#------------------------------------------------------------------------------ #$Date: 2021-11-06 00:51:34 +0200 (Sat, 06 Nov 2021) $ #$Revision: 270327 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/06/10/7061045.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7061045 loop_ _publ_author_name 'Sato, Hiroki' 'Tsukamoto, Tadashi' 'Sogawa, Hiromitsu' 'Kuwata, Shigeki' 'Takata, Toshikazu' _publ_section_title ; Ruthenium macrocycles bearing pyridine bis(carboxamide): synthesis, structure, and catalytic activity for hydrosilylation ; _journal_issue 39 _journal_name_full 'New Journal of Chemistry' _journal_page_first 18282 _journal_page_last 18289 _journal_paper_doi 10.1039/D0NJ06133F _journal_volume 45 _journal_year 2021 _chemical_formula_moiety 'C34.3 H41.56 N3.65 O11 Ru' _chemical_formula_sum 'C34.3 H41.56 N3.65 O11 Ru' _chemical_formula_weight 782.05 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_update_record ; 2020-02-01 deposited with the CCDC. 2021-08-30 downloaded from the CCDC. ; _cell_angle_alpha 68.755(18) _cell_angle_beta 77.07(2) _cell_angle_gamma 74.08(2) _cell_formula_units_Z 2 _cell_length_a 10.629(4) _cell_length_b 12.451(4) _cell_length_c 15.252(5) _cell_measurement_reflns_used 5630 _cell_measurement_temperature 93 _cell_measurement_theta_max 27.48 _cell_measurement_theta_min 3.03 _cell_volume 1791.6(11) _computing_cell_refinement CrystalClear _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction CrystalClear _computing_molecular_graphics 'CrystalStructure 4.2.5' _computing_publication_material 'CrystalStructure 4.2.5 (Rigaku, 2017)' _computing_structure_refinement 'SHELXL Version 2014/7 (Sheldrick, 2008)' _computing_structure_solution 'SIR92 (Altomare, et al., 1994)' _diffrn_ambient_temperature 93 _diffrn_detector_area_resol_mean 7.111 _diffrn_measured_fraction_theta_full 0.981 _diffrn_measured_fraction_theta_max 0.956 _diffrn_measurement_device_type 'Rigaku Saturn724' _diffrn_measurement_method \w _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_reflns_av_R_equivalents 0.0571 _diffrn_reflns_Laue_measured_fraction_full 0.981 _diffrn_reflns_Laue_measured_fraction_max 0.956 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 14821 _diffrn_reflns_point_group_measured_fraction_full 0.981 _diffrn_reflns_point_group_measured_fraction_max 0.956 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.558 _diffrn_reflns_theta_min 3.026 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.501 _exptl_absorpt_correction_T_max 0.975 _exptl_absorpt_correction_T_min 0.738 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'REQAB (Rigaku, 1998)' _exptl_crystal_colour red _exptl_crystal_density_diffrn 1.450 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 809.82 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: dimethylformamide/water' _exptl_crystal_size_max 0.190 _exptl_crystal_size_mid 0.050 _exptl_crystal_size_min 0.050 _refine_diff_density_max 1.29 _refine_diff_density_min -0.50 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.986 _refine_ls_hydrogen_treatment mixed _refine_ls_number_parameters 483 _refine_ls_number_reflns 7913 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0668 _refine_ls_R_factor_gt 0.0490 _refine_ls_shift/su_max 0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0526P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1146 _refine_ls_wR_factor_ref 0.1229 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5648 _reflns_number_total 7913 _reflns_threshold_expression F^2^>2.0\s(F^2^) _cod_data_source_file d0nj06133f2.cif _cod_data_source_block RuMC33CO2H2O _cod_original_cell_volume 1791.5(11) _cod_database_code 7061045 _shelx_res_file ; shelxl.res created by SHELXL-2014/7 TITL Takata160710 CELL 0.71075 10.62850 12.45120 15.25200 68.75460 77.06780 74.07550 ZERR 2 0.00400 0.00370 0.00510 0.01780 0.01970 0.02010 LATT 1 SFAC C H N O RU UNIT 68.600000 83.120000 7.300000 22 2 L.S. 5 FMAP 2 PLAN 25 WPDB -2 HTAB BOND $H CONF LIST 4 TEMP -179.8 ACTA SIZE 0.190 0.050 0.050 DFIX 1.15 C36 O12 EADP C36 O12 WGHT 0.052600 FVAR 0.49488 0.65137 RU1 5 0.308495 0.908954 0.883892 11.00000 0.01358 0.02679 = 0.02392 -0.01594 -0.00077 -0.00433 O1 4 -0.005782 0.818454 1.095039 11.00000 0.01636 0.02184 = 0.02844 -0.00776 -0.00133 -0.00517 O2 4 0.662073 0.867860 0.982664 11.00000 0.01345 0.05236 = 0.04536 -0.03570 -0.00440 -0.00372 O3 4 0.124518 0.531699 0.732009 11.00000 0.03963 0.01914 = 0.01769 -0.00610 -0.00366 -0.00748 O4 4 0.346347 0.350497 0.703902 11.00000 0.03159 0.04832 = 0.03678 -0.01369 -0.01243 0.00435 O5 4 0.562690 0.258240 0.577515 11.00000 0.03134 0.06064 = 0.03033 -0.02006 -0.00682 0.00115 O6 4 0.837838 0.211599 0.532940 11.00000 0.02702 0.02294 = 0.02784 -0.00776 -0.00485 -0.00440 O7 4 0.979591 0.322746 0.612607 11.00000 0.03069 0.02558 = 0.03456 -0.01672 -0.00909 0.00253 O8 4 0.750958 0.591335 0.619099 11.00000 0.03138 0.02575 = 0.02868 -0.01894 -0.00784 -0.00009 O9 4 0.280193 1.012353 0.676681 11.00000 0.04368 0.07387 = 0.02312 -0.01906 -0.00270 -0.01825 O10 4 0.255651 1.080100 0.892011 11.00000 0.01395 0.02166 = 0.02641 -0.01235 -0.00433 -0.00301 PART 1 O11 4 0.358687 0.725584 0.905016 21.00000 0.02599 0.01726 = 0.02340 -0.01269 -0.01124 0.00338 C33 1 0.393421 0.684254 0.835024 21.00000 0.02983 0.03799 = 0.04796 -0.03763 0.00620 -0.01227 AFIX 43 H36 2 0.402400 0.734510 0.770997 21.00000 -1.20000 AFIX 0 N4 3 0.416653 0.564841 0.857377 21.00000 0.02824 0.02785 = 0.03729 -0.02011 -0.00856 0.00038 C34 1 0.385665 0.478428 0.952246 21.00000 0.08309 0.03231 = 0.04888 -0.00769 -0.00770 -0.01357 AFIX 137 H37 2 0.467942 0.427076 0.974810 21.00000 -1.50000 H38 2 0.329855 0.430552 0.947233 21.00000 -1.50000 H39 2 0.338782 0.520723 0.997195 21.00000 -1.50000 AFIX 0 C35 1 0.462954 0.517660 0.778316 21.00000 0.03893 0.04424 = 0.05628 -0.03801 0.00780 -0.01459 AFIX 137 H40 2 0.556849 0.479778 0.778499 21.00000 -1.50000 H41 2 0.450841 0.582005 0.718330 21.00000 -1.50000 H42 2 0.412261 0.459520 0.785036 21.00000 -1.50000 AFIX 0 PART 2 C36 1 0.357924 0.771084 0.856358 -21.00000 0.01406 0.03297 = 0.02608 -0.00540 -0.00348 -0.00567 O12 4 0.393060 0.679779 0.847699 -21.00000 0.01406 0.03297 = 0.02608 -0.00540 -0.00348 -0.00567 PART 0 N1 3 0.324208 0.852260 1.024540 11.00000 0.01419 0.01711 = 0.02649 -0.01125 -0.00537 -0.00113 N2 3 0.116551 0.885548 0.946775 11.00000 0.01452 0.02172 = 0.02444 -0.01466 -0.00254 -0.00316 N3 3 0.505571 0.911821 0.883551 11.00000 0.01403 0.03696 = 0.02812 -0.02448 0.00169 -0.00607 C1 1 0.097176 0.845766 1.040573 11.00000 0.01529 0.01426 = 0.02604 -0.01072 -0.00278 -0.00180 C2 1 0.217430 0.830084 1.085866 11.00000 0.01979 0.01254 = 0.02413 -0.00842 -0.00336 -0.00295 C3 1 0.221695 0.795401 1.182762 11.00000 0.02344 0.01609 = 0.02575 -0.00897 -0.00493 -0.00238 AFIX 43 H1 2 0.145817 0.779594 1.227827 11.00000 -1.20000 AFIX 0 C4 1 0.342199 0.784598 1.211555 11.00000 0.03231 0.01891 = 0.02641 -0.00551 -0.01293 -0.00150 AFIX 43 H2 2 0.348194 0.760625 1.277395 11.00000 -1.20000 AFIX 0 C5 1 0.452461 0.808158 1.145984 11.00000 0.02119 0.02154 = 0.03141 -0.01369 -0.01090 0.00119 AFIX 43 H3 2 0.534069 0.800083 1.165889 11.00000 -1.20000 AFIX 0 C6 1 0.440621 0.843858 1.050475 11.00000 0.01498 0.01934 = 0.03470 -0.01860 -0.00719 0.00181 C7 1 0.546440 0.876025 0.967645 11.00000 0.01452 0.02851 = 0.03957 -0.02645 -0.00327 -0.00029 C8 1 0.008617 0.898926 0.895152 11.00000 0.01766 0.02647 = 0.02396 -0.01145 -0.00347 -0.00457 AFIX 23 H4 2 -0.000520 0.975708 0.843600 11.00000 -1.20000 H5 2 -0.075440 0.898605 0.939146 11.00000 -1.20000 AFIX 0 C9 1 0.034389 0.800258 0.853035 11.00000 0.01427 0.02412 = 0.02458 -0.01083 -0.00409 -0.00696 C10 1 0.035241 0.684867 0.910795 11.00000 0.03826 0.03196 = 0.01713 -0.00767 0.00009 -0.01560 AFIX 43 H6 2 0.016437 0.668254 0.977702 11.00000 -1.20000 AFIX 0 C11 1 0.062688 0.592931 0.873946 11.00000 0.04435 0.02241 = 0.01925 -0.00642 -0.00039 -0.01389 AFIX 43 H7 2 0.060874 0.514838 0.915114 11.00000 -1.20000 AFIX 0 C12 1 0.092600 0.615711 0.777197 11.00000 0.02078 0.02380 = 0.02190 -0.01082 -0.00420 -0.00599 C13 1 0.091519 0.729677 0.717602 11.00000 0.02640 0.02405 = 0.01580 -0.00673 -0.00428 -0.00442 AFIX 43 H8 2 0.110666 0.745563 0.650776 11.00000 -1.20000 AFIX 0 C14 1 0.062561 0.820799 0.755151 11.00000 0.02549 0.02150 = 0.02336 -0.00429 -0.00761 -0.00544 AFIX 43 H9 2 0.061811 0.899048 0.713479 11.00000 -1.20000 AFIX 0 C15 1 0.136381 0.409793 0.788205 11.00000 0.03960 0.02067 = 0.02667 -0.00568 -0.00681 -0.01049 AFIX 23 H10 2 0.047914 0.391086 0.813572 11.00000 -1.20000 H11 2 0.184544 0.391313 0.842207 11.00000 -1.20000 AFIX 0 C16 1 0.211423 0.340100 0.723626 11.00000 0.03747 0.02292 = 0.03189 -0.00808 -0.00714 -0.00528 AFIX 23 H12 2 0.205974 0.256220 0.754359 11.00000 -1.20000 H13 2 0.172710 0.370396 0.663707 11.00000 -1.20000 AFIX 0 C17 1 0.388835 0.411574 0.609405 11.00000 0.03614 0.03898 = 0.04603 -0.01213 -0.00303 -0.01140 AFIX 23 H14 2 0.459424 0.450506 0.607685 11.00000 -1.20000 H15 2 0.314177 0.473738 0.582032 11.00000 -1.20000 AFIX 0 C18 1 0.440192 0.331239 0.550163 11.00000 0.04083 0.04741 = 0.02899 -0.00842 -0.01016 -0.01073 AFIX 23 H16 2 0.376106 0.282014 0.559814 11.00000 -1.20000 H17 2 0.452479 0.378349 0.482047 11.00000 -1.20000 AFIX 0 C19 1 0.629442 0.191993 0.516071 11.00000 0.03772 0.04283 = 0.03923 -0.01532 -0.00781 -0.01237 AFIX 23 H18 2 0.640086 0.245136 0.449685 11.00000 -1.20000 H19 2 0.577833 0.134985 0.519626 11.00000 -1.20000 AFIX 0 C20 1 0.763863 0.126885 0.546579 11.00000 0.03297 0.02986 = 0.03763 -0.01603 -0.00378 -0.00885 AFIX 23 H20 2 0.753544 0.077875 0.614284 11.00000 -1.20000 H21 2 0.809875 0.074544 0.508195 11.00000 -1.20000 AFIX 0 C21 1 0.963694 0.161519 0.562968 11.00000 0.02921 0.02328 = 0.03638 -0.01413 -0.00138 -0.00158 AFIX 23 H22 2 1.016148 0.108419 0.526630 11.00000 -1.20000 H23 2 0.953828 0.114399 0.631178 11.00000 -1.20000 AFIX 0 C22 1 1.033737 0.257618 0.547357 11.00000 0.02545 0.02760 = 0.04031 -0.02081 0.00179 -0.00299 AFIX 23 H24 2 1.128145 0.222424 0.553786 11.00000 -1.20000 H25 2 1.028738 0.312544 0.481733 11.00000 -1.20000 AFIX 0 C23 1 0.871269 0.418643 0.583628 11.00000 0.02603 0.02306 = 0.02927 -0.01417 -0.00496 -0.00227 AFIX 23 H26 2 0.791749 0.389393 0.587668 11.00000 -1.20000 H27 2 0.893389 0.468953 0.517573 11.00000 -1.20000 AFIX 0 C24 1 0.848391 0.486916 0.652803 11.00000 0.03039 0.02099 = 0.02652 -0.00926 -0.00454 -0.00509 AFIX 23 H28 2 0.816549 0.439302 0.717676 11.00000 -1.20000 H29 2 0.931361 0.507388 0.654338 11.00000 -1.20000 AFIX 0 C25 1 0.721838 0.672183 0.666577 11.00000 0.02201 0.02956 = 0.02658 -0.01804 0.00344 -0.00989 C26 1 0.761306 0.652173 0.752270 11.00000 0.02187 0.03298 = 0.02732 -0.01724 -0.00155 -0.00322 AFIX 43 H30 2 0.813940 0.578036 0.782661 11.00000 -1.20000 AFIX 0 C27 1 0.724240 0.740189 0.794178 11.00000 0.01985 0.04425 = 0.02673 -0.02233 -0.00164 -0.00368 AFIX 43 H31 2 0.752110 0.725366 0.853251 11.00000 -1.20000 AFIX 0 C28 1 0.647432 0.849320 0.751806 11.00000 0.01657 0.03349 = 0.03079 -0.02186 0.00572 -0.00994 C29 1 0.609234 0.868437 0.664680 11.00000 0.02355 0.02669 = 0.02891 -0.01413 0.00187 -0.00680 AFIX 43 H32 2 0.556564 0.942601 0.634383 11.00000 -1.20000 AFIX 0 C30 1 0.646099 0.782138 0.621253 11.00000 0.03013 0.03001 = 0.02512 -0.01336 -0.00339 -0.00568 AFIX 43 H33 2 0.620305 0.797354 0.561402 11.00000 -1.20000 AFIX 0 C31 1 0.603818 0.943660 0.799698 11.00000 0.01807 0.03911 = 0.03458 -0.02492 0.00614 -0.01256 AFIX 23 H34 2 0.681514 0.954254 0.818836 11.00000 -1.20000 H35 2 0.565576 1.019497 0.754129 11.00000 -1.20000 AFIX 0 C32 1 0.291172 0.969946 0.756141 11.00000 0.01688 0.04611 = 0.03443 -0.02378 0.00255 -0.01218 H43 2 0.171348 1.104032 0.904175 11.00000 0.01926 H44 2 0.280726 1.092473 0.930139 11.00000 0.02734 HKLF 4 REM Takata160710 REM R1 = 0.0490 for 5648 Fo > 4sig(Fo) and 0.0668 for all 7913 data REM 483 parameters refined using 1 restraints END WGHT 0.0527 0.0000 REM Instructions for potential hydrogen bonds HTAB C35 O4 EQIV $1 -x+1, -y+1, -z+2 HTAB C3 O7_$1 HTAB C5 O4_$1 EQIV $2 -x+1, -y+1, -z+1 HTAB C13 O6_$2 EQIV $3 -x, -y+1, -z+2 HTAB C15 O1_$3 EQIV $4 x, y-1, z HTAB C16 O10_$4 EQIV $5 x-1, y, z HTAB C16 O7_$5 HTAB C23 O6 EQIV $6 -x, -y+2, -z+2 HTAB O10 O1_$6 EQIV $7 -x+1, -y+2, -z+2 HTAB O10 O2_$7 REM Highest difference peak 1.287, deepest hole -0.505, 1-sigma level 0.142 Q1 1 0.3642 0.9472 0.8372 11.00000 0.05 1.29 Q2 1 0.9206 0.7186 0.6567 11.00000 0.05 0.96 Q3 1 0.2446 0.8721 0.9322 11.00000 0.05 0.80 Q4 1 0.5375 0.1965 0.5592 11.00000 0.05 0.79 Q5 1 0.2007 0.9001 0.8913 11.00000 0.05 0.79 Q6 1 0.2608 0.9142 0.8243 11.00000 0.05 0.76 Q7 1 0.2623 0.5800 1.0725 11.00000 0.05 0.76 Q8 1 0.4204 0.9177 0.8767 11.00000 0.05 0.76 Q9 1 0.4839 0.4964 0.9410 11.00000 0.05 0.70 Q10 1 0.2679 0.9543 0.8460 11.00000 0.05 0.63 Q11 1 0.2901 0.8971 0.9717 11.00000 0.05 0.61 Q12 1 0.3125 0.7967 0.9218 11.00000 0.05 0.60 Q13 1 0.3694 0.9450 0.9105 11.00000 0.05 0.59 Q14 1 0.5335 0.3173 0.5297 11.00000 0.05 0.59 Q15 1 0.4475 0.5064 1.0162 11.00000 0.05 0.58 Q16 1 0.2842 0.8256 0.9034 11.00000 0.05 0.55 Q17 1 0.6640 0.7529 0.6322 11.00000 0.05 0.55 Q18 1 0.1241 0.4669 0.7590 11.00000 0.05 0.54 Q19 1 0.4761 0.8753 1.0108 11.00000 0.05 0.53 Q20 1 1.1008 0.1635 0.5558 11.00000 0.05 0.51 Q21 1 0.8151 0.1554 0.4874 11.00000 0.05 0.50 Q22 1 0.5819 0.4595 0.9501 11.00000 0.05 0.48 Q23 1 0.6085 0.8025 0.6622 11.00000 0.05 0.48 Q24 1 1.0032 0.1975 0.5771 11.00000 0.05 0.46 Q25 1 0.8566 0.4521 0.6177 11.00000 0.05 0.46 ; _shelx_res_checksum 79941 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 +X,+Y,+Z 2 -X,-Y,-Z 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.30849(3) 0.90895(3) 0.88389(2) 0.01949(10) Uani 1 1 d . . . . . O1 O -0.0058(2) 0.8185(2) 1.09504(17) 0.0224(5) Uani 1 1 d . . . . . O2 O 0.6621(2) 0.8679(2) 0.9827(2) 0.0319(6) Uani 1 1 d . . . . . O3 O 0.1245(3) 0.5317(2) 0.73201(17) 0.0252(6) Uani 1 1 d . . . . . O4 O 0.3463(3) 0.3505(3) 0.7039(2) 0.0403(7) Uani 1 1 d . . . . . O5 O 0.5627(3) 0.2582(3) 0.5775(2) 0.0411(7) Uani 1 1 d . . . . . O6 O 0.8378(2) 0.2116(2) 0.53294(18) 0.0261(6) Uani 1 1 d . . . . . O7 O 0.9796(3) 0.3227(2) 0.61261(19) 0.0293(6) Uani 1 1 d . . . . . O8 O 0.7510(3) 0.5913(2) 0.61910(18) 0.0263(6) Uani 1 1 d . . . . . O9 O 0.2802(3) 1.0124(3) 0.6767(2) 0.0450(8) Uani 1 1 d . . . . . O10 O 0.2557(2) 1.0801(2) 0.89201(19) 0.0192(5) Uani 1 1 d . . . . . O11 O 0.3587(4) 0.7256(4) 0.9050(3) 0.0208(10) Uani 0.651(6) 1 d . . P A 1 C33 C 0.393(2) 0.684(2) 0.8350(19) 0.033(4) Uani 0.651(6) 1 d . . P A 1 H36 H 0.4024 0.7345 0.7710 0.039 Uiso 0.651(6) 1 calc R U P A 1 N4 N 0.4167(5) 0.5648(4) 0.8574(4) 0.0290(13) Uani 0.651(6) 1 d . . P A 1 C34 C 0.3857(9) 0.4784(6) 0.9522(5) 0.056(2) Uani 0.651(6) 1 d . . P A 1 H37 H 0.4679 0.4271 0.9748 0.084 Uiso 0.651(6) 1 calc R U P A 1 H38 H 0.3299 0.4306 0.9472 0.084 Uiso 0.651(6) 1 calc R U P A 1 H39 H 0.3388 0.5207 0.9972 0.084 Uiso 0.651(6) 1 calc R U P A 1 C35 C 0.4630(7) 0.5177(6) 0.7783(5) 0.0414(19) Uani 0.651(6) 1 d . . P A 1 H40 H 0.5568 0.4798 0.7785 0.062 Uiso 0.651(6) 1 calc R U P A 1 H41 H 0.4508 0.5820 0.7183 0.062 Uiso 0.651(6) 1 calc R U P A 1 H42 H 0.4123 0.4595 0.7850 0.062 Uiso 0.651(6) 1 calc R U P A 1 C36 C 0.3579(11) 0.7711(12) 0.8564(10) 0.025(3) Uani 0.349(6) 1 d D . P A 2 O12 O 0.393(3) 0.680(2) 0.848(2) 0.025(3) Uani 0.349(6) 1 d D . P A 2 N1 N 0.3242(3) 0.8523(2) 1.0245(2) 0.0181(6) Uani 1 1 d . . . . . N2 N 0.1166(3) 0.8855(2) 0.9468(2) 0.0183(6) Uani 1 1 d . . . . . N3 N 0.5056(3) 0.9118(3) 0.8836(2) 0.0230(7) Uani 1 1 d . . . . . C1 C 0.0972(3) 0.8458(3) 1.0406(2) 0.0176(7) Uani 1 1 d . . . . . C2 C 0.2174(3) 0.8301(3) 1.0859(2) 0.0181(7) Uani 1 1 d . . . . . C3 C 0.2217(3) 0.7954(3) 1.1828(3) 0.0212(7) Uani 1 1 d . . . . . H1 H 0.1458 0.7796 1.2278 0.025 Uiso 1 1 calc R U . . . C4 C 0.3422(4) 0.7846(3) 1.2116(3) 0.0257(8) Uani 1 1 d . . . . . H2 H 0.3482 0.7606 1.2774 0.031 Uiso 1 1 calc R U . . . C5 C 0.4525(3) 0.8082(3) 1.1460(3) 0.0232(8) Uani 1 1 d . . . . . H3 H 0.5341 0.8001 1.1659 0.028 Uiso 1 1 calc R U . . . C6 C 0.4406(3) 0.8439(3) 1.0505(3) 0.0207(7) Uani 1 1 d . . . . . C7 C 0.5464(3) 0.8760(3) 0.9676(3) 0.0241(8) Uani 1 1 d . . . . . C8 C 0.0086(3) 0.8989(3) 0.8952(2) 0.0217(7) Uani 1 1 d . . . . . H4 H -0.0005 0.9757 0.8436 0.026 Uiso 1 1 calc R U . . . H5 H -0.0754 0.8986 0.9391 0.026 Uiso 1 1 calc R U . . . C9 C 0.0344(3) 0.8003(3) 0.8530(2) 0.0193(7) Uani 1 1 d . . . . . C10 C 0.0352(4) 0.6849(3) 0.9108(3) 0.0281(8) Uani 1 1 d . . . . . H6 H 0.0164 0.6683 0.9777 0.034 Uiso 1 1 calc R U . . . C11 C 0.0627(4) 0.5929(3) 0.8739(3) 0.0280(8) Uani 1 1 d . . . . . H7 H 0.0609 0.5148 0.9151 0.034 Uiso 1 1 calc R U . . . C12 C 0.0926(3) 0.6157(3) 0.7772(2) 0.0207(7) Uani 1 1 d . . . . . C13 C 0.0915(3) 0.7297(3) 0.7176(2) 0.0220(7) Uani 1 1 d . . . . . H8 H 0.1107 0.7456 0.6508 0.026 Uiso 1 1 calc R U . . . C14 C 0.0626(3) 0.8208(3) 0.7552(3) 0.0235(8) Uani 1 1 d . . . . . H9 H 0.0618 0.8990 0.7135 0.028 Uiso 1 1 calc R U . . . C15 C 0.1364(4) 0.4098(3) 0.7882(3) 0.0283(8) Uani 1 1 d . . . . . H10 H 0.0479 0.3911 0.8136 0.034 Uiso 1 1 calc R U . . . H11 H 0.1845 0.3913 0.8422 0.034 Uiso 1 1 calc R U . . . C16 C 0.2114(4) 0.3401(3) 0.7236(3) 0.0308(9) Uani 1 1 d . . . . . H12 H 0.2060 0.2562 0.7544 0.037 Uiso 1 1 calc R U . . . H13 H 0.1727 0.3704 0.6637 0.037 Uiso 1 1 calc R U . . . C17 C 0.3888(4) 0.4116(4) 0.6094(3) 0.0406(10) Uani 1 1 d . . . . . H14 H 0.4594 0.4505 0.6077 0.049 Uiso 1 1 calc R U . . . H15 H 0.3142 0.4737 0.5820 0.049 Uiso 1 1 calc R U . . . C18 C 0.4402(4) 0.3312(4) 0.5502(3) 0.0390(10) Uani 1 1 d . . . . . H16 H 0.3761 0.2820 0.5598 0.047 Uiso 1 1 calc R U . . . H17 H 0.4525 0.3783 0.4820 0.047 Uiso 1 1 calc R U . . . C19 C 0.6294(4) 0.1920(4) 0.5161(3) 0.0381(10) Uani 1 1 d . . . . . H18 H 0.6401 0.2451 0.4497 0.046 Uiso 1 1 calc R U . . . H19 H 0.5778 0.1350 0.5196 0.046 Uiso 1 1 calc R U . . . C20 C 0.7639(4) 0.1269(3) 0.5466(3) 0.0317(9) Uani 1 1 d . . . . . H20 H 0.7535 0.0779 0.6143 0.038 Uiso 1 1 calc R U . . . H21 H 0.8099 0.0745 0.5082 0.038 Uiso 1 1 calc R U . . . C21 C 0.9637(4) 0.1615(3) 0.5630(3) 0.0297(9) Uani 1 1 d . . . . . H22 H 1.0161 0.1084 0.5266 0.036 Uiso 1 1 calc R U . . . H23 H 0.9538 0.1144 0.6312 0.036 Uiso 1 1 calc R U . . . C22 C 1.0337(4) 0.2576(3) 0.5474(3) 0.0299(9) Uani 1 1 d . . . . . H24 H 1.1281 0.2224 0.5538 0.036 Uiso 1 1 calc R U . . . H25 H 1.0287 0.3125 0.4817 0.036 Uiso 1 1 calc R U . . . C23 C 0.8713(3) 0.4186(3) 0.5836(3) 0.0249(8) Uani 1 1 d . . . . . H26 H 0.7917 0.3894 0.5877 0.030 Uiso 1 1 calc R U . . . H27 H 0.8934 0.4690 0.5176 0.030 Uiso 1 1 calc R U . . . C24 C 0.8484(4) 0.4869(3) 0.6528(3) 0.0255(8) Uani 1 1 d . . . . . H28 H 0.8165 0.4393 0.7177 0.031 Uiso 1 1 calc R U . . . H29 H 0.9314 0.5074 0.6543 0.031 Uiso 1 1 calc R U . . . C25 C 0.7218(3) 0.6722(3) 0.6666(3) 0.0237(8) Uani 1 1 d . . . . . C26 C 0.7613(3) 0.6522(3) 0.7523(3) 0.0261(8) Uani 1 1 d . . . . . H30 H 0.8139 0.5780 0.7827 0.031 Uiso 1 1 calc R U . . . C27 C 0.7242(3) 0.7402(3) 0.7942(3) 0.0281(9) Uani 1 1 d . . . . . H31 H 0.7521 0.7254 0.8533 0.034 Uiso 1 1 calc R U . . . C28 C 0.6474(3) 0.8493(3) 0.7518(3) 0.0242(8) Uani 1 1 d . . . . . C29 C 0.6092(4) 0.8684(3) 0.6647(3) 0.0255(8) Uani 1 1 d . . . . . H32 H 0.5566 0.9426 0.6344 0.031 Uiso 1 1 calc R U . . . C30 C 0.6461(4) 0.7821(3) 0.6213(3) 0.0274(8) Uani 1 1 d . . . . . H33 H 0.6203 0.7974 0.5614 0.033 Uiso 1 1 calc R U . . . C31 C 0.6038(3) 0.9437(3) 0.7997(3) 0.0271(8) Uani 1 1 d . . . . . H34 H 0.6815 0.9543 0.8188 0.033 Uiso 1 1 calc R U . . . H35 H 0.5656 1.0195 0.7541 0.033 Uiso 1 1 calc R U . . . C32 C 0.2912(3) 0.9699(4) 0.7561(3) 0.0292(9) Uani 1 1 d . . . . . H43 H 0.171(4) 1.104(3) 0.904(3) 0.019(10) Uiso 1 1 d . . . . . H44 H 0.281(4) 1.092(4) 0.930(3) 0.027(12) Uiso 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.01358(14) 0.02679(17) 0.02392(15) -0.01594(12) -0.00077(10) -0.00433(11) O1 0.0164(12) 0.0218(13) 0.0284(13) -0.0078(11) -0.0013(10) -0.0052(10) O2 0.0135(12) 0.0524(17) 0.0454(17) -0.0357(15) -0.0044(11) -0.0037(12) O3 0.0396(15) 0.0191(12) 0.0177(12) -0.0061(10) -0.0037(11) -0.0075(11) O4 0.0316(16) 0.0483(18) 0.0368(17) -0.0137(15) -0.0124(13) 0.0044(14) O5 0.0313(16) 0.061(2) 0.0303(15) -0.0201(15) -0.0068(12) 0.0011(14) O6 0.0270(13) 0.0229(13) 0.0278(14) -0.0078(11) -0.0049(11) -0.0044(11) O7 0.0307(14) 0.0256(14) 0.0346(15) -0.0167(12) -0.0091(12) 0.0025(11) O8 0.0314(14) 0.0258(14) 0.0287(14) -0.0189(12) -0.0078(11) -0.0001(11) O9 0.0437(18) 0.074(2) 0.0231(15) -0.0191(16) -0.0027(13) -0.0183(16) O10 0.0139(12) 0.0217(13) 0.0264(14) -0.0124(11) -0.0043(10) -0.0030(10) O11 0.026(2) 0.017(2) 0.023(2) -0.013(2) -0.0112(19) 0.0034(17) C33 0.030(5) 0.038(8) 0.048(10) -0.038(8) 0.006(6) -0.012(5) N4 0.028(3) 0.028(3) 0.037(3) -0.020(2) -0.009(2) 0.000(2) C34 0.083(6) 0.032(4) 0.049(5) -0.008(3) -0.008(4) -0.014(4) C35 0.039(4) 0.044(4) 0.056(5) -0.038(4) 0.008(3) -0.015(3) C36 0.014(5) 0.033(6) 0.026(5) -0.005(5) -0.003(4) -0.006(5) O12 0.014(5) 0.033(6) 0.026(5) -0.005(5) -0.003(4) -0.006(5) N1 0.0142(13) 0.0171(14) 0.0265(15) -0.0112(12) -0.0054(11) -0.0011(11) N2 0.0145(13) 0.0217(15) 0.0244(15) -0.0147(13) -0.0025(11) -0.0032(11) N3 0.0140(14) 0.0370(18) 0.0281(16) -0.0245(15) 0.0017(12) -0.0061(13) C1 0.0153(15) 0.0143(16) 0.0260(18) -0.0107(14) -0.0028(13) -0.0018(13) C2 0.0198(16) 0.0125(16) 0.0241(17) -0.0084(14) -0.0034(13) -0.0030(13) C3 0.0234(17) 0.0161(17) 0.0258(18) -0.0090(15) -0.0049(14) -0.0024(14) C4 0.032(2) 0.0189(18) 0.0264(19) -0.0055(15) -0.0129(16) -0.0015(15) C5 0.0212(17) 0.0215(18) 0.031(2) -0.0137(16) -0.0109(15) 0.0012(14) C6 0.0150(16) 0.0193(17) 0.035(2) -0.0186(16) -0.0072(14) 0.0018(13) C7 0.0145(16) 0.0285(19) 0.040(2) -0.0264(18) -0.0033(15) -0.0003(14) C8 0.0177(16) 0.0265(19) 0.0240(17) -0.0114(15) -0.0035(14) -0.0046(14) C9 0.0143(16) 0.0241(18) 0.0246(17) -0.0108(15) -0.0041(13) -0.0070(13) C10 0.038(2) 0.032(2) 0.0171(17) -0.0077(16) 0.0001(15) -0.0156(17) C11 0.044(2) 0.0224(19) 0.0192(18) -0.0064(15) -0.0004(16) -0.0139(17) C12 0.0208(17) 0.0238(18) 0.0219(17) -0.0108(15) -0.0042(14) -0.0060(14) C13 0.0264(18) 0.0241(19) 0.0158(16) -0.0067(14) -0.0043(14) -0.0044(15) C14 0.0255(18) 0.0215(18) 0.0234(18) -0.0043(15) -0.0076(14) -0.0054(15) C15 0.040(2) 0.0207(19) 0.0267(19) -0.0057(16) -0.0068(17) -0.0105(16) C16 0.037(2) 0.0229(19) 0.032(2) -0.0081(17) -0.0071(17) -0.0053(17) C17 0.036(2) 0.039(2) 0.046(3) -0.012(2) -0.003(2) -0.0114(19) C18 0.041(2) 0.047(3) 0.029(2) -0.008(2) -0.0102(18) -0.011(2) C19 0.038(2) 0.043(3) 0.039(2) -0.015(2) -0.0078(19) -0.012(2) C20 0.033(2) 0.030(2) 0.038(2) -0.0160(18) -0.0038(17) -0.0089(17) C21 0.029(2) 0.0233(19) 0.036(2) -0.0141(17) -0.0014(17) -0.0016(16) C22 0.0254(19) 0.028(2) 0.040(2) -0.0208(18) 0.0018(17) -0.0030(16) C23 0.0260(19) 0.0231(19) 0.0293(19) -0.0142(16) -0.0050(15) -0.0023(15) C24 0.030(2) 0.0210(18) 0.0265(19) -0.0093(16) -0.0045(15) -0.0051(15) C25 0.0220(18) 0.030(2) 0.0266(19) -0.0180(17) 0.0034(14) -0.0099(15) C26 0.0219(18) 0.033(2) 0.0273(19) -0.0172(17) -0.0016(15) -0.0032(16) C27 0.0199(18) 0.044(2) 0.0267(19) -0.0223(18) -0.0016(15) -0.0037(17) C28 0.0166(16) 0.033(2) 0.0308(19) -0.0219(17) 0.0057(14) -0.0099(15) C29 0.0235(18) 0.0267(19) 0.0289(19) -0.0141(16) 0.0019(15) -0.0068(15) C30 0.030(2) 0.030(2) 0.0251(19) -0.0134(16) -0.0034(15) -0.0057(17) C31 0.0181(17) 0.039(2) 0.035(2) -0.0249(18) 0.0061(15) -0.0126(16) C32 0.0169(17) 0.046(2) 0.034(2) -0.0238(19) 0.0026(15) -0.0122(16) 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 for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.0000 0.0000 ; International Tables for Crystallography (Vol. C, Table 6.1.1.4) ; N N 0.0061 0.0033 ; International Tables for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.0106 0.0060 ; International Tables for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Ru Ru -1.2594 0.8363 ; International Tables for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; 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 C36 Ru1 C32 81.5(5) . . ? C36 Ru1 N1 102.0(5) . . ? C32 Ru1 N1 176.47(14) . . ? C36 Ru1 O10 170.9(5) . . ? C32 Ru1 O10 89.63(14) . . ? N1 Ru1 O10 86.85(11) . . ? C36 Ru1 N2 94.5(4) . . ? C32 Ru1 N2 101.96(14) . . ? N1 Ru1 N2 77.98(11) . . ? O10 Ru1 N2 89.40(10) . . ? C36 Ru1 N3 92.1(4) . . ? C32 Ru1 N3 102.68(14) . . ? N1 Ru1 N3 77.24(11) . . ? O10 Ru1 N3 87.73(11) . . ? N2 Ru1 N3 155.17(12) . . ? C32 Ru1 O11 101.48(17) . . ? N1 Ru1 O11 82.04(14) . . ? O10 Ru1 O11 168.76(14) . . ? N2 Ru1 O11 86.63(14) . . ? N3 Ru1 O11 91.47(14) . . ? C12 O3 C15 119.1(3) . . ? C17 O4 C16 115.2(3) . . ? C19 O5 C18 113.1(3) . . ? C20 O6 C21 113.4(3) . . ? C23 O7 C22 114.5(3) . . ? C25 O8 C24 116.7(3) . . ? Ru1 O10 H43 113(2) . . ? Ru1 O10 H44 119(3) . . ? H43 O10 H44 102(4) . . ? C33 O11 Ru1 122.0(12) . . ? O11 C33 N4 117(2) . . ? O11 C33 H36 121.7 . . ? N4 C33 H36 121.7 . . ? C33 N4 C35 116.6(12) . . ? C33 N4 C34 126.8(11) . . ? C35 N4 C34 116.1(5) . . ? N4 C34 H37 109.5 . . ? N4 C34 H38 109.5 . . ? H37 C34 H38 109.5 . . ? N4 C34 H39 109.5 . . ? H37 C34 H39 109.5 . . ? H38 C34 H39 109.5 . . ? N4 C35 H40 109.5 . . ? N4 C35 H41 109.5 . . ? H40 C35 H41 109.5 . . ? N4 C35 H42 109.5 . . ? H40 C35 H42 109.5 . . ? H41 C35 H42 109.5 . . ? O12 C36 Ru1 173(2) . . ? C2 N1 C6 123.5(3) . . ? C2 N1 Ru1 117.9(2) . . ? C6 N1 Ru1 118.6(2) . . ? C1 N2 C8 118.5(3) . . ? C1 N2 Ru1 115.8(2) . . ? C8 N2 Ru1 125.3(2) . . ? C7 N3 C31 116.8(3) . . ? C7 N3 Ru1 116.7(2) . . ? C31 N3 Ru1 126.4(2) . . ? O1 C1 N2 128.4(3) . . ? O1 C1 C2 117.8(3) . . ? N2 C1 C2 113.8(3) . . ? N1 C2 C3 120.1(3) . . ? N1 C2 C1 114.4(3) . . ? C3 C2 C1 125.5(3) . . ? C2 C3 C4 117.5(3) . . ? C2 C3 H1 121.3 . . ? C4 C3 H1 121.3 . . ? C5 C4 C3 121.3(3) . . ? C5 C4 H2 119.4 . . ? C3 C4 H2 119.4 . . ? C4 C5 C6 118.1(3) . . ? C4 C5 H3 120.9 . . ? C6 C5 H3 120.9 . . ? N1 C6 C5 119.5(3) . . ? N1 C6 C7 113.5(3) . . ? C5 C6 C7 127.0(3) . . ? O2 C7 N3 126.4(4) . . ? O2 C7 C6 119.6(3) . . ? N3 C7 C6 113.9(3) . . ? N2 C8 C9 111.4(3) . . ? N2 C8 H4 109.4 . . ? C9 C8 H4 109.4 . . ? N2 C8 H5 109.4 . . ? C9 C8 H5 109.4 . . ? H4 C8 H5 108.0 . . ? C10 C9 C14 117.1(3) . . ? C10 C9 C8 121.1(3) . . ? C14 C9 C8 121.8(3) . . ? C9 C10 C11 122.0(3) . . ? C9 C10 H6 119.0 . . ? C11 C10 H6 119.0 . . ? C12 C11 C10 119.5(3) . . ? C12 C11 H7 120.3 . . ? C10 C11 H7 120.3 . . ? C11 C12 C13 120.0(3) . . ? C11 C12 O3 125.0(3) . . ? C13 C12 O3 115.0(3) . . ? C12 C13 C14 120.0(3) . . ? C12 C13 H8 120.0 . . ? C14 C13 H8 120.0 . . ? C13 C14 C9 121.4(3) . . ? C13 C14 H9 119.3 . . ? C9 C14 H9 119.3 . . ? O3 C15 C16 106.5(3) . . ? O3 C15 H10 110.4 . . ? C16 C15 H10 110.4 . . ? O3 C15 H11 110.4 . . ? C16 C15 H11 110.4 . . ? H10 C15 H11 108.6 . . ? O4 C16 C15 108.9(3) . . ? O4 C16 H12 109.9 . . ? C15 C16 H12 109.9 . . ? O4 C16 H13 109.9 . . ? C15 C16 H13 109.9 . . ? H12 C16 H13 108.3 . . ? O4 C17 C18 111.9(4) . . ? O4 C17 H14 109.2 . . ? C18 C17 H14 109.2 . . ? O4 C17 H15 109.2 . . ? C18 C17 H15 109.2 . . ? H14 C17 H15 107.9 . . ? O5 C18 C17 108.7(3) . . ? O5 C18 H16 109.9 . . ? C17 C18 H16 109.9 . . ? O5 C18 H17 109.9 . . ? C17 C18 H17 109.9 . . ? H16 C18 H17 108.3 . . ? O5 C19 C20 108.3(3) . . ? O5 C19 H18 110.0 . . ? C20 C19 H18 110.0 . . ? O5 C19 H19 110.0 . . ? C20 C19 H19 110.0 . . ? H18 C19 H19 108.4 . . ? O6 C20 C19 108.0(3) . . ? O6 C20 H20 110.1 . . ? C19 C20 H20 110.1 . . ? O6 C20 H21 110.1 . . ? C19 C20 H21 110.1 . . ? H20 C20 H21 108.4 . . ? O6 C21 C22 109.6(3) . . ? O6 C21 H22 109.8 . . ? C22 C21 H22 109.8 . . ? O6 C21 H23 109.8 . . ? C22 C21 H23 109.8 . . ? H22 C21 H23 108.2 . . ? O7 C22 C21 113.0(3) . . ? O7 C22 H24 109.0 . . ? C21 C22 H24 109.0 . . ? O7 C22 H25 109.0 . . ? C21 C22 H25 109.0 . . ? H24 C22 H25 107.8 . . ? O7 C23 C24 104.7(3) . . ? O7 C23 H26 110.8 . . ? C24 C23 H26 110.8 . . ? O7 C23 H27 110.8 . . ? C24 C23 H27 110.8 . . ? H26 C23 H27 108.9 . . ? O8 C24 C23 106.2(3) . . ? O8 C24 H28 110.5 . . ? C23 C24 H28 110.5 . . ? O8 C24 H29 110.5 . . ? C23 C24 H29 110.5 . . ? H28 C24 H29 108.7 . . ? O8 C25 C26 125.2(3) . . ? O8 C25 C30 115.0(3) . . ? C26 C25 C30 119.8(3) . . ? C25 C26 C27 120.0(4) . . ? C25 C26 H30 120.0 . . ? C27 C26 H30 120.0 . . ? C28 C27 C26 121.5(4) . . ? C28 C27 H31 119.3 . . ? C26 C27 H31 119.3 . . ? C27 C28 C29 117.7(3) . . ? C27 C28 C31 121.1(3) . . ? C29 C28 C31 121.2(3) . . ? C30 C29 C28 121.7(4) . . ? C30 C29 H32 119.2 . . ? C28 C29 H32 119.2 . . ? C29 C30 C25 119.2(4) . . ? C29 C30 H33 120.4 . . ? C25 C30 H33 120.4 . . ? N3 C31 C28 111.2(3) . . ? N3 C31 H34 109.4 . . ? C28 C31 H34 109.4 . . ? N3 C31 H35 109.4 . . ? C28 C31 H35 109.4 . . ? H34 C31 H35 108.0 . . ? O9 C32 Ru1 177.3(4) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C36 1.824(13) . ? Ru1 C32 1.849(4) . ? Ru1 N1 2.031(3) . ? Ru1 O10 2.092(3) . ? Ru1 N2 2.101(3) . ? Ru1 N3 2.104(3) . ? Ru1 O11 2.116(4) . ? O1 C1 1.263(4) . ? O2 C7 1.270(4) . ? O3 C12 1.381(4) . ? O3 C15 1.434(4) . ? O4 C17 1.401(5) . ? O4 C16 1.430(5) . ? O5 C19 1.415(5) . ? O5 C18 1.419(5) . ? O6 C20 1.413(4) . ? O6 C21 1.413(4) . ? O7 C23 1.427(4) . ? O7 C22 1.432(4) . ? O8 C25 1.375(4) . ? O8 C24 1.429(4) . ? O9 C32 1.152(5) . ? O10 H43 0.86(4) . ? O10 H44 0.77(4) . ? O11 C33 1.288(19) . ? C33 N4 1.36(2) . ? C33 H36 0.9500 . ? N4 C35 1.460(7) . ? N4 C34 1.487(9) . ? C34 H37 0.9800 . ? C34 H38 0.9800 . ? C34 H39 0.9800 . ? C35 H40 0.9800 . ? C35 H41 0.9800 . ? C35 H42 0.9800 . ? C36 O12 1.142(18) . ? N1 C2 1.322(4) . ? N1 C6 1.348(4) . ? N2 C1 1.321(4) . ? N2 C8 1.472(4) . ? N3 C7 1.327(5) . ? N3 C31 1.465(4) . ? C1 C2 1.520(4) . ? C2 C3 1.389(5) . ? C3 C4 1.402(5) . ? C3 H1 0.9500 . ? C4 C5 1.382(5) . ? C4 H2 0.9500 . ? C5 C6 1.385(5) . ? C5 H3 0.9500 . ? C6 C7 1.505(5) . ? C8 C9 1.518(5) . ? C8 H4 0.9900 . ? C8 H5 0.9900 . ? C9 C10 1.385(5) . ? C9 C14 1.396(5) . ? C10 C11 1.386(5) . ? C10 H6 0.9500 . ? C11 C12 1.377(5) . ? C11 H7 0.9500 . ? C12 C13 1.379(5) . ? C13 C14 1.382(5) . ? C13 H8 0.9500 . ? C14 H9 0.9500 . ? C15 C16 1.499(5) . ? C15 H10 0.9900 . ? C15 H11 0.9900 . ? C16 H12 0.9900 . ? C16 H13 0.9900 . ? C17 C18 1.500(6) . ? C17 H14 0.9900 . ? C17 H15 0.9900 . ? C18 H16 0.9900 . ? C18 H17 0.9900 . ? C19 C20 1.518(5) . ? C19 H18 0.9900 . ? C19 H19 0.9900 . ? C20 H20 0.9900 . ? C20 H21 0.9900 . ? C21 C22 1.499(5) . ? C21 H22 0.9900 . ? C21 H23 0.9900 . ? C22 H24 0.9900 . ? C22 H25 0.9900 . ? C23 C24 1.522(5) . ? C23 H26 0.9900 . ? C23 H27 0.9900 . ? C24 H28 0.9900 . ? C24 H29 0.9900 . ? C25 C26 1.378(5) . ? C25 C30 1.400(5) . ? C26 C27 1.387(5) . ? C26 H30 0.9500 . ? C27 C28 1.386(5) . ? C27 H31 0.9500 . ? C28 C29 1.395(5) . ? C28 C31 1.516(5) . ? C29 C30 1.384(5) . ? C29 H32 0.9500 . ? C30 H33 0.9500 . ? C31 H34 0.9900 . ? C31 H35 0.9900 . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_angle_DHA _geom_hbond_publ_flag O10 H43 O1 . . 2_577 2.606(3) 0.86(4) 1.76(4) 166(3) no O10 H44 O2 . . 2_677 2.607(5) 0.77(5) 1.84(5) 176(4) no 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 Ru1 O11 C33 N4 -176.6(11) . . . . ? O11 C33 N4 C35 -176.8(13) . . . . ? O11 C33 N4 C34 11(3) . . . . ? C8 N2 C1 O1 -1.6(5) . . . . ? Ru1 N2 C1 O1 -175.9(3) . . . . ? C8 N2 C1 C2 177.2(2) . . . . ? Ru1 N2 C1 C2 2.9(3) . . . . ? C6 N1 C2 C3 -0.4(5) . . . . ? Ru1 N1 C2 C3 -177.6(2) . . . . ? C6 N1 C2 C1 179.7(3) . . . . ? Ru1 N1 C2 C1 2.6(4) . . . . ? O1 C1 C2 N1 175.3(3) . . . . ? N2 C1 C2 N1 -3.6(4) . . . . ? O1 C1 C2 C3 -4.5(5) . . . . ? N2 C1 C2 C3 176.5(3) . . . . ? N1 C2 C3 C4 -0.4(5) . . . . ? C1 C2 C3 C4 179.4(3) . . . . ? C2 C3 C4 C5 0.3(5) . . . . ? C3 C4 C5 C6 0.5(5) . . . . ? C2 N1 C6 C5 1.3(5) . . . . ? Ru1 N1 C6 C5 178.4(2) . . . . ? C2 N1 C6 C7 -178.8(3) . . . . ? Ru1 N1 C6 C7 -1.6(4) . . . . ? C4 C5 C6 N1 -1.3(5) . . . . ? C4 C5 C6 C7 178.8(3) . . . . ? C31 N3 C7 O2 0.8(5) . . . . ? Ru1 N3 C7 O2 177.8(3) . . . . ? C31 N3 C7 C6 -179.5(3) . . . . ? Ru1 N3 C7 C6 -2.5(4) . . . . ? N1 C6 C7 O2 -177.6(3) . . . . ? C5 C6 C7 O2 2.3(5) . . . . ? N1 C6 C7 N3 2.7(4) . . . . ? C5 C6 C7 N3 -177.4(3) . . . . ? C1 N2 C8 C9 -103.7(3) . . . . ? Ru1 N2 C8 C9 70.0(3) . . . . ? N2 C8 C9 C10 66.9(4) . . . . ? N2 C8 C9 C14 -110.9(4) . . . . ? C14 C9 C10 C11 0.0(5) . . . . ? C8 C9 C10 C11 -177.9(3) . . . . ? C9 C10 C11 C12 1.3(6) . . . . ? C10 C11 C12 C13 -1.8(6) . . . . ? C10 C11 C12 O3 178.5(3) . . . . ? C15 O3 C12 C11 -4.2(5) . . . . ? C15 O3 C12 C13 176.1(3) . . . . ? C11 C12 C13 C14 1.1(5) . . . . ? O3 C12 C13 C14 -179.2(3) . . . . ? C12 C13 C14 C9 0.2(5) . . . . ? C10 C9 C14 C13 -0.7(5) . . . . ? C8 C9 C14 C13 177.2(3) . . . . ? C12 O3 C15 C16 -162.5(3) . . . . ? C17 O4 C16 C15 -113.4(4) . . . . ? O3 C15 C16 O4 71.8(4) . . . . ? C16 O4 C17 C18 -88.4(4) . . . . ? C19 O5 C18 C17 -170.7(4) . . . . ? O4 C17 C18 O5 -70.9(5) . . . . ? C18 O5 C19 C20 174.6(3) . . . . ? C21 O6 C20 C19 177.4(3) . . . . ? O5 C19 C20 O6 -64.4(4) . . . . ? C20 O6 C21 C22 -179.1(3) . . . . ? C23 O7 C22 C21 -86.4(4) . . . . ? O6 C21 C22 O7 72.1(4) . . . . ? C22 O7 C23 C24 -169.7(3) . . . . ? C25 O8 C24 C23 -174.9(3) . . . . ? O7 C23 C24 O8 173.3(3) . . . . ? C24 O8 C25 C26 -11.7(5) . . . . ? C24 O8 C25 C30 168.2(3) . . . . ? O8 C25 C26 C27 -179.1(3) . . . . ? C30 C25 C26 C27 1.0(6) . . . . ? C25 C26 C27 C28 0.0(6) . . . . ? C26 C27 C28 C29 -0.6(5) . . . . ? C26 C27 C28 C31 178.1(3) . . . . ? C27 C28 C29 C30 0.0(5) . . . . ? C31 C28 C29 C30 -178.6(3) . . . . ? C28 C29 C30 C25 1.1(6) . . . . ? O8 C25 C30 C29 178.5(3) . . . . ? C26 C25 C30 C29 -1.6(6) . . . . ? C7 N3 C31 C28 105.5(4) . . . . ? Ru1 N3 C31 C28 -71.2(4) . . . . ? C27 C28 C31 N3 -70.1(4) . . . . ? C29 C28 C31 N3 108.5(4) . . . . ?