#------------------------------------------------------------------------------ #$Date: 2021-10-13 01:55:19 +0300 (Wed, 13 Oct 2021) $ #$Revision: 269903 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/85/7708544.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_7708544 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 'C32 H20 Cl2 N8 O6 Re2' _chemical_formula_weight 1055.86 _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 space' _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 89.948(4) _cell_angle_beta 76.460(4) _cell_angle_gamma 73.825(4) _cell_formula_units_Z 2 _cell_length_a 10.8275(13) _cell_length_b 12.8483(16) _cell_length_c 13.1018(18) _cell_measurement_reflns_used 3751 _cell_measurement_temperature 193(2) _cell_measurement_theta_max 23.86 _cell_measurement_theta_min 2.95 _cell_volume 1697.8(4) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _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 2014/4 (Sheldrick, 2014)' _diffrn_ambient_temperature 193(2) _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type 'Bruker kappa APEX-II CCD Quazar' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1083 _diffrn_reflns_av_unetI/netI 0.0939 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 35952 _diffrn_reflns_point_group_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.371 _diffrn_reflns_theta_min 2.868 _diffrn_source 'Incoatec microfocus sealed tube' _exptl_absorpt_coefficient_mu 7.337 _exptl_absorpt_correction_T_max 0.7458 _exptl_absorpt_correction_T_min 0.6386 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Bruker-AXS)' _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 2.065 _exptl_crystal_description plate _exptl_crystal_F_000 1000 _exptl_crystal_size_max 0.060 _exptl_crystal_size_mid 0.020 _exptl_crystal_size_min 0.020 _refine_diff_density_max 1.264 _refine_diff_density_min -1.657 _refine_diff_density_rms 0.235 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 451 _refine_ls_number_reflns 6908 _refine_ls_number_restraints 12 _refine_ls_restrained_S_all 1.028 _refine_ls_R_factor_all 0.0888 _refine_ls_R_factor_gt 0.0435 _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^)+(0.0294P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0744 _refine_ls_wR_factor_ref 0.0901 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4405 _reflns_number_total 6908 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1dt02161c2.cif _cod_data_source_block 1 _cod_database_code 7708544 _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 0.667 _shelx_estimated_absorpt_t_max 0.867 _shelx_res_file ; TITL ALP063_a.res in P-1 ALP063_a.res created by SHELXL-2018/3 at 16:29:26 on 10-Mar-2020 CELL 0.71073 10.8275 12.8483 13.1018 89.948 76.460 73.825 ZERR 2.000 0.0013 0.0016 0.0018 0.004 0.004 0.004 LATT 1 SFAC C H N O Cl Re UNIT 64 40 16 12 4 4 SHEL 8 0.8 OMIT 0 -1 3 ISOR 0.01 C15 O1 L.S. 10 ACTA BOND $H FMAP 2 PLAN 20 SIZE 0.02 0.02 0.06 TEMP -80.130 WGHT 0.029400 FVAR 0.24703 RE1 6 0.650278 0.502572 0.757879 11.00000 0.02184 0.02485 = 0.02002 0.00353 -0.00252 -0.00607 RE2 6 0.706247 0.978360 0.250732 11.00000 0.02270 0.02440 = 0.01970 0.00474 -0.00553 -0.00569 CL1 5 0.868957 0.363979 0.716430 11.00000 0.02752 0.03065 = 0.03368 0.01322 -0.00515 -0.00208 CL2 5 0.611139 0.837662 0.199979 11.00000 0.04043 0.03638 = 0.03344 0.01141 -0.01657 -0.02053 O1 4 0.550526 0.374761 0.942267 11.00000 0.07737 0.04604 = 0.02617 0.01268 0.01273 -0.02634 O2 4 0.721025 0.645946 0.909670 11.00000 0.04686 0.06854 = 0.03375 -0.00200 -0.00536 -0.02961 O3 4 0.375804 0.666338 0.803875 11.00000 0.02591 0.05193 = 0.04790 -0.01031 -0.00508 0.00754 O4 4 0.818544 0.845951 0.418381 11.00000 0.05845 0.04393 = 0.02841 0.01123 -0.02139 0.00026 O5 4 0.454899 1.093607 0.416029 11.00000 0.03981 0.05794 = 0.04084 0.00256 -0.00315 -0.01756 O6 4 0.838211 1.143164 0.309329 11.00000 0.04193 0.04677 = 0.05167 -0.00496 -0.01322 -0.02379 N1 3 0.613397 0.410574 0.632274 11.00000 0.01864 0.02425 = 0.03029 0.00085 0.00006 -0.00757 N2 3 0.735051 0.561640 0.612538 11.00000 0.01971 0.01688 = 0.02333 0.00288 0.00066 -0.00120 N3 3 0.812347 0.631996 0.590344 11.00000 0.04320 0.03041 = 0.01646 0.00226 -0.00376 -0.01934 N4 3 0.816096 0.543246 0.443989 11.00000 0.02090 0.02315 = 0.02255 0.00499 -0.00545 -0.00479 N5 3 0.872464 0.900338 0.117946 11.00000 0.01588 0.01677 = 0.03590 0.00165 -0.00566 -0.00216 N6 3 0.652737 1.051197 0.112976 11.00000 0.01601 0.02034 = 0.02502 0.00446 -0.00073 -0.00236 N7 3 0.541849 1.124446 0.096355 11.00000 0.02516 0.01909 = 0.03511 0.00530 -0.01129 0.00048 N8 3 0.681703 1.056427 -0.057320 11.00000 0.01445 0.02065 = 0.02425 0.00436 -0.00506 -0.00280 C1 1 0.586047 0.423594 0.874635 11.00000 0.03323 0.02829 = 0.03250 -0.00678 -0.00188 -0.00255 C2 1 0.697058 0.590087 0.850957 11.00000 0.02225 0.04566 = 0.03153 0.01046 -0.00126 -0.00510 C3 1 0.482060 0.602609 0.783271 11.00000 0.03244 0.03543 = 0.02533 0.00481 -0.00690 -0.01633 C4 1 0.545932 0.337609 0.646567 11.00000 0.03199 0.02806 = 0.02752 0.00571 -0.00369 -0.01601 AFIX 43 H4 2 0.510856 0.322580 0.716678 11.00000 -1.20000 AFIX 0 C5 1 0.523851 0.282397 0.565509 11.00000 0.03384 0.02728 = 0.03235 -0.00025 0.00200 -0.01873 AFIX 43 H5 2 0.475994 0.230136 0.579738 11.00000 -1.20000 AFIX 0 C6 1 0.572707 0.304609 0.463241 11.00000 0.02437 0.02691 = 0.03025 -0.00824 0.00099 -0.00462 AFIX 43 H6 2 0.556229 0.269582 0.406112 11.00000 -1.20000 AFIX 0 C7 1 0.645509 0.378024 0.445007 11.00000 0.02206 0.02772 = 0.01869 -0.00088 0.00037 -0.01092 AFIX 43 H7 2 0.682442 0.393026 0.375313 11.00000 -1.20000 AFIX 0 C8 1 0.663588 0.429666 0.531274 11.00000 0.02346 0.01439 = 0.02619 0.00465 -0.00614 -0.00656 C9 1 0.737315 0.509616 0.525916 11.00000 0.02709 0.01739 = 0.02547 0.00595 -0.00074 -0.00087 C10 1 0.858392 0.619869 0.489011 11.00000 0.03258 0.02201 = 0.03536 0.01183 -0.01294 -0.01800 AFIX 43 H10 2 0.914454 0.658995 0.450438 11.00000 -1.20000 AFIX 0 C11 1 0.852141 0.510786 0.331767 11.00000 0.01897 0.03788 = 0.01061 0.00377 0.00079 -0.01290 C12 1 0.934107 0.409364 0.297663 11.00000 0.03463 0.03774 = 0.03802 0.00153 -0.01565 -0.00241 AFIX 43 H12 2 0.967792 0.360819 0.345930 11.00000 -1.20000 AFIX 0 C13 1 0.966924 0.378833 0.192566 11.00000 0.03478 0.03075 = 0.05581 -0.01330 0.00558 -0.01334 AFIX 43 H13 2 1.022609 0.307999 0.167351 11.00000 -1.20000 AFIX 0 C14 1 0.919158 0.450908 0.123150 11.00000 0.06851 0.07261 = 0.02317 -0.01678 0.00985 -0.04683 AFIX 43 H14 2 0.942784 0.429492 0.050155 11.00000 -1.20000 AFIX 0 C15 1 0.837958 0.553095 0.158491 11.00000 0.06078 0.03460 = 0.02474 0.01237 -0.00479 -0.02401 AFIX 43 H15 2 0.804371 0.602432 0.110760 11.00000 -1.20000 AFIX 0 C16 1 0.805829 0.583053 0.264880 11.00000 0.03681 0.02777 = 0.02900 -0.00150 0.00416 -0.01657 AFIX 43 H16 2 0.751469 0.654082 0.290837 11.00000 -1.20000 AFIX 0 C17 1 0.772117 0.895619 0.356724 11.00000 0.03719 0.04330 = 0.01750 -0.00621 -0.00398 -0.01225 C18 1 0.549462 1.049900 0.353816 11.00000 0.04125 0.03286 = 0.01261 0.00005 -0.00897 -0.01944 C19 1 0.787257 1.082427 0.284591 11.00000 0.02459 0.02564 = 0.01983 0.00619 -0.00193 0.00660 C20 1 0.983328 0.827674 0.126534 11.00000 0.02980 0.02528 = 0.03154 0.00749 -0.01598 -0.00645 AFIX 43 H20 2 0.990438 0.805599 0.194656 11.00000 -1.20000 AFIX 0 C21 1 1.086970 0.783184 0.043604 11.00000 0.02054 0.01989 = 0.04253 -0.00418 -0.00480 0.00196 AFIX 43 H21 2 1.162661 0.729288 0.053632 11.00000 -1.20000 AFIX 0 C22 1 1.081045 0.817382 -0.056055 11.00000 0.02454 0.03023 = 0.03118 0.00020 -0.00805 -0.00270 AFIX 43 H22 2 1.153817 0.790063 -0.115036 11.00000 -1.20000 AFIX 0 C23 1 0.966778 0.891985 -0.067031 11.00000 0.02436 0.02249 = 0.02899 0.00268 -0.00405 -0.00952 AFIX 43 H23 2 0.959622 0.916269 -0.134485 11.00000 -1.20000 AFIX 0 C24 1 0.862421 0.931682 0.019747 11.00000 0.02870 0.02477 = 0.01747 0.00110 -0.00776 -0.01311 C25 1 0.735170 1.011773 0.022467 11.00000 0.02479 0.01907 = 0.02580 0.00746 -0.00637 -0.00040 C26 1 0.562499 1.127395 -0.006379 11.00000 0.02905 0.03445 = 0.02692 0.00600 -0.00832 -0.00585 AFIX 43 H26 2 0.502284 1.173067 -0.041158 11.00000 -1.20000 AFIX 0 C27 1 0.733071 1.034573 -0.168868 11.00000 0.02595 0.02889 = 0.01871 -0.00274 -0.00756 -0.00905 C28 1 0.744937 0.933989 -0.214700 11.00000 0.03582 0.03526 = 0.02411 0.00680 -0.00219 -0.01364 AFIX 43 H28 2 0.717391 0.880278 -0.172909 11.00000 -1.20000 AFIX 0 C29 1 0.797366 0.912648 -0.322038 11.00000 0.03113 0.04642 = 0.04096 -0.01800 -0.00710 -0.01314 AFIX 43 H29 2 0.806679 0.844043 -0.354819 11.00000 -1.20000 AFIX 0 C30 1 0.835933 0.992472 -0.380783 11.00000 0.04247 0.06007 = 0.02716 -0.00925 -0.00162 -0.01848 AFIX 43 H30 2 0.872717 0.978081 -0.454399 11.00000 -1.20000 AFIX 0 C31 1 0.821841 1.093729 -0.333983 11.00000 0.04704 0.05814 = 0.03887 0.01531 -0.01326 -0.02922 AFIX 43 H31 2 0.848227 1.147974 -0.375642 11.00000 -1.20000 AFIX 0 C32 1 0.770265 1.114818 -0.228582 11.00000 0.02752 0.03908 = 0.02319 0.00676 -0.00323 -0.01050 AFIX 43 H32 2 0.759826 1.183876 -0.196190 11.00000 -1.20000 AFIX 0 HKLF 4 REM ALP063_a.res in P-1 REM wR2 = 0.090148, GooF = S = 1.02733, Restrained GooF = 1.02752 for all data REM R1 = 0.043544 for 4405 Fo > 4sig(Fo) and 0.088810 for all 6908 data REM 451 parameters refined using 12 restraints END WGHT 0.0292 0.0000 REM Highest difference peak 1.264, deepest hole -1.657, 1-sigma level 0.235 Q1 1 0.7350 0.3764 0.7766 11.00000 0.05 1.26 Q2 1 0.7655 0.4576 0.7401 11.00000 0.05 1.26 Q3 1 0.5849 1.0253 0.2705 11.00000 0.05 1.18 Q4 1 0.6641 0.4209 0.6634 11.00000 0.05 1.18 Q5 1 0.6758 0.9461 0.3621 11.00000 0.05 1.08 Q6 1 0.7111 1.2234 0.3242 11.00000 0.05 0.97 Q7 1 0.6340 0.9326 0.2208 11.00000 0.05 0.96 Q8 1 0.6140 0.9963 0.3450 11.00000 0.05 0.93 Q9 1 0.7947 0.9397 0.1528 11.00000 0.05 0.92 Q10 1 0.8751 0.9819 0.2274 11.00000 0.05 0.92 Q11 1 0.9090 1.0837 0.3180 11.00000 0.05 0.91 Q12 1 0.6210 0.9636 0.1892 11.00000 0.05 0.91 Q13 1 0.9012 1.1217 -0.3585 11.00000 0.05 0.90 Q14 1 0.7343 0.5332 0.7878 11.00000 0.05 0.88 Q15 1 0.4986 0.4926 0.7651 11.00000 0.05 0.87 Q16 1 0.5420 0.6165 0.7939 11.00000 0.05 0.87 Q17 1 0.6416 0.6204 0.7893 11.00000 0.05 0.86 Q18 1 1.0745 0.3942 0.3107 11.00000 0.05 0.86 Q19 1 0.6932 0.9146 0.1530 11.00000 0.05 0.85 Q20 1 0.7140 0.8571 0.2288 11.00000 0.05 0.84 ; _shelx_res_checksum 54117 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 Re1 Re 0.65028(4) 0.50257(3) 0.75788(3) 0.02281(11) Uani 1 1 d . . . . . Re2 Re 0.70625(4) 0.97836(3) 0.25073(3) 0.02242(11) Uani 1 1 d . . . . . Cl1 Cl 0.8690(2) 0.36398(19) 0.71643(19) 0.0323(6) Uani 1 1 d . . . . . Cl2 Cl 0.6111(2) 0.83766(19) 0.19998(19) 0.0335(6) Uani 1 1 d . . . . . O1 O 0.5505(7) 0.3748(6) 0.9423(5) 0.052(2) Uani 1 1 d . U . . . O2 O 0.7210(7) 0.6459(6) 0.9097(5) 0.048(2) Uani 1 1 d . . . . . O3 O 0.3758(7) 0.6663(6) 0.8039(6) 0.046(2) Uani 1 1 d . . . . . O4 O 0.8185(7) 0.8460(5) 0.4184(5) 0.0448(19) Uani 1 1 d . . . . . O5 O 0.4549(7) 1.0936(6) 0.4160(6) 0.0466(19) Uani 1 1 d . . . . . O6 O 0.8382(7) 1.1432(6) 0.3093(6) 0.0442(19) Uani 1 1 d . . . . . N1 N 0.6134(7) 0.4106(6) 0.6323(6) 0.0251(18) Uani 1 1 d . . . . . N2 N 0.7351(6) 0.5616(5) 0.6125(6) 0.0218(17) Uani 1 1 d . . . . . N3 N 0.8123(7) 0.6320(6) 0.5903(6) 0.0288(19) Uani 1 1 d . . . . . N4 N 0.8161(7) 0.5432(6) 0.4440(6) 0.0225(17) Uani 1 1 d . . . . . N5 N 0.8725(7) 0.9003(5) 0.1179(6) 0.0235(18) Uani 1 1 d . . . . . N6 N 0.6527(7) 1.0512(6) 0.1130(6) 0.0218(17) Uani 1 1 d . . . . . N7 N 0.5418(7) 1.1244(6) 0.0964(6) 0.0272(18) Uani 1 1 d . . . . . N8 N 0.6817(7) 1.0564(5) -0.0573(6) 0.0202(16) Uani 1 1 d . . . . . C1 C 0.5860(9) 0.4236(8) 0.8746(8) 0.034(2) Uani 1 1 d . . . . . C2 C 0.6971(9) 0.5901(8) 0.8510(8) 0.035(2) Uani 1 1 d . . . . . C3 C 0.4821(10) 0.6026(8) 0.7833(7) 0.030(2) Uani 1 1 d . . . . . C4 C 0.5459(8) 0.3376(7) 0.6466(7) 0.028(2) Uani 1 1 d . . . . . H4 H 0.510856 0.322580 0.716678 0.034 Uiso 1 1 calc R U . . . C5 C 0.5239(9) 0.2824(7) 0.5655(7) 0.031(2) Uani 1 1 d . . . . . H5 H 0.475994 0.230136 0.579738 0.037 Uiso 1 1 calc R U . . . C6 C 0.5727(8) 0.3046(7) 0.4632(7) 0.029(2) Uani 1 1 d . . . . . H6 H 0.556229 0.269582 0.406112 0.035 Uiso 1 1 calc R U . . . C7 C 0.6455(8) 0.3780(7) 0.4450(7) 0.023(2) Uani 1 1 d . . . . . H7 H 0.682442 0.393026 0.375313 0.028 Uiso 1 1 calc R U . . . C8 C 0.6636(8) 0.4297(7) 0.5313(7) 0.021(2) Uani 1 1 d . . . . . C9 C 0.7373(9) 0.5096(7) 0.5259(7) 0.025(2) Uani 1 1 d . . . . . C10 C 0.8584(9) 0.6199(7) 0.4890(7) 0.027(2) Uani 1 1 d . . . . . H10 H 0.914454 0.658995 0.450438 0.032 Uiso 1 1 calc R U . . . C11 C 0.8521(8) 0.5108(8) 0.3318(7) 0.022(2) Uani 1 1 d . . . . . C12 C 0.9341(9) 0.4094(8) 0.2977(8) 0.037(3) Uani 1 1 d . . . . . H12 H 0.967792 0.360819 0.345930 0.045 Uiso 1 1 calc R U . . . C13 C 0.9669(10) 0.3788(8) 0.1926(9) 0.042(3) Uani 1 1 d . . . . . H13 H 1.022609 0.307999 0.167351 0.051 Uiso 1 1 calc R U . . . C14 C 0.9192(11) 0.4509(10) 0.1231(9) 0.053(3) Uani 1 1 d . . . . . H14 H 0.942784 0.429492 0.050155 0.063 Uiso 1 1 calc R U . . . C15 C 0.8380(10) 0.5531(8) 0.1585(8) 0.039(3) Uani 1 1 d . U . . . H15 H 0.804371 0.602432 0.110760 0.047 Uiso 1 1 calc R U . . . C16 C 0.8058(9) 0.5831(8) 0.2649(7) 0.032(2) Uani 1 1 d . . . . . H16 H 0.751469 0.654082 0.290837 0.038 Uiso 1 1 calc R U . . . C17 C 0.7721(9) 0.8956(8) 0.3567(7) 0.033(2) Uani 1 1 d . . . . . C18 C 0.5495(10) 1.0499(8) 0.3538(7) 0.027(2) Uani 1 1 d . . . . . C19 C 0.7873(9) 1.0824(7) 0.2846(7) 0.027(2) Uani 1 1 d . . . . . C20 C 0.9833(9) 0.8277(7) 0.1265(7) 0.028(2) Uani 1 1 d . . . . . H20 H 0.990438 0.805599 0.194656 0.033 Uiso 1 1 calc R U . . . C21 C 1.0870(9) 0.7832(7) 0.0436(8) 0.030(2) Uani 1 1 d . . . . . H21 H 1.162661 0.729288 0.053632 0.036 Uiso 1 1 calc R U . . . C22 C 1.0810(9) 0.8174(7) -0.0561(7) 0.030(2) Uani 1 1 d . . . . . H22 H 1.153817 0.790063 -0.115036 0.035 Uiso 1 1 calc R U . . . C23 C 0.9668(8) 0.8920(7) -0.0670(7) 0.025(2) Uani 1 1 d . . . . . H23 H 0.959622 0.916269 -0.134485 0.030 Uiso 1 1 calc R U . . . C24 C 0.8624(9) 0.9317(7) 0.0197(7) 0.022(2) Uani 1 1 d . . . . . C25 C 0.7352(9) 1.0118(7) 0.0225(7) 0.024(2) Uani 1 1 d . . . . . C26 C 0.5625(9) 1.1274(8) -0.0064(7) 0.031(2) Uani 1 1 d . . . . . H26 H 0.502284 1.173067 -0.041158 0.037 Uiso 1 1 calc R U . . . C27 C 0.7331(8) 1.0346(7) -0.1689(7) 0.024(2) Uani 1 1 d . . . . . C28 C 0.7449(9) 0.9340(8) -0.2147(7) 0.032(2) Uani 1 1 d . . . . . H28 H 0.717391 0.880278 -0.172909 0.038 Uiso 1 1 calc R U . . . C29 C 0.7974(9) 0.9126(9) -0.3220(8) 0.039(3) Uani 1 1 d . . . . . H29 H 0.806679 0.844043 -0.354819 0.047 Uiso 1 1 calc R U . . . C30 C 0.8359(10) 0.9925(9) -0.3808(8) 0.044(3) Uani 1 1 d . . . . . H30 H 0.872717 0.978081 -0.454399 0.052 Uiso 1 1 calc R U . . . C31 C 0.8218(10) 1.0937(9) -0.3340(8) 0.045(3) Uani 1 1 d . . . . . H31 H 0.848227 1.147974 -0.375642 0.054 Uiso 1 1 calc R U . . . C32 C 0.7703(9) 1.1148(8) -0.2286(7) 0.030(2) Uani 1 1 d . . . . . H32 H 0.759826 1.183876 -0.196190 0.036 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.0218(2) 0.0249(2) 0.0200(2) 0.00353(17) -0.00252(17) -0.00607(18) Re2 0.0227(2) 0.0244(2) 0.0197(2) 0.00474(17) -0.00553(17) -0.00569(18) Cl1 0.0275(14) 0.0306(14) 0.0337(14) 0.0132(11) -0.0052(11) -0.0021(11) Cl2 0.0404(15) 0.0364(14) 0.0334(14) 0.0114(12) -0.0166(12) -0.0205(12) O1 0.077(6) 0.046(5) 0.026(4) 0.013(4) 0.013(4) -0.026(4) O2 0.047(5) 0.069(6) 0.034(5) -0.002(4) -0.005(4) -0.030(4) O3 0.026(4) 0.052(5) 0.048(5) -0.010(4) -0.005(4) 0.008(4) O4 0.058(5) 0.044(5) 0.028(4) 0.011(4) -0.021(4) 0.000(4) O5 0.040(5) 0.058(5) 0.041(5) 0.003(4) -0.003(4) -0.018(4) O6 0.042(5) 0.047(5) 0.052(5) -0.005(4) -0.013(4) -0.024(4) N1 0.019(4) 0.024(4) 0.030(5) 0.001(4) 0.000(3) -0.008(3) N2 0.020(4) 0.017(4) 0.023(4) 0.003(3) 0.001(3) -0.001(3) N3 0.043(5) 0.030(5) 0.016(4) 0.002(4) -0.004(4) -0.019(4) N4 0.021(4) 0.023(4) 0.023(4) 0.005(3) -0.005(3) -0.005(3) N5 0.016(4) 0.017(4) 0.036(5) 0.002(4) -0.006(4) -0.002(3) N6 0.016(4) 0.020(4) 0.025(4) 0.004(3) -0.001(3) -0.002(3) N7 0.025(5) 0.019(4) 0.035(5) 0.005(4) -0.011(4) 0.000(4) N8 0.014(4) 0.021(4) 0.024(4) 0.004(3) -0.005(3) -0.003(3) C1 0.033(6) 0.028(6) 0.032(6) -0.007(5) -0.002(5) -0.003(5) C2 0.022(6) 0.046(7) 0.032(6) 0.010(5) -0.001(5) -0.005(5) C3 0.032(6) 0.035(6) 0.025(6) 0.005(5) -0.007(5) -0.016(5) C4 0.032(6) 0.028(5) 0.028(6) 0.006(4) -0.004(4) -0.016(5) C5 0.034(6) 0.027(6) 0.032(6) 0.000(5) 0.002(5) -0.019(5) C6 0.024(5) 0.027(5) 0.030(6) -0.008(4) 0.001(4) -0.005(4) C7 0.022(5) 0.028(5) 0.019(5) -0.001(4) 0.000(4) -0.011(4) C8 0.023(5) 0.014(5) 0.026(5) 0.005(4) -0.006(4) -0.007(4) C9 0.027(6) 0.017(5) 0.025(6) 0.006(4) -0.001(4) -0.001(4) C10 0.033(6) 0.022(5) 0.035(6) 0.012(4) -0.013(5) -0.018(5) C11 0.019(5) 0.038(6) 0.011(5) 0.004(4) 0.001(4) -0.013(5) C12 0.035(6) 0.038(6) 0.038(7) 0.002(5) -0.016(5) -0.002(5) C13 0.035(7) 0.031(6) 0.056(8) -0.013(6) 0.006(6) -0.013(5) C14 0.069(9) 0.073(9) 0.023(6) -0.017(6) 0.010(6) -0.047(8) C15 0.061(6) 0.035(5) 0.025(5) 0.012(4) -0.005(5) -0.024(5) C16 0.037(6) 0.028(6) 0.029(6) -0.001(5) 0.004(5) -0.017(5) C17 0.037(6) 0.043(6) 0.017(5) -0.006(5) -0.004(5) -0.012(5) C18 0.041(6) 0.033(6) 0.013(5) 0.000(4) -0.009(5) -0.019(5) C19 0.025(5) 0.026(5) 0.020(5) 0.006(4) -0.002(4) 0.007(4) C20 0.030(6) 0.025(5) 0.032(6) 0.007(5) -0.016(5) -0.006(5) C21 0.021(5) 0.020(5) 0.043(7) -0.004(5) -0.005(5) 0.002(4) C22 0.025(6) 0.030(6) 0.031(6) 0.000(5) -0.008(5) -0.003(5) C23 0.024(5) 0.022(5) 0.029(6) 0.003(4) -0.004(4) -0.010(4) C24 0.029(6) 0.025(5) 0.017(5) 0.001(4) -0.008(4) -0.013(4) C25 0.025(6) 0.019(5) 0.026(6) 0.007(4) -0.006(4) 0.000(4) C26 0.029(6) 0.034(6) 0.027(6) 0.006(5) -0.008(5) -0.006(5) C27 0.026(5) 0.029(6) 0.019(5) -0.003(4) -0.008(4) -0.009(4) C28 0.036(6) 0.035(6) 0.024(6) 0.007(5) -0.002(5) -0.014(5) C29 0.031(6) 0.046(7) 0.041(7) -0.018(6) -0.007(5) -0.013(5) C30 0.042(7) 0.060(8) 0.027(6) -0.009(6) -0.002(5) -0.018(6) C31 0.047(7) 0.058(8) 0.039(7) 0.015(6) -0.013(6) -0.029(6) C32 0.028(6) 0.039(6) 0.023(6) 0.007(5) -0.003(4) -0.011(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Cl Cl 0.1484 0.1585 '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 C3 Re1 C2 89.0(4) . . ? C3 Re1 C1 89.5(4) . . ? C2 Re1 C1 90.1(4) . . ? C3 Re1 N2 97.2(3) . . ? C2 Re1 N2 98.1(3) . . ? C1 Re1 N2 169.5(3) . . ? C3 Re1 N1 93.0(3) . . ? C2 Re1 N1 171.9(3) . . ? C1 Re1 N1 97.7(3) . . ? N2 Re1 N1 73.9(3) . . ? C3 Re1 Cl1 176.5(3) . . ? C2 Re1 Cl1 94.5(3) . . ? C1 Re1 Cl1 90.7(3) . . ? N2 Re1 Cl1 82.09(18) . . ? N1 Re1 Cl1 83.53(19) . . ? C19 Re2 C17 87.0(4) . . ? C19 Re2 C18 89.5(4) . . ? C17 Re2 C18 89.3(4) . . ? C19 Re2 N6 96.7(3) . . ? C17 Re2 N6 170.8(3) . . ? C18 Re2 N6 99.1(3) . . ? C19 Re2 N5 93.9(3) . . ? C17 Re2 N5 97.0(3) . . ? C18 Re2 N5 173.1(3) . . ? N6 Re2 N5 74.5(3) . . ? C19 Re2 Cl2 177.1(3) . . ? C17 Re2 Cl2 92.9(3) . . ? C18 Re2 Cl2 93.5(3) . . ? N6 Re2 Cl2 82.94(18) . . ? N5 Re2 Cl2 83.23(18) . . ? C4 N1 C8 116.9(7) . . ? C4 N1 Re1 125.6(6) . . ? C8 N1 Re1 117.5(5) . . ? C9 N2 N3 110.3(7) . . ? C9 N2 Re1 116.5(6) . . ? N3 N2 Re1 131.8(5) . . ? C10 N3 N2 104.8(7) . . ? C9 N4 C10 104.7(7) . . ? C9 N4 C11 130.5(7) . . ? C10 N4 C11 124.8(7) . . ? C20 N5 C24 118.0(8) . . ? C20 N5 Re2 124.7(6) . . ? C24 N5 Re2 117.3(6) . . ? C25 N6 N7 109.6(7) . . ? C25 N6 Re2 116.2(6) . . ? N7 N6 Re2 133.8(6) . . ? C26 N7 N6 105.2(7) . . ? C25 N8 C26 103.7(7) . . ? C25 N8 C27 129.4(7) . . ? C26 N8 C27 126.8(7) . . ? O1 C1 Re1 178.3(9) . . ? O2 C2 Re1 177.5(9) . . ? O3 C3 Re1 177.1(8) . . ? N1 C4 C5 123.8(9) . . ? N1 C4 H4 118.1 . . ? C5 C4 H4 118.1 . . ? C4 C5 C6 118.7(8) . . ? C4 C5 H5 120.7 . . ? C6 C5 H5 120.7 . . ? C7 C6 C5 119.3(8) . . ? C7 C6 H6 120.4 . . ? C5 C6 H6 120.4 . . ? C6 C7 C8 118.3(8) . . ? C6 C7 H7 120.9 . . ? C8 C7 H7 120.9 . . ? N1 C8 C7 123.1(7) . . ? N1 C8 C9 111.7(7) . . ? C7 C8 C9 125.3(8) . . ? N2 C9 N4 108.4(7) . . ? N2 C9 C8 119.6(8) . . ? N4 C9 C8 132.0(8) . . ? N3 C10 N4 111.8(8) . . ? N3 C10 H10 124.1 . . ? N4 C10 H10 124.1 . . ? C16 C11 C12 122.2(9) . . ? C16 C11 N4 119.0(8) . . ? C12 C11 N4 118.8(8) . . ? C11 C12 C13 118.7(9) . . ? C11 C12 H12 120.7 . . ? C13 C12 H12 120.7 . . ? C12 C13 C14 120.0(10) . . ? C12 C13 H13 120.0 . . ? C14 C13 H13 120.0 . . ? C15 C14 C13 120.6(10) . . ? C15 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? C14 C15 C16 118.8(10) . . ? C14 C15 H15 120.6 . . ? C16 C15 H15 120.6 . . ? C11 C16 C15 119.7(9) . . ? C11 C16 H16 120.2 . . ? C15 C16 H16 120.2 . . ? O4 C17 Re2 176.4(9) . . ? O5 C18 Re2 179.7(9) . . ? O6 C19 Re2 176.7(8) . . ? N5 C20 C21 123.7(9) . . ? N5 C20 H20 118.1 . . ? C21 C20 H20 118.1 . . ? C20 C21 C22 119.2(9) . . ? C20 C21 H21 120.4 . . ? C22 C21 H21 120.4 . . ? C23 C22 C21 118.1(9) . . ? C23 C22 H22 120.9 . . ? C21 C22 H22 120.9 . . ? C22 C23 C24 120.2(9) . . ? C22 C23 H23 119.9 . . ? C24 C23 H23 119.9 . . ? N5 C24 C23 120.7(8) . . ? N5 C24 C25 111.9(8) . . ? C23 C24 C25 127.3(8) . . ? N6 C25 N8 109.6(8) . . ? N6 C25 C24 119.8(8) . . ? N8 C25 C24 130.5(8) . . ? N7 C26 N8 111.8(8) . . ? N7 C26 H26 124.1 . . ? N8 C26 H26 124.1 . . ? C32 C27 C28 121.3(9) . . ? C32 C27 N8 119.1(8) . . ? C28 C27 N8 119.6(8) . . ? C29 C28 C27 119.3(9) . . ? C29 C28 H28 120.4 . . ? C27 C28 H28 120.4 . . ? C30 C29 C28 119.1(9) . . ? C30 C29 H29 120.5 . . ? C28 C29 H29 120.5 . . ? C29 C30 C31 121.1(10) . . ? C29 C30 H30 119.4 . . ? C31 C30 H30 119.4 . . ? C32 C31 C30 119.9(10) . . ? C32 C31 H31 120.1 . . ? C30 C31 H31 120.1 . . ? C31 C32 C27 119.3(9) . . ? C31 C32 H32 120.3 . . ? C27 C32 H32 120.3 . . ? 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 C3 1.869(10) . ? Re1 C2 1.902(11) . ? Re1 C1 1.935(10) . ? Re1 N2 2.147(7) . ? Re1 N1 2.200(7) . ? Re1 Cl1 2.474(2) . ? Re2 C19 1.895(10) . ? Re2 C17 1.899(10) . ? Re2 C18 1.900(10) . ? Re2 N6 2.157(7) . ? Re2 N5 2.191(7) . ? Re2 Cl2 2.476(2) . ? O1 C1 1.140(11) . ? O2 C2 1.171(11) . ? O3 C3 1.182(10) . ? O4 C17 1.150(10) . ? O5 C18 1.148(10) . ? O6 C19 1.159(10) . ? N1 C4 1.328(10) . ? N1 C8 1.358(10) . ? N2 C9 1.309(10) . ? N2 N3 1.382(9) . ? N3 C10 1.297(11) . ? N4 C9 1.357(10) . ? N4 C10 1.380(10) . ? N4 C11 1.459(10) . ? N5 C20 1.328(10) . ? N5 C24 1.367(10) . ? N6 C25 1.309(10) . ? N6 N7 1.366(9) . ? N7 C26 1.314(11) . ? N8 C25 1.362(10) . ? N8 C26 1.373(11) . ? N8 C27 1.434(10) . ? C4 C5 1.379(12) . ? C4 H4 0.9500 . ? C5 C6 1.381(12) . ? C5 H5 0.9500 . ? C6 C7 1.376(11) . ? C6 H6 0.9500 . ? C7 C8 1.390(11) . ? C7 H7 0.9500 . ? C8 C9 1.459(11) . ? C10 H10 0.9500 . ? C11 C16 1.351(12) . ? C11 C12 1.362(12) . ? C12 C13 1.368(13) . ? C12 H12 0.9500 . ? C13 C14 1.380(15) . ? C13 H13 0.9500 . ? C14 C15 1.371(14) . ? C14 H14 0.9500 . ? C15 C16 1.383(12) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C20 C21 1.356(12) . ? C20 H20 0.9500 . ? C21 C22 1.387(12) . ? C21 H21 0.9500 . ? C22 C23 1.376(11) . ? C22 H22 0.9500 . ? C23 C24 1.381(12) . ? C23 H23 0.9500 . ? C24 C25 1.465(11) . ? C26 H26 0.9500 . ? C27 C32 1.385(11) . ? C27 C28 1.386(12) . ? C28 C29 1.384(12) . ? C28 H28 0.9500 . ? C29 C30 1.380(14) . ? C29 H29 0.9500 . ? C30 C31 1.392(13) . ? C30 H30 0.9500 . ? C31 C32 1.359(13) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ?