#------------------------------------------------------------------------------ #$Date: 2021-11-05 02:01:28 +0200 (Fri, 05 Nov 2021) $ #$Revision: 270312 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/86/7708699.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_7708699 loop_ _publ_author_name 'Lahiri, Goutam Kumar' 'Bera, Sudip Kumar' _publ_section_title ; Structural and electronic forms of doubly oxido/Pz and triply oxido/(Pz)2 bridged mixed valent and isovalent diruthenium complexes (Pz=Pyrazolate) ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D1DT03076K _journal_year 2021 _chemical_formula_moiety 'C23 H31 N2 O9 Ru2' _chemical_formula_sum 'C23 H31 N2 O9 Ru2' _chemical_formula_weight 681.64 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2021-07-03 _audit_creation_method ; Olex2 1.3 (compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272) ; _audit_update_record ; 2021-07-25 deposited with the CCDC. 2021-11-04 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 109.249(2) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 30.4609(5) _cell_length_b 8.14030(10) _cell_length_c 23.6002(4) _cell_measurement_reflns_used 8446 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 72.5830 _cell_measurement_theta_min 3.0520 _cell_volume 5524.77(16) _computing_cell_refinement 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_collection 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' _diffrn_ambient_temperature 293(2) _diffrn_detector 'CCD plate' _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -191.00 -11.00 1.00 1.00 -- -101.00 0.00 108.00 180 2 \w -122.00 -8.00 1.00 1.00 -- -32.00 -72.00 -36.00 114 3 \w -135.00 -13.00 1.00 1.00 -- -101.00 72.00 108.00 122 4 \w -135.00 -15.00 1.00 1.00 -- -101.00 72.00-180.00 120 5 \w -53.00 35.00 1.00 1.00 -- -32.00 0.00 108.00 88 6 \w -96.00 -17.00 1.00 1.00 -- -101.00 72.00-108.00 79 7 \w -44.00 -14.00 1.00 1.00 -- -101.00 72.00 -36.00 30 8 \w -191.00-161.00 1.00 1.00 -- -101.00 -72.00-108.00 30 9 \w -191.00-125.00 1.00 1.00 -- -101.00 -72.00 36.00 66 10 \w -97.00 -67.00 1.00 1.00 -- -101.00 -72.00 -36.00 30 11 \w -135.00-105.00 1.00 1.00 -- -101.00 72.00 36.00 30 12 \w -191.00 -58.00 1.00 1.00 -- -101.00 0.00-180.00 133 13 \w -191.00 -69.00 1.00 1.00 -- -101.00 -72.00-180.00 122 14 \w -96.00 -48.00 1.00 1.00 -- -32.00 0.00 36.00 48 ; _diffrn_measurement_device 'abstract diffractometer' _diffrn_measurement_device_type 'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0440007000 _diffrn_orient_matrix_UB_12 -0.0853562000 _diffrn_orient_matrix_UB_13 0.0415569000 _diffrn_orient_matrix_UB_21 -0.0191558000 _diffrn_orient_matrix_UB_22 0.0134989000 _diffrn_orient_matrix_UB_23 0.0526511000 _diffrn_orient_matrix_UB_31 -0.0237923000 _diffrn_orient_matrix_UB_32 -0.1683433000 _diffrn_orient_matrix_UB_33 -0.0168243000 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.1051 _diffrn_reflns_av_unetI/netI 0.0750 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_number 20899 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_theta_full 64.997 _diffrn_reflns_theta_max 64.997 _diffrn_reflns_theta_min 3.073 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_source_type 'Enhance (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 9.292 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.21744 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_density_diffrn 1.639 _exptl_crystal_description block _exptl_crystal_F_000 2744 _exptl_crystal_size_max 0.365 _exptl_crystal_size_mid 0.325 _exptl_crystal_size_min 0.102 _refine_diff_density_max 1.859 _refine_diff_density_min -0.965 _refine_diff_density_rms 0.226 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 333 _refine_ls_number_reflns 4693 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.092 _refine_ls_R_factor_all 0.0692 _refine_ls_R_factor_gt 0.0572 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0972P)^2^+9.3906P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1478 _refine_ls_wR_factor_ref 0.1622 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3976 _reflns_number_total 4693 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1dt03076k2.cif _cod_data_source_block 1a _cod_database_code 7708699 _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. ; _reflns_odcompleteness_completeness 97.55 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 72.66 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2.a Aromatic/amide H refined with riding coordinates: C13(H13), C3(H3), C8(H8), C22(H22), C23(H23), C18(H18), C21(H21) 2.b Idealised Me refined as rotating group: C10(H10A,H10B,H10C), C1(H1A,H1B,H1C), C20(H20A,H20B,H20C), C11(H11A,H11B, H11C), C15(H15A,H15B,H15C), C6(H6A,H6B,H6C), C5(H5A,H5B,H5C), C16(H16A,H16B, H16C) ; _smtbx_masks_void_probe_radius 1.2 _smtbx_masks_void_truncation_radius 1.2 _shelx_res_file ; TITL gkl-sb-p2_cu_a.res in C2/c gkl-sb-p2_cu.res created by SHELXL-2018/3 at 12:10:41 on 03-Jul-2021 REM Old TITL GKL-SB-P2_Cu in C2/c REM SHELXT solution in C2/c REM R1 0.139, Rweak 0.004, Alpha 0.057, Orientation as input REM Formula found by SHELXT: C44 N5 O20 I4 CELL 1.54184 30.4609 8.1403 23.6002 90 109.249 90 ZERR 8 0.0005 0.0001 0.0004 0 0.002 0 LATT 7 SYMM -X,+Y,0.5-Z SFAC C H N O Ru UNIT 184 248 16 72 16 L.S. 100 0 0 PLAN 6 CONF list 4 ABIN MORE -1 BOND $H fmap 2 53 acta OMIT -3 130 OMIT -8 0 4 OMIT 3 3 0 OMIT -3 3 1 OMIT -5 3 1 OMIT -5 3 2 OMIT 3 1 0 OMIT -8 0 6 OMIT -5 1 1 OMIT -9 1 6 REM REM REM WGHT 0.097200 9.390600 FVAR 0.08973 RU1 5 0.325140 0.369551 0.671661 11.00000 0.02230 0.02136 = 0.01852 -0.00015 0.00908 -0.00270 RU2 5 0.394754 0.255462 0.593411 11.00000 0.02022 0.02017 = 0.02297 0.00072 0.00994 -0.00253 O5 4 0.297545 0.141631 0.666987 11.00000 0.02763 0.02410 = 0.02427 -0.00257 0.00891 -0.00637 O4 4 0.265340 0.469195 0.675616 11.00000 0.02775 0.02263 = 0.03245 -0.00116 0.01558 0.00151 O2 4 0.348439 0.602803 0.675891 11.00000 0.02067 0.02814 = 0.02320 -0.00249 0.00894 -0.00404 O1 4 0.377689 0.281100 0.660844 11.00000 0.02314 0.02722 = 0.02610 0.00035 0.00797 -0.00392 O7 4 0.457360 0.150084 0.639503 11.00000 0.02524 0.02772 = 0.03625 0.00580 0.01146 0.00690 O3 4 0.348149 0.340772 0.763392 11.00000 0.03174 0.03451 = 0.01992 0.00496 0.01070 0.00082 O8 4 0.412755 0.234592 0.517814 11.00000 0.03119 0.03554 = 0.02684 0.00204 0.01556 -0.00322 O9 4 0.366407 0.029199 0.579060 11.00000 0.02502 0.02195 = 0.03002 -0.00359 0.01397 -0.00472 O6 4 0.421530 0.483715 0.601869 11.00000 0.02016 0.02619 = 0.03133 0.00146 0.00911 -0.00317 N2 3 0.330525 0.350100 0.548439 11.00000 0.01949 0.02634 = 0.02121 -0.00129 0.00793 -0.00297 N1 3 0.302684 0.396218 0.580299 11.00000 0.02279 0.02355 = 0.01707 -0.00158 0.00924 0.00034 C10 1 0.246456 -0.074551 0.667460 11.00000 0.03794 0.02481 = 0.04306 -0.00088 0.01905 -0.01461 AFIX 137 H10A 2 0.221372 -0.096881 0.631075 11.00000 -1.50000 H10B 2 0.237289 -0.103993 0.701332 11.00000 -1.50000 H10C 2 0.273226 -0.137656 0.668043 11.00000 -1.50000 AFIX 0 C14 1 0.493113 0.234972 0.666625 11.00000 0.02064 0.03391 = 0.02995 0.00040 0.01232 0.00334 C17 1 0.412047 0.101142 0.489919 11.00000 0.03481 0.04345 = 0.02365 0.00429 0.01364 0.00933 C7 1 0.229035 0.388838 0.675431 11.00000 0.03408 0.03845 = 0.01756 -0.00254 0.01361 -0.00010 C9 1 0.258296 0.107274 0.670514 11.00000 0.03175 0.03333 = 0.01614 -0.00351 0.00858 -0.00604 C13 1 0.496831 0.403885 0.667048 11.00000 0.01922 0.04309 = 0.04478 0.00017 0.01215 -0.00318 AFIX 43 H13 2 0.525025 0.447442 0.691164 11.00000 -1.20000 AFIX 0 C3 1 0.381924 0.607695 0.782646 11.00000 0.02181 0.03772 = 0.01822 -0.00736 0.00526 -0.00016 AFIX 43 H3 2 0.399068 0.674698 0.814072 11.00000 -1.20000 AFIX 0 C1 1 0.383069 0.847181 0.717827 11.00000 0.02943 0.03301 = 0.03661 -0.00775 0.01695 -0.00927 AFIX 137 H1A 2 0.408481 0.848606 0.702265 11.00000 -1.50000 H1B 2 0.392159 0.902003 0.755965 11.00000 -1.50000 H1C 2 0.356811 0.902588 0.690356 11.00000 -1.50000 AFIX 0 C4 1 0.370801 0.450538 0.798713 11.00000 0.02218 0.04428 = 0.02418 -0.00664 0.01151 -0.00140 C8 1 0.224868 0.218797 0.674887 11.00000 0.03061 0.03386 = 0.04149 -0.00747 0.02057 -0.01058 AFIX 43 H8 2 0.197381 0.175710 0.677684 11.00000 -1.20000 AFIX 0 C2 1 0.370347 0.674852 0.725382 11.00000 0.01582 0.03420 = 0.02516 -0.00611 0.01033 -0.00213 C20 1 0.343062 -0.228716 0.537456 11.00000 0.05569 0.02464 = 0.04199 0.00125 0.00329 -0.00220 AFIX 137 H20A 2 0.346563 -0.262383 0.577697 11.00000 -1.50000 H20B 2 0.355411 -0.312113 0.518200 11.00000 -1.50000 H20C 2 0.310688 -0.212633 0.515453 11.00000 -1.50000 AFIX 0 C19 1 0.368618 -0.072528 0.539030 11.00000 0.03317 0.02819 = 0.02746 0.00351 0.00286 0.00755 C11 1 0.474554 0.697157 0.638501 11.00000 0.02656 0.03309 = 0.08171 -0.01234 0.01893 -0.01078 AFIX 137 H11A 2 0.488115 0.723714 0.608248 11.00000 -1.50000 H11B 2 0.496194 0.722936 0.677378 11.00000 -1.50000 H11C 2 0.446608 0.759884 0.631802 11.00000 -1.50000 AFIX 0 C22 1 0.264635 0.445422 0.484366 11.00000 0.03006 0.03074 = 0.02055 0.00486 0.00522 0.00166 AFIX 43 H22 2 0.241899 0.477306 0.448917 11.00000 -1.20000 AFIX 0 C15 1 0.535081 0.135097 0.700146 11.00000 0.02662 0.03929 = 0.04989 0.00488 0.01520 0.00980 AFIX 137 H15A 2 0.525880 0.046260 0.720521 11.00000 -1.50000 H15B 2 0.557086 0.203542 0.728961 11.00000 -1.50000 H15C 2 0.549113 0.091632 0.672389 11.00000 -1.50000 AFIX 0 C23 1 0.307399 0.379862 0.491076 11.00000 0.03155 0.02955 = 0.02079 -0.00501 0.01524 -0.00515 AFIX 43 H23 2 0.318718 0.358996 0.459687 11.00000 -1.20000 AFIX 0 C6 1 0.188633 0.493850 0.674155 11.00000 0.03424 0.04424 = 0.04332 -0.00312 0.02208 0.00644 AFIX 137 H6A 2 0.198296 0.573765 0.705766 11.00000 -1.50000 H6B 2 0.164519 0.426440 0.679727 11.00000 -1.50000 H6C 2 0.177062 0.548979 0.636152 11.00000 -1.50000 AFIX 0 C12 1 0.463203 0.517165 0.635491 11.00000 0.02391 0.02463 = 0.03309 -0.00573 0.01250 -0.00349 C5 1 0.386752 0.404431 0.864030 11.00000 0.04434 0.05617 = 0.02166 -0.00297 0.00714 -0.00812 AFIX 137 H5A 2 0.374583 0.481689 0.885772 11.00000 -1.50000 H5B 2 0.420112 0.405918 0.879620 11.00000 -1.50000 H5C 2 0.375748 0.296238 0.868416 11.00000 -1.50000 AFIX 0 C16 1 0.435344 0.108153 0.441536 11.00000 0.08818 0.06150 = 0.04418 0.00610 0.04672 0.01563 AFIX 137 H16A 2 0.419704 0.187633 0.411646 11.00000 -1.50000 H16B 2 0.433577 0.002095 0.423126 11.00000 -1.50000 H16C 2 0.467356 0.139123 0.459505 11.00000 -1.50000 AFIX 0 C18 1 0.391250 -0.043425 0.497741 11.00000 0.06388 0.03611 = 0.03146 -0.00329 0.01730 0.00379 AFIX 43 H18 2 0.392512 -0.130422 0.472782 11.00000 -1.20000 AFIX 0 C21 1 0.262730 0.453765 0.542249 11.00000 0.02427 0.02276 = 0.03030 -0.00016 0.00742 -0.00179 AFIX 43 H21 2 0.237800 0.492890 0.552803 11.00000 -1.20000 AFIX 0 HKLF 4 REM gkl-sb-p2_cu_a.res in C2/c REM wR2 = 0.1622, GooF = S = 1.092, Restrained GooF = 1.092 for all data REM R1 = 0.0572 for 3976 Fo > 4sig(Fo) and 0.0692 for all 4693 data REM 333 parameters refined using 0 restraints END WGHT 0.0971 9.3875 REM Highest difference peak 1.859, deepest hole -0.965, 1-sigma level 0.226 Q1 1 0.3420 0.3604 0.6384 11.00000 0.05 1.86 Q2 1 0.3593 0.4159 0.6739 11.00000 0.05 1.27 Q3 1 0.3848 0.2583 0.6324 11.00000 0.05 1.20 Q4 1 0.4135 0.2435 0.5576 11.00000 0.05 1.16 Q5 1 0.3631 0.2292 0.5794 11.00000 0.05 1.13 Q6 1 0.2949 0.3166 0.6623 11.00000 0.05 1.06 ; _shelx_res_checksum 20731 _shelx_hkl_file ; 0 0 -1 0.06 0.11 0 0 1 0.02 0.12 0 0 1 0.00 0.17 0 0 2 107.70 3.89 0 0 -2 98.40 4.32 0 0 -2 104.06 5.57 0 0 2 115.05 7.51 0 0 2 97.07 5.56 0 0 -3 0.89 0.64 0 0 3 0.93 0.36 0 0 3 -0.13 0.58 0 0 3 0.58 0.28 0 0 -3 0.78 0.74 0 0 4 1164.46 33.27 0 0 -4 1139.43 20.08 0 0 -5 1.11 0.82 0 0 -5 -0.19 0.40 0 0 5 0.02 1.37 0 0 -6 3010.27 56.52 0 0 6 3050.32 79.24 0 0 7 1.55 2.03 0 0 -7 1.14 1.33 0 0 8 1276.76 58.76 0 0 -8 1344.31 45.48 0 0 9 -5.09 5.31 0 0 -9 0.81 1.40 0 0 10 161.18 22.74 0 0 -10 118.29 13.04 0 0 11 -0.28 3.74 0 0 12 2718.40 113.44 0 0 13 -4.24 4.35 0 0 -14 605.47 34.94 0 0 14 522.07 46.98 0 0 14 688.63 56.29 0 0 15 1.16 5.32 0 0 -15 1.92 2.75 0 0 15 5.04 6.82 0 0 16 273.34 37.15 0 0 -16 316.57 26.04 0 0 16 294.43 36.62 0 0 -17 2.15 2.60 0 0 17 4.32 5.91 0 0 17 -5.00 6.74 0 0 18 161.77 29.05 0 0 18 154.08 30.00 0 0 -18 217.98 22.38 0 0 -18 146.07 15.36 0 0 -19 -1.99 2.86 0 0 -19 -1.25 1.48 0 0 19 4.99 7.20 0 0 -20 81.18 11.22 0 0 20 82.01 20.69 0 0 20 69.06 18.29 0 0 21 -0.45 5.32 0 0 -21 0.19 2.16 0 0 21 4.66 6.88 0 0 22 306.54 38.69 0 0 -22 255.51 19.03 0 0 22 254.02 34.57 0 0 23 -2.34 4.62 0 0 -23 -1.05 1.47 0 0 23 5.33 4.02 0 0 24 184.07 26.37 0 0 24 235.91 29.90 0 0 -24 168.29 12.94 0 0 25 0.36 2.66 0 0 25 -1.62 3.32 0 0 26 415.92 33.07 0 0 26 403.23 31.95 0 2 0 233.54 10.40 0 -2 1 884.01 24.59 0 2 1 918.85 22.98 0 2 2 4.94 1.17 0 -2 2 2.09 1.13 0 2 2 2.20 0.72 0 -2 -3 74.21 6.35 0 2 3 86.81 5.05 0 -2 3 92.23 8.10 0 2 4 286.43 10.23 0 -2 -4 268.68 13.80 0 -2 4 287.91 16.64 0 -2 -5 19.72 3.58 0 2 5 17.79 2.24 0 -2 5 16.46 4.24 0 2 6 428.35 14.29 0 -2 6 459.54 26.31 0 -2 -6 486.04 21.63 0 2 7 464.10 16.09 0 -2 7 528.72 31.18 0 2 7 589.84 34.05 0 -2 -7 529.21 23.91 0 -2 8 11.41 4.75 0 2 8 14.16 5.63 0 2 8 12.70 2.54 0 -2 -8 19.63 4.54 0 2 9 54.32 12.03 0 2 9 38.00 4.90 0 -2 -9 54.59 8.28 0 -2 9 41.35 9.74 0 -2 -10 70.86 9.77 0 -2 10 59.04 12.87 0 2 10 57.16 5.82 0 2 10 75.47 14.96 0 -2 11 211.42 26.26 0 2 11 307.80 33.20 0 -2 -11 275.20 20.82 0 2 12 229.20 31.08 0 -2 12 137.70 22.52 0 -2 13 266.21 33.11 0 -2 13 207.86 30.11 0 -2 -13 270.51 27.74 0 -2 -13 228.47 18.09 0 2 -13 293.84 23.96 0 -2 13 269.13 33.11 0 -2 -14 39.98 9.99 0 -2 14 46.41 15.34 0 -2 14 25.52 11.29 0 2 -14 42.40 9.07 0 2 14 50.73 14.79 0 -2 14 28.45 12.27 0 2 -15 140.86 17.63 0 -2 -15 140.83 19.82 0 2 15 86.12 19.98 0 -2 -15 118.95 14.57 0 2 15 153.71 26.16 0 -2 15 128.43 25.72 0 -2 15 93.94 20.24 0 2 -16 352.58 29.26 0 -2 16 257.74 38.20 0 2 16 267.73 36.22 0 -2 -16 355.94 32.11 0 -2 -16 345.17 26.29 0 2 16 277.94 36.24 0 -2 16 300.29 39.49 0 -2 -17 97.03 13.64 0 2 17 79.54 19.63 0 -2 17 129.86 26.23 0 -2 -17 129.29 18.88 0 -2 17 55.33 17.76 0 -2 -17 98.23 13.35 0 -2 18 24.68 12.46 0 2 18 11.42 5.72 0 -2 -18 17.40 5.56 0 -2 18 11.36 7.96 0 -2 -18 20.40 6.37 0 -2 19 76.18 20.46 0 -2 -19 81.66 12.48 0 2 19 44.98 15.18 0 -2 19 54.45 16.13 0 2 20 22.81 9.32 0 -2 20 40.26 15.50 0 -2 20 18.71 9.12 0 -2 -20 45.88 9.02 0 2 20 30.44 11.66 0 -2 21 54.80 16.67 0 -2 21 49.67 15.17 0 2 21 36.53 12.04 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17 -1.82 1.57 -36 0 16 28.31 4.92 -36 0 15 2.86 1.82 -36 0 14 14.58 3.78 -36 0 13 1.00 1.33 -36 0 12 8.77 3.13 -36 0 11 0.36 0.25 -36 0 10 109.95 11.27 -36 0 9 -3.76 2.16 -36 0 8 182.09 13.79 -36 0 6 45.31 6.53 -36 0 5 0.34 0.79 -36 0 4 128.83 11.21 -36 0 3 1.21 1.39 -36 2 15 10.10 2.79 -36 2 14 7.17 2.49 36 -2 -14 9.79 3.27 -36 2 13 -0.18 0.78 -36 -2 13 0.02 0.55 36 -2 -13 0.17 1.53 36 -2 -12 19.75 5.39 36 -2 -11 19.24 5.42 36 -2 -10 1.99 1.38 36 -2 -9 42.75 8.33 36 -2 -8 70.87 10.74 36 -2 -7 8.38 3.84 TITL GKL-SB-P2_Cu in C2/c REM C2/c (#15 in standard setting) CELL 1.54184 30.460852 8.140295 23.600177 90.0000 109.2489 90.0000 ZERR 24.00 0.000458 0.000133 0.000422 0.0000 0.0018 0.0000 LATT 7 SYMM -x, y,-z+1/2 SFAC C H N O UNIT 264.00 240.00 24.00 24.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 46244 _shelx_fab_file ; -35 1 5 2.2918 0.7129 -35 1 6 0.8857 0.0446 -35 1 7 2.9387 0.4900 -35 1 8 0.5649 0.2193 -35 1 9 2.1030 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0.1939 21 1 14 0.9515 -0.3660 21 1 15 0.3693 0.4309 21 3 0 -1.3185 0.1990 21 3 1 0.5166 0.0217 21 3 2 -0.5557 0.0398 21 3 3 0.4533 0.0957 21 3 4 0.3234 -0.0242 21 3 5 -0.0584 0.1002 21 3 6 0.7413 0.0356 21 3 7 -0.2762 -0.0383 21 3 8 0.7021 0.1593 21 3 9 0.1460 -0.2266 21 3 10 0.6067 0.2719 21 3 11 0.9075 -0.3088 21 3 12 0.8171 0.3486 21 3 13 1.3683 -0.2666 21 3 14 1.3358 0.4060 21 5 0 0.2500 0.2152 21 5 1 -0.1997 -0.1213 21 5 2 1.6207 0.0528 21 5 3 -0.8864 -0.0729 21 5 4 2.6711 -0.2306 21 5 5 -0.9002 0.2134 21 5 6 2.2877 -0.3108 21 5 7 -0.2742 0.5712 21 5 8 0.6916 -0.0619 21 5 9 0.4059 0.7402 21 5 10 -0.7984 0.3153 21 7 0 1.2065 0.6050 21 7 1 -3.7837 -0.3224 21 7 2 1.1910 0.6734 21 7 3 -2.6360 -0.1594 22 0 0 2.0928 -0.3299 22 0 2 1.3299 -0.4484 22 0 4 1.0028 -0.3848 22 0 6 1.0936 -0.1666 22 0 8 1.2925 0.0211 22 0 10 1.2614 0.0394 22 0 12 0.8685 -0.0550 22 0 14 0.2692 -0.0835 22 2 0 0.2313 -0.1423 22 2 1 -3.2029 0.2710 22 2 2 0.4933 -0.1731 22 2 3 -2.8642 0.2456 22 2 4 0.8443 -0.0627 22 2 5 -2.4179 0.3590 22 2 6 0.8077 0.0791 22 2 7 -1.6916 0.4497 22 2 8 0.4852 0.0979 22 2 9 -0.8480 0.3268 22 2 10 0.4887 -0.0210 22 2 11 -0.3414 0.0373 22 2 12 1.1438 -0.1228 22 2 13 -0.4057 -0.1496 22 2 14 1.9852 -0.0684 22 4 0 0.1859 0.3811 22 4 1 1.5811 -0.0965 22 4 2 1.1058 0.2034 22 4 3 1.5736 -0.0379 22 4 4 1.7160 -0.1051 22 4 5 1.8524 0.0532 22 4 6 1.3798 -0.1422 22 4 7 2.1794 0.0999 22 4 8 0.3991 0.2805 22 4 9 2.1216 0.0968 22 4 10 -0.4260 0.8828 22 4 11 1.6977 0.0834 22 6 0 -0.6991 0.3444 22 6 1 -1.7385 -0.3650 22 6 2 -0.8025 0.3347 22 6 3 -1.6015 -0.0993 22 6 4 -0.5202 0.1782 22 6 5 -1.2139 0.2813 22 6 6 -0.0405 0.0258 23 1 0 2.6922 0.0262 23 1 1 -3.0980 0.1814 23 1 2 2.3872 -0.0599 23 1 3 -2.0989 0.1597 23 1 4 2.2087 -0.0587 23 1 5 -1.2462 0.2645 23 1 6 1.9326 0.0874 23 1 7 -0.5805 0.3417 23 1 8 1.5174 0.2463 23 1 9 -0.1426 0.2673 23 1 10 1.1495 0.2034 23 1 11 0.1091 0.1307 23 1 12 0.8903 -0.0858 23 1 13 0.3255 0.1384 23 1 14 0.5570 -0.3950 23 3 0 -2.3651 0.1264 23 3 1 1.3255 0.2236 23 3 2 -1.4052 -0.0081 23 3 3 0.5151 0.2372 23 3 4 -0.1757 -0.0291 23 3 5 -0.2076 0.1654 23 3 6 0.5950 0.0925 23 3 7 -0.4258 -0.0152 23 3 8 0.7734 0.2800 23 3 9 -0.2575 -0.1652 23 3 10 0.7422 0.4301 23 3 11 -0.1300 -0.1512 23 3 12 0.9261 0.4972 23 5 0 -0.9631 0.2280 23 5 1 0.1681 -0.2189 23 5 2 0.6175 0.0998 23 5 3 -0.4529 -0.0781 23 5 4 1.5250 -0.1064 23 5 5 -0.5321 0.3269 23 5 6 0.9703 -0.0762 23 5 7 -0.1775 0.7288 23 5 8 -0.3875 0.2451 23 7 0 1.6075 0.6864 24 0 0 2.7303 0.1116 24 0 2 3.0437 -0.0328 24 0 4 3.5987 -0.0195 24 0 6 3.6074 0.1309 24 0 8 2.7535 0.2427 24 0 10 1.3564 0.1875 24 0 12 0.0177 0.0230 24 2 0 1.0273 0.0056 24 2 1 -2.8902 0.2309 24 2 2 1.4424 -0.0125 24 2 3 -3.5135 0.2033 24 2 4 1.5718 0.0910 24 2 5 -3.6144 0.2999 24 2 6 1.2800 0.1983 24 2 7 -2.9368 0.3407 24 2 8 0.8797 0.1677 24 2 9 -1.8759 0.2019 24 2 10 0.8285 0.0080 24 2 11 -1.1170 -0.0050 24 2 12 1.1560 -0.1256 24 4 0 -2.1046 0.2371 24 4 1 2.0617 -0.2002 24 4 2 -0.4190 0.0892 24 4 3 1.9317 -0.0979 24 4 4 0.8041 -0.1046 24 4 5 1.9000 0.0491 24 4 6 0.7949 0.0490 24 4 7 1.5924 0.1378 24 4 8 0.0055 0.6179 24 4 9 0.8636 0.1502 24 6 0 -0.5291 0.3899 24 6 1 -1.3563 -0.2577 24 6 2 -0.6373 0.3602 24 6 3 -1.1845 0.0506 24 6 4 -0.3789 0.1885 25 1 0 3.9674 0.3382 25 1 1 -3.1126 -0.0558 25 1 2 4.0109 0.1685 25 1 3 -2.7847 -0.0510 25 1 4 3.6988 0.1402 25 1 5 -2.5373 0.0388 25 1 6 2.8247 0.2998 25 1 7 -1.9987 0.0574 25 1 8 1.6422 0.4603 25 1 9 -1.0638 -0.0570 25 1 10 0.6071 0.3832 25 1 11 0.0229 -0.1672 25 1 12 -0.0977 0.0527 25 3 0 -2.3018 -0.0326 25 3 1 0.1006 0.0765 25 3 2 -0.9177 -0.0957 25 3 3 -0.8399 0.0776 25 3 4 0.4809 -0.0465 25 3 5 -1.2148 0.0010 25 3 6 1.1069 0.1287 25 3 7 -1.0917 -0.1318 25 3 8 0.9335 0.3338 25 3 9 -0.9068 -0.1607 25 3 10 0.5297 0.4528 25 5 0 -1.9463 0.2576 25 5 1 0.9729 -0.2997 25 5 2 -0.2145 0.1507 25 5 3 0.3933 -0.1031 25 5 4 0.6671 0.0056 25 5 5 0.1478 0.3419 25 5 6 0.3027 0.0958 26 0 0 3.8519 0.3790 26 0 2 4.2466 0.1822 26 0 4 4.3967 0.1230 26 0 6 3.4818 0.1987 26 0 8 1.6882 0.2545 26 0 10 -0.0989 0.1755 26 2 0 2.2486 0.0662 26 2 1 -4.1506 -0.2159 26 2 2 2.5145 0.0464 26 2 3 -4.9318 -0.1614 26 2 4 2.1901 0.1328 26 2 5 -4.6832 -0.0292 26 2 6 1.4413 0.2166 26 2 7 -3.3644 0.0060 26 2 8 0.6864 0.1786 26 2 9 -1.7189 -0.0958 26 2 10 0.2549 0.0399 26 4 0 -2.4081 0.1363 26 4 1 1.4997 -0.3456 26 4 2 -0.2304 0.0274 26 4 3 1.5729 -0.2001 26 4 4 1.0858 -0.0636 26 4 5 1.5164 -0.0125 26 4 6 0.9564 0.1972 26 4 7 0.9836 0.0994 26 6 0 -0.5272 0.4336 27 1 0 4.2894 0.2062 27 1 1 -3.5128 -0.3900 27 1 2 4.0791 -0.0213 27 1 3 -3.3797 -0.3147 27 1 4 3.2478 -0.0276 27 1 5 -3.0741 -0.2219 27 1 6 1.8633 0.2053 27 1 7 -2.0757 -0.2436 27 1 8 0.4544 0.4413 27 1 9 -0.4851 -0.3651 27 1 10 -0.4802 0.4307 27 3 0 -0.9902 -0.0755 27 3 1 -1.7148 -0.1659 27 3 2 0.5103 -0.0828 27 3 3 -1.9403 -0.1262 27 3 4 1.5308 0.0001 27 3 5 -1.4571 -0.1737 27 3 6 1.4757 0.1736 27 3 7 -0.7746 -0.2472 27 3 8 0.6408 0.3332 27 5 0 -1.5514 0.3783 27 5 1 1.4863 -0.3836 27 5 2 -0.0406 0.2488 27 5 3 1.0818 -0.1930 28 0 0 3.0045 0.1147 28 0 2 3.1213 -0.0812 28 0 4 2.7823 -0.1458 28 0 6 1.5488 -0.0658 28 0 8 0.0504 0.0231 28 2 0 2.6729 -0.0199 28 2 1 -4.5858 -0.4488 28 2 2 2.6384 -0.0490 28 2 3 -4.7727 -0.2726 28 2 4 1.9268 0.0247 28 2 5 -3.7940 -0.1336 28 2 6 0.9108 0.1140 28 2 7 -1.9420 -0.1587 28 2 8 0.0079 0.1209 28 4 0 -0.9143 0.1904 28 4 1 0.8227 -0.3995 28 4 2 1.0535 0.0684 28 4 3 1.3553 -0.2408 28 4 4 1.7757 0.0052 29 1 0 2.9801 -0.2923 29 1 1 -2.8444 -0.3349 29 1 2 2.5969 -0.4930 29 1 3 -2.5842 -0.2014 29 1 4 1.6848 -0.4095 29 1 5 -2.0403 -0.1438 29 1 6 0.5502 -0.0650 29 1 7 -0.7780 -0.2365 29 3 0 0.3103 0.0086 29 3 1 -1.9370 -0.0568 29 3 2 1.5073 -0.0110 29 3 3 -1.3132 -0.0002 29 3 4 1.8366 0.0411 29 3 5 -0.2380 -0.0812 30 0 0 1.0939 -0.2358 30 0 2 1.2576 -0.3695 30 0 4 1.0518 -0.3961 30 0 6 0.4066 -0.2863 30 2 0 2.1720 -0.1272 30 2 1 -2.9916 0.0153 30 2 2 1.9491 -0.1774 30 2 3 -2.6939 0.2234 30 2 4 1.1865 -0.1245 30 2 5 -1.5371 0.2343 30 4 0 0.5004 0.2015 30 4 1 0.8741 -0.2854 31 1 0 1.5754 -0.5337 31 1 1 -1.1943 0.1764 31 1 2 1.3445 -0.6667 31 1 3 -0.9567 0.2789 31 1 4 0.8188 -0.5220 31 3 0 0.6822 0.0226 31 3 1 -0.6091 0.4560 31 3 2 1.4172 -0.0627 32 0 0 0.1134 0.0104 32 0 2 0.5659 -0.1019 32 2 0 1.5684 -0.0842 32 2 1 -0.8447 0.8547 32 2 2 1.2648 -0.1802 33 1 0 1.1453 -0.1196 33 1 1 0.1559 0.6525 0 0 0 0.0 0.0 ; _shelx_fab_checksum 95790 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling - Detector area scaling ; _oxdiff_exptl_absorpt_empirical_full_max 2.676 _oxdiff_exptl_absorpt_empirical_full_min 0.389 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.32514(2) 0.36955(5) 0.67166(2) 0.02015(19) Uani 1 1 d . . . . . Ru2 Ru 0.39475(2) 0.25546(5) 0.59341(2) 0.02042(19) Uani 1 1 d . . . . . O5 O 0.29755(14) 0.1416(5) 0.66699(19) 0.0252(9) Uani 1 1 d . . . . . O4 O 0.26534(14) 0.4692(5) 0.6756(2) 0.0262(9) Uani 1 1 d . . . . . O2 O 0.34844(13) 0.6028(5) 0.67589(19) 0.0236(9) Uani 1 1 d . . . . . O1 O 0.37769(14) 0.2811(5) 0.6608(2) 0.0255(9) Uani 1 1 d . . . . . O7 O 0.45736(14) 0.1501(5) 0.6395(2) 0.0294(10) Uani 1 1 d . . . . . O3 O 0.34815(15) 0.3408(6) 0.76339(19) 0.0282(10) Uani 1 1 d . . . . . O8 O 0.41276(16) 0.2346(5) 0.5178(2) 0.0297(10) Uani 1 1 d . . . . . O9 O 0.36641(14) 0.0292(5) 0.5791(2) 0.0245(9) Uani 1 1 d . . . . . O6 O 0.42153(13) 0.4837(5) 0.6019(2) 0.0257(9) Uani 1 1 d . . . . . N2 N 0.33052(16) 0.3501(6) 0.5484(2) 0.0220(11) Uani 1 1 d . . . . . N1 N 0.30268(16) 0.3962(6) 0.5803(2) 0.0205(10) Uani 1 1 d . . . . . C10 C 0.2465(2) -0.0746(8) 0.6675(3) 0.0339(15) Uani 1 1 d . . . . . H10A H 0.221372 -0.096881 0.631075 0.051 Uiso 1 1 calc R U . . . H10B H 0.237289 -0.103993 0.701332 0.051 Uiso 1 1 calc R U . . . H10C H 0.273226 -0.137656 0.668043 0.051 Uiso 1 1 calc R U . . . C14 C 0.4931(2) 0.2350(8) 0.6666(3) 0.0272(14) Uani 1 1 d . . . . . C17 C 0.4120(2) 0.1011(9) 0.4899(3) 0.0330(15) Uani 1 1 d . . . . . C7 C 0.2290(2) 0.3888(8) 0.6754(3) 0.0288(14) Uani 1 1 d . . . . . C9 C 0.2583(2) 0.1073(8) 0.6705(3) 0.0269(14) Uani 1 1 d . . . . . C13 C 0.4968(2) 0.4039(9) 0.6670(3) 0.0353(16) Uani 1 1 d . . . . . H13 H 0.525025 0.447442 0.691164 0.042 Uiso 1 1 calc R U . . . C3 C 0.3819(2) 0.6077(8) 0.7826(3) 0.0262(14) Uani 1 1 d . . . . . H3 H 0.399068 0.674698 0.814072 0.031 Uiso 1 1 calc R U . . . C1 C 0.3831(2) 0.8472(8) 0.7178(3) 0.0315(15) Uani 1 1 d . . . . . H1A H 0.408481 0.848606 0.702265 0.047 Uiso 1 1 calc R U . . . H1B H 0.392159 0.902003 0.755965 0.047 Uiso 1 1 calc R U . . . H1C H 0.356811 0.902588 0.690356 0.047 Uiso 1 1 calc R U . . . C4 C 0.3708(2) 0.4505(9) 0.7987(3) 0.0293(14) Uani 1 1 d . . . . . C8 C 0.2249(2) 0.2188(9) 0.6749(3) 0.0332(16) Uani 1 1 d . . . . . H8 H 0.197381 0.175710 0.677684 0.040 Uiso 1 1 calc R U . . . C2 C 0.37035(19) 0.6749(8) 0.7254(3) 0.0242(13) Uani 1 1 d . . . . . C20 C 0.3431(3) -0.2287(9) 0.5375(4) 0.0439(19) Uani 1 1 d . . . . . H20A H 0.346563 -0.262383 0.577697 0.066 Uiso 1 1 calc R U . . . H20B H 0.355411 -0.312113 0.518200 0.066 Uiso 1 1 calc R U . . . H20C H 0.310688 -0.212633 0.515453 0.066 Uiso 1 1 calc R U . . . C19 C 0.3686(2) -0.0725(8) 0.5390(3) 0.0314(15) Uani 1 1 d . . . . . C11 C 0.4746(2) 0.6972(9) 0.6385(4) 0.047(2) Uani 1 1 d . . . . . H11A H 0.488115 0.723714 0.608248 0.070 Uiso 1 1 calc R U . . . H11B H 0.496194 0.722936 0.677378 0.070 Uiso 1 1 calc R U . . . H11C H 0.446608 0.759884 0.631802 0.070 Uiso 1 1 calc R U . . . C22 C 0.2646(2) 0.4454(8) 0.4844(3) 0.0279(14) Uani 1 1 d . . . . . H22 H 0.241899 0.477306 0.448917 0.033 Uiso 1 1 calc R U . . . C15 C 0.5351(2) 0.1351(9) 0.7001(4) 0.0380(17) Uani 1 1 d . . . . . H15A H 0.525880 0.046260 0.720521 0.057 Uiso 1 1 calc R U . . . H15B H 0.557086 0.203542 0.728961 0.057 Uiso 1 1 calc R U . . . H15C H 0.549113 0.091632 0.672389 0.057 Uiso 1 1 calc R U . . . C23 C 0.3074(2) 0.3799(8) 0.4911(3) 0.0257(14) Uani 1 1 d . . . . . H23 H 0.318718 0.358996 0.459687 0.031 Uiso 1 1 calc R U . . . C6 C 0.1886(2) 0.4939(9) 0.6742(4) 0.0383(17) Uani 1 1 d . . . . . H6A H 0.198296 0.573765 0.705766 0.057 Uiso 1 1 calc R U . . . H6B H 0.164519 0.426440 0.679727 0.057 Uiso 1 1 calc R U . . . H6C H 0.177062 0.548979 0.636152 0.057 Uiso 1 1 calc R U . . . C12 C 0.4632(2) 0.5172(8) 0.6355(3) 0.0264(14) Uani 1 1 d . . . . . C5 C 0.3868(3) 0.4044(10) 0.8640(3) 0.0416(17) Uani 1 1 d . . . . . H5A H 0.374583 0.481689 0.885772 0.062 Uiso 1 1 calc R U . . . H5B H 0.420112 0.405918 0.879620 0.062 Uiso 1 1 calc R U . . . H5C H 0.375748 0.296238 0.868416 0.062 Uiso 1 1 calc R U . . . C16 C 0.4353(4) 0.1082(11) 0.4415(4) 0.058(2) Uani 1 1 d . . . . . H16A H 0.419704 0.187633 0.411646 0.088 Uiso 1 1 calc R U . . . H16B H 0.433577 0.002095 0.423126 0.088 Uiso 1 1 calc R U . . . H16C H 0.467356 0.139123 0.459505 0.088 Uiso 1 1 calc R U . . . C18 C 0.3912(3) -0.0434(10) 0.4977(3) 0.0434(18) Uani 1 1 d . . . . . H18 H 0.392512 -0.130422 0.472782 0.052 Uiso 1 1 calc R U . . . C21 C 0.2627(2) 0.4538(8) 0.5422(3) 0.0262(13) Uani 1 1 d . . . . . H21 H 0.237800 0.492890 0.552803 0.031 Uiso 1 1 calc R U . . . 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 0.0223(3) 0.0214(3) 0.0185(3) -0.00015(17) 0.0091(2) -0.00270(16) Ru2 0.0202(3) 0.0202(3) 0.0230(3) 0.00072(17) 0.0099(2) -0.00253(16) O5 0.028(2) 0.024(2) 0.024(2) -0.0026(17) 0.0089(18) -0.0064(17) O4 0.028(2) 0.023(2) 0.032(2) -0.0012(18) 0.0156(18) 0.0015(17) O2 0.0207(19) 0.028(2) 0.023(2) -0.0025(18) 0.0089(17) -0.0040(16) O1 0.023(2) 0.027(2) 0.026(2) 0.0004(18) 0.0080(18) -0.0039(17) O7 0.025(2) 0.028(2) 0.036(3) 0.006(2) 0.0115(19) 0.0069(18) O3 0.032(2) 0.035(3) 0.020(2) 0.005(2) 0.0107(18) 0.0008(19) O8 0.031(2) 0.036(3) 0.027(2) 0.002(2) 0.016(2) -0.0032(18) O9 0.0250(19) 0.022(2) 0.030(2) -0.0036(18) 0.0140(18) -0.0047(17) O6 0.0202(19) 0.026(2) 0.031(2) 0.0015(19) 0.0091(18) -0.0032(17) N2 0.019(2) 0.026(3) 0.021(3) -0.001(2) 0.008(2) -0.003(2) N1 0.023(2) 0.024(3) 0.017(3) -0.002(2) 0.009(2) 0.000(2) C10 0.038(3) 0.025(3) 0.043(4) -0.001(3) 0.019(3) -0.015(3) C14 0.021(3) 0.034(4) 0.030(4) 0.000(3) 0.012(3) 0.003(2) C17 0.035(3) 0.043(4) 0.024(3) 0.004(3) 0.014(3) 0.009(3) C7 0.034(3) 0.038(4) 0.018(3) -0.003(3) 0.014(3) 0.000(3) C9 0.032(3) 0.033(4) 0.016(3) -0.004(3) 0.009(3) -0.006(3) C13 0.019(3) 0.043(4) 0.045(4) 0.000(3) 0.012(3) -0.003(3) C3 0.022(3) 0.038(4) 0.018(3) -0.007(3) 0.005(2) 0.000(3) C1 0.029(3) 0.033(4) 0.037(4) -0.008(3) 0.017(3) -0.009(3) C4 0.022(3) 0.044(4) 0.024(3) -0.007(3) 0.012(2) -0.001(3) C8 0.031(3) 0.034(4) 0.041(4) -0.007(3) 0.021(3) -0.011(3) C2 0.016(2) 0.034(4) 0.025(3) -0.006(3) 0.010(2) -0.002(2) C20 0.056(5) 0.025(4) 0.042(5) 0.001(3) 0.003(4) -0.002(3) C19 0.033(3) 0.028(4) 0.027(4) 0.004(3) 0.003(3) 0.008(3) C11 0.027(3) 0.033(4) 0.082(6) -0.012(4) 0.019(4) -0.011(3) C22 0.030(3) 0.031(4) 0.021(3) 0.005(3) 0.005(3) 0.002(3) C15 0.027(3) 0.039(4) 0.050(5) 0.005(3) 0.015(3) 0.010(3) C23 0.032(3) 0.030(4) 0.021(3) -0.005(3) 0.015(3) -0.005(3) C6 0.034(3) 0.044(4) 0.043(4) -0.003(3) 0.022(3) 0.006(3) C12 0.024(3) 0.025(3) 0.033(4) -0.006(3) 0.012(3) -0.003(2) C5 0.044(4) 0.056(5) 0.022(4) -0.003(3) 0.007(3) -0.008(4) C16 0.088(7) 0.061(6) 0.044(5) 0.006(4) 0.047(5) 0.016(5) C18 0.064(5) 0.036(4) 0.031(4) -0.003(3) 0.017(4) 0.004(4) C21 0.024(3) 0.023(3) 0.030(3) 0.000(3) 0.007(3) -0.002(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru 0.0552 3.2960 '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 O5 Ru1 O3 86.81(18) . . ? O5 Ru1 N1 92.94(19) . . ? O4 Ru1 O5 90.34(17) . . ? O4 Ru1 O3 89.81(18) . . ? O4 Ru1 N1 90.73(18) . . ? O2 Ru1 O5 176.18(16) . . ? O2 Ru1 O4 85.86(16) . . ? O2 Ru1 O3 93.60(18) . . ? O2 Ru1 N1 86.69(18) . . ? O1 Ru1 O5 89.91(18) . . ? O1 Ru1 O4 174.98(19) . . ? O1 Ru1 O2 93.84(18) . . ? O1 Ru1 O3 95.21(18) . . ? O1 Ru1 N1 84.24(19) . . ? N1 Ru1 O3 179.40(19) . . ? O1 Ru2 O7 93.85(19) . . ? O1 Ru2 O8 178.10(19) . . ? O1 Ru2 O9 91.23(18) . . ? O1 Ru2 O6 91.73(18) . . ? O1 Ru2 N2 84.92(19) . . ? O8 Ru2 O7 87.59(19) . . ? O8 Ru2 N2 93.70(19) . . ? O9 Ru2 O7 88.78(17) . . ? O9 Ru2 O8 90.04(18) . . ? O9 Ru2 N2 88.48(18) . . ? O6 Ru2 O7 93.33(17) . . ? O6 Ru2 O8 86.94(18) . . ? O6 Ru2 O9 176.24(17) . . ? O6 Ru2 N2 89.47(18) . . ? N2 Ru2 O7 176.98(18) . . ? C9 O5 Ru1 125.9(4) . . ? C7 O4 Ru1 125.7(4) . . ? C2 O2 Ru1 123.0(4) . . ? Ru2 O1 Ru1 131.9(2) . . ? C14 O7 Ru2 122.3(4) . . ? C4 O3 Ru1 122.5(4) . . ? C17 O8 Ru2 124.2(4) . . ? C19 O9 Ru2 126.4(4) . . ? C12 O6 Ru2 122.9(4) . . ? N1 N2 Ru2 118.8(4) . . ? C23 N2 Ru2 134.0(4) . . ? C23 N2 N1 107.2(5) . . ? N2 N1 Ru1 120.0(4) . . ? C21 N1 Ru1 131.2(4) . . ? C21 N1 N2 108.7(5) . . ? H10A C10 H10B 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? O7 C14 C13 126.9(6) . . ? O7 C14 C15 114.2(6) . . ? C13 C14 C15 118.8(6) . . ? O8 C17 C16 115.0(7) . . ? O8 C17 C18 126.4(6) . . ? C18 C17 C16 118.6(7) . . ? O4 C7 C8 125.7(6) . . ? O4 C7 C6 114.4(6) . . ? C8 C7 C6 119.9(6) . . ? O5 C9 C10 115.4(6) . . ? O5 C9 C8 126.5(6) . . ? C8 C9 C10 118.1(6) . . ? C14 C13 H13 116.2 . . ? C14 C13 C12 127.6(6) . . ? C12 C13 H13 116.2 . . ? C4 C3 H3 116.1 . . ? C2 C3 H3 116.1 . . ? C2 C3 C4 127.8(6) . . ? H1A C1 H1B 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? O3 C4 C3 126.4(6) . . ? O3 C4 C5 115.0(6) . . ? C3 C4 C5 118.6(6) . . ? C7 C8 C9 125.7(6) . . ? C7 C8 H8 117.2 . . ? C9 C8 H8 117.2 . . ? O2 C2 C3 126.5(6) . . ? O2 C2 C1 113.7(6) . . ? C3 C2 C1 119.8(6) . . ? H20A C20 H20B 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? O9 C19 C20 114.8(6) . . ? O9 C19 C18 124.7(7) . . ? C18 C19 C20 120.4(7) . . ? H11A C11 H11B 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C12 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? C12 C11 H11C 109.5 . . ? C23 C22 H22 127.7 . . ? C23 C22 C21 104.6(5) . . ? C21 C22 H22 127.7 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15B 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N2 C23 C22 110.8(5) . . ? N2 C23 H23 124.6 . . ? C22 C23 H23 124.6 . . ? C7 C6 H6A 109.5 . . ? C7 C6 H6B 109.5 . . ? C7 C6 H6C 109.5 . . ? H6A C6 H6B 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O6 C12 C13 126.2(6) . . ? O6 C12 C11 113.7(6) . . ? C13 C12 C11 120.1(6) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5B 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C17 C16 H16A 109.5 . . ? C17 C16 H16B 109.5 . . ? C17 C16 H16C 109.5 . . ? H16A C16 H16B 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C17 C18 C19 126.7(7) . . ? C17 C18 H18 116.7 . . ? C19 C18 H18 116.7 . . ? N1 C21 C22 108.7(5) . . ? N1 C21 H21 125.7 . . ? C22 C21 H21 125.7 . . ? 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 O5 2.025(4) . ? Ru1 O4 2.024(4) . ? Ru1 O2 2.018(4) . ? Ru1 O1 1.848(4) . ? Ru1 O3 2.057(4) . ? Ru1 N1 2.047(5) . ? Ru2 O1 1.842(4) . ? Ru2 O7 2.046(4) . ? Ru2 O8 2.039(5) . ? Ru2 O9 2.015(4) . ? Ru2 O6 2.012(4) . ? Ru2 N2 2.044(5) . ? O5 C9 1.257(8) . ? O4 C7 1.284(8) . ? O2 C2 1.280(7) . ? O7 C14 1.270(8) . ? O3 C4 1.261(8) . ? O8 C17 1.267(8) . ? O9 C19 1.275(8) . ? O6 C12 1.285(7) . ? N2 N1 1.359(7) . ? N2 C23 1.326(8) . ? N1 C21 1.337(8) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C10 C9 1.519(9) . ? C14 C13 1.379(10) . ? C14 C15 1.501(9) . ? C17 C16 1.531(10) . ? C17 C18 1.377(11) . ? C7 C8 1.390(9) . ? C7 C6 1.491(9) . ? C9 C8 1.393(10) . ? C13 H13 0.9300 . ? C13 C12 1.397(10) . ? C3 H3 0.9300 . ? C3 C4 1.407(10) . ? C3 C2 1.391(9) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C1 C2 1.482(9) . ? C4 C5 1.503(10) . ? C8 H8 0.9300 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C20 C19 1.485(10) . ? C19 C18 1.387(11) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C11 C12 1.502(10) . ? C22 H22 0.9300 . ? C22 C23 1.368(9) . ? C22 C21 1.388(9) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C23 H23 0.9300 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C18 H18 0.9300 . ? C21 H21 0.9300 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Ru1 O5 C9 C10 -178.3(4) . . . . ? Ru1 O5 C9 C8 3.9(9) . . . . ? Ru1 O4 C7 C8 2.7(9) . . . . ? Ru1 O4 C7 C6 -175.7(4) . . . . ? Ru1 O2 C2 C3 0.6(8) . . . . ? Ru1 O2 C2 C1 -178.5(4) . . . . ? Ru1 O3 C4 C3 3.1(8) . . . . ? Ru1 O3 C4 C5 -177.1(4) . . . . ? Ru1 N1 C21 C22 -179.8(4) . . . . ? Ru2 O7 C14 C13 -3.9(10) . . . . ? Ru2 O7 C14 C15 177.3(4) . . . . ? Ru2 O8 C17 C16 -169.2(5) . . . . ? Ru2 O8 C17 C18 13.3(10) . . . . ? Ru2 O9 C19 C20 -178.0(4) . . . . ? Ru2 O9 C19 C18 -0.2(9) . . . . ? Ru2 O6 C12 C13 5.0(9) . . . . ? Ru2 O6 C12 C11 -175.7(5) . . . . ? Ru2 N2 N1 Ru1 -0.3(6) . . . . ? Ru2 N2 N1 C21 -179.9(4) . . . . ? Ru2 N2 C23 C22 -180.0(4) . . . . ? O5 Ru1 O1 Ru2 96.2(3) . . . . ? O5 C9 C8 C7 0.8(12) . . . . ? O4 C7 C8 C9 -4.4(12) . . . . ? O2 Ru1 O1 Ru2 -83.0(3) . . . . ? O7 Ru2 O1 Ru1 179.4(3) . . . . ? O7 C14 C13 C12 -3.7(12) . . . . ? O3 Ru1 O1 Ru2 -177.0(3) . . . . ? O8 C17 C18 C19 -2.5(13) . . . . ? O9 Ru2 O1 Ru1 -91.7(3) . . . . ? O9 C19 C18 C17 -4.9(12) . . . . ? O6 Ru2 O1 Ru1 86.0(3) . . . . ? N2 Ru2 O1 Ru1 -3.4(3) . . . . ? N2 N1 C21 C22 -0.2(7) . . . . ? N1 Ru1 O1 Ru2 3.2(3) . . . . ? N1 N2 C23 C22 0.1(7) . . . . ? C10 C9 C8 C7 -177.0(7) . . . . ? C14 C13 C12 O6 3.1(12) . . . . ? C14 C13 C12 C11 -176.1(7) . . . . ? C4 C3 C2 O2 -2.5(10) . . . . ? C4 C3 C2 C1 176.6(6) . . . . ? C2 C3 C4 O3 0.3(10) . . . . ? C2 C3 C4 C5 -179.5(6) . . . . ? C20 C19 C18 C17 172.8(7) . . . . ? C15 C14 C13 C12 175.0(7) . . . . ? C23 N2 N1 Ru1 179.7(4) . . . . ? C23 N2 N1 C21 0.0(6) . . . . ? C23 C22 C21 N1 0.3(7) . . . . ? C6 C7 C8 C9 173.9(7) . . . . ? C16 C17 C18 C19 -180.0(8) . . . . ? C21 C22 C23 N2 -0.2(7) . . . . ? loop_ _smtbx_masks_void_nr _smtbx_masks_void_average_x _smtbx_masks_void_average_y _smtbx_masks_void_average_z _smtbx_masks_void_volume _smtbx_masks_void_count_electrons _smtbx_masks_void_content 1 0.000 0.000 0.000 79.7 16.8 ? 2 0.000 0.000 0.500 79.7 16.8 ? 3 0.500 0.500 0.000 79.7 16.8 ? 4 0.500 0.500 0.500 79.7 16.8 ?