#------------------------------------------------------------------------------ #$Date: 2021-07-05 20:29:19 +0300 (Mon, 05 Jul 2021) $ #$Revision: 267145 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/75/7707514.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_7707514 loop_ _publ_author_name 'Cheung, Wai-Man' 'Chong, Man-Chun' 'Sung, Herman H.-Y.' 'Cheng, Shun-Cheung' 'Williams, Ian D.' 'Ko, Chi-Chiu' 'Leung, Wa-Hung' _publ_section_title ; Synthesis, structure and reactivity of iridium complexes containing a bis-cyclometalated tridentate C^N^C ligand. ; _journal_issue 24 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 8512 _journal_page_last 8523 _journal_paper_doi 10.1039/d1dt01269j _journal_volume 50 _journal_year 2021 _chemical_formula_moiety 'C41 H51 Cl2 Hg Ir2 N' _chemical_formula_sum 'C41 H51 Cl2 Hg Ir2 N' _chemical_formula_weight 1213.71 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2020-04-17 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2021-03-25 deposited with the CCDC. 2021-05-27 downloaded from the CCDC. ; _cell_angle_alpha 69.278(4) _cell_angle_beta 72.867(4) _cell_angle_gamma 83.902(3) _cell_formula_units_Z 2 _cell_length_a 10.6104(4) _cell_length_b 12.0252(5) _cell_length_c 16.6227(8) _cell_measurement_reflns_used 8127 _cell_measurement_temperature 173.00(10) _cell_measurement_theta_max 71.8560 _cell_measurement_theta_min 2.9450 _cell_volume 1895.68(15) _computing_cell_refinement 'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)' _computing_data_collection 'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)' _computing_data_reduction 'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)' _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 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 173.00(10) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 5.1788 _diffrn_detector_type Atlas _diffrn_measured_fraction_theta_full 0.982 _diffrn_measured_fraction_theta_max 0.947 _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 27.00 126.00 1.00 3.00 -- 105.39 -61.00 150.00 99 2 \w -130.00 53.00 1.00 2.00 -- -37.73 0.00-120.00 183 3 \w 27.00 82.00 1.00 2.00 -- 37.73-125.00-180.00 55 4 \w 27.00 61.00 1.00 2.00 -- 37.73-125.00 90.00 34 5 \w 28.00 88.00 1.00 2.00 -- 37.73-125.00 -30.00 60 6 \w 103.00 175.00 1.00 3.00 -- 105.39 77.00 150.00 72 7 \w 34.00 109.00 1.00 3.00 -- 105.39-111.00 -30.00 75 8 \w 20.00 107.00 1.00 3.00 -- 105.39 -94.00 120.00 87 9 \w 105.00 178.00 1.00 3.00 -- 105.39 111.00 120.00 73 10 \w 79.00 172.00 1.00 3.00 -- 105.39 45.00 -60.00 93 11 \w 69.00 175.00 1.00 3.00 -- 105.39 30.00-120.00 106 12 \w 33.00 113.00 1.00 3.00 -- 105.39-133.00 106.00 80 ; _diffrn_measurement_device 'kappa diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.1073631000 _diffrn_orient_matrix_UB_12 -0.0770709000 _diffrn_orient_matrix_UB_13 0.0794866000 _diffrn_orient_matrix_UB_21 -0.0619586000 _diffrn_orient_matrix_UB_22 -0.0229382000 _diffrn_orient_matrix_UB_23 -0.0656486000 _diffrn_orient_matrix_UB_31 0.0878578000 _diffrn_orient_matrix_UB_32 -0.1108847000 _diffrn_orient_matrix_UB_33 0.0015646000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0215 _diffrn_reflns_av_unetI/netI 0.0305 _diffrn_reflns_Laue_measured_fraction_full 0.982 _diffrn_reflns_Laue_measured_fraction_max 0.947 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 10545 _diffrn_reflns_point_group_measured_fraction_full 0.982 _diffrn_reflns_point_group_measured_fraction_max 0.947 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 71.932 _diffrn_reflns_theta_min 2.957 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_current 0.80 _diffrn_source_power 0.040 _diffrn_source_target Cu _diffrn_source_type 'SuperNova (Cu) X-ray Source' _diffrn_source_voltage 50 _exptl_absorpt_coefficient_mu 21.942 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.53422 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.69a (Rigaku Oxford Diffraction, 2020) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour red _exptl_crystal_colour_primary red _exptl_crystal_density_diffrn 2.126 _exptl_crystal_description block _exptl_crystal_F_000 1144 _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _refine_diff_density_max 1.325 _refine_diff_density_min -1.804 _refine_diff_density_rms 0.138 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 523 _refine_ls_number_reflns 7056 _refine_ls_number_restraints 128 _refine_ls_restrained_S_all 1.014 _refine_ls_R_factor_all 0.0262 _refine_ls_R_factor_gt 0.0245 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0340P)^2^+3.0616P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0625 _refine_ls_wR_factor_ref 0.0637 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6636 _reflns_number_total 7056 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1dt01269j2.cif _cod_data_source_block wai252_173k _cod_depositor_comments 'Adding full bibliography for 7707513--7707520.cif.' _cod_original_cell_volume 1895.69(15) _cod_database_code 7707514 _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. ; _diffrn_oxdiff_digest_frames ; 01f351406aaf6dcd27e3e81f9eacf003ed000289fdb ; _diffrn_oxdiff_digest_hkl ; 01197a37759465d848e20c79bff56b7e86f885 ; _reflns_odcompleteness_completeness 98.43 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _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 At 1.5 times of: All C(H,H,H) groups 2. Restrained distances C43-C42 = C43-C44 = C45-C44 1.52 with sigma of 0.02 Ir2-Cl2A \\sim Ir2-Cl2 with sigma of 0.02 C18-C21 \\sim C18-C19 \\sim C18-C20 with sigma of 0.02 C20A-C18A \\sim C19A-C18A \\sim C21A-C18A with sigma of 0.02 C18-C3 \\sim C3-C18A with sigma of 0.02 3. Uiso/Uaniso restraints and constraints Uanis(C21A) \\sim Ueq, Uanis(C19A) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.01 Uanis(C18A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.003 Uanis(C18) \\sim Ueq, Uanis(C20A) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.01 4. Rigid body (RIGU) restrains C41, C42, C43, C44, C45, C46, C47, C48 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001 C41, C42A, C43A, C44A, C45A, C46A, C47, C48 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001 5. Others Fixed Sof: Cl2(0.5) Cl2A(0.5) C18(0.65) C18A(0.35) C19(0.65) H19A(0.65) H19B(0.65) H19C(0.65) C19A(0.35) H19D(0.35) H19E(0.35) H19F(0.35) C20(0.65) H20A(0.65) H20B(0.65) H20C(0.65) C20A(0.35) H20D(0.35) H20E(0.35) H20F(0.35) C21(0.65) H21A(0.65) H21B(0.65) H21C(0.65) C21A(0.35) H21D(0.35) H21E(0.35) H21F(0.35) H41(0.5) H41A(0.5) C42(0.5) H42(0.5) C42A(0.5) H42A(0.5) C43(0.5) H43A(0.5) H43B(0.5) C43A(0.5) H43C(0.5) H43D(0.5) C44(0.5) H44A(0.5) H44B(0.5) C44A(0.5) H44C(0.5) H44D(0.5) C45(0.5) H45(0.5) C45A(0.5) H45A(0.5) C46(0.5) H46(0.5) C46A(0.5) H46A(0.5) H47A(0.5) H47B(0.5) H47C(0.5) H47D(0.5) 6.a Ternary CH refined with riding coordinates: C31(H31), C32(H32), C35(H35), C36(H36), C41(H41), C41(H41A), C42(H42), C42A(H42A), C45(H45), C45A(H45A), C46(H46), C46A(H46A) 6.b Secondary CH2 refined with riding coordinates: C33(H33A,H33B), C34(H34A,H34B), C37(H37A,H37B), C38(H38A,H38B), C43(H43A, H43B), C43A(H43C,H43D), C44(H44A,H44B), C44A(H44C,H44D), C47(H47A,H47B), C47(H47C,H47D), C48(H48A,H48B) 6.c Aromatic/amide H refined with riding coordinates: C2(H2), C4(H4), C5(H5), C8(H8), C9(H9), C10(H10), C13(H13), C14(H14), C16(H16) 6.d Idealised Me refined as rotating group: C19(H19A,H19B,H19C), C19A(H19D,H19E,H19F), C20(H20A,H20B,H20C), C20A(H20D, H20E,H20F), C21(H21A,H21B,H21C), C21A(H21D,H21E,H21F), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C) ; _shelx_res_file ; wai252_173k.res created by SHELXL-2014/7 TITL wai252_173k_a.res in P-1 REM Old TITL wai252_173K in P-1 REM SHELXT solution in P-1 REM R1 0.120, Rweak 0.006, Alpha 0.061, Orientation as input REM Formula found by SHELXT: Cl2 Ir3 C35 N8 CELL 1.54184 10.6104 12.0252 16.6227 69.278 72.867 83.902 ZERR 2 0.0004 0.0005 0.0008 0.004 0.004 0.003 LATT 1 SFAC C H Cl Hg Ir N UNIT 82 102 4 2 4 2 DFIX 1.52 C43 C42 C43 C44 C45 C44 SADI Ir2 Cl2A Ir2 Cl2 SADI C18 C21 C18 C19 C18 C20 SADI C20A C18A C19A C18A C21A C18A SADI C18 C3 C3 C18A RIGU 0.001 0.001 C41 C42 C43 C44 C45 C46 C47 C48 RIGU 0.001 0.001 C41 C42A C43A C44A C45A C46A > C48 ISOR 0.05 0.01 C21A C19A ISOR 0.01 0.003 C18A ISOR 0.05 0.01 C18 C20A L.S. 10 PLAN 20 TEMP -100 BOND $H list 4 fmap 2 acta REM REM REM WGHT 0.034000 3.061600 FVAR 0.23871 HG1 4 0.175298 0.635943 0.237075 11.00000 0.01883 0.02019 = 0.03033 -0.00019 -0.00609 0.00077 IR1 5 0.296658 0.471650 0.336094 11.00000 0.01459 0.01512 = 0.01626 -0.00285 0.00094 -0.00013 IR2 5 0.094297 0.816116 0.114320 11.00000 0.01405 0.03655 = 0.01380 -0.00210 -0.00526 -0.00336 CL1 3 -0.069062 0.817985 0.243433 11.00000 0.02190 0.07687 = 0.03385 -0.02351 0.00168 0.00199 PART 1 CL2 3 -0.015188 0.685057 0.090514 10.50000 0.03069 0.06555 = 0.05383 -0.02961 -0.00679 -0.01901 PART 0 PART 2 CL2A 3 -0.010265 0.637856 0.127291 10.50000 0.03690 0.03189 = 0.05658 -0.00488 -0.02549 -0.01274 PART 0 N1 6 0.451100 0.477238 0.226589 11.00000 0.01605 0.02172 = 0.01769 -0.00507 0.00066 0.00074 C1 1 0.405991 0.621054 0.318132 11.00000 0.01921 0.01815 = 0.02240 -0.00275 -0.00401 0.00173 C2 1 0.370207 0.716830 0.350614 11.00000 0.02517 0.02015 = 0.02447 -0.00644 -0.00033 0.00192 AFIX 43 H2 2 0.284755 0.716670 0.390159 11.00000 -1.20000 AFIX 0 C3 1 0.452995 0.810743 0.327877 11.00000 0.03260 0.01924 = 0.02118 -0.00418 -0.00561 0.00133 C4 1 0.582744 0.806414 0.275582 11.00000 0.03020 0.01871 = 0.02277 0.00012 -0.00767 -0.00783 AFIX 43 H4 2 0.643994 0.865781 0.264685 11.00000 -1.20000 AFIX 0 C5 1 0.622450 0.716445 0.239676 11.00000 0.01783 0.02587 = 0.02163 -0.00347 -0.00238 -0.00434 AFIX 43 H5 2 0.709972 0.714881 0.203242 11.00000 -1.20000 AFIX 0 C6 1 0.532529 0.627724 0.257499 11.00000 0.01892 0.01843 = 0.01865 -0.00206 -0.00200 -0.00173 C7 1 0.556789 0.546404 0.206538 11.00000 0.01738 0.02179 = 0.02179 -0.00480 -0.00335 0.00079 C8 1 0.667008 0.543633 0.136874 11.00000 0.01758 0.03297 = 0.02782 -0.00973 -0.00003 -0.00236 AFIX 43 H8 2 0.742415 0.589925 0.123613 11.00000 -1.20000 AFIX 0 C9 1 0.666210 0.472792 0.086795 11.00000 0.02281 0.04836 = 0.02880 -0.01873 0.00667 0.00064 AFIX 43 H9 2 0.742026 0.468710 0.040111 11.00000 -1.20000 AFIX 0 C10 1 0.554331 0.407946 0.105126 11.00000 0.02811 0.04455 = 0.03099 -0.02126 -0.00139 -0.00294 AFIX 43 H10 2 0.552127 0.361472 0.069735 11.00000 -1.20000 AFIX 0 C11 1 0.445276 0.411333 0.175672 11.00000 0.02273 0.02725 = 0.02290 -0.01194 -0.00186 -0.00042 C12 1 0.317337 0.356255 0.201276 11.00000 0.02338 0.02600 = 0.02414 -0.00973 -0.00373 -0.00225 C13 1 0.283922 0.297763 0.150756 11.00000 0.03097 0.04353 = 0.02983 -0.01815 -0.00019 -0.00865 AFIX 43 H13 2 0.348708 0.286783 0.100756 11.00000 -1.20000 AFIX 0 C14 1 0.157730 0.256239 0.173315 11.00000 0.03546 0.04654 = 0.03940 -0.02085 -0.00869 -0.01017 AFIX 43 H14 2 0.136513 0.217112 0.138367 11.00000 -1.20000 AFIX 0 C15 1 0.060423 0.270559 0.246556 11.00000 0.02567 0.03033 = 0.03147 -0.00327 -0.01004 -0.00419 C16 1 0.096182 0.326834 0.296837 11.00000 0.02108 0.02725 = 0.02548 -0.00463 -0.00302 -0.00322 AFIX 43 H16 2 0.031179 0.335166 0.347710 11.00000 -1.20000 AFIX 0 C17 1 0.222334 0.371754 0.276669 11.00000 0.01934 0.02177 = 0.02088 -0.00392 -0.00440 0.00046 PART 1 C18 1 0.397237 0.920684 0.356085 10.65000 0.02650 0.01694 = 0.02949 -0.00689 -0.01531 0.00245 PART 0 PART 2 C18A 1 0.424101 0.916185 0.363641 10.35000 0.02284 0.02829 = 0.02075 -0.00781 -0.01223 0.00199 PART 0 PART 1 C19 1 0.474771 0.928155 0.418100 10.65000 0.06783 0.03615 = 0.05361 -0.02695 -0.03962 0.01360 AFIX 137 H19A 2 0.460703 0.855518 0.470719 10.65000 -1.50000 H19B 2 0.444498 0.997084 0.437189 10.65000 -1.50000 H19C 2 0.568906 0.936662 0.386222 10.65000 -1.50000 AFIX 0 PART 0 PART 2 C19A 1 0.378946 0.870744 0.466676 10.35000 0.07030 0.05361 = 0.04882 -0.02042 -0.01359 0.01468 AFIX 137 H19D 2 0.317431 0.804508 0.488007 10.35000 -1.50000 H19E 2 0.334886 0.935244 0.487675 10.35000 -1.50000 H19F 2 0.455785 0.843561 0.489918 10.35000 -1.50000 AFIX 0 PART 0 PART 1 C20 1 0.250958 0.913207 0.403963 10.65000 0.03545 0.03158 = 0.07631 -0.03721 0.00141 0.00311 AFIX 137 H20A 2 0.201433 0.905561 0.364877 10.65000 -1.50000 H20B 2 0.222852 0.985457 0.418963 10.65000 -1.50000 H20C 2 0.234098 0.843774 0.458975 10.65000 -1.50000 AFIX 0 PART 0 PART 2 C20A 1 0.304275 0.976023 0.331277 10.35000 0.08085 0.06675 = 0.07843 -0.03593 -0.02875 0.00870 AFIX 137 H20D 2 0.331398 1.013447 0.266011 10.35000 -1.50000 H20E 2 0.268404 1.036668 0.358792 10.35000 -1.50000 H20F 2 0.236557 0.916138 0.348374 10.35000 -1.50000 AFIX 0 PART 0 PART 1 C21 1 0.420419 1.032448 0.274111 10.65000 0.07038 0.01828 = 0.04097 -0.00871 -0.01691 0.00199 AFIX 137 H21A 2 0.515247 1.042799 0.244743 10.65000 -1.50000 H21B 2 0.385516 1.101372 0.292221 10.65000 -1.50000 H21C 2 0.375471 1.025388 0.232403 10.65000 -1.50000 AFIX 0 PART 0 PART 2 C21A 1 0.535968 1.005117 0.335308 10.35000 0.07267 0.05004 = 0.08255 -0.04100 -0.00121 -0.01056 AFIX 137 H21D 2 0.611324 0.963507 0.355790 10.35000 -1.50000 H21E 2 0.505067 1.067197 0.362100 10.35000 -1.50000 H21F 2 0.562904 1.041399 0.269952 10.35000 -1.50000 AFIX 0 PART 0 C22 1 -0.079955 0.224130 0.273846 11.00000 0.02779 0.04712 = 0.04919 -0.01506 -0.01601 -0.00573 C23 1 -0.089528 0.099765 0.344440 11.00000 0.04378 0.04876 = 0.07549 -0.00897 -0.01320 -0.01628 AFIX 137 H23A 2 -0.034226 0.044470 0.317475 11.00000 -1.50000 H23B 2 -0.181368 0.072899 0.367031 11.00000 -1.50000 H23C 2 -0.059117 0.102320 0.394001 11.00000 -1.50000 AFIX 0 C24 1 -0.118269 0.218023 0.193341 11.00000 0.03616 0.14989 = 0.06738 -0.04137 -0.02319 -0.01701 AFIX 137 H24A 2 -0.103727 0.295722 0.145596 11.00000 -1.50000 H24B 2 -0.211542 0.196480 0.211643 11.00000 -1.50000 H24C 2 -0.063991 0.157970 0.171405 11.00000 -1.50000 AFIX 0 C25 1 -0.181460 0.305369 0.313909 11.00000 0.02289 0.06568 = 0.09911 -0.03352 -0.01724 -0.00256 AFIX 137 H25A 2 -0.168641 0.301736 0.370812 11.00000 -1.50000 H25B 2 -0.270778 0.278685 0.324228 11.00000 -1.50000 H25C 2 -0.169548 0.387378 0.272180 11.00000 -1.50000 AFIX 0 C31 1 0.413862 0.375633 0.430149 11.00000 0.02755 0.02065 = 0.02095 -0.00083 -0.01045 0.00458 AFIX 13 H31 2 0.511342 0.386872 0.404083 11.00000 -1.20000 AFIX 0 C32 1 0.359507 0.293092 0.405512 11.00000 0.02937 0.01720 = 0.02229 -0.00102 -0.00980 0.00422 AFIX 13 H32 2 0.425951 0.256349 0.365507 11.00000 -1.20000 AFIX 0 C33 1 0.243230 0.214254 0.465981 11.00000 0.03904 0.01773 = 0.02727 0.00106 -0.00833 -0.00421 AFIX 23 H33A 2 0.270610 0.153519 0.516159 11.00000 -1.20000 H33B 2 0.216933 0.172195 0.431913 11.00000 -1.20000 AFIX 0 C34 1 0.123072 0.282050 0.504430 11.00000 0.03662 0.02809 = 0.02451 -0.00407 0.00479 -0.01532 AFIX 23 H34A 2 0.041651 0.242126 0.511394 11.00000 -1.20000 H34B 2 0.124637 0.278110 0.564634 11.00000 -1.20000 AFIX 0 C35 1 0.118399 0.412613 0.446055 11.00000 0.02139 0.02890 = 0.02214 -0.00551 0.00665 -0.00733 AFIX 13 H35 2 0.034502 0.436756 0.428502 11.00000 -1.20000 AFIX 0 C36 1 0.178788 0.504192 0.456653 11.00000 0.02484 0.02417 = 0.02536 -0.00805 0.00945 -0.00409 AFIX 13 H36 2 0.129600 0.581341 0.445180 11.00000 -1.20000 AFIX 0 C37 1 0.253913 0.481988 0.525513 11.00000 0.04388 0.03255 = 0.01990 -0.01103 0.00386 -0.00712 AFIX 23 H37A 2 0.190834 0.457334 0.585939 11.00000 -1.20000 H37B 2 0.295145 0.557322 0.516099 11.00000 -1.20000 AFIX 0 C38 1 0.361433 0.386580 0.521856 11.00000 0.04138 0.03054 = 0.02496 -0.00617 -0.01110 -0.00376 AFIX 23 H38A 2 0.435141 0.406336 0.539603 11.00000 -1.20000 H38B 2 0.324961 0.308963 0.565577 11.00000 -1.20000 AFIX 0 C41 1 0.226492 0.912707 0.139994 11.00000 0.03056 0.02618 = 0.02974 -0.00448 -0.00766 -0.00467 PART 1 AFIX 13 H41 2 0.206399 0.894958 0.205969 10.50000 -1.20000 AFIX 13 PART 0 PART 2 H41A 2 0.199492 0.927197 0.198392 10.50000 -1.20000 AFIX 0 PART 0 PART 1 C42 1 0.143981 0.991367 0.108804 10.50000 0.02657 0.02881 = 0.02373 0.00263 -0.00105 -0.00461 AFIX 13 H42 2 0.080781 1.022790 0.153687 10.50000 -1.20000 AFIX 0 PART 0 PART 2 C42A 1 0.162239 0.987903 0.067826 10.50000 0.03057 0.03395 = 0.03141 0.00047 -0.00870 -0.00399 AFIX 13 H42A 2 0.094261 1.043966 0.087885 10.50000 -1.20000 AFIX 0 PART 0 PART 1 C43 1 0.179440 1.078658 0.012809 10.50000 0.03733 0.03917 = 0.02585 0.00568 -0.00111 -0.00318 AFIX 23 H43A 2 0.239315 1.140185 0.007557 10.50000 -1.20000 H43B 2 0.098228 1.118904 -0.001131 10.50000 -1.20000 AFIX 0 PART 0 PART 2 C43A 1 0.231278 1.035273 -0.032710 10.50000 0.04186 0.04266 = 0.03165 -0.00045 -0.00753 -0.00364 AFIX 23 H43C 2 0.189894 1.111373 -0.060664 10.50000 -1.20000 H43D 2 0.325114 1.050977 -0.041918 10.50000 -1.20000 AFIX 0 PART 0 PART 1 C44 1 0.246152 1.016984 -0.055127 10.50000 0.01977 0.04074 = 0.02401 0.00477 -0.00092 -0.00587 AFIX 23 H44A 2 0.227454 1.062257 -0.113001 10.50000 -1.20000 H44B 2 0.342819 1.016680 -0.064848 10.50000 -1.20000 AFIX 0 PART 0 PART 2 C44A 1 0.222716 0.947591 -0.077725 10.50000 0.04358 0.04105 = 0.02693 0.00366 -0.00904 -0.00204 AFIX 23 H44C 2 0.149360 0.971942 -0.105895 10.50000 -1.20000 H44D 2 0.305265 0.952222 -0.126073 10.50000 -1.20000 AFIX 0 PART 0 PART 1 C45 1 0.199340 0.892339 -0.024391 10.50000 0.02118 0.04104 = 0.01751 0.00575 -0.00020 -0.00629 AFIX 13 H45 2 0.157719 0.876409 -0.065939 10.50000 -1.20000 AFIX 0 PART 0 PART 2 C45A 1 0.201960 0.823275 -0.017750 10.50000 0.02778 0.04042 = 0.01423 -0.00096 -0.00408 -0.00004 AFIX 13 H45A 2 0.163005 0.773029 -0.041095 10.50000 -1.20000 AFIX 0 PART 0 PART 1 C46 1 0.268161 0.792992 0.020556 10.50000 0.02285 0.03935 = 0.01168 -0.00116 -0.00012 -0.00400 AFIX 13 H46 2 0.268844 0.721021 0.003530 10.50000 -1.20000 AFIX 0 PART 0 PART 2 C46A 1 0.281374 0.757127 0.040026 10.50000 0.02454 0.03554 = 0.01062 -0.00077 -0.00118 -0.00186 AFIX 13 H46A 2 0.287910 0.669911 0.050085 10.50000 -1.20000 AFIX 0 PART 0 C47 1 0.395227 0.808966 0.045096 11.00000 0.02628 0.04101 = 0.03036 -0.00865 -0.00844 0.00077 PART 1 AFIX 23 H47A 2 0.426727 0.729902 0.077316 10.50000 -1.20000 H47B 2 0.465440 0.845214 -0.010650 10.50000 -1.20000 AFIX 23 PART 0 PART 2 H47C 2 0.443505 0.857110 -0.016485 10.50000 -1.20000 H47D 2 0.454428 0.743218 0.067261 10.50000 -1.20000 AFIX 0 PART 0 C48 1 0.370591 0.886649 0.103057 11.00000 0.02986 0.04529 = 0.03369 -0.01255 -0.01192 0.00080 AFIX 23 H48A 2 0.408960 0.847001 0.153765 11.00000 -1.20000 H48B 2 0.417469 0.962974 0.067236 11.00000 -1.20000 AFIX 0 HKLF 4 REM wai252_173k_a.res in P-1 REM R1 = 0.0245 for 6636 Fo > 4sig(Fo) and 0.0262 for all 7056 data REM 523 parameters refined using 128 restraints END WGHT 0.0323 1.9763 REM Highest difference peak 1.325, deepest hole -1.804, 1-sigma level 0.138 Q1 1 0.2169 0.5841 0.3168 11.00000 0.05 1.33 Q2 1 0.1664 0.5855 0.3270 11.00000 0.05 1.23 Q3 1 0.1578 0.7149 0.1351 11.00000 0.05 1.20 Q4 1 0.3119 0.5266 0.2467 11.00000 0.05 1.11 Q5 1 0.0832 0.7597 0.2070 11.00000 0.05 1.06 Q6 1 0.2450 0.5401 0.2501 11.00000 0.05 1.01 Q7 1 0.3613 0.3852 0.3468 11.00000 0.05 0.98 Q8 1 0.1211 0.8775 0.0254 11.00000 0.05 0.94 Q9 1 0.2824 0.4140 0.4236 11.00000 0.05 0.92 Q10 1 0.1115 0.8988 0.0607 11.00000 0.05 0.88 Q11 1 0.3196 0.5554 0.2810 11.00000 0.05 0.83 Q12 1 0.1608 0.5613 0.2828 11.00000 0.05 0.79 Q13 1 0.0364 0.9070 0.1020 11.00000 0.05 0.79 Q14 1 0.2772 0.3852 0.3950 11.00000 0.05 0.76 Q15 1 0.1872 0.4762 0.3298 11.00000 0.05 0.75 Q16 1 0.0994 0.9656 0.1060 11.00000 0.05 0.73 Q17 1 0.1180 0.7724 0.0767 11.00000 0.05 0.69 Q18 1 0.3837 0.6144 0.1919 11.00000 0.05 0.69 Q19 1 0.2983 0.3242 0.3422 11.00000 0.05 0.68 Q20 1 0.3993 0.6043 0.2090 11.00000 0.05 0.64 ; _shelx_res_checksum 89705 _shelx_hkl_file ; 0 0 -1 155.26 4.19 0 0 -2 2816.74 58.63 0 0 -3 2.34 1.12 0 0 -4 61.86 4.23 0 0 -5 1351.69 33.85 0 0 -6 218.91 10.31 0 0 -7 489.75 18.05 0 0 -8 1286.68 36.40 0 0 -9 4262.96 98.25 0 0 -10 341.20 16.33 0 0 -11 506.82 21.25 0 0 -11 511.18 17.37 0 0 -12 289.96 12.79 0 0 -13 309.00 13.85 0 0 -14 666.82 22.80 0 0 -15 0.87 1.58 0 0 -16 1.57 1.57 0 0 -17 321.77 11.74 0 0 -18 302.25 9.57 0 1 -17 3.38 1.34 0 1 -16 893.29 24.92 0 -1 16 895.55 22.70 0 1 -15 103.68 7.06 0 -1 15 103.59 6.30 0 1 -14 1.54 1.87 0 1 -13 163.83 9.64 0 1 -12 669.30 21.92 0 1 -11 20.69 3.98 0 1 -11 16.88 2.81 0 1 -10 9.13 2.83 0 1 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1960.60 49.02 5 -5 7 855.18 26.42 5 -5 8 286.75 13.50 5 -5 9 5.24 2.04 5 -5 10 128.98 8.62 5 -5 11 71.51 6.14 5 -5 12 71.34 5.70 5 -5 13 8.34 1.95 5 -5 14 831.01 21.36 5 -4 -15 398.58 12.70 5 -4 -14 205.17 8.50 5 -4 -13 1.54 1.07 5 -4 -12 415.31 15.06 5 -4 -11 549.87 18.28 5 -4 -10 938.17 26.76 5 -4 -9 1.34 1.34 5 -4 -9 0.54 1.16 5 -4 -8 102.76 6.21 5 -4 -8 105.22 6.81 5 -4 -7 835.07 25.54 5 -4 -7 816.63 21.93 5 -4 -7 794.12 23.67 5 -4 -6 267.97 12.28 5 -4 -6 256.97 10.87 5 -4 -5 218.75 10.81 5 -4 -4 340.61 13.68 5 -4 -3 400.53 15.10 5 -4 -2 3971.28 87.33 5 -4 -2 3894.66 87.41 5 -4 -1 1621.14 41.29 5 -4 -1 1625.14 41.12 5 -4 0 1165.02 31.50 5 -4 0 1124.22 31.81 5 -4 1 233.76 11.71 5 -4 2 327.74 14.71 5 -4 3 50.68 5.58 5 -4 4 5.58 2.20 5 -4 5 488.58 19.97 5 -4 6 9.59 1.98 5 -4 6 8.30 2.63 5 -4 7 3766.35 88.60 5 -4 7 3855.17 84.41 5 -4 7 3596.38 81.34 5 -4 8 209.97 12.16 5 -4 8 220.64 11.02 5 -4 8 198.88 9.50 5 -4 9 1076.43 31.02 5 -4 9 1001.71 28.57 5 -4 10 25.97 3.92 5 -4 10 20.53 3.13 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3 -5 405.13 18.50 5 3 -5 395.78 14.10 5 3 -4 1220.65 36.77 5 3 -3 104.41 8.05 5 3 -2 258.57 12.65 5 3 -1 1312.98 36.08 5 3 0 2418.91 58.08 5 3 1 2440.59 57.73 5 3 2 54.45 4.89 -5 -3 -3 53.62 4.86 -5 -3 -4 519.22 17.88 -5 -3 -5 1372.26 36.47 -5 -3 -6 54.06 5.19 -5 -3 -7 586.01 20.59 -5 -3 -8 295.74 14.17 -5 -3 -9 3483.99 82.88 -5 -3 -10 907.19 30.18 -5 -3 -11 369.27 17.56 5 3 12 2.76 1.33 -5 -3 -12 2.13 1.76 -5 -3 -12 2.75 1.40 -5 -3 -13 34.07 4.02 -5 -3 -13 35.22 4.32 -5 -3 -14 356.70 14.37 -5 -3 -14 368.71 15.05 -5 -3 -15 18.56 2.98 -5 -3 -15 20.64 3.44 -5 -3 -16 66.84 5.31 -5 -3 -16 73.25 6.15 -5 -3 -17 26.23 3.71 -5 -3 -18 804.37 22.90 -5 -3 -19 16.49 2.21 -5 -3 -20 70.17 3.43 -5 -4 12 440.93 13.37 -5 -4 12 462.40 13.83 -5 -4 11 169.69 8.56 -5 -4 11 176.85 8.74 -5 -4 10 224.42 11.24 5 4 -10 233.53 9.74 -5 -4 9 298.04 14.27 5 4 -9 310.24 12.48 -5 -4 8 228.96 12.62 5 4 -8 215.81 10.45 -5 -4 7 824.46 27.46 5 4 -7 783.75 24.05 -5 -4 6 359.90 16.31 5 4 -6 366.35 13.85 -5 -4 5 207.13 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8.06 -5 -5 2 249.10 11.54 5 5 -2 249.81 13.14 5 5 -1 1093.27 32.70 5 5 0 163.80 9.75 5 5 1 7.01 2.22 5 5 2 1504.56 40.10 5 5 3 602.45 20.62 5 5 4 2515.54 60.55 -5 -5 -5 1.92 1.43 -5 -5 -6 8.97 2.43 -5 -5 -7 122.40 8.45 -5 -5 -8 342.26 15.49 -5 -5 -9 7.85 2.54 -5 -5 -10 229.66 13.06 -5 -5 -11 939.54 31.87 -5 -5 -11 934.27 27.37 -5 -5 -12 1659.83 46.10 -5 -5 -12 1577.09 40.45 -5 -5 -13 622.94 21.44 -5 -5 -13 598.00 19.07 -5 -5 -14 69.88 6.43 -5 -5 -14 67.40 5.44 -5 -5 -15 6.83 2.61 -5 -5 -15 6.42 2.10 -5 -5 -16 1.41 1.52 -5 -5 -16 6.14 1.92 -5 -5 -17 229.85 11.03 -5 -5 -17 229.11 9.93 -5 -5 -18 9.59 1.86 -5 -5 -19 49.91 3.39 -5 -6 10 100.24 5.47 -5 -6 10 105.02 5.57 -5 -6 9 420.70 15.01 -5 -6 9 392.08 14.29 -5 -6 8 528.91 19.32 -5 -6 8 531.97 18.56 -5 -6 7 147.24 9.87 -5 -6 7 147.67 9.11 -5 -6 6 126.93 9.49 -5 -6 6 127.70 8.64 -5 -6 5 629.00 23.50 -5 -6 5 618.55 21.73 -5 -6 4 933.52 30.53 -5 -6 4 953.53 28.58 -5 -6 3 762.21 26.20 -5 -6 3 794.89 23.87 -5 -6 2 26.20 4.03 5 6 -2 28.99 4.38 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11.37 -10 -9 -5 59.74 4.50 -10 -9 -5 69.20 4.66 -10 -9 -6 347.98 12.58 -10 -9 -7 6.50 1.84 -10 -9 -8 11.77 2.26 -10 -9 -9 115.80 6.98 -10 -9 -10 74.87 5.51 -10 -9 -11 76.27 5.21 -10 -9 -11 72.83 5.29 -10 -9 -12 58.34 4.11 -10 -9 -12 55.61 4.45 -10 -9 -13 160.61 7.48 -10 -9 -14 300.97 10.33 -10 -10 -6 53.84 3.64 -10 -10 -7 383.39 12.41 -10 -10 -8 69.15 4.64 -10 -10 -8 70.85 3.93 -10 -10 -9 1.58 1.18 -10 -10 -9 -1.89 1.02 -10 -10 -10 0.84 1.18 -10 -10 -10 2.23 1.03 -10 -10 -11 200.86 7.76 -10 -10 -11 193.96 7.55 -10 -10 -12 7.00 1.40 11 -5 -3 99.69 4.67 11 -5 -2 4.45 1.25 11 -5 -1 237.09 8.87 11 -5 0 267.80 9.80 11 -5 1 483.09 14.67 11 -5 2 4.36 1.38 11 -5 3 8.95 1.72 11 -5 4 194.50 7.78 11 -5 5 146.80 6.28 11 -5 6 44.81 3.01 11 -4 -4 12.14 2.53 11 -4 -3 533.21 15.76 11 -4 -2 33.32 3.33 11 -4 -1 142.93 7.35 11 -4 0 136.55 7.35 11 -4 1 12.24 2.35 11 -4 2 651.64 19.93 11 -4 3 87.78 5.85 11 -4 4 19.28 2.78 11 -4 5 25.44 3.06 11 -4 6 296.92 11.10 11 -4 7 1.39 1.16 11 -4 8 3.11 1.14 11 -4 9 246.90 8.06 11 -3 -5 378.28 11.65 11 -3 -4 9.36 1.83 11 -3 -3 18.53 2.67 11 -3 -2 232.37 10.21 11 -3 -1 655.65 20.58 11 -3 0 101.94 6.90 11 -3 1 19.76 3.14 11 -3 2 318.28 13.23 11 -3 3 307.33 12.97 11 -3 4 838.55 25.04 11 -3 5 8.36 2.20 11 -3 6 29.08 3.66 11 -3 7 147.46 7.98 11 -3 8 173.37 8.39 11 -3 9 31.83 3.18 11 -3 10 47.63 3.50 11 -3 11 123.81 5.16 11 -2 -5 144.18 6.47 11 -2 -4 395.85 13.25 11 -2 -3 272.58 11.16 11 -2 -2 18.88 2.98 11 -2 -1 14.36 2.84 11 -2 0 815.33 25.10 11 -2 1 127.12 8.23 11 -2 2 173.00 9.79 11 -2 3 357.20 14.97 11 -2 4 58.08 5.67 11 -2 5 1392.15 37.87 11 -2 6 362.54 14.91 11 -2 7 92.83 6.79 11 -2 8 36.17 4.17 11 -2 9 174.78 8.90 11 -2 10 23.59 2.98 11 -2 11 2.72 1.24 -11 2 -11 3.31 1.09 11 -2 12 159.21 6.44 11 -1 -5 110.53 5.39 11 -1 -4 372.19 12.67 -11 1 4 370.40 10.70 11 -1 -3 5.10 1.82 -11 1 3 4.59 1.27 11 -1 -2 882.60 25.70 11 -1 -1 100.48 7.05 11 -1 0 1.10 1.47 11 -1 1 149.77 9.19 11 -1 2 589.51 20.83 11 -1 3 53.07 5.58 11 -1 4 2.71 1.94 11 -1 5 698.31 23.55 11 -1 6 163.78 9.81 11 -1 7 1467.50 39.77 11 -1 8 11.76 2.82 11 -1 9 63.85 5.61 11 -1 10 50.27 4.74 11 -1 11 120.24 6.85 11 -1 12 0.23 0.95 -11 1 -12 0.91 0.96 -11 1 -13 43.08 2.73 11 0 -4 132.74 6.48 -11 0 4 133.46 6.09 11 0 -3 7.97 1.90 -11 0 3 9.46 1.89 11 0 -2 355.16 13.52 -11 0 2 338.22 12.26 11 0 -1 447.30 16.19 -11 0 1 417.35 14.37 11 0 0 704.43 22.63 -11 0 0 680.75 20.19 11 0 1 11.33 2.81 -11 0 -1 6.85 1.73 11 0 2 1.85 1.69 11 0 3 381.08 16.00 11 0 4 278.47 13.33 11 0 5 75.07 6.66 11 0 6 146.04 9.39 11 0 7 178.74 10.37 11 0 8 1076.97 31.60 11 0 9 503.98 18.63 11 0 10 30.17 3.98 11 0 11 12.19 2.57 11 0 12 125.67 6.95 11 0 13 40.79 3.44 -11 0 -13 43.06 3.27 -11 0 -14 -0.25 0.74 11 1 -4 552.73 14.83 -11 -1 4 568.72 16.22 11 1 -3 59.01 4.20 -11 -1 3 57.04 4.43 11 1 -2 120.24 6.87 -11 -1 2 117.01 6.79 11 1 -1 284.47 11.84 -11 -1 1 285.82 11.78 11 1 0 24.89 3.55 -11 -1 0 28.30 3.57 11 1 1 879.24 26.32 -11 -1 -1 850.34 24.79 11 1 2 190.19 10.31 -11 -1 -2 185.57 9.19 11 1 3 37.40 4.66 -11 -1 -3 33.96 3.75 11 1 4 38.53 4.70 -11 -1 -4 29.81 3.46 11 1 5 460.20 17.72 -11 -1 -5 439.31 14.70 11 1 6 -0.85 2.12 11 1 7 23.29 3.91 11 1 8 659.93 22.59 11 1 9 64.89 5.96 11 1 10 1073.36 30.85 11 1 11 49.29 4.81 11 1 12 2.41 1.60 11 1 13 31.96 3.22 -11 -1 -13 34.03 3.25 -11 -1 -14 226.05 8.15 -11 -2 4 158.72 6.91 -11 -2 3 167.48 7.90 -11 -2 2 594.32 18.85 11 2 -1 106.67 6.11 -11 -2 1 98.49 6.69 11 2 0 19.30 2.95 -11 -2 0 16.56 2.99 11 2 1 495.73 17.20 -11 -2 -1 494.03 17.80 11 2 2 157.08 8.87 -11 -2 -2 157.48 8.95 11 2 3 555.57 19.16 -11 -2 -3 546.47 18.74 11 2 4 132.46 8.34 -11 -2 -4 137.31 8.03 11 2 5 1.56 1.74 -11 -2 -5 1.78 1.42 11 2 6 384.13 15.39 -11 -2 -6 350.25 13.51 11 2 7 388.41 15.65 -11 -2 -7 376.01 13.67 11 2 8 112.22 7.73 -11 -2 -8 106.22 6.08 11 2 9 85.52 6.68 11 2 10 257.19 11.92 11 2 11 622.63 20.00 11 2 12 446.13 15.38 11 2 13 3.71 1.54 -11 -2 -14 2.68 1.18 -11 -2 -15 104.81 4.72 -11 -3 3 104.48 5.76 -11 -3 2 9.80 2.14 -11 -3 1 715.69 22.03 -11 -3 0 178.49 9.62 -11 -3 -1 303.25 13.37 -11 -3 -2 171.02 9.76 -11 -3 -3 139.64 8.74 -11 -3 -4 702.39 22.87 11 3 5 447.76 16.11 -11 -3 -5 427.66 16.49 11 3 6 -4.11 1.97 -11 -3 -6 0.36 1.35 11 3 7 56.66 5.20 -11 -3 -7 60.92 5.30 11 3 8 447.59 16.40 -11 -3 -8 423.48 15.24 11 3 9 58.85 5.34 -11 -3 -9 57.74 4.70 11 3 10 15.08 2.89 -11 -3 -10 19.63 2.62 11 3 11 410.54 14.52 -11 -3 -11 365.31 11.96 11 3 12 2.73 1.50 11 3 13 955.44 24.76 -11 -3 -14 78.65 4.73 -11 -3 -15 22.83 2.17 -11 -4 3 547.39 15.26 -11 -4 2 96.12 5.64 -11 -4 1 50.70 4.50 -11 -4 0 138.40 8.13 -11 -4 -1 876.36 26.41 -11 -4 -2 39.82 4.69 -11 -4 -3 26.64 4.10 -11 -4 -4 597.79 21.01 -11 -4 -5 191.58 10.54 -11 -4 -6 1015.18 29.90 -11 -4 -7 36.81 4.42 -11 -4 -8 27.21 3.64 -11 -4 -9 137.74 7.93 -11 -4 -10 384.81 13.97 -11 -4 -11 7.25 1.79 -11 -4 -12 29.97 2.96 -11 -4 -13 207.20 7.45 -11 -4 -14 451.87 13.54 -11 -4 -15 445.06 12.08 -11 -5 2 199.81 7.45 -11 -5 1 470.77 14.77 -11 -5 0 58.09 4.77 -11 -5 -1 35.31 4.01 -11 -5 -2 504.31 18.11 -11 -5 -3 341.24 14.51 -11 -5 -4 95.85 7.31 -11 -5 -5 236.06 11.94 -11 -5 -6 145.74 9.21 -11 -5 -7 870.48 26.88 -11 -5 -8 505.08 18.33 -11 -5 -9 2.81 1.65 -11 -5 -10 7.67 2.06 -11 -5 -11 210.87 9.51 -11 -5 -12 88.13 5.44 -11 -5 -13 1.93 1.21 -11 -5 -13 -2.35 1.16 -11 -5 -14 187.58 6.72 -11 -5 -14 186.23 6.64 -11 -6 0 495.40 14.87 -11 -6 -1 111.10 6.40 -11 -6 -2 105.80 6.73 -11 -6 -3 0.60 1.76 -11 -6 -4 640.25 21.13 -11 -6 -5 10.59 2.71 -11 -6 -6 6.03 2.32 -11 -6 -7 518.52 18.79 -11 -6 -8 6.51 2.43 -11 -6 -9 820.30 24.98 -11 -6 -10 91.93 6.44 -11 -6 -11 3.00 1.58 -11 -6 -12 10.46 2.07 -11 -6 -13 199.88 8.22 -11 -6 -14 4.51 1.25 -11 -7 -2 256.45 9.70 -11 -7 -3 63.74 4.74 -11 -7 -4 109.13 6.74 -11 -7 -5 174.42 9.04 -11 -7 -6 274.38 11.99 -11 -7 -7 69.62 5.77 -11 -7 -8 93.17 6.64 -11 -7 -9 347.70 13.74 -11 -7 -10 243.11 10.76 -11 -7 -11 280.05 11.29 -11 -7 -12 4.24 1.54 -11 -7 -13 11.24 1.97 -11 -7 -14 63.13 3.78 -11 -8 -4 120.26 5.07 -11 -8 -4 125.13 5.91 -11 -8 -5 71.82 4.72 -11 -8 -6 0.10 1.31 -11 -8 -7 405.78 14.04 -11 -8 -8 -0.33 1.51 -11 -8 -9 90.15 5.77 -11 -8 -10 344.39 12.42 -11 -8 -11 28.95 3.13 -11 -8 -12 404.46 11.70 -11 -8 -12 441.65 13.38 -11 -8 -13 30.92 2.77 -11 -9 -7 51.33 3.52 -11 -9 -8 88.37 4.91 -11 -9 -8 86.11 4.58 -11 -9 -9 233.44 8.65 -11 -9 -9 219.21 8.17 -11 -9 -10 39.13 3.12 -11 -9 -10 45.00 3.22 12 -4 2 200.27 7.32 12 -4 3 33.90 2.73 12 -4 4 29.95 2.48 12 -3 -1 16.99 2.00 12 -3 0 56.46 3.83 12 -3 1 244.42 9.18 12 -3 2 82.53 5.04 12 -3 3 654.82 18.51 12 -3 4 7.18 1.68 12 -3 5 2.42 1.10 12 -3 6 81.09 4.72 12 -3 7 311.11 10.22 12 -3 8 1.98 0.80 12 -2 -1 391.73 12.38 12 -2 0 259.44 9.86 12 -2 1 166.07 7.83 12 -2 2 29.47 3.30 12 -2 3 112.68 6.59 12 -2 4 533.07 16.95 12 -2 5 285.39 11.18 12 -2 6 12.67 2.32 12 -2 7 29.25 3.08 12 -2 8 244.75 9.26 12 -2 9 75.25 4.36 12 -1 -1 33.52 3.10 12 -1 0 36.86 3.51 12 -1 1 664.48 19.61 12 -1 2 1.53 1.42 12 -1 3 76.72 5.59 12 -1 4 405.00 14.61 12 -1 5 16.98 2.92 12 -1 6 940.22 26.22 12 -1 7 70.21 5.22 12 -1 8 22.76 2.93 12 -1 9 96.24 5.55 12 -1 10 238.36 8.79 12 -1 11 1.80 0.95 12 0 -1 403.84 12.50 12 0 0 49.76 4.00 12 0 1 17.54 2.67 12 0 2 226.44 9.95 12 0 3 265.24 11.26 12 0 4 114.53 7.09 12 0 5 92.86 6.40 12 0 6 353.68 13.68 12 0 7 634.10 19.81 12 0 8 511.71 16.83 12 0 9 12.67 2.25 12 0 10 17.87 2.45 12 0 11 102.85 5.28 12 1 0 543.81 15.24 -12 -1 0 519.49 14.31 12 1 1 163.35 7.56 -12 -1 -1 154.84 6.41 12 1 2 3.24 1.46 -12 -1 -2 2.40 1.04 12 1 3 1.46 1.39 12 1 4 402.15 14.44 12 1 5 11.06 2.37 12 1 6 53.82 4.76 12 1 7 419.94 14.92 12 1 8 9.49 2.31 12 1 9 938.57 25.57 12 1 10 65.88 4.69 12 1 11 9.07 1.73 12 1 12 12.02 1.68 -12 -2 1 25.35 2.31 -12 -2 0 232.55 8.62 -12 -2 -1 53.17 3.95 12 2 2 539.75 15.66 -12 -2 -2 555.77 16.38 12 2 3 23.84 2.81 -12 -2 -3 19.04 2.55 12 2 4 6.77 1.76 -12 -2 -4 6.30 1.57 12 2 5 117.95 6.72 -12 -2 -5 118.84 5.95 12 2 6 281.64 11.31 -12 -2 -6 273.36 9.50 12 2 7 11.41 2.29 12 2 8 2.08 1.60 12 2 9 232.25 9.73 12 2 10 291.28 10.74 12 2 11 504.19 14.69 12 2 12 4.36 1.16 -12 -2 -13 2.08 0.84 -12 -3 0 77.09 4.51 -12 -3 -1 8.93 1.75 -12 -3 -2 120.76 6.45 -12 -3 -3 477.14 15.34 -12 -3 -4 279.47 10.83 -12 -3 -5 23.75 2.92 -12 -3 -6 9.99 2.02 -12 -3 -7 425.37 13.53 -12 -3 -8 175.11 7.19 12 3 10 105.31 5.19 -12 -3 -13 147.64 5.70 -12 -4 -1 19.15 2.43 -12 -4 -2 88.40 5.38 -12 -4 -3 318.97 11.74 -12 -4 -4 14.52 2.47 -12 -4 -5 626.16 18.94 -12 -4 -6 147.92 7.52 -12 -4 -7 15.33 2.35 -12 -4 -8 113.91 6.10 -12 -4 -9 554.37 16.01 -12 -4 -10 1.68 1.08 -12 -4 -11 -0.86 0.72 -12 -5 -2 414.20 12.99 -12 -5 -3 134.04 6.68 -12 -5 -4 44.14 3.90 -12 -5 -5 339.35 12.35 -12 -5 -6 251.93 10.24 -12 -5 -7 534.71 16.62 -12 -5 -8 52.86 4.14 -12 -5 -9 1.34 1.10 -12 -5 -10 242.24 8.93 -12 -5 -11 119.96 5.23 -12 -6 -3 556.03 15.45 -12 -6 -4 4.20 1.47 -12 -6 -5 50.87 3.97 -12 -6 -6 377.76 12.81 -12 -6 -7 20.82 2.70 -12 -6 -8 478.40 14.85 -12 -6 -9 79.06 4.87 -12 -6 -10 21.66 2.44 -12 -6 -11 1.72 0.91 -12 -7 -6 56.84 3.79 -12 -7 -7 18.62 2.31 -12 -7 -8 348.43 11.32 -12 -7 -9 154.48 6.63 -12 -7 -10 312.31 9.99 TITL wai252_173K in P-1 REM P-1 (#2 in standard setting) CELL 1.54184 10.610385 12.025208 16.622725 69.2778 72.8670 83.9022 ZERR 8.00 0.000424 0.000459 0.000752 0.0038 0.0038 0.0032 LATT 1 SFAC C H N O UNIT 88.00 80.00 8.00 8.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 14446 _olex2_date_sample_data_collection 2020-04-16 _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 1.384 _oxdiff_exptl_absorpt_empirical_full_min 0.752 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' 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 Hg1 Hg 0.17530(2) 0.63594(2) 0.23707(2) 0.02569(6) Uani 1 1 d . . . . . Ir1 Ir 0.29666(2) 0.47165(2) 0.33609(2) 0.01720(6) Uani 1 1 d . . . . . Ir2 Ir 0.09430(2) 0.81612(2) 0.11432(2) 0.02269(6) Uani 1 1 d D . . . . Cl1 Cl -0.06906(12) 0.81798(14) 0.24343(9) 0.0452(3) Uani 1 1 d . . . . . Cl2 Cl -0.0152(3) 0.6851(4) 0.0905(3) 0.0470(8) Uani 0.5 1 d D . P A 1 Cl2A Cl -0.0103(3) 0.6379(3) 0.1273(3) 0.0408(8) Uani 0.5 1 d D . P A 2 N1 N 0.4511(3) 0.4772(3) 0.2266(2) 0.0202(7) Uani 1 1 d . . . . . C1 C 0.4060(4) 0.6211(4) 0.3181(3) 0.0216(8) Uani 1 1 d . . . . . C2 C 0.3702(4) 0.7168(4) 0.3506(3) 0.0252(9) Uani 1 1 d . . . . . H2 H 0.2848 0.7167 0.3902 0.030 Uiso 1 1 calc R . . . . C3 C 0.4530(5) 0.8107(4) 0.3279(3) 0.0256(9) Uani 1 1 d D . . . . C4 C 0.5827(5) 0.8064(4) 0.2756(3) 0.0252(9) Uani 1 1 d . . . . . H4 H 0.6440 0.8658 0.2647 0.030 Uiso 1 1 calc R . . . . C5 C 0.6225(4) 0.7164(4) 0.2397(3) 0.0234(8) Uani 1 1 d . . . . . H5 H 0.7100 0.7149 0.2032 0.028 Uiso 1 1 calc R . . . . C6 C 0.5325(4) 0.6277(3) 0.2575(3) 0.0204(8) Uani 1 1 d . . . . . C7 C 0.5568(4) 0.5464(4) 0.2065(3) 0.0216(8) Uani 1 1 d . . . . . C8 C 0.6670(4) 0.5436(4) 0.1369(3) 0.0275(9) Uani 1 1 d . . . . . H8 H 0.7424 0.5899 0.1236 0.033 Uiso 1 1 calc R . . . . C9 C 0.6662(5) 0.4728(5) 0.0868(3) 0.0350(11) Uani 1 1 d . . . . . H9 H 0.7420 0.4687 0.0401 0.042 Uiso 1 1 calc R . . . . C10 C 0.5543(5) 0.4079(5) 0.1051(3) 0.0335(10) Uani 1 1 d . . . . . H10 H 0.5521 0.3615 0.0697 0.040 Uiso 1 1 calc R . . . . C11 C 0.4453(4) 0.4113(4) 0.1757(3) 0.0243(9) Uani 1 1 d . . . . . C12 C 0.3173(4) 0.3563(4) 0.2013(3) 0.0246(9) Uani 1 1 d . . . . . C13 C 0.2839(5) 0.2978(5) 0.1508(3) 0.0344(11) Uani 1 1 d . . . . . H13 H 0.3487 0.2868 0.1008 0.041 Uiso 1 1 calc R . . . . C14 C 0.1577(5) 0.2562(5) 0.1733(4) 0.0383(11) Uani 1 1 d . . . . . H14 H 0.1365 0.2171 0.1384 0.046 Uiso 1 1 calc R . . . . C15 C 0.0604(5) 0.2706(4) 0.2466(3) 0.0304(10) Uani 1 1 d . . . . . C16 C 0.0962(4) 0.3268(4) 0.2968(3) 0.0263(9) Uani 1 1 d . . . . . H16 H 0.0312 0.3352 0.3477 0.032 Uiso 1 1 calc R . . . . C17 C 0.2223(4) 0.3718(4) 0.2767(3) 0.0219(8) Uani 1 1 d . . . . . C18 C 0.3972(10) 0.9207(8) 0.3561(7) 0.023(3) Uani 0.65 1 d D U P B 1 C18A C 0.4241(18) 0.9162(15) 0.3636(12) 0.023(5) Uani 0.35 1 d D U P B 2 C19 C 0.4748(10) 0.9282(8) 0.4181(7) 0.045(2) Uani 0.65 1 d D . P B 1 H19A H 0.4607 0.8555 0.4707 0.068 Uiso 0.65 1 calc GR . P B 1 H19B H 0.4445 0.9971 0.4372 0.068 Uiso 0.65 1 calc GR . P B 1 H19C H 0.5689 0.9367 0.3862 0.068 Uiso 0.65 1 calc GR . P B 1 C19A C 0.379(2) 0.8707(17) 0.4667(12) 0.059(5) Uani 0.35 1 d D U P B 2 H19D H 0.3174 0.8045 0.4880 0.088 Uiso 0.35 1 calc GR . P B 2 H19E H 0.3349 0.9352 0.4877 0.088 Uiso 0.35 1 calc GR . P B 2 H19F H 0.4558 0.8436 0.4899 0.088 Uiso 0.35 1 calc GR . P B 2 C20 C 0.2510(8) 0.9132(7) 0.4040(7) 0.047(2) Uani 0.65 1 d D . P B 1 H20A H 0.2014 0.9056 0.3649 0.070 Uiso 0.65 1 calc GR . P B 1 H20B H 0.2229 0.9855 0.4190 0.070 Uiso 0.65 1 calc GR . P B 1 H20C H 0.2341 0.8438 0.4590 0.070 Uiso 0.65 1 calc GR . P B 1 C20A C 0.304(2) 0.976(2) 0.3313(17) 0.071(6) Uani 0.35 1 d D U P B 2 H20D H 0.3314 1.0134 0.2660 0.107 Uiso 0.35 1 calc GR . P B 2 H20E H 0.2684 1.0367 0.3588 0.107 Uiso 0.35 1 calc GR . P B 2 H20F H 0.2366 0.9161 0.3484 0.107 Uiso 0.35 1 calc GR . P B 2 C21 C 0.4204(10) 1.0324(6) 0.2741(6) 0.043(2) Uani 0.65 1 d D . P B 1 H21A H 0.5152 1.0428 0.2447 0.065 Uiso 0.65 1 calc GR . P B 1 H21B H 0.3855 1.1014 0.2922 0.065 Uiso 0.65 1 calc GR . P B 1 H21C H 0.3755 1.0254 0.2324 0.065 Uiso 0.65 1 calc GR . P B 1 C21A C 0.536(2) 1.0051(17) 0.3353(16) 0.067(5) Uani 0.35 1 d D U P B 2 H21D H 0.6113 0.9635 0.3558 0.101 Uiso 0.35 1 calc GR . P B 2 H21E H 0.5051 1.0672 0.3621 0.101 Uiso 0.35 1 calc GR . P B 2 H21F H 0.5629 1.0414 0.2700 0.101 Uiso 0.35 1 calc GR . P B 2 C22 C -0.0800(5) 0.2241(5) 0.2738(4) 0.0401(12) Uani 1 1 d . . . . . C23 C -0.0895(7) 0.0998(6) 0.3444(5) 0.0589(17) Uani 1 1 d . . . . . H23A H -0.0342 0.0445 0.3175 0.088 Uiso 1 1 calc GR . . . . H23B H -0.1814 0.0729 0.3670 0.088 Uiso 1 1 calc GR . . . . H23C H -0.0591 0.1023 0.3940 0.088 Uiso 1 1 calc GR . . . . C24 C -0.1183(7) 0.2180(9) 0.1933(5) 0.080(3) Uani 1 1 d . . . . . H24A H -0.1037 0.2957 0.1456 0.120 Uiso 1 1 calc GR . . . . H24B H -0.2115 0.1965 0.2116 0.120 Uiso 1 1 calc GR . . . . H24C H -0.0640 0.1580 0.1714 0.120 Uiso 1 1 calc GR . . . . C25 C -0.1815(6) 0.3054(6) 0.3139(6) 0.0607(19) Uani 1 1 d . . . . . H25A H -0.1686 0.3017 0.3708 0.091 Uiso 1 1 calc GR . . . . H25B H -0.2708 0.2787 0.3242 0.091 Uiso 1 1 calc GR . . . . H25C H -0.1695 0.3874 0.2722 0.091 Uiso 1 1 calc GR . . . . C31 C 0.4139(5) 0.3756(4) 0.4301(3) 0.0243(9) Uani 1 1 d . . . . . H31 H 0.5113 0.3869 0.4041 0.029 Uiso 1 1 calc R . . . . C32 C 0.3595(5) 0.2931(4) 0.4055(3) 0.0243(9) Uani 1 1 d . . . . . H32 H 0.4260 0.2563 0.3655 0.029 Uiso 1 1 calc R . . . . C33 C 0.2432(5) 0.2143(4) 0.4660(3) 0.0303(10) Uani 1 1 d . . . . . H33A H 0.2706 0.1535 0.5162 0.036 Uiso 1 1 calc R . . . . H33B H 0.2169 0.1722 0.4319 0.036 Uiso 1 1 calc R . . . . C34 C 0.1231(5) 0.2821(4) 0.5044(3) 0.0329(11) Uani 1 1 d . . . . . H34A H 0.0417 0.2421 0.5114 0.040 Uiso 1 1 calc R . . . . H34B H 0.1246 0.2781 0.5646 0.040 Uiso 1 1 calc R . . . . C35 C 0.1184(4) 0.4126(4) 0.4461(3) 0.0274(9) Uani 1 1 d . . . . . H35 H 0.0345 0.4368 0.4285 0.033 Uiso 1 1 calc R . . . . C36 C 0.1788(5) 0.5042(4) 0.4567(3) 0.0283(10) Uani 1 1 d . . . . . H36 H 0.1296 0.5813 0.4452 0.034 Uiso 1 1 calc R . . . . C37 C 0.2539(5) 0.4820(4) 0.5255(3) 0.0339(11) Uani 1 1 d . . . . . H37A H 0.1908 0.4573 0.5859 0.041 Uiso 1 1 calc R . . . . H37B H 0.2951 0.5573 0.5161 0.041 Uiso 1 1 calc R . . . . C38 C 0.3614(5) 0.3866(4) 0.5219(3) 0.0325(10) Uani 1 1 d . . . . . H38A H 0.4351 0.4063 0.5396 0.039 Uiso 1 1 calc R . . . . H38B H 0.3250 0.3090 0.5656 0.039 Uiso 1 1 calc R . . . . C41 C 0.2265(5) 0.9127(4) 0.1400(3) 0.0300(9) Uani 1 1 d . U . . . H41 H 0.2064 0.8950 0.2060 0.036 Uiso 0.5 1 calc R . P A 1 H41A H 0.1995 0.9272 0.1984 0.036 Uiso 0.5 1 calc R . P A 2 C42 C 0.1440(10) 0.9914(9) 0.1088(7) 0.0306(18) Uani 0.5 1 d D U P A 1 H42 H 0.0808 1.0228 0.1537 0.037 Uiso 0.5 1 calc R . P A 1 C42A C 0.1622(11) 0.9879(10) 0.0678(8) 0.0349(19) Uani 0.5 1 d . U P A 2 H42A H 0.0943 1.0440 0.0879 0.042 Uiso 0.5 1 calc R . P A 2 C43 C 0.1794(11) 1.0787(9) 0.0128(6) 0.0403(19) Uani 0.5 1 d D U P A 1 H43A H 0.2393 1.1402 0.0076 0.048 Uiso 0.5 1 calc R . P A 1 H43B H 0.0982 1.1189 -0.0011 0.048 Uiso 0.5 1 calc R . P A 1 C43A C 0.2313(16) 1.0353(12) -0.0327(9) 0.042(2) Uani 0.5 1 d . U P A 2 H43C H 0.1899 1.1114 -0.0607 0.051 Uiso 0.5 1 calc R . P A 2 H43D H 0.3251 1.0510 -0.0419 0.051 Uiso 0.5 1 calc R . P A 2 C44 C 0.2462(12) 1.0170(10) -0.0551(7) 0.033(2) Uani 0.5 1 d D U P A 1 H44A H 0.2275 1.0623 -0.1130 0.040 Uiso 0.5 1 calc R . P A 1 H44B H 0.3428 1.0167 -0.0648 0.040 Uiso 0.5 1 calc R . P A 1 C44A C 0.2227(12) 0.9476(10) -0.0777(7) 0.041(2) Uani 0.5 1 d . U P A 2 H44C H 0.1494 0.9719 -0.1059 0.050 Uiso 0.5 1 calc R . P A 2 H44D H 0.3053 0.9522 -0.1261 0.050 Uiso 0.5 1 calc R . P A 2 C45 C 0.1993(9) 0.8923(10) -0.0244(7) 0.0317(17) Uani 0.5 1 d D U P A 1 H45 H 0.1577 0.8764 -0.0659 0.038 Uiso 0.5 1 calc R . P A 1 C45A C 0.2020(10) 0.8233(10) -0.0177(6) 0.0302(17) Uani 0.5 1 d . U P A 2 H45A H 0.1630 0.7730 -0.0411 0.036 Uiso 0.5 1 calc R . P A 2 C46 C 0.2682(11) 0.7930(11) 0.0206(7) 0.0275(17) Uani 0.5 1 d . U P A 1 H46 H 0.2688 0.7210 0.0035 0.033 Uiso 0.5 1 calc R . P A 1 C46A C 0.2814(11) 0.7571(10) 0.0400(7) 0.0263(17) Uani 0.5 1 d . U P A 2 H46A H 0.2879 0.6699 0.0501 0.032 Uiso 0.5 1 calc R . P A 2 C47 C 0.3952(5) 0.8090(5) 0.0451(3) 0.0334(9) Uani 1 1 d . U . . . H47A H 0.4267 0.7299 0.0773 0.040 Uiso 0.5 1 calc R . P A 1 H47B H 0.4654 0.8452 -0.0107 0.040 Uiso 0.5 1 calc R . P A 1 H47C H 0.4435 0.8571 -0.0165 0.040 Uiso 0.5 1 calc R . P A 2 H47D H 0.4544 0.7432 0.0673 0.040 Uiso 0.5 1 calc R . P A 2 C48 C 0.3706(5) 0.8866(5) 0.1031(4) 0.0359(10) Uani 1 1 d . U . . . H48A H 0.4090 0.8470 0.1538 0.043 Uiso 1 1 calc R . . . . H48B H 0.4175 0.9630 0.0672 0.043 Uiso 1 1 calc R . . . . 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 Hg1 0.01883(9) 0.02019(9) 0.03033(10) -0.00019(7) -0.00609(7) 0.00077(6) Ir1 0.01459(9) 0.01512(9) 0.01626(9) -0.00285(6) 0.00094(6) -0.00013(6) Ir2 0.01405(9) 0.03655(11) 0.01380(9) -0.00210(7) -0.00526(7) -0.00336(7) Cl1 0.0219(6) 0.0769(9) 0.0338(6) -0.0235(6) 0.0017(5) 0.0020(6) Cl2 0.0307(15) 0.066(2) 0.054(2) -0.0296(18) -0.0068(15) -0.0190(17) Cl2A 0.0369(15) 0.0319(15) 0.057(2) -0.0049(13) -0.0255(16) -0.0127(12) N1 0.0160(16) 0.0217(16) 0.0177(16) -0.0051(13) 0.0007(13) 0.0007(13) C1 0.019(2) 0.0182(18) 0.022(2) -0.0028(16) -0.0040(16) 0.0017(15) C2 0.025(2) 0.0201(19) 0.024(2) -0.0064(17) -0.0003(17) 0.0019(17) C3 0.033(2) 0.0192(19) 0.021(2) -0.0042(17) -0.0056(18) 0.0013(17) C4 0.030(2) 0.0187(19) 0.023(2) 0.0001(16) -0.0077(18) -0.0078(17) C5 0.018(2) 0.026(2) 0.022(2) -0.0035(17) -0.0024(16) -0.0043(16) C6 0.019(2) 0.0184(18) 0.0186(19) -0.0021(15) -0.0020(15) -0.0017(15) C7 0.017(2) 0.0218(19) 0.022(2) -0.0048(16) -0.0034(16) 0.0008(16) C8 0.018(2) 0.033(2) 0.028(2) -0.0097(19) 0.0000(17) -0.0024(17) C9 0.023(2) 0.048(3) 0.029(2) -0.019(2) 0.0067(19) 0.001(2) C10 0.028(2) 0.045(3) 0.031(2) -0.021(2) -0.001(2) -0.003(2) C11 0.023(2) 0.027(2) 0.023(2) -0.0119(17) -0.0019(17) -0.0004(17) C12 0.023(2) 0.026(2) 0.024(2) -0.0097(18) -0.0037(17) -0.0022(17) C13 0.031(3) 0.044(3) 0.030(2) -0.018(2) 0.000(2) -0.009(2) C14 0.035(3) 0.047(3) 0.039(3) -0.021(2) -0.009(2) -0.010(2) C15 0.026(2) 0.030(2) 0.031(2) -0.0033(19) -0.0100(19) -0.0042(18) C16 0.021(2) 0.027(2) 0.025(2) -0.0046(18) -0.0030(17) -0.0032(17) C17 0.019(2) 0.0218(19) 0.021(2) -0.0039(16) -0.0044(16) 0.0005(16) C18 0.027(5) 0.017(4) 0.029(5) -0.007(3) -0.015(4) 0.002(3) C18A 0.023(8) 0.028(8) 0.021(7) -0.008(6) -0.012(6) 0.002(5) C19 0.068(6) 0.036(4) 0.054(6) -0.027(4) -0.040(5) 0.014(4) C19A 0.070(9) 0.054(8) 0.049(8) -0.020(6) -0.014(7) 0.015(7) C20 0.035(5) 0.032(4) 0.076(7) -0.037(4) 0.001(4) 0.003(3) C20A 0.081(10) 0.067(9) 0.078(10) -0.036(8) -0.029(8) 0.009(8) C21 0.070(6) 0.018(3) 0.041(5) -0.009(3) -0.017(4) 0.002(4) C21A 0.073(9) 0.050(8) 0.083(10) -0.041(7) -0.001(7) -0.011(7) C22 0.028(3) 0.047(3) 0.049(3) -0.015(3) -0.016(2) -0.006(2) C23 0.044(4) 0.049(3) 0.075(5) -0.009(3) -0.013(3) -0.016(3) C24 0.036(4) 0.150(8) 0.067(5) -0.041(5) -0.023(3) -0.017(4) C25 0.023(3) 0.066(4) 0.099(6) -0.034(4) -0.017(3) -0.003(3) C31 0.028(2) 0.0206(19) 0.021(2) -0.0008(16) -0.0105(17) 0.0046(17) C32 0.029(2) 0.0172(18) 0.022(2) -0.0010(16) -0.0098(18) 0.0042(17) C33 0.039(3) 0.0177(19) 0.027(2) 0.0011(17) -0.008(2) -0.0042(18) C34 0.037(3) 0.028(2) 0.025(2) -0.0041(19) 0.0048(19) -0.015(2) C35 0.021(2) 0.029(2) 0.022(2) -0.0055(18) 0.0067(17) -0.0073(17) C36 0.025(2) 0.024(2) 0.025(2) -0.0080(18) 0.0094(18) -0.0041(17) C37 0.044(3) 0.033(2) 0.020(2) -0.0110(19) 0.004(2) -0.007(2) C38 0.041(3) 0.031(2) 0.025(2) -0.0062(19) -0.011(2) -0.004(2) C41 0.0306(17) 0.0262(17) 0.0297(18) -0.0045(14) -0.0077(14) -0.0047(13) C42 0.027(2) 0.029(3) 0.024(3) 0.003(2) -0.001(2) -0.005(2) C42A 0.031(3) 0.034(4) 0.031(3) 0.000(2) -0.009(2) -0.004(2) C43 0.037(5) 0.039(3) 0.026(3) 0.006(2) -0.001(2) -0.003(2) C43A 0.042(6) 0.043(3) 0.032(3) 0.000(2) -0.008(3) -0.004(3) C44 0.020(4) 0.041(3) 0.024(3) 0.005(2) -0.001(3) -0.006(2) C44A 0.044(5) 0.041(3) 0.027(3) 0.004(3) -0.009(3) -0.002(3) C45 0.021(3) 0.041(3) 0.018(3) 0.006(2) 0.000(3) -0.006(2) C45A 0.028(3) 0.040(3) 0.014(3) -0.001(3) -0.004(3) 0.000(2) C46 0.023(3) 0.039(3) 0.012(4) -0.001(2) 0.000(3) -0.004(2) C46A 0.025(3) 0.036(3) 0.011(3) -0.001(2) -0.001(2) -0.002(2) C47 0.0263(17) 0.041(2) 0.030(2) -0.0086(17) -0.0084(14) 0.0008(15) C48 0.0299(17) 0.045(2) 0.034(2) -0.0125(19) -0.0119(15) 0.0008(14) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hg Hg -4.2923 7.6849 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -4.7710 6.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Hg1 Ir2 169.439(9) . . ? N1 Ir1 Hg1 90.67(10) . . ? N1 Ir1 C1 77.30(15) . . ? N1 Ir1 C17 77.99(15) . . ? N1 Ir1 C31 92.65(15) . . ? N1 Ir1 C32 88.86(15) . . ? N1 Ir1 C35 160.94(16) . . ? N1 Ir1 C36 160.32(17) . . ? C1 Ir1 Hg1 81.20(11) . . ? C1 Ir1 C17 148.08(16) . . ? C1 Ir1 C31 83.44(16) . . ? C1 Ir1 C32 119.22(16) . . ? C1 Ir1 C35 121.70(17) . . ? C1 Ir1 C36 83.89(17) . . ? C17 Ir1 Hg1 79.19(11) . . ? C17 Ir1 C31 117.65(16) . . ? C17 Ir1 C32 80.04(16) . . ? C17 Ir1 C35 84.61(17) . . ? C17 Ir1 C36 121.66(17) . . ? C31 Ir1 Hg1 163.16(11) . . ? C32 Ir1 Hg1 158.85(12) . . ? C32 Ir1 C31 37.84(16) . . ? C35 Ir1 Hg1 93.67(13) . . ? C35 Ir1 C31 88.54(18) . . ? C35 Ir1 C32 80.45(17) . . ? C36 Ir1 Hg1 92.16(13) . . ? C36 Ir1 C31 79.34(18) . . ? C36 Ir1 C32 95.36(17) . . ? C36 Ir1 C35 38.03(17) . . ? Cl1 Ir2 Hg1 79.68(4) . . ? Cl1 Ir2 Cl2A 87.05(11) . . ? Cl2 Ir2 Hg1 89.05(12) . . ? Cl2 Ir2 Cl1 93.44(10) . . ? Cl2A Ir2 Hg1 73.27(8) . . ? C41 Ir2 Hg1 81.85(12) . . ? C41 Ir2 Cl1 91.67(14) . . ? C41 Ir2 Cl2 168.61(17) . . ? C41 Ir2 Cl2A 154.92(15) . . ? C41 Ir2 C42 34.8(3) . . ? C41 Ir2 C45 86.3(3) . . ? C41 Ir2 C46A 81.5(3) . . ? C42 Ir2 Hg1 113.7(3) . . ? C42 Ir2 Cl1 84.1(3) . . ? C42 Ir2 Cl2 156.1(3) . . ? C42A Ir2 Hg1 124.2(3) . . ? C42A Ir2 Cl1 99.9(4) . . ? C42A Ir2 Cl2A 161.9(3) . . ? C42A Ir2 C41 42.4(3) . . ? C42A Ir2 C45A 82.1(5) . . ? C42A Ir2 C46A 91.5(4) . . ? C45 Ir2 Hg1 126.3(3) . . ? C45 Ir2 Cl1 153.1(3) . . ? C45 Ir2 Cl2 93.7(3) . . ? C45 Ir2 C42 79.0(4) . . ? C45A Ir2 Hg1 111.3(3) . . ? C45A Ir2 Cl1 165.4(3) . . ? C45A Ir2 Cl2A 87.1(3) . . ? C45A Ir2 C41 99.3(3) . . ? C45A Ir2 C46A 38.6(4) . . ? C46 Ir2 Hg1 87.3(3) . . ? C46 Ir2 Cl1 165.9(3) . . ? C46 Ir2 Cl2 91.6(3) . . ? C46 Ir2 C41 81.1(3) . . ? C46 Ir2 C42 96.5(4) . . ? C46 Ir2 C45 39.1(4) . . ? C46A Ir2 Hg1 75.0(3) . . ? C46A Ir2 Cl1 154.5(3) . . ? C46A Ir2 Cl2A 89.0(3) . . ? C7 N1 Ir1 119.0(3) . . ? C7 N1 C11 121.8(4) . . ? C11 N1 Ir1 119.2(3) . . ? C2 C1 Ir1 131.2(3) . . ? C2 C1 C6 115.9(4) . . ? C6 C1 Ir1 112.7(3) . . ? C1 C2 H2 118.3 . . ? C3 C2 C1 123.3(4) . . ? C3 C2 H2 118.3 . . ? C2 C3 C4 118.4(4) . . ? C2 C3 C18 119.1(5) . . ? C2 C3 C18A 126.7(8) . . ? C4 C3 C18 122.3(5) . . ? C4 C3 C18A 114.5(8) . . ? C3 C4 H4 119.7 . . ? C5 C4 C3 120.6(4) . . ? C5 C4 H4 119.7 . . ? C4 C5 H5 120.3 . . ? C4 C5 C6 119.5(4) . . ? C6 C5 H5 120.3 . . ? C1 C6 C7 115.7(4) . . ? C5 C6 C1 121.6(4) . . ? C5 C6 C7 122.2(4) . . ? N1 C7 C6 113.0(4) . . ? N1 C7 C8 119.7(4) . . ? C8 C7 C6 127.0(4) . . ? C7 C8 H8 120.2 . . ? C9 C8 C7 119.6(4) . . ? C9 C8 H8 120.2 . . ? C8 C9 H9 120.1 . . ? C10 C9 C8 119.8(4) . . ? C10 C9 H9 120.1 . . ? C9 C10 H10 120.2 . . ? C9 C10 C11 119.7(4) . . ? C11 C10 H10 120.2 . . ? N1 C11 C10 119.3(4) . . ? N1 C11 C12 113.0(4) . . ? C10 C11 C12 127.6(4) . . ? C13 C12 C11 122.5(4) . . ? C13 C12 C17 120.4(4) . . ? C17 C12 C11 116.8(4) . . ? C12 C13 H13 119.8 . . ? C14 C13 C12 120.3(5) . . ? C14 C13 H13 119.8 . . ? C13 C14 H14 119.4 . . ? C13 C14 C15 121.2(5) . . ? C15 C14 H14 119.4 . . ? C14 C15 C22 122.4(5) . . ? C16 C15 C14 117.5(4) . . ? C16 C15 C22 120.0(5) . . ? C15 C16 H16 118.1 . . ? C15 C16 C17 123.7(4) . . ? C17 C16 H16 118.1 . . ? C12 C17 Ir1 112.4(3) . . ? C16 C17 Ir1 130.8(3) . . ? C16 C17 C12 116.7(4) . . ? C19 C18 C3 106.0(7) . . ? C20 C18 C3 114.1(7) . . ? C20 C18 C19 109.5(8) . . ? C21 C18 C3 109.8(7) . . ? C21 C18 C19 109.4(8) . . ? C21 C18 C20 107.9(8) . . ? C19A C18A C3 110.6(13) . . ? C20A C18A C3 102.7(13) . . ? C20A C18A C19A 107.1(17) . . ? C20A C18A C21A 111.8(17) . . ? C21A C18A C3 117.6(13) . . ? C21A C18A C19A 106.7(16) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19B 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18A C19A H19D 109.5 . . ? C18A C19A H19E 109.5 . . ? C18A C19A H19F 109.5 . . ? H19D C19A H19E 109.5 . . ? H19D C19A H19F 109.5 . . ? H19E C19A H19F 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20B 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18A C20A H20D 109.5 . . ? C18A C20A H20E 109.5 . . ? C18A C20A H20F 109.5 . . ? H20D C20A H20E 109.5 . . ? H20D C20A H20F 109.5 . . ? H20E C20A H20F 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21B 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C18A C21A H21D 109.5 . . ? C18A C21A H21E 109.5 . . ? C18A C21A H21F 109.5 . . ? H21D C21A H21E 109.5 . . ? H21D C21A H21F 109.5 . . ? H21E C21A H21F 109.5 . . ? C15 C22 C23 109.0(4) . . ? C15 C22 C24 111.5(5) . . ? C15 C22 C25 111.4(4) . . ? C23 C22 C24 109.3(6) . . ? C23 C22 C25 108.5(6) . . ? C24 C22 C25 107.1(6) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23B 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C22 C25 H25A 109.5 . . ? C22 C25 H25B 109.5 . . ? C22 C25 H25C 109.5 . . ? H25A C25 H25B 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Ir1 C31 H31 114.4 . . ? C32 C31 Ir1 70.2(2) . . ? C32 C31 H31 114.4 . . ? C32 C31 C38 121.7(4) . . ? C38 C31 Ir1 114.4(3) . . ? C38 C31 H31 114.4 . . ? Ir1 C32 H32 114.1 . . ? C31 C32 Ir1 72.0(2) . . ? C31 C32 H32 114.1 . . ? C31 C32 C33 123.6(4) . . ? C33 C32 Ir1 111.6(3) . . ? C33 C32 H32 114.1 . . ? C32 C33 H33A 108.8 . . ? C32 C33 H33B 108.8 . . ? C32 C33 C34 113.6(4) . . ? H33A C33 H33B 107.7 . . ? C34 C33 H33A 108.8 . . ? C34 C33 H33B 108.8 . . ? C33 C34 H34A 108.9 . . ? C33 C34 H34B 108.9 . . ? H34A C34 H34B 107.7 . . ? C35 C34 C33 113.4(4) . . ? C35 C34 H34A 108.9 . . ? C35 C34 H34B 108.9 . . ? Ir1 C35 H35 114.3 . . ? C34 C35 Ir1 113.5(3) . . ? C34 C35 H35 114.3 . . ? C36 C35 Ir1 70.6(2) . . ? C36 C35 C34 122.4(5) . . ? C36 C35 H35 114.3 . . ? Ir1 C36 H36 114.0 . . ? C35 C36 Ir1 71.4(2) . . ? C35 C36 H36 114.0 . . ? C35 C36 C37 123.4(4) . . ? C37 C36 Ir1 112.9(3) . . ? C37 C36 H36 114.0 . . ? C36 C37 H37A 108.9 . . ? C36 C37 H37B 108.9 . . ? C36 C37 C38 113.6(4) . . ? H37A C37 H37B 107.7 . . ? C38 C37 H37A 108.9 . . ? C38 C37 H37B 108.9 . . ? C31 C38 C37 112.7(4) . . ? C31 C38 H38A 109.0 . . ? C31 C38 H38B 109.0 . . ? C37 C38 H38A 109.0 . . ? C37 C38 H38B 109.0 . . ? H38A C38 H38B 107.8 . . ? Ir2 C41 H41 109.4 . . ? Ir2 C41 H41A 117.8 . . ? C42 C41 Ir2 75.0(5) . . ? C42 C41 H41 109.4 . . ? C42 C41 C48 133.8(6) . . ? C42A C41 Ir2 66.2(5) . . ? C42A C41 H41A 117.8 . . ? C48 C41 Ir2 113.7(3) . . ? C48 C41 H41 109.4 . . ? C48 C41 H41A 117.8 . . ? C48 C41 C42A 113.0(6) . . ? Ir2 C42 H42 114.9 . . ? C41 C42 Ir2 70.2(5) . . ? C41 C42 H42 114.9 . . ? C41 C42 C43 122.4(9) . . ? C43 C42 Ir2 111.3(8) . . ? C43 C42 H42 114.9 . . ? Ir2 C42A H42A 112.9 . . ? C41 C42A Ir2 71.4(4) . . ? C41 C42A H42A 112.9 . . ? C41 C42A C43A 125.5(10) . . ? C43A C42A Ir2 114.4(9) . . ? C43A C42A H42A 112.9 . . ? C42 C43 H43A 109.2 . . ? C42 C43 H43B 109.2 . . ? C42 C43 C44 112.1(9) . . ? H43A C43 H43B 107.9 . . ? C44 C43 H43A 109.2 . . ? C44 C43 H43B 109.2 . . ? C42A C43A H43C 109.3 . . ? C42A C43A H43D 109.3 . . ? H43C C43A H43D 108.0 . . ? C44A C43A C42A 111.5(11) . . ? C44A C43A H43C 109.3 . . ? C44A C43A H43D 109.3 . . ? C43 C44 H44A 109.3 . . ? C43 C44 H44B 109.3 . . ? H44A C44 H44B 107.9 . . ? C45 C44 C43 111.8(9) . . ? C45 C44 H44A 109.3 . . ? C45 C44 H44B 109.3 . . ? C43A C44A H44C 108.6 . . ? C43A C44A H44D 108.6 . . ? H44C C44A H44D 107.5 . . ? C45A C44A C43A 114.8(10) . . ? C45A C44A H44C 108.6 . . ? C45A C44A H44D 108.6 . . ? Ir2 C45 H45 113.8 . . ? C44 C45 Ir2 116.7(7) . . ? C44 C45 H45 113.8 . . ? C46 C45 Ir2 68.7(6) . . ? C46 C45 C44 122.7(10) . . ? C46 C45 H45 113.8 . . ? Ir2 C45A H45A 113.4 . . ? C44A C45A Ir2 110.2(8) . . ? C44A C45A H45A 113.4 . . ? C46A C45A Ir2 73.3(6) . . ? C46A C45A C44A 126.1(10) . . ? C46A C45A H45A 113.4 . . ? Ir2 C46 H46 114.6 . . ? C45 C46 Ir2 72.2(6) . . ? C45 C46 H46 114.6 . . ? C45 C46 C47 121.6(9) . . ? C47 C46 Ir2 112.4(6) . . ? C47 C46 H46 114.6 . . ? Ir2 C46A H46A 115.2 . . ? C45A C46A Ir2 68.0(6) . . ? C45A C46A H46A 115.2 . . ? C45A C46A C47 122.1(9) . . ? C47 C46A Ir2 112.2(7) . . ? C47 C46A H46A 115.2 . . ? C46 C47 H47A 109.2 . . ? C46 C47 H47B 109.2 . . ? C46A C47 H47C 107.9 . . ? C46A C47 H47D 107.9 . . ? C46A C47 C48 117.7(6) . . ? H47A C47 H47B 107.9 . . ? H47C C47 H47D 107.2 . . ? C48 C47 C46 112.2(6) . . ? C48 C47 H47A 109.2 . . ? C48 C47 H47B 109.2 . . ? C48 C47 H47C 107.9 . . ? C48 C47 H47D 107.9 . . ? C41 C48 C47 114.5(4) . . ? C41 C48 H48A 108.6 . . ? C41 C48 H48B 108.6 . . ? C47 C48 H48A 108.6 . . ? C47 C48 H48B 108.6 . . ? H48A C48 H48B 107.6 . . ? 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 Hg1 Ir1 2.5841(3) . ? Hg1 Ir2 2.6656(3) . ? Ir1 N1 2.045(3) . ? Ir1 C1 2.126(4) . ? Ir1 C17 2.131(4) . ? Ir1 C31 2.211(4) . ? Ir1 C32 2.187(4) . ? Ir1 C35 2.180(4) . ? Ir1 C36 2.170(4) . ? Ir2 Cl1 2.3335(12) . ? Ir2 Cl2 2.256(3) . ? Ir2 Cl2A 2.431(3) . ? Ir2 C41 2.133(5) . ? Ir2 C42 2.191(11) . ? Ir2 C42A 2.060(11) . ? Ir2 C45 2.146(10) . ? Ir2 C45A 2.131(9) . ? Ir2 C46 2.101(11) . ? Ir2 C46A 2.201(11) . ? N1 C7 1.357(6) . ? N1 C11 1.365(6) . ? C1 C2 1.410(6) . ? C1 C6 1.412(6) . ? C2 H2 0.9500 . ? C2 C3 1.379(6) . ? C3 C4 1.402(6) . ? C3 C18 1.558(9) . ? C3 C18A 1.549(15) . ? C4 H4 0.9500 . ? C4 C5 1.384(6) . ? C5 H5 0.9500 . ? C5 C6 1.401(6) . ? C6 C7 1.464(6) . ? C7 C8 1.390(6) . ? C8 H8 0.9500 . ? C8 C9 1.388(7) . ? C9 H9 0.9500 . ? C9 C10 1.388(7) . ? C10 H10 0.9500 . ? C10 C11 1.393(6) . ? C11 C12 1.454(6) . ? C12 C13 1.404(7) . ? C12 C17 1.415(6) . ? C13 H13 0.9500 . ? C13 C14 1.377(7) . ? C14 H14 0.9500 . ? C14 C15 1.396(7) . ? C15 C16 1.394(7) . ? C15 C22 1.528(7) . ? C16 H16 0.9500 . ? C16 C17 1.399(6) . ? C18 C19 1.526(11) . ? C18 C20 1.517(11) . ? C18 C21 1.517(10) . ? C18A C19A 1.540(17) . ? C18A C20A 1.536(17) . ? C18A C21A 1.536(17) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C19A H19D 0.9800 . ? C19A H19E 0.9800 . ? C19A H19F 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C20A H20D 0.9800 . ? C20A H20E 0.9800 . ? C20A H20F 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C21A H21D 0.9800 . ? C21A H21E 0.9800 . ? C21A H21F 0.9800 . ? C22 C23 1.531(8) . ? C22 C24 1.536(9) . ? C22 C25 1.540(8) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C31 H31 1.0000 . ? C31 C32 1.426(6) . ? C31 C38 1.509(6) . ? C32 H32 1.0000 . ? C32 C33 1.508(6) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C33 C34 1.538(7) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C34 C35 1.531(6) . ? C35 H35 1.0000 . ? C35 C36 1.417(7) . ? C36 H36 1.0000 . ? C36 C37 1.514(7) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C37 C38 1.534(7) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C41 H41 1.0000 . ? C41 H41A 1.0000 . ? C41 C42 1.294(11) . ? C41 C42A 1.518(12) . ? C41 C48 1.515(7) . ? C42 H42 1.0000 . ? C42 C43 1.528(11) . ? C42A H42A 1.0000 . ? C42A C43A 1.532(17) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C43 C44 1.529(13) . ? C43A H43C 0.9900 . ? C43A H43D 0.9900 . ? C43A C44A 1.516(19) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C44 C45 1.490(13) . ? C44A H44C 0.9900 . ? C44A H44D 0.9900 . ? C44A C45A 1.471(14) . ? C45 H45 1.0000 . ? C45 C46 1.422(15) . ? C45A H45A 1.0000 . ? C45A C46A 1.435(13) . ? C46 H46 1.0000 . ? C46 C47 1.567(12) . ? C46A H46A 1.0000 . ? C46A C47 1.453(12) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C47 H47C 0.9900 . ? C47 H47D 0.9900 . ? C47 C48 1.519(7) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ?