#------------------------------------------------------------------------------ #$Date: 2020-10-06 11:55:54 +0300 (Tue, 06 Oct 2020) $ #$Revision: 257548 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/53/7705308.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_7705308 loop_ _publ_author_name 'Gallardo-Villagr\'an, Manuel' 'Rivada-Wheelaghan, Orestes' 'Rahaman, S. M. Wahidur' 'Fayzullin, Robert R.' 'Khusnutdinova, Julia R.' _publ_section_title ; Proton-responsive naphthyridinone-based RuII complexes and their reactivity with water and alcohols. ; _journal_issue 36 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 12756 _journal_page_last 12766 _journal_paper_doi 10.1039/d0dt02505d _journal_volume 49 _journal_year 2020 _chemical_formula_moiety 'C32 H48 N4 O4 P2 Ru, 4.732(C H4 O)' _chemical_formula_sum 'C36.73 H66.93 N4 O8.73 P2 Ru' _chemical_formula_weight 867.39 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2020-06-14 deposited with the CCDC. 2020-08-25 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 94.7465(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 11.71671(13) _cell_length_b 13.94222(15) _cell_length_c 25.5940(3) _cell_measurement_reflns_used 81696 _cell_measurement_temperature 99(2) _cell_measurement_theta_max 33.5740 _cell_measurement_theta_min 2.8080 _cell_volume 4166.62(8) _computing_cell_refinement 'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)' _computing_molecular_graphics ; WinGX (Farrugia, 2012); Olex2 (Dolomanov et al., 2009); ORTEP-3 (Farrugia, 2012); PLATON (Spek, 2009); enCIFer (Allen, 2004) ; _computing_publication_material ; WinGX (Farrugia, 2012); PLATON (Spek, 2009); ORTEP-3 (Farrugia, 2012); Olex2 (Dolomanov et al., 2009); enCIFer (Allen, 2004) ; _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT-2018/2 (Sheldrick, 2015)' _diffrn_ambient_temperature 99(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'XtaLAB Pro: Kappa dual offset/far' _diffrn_measurement_method '\w scans' _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0567 _diffrn_reflns_av_unetI/netI 0.0208 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_number 223268 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 32.150 _diffrn_reflns_theta_min 2.275 _diffrn_source 'microfocus sealed X-ray tube' _exptl_absorpt_coefficient_mu 0.508 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.713 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.20a (Rigaku Oxford Diffraction, 2015). Numerical absorption correction based on gaussian integration over a multifaceted crystal model. Empirical absorption correction using spherical harmonics, frame scaling and detector area scaling, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.383 _exptl_crystal_description prism _exptl_crystal_F_000 1837 _exptl_crystal_recrystallization_method 'from a concentrated methanol solution at -20 \%C' _exptl_crystal_size_max 0.146 _exptl_crystal_size_mid 0.079 _exptl_crystal_size_min 0.062 _refine_diff_density_max 1.080 _refine_diff_density_min -0.940 _refine_diff_density_rms 0.078 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 561 _refine_ls_number_reflns 14635 _refine_ls_number_restraints 105 _refine_ls_restrained_S_all 1.100 _refine_ls_R_factor_all 0.0368 _refine_ls_R_factor_gt 0.0322 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0350P)^2^+3.1779P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0785 _refine_ls_wR_factor_ref 0.0803 _reflns_Friedel_coverage 0.000 _reflns_number_gt 13266 _reflns_number_total 14635 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0dt02505d2.cif _cod_data_source_block jk440 _cod_depositor_comments 'Adding full bibliography for 7705307--7705310.cif.' _cod_original_cell_volume 4166.61(8) _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 7705308 _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_min 0.930 _shelx_estimated_absorpt_t_max 0.969 _shelx_res_file ; TITL jk440 in P2(1)/n shelx.res created by SHELXL-2018/3 at 18:03:05 on 10-Apr-2020 CELL 0.71073 11.716712 13.942223 25.593950 90.0000 94.7465 90.0000 ZERR 4.00 0.000125 0.000152 0.000275 0.0000 0.0010 0.0000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H N O P RU UNIT 146.93 267.71 16 34.93 8 4 MERG 2 OMIT -2.00 64.30 SADI O3 H3 O4 H4 O5 H5 O6 H6 O7 H7 O81 H81 O91 H91 SIMU 0.01 O81 > C92 RIGU O81 > C92 MORE -1 HTAB O3 N12 HTAB O4 N22 HTAB O5 O6 HTAB O6 O1 HTAB O7 O2 HTAB O81 O2 HTAB O82 O2 HTAB O91 O7 EQIV $1 -x+3/2, y-1/2, -z+3/2 HTAB O92 O2_$1 FMAP 2 PLAN 32 SIZE 0.062 0.079 0.146 ACTA BOND $H CONF LIST 4 L.S. 20 TEMP -174.15 WGHT 0.035000 3.177900 FVAR 0.26577 0.73158 0.73651 0.68121 RU1 6 0.198697 0.288349 0.630665 11.00000 0.01105 0.01141 = 0.01236 -0.00149 -0.00147 -0.00064 P1 5 0.172855 0.132758 0.607156 11.00000 0.01184 0.01171 = 0.01466 -0.00085 -0.00144 -0.00071 P2 5 0.010944 0.325552 0.625579 11.00000 0.01244 0.01291 = 0.01371 0.00040 -0.00041 0.00061 O1 4 0.347211 0.615185 0.571243 11.00000 0.03447 0.01463 = 0.02335 -0.00086 -0.00126 -0.00660 O2 4 0.554920 0.289323 0.763540 11.00000 0.02522 0.03621 = 0.04387 -0.00109 -0.01572 -0.00134 O3 4 0.237076 0.437784 0.649765 11.00000 0.02013 0.01431 = 0.01549 -0.00280 -0.00182 -0.00333 H3 2 0.258108 0.452373 0.618866 11.00000 0.04861 C3 1 0.309253 0.477356 0.691629 11.00000 0.03033 0.01896 = 0.02544 -0.00696 -0.01023 -0.00026 AFIX 137 H3A 2 0.321583 0.545643 0.684971 11.00000 -1.50000 H3B 2 0.383024 0.443839 0.694262 11.00000 -1.50000 H3C 2 0.272948 0.469890 0.724535 11.00000 -1.50000 AFIX 0 O4 4 0.384930 0.265891 0.642487 11.00000 0.01245 0.02062 = 0.02338 -0.00247 -0.00121 -0.00221 H4 2 0.386864 0.272868 0.677585 11.00000 0.05272 C4 1 0.472571 0.317676 0.619547 11.00000 0.01433 0.02255 = 0.03933 0.00107 0.00151 -0.00279 AFIX 137 H4A 2 0.477056 0.296256 0.583306 11.00000 -1.50000 H4B 2 0.546126 0.306099 0.639662 11.00000 -1.50000 H4C 2 0.454959 0.386378 0.619858 11.00000 -1.50000 AFIX 0 N11 3 0.223299 0.304169 0.547691 11.00000 0.01267 0.01227 = 0.01487 -0.00112 -0.00040 -0.00065 N12 3 0.288382 0.461954 0.557703 11.00000 0.01722 0.01265 = 0.01775 -0.00102 0.00034 -0.00235 N21 3 0.171091 0.269103 0.712877 11.00000 0.01940 0.01320 = 0.01321 -0.00051 -0.00257 0.00142 N22 3 0.366098 0.271847 0.739741 11.00000 0.02144 0.01727 = 0.02195 -0.00248 -0.00875 0.00140 C11 1 0.142826 0.141731 0.535801 11.00000 0.01590 0.01317 = 0.01558 -0.00214 -0.00022 -0.00199 AFIX 23 H11A 2 0.172331 0.083874 0.518983 11.00000 -1.20000 H11B 2 0.058981 0.144477 0.527077 11.00000 -1.20000 AFIX 0 C12 1 0.197467 0.229404 0.514655 11.00000 0.01333 0.01375 = 0.01559 -0.00172 0.00007 -0.00022 C13 1 0.214876 0.231016 0.461161 11.00000 0.01991 0.01633 = 0.01572 -0.00281 0.00028 -0.00014 AFIX 43 H13 2 0.194016 0.177160 0.439720 11.00000 -1.20000 AFIX 0 C14 1 0.262241 0.310725 0.439699 11.00000 0.02098 0.01928 = 0.01519 -0.00067 0.00211 0.00099 AFIX 43 H14 2 0.274883 0.312566 0.403525 11.00000 -1.20000 AFIX 0 C15 1 0.291307 0.388863 0.472315 11.00000 0.01518 0.01554 = 0.01643 0.00123 0.00124 0.00135 C16 1 0.344805 0.473683 0.454270 11.00000 0.01966 0.01837 = 0.01952 0.00382 0.00287 0.00102 AFIX 43 H16 2 0.364062 0.477553 0.418998 11.00000 -1.20000 AFIX 0 C17 1 0.368012 0.548278 0.487239 11.00000 0.01811 0.01622 = 0.02225 0.00415 0.00075 -0.00134 AFIX 43 H17 2 0.406216 0.603335 0.475478 11.00000 -1.20000 AFIX 0 C18 1 0.334617 0.544324 0.540579 11.00000 0.01738 0.01464 = 0.02054 0.00213 -0.00259 -0.00103 C19 1 0.267987 0.385539 0.525833 11.00000 0.01192 0.01346 = 0.01591 -0.00027 -0.00041 0.00068 C21 1 -0.034955 0.267826 0.684720 11.00000 0.01747 0.01885 = 0.01686 0.00227 0.00162 0.00037 AFIX 23 H21A 2 -0.099002 0.304663 0.697779 11.00000 -1.20000 H21B 2 -0.062835 0.202257 0.676009 11.00000 -1.20000 AFIX 0 C22 1 0.061947 0.262655 0.726706 11.00000 0.02222 0.01624 = 0.01545 0.00085 0.00146 0.00229 C23 1 0.034303 0.247489 0.778268 11.00000 0.03131 0.02784 = 0.01862 0.00386 0.00505 0.00324 AFIX 43 H23 2 -0.043588 0.242403 0.785675 11.00000 -1.20000 AFIX 0 C24 1 0.119718 0.239985 0.818057 11.00000 0.04293 0.02793 = 0.01475 0.00354 0.00167 0.00343 AFIX 43 H24 2 0.102007 0.228961 0.853113 11.00000 -1.20000 AFIX 0 C25 1 0.233047 0.248875 0.805971 11.00000 0.03730 0.01567 = 0.01633 0.00102 -0.00698 0.00232 C26 1 0.328362 0.242365 0.844865 11.00000 0.04877 0.01987 = 0.01946 0.00197 -0.01421 0.00067 AFIX 43 H26 2 0.315513 0.229980 0.880404 11.00000 -1.20000 AFIX 0 C27 1 0.435363 0.253734 0.831092 11.00000 0.04459 0.01718 = 0.02829 0.00133 -0.02185 -0.00060 AFIX 43 H27 2 0.498218 0.249771 0.856942 11.00000 -1.20000 AFIX 0 C28 1 0.455536 0.272043 0.776941 11.00000 0.02919 0.01541 = 0.03144 -0.00181 -0.01467 0.00034 C29 1 0.257608 0.262907 0.753190 11.00000 0.02560 0.01125 = 0.01690 -0.00184 -0.00671 0.00244 C31 1 0.052797 0.054182 0.624474 11.00000 0.01502 0.01373 = 0.01782 0.00080 -0.00060 -0.00191 AFIX 13 H31 2 -0.017760 0.094816 0.621118 11.00000 -1.20000 AFIX 0 C32 1 0.066391 0.019296 0.681532 11.00000 0.02516 0.01856 = 0.01796 0.00208 0.00033 -0.00302 AFIX 137 H32A 2 0.124592 -0.031286 0.685101 11.00000 -1.50000 H32B 2 -0.006863 -0.006123 0.691307 11.00000 -1.50000 H32C 2 0.090125 0.073025 0.704618 11.00000 -1.50000 AFIX 0 C33 1 0.029580 -0.030883 0.586913 11.00000 0.02122 0.01630 = 0.02154 -0.00138 -0.00138 -0.00606 AFIX 137 H33A 2 0.008276 -0.006827 0.551466 11.00000 -1.50000 H33B 2 -0.033117 -0.069761 0.598660 11.00000 -1.50000 H33C 2 0.098776 -0.070311 0.586660 11.00000 -1.50000 AFIX 0 C41 1 0.297670 0.049295 0.615942 11.00000 0.01501 0.01501 = 0.02614 -0.00204 -0.00286 0.00166 AFIX 13 H41 2 0.267787 -0.016551 0.607453 11.00000 -1.20000 AFIX 0 C42 1 0.352496 0.046069 0.672861 11.00000 0.02056 0.02520 = 0.03143 0.00386 -0.00750 0.00254 AFIX 137 H42A 2 0.396746 0.104822 0.680389 11.00000 -1.50000 H42B 2 0.403353 -0.009661 0.677267 11.00000 -1.50000 H42C 2 0.292200 0.040999 0.697068 11.00000 -1.50000 AFIX 0 C43 1 0.388943 0.070461 0.577964 11.00000 0.01588 0.02607 = 0.03303 -0.00840 0.00197 0.00179 AFIX 137 H43A 2 0.355615 0.062746 0.541812 11.00000 -1.50000 H43B 2 0.453074 0.025775 0.584583 11.00000 -1.50000 H43C 2 0.416519 0.136400 0.583207 11.00000 -1.50000 AFIX 0 C51 1 -0.034189 0.452800 0.633102 11.00000 0.01646 0.01474 = 0.02371 -0.00117 0.00064 0.00189 AFIX 13 H51 2 -0.119569 0.453237 0.626823 11.00000 -1.20000 AFIX 0 C52 1 0.010330 0.521238 0.592146 11.00000 0.02854 0.01493 = 0.02604 0.00268 -0.00187 0.00090 AFIX 137 H52A 2 0.091304 0.535527 0.601604 11.00000 -1.50000 H52B 2 -0.033979 0.580917 0.591251 11.00000 -1.50000 H52C 2 0.001995 0.490819 0.557521 11.00000 -1.50000 AFIX 0 C53 1 -0.006642 0.492494 0.688664 11.00000 0.02920 0.01947 = 0.02643 -0.00659 0.00579 0.00088 AFIX 137 H53A 2 -0.040845 0.450891 0.713997 11.00000 -1.50000 H53B 2 -0.038072 0.557382 0.690802 11.00000 -1.50000 H53C 2 0.076576 0.494547 0.696664 11.00000 -1.50000 AFIX 0 C61 1 -0.096382 0.279150 0.574279 11.00000 0.01249 0.01539 = 0.01777 0.00065 -0.00203 0.00044 AFIX 13 H61 2 -0.078447 0.209612 0.569986 11.00000 -1.20000 AFIX 0 C62 1 -0.087925 0.325481 0.520302 11.00000 0.01822 0.02509 = 0.01766 0.00250 -0.00256 -0.00059 AFIX 137 H62A 2 -0.119406 0.390591 0.520471 11.00000 -1.50000 H62B 2 -0.131502 0.287186 0.493437 11.00000 -1.50000 H62C 2 -0.007470 0.328233 0.512551 11.00000 -1.50000 AFIX 0 C63 1 -0.219760 0.283558 0.590546 11.00000 0.01332 0.02190 = 0.02509 0.00115 -0.00053 0.00012 AFIX 137 H63A 2 -0.225446 0.245383 0.622376 11.00000 -1.50000 H63B 2 -0.272400 0.257776 0.562243 11.00000 -1.50000 H63C 2 -0.240033 0.350324 0.597380 11.00000 -1.50000 AFIX 0 O5 4 0.210057 0.923889 0.483882 11.00000 0.02458 0.02160 = 0.02905 0.00034 0.00401 0.00357 H5 2 0.249566 0.882406 0.501876 11.00000 0.03687 C5 1 0.275487 0.956631 0.443430 11.00000 0.03017 0.02201 = 0.02645 -0.00069 0.00287 0.00047 AFIX 137 H5A 2 0.224074 0.975430 0.413003 11.00000 -1.50000 H5B 2 0.326214 0.905137 0.433365 11.00000 -1.50000 H5C 2 0.321520 1.012017 0.455887 11.00000 -1.50000 AFIX 0 O6 4 0.355430 0.794836 0.538300 11.00000 0.02184 0.01887 = 0.03509 0.00676 -0.00205 -0.00203 H6 2 0.349078 0.736104 0.546336 11.00000 0.03709 C6 1 0.473471 0.815077 0.537692 11.00000 0.02486 0.02797 = 0.04409 -0.00022 0.00044 -0.00505 AFIX 137 H6A 2 0.508913 0.767757 0.515792 11.00000 -1.50000 H6B 2 0.510003 0.812075 0.573510 11.00000 -1.50000 H6C 2 0.483373 0.879438 0.523353 11.00000 -1.50000 AFIX 0 O7 4 0.718364 0.190199 0.727874 21.00000 0.02261 0.03276 = 0.04543 -0.01286 0.00915 -0.00086 AFIX 147 H7 2 0.665030 0.224052 0.737896 21.00000 -1.50000 AFIX 0 C7 1 0.671886 0.115132 0.695791 21.00000 0.03071 0.02560 = 0.02593 -0.00036 0.00736 -0.00060 AFIX 137 H7A 2 0.622639 0.142091 0.666618 21.00000 -1.50000 H7B 2 0.626609 0.072645 0.716521 21.00000 -1.50000 H7C 2 0.734139 0.078539 0.681958 21.00000 -1.50000 AFIX 0 PART 1 SAME 0.01 O82 C82 O81 4 0.690859 0.388857 0.838980 31.00000 0.01771 0.03860 = 0.02975 -0.01418 0.00210 -0.00081 H81 2 0.649790 0.354759 0.815534 31.00000 0.04745 C81 1 0.804355 0.366209 0.830001 31.00000 0.01822 0.03165 = 0.02955 0.00319 0.00414 0.00504 AFIX 137 H81A 2 0.816747 0.379107 0.793257 31.00000 -1.50000 H81B 2 0.818652 0.298193 0.837670 31.00000 -1.50000 H81C 2 0.856881 0.405518 0.852807 31.00000 -1.50000 AFIX 0 PART 2 SAME 0.01 O5 C5 O82 4 0.759324 0.275210 0.820648 -31.00000 0.03445 0.07923 = 0.04218 0.01817 -0.01004 0.00037 AFIX 147 H82 2 0.706558 0.266675 0.796831 -31.00000 -1.50000 AFIX 0 C82 1 0.781471 0.374898 0.826580 -31.00000 0.05265 0.08173 = 0.05009 -0.02030 -0.02405 0.03495 AFIX 137 H82A 2 0.826043 0.397071 0.798156 -31.00000 -1.50000 H82B 2 0.824894 0.386530 0.860374 -31.00000 -1.50000 H82C 2 0.708764 0.409906 0.825306 -31.00000 -1.50000 AFIX 0 PART 0 PART 1 SAME 0.01 O92 C92 O91 4 0.799609 0.097407 0.820204 41.00000 0.04568 0.06967 = 0.02951 -0.01094 0.00126 0.02241 H91 2 0.772131 0.132136 0.792173 41.00000 0.03881 C91 1 0.856512 0.016199 0.801028 41.00000 0.08322 0.08199 = 0.05087 0.01784 0.02015 0.05410 AFIX 137 H91A 2 0.800073 -0.026944 0.783053 41.00000 -1.50000 H91B 2 0.897534 -0.017702 0.830418 41.00000 -1.50000 H91C 2 0.911153 0.037267 0.776396 41.00000 -1.50000 AFIX 0 PART 2 SAME 0.01 O6 C6 O92 4 0.805398 -0.082042 0.804072 -41.00000 0.04911 0.06935 = 0.05708 0.01261 0.01871 0.01972 AFIX 147 H92 2 0.837640 -0.114617 0.781929 -41.00000 -1.50000 AFIX 0 C92 1 0.836355 0.014678 0.799789 -41.00000 0.02656 0.07478 = 0.03295 -0.01965 0.00724 -0.00264 AFIX 137 H92A 2 0.838247 0.031568 0.762702 -41.00000 -1.50000 H92B 2 0.912275 0.024928 0.818004 -41.00000 -1.50000 H92C 2 0.780166 0.055093 0.815668 -41.00000 -1.50000 PART 0 AFIX 0 HKLF 4 REM jk440 in P2(1)/n REM wR2 = 0.0803, GooF = S = 1.096, Restrained GooF = 1.100 for all data REM R1 = 0.0322 for 13266 Fo > 4sig(Fo) and 0.0368 for all 14635 data REM 561 parameters refined using 105 restraints END WGHT 0.0349 3.2090 REM Highest difference peak 1.080, deepest hole -0.940, 1-sigma level 0.078 Q1 1 0.5789 0.2613 0.7441 11.00000 0.05 1.08 Q2 1 0.1790 0.2636 0.6057 11.00000 0.05 1.07 Q3 1 0.2165 0.3148 0.6540 11.00000 0.05 0.92 Q4 1 0.1825 0.3249 0.6107 11.00000 0.05 0.89 Q5 1 0.2127 0.2375 0.6459 11.00000 0.05 0.75 Q6 1 0.1555 0.2808 0.6478 11.00000 0.05 0.68 Q7 1 0.2162 0.2252 0.4899 11.00000 0.05 0.56 Q8 1 0.2515 0.2589 0.7831 11.00000 0.05 0.55 Q9 1 0.3536 0.5430 0.5157 11.00000 0.05 0.55 Q10 1 0.2811 0.3829 0.4996 11.00000 0.05 0.54 Q11 1 0.2781 0.4244 0.5435 11.00000 0.05 0.54 Q12 1 0.2276 0.2793 0.4519 11.00000 0.05 0.54 Q13 1 0.1906 0.1641 0.6331 11.00000 0.05 0.53 Q14 1 0.1567 0.1394 0.5698 11.00000 0.05 0.52 Q15 1 0.3062 0.5011 0.5497 11.00000 0.05 0.52 Q16 1 0.0437 0.2701 0.7508 11.00000 0.05 0.50 Q17 1 0.0421 0.0152 0.6046 11.00000 0.05 0.50 Q18 1 0.1883 0.1871 0.6160 11.00000 0.05 0.50 Q19 1 0.2761 0.3551 0.4542 11.00000 0.05 0.50 Q20 1 0.4606 0.2485 0.8079 11.00000 0.05 0.50 Q21 1 0.3594 0.5059 0.4743 11.00000 0.05 0.49 Q22 1 0.1670 0.2612 0.8142 11.00000 0.05 0.48 Q23 1 0.2517 0.3406 0.5371 11.00000 0.05 0.48 Q24 1 0.0609 0.0418 0.6531 11.00000 0.05 0.48 Q25 1 0.3137 0.4340 0.4644 11.00000 0.05 0.48 Q26 1 -0.0113 0.3054 0.6547 11.00000 0.05 0.47 Q27 1 0.2098 0.2657 0.5308 11.00000 0.05 0.47 Q28 1 0.0831 0.2552 0.7921 11.00000 0.05 0.46 Q29 1 0.1642 0.1913 0.5249 11.00000 0.05 0.45 Q30 1 -0.0023 0.4807 0.6139 11.00000 0.05 0.45 Q31 1 -0.0928 0.3080 0.5475 11.00000 0.05 0.44 Q32 1 0.3653 0.2555 0.8310 11.00000 0.05 0.43 ; _shelx_res_checksum 99261 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' 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 0.19870(2) 0.28835(2) 0.63066(2) 0.01175(3) Uani 1 1 d . . . . . P1 P 0.17285(3) 0.13276(2) 0.60716(2) 0.01288(6) Uani 1 1 d . . . . . P2 P 0.01094(3) 0.32555(2) 0.62558(2) 0.01310(6) Uani 1 1 d . . . . . O1 O 0.34721(11) 0.61519(8) 0.57124(4) 0.0244(2) Uani 1 1 d . . . . . O2 O 0.55492(11) 0.28932(10) 0.76354(6) 0.0361(3) Uani 1 1 d . . . . . O3 O 0.23708(9) 0.43778(7) 0.64977(4) 0.01683(18) Uani 1 1 d D . . . . H3 H 0.258(2) 0.4524(19) 0.6189(7) 0.049(7) Uiso 1 1 d D . . . . C3 C 0.30925(14) 0.47736(11) 0.69163(6) 0.0256(3) Uani 1 1 d . . . . . H3A H 0.321583 0.545643 0.684971 0.038 Uiso 1 1 calc R U . . . H3B H 0.383024 0.443839 0.694262 0.038 Uiso 1 1 calc R U . . . H3C H 0.272948 0.469890 0.724535 0.038 Uiso 1 1 calc R U . . . O4 O 0.38493(8) 0.26589(8) 0.64249(4) 0.01897(19) Uani 1 1 d D . . . . H4 H 0.387(2) 0.273(2) 0.6776(6) 0.053(8) Uiso 1 1 d D . . . . C4 C 0.47257(13) 0.31768(12) 0.61955(7) 0.0254(3) Uani 1 1 d . . . . . H4A H 0.477056 0.296256 0.583306 0.038 Uiso 1 1 calc R U . . . H4B H 0.546126 0.306099 0.639662 0.038 Uiso 1 1 calc R U . . . H4C H 0.454959 0.386378 0.619858 0.038 Uiso 1 1 calc R U . . . N11 N 0.22330(9) 0.30417(8) 0.54769(4) 0.01336(19) Uani 1 1 d . . . . . N12 N 0.28838(10) 0.46195(8) 0.55770(5) 0.0159(2) Uani 1 1 d . . . . . N21 N 0.17109(10) 0.26910(8) 0.71288(4) 0.0155(2) Uani 1 1 d . . . . . N22 N 0.36610(11) 0.27185(9) 0.73974(5) 0.0208(2) Uani 1 1 d . . . . . C11 C 0.14283(11) 0.14173(9) 0.53580(5) 0.0150(2) Uani 1 1 d . . . . . H11A H 0.172331 0.083874 0.518983 0.018 Uiso 1 1 calc R U . . . H11B H 0.058981 0.144477 0.527077 0.018 Uiso 1 1 calc R U . . . C12 C 0.19747(11) 0.22940(9) 0.51466(5) 0.0143(2) Uani 1 1 d . . . . . C13 C 0.21488(12) 0.23102(10) 0.46116(5) 0.0174(2) Uani 1 1 d . . . . . H13 H 0.194016 0.177160 0.439720 0.021 Uiso 1 1 calc R U . . . C14 C 0.26224(12) 0.31072(10) 0.43970(5) 0.0184(2) Uani 1 1 d . . . . . H14 H 0.274883 0.312566 0.403525 0.022 Uiso 1 1 calc R U . . . C15 C 0.29131(11) 0.38886(10) 0.47232(5) 0.0157(2) Uani 1 1 d . . . . . C16 C 0.34480(12) 0.47368(10) 0.45427(6) 0.0191(2) Uani 1 1 d . . . . . H16 H 0.364062 0.477553 0.418998 0.023 Uiso 1 1 calc R U . . . C17 C 0.36801(12) 0.54828(10) 0.48724(6) 0.0189(2) Uani 1 1 d . . . . . H17 H 0.406216 0.603335 0.475478 0.023 Uiso 1 1 calc R U . . . C18 C 0.33462(12) 0.54432(10) 0.54058(6) 0.0178(2) Uani 1 1 d . . . . . C19 C 0.26799(11) 0.38554(9) 0.52583(5) 0.0138(2) Uani 1 1 d . . . . . C21 C -0.03496(12) 0.26783(10) 0.68472(5) 0.0177(2) Uani 1 1 d . . . . . H21A H -0.099002 0.304663 0.697779 0.021 Uiso 1 1 calc R U . . . H21B H -0.062835 0.202257 0.676009 0.021 Uiso 1 1 calc R U . . . C22 C 0.06195(12) 0.26265(10) 0.72671(5) 0.0180(2) Uani 1 1 d . . . . . C23 C 0.03430(15) 0.24749(12) 0.77827(6) 0.0258(3) Uani 1 1 d . . . . . H23 H -0.043588 0.242403 0.785675 0.031 Uiso 1 1 calc R U . . . C24 C 0.11972(17) 0.23999(13) 0.81806(6) 0.0286(3) Uani 1 1 d . . . . . H24 H 0.102007 0.228961 0.853113 0.034 Uiso 1 1 calc R U . . . C25 C 0.23305(15) 0.24888(11) 0.80597(6) 0.0236(3) Uani 1 1 d . . . . . C26 C 0.32836(17) 0.24236(12) 0.84486(6) 0.0303(4) Uani 1 1 d . . . . . H26 H 0.315513 0.229980 0.880404 0.036 Uiso 1 1 calc R U . . . C27 C 0.43536(17) 0.25373(12) 0.83109(7) 0.0314(4) Uani 1 1 d . . . . . H27 H 0.498218 0.249771 0.856942 0.038 Uiso 1 1 calc R U . . . C28 C 0.45554(15) 0.27204(11) 0.77694(7) 0.0263(3) Uani 1 1 d . . . . . C29 C 0.25761(13) 0.26291(10) 0.75319(5) 0.0184(2) Uani 1 1 d . . . . . C31 C 0.05280(11) 0.05418(9) 0.62447(5) 0.0156(2) Uani 1 1 d . . . . . H31 H -0.017760 0.094816 0.621118 0.019 Uiso 1 1 calc R U . . . C32 C 0.06639(13) 0.01930(11) 0.68153(6) 0.0206(3) Uani 1 1 d . . . . . H32A H 0.124592 -0.031286 0.685101 0.031 Uiso 1 1 calc R U . . . H32B H -0.006863 -0.006123 0.691307 0.031 Uiso 1 1 calc R U . . . H32C H 0.090125 0.073025 0.704618 0.031 Uiso 1 1 calc R U . . . C33 C 0.02958(13) -0.03088(10) 0.58691(6) 0.0199(3) Uani 1 1 d . . . . . H33A H 0.008276 -0.006827 0.551466 0.030 Uiso 1 1 calc R U . . . H33B H -0.033117 -0.069761 0.598660 0.030 Uiso 1 1 calc R U . . . H33C H 0.098776 -0.070311 0.586660 0.030 Uiso 1 1 calc R U . . . C41 C 0.29767(12) 0.04930(10) 0.61594(6) 0.0190(3) Uani 1 1 d . . . . . H41 H 0.267787 -0.016551 0.607453 0.023 Uiso 1 1 calc R U . . . C42 C 0.35250(14) 0.04607(12) 0.67286(7) 0.0263(3) Uani 1 1 d . . . . . H42A H 0.396746 0.104822 0.680389 0.039 Uiso 1 1 calc R U . . . H42B H 0.403353 -0.009661 0.677267 0.039 Uiso 1 1 calc R U . . . H42C H 0.292200 0.040999 0.697068 0.039 Uiso 1 1 calc R U . . . C43 C 0.38894(13) 0.07046(12) 0.57796(7) 0.0250(3) Uani 1 1 d . . . . . H43A H 0.355615 0.062746 0.541812 0.037 Uiso 1 1 calc R U . . . H43B H 0.453074 0.025775 0.584583 0.037 Uiso 1 1 calc R U . . . H43C H 0.416519 0.136400 0.583207 0.037 Uiso 1 1 calc R U . . . C51 C -0.03419(12) 0.45280(10) 0.63310(6) 0.0184(2) Uani 1 1 d . . . . . H51 H -0.119569 0.453237 0.626823 0.022 Uiso 1 1 calc R U . . . C52 C 0.01033(14) 0.52124(11) 0.59215(6) 0.0234(3) Uani 1 1 d . . . . . H52A H 0.091304 0.535527 0.601604 0.035 Uiso 1 1 calc R U . . . H52B H -0.033979 0.580917 0.591251 0.035 Uiso 1 1 calc R U . . . H52C H 0.001995 0.490819 0.557521 0.035 Uiso 1 1 calc R U . . . C53 C -0.00664(14) 0.49249(11) 0.68866(6) 0.0248(3) Uani 1 1 d . . . . . H53A H -0.040845 0.450891 0.713997 0.037 Uiso 1 1 calc R U . . . H53B H -0.038072 0.557382 0.690802 0.037 Uiso 1 1 calc R U . . . H53C H 0.076576 0.494547 0.696664 0.037 Uiso 1 1 calc R U . . . C61 C -0.09638(11) 0.27915(10) 0.57428(5) 0.0154(2) Uani 1 1 d . . . . . H61 H -0.078447 0.209612 0.569986 0.018 Uiso 1 1 calc R U . . . C62 C -0.08792(12) 0.32548(11) 0.52030(6) 0.0205(3) Uani 1 1 d . . . . . H62A H -0.119406 0.390591 0.520471 0.031 Uiso 1 1 calc R U . . . H62B H -0.131502 0.287186 0.493437 0.031 Uiso 1 1 calc R U . . . H62C H -0.007470 0.328233 0.512551 0.031 Uiso 1 1 calc R U . . . C63 C -0.21976(12) 0.28356(11) 0.59055(6) 0.0202(3) Uani 1 1 d . . . . . H63A H -0.225446 0.245383 0.622376 0.030 Uiso 1 1 calc R U . . . H63B H -0.272400 0.257776 0.562243 0.030 Uiso 1 1 calc R U . . . H63C H -0.240033 0.350324 0.597380 0.030 Uiso 1 1 calc R U . . . O5 O 0.21006(10) 0.92389(8) 0.48388(5) 0.0250(2) Uani 1 1 d D . . . . H5 H 0.2496(19) 0.8824(15) 0.5019(8) 0.037(6) Uiso 1 1 d D . . . . C5 C 0.27549(15) 0.95663(12) 0.44343(6) 0.0262(3) Uani 1 1 d D . . . . H5A H 0.224074 0.975430 0.413003 0.039 Uiso 1 1 calc R U . . . H5B H 0.326214 0.905137 0.433365 0.039 Uiso 1 1 calc R U . . . H5C H 0.321520 1.012017 0.455887 0.039 Uiso 1 1 calc R U . . . O6 O 0.35543(10) 0.79484(8) 0.53830(5) 0.0255(2) Uani 1 1 d D . . . . H6 H 0.349(2) 0.7361(11) 0.5463(9) 0.037(6) Uiso 1 1 d D . . . . C6 C 0.47347(15) 0.81508(14) 0.53769(8) 0.0324(4) Uani 1 1 d D . . . . H6A H 0.508913 0.767757 0.515792 0.049 Uiso 1 1 calc R U . . . H6B H 0.510003 0.812075 0.573510 0.049 Uiso 1 1 calc R U . . . H6C H 0.483373 0.879438 0.523353 0.049 Uiso 1 1 calc R U . . . O7 O 0.71836(15) 0.19020(14) 0.72787(8) 0.0333(5) Uani 0.732(4) 1 d D . P . . H7 H 0.665030 0.224052 0.737896 0.050 Uiso 0.732(4) 1 calc DR U P . . C7 C 0.6719(2) 0.11513(17) 0.69579(9) 0.0271(5) Uani 0.732(4) 1 d . . P . . H7A H 0.622639 0.142091 0.666618 0.041 Uiso 0.732(4) 1 calc R U P . . H7B H 0.626609 0.072645 0.716521 0.041 Uiso 0.732(4) 1 calc R U P . . H7C H 0.734139 0.078539 0.681958 0.041 Uiso 0.732(4) 1 calc R U P . . O81 O 0.69086(13) 0.38886(13) 0.83898(7) 0.0287(5) Uani 0.737(4) 1 d D U P A 1 H81 H 0.650(3) 0.355(2) 0.8155(11) 0.047(10) Uiso 0.737(4) 1 d D . P A 1 C81 C 0.8044(3) 0.3662(3) 0.83000(19) 0.0264(7) Uani 0.737(4) 1 d D U P A 1 H81A H 0.816747 0.379107 0.793257 0.040 Uiso 0.737(4) 1 calc R U P A 1 H81B H 0.818652 0.298193 0.837670 0.040 Uiso 0.737(4) 1 calc R U P A 1 H81C H 0.856881 0.405518 0.852807 0.040 Uiso 0.737(4) 1 calc R U P A 1 O82 O 0.7593(6) 0.2752(5) 0.8206(3) 0.0527(18) Uani 0.263(4) 1 d D U P A 2 H82 H 0.706558 0.266675 0.796831 0.079 Uiso 0.263(4) 1 calc R U P A 2 C82 C 0.7815(14) 0.3749(8) 0.8266(9) 0.063(4) Uani 0.263(4) 1 d D U P A 2 H82A H 0.826043 0.397071 0.798156 0.095 Uiso 0.263(4) 1 calc R U P A 2 H82B H 0.824894 0.386530 0.860374 0.095 Uiso 0.263(4) 1 calc R U P A 2 H82C H 0.708764 0.409906 0.825306 0.095 Uiso 0.263(4) 1 calc R U P A 2 O91 O 0.7996(2) 0.0974(2) 0.82020(9) 0.0484(7) Uani 0.681(4) 1 d D U P B 1 H91 H 0.772(3) 0.132(2) 0.7922(10) 0.039(9) Uiso 0.681(4) 1 d D . P B 1 C91 C 0.8565(7) 0.0162(5) 0.8010(3) 0.071(2) Uani 0.681(4) 1 d D U P B 1 H91A H 0.800073 -0.026944 0.783053 0.107 Uiso 0.681(4) 1 calc R U P B 1 H91B H 0.897534 -0.017702 0.830418 0.107 Uiso 0.681(4) 1 calc R U P B 1 H91C H 0.911153 0.037267 0.776396 0.107 Uiso 0.681(4) 1 calc R U P B 1 O92 O 0.8054(5) -0.0820(4) 0.8041(2) 0.0577(17) Uani 0.319(4) 1 d D U P B 2 H92 H 0.837640 -0.114617 0.781929 0.087 Uiso 0.319(4) 1 calc R U P B 2 C92 C 0.8364(11) 0.0147(8) 0.7998(5) 0.045(2) Uani 0.319(4) 1 d D U P B 2 H92A H 0.838247 0.031568 0.762702 0.067 Uiso 0.319(4) 1 calc R U P B 2 H92B H 0.912275 0.024928 0.818004 0.067 Uiso 0.319(4) 1 calc R U P B 2 H92C H 0.780166 0.055093 0.815668 0.067 Uiso 0.319(4) 1 calc R U P B 2 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 0.01105(5) 0.01141(5) 0.01236(5) -0.00149(3) -0.00147(3) -0.00064(3) P1 0.01184(13) 0.01171(13) 0.01466(14) -0.00085(11) -0.00144(11) -0.00071(10) P2 0.01244(13) 0.01291(14) 0.01371(14) 0.00040(11) -0.00041(11) 0.00061(11) O1 0.0345(6) 0.0146(5) 0.0234(5) -0.0009(4) -0.0013(4) -0.0066(4) O2 0.0252(6) 0.0362(7) 0.0439(8) -0.0011(6) -0.0157(5) -0.0013(5) O3 0.0201(5) 0.0143(4) 0.0155(4) -0.0028(3) -0.0018(3) -0.0033(3) C3 0.0303(8) 0.0190(7) 0.0254(7) -0.0070(5) -0.0102(6) -0.0003(6) O4 0.0124(4) 0.0206(5) 0.0234(5) -0.0025(4) -0.0012(4) -0.0022(3) C4 0.0143(6) 0.0226(7) 0.0393(9) 0.0011(6) 0.0015(6) -0.0028(5) N11 0.0127(4) 0.0123(5) 0.0149(5) -0.0011(4) -0.0004(4) -0.0007(3) N12 0.0172(5) 0.0127(5) 0.0177(5) -0.0010(4) 0.0003(4) -0.0023(4) N21 0.0194(5) 0.0132(5) 0.0132(5) -0.0005(4) -0.0026(4) 0.0014(4) N22 0.0214(6) 0.0173(5) 0.0220(6) -0.0025(4) -0.0087(5) 0.0014(4) C11 0.0159(5) 0.0132(5) 0.0156(5) -0.0021(4) -0.0002(4) -0.0020(4) C12 0.0133(5) 0.0138(5) 0.0156(5) -0.0017(4) 0.0001(4) -0.0002(4) C13 0.0199(6) 0.0163(6) 0.0157(6) -0.0028(4) 0.0003(5) -0.0001(5) C14 0.0210(6) 0.0193(6) 0.0152(6) -0.0007(5) 0.0021(5) 0.0010(5) C15 0.0152(5) 0.0155(6) 0.0164(6) 0.0012(4) 0.0012(4) 0.0013(4) C16 0.0197(6) 0.0184(6) 0.0195(6) 0.0038(5) 0.0029(5) 0.0010(5) C17 0.0181(6) 0.0162(6) 0.0223(6) 0.0042(5) 0.0008(5) -0.0013(5) C18 0.0174(6) 0.0146(6) 0.0205(6) 0.0021(5) -0.0026(5) -0.0010(4) C19 0.0119(5) 0.0135(5) 0.0159(5) -0.0003(4) -0.0004(4) 0.0007(4) C21 0.0175(6) 0.0189(6) 0.0169(6) 0.0023(5) 0.0016(5) 0.0004(5) C22 0.0222(6) 0.0162(6) 0.0155(6) 0.0008(4) 0.0015(5) 0.0023(5) C23 0.0313(8) 0.0278(8) 0.0186(6) 0.0039(6) 0.0050(6) 0.0032(6) C24 0.0429(9) 0.0279(8) 0.0147(6) 0.0035(5) 0.0017(6) 0.0034(7) C25 0.0373(8) 0.0157(6) 0.0163(6) 0.0010(5) -0.0070(5) 0.0023(6) C26 0.0488(10) 0.0199(7) 0.0195(7) 0.0020(5) -0.0142(7) 0.0007(7) C27 0.0446(10) 0.0172(7) 0.0283(8) 0.0013(6) -0.0218(7) -0.0006(6) C28 0.0292(8) 0.0154(6) 0.0314(8) -0.0018(5) -0.0147(6) 0.0003(5) C29 0.0256(7) 0.0112(5) 0.0169(6) -0.0018(4) -0.0067(5) 0.0024(5) C31 0.0150(5) 0.0137(5) 0.0178(6) 0.0008(4) -0.0006(4) -0.0019(4) C32 0.0252(7) 0.0186(6) 0.0180(6) 0.0021(5) 0.0003(5) -0.0030(5) C33 0.0212(6) 0.0163(6) 0.0215(6) -0.0014(5) -0.0014(5) -0.0061(5) C41 0.0150(6) 0.0150(6) 0.0261(7) -0.0020(5) -0.0029(5) 0.0017(4) C42 0.0206(7) 0.0252(7) 0.0314(8) 0.0039(6) -0.0075(6) 0.0025(5) C43 0.0159(6) 0.0261(7) 0.0330(8) -0.0084(6) 0.0020(5) 0.0018(5) C51 0.0165(6) 0.0147(6) 0.0237(6) -0.0012(5) 0.0006(5) 0.0019(4) C52 0.0285(7) 0.0149(6) 0.0260(7) 0.0027(5) -0.0019(6) 0.0009(5) C53 0.0292(7) 0.0195(7) 0.0264(7) -0.0066(5) 0.0058(6) 0.0009(6) C61 0.0125(5) 0.0154(6) 0.0178(6) 0.0006(4) -0.0020(4) 0.0004(4) C62 0.0182(6) 0.0251(7) 0.0177(6) 0.0025(5) -0.0026(5) -0.0006(5) C63 0.0133(5) 0.0219(6) 0.0251(7) 0.0012(5) -0.0005(5) 0.0001(5) O5 0.0246(5) 0.0216(5) 0.0291(6) 0.0003(4) 0.0040(4) 0.0036(4) C5 0.0302(8) 0.0220(7) 0.0264(7) -0.0007(6) 0.0029(6) 0.0005(6) O6 0.0218(5) 0.0189(5) 0.0351(6) 0.0068(4) -0.0021(4) -0.0020(4) C6 0.0249(8) 0.0280(8) 0.0441(10) -0.0002(7) 0.0004(7) -0.0051(6) O7 0.0226(8) 0.0328(9) 0.0454(11) -0.0129(8) 0.0091(7) -0.0009(6) C7 0.0307(11) 0.0256(11) 0.0259(10) -0.0004(8) 0.0074(8) -0.0006(8) O81 0.0177(7) 0.0386(10) 0.0297(9) -0.0142(7) 0.0021(6) -0.0008(6) C81 0.0182(13) 0.0316(12) 0.0296(15) 0.0032(10) 0.0041(12) 0.0050(10) O82 0.034(3) 0.079(4) 0.042(3) 0.018(3) -0.010(2) 0.000(3) C82 0.053(7) 0.082(6) 0.050(6) -0.020(5) -0.024(5) 0.035(5) O91 0.0457(13) 0.0697(18) 0.0295(11) -0.0109(11) 0.0013(9) 0.0224(12) C91 0.083(5) 0.082(4) 0.051(3) 0.018(3) 0.020(3) 0.054(3) O92 0.049(3) 0.069(4) 0.057(3) 0.013(3) 0.019(3) 0.020(3) C92 0.027(3) 0.075(5) 0.033(4) -0.020(4) 0.007(3) -0.003(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 N21 Ru1 N11 178.39(4) . . ? N21 Ru1 O3 86.86(4) . . ? N11 Ru1 O3 94.61(4) . . ? N21 Ru1 O4 94.28(4) . . ? N11 Ru1 O4 86.49(4) . . ? O3 Ru1 O4 85.49(4) . . ? N21 Ru1 P2 82.04(3) . . ? N11 Ru1 P2 97.34(3) . . ? O3 Ru1 P2 88.58(3) . . ? O4 Ru1 P2 173.19(3) . . ? N21 Ru1 P1 96.41(3) . . ? N11 Ru1 P1 82.16(3) . . ? O3 Ru1 P1 175.04(3) . . ? O4 Ru1 P1 90.54(3) . . ? P2 Ru1 P1 95.550(13) . . ? C11 P1 C31 100.97(6) . . ? C11 P1 C41 104.24(6) . . ? C31 P1 C41 101.76(6) . . ? C11 P1 Ru1 102.09(4) . . ? C31 P1 Ru1 125.90(5) . . ? C41 P1 Ru1 118.59(5) . . ? C21 P2 C61 101.71(6) . . ? C21 P2 C51 103.13(7) . . ? C61 P2 C51 102.89(6) . . ? C21 P2 Ru1 101.70(5) . . ? C61 P2 Ru1 124.14(5) . . ? C51 P2 Ru1 119.77(5) . . ? C3 O3 Ru1 129.77(9) . . ? C3 O3 H3 113.5(18) . . ? Ru1 O3 H3 95.1(18) . . ? O3 C3 H3A 109.5 . . ? O3 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? O3 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C4 O4 Ru1 127.81(9) . . ? C4 O4 H4 113.4(18) . . ? Ru1 O4 H4 93.7(18) . . ? O4 C4 H4A 109.5 . . ? O4 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? O4 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C12 N11 C19 116.63(11) . . ? C12 N11 Ru1 119.20(9) . . ? C19 N11 Ru1 124.14(8) . . ? C19 N12 C18 121.84(12) . . ? C22 N21 C29 116.60(12) . . ? C22 N21 Ru1 118.67(9) . . ? C29 N21 Ru1 124.73(10) . . ? C29 N22 C28 120.69(14) . . ? C12 C11 P1 111.21(9) . . ? C12 C11 H11A 109.4 . . ? P1 C11 H11A 109.4 . . ? C12 C11 H11B 109.4 . . ? P1 C11 H11B 109.4 . . ? H11A C11 H11B 108.0 . . ? N11 C12 C13 123.52(12) . . ? N11 C12 C11 118.64(11) . . ? C13 C12 C11 117.79(11) . . ? C14 C13 C12 119.93(13) . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C13 C14 C15 118.51(13) . . ? C13 C14 H14 120.7 . . ? C15 C14 H14 120.7 . . ? C14 C15 C19 119.61(12) . . ? C14 C15 C16 122.85(13) . . ? C19 C15 C16 117.54(12) . . ? C17 C16 C15 120.28(13) . . ? C17 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? C16 C17 C18 120.10(13) . . ? C16 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? O1 C18 N12 119.36(13) . . ? O1 C18 C17 121.86(13) . . ? N12 C18 C17 118.77(12) . . ? N12 C19 N11 117.10(12) . . ? N12 C19 C15 121.22(12) . . ? N11 C19 C15 121.69(12) . . ? C22 C21 P2 110.88(10) . . ? C22 C21 H21A 109.5 . . ? P2 C21 H21A 109.5 . . ? C22 C21 H21B 109.5 . . ? P2 C21 H21B 109.5 . . ? H21A C21 H21B 108.1 . . ? N21 C22 C23 123.49(13) . . ? N21 C22 C21 118.93(12) . . ? C23 C22 C21 117.53(13) . . ? C24 C23 C22 119.98(16) . . ? C24 C23 H23 120.0 . . ? C22 C23 H23 120.0 . . ? C23 C24 C25 118.59(15) . . ? C23 C24 H24 120.7 . . ? C25 C24 H24 120.7 . . ? C24 C25 C29 119.73(14) . . ? C24 C25 C26 122.76(15) . . ? C29 C25 C26 117.49(16) . . ? C27 C26 C25 120.08(16) . . ? C27 C26 H26 120.0 . . ? C25 C26 H26 120.0 . . ? C26 C27 C28 120.22(14) . . ? C26 C27 H27 119.9 . . ? C28 C27 H27 119.9 . . ? O2 C28 N22 119.05(17) . . ? O2 C28 C27 121.36(15) . . ? N22 C28 C27 119.59(16) . . ? N22 C29 N21 116.74(13) . . ? N22 C29 C25 121.69(13) . . ? N21 C29 C25 121.57(14) . . ? C32 C31 C33 110.47(11) . . ? C32 C31 P1 113.04(9) . . ? C33 C31 P1 113.74(10) . . ? C32 C31 H31 106.3 . . ? C33 C31 H31 106.3 . . ? P1 C31 H31 106.3 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C43 C41 C42 110.28(12) . . ? C43 C41 P1 112.60(10) . . ? C42 C41 P1 113.10(10) . . ? C43 C41 H41 106.8 . . ? C42 C41 H41 106.8 . . ? P1 C41 H41 106.8 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C53 C51 C52 110.49(12) . . ? C53 C51 P2 113.50(10) . . ? C52 C51 P2 113.83(10) . . ? C53 C51 H51 106.1 . . ? C52 C51 H51 106.1 . . ? P2 C51 H51 106.1 . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C51 C53 H53A 109.5 . . ? C51 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C51 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C62 C61 C63 111.02(11) . . ? C62 C61 P2 113.52(9) . . ? C63 C61 P2 113.03(10) . . ? C62 C61 H61 106.2 . . ? C63 C61 H61 106.2 . . ? P2 C61 H61 106.2 . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C61 C63 H63A 109.5 . . ? C61 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C61 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C5 O5 H5 108.2(16) . . ? O5 C5 H5A 109.5 . . ? O5 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? O5 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C6 O6 H6 107.5(17) . . ? O6 C6 H6A 109.5 . . ? O6 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? O6 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C7 O7 H7 109.5 . . ? O7 C7 H7A 109.5 . . ? O7 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? O7 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C81 O81 H81 104(2) . . ? O81 C81 H81A 109.5 . . ? O81 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? O81 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? C82 O82 H82 109.5 . . ? O82 C82 H82A 109.5 . . ? O82 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? O82 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? C91 O91 H91 107(2) . . ? O91 C91 H91A 109.5 . . ? O91 C91 H91B 109.5 . . ? H91A C91 H91B 109.5 . . ? O91 C91 H91C 109.5 . . ? H91A C91 H91C 109.5 . . ? H91B C91 H91C 109.5 . . ? C92 O92 H92 109.5 . . ? O92 C92 H92A 109.5 . . ? O92 C92 H92B 109.5 . . ? H92A C92 H92B 109.5 . . ? O92 C92 H92C 109.5 . . ? H92A C92 H92C 109.5 . . ? H92B C92 H92C 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 Ru1 N21 2.1718(12) . ? Ru1 N11 2.1778(11) . ? Ru1 O3 2.1784(10) . ? Ru1 O4 2.2004(10) . ? Ru1 P2 2.2534(3) . ? Ru1 P1 2.2648(3) . ? P1 C11 1.8353(13) . ? P1 C31 1.8651(14) . ? P1 C41 1.8679(14) . ? P2 C21 1.8338(14) . ? P2 C61 1.8576(13) . ? P2 C51 1.8658(14) . ? O1 C18 1.2628(17) . ? O2 C28 1.264(2) . ? O3 C3 1.4204(17) . ? O3 H3 0.872(15) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? O4 C4 1.4213(18) . ? O4 H4 0.902(15) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? N11 C12 1.3604(16) . ? N11 C19 1.3866(17) . ? N12 C19 1.3510(17) . ? N12 C18 1.3578(18) . ? N21 C22 1.3578(19) . ? N21 C29 1.3880(17) . ? N22 C29 1.350(2) . ? N22 C28 1.3563(18) . ? C11 C12 1.5014(18) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.4010(19) . ? C13 C14 1.377(2) . ? C13 H13 0.9500 . ? C14 C15 1.3974(19) . ? C14 H14 0.9500 . ? C15 C19 1.4195(19) . ? C15 C16 1.4327(19) . ? C16 C17 1.353(2) . ? C16 H16 0.9500 . ? C17 C18 1.452(2) . ? C17 H17 0.9500 . ? C21 C22 1.499(2) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.401(2) . ? C23 C24 1.371(2) . ? C23 H23 0.9500 . ? C24 C25 1.394(3) . ? C24 H24 0.9500 . ? C25 C29 1.418(2) . ? C25 C26 1.436(2) . ? C26 C27 1.339(3) . ? C26 H26 0.9500 . ? C27 C28 1.448(3) . ? C27 H27 0.9500 . ? C31 C32 1.5349(19) . ? C31 C33 1.5367(19) . ? C31 H31 1.0000 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C41 C43 1.532(2) . ? C41 C42 1.543(2) . ? C41 H41 1.0000 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C51 C53 1.535(2) . ? C51 C52 1.540(2) . ? C51 H51 1.0000 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C61 C62 1.536(2) . ? C61 C63 1.5383(19) . ? C61 H61 1.0000 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? O5 C5 1.414(2) . ? O5 H5 0.852(15) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? O6 C6 1.413(2) . ? O6 H6 0.849(15) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? O7 C7 1.411(3) . ? O7 H7 0.8400 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? O81 C81 1.404(4) . ? O81 H81 0.877(16) . ? C81 H81A 0.9800 . ? C81 H81B 0.9800 . ? C81 H81C 0.9800 . ? O82 C82 1.420(9) . ? O82 H82 0.8400 . ? C82 H82A 0.9800 . ? C82 H82B 0.9800 . ? C82 H82C 0.9800 . ? O91 C91 1.422(7) . ? O91 H91 0.903(16) . ? C91 H91A 0.9800 . ? C91 H91B 0.9800 . ? C91 H91C 0.9800 . ? O92 C92 1.403(9) . ? O92 H92 0.8400 . ? C92 H92A 0.9800 . ? C92 H92B 0.9800 . ? C92 H92C 0.9800 . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag O3 H3 N12 0.872(15) 1.639(15) 2.5022(16) 170(3) . yes O4 H4 N22 0.902(15) 1.629(16) 2.5184(17) 168(3) . yes O5 H5 O6 0.852(15) 1.925(15) 2.7723(16) 173(2) . yes O6 H6 O1 0.849(15) 1.803(15) 2.6471(16) 172(2) . yes O7 H7 O2 0.84 1.75 2.588(2) 175.4 . yes O81^a H81^a O2 0.877(16) 1.896(17) 2.772(2) 176(4) . yes O82^b H82^b O2 0.84 1.93 2.708(6) 153.1 . yes O91^a H91^a O7 0.903(16) 1.894(17) 2.791(3) 172(3) . yes O92^b H92^b O2 0.84 2.23 3.059(6) 168.9 2_646 yes 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 C31 P1 C11 C12 157.82(9) . . . . ? C41 P1 C11 C12 -96.91(10) . . . . ? Ru1 P1 C11 C12 27.10(10) . . . . ? C19 N11 C12 C13 0.69(19) . . . . ? Ru1 N11 C12 C13 -177.17(10) . . . . ? C19 N11 C12 C11 -176.66(11) . . . . ? Ru1 N11 C12 C11 5.48(15) . . . . ? P1 C11 C12 N11 -22.82(15) . . . . ? P1 C11 C12 C13 159.68(10) . . . . ? N11 C12 C13 C14 1.1(2) . . . . ? C11 C12 C13 C14 178.50(13) . . . . ? C12 C13 C14 C15 -0.4(2) . . . . ? C13 C14 C15 C19 -2.1(2) . . . . ? C13 C14 C15 C16 177.67(13) . . . . ? C14 C15 C16 C17 178.08(14) . . . . ? C19 C15 C16 C17 -2.1(2) . . . . ? C15 C16 C17 C18 -2.5(2) . . . . ? C19 N12 C18 O1 176.83(13) . . . . ? C19 N12 C18 C17 -3.0(2) . . . . ? C16 C17 C18 O1 -174.70(14) . . . . ? C16 C17 C18 N12 5.2(2) . . . . ? C18 N12 C19 N11 178.38(12) . . . . ? C18 N12 C19 C15 -1.70(19) . . . . ? C12 N11 C19 N12 176.66(11) . . . . ? Ru1 N11 C19 N12 -5.59(16) . . . . ? C12 N11 C19 C15 -3.25(18) . . . . ? Ru1 N11 C19 C15 174.49(9) . . . . ? C14 C15 C19 N12 -175.86(12) . . . . ? C16 C15 C19 N12 4.35(19) . . . . ? C14 C15 C19 N11 4.05(19) . . . . ? C16 C15 C19 N11 -175.74(12) . . . . ? C61 P2 C21 C22 157.60(10) . . . . ? C51 P2 C21 C22 -96.00(11) . . . . ? Ru1 P2 C21 C22 28.68(10) . . . . ? C29 N21 C22 C23 -2.0(2) . . . . ? Ru1 N21 C22 C23 178.11(12) . . . . ? C29 N21 C22 C21 -179.35(12) . . . . ? Ru1 N21 C22 C21 0.75(17) . . . . ? P2 C21 C22 N21 -20.99(16) . . . . ? P2 C21 C22 C23 161.49(12) . . . . ? N21 C22 C23 C24 1.1(2) . . . . ? C21 C22 C23 C24 178.53(15) . . . . ? C22 C23 C24 C25 0.7(3) . . . . ? C23 C24 C25 C29 -1.6(2) . . . . ? C23 C24 C25 C26 179.83(16) . . . . ? C24 C25 C26 C27 -178.43(16) . . . . ? C29 C25 C26 C27 2.9(2) . . . . ? C25 C26 C27 C28 -0.4(2) . . . . ? C29 N22 C28 O2 -173.57(14) . . . . ? C29 N22 C28 C27 5.7(2) . . . . ? C26 C27 C28 O2 175.24(16) . . . . ? C26 C27 C28 N22 -4.0(2) . . . . ? C28 N22 C29 N21 176.32(13) . . . . ? C28 N22 C29 C25 -3.0(2) . . . . ? C22 N21 C29 N22 -178.29(12) . . . . ? Ru1 N21 C29 N22 1.59(17) . . . . ? C22 N21 C29 C25 1.07(19) . . . . ? Ru1 N21 C29 C25 -179.05(10) . . . . ? C24 C25 C29 N22 -179.98(14) . . . . ? C26 C25 C29 N22 -1.3(2) . . . . ? C24 C25 C29 N21 0.7(2) . . . . ? C26 C25 C29 N21 179.35(13) . . . . ? C11 P1 C31 C32 170.14(10) . . . . ? C41 P1 C31 C32 62.91(11) . . . . ? Ru1 P1 C31 C32 -76.05(11) . . . . ? C11 P1 C31 C33 43.12(11) . . . . ? C41 P1 C31 C33 -64.11(11) . . . . ? Ru1 P1 C31 C33 156.93(8) . . . . ? C11 P1 C41 C43 43.18(11) . . . . ? C31 P1 C41 C43 147.86(10) . . . . ? Ru1 P1 C41 C43 -69.43(11) . . . . ? C11 P1 C41 C42 169.03(10) . . . . ? C31 P1 C41 C42 -86.29(11) . . . . ? Ru1 P1 C41 C42 56.42(12) . . . . ? C21 P2 C51 C53 43.91(12) . . . . ? C61 P2 C51 C53 149.40(11) . . . . ? Ru1 P2 C51 C53 -68.02(12) . . . . ? C21 P2 C51 C52 171.45(10) . . . . ? C61 P2 C51 C52 -83.05(11) . . . . ? Ru1 P2 C51 C52 59.52(11) . . . . ? C21 P2 C61 C62 173.10(10) . . . . ? C51 P2 C61 C62 66.51(11) . . . . ? Ru1 P2 C61 C62 -73.89(11) . . . . ? C21 P2 C61 C63 45.51(11) . . . . ? C51 P2 C61 C63 -61.08(11) . . . . ? Ru1 P2 C61 C63 158.51(8) . . . . ?