#------------------------------------------------------------------------------ #$Date: 2024-07-24 04:56:58 +0300 (Wed, 24 Jul 2024) $ #$Revision: 293522 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/02/32/2023207.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_2023207 loop_ _publ_author_name 'Rudnitskaya, Olga V.' 'Komarovskikh, Milena R.' 'Pekarskaya, Maria G.' 'Pshenichnyy, Daniil S.' 'Akkurt, Mehmet' 'Khalilov, Ali N.' 'Bhattarai, Ajaya' 'Mamedov, Ibrahim G.' _publ_section_title ; Synthesis, molecular and crystal structure of [(NH2)2CSSC(NH2)2]2[RuBr6]Br2·3H2O ; _journal_coeditor_code NY2005 _journal_issue 8 _journal_name_full 'Acta Crystallographica Section E Crystallographic Communications' _journal_paper_doi 10.1107/S2056989024006832 _journal_volume 80 _journal_year 2024 _chemical_formula_iupac '(C2 H8 N4 S2)2 [Ru Br6] Br2, 3H2 O' _chemical_formula_moiety '2(C2 H8 N4 S2 2+), Br6 Ru 2-, 2(Br -), 3(H2 O)' _chemical_formula_sum 'C4 H22 Br8 N8 O3 Ru S4' _chemical_formula_weight 1098.88 _chemical_name_systematic ; Bis[dithiobis(formamidinium)] hexabromidoruthenium dibromide trihydrate ; _space_group_crystal_system orthorhombic _space_group_IT_number 63 _space_group_name_Hall '-C 2c 2' _space_group_name_H-M_alt 'C m c m' _atom_sites_solution_hydrogens difmap _atom_sites_solution_primary difmap _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2018/3 _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 11.6462(3) _cell_length_b 13.9943(4) _cell_length_c 16.9225(5) _cell_measurement_reflns_used 1291 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 26.60 _cell_measurement_theta_min 2.28 _cell_volume 2758.04(13) _computing_cell_refinement ; SAINT (Bruker, 2016) ; _computing_data_collection ; APEX3 (Bruker, 2016) ; _computing_data_reduction ; SAINT (Bruker, 2016) ; _computing_molecular_graphics ; ORTEP-3 for Windows (Farrugia, 2012) ; _computing_publication_material ; PLATON (Spek, 2020) ; _computing_structure_refinement ; SHELXL2019/3 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT2014/5 (Sheldrick, 2015a) ; _diffrn_ambient_temperature 150(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Bruker D8 Venture' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0434 _diffrn_reflns_av_unetI/netI 0.0235 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 22642 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 30.522 _diffrn_reflns_theta_min 2.275 _diffrn_source microsource _exptl_absorpt_coefficient_mu 12.485 _exptl_absorpt_correction_T_max 0.0998 _exptl_absorpt_correction_T_min 0.0425 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Krause et al., 2015) ; _exptl_crystal_colour black _exptl_crystal_density_diffrn 2.646 _exptl_crystal_description plate _exptl_crystal_F_000 2056 _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.020 _refine_diff_density_max 1.061 _refine_diff_density_min -0.594 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_hydrogen_treatment refxyz _refine_ls_matrix_type full _refine_ls_number_parameters 93 _refine_ls_number_reflns 2269 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.069 _refine_ls_R_factor_all 0.0266 _refine_ls_R_factor_gt 0.0227 _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^)+(0.0237P)^2^+6.8980P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0552 _refine_ls_wR_factor_ref 0.0567 _reflns_number_gt 2057 _reflns_number_total 2269 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ny2005.cif _cod_data_source_block I _cod_database_code 2023207 _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 0.117 _shelx_estimated_absorpt_t_max 0.788 _shelx_hkl_file ; 2 0 0 903.881 46.3214 4 2 0 0 978.184 46.1967 3 -2 0 0 937.021 46.2366 2 -2 0 0 985.997 46.2142 3 -2 0 0 994.518 46.3143 4 -4 0 0 9780.93 477.546 1 4 0 0 9999.99 477.847 1 -6 0 0 6155.65 295.218 4 -6 0 0 6254.08 295.040 3 -6 0 0 6336.21 295.257 2 6 0 0 6141.73 294.886 3 -6 0 0 5880.28 295.041 2 -8 0 0 1142.80 54.5598 3 -8 0 0 1134.97 54.8326 2 8 0 0 1067.94 54.2720 3 -10 0 0 3113.25 140.322 3 -10 0 0 3086.57 140.683 2 10 0 0 2499.16 141.104 4 -12 0 0 486.780 24.1813 2 12 0 0 423.388 24.5796 4 -14 0 0 776.708 38.8285 3 14 0 0 768.820 39.8871 4 -16 0 0 179.273 11.8923 2 16 0 0 188.615 11.9893 4 -1 1 0 218.218 10.8111 3 -1 1 0 215.831 10.6010 2 1 -1 0 217.070 10.7560 4 1 1 0 223.795 10.7142 4 -1 -1 0 214.004 10.7773 2 1 -1 0 219.670 10.8104 3 -1 -1 0 229.932 10.7371 4 3 -1 0 230.351 11.7859 3 3 -1 0 239.377 11.8441 4 -3 1 0 222.216 11.6221 2 -3 1 0 236.413 11.7910 4 -3 -1 0 239.316 11.9016 2 -3 -1 0 240.439 11.5801 3 -3 -1 0 233.246 11.8220 2 -3 1 0 241.099 11.8374 3 3 1 0 225.699 11.5059 3 -5 1 0 183.754 9.89987 2 -5 1 0 191.558 10.0947 4 5 -1 0 189.804 10.0201 3 -5 -1 0 204.121 9.89067 3 -5 -1 0 193.581 10.2439 2 5 -1 0 201.533 10.3512 4 -5 1 0 191.335 10.0934 3 -5 -1 0 187.088 10.2973 4 -5 1 0 190.255 10.0293 2 5 1 0 186.681 9.70451 3 -5 -1 0 179.811 10.0596 2 7 1 0 1.60677 1.86707 4 -7 1 0 0.68255 1.08671 3 7 -1 0 2.21282 1.57741 4 7 1 0 0.45438 0.79564 3 -7 1 0 3.43026 1.38024 2 -7 -1 0 -0.7639 0.94303 2 7 -1 0 1.93820 0.97310 3 -7 1 0 -0.1264 0.89002 2 -7 -1 0 1.49415 0.96428 3 -9 -1 0 385.681 19.1584 3 -9 -1 0 385.241 19.9697 2 -9 1 0 390.196 19.5315 2 -9 1 0 382.285 19.4374 3 9 1 0 368.943 18.8769 3 9 1 0 316.780 20.6189 4 -11 1 0 38.6850 4.11682 2 -11 1 0 35.1795 3.83142 3 -11 -1 0 35.3164 4.25636 2 -11 -1 0 31.0318 3.30928 3 11 -1 0 32.6901 5.04856 4 11 1 0 29.5286 4.32395 4 13 -1 0 87.7090 7.65323 4 13 1 0 82.2881 7.13574 4 -13 -1 0 94.8550 6.62255 3 -13 1 0 99.7668 6.76862 2 -13 -1 0 90.0974 6.93277 2 -13 1 0 75.8144 6.11047 3 15 1 0 15.6767 3.66413 4 -15 -1 0 16.0100 2.74155 3 -15 -1 0 16.4225 3.58382 2 -15 1 0 10.3298 3.18595 2 -15 1 0 15.7450 3.01949 3 15 -1 0 15.7769 4.09905 4 0 2 0 122.117 6.00844 3 0 2 0 116.274 5.94481 4 0 2 0 123.498 5.95302 2 0 -2 0 114.295 5.99200 3 0 -2 0 116.858 5.86839 2 2 2 0 425.913 19.8555 4 -2 -2 0 407.030 19.9800 2 -2 2 0 407.284 19.7051 2 2 -2 0 415.228 19.6379 2 2 -2 0 400.481 20.0311 3 -2 -2 0 398.028 20.0178 2 -2 -2 0 408.666 19.6648 3 -2 -2 0 420.452 19.9080 4 -2 2 0 387.971 20.0241 3 -2 2 0 392.768 19.9201 4 -4 2 0 388.788 19.7279 4 -4 -2 0 396.835 19.3678 3 -4 -2 0 408.035 19.9586 2 4 2 0 421.339 19.5175 3 -4 -2 0 385.631 19.8124 2 4 2 0 401.171 19.8071 4 -4 2 0 386.687 19.4689 2 -4 2 0 395.269 19.5204 2 -4 2 0 387.022 19.8431 3 4 -2 0 388.462 19.8162 3 4 -2 0 397.457 19.7936 4 -6 -2 0 13.6050 2.29964 4 6 2 0 12.9836 1.49132 3 -6 -2 0 10.7764 1.96200 2 6 2 0 10.0447 2.02394 4 -6 2 0 10.6356 1.61504 2 -6 2 0 9.01034 1.77774 3 6 -2 0 9.47289 1.96067 4 -6 -2 0 12.8999 1.62348 3 -6 2 0 10.6972 1.51933 2 6 -2 0 8.68139 1.57355 3 -8 2 0 317.745 16.8596 3 -8 2 0 309.797 16.6183 2 -8 -2 0 323.871 17.0985 2 -8 -2 0 319.476 16.3541 3 8 2 0 317.135 17.0949 4 8 -2 0 336.373 17.2848 4 10 2 0 66.6707 5.81149 4 -10 -2 0 70.8724 4.79553 3 -10 2 0 70.4748 5.30279 3 10 -2 0 68.7921 6.20993 4 -10 2 0 77.8831 5.39368 2 -10 -2 0 80.4150 5.82366 2 -12 -2 0 3.47571 2.37635 2 -12 2 0 5.60197 1.95143 3 12 -2 0 1.68359 3.31192 4 -12 -2 0 4.90139 1.69367 3 -12 2 0 9.61316 2.43598 2 12 2 0 3.18449 2.40635 4 14 -2 0 123.809 10.8604 4 14 2 0 172.099 10.3192 4 -14 -2 0 161.648 9.96439 3 -14 -2 0 167.681 10.3951 2 -14 2 0 145.276 9.49793 3 -14 2 0 149.625 9.81239 2 16 2 0 -4.7510 2.44252 4 16 -2 0 6.10693 3.70673 4 -16 2 0 1.90304 2.67672 2 -16 -2 0 -1.8169 2.40405 2 -16 2 0 2.44741 2.19292 3 -1 3 0 354.665 18.0321 3 1 -3 0 359.198 18.0362 3 1 -3 0 362.941 17.9649 4 1 -3 0 366.184 17.5506 2 -1 -3 0 375.472 17.8158 3 1 3 0 376.348 17.7897 3 -1 -3 0 373.728 17.8151 4 -1 -3 0 365.397 17.9068 2 1 3 0 362.241 17.8303 4 -1 3 0 354.094 17.5298 2 -1 3 0 357.518 17.9332 4 -3 3 0 7665.13 366.583 2 -5 3 0 91.8641 5.10632 2 -5 3 0 91.1098 5.09583 2 -5 -3 0 90.2126 5.54237 2 -5 -3 0 96.0947 4.96674 3 5 -3 0 99.2317 5.65780 4 -5 -3 0 86.3972 5.66171 2 -5 3 0 89.6904 5.45124 4 5 3 0 105.054 5.56064 4 5 -3 0 95.0690 5.60218 3 5 3 0 73.4890 5.19209 3 -5 3 0 95.2169 5.69162 3 7 3 0 2443.05 113.830 4 7 -3 0 2436.31 114.022 4 7 3 0 2138.38 113.460 3 -7 -3 0 2340.93 114.104 2 -7 -3 0 2465.83 113.311 3 -7 3 0 2361.67 113.457 2 -7 3 0 2312.95 113.455 2 -7 3 0 2327.52 113.977 3 -9 3 0 163.705 9.48470 3 9 3 0 153.612 9.39457 4 9 3 0 157.604 8.96919 3 9 -3 0 170.666 9.91513 4 -9 3 0 166.185 9.11316 2 -9 -3 0 145.342 9.48210 2 -9 -3 0 154.040 8.63696 3 11 -3 0 233.317 14.3050 4 -11 -3 0 236.718 12.6710 3 11 3 0 250.737 13.6676 4 -11 3 0 238.987 14.2238 2 -11 -3 0 233.079 13.7888 2 -11 3 0 241.286 13.5359 3 13 3 0 185.942 10.9773 4 -13 -3 0 177.072 9.91689 3 -13 3 0 187.780 10.9186 3 -13 3 0 167.588 10.5734 2 -13 -3 0 173.152 11.3078 2 -15 -3 0 43.3201 5.36243 2 15 -3 0 22.1196 5.21595 4 -15 3 0 40.3027 5.26771 2 15 3 0 41.1911 4.82608 4 0 4 0 8.37434 1.12639 3 0 -4 0 9.10006 1.06591 4 0 -4 0 8.77754 0.93777 2 0 -4 0 9.46033 1.18757 3 2 4 0 1331.43 64.3537 3 2 -4 0 1281.93 64.8308 3 -2 -4 0 1354.63 64.6931 2 2 -4 0 1328.14 64.7323 4 -2 -4 0 1376.71 64.5253 4 -2 4 0 1317.90 64.8703 3 -2 -4 0 1341.10 64.7327 2 -2 -4 0 1371.95 64.4229 3 -4 4 0 4.59005 0.79807 2 4 -4 0 4.06817 1.30287 3 -4 4 0 5.28265 1.38343 3 -4 4 0 4.44007 0.80358 2 -4 -4 0 7.32312 1.56220 4 -4 -4 0 6.29557 0.89116 3 -4 4 0 5.21035 1.29145 4 4 4 0 6.66647 1.23136 4 4 -4 0 4.84829 1.48807 4 -4 -4 0 5.23541 1.20918 2 -4 -4 0 8.14258 1.54563 2 -4 -4 0 7.17370 1.21658 3 -6 -4 0 405.783 20.1405 3 -6 4 0 389.171 21.0138 3 6 -4 0 408.668 20.9204 4 -6 -4 0 420.669 21.1733 2 -6 4 0 421.157 20.3351 2 6 4 0 440.264 20.7220 4 -6 4 0 380.173 20.2466 2 -8 -4 0 43.9318 4.18163 2 -8 -4 0 51.5180 3.34565 3 -8 4 0 44.3063 3.44896 2 -8 4 0 47.6539 4.08754 3 8 4 0 48.1290 4.02248 4 8 4 0 50.1228 3.46946 3 -8 4 0 44.1971 3.42969 2 8 -4 0 44.6703 4.26119 4 10 4 0 12.5365 2.58008 4 10 4 0 9.07707 1.91745 3 10 -4 0 15.7066 3.22409 4 -10 -4 0 9.01229 2.52930 2 -10 4 0 9.69561 2.49407 3 -10 4 0 13.4030 2.10353 2 -10 -4 0 11.8102 1.79715 3 -12 4 0 179.293 10.4537 2 -12 -4 0 180.334 11.2864 2 12 4 0 195.044 10.9088 4 -12 -4 0 178.513 9.76117 3 -12 4 0 182.390 11.0177 3 12 -4 0 158.809 11.6041 4 14 -4 0 34.6203 5.74517 4 -14 -4 0 40.9687 3.37141 3 -14 4 0 44.6851 5.00032 3 14 4 0 45.8721 4.94112 4 -14 -4 0 40.0734 5.23432 2 -14 4 0 42.2350 4.40999 2 -16 4 0 75.5139 6.50096 3 -16 -4 0 93.7516 8.05627 2 16 4 0 84.5656 6.66762 4 16 -4 0 64.6884 11.5232 4 -16 4 0 81.0632 6.68699 2 -1 -5 0 311.959 15.7342 3 -1 5 0 307.699 15.9553 3 1 -5 0 308.335 15.8876 4 1 -5 0 321.501 15.7778 4 1 5 0 322.324 15.7480 4 1 5 0 322.308 15.7159 3 1 -5 0 322.206 15.3638 2 -1 -5 0 297.392 15.6818 2 -1 -5 0 310.533 15.6443 4 -1 -5 0 324.518 15.7078 2 1 -5 0 308.241 15.9533 3 -3 -5 0 60.2395 3.94135 2 3 5 0 60.9894 3.43879 3 3 -5 0 52.8933 3.91431 3 3 -5 0 57.0785 3.94333 4 -3 -5 0 59.7571 3.81577 2 -3 5 0 55.0559 4.00687 3 -3 5 0 53.6037 3.73055 4 -3 -5 0 60.6348 3.65802 4 -3 -5 0 57.5525 3.38453 3 3 5 0 61.6897 3.65622 4 -5 5 0 262.700 13.0921 2 -5 -5 0 255.771 13.1166 3 -5 5 0 252.979 14.1286 3 -5 -5 0 265.969 14.1467 2 -5 -5 0 273.898 13.2939 3 -5 5 0 260.579 13.0736 2 5 5 0 283.864 13.6839 4 5 -5 0 259.836 13.9442 4 7 -5 0 135.137 8.31051 4 -7 5 0 132.672 7.42786 2 -7 5 0 131.527 8.35787 3 -7 -5 0 140.930 7.24568 3 -7 -5 0 142.937 7.33602 3 -7 5 0 136.667 7.69953 2 -7 -5 0 133.868 8.45282 2 7 5 0 149.535 7.99020 4 -9 5 0 13.7835 2.16755 2 -9 -5 0 13.0334 1.63582 3 -9 -5 0 10.0591 2.58611 2 9 5 0 16.8929 2.66472 4 -9 5 0 14.1652 1.94969 2 9 -5 0 13.9059 2.99642 4 -9 -5 0 13.8264 1.77951 3 -9 5 0 12.3305 2.60356 3 -11 -5 0 126.290 7.17491 3 11 -5 0 136.881 9.07176 4 -11 -5 0 124.539 8.65063 2 11 5 0 142.775 8.23667 4 -11 5 0 122.743 8.50504 3 -11 5 0 123.552 7.69287 2 13 -5 0 14.4697 3.85389 4 13 5 0 14.8558 3.29908 4 -13 -5 0 10.2063 1.77007 3 -13 -5 0 15.8377 3.35279 2 -13 5 0 17.5622 2.90139 2 -13 5 0 13.6637 3.00552 3 -15 5 0 6.02611 2.58198 3 15 -5 0 16.3488 4.68750 4 -15 5 0 7.74446 2.79422 2 -15 -5 0 8.60245 3.51682 2 15 5 0 7.31314 2.94327 4 0 -6 0 5138.00 233.670 2 0 -6 0 4818.98 233.838 4 0 -6 0 4905.43 233.671 2 0 6 0 4861.44 234.044 3 0 -6 0 4662.47 234.027 3 -2 -6 0 28.8636 2.35446 4 -2 -6 0 32.3183 2.36547 3 -2 -6 0 35.3870 2.63674 2 2 6 0 33.0076 2.33126 3 -2 -6 0 32.9197 2.47291 2 2 -6 0 31.0426 2.72504 4 2 -6 0 30.2372 2.71514 3 -2 6 0 29.7600 2.57301 4 -2 6 0 27.1067 2.72335 3 2 6 0 32.8983 2.52381 4 -4 -6 0 1393.26 66.8365 3 4 -6 0 1364.04 67.4735 4 4 6 0 1386.23 67.1173 4 -4 -6 0 1435.47 67.0285 3 -4 -6 0 1334.84 67.5260 2 -4 6 0 1395.40 67.7505 3 -6 6 0 886.258 42.8757 2 -6 -6 0 912.906 44.2030 2 6 -6 0 873.074 43.9245 4 -6 -6 0 894.135 43.0037 3 -6 6 0 869.651 42.8292 2 -6 6 0 861.459 44.1668 3 -6 -6 0 880.732 42.9431 3 6 6 0 917.427 43.5560 4 -8 -6 0 103.598 5.42537 3 -8 -6 0 105.730 5.63957 3 -8 6 0 93.9018 5.59872 2 -8 6 0 96.5432 5.63621 2 8 6 0 101.016 6.29482 4 8 -6 0 102.219 6.98259 4 -8 -6 0 100.245 6.95225 2 -8 6 0 94.4703 6.84816 3 10 6 0 685.097 32.4321 4 -10 -6 0 639.222 31.4941 3 -10 -6 0 631.456 31.3387 3 -10 -6 0 614.420 33.1432 2 -10 6 0 624.838 31.8318 2 10 -6 0 664.672 33.1255 4 -10 6 0 637.922 33.0866 3 -12 -6 0 38.6771 4.97368 2 -12 6 0 40.1623 3.77936 2 -12 6 0 42.9823 4.96585 3 -12 -6 0 38.2420 2.91306 3 12 6 0 44.4081 4.40548 4 12 -6 0 56.0164 8.58183 4 -14 -6 0 179.853 11.8539 2 -14 6 0 176.223 10.4235 2 -14 6 0 173.194 11.2739 3 14 -6 0 171.141 12.2088 4 14 6 0 185.070 10.8168 4 1 7 0 1373.80 64.4216 3 1 7 0 1301.31 64.3927 4 1 -7 0 1406.04 63.9174 2 -1 -7 0 1275.33 64.2764 2 -1 7 0 1356.00 64.7107 3 -1 -7 0 1353.93 64.2817 2 1 -7 0 1231.13 64.6013 3 1 -7 0 1346.49 63.9378 2 1 -7 0 1317.14 64.6221 4 -1 -7 0 1307.06 64.4645 3 -3 -7 0 207.248 11.0226 2 3 7 0 203.735 10.8490 4 -3 -7 0 210.680 10.7124 3 -3 -7 0 193.647 11.0382 2 3 -7 0 212.014 11.2420 4 3 7 0 204.651 10.5689 3 -3 7 0 206.700 11.3820 3 -5 7 0 1642.49 80.2314 3 5 7 0 1624.76 79.4812 4 -5 -7 0 1641.80 80.0643 2 5 -7 0 1657.58 79.9495 4 -5 -7 0 1635.94 79.1032 3 -7 -7 0 58.4135 4.88207 2 7 -7 0 64.3143 5.06829 4 -7 -7 0 57.8337 3.55980 3 -7 7 0 54.6690 4.81141 3 7 7 0 62.2555 4.77332 4 -7 -7 0 56.0590 3.54825 3 -7 7 0 61.6703 3.42461 2 -7 7 0 61.3650 3.56493 2 -9 7 0 741.487 38.7989 2 9 7 0 827.183 39.6010 4 -9 7 0 808.911 38.8732 2 9 -7 0 835.517 40.3265 4 -9 7 0 793.355 40.4201 3 -9 -7 0 790.709 40.4554 2 -9 -7 0 779.954 38.6187 3 -11 7 0 46.0554 4.91226 3 11 7 0 48.5238 4.36448 4 -11 -7 0 42.1126 2.71463 3 -11 7 0 37.0223 3.41059 2 11 -7 0 44.4652 5.20164 4 -11 -7 0 39.1790 6.74350 2 -13 7 0 174.453 11.5193 3 13 7 0 186.103 10.9026 4 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775.948 42.9398 4 5 -7 -10 872.432 44.3239 2 5 7 10 896.245 43.3414 4 -7 -7 -10 107.358 7.96532 2 7 7 -10 107.897 7.92058 2 -7 7 10 97.7277 7.97876 3 7 -7 10 106.639 7.37106 4 -7 7 -10 109.650 7.12825 3 7 -7 -10 114.628 7.43135 4 -7 -7 10 116.745 8.41005 3 7 7 10 125.273 7.87013 4 -7 7 -10 124.144 7.45062 2 -7 -7 10 96.2727 6.26611 4 7 -7 -10 105.315 7.51685 2 -9 -7 -10 640.152 34.5177 2 9 7 -10 664.739 34.3970 2 9 7 -10 652.876 32.3249 4 -9 7 10 631.651 34.6339 3 -9 -7 10 560.707 34.2824 3 9 7 10 694.545 33.8938 4 9 -7 -10 709.711 33.4633 4 -9 7 -10 674.023 33.5122 2 -9 7 -10 671.649 33.5368 3 9 -7 -10 680.716 33.6187 2 11 7 -10 55.4213 3.94923 4 11 -7 10 51.3088 5.68566 4 11 7 -10 57.6605 6.38446 2 -11 7 10 44.0603 5.95331 3 -11 -7 -10 53.7263 6.44477 2 11 7 10 64.6260 5.84785 4 -11 7 -10 48.5078 5.28006 2 11 -7 -10 51.5077 4.83446 4 11 -7 -10 53.8706 5.06095 2 -11 -7 10 44.9441 5.62004 3 13 -7 10 137.979 10.7356 4 -13 7 10 158.258 14.6512 3 -13 7 -10 151.924 9.51182 3 13 7 10 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2 2 -23 2.22660 3.71571 2 -2 2 23 9.13813 3.83775 3 2 -2 23 3.45164 3.28992 3 -2 -2 -23 3.06857 3.57885 2 2 -2 -23 -2.3150 3.42509 2 2 2 23 6.59305 3.22513 3 -4 -2 -23 42.9897 6.74008 2 4 2 -23 37.7175 6.68786 2 -4 2 23 32.4041 5.41284 3 4 -2 23 39.9468 5.22162 3 -4 -2 23 47.4497 5.84793 3 4 -2 -23 42.5073 6.81455 2 4 2 23 50.2568 5.29456 3 -1 -3 -23 11.5264 4.50721 2 1 -3 23 5.93417 3.71661 3 -1 3 23 11.9540 3.68726 3 1 3 -23 -2.4559 3.42663 2 1 3 23 11.6609 3.44998 3 1 -3 -23 11.5009 3.75666 2 -3 3 23 15.8962 5.62301 3 -3 -3 -23 11.3480 4.89767 2 3 3 -23 11.7545 4.24696 2 3 -3 23 14.2967 3.83860 3 -3 -3 23 10.4411 3.87731 3 3 3 23 10.0319 3.19670 3 3 -3 -23 12.6101 4.53293 2 0 4 -23 39.8630 8.10792 2 0 -4 23 35.1715 7.31931 3 0 -4 -23 41.5382 6.35223 2 0 4 23 50.5866 6.02206 3 -2 4 23 69.6603 6.82715 3 -2 -4 -23 56.5891 7.48689 2 2 -4 23 62.4830 7.22855 3 2 4 -23 46.5638 7.08057 2 2 -4 -23 76.4060 7.82960 2 2 4 23 54.0238 6.03597 3 -2 -4 23 57.1894 6.72207 3 -1 5 23 49.3551 6.49507 3 1 5 -23 52.1794 6.97481 2 1 -5 23 74.2798 7.38527 3 -1 -5 -23 87.2499 8.65492 2 1 5 23 62.9693 6.57439 3 -1 -5 23 70.1572 7.44895 3 1 -5 -23 49.6929 6.88264 2 3 5 -23 11.5153 4.68484 2 -3 -5 -23 8.00996 4.93937 2 -3 5 23 14.5854 4.31960 3 3 -5 23 13.3589 3.97397 3 3 -5 -23 10.4099 4.05635 2 -3 -5 23 13.1097 4.26434 3 3 5 23 12.8149 3.50013 3 0 -6 -23 -1.7194 3.53783 2 0 6 23 2.87811 3.61902 3 0 6 -23 -0.6666 3.78090 2 0 -6 23 -0.3222 3.45466 3 0 0 -24 4.76889 3.83734 2 -2 0 24 12.2395 4.00825 3 2 0 -24 14.2355 4.37609 2 2 0 24 14.0948 3.49795 3 -2 0 -24 8.69810 4.29699 2 1 -1 24 7.90041 5.03781 3 -1 1 24 11.0516 4.85210 3 -1 -1 -24 -4.3469 3.53566 2 1 1 -24 11.5317 4.13088 2 -1 -1 24 4.65909 3.47958 3 1 1 24 5.59411 3.19800 3 1 -1 -24 3.28538 4.14024 2 -1 1 -24 5.09184 3.92242 2 0 2 24 20.4607 4.18106 3 0 -2 -24 19.1979 4.82442 2 0 -2 24 18.0419 4.17851 3 0 2 -24 14.4943 4.74341 2 0 0 0 0.00 0.00 0 _exptl_absorpt_process_details ) SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10 ) _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_max 0.0998 _exptl_absorpt_correction_T_min 0.0425 _exptl_special_details ) The following wavelength and cell were deduced by SADABS from the direction cosines etc. They are given here for emergency use only: CELL 0.71073 11.646 13.994 16.928 90.013 90.012 90.011 ) ; _shelx_hkl_checksum 52215 _shelx_res_file ; TITL 21popova02 in Cmcm 21popova02.res created by SHELXL-2018/3 at 21:03:17 on 19-Mar-2021 CELL 0.71073 11.6462 13.9943 16.9225 90 90 90 ZERR 4 0.0003 0.0004 0.0005 0 0 0 LATT 7 SYMM -X,-Y,0.5+Z SYMM -X,+Y,0.5-Z SYMM +X,-Y,-Z SFAC C H Br N O Ru S UNIT 16 88 32 32 12 4 16 EQIV $1 1-X,1-Y,-0.5+Z EQIV $2 +X,1-Y,1-Z EQIV $3 -0.5+X,0.5+Y,+Z SADI 0.002 O1 H1c O1 H1d L.S. 12 PLAN 12 SIZE 0.3 0.2 0.02 TEMP -123 CONF HTAB N1 O1 HTAB O1 Br3 HTAB O1 O2 HTAB N1 Br4 HTAB N2 Br1_$1 HTAB N2 Br2_$2 HTAB N2 Br4 HTAB O2 Br4_$3 BOND $H MORE 3 LIST 4 fmap 2 acta WGHT 0.023700 6.898000 FVAR 0.10198 RU1 6 0.500000 0.654226 0.750000 10.25000 0.01735 0.01668 = 0.01860 0.00000 0.00000 0.00000 BR1 3 0.500000 0.779299 0.853648 10.50000 0.02324 0.02066 = 0.02144 -0.00283 0.00000 0.00000 BR2 3 0.500000 0.525830 0.648217 10.50000 0.03078 0.02150 = 0.02447 -0.00468 0.00000 0.00000 BR3 3 0.286493 0.655508 0.750000 10.50000 0.01777 0.02213 = 0.03706 0.00000 0.00000 -0.00096 BR4 3 0.500000 0.171689 0.584162 10.50000 0.02496 0.02304 = 0.03352 0.00104 0.00000 0.00000 S1 7 0.182836 0.474936 0.556227 11.00000 0.02798 0.02385 = 0.02382 0.00161 0.00335 0.00435 N1 4 0.295711 0.332734 0.618124 11.00000 0.02868 0.02557 = 0.02979 0.00426 0.00333 0.00404 H1A 2 0.264405 0.352801 0.657108 11.00000 -1.20000 H1B 2 0.329722 0.285348 0.616491 11.00000 -1.20000 N2 4 0.332149 0.351629 0.486328 11.00000 0.03704 0.02718 = 0.03452 0.00342 0.01277 0.00627 H2A 2 0.331017 0.386071 0.442806 11.00000 -1.20000 H2B 2 0.379921 0.309724 0.489335 11.00000 -1.20000 C1 1 0.281565 0.377713 0.551652 11.00000 0.02282 0.01990 = 0.02950 0.00153 0.00233 -0.00191 O1 5 0.206097 0.429934 0.750000 10.50000 0.03292 0.02537 = 0.03329 0.00000 0.00000 0.00033 H1C 2 0.248910 0.478367 0.750000 10.50000 -1.50000 H1D 2 0.136240 0.445318 0.750000 10.50000 -1.50000 O2 5 0.000000 0.532135 0.750000 10.25000 0.04169 0.03183 = 0.03453 0.00000 0.00000 0.00000 H2 2 0.000000 0.579395 0.709457 10.50000 -1.50000 HKLF 4 REM 21popova02 in Cmcm REM wR2 = 0.056656, GooF = S = 1.06922, Restrained GooF = 1.06898 for all data REM R1 = 0.022692 for 2057 Fo > 4sig(Fo) and 0.026567 for all 2269 data REM 93 parameters refined using 1 restraints END WGHT 0.0237 6.8977 REM Highest difference peak 1.061, deepest hole -0.594, 1-sigma level 0.112 Q1 1 0.5000 0.3127 0.7500 10.25000 0.05 1.06 Q2 1 0.3374 0.3401 0.3784 11.00000 0.05 0.76 Q3 1 0.2917 0.6273 0.7825 11.00000 0.05 0.64 Q4 1 0.1769 0.5336 0.5876 11.00000 0.05 0.63 Q5 1 0.5505 0.7607 0.8517 11.00000 0.05 0.62 Q6 1 0.5000 0.1651 0.6328 10.50000 0.05 0.53 Q7 1 0.1281 0.3263 0.7500 10.50000 0.05 0.50 Q8 1 0.5338 0.6180 0.7500 10.50000 0.05 0.49 Q9 1 0.5392 0.5265 0.5991 11.00000 0.05 0.49 Q10 1 0.0417 0.4727 0.7500 10.50000 0.05 0.47 Q11 1 0.5363 0.7296 0.7500 10.50000 0.05 0.46 Q12 1 0.4395 0.4990 0.6529 11.00000 0.05 0.42 ; _shelx_res_checksum 53256 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y, -z-1/2' 'x, -y, z-1/2' '-x, y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, y+1/2, -z-1/2' 'x+1/2, -y+1/2, z-1/2' '-x+1/2, y+1/2, z' 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_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ru Ru1 0.500000 0.65423(2) 0.750000 0.01754(8) Uani d 1 . . Br Br1 0.500000 0.77930(2) 0.85365(2) 0.02178(8) Uani d 1 . . Br Br2 0.500000 0.52583(2) 0.64822(2) 0.02559(8) Uani d 1 . . Br Br3 0.28649(3) 0.65551(2) 0.750000 0.02565(9) Uani d 1 . . Br Br4 0.500000 0.17169(2) 0.58416(2) 0.02717(9) Uani d 1 . . S S1 0.18284(5) 0.47494(4) 0.55623(4) 0.02521(13) Uani d 1 . . N N1 0.2957(2) 0.33273(17) 0.61812(15) 0.0280(5) Uani d 1 . . H H1A 0.264(3) 0.353(2) 0.657(2) 0.034 Uiso d 1 . . H H1B 0.330(3) 0.285(2) 0.616(2) 0.034 Uiso d 1 . . N N2 0.3321(2) 0.35163(17) 0.48633(16) 0.0329(5) Uani d 1 . . H H2A 0.331(3) 0.386(3) 0.443(2) 0.039 Uiso d 1 . . H H2B 0.380(3) 0.310(2) 0.489(2) 0.039 Uiso d 1 . . C C1 0.2816(2) 0.37771(17) 0.55165(16) 0.0241(5) Uani d 1 . . O O1 0.2061(2) 0.4299(2) 0.750000 0.0305(6) Uani d 1 . . H H1C 0.249(4) 0.478(3) 0.750000 0.046 Uiso d 1 . . H H1D 0.136(3) 0.445(4) 0.750000 0.046 Uiso d 1 . . O O2 0.000000 0.5321(3) 0.750000 0.0360(9) Uani d 1 . . H H2 0.000000 0.579(4) 0.709(3) 0.054 Uiso d 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 Ru1 0.01735(16) 0.01668(16) 0.01860(17) 0.000 0.000 0.000 Br1 0.02324(15) 0.02066(15) 0.02144(16) 0.000 0.000 -0.00283(11) Br2 0.03078(18) 0.02150(16) 0.02447(17) 0.000 0.000 -0.00468(12) Br3 0.01777(15) 0.02213(16) 0.0371(2) -0.00096(11) 0.000 0.000 Br4 0.02496(16) 0.02304(16) 0.0335(2) 0.000 0.000 0.00104(13) S1 0.0280(3) 0.0238(3) 0.0238(3) 0.0043(2) 0.0033(2) 0.0016(2) N1 0.0287(11) 0.0256(11) 0.0298(12) 0.0040(8) 0.0033(9) 0.0043(9) N2 0.0370(13) 0.0272(11) 0.0345(13) 0.0063(10) 0.0128(11) 0.0034(10) C1 0.0228(11) 0.0199(10) 0.0295(13) -0.0019(9) 0.0023(9) 0.0015(9) O1 0.0329(14) 0.0254(13) 0.0333(15) 0.0003(11) 0.000 0.000 O2 0.042(2) 0.032(2) 0.035(2) 0.000 0.000 0.000 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' Br Br -0.2901 2.4595 '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' Ru Ru -1.2594 0.8363 '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 Br1 Ru1 Br1 . 10_557 90.122(19) ? Br1 Ru1 Br3 . 3_656 89.708(8) ? Br1 Ru1 Br3 10_557 3_656 89.708(8) ? Br1 Ru1 Br3 . . 89.708(8) ? Br1 Ru1 Br3 10_557 . 89.708(8) ? Br3 Ru1 Br3 3_656 . 179.17(2) ? Br1 Ru1 Br2 . 10_557 91.151(12) ? Br1 Ru1 Br2 10_557 10_557 178.727(16) ? Br3 Ru1 Br2 3_656 10_557 90.298(8) ? Br3 Ru1 Br2 . 10_557 90.298(8) ? Br1 Ru1 Br2 . . 178.729(16) ? Br1 Ru1 Br2 10_557 . 91.150(12) ? Br3 Ru1 Br2 3_656 . 90.298(8) ? Br3 Ru1 Br2 . . 90.298(8) ? Br2 Ru1 Br2 10_557 . 87.58(2) ? C1 S1 S1 . 4_566 102.90(9) ? C1 N1 H1A . . 119(2) ? C1 N1 H1B . . 117(3) ? H1A N1 H1B . . 124(4) ? C1 N2 H2A . . 123(2) ? C1 N2 H2B . . 117(3) ? H2A N2 H2B . . 117(3) ? N1 C1 N2 . . 122.7(2) ? N1 C1 S1 . . 114.4(2) ? N2 C1 S1 . . 122.8(2) ? H1C O1 H1D . . 112(5) ? 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 Ru1 Br1 . 2.4779(4) y Ru1 Br1 10_557 2.4779(4) y Ru1 Br3 3_656 2.4866(3) y Ru1 Br3 . 2.4866(3) y Ru1 Br2 10_557 2.4890(4) y Ru1 Br2 . 2.4890(4) y S1 C1 . 1.783(2) ? S1 S1 4_566 2.0282(12) ? N1 C1 . 1.299(3) ? N1 H1A . 0.80(4) ? N1 H1B . 0.77(3) ? N2 C1 . 1.305(3) ? N2 H2A . 0.88(4) ? N2 H2B . 0.81(3) ? O1 H1C . 0.84(3) ? O1 H1D . 0.84(3) ? O2 H2 . 0.95(5) ? 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 _geom_hbond_publ_flag N1 H1A O1 . 0.80(4) 2.02(4) 2.814(3) 167(3) yes O1 H1C Br3 . 0.84(3) 2.52(3) 3.293(3) 154(4) yes O1 H1D O2 . 0.84(3) 2.00(4) 2.794(4) 157(5) yes N1 H1B Br4 . 0.77(3) 2.60(4) 3.327(2) 157(3) yes N2 H2B Br1 2_664 0.81(3) 2.96(4) 3.496(2) 125(3) yes N2 H2A Br2 4_566 0.88(4) 2.79(4) 3.456(2) 134(3) yes N2 H2B Br4 . 0.81(3) 2.87(4) 3.592(3) 149(3) yes O2 H2 Br4 5_455 0.95(5) 2.48(5) 3.419(2) 167(4) yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag S1 S1 C1 N1 4_566 . . . -179.53(18) ? S1 S1 C1 N2 4_566 . . . -2.0(2) ?