#------------------------------------------------------------------------------ #$Date: 2021-10-13 01:55:19 +0300 (Wed, 13 Oct 2021) $ #$Revision: 269903 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/85/7708546.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_7708546 loop_ _publ_author_name 'Poirot, Alexandre' 'Vanucci-Bacqu\'e, Corinne' 'Delavaux-Nicot, B\'eatrice' 'Leygue, Nadine' 'Saffon-Merceron, Nathalie' 'Alary, Fabienne' 'Bedos-Belval, Florence' 'Benoist, Eric' 'Fery-Forgues, Suzanne' _publ_section_title ; Phenyl-pyta-tricarbonylrhenium(I) complexes: combining a simplified structure and steric hindrance to modulate the photoluminescence properties. ; _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_paper_doi 10.1039/d1dt02161c _journal_year 2021 _chemical_formula_sum 'C27 H25 Cl4 N4 O3 Re' _chemical_formula_weight 781.51 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2021-06-11 deposited with the CCDC. 2021-09-02 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 112.3536(18) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 16.9598(9) _cell_length_b 10.7879(5) _cell_length_c 17.1754(8) _cell_measurement_reflns_used 9983 _cell_measurement_temperature 193(2) _cell_measurement_theta_max 28.28 _cell_measurement_theta_min 2.87 _cell_volume 2906.3(2) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX3' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT (Sheldrick 2015)' _diffrn_ambient_temperature 193(2) _diffrn_detector_area_resol_mean 7.3910 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type 'Bruker D8-Venture Photon III-C14 detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0329 _diffrn_reflns_av_unetI/netI 0.0115 _diffrn_reflns_Laue_measured_fraction_full 0.995 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 145772 _diffrn_reflns_point_group_measured_fraction_full 0.995 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.308 _diffrn_reflns_theta_min 3.049 _diffrn_source 'fine-focus sealed tube' _exptl_absorpt_coefficient_mu 4.585 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_correction_T_min 0.5799 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Bruker-AXS)' _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.786 _exptl_crystal_description plate _exptl_crystal_F_000 1528 _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.100 _refine_diff_density_max 1.026 _refine_diff_density_min -1.138 _refine_diff_density_rms 0.104 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 427 _refine_ls_number_reflns 7201 _refine_ls_number_restraints 360 _refine_ls_restrained_S_all 1.243 _refine_ls_R_factor_all 0.0268 _refine_ls_R_factor_gt 0.0239 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0409P)^2^+3.8183P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0679 _refine_ls_wR_factor_ref 0.0700 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6607 _reflns_number_total 7201 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1dt02161c2.cif _cod_data_source_block 3 _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 7708546 _shelx_shelxl_version_number 2018/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.461 _shelx_estimated_absorpt_t_max 0.657 _exptl_absorpt_special_details ; SADABS-2016/2 Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10. ; _shelx_res_file ; TITL cvb5_132_a.res in P2(1)/n cvb5_132_a.res created by SHELXL-2018/3 at 18:09:52 on 19-Mar-2021 CELL 0.71073 16.95980 10.78790 17.17540 90.0000 112.3536 90.0000 ZERR 4.00 0.00090 0.00050 0.00080 0.0000 0.0018 0.0000 LATT 1 SYMM 1/2-X, 1/2+Y, 1/2-Z SFAC C H Cl N O Re UNIT 108 100 16 16 12 4 L.S. 10 ACTA OMIT 2 0 0 OMIT 0 0 2 OMIT -2 0 2 OMIT 2 1 0 OMIT -2 2 1 OMIT 4 0 2 BOND $H DELU C27 > Cl4" SIMU 0.01 C27 > Cl4" ISOR 0.01 C27 > Cl4" FMAP 2 PLAN 20 CONF SIZE 0.10 0.20 0.20 TEMP -80.150 WGHT 0.040900 3.818300 FVAR 0.10012 0.51506 0.10866 0.31617 RE1 6 1.073527 0.225079 0.704143 11.00000 0.03181 0.03027 = 0.01646 0.00009 0.00651 0.00095 CL1 3 1.170396 0.385949 0.688885 11.00000 0.03399 0.03063 = 0.03130 0.00309 0.00435 -0.00158 O1 5 1.210438 0.128716 0.867509 11.00000 0.05082 0.06941 = 0.02947 0.01649 0.00171 0.00444 O2 5 0.956736 0.021126 0.723138 11.00000 0.07424 0.07863 = 0.04515 -0.00887 0.02631 -0.03635 O3 5 1.007161 0.394070 0.808951 11.00000 0.11507 0.05661 = 0.05538 -0.00059 0.05851 0.01544 N1 4 1.110729 0.120239 0.613359 11.00000 0.03158 0.02548 = 0.02157 0.00066 0.00755 -0.00052 N2 4 0.993047 0.290944 0.581624 11.00000 0.02875 0.03422 = 0.02034 -0.00346 0.00579 0.00299 N3 4 0.932974 0.383241 0.554613 11.00000 0.03488 0.04475 = 0.02457 -0.00231 0.00533 0.01246 N4 4 0.961794 0.313844 0.446984 11.00000 0.03297 0.03043 = 0.01811 0.00100 0.00612 0.00307 C1 1 1.158249 0.163986 0.805827 11.00000 0.04249 0.03672 = 0.02736 0.00242 0.01092 -0.00239 C2 1 0.999420 0.097446 0.714231 11.00000 0.05028 0.05066 = 0.02335 -0.00349 0.01516 -0.00859 C3 1 1.032980 0.331127 0.770231 11.00000 0.05871 0.04120 = 0.02438 0.00254 0.01925 0.00361 C4 1 1.168620 0.028402 0.634200 11.00000 0.03717 0.02935 = 0.03130 0.00560 0.00925 0.00326 AFIX 43 H4 2 1.197860 0.008871 0.692040 11.00000 -1.20000 AFIX 0 C5 1 1.187317 -0.038759 0.574864 11.00000 0.04081 0.02757 = 0.04312 0.00285 0.01814 0.00509 AFIX 43 H5 2 1.228862 -0.102795 0.591920 11.00000 -1.20000 AFIX 0 C6 1 1.145077 -0.011887 0.490698 11.00000 0.04333 0.02871 = 0.03824 -0.00357 0.02136 0.00142 AFIX 43 H6 2 1.156007 -0.058616 0.448995 11.00000 -1.20000 AFIX 0 C7 1 1.086148 0.084691 0.467580 11.00000 0.03702 0.03135 = 0.02600 -0.00341 0.01251 -0.00071 AFIX 43 H7 2 1.057025 0.106029 0.410034 11.00000 -1.20000 AFIX 0 C8 1 1.070907 0.148977 0.530290 11.00000 0.02851 0.02502 = 0.02371 -0.00039 0.00885 -0.00101 C9 1 1.009956 0.249627 0.516934 11.00000 0.02694 0.02872 = 0.01847 -0.00085 0.00525 -0.00020 C10 1 0.915271 0.394376 0.473707 11.00000 0.03751 0.04106 = 0.02378 0.00023 0.00482 0.01091 AFIX 43 H10 2 0.875014 0.451470 0.438052 11.00000 -1.20000 AFIX 0 C11 1 0.954872 0.300366 0.360931 11.00000 0.03504 0.03010 = 0.01610 0.00197 0.00539 0.00168 C12 1 0.878317 0.256712 0.302482 11.00000 0.03340 0.03855 = 0.02129 0.00083 0.00814 -0.00719 AFIX 43 H12 2 0.832892 0.235184 0.319416 11.00000 -1.20000 AFIX 0 C13 1 0.868958 0.244933 0.219342 11.00000 0.03671 0.04341 = 0.02089 -0.00083 0.00769 -0.01030 AFIX 43 H13 2 0.816862 0.213865 0.179404 11.00000 -1.20000 AFIX 0 C14 1 0.934363 0.277668 0.192633 11.00000 0.03500 0.02951 = 0.02354 0.00180 0.01105 -0.00024 C15 1 1.010788 0.320824 0.252997 11.00000 0.03154 0.04188 = 0.02619 0.00048 0.01092 -0.00213 AFIX 43 H15 2 1.056682 0.341499 0.236556 11.00000 -1.20000 AFIX 0 C16 1 1.020857 0.334069 0.336935 11.00000 0.03087 0.04099 = 0.02449 -0.00197 0.00537 -0.00574 AFIX 43 H16 2 1.072510 0.365910 0.377171 11.00000 -1.20000 AFIX 0 C17 1 0.918175 0.266546 0.098753 11.00000 0.03771 0.03248 = 0.02120 0.00018 0.01187 -0.00071 C18 1 0.837831 0.340685 0.048165 11.00000 0.04333 0.04151 = 0.02524 0.00345 0.01422 0.00934 AFIX 23 H18A 2 0.846822 0.429113 0.064586 11.00000 -1.20000 H18B 2 0.789228 0.309893 0.061188 11.00000 -1.20000 AFIX 0 C19 1 0.816805 0.328394 -0.046833 11.00000 0.04803 0.05865 = 0.02310 0.00826 0.01139 0.01255 AFIX 13 H19 2 0.764139 0.377030 -0.078585 11.00000 -1.20000 AFIX 0 C20 1 0.801779 0.192048 -0.072240 11.00000 0.05569 0.06569 = 0.02348 -0.00830 0.00852 -0.00375 AFIX 23 H20A 2 0.787196 0.183495 -0.133539 11.00000 -1.20000 H20B 2 0.753677 0.159347 -0.059147 11.00000 -1.20000 AFIX 0 C21 1 0.883486 0.118334 -0.023367 11.00000 0.06690 0.04152 = 0.03126 -0.01162 0.01096 0.00452 AFIX 13 H21 2 0.874511 0.029118 -0.040252 11.00000 -1.20000 AFIX 0 C22 1 0.957361 0.170112 -0.043777 11.00000 0.06651 0.06908 = 0.03441 -0.00889 0.02073 0.01825 AFIX 23 H22A 2 1.009788 0.121881 -0.013488 11.00000 -1.20000 H22B 2 0.944042 0.162819 -0.104935 11.00000 -1.20000 AFIX 0 C23 1 0.971808 0.306077 -0.017324 11.00000 0.05095 0.06566 = 0.03037 0.00015 0.02289 0.00466 AFIX 13 H23 2 1.020541 0.339451 -0.030162 11.00000 -1.20000 AFIX 0 C24 1 0.992330 0.317130 0.077331 11.00000 0.04354 0.04826 = 0.02767 -0.00020 0.01753 -0.00179 AFIX 23 H24A 2 1.002529 0.405154 0.094537 11.00000 -1.20000 H24B 2 1.044905 0.269969 0.108890 11.00000 -1.20000 AFIX 0 C25 1 0.904138 0.129711 0.071544 11.00000 0.05428 0.03493 = 0.02883 -0.00315 0.00850 0.00040 AFIX 23 H25A 2 0.956144 0.081396 0.103149 11.00000 -1.20000 H25B 2 0.856519 0.095291 0.084708 11.00000 -1.20000 AFIX 0 C26 1 0.891211 0.379393 -0.066518 11.00000 0.06417 0.05994 = 0.02585 0.00913 0.02044 0.00779 AFIX 23 H26A 2 0.878265 0.372475 -0.127628 11.00000 -1.20000 H26B 2 0.900037 0.468056 -0.050707 11.00000 -1.20000 AFIX 0 SAME C27 Cl3 Cl4 Cl2 SAME C27' Cl2' > Cl4' SAME C27" Cl2" > Cl4" PART 1 10.5 C27 1 0.260693 0.200053 0.155033 10.50000 0.10335 0.09291 = 0.08219 -0.00373 0.03006 -0.00705 AFIX 13 H27 2 0.320118 0.167792 0.171512 10.50000 -1.20000 AFIX 0 CL2 3 0.200369 0.119528 0.203725 10.50000 0.07597 0.05374 = 0.04958 0.00885 0.00124 -0.01161 CL3 3 0.256649 0.356089 0.181310 10.50000 0.17419 0.06472 = 0.08806 -0.01930 0.06885 -0.03344 CL4 3 0.207943 0.227698 0.043102 10.50000 0.14891 0.19215 = 0.07058 0.02181 0.03340 -0.04907 PART 2 10.25 C27' 1 0.216389 0.209168 0.064990 10.25000 0.12777 0.13307 = 0.11623 -0.00288 0.02618 -0.01204 AFIX 13 H27' 2 0.163243 0.158008 0.043747 10.25000 -1.20000 AFIX 0 CL2' 3 0.309945 0.142621 0.130412 10.25000 0.09809 0.11764 = 0.12912 -0.04238 0.06244 -0.01144 CL3' 3 0.220104 0.339556 0.125132 10.25000 0.13772 0.12694 = 0.15647 0.02343 0.02792 -0.00417 CL4' 3 0.253462 0.275281 -0.006374 10.25000 0.21864 0.24536 = 0.17383 0.01716 0.05688 -0.02647 PART 3 10.25 C27" 1 0.279614 0.194890 0.144153 10.25000 0.09585 0.09434 = 0.06907 -0.01349 0.03921 -0.00652 AFIX 13 H27" 2 0.335771 0.161335 0.147479 10.25000 -1.20000 AFIX 0 CL2" 3 0.248720 0.089881 0.198245 10.25000 0.14521 0.05869 = 0.03580 0.00587 -0.01999 -0.04208 CL3" 3 0.306917 0.326018 0.196527 10.25000 0.08970 0.08909 = 0.05477 -0.01131 0.02543 -0.03607 CL4" 3 0.221392 0.192824 0.039819 10.25000 0.07407 0.11208 = 0.03621 -0.03618 0.02511 -0.04032 PART 0 HKLF 4 REM cvb5_132_a.res in P2(1)/n REM wR2 = 0.0700, GooF = S = 1.077, Restrained GooF = 1.243 for all data REM R1 = 0.0239 for 6607 Fo > 4sig(Fo) and 0.0268 for all 7201 data REM 427 parameters refined using 360 restraints END WGHT 0.0409 3.8183 REM Highest difference peak 1.026, deepest hole -1.138, 1-sigma level 0.104 Q1 1 0.2875 0.0661 0.1880 11.00000 0.05 0.95 Q2 1 0.2193 0.2939 0.0824 11.00000 0.05 0.93 Q3 1 1.0450 0.2318 0.7243 11.00000 0.05 0.83 Q4 1 0.2690 0.2253 0.1938 11.00000 0.05 0.83 Q5 1 1.1003 0.2385 0.6842 11.00000 0.05 0.71 Q6 1 1.0619 0.2836 0.6926 11.00000 0.05 0.71 Q7 1 0.8915 0.2760 0.4032 11.00000 0.05 0.46 Q8 1 0.8960 0.2565 0.2104 11.00000 0.05 0.44 Q9 1 0.8374 0.1621 -0.0367 11.00000 0.05 0.43 Q10 1 0.9162 0.2895 0.3309 11.00000 0.05 0.42 Q11 1 0.9365 0.0853 0.7160 11.00000 0.05 0.40 Q12 1 0.9229 0.2749 0.1366 11.00000 0.05 0.39 Q13 1 0.2765 0.1559 0.0884 11.00000 0.05 0.38 Q14 1 1.1751 -0.0125 0.5356 11.00000 0.05 0.36 Q15 1 0.9580 0.2818 0.0890 11.00000 0.05 0.36 Q16 1 0.2041 0.1950 0.1344 11.00000 0.05 0.35 Q17 1 0.8948 0.1250 0.0227 11.00000 0.05 0.33 Q18 1 1.0387 0.1866 0.6691 11.00000 0.05 0.31 Q19 1 1.1227 0.0615 0.6136 11.00000 0.05 0.31 Q20 1 0.9875 0.2945 0.0306 11.00000 0.05 0.31 ; _shelx_res_checksum 54073 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re 1.07353(2) 0.22508(2) 0.70414(2) 0.02697(5) Uani 1 1 d . . . . . Cl1 Cl 1.17040(4) 0.38595(7) 0.68889(4) 0.03436(15) Uani 1 1 d . . . . . O1 O 1.21044(17) 0.1287(3) 0.86751(15) 0.0539(7) Uani 1 1 d . . . . . O2 O 0.9567(2) 0.0211(3) 0.72314(18) 0.0649(8) Uani 1 1 d . . . . . O3 O 1.0072(2) 0.3941(3) 0.80895(19) 0.0680(9) Uani 1 1 d . . . . . N1 N 1.11073(15) 0.1202(2) 0.61336(14) 0.0270(4) Uani 1 1 d . . . . . N2 N 0.99305(15) 0.2909(2) 0.58162(15) 0.0288(5) Uani 1 1 d . . . . . N3 N 0.93297(16) 0.3832(3) 0.55461(16) 0.0365(6) Uani 1 1 d . . . . . N4 N 0.96179(15) 0.3138(2) 0.44698(14) 0.0282(5) Uani 1 1 d . . . . . C1 C 1.1582(2) 0.1640(3) 0.80583(19) 0.0362(6) Uani 1 1 d . . . . . C2 C 0.9994(2) 0.0974(3) 0.71423(19) 0.0411(7) Uani 1 1 d . . . . . C3 C 1.0330(2) 0.3311(3) 0.77023(19) 0.0404(7) Uani 1 1 d . . . . . C4 C 1.16862(19) 0.0284(3) 0.63420(19) 0.0337(6) Uani 1 1 d . . . . . H4 H 1.197860 0.008871 0.692040 0.040 Uiso 1 1 calc R U . . . C5 C 1.1873(2) -0.0388(3) 0.5749(2) 0.0365(6) Uani 1 1 d . . . . . H5 H 1.228862 -0.102795 0.591920 0.044 Uiso 1 1 calc R U . . . C6 C 1.1451(2) -0.0119(3) 0.4907(2) 0.0350(6) Uani 1 1 d . . . . . H6 H 1.156007 -0.058616 0.448995 0.042 Uiso 1 1 calc R U . . . C7 C 1.08615(19) 0.0847(3) 0.46758(18) 0.0313(6) Uani 1 1 d . . . . . H7 H 1.057025 0.106029 0.410034 0.038 Uiso 1 1 calc R U . . . C8 C 1.07091(17) 0.1490(2) 0.53029(17) 0.0261(5) Uani 1 1 d . . . . . C9 C 1.00996(17) 0.2496(3) 0.51693(16) 0.0257(5) Uani 1 1 d . . . . . C10 C 0.9153(2) 0.3944(3) 0.47371(18) 0.0361(6) Uani 1 1 d . . . . . H10 H 0.875014 0.451470 0.438052 0.043 Uiso 1 1 calc R U . . . C11 C 0.95487(19) 0.3004(3) 0.36093(17) 0.0284(5) Uani 1 1 d . . . . . C12 C 0.8783(2) 0.2567(3) 0.30248(18) 0.0317(6) Uani 1 1 d . . . . . H12 H 0.832892 0.235184 0.319416 0.038 Uiso 1 1 calc R U . . . C13 C 0.8690(2) 0.2449(3) 0.21934(19) 0.0346(6) Uani 1 1 d . . . . . H13 H 0.816862 0.213865 0.179404 0.042 Uiso 1 1 calc R U . . . C14 C 0.9344(2) 0.2777(3) 0.19263(18) 0.0294(6) Uani 1 1 d . . . . . C15 C 1.01079(19) 0.3208(3) 0.25300(18) 0.0332(6) Uani 1 1 d . . . . . H15 H 1.056682 0.341499 0.236556 0.040 Uiso 1 1 calc R U . . . C16 C 1.02086(18) 0.3341(3) 0.33694(18) 0.0336(6) Uani 1 1 d . . . . . H16 H 1.072510 0.365910 0.377171 0.040 Uiso 1 1 calc R U . . . C17 C 0.9182(2) 0.2665(3) 0.09875(18) 0.0303(6) Uani 1 1 d . . . . . C18 C 0.8378(2) 0.3407(3) 0.04816(18) 0.0363(6) Uani 1 1 d . . . . . H18A H 0.846822 0.429113 0.064586 0.044 Uiso 1 1 calc R U . . . H18B H 0.789228 0.309893 0.061188 0.044 Uiso 1 1 calc R U . . . C19 C 0.8168(2) 0.3284(4) -0.04683(19) 0.0439(8) Uani 1 1 d . . . . . H19 H 0.764139 0.377030 -0.078585 0.053 Uiso 1 1 calc R U . . . C20 C 0.8018(3) 0.1920(4) -0.0722(2) 0.0502(9) Uani 1 1 d . . . . . H20A H 0.787196 0.183495 -0.133539 0.060 Uiso 1 1 calc R U . . . H20B H 0.753677 0.159347 -0.059147 0.060 Uiso 1 1 calc R U . . . C21 C 0.8835(3) 0.1183(4) -0.0234(2) 0.0488(9) Uani 1 1 d . . . . . H21 H 0.874511 0.029118 -0.040252 0.059 Uiso 1 1 calc R U . . . C22 C 0.9574(3) 0.1701(4) -0.0438(2) 0.0562(10) Uani 1 1 d . . . . . H22A H 1.009788 0.121881 -0.013488 0.067 Uiso 1 1 calc R U . . . H22B H 0.944042 0.162819 -0.104935 0.067 Uiso 1 1 calc R U . . . C23 C 0.9718(2) 0.3061(4) -0.0173(2) 0.0468(8) Uani 1 1 d . . . . . H23 H 1.020541 0.339451 -0.030162 0.056 Uiso 1 1 calc R U . . . C24 C 0.9923(2) 0.3171(3) 0.07733(19) 0.0386(7) Uani 1 1 d . . . . . H24A H 1.002529 0.405154 0.094537 0.046 Uiso 1 1 calc R U . . . H24B H 1.044905 0.269969 0.108890 0.046 Uiso 1 1 calc R U . . . C25 C 0.9041(2) 0.1297(3) 0.0715(2) 0.0415(7) Uani 1 1 d . . . . . H25A H 0.956144 0.081396 0.103149 0.050 Uiso 1 1 calc R U . . . H25B H 0.856519 0.095291 0.084708 0.050 Uiso 1 1 calc R U . . . C26 C 0.8912(3) 0.3794(4) -0.0665(2) 0.0490(9) Uani 1 1 d . . . . . H26A H 0.878265 0.372475 -0.127628 0.059 Uiso 1 1 calc R U . . . H26B H 0.900037 0.468056 -0.050707 0.059 Uiso 1 1 calc R U . . . C27 C 0.2607(10) 0.2001(10) 0.1550(7) 0.094(3) Uani 0.5 1 d D U P A 1 H27 H 0.320118 0.167792 0.171512 0.113 Uiso 0.5 1 calc R U P A 1 Cl2 Cl 0.20037(19) 0.1195(3) 0.20373(18) 0.0665(7) Uani 0.5 1 d D U P A 1 Cl3 Cl 0.2566(4) 0.3561(4) 0.1813(3) 0.1034(14) Uani 0.5 1 d D U P A 1 Cl4 Cl 0.2079(6) 0.2277(8) 0.0431(4) 0.140(3) Uani 0.5 1 d D U P A 1 C27' C 0.2164(14) 0.209(2) 0.0650(12) 0.132(4) Uani 0.25 1 d D U P B 2 H27' H 0.163243 0.158008 0.043747 0.158 Uiso 0.25 1 calc R U P B 2 Cl2' Cl 0.3099(5) 0.1426(8) 0.1304(5) 0.1092(19) Uani 0.25 1 d D U P B 2 Cl3' Cl 0.2201(7) 0.3396(11) 0.1251(8) 0.149(3) Uani 0.25 1 d D U P B 2 Cl4' Cl 0.2535(12) 0.2753(16) -0.0064(10) 0.218(4) Uani 0.25 1 d D U P B 2 C27" C 0.2796(17) 0.1949(16) 0.1442(8) 0.084(3) Uani 0.25 1 d D U P C 3 H27" H 0.335771 0.161335 0.147479 0.101 Uiso 0.25 1 calc R U P C 3 Cl2" Cl 0.2487(6) 0.0899(6) 0.1982(3) 0.096(2) Uani 0.25 1 d D U P C 3 Cl3" Cl 0.3069(5) 0.3260(8) 0.1965(4) 0.0785(18) Uani 0.25 1 d D U P C 3 Cl4" Cl 0.2214(6) 0.1928(10) 0.0398(5) 0.0729(18) Uani 0.25 1 d D U P C 3 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 Re1 0.03181(7) 0.03027(7) 0.01646(6) 0.00009(4) 0.00651(5) 0.00095(4) Cl1 0.0340(3) 0.0306(3) 0.0313(3) 0.0031(3) 0.0043(3) -0.0016(3) O1 0.0508(14) 0.0694(18) 0.0295(12) 0.0165(12) 0.0017(10) 0.0044(13) O2 0.0742(19) 0.079(2) 0.0452(15) -0.0089(14) 0.0263(14) -0.0364(17) O3 0.115(3) 0.0566(17) 0.0554(17) -0.0006(14) 0.0585(18) 0.0154(17) N1 0.0316(11) 0.0255(10) 0.0216(10) 0.0007(8) 0.0076(9) -0.0005(9) N2 0.0288(11) 0.0342(12) 0.0203(11) -0.0035(9) 0.0058(9) 0.0030(9) N3 0.0349(12) 0.0447(15) 0.0246(11) -0.0023(10) 0.0053(10) 0.0125(11) N4 0.0330(11) 0.0304(11) 0.0181(10) 0.0010(9) 0.0061(9) 0.0031(10) C1 0.0425(16) 0.0367(15) 0.0274(13) 0.0024(12) 0.0109(12) -0.0024(13) C2 0.0503(18) 0.0507(19) 0.0233(13) -0.0035(13) 0.0152(13) -0.0086(15) C3 0.059(2) 0.0412(17) 0.0244(13) 0.0025(13) 0.0193(13) 0.0036(15) C4 0.0372(14) 0.0294(13) 0.0313(14) 0.0056(11) 0.0093(11) 0.0033(11) C5 0.0408(16) 0.0276(13) 0.0431(17) 0.0028(12) 0.0181(13) 0.0051(12) C6 0.0433(16) 0.0287(13) 0.0382(15) -0.0036(12) 0.0214(13) 0.0014(12) C7 0.0370(14) 0.0314(13) 0.0260(13) -0.0034(11) 0.0125(11) -0.0007(11) C8 0.0285(12) 0.0250(12) 0.0237(12) -0.0004(10) 0.0089(10) -0.0010(10) C9 0.0269(12) 0.0287(12) 0.0185(12) -0.0009(10) 0.0052(10) -0.0002(10) C10 0.0375(15) 0.0411(16) 0.0238(13) 0.0002(12) 0.0048(11) 0.0109(13) C11 0.0350(14) 0.0301(13) 0.0161(11) 0.0020(10) 0.0054(10) 0.0017(11) C12 0.0334(14) 0.0385(14) 0.0213(13) 0.0008(11) 0.0081(11) -0.0072(12) C13 0.0367(15) 0.0434(16) 0.0209(13) -0.0008(12) 0.0077(12) -0.0103(13) C14 0.0350(14) 0.0295(14) 0.0235(13) 0.0018(10) 0.0110(11) -0.0002(11) C15 0.0315(13) 0.0419(16) 0.0262(13) 0.0005(12) 0.0109(11) -0.0021(12) C16 0.0309(13) 0.0410(16) 0.0245(13) -0.0020(12) 0.0054(10) -0.0057(12) C17 0.0377(15) 0.0325(14) 0.0212(13) 0.0002(10) 0.0119(11) -0.0007(11) C18 0.0433(16) 0.0415(16) 0.0252(13) 0.0034(12) 0.0142(12) 0.0093(13) C19 0.0480(18) 0.059(2) 0.0231(14) 0.0083(14) 0.0114(13) 0.0125(17) C20 0.056(2) 0.066(2) 0.0235(15) -0.0083(15) 0.0085(14) -0.0038(19) C21 0.067(2) 0.0415(18) 0.0313(16) -0.0116(14) 0.0110(15) 0.0045(17) C22 0.067(2) 0.069(3) 0.0344(17) -0.0089(18) 0.0207(17) 0.018(2) C23 0.0510(19) 0.066(2) 0.0304(16) 0.0001(16) 0.0229(14) 0.0047(17) C24 0.0435(16) 0.0483(18) 0.0277(14) -0.0002(13) 0.0175(12) -0.0018(14) C25 0.0543(19) 0.0349(15) 0.0288(14) -0.0031(12) 0.0085(13) 0.0004(14) C26 0.064(2) 0.060(2) 0.0259(14) 0.0091(15) 0.0204(15) 0.0078(18) C27 0.103(5) 0.093(4) 0.082(4) -0.004(4) 0.030(4) -0.007(4) Cl2 0.0760(16) 0.0537(13) 0.0496(12) 0.0088(10) 0.0012(12) -0.0116(12) Cl3 0.174(4) 0.0647(18) 0.088(3) -0.0193(18) 0.069(3) -0.033(3) Cl4 0.149(5) 0.192(6) 0.071(3) 0.022(3) 0.033(3) -0.049(4) C27' 0.128(5) 0.133(5) 0.116(5) -0.003(5) 0.026(5) -0.012(5) Cl2' 0.098(4) 0.118(5) 0.129(4) -0.042(4) 0.062(3) -0.011(3) Cl3' 0.138(6) 0.127(5) 0.156(6) 0.023(5) 0.028(5) -0.004(5) Cl4' 0.219(9) 0.245(9) 0.174(7) 0.017(6) 0.057(7) -0.026(8) C27" 0.096(5) 0.094(5) 0.069(4) -0.013(4) 0.039(4) -0.007(5) Cl2" 0.145(5) 0.059(3) 0.036(2) 0.006(2) -0.020(3) -0.042(4) Cl3" 0.090(4) 0.089(4) 0.055(3) -0.011(3) 0.025(3) -0.036(3) Cl4" 0.074(3) 0.112(4) 0.036(2) -0.036(3) 0.025(2) -0.040(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' 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' Re Re -1.0185 7.2310 '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 C1 Re1 C3 88.80(14) . . ? C1 Re1 C2 87.74(14) . . ? C3 Re1 C2 88.85(15) . . ? C1 Re1 N2 171.12(12) . . ? C3 Re1 N2 98.37(12) . . ? C2 Re1 N2 97.59(12) . . ? C1 Re1 N1 98.73(11) . . ? C3 Re1 N1 172.05(11) . . ? C2 Re1 N1 93.98(12) . . ? N2 Re1 N1 73.91(9) . . ? C1 Re1 Cl1 92.30(10) . . ? C3 Re1 Cl1 92.66(11) . . ? C2 Re1 Cl1 178.49(11) . . ? N2 Re1 Cl1 82.19(7) . . ? N1 Re1 Cl1 84.53(6) . . ? C4 N1 C8 117.9(2) . . ? C4 N1 Re1 124.51(19) . . ? C8 N1 Re1 117.58(18) . . ? C9 N2 N3 109.3(2) . . ? C9 N2 Re1 116.78(19) . . ? N3 N2 Re1 133.20(18) . . ? C10 N3 N2 105.4(2) . . ? C9 N4 C10 104.9(2) . . ? C9 N4 C11 129.9(2) . . ? C10 N4 C11 125.1(2) . . ? O1 C1 Re1 178.8(3) . . ? O2 C2 Re1 177.7(3) . . ? O3 C3 Re1 178.7(4) . . ? N1 C4 C5 122.6(3) . . ? N1 C4 H4 118.7 . . ? C5 C4 H4 118.7 . . ? C6 C5 C4 119.3(3) . . ? C6 C5 H5 120.3 . . ? C4 C5 H5 120.3 . . ? C5 C6 C7 119.1(3) . . ? C5 C6 H6 120.4 . . ? C7 C6 H6 120.4 . . ? C8 C7 C6 118.6(3) . . ? C8 C7 H7 120.7 . . ? C6 C7 H7 120.7 . . ? N1 C8 C7 122.4(3) . . ? N1 C8 C9 112.0(2) . . ? C7 C8 C9 125.6(3) . . ? N2 C9 N4 108.7(2) . . ? N2 C9 C8 119.1(2) . . ? N4 C9 C8 132.2(3) . . ? N3 C10 N4 111.7(3) . . ? N3 C10 H10 124.2 . . ? N4 C10 H10 124.2 . . ? C16 C11 C12 121.0(3) . . ? C16 C11 N4 121.3(3) . . ? C12 C11 N4 117.7(3) . . ? C13 C12 C11 119.2(3) . . ? C13 C12 H12 120.4 . . ? C11 C12 H12 120.4 . . ? C12 C13 C14 121.5(3) . . ? C12 C13 H13 119.2 . . ? C14 C13 H13 119.2 . . ? C15 C14 C13 118.0(3) . . ? C15 C14 C17 123.4(3) . . ? C13 C14 C17 118.6(3) . . ? C16 C15 C14 121.1(3) . . ? C16 C15 H15 119.5 . . ? C14 C15 H15 119.5 . . ? C11 C16 C15 119.2(3) . . ? C11 C16 H16 120.4 . . ? C15 C16 H16 120.4 . . ? C18 C17 C14 108.7(2) . . ? C18 C17 C24 108.1(3) . . ? C14 C17 C24 112.8(2) . . ? C18 C17 C25 109.1(3) . . ? C14 C17 C25 109.8(2) . . ? C24 C17 C25 108.3(3) . . ? C17 C18 C19 110.7(3) . . ? C17 C18 H18A 109.5 . . ? C19 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? C19 C18 H18B 109.5 . . ? H18A C18 H18B 108.1 . . ? C26 C19 C20 110.2(3) . . ? C26 C19 C18 109.0(3) . . ? C20 C19 C18 109.4(3) . . ? C26 C19 H19 109.4 . . ? C20 C19 H19 109.4 . . ? C18 C19 H19 109.4 . . ? C19 C20 C21 108.9(3) . . ? C19 C20 H20A 109.9 . . ? C21 C20 H20A 109.9 . . ? C19 C20 H20B 109.9 . . ? C21 C20 H20B 109.9 . . ? H20A C20 H20B 108.3 . . ? C22 C21 C25 109.8(3) . . ? C22 C21 C20 109.4(3) . . ? C25 C21 C20 109.4(3) . . ? C22 C21 H21 109.4 . . ? C25 C21 H21 109.4 . . ? C20 C21 H21 109.4 . . ? C23 C22 C21 109.6(3) . . ? C23 C22 H22A 109.8 . . ? C21 C22 H22A 109.8 . . ? C23 C22 H22B 109.8 . . ? C21 C22 H22B 109.8 . . ? H22A C22 H22B 108.2 . . ? C26 C23 C22 108.9(3) . . ? C26 C23 C24 110.0(3) . . ? C22 C23 C24 109.7(3) . . ? C26 C23 H23 109.4 . . ? C22 C23 H23 109.4 . . ? C24 C23 H23 109.4 . . ? C23 C24 C17 110.5(3) . . ? C23 C24 H24A 109.6 . . ? C17 C24 H24A 109.6 . . ? C23 C24 H24B 109.6 . . ? C17 C24 H24B 109.6 . . ? H24A C24 H24B 108.1 . . ? C21 C25 C17 110.2(3) . . ? C21 C25 H25A 109.6 . . ? C17 C25 H25A 109.6 . . ? C21 C25 H25B 109.6 . . ? C17 C25 H25B 109.6 . . ? H25A C25 H25B 108.1 . . ? C23 C26 C19 109.4(3) . . ? C23 C26 H26A 109.8 . . ? C19 C26 H26A 109.8 . . ? C23 C26 H26B 109.8 . . ? C19 C26 H26B 109.8 . . ? H26A C26 H26B 108.2 . . ? Cl3 C27 Cl2 105.2(7) . . ? Cl3 C27 Cl4 93.6(7) . . ? Cl2 C27 Cl4 116.1(8) . . ? Cl3 C27 H27 113.3 . . ? Cl2 C27 H27 113.3 . . ? Cl4 C27 H27 113.3 . . ? Cl2' C27' Cl4' 98.2(13) . . ? Cl2' C27' Cl3' 97.7(11) . . ? Cl4' C27' Cl3' 98.5(13) . . ? Cl2' C27' H27' 119.3 . . ? Cl4' C27' H27' 119.3 . . ? Cl3' C27' H27' 119.3 . . ? Cl3" C27" Cl2" 111.2(9) . . ? Cl3" C27" Cl4" 121.5(11) . . ? Cl2" C27" Cl4" 113.7(10) . . ? Cl3" C27" H27" 102.5 . . ? Cl2" C27" H27" 102.5 . . ? Cl4" C27" H27" 102.5 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re1 C1 1.908(3) . ? Re1 C3 1.914(3) . ? Re1 C2 1.916(3) . ? Re1 N2 2.147(2) . ? Re1 N1 2.204(2) . ? Re1 Cl1 2.4712(7) . ? O1 C1 1.156(4) . ? O2 C2 1.144(4) . ? O3 C3 1.147(4) . ? N1 C4 1.344(4) . ? N1 C8 1.362(3) . ? N2 C9 1.326(4) . ? N2 N3 1.373(3) . ? N3 C10 1.311(4) . ? N4 C9 1.358(3) . ? N4 C10 1.365(4) . ? N4 C11 1.445(3) . ? C4 C5 1.382(4) . ? C4 H4 0.9500 . ? C5 C6 1.378(5) . ? C5 H5 0.9500 . ? C6 C7 1.393(4) . ? C6 H6 0.9500 . ? C7 C8 1.386(4) . ? C7 H7 0.9500 . ? C8 C9 1.456(4) . ? C10 H10 0.9500 . ? C11 C16 1.380(4) . ? C11 C12 1.387(4) . ? C12 C13 1.381(4) . ? C12 H12 0.9500 . ? C13 C14 1.397(4) . ? C13 H13 0.9500 . ? C14 C15 1.396(4) . ? C14 C17 1.534(4) . ? C15 C16 1.393(4) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 C18 1.533(4) . ? C17 C24 1.538(4) . ? C17 C25 1.539(4) . ? C18 C19 1.538(4) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C26 1.528(5) . ? C19 C20 1.528(6) . ? C19 H19 1.0000 . ? C20 C21 1.540(6) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.529(6) . ? C21 C25 1.536(4) . ? C21 H21 1.0000 . ? C22 C23 1.527(6) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C26 1.526(5) . ? C23 C24 1.532(4) . ? C23 H23 1.0000 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 Cl3 1.751(11) . ? C27 Cl2 1.775(11) . ? C27 Cl4 1.810(11) . ? C27 H27 1.0000 . ? C27' Cl2' 1.714(16) . ? C27' Cl4' 1.730(16) . ? C27' Cl3' 1.732(16) . ? C27' H27' 1.0000 . ? C27" Cl3" 1.646(13) . ? C27" Cl2" 1.671(13) . ? C27" Cl4" 1.685(13) . ? C27" H27" 1.0000 . ? 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 C9 N2 N3 C10 0.2(3) . . . . ? Re1 N2 N3 C10 169.5(2) . . . . ? C8 N1 C4 C5 -1.5(4) . . . . ? Re1 N1 C4 C5 177.0(2) . . . . ? N1 C4 C5 C6 -0.3(5) . . . . ? C4 C5 C6 C7 1.7(5) . . . . ? C5 C6 C7 C8 -1.2(4) . . . . ? C4 N1 C8 C7 2.1(4) . . . . ? Re1 N1 C8 C7 -176.6(2) . . . . ? C4 N1 C8 C9 179.9(2) . . . . ? Re1 N1 C8 C9 1.2(3) . . . . ? C6 C7 C8 N1 -0.7(4) . . . . ? C6 C7 C8 C9 -178.2(3) . . . . ? N3 N2 C9 N4 0.2(3) . . . . ? Re1 N2 C9 N4 -171.15(18) . . . . ? N3 N2 C9 C8 -178.7(2) . . . . ? Re1 N2 C9 C8 10.0(3) . . . . ? C10 N4 C9 N2 -0.4(3) . . . . ? C11 N4 C9 N2 -177.5(3) . . . . ? C10 N4 C9 C8 178.2(3) . . . . ? C11 N4 C9 C8 1.2(5) . . . . ? N1 C8 C9 N2 -7.3(4) . . . . ? C7 C8 C9 N2 170.4(3) . . . . ? N1 C8 C9 N4 174.2(3) . . . . ? C7 C8 C9 N4 -8.1(5) . . . . ? N2 N3 C10 N4 -0.5(4) . . . . ? C9 N4 C10 N3 0.6(4) . . . . ? C11 N4 C10 N3 177.8(3) . . . . ? C9 N4 C11 C16 -70.6(4) . . . . ? C10 N4 C11 C16 112.9(4) . . . . ? C9 N4 C11 C12 111.8(4) . . . . ? C10 N4 C11 C12 -64.7(4) . . . . ? C16 C11 C12 C13 1.2(5) . . . . ? N4 C11 C12 C13 178.8(3) . . . . ? C11 C12 C13 C14 -0.9(5) . . . . ? C12 C13 C14 C15 1.2(5) . . . . ? C12 C13 C14 C17 -177.8(3) . . . . ? C13 C14 C15 C16 -1.7(5) . . . . ? C17 C14 C15 C16 177.2(3) . . . . ? C12 C11 C16 C15 -1.7(5) . . . . ? N4 C11 C16 C15 -179.2(3) . . . . ? C14 C15 C16 C11 1.9(5) . . . . ? C15 C14 C17 C18 -124.2(3) . . . . ? C13 C14 C17 C18 54.7(4) . . . . ? C15 C14 C17 C24 -4.3(4) . . . . ? C13 C14 C17 C24 174.6(3) . . . . ? C15 C14 C17 C25 116.6(3) . . . . ? C13 C14 C17 C25 -64.5(4) . . . . ? C14 C17 C18 C19 -177.8(3) . . . . ? C24 C17 C18 C19 59.4(3) . . . . ? C25 C17 C18 C19 -58.1(4) . . . . ? C17 C18 C19 C26 -60.7(4) . . . . ? C17 C18 C19 C20 59.9(4) . . . . ? C26 C19 C20 C21 59.3(4) . . . . ? C18 C19 C20 C21 -60.6(4) . . . . ? C19 C20 C21 C22 -59.3(4) . . . . ? C19 C20 C21 C25 61.0(4) . . . . ? C25 C21 C22 C23 -59.4(4) . . . . ? C20 C21 C22 C23 60.6(4) . . . . ? C21 C22 C23 C26 -61.0(4) . . . . ? C21 C22 C23 C24 59.4(4) . . . . ? C26 C23 C24 C17 59.7(4) . . . . ? C22 C23 C24 C17 -60.1(4) . . . . ? C18 C17 C24 C23 -58.6(4) . . . . ? C14 C17 C24 C23 -178.8(3) . . . . ? C25 C17 C24 C23 59.4(4) . . . . ? C22 C21 C25 C17 59.9(4) . . . . ? C20 C21 C25 C17 -60.1(4) . . . . ? C18 C17 C25 C21 58.2(4) . . . . ? C14 C17 C25 C21 177.2(3) . . . . ? C24 C17 C25 C21 -59.2(4) . . . . ? C22 C23 C26 C19 60.4(4) . . . . ? C24 C23 C26 C19 -59.7(4) . . . . ? C20 C19 C26 C23 -60.3(4) . . . . ? C18 C19 C26 C23 59.8(4) . . . . ?