#------------------------------------------------------------------------------ #$Date: 2024-06-01 01:12:21 +0300 (Sat, 01 Jun 2024) $ #$Revision: 292131 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/17/1571734.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_1571734 loop_ _publ_author_name 'Ye, Christopher Z.' 'Del Rosal, Iker' 'Kelly, Sheridon N.' 'Brackbill, I. Joseph' 'Maron, Laurent' 'Camp, Cl\'ement' 'Arnold, John' _publ_section_title ; Photolysis-driven bond activation by thorium and uranium tetraosmate polyhydride complexes ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D4SC02380C _journal_year 2024 _chemical_formula_moiety '0.333(C30 H45 Os3), C30 H45 Os3 U' _chemical_formula_sum 'C40 H60 Os4 U' _chemical_formula_weight 1539.71 _space_group_crystal_system cubic _space_group_IT_number 205 _space_group_name_Hall '-P 2ac 2ab 3' _space_group_name_H-M_alt 'P a -3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _atom_sites_solution_secondary difmap _audit_creation_date 2023-05-05 _audit_creation_method ; Olex2 1.5 (compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748) ; _audit_update_record ; 2024-04-08 deposited with the CCDC. 2024-05-20 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 21.395(2) _cell_length_b 21.395(2) _cell_length_c 21.395(2) _cell_measurement_reflns_used 125415 _cell_measurement_temperature 100 _cell_measurement_theta_max 27.804 _cell_measurement_theta_min 1.952 _cell_volume 9793.5(16) _computing_cell_refinement 'SAINT V8.38A Bruker, Madison WI' _computing_data_collection 'Bruker APEX3 Bruker, Madison WI' _computing_data_reduction 'SAINT V8.38A Bruker, Madison WI' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2014/7 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 100 _diffrn_detector_area_resol_mean 10.42 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker D8 with PHOTON-II CPAD detector' _diffrn_measurement_method '\f and \w shutterless scans' _diffrn_radiation_monochromator 'silicon 111' _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.7288 _diffrn_reflns_av_R_equivalents 0.1087 _diffrn_reflns_av_unetI/netI 0.0356 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_number 125415 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.930 _diffrn_reflns_theta_max 27.804 _diffrn_reflns_theta_min 1.952 _diffrn_source 'Advanced Light Source, station 12.2.1' _exptl_absorpt_coefficient_mu 12.483 _exptl_absorpt_correction_T_max 0.7441 _exptl_absorpt_correction_T_min 0.4843 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1747 before and 0.1221 after correction. The Ratio of minimum to maximum transmission is 0.6509. The \l/2 correction factor is Not present. ; _exptl_crystal_colour yellow _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 2.089 _exptl_crystal_description block _exptl_crystal_F_000 5568 _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _refine_diff_density_max 1.352 _refine_diff_density_min -1.910 _refine_diff_density_rms 0.301 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.109 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 206 _refine_ls_number_reflns 3605 _refine_ls_number_restraints 75 _refine_ls_restrained_S_all 1.103 _refine_ls_R_factor_all 0.0372 _refine_ls_R_factor_gt 0.0342 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0530P)^2^+52.5146P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0965 _refine_ls_wR_factor_ref 0.0986 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3289 _reflns_number_total 3605 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc02380c2.cif _cod_data_source_block czy_ii_125_0m _cod_original_cell_volume 9793(3) _cod_database_code 1571734 _shelx_shelxl_version_number 2014/7 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.574 _shelx_estimated_absorpt_t_min 0.368 _olex2_refinement_description ; 1. Rigid body (RIGU) restrains C2, C3, C4, C5, C6, C7, C8, C9, C10, C11 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 2. Others Fixed Sof: C2(0.3333) C3(0.3333) C4(0.3333) C5(0.3333) C6(0.3333) C7(0.3333) H7A(0.3333) H7B(0.3333) H7C(0.3333) C8(0.3333) H8A(0.3333) H8B(0.3333) H8C(0.3333) C9(0.3333) H9A(0.3333) H9B(0.3333) H9C(0.3333) C10(0.3333) H10A(0.3333) H10B(0.3333) H10C(0.3333) C11(0.3333) H11A(0.3333) H11B(0.3333) H11C(0.3333) 3.a Idealised Me refined as rotating group: C00B(H00A,H00B,H00C), C00C(H00D,H00E,H00F), C00D(H00G,H00H,H00I), C00E(H00J, H00K,H00L), C00F(H00M,H00N,H00O), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B, H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C) ; _smtbx_masks_void_probe_radius 1.2 _smtbx_masks_void_truncation_radius 1.2 _shelx_res_file ; czy_ii_125_0m.res created by SHELXL-2014/7 TITL czy_ii_125_0m_a.res in Pa-3 REM Old TITL CZY_II_125_0m in Pa-3 REM SHELXT solution in Pa-3 REM R1 0.112, Rweak 0.003, Alpha 0.021, Orientation as input REM Formula found by SHELXT: C36 U5 CELL 0.7288 21.3949 21.3949 21.3949 90 90 90 ZERR 8 0.0021 0.0021 0.0021 0 0 0 LATT 1 SYMM 0.5-X,-Y,0.5+Z SYMM -X,0.5+Y,0.5-Z SYMM 0.5+X,0.5-Y,-Z SYMM +Z,+X,+Y SYMM 0.5+Z,0.5-X,-Y SYMM 0.5-Z,-X,0.5+Y SYMM -Z,0.5+X,0.5-Y SYMM +Y,+Z,+X SYMM -Y,0.5+Z,0.5-X SYMM 0.5+Y,0.5-Z,-X SYMM 0.5-Y,-Z,0.5+X SFAC C H Os1 U DISP C 0.0034 0.0017 11.92 DISP H 0 0 0.67 DISP Os1 -1.2848 7.9466 33486.29 DISP U -10.9608 4.158 18355.36 UNIT 320 480 32 8 RIGU C2 C3 C4 C5 C6 C7 C8 C9 C10 C11 L.S. 10 PLAN 15 SIZE 0.1 0.1 0.05 TEMP -173.15 CONF list 4 MORE -1 BOND $H fmap 2 53 acta ABIN SHEL 100 0.78 OMIT 0 6 6 OMIT 0 2 3 OMIT 1 1 1 OMIT 0 2 7 REM REM REM WGHT 0.053000 52.514599 FVAR 0.07621 OS2 3 0.602277 0.602277 0.602277 10.33333 0.02370 0.02370 = 0.02370 -0.00312 -0.00312 -0.00312 U1 4 0.681858 0.681858 0.681858 10.33333 0.02398 0.02398 = 0.02398 -0.00276 -0.00276 -0.00276 OS1 3 0.669906 0.646622 0.814631 11.00000 0.02690 0.03607 = 0.02310 -0.00083 -0.00404 0.00210 C004 1 0.618548 0.659264 0.905795 11.00000 0.03364 0.04693 = 0.03330 0.00221 -0.00244 0.00470 C005 1 0.680734 0.683211 0.911838 11.00000 0.03206 0.05098 = 0.02730 -0.00611 0.00050 0.00194 C006 1 0.687579 0.577106 0.890446 11.00000 0.05350 0.04427 = 0.02346 0.00158 0.00030 0.01864 C008 1 0.622717 0.594876 0.892484 11.00000 0.03630 0.05028 = 0.02945 0.00848 -0.00483 -0.00487 C00A 1 0.723252 0.634508 0.902572 11.00000 0.02700 0.05927 = 0.02233 0.00384 -0.00532 0.00862 C00B 1 0.712020 0.513088 0.883693 11.00000 0.09817 0.06328 = 0.02972 0.00174 0.00115 0.03179 AFIX 137 H00A 2 0.679973 0.486435 0.864699 11.00000 -1.50000 H00B 2 0.723144 0.496561 0.924939 11.00000 -1.50000 H00C 2 0.749201 0.513683 0.856947 11.00000 -1.50000 AFIX 0 C00C 1 0.793030 0.638391 0.909318 11.00000 0.03162 0.10945 = 0.04363 0.00974 -0.00767 0.00738 AFIX 137 H00D 2 0.812881 0.610334 0.879039 11.00000 -1.50000 H00E 2 0.804982 0.625973 0.951757 11.00000 -1.50000 H00F 2 0.806750 0.681399 0.901558 11.00000 -1.50000 AFIX 0 C00D 1 0.559365 0.696094 0.915594 11.00000 0.03734 0.07175 = 0.06276 0.00919 0.01544 0.01424 AFIX 137 H00G 2 0.559897 0.733254 0.888819 11.00000 -1.50000 H00H 2 0.556455 0.708928 0.959468 11.00000 -1.50000 H00I 2 0.523232 0.670064 0.904871 11.00000 -1.50000 AFIX 0 C00E 1 0.567320 0.548008 0.888903 11.00000 0.06258 0.05548 = 0.07263 0.00365 -0.00419 -0.01679 AFIX 137 H00J 2 0.529076 0.570424 0.877369 11.00000 -1.50000 H00K 2 0.561578 0.528009 0.929710 11.00000 -1.50000 H00L 2 0.576379 0.516041 0.857373 11.00000 -1.50000 AFIX 0 C00F 1 0.696173 0.748893 0.931950 11.00000 0.05311 0.05895 = 0.05104 -0.01670 0.00408 -0.01218 AFIX 137 H00M 2 0.727245 0.766700 0.903393 11.00000 -1.50000 H00N 2 0.713136 0.748245 0.974494 11.00000 -1.50000 H00O 2 0.658181 0.774465 0.931049 11.00000 -1.50000 AFIX 0 PART -1 C2 1 0.519520 0.540860 0.594472 10.33333 0.02838 0.01598 = 0.02463 -0.00203 -0.00563 -0.00759 C3 1 0.578504 0.509329 0.567647 10.33333 0.02860 0.01653 = 0.02526 -0.00301 -0.00702 -0.00040 C4 1 0.596630 0.541892 0.515307 10.33333 0.01782 0.01933 = 0.02261 -0.00654 -0.00736 0.00146 C5 1 0.555958 0.594591 0.506142 10.33333 0.02036 0.02736 = 0.02941 0.00603 0.00489 0.00552 C6 1 0.509747 0.590629 0.555340 10.33333 0.01272 0.01916 = 0.02355 -0.00368 -0.00106 -0.00328 C7 1 0.455613 0.642290 0.554000 10.33333 0.02661 0.03394 = 0.06147 -0.00271 0.00157 0.00763 AFIX 137 H7A 2 0.435281 0.644168 0.595002 10.33333 -1.50000 H7B 2 0.424672 0.631161 0.522110 10.33333 -1.50000 H7C 2 0.473753 0.683161 0.544067 10.33333 -1.50000 AFIX 0 C8 1 0.560892 0.636229 0.449643 10.33333 0.05590 0.03988 = 0.03002 0.00975 -0.00027 0.00013 AFIX 137 H8A 2 0.602986 0.654165 0.447522 10.33333 -1.50000 H8B 2 0.530064 0.669961 0.452797 10.33333 -1.50000 H8C 2 0.552836 0.611670 0.411826 10.33333 -1.50000 AFIX 0 C9 1 0.650561 0.519066 0.475020 10.33333 0.03962 0.06175 = 0.05112 -0.00928 0.01069 0.01678 AFIX 137 H9A 2 0.667485 0.554119 0.450876 10.33333 -1.50000 H9B 2 0.635556 0.486626 0.446373 10.33333 -1.50000 H9C 2 0.683396 0.501742 0.501852 10.33333 -1.50000 AFIX 0 C10 1 0.595720 0.450685 0.599942 10.33333 0.07723 0.01747 = 0.06667 0.00270 -0.03895 -0.00628 AFIX 137 H10A 2 0.640727 0.450588 0.608455 10.33333 -1.50000 H10B 2 0.585136 0.414930 0.573339 10.33333 -1.50000 H10C 2 0.572705 0.447677 0.639431 10.33333 -1.50000 AFIX 0 C11 1 0.473049 0.526811 0.646426 10.33333 0.05670 0.04219 = 0.04315 -0.00347 0.01212 -0.01929 AFIX 137 H11A 2 0.489354 0.493088 0.672789 10.33333 -1.50000 H11B 2 0.433100 0.513910 0.628102 10.33333 -1.50000 H11C 2 0.466757 0.564386 0.671856 10.33333 -1.50000 AFIX 0 HKLF 4 REM czy_ii_125_0m_a.res in Pa-3 REM R1 = 0.0342 for 3289 Fo > 4sig(Fo) and 0.0372 for all 3605 data REM 206 parameters refined using 75 restraints END WGHT 0.0530 52.5149 REM Highest difference peak 1.352, deepest hole -1.910, 1-sigma level 0.301 Q1 1 0.5810 0.5797 0.7504 11.00000 0.05 1.35 Q2 1 0.7463 0.4173 0.9149 11.00000 0.05 1.29 Q3 1 0.7518 0.7518 0.7518 10.33333 0.05 1.22 Q4 1 0.8340 0.8340 0.8340 10.33333 0.05 1.12 Q5 1 0.8251 0.8251 0.8251 10.33333 0.05 1.08 Q6 1 0.5818 0.4182 0.9182 10.33333 0.05 1.05 Q7 1 0.6589 0.5114 0.8006 11.00000 0.05 0.88 Q8 1 0.6562 0.5186 0.6890 11.00000 0.05 0.85 Q9 1 0.8167 0.6983 0.8200 11.00000 0.05 0.81 Q10 1 0.7558 0.7451 1.0806 11.00000 0.05 0.77 Q11 1 0.6745 0.4800 0.9197 11.00000 0.05 0.73 Q12 1 0.5182 0.4979 0.9785 11.00000 0.05 0.71 Q13 1 0.5171 0.5609 0.9815 11.00000 0.05 0.68 Q14 1 0.6432 0.4998 0.4974 11.00000 0.05 0.66 Q15 1 0.5184 0.5171 0.5812 11.00000 0.05 0.65 ; _shelx_res_checksum 12621 _shelx_fab_file ; 0 2 0 -39.2160 2.1135 0 2 1 -165.8865 -19.8103 0 2 2 8.3271 -3.0881 0 2 3 -64.2743 -0.4120 0 2 4 5.5503 -5.1650 0 2 5 -20.8839 -6.0785 0 2 6 -17.8170 9.3036 0 2 7 12.1366 5.3394 0 2 8 16.5232 -2.9470 0 2 9 0.1664 2.1705 0 2 10 -25.1837 1.6903 0 2 11 13.9905 -12.6685 0 2 12 5.7233 10.9477 0 2 13 -11.0303 12.0210 0 2 14 8.6942 -13.1738 0 2 15 3.4199 -1.7285 0 2 16 -4.6159 -2.5970 0 2 17 -4.0326 -12.5661 0 2 18 0.9476 5.6079 0 2 19 0.5509 18.1467 0 2 20 0.5847 -2.3578 0 2 21 2.3106 -3.5692 0 2 22 -3.6464 3.7786 0 2 23 1.2337 -16.0437 0 2 24 6.0993 -2.4421 0 2 25 0.6937 16.5438 0 2 26 -1.0536 -1.7767 0 2 27 -2.7180 -4.0028 0 2 28 1.2425 2.9603 0 4 0 -33.8306 4.0425 0 4 1 13.8965 -10.1396 0 4 2 -14.1150 -12.7430 0 4 3 41.3798 5.2863 0 4 4 29.0211 -1.9563 0 4 5 46.6451 9.8571 0 4 6 50.7046 4.1114 0 4 7 -40.1778 -13.0922 0 4 8 17.0527 -2.3234 0 4 9 5.2494 3.6538 0 4 10 -5.9943 1.0852 0 4 11 -10.1498 12.8422 0 4 12 4.5745 2.9577 0 4 13 16.2747 -14.5877 0 4 14 -4.6367 -1.2484 0 4 15 10.0964 3.8821 0 4 16 -7.3273 -1.9269 0 4 17 3.9841 11.4701 0 4 18 8.3701 1.5406 0 4 19 -0.3637 -15.4897 0 4 20 -6.3511 1.0090 0 4 21 -0.8472 3.6060 0 4 22 -1.0248 -0.2778 0 4 23 -1.6705 12.4137 0 4 24 2.1350 -2.0375 0 4 25 -3.7038 -14.8954 0 4 26 -3.8231 -2.1405 0 4 27 0.5301 5.7612 0 4 28 2.4463 3.3095 0 6 0 47.2996 -19.3159 0 6 1 -34.7570 12.9031 0 6 2 34.5922 8.6096 0 6 3 -7.4407 4.4366 0 6 4 21.8880 5.6762 0 6 5 24.0284 -2.4187 0 6 6 -235.6704 -22.6248 0 6 7 -5.6073 1.6406 0 6 8 26.9082 12.9440 0 6 9 11.6382 -0.2037 0 6 10 -26.6117 6.4797 0 6 11 0.0796 -7.7315 0 6 12 32.1065 -13.3667 0 6 13 -7.1815 9.3065 0 6 14 1.5947 7.1574 0 6 15 1.7328 -1.4867 0 6 16 -4.3735 -0.4665 0 6 17 -5.1002 -8.5893 0 6 18 -1.5005 -7.4344 0 6 19 -1.5761 7.4249 0 6 20 -4.3422 10.5122 0 6 21 5.4167 -2.3741 0 6 22 -2.0941 -1.2884 0 6 23 -2.8098 -4.8231 0 6 24 0.6048 -5.7493 0 6 25 13.2689 8.1726 0 6 26 -0.0273 3.7419 0 6 27 0.8375 -2.8085 0 6 28 -1.2143 -3.8217 0 8 0 28.6380 26.6331 0 8 1 34.1133 3.8420 0 8 2 -27.6648 -12.6010 0 8 3 2.7720 -2.0890 0 8 4 2.8301 -6.9969 0 8 5 -35.2422 0.2672 0 8 6 40.8971 22.9968 0 8 7 32.0787 -4.6448 0 8 8 9.7045 -15.1155 0 8 9 14.5474 0.0511 0 8 10 -15.1777 -3.4690 0 8 11 -7.9486 0.4170 0 8 12 3.1821 13.7439 0 8 13 0.7295 2.3604 0 8 14 -7.2934 -10.3116 0 8 15 -6.3098 -0.4529 0 8 16 4.8588 -0.4755 0 8 17 1.1774 -5.0231 0 8 18 9.7131 10.0198 0 8 19 -1.3638 3.8100 0 8 20 2.8972 -8.9107 0 8 21 0.3467 1.6581 0 8 22 5.2971 1.9586 0 8 23 -3.9318 -1.3966 0 8 24 9.1958 6.2902 0 8 25 -3.0386 3.2195 0 8 26 -4.4624 -9.1456 0 8 27 4.4595 -3.7930 0 10 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19 4.2324 -1.3349 12 16 20 4.3069 -4.4412 12 17 12 0.8808 0.6328 12 17 13 4.2493 -4.6184 12 17 14 1.6653 1.0820 12 17 15 2.5831 -2.6345 12 17 16 -0.9836 2.0011 12 17 17 -2.5170 1.0514 12 17 18 0.7131 -1.1266 12 17 19 -1.7810 0.1292 12 17 20 0.2912 2.6682 12 18 12 3.2881 0.4322 12 18 13 -3.7189 0.0158 12 18 14 0.2968 -1.6249 12 18 15 -6.0622 -0.0510 12 18 16 3.1380 -1.2050 12 18 17 6.2890 0.3958 12 18 18 2.7379 -4.1387 12 18 19 -5.5116 -0.0265 12 19 12 0.8712 -1.0203 12 19 13 -0.2258 2.2139 12 19 14 1.0020 0.3232 12 19 15 -2.2971 3.0244 12 19 16 1.4330 -1.6038 12 19 17 0.6637 -2.1771 12 19 18 1.3114 -0.8760 12 20 12 -2.4707 -2.8308 12 20 13 -2.4874 2.3332 12 20 14 1.3516 0.9362 12 20 15 -0.3795 0.6739 12 20 16 1.4445 -3.6224 12 20 17 -3.4114 1.6985 12 21 12 -0.3257 3.8145 12 21 13 1.4644 -0.5957 12 21 14 2.8001 -4.8699 12 21 15 -1.2922 0.1484 12 22 12 0.8844 -1.2054 12 22 13 -3.1728 0.4675 12 22 14 -0.2121 -0.3631 12 23 12 -3.2371 2.2101 13 13 13 -7.6913 -2.6630 13 14 13 3.1657 -0.8416 13 14 14 0.8156 1.1222 13 14 15 -4.4046 0.4474 13 14 16 1.1537 0.2774 13 14 17 -2.8349 -0.9296 13 14 18 2.2888 -0.3019 13 14 19 0.4922 -0.0643 13 14 20 3.9075 -2.2876 13 14 21 3.4661 -0.8269 13 15 13 1.5294 3.5166 13 15 14 1.1015 4.2780 13 15 15 1.4464 -0.4302 13 15 16 2.1893 0.0059 13 15 17 -4.5882 1.6844 13 15 18 -2.2458 -0.1223 13 15 19 4.3071 -0.5040 13 15 20 -2.5473 1.3286 13 16 13 0.1159 -1.6277 13 16 14 -3.6952 -1.6502 13 16 15 3.5058 -0.1908 13 16 16 -3.8200 2.9255 13 16 17 0.9169 -2.0131 13 16 18 2.2472 -3.1820 13 16 19 0.6336 -1.8742 13 16 20 -4.8053 5.0153 13 17 13 2.1924 -2.5441 13 17 14 -0.4162 -1.2850 13 17 15 0.9688 -0.8211 13 17 16 -1.7351 -1.1177 13 17 17 2.0434 -5.7515 13 17 18 2.4723 -0.7315 13 17 19 1.1957 1.3278 13 18 13 -3.7310 -0.0591 13 18 14 -3.1518 0.5807 13 18 15 0.9118 0.1256 13 18 16 -1.0912 -2.4273 13 18 17 0.2068 0.2073 13 18 18 -0.0839 1.7750 13 19 13 -0.1380 -2.1303 13 19 14 -2.7998 2.1899 13 19 15 2.0652 -3.9952 13 19 16 1.8180 1.6494 13 19 17 -1.1098 3.7153 13 20 13 3.7386 -3.1596 13 20 14 4.0594 -3.8475 13 20 15 -0.1929 -1.0113 13 20 16 -0.4886 1.4578 13 21 13 -5.9361 -0.3029 13 21 14 1.8508 -3.0126 13 22 13 -0.8950 0.7296 14 14 14 1.9408 0.0777 14 15 14 -0.6990 -2.5141 14 15 15 -3.2406 1.0363 14 15 16 5.0960 1.3029 14 15 17 3.2983 -2.4620 14 15 18 -1.6563 -4.2130 14 15 19 -0.5114 0.5761 14 15 20 2.4842 2.6733 14 16 14 -1.1581 -2.9341 14 16 15 -2.8444 0.0543 14 16 16 1.0896 1.0346 14 16 17 1.2756 -1.9745 14 16 18 0.1906 -1.6506 14 16 19 0.0528 2.1510 14 17 14 -0.8944 -0.2726 14 17 15 -3.9951 -0.1410 14 17 16 0.0953 -2.9340 14 17 17 1.8357 -1.9553 14 17 18 -3.5864 2.0756 14 18 14 0.9184 3.0065 14 18 15 3.6659 -3.5011 14 18 16 -1.9390 -1.0304 14 18 17 1.9160 1.6784 14 19 14 -0.1885 -3.9997 14 19 15 1.2540 -2.9040 14 19 16 1.8538 4.8206 14 20 14 1.1003 -1.8499 14 20 15 -3.6076 1.1972 14 21 14 -3.3975 5.3025 15 15 15 0.1446 1.1362 15 16 15 -1.4429 -2.4834 15 16 16 0.3740 -2.1584 15 16 17 -1.0368 -1.9442 15 16 18 0.9346 3.2286 15 17 15 -2.3927 -2.3814 15 17 16 4.3443 -0.5989 15 17 17 2.0588 3.5453 15 18 15 2.4373 -1.1000 15 18 16 -0.2422 2.2455 15 19 15 -1.6849 6.1742 16 16 16 2.9699 -3.9183 16 17 16 -2.9585 2.7154 16 17 17 -3.0846 8.0365 0 0 0 0.0 0.0 ; _shelx_fab_checksum 69635 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' '-z, -x, -y' '-z-1/2, x-1/2, y' 'z-1/2, x, -y-1/2' 'z, -x-1/2, y-1/2' '-y, -z, -x' 'y, -z-1/2, x-1/2' '-y-1/2, z-1/2, x' 'y-1/2, z, -x-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 Os2 Os 0.60228(2) 0.60228(2) 0.60228(2) 0.02370(12) Uani 1 3 d S T P . . U1 U 0.68186(2) 0.68186(2) 0.68186(2) 0.02398(12) Uani 1 3 d S T P . . Os1 Os 0.66991(2) 0.64662(2) 0.81463(2) 0.02869(11) Uani 1 1 d . . . . . C004 C 0.6185(4) 0.6593(4) 0.9058(3) 0.0380(16) Uani 1 1 d . . . . . C005 C 0.6807(3) 0.6832(4) 0.9118(3) 0.0368(16) Uani 1 1 d . . . . . C006 C 0.6876(4) 0.5771(4) 0.8904(3) 0.0404(18) Uani 1 1 d . . . . . C008 C 0.6227(4) 0.5949(4) 0.8925(3) 0.0387(17) Uani 1 1 d . . . . . C00A C 0.7233(3) 0.6345(4) 0.9026(3) 0.0362(16) Uani 1 1 d . . . . . C00B C 0.7120(6) 0.5131(5) 0.8837(4) 0.064(3) Uani 1 1 d . . . . . H00A H 0.6800 0.4864 0.8647 0.096 Uiso 1 1 calc R U . . . H00B H 0.7231 0.4966 0.9249 0.096 Uiso 1 1 calc R U . . . H00C H 0.7492 0.5137 0.8569 0.096 Uiso 1 1 calc R U . . . C00C C 0.7930(4) 0.6384(6) 0.9093(4) 0.062(3) Uani 1 1 d . . . . . H00D H 0.8129 0.6103 0.8790 0.092 Uiso 1 1 calc R U . . . H00E H 0.8050 0.6260 0.9518 0.092 Uiso 1 1 calc R U . . . H00F H 0.8068 0.6814 0.9016 0.092 Uiso 1 1 calc R U . . . C00D C 0.5594(4) 0.6961(5) 0.9156(5) 0.057(2) Uani 1 1 d . . . . . H00G H 0.5599 0.7333 0.8888 0.086 Uiso 1 1 calc R U . . . H00H H 0.5565 0.7089 0.9595 0.086 Uiso 1 1 calc R U . . . H00I H 0.5232 0.6701 0.9049 0.086 Uiso 1 1 calc R U . . . C00E C 0.5673(5) 0.5480(5) 0.8889(5) 0.064(3) Uani 1 1 d . . . . . H00J H 0.5291 0.5704 0.8774 0.095 Uiso 1 1 calc R U . . . H00K H 0.5616 0.5280 0.9297 0.095 Uiso 1 1 calc R U . . . H00L H 0.5764 0.5160 0.8574 0.095 Uiso 1 1 calc R U . . . C00F C 0.6962(5) 0.7489(4) 0.9320(4) 0.054(2) Uani 1 1 d . . . . . H00M H 0.7272 0.7667 0.9034 0.082 Uiso 1 1 calc R U . . . H00N H 0.7131 0.7482 0.9745 0.082 Uiso 1 1 calc R U . . . H00O H 0.6582 0.7745 0.9310 0.082 Uiso 1 1 calc R U . . . C2 C 0.5195(19) 0.5409(18) 0.5945(13) 0.023(4) Uani 0.3333 1 d . U P A -1 C3 C 0.579(2) 0.5093(13) 0.5676(18) 0.023(5) Uani 0.3333 1 d . U P A -1 C4 C 0.5966(15) 0.5419(16) 0.515(2) 0.020(5) Uani 0.3333 1 d . U P A -1 C5 C 0.5560(17) 0.5946(15) 0.5061(15) 0.026(6) Uani 0.3333 1 d . U P A -1 C6 C 0.5097(14) 0.5906(19) 0.5553(17) 0.018(5) Uani 0.3333 1 d . U P A -1 C7 C 0.4556(11) 0.6423(11) 0.5540(14) 0.041(5) Uani 0.3333 1 d . U P A -1 H7A H 0.4353 0.6442 0.5950 0.061 Uiso 0.3333 1 calc R U P A -1 H7B H 0.4247 0.6312 0.5221 0.061 Uiso 0.3333 1 calc R U P A -1 H7C H 0.4738 0.6832 0.5441 0.061 Uiso 0.3333 1 calc R U P A -1 C8 C 0.5609(15) 0.6362(12) 0.4496(11) 0.042(5) Uani 0.3333 1 d . U P A -1 H8A H 0.6030 0.6542 0.4475 0.063 Uiso 0.3333 1 calc R U P A -1 H8B H 0.5301 0.6700 0.4528 0.063 Uiso 0.3333 1 calc R U P A -1 H8C H 0.5528 0.6117 0.4118 0.063 Uiso 0.3333 1 calc R U P A -1 C9 C 0.6506(12) 0.5191(15) 0.4750(14) 0.051(6) Uani 0.3333 1 d . U P A -1 H9A H 0.6675 0.5541 0.4509 0.076 Uiso 0.3333 1 calc R U P A -1 H9B H 0.6356 0.4866 0.4464 0.076 Uiso 0.3333 1 calc R U P A -1 H9C H 0.6834 0.5017 0.5019 0.076 Uiso 0.3333 1 calc R U P A -1 C10 C 0.5957(15) 0.4507(10) 0.5999(14) 0.054(6) Uani 0.3333 1 d . U P A -1 H10A H 0.6407 0.4506 0.6085 0.081 Uiso 0.3333 1 calc R U P A -1 H10B H 0.5851 0.4149 0.5733 0.081 Uiso 0.3333 1 calc R U P A -1 H10C H 0.5727 0.4477 0.6394 0.081 Uiso 0.3333 1 calc R U P A -1 C11 C 0.4730(14) 0.5268(13) 0.6464(12) 0.047(5) Uani 0.3333 1 d . U P A -1 H11A H 0.4894 0.4931 0.6728 0.071 Uiso 0.3333 1 calc R U P A -1 H11B H 0.4331 0.5139 0.6281 0.071 Uiso 0.3333 1 calc R U P A -1 H11C H 0.4668 0.5644 0.6719 0.071 Uiso 0.3333 1 calc R U P A -1 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 Os2 0.02370(12) 0.02370(12) 0.02370(12) -0.00312(8) -0.00312(8) -0.00312(8) U1 0.02398(12) 0.02398(12) 0.02398(12) -0.00276(8) -0.00276(8) -0.00276(8) Os1 0.02690(15) 0.03607(16) 0.02310(15) -0.00083(10) -0.00404(9) 0.00210(10) C004 0.034(4) 0.047(4) 0.033(4) 0.002(3) -0.002(3) 0.005(3) C005 0.032(4) 0.051(4) 0.027(3) -0.006(3) 0.001(3) 0.002(3) C006 0.054(5) 0.044(4) 0.023(3) 0.002(3) 0.000(3) 0.019(3) C008 0.036(4) 0.050(4) 0.029(4) 0.008(3) -0.005(3) -0.005(3) C00A 0.027(3) 0.059(5) 0.022(3) 0.004(3) -0.005(3) 0.009(3) C00B 0.098(8) 0.063(6) 0.030(4) 0.002(4) 0.001(5) 0.032(6) C00C 0.032(4) 0.109(9) 0.044(5) 0.010(5) -0.008(4) 0.007(5) C00D 0.037(4) 0.072(6) 0.063(6) 0.009(5) 0.015(4) 0.014(4) C00E 0.063(6) 0.055(6) 0.073(7) 0.004(5) -0.004(5) -0.017(5) C00F 0.053(5) 0.059(6) 0.051(5) -0.017(4) 0.004(4) -0.012(4) C2 0.028(8) 0.016(8) 0.025(7) -0.002(6) -0.006(6) -0.008(6) C3 0.029(9) 0.017(7) 0.025(9) -0.003(6) -0.007(6) 0.000(6) C4 0.018(8) 0.019(9) 0.023(9) -0.007(6) -0.007(7) 0.001(6) C5 0.020(10) 0.027(9) 0.029(9) 0.006(7) 0.005(8) 0.006(7) C6 0.013(7) 0.019(8) 0.024(9) -0.004(7) -0.001(7) -0.003(6) C7 0.027(8) 0.034(9) 0.061(15) -0.003(9) 0.002(9) 0.008(7) C8 0.056(14) 0.040(10) 0.030(8) 0.010(8) 0.000(8) 0.000(9) C9 0.040(10) 0.062(15) 0.051(12) -0.009(10) 0.011(9) 0.017(10) C10 0.077(15) 0.017(7) 0.067(13) 0.003(7) -0.039(11) -0.006(7) C11 0.057(12) 0.042(12) 0.043(9) -0.003(8) 0.012(9) -0.019(9) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0034 0.0017 'Calculated using XDISP in WinGX (Farrugia, 1999)' H H 0.0000 0.0000 'Calculated using XDISP in WinGX (Farrugia, 1999)' Os Os -1.2848 7.9466 'Calculated using XDISP in WinGX (Farrugia, 1999)' U U -10.9608 4.1580 'Calculated using XDISP in WinGX (Farrugia, 1999)' 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 C2 Os2 U1 148.1(8) . . ? C2 Os2 C4 63.7(10) . . ? C2 Os2 C5 62.8(10) . . ? C2 Os2 C6 35.9(9) . . ? C3 Os2 U1 148.9(8) . . ? C3 Os2 C2 41.1(9) . . ? C3 Os2 C4 35.9(10) . . ? C3 Os2 C5 61.9(10) . . ? C3 Os2 C6 62.6(10) . . ? C4 Os2 U1 146.4(9) . . ? C4 Os2 C5 36.8(9) . . ? C5 Os2 U1 144.1(8) . . ? C6 Os2 U1 146.7(9) . . ? C6 Os2 C4 61.3(7) . . ? C6 Os2 C5 37.3(10) . . ? Os2 U1 Os1 110.998(9) . 9 ? Os2 U1 Os1 110.998(9) . 5 ? Os2 U1 Os1 110.999(9) . . ? Os1 U1 Os1 107.902(9) 9 5 ? Os1 U1 Os1 107.903(9) 9 . ? Os1 U1 Os1 107.900(9) 5 . ? C004 Os1 U1 147.61(19) . . ? C005 Os1 U1 142.9(2) . . ? C005 Os1 C004 37.2(3) . . ? C005 Os1 C008 61.8(3) . . ? C006 Os1 U1 148.76(19) . . ? C006 Os1 C004 62.2(3) . . ? C006 Os1 C005 62.6(3) . . ? C006 Os1 C008 37.5(3) . . ? C008 Os1 U1 151.8(2) . . ? C008 Os1 C004 36.5(3) . . ? C00A Os1 U1 143.40(19) . . ? C00A Os1 C004 62.0(3) . . ? C00A Os1 C005 36.6(3) . . ? C00A Os1 C006 38.6(3) . . ? C00A Os1 C008 62.8(3) . . ? C005 C004 Os1 70.6(4) . . ? C005 C004 C00D 125.6(8) . . ? C008 C004 Os1 71.2(4) . . ? C008 C004 C005 108.0(7) . . ? C008 C004 C00D 126.3(8) . . ? C00D C004 Os1 126.4(6) . . ? C004 C005 Os1 72.2(4) . . ? C004 C005 C00F 124.3(7) . . ? C00A C005 Os1 71.0(4) . . ? C00A C005 C004 109.0(7) . . ? C00A C005 C00F 126.4(7) . . ? C00F C005 Os1 128.0(6) . . ? C008 C006 Os1 71.5(4) . . ? C008 C006 C00A 105.9(6) . . ? C008 C006 C00B 126.2(9) . . ? C00A C006 Os1 70.1(4) . . ? C00A C006 C00B 127.6(8) . . ? C00B C006 Os1 127.5(5) . . ? C004 C008 Os1 72.3(4) . . ? C004 C008 C006 109.0(7) . . ? C004 C008 C00E 126.3(8) . . ? C006 C008 Os1 70.9(4) . . ? C006 C008 C00E 124.3(8) . . ? C00E C008 Os1 128.7(6) . . ? C005 C00A Os1 72.4(4) . . ? C005 C00A C006 108.1(6) . . ? C005 C00A C00C 126.3(8) . . ? C006 C00A Os1 71.4(4) . . ? C006 C00A C00C 125.4(8) . . ? C00C C00A Os1 125.9(5) . . ? C006 C00B H00A 109.5 . . ? C006 C00B H00B 109.5 . . ? C006 C00B H00C 109.5 . . ? H00A C00B H00B 109.5 . . ? H00A C00B H00C 109.5 . . ? H00B C00B H00C 109.5 . . ? C00A C00C H00D 109.5 . . ? C00A C00C H00E 109.5 . . ? C00A C00C H00F 109.5 . . ? H00D C00C H00E 109.5 . . ? H00D C00C H00F 109.5 . . ? H00E C00C H00F 109.5 . . ? C004 C00D H00G 109.5 . . ? C004 C00D H00H 109.5 . . ? C004 C00D H00I 109.5 . . ? H00G C00D H00H 109.5 . . ? H00G C00D H00I 109.5 . . ? H00H C00D H00I 109.5 . . ? C008 C00E H00J 109.5 . . ? C008 C00E H00K 109.5 . . ? C008 C00E H00L 109.5 . . ? H00J C00E H00K 109.5 . . ? H00J C00E H00L 109.5 . . ? H00K C00E H00L 109.5 . . ? C005 C00F H00M 109.5 . . ? C005 C00F H00N 109.5 . . ? C005 C00F H00O 109.5 . . ? H00M C00F H00N 109.5 . . ? H00M C00F H00O 109.5 . . ? H00N C00F H00O 109.5 . . ? C3 C2 Os2 68.5(15) . . ? C6 C2 Os2 72.9(17) . . ? C6 C2 C3 104(3) . . ? C6 C2 C11 120(4) . . ? C11 C2 Os2 125.8(18) . . ? C11 C2 C3 136(4) . . ? C2 C3 Os2 70.5(15) . . ? C4 C3 Os2 75.5(18) . . ? C4 C3 C2 108(3) . . ? C4 C3 C10 138(4) . . ? C10 C3 Os2 123.8(19) . . ? C10 C3 C2 114(4) . . ? C3 C4 Os2 68.6(16) . . ? C3 C4 C5 110(2) . . ? C3 C4 C9 121(3) . . ? C5 C4 Os2 72.4(18) . . ? C5 C4 C9 129(4) . . ? C9 C4 Os2 127(2) . . ? C4 C5 Os2 70.8(19) . . ? C4 C5 C6 106(2) . . ? C4 C5 C8 122(3) . . ? C6 C5 Os2 69(2) . . ? C6 C5 C8 132(4) . . ? C8 C5 Os2 130(2) . . ? C2 C6 Os2 71.1(16) . . ? C2 C6 C5 113(2) . . ? C2 C6 C7 131(3) . . ? C5 C6 Os2 73.4(19) . . ? C5 C6 C7 116(3) . . ? C7 C6 Os2 125(2) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7B 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9B 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C3 C10 H10A 109.5 . . ? C3 C10 H10B 109.5 . . ? C3 C10 H10C 109.5 . . ? H10A C10 H10B 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C2 C11 H11A 109.5 . . ? C2 C11 H11B 109.5 . . ? C2 C11 H11C 109.5 . . ? H11A C11 H11B 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Os2 U1 2.9490(6) . ? Os2 C2 2.21(3) . ? Os2 C3 2.18(3) . ? Os2 C4 2.27(4) . ? Os2 C5 2.29(3) . ? Os2 C6 2.23(4) . ? U1 Os1 2.9501(4) 5 ? U1 Os1 2.9501(4) . ? U1 Os1 2.9501(4) 9 ? Os1 C004 2.255(8) . ? Os1 C005 2.234(7) . ? Os1 C006 2.233(7) . ? Os1 C008 2.240(7) . ? Os1 C00A 2.216(6) . ? C004 C005 1.432(11) . ? C004 C008 1.410(11) . ? C004 C00D 1.506(11) . ? C005 C00A 1.397(11) . ? C005 C00F 1.506(11) . ? C006 C008 1.440(11) . ? C006 C00A 1.469(12) . ? C006 C00B 1.473(12) . ? C008 C00E 1.554(12) . ? C00A C00C 1.502(11) . ? C00B H00A 0.9800 . ? C00B H00B 0.9800 . ? C00B H00C 0.9800 . ? C00C H00D 0.9800 . ? C00C H00E 0.9800 . ? C00C H00F 0.9800 . ? C00D H00G 0.9800 . ? C00D H00H 0.9800 . ? C00D H00I 0.9800 . ? C00E H00J 0.9800 . ? C00E H00K 0.9800 . ? C00E H00L 0.9800 . ? C00F H00M 0.9800 . ? C00F H00N 0.9800 . ? C00F H00O 0.9800 . ? C2 C3 1.54(4) . ? C2 C6 1.37(3) . ? C2 C11 1.52(4) . ? C3 C4 1.37(4) . ? C3 C10 1.48(4) . ? C4 C5 1.44(4) . ? C4 C9 1.52(4) . ? C5 C6 1.45(4) . ? C5 C8 1.51(4) . ? C6 C7 1.60(4) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? 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 Os2 C2 C3 C4 -66.6(17) . . . . ? Os2 C2 C3 C10 119(2) . . . . ? Os2 C2 C6 C5 62(2) . . . . ? Os2 C2 C6 C7 -120(3) . . . . ? Os2 C3 C4 C5 -61(2) . . . . ? Os2 C3 C4 C9 122(3) . . . . ? Os2 C4 C5 C6 -61(2) . . . . ? Os2 C4 C5 C8 126(3) . . . . ? Os2 C5 C6 C2 -60.7(19) . . . . ? Os2 C5 C6 C7 121(3) . . . . ? Os1 C004 C005 C00A -61.8(5) . . . . ? Os1 C004 C005 C00F 124.3(8) . . . . ? Os1 C004 C008 C006 61.8(5) . . . . ? Os1 C004 C008 C00E -125.5(8) . . . . ? Os1 C005 C00A C006 -62.9(5) . . . . ? Os1 C005 C00A C00C 122.1(8) . . . . ? Os1 C006 C008 C004 -62.7(5) . . . . ? Os1 C006 C008 C00E 124.5(8) . . . . ? Os1 C006 C00A C005 63.5(5) . . . . ? Os1 C006 C00A C00C -121.3(7) . . . . ? C004 C005 C00A Os1 62.6(5) . . . . ? C004 C005 C00A C006 -0.3(8) . . . . ? C004 C005 C00A C00C -175.3(7) . . . . ? C005 C004 C008 Os1 -61.3(5) . . . . ? C005 C004 C008 C006 0.5(8) . . . . ? C005 C004 C008 C00E 173.2(8) . . . . ? C008 C004 C005 Os1 61.7(5) . . . . ? C008 C004 C005 C00A -0.1(9) . . . . ? C008 C004 C005 C00F -174.0(7) . . . . ? C008 C006 C00A Os1 -63.0(5) . . . . ? C008 C006 C00A C005 0.6(8) . . . . ? C008 C006 C00A C00C 175.7(7) . . . . ? C00A C006 C008 Os1 62.0(5) . . . . ? C00A C006 C008 C004 -0.6(8) . . . . ? C00A C006 C008 C00E -173.5(7) . . . . ? C00B C006 C008 Os1 -123.4(7) . . . . ? C00B C006 C008 C004 174.0(7) . . . . ? C00B C006 C008 C00E 1.1(12) . . . . ? C00B C006 C00A Os1 122.5(8) . . . . ? C00B C006 C00A C005 -174.0(7) . . . . ? C00B C006 C00A C00C 1.2(12) . . . . ? C00D C004 C005 Os1 -121.4(8) . . . . ? C00D C004 C005 C00A 176.8(7) . . . . ? C00D C004 C005 C00F 2.9(12) . . . . ? C00D C004 C008 Os1 121.8(8) . . . . ? C00D C004 C008 C006 -176.4(8) . . . . ? C00D C004 C008 C00E -3.7(13) . . . . ? C00F C005 C00A Os1 -123.7(8) . . . . ? C00F C005 C00A C006 173.5(7) . . . . ? C00F C005 C00A C00C -1.6(13) . . . . ? C2 C3 C4 Os2 63.3(15) . . . . ? C2 C3 C4 C5 2(3) . . . . ? C2 C3 C4 C9 -175(3) . . . . ? C3 C2 C6 Os2 -61.9(14) . . . . ? C3 C2 C6 C5 0(3) . . . . ? C3 C2 C6 C7 178(3) . . . . ? C3 C4 C5 Os2 58.7(18) . . . . ? C3 C4 C5 C6 -2(2) . . . . ? C3 C4 C5 C8 -175(3) . . . . ? C4 C5 C6 Os2 62.0(19) . . . . ? C4 C5 C6 C2 1(2) . . . . ? C4 C5 C6 C7 -177(3) . . . . ? C6 C2 C3 Os2 65.1(16) . . . . ? C6 C2 C3 C4 -2(3) . . . . ? C6 C2 C3 C10 -176(3) . . . . ? C8 C5 C6 Os2 -126(4) . . . . ? C8 C5 C6 C2 173(4) . . . . ? C8 C5 C6 C7 -5(5) . . . . ? C9 C4 C5 Os2 -124(4) . . . . ? C9 C4 C5 C6 175(4) . . . . ? C9 C4 C5 C8 2(5) . . . . ? C10 C3 C4 Os2 -125(3) . . . . ? C10 C3 C4 C5 174(4) . . . . ? C10 C3 C4 C9 -3(5) . . . . ? C11 C2 C3 Os2 -120(3) . . . . ? C11 C2 C3 C4 174(3) . . . . ? C11 C2 C3 C10 -1(4) . . . . ? C11 C2 C6 Os2 122(2) . . . . ? C11 C2 C6 C5 -176(3) . . . . ? C11 C2 C6 C7 2(4) . . . . ? 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 -0.139 -0.139 0.861 204.3 23.1 ? 2 0.139 0.361 0.639 204.3 25.7 ? 3 0.139 0.139 0.139 204.3 21.7 ? 4 -0.139 0.639 0.361 204.3 21.7 ? 5 0.067 0.742 0.217 7.4 1.2 ? 6 0.067 0.758 0.717 7.4 0.0 ? 7 0.217 0.067 0.742 7.4 1.0 ? 8 0.217 0.433 0.242 7.4 0.0 ? 9 0.361 0.639 0.139 204.3 30.7 ? 10 0.361 0.861 0.639 204.3 21.7 ? 11 0.242 0.217 0.433 7.4 0.0 ? 12 0.242 0.283 0.933 7.4 0.6 ? 13 0.258 0.717 0.433 7.4 1.2 ? 14 0.258 0.783 0.933 7.4 0.0 ? 15 0.283 0.567 0.742 7.4 0.0 ? 16 0.283 0.933 0.242 7.4 1.1 ? 17 0.639 0.361 0.861 204.3 21.7 ? 18 0.639 0.139 0.361 204.3 25.9 ? 19 0.433 0.242 0.217 7.4 0.0 ? 20 0.433 0.258 0.717 7.4 0.5 ? 21 0.567 0.742 0.283 7.4 0.2 ? 22 0.567 0.758 0.783 7.4 1.4 ? 23 0.717 0.067 0.758 7.4 0.0 ? 24 0.717 0.433 0.258 7.4 1.2 ? 25 0.742 0.217 0.067 7.4 1.7 ? 26 0.742 0.283 0.567 7.4 0.0 ? 27 0.758 0.717 0.067 7.4 0.2 ? 28 0.758 0.783 0.567 7.4 1.1 ? 29 0.783 0.567 0.758 7.4 1.3 ? 30 0.783 0.933 0.258 7.4 0.0 ? 31 0.933 0.242 0.283 7.4 1.4 ? 32 0.933 0.258 0.783 7.4 0.0 ?