#------------------------------------------------------------------------------ #$Date: 2023-05-04 08:23:17 +0300 (Thu, 04 May 2023) $ #$Revision: 282980 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/71/29/7712930.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_7712930 loop_ _publ_author_name 'Stephens, Liam J.' 'Dallerba, Elena' 'Kelderman, Jenisi T. A.' 'Levina, Aviva' 'Werrett, Melissa V.' 'Lay, Peter A.' 'Massi, Massimiliano' 'Andrews, Philip C.' _publ_section_title ; Synthesis and the photophysical and biological properties of tricarbonyl Re(I) diimine complexes bound to thiotetrazolato ligands. ; _journal_issue 15 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 4835 _journal_page_last 4848 _journal_paper_doi 10.1039/d2dt03237f _journal_volume 52 _journal_year 2023 _chemical_formula_moiety 'C23 H15 N6 O4 Re S' _chemical_formula_sum 'C23 H15 N6 O4 Re S' _chemical_formula_weight 657.67 _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_Hall 'P 2ac 2ab' _space_group_name_H-M_alt 'P 21 21 21' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2023-02-21 deposited with the CCDC. 2023-03-14 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 11.5391(3) _cell_length_b 13.2808(3) _cell_length_c 14.9093(4) _cell_measurement_reflns_used 8720 _cell_measurement_temperature 123(2) _cell_measurement_theta_max 29.2420 _cell_measurement_theta_min 3.5250 _cell_volume 2284.83(10) _computing_cell_refinement 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_data_collection 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_data_reduction 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 123(2) _diffrn_detector_area_resol_mean 10.0000 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.839 _diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix' _diffrn_measurement_method '\w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0514 _diffrn_reflns_av_unetI/netI 0.0568 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.839 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 16437 _diffrn_reflns_point_group_measured_fraction_full 0.987 _diffrn_reflns_point_group_measured_fraction_max 0.782 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 30.540 _diffrn_reflns_theta_min 3.359 _diffrn_source 'micro-focus sealed X-ray tube' _exptl_absorpt_coefficient_mu 5.454 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.73194 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.912 _exptl_crystal_description plate _exptl_crystal_F_000 1272 _exptl_crystal_size_max 0.210 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.150 _refine_diff_density_max 0.636 _refine_diff_density_min -0.640 _refine_diff_density_rms 0.127 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.473(10) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 318 _refine_ls_number_reflns 5473 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.000 _refine_ls_R_factor_all 0.0352 _refine_ls_R_factor_gt 0.0296 _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^)+(0.0128P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0520 _refine_ls_wR_factor_ref 0.0538 _reflns_Friedel_coverage 0.670 _reflns_Friedel_fraction_full 0.974 _reflns_Friedel_fraction_max 0.710 _reflns_number_gt 4987 _reflns_number_total 5473 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d2dt03237f2.cif _cod_data_source_block jk-1-09 _cod_database_code 7712930 _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 0.394 _shelx_estimated_absorpt_t_max 0.495 _shelx_res_file ; TITL jk-1-09_a.res in P2(1)2(1)2(1) C:\X-RAYD~1\PASTRU~1\X-RAYD~1\Re9\jk-1-09.res created by SHELXL-2018/3 at 14:47:05 on 25-Nov-2022 CELL 0.71073 11.5391 13.2808 14.9093 90.000 90.000 90.000 ZERR 4.0000 0.0003 0.0003 0.0004 0.000 0.000 0.000 LATT -1 SYMM 0.5-X, -Y, 0.5+Z SYMM 0.5+X, 0.5-Y, -Z SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O RE S UNIT 92 60 24 16 4 4 TWIN -1 0 0 0 -1 0 0 0 -1 2 ACTA FMAP 2 1 53 PLAN 5 0 0 LIST 4 1 SIZE 0.15 0.15 0.21 TEMP -150 L.S. 20 WGHT 0.012800 BASF 0.47293 FVAR 0.24910 RE01 5 0.366634 0.654250 0.715456 11.00000 0.01797 0.01614 = 0.01915 -0.00079 -0.00182 0.00214 S1 6 0.475624 0.542023 0.496824 11.00000 0.03579 0.02012 = 0.02345 0.00286 0.00733 -0.00146 O1 4 0.330492 0.756916 0.533595 11.00000 0.10041 0.02883 = 0.02639 0.00318 -0.01238 0.02172 O2 4 0.100859 0.650581 0.724217 11.00000 0.01875 0.04162 = 0.07397 -0.01981 -0.00372 0.00801 O3 4 0.377355 0.868645 0.792636 11.00000 0.03216 0.01618 = 0.03594 -0.00808 -0.00070 0.00048 O4 4 0.452948 0.093066 0.303712 11.00000 0.02877 0.03066 = 0.02826 -0.01100 0.00244 -0.00487 N3 3 0.379949 0.502199 0.660284 11.00000 0.01630 0.01732 = 0.01859 0.00144 -0.00417 0.00101 N4 3 0.340028 0.420029 0.706982 11.00000 0.02535 0.02002 = 0.02077 0.00039 0.00475 -0.00374 N5 3 0.352752 0.340926 0.659368 11.00000 0.02506 0.02401 = 0.01886 -0.00099 0.00303 -0.00540 N6 3 0.403456 0.369859 0.580155 11.00000 0.02098 0.01919 = 0.01599 0.00077 0.00274 0.00091 N7 3 0.553959 0.646460 0.717055 11.00000 0.02286 0.01684 = 0.01554 -0.00238 0.00223 -0.00085 N8 3 0.404052 0.575032 0.839587 11.00000 0.01841 0.01454 = 0.02331 -0.00564 0.00628 -0.00081 C1 1 0.420253 0.471658 0.580414 11.00000 0.01720 0.02163 = 0.01658 0.00185 -0.00661 0.00061 C2 1 0.419869 0.299125 0.509932 11.00000 0.01666 0.01863 = 0.02323 0.00157 -0.00243 0.00418 C3 1 0.524178 0.296078 0.463278 11.00000 0.01908 0.02246 = 0.03366 -0.00503 0.00015 -0.00101 AFIX 43 H3 2 0.585406 0.340615 0.478787 11.00000 -1.20000 AFIX 0 C4 1 0.538184 0.227287 0.393698 11.00000 0.02040 0.02777 = 0.02472 -0.00319 0.00147 -0.00013 AFIX 43 H4 2 0.609156 0.224851 0.361478 11.00000 -1.20000 AFIX 0 C5 1 0.448725 0.162333 0.371352 11.00000 0.03011 0.01775 = 0.01742 -0.00462 -0.00630 0.00170 C6 1 0.346169 0.165359 0.418827 11.00000 0.02570 0.02085 = 0.02925 -0.00627 -0.00440 -0.00595 AFIX 43 H6 2 0.285254 0.120356 0.403649 11.00000 -1.20000 AFIX 0 C7 1 0.331027 0.233028 0.488143 11.00000 0.02312 0.02621 = 0.02454 -0.00093 0.00233 -0.00046 AFIX 43 H7 2 0.260280 0.234347 0.520710 11.00000 -1.20000 AFIX 0 C8 1 0.547746 0.098603 0.243164 11.00000 0.04191 0.04394 = 0.03015 -0.01536 0.01088 -0.00166 AFIX 137 H8A 2 0.537629 0.048473 0.195569 11.00000 -1.50000 H8B 2 0.620030 0.085098 0.275506 11.00000 -1.50000 H8C 2 0.550994 0.166057 0.216634 11.00000 -1.50000 AFIX 0 C9 1 0.348091 0.715891 0.600558 11.00000 0.04102 0.02107 = 0.03097 -0.00451 -0.00353 0.00306 C10 1 0.201362 0.651463 0.723064 11.00000 0.03047 0.01844 = 0.03296 -0.00348 -0.00398 0.00624 C11 1 0.371013 0.787479 0.765833 11.00000 0.01374 0.03175 = 0.02812 0.00507 0.00393 0.00386 C12 1 0.628221 0.685372 0.658207 11.00000 0.03234 0.02321 = 0.01806 -0.00133 0.00110 -0.00479 AFIX 43 H12 2 0.598211 0.722347 0.608853 11.00000 -1.20000 AFIX 0 C13 1 0.749099 0.674305 0.665674 11.00000 0.02182 0.03399 = 0.02845 -0.00780 0.01123 -0.00936 AFIX 43 H13 2 0.798997 0.704945 0.622968 11.00000 -1.20000 AFIX 0 C14 1 0.794251 0.619255 0.734679 11.00000 0.01775 0.02906 = 0.03806 -0.01035 0.00508 -0.00519 AFIX 43 H14 2 0.875669 0.610090 0.739437 11.00000 -1.20000 AFIX 0 C15 1 0.720271 0.576517 0.798181 11.00000 0.01930 0.01699 = 0.02904 -0.00649 -0.00382 -0.00078 C16 1 0.599645 0.594179 0.788887 11.00000 0.01872 0.01159 = 0.01952 -0.00350 -0.00070 0.00144 C17 1 0.519640 0.555142 0.853153 11.00000 0.01851 0.01503 = 0.01802 -0.00155 -0.00617 0.00229 C18 1 0.560505 0.498772 0.926525 11.00000 0.02942 0.01713 = 0.02673 -0.00054 -0.00794 -0.00083 C19 1 0.478909 0.463236 0.987876 11.00000 0.03766 0.02587 = 0.02672 0.00137 0.00006 0.00044 AFIX 43 H19 2 0.502994 0.426074 1.039031 11.00000 -1.20000 AFIX 0 C20 1 0.364097 0.482372 0.973708 11.00000 0.03902 0.03044 = 0.02311 0.00139 0.00891 -0.00503 AFIX 43 H20 2 0.307779 0.456722 1.014182 11.00000 -1.20000 AFIX 0 C21 1 0.328942 0.540052 0.899226 11.00000 0.01992 0.02783 = 0.02441 -0.00912 0.00268 -0.00352 AFIX 43 H21 2 0.248892 0.554333 0.891490 11.00000 -1.20000 AFIX 0 C22 1 0.758647 0.519973 0.874108 11.00000 0.01740 0.02527 = 0.03781 -0.00175 -0.01151 0.00413 AFIX 43 H22 2 0.839201 0.508077 0.881913 11.00000 -1.20000 AFIX 0 C23 1 0.682983 0.482904 0.935246 11.00000 0.03654 0.01631 = 0.02597 0.00102 -0.01382 0.00240 AFIX 43 H23 2 0.711612 0.445636 0.984916 11.00000 -1.20000 AFIX 0 HKLF 4 REM jk-1-09_a.res in P2(1)2(1)2(1) REM wR2 = 0.0538, GooF = S = 1.000, Restrained GooF = 1.000 for all data REM R1 = 0.0296 for 4987 Fo > 4sig(Fo) and 0.0352 for all 5473 data REM 318 parameters refined using 0 restraints END WGHT 0.0128 0.0000 REM Highest difference peak 0.636, deepest hole -0.640, 1-sigma level 0.127 Q1 1 0.3594 0.7193 0.7840 11.00000 0.05 0.64 Q2 1 0.8907 0.6507 0.7131 11.00000 0.05 0.57 Q3 1 0.6359 0.5398 0.7815 11.00000 0.05 0.56 Q4 1 0.3728 0.7487 0.7159 11.00000 0.05 0.50 Q5 1 0.3667 0.6563 0.8569 11.00000 0.05 0.49 ; _shelx_res_checksum 74579 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Re01 Re 0.36663(2) 0.65425(2) 0.71546(2) 0.01775(7) Uani 1 1 d . . . . . S1 S 0.47562(16) 0.54202(12) 0.49682(12) 0.0265(4) Uani 1 1 d . . . . . O1 O 0.3305(6) 0.7569(4) 0.5336(4) 0.0519(19) Uani 1 1 d . . . . . O2 O 0.1009(4) 0.6506(4) 0.7242(4) 0.0448(13) Uani 1 1 d . . . . . O3 O 0.3774(4) 0.8686(3) 0.7926(3) 0.0281(10) Uani 1 1 d . . . . . O4 O 0.4529(4) 0.0931(3) 0.3037(3) 0.0292(12) Uani 1 1 d . . . . . N3 N 0.3799(5) 0.5022(3) 0.6603(3) 0.0174(11) Uani 1 1 d . . . . . N4 N 0.3400(4) 0.4200(4) 0.7070(4) 0.0220(12) Uani 1 1 d . . . . . N5 N 0.3528(4) 0.3409(4) 0.6594(3) 0.0226(11) Uani 1 1 d . . . . . N6 N 0.4035(4) 0.3699(3) 0.5802(3) 0.0187(12) Uani 1 1 d . . . . . N7 N 0.5540(4) 0.6465(4) 0.7171(4) 0.0184(10) Uani 1 1 d . . . . . N8 N 0.4041(4) 0.5750(4) 0.8396(4) 0.0188(12) Uani 1 1 d . . . . . C1 C 0.4203(5) 0.4717(5) 0.5804(4) 0.0185(13) Uani 1 1 d . . . . . C2 C 0.4199(6) 0.2991(5) 0.5099(4) 0.0195(13) Uani 1 1 d . . . . . C3 C 0.5242(6) 0.2961(5) 0.4633(5) 0.0251(15) Uani 1 1 d . . . . . H3 H 0.585406 0.340615 0.478787 0.030 Uiso 1 1 calc R U . . . C4 C 0.5382(6) 0.2273(5) 0.3937(5) 0.0243(15) Uani 1 1 d . . . . . H4 H 0.609156 0.224851 0.361478 0.029 Uiso 1 1 calc R U . . . C5 C 0.4487(5) 0.1623(5) 0.3714(4) 0.0218(13) Uani 1 1 d . . . . . C6 C 0.3462(5) 0.1654(5) 0.4188(4) 0.0253(14) Uani 1 1 d . . . . . H6 H 0.285254 0.120356 0.403649 0.030 Uiso 1 1 calc R U . . . C7 C 0.3310(6) 0.2330(5) 0.4881(5) 0.0246(15) Uani 1 1 d . . . . . H7 H 0.260280 0.234347 0.520710 0.030 Uiso 1 1 calc R U . . . C8 C 0.5477(7) 0.0986(6) 0.2432(5) 0.039(2) Uani 1 1 d . . . . . H8A H 0.537629 0.048473 0.195569 0.058 Uiso 1 1 calc R U . . . H8B H 0.620030 0.085098 0.275506 0.058 Uiso 1 1 calc R U . . . H8C H 0.550994 0.166057 0.216634 0.058 Uiso 1 1 calc R U . . . C9 C 0.3481(7) 0.7159(5) 0.6006(5) 0.0310(17) Uani 1 1 d . . . . . C10 C 0.2014(5) 0.6515(5) 0.7231(5) 0.0273(14) Uani 1 1 d . . . . . C11 C 0.3710(6) 0.7875(5) 0.7658(4) 0.0245(14) Uani 1 1 d . . . . . C12 C 0.6282(7) 0.6854(4) 0.6582(4) 0.0245(14) Uani 1 1 d . . . . . H12 H 0.598211 0.722347 0.608853 0.029 Uiso 1 1 calc R U . . . C13 C 0.7491(6) 0.6743(5) 0.6657(5) 0.0281(16) Uani 1 1 d . . . . . H13 H 0.798997 0.704945 0.622968 0.034 Uiso 1 1 calc R U . . . C14 C 0.7943(6) 0.6193(5) 0.7347(5) 0.0283(17) Uani 1 1 d . . . . . H14 H 0.875669 0.610090 0.739437 0.034 Uiso 1 1 calc R U . . . C15 C 0.7203(5) 0.5765(4) 0.7982(5) 0.0218(14) Uani 1 1 d . . . . . C16 C 0.5996(5) 0.5942(4) 0.7889(5) 0.0166(12) Uani 1 1 d . . . . . C17 C 0.5196(5) 0.5551(4) 0.8532(4) 0.0172(13) Uani 1 1 d . . . . . C18 C 0.5605(6) 0.4988(5) 0.9265(5) 0.0244(15) Uani 1 1 d . . . . . C19 C 0.4789(7) 0.4632(5) 0.9879(5) 0.0301(16) Uani 1 1 d . . . . . H19 H 0.502994 0.426074 1.039031 0.036 Uiso 1 1 calc R U . . . C20 C 0.3641(8) 0.4824(5) 0.9737(4) 0.0309(15) Uani 1 1 d . . . . . H20 H 0.307779 0.456722 1.014182 0.037 Uiso 1 1 calc R U . . . C21 C 0.3289(6) 0.5401(5) 0.8992(4) 0.0241(15) Uani 1 1 d . . . . . H21 H 0.248892 0.554333 0.891490 0.029 Uiso 1 1 calc R U . . . C22 C 0.7586(6) 0.5200(5) 0.8741(5) 0.0268(16) Uani 1 1 d . . . . . H22 H 0.839201 0.508077 0.881913 0.032 Uiso 1 1 calc R U . . . C23 C 0.6830(6) 0.4829(5) 0.9352(5) 0.0263(16) Uani 1 1 d . . . . . H23 H 0.711612 0.445636 0.984916 0.032 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 Re01 0.01797(11) 0.01614(10) 0.01915(10) -0.00079(11) -0.00182(11) 0.00214(10) S1 0.0358(10) 0.0201(8) 0.0234(8) 0.0029(7) 0.0073(8) -0.0015(7) O1 0.100(6) 0.029(3) 0.026(3) 0.003(2) -0.012(3) 0.022(3) O2 0.019(2) 0.042(3) 0.074(4) -0.020(4) -0.004(2) 0.008(2) O3 0.032(2) 0.016(2) 0.036(3) -0.008(2) -0.001(3) 0.0005(18) O4 0.029(3) 0.031(3) 0.028(3) -0.011(2) 0.002(2) -0.0049(19) N3 0.016(3) 0.017(2) 0.019(3) 0.0014(19) -0.004(2) 0.001(2) N4 0.025(3) 0.020(2) 0.021(3) 0.000(2) 0.005(3) -0.0037(19) N5 0.025(3) 0.024(2) 0.019(2) -0.001(2) 0.003(2) -0.005(3) N6 0.021(3) 0.019(3) 0.016(2) 0.001(2) 0.003(2) 0.0009(19) N7 0.023(2) 0.017(2) 0.016(2) -0.002(4) 0.002(2) -0.001(2) N8 0.018(3) 0.015(2) 0.023(3) -0.006(2) 0.006(2) -0.0008(19) C1 0.017(3) 0.022(3) 0.017(3) 0.002(3) -0.007(3) 0.001(3) C2 0.017(3) 0.019(3) 0.023(3) 0.002(3) -0.002(3) 0.004(2) C3 0.019(3) 0.022(3) 0.034(4) -0.005(3) 0.000(3) -0.001(3) C4 0.020(3) 0.028(4) 0.025(4) -0.003(3) 0.001(3) 0.000(3) C5 0.030(3) 0.018(3) 0.017(3) -0.005(3) -0.006(2) 0.002(3) C6 0.026(4) 0.021(3) 0.029(3) -0.006(3) -0.004(3) -0.006(3) C7 0.023(4) 0.026(3) 0.025(4) -0.001(3) 0.002(3) 0.000(3) C8 0.042(5) 0.044(5) 0.030(4) -0.015(4) 0.011(4) -0.002(4) C9 0.041(5) 0.021(3) 0.031(4) -0.005(3) -0.004(4) 0.003(3) C10 0.030(3) 0.018(3) 0.033(4) -0.003(5) -0.004(3) 0.006(3) C11 0.014(3) 0.032(3) 0.028(4) 0.005(3) 0.004(3) 0.004(3) C12 0.032(4) 0.023(3) 0.018(3) -0.001(2) 0.001(3) -0.005(3) C13 0.022(3) 0.034(4) 0.028(4) -0.008(3) 0.011(3) -0.009(3) C14 0.018(3) 0.029(3) 0.038(5) -0.010(3) 0.005(3) -0.005(3) C15 0.019(3) 0.017(3) 0.029(4) -0.006(3) -0.004(3) -0.001(2) C16 0.019(3) 0.012(3) 0.020(3) -0.003(3) -0.001(3) 0.001(2) C17 0.019(3) 0.015(3) 0.018(3) -0.002(3) -0.006(3) 0.002(2) C18 0.029(4) 0.017(3) 0.027(4) -0.001(3) -0.008(3) -0.001(3) C19 0.038(4) 0.026(4) 0.027(4) 0.001(3) 0.000(3) 0.000(3) C20 0.039(4) 0.030(4) 0.023(3) 0.001(3) 0.009(4) -0.005(4) C21 0.020(3) 0.028(3) 0.024(3) -0.009(3) 0.003(3) -0.004(3) C22 0.017(3) 0.025(4) 0.038(4) -0.002(3) -0.012(3) 0.004(3) C23 0.037(4) 0.016(3) 0.026(4) 0.001(3) -0.014(3) 0.002(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' 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' S S 0.1246 0.1234 '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 C9 Re01 C10 87.1(3) . . ? C9 Re01 C11 87.6(3) . . ? C10 Re01 C11 91.2(3) . . ? C9 Re01 N7 98.2(3) . . ? C10 Re01 N7 174.4(2) . . ? C11 Re01 N7 90.8(2) . . ? C9 Re01 N8 173.6(3) . . ? C10 Re01 N8 98.0(3) . . ? C11 Re01 N8 96.2(2) . . ? N7 Re01 N8 76.6(2) . . ? C9 Re01 N3 93.8(2) . . ? C10 Re01 N3 94.3(3) . . ? C11 Re01 N3 174.4(3) . . ? N7 Re01 N3 83.67(19) . . ? N8 Re01 N3 81.91(18) . . ? C5 O4 C8 117.5(5) . . ? C1 N3 N4 109.0(5) . . ? C1 N3 Re01 129.6(4) . . ? N4 N3 Re01 121.3(4) . . ? N5 N4 N3 109.5(5) . . ? N4 N5 N6 107.3(5) . . ? C1 N6 N5 109.6(5) . . ? C1 N6 C2 129.7(5) . . ? N5 N6 C2 120.4(5) . . ? C12 N7 C16 117.4(5) . . ? C12 N7 Re01 128.1(5) . . ? C16 N7 Re01 114.4(4) . . ? C21 N8 C17 117.9(6) . . ? C21 N8 Re01 127.7(4) . . ? C17 N8 Re01 114.3(4) . . ? N3 C1 N6 104.6(5) . . ? N3 C1 S1 128.4(5) . . ? N6 C1 S1 127.0(5) . . ? C7 C2 C3 120.2(6) . . ? C7 C2 N6 119.5(6) . . ? C3 C2 N6 120.2(6) . . ? C2 C3 C4 119.5(6) . . ? C5 C4 C3 120.1(6) . . ? O4 C5 C6 115.4(6) . . ? O4 C5 C4 124.8(6) . . ? C6 C5 C4 119.8(6) . . ? C5 C6 C7 120.8(6) . . ? C6 C7 C2 119.6(6) . . ? O1 C9 Re01 175.2(7) . . ? O2 C10 Re01 177.4(8) . . ? O3 C11 Re01 176.6(6) . . ? N7 C12 C13 123.1(6) . . ? C14 C13 C12 119.6(6) . . ? C13 C14 C15 119.7(6) . . ? C14 C15 C16 117.8(6) . . ? C14 C15 C22 124.2(6) . . ? C16 C15 C22 117.9(6) . . ? N7 C16 C15 122.2(6) . . ? N7 C16 C17 117.1(5) . . ? C15 C16 C17 120.6(6) . . ? N8 C17 C18 122.8(6) . . ? N8 C17 C16 117.3(5) . . ? C18 C17 C16 119.9(6) . . ? C19 C18 C17 117.6(6) . . ? C19 C18 C23 123.8(7) . . ? C17 C18 C23 118.6(7) . . ? C20 C19 C18 119.4(7) . . ? C19 C20 C21 120.2(7) . . ? N8 C21 C20 122.1(6) . . ? C23 C22 C15 121.6(6) . . ? C22 C23 C18 121.4(7) . . ? 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 Re01 C9 1.911(7) . ? Re01 C10 1.911(6) . ? Re01 C11 1.923(6) . ? Re01 N7 2.164(5) . ? Re01 N8 2.172(5) . ? Re01 N3 2.186(5) . ? S1 C1 1.684(6) . ? O1 C9 1.155(8) . ? O2 C10 1.160(8) . ? O3 C11 1.152(7) . ? O4 C5 1.366(8) . ? O4 C8 1.420(8) . ? N3 C1 1.341(8) . ? N3 N4 1.374(7) . ? N4 N5 1.276(7) . ? N5 N6 1.373(7) . ? N6 C1 1.366(8) . ? N6 C2 1.419(8) . ? N7 C12 1.331(8) . ? N7 C16 1.381(8) . ? N8 C21 1.326(8) . ? N8 C17 1.375(8) . ? C2 C7 1.388(8) . ? C2 C3 1.391(9) . ? C3 C4 1.392(9) . ? C4 C5 1.386(9) . ? C5 C6 1.380(9) . ? C6 C7 1.381(9) . ? C12 C13 1.407(10) . ? C13 C14 1.365(10) . ? C14 C15 1.395(10) . ? C15 C16 1.418(8) . ? C15 C22 1.429(9) . ? C16 C17 1.428(9) . ? C17 C18 1.407(9) . ? C18 C19 1.395(10) . ? C18 C23 1.435(9) . ? C19 C20 1.365(11) . ? C20 C21 1.409(10) . ? C22 C23 1.355(10) . ?