#------------------------------------------------------------------------------ #$Date: 2014-10-25 20:23:10 +0300 (Sat, 25 Oct 2014) $ #$Revision: 125873 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/01/80/2018058.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2018058 loop_ _publ_author_name 'Kochel, Andrzej' 'Ho\/ly\'nska, Ma\/lgorzata' _publ_section_title ; Diammonium hexakis(thiocyanato-\kN)rhenate(IV) dimethyl sulfone tetrasolvate ; _journal_coeditor_code FA3250 _journal_issue 5 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first m134 _journal_page_last m136 _journal_volume 67 _journal_year 2011 _chemical_formula_iupac '(N1 H4)2 [Re (N C S)6] , 4C2 H6 O2 S' _chemical_formula_moiety '2(H4 N +), C6 N6 Re S6 2-, 4(C2 H6 O2 S)' _chemical_formula_sum 'C14 H32 N8 O8 Re S10' _chemical_formula_weight 947.28 _chemical_name_systematic ; Diammonium hexakis(thiocyanato-\kN)rhenate(IV) dimethyl sulfone tetrasolvate ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL97 _cell_angle_alpha 90.00 _cell_angle_beta 113.57(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 13.128(3) _cell_length_b 9.493(3) _cell_length_c 15.412(4) _cell_measurement_reflns_used 3295 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 28.73 _cell_measurement_theta_min 2.88 _cell_volume 1760.5(9) _computing_cell_refinement 'CrysAlis RED (Oxford Diffraction, 2009)' _computing_data_collection 'CrysAlis CCD (Oxford Diffraction, 2009)' _computing_data_reduction 'CrysAlis RED (Oxford Diffraction, 2009)' _computing_molecular_graphics ; DIAMOND (Brandenburg, 2010) and SHELXTL (Sheldrick, 2008) ; _computing_publication_material 'SHELXL97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.928 _diffrn_measurement_device_type 'Oxford KM-4 CCD area-detector' _diffrn_measurement_method \w _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0250 _diffrn_reflns_av_sigmaI/netI 0.0270 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 11719 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 28.73 _diffrn_reflns_theta_min 2.88 _exptl_absorpt_coefficient_mu 4.092 _exptl_absorpt_correction_T_max 0.956 _exptl_absorpt_correction_T_min 0.789 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details '(CrysAlis RED; Oxford Diffraction, 2009)' _exptl_crystal_colour red _exptl_crystal_density_diffrn 1.787 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 942 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.05 _refine_diff_density_max 0.88 _refine_diff_density_min -0.74 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 191 _refine_ls_number_reflns 4234 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.004 _refine_ls_R_factor_all 0.0318 _refine_ls_R_factor_gt 0.0233 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0355P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0555 _refine_ls_wR_factor_ref 0.0571 _reflns_number_gt 3483 _reflns_number_total 4234 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file fa3250.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'P 21/c' _cod_original_cell_volume 1760.5(8) _cod_database_code 2018058 _iucr_refine_instructions_details ; TITL AKI.INS in P2(1)/c New: P21/c CELL 0.71073 13.128 9.493 15.412 90.00 113.57 90.00 ZERR 2 0.003 0.003 0.004 0.00 0.03 0.00 LATT 1 SYMM - X , 0.50000 + Y , 0.50000 - Z SFAC C H N O Re S UNIT 28 64 16 16 2 20 L.S. 10 TEMP -173 EQIV $1 -x+1, y-1/2, -z+1/2 EQIV $2 -x, y-1/2, -z+1/2 EQIV $3 x, y-1, z EQIV $4 -x, -y+1, -z EQIV $5 x,y+1,z HTAB N4 S1_$1 HTAB N4 O2_$2 HTAB N4 O4_$2 HTAB N4 O1_$3 HTAB N4 O1_$4 RTAB n S1 S3_$5 RTAB n S2 S2_$4 FMAP 2 PLAN 30 ACTA 50 HTAB 2 list 6 BOND $H WGHT 0.035500 FVAR 1.84937 RE1 5 0.500000 0.500000 0.000000 10.50000 0.01127 0.01794 = 0.01593 0.00062 0.00376 0.00087 S1 6 0.684504 0.758361 0.287207 11.00000 0.02905 0.02389 = 0.02046 -0.00255 0.00000 0.00364 S2 6 0.141844 0.487635 0.015079 11.00000 0.01514 0.02849 = 0.02461 0.00050 0.01000 -0.00191 S3 6 0.606936 0.096918 0.201397 11.00000 0.02497 0.02337 = 0.03116 0.00915 0.00897 0.00135 N1 3 0.573619 0.611032 0.119764 11.00000 0.01325 0.02285 = 0.02077 0.00112 0.00430 0.00245 N2 3 0.353395 0.499899 0.014892 11.00000 0.01550 0.01962 = 0.02025 0.00081 0.00658 0.00109 N3 3 0.542920 0.322823 0.077205 11.00000 0.01495 0.02077 = 0.02177 0.00023 0.00540 0.00039 C1 1 0.620562 0.672175 0.191025 11.00000 0.01563 0.01866 = 0.02134 0.00496 0.00562 0.00431 C2 1 0.265543 0.493698 0.015716 11.00000 0.01934 0.01468 = 0.01416 0.00136 0.00479 0.00178 C3 1 0.569818 0.228511 0.130329 11.00000 0.01335 0.02248 = 0.02174 -0.00491 0.00554 -0.00130 S4 6 0.045997 0.824920 0.216102 11.00000 0.01472 0.02113 = 0.01335 0.00228 0.00570 -0.00015 O1 4 -0.009981 0.889094 0.123320 11.00000 0.01772 0.02724 = 0.01511 0.00559 0.00451 0.00017 O2 4 -0.019614 0.812132 0.272061 11.00000 0.02209 0.03665 = 0.02204 0.00859 0.01462 0.00404 C4 1 0.093728 0.658452 0.202120 11.00000 0.02280 0.02436 = 0.02282 -0.00325 0.00688 0.00181 AFIX 137 H4A 2 0.030312 0.598422 0.165528 11.00000 -1.50000 H4B 2 0.134734 0.616184 0.264466 11.00000 -1.50000 H4C 2 0.142946 0.667250 0.168512 11.00000 -1.50000 AFIX 0 C5 1 0.167401 0.921830 0.279105 11.00000 0.02225 0.02293 = 0.01889 -0.00221 0.00436 -0.00535 AFIX 137 H5A 2 0.210257 0.874519 0.339249 11.00000 -1.50000 H5B 2 0.147237 1.016768 0.291625 11.00000 -1.50000 H5C 2 0.212373 0.928214 0.241555 11.00000 -1.50000 AFIX 0 S5 6 0.252406 0.572693 0.515357 11.00000 0.01411 0.01862 = 0.01746 0.00253 0.00552 0.00068 O3 4 0.179118 0.543689 0.563401 11.00000 0.01993 0.02717 = 0.02332 0.00013 0.01118 -0.00280 O4 4 0.207919 0.665469 0.434808 11.00000 0.02700 0.02485 = 0.02117 0.00791 0.00842 0.00528 C6 1 0.291758 0.413292 0.479562 11.00000 0.02103 0.02267 = 0.02953 -0.00041 0.01100 0.00440 AFIX 137 H6A 2 0.342483 0.432726 0.448553 11.00000 -1.50000 H6B 2 0.225523 0.364865 0.435106 11.00000 -1.50000 H6C 2 0.329211 0.353402 0.535068 11.00000 -1.50000 AFIX 0 C7 1 0.375523 0.643869 0.598298 11.00000 0.01996 0.02765 = 0.02885 0.00102 0.00339 -0.00424 AFIX 137 H7A 2 0.359278 0.732700 0.622576 11.00000 -1.50000 H7B 2 0.427354 0.661425 0.568111 11.00000 -1.50000 H7C 2 0.409016 0.577419 0.650745 11.00000 -1.50000 AFIX 0 N4 3 0.033504 0.180376 0.068812 11.00000 0.01833 0.01754 = 0.01882 -0.00262 0.00920 -0.00012 AFIX 3 H1 2 0.106907 0.202528 0.098996 11.00000 -1.20000 H2 2 -0.007065 0.236977 0.090743 11.00000 -1.20000 H3 2 0.023980 0.088828 0.081764 11.00000 -1.20000 H4 2 0.011120 0.192614 0.005336 11.00000 -1.20000 rem dfix 0.91 0.003 N4 H1 N4 H2 N4 H3 N4 H4 rem dfix 1.5 0.01 H1 H2 H1 H3 H1 H4 H2 H3 H2 H4 H3 H4 HKLF 4 REM AKI.INS in P2(1)/c New: P21/c REM R1 = 0.0233 for 3483 Fo > 4sig(Fo) and 0.0318 for all 4234 data REM 191 parameters refined using 0 restraints END WGHT 0.0372 0.0000 REM Highest difference peak 0.882, deepest hole -0.741, 1-sigma level 0.115 Q1 1 0.4999 0.4987 0.0627 11.00000 0.05 0.88 Q2 1 0.6062 0.5017 0.1051 11.00000 0.05 0.82 Q3 1 0.3126 0.7582 0.7093 11.00000 0.05 0.81 Q4 1 0.2507 0.4326 0.5149 11.00000 0.05 0.80 Q5 1 0.5594 0.5032 0.0329 11.00000 0.05 0.72 Q6 1 0.6088 -0.0954 0.2000 11.00000 0.05 0.70 Q7 1 -0.0463 0.6750 0.2827 11.00000 0.05 0.68 Q8 1 0.5335 0.5600 0.0783 11.00000 0.05 0.55 Q9 1 0.0660 0.7364 0.2054 11.00000 0.05 0.55 Q10 1 0.5024 0.3920 0.0028 11.00000 0.05 0.53 Q11 1 0.3115 0.6159 0.5680 11.00000 0.05 0.52 Q12 1 0.4061 0.5076 0.0232 11.00000 0.05 0.48 Q13 1 0.2706 0.5004 0.4889 11.00000 0.05 0.48 Q14 1 0.4097 0.4200 -0.0080 11.00000 0.05 0.47 Q15 1 0.3401 0.4983 -0.0637 11.00000 0.05 0.47 Q16 1 0.2119 0.6424 0.4696 11.00000 0.05 0.45 Q17 1 0.4596 0.4250 0.0381 11.00000 0.05 0.44 Q18 1 0.5343 0.4470 0.0855 11.00000 0.05 0.44 Q19 1 0.6051 0.5864 0.1654 11.00000 0.05 0.44 Q20 1 -0.0165 0.8208 0.2328 11.00000 0.05 0.42 Q21 1 0.2314 0.5337 0.5632 11.00000 0.05 0.39 Q22 1 -0.0743 0.7813 0.2535 11.00000 0.05 0.39 Q23 1 0.6330 0.6833 0.2444 11.00000 0.05 0.39 Q24 1 0.2098 0.5004 0.0276 11.00000 0.05 0.39 Q25 1 0.2031 0.4233 0.0599 11.00000 0.05 0.38 Q26 1 0.5727 0.3673 0.1007 11.00000 0.05 0.36 Q27 1 0.6714 0.7412 0.2303 11.00000 0.05 0.36 Q28 1 0.2020 0.3368 0.4737 11.00000 0.05 0.36 Q29 1 0.6802 0.1004 0.2568 11.00000 0.05 0.36 Q30 1 0.4083 0.5881 -0.0107 11.00000 0.05 0.35 ; loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Re Re1 0.5000 0.5000 0.0000 0.01558(5) Uani d S 1 . . S S1 0.68450(6) 0.75836(8) 0.28721(5) 0.02761(16) Uani d . 1 . . S S2 0.14184(6) 0.48764(7) 0.01508(5) 0.02210(14) Uani d . 1 . . S S3 0.60694(6) 0.09692(8) 0.20140(5) 0.02721(16) Uani d . 1 . . N N1 0.57362(18) 0.6110(2) 0.11976(15) 0.0198(5) Uani d . 1 . . N N2 0.3534(2) 0.4999(2) 0.01489(16) 0.0186(4) Uani d . 1 . . N N3 0.54292(18) 0.3228(2) 0.07720(15) 0.0198(5) Uani d . 1 . . C C1 0.6206(2) 0.6722(3) 0.19103(18) 0.0191(5) Uani d . 1 . . C C2 0.2655(2) 0.4937(3) 0.01572(17) 0.0167(5) Uani d . 1 . . C C3 0.5698(2) 0.2285(3) 0.13033(18) 0.0197(5) Uani d . 1 . . S S4 0.04600(5) 0.82492(7) 0.21610(4) 0.01637(13) Uani d . 1 . . O O1 -0.00998(14) 0.88909(19) 0.12332(12) 0.0207(4) Uani d . 1 . . O O2 -0.01961(15) 0.8121(2) 0.27206(12) 0.0251(4) Uani d . 1 . . C C4 0.0937(2) 0.6585(3) 0.20212(18) 0.0240(6) Uani d . 1 . . H H4A 0.0303 0.5984 0.1655 0.036 Uiso calc R 1 . . H H4B 0.1347 0.6162 0.2645 0.036 Uiso calc R 1 . . H H4C 0.1429 0.6672 0.1685 0.036 Uiso calc R 1 . . C C5 0.1674(2) 0.9218(3) 0.27910(18) 0.0226(6) Uani d . 1 . . H H5A 0.2103 0.8745 0.3392 0.034 Uiso calc R 1 . . H H5B 0.1472 1.0168 0.2916 0.034 Uiso calc R 1 . . H H5C 0.2124 0.9282 0.2416 0.034 Uiso calc R 1 . . S S5 0.25241(5) 0.57269(7) 0.51536(4) 0.01698(13) Uani d . 1 . . O O3 0.17912(16) 0.5437(2) 0.56340(13) 0.0227(4) Uani d . 1 . . O O4 0.20792(16) 0.6655(2) 0.43481(13) 0.0247(4) Uani d . 1 . . C C6 0.2918(2) 0.4133(3) 0.47956(19) 0.0241(6) Uani d . 1 . . H H6A 0.3425 0.4327 0.4486 0.036 Uiso calc R 1 . . H H6B 0.2255 0.3649 0.4351 0.036 Uiso calc R 1 . . H H6C 0.3292 0.3534 0.5351 0.036 Uiso calc R 1 . . C C7 0.3755(2) 0.6439(3) 0.59830(19) 0.0275(6) Uani d . 1 . . H H7A 0.3593 0.7327 0.6226 0.041 Uiso calc R 1 . . H H7B 0.4274 0.6614 0.5681 0.041 Uiso calc R 1 . . H H7C 0.4090 0.5774 0.6507 0.041 Uiso calc R 1 . . N N4 0.03350(17) 0.1804(2) 0.06881(14) 0.0177(4) Uani d . 1 . . H H1 0.1069 0.2025 0.0990 0.021 Uiso d R 1 . . H H2 -0.0071 0.2370 0.0907 0.021 Uiso d R 1 . . H H3 0.0240 0.0888 0.0818 0.021 Uiso d R 1 . . H H4 0.0111 0.1926 0.0053 0.021 Uiso d R 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Re1 0.01127(8) 0.01794(8) 0.01593(7) 0.00087(6) 0.00376(5) 0.00062(6) S1 0.0290(4) 0.0239(4) 0.0205(3) 0.0036(3) 0.0000(3) -0.0025(3) S2 0.0151(3) 0.0285(4) 0.0246(3) -0.0019(3) 0.0100(3) 0.0005(3) S3 0.0250(4) 0.0234(4) 0.0312(4) 0.0013(3) 0.0090(3) 0.0092(3) N1 0.0133(11) 0.0228(12) 0.0208(11) 0.0024(9) 0.0043(9) 0.0011(9) N2 0.0155(11) 0.0196(11) 0.0203(11) 0.0011(10) 0.0066(8) 0.0008(9) N3 0.0149(11) 0.0208(12) 0.0218(11) 0.0004(9) 0.0054(9) 0.0002(9) C1 0.0156(13) 0.0187(14) 0.0213(12) 0.0043(11) 0.0056(10) 0.0050(11) C2 0.0193(13) 0.0147(12) 0.0142(11) 0.0018(11) 0.0048(9) 0.0014(10) C3 0.0133(13) 0.0225(14) 0.0217(13) -0.0013(11) 0.0055(10) -0.0049(11) S4 0.0147(3) 0.0211(3) 0.0134(3) -0.0001(3) 0.0057(2) 0.0023(2) O1 0.0177(10) 0.0272(11) 0.0151(8) 0.0002(8) 0.0045(7) 0.0056(8) O2 0.0221(10) 0.0366(12) 0.0220(9) 0.0040(9) 0.0146(8) 0.0086(8) C4 0.0228(15) 0.0244(15) 0.0228(13) 0.0018(12) 0.0069(11) -0.0032(11) C5 0.0223(14) 0.0229(15) 0.0189(12) -0.0054(12) 0.0044(11) -0.0022(11) S5 0.0141(3) 0.0186(3) 0.0175(3) 0.0007(3) 0.0055(2) 0.0025(3) O3 0.0199(10) 0.0272(10) 0.0233(10) -0.0028(8) 0.0112(8) 0.0001(8) O4 0.0270(11) 0.0249(11) 0.0212(9) 0.0053(9) 0.0084(8) 0.0079(8) C6 0.0210(15) 0.0227(15) 0.0295(14) 0.0044(12) 0.0110(12) -0.0004(12) C7 0.0200(15) 0.0277(16) 0.0288(14) -0.0042(12) 0.0034(12) 0.0010(12) N4 0.0183(11) 0.0175(11) 0.0188(10) -0.0001(9) 0.0092(9) -0.0026(9) 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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 Re1 N1 . 3_665 180.0 ? N1 Re1 N3 . . 88.69(8) yes N1 Re1 N3 3_665 . 91.31(8) ? N1 Re1 N3 . 3_665 91.31(8) ? N1 Re1 N3 3_665 3_665 88.69(8) ? N3 Re1 N3 . 3_665 180.0 ? N1 Re1 N2 . . 91.49(9) yes N1 Re1 N2 3_665 . 88.51(9) ? N3 Re1 N2 . . 89.24(9) yes N3 Re1 N2 3_665 . 90.76(9) ? N1 Re1 N2 . 3_665 88.51(9) yes N1 Re1 N2 3_665 3_665 91.49(9) ? N3 Re1 N2 . 3_665 90.76(9) ? N3 Re1 N2 3_665 3_665 89.24(9) ? N2 Re1 N2 . 3_665 180.0 ? C1 N1 Re1 . . 177.1(2) ? C2 N2 Re1 . . 173.9(2) ? C3 N3 Re1 . . 172.9(2) ? N1 C1 S1 . . 178.9(2) ? N2 C2 S2 . . 178.7(3) ? N3 C3 S3 . . 178.7(2) ? O2 S4 O1 . . 115.71(11) ? O2 S4 C4 . . 109.05(13) ? O1 S4 C4 . . 108.85(12) ? O2 S4 C5 . . 109.81(13) ? O1 S4 C5 . . 108.29(12) ? C4 S4 C5 . . 104.54(14) ? S4 C4 H4A . . 109.5 ? S4 C4 H4B . . 109.5 ? H4A C4 H4B . . 109.5 ? S4 C4 H4C . . 109.5 ? H4A C4 H4C . . 109.5 ? H4B C4 H4C . . 109.5 ? S4 C5 H5A . . 109.5 ? S4 C5 H5B . . 109.5 ? H5A C5 H5B . . 109.5 ? S4 C5 H5C . . 109.5 ? H5A C5 H5C . . 109.5 ? H5B C5 H5C . . 109.5 ? O4 S5 O3 . . 115.53(12) ? O4 S5 C7 . . 109.37(14) ? O3 S5 C7 . . 107.90(13) ? O4 S5 C6 . . 108.93(13) ? O3 S5 C6 . . 109.50(13) ? C7 S5 C6 . . 105.11(14) ? S5 C6 H6A . . 109.5 ? S5 C6 H6B . . 109.5 ? H6A C6 H6B . . 109.5 ? S5 C6 H6C . . 109.5 ? H6A C6 H6C . . 109.5 ? H6B C6 H6C . . 109.5 ? S5 C7 H7A . . 109.5 ? S5 C7 H7B . . 109.5 ? H7A C7 H7B . . 109.5 ? S5 C7 H7C . . 109.5 ? H7A C7 H7C . . 109.5 ? H7B C7 H7C . . 109.5 ? H1 N4 H2 . . 109.3 ? H1 N4 H3 . . 108.5 ? H2 N4 H3 . . 109.2 ? H1 N4 H4 . . 109.9 ? H2 N4 H4 . . 109.8 ? H3 N4 H4 . . 110.1 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Re1 N1 . 2.006(2) yes Re1 N1 3_665 2.006(2) ? Re1 N2 . 2.027(2) yes Re1 N3 . 2.006(2) yes Re1 N3 3_665 2.007(2) ? Re1 N2 3_665 2.027(2) ? S1 C1 . 1.605(3) yes S2 C2 . 1.621(3) yes S3 C3 . 1.603(3) yes N1 C1 . 1.175(3) yes N2 C2 . 1.160(4) yes N3 C3 . 1.169(3) yes S4 O1 . 1.4545(18) yes S4 O2 . 1.4472(18) yes S4 C4 . 1.745(3) ? S4 C5 . 1.758(3) ? C4 H4A . 0.9800 ? C4 H4B . 0.9800 ? C4 H4C . 0.9800 ? C5 H5A . 0.9800 ? C5 H5B . 0.9800 ? C5 H5C . 0.9800 ? S5 O4 . 1.4415(19) yes S5 O3 . 1.456(2) yes S5 C7 . 1.747(3) ? S5 C6 . 1.758(3) ? C6 H6A . 0.9800 ? C6 H6B . 0.9800 ? C6 H6C . 0.9800 ? C7 H7A . 0.9800 ? C7 H7B . 0.9800 ? C7 H7C . 0.9800 ? N4 H1 . 0.9114 ? N4 H2 . 0.9114 ? N4 H3 . 0.9114 ? N4 H4 . 0.9094 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA N4 H2 O2 2_545 0.91 2.12 2.823(3) 133 N4 H2 O4 2_545 0.91 2.60 3.151(3) 120 N4 H3 O1 1_545 0.91 2.11 3.010(3) 172 N4 H4 O1 3_565 0.91 2.12 2.927(3) 147 _journal_paper_doi 10.1107/S0108270111010535