#------------------------------------------------------------------------------ #$Date: 2021-10-13 01:55:19 +0300 (Wed, 13 Oct 2021) $ #$Revision: 269903 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/85/7708545.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_7708545 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 'C21 H19 Cl4 N4 O3 Re' _chemical_formula_weight 703.40 _space_group_crystal_system orthorhombic _space_group_IT_number 61 _space_group_name_Hall '-P 2ac 2ab' _space_group_name_H-M_alt 'P b c a' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _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 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 10.9645(7) _cell_length_b 18.8237(11) _cell_length_c 25.0238(15) _cell_measurement_reflns_used 9977 _cell_measurement_temperature 193(2) _cell_measurement_theta_max 29.33 _cell_measurement_theta_min 2.97 _cell_volume 5164.7(5) _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 0.994 _diffrn_measured_fraction_theta_max 0.987 _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 0.0665 _diffrn_reflns_av_unetI/netI 0.0244 _diffrn_reflns_Laue_measured_fraction_full 0.994 _diffrn_reflns_Laue_measured_fraction_max 0.987 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_number 165560 _diffrn_reflns_point_group_measured_fraction_full 0.994 _diffrn_reflns_point_group_measured_fraction_max 0.987 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 30.904 _diffrn_reflns_theta_min 3.285 _diffrn_source 'Incoatec microfocus sealed tube' _exptl_absorpt_coefficient_mu 5.149 _exptl_absorpt_correction_T_max 0.7461 _exptl_absorpt_correction_T_min 0.6424 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Bruker-AXS)' _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.809 _exptl_crystal_description plate _exptl_crystal_F_000 2720 _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.120 _exptl_crystal_size_min 0.040 _refine_diff_density_max 1.323 _refine_diff_density_min -1.303 _refine_diff_density_rms 0.119 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 301 _refine_ls_number_reflns 8050 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.090 _refine_ls_R_factor_all 0.0456 _refine_ls_R_factor_gt 0.0284 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0034P)^2^+16.9566P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0513 _refine_ls_wR_factor_ref 0.0561 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6232 _reflns_number_total 8050 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1dt02161c2.cif _cod_data_source_block 2 _cod_database_code 7708545 _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 0.426 _shelx_estimated_absorpt_t_max 0.821 _shelx_res_file ; TITL cvb5_131_a.res in Pbca cvb5_131_a.res created by SHELXL-2018/3 at 18:43:36 on 19-Mar-2021 CELL 0.71073 10.9645 18.8237 25.0238 90.000 90.000 90.000 ZERR 8.000 0.0007 0.0011 0.0015 0.000 0.000 0.000 LATT 1 SYMM 1/2-X, -Y, 1/2+Z SYMM -X, 1/2+Y, 1/2-Z SYMM 1/2+X, 1/2-Y, -Z SFAC C H N O Cl Re UNIT 168 152 32 24 32 8 OMIT 1 1 2 OMIT 0 2 2 OMIT 0 2 0 OMIT 0 2 1 OMIT 1 0 2 OMIT 0 0 2 OMIT 1 1 1 OMIT 1 2 1 OMIT 5 4 11 OMIT 0 0 4 OMIT 2 4 18 OMIT 1 2 3 OMIT 2 2 0 OMIT 2 2 1 OMIT 1 4 1 OMIT 0 2 3 OMIT 0 2 5 OMIT 2 0 0 OMIT 1 1 3 OMIT 2 3 1 OMIT 1 2 5 OMIT 0 4 1 L.S. 10 ACTA BOND $H FMAP 2 PLAN 20 SIZE 0.040 0.120 0.200 TEMP -80.1500 WGHT 0.003400 16.956600 FVAR 0.14282 RE1 6 0.727651 0.644333 0.569778 11.00000 0.02293 0.01705 = 0.02218 -0.00338 0.00031 0.00114 CL1 5 0.879528 0.681566 0.502089 11.00000 0.02951 0.02248 = 0.03707 0.00143 0.00722 0.00013 O1 4 0.633615 0.796023 0.586637 11.00000 0.07022 0.02498 = 0.05106 -0.00713 -0.00093 0.01495 O2 4 0.903657 0.669817 0.662949 11.00000 0.03804 0.07395 = 0.04120 -0.01886 -0.01284 0.00491 O3 4 0.532254 0.595686 0.648659 11.00000 0.04905 0.04769 = 0.04150 -0.00468 0.01503 -0.01298 N1 3 0.619788 0.613965 0.499160 11.00000 0.02146 0.02221 = 0.02663 -0.00263 -0.00043 0.00216 N2 3 0.790501 0.540307 0.546974 11.00000 0.02499 0.01529 = 0.02053 -0.00255 -0.00116 0.00330 N3 3 0.882076 0.497511 0.565948 11.00000 0.02778 0.01970 = 0.02381 -0.00149 -0.00508 0.00353 N4 3 0.812046 0.454986 0.489346 11.00000 0.02419 0.01624 = 0.02334 -0.00366 -0.00171 0.00244 C1 1 0.667623 0.739268 0.579791 11.00000 0.03257 0.02567 = 0.02857 -0.00141 -0.00150 0.00243 C2 1 0.837544 0.660557 0.628113 11.00000 0.02873 0.02958 = 0.03403 -0.00667 0.00378 0.00231 C3 1 0.606632 0.612680 0.619098 11.00000 0.03059 0.02565 = 0.02924 -0.00883 -0.00148 -0.00080 C4 1 0.527882 0.652334 0.478808 11.00000 0.02817 0.03119 = 0.03597 -0.00265 -0.00263 0.00792 AFIX 43 H4 2 0.507571 0.696212 0.495320 11.00000 -1.20000 AFIX 0 C5 1 0.461471 0.630692 0.434803 11.00000 0.03157 0.04103 = 0.03967 0.00057 -0.01000 0.01172 AFIX 43 H5 2 0.397363 0.659506 0.421297 11.00000 -1.20000 AFIX 0 C6 1 0.489245 0.566735 0.410649 11.00000 0.03249 0.04663 = 0.03504 -0.00427 -0.01402 0.00305 AFIX 43 H6 2 0.443769 0.550709 0.380667 11.00000 -1.20000 AFIX 0 C7 1 0.584636 0.526123 0.430795 11.00000 0.02876 0.03000 = 0.03095 -0.00544 -0.00624 0.00047 AFIX 43 H7 2 0.605771 0.482040 0.414799 11.00000 -1.20000 AFIX 0 C8 1 0.648117 0.551326 0.474661 11.00000 0.01989 0.02082 = 0.02325 0.00003 -0.00009 0.00095 C9 1 0.748656 0.515041 0.501541 11.00000 0.02263 0.01571 = 0.02146 0.00041 0.00058 -0.00081 C10 1 0.892717 0.446895 0.530555 11.00000 0.02934 0.01983 = 0.02677 -0.00107 -0.00424 0.00465 AFIX 43 H10 2 0.949664 0.409014 0.533136 11.00000 -1.20000 AFIX 0 C11 1 0.803297 0.409770 0.442748 11.00000 0.02424 0.01893 = 0.02299 -0.00310 0.00036 0.00174 C12 1 0.834304 0.435841 0.393242 11.00000 0.03501 0.02154 = 0.02802 0.00053 0.00306 -0.00333 AFIX 43 H12 2 0.861595 0.483451 0.389293 11.00000 -1.20000 AFIX 0 C13 1 0.825066 0.391433 0.349129 11.00000 0.03285 0.03398 = 0.02098 -0.00042 0.00324 0.00095 AFIX 43 H13 2 0.844791 0.409544 0.314764 11.00000 -1.20000 AFIX 0 C14 1 0.787871 0.321475 0.353922 11.00000 0.02335 0.02998 = 0.02468 -0.00745 -0.00132 0.00221 C15 1 0.757963 0.296572 0.404932 11.00000 0.04376 0.01874 = 0.03055 -0.00380 0.00117 -0.00350 AFIX 43 H15 2 0.732255 0.248705 0.409163 11.00000 -1.20000 AFIX 0 C16 1 0.765013 0.340178 0.449408 11.00000 0.03817 0.01851 = 0.02620 -0.00101 0.00293 -0.00139 AFIX 43 H16 2 0.744006 0.322711 0.483815 11.00000 -1.20000 AFIX 0 C17 1 0.776883 0.270467 0.306315 11.00000 0.03940 0.03511 = 0.02826 -0.01231 -0.00671 0.00352 C18 1 0.848399 0.202107 0.317637 11.00000 0.09078 0.04148 = 0.04861 -0.02023 -0.01613 0.02253 AFIX 137 H18A 2 0.810981 0.176963 0.347756 11.00000 -1.50000 H18B 2 0.933015 0.214054 0.326489 11.00000 -1.50000 H18C 2 0.846911 0.171612 0.285903 11.00000 -1.50000 AFIX 0 C19 1 0.641440 0.254343 0.297882 11.00000 0.05009 0.06566 = 0.04673 -0.02467 -0.00489 -0.01622 AFIX 137 H19A 2 0.608474 0.231235 0.329866 11.00000 -1.50000 H19B 2 0.631831 0.222710 0.267064 11.00000 -1.50000 H19C 2 0.597283 0.298758 0.291318 11.00000 -1.50000 AFIX 0 C20 1 0.827446 0.303648 0.255105 11.00000 0.04880 0.06142 = 0.02651 -0.01281 -0.00113 -0.00173 AFIX 137 H20A 2 0.820819 0.269441 0.225725 11.00000 -1.50000 H20B 2 0.913277 0.316321 0.260440 11.00000 -1.50000 H20C 2 0.780636 0.346442 0.246340 11.00000 -1.50000 AFIX 0 C21 1 0.387856 0.478055 0.804134 11.00000 0.05790 0.04841 = 0.03413 -0.00387 0.00978 0.01018 AFIX 13 H21 2 0.392867 0.511228 0.835270 11.00000 -1.20000 AFIX 0 CL2 5 0.430461 0.524261 0.746396 11.00000 0.11987 0.06696 = 0.04752 0.01337 0.00888 0.00602 CL3 5 0.239797 0.447041 0.799170 11.00000 0.05505 0.26044 = 0.10052 -0.06333 0.03354 -0.03678 CL4 5 0.489178 0.408795 0.814479 11.00000 0.11096 0.05609 = 0.07018 0.00117 -0.00241 0.03122 HKLF 4 REM cvb5_131_a.res in Pbca REM wR2 = 0.056148, GooF = S = 1.09036, Restrained GooF = 1.09036 for all data REM R1 = 0.028430 for 6232 Fo > 4sig(Fo) and 0.045590 for all 8050 data REM 301 parameters refined using 0 restraints END WGHT 0.0034 16.9554 REM Highest difference peak 1.323, deepest hole -1.303, 1-sigma level 0.119 Q1 1 0.3397 0.5130 0.7480 11.00000 0.05 1.32 Q2 1 0.4125 0.3985 0.8193 11.00000 0.05 0.82 Q3 1 0.2357 0.4887 0.8096 11.00000 0.05 0.64 Q4 1 0.2353 0.4514 0.7792 11.00000 0.05 0.62 Q5 1 0.2578 0.4873 0.8455 11.00000 0.05 0.62 Q6 1 0.2309 0.3986 0.8201 11.00000 0.05 0.60 Q7 1 0.5311 0.4408 0.7924 11.00000 0.05 0.59 Q8 1 0.7622 0.2292 0.4910 11.00000 0.05 0.58 Q9 1 0.8043 0.6465 0.5689 11.00000 0.05 0.58 Q10 1 0.6912 0.7037 0.5876 11.00000 0.05 0.51 Q11 1 0.2378 0.4303 0.7255 11.00000 0.05 0.50 Q12 1 0.7419 0.6270 0.5915 11.00000 0.05 0.48 Q13 1 0.6636 0.6806 0.6015 11.00000 0.05 0.48 Q14 1 0.7619 0.4792 0.3293 11.00000 0.05 0.47 Q15 1 0.7853 0.6473 0.6101 11.00000 0.05 0.44 Q16 1 0.7309 0.7169 0.5690 11.00000 0.05 0.44 Q17 1 0.7427 0.1177 0.2618 11.00000 0.05 0.44 Q18 1 0.6015 0.5313 0.7578 11.00000 0.05 0.43 Q19 1 0.8215 0.6324 0.5372 11.00000 0.05 0.43 Q20 1 0.5799 0.4909 0.5184 11.00000 0.05 0.43 ; _shelx_res_checksum 16253 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, 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 0.72765(2) 0.64433(2) 0.56978(2) 0.02072(3) Uani 1 1 d . . . . . Cl1 Cl 0.87953(8) 0.68157(4) 0.50209(4) 0.02969(17) Uani 1 1 d . . . . . O1 O 0.6336(3) 0.79602(14) 0.58664(12) 0.0488(8) Uani 1 1 d . . . . . O2 O 0.9037(3) 0.66982(18) 0.66295(12) 0.0511(8) Uani 1 1 d . . . . . O3 O 0.5323(3) 0.59569(16) 0.64866(11) 0.0461(7) Uani 1 1 d . . . . . N1 N 0.6198(2) 0.61397(14) 0.49916(11) 0.0234(5) Uani 1 1 d . . . . . N2 N 0.7905(2) 0.54031(13) 0.54697(10) 0.0203(5) Uani 1 1 d . . . . . N3 N 0.8821(2) 0.49751(13) 0.56595(11) 0.0238(5) Uani 1 1 d . . . . . N4 N 0.8120(2) 0.45499(13) 0.48935(10) 0.0213(5) Uani 1 1 d . . . . . C1 C 0.6676(3) 0.73927(18) 0.57979(13) 0.0289(7) Uani 1 1 d . . . . . C2 C 0.8375(3) 0.66056(18) 0.62811(15) 0.0308(7) Uani 1 1 d . . . . . C3 C 0.6066(3) 0.61268(18) 0.61910(14) 0.0285(7) Uani 1 1 d . . . . . C4 C 0.5279(3) 0.6523(2) 0.47881(14) 0.0318(7) Uani 1 1 d . . . . . H4 H 0.507571 0.696212 0.495320 0.038 Uiso 1 1 calc R U . . . C5 C 0.4615(3) 0.6307(2) 0.43480(16) 0.0374(8) Uani 1 1 d . . . . . H5 H 0.397363 0.659506 0.421297 0.045 Uiso 1 1 calc R U . . . C6 C 0.4892(3) 0.5667(2) 0.41065(15) 0.0381(9) Uani 1 1 d . . . . . H6 H 0.443769 0.550709 0.380667 0.046 Uiso 1 1 calc R U . . . C7 C 0.5846(3) 0.52612(18) 0.43080(14) 0.0299(7) Uani 1 1 d . . . . . H7 H 0.605771 0.482040 0.414799 0.036 Uiso 1 1 calc R U . . . C8 C 0.6481(3) 0.55133(16) 0.47466(12) 0.0213(6) Uani 1 1 d . . . . . C9 C 0.7487(3) 0.51504(15) 0.50154(12) 0.0199(6) Uani 1 1 d . . . . . C10 C 0.8927(3) 0.44689(17) 0.53055(13) 0.0253(7) Uani 1 1 d . . . . . H10 H 0.949664 0.409014 0.533136 0.030 Uiso 1 1 calc R U . . . C11 C 0.8033(3) 0.40977(16) 0.44275(12) 0.0221(6) Uani 1 1 d . . . . . C12 C 0.8343(3) 0.43584(18) 0.39324(13) 0.0282(7) Uani 1 1 d . . . . . H12 H 0.861595 0.483451 0.389293 0.034 Uiso 1 1 calc R U . . . C13 C 0.8251(3) 0.39143(19) 0.34913(13) 0.0293(7) Uani 1 1 d . . . . . H13 H 0.844791 0.409544 0.314764 0.035 Uiso 1 1 calc R U . . . C14 C 0.7879(3) 0.32148(18) 0.35392(13) 0.0260(7) Uani 1 1 d . . . . . C15 C 0.7580(3) 0.29657(17) 0.40493(13) 0.0310(8) Uani 1 1 d . . . . . H15 H 0.732255 0.248705 0.409163 0.037 Uiso 1 1 calc R U . . . C16 C 0.7650(3) 0.34018(16) 0.44941(13) 0.0276(7) Uani 1 1 d . . . . . H16 H 0.744006 0.322711 0.483815 0.033 Uiso 1 1 calc R U . . . C17 C 0.7769(4) 0.2705(2) 0.30631(14) 0.0343(8) Uani 1 1 d . . . . . C18 C 0.8484(5) 0.2021(2) 0.31764(19) 0.0603(14) Uani 1 1 d . . . . . H18A H 0.810981 0.176963 0.347756 0.090 Uiso 1 1 calc R U . . . H18B H 0.933015 0.214054 0.326489 0.090 Uiso 1 1 calc R U . . . H18C H 0.846911 0.171612 0.285903 0.090 Uiso 1 1 calc R U . . . C19 C 0.6414(4) 0.2543(3) 0.29788(18) 0.0542(12) Uani 1 1 d . . . . . H19A H 0.608474 0.231235 0.329866 0.081 Uiso 1 1 calc R U . . . H19B H 0.631831 0.222710 0.267064 0.081 Uiso 1 1 calc R U . . . H19C H 0.597283 0.298758 0.291318 0.081 Uiso 1 1 calc R U . . . C20 C 0.8274(4) 0.3036(2) 0.25511(15) 0.0456(10) Uani 1 1 d . . . . . H20A H 0.820819 0.269441 0.225725 0.068 Uiso 1 1 calc R U . . . H20B H 0.913277 0.316321 0.260440 0.068 Uiso 1 1 calc R U . . . H20C H 0.780636 0.346442 0.246340 0.068 Uiso 1 1 calc R U . . . C21 C 0.3879(4) 0.4781(2) 0.80413(17) 0.0468(10) Uani 1 1 d . . . . . H21 H 0.392867 0.511228 0.835270 0.056 Uiso 1 1 calc R U . . . Cl2 Cl 0.43046(17) 0.52426(8) 0.74640(5) 0.0781(4) Uani 1 1 d . . . . . Cl3 Cl 0.23980(16) 0.44704(16) 0.79917(8) 0.1387(10) Uani 1 1 d . . . . . Cl4 Cl 0.48918(16) 0.40879(7) 0.81448(6) 0.0791(4) Uani 1 1 d . . . . . 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 0.02293(5) 0.01705(5) 0.02218(5) -0.00338(5) 0.00031(5) 0.00114(5) Cl1 0.0295(4) 0.0225(4) 0.0371(4) 0.0014(3) 0.0072(3) 0.0001(3) O1 0.070(2) 0.0250(13) 0.0511(17) -0.0071(12) -0.0009(15) 0.0149(13) O2 0.0380(16) 0.074(2) 0.0412(16) -0.0189(15) -0.0128(13) 0.0049(15) O3 0.0490(17) 0.0477(17) 0.0415(16) -0.0047(13) 0.0150(14) -0.0130(14) N1 0.0215(13) 0.0222(13) 0.0266(13) -0.0026(11) -0.0004(11) 0.0022(10) N2 0.0250(14) 0.0153(11) 0.0205(12) -0.0026(9) -0.0012(10) 0.0033(10) N3 0.0278(13) 0.0197(12) 0.0238(13) -0.0015(11) -0.0051(11) 0.0035(10) N4 0.0242(13) 0.0162(12) 0.0233(13) -0.0037(10) -0.0017(10) 0.0024(10) C1 0.0326(18) 0.0257(16) 0.0286(18) -0.0014(13) -0.0015(14) 0.0024(14) C2 0.0287(18) 0.0296(18) 0.0340(18) -0.0067(14) 0.0038(14) 0.0023(14) C3 0.0306(18) 0.0257(17) 0.0292(17) -0.0088(14) -0.0015(14) -0.0008(14) C4 0.0282(17) 0.0312(19) 0.0360(18) -0.0026(15) -0.0026(14) 0.0079(14) C5 0.0316(18) 0.041(2) 0.040(2) 0.0006(17) -0.0100(16) 0.0117(15) C6 0.0325(19) 0.047(2) 0.0350(19) -0.0043(17) -0.0140(16) 0.0030(17) C7 0.0288(17) 0.0300(17) 0.0309(17) -0.0054(15) -0.0062(15) 0.0005(13) C8 0.0199(14) 0.0208(15) 0.0232(15) 0.0000(12) -0.0001(12) 0.0009(11) C9 0.0226(16) 0.0157(13) 0.0215(14) 0.0004(11) 0.0006(11) -0.0008(10) C10 0.0293(17) 0.0198(15) 0.0268(16) -0.0011(12) -0.0042(13) 0.0047(12) C11 0.0242(15) 0.0189(14) 0.0230(15) -0.0031(11) 0.0004(11) 0.0017(11) C12 0.0350(19) 0.0215(15) 0.0280(16) 0.0005(13) 0.0031(14) -0.0033(14) C13 0.0328(18) 0.0340(18) 0.0210(15) -0.0004(14) 0.0032(14) 0.0010(15) C14 0.0233(16) 0.0300(17) 0.0247(15) -0.0075(13) -0.0013(12) 0.0022(13) C15 0.044(2) 0.0187(14) 0.0305(17) -0.0038(13) 0.0012(15) -0.0035(14) C16 0.0382(18) 0.0185(14) 0.0262(15) -0.0010(11) 0.0029(14) -0.0014(13) C17 0.0394(19) 0.0351(19) 0.0283(17) -0.0123(14) -0.0067(16) 0.0035(16) C18 0.091(4) 0.041(2) 0.049(3) -0.020(2) -0.016(3) 0.023(3) C19 0.050(3) 0.066(3) 0.047(2) -0.025(2) -0.005(2) -0.016(2) C20 0.049(2) 0.061(3) 0.0265(18) -0.0128(19) -0.0011(17) -0.002(2) C21 0.058(3) 0.048(2) 0.034(2) -0.0039(18) 0.0098(19) 0.010(2) Cl2 0.1199(13) 0.0670(8) 0.0475(7) 0.0134(7) 0.0089(8) 0.0060(9) Cl3 0.0550(9) 0.260(3) 0.1005(13) -0.0633(17) 0.0335(9) -0.0368(14) Cl4 0.1110(13) 0.0561(8) 0.0702(9) 0.0012(7) -0.0024(8) 0.0312(8) 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 89.67(15) . . ? C3 Re1 C1 88.16(15) . . ? C2 Re1 C1 88.16(14) . . ? C3 Re1 N2 96.32(12) . . ? C2 Re1 N2 98.37(12) . . ? C1 Re1 N2 172.08(12) . . ? C3 Re1 N1 93.70(13) . . ? C2 Re1 N1 171.87(12) . . ? C1 Re1 N1 99.33(12) . . ? N2 Re1 N1 73.92(10) . . ? C3 Re1 Cl1 176.99(10) . . ? C2 Re1 Cl1 93.04(11) . . ? C1 Re1 Cl1 93.23(11) . . ? N2 Re1 Cl1 82.00(7) . . ? N1 Re1 Cl1 83.44(7) . . ? C4 N1 C8 117.8(3) . . ? C4 N1 Re1 124.7(2) . . ? C8 N1 Re1 117.6(2) . . ? C9 N2 N3 110.0(2) . . ? C9 N2 Re1 116.51(19) . . ? N3 N2 Re1 132.57(19) . . ? C10 N3 N2 105.0(2) . . ? C9 N4 C10 104.7(2) . . ? C9 N4 C11 129.4(3) . . ? C10 N4 C11 125.8(3) . . ? O1 C1 Re1 178.5(3) . . ? O2 C2 Re1 179.5(3) . . ? O3 C3 Re1 177.9(3) . . ? N1 C4 C5 122.7(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 118.5(3) . . ? C8 C7 H7 120.7 . . ? C6 C7 H7 120.7 . . ? N1 C8 C7 122.6(3) . . ? N1 C8 C9 111.6(3) . . ? C7 C8 C9 125.8(3) . . ? N2 C9 N4 108.4(3) . . ? N2 C9 C8 119.5(3) . . ? N4 C9 C8 132.1(3) . . ? N3 C10 N4 111.9(3) . . ? N3 C10 H10 124.1 . . ? N4 C10 H10 124.1 . . ? C12 C11 C16 121.4(3) . . ? C12 C11 N4 120.0(3) . . ? C16 C11 N4 118.6(3) . . ? C11 C12 C13 118.9(3) . . ? C11 C12 H12 120.5 . . ? C13 C12 H12 120.5 . . ? C14 C13 C12 121.7(3) . . ? C14 C13 H13 119.1 . . ? C12 C13 H13 119.1 . . ? C13 C14 C15 117.8(3) . . ? C13 C14 C17 123.5(3) . . ? C15 C14 C17 118.7(3) . . ? C16 C15 C14 121.4(3) . . ? C16 C15 H15 119.3 . . ? C14 C15 H15 119.3 . . ? C15 C16 C11 118.7(3) . . ? C15 C16 H16 120.6 . . ? C11 C16 H16 120.6 . . ? C20 C17 C19 108.5(3) . . ? C20 C17 C18 108.2(4) . . ? C19 C17 C18 110.8(4) . . ? C20 C17 C14 111.5(3) . . ? C19 C17 C14 107.9(3) . . ? C18 C17 C14 110.0(3) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? Cl3 C21 Cl4 111.0(3) . . ? Cl3 C21 Cl2 111.0(3) . . ? Cl4 C21 Cl2 109.0(2) . . ? Cl3 C21 H21 108.6 . . ? Cl4 C21 H21 108.6 . . ? Cl2 C21 H21 108.6 . . ? 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 Re1 C3 1.908(4) . ? Re1 C2 1.917(4) . ? Re1 C1 1.921(3) . ? Re1 N2 2.153(2) . ? Re1 N1 2.202(3) . ? Re1 Cl1 2.4766(8) . ? O1 C1 1.144(4) . ? O2 C2 1.147(4) . ? O3 C3 1.147(4) . ? N1 C4 1.340(4) . ? N1 C8 1.365(4) . ? N2 C9 1.315(4) . ? N2 N3 1.372(3) . ? N3 C10 1.306(4) . ? N4 C9 1.362(4) . ? N4 C10 1.367(4) . ? N4 C11 1.447(4) . ? C4 C5 1.382(5) . ? C4 H4 0.9500 . ? C5 C6 1.381(5) . ? C5 H5 0.9500 . ? C6 C7 1.390(5) . ? C6 H6 0.9500 . ? C7 C8 1.384(4) . ? C7 H7 0.9500 . ? C8 C9 1.461(4) . ? C10 H10 0.9500 . ? C11 C12 1.375(4) . ? C11 C16 1.386(4) . ? C12 C13 1.388(5) . ? C12 H12 0.9500 . ? C13 C14 1.384(5) . ? C13 H13 0.9500 . ? C14 C15 1.399(5) . ? C14 C17 1.535(4) . ? C15 C16 1.385(4) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 C20 1.530(6) . ? C17 C19 1.530(6) . ? C17 C18 1.533(6) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 Cl3 1.730(5) . ? C21 Cl4 1.732(5) . ? C21 Cl2 1.750(4) . ? C21 H21 1.0000 . ?