#------------------------------------------------------------------------------ #$Date: 2021-10-29 02:34:01 +0300 (Fri, 29 Oct 2021) $ #$Revision: 270117 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/86/7708604.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_7708604 loop_ _publ_author_name 'Bezzubov, Stanislav' 'Ermolov, Kirill' 'Gorbunov, Alexander' 'Kalle, Paulina' 'Lentin, Ivan' 'Latyshev, Gennadij' 'Kovalev, Vladimir' 'Vatsouro, Ivan' _publ_section_title ; Inherently dinuclear iridium(III) meso architectures accessed by cyclometalation of calix[4]arene-based bis(aryltriazoles) ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D1DT03579G _journal_year 2021 _chemical_formula_moiety 'C140 H168 Cl2 Ir2 N12 O8, 6.5(C2 H4 Cl2), 2(C H2 Cl2)' _chemical_formula_sum 'C155 H198 Cl19 Ir2 N12 O8' _chemical_formula_weight 3415.19 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _audit_creation_date 2020-11-18 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2020-11-18 deposited with the CCDC. 2021-10-27 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 103.304(2) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 19.6360(13) _cell_length_b 13.1399(6) _cell_length_c 34.199(2) _cell_measurement_reflns_used 9927 _cell_measurement_temperature 100 _cell_measurement_theta_max 28.34 _cell_measurement_theta_min 2.38 _cell_volume 8587.1(9) _computing_cell_refinement 'SAINT v8.37A (Bruker, 2015)' _computing_data_collection 'APEX3 v.2017.3_0 (Bruker AXS, 2017)' _computing_data_reduction 'SAINT v8.37A (Bruker, 2015)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'XT (Sheldrick, 2015)' _diffrn_ambient_temperature 100.0 _diffrn_detector 'PHOTON II area detector' _diffrn_detector_area_resol_mean 10.4 _diffrn_detector_type 'CMOS sensor' _diffrn_measured_fraction_theta_full 0.976 _diffrn_measured_fraction_theta_max 0.976 _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\w scan' _diffrn_radiation_monochromator 'mirror optics' _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0952 _diffrn_reflns_av_unetI/netI 0.0684 _diffrn_reflns_Laue_measured_fraction_full 0.976 _diffrn_reflns_Laue_measured_fraction_max 0.976 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_number 97984 _diffrn_reflns_point_group_measured_fraction_full 0.976 _diffrn_reflns_point_group_measured_fraction_max 0.976 _diffrn_reflns_theta_full 25.200 _diffrn_reflns_theta_max 25.200 _diffrn_reflns_theta_min 1.975 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_source_type 'X-ray tube' _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 1.898 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_correction_T_min 0.6090 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1375 before and 0.0685 after correction. The Ratio of minimum to maximum transmission is 0.8167. The \l/2 correction factor is Not present.' _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.321 _exptl_crystal_description needle _exptl_crystal_F_000 3506 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: CH2Cl2, C2H4Cl2' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.02 _refine_diff_density_max 1.815 _refine_diff_density_min -2.568 _refine_diff_density_rms 0.172 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 819 _refine_ls_number_reflns 15109 _refine_ls_number_restraints 40 _refine_ls_restrained_S_all 1.052 _refine_ls_R_factor_all 0.1011 _refine_ls_R_factor_gt 0.0741 _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^)+(0.0758P)^2^+102.7877P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1756 _refine_ls_wR_factor_ref 0.1895 _reflns_Friedel_coverage 0.000 _reflns_number_gt 11175 _reflns_number_total 15109 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1dt03579g2.cif _cod_data_source_block v839e _cod_original_cell_volume 8587.0(9) _cod_database_code 7708604 _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 0.963 _shelx_estimated_absorpt_t_min 0.556 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All C(H,H,H,H,H, H,H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances C21-C028 = C02Z-C028 = C032-C02Z = C21-C20 1.54 with sigma of 0.02 Cl00-C02M \\sim Cl8-C02M \\sim Cl-C02I \\sim Cl7-C02I \\sim Cl10-C02I \\sim Cl6-C02I with sigma of 0.01 C0AA-C02A \\sim C3-C02A \\sim C18B-C02A with sigma of 0.01 C02Z-C028 \\sim C21-C028 \\sim C21-C20 \\sim C032-C02Z with sigma of 0.01 C0AA-C02A \\sim C4-C02A \\sim C5-C02A \\sim C3-C02A \\sim C18A-C02A \\sim C18B-C02A with sigma of 0.01 3. Uiso/Uaniso restraints and constraints Uanis(Cl) = Uanis(Cl7) = Uanis(Cl10) = Uanis(Cl6) Uanis(C02M) = Uanis(Cl00) = Uanis(Cl8) = Uanis(C02I) = Uanis(Cl6) = Uanis(Cl7) = Uanis(Cl10) = Uanis(Cl) Uanis(C12) = Uanis(C1AA) = Uanis(C0) = Uanis(C13) = Uanis(C9) = Uanis(C7) Uanis(C028) = Uanis(C21) = Uanis(C20) = Uanis(C032) = Uanis(C02Z) Uanis(C4) = Uanis(C0AA) = Uanis(C18B) = Uanis(C18A) = Uanis(C3) = Uanis(C5) Uanis(C02G) = Uanis(C02F) Uanis(C02N) = Uanis(Cl03) Uanis(C011) = Uanis(C00O) = Uanis(N2) = Uanis(N00E) = Uanis(N00M) Uanis(C2) = Uanis(C00N) = Uanis(C00P) Uanis(C018) = Uanis(C01M) = Uanis(C013) Uanis(C02A) = Uanis(C4) = Uanis(C0AA) = Uanis(C18B) = Uanis(C18A) = Uanis(C3) = Uanis(C5) 4. Others Fixed Sof: Cl00(0.75) Cl(0.25) H02K(0.5) H02L(0.5) H02I(0.5) H02J(0.5) HB(0.25) H2AA(0.25) HC(0.25) HD(0.25) HE(0.25) HF(0.25) HG(0.25) HH(0.25) C12(0.75) H12A(0.75) H12B(0.75) H12C(0.75) H3AA(0.75) HI(0.75) HJ(0.25) HK(0.25) C1AA(0.75) H1AA(0.75) H1AB(0.75) H1AC(0.75) C0(0.75) H0A(0.75) H0B(0.75) H0C(0.75) C0AA(0.5) H0AA(0.5) H0AB(0.5) H0AC(0.5) C02Z(0.5) H02(0.5) HO(0.5) C032(0.5) H03A(0.5) H03B(0.5) H03C(0.5) Cl8(0.25) C20(0.5) H20A(0.5) H20B(0.5) H20C(0.5) C21(0.5) H21A(0.5) H21B(0.5) C18B(0.5) H18A(0.5) H18B(0.5) H18C(0.5) C3(0.5) H3A(0.5) H3B(0.5) H3C(0.5) Cl6(0.25) Cl7(0.25) Cl10(0.25) C13(0.25) H13A(0.25) H13B(0.25) H13C(0.25) C9(0.25) H9A(0.25) H9B(0.25) H9C(0.25) C7(0.25) H7A(0.25) H7B(0.25) H7C(0.25) C4(0.5) H4A(0.5) H4B(0.5) H4C(0.5) C5(0.5) H5A(0.5) H5B(0.5) H5C(0.5) C18A(0.5) H18D(0.5) H18E(0.5) H18F(0.5) Cl0A(0.75) Cl2(0.75) C6(0.75) H6A(0.75) H6B(0.75) C8(0.75) H8A(0.75) H8B(0.75) 5.a Secondary CH2 refined with riding coordinates: C00J(H00A,H00B), C00Y(H00C,H00D), C010(H01A,H01B), C017(H01C,H01D), C018(H01E, H01F), C01T(H01S,H01T), C01X(H01U,H01W), C01Z(H01X,H01Y), C020(H02A,H02B), C028(H02K,H02L), C028(H02I,H02J), C02C(H02M,H02N), C02D(H02O,H02P), C02F(H4AA, H), C02G(H5AA,HA), C02I(HB,H2AA), C02I(HC,HD), C02I(HE,HF), C02I(HG,HH), C02M(H3AA,HI), C02M(HJ,HK), C02N(H6AA,HL), C02Z(H02,HO), C21(H21A,H21B), C6(H6A,H6B), C8(H8A,H8B) 5.b Aromatic/amide H refined with riding coordinates: C00P(H00P), C00R(H00R), C00S(H00S), C00W(H00W), C011(H011), C014(H014), C016(H016), C01A(H01G), C01B(H01H), C01D(H01I), C01G(H01J), C01I(H01K), C01J(H01L), C01L(H01M), C01P(H01Q), C01R(H01R), C01V(H01V), C025(H025) 5.c Idealised Me refined as rotating group: C01O(H01N,H01O,H01P), C021(H02C,H02D,H02E), C024(H02F,H02G,H02H), C02E(H02Q, H02R,H02S), C02K(H02T,H02U,H02V), C12(H12A,H12B,H12C), C02O(H02W,H02X,H02Y), C1AA(H1AA,H1AB,H1AC), C0(H0A,H0B,H0C), C02U(H02Z,HM,HN), C0AA(H0AA,H0AB,H0AC), C032(H03A,H03B,H03C), C20(H20A,H20B,H20C), C18B(H18A,H18B,H18C), C3(H3A,H3B, H3C), C13(H13A,H13B,H13C), C9(H9A,H9B,H9C), C7(H7A,H7B,H7C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C18A(H18D,H18E,H18F) ; _smtbx_masks_void_probe_radius 1.2 _smtbx_masks_void_truncation_radius 1.2 _shelx_res_file ; v839e.res created by SHELXL-2014/7 TITL v839e_a.res in P2(1)/c REM Old TITL v839e in P2(1)/c REM SHELXT solution in P2(1)/c REM R1 0.187, Rweak 0.081, Alpha 0.072, Orientation as input REM Formula found by SHELXT: C72 N20 O14 Cl7 Ir CELL 0.71073 19.636 13.1399 34.1989 90 103.304 90 ZERR 2 0.0013 0.0006 0.0022 0 0.002 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Cl Ir N O UNIT 310 396 38 4 24 16 DFIX 1.54 C21 C028 C02Z C028 C032 C02Z C21 C20 SADI 0.01 Cl00 C02M Cl8 C02M Cl C02I Cl7 C02I Cl10 C02I Cl6 C02I SADI 0.01 C0AA C02A C3 C02A C18B C02A SADI 0.01 C02Z C028 C21 C028 C21 C20 C032 C02Z SADI 0.01 C0AA C02A C4 C02A C5 C02A C3 C02A C18A C02A C18B C02A EADP Cl Cl7 Cl10 Cl6 EADP C02M Cl00 Cl8 C02I Cl6 Cl7 Cl10 Cl EADP C12 C1AA C0 C13 C9 C7 EADP C028 C21 C20 C032 C02Z EADP C4 C0AA C18B C18A C3 C5 EADP C02G C02F EADP C02N Cl03 EADP C011 C00O N2 N00E N00M EADP C2 C00N C00P EADP C018 C01M C013 EADP C02A C4 C0AA C18B C18A C3 C5 L.S. 8 PLAN 34 SIZE 0.35 0.12 0.02 TEMP -173.15 CONF list 4 MORE -1 BOND $H ABIN fmap 2 acta OMIT -2 50.4 OMIT 1 0 2 OMIT 0 1 1 OMIT -7 10 31 OMIT -6 10 31 OMIT -4 10 31 OMIT -5 10 31 OMIT 1 1 0 OMIT -3 10 31 OMIT 5 15 6 OMIT -1 1 1 OMIT -6 9 33 REM REM REM WGHT 0.075800 102.787704 FVAR 0.06293 IR1 4 0.492760 -0.112160 0.464357 11.00000 0.02208 0.02202 = 0.02182 -0.00161 0.00857 -0.00054 CL1 3 0.415186 0.022174 0.483369 11.00000 0.02585 0.02004 = 0.02276 -0.00437 0.00885 0.00208 CL03 3 0.963252 1.093987 0.542191 11.00000 0.07156 0.04336 = 0.05967 -0.00543 0.01943 -0.00221 CL04 3 0.487893 0.341369 0.670640 11.00000 0.05511 0.08463 = 0.04616 0.00018 0.00955 -0.00293 CL05 3 0.553565 0.501088 0.633575 11.00000 0.10227 0.04239 = 0.07490 -0.00017 0.01739 -0.01373 CL06 3 0.582490 0.761765 0.636936 11.00000 0.07852 0.04311 = 0.09578 -0.00175 0.01515 -0.00597 PART 1 CL00 3 0.685005 0.548236 0.579709 10.75000 0.06883 0.06753 = 0.07385 0.00813 0.01755 0.00030 PART 0 CL08 3 0.749407 0.818504 0.638197 11.00000 0.06042 0.11996 = 0.08313 -0.00900 0.00234 0.02784 O00A 6 0.713600 0.303694 0.406527 11.00000 0.04246 0.02859 = 0.02710 -0.00721 0.02126 -0.01224 O00B 6 0.607763 0.307430 0.312246 11.00000 0.02633 0.02366 = 0.05293 0.00017 0.01971 0.00154 N1 5 0.508160 -0.033185 0.415932 11.00000 0.02424 0.01994 = 0.03952 -0.00746 0.01452 -0.00057 N2 5 0.523712 0.213906 0.494452 11.00000 0.02887 0.02355 = 0.02983 -0.00150 0.00889 -0.00309 N00E 5 0.568210 0.214976 0.470738 11.00000 0.02887 0.02355 = 0.02983 -0.00150 0.00889 -0.00309 O00G 6 0.702945 0.108866 0.335162 11.00000 0.03285 0.02868 = 0.04515 -0.00602 0.02169 -0.00932 N00H 5 0.546494 0.043081 0.370879 11.00000 0.04501 0.03150 = 0.02728 0.00465 0.02780 0.00912 O00I 6 0.778691 0.083316 0.429294 11.00000 0.04294 0.02241 = 0.05406 0.00303 0.02324 -0.00464 C00J 1 0.602241 0.331263 0.423649 11.00000 0.03668 0.02474 = 0.02777 0.00247 0.01999 -0.00577 AFIX 23 H00A 2 0.606804 0.406077 0.421966 11.00000 -1.20000 H00B 2 0.578505 0.305764 0.396719 11.00000 -1.20000 AFIX 0 C00K 1 0.463898 -0.057867 0.380175 11.00000 0.03453 0.02097 = 0.02183 -0.00137 0.00534 0.00883 N00L 5 0.559115 0.027549 0.411020 11.00000 0.03230 0.02269 = 0.04487 -0.00395 0.02267 0.00276 N00M 5 0.559611 0.305650 0.453164 11.00000 0.02887 0.02355 = 0.02983 -0.00150 0.00889 -0.00309 C00N 1 0.439720 0.311064 0.519098 11.00000 0.02681 0.02571 = 0.02745 -0.00624 0.00821 -0.00508 C00O 1 0.486881 0.304342 0.492159 11.00000 0.02887 0.02355 = 0.02983 -0.00150 0.00889 -0.00309 C00P 1 0.397560 0.225353 0.571766 11.00000 0.02681 0.02571 = 0.02745 -0.00624 0.00821 -0.00508 AFIX 43 H00P 2 0.398458 0.169393 0.589467 11.00000 -1.20000 AFIX 0 C2 1 0.442015 0.225493 0.544407 11.00000 0.02681 0.02571 = 0.02745 -0.00624 0.00821 -0.00508 C00R 1 0.489031 -0.005753 0.351038 11.00000 0.04645 0.03116 = 0.01976 0.00453 0.01074 0.00545 AFIX 43 H00R 2 0.469514 -0.004947 0.322913 11.00000 -1.20000 AFIX 0 C00S 1 0.364961 -0.242727 0.425234 11.00000 0.02939 0.03646 = 0.03231 -0.00189 0.00532 -0.00788 AFIX 43 H00S 2 0.366999 -0.272225 0.450840 11.00000 -1.20000 AFIX 0 C00T 1 0.705347 0.423273 0.319585 11.00000 0.03136 0.02313 = 0.02913 0.00433 0.00931 -0.00030 C1 1 0.414202 -0.169730 0.420798 11.00000 0.01933 0.03604 = 0.02534 -0.01073 0.00135 -0.00139 C00V 1 0.408904 -0.129043 0.382144 11.00000 0.03376 0.03248 = 0.02010 -0.00385 0.00639 0.00383 C00W 1 0.352960 0.306160 0.572810 11.00000 0.03258 0.03166 = 0.03615 -0.01411 0.01498 -0.00278 AFIX 43 H00W 2 0.322819 0.304114 0.590905 11.00000 -1.20000 AFIX 0 C00X 1 0.668701 0.339680 0.300683 11.00000 0.02566 0.03170 = 0.03701 0.00962 0.01142 0.00392 C00Y 1 0.685974 0.476613 0.355418 11.00000 0.03194 0.02503 = 0.04028 -0.00642 0.01928 -0.00053 AFIX 23 H00C 2 0.673827 0.548531 0.348484 11.00000 -1.20000 H00D 2 0.644537 0.443122 0.361619 11.00000 -1.20000 AFIX 0 C00Z 1 0.746017 0.472126 0.391535 11.00000 0.02656 0.02191 = 0.03623 -0.00850 0.01652 -0.00027 C010 1 0.674588 0.283381 0.436457 11.00000 0.03250 0.04352 = 0.03434 0.00206 0.01493 -0.00925 AFIX 23 H01A 2 0.699568 0.311986 0.462613 11.00000 -1.20000 H01B 2 0.670073 0.208983 0.439672 11.00000 -1.20000 AFIX 0 C011 1 0.511966 0.364294 0.465281 11.00000 0.02887 0.02355 = 0.02983 -0.00150 0.00889 -0.00309 AFIX 43 H011 2 0.498558 0.431919 0.457152 11.00000 -1.20000 AFIX 0 C012 1 0.821586 0.373806 0.444562 11.00000 0.03642 0.02728 = 0.03467 0.00123 0.02033 0.00369 C013 1 0.692671 0.284402 0.271789 11.00000 0.02850 0.02973 = 0.03657 -0.00619 0.01266 -0.00529 C014 1 0.355879 -0.159166 0.349455 11.00000 0.04075 0.03867 = 0.02929 0.00200 0.00469 0.00480 AFIX 43 H014 2 0.352618 -0.129700 0.323723 11.00000 -1.20000 AFIX 0 C015 1 0.759864 0.383895 0.415275 11.00000 0.03512 0.02260 = 0.03681 -0.00411 0.02448 -0.00253 C016 1 0.395883 0.393316 0.521314 11.00000 0.04267 0.02586 = 0.04314 -0.00043 0.01717 0.00477 AFIX 43 H016 2 0.396316 0.451274 0.504767 11.00000 -1.20000 AFIX 0 C017 1 0.844543 0.270822 0.463780 11.00000 0.04559 0.02052 = 0.03270 0.00435 0.01510 -0.00045 AFIX 23 H01C 2 0.881660 0.280593 0.488528 11.00000 -1.20000 H01D 2 0.804388 0.236554 0.471172 11.00000 -1.20000 AFIX 0 C018 1 0.660416 0.182772 0.255709 11.00000 0.02850 0.02973 = 0.03657 -0.00619 0.01266 -0.00529 AFIX 23 H01E 2 0.619490 0.167918 0.267110 11.00000 -1.20000 H01F 2 0.644207 0.186200 0.226104 11.00000 -1.20000 AFIX 0 PART 1 CL 3 0.736701 0.422064 0.530630 10.25000 0.06883 0.06753 = 0.07385 0.00813 0.01755 0.00030 PART 0 C01A 1 0.867203 0.456008 0.452337 11.00000 0.03698 0.02215 = 0.03390 -0.00384 0.01429 0.00282 AFIX 43 H01G 2 0.908600 0.450347 0.473034 11.00000 -1.20000 AFIX 0 C01B 1 0.750986 0.319241 0.259654 11.00000 0.03277 0.03211 = 0.02414 -0.00460 0.00388 -0.00409 AFIX 43 H01H 2 0.766550 0.282728 0.239368 11.00000 -1.20000 AFIX 0 C01C 1 0.871944 0.205656 0.434183 11.00000 0.04571 0.02186 = 0.02503 0.00623 0.00730 0.00504 C01D 1 0.351189 0.390702 0.547890 11.00000 0.04047 0.03070 = 0.04884 -0.00571 0.01889 0.01320 AFIX 43 H01I 2 0.320179 0.445611 0.548924 11.00000 -1.20000 AFIX 0 C01E 1 0.957527 0.183231 0.392874 11.00000 0.03293 0.02754 = 0.02884 0.00628 0.00645 0.01131 C01F 1 0.735521 0.066672 0.307159 11.00000 0.03024 0.01895 = 0.04788 -0.00726 0.02163 -0.00655 C01G 1 0.764607 0.455036 0.306825 11.00000 0.02737 0.02859 = 0.02896 -0.00218 0.00656 -0.00042 AFIX 43 H01J 2 0.790067 0.512163 0.319544 11.00000 -1.20000 AFIX 0 C01H 1 0.787870 0.405797 0.275987 11.00000 0.02829 0.04253 = 0.02913 0.00874 0.00779 -0.00015 C01I 1 0.931468 0.235194 0.421689 11.00000 0.03058 0.02671 = 0.03284 0.01209 0.00564 0.00112 AFIX 43 H01K 2 0.955716 0.294202 0.433499 11.00000 -1.20000 AFIX 0 C01J 1 0.919916 0.099375 0.375083 11.00000 0.04082 0.02725 = 0.02631 -0.00144 0.01056 0.00958 AFIX 43 H01L 2 0.935646 0.063696 0.354656 11.00000 -1.20000 AFIX 0 C01L 1 0.312839 -0.272566 0.392316 11.00000 0.04009 0.04560 = 0.03963 -0.01234 0.00690 -0.01233 AFIX 43 H01M 2 0.279664 -0.322199 0.395956 11.00000 -1.20000 AFIX 0 C01M 1 0.714481 0.098842 0.267160 11.00000 0.02850 0.02973 = 0.03657 -0.00619 0.01266 -0.00529 C01N 1 0.906483 0.637334 0.439349 11.00000 0.03896 0.02794 = 0.04680 -0.00621 0.01038 -0.00309 C01O 1 0.752247 -0.118796 0.502357 11.00000 0.03964 0.05949 = 0.07583 0.02597 0.00214 -0.00328 AFIX 137 H01N 2 0.779824 -0.173035 0.493776 11.00000 -1.50000 H01O 2 0.708429 -0.147196 0.506698 11.00000 -1.50000 H01P 2 0.779001 -0.088742 0.527441 11.00000 -1.50000 AFIX 0 C01P 1 0.748580 0.058064 0.239091 11.00000 0.03192 0.04352 = 0.03662 -0.01138 0.00610 -0.00013 AFIX 43 H01Q 2 0.733229 0.077158 0.211680 11.00000 -1.20000 AFIX 0 C01Q 1 0.791201 0.000044 0.319398 11.00000 0.03511 0.02501 = 0.04516 -0.00770 0.01629 0.00052 C01R 1 0.308068 -0.232462 0.354924 11.00000 0.03425 0.05223 = 0.03549 -0.00814 -0.00150 -0.00976 AFIX 43 H01R 2 0.272326 -0.254571 0.332863 11.00000 -1.20000 AFIX 0 C01S 1 0.859289 0.065533 0.386318 11.00000 0.04198 0.02228 = 0.03065 0.00779 0.00747 0.00784 C01T 1 0.595095 0.105553 0.354843 11.00000 0.05360 0.03575 = 0.05909 0.01373 0.04322 -0.00002 AFIX 23 H01S 2 0.613019 0.161265 0.373929 11.00000 -1.20000 H01T 2 0.570145 0.136542 0.329144 11.00000 -1.20000 AFIX 0 C01U 1 0.837515 0.118271 0.416923 11.00000 0.02949 0.02715 = 0.03523 0.00168 0.00933 0.00078 C01V 1 0.793424 0.552923 0.400355 11.00000 0.03561 0.02033 = 0.04108 0.00573 0.01827 0.00859 AFIX 43 H01V 2 0.783717 0.613803 0.385106 11.00000 -1.20000 AFIX 0 C01W 1 0.853889 0.547508 0.430440 11.00000 0.03556 0.02313 = 0.04114 -0.00794 0.01682 -0.00247 C01X 1 0.819337 -0.023946 0.363444 11.00000 0.04673 0.02325 = 0.04670 -0.00551 0.01605 0.00283 AFIX 23 H01U 2 0.850841 -0.083601 0.365943 11.00000 -1.20000 H01W 2 0.779902 -0.042055 0.375670 11.00000 -1.20000 AFIX 0 C01Y 1 0.804427 -0.009766 0.249970 11.00000 0.03125 0.04951 = 0.04902 -0.02340 0.01593 -0.00492 C01Z 1 0.526205 0.374114 0.630741 11.00000 0.05090 0.04656 = 0.04940 -0.00600 0.01559 -0.00317 AFIX 23 H01X 2 0.566931 0.329314 0.631237 11.00000 -1.20000 H01Y 2 0.491885 0.362832 0.604959 11.00000 -1.20000 AFIX 0 C020 1 0.736093 -0.037992 0.470328 11.00000 0.03960 0.05634 = 0.06280 0.02355 -0.00500 -0.00561 AFIX 23 H02A 2 0.707462 -0.068427 0.445443 11.00000 -1.20000 H02B 2 0.707831 0.016056 0.479140 11.00000 -1.20000 AFIX 0 C021 1 1.037226 0.165072 0.343993 11.00000 0.04689 0.06260 = 0.05121 0.00018 0.02573 -0.00427 AFIX 137 H02C 2 1.039468 0.091124 0.347802 11.00000 -1.50000 H02D 2 1.081112 0.189241 0.338234 11.00000 -1.50000 H02E 2 0.998164 0.182047 0.321447 11.00000 -1.50000 AFIX 0 C022 1 1.026300 0.215782 0.381862 11.00000 0.04203 0.04019 = 0.03250 0.00222 0.01323 0.00101 C023 1 0.850209 0.443957 0.260141 11.00000 0.04174 0.05314 = 0.04388 -0.00714 0.02339 -0.01533 C024 1 1.087986 0.186770 0.417787 11.00000 0.04049 0.08360 = 0.05510 -0.00333 0.01121 0.00145 AFIX 137 H02F 2 1.083291 0.223989 0.441861 11.00000 -1.50000 H02G 2 1.132528 0.204680 0.411247 11.00000 -1.50000 H02H 2 1.086864 0.113429 0.422807 11.00000 -1.50000 AFIX 0 C025 1 0.824811 -0.037680 0.290090 11.00000 0.03491 0.03004 = 0.05383 -0.01445 0.00948 0.00312 AFIX 43 H025 2 0.862717 -0.083799 0.298107 11.00000 -1.20000 AFIX 0 C028 1 0.549097 0.368829 0.296649 11.00000 0.03414 0.08652 = 0.09602 0.02181 0.01607 0.01038 PART 2 AFIX 23 H02K 2 0.563098 0.440897 0.301673 10.50000 -1.20000 H02L 2 0.512999 0.354212 0.311871 10.50000 -1.20000 AFIX 23 PART 0 PART 1 H02I 2 0.551799 0.388007 0.269052 10.50000 -1.20000 H02J 2 0.555248 0.432326 0.312661 10.50000 -1.20000 AFIX 0 PART 0 C02A 1 0.844091 -0.049061 0.218710 11.00000 0.06376 0.09822 = 0.06842 -0.02248 0.03724 0.01682 C02C 1 0.798715 0.008195 0.461269 11.00000 0.05542 0.03695 = 0.04762 0.01636 0.01449 -0.00222 AFIX 23 H02M 2 0.826832 0.041388 0.485685 11.00000 -1.20000 H02N 2 0.827818 -0.045304 0.452825 11.00000 -1.20000 AFIX 0 C02D 1 0.654332 0.044383 0.348108 11.00000 0.05143 0.02707 = 0.11552 -0.00566 0.04649 -0.00421 AFIX 23 H02O 2 0.677604 0.009584 0.373322 11.00000 -1.20000 H02P 2 0.637049 -0.008163 0.327463 11.00000 -1.20000 AFIX 0 C02E 1 0.890647 0.528575 0.286099 11.00000 0.04393 0.06112 = 0.06831 -0.01265 0.02580 -0.01679 AFIX 137 H02Q 2 0.859346 0.586263 0.286860 11.00000 -1.50000 H02R 2 0.929616 0.550684 0.274669 11.00000 -1.50000 H02S 2 0.908939 0.503098 0.313434 11.00000 -1.50000 AFIX 0 C02F 1 0.673869 0.883645 0.611966 11.00000 0.07219 0.06394 = 0.05494 0.00809 -0.00162 0.00271 AFIX 23 H4AA 2 0.661237 0.936534 0.629668 11.00000 -1.20000 H 2 0.684350 0.918141 0.588291 11.00000 -1.20000 AFIX 0 C02G 1 0.613969 0.814579 0.598544 11.00000 0.07219 0.06394 = 0.05494 0.00809 -0.00162 0.00271 AFIX 23 H5AA 2 0.628181 0.759006 0.582561 11.00000 -1.20000 HA 2 0.575630 0.852683 0.580643 11.00000 -1.20000 AFIX 0 C02I 1 0.787892 0.532662 0.535823 11.00000 0.06883 0.06753 = 0.07385 0.00813 0.01755 0.00030 PART 1 AFIX 23 HB 2 0.836474 0.518733 0.550757 10.25000 -1.20000 H2AA 2 0.788756 0.562062 0.509288 10.25000 -1.20000 AFIX 23 PART 0 PART 4 HC 2 0.813844 0.573571 0.519741 10.25000 -1.20000 HD 2 0.752944 0.490840 0.517118 10.25000 -1.20000 AFIX 23 PART 0 PART 2 HE 2 0.837183 0.555646 0.541117 10.25000 -1.20000 HF 2 0.767371 0.546078 0.507036 10.25000 -1.20000 AFIX 23 PART 0 PART 3 HG 2 0.820429 0.572730 0.523676 10.25000 -1.20000 HH 2 0.753007 0.500241 0.513811 10.25000 -1.20000 AFIX 0 PART 0 C02K 1 0.823504 0.484376 0.217032 11.00000 0.07183 0.10766 = 0.05746 0.01485 0.03147 -0.03396 AFIX 137 H02T 2 0.795536 0.431686 0.200410 11.00000 -1.50000 H02U 2 0.863463 0.502281 0.205719 11.00000 -1.50000 H02V 2 0.794531 0.544866 0.217551 11.00000 -1.50000 AFIX 0 PART 1 C12 1 0.920226 0.665127 0.484343 10.75000 0.05116 0.03405 = 0.05948 -0.00625 0.00618 -0.01059 AFIX 137 H12A 2 0.875711 0.680468 0.491413 10.75000 -1.50000 H12B 2 0.950836 0.724876 0.489654 10.75000 -1.50000 H12C 2 0.942856 0.607681 0.500528 10.75000 -1.50000 AFIX 0 PART 0 C02M 1 0.750850 0.602982 0.559415 11.00000 0.06883 0.06753 = 0.07385 0.00813 0.01755 0.00030 PART 1 AFIX 23 H3AA 2 0.729847 0.659556 0.541547 10.75000 -1.20000 HI 2 0.786458 0.632885 0.581730 10.75000 -1.20000 AFIX 23 PART 0 PART 2 HJ 2 0.725334 0.641232 0.535580 10.25000 -1.20000 HK 2 0.792419 0.645993 0.569946 10.25000 -1.20000 AFIX 0 PART 0 C02N 1 0.991503 0.986243 0.518743 11.00000 0.07156 0.04336 = 0.05967 -0.00543 0.01943 -0.00221 AFIX 23 H6AA 2 1.033221 0.956230 0.536970 11.00000 -1.20000 HL 2 0.954023 0.934228 0.513680 11.00000 -1.20000 AFIX 0 C02O 1 1.027438 0.332031 0.375955 11.00000 0.06908 0.05167 = 0.05939 -0.00345 0.03219 -0.01199 AFIX 137 H02W 2 0.987558 0.352206 0.354422 11.00000 -1.50000 H02X 2 1.071102 0.351625 0.368715 11.00000 -1.50000 H02Y 2 1.024378 0.366159 0.400973 11.00000 -1.50000 AFIX 0 PART 1 C1AA 1 0.976834 0.601653 0.431042 10.75000 0.05116 0.03405 = 0.05948 -0.00625 0.00618 -0.01059 AFIX 137 H1AA 2 0.993752 0.542070 0.447689 10.75000 -1.50000 H1AB 2 1.011269 0.656683 0.437566 10.75000 -1.50000 H1AC 2 0.970083 0.583586 0.402605 10.75000 -1.50000 AFIX 0 C0 1 0.883050 0.729790 0.414204 10.75000 0.05116 0.03405 = 0.05948 -0.00625 0.00618 -0.01059 AFIX 137 H0A 2 0.876855 0.712454 0.385730 10.75000 -1.50000 H0B 2 0.918433 0.783396 0.421341 10.75000 -1.50000 H0C 2 0.838535 0.753991 0.419093 10.75000 -1.50000 AFIX 0 PART 0 C02U 1 0.901022 0.355342 0.259346 11.00000 0.05105 0.07036 = 0.10446 -0.03885 0.04753 -0.01428 AFIX 137 H02Z 2 0.913618 0.323474 0.285944 11.00000 -1.50000 HM 2 0.943348 0.381177 0.252159 11.00000 -1.50000 HN 2 0.878484 0.304902 0.239427 11.00000 -1.50000 AFIX 0 PART 2 C0AA 1 0.792137 -0.086108 0.180440 10.50000 0.06376 0.09822 = 0.06842 -0.02248 0.03724 0.01682 AFIX 137 H0AA 2 0.817902 -0.105694 0.160238 10.50000 -1.50000 H0AB 2 0.759311 -0.031213 0.169788 10.50000 -1.50000 H0AC 2 0.766167 -0.144971 0.186964 10.50000 -1.50000 AFIX 0 C02Z 1 0.516383 0.356847 0.252783 10.50000 0.03414 0.08652 = 0.09602 0.02181 0.01607 0.01038 AFIX 23 H02 2 0.497117 0.287418 0.246998 10.50000 -1.20000 HO 2 0.551227 0.369326 0.236508 10.50000 -1.20000 AFIX 0 C032 1 0.458636 0.435278 0.243609 10.50000 0.03414 0.08652 = 0.09602 0.02181 0.01607 0.01038 AFIX 137 H03A 2 0.472070 0.490264 0.227539 10.50000 -1.50000 H03B 2 0.450912 0.463193 0.268809 10.50000 -1.50000 H03C 2 0.415467 0.403251 0.228530 10.50000 -1.50000 AFIX 0 CL8 3 0.702029 0.652245 0.591703 10.25000 0.06883 0.06753 = 0.07385 0.00813 0.01755 0.00030 PART 0 PART 1 C20 1 0.420431 0.399701 0.268509 10.50000 0.03414 0.08652 = 0.09602 0.02181 0.01607 0.01038 AFIX 137 H20A 2 0.379391 0.358383 0.256507 10.50000 -1.50000 H20B 2 0.439214 0.430829 0.247159 10.50000 -1.50000 H20C 2 0.406840 0.453213 0.285173 10.50000 -1.50000 AFIX 0 C21 1 0.475642 0.332976 0.294213 10.50000 0.03414 0.08652 = 0.09602 0.02181 0.01607 0.01038 AFIX 23 H21A 2 0.467461 0.330205 0.321697 10.50000 -1.20000 H21B 2 0.470632 0.263004 0.283189 10.50000 -1.20000 AFIX 0 C18B 1 0.855797 -0.164965 0.224527 10.50000 0.06376 0.09822 = 0.06842 -0.02248 0.03724 0.01682 AFIX 137 H18A 2 0.810696 -0.200232 0.216991 10.50000 -1.50000 H18B 2 0.877665 -0.179209 0.252753 10.50000 -1.50000 H18C 2 0.886448 -0.188913 0.207526 10.50000 -1.50000 AFIX 0 C3 1 0.917162 0.000800 0.230416 10.50000 0.06376 0.09822 = 0.06842 -0.02248 0.03724 0.01682 AFIX 137 H3A 2 0.945667 -0.022826 0.212158 10.50000 -1.50000 H3B 2 0.939944 -0.018090 0.258052 10.50000 -1.50000 H3C 2 0.912253 0.074962 0.228468 10.50000 -1.50000 AFIX 0 PART 0 PART 4 CL6 3 0.845789 0.453591 0.568387 10.25000 0.06883 0.06753 = 0.07385 0.00813 0.01755 0.00030 PART 0 PART 2 CL7 3 0.790053 0.401962 0.541640 10.25000 0.06883 0.06753 = 0.07385 0.00813 0.01755 0.00030 PART 0 PART 3 CL10 3 0.834557 0.438632 0.567017 10.25000 0.06883 0.06753 = 0.07385 0.00813 0.01755 0.00030 PART 0 PART 2 C13 1 0.858164 0.736238 0.445851 10.25000 0.05116 0.03405 = 0.05948 -0.00625 0.00618 -0.01059 AFIX 137 H13A 2 0.816478 0.739498 0.423698 10.25000 -1.50000 H13B 2 0.885480 0.798841 0.446357 10.25000 -1.50000 H13C 2 0.843904 0.728976 0.471351 10.25000 -1.50000 AFIX 0 C9 1 0.963273 0.625523 0.474554 10.25000 0.05116 0.03405 = 0.05948 -0.00625 0.00618 -0.01059 AFIX 137 H9A 2 0.944048 0.612844 0.498130 10.25000 -1.50000 H9B 2 0.991490 0.687789 0.478750 10.25000 -1.50000 H9C 2 0.992692 0.567947 0.470596 10.25000 -1.50000 AFIX 0 C7 1 0.929447 0.660614 0.398991 10.25000 0.05116 0.03405 = 0.05948 -0.00625 0.00618 -0.01059 AFIX 137 H7A 2 0.956463 0.603099 0.392316 10.25000 -1.50000 H7B 2 0.958372 0.722187 0.402316 10.25000 -1.50000 H7C 2 0.887773 0.671017 0.377269 10.25000 -1.50000 AFIX 0 PART 0 PART 1 C4 1 0.807778 -0.018262 0.175484 10.50000 0.06376 0.09822 = 0.06842 -0.02248 0.03724 0.01682 AFIX 137 H4A 2 0.831361 -0.051277 0.156541 10.50000 -1.50000 H4B 2 0.810192 0.055786 0.172657 10.50000 -1.50000 H4C 2 0.758676 -0.039699 0.169752 10.50000 -1.50000 AFIX 0 PART 0 PART 2 C5 1 0.880044 0.043052 0.203833 10.50000 0.06376 0.09822 = 0.06842 -0.02248 0.03724 0.01682 AFIX 137 H5A 2 0.918334 0.019089 0.192200 10.50000 -1.50000 H5B 2 0.898765 0.088464 0.226488 10.50000 -1.50000 H5C 2 0.845836 0.080025 0.183376 10.50000 -1.50000 AFIX 0 C18A 1 0.898129 -0.133063 0.234556 10.50000 0.06376 0.09822 = 0.06842 -0.02248 0.03724 0.01682 AFIX 137 H18D 2 0.875250 -0.189108 0.245463 10.50000 -1.50000 H18E 2 0.935774 -0.105144 0.255767 10.50000 -1.50000 H18F 2 0.917739 -0.158374 0.212520 10.50000 -1.50000 AFIX 0 PART 0 CL0A 3 0.404040 0.125153 0.253699 10.75000 0.10300 0.08589 = 0.05081 0.01543 0.02440 0.04131 CL2 3 0.298324 0.257364 0.178583 10.75000 0.13377 0.03148 = 0.08902 -0.01616 0.01162 0.01804 C6 1 0.291469 0.248534 0.225475 10.75000 0.10115 AFIX 23 H6A 2 0.308708 0.314333 0.238052 10.75000 -1.20000 H6B 2 0.240585 0.247177 0.224169 10.75000 -1.20000 AFIX 0 C8 1 0.322642 0.168772 0.255761 10.75000 0.10165 AFIX 23 H8A 2 0.290267 0.109988 0.252279 10.75000 -1.20000 H8B 2 0.325401 0.196856 0.282943 10.75000 -1.20000 AFIX 0 HKLF 4 REM v839e_a.res in P2(1)/c REM R1 = 0.0741 for 11175 Fo > 4sig(Fo) and 0.1011 for all 15109 data REM 819 parameters refined using 40 restraints END WGHT 0.0758 102.7954 REM Highest difference peak 1.815, deepest hole -2.568, 1-sigma level 0.172 Q1 1 0.3795 0.1669 0.2837 11.00000 0.05 1.77 Q2 1 0.2729 0.2303 0.2010 11.00000 0.05 1.70 Q3 1 0.8818 0.4778 0.5632 11.00000 0.05 1.63 Q4 1 0.3403 0.1131 0.2787 11.00000 0.05 1.52 Q5 1 0.5243 -0.1066 0.4860 11.00000 0.05 1.36 Q6 1 0.5677 0.7836 0.6095 11.00000 0.05 1.31 Q7 1 0.4317 0.0201 0.2935 11.00000 0.05 1.30 Q8 1 0.5161 -0.0536 0.4652 11.00000 0.05 1.29 Q9 1 0.5522 -0.1131 0.4492 11.00000 0.05 1.23 Q10 1 0.4594 -0.1103 0.4415 11.00000 0.05 1.21 Q11 1 0.4698 -0.0549 0.4654 11.00000 0.05 1.21 Q12 1 0.4416 0.1387 0.5432 11.00000 0.05 1.15 Q13 1 0.5183 -0.1691 0.4669 11.00000 0.05 1.11 Q14 1 0.7591 0.8950 0.6519 11.00000 0.05 1.06 Q15 1 0.4780 0.2344 0.6800 11.00000 0.05 1.04 Q16 1 0.3026 0.2764 0.2354 11.00000 0.05 0.99 Q17 1 0.6218 0.4940 0.5885 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0.0859 18 2 10 0.5648 -0.0833 18 2 11 -2.4480 0.1873 18 2 12 -4.2357 0.0874 18 2 13 2.2624 0.1342 18 2 14 -5.3901 0.0306 18 2 15 -5.9255 0.1219 18 2 16 1.6495 -0.2332 18 2 17 1.7370 -0.0656 18 3 0 2.3914 -0.0388 18 3 1 1.2373 -0.1761 18 3 2 -0.5102 0.0070 18 3 3 -6.4770 0.0575 18 3 4 -4.6525 0.0197 18 3 5 -2.9886 0.0872 18 3 6 0.5715 0.1297 18 3 7 0.1053 -0.2571 18 3 8 -0.9550 0.0039 18 3 9 -0.3310 -0.1362 18 3 10 -2.9734 -0.1271 18 3 11 2.4292 0.0591 18 3 12 2.4268 -0.4481 18 3 13 2.6233 0.1892 18 3 14 4.1356 -0.5448 18 3 15 -0.9961 -0.0571 18 3 16 3.5903 0.1561 18 3 17 4.5402 0.2227 18 4 0 -1.2107 0.2593 18 4 1 -4.8436 0.0419 18 4 2 -2.7269 0.1230 18 4 3 0.7626 0.0660 18 4 4 2.2993 -0.0226 18 4 5 1.7110 -0.1188 18 4 6 0.5792 -0.0125 18 4 7 3.3691 -0.0767 18 4 8 -3.8867 0.0490 18 4 9 2.2854 0.2320 18 4 10 2.2353 -0.2096 18 4 11 0.4935 0.4787 18 4 12 0.4590 -0.2414 18 4 13 0.2186 0.5010 18 4 14 -2.1018 0.4392 18 4 15 -4.5602 -0.0857 18 4 16 0.9074 0.1137 18 5 0 -0.2201 -0.0080 18 5 1 2.0342 -0.1126 18 5 2 -4.3870 0.0314 18 5 3 1.3167 -0.0985 18 5 4 -1.2118 -0.0760 18 5 5 -0.1766 0.2018 18 5 6 0.3866 -0.0773 18 5 7 3.2507 0.4525 18 5 8 -0.8957 -0.1500 18 5 9 0.5928 0.1960 18 5 10 1.1010 0.0875 18 5 11 3.1175 0.2259 18 5 12 -5.9769 -0.3085 18 5 13 -5.2375 -0.5426 18 5 14 1.6260 -0.0925 18 5 15 1.4401 -0.3396 18 6 0 -5.4897 0.0965 18 6 1 2.1695 0.0473 18 6 2 -0.2381 -0.0228 18 6 3 7.3187 0.1767 18 6 4 8.7317 -0.3096 18 6 5 0.3587 0.3465 18 6 6 2.3138 -0.5328 18 6 7 2.7938 0.0492 18 6 8 1.8718 -0.1095 18 6 9 -2.0742 -0.2962 18 6 10 -4.4778 -0.2802 18 6 11 -2.6528 -0.0149 18 6 12 -0.0649 0.0464 18 6 13 3.2326 0.1912 18 7 0 0.2684 -0.4566 18 7 1 4.3750 0.1351 18 7 2 2.0041 -0.4222 18 7 3 -6.0060 0.1698 18 7 4 -3.5616 -0.2676 18 7 5 -7.0830 0.4225 18 7 6 0.3166 -0.2434 18 7 7 -13.4832 0.3715 18 7 8 -1.9540 0.1508 18 7 9 -9.6502 0.3872 18 7 10 -1.8937 0.0543 18 7 11 4.6391 0.0623 18 8 0 -0.0493 -0.0927 18 8 1 -2.0879 0.4167 18 8 2 -0.6829 0.0028 18 8 3 -4.0485 0.2896 18 8 4 2.4629 -0.2187 18 8 5 -8.8408 0.4114 18 8 6 11.5139 -0.3662 18 8 7 -12.6732 0.1217 18 8 8 11.9008 -0.2919 18 9 0 0.7505 -0.2578 18 9 1 -0.1058 -0.2043 18 9 2 0.0841 -0.1949 18 9 3 -2.5205 -0.1238 18 9 4 6.7323 -0.0008 19 0 0 -7.7507 -0.0706 19 0 2 4.3841 -0.0989 19 0 4 -4.1514 -0.0576 19 0 6 -1.2990 -0.0198 19 0 8 1.8363 0.0359 19 0 10 2.4579 -0.0050 19 0 12 -1.8142 -0.0649 19 0 14 -4.3434 0.0945 19 1 0 4.3422 0.0406 19 1 1 3.0595 -0.0341 19 1 2 -3.5543 0.0955 19 1 3 -2.7475 -0.0692 19 1 4 -1.7452 0.3066 19 1 5 -0.4638 0.1532 19 1 6 2.3308 0.3562 19 1 7 -1.1620 0.1684 19 1 8 0.4008 0.2731 19 1 9 0.2453 0.0720 19 1 10 -0.5815 0.1104 19 1 11 -3.5911 0.3696 19 1 12 0.3566 -0.4404 19 1 13 4.4694 0.0896 19 1 14 1.3497 -0.4756 19 1 15 1.7891 -0.6374 19 2 0 -5.3119 0.0458 19 2 1 -0.3233 0.0443 19 2 2 0.6733 0.2364 19 2 3 2.0641 0.0346 19 2 4 6.5154 -0.1351 19 2 5 0.3820 -0.0109 19 2 6 0.4594 -0.0200 19 2 7 0.4186 -0.0962 19 2 8 3.6750 0.0631 19 2 9 0.7929 -0.1615 19 2 10 1.9333 -0.2201 19 2 11 0.1946 -0.0516 19 2 12 -1.3785 -0.1858 19 2 13 3.3959 0.1210 19 2 14 -2.2694 0.2625 19 2 15 -6.4990 0.4032 19 3 0 6.5214 -0.1260 19 3 1 6.4456 -0.2279 19 3 2 3.7194 -0.0861 19 3 3 -1.8916 -0.0873 19 3 4 -2.7969 0.0011 19 3 5 -4.8725 0.1016 19 3 6 1.3037 -0.0160 19 3 7 -2.0114 -0.2471 19 3 8 -0.9224 0.0583 19 3 9 -1.8385 -0.2731 19 3 10 -4.9196 0.3642 19 3 11 -1.7791 0.1982 19 3 12 -1.3067 0.1052 19 3 13 -1.5869 0.3040 19 3 14 -0.1709 -0.5219 19 4 0 0.6593 0.0143 19 4 1 -4.8029 -0.0026 19 4 2 -4.4763 0.2179 19 4 3 -0.3675 0.0581 19 4 4 0.2249 0.1200 19 4 5 -1.8571 -0.1239 19 4 6 2.3663 0.0768 19 4 7 1.8471 -0.2288 19 4 8 -1.1924 0.4034 19 4 9 1.3213 -0.1860 19 4 10 3.4972 -0.1128 19 4 11 0.2940 -0.1263 19 4 12 3.2541 -0.7312 19 4 13 6.4458 0.2695 19 5 0 0.4666 0.1703 19 5 1 3.0658 -0.0456 19 5 2 -6.5030 0.2186 19 5 3 -0.5789 -0.4064 19 5 4 -5.1570 0.0740 19 5 5 -3.0166 -0.3112 19 5 6 0.5317 0.0648 19 5 7 2.4099 -0.0769 19 5 8 -2.0621 -0.0507 19 5 9 -1.9622 -0.0254 19 5 10 1.5237 0.3115 19 5 11 4.2926 0.8026 19 5 12 -7.5227 -0.1081 19 6 0 -8.5956 0.2225 19 6 1 0.8987 -0.3432 19 6 2 -8.5408 0.3130 19 6 3 5.3108 -0.2147 19 6 4 5.0188 0.3761 19 6 5 8.8901 0.1366 19 6 6 -0.3965 0.1502 19 6 7 9.8532 0.1761 19 6 8 2.3029 0.2395 19 6 9 -0.1292 0.0071 19 6 10 -3.9780 -0.5741 19 7 0 -2.5498 0.1643 19 7 1 9.6376 -0.1699 19 7 2 3.9242 0.0313 19 7 3 10.7729 -0.3458 19 7 4 -5.7209 0.0168 19 7 5 14.1806 -0.2921 19 7 6 -6.2789 -0.4517 19 7 7 -7.2652 0.0059 19 8 0 -5.2098 -0.2210 19 8 1 -0.8969 0.1189 19 8 2 -9.3586 0.0494 19 8 3 6.1365 0.2552 19 8 4 -17.9162 -0.0368 20 0 0 -4.2416 -0.0222 20 0 2 2.2320 -0.0776 20 0 4 -5.2268 -0.0970 20 0 6 -0.0254 -0.0679 20 0 8 1.1202 0.0611 20 0 10 3.6731 -0.0489 20 0 12 2.9935 -0.2039 20 1 0 1.8908 -0.0589 20 1 1 5.1375 -0.0563 20 1 2 -3.6265 -0.1353 20 1 3 0.8413 -0.2196 20 1 4 -2.9113 -0.1071 20 1 5 0.8704 -0.0369 20 1 6 0.1041 0.2157 20 1 7 -3.4611 -0.1487 20 1 8 -0.0060 0.4220 20 1 9 -1.0775 -0.1501 20 1 10 1.5837 0.4045 20 1 11 -3.5130 0.0807 20 1 12 -3.8892 0.2986 20 2 0 -5.0137 -0.0535 20 2 1 -1.8905 -0.0008 20 2 2 -5.0623 0.0934 20 2 3 0.5638 0.1194 20 2 4 1.8554 -0.0378 20 2 5 0.5157 0.0112 20 2 6 0.1742 0.2444 20 2 7 -0.4540 -0.0243 20 2 8 6.2060 0.2672 20 2 9 1.5939 -0.0766 20 2 10 1.0450 0.1947 20 2 11 1.8394 -0.2181 20 2 12 -1.5413 -0.3471 20 3 0 4.7225 -0.0439 20 3 1 4.6861 0.0149 20 3 2 5.4509 0.0241 20 3 3 3.6457 0.0266 20 3 4 0.0604 0.2483 20 3 5 -1.4393 0.1762 20 3 6 1.6630 -0.0301 20 3 7 -2.2514 -0.0971 20 3 8 -0.3096 -0.2308 20 3 9 -0.3360 -0.6537 20 3 10 -4.1740 0.1188 20 3 11 -0.0504 -0.1365 20 4 0 5.7647 -0.1980 20 4 1 -4.1180 -0.1545 20 4 2 0.0575 -0.0266 20 4 3 1.2744 -0.1259 20 4 4 -2.8061 -0.1677 20 4 5 -2.7954 -0.1023 20 4 6 0.0412 -0.2662 20 4 7 0.4031 -0.1098 20 4 8 1.9333 0.6074 20 4 9 -0.1989 0.0853 20 4 10 0.6432 0.7124 20 5 0 8.5072 0.1321 20 5 1 3.6718 0.3573 20 5 2 -0.4298 0.2212 20 5 3 -0.4572 0.1646 20 5 4 -6.8439 0.1582 20 5 5 -5.8006 0.0663 20 5 6 6.0009 0.1837 20 5 7 0.2898 -0.2949 20 5 8 1.2990 -0.0824 20 6 0 -4.1833 -0.1442 20 6 1 -7.7093 -0.2298 20 6 2 -13.3343 -0.2227 20 6 3 -11.0971 -0.3500 20 6 4 4.3628 -0.0128 20 6 5 0.1745 -0.4119 20 6 6 0.4625 0.3224 20 7 0 -1.1178 0.3680 20 7 1 -0.4524 -0.0314 20 7 2 10.9049 0.4953 20 7 3 5.8496 -0.2336 21 0 0 1.3676 0.0533 21 0 2 2.9757 0.0752 21 0 4 -6.4424 0.0128 21 0 6 0.4654 0.0089 21 0 8 -0.7027 0.2791 21 1 0 2.3332 -0.0477 21 1 1 2.6667 -0.1538 21 1 2 -1.0415 -0.1210 21 1 3 3.6312 -0.2229 21 1 4 -0.1833 -0.4411 21 1 5 4.6855 0.1291 21 1 6 -1.5982 -0.1212 21 1 7 -3.7438 -0.1017 21 1 8 -1.6723 0.2564 21 1 9 -2.5824 -0.1606 21 2 0 -0.9136 0.0601 21 2 1 -0.5071 0.0649 21 2 2 -5.6505 -0.0428 21 2 3 -2.6969 0.3485 21 2 4 -3.9611 -0.2835 21 2 5 -2.3310 0.0842 21 2 6 -3.7561 -0.0136 21 2 7 -1.1783 -0.2252 21 2 8 9.4468 -0.0520 21 3 0 -0.8759 -0.4796 21 3 1 -1.1349 0.0836 21 3 2 4.0743 -0.2798 21 3 3 2.6921 0.1114 21 3 4 5.1289 0.2063 21 3 5 4.4398 0.2606 21 3 6 3.4847 0.3140 21 3 7 -0.7043 0.4981 21 4 0 3.8675 0.1206 21 4 1 -6.5312 0.2079 21 4 2 7.4307 0.1931 21 4 3 0.4256 -0.1009 21 4 4 -5.1800 -0.1301 21 4 5 -2.4135 -0.1695 21 4 6 -9.1369 -0.7635 21 5 0 12.5888 -0.1796 21 5 1 4.9462 -0.2666 21 5 2 8.0673 -0.1734 21 5 3 5.3944 0.1016 21 5 4 -11.1203 -0.0213 21 6 0 6.0465 0.1625 21 6 1 -2.3078 0.4686 22 0 0 0.6705 -0.1791 22 0 2 3.1739 -0.1578 22 0 4 -7.3991 -0.1189 22 1 0 -0.1052 -0.1862 22 1 1 -0.2257 -0.1998 22 1 2 -0.9012 -0.0931 22 1 3 4.3821 -0.4304 22 1 4 3.4466 -0.5793 22 1 5 8.8121 0.1167 22 2 0 2.7986 0.2231 22 2 1 7.9889 -0.1197 22 2 2 -2.5650 0.3119 22 2 3 -1.1515 0.5967 22 2 4 -6.4368 -0.0403 22 3 0 -11.2688 -0.4169 22 3 1 -1.8866 0.0441 22 3 2 -4.8043 -0.5806 22 3 3 -4.6042 -0.0129 22 4 0 -4.7109 -0.0221 22 4 1 -3.3047 0.7036 0 0 0 0.0 0.0 ; _shelx_fab_checksum 7760 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -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 Ir1 Ir 0.49276(2) -0.11216(2) 0.46436(2) 0.02140(11) Uani 1 1 d . . . . . Cl1 Cl 0.41519(10) 0.02217(15) 0.48337(6) 0.0224(4) Uani 1 1 d . . . . . Cl03 Cl 0.96325(17) 1.0940(2) 0.54219(10) 0.0575(8) Uani 1 1 d . . . . . Cl04 Cl 0.48789(16) 0.3414(3) 0.67064(9) 0.0623(8) Uani 1 1 d . . . . . Cl05 Cl 0.5536(2) 0.5011(2) 0.63358(11) 0.0737(10) Uani 1 1 d . . . . . Cl06 Cl 0.5825(2) 0.7618(2) 0.63694(12) 0.0733(10) Uani 1 1 d . . . . . Cl00 Cl 0.6850(2) 0.5482(4) 0.57971(15) 0.0699(9) Uani 0.75 1 d D . P A 1 Cl08 Cl 0.7494(2) 0.8185(4) 0.63820(13) 0.0901(13) Uani 1 1 d . . . . . O00A O 0.7136(3) 0.3037(5) 0.40653(18) 0.0306(15) Uani 1 1 d . . . . . O00B O 0.6078(3) 0.3074(5) 0.3122(2) 0.0326(15) Uani 1 1 d . . . . . N1 N 0.5082(4) -0.0332(5) 0.4159(2) 0.0267(17) Uani 1 1 d . . . . . N2 N 0.5237(4) 0.2139(5) 0.4945(2) 0.0271(8) Uani 1 1 d . . . . . N00E N 0.5682(4) 0.2150(5) 0.4707(2) 0.0271(8) Uani 1 1 d . . . . . O00G O 0.7029(3) 0.1089(5) 0.3352(2) 0.0335(15) Uani 1 1 d . . . . . N00H N 0.5465(4) 0.0431(6) 0.3709(2) 0.0314(19) Uani 1 1 d . . . . . O00I O 0.7787(4) 0.0833(5) 0.4293(2) 0.0378(16) Uani 1 1 d . . . . . C00J C 0.6022(5) 0.3313(7) 0.4236(3) 0.028(2) Uani 1 1 d . . . . . H00A H 0.6068 0.4061 0.4220 0.033 Uiso 1 1 calc R . . . . H00B H 0.5785 0.3058 0.3967 0.033 Uiso 1 1 calc R . . . . C00K C 0.4639(5) -0.0579(6) 0.3802(3) 0.0260(19) Uani 1 1 d . . . . . N00L N 0.5591(4) 0.0275(5) 0.4110(2) 0.0311(18) Uani 1 1 d . . . . . N00M N 0.5596(4) 0.3057(5) 0.4532(2) 0.0271(8) Uani 1 1 d . . . . . C00N C 0.4397(5) 0.3111(7) 0.5191(3) 0.0263(11) Uani 1 1 d . . . . . C00O C 0.4869(5) 0.3043(7) 0.4922(3) 0.0271(8) Uani 1 1 d . . . . . C00P C 0.3976(4) 0.2254(7) 0.5718(3) 0.0263(11) Uani 1 1 d . . . . . H00P H 0.3985 0.1694 0.5895 0.032 Uiso 1 1 calc R . . . . C2 C 0.4420(5) 0.2255(7) 0.5444(3) 0.0263(11) Uani 1 1 d . . . . . C00R C 0.4890(5) -0.0058(7) 0.3510(3) 0.032(2) Uani 1 1 d . . . . . H00R H 0.4695 -0.0049 0.3229 0.038 Uiso 1 1 calc R . . . . C00S C 0.3650(5) -0.2427(7) 0.4252(3) 0.033(2) Uani 1 1 d . . . . . H00S H 0.3670 -0.2722 0.4508 0.040 Uiso 1 1 calc R . . . . C00T C 0.7053(5) 0.4233(7) 0.3196(3) 0.027(2) Uani 1 1 d . . . . . C1 C 0.4142(4) -0.1697(7) 0.4208(3) 0.028(2) Uani 1 1 d . . . . . C00V C 0.4089(5) -0.1290(7) 0.3821(3) 0.029(2) Uani 1 1 d . . . . . C00W C 0.3530(5) 0.3062(7) 0.5728(3) 0.032(2) Uani 1 1 d . . . . . H00W H 0.3228 0.3041 0.5909 0.039 Uiso 1 1 calc R . . . . C00X C 0.6687(5) 0.3397(7) 0.3007(3) 0.031(2) Uani 1 1 d . . . . . C00Y C 0.6860(5) 0.4766(7) 0.3554(3) 0.031(2) Uani 1 1 d . . . . . H00C H 0.6738 0.5485 0.3485 0.037 Uiso 1 1 calc R . . . . H00D H 0.6445 0.4431 0.3616 0.037 Uiso 1 1 calc R . . . . C00Z C 0.7460(5) 0.4721(6) 0.3915(3) 0.027(2) Uani 1 1 d . . . . . C010 C 0.6746(5) 0.2834(8) 0.4365(3) 0.036(2) Uani 1 1 d . . . . . H01A H 0.6996 0.3120 0.4626 0.043 Uiso 1 1 calc R . . . . H01B H 0.6701 0.2090 0.4397 0.043 Uiso 1 1 calc R . . . . C011 C 0.5120(5) 0.3643(7) 0.4653(3) 0.0271(8) Uani 1 1 d . . . . . H011 H 0.4986 0.4319 0.4572 0.032 Uiso 1 1 calc R . . . . C012 C 0.8216(5) 0.3738(7) 0.4446(3) 0.031(2) Uani 1 1 d . . . . . C013 C 0.6927(5) 0.2844(7) 0.2718(3) 0.0308(12) Uani 1 1 d . . . . . C014 C 0.3559(5) -0.1592(8) 0.3495(3) 0.037(2) Uani 1 1 d . . . . . H014 H 0.3526 -0.1297 0.3237 0.044 Uiso 1 1 calc R . . . . C015 C 0.7599(5) 0.3839(7) 0.4153(3) 0.029(2) Uani 1 1 d . . . . . C016 C 0.3959(5) 0.3933(7) 0.5213(3) 0.036(2) Uani 1 1 d . . . . . H016 H 0.3963 0.4513 0.5048 0.043 Uiso 1 1 calc R . . . . C017 C 0.8445(5) 0.2708(7) 0.4638(3) 0.032(2) Uani 1 1 d . . . . . H01C H 0.8817 0.2806 0.4885 0.038 Uiso 1 1 calc R . . . . H01D H 0.8044 0.2366 0.4712 0.038 Uiso 1 1 calc R . . . . C018 C 0.6604(5) 0.1828(7) 0.2557(3) 0.0308(12) Uani 1 1 d . . . . . H01E H 0.6195 0.1679 0.2671 0.037 Uiso 1 1 calc R . . . . H01F H 0.6442 0.1862 0.2261 0.037 Uiso 1 1 calc R . . . . Cl Cl 0.7367(7) 0.4221(9) 0.5306(4) 0.0699(9) Uani 0.25 1 d D . P B 1 C01A C 0.8672(5) 0.4560(7) 0.4523(3) 0.030(2) Uani 1 1 d . . . . . H01G H 0.9086 0.4503 0.4730 0.036 Uiso 1 1 calc R . . . . C01B C 0.7510(5) 0.3192(7) 0.2597(3) 0.030(2) Uani 1 1 d . . . . . H01H H 0.7665 0.2827 0.2394 0.036 Uiso 1 1 calc R . . . . C01C C 0.8719(5) 0.2057(7) 0.4342(3) 0.031(2) Uani 1 1 d . . . . . C01D C 0.3512(5) 0.3907(8) 0.5479(3) 0.039(2) Uani 1 1 d . . . . . H01I H 0.3202 0.4456 0.5489 0.046 Uiso 1 1 calc R . . . . C01E C 0.9575(5) 0.1832(7) 0.3929(3) 0.030(2) Uani 1 1 d . . . . . C01F C 0.7355(5) 0.0667(7) 0.3072(3) 0.030(2) Uani 1 1 d . . . . . C01G C 0.7646(5) 0.4550(7) 0.3068(3) 0.028(2) Uani 1 1 d . . . . . H01J H 0.7901 0.5122 0.3195 0.034 Uiso 1 1 calc R . . . . C01H C 0.7879(5) 0.4058(8) 0.2760(3) 0.033(2) Uani 1 1 d . . . . . C01I C 0.9315(5) 0.2352(7) 0.4217(3) 0.030(2) Uani 1 1 d . . . . . H01K H 0.9557 0.2942 0.4335 0.036 Uiso 1 1 calc R . . . . C01J C 0.9199(5) 0.0994(7) 0.3751(3) 0.031(2) Uani 1 1 d . . . . . H01L H 0.9356 0.0637 0.3547 0.037 Uiso 1 1 calc R . . . . C01L C 0.3128(5) -0.2726(8) 0.3923(3) 0.042(3) Uani 1 1 d . . . . . H01M H 0.2797 -0.3222 0.3960 0.051 Uiso 1 1 calc R . . . . C01M C 0.7145(5) 0.0988(7) 0.2672(3) 0.0308(12) Uani 1 1 d . . . . . C01N C 0.9065(5) 0.6373(7) 0.4393(3) 0.038(2) Uani 1 1 d . . . . . C01O C 0.7522(6) -0.1188(9) 0.5024(4) 0.060(3) Uani 1 1 d . . . . . H01N H 0.7798 -0.1730 0.4938 0.090 Uiso 1 1 calc GR . . . . H01O H 0.7084 -0.1472 0.5067 0.090 Uiso 1 1 calc GR . . . . H01P H 0.7790 -0.0887 0.5274 0.090 Uiso 1 1 calc GR . . . . C01P C 0.7486(5) 0.0581(8) 0.2391(3) 0.038(2) Uani 1 1 d . . . . . H01Q H 0.7332 0.0772 0.2117 0.045 Uiso 1 1 calc R . . . . C01Q C 0.7912(5) 0.0000(7) 0.3194(3) 0.034(2) Uani 1 1 d . . . . . C01R C 0.3081(5) -0.2325(8) 0.3549(3) 0.042(3) Uani 1 1 d . . . . . H01R H 0.2723 -0.2546 0.3329 0.051 Uiso 1 1 calc R . . . . C01S C 0.8593(5) 0.0655(7) 0.3863(3) 0.032(2) Uani 1 1 d . . . . . C01T C 0.5951(6) 0.1056(8) 0.3548(4) 0.045(3) Uani 1 1 d . . . . . H01S H 0.6130 0.1613 0.3739 0.053 Uiso 1 1 calc R . . . . H01T H 0.5701 0.1365 0.3291 0.053 Uiso 1 1 calc R . . . . C01U C 0.8375(5) 0.1183(7) 0.4169(3) 0.030(2) Uani 1 1 d . . . . . C01V C 0.7934(5) 0.5529(7) 0.4004(3) 0.031(2) Uani 1 1 d . . . . . H01V H 0.7837 0.6138 0.3851 0.037 Uiso 1 1 calc R . . . . C01W C 0.8539(5) 0.5475(7) 0.4304(3) 0.032(2) Uani 1 1 d . . . . . C01X C 0.8193(5) -0.0239(7) 0.3634(3) 0.038(2) Uani 1 1 d . . . . . H01U H 0.8508 -0.0836 0.3659 0.046 Uiso 1 1 calc R . . . . H01W H 0.7799 -0.0421 0.3757 0.046 Uiso 1 1 calc R . . . . C01Y C 0.8044(5) -0.0098(8) 0.2500(3) 0.042(3) Uani 1 1 d . . . . . C01Z C 0.5262(6) 0.3741(8) 0.6307(3) 0.048(3) Uani 1 1 d . . . . . H01X H 0.5669 0.3293 0.6312 0.058 Uiso 1 1 calc R . . . . H01Y H 0.4919 0.3628 0.6050 0.058 Uiso 1 1 calc R . . . . C020 C 0.7361(6) -0.0380(9) 0.4703(4) 0.056(3) Uani 1 1 d . . . . . H02A H 0.7075 -0.0684 0.4454 0.067 Uiso 1 1 calc R . . . . H02B H 0.7078 0.0161 0.4791 0.067 Uiso 1 1 calc R . . . . C021 C 1.0372(6) 0.1651(10) 0.3440(3) 0.051(3) Uani 1 1 d . . . . . H02C H 1.0395 0.0911 0.3478 0.077 Uiso 1 1 calc GR . . . . H02D H 1.0811 0.1892 0.3382 0.077 Uiso 1 1 calc GR . . . . H02E H 0.9982 0.1820 0.3214 0.077 Uiso 1 1 calc GR . . . . C022 C 1.0263(5) 0.2158(8) 0.3819(3) 0.037(2) Uani 1 1 d . . . . . C023 C 0.8502(6) 0.4440(9) 0.2601(3) 0.044(3) Uani 1 1 d . . . . . C024 C 1.0880(6) 0.1868(11) 0.4178(4) 0.060(3) Uani 1 1 d . . . . . H02F H 1.0833 0.2240 0.4419 0.090 Uiso 1 1 calc GR . . . . H02G H 1.1325 0.2047 0.4112 0.090 Uiso 1 1 calc GR . . . . H02H H 1.0869 0.1134 0.4228 0.090 Uiso 1 1 calc GR . . . . C025 C 0.8248(5) -0.0377(7) 0.2901(3) 0.040(2) Uani 1 1 d . . . . . H025 H 0.8627 -0.0838 0.2981 0.048 Uiso 1 1 calc R . . . . C028 C 0.5491(6) 0.3688(11) 0.2966(4) 0.072(3) Uani 1 1 d D . . . . H02K H 0.5631 0.4409 0.3017 0.086 Uiso 0.5 1 calc R . P C 2 H02L H 0.5130 0.3542 0.3119 0.086 Uiso 0.5 1 calc R . P C 2 H02I H 0.5518 0.3880 0.2691 0.086 Uiso 0.5 1 calc R . P D 1 H02J H 0.5552 0.4323 0.3127 0.086 Uiso 0.5 1 calc R . P D 1 C02A C 0.8441(6) -0.0491(10) 0.2187(4) 0.073(3) Uani 1 1 d D . . . . C02C C 0.7987(6) 0.0082(8) 0.4613(3) 0.046(3) Uani 1 1 d . . . . . H02M H 0.8268 0.0414 0.4857 0.055 Uiso 1 1 calc R . . . . H02N H 0.8278 -0.0453 0.4528 0.055 Uiso 1 1 calc R . . . . C02D C 0.6543(6) 0.0444(8) 0.3481(5) 0.060(4) Uani 1 1 d . . . . . H02O H 0.6776 0.0096 0.3733 0.072 Uiso 1 1 calc R . . . . H02P H 0.6370 -0.0082 0.3275 0.072 Uiso 1 1 calc R . . . . C02E C 0.8906(6) 0.5286(9) 0.2861(4) 0.056(3) Uani 1 1 d . . . . . H02Q H 0.8593 0.5863 0.2869 0.084 Uiso 1 1 calc GR . . . . H02R H 0.9296 0.5507 0.2747 0.084 Uiso 1 1 calc GR . . . . H02S H 0.9089 0.5031 0.3134 0.084 Uiso 1 1 calc GR . . . . C02F C 0.6739(7) 0.8836(10) 0.6120(4) 0.066(3) Uani 1 1 d . . . . . H4AA H 0.6612 0.9365 0.6297 0.080 Uiso 1 1 calc R . . . . H H 0.6844 0.9181 0.5883 0.080 Uiso 1 1 calc R . . . . C02G C 0.6140(7) 0.8146(11) 0.5985(4) 0.066(3) Uani 1 1 d . . . . . H5AA H 0.6282 0.7590 0.5826 0.080 Uiso 1 1 calc R . . . . HA H 0.5756 0.8527 0.5806 0.080 Uiso 1 1 calc R . . . . C02I C 0.7879(6) 0.5327(9) 0.5358(4) 0.0699(9) Uani 1 1 d D . . . . HB H 0.8365 0.5187 0.5508 0.084 Uiso 0.25 1 calc R . P B 1 H2AA H 0.7888 0.5621 0.5093 0.084 Uiso 0.25 1 calc R . P B 1 HC H 0.8138 0.5736 0.5197 0.084 Uiso 0.25 1 calc R . P B 4 HD H 0.7529 0.4908 0.5171 0.084 Uiso 0.25 1 calc R . P B 4 HE H 0.8372 0.5556 0.5411 0.084 Uiso 0.25 1 calc R . P B 2 HF H 0.7674 0.5461 0.5070 0.084 Uiso 0.25 1 calc R . P B 2 HG H 0.8204 0.5727 0.5237 0.084 Uiso 0.25 1 calc R . P B 3 HH H 0.7530 0.5002 0.5138 0.084 Uiso 0.25 1 calc R . P B 3 C02K C 0.8235(7) 0.4844(12) 0.2170(4) 0.076(4) Uani 1 1 d . . . . . H02T H 0.7955 0.4317 0.2004 0.114 Uiso 1 1 calc GR . . . . H02U H 0.8635 0.5023 0.2057 0.114 Uiso 1 1 calc GR . . . . H02V H 0.7945 0.5449 0.2176 0.114 Uiso 1 1 calc GR . . . . C12 C 0.9202(8) 0.6651(11) 0.4843(5) 0.049(2) Uani 0.75 1 d . . P E 1 H12A H 0.8757 0.6805 0.4914 0.074 Uiso 0.75 1 calc GR . P E 1 H12B H 0.9508 0.7249 0.4897 0.074 Uiso 0.75 1 calc GR . P E 1 H12C H 0.9429 0.6077 0.5005 0.074 Uiso 0.75 1 calc GR . P E 1 C02M C 0.7508(7) 0.6030(9) 0.5594(4) 0.0699(9) Uani 1 1 d D . . . . H3AA H 0.7298 0.6596 0.5415 0.084 Uiso 0.75 1 calc R . P A 1 HI H 0.7865 0.6329 0.5817 0.084 Uiso 0.75 1 calc R . P A 1 HJ H 0.7253 0.6412 0.5356 0.084 Uiso 0.25 1 calc R . P A 2 HK H 0.7924 0.6460 0.5699 0.084 Uiso 0.25 1 calc R . P A 2 C02N C 0.9915(7) 0.9862(9) 0.5187(4) 0.0575(8) Uani 1 1 d . . . . . H6AA H 1.0332 0.9562 0.5370 0.069 Uiso 1 1 calc R . . . . HL H 0.9540 0.9342 0.5137 0.069 Uiso 1 1 calc R . . . . C02O C 1.0274(7) 0.3320(9) 0.3760(4) 0.057(3) Uani 1 1 d . . . . . H02W H 0.9876 0.3522 0.3544 0.086 Uiso 1 1 calc GR . . . . H02X H 1.0711 0.3516 0.3687 0.086 Uiso 1 1 calc GR . . . . H02Y H 1.0244 0.3662 0.4010 0.086 Uiso 1 1 calc GR . . . . C1AA C 0.9768(8) 0.6017(11) 0.4310(5) 0.049(2) Uani 0.75 1 d . . P E 1 H1AA H 0.9938 0.5421 0.4477 0.074 Uiso 0.75 1 calc GR . P E 1 H1AB H 1.0113 0.6567 0.4376 0.074 Uiso 0.75 1 calc GR . P E 1 H1AC H 0.9701 0.5836 0.4026 0.074 Uiso 0.75 1 calc GR . P E 1 C0 C 0.8830(8) 0.7298(11) 0.4142(5) 0.049(2) Uani 0.75 1 d . . P E 1 H0A H 0.8769 0.7125 0.3857 0.074 Uiso 0.75 1 calc GR . P E 1 H0B H 0.9184 0.7834 0.4213 0.074 Uiso 0.75 1 calc GR . P E 1 H0C H 0.8385 0.7540 0.4191 0.074 Uiso 0.75 1 calc GR . P E 1 C02U C 0.9010(6) 0.3553(10) 0.2593(5) 0.070(4) Uani 1 1 d . . . . . H02Z H 0.9136 0.3235 0.2859 0.106 Uiso 1 1 calc GR . . . . HM H 0.9433 0.3812 0.2522 0.106 Uiso 1 1 calc GR . . . . HN H 0.8785 0.3049 0.2394 0.106 Uiso 1 1 calc GR . . . . C0AA C 0.7921(12) -0.086(2) 0.1804(6) 0.073(3) Uani 0.5 1 d D . P F 2 H0AA H 0.8179 -0.1057 0.1602 0.110 Uiso 0.5 1 calc GR . P F 2 H0AB H 0.7593 -0.0312 0.1698 0.110 Uiso 0.5 1 calc GR . P F 2 H0AC H 0.7662 -0.1450 0.1870 0.110 Uiso 0.5 1 calc GR . P F 2 C02Z C 0.5164(11) 0.357(2) 0.2528(5) 0.072(3) Uani 0.5 1 d D . P G 2 H02 H 0.4971 0.2874 0.2470 0.086 Uiso 0.5 1 calc R . P G 2 HO H 0.5512 0.3693 0.2365 0.086 Uiso 0.5 1 calc R . P G 2 C032 C 0.4586(12) 0.435(2) 0.2436(10) 0.072(3) Uani 0.5 1 d D . P G 2 H03A H 0.4721 0.4903 0.2275 0.108 Uiso 0.5 1 calc GR . P G 2 H03B H 0.4509 0.4632 0.2688 0.108 Uiso 0.5 1 calc GR . P G 2 H03C H 0.4155 0.4033 0.2285 0.108 Uiso 0.5 1 calc GR . P G 2 Cl8 Cl 0.7020(7) 0.6522(11) 0.5917(4) 0.0699(9) Uani 0.25 1 d D . P A 2 C20 C 0.4204(12) 0.400(2) 0.2685(9) 0.072(3) Uani 0.5 1 d D . P G 1 H20A H 0.3794 0.3584 0.2565 0.108 Uiso 0.5 1 calc GR . P G 1 H20B H 0.4392 0.4308 0.2472 0.108 Uiso 0.5 1 calc GR . P G 1 H20C H 0.4068 0.4532 0.2852 0.108 Uiso 0.5 1 calc GR . P G 1 C21 C 0.4756(7) 0.333(2) 0.2942(9) 0.072(3) Uani 0.5 1 d D . P G 1 H21A H 0.4675 0.3302 0.3217 0.086 Uiso 0.5 1 calc R . P G 1 H21B H 0.4706 0.2630 0.2832 0.086 Uiso 0.5 1 calc R . P G 1 C18B C 0.8558(16) -0.1650(13) 0.2245(9) 0.073(3) Uani 0.5 1 d D . P F 1 H18A H 0.8107 -0.2002 0.2170 0.110 Uiso 0.5 1 calc GR . P F 1 H18B H 0.8777 -0.1792 0.2528 0.110 Uiso 0.5 1 calc GR . P F 1 H18C H 0.8864 -0.1889 0.2075 0.110 Uiso 0.5 1 calc GR . P F 1 C3 C 0.9172(10) 0.001(2) 0.2304(9) 0.073(3) Uani 0.5 1 d D . P F 1 H3A H 0.9457 -0.0228 0.2122 0.110 Uiso 0.5 1 calc GR . P F 1 H3B H 0.9399 -0.0181 0.2581 0.110 Uiso 0.5 1 calc GR . P F 1 H3C H 0.9123 0.0750 0.2285 0.110 Uiso 0.5 1 calc GR . P F 1 Cl6 Cl 0.8458(9) 0.4536(13) 0.5684(7) 0.0699(9) Uani 0.25 1 d D . P B 4 Cl7 Cl 0.7901(8) 0.4020(7) 0.5416(5) 0.0699(9) Uani 0.25 1 d D . P B 2 Cl10 Cl 0.8346(9) 0.4386(14) 0.5670(7) 0.0699(9) Uani 0.25 1 d D . P B 3 C13 C 0.858(2) 0.736(3) 0.4459(15) 0.049(2) Uani 0.25 1 d . . P E 2 H13A H 0.8165 0.7395 0.4237 0.074 Uiso 0.25 1 calc GR . P E 2 H13B H 0.8855 0.7988 0.4464 0.074 Uiso 0.25 1 calc GR . P E 2 H13C H 0.8439 0.7290 0.4714 0.074 Uiso 0.25 1 calc GR . P E 2 C9 C 0.963(2) 0.626(3) 0.4746(15) 0.049(2) Uani 0.25 1 d . . P E 2 H9A H 0.9440 0.6128 0.4981 0.074 Uiso 0.25 1 calc GR . P E 2 H9B H 0.9915 0.6878 0.4787 0.074 Uiso 0.25 1 calc GR . P E 2 H9C H 0.9927 0.5679 0.4706 0.074 Uiso 0.25 1 calc GR . P E 2 C7 C 0.929(2) 0.661(3) 0.3990(14) 0.049(2) Uani 0.25 1 d . . P E 2 H7A H 0.9565 0.6031 0.3923 0.074 Uiso 0.25 1 calc GR . P E 2 H7B H 0.9584 0.7222 0.4023 0.074 Uiso 0.25 1 calc GR . P E 2 H7C H 0.8878 0.6710 0.3773 0.074 Uiso 0.25 1 calc GR . P E 2 C4 C 0.8078(14) -0.018(2) 0.1755(5) 0.073(3) Uani 0.5 1 d D . P F 1 H4A H 0.8314 -0.0513 0.1565 0.110 Uiso 0.5 1 calc GR . P F 1 H4B H 0.8102 0.0558 0.1727 0.110 Uiso 0.5 1 calc GR . P F 1 H4C H 0.7587 -0.0397 0.1698 0.110 Uiso 0.5 1 calc GR . P F 1 C5 C 0.8800(14) 0.0431(16) 0.2038(9) 0.073(3) Uani 0.5 1 d D . P F 2 H5A H 0.9183 0.0191 0.1922 0.110 Uiso 0.5 1 calc GR . P F 2 H5B H 0.8988 0.0885 0.2265 0.110 Uiso 0.5 1 calc GR . P F 2 H5C H 0.8458 0.0800 0.1834 0.110 Uiso 0.5 1 calc GR . P F 2 C18A C 0.8981(14) -0.133(2) 0.2346(8) 0.073(3) Uani 0.5 1 d D . P F 2 H18D H 0.8752 -0.1891 0.2455 0.110 Uiso 0.5 1 calc GR . P F 2 H18E H 0.9358 -0.1051 0.2558 0.110 Uiso 0.5 1 calc GR . P F 2 H18F H 0.9177 -0.1584 0.2125 0.110 Uiso 0.5 1 calc GR . P F 2 Cl0A Cl 0.4040(3) 0.1252(4) 0.25370(14) 0.0788(15) Uani 0.75 1 d . . P . . Cl2 Cl 0.2983(3) 0.2574(3) 0.17858(17) 0.0870(17) Uani 0.75 1 d . . P . . C6 C 0.2915(13) 0.2485(19) 0.2255(7) 0.101(7) Uiso 0.75 1 d . . P . . H6A H 0.3087 0.3143 0.2381 0.121 Uiso 0.75 1 calc R . P . . H6B H 0.2406 0.2472 0.2242 0.121 Uiso 0.75 1 calc R . P . . C8 C 0.3226(13) 0.169(2) 0.2558(8) 0.102(7) Uiso 0.75 1 d . . P . . H8A H 0.2903 0.1100 0.2523 0.122 Uiso 0.75 1 calc R . P . . H8B H 0.3254 0.1969 0.2829 0.122 Uiso 0.75 1 calc R . P . . 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 Ir1 0.02208(18) 0.02202(18) 0.02182(18) -0.00161(15) 0.00857(12) -0.00054(15) Cl1 0.0259(11) 0.0200(10) 0.0228(11) -0.0044(8) 0.0089(8) 0.0021(8) Cl03 0.072(2) 0.0434(16) 0.0597(18) -0.0054(13) 0.0194(15) -0.0022(14) Cl04 0.0551(18) 0.085(2) 0.0462(17) 0.0002(16) 0.0096(14) -0.0029(17) Cl05 0.102(3) 0.0424(17) 0.075(2) -0.0002(16) 0.017(2) -0.0137(17) Cl06 0.079(2) 0.0431(18) 0.096(3) -0.0017(17) 0.015(2) -0.0060(16) Cl00 0.069(2) 0.068(2) 0.074(2) 0.0081(18) 0.0175(18) 0.0003(17) Cl08 0.060(2) 0.120(3) 0.083(3) -0.009(2) 0.0023(19) 0.028(2) O00A 0.042(4) 0.029(3) 0.027(3) -0.007(3) 0.021(3) -0.012(3) O00B 0.026(3) 0.024(3) 0.053(4) 0.000(3) 0.020(3) 0.002(3) N1 0.024(4) 0.020(4) 0.040(5) -0.007(3) 0.015(3) -0.001(3) N2 0.0289(19) 0.0236(17) 0.030(2) -0.0015(15) 0.0089(15) -0.0031(14) N00E 0.0289(19) 0.0236(17) 0.030(2) -0.0015(15) 0.0089(15) -0.0031(14) O00G 0.033(3) 0.029(3) 0.045(4) -0.006(3) 0.022(3) -0.009(3) N00H 0.045(5) 0.032(4) 0.027(4) 0.005(3) 0.028(4) 0.009(4) O00I 0.043(4) 0.022(3) 0.054(4) 0.003(3) 0.023(3) -0.005(3) C00J 0.037(5) 0.025(5) 0.028(5) 0.002(4) 0.020(4) -0.006(4) C00K 0.035(5) 0.021(4) 0.022(5) -0.001(4) 0.005(4) 0.009(4) N00L 0.032(4) 0.023(4) 0.045(5) -0.004(4) 0.023(4) 0.003(3) N00M 0.0289(19) 0.0236(17) 0.030(2) -0.0015(15) 0.0089(15) -0.0031(14) C00N 0.027(3) 0.026(3) 0.027(3) -0.006(2) 0.008(2) -0.005(2) C00O 0.0289(19) 0.0236(17) 0.030(2) -0.0015(15) 0.0089(15) -0.0031(14) C00P 0.027(3) 0.026(3) 0.027(3) -0.006(2) 0.008(2) -0.005(2) C2 0.027(3) 0.026(3) 0.027(3) -0.006(2) 0.008(2) -0.005(2) C00R 0.046(6) 0.031(5) 0.020(5) 0.005(4) 0.011(4) 0.005(4) C00S 0.029(5) 0.036(5) 0.032(5) -0.002(4) 0.005(4) -0.008(4) C00T 0.031(5) 0.023(4) 0.029(5) 0.004(4) 0.009(4) 0.000(4) C1 0.019(4) 0.036(5) 0.025(5) -0.011(4) 0.001(4) -0.001(4) C00V 0.034(5) 0.032(5) 0.020(5) -0.004(4) 0.006(4) 0.004(4) C00W 0.033(5) 0.032(5) 0.036(5) -0.014(4) 0.015(4) -0.003(4) C00X 0.026(5) 0.032(5) 0.037(5) 0.010(4) 0.011(4) 0.004(4) C00Y 0.032(5) 0.025(5) 0.040(6) -0.006(4) 0.019(4) -0.001(4) C00Z 0.027(5) 0.022(5) 0.036(5) -0.009(4) 0.017(4) 0.000(4) C010 0.033(5) 0.044(6) 0.034(6) 0.002(5) 0.015(4) -0.009(4) C011 0.0289(19) 0.0236(17) 0.030(2) -0.0015(15) 0.0089(15) -0.0031(14) C012 0.036(5) 0.027(5) 0.035(5) 0.001(4) 0.020(4) 0.004(4) C013 0.029(3) 0.030(3) 0.037(3) -0.006(2) 0.013(2) -0.005(2) C014 0.041(6) 0.039(6) 0.029(5) 0.002(4) 0.005(4) 0.005(5) C015 0.035(5) 0.023(4) 0.037(5) -0.004(4) 0.024(4) -0.003(4) C016 0.043(6) 0.026(5) 0.043(6) 0.000(5) 0.017(5) 0.005(4) C017 0.046(6) 0.021(5) 0.033(5) 0.004(4) 0.015(4) 0.000(4) C018 0.029(3) 0.030(3) 0.037(3) -0.006(2) 0.013(2) -0.005(2) Cl 0.069(2) 0.068(2) 0.074(2) 0.0081(18) 0.0175(18) 0.0003(17) C01A 0.037(5) 0.022(5) 0.034(5) -0.004(4) 0.014(4) 0.003(4) C01B 0.033(5) 0.032(5) 0.024(5) -0.005(4) 0.004(4) -0.004(4) C01C 0.046(6) 0.022(5) 0.025(5) 0.006(4) 0.007(4) 0.005(4) C01D 0.040(6) 0.031(5) 0.049(6) -0.006(5) 0.019(5) 0.013(5) C01E 0.033(5) 0.028(5) 0.029(5) 0.006(4) 0.006(4) 0.011(4) C01F 0.030(5) 0.019(4) 0.048(6) -0.007(4) 0.022(4) -0.007(4) C01G 0.027(5) 0.029(5) 0.029(5) -0.002(4) 0.007(4) 0.000(4) C01H 0.028(5) 0.043(6) 0.029(5) 0.009(4) 0.008(4) 0.000(4) C01I 0.031(5) 0.027(5) 0.033(5) 0.012(4) 0.006(4) 0.001(4) C01J 0.041(5) 0.027(5) 0.026(5) -0.001(4) 0.011(4) 0.010(4) C01L 0.040(6) 0.046(6) 0.040(6) -0.012(5) 0.007(5) -0.012(5) C01M 0.029(3) 0.030(3) 0.037(3) -0.006(2) 0.013(2) -0.005(2) C01N 0.039(6) 0.028(5) 0.047(6) -0.006(4) 0.010(5) -0.003(4) C01O 0.040(6) 0.059(8) 0.076(9) 0.026(7) 0.002(6) -0.003(6) C01P 0.032(5) 0.044(6) 0.037(6) -0.011(5) 0.006(4) 0.000(5) C01Q 0.035(5) 0.025(5) 0.045(6) -0.008(4) 0.016(5) 0.001(4) C01R 0.034(6) 0.052(7) 0.035(6) -0.008(5) -0.001(5) -0.010(5) C01S 0.042(6) 0.022(5) 0.031(5) 0.008(4) 0.007(4) 0.008(4) C01T 0.054(7) 0.036(6) 0.059(7) 0.014(5) 0.043(6) 0.000(5) C01U 0.029(5) 0.027(5) 0.035(5) 0.002(4) 0.009(4) 0.001(4) C01V 0.036(5) 0.020(5) 0.041(6) 0.006(4) 0.018(4) 0.009(4) C01W 0.036(5) 0.023(5) 0.041(6) -0.008(4) 0.017(5) -0.002(4) C01X 0.047(6) 0.023(5) 0.047(6) -0.006(4) 0.016(5) 0.003(4) C01Y 0.031(5) 0.050(6) 0.049(7) -0.023(5) 0.016(5) -0.005(5) C01Z 0.051(7) 0.047(7) 0.049(7) -0.006(5) 0.016(5) -0.003(5) C020 0.040(6) 0.056(7) 0.063(8) 0.024(6) -0.005(6) -0.006(6) C021 0.047(7) 0.063(8) 0.051(7) 0.000(6) 0.026(6) -0.004(6) C022 0.042(6) 0.040(6) 0.032(6) 0.002(5) 0.013(5) 0.001(5) C023 0.042(6) 0.053(7) 0.044(6) -0.007(5) 0.023(5) -0.015(5) C024 0.040(7) 0.084(9) 0.055(8) -0.003(7) 0.011(6) 0.001(6) C025 0.035(6) 0.030(5) 0.054(7) -0.014(5) 0.009(5) 0.003(4) C028 0.034(5) 0.087(7) 0.096(8) 0.022(6) 0.016(5) 0.010(5) C02A 0.064(6) 0.098(7) 0.068(6) -0.022(6) 0.037(5) 0.017(5) C02C 0.055(7) 0.037(6) 0.048(7) 0.016(5) 0.014(5) -0.002(5) C02D 0.051(7) 0.027(6) 0.116(11) -0.006(6) 0.046(7) -0.004(5) C02E 0.044(7) 0.061(8) 0.068(8) -0.013(7) 0.026(6) -0.017(6) C02F 0.072(6) 0.064(6) 0.055(6) 0.008(5) -0.002(5) 0.003(5) C02G 0.072(6) 0.064(6) 0.055(6) 0.008(5) -0.002(5) 0.003(5) C02I 0.069(2) 0.068(2) 0.074(2) 0.0081(18) 0.0175(18) 0.0003(17) C02K 0.072(9) 0.108(12) 0.057(9) 0.015(8) 0.031(7) -0.034(9) C12 0.051(5) 0.034(4) 0.059(6) -0.006(4) 0.006(4) -0.011(4) C02M 0.069(2) 0.068(2) 0.074(2) 0.0081(18) 0.0175(18) 0.0003(17) C02N 0.072(2) 0.0434(16) 0.0597(18) -0.0054(13) 0.0194(15) -0.0022(14) C02O 0.069(8) 0.052(7) 0.059(8) -0.003(6) 0.032(7) -0.012(6) C1AA 0.051(5) 0.034(4) 0.059(6) -0.006(4) 0.006(4) -0.011(4) C0 0.051(5) 0.034(4) 0.059(6) -0.006(4) 0.006(4) -0.011(4) C02U 0.051(8) 0.070(9) 0.104(11) -0.039(8) 0.048(8) -0.014(6) C0AA 0.064(6) 0.098(7) 0.068(6) -0.022(6) 0.037(5) 0.017(5) C02Z 0.034(5) 0.087(7) 0.096(8) 0.022(6) 0.016(5) 0.010(5) C032 0.034(5) 0.087(7) 0.096(8) 0.022(6) 0.016(5) 0.010(5) Cl8 0.069(2) 0.068(2) 0.074(2) 0.0081(18) 0.0175(18) 0.0003(17) C20 0.034(5) 0.087(7) 0.096(8) 0.022(6) 0.016(5) 0.010(5) C21 0.034(5) 0.087(7) 0.096(8) 0.022(6) 0.016(5) 0.010(5) C18B 0.064(6) 0.098(7) 0.068(6) -0.022(6) 0.037(5) 0.017(5) C3 0.064(6) 0.098(7) 0.068(6) -0.022(6) 0.037(5) 0.017(5) Cl6 0.069(2) 0.068(2) 0.074(2) 0.0081(18) 0.0175(18) 0.0003(17) Cl7 0.069(2) 0.068(2) 0.074(2) 0.0081(18) 0.0175(18) 0.0003(17) Cl10 0.069(2) 0.068(2) 0.074(2) 0.0081(18) 0.0175(18) 0.0003(17) C13 0.051(5) 0.034(4) 0.059(6) -0.006(4) 0.006(4) -0.011(4) C9 0.051(5) 0.034(4) 0.059(6) -0.006(4) 0.006(4) -0.011(4) C7 0.051(5) 0.034(4) 0.059(6) -0.006(4) 0.006(4) -0.011(4) C4 0.064(6) 0.098(7) 0.068(6) -0.022(6) 0.037(5) 0.017(5) C5 0.064(6) 0.098(7) 0.068(6) -0.022(6) 0.037(5) 0.017(5) C18A 0.064(6) 0.098(7) 0.068(6) -0.022(6) 0.037(5) 0.017(5) Cl0A 0.103(4) 0.086(3) 0.051(3) 0.015(2) 0.024(2) 0.041(3) Cl2 0.134(5) 0.031(2) 0.089(4) -0.016(2) 0.012(3) 0.018(3) 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' Cl Cl 0.1484 0.1585 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Cl1 Ir1 Cl1 82.28(7) . 3_656 ? N1 Ir1 Cl1 93.7(2) . . ? N1 Ir1 Cl1 97.0(2) . 3_656 ? N2 Ir1 Cl1 91.1(2) 3_656 3_656 ? N2 Ir1 Cl1 94.6(2) 3_656 . ? N2 Ir1 N1 169.1(3) 3_656 . ? N2 Ir1 C2 79.9(3) 3_656 3_656 ? N2 Ir1 C1 92.8(3) 3_656 . ? C2 Ir1 Cl1 94.3(2) 3_656 3_656 ? C2 Ir1 Cl1 173.6(3) 3_656 . ? C2 Ir1 N1 92.1(3) 3_656 . ? C1 Ir1 Cl1 173.9(3) . 3_656 ? C1 Ir1 Cl1 92.8(3) . . ? C1 Ir1 N1 79.8(3) . . ? C1 Ir1 C2 91.0(3) . 3_656 ? Ir1 Cl1 Ir1 97.72(7) . 3_656 ? C015 O00A C010 114.8(7) . . ? C028 O00B C00X 113.3(8) . . ? C00K N1 Ir1 115.1(6) . . ? N00L N1 Ir1 132.1(6) . . ? N00L N1 C00K 112.0(8) . . ? N00E N2 Ir1 132.0(6) . 3_656 ? N00E N2 C00O 111.5(7) . . ? C00O N2 Ir1 116.2(6) . 3_656 ? N2 N00E N00M 104.7(7) . . ? C01F O00G C02D 115.3(7) . . ? N00L N00H C01T 118.9(8) . . ? C00R N00H N00L 112.2(7) . . ? C00R N00H C01T 128.9(8) . . ? C01U O00I C02C 110.5(7) . . ? H00A C00J H00B 108.2 . . ? N00M C00J H00A 109.6 . . ? N00M C00J H00B 109.6 . . ? N00M C00J C010 110.1(7) . . ? C010 C00J H00A 109.6 . . ? C010 C00J H00B 109.6 . . ? N1 C00K C00R 105.5(8) . . ? N1 C00K C00V 116.2(8) . . ? C00R C00K C00V 138.3(9) . . ? N1 N00L N00H 104.7(7) . . ? N00E N00M C00J 118.5(7) . . ? N00E N00M C011 113.5(7) . . ? C011 N00M C00J 128.1(7) . . ? C2 C00N C00O 113.9(8) . . ? C016 C00N C00O 125.0(8) . . ? C016 C00N C2 121.1(8) . . ? N2 C00O C00N 114.7(8) . . ? N2 C00O C011 105.4(8) . . ? C011 C00O C00N 139.8(9) . . ? C2 C00P H00P 119.8 . . ? C00W C00P H00P 119.8 . . ? C00W C00P C2 120.4(9) . . ? C00N C2 Ir1 115.2(6) . 3_656 ? C00N C2 C00P 117.8(8) . . ? C00P C2 Ir1 126.9(7) . 3_656 ? N00H C00R C00K 105.6(8) . . ? N00H C00R H00R 127.2 . . ? C00K C00R H00R 127.2 . . ? C1 C00S H00S 119.8 . . ? C01L C00S H00S 119.8 . . ? C01L C00S C1 120.3(9) . . ? C00X C00T C00Y 122.4(8) . . ? C00X C00T C01G 118.1(8) . . ? C01G C00T C00Y 119.4(8) . . ? C00S C1 Ir1 127.3(7) . . ? C00S C1 C00V 117.4(8) . . ? C00V C1 Ir1 115.3(6) . . ? C1 C00V C00K 113.3(8) . . ? C014 C00V C00K 125.0(8) . . ? C014 C00V C1 121.6(9) . . ? C00P C00W H00W 119.2 . . ? C00P C00W C01D 121.5(9) . . ? C01D C00W H00W 119.2 . . ? C00T C00X O00B 119.3(8) . . ? C00T C00X C013 121.3(8) . . ? C013 C00X O00B 119.3(8) . . ? C00T C00Y H00C 109.6 . . ? C00T C00Y H00D 109.6 . . ? H00C C00Y H00D 108.1 . . ? C00Z C00Y C00T 110.3(7) . . ? C00Z C00Y H00C 109.6 . . ? C00Z C00Y H00D 109.6 . . ? C015 C00Z C00Y 121.3(8) . . ? C01V C00Z C00Y 120.4(8) . . ? C01V C00Z C015 118.1(9) . . ? O00A C010 C00J 109.5(8) . . ? O00A C010 H01A 109.8 . . ? O00A C010 H01B 109.8 . . ? C00J C010 H01A 109.8 . . ? C00J C010 H01B 109.8 . . ? H01A C010 H01B 108.2 . . ? N00M C011 C00O 104.9(8) . . ? N00M C011 H011 127.6 . . ? C00O C011 H011 127.6 . . ? C015 C012 C017 121.1(8) . . ? C01A C012 C015 118.7(9) . . ? C01A C012 C017 119.6(9) . . ? C00X C013 C018 122.2(8) . . ? C01B C013 C00X 118.6(8) . . ? C01B C013 C018 119.0(8) . . ? C00V C014 H014 120.3 . . ? C01R C014 C00V 119.4(9) . . ? C01R C014 H014 120.3 . . ? O00A C015 C00Z 118.4(8) . . ? O00A C015 C012 120.4(8) . . ? C012 C015 C00Z 121.0(8) . . ? C00N C016 H016 119.9 . . ? C00N C016 C01D 120.2(9) . . ? C01D C016 H016 119.9 . . ? C012 C017 H01C 109.8 . . ? C012 C017 H01D 109.8 . . ? H01C C017 H01D 108.3 . . ? C01C C017 C012 109.2(7) . . ? C01C C017 H01C 109.8 . . ? C01C C017 H01D 109.8 . . ? C013 C018 H01E 109.8 . . ? C013 C018 H01F 109.8 . . ? H01E C018 H01F 108.2 . . ? C01M C018 C013 109.6(7) . . ? C01M C018 H01E 109.8 . . ? C01M C018 H01F 109.8 . . ? C012 C01A H01G 119.0 . . ? C012 C01A C01W 122.0(9) . . ? C01W C01A H01G 119.0 . . ? C013 C01B H01H 118.7 . . ? C013 C01B C01H 122.7(9) . . ? C01H C01B H01H 118.7 . . ? C01I C01C C017 120.0(9) . . ? C01I C01C C01U 117.4(9) . . ? C01U C01C C017 122.4(9) . . ? C00W C01D C016 119.0(9) . . ? C00W C01D H01I 120.5 . . ? C016 C01D H01I 120.5 . . ? C01I C01E C022 121.5(9) . . ? C01J C01E C01I 117.1(9) . . ? C01J C01E C022 121.4(8) . . ? O00G C01F C01M 118.4(8) . . ? O00G C01F C01Q 120.1(9) . . ? C01Q C01F C01M 121.3(8) . . ? C00T C01G H01J 118.8 . . ? C00T C01G C01H 122.5(9) . . ? C01H C01G H01J 118.8 . . ? C01B C01H C01G 116.7(8) . . ? C01B C01H C023 120.6(9) . . ? C01G C01H C023 122.7(9) . . ? C01C C01I C01E 123.6(9) . . ? C01C C01I H01K 118.2 . . ? C01E C01I H01K 118.2 . . ? C01E C01J H01L 119.0 . . ? C01E C01J C01S 122.1(8) . . ? C01S C01J H01L 119.0 . . ? C00S C01L H01M 119.1 . . ? C01R C01L C00S 121.8(10) . . ? C01R C01L H01M 119.1 . . ? C01F C01M C018 120.2(8) . . ? C01P C01M C018 121.2(9) . . ? C01P C01M C01F 118.4(9) . . ? C01W C01N C13 104.3(17) . . ? C01W C01N C7 106.7(17) . . ? C12 C01N C01W 109.4(9) . . ? C12 C01N C1AA 107.2(11) . . ? C1AA C01N C01W 108.4(8) . . ? C0 C01N C01W 113.7(9) . . ? C0 C01N C12 109.9(10) . . ? C0 C01N C1AA 108.0(11) . . ? C9 C01N C01W 115.6(19) . . ? C9 C01N C13 109(3) . . ? C9 C01N C7 115(3) . . ? C7 C01N C13 105(3) . . ? H01N C01O H01O 109.5 . . ? H01N C01O H01P 109.5 . . ? H01O C01O H01P 109.5 . . ? C020 C01O H01N 109.5 . . ? C020 C01O H01O 109.5 . . ? C020 C01O H01P 109.5 . . ? C01M C01P H01Q 118.9 . . ? C01Y C01P C01M 122.2(10) . . ? C01Y C01P H01Q 118.9 . . ? C01F C01Q C01X 120.9(8) . . ? C01F C01Q C025 118.2(10) . . ? C025 C01Q C01X 120.7(9) . . ? C014 C01R H01R 120.3 . . ? C01L C01R C014 119.4(9) . . ? C01L C01R H01R 120.3 . . ? C01J C01S C01X 118.2(8) . . ? C01U C01S C01J 118.1(9) . . ? C01U C01S C01X 123.7(9) . . ? N00H C01T H01S 109.4 . . ? N00H C01T H01T 109.4 . . ? N00H C01T C02D 111.1(8) . . ? H01S C01T H01T 108.0 . . ? C02D C01T H01S 109.4 . . ? C02D C01T H01T 109.4 . . ? O00I C01U C01S 118.7(8) . . ? C01C C01U O00I 119.8(8) . . ? C01C C01U C01S 121.5(9) . . ? C00Z C01V H01V 118.8 . . ? C01W C01V C00Z 122.4(9) . . ? C01W C01V H01V 118.8 . . ? C01A C01W C01N 120.7(9) . . ? C01V C01W C01A 117.5(8) . . ? C01V C01W C01N 121.7(9) . . ? C01Q C01X C01S 112.1(8) . . ? C01Q C01X H01U 109.2 . . ? C01Q C01X H01W 109.2 . . ? C01S C01X H01U 109.2 . . ? C01S C01X H01W 109.2 . . ? H01U C01X H01W 107.9 . . ? C01P C01Y C02A 121.2(10) . . ? C025 C01Y C01P 117.6(9) . . ? C025 C01Y C02A 121.2(10) . . ? Cl04 C01Z H01X 109.3 . . ? Cl04 C01Z H01Y 109.3 . . ? Cl05 C01Z Cl04 111.8(6) . . ? Cl05 C01Z H01X 109.3 . . ? Cl05 C01Z H01Y 109.3 . . ? H01X C01Z H01Y 107.9 . . ? C01O C020 H02A 108.9 . . ? C01O C020 H02B 108.9 . . ? H02A C020 H02B 107.7 . . ? C02C C020 C01O 113.5(9) . . ? C02C C020 H02A 108.9 . . ? C02C C020 H02B 108.9 . . ? H02C C021 H02D 109.5 . . ? H02C C021 H02E 109.5 . . ? H02D C021 H02E 109.5 . . ? C022 C021 H02C 109.5 . . ? C022 C021 H02D 109.5 . . ? C022 C021 H02E 109.5 . . ? C01E C022 C024 107.7(8) . . ? C021 C022 C01E 113.0(9) . . ? C021 C022 C024 109.2(9) . . ? C021 C022 C02O 108.3(9) . . ? C02O C022 C01E 110.3(8) . . ? C02O C022 C024 108.2(10) . . ? C01H C023 C02K 109.1(9) . . ? C01H C023 C02U 109.4(9) . . ? C02E C023 C01H 112.6(9) . . ? C02E C023 C02K 108.8(10) . . ? C02E C023 C02U 108.0(10) . . ? C02U C023 C02K 108.9(11) . . ? C022 C024 H02F 109.5 . . ? C022 C024 H02G 109.5 . . ? C022 C024 H02H 109.5 . . ? H02F C024 H02G 109.5 . . ? H02F C024 H02H 109.5 . . ? H02G C024 H02H 109.5 . . ? C01Q C025 H025 118.9 . . ? C01Y C025 C01Q 122.3(10) . . ? C01Y C025 H025 118.9 . . ? O00B C028 H02K 108.2 . . ? O00B C028 H02L 108.2 . . ? O00B C028 H02I 106.8 . . ? O00B C028 H02J 106.8 . . ? O00B C028 C02Z 116.4(13) . . ? O00B C028 C21 122.2(13) . . ? H02K C028 H02L 107.3 . . ? H02I C028 H02J 106.6 . . ? C02Z C028 H02K 108.2 . . ? C02Z C028 H02L 108.2 . . ? C21 C028 H02I 106.8 . . ? C21 C028 H02J 106.8 . . ? C0AA C02A C01Y 110.6(12) . . ? C0AA C02A C5 103.4(18) . . ? C18B C02A C01Y 108.8(13) . . ? C3 C02A C01Y 105.3(12) . . ? C3 C02A C18B 106.4(18) . . ? C4 C02A C01Y 112.3(12) . . ? C4 C02A C18B 113.9(18) . . ? C4 C02A C3 109.6(19) . . ? C5 C02A C01Y 107.9(12) . . ? C18A C02A C01Y 114.3(13) . . ? C18A C02A C0AA 109.9(18) . . ? C18A C02A C5 110.3(17) . . ? O00I C02C C020 110.1(9) . . ? O00I C02C H02M 109.6 . . ? O00I C02C H02N 109.6 . . ? C020 C02C H02M 109.6 . . ? C020 C02C H02N 109.6 . . ? H02M C02C H02N 108.2 . . ? O00G C02D C01T 109.5(8) . . ? O00G C02D H02O 109.8 . . ? O00G C02D H02P 109.8 . . ? C01T C02D H02O 109.8 . . ? C01T C02D H02P 109.8 . . ? H02O C02D H02P 108.2 . . ? C023 C02E H02Q 109.5 . . ? C023 C02E H02R 109.5 . . ? C023 C02E H02S 109.5 . . ? H02Q C02E H02R 109.5 . . ? H02Q C02E H02S 109.5 . . ? H02R C02E H02S 109.5 . . ? Cl08 C02F H4AA 109.2 . . ? Cl08 C02F H 109.2 . . ? H4AA C02F H 107.9 . . ? C02G C02F Cl08 112.1(10) . . ? C02G C02F H4AA 109.2 . . ? C02G C02F H 109.2 . . ? Cl06 C02G H5AA 108.7 . . ? Cl06 C02G HA 108.7 . . ? C02F C02G Cl06 114.3(10) . . ? C02F C02G H5AA 108.7 . . ? C02F C02G HA 108.7 . . ? H5AA C02G HA 107.6 . . ? Cl C02I HB 111.2 . . ? Cl C02I H2AA 111.2 . . ? HB C02I H2AA 109.1 . . ? HC C02I HD 108.1 . . ? HE C02I HF 106.5 . . ? HG C02I HH 108.1 . . ? C02M C02I Cl 103.0(9) . . ? C02M C02I HB 111.2 . . ? C02M C02I H2AA 111.2 . . ? C02M C02I HC 109.6 . . ? C02M C02I HD 109.6 . . ? C02M C02I HE 106.6 . . ? C02M C02I HF 106.6 . . ? C02M C02I HG 109.5 . . ? C02M C02I HH 109.5 . . ? C02M C02I Cl6 110.2(13) . . ? C02M C02I Cl7 123.1(10) . . ? C02M C02I Cl10 110.7(13) . . ? Cl6 C02I HC 109.6 . . ? Cl6 C02I HD 109.6 . . ? Cl7 C02I HE 106.6 . . ? Cl7 C02I HF 106.6 . . ? Cl10 C02I HG 109.5 . . ? Cl10 C02I HH 109.5 . . ? C023 C02K H02T 109.5 . . ? C023 C02K H02U 109.5 . . ? C023 C02K H02V 109.5 . . ? H02T C02K H02U 109.5 . . ? H02T C02K H02V 109.5 . . ? H02U C02K H02V 109.5 . . ? C01N C12 H12A 109.5 . . ? C01N C12 H12B 109.5 . . ? C01N C12 H12C 109.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Cl00 C02M H3AA 108.2 . . ? Cl00 C02M HI 108.2 . . ? C02I C02M Cl00 116.6(8) . . ? C02I C02M H3AA 108.2 . . ? C02I C02M HI 108.2 . . ? C02I C02M HJ 94.9 . . ? C02I C02M HK 94.9 . . ? C02I C02M Cl8 164.3(9) . . ? H3AA C02M HI 107.3 . . ? HJ C02M HK 103.2 . . ? Cl8 C02M HJ 94.9 . . ? Cl8 C02M HK 94.9 . . ? Cl03 C02N H6AA 109.4 . . ? Cl03 C02N HL 109.4 . . ? C02N C02N Cl03 111.2(12) 3_776 . ? C02N C02N H6AA 109.4 3_776 . ? C02N C02N HL 109.4 3_776 . ? H6AA C02N HL 108.0 . . ? C022 C02O H02W 109.5 . . ? C022 C02O H02X 109.5 . . ? C022 C02O H02Y 109.5 . . ? H02W C02O H02X 109.5 . . ? H02W C02O H02Y 109.5 . . ? H02X C02O H02Y 109.5 . . ? C01N C1AA H1AA 109.5 . . ? C01N C1AA H1AB 109.5 . . ? C01N C1AA H1AC 109.5 . . ? H1AA C1AA H1AB 109.5 . . ? H1AA C1AA H1AC 109.5 . . ? H1AB C1AA H1AC 109.5 . . ? C01N C0 H0A 109.5 . . ? C01N C0 H0B 109.5 . . ? C01N C0 H0C 109.5 . . ? H0A C0 H0B 109.5 . . ? H0A C0 H0C 109.5 . . ? H0B C0 H0C 109.5 . . ? C023 C02U H02Z 109.5 . . ? C023 C02U HM 109.5 . . ? C023 C02U HN 109.5 . . ? H02Z C02U HM 109.5 . . ? H02Z C02U HN 109.5 . . ? HM C02U HN 109.5 . . ? C02A C0AA H0AA 109.5 . . ? C02A C0AA H0AB 109.5 . . ? C02A C0AA H0AC 109.5 . . ? H0AA C0AA H0AB 109.5 . . ? H0AA C0AA H0AC 109.5 . . ? H0AB C0AA H0AC 109.5 . . ? C028 C02Z H02 110.7 . . ? C028 C02Z HO 110.7 . . ? C028 C02Z C032 105.3(18) . . ? H02 C02Z HO 108.8 . . ? C032 C02Z H02 110.7 . . ? C032 C02Z HO 110.7 . . ? C02Z C032 H03A 109.5 . . ? C02Z C032 H03B 109.5 . . ? C02Z C032 H03C 109.5 . . ? H03A C032 H03B 109.5 . . ? H03A C032 H03C 109.5 . . ? H03B C032 H03C 109.5 . . ? H20A C20 H20B 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C21 C20 H20A 109.5 . . ? C21 C20 H20B 109.5 . . ? C21 C20 H20C 109.5 . . ? C028 C21 C20 113.7(17) . . ? C028 C21 H21A 108.8 . . ? C028 C21 H21B 108.8 . . ? C20 C21 H21A 108.8 . . ? C20 C21 H21B 108.8 . . ? H21A C21 H21B 107.7 . . ? C02A C18B H18A 109.5 . . ? C02A C18B H18B 109.5 . . ? C02A C18B H18C 109.5 . . ? H18A C18B H18B 109.5 . . ? H18A C18B H18C 109.5 . . ? H18B C18B H18C 109.5 . . ? C02A C3 H3A 109.5 . . ? C02A C3 H3B 109.5 . . ? C02A C3 H3C 109.5 . . ? H3A C3 H3B 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C01N C13 H13A 109.5 . . ? C01N C13 H13B 109.5 . . ? C01N C13 H13C 109.5 . . ? H13A C13 H13B 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C01N C9 H9A 109.5 . . ? C01N C9 H9B 109.5 . . ? C01N C9 H9C 109.5 . . ? H9A C9 H9B 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C01N C7 H7A 109.5 . . ? C01N C7 H7B 109.5 . . ? C01N C7 H7C 109.5 . . ? H7A C7 H7B 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C02A C4 H4A 109.5 . . ? C02A C4 H4B 109.5 . . ? C02A C4 H4C 109.5 . . ? H4A C4 H4B 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C02A C5 H5A 109.5 . . ? C02A C5 H5B 109.5 . . ? C02A C5 H5C 109.5 . . ? H5A C5 H5B 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C02A C18A H18D 109.5 . . ? C02A C18A H18E 109.5 . . ? C02A C18A H18F 109.5 . . ? H18D C18A H18E 109.5 . . ? H18D C18A H18F 109.5 . . ? H18E C18A H18F 109.5 . . ? Cl2 C6 H6A 105.4 . . ? Cl2 C6 H6B 105.4 . . ? H6A C6 H6B 106.0 . . ? C8 C6 Cl2 127.6(19) . . ? C8 C6 H6A 105.4 . . ? C8 C6 H6B 105.4 . . ? Cl0A C8 H8A 108.2 . . ? Cl0A C8 H8B 108.2 . . ? C6 C8 Cl0A 116.2(18) . . ? C6 C8 H8A 108.2 . . ? C6 C8 H8B 108.2 . . ? H8A C8 H8B 107.4 . . ? 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 Ir1 Cl1 2.5129(19) . ? Ir1 Cl1 2.525(2) 3_656 ? Ir1 N1 2.035(8) . ? Ir1 N2 2.021(7) 3_656 ? Ir1 C2 2.031(9) 3_656 ? Ir1 C1 2.028(8) . ? Cl1 Ir1 2.525(2) 3_656 ? Cl03 C02N 1.778(12) . ? Cl04 C01Z 1.757(11) . ? Cl05 C01Z 1.749(11) . ? Cl06 C02G 1.721(14) . ? Cl00 C02M 1.756(10) . ? Cl08 C02F 1.768(13) . ? O00A C010 1.438(10) . ? O00A C015 1.379(10) . ? O00B C00X 1.409(10) . ? O00B C028 1.407(13) . ? N1 C00K 1.366(11) . ? N1 N00L 1.320(10) . ? N2 Ir1 2.021(7) 3_656 ? N2 N00E 1.322(10) . ? N2 C00O 1.384(11) . ? N00E N00M 1.328(10) . ? O00G C01F 1.384(11) . ? O00G C02D 1.421(12) . ? N00H N00L 1.353(11) . ? N00H C00R 1.339(12) . ? N00H C01T 1.458(11) . ? O00I C01U 1.396(11) . ? O00I C02C 1.458(12) . ? C00J H00A 0.9900 . ? C00J H00B 0.9900 . ? C00J N00M 1.491(10) . ? C00J C010 1.523(13) . ? C00K C00R 1.390(13) . ? C00K C00V 1.442(13) . ? N00M C011 1.349(11) . ? C00N C00O 1.451(12) . ? C00N C2 1.413(13) . ? C00N C016 1.395(13) . ? C00O C011 1.384(12) . ? C00P H00P 0.9500 . ? C00P C2 1.419(12) . ? C00P C00W 1.382(13) . ? C2 Ir1 2.031(9) 3_656 ? C00R H00R 0.9500 . ? C00S H00S 0.9500 . ? C00S C1 1.395(13) . ? C00S C01L 1.392(13) . ? C00T C00X 1.389(13) . ? C00T C00Y 1.534(12) . ? C00T C01G 1.397(12) . ? C1 C00V 1.407(13) . ? C00V C014 1.398(13) . ? C00W H00W 0.9500 . ? C00W C01D 1.396(14) . ? C00X C013 1.393(13) . ? C00Y H00C 0.9900 . ? C00Y H00D 0.9900 . ? C00Y C00Z 1.500(13) . ? C00Z C015 1.406(13) . ? C00Z C01V 1.398(13) . ? C010 H01A 0.9900 . ? C010 H01B 0.9900 . ? C011 H011 0.9500 . ? C012 C015 1.390(13) . ? C012 C017 1.526(12) . ? C012 C01A 1.389(13) . ? C013 C018 1.525(12) . ? C013 C01B 1.383(12) . ? C014 H014 0.9500 . ? C014 C01R 1.387(14) . ? C016 H016 0.9500 . ? C016 C01D 1.402(13) . ? C017 H01C 0.9900 . ? C017 H01D 0.9900 . ? C017 C01C 1.516(13) . ? C018 H01E 0.9900 . ? C018 H01F 0.9900 . ? C018 C01M 1.518(13) . ? Cl C02I 1.753(11) . ? C01A H01G 0.9500 . ? C01A C01W 1.409(13) . ? C01B H01H 0.9500 . ? C01B C01H 1.394(13) . ? C01C C01I 1.389(13) . ? C01C C01U 1.393(13) . ? C01D H01I 0.9500 . ? C01E C01I 1.390(13) . ? C01E C01J 1.387(13) . ? C01E C022 1.544(13) . ? C01F C01M 1.400(14) . ? C01F C01Q 1.388(13) . ? C01G H01J 0.9500 . ? C01G C01H 1.400(13) . ? C01H C023 1.533(13) . ? C01I H01K 0.9500 . ? C01J H01L 0.9500 . ? C01J C01S 1.405(13) . ? C01L H01M 0.9500 . ? C01L C01R 1.366(15) . ? C01M C01P 1.397(13) . ? C01N C01W 1.552(13) . ? C01N C12 1.544(18) . ? C01N C1AA 1.546(18) . ? C01N C0 1.498(18) . ? C01N C13 1.65(5) . ? C01N C9 1.45(5) . ? C01N C7 1.58(5) . ? C01O H01N 0.9800 . ? C01O H01O 0.9800 . ? C01O H01P 0.9800 . ? C01O C020 1.506(15) . ? C01P H01Q 0.9500 . ? C01P C01Y 1.396(14) . ? C01Q C01X 1.513(14) . ? C01Q C025 1.411(13) . ? C01R H01R 0.9500 . ? C01S C01U 1.402(13) . ? C01S C01X 1.526(13) . ? C01T H01S 0.9900 . ? C01T H01T 0.9900 . ? C01T C02D 1.475(14) . ? C01V H01V 0.9500 . ? C01V C01W 1.382(14) . ? C01X H01U 0.9900 . ? C01X H01W 0.9900 . ? C01Y C025 1.387(15) . ? C01Y C02A 1.549(15) . ? C01Z H01X 0.9900 . ? C01Z H01Y 0.9900 . ? C020 H02A 0.9900 . ? C020 H02B 0.9900 . ? C020 C02C 1.467(15) . ? C021 H02C 0.9800 . ? C021 H02D 0.9800 . ? C021 H02E 0.9800 . ? C021 C022 1.515(14) . ? C022 C024 1.561(15) . ? C022 C02O 1.542(15) . ? C023 C02E 1.527(15) . ? C023 C02K 1.541(17) . ? C023 C02U 1.538(17) . ? C024 H02F 0.9800 . ? C024 H02G 0.9800 . ? C024 H02H 0.9800 . ? C025 H025 0.9500 . ? C028 H02K 0.9900 . ? C028 H02L 0.9900 . ? C028 H02I 0.9900 . ? C028 H02J 0.9900 . ? C028 C02Z 1.498(10) . ? C028 C21 1.501(10) . ? C02A C0AA 1.541(12) . ? C02A C18B 1.546(12) . ? C02A C3 1.544(12) . ? C02A C4 1.540(12) . ? C02A C5 1.545(13) . ? C02A C18A 1.541(12) . ? C02C H02M 0.9900 . ? C02C H02N 0.9900 . ? C02D H02O 0.9900 . ? C02D H02P 0.9900 . ? C02E H02Q 0.9800 . ? C02E H02R 0.9800 . ? C02E H02S 0.9800 . ? C02F H4AA 0.9900 . ? C02F H 0.9900 . ? C02F C02G 1.473(18) . ? C02G H5AA 0.9900 . ? C02G HA 0.9900 . ? C02I HB 0.9900 . ? C02I H2AA 0.9900 . ? C02I HC 0.9900 . ? C02I HD 0.9900 . ? C02I HE 0.9900 . ? C02I HF 0.9900 . ? C02I HG 0.9900 . ? C02I HH 0.9900 . ? C02I C02M 1.518(18) . ? C02I Cl6 1.741(11) . ? C02I Cl7 1.728(11) . ? C02I Cl10 1.748(11) . ? C02K H02T 0.9800 . ? C02K H02U 0.9800 . ? C02K H02V 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C02M H3AA 0.9900 . ? C02M HI 0.9900 . ? C02M HJ 0.9900 . ? C02M HK 0.9900 . ? C02M Cl8 1.745(11) . ? C02N C02N 1.44(2) 3_776 ? C02N H6AA 0.9900 . ? C02N HL 0.9900 . ? C02O H02W 0.9800 . ? C02O H02X 0.9800 . ? C02O H02Y 0.9800 . ? C1AA H1AA 0.9800 . ? C1AA H1AB 0.9800 . ? C1AA H1AC 0.9800 . ? C0 H0A 0.9800 . ? C0 H0B 0.9800 . ? C0 H0C 0.9800 . ? C02U H02Z 0.9800 . ? C02U HM 0.9800 . ? C02U HN 0.9800 . ? C0AA H0AA 0.9800 . ? C0AA H0AB 0.9800 . ? C0AA H0AC 0.9800 . ? C02Z H02 0.9900 . ? C02Z HO 0.9900 . ? C02Z C032 1.511(10) . ? C032 H03A 0.9800 . ? C032 H03B 0.9800 . ? C032 H03C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C20 C21 1.509(10) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C18B H18A 0.9800 . ? C18B H18B 0.9800 . ? C18B H18C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C18A H18D 0.9800 . ? C18A H18E 0.9800 . ? C18A H18F 0.9800 . ? Cl0A C8 1.71(2) . ? Cl2 C6 1.64(2) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C6 C8 1.50(3) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? 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 N1 C00K C00R -172.5(6) . . . . ? Ir1 N1 C00K C00V 5.4(9) . . . . ? Ir1 N1 N00L N00H 169.6(6) . . . . ? Ir1 N2 N00E N00M -174.0(6) 3_656 . . . ? Ir1 N2 C00O C00N -2.0(10) 3_656 . . . ? Ir1 N2 C00O C011 174.1(6) 3_656 . . . ? Ir1 C1 C00V C00K 3.9(10) . . . . ? Ir1 C1 C00V C014 -177.9(7) . . . . ? Cl08 C02F C02G Cl06 66.9(13) . . . . ? O00B C00X C013 C018 -7.5(14) . . . . ? O00B C00X C013 C01B 177.6(8) . . . . ? O00B C028 C02Z C032 -176.4(16) . . . . ? O00B C028 C21 C20 -167(2) . . . . ? N1 C00K C00R N00H 1.7(9) . . . . ? N1 C00K C00V C1 -6.0(11) . . . . ? N1 C00K C00V C014 175.8(8) . . . . ? N2 N00E N00M C00J -179.3(7) . . . . ? N2 N00E N00M C011 1.2(9) . . . . ? N2 C00O C011 N00M 1.3(10) . . . . ? N00E N2 C00O C00N -176.7(7) . . . . ? N00E N2 C00O C011 -0.6(10) . . . . ? N00E N00M C011 C00O -1.6(10) . . . . ? O00G C01F C01M C018 3.7(12) . . . . ? O00G C01F C01M C01P 178.4(8) . . . . ? O00G C01F C01Q C01X -2.8(13) . . . . ? O00G C01F C01Q C025 -177.3(8) . . . . ? N00H C01T C02D O00G -176.0(10) . . . . ? C00J N00M C011 C00O 178.9(8) . . . . ? C00K N1 N00L N00H 0.7(9) . . . . ? C00K C00V C014 C01R 176.6(9) . . . . ? N00L N1 C00K C00R -1.5(9) . . . . ? N00L N1 C00K C00V 176.3(7) . . . . ? N00L N00H C00R C00K -1.4(10) . . . . ? N00L N00H C01T C02D 85.5(12) . . . . ? N00M C00J C010 O00A 176.6(7) . . . . ? C00N C00O C011 N00M 175.8(11) . . . . ? C00N C016 C01D C00W 2.0(15) . . . . ? C00O N2 N00E N00M -0.3(9) . . . . ? C00O C00N C2 Ir1 -2.3(10) . . . 3_656 ? C00O C00N C2 C00P -180.0(8) . . . . ? C00O C00N C016 C01D 178.6(9) . . . . ? C00P C00W C01D C016 -0.1(15) . . . . ? C2 C00N C00O N2 2.7(11) . . . . ? C2 C00N C00O C011 -171.4(11) . . . . ? C2 C00N C016 C01D -2.3(14) . . . . ? C2 C00P C00W C01D -1.4(14) . . . . ? C00R N00H N00L N1 0.4(9) . . . . ? C00R N00H C01T C02D -92.9(13) . . . . ? C00R C00K C00V C1 170.8(10) . . . . ? C00R C00K C00V C014 -7.3(17) . . . . ? C00S C1 C00V C00K -177.3(8) . . . . ? C00S C1 C00V C014 0.9(13) . . . . ? C00S C01L C01R C014 -0.7(17) . . . . ? C00T C00X C013 C018 169.6(9) . . . . ? C00T C00X C013 C01B -5.3(14) . . . . ? C00T C00Y C00Z C015 -79.5(10) . . . . ? C00T C00Y C00Z C01V 94.8(9) . . . . ? C00T C01G C01H C01B -3.2(14) . . . . ? C00T C01G C01H C023 176.3(9) . . . . ? C1 C00S C01L C01R 0.2(16) . . . . ? C1 C00V C014 C01R -1.4(14) . . . . ? C00V C00K C00R N00H -175.4(10) . . . . ? C00V C014 C01R C01L 1.2(16) . . . . ? C00W C00P C2 Ir1 -176.3(7) . . . 3_656 ? C00W C00P C2 C00N 1.0(13) . . . . ? C00X O00B C028 C02Z 73.8(17) . . . . ? C00X O00B C028 C21 161.1(18) . . . . ? C00X C00T C00Y C00Z 119.6(9) . . . . ? C00X C00T C01G C01H 0.0(14) . . . . ? C00X C013 C018 C01M -115.9(10) . . . . ? C00X C013 C01B C01H 1.9(15) . . . . ? C00Y C00T C00X O00B 5.7(13) . . . . ? C00Y C00T C00X C013 -171.4(9) . . . . ? C00Y C00T C01G C01H 175.9(8) . . . . ? C00Y C00Z C015 O00A -5.1(12) . . . . ? C00Y C00Z C015 C012 169.4(8) . . . . ? C00Y C00Z C01V C01W -172.3(8) . . . . ? C00Z C01V C01W C01A 0.5(13) . . . . ? C00Z C01V C01W C01N 179.0(8) . . . . ? C010 O00A C015 C00Z -112.1(9) . . . . ? C010 O00A C015 C012 73.4(10) . . . . ? C010 C00J N00M N00E -34.8(11) . . . . ? C010 C00J N00M C011 144.6(9) . . . . ? C012 C017 C01C C01I 64.0(11) . . . . ? C012 C017 C01C C01U -112.6(10) . . . . ? C012 C01A C01W C01N -179.0(8) . . . . ? C012 C01A C01W C01V -0.4(13) . . . . ? C013 C018 C01M C01F 71.3(11) . . . . ? C013 C018 C01M C01P -103.3(10) . . . . ? C013 C01B C01H C01G 2.3(14) . . . . ? C013 C01B C01H C023 -177.2(9) . . . . ? C015 O00A C010 C00J 98.8(9) . . . . ? C015 C00Z C01V C01W 2.2(13) . . . . ? C015 C012 C017 C01C 74.8(11) . . . . ? C015 C012 C01A C01W -2.4(13) . . . . ? C016 C00N C00O N2 -178.1(9) . . . . ? C016 C00N C00O C011 7.8(18) . . . . ? C016 C00N C2 Ir1 178.5(7) . . . 3_656 ? C016 C00N C2 C00P 0.9(13) . . . . ? C017 C012 C015 O00A 8.2(12) . . . . ? C017 C012 C015 C00Z -166.1(8) . . . . ? C017 C012 C01A C01W 169.1(8) . . . . ? C017 C01C C01I C01E -175.9(8) . . . . ? C017 C01C C01U O00I -5.4(13) . . . . ? C017 C01C C01U C01S 172.7(9) . . . . ? C018 C013 C01B C01H -173.3(9) . . . . ? C018 C01M C01P C01Y 171.8(9) . . . . ? Cl C02I C02M Cl00 10.3(13) . . . . ? C01A C012 C015 O00A 179.5(7) . . . . ? C01A C012 C015 C00Z 5.2(13) . . . . ? C01A C012 C017 C01C -96.5(10) . . . . ? C01B C013 C018 C01M 59.1(11) . . . . ? C01B C01H C023 C02E -170.7(10) . . . . ? C01B C01H C023 C02K 68.4(13) . . . . ? C01B C01H C023 C02U -50.7(13) . . . . ? C01E C01J C01S C01U -0.9(13) . . . . ? C01E C01J C01S C01X 176.8(8) . . . . ? C01F O00G C02D C01T -144.1(10) . . . . ? C01F C01M C01P C01Y -2.8(14) . . . . ? C01F C01Q C01X C01S -71.8(12) . . . . ? C01F C01Q C025 C01Y 0.5(15) . . . . ? C01G C00T C00X O00B -178.5(8) . . . . ? C01G C00T C00X C013 4.4(14) . . . . ? C01G C00T C00Y C00Z -56.2(11) . . . . ? C01G C01H C023 C02E 9.8(15) . . . . ? C01G C01H C023 C02K -111.1(12) . . . . ? C01G C01H C023 C02U 129.9(11) . . . . ? C01I C01C C01U O00I 178.0(8) . . . . ? C01I C01C C01U C01S -3.9(13) . . . . ? C01I C01E C01J C01S -2.0(13) . . . . ? C01I C01E C022 C021 -167.4(9) . . . . ? C01I C01E C022 C024 72.0(11) . . . . ? C01I C01E C022 C02O -46.0(12) . . . . ? C01J C01E C01I C01C 2.1(13) . . . . ? C01J C01E C022 C021 14.2(13) . . . . ? C01J C01E C022 C024 -106.5(10) . . . . ? C01J C01E C022 C02O 135.6(10) . . . . ? C01J C01S C01U O00I -177.9(8) . . . . ? C01J C01S C01U C01C 4.0(14) . . . . ? C01J C01S C01X C01Q -62.5(11) . . . . ? C01L C00S C1 Ir1 178.3(7) . . . . ? C01L C00S C1 C00V -0.3(14) . . . . ? C01M C01F C01Q C01X 172.3(9) . . . . ? C01M C01F C01Q C025 -2.2(14) . . . . ? C01M C01P C01Y C025 1.2(15) . . . . ? C01M C01P C01Y C02A -176.4(10) . . . . ? C01O C020 C02C O00I 178.4(10) . . . . ? C01P C01Y C025 C01Q 0.0(15) . . . . ? C01P C01Y C02A C0AA -48.3(19) . . . . ? C01P C01Y C02A C18B -135.8(16) . . . . ? C01P C01Y C02A C3 110.4(16) . . . . ? C01P C01Y C02A C4 -9(2) . . . . ? C01P C01Y C02A C5 64.1(17) . . . . ? C01P C01Y C02A C18A -172.9(16) . . . . ? C01Q C01F C01M C018 -171.4(8) . . . . ? C01Q C01F C01M C01P 3.3(13) . . . . ? C01T N00H N00L N1 -178.2(7) . . . . ? C01T N00H C00R C00K 177.1(8) . . . . ? C01U O00I C02C C020 -172.5(9) . . . . ? C01U C01C C01I C01E 0.8(14) . . . . ? C01U C01S C01X C01Q 115.1(10) . . . . ? C01V C00Z C015 O00A -179.5(7) . . . . ? C01V C00Z C015 C012 -5.1(12) . . . . ? C01X C01Q C025 C01Y -174.0(9) . . . . ? C01X C01S C01U O00I 4.6(14) . . . . ? C01X C01S C01U C01C -173.6(9) . . . . ? C022 C01E C01I C01C -176.4(8) . . . . ? C022 C01E C01J C01S 176.5(8) . . . . ? C025 C01Q C01X C01S 102.6(10) . . . . ? C025 C01Y C02A C0AA 134.2(17) . . . . ? C025 C01Y C02A C18B 46.7(18) . . . . ? C025 C01Y C02A C3 -67.1(18) . . . . ? C025 C01Y C02A C4 173.7(17) . . . . ? C025 C01Y C02A C5 -113.5(16) . . . . ? C025 C01Y C02A C18A 10(2) . . . . ? C028 O00B C00X C00T 77.1(12) . . . . ? C028 O00B C00X C013 -105.8(11) . . . . ? C02A C01Y C025 C01Q 177.6(10) . . . . ? C02C O00I C01U C01C -93.2(10) . . . . ? C02C O00I C01U C01S 88.7(10) . . . . ? C02D O00G C01F C01M 105.5(10) . . . . ? C02D O00G C01F C01Q -79.3(12) . . . . ? C12 C01N C01W C01A -54.9(12) . . . . ? C12 C01N C01W C01V 126.6(11) . . . . ? C1AA C01N C01W C01A 61.7(13) . . . . ? C1AA C01N C01W C01V -116.8(11) . . . . ? C0 C01N C01W C01A -178.2(10) . . . . ? C0 C01N C01W C01V 3.4(14) . . . . ? Cl7 C02I C02M Cl8 -3(5) . . . . ? C13 C01N C01W C01A -128(2) . . . . ? C13 C01N C01W C01V 53(2) . . . . ? C9 C01N C01W C01A -8(3) . . . . ? C9 C01N C01W C01V 173(2) . . . . ? C7 C01N C01W C01A 121(2) . . . . ? C7 C01N C01W C01V -57(2) . . . . ? Cl2 C6 C8 Cl0A 36(3) . . . . ? 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 0.101 -0.172 0.369 191.7 46.1 '1 CH2Cl2' 2 -0.101 0.172 0.631 191.7 45.4 '1 CH2Cl2' 3 -0.101 0.328 0.131 191.7 45.4 '1 CH2Cl2' 4 0.101 0.672 0.869 191.7 46.1 '1 CH2Cl2' 5 0.181 0.736 0.654 8.5 0.0 ? 6 0.181 0.764 0.154 8.5 0.0 ? 7 0.819 0.236 0.846 8.5 0.0 ? 8 0.819 0.264 0.346 8.5 0.0 ?