# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_global _journal_coden_Cambridge 182 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Konchenko, Sergey' 'Llusar, Rosa' 'Petrov, Pavel' 'Virovets, Aleksandr' 'Bogomyakov, Artem' 'Gomez Garcia, Carlos' 'Polo, Victor' _publ_contact_author_name 'Dr. Alexander Virovets' _publ_contact_author_address ; Institute of Inorganic Chemistry SD RAS Ak.Lavrentiev prosp. 3 Novosibirsk 630090 Russia ; _publ_contact_author_fax '+7 3833 309489' _publ_contact_author_email a_v_virovets@yahoo.com _publ_section_title ; Synthesis, molecular and electronic structure of an incomplete cuboidal Re3S4 cluster with an unusual quadruplet ground state ; # Attachment '- Konchenko_Re3S4_cifs.txt' #TrackingRef '- Konchenko_Re3S4_cifs.txt' data_1Br*3MeCN _database_code_depnum_ccdc_archive 'CCDC 855429' #TrackingRef '- Konchenko_Re3S4_cifs.txt' _vrf_PLAT214_I ; PROBLEM: Atom C33S (Anion/Solvent) ADP max/min Ratio 9.1 prola RESPONSE: This atom belongs to disordered solvent molecule. ; _vrf_PLAT601_I ; PROBLEM: Structure Contains Solvent Accessible VOIDS of . 384 A**3 RESPONSE: All our attemts to localize more solvent molecules failed. We tried to refine residual density peaks as disordered solvent molecules but no reasonable geometry was obtained. We did not applied PLATON/SQUEEZE procedure because R value is already very good (0.0339). It means that missing disordered molecules add almost nothing to the diffraction pattern. ; _vrf_PLAT761_I ; PROBLEM: CIF Contains no X-H Bonds ...................... ? RESPONSE: All H atoms are in geometrically calculated positions. ; _vrf_PLAT762_I ; PROBLEM: CIF Contains no X-Y-H or H-Y-H Angles .......... ? RESPONSE: All H atoms are in geometrically calculated positions. ; _vrf_PLAT430_I ; PROBLEM: Short Inter D...A Contact N2AS .. N3BS .. 2.61 Ang. RESPONSE: Both atoms belong to disordered MeCN solvent molecule. ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_sum 'C84 H81 Br4 N3 P6 Re3 S4' _chemical_formula_weight 2324.82 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 44.6606(12) _cell_length_b 13.7072(4) _cell_length_c 29.2555(8) _cell_angle_alpha 90.00 _cell_angle_beta 98.4630(10) _cell_angle_gamma 90.00 _cell_volume 17714.4(9) _cell_formula_units_Z 8 _cell_measurement_temperature 100.0(2) _cell_measurement_reflns_used 9930 _cell_measurement_theta_min 2.3514 _cell_measurement_theta_max 31.5933 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.743 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 9000 _exptl_absorpt_coefficient_mu 6.140 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.647042 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details 'based on intensities (SADABS, Bruker, 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100.0(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8Apex CCD detector' _diffrn_measurement_method 'combined omega- and phi-scans' _diffrn_detector_area_resol_mean 25 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 54964 _diffrn_reflns_av_R_equivalents 0.0234 _diffrn_reflns_av_sigmaI/netI 0.0361 _diffrn_reflns_limit_h_min -63 _diffrn_reflns_limit_h_max 64 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 31.62 _reflns_number_total 26356 _reflns_number_gt 21811 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 V.1.27 (Bruker, 2005)' _computing_cell_refinement 'Apex2 V.1.27 (Bruker, 2005)' _computing_data_reduction 'Apex2 V.1.27 (Bruker, 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL V6.22 (Bruker, 2000-2005)' _computing_publication_material 'local programs' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0424P)^2^+204.4582P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 26356 _refine_ls_number_parameters 975 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0473 _refine_ls_R_factor_gt 0.0339 _refine_ls_wR_factor_ref 0.0976 _refine_ls_wR_factor_gt 0.0915 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re 0.117681(4) 0.952507(12) 0.157264(5) 0.01078(4) Uani 1 1 d . . . Re2 Re 0.157673(4) 0.808024(12) 0.138910(6) 0.01142(4) Uani 1 1 d . . . Re3 Re 0.124680(4) 0.909887(13) 0.066194(6) 0.01293(4) Uani 1 1 d . . . S1 S 0.16148(2) 0.97526(8) 0.12333(4) 0.01302(19) Uani 1 1 d . . . S2 S 0.12067(2) 0.79290(8) 0.18409(4) 0.01391(19) Uani 1 1 d . . . S3 S 0.07979(2) 0.91785(9) 0.09783(4) 0.0170(2) Uani 1 1 d . . . S4 S 0.12782(3) 0.74409(9) 0.07379(4) 0.0178(2) Uani 1 1 d . . . Br1 Br 0.148681(9) 1.00457(3) 0.235181(14) 0.01462(8) Uani 1 1 d . . . Br2 Br 0.204697(10) 0.78283(4) 0.098859(15) 0.01770(9) Uani 1 1 d . . . Br3 Br 0.114997(11) 1.08614(4) 0.034837(16) 0.02188(10) Uani 1 1 d . . . Br4 Br 0.09046(2) 0.26234(5) 0.32931(2) 0.05018(18) Uani 1 1 d . . . P11 P 0.10838(3) 1.13439(8) 0.15763(4) 0.0141(2) Uani 1 1 d . . . P12 P 0.07582(2) 0.95829(8) 0.20536(4) 0.0132(2) Uani 1 1 d . . . P21 P 0.20079(3) 0.81923(9) 0.20509(4) 0.0146(2) Uani 1 1 d . . . P22 P 0.16527(3) 0.63017(9) 0.15813(4) 0.0192(2) Uani 1 1 d . . . P31 P 0.16190(3) 0.92473(9) 0.00817(4) 0.0161(2) Uani 1 1 d . . . P32 P 0.09124(3) 0.85986(10) -0.00692(4) 0.0179(2) Uani 1 1 d . . . C11 C 0.08901(11) 1.1569(3) 0.20806(16) 0.0180(9) Uani 1 1 d . . . H11F H 0.1035 1.1487 0.2369 0.022 Uiso 1 1 calc R . . H11G H 0.0812 1.2246 0.2071 0.022 Uiso 1 1 calc R . . C12 C 0.06277(10) 1.0850(3) 0.20756(17) 0.0184(9) Uani 1 1 d . . . H12F H 0.0473 1.0982 0.1804 0.022 Uiso 1 1 calc R . . H12G H 0.0532 1.0945 0.2357 0.022 Uiso 1 1 calc R . . C21 C 0.21967(11) 0.6995(4) 0.20615(17) 0.0202(9) Uani 1 1 d . . . H21F H 0.2302 0.6930 0.1788 0.024 Uiso 1 1 calc R . . H21G H 0.2350 0.6944 0.2341 0.024 Uiso 1 1 calc R . . C22 C 0.19668(12) 0.6181(4) 0.20612(17) 0.0229(10) Uani 1 1 d . . . H22F H 0.1885 0.6189 0.2358 0.027 Uiso 1 1 calc R . . H22G H 0.2069 0.5546 0.2036 0.027 Uiso 1 1 calc R . . C31 C 0.13712(11) 0.9392(4) -0.04730(16) 0.0215(10) Uani 1 1 d . . . H31F H 0.1255 1.0008 -0.0478 0.026 Uiso 1 1 calc R . . H31G H 0.1492 0.9402 -0.0731 0.026 Uiso 1 1 calc R . . C32 C 0.11576(11) 0.8519(4) -0.05182(16) 0.0229(10) Uani 1 1 d . . . H32F H 0.1276 0.7905 -0.0482 0.027 Uiso 1 1 calc R . . H32G H 0.1033 0.8517 -0.0827 0.027 Uiso 1 1 calc R . . C111 C 0.08229(11) 1.2028(4) 0.11479(16) 0.0185(9) Uani 1 1 d . . . C112 C 0.05461(11) 1.1611(4) 0.09560(17) 0.0222(10) Uani 1 1 d . . . H11C H 0.0508 1.0941 0.1009 0.027 Uiso 1 1 calc R . . C113 C 0.03270(13) 1.2175(4) 0.06878(19) 0.0290(12) Uani 1 1 d . . . H11A H 0.0139 1.1892 0.0562 0.035 Uiso 1 1 calc R . . C114 C 0.03845(15) 1.3150(5) 0.0604(2) 0.0372(14) Uani 1 1 d . . . H11D H 0.0235 1.3534 0.0422 0.045 Uiso 1 1 calc R . . C115 C 0.06577(15) 1.3559(4) 0.0784(2) 0.0379(14) Uani 1 1 d . . . H11E H 0.0697 1.4223 0.0722 0.046 Uiso 1 1 calc R . . C116 C 0.08778(13) 1.3004(4) 0.1058(2) 0.0289(11) Uani 1 1 d . . . H11B H 0.1065 1.3293 0.1183 0.035 Uiso 1 1 calc R . . C121 C 0.14275(11) 1.2078(3) 0.16667(17) 0.0191(9) Uani 1 1 d . . . C122 C 0.15373(12) 1.2466(4) 0.20948(19) 0.0256(10) Uani 1 1 d . . . H12A H 0.1427 1.2379 0.2346 0.031 Uiso 1 1 calc R . . C123 C 0.18086(13) 1.2985(4) 0.2162(2) 0.0335(13) Uani 1 1 d . . . H12C H 0.1884 1.3243 0.2458 0.040 Uiso 1 1 calc R . . C124 C 0.19672(13) 1.3122(4) 0.1796(2) 0.0349(13) Uani 1 1 d . . . H12D H 0.2151 1.3484 0.1840 0.042 Uiso 1 1 calc R . . C125 C 0.18623(14) 1.2739(4) 0.1370(2) 0.0353(13) Uani 1 1 d . . . H12E H 0.1975 1.2829 0.1122 0.042 Uiso 1 1 calc R . . C126 C 0.15929(13) 1.2221(4) 0.1300(2) 0.0284(11) Uani 1 1 d . . . H12B H 0.1520 1.1963 0.1003 0.034 Uiso 1 1 calc R . . C131 C 0.04159(10) 0.8876(4) 0.18724(16) 0.0173(9) Uani 1 1 d . . . C132 C 0.04250(12) 0.7966(4) 0.16542(19) 0.0247(10) Uani 1 1 d . . . H13B H 0.0611 0.7725 0.1579 0.030 Uiso 1 1 calc R . . C133 C 0.01635(12) 0.7420(4) 0.1549(2) 0.0309(12) Uani 1 1 d . . . H13D H 0.0171 0.6806 0.1401 0.037 Uiso 1 1 calc R . . C134 C -0.01099(12) 0.7762(5) 0.1659(2) 0.0307(12) Uani 1 1 d . . . H13E H -0.0289 0.7383 0.1587 0.037 Uiso 1 1 calc R . . C135 C -0.01209(11) 0.8659(4) 0.18749(17) 0.0243(10) Uani 1 1 d . . . H13C H -0.0307 0.8896 0.1950 0.029 Uiso 1 1 calc R . . C136 C 0.01401(10) 0.9209(4) 0.19801(16) 0.0195(9) Uani 1 1 d . . . H13A H 0.0131 0.9823 0.2128 0.023 Uiso 1 1 calc R . . C141 C 0.08494(10) 0.9215(3) 0.26560(15) 0.0157(8) Uani 1 1 d . . . C142 C 0.08977(11) 0.9909(4) 0.30065(17) 0.0228(10) Uani 1 1 d . . . H14B H 0.0885 1.0585 0.2933 0.027 Uiso 1 1 calc R . . C143 C 0.09648(12) 0.9610(5) 0.34650(18) 0.0295(12) Uani 1 1 d . . . H14D H 0.0995 1.0085 0.3704 0.035 Uiso 1 1 calc R . . C144 C 0.09885(13) 0.8640(5) 0.35764(18) 0.0325(13) Uani 1 1 d . . . H14E H 0.1039 0.8444 0.3890 0.039 Uiso 1 1 calc R . . C145 C 0.09387(12) 0.7943(4) 0.32286(19) 0.0287(11) Uani 1 1 d . . . H14C H 0.0954 0.7270 0.3305 0.034 Uiso 1 1 calc R . . C146 C 0.08675(11) 0.8228(4) 0.27710(17) 0.0222(10) Uani 1 1 d . . . H14A H 0.0831 0.7749 0.2535 0.027 Uiso 1 1 calc R . . C211 C 0.22978(10) 0.9084(4) 0.19682(16) 0.0190(9) Uani 1 1 d . . . C212 C 0.22341(11) 1.0078(4) 0.19823(16) 0.0202(9) Uani 1 1 d . . . H21A H 0.2045 1.0287 0.2057 0.024 Uiso 1 1 calc R . . C213 C 0.24461(12) 1.0768(4) 0.18871(18) 0.0270(11) Uani 1 1 d . . . H21B H 0.2401 1.1444 0.1895 0.032 Uiso 1 1 calc R . . C214 C 0.27256(13) 1.0460(5) 0.17801(19) 0.0314(12) Uani 1 1 d . . . H21C H 0.2871 1.0927 0.1714 0.038 Uiso 1 1 calc R . . C215 C 0.27909(12) 0.9478(5) 0.1771(2) 0.0316(12) Uani 1 1 d . . . H21E H 0.2982 0.9273 0.1700 0.038 Uiso 1 1 calc R . . C216 C 0.25802(11) 0.8783(5) 0.18638(18) 0.0266(11) Uani 1 1 d . . . H21D H 0.2628 0.8108 0.1857 0.032 Uiso 1 1 calc R . . C221 C 0.19690(11) 0.8275(4) 0.26646(15) 0.0186(9) Uani 1 1 d . . . C222 C 0.21875(13) 0.8765(5) 0.29693(19) 0.0325(13) Uani 1 1 d . . . H22C H 0.2341 0.9132 0.2854 0.039 Uiso 1 1 calc R . . C223 C 0.21813(16) 0.8717(6) 0.3441(2) 0.0465(18) Uani 1 1 d . . . H22E H 0.2330 0.9055 0.3648 0.056 Uiso 1 1 calc R . . C224 C 0.19621(15) 0.8184(5) 0.36105(19) 0.0382(15) Uani 1 1 d . . . H22D H 0.1963 0.8138 0.3935 0.046 Uiso 1 1 calc R . . C225 C 0.17404(13) 0.7714(4) 0.33119(18) 0.0292(12) Uani 1 1 d . . . H22B H 0.1587 0.7356 0.3431 0.035 Uiso 1 1 calc R . . C226 C 0.17415(12) 0.7763(4) 0.28440(17) 0.0229(10) Uani 1 1 d . . . H22A H 0.1586 0.7447 0.2640 0.027 Uiso 1 1 calc R . . C231 C 0.17554(13) 0.5523(4) 0.11195(19) 0.0262(11) Uani 1 1 d . . . C232 C 0.20558(13) 0.5377(4) 0.10699(18) 0.0261(11) Uani 1 1 d . . . H23A H 0.2212 0.5642 0.1291 0.031 Uiso 1 1 calc R . . C233 C 0.21302(15) 0.4844(4) 0.0699(2) 0.0343(13) Uani 1 1 d . . . H23B H 0.2337 0.4745 0.0669 0.041 Uiso 1 1 calc R . . C234 C 0.19086(19) 0.4461(5) 0.0376(2) 0.0476(19) Uani 1 1 d . . . H23E H 0.1962 0.4108 0.0121 0.057 Uiso 1 1 calc R . . C235 C 0.16092(19) 0.4588(5) 0.0422(3) 0.051(2) Uani 1 1 d . . . H23D H 0.1456 0.4311 0.0201 0.062 Uiso 1 1 calc R . . C236 C 0.15307(15) 0.5123(5) 0.0791(2) 0.0397(15) Uani 1 1 d . . . H23C H 0.1323 0.5215 0.0820 0.048 Uiso 1 1 calc R . . C241 C 0.13336(15) 0.5663(4) 0.1773(2) 0.0357(14) Uani 1 1 d . . . C242 C 0.13756(18) 0.5050(5) 0.2149(3) 0.0490(19) Uani 1 1 d . . . H24B H 0.1573 0.4957 0.2313 0.059 Uiso 1 1 calc R . . C243 C 0.1132(2) 0.4563(6) 0.2292(4) 0.071(3) Uani 1 1 d . . . H24D H 0.1162 0.4149 0.2555 0.085 Uiso 1 1 calc R . . C244 C 0.0846(2) 0.4695(6) 0.2042(4) 0.074(3) Uani 1 1 d . . . H24E H 0.0679 0.4368 0.2140 0.089 Uiso 1 1 calc R . . C245 C 0.07960(18) 0.5287(5) 0.1656(4) 0.057(2) Uani 1 1 d . . . H24C H 0.0599 0.5350 0.1483 0.069 Uiso 1 1 calc R . . C246 C 0.10401(15) 0.5788(4) 0.1526(3) 0.0436(17) Uani 1 1 d . . . H24A H 0.1009 0.6219 0.1269 0.052 Uiso 1 1 calc R . . C311 C 0.18635(11) 1.0315(4) 0.01633(16) 0.0200(9) Uani 1 1 d . . . C312 C 0.18090(13) 1.1142(4) -0.01153(18) 0.0256(11) Uani 1 1 d . . . H31A H 0.1641 1.1155 -0.0356 0.031 Uiso 1 1 calc R . . C313 C 0.19988(16) 1.1944(4) -0.0041(2) 0.0350(14) Uani 1 1 d . . . H31D H 0.1963 1.2501 -0.0234 0.042 Uiso 1 1 calc R . . C314 C 0.22404(15) 1.1937(5) 0.0313(2) 0.0362(14) Uani 1 1 d . . . H31C H 0.2366 1.2496 0.0369 0.043 Uiso 1 1 calc R . . C315 C 0.22987(13) 1.1116(5) 0.0585(2) 0.0325(13) Uani 1 1 d . . . H31E H 0.2469 1.1103 0.0822 0.039 Uiso 1 1 calc R . . C316 C 0.21105(12) 1.0309(4) 0.05132(18) 0.0248(10) Uani 1 1 d . . . H31B H 0.2150 0.9749 0.0704 0.030 Uiso 1 1 calc R . . C321 C 0.18699(10) 0.8315(4) -0.01140(15) 0.0181(9) Uani 1 1 d . . . C322 C 0.18100(12) 0.7324(4) -0.00951(17) 0.0242(10) Uani 1 1 d . . . H32A H 0.1651 0.7101 0.0060 0.029 Uiso 1 1 calc R . . C323 C 0.19811(14) 0.6657(4) -0.03015(19) 0.0313(12) Uani 1 1 d . . . H32B H 0.1939 0.5980 -0.0285 0.038 Uiso 1 1 calc R . . C324 C 0.22126(14) 0.6973(5) -0.0532(2) 0.0357(14) Uani 1 1 d . . . H32D H 0.2328 0.6512 -0.0675 0.043 Uiso 1 1 calc R . . C325 C 0.22766(13) 0.7963(5) -0.05536(19) 0.0318(13) Uani 1 1 d . . . H32E H 0.2436 0.8180 -0.0710 0.038 Uiso 1 1 calc R . . C326 C 0.21058(11) 0.8632(4) -0.03463(17) 0.0237(10) Uani 1 1 d . . . H32C H 0.2149 0.9309 -0.0362 0.028 Uiso 1 1 calc R . . C331 C 0.05945(11) 0.9336(4) -0.03432(16) 0.0197(9) Uani 1 1 d . . . C332 C 0.04716(12) 0.9087(4) -0.07970(17) 0.0235(10) Uani 1 1 d . . . H33B H 0.0561 0.8580 -0.0952 0.028 Uiso 1 1 calc R . . C333 C 0.02190(12) 0.9578(4) -0.10224(19) 0.0281(11) Uani 1 1 d . . . H33A H 0.0138 0.9404 -0.1330 0.034 Uiso 1 1 calc R . . C334 C 0.00876(12) 1.0310(5) -0.08031(19) 0.0312(12) Uani 1 1 d . . . H33D H -0.0082 1.0653 -0.0960 0.037 Uiso 1 1 calc R . . C335 C 0.02045(14) 1.0549(5) -0.0348(2) 0.0381(15) Uani 1 1 d . . . H33E H 0.0111 1.1048 -0.0192 0.046 Uiso 1 1 calc R . . C336 C 0.04574(12) 1.0059(5) -0.01209(19) 0.0314(13) Uani 1 1 d . . . H33C H 0.0536 1.0225 0.0189 0.038 Uiso 1 1 calc R . . C341 C 0.07280(12) 0.7417(4) -0.00557(18) 0.0254(11) Uani 1 1 d . . . C342 C 0.0789(2) 0.6659(5) -0.0329(4) 0.073(3) Uani 1 1 d . . . H34D H 0.0929 0.6740 -0.0540 0.087 Uiso 1 1 calc R . . C343 C 0.0645(3) 0.5772(7) -0.0300(5) 0.101(5) Uani 1 1 d . . . H34E H 0.0697 0.5241 -0.0481 0.121 Uiso 1 1 calc R . . C344 C 0.0436(2) 0.5641(5) -0.0023(3) 0.062(2) Uani 1 1 d . . . H34B H 0.0334 0.5033 -0.0019 0.074 Uiso 1 1 calc R . . C345 C 0.03706(19) 0.6389(7) 0.0255(2) 0.060(2) Uani 1 1 d . . . H34A H 0.0227 0.6300 0.0461 0.072 Uiso 1 1 calc R . . C346 C 0.05156(18) 0.7279(6) 0.0232(2) 0.054(2) Uani 1 1 d . . . H34C H 0.0467 0.7804 0.0420 0.065 Uiso 1 1 calc R . . N1S N 0.21987(17) 1.1139(6) 0.3268(3) 0.072(2) Uani 1 1 d . . . C11S C 0.19606(17) 1.1331(6) 0.3330(2) 0.0486(18) Uani 1 1 d . . . C12S C 0.16583(19) 1.1558(9) 0.3422(3) 0.069(3) Uani 1 1 d . . . N2AS N 0.1820(3) 0.5897(8) 0.4160(4) 0.051(3) Uani 0.604(11) 1 d P . . N2BS N 0.1468(7) 0.542(3) 0.3247(15) 0.145(15) Uani 0.396(11) 1 d P . . C21S C 0.1639(3) 0.5372(9) 0.4031(4) 0.046(3) Uani 0.604(11) 1 d P . . C22S C 0.1402(6) 0.4987(19) 0.3573(12) 0.066(7) Uani 0.396(11) 1 d P . . C23S C 0.1377(3) 0.4587(10) 0.3900(6) 0.107(5) Uani 1 1 d . . . N3AS N 0.1025(7) 0.6421(17) 0.4308(11) 0.230(18) Uani 0.735(17) 1 d P . . N3BS N 0.1369(9) 0.6885(19) 0.4404(9) 0.067(11) Uani 0.265(17) 1 d P . . C31S C 0.0827(4) 0.6941(11) 0.4448(7) 0.139(7) Uani 1 1 d . . . C32S C 0.0613(3) 0.7522(10) 0.4521(4) 0.065(4) Uani 0.735(17) 1 d P . . C33S C 0.1122(12) 0.7040(18) 0.4512(8) 0.058(13) Uani 0.265(17) 1 d P . . 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 0.01039(7) 0.01278(7) 0.00931(7) -0.00013(6) 0.00185(5) 0.00124(6) Re2 0.01092(7) 0.01396(8) 0.00910(7) -0.00082(6) 0.00051(5) 0.00216(6) Re3 0.01217(7) 0.01768(8) 0.00868(7) -0.00034(6) 0.00068(5) 0.00356(6) S1 0.0124(4) 0.0161(5) 0.0107(5) 0.0004(4) 0.0023(3) 0.0008(4) S2 0.0158(5) 0.0128(5) 0.0137(5) 0.0016(4) 0.0042(4) 0.0010(4) S3 0.0119(4) 0.0258(6) 0.0129(5) -0.0031(4) 0.0008(4) 0.0016(4) S4 0.0189(5) 0.0185(5) 0.0143(5) -0.0042(4) -0.0029(4) 0.0042(4) Br1 0.01466(18) 0.01700(19) 0.01192(19) -0.00111(15) 0.00097(14) 0.00083(15) Br2 0.01529(19) 0.0255(2) 0.01255(19) -0.00028(16) 0.00277(15) 0.00689(17) Br3 0.0272(2) 0.0234(2) 0.0159(2) 0.00306(17) 0.00617(17) 0.00871(19) Br4 0.0826(5) 0.0371(3) 0.0331(3) 0.0021(3) 0.0160(3) 0.0085(4) P11 0.0152(5) 0.0129(5) 0.0143(5) 0.0002(4) 0.0030(4) 0.0012(4) P12 0.0118(5) 0.0159(5) 0.0122(5) -0.0009(4) 0.0026(4) 0.0001(4) P21 0.0136(5) 0.0181(5) 0.0115(5) -0.0006(4) 0.0000(4) 0.0022(4) P22 0.0205(6) 0.0149(5) 0.0221(6) -0.0022(5) 0.0032(5) 0.0020(5) P31 0.0152(5) 0.0234(6) 0.0100(5) 0.0003(4) 0.0026(4) 0.0022(4) P32 0.0157(5) 0.0248(6) 0.0120(5) 0.0001(4) -0.0019(4) 0.0034(5) C11 0.020(2) 0.017(2) 0.019(2) -0.0029(17) 0.0077(17) 0.0016(17) C12 0.017(2) 0.018(2) 0.022(2) -0.0017(17) 0.0056(17) 0.0020(17) C21 0.023(2) 0.022(2) 0.015(2) 0.0018(17) -0.0018(17) 0.0090(19) C22 0.036(3) 0.015(2) 0.017(2) 0.0025(17) 0.0027(19) 0.010(2) C31 0.020(2) 0.032(3) 0.011(2) 0.0013(18) -0.0005(16) 0.004(2) C32 0.021(2) 0.036(3) 0.011(2) -0.0044(19) -0.0013(17) 0.005(2) C111 0.021(2) 0.019(2) 0.015(2) 0.0026(17) 0.0022(17) 0.0051(18) C112 0.024(2) 0.023(2) 0.019(2) 0.0008(18) 0.0006(18) 0.0058(19) C113 0.026(3) 0.036(3) 0.023(3) 0.001(2) -0.003(2) 0.013(2) C114 0.040(3) 0.033(3) 0.036(3) 0.011(3) -0.005(3) 0.016(3) C115 0.048(4) 0.018(3) 0.044(4) 0.010(2) -0.005(3) 0.006(2) C116 0.033(3) 0.020(2) 0.031(3) 0.007(2) -0.002(2) 0.003(2) C121 0.020(2) 0.016(2) 0.022(2) 0.0020(17) 0.0031(18) -0.0003(17) C122 0.028(3) 0.023(2) 0.024(3) 0.000(2) 0.000(2) -0.002(2) C123 0.031(3) 0.029(3) 0.037(3) -0.005(2) -0.003(2) -0.009(2) C124 0.027(3) 0.021(3) 0.057(4) -0.003(3) 0.006(3) -0.007(2) C125 0.034(3) 0.025(3) 0.050(4) -0.002(3) 0.019(3) -0.010(2) C126 0.029(3) 0.028(3) 0.031(3) -0.001(2) 0.011(2) -0.005(2) C131 0.0140(19) 0.024(2) 0.014(2) 0.0004(17) 0.0012(15) -0.0004(17) C132 0.019(2) 0.026(3) 0.029(3) -0.002(2) 0.0040(19) 0.000(2) C133 0.024(3) 0.028(3) 0.040(3) -0.007(2) 0.002(2) -0.006(2) C134 0.018(2) 0.038(3) 0.036(3) -0.005(2) 0.002(2) -0.009(2) C135 0.013(2) 0.039(3) 0.021(2) -0.002(2) 0.0028(17) -0.002(2) C136 0.016(2) 0.027(2) 0.016(2) -0.0022(18) 0.0040(16) -0.0022(18) C141 0.0138(19) 0.023(2) 0.0113(19) 0.0004(16) 0.0041(15) -0.0009(17) C142 0.022(2) 0.030(3) 0.017(2) 0.0002(19) 0.0049(18) -0.006(2) C143 0.027(3) 0.048(3) 0.013(2) -0.003(2) 0.0023(19) -0.007(2) C144 0.031(3) 0.052(4) 0.014(2) 0.006(2) 0.004(2) 0.000(3) C145 0.027(3) 0.033(3) 0.027(3) 0.011(2) 0.010(2) 0.002(2) C146 0.023(2) 0.027(3) 0.018(2) 0.0009(19) 0.0071(18) 0.003(2) C211 0.017(2) 0.027(2) 0.013(2) -0.0038(17) -0.0005(16) -0.0028(18) C212 0.019(2) 0.025(2) 0.016(2) -0.0030(18) -0.0006(17) -0.0024(19) C213 0.027(3) 0.029(3) 0.023(3) -0.004(2) 0.000(2) -0.007(2) C214 0.026(3) 0.045(3) 0.023(3) -0.003(2) 0.003(2) -0.014(2) C215 0.015(2) 0.048(3) 0.033(3) -0.005(3) 0.006(2) -0.003(2) C216 0.017(2) 0.038(3) 0.025(3) -0.002(2) 0.0025(19) 0.000(2) C221 0.019(2) 0.025(2) 0.012(2) -0.0012(17) 0.0005(16) 0.0085(18) C222 0.027(3) 0.051(4) 0.018(3) -0.002(2) 0.000(2) -0.006(3) C223 0.047(4) 0.074(5) 0.016(3) -0.009(3) -0.004(2) -0.012(4) C224 0.044(3) 0.057(4) 0.013(3) 0.004(2) 0.005(2) 0.006(3) C225 0.031(3) 0.039(3) 0.019(2) 0.009(2) 0.007(2) 0.010(2) C226 0.024(2) 0.028(3) 0.016(2) 0.0034(19) 0.0017(18) 0.004(2) C231 0.031(3) 0.018(2) 0.028(3) -0.006(2) -0.003(2) 0.009(2) C232 0.035(3) 0.022(2) 0.020(2) -0.0010(19) 0.002(2) 0.012(2) C233 0.049(4) 0.028(3) 0.027(3) 0.000(2) 0.009(3) 0.019(3) C234 0.078(5) 0.035(3) 0.027(3) -0.012(3) -0.003(3) 0.029(3) C235 0.069(5) 0.035(4) 0.042(4) -0.020(3) -0.021(3) 0.016(3) C236 0.037(3) 0.032(3) 0.045(4) -0.017(3) -0.012(3) 0.011(3) C241 0.040(3) 0.014(2) 0.059(4) -0.005(2) 0.023(3) -0.002(2) C242 0.054(4) 0.025(3) 0.075(5) 0.011(3) 0.030(4) 0.002(3) C243 0.086(7) 0.031(4) 0.109(8) 0.020(4) 0.053(6) 0.004(4) C244 0.060(5) 0.034(4) 0.142(10) 0.000(5) 0.059(6) -0.007(4) C245 0.042(4) 0.028(3) 0.109(7) -0.007(4) 0.030(4) -0.002(3) C246 0.038(3) 0.020(3) 0.077(5) -0.011(3) 0.019(3) -0.008(2) C311 0.023(2) 0.024(2) 0.014(2) -0.0020(17) 0.0073(17) -0.0018(19) C312 0.038(3) 0.024(2) 0.017(2) -0.0002(19) 0.009(2) 0.002(2) C313 0.059(4) 0.024(3) 0.024(3) -0.002(2) 0.014(3) -0.006(3) C314 0.050(4) 0.038(3) 0.023(3) -0.006(2) 0.014(3) -0.021(3) C315 0.028(3) 0.046(3) 0.025(3) -0.002(2) 0.007(2) -0.013(3) C316 0.023(2) 0.033(3) 0.019(2) 0.001(2) 0.0045(18) -0.003(2) C321 0.016(2) 0.027(2) 0.011(2) -0.0017(17) 0.0017(15) 0.0064(18) C322 0.025(2) 0.030(3) 0.016(2) -0.0008(19) -0.0006(18) 0.004(2) C323 0.043(3) 0.027(3) 0.023(3) -0.006(2) 0.001(2) 0.012(2) C324 0.037(3) 0.047(4) 0.023(3) -0.010(2) 0.003(2) 0.019(3) C325 0.026(3) 0.049(4) 0.022(3) -0.002(2) 0.009(2) 0.011(3) C326 0.020(2) 0.035(3) 0.017(2) -0.001(2) 0.0060(18) 0.006(2) C331 0.017(2) 0.025(2) 0.016(2) 0.0041(18) -0.0020(16) 0.0016(18) C332 0.023(2) 0.026(2) 0.018(2) 0.0008(19) -0.0054(18) -0.001(2) C333 0.026(3) 0.036(3) 0.020(2) 0.006(2) -0.0086(19) 0.001(2) C334 0.022(2) 0.044(3) 0.025(3) 0.007(2) -0.006(2) 0.009(2) C335 0.032(3) 0.053(4) 0.028(3) 0.000(3) 0.000(2) 0.023(3) C336 0.025(3) 0.049(4) 0.018(2) -0.005(2) -0.0019(19) 0.014(2) C341 0.025(2) 0.029(3) 0.018(2) 0.005(2) -0.0098(18) -0.001(2) C342 0.072(6) 0.026(3) 0.131(9) -0.022(5) 0.051(6) -0.007(4) C343 0.090(8) 0.033(4) 0.193(14) -0.026(6) 0.063(9) -0.010(5) C344 0.066(5) 0.027(3) 0.088(7) 0.021(4) -0.007(5) -0.010(3) C345 0.060(5) 0.085(6) 0.030(4) 0.011(4) -0.006(3) -0.045(5) C346 0.062(5) 0.069(5) 0.033(4) -0.016(3) 0.011(3) -0.039(4) N1S 0.054(4) 0.071(5) 0.097(6) -0.022(5) 0.028(4) -0.032(4) C11S 0.049(4) 0.061(5) 0.038(4) 0.002(3) 0.011(3) -0.028(4) C12S 0.046(4) 0.125(9) 0.038(4) -0.008(5) 0.012(3) 0.005(5) N2AS 0.071(8) 0.039(6) 0.044(6) 0.013(5) 0.008(5) -0.004(5) N2BS 0.067(18) 0.18(4) 0.19(4) -0.03(3) 0.02(2) -0.02(2) C21S 0.063(8) 0.032(6) 0.042(7) 0.001(5) 0.005(6) 0.011(6) C22S 0.048(12) 0.049(14) 0.10(2) -0.028(14) 0.014(14) -0.004(11) C23S 0.113(11) 0.071(8) 0.123(12) -0.013(8) -0.027(9) 0.001(8) N3AS 0.29(3) 0.113(17) 0.35(3) 0.15(2) 0.25(3) 0.14(2) N3BS 0.12(3) 0.030(13) 0.040(15) 0.007(11) -0.031(16) -0.005(16) C31S 0.099(11) 0.098(11) 0.23(2) 0.102(12) 0.048(12) -0.005(9) C32S 0.072(8) 0.073(9) 0.056(7) -0.011(6) 0.026(6) -0.005(7) C33S 0.14(4) 0.012(11) 0.014(11) 0.010(8) -0.012(16) 0.006(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re1 Re2 2.7718(2) . ? Re1 Re3 2.7897(2) . ? Re1 S1 2.3411(10) . ? Re1 S2 2.3215(11) . ? Re1 S3 2.2907(11) . ? Re1 Br1 2.5872(5) . ? Re1 P11 2.5277(12) . ? Re1 P12 2.5010(11) . ? Re2 Re3 2.7791(2) . ? Re2 S1 2.3483(11) . ? Re2 S2 2.2727(10) . ? Re2 S4 2.3297(11) . ? Re2 Br2 2.5743(5) . ? Re2 P21 2.5265(11) . ? Re2 P22 2.5136(13) . ? Re3 S1 2.3430(11) . ? Re3 S3 2.3312(11) . ? Re3 S4 2.2858(12) . ? Re3 Br3 2.5978(5) . ? Re3 P31 2.5527(11) . ? Re3 P32 2.5170(12) . ? P11 C11 1.843(5) . ? P11 C111 1.838(5) . ? P11 C121 1.822(5) . ? P12 C12 1.836(5) . ? P12 C131 1.822(5) . ? P12 C141 1.821(5) . ? P21 C21 1.844(5) . ? P21 C211 1.823(5) . ? P21 C221 1.833(5) . ? P22 C22 1.840(5) . ? P22 C231 1.832(5) . ? P22 C241 1.829(6) . ? P31 C31 1.836(5) . ? P31 C311 1.820(5) . ? P31 C321 1.846(5) . ? P32 C32 1.833(5) . ? P32 C331 1.829(5) . ? P32 C341 1.821(6) . ? C11 C12 1.529(6) . ? C21 C22 1.516(7) . ? C31 C32 1.524(7) . ? C111 C112 1.403(7) . ? C111 C116 1.392(7) . ? C112 C113 1.395(7) . ? C113 C114 1.389(9) . ? C114 C115 1.375(9) . ? C115 C116 1.398(8) . ? C121 C122 1.383(7) . ? C121 C126 1.403(7) . ? C122 C123 1.394(8) . ? C123 C124 1.379(9) . ? C124 C125 1.369(9) . ? C125 C126 1.386(8) . ? C131 C132 1.405(7) . ? C131 C136 1.393(6) . ? C132 C133 1.383(7) . ? C133 C134 1.389(8) . ? C134 C135 1.386(8) . ? C135 C136 1.384(7) . ? C141 C142 1.393(7) . ? C141 C146 1.393(7) . ? C142 C143 1.393(7) . ? C143 C144 1.369(9) . ? C144 C145 1.389(9) . ? C145 C146 1.386(7) . ? C211 C212 1.393(7) . ? C211 C216 1.403(7) . ? C212 C213 1.396(7) . ? C213 C214 1.396(8) . ? C214 C215 1.378(9) . ? C215 C216 1.394(8) . ? C221 C222 1.394(7) . ? C221 C226 1.399(7) . ? C222 C223 1.387(8) . ? C223 C224 1.371(10) . ? C224 C225 1.380(9) . ? C225 C226 1.371(7) . ? C231 C232 1.385(8) . ? C231 C236 1.396(8) . ? C232 C233 1.389(7) . ? C233 C234 1.368(10) . ? C234 C235 1.374(11) . ? C235 C236 1.393(9) . ? C241 C242 1.376(10) . ? C241 C246 1.410(10) . ? C242 C243 1.391(10) . ? C243 C244 1.389(15) . ? C244 C245 1.384(14) . ? C245 C246 1.387(9) . ? C311 C312 1.397(7) . ? C311 C316 1.390(7) . ? C312 C313 1.385(8) . ? C313 C314 1.381(9) . ? C314 C315 1.381(9) . ? C315 C316 1.386(8) . ? C321 C322 1.387(7) . ? C321 C326 1.404(7) . ? C322 C323 1.385(7) . ? C323 C324 1.383(9) . ? C324 C325 1.391(9) . ? C325 C326 1.388(7) . ? C331 C332 1.402(7) . ? C331 C336 1.378(7) . ? C332 C333 1.393(7) . ? C333 C334 1.368(8) . ? C334 C335 1.396(8) . ? C335 C336 1.396(8) . ? C341 C342 1.363(9) . ? C341 C346 1.371(9) . ? C342 C343 1.383(12) . ? C343 C344 1.334(14) . ? C344 C345 1.366(13) . ? C345 C346 1.388(10) . ? N1S C11S 1.136(10) . ? C11S C12S 1.449(11) . ? N2AS C21S 1.107(16) . ? N2BS C22S 1.19(5) . ? C21S C22S 1.67(3) . ? C21S C23S 1.59(2) . ? C22S C23S 1.12(3) . ? N3AS N3BS 1.65(5) . ? N3AS C31S 1.25(2) . ? N3AS C33S 1.09(4) . ? N3BS C33S 1.21(5) . ? C31S C32S 1.28(2) . ? C31S C33S 1.31(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Re2 Re1 Re3 59.960(6) . . ? S1 Re1 Re2 53.89(3) . . ? S1 Re1 Re3 53.48(3) . . ? S1 Re1 Br1 87.97(3) . . ? S1 Re1 P11 91.06(4) . . ? S1 Re1 P12 167.09(4) . . ? S2 Re1 Re2 52.09(3) . . ? S2 Re1 Re3 96.70(3) . . ? S2 Re1 S1 105.01(4) . . ? S2 Re1 Br1 88.02(3) . . ? S2 Re1 P11 158.33(4) . . ? S2 Re1 P12 81.38(4) . . ? S3 Re1 Re2 97.46(3) . . ? S3 Re1 Re3 53.54(3) . . ? S3 Re1 S1 106.01(4) . . ? S3 Re1 S2 93.47(4) . . ? S3 Re1 Br1 164.98(3) . . ? S3 Re1 P11 95.99(4) . . ? S3 Re1 P12 84.48(4) . . ? Br1 Re1 Re2 95.235(11) . . ? Br1 Re1 Re3 141.131(12) . . ? P11 Re1 Re2 144.74(3) . . ? P11 Re1 Re3 104.61(3) . . ? P11 Re1 Br1 77.95(3) . . ? P12 Re1 Re2 133.47(3) . . ? P12 Re1 Re3 137.90(3) . . ? P12 Re1 Br1 80.96(3) . . ? P12 Re1 P11 80.18(4) . . ? Re1 Re2 Re3 60.340(6) . . ? S1 Re2 Re1 53.65(3) . . ? S1 Re2 Re3 53.59(3) . . ? S1 Re2 Br2 87.44(3) . . ? S1 Re2 P21 91.18(4) . . ? S1 Re2 P22 168.22(4) . . ? S2 Re2 Re1 53.70(3) . . ? S2 Re2 Re3 98.17(3) . . ? S2 Re2 S1 106.35(4) . . ? S2 Re2 S4 93.65(4) . . ? S2 Re2 Br2 164.65(3) . . ? S2 Re2 P21 95.59(4) . . ? S2 Re2 P22 82.37(4) . . ? S4 Re2 Re1 96.87(3) . . ? S4 Re2 Re3 52.26(3) . . ? S4 Re2 S1 104.93(4) . . ? S4 Re2 Br2 89.10(3) . . ? S4 Re2 P21 158.35(4) . . ? S4 Re2 P22 81.96(4) . . ? Br2 Re2 Re1 140.907(13) . . ? Br2 Re2 Re3 95.458(12) . . ? P21 Re2 Re1 104.38(3) . . ? P21 Re2 Re3 144.54(3) . . ? P21 Re2 Br2 77.06(3) . . ? P22 Re2 Re1 135.99(3) . . ? P22 Re2 Re3 134.22(3) . . ? P22 Re2 Br2 83.07(3) . . ? P22 Re2 P21 79.92(4) . . ? Re2 Re3 Re1 59.699(6) . . ? S1 Re3 Re1 53.41(3) . . ? S1 Re3 Re2 53.76(3) . . ? S1 Re3 Br3 87.65(3) . . ? S1 Re3 P31 89.25(4) . . ? S1 Re3 P32 167.59(4) . . ? S3 Re3 Re1 52.21(3) . . ? S3 Re3 Re2 96.30(3) . . ? S3 Re3 S1 104.65(4) . . ? S3 Re3 Br3 89.34(3) . . ? S3 Re3 P31 160.48(4) . . ? S3 Re3 P32 84.99(4) . . ? S4 Re3 Re1 97.43(3) . . ? S4 Re3 Re2 53.70(3) . . ? S4 Re3 S1 106.52(4) . . ? S4 Re3 S3 92.98(4) . . ? S4 Re3 Br3 164.50(3) . . ? S4 Re3 P31 96.16(4) . . ? S4 Re3 P32 80.33(4) . . ? Br3 Re3 Re1 96.100(12) . . ? Br3 Re3 Re2 141.214(14) . . ? P31 Re3 Re1 142.54(3) . . ? P31 Re3 Re2 103.02(3) . . ? P31 Re3 Br3 77.40(3) . . ? P32 Re3 Re1 137.12(3) . . ? P32 Re3 Re2 134.03(3) . . ? P32 Re3 Br3 84.61(3) . . ? P32 Re3 P31 79.61(4) . . ? Re1 S1 Re2 72.47(3) . . ? Re1 S1 Re3 73.11(3) . . ? Re3 S1 Re2 72.66(3) . . ? Re2 S2 Re1 74.21(3) . . ? Re1 S3 Re3 74.25(3) . . ? Re3 S4 Re2 74.04(3) . . ? C11 P11 Re1 105.38(16) . . ? C111 P11 Re1 126.05(16) . . ? C111 P11 C11 97.8(2) . . ? C121 P11 Re1 114.20(16) . . ? C121 P11 C11 106.0(2) . . ? C121 P11 C111 104.7(2) . . ? C12 P12 Re1 108.49(15) . . ? C131 P12 Re1 118.96(15) . . ? C131 P12 C12 104.9(2) . . ? C141 P12 Re1 117.17(14) . . ? C141 P12 C12 104.8(2) . . ? C141 P12 C131 101.1(2) . . ? C21 P21 Re2 104.71(16) . . ? C211 P21 Re2 114.53(16) . . ? C211 P21 C21 105.5(2) . . ? C211 P21 C221 105.1(2) . . ? C221 P21 Re2 125.66(16) . . ? C221 P21 C21 98.5(2) . . ? C22 P22 Re2 108.68(16) . . ? C231 P22 Re2 116.11(18) . . ? C231 P22 C22 105.4(2) . . ? C241 P22 Re2 116.55(19) . . ? C241 P22 C22 105.3(3) . . ? C241 P22 C231 103.8(3) . . ? C31 P31 Re3 103.28(16) . . ? C31 P31 C321 96.6(2) . . ? C311 P31 Re3 114.43(15) . . ? C311 P31 C31 107.5(2) . . ? C311 P31 C321 102.6(2) . . ? C321 P31 Re3 129.47(16) . . ? C32 P32 Re3 106.44(16) . . ? C331 P32 Re3 123.18(17) . . ? C331 P32 C32 103.1(2) . . ? C341 P32 Re3 115.97(16) . . ? C341 P32 C32 106.4(3) . . ? C341 P32 C331 100.2(2) . . ? C12 C11 P11 109.5(3) . . ? C11 C12 P12 111.3(3) . . ? C22 C21 P21 110.3(3) . . ? C21 C22 P22 112.0(3) . . ? C32 C31 P31 106.3(3) . . ? C31 C32 P32 108.9(3) . . ? C112 C111 P11 119.8(4) . . ? C116 C111 P11 120.5(4) . . ? C116 C111 C112 119.1(5) . . ? C113 C112 C111 120.2(5) . . ? C114 C113 C112 120.0(6) . . ? C115 C114 C113 120.1(5) . . ? C114 C115 C116 120.4(5) . . ? C111 C116 C115 120.2(5) . . ? C122 C121 P11 121.5(4) . . ? C122 C121 C126 118.8(5) . . ? C126 C121 P11 119.6(4) . . ? C121 C122 C123 120.6(5) . . ? C124 C123 C122 119.7(6) . . ? C125 C124 C123 120.5(5) . . ? C124 C125 C126 120.3(6) . . ? C125 C126 C121 120.1(5) . . ? C132 C131 P12 121.7(4) . . ? C136 C131 P12 119.5(4) . . ? C136 C131 C132 118.7(4) . . ? C133 C132 C131 120.1(5) . . ? C132 C133 C134 120.5(5) . . ? C135 C134 C133 119.8(5) . . ? C136 C135 C134 120.0(5) . . ? C135 C136 C131 121.0(5) . . ? C142 C141 P12 120.8(4) . . ? C142 C141 C146 119.2(4) . . ? C146 C141 P12 120.0(4) . . ? C143 C142 C141 119.7(5) . . ? C144 C143 C142 120.9(5) . . ? C143 C144 C145 119.6(5) . . ? C146 C145 C144 120.2(5) . . ? C145 C146 C141 120.2(5) . . ? C212 C211 P21 120.0(4) . . ? C212 C211 C216 119.2(5) . . ? C216 C211 P21 120.7(4) . . ? C211 C212 C213 120.6(5) . . ? C212 C213 C214 119.7(5) . . ? C215 C214 C213 119.9(5) . . ? C214 C215 C216 120.9(5) . . ? C215 C216 C211 119.7(5) . . ? C222 C221 P21 119.9(4) . . ? C222 C221 C226 118.7(5) . . ? C226 C221 P21 121.0(4) . . ? C223 C222 C221 119.9(6) . . ? C224 C223 C222 120.3(6) . . ? C223 C224 C225 120.3(5) . . ? C226 C225 C224 120.1(5) . . ? C225 C226 C221 120.6(5) . . ? C232 C231 P22 120.9(4) . . ? C232 C231 C236 118.7(5) . . ? C236 C231 P22 120.3(4) . . ? C231 C232 C233 120.3(6) . . ? C234 C233 C232 120.6(6) . . ? C233 C234 C235 120.0(6) . . ? C234 C235 C236 120.1(6) . . ? C235 C236 C231 120.2(6) . . ? C242 C241 P22 121.1(6) . . ? C242 C241 C246 119.3(6) . . ? C246 C241 P22 119.6(5) . . ? C241 C242 C243 120.9(8) . . ? C244 C243 C242 118.7(9) . . ? C245 C244 C243 122.0(7) . . ? C244 C245 C246 118.4(8) . . ? C245 C246 C241 120.6(8) . . ? C312 C311 P31 121.8(4) . . ? C316 C311 P31 119.2(4) . . ? C316 C311 C312 119.1(5) . . ? C313 C312 C311 120.1(5) . . ? C314 C313 C312 120.4(6) . . ? C313 C314 C315 119.8(5) . . ? C314 C315 C316 120.3(6) . . ? C315 C316 C311 120.3(5) . . ? C322 C321 P31 122.4(4) . . ? C322 C321 C326 119.1(5) . . ? C326 C321 P31 117.9(4) . . ? C323 C322 C321 120.4(5) . . ? C324 C323 C322 120.4(6) . . ? C323 C324 C325 120.1(5) . . ? C326 C325 C324 119.7(5) . . ? C325 C326 C321 120.4(5) . . ? C332 C331 P32 116.8(4) . . ? C336 C331 P32 124.1(4) . . ? C336 C331 C332 118.9(5) . . ? C333 C332 C331 120.5(5) . . ? C334 C333 C332 120.3(5) . . ? C333 C334 C335 119.6(5) . . ? C336 C335 C334 120.2(6) . . ? C331 C336 C335 120.4(5) . . ? C342 C341 P32 122.4(5) . . ? C342 C341 C346 118.2(6) . . ? C346 C341 P32 119.4(5) . . ? C341 C342 C343 119.9(9) . . ? C344 C343 C342 121.9(9) . . ? C343 C344 C345 119.3(8) . . ? C344 C345 C346 119.3(8) . . ? C341 C346 C345 121.3(8) . . ? N1S C11S C12S 178.2(10) . . ? N2AS C21S C22S 145.7(17) . . ? N2AS C21S C23S 174.0(14) . . ? C23S C21S C22S 40.3(11) . . ? N2BS C22S C21S 106(2) . . ? C23S C22S N2BS 171(3) . . ? C23S C22S C21S 66.3(19) . . ? C22S C23S C21S 73.5(17) . . ? C31S N3AS N3BS 114(3) . . ? C33S N3AS N3BS 47(3) . . ? C33S N3AS C31S 68(3) . . ? C33S N3BS N3AS 41.5(19) . . ? N3AS C31S C32S 170(2) . . ? N3AS C31S C33S 50(2) . . ? C32S C31S C33S 132(2) . . ? N3AS C33S N3BS 91(3) . . ? N3AS C33S C31S 62(3) . . ? N3BS C33S C31S 152(3) . . ? _diffrn_measured_fraction_theta_max 0.885 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 3.921 _refine_diff_density_min -2.058 _refine_diff_density_rms 0.194 data_2Br*4.5CH2Cl2 _database_code_depnum_ccdc_archive 'CCDC 855430' #TrackingRef '- Konchenko_Re3S4_cifs.txt' _vrf_LABEL01_I ; PROBLEM: An _atom_site_label occurs more than once in the atom list. RESPONSE: Atom Br4 is splitted over 2 positions with PART instructions. Using 'PART' allows us to have the same 4-character name for both positions of disordered atom(s). ; _vrf_PLAT070_I ; PROBLEM: Duplicate Atomic Label on INPUT ................ BR4 RESPONSE: Atom Br4 is splitted over 2 positions with PART instructions. Using 'PART' allows us to have the same 4-character name for both positions of disordered atom(s). ; _vrf_PLAT214_I ; PROBLEM: Atom C4S (Anion/Solvent) ADP max/min Ratio 6.5 prola RESPONSE: This is because of disorder. We had not enough of good diffraction data to split the positions and described them with a.d.p. ellipsoids. ; _vrf_PLAT431_I ; PROBLEM: Short Inter HL..A Contact Cl3 .. Cl4 .. 2.95 Ang. RESPONSE: Both Cl atoms belong to severely disordered of CH2Cl2 solvent molecule. ; _vrf_PLAT761_I ; PROBLEM: CIF Contains no X-H Bonds ...................... ? RESPONSE: All H atoms are in geometrically calculated positions. ; _vrf_PLAT762_I ; PROBLEM: CIF Contains no X-Y-H or H-Y-H Angles .......... ? RESPONSE: All H atoms are in geometrically calculated positions. ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_sum 'C82.50 H81 Br2.60 Cl10.40 P6 Re3 S4' _chemical_formula_weight 2521.58 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' P P 0.1023 0.0942 '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' Cl Cl 0.1484 0.1585 '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' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.6395(3) _cell_length_b 15.3991(3) _cell_length_c 22.8431(5) _cell_angle_alpha 80.5320(10) _cell_angle_beta 72.6390(10) _cell_angle_gamma 83.4320(10) _cell_volume 4506.04(17) _cell_formula_units_Z 2 _cell_measurement_temperature 100.0(2) _cell_measurement_reflns_used 9927 _cell_measurement_theta_min 2.4379 _cell_measurement_theta_max 30.6227 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.858 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2446 _exptl_absorpt_coefficient_mu 5.723 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.779722 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details 'based on intensities (SADABS, Bruker, 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100.0(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8Apex CCD detector' _diffrn_measurement_method 'combined omega- and phi-scans' _diffrn_detector_area_resol_mean 25 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 47320 _diffrn_reflns_av_R_equivalents 0.0273 _diffrn_reflns_av_sigmaI/netI 0.0519 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 31.57 _reflns_number_total 23261 _reflns_number_gt 17767 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 V.1.27 (Bruker, 2005)' _computing_cell_refinement 'Apex2 V.1.27 (Bruker, 2005)' _computing_data_reduction 'Apex2 V.1.27 (Bruker, 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL V6.22 (Bruker, 2000-2005)' _computing_publication_material 'local programs' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0401P)^2^+61.1813P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 23261 _refine_ls_number_parameters 1032 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.0761 _refine_ls_R_factor_gt 0.0497 _refine_ls_wR_factor_ref 0.1290 _refine_ls_wR_factor_gt 0.1151 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re 0.34141(2) 0.276422(19) 0.187418(12) 0.01637(7) Uani 1 1 d . . . Re2 Re 0.14501(2) 0.313309(18) 0.262628(12) 0.01511(6) Uani 1 1 d . . . Re3 Re 0.21759(2) 0.139515(18) 0.249640(12) 0.01521(6) Uani 1 1 d . . . S1 S 0.18604(13) 0.24857(12) 0.17196(8) 0.0178(3) Uani 1 1 d . . . S2 S 0.29893(14) 0.36436(12) 0.26409(8) 0.0206(4) Uani 1 1 d . . . S3 S 0.38287(13) 0.15181(12) 0.25061(8) 0.0196(3) Uani 1 1 d . . . S4 S 0.14825(13) 0.20015(11) 0.34234(8) 0.0160(3) Uani 1 1 d . . . Br1 Br 0.43208(8) 0.20127(7) 0.09289(5) 0.0242(4) Uani 0.484(4) 1 d P . . Cl1T Cl 0.43208(8) 0.20127(7) 0.09289(5) 0.0242(4) Uani 0.52 1 d P . . Br2 Br 0.11182(8) 0.45815(7) 0.19634(5) 0.0233(3) Uani 0.566(4) 1 d P . . Cl2T Cl 0.11182(8) 0.45815(7) 0.19634(5) 0.0233(3) Uani 0.43 1 d P . . Br3 Br 0.04403(8) 0.08199(7) 0.26023(5) 0.0237(3) Uani 0.549(4) 1 d P . . Cl3T Cl 0.04403(8) 0.08199(7) 0.26023(5) 0.0237(3) Uani 0.45 1 d P . . Br4 Br 0.7598(5) 0.6180(3) 0.3304(4) 0.155(3) Uani 0.571(12) 1 d P A 1 Br4 Br 0.7843(4) 0.6267(4) 0.2919(8) 0.196(6) Uani 0.429(12) 1 d P A 2 P11 P 0.52136(15) 0.30770(14) 0.18000(9) 0.0242(4) Uani 1 1 d . . . P12 P 0.36860(15) 0.40223(14) 0.10003(9) 0.0225(4) Uani 1 1 d . . . P21 P 0.07392(15) 0.40732(12) 0.34695(9) 0.0196(4) Uani 1 1 d . . . P22 P -0.04462(14) 0.31388(12) 0.27377(8) 0.0181(4) Uani 1 1 d . . . P31 P 0.24037(14) 0.00211(13) 0.32181(9) 0.0199(4) Uani 1 1 d . . . P32 P 0.26330(15) 0.02704(13) 0.17480(9) 0.0229(4) Uani 1 1 d . . . C1 C 0.5611(6) 0.4009(6) 0.1178(4) 0.0321(19) Uani 1 1 d . . . H1A H 0.5429 0.4570 0.1356 0.038 Uiso 1 1 calc R . . H1B H 0.6367 0.3953 0.0997 0.038 Uiso 1 1 calc R . . C2 C 0.5096(6) 0.4033(6) 0.0673(4) 0.0272(17) Uani 1 1 d . . . H2A H 0.5359 0.3516 0.0451 0.033 Uiso 1 1 calc R . . H2B H 0.5266 0.4573 0.0371 0.033 Uiso 1 1 calc R . . C3 C -0.0665(6) 0.4172(5) 0.3658(3) 0.0231(15) Uani 1 1 d . . . H3A H -0.0949 0.3694 0.3993 0.028 Uiso 1 1 calc R . . H3B H -0.0927 0.4742 0.3813 0.028 Uiso 1 1 calc R . . C4 C -0.1038(6) 0.4119(5) 0.3100(4) 0.0267(17) Uani 1 1 d . . . H4A H -0.0862 0.4654 0.2794 0.032 Uiso 1 1 calc R . . H4B H -0.1796 0.4098 0.3233 0.032 Uiso 1 1 calc R . . C5 C 0.2935(6) -0.0851(5) 0.2729(4) 0.0293(18) Uani 1 1 d . . . H5A H 0.3673 -0.0777 0.2514 0.035 Uiso 1 1 calc R . . H5B H 0.2872 -0.1437 0.2986 0.035 Uiso 1 1 calc R . . C6 C 0.2335(7) -0.0784(5) 0.2257(4) 0.0304(19) Uani 1 1 d . . . H6A H 0.1587 -0.0792 0.2468 0.036 Uiso 1 1 calc R . . H6B H 0.2548 -0.1285 0.2014 0.036 Uiso 1 1 calc R . . C111 C 0.6205(6) 0.2185(6) 0.1605(4) 0.0319(19) Uani 1 1 d . . . C112 C 0.6717(7) 0.2088(7) 0.0981(5) 0.045(2) Uani 1 1 d . . . H11A H 0.6564 0.2501 0.0657 0.054 Uiso 1 1 calc R . . C113 C 0.7188(8) 0.0890(8) 0.1924(6) 0.057(3) Uani 1 1 d . . . H11B H 0.7352 0.0479 0.2245 0.069 Uiso 1 1 calc R . . C114 C 0.7683(8) 0.0802(8) 0.1317(6) 0.058(3) Uani 1 1 d . . . H11C H 0.8196 0.0335 0.1220 0.070 Uiso 1 1 calc R . . C115 C 0.7438(8) 0.1393(9) 0.0845(6) 0.062(3) Uani 1 1 d . . . H11D H 0.7771 0.1318 0.0426 0.074 Uiso 1 1 calc R . . C116 C 0.6444(7) 0.1579(7) 0.2071(5) 0.040(2) Uani 1 1 d . . . H11E H 0.6099 0.1635 0.2492 0.048 Uiso 1 1 calc R . . C121 C 0.5438(6) 0.3418(6) 0.2475(4) 0.0308(18) Uani 1 1 d . . . C122 C 0.6044(7) 0.4108(7) 0.2409(5) 0.042(2) Uani 1 1 d . . . H12A H 0.6354 0.4402 0.2007 0.051 Uiso 1 1 calc R . . C123 C 0.6207(9) 0.4380(8) 0.2927(6) 0.055(3) Uani 1 1 d . . . H12B H 0.6604 0.4869 0.2878 0.066 Uiso 1 1 calc R . . C124 C 0.5785(9) 0.3931(9) 0.3507(6) 0.061(3) Uani 1 1 d . . . H12C H 0.5911 0.4101 0.3858 0.073 Uiso 1 1 calc R . . C125 C 0.5179(9) 0.3231(9) 0.3583(5) 0.054(3) Uani 1 1 d . . . H12D H 0.4889 0.2927 0.3984 0.065 Uiso 1 1 calc R . . C126 C 0.4999(7) 0.2979(7) 0.3068(4) 0.036(2) Uani 1 1 d . . . H12E H 0.4576 0.2507 0.3120 0.043 Uiso 1 1 calc R . . C131 C 0.3357(6) 0.5193(5) 0.1091(4) 0.0298(18) Uani 1 1 d . . . C132 C 0.3572(7) 0.5524(6) 0.1574(4) 0.037(2) Uani 1 1 d . . . H13A H 0.3815 0.5134 0.1877 0.044 Uiso 1 1 calc R . . C133 C 0.3429(9) 0.6419(7) 0.1607(5) 0.053(3) Uani 1 1 d . . . H13B H 0.3604 0.6649 0.1921 0.063 Uiso 1 1 calc R . . C134 C 0.3032(10) 0.6979(7) 0.1185(5) 0.059(3) Uani 1 1 d . . . H13C H 0.2923 0.7592 0.1215 0.071 Uiso 1 1 calc R . . C135 C 0.2791(9) 0.6663(7) 0.0721(5) 0.051(3) Uani 1 1 d . . . H13D H 0.2517 0.7055 0.0432 0.062 Uiso 1 1 calc R . . C136 C 0.2951(7) 0.5773(6) 0.0676(4) 0.035(2) Uani 1 1 d . . . H13E H 0.2781 0.5554 0.0356 0.042 Uiso 1 1 calc R . . C141 C 0.3232(6) 0.3882(5) 0.0347(4) 0.0267(17) Uani 1 1 d . . . C142 C 0.3902(7) 0.3705(6) -0.0217(4) 0.0324(19) Uani 1 1 d . . . H14A H 0.4624 0.3687 -0.0279 0.039 Uiso 1 1 calc R . . C143 C 0.3530(8) 0.3555(6) -0.0688(4) 0.038(2) Uani 1 1 d . . . H14B H 0.3997 0.3434 -0.1072 0.046 Uiso 1 1 calc R . . C144 C 0.2481(8) 0.3582(6) -0.0605(4) 0.040(2) Uani 1 1 d . . . H14C H 0.2228 0.3475 -0.0930 0.048 Uiso 1 1 calc R . . C145 C 0.1797(7) 0.3765(6) -0.0045(4) 0.036(2) Uani 1 1 d . . . H14D H 0.1076 0.3790 0.0013 0.043 Uiso 1 1 calc R . . C146 C 0.2173(6) 0.3910(6) 0.0430(4) 0.0284(17) Uani 1 1 d . . . H14E H 0.1706 0.4029 0.0814 0.034 Uiso 1 1 calc R . . C211 C 0.1112(7) 0.5211(5) 0.3303(4) 0.0276(17) Uani 1 1 d . . . C212 C 0.1997(8) 0.5410(6) 0.3423(4) 0.039(2) Uani 1 1 d . . . H21A H 0.2430 0.4953 0.3569 0.046 Uiso 1 1 calc R . . C213 C 0.2242(9) 0.6292(7) 0.3327(5) 0.051(3) Uani 1 1 d . . . H21B H 0.2833 0.6437 0.3420 0.062 Uiso 1 1 calc R . . C214 C 0.1627(11) 0.6944(7) 0.3100(5) 0.056(3) Uani 1 1 d . . . H21C H 0.1802 0.7539 0.3029 0.067 Uiso 1 1 calc R . . C215 C 0.0770(10) 0.6751(6) 0.2974(4) 0.048(3) Uani 1 1 d . . . H21D H 0.0353 0.7214 0.2818 0.058 Uiso 1 1 calc R . . C216 C 0.0493(8) 0.5881(5) 0.3070(4) 0.034(2) Uani 1 1 d . . . H21E H -0.0104 0.5749 0.2979 0.041 Uiso 1 1 calc R . . C221 C 0.1013(6) 0.3718(5) 0.4216(3) 0.0235(16) Uani 1 1 d . . . C222 C 0.0271(7) 0.3923(5) 0.4758(4) 0.0286(17) Uani 1 1 d . . . H22A H -0.0385 0.4187 0.4738 0.034 Uiso 1 1 calc R . . C223 C 0.0488(8) 0.3743(6) 0.5319(4) 0.036(2) Uani 1 1 d . . . H22B H -0.0023 0.3878 0.5684 0.043 Uiso 1 1 calc R . . C224 C 0.1443(8) 0.3367(6) 0.5355(4) 0.038(2) Uani 1 1 d . . . H22C H 0.1594 0.3256 0.5742 0.046 Uiso 1 1 calc R . . C225 C 0.2181(7) 0.3153(7) 0.4822(4) 0.036(2) Uani 1 1 d . . . H22D H 0.2837 0.2891 0.4843 0.043 Uiso 1 1 calc R . . C226 C 0.1961(6) 0.3322(6) 0.4257(4) 0.0292(18) Uani 1 1 d . . . H22E H 0.2464 0.3166 0.3895 0.035 Uiso 1 1 calc R . . C231 C -0.0784(6) 0.3295(5) 0.2007(3) 0.0231(15) Uani 1 1 d . . . C232 C -0.0564(6) 0.2599(6) 0.1650(4) 0.0278(17) Uani 1 1 d . . . H23A H -0.0270 0.2047 0.1797 0.033 Uiso 1 1 calc R . . C233 C -0.0777(7) 0.2718(7) 0.1084(4) 0.040(2) Uani 1 1 d . . . H23B H -0.0627 0.2246 0.0843 0.048 Uiso 1 1 calc R . . C234 C -0.1203(7) 0.3516(7) 0.0868(4) 0.041(2) Uani 1 1 d . . . H23C H -0.1340 0.3597 0.0478 0.049 Uiso 1 1 calc R . . C235 C -0.1428(8) 0.4189(7) 0.1219(5) 0.042(2) Uani 1 1 d . . . H23D H -0.1732 0.4736 0.1073 0.050 Uiso 1 1 calc R . . C236 C -0.1219(7) 0.4085(6) 0.1788(4) 0.0329(19) Uani 1 1 d . . . H23E H -0.1376 0.4561 0.2026 0.039 Uiso 1 1 calc R . . C241 C -0.1298(5) 0.2317(5) 0.3256(3) 0.0215(15) Uani 1 1 d . . . C242 C -0.1184(6) 0.2010(5) 0.3839(3) 0.0223(15) Uani 1 1 d . . . H24A H -0.0617 0.2170 0.3949 0.027 Uiso 1 1 calc R . . C243 C -0.1891(6) 0.1471(5) 0.4265(4) 0.0252(16) Uani 1 1 d . . . H24B H -0.1820 0.1282 0.4668 0.030 Uiso 1 1 calc R . . C244 C -0.2690(7) 0.1210(6) 0.4106(4) 0.040(2) Uani 1 1 d . . . H24C H -0.3161 0.0827 0.4395 0.048 Uiso 1 1 calc R . . C245 C -0.2815(7) 0.1505(7) 0.3523(4) 0.044(3) Uani 1 1 d . . . H24D H -0.3376 0.1330 0.3415 0.052 Uiso 1 1 calc R . . C246 C -0.2114(7) 0.2058(6) 0.3098(4) 0.034(2) Uani 1 1 d . . . H24E H -0.2197 0.2257 0.2699 0.041 Uiso 1 1 calc R . . C311 C 0.3299(6) 0.0101(5) 0.3655(4) 0.0288(18) Uani 1 1 d . . . C312 C 0.4327(6) -0.0166(7) 0.3464(5) 0.041(2) Uani 1 1 d . . . H31A H 0.4591 -0.0465 0.3112 0.049 Uiso 1 1 calc R . . C313 C 0.4989(8) 0.0008(8) 0.3797(7) 0.064(4) Uani 1 1 d . . . H31B H 0.5699 -0.0180 0.3669 0.077 Uiso 1 1 calc R . . C314 C 0.4615(9) 0.0445(9) 0.4304(6) 0.063(4) Uani 1 1 d . . . H31C H 0.5070 0.0575 0.4517 0.076 Uiso 1 1 calc R . . C315 C 0.3590(9) 0.0694(8) 0.4503(5) 0.054(3) Uani 1 1 d . . . H31D H 0.3331 0.0986 0.4860 0.065 Uiso 1 1 calc R . . C316 C 0.2923(7) 0.0520(6) 0.4183(4) 0.036(2) Uani 1 1 d . . . H31E H 0.2209 0.0688 0.4326 0.044 Uiso 1 1 calc R . . C321 C 0.1342(5) -0.0505(5) 0.3820(3) 0.0215(15) Uani 1 1 d . . . C322 C 0.0361(6) -0.0111(5) 0.4013(4) 0.0278(17) Uani 1 1 d . . . H32A H 0.0207 0.0474 0.3839 0.033 Uiso 1 1 calc R . . C323 C -0.0406(7) -0.0577(6) 0.4464(4) 0.035(2) Uani 1 1 d . . . H32B H -0.1088 -0.0315 0.4585 0.042 Uiso 1 1 calc R . . C324 C -0.0175(7) -0.1416(6) 0.4736(4) 0.0328(19) Uani 1 1 d . . . H32C H -0.0695 -0.1728 0.5046 0.039 Uiso 1 1 calc R . . C325 C 0.0812(7) -0.1799(5) 0.4554(4) 0.0293(18) Uani 1 1 d . . . H32D H 0.0970 -0.2375 0.4741 0.035 Uiso 1 1 calc R . . C326 C 0.1578(6) -0.1348(5) 0.4102(4) 0.0268(16) Uani 1 1 d . . . H32E H 0.2260 -0.1612 0.3984 0.032 Uiso 1 1 calc R . . C331 C 0.1853(7) 0.0411(6) 0.1215(4) 0.0298(18) Uani 1 1 d . . . C332 C 0.1079(8) -0.0150(7) 0.1271(4) 0.045(3) Uani 1 1 d . . . H33A H 0.0939 -0.0622 0.1603 0.054 Uiso 1 1 calc R . . C333 C 0.0518(8) -0.0019(8) 0.0846(5) 0.053(3) Uani 1 1 d . . . H33B H 0.0005 -0.0410 0.0884 0.064 Uiso 1 1 calc R . . C334 C 0.0693(8) 0.0673(8) 0.0368(5) 0.047(3) Uani 1 1 d . . . H33C H 0.0288 0.0766 0.0087 0.056 Uiso 1 1 calc R . . C335 C 0.1464(7) 0.1233(7) 0.0298(4) 0.040(2) Uani 1 1 d . . . H33D H 0.1598 0.1702 -0.0036 0.048 Uiso 1 1 calc R . . C336 C 0.2033(6) 0.1103(6) 0.0718(4) 0.0285(17) Uani 1 1 d . . . H33E H 0.2556 0.1488 0.0670 0.034 Uiso 1 1 calc R . . C341 C 0.3904(7) -0.0109(5) 0.1274(4) 0.0298(18) Uani 1 1 d . . . C342 C 0.3928(8) -0.0618(6) 0.0810(4) 0.039(2) Uani 1 1 d . . . H34A H 0.3316 -0.0672 0.0706 0.047 Uiso 1 1 calc R . . C343 C 0.4854(10) -0.1039(7) 0.0504(5) 0.054(3) Uani 1 1 d . . . H34B H 0.4876 -0.1379 0.0188 0.065 Uiso 1 1 calc R . . C344 C 0.5735(9) -0.0962(7) 0.0660(5) 0.059(3) Uani 1 1 d . . . H34C H 0.6362 -0.1257 0.0453 0.071 Uiso 1 1 calc R . . C345 C 0.5725(8) -0.0467(7) 0.1111(5) 0.050(3) Uani 1 1 d . . . H34D H 0.6342 -0.0415 0.1210 0.060 Uiso 1 1 calc R . . C346 C 0.4804(7) -0.0041(6) 0.1421(5) 0.038(2) Uani 1 1 d . . . H34E H 0.4794 0.0299 0.1734 0.045 Uiso 1 1 calc R . . Cl1 Cl 1.0097(4) 0.6218(3) 0.0880(2) 0.0836(18) Uani 0.844(10) 1 d P A . Cl2 Cl 1.0422(6) 0.7812(4) 0.1275(4) 0.142(3) Uani 0.835(11) 1 d P A . Cl1A Cl 0.8926(11) 0.6567(8) 0.1947(5) 0.087(5) Uani 0.320(10) 1 d P . . C1SA C 1.0146(13) 0.6692(9) 0.1505(7) 0.024(3) Uani 0.50 1 d P A . C1SB C 0.9939(10) 0.7411(9) 0.0730(6) 0.014(2) Uani 0.50 1 d PU . . Cl3 Cl 0.4519(6) 0.7399(5) 0.3666(5) 0.183(3) Uani 1 1 d . . . Cl4 Cl 0.5048(6) 0.7791(4) 0.4752(3) 0.143(2) Uani 1 1 d . . . C2S C 0.542(3) 0.699(3) 0.4283(15) 0.235(18) Uani 1 1 d . . . Cl5 Cl 0.8971(4) 0.9002(4) 0.2646(3) 0.173(3) Uani 1 1 d . . . Cl6 Cl 0.7445(4) 0.8733(4) 0.3855(2) 0.1121(17) Uani 1 1 d . . . C3S C 0.8558(13) 0.8393(15) 0.3335(9) 0.116(7) Uani 1 1 d . . . Cl7 Cl 0.2876(5) 0.6355(4) 0.5086(4) 0.162(3) Uani 1 1 d . . . Cl8 Cl 0.3923(5) 0.4852(5) 0.4501(5) 0.204(4) Uani 1 1 d . . . C4S C 0.314(3) 0.501(3) 0.515(2) 0.43(4) Uani 1 1 d . . . Cl9 Cl 0.4742(7) 0.2519(6) 0.7812(4) 0.099(4) Uani 0.489(9) 1 d PD . . Cl10 Cl 0.2340(8) 0.1954(7) 0.8420(5) 0.035(4) Uani 0.192(8) 1 d PD . . Cl11 Cl 0.3534(8) 0.1419(6) 0.7503(4) 0.060(3) Uani 0.320(9) 1 d PD . . C5S C 0.3517(14) 0.2267(17) 0.7854(12) 0.103(11) Uiso 0.50 1 d PD . . 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 0.01554(12) 0.01959(14) 0.01359(13) -0.00304(10) -0.00136(9) -0.00613(10) Re2 0.01703(12) 0.01618(13) 0.01210(13) -0.00342(9) -0.00168(9) -0.00563(10) Re3 0.01472(12) 0.01727(13) 0.01373(13) -0.00422(10) -0.00173(9) -0.00478(9) S1 0.0171(7) 0.0231(9) 0.0133(8) -0.0046(6) -0.0018(6) -0.0057(6) S2 0.0208(8) 0.0241(9) 0.0173(9) -0.0061(7) -0.0010(6) -0.0096(7) S3 0.0161(7) 0.0220(9) 0.0204(9) -0.0015(7) -0.0043(6) -0.0051(6) S4 0.0171(7) 0.0164(8) 0.0140(8) -0.0034(6) -0.0012(6) -0.0058(6) Br1 0.0228(6) 0.0289(6) 0.0194(6) -0.0067(4) -0.0002(4) -0.0064(4) Cl1T 0.0228(6) 0.0289(6) 0.0194(6) -0.0067(4) -0.0002(4) -0.0064(4) Br2 0.0242(5) 0.0222(5) 0.0199(6) -0.0023(4) 0.0004(4) -0.0066(4) Cl2T 0.0242(5) 0.0222(5) 0.0199(6) -0.0023(4) 0.0004(4) -0.0066(4) Br3 0.0228(5) 0.0280(6) 0.0220(6) -0.0076(4) -0.0056(4) -0.0048(4) Cl3T 0.0228(5) 0.0280(6) 0.0220(6) -0.0076(4) -0.0056(4) -0.0048(4) Br4 0.176(5) 0.066(3) 0.333(8) -0.119(4) -0.221(6) 0.073(3) Br4 0.047(2) 0.028(2) 0.487(16) 0.010(5) -0.060(5) -0.0035(17) P11 0.0186(9) 0.0319(11) 0.0227(10) -0.0017(8) -0.0046(7) -0.0104(8) P12 0.0208(9) 0.0275(10) 0.0169(9) 0.0002(7) -0.0015(7) -0.0078(7) P21 0.0254(9) 0.0176(9) 0.0157(9) -0.0054(7) -0.0019(7) -0.0070(7) P22 0.0178(8) 0.0201(9) 0.0163(9) -0.0025(7) -0.0035(7) -0.0044(7) P31 0.0167(8) 0.0197(9) 0.0228(10) -0.0027(7) -0.0033(7) -0.0058(7) P32 0.0236(9) 0.0235(10) 0.0201(10) -0.0088(8) 0.0019(7) -0.0093(7) C1 0.028(4) 0.038(5) 0.030(4) 0.004(4) -0.007(3) -0.017(4) C2 0.019(3) 0.035(4) 0.021(4) 0.008(3) 0.000(3) -0.009(3) C3 0.027(4) 0.018(4) 0.021(4) -0.001(3) -0.002(3) -0.005(3) C4 0.021(3) 0.023(4) 0.035(5) -0.003(3) -0.008(3) 0.001(3) C5 0.031(4) 0.020(4) 0.030(4) -0.008(3) 0.003(3) 0.003(3) C6 0.038(4) 0.019(4) 0.028(4) -0.010(3) 0.008(3) -0.012(3) C111 0.017(3) 0.042(5) 0.038(5) -0.006(4) -0.009(3) -0.009(3) C112 0.020(4) 0.059(7) 0.051(6) -0.011(5) 0.001(4) -0.005(4) C113 0.036(5) 0.053(7) 0.080(9) 0.001(6) -0.019(6) 0.003(5) C114 0.030(5) 0.047(7) 0.091(10) -0.015(6) -0.008(6) 0.000(5) C115 0.030(5) 0.068(8) 0.077(9) -0.022(7) 0.008(5) -0.006(5) C116 0.025(4) 0.045(6) 0.052(6) -0.005(4) -0.016(4) -0.003(4) C121 0.027(4) 0.036(5) 0.034(5) -0.004(4) -0.015(3) -0.008(3) C122 0.034(5) 0.046(6) 0.051(6) -0.010(5) -0.015(4) -0.008(4) C123 0.047(6) 0.063(7) 0.071(8) -0.026(6) -0.030(6) -0.012(5) C124 0.048(6) 0.092(10) 0.058(7) -0.031(7) -0.025(6) -0.013(6) C125 0.058(7) 0.081(8) 0.035(6) -0.008(5) -0.025(5) -0.020(6) C126 0.034(4) 0.048(6) 0.034(5) -0.007(4) -0.018(4) -0.008(4) C131 0.028(4) 0.027(4) 0.027(4) -0.004(3) 0.007(3) -0.010(3) C132 0.044(5) 0.039(5) 0.030(5) -0.008(4) -0.005(4) -0.021(4) C133 0.072(7) 0.043(6) 0.037(6) -0.012(5) 0.009(5) -0.031(5) C134 0.086(9) 0.025(5) 0.043(6) -0.006(4) 0.022(6) -0.014(5) C135 0.070(7) 0.030(5) 0.033(6) -0.002(4) 0.016(5) -0.002(5) C136 0.036(5) 0.028(4) 0.029(5) -0.001(3) 0.010(3) -0.006(4) C141 0.028(4) 0.030(4) 0.021(4) 0.003(3) -0.006(3) -0.008(3) C142 0.034(4) 0.038(5) 0.023(4) -0.007(4) -0.004(3) -0.001(4) C143 0.051(6) 0.043(5) 0.021(4) -0.008(4) -0.009(4) 0.000(4) C144 0.054(6) 0.041(5) 0.031(5) 0.001(4) -0.025(4) -0.006(4) C145 0.036(5) 0.042(5) 0.029(5) 0.012(4) -0.016(4) -0.010(4) C146 0.026(4) 0.035(5) 0.022(4) 0.003(3) -0.006(3) -0.004(3) C211 0.042(5) 0.021(4) 0.018(4) -0.007(3) 0.001(3) -0.012(3) C212 0.048(5) 0.029(5) 0.037(5) -0.010(4) 0.001(4) -0.019(4) C213 0.069(7) 0.047(6) 0.039(6) -0.012(5) -0.003(5) -0.032(6) C214 0.100(10) 0.031(5) 0.033(6) -0.006(4) -0.002(6) -0.028(6) C215 0.089(8) 0.024(5) 0.029(5) -0.008(4) -0.010(5) -0.005(5) C216 0.061(6) 0.019(4) 0.020(4) -0.005(3) -0.002(4) -0.009(4) C221 0.037(4) 0.021(4) 0.012(3) -0.001(3) -0.005(3) -0.011(3) C222 0.043(5) 0.018(4) 0.022(4) -0.008(3) -0.002(3) -0.004(3) C223 0.064(6) 0.022(4) 0.017(4) -0.004(3) 0.001(4) -0.009(4) C224 0.065(6) 0.038(5) 0.018(4) -0.008(4) -0.014(4) -0.018(5) C225 0.038(5) 0.052(6) 0.027(4) -0.008(4) -0.016(4) -0.014(4) C226 0.034(4) 0.036(5) 0.020(4) -0.008(3) -0.004(3) -0.014(4) C231 0.020(3) 0.030(4) 0.018(4) 0.003(3) -0.005(3) -0.006(3) C232 0.023(4) 0.041(5) 0.021(4) -0.004(3) -0.009(3) -0.001(3) C233 0.035(5) 0.063(7) 0.026(5) -0.011(4) -0.013(4) -0.008(4) C234 0.031(4) 0.070(7) 0.022(4) 0.006(4) -0.012(3) -0.013(4) C235 0.042(5) 0.043(6) 0.041(6) 0.010(4) -0.021(4) -0.008(4) C236 0.036(4) 0.034(5) 0.030(5) 0.003(4) -0.013(4) -0.008(4) C241 0.020(3) 0.022(4) 0.020(4) -0.002(3) -0.001(3) -0.006(3) C242 0.021(3) 0.026(4) 0.022(4) -0.005(3) -0.008(3) -0.004(3) C243 0.021(3) 0.031(4) 0.021(4) 0.000(3) -0.003(3) -0.008(3) C244 0.030(4) 0.045(5) 0.039(5) 0.020(4) -0.010(4) -0.020(4) C245 0.039(5) 0.055(6) 0.042(5) 0.016(4) -0.021(4) -0.030(5) C246 0.039(5) 0.038(5) 0.031(5) 0.012(4) -0.021(4) -0.018(4) C311 0.021(4) 0.029(4) 0.038(5) 0.011(3) -0.015(3) -0.014(3) C312 0.022(4) 0.044(5) 0.055(6) 0.006(4) -0.011(4) -0.006(4) C313 0.033(5) 0.063(8) 0.093(10) 0.036(7) -0.036(6) -0.013(5) C314 0.058(7) 0.076(9) 0.067(8) 0.033(7) -0.043(6) -0.046(7) C315 0.061(7) 0.070(8) 0.041(6) 0.018(5) -0.030(5) -0.040(6) C316 0.036(5) 0.043(5) 0.036(5) 0.011(4) -0.023(4) -0.018(4) C321 0.021(3) 0.026(4) 0.017(4) -0.006(3) 0.000(3) -0.009(3) C322 0.026(4) 0.024(4) 0.027(4) 0.005(3) -0.001(3) -0.007(3) C323 0.027(4) 0.040(5) 0.032(5) 0.001(4) 0.001(3) -0.012(4) C324 0.032(4) 0.040(5) 0.026(4) -0.003(4) -0.002(3) -0.020(4) C325 0.043(5) 0.023(4) 0.023(4) 0.003(3) -0.009(3) -0.014(3) C326 0.027(4) 0.030(4) 0.024(4) -0.004(3) -0.007(3) -0.006(3) C331 0.035(4) 0.035(5) 0.022(4) -0.016(3) -0.003(3) -0.011(4) C332 0.048(6) 0.062(7) 0.030(5) -0.018(4) -0.004(4) -0.032(5) C333 0.050(6) 0.076(8) 0.043(6) -0.025(6) -0.009(5) -0.032(6) C334 0.048(6) 0.067(7) 0.033(5) -0.020(5) -0.015(4) -0.014(5) C335 0.037(5) 0.057(6) 0.030(5) -0.017(4) -0.009(4) -0.010(4) C336 0.027(4) 0.040(5) 0.020(4) -0.016(3) -0.002(3) -0.006(3) C341 0.037(4) 0.019(4) 0.024(4) -0.006(3) 0.009(3) -0.008(3) C342 0.052(6) 0.033(5) 0.025(5) -0.011(4) 0.006(4) -0.006(4) C343 0.079(8) 0.032(5) 0.034(6) -0.012(4) 0.014(5) -0.002(5) C344 0.052(7) 0.043(6) 0.053(7) -0.002(5) 0.023(5) 0.009(5) C345 0.032(5) 0.044(6) 0.059(7) -0.014(5) 0.013(4) 0.001(4) C346 0.029(4) 0.029(5) 0.044(5) -0.008(4) 0.009(4) -0.007(3) Cl1 0.090(3) 0.111(4) 0.067(3) -0.010(2) -0.046(2) -0.018(3) Cl2 0.150(6) 0.049(3) 0.214(8) -0.018(4) -0.037(5) 0.009(3) Cl1A 0.124(11) 0.076(8) 0.063(7) -0.010(6) -0.035(7) 0.012(7) C1SA 0.044(9) 0.005(6) 0.021(8) 0.004(5) -0.009(7) -0.004(6) C1SB 0.018(4) 0.016(4) 0.010(4) 0.006(3) -0.009(3) -0.004(3) Cl3 0.174(7) 0.113(5) 0.278(10) 0.000(6) -0.110(7) 0.005(5) Cl4 0.208(7) 0.111(4) 0.111(4) 0.011(3) -0.061(4) -0.010(4) C2S 0.20(3) 0.31(5) 0.17(3) -0.12(3) -0.04(2) 0.12(3) Cl5 0.091(3) 0.149(5) 0.212(7) 0.108(5) -0.009(4) -0.020(3) Cl6 0.091(3) 0.136(4) 0.112(4) -0.044(3) -0.041(3) 0.052(3) C3S 0.075(11) 0.151(19) 0.089(13) -0.010(12) 0.014(9) 0.012(11) Cl7 0.102(4) 0.114(5) 0.229(8) -0.036(5) 0.016(4) -0.001(3) Cl8 0.092(4) 0.162(6) 0.336(12) -0.121(7) 0.023(5) -0.023(4) C4S 0.38(5) 0.41(5) 0.41(5) -0.38(5) 0.30(4) -0.34(5) Cl9 0.123(7) 0.094(6) 0.125(7) -0.073(6) -0.086(6) 0.037(5) Cl10 0.041(6) 0.039(6) 0.040(7) -0.026(5) -0.031(5) 0.025(5) Cl11 0.080(7) 0.056(6) 0.049(5) -0.019(4) -0.030(5) 0.025(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re1 Re2 2.7707(4) . ? Re1 Re3 2.7773(4) . ? Re1 S1 2.3461(17) . ? Re1 S2 2.2873(18) . ? Re1 S3 2.3265(18) . ? Re1 Br1 2.5362(11) . ? Re1 P11 2.5060(19) . ? Re1 P12 2.5151(19) . ? Re2 Re3 2.7768(4) . ? Re2 S1 2.3360(17) . ? Re2 S2 2.3355(17) . ? Re2 S4 2.3110(17) . ? Re2 Br2 2.5572(10) . ? Re2 P21 2.4955(19) . ? Re2 P22 2.5213(18) . ? Re3 S1 2.3376(18) . ? Re3 S3 2.2906(17) . ? Re3 S4 2.3459(17) . ? Re3 Br3 2.5524(10) . ? Re3 P31 2.5098(19) . ? Re3 P32 2.530(2) . ? Br4 Cl1A 2.277(19) . ? P11 C1 1.849(8) . ? P11 C111 1.825(9) . ? P11 C121 1.826(9) . ? P12 C2 1.844(7) . ? P12 C131 1.837(9) . ? P12 C141 1.830(8) . ? P21 C3 1.827(8) . ? P21 C211 1.828(8) . ? P21 C221 1.838(8) . ? P22 C4 1.830(8) . ? P22 C231 1.833(8) . ? P22 C241 1.837(7) . ? P31 C5 1.835(8) . ? P31 C311 1.818(8) . ? P31 C321 1.833(7) . ? P32 C6 1.845(8) . ? P32 C331 1.815(9) . ? P32 C341 1.837(8) . ? C1 C2 1.513(11) . ? C3 C4 1.524(11) . ? C5 C6 1.519(13) . ? C111 C112 1.410(13) . ? C111 C116 1.386(13) . ? C112 C115 1.378(15) . ? C113 C114 1.370(17) . ? C113 C116 1.391(14) . ? C114 C115 1.387(18) . ? C121 C122 1.381(12) . ? C121 C126 1.400(12) . ? C122 C123 1.402(14) . ? C123 C124 1.378(17) . ? C124 C125 1.390(16) . ? C125 C126 1.392(13) . ? C131 C132 1.406(12) . ? C131 C136 1.387(13) . ? C132 C133 1.382(14) . ? C133 C134 1.378(17) . ? C134 C135 1.371(17) . ? C135 C136 1.378(13) . ? C141 C142 1.387(11) . ? C141 C146 1.396(11) . ? C142 C143 1.380(12) . ? C143 C144 1.383(14) . ? C144 C145 1.390(14) . ? C145 C146 1.387(12) . ? C211 C212 1.392(13) . ? C211 C216 1.395(13) . ? C212 C213 1.402(13) . ? C213 C214 1.371(17) . ? C214 C215 1.358(17) . ? C215 C216 1.399(12) . ? C221 C222 1.401(11) . ? C221 C226 1.387(12) . ? C222 C223 1.378(12) . ? C223 C224 1.384(14) . ? C224 C225 1.390(13) . ? C225 C226 1.386(11) . ? C231 C232 1.403(12) . ? C231 C236 1.376(11) . ? C232 C233 1.388(11) . ? C233 C234 1.378(14) . ? C234 C235 1.366(15) . ? C235 C236 1.393(13) . ? C241 C242 1.388(10) . ? C241 C246 1.384(11) . ? C242 C243 1.386(10) . ? C243 C244 1.364(12) . ? C244 C245 1.388(13) . ? C245 C246 1.393(11) . ? C311 C312 1.373(12) . ? C311 C316 1.396(14) . ? C312 C313 1.413(15) . ? C313 C314 1.369(19) . ? C314 C315 1.365(17) . ? C315 C316 1.397(12) . ? C321 C322 1.380(11) . ? C321 C326 1.398(11) . ? C322 C323 1.399(10) . ? C323 C324 1.384(13) . ? C324 C325 1.377(12) . ? C325 C326 1.388(11) . ? C331 C332 1.403(11) . ? C331 C336 1.407(12) . ? C332 C333 1.383(15) . ? C333 C334 1.380(16) . ? C334 C335 1.393(13) . ? C335 C336 1.380(12) . ? C341 C342 1.410(12) . ? C341 C346 1.384(13) . ? C342 C343 1.392(14) . ? C343 C344 1.374(18) . ? C344 C345 1.374(17) . ? C345 C346 1.394(12) . ? Cl1 C1SA 1.728(16) . ? Cl1 C1SB 1.814(14) . ? Cl2 C1SA 1.768(14) . ? Cl2 C1SB 1.790(15) . ? Cl1A C1SA 1.68(2) . ? C1SA C1SB 2.007(18) . ? Cl3 C2S 2.11(3) . ? Cl4 C2S 1.70(3) . ? Cl5 C3S 1.667(19) . ? Cl6 C3S 1.714(16) . ? Cl7 C4S 2.05(4) . ? Cl8 C4S 1.58(2) . ? Cl9 C5S 1.729(17) . ? Cl10 Cl11 2.438(14) . ? Cl10 C5S 1.793(17) . ? Cl11 C5S 1.636(18) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Re2 Re1 Re3 60.066(9) . . ? S1 Re1 Re2 53.55(4) . . ? S1 Re1 Re3 53.49(4) . . ? S1 Re1 Br1 86.99(5) . . ? S1 Re1 P11 168.09(6) . . ? S1 Re1 P12 91.44(6) . . ? S2 Re1 Re2 53.98(4) . . ? S2 Re1 Re3 98.40(4) . . ? S2 Re1 S1 106.45(6) . . ? S2 Re1 S3 93.97(7) . . ? S2 Re1 Br1 164.57(5) . . ? S2 Re1 P11 83.04(7) . . ? S2 Re1 P12 95.05(7) . . ? S3 Re1 Re2 96.87(4) . . ? S3 Re1 Re3 52.43(4) . . ? S3 Re1 S1 104.97(6) . . ? S3 Re1 Br1 89.69(5) . . ? S3 Re1 P11 81.04(6) . . ? S3 Re1 P12 158.18(6) . . ? Br1 Re1 Re2 140.39(3) . . ? Br1 Re1 Re3 95.72(3) . . ? P11 Re1 Re2 136.86(5) . . ? P11 Re1 Re3 133.47(5) . . ? P11 Re1 Br1 82.73(5) . . ? P11 Re1 P12 80.38(7) . . ? P12 Re1 Re2 104.50(5) . . ? P12 Re1 Re3 144.73(5) . . ? P12 Re1 Br1 76.69(5) . . ? Re1 Re2 Re3 60.084(10) . . ? S1 Re2 Re1 53.88(4) . . ? S1 Re2 Re3 53.58(4) . . ? S1 Re2 Br2 86.46(5) . . ? S1 Re2 P21 166.16(6) . . ? S1 Re2 P22 90.90(6) . . ? S2 Re2 Re1 52.38(4) . . ? S2 Re2 Re3 97.24(5) . . ? S2 Re2 S1 105.22(6) . . ? S2 Re2 Br2 88.94(5) . . ? S2 Re2 P21 81.31(6) . . ? S2 Re2 P22 158.49(6) . . ? S4 Re2 Re1 97.19(4) . . ? S4 Re2 Re3 53.98(4) . . ? S4 Re2 S1 106.73(6) . . ? S4 Re2 S2 92.80(6) . . ? S4 Re2 Br2 165.68(5) . . ? S4 Re2 P21 84.81(6) . . ? S4 Re2 P22 96.14(6) . . ? Br2 Re2 Re1 95.12(2) . . ? Br2 Re2 Re3 139.84(3) . . ? P21 Re2 Re1 133.67(4) . . ? P21 Re2 Re3 138.74(5) . . ? P21 Re2 Br2 81.41(5) . . ? P21 Re2 P22 80.07(6) . . ? P22 Re2 Re1 144.64(4) . . ? P22 Re2 Re3 103.85(4) . . ? P22 Re2 Br2 77.73(5) . . ? Re2 Re3 Re1 59.850(10) . . ? S1 Re3 Re1 53.77(4) . . ? S1 Re3 Re2 53.52(4) . . ? S1 Re3 S4 105.54(6) . . ? S1 Re3 Br3 87.71(5) . . ? S1 Re3 P31 168.64(6) . . ? S1 Re3 P32 90.15(7) . . ? S3 Re3 Re1 53.62(5) . . ? S3 Re3 Re2 97.57(5) . . ? S3 Re3 S1 106.42(6) . . ? S3 Re3 S4 92.14(6) . . ? S3 Re3 Br3 164.26(5) . . ? S3 Re3 P31 80.47(6) . . ? S3 Re3 P32 95.93(7) . . ? S4 Re3 Re1 96.19(4) . . ? S4 Re3 Re2 52.82(4) . . ? S4 Re3 Br3 90.65(5) . . ? S4 Re3 P31 82.87(6) . . ? S4 Re3 P32 159.57(6) . . ? Br3 Re3 Re1 141.33(3) . . ? Br3 Re3 Re2 96.46(3) . . ? P31 Re3 Re1 134.06(4) . . ? P31 Re3 Re2 135.65(5) . . ? P31 Re3 Br3 84.51(5) . . ? P31 Re3 P32 80.02(7) . . ? P32 Re3 Re1 103.72(4) . . ? P32 Re3 Re2 143.52(5) . . ? P32 Re3 Br3 76.72(5) . . ? Re2 S1 Re1 72.57(5) . . ? Re2 S1 Re3 72.90(5) . . ? Re3 S1 Re1 72.74(5) . . ? Re1 S2 Re2 73.64(5) . . ? Re3 S3 Re1 73.95(5) . . ? Re2 S4 Re3 73.20(5) . . ? C1 P11 Re1 108.5(3) . . ? C111 P11 Re1 116.3(3) . . ? C111 P11 C1 105.4(4) . . ? C111 P11 C121 103.3(4) . . ? C121 P11 Re1 117.7(3) . . ? C121 P11 C1 104.2(4) . . ? C2 P12 Re1 104.9(3) . . ? C131 P12 Re1 125.0(3) . . ? C131 P12 C2 100.1(4) . . ? C141 P12 Re1 115.6(3) . . ? C141 P12 C2 104.1(4) . . ? C141 P12 C131 104.2(4) . . ? C3 P21 Re2 109.2(3) . . ? C3 P21 C211 104.7(4) . . ? C3 P21 C221 104.8(4) . . ? C211 P21 Re2 116.9(3) . . ? C211 P21 C221 100.9(4) . . ? C221 P21 Re2 118.8(3) . . ? C4 P22 Re2 105.4(3) . . ? C4 P22 C231 104.6(4) . . ? C4 P22 C241 99.0(4) . . ? C231 P22 Re2 115.1(2) . . ? C231 P22 C241 105.5(3) . . ? C241 P22 Re2 124.4(3) . . ? C5 P31 Re3 106.1(3) . . ? C311 P31 Re3 113.9(3) . . ? C311 P31 C5 107.6(4) . . ? C311 P31 C321 101.5(4) . . ? C321 P31 Re3 124.0(3) . . ? C321 P31 C5 102.3(4) . . ? C6 P32 Re3 103.4(3) . . ? C331 P32 Re3 114.1(3) . . ? C331 P32 C6 107.4(4) . . ? C331 P32 C341 102.9(4) . . ? C341 P32 Re3 129.3(3) . . ? C341 P32 C6 96.8(4) . . ? C2 C1 P11 111.6(5) . . ? C1 C2 P12 110.9(5) . . ? C4 C3 P21 112.1(5) . . ? C3 C4 P22 110.9(5) . . ? C6 C5 P31 108.1(5) . . ? C5 C6 P32 106.3(5) . . ? C112 C111 P11 120.7(7) . . ? C116 C111 P11 120.0(7) . . ? C116 C111 C112 119.2(9) . . ? C115 C112 C111 119.7(11) . . ? C114 C113 C116 120.2(11) . . ? C113 C114 C115 120.3(11) . . ? C112 C115 C114 120.4(12) . . ? C111 C116 C113 120.3(10) . . ? C122 C121 P11 120.7(7) . . ? C122 C121 C126 119.1(8) . . ? C126 C121 P11 120.2(6) . . ? C121 C122 C123 121.0(10) . . ? C124 C123 C122 119.3(10) . . ? C123 C124 C125 120.7(10) . . ? C124 C125 C126 119.7(11) . . ? C125 C126 C121 120.3(9) . . ? C132 C131 P12 119.3(7) . . ? C136 C131 P12 121.9(7) . . ? C136 C131 C132 118.7(8) . . ? C133 C132 C131 119.7(10) . . ? C134 C133 C132 120.0(10) . . ? C135 C134 C133 121.0(10) . . ? C134 C135 C136 119.5(11) . . ? C135 C136 C131 121.1(10) . . ? C142 C141 P12 122.3(6) . . ? C142 C141 C146 118.9(8) . . ? C146 C141 P12 118.7(6) . . ? C143 C142 C141 120.6(8) . . ? C142 C143 C144 120.4(9) . . ? C143 C144 C145 119.8(8) . . ? C146 C145 C144 119.7(8) . . ? C145 C146 C141 120.5(8) . . ? C212 C211 P21 119.9(7) . . ? C212 C211 C216 120.2(8) . . ? C216 C211 P21 119.8(7) . . ? C211 C212 C213 119.4(10) . . ? C214 C213 C212 119.8(11) . . ? C215 C214 C213 121.0(9) . . ? C214 C215 C216 120.9(11) . . ? C211 C216 C215 118.7(10) . . ? C222 C221 P21 118.7(6) . . ? C226 C221 P21 122.2(6) . . ? C226 C221 C222 118.9(7) . . ? C223 C222 C221 120.3(9) . . ? C222 C223 C224 120.6(8) . . ? C223 C224 C225 119.5(8) . . ? C226 C225 C224 120.0(9) . . ? C225 C226 C221 120.7(8) . . ? C232 C231 P22 119.2(6) . . ? C236 C231 P22 121.8(7) . . ? C236 C231 C232 119.0(7) . . ? C233 C232 C231 119.9(8) . . ? C234 C233 C232 120.5(9) . . ? C235 C234 C233 119.5(8) . . ? C234 C235 C236 120.9(9) . . ? C231 C236 C235 120.1(9) . . ? C242 C241 P22 119.6(6) . . ? C246 C241 P22 121.2(6) . . ? C246 C241 C242 118.9(7) . . ? C243 C242 C241 120.6(7) . . ? C244 C243 C242 120.3(7) . . ? C243 C244 C245 120.0(7) . . ? C244 C245 C246 119.8(8) . . ? C241 C246 C245 120.4(8) . . ? C312 C311 P31 123.3(8) . . ? C312 C311 C316 119.3(8) . . ? C316 C311 P31 117.1(6) . . ? C311 C312 C313 119.5(11) . . ? C314 C313 C312 120.6(11) . . ? C315 C314 C313 120.2(10) . . ? C314 C315 C316 120.0(12) . . ? C311 C316 C315 120.4(10) . . ? C322 C321 P31 124.0(6) . . ? C322 C321 C326 119.8(7) . . ? C326 C321 P31 116.2(6) . . ? C321 C322 C323 119.7(8) . . ? C324 C323 C322 120.3(8) . . ? C325 C324 C323 119.8(7) . . ? C324 C325 C326 120.5(8) . . ? C325 C326 C321 119.8(8) . . ? C332 C331 P32 122.8(7) . . ? C332 C331 C336 118.0(8) . . ? C336 C331 P32 119.2(6) . . ? C333 C332 C331 120.3(10) . . ? C334 C333 C332 120.9(9) . . ? C333 C334 C335 119.9(10) . . ? C336 C335 C334 119.6(10) . . ? C335 C336 C331 121.3(8) . . ? C342 C341 P32 117.3(7) . . ? C346 C341 P32 122.6(7) . . ? C346 C341 C342 119.2(8) . . ? C343 C342 C341 119.7(10) . . ? C344 C343 C342 119.8(10) . . ? C345 C344 C343 121.2(10) . . ? C344 C345 C346 119.6(11) . . ? C341 C346 C345 120.4(10) . . ? C1SA Cl1 C1SB 69.0(6) . . ? C1SA Cl2 C1SB 68.7(7) . . ? C1SA Cl1A Br4 147.0(9) . . ? Cl1 C1SA Cl2 110.5(8) . . ? Cl1 C1SA C1SB 57.5(6) . . ? Cl2 C1SA C1SB 56.2(6) . . ? Cl1A C1SA Cl1 98.6(9) . . ? Cl1A C1SA Cl2 112.7(10) . . ? Cl1A C1SA C1SB 102.0(10) . . ? Cl1 C1SB C1SA 53.5(5) . . ? Cl2 C1SB Cl1 105.7(6) . . ? Cl2 C1SB C1SA 55.1(6) . . ? Cl4 C2S Cl3 100.7(15) . . ? Cl5 C3S Cl6 119.4(12) . . ? Cl8 C4S Cl7 105(2) . . ? C5S Cl10 Cl11 42.1(6) . . ? C5S Cl11 Cl10 47.3(7) . . ? Cl9 C5S Cl10 140.1(18) . . ? Cl11 C5S Cl9 112.2(13) . . ? Cl11 C5S Cl10 90.5(10) . . ? _diffrn_measured_fraction_theta_max 0.771 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 2.747 _refine_diff_density_min -3.012 _refine_diff_density_rms 0.219 #= END of CIF file submission