# Electronic Supplementary Material (ESI) for Physical Chemistry Chemical Physics # This journal is © The Owner Societies 2011 data_global _journal_name_full 'Energy Environ.Sci.' _journal_coden_cambridge 1148 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name _publ_author_address N.Planas ;Institute of Chemical Research of Catalonia (ICIQ) Avd. Paisos Catalans 16 E-43007 Tarragona, Spain ; T.Ono ;Institute of Chemical Research of Catalonia (ICIQ) Avd. Paisos Catalans 16 E-43007 Tarragona, Spain ; L.Vaquer ;Institute of Chemical Research of Catalonia (ICIQ) Avd. Paisos Catalans 16 E-43007 Tarragona, Spain ; P.Miro ;Department of Chemistry and Supercomputing Institute University of Minnesota 207 Pleasant St. SE Minneapolis; MN 55455-0431 (USA) Avd. Paisos Catalans 16 E-43007 Tarragona, Spain ; J.Benet-Buchholz ;X-ray Diffraction Unit Institute of Chemical Research of Catalonia (ICIQ) Avd. Paisos Catalans 16 E-43007 Tarragona, Spain ; L.Gagliardi ;Department of Chemistry and Supercomputing Institute University of Minnesota 207 Pleasant St. SE Minneapolis; MN 55455-0431 (USA) Avd. Paisos Catalans 16 E-43007 Tarragona, Spain ; ; C.Cramer ; ;Department of Chemistry and Supercomputing Institute University of Minnesota 207 Pleasant St. SE Minneapolis; MN 55455-0431 (USA) Avd. Paisos Catalans 16 E-43007 Tarragona, Spain ; A.Llobet ;Institute of Chemical Research of Catalonia (ICIQ) Avd. Paisos Catalans 16 E-43007 Tarragona, Spain ; #TrackingRef '- LV009Rub_0m.cif' _publ_contact_author ; Dr. Benet-Buchholz, Jordi Institute of Chemical Research of Catalonia (ICIQ) X-ray Diffraction Unit Avgda. Pa\=isos Catalans 16 E-43007 Tarragona, Spain ; _publ_contact_author_email jbenet@iciq.es _publ_contact_author_fax '+34 977 920 224' _publ_contact_author_phone '+34 977 920 204' _publ_contact_letter ; ? ; _publ_requested_coeditor_name ? #------------------------------------------------------------------------- #3 Publication details _publ_section_title ; Carbon Dioxide Reduction by Mononuclear Ruthenium Polypyridyl Complexes ; _publ_contact_author_name 'Dr. Benet-Buchholz, Jordi' data_lv009rub_0m _database_code_depnum_ccdc_archive 'CCDC 833745' _ccdc_compound_id 1 _ccdc_biological_activity ? _ccdc_polymorph ? _ccdc_chemdiag_type ? _ccdc_chemdiag_records ? _ccdc_disorder ? _ccdc_comments ? _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H22 Cl3 N7 Ru' _chemical_formula_weight 675.96 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 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 9.2018(4) _cell_length_b 17.8945(8) _cell_length_c 16.4125(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.386(2) _cell_angle_gamma 90.00 _cell_volume 2702.4(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9886 _cell_measurement_theta_min 2.49 _cell_measurement_theta_max 36.39 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.661 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1360 _exptl_absorpt_coefficient_mu 0.912 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.81 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ; SADABS Version 2008/1 Bruker-Nonius Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_special_details ; It should be noted that the esd's of the cell dimensions are probably too low; they should be multiplied by a factor of 2 to 10 ; _diffrn_ambient_temperature 100(2) _diffrn_measurement_specimen_suppport 'magnetic support whith 10 micron nylon fiber cryoloop' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'rotating anode X-ray tube' _diffrn_source_type 'Bruker-Nonius FR 591' _diffrn_source_power 50 _diffrn_source_current 70 _diffrn_source_size '3 mm x 0.3 mm fine focus' _diffrn_radiation_monochromator 'Multilayer Montel 200 mirrors' _diffrn_detector_type '4K CCD area detector APEX II' _diffrn_measurement_device_type 'Kappa 4-axis goniometer bruker-nonius' _diffrn_measurement_method ; Fullsphere data collection, phi and omega scans ; _diffrn_detector_area_resol_mean 512 _diffrn_reflns_number 57966 _diffrn_reflns_av_R_equivalents 0.0331 _diffrn_reflns_av_sigmaI/netI 0.0278 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 36.53 _reflns_number_total 12963 _reflns_number_gt 11264 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 v2009.1-0' _computing_cell_refinement 'Bruker APEX2 v2009.1-0' _computing_data_reduction 'Bruker SAINT V7.60A' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXS-97 (Sheldrick, 2008)' _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^)+(0.0439P)^2^+1.7450P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12963 _refine_ls_number_parameters 361 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0392 _refine_ls_R_factor_gt 0.0310 _refine_ls_wR_factor_ref 0.0971 _refine_ls_wR_factor_gt 0.0864 _refine_ls_goodness_of_fit_ref 1.184 _refine_ls_restrained_S_all 1.184 _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 C1 C 0.30414(17) 0.24864(8) 0.96932(9) 0.0156(2) Uani 1 1 d . . . H1A H 0.3675 0.2901 0.9767 0.019 Uiso 1 1 calc R . . C2 C 0.18753(18) 0.24296(9) 1.02170(10) 0.0190(3) Uani 1 1 d . . . H2A H 0.1725 0.2792 1.0630 0.023 Uiso 1 1 calc R . . C3 C 0.09253(19) 0.18274(10) 1.01242(10) 0.0213(3) Uani 1 1 d . . . H3A H 0.0131 0.1757 1.0483 0.026 Uiso 1 1 calc R . . C4 C 0.11821(17) 0.13385(9) 0.94937(10) 0.0190(3) Uani 1 1 d . . . H4A H 0.0531 0.0934 0.9406 0.023 Uiso 1 1 calc R . . C5 C 0.24020(16) 0.14241(8) 0.89685(8) 0.0143(2) Uani 1 1 d . . . C7 C 0.35569(16) 0.08112(7) 0.78510(8) 0.0134(2) Uani 1 1 d . . . C8 C 0.35291(16) 0.02324(7) 0.72093(8) 0.0138(2) Uani 1 1 d . . . C9 C 0.25516(17) -0.03330(8) 0.70313(9) 0.0162(2) Uani 1 1 d . . . H9A H 0.1682 -0.0394 0.7333 0.019 Uiso 1 1 calc R . . C10 C 0.29026(18) -0.08120(8) 0.63852(10) 0.0179(2) Uani 1 1 d . . . H10A H 0.2266 -0.1214 0.6257 0.021 Uiso 1 1 calc R . . C11 C 0.41647(18) -0.07163(8) 0.59225(10) 0.0185(3) Uani 1 1 d . . . H11A H 0.4359 -0.1047 0.5484 0.022 Uiso 1 1 calc R . . C12 C 0.51409(17) -0.01383(8) 0.61011(9) 0.0176(2) Uani 1 1 d . . . H12A H 0.5996 -0.0065 0.5790 0.021 Uiso 1 1 calc R . . C13 C 0.48005(16) 0.03240(8) 0.67552(9) 0.0148(2) Uani 1 1 d . . . C14 C 0.56160(16) 0.09391(8) 0.71387(8) 0.0145(2) Uani 1 1 d . . . C15 C 0.78016(16) 0.16351(8) 0.72572(9) 0.0158(2) Uani 1 1 d . . . C16 C 0.92369(18) 0.16261(10) 0.69440(11) 0.0222(3) Uani 1 1 d . . . H17A H 0.9455 0.1313 0.6494 0.027 Uiso 1 1 calc R . . C17 C 1.03126(18) 0.20600(9) 0.72787(11) 0.0208(3) Uani 1 1 d . . . H18A H 1.1280 0.2043 0.7080 0.025 Uiso 1 1 calc R . . C18 C 0.99322(17) 0.25279(9) 0.79217(10) 0.0188(3) Uani 1 1 d . . . H19A H 1.0639 0.2844 0.8169 0.023 Uiso 1 1 calc R . . C19 C 0.85148(17) 0.25276(9) 0.81966(9) 0.0171(2) Uani 1 1 d . . . H20A H 0.8284 0.2855 0.8632 0.021 Uiso 1 1 calc R . . C20 C 0.63173(18) 0.07810(8) 0.94632(9) 0.0173(2) Uani 1 1 d . . . H1B H 0.5960 0.0490 0.9021 0.021 Uiso 1 1 calc R . . C21 C 0.68913(19) 0.04194(9) 1.01316(10) 0.0217(3) Uani 1 1 d . . . H2B H 0.6943 -0.0111 1.0146 0.026 Uiso 1 1 calc R . . C22 C 0.73910(19) 0.08391(10) 1.07817(10) 0.0226(3) Uani 1 1 d . . . H3B H 0.7785 0.0602 1.1251 0.027 Uiso 1 1 calc R . . C23 C 0.73092(18) 0.16109(10) 1.07392(9) 0.0197(3) Uani 1 1 d . . . H4B H 0.7633 0.1908 1.1184 0.024 Uiso 1 1 calc R . . C24 C 0.67506(16) 0.19480(8) 1.00414(8) 0.0150(2) Uani 1 1 d . . . C25 C 0.66604(17) 0.27582(8) 0.99173(9) 0.0156(2) Uani 1 1 d . . . C26 C 0.72390(19) 0.32865(10) 1.04529(9) 0.0213(3) Uani 1 1 d . . . H7B H 0.7748 0.3132 1.0929 0.026 Uiso 1 1 calc R . . C27 C 0.7063(2) 0.40410(10) 1.02825(11) 0.0246(3) Uani 1 1 d . . . H8B H 0.7432 0.4409 1.0646 0.030 Uiso 1 1 calc R . . C28 C 0.63435(19) 0.42508(9) 0.95771(11) 0.0221(3) Uani 1 1 d . . . H9B H 0.6192 0.4764 0.9455 0.026 Uiso 1 1 calc R . . C29 C 0.58473(17) 0.37024(8) 0.90514(10) 0.0173(2) Uani 1 1 d . . . H10B H 0.5386 0.3849 0.8557 0.021 Uiso 1 1 calc R . . C1D C 0.7369(2) 0.40539(13) 0.70968(14) 0.0327(4) Uani 1 1 d . . . H1D1 H 0.6831 0.3575 0.7076 0.039 Uiso 1 1 calc R . . H1D2 H 0.7699 0.4132 0.7666 0.039 Uiso 1 1 calc R . . Cl2 Cl 0.43338(4) 0.285080(19) 0.73917(2) 0.01746(6) Uani 1 1 d . . . Cl1D Cl 0.89129(5) 0.39905(3) 0.64562(3) 0.03081(9) Uani 1 1 d . . . Cl2D Cl 0.61859(6) 0.47857(3) 0.68169(4) 0.03820(12) Uani 1 1 d . . . N1 N 0.33635(14) 0.19994(6) 0.90785(7) 0.01254(19) Uani 1 1 d . . . N2 N 0.24901(14) 0.08869(7) 0.83714(8) 0.0150(2) Uani 1 1 d . . . N3 N 0.48329(14) 0.11993(7) 0.77927(7) 0.01303(19) Uani 1 1 d . . . N4 N 0.68927(15) 0.11347(8) 0.68748(8) 0.0182(2) Uani 1 1 d . . . N5 N 0.74267(14) 0.20941(6) 0.78909(7) 0.01316(19) Uani 1 1 d . . . N6 N 0.62427(14) 0.15307(7) 0.94112(7) 0.01328(19) Uani 1 1 d . . . N7 N 0.59930(14) 0.29667(7) 0.92123(8) 0.0142(2) Uani 1 1 d . . . Ru1 Ru 0.537393(12) 0.209566(6) 0.847083(6) 0.01041(3) 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 C1 0.0164(6) 0.0151(5) 0.0152(5) -0.0015(4) 0.0010(4) 0.0001(4) C2 0.0181(7) 0.0204(6) 0.0187(6) -0.0034(5) 0.0040(5) 0.0007(5) C3 0.0179(7) 0.0241(7) 0.0221(7) -0.0027(5) 0.0066(5) -0.0023(5) C4 0.0160(6) 0.0198(6) 0.0213(6) -0.0016(5) 0.0033(5) -0.0029(5) C5 0.0135(6) 0.0140(5) 0.0153(5) 0.0007(4) -0.0003(4) -0.0003(4) C7 0.0150(6) 0.0125(5) 0.0125(5) 0.0005(4) -0.0016(4) -0.0010(4) C8 0.0167(6) 0.0119(5) 0.0128(5) -0.0001(4) -0.0013(4) -0.0006(4) C9 0.0185(6) 0.0141(5) 0.0161(5) -0.0002(4) -0.0011(5) -0.0021(4) C10 0.0202(7) 0.0128(5) 0.0208(6) -0.0031(4) -0.0017(5) -0.0021(5) C11 0.0214(7) 0.0144(5) 0.0198(6) -0.0047(5) -0.0002(5) 0.0006(5) C12 0.0185(6) 0.0170(6) 0.0174(6) -0.0035(4) 0.0009(5) -0.0003(5) C13 0.0151(6) 0.0141(5) 0.0152(5) -0.0013(4) -0.0015(4) -0.0008(4) C14 0.0145(6) 0.0155(5) 0.0135(5) -0.0014(4) 0.0004(4) -0.0012(4) C15 0.0150(6) 0.0166(5) 0.0159(5) -0.0010(4) 0.0016(4) -0.0030(4) C16 0.0168(7) 0.0253(7) 0.0246(7) -0.0069(6) 0.0060(5) -0.0043(5) C17 0.0146(6) 0.0241(7) 0.0239(7) -0.0026(5) 0.0040(5) -0.0032(5) C18 0.0142(6) 0.0210(6) 0.0213(6) -0.0014(5) 0.0004(5) -0.0038(5) C19 0.0149(6) 0.0185(6) 0.0179(6) -0.0023(5) 0.0000(5) -0.0025(5) C20 0.0210(7) 0.0143(5) 0.0167(6) 0.0025(4) -0.0014(5) 0.0022(5) C21 0.0230(7) 0.0209(6) 0.0214(7) 0.0073(5) -0.0017(5) 0.0031(5) C22 0.0203(7) 0.0298(8) 0.0176(6) 0.0089(5) -0.0028(5) 0.0018(6) C23 0.0177(7) 0.0283(7) 0.0132(5) 0.0031(5) -0.0026(5) -0.0026(5) C24 0.0136(6) 0.0192(6) 0.0123(5) 0.0001(4) -0.0009(4) -0.0018(4) C25 0.0155(6) 0.0186(6) 0.0126(5) -0.0019(4) 0.0005(4) -0.0031(5) C26 0.0227(7) 0.0266(7) 0.0146(6) -0.0046(5) 0.0007(5) -0.0101(6) C27 0.0272(8) 0.0235(7) 0.0231(7) -0.0102(6) 0.0045(6) -0.0111(6) C28 0.0217(7) 0.0163(6) 0.0283(7) -0.0058(5) 0.0045(6) -0.0043(5) C29 0.0160(6) 0.0142(5) 0.0216(6) -0.0017(4) 0.0010(5) -0.0012(4) C1D 0.0249(9) 0.0385(10) 0.0348(10) 0.0128(8) 0.0042(7) -0.0047(7) Cl2 0.01837(16) 0.01752(14) 0.01643(14) 0.00529(10) -0.00424(11) -0.00055(11) Cl1D 0.0278(2) 0.02696(19) 0.0377(2) 0.00774(16) 0.00698(18) 0.00233(16) Cl2D 0.0304(2) 0.0295(2) 0.0550(3) 0.0051(2) 0.0149(2) 0.00121(18) N1 0.0137(5) 0.0125(4) 0.0115(4) 0.0004(3) 0.0000(4) 0.0006(4) N2 0.0155(5) 0.0144(5) 0.0152(5) -0.0011(4) 0.0001(4) -0.0017(4) N3 0.0148(5) 0.0128(4) 0.0115(4) -0.0004(3) 0.0003(4) -0.0008(4) N4 0.0157(5) 0.0208(6) 0.0181(5) -0.0038(4) 0.0021(4) -0.0047(4) N5 0.0130(5) 0.0138(5) 0.0126(4) 0.0010(3) -0.0002(4) -0.0013(4) N6 0.0136(5) 0.0144(5) 0.0118(4) 0.0013(3) -0.0007(4) 0.0005(4) N7 0.0141(5) 0.0141(5) 0.0145(5) -0.0009(4) -0.0002(4) -0.0013(4) Ru1 0.01118(5) 0.01043(5) 0.00962(5) 0.00043(3) -0.00076(3) -0.00036(3) _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 C1 N1 1.3671(18) . ? C1 C2 1.383(2) . ? C2 C3 1.395(2) . ? C3 C4 1.377(2) . ? C4 C5 1.428(2) . ? C5 N1 1.3687(18) . ? C5 N2 1.3756(18) . ? C7 N2 1.3125(18) . ? C7 N3 1.3680(18) . ? C7 C8 1.4772(19) . ? C8 C9 1.384(2) . ? C8 C13 1.401(2) . ? C9 C10 1.403(2) . ? C10 C11 1.402(2) . ? C11 C12 1.400(2) . ? C12 C13 1.393(2) . ? C13 C14 1.471(2) . ? C14 N4 1.3028(19) . ? C14 N3 1.3778(18) . ? C15 N5 1.3712(19) . ? C15 N4 1.374(2) . ? C15 C16 1.421(2) . ? C16 C17 1.370(2) . ? C17 C18 1.394(2) . ? C18 C19 1.383(2) . ? C19 N5 1.3598(19) . ? C20 N6 1.3460(19) . ? C20 C21 1.376(2) . ? C21 C22 1.381(3) . ? C22 C23 1.385(3) . ? C23 C24 1.390(2) . ? C24 N6 1.3562(19) . ? C24 C25 1.466(2) . ? C25 N7 1.359(2) . ? C25 C26 1.394(2) . ? C26 C27 1.388(3) . ? C27 C28 1.382(3) . ? C28 C29 1.382(2) . ? C29 N7 1.3491(19) . ? C1D Cl2D 1.762(2) . ? C1D Cl1D 1.776(2) . ? Cl2 Ru1 2.4199(4) . ? N1 Ru1 2.1146(12) . ? N3 Ru1 2.0130(12) . ? N5 Ru1 2.1209(13) . ? N6 Ru1 2.0066(12) . ? N7 Ru1 2.0557(12) . ? 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 N1 C1 C2 125.78(14) . . ? C1 C2 C3 118.49(14) . . ? C4 C3 C2 117.53(14) . . ? C3 C4 C5 121.68(14) . . ? N1 C5 N2 125.35(13) . . ? N1 C5 C4 120.73(13) . . ? N2 C5 C4 113.92(13) . . ? N2 C7 N3 129.73(13) . . ? N2 C7 C8 121.79(13) . . ? N3 C7 C8 108.47(12) . . ? C9 C8 C13 121.15(13) . . ? C9 C8 C7 132.17(13) . . ? C13 C8 C7 106.66(12) . . ? C8 C9 C10 116.98(14) . . ? C11 C10 C9 122.03(14) . . ? C12 C11 C10 120.63(13) . . ? C13 C12 C11 116.94(14) . . ? C12 C13 C8 122.24(13) . . ? C12 C13 C14 131.11(14) . . ? C8 C13 C14 106.57(12) . . ? N4 C14 N3 130.23(13) . . ? N4 C14 C13 121.14(13) . . ? N3 C14 C13 108.55(12) . . ? N5 C15 N4 125.55(13) . . ? N5 C15 C16 121.37(14) . . ? N4 C15 C16 113.06(13) . . ? C17 C16 C15 121.29(15) . . ? C16 C17 C18 117.36(15) . . ? C19 C18 C17 119.28(14) . . ? N5 C19 C18 125.00(14) . . ? N6 C20 C21 122.58(15) . . ? C20 C21 C22 118.96(15) . . ? C21 C22 C23 119.06(15) . . ? C22 C23 C24 119.60(15) . . ? N6 C24 C23 120.87(14) . . ? N6 C24 C25 114.81(12) . . ? C23 C24 C25 124.32(14) . . ? N7 C25 C26 121.28(15) . . ? N7 C25 C24 114.50(12) . . ? C26 C25 C24 124.19(14) . . ? C27 C26 C25 119.27(16) . . ? C28 C27 C26 119.20(14) . . ? C27 C28 C29 118.97(16) . . ? N7 C29 C28 122.59(15) . . ? Cl2D C1D Cl1D 112.86(11) . . ? C1 N1 C5 115.71(12) . . ? C1 N1 Ru1 119.40(10) . . ? C5 N1 Ru1 124.46(9) . . ? C7 N2 C5 125.71(13) . . ? C7 N3 C14 109.67(11) . . ? C7 N3 Ru1 125.10(9) . . ? C14 N3 Ru1 124.84(10) . . ? C14 N4 C15 124.79(13) . . ? C19 N5 C15 115.67(13) . . ? C19 N5 Ru1 119.31(10) . . ? C15 N5 Ru1 124.79(10) . . ? C20 N6 C24 118.90(13) . . ? C20 N6 Ru1 124.81(10) . . ? C24 N6 Ru1 116.27(10) . . ? C29 N7 C25 118.59(13) . . ? C29 N7 Ru1 126.67(11) . . ? C25 N7 Ru1 114.69(10) . . ? N6 Ru1 N3 96.87(5) . . ? N6 Ru1 N7 79.59(5) . . ? N3 Ru1 N7 176.43(5) . . ? N6 Ru1 N1 86.64(5) . . ? N3 Ru1 N1 88.97(5) . . ? N7 Ru1 N1 91.28(5) . . ? N6 Ru1 N5 89.60(5) . . ? N3 Ru1 N5 88.20(5) . . ? N7 Ru1 N5 91.29(5) . . ? N1 Ru1 N5 175.00(4) . . ? N6 Ru1 Cl2 176.21(4) . . ? N3 Ru1 Cl2 86.86(4) . . ? N7 Ru1 Cl2 96.69(4) . . ? N1 Ru1 Cl2 92.73(3) . . ? N5 Ru1 Cl2 91.23(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 0.0(3) . . . . ? C1 C2 C3 C4 -2.3(3) . . . . ? C2 C3 C4 C5 2.2(3) . . . . ? C3 C4 C5 N1 0.1(2) . . . . ? C3 C4 C5 N2 -179.92(15) . . . . ? N2 C7 C8 C9 -3.5(2) . . . . ? N3 C7 C8 C9 175.42(15) . . . . ? N2 C7 C8 C13 178.31(13) . . . . ? N3 C7 C8 C13 -2.77(16) . . . . ? C13 C8 C9 C10 0.8(2) . . . . ? C7 C8 C9 C10 -177.23(15) . . . . ? C8 C9 C10 C11 -1.6(2) . . . . ? C9 C10 C11 C12 1.0(2) . . . . ? C10 C11 C12 C13 0.5(2) . . . . ? C11 C12 C13 C8 -1.3(2) . . . . ? C11 C12 C13 C14 175.22(15) . . . . ? C9 C8 C13 C12 0.7(2) . . . . ? C7 C8 C13 C12 179.14(14) . . . . ? C9 C8 C13 C14 -176.56(13) . . . . ? C7 C8 C13 C14 1.88(15) . . . . ? C12 C13 C14 N4 -0.2(3) . . . . ? C8 C13 C14 N4 176.70(14) . . . . ? C12 C13 C14 N3 -177.34(15) . . . . ? C8 C13 C14 N3 -0.41(16) . . . . ? N5 C15 C16 C17 1.9(3) . . . . ? N4 C15 C16 C17 -176.58(17) . . . . ? C15 C16 C17 C18 -2.0(3) . . . . ? C16 C17 C18 C19 0.8(2) . . . . ? C17 C18 C19 N5 0.6(3) . . . . ? N6 C20 C21 C22 1.1(3) . . . . ? C20 C21 C22 C23 -0.5(3) . . . . ? C21 C22 C23 C24 -1.0(3) . . . . ? C22 C23 C24 N6 2.1(2) . . . . ? C22 C23 C24 C25 -177.72(15) . . . . ? N6 C24 C25 N7 4.17(19) . . . . ? C23 C24 C25 N7 -176.04(14) . . . . ? N6 C24 C25 C26 -173.93(14) . . . . ? C23 C24 C25 C26 5.9(2) . . . . ? N7 C25 C26 C27 3.4(2) . . . . ? C24 C25 C26 C27 -178.66(15) . . . . ? C25 C26 C27 C28 -1.3(3) . . . . ? C26 C27 C28 C29 -1.4(3) . . . . ? C27 C28 C29 N7 2.3(2) . . . . ? C2 C1 N1 C5 2.3(2) . . . . ? C2 C1 N1 Ru1 -170.42(13) . . . . ? N2 C5 N1 C1 177.76(14) . . . . ? C4 C5 N1 C1 -2.3(2) . . . . ? N2 C5 N1 Ru1 -9.9(2) . . . . ? C4 C5 N1 Ru1 170.00(11) . . . . ? N3 C7 N2 C5 3.7(2) . . . . ? C8 C7 N2 C5 -177.65(13) . . . . ? N1 C5 N2 C7 5.0(2) . . . . ? C4 C5 N2 C7 -174.97(14) . . . . ? N2 C7 N3 C14 -178.64(14) . . . . ? C8 C7 N3 C14 2.55(16) . . . . ? N2 C7 N3 Ru1 -5.6(2) . . . . ? C8 C7 N3 Ru1 175.63(9) . . . . ? N4 C14 N3 C7 -178.14(16) . . . . ? C13 C14 N3 C7 -1.37(16) . . . . ? N4 C14 N3 Ru1 8.8(2) . . . . ? C13 C14 N3 Ru1 -174.47(9) . . . . ? N3 C14 N4 C15 5.0(3) . . . . ? C13 C14 N4 C15 -171.42(15) . . . . ? N5 C15 N4 C14 -11.3(3) . . . . ? C16 C15 N4 C14 167.07(16) . . . . ? C18 C19 N5 C15 -0.7(2) . . . . ? C18 C19 N5 Ru1 174.00(12) . . . . ? N4 C15 N5 C19 177.77(15) . . . . ? C16 C15 N5 C19 -0.5(2) . . . . ? N4 C15 N5 Ru1 3.4(2) . . . . ? C16 C15 N5 Ru1 -174.89(12) . . . . ? C21 C20 N6 C24 -0.1(2) . . . . ? C21 C20 N6 Ru1 -178.29(12) . . . . ? C23 C24 N6 C20 -1.5(2) . . . . ? C25 C24 N6 C20 178.31(13) . . . . ? C23 C24 N6 Ru1 176.88(11) . . . . ? C25 C24 N6 Ru1 -3.32(16) . . . . ? C28 C29 N7 C25 -0.3(2) . . . . ? C28 C29 N7 Ru1 -177.69(12) . . . . ? C26 C25 N7 C29 -2.5(2) . . . . ? C24 C25 N7 C29 179.31(13) . . . . ? C26 C25 N7 Ru1 175.12(12) . . . . ? C24 C25 N7 Ru1 -3.03(16) . . . . ? C20 N6 Ru1 N3 -0.88(13) . . . . ? C24 N6 Ru1 N3 -179.14(10) . . . . ? C20 N6 Ru1 N7 179.60(13) . . . . ? C24 N6 Ru1 N7 1.34(10) . . . . ? C20 N6 Ru1 N1 87.68(13) . . . . ? C24 N6 Ru1 N1 -90.58(11) . . . . ? C20 N6 Ru1 N5 -89.01(13) . . . . ? C24 N6 Ru1 N5 92.73(11) . . . . ? C20 N6 Ru1 Cl2 168.3(5) . . . . ? C24 N6 Ru1 Cl2 -9.9(6) . . . . ? C7 N3 Ru1 N6 87.13(12) . . . . ? C14 N3 Ru1 N6 -100.81(12) . . . . ? C7 N3 Ru1 N7 94.6(8) . . . . ? C14 N3 Ru1 N7 -93.3(8) . . . . ? C7 N3 Ru1 N1 0.64(11) . . . . ? C14 N3 Ru1 N1 172.69(12) . . . . ? C7 N3 Ru1 N5 176.52(12) . . . . ? C14 N3 Ru1 N5 -11.43(12) . . . . ? C7 N3 Ru1 Cl2 -92.16(11) . . . . ? C14 N3 Ru1 Cl2 79.90(11) . . . . ? C29 N7 Ru1 N6 178.47(13) . . . . ? C25 N7 Ru1 N6 1.03(10) . . . . ? C29 N7 Ru1 N3 170.9(7) . . . . ? C25 N7 Ru1 N3 -6.6(8) . . . . ? C29 N7 Ru1 N1 -95.18(13) . . . . ? C25 N7 Ru1 N1 87.38(11) . . . . ? C29 N7 Ru1 N5 89.11(13) . . . . ? C25 N7 Ru1 N5 -88.33(11) . . . . ? C29 N7 Ru1 Cl2 -2.27(13) . . . . ? C25 N7 Ru1 Cl2 -179.71(10) . . . . ? C1 N1 Ru1 N6 81.38(11) . . . . ? C5 N1 Ru1 N6 -90.66(12) . . . . ? C1 N1 Ru1 N3 178.32(11) . . . . ? C5 N1 Ru1 N3 6.28(12) . . . . ? C1 N1 Ru1 N7 1.88(11) . . . . ? C5 N1 Ru1 N7 -170.15(12) . . . . ? C1 N1 Ru1 N5 122.8(5) . . . . ? C5 N1 Ru1 N5 -49.2(6) . . . . ? C1 N1 Ru1 Cl2 -94.88(10) . . . . ? C5 N1 Ru1 Cl2 93.09(11) . . . . ? C19 N5 Ru1 N6 -71.17(11) . . . . ? C15 N5 Ru1 N6 103.00(12) . . . . ? C19 N5 Ru1 N3 -168.05(11) . . . . ? C15 N5 Ru1 N3 6.11(12) . . . . ? C19 N5 Ru1 N7 8.41(11) . . . . ? C15 N5 Ru1 N7 -177.43(12) . . . . ? C19 N5 Ru1 N1 -112.5(5) . . . . ? C15 N5 Ru1 N1 61.6(6) . . . . ? C19 N5 Ru1 Cl2 105.13(11) . . . . ? C15 N5 Ru1 Cl2 -80.70(11) . . . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 36.53 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 1.263 _refine_diff_density_min -0.739 _refine_diff_density_rms 0.158