#------------------------------------------------------------------------------ #$Date: 2023-05-04 08:23:17 +0300 (Thu, 04 May 2023) $ #$Revision: 282980 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/71/29/7712934.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_7712934 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 'C22 H18 N7 O3 Re S' _chemical_formula_sum 'C22 H18 N7 O3 Re S' _chemical_formula_weight 646.69 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _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 104.007(6) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 21.2128(12) _cell_length_b 9.4134(4) _cell_length_c 11.9069(6) _cell_measurement_reflns_used 5076 _cell_measurement_temperature 123(2) _cell_measurement_theta_max 30.3820 _cell_measurement_theta_min 3.5250 _cell_volume 2306.9(2) _computing_cell_refinement 'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)' _computing_data_collection 'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)' _computing_data_reduction 'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT (Sheldrick, 2015)' _diffrn_ambient_temperature 123(2) _diffrn_detector_area_resol_mean 10.0000 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _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 0.0880 _diffrn_reflns_av_unetI/netI 0.0645 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 22483 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.999 _diffrn_reflns_theta_min 3.527 _diffrn_source 'micro-focus sealed X-ray tube' _exptl_absorpt_coefficient_mu 5.398 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.68062 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.81a (Rigaku Oxford Diffraction, 2020) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.862 _exptl_crystal_description plate _exptl_crystal_F_000 1256 _exptl_crystal_size_max 0.110 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.080 _refine_diff_density_max 1.902 _refine_diff_density_min -1.071 _refine_diff_density_rms 0.165 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 383 _refine_ls_number_reflns 4532 _refine_ls_number_restraints 49 _refine_ls_restrained_S_all 1.047 _refine_ls_R_factor_all 0.0647 _refine_ls_R_factor_gt 0.0412 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0396P)^2^+4.8509P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0859 _refine_ls_wR_factor_ref 0.0946 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3442 _reflns_number_total 4532 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d2dt03237f2.cif _cod_data_source_block ls-2-108 _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 7712934 _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 0.588 _shelx_estimated_absorpt_t_max 0.672 _shelx_res_file ; TITL ls-2-108_a.res in P2(1)/c C:\X-RAYD~1\PASTRU~1\X-RAYD~1\Re4\ls-2-108.res created by SHELXL-2018/3 at 15:05:26 on 24-Nov-2022 CELL 0.71073 21.2128 9.4134 11.9069 90.000 104.007 90.000 ZERR 4.0000 0.0012 0.0004 0.0006 0.000 0.006 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O RE S UNIT 88 72 28 12 4 4 OMIT -2 52 SADI 0.01 C5 N5 C5' N5' SADI 0.01 N5 C8 N5 C9 N5' C8' N5' C9' SADI 0.01 C2 C3 C3 C4 C4 C5 C5 C6 C6 C7 C7 C2 SADI 0.01 C2 C3' C3' C4' C4' C5' C5' C6' C6' C7' C7' C2 ISOR 0.01 C8 C8' OMIT -2 2 2 OMIT -3 2 2 OMIT -21 5 6 ACTA FMAP 2 1 53 PLAN 5 0 0 SIZE 0.08 0.11 0.1 TEMP -150 L.S. 20 WGHT 0.039600 4.850900 FVAR 0.05456 RE1 5 0.145660 0.368161 0.128756 11.00000 0.02986 0.01398 = 0.02307 -0.00146 0.00459 -0.00012 S1 6 0.275574 0.105500 0.277750 11.00000 0.04582 0.02166 = 0.04086 0.00145 0.00918 0.00528 O1 4 0.197787 0.161662 -0.028263 11.00000 0.04870 0.02136 = 0.03333 -0.00949 0.01382 0.00852 O2 4 0.101137 0.116966 0.254820 11.00000 0.04606 0.02059 = 0.04586 0.00448 0.01579 -0.00240 O3 4 0.016087 0.347983 -0.052941 11.00000 0.03316 0.04790 = 0.02645 -0.00732 -0.00458 -0.00370 N1 3 0.238191 0.383636 0.251337 11.00000 0.03821 0.01301 = 0.02681 0.00050 0.01005 0.00314 N2 3 0.261772 0.512618 0.297967 11.00000 0.03907 0.01613 = 0.03092 -0.00232 0.00387 0.00137 N3 3 0.315140 0.496373 0.375320 11.00000 0.02881 0.02870 = 0.03673 0.00091 0.00030 0.00357 N4 3 0.328042 0.355064 0.379666 11.00000 0.03094 0.03300 = 0.03008 -0.00061 0.00280 0.00097 PART 1 N5 3 0.547827 0.142250 0.699480 10.50000 0.04379 0.05792 = 0.05732 0.00560 -0.00575 0.01687 PART 2 N5' 3 0.557269 0.229827 0.716197 10.50000 0.04631 0.07313 = 0.07325 0.00022 -0.00645 0.04073 PART 0 N6 3 0.177805 0.568419 0.072058 11.00000 0.03172 0.01363 = 0.02565 -0.00068 0.00160 0.00072 N7 3 0.111919 0.528908 0.231756 11.00000 0.02634 0.02161 = 0.02245 -0.00361 0.00027 0.00198 C1 1 0.280658 0.281122 0.303536 11.00000 0.03136 0.02809 = 0.02594 -0.00077 0.00899 -0.00073 C2 1 0.383271 0.303522 0.462756 11.00000 0.02967 0.05042 = 0.03446 0.01285 0.00470 0.00291 PART 1 C3 1 0.445144 0.342058 0.454362 10.50000 0.04029 0.05818 = 0.03324 0.00749 0.00841 0.00851 AFIX 43 H3 2 0.451362 0.403553 0.394700 10.50000 -1.20000 AFIX 0 C4 1 0.497531 0.287598 0.536149 10.50000 0.02797 0.03524 = 0.05202 0.00613 -0.00325 -0.00478 AFIX 43 H4 2 0.539940 0.317347 0.533492 10.50000 -1.20000 AFIX 0 C5 1 0.491446 0.191619 0.622069 10.50000 0.04809 0.03528 = 0.04779 0.00773 -0.01018 0.01343 C6 1 0.429465 0.142150 0.621753 10.50000 0.05664 0.02777 = 0.04619 -0.00638 0.00627 -0.00529 AFIX 43 H6 2 0.423571 0.071849 0.675540 10.50000 -1.20000 AFIX 0 C7 1 0.376298 0.197650 0.541134 10.50000 0.05139 0.04992 = 0.03342 0.02015 -0.00696 0.01175 AFIX 43 H7 2 0.334096 0.162494 0.539412 10.50000 -1.20000 AFIX 0 PART 2 C3' 1 0.429253 0.213546 0.438378 10.50000 0.03116 0.04079 = 0.07311 0.00331 0.00681 0.00494 AFIX 43 H3A 2 0.423080 0.167885 0.365369 10.50000 -1.20000 AFIX 0 C4' 1 0.484959 0.192718 0.525336 10.50000 0.04695 0.05794 = 0.08994 0.01858 0.03055 0.02300 AFIX 43 H4A 2 0.516032 0.127680 0.509805 10.50000 -1.20000 AFIX 0 C5' 1 0.499701 0.257759 0.632923 10.50000 0.01827 0.08623 = 0.04978 0.02946 0.01066 0.00012 C6' 1 0.453126 0.348622 0.656342 10.50000 0.05970 0.11336 = 0.04598 -0.00507 -0.00039 0.04296 AFIX 43 H6A 2 0.459771 0.395726 0.728828 10.50000 -1.20000 AFIX 0 C7' 1 0.396486 0.368790 0.570791 10.50000 0.04897 0.12740 = 0.04686 0.01146 0.00877 0.03776 AFIX 43 H7A 2 0.364642 0.431241 0.587030 10.50000 -1.20000 AFIX 0 PART 1 C8 1 0.610754 0.209756 0.715371 10.50000 0.03654 0.06449 = 0.07100 0.01378 0.00298 0.01542 AFIX 137 H8A 2 0.632153 0.175317 0.656301 10.50000 -1.50000 H8B 2 0.637604 0.186670 0.792424 10.50000 -1.50000 H8C 2 0.605069 0.312941 0.708139 10.50000 -1.50000 AFIX 0 PART 2 C8' 1 0.607872 0.160778 0.673516 10.50000 0.04879 0.08137 = 0.09187 0.00761 0.00473 0.01037 AFIX 137 H8D 2 0.591428 0.070781 0.636362 10.50000 -1.50000 H8E 2 0.645361 0.142214 0.738254 10.50000 -1.50000 H8F 2 0.621072 0.222612 0.617049 10.50000 -1.50000 AFIX 0 PART 1 C9 1 0.540191 0.046323 0.790692 10.50000 0.05008 0.07279 = 0.05830 0.02329 -0.00504 0.01093 AFIX 137 H9A 2 0.520029 0.097190 0.844786 10.50000 -1.50000 H9B 2 0.582887 0.010653 0.832167 10.50000 -1.50000 H9C 2 0.512499 -0.033648 0.756714 10.50000 -1.50000 AFIX 0 PART 2 C9' 1 0.579569 0.332685 0.807986 10.50000 0.06187 0.11833 = 0.03887 0.01182 0.00029 0.02270 AFIX 137 H9D 2 0.605561 0.405808 0.781597 10.50000 -1.50000 H9E 2 0.606202 0.284644 0.876146 10.50000 -1.50000 H9F 2 0.542004 0.377072 0.828207 10.50000 -1.50000 AFIX 0 PART 0 C10 1 0.215454 0.579543 -0.003250 11.00000 0.03479 0.03046 = 0.02272 -0.00064 0.00583 -0.00649 AFIX 43 H10 2 0.222678 0.497799 -0.045227 11.00000 -1.20000 AFIX 0 C11 1 0.243831 0.705855 -0.021309 11.00000 0.04227 0.03562 = 0.03504 0.00357 0.01784 -0.00135 AFIX 43 H11 2 0.271017 0.710322 -0.073968 11.00000 -1.20000 AFIX 0 C12 1 0.232877 0.825376 0.036716 11.00000 0.03702 0.02523 = 0.03431 0.00612 0.00107 -0.00639 AFIX 43 H12 2 0.252256 0.913363 0.024950 11.00000 -1.20000 AFIX 0 C13 1 0.193180 0.815567 0.112546 11.00000 0.04002 0.01029 = 0.03694 -0.00137 -0.00631 0.00009 AFIX 43 H13 2 0.184393 0.897349 0.152969 11.00000 -1.20000 AFIX 0 C14 1 0.166510 0.687181 0.129199 11.00000 0.03302 0.01027 = 0.02652 0.00146 0.00201 0.00128 C15 1 0.125709 0.664407 0.212403 11.00000 0.02452 0.02047 = 0.02712 -0.00576 -0.00075 0.00143 C16 1 0.103809 0.775733 0.269584 11.00000 0.04116 0.02823 = 0.03768 -0.00459 0.00506 0.00019 AFIX 43 H16 2 0.113889 0.871141 0.254625 11.00000 -1.20000 AFIX 0 C17 1 0.067175 0.746498 0.348543 11.00000 0.03840 0.03511 = 0.03703 -0.01016 0.00893 0.00468 AFIX 43 H17 2 0.051912 0.821080 0.388791 11.00000 -1.20000 AFIX 0 C18 1 0.053459 0.607705 0.367277 11.00000 0.03644 0.03976 = 0.03156 -0.00679 0.00933 0.00570 AFIX 43 H18 2 0.028480 0.584666 0.421078 11.00000 -1.20000 AFIX 0 C19 1 0.076064 0.501791 0.307727 11.00000 0.02613 0.02515 = 0.02653 -0.00018 0.00179 0.00052 AFIX 43 H19 2 0.065885 0.405907 0.320942 11.00000 -1.20000 AFIX 0 C20 1 0.179883 0.238299 0.032795 11.00000 0.02948 0.01914 = 0.03380 0.00578 0.00456 -0.00788 C21 1 0.118922 0.207908 0.205379 11.00000 0.02452 0.02523 = 0.02956 -0.00486 0.00598 0.00078 C22 1 0.064505 0.360975 0.016000 11.00000 0.04969 0.01265 = 0.03099 -0.00235 0.01822 -0.00060 HKLF 4 REM ls-2-108_a.res in P2(1)/c REM wR2 = 0.0946, GooF = S = 1.051, Restrained GooF = 1.047 for all data REM R1 = 0.0412 for 3442 Fo > 4sig(Fo) and 0.0647 for all 4532 data REM 383 parameters refined using 49 restraints END WGHT 0.0396 4.8414 REM Highest difference peak 1.902, deepest hole -1.071, 1-sigma level 0.165 Q1 1 0.1843 0.3709 0.1716 11.00000 0.05 1.90 Q2 1 0.0992 0.3654 0.0933 11.00000 0.05 1.78 Q3 1 0.0999 0.3674 0.1387 11.00000 0.05 1.73 Q4 1 0.1852 0.3734 0.0897 11.00000 0.05 1.14 Q5 1 0.1400 0.3039 0.1850 11.00000 0.05 0.72 ; _shelx_res_checksum 86765 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -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 Re1 Re 0.14566(2) 0.36816(3) 0.12876(2) 0.02261(10) Uani 1 1 d . . . . . S1 S 0.27557(10) 0.1055(2) 0.27775(17) 0.0363(5) Uani 1 1 d . . . . . O1 O 0.1978(3) 0.1617(6) -0.0283(4) 0.0338(13) Uani 1 1 d . . . . . O2 O 0.1011(3) 0.1170(6) 0.2548(5) 0.0367(12) Uani 1 1 d . . . . . O3 O 0.0161(3) 0.3480(6) -0.0529(4) 0.0379(14) Uani 1 1 d . . . . . N1 N 0.2382(3) 0.3836(6) 0.2513(5) 0.0256(13) Uani 1 1 d . . . . . N2 N 0.2618(3) 0.5126(6) 0.2980(5) 0.0295(14) Uani 1 1 d . . . . . N3 N 0.3151(3) 0.4964(7) 0.3753(5) 0.0327(15) Uani 1 1 d . . . . . N4 N 0.3280(3) 0.3551(7) 0.3797(5) 0.0321(14) Uani 1 1 d . . . . . N5 N 0.5478(7) 0.142(2) 0.6995(16) 0.056(5) Uani 0.5 1 d D . P A 1 N5' N 0.5573(9) 0.230(2) 0.7162(16) 0.068(6) Uani 0.5 1 d D . P B 2 N6 N 0.1778(3) 0.5684(6) 0.0721(5) 0.0246(13) Uani 1 1 d . . . . . N7 N 0.1119(3) 0.5289(6) 0.2318(5) 0.0244(13) Uani 1 1 d . . . . . C1 C 0.2807(4) 0.2811(8) 0.3035(6) 0.0281(17) Uani 1 1 d . . . . . C2 C 0.3833(4) 0.3035(9) 0.4628(7) 0.039(2) Uani 1 1 d D . . . . C3 C 0.4451(5) 0.342(2) 0.4544(13) 0.044(4) Uani 0.5 1 d D . P A 1 H3 H 0.451362 0.403553 0.394700 0.053 Uiso 0.5 1 calc R U P A 1 C4 C 0.4975(8) 0.288(2) 0.5361(14) 0.041(4) Uani 0.5 1 d D . P A 1 H4 H 0.539940 0.317347 0.533492 0.049 Uiso 0.5 1 calc R U P A 1 C5 C 0.4914(7) 0.192(2) 0.622(2) 0.047(8) Uani 0.5 1 d D . P A 1 C6 C 0.4295(6) 0.1421(18) 0.6218(14) 0.045(4) Uani 0.5 1 d D . P A 1 H6 H 0.423571 0.071849 0.675540 0.054 Uiso 0.5 1 calc R U P A 1 C7 C 0.3763(8) 0.1977(17) 0.5411(13) 0.048(5) Uani 0.5 1 d D . P A 1 H7 H 0.334096 0.162494 0.539412 0.057 Uiso 0.5 1 calc R U P A 1 C3' C 0.4293(6) 0.2135(18) 0.4384(17) 0.049(5) Uani 0.5 1 d D . P B 2 H3A H 0.423080 0.167885 0.365369 0.059 Uiso 0.5 1 calc R U P B 2 C4' C 0.4850(9) 0.193(3) 0.5253(16) 0.063(6) Uani 0.5 1 d D . P B 2 H4A H 0.516032 0.127680 0.509805 0.075 Uiso 0.5 1 calc R U P B 2 C5' C 0.4997(8) 0.258(3) 0.6329(16) 0.051(8) Uani 0.5 1 d D . P B 2 C6' C 0.4531(8) 0.349(3) 0.6563(17) 0.075(8) Uani 0.5 1 d D . P B 2 H6A H 0.459771 0.395726 0.728828 0.090 Uiso 0.5 1 calc R U P B 2 C7' C 0.3965(9) 0.369(3) 0.5708(11) 0.075(8) Uani 0.5 1 d D . P B 2 H7A H 0.364642 0.431241 0.587030 0.090 Uiso 0.5 1 calc R U P B 2 C8 C 0.6108(10) 0.210(3) 0.715(2) 0.059(7) Uani 0.5 1 d D U P A 1 H8A H 0.632153 0.175317 0.656301 0.089 Uiso 0.5 1 calc R U P A 1 H8B H 0.637604 0.186670 0.792424 0.089 Uiso 0.5 1 calc R U P A 1 H8C H 0.605069 0.312941 0.708139 0.089 Uiso 0.5 1 calc R U P A 1 C8' C 0.6079(12) 0.161(4) 0.674(3) 0.076(10) Uani 0.5 1 d D U P B 2 H8D H 0.591428 0.070781 0.636362 0.114 Uiso 0.5 1 calc R U P B 2 H8E H 0.645361 0.142214 0.738254 0.114 Uiso 0.5 1 calc R U P B 2 H8F H 0.621072 0.222612 0.617049 0.114 Uiso 0.5 1 calc R U P B 2 C9 C 0.5402(10) 0.046(2) 0.7907(17) 0.064(6) Uani 0.5 1 d D . P A 1 H9A H 0.520029 0.097190 0.844786 0.095 Uiso 0.5 1 calc R U P A 1 H9B H 0.582887 0.010653 0.832167 0.095 Uiso 0.5 1 calc R U P A 1 H9C H 0.512499 -0.033648 0.756714 0.095 Uiso 0.5 1 calc R U P A 1 C9' C 0.5796(11) 0.333(3) 0.8080(16) 0.075(8) Uani 0.5 1 d D . P B 2 H9D H 0.605561 0.405808 0.781597 0.113 Uiso 0.5 1 calc R U P B 2 H9E H 0.606202 0.284644 0.876146 0.113 Uiso 0.5 1 calc R U P B 2 H9F H 0.542004 0.377072 0.828207 0.113 Uiso 0.5 1 calc R U P B 2 C10 C 0.2155(4) 0.5795(8) -0.0032(6) 0.0295(17) Uani 1 1 d . . . . . H10 H 0.222678 0.497799 -0.045227 0.035 Uiso 1 1 calc R U . . . C11 C 0.2438(4) 0.7059(9) -0.0213(7) 0.0362(19) Uani 1 1 d . . . . . H11 H 0.271017 0.710322 -0.073968 0.043 Uiso 1 1 calc R U . . . C12 C 0.2329(4) 0.8254(8) 0.0367(7) 0.0335(18) Uani 1 1 d . . . . . H12 H 0.252256 0.913363 0.024950 0.040 Uiso 1 1 calc R U . . . C13 C 0.1932(4) 0.8156(8) 0.1125(7) 0.0318(18) Uani 1 1 d . . . . . H13 H 0.184393 0.897349 0.152969 0.038 Uiso 1 1 calc R U . . . C14 C 0.1665(4) 0.6872(7) 0.1292(6) 0.0242(15) Uani 1 1 d . . . . . C15 C 0.1257(3) 0.6644(7) 0.2124(6) 0.0252(16) Uani 1 1 d . . . . . C16 C 0.1038(4) 0.7757(9) 0.2696(7) 0.0365(19) Uani 1 1 d . . . . . H16 H 0.113889 0.871141 0.254625 0.044 Uiso 1 1 calc R U . . . C17 C 0.0672(4) 0.7465(9) 0.3485(7) 0.0369(19) Uani 1 1 d . . . . . H17 H 0.051912 0.821080 0.388791 0.044 Uiso 1 1 calc R U . . . C18 C 0.0535(4) 0.6077(9) 0.3673(6) 0.0357(18) Uani 1 1 d . . . . . H18 H 0.028480 0.584666 0.421078 0.043 Uiso 1 1 calc R U . . . C19 C 0.0761(3) 0.5018(8) 0.3077(6) 0.0267(16) Uani 1 1 d . . . . . H19 H 0.065885 0.405907 0.320942 0.032 Uiso 1 1 calc R U . . . C20 C 0.1799(4) 0.2383(8) 0.0328(6) 0.0280(17) Uani 1 1 d . . . . . C21 C 0.1189(4) 0.2079(8) 0.2054(6) 0.0265(16) Uani 1 1 d . . . . . C22 C 0.0645(4) 0.3610(8) 0.0160(6) 0.0297(16) 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 0.02986(16) 0.01398(15) 0.02307(15) -0.00146(12) 0.00459(10) -0.00012(13) S1 0.0458(11) 0.0217(10) 0.0409(10) 0.0015(8) 0.0092(9) 0.0053(8) O1 0.049(3) 0.021(3) 0.033(3) -0.009(2) 0.014(3) 0.009(2) O2 0.046(3) 0.021(3) 0.046(3) 0.004(3) 0.016(3) -0.002(3) O3 0.033(3) 0.048(4) 0.026(3) -0.007(2) -0.005(2) -0.004(3) N1 0.038(3) 0.013(3) 0.027(3) 0.000(2) 0.010(3) 0.003(3) N2 0.039(4) 0.016(3) 0.031(3) -0.002(3) 0.004(3) 0.001(3) N3 0.029(3) 0.029(4) 0.037(4) 0.001(3) 0.000(3) 0.004(3) N4 0.031(3) 0.033(4) 0.030(3) -0.001(3) 0.003(3) 0.001(3) N5 0.044(10) 0.058(13) 0.057(10) 0.006(11) -0.006(8) 0.017(10) N5' 0.046(12) 0.073(15) 0.073(14) 0.000(12) -0.006(10) 0.041(12) N6 0.032(3) 0.014(3) 0.026(3) -0.001(2) 0.002(3) 0.001(2) N7 0.026(3) 0.022(3) 0.022(3) -0.004(2) 0.000(3) 0.002(2) C1 0.031(4) 0.028(4) 0.026(4) -0.001(3) 0.009(3) -0.001(3) C2 0.030(4) 0.050(5) 0.034(4) 0.013(4) 0.005(4) 0.003(4) C3 0.040(9) 0.058(13) 0.033(9) 0.007(8) 0.008(7) 0.009(9) C4 0.028(9) 0.035(11) 0.052(13) 0.006(9) -0.003(8) -0.005(8) C5 0.048(15) 0.035(13) 0.048(14) 0.008(10) -0.010(11) 0.013(10) C6 0.057(11) 0.028(9) 0.046(9) -0.006(8) 0.006(8) -0.005(8) C7 0.051(11) 0.050(12) 0.033(9) 0.020(8) -0.007(8) 0.012(9) C3' 0.031(9) 0.041(12) 0.073(13) 0.003(9) 0.007(9) 0.005(8) C4' 0.047(13) 0.058(16) 0.09(2) 0.019(13) 0.031(13) 0.023(11) C5' 0.018(9) 0.09(2) 0.050(15) 0.029(14) 0.011(9) 0.000(12) C6' 0.060(13) 0.11(2) 0.046(11) -0.005(12) 0.000(10) 0.043(14) C7' 0.049(11) 0.13(2) 0.047(11) 0.011(14) 0.009(9) 0.038(14) C8 0.037(11) 0.064(15) 0.071(14) 0.014(12) 0.003(10) 0.015(10) C8' 0.049(13) 0.081(17) 0.092(17) 0.008(13) 0.005(12) 0.010(12) C9 0.050(12) 0.073(16) 0.058(12) 0.023(11) -0.005(10) 0.011(11) C9' 0.062(14) 0.12(2) 0.039(11) 0.012(12) 0.000(10) 0.023(14) C10 0.035(4) 0.030(4) 0.023(3) -0.001(3) 0.006(3) -0.006(3) C11 0.042(5) 0.036(5) 0.035(4) 0.004(4) 0.018(4) -0.001(4) C12 0.037(4) 0.025(4) 0.034(4) 0.006(3) 0.001(3) -0.006(3) C13 0.040(4) 0.010(3) 0.037(4) -0.001(3) -0.006(4) 0.000(3) C14 0.033(4) 0.010(3) 0.027(4) 0.001(3) 0.002(3) 0.001(3) C15 0.025(4) 0.020(4) 0.027(4) -0.006(3) -0.001(3) 0.001(3) C16 0.041(5) 0.028(4) 0.038(4) -0.005(3) 0.005(4) 0.000(4) C17 0.038(4) 0.035(5) 0.037(4) -0.010(4) 0.009(4) 0.005(4) C18 0.036(4) 0.040(5) 0.032(4) -0.007(4) 0.009(3) 0.006(4) C19 0.026(4) 0.025(4) 0.027(4) 0.000(3) 0.002(3) 0.001(3) C20 0.029(4) 0.019(4) 0.034(4) 0.006(3) 0.005(3) -0.008(3) C21 0.025(4) 0.025(4) 0.030(4) -0.005(3) 0.006(3) 0.001(3) C22 0.050(5) 0.013(3) 0.031(4) -0.002(3) 0.018(4) -0.001(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 C22 Re1 C21 89.2(3) . . ? C22 Re1 C20 88.0(3) . . ? C21 Re1 C20 88.9(3) . . ? C22 Re1 N1 177.5(3) . . ? C21 Re1 N1 93.3(3) . . ? C20 Re1 N1 91.9(3) . . ? C22 Re1 N6 96.3(3) . . ? C21 Re1 N6 169.6(3) . . ? C20 Re1 N6 100.1(3) . . ? N1 Re1 N6 81.3(2) . . ? C22 Re1 N7 93.3(3) . . ? C21 Re1 N7 95.9(3) . . ? C20 Re1 N7 175.0(3) . . ? N1 Re1 N7 86.6(2) . . ? N6 Re1 N7 75.0(2) . . ? C1 N1 N2 107.7(6) . . ? C1 N1 Re1 131.0(5) . . ? N2 N1 Re1 121.1(4) . . ? N3 N2 N1 110.8(6) . . ? N2 N3 N4 106.2(6) . . ? N3 N4 C1 111.4(6) . . ? N3 N4 C2 119.0(6) . . ? C1 N4 C2 129.5(7) . . ? C5 N5 C8 123.6(16) . . ? C5 N5 C9 117.8(14) . . ? C8 N5 C9 116.2(17) . . ? C5' N5' C8' 115.4(19) . . ? C5' N5' C9' 118.5(16) . . ? C8' N5' C9' 115(2) . . ? C10 N6 C14 118.4(6) . . ? C10 N6 Re1 124.0(5) . . ? C14 N6 Re1 116.9(5) . . ? C19 N7 C15 118.7(6) . . ? C19 N7 Re1 124.5(5) . . ? C15 N7 Re1 116.7(5) . . ? N1 C1 N4 103.9(6) . . ? N1 C1 S1 127.4(6) . . ? N4 C1 S1 128.7(6) . . ? C3' C2 C7' 118.2(13) . . ? C3 C2 C7 119.3(11) . . ? C3' C2 N4 124.7(10) . . ? C3 C2 N4 119.6(8) . . ? C7' C2 N4 116.1(9) . . ? C7 C2 N4 120.3(8) . . ? C4 C3 C2 117.6(12) . . ? C3 C4 C5 123.7(14) . . ? C4 C5 C6 118.0(14) . . ? C4 C5 N5 118.8(13) . . ? C6 C5 N5 123.1(13) . . ? C7 C6 C5 118.8(14) . . ? C6 C7 C2 121.9(14) . . ? C2 C3' C4' 116.8(15) . . ? C3' C4' C5' 126.2(16) . . ? C6' C5' C4' 116.5(15) . . ? C6' C5' N5' 121.1(15) . . ? C4' C5' N5' 122.4(14) . . ? C5' C6' C7' 118.0(16) . . ? C6' C7' C2 124.3(15) . . ? N6 C10 C11 121.8(7) . . ? C12 C11 C10 119.9(7) . . ? C11 C12 C13 118.7(7) . . ? C14 C13 C12 119.6(7) . . ? N6 C14 C13 121.6(7) . . ? N6 C14 C15 114.7(6) . . ? C13 C14 C15 123.6(7) . . ? N7 C15 C16 121.4(7) . . ? N7 C15 C14 116.1(6) . . ? C16 C15 C14 122.5(7) . . ? C17 C16 C15 119.5(8) . . ? C18 C17 C16 118.5(8) . . ? C17 C18 C19 119.6(8) . . ? N7 C19 C18 122.4(7) . . ? O1 C20 Re1 176.9(7) . . ? O2 C21 Re1 176.1(7) . . ? O3 C22 Re1 175.9(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 C22 1.911(8) . ? Re1 C21 1.918(8) . ? Re1 C20 1.931(8) . ? Re1 N1 2.149(6) . ? Re1 N6 2.167(6) . ? Re1 N7 2.175(6) . ? S1 C1 1.680(8) . ? O1 C20 1.152(9) . ? O2 C21 1.153(9) . ? O3 C22 1.156(9) . ? N1 C1 1.363(9) . ? N1 N2 1.378(8) . ? N2 N3 1.284(8) . ? N3 N4 1.357(9) . ? N4 C1 1.369(9) . ? N4 C2 1.423(9) . ? N5 C5 1.401(14) . ? N5 C8 1.449(14) . ? N5 C9 1.451(14) . ? N5' C5' 1.399(14) . ? N5' C8' 1.448(14) . ? N5' C9' 1.451(14) . ? N6 C10 1.341(10) . ? N6 C14 1.360(9) . ? N7 C19 1.340(10) . ? N7 C15 1.341(9) . ? C2 C3' 1.375(10) . ? C2 C3 1.388(9) . ? C2 C7' 1.391(10) . ? C2 C7 1.397(9) . ? C3 C4 1.386(9) . ? C4 C5 1.394(10) . ? C5 C6 1.394(10) . ? C6 C7 1.394(9) . ? C3' C4' 1.384(10) . ? C4' C5' 1.386(10) . ? C5' C6' 1.385(10) . ? C6' C7' 1.387(10) . ? C10 C11 1.373(11) . ? C11 C12 1.369(11) . ? C12 C13 1.379(12) . ? C13 C14 1.369(10) . ? C14 C15 1.480(11) . ? C15 C16 1.389(11) . ? C16 C17 1.385(12) . ? C17 C18 1.369(12) . ? C18 C19 1.375(11) . ?