0.8772(5) 0.2459(4) 0.4590(4) 0.1025 1.0000 Uani . U . . . . . H21 H 0.5246 0.5205 0.1313 0.0394 1.0000 Uiso R . . . . . . H22 H 0.4860 0.5644 0.1908 0.0394 1.0000 Uiso R . . . . . . H23 H 0.4197 0.5321 0.1359 0.0395 1.0000 Uiso R . . . . . . H31 H 0.5205 0.4909 0.3282 0.0390 1.0000 Uiso R . . . . . . H32 H 0.4350 0.4446 0.3465 0.0394 1.0000 Uiso R . . . . . . H33 H 0.4257 0.5202 0.3087 0.0392 1.0000 Uiso R . . . . . . H41 H 0.4445 0.3034 0.3161 0.0380 1.0000 Uiso R . . . . . . H42 H 0.5064 0.2647 0.2639 0.0382 1.0000 Uiso R . . . . . . H43 H 0.3983 0.2672 0.2537 0.0382 1.0000 Uiso R . . . . . . H51 H 0.4275 0.2978 0.1234 0.0389 1.0000 Uiso R . . . . . . H52 H 0.4415 0.3724 0.0844 0.0387 1.0000 Uiso R . . . . . . H53 H 0.5238 0.3263 0.1116 0.0395 1.0000 Uiso R . . . . . . H61 H 0.6364 0.3812 0.2674 0.0339 1.0000 Uiso R . . . . . . H62 H 0.6421 0.4571 0.2286 0.0342 1.0000 Uiso R . . . . . . H63 H 0.6469 0.3809 0.1922 0.0340 1.0000 Uiso R . . . . . . H101 H 0.2386 0.4392 0.4953 0.0780 1.0000 Uiso R . . . . . . H102 H 0.1616 0.4020 0.4402 0.0777 1.0000 Uiso R . . . . . . H103 H 0.2460 0.4624 0.4149 0.0777 1.0000 Uiso R . . . . . . H121 H 0.3055 0.2209 0.4594 0.0720 1.0000 Uiso R . . . . . . H122 H 0.1967 0.2511 0.4544 0.0723 1.0000 Uiso R . . . . . . H123 H 0.2607 0.2716 0.5223 0.0720 1.0000 Uiso R . . . . . . H131 H 0.6234 0.3857 0.5343 0.1008 1.0000 Uiso R . . . . . . H132 H 0.5812 0.4498 0.4774 0.1012 1.0000 Uiso R . . . . . . H133 H 0.5099 0.3858 0.5139 0.1011 1.0000 Uiso R . . . . . . H151 H 0.6214 0.2312 0.5023 0.1091 1.0000 Uiso R . . . . . . H152 H 0.5160 0.2266 0.4614 0.1089 1.0000 Uiso R . . . . . . H153 H 0.6151 0.2096 0.4207 0.1092 1.0000 Uiso R . . . . . . H161 H 0.8892 0.3768 0.5440 0.1731 1.0000 Uiso R . . . . . . H162 H 0.9217 0.4447 0.4898 0.1730 1.0000 Uiso R . . . . . . H163 H 0.8155 0.4056 0.4834 0.1731 1.0000 Uiso R . . . . . . H181 H 0.8660 0.2347 0.5082 0.1511 1.0000 Uiso R . . . . . . H182 H 0.8155 0.2414 0.4325 0.1509 1.0000 Uiso R . . . . . . H183 H 0.9226 0.2059 0.4418 0.1512 1.0000 Uiso 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 Ru1 0.01200(11) 0.02100(12) 0.02409(13) -0.00019(9) -0.00033(9) 0.00030(9) Re1 0.01310(7) 0.02884(8) 0.03381(8) -0.00010(5) 0.00131(5) -0.00001(5) C1 0.0165(10) 0.0283(16) 0.0292(16) 0.0006(13) -0.0004(11) 0.0016(11) C2 0.0384(19) 0.0378(17) 0.0394(19) 0.0031(13) 0.0086(15) 0.0038(15) C3 0.0182(14) 0.0373(18) 0.0409(17) -0.0023(12) 0.0003(13) 0.0010(13) C4 0.0232(15) 0.0340(16) 0.0405(19) 0.0006(12) -0.0042(14) -0.0031(13) C5 0.0220(15) 0.0360(18) 0.0409(18) -0.0027(12) 0.0014(14) -0.0017(14) C6 0.0196(10) 0.0333(18) 0.046(2) -0.0039(15) 0.0057(13) -0.0035(13) O1 0.092(3) 0.0494(18) 0.054(2) 0.0147(14) 0.0173(17) 0.0215(17) O2 0.0375(14) 0.0538(17) 0.0481(16) -0.0140(12) 0.0005(12) 0.0034(13) O3 0.0463(16) 0.0441(16) 0.0575(18) 0.0144(12) -0.0113(13) -0.0068(13) O4 0.0538(17) 0.0498(17) 0.0477(16) -0.0117(12) 0.0049(13) -0.0012(14) O5 0.0181(10) 0.0593(18) 0.081(2) -0.0033(16) 0.0065(13) -0.0040(12) N1 0.0158(9) 0.0274(14) 0.0289(14) -0.0006(11) -0.0015(10) 0.0006(10) N2 0.0237(13) 0.0249(12) 0.0306(14) 0.0021(10) -0.0034(11) -0.0001(10) N3 0.0221(12) 0.0256(13) 0.0297(13) -0.0018(10) 0.0001(10) 0.0017(11) N4 0.0230(13) 0.0243(12) 0.0288(14) 0.0017(10) 0.0023(10) -0.0006(10) N5 0.0205(12) 0.0302(14) 0.0273(13) -0.0032(10) -0.0013(10) -0.0003(11) N6 0.0136(10) 0.0273(13) 0.0278(13) -0.0011(11) 0.0007(9) 0.0009(10) F1 0.0384(14) 0.136(3) 0.0619(16) 0.0233(17) 0.0138(12) 0.0143(16) F2 0.0326(11) 0.0594(15) 0.0617(14) -0.0111(12) -0.0179(10) 0.0088(10) F3 0.0614(16) 0.0369(11) 0.113(2) -0.0120(14) -0.0195(15) 0.0203(11) F4 0.0274(11) 0.0588(14) 0.0619(15) 0.0041(12) -0.0073(10) 0.0071(10) F5 0.0422(13) 0.0560(15) 0.0731(17) 0.0140(12) 0.0108(12) -0.0157(11) F6 0.0516(15) 0.0730(17) 0.0491(13) -0.0174(12) -0.0128(11) -0.0079(13) F7 0.0800(18) 0.0445(13) 0.0538(15) -0.0131(11) -0.0202(13) 0.0122(13) F8 0.0265(11) 0.0640(17) 0.144(3) -0.0371(17) -0.0090(13) 0.0019(11) F9 0.125(3) 0.0473(15) 0.089(2) 0.0105(14) -0.0545(19) 0.0235(16) S1 0.0241(4) 0.0282(4) 0.0457(5) -0.0031(4) -0.0050(3) 0.0031(3) S2 0.0234(4) 0.0371(5) 0.0285(4) 0.0052(3) -0.0019(3) -0.0018(3) S3 0.0242(4) 0.0234(4) 0.0408(5) 0.0003(3) 0.0012(3) 0.0016(3) O6 0.0473(16) 0.0281(11) 0.077(2) -0.0063(13) -0.0253(14) 0.0064(11) O7 0.0371(14) 0.0402(15) 0.0547(15) -0.0097(12) -0.0145(12) -0.0006(11) O8 0.0370(15) 0.086(2) 0.0586(17) 0.0152(16) 0.0083(13) 0.0005(15) O9 0.0410(15) 0.0586(17) 0.0300(12) -0.0034(11) -0.0065(11) 0.0012(13) O10 0.0355(14) 0.0558(17) 0.0391(14) 0.0162(12) 0.0020(11) -0.0087(12) O11 0.0385(15) 0.0470(14) 0.0579(18) 0.0050(13) -0.0066(13) 0.0101(12) O12 0.0506(15) 0.0270(12) 0.0423(15) 0.0040(10) -0.0031(12) 0.0015(11) O13 0.0374(14) 0.0357(15) 0.079(2) 0.0067(14) 0.0252(13) 0.0020(12) O14 0.0384(14) 0.0273(12) 0.0580(17) -0.0104(11) 0.0014(12) 0.0033(10) C7 0.0286(14) 0.0386(15) 0.0438(17) -0.0015(15) -0.0039(12) 0.0063(13) C8 0.0274(14) 0.0424(18) 0.0392(16) 0.0026(13) -0.0019(13) -0.0043(11) C9 0.0452(16) 0.0314(17) 0.061(2) -0.0058(12) -0.0168(13) 0.0113(16) O15 0.0522(17) 0.0543(18) 0.0539(18) 0.0010(14) 0.0270(13) -0.0063(14) O16 0.0430(15) 0.0500(16) 0.0339(13) 0.0077(12) -0.0001(11) 0.0034(12) O17 0.100(4) 0.156(5) 0.131(4) -0.037(4) 0.071(3) -0.008(3) C10 0.049(2) 0.049(2) 0.058(3) 0.016(2) 0.011(2) 0.0100(17) C11 0.0348(17) 0.0396(17) 0.0297(18) 0.0024(14) 0.0045(13) -0.0050(14) C12 0.049(2) 0.039(2) 0.056(3) 0.0113(18) 0.0103(19) -0.0034(18) C13 0.062(3) 0.099(4) 0.040(2) -0.012(2) -0.004(2) 0.012(3) C14 0.0339(19) 0.055(2) 0.0351(16) 0.0099(14) -0.0042(15) 0.0055(17) C15 0.069(3) 0.064(2) 0.084(4) 0.035(3) 0.008(3) 0.006(3) C16 0.163(7) 0.071(4) 0.112(6) -0.027(4) 0.070(5) 0.000(4) C17 0.046(2) 0.063(2) 0.054(3) -0.014(2) -0.0018(17) 0.0078(19) C18 0.113(5) 0.061(3) 0.129(6) -0.009(3) -0.049(4) -0.011(3) _refine_ls_extinction_coef 117(7) _refine_ls_extinction_method 'Larson (1970), Equation 22' _oxford_refine_ls_scale 0.13874(4) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ru1 . N1 . 2.028(2) yes Ru1 . N2 . 2.101(3) yes Ru1 . N3 . 2.098(3) yes Ru1 . N4 . 2.108(3) yes Ru1 . N5 . 2.111(3) yes Ru1 . N6 . 2.086(2) yes Re1 . C1 . 2.114(3) yes Re1 . C2 . 2.022(4) yes Re1 . C3 . 2.020(4) yes Re1 . C4 . 2.013(4) yes Re1 . C5 . 2.010(4) yes Re1 . C6 . 1.985(3) yes C1 . N1 . 1.139(4) yes C2 . O1 . 1.124(5) yes C3 . O2 . 1.125(4) yes C4 . O3 . 1.124(4) yes C5 . O4 . 1.119(4) yes C6 . O5 . 1.128(4) yes N2 . H21 . 0.890 no N2 . H22 . 0.868 no N2 . H23 . 0.884 no N3 . H31 . 0.870 no N3 . H32 . 0.881 no N3 . H33 . 0.864 no N4 . H41 . 0.891 no N4 . H42 . 0.884 no N4 . H43 . 0.896 no N5 . H51 . 0.878 no N5 . H52 . 0.878 no N5 . H53 . 0.860 no N6 . H61 . 0.871 no N6 . H62 . 0.884 no N6 . H63 . 0.871 no F1 . C7 . 1.307(5) yes F2 . C7 . 1.322(4) yes F3 . C7 . 1.316(4) yes F4 . C8 . 1.330(4) yes F5 . C8 . 1.338(4) yes F6 . C8 . 1.324(4) yes F7 . C9 . 1.330(4) yes F8 . C9 . 1.331(5) yes F9 . C9 . 1.333(5) yes S1 . O6 . 1.437(3) yes S1 . O7 . 1.438(3) yes S1 . O8 . 1.432(3) yes S1 . C7 . 1.829(4) yes S2 . O9 . 1.434(3) yes S2 . O10 . 1.434(3) yes S2 . O11 . 1.446(3) yes S2 . C8 . 1.826(3) yes S3 . O12 . 1.436(3) yes S3 . O13 . 1.447(3) yes S3 . O14 . 1.434(3) yes S3 . C9 . 1.811(4) yes O15 . C11 . 1.217(4) yes O16 . C14 . 1.203(4) yes O17 . C17 . 1.179(6) yes C10 . C11 . 1.475(5) yes C10 . H101 . 0.960 no C10 . H102 . 0.965 no C10 . H103 . 0.958 no C11 . C12 . 1.498(5) yes C12 . H121 . 0.950 no C12 . H122 . 0.943 no C12 . H123 . 0.968 no C13 . C14 . 1.486(6) yes C13 . H131 . 0.958 no C13 . H132 . 0.969 no C13 . H133 . 0.954 no C14 . C15 . 1.494(6) yes C15 . H151 . 0.959 no C15 . H152 . 0.972 no C15 . H153 . 0.967 no C16 . C17 . 1.443(7) yes C16 . H161 . 0.964 no C16 . H162 . 0.956 no C16 . H163 . 0.953 no C17 . C18 . 1.490(8) yes C18 . H181 . 0.960 no C18 . H182 . 0.954 no C18 . H183 . 0.949 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 . Ru1 . N2 . 91.60(10) yes N1 . Ru1 . N3 . 89.65(10) yes N2 . Ru1 . N3 . 89.91(11) yes N1 . Ru1 . N4 . 88.55(10) yes N2 . Ru1 . N4 . 178.54(10) yes N3 . Ru1 . N4 . 91.54(10) yes N1 . Ru1 . N5 . 89.87(10) yes N2 . Ru1 . N5 . 91.06(11) yes N3 . Ru1 . N5 . 178.93(10) yes N4 . Ru1 . N5 . 87.49(10) yes N1 . Ru1 . N6 . 178.16(10) yes N2 . Ru1 . N6 . 89.34(10) yes N3 . Ru1 . N6 . 88.78(10) yes N4 . Ru1 . N6 . 90.54(10) yes N5 . Ru1 . N6 . 91.69(10) yes C1 . Re1 . C2 . 87.50(14) yes C1 . Re1 . C3 . 90.16(12) yes C2 . Re1 . C3 . 90.87(15) yes C1 . Re1 . C4 . 89.66(13) yes C2 . Re1 . C4 . 177.00(14) yes C3 . Re1 . C4 . 90.10(15) yes C1 . Re1 . C5 . 90.02(13) yes C2 . Re1 . C5 . 89.03(15) yes C3 . Re1 . C5 . 179.79(13) yes C4 . Re1 . C5 . 90.00(15) yes C1 . Re1 . C6 . 179.51(13) yes C2 . Re1 . C6 . 92.98(15) yes C3 . Re1 . C6 . 89.74(14) yes C4 . Re1 . C6 . 89.86(14) yes C5 . Re1 . C6 . 90.08(14) yes Re1 . C1 . N1 . 177.5(3) yes Re1 . C2 . O1 . 176.7(3) yes Re1 . C3 . O2 . 178.5(3) yes Re1 . C4 . O3 . 178.5(3) yes Re1 . C5 . O4 . 178.2(3) yes Re1 . C6 . O5 . 178.0(3) yes Ru1 . N1 . C1 . 175.1(3) yes Ru1 . N2 . H21 . 109.9 no Ru1 . N2 . H22 . 110.9 no H21 . N2 . H22 . 109.3 no Ru1 . N2 . H23 . 109.4 no H21 . N2 . H23 . 106.9 no H22 . N2 . H23 . 110.3 no Ru1 . N3 . H31 . 112.2 no Ru1 . N3 . H32 . 110.3 no H31 . N3 . H32 . 108.4 no Ru1 . N3 . H33 . 110.7 no H31 . N3 . H33 . 107.0 no H32 . N3 . H33 . 108.1 no Ru1 . N4 . H41 . 110.1 no Ru1 . N4 . H42 . 110.8 no H41 . N4 . H42 . 109.2 no Ru1 . N4 . H43 . 110.5 no H41 . N4 . H43 . 106.3 no H42 . N4 . H43 . 109.8 no Ru1 . N5 . H51 . 110.5 no Ru1 . N5 . H52 . 111.9 no H51 . N5 . H52 . 108.1 no Ru1 . N5 . H53 . 110.9 no H51 . N5 . H53 . 106.7 no H52 . N5 . H53 . 108.5 no Ru1 . N6 . H61 . 109.9 no Ru1 . N6 . H62 . 108.7 no H61 . N6 . H62 . 108.4 no Ru1 . N6 . H63 . 113.5 no H61 . N6 . H63 . 109.8 no H62 . N6 . H63 . 106.4 no O6 . S1 . O7 . 114.84(17) yes O6 . S1 . O8 . 115.0(2) yes O7 . S1 . O8 . 114.59(19) yes O6 . S1 . C7 . 103.46(17) yes O7 . S1 . C7 . 103.23(17) yes O8 . S1 . C7 . 103.51(18) yes O9 . S2 . O10 . 115.79(18) yes O9 . S2 . O11 . 115.17(17) yes O10 . S2 . O11 . 113.95(18) yes O9 . S2 . C8 . 102.79(17) yes O10 . S2 . C8 . 102.70(16) yes O11 . S2 . C8 . 104.01(17) yes O12 . S3 . O13 . 113.88(16) yes O12 . S3 . O14 . 116.21(17) yes O13 . S3 . O14 . 114.13(17) yes O12 . S3 . C9 . 104.12(17) yes O13 . S3 . C9 . 103.1(2) yes O14 . S3 . C9 . 103.24(17) yes S1 . C7 . F2 . 111.4(3) yes S1 . C7 . F3 . 110.6(3) yes F2 . C7 . F3 . 107.1(3) yes S1 . C7 . F1 . 111.8(3) yes F2 . C7 . F1 . 108.4(3) yes F3 . C7 . F1 . 107.3(3) yes S2 . C8 . F5 . 111.2(3) yes S2 . C8 . F4 . 111.2(3) yes F5 . C8 . F4 . 107.6(3) yes S2 . C8 . F6 . 111.6(2) yes F5 . C8 . F6 . 107.3(3) yes F4 . C8 . F6 . 107.8(3) yes S3 . C9 . F9 . 110.3(3) yes S3 . C9 . F8 . 111.6(3) yes F9 . C9 . F8 . 107.6(3) yes S3 . C9 . F7 . 111.4(3) yes F9 . C9 . F7 . 108.1(4) yes F8 . C9 . F7 . 107.6(3) yes C11 . C10 . H101 . 110.6 no C11 . C10 . H102 . 107.2 no H101 . C10 . H102 . 108.0 no C11 . C10 . H103 . 111.5 no H101 . C10 . H103 . 109.3 no H102 . C10 . H103 . 110.1 no C10 . C11 . O15 . 121.5(4) yes C10 . C11 . C12 . 118.0(3) yes O15 . C11 . C12 . 120.5(4) yes C11 . C12 . H121 . 110.6 no C11 . C12 . H122 . 108.8 no H121 . C12 . H122 . 108.7 no C11 . C12 . H123 . 110.1 no H121 . C12 . H123 . 110.1 no H122 . C12 . H123 . 108.5 no C14 . C13 . H131 . 108.8 no C14 . C13 . H132 . 109.9 no H131 . C13 . H132 . 109.8 no C14 . C13 . H133 . 109.2 no H131 . C13 . H133 . 109.0 no H132 . C13 . H133 . 110.2 no C13 . C14 . O16 . 121.2(4) yes C13 . C14 . C15 . 118.0(4) yes O16 . C14 . C15 . 120.8(4) yes C14 . C15 . H151 . 110.0 no C14 . C15 . H152 . 109.1 no H151 . C15 . H152 . 110.7 no C14 . C15 . H153 . 108.5 no H151 . C15 . H153 . 109.4 no H152 . C15 . H153 . 109.1 no C17 . C16 . H161 . 109.9 no C17 . C16 . H162 . 110.4 no H161 . C16 . H162 . 109.3 no C17 . C16 . H163 . 109.6 no H161 . C16 . H163 . 108.2 no H162 . C16 . H163 . 109.4 no C16 . C17 . O17 . 119.5(6) yes C16 . C17 . C18 . 116.0(5) yes O17 . C17 . C18 . 124.5(6) yes C17 . C18 . H181 . 111.4 no C17 . C18 . H182 . 109.8 no H181 . C18 . H182 . 109.1 no C17 . C18 . H183 . 108.6 no H181 . C18 . H183 . 108.9 no H182 . C18 . H183 . 109.0 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag N2 . H21 . O10 2_665 149 0.89 2.34 3.133(6) yes N2 . H22 . O7 . 126 0.87 2.47 3.062(6) yes N2 . H22 . O13 3_655 142 0.87 2.39 3.121(6) yes N2 . H23 . O9 . 164 0.88 2.12 2.980(6) yes N3 . H31 . O8 . 153 0.87 2.47 3.273(6) yes N3 . H32 . O15 . 165 0.88 2.10 2.962(6) yes N3 . H33 . O13 3_655 151 0.86 2.43 3.209(6) yes N3 . H33 . O14 3_655 148 0.86 2.35 3.114(6) yes N4 . H41 . O15 . 154 0.89 2.08 2.909(6) yes N4 . H42 . O13 . 159 0.88 2.14 2.985(6) yes N4 . H43 . O6 3_645 154 0.90 2.18 3.015(6) yes N5 . H51 . O6 3_645 156 0.88 2.38 3.205(6) yes N5 . H52 . O11 . 172 0.88 2.15 3.018(6) yes N5 . H53 . O12 . 149 0.86 2.51 3.279(6) yes N6 . H61 . O16 . 151 0.87 2.20 2.995(6) yes N6 . H62 . O7 . 154 0.88 2.22 3.046(6) yes N6 . H63 . O10 2_665 122 0.87 2.44 2.992(6) yes N6 . H63 . O12 . 140 0.87 2.33 3.052(6) yes C13 . H131 . O14 4_555 160 0.96 2.51 3.423(6) yes data_3-water _database_code_depnum_ccdc_archive 'CCDC 914948' #TrackingRef 'CrystallographicData.cif' #============================================================================== _audit_creation_date 08-10-30 _audit_creation_method CRYSTALS_ver_12.86 _oxford_structure_analysis_title 5997 _chemical_name_systematic . _chemical_melting_point 'not measured' _cell_length_a 8.1564(2) _cell_length_b 14.5998(3) _cell_length_c 26.8390(5) _cell_angle_alpha 90 _cell_angle_beta 92.2195(8) _cell_angle_gamma 90 _cell_volume 3193.64(12) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1 ' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y+1/2,-z+1/2 x,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' F 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Re -1.0185 7.2310 28.7621 1.6719 15.7189 9.0923 14.5564 0.3505 5.4417 52.0861 10.4720 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Ru -1.2594 0.8363 19.2674 0.8085 12.9182 8.4347 4.8634 24.7997 1.5676 94.2928 5.3787 'International Tables Vol C 4.2.6.8 and 6.1.1.4' S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C9 H15 F9 N6 O14 Re1 Ru1 S3 # Dc = 2.05 Fooo = 2004.00 Mu = 45.70 M = 985.70 # Found Formula = C9 H21 F9 N6 O17 Re1 Ru1 S3 # Dc = 2.16 FOOO = 2004.00 Mu = 45.82 M = 1039.75 _chemical_formula_sum 'C9 H21 F9 N6 O17 Re1 Ru1 S3' _chemical_formula_moiety 'C6 H15 N6 O5 Re Ru, 3(C F3 O3 S), 3(H2 O)' _chemical_compound_source . _chemical_formula_weight 1039.75 _cell_measurement_reflns_used 6937 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description plate _exptl_crystal_colour clear_pale_yellow _exptl_crystal_size_min 0.02 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_max 0.23 _exptl_crystal_density_diffrn 2.162 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 2004 _exptl_absorpt_coefficient_mu 4.582 # Sheldrick geometric approximatio 0.66 0.91 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.60 _exptl_absorpt_correction_T_max 0.91 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device 'Nonius KappaCCD' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% . _diffrn_ambient_temperature 150 _diffrn_reflns_number 30746 _reflns_number_total 7213 _diffrn_reflns_av_R_equivalents 0.069 # Number of reflections with Friedels Law is 7213 # Number of reflections without Friedels Law is 13426 # Theoretical number of reflections is about 7356 _diffrn_reflns_theta_min 5.117 _diffrn_reflns_theta_max 27.526 _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.324 _diffrn_measured_fraction_theta_full 0.990 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _reflns_limit_h_min -10 _reflns_limit_h_max 10 _reflns_limit_k_min 0 _reflns_limit_k_max 18 _reflns_limit_l_min 0 _reflns_limit_l_max 34 _oxford_diffrn_Wilson_B_factor 2.10 _oxford_diffrn_Wilson_scale 102.81 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.12 _refine_diff_density_max 1.57 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>2.0\s(I) _refine_ls_number_reflns 4920 _refine_ls_number_restraints 163 _refine_ls_number_parameters 415 _oxford_refine_ls_R_factor_ref 0.0401 _refine_ls_wR_factor_ref 0.0395 _refine_ls_goodness_of_fit_ref 1.1145 _refine_ls_shift/su_max 0.002574 # The values computed from all data _oxford_reflns_number_all 7212 _refine_ls_R_factor_all 0.0749 _refine_ls_wR_factor_all 0.0668 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 4920 _refine_ls_R_factor_gt 0.0401 _refine_ls_wR_factor_gt 0.0395 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment none # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.525 0.112 0.288 ; # Insert your own references if required - in alphabetical order 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Re1 Re 0.66927(3) 0.71775(2) 0.951713(9) 0.0300 1.0000 Uani . U . . . . . Ru1 Ru 0.73582(5) 0.72081(3) 0.756717(15) 0.0202 1.0000 Uani . U . . . . . C1 C 0.7090(7) 0.7151(5) 0.8745(2) 0.0278 1.0000 Uani . U . . . . . C2 C 0.6912(9) 0.8541(5) 0.9488(2) 0.0340 1.0000 Uani . U . . . . . C3 C 0.9065(9) 0.7003(6) 0.9693(2) 0.0475 1.0000 Uani . U . . . . . C4 C 0.6464(10) 0.5801(5) 0.9507(3) 0.0407 1.0000 Uani . U . . . . . C5 C 0.4287(8) 0.7280(5) 0.9327(2) 0.0308 1.0000 Uani . U . . . . . C6 C 0.6284(8) 0.7257(5) 1.0237(2) 0.0337 1.0000 Uani . U . . . . . O1 O 0.7122(9) 0.9316(4) 0.9466(2) 0.0665 1.0000 Uani . U . . . . . O2 O 1.0379(7) 0.6868(7) 0.9808(2) 0.0898 1.0000 Uani . U . . . . . O3 O 0.6371(8) 0.5032(4) 0.9495(2) 0.0569 1.0000 Uani . U . . . . . O4 O 0.2953(6) 0.7303(4) 0.9223(2) 0.0445 1.0000 Uani . U . . . . . O5 O 0.6053(7) 0.7338(4) 1.06525(17) 0.0466 1.0000 Uani . U . . . . . N1 N 0.7227(6) 0.7156(4) 0.83197(17) 0.0252 1.0000 Uani . U . . . . . N2 N 0.5642(6) 0.6142(3) 0.74835(18) 0.0256 1.0000 Uani . U . . . . . N3 N 0.9221(6) 0.6216(4) 0.76116(19) 0.0267 1.0000 Uani . U . . . . . N4 N 0.9060(6) 0.8284(3) 0.76405(18) 0.0248 1.0000 Uani . U . . . . . N5 N 0.5467(6) 0.8185(3) 0.75416(19) 0.0259 1.0000 Uani . U . . . . . N6 N 0.7519(6) 0.7260(3) 0.67870(16) 0.0232 1.0000 Uani . U . . . . . S1 S 0.20375(17) 0.71364(11) 0.65846(5) 0.0262 1.0000 Uani . . . . . . . O6 O 0.3773(5) 0.7179(4) 0.66802(16) 0.0373 1.0000 Uani . . . . . . . O7 O 0.1119(5) 0.7915(3) 0.67577(17) 0.0344 1.0000 Uani . . . . . . . O8 O 0.1281(6) 0.6268(3) 0.66903(17) 0.0346 1.0000 Uani . . . . . . . C7 C 0.1799(8) 0.7236(5) 0.5907(2) 0.0335 1.0000 Uani . . . . . . . F1 F 0.0208(5) 0.7195(3) 0.57702(15) 0.0467 1.0000 Uani . . . . . . . F2 F 0.2580(6) 0.6566(4) 0.56801(16) 0.0540 1.0000 Uani . . . . . . . F3 F 0.2388(5) 0.8026(3) 0.57523(15) 0.0472 1.0000 Uani . . . . . . . S2 S 0.2993(2) 0.48819(11) 0.84541(6) 0.0295 1.0000 Uani . . . . . . . O9 O 0.4039(6) 0.4100(3) 0.85275(19) 0.0404 1.0000 Uani . . . . . . . O10 O 0.1822(7) 0.4819(4) 0.80443(18) 0.0446 1.0000 Uani . . . . . . . O11 O 0.3844(6) 0.5749(3) 0.84972(18) 0.0382 1.0000 Uani . . . . . . . C8 C 0.1714(9) 0.4878(5) 0.8995(3) 0.0389 1.0000 Uani . . . . . . . F4 F 0.0587(6) 0.5548(4) 0.89541(19) 0.0594 1.0000 Uani . . . . . . . F5 F 0.2586(6) 0.5022(4) 0.94159(16) 0.0567 1.0000 Uani . . . . . . . F6 F 0.0937(7) 0.4083(4) 0.9035(2) 0.0698 1.0000 Uani . . . . . . . S3 S 0.2509(2) 0.94559(11) 0.86448(6) 0.0334 1.0000 Uani . . . . . . . O12 O 0.1251(6) 0.8765(4) 0.8556(2) 0.0449 1.0000 Uani . . . . . . . O13 O 0.2390(7) 1.0241(4) 0.83209(19) 0.0486 1.0000 Uani . . . . . . . O14 O 0.4120(6) 0.9073(4) 0.8717(2) 0.0495 1.0000 Uani . . . . . . . C9 C 0.2025(14) 0.9898(6) 0.9257(3) 0.0604 1.0000 Uani . . . . . . . F7 F 0.2990(11) 1.0605(5) 0.9374(2) 0.1130 1.0000 Uani . . . . . . . F8 F 0.2238(9) 0.9271(4) 0.96030(17) 0.0840 1.0000 Uani . . . . . . . F9 F 0.0513(9) 1.0190(4) 0.9264(2) 0.0929 1.0000 Uani . . . . . . . O15 O 0.2382(5) 0.7252(3) 0.79984(17) 0.0363 1.0000 Uani . . . . . . . O16 O 0.7389(7) 0.4696(4) 0.8145(2) 0.0535 1.0000 Uani . . . . . . . O17 O 0.6832(7) 0.9634(4) 0.8175(2) 0.0524 1.0000 Uani . . . . . . . H21 H 0.4813 0.6324 0.7284 0.0383 1.0000 Uiso R . . . . . . H22 H 0.6118 0.5656 0.7351 0.0382 1.0000 Uiso R . . . . . . H23 H 0.5269 0.5994 0.7778 0.0381 1.0000 Uiso R . . . . . . H31 H 0.9456 0.6029 0.7308 0.0411 1.0000 Uiso R . . . . . . H32 H 0.8888 0.5737 0.7786 0.0409 1.0000 Uiso R . . . . . . H33 H 1.0117 0.6448 0.7761 0.0411 1.0000 Uiso R . . . . . . H41 H 0.9171 0.8451 0.7959 0.0351 1.0000 Uiso R . . . . . . H42 H 0.8724 0.8763 0.7456 0.0350 1.0000 Uiso R . . . . . . H43 H 1.0029 0.8099 0.7538 0.0352 1.0000 Uiso R . . . . . . H51 H 0.5795 0.8687 0.7708 0.0380 1.0000 Uiso R . . . . . . H52 H 0.4569 0.7959 0.7675 0.0381 1.0000 Uiso R . . . . . . H53 H 0.5231 0.8336 0.7226 0.0383 1.0000 Uiso R . . . . . . H61 H 0.8449 0.7527 0.6706 0.0352 1.0000 Uiso R . . . . . . H62 H 0.6682 0.7573 0.6649 0.0354 1.0000 Uiso R . . . . . . H63 H 0.7507 0.6698 0.6662 0.0350 1.0000 Uiso R . . . . . . H151 H 0.2807 0.6851 0.8173 0.0552 1.0000 Uiso R . . . . . . H152 H 0.2038 0.7640 0.8188 0.0551 1.0000 Uiso R . . . . . . H161 H 0.6581 0.4671 0.8316 0.0790 1.0000 Uiso R . . . . . . H162 H 0.8000 0.4265 0.8216 0.0789 1.0000 Uiso R . . . . . . H171 H 0.6208 0.9610 0.8407 0.0779 1.0000 Uiso R . . . . . . H172 H 0.7408 1.0081 0.8243 0.0779 1.0000 Uiso 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 0.03211(13) 0.03818(14) 0.01973(11) -0.00152(12) 0.00173(8) -0.00296(13) Ru1 0.0208(2) 0.0213(2) 0.01839(19) -0.00020(19) 0.00036(16) -0.00003(19) C1 0.028(3) 0.035(3) 0.0212(13) -0.005(2) 0.0015(19) -0.002(3) C2 0.051(4) 0.0405(15) 0.011(2) -0.005(2) -0.003(2) -0.013(3) C3 0.0359(18) 0.083(5) 0.023(3) -0.007(3) -0.002(2) 0.001(3) C4 0.054(4) 0.0382(15) 0.030(3) 0.000(2) -0.001(3) 0.006(3) C5 0.0336(15) 0.033(3) 0.026(3) 0.004(3) 0.0018(19) -0.005(2) C6 0.040(3) 0.039(3) 0.0222(15) 0.005(2) 0.005(2) 0.009(3) O1 0.106(5) 0.044(2) 0.048(3) -0.002(3) -0.004(3) -0.031(3) O2 0.034(2) 0.189(9) 0.045(3) -0.031(4) -0.002(2) 0.011(4) O3 0.076(4) 0.0391(18) 0.054(3) 0.003(3) -0.015(3) 0.005(3) O4 0.0334(18) 0.044(3) 0.056(3) 0.007(3) 0.001(2) -0.002(2) O5 0.057(3) 0.058(3) 0.0247(17) 0.002(2) 0.011(2) 0.009(3) N1 0.021(2) 0.035(3) 0.0201(12) -0.003(2) 0.0018(16) -0.001(2) N2 0.029(2) 0.021(2) 0.027(2) 0.0011(19) 0.001(2) -0.0033(16) N3 0.024(2) 0.027(2) 0.028(2) -0.003(2) -0.0016(19) 0.0027(16) N4 0.022(2) 0.025(2) 0.027(2) 0.0024(19) -0.0030(18) -0.0023(16) N5 0.026(2) 0.021(2) 0.030(2) -0.0024(19) -0.0029(19) 0.0021(15) N6 0.027(2) 0.023(2) 0.0203(14) 0.0007(18) 0.0038(16) -0.001(2) S1 0.0239(7) 0.0278(7) 0.0267(7) 0.0000(6) 0.0009(5) -0.0003(7) O6 0.025(2) 0.055(3) 0.032(2) 0.005(2) -0.0040(17) 0.000(2) O7 0.029(2) 0.036(3) 0.039(2) -0.007(2) 0.0073(18) 0.001(2) O8 0.038(3) 0.028(2) 0.038(2) 0.0061(19) 0.009(2) -0.0015(19) C7 0.034(3) 0.037(3) 0.029(3) 0.001(3) -0.003(2) -0.001(3) F1 0.038(2) 0.059(3) 0.042(2) 0.008(2) -0.0158(17) -0.006(2) F2 0.058(3) 0.066(3) 0.039(2) -0.014(2) 0.008(2) 0.010(2) F3 0.048(2) 0.052(3) 0.041(2) 0.0148(19) 0.0010(19) -0.015(2) S2 0.0348(9) 0.0239(8) 0.0297(7) -0.0008(6) -0.0001(6) 0.0007(6) O9 0.039(3) 0.035(3) 0.047(3) 0.002(2) -0.002(2) 0.010(2) O10 0.057(3) 0.042(3) 0.034(2) -0.004(2) -0.011(2) 0.003(2) O11 0.040(3) 0.030(2) 0.045(3) 0.001(2) 0.006(2) -0.006(2) C8 0.037(4) 0.036(4) 0.044(4) -0.007(3) 0.005(3) -0.007(3) F4 0.049(3) 0.065(3) 0.065(3) -0.016(3) 0.013(2) 0.014(2) F5 0.065(3) 0.072(3) 0.033(2) -0.003(2) 0.001(2) -0.004(3) F6 0.069(3) 0.060(3) 0.082(4) -0.002(3) 0.025(3) -0.028(3) S3 0.0401(9) 0.0288(8) 0.0313(8) 0.0021(7) 0.0001(7) 0.0027(7) O12 0.045(3) 0.039(3) 0.050(3) -0.006(2) -0.004(2) -0.006(2) O13 0.066(4) 0.041(3) 0.040(3) 0.012(2) 0.014(3) 0.010(3) O14 0.032(3) 0.049(3) 0.067(4) 0.022(3) 0.000(2) 0.004(2) C9 0.096(8) 0.043(5) 0.043(5) -0.002(4) 0.009(5) -0.001(5) F7 0.205(8) 0.067(4) 0.066(4) -0.026(3) -0.003(5) -0.049(5) F8 0.156(6) 0.062(3) 0.034(3) 0.010(2) 0.008(3) 0.008(4) F9 0.131(6) 0.076(4) 0.075(4) 0.003(3) 0.047(4) 0.046(4) O15 0.037(2) 0.033(3) 0.038(2) -0.002(2) -0.0029(19) 0.006(2) O16 0.043(3) 0.044(3) 0.074(4) 0.020(3) 0.006(3) 0.011(2) O17 0.058(3) 0.045(3) 0.055(3) -0.020(3) 0.019(3) -0.018(3) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.10281(13) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Re1 . C1 . 2.109(6) yes Re1 . C2 . 2.001(7) yes Re1 . C3 . 1.990(7) yes Re1 . C4 . 2.019(8) yes Re1 . C5 . 2.013(6) yes Re1 . C6 . 1.978(6) yes Ru1 . N1 . 2.028(5) yes Ru1 . N2 . 2.100(5) yes Ru1 . N3 . 2.100(5) yes Ru1 . N4 . 2.100(5) yes Ru1 . N5 . 2.100(5) yes Ru1 . N6 . 2.104(4) yes C1 . N1 . 1.152(7) yes C2 . O1 . 1.146(9) yes C3 . O2 . 1.121(9) yes C4 . O3 . 1.125(9) yes C5 . O4 . 1.114(8) yes C6 . O5 . 1.143(8) yes N2 . H21 . 0.888 no N2 . H22 . 0.888 no N2 . H23 . 0.884 no N3 . H31 . 0.888 no N3 . H32 . 0.888 no N3 . H33 . 0.886 no N4 . H41 . 0.889 no N4 . H42 . 0.894 no N4 . H43 . 0.890 no N5 . H51 . 0.893 no N5 . H52 . 0.891 no N5 . H53 . 0.889 no N6 . H61 . 0.888 no N6 . H62 . 0.889 no N6 . H63 . 0.886 no S1 . O6 . 1.430(4) yes S1 . O7 . 1.448(5) yes S1 . O8 . 1.443(5) yes S1 . C7 . 1.828(6) yes C7 . F1 . 1.336(7) yes C7 . F2 . 1.328(8) yes C7 . F3 . 1.322(8) yes S2 . O9 . 1.434(5) yes S2 . O10 . 1.432(5) yes S2 . O11 . 1.446(5) yes S2 . C8 . 1.820(7) yes C8 . F4 . 1.343(9) yes C8 . F5 . 1.329(8) yes C8 . F6 . 1.329(8) yes S3 . O12 . 1.452(5) yes S3 . O13 . 1.440(5) yes S3 . O14 . 1.434(5) yes S3 . C9 . 1.824(9) yes C9 . F7 . 1.328(11) yes C9 . F8 . 1.310(10) yes C9 . F9 . 1.306(12) yes O15 . H151 . 0.818 no O15 . H152 . 0.818 no O16 . H161 . 0.819 no O16 . H162 . 0.821 no O17 . H171 . 0.821 no O17 . H172 . 0.821 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C1 . Re1 . C2 . 87.8(3) yes C1 . Re1 . C3 . 92.6(2) yes C2 . Re1 . C3 . 92.8(3) yes C1 . Re1 . C4 . 89.3(3) yes C2 . Re1 . C4 . 177.0(2) yes C3 . Re1 . C4 . 87.9(3) yes C1 . Re1 . C5 . 86.4(2) yes C2 . Re1 . C5 . 90.2(3) yes C3 . Re1 . C5 . 176.8(3) yes C4 . Re1 . C5 . 89.0(3) yes C1 . Re1 . C6 . 177.5(3) yes C2 . Re1 . C6 . 89.9(3) yes C3 . Re1 . C6 . 88.6(3) yes C4 . Re1 . C6 . 93.0(3) yes C5 . Re1 . C6 . 92.5(3) yes N1 . Ru1 . N2 . 91.0(2) yes N1 . Ru1 . N3 . 89.1(2) yes N2 . Ru1 . N3 . 88.4(2) yes N1 . Ru1 . N4 . 89.7(2) yes N2 . Ru1 . N4 . 179.10(19) yes N3 . Ru1 . N4 . 92.1(2) yes N1 . Ru1 . N5 . 89.5(2) yes N2 . Ru1 . N5 . 90.84(19) yes N3 . Ru1 . N5 . 178.3(2) yes N4 . Ru1 . N5 . 88.7(2) yes N1 . Ru1 . N6 . 179.45(18) yes N2 . Ru1 . N6 . 89.28(19) yes N3 . Ru1 . N6 . 90.51(19) yes N4 . Ru1 . N6 . 89.98(19) yes N5 . Ru1 . N6 . 90.96(19) yes Re1 . C1 . N1 . 176.5(5) yes Re1 . C2 . O1 . 176.4(7) yes Re1 . C3 . O2 . 176.3(8) yes Re1 . C4 . O3 . 178.3(7) yes Re1 . C5 . O4 . 177.5(6) yes Re1 . C6 . O5 . 177.4(6) yes Ru1 . N1 . C1 . 176.9(5) yes Ru1 . N2 . H21 . 109.4 no Ru1 . N2 . H22 . 109.5 no H21 . N2 . H22 . 109.4 no Ru1 . N2 . H23 . 109.6 no H21 . N2 . H23 . 109.4 no H22 . N2 . H23 . 109.5 no Ru1 . N3 . H31 . 109.9 no Ru1 . N3 . H32 . 109.7 no H31 . N3 . H32 . 108.9 no Ru1 . N3 . H33 . 110.1 no H31 . N3 . H33 . 109.2 no H32 . N3 . H33 . 109.1 no Ru1 . N4 . H41 . 109.7 no Ru1 . N4 . H42 . 110.3 no H41 . N4 . H42 . 109.5 no Ru1 . N4 . H43 . 109.6 no H41 . N4 . H43 . 108.8 no H42 . N4 . H43 . 108.9 no Ru1 . N5 . H51 . 109.6 no Ru1 . N5 . H52 . 110.4 no H51 . N5 . H52 . 109.7 no Ru1 . N5 . H53 . 109.3 no H51 . N5 . H53 . 108.8 no H52 . N5 . H53 . 108.9 no Ru1 . N6 . H61 . 110.3 no Ru1 . N6 . H62 . 110.9 no H61 . N6 . H62 . 108.8 no Ru1 . N6 . H63 . 110.0 no H61 . N6 . H63 . 108.1 no H62 . N6 . H63 . 108.7 no O6 . S1 . O7 . 115.4(3) yes O6 . S1 . O8 . 115.5(3) yes O7 . S1 . O8 . 113.3(3) yes O6 . S1 . C7 . 104.0(3) yes O7 . S1 . C7 . 102.7(3) yes O8 . S1 . C7 . 103.7(3) yes S1 . C7 . F1 . 109.5(4) yes S1 . C7 . F2 . 111.2(5) yes F1 . C7 . F2 . 108.6(6) yes S1 . C7 . F3 . 110.8(5) yes F1 . C7 . F3 . 108.3(6) yes F2 . C7 . F3 . 108.2(5) yes O9 . S2 . O10 . 115.5(3) yes O9 . S2 . O11 . 113.9(3) yes O10 . S2 . O11 . 114.9(3) yes O9 . S2 . C8 . 104.2(3) yes O10 . S2 . C8 . 103.1(3) yes O11 . S2 . C8 . 103.1(3) yes S2 . C8 . F4 . 110.1(5) yes S2 . C8 . F5 . 111.9(5) yes F4 . C8 . F5 . 107.2(6) yes S2 . C8 . F6 . 111.0(5) yes F4 . C8 . F6 . 108.4(6) yes F5 . C8 . F6 . 108.1(6) yes O12 . S3 . O13 . 115.0(3) yes O12 . S3 . O14 . 112.9(3) yes O13 . S3 . O14 . 115.6(3) yes O12 . S3 . C9 . 102.6(4) yes O13 . S3 . C9 . 104.5(4) yes O14 . S3 . C9 . 104.2(4) yes S3 . C9 . F7 . 109.9(7) yes S3 . C9 . F8 . 111.3(6) yes F7 . C9 . F8 . 108.4(8) yes S3 . C9 . F9 . 111.4(7) yes F7 . C9 . F9 . 107.1(8) yes F8 . C9 . F9 . 108.5(8) yes H151 . O15 . H152 . 106.7 no H161 . O16 . H162 . 109.2 no H171 . O17 . H172 . 103.3 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag N2 . H21 . O6 . 152 0.89 2.19 3.002(10) yes N2 . H22 . O13 3_646 141 0.89 2.30 3.039(10) yes N2 . H23 . O11 . 169 0.88 2.32 3.192(10) yes N3 . H31 . O8 1_655 142 0.89 2.30 3.043(10) yes N3 . H31 . O13 3_646 128 0.89 2.50 3.124(10) yes N3 . H32 . O16 . 164 0.89 2.20 3.061(10) yes N3 . H33 . O15 1_655 168 0.89 2.26 3.132(10) yes N4 . H41 . O12 1_655 139 0.89 2.33 3.064(10) yes N4 . H42 . O10 3_656 172 0.89 2.08 2.969(10) yes N4 . H43 . O7 1_655 134 0.89 2.32 3.006(10) yes N4 . H43 . O15 1_655 131 0.89 2.56 3.215(10) yes N5 . H51 . O17 . 168 0.89 2.03 2.907(10) yes N5 . H52 . O15 . 175 0.89 2.26 3.151(10) yes N5 . H53 . O9 3_656 150 0.89 2.40 3.204(10) yes N6 . H61 . O7 1_655 158 0.89 2.25 3.092(10) yes N6 . H62 . O6 . 127 0.89 2.45 3.060(10) yes N6 . H62 . O9 3_656 139 0.89 2.35 3.076(10) yes N6 . H63 . O13 3_646 157 0.89 2.13 2.964(10) yes O15 . H151 . O11 . 171 0.82 2.00 2.812(10) yes O15 . H152 . O12 . 170 0.82 2.03 2.842(10) yes O16 . H161 . O9 . 154 0.82 2.32 3.081(10) yes O16 . H162 . O7 3_646 159 0.82 2.10 2.879(10) yes O17 . H171 . O14 . 150 0.82 2.08 2.817(10) yes O17 . H172 . O8 3_656 171 0.82 2.04 2.855(10) yes