data_global # 1. SUBMISSION DETAILS #---------------------- _publ_contact_author_name 'Golobic, A' _publ_contact_author_address ; #<< address of contact author Dr. Amalija Golobic Faculty of Chemistry and Chemical Tecnology University of Ljubljana Askerceva 5 1000 Ljubljana Slovenia ; _publ_contact_author_email AMALIJA.GOLOBIC@fkkt.UNI-LJ.SI _publ_contact_author_fax 386012419220 _publ_contact_author_phone 386012419104 _publ_contact_letter ; #<< contact letter Dear Madame or Sir, I would kindly ask you to deposit this CIF file, containing data of three structures, which are reported in the manuscript which will be considered for the publication in the journal .... According to the instructions for Authors for this journal I'm sending you this file prior to the submission of the manuscript to the. The title of the manuscript is: The authors are: Yours Sincerely, Amalija Golobic Ljubljana, January 2011 ; data_compound1 # k357 # 2. EXPERIMENTAL DATA #--------------------- _publ_section_exptl_prep ; ? #<< material & crystal preparation text ; _publ_section_exptl_refinement ; ? #<< crystallographic methods used ; _chemical_formula_sum 'C14 H14 Cl3 N2 O Ru S' _chemical_formula_moiety ? _chemical_formula_weight 465.76 _chemical_melting_point ? _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M p_-1 _symmetry_space_group_name_Hall -p_1 loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,-y,-z _cell_length_a 8.8592(1) _cell_length_b 11.7145(2) _cell_length_c 16.7731(3) _cell_angle_alpha 92.5915(7) _cell_angle_beta 103.1136(7) _cell_angle_gamma 93.3115(7) _cell_volume 1689.46(5) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.831 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 6895 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 27.48 _cell_measurement_temperature 150 _exptl_absorpt_coefficient_mu 1.527 _exptl_crystal_description prism _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_size_rad ? _exptl_crystal_colour red #<< use NfA code _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method '\w scans with \k offsets' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(DENZO-SMN; Otwinovski, Minor 1997)' _exptl_absorpt_correction_T_min 0.474 _exptl_absorpt_correction_T_max 0.808 _diffrn_ambient_temperature 150(2) _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 24614 _reflns_number_total 7691 _reflns_Friedel_coverage ? _reflns_number_gt 6426 _reflns_threshold_expression 'F2 > 2.00 sig(F2 )' _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_av_R_equivalents .031 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? #<< do not append units _diffrn_standards_decay_% ? #<< do not append % _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .03 _refine_ls_wR_factor_ref .03 _refine_ls_goodness_of_fit_ref 1.218 _refine_ls_number_reflns 7201 _refine_ls_number_parameters 397 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .0005 _refine_diff_density_min -.962 _refine_diff_density_max .749 _refine_ls_extinction_method none _refine_ls_extinction_coef .00000 _refine_ls_abs_structure_details none _refine_ls_abs_structure_Flack ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'COLLECT (Nonius, 2000)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'XTAL3.6 (Hall et al., 1999)' _computing_molecular_graphics 'ORTEPIII (Farrugia, 1997)' _computing_publication_material 'XTAL3.6 (Hall et al., 1999) ' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 56 .002 .002 'Int. Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 56 0 0 'Int. Tables Vol IV Tables 2.2B and 2.3.1' Ru ? 0 4 -1.42 .836 'Int. Tables Vol IV Tables 2.2B and 2.3.1' Cl ? 0 12 .132 .159 'Int. Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 4 .008 .006 'Int. Tables Vol IV Tables 2.2B and 2.3.1' S ? 0 4 .11 .124 'Int. Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 8 .004 .003 'Int. Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ru1a .22787(4) .25685(3) -.12051(2) .01545(16) Uani ? ? 1.00000 ? ? Ru1b .32140(4) .30381(3) .36124(2) .01520(16) Uani ? ? 1.00000 ? ? Cl1a .43109(15) .16843(11) -.16251(9) .0274(6) Uani ? ? 1.00000 ? ? Cl2a .03927(14) .15536(11) -.22495(8) .0241(5) Uani ? ? 1.00000 ? ? Cl3a .39669(14) .35816(11) -.00937(7) .0225(5) Uani ? ? 1.00000 ? ? Cl1b .51136(14) .45560(10) .39464(7) .0219(5) Uani ? ? 1.00000 ? ? Cl2b .15224(14) .13800(10) .33994(8) .0232(5) Uani ? ? 1.00000 ? ? Cl3b .20320(14) .38350(11) .23951(7) .0225(5) Uani ? ? 1.00000 ? ? S1a .26495(14) .39954(10) -.20477(7) .0189(5) Uani ? ? 1.00000 ? ? S1b .15032(14) .39724(11) .42239(7) .0185(5) Uani ? ? 1.00000 ? ? O1a .1737(5) .5015(3) -.2029(3) .0292(18) Uani ? ? 1.00000 ? ? O1b .1543(4) .3778(3) .5096(2) .0252(16) Uani ? ? 1.00000 ? ? N1a .0436(5) .3197(4) -.0776(2) .0174(17) Uani ? ? 1.00000 ? ? N2a .2028(5) .1360(4) -.0351(3) .0211(18) Uani ? ? 1.00000 ? ? N1b .4521(5) .2270(4) .4628(3) .0194(17) Uani ? ? 1.00000 ? ? N2b .4736(5) .2153(4) .3063(3) .0200(18) Uani ? ? 1.00000 ? ? C2a -.0446(6) .4035(4) -.1056(3) .020(2) Uani ? ? 1.00000 ? ? C3a -.1613(6) .4393(5) -.0679(3) .023(2) Uani ? ? 1.00000 ? ? C4a -.1851(6) .3892(5) .0003(3) .026(2) Uani ? ? 1.00000 ? ? C5a -.0957(6) .2983(5) .0313(3) .024(2) Uani ? ? 1.00000 ? ? C6a .0158(6) .2645(4) -.0113(3) .020(2) Uani ? ? 1.00000 ? ? C7a -.1090(7) .2402(6) .1029(3) .032(3) Uani ? ? 1.00000 ? ? C8a -.0234(8) .1510(6) .1273(3) .035(3) Uani ? ? 1.00000 ? ? C9a .0844(7) .1104(5) .0819(3) .030(2) Uani ? ? 1.00000 ? ? C10a .1040(6) .1686(4) .0126(3) .022(2) Uani ? ? 1.00000 ? ? C11a .1740(8) .0151(5) .1007(4) .037(3) Uani ? ? 1.00000 ? ? C12a .2707(7) -.0171(5) .0525(4) .037(3) Uani ? ? 1.00000 ? ? C13a .2836(6) .0450(5) -.0160(4) .029(2) Uani ? ? 1.00000 ? ? C14a .4628(7) .4505(5) -.1859(3) .027(2) Uani ? ? 1.00000 ? ? C15a .2343(7) .3454(5) -.3079(3) .028(2) Uani ? ? 1.00000 ? ? C2b .4427(6) .2375(5) .5406(3) .023(2) Uani ? ? 1.00000 ? ? C3b .5424(7) .1842(5) .6029(3) .029(2) Uani ? ? 1.00000 ? ? C4b .6542(7) .1180(5) .5839(4) .030(2) Uani ? ? 1.00000 ? ? C5b .6674(6) .1051(5) .5016(3) .025(2) Uani ? ? 1.00000 ? ? C6b .5639(6) .1622(4) .4434(3) .021(2) Uani ? ? 1.00000 ? ? C7b .7788(6) .0366(5) .4747(4) .032(3) Uani ? ? 1.00000 ? ? C8b .7866(7) .0283(5) .3949(4) .033(3) Uani ? ? 1.00000 ? ? C9b .6859(6) .0889(5) .3345(4) .026(2) Uani ? ? 1.00000 ? ? C10b .5738(6) .1550(4) .3591(3) .019(2) Uani ? ? 1.00000 ? ? C11b .6897(7) .0867(5) .2511(4) .030(2) Uani ? ? 1.00000 ? ? C12b .5881(7) .1478(5) .1987(4) .031(3) Uani ? ? 1.00000 ? ? C13b .4800(6) .2116(5) .2278(3) .025(2) Uani ? ? 1.00000 ? ? C14b -.0452(6) .3656(5) .3679(3) .027(2) Uani ? ? 1.00000 ? ? C15b .1689(7) .5477(5) .4135(4) .028(2) Uani ? ? 1.00000 ? ? H2a -.02219 .44014 -.14712 .01470 Uiso ? ? 1.00000 ? ? H3a -.22938 .48471 -.09011 .02776 Uiso ? ? 1.00000 ? ? H4a -.26567 .39991 .01916 .03829 Uiso ? ? 1.00000 ? ? H7a -.18659 .26468 .12881 .02225 Uiso ? ? 1.00000 ? ? H8a -.03472 .11013 .17678 .04276 Uiso ? ? 1.00000 ? ? H11a .15961 -.02948 .14714 .03154 Uiso ? ? 1.00000 ? ? H12a .31799 -.09179 .06114 .05103 Uiso ? ? 1.00000 ? ? H13a .35018 .01570 -.05881 .03957 Uiso ? ? 1.00000 ? ? H141a .52909 .37307 -.18752 .03115 Uiso ? ? 1.00000 ? ? H142a .46623 .49009 -.22537 .05561 Uiso ? ? 1.00000 ? ? H143a .48596 .47759 -.13768 .04546 Uiso ? ? 1.00000 ? ? H151a .27624 .39801 -.33695 .02566 Uiso ? ? 1.00000 ? ? H152a .30838 .27689 -.30665 .03470 Uiso ? ? 1.00000 ? ? H153a .15242 .31379 -.32868 .04820 Uiso ? ? 1.00000 ? ? H2b .35090 .28042 .55802 .05134 Uiso ? ? 1.00000 ? ? H3b .52593 .19496 .66336 .02538 Uiso ? ? 1.00000 ? ? H4b .72854 .08404 .62881 .03634 Uiso ? ? 1.00000 ? ? H7b .87562 -.00578 .51378 .04475 Uiso ? ? 1.00000 ? ? H8b .86840 -.01221 .38349 .03229 Uiso ? ? 1.00000 ? ? H11b .76792 .04273 .23472 .02695 Uiso ? ? 1.00000 ? ? H12b .60199 .15089 .14429 .04476 Uiso ? ? 1.00000 ? ? H13b .42122 .25149 .19392 .02940 Uiso ? ? 1.00000 ? ? H141b -.06358 .28231 .37659 .03527 Uiso ? ? 1.00000 ? ? H142b -.10984 .39987 .39597 .03527 Uiso ? ? 1.00000 ? ? H143b -.06925 .36725 .31509 .04557 Uiso ? ? 1.00000 ? ? H151b .08077 .58064 .43298 .03800 Uiso ? ? 1.00000 ? ? H152b .25544 .57340 .44919 .02997 Uiso ? ? 1.00000 ? ? H153b .15763 .56365 .36208 .04430 Uiso ? ? 1.00000 ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ru1a .01525(18) .01513(19) .01591(19) .00258(13) .00278(14) .00234(14) Ru1b .01567(19) .0165(2) .01398(18) .00228(13) .00382(14) .00284(13) Cl1a .0232(6) .0244(6) .0357(7) .0105(5) .0071(5) .0001(5) Cl2a .0230(6) .0251(6) .0218(6) -.0024(5) .0015(5) -.0014(5) Cl3a .0198(6) .0245(6) .0210(6) -.0023(4) .0011(4) -.0004(4) Cl1b .0219(6) .0225(6) .0213(6) -.0029(4) .0061(4) .0005(4) Cl2b .0231(6) .0208(6) .0244(6) -.0019(4) .0027(5) .0053(5) Cl3b .0252(6) .0258(6) .0163(5) .0035(5) .0029(4) .0070(4) S1a .0203(6) .0213(6) .0167(5) .0042(4) .0064(4) .0044(4) S1b .0179(5) .0228(6) .0164(5) .0054(4) .0055(4) .0047(4) O1a .034(2) .026(2) .035(2) .0151(16) .0181(17) .0123(16) O1b .0239(18) .038(2) .0158(17) .0089(16) .0069(14) .0077(15) N1a .017(2) .021(2) .0138(18) .0010(15) .0035(15) .0030(15) N2a .018(2) .020(2) .022(2) -.0008(16) -.0033(16) .0055(16) N1b .016(2) .019(2) .023(2) .0026(15) .0048(16) .0030(16) N2b .019(2) .021(2) .021(2) -.0012(16) .0081(16) -.0013(16) C2a .018(2) .021(2) .020(2) .0017(18) .0052(19) .0023(19) C3a .016(2) .025(3) .027(3) .0035(19) .005(2) -.003(2) C4a .018(2) .031(3) .028(3) -.004(2) .010(2) -.008(2) C5a .022(2) .030(3) .020(2) -.011(2) .008(2) -.001(2) C6a .017(2) .024(2) .016(2) -.0056(18) .0017(18) -.0008(18) C7a .036(3) .043(3) .018(3) -.012(3) .011(2) -.002(2) C8a .038(3) .046(4) .017(3) -.019(3) .003(2) .006(2) C9a .032(3) .033(3) .018(2) -.015(2) -.006(2) .008(2) C10a .023(2) .020(2) .019(2) -.0073(19) -.001(2) .0030(19) C11a .037(3) .033(3) .032(3) -.011(3) -.009(3) .018(3) C12a .027(3) .028(3) .046(4) -.006(2) -.013(3) .017(3) C13a .020(2) .020(3) .040(3) .001(2) -.007(2) .011(2) C14a .027(3) .032(3) .023(3) -.007(2) .007(2) .004(2) C15a .028(3) .037(3) .018(2) -.003(2) .006(2) .002(2) C2b .025(3) .025(3) .019(2) .005(2) .004(2) .005(2) C3b .032(3) .034(3) .023(3) .008(2) .004(2) .010(2) C4b .025(3) .034(3) .028(3) .007(2) -.001(2) .014(2) C5b .018(2) .024(3) .032(3) .003(2) .003(2) .007(2) C6b .017(2) .019(2) .027(3) .0022(18) .005(2) .004(2) C7b .018(2) .029(3) .051(4) .006(2) .008(2) .009(3) C8b .022(3) .027(3) .054(4) .007(2) .014(3) .004(3) C9b .019(2) .021(2) .039(3) -.001(2) .012(2) -.003(2) C10b .019(2) .013(2) .027(3) .0001(17) .010(2) .0013(18) C11b .026(3) .024(3) .041(3) -.004(2) .016(2) -.010(2) C12b .031(3) .034(3) .030(3) -.004(2) .014(2) -.008(2) C13b .026(3) .025(3) .023(3) -.003(2) .008(2) -.005(2) C14b .020(2) .037(3) .026(3) .005(2) .006(2) .006(2) C15b .028(3) .027(3) .029(3) .010(2) .008(2) .002(2) # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1A Cl1A 2.3528(14) . . yes Ru1A Cl2A 2.3512(13) . . yes Ru1A Cl3A 2.3346(12) . . yes Ru1A S1A 2.2935(12) . . yes Ru1A N1A 2.086(4) . . yes Ru1A N2A 2.097(5) . . yes Ru1B N2B 2.093(5) . . yes Ru1B Cl3B 2.3350(12) . . yes Ru1B Cl1B 2.3333(13) . . yes Ru1B Cl2B 2.3461(13) . . yes Ru1B S1B 2.3114(13) . . yes Ru1B N1B 2.102(5) . . yes S1A C14A 1.772(6) . . yes S1A O1A 1.484(4) . . yes S1A C15A 1.771(5) . . yes S1B C14B 1.775(5) . . yes S1B C15B 1.777(6) . . yes S1B O1B 1.483(3) . . yes N1A C2A 1.326(7) . . yes N1A C6A 1.374(6) . . yes N2A C10A 1.371(7) . . yes N2A C13A 1.329(7) . . yes N1B C6B 1.369(7) . . yes N1B C2B 1.327(7) . . yes N2B C10B 1.358(7) . . yes N2B C13B 1.330(7) . . yes C2A C3A 1.403(8) . . no C3A C4A 1.361(7) . . no C4A C5A 1.411(8) . . no C5A C6A 1.408(8) . . no C5A C7A 1.431(8) . . no C6A C10A 1.426(7) . . no C7A C8A 1.351(10) . . no C8A C9A 1.438(9) . . no C9A C10A 1.413(7) . . no C9A C11A 1.413(9) . . no C11A C12A 1.362(9) . . no C12A C13A 1.410(9) . . no C2A H2A 0.8880 . . no C3A H3A 0.8594 . . no C4A H4A 0.8570 . . no C7A H7A 0.9437 . . no C8A H8A 0.9981 . . no C11A H11A 0.9848 . . no C12A H12A 0.9942 . . no C13A H13A 1.0838 . . no C14A H141A 1.1113 . . no C14A H143A 0.8312 . . no C14A H142A 0.8304 . . no C15A H153A 0.7921 . . no C15A H152A 1.0637 . . no C15A H151A 0.9155 . . no C2B C3B 1.402(8) . . no C3B C4B 1.376(9) . . no C4B C5B 1.414(8) . . no C5B C6B 1.402(7) . . no C5B C7B 1.443(8) . . no C6B C10B 1.435(7) . . no C7B C8B 1.355(9) . . no C8B C9B 1.433(9) . . no C9B C10B 1.415(8) . . no C9B C11B 1.406(9) . . no C11B C12B 1.367(9) . . no C12B C13B 1.406(8) . . no C2B H2B 1.0683 . . no C3B H3B 1.0599 . . no C4B H4B 0.9958 . . no C7B H7B 1.1115 . . no C8B H8B 0.9389 . . no C11B H11B 0.9674 . . no C12B H12B 0.9501 . . no C13B H13B 0.8546 . . no C14B H141B 1.0025 . . no C14B H142B 0.9179 . . no C14B H143B 0.8642 . . no C15B H151B 1.0022 . . no C15B H152B 0.8863 . . no C15B H153B 0.8754 . . no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1A Ru1A Cl2A 91.97(5) . . . yes Cl1A Ru1A Cl3A 92.93(5) . . . yes Cl1A Ru1A S1A 86.62(5) . . . yes Cl1A Ru1A N1A 174.11(13) . . . yes Cl1A Ru1A N2A 94.74(13) . . . yes Cl2A Ru1A Cl3A 174.42(5) . . . yes Cl2A Ru1A S1A 92.39(4) . . . yes Cl2A Ru1A N1A 86.83(11) . . . yes Cl2A Ru1A N2A 92.18(13) . . . yes Cl3A Ru1A S1A 90.55(4) . . . yes Cl3A Ru1A N1A 88.03(11) . . . yes Cl3A Ru1A N2A 84.77(13) . . . yes S1A Ru1A N1A 99.19(12) . . . yes S1A Ru1A N2A 175.18(14) . . . yes N1A Ru1A N2A 79.56(17) . . . yes Cl1B Ru1B N1B 85.79(13) . . . yes Cl1B Ru1B N2B 88.21(13) . . . yes Cl2B Ru1B Cl3B 95.18(5) . . . yes Cl2B Ru1B S1B 89.61(5) . . . yes Cl2B Ru1B N1B 86.93(13) . . . yes Cl2B Ru1B N2B 89.04(13) . . . yes Cl3B Ru1B S1B 87.22(4) . . . yes Cl3B Ru1B N1B 172.19(13) . . . yes Cl3B Ru1B N2B 93.34(14) . . . yes S1B Ru1B N1B 100.33(13) . . . yes S1B Ru1B N2B 178.58(13) . . . yes N1B Ru1B N2B 79.16(18) . . . yes Cl1B Ru1B Cl3B 91.85(4) . . . yes Cl1B Ru1B S1B 93.08(5) . . . yes Cl1B Ru1B Cl2B 172.59(5) . . . yes Ru1A S1A C15A 111.2(2) . . . yes O1A S1A C14A 106.8(3) . . . yes Ru1A S1A O1A 117.18(19) . . . yes Ru1A S1A C14A 111.64(18) . . . yes C14A S1A C15A 100.4(3) . . . yes O1A S1A C15A 108.3(3) . . . yes Ru1B S1B C14B 111.61(18) . . . yes Ru1B S1B O1B 117.98(16) . . . yes O1B S1B C14B 106.3(2) . . . yes O1B S1B C15B 107.4(3) . . . yes C14B S1B C15B 100.5(3) . . . yes Ru1B S1B C15B 111.5(2) . . . yes Ru1A N1A C2A 128.6(3) . . . yes Ru1A N1A C6A 112.8(3) . . . yes C2A N1A C6A 118.6(4) . . . yes Ru1A N2A C13A 128.3(4) . . . yes C10A N2A C13A 118.9(5) . . . yes Ru1A N2A C10A 112.2(3) . . . yes Ru1B N1B C2B 128.5(4) . . . yes Ru1B N1B C6B 113.0(3) . . . yes C2B N1B C6B 118.4(5) . . . yes Ru1B N2B C10B 113.8(4) . . . yes Ru1B N2B C13B 127.5(4) . . . yes C10B N2B C13B 118.7(5) . . . yes N1A C2A C3A 121.9(5) . . . yes C2A C3A C4A 120.2(5) . . . no C3A C4A C5A 119.8(5) . . . no C4A C5A C6A 116.9(5) . . . no C4A C5A C7A 124.8(5) . . . no C6A C5A C7A 118.4(5) . . . no N1A C6A C5A 122.6(5) . . . yes C5A C6A C10A 120.5(5) . . . no N1A C6A C10A 116.9(5) . . . yes C5A C7A C8A 121.5(5) . . . no C7A C8A C9A 121.1(5) . . . no C10A C9A C11A 116.2(5) . . . no C8A C9A C10A 118.7(5) . . . no C8A C9A C11A 125.1(5) . . . no N2A C10A C9A 123.1(5) . . . yes C6A C10A C9A 119.7(5) . . . no N2A C10A C6A 117.2(4) . . . yes C9A C11A C12A 120.2(6) . . . no C11A C12A C13A 120.4(6) . . . no N2A C13A C12A 121.3(5) . . . yes N1A C2A H2A 117.25 . . . no C3A C2A H2A 120.69 . . . no C2A C3A H3A 122.54 . . . no C4A C3A H3A 116.60 . . . no C3A C4A H4A 122.00 . . . no C5A C4A H4A 116.75 . . . no C8A C7A H7A 122.93 . . . no C5A C7A H7A 115.40 . . . no C9A C8A H8A 117.93 . . . no C7A C8A H8A 120.96 . . . no C9A C11A H11A 118.26 . . . no C12A C11A H11A 121.44 . . . no C11A C12A H12A 118.38 . . . no C13A C12A H12A 120.51 . . . no C12A C13A H13A 121.50 . . . no N2A C13A H13A 116.94 . . . no S1A C14A H141A 105.71 . . . no S1A C14A H142A 103.56 . . . no S1A C14A H143A 105.89 . . . no H142A C14A H143A 122.45 . . . no H141A C14A H142A 111.43 . . . no H141A C14A H143A 106.50 . . . no S1A C15A H153A 117.94 . . . no H151A C15A H152A 102.73 . . . no H151A C15A H153A 118.26 . . . no H152A C15A H153A 101.14 . . . no S1A C15A H151A 108.87 . . . no S1A C15A H152A 105.48 . . . no N1B C2B C3B 122.3(5) . . . yes C2B C3B C4B 119.8(5) . . . no C3B C4B C5B 119.4(5) . . . no C4B C5B C6B 117.0(5) . . . no C4B C5B C7B 124.0(5) . . . no C6B C5B C7B 118.9(5) . . . no N1B C6B C5B 123.1(5) . . . yes N1B C6B C10B 117.1(5) . . . yes C5B C6B C10B 119.8(5) . . . no C5B C7B C8B 121.3(5) . . . no C7B C8B C9B 121.0(6) . . . no C8B C9B C10B 118.8(6) . . . no C8B C9B C11B 124.3(5) . . . no C10B C9B C11B 117.0(5) . . . no N2B C10B C6B 116.9(5) . . . yes N2B C10B C9B 122.9(5) . . . yes C6B C10B C9B 120.2(5) . . . no C9B C11B C12B 119.4(6) . . . no C11B C12B C13B 120.3(6) . . . no N2B C13B C12B 121.7(5) . . . yes N1B C2B H2B 121.18 . . . no C3B C2B H2B 116.28 . . . no C2B C3B H3B 117.86 . . . no C4B C3B H3B 122.34 . . . no C3B C4B H4B 119.37 . . . no C5B C4B H4B 121.12 . . . no C5B C7B H7B 127.30 . . . no C8B C7B H7B 111.01 . . . no C7B C8B H8B 115.70 . . . no C9B C8B H8B 122.93 . . . no C9B C11B H11B 116.75 . . . no C12B C11B H11B 123.83 . . . no C11B C12B H12B 116.69 . . . no C13B C12B H12B 122.70 . . . no N2B C13B H13B 120.35 . . . no C12B C13B H13B 117.89 . . . no S1B C14B H141B 102.83 . . . no S1B C14B H142B 109.04 . . . no S1B C14B H143B 119.81 . . . no H141B C14B H142B 102.80 . . . no H141B C14B H143B 102.67 . . . no H142B C14B H143B 116.86 . . . no S1B C15B H151B 106.87 . . . no S1B C15B H152B 106.40 . . . no S1B C15B H153B 110.66 . . . no H151B C15B H152B 106.75 . . . no H151B C15B H153B 106.84 . . . no H152B C15B H153B 118.72 . . . no #-------------------------------------------------------------------------- # Special items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #-------------------------------------------------------------------------- loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 924 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 11 _reflns_limit_k_min -15 _reflns_limit_k_max 15 _reflns_limit_l_min -21 _reflns_limit_l_max 21 _reflns_number_observed ? _reflns_d_resolution_high .771 _reflns_d_resolution_low 16.306 _diffrn_reflns_av_sigmaI/netI .043 _diffrn_reflns_theta_min 1.25 _diffrn_reflns_reduction_process ? _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .043 _refine_ls_wR_factor_all .056 _refine_ls_goodness_of_fit_all 2.082 _refine_ls_shift/su_mean .000015 data_compound2 # k574 # 2. EXPERIMENTAL DATA #--------------------- _publ_section_exptl_prep ; ? #<< material & crystal preparation text ; _publ_section_exptl_refinement ; ? #<< crystallographic methods used ; _chemical_formula_sum 'C12 H19 Cl4 N2 O5 Ru1' _chemical_formula_moiety ? _chemical_formula_weight 514.16 _chemical_melting_point ? _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P_-1 _symmetry_space_group_name_Hall -p_1 loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,-y,-z _cell_length_a 8.1409(2) _cell_length_b 9.2715(2) _cell_length_c 13.0919(3) _cell_angle_alpha 86.061(1) _cell_angle_beta 77.551(1) _cell_angle_gamma 78.652(1) _cell_volume 945.70(4) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.806 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 3996 _cell_measurement_theta_min 2.04 _cell_measurement_theta_max 27.48 _cell_measurement_temperature 150 _exptl_absorpt_coefficient_mu 1.418 _exptl_crystal_description prism _exptl_crystal_size_max 0.175 _exptl_crystal_size_mid 0.125 _exptl_crystal_size_min 0.10 _exptl_crystal_size_rad ? _exptl_crystal_colour brown _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method '\w scans with \k offsets' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(DENZO-SMN; Otwinovski, Minor 1997)' _exptl_absorpt_correction_T_min 0.714 _exptl_absorpt_correction_T_max 0.868 _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 16369 _reflns_number_total 4297 _reflns_Friedel_coverage 0 _reflns_number_gt 3358 _reflns_threshold_expression 'F2 > 2.00 sig(F2 )' _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_av_R_equivalents .039 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? #<< do not append units _diffrn_standards_decay_% ? #<< do not append % _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .033 _refine_ls_wR_factor_ref .030 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_number_reflns 3939 _refine_ls_number_parameters 217 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .0053 _refine_diff_density_min -.614 _refine_diff_density_max .792 _refine_ls_extinction_method none _refine_ls_extinction_coef .00000 _refine_ls_abs_structure_details none _refine_ls_abs_structure_Flack ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'COLLECT (Nonius, 2000)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'XTAL3.6 (Hall et al., 1999)' _computing_molecular_graphics 'ORTEPIII (Farrugia, 1997)' _computing_publication_material 'XTAL3.6 (Hall et al., 1999) ' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 24 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 38 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Ru ? 0 2 -1.42 .836 'Int Tables Vol IV Tables 2.2B and 2.3.1' Cl ? 0 8 .132 .159 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 10 .008 .006 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 4 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1' Na ? 0 0 .03 .025 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ru .21343(6) .66981(5) .72445(4) .0134(3) Uani ? ? 1.00000 ? ? Cl1 -.06234(19) .79984(16) .79305(11) .0193(10) Uani ? ? 1.00000 ? ? Cl2 .48832(19) .54529(16) .64808(11) .0198(10) Uani ? ? 1.00000 ? ? Cl3 .0915(2) .45887(16) .71254(12) .0216(10) Uani ? ? 1.00000 ? ? Cl4 .2542(2) .58811(17) .89555(11) .0220(10) Uani ? ? 1.00000 ? ? O1W .3671(6) .7260(5) 1.1194(4) .031(4) Uani ? ? 1.00000 ? ? O2W .1001(6) 1.2798(5) .9491(3) .026(3) Uani ? ? 1.00000 ? ? O3W .6949(6) .5400(5) .8226(4) .028(3) Uani ? ? 1.00000 ? ? O4W .6082(6) .7443(5) .9757(4) .029(3) Uani ? ? 1.00000 ? ? N1 .1916(6) .7551(5) .5771(4) .016(3) Uani ? ? 1.00000 ? ? N2 .3021(6) .8620(5) .7275(4) .016(3) Uani ? ? 1.00000 ? ? C2 .1482(8) .6924(7) .5010(5) .021(4) Uani ? ? 1.00000 ? ? C3 .1419(8) .7646(8) .4041(5) .025(5) Uani ? ? 1.00000 ? ? C4 .1794(8) .9033(8) .3862(5) .024(4) Uani ? ? 1.00000 ? ? C5 .2737(9) 1.1156(7) .4550(5) .025(4) Uani ? ? 1.00000 ? ? C6 .3231(8) 1.1721(7) .5331(5) .024(4) Uani ? ? 1.00000 ? ? C7 .3957(8) 1.1380(7) .7115(6) .024(4) Uani ? ? 1.00000 ? ? C8 .4103(9) 1.0466(7) .7968(5) .026(5) Uani ? ? 1.00000 ? ? C9 .3609(8) .9097(7) .8038(5) .021(4) Uani ? ? 1.00000 ? ? C10 .2339(7) .8926(6) .5591(5) .016(4) Uani ? ? 1.00000 ? ? C11 .2276(8) .9716(7) .4645(5) .019(4) Uani ? ? 1.00000 ? ? C12 .2899(7) .9506(6) .6407(5) .016(4) Uani ? ? 1.00000 ? ? C13 .3348(8) 1.0906(6) .6290(5) .019(4) Uani ? ? 1.00000 ? ? H2 .11863 .58945 .51817 .04700 Uiso ? ? 1.00000 ? ? H3 .11022 .71716 .35458 .05600 Uiso ? ? 1.00000 ? ? H4 .17838 .94530 .32324 .05600 Uiso ? ? 1.00000 ? ? H5 .27148 1.16463 .39712 .05700 Uiso ? ? 1.00000 ? ? H6 .35598 1.26173 .52615 .05800 Uiso ? ? 1.00000 ? ? H7 .42434 1.22568 .70295 .05900 Uiso ? ? 1.00000 ? ? H8 .45243 1.07051 .85771 .06100 Uiso ? ? 1.00000 ? ? H9 .35611 .85171 .86693 .05100 Uiso ? ? 1.00000 ? ? H11 .33886 .63157 1.12956 .09600 Uiso ? ? 1.00000 ? ? H12 .25289 .80418 1.10346 .05100 Uiso ? ? 1.00000 ? ? H13 .45847 .73221 1.05953 .04000 Uiso ? ? 1.00000 ? ? H21 .02012 1.31107 .99993 .06700 Uiso ? ? 1.00000 ? ? H22 .10319 1.32948 .90826 .05900 Uiso ? ? 1.00000 ? ? H31 .80035 .53693 .78968 .06200 Uiso ? ? 1.00000 ? ? H32 .64076 .55761 .77191 .08000 Uiso ? ? 1.00000 ? ? H41 .63141 .68464 .93202 .09500 Uiso ? ? 1.00000 ? ? H42 .70270 .74120 .99743 .06400 Uiso ? ? 1.00000 ? ? O5W1 -.1101(11) 1.0843(10) .9277(9) .036(3) Uiso ? ? .63(3) ? ? O5W2 -.0819(19) 1.1167(16) .8691(15) .035(6) Uiso ? ? .37(3) ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ru .0131(3) .0120(3) .0152(3) -.00307(17) -.00259(18) -.00030(16) Cl1 .0163(8) .0184(7) .0210(7) -.0008(6) -.0013(6) -.0015(6) Cl2 .0153(8) .0210(7) .0213(7) -.0007(6) -.0014(6) -.0018(6) Cl3 .0196(8) .0160(7) .0295(8) -.0063(6) -.0020(6) -.0029(6) Cl4 .0229(8) .0239(8) .0179(7) -.0027(6) -.0040(6) .0034(6) O1W .028(3) .035(3) .033(3) -.011(2) -.001(2) -.009(2) O2W .027(3) .028(2) .022(2) -.008(2) -.002(2) .0015(18) O3W .018(2) .036(3) .030(3) -.008(2) -.004(2) -.005(2) O4W .028(3) .032(3) .028(2) -.007(2) -.007(2) -.002(2) N1 .012(3) .016(2) .019(3) -.001(2) -.001(2) .000(2) N2 .013(3) .016(2) .017(2) -.002(2) -.002(2) -.001(2) C2 .017(3) .026(3) .022(3) -.005(3) -.006(3) -.006(3) C3 .019(3) .035(4) .019(3) .000(3) -.004(3) -.006(3) C4 .018(3) .034(4) .015(3) .003(3) -.001(3) .003(3) C5 .019(3) .022(3) .026(3) .002(3) .003(3) .010(3) C6 .018(3) .015(3) .033(4) -.002(3) .006(3) .001(3) C7 .015(3) .016(3) .040(4) -.004(2) .003(3) -.010(3) C8 .023(4) .027(4) .032(4) -.004(3) -.008(3) -.011(3) C9 .021(3) .024(3) .020(3) -.006(3) -.006(3) -.004(2) C10 .010(3) .018(3) .017(3) -.001(2) .000(2) -.001(2) C11 .011(3) .021(3) .019(3) .004(2) .002(2) .002(2) C12 .009(3) .016(3) .021(3) -.000(2) -.000(2) .000(2) C13 .010(3) .014(3) .031(3) -.003(2) .003(3) -.004(2) # 5. Molecular Geometry #---------------------- # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru Cl1 2.3483(16) . . yes Ru Cl2 2.3490(16) . . yes Ru Cl3 2.3890(16) . . yes Ru Cl4 2.3854(15) . . yes Ru N1 2.064(5) . . yes Ru N2 2.056(5) . . yes O5W2 H12 1.4225 . 2_577 no O1W H11 0.9419 . . no O1W H13 0.9645 . . no O2W H22 0.6809 . . no O2W H21 0.8463 . . no O3W H31 0.8695 . . no O3W H32 0.8627 . . no N1 C10 1.377(7) . . yes N1 C2 1.330(8) . . yes N2 C9 1.331(8) . . yes N2 C12 1.365(8) . . yes O4W H42 0.8707 . . no O4W H41 0.7902 . . no C2 C3 1.399(9) . . no C3 C4 1.373(10) . . no C4 C11 1.402(9) . . no C5 C11 1.447(9) . . no C5 C6 1.347(9) . . no C6 C13 1.432(9) . . no C7 C13 1.410(10) . . no C7 C8 1.366(10) . . no C8 C9 1.397(9) . . no C10 C12 1.423(9) . . no C10 C11 1.400(9) . . no C12 C13 1.406(8) . . no C2 H2 1.0282 . . no C3 H3 0.9144 . . no C4 H4 0.8881 . . no C5 H5 0.8582 . . no C6 H6 0.9150 . . no C7 H7 0.8824 . . no C8 H8 0.9873 . . no C9 H9 0.9524 . . no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1 Ru Cl2 177.28(5) . . . yes Cl1 Ru Cl3 88.89(6) . . . yes Cl1 Ru Cl4 91.17(5) . . . yes Cl1 Ru N1 89.81(14) . . . yes Cl1 Ru N2 87.85(14) . . . yes Cl2 Ru Cl3 91.61(6) . . . yes Cl2 Ru Cl4 91.51(5) . . . yes Cl2 Ru N1 87.48(14) . . . yes Cl2 Ru N2 91.46(14) . . . yes Cl3 Ru Cl4 89.60(6) . . . yes Cl3 Ru N1 95.66(14) . . . yes Cl3 Ru N2 174.78(15) . . . yes Cl4 Ru N1 174.67(14) . . . yes Cl4 Ru N2 94.54(15) . . . yes N1 Ru N2 80.26(19) . . . yes H11 O1W H13 112.56 . . . no H21 O2W H22 111.07 . . . no H31 O3W H32 101.72 . . . no Ru N1 C2 128.2(4) . . . yes Ru N1 C10 112.7(4) . . . yes C2 N1 C10 119.1(5) . . . yes Ru N2 C9 128.1(4) . . . yes Ru N2 C12 113.4(4) . . . yes C9 N2 C12 118.5(5) . . . yes H41 O4W H42 105.09 . . . no N1 C2 C3 121.2(6) . . . yes C2 C3 C4 120.2(6) . . . no C3 C4 C11 119.9(6) . . . no C6 C5 C11 121.9(6) . . . no C5 C6 C13 121.2(6) . . . no C8 C7 C13 119.2(6) . . . no C7 C8 C9 120.6(6) . . . no N2 C9 C8 121.8(6) . . . yes C11 C10 C12 120.7(5) . . . no N1 C10 C12 116.8(5) . . . yes N1 C10 C11 122.5(6) . . . yes C4 C11 C10 117.1(6) . . . no C5 C11 C10 117.5(6) . . . no C4 C11 C5 125.4(6) . . . no N2 C12 C10 116.6(5) . . . yes N2 C12 C13 122.9(6) . . . yes C10 C12 C13 120.5(6) . . . no C6 C13 C12 118.3(6) . . . no C7 C13 C12 117.2(6) . . . no C6 C13 C7 124.5(6) . . . no N1 C2 H2 116.07 . . . no C3 C2 H2 122.69 . . . no C4 C3 H3 121.94 . . . no C2 C3 H3 117.86 . . . no C11 C4 H4 121.60 . . . no C3 C4 H4 118.40 . . . no C11 C5 H5 118.32 . . . no C6 C5 H5 119.81 . . . no C5 C6 H6 121.79 . . . no C13 C6 H6 116.97 . . . no C8 C7 H7 124.56 . . . no C13 C7 H7 116.28 . . . no C9 C8 H8 114.87 . . . no C7 C8 H8 124.55 . . . no N2 C9 H9 117.23 . . . no C8 C9 H9 120.66 . . . no _exptl_crystal_F_000 514 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 7 _reflns_limit_k_min -8 _reflns_limit_k_max 8 _reflns_limit_l_min -12 _reflns_limit_l_max 12 _reflns_number_observed ? _reflns_d_resolution_high .77 _reflns_d_resolution_low 9.087 _diffrn_reflns_av_sigmaI/netI .054 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 150 _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .058 _refine_ls_wR_factor_all .067 _refine_ls_goodness_of_fit_all 2.145 _refine_ls_shift/su_mean .0002 data_compound3 # k588 # 2. EXPERIMENTAL DATA #--------------------- _publ_section_exptl_prep ; ? #<< material & crystal preparation text ; _publ_section_exptl_refinement ; ? #<< crystallographic methods used ; _chemical_formula_sum 'C42 H48 Cl2 N6 O6 Ru1' _chemical_formula_moiety ? _chemical_formula_weight 904.858 _chemical_melting_point ? _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P_b_c_a _symmetry_space_group_name_Hall -p_2ac_2ab loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z 1/2-x,-y,1/2+z 1/2+x,1/2-y,-z -x,1/2+y,1/2-z -x,-y,-z 1/2+x,+y,1/2-z 1/2-x,1/2+y,+z +x,1/2-y,1/2+z _cell_length_a 18.5607(3) _cell_length_b 18.6235(3) _cell_length_c 23.7095(5) _cell_angle_alpha 90.00000 _cell_angle_beta 90.00000 _cell_angle_gamma 90.00000 _cell_volume 8195.5(3) _cell_formula_units_Z 8 _exptl_crystal_density_diffrn 1.466 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 8491 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 25.68 _cell_measurement_temperature 150 _exptl_absorpt_coefficient_mu .568 _exptl_crystal_description PRISM _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_size_rad ? _exptl_crystal_colour RED _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method '\w scans with \k offsets' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(DENZO-SMN; Otwinovski, Minor 1997)' _exptl_absorpt_correction_T_min 0.779 _exptl_absorpt_correction_T_max 0.893 _diffrn_ambient_temperature 150(2) _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 63674 # No. of integrated reflections _reflns_number_total 7780 _reflns_Friedel_coverage 0 _reflns_number_gt 3675 _reflns_threshold_expression 'F2 > 2.00 sig(F2 )' _diffrn_reflns_theta_max 25.68 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_av_R_equivalents .1 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? #<< do not append units _diffrn_standards_decay_% ? #<< do not append % _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .068 _refine_ls_wR_factor_ref .045 _refine_ls_goodness_of_fit_ref 1.1 _refine_ls_number_reflns 6147 _refine_ls_number_parameters 454 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .002 _refine_diff_density_min -3.293 # riple close to Ru _refine_diff_density_max 1.857 _refine_ls_extinction_method none _refine_ls_extinction_coef .00000 _refine_ls_abs_structure_details none _refine_ls_abs_structure_Flack ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'COLLECT (Nonius, 2000)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'XTAL3.6 (Hall et al., 1999)' _computing_molecular_graphics 'ORTEPIII (Farrugia, 1997)' _computing_publication_material 'XTAL3.6 (Hall et al., 1999) ' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 336 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 384 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 48 .008 .006 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 48 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1' Ru ? 0 8 -1.42 .836 'Int Tables Vol IV Tables 2.2B and 2.3.1' Cl ? 0 16 .132 .159 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ru .79634(4) .41169(5) .37553(4) .0191(4) Uani ? ? 1.00000 ? ? Cl1 .89448(15) .27686(15) .56915(11) .0326(16) Uani ? ? 1.00000 ? ? Cl2 .88453(15) .5854(2) .17762(13) .0457(17) Uani ? ? 1.00000 ? ? O1M .6012(6) .3747(6) .1676(5) .072(3) Uiso ? ? 1.00000 ? ? O2M .7214(5) .5512(5) .2022(4) .052(2) Uiso ? ? 1.00000 ? ? O3M .6545(6) .2401(6) .2084(5) .078(3) Uiso ? ? 1.00000 ? ? O4M .7254(10) .6252(11) .4677(8) .144(6) Uiso ? ? 1.00000 ? ? O5M .6029(9) .3806(9) .5483(7) .120(5) Uiso ? ? 1.00000 ? ? O6M .7468(9) .2433(9) .5264(7) .112(5) Uiso ? ? 1.00000 ? ? N1A .8761(4) .4883(4) .3683(4) .020(5) Uani ? ? 1.00000 ? ? N1B .7102(5) .4802(4) .3618(3) .021(5) Uani ? ? 1.00000 ? ? N1C .8056(4) .3809(4) .2921(3) .019(4) Uani ? ? 1.00000 ? ? N10A .8031(5) .4445(4) .4590(4) .024(5) Uani ? ? 1.00000 ? ? N10B .7122(5) .3415(4) .3898(3) .019(5) Uani ? ? 1.00000 ? ? N10C .8764(5) .3351(5) .3824(4) .023(5) Uani ? ? 1.00000 ? ? C2A .9098(6) .5120(6) .3217(5) .025(6) Uani ? ? 1.00000 ? ? C2B .7099(7) .5497(6) .3472(5) .031(6) Uani ? ? 1.00000 ? ? C2C .7694(5) .4057(6) .2479(5) .025(6) Uani ? ? 1.00000 ? ? C3A .9661(7) .5603(6) .3240(5) .031(7) Uani ? ? 1.00000 ? ? C3B .6467(6) .5877(7) .3381(5) .033(6) Uani ? ? 1.00000 ? ? C3C .7827(6) .3817(6) .1926(5) .029(6) Uani ? ? 1.00000 ? ? C4A .9894(5) .5867(7) .3747(6) .025(5) Uani ? ? 1.00000 ? ? C4B .5810(6) .5550(6) .3427(5) .031(7) Uani ? ? 1.00000 ? ? C4C .8366(7) .3316(6) .1832(5) .032(6) Uani ? ? 1.00000 ? ? C5A .9707(6) .5934(6) .4793(5) .028(6) Uani ? ? 1.00000 ? ? C5B .5131(6) .4419(7) .3657(6) .033(7) Uani ? ? 1.00000 ? ? C5C .9344(7) .2553(7) .2241(5) .034(8) Uani ? ? 1.00000 ? ? C6A .9322(6) .5727(6) .5251(5) .028(7) Uani ? ? 1.00000 ? ? C6B .5150(6) .3724(7) .3826(5) .034(7) Uani ? ? 1.00000 ? ? C6C .9710(5) .2327(6) .2693(5) .024(6) Uani ? ? 1.00000 ? ? C7A .8314(6) .4998(6) .5669(5) .029(6) Uani ? ? 1.00000 ? ? C7B .5852(6) .2635(6) .4098(6) .036(7) Uani ? ? 1.00000 ? ? C7C .9876(6) .2338(6) .3755(6) .028(6) Uani ? ? 1.00000 ? ? C8A .7775(6) .4527(7) .5571(4) .029(6) Uani ? ? 1.00000 ? ? C8B .6518(7) .2339(6) .4169(5) .035(7) Uani ? ? 1.00000 ? ? C8C .9641(7) .2598(6) .4258(5) .024(7) Uani ? ? 1.00000 ? ? C9A .7646(5) .4249(5) .5045(5) .024(6) Uani ? ? 1.00000 ? ? C9B .7136(6) .2739(6) .4065(5) .033(6) Uani ? ? 1.00000 ? ? C9C .9089(6) .3096(6) .4288(5) .025(6) Uani ? ? 1.00000 ? ? C11A .8582(6) .4935(5) .4671(4) .021(6) Uani ? ? 1.00000 ? ? C11B .6437(5) .4467(6) .3676(5) .024(6) Uani ? ? 1.00000 ? ? C11C .8589(5) .3311(5) .2825(4) .017(5) Uani ? ? 1.00000 ? ? C12A .8740(5) .5216(6) .5209(5) .025(6) Uani ? ? 1.00000 ? ? C12B .5786(6) .4815(6) .3580(5) .029(7) Uani ? ? 1.00000 ? ? C12C .8767(5) .3061(5) .2288(4) .021(6) Uani ? ? 1.00000 ? ? C13A .8978(5) .5161(5) .4196(5) .018(6) Uani ? ? 1.00000 ? ? C13B .6459(6) .3717(6) .3829(5) .025(6) Uani ? ? 1.00000 ? ? C13C .8980(5) .3073(5) .3306(4) .017(6) Uani ? ? 1.00000 ? ? C14A .9541(6) .5656(5) .4242(5) .021(6) Uani ? ? 1.00000 ? ? C14B .5810(6) .3354(6) .3920(5) .028(7) Uani ? ? 1.00000 ? ? C14C .9532(6) .2574(6) .3249(5) .023(7) Uani ? ? 1.00000 ? ? C1M .5736(7) .4057(8) .2174(6) .045(3) Uiso ? ? 1.00000 ? ? C2M .6826(7) .6162(7) .1959(6) .047(3) Uiso ? ? 1.00000 ? ? C3M .6706(9) .2308(9) .2679(7) .066(4) Uiso ? ? 1.00000 ? ? C4M .6630(10) .5946(12) .4916(8) .086(5) Uiso ? ? 1.00000 ? ? C5M .5546(13) .4262(13) .5278(10) .108(8) Uiso ? ? 1.00000 ? ? C6M .6950(11) .2408(11) .5728(8) .091(6) Uiso ? ? 1.00000 ? ? H2A .89490 .49710 .28650 .03400 Uiso ? ? 1.00000 ? ? H2B .75341 .57330 .34320 .04100 Uiso ? ? 1.00000 ? ? H2C .73230 .43900 .25310 .03400 Uiso ? ? 1.00000 ? ? H3A .98900 .57470 .29071 .03700 Uiso ? ? 1.00000 ? ? H3B .64910 .63500 .32981 .04400 Uiso ? ? 1.00000 ? ? H3C .75521 .39930 .16260 .04000 Uiso ? ? 1.00000 ? ? H4A 1.02900 .61830 .37561 .03200 Uiso ? ? 1.00000 ? ? H4B .53990 .58000 .33641 .04300 Uiso ? ? 1.00000 ? ? H4C .84510 .31690 .14660 .03800 Uiso ? ? 1.00000 ? ? H5A 1.00780 .62620 .48301 .03700 Uiso ? ? 1.00000 ? ? H5B .46940 .46290 .36020 .04100 Uiso ? ? 1.00000 ? ? H5C .94720 .23720 .18790 .04100 Uiso ? ? 1.00000 ? ? H6A .94430 .59170 .56000 .04100 Uiso ? ? 1.00000 ? ? H6B .47150 .34760 .38790 .04200 Uiso ? ? 1.00000 ? ? H6C 1.00901 .20160 .26440 .03300 Uiso ? ? 1.00000 ? ? H7A .84011 .51600 .60360 .03900 Uiso ? ? 1.00000 ? ? H7B .54351 .23650 .41650 .04300 Uiso ? ? 1.00000 ? ? H7C 1.02550 .20160 .37450 .03500 Uiso ? ? 1.00000 ? ? H8A .74961 .43699 .58751 .04400 Uiso ? ? 1.00000 ? ? H8B .65610 .18620 .42920 .04600 Uiso ? ? 1.00000 ? ? H8C .98640 .24380 .45930 .03200 Uiso ? ? 1.00000 ? ? H9A .72850 .39000 .50020 .03600 Uiso ? ? 1.00000 ? ? H9B .75701 .25000 .40911 .04600 Uiso ? ? 1.00000 ? ? H9C .89321 .32510 .46400 .03400 Uiso ? ? 1.00000 ? ? H1M1 .59050 .45360 .22030 .07900 Uiso ? ? 1.00000 ? ? H1M2 .52201 .40460 .21640 .07900 Uiso ? ? 1.00000 ? ? H1M3 .59040 .37780 .24890 .07900 Uiso ? ? 1.00000 ? ? H2M1 .68899 .62960 .15490 .08000 Uiso ? ? 1.00000 ? ? H2M2 .69939 .65100 .21830 .08000 Uiso ? ? 1.00000 ? ? H2M3 .63280 .60460 .20021 .08000 Uiso ? ? 1.00000 ? ? H3M1 .63260 .24880 .29180 .15100 Uiso ? ? 1.00000 ? ? H3M2 .67109 .17640 .27650 .15100 Uiso ? ? 1.00000 ? ? H3M3 .71560 .24780 .27960 .15100 Uiso ? ? 1.00000 ? ? H4M1 .62641 .63331 .49951 .09000 Uiso ? ? 1.00000 ? ? H4M2 .64012 .55893 .46512 .09000 Uiso ? ? 1.00000 ? ? H4M3 .67391 .56956 .52816 .09000 Uiso ? ? 1.00000 ? ? H5M1 .57050 .46980 .51520 .20800 Uiso ? ? 1.00000 ? ? H5M2 .51419 .43600 .55670 .20800 Uiso ? ? 1.00000 ? ? H5M3 .52560 .40250 .49670 .20800 Uiso ? ? 1.00000 ? ? H6M1 .68660 .19600 .58631 .14500 Uiso ? ? 1.00000 ? ? H6M2 .65140 .26410 .55890 .14500 Uiso ? ? 1.00000 ? ? H6M3 .71390 .27280 .60290 .14500 Uiso ? ? 1.00000 ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ru .0205(4) .0174(4) .0193(4) -.0006(5) .0018(5) -.0010(5) Cl1 .0349(15) .0344(16) .0285(16) -.0086(14) -.0005(13) .0060(14) Cl2 .0347(15) .0443(16) .058(2) .0039(17) .0086(14) -.0057(19) N1A .023(5) .014(4) .022(5) -.001(4) -.004(4) -.002(4) N1B .022(5) .021(4) .019(5) .007(4) .003(4) -.003(3) N1C .025(5) .015(4) .019(5) -.005(4) .003(4) -.002(3) N10A .020(5) .023(4) .029(5) -.002(5) .004(4) -.003(4) N10B .020(5) .015(4) .023(5) -.003(4) .002(4) -.003(3) N10C .013(4) .024(5) .030(6) -.000(4) .004(5) -.001(5) C2A .026(6) .029(6) .019(6) -.001(5) .003(5) .004(5) C2B .034(7) .028(6) .030(6) .002(6) -.001(6) .002(5) C2C .030(6) .021(5) .025(6) -.003(5) .002(5) .001(6) C3A .032(7) .021(6) .040(8) -.006(5) .005(6) .000(6) C3B .043(7) .025(6) .031(6) .014(7) .011(5) .004(6) C3C .028(6) .034(6) .026(6) .005(5) -.003(5) .002(5) C4A .020(5) .024(5) .032(6) -.006(6) .001(6) .001(7) C4B .028(7) .027(6) .038(7) .008(5) .004(5) .003(5) C4C .050(7) .032(6) .014(6) -.002(6) -.001(5) -.002(5) C5A .031(6) .015(5) .038(7) -.001(6) -.014(5) -.006(6) C5B .011(6) .042(8) .044(9) .005(5) -.008(6) -.009(7) C5C .035(7) .041(8) .025(8) -.005(6) -.001(6) -.003(6) C6A .030(6) .028(7) .026(7) -.001(5) -.003(5) -.001(5) C6B .020(6) .049(8) .034(7) -.002(6) .002(6) -.002(7) C6C .014(5) .025(5) .032(7) -.004(5) .007(5) -.002(5) C7A .038(7) .035(7) .016(6) -.001(6) -.007(5) -.004(5) C7B .029(7) .027(7) .051(8) -.008(6) .009(6) -.005(6) C7C .029(6) .010(5) .044(8) .000(5) -.002(7) -.002(7) C8A .036(7) .037(6) .014(6) .009(6) .013(5) .001(5) C8B .036(7) .023(6) .046(8) -.005(6) .011(6) .008(6) C8C .029(7) .026(7) .017(7) .003(5) -.002(6) .003(5) C9A .023(5) .020(6) .030(7) -.000(5) .005(5) .006(5) C9B .025(6) .022(6) .052(7) -.001(6) .012(6) .006(6) C9C .027(6) .027(6) .022(6) -.000(5) -.002(5) .003(5) C11A .027(6) .019(6) .018(6) .009(5) .005(5) -.006(4) C11B .022(6) .031(6) .018(6) .001(5) .002(5) -.007(5) C11C .017(5) .013(5) .022(6) .002(4) .003(5) .000(4) C12A .022(6) .026(6) .028(7) .007(5) -.001(5) -.002(5) C12B .033(7) .029(6) .025(7) .006(5) .001(5) -.002(5) C12C .026(6) .013(5) .024(6) .002(5) -.001(5) -.005(5) C13A .014(5) .010(5) .031(7) .002(5) .001(5) .004(5) C13B .031(6) .024(6) .019(6) -.004(6) -.005(5) -.011(5) C13C .014(5) .014(5) .023(6) -.003(5) .002(5) -.002(5) C14A .014(5) .019(6) .031(7) .002(4) -.001(5) -.005(5) C14B .022(6) .030(7) .032(7) -.001(5) .001(5) -.007(5) C14C .024(7) .023(6) .021(7) -.004(5) .003(6) -.001(5) # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru N1A 2.063(8) . . yes Ru N1B 2.071(9) . . yes Ru N1C 2.067(7) . . yes Ru N10A 2.075(9) . . yes Ru N10B 2.065(9) . . yes Ru N10C 2.066(9) . . yes O1M C1M 1.411(18) . . yes O2M C2M 1.416(16) . . yes O3M C3M 1.45(2) . . yes O4M C4M 1.41(3) . . yes N1A C13A 1.382(15) . . yes N1A C2A 1.344(15) . . yes N1B C2B 1.340(13) . . yes N1B C11B 1.390(13) . . yes N1C C11C 1.375(12) . . yes N1C C2C 1.328(13) . . yes O5M C5M 1.33(3) . . yes N10A C9A 1.345(14) . . yes N10A C11A 1.384(13) . . yes N10B C9B 1.320(13) . . yes N10B C13B 1.363(14) . . yes N10C C9C 1.342(15) . . yes N10C C13C 1.392(13) . . yes O6M C6M 1.46(3) . . yes C2A C3A 1.380(17) . . no C2B C3B 1.387(17) . . no C2C C3C 1.407(17) . . no C3A C4A 1.369(18) . . no C3B C4B 1.367(16) . . no C3C C4C 1.386(17) . . no C4A C14A 1.400(18) . . no C4B C12B 1.417(16) . . no C4C C12C 1.396(15) . . no C5A C6A 1.356(16) . . no C5A C14A 1.439(16) . . no C5B C6B 1.355(18) . . no C5B C12B 1.434(16) . . no C5C C6C 1.337(17) . . no C5C C12C 1.433(16) . . no C6A C12A 1.443(15) . . no C6B C14B 1.423(16) . . no C6C C14C 1.435(17) . . no C7A C12A 1.407(16) . . no C7A C8A 1.351(16) . . no C7B C14B 1.406(16) . . no C7B C8B 1.364(17) . . no C7C C8C 1.359(18) . . no C7C C14C 1.428(18) . . no C8A C9A 1.371(15) . . no C8B C9B 1.390(17) . . no C8C C9C 1.384(17) . . no C11A C12A 1.410(15) . . no C11A C13A 1.409(15) . . no C11B C12B 1.390(15) . . no C11B C13B 1.444(16) . . no C11C C13C 1.423(13) . . no C11C C12C 1.395(13) . . no C13A C14A 1.398(14) . . no C13B C14B 1.398(16) . . no C13C C14C 1.390(15) . . no C2A H2A 0.9220 . . no C2B H2B 0.9243 . . no C2C H2C 0.9349 . . no C3A H3A 0.9357 . . no C3B H3B 0.9037 . . no C3C H3C 0.9347 . . no C4A H4A 0.9418 . . no C4B H4B 0.9061 . . no C4C H4C 0.9235 . . no C5A H5A 0.9247 . . no C5B H5B 0.9099 . . no C5C H5C 0.9522 . . no C6A H6A 0.9275 . . no C6B H6B 0.9386 . . no C6C H6C 0.9201 . . no C7A H7A 0.9350 . . no C7B H7B 0.9364 . . no C7C H7C 0.9247 . . no C8A H8A 0.9346 . . no C8B H8B 0.9384 . . no C8C H8C 0.9439 . . no C9A H9A 0.9390 . . no C9B H9B 0.9226 . . no C9C H9C 0.9299 . . no C1M H1M3 0.9618 . . no C1M H1M2 0.9581 . . no C1M H1M1 0.9481 . . no C2M H2M3 0.9547 . . no C2M H2M1 1.0106 . . no C2M H2M2 0.8940 . . no C3M H3M3 0.9353 . . no C3M H3M2 1.0335 . . no C3M H3M1 0.9648 . . no C4M H4M2 1.0079 . . no C4M H4M3 1.0049 . . no C4M H4M1 1.0080 . . no C5M H5M2 1.0322 . . no C5M H5M3 1.0140 . . no C5M H5M1 0.9141 . . no C6M H6M1 0.9072 . . no C6M H6M2 0.9756 . . no C6M H6M3 0.9937 . . no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1A Ru N1B 96.6(3) . . . yes N1A Ru N1C 93.0(3) . . . yes N1A Ru N10A 80.3(4) . . . yes N1A Ru N10B 173.9(3) . . . yes N1A Ru N10C 88.2(3) . . . yes N1B Ru N1C 94.9(3) . . . yes N1B Ru N10A 90.9(3) . . . yes N1B Ru N10B 80.3(3) . . . yes N1B Ru N10C 173.1(3) . . . yes N1C Ru N10A 171.7(3) . . . yes N1C Ru N10B 92.5(3) . . . yes N1C Ru N10C 79.9(3) . . . yes N10A Ru N10B 94.4(3) . . . yes N10A Ru N10C 94.9(4) . . . yes N10B Ru N10C 95.4(3) . . . yes Ru N1A C2A 129.0(7) . . . yes Ru N1A C13A 113.3(7) . . . yes C2A N1A C13A 117.7(8) . . . yes Ru N1B C2B 129.7(8) . . . yes Ru N1B C11B 113.2(6) . . . yes C2B N1B C11B 117.1(10) . . . yes Ru N1C C2C 128.1(7) . . . yes Ru N1C C11C 113.9(6) . . . yes C2C N1C C11C 117.9(8) . . . yes Ru N10A C9A 130.8(7) . . . yes Ru N10A C11A 111.8(7) . . . yes C9A N10A C11A 117.4(9) . . . yes Ru N10B C9B 129.7(8) . . . yes Ru N10B C13B 113.7(6) . . . yes C9B N10B C13B 116.6(9) . . . yes Ru N10C C9C 129.2(8) . . . yes Ru N10C C13C 113.2(7) . . . yes C9C N10C C13C 117.5(9) . . . yes N1A C2A C3A 122.3(11) . . . yes N1B C2B C3B 122.5(11) . . . yes N1C C2C C3C 122.4(9) . . . yes C2A C3A C4A 120.5(11) . . . no C2B C3B C4B 121.0(12) . . . no C2C C3C C4C 119.4(10) . . . no C3A C4A C14A 119.2(10) . . . no C3B C4B C12B 118.6(11) . . . no C3C C4C C12C 119.3(10) . . . no C6A C5A C14A 120.8(10) . . . no C6B C5B C12B 120.5(11) . . . no C6C C5C C12C 121.7(11) . . . no C5A C6A C12A 121.8(11) . . . no C5B C6B C14B 122.1(11) . . . no C5C C6C C14C 121.2(10) . . . no C8A C7A C12A 118.1(10) . . . no C8B C7B C14B 118.2(10) . . . no C8C C7C C14C 118.9(10) . . . no C7A C8A C9A 122.1(10) . . . no C7B C8B C9B 120.6(11) . . . no C7C C8C C9C 121.4(11) . . . no N10A C9A C8A 122.3(9) . . . yes N10B C9B C8B 123.2(10) . . . yes N10C C9C C8C 121.9(11) . . . yes N10A C11A C12A 121.6(9) . . . yes N10A C11A C13A 118.1(9) . . . yes C12A C11A C13A 120.3(9) . . . no N1B C11B C12B 123.1(10) . . . yes N1B C11B C13B 115.7(9) . . . yes C12B C11B C13B 121.1(9) . . . no N1C C11C C12C 123.1(8) . . . yes N1C C11C C13C 116.4(8) . . . yes C12C C11C C13C 120.5(8) . . . no C6A C12A C7A 123.9(11) . . . no C6A C12A C11A 117.6(10) . . . no C7A C12A C11A 118.5(10) . . . no C4B C12B C5B 123.8(10) . . . no C4B C12B C11B 117.7(10) . . . no C5B C12B C11B 118.5(10) . . . no C4C C12C C5C 124.3(10) . . . no C4C C12C C11C 117.8(9) . . . no C5C C12C C11C 117.9(9) . . . no N1A C13A C11A 116.1(8) . . . yes N1A C13A C14A 122.3(10) . . . yes C11A C13A C14A 121.6(10) . . . no N10B C13B C11B 117.1(9) . . . yes N10B C13B C14B 124.1(10) . . . yes C11B C13B C14B 118.8(10) . . . no N10C C13C C11C 116.4(8) . . . yes N10C C13C C14C 123.2(9) . . . yes C11C C13C C14C 120.4(9) . . . no C4A C14A C5A 124.1(10) . . . no C4A C14A C13A 118.0(11) . . . no C5A C14A C13A 117.9(10) . . . no C6B C14B C7B 123.8(10) . . . no C6B C14B C13B 118.9(10) . . . no C7B C14B C13B 117.3(10) . . . no C6C C14C C7C 124.8(10) . . . no C6C C14C C13C 118.3(10) . . . no C7C C14C C13C 117.0(10) . . . no N1A C2A H2A 120.37 . . . no C3A C2A H2A 117.33 . . . no N1B C2B H2B 118.83 . . . no C3B C2B H2B 118.71 . . . no N1C C2C H2C 119.96 . . . no C3C C2C H2C 117.57 . . . no C2A C3A H3A 119.83 . . . no C4A C3A H3A 119.62 . . . no C2B C3B H3B 119.31 . . . no C4B C3B H3B 119.70 . . . no C2C C3C H3C 120.13 . . . no C4C C3C H3C 120.51 . . . no C3A C4A H4A 119.41 . . . no C14A C4A H4A 121.42 . . . no C3B C4B H4B 120.59 . . . no C12B C4B H4B 120.81 . . . no C3C C4C H4C 118.29 . . . no C12C C4C H4C 122.40 . . . no C6A C5A H5A 120.27 . . . no C14A C5A H5A 118.92 . . . no C6B C5B H5B 118.43 . . . no C12B C5B H5B 121.10 . . . no C6C C5C H5C 118.97 . . . no C12C C5C H5C 119.35 . . . no C5A C6A H6A 118.58 . . . no C12A C6A H6A 119.63 . . . no C5B C6B H6B 119.15 . . . no C14B C6B H6B 118.77 . . . no C5C C6C H6C 119.12 . . . no C14C C6C H6C 119.63 . . . no C8A C7A H7A 119.85 . . . no C12A C7A H7A 122.08 . . . no C8B C7B H7B 120.73 . . . no C14B C7B H7B 121.10 . . . no C8C C7C H7C 119.85 . . . no C14C C7C H7C 121.20 . . . no C7A C8A H8A 118.74 . . . no C9A C8A H8A 119.12 . . . no C7B C8B H8B 119.87 . . . no C9B C8B H8B 119.50 . . . no C7C C8C H8C 119.03 . . . no C9C C8C H8C 119.54 . . . no N10A C9A H9A 118.69 . . . no C8A C9A H9A 118.99 . . . no N10B C9B H9B 119.83 . . . no C8B C9B H9B 116.76 . . . no N10C C9C H9C 119.03 . . . no C8C C9C H9C 119.08 . . . no O1M C1M H1M1 109.00 . . . no O1M C1M H1M2 109.48 . . . no O1M C1M H1M3 108.13 . . . no H1M1 C1M H1M2 110.65 . . . no H1M1 C1M H1M3 110.17 . . . no H1M2 C1M H1M3 109.37 . . . no O2M C2M H2M1 104.64 . . . no O2M C2M H2M2 112.31 . . . no O2M C2M H2M3 106.71 . . . no H2M1 C2M H2M2 110.58 . . . no H2M1 C2M H2M3 105.81 . . . no H2M2 C2M H2M3 115.97 . . . no O3M C3M H3M1 112.25 . . . no O3M C3M H3M2 108.08 . . . no O3M C3M H3M3 115.56 . . . no H3M1 C3M H3M2 103.36 . . . no H3M1 C3M H3M3 111.16 . . . no H3M2 C3M H3M3 105.39 . . . no O4M C4M H4M1 109.83 . . . no O4M C4M H4M2 111.24 . . . no O4M C4M H4M3 111.64 . . . no H4M1 C4M H4M2 107.66 . . . no H4M1 C4M H4M3 107.89 . . . no H4M2 C4M H4M3 108.44 . . . no O5M C5M H5M1 118.04 . . . no O5M C5M H5M2 111.16 . . . no O5M C5M H5M3 110.27 . . . no H5M1 C5M H5M2 107.13 . . . no H5M1 C5M H5M3 108.68 . . . no H5M2 C5M H5M3 100.02 . . . no O6M C6M H6M1 114.08 . . . no O6M C6M H6M2 106.09 . . . no O6M C6M H6M3 106.81 . . . no H6M1 C6M H6M2 112.69 . . . no H6M1 C6M H6M3 111.02 . . . no H6M2 C6M H6M3 105.59 . . . no _exptl_crystal_F_000 3672 _reflns_limit_h_min 0 _reflns_limit_h_max 22 _reflns_limit_k_min 0 _reflns_limit_k_max 22 _reflns_limit_l_min 0 _reflns_limit_l_max 28 _reflns_number_observed ? _reflns_d_resolution_high .82 _reflns_d_resolution_low 11.855 _diffrn_reflns_av_sigmaI/netI .166 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_reduction_process ? _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .197 _refine_ls_wR_factor_all .085 _refine_ls_goodness_of_fit_all 1.369 _refine_ls_shift/su_mean .0002