#------------------------------------------------------------------------------ #$Date: 2026-05-07 23:59:01 +0100 (Thu, 07 May 2026) $ #$Revision: 305893 $ #$URL: svn://www.crystallography.net/cod/cif/7/72/09/7720998.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_7720998 loop_ _publ_author_name 'Bera, Jitendra K.' 'Yadav, Sudhir' 'Chourasia, Vishal' 'Ranjan, Prabodh' 'De, Subhabrata' 'Saptal, Vitthal Bhimrao' _publ_section_title ; Cooperative Ruthenium Catalyst for Deaminative Coupling of Primary Amines to Symmetrical Secondary Amines ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D6DT00770H _journal_year 2026 _chemical_formula_moiety 'C52 H43 N4 O P2 Ru, C4 H10 O' _chemical_formula_sum 'C56 H53 N4 O2 P2 Ru' _chemical_formula_weight 977.03 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _atom_sites_solution_hydrogens mixed _audit_creation_date 2022-03-01 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2022-03-23 deposited with the CCDC. 2026-05-05 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 116.642(2) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 40.571(2) _cell_length_b 11.2694(5) _cell_length_c 24.0395(11) _cell_measurement_reflns_used 9541 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 28.33 _cell_measurement_theta_min 2.36 _cell_volume 9824.1(8) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' _diffrn_ambient_temperature 100.15 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0665 _diffrn_reflns_av_unetI/netI 0.0454 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 47 _diffrn_reflns_limit_h_min -47 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_number 56524 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 24.712 _diffrn_reflns_theta_max 24.712 _diffrn_reflns_theta_min 2.226 _exptl_absorpt_coefficient_mu 0.430 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_correction_T_min 0.6233 _exptl_absorpt_correction_type none _exptl_crystal_colour red _exptl_crystal_density_diffrn 1.321 _exptl_crystal_description block _exptl_crystal_F_000 4056 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.18 _refine_diff_density_max 0.710 _refine_diff_density_min -0.542 _refine_diff_density_rms 0.089 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 593 _refine_ls_number_reflns 8373 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.029 _refine_ls_R_factor_all 0.0614 _refine_ls_R_factor_gt 0.0412 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0405P)^2^+31.7943P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0940 _refine_ls_wR_factor_ref 0.1016 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6554 _reflns_number_total 8373 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d6dt00770h2.cif _cod_data_source_block 2 _cod_original_cell_volume 9824.2(8) _cod_database_code 7720998 _shelx_shelxl_version_number 2018/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.927 _shelx_estimated_absorpt_t_min 0.919 _exptl_absorpt_special_details SADABS _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Others Fixed Sof: C13(0.5) C13A(0.5) 3.a Secondary CH2 refined with riding coordinates: C2S(H2SA,H2SB), C3S(H3SA,H3SB) 3.b Aromatic/amide H refined with riding coordinates: C1(H1), C2(H2), C3(H3), C6(H6), C7(H7), C10(H10), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C24(H24), C25(H25), C26(H26), C27(H27), C28(H28), C30(H30), C31(H31), C32(H32), C33(H33), C34(H34), C36(H36), C37(H37), C38(H38), C39(H39), C40(H40), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46), C48(H48), C49(H49), C50(H50), C51(H51), C52(H52) 3.c Idealised Me refined as rotating group: C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C1S(H1SA,H1SB,H1SC), C4S(H4SA,H4SB, H4SC) ; _shelx_res_file ; TITL 8augd_a.res in C2/c 2.res created by SHELXL-2018/3 at 20:47:03 on 01-Mar-2022 REM Old TITL 8augd in C2/c REM SHELXT solution in C2/c REM R1 0.120, Rweak 0.006, Alpha 0.035, Orientation as input REM Formula found by SHELXT: C56 N3 O2 P2 Ru REM 8augd_a.res in C2/c REM R1= 0.0847 for 8526 Fo > 4sig(Fo) and 0.1251 for all 12299 data REM 257 parameters refined using 0 restraints REM 261 parameters refined using 0 restraints REM Highest difference peak 1.645, deepest hole -2.894, 1-sigma level 0.163 REM 595 parameters refined using 0 restraints REM Highest difference peak 0.764, deepest hole -0.743, 1-sigma level 0.105 REM Highest difference peak 0.758, deepest hole -0.714, 1-sigma level 0.103 REM Highest difference peak 0.760, deepest hole -0.720, 1-sigma level 0.103 REM 590 parameters refined using 0 restraints REM Highest difference peak 1.559, deepest hole -0.686, 1-sigma level 0.111 REM 585 parameters refined using 0 restraints REM Highest difference peak 0.761, deepest hole -0.523, 1-sigma level 0.100 REM 593 parameters refined using 0 restraints REM Highest difference peak 0.722, deepest hole -0.538, 1-sigma level 0.090 REM Highest difference peak 0.709, deepest hole -0.542, 1-sigma level 0.089 REM Highest difference peak 0.710, deepest hole -0.542, 1-sigma level 0.089 CELL 0.71073 40.5713 11.2694 24.0395 90 116.642 90 ZERR 8 0.0021 0.0005 0.0011 0 0.002 0 LATT 7 SYMM -X,+Y,0.5-Z SFAC C H N O P Ru UNIT 448 424 32 16 16 8 L.S. 20 PLAN 5 SIZE 0.18 0.19 0.2 TEMP -173 GRID BOND $H fmap 2 acta MERG 2 SHEL 99999 0.85 OMIT -2 50.1 OMIT 0 2 2 OMIT -1 1 1 REM REM REM WGHT 0.040500 31.794300 FVAR 0.08719 P1 5 0.598097 0.763044 0.519044 11.00000 0.01813 0.01445 = 0.01705 -0.00021 0.00745 -0.00025 O1 4 0.549500 1.001429 0.561178 11.00000 0.04215 0.01355 = 0.03345 0.00095 0.01958 0.00330 N1 3 0.549553 0.487021 0.561688 11.00000 0.02183 0.01416 = 0.02853 0.00009 0.00619 -0.00177 C1 1 0.531012 0.388557 0.537028 11.00000 0.01985 0.01992 = 0.03177 -0.00204 0.00480 -0.00251 AFIX 43 H1 2 0.506143 0.395956 0.506280 11.00000 -1.20000 AFIX 0 P2 5 0.561042 0.762887 0.677018 11.00000 0.01748 0.01368 = 0.01861 0.00044 0.00843 -0.00070 N2 3 0.603700 0.580261 0.628540 11.00000 0.01507 0.01688 = 0.01634 0.00021 0.00443 -0.00025 C2 1 0.545637 0.274128 0.553273 11.00000 0.03127 0.01532 = 0.03225 -0.00230 0.01296 -0.00593 AFIX 43 H2 2 0.531094 0.206446 0.533683 11.00000 -1.20000 AFIX 0 N3 3 0.638853 0.784235 0.671793 11.00000 0.01744 0.01958 = 0.02270 -0.00400 0.00866 -0.00688 C3 1 0.580939 0.261831 0.597481 11.00000 0.03565 0.01458 = 0.03383 0.00287 0.01645 0.00372 AFIX 43 H3 2 0.591513 0.185172 0.609458 11.00000 -1.20000 AFIX 0 N4 3 0.660412 0.878404 0.700067 11.00000 0.02413 0.02568 = 0.02789 -0.00696 0.01088 -0.01130 C4 1 0.601761 0.363872 0.625452 11.00000 0.02405 0.02063 = 0.02253 0.00132 0.01178 0.00237 C5 1 0.584912 0.475932 0.605208 11.00000 0.02437 0.01632 = 0.01869 0.00129 0.01162 0.00079 C6 1 0.638682 0.360170 0.671698 11.00000 0.03000 0.02120 = 0.03149 0.00643 0.01287 0.00761 AFIX 43 H6 2 0.650751 0.286206 0.686124 11.00000 -1.20000 AFIX 0 C7 1 0.656754 0.463129 0.695332 11.00000 0.01811 0.03110 = 0.02570 0.00403 0.00404 0.00343 AFIX 43 H7 2 0.681433 0.461587 0.727248 11.00000 -1.20000 AFIX 0 C8 1 0.638888 0.573207 0.672501 11.00000 0.02001 0.02230 = 0.02141 -0.00081 0.01053 0.00124 C9 1 0.657661 0.683154 0.695999 11.00000 0.01627 0.02607 = 0.02214 0.00000 0.00854 -0.00151 C10 1 0.692687 0.711461 0.741873 11.00000 0.01944 0.03682 = 0.03402 0.00248 0.00290 -0.00344 AFIX 43 H10 2 0.711881 0.658636 0.766892 11.00000 -1.20000 AFIX 0 C11 1 0.693187 0.834052 0.742741 11.00000 0.02607 0.03690 = 0.03153 -0.00463 0.00753 -0.01260 C12 1 0.722878 0.918053 0.785758 11.00000 0.03304 0.04738 = 0.05977 -0.01041 -0.00114 -0.01652 PART 2 C13 1 0.716715 1.046323 0.762207 10.50000 0.06511 PART 0 C14 1 0.715090 0.944726 0.840946 11.00000 0.03749 0.13219 = 0.12363 -0.10507 0.01371 -0.01554 AFIX 137 H14A 2 0.732545 1.004616 0.867587 11.00000 -1.50000 H14B 2 0.717859 0.871928 0.864945 11.00000 -1.50000 H14C 2 0.689864 0.974775 0.825767 11.00000 -1.50000 AFIX 0 C15 1 0.760244 0.857365 0.810541 11.00000 0.02516 0.10125 = 0.06087 -0.03696 0.01127 -0.02394 AFIX 137 H15A 2 0.765020 0.833476 0.775625 11.00000 -1.50000 H15B 2 0.760304 0.787035 0.834563 11.00000 -1.50000 H15C 2 0.779497 0.912459 0.837413 11.00000 -1.50000 AFIX 0 C16 1 0.563441 0.909425 0.578016 11.00000 0.02123 0.01605 = 0.02172 -0.00606 0.01089 -0.00602 C17 1 0.630161 0.646990 0.520984 11.00000 0.02051 0.02353 = 0.01203 0.00128 0.00533 0.00275 C18 1 0.618568 0.528779 0.512698 11.00000 0.02188 0.02338 = 0.01835 -0.00102 0.00649 0.00057 AFIX 43 H18 2 0.593878 0.510410 0.504030 11.00000 -1.20000 AFIX 0 C19 1 0.642408 0.438766 0.516922 11.00000 0.03491 0.01939 = 0.02239 -0.00101 0.00935 0.00518 AFIX 43 H19 2 0.634278 0.358654 0.511715 11.00000 -1.20000 AFIX 0 C20 1 0.678268 0.464929 0.528767 11.00000 0.03081 0.03336 = 0.03035 0.00446 0.00967 0.01656 AFIX 43 H20 2 0.694801 0.402909 0.531564 11.00000 -1.20000 AFIX 0 C21 1 0.689911 0.581167 0.536489 11.00000 0.02293 0.04107 = 0.04006 0.00806 0.01031 0.00791 AFIX 43 H21 2 0.714412 0.599176 0.543876 11.00000 -1.20000 AFIX 0 C22 1 0.666320 0.671741 0.533597 11.00000 0.02431 0.02657 = 0.02652 0.00245 0.00746 0.00094 AFIX 43 H22 2 0.674882 0.751409 0.540276 11.00000 -1.20000 AFIX 0 C23 1 0.620329 0.899320 0.510111 11.00000 0.01647 0.01578 = 0.02798 0.00231 0.01071 0.00084 C24 1 0.636564 0.978839 0.559245 11.00000 0.02839 0.02270 = 0.02869 -0.00171 0.01657 -0.00609 AFIX 43 H24 2 0.636187 0.963789 0.597839 11.00000 -1.20000 AFIX 0 C25 1 0.653339 1.080520 0.551268 11.00000 0.03517 0.02407 = 0.03710 -0.00690 0.01823 -0.00886 AFIX 43 H25 2 0.664259 1.135302 0.584649 11.00000 -1.20000 AFIX 0 C26 1 0.654416 1.103256 0.495935 11.00000 0.02743 0.02173 = 0.04336 0.00805 0.02005 -0.00195 AFIX 43 H26 2 0.666032 1.173086 0.491198 11.00000 -1.20000 AFIX 0 C27 1 0.638486 1.023859 0.447215 11.00000 0.03095 0.03460 = 0.02990 0.01124 0.01713 0.00163 AFIX 43 H27 2 0.639296 1.038632 0.408940 11.00000 -1.20000 AFIX 0 C28 1 0.621390 0.923008 0.454302 11.00000 0.02848 0.02658 = 0.02452 0.00142 0.01181 -0.00241 AFIX 43 H28 2 0.610216 0.869178 0.420533 11.00000 -1.20000 AFIX 0 C29 1 0.559357 0.749905 0.440915 11.00000 0.01900 0.01729 = 0.01755 0.00301 0.00731 -0.00027 C30 1 0.558127 0.669148 0.396306 11.00000 0.02573 0.01932 = 0.01869 -0.00010 0.00791 0.00279 AFIX 43 H30 2 0.578228 0.616595 0.405573 11.00000 -1.20000 AFIX 0 C31 1 0.527776 0.664866 0.338449 11.00000 0.03768 0.02033 = 0.01857 -0.00253 0.00982 -0.00027 AFIX 43 H31 2 0.527007 0.608081 0.308683 11.00000 -1.20000 AFIX 0 C32 1 0.498592 0.742225 0.323499 11.00000 0.02572 0.02710 = 0.01773 0.00382 0.00580 -0.00061 AFIX 43 H32 2 0.477940 0.739267 0.283596 11.00000 -1.20000 AFIX 0 C33 1 0.499769 0.823742 0.367113 11.00000 0.02403 0.02943 = 0.02500 0.00770 0.00836 0.00658 AFIX 43 H33 2 0.479900 0.877662 0.357023 11.00000 -1.20000 AFIX 0 C34 1 0.529687 0.827656 0.425526 11.00000 0.02708 0.02347 = 0.02099 -0.00246 0.01010 0.00181 AFIX 43 H34 2 0.530047 0.883599 0.455356 11.00000 -1.20000 AFIX 0 C35 1 0.568779 0.901027 0.721871 11.00000 0.02038 0.01690 = 0.01467 0.00148 0.00479 0.00276 C36 1 0.549987 0.920920 0.757492 11.00000 0.02800 0.02080 = 0.02217 0.00364 0.01246 0.00244 AFIX 43 H36 2 0.533043 0.863466 0.758194 11.00000 -1.20000 AFIX 0 C37 1 0.556066 1.024722 0.791907 11.00000 0.03679 0.02408 = 0.01875 0.00152 0.01346 0.00934 AFIX 43 H37 2 0.543352 1.038092 0.816265 11.00000 -1.20000 AFIX 0 C38 1 0.580560 1.108346 0.790701 11.00000 0.03885 0.01977 = 0.01511 -0.00226 0.00676 0.00306 AFIX 43 H38 2 0.584422 1.179729 0.813822 11.00000 -1.20000 AFIX 0 C39 1 0.599436 1.088860 0.756155 11.00000 0.03050 0.02038 = 0.02273 -0.00249 0.00945 -0.00512 AFIX 43 H39 2 0.616443 1.146442 0.755803 11.00000 -1.20000 AFIX 0 C40 1 0.593644 0.984908 0.721733 11.00000 0.02304 0.02117 = 0.02072 -0.00210 0.00929 -0.00164 AFIX 43 H40 2 0.606796 0.971532 0.698090 11.00000 -1.20000 AFIX 0 C41 1 0.511155 0.744916 0.649107 11.00000 0.01860 0.01862 = 0.02072 -0.00318 0.00961 -0.00112 C42 1 0.494841 0.663647 0.671959 11.00000 0.02223 0.01966 = 0.02619 0.00116 0.01171 0.00140 AFIX 43 H42 2 0.509762 0.608951 0.703192 11.00000 -1.20000 AFIX 0 C43 1 0.456752 0.661151 0.649654 11.00000 0.02662 0.02122 = 0.03402 -0.00348 0.01733 -0.00489 AFIX 43 H43 2 0.445794 0.604364 0.665440 11.00000 -1.20000 AFIX 0 C44 1 0.434884 0.740491 0.604863 11.00000 0.01852 0.03340 = 0.02586 -0.00618 0.00867 -0.00159 AFIX 43 H44 2 0.408870 0.738626 0.589752 11.00000 -1.20000 AFIX 0 C45 1 0.450794 0.822746 0.581933 11.00000 0.02465 0.03749 = 0.03028 0.00772 0.01089 0.00682 AFIX 43 H45 2 0.435762 0.878592 0.551529 11.00000 -1.20000 AFIX 0 C46 1 0.488623 0.824140 0.603116 11.00000 0.02503 0.03110 = 0.02963 0.00741 0.01376 0.00163 AFIX 43 H46 2 0.499358 0.879490 0.586215 11.00000 -1.20000 AFIX 0 C47 1 0.583121 0.652204 0.738266 11.00000 0.02107 0.02300 = 0.02533 0.00617 0.01636 0.00435 C48 1 0.573950 0.532407 0.726605 11.00000 0.02673 0.02412 = 0.03736 0.00611 0.02189 0.00426 AFIX 43 H48 2 0.554632 0.508597 0.687739 11.00000 -1.20000 AFIX 0 C49 1 0.593053 0.447675 0.771816 11.00000 0.04046 0.02653 = 0.05419 0.02023 0.03466 0.01295 AFIX 43 H49 2 0.586504 0.366296 0.763906 11.00000 -1.20000 AFIX 0 C50 1 0.621306 0.481240 0.827760 11.00000 0.03978 0.04820 = 0.04823 0.02982 0.02754 0.02308 AFIX 43 H50 2 0.634040 0.423059 0.858581 11.00000 -1.20000 AFIX 0 C51 1 0.631297 0.598764 0.839464 11.00000 0.02658 0.05641 = 0.02980 0.01438 0.01058 0.01321 AFIX 43 H51 2 0.651108 0.621537 0.878007 11.00000 -1.20000 AFIX 0 C52 1 0.612259 0.684064 0.794607 11.00000 0.02402 0.03104 = 0.02821 0.00413 0.01320 0.00456 AFIX 43 H52 2 0.619296 0.765057 0.802656 11.00000 -1.20000 AFIX 0 RU1 6 0.582519 0.762223 0.601613 11.00000 0.01634 0.01124 = 0.01589 -0.00110 0.00675 -0.00183 H 2 0.544652 0.725016 0.557794 11.00000 0.04243 PART 2 C13A 1 0.727583 1.018288 0.740658 10.50000 0.05200 PART 0 C1S 1 0.697581 0.785355 0.415829 11.00000 0.07554 0.06452 = 0.07501 0.01164 0.04039 -0.00751 AFIX 137 H1SA 2 0.677827 0.748523 0.422692 11.00000 -1.50000 H1SB 2 0.687565 0.852259 0.387038 11.00000 -1.50000 H1SC 2 0.716943 0.813897 0.455577 11.00000 -1.50000 AFIX 0 C2S 1 0.713482 0.695807 0.388604 11.00000 0.08020 0.09707 = 0.07686 0.02140 0.04666 -0.00047 AFIX 23 H2SA 2 0.695192 0.675174 0.345759 11.00000 -1.20000 H2SB 2 0.735667 0.728547 0.386942 11.00000 -1.20000 AFIX 0 O3S 4 0.723090 0.591734 0.427692 11.00000 0.06071 0.08924 = 0.06778 -0.01853 0.03545 -0.00484 C3S 1 0.738484 0.497994 0.407079 11.00000 0.07677 0.12888 = 0.09564 -0.04132 0.05495 -0.01216 AFIX 23 H3SA 2 0.761708 0.524792 0.407025 11.00000 -1.20000 H3SB 2 0.721068 0.474711 0.364122 11.00000 -1.20000 AFIX 0 C4S 1 0.746098 0.392132 0.450787 11.00000 0.06834 0.09520 = 0.13251 -0.02635 0.05128 0.01250 AFIX 137 H4SA 2 0.762527 0.416627 0.493482 11.00000 -1.50000 H4SB 2 0.757838 0.328672 0.438150 11.00000 -1.50000 H4SC 2 0.722815 0.363156 0.448779 11.00000 -1.50000 AFIX 0 HKLF 4 REM 8augd_a.res in C2/c REM wR2 = 0.1016, GooF = S = 1.029, Restrained GooF = 1.029 for all data REM R1 = 0.0412 for 6554 Fo > 4sig(Fo) and 0.0614 for all 8373 data REM 593 parameters refined using 0 restraints END WGHT 0.0405 31.7946 REM Highest difference peak 0.710, deepest hole -0.542, 1-sigma level 0.089 Q1 1 0.7348 0.9816 0.7191 11.00000 0.05 0.71 Q2 1 0.7042 1.0689 0.7717 11.00000 0.05 0.64 Q3 1 0.7124 1.0570 0.7203 11.00000 0.05 0.62 Q4 1 0.5689 0.7597 0.6406 11.00000 0.05 0.57 Q5 1 0.7288 0.7745 0.4040 11.00000 0.05 0.56 ; _shelx_res_checksum 90916 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' 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 P1 P 0.59810(2) 0.76304(7) 0.51904(4) 0.01670(19) Uani 1 1 d . . . . . O1 O 0.54950(7) 1.00143(19) 0.56118(11) 0.0287(6) Uani 1 1 d . . . . . N1 N 0.54955(7) 0.4870(2) 0.56169(13) 0.0234(7) Uani 1 1 d . . . . . C1 C 0.53101(9) 0.3886(3) 0.53703(16) 0.0264(8) Uani 1 1 d . . . . . H1 H 0.506143 0.395956 0.506280 0.032 Uiso 1 1 calc R . . . . P2 P 0.56104(2) 0.76289(7) 0.67702(4) 0.01646(18) Uani 1 1 d . . . . . N2 N 0.60370(7) 0.5803(2) 0.62854(12) 0.0171(6) Uani 1 1 d . . . . . C2 C 0.54564(10) 0.2741(3) 0.55327(16) 0.0268(8) Uani 1 1 d . . . . . H2 H 0.531094 0.206446 0.533683 0.032 Uiso 1 1 calc R . . . . N3 N 0.63885(7) 0.7842(2) 0.67179(12) 0.0200(6) Uani 1 1 d . . . . . C3 C 0.58094(10) 0.2618(3) 0.59748(16) 0.0277(8) Uani 1 1 d . . . . . H3 H 0.591513 0.185172 0.609458 0.033 Uiso 1 1 calc R . . . . N4 N 0.66041(8) 0.8784(2) 0.70007(13) 0.0262(7) Uani 1 1 d . . . . . C4 C 0.60176(9) 0.3639(3) 0.62545(15) 0.0219(7) Uani 1 1 d . . . . . C5 C 0.58491(9) 0.4759(3) 0.60521(15) 0.0191(7) Uani 1 1 d . . . . . C6 C 0.63868(10) 0.3602(3) 0.67170(16) 0.0279(8) Uani 1 1 d . . . . . H6 H 0.650751 0.286206 0.686124 0.033 Uiso 1 1 calc R . . . . C7 C 0.65675(9) 0.4631(3) 0.69533(16) 0.0271(8) Uani 1 1 d . . . . . H7 H 0.681433 0.461587 0.727248 0.033 Uiso 1 1 calc R . . . . C8 C 0.63889(9) 0.5732(3) 0.67250(15) 0.0208(7) Uani 1 1 d . . . . . C9 C 0.65766(9) 0.6832(3) 0.69600(15) 0.0215(7) Uani 1 1 d . . . . . C10 C 0.69269(10) 0.7115(3) 0.74187(17) 0.0335(9) Uani 1 1 d . . . . . H10 H 0.711881 0.658636 0.766892 0.040 Uiso 1 1 calc R . . . . C11 C 0.69319(10) 0.8341(3) 0.74274(17) 0.0335(9) Uani 1 1 d . . . . . C12 C 0.72288(12) 0.9181(4) 0.7858(2) 0.0549(13) Uani 1 1 d . . . . . C13 C 0.7167(3) 1.0463(10) 0.7622(5) 0.065(3) Uiso 0.5 1 d . . P A 2 C14 C 0.71509(14) 0.9447(6) 0.8409(3) 0.106(3) Uani 1 1 d . . . . . H14A H 0.732545 1.004616 0.867587 0.159 Uiso 1 1 calc GR . . . . H14B H 0.717859 0.871928 0.864945 0.159 Uiso 1 1 calc GR . . . . H14C H 0.689864 0.974775 0.825767 0.159 Uiso 1 1 calc GR . . . . C15 C 0.76024(11) 0.8574(5) 0.8105(2) 0.0654(15) Uani 1 1 d . . . . . H15A H 0.765020 0.833476 0.775625 0.098 Uiso 1 1 calc GR . . . . H15B H 0.760304 0.787035 0.834563 0.098 Uiso 1 1 calc GR . . . . H15C H 0.779497 0.912459 0.837413 0.098 Uiso 1 1 calc GR . . . . C16 C 0.56344(9) 0.9094(3) 0.57802(15) 0.0192(7) Uani 1 1 d . . . . . C17 C 0.63016(9) 0.6470(3) 0.52098(14) 0.0194(7) Uani 1 1 d . . . . . C18 C 0.61857(9) 0.5288(3) 0.51270(15) 0.0222(8) Uani 1 1 d . . . . . H18 H 0.593878 0.510410 0.504030 0.027 Uiso 1 1 calc R . . . . C19 C 0.64241(10) 0.4388(3) 0.51692(15) 0.0269(8) Uani 1 1 d . . . . . H19 H 0.634278 0.358654 0.511715 0.032 Uiso 1 1 calc R . . . . C20 C 0.67827(10) 0.4649(3) 0.52877(17) 0.0330(9) Uani 1 1 d . . . . . H20 H 0.694801 0.402909 0.531564 0.040 Uiso 1 1 calc R . . . . C21 C 0.68991(10) 0.5812(3) 0.53649(18) 0.0361(9) Uani 1 1 d . . . . . H21 H 0.714412 0.599176 0.543876 0.043 Uiso 1 1 calc R . . . . C22 C 0.66632(9) 0.6717(3) 0.53360(16) 0.0273(8) Uani 1 1 d . . . . . H22 H 0.674882 0.751409 0.540276 0.033 Uiso 1 1 calc R . . . . C23 C 0.62033(9) 0.8993(3) 0.51011(15) 0.0198(7) Uani 1 1 d . . . . . C24 C 0.63656(9) 0.9788(3) 0.55924(16) 0.0252(8) Uani 1 1 d . . . . . H24 H 0.636187 0.963789 0.597839 0.030 Uiso 1 1 calc R . . . . C25 C 0.65334(10) 1.0805(3) 0.55127(18) 0.0314(9) Uani 1 1 d . . . . . H25 H 0.664259 1.135302 0.584649 0.038 Uiso 1 1 calc R . . . . C26 C 0.65442(10) 1.1033(3) 0.49593(17) 0.0293(9) Uani 1 1 d . . . . . H26 H 0.666032 1.173086 0.491198 0.035 Uiso 1 1 calc R . . . . C27 C 0.63849(10) 1.0239(3) 0.44721(17) 0.0305(9) Uani 1 1 d . . . . . H27 H 0.639296 1.038632 0.408940 0.037 Uiso 1 1 calc R . . . . C28 C 0.62139(9) 0.9230(3) 0.45430(16) 0.0266(8) Uani 1 1 d . . . . . H28 H 0.610216 0.869178 0.420533 0.032 Uiso 1 1 calc R . . . . C29 C 0.55936(9) 0.7499(3) 0.44092(14) 0.0183(7) Uani 1 1 d . . . . . C30 C 0.55813(9) 0.6691(3) 0.39631(15) 0.0220(8) Uani 1 1 d . . . . . H30 H 0.578228 0.616595 0.405573 0.026 Uiso 1 1 calc R . . . . C31 C 0.52778(10) 0.6649(3) 0.33845(15) 0.0266(8) Uani 1 1 d . . . . . H31 H 0.527007 0.608081 0.308683 0.032 Uiso 1 1 calc R . . . . C32 C 0.49859(9) 0.7422(3) 0.32350(15) 0.0250(8) Uani 1 1 d . . . . . H32 H 0.477940 0.739267 0.283596 0.030 Uiso 1 1 calc R . . . . C33 C 0.49977(9) 0.8237(3) 0.36711(16) 0.0271(8) Uani 1 1 d . . . . . H33 H 0.479900 0.877662 0.357023 0.033 Uiso 1 1 calc R . . . . C34 C 0.52969(9) 0.8277(3) 0.42553(15) 0.0241(8) Uani 1 1 d . . . . . H34 H 0.530047 0.883599 0.455356 0.029 Uiso 1 1 calc R . . . . C35 C 0.56878(9) 0.9010(3) 0.72187(14) 0.0185(7) Uani 1 1 d . . . . . C36 C 0.54999(9) 0.9209(3) 0.75749(15) 0.0232(8) Uani 1 1 d . . . . . H36 H 0.533043 0.863466 0.758194 0.028 Uiso 1 1 calc R . . . . C37 C 0.55607(10) 1.0247(3) 0.79191(15) 0.0262(8) Uani 1 1 d . . . . . H37 H 0.543352 1.038092 0.816265 0.031 Uiso 1 1 calc R . . . . C38 C 0.58056(10) 1.1083(3) 0.79070(15) 0.0266(8) Uani 1 1 d . . . . . H38 H 0.584422 1.179729 0.813822 0.032 Uiso 1 1 calc R . . . . C39 C 0.59944(10) 1.0889(3) 0.75616(15) 0.0255(8) Uani 1 1 d . . . . . H39 H 0.616443 1.146442 0.755803 0.031 Uiso 1 1 calc R . . . . C40 C 0.59364(9) 0.9849(3) 0.72173(15) 0.0218(8) Uani 1 1 d . . . . . H40 H 0.606796 0.971532 0.698090 0.026 Uiso 1 1 calc R . . . . C41 C 0.51115(9) 0.7449(3) 0.64911(15) 0.0190(7) Uani 1 1 d . . . . . C42 C 0.49484(9) 0.6636(3) 0.67196(16) 0.0224(8) Uani 1 1 d . . . . . H42 H 0.509762 0.608951 0.703192 0.027 Uiso 1 1 calc R . . . . C43 C 0.45675(9) 0.6612(3) 0.64965(16) 0.0259(8) Uani 1 1 d . . . . . H43 H 0.445794 0.604364 0.665440 0.031 Uiso 1 1 calc R . . . . C44 C 0.43488(9) 0.7405(3) 0.60486(16) 0.0264(8) Uani 1 1 d . . . . . H44 H 0.408870 0.738626 0.589752 0.032 Uiso 1 1 calc R . . . . C45 C 0.45079(10) 0.8227(3) 0.58193(17) 0.0313(9) Uani 1 1 d . . . . . H45 H 0.435762 0.878592 0.551529 0.038 Uiso 1 1 calc R . . . . C46 C 0.48862(9) 0.8241(3) 0.60312(16) 0.0280(8) Uani 1 1 d . . . . . H46 H 0.499358 0.879490 0.586215 0.034 Uiso 1 1 calc R . . . . C47 C 0.58312(9) 0.6522(3) 0.73827(15) 0.0209(7) Uani 1 1 d . . . . . C48 C 0.57395(10) 0.5324(3) 0.72661(17) 0.0266(8) Uani 1 1 d . . . . . H48 H 0.554632 0.508597 0.687739 0.032 Uiso 1 1 calc R . . . . C49 C 0.59305(11) 0.4477(3) 0.77182(19) 0.0354(10) Uani 1 1 d . . . . . H49 H 0.586504 0.366296 0.763906 0.042 Uiso 1 1 calc R . . . . C50 C 0.62131(11) 0.4812(4) 0.8278(2) 0.0425(11) Uani 1 1 d . . . . . H50 H 0.634040 0.423059 0.858581 0.051 Uiso 1 1 calc R . . . . C51 C 0.63130(10) 0.5988(4) 0.83946(18) 0.0384(10) Uani 1 1 d . . . . . H51 H 0.651108 0.621537 0.878007 0.046 Uiso 1 1 calc R . . . . C52 C 0.61226(9) 0.6841(3) 0.79461(16) 0.0272(8) Uani 1 1 d . . . . . H52 H 0.619296 0.765057 0.802656 0.033 Uiso 1 1 calc R . . . . Ru1 Ru 0.58252(2) 0.76222(2) 0.60161(2) 0.01466(9) Uani 1 1 d . . . . . H H 0.5447(10) 0.725(3) 0.5578(17) 0.042(11) Uiso 1 1 d . . . . . C13A C 0.7276(3) 1.0183(9) 0.7407(5) 0.052(2) Uiso 0.5 1 d . . P A 2 C1S C 0.69758(15) 0.7854(5) 0.4158(3) 0.0692(15) Uani 1 1 d . . . . . H1SA H 0.677827 0.748523 0.422692 0.104 Uiso 1 1 calc GR . . . . H1SB H 0.687565 0.852259 0.387038 0.104 Uiso 1 1 calc GR . . . . H1SC H 0.716943 0.813897 0.455577 0.104 Uiso 1 1 calc GR . . . . C2S C 0.71348(17) 0.6958(6) 0.3886(3) 0.0804(17) Uani 1 1 d . . . . . H2SA H 0.695192 0.675174 0.345759 0.097 Uiso 1 1 calc R . . . . H2SB H 0.735667 0.728547 0.386942 0.097 Uiso 1 1 calc R . . . . O3S O 0.72309(9) 0.5917(3) 0.42769(16) 0.0701(10) Uani 1 1 d . . . . . C3S C 0.73848(18) 0.4980(7) 0.4071(3) 0.094(2) Uani 1 1 d . . . . . H3SA H 0.761708 0.524792 0.407025 0.113 Uiso 1 1 calc R . . . . H3SB H 0.721068 0.474711 0.364122 0.113 Uiso 1 1 calc R . . . . C4S C 0.74610(17) 0.3921(6) 0.4508(3) 0.096(2) Uani 1 1 d . . . . . H4SA H 0.762527 0.416627 0.493482 0.145 Uiso 1 1 calc GR . . . . H4SB H 0.757838 0.328672 0.438150 0.145 Uiso 1 1 calc GR . . . . H4SC H 0.722815 0.363156 0.448779 0.145 Uiso 1 1 calc GR . . . . 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 P1 0.0181(4) 0.0144(4) 0.0171(4) -0.0002(3) 0.0074(4) -0.0002(3) O1 0.0421(16) 0.0136(13) 0.0335(15) 0.0010(10) 0.0196(13) 0.0033(11) N1 0.0218(16) 0.0142(14) 0.0285(17) 0.0001(12) 0.0062(14) -0.0018(12) C1 0.0198(18) 0.0199(18) 0.032(2) -0.0020(15) 0.0048(16) -0.0025(15) P2 0.0175(4) 0.0137(4) 0.0186(4) 0.0004(3) 0.0084(4) -0.0007(3) N2 0.0151(14) 0.0169(14) 0.0163(14) 0.0002(11) 0.0044(12) -0.0002(11) C2 0.031(2) 0.0153(17) 0.032(2) -0.0023(15) 0.0130(17) -0.0059(15) N3 0.0174(14) 0.0196(15) 0.0227(15) -0.0040(12) 0.0087(12) -0.0069(12) C3 0.036(2) 0.0146(16) 0.034(2) 0.0029(15) 0.0165(17) 0.0037(16) N4 0.0241(16) 0.0257(16) 0.0279(17) -0.0070(13) 0.0109(14) -0.0113(13) C4 0.0240(19) 0.0206(18) 0.0225(19) 0.0013(14) 0.0118(16) 0.0024(15) C5 0.0244(18) 0.0163(16) 0.0187(18) 0.0013(14) 0.0116(15) 0.0008(15) C6 0.030(2) 0.0212(19) 0.031(2) 0.0064(15) 0.0129(18) 0.0076(16) C7 0.0181(18) 0.031(2) 0.026(2) 0.0040(16) 0.0040(16) 0.0034(16) C8 0.0200(18) 0.0223(18) 0.0214(19) -0.0008(14) 0.0105(16) 0.0012(14) C9 0.0163(17) 0.0261(19) 0.0221(19) 0.0000(14) 0.0085(15) -0.0015(15) C10 0.0194(19) 0.037(2) 0.034(2) 0.0025(17) 0.0029(17) -0.0034(16) C11 0.026(2) 0.037(2) 0.032(2) -0.0046(17) 0.0075(18) -0.0126(17) C12 0.033(2) 0.047(3) 0.060(3) -0.010(2) -0.001(2) -0.017(2) C14 0.037(3) 0.132(6) 0.124(5) -0.105(5) 0.014(3) -0.016(3) C15 0.025(2) 0.101(4) 0.061(3) -0.037(3) 0.011(2) -0.024(3) C16 0.0212(18) 0.0161(18) 0.0217(18) -0.0061(14) 0.0109(15) -0.0060(15) C17 0.0205(18) 0.0235(18) 0.0120(17) 0.0013(13) 0.0053(14) 0.0027(14) C18 0.0219(18) 0.0234(18) 0.0184(18) -0.0010(14) 0.0065(15) 0.0006(15) C19 0.035(2) 0.0194(18) 0.0224(19) -0.0010(14) 0.0093(17) 0.0052(16) C20 0.031(2) 0.033(2) 0.030(2) 0.0045(17) 0.0097(18) 0.0166(18) C21 0.023(2) 0.041(2) 0.040(2) 0.0081(18) 0.0103(18) 0.0079(18) C22 0.0243(19) 0.0266(19) 0.027(2) 0.0025(15) 0.0075(16) 0.0009(16) C23 0.0165(17) 0.0158(17) 0.028(2) 0.0023(14) 0.0107(15) 0.0008(14) C24 0.028(2) 0.0227(18) 0.029(2) -0.0017(15) 0.0166(17) -0.0061(16) C25 0.035(2) 0.0241(19) 0.037(2) -0.0069(16) 0.0182(19) -0.0089(17) C26 0.027(2) 0.0217(19) 0.043(2) 0.0081(16) 0.0200(19) -0.0019(15) C27 0.031(2) 0.035(2) 0.030(2) 0.0112(17) 0.0171(18) 0.0016(17) C28 0.028(2) 0.0266(19) 0.025(2) 0.0014(15) 0.0118(17) -0.0024(16) C29 0.0190(16) 0.0173(17) 0.0176(17) 0.0030(13) 0.0073(14) -0.0003(14) C30 0.0257(19) 0.0193(17) 0.0187(18) -0.0001(14) 0.0079(16) 0.0028(15) C31 0.038(2) 0.0203(18) 0.0186(19) -0.0025(14) 0.0098(17) -0.0003(16) C32 0.0257(18) 0.0271(19) 0.0177(18) 0.0038(15) 0.0058(15) -0.0006(16) C33 0.0240(19) 0.029(2) 0.025(2) 0.0077(16) 0.0084(16) 0.0066(16) C34 0.0271(19) 0.0235(18) 0.0210(19) -0.0025(14) 0.0101(16) 0.0018(15) C35 0.0204(18) 0.0169(16) 0.0147(17) 0.0015(13) 0.0048(14) 0.0028(14) C36 0.0280(19) 0.0208(18) 0.0222(19) 0.0036(14) 0.0125(16) 0.0024(15) C37 0.037(2) 0.0241(19) 0.0187(19) 0.0015(14) 0.0135(17) 0.0093(17) C38 0.039(2) 0.0198(18) 0.0151(18) -0.0023(14) 0.0068(17) 0.0031(16) C39 0.030(2) 0.0204(18) 0.0227(19) -0.0025(14) 0.0095(16) -0.0051(15) C40 0.0230(19) 0.0212(18) 0.0207(19) -0.0021(14) 0.0093(15) -0.0016(15) C41 0.0186(16) 0.0186(17) 0.0207(17) -0.0032(14) 0.0096(14) -0.0011(14) C42 0.0222(19) 0.0197(18) 0.026(2) 0.0012(14) 0.0117(16) 0.0014(14) C43 0.027(2) 0.0212(18) 0.034(2) -0.0035(15) 0.0173(17) -0.0049(15) C44 0.0185(17) 0.033(2) 0.0259(19) -0.0062(16) 0.0087(15) -0.0016(16) C45 0.025(2) 0.037(2) 0.030(2) 0.0077(17) 0.0109(17) 0.0068(17) C46 0.025(2) 0.031(2) 0.030(2) 0.0074(16) 0.0138(17) 0.0016(16) C47 0.0211(18) 0.0230(18) 0.0253(19) 0.0062(14) 0.0164(16) 0.0043(14) C48 0.027(2) 0.0241(19) 0.037(2) 0.0061(16) 0.0219(18) 0.0043(16) C49 0.040(2) 0.027(2) 0.054(3) 0.0202(19) 0.035(2) 0.0129(18) C50 0.040(2) 0.048(3) 0.048(3) 0.030(2) 0.028(2) 0.023(2) C51 0.027(2) 0.056(3) 0.030(2) 0.0144(19) 0.0106(18) 0.0132(19) C52 0.0240(19) 0.031(2) 0.028(2) 0.0041(16) 0.0132(17) 0.0046(16) Ru1 0.01634(14) 0.01124(14) 0.01589(14) -0.00110(11) 0.00675(11) -0.00183(11) C1S 0.076(4) 0.065(3) 0.075(4) 0.012(3) 0.040(3) -0.008(3) C2S 0.080(4) 0.097(5) 0.077(4) 0.021(4) 0.047(4) 0.000(4) O3S 0.061(2) 0.089(3) 0.068(2) -0.019(2) 0.035(2) -0.005(2) C3S 0.077(4) 0.129(6) 0.096(5) -0.041(5) 0.055(4) -0.012(4) C4S 0.068(4) 0.095(5) 0.133(6) -0.026(5) 0.051(4) 0.012(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C17 P1 C23 102.66(15) . . ? C17 P1 C29 103.94(14) . . ? C17 P1 Ru1 115.80(10) . . ? C23 P1 Ru1 115.81(11) . . ? C29 P1 C23 100.79(14) . . ? C29 P1 Ru1 115.77(11) . . ? C1 N1 C5 117.6(3) . . ? N1 C1 H1 117.9 . . ? N1 C1 C2 124.3(3) . . ? C2 C1 H1 117.9 . . ? C35 P2 Ru1 115.63(11) . . ? C41 P2 C35 100.26(14) . . ? C41 P2 Ru1 116.72(11) . . ? C47 P2 C35 102.25(15) . . ? C47 P2 C41 106.31(15) . . ? C47 P2 Ru1 113.83(11) . . ? C5 N2 Ru1 127.1(2) . . ? C8 N2 C5 117.9(3) . . ? C8 N2 Ru1 115.0(2) . . ? C1 C2 H2 120.7 . . ? C3 C2 C1 118.7(3) . . ? C3 C2 H2 120.7 . . ? N4 N3 C9 109.5(3) . . ? N4 N3 Ru1 134.7(2) . . ? C9 N3 Ru1 115.8(2) . . ? C2 C3 H3 120.4 . . ? C2 C3 C4 119.2(3) . . ? C4 C3 H3 120.4 . . ? N3 N4 C11 106.6(3) . . ? C3 C4 C5 118.1(3) . . ? C3 C4 C6 123.4(3) . . ? C6 C4 C5 118.4(3) . . ? N1 C5 N2 116.0(3) . . ? N1 C5 C4 122.1(3) . . ? N2 C5 C4 121.9(3) . . ? C4 C6 H6 120.3 . . ? C7 C6 C4 119.3(3) . . ? C7 C6 H6 120.3 . . ? C6 C7 H7 120.0 . . ? C6 C7 C8 120.1(3) . . ? C8 C7 H7 120.0 . . ? N2 C8 C7 122.3(3) . . ? N2 C8 C9 116.6(3) . . ? C7 C8 C9 121.0(3) . . ? N3 C9 C8 117.6(3) . . ? N3 C9 C10 109.1(3) . . ? C10 C9 C8 133.3(3) . . ? C9 C10 H10 127.9 . . ? C11 C10 C9 104.1(3) . . ? C11 C10 H10 127.9 . . ? N4 C11 C10 110.7(3) . . ? N4 C11 C12 119.6(3) . . ? C10 C11 C12 129.5(4) . . ? C11 C12 C13 112.9(5) . . ? C11 C12 C14 107.8(4) . . ? C11 C12 C15 109.5(4) . . ? C11 C12 C13A 105.8(5) . . ? C13 C12 C13A 31.9(5) . . ? C14 C12 C13 94.2(6) . . ? C14 C12 C13A 124.9(6) . . ? C15 C12 C13 122.6(6) . . ? C15 C12 C14 107.9(4) . . ? C15 C12 C13A 100.3(5) . . ? C13A C13 C12 80.6(11) . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14B 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15B 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O1 C16 Ru1 176.6(3) . . ? C18 C17 P1 119.2(2) . . ? C22 C17 P1 122.1(3) . . ? C22 C17 C18 118.6(3) . . ? C17 C18 H18 119.6 . . ? C19 C18 C17 120.8(3) . . ? C19 C18 H18 119.6 . . ? C18 C19 H19 120.0 . . ? C18 C19 C20 119.9(3) . . ? C20 C19 H19 120.0 . . ? C19 C20 H20 120.1 . . ? C21 C20 C19 119.8(3) . . ? C21 C20 H20 120.1 . . ? C20 C21 H21 119.7 . . ? C20 C21 C22 120.6(4) . . ? C22 C21 H21 119.7 . . ? C17 C22 H22 119.9 . . ? C21 C22 C17 120.3(3) . . ? C21 C22 H22 119.9 . . ? C24 C23 P1 120.6(3) . . ? C28 C23 P1 120.2(3) . . ? C28 C23 C24 119.3(3) . . ? C23 C24 H24 120.4 . . ? C25 C24 C23 119.3(3) . . ? C25 C24 H24 120.4 . . ? C24 C25 H25 119.4 . . ? C26 C25 C24 121.2(3) . . ? C26 C25 H25 119.4 . . ? C25 C26 H26 120.2 . . ? C25 C26 C27 119.6(3) . . ? C27 C26 H26 120.2 . . ? C26 C27 H27 120.1 . . ? C28 C27 C26 119.9(3) . . ? C28 C27 H27 120.1 . . ? C23 C28 H28 119.6 . . ? C27 C28 C23 120.8(3) . . ? C27 C28 H28 119.6 . . ? C30 C29 P1 124.1(2) . . ? C30 C29 C34 118.5(3) . . ? C34 C29 P1 117.4(2) . . ? C29 C30 H30 119.8 . . ? C31 C30 C29 120.4(3) . . ? C31 C30 H30 119.8 . . ? C30 C31 H31 119.6 . . ? C32 C31 C30 120.8(3) . . ? C32 C31 H31 119.6 . . ? C31 C32 H32 120.4 . . ? C33 C32 C31 119.3(3) . . ? C33 C32 H32 120.4 . . ? C32 C33 H33 119.7 . . ? C32 C33 C34 120.5(3) . . ? C34 C33 H33 119.7 . . ? C29 C34 H34 119.8 . . ? C33 C34 C29 120.5(3) . . ? C33 C34 H34 119.8 . . ? C36 C35 P2 119.9(2) . . ? C40 C35 P2 120.7(2) . . ? C40 C35 C36 119.4(3) . . ? C35 C36 H36 120.0 . . ? C37 C36 C35 120.0(3) . . ? C37 C36 H36 120.0 . . ? C36 C37 H37 120.0 . . ? C38 C37 C36 120.0(3) . . ? C38 C37 H37 120.0 . . ? C37 C38 H38 119.8 . . ? C39 C38 C37 120.3(3) . . ? C39 C38 H38 119.8 . . ? C38 C39 H39 119.9 . . ? C38 C39 C40 120.1(3) . . ? C40 C39 H39 119.9 . . ? C35 C40 C39 120.2(3) . . ? C35 C40 H40 119.9 . . ? C39 C40 H40 119.9 . . ? C42 C41 P2 125.1(3) . . ? C42 C41 C46 118.6(3) . . ? C46 C41 P2 116.2(2) . . ? C41 C42 H42 119.7 . . ? C41 C42 C43 120.6(3) . . ? C43 C42 H42 119.7 . . ? C42 C43 H43 119.9 . . ? C44 C43 C42 120.3(3) . . ? C44 C43 H43 119.9 . . ? C43 C44 H44 120.1 . . ? C43 C44 C45 119.8(3) . . ? C45 C44 H44 120.1 . . ? C44 C45 H45 119.9 . . ? C44 C45 C46 120.1(3) . . ? C46 C45 H45 119.9 . . ? C41 C46 H46 119.7 . . ? C45 C46 C41 120.6(3) . . ? C45 C46 H46 119.7 . . ? C48 C47 P2 120.5(3) . . ? C52 C47 P2 120.3(3) . . ? C52 C47 C48 118.7(3) . . ? C47 C48 H48 119.9 . . ? C49 C48 C47 120.1(4) . . ? C49 C48 H48 119.9 . . ? C48 C49 H49 119.9 . . ? C50 C49 C48 120.3(4) . . ? C50 C49 H49 119.9 . . ? C49 C50 H50 119.8 . . ? C49 C50 C51 120.4(4) . . ? C51 C50 H50 119.8 . . ? C50 C51 H51 120.1 . . ? C50 C51 C52 119.7(4) . . ? C52 C51 H51 120.1 . . ? C47 C52 C51 120.8(4) . . ? C47 C52 H52 119.6 . . ? C51 C52 H52 119.6 . . ? P1 Ru1 H 89.2(14) . . ? P2 Ru1 P1 174.50(3) . . ? P2 Ru1 H 85.6(14) . . ? N2 Ru1 P1 91.99(7) . . ? N2 Ru1 P2 90.40(7) . . ? N2 Ru1 H 95.1(14) . . ? N3 Ru1 P1 93.92(7) . . ? N3 Ru1 P2 91.47(7) . . ? N3 Ru1 N2 75.00(10) . . ? N3 Ru1 H 169.7(14) . . ? C16 Ru1 P1 88.32(10) . . ? C16 Ru1 P2 89.11(10) . . ? C16 Ru1 N2 177.91(12) . . ? C16 Ru1 N3 107.05(12) . . ? C16 Ru1 H 82.8(14) . . ? C13 C13A C12 67.5(10) . . ? H1SA C1S H1SB 109.5 . . ? H1SA C1S H1SC 109.5 . . ? H1SB C1S H1SC 109.5 . . ? C2S C1S H1SA 109.5 . . ? C2S C1S H1SB 109.5 . . ? C2S C1S H1SC 109.5 . . ? C1S C2S H2SA 110.1 . . ? C1S C2S H2SB 110.1 . . ? H2SA C2S H2SB 108.4 . . ? O3S C2S C1S 107.9(4) . . ? O3S C2S H2SA 110.1 . . ? O3S C2S H2SB 110.1 . . ? C3S O3S C2S 114.1(5) . . ? O3S C3S H3SA 109.9 . . ? O3S C3S H3SB 109.9 . . ? O3S C3S C4S 109.0(5) . . ? H3SA C3S H3SB 108.3 . . ? C4S C3S H3SA 109.9 . . ? C4S C3S H3SB 109.9 . . ? C3S C4S H4SA 109.5 . . ? C3S C4S H4SB 109.5 . . ? C3S C4S H4SC 109.5 . . ? H4SA C4S H4SB 109.5 . . ? H4SA C4S H4SC 109.5 . . ? H4SB C4S H4SC 109.5 . . ? 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 P1 C17 1.830(3) . ? P1 C23 1.842(3) . ? P1 C29 1.836(3) . ? P1 Ru1 2.3376(9) . ? O1 C16 1.163(4) . ? N1 C1 1.322(4) . ? N1 C5 1.350(4) . ? C1 H1 0.9500 . ? C1 C2 1.400(5) . ? P2 C35 1.839(3) . ? P2 C41 1.836(3) . ? P2 C47 1.828(3) . ? P2 Ru1 2.3370(9) . ? N2 C5 1.376(4) . ? N2 C8 1.345(4) . ? N2 Ru1 2.205(3) . ? C2 H2 0.9500 . ? C2 C3 1.355(5) . ? N3 N4 1.349(4) . ? N3 C9 1.349(4) . ? N3 Ru1 2.162(3) . ? C3 H3 0.9500 . ? C3 C4 1.407(5) . ? N4 C11 1.359(5) . ? C4 C5 1.414(4) . ? C4 C6 1.410(5) . ? C6 H6 0.9500 . ? C6 C7 1.354(5) . ? C7 H7 0.9500 . ? C7 C8 1.417(5) . ? C8 C9 1.431(5) . ? C9 C10 1.390(5) . ? C10 H10 0.9500 . ? C10 C11 1.382(5) . ? C11 C12 1.516(5) . ? C12 C13 1.532(12) . ? C12 C14 1.525(7) . ? C12 C15 1.520(6) . ? C12 C13A 1.635(11) . ? C13 C13A 0.876(12) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 Ru1 1.811(3) . ? C17 C18 1.397(5) . ? C17 C22 1.387(5) . ? C18 H18 0.9500 . ? C18 C19 1.374(5) . ? C19 H19 0.9500 . ? C19 C20 1.383(5) . ? C20 H20 0.9500 . ? C20 C21 1.377(5) . ? C21 H21 0.9500 . ? C21 C22 1.380(5) . ? C22 H22 0.9500 . ? C23 C24 1.391(5) . ? C23 C28 1.387(5) . ? C24 H24 0.9500 . ? C24 C25 1.389(5) . ? C25 H25 0.9500 . ? C25 C26 1.374(5) . ? C26 H26 0.9500 . ? C26 C27 1.382(5) . ? C27 H27 0.9500 . ? C27 C28 1.381(5) . ? C28 H28 0.9500 . ? C29 C30 1.390(4) . ? C29 C34 1.398(4) . ? C30 H30 0.9500 . ? C30 C31 1.385(5) . ? C31 H31 0.9500 . ? C31 C32 1.382(5) . ? C32 H32 0.9500 . ? C32 C33 1.379(5) . ? C33 H33 0.9500 . ? C33 C34 1.385(5) . ? C34 H34 0.9500 . ? C35 C36 1.397(5) . ? C35 C40 1.384(5) . ? C36 H36 0.9500 . ? C36 C37 1.390(5) . ? C37 H37 0.9500 . ? C37 C38 1.379(5) . ? C38 H38 0.9500 . ? C38 C39 1.376(5) . ? C39 H39 0.9500 . ? C39 C40 1.392(4) . ? C40 H40 0.9500 . ? C41 C42 1.380(4) . ? C41 C46 1.396(5) . ? C42 H42 0.9500 . ? C42 C43 1.390(5) . ? C43 H43 0.9500 . ? C43 C44 1.374(5) . ? C44 H44 0.9500 . ? C44 C45 1.378(5) . ? C45 H45 0.9500 . ? C45 C46 1.384(5) . ? C46 H46 0.9500 . ? C47 C48 1.395(5) . ? C47 C52 1.387(5) . ? C48 H48 0.9500 . ? C48 C49 1.392(5) . ? C49 H49 0.9500 . ? C49 C50 1.372(6) . ? C50 H50 0.9500 . ? C50 C51 1.377(6) . ? C51 H51 0.9500 . ? C51 C52 1.392(5) . ? C52 H52 0.9500 . ? Ru1 H 1.48(4) . ? C1S H1SA 0.9800 . ? C1S H1SB 0.9800 . ? C1S H1SC 0.9800 . ? C1S C2S 1.497(8) . ? C2S H2SA 0.9900 . ? C2S H2SB 0.9900 . ? C2S O3S 1.443(6) . ? O3S C3S 1.424(7) . ? C3S H3SA 0.9900 . ? C3S H3SB 0.9900 . ? C3S C4S 1.527(9) . ? C4S H4SA 0.9800 . ? C4S H4SB 0.9800 . ? C4S H4SC 0.9800 . ?