#------------------------------------------------------------------------------ #$Date: 2022-12-20 01:09:18 +0200 (Tue, 20 Dec 2022) $ #$Revision: 279935 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/56/81/1568133.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_1568133 loop_ _publ_author_name 'Ye, Christopher Z.' 'Del Rosal, Iker' 'Boreen, Michael' 'Ouellette, Erik T.' 'Russo, Dominic R.' 'Maron, Laurent' 'Arnold, John' 'Camp, Cl\'ement' _publ_section_title ; A Versatile Strategy for the Formation of Hydride-Bridged Actinide-Iridium Multimetallics ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D2SC04903A _journal_year 2023 _chemical_formula_moiety 'C40 H60 Ir4 U, C6 H14' _chemical_formula_sum 'C46 H74 Ir4 U' _chemical_formula_weight 1633.88 _chemical_melting_point 499 _chemical_name_systematic U{(\m-H)3IrCp*}4 _chemical_properties_physical Air-sensitive,Moisture-sensitive _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 _audit_creation_date 2022-08-05 _audit_creation_method ; Olex2 1.3 (compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408) ; _audit_update_record ; 2022-08-29 deposited with the CCDC. 2022-12-19 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 107.318(5) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 14.8239(6) _cell_length_b 21.1789(6) _cell_length_c 17.2427(8) _cell_measurement_reflns_used 16005 _cell_measurement_temperature 100.0 _cell_measurement_theta_max 29.6730 _cell_measurement_theta_min 3.1950 _cell_volume 5168.0(4) _computing_cell_refinement 'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)' _computing_data_collection 'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)' _computing_data_reduction 'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2014/7 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 100.0 _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 5.8140 _diffrn_detector_type 'Pilatus 200K' _diffrn_measured_fraction_theta_full 0.998 _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 -19.00 45.00 0.50 2.50 -- 2.33 77.00 -30.00 128 2 \w -20.00 15.00 0.50 2.50 -- 2.33 77.00 -90.00 70 3 \w -8.00 38.00 0.50 2.50 -- 2.33 77.00 90.00 92 4 \w -11.00 16.00 0.50 2.50 -- 2.33 -99.00 -60.00 54 5 \w -12.00 35.00 0.50 2.50 -- 2.33 -99.00-120.00 94 6 \w -12.00 25.00 0.50 2.50 -- 2.33 -99.00 30.00 74 7 \w -11.00 36.00 0.50 2.50 -- 2.33 -99.00 60.00 94 8 \w -25.00 0.00 0.50 2.50 -- 2.33 -93.00 97.00 50 9 \w -27.00 -2.00 0.50 2.50 -- -2.02 -93.00 97.00 50 10 \w -26.00 -1.00 0.50 2.50 -- -2.02 93.00-150.00 50 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'ROD, Synergy Custom DW system, Pilatus 200K' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0209561000 _diffrn_orient_matrix_UB_12 -0.0275919000 _diffrn_orient_matrix_UB_13 0.0104054000 _diffrn_orient_matrix_UB_21 -0.0453108000 _diffrn_orient_matrix_UB_22 0.0140593000 _diffrn_orient_matrix_UB_23 -0.0151920000 _diffrn_orient_matrix_UB_31 -0.0044380000 _diffrn_orient_matrix_UB_32 -0.0128049000 _diffrn_orient_matrix_UB_33 -0.0389425000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0472 _diffrn_reflns_av_unetI/netI 0.0262 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 31322 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.372 _diffrn_reflns_theta_min 3.135 _diffrn_source 'Rotating-anode X-ray tube' _diffrn_source_type 'Rigaku (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 13.411 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.13241 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.41.122a (Rigaku Oxford Diffraction, 2021) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour orange _exptl_crystal_colour_primary orange _exptl_crystal_density_diffrn 2.100 _exptl_crystal_description Rod _exptl_crystal_F_000 3000 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: n-hexane' _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _refine_diff_density_max 1.361 _refine_diff_density_min -2.043 _refine_diff_density_rms 0.254 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.389 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 290 _refine_ls_number_reflns 5280 _refine_ls_number_restraints 48 _refine_ls_restrained_S_all 1.382 _refine_ls_R_factor_all 0.0400 _refine_ls_R_factor_gt 0.0376 _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^)+269.2035P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0949 _refine_ls_wR_factor_ref 0.0956 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5003 _reflns_number_total 5280 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d2sc04903a2.cif _cod_data_source_block czy_ii_020_b _cod_database_code 1568133 _shelx_shelxl_version_number 2014/7 _chemical_oxdiff_formula 'U Ir4 C46 H74' _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 0.413 _shelx_estimated_absorpt_t_min 0.108 _reflns_odcompleteness_completeness 99.69 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Uiso/Uaniso restraints and constraints Uanis(C5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.1 Uanis(C3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.1 Uanis(C2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.1 Uanis(C8) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.1 Uanis(C7) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.1 Uanis(C13) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.1 Uanis(C9) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.1 Uanis(C10) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.1 Uanis(C5) = Uanis(C24) Uanis(C3) = Uanis(C23) Uanis(C2) = Uanis(C22) Uanis(C8) = Uanis(C26) Uanis(C7) = Uanis(C25) Uanis(C13) = Uanis(C18) Uanis(C9) = Uanis(C19) Uanis(C10) = Uanis(C15) 3. Others Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(H12C)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(H13C)= Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(H10C)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)= Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(H11C)=Sof(C26)=Sof(C22)=Sof(C23)=Sof(C24)= Sof(C25)=1-FVAR(1) Sof(C2)=Sof(C5)=Sof(C7)=Sof(C3)=Sof(C8)=Sof(C16)=Sof(H16A)=Sof(H16B)= Sof(H16C)=Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=Sof(C18)=Sof(H18A)=Sof(H18B)= Sof(H18C)=Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(H19C)=Sof(C17)=Sof(H17A)=Sof(H17B)= Sof(H17C)=FVAR(1) 4.a Secondary CH2 refined with riding coordinates: C4(H4A,H4B), C1(H1A,H1B) 4.b Idealised Me refined as rotating group: C20(H20A,H20B,H20C), C00C(H00A,H00B,H00C), C00L(H00D,H00E,H00F), C00X(H00G, H00H,H00I), C6(H6A,H6B,H6C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C10(H10A,H10B,H10C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C16(H16A,H16B,H16C), C15(H15A,H15B,H15C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C17(H17A,H17B, H17C), C14(H14A,H14B,H14C) ; _shelx_res_file ; czy_ii_020_b.res created by SHELXL-2014/7 TITL czy_ii_020_b_a.res in C2/c REM Old TITL CZY_II_020_b in C2/m REM SHELXT solution in C2/c REM R1 0.085, Rweak 0.011, Alpha 0.048, Orientation as input REM Formula found by SHELXT: C75 U5 CELL 0.71073 14.8239 21.1789 17.2427 90 107.318 90 ZERR 4 0.0006 0.0006 0.0008 0 0.005 0 LATT 7 SYMM -X,+Y,0.5-Z SFAC C H Ir U UNIT 184 296 16 4 EADP C5 C24 ISOR 0.01 0.1 C5 EADP C3 C23 ISOR 0.01 0.1 C3 EADP C2 C22 ISOR 0.01 0.1 C2 EADP C8 C26 ISOR 0.01 0.1 C8 EADP C7 C25 ISOR 0.01 0.1 C7 EADP C13 C18 ISOR 0.01 0.1 C13 EADP C9 C19 ISOR 0.01 0.1 C9 EADP C10 C15 ISOR 0.01 0.1 C10 L.S. 10 0 0 PLAN 50 SIZE 0.08 0.08 0.3 CONF BOND $H list 4 MORE -1 fmap 2 53 acta SHEL 1000 0.8 OMIT 1 1 2 REM REM REM WGHT 0.000000 269.203491 FVAR 0.08404 0.48276 U001 4 0.500000 0.244149 0.250000 10.50000 0.00839 0.00865 = 0.01144 0.00000 0.00536 0.00000 IR1 3 0.373431 0.156965 0.302367 11.00000 0.00956 0.01063 = 0.01488 0.00098 0.00620 -0.00137 IR 3 0.581809 0.329695 0.388144 11.00000 0.01235 0.01008 = 0.01115 -0.00086 0.00459 -0.00145 C005 1 0.552974 0.369232 0.496545 11.00000 0.01918 0.01923 = 0.01831 -0.00762 0.00863 0.00455 C006 1 0.646173 0.342012 0.522238 11.00000 0.01238 0.01939 = 0.01368 -0.00501 0.00100 -0.00522 C007 1 0.552418 0.419398 0.440229 11.00000 0.02951 0.01739 = 0.01267 -0.00884 0.00695 0.00135 C009 1 0.702565 0.376723 0.480511 11.00000 0.01460 0.01929 = 0.01654 -0.00805 0.00649 -0.00614 C20 1 0.469595 0.461022 0.398771 11.00000 0.04243 0.02004 = 0.03090 -0.00516 -0.00332 0.01354 AFIX 137 H20A 2 0.470082 0.469661 0.344242 11.00000 -1.50000 H20B 2 0.474109 0.499979 0.428148 11.00000 -1.50000 H20C 2 0.411858 0.439931 0.397525 11.00000 -1.50000 AFIX 0 C00C 1 0.810140 0.370570 0.496286 11.00000 0.02579 0.03729 = 0.02240 -0.00699 0.01793 -0.01173 AFIX 137 H00A 2 0.831350 0.331007 0.522578 11.00000 -1.50000 H00B 2 0.841640 0.404579 0.530547 11.00000 -1.50000 H00C 2 0.824431 0.372291 0.445559 11.00000 -1.50000 AFIX 0 C00I 1 0.644035 0.423972 0.431071 11.00000 0.03725 0.01612 = 0.02561 -0.00239 0.01412 -0.01090 C00L 1 0.471943 0.350361 0.527549 11.00000 0.01765 0.04497 = 0.02271 -0.00747 0.00848 0.00039 AFIX 137 H00D 2 0.413882 0.352633 0.484035 11.00000 -1.50000 H00E 2 0.468885 0.378482 0.570361 11.00000 -1.50000 H00F 2 0.481438 0.307946 0.548004 11.00000 -1.50000 AFIX 0 C00X 1 0.677178 0.472479 0.381184 11.00000 0.05885 0.02358 = 0.04190 -0.00443 0.02704 -0.02153 AFIX 137 H00G 2 0.721448 0.453306 0.357513 11.00000 -1.50000 H00H 2 0.707173 0.506851 0.415532 11.00000 -1.50000 H00I 2 0.623946 0.488065 0.338846 11.00000 -1.50000 AFIX 0 C4 1 0.131368 0.338854 0.247219 11.00000 0.09870 0.03887 = 0.06352 0.01163 0.04685 0.00631 AFIX 23 H4A 2 0.131418 0.298415 0.220819 11.00000 -1.20000 H4B 2 0.122316 0.371301 0.205901 11.00000 -1.20000 AFIX 0 C6 1 0.226180 0.348332 0.308093 11.00000 0.07890 0.04545 = 0.09174 0.00963 0.03668 0.02042 AFIX 137 H6A 2 0.274675 0.342065 0.282342 11.00000 -1.50000 H6B 2 0.234321 0.318540 0.351602 11.00000 -1.50000 H6C 2 0.230370 0.390471 0.329388 11.00000 -1.50000 AFIX 0 C1 1 0.048129 0.340521 0.281023 11.00000 0.08161 0.03224 = 0.04876 -0.00160 0.03255 0.00747 AFIX 23 H1A 2 0.052307 0.304210 0.316205 11.00000 -1.20000 H1B 2 0.053536 0.378020 0.314400 11.00000 -1.20000 AFIX 0 PART 2 C2 1 0.373965 0.062746 0.353285 21.00000 0.01632 0.01304 = 0.00862 -0.00013 0.00315 -0.00704 C5 1 0.271457 0.140529 0.369379 21.00000 0.01211 0.02016 = 0.01522 0.00162 0.00733 -0.00242 C7 1 0.232778 0.111714 0.290503 21.00000 0.00976 0.01477 = 0.01431 -0.00171 0.00883 -0.00442 C3 1 0.357731 0.109539 0.409830 21.00000 0.01783 0.01459 = 0.01605 0.00302 0.00930 0.00018 C8 1 0.295997 0.064341 0.280473 21.00000 0.01576 0.01569 = 0.01590 0.00787 0.00820 -0.00320 PART 3 C12 1 0.265782 0.179400 0.449662 -21.00000 0.04375 0.03210 = 0.02396 -0.00869 0.01716 -0.00317 AFIX 137 H12A 2 0.321845 0.200409 0.481803 -21.00000 -1.50000 H12B 2 0.239045 0.155251 0.484514 -21.00000 -1.50000 H12C 2 0.220725 0.210210 0.420808 -21.00000 -1.50000 AFIX 0 C13 1 0.133739 0.152031 0.268533 -21.00000 0.01324 0.04141 = 0.04199 0.01766 0.01296 -0.00154 AFIX 137 H13A 2 0.135656 0.197107 0.274663 -21.00000 -1.50000 H13B 2 0.091003 0.134537 0.295117 -21.00000 -1.50000 H13C 2 0.112480 0.141492 0.211830 -21.00000 -1.50000 AFIX 0 C10 1 0.423588 0.004020 0.329331 -21.00000 0.02323 0.01846 = 0.03163 0.00994 -0.00357 0.00044 AFIX 137 H10A 2 0.412351 -0.007116 0.273280 -21.00000 -1.50000 H10B 2 0.412028 -0.031991 0.358828 -21.00000 -1.50000 H10C 2 0.487976 0.017414 0.351843 -21.00000 -1.50000 AFIX 0 C9 1 0.236880 0.043281 0.191301 -21.00000 0.02355 0.02681 = 0.02498 -0.00075 -0.00870 -0.01570 AFIX 137 H9A 2 0.184310 0.067046 0.158199 -21.00000 -1.50000 H9B 2 0.216484 0.001320 0.198860 -21.00000 -1.50000 H9C 2 0.285485 0.041230 0.164984 -21.00000 -1.50000 AFIX 0 C11 1 0.442804 0.087746 0.487262 -21.00000 0.02913 0.02851 = 0.01203 0.00028 0.00083 -0.00723 AFIX 137 H11A 2 0.497467 0.066683 0.480815 -21.00000 -1.50000 H11B 2 0.417850 0.063894 0.523560 -21.00000 -1.50000 H11C 2 0.460225 0.129155 0.509283 -21.00000 -1.50000 AFIX 0 PART 2 C16 1 0.419102 0.120141 0.494666 21.00000 0.02488 0.03337 = 0.02153 0.00389 0.01598 -0.00676 AFIX 137 H16A 2 0.482750 0.107876 0.498957 21.00000 -1.50000 H16B 2 0.396228 0.095330 0.531458 21.00000 -1.50000 H16C 2 0.417819 0.164038 0.508175 21.00000 -1.50000 AFIX 0 C15 1 0.452954 0.014389 0.369931 21.00000 0.02323 0.01846 = 0.03163 0.00994 -0.00357 0.00044 AFIX 137 H15A 2 0.460406 0.000004 0.319396 21.00000 -1.50000 H15B 2 0.437623 -0.020782 0.398799 21.00000 -1.50000 H15C 2 0.510810 0.033350 0.402131 21.00000 -1.50000 AFIX 0 C18 1 0.132254 0.124179 0.236520 21.00000 0.01324 0.04141 = 0.04199 0.01766 0.01296 -0.00154 AFIX 137 H18A 2 0.122128 0.168872 0.229783 21.00000 -1.50000 H18B 2 0.087982 0.106605 0.261433 21.00000 -1.50000 H18C 2 0.123441 0.104898 0.184399 21.00000 -1.50000 AFIX 0 C19 1 0.280970 0.023432 0.207103 21.00000 0.02355 0.02681 = 0.02498 -0.00075 -0.00870 -0.01570 AFIX 137 H19A 2 0.242774 0.045509 0.160157 21.00000 -1.50000 H19B 2 0.249546 -0.014750 0.214397 21.00000 -1.50000 H19C 2 0.340936 0.013255 0.199619 21.00000 -1.50000 AFIX 0 C17 1 0.230353 0.189549 0.410520 21.00000 0.05283 0.03508 = 0.04030 0.00813 0.04054 0.00640 AFIX 137 H17A 2 0.278675 0.219040 0.437539 21.00000 -1.50000 H17B 2 0.205024 0.169833 0.449658 21.00000 -1.50000 H17C 2 0.180812 0.211432 0.370933 21.00000 -1.50000 AFIX 0 PART 3 C26 1 0.275698 0.075541 0.273938 -21.00000 0.01576 0.01569 = 0.01590 0.00787 0.00820 -0.00320 C22 1 0.360253 0.055420 0.335488 -21.00000 0.01632 0.01304 = 0.00862 -0.00013 0.00315 -0.00704 C23 1 0.368917 0.093243 0.405940 -21.00000 0.01783 0.01459 = 0.01605 0.00302 0.00930 0.00018 C24 1 0.290279 0.136310 0.390271 -21.00000 0.01211 0.02016 = 0.01522 0.00162 0.00733 -0.00242 C25 1 0.231372 0.125224 0.306261 -21.00000 0.00976 0.01477 = 0.01431 -0.00171 0.00883 -0.00442 PART 0 C14 1 0.681018 0.289945 0.581776 11.00000 0.02061 0.02741 = 0.01851 0.00056 0.00234 0.00450 AFIX 137 H14A 2 0.628763 0.264010 0.584075 11.00000 -1.50000 H14B 2 0.710918 0.307510 0.634507 11.00000 -1.50000 H14C 2 0.725819 0.264777 0.565098 11.00000 -1.50000 AFIX 0 HKLF 4 REM czy_ii_020_b_a.res in C2/c REM R1 = 0.0376 for 5003 Fo > 4sig(Fo) and 0.0400 for all 5280 data REM 290 parameters refined using 48 restraints END WGHT 0.0000 269.1703 REM Highest difference peak 1.361, deepest hole -2.043, 1-sigma level 0.254 Q1 1 0.3365 0.1877 0.3097 11.00000 0.05 1.36 Q2 1 0.4763 0.1621 0.3245 11.00000 0.05 1.31 Q3 1 0.4077 0.1839 0.2905 11.00000 0.05 1.27 Q4 1 0.3728 0.2973 0.3027 11.00000 0.05 1.20 Q5 1 0.3804 0.0194 0.1178 11.00000 0.05 1.17 Q6 1 0.7399 0.3773 0.3621 11.00000 0.05 1.16 Q7 1 0.2198 0.1031 0.3362 11.00000 0.05 1.13 Q8 1 0.4593 0.0977 0.2602 11.00000 0.05 1.11 Q9 1 0.3963 0.1250 0.3357 11.00000 0.05 1.10 Q10 1 0.4761 0.2090 0.2274 11.00000 0.05 1.10 Q11 1 0.5982 0.2395 0.3650 11.00000 0.05 1.09 Q12 1 0.3645 0.1214 0.2749 11.00000 0.05 1.07 Q13 1 0.4778 0.2649 0.4246 11.00000 0.05 1.06 Q14 1 0.5615 0.2990 0.3586 11.00000 0.05 1.05 Q15 1 0.4261 0.2779 0.4592 11.00000 0.05 1.03 Q16 1 0.6516 0.4422 0.5255 11.00000 0.05 0.98 Q17 1 0.5580 0.4028 0.5576 11.00000 0.05 0.98 Q18 1 0.3559 0.3418 0.4825 11.00000 0.05 0.97 Q19 1 0.2633 0.1003 0.3773 11.00000 0.05 0.97 Q20 1 0.1622 0.0053 0.2244 11.00000 0.05 0.95 Q21 1 0.4948 0.4448 0.2855 11.00000 0.05 0.94 Q22 1 0.4806 0.0453 0.4581 11.00000 0.05 0.94 Q23 1 0.3798 0.1605 0.2187 11.00000 0.05 0.93 Q24 1 0.0393 0.2461 0.2596 11.00000 0.05 0.92 Q25 1 0.4995 0.3214 0.3144 11.00000 0.05 0.92 Q26 1 0.7483 0.3170 0.5162 11.00000 0.05 0.91 Q27 1 0.6965 0.5336 0.4828 11.00000 0.05 0.90 Q28 1 0.5572 0.3639 0.3437 11.00000 0.05 0.90 Q29 1 0.4695 0.3223 0.3594 11.00000 0.05 0.90 Q30 1 0.6244 0.3316 0.3133 11.00000 0.05 0.89 Q31 1 0.4327 0.1832 0.3608 11.00000 0.05 0.88 Q32 1 0.9245 0.3801 0.6126 11.00000 0.05 0.87 Q33 1 0.0393 0.2597 0.2729 11.00000 0.05 0.87 Q34 1 0.4229 0.5048 0.3171 11.00000 0.05 0.85 Q35 1 0.5454 0.5430 0.3764 11.00000 0.05 0.82 Q36 1 0.2930 0.4606 0.4420 11.00000 0.05 0.82 Q37 1 0.5356 0.0046 0.3800 11.00000 0.05 0.81 Q38 1 0.2564 0.1022 0.4598 11.00000 0.05 0.79 Q39 1 0.3255 0.0882 0.4785 11.00000 0.05 0.79 Q40 1 0.3226 0.2872 0.3371 11.00000 0.05 0.79 Q41 1 0.5385 0.3959 0.2713 11.00000 0.05 0.77 Q42 1 0.3252 0.0004 0.4978 11.00000 0.05 0.76 Q43 1 0.6020 0.2909 0.4167 11.00000 0.05 0.76 Q44 1 0.0800 0.3985 0.2812 11.00000 0.05 0.76 Q45 1 0.3255 0.0743 0.3137 11.00000 0.05 0.76 Q46 1 0.3433 0.3808 0.3181 11.00000 0.05 0.75 Q47 1 0.1649 0.1832 0.2188 11.00000 0.05 0.75 Q48 1 0.8137 0.2319 0.6464 11.00000 0.05 0.75 Q49 1 0.5829 0.3769 0.4245 11.00000 0.05 0.75 Q50 1 0.9281 0.3058 0.5784 11.00000 0.05 0.75 ; _shelx_res_checksum 77808 _shelx_hkl_file ; 0 0 -3 6.76 2.16 0 0 -4 29.23 3.32 0 0 4 27.63 2.36 0 0 5 35.64 3.93 0 0 -5 44.07 4.47 0 0 5 38.99 3.09 0 0 6 615.01 20.40 0 0 -6 649.22 20.50 0 0 6 620.08 21.23 0 0 6 646.36 20.13 0 0 7 10.20 4.78 0 0 7 9.75 4.17 0 0 7 13.98 3.32 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596.55 22.97 0 -10 16 450.99 23.02 0 10 16 482.92 21.96 0 10 16 501.53 22.19 0 -10 16 526.44 22.55 0 10 16 521.23 22.07 0 10 16 501.30 24.94 0 10 16 432.93 24.04 0 10 16 461.20 22.81 0 10 -17 228.77 18.05 0 10 17 223.41 20.43 0 10 17 108.45 13.09 0 10 17 206.56 14.58 0 -10 17 178.19 14.59 0 -10 17 151.57 15.26 0 10 17 198.65 15.17 0 10 17 195.43 15.09 0 -10 17 173.24 14.88 0 10 17 202.53 15.13 0 -10 17 205.56 15.67 0 10 17 250.39 18.65 0 10 17 218.46 17.95 0 10 17 170.76 14.88 0 10 -18 443.01 21.87 0 10 18 395.04 25.35 0 10 18 299.96 18.29 0 10 18 179.49 17.30 0 10 18 301.86 19.29 0 -10 18 322.46 20.18 0 10 18 348.37 20.60 0 -10 18 362.93 20.24 0 10 18 343.21 19.81 0 -10 18 426.68 20.98 0 -10 18 377.59 20.40 0 10 18 236.17 21.91 0 10 19 295.03 23.22 0 10 19 238.67 17.93 0 10 19 246.31 16.69 0 10 19 241.75 16.57 0 10 20 291.81 19.98 0 10 20 518.65 28.35 0 12 0 6301.96 191.46 0 12 0 6822.40 191.29 0 12 1 1336.79 44.65 0 12 1 1373.69 43.57 0 -12 -2 1286.20 40.61 0 -12 2 1203.15 40.53 0 12 2 1189.71 39.79 0 -12 -2 1273.45 38.25 0 -12 -2 1257.99 39.68 0 -12 3 166.67 7.76 0 12 3 163.56 9.42 0 -12 -3 165.36 9.53 0 -12 3 173.37 10.01 0 -12 3 151.37 6.41 0 12 3 165.29 5.78 0 12 3 164.56 5.80 0 -12 -3 158.02 8.40 0 -12 -3 163.73 9.45 0 -12 -4 34.23 4.67 0 -12 4 40.02 4.25 0 12 4 42.32 5.94 0 -12 -4 40.94 5.77 0 -12 4 43.38 6.33 0 12 4 42.82 3.24 0 12 4 39.08 3.22 0 12 4 40.43 3.64 0 -12 4 42.06 3.33 0 -12 4 41.35 3.97 0 -12 4 39.65 3.29 0 -12 -4 39.48 6.14 0 -12 -4 41.58 5.54 0 -12 5 5.26 3.15 0 12 5 4.66 4.89 0 -12 5 4.17 5.66 0 12 5 2.10 5.17 0 -12 -5 4.56 4.54 0 -12 -5 7.01 3.93 0 12 5 4.25 2.97 0 12 5 4.69 2.92 0 -12 5 3.50 2.99 0 -12 5 4.07 3.01 0 -12 5 2.20 3.69 0 12 5 4.68 3.32 0 -12 -5 3.79 4.77 0 -12 -5 1.35 5.48 0 -12 6 585.99 19.78 0 -12 -6 634.80 22.64 0 -12 6 641.44 23.83 0 12 6 674.18 24.01 0 -12 -6 567.60 20.84 0 12 6 592.24 19.91 0 -12 6 659.61 20.70 0 12 6 624.58 20.02 0 -12 -6 617.20 21.90 0 12 6 617.57 19.98 0 -12 6 599.65 19.89 0 -12 6 603.82 19.90 0 -12 -6 656.64 23.32 0 -12 -7 0.50 4.31 0 -12 7 -2.27 5.77 0 12 7 -2.50 6.05 0 -12 -7 -0.22 5.15 0 -12 7 4.93 5.00 0 12 7 8.75 4.27 0 -12 7 3.77 4.26 0 -12 -7 3.48 5.80 0 12 7 4.99 3.99 0 -12 -7 1.02 5.96 0 -12 8 228.59 13.33 0 12 8 238.68 13.37 0 -12 -8 222.97 12.15 0 -12 8 265.17 11.57 0 12 8 238.01 10.71 0 -12 -8 243.65 12.72 0 12 8 278.88 11.11 0 -12 8 220.67 10.59 0 12 8 284.11 13.29 0 -12 -8 221.80 12.75 0 12 8 251.49 12.25 0 12 -9 51.54 5.44 0 -12 -9 58.19 7.16 0 -12 9 60.23 8.71 0 12 9 55.05 8.34 0 -12 -9 63.50 8.34 0 -12 9 65.51 6.61 0 -12 9 68.21 7.34 0 12 9 64.49 6.61 0 12 9 102.59 7.37 0 12 9 71.53 8.29 0 12 9 89.81 8.58 0 12 -10 485.42 17.13 0 12 -10 480.58 21.25 0 12 10 478.05 20.72 0 -12 10 482.25 18.70 0 12 10 447.04 18.11 0 12 10 511.66 18.10 0 -12 -10 473.45 20.26 0 -12 10 456.48 18.23 0 12 10 507.44 20.33 0 12 10 465.41 19.60 0 12 -11 332.80 18.44 0 12 11 337.92 17.27 0 -12 11 367.83 15.74 0 12 11 360.97 14.96 0 -12 11 379.26 16.14 0 12 11 335.69 15.42 0 12 11 328.68 17.08 0 12 -11 370.85 14.14 0 12 11 379.08 17.48 0 12 -12 291.92 17.82 0 12 12 298.17 16.09 0 12 12 252.86 13.78 0 12 12 280.32 13.38 0 -12 12 262.06 14.32 0 -12 12 253.19 14.01 0 12 12 318.18 16.08 0 12 12 282.61 15.82 0 12 -12 309.41 12.76 0 12 -13 3.99 12.37 0 12 13 -1.72 6.36 0 12 13 7.74 7.92 0 -12 13 8.80 8.09 0 12 13 1.54 7.88 0 12 13 -1.53 7.37 0 -12 13 2.95 8.53 0 12 13 3.87 9.29 0 12 -13 10.03 5.58 0 12 13 10.94 8.73 0 12 13 9.87 9.14 0 12 -14 1027.69 36.39 0 12 14 894.31 32.56 0 12 14 1056.68 36.68 0 -12 14 925.04 33.87 0 -12 14 900.52 33.63 0 -12 14 903.47 33.75 0 12 14 929.08 34.01 0 12 14 958.80 34.14 0 12 14 933.00 33.06 0 12 14 1046.85 36.17 0 12 14 935.17 36.14 0 12 -14 1017.19 31.83 0 12 14 954.61 36.81 0 12 15 152.65 18.62 0 12 -15 206.56 16.97 0 12 15 154.53 13.68 0 12 15 145.36 12.65 0 -12 15 194.62 14.08 0 12 15 166.57 12.83 0 12 15 147.84 12.83 0 -12 15 182.98 13.54 0 -12 15 177.77 13.40 0 12 15 161.03 14.92 0 12 15 143.59 14.62 0 12 15 182.82 14.37 0 12 16 534.60 28.82 0 12 16 383.34 20.40 0 12 -16 566.62 25.29 0 12 16 483.13 23.48 0 -12 16 550.92 23.07 0 12 16 496.93 22.71 0 12 16 473.33 21.74 0 12 16 459.08 22.30 0 -12 16 436.00 22.46 0 -12 16 492.83 22.78 0 12 16 550.20 26.01 0 12 16 546.24 23.98 0 12 16 566.39 25.73 0 12 -17 125.43 17.16 0 12 17 124.33 19.79 0 12 17 90.88 12.40 0 12 17 51.26 10.62 0 -12 17 98.96 13.06 0 -12 17 129.61 14.03 0 -12 17 90.01 13.30 0 -12 17 136.23 13.51 0 12 17 93.64 12.59 0 12 17 113.66 13.23 0 12 17 103.36 12.86 0 12 17 69.48 14.39 0 12 17 112.02 15.69 0 12 18 22.76 18.40 0 12 -18 40.17 15.50 0 -12 18 17.93 11.68 0 12 18 5.29 11.60 0 -12 18 13.58 11.71 0 -12 18 2.56 11.56 0 -12 18 31.68 12.45 0 12 18 1.40 11.68 0 12 18 21.88 11.65 0 12 18 25.03 10.72 0 12 18 8.98 9.32 0 12 19 96.71 22.55 0 12 19 110.52 14.43 0 -12 19 110.98 14.95 0 12 19 117.56 13.76 0 14 0 691.83 26.14 0 14 1 362.55 17.61 0 -14 -1 361.37 13.99 0 -14 2 16.48 6.10 0 -14 -2 16.02 5.66 0 14 2 10.11 5.81 0 -14 -2 18.18 6.07 0 -14 -2 19.98 4.98 0 -14 3 1757.28 55.11 0 -14 -3 1717.58 54.53 0 14 3 1625.51 53.55 0 -14 -3 1713.62 52.26 0 -14 -3 1768.76 54.01 0 14 4 169.52 10.45 0 -14 -4 167.09 8.81 0 -14 4 172.35 11.10 0 -14 -4 180.28 10.58 0 -14 4 157.57 7.13 0 14 4 168.63 6.39 0 -14 -4 171.16 9.26 0 -14 -4 176.85 10.72 0 -14 5 212.45 9.09 0 14 5 198.20 11.61 0 -14 5 208.49 12.18 0 -14 -5 183.44 9.54 0 14 5 201.13 12.50 0 -14 -5 182.68 11.10 0 -14 5 205.54 7.97 0 14 5 194.56 7.84 0 -14 5 207.22 8.68 0 -14 -5 214.23 10.76 0 14 5 193.78 7.82 0 14 5 191.58 8.25 0 -14 5 209.99 8.02 0 -14 -5 209.90 11.98 0 14 6 860.03 31.31 0 -14 6 878.66 28.24 0 14 6 951.48 33.01 0 -14 6 906.25 32.55 0 -14 -6 911.78 31.52 0 -14 6 956.29 28.65 0 14 6 871.30 27.75 0 -14 6 895.06 27.83 0 14 6 875.40 27.75 0 -14 -6 918.32 30.40 0 -14 6 879.77 27.84 0 14 6 935.07 28.18 0 -14 -6 919.39 32.22 0 14 7 1066.18 36.14 0 -14 7 985.45 32.55 0 14 7 1094.64 37.62 0 -14 -7 1036.19 35.99 0 -14 7 1101.58 37.67 0 14 7 1115.48 33.18 0 -14 7 1059.06 33.03 0 -14 7 1195.16 33.90 0 14 7 1033.68 32.94 0 -14 -7 1087.11 35.59 0 14 7 1023.91 32.87 0 -14 7 1045.63 32.91 0 -14 -7 1082.61 37.04 0 -14 8 1375.62 44.20 0 14 8 1547.14 49.77 0 -14 8 1484.50 49.37 0 -14 -8 1472.32 47.95 0 -14 -8 1564.65 48.01 0 -14 8 1453.05 45.17 0 14 8 1591.69 45.31 0 -14 8 1643.88 46.01 0 14 8 1411.35 44.98 0 14 8 1380.02 45.06 0 -14 8 1492.45 45.09 0 -14 -8 1459.48 48.94 0 -14 9 249.41 10.40 0 -14 9 265.49 15.35 0 14 9 289.40 15.75 0 -14 -9 273.00 14.02 0 -14 9 250.13 11.88 0 -14 9 315.31 13.28 0 -14 -9 261.94 14.61 0 -14 9 263.05 12.04 0 14 9 260.46 12.01 0 14 9 303.80 12.43 0 14 9 276.39 12.13 0 14 -10 26.24 5.37 0 -14 10 23.53 7.87 0 -14 -10 18.00 6.90 0 14 10 21.80 8.27 0 14 10 21.97 6.32 0 -14 10 25.54 7.15 0 14 10 29.69 6.33 0 -14 -10 13.30 8.09 0 -14 10 25.91 6.43 0 -14 10 20.35 5.87 0 14 10 23.57 6.45 0 14 10 18.96 8.10 0 14 -11 10.71 12.24 0 -14 11 23.16 8.45 0 14 11 21.85 8.69 0 -14 11 20.01 6.83 0 -14 11 17.92 6.57 0 -14 11 15.15 7.26 0 14 11 21.90 7.15 0 14 11 25.95 6.97 0 14 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9.61 0 14 15 38.12 11.89 0 14 15 44.31 11.82 0 14 15 28.95 10.44 0 14 -16 94.95 16.72 0 14 16 88.30 19.49 0 -14 16 71.63 10.91 0 14 16 80.24 12.86 0 -14 16 54.39 11.79 0 14 16 77.02 11.69 0 14 16 72.80 11.26 0 -14 16 62.48 11.94 0 -14 16 58.53 11.69 0 14 16 76.77 11.63 0 14 16 80.10 14.21 0 14 16 74.02 14.31 0 14 -17 774.45 30.15 0 14 17 718.67 35.43 0 -14 17 582.37 27.03 0 -14 17 665.09 27.55 0 14 17 552.77 26.72 0 -14 17 543.95 28.20 0 -14 17 633.08 27.34 0 14 17 738.41 27.50 0 14 17 592.06 27.21 0 14 17 626.13 29.31 0 -14 17 689.85 28.34 0 14 18 113.96 23.36 0 14 18 95.19 14.89 0 14 18 65.51 12.69 0 -14 18 133.02 14.56 0 14 19 608.72 29.56 0 14 19 628.19 28.76 0 -14 19 665.07 29.25 0 -16 1 85.80 8.99 0 16 1 105.90 9.66 0 -16 -1 86.47 7.23 0 -16 -2 116.54 9.84 0 -16 2 114.39 9.86 0 16 2 135.03 10.31 0 -16 -2 115.93 8.12 0 -16 -2 107.62 9.49 0 -16 3 1150.26 40.14 0 -16 -3 1153.81 39.59 0 16 3 1114.87 38.70 0 -16 -3 1184.18 37.06 0 -16 -3 1164.36 39.01 0 -16 4 126.16 10.70 0 -16 -4 117.96 9.73 0 16 4 127.64 9.71 0 -16 -4 111.20 8.02 0 -16 -4 128.53 9.01 0 -16 -4 129.86 10.32 0 16 5 381.93 17.45 0 -16 -5 374.73 17.29 0 16 5 380.07 18.88 0 -16 5 360.96 18.08 0 -16 -5 359.32 15.21 0 -16 -5 389.28 16.01 0 -16 -5 412.90 18.09 0 16 6 331.11 16.11 0 -16 6 307.10 16.71 0 -16 -6 286.36 13.69 0 16 6 327.00 17.59 0 -16 -6 324.91 16.01 0 16 6 315.03 11.55 0 16 6 315.56 11.58 0 -16 -6 307.12 14.82 0 -16 6 350.58 11.84 0 -16 6 348.99 11.83 0 -16 6 324.70 12.61 0 -16 -6 320.52 16.84 0 16 7 545.72 22.54 0 -16 7 554.55 18.81 0 -16 7 541.54 23.43 0 16 7 589.31 24.57 0 -16 -7 544.67 22.38 0 -16 -7 497.08 20.42 0 -16 -7 579.97 21.76 0 16 7 540.00 18.35 0 -16 7 559.39 18.57 0 -16 7 546.11 18.54 0 16 7 521.17 18.28 0 -16 7 605.83 19.57 0 16 7 530.99 18.77 0 -16 -7 574.10 23.45 0 -16 8 997.98 30.81 0 16 8 982.33 34.98 0 -16 -8 888.83 33.17 0 16 8 1031.49 36.89 0 -16 8 1046.23 36.45 0 -16 8 992.61 31.19 0 16 8 917.26 30.89 0 -16 -8 976.61 34.34 0 -16 8 1025.56 31.25 0 16 8 979.05 31.22 0 -16 8 1073.86 32.08 0 16 8 929.13 30.86 0 -16 -8 965.29 35.78 0 16 9 11.97 8.20 0 -16 9 9.06 4.27 0 16 9 5.86 8.88 0 -16 9 10.56 8.11 0 -16 -9 5.99 7.10 0 -16 9 3.67 5.57 0 -16 -9 18.59 8.66 0 16 9 6.60 5.56 0 -16 9 6.71 5.65 0 -16 9 10.25 6.69 0 16 9 6.80 5.65 0 16 9 17.16 6.02 0 -16 -9 9.78 8.32 0 16 10 1386.76 48.01 0 -16 10 1307.96 43.14 0 -16 10 1514.07 45.24 0 -16 10 1616.80 46.16 0 -16 -10 1565.57 48.61 0 16 10 1321.83 44.78 0 16 10 1421.50 45.14 0 16 10 1441.67 44.95 0 -16 10 1419.94 45.08 0 -16 10 1506.39 49.94 0 -16 -10 1539.86 48.33 0 16 10 1553.97 50.69 0 16 -11 1044.09 33.04 0 16 11 967.14 35.77 0 -16 11 897.38 30.61 0 -16 11 1043.55 37.57 0 16 11 1061.74 38.52 0 -16 11 1043.97 33.40 0 16 11 940.83 32.73 0 -16 11 1040.88 34.02 0 -16 -11 1044.95 36.32 0 -16 11 1057.36 33.47 0 16 11 960.99 33.09 0 16 11 996.30 33.40 0 16 12 843.80 31.95 0 -16 12 748.63 26.51 0 16 -12 896.16 34.20 0 -16 12 861.99 33.48 0 16 12 960.76 35.23 0 16 12 863.12 30.15 0 16 12 904.29 30.18 0 -16 12 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226.25 10.80 -10 10 3 32.69 6.72 10 10 -3 21.55 8.70 -10 -10 3 20.33 5.93 -10 10 3 8.46 2.23 -10 10 2 196.85 11.27 10 10 -2 173.37 12.20 -10 -10 2 172.70 14.35 -10 10 1 3.48 5.82 10 10 -1 -1.42 9.57 -10 -10 1 8.56 8.59 -10 10 0 209.84 11.18 10 10 0 182.53 13.41 -10 -10 0 168.69 13.82 10 10 1 604.50 24.83 -10 10 -1 653.57 23.06 -10 -10 -1 608.10 24.83 -10 10 -1 599.27 23.46 -10 -10 -1 625.90 23.77 -10 10 -1 601.94 23.45 -10 -10 -1 630.05 23.73 -10 -10 -1 626.54 26.51 10 10 2 1222.75 42.28 -10 10 -2 1157.53 43.18 -10 -10 -2 1225.71 41.72 -10 10 -2 1314.69 40.29 -10 10 -2 1248.90 41.08 -10 -10 -2 1215.91 40.86 -10 10 -2 1227.57 40.93 -10 -10 -2 1226.68 40.84 -10 -10 -2 1238.52 44.29 -10 10 -3 16.76 12.34 10 10 3 -2.57 12.38 -10 10 -3 8.86 5.60 -10 -10 -3 9.92 6.39 -10 10 -3 4.13 7.21 -10 -10 -3 3.55 7.75 -10 10 -3 6.83 7.29 -10 -10 -3 6.45 8.11 -10 -10 -3 2.79 8.65 -10 10 -4 871.14 34.16 10 10 4 840.32 33.42 -10 -10 -4 797.02 30.20 -10 10 -4 866.12 31.21 -10 -10 -4 892.16 31.29 -10 10 -4 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19.83 10 12 -14 1913.67 64.58 -10 12 14 1978.14 65.38 -10 12 14 1969.02 62.29 -10 12 14 2056.17 61.68 10 12 -13 747.45 28.90 -10 12 13 727.75 29.07 10 -12 -13 688.80 28.20 -10 12 13 710.36 29.40 10 -12 -13 699.35 29.99 10 12 -13 683.76 29.18 -10 12 13 656.26 25.58 -10 12 13 689.90 24.68 -10 12 12 1535.62 51.50 10 -12 -12 1530.65 51.06 -10 12 12 1527.83 52.28 10 -12 -12 1536.99 51.95 10 12 -12 1523.89 51.60 -10 12 12 1464.69 47.81 -10 12 12 1520.90 46.95 -10 12 11 150.79 12.70 10 -12 -11 143.06 13.84 10 12 -11 151.20 13.38 -10 12 11 141.55 9.55 10 -12 -11 159.20 12.22 -10 12 11 158.21 13.30 -10 12 10 27.54 9.17 10 -12 -10 23.60 10.79 10 -12 -10 37.33 11.02 10 12 -10 22.01 9.50 -10 12 10 30.28 6.32 -10 12 10 25.59 8.91 10 -12 -10 30.27 8.41 -10 12 9 36.55 9.48 10 12 -9 37.02 2.74 10 -12 -9 52.08 11.73 10 -12 -9 45.81 10.68 10 12 -9 48.90 10.44 -10 12 9 42.70 5.74 -10 -12 9 51.61 7.53 -10 12 9 48.86 9.26 -10 12 8 20.37 8.56 10 -12 -8 20.49 10.81 10 12 -8 15.44 9.98 -10 12 8 12.36 4.60 10 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4.76 10.92 -15 -15 2 10.05 11.37 -15 15 2 4.35 10.64 -15 -15 2 4.97 11.00 -15 -15 2 -13.65 21.83 -15 -15 1 30.36 11.84 -15 15 1 24.80 11.40 -15 -15 1 17.87 11.93 -15 15 1 25.24 11.02 -15 -15 1 27.03 11.93 -15 -15 1 36.77 23.53 -15 15 0 143.32 14.77 -15 -15 0 165.55 15.82 -15 15 0 161.91 14.87 -15 -15 0 171.62 15.14 15 15 1 30.32 17.16 -15 15 -1 11.85 11.52 -15 -15 -1 32.78 12.54 -15 15 -1 25.95 11.91 -15 -15 -1 27.00 12.83 -15 -15 -1 27.05 22.46 15 15 2 561.99 29.35 -15 -15 -2 557.78 25.81 15 15 3 45.17 19.37 -15 15 -3 71.00 13.31 -15 -15 -3 52.94 13.61 -15 -15 -3 54.09 21.34 -15 15 -4 -3.91 12.42 -15 -15 -4 -0.78 12.37 15 17 -12 767.96 32.36 15 17 -11 788.78 33.02 15 17 -10 31.11 13.41 15 17 -9 96.00 15.37 -15 17 8 1.98 12.16 15 17 -8 -10.82 13.70 -15 17 7 127.78 15.44 -15 -17 7 185.48 30.81 -15 17 6 207.73 17.91 -15 -17 6 338.00 37.52 -15 17 5 115.45 14.37 -15 -17 5 133.99 31.76 -15 17 4 13.12 11.16 -15 -17 4 31.17 28.25 -15 17 3 86.78 13.18 -15 17 3 76.41 12.25 -15 -17 3 103.19 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30.72 11.21 -18 8 6 282.18 17.29 18 -8 -6 254.23 16.55 18 -8 -5 625.16 25.85 -18 8 4 26.33 16.51 18 -8 -4 13.88 9.74 -18 8 3 1217.67 45.84 -18 8 2 90.59 18.86 18 -10 -11 154.50 15.58 -18 10 10 414.83 23.49 18 -10 -10 354.86 21.08 -18 10 9 39.95 12.70 18 -10 -9 28.59 11.37 -18 10 8 14.90 11.45 18 -10 -8 24.34 11.43 -18 10 7 116.59 13.29 18 -10 -7 104.67 12.68 18 -10 -6 64.72 11.55 -18 10 4 53.65 18.57 -18 12 9 16.52 12.88 -18 12 8 43.22 12.15 19 -1 -12 101.99 15.46 19 -1 -11 1794.62 60.91 19 1 -11 1783.26 60.33 19 -1 -10 91.17 14.99 19 1 -10 71.84 13.73 19 -1 -10 79.04 13.86 19 -1 -9 234.84 17.65 19 1 -9 238.27 17.82 19 1 -8 207.54 16.51 19 -1 -8 191.01 15.99 19 -1 -7 18.37 11.45 19 1 -7 26.43 11.89 19 -1 -6 7.31 9.60 19 -1 -6 6.68 10.73 19 1 -6 -11.34 11.94 19 -1 -5 164.21 12.96 19 1 -5 166.15 15.68 19 -1 -5 162.43 14.87 19 1 -4 385.52 20.70 19 -1 -4 348.83 19.50 -19 1 4 310.94 21.99 -19 -1 4 332.55 23.95 19 -1 -3 51.68 11.55 19 1 -3 34.69 11.98 -19 1 3 28.93 13.39 -19 -1 3 41.97 14.91 19 -1 -2 35.97 10.88 19 1 -2 46.80 11.60 -19 1 2 47.09 13.23 -19 -1 2 43.04 14.93 19 1 -1 341.77 18.24 -19 1 1 274.14 20.05 -19 -1 1 293.30 21.72 -19 -1 0 3.04 13.61 -19 -1 -1 7.95 13.01 -19 -1 -2 25.43 13.84 19 -3 -14 676.51 30.89 19 -3 -13 64.63 15.16 19 -3 -12 50.96 14.71 19 -3 -11 118.65 16.22 19 -3 -10 134.16 16.73 19 3 -10 123.23 14.64 19 -3 -10 100.31 14.09 19 -3 -9 85.51 14.80 19 -3 -9 88.66 13.35 19 3 -8 691.10 30.45 19 -3 -8 677.56 29.50 19 3 -7 137.05 15.32 19 -3 -7 124.48 14.30 19 3 -6 -3.58 11.76 19 -3 -6 0.72 10.66 19 3 -5 195.75 16.08 19 -3 -5 154.80 14.76 19 -3 -4 899.53 34.48 19 3 -4 976.74 36.74 19 -3 -4 930.91 35.03 19 -3 -3 154.68 13.32 19 3 -3 192.79 15.99 19 -3 -3 167.04 14.19 -19 -3 3 144.84 19.63 19 3 -2 183.00 15.60 -19 -3 2 158.21 19.85 19 3 -1 182.82 15.69 -19 -3 1 164.43 19.84 19 3 0 5.27 11.37 -19 -3 0 16.07 14.95 -19 5 11 557.24 28.80 -19 5 10 6.13 13.16 19 -5 -10 -8.36 12.44 -19 5 9 7.44 12.72 19 -5 -9 12.53 12.69 -19 5 8 275.50 18.79 19 -5 -8 265.78 18.24 19 -5 -7 381.24 20.81 19 5 -6 30.60 12.93 19 -5 -6 25.68 11.42 19 5 -5 143.62 15.33 19 -5 -5 141.54 13.74 19 5 -4 136.85 15.09 19 -5 -4 128.02 13.12 -19 -5 3 249.14 24.63 -19 -5 2 17.44 17.77 -19 7 10 136.56 16.35 19 -7 -10 112.22 14.47 -19 7 9 64.74 14.01 19 -7 -9 86.05 13.60 -19 7 8 146.17 15.28 19 -7 -8 130.85 14.40 19 -7 -7 427.80 21.84 19 -7 -6 22.06 11.12 -19 9 9 340.11 21.00 19 -9 -9 309.44 19.79 19 -9 -8 443.90 22.88 20 0 -10 720.44 31.64 20 0 -6 618.44 27.93 20 0 -5 73.18 13.34 20 0 -4 529.90 25.17 20 -2 -7 472.90 24.13 20 -2 -6 295.54 19.25 20 -2 -5 135.11 14.70 20 2 -4 309.20 19.69 -20 -2 4 270.14 24.51 20 2 -3 42.58 12.85 -20 -2 3 28.12 16.49 -20 -2 2 32.83 16.53 20 -4 -7 374.00 21.23 20 -4 -6 7.49 11.54 20 -6 -8 70.15 13.28 0 0 0 0.00 0.00 TITL CZY_II_020_b in C2/m REM C2/m (#12 in standard setting) CELL 0.71073 14.823908 21.178942 17.242659 90.0000 107.3184 90.0000 ZERR 6.00 0.000558 0.000647 0.000772 0.0000 0.0046 0.0000 LATT 7 SYMM -x, y,-z SFAC C H Ir U UNIT 276.00 444.00 24.00 6.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 35286 _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 ; _oxdiff_exptl_absorpt_empirical_full_max 4.487 _oxdiff_exptl_absorpt_empirical_full_min 0.722 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 U001 U 0.5000 0.24415(2) 0.2500 0.00897(12) Uani 1 2 d S T P A . Ir1 Ir 0.37343(3) 0.15697(2) 0.30237(2) 0.01113(10) Uani 1 1 d . . . . . Ir Ir 0.58181(3) 0.32970(2) 0.38814(2) 0.01095(10) Uani 1 1 d . . . . . C005 C 0.5530(8) 0.3692(5) 0.4965(6) 0.018(2) Uani 1 1 d . . . . . C006 C 0.6462(7) 0.3420(5) 0.5222(6) 0.016(2) Uani 1 1 d . . . . . C007 C 0.5524(8) 0.4194(5) 0.4402(6) 0.020(2) Uani 1 1 d . . . . . C009 C 0.7026(7) 0.3767(5) 0.4805(6) 0.016(2) Uani 1 1 d . . . . . C20 C 0.4696(10) 0.4610(6) 0.3988(8) 0.034(3) Uani 1 1 d . . . . . H20A H 0.4701 0.4697 0.3442 0.051 Uiso 1 1 calc R U . . . H20B H 0.4741 0.5000 0.4281 0.051 Uiso 1 1 calc R U . . . H20C H 0.4119 0.4399 0.3975 0.051 Uiso 1 1 calc R U . . . C00C C 0.8101(8) 0.3706(6) 0.4963(7) 0.026(3) Uani 1 1 d . . . . . H00A H 0.8313 0.3310 0.5226 0.039 Uiso 1 1 calc R U . . . H00B H 0.8416 0.4046 0.5305 0.039 Uiso 1 1 calc R U . . . H00C H 0.8244 0.3723 0.4456 0.039 Uiso 1 1 calc R U . . . C00I C 0.6440(9) 0.4240(5) 0.4311(7) 0.025(3) Uani 1 1 d . . . . . C00L C 0.4719(8) 0.3504(6) 0.5275(7) 0.028(3) Uani 1 1 d . . . . . H00D H 0.4139 0.3526 0.4840 0.042 Uiso 1 1 calc R U . . . H00E H 0.4689 0.3785 0.5704 0.042 Uiso 1 1 calc R U . . . H00F H 0.4814 0.3079 0.5480 0.042 Uiso 1 1 calc R U . . . C00X C 0.6772(11) 0.4725(6) 0.3812(9) 0.039(3) Uani 1 1 d . . . . . H00G H 0.7214 0.4533 0.3575 0.058 Uiso 1 1 calc R U . . . H00H H 0.7072 0.5069 0.4155 0.058 Uiso 1 1 calc R U . . . H00I H 0.6239 0.4881 0.3388 0.058 Uiso 1 1 calc R U . . . C4 C 0.1314(15) 0.3389(8) 0.2472(12) 0.062(5) Uani 1 1 d . . . . . H4A H 0.1314 0.2984 0.2208 0.075 Uiso 1 1 calc R U . . . H4B H 0.1223 0.3713 0.2059 0.075 Uiso 1 1 calc R U . . . C6 C 0.2262(15) 0.3483(9) 0.3081(13) 0.070(6) Uani 1 1 d . . . . . H6A H 0.2747 0.3421 0.2823 0.104 Uiso 1 1 calc R U . . . H6B H 0.2343 0.3185 0.3516 0.104 Uiso 1 1 calc R U . . . H6C H 0.2304 0.3905 0.3294 0.104 Uiso 1 1 calc R U . . . C1 C 0.0481(12) 0.3405(7) 0.2810(10) 0.051(4) Uani 1 1 d . . . . . H1A H 0.0523 0.3042 0.3162 0.062 Uiso 1 1 calc R U . . . H1B H 0.0535 0.3780 0.3144 0.062 Uiso 1 1 calc R U . . . C2 C 0.374(3) 0.063(2) 0.353(2) 0.013(5) Uani 0.483(16) 1 d . U P A 2 C5 C 0.271(3) 0.141(2) 0.369(2) 0.015(5) Uani 0.483(16) 1 d . U P A 2 C7 C 0.233(3) 0.1117(16) 0.291(2) 0.012(5) Uani 0.483(16) 1 d . U P A 2 C3 C 0.358(3) 0.1095(15) 0.410(3) 0.015(5) Uani 0.483(16) 1 d . U P A 2 C8 C 0.296(3) 0.0643(19) 0.280(3) 0.015(5) Uani 0.483(16) 1 d . U P A 2 C12 C 0.266(2) 0.1794(15) 0.4497(19) 0.032(7) Uani 0.517(16) 1 d . . P A 3 H12A H 0.3218 0.2004 0.4818 0.048 Uiso 0.517(16) 1 calc R U P A 3 H12B H 0.2390 0.1553 0.4845 0.048 Uiso 0.517(16) 1 calc R U P A 3 H12C H 0.2207 0.2102 0.4208 0.048 Uiso 0.517(16) 1 calc R U P A 3 C13 C 0.1337(19) 0.1520(15) 0.2685(19) 0.031(5) Uani 0.517(16) 1 d . U P A 3 H13A H 0.1357 0.1971 0.2747 0.047 Uiso 0.517(16) 1 calc R U P A 3 H13B H 0.0910 0.1345 0.2951 0.047 Uiso 0.517(16) 1 calc R U P A 3 H13C H 0.1125 0.1415 0.2118 0.047 Uiso 0.517(16) 1 calc R U P A 3 C10 C 0.4236(18) 0.0040(12) 0.3293(17) 0.027(4) Uani 0.517(16) 1 d . U P A 3 H10A H 0.4124 -0.0071 0.2733 0.040 Uiso 0.517(16) 1 calc R U P A 3 H10B H 0.4120 -0.0320 0.3588 0.040 Uiso 0.517(16) 1 calc R U P A 3 H10C H 0.4880 0.0174 0.3518 0.040 Uiso 0.517(16) 1 calc R U P A 3 C9 C 0.2369(19) 0.0433(13) 0.1913(16) 0.029(5) Uani 0.517(16) 1 d . U P A 3 H9A H 0.1843 0.0670 0.1582 0.043 Uiso 0.517(16) 1 calc R U P A 3 H9B H 0.2165 0.0013 0.1989 0.043 Uiso 0.517(16) 1 calc R U P A 3 H9C H 0.2855 0.0412 0.1650 0.043 Uiso 0.517(16) 1 calc R U P A 3 C11 C 0.4428(19) 0.0877(14) 0.4873(14) 0.024(5) Uani 0.517(16) 1 d . . P A 3 H11A H 0.4975 0.0667 0.4808 0.037 Uiso 0.517(16) 1 calc R U P A 3 H11B H 0.4178 0.0639 0.5236 0.037 Uiso 0.517(16) 1 calc R U P A 3 H11C H 0.4602 0.1292 0.5093 0.037 Uiso 0.517(16) 1 calc R U P A 3 C16 C 0.4191(19) 0.1201(15) 0.4947(16) 0.025(6) Uani 0.483(16) 1 d . . P A 2 H16A H 0.4827 0.1079 0.4990 0.037 Uiso 0.483(16) 1 calc R U P A 2 H16B H 0.3962 0.0953 0.5315 0.037 Uiso 0.483(16) 1 calc R U P A 2 H16C H 0.4178 0.1640 0.5082 0.037 Uiso 0.483(16) 1 calc R U P A 2 C15 C 0.453(2) 0.0144(13) 0.3699(19) 0.027(4) Uani 0.483(16) 1 d . . P A 2 H15A H 0.4604 0.0000 0.3194 0.040 Uiso 0.483(16) 1 calc R U P A 2 H15B H 0.4376 -0.0208 0.3988 0.040 Uiso 0.483(16) 1 calc R U P A 2 H15C H 0.5108 0.0334 0.4021 0.040 Uiso 0.483(16) 1 calc R U P A 2 C18 C 0.132(2) 0.1242(16) 0.237(2) 0.031(5) Uani 0.483(16) 1 d . . P A 2 H18A H 0.1221 0.1689 0.2298 0.047 Uiso 0.483(16) 1 calc R U P A 2 H18B H 0.0880 0.1066 0.2614 0.047 Uiso 0.483(16) 1 calc R U P A 2 H18C H 0.1234 0.1049 0.1844 0.047 Uiso 0.483(16) 1 calc R U P A 2 C19 C 0.281(2) 0.0234(14) 0.2071(17) 0.029(5) Uani 0.483(16) 1 d . . P A 2 H19A H 0.2428 0.0455 0.1602 0.043 Uiso 0.483(16) 1 calc R U P A 2 H19B H 0.2495 -0.0148 0.2144 0.043 Uiso 0.483(16) 1 calc R U P A 2 H19C H 0.3409 0.0133 0.1996 0.043 Uiso 0.483(16) 1 calc R U P A 2 C17 C 0.230(3) 0.1895(16) 0.411(2) 0.037(8) Uani 0.483(16) 1 d . . P A 2 H17A H 0.2787 0.2190 0.4375 0.055 Uiso 0.483(16) 1 calc R U P A 2 H17B H 0.2050 0.1698 0.4497 0.055 Uiso 0.483(16) 1 calc R U P A 2 H17C H 0.1808 0.2114 0.3709 0.055 Uiso 0.483(16) 1 calc R U P A 2 C26 C 0.276(2) 0.0755(17) 0.274(3) 0.015(5) Uani 0.517(16) 1 d . . P A 3 C22 C 0.360(3) 0.0554(19) 0.335(2) 0.013(5) Uani 0.517(16) 1 d . . P A 3 C23 C 0.369(3) 0.0932(14) 0.406(3) 0.015(5) Uani 0.517(16) 1 d . . P A 3 C24 C 0.290(2) 0.1363(19) 0.3903(18) 0.015(5) Uani 0.517(16) 1 d . . P A 3 C25 C 0.231(3) 0.1252(15) 0.306(2) 0.012(5) Uani 0.517(16) 1 d . . P A 3 C14 C 0.6810(8) 0.2899(5) 0.5818(7) 0.023(2) Uani 1 1 d . . . . . H14A H 0.6288 0.2640 0.5841 0.034 Uiso 1 1 calc R U . . . H14B H 0.7109 0.3075 0.6345 0.034 Uiso 1 1 calc R U . . . H14C H 0.7258 0.2648 0.5651 0.034 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 U001 0.0084(2) 0.0086(2) 0.0114(2) 0.000 0.00536(19) 0.000 Ir1 0.00956(18) 0.01063(18) 0.0149(2) 0.00098(13) 0.00620(15) -0.00137(13) Ir 0.01235(18) 0.01008(18) 0.01115(19) -0.00086(13) 0.00459(14) -0.00145(13) C005 0.019(5) 0.019(5) 0.018(5) -0.008(4) 0.009(4) 0.005(4) C006 0.012(5) 0.019(5) 0.014(5) -0.005(4) 0.001(4) -0.005(4) C007 0.030(6) 0.017(5) 0.013(5) -0.009(4) 0.007(5) 0.001(4) C009 0.015(5) 0.019(5) 0.017(5) -0.008(4) 0.006(4) -0.006(4) C20 0.042(8) 0.020(6) 0.031(7) -0.005(5) -0.003(6) 0.014(5) C00C 0.026(6) 0.037(7) 0.022(6) -0.007(5) 0.018(5) -0.012(5) C00I 0.037(7) 0.016(5) 0.026(6) -0.002(5) 0.014(5) -0.011(5) C00L 0.018(6) 0.045(7) 0.023(6) -0.007(5) 0.008(5) 0.000(5) C00X 0.059(9) 0.024(6) 0.042(8) -0.004(6) 0.027(7) -0.022(6) C4 0.099(15) 0.039(9) 0.064(12) 0.012(8) 0.047(11) 0.006(9) C6 0.079(14) 0.045(10) 0.092(15) 0.010(10) 0.037(12) 0.020(10) C1 0.082(12) 0.032(8) 0.049(9) -0.002(7) 0.033(8) 0.007(8) C2 0.016(9) 0.013(8) 0.009(11) 0.000(8) 0.003(8) -0.007(6) C5 0.012(10) 0.020(6) 0.015(11) 0.002(8) 0.007(8) -0.002(7) C7 0.010(5) 0.015(10) 0.014(10) -0.002(7) 0.009(7) -0.004(7) C3 0.018(8) 0.015(11) 0.016(6) 0.003(8) 0.009(5) 0.000(8) C8 0.016(11) 0.016(10) 0.016(7) 0.008(7) 0.008(8) -0.003(8) C12 0.044(19) 0.032(16) 0.024(16) -0.009(13) 0.017(14) -0.003(13) C13 0.013(7) 0.041(16) 0.042(16) 0.018(10) 0.013(10) -0.002(11) C10 0.023(12) 0.018(9) 0.032(14) 0.010(10) -0.004(10) 0.000(8) C9 0.024(13) 0.027(12) 0.025(11) -0.001(8) -0.009(11) -0.016(9) C11 0.029(14) 0.029(15) 0.012(11) 0.000(10) 0.001(10) -0.007(11) C16 0.025(14) 0.033(16) 0.022(13) 0.004(12) 0.016(11) -0.007(12) C15 0.023(12) 0.018(9) 0.032(14) 0.010(10) -0.004(10) 0.000(8) C18 0.013(7) 0.041(16) 0.042(16) 0.018(10) 0.013(10) -0.002(11) C19 0.024(13) 0.027(12) 0.025(11) -0.001(8) -0.009(11) -0.016(9) C17 0.05(2) 0.035(17) 0.04(2) 0.008(16) 0.041(19) 0.006(16) C26 0.016(11) 0.016(10) 0.016(7) 0.008(7) 0.008(8) -0.003(8) C22 0.016(9) 0.013(8) 0.009(11) 0.000(8) 0.003(8) -0.007(6) C23 0.018(8) 0.015(11) 0.016(6) 0.003(8) 0.009(5) 0.000(8) C24 0.012(10) 0.020(6) 0.015(11) 0.002(8) 0.007(8) -0.002(7) C25 0.010(5) 0.015(10) 0.014(10) -0.002(7) 0.009(7) -0.004(7) C14 0.021(5) 0.027(6) 0.019(6) 0.001(5) 0.002(5) 0.005(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 '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 Ir1 U001 Ir1 102.77(2) . 2_655 ? Ir U001 Ir1 106.404(11) 2_655 2_655 ? Ir U001 Ir1 118.944(11) 2_655 . ? Ir U001 Ir1 106.404(10) . . ? Ir U001 Ir1 118.944(11) . 2_655 ? Ir U001 Ir 104.24(2) 2_655 . ? C2 Ir1 U001 140.2(12) . . ? C2 Ir1 C5 64.0(17) . . ? C2 Ir1 C7 62.5(15) . . ? C2 Ir1 C3 39.1(13) . . ? C2 Ir1 C8 37.7(14) . . ? C5 Ir1 U001 149.5(11) . . ? C5 Ir1 C7 38.0(12) . . ? C5 Ir1 C8 63.3(16) . . ? C7 Ir1 U001 153.3(10) . . ? C3 Ir1 U001 141.7(11) . . ? C3 Ir1 C5 38.0(13) . . ? C3 Ir1 C7 63.3(15) . . ? C3 Ir1 C8 64.0(16) . . ? C8 Ir1 U001 146.3(13) . . ? C8 Ir1 C7 36.8(12) . . ? C26 Ir1 U001 148.4(12) . . ? C26 Ir1 C22 37.8(12) . . ? C26 Ir1 C23 62.4(15) . . ? C26 Ir1 C24 63.0(15) . . ? C26 Ir1 C25 37.8(12) . . ? C22 Ir1 U001 141.8(11) . . ? C22 Ir1 C23 37.0(12) . . ? C22 Ir1 C24 62.6(15) . . ? C23 Ir1 U001 141.8(10) . . ? C23 Ir1 C24 37.2(12) . . ? C24 Ir1 U001 147.8(10) . . ? C25 Ir1 U001 152.6(9) . . ? C25 Ir1 C22 63.3(14) . . ? C25 Ir1 C23 62.9(13) . . ? C25 Ir1 C24 38.2(11) . . ? C005 Ir U001 141.4(3) . . ? C005 Ir C006 37.8(4) . . ? C005 Ir C009 62.9(4) . . ? C005 Ir C00I 62.9(4) . . ? C006 Ir U001 148.4(3) . . ? C006 Ir C009 37.9(4) . . ? C007 Ir U001 140.9(3) . . ? C007 Ir C005 38.1(4) . . ? C007 Ir C006 63.4(4) . . ? C007 Ir C009 62.6(4) . . ? C007 Ir C00I 37.3(4) . . ? C009 Ir U001 153.5(3) . . ? C00I Ir U001 147.9(3) . . ? C00I Ir C006 63.0(4) . . ? C00I Ir C009 37.2(4) . . ? C006 C005 Ir 72.4(6) . . ? C006 C005 C00L 125.3(10) . . ? C007 C005 Ir 70.8(6) . . ? C007 C005 C006 108.4(9) . . ? C007 C005 C00L 126.2(10) . . ? C00L C005 Ir 125.2(8) . . ? C005 C006 Ir 69.8(6) . . ? C005 C006 C009 106.6(9) . . ? C005 C006 C14 127.8(10) . . ? C009 C006 Ir 71.3(6) . . ? C009 C006 C14 125.6(10) . . ? C14 C006 Ir 125.4(7) . . ? C005 C007 Ir 71.1(6) . . ? C005 C007 C20 126.3(11) . . ? C20 C007 Ir 122.9(7) . . ? C00I C007 Ir 72.6(6) . . ? C00I C007 C005 108.2(10) . . ? C00I C007 C20 125.4(11) . . ? C006 C009 Ir 70.9(6) . . ? C006 C009 C00C 125.9(10) . . ? C00C C009 Ir 130.7(7) . . ? C00I C009 Ir 70.9(6) . . ? C00I C009 C006 108.2(9) . . ? C00I C009 C00C 125.3(10) . . ? C007 C20 H20A 109.5 . . ? C007 C20 H20B 109.5 . . ? C007 C20 H20C 109.5 . . ? H20A C20 H20B 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C009 C00C H00A 109.5 . . ? C009 C00C H00B 109.5 . . ? C009 C00C H00C 109.5 . . ? H00A C00C H00B 109.5 . . ? H00A C00C H00C 109.5 . . ? H00B C00C H00C 109.5 . . ? C007 C00I Ir 70.1(6) . . ? C007 C00I C009 108.5(9) . . ? C007 C00I C00X 126.5(12) . . ? C009 C00I Ir 71.9(6) . . ? C009 C00I C00X 124.9(12) . . ? C00X C00I Ir 126.2(8) . . ? C005 C00L H00D 109.5 . . ? C005 C00L H00E 109.5 . . ? C005 C00L H00F 109.5 . . ? H00D C00L H00E 109.5 . . ? H00D C00L H00F 109.5 . . ? H00E C00L H00F 109.5 . . ? C00I C00X H00G 109.5 . . ? C00I C00X H00H 109.5 . . ? C00I C00X H00I 109.5 . . ? H00G C00X H00H 109.5 . . ? H00G C00X H00I 109.5 . . ? H00H C00X H00I 109.5 . . ? H4A C4 H4B 107.5 . . ? C6 C4 H4A 108.4 . . ? C6 C4 H4B 108.4 . . ? C6 C4 C1 115.5(16) . . ? C1 C4 H4A 108.4 . . ? C1 C4 H4B 108.4 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6B 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C4 C1 H1A 108.3 . . ? C4 C1 H1B 108.3 . . ? C1 C1 C4 115.8(17) 2 . ? C1 C1 H1A 108.3 2 . ? C1 C1 H1B 108.3 2 . ? H1A C1 H1B 107.4 . . ? C3 C2 Ir1 70(2) . . ? C3 C2 C15 127(3) . . ? C8 C2 Ir1 74(2) . . ? C8 C2 C3 109(4) . . ? C8 C2 C15 124(3) . . ? C15 C2 Ir1 127(3) . . ? C7 C5 Ir1 73(2) . . ? C7 C5 C17 130(3) . . ? C3 C5 Ir1 71(3) . . ? C3 C5 C7 108(4) . . ? C3 C5 C17 122(3) . . ? C17 C5 Ir1 126(3) . . ? C5 C7 Ir1 69(2) . . ? C5 C7 C18 123(3) . . ? C8 C7 Ir1 72(2) . . ? C8 C7 C5 109(4) . . ? C8 C7 C18 127(3) . . ? C18 C7 Ir1 134(3) . . ? C2 C3 Ir1 70(3) . . ? C2 C3 C16 126(3) . . ? C5 C3 Ir1 71(2) . . ? C5 C3 C2 107(4) . . ? C5 C3 C16 127(3) . . ? C16 C3 Ir1 125(3) . . ? C2 C8 Ir1 69(2) . . ? C2 C8 C19 127(3) . . ? C7 C8 Ir1 72(2) . . ? C7 C8 C2 107(4) . . ? C7 C8 C19 125(3) . . ? C19 C8 Ir1 126(3) . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C24 C12 H12A 109.5 . . ? C24 C12 H12B 109.5 . . ? C24 C12 H12C 109.5 . . ? H13A C13 H13B 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C25 C13 H13A 109.5 . . ? C25 C13 H13B 109.5 . . ? C25 C13 H13C 109.5 . . ? H10A C10 H10B 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C22 C10 H10A 109.5 . . ? C22 C10 H10B 109.5 . . ? C22 C10 H10C 109.5 . . ? H9A C9 H9B 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C26 C9 H9A 109.5 . . ? C26 C9 H9B 109.5 . . ? C26 C9 H9C 109.5 . . ? H11A C11 H11B 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C23 C11 H11A 109.5 . . ? C23 C11 H11B 109.5 . . ? C23 C11 H11C 109.5 . . ? C3 C16 H16A 109.5 . . ? C3 C16 H16B 109.5 . . ? C3 C16 H16C 109.5 . . ? H16A C16 H16B 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C2 C15 H15A 109.5 . . ? C2 C15 H15B 109.5 . . ? C2 C15 H15C 109.5 . . ? H15A C15 H15B 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C7 C18 H18A 109.5 . . ? C7 C18 H18B 109.5 . . ? C7 C18 H18C 109.5 . . ? H18A C18 H18B 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C8 C19 H19A 109.5 . . ? C8 C19 H19B 109.5 . . ? C8 C19 H19C 109.5 . . ? H19A C19 H19B 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C5 C17 H17A 109.5 . . ? C5 C17 H17B 109.5 . . ? C5 C17 H17C 109.5 . . ? H17A C17 H17B 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C9 C26 Ir1 126(3) . . ? C22 C26 Ir1 72(2) . . ? C22 C26 C9 124(3) . . ? C25 C26 Ir1 72(2) . . ? C25 C26 C9 127(3) . . ? C25 C26 C22 109(4) . . ? C10 C22 Ir1 126(3) . . ? C26 C22 Ir1 70(2) . . ? C26 C22 C10 127(3) . . ? C23 C22 Ir1 72(2) . . ? C23 C22 C10 126(3) . . ? C23 C22 C26 107(4) . . ? C11 C23 Ir1 127(2) . . ? C22 C23 Ir1 71(2) . . ? C22 C23 C11 127(3) . . ? C22 C23 C24 109(3) . . ? C24 C23 Ir1 72(2) . . ? C24 C23 C11 123(3) . . ? C12 C24 Ir1 129(3) . . ? C23 C24 Ir1 71(2) . . ? C23 C24 C12 127(3) . . ? C23 C24 C25 107(3) . . ? C25 C24 Ir1 70(2) . . ? C25 C24 C12 125(3) . . ? C13 C25 Ir1 132(2) . . ? C26 C25 Ir1 70(2) . . ? C26 C25 C13 127(3) . . ? C26 C25 C24 107(3) . . ? C24 C25 Ir1 72(2) . . ? C24 C25 C13 125(3) . . ? C006 C14 H14A 109.5 . . ? C006 C14 H14B 109.5 . . ? C006 C14 H14C 109.5 . . ? H14A C14 H14B 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 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 U001 Ir1 2.9587(5) . ? U001 Ir1 2.9587(5) 2_655 ? U001 Ir 2.9507(5) 2_655 ? U001 Ir 2.9508(5) . ? Ir1 C2 2.18(5) . ? Ir1 C5 2.19(4) . ? Ir1 C7 2.25(4) . ? Ir1 C3 2.18(5) . ? Ir1 C8 2.25(4) . ? Ir1 C26 2.21(4) . ? Ir1 C22 2.25(4) . ? Ir1 C23 2.26(4) . ? Ir1 C24 2.26(4) . ? Ir1 C25 2.23(4) . ? Ir C005 2.203(10) . ? Ir C006 2.239(10) . ? Ir C007 2.200(10) . ? Ir C009 2.244(10) . ? Ir C00I 2.231(11) . ? C005 C006 1.440(14) . ? C005 C007 1.438(16) . ? C005 C00L 1.507(15) . ? C006 C009 1.454(14) . ? C006 C14 1.490(15) . ? C007 C20 1.508(16) . ? C007 C00I 1.416(16) . ? C009 C00C 1.541(15) . ? C009 C00I 1.428(16) . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C00C H00A 0.9600 . ? C00C H00B 0.9600 . ? C00C H00C 0.9600 . ? C00I C00X 1.513(16) . ? C00L H00D 0.9600 . ? C00L H00E 0.9600 . ? C00L H00F 0.9600 . ? C00X H00G 0.9600 . ? C00X H00H 0.9600 . ? C00X H00I 0.9600 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C4 C6 1.50(3) . ? C4 C1 1.51(2) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C1 C1 1.51(3) 2 ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.46(5) . ? C2 C8 1.43(5) . ? C2 C15 1.52(5) . ? C5 C7 1.44(5) . ? C5 C3 1.42(5) . ? C5 C17 1.49(5) . ? C7 C8 1.42(5) . ? C7 C18 1.53(5) . ? C3 C16 1.49(5) . ? C8 C19 1.49(6) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C12 C24 1.49(5) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C13 C25 1.51(5) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C10 C22 1.46(5) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C9 C26 1.53(5) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C11 C23 1.51(5) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C26 C22 1.44(5) . ? C26 C25 1.44(5) . ? C22 C23 1.43(5) . ? C23 C24 1.44(5) . ? C24 C25 1.47(4) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? 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 Ir1 C2 C3 C5 62(3) . . . . ? Ir1 C2 C3 C16 -120(4) . . . . ? Ir1 C2 C8 C7 -61(3) . . . . ? Ir1 C2 C8 C19 120(4) . . . . ? Ir1 C5 C7 C8 61(3) . . . . ? Ir1 C5 C7 C18 -129(3) . . . . ? Ir1 C5 C3 C2 -62(3) . . . . ? Ir1 C5 C3 C16 120(4) . . . . ? Ir1 C7 C8 C2 59(3) . . . . ? Ir1 C7 C8 C19 -122(4) . . . . ? Ir1 C26 C22 C10 -120(4) . . . . ? Ir1 C26 C22 C23 62(3) . . . . ? Ir1 C26 C25 C13 128(4) . . . . ? Ir1 C26 C25 C24 -63(3) . . . . ? Ir1 C22 C23 C11 -122(4) . . . . ? Ir1 C22 C23 C24 62(3) . . . . ? Ir1 C23 C24 C12 -125(4) . . . . ? Ir1 C23 C24 C25 61(3) . . . . ? Ir1 C24 C25 C13 -129(3) . . . . ? Ir1 C24 C25 C26 62(3) . . . . ? Ir C005 C006 C009 62.2(7) . . . . ? Ir C005 C006 C14 -119.7(11) . . . . ? Ir C005 C007 C20 117.5(11) . . . . ? Ir C005 C007 C00I -63.5(7) . . . . ? Ir C006 C009 C00C -127.0(10) . . . . ? Ir C006 C009 C00I 61.4(7) . . . . ? Ir C007 C00I C009 -62.0(8) . . . . ? Ir C007 C00I C00X 121.0(12) . . . . ? Ir C009 C00I C007 60.9(8) . . . . ? Ir C009 C00I C00X -122.0(12) . . . . ? C005 C006 C009 Ir -61.2(7) . . . . ? C005 C006 C009 C00C 171.9(10) . . . . ? C005 C006 C009 C00I 0.2(11) . . . . ? C005 C007 C00I Ir 62.5(7) . . . . ? C005 C007 C00I C009 0.5(12) . . . . ? C005 C007 C00I C00X -176.5(11) . . . . ? C006 C005 C007 Ir 63.1(7) . . . . ? C006 C005 C007 C20 -179.4(10) . . . . ? C006 C005 C007 C00I -0.4(12) . . . . ? C006 C009 C00I Ir -61.4(7) . . . . ? C006 C009 C00I C007 -0.5(12) . . . . ? C006 C009 C00I C00X 176.6(11) . . . . ? C007 C005 C006 Ir -62.1(7) . . . . ? C007 C005 C006 C009 0.1(11) . . . . ? C007 C005 C006 C14 178.3(10) . . . . ? C20 C007 C00I Ir -118.4(11) . . . . ? C20 C007 C00I C009 179.6(10) . . . . ? C20 C007 C00I C00X 2.6(18) . . . . ? C00C C009 C00I Ir 126.9(10) . . . . ? C00C C009 C00I C007 -172.2(10) . . . . ? C00C C009 C00I C00X 4.9(18) . . . . ? C00L C005 C006 Ir 121.1(11) . . . . ? C00L C005 C006 C009 -176.7(10) . . . . ? C00L C005 C006 C14 1.5(17) . . . . ? C00L C005 C007 Ir -120.1(11) . . . . ? C00L C005 C007 C20 -2.7(17) . . . . ? C00L C005 C007 C00I 176.4(10) . . . . ? C6 C4 C1 C1 171.5(11) . . . 2 ? C5 C7 C8 Ir1 -59(3) . . . . ? C5 C7 C8 C2 1(5) . . . . ? C5 C7 C8 C19 180(4) . . . . ? C7 C5 C3 Ir1 64(3) . . . . ? C7 C5 C3 C2 2(5) . . . . ? C7 C5 C3 C16 -175(4) . . . . ? C3 C2 C8 Ir1 62(3) . . . . ? C3 C2 C8 C7 1(5) . . . . ? C3 C2 C8 C19 -178(4) . . . . ? C3 C5 C7 Ir1 -63(3) . . . . ? C3 C5 C7 C8 -2(5) . . . . ? C3 C5 C7 C18 168(4) . . . . ? C8 C2 C3 Ir1 -64(3) . . . . ? C8 C2 C3 C5 -2(5) . . . . ? C8 C2 C3 C16 176(4) . . . . ? C12 C24 C25 Ir1 124(4) . . . . ? C12 C24 C25 C13 -5(6) . . . . ? C12 C24 C25 C26 -174(3) . . . . ? C10 C22 C23 Ir1 122(4) . . . . ? C10 C22 C23 C11 -1(7) . . . . ? C10 C22 C23 C24 -176(4) . . . . ? C9 C26 C22 Ir1 123(4) . . . . ? C9 C26 C22 C10 2(6) . . . . ? C9 C26 C22 C23 -175(3) . . . . ? C9 C26 C25 Ir1 -122(4) . . . . ? C9 C26 C25 C13 6(6) . . . . ? C9 C26 C25 C24 174(3) . . . . ? C11 C23 C24 Ir1 123(3) . . . . ? C11 C23 C24 C12 -3(6) . . . . ? C11 C23 C24 C25 -177(3) . . . . ? C15 C2 C3 Ir1 122(4) . . . . ? C15 C2 C3 C5 -175(4) . . . . ? C15 C2 C3 C16 3(7) . . . . ? C15 C2 C8 Ir1 -124(4) . . . . ? C15 C2 C8 C7 174(4) . . . . ? C15 C2 C8 C19 -5(7) . . . . ? C18 C7 C8 Ir1 132(4) . . . . ? C18 C7 C8 C2 -169(4) . . . . ? C18 C7 C8 C19 10(7) . . . . ? C17 C5 C7 Ir1 123(4) . . . . ? C17 C5 C7 C8 -176(4) . . . . ? C17 C5 C7 C18 -6(6) . . . . ? C17 C5 C3 Ir1 -121(4) . . . . ? C17 C5 C3 C2 177(4) . . . . ? C17 C5 C3 C16 -1(6) . . . . ? C26 C22 C23 Ir1 -61(3) . . . . ? C26 C22 C23 C11 177(4) . . . . ? C26 C22 C23 C24 1(5) . . . . ? C22 C26 C25 Ir1 63(3) . . . . ? C22 C26 C25 C13 -169(3) . . . . ? C22 C26 C25 C24 0(4) . . . . ? C22 C23 C24 Ir1 -62(3) . . . . ? C22 C23 C24 C12 173(4) . . . . ? C22 C23 C24 C25 -1(4) . . . . ? C23 C24 C25 Ir1 -62(3) . . . . ? C23 C24 C25 C13 169(3) . . . . ? C23 C24 C25 C26 0(4) . . . . ? C25 C26 C22 Ir1 -63(3) . . . . ? C25 C26 C22 C10 177(4) . . . . ? C25 C26 C22 C23 -1(5) . . . . ? C14 C006 C009 Ir 120.6(10) . . . . ? C14 C006 C009 C00C -6.4(16) . . . . ? C14 C006 C009 C00I -178.0(10) . . . . ?