# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1761 #======================================================================= data_global #======================================================================= _audit_creation_date 13-01-00 # 1. SUBMISSION DETAILS _publ_contact_author_name # Name of author for correspondance ; Prof. Jean Fischer ; _publ_contact_author_address # Address of author for correspondance ;Universite Louis Pasteur Laboratoire de Cristallochimie et de Chimie Structurale 4, rue Blaise Pascal 67070 Strasbourg cedex France ; _publ_contact_author_phone '+33 (0)3 88 41 60 58' _publ_contact_author_fax '+33 (0)3 88 41 53 63' _publ_contact_author_email fischer@chimie.u-strasbg.fr _publ_requested_journal 'Chem. Comm.' _publ_contact_letter ; ; _publ_requested_category FM #======================================================================= # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #======================================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; A Photochromic system based on photochemical or thermal chelate exchange on Ru(phen)2L2+ (L=diimine or dinitrile ligand) ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Baranoff Etienne' ; Universite Louis Pasteur Laboratoire de Chimie Organo-minerale UMR 7513 4, rue Blaise Pascal 67070 Strasbourf cedex France ; 'Collin Jean-Paul' ; Universite Louis Pasteur Laboratoire de Chimie Organo-minerale UMR 7513 4, rue Blaise Pascal 67070 Strasbourf cedex France ; 'Furusho Yoshio' ; Universite Louis Pasteur Laboratoire de Chimie Organo-minerale UMR 7513 4, rue Blaise Pascal 67070 Strasbourf cedex France ; 'Laemmel Anne-Chantal' ; Universite Louis Pasteur Laboratoire de Chimie Organo-minerale UMR 7513 4, rue Blaise Pascal 67070 Strasbourf cedex France ; 'Sauvage Jean-Pierre' ; Universite Louis Pasteur Laboratoire de Chimie Organo-minerale UMR 7513 4, rue Blaise Pascal 67070 Strasbourf cedex France ; # 4. TEXT _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_exptl_prep ; ? ; _publ_section_exptl_refinement ; ? ; _publ_section_references ; Burla, M.C., Camalli, M., Cascarano, G.,Giacovazzo, C., Polidori, G., Spagna, R. &Viterbo, D. (1989). SIR. J. Appl. Cryst. 22, 389-393. OpenMoleN, Interactive Intelligent Structure solution (1997) Nonius B.V., Delft, The Netherlands. KappaCCD Operation Manual (1997), Nonius B.V., Delft, The Nederlands. Otwinowski, Z. & Minor, W. (1997), Methods in Enzymology, 276, 307-326. ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ; ? ; #======================================================================= # If more than one structure is reported, sections 5-10 should be filled in # per structure. For each data set, replace the ? in the data_? line below # by a unique identifier. data_st502 #======================================================================= # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C57 H49 F12 N6 O3 P2 Ru' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C57 H49 F12 N6 O3 P2 Ru' _chemical_formula_weight 1257.06 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0.002 0.002 International_Tables_Vol_IV_Table_2.3.1 H ? 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1 F ? 0.014 0.010 International_Tables_Vol_IV_Table_2.3.1 N ? 0.004 0.003 International_Tables_Vol_IV_Table_2.3.1 O ? 0.008 0.006 International_Tables_Vol_IV_Table_2.3.1 P ? 0.090 0.095 International_Tables_Vol_IV_Table_2.3.1 Ru ? -1.420 0.836 International_Tables_Vol_IV_Table_2.3.1 #======================================================================= # 6. CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' 1/2-x,-y,1/2+z -x,1/2+y,1/2-z 1/2+x,1/2-y,-z -x,-y,-z 1/2+x,+y,1/2-z +x,1/2-y,1/2+z 1/2-x,1/2+y,+z _cell_length_a 17.9740(6) _cell_length_b 21.1890(9) _cell_length_c 29.793(1) _cell_angle_alpha 90 _cell_angle_beta 90.00(1) _cell_angle_gamma 90 _cell_volume 11346(1) _cell_formula_units_Z 8 _cell_measurement_temperature 294 _cell_measurement_reflns_used 22153 _cell_measurement_theta_min 1.4 _cell_measurement_theta_max 27.5 _cell_special_details ; Cell parameters refined using Scalepack part of DENZO Z. Otwinowski, W. Minor, 1997 ; _exptl_crystal_description prism _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.47 _exptl_crystal_density_method 'none' _exptl_crystal_F_000 5112 _exptl_absorpt_coefficient_mu 0.422 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? #======================================================================= # 7. EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 294 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_source xray_tube _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_measurement_details ; 22153 reflections were collected using program Collect ("Collect" Data collection software, Nonius B.V., 1998) The conditions were as follow : crystal to detector distance = 38. mm. Scan angle = 2.0 deg 1 scans of 90 sec per frame. Data collection was divided into 1 set(s) with the following starting angles and number of frames : Set 1 Theta = 9.30 Omega = 180.00 Kappa = 0.00 116 frames Friedel pairs were averaged. Internal R = 0.04 ; _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 22153 _diffrn_reflns_av_R_equivalents 0.040 _diffrn_reflns_av_sigmaI/netI 0.333 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 27.49 _reflns_number_total 13690 _reflns_number_gt 4186 _reflns_threshold_expression >3.0\s(I) _computing_structure_solution Direct_methods_(SIR,_Burla_et_al.,_1989) _computing_structure_refinement LSFM_OpenMoleN_(_1997) _computing_molecular_graphics ? _computing_publication_material CIFGEN_IN_OpenMoleN_(_1997) #======================================================================= # 8. REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme '4Fo^2^/(\s^2^(Fo^2^) + 0.0064 Fo^4^)' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 4186 _refine_ls_number_parameters 727 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.187 _refine_ls_R_factor_gt 0.066 _refine_ls_wR_factor_all 0.848 _refine_ls_wR_factor_ref 0.095 _refine_ls_goodness_of_fit_all 9.820 _refine_ls_goodness_of_fit_ref 1.553 _refine_ls_shift/su_max 0.151 _refine_ls_shift/esd_mean 0.007 _refine_diff_density_max 0.940 _refine_diff_density_min -0.217 #======================================================================= # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_type_symbol RU 0.24654(4) 0.17118(4) 0.71800(3) 0.0293(3) Uani ? ? Ru N1 0.3305(4) 0.2364(4) 0.7258(3) 0.035(5) Uani ? ? N C1 0.3412(6) 0.2895(5) 0.7018(4) 0.048(7) Uani ? ? C C2 0.4018(6) 0.3315(5) 0.7107(5) 0.058(8) Uani ? ? C C3 0.4488(6) 0.3196(5) 0.7452(5) 0.062(8) Uani ? ? C C4 0.4392(5) 0.2635(5) 0.7697(4) 0.050(7) Uani ? ? C C5 0.4886(5) 0.2426(6) 0.8058(4) 0.059(7) Uani ? ? C C6 0.4778(6) 0.1856(6) 0.8288(4) 0.057(7) Uani ? ? C C7 0.4157(6) 0.1483(5) 0.8163(4) 0.046(7) Uani ? ? C C8 0.4028(6) 0.0883(6) 0.8372(4) 0.052(7) Uani ? ? C C9 0.3462(6) 0.0526(5) 0.8232(4) 0.047(7) Uani ? ? C C10 0.2975(6) 0.0739(4) 0.7888(4) 0.042(6) Uani ? ? C N2 0.3080(4) 0.1312(3) 0.7687(3) 0.034(5) Uani ? ? N C11 0.3670(5) 0.1675(5) 0.7827(4) 0.036(5) Uani ? ? C C12 0.3794(5) 0.2237(4) 0.7596(4) 0.033(6) Uani ? ? C N3 0.1766(4) 0.2114(3) 0.7648(3) 0.031(4) Uani ? ? N C13 0.1857(5) 0.2660(4) 0.7868(4) 0.038(6) Uani ? ? C C14 0.1328(5) 0.2874(5) 0.8185(4) 0.044(6) Uani ? ? C C15 0.0736(5) 0.2527(5) 0.8287(4) 0.041(6) Uani ? ? C C16 0.0626(5) 0.1951(5) 0.8058(4) 0.039(6) Uani ? ? C C17 -0.0030(5) 0.1533(5) 0.8117(4) 0.049(7) Uani ? ? C C18 -0.0103(5) 0.0990(5) 0.7886(4) 0.049(7) Uani ? ? C C19 0.0442(5) 0.0800(5) 0.7561(4) 0.040(6) Uani ? ? C C20 0.0352(5) 0.0269(5) 0.7296(4) 0.040(6) Uani ? ? C C21 0.0898(6) 0.0143(5) 0.6983(4) 0.044(7) Uani ? ? C C22 0.1536(6) 0.0527(5) 0.6929(4) 0.047(7) Uani ? ? C N4 0.1617(4) 0.1040(3) 0.7185(3) 0.030(4) Uani ? ? N C23 0.1080(5) 0.1199(4) 0.7503(4) 0.035(6) Uani ? ? C C24 0.1154(5) 0.1753(4) 0.7743(3) 0.032(5) Uani ? ? C N5 0.3052(4) 0.1236(3) 0.6698(3) 0.030(4) Uani ? ? N C25 0.3257(5) 0.0960(5) 0.6402(4) 0.038(6) Uani ? ? C C26 0.3486(6) 0.0593(5) 0.6024(4) 0.049(7) Uani ? ? C C27 0.4215(6) 0.0404(6) 0.5950(4) 0.070(8) Uani ? ? C C28 0.4413(7) 0.0071(6) 0.5570(5) 0.082(9) Uani ? ? C C29 0.3862(7) -0.0090(6) 0.5272(4) 0.073(9) Uani ? ? C C30 0.3118(7) 0.0064(6) 0.5335(5) 0.084(9) Uani ? ? C C31 0.2919(6) 0.0399(5) 0.5713(4) 0.060(8) Uani ? ? C O1 0.2241(4) 0.0567(4) 0.5835(3) 0.100(6) Uani ? ? O C32 0.1680(8) 0.0623(7) 0.5434(6) 0.12(1) Uani ? ? C C33 0.1029(8) 0.0876(6) 0.5590(6) 0.09(1) Uani ? ? C O2 0.1129(4) 0.1432(4) 0.5827(3) 0.070(5) Uani ? ? O C34 0.1248(5) 0.1974(5) 0.5598(4) 0.047(7) Uani ? ? C C35 0.1108(7) 0.2061(5) 0.5153(4) 0.063(8) Uani ? ? C C36 0.1274(9) 0.2650(7) 0.4952(5) 0.11(1) Uani ? ? C C37 0.153(1) 0.3111(7) 0.5201(6) 0.13(1) Uani ? ? C C38 0.169(1) 0.3039(6) 0.5662(5) 0.10(1) Uani ? ? C C39 0.1535(6) 0.2456(5) 0.5856(4) 0.049(7) Uani ? ? C C40 0.1744(5) 0.2312(5) 0.6308(4) 0.043(7) Uani ? ? C N6 0.1947(4) 0.2141(3) 0.6653(3) 0.036(5) Uani ? ? N P1 0.3444(2) -0.0821(1) 0.7025(1) 0.045(2) Uani ? ? P F1 0.3878(6) -0.0820(4) 0.7472(4) 0.140(7) Uani ? ? F F2 0.3086(7) -0.0791(5) 0.6561(4) 0.178(9) Uani ? ? F F3 0.2730(5) -0.0923(7) 0.7266(5) 0.19(1) Uani ? ? F F4 0.4190(6) -0.0664(6) 0.6806(4) 0.20(1) Uani ? ? F F5 0.3564(7) -0.1549(3) 0.7000(4) 0.117(8) Uani ? ? F F6 0.3329(5) -0.0097(3) 0.7050(3) 0.102(6) Uani ? ? F P2 0.4694(2) -0.0832(2) 0.9124(1) 0.062(2) Uani ? ? P F7 0.5083(6) -0.0842(5) 0.9576(3) 0.132(7) Uani ? ? F F8 0.4269(9) -0.0819(5) 0.8674(4) 0.23(1) Uani ? ? F F9 0.4536(7) -0.1569(3) 0.9158(3) 0.112(8) Uani ? ? F F10 0.4779(4) -0.0111(3) 0.9079(3) 0.098(6) Uani ? ? F F11 0.5425(6) -0.0924(6) 0.8870(4) 0.241(9) Uani ? ? F F12 0.3994(5) -0.0733(5) 0.9418(5) 0.173(9) Uani ? ? F C41 0.1313(8) 0.0705(8) 0.8886(6) 0.11(1) Uani ? ? C C42 0.2046(7) 0.0969(6) 0.9043(4) 0.067(8) Uani ? ? C C43 0.2253(7) 0.1606(6) 0.8973(5) 0.08(1) Uani ? ? C C44 0.2927(6) 0.1855(6) 0.9115(5) 0.068(8) Uani ? ? C C45 0.3407(6) 0.1446(6) 0.9344(4) 0.060(8) Uani ? ? C C46 0.3233(6) 0.0860(6) 0.9428(5) 0.071(8) Uani ? ? C C47 0.2569(8) 0.0597(6) 0.9279(4) 0.074(9) Uani ? ? C C48 0.4147(8) 0.1714(9) 0.9500(6) 0.12(1) Uani ? ? C C49 0.356(1) 0.096(1) 0.3598(8) 0.10(1) Uani ? ? C C50 0.431(1) 0.114(1) 0.3864(9) 0.12(2) Uani ? ? C C51 0.430(1) 0.133(2) 0.434(1) 0.16(2) Uani ? ? C C52 0.347(1) 0.138(2) 0.4466(9) 0.15(2) Uani ? ? C C53 0.287(1) 0.127(2) 0.421(1) 0.15(2) Uani ? ? C C54 0.294(1) 0.106(2) 0.381(1) 0.15(2) Uani ? ? C C55 0.361(2) 0.071(2) 0.326(1) 0.29(3) Uani ? ? C C56 0.3340 0.1536 0.4845 0.19(4) Uani ? ? C O3 0.421(1) 0.258(1) 0.0933(8) 0.17(2) Uani ? ? O C57 0.366(1) 0.233(2) 0.084(1) 0.16(3) Uani ? ? C H1 0.3076 0.2993 0.6782 0.0658 Uiso calc C1 H H2 0.4090 0.3678 0.6925 0.0857 Uiso calc C2 H H3 0.4874 0.3484 0.7526 0.0836 Uiso calc C3 H H4 0.5295 0.2687 0.8140 0.0836 Uiso calc C5 H H5 0.5109 0.1724 0.8518 0.0757 Uiso calc C6 H H6 0.4342 0.0741 0.8609 0.0715 Uiso calc C8 H H7 0.3384 0.0123 0.8363 0.0651 Uiso calc C9 H H8 0.2571 0.0480 0.7796 0.0560 Uiso calc C10 H H9 0.2286 0.2910 0.7810 0.0502 Uiso calc C13 H H10 0.1397 0.3271 0.8326 0.0579 Uiso calc C14 H H11 0.0395 0.2663 0.8510 0.0537 Uiso calc C15 H H12 -0.0409 0.1652 0.8323 0.0656 Uiso calc C17 H H13 -0.0522 0.0727 0.7940 0.0651 Uiso calc C18 H H14 -0.0069 0.0001 0.7329 0.0528 Uiso calc C20 H H15 0.0843 -0.0216 0.6795 0.0631 Uiso calc C21 H H16 0.1903 0.0421 0.6712 0.0619 Uiso calc C22 H H17 0.4585 0.0506 0.6166 0.0930 Uiso calc C27 H H18 0.4917 -0.0043 0.5516 0.1067 Uiso calc C28 H H19 0.3996 -0.0319 0.5010 0.0965 Uiso calc C29 H H20 0.2753 -0.0059 0.5122 0.1119 Uiso calc C30 H H21 0.1587 0.0217 0.5311 0.1563 Uiso calc C32 H H22 0.1882 0.0889 0.5208 0.1563 Uiso calc C32 H H23 0.0799 0.0576 0.5783 0.1375 Uiso calc C33 H H24 0.0713 0.0959 0.5342 0.1375 Uiso calc C33 H H25 0.0901 0.1730 0.4979 0.0828 Uiso calc C35 H H26 0.1203 0.2709 0.4639 0.1570 Uiso calc C36 H H27 0.1603 0.3511 0.5066 0.2253 Uiso calc C37 H H28 0.1889 0.3376 0.5833 0.1716 Uiso calc C38 H H29 0.1913 0.1877 0.8823 0.1040 Uiso calc C43 H H30 0.3057 0.2282 0.9059 0.0882 Uiso calc C44 H H31 0.3570 0.0606 0.9594 0.0988 Uiso calc C46 H H32 0.2465 0.0165 0.9336 0.1050 Uiso calc C47 H H33 0.1283 0.0271 0.8965 0.1429 Uiso calc C41 H H34 0.0918 0.0929 0.9026 0.1429 Uiso calc C41 H H35 0.1276 0.0748 0.8570 0.1429 Uiso calc C41 H H36 0.4422 0.1395 0.9650 0.1696 Uiso calc C48 H H37 0.4421 0.1858 0.9247 0.1696 Uiso calc C48 H H38 0.4061 0.2056 0.9699 0.1696 Uiso calc C48 H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol RU 0.0314(3) 0.0250(3) 0.0321(4) -0.0015(4) 0.0005(5) -0.0006(5) Ru N1 0.033(4) 0.035(5) 0.037(6) -0.007(4) 0.009(4) -0.000(4) N C1 0.046(6) 0.034(6) 0.072(9) 0.002(6) 0.003(6) -0.016(6) C C2 0.071(7) 0.029(6) 0.10(1) -0.021(6) 0.020(8) 0.003(8) C C3 0.045(6) 0.061(7) 0.09(1) -0.019(6) 0.010(7) -0.022(8) C C4 0.040(6) 0.044(6) 0.072(9) -0.008(6) 0.004(6) -0.008(7) C C5 0.032(5) 0.092(9) 0.068(8) -0.004(7) -0.013(6) -0.043(7) C C6 0.049(6) 0.075(8) 0.051(8) 0.004(7) -0.009(6) -0.004(7) C C7 0.049(6) 0.060(7) 0.032(7) -0.000(6) 0.012(6) -0.015(6) C C8 0.046(6) 0.079(8) 0.039(7) 0.022(6) 0.006(6) -0.005(7) C C9 0.077(7) 0.036(6) 0.037(7) 0.022(6) 0.009(6) 0.019(6) C C10 0.053(6) 0.032(5) 0.044(7) 0.005(6) 0.009(6) 0.005(6) C N2 0.040(4) 0.033(5) 0.028(5) 0.010(4) -0.000(4) -0.005(4) N C11 0.031(4) 0.043(6) 0.034(6) 0.001(5) 0.001(5) -0.006(6) C C12 0.029(5) 0.033(6) 0.039(7) 0.003(5) 0.002(5) -0.013(5) C N3 0.034(4) 0.031(4) 0.029(5) 0.004(4) 0.000(4) 0.001(4) N C13 0.046(5) 0.027(5) 0.043(7) -0.010(5) 0.005(6) -0.007(6) C C14 0.052(6) 0.038(6) 0.043(7) 0.008(6) 0.003(6) -0.004(6) C C15 0.050(6) 0.033(6) 0.041(7) 0.002(6) 0.008(6) -0.002(6) C C16 0.041(5) 0.043(6) 0.033(6) 0.007(5) 0.013(5) 0.009(6) C C17 0.040(5) 0.064(8) 0.047(8) -0.008(6) 0.006(6) -0.000(7) C C18 0.034(5) 0.062(7) 0.054(8) -0.007(6) -0.009(6) -0.006(7) C C19 0.032(5) 0.044(6) 0.046(7) 0.002(6) -0.007(5) 0.007(7) C C20 0.036(5) 0.035(6) 0.050(8) -0.015(5) -0.012(5) 0.006(6) C C21 0.063(7) 0.022(5) 0.061(8) -0.008(6) -0.019(7) -0.001(6) C C22 0.053(6) 0.035(6) 0.055(8) -0.000(6) -0.003(7) -0.018(6) C N4 0.026(4) 0.024(4) 0.043(5) -0.004(4) 0.003(4) 0.001(4) N C23 0.047(6) 0.035(6) 0.026(6) 0.006(5) 0.001(5) -0.002(6) C C24 0.031(4) 0.029(5) 0.036(7) -0.004(5) 0.004(5) 0.003(5) C N5 0.032(4) 0.024(4) 0.035(5) -0.003(4) -0.002(4) -0.003(4) N C25 0.037(5) 0.046(7) 0.033(6) -0.003(5) -0.004(5) 0.000(6) C C26 0.051(6) 0.066(8) 0.035(7) 0.003(6) 0.002(6) -0.004(6) C C27 0.053(7) 0.092(9) 0.070(9) -0.004(7) 0.021(7) -0.040(8) C C28 0.076(8) 0.078(9) 0.09(1) -0.009(8) 0.029(8) -0.032(9) C C29 0.093(9) 0.063(9) 0.067(9) 0.002(8) 0.014(8) -0.035(8) C C30 0.086(9) 0.11(1) 0.065(9) 0.014(9) -0.026(8) -0.055(8) C C31 0.067(7) 0.068(8) 0.048(8) -0.009(7) -0.007(7) -0.023(7) C O1 0.043(4) 0.158(7) 0.146(8) 0.021(5) -0.021(5) -0.117(6) O C32 0.085(9) 0.16(1) 0.11(1) 0.02(1) -0.039(9) -0.09(1) C C33 0.110(9) 0.045(8) 0.16(1) -0.016(8) -0.08(1) 0.00(1) C O2 0.096(5) 0.059(5) 0.060(6) -0.031(5) -0.031(5) 0.005(5) O C34 0.054(6) 0.057(7) 0.033(7) -0.007(6) -0.011(6) 0.003(6) C C35 0.077(8) 0.053(8) 0.062(9) -0.005(7) -0.008(8) -0.005(7) C C36 0.19(1) 0.09(1) 0.08(1) -0.01(1) -0.07(1) -0.026(9) C C37 0.36(2) 0.07(1) 0.09(1) 0.01(1) -0.10(1) 0.042(9) C C38 0.26(2) 0.049(8) 0.09(1) -0.01(1) -0.09(1) 0.014(9) C C39 0.092(8) 0.039(6) 0.033(7) -0.001(7) -0.011(7) 0.014(6) C C40 0.045(6) 0.027(6) 0.066(9) 0.001(5) -0.004(6) 0.000(6) C N6 0.035(4) 0.033(5) 0.039(6) 0.005(4) -0.002(4) -0.001(5) N P1 0.049(2) 0.032(1) 0.062(2) 0.002(2) -0.003(2) 0.001(2) P F1 0.234(9) 0.077(5) 0.151(8) 0.015(7) -0.107(7) 0.000(7) F F2 0.30(1) 0.172(9) 0.110(7) -0.030(9) -0.118(7) -0.003(8) F F3 0.078(5) 0.26(1) 0.33(2) -0.006(7) 0.082(7) 0.07(1) F F4 0.157(7) 0.22(1) 0.23(1) 0.001(8) 0.122(7) 0.02(1) F F5 0.28(1) 0.038(4) 0.15(1) 0.018(7) -0.03(1) -0.019(5) F F6 0.172(7) 0.051(4) 0.120(8) 0.020(5) -0.008(7) 0.009(5) F P2 0.097(2) 0.054(2) 0.045(2) -0.011(2) 0.001(2) 0.004(2) P F7 0.171(8) 0.179(9) 0.075(6) -0.031(8) -0.040(6) 0.030(7) F F8 0.55(2) 0.155(8) 0.142(9) -0.163(9) -0.191(9) 0.038(7) F F9 0.35(1) 0.040(5) 0.101(8) -0.027(7) 0.050(9) -0.003(5) F F10 0.109(5) 0.059(5) 0.146(8) -0.021(5) -0.004(6) 0.015(5) F F11 0.249(8) 0.24(1) 0.233(9) 0.126(8) 0.198(6) 0.129(8) F F12 0.121(6) 0.158(9) 0.27(1) 0.010(7) 0.073(8) 0.058(9) F C41 0.09(1) 0.14(1) 0.10(1) 0.01(1) -0.00(1) 0.01(1) C C42 0.071(8) 0.089(9) 0.047(8) -0.001(8) 0.005(7) 0.012(8) C C43 0.094(9) 0.074(9) 0.07(1) 0.014(8) -0.009(8) 0.014(8) C C44 0.068(7) 0.061(8) 0.07(1) 0.014(7) 0.008(8) -0.006(8) C C45 0.049(6) 0.084(9) 0.053(9) -0.003(7) 0.008(7) 0.001(8) C C46 0.052(6) 0.12(1) 0.062(9) 0.032(7) -0.004(7) -0.005(9) C C47 0.13(1) 0.069(8) 0.045(7) 0.021(8) 0.041(8) 0.015(7) C C48 0.087(9) 0.21(2) 0.09(1) -0.04(1) -0.01(1) -0.00(1) C C49 0.18(1) 0.07(1) 0.09(1) 0.01(1) 0.10(1) 0.02(1) C C50 0.11(1) 0.06(1) 0.26(3) -0.01(1) 0.07(2) 0.02(2) C C51 0.15(2) 0.06(1) 0.47(4) 0.04(1) 0.14(2) 0.13(2) C C52 0.44(3) 0.06(1) 0.11(2) -0.08(2) -0.18(2) 0.02(1) C C53 0.33(3) 0.07(1) 0.16(2) 0.01(2) 0.05(2) 0.01(1) C C54 0.19(2) 0.08(1) 0.22(2) -0.02(1) -0.01(2) 0.03(1) C C55 0.46(5) 0.18(2) 0.29(3) 0.04(3) 0.22(3) 0.16(2) C C56 0.09(2) 0.39(6) 0.21(5) -0.02(3) -0.02(3) 0.15(4) C O3 0.12(1) 0.27(2) 0.16(2) 0.07(2) -0.10(1) -0.14(2) O C57 0.09(2) 0.37(4) 0.12(3) 0.13(2) 0.00(2) -0.09(3) C # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag RU N1 2.059(9) . . ? RU N2 2.054(9) . . ? RU N3 2.061(9) . . ? RU N4 2.085(8) . . ? RU N5 2.05(1) . . ? RU N6 2.04(1) . . ? N1 C1 1.35(1) . . ? N1 C12 1.36(1) . . ? C1 C2 1.43(2) . . ? C2 C3 1.35(2) . . ? C3 C4 1.41(2) . . ? C4 C5 1.46(2) . . ? C4 C12 1.40(1) . . ? C5 C6 1.40(2) . . ? C6 C7 1.42(2) . . ? C7 C8 1.43(2) . . ? C7 C11 1.39(2) . . ? C8 C9 1.34(2) . . ? C9 C10 1.42(2) . . ? C10 N2 1.37(1) . . ? N2 C11 1.37(1) . . ? C11 C12 1.39(2) . . ? N3 C13 1.34(1) . . ? N3 C24 1.37(1) . . ? C13 C14 1.41(2) . . ? C14 C15 1.33(1) . . ? C15 C16 1.41(2) . . ? C16 C17 1.49(2) . . ? C16 C24 1.40(1) . . ? C17 C18 1.35(2) . . ? C18 C19 1.44(2) . . ? C19 C20 1.38(1) . . ? C19 C23 1.44(1) . . ? C20 C21 1.38(2) . . ? C21 C22 1.41(2) . . ? C22 N4 1.34(1) . . ? N4 C23 1.39(1) . . ? C23 C24 1.38(1) . . ? N5 C25 1.12(1) . . ? C25 C26 1.43(2) . . ? C26 C27 1.39(2) . . ? C26 C31 1.44(2) . . ? C27 C28 1.38(2) . . ? C28 C29 1.37(2) . . ? C29 C30 1.39(2) . . ? C30 C31 1.38(2) . . ? C31 O1 1.32(2) . . ? O1 C32 1.57(2) . . ? C32 C33 1.37(2) . . ? C33 O2 1.39(2) . . ? O2 C34 1.35(1) . . ? C34 C35 1.36(2) . . ? C34 C39 1.38(2) . . ? C35 C36 1.41(2) . . ? C36 C37 1.31(2) . . ? C37 C38 1.41(2) . . ? C38 C39 1.39(2) . . ? C39 C40 1.43(2) . . ? C40 N6 1.15(1) . . ? P1 F1 1.54(1) . . ? P1 F2 1.53(1) . . ? P1 F3 1.49(1) . . ? P1 F4 1.53(1) . . ? P1 F5 1.560(9) . . ? P1 F6 1.550(9) . . ? F1 F4 2.09(2) . . ? F4 F6 2.09(1) . . ? P2 F7 1.52(1) . . ? P2 F8 1.54(1) . . ? P2 F9 1.591(9) . . ? P2 F10 1.540(8) . . ? P2 F11 1.53(1) . . ? P2 F12 1.55(1) . . ? F7 F12 2.03(2) . . ? C41 C42 1.50(2) . . ? C42 C43 1.41(2) . . ? C42 C47 1.41(2) . . ? C43 C44 1.39(2) . . ? C44 C45 1.40(2) . . ? C45 C46 1.30(2) . . ? C45 C48 1.52(2) . . ? C46 C47 1.39(2) . . ? C49 C50 1.61(2) . . ? C49 C54 1.29(2) . . ? C49 C55 1.16(2) . . ? C50 C51 1.4596 . . ? C51 C52 1.5538 . . ? C52 C53 1.3337 . . ? C52 C56 1.2008 . . ? C53 C54 1.2777 . . ? O3 C57 1.15(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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 RU N2 78.4(4) . . . ? N1 RU N3 95.3(4) . . . ? N1 RU N4 173.1(4) . . . ? N1 RU N5 91.8(3) . . . ? N1 RU N6 97.0(4) . . . ? N2 RU N3 90.0(3) . . . ? N2 RU N4 96.1(4) . . . ? N2 RU N5 92.1(3) . . . ? N2 RU N6 174.6(4) . . . ? N3 RU N4 80.3(4) . . . ? N3 RU N5 172.8(3) . . . ? N3 RU N6 93.4(4) . . . ? N4 RU N5 92.6(4) . . . ? N4 RU N6 88.6(4) . . . ? N5 RU N6 85.1(3) . . . ? RU N1 C1 127.3(8) . . . ? RU N1 C12 115.0(8) . . . ? C1 N1 C12 117(1) . . . ? N1 C1 C2 122(1) . . . ? C1 C2 C3 119(1) . . . ? C2 C3 C4 118(1) . . . ? C3 C4 C5 124(1) . . . ? C3 C4 C12 119(1) . . . ? C5 C4 C12 116(1) . . . ? C4 C5 C6 122(1) . . . ? C5 C6 C7 117(1) . . . ? C6 C7 C8 120(1) . . . ? C6 C7 C11 121(1) . . . ? C8 C7 C11 118(1) . . . ? C7 C8 C9 119(1) . . . ? C8 C9 C10 121(1) . . . ? C9 C10 N2 120(1) . . . ? RU N2 C10 127.8(8) . . . ? RU N2 C11 114.1(8) . . . ? C10 N2 C11 118(1) . . . ? C7 C11 N2 122(1) . . . ? C7 C11 C12 120(1) . . . ? N2 C11 C12 116(1) . . . ? N1 C12 C4 122(1) . . . ? N1 C12 C11 115(1) . . . ? C4 C12 C11 122(1) . . . ? RU N3 C13 127.9(8) . . . ? RU N3 C24 113.5(7) . . . ? C13 N3 C24 118(1) . . . ? N3 C13 C14 121(1) . . . ? C13 C14 C15 121(1) . . . ? C14 C15 C16 118(1) . . . ? C15 C16 C17 124(1) . . . ? C15 C16 C24 119(1) . . . ? C17 C16 C24 116(1) . . . ? C16 C17 C18 121(1) . . . ? C17 C18 C19 121(1) . . . ? C18 C19 C20 122(1) . . . ? C18 C19 C23 117(1) . . . ? C20 C19 C23 120(1) . . . ? C19 C20 C21 117(1) . . . ? C20 C21 C22 122(1) . . . ? C21 C22 N4 119(1) . . . ? RU N4 C22 129.1(8) . . . ? RU N4 C23 110.3(7) . . . ? C22 N4 C23 120(1) . . . ? C19 C23 N4 119(1) . . . ? C19 C23 C24 120(1) . . . ? N4 C23 C24 119(1) . . . ? N3 C24 C16 121(1) . . . ? N3 C24 C23 116(1) . . . ? C16 C24 C23 122(1) . . . ? RU N5 C25 168(1) . . . ? N5 C25 C26 177(1) . . . ? C25 C26 C27 123(1) . . . ? C25 C26 C31 117(1) . . . ? C27 C26 C31 119(1) . . . ? C26 C27 C28 121(1) . . . ? C27 C28 C29 118(1) . . . ? C28 C29 C30 123(1) . . . ? C29 C30 C31 118(1) . . . ? C26 C31 C30 119(1) . . . ? C26 C31 O1 113(1) . . . ? C30 C31 O1 127(1) . . . ? C31 O1 C32 113(1) . . . ? O1 C32 C33 108(1) . . . ? C32 C33 O2 113(1) . . . ? C33 O2 C34 119(1) . . . ? O2 C34 C35 125(1) . . . ? O2 C34 C39 114(1) . . . ? C35 C34 C39 120(1) . . . ? C34 C35 C36 119(1) . . . ? C35 C36 C37 119(1) . . . ? C36 C37 C38 122(1) . . . ? C37 C38 C39 117(1) . . . ? C34 C39 C38 120(1) . . . ? C34 C39 C40 117(1) . . . ? C38 C39 C40 121(1) . . . ? C39 C40 N6 172(1) . . . ? RU N6 C40 167(1) . . . ? F1 P1 F2 174.0(9) . . . ? F1 P1 F3 91(1) . . . ? F1 P1 F4 85.7(8) . . . ? F1 P1 F5 88.5(6) . . . ? F1 P1 F6 91.4(6) . . . ? F2 P1 F3 94.5(9) . . . ? F2 P1 F4 88(1) . . . ? F2 P1 F5 93.2(7) . . . ? F2 P1 F6 86.9(7) . . . ? F3 P1 F4 174(1) . . . ? F3 P1 F5 90.0(8) . . . ? F3 P1 F6 90.3(8) . . . ? F4 P1 F5 94.2(8) . . . ? F4 P1 F6 85.6(7) . . . ? F5 P1 F6 180(1) . . . ? P1 F1 F4 46.9(6) . . . ? P1 F4 F1 47.4(5) . . . ? P1 F4 F6 47.6(4) . . . ? F1 F4 F6 64.0(6) . . . ? P1 F6 F4 46.8(4) . . . ? F7 P2 F8 177(1) . . . ? F7 P2 F9 90.7(7) . . . ? F7 P2 F10 92.6(6) . . . ? F7 P2 F11 92.4(9) . . . ? F7 P2 F12 82.8(8) . . . ? F8 P2 F9 89.1(7) . . . ? F8 P2 F10 87.4(7) . . . ? F8 P2 F11 89(1) . . . ? F8 P2 F12 94(1) . . . ? F9 P2 F10 175.2(7) . . . ? F9 P2 F11 93.5(8) . . . ? F9 P2 F12 87.2(7) . . . ? F10 P2 F11 89.9(7) . . . ? F10 P2 F12 89.7(6) . . . ? F11 P2 F12 175(1) . . . ? P2 F7 F12 49.2(6) . . . ? P2 F12 F7 48.0(5) . . . ? C41 C42 C43 122(1) . . . ? C41 C42 C47 121(1) . . . ? C43 C42 C47 115(1) . . . ? C42 C43 C44 123(1) . . . ? C43 C44 C45 116(1) . . . ? C44 C45 C46 122(1) . . . ? C44 C45 C48 117(1) . . . ? C46 C45 C48 120(1) . . . ? C45 C46 C47 121(1) . . . ? C42 C47 C46 120(1) . . . ? C50 C49 C54 116(1) . . . ? C50 C49 C55 118(1) . . . ? C54 C49 C55 124(1) . . . ? C49 C50 C51 122.3(7) . . . ? C50 C51 C52 105.26 . . . ? C51 C52 C53 128.47 . . . ? C51 C52 C56 115.79 . . . ? C53 C52 C56 115.74 . . . ? C52 C53 C54 120.75 . . . ? C49 C54 C53 126(1) . . . ?