Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_name_full 'J.Chem.Soc.,Dalton Trans.' _journal_coden_Cambridge 0186 loop_ _publ_author_name J.Dilworth A.R.Cowley P.S.Donnelly J.Woollard-Shore _publ_contact_author_name 'Prof J Dilworth' _publ_contact_author_address ; Inorganic Chemistry Laboratory University of Oxford South Parks Road Oxford OX1 3QR UNITED KINGDOM ; _publ_contact_author_email JON.DILWORTH@CHEM.OX.AC.UK _publ_section_title ; Synthesis and Characterisation of New Homoleptic Rhenium Thiosemicarbazone Complexes ; data_CRYSTALS_1 _database_code_CSD 196178 _audit_creation_date 01-24-10 _audit_creation_method CRYSTALS_ver_12-03-99 # Diffractometer details #========================================================================== _diffrn_measurement_device_type ; Nonius KappaCCD ; _diffrn_radiation_monochromator graphite _computing_data_collection ; KappaCCD software 'Collect' (Nonius, 2000) ; _computing_data_reduction ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; #========================================================================== # General computing #========================================================================== _computing_structure_refinement ; CRYSTALS (Watkin et al, 2001) ; _computing_publication_material ; CRYSTALS (Watkin et al, 2001) ; _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point 'not measured' _refine_ls_matrix_type full _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed #============================================================= _cell_length_a 13.3321(2) _cell_angle_alpha 106.4656(8) _cell_length_b 17.7129(3) _cell_angle_beta 100.6320(8) _cell_length_c 19.3778(4) _cell_angle_gamma 93.6732(8) _cell_volume 4280.1 _symmetry_cell_setting 'Triclinic ' _symmetry_space_group_name_H-M 'P -1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 International_Tables_Vol_IV_Table_2.2B 'Cl ' 0.1320 0.1590 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 International_Tables_Vol_IV_Table_2.2B 'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 International_Tables_Vol_IV_Table_2.2B 'O ' 0.0080 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 International_Tables_Vol_IV_Table_2.2B 'P ' 0.0900 0.0950 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 International_Tables_Vol_IV_Table_2.2B 'Re ' -1.5980 7.2320 28.7621 1.6719 15.7189 9.0923 14.5564 0.3505 5.4417 52.0861 10.4720 International_Tables_Vol_IV_Table_2.2B _chemical_formula_sum ' C44 H42 Cl2 N2 O5 P2 Re2 ' _chemical_formula_moiety ' C44 H42 Cl2 N2 O5 P2 Re2 ' _chemical_compound_source ; ? ; _chemical_formula_weight 1184.09 _cell_measurement_reflns_used 55415 _cell_measurement_theta_min 5 _cell_measurement_theta_max 28 _cell_measurement_temperature 150 _cell_formula_units_Z 4 _exptl_crystal_description ' fragment ' _exptl_crystal_colour ' red ' _exptl_crystal_size_min 0.03 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_max 0.12 _exptl_crystal_density_diffrn 1.837 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 2285.737 _exptl_absorpt_coefficient_mu 5.898 _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _exptl_absorpt_correction_T_min 0.49 _exptl_absorpt_correction_T_max 0.84 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 150 _diffrn_reflns_number 55415 _reflns_number_total 19351 _diffrn_reflns_av_R_equivalents 0.068 _diffrn_measured_fraction_theta_max 0.992 _reflns_number_gt 13260 _diffrn_reflns_theta_min 5.17 _diffrn_reflns_theta_max 27.51 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _reflns_limit_h_min -17 _reflns_limit_h_max 16 _reflns_limit_k_min -23 _reflns_limit_k_max 22 _reflns_limit_l_min 0 _reflns_limit_l_max 25 _refine_diff_density_min -4.32 _refine_diff_density_max 3.55 _reflns_threshold_expression >3.00\s(I) _refine_ls_number_reflns 13260 _refine_ls_number_parameters 1035 _refine_ls_R_factor_gt 0.0451 _refine_ls_wR_factor_ref 0.0484 _refine_ls_goodness_of_fit_ref 1.0703 _refine_ls_shift/su_max 0.031930 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 4 parameters, Carruthers & Watkin , 1979, 4.34 -.525 3.38 0.665 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type Re1 0.31444(2) 0.293501(15) 0.107759(14) 0.0183 1.0000 Uani Cl1 0.47409(14) 0.34396(11) 0.1919(1) 0.0315 1.0000 Uani Cl2 0.34518(14) 0.3236(1) 0.00242(9) 0.0257 1.0000 Uani N1 0.1633(5) 0.2520(3) 0.0556(3) 0.0216 1.0000 Uani C1 0.0996(5) 0.2284(4) 0.0897(4) 0.0246 1.0000 Uani C2 0.1437(6) 0.2279(4) 0.1626(4) 0.0263 1.0000 Uani C3 0.0901(7) 0.2047(5) 0.2097(5) 0.0374 1.0000 Uani C4 0.1409(8) 0.2040(6) 0.2784(5) 0.0475 1.0000 Uani C5 0.2460(7) 0.2273(5) 0.2981(4) 0.0372 1.0000 Uani C6 0.2977(7) 0.2522(5) 0.2504(4) 0.0328 1.0000 Uani N2 0.2472(5) 0.2530(3) 0.1839(3) 0.0239 1.0000 Uani C7 -0.0142(7) 0.2051(5) 0.0574(5) 0.0372 1.0000 Uani P1 0.38314(15) 0.1662(1) 0.0606(1) 0.0236 1.0000 Uani C8 0.4896(6) 0.1715(4) 0.0133(4) 0.0253 1.0000 Uani C9 0.5721(7) 0.2312(5) 0.0443(5) 0.0358 1.0000 Uani C10 0.6553(7) 0.2345(6) 0.0114(5) 0.0417 1.0000 Uani C11 0.6576(7) 0.1770(6) -0.0539(5) 0.0433 1.0000 Uani C12 0.5749(8) 0.1189(5) -0.0860(5) 0.0384 1.0000 Uani C13 0.4902(7) 0.1147(5) -0.0540(4) 0.0326 1.0000 Uani C14 0.4316(7) 0.1251(4) 0.1347(4) 0.0350 1.0000 Uani C15 0.5352(9) 0.1289(6) 0.1633(6) 0.0560 1.0000 Uani C16 0.5674(13) 0.1019(7) 0.2234(7) 0.0831 1.0000 Uani C17 0.4963(15) 0.0739(6) 0.2577(6) 0.0799 1.0000 Uani C18 0.3938(13) 0.0690(6) 0.2284(6) 0.0670 1.0000 Uani C19 0.3595(9) 0.0947(5) 0.1673(5) 0.0453 1.0000 Uani C20 0.2934(6) 0.0871(4) -0.0072(4) 0.0289 1.0000 Uani C21 0.3007(6) 0.0067(4) -0.0110(5) 0.0319 1.0000 Uani C22 0.2362(7) -0.0530(5) -0.0685(5) 0.0390 1.0000 Uani C23 0.1689(7) -0.0342(5) -0.1211(5) 0.0387 1.0000 Uani C24 0.1594(6) 0.0442(5) -0.1183(4) 0.0319 1.0000 Uani C25 0.2211(6) 0.1056(4) -0.0600(4) 0.0283 1.0000 Uani P2 0.26184(13) 0.4269(1) 0.15738(9) 0.0188 1.0000 Uani C26 0.3206(5) 0.5091(4) 0.1323(4) 0.0227 1.0000 Uani C27 0.4187(6) 0.5083(5) 0.1158(4) 0.0293 1.0000 Uani C28 0.4587(5) 0.5690(5) 0.0935(5) 0.0305 1.0000 Uani C29 0.4044(6) 0.6323(5) 0.0888(5) 0.0330 1.0000 Uani C30 0.3081(6) 0.6353(4) 0.1075(4) 0.0307 1.0000 Uani C31 0.2665(6) 0.5735(4) 0.1289(4) 0.0272 1.0000 Uani C32 0.2842(5) 0.4607(4) 0.2583(4) 0.0194 1.0000 Uani C33 0.3625(5) 0.5215(4) 0.2982(4) 0.0269 1.0000 Uani C34 0.3841(6) 0.5456(5) 0.3753(4) 0.0323 1.0000 Uani C35 0.3267(6) 0.5075(6) 0.4113(4) 0.0399 1.0000 Uani C36 0.2486(7) 0.4467(5) 0.3722(4) 0.0342 1.0000 Uani C37 0.2274(6) 0.4228(4) 0.2956(4) 0.0267 1.0000 Uani C38 0.1255(5) 0.4280(4) 0.1220(4) 0.0225 1.0000 Uani C39 0.0954(6) 0.4124(4) 0.0457(4) 0.0262 1.0000 Uani C40 -0.0074(6) 0.4095(5) 0.0137(4) 0.0331 1.0000 Uani C41 -0.0804(6) 0.4219(5) 0.0559(5) 0.0363 1.0000 Uani C42 -0.0523(6) 0.4384(6) 0.1314(5) 0.0454 1.0000 Uani C43 0.0512(6) 0.4418(5) 0.1647(4) 0.0309 1.0000 Uani Re2 0.23738(2) 0.287165(16) 0.585120(14) 0.0184 1.0000 Uani Cl3 0.37511(14) 0.39066(11) 0.6348(1) 0.0321 1.0000 Uani Cl4 0.17036(15) 0.30526(12) 0.47050(9) 0.0308 1.0000 Uani N3 0.1273(4) 0.1931(3) 0.5625(3) 0.0225 1.0000 Uani C44 0.1189(5) 0.1552(4) 0.6092(4) 0.0240 1.0000 Uani C45 0.1954(5) 0.1829(4) 0.6769(4) 0.0213 1.0000 Uani C46 0.2031(7) 0.1525(5) 0.7355(4) 0.0341 1.0000 Uani C47 0.2820(7) 0.1845(5) 0.7958(4) 0.0367 1.0000 Uani C48 0.3489(6) 0.2485(5) 0.7975(4) 0.0344 1.0000 Uani C49 0.3372(5) 0.2786(4) 0.7396(4) 0.0252 1.0000 Uani N4 0.2623(4) 0.2466(3) 0.6786(3) 0.0205 1.0000 Uani C50 0.0353(7) 0.0881(5) 0.5951(4) 0.0364 1.0000 Uani P3 0.36327(14) 0.20249(12) 0.5339(1) 0.0262 1.0000 Uani C51 0.4473(6) 0.2430(6) 0.4837(4) 0.0364 1.0000 Uani C52 0.5272(6) 0.1988(7) 0.4608(4) 0.0453 1.0000 Uani C53 0.5862(7) 0.2260(9) 0.4175(5) 0.0618 1.0000 Uani C54 0.5688(8) 0.293(1) 0.3996(6) 0.0683 1.0000 Uani C55 0.4932(8) 0.3368(8) 0.4234(5) 0.0593 1.0000 Uani C56 0.4320(6) 0.3106(5) 0.4655(4) 0.0355 1.0000 Uani C57 0.4501(6) 0.1846(4) 0.6100(4) 0.0268 1.0000 Uani C58 0.5390(6) 0.2364(5) 0.6458(4) 0.0323 1.0000 Uani C59 0.6026(7) 0.2278(6) 0.7085(5) 0.0409 1.0000 Uani C60 0.5774(8) 0.1682(6) 0.7364(5) 0.0466 1.0000 Uani C61 0.4853(9) 0.1162(6) 0.7021(6) 0.0498 1.0000 Uani C62 0.4226(7) 0.1241(5) 0.6382(5) 0.0361 1.0000 Uani C63 0.3119(6) 0.1045(5) 0.4688(4) 0.0323 1.0000 Uani C64 0.3674(7) 0.0405(6) 0.4646(6) 0.0584 1.0000 Uani C65 0.3283(9) -0.0326(6) 0.4110(7) 0.0695 1.0000 Uani C66 0.2364(8) -0.0406(6) 0.3622(6) 0.0571 1.0000 Uani C67 0.1824(7) 0.0238(6) 0.3675(5) 0.0458 1.0000 Uani C68 0.2194(6) 0.0972(5) 0.4202(4) 0.0312 1.0000 Uani P4 0.12980(13) 0.3835(1) 0.64498(9) 0.0194 1.0000 Uani C69 0.1179(6) 0.4738(4) 0.6185(4) 0.0247 1.0000 Uani C70 0.1814(7) 0.5002(5) 0.5796(5) 0.0395 1.0000 Uani C71 0.1701(9) 0.5718(6) 0.5628(6) 0.0518 1.0000 Uani C72 0.0964(8) 0.6171(6) 0.5847(6) 0.0455 1.0000 Uani C73 0.0296(8) 0.5920(6) 0.6251(7) 0.0527 1.0000 Uani C74 0.0405(7) 0.5206(5) 0.6403(6) 0.0443 1.0000 Uani C75 0.1816(5) 0.4191(4) 0.7445(4) 0.0209 1.0000 Uani C76 0.2547(6) 0.4856(4) 0.7745(4) 0.0269 1.0000 Uani C77 0.2991(6) 0.5088(5) 0.8493(4) 0.0325 1.0000 Uani C78 0.2730(6) 0.4641(6) 0.8926(4) 0.0356 1.0000 Uani C79 0.2031(6) 0.3978(5) 0.8638(4) 0.0324 1.0000 Uani C80 0.1569(6) 0.3738(4) 0.7882(4) 0.0258 1.0000 Uani C81 -0.0049(6) 0.3443(4) 0.6320(4) 0.0239 1.0000 Uani C82 -0.0622(6) 0.3632(5) 0.6870(4) 0.0310 1.0000 Uani C83 -0.1663(7) 0.3359(6) 0.6696(5) 0.0423 1.0000 Uani C84 -0.2125(7) 0.2901(6) 0.6004(5) 0.0476 1.0000 Uani C85 -0.1568(6) 0.2711(6) 0.5457(5) 0.0421 1.0000 Uani C86 -0.0523(5) 0.2982(5) 0.5616(4) 0.0277 1.0000 Uani Re3 -0.04904(2) 0.22460(2) -0.164175(18) 0.0344 1.0000 Uani O1 -0.0792(8) 0.3171(5) -0.1667(4) 0.0745 1.0000 Uani O2 0.0604(5) 0.2366(4) -0.0968(3) 0.0431 1.0000 Uani O3 -0.0260(6) 0.1766(6) -0.2476(4) 0.0737 1.0000 Uani O4 -0.1503(8) 0.1795(9) -0.1453(8) 0.1205 1.0000 Uani Re4 -0.12308(3) 0.10323(2) 0.35228(2) 0.0505 1.0000 Uani O5 -0.1682(14) 0.1777(7) 0.3263(8) 0.1627 1.0000 Uani O6 -0.0336(6) 0.1348(5) 0.4313(4) 0.0653 1.0000 Uani O7 -0.0746(8) 0.0395(6) 0.2891(5) 0.0831 1.0000 Uani O8 -0.2252(9) 0.0485(9) 0.3624(9) 0.1341 1.0000 Uani O9 0.0844(13) 0.0350(9) 0.0691(11) 0.1532 1.0000 Uani C87 0.1074(15) -0.0126(11) 0.1145(18) 0.1536 1.0000 Uani O10 -0.177(1) 0.2347(6) 0.2018(6) 0.1015 1.0000 Uani C88 -0.2222(14) 0.3018(8) 0.2133(8) 0.0881 1.0000 Uani H1 0.126(7) 0.260(6) 0.009(5) 0.04(3) 1.0000 Uiso H2 0.091(7) 0.168(6) 0.515(4) 0.04(3) 1.0000 Uiso H3 0.0290 0.0121 0.0238 0.1999 1.0000 Uiso H4 -0.1738 0.2148 0.2454 0.1228 1.0000 Uiso H31 0.0142 0.1884 0.1938 0.0428 1.0000 Uiso H41 0.1030 0.1873 0.3127 0.0583 1.0000 Uiso H51 0.2853 0.2263 0.3470 0.0444 1.0000 Uiso H61 0.3734 0.2696 0.2660 0.0386 1.0000 Uiso H71 -0.0483 0.1889 0.0937 0.0437 1.0000 Uiso H72 -0.0451 0.2513 0.0460 0.0437 1.0000 Uiso H73 -0.0244 0.1597 0.0112 0.0437 1.0000 Uiso H91 0.5713 0.2727 0.0914 0.0430 1.0000 Uiso H101 0.7135 0.2781 0.0347 0.0519 1.0000 Uiso H111 0.7184 0.1778 -0.0773 0.0572 1.0000 Uiso H121 0.5758 0.0785 -0.1338 0.0516 1.0000 Uiso H131 0.4310 0.0721 -0.0784 0.0402 1.0000 Uiso H151 0.5872 0.1512 0.1407 0.0633 1.0000 Uiso H161 0.6426 0.1026 0.2424 0.0865 1.0000 Uiso H171 0.5199 0.0577 0.3028 0.0923 1.0000 Uiso H181 0.3424 0.0465 0.2512 0.0840 1.0000 Uiso H191 0.2842 0.0915 0.1470 0.0599 1.0000 Uiso H211 0.3513 -0.0073 0.0270 0.0392 1.0000 Uiso H221 0.2397 -0.1098 -0.0709 0.0468 1.0000 Uiso H231 0.1252 -0.0778 -0.1627 0.0433 1.0000 Uiso H241 0.1092 0.0569 -0.1573 0.0360 1.0000 Uiso H251 0.2133 0.1623 -0.0565 0.0338 1.0000 Uiso H271 0.4596 0.4639 0.1203 0.0363 1.0000 Uiso H281 0.5280 0.5673 0.0806 0.0369 1.0000 Uiso H291 0.4341 0.6756 0.0720 0.0397 1.0000 Uiso H301 0.2694 0.6814 0.1056 0.0358 1.0000 Uiso H311 0.1974 0.5753 0.1420 0.0316 1.0000 Uiso H331 0.4037 0.5483 0.2716 0.0296 1.0000 Uiso H341 0.4400 0.5896 0.4040 0.0348 1.0000 Uiso H351 0.3418 0.5243 0.4663 0.0450 1.0000 Uiso H361 0.2077 0.4200 0.3989 0.0412 1.0000 Uiso H371 0.1716 0.3785 0.2672 0.0331 1.0000 Uiso H391 0.1478 0.4034 0.0143 0.0306 1.0000 Uiso H401 -0.0286 0.3981 -0.0408 0.0377 1.0000 Uiso H411 -0.1543 0.4190 0.0319 0.0383 1.0000 Uiso H421 -0.1055 0.4479 0.1621 0.0502 1.0000 Uiso H431 0.0719 0.4541 0.2194 0.0352 1.0000 Uiso H461 0.1522 0.1078 0.7341 0.0406 1.0000 Uiso H471 0.2911 0.1618 0.8380 0.0440 1.0000 Uiso H481 0.4059 0.2727 0.8414 0.0396 1.0000 Uiso H491 0.3852 0.3255 0.7422 0.0292 1.0000 Uiso H501 0.0433 0.0673 0.6385 0.0421 1.0000 Uiso H502 -0.0334 0.1076 0.5871 0.0421 1.0000 Uiso H503 0.0403 0.0446 0.5503 0.0421 1.0000 Uiso H521 0.5410 0.1498 0.4751 0.0490 1.0000 Uiso H531 0.6417 0.1954 0.3997 0.0684 1.0000 Uiso H541 0.6113 0.3110 0.3685 0.0757 1.0000 Uiso H551 0.4822 0.3870 0.4107 0.0670 1.0000 Uiso H561 0.3765 0.3418 0.4822 0.0414 1.0000 Uiso H581 0.5580 0.2807 0.6263 0.0363 1.0000 Uiso H591 0.6666 0.2656 0.7330 0.0473 1.0000 Uiso H601 0.6236 0.1613 0.7806 0.0517 1.0000 Uiso H611 0.4647 0.0737 0.7233 0.0642 1.0000 Uiso H621 0.3585 0.0865 0.6133 0.0437 1.0000 Uiso H641 0.4348 0.0462 0.4994 0.0580 1.0000 Uiso H651 0.3677 -0.0792 0.4083 0.0703 1.0000 Uiso H661 0.2092 -0.0923 0.3235 0.0577 1.0000 Uiso H671 0.1149 0.0179 0.3326 0.0481 1.0000 Uiso H681 0.1796 0.1435 0.4227 0.0346 1.0000 Uiso H701 0.2364 0.4681 0.5630 0.0530 1.0000 Uiso H711 0.2171 0.5897 0.5343 0.0662 1.0000 Uiso H721 0.0894 0.6679 0.5723 0.0565 1.0000 Uiso H731 -0.0242 0.6251 0.6423 0.0701 1.0000 Uiso H741 -0.0078 0.5016 0.6675 0.0585 1.0000 Uiso H761 0.2753 0.5167 0.7424 0.0333 1.0000 Uiso H771 0.3498 0.5577 0.8716 0.0348 1.0000 Uiso H781 0.3060 0.4807 0.9462 0.0423 1.0000 Uiso H791 0.1847 0.3663 0.8960 0.0439 1.0000 Uiso H801 0.1068 0.3245 0.7663 0.0316 1.0000 Uiso H821 -0.0285 0.3961 0.7383 0.0358 1.0000 Uiso H831 -0.2079 0.3501 0.7084 0.0513 1.0000 Uiso H841 -0.2874 0.2700 0.5890 0.0543 1.0000 Uiso H851 -0.1914 0.2381 0.4947 0.0481 1.0000 Uiso H861 -0.0116 0.2843 0.5223 0.0326 1.0000 Uiso H871 0.1635 0.0166 0.1577 0.2055 1.0000 Uiso H872 0.0447 -0.0260 0.1322 0.2055 1.0000 Uiso H873 0.1307 -0.0625 0.0863 0.2055 1.0000 Uiso H881 -0.2254 0.3221 0.1699 0.0959 1.0000 Uiso H882 -0.1813 0.3428 0.2584 0.0959 1.0000 Uiso H883 -0.2934 0.2904 0.2203 0.0959 1.0000 Uiso 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 0.02191(13) 0.01614(12) 0.01655(12) 0.00436(9) 0.0032(1) 0.0054(1) Cl1 0.0303(9) 0.0310(9) 0.0289(9) 0.0059(7) -0.0015(7) 0.0078(7) Cl2 0.0321(9) 0.0281(8) 0.0213(8) 0.0122(6) 0.0078(7) 0.0089(7) N1 0.032(3) 0.008(2) 0.024(3) 0.004(2) 0.003(2) 0.008(2) C1 0.020(3) 0.022(3) 0.025(3) 0.002(3) 0.001(3) -0.008(3) C2 0.044(4) 0.017(3) 0.020(3) 0.009(3) 0.006(3) -0.002(3) C3 0.038(4) 0.036(4) 0.032(4) 0.006(3) 0.005(3) -0.008(4) C4 0.062(6) 0.055(6) 0.029(4) 0.017(4) 0.017(4) -0.010(5) C5 0.058(5) 0.036(4) 0.017(3) 0.010(3) 0.004(3) 0.002(4) C6 0.043(4) 0.032(4) 0.022(4) 0.008(3) 0.003(3) 0.002(3) N2 0.031(3) 0.019(3) 0.018(3) 0.001(2) 0.004(2) -0.000(2) C7 0.040(5) 0.040(5) 0.029(4) 0.011(3) 0.003(3) -0.002(4) P1 0.0314(9) 0.0181(8) 0.0214(8) 0.0047(7) 0.0054(7) 0.0100(7) C8 0.032(4) 0.025(3) 0.026(3) 0.015(3) 0.009(3) 0.010(3) C9 0.040(4) 0.036(4) 0.032(4) 0.006(3) 0.012(3) 0.011(4) C10 0.042(5) 0.041(5) 0.047(5) 0.016(4) 0.014(4) 0.012(4) C11 0.037(5) 0.059(6) 0.047(5) 0.028(5) 0.017(4) 0.022(4) C12 0.059(6) 0.037(4) 0.033(4) 0.017(3) 0.026(4) 0.027(4) C13 0.043(4) 0.026(4) 0.031(4) 0.011(3) 0.008(3) 0.012(3) C14 0.054(5) 0.020(3) 0.027(4) 0.005(3) 0.000(4) 0.015(3) C15 0.073(7) 0.034(5) 0.052(6) 0.017(4) -0.020(5) 0.014(5) C16 0.114(11) 0.049(6) 0.053(7) 0.006(6) -0.054(8) 0.022(7) C17 0.168(15) 0.027(5) 0.037(6) 0.018(4) -0.018(8) 0.021(7) C18 0.153(13) 0.026(4) 0.031(5) 0.013(4) 0.029(7) 0.026(6) C19 0.086(7) 0.031(4) 0.032(4) 0.018(4) 0.026(5) 0.029(5) C20 0.041(4) 0.018(3) 0.029(4) 0.007(3) 0.014(3) 0.001(3) C21 0.039(4) 0.021(3) 0.038(4) 0.010(3) 0.009(3) 0.013(3) C22 0.051(5) 0.021(4) 0.045(5) 0.009(3) 0.011(4) 0.006(3) C23 0.051(5) 0.027(4) 0.030(4) -0.003(3) 0.010(4) -0.005(4) C24 0.039(4) 0.025(4) 0.026(4) -0.000(3) 0.007(3) -0.000(3) C25 0.039(4) 0.024(3) 0.022(3) 0.006(3) 0.006(3) 0.007(3) P2 0.0190(8) 0.0172(8) 0.0186(8) 0.0018(6) 0.0045(6) 0.0052(6) C26 0.022(3) 0.017(3) 0.024(3) 0.002(3) 0.000(3) -0.001(2) C27 0.022(3) 0.034(4) 0.035(4) 0.015(3) 0.005(3) 0.006(3) C28 0.017(3) 0.031(4) 0.044(4) 0.017(3) 0.000(3) -0.001(3) C29 0.028(4) 0.028(4) 0.043(4) 0.020(3) -0.002(3) -0.011(3) C30 0.037(4) 0.020(3) 0.033(4) 0.012(3) -0.005(3) 0.003(3) C31 0.027(4) 0.026(4) 0.025(3) 0.004(3) 0.005(3) 0.005(3) C32 0.022(3) 0.015(3) 0.021(3) 0.003(2) 0.007(3) 0.004(2) C33 0.018(3) 0.030(4) 0.026(4) 0.002(3) 0.001(3) -0.006(3) C34 0.025(4) 0.041(4) 0.022(3) -0.002(3) 0.001(3) -0.007(3) C35 0.030(4) 0.060(6) 0.022(4) 0.005(4) 0.002(3) -0.002(4) C36 0.039(4) 0.036(4) 0.028(4) 0.009(3) 0.010(3) 0.004(3) C37 0.030(4) 0.024(3) 0.028(4) 0.008(3) 0.013(3) -0.000(3) C38 0.023(3) 0.012(3) 0.028(3) 0.003(3) -0.001(3) -0.002(2) C39 0.027(4) 0.026(4) 0.024(3) 0.005(3) 0.003(3) 0.007(3) C40 0.032(4) 0.032(4) 0.031(4) 0.004(3) -0.001(3) 0.013(3) C41 0.025(4) 0.032(4) 0.038(4) -0.001(3) -0.008(3) 0.004(3) C42 0.020(4) 0.057(6) 0.049(5) 0.001(4) 0.005(4) 0.003(4) C43 0.023(3) 0.040(4) 0.025(4) -0.002(3) 0.008(3) 0.013(3) Re2 0.01806(12) 0.02102(14) 0.01492(12) 0.0026(1) 0.00523(9) 0.0008(1) Cl3 0.0274(9) 0.0315(9) 0.0317(9) -0.0001(7) 0.0109(7) -0.0075(7) Cl4 0.0360(9) 0.040(1) 0.0207(8) 0.0129(7) 0.0097(7) 0.0090(8) N3 0.020(3) 0.025(3) 0.021(3) 0.004(2) 0.006(2) 0.006(2) C44 0.026(3) 0.019(3) 0.022(3) 0.000(3) 0.006(3) 0.001(3) C45 0.022(3) 0.018(3) 0.024(3) 0.004(3) 0.007(3) 0.004(2) C46 0.046(5) 0.025(4) 0.030(4) 0.007(3) 0.009(3) 0.003(3) C47 0.045(5) 0.048(5) 0.018(3) 0.010(3) 0.005(3) 0.010(4) C48 0.031(4) 0.049(5) 0.019(3) 0.004(3) 0.003(3) 0.009(4) C49 0.019(3) 0.031(4) 0.023(3) 0.003(3) 0.007(3) 0.003(3) N4 0.018(3) 0.023(3) 0.020(3) 0.005(2) 0.007(2) 0.004(2) C50 0.043(5) 0.035(4) 0.027(4) 0.009(3) 0.004(3) -0.015(4) P3 0.0180(8) 0.033(1) 0.0213(8) -0.0022(7) 0.0043(7) 0.0041(7) C51 0.018(3) 0.068(6) 0.011(3) -0.004(3) -0.001(3) -0.003(3) C52 0.020(4) 0.079(7) 0.023(4) -0.008(4) 0.007(3) 0.012(4) C53 0.020(4) 0.125(11) 0.026(4) 0.001(6) 0.007(3) -0.004(5) C54 0.030(5) 0.128(12) 0.031(5) 0.005(6) 0.008(4) -0.018(6) C55 0.048(6) 0.089(8) 0.030(5) 0.004(5) 0.013(4) -0.017(5) C56 0.030(4) 0.048(5) 0.025(4) 0.006(3) 0.011(3) -0.008(4) C57 0.025(3) 0.030(4) 0.021(3) -0.003(3) 0.008(3) 0.010(3) C58 0.025(4) 0.052(5) 0.014(3) 0.000(3) 0.005(3) 0.003(3) C59 0.033(4) 0.056(5) 0.030(4) 0.009(4) 0.002(3) 0.005(4) C60 0.056(6) 0.052(5) 0.021(4) 0.002(4) -0.007(4) 0.015(5) C61 0.077(7) 0.038(5) 0.046(5) 0.019(4) 0.023(5) 0.030(5) C62 0.038(4) 0.031(4) 0.041(5) 0.006(3) 0.014(4) 0.017(3) C63 0.024(4) 0.031(4) 0.031(4) -0.006(3) 0.003(3) 0.005(3) C64 0.031(5) 0.050(6) 0.065(7) -0.017(5) -0.013(4) 0.014(4) C65 0.068(7) 0.043(6) 0.065(7) -0.026(5) -0.007(6) 0.028(5) C66 0.053(6) 0.033(5) 0.058(6) -0.024(4) 0.003(5) 0.009(4) C67 0.040(5) 0.047(5) 0.033(4) -0.007(4) -0.002(4) -0.003(4) C68 0.022(3) 0.036(4) 0.029(4) -0.000(3) 0.006(3) -0.002(3) P4 0.0218(8) 0.0210(8) 0.0161(7) 0.0051(6) 0.0066(6) 0.0032(6) C69 0.030(4) 0.023(3) 0.021(3) 0.008(3) 0.003(3) 0.007(3) C70 0.043(5) 0.037(4) 0.052(5) 0.024(4) 0.027(4) 0.009(4) C71 0.076(7) 0.047(5) 0.042(5) 0.024(4) 0.024(5) -0.000(5) C72 0.057(6) 0.035(5) 0.049(5) 0.022(4) 0.007(4) 0.010(4) C73 0.046(5) 0.045(5) 0.083(8) 0.040(5) 0.017(5) 0.024(4) C74 0.034(4) 0.038(5) 0.074(7) 0.028(5) 0.023(4) 0.018(4) C75 0.025(3) 0.020(3) 0.017(3) 0.002(2) 0.006(3) 0.010(3) C76 0.024(3) 0.026(4) 0.033(4) 0.010(3) 0.008(3) 0.010(3) C77 0.023(4) 0.032(4) 0.031(4) -0.003(3) -0.002(3) 0.007(3) C78 0.032(4) 0.055(5) 0.018(3) 0.006(3) 0.003(3) 0.027(4) C79 0.039(4) 0.043(5) 0.027(4) 0.020(3) 0.017(3) 0.023(4) C80 0.029(4) 0.028(4) 0.022(3) 0.008(3) 0.007(3) 0.009(3) C81 0.026(3) 0.017(3) 0.030(4) 0.008(3) 0.008(3) 0.005(3) C82 0.035(4) 0.027(4) 0.028(4) -0.003(3) 0.014(3) 0.007(3) C83 0.041(5) 0.052(5) 0.036(4) 0.008(4) 0.020(4) 0.008(4) C84 0.023(4) 0.064(6) 0.048(5) 0.004(5) 0.012(4) -0.001(4) C85 0.026(4) 0.058(6) 0.036(4) 0.006(4) 0.005(3) 0.002(4) C86 0.017(3) 0.045(4) 0.019(3) 0.009(3) 0.001(3) 0.007(3) Re3 0.02689(16) 0.0477(2) 0.02818(16) 0.00931(14) 0.00765(12) 0.00639(13) O1 0.103(7) 0.075(6) 0.051(4) 0.018(4) 0.015(4) 0.056(5) O2 0.051(4) 0.038(3) 0.036(3) 0.007(3) 0.001(3) 0.015(3) O3 0.051(4) 0.105(7) 0.040(4) -0.017(4) 0.005(3) 0.025(4) O4 0.066(6) 0.178(13) 0.150(12) 0.095(11) 0.038(7) 0.002(7) Re4 0.0519(2) 0.0423(2) 0.0390(2) -0.00128(16) -0.01709(17) 0.01364(17) O5 0.227(17) 0.063(7) 0.141(11) 0.023(7) -0.097(12) 0.035(8) O6 0.051(4) 0.062(5) 0.058(5) -0.010(4) -0.011(4) 0.011(4) O7 0.102(7) 0.090(7) 0.044(4) 0.004(4) -0.003(4) 0.037(6) O8 0.068(7) 0.142(12) 0.163(13) 0.04(1) -0.018(8) -0.030(7) O9 0.160(14) 0.117(11) 0.222(18) 0.066(12) 0.105(13) 0.05(1) C87 0.092(12) 0.081(11) 0.34(4) 0.125(18) 0.081(18) 0.008(9) O10 0.14(1) 0.069(6) 0.097(8) 0.009(6) 0.053(7) 0.022(6) C88 0.123(13) 0.053(7) 0.064(8) 0.002(6) -0.014(8) 0.005(8) _refine_ls_extinction_method None loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Re1 . Cl1 . 2.3744(18) yes Re1 . Cl2 . 2.3485(16) yes Re1 . N1 . 2.065(6) yes Re1 . N2 . 2.121(6) yes Re1 . P1 . 2.4824(17) yes Re1 . P2 . 2.4849(16) yes N1 . C1 . 1.285(9) yes N1 . H1 . 0.99(7) yes C1 . C2 . 1.43(1) yes C1 . C7 . 1.512(11) yes C2 . C3 . 1.389(11) yes C2 . N2 . 1.37(1) yes C3 . C4 . 1.380(13) yes C3 . H31 . 1.000 no C4 . C5 . 1.386(14) yes C4 . H41 . 1.000 no C5 . C6 . 1.396(12) yes C5 . H51 . 1.000 no C6 . N2 . 1.34(1) yes C6 . H61 . 1.000 no C7 . H71 . 1.000 no C7 . H72 . 1.000 no C7 . H73 . 1.000 no P1 . C8 . 1.837(7) yes P1 . C14 . 1.821(8) yes P1 . C20 . 1.812(8) yes C8 . C9 . 1.391(11) yes C8 . C13 . 1.406(11) yes C9 . C10 . 1.382(12) yes C9 . H91 . 1.000 no C10 . C11 . 1.389(14) yes C10 . H101 . 1.00 no C11 . C12 . 1.379(14) yes C11 . H111 . 1.000 no C12 . C13 . 1.393(12) yes C12 . H121 . 1.000 no C13 . H131 . 1.000 no C14 . C15 . 1.381(14) yes C14 . C19 . 1.402(14) yes C15 . C16 . 1.388(15) yes C15 . H151 . 1.000 no C16 . C17 . 1.39(2) yes C16 . H161 . 1.000 no C17 . C18 . 1.37(2) yes C17 . H171 . 1.00 no C18 . C19 . 1.398(13) yes C18 . H181 . 1.000 no C19 . H191 . 1.000 no C20 . C21 . 1.42(1) yes C20 . C25 . 1.397(11) yes C21 . C22 . 1.401(12) yes C21 . H211 . 1.000 no C22 . C23 . 1.359(13) yes C22 . H221 . 1.000 no C23 . C24 . 1.390(12) yes C23 . H231 . 1.000 no C24 . C25 . 1.41(1) yes C24 . H241 . 1.000 no C25 . H251 . 1.000 no P2 . C26 . 1.833(7) yes P2 . C32 . 1.836(7) yes P2 . C38 . 1.823(7) yes C26 . C27 . 1.40(1) yes C26 . C31 . 1.40(1) yes C27 . C28 . 1.378(11) yes C27 . H271 . 1.000 no C28 . C29 . 1.389(11) yes C28 . H281 . 1.000 no C29 . C30 . 1.397(12) yes C29 . H291 . 1.000 no C30 . C31 . 1.393(11) yes C30 . H301 . 1.000 no C31 . H311 . 1.000 no C32 . C33 . 1.390(9) yes C32 . C37 . 1.40(1) yes C33 . C34 . 1.40(1) yes C33 . H331 . 1.000 no C34 . C35 . 1.387(12) yes C34 . H341 . 1.000 no C35 . C36 . 1.386(12) yes C35 . H351 . 1.000 no C36 . C37 . 1.391(11) yes C36 . H361 . 1.000 no C37 . H371 . 1.000 no C38 . C39 . 1.40(1) yes C38 . C43 . 1.39(1) yes C39 . C40 . 1.39(1) yes C39 . H391 . 1.000 no C40 . C41 . 1.372(12) yes C40 . H401 . 1.000 no C41 . C42 . 1.381(13) yes C41 . H411 . 1.000 no C42 . C43 . 1.401(11) yes C42 . H421 . 1.000 no C43 . H431 . 1.000 no Re2 . Cl3 . 2.3611(17) yes Re2 . Cl4 . 2.3542(17) yes Re2 . N3 . 2.038(6) yes Re2 . N4 . 2.110(6) yes Re2 . P3 . 2.4788(18) yes Re2 . P4 . 2.4740(17) yes N3 . C44 . 1.287(9) yes N3 . H2 . 0.92(7) yes C44 . C45 . 1.44(1) yes C44 . C50 . 1.51(1) yes C45 . C46 . 1.379(11) yes C45 . N4 . 1.382(9) yes C46 . C47 . 1.374(12) yes C46 . H461 . 1.000 no C47 . C48 . 1.387(13) yes C47 . H471 . 1.000 no C48 . C49 . 1.360(11) yes C48 . H481 . 1.000 no C49 . N4 . 1.351(9) yes C49 . H491 . 1.000 no C50 . H501 . 1.000 no C50 . H502 . 1.00 no C50 . H503 . 1.000 no P3 . C51 . 1.848(9) yes P3 . C57 . 1.815(8) yes P3 . C63 . 1.833(8) yes C51 . C52 . 1.424(11) yes C51 . C56 . 1.357(14) yes C52 . C53 . 1.408(15) yes C52 . H521 . 1.000 no C53 . C54 . 1.35(2) yes C53 . H531 . 1.000 no C54 . C55 . 1.379(18) yes C54 . H541 . 1.000 no C55 . C56 . 1.399(12) yes C55 . H551 . 1.000 no C56 . H561 . 1.000 no C57 . C58 . 1.387(11) yes C57 . C62 . 1.391(12) yes C58 . C59 . 1.400(12) yes C58 . H581 . 1.000 no C59 . C60 . 1.367(15) yes C59 . H591 . 1.000 no C60 . C61 . 1.416(15) yes C60 . H601 . 1.000 no C61 . C62 . 1.409(13) yes C61 . H611 . 1.00 no C62 . H621 . 1.000 no C63 . C64 . 1.385(12) yes C63 . C68 . 1.381(11) yes C64 . C65 . 1.407(13) yes C64 . H641 . 1.000 no C65 . C66 . 1.375(15) yes C65 . H651 . 1.00 no C66 . C67 . 1.376(14) yes C66 . H661 . 1.000 no C67 . C68 . 1.399(11) yes C67 . H671 . 1.000 no C68 . H681 . 1.000 no P4 . C69 . 1.820(7) yes P4 . C75 . 1.832(7) yes P4 . C81 . 1.829(7) yes C69 . C70 . 1.375(11) yes C69 . C74 . 1.415(11) yes C70 . C71 . 1.405(13) yes C70 . H701 . 1.000 no C71 . C72 . 1.362(15) yes C71 . H711 . 1.000 no C72 . C73 . 1.416(15) yes C72 . H721 . 1.000 no C73 . C74 . 1.389(12) yes C73 . H731 . 1.00 no C74 . H741 . 1.000 no C75 . C76 . 1.39(1) yes C75 . C80 . 1.39(1) yes C76 . C77 . 1.391(11) yes C76 . H761 . 1.000 no C77 . C78 . 1.379(13) yes C77 . H771 . 1.000 no C78 . C79 . 1.362(13) yes C78 . H781 . 1.000 no C79 . C80 . 1.409(11) yes C79 . H791 . 1.000 no C80 . H801 . 1.000 no C81 . C82 . 1.40(1) yes C81 . C86 . 1.38(1) yes C82 . C83 . 1.386(12) yes C82 . H821 . 1.000 no C83 . C84 . 1.361(13) yes C83 . H831 . 1.000 no C84 . C85 . 1.382(12) yes C84 . H841 . 1.000 no C85 . C86 . 1.391(11) yes C85 . H851 . 1.000 no C86 . H861 . 1.000 no Re3 . O1 . 1.724(8) yes Re3 . O2 . 1.726(6) yes Re3 . O3 . 1.694(7) yes Re3 . O4 . 1.67(1) yes Re4 . O5 . 1.65(1) yes Re4 . O6 . 1.685(7) yes Re4 . O7 . 1.671(9) yes Re4 . O8 . 1.695(13) yes O9 . C87 . 1.39(3) yes O9 . H3 . 1.00 no C87 . H871 . 1.00 no C87 . H872 . 1.000 no C87 . H873 . 1.00 no O10 . C88 . 1.349(18) yes O10 . H4 . 1.000 no C88 . H881 . 1.000 no C88 . H882 . 1.000 no C88 . H883 . 1.000 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Cl1 . Re1 . Cl2 . 101.67(7) yes Cl1 . Re1 . N1 . 167.25(17) yes Cl2 . Re1 . N1 . 90.25(17) yes Cl1 . Re1 . N2 . 93.93(17) yes Cl2 . Re1 . N2 . 164.41(17) yes N1 . Re1 . N2 . 74.2(2) yes Cl1 . Re1 . P1 . 89.45(6) yes Cl2 . Re1 . P1 . 86.91(6) yes N1 . Re1 . P1 . 95.79(15) yes N2 . Re1 . P1 . 93.07(16) yes Cl1 . Re1 . P2 . 86.08(6) yes Cl2 . Re1 . P2 . 91.41(6) yes N1 . Re1 . P2 . 89.12(15) yes N2 . Re1 . P2 . 89.86(16) yes P1 . Re1 . P2 . 174.82(6) yes Re1 . N1 . C1 . 120.9(5) yes Re1 . N1 . H1 . 126.4(57) yes C1 . N1 . H1 . 110.8(58) yes N1 . C1 . C2 . 114.9(6) yes N1 . C1 . C7 . 123.5(7) yes C2 . C1 . C7 . 121.6(7) yes C1 . C2 . C3 . 125.1(7) yes C1 . C2 . N2 . 113.9(6) yes C3 . C2 . N2 . 121.0(7) yes C2 . C3 . C4 . 120.5(8) yes C2 . C3 . H31 . 119.7 no C4 . C3 . H31 . 119.7 no C3 . C4 . C5 . 117.7(8) yes C3 . C4 . H41 . 121.1 no C5 . C4 . H41 . 121.1 no C4 . C5 . C6 . 120.7(7) yes C4 . C5 . H51 . 119.7 no C6 . C5 . H51 . 119.7 no C5 . C6 . N2 . 121.0(8) yes C5 . C6 . H61 . 119.5 no N2 . C6 . H61 . 119.5 no Re1 . N2 . C2 . 115.8(5) yes Re1 . N2 . C6 . 125.1(5) yes C2 . N2 . C6 . 119.1(6) yes C1 . C7 . H71 . 109.5 no C1 . C7 . H72 . 109.5 no H71 . C7 . H72 . 109.5 no C1 . C7 . H73 . 109.5 no H71 . C7 . H73 . 109.5 no H72 . C7 . H73 . 109.5 no Re1 . P1 . C8 . 115.4(2) yes Re1 . P1 . C14 . 111.4(3) yes C8 . P1 . C14 . 105.6(4) yes Re1 . P1 . C20 . 116.3(3) yes C8 . P1 . C20 . 101.7(3) yes C14 . P1 . C20 . 105.2(4) yes P1 . C8 . C9 . 120.5(6) yes P1 . C8 . C13 . 120.8(6) yes C9 . C8 . C13 . 118.7(7) yes C8 . C9 . C10 . 121.6(8) yes C8 . C9 . H91 . 119.2 no C10 . C9 . H91 . 119.2 no C9 . C10 . C11 . 119.8(9) yes C9 . C10 . H101 . 120.1 no C11 . C10 . H101 . 120.1 no C10 . C11 . C12 . 119.0(8) yes C10 . C11 . H111 . 120.5 no C12 . C11 . H111 . 120.5 no C11 . C12 . C13 . 122.1(8) yes C11 . C12 . H121 . 119.0 no C13 . C12 . H121 . 119.0 no C8 . C13 . C12 . 118.7(8) yes C8 . C13 . H131 . 120.7 no C12 . C13 . H131 . 120.7 no P1 . C14 . C15 . 122.6(8) yes P1 . C14 . C19 . 117.6(7) yes C15 . C14 . C19 . 119.5(9) yes C14 . C15 . C16 . 120.0(13) yes C14 . C15 . H151 . 120.0 no C16 . C15 . H151 . 120.0 no C15 . C16 . C17 . 120.9(13) yes C15 . C16 . H161 . 119.6 no C17 . C16 . H161 . 119.6 no C16 . C17 . C18 . 118.8(9) yes C16 . C17 . H171 . 120.6 no C18 . C17 . H171 . 120.6 no C17 . C18 . C19 . 121.3(12) yes C17 . C18 . H181 . 119.3 no C19 . C18 . H181 . 119.3 no C14 . C19 . C18 . 119.4(11) yes C14 . C19 . H191 . 120.3 no C18 . C19 . H191 . 120.3 no P1 . C20 . C21 . 121.0(6) yes P1 . C20 . C25 . 119.1(5) yes C21 . C20 . C25 . 119.7(7) yes C20 . C21 . C22 . 119.2(7) yes C20 . C21 . H211 . 120.4 no C22 . C21 . H211 . 120.4 no C21 . C22 . C23 . 120.6(7) yes C21 . C22 . H221 . 119.7 no C23 . C22 . H221 . 119.7 no C22 . C23 . C24 . 121.3(7) yes C22 . C23 . H231 . 119.3 no C24 . C23 . H231 . 119.3 no C23 . C24 . C25 . 119.5(8) yes C23 . C24 . H241 . 120.3 no C25 . C24 . H241 . 120.3 no C20 . C25 . C24 . 119.7(7) yes C20 . C25 . H251 . 120.2 no C24 . C25 . H251 . 120.2 no Re1 . P2 . C26 . 117.4(2) yes Re1 . P2 . C32 . 113.2(2) yes C26 . P2 . C32 . 105.2(3) yes Re1 . P2 . C38 . 111.0(2) yes C26 . P2 . C38 . 101.6(3) yes C32 . P2 . C38 . 107.4(3) yes P2 . C26 . C27 . 121.2(5) yes P2 . C26 . C31 . 119.6(5) yes C27 . C26 . C31 . 119.1(7) yes C26 . C27 . C28 . 119.9(7) yes C26 . C27 . H271 . 120.0 no C28 . C27 . H271 . 120.0 no C27 . C28 . C29 . 121.0(7) yes C27 . C28 . H281 . 119.5 no C29 . C28 . H281 . 119.5 no C28 . C29 . C30 . 119.7(7) yes C28 . C29 . H291 . 120.1 no C30 . C29 . H291 . 120.1 no C29 . C30 . C31 . 119.5(7) yes C29 . C30 . H301 . 120.2 no C31 . C30 . H301 . 120.2 no C26 . C31 . C30 . 120.6(7) yes C26 . C31 . H311 . 119.7 no C30 . C31 . H311 . 119.7 no P2 . C32 . C33 . 119.6(5) yes P2 . C32 . C37 . 120.6(5) yes C33 . C32 . C37 . 119.7(6) yes C32 . C33 . C34 . 120.5(7) yes C32 . C33 . H331 . 119.8 no C34 . C33 . H331 . 119.8 no C33 . C34 . C35 . 119.0(7) yes C33 . C34 . H341 . 120.5 no C35 . C34 . H341 . 120.5 no C34 . C35 . C36 . 121.1(7) yes C34 . C35 . H351 . 119.5 no C36 . C35 . H351 . 119.5 no C35 . C36 . C37 . 119.8(7) yes C35 . C36 . H361 . 120.1 no C37 . C36 . H361 . 120.1 no C32 . C37 . C36 . 119.9(7) yes C32 . C37 . H371 . 120.0 no C36 . C37 . H371 . 120.0 no P2 . C38 . C39 . 115.9(5) yes P2 . C38 . C43 . 125.2(6) yes C39 . C38 . C43 . 118.9(7) yes C38 . C39 . C40 . 119.8(7) yes C38 . C39 . H391 . 120.1 no C40 . C39 . H391 . 120.1 no C39 . C40 . C41 . 121.0(7) yes C39 . C40 . H401 . 119.5 no C41 . C40 . H401 . 119.5 no C40 . C41 . C42 . 120.2(7) yes C40 . C41 . H411 . 119.9 no C42 . C41 . H411 . 119.9 no C41 . C42 . C43 . 119.6(8) yes C41 . C42 . H421 . 120.2 no C43 . C42 . H421 . 120.2 no C38 . C43 . C42 . 120.4(7) yes C38 . C43 . H431 . 119.8 no C42 . C43 . H431 . 119.8 no Cl3 . Re2 . Cl4 . 101.90(7) yes Cl3 . Re2 . N3 . 168.14(18) yes Cl4 . Re2 . N3 . 89.95(18) yes Cl3 . Re2 . N4 . 93.85(16) yes Cl4 . Re2 . N4 . 164.21(16) yes N3 . Re2 . N4 . 74.3(2) yes Cl3 . Re2 . P3 . 86.87(6) yes Cl4 . Re2 . P3 . 92.23(6) yes N3 . Re2 . P3 . 93.17(16) yes N4 . Re2 . P3 . 89.84(15) yes Cl3 . Re2 . P4 . 86.34(6) yes Cl4 . Re2 . P4 . 90.48(6) yes N3 . Re2 . P4 . 93.20(16) yes N4 . Re2 . P4 . 89.29(15) yes P3 . Re2 . P4 . 173.08(6) yes Re2 . N3 . C44 . 122.0(5) yes Re2 . N3 . H2 . 121.8(61) yes C44 . N3 . H2 . 114.6(61) yes N3 . C44 . C45 . 114.5(6) yes N3 . C44 . C50 . 122.9(7) yes C45 . C44 . C50 . 122.5(7) yes C44 . C45 . C46 . 125.9(7) yes C44 . C45 . N4 . 112.4(6) yes C46 . C45 . N4 . 121.7(6) yes C45 . C46 . C47 . 118.9(7) yes C45 . C46 . H461 . 120.5 no C47 . C46 . H461 . 120.5 no C46 . C47 . C48 . 119.2(7) yes C46 . C47 . H471 . 120.4 no C48 . C47 . H471 . 120.4 no C47 . C48 . C49 . 120.3(7) yes C47 . C48 . H481 . 119.8 no C49 . C48 . H481 . 119.8 no C48 . C49 . N4 . 121.7(7) yes C48 . C49 . H491 . 119.1 no N4 . C49 . H491 . 119.1 no Re2 . N4 . C45 . 116.7(4) yes Re2 . N4 . C49 . 125.2(5) yes C45 . N4 . C49 . 118.1(6) yes C44 . C50 . H501 . 109.5 no C44 . C50 . H502 . 109.5 no H501 . C50 . H502 . 109.5 no C44 . C50 . H503 . 109.5 no H501 . C50 . H503 . 109.5 no H502 . C50 . H503 . 109.5 no Re2 . P3 . C51 . 117.2(3) yes Re2 . P3 . C57 . 108.1(2) yes C51 . P3 . C57 . 105.2(3) yes Re2 . P3 . C63 . 117.0(2) yes C51 . P3 . C63 . 102.2(4) yes C57 . P3 . C63 . 106.0(4) yes P3 . C51 . C52 . 117.8(8) yes P3 . C51 . C56 . 122.1(6) yes C52 . C51 . C56 . 120.0(8) yes C51 . C52 . C53 . 118.0(11) yes C51 . C52 . H521 . 121.0 no C53 . C52 . H521 . 121.0 no C52 . C53 . C54 . 120.8(10) yes C52 . C53 . H531 . 119.6 no C54 . C53 . H531 . 119.6 no C53 . C54 . C55 . 121.1(10) yes C53 . C54 . H541 . 119.5 no C55 . C54 . H541 . 119.5 no C54 . C55 . C56 . 119.5(12) yes C54 . C55 . H551 . 120.2 no C56 . C55 . H551 . 120.2 no C51 . C56 . C55 . 120.5(9) yes C51 . C56 . H561 . 119.7 no C55 . C56 . H561 . 119.7 no P3 . C57 . C58 . 120.2(6) yes P3 . C57 . C62 . 120.3(6) yes C58 . C57 . C62 . 119.1(7) yes C57 . C58 . C59 . 121.3(8) yes C57 . C58 . H581 . 119.3 no C59 . C58 . H581 . 119.3 no C58 . C59 . C60 . 120.3(8) yes C58 . C59 . H591 . 119.9 no C60 . C59 . H591 . 119.9 no C59 . C60 . C61 . 119.3(8) yes C59 . C60 . H601 . 120.4 no C61 . C60 . H601 . 120.4 no C60 . C61 . C62 . 120.2(9) yes C60 . C61 . H611 . 119.9 no C62 . C61 . H611 . 119.9 no C57 . C62 . C61 . 119.8(8) yes C57 . C62 . H621 . 120.1 no C61 . C62 . H621 . 120.1 no P3 . C63 . C64 . 121.2(6) yes P3 . C63 . C68 . 118.3(6) yes C64 . C63 . C68 . 120.4(7) yes C63 . C64 . C65 . 119.6(9) yes C63 . C64 . H641 . 120.2 no C65 . C64 . H641 . 120.2 no C64 . C65 . C66 . 120.5(9) yes C64 . C65 . H651 . 119.7 no C66 . C65 . H651 . 119.7 no C65 . C66 . C67 . 118.9(8) yes C65 . C66 . H661 . 120.5 no C67 . C66 . H661 . 120.5 no C66 . C67 . C68 . 121.8(8) yes C66 . C67 . H671 . 119.1 no C68 . C67 . H671 . 119.1 no C63 . C68 . C67 . 118.8(8) yes C63 . C68 . H681 . 120.6 no C67 . C68 . H681 . 120.6 no Re2 . P4 . C69 . 118.5(2) yes Re2 . P4 . C75 . 109.7(2) yes C69 . P4 . C75 . 104.2(3) yes Re2 . P4 . C81 . 114.8(2) yes C69 . P4 . C81 . 101.9(3) yes C75 . P4 . C81 . 106.7(3) yes P4 . C69 . C70 . 123.7(6) yes P4 . C69 . C74 . 118.5(6) yes C70 . C69 . C74 . 117.8(7) yes C69 . C70 . C71 . 120.9(8) yes C69 . C70 . H701 . 119.6 no C71 . C70 . H701 . 119.6 no C70 . C71 . C72 . 121.2(9) yes C70 . C71 . H711 . 119.4 no C72 . C71 . H711 . 119.4 no C71 . C72 . C73 . 119.6(8) yes C71 . C72 . H721 . 120.2 no C73 . C72 . H721 . 120.2 no C72 . C73 . C74 . 118.6(9) yes C72 . C73 . H731 . 120.7 no C74 . C73 . H731 . 120.7 no C69 . C74 . C73 . 121.9(8) yes C69 . C74 . H741 . 119.1 no C73 . C74 . H741 . 119.1 no P4 . C75 . C76 . 120.1(5) yes P4 . C75 . C80 . 119.3(5) yes C76 . C75 . C80 . 120.1(6) yes C75 . C76 . C77 . 119.6(7) yes C75 . C76 . H761 . 120.2 no C77 . C76 . H761 . 120.2 no C76 . C77 . C78 . 119.9(7) yes C76 . C77 . H771 . 120.1 no C78 . C77 . H771 . 120.1 no C77 . C78 . C79 . 121.2(7) yes C77 . C78 . H781 . 119.4 no C79 . C78 . H781 . 119.4 no C78 . C79 . C80 . 119.7(7) yes C78 . C79 . H791 . 120.2 no C80 . C79 . H791 . 120.2 no C75 . C80 . C79 . 119.4(7) yes C75 . C80 . H801 . 120.3 no C79 . C80 . H801 . 120.3 no P4 . C81 . C82 . 123.9(6) yes P4 . C81 . C86 . 116.2(5) yes C82 . C81 . C86 . 119.8(7) yes C81 . C82 . C83 . 119.2(7) yes C81 . C82 . H821 . 120.4 no C83 . C82 . H821 . 120.4 no C82 . C83 . C84 . 120.8(8) yes C82 . C83 . H831 . 119.6 no C84 . C83 . H831 . 119.6 no C83 . C84 . C85 . 120.4(8) yes C83 . C84 . H841 . 119.8 no C85 . C84 . H841 . 119.8 no C84 . C85 . C86 . 119.8(8) yes C84 . C85 . H851 . 120.1 no C86 . C85 . H851 . 120.1 no C81 . C86 . C85 . 119.9(7) yes C81 . C86 . H861 . 120.1 no C85 . C86 . H861 . 120.1 no O1 . Re3 . O2 . 108.5(4) yes O1 . Re3 . O3 . 107.3(5) yes O2 . Re3 . O3 . 109.9(3) yes O1 . Re3 . O4 . 106.7(6) yes O2 . Re3 . O4 . 111.7(5) yes O3 . Re3 . O4 . 112.5(6) yes O5 . Re4 . O6 . 112.0(5) yes O5 . Re4 . O7 . 114.4(8) yes O6 . Re4 . O7 . 108.7(4) yes O5 . Re4 . O8 . 106.6(9) yes O6 . Re4 . O8 . 110.8(6) yes O7 . Re4 . O8 . 104.1(7) yes C87 . O9 . H3 . 116.8 no O9 . C87 . H871 . 109.5 no O9 . C87 . H872 . 109.5 no H871 . C87 . H872 . 109.5 no O9 . C87 . H873 . 109.5 no H871 . C87 . H873 . 109.5 no H872 . C87 . H873 . 109.5 no C88 . O10 . H4 . 109.1 no O10 . C88 . H881 . 109.5 no O10 . C88 . H882 . 109.5 no H881 . C88 . H882 . 109.5 no O10 . C88 . H883 . 109.5 no H881 . C88 . H883 . 109.5 no H882 . C88 . H883 . 109.5 no data_CRYSTALS_2 _database_code_CSD 196179 #========================================================================== # Diffractometer details #========================================================================== _diffrn_measurement_device_type ; Nonius KappaCCD ; _diffrn_radiation_monochromator graphite _computing_data_collection ; KappaCCD software 'Collect' (Nonius, 2000) ; _computing_data_reduction ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; #========================================================================== # General computing #========================================================================== _computing_structure_refinement ; CRYSTALS (Watkin et al, 2001) ; _computing_publication_material ; CRYSTALS (Watkin et al, 2001) ; _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point 'not measured' _refine_ls_matrix_type full _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref #************************************************************************** _cell_length_a 12.8385(5) _cell_angle_alpha 90 _cell_length_b 8.5154(3) _cell_angle_beta 96.2545(17) _cell_length_c 22.3598(8) _cell_angle_gamma 90 _cell_volume 2429.9 _symmetry_cell_setting 'Monoclinic ' _symmetry_space_group_name_H-M 'P 1 21/c 1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y+1/2,-z+1/2 x,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 International_Tables_Vol_IV_Table_2.2B 'Cl ' 0.1320 0.1590 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 International_Tables_Vol_IV_Table_2.2B 'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 International_Tables_Vol_IV_Table_2.2B 'O ' 0.0080 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 International_Tables_Vol_IV_Table_2.2B 'Re ' -1.5980 7.2320 28.7621 1.6719 15.7189 9.0923 14.5564 0.3505 5.4417 52.0861 10.4720 International_Tables_Vol_IV_Table_2.2B 'S ' 0.1100 0.1240 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 International_Tables_Vol_IV_Table_2.2B _chemical_formula_sum ' C19 H26 Cl1 N8 O1 Re1 S2 ' _chemical_formula_moiety ' C19 H26 Cl1 N8 O1 Re1 S2 ' _chemical_compound_source ; synthesis as described ; _chemical_formula_weight 668.24 _cell_measurement_reflns_used 22649 _cell_measurement_theta_min 5 _cell_measurement_theta_max 28 _cell_measurement_temperature 150 _cell_formula_units_Z 4 _exptl_crystal_description ' fragment ' _exptl_crystal_colour ' dark brown ' _exptl_crystal_size_min 0.03 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_max 0.10 _exptl_crystal_density_diffrn 1.827 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 1307.255 _exptl_absorpt_coefficient_mu 5.311 _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _exptl_absorpt_correction_T_min 0.59 _exptl_absorpt_correction_T_max 0.85 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 150 _diffrn_reflns_number 22649 _reflns_number_total 5728 _diffrn_reflns_av_R_equivalents 0.060 _diffrn_measured_fraction_theta_max 0.976 _reflns_number_gt 3696 _diffrn_reflns_theta_min 5.12 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _reflns_limit_h_min -16 _reflns_limit_h_max 16 _reflns_limit_k_min 0 _reflns_limit_k_max 11 _reflns_limit_l_min 0 _reflns_limit_l_max 28 _refine_diff_density_min -1.94 _refine_diff_density_max 1.68 _reflns_threshold_expression >3.00\s(I) _refine_ls_number_reflns 3696 _refine_ls_number_parameters 289 _refine_ls_R_factor_gt 0.0478 _refine_ls_wR_factor_ref 0.0461 _refine_ls_goodness_of_fit_ref 1.0055 _refine_ls_shift/su_max 0.010940 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 4 parameters (Carruthers & Watkin , 1979) 4.01 0.529 3.35 0.763 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type Re1 0.241699(16) 0.25708(3) 0.465456(9) 0.0132 1.0000 Uani N1 0.1888(5) 0.1314(7) 0.5365(2) 0.0180 1.0000 Uani C1 0.2524(6) 0.0500(8) 0.5779(4) 0.0206 1.0000 Uani C2 0.2158(6) -0.0218(8) 0.6270(3) 0.0208 1.0000 Uani C3 0.1102(6) -0.0090(8) 0.6339(3) 0.0225 1.0000 Uani C4 0.0435(6) 0.0744(8) 0.5927(3) 0.0191 1.0000 Uani C5 0.0848(5) 0.1465(8) 0.5437(3) 0.0166 1.0000 Uani C6 0.0255(4) 0.2393(7) 0.4991(3) 0.0154 1.0000 Uani C7 -0.0898(5) 0.2638(8) 0.4953(3) 0.0206 1.0000 Uani N2 0.0840(4) 0.3043(6) 0.4611(2) 0.0130 1.0000 Uani N3 0.0309(4) 0.3962(6) 0.4147(3) 0.0175 1.0000 Uani C8 0.0982(5) 0.4757(7) 0.3858(3) 0.0163 1.0000 Uani S1 0.23566(15) 0.4766(2) 0.40696(9) 0.0184 1.0000 Uani N4 0.0647(5) 0.5653(7) 0.3390(3) 0.0221 1.0000 Uani C9 -0.0452(6) 0.5719(9) 0.3135(4) 0.0283 1.0000 Uani N5 0.3200(4) 0.3766(6) 0.5387(2) 0.0137 1.0000 Uani C10 0.2706(6) 0.4568(8) 0.5812(3) 0.0172 1.0000 Uani C11 0.3252(6) 0.5216(8) 0.6310(3) 0.0201 1.0000 Uani C12 0.4342(6) 0.5103(9) 0.6392(3) 0.0220 1.0000 Uani C13 0.4860(6) 0.4308(7) 0.5973(3) 0.0201 1.0000 Uani C14 0.4266(5) 0.3626(8) 0.5462(3) 0.0171 1.0000 Uani C15 0.4707(4) 0.2687(7) 0.5021(3) 0.0148 1.0000 Uani C16 0.5848(5) 0.2428(9) 0.4997(3) 0.0235 1.0000 Uani N6 0.3996(4) 0.2070(6) 0.4631(2) 0.0124 1.0000 Uani N7 0.4360(4) 0.1132(6) 0.4189(2) 0.0126 1.0000 Uani C17 0.3584(5) 0.0349(8) 0.3876(3) 0.0181 1.0000 Uani S2 0.22617(15) 0.03815(19) 0.40561(9) 0.0187 1.0000 Uani N8 0.3767(5) -0.0585(7) 0.3429(3) 0.0206 1.0000 Uani C18 0.4790(6) -0.0659(9) 0.3193(3) 0.0257 1.0000 Uani Cl1 0.21422(14) 0.7447(2) 0.25836(7) 0.0290 1.0000 Uani O1 0.3523(5) 0.4351(9) 0.2685(3) 0.0478 1.0000 Uani C19 0.2850(9) 0.3024(11) 0.2610(4) 0.0460 1.0000 Uani H1 0.1119 0.6219 0.3136 0.0265 1.0000 Uiso H2 0.3250 -0.1211 0.3160 0.0248 1.0000 Uiso H3 0.3087 0.5327 0.2653 0.0576 1.0000 Uiso H11 0.3286 0.0416 0.5727 0.0243 1.0000 Uiso H21 0.2644 -0.0815 0.6567 0.0247 1.0000 Uiso H31 0.0819 -0.0604 0.6689 0.0277 1.0000 Uiso H41 -0.0328 0.0833 0.5976 0.0229 1.0000 Uiso H71 -0.1127 0.3332 0.4602 0.0249 1.0000 Uiso H72 -0.1079 0.3146 0.5331 0.0249 1.0000 Uiso H73 -0.1263 0.1602 0.4899 0.0249 1.0000 Uiso H91 -0.0526 0.6464 0.2787 0.0331 1.0000 Uiso H92 -0.0893 0.6088 0.3449 0.0331 1.0000 Uiso H93 -0.0687 0.4649 0.2994 0.0331 1.0000 Uiso H101 0.1926 0.4678 0.5754 0.0206 1.0000 Uiso H111 0.2870 0.5771 0.6615 0.0241 1.0000 Uiso H121 0.4746 0.5593 0.6752 0.0263 1.0000 Uiso H131 0.5641 0.4214 0.6028 0.0238 1.0000 Uiso H161 0.5953 0.1732 0.4648 0.0282 1.0000 Uiso H162 0.6155 0.1917 0.5379 0.0282 1.0000 Uiso H163 0.6201 0.3459 0.4948 0.0282 1.0000 Uiso H181 0.4758 -0.1437 0.2857 0.0313 1.0000 Uiso H182 0.5337 -0.0991 0.3522 0.0313 1.0000 Uiso H183 0.4972 0.0399 0.3041 0.0313 1.0000 Uiso H191 0.3279 0.2042 0.2641 0.0548 1.0000 Uiso H192 0.2364 0.3026 0.2930 0.0548 1.0000 Uiso H193 0.2433 0.3071 0.2205 0.0548 1.0000 Uiso 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 0.00917(13) 0.01671(13) 0.01384(13) -0.00060(14) 0.00182(7) -0.00327(13) N1 0.024(3) 0.017(2) 0.013(2) 0.0004(19) 0.002(2) -0.009(2) C1 0.022(3) 0.023(3) 0.016(3) 0.002(3) -0.003(3) -0.001(3) C2 0.025(3) 0.019(3) 0.017(3) -0.000(2) -0.000(2) 0.001(2) C3 0.026(3) 0.022(3) 0.021(3) 0.005(2) 0.011(3) -0.008(3) C4 0.019(3) 0.019(3) 0.019(3) 0.000(2) 0.002(2) -0.002(2) C5 0.012(3) 0.019(3) 0.018(3) -0.002(2) -0.002(2) -0.001(2) C6 0.013(2) 0.011(2) 0.022(2) 0.000(3) 0.0032(19) -0.005(2) C7 0.011(2) 0.021(3) 0.031(3) 0.004(3) 0.005(2) 0.003(3) N2 0.0081(9) 0.0167(9) 0.0144(9) -0.0010(9) 0.0015(9) -0.0009(9) N3 0.012(2) 0.020(2) 0.020(2) -0.004(2) -0.000(2) 0.0012(19) C8 0.012(3) 0.016(3) 0.022(3) 0.001(2) 0.002(2) 0.001(2) S1 0.0121(9) 0.0237(8) 0.019(1) 0.0045(7) 0.0009(7) -0.0053(6) N4 0.019(3) 0.026(3) 0.021(3) 0.003(2) 0.002(2) -0.002(2) C9 0.018(3) 0.034(4) 0.031(4) 0.003(3) -0.007(3) 0.003(3) N5 0.016(2) 0.014(2) 0.011(2) 0.0012(18) 0.0018(19) -0.0040(19) C10 0.012(3) 0.025(3) 0.015(3) 0.003(2) 0.000(3) 0.003(2) C11 0.019(3) 0.025(3) 0.017(3) 0.001(2) 0.002(2) -0.000(2) C12 0.023(3) 0.027(3) 0.016(3) -0.007(3) 0.001(2) -0.002(3) C13 0.025(3) 0.014(3) 0.021(3) 0.004(2) -0.001(3) -0.006(2) C14 0.016(3) 0.021(3) 0.014(3) 0.003(2) -0.002(2) -0.003(2) C15 0.009(2) 0.013(3) 0.021(2) -0.003(2) 0.001(2) 0.001(2) C16 0.009(2) 0.031(3) 0.031(3) -0.007(4) 0.002(2) -0.003(3) N6 0.0091(9) 0.0142(9) 0.0141(9) -0.0005(9) 0.0016(9) -0.0019(8) N7 0.004(2) 0.017(2) 0.017(2) -0.0015(18) -0.0004(17) -0.0007(18) C17 0.014(3) 0.025(3) 0.014(3) -0.000(2) -0.006(2) -0.003(2) S2 0.0144(9) 0.0179(7) 0.0243(11) -0.0057(7) 0.0041(8) -0.0062(6) N8 0.015(3) 0.027(3) 0.020(3) -0.004(2) 0.003(2) -0.004(2) C18 0.024(4) 0.030(3) 0.025(3) -0.010(3) 0.007(3) 0.001(3) Cl1 0.0373(9) 0.0293(8) 0.0201(6) -0.0016(9) 0.0022(6) -0.0128(9) O1 0.031(3) 0.070(5) 0.043(4) -0.002(3) 0.006(3) 0.008(3) C19 0.062(7) 0.039(4) 0.036(5) 0.006(4) 0.001(5) 0.007(4) _refine_ls_extinction_method None loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Re1 . N1 . 2.089(6) yes Re1 . N2 . 2.056(5) yes Re1 . S1 . 2.2778(18) yes Re1 . N5 . 2.090(5) yes Re1 . N6 . 2.078(5) yes Re1 . S2 . 2.2908(17) yes N1 . C1 . 1.36(1) yes N1 . C5 . 1.368(9) yes C1 . C2 . 1.38(1) yes C1 . H11 . 1.000 no C2 . C3 . 1.39(1) yes C2 . H21 . 1.000 no C3 . C4 . 1.38(1) yes C3 . H31 . 1.000 no C4 . C5 . 1.41(1) yes C4 . H41 . 1.000 no C5 . C6 . 1.427(9) yes C6 . C7 . 1.488(8) yes C6 . N2 . 1.315(8) yes C7 . H71 . 1.000 no C7 . H72 . 1.000 no C7 . H73 . 1.000 no N2 . N3 . 1.414(8) yes N3 . C8 . 1.320(9) yes C8 . S1 . 1.777(7) yes C8 . N4 . 1.328(9) yes N4 . C9 . 1.464(9) yes N4 . H1 . 1.000 no C9 . H91 . 1.000 no C9 . H92 . 1.000 no C9 . H93 . 1.000 no N5 . C10 . 1.379(9) yes N5 . C14 . 1.366(9) yes C10 . C11 . 1.37(1) yes C10 . H101 . 1.000 no C11 . C12 . 1.39(1) yes C11 . H111 . 1.000 no C12 . C13 . 1.38(1) yes C12 . H121 . 1.000 no C13 . C14 . 1.427(9) yes C13 . H131 . 1.000 no C14 . C15 . 1.434(9) yes C15 . C16 . 1.488(8) yes C15 . N6 . 1.303(8) yes C16 . H161 . 1.000 no C16 . H162 . 1.000 no C16 . H163 . 1.000 no N6 . N7 . 1.390(7) yes N7 . C17 . 1.332(8) yes C17 . S2 . 1.786(7) yes C17 . N8 . 1.320(9) yes N8 . C18 . 1.469(9) yes N8 . H2 . 1.000 no C18 . H181 . 1.000 no C18 . H182 . 1.000 no C18 . H183 . 1.000 no O1 . C19 . 1.421(13) yes O1 . H3 . 1.000 no C19 . H191 . 1.00 no C19 . H192 . 1.000 no C19 . H193 . 1.00 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 . Re1 . N2 . 74.7(2) yes N1 . Re1 . S1 . 149.69(18) yes N2 . Re1 . S1 . 80.83(16) yes N1 . Re1 . N5 . 79.8(2) yes N2 . Re1 . N5 . 109.2(2) yes S1 . Re1 . N5 . 91.92(15) yes N1 . Re1 . N6 . 108.3(2) yes N2 . Re1 . N6 . 175.82(19) yes S1 . Re1 . N6 . 97.24(15) yes N5 . Re1 . N6 . 74.5(2) yes N1 . Re1 . S2 . 90.72(16) yes N2 . Re1 . S2 . 96.26(15) yes S1 . Re1 . S2 . 109.70(5) yes N5 . Re1 . S2 . 149.07(16) yes N6 . Re1 . S2 . 80.85(15) yes Re1 . N1 . C1 . 124.0(5) yes Re1 . N1 . C5 . 116.4(4) yes C1 . N1 . C5 . 119.4(6) yes N1 . C1 . C2 . 122.4(7) yes N1 . C1 . H11 . 118.8 no C2 . C1 . H11 . 118.8 no C1 . C2 . C3 . 118.3(7) yes C1 . C2 . H21 . 120.8 no C3 . C2 . H21 . 120.8 no C2 . C3 . C4 . 120.5(6) yes C2 . C3 . H31 . 119.7 no C4 . C3 . H31 . 119.7 no C3 . C4 . C5 . 118.9(6) yes C3 . C4 . H41 . 120.5 no C5 . C4 . H41 . 120.5 no N1 . C5 . C4 . 120.4(6) yes N1 . C5 . C6 . 115.0(6) yes C4 . C5 . C6 . 124.6(6) yes C5 . C6 . C7 . 124.7(5) yes C5 . C6 . N2 . 112.7(5) yes C7 . C6 . N2 . 122.6(5) yes C6 . C7 . H71 . 109.5 no C6 . C7 . H72 . 109.5 no H71 . C7 . H72 . 109.5 no C6 . C7 . H73 . 109.5 no H71 . C7 . H73 . 109.5 no H72 . C7 . H73 . 109.5 no Re1 . N2 . C6 . 121.1(4) yes Re1 . N2 . N3 . 122.5(4) yes C6 . N2 . N3 . 116.2(5) yes N2 . N3 . C8 . 110.7(5) yes N3 . C8 . S1 . 123.8(5) yes N3 . C8 . N4 . 120.5(6) yes S1 . C8 . N4 . 115.7(5) yes Re1 . S1 . C8 . 96.9(2) yes C8 . N4 . C9 . 123.0(6) yes C8 . N4 . H1 . 124.2 no C9 . N4 . H1 . 112.2 no N4 . C9 . H91 . 109.5 no N4 . C9 . H92 . 109.5 no H91 . C9 . H92 . 109.5 no N4 . C9 . H93 . 109.5 no H91 . C9 . H93 . 109.5 no H92 . C9 . H93 . 109.5 no Re1 . N5 . C10 . 124.3(5) yes Re1 . N5 . C14 . 116.3(4) yes C10 . N5 . C14 . 119.2(6) yes N5 . C10 . C11 . 121.9(7) yes N5 . C10 . H101 . 119.1 no C11 . C10 . H101 . 119.1 no C10 . C11 . C12 . 119.9(6) yes C10 . C11 . H111 . 120.1 no C12 . C11 . H111 . 120.1 no C11 . C12 . C13 . 119.6(6) yes C11 . C12 . H121 . 120.2 no C13 . C12 . H121 . 120.2 no C12 . C13 . C14 . 119.2(7) yes C12 . C13 . H131 . 120.4 no C14 . C13 . H131 . 120.4 no N5 . C14 . C13 . 120.3(6) yes N5 . C14 . C15 . 115.4(6) yes C13 . C14 . C15 . 124.2(6) yes C14 . C15 . C16 . 124.9(5) yes C14 . C15 . N6 . 112.7(5) yes C16 . C15 . N6 . 122.5(5) yes C15 . C16 . H161 . 109.5 no C15 . C16 . H162 . 109.5 no H161 . C16 . H162 . 109.5 no C15 . C16 . H163 . 109.5 no H161 . C16 . H163 . 109.5 no H162 . C16 . H163 . 109.5 no Re1 . N6 . C15 . 121.0(4) yes Re1 . N6 . N7 . 122.7(4) yes C15 . N6 . N7 . 116.2(5) yes N6 . N7 . C17 . 111.7(5) yes N7 . C17 . S2 . 123.3(5) yes N7 . C17 . N8 . 121.0(6) yes S2 . C17 . N8 . 115.6(5) yes Re1 . S2 . C17 . 96.9(2) yes C17 . N8 . C18 . 122.6(6) yes C17 . N8 . H2 . 128.1 no C18 . N8 . H2 . 108.8 no N8 . C18 . H181 . 109.5 no N8 . C18 . H182 . 109.5 no H181 . C18 . H182 . 109.5 no N8 . C18 . H183 . 109.5 no H181 . C18 . H183 . 109.5 no H182 . C18 . H183 . 109.5 no C19 . O1 . H3 . 109.0 no O1 . C19 . H191 . 109.5 no O1 . C19 . H192 . 109.5 no H191 . C19 . H192 . 109.5 no O1 . C19 . H193 . 109.5 no H191 . C19 . H193 . 109.5 no H192 . C19 . H193 . 109.5 no data_CRYSTALS_3 _database_code_CSD 196180 #========================================================================== # Diffractometer details #========================================================================== _diffrn_measurement_device_type ; Nonius KappaCCD ; _diffrn_radiation_monochromator graphite _computing_data_collection ; KappaCCD software 'Collect' (Nonius, 2000) ; _computing_data_reduction ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; #========================================================================== # General computing #========================================================================== _computing_structure_refinement ; CRYSTALS (Watkin et al, 2001) ; _computing_publication_material ; CRYSTALS (Watkin et al, 2001) ; _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point 'not measured' _refine_ls_matrix_type full _atom_sites_solution_primary direct _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed #************************************************************************** _cell_length_a 8.8775(2) _cell_angle_alpha 96.4542(11) _cell_length_b 11.9729(2) _cell_angle_beta 93.2383(11) _cell_length_c 12.6197(3) _cell_angle_gamma 103.1595(9) _cell_volume 1293.2 _symmetry_cell_setting 'Triclinic ' _symmetry_space_group_name_H-M 'P -1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 International_Tables_Vol_IV_Table_2.2B 'Cl ' 0.1320 0.1590 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 International_Tables_Vol_IV_Table_2.2B 'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 International_Tables_Vol_IV_Table_2.2B 'O ' 0.0080 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 International_Tables_Vol_IV_Table_2.2B 'Re ' -1.5980 7.2320 28.7621 1.6719 15.7189 9.0923 14.5564 0.3505 5.4417 52.0861 10.4720 International_Tables_Vol_IV_Table_2.2B 'S ' 0.1100 0.1240 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 International_Tables_Vol_IV_Table_2.2B _chemical_formula_sum ' C21 H30 Cl1 N8 O1 Re1 S2 ' _chemical_formula_moiety ' C21 H30 Cl1 N8 O1 Re1 S2 ' _chemical_compound_source ; synthesis as described ; _chemical_formula_weight 696.32 _cell_measurement_reflns_used 21583 _cell_measurement_theta_min 5 _cell_measurement_theta_max 28 _cell_measurement_temperature 150 _cell_formula_units_Z 2 _exptl_crystal_description ' plate ' _exptl_crystal_colour ' dark brown ' _exptl_crystal_size_min 0.03 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_max 0.15 _exptl_crystal_density_diffrn 1.788 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 685.624 _exptl_absorpt_coefficient_mu 4.989 _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _exptl_absorpt_correction_T_min 0.47 _exptl_absorpt_correction_T_max 0.86 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 150 _diffrn_reflns_number 21583 _reflns_number_total 5857 _diffrn_reflns_av_R_equivalents 0.047 _diffrn_measured_fraction_theta_max 0.995 _reflns_number_gt 5177 _diffrn_reflns_theta_min 5.10 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _reflns_limit_h_min -11 _reflns_limit_h_max 11 _reflns_limit_k_min -15 _reflns_limit_k_max 15 _reflns_limit_l_min 0 _reflns_limit_l_max 16 _refine_diff_density_min -1.65 _refine_diff_density_max 1.10 _reflns_threshold_expression >3.00\s(I) _refine_ls_number_reflns 5177 _refine_ls_number_parameters 334 _refine_ls_R_factor_gt 0.0268 _refine_ls_wR_factor_ref 0.0316 _refine_ls_goodness_of_fit_ref 0.9856 _refine_ls_shift/su_max 0.019954 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 3 parameters (Carruthers & Watkin , 1979) 2.39 -.476 1.36 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type Re1 0.272555(17) 0.062575(12) 0.25912(1) 0.0179 1.0000 Uani N1 0.3407(4) -0.0774(3) 0.1783(2) 0.0204 1.0000 Uani C1 0.3932(5) -0.1591(3) 0.2266(3) 0.0237 1.0000 Uani C2 0.4359(5) -0.2504(4) 0.1706(3) 0.0284 1.0000 Uani C3 0.4207(5) -0.2627(4) 0.0579(4) 0.0296 1.0000 Uani C4 0.3651(4) -0.1826(3) 0.0071(3) 0.0244 1.0000 Uani C5 0.3246(4) -0.0891(3) 0.0681(3) 0.0188 1.0000 Uani C6 0.2613(4) -0.0022(3) 0.0249(3) 0.0187 1.0000 Uani C7 0.2418(5) 0.0067(4) -0.0919(3) 0.0258 1.0000 Uani N2 0.2204(4) 0.0698(3) 0.0995(2) 0.0196 1.0000 Uani N3 0.1551(4) 0.1544(3) 0.0626(2) 0.0211 1.0000 Uani C8 0.1016(4) 0.2133(3) 0.1403(3) 0.0227 1.0000 Uani S1 0.10267(11) 0.17955(8) 0.27473(7) 0.0237 1.0000 Uani N4 0.0358(4) 0.2990(3) 0.1222(3) 0.0262 1.0000 Uani C9 0.0240(5) 0.3395(4) 0.0173(3) 0.0309 1.0000 Uani C10 0.1758(7) 0.4119(5) -0.0097(4) 0.0445 1.0000 Uani N5 0.1134(4) -0.0708(3) 0.3126(2) 0.0207 1.0000 Uani C11 0.0060(5) -0.1528(3) 0.2473(3) 0.0278 1.0000 Uani C12 -0.0908(6) -0.2448(4) 0.2843(4) 0.0354 1.0000 Uani C13 -0.0761(6) -0.2555(4) 0.3937(4) 0.0389 1.0000 Uani C14 0.0311(5) -0.1748(4) 0.4609(3) 0.0314 1.0000 Uani C15 0.1268(4) -0.0813(3) 0.4197(3) 0.0224 1.0000 Uani C16 0.2462(4) 0.0067(3) 0.4811(3) 0.0217 1.0000 Uani C17 0.2744(5) 0.0189(4) 0.6000(3) 0.0274 1.0000 Uani N6 0.3324(4) 0.0758(3) 0.4213(2) 0.0206 1.0000 Uani N7 0.4516(4) 0.1623(3) 0.4750(2) 0.0233 1.0000 Uani C18 0.5404(5) 0.2173(3) 0.4082(3) 0.0233 1.0000 Uani S2 0.51965(11) 0.17182(8) 0.26689(7) 0.0226 1.0000 Uani N8 0.6567(5) 0.3090(3) 0.4429(3) 0.0300 1.0000 Uani C19 0.6858(6) 0.3636(4) 0.5542(3) 0.0357 1.0000 Uani C20 0.7591(8) 0.4906(5) 0.5575(5) 0.0587 1.0000 Uani Cl1 0.85620(14) 0.4387(1) 0.27031(9) 0.0390 1.0000 Uani O1 0.5803(8) 0.5465(6) 0.2651(7) 0.0557 0.592(8) Uani C21 0.463(3) 0.459(3) 0.2057(15) 0.0608 0.592(8) Uani O101 0.5524(12) 0.4966(9) 0.162(1) 0.0591 0.408(8) Uani C121 0.448(5) 0.460(4) 0.239(2) 0.0551 0.408(8) Uani H1 -0.005(5) 0.330(4) 0.175(4) 0.02(1) 1.0000 Uiso H2 0.714(7) 0.344(5) 0.394(5) 0.043(15) 1.0000 Uiso H3 0.6717 0.5107 0.2668 0.0684 0.5918 Uiso H4 0.6472 0.4785 0.1960 0.0731 0.4082 Uiso H11 0.4009 -0.1522 0.3066 0.0290 1.0000 Uiso H21 0.4772 -0.3072 0.2092 0.0358 1.0000 Uiso H31 0.4501 -0.3289 0.0153 0.0363 1.0000 Uiso H41 0.3533 -0.1906 -0.0729 0.0297 1.0000 Uiso H71 0.2802 -0.0560 -0.1332 0.0323 1.0000 Uiso H72 0.3027 0.0837 -0.1065 0.0323 1.0000 Uiso H73 0.1295 -0.0018 -0.1142 0.0323 1.0000 Uiso H91 -0.0552 0.3870 0.0175 0.0391 1.0000 Uiso H92 -0.0100 0.2707 -0.0386 0.0391 1.0000 Uiso H101 0.1616 0.4373 -0.0817 0.0569 1.0000 Uiso H102 0.2107 0.4814 0.0453 0.0569 1.0000 Uiso H103 0.2559 0.3651 -0.0108 0.0569 1.0000 Uiso H111 -0.0031 -0.1460 0.1691 0.0334 1.0000 Uiso H121 -0.1698 -0.3026 0.2343 0.0412 1.0000 Uiso H131 -0.1439 -0.3220 0.4224 0.0468 1.0000 Uiso H141 0.0418 -0.1819 0.5391 0.0390 1.0000 Uiso H171 0.1962 -0.0419 0.6286 0.0344 1.0000 Uiso H172 0.3812 0.0097 0.6196 0.0344 1.0000 Uiso H173 0.2646 0.0972 0.6314 0.0344 1.0000 Uiso H191 0.7574 0.3263 0.5941 0.0413 1.0000 Uiso H192 0.5854 0.3537 0.5882 0.0413 1.0000 Uiso H201 0.7789 0.5278 0.6336 0.0640 1.0000 Uiso H202 0.8596 0.5005 0.5235 0.0640 1.0000 Uiso H203 0.6875 0.5279 0.5176 0.0640 1.0000 Uiso H211 0.3650 0.4861 0.1991 0.0731 0.5918 Uiso H212 0.4962 0.4398 0.1327 0.0731 0.5918 Uiso H213 0.4448 0.3881 0.2430 0.0731 0.5918 Uiso H1211 0.3436 0.4718 0.2169 0.0674 0.4082 Uiso H1212 0.4872 0.5051 0.3103 0.0674 0.4082 Uiso H1213 0.4395 0.3755 0.2433 0.0674 0.4082 Uiso 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 0.02544(8) 0.01784(8) 0.01247(7) 0.00546(5) 0.00474(5) 0.00657(5) N1 0.0254(15) 0.0220(15) 0.0180(14) 0.0057(12) 0.0065(12) 0.0113(12) C1 0.0320(19) 0.0166(16) 0.0240(18) 0.0045(14) 0.0041(15) 0.0072(14) C2 0.0291(19) 0.028(2) 0.033(2) 0.0100(16) 0.0072(16) 0.0113(16) C3 0.032(2) 0.0247(19) 0.034(2) 0.0028(16) 0.0112(17) 0.0087(16) C4 0.0253(18) 0.0232(18) 0.0258(19) 0.0010(15) 0.0062(15) 0.0078(14) C5 0.0207(16) 0.0201(16) 0.0167(16) 0.0050(13) 0.0081(13) 0.0043(13) C6 0.0182(16) 0.0212(17) 0.0157(16) 0.0039(13) 0.0010(12) 0.0020(13) C7 0.0321(19) 0.032(2) 0.0162(17) 0.0060(15) 0.0038(14) 0.0128(16) N2 0.0232(15) 0.0212(15) 0.0169(14) 0.0080(11) 0.0049(11) 0.0070(12) N3 0.0262(15) 0.0217(15) 0.0182(14) 0.0078(12) 0.0027(12) 0.0090(12) C8 0.0263(18) 0.0224(17) 0.0214(18) 0.0078(14) 0.0046(14) 0.0070(14) S1 0.0328(5) 0.0250(4) 0.0181(4) 0.0078(3) 0.0093(4) 0.0128(4) N4 0.0356(18) 0.0260(16) 0.0230(16) 0.0084(13) 0.0084(14) 0.0157(14) C9 0.043(2) 0.031(2) 0.0236(19) 0.0066(16) 0.0010(17) 0.0184(18) C10 0.060(3) 0.043(3) 0.039(3) 0.024(2) 0.013(2) 0.019(2) N5 0.0275(15) 0.0183(14) 0.0176(14) 0.0045(11) 0.0065(12) 0.0058(12) C11 0.034(2) 0.0239(19) 0.0259(19) 0.0024(15) 0.0048(16) 0.0068(16) C12 0.041(2) 0.029(2) 0.033(2) 0.0040(17) 0.0091(19) 0.0003(18) C13 0.048(3) 0.031(2) 0.038(2) 0.0133(19) 0.018(2) 0.0024(19) C14 0.040(2) 0.030(2) 0.027(2) 0.0140(17) 0.0141(17) 0.0078(18) C15 0.0285(18) 0.0230(17) 0.0204(17) 0.0093(14) 0.0091(14) 0.0107(15) C16 0.0290(18) 0.0271(18) 0.0137(16) 0.0098(14) 0.0056(13) 0.0121(15) C17 0.0297(19) 0.038(2) 0.0185(17) 0.0114(16) 0.0077(14) 0.0109(17) N6 0.0277(16) 0.0199(14) 0.0177(14) 0.0057(11) 0.0074(12) 0.0098(12) N7 0.0304(16) 0.0225(15) 0.0163(14) 0.0016(12) 0.0033(12) 0.0051(13) C18 0.0293(19) 0.0260(18) 0.0157(16) 0.0020(14) 0.0013(14) 0.0094(15) S2 0.0283(5) 0.0235(4) 0.0158(4) 0.0039(3) 0.0064(3) 0.0036(4) N8 0.0383(19) 0.0270(17) 0.0227(17) 0.0065(14) 0.0030(14) 0.0018(14) C19 0.049(3) 0.033(2) 0.0205(19) -0.0017(17) -0.0039(18) 0.0056(19) C20 0.070(4) 0.048(3) 0.042(3) -0.007(2) 0.007(3) -0.013(3) Cl1 0.0491(6) 0.0372(6) 0.0393(6) 0.0125(5) 0.0215(5) 0.0198(5) O1 0.047(3) 0.041(3) 0.083(5) 0.008(3) 0.001(3) 0.019(2) C21 0.056(7) 0.050(4) 0.077(11) -0.003(11) 0.001(7) 0.020(5) O101 0.050(4) 0.051(4) 0.082(5) 0.015(4) 0.005(4) 0.020(3) C121 0.052(7) 0.044(4) 0.072(11) -0.002(11) 0.007(7) 0.022(5) _refine_ls_extinction_method None loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Re1 . N1 . 2.088(3) yes Re1 . N2 . 2.057(3) yes Re1 . S1 . 2.2821(9) yes Re1 . N5 . 2.080(3) yes Re1 . N6 . 2.064(3) yes Re1 . S2 . 2.2743(9) yes N1 . C1 . 1.362(5) yes N1 . C5 . 1.379(5) yes C1 . C2 . 1.373(5) yes C1 . H11 . 1.000 no C2 . C3 . 1.409(6) yes C2 . H21 . 1.000 no C3 . C4 . 1.376(6) yes C3 . H31 . 1.000 no C4 . C5 . 1.413(5) yes C4 . H41 . 1.000 no C5 . C6 . 1.434(5) yes C6 . C7 . 1.493(5) yes C6 . N2 . 1.326(5) yes C7 . H71 . 1.000 no C7 . H72 . 1.000 no C7 . H73 . 1.000 no N2 . N3 . 1.386(4) yes N3 . C8 . 1.316(5) yes C8 . S1 . 1.788(4) yes C8 . N4 . 1.326(5) yes N4 . C9 . 1.467(5) yes N4 . H1 . 0.86(5) yes C9 . C10 . 1.507(7) yes C9 . H91 . 1.000 no C9 . H92 . 1.000 no C10 . H101 . 1.000 no C10 . H102 . 1.000 no C10 . H103 . 1.000 no N5 . C11 . 1.363(5) yes N5 . C15 . 1.372(5) yes C11 . C12 . 1.378(6) yes C11 . H111 . 1.000 no C12 . C13 . 1.402(7) yes C12 . H121 . 1.000 no C13 . C14 . 1.366(7) yes C13 . H131 . 1.000 no C14 . C15 . 1.411(5) yes C14 . H141 . 1.000 no C15 . C16 . 1.432(6) yes C16 . C17 . 1.492(5) yes C16 . N6 . 1.325(5) yes C17 . H171 . 1.000 no C17 . H172 . 1.000 no C17 . H173 . 1.000 no N6 . N7 . 1.383(5) yes N7 . C18 . 1.315(5) yes C18 . S2 . 1.792(4) yes C18 . N8 . 1.336(5) yes N8 . C19 . 1.464(5) yes N8 . H2 . 0.90(6) yes C19 . C20 . 1.507(7) yes C19 . H191 . 1.000 no C19 . H192 . 1.000 no C20 . H201 . 1.000 no C20 . H202 . 1.000 no C20 . H203 . 1.000 no O1 . C21 . 1.409(9) yes O1 . O101 . 1.350(13) yes O1 . C121 . 1.38(2) yes O1 . H3 . 1.000 no O1 . H1212 . 1.088 no C21 . O101 . 1.036(18) yes C21 . C121 . 0.45(2) yes C21 . H211 . 1.00 no C21 . H212 . 1.000 no C21 . H213 . 1.00 no C21 . H1211 . 1.12 no C21 . H1213 . 1.13 no O101 . C121 . 1.413(9) yes O101 . H4 . 1.00 no O101 . H212 . 0.786 no C121 . H211 . 1.00 no C121 . H213 . 0.86 no C121 . H1211 . 1.00 no C121 . H1212 . 1.00 no C121 . H1213 . 1.00 no H211 . H1211 . 0.339 no H213 . H1213 . 0.148 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 . Re1 . N2 . 74.98(12) yes N1 . Re1 . S1 . 149.93(9) yes N2 . Re1 . S1 . 80.83(9) yes N1 . Re1 . N5 . 81.34(12) yes N2 . Re1 . N5 . 110.47(12) yes S1 . Re1 . N5 . 90.84(9) yes N1 . Re1 . N6 . 110.17(12) yes N2 . Re1 . N6 . 173.42(12) yes S1 . Re1 . N6 . 95.45(9) yes N5 . Re1 . N6 . 74.86(12) yes N1 . Re1 . S2 . 90.20(9) yes N2 . Re1 . S2 . 95.63(9) yes S1 . Re1 . S2 . 109.91(4) yes N5 . Re1 . S2 . 149.14(9) yes N6 . Re1 . S2 . 80.48(9) yes Re1 . N1 . C1 . 124.8(2) yes Re1 . N1 . C5 . 116.7(2) yes C1 . N1 . C5 . 118.5(3) yes N1 . C1 . C2 . 123.1(4) yes N1 . C1 . H11 . 118.5 no C2 . C1 . H11 . 118.5 no C1 . C2 . C3 . 118.8(4) yes C1 . C2 . H21 . 120.6 no C3 . C2 . H21 . 120.6 no C2 . C3 . C4 . 119.3(4) yes C2 . C3 . H31 . 120.3 no C4 . C3 . H31 . 120.3 no C3 . C4 . C5 . 119.8(4) yes C3 . C4 . H41 . 120.1 no C5 . C4 . H41 . 120.1 no N1 . C5 . C4 . 120.5(3) yes N1 . C5 . C6 . 114.3(3) yes C4 . C5 . C6 . 125.2(3) yes C5 . C6 . C7 . 123.8(3) yes C5 . C6 . N2 . 113.1(3) yes C7 . C6 . N2 . 123.1(3) yes C6 . C7 . H71 . 109.5 no C6 . C7 . H72 . 109.5 no H71 . C7 . H72 . 109.5 no C6 . C7 . H73 . 109.5 no H71 . C7 . H73 . 109.5 no H72 . C7 . H73 . 109.5 no Re1 . N2 . C6 . 120.5(2) yes Re1 . N2 . N3 . 123.3(2) yes C6 . N2 . N3 . 115.9(3) yes N2 . N3 . C8 . 111.9(3) yes N3 . C8 . S1 . 123.0(3) yes N3 . C8 . N4 . 121.6(3) yes S1 . C8 . N4 . 115.3(3) yes Re1 . S1 . C8 . 97.05(13) yes C8 . N4 . C9 . 123.3(3) yes C8 . N4 . H1 . 117.(3) yes C9 . N4 . H1 . 119.(3) yes N4 . C9 . C10 . 112.6(4) yes N4 . C9 . H91 . 108.7 no C10 . C9 . H91 . 108.7 no N4 . C9 . H92 . 108.7 no C10 . C9 . H92 . 108.7 no H91 . C9 . H92 . 109.5 no C9 . C10 . H101 . 109.5 no C9 . C10 . H102 . 109.5 no H101 . C10 . H102 . 109.5 no C9 . C10 . H103 . 109.5 no H101 . C10 . H103 . 109.5 no H102 . C10 . H103 . 109.5 no Re1 . N5 . C11 . 124.2(3) yes Re1 . N5 . C15 . 117.2(2) yes C11 . N5 . C15 . 118.4(3) yes N5 . C11 . C12 . 122.9(4) yes N5 . C11 . H111 . 118.6 no C12 . C11 . H111 . 118.6 no C11 . C12 . C13 . 118.5(4) yes C11 . C12 . H121 . 120.7 no C13 . C12 . H121 . 120.7 no C12 . C13 . C14 . 119.8(4) yes C12 . C13 . H131 . 120.1 no C14 . C13 . H131 . 120.1 no C13 . C14 . C15 . 119.7(4) yes C13 . C14 . H141 . 120.1 no C15 . C14 . H141 . 120.1 no N5 . C15 . C14 . 120.7(4) yes N5 . C15 . C16 . 114.2(3) yes C14 . C15 . C16 . 125.1(4) yes C15 . C16 . C17 . 124.0(3) yes C15 . C16 . N6 . 113.1(3) yes C17 . C16 . N6 . 122.9(4) yes C16 . C17 . H171 . 109.5 no C16 . C17 . H172 . 109.5 no H171 . C17 . H172 . 109.5 no C16 . C17 . H173 . 109.5 no H171 . C17 . H173 . 109.5 no H172 . C17 . H173 . 109.5 no Re1 . N6 . C16 . 120.2(3) yes Re1 . N6 . N7 . 123.0(2) yes C16 . N6 . N7 . 116.4(3) yes N6 . N7 . C18 . 111.6(3) yes N7 . C18 . S2 . 122.8(3) yes N7 . C18 . N8 . 121.5(3) yes S2 . C18 . N8 . 115.7(3) yes Re1 . S2 . C18 . 96.70(13) yes C18 . N8 . C19 . 123.7(4) yes C18 . N8 . H2 . 118.(4) yes C19 . N8 . H2 . 117.(4) yes N8 . C19 . C20 . 109.6(4) yes N8 . C19 . H191 . 109. no C20 . C19 . H191 . 109. no N8 . C19 . H192 . 109.4 no C20 . C19 . H192 . 109.4 no H191 . C19 . H192 . 109.5 no C19 . C20 . H201 . 109.5 no C19 . C20 . H202 . 109.5 no H201 . C20 . H202 . 109.5 no C19 . C20 . H203 . 109.5 no H201 . C20 . H203 . 109.5 no H202 . C20 . H203 . 109.5 no C21 . O1 . O101 . 44.1(8) yes C21 . O1 . C121 . 18.4(10) yes O101 . O1 . C121 . 62.4(8) yes C21 . O1 . H3 . 103.0 no O101 . O1 . H3 . 85.3 no C121 . O1 . H3 . 108.4 no C21 . O1 . H1212 . 64.4 no O101 . O1 . H1212 . 108.5 no C121 . O1 . H1212 . 46.1 no H3 . O1 . H1212 . 113.4 no O1 . C21 . O101 . 64.9(9) yes O1 . C21 . C121 . 76.6(39) yes O101 . C21 . C121 . 141.5(44) yes O1 . C21 . H211 . 109.5 no O101 . C21 . H211 . 116.6 no C121 . C21 . H211 . 76.9(133) no O1 . C21 . H212 . 109.5 no O101 . C21 . H212 . 45.4 no C121 . C21 . H212 . 168.1(154) no H211 . C21 . H212 . 109.5 no O1 . C21 . H213 . 109.5 no O101 . C21 . H213 . 132.7 no C121 . C21 . H213 . 58.6(118) no H211 . C21 . H213 . 109.5 no H212 . C21 . H213 . 109.5 no O1 . C21 . H1211 . 112.7 no O101 . C21 . H1211 . 133.7 no C121 . C21 . H1211 . 62.8(117) no H211 . C21 . H1211 . 17.2 no H212 . C21 . H1211 . 121.2 no O1 . C21 . H1213 . 112.6 no O101 . C21 . H1213 . 132.2 no C121 . C21 . H1213 . 61.4(117) no H211 . C21 . H1213 . 109.0 no H212 . C21 . H1213 . 106.7 no H213 . C21 . H1211 . 92.9 no H213 . C21 . H1213 . 3.40 no H1211 . C21 . H1213 . 92.8 no O1 . O101 . C21 . 71.0(9) yes O1 . O101 . C121 . 59.7(12) yes C21 . O101 . C121 . 11.3(15) yes O1 . O101 . H4 . 69.9 no C21 . O101 . H4 . 104.6 no C121 . O101 . H4 . 98.7 no O1 . O101 . H212 . 134.4 no C21 . O101 . H212 . 64.9 no C121 . O101 . H212 . 75.9 no H4 . O101 . H212 . 110.3 no O1 . C121 . C21 . 85.0(35) yes O1 . C121 . O101 . 57.9(8) yes C21 . C121 . O101 . 27.1(31) yes O1 . C121 . H211 . 112.1 no C21 . C121 . H211 . 77.4(136) no O101 . C121 . H211 . 90.2 no O1 . C121 . H213 . 123.3 no C21 . C121 . H213 . 95.0(131) no O101 . C121 . H213 . 108.0 no H211 . C121 . H213 . 123.2 no O1 . C121 . H1211 . 124.8 no C21 . C121 . H1211 . 93.8(134) no O101 . C121 . H1211 . 109.5 no H211 . C121 . H1211 . 19.5 no H213 . C121 . H1211 . 111.8 no O1 . C121 . H1212 . 51.6 no C21 . C121 . H1212 . 136.6 no O101 . C121 . H1212 . 109.5 no H211 . C121 . H1212 . 115.1 no H213 . C121 . H1212 . 108.6 no O1 . C121 . H1213 . 125.6 no C21 . C121 . H1213 . 95.6(128) no O101 . C121 . H1213 . 109.5 no H211 . C121 . H1213 . 121.0 no H213 . C121 . H1213 . 2.4 no H1211 . C121 . H1212 . 109.5 no H1211 . C121 . H1213 . 109.5 no H1212 . C121 . H1213 . 109.5 no C21 . H211 . C121 . 25.8 no C21 . H211 . H1211 . 102.2 no C121 . H211 . H1211 . 80.5 no C21 . H212 . O101 . 69.7 no C21 . H213 . C121 . 26.4 no C21 . H213 . H1213 . 153.0 no C121 . H213 . H1213 . 163.8 no C21 . H1211 . C121 . 23.4 no C21 . H1211 . H211 . 60.7 no C121 . H1211 . H211 . 79.9 no O1 . H1212 . C121 . 82.3 no C21 . H1213 . C121 . 23.0 no C21 . H1213 . H213 . 23.6 no C121 . H1213 . H213 . 13.8 no data_CRYSTALS_4 _database_code_CSD 196181 _audit_creation_date 01-22-10 _audit_creation_method CRYSTALS_ver_12-03-99 # Diffractometer details #========================================================================== _diffrn_measurement_device_type ; Nonius KappaCCD ; _diffrn_radiation_monochromator graphite _computing_data_collection ; KappaCCD software 'Collect' (Nonius, 2000) ; _computing_data_reduction ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; #========================================================================== # General computing #========================================================================== _computing_structure_refinement ; CRYSTALS (Watkin et al, 2001) ; _computing_publication_material ; CRYSTALS (Watkin et al, 2001) ; _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point 'not measured' _refine_ls_matrix_type full _atom_sites_solution_primary direct _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed #************************************************************************** _cell_length_a 8.6587(2) _cell_angle_alpha 90 _cell_length_b 12.7664(2) _cell_angle_beta 90 _cell_length_c 21.9866(4) _cell_angle_gamma 90 _cell_volume 2430.4 _symmetry_cell_setting 'Orthorhombic ' _symmetry_space_group_name_H-M 'P c c n ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y,z+1/2 x+1/2,-y,-z+1/2 x,-y+1/2,z+1/2 -x,y+1/2,-z+1/2 -x+1/2,-y+1/2,z x+1/2,y+1/2,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 International_Tables_Vol_IV_Table_2.2B 'Cl ' 0.1320 0.1590 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 International_Tables_Vol_IV_Table_2.2B 'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 International_Tables_Vol_IV_Table_2.2B 'O ' 0.0080 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 International_Tables_Vol_IV_Table_2.2B 'Re ' -1.5980 7.2320 28.7621 1.6719 15.7189 9.0923 14.5564 0.3505 5.4417 52.0861 10.4720 International_Tables_Vol_IV_Table_2.2B 'S ' 0.1100 0.1240 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 International_Tables_Vol_IV_Table_2.2B _chemical_formula_sum ' C18 H26 Cl1 N8 O2 Re1 S2 ' _chemical_formula_moiety ' C18 H26 Cl1 N8 O2 Re1 S2 ' _chemical_compound_source ; synthesis as described ; _chemical_formula_weight 672.24 _cell_measurement_reflns_used 16068 _cell_measurement_theta_min 5 _cell_measurement_theta_max 28 _cell_measurement_temperature 150 _cell_formula_units_Z 4 _exptl_crystal_description ' block ' _exptl_crystal_colour ' black ' _exptl_crystal_size_min 0.06 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_max 0.12 _exptl_crystal_density_diffrn 1.837 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 1315.278 _exptl_absorpt_coefficient_mu 5.314 _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _exptl_absorpt_correction_T_min 0.59 _exptl_absorpt_correction_T_max 0.73 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 150 _diffrn_reflns_number 16068 _reflns_number_total 2765 _diffrn_reflns_av_R_equivalents 0.033 _diffrn_measured_fraction_theta_max 0.997 _reflns_number_gt 1861 _diffrn_reflns_theta_min 5.14 _diffrn_reflns_theta_max 27.45 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _reflns_limit_h_min 0 _reflns_limit_h_max 11 _reflns_limit_k_min 0 _reflns_limit_k_max 16 _reflns_limit_l_min 0 _reflns_limit_l_max 28 _refine_diff_density_min -1.03 _refine_diff_density_max 0.65 _reflns_threshold_expression >3.00\s(I) _refine_ls_number_reflns 1861 _refine_ls_number_parameters 158 _refine_ls_R_factor_gt 0.0197 _refine_ls_wR_factor_ref 0.0259 _refine_ls_goodness_of_fit_ref 0.9780 _refine_ls_shift/su_max 0.005382 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 3 parameters, Carruthers & Watkin , 1979, 1.69 0.402 1.28 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type Re1 0.2500 0.7500 0.467426(6) 0.0147 0.5000 Uani S1 0.46596(8) 0.74892(7) 0.40778(3) 0.0194 1.0000 Uani C1 0.4574(4) 0.6138(2) 0.38764(14) 0.0208 1.0000 Uani N1 0.3775(3) 0.5438(2) 0.41870(12) 0.0198 1.0000 Uani N2 0.2911(3) 0.5913(2) 0.46433(11) 0.0180 1.0000 Uani C2 0.2268(3) 0.5279(2) 0.50496(14) 0.0181 1.0000 Uani C3 0.1382(4) 0.5820(2) 0.55009(14) 0.0191 1.0000 Uani C4 0.0695(4) 0.5359(3) 0.60127(14) 0.0269 1.0000 Uani C5 -0.0106(5) 0.5967(3) 0.64174(14) 0.0313 1.0000 Uani C6 -0.0241(4) 0.7046(3) 0.63146(15) 0.0280 1.0000 Uani C7 0.0467(4) 0.7475(3) 0.58158(13) 0.0227 1.0000 Uani N3 0.1256(3) 0.6878(2) 0.54055(11) 0.0185 1.0000 Uani N4 0.5413(4) 0.5840(3) 0.34009(14) 0.0311 1.0000 Uani C8 0.2502(4) 0.4117(2) 0.50308(16) 0.0261 1.0000 Uani O1 0.4886(4) 0.5832(2) 0.74349(14) 0.0460 1.0000 Uani C9 0.3439(7) 0.6247(4) 0.7553(2) 0.0606 1.0000 Uani Cl1 0.7500 0.7500 0.76566(5) 0.0274 0.5000 Uani H1 0.525(5) 0.519(3) 0.3224(17) 0.03(1) 1.0000 Uiso H2 0.587(6) 0.626(4) 0.323(2) 0.044(14) 1.0000 Uiso H3 0.560(7) 0.630(4) 0.748(2) 0.065(17) 1.0000 Uiso H41 0.0791 0.4587 0.6082 0.0323 1.0000 Uiso H51 -0.0591 0.5643 0.6785 0.0375 1.0000 Uiso H61 -0.0846 0.7496 0.6601 0.0336 1.0000 Uiso H71 0.0403 0.8249 0.5751 0.0273 1.0000 Uiso H81 0.1925 0.3784 0.5374 0.0313 1.0000 Uiso H82 0.3628 0.3956 0.5071 0.0313 1.0000 Uiso H83 0.2110 0.3836 0.4635 0.0313 1.0000 Uiso H91 0.2637 0.5693 0.7494 0.0727 1.0000 Uiso H92 0.3401 0.6505 0.7983 0.0727 1.0000 Uiso H93 0.3235 0.6843 0.7269 0.0727 1.0000 Uiso 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 0.0173(1) 0.0137(1) 0.0131(1) 0.0000 0.0000 -0.00111(8) S1 0.0213(3) 0.0172(3) 0.0199(3) -0.0014(3) 0.0044(3) -0.0026(4) C1 0.0208(15) 0.0187(15) 0.0228(15) -0.0036(12) -0.0013(12) 0.0015(12) N1 0.0222(14) 0.0156(12) 0.0215(12) -0.002(1) 0.0033(11) -0.0012(11) N2 0.0212(14) 0.0136(13) 0.0193(14) -0.0035(9) 0.0006(9) -0.0008(11) C2 0.0169(18) 0.0166(14) 0.0207(14) 0.0038(12) -0.0047(11) -0.0042(12) C3 0.0190(14) 0.0209(15) 0.0174(13) 0.0028(13) -0.0041(12) -0.0016(13) C4 0.0296(18) 0.0287(18) 0.0223(14) 0.0064(14) 0.0003(14) -0.0079(15) C5 0.035(2) 0.041(2) 0.0175(14) 0.0054(14) 0.0038(14) -0.0089(17) C6 0.0277(18) 0.0363(18) 0.0202(14) -0.0045(15) 0.0025(14) -0.0010(16) C7 0.0250(15) 0.0244(14) 0.0188(12) -0.0036(15) 0.0011(11) -0.0046(15) N3 0.0163(13) 0.0241(15) 0.0152(11) 0.0007(11) 0.001(1) -0.0030(11) N4 0.0391(18) 0.0233(15) 0.0310(15) -0.0062(14) 0.0135(14) -0.0061(14) C8 0.0285(16) 0.0171(14) 0.0326(15) 0.0022(12) 0.0017(16) -0.0021(16) O1 0.0509(19) 0.0332(16) 0.0539(18) -0.0115(14) 0.0063(16) -0.0069(15) C9 0.065(3) 0.065(3) 0.052(3) -0.017(3) -0.007(3) 0.018(3) Cl1 0.0254(5) 0.0348(6) 0.0220(5) 0.0000 0.0000 0.0059(6) _refine_ls_extinction_method None loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Re1 . S1 . 2.2840(7) yes Re1 . S1 7_565 2.2840(7) yes Re1 . N2 . 2.059(3) yes Re1 . N2 7_565 2.059(3) yes Re1 . N3 . 2.091(3) yes Re1 . N3 7_565 2.091(3) yes S1 . C1 . 1.782(3) yes C1 . N1 . 1.320(4) yes C1 . N4 . 1.329(4) yes N1 . N2 . 1.391(4) yes N2 . C2 . 1.327(4) yes C2 . C3 . 1.432(5) yes C2 . C8 . 1.498(4) yes C3 . C4 . 1.402(4) yes C3 . N3 . 1.372(4) yes C4 . C5 . 1.370(5) yes C4 . H41 . 1.000 no C5 . C6 . 1.400(5) yes C5 . H51 . 1.000 no C6 . C7 . 1.371(4) yes C6 . H61 . 1.000 no C7 . N3 . 1.364(4) yes C7 . H71 . 1.000 no N4 . H1 . 0.93(4) no N4 . H2 . 0.76(5) no C8 . H81 . 1.000 no C8 . H82 . 1.000 no C8 . H83 . 1.000 no O1 . C9 . 1.384(6) yes O1 . H3 . 0.86(5) no C9 . H91 . 1.000 no C9 . H92 . 1.000 no C9 . H93 . 1.000 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag S1 . Re1 . S1 7_565 109.92(4) yes S1 . Re1 . N2 . 80.42(8) yes S1 7_565 Re1 . N2 . 97.38(8) yes S1 . Re1 . N2 7_565 97.38(8) yes S1 7_565 Re1 . N2 7_565 80.42(8) yes N2 . Re1 . N2 7_565 176.22(13) yes S1 . Re1 . N3 . 149.38(8) yes S1 7_565 Re1 . N3 . 91.27(7) yes N2 . Re1 . N3 . 74.98(11) yes N2 7_565 Re1 . N3 . 108.1(1) yes S1 . Re1 . N3 7_565 91.27(7) yes S1 7_565 Re1 . N3 7_565 149.38(8) yes N2 . Re1 . N3 7_565 108.1(1) yes N2 7_565 Re1 . N3 7_565 74.98(11) yes N3 . Re1 . N3 7_565 79.51(14) yes Re1 . S1 . C1 . 96.57(11) yes S1 . C1 . N1 . 123.3(2) yes S1 . C1 . N4 . 116.7(3) yes N1 . C1 . N4 . 120.0(3) yes C1 . N1 . N2 . 111.1(3) yes Re1 . N2 . N1 . 123.1(2) yes Re1 . N2 . C2 . 120.3(2) yes N1 . N2 . C2 . 116.5(3) yes N2 . C2 . C3 . 113.4(3) yes N2 . C2 . C8 . 121.9(3) yes C3 . C2 . C8 . 124.7(3) yes C2 . C3 . C4 . 125.5(3) yes C2 . C3 . N3 . 114.3(3) yes C4 . C3 . N3 . 120.2(3) yes C3 . C4 . C5 . 119.9(3) yes C3 . C4 . H41 . 120.1 no C5 . C4 . H41 . 120.1 no C4 . C5 . C6 . 119.7(3) yes C4 . C5 . H51 . 120.2 no C6 . C5 . H51 . 120.2 no C5 . C6 . C7 . 119.0(3) yes C5 . C6 . H61 . 120.5 no C7 . C6 . H61 . 120.5 no C6 . C7 . N3 . 122.0(3) yes C6 . C7 . H71 . 119.0 no N3 . C7 . H71 . 119.0 no Re1 . N3 . C3 . 116.8(2) yes Re1 . N3 . C7 . 123.7(2) yes C3 . N3 . C7 . 119.3(3) yes C1 . N4 . H1 . 120.1(25) no C1 . N4 . H2 . 118.0(34) no H1 . N4 . H2 . 120.1(41) no C2 . C8 . H81 . 109.5 no C2 . C8 . H82 . 109.5 no H81 . C8 . H82 . 109.5 no C2 . C8 . H83 . 109.5 no H81 . C8 . H83 . 109.5 no H82 . C8 . H83 . 109.5 no C9 . O1 . H3 . 110.8(36) no O1 . C9 . H91 . 109.5 no O1 . C9 . H92 . 109.5 no H91 . C9 . H92 . 109.5 no O1 . C9 . H93 . 109.5 no H91 . C9 . H93 . 109.5 no H92 . C9 . H93 . 109.5 no