# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2199 ############################################################################# # Reactions of the dirhenium(III,III) complex cis-Re2(æ-O2CMe)2Cl4(H2O)2 # # that lead to the dirhenium(III,II) complexes Re2(æ-O2CMe)Cl4(PR3)2 and # # tetrarheniumcyclodiyne clusters of the type Re4(æ-O)4Cl4(PR3)4 # # # # Jitendra K. Bera, Sophia S. Lau, Phillip E. Fanwick and Richard A. Walton # # # # Paper ref. B005975G # # Submitted to Dalton Transaction # # E Mail: rawalton@purdue.edu # # Sample Codes Complexes 3, 8, 13, 14 and 15 # ############################################################################# #==================================================================== data_global #==================================================================== _audit_creation_date 19-10-99 _audit_creation_method from_MolEN_and_SHELXL _audit_update_record ; ? ; # 1. SUBMISSION DETAILS _publ_contact_author_name 'Phillip E. Fanwick' _publ_contact_author_address ; Department of Chemistry Purdue University W. Lafayette IN 47907 USA ; _publ_contact_author_email 'fanwick@.xray.chem.purdue.edu' _publ_contact_author_fax '1(765)4940239' _publ_contact_author_phone '1(765)4944572' _publ_requested_journal ? _publ_requested_category ? _publ_requested_coeditor_name ? # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_Cambridge 1078 _journal_name_full ? _journal_volume 9 _journal_year 1999 _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? # 3. TITLE AND AUTHOR LIST _publ_section_title ; ? ; _publ_section_title_footnote ; ? ; # The loop structure below should contain the names and addresses and footnotes # of all authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address _publ_author_footnote 'RICHARD A. WALTON' ; Department of Chemistry Purdue University W. Lafayette IN 47907 USA ; ; ? ; 'JITENDRA K. BERA' ; Department of Chemistry Purdue University W. Lafayette IN 47907 USA ; ; ? ; 'FANWICK, PHILLIP E.' ; Department of Chemistry Purdue University W. Lafayette IN 47907 USA ; ; ? ; # 4. TEXT _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _database_code_CSD 'J0150P' _publ_section_experimental ; ? ; _publ_section_references ; P. T. Beurskens, G. Admirall, G. Beurskens, W. P. Bosman S. Garcia-Granda, R. O. Gould, J. M. M. Smits, '& C. Smykalla (1992). The DIRDIF92 Program System, 'Technical Report. Crystallography Laboratory, Univ. of Nijmegen, The Netherlands. Enraf-Nonius (1993), CAD4 Express, Enraf-Nonius, Delft, The Netherlands. Hall S.R. & du Boulay, D. (1995) Editors U. of Western Aurtralia Johnson, C.K. (1976). ORTEP. Report ORNL-5138. Oak Ridge National Laboratory, Tennessee, USA. Nonius(1998), Collect Users Manual, Nonius 'Delft, The Netherlands. Otwinowski Z. & Minor, W. (1996). Methods Enzymol., 276, 307-327. Sheldrick, G.M. (1997). SHELXL97, Program for the Refinement of Crystal Structures. Univ. of G\"ottingen, Germany. Spek A.L.(1997) PLATON. Program. Univ. of Ultrecht, The Netherlands Spek A.L.(1997) PLUTON. Molecular Graphics Program. Univ. of Ultrecht, The Netherlands ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ;? ; data_J0150P # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.06 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C44 H45 Cl4 O2 P2 Re2' _chemical_formula_structural ? _chemical_formula_weight 1182.01 _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 9.8942(5) _cell_length_b 13.5625(9) _cell_length_c 18.4975(12) _cell_angle_alpha 69.437(3) _cell_angle_beta 76.902(4) _cell_angle_gamma 69.586(3) _cell_volume 2162.7(3) _cell_measurement_reflns_used 17466 _cell_measurement_theta_min 4 _cell_measurement_theta_max 27 _cell_formula_units_z 2 _exptl_crystal_density_diffrn 1.82 _exptl_crystal_density_meas ? _diffrn_radiation_type MO-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 6.027 _cell_measurement_temperature 173 _exptl_crystal_F_000 1146 # 6. DATA COLLECTION _diffrn_ambient_temperature 173 _diffrn_measurement_device_type ? _exptl_absorpt_correction_type refined_empirical_(Spek,_1997 _exptl_absorpt_correction_T_min 0.4970 _exptl_absorpt_correction_T_max 0.8390 _diffrn_reflns_number 17466 _reflns_number_total 9088 _reflns_number_gt 5846 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.063 _diffrn_reflns_theta_min 4.02 _diffrn_reflns_theta_max 27.45 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_max 23 # 7. REFINEMENT DATA _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R_factor_obs 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_R_factor_gt 0.041 _refine_ls_wR_factor_ref 0.099 _refine_ls_hydrogen_treatment H_atoms_riding _refine_ls_number_reflns 9082 _refine_ls_d_res_high 0.77 _refine_ls_number_parameters 489 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 0.998 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0361P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.002 _refine_diff_density_max 0.97 _refine_diff_density_min -1.16 _refine_ls_extinction_method SHELXL97_(Sheldrick_1997) _refine_ls_extinction_coef 0.23E-02 _atom_type_scat_source 'International Tables for Crystallography (Vol C)' # 8. COMPUTING DATA _computing_data_collection Collect_(Nonius,_1998) _computing_cell_refinement DENZO/SCALEPACK_(Otwinowski,_1996) _computing_data_reduction DENZO/SCALEPACK_(Otwinowski,_1996) _computing_structure_solution PATTY_(DIRDIF92,_Beurskins,_1992) _computing_structure_refinement SHELX97_(Sheldrick,_1997) _computing_molecular_graphics ; ORTEP (Johnson, 1976) Xtal_GX (Hall, 1995) PLUTON (Spek, 1991) ; _computing_publication_material CIF_VAX_MolEN_(Fair,_1990) # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag Re1 0.18756(3) 0.34486(2) 0.201680(17) 0.01926(12) Uani ? Re2 0.01020(3) 0.40935(2) 0.285803(17) 0.01955(12) Uani ? Cl11 0.0862(2) 0.27402(17) 0.13517(12) 0.0273(7) Uani ? Cl12 0.2233(2) 0.47848(16) 0.08116(11) 0.0259(7) Uani ? Cl21 -0.1901(2) 0.36527(16) 0.27167(12) 0.0260(7) Uani ? Cl22 -0.0024(2) 0.29454(17) 0.41593(11) 0.0301(7) Uani ? P1 0.2555(2) 0.15813(17) 0.28864(12) 0.0212(7) Uani ? P2 -0.0907(2) 0.58511(16) 0.19524(11) 0.0189(7) Uani ? O1 0.3334(5) 0.3878(4) 0.2409(3) 0.024(2) Uani ? O2 0.1537(6) 0.4636(4) 0.3204(3) 0.025(2) Uani ? C1 0.2866(8) 0.4382(6) 0.2920(5) 0.022(3) Uani ? C2 0.3926(10) 0.4675(8) 0.3173(5) 0.041(4) Uani ? H2A 0.3916 0.5419 0.2882 0.0530 Uiso calc H2B 0.4877 0.4185 0.3088 0.0530 Uiso calc H2C 0.3686 0.4615 0.3717 0.0530 Uiso calc C110 0.3958(8) 0.0771(7) 0.2304(5) 0.026(3) Uani ? H11A 0.4359 0.0028 0.2631 0.0340 Uiso calc H11B 0.3535 0.0728 0.1895 0.0340 Uiso calc C111 0.5146(8) 0.1319(7) 0.1950(5) 0.025(3) Uani ? C112 0.4975(9) 0.2226(7) 0.1292(5) 0.027(3) Uani ? H112 0.4171 0.2435 0.1031 0.0360 Uiso calc C113 0.5956(9) 0.2829(8) 0.1008(5) 0.033(3) Uani ? H113 0.5824 0.3424 0.0558 0.0430 Uiso calc C114 0.7132(9) 0.2538(8) 0.1400(5) 0.037(4) Uani ? H114 0.7771 0.2962 0.1225 0.0480 Uiso calc C115 0.7383(10) 0.1607(9) 0.2063(5) 0.044(4) Uani ? H115 0.8197 0.1397 0.2316 0.0570 Uiso calc C116 0.6388(9) 0.1016(8) 0.2327(5) 0.035(4) Uani ? H116 0.6538 0.0402 0.2765 0.0450 Uiso calc C120 0.3432(8) 0.1371(7) 0.3721(5) 0.026(3) Uani ? H12A 0.4416 0.1411 0.3537 0.0350 Uiso calc H12B 0.2919 0.1972 0.3942 0.0350 Uiso calc C121 0.3493(8) 0.0289(7) 0.4362(5) 0.027(3) Uani ? C122 0.4558(9) -0.0691(8) 0.4327(6) 0.039(4) Uani ? H122 0.5281 -0.0688 0.3906 0.0500 Uiso calc C123 0.4562(10) -0.1650(9) 0.4895(6) 0.049(4) Uani ? H123 0.5253 -0.2304 0.4848 0.0630 Uiso calc C124 0.3533(10) -0.1662(9) 0.5552(6) 0.050(4) Uani ? H124 0.3549 -0.2322 0.5943 0.0650 Uiso calc C125 0.2514(10) -0.0719(9) 0.5621(5) 0.043(4) Uani ? H125 0.1841 -0.0726 0.6063 0.0560 Uiso calc C126 0.2478(9) 0.0264(8) 0.5026(5) 0.034(3) Uani ? H126 0.1770 0.0911 0.5072 0.0430 Uiso calc C130 0.1062(8) 0.0944(7) 0.3256(5) 0.026(3) Uani ? H13A 0.0781 0.0910 0.3799 0.0340 Uiso calc H13B 0.0235 0.1434 0.2981 0.0340 Uiso calc C131 0.1333(8) -0.0192(7) 0.3195(5) 0.024(3) Uani ? C132 0.1309(10) -0.0356(7) 0.2497(5) 0.035(4) Uani ? H132 0.1181 0.0240 0.2047 0.0460 Uiso calc C133 0.1473(11) -0.1380(8) 0.2466(5) 0.042(4) Uani ? H133 0.1411 -0.1470 0.2000 0.0540 Uiso calc C134 0.1730(11) -0.2287(8) 0.3116(6) 0.047(4) Uani ? H134 0.1882 -0.2989 0.3086 0.0610 Uiso calc C135 0.1758(11) -0.2139(8) 0.3806(6) 0.044(4) Uani ? H135 0.1907 -0.2745 0.4248 0.0570 Uiso calc C136 0.1569(9) -0.1105(8) 0.3860(5) 0.035(4) Uani ? H136 0.1600 -0.1019 0.4333 0.0460 Uiso calc C210 0.0165(8) 0.6819(6) 0.1685(5) 0.024(3) Uani ? H21A 0.0167 0.7010 0.2143 0.0310 Uiso calc H21B 0.1161 0.6450 0.1521 0.0310 Uiso calc C211 -0.0371(8) 0.7862(6) 0.1049(5) 0.022(3) Uani ? C212 -0.1393(8) 0.8794(6) 0.1211(5) 0.026(3) Uani ? H212 -0.1694 0.8796 0.1725 0.0330 Uiso calc C213 -0.1970(8) 0.9728(7) 0.0609(5) 0.029(3) Uani ? H213 -0.2682 1.0332 0.0725 0.0380 Uiso calc C214 -0.1493(8) 0.9751(7) -0.0140(5) 0.027(3) Uani ? H214 -0.1878 1.0373 -0.0538 0.0350 Uiso calc C215 -0.0444(8) 0.8864(7) -0.0318(5) 0.027(3) Uani ? H215 -0.0115 0.8892 -0.0835 0.0350 Uiso calc C216 0.0138(8) 0.7905(7) 0.0284(4) 0.022(3) Uani ? H216 0.0859 0.7309 0.0163 0.0290 Uiso calc C220 -0.1411(8) 0.5821(7) 0.1063(4) 0.023(3) Uani ? H22A -0.0828 0.6173 0.0617 0.0300 Uiso calc H22B -0.1179 0.5060 0.1075 0.0300 Uiso calc C221 -0.3015(8) 0.6394(6) 0.0957(4) 0.021(3) Uani ? C222 -0.3976(9) 0.5733(7) 0.1170(5) 0.028(3) Uani ? H222 -0.3631 0.4969 0.1361 0.0360 Uiso calc C223 -0.5426(9) 0.6252(8) 0.1087(5) 0.034(3) Uani ? H223 -0.6058 0.5826 0.1234 0.0440 Uiso calc C224 -0.5973(9) 0.7379(7) 0.0795(5) 0.034(3) Uani ? H224 -0.6953 0.7712 0.0735 0.0440 Uiso calc C225 -0.5008(9) 0.8006(8) 0.0591(6) 0.039(4) Uani ? H225 -0.5357 0.8770 0.0405 0.0500 Uiso calc C226 -0.3563(9) 0.7517(7) 0.0659(5) 0.031(3) Uani ? H226 -0.2938 0.7951 0.0501 0.0410 Uiso calc C230 -0.2596(8) 0.6517(7) 0.2473(5) 0.027(3) Uani ? H23A -0.2925 0.7293 0.2187 0.0350 Uiso calc H23B -0.3339 0.6188 0.2499 0.0350 Uiso calc C231 -0.2391(8) 0.6400(7) 0.3297(5) 0.028(3) Uani ? C232 -0.1863(10) 0.7104(9) 0.3466(5) 0.041(4) Uani ? H232 -0.1699 0.7718 0.3072 0.0530 Uiso calc C233 -0.1580(11) 0.6919(12) 0.4196(7) 0.061(6) Uani ? H233 -0.1224 0.7410 0.4287 0.0790 Uiso calc C234 -0.1797(12) 0.6045(11) 0.4793(7) 0.062(5) Uani ? H234 -0.1546 0.5904 0.5282 0.0800 Uiso calc C235 -0.2417(14) 0.5360(9) 0.4645(6) 0.064(5) Uani ? H235 -0.2655 0.4787 0.5054 0.0840 Uiso calc C236 -0.2677(11) 0.5521(8) 0.3912(5) 0.042(4) Uani ? H236 -0.3049 0.5038 0.3823 0.0540 Uiso calc loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Re1 0.01950(17) 0.01946(18) 0.02022(18) -0.00642(13) -0.00272(13) -0.00668(13) Re2 0.02034(17) 0.01879(18) 0.01851(18) -0.00506(13) -0.00295(13) -0.00469(13) Cl11 0.0314(11) 0.0292(11) 0.0279(11) -0.0114(9) -0.0078(9) -0.0114(9) Cl12 0.0250(10) 0.0268(11) 0.0238(10) -0.0080(8) -0.0007(8) -0.0061(8) Cl21 0.0221(9) 0.0277(11) 0.0288(11) -0.0109(8) -0.0040(8) -0.0051(9) Cl22 0.0350(11) 0.0287(11) 0.0194(10) -0.0061(9) -0.0003(8) -0.0036(8) P1 0.0185(10) 0.0189(11) 0.0264(11) -0.0042(8) -0.0032(9) -0.0079(9) P2 0.0197(10) 0.0184(10) 0.0193(10) -0.0055(8) -0.0051(8) -0.0049(8) O1 0.023(3) 0.026(3) 0.027(3) -0.008(2) -0.007(2) -0.011(3) O2 0.025(3) 0.026(3) 0.028(3) -0.007(2) -0.012(3) -0.007(3) C1 0.024(4) 0.020(4) 0.023(4) -0.007(3) -0.005(3) -0.005(3) C2 0.048(6) 0.042(6) 0.040(6) -0.012(5) -0.011(5) -0.018(5) C110 0.024(4) 0.022(4) 0.034(5) -0.002(3) 0.000(4) -0.018(4) C111 0.017(4) 0.028(5) 0.034(5) -0.002(3) 0.002(3) -0.021(4) C112 0.023(4) 0.033(5) 0.025(4) -0.003(4) -0.002(3) -0.013(4) C113 0.033(5) 0.038(5) 0.025(5) -0.013(4) 0.010(4) -0.012(4) C114 0.028(5) 0.051(6) 0.042(6) -0.021(4) 0.009(4) -0.026(5) C115 0.032(5) 0.074(8) 0.033(5) -0.027(5) 0.011(4) -0.023(5) C116 0.032(5) 0.044(6) 0.025(5) -0.012(4) -0.007(4) -0.003(4) C120 0.021(4) 0.031(5) 0.027(4) -0.008(4) 0.001(3) -0.011(4) C121 0.022(4) 0.027(5) 0.029(5) -0.009(3) -0.003(4) -0.003(4) C122 0.027(5) 0.045(6) 0.038(5) -0.010(4) -0.008(4) -0.002(5) C123 0.031(5) 0.043(6) 0.056(7) -0.007(4) -0.015(5) 0.008(5) C124 0.035(5) 0.046(6) 0.053(7) -0.016(5) -0.025(5) 0.021(5) C125 0.040(6) 0.061(7) 0.026(5) -0.026(5) -0.015(4) 0.008(5) C126 0.031(5) 0.037(5) 0.025(5) -0.007(4) -0.002(4) -0.004(4) C130 0.023(4) 0.027(5) 0.029(5) -0.012(4) 0.001(4) -0.006(4) C131 0.023(4) 0.023(4) 0.030(5) -0.011(3) 0.001(3) -0.010(4) C132 0.046(6) 0.028(5) 0.035(5) -0.019(4) -0.007(4) -0.006(4) C133 0.063(6) 0.047(6) 0.028(5) -0.031(5) 0.001(5) -0.016(5) C134 0.052(6) 0.036(6) 0.060(7) -0.012(5) -0.005(5) -0.024(5) C135 0.061(7) 0.020(5) 0.042(6) -0.006(5) -0.011(5) -0.001(4) C136 0.041(5) 0.042(6) 0.030(5) -0.023(4) -0.003(4) -0.009(4) C210 0.021(4) 0.028(5) 0.024(4) -0.006(3) -0.004(3) -0.011(4) C211 0.019(4) 0.018(4) 0.029(4) -0.003(3) -0.008(3) -0.007(3) C212 0.026(4) 0.024(4) 0.026(4) -0.011(4) 0.001(4) -0.005(4) C213 0.022(4) 0.019(4) 0.042(5) -0.001(3) -0.005(4) -0.008(4) C214 0.024(4) 0.021(4) 0.030(5) -0.008(3) -0.011(4) 0.004(4) C215 0.030(4) 0.030(5) 0.023(4) -0.015(4) -0.003(4) -0.005(4) C216 0.020(4) 0.022(4) 0.026(4) -0.010(3) 0.001(3) -0.008(3) C220 0.021(4) 0.027(4) 0.022(4) -0.009(3) -0.003(3) -0.006(3) C221 0.017(4) 0.025(4) 0.021(4) -0.004(3) -0.009(3) -0.006(3) C222 0.034(5) 0.023(4) 0.031(5) -0.014(4) -0.010(4) -0.005(4) C223 0.022(4) 0.044(6) 0.038(5) -0.018(4) -0.001(4) -0.009(4) C224 0.019(4) 0.029(5) 0.043(5) 0.003(4) -0.014(4) -0.002(4) C225 0.026(5) 0.029(5) 0.060(6) -0.001(4) -0.022(5) -0.009(5) C226 0.025(4) 0.032(5) 0.036(5) -0.013(4) -0.010(4) -0.002(4) C230 0.026(4) 0.019(4) 0.030(5) -0.004(3) 0.001(4) -0.006(4) C231 0.019(4) 0.033(5) 0.019(4) 0.002(4) 0.001(3) -0.005(4) C232 0.043(6) 0.059(7) 0.031(5) -0.028(5) 0.008(4) -0.021(5) C233 0.056(7) 0.104(10) 0.053(7) -0.046(7) 0.018(6) -0.051(8) C234 0.058(7) 0.067(8) 0.040(7) 0.018(6) -0.011(6) -0.025(6) C235 0.112(10) 0.035(6) 0.023(5) 0.002(7) 0.001(6) -0.011(5) C236 0.063(7) 0.025(5) 0.037(6) -0.006(5) -0.008(5) -0.015(4) # 10. MOLECULAR GEOMETRY _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_publ_flag Re(1) O(1) 2.076(5) ? Re(1) Re(2) 2.2166(4) ? Re(1) Cl(11) 2.3462(18) ? Re(1) Cl(12) 2.3730(19) ? Re(1) P(1) 2.428(2) ? Re(2) O(2) 2.106(5) ? Re(2) Cl(21) 2.3508(18) ? Re(2) Cl(22) 2.3666(19) ? Re(2) P(2) 2.4036(19) ? P(1) C(120) 1.828(8) ? P(1) C(110) 1.841(8) ? P(1) C(130) 1.848(7) ? P(2) C(230) 1.834(8) ? P(2) C(210) 1.835(8) ? P(2) C(220) 1.841(8) ? O(1) C(1) 1.269(9) ? O(2) C(1) 1.274(9) ? C(1) C(2) 1.457(11) ? C(110) C(111) 1.511(11) ? C(111) C(112) 1.385(11) ? C(111) C(116) 1.414(11) ? C(112) C(113) 1.382(11) ? C(113) C(114) 1.377(12) ? C(114) C(115) 1.412(13) ? C(115) C(116) 1.382(12) ? C(120) C(121) 1.520(11) ? C(121) C(122) 1.390(12) ? C(121) C(126) 1.399(11) ? C(122) C(123) 1.355(13) ? C(123) C(124) 1.396(14) ? C(124) C(125) 1.351(14) ? C(125) C(126) 1.394(12) ? C(130) C(131) 1.509(11) ? C(131) C(132) 1.391(12) ? C(131) C(136) 1.400(11) ? C(132) C(133) 1.362(12) ? C(133) C(134) 1.381(13) ? C(134) C(135) 1.366(13) ? C(135) C(136) 1.385(13) ? C(210) C(211) 1.502(10) ? C(211) C(216) 1.379(11) ? C(211) C(212) 1.395(11) ? C(212) C(213) 1.401(11) ? C(213) C(214) 1.351(12) ? C(214) C(215) 1.373(11) ? C(215) C(216) 1.419(11) ? C(220) C(221) 1.528(10) ? C(221) C(226) 1.374(11) ? C(221) C(222) 1.428(10) ? C(222) C(223) 1.377(11) ? C(223) C(224) 1.377(12) ? C(224) C(225) 1.399(12) ? C(225) C(226) 1.364(11) ? C(230) C(231) 1.530(11) ? C(231) C(232) 1.383(12) ? C(231) C(236) 1.390(12) ? C(232) C(233) 1.359(14) ? C(233) C(234) 1.349(16) ? C(234) C(235) 1.402(17) ? C(235) C(236) 1.365(13) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag O(1) Re(1) Re(2) 90.61(15) ? O(1) Re(1) Cl(11) 162.80(16) ? Re(2) Re(1) Cl(11) 106.53(5) ? O(1) Re(1) Cl(12) 86.87(15) ? Re(2) Re(1) Cl(12) 114.60(5) ? Cl(11) Re(1) Cl(12) 87.21(7) ? O(1) Re(1) P(1) 91.77(15) ? Re(2) Re(1) P(1) 94.57(5) ? Cl(11) Re(1) P(1) 85.58(7) ? Cl(12) Re(1) P(1) 150.80(7) ? O(2) Re(2) Re(1) 89.70(16) ? O(2) Re(2) Cl(21) 165.74(16) ? Re(1) Re(2) Cl(21) 104.54(5) ? O(2) Re(2) Cl(22) 84.91(16) ? Re(1) Re(2) Cl(22) 117.28(5) ? Cl(21) Re(2) Cl(22) 87.79(7) ? O(2) Re(2) P(2) 94.41(15) ? Re(1) Re(2) P(2) 96.12(5) ? Cl(21) Re(2) P(2) 84.97(7) ? Cl(22) Re(2) P(2) 146.56(7) ? C(120) P(1) C(110) 104.3(4) ? C(120) P(1) C(130) 107.5(4) ? C(110) P(1) C(130) 108.0(4) ? C(120) P(1) Re(1) 116.4(3) ? C(110) P(1) Re(1) 105.3(3) ? C(130) P(1) Re(1) 114.6(3) ? C(230) P(2) C(210) 103.6(4) ? C(230) P(2) C(220) 106.2(4) ? C(210) P(2) C(220) 109.0(4) ? C(230) P(2) Re(2) 105.7(3) ? C(210) P(2) Re(2) 114.8(2) ? C(220) P(2) Re(2) 116.4(3) ? C(1) O(1) Re(1) 118.7(5) ? C(1) O(2) Re(2) 117.9(5) ? O(1) C(1) O(2) 122.8(7) ? O(1) C(1) C(2) 116.8(7) ? O(2) C(1) C(2) 120.4(8) ? C(111) C(110) P(1) 109.0(5) ? C(112) C(111) C(116) 117.4(8) ? C(112) C(111) C(110) 120.8(7) ? C(116) C(111) C(110) 121.4(8) ? C(113) C(112) C(111) 122.3(8) ? C(114) C(113) C(112) 119.2(8) ? C(113) C(114) C(115) 121.1(8) ? C(116) C(115) C(114) 118.2(9) ? C(115) C(116) C(111) 121.7(9) ? C(121) C(120) P(1) 115.4(6) ? C(122) C(121) C(126) 117.7(8) ? C(122) C(121) C(120) 122.4(8) ? C(126) C(121) C(120) 119.8(8) ? C(123) C(122) C(121) 121.1(9) ? C(122) C(123) C(124) 120.3(10) ? C(125) C(124) C(123) 120.3(9) ? C(124) C(125) C(126) 119.6(9) ? C(125) C(126) C(121) 120.8(9) ? C(131) C(130) P(1) 118.1(6) ? C(132) C(131) C(136) 118.7(8) ? C(132) C(131) C(130) 121.7(7) ? C(136) C(131) C(130) 119.6(8) ? C(133) C(132) C(131) 120.6(8) ? C(132) C(133) C(134) 120.9(9) ? C(135) C(134) C(133) 119.0(9) ? C(134) C(135) C(136) 121.5(9) ? C(135) C(136) C(131) 119.2(8) ? C(211) C(210) P(2) 114.6(5) ? C(216) C(211) C(212) 118.6(7) ? C(216) C(211) C(210) 119.7(7) ? C(212) C(211) C(210) 121.7(7) ? C(211) C(212) C(213) 120.8(8) ? C(214) C(213) C(212) 120.0(8) ? C(213) C(214) C(215) 120.5(8) ? C(214) C(215) C(216) 120.3(8) ? C(211) C(216) C(215) 119.6(8) ? C(221) C(220) P(2) 113.9(5) ? C(226) C(221) C(222) 118.9(7) ? C(226) C(221) C(220) 122.5(7) ? C(222) C(221) C(220) 118.6(7) ? C(223) C(222) C(221) 118.5(8) ? C(222) C(223) C(224) 122.4(8) ? C(223) C(224) C(225) 117.9(8) ? C(226) C(225) C(224) 121.2(8) ? C(225) C(226) C(221) 121.1(8) ? C(231) C(230) P(2) 111.7(5) ? C(232) C(231) C(236) 117.1(8) ? C(232) C(231) C(230) 123.2(8) ? C(236) C(231) C(230) 119.6(8) ? C(233) C(232) C(231) 121.4(10) ? C(234) C(233) C(232) 122.2(11) ? C(233) C(234) C(235) 117.3(10) ? C(236) C(235) C(234) 121.0(11) ? C(235) C(236) C(231) 120.7(10) ? #===END data_J0403B # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description chunk _exptl_crystal_colour 'olive green' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.39 _exptl_crystal_size_min 0.35 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C36 H66 Cl3 O P2 Re' _chemical_formula_structural ? _chemical_formula_weight 869.43 _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 9.9534(5) _cell_length_b 10.2535(5) _cell_length_c 10.9010(5) _cell_angle_alpha 114.311(3) _cell_angle_beta 107.608(3) _cell_angle_gamma 93.089(3) _cell_volume 945.76(19) _cell_measurement_reflns_used 7186 _cell_measurement_theta_min 4 _cell_measurement_theta_max 27 _cell_formula_units_z 1 _exptl_crystal_density_diffrn 1.53 _exptl_crystal_density_meas ? _diffrn_radiation_type MO-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 3.579 _cell_measurement_temperature 193 _exptl_crystal_F_000 446 # 6. DATA COLLECTION _diffrn_ambient_temperature 193 _diffrn_measurement_device_type ? _exptl_absorpt_correction_type refined_empirical_(Otwinowski_&_Minor,_1996 _exptl_absorpt_correction_T_min 0.1950 _exptl_absorpt_correction_T_max 0.2857 _diffrn_reflns_number 7186 _reflns_number_total 0 _reflns_number_gt 0 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.069 _diffrn_reflns_theta_min 4.00 _diffrn_reflns_theta_max 27.49 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_max 14 # 7. REFINEMENT DATA _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R_factor_obs 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_R_factor_gt 0.043 _refine_ls_wR_factor_ref 0.114 _refine_ls_hydrogen_treatment H_atoms_riding _refine_ls_number_reflns 3917 _refine_ls_number_parameters 201 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 1.102 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+5.9456P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.001 _refine_diff_density_max 1.91 _refine_diff_density_min -2.09 _refine_ls_extinction_method SHELXL97_(Sheldrick_1997) _refine_ls_extinction_coef 0.21E-01 _atom_type_scat_source 'International Tables for Crystallography (Vol C)' # 8. COMPUTING DATA _computing_data_collection Collect_(Nonius,_1998) _computing_cell_refinement DENZO/SCALEPACK_(Otwinowski,_1996) _computing_data_reduction DENZO/SCALEPACK_(Otwinowski,_1996) _computing_structure_solution PATTY_(DIRDIF92,_Beurskins,_1992) _computing_structure_refinement SHELX97_(Sheldrick,_1997) _computing_molecular_graphics ; ORTEP (Johnson, 1976) Xtal_GX (Hall, 1995) PLUTON (Spek, 1991) ; _computing_publication_material CIF_VAX_MolEN_(Fair,_1990) # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag Re 0.0000 0.0000 0.0000 0.02721(13) Uani ? Cl(1) 0.0127(4) 0.2461(4) 0.1123(4) 0.0407(13) Uani ? Cl(2) 0.15951(18) 0.0413(2) -0.11097(17) 0.0407(6) Uani ? P(1) 0.21152(17) 0.03149(15) 0.21685(15) 0.0254(4) Uani ? O(1) 0.0092(16) 0.1832(16) 0.0826(15) 0.056(4) Uiso ? C(11) 0.3791(7) 0.1398(6) 0.2388(6) 0.028(2) Uani ? C(12) 0.3776(8) 0.3017(8) 0.2790(10) 0.046(3) Uani ? C(13) 0.5046(9) 0.3732(9) 0.2619(12) 0.061(4) Uani ? C(14) 0.6471(8) 0.3557(9) 0.3494(10) 0.051(3) Uani ? C(15) 0.6469(8) 0.1990(9) 0.3147(9) 0.048(3) Uani ? C(16) 0.5205(8) 0.1286(8) 0.3327(8) 0.042(3) Uani ? C(21) 0.1719(7) 0.1060(7) 0.3865(6) 0.0288(18) Uani ? C(22) 0.1175(9) 0.2474(8) 0.4237(8) 0.045(3) Uani ? C(23) 0.0677(8) 0.2828(9) 0.5517(7) 0.047(3) Uani ? C(24) 0.1841(9) 0.2884(9) 0.6823(8) 0.048(3) Uani ? C(25) 0.2401(9) 0.1483(9) 0.6434(7) 0.044(3) Uani ? C(26) 0.2930(8) 0.1148(8) 0.5190(6) 0.035(2) Uani ? C(31) 0.2626(7) -0.1443(6) 0.2029(6) 0.030(2) Uani ? C(32) 0.1478(8) -0.2462(7) 0.2063(8) 0.037(2) Uani ? C(33) 0.1945(9) -0.3860(8) 0.2011(8) 0.044(3) Uani ? C(34) 0.2368(9) -0.4629(7) 0.0693(8) 0.042(3) Uani ? C(35) 0.3570(9) -0.3641(8) 0.0717(9) 0.045(3) Uani ? C(36) 0.3139(8) -0.2216(7) 0.0761(8) 0.039(3) Uani ? H(11) 0.3840 0.0991 0.1421 0.0370 Uiso calc H(21) 0.0914 0.0333 0.3691 0.0370 Uiso calc H(31) 0.3463 -0.1186 0.2902 0.0390 Uiso calc H(12A) 0.2883 0.3099 0.2176 0.0600 Uiso calc H(12B) 0.3825 0.3522 0.3780 0.0600 Uiso calc H(13A) 0.4940 0.3293 0.1610 0.0790 Uiso calc H(13B) 0.5044 0.4764 0.2929 0.0790 Uiso calc H(14A) 0.7245 0.3941 0.3290 0.0670 Uiso calc H(14B) 0.6644 0.4115 0.4513 0.0670 Uiso calc H(15A) 0.7361 0.1919 0.3774 0.0620 Uiso calc H(15B) 0.6426 0.1459 0.2161 0.0620 Uiso calc H(16A) 0.5231 0.0265 0.3069 0.0550 Uiso calc H(16B) 0.5284 0.1767 0.4328 0.0550 Uiso calc H(22A) 0.0378 0.2384 0.3410 0.0590 Uiso calc H(22B) 0.1938 0.3264 0.4476 0.0590 Uiso calc H(23A) 0.0388 0.3765 0.5775 0.0610 Uiso calc H(23B) -0.0158 0.2092 0.5232 0.0610 Uiso calc H(24A) 0.2627 0.3704 0.7191 0.0610 Uiso calc H(24B) 0.1452 0.3029 0.7574 0.0610 Uiso calc H(25A) 0.1640 0.0681 0.6173 0.0580 Uiso calc H(25B) 0.3186 0.1567 0.7267 0.0580 Uiso calc H(26A) 0.3247 0.0225 0.4945 0.0460 Uiso calc H(26B) 0.3745 0.1907 0.5475 0.0460 Uiso calc H(32A) 0.1270 -0.1959 0.2936 0.0490 Uiso calc H(32B) 0.0599 -0.2704 0.1248 0.0490 Uiso calc H(33A) 0.1163 -0.4503 0.1969 0.0580 Uiso calc H(33B) 0.2759 -0.3634 0.2879 0.0580 Uiso calc H(34A) 0.2678 -0.5514 0.0680 0.0550 Uiso calc H(34B) 0.1537 -0.4905 -0.0176 0.0550 Uiso calc H(35A) 0.3811 -0.4146 -0.0135 0.0590 Uiso calc H(35B) 0.4419 -0.3417 0.1555 0.0590 Uiso calc H(36A) 0.2373 -0.2427 -0.0136 0.0500 Uiso calc H(36B) 0.3958 -0.1573 0.0859 0.0500 Uiso calc loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Re 0.0244(2) 0.0358(2) 0.02006(18) 0.00724(14) 0.00623(12) 0.01237(14) Cl(1) 0.0389(19) 0.0363(18) 0.0359(17) 0.0045(15) -0.0006(13) 0.0163(15) Cl(2) 0.0307(8) 0.0655(11) 0.0309(7) 0.0058(8) 0.0118(6) 0.0263(8) P(1) 0.0263(7) 0.0242(6) 0.0215(6) 0.0044(6) 0.0057(5) 0.0085(5) C(11) 0.030(3) 0.027(3) 0.024(3) 0.004(2) 0.008(2) 0.010(2) C(12) 0.038(4) 0.035(3) 0.077(5) 0.011(3) 0.023(4) 0.033(4) C(13) 0.040(5) 0.050(4) 0.108(8) 0.009(4) 0.025(5) 0.051(5) C(14) 0.030(4) 0.045(4) 0.071(5) 0.000(3) 0.017(4) 0.020(4) C(15) 0.026(3) 0.052(4) 0.058(4) 0.005(3) 0.008(3) 0.024(4) C(16) 0.030(4) 0.043(4) 0.051(4) 0.006(3) 0.008(3) 0.023(3) C(21) 0.027(3) 0.033(3) 0.017(2) 0.006(2) 0.003(2) 0.006(2) C(22) 0.047(4) 0.041(4) 0.037(3) 0.017(3) 0.013(3) 0.009(3) C(23) 0.043(4) 0.053(4) 0.029(3) 0.012(4) 0.016(3) 0.002(3) C(24) 0.044(4) 0.052(4) 0.034(3) -0.001(3) 0.018(3) 0.006(3) C(25) 0.054(5) 0.056(4) 0.021(3) 0.008(4) 0.010(3) 0.018(3) C(26) 0.042(4) 0.049(4) 0.017(2) 0.016(3) 0.008(2) 0.019(3) C(31) 0.030(3) 0.029(3) 0.026(3) 0.008(2) 0.007(2) 0.010(2) C(32) 0.044(4) 0.031(3) 0.038(3) 0.004(3) 0.020(3) 0.013(3) C(33) 0.050(5) 0.039(4) 0.046(4) 0.011(3) 0.012(3) 0.024(3) C(34) 0.056(5) 0.025(3) 0.041(4) 0.006(3) 0.011(3) 0.015(3) C(35) 0.048(4) 0.033(3) 0.051(4) 0.015(3) 0.021(3) 0.012(3) C(36) 0.049(4) 0.029(3) 0.042(4) 0.009(3) 0.025(3) 0.013(3) # 10. MOLECULAR GEOMETRY _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_publ_flag Re O(1) 1.699(14) ? Re O(1) 1.699(14) ? Re Cl(1) 2.282(4) ? Re Cl(1) 2.282(4) ? Re Cl(2) 2.3822(16) ? Re Cl(2) 2.3822(16) ? Re P(1) 2.5322(14) ? Re P(1) 2.5322(14) ? P(1) C(11) 1.847(7) ? P(1) C(31) 1.858(6) ? P(1) C(21) 1.863(6) ? C(11) C(16) 1.512(9) ? C(11) C(12) 1.534(8) ? C(12) C(13) 1.525(12) ? C(13) C(14) 1.518(11) ? C(14) C(15) 1.492(11) ? C(15) C(16) 1.519(11) ? C(21) C(22) 1.515(8) ? C(21) C(26) 1.541(7) ? C(22) C(23) 1.531(10) ? C(23) C(24) 1.517(10) ? C(24) C(25) 1.510(10) ? C(25) C(26) 1.517(9) ? C(31) C(32) 1.525(10) ? C(31) C(36) 1.539(8) ? C(32) C(33) 1.515(9) ? C(33) C(34) 1.527(10) ? C(34) C(35) 1.513(11) ? C(35) C(36) 1.531(9) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag O(1) Re O(1) 179.9990(10) ? O(1) Re Cl(1) 0.4(5) ? O(1) Re Cl(1) 179.6(5) ? O(1) Re Cl(1) 179.6(5) ? O(1) Re Cl(1) 0.4(5) ? Cl(1) Re Cl(1) 180.0(5) ? O(1) Re Cl(2) 91.0(5) ? O(1) Re Cl(2) 89.0(5) ? Cl(1) Re Cl(2) 90.76(12) ? Cl(1) Re Cl(2) 89.24(12) ? O(1) Re Cl(2) 89.0(5) ? O(1) Re Cl(2) 91.0(5) ? Cl(1) Re Cl(2) 89.24(12) ? Cl(1) Re Cl(2) 90.76(12) ? Cl(2) Re Cl(2) 180.00(5) ? O(1) Re P(1) 91.7(5) ? O(1) Re P(1) 88.3(5) ? Cl(1) Re P(1) 91.97(9) ? Cl(1) Re P(1) 88.03(9) ? Cl(2) Re P(1) 90.68(5) ? Cl(2) Re P(1) 89.32(5) ? O(1) Re P(1) 88.3(5) ? O(1) Re P(1) 91.7(5) ? Cl(1) Re P(1) 88.03(9) ? Cl(1) Re P(1) 91.97(9) ? Cl(2) Re P(1) 89.31(5) ? Cl(2) Re P(1) 90.69(5) ? P(1) Re P(1) 180.00(5) ? C(11) P(1) C(31) 103.0(3) ? C(11) P(1) C(21) 111.1(3) ? C(31) P(1) C(21) 103.3(3) ? C(11) P(1) Re 112.94(19) ? C(31) P(1) Re 112.9(2) ? C(21) P(1) Re 112.74(19) ? C(16) C(11) C(12) 108.8(6) ? C(16) C(11) P(1) 118.1(5) ? C(12) C(11) P(1) 114.9(4) ? C(13) C(12) C(11) 110.8(6) ? C(14) C(13) C(12) 111.6(7) ? C(15) C(14) C(13) 111.1(7) ? C(14) C(15) C(16) 112.1(6) ? C(11) C(16) C(15) 111.0(6) ? C(22) C(21) C(26) 110.5(5) ? C(22) C(21) P(1) 116.2(5) ? C(26) C(21) P(1) 114.5(4) ? C(21) C(22) C(23) 110.3(6) ? C(24) C(23) C(22) 112.5(6) ? C(25) C(24) C(23) 110.7(6) ? C(24) C(25) C(26) 111.7(6) ? C(25) C(26) C(21) 110.4(5) ? C(32) C(31) C(36) 112.4(5) ? C(32) C(31) P(1) 113.2(4) ? C(36) C(31) P(1) 113.3(5) ? C(33) C(32) C(31) 112.2(6) ? C(32) C(33) C(34) 110.3(6) ? C(35) C(34) C(33) 110.8(6) ? C(34) C(35) C(36) 111.5(6) ? C(35) C(36) C(31) 110.9(6) ? #===END data_J4602X # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.06 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C55 H54 Cl7 O2 P4 Re' _chemical_formula_structural ? _chemical_formula_weight 1305.31 _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 9.4968(3) _cell_length_b 12.9135(5) _cell_length_c 24.8886(10) _cell_angle_alpha 97.9692(19) _cell_angle_beta 91.753(2) _cell_angle_gamma 110.195(2) _cell_volume 2826.8(4) _cell_measurement_reflns_used 19987 _cell_measurement_theta_min 4 _cell_measurement_theta_max 27 _cell_formula_units_z 2 _exptl_crystal_density_diffrn 1.53 _exptl_crystal_density_meas ? _diffrn_radiation_type MO-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 2.662 _cell_measurement_temperature 173 _exptl_crystal_F_000 1308 # 6. DATA COLLECTION _diffrn_ambient_temperature 173 _diffrn_measurement_device_type ? _exptl_absorpt_correction_type refined_empirical_(Otwinowski_&_Minor,_1996 _exptl_absorpt_correction_T_min 0.6945 _exptl_absorpt_correction_T_max 0.8467 _diffrn_reflns_number 19987 _reflns_number_total 11859 _reflns_number_gt 9756 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.066 _diffrn_reflns_theta_min 4.00 _diffrn_reflns_theta_max 27.87 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_max 32 # 7. REFINEMENT DATA _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R_factor_obs 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_R_factor_gt 0.061 _refine_ls_wR_factor_ref 0.123 _refine_ls_hydrogen_treatment H_atoms_riding _refine_ls_number_reflns 9285 _refine_ls_d_res_high 0.84 _refine_ls_number_parameters 625 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0191P)^2^+21.7174P] where P=(Fo^2^+2Fc^2^)/' _refine_ls_shift/su_max 0.007 _refine_diff_density_max 1.41 _refine_diff_density_min -1.48 _refine_ls_extinction_method none _atom_type_scat_source 'International Tables for Crystallography (Vol C) ' # 8. COMPUTING DATA _computing_data_collection Collect_(Nonius,_1998) _computing_cell_refinement DENZO/SCALEPACK_(Otwinowski,_1996) _computing_data_reduction DENZO/SCALEPACK_(Otwinowski,_1996) _computing_structure_solution Direct_methods_(Shelxs97,_Sheldrick,_1997) _computing_structure_refinement SHELX97_(Sheldrick,_1997) _computing_molecular_graphics ; ORTEP (Johnson, 1976) Xtal_GX (Hall, 1995) PLUTON (Spek, 1991) ; _computing_publication_material CIF_VAX_MolEN_(Fair,_1990) # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag Re(1) 0.5000 0.5000 0.0000 0.02220(14) Uani ? Re(2) 0.5000 0.5000 0.5000 0.03473(18) Uani ? Cl(1) 0.7988(3) 0.5952(2) 0.25748(9) 0.0466(8) Uani ? Cl(91) 0.8724(5) 0.9195(3) 0.3425(2) 0.127(2) Uani ? Cl(92) 0.5894(6) 0.8825(5) 0.2824(2) 0.145(3) Uani ? Cl(93) 1.2352(7) 0.9648(4) 0.2624(2) 0.155(3) Uani ? Cl(94) 1.0310(6) 0.8440(3) 0.17060(18) 0.139(2) Uani ? Cl(95) 0.1252(6) 0.7047(3) 0.8210(2) 0.122(2) Uani ? Cl(96) 0.3715(9) 0.8119(6) 0.7619(2) 0.193(4) Uani ? P(1) 0.5604(2) 0.62468(16) 0.08896(8) 0.0260(6) Uani ? P(2) 0.5582(2) 0.37706(16) 0.05898(8) 0.0251(6) Uani ? P(3) 0.5256(3) 0.6540(2) 0.44747(10) 0.0409(8) Uani ? P(4) 0.5829(3) 0.4282(2) 0.41435(10) 0.0438(9) Uani ? O(1) 0.6975(6) 0.5511(4) -0.0055(2) 0.0281(17) Uani ? O(2) 0.7095(8) 0.5732(5) 0.5201(2) 0.059(2) Uani ? C(11) 0.7124(8) 0.5920(6) 0.1202(3) 0.029(3) Uani ? C(21) 0.6649(10) 0.4659(6) 0.1225(3) 0.033(3) Uani ? C(31) 0.6423(12) 0.6401(9) 0.3906(4) 0.052(4) Uani ? C(41) 0.7145(11) 0.5542(9) 0.3935(4) 0.055(4) Uani ? C(111) 0.4103(9) 0.6028(6) 0.1347(3) 0.031(3) Uani ? C(112) 0.2706(9) 0.5964(7) 0.1143(4) 0.039(3) Uani ? C(113) 0.1528(10) 0.5823(8) 0.1486(4) 0.049(3) Uani ? C(114) 0.1746(11) 0.5731(8) 0.2023(4) 0.050(4) Uani ? C(115) 0.3163(11) 0.5799(8) 0.2222(4) 0.048(3) Uani ? C(116) 0.4344(10) 0.5946(7) 0.1890(4) 0.040(3) Uani ? C(121) 0.6388(9) 0.7749(6) 0.0905(3) 0.030(3) Uani ? C(122) 0.7434(9) 0.8166(7) 0.0540(4) 0.037(3) Uani ? C(123) 0.7987(10) 0.9310(7) 0.0520(4) 0.045(3) Uani ? C(124) 0.7521(11) 1.0028(7) 0.0861(5) 0.052(4) Uani ? C(125) 0.6523(12) 0.9638(7) 0.1234(4) 0.051(4) Uani ? C(126) 0.5931(11) 0.8481(7) 0.1260(4) 0.043(3) Uani ? C(211) 0.4059(9) 0.2715(6) 0.0842(3) 0.029(2) Uani ? C(212) 0.2673(10) 0.2803(8) 0.0864(4) 0.043(3) Uani ? C(213) 0.1516(11) 0.2032(8) 0.1082(4) 0.053(4) Uani ? C(214) 0.1760(12) 0.1166(8) 0.1288(4) 0.054(4) Uani ? C(215) 0.3148(12) 0.1075(8) 0.1277(4) 0.052(4) Uani ? C(216) 0.4301(11) 0.1823(7) 0.1060(4) 0.043(3) Uani ? C(221) 0.6817(9) 0.3081(7) 0.0286(3) 0.029(2) Uani ? C(222) 0.6222(10) 0.2005(7) -0.0007(3) 0.037(3) Uani ? C(223) 0.7176(11) 0.1518(8) -0.0264(4) 0.047(3) Uani ? C(224) 0.8701(11) 0.2100(8) -0.0240(4) 0.048(4) Uani ? C(225) 0.9295(10) 0.3180(8) 0.0048(4) 0.045(3) Uani ? C(226) 0.8357(9) 0.3665(7) 0.0310(4) 0.036(3) Uani ? C(311) 0.3622(11) 0.6637(8) 0.4131(4) 0.050(4) Uani ? C(312) 0.2310(13) 0.5730(10) 0.3983(5) 0.070(5) Uani ? C(313) 0.1115(15) 0.5790(13) 0.3677(5) 0.080(5) Uani ? C(314) 0.1189(18) 0.6712(15) 0.3499(6) 0.095(7) Uani ? C(315) 0.2517(18) 0.7640(15) 0.3597(6) 0.098(7) Uani ? C(316) 0.3707(16) 0.7595(12) 0.3910(5) 0.089(6) Uani ? C(321) 0.6226(13) 0.7898(8) 0.4866(4) 0.052(4) Uani ? C(322) 0.5456(16) 0.8496(11) 0.5132(6) 0.083(5) Uani ? C(323) 0.621(2) 0.9490(13) 0.5478(8) 0.118(8) Uani ? C(324) 0.774(2) 0.9887(14) 0.5571(7) 0.114(8) Uani ? C(325) 0.8508(17) 0.9283(12) 0.5344(6) 0.095(6) Uani ? C(326) 0.7767(16) 0.8271(10) 0.4978(5) 0.079(5) Uani ? C(411) 0.4423(12) 0.3598(9) 0.3576(4) 0.050(3) Uani ? C(412) 0.3096(13) 0.2800(9) 0.3686(5) 0.066(4) Uani ? C(413) 0.1987(15) 0.2233(11) 0.3269(5) 0.079(5) Uani ? C(414) 0.2186(14) 0.2496(10) 0.2758(5) 0.071(5) Uani ? C(415) 0.3499(15) 0.3276(10) 0.2639(5) 0.073(5) Uani ? C(416) 0.4640(13) 0.3842(9) 0.3056(4) 0.057(4) Uani ? C(421) 0.6968(14) 0.3405(10) 0.4165(4) 0.062(5) Uani ? C(422) 0.8203(15) 0.3757(12) 0.4542(6) 0.093(6) Uani ? C(423) 0.9119(19) 0.3140(16) 0.4578(8) 0.125(9) Uani ? C(424) 0.880(3) 0.218(2) 0.4218(8) 0.152(14) Uani ? C(425) 0.753(3) 0.1761(17) 0.3859(7) 0.146(10) Uani ? C(426) 0.664(2) 0.2430(15) 0.3824(6) 0.116(8) Uani ? C(910) 0.763(2) 0.8611(15) 0.2811(6) 0.117(9) Uani ? C(920) 1.1311(18) 0.8343(11) 0.2272(6) 0.100(6) Uani ? C(930) 0.204(3) 0.6913(15) 0.7567(9) 0.175(13) Uani ? H(112) 0.2542 0.6014 0.0778 0.0510 Uiso calc H(113) 0.0591 0.5793 0.1349 0.0630 Uiso calc H(114) 0.0961 0.5625 0.2249 0.0650 Uiso calc H(115) 0.3325 0.5745 0.2585 0.0630 Uiso calc H(116) 0.5285 0.5990 0.2030 0.0530 Uiso calc H(11A) 0.7997 0.6147 0.0994 0.0370 Uiso calc H(11B) 0.7405 0.6336 0.1568 0.0370 Uiso calc H(122) 0.7766 0.7684 0.0309 0.0480 Uiso calc H(123) 0.8679 0.9586 0.0272 0.0580 Uiso calc H(124) 0.7884 1.0787 0.0838 0.0680 Uiso calc H(125) 0.6233 1.0135 0.1472 0.0670 Uiso calc H(126) 0.5244 0.8212 0.1511 0.0560 Uiso calc H(212) 0.2500 0.3390 0.0730 0.0560 Uiso calc H(213) 0.0573 0.2100 0.1089 0.0680 Uiso calc H(214) 0.0985 0.0648 0.1434 0.0710 Uiso calc H(215) 0.3314 0.0494 0.1420 0.0680 Uiso calc H(216) 0.5241 0.1749 0.1055 0.0560 Uiso calc H(21A) 0.6032 0.4487 0.1527 0.0430 Uiso calc H(21B) 0.7543 0.4479 0.1293 0.0430 Uiso calc H(222) 0.5191 0.1611 -0.0031 0.0480 Uiso calc H(223) 0.6779 0.0793 -0.0454 0.0610 Uiso calc H(224) 0.9329 0.1773 -0.0416 0.0630 Uiso calc H(225) 1.0324 0.3577 0.0066 0.0580 Uiso calc H(226) 0.8760 0.4387 0.0503 0.0470 Uiso calc H(312) 0.2230 0.5054 0.4093 0.0910 Uiso calc H(313) 0.0241 0.5164 0.3596 0.1040 Uiso calc H(314) 0.0356 0.6749 0.3308 0.1230 Uiso calc H(315) 0.2598 0.8283 0.3451 0.1270 Uiso calc H(316) 0.4591 0.8216 0.3976 0.1150 Uiso calc H(31A) 0.5797 0.6206 0.3566 0.0680 Uiso calc H(31B) 0.7206 0.7119 0.3902 0.0680 Uiso calc H(322) 0.4411 0.8235 0.5081 0.1090 Uiso calc H(323) 0.5658 0.9893 0.5651 0.1540 Uiso calc H(324) 0.8244 1.0572 0.5789 0.1490 Uiso calc H(325) 0.9544 0.9522 0.5424 0.1220 Uiso calc H(326) 0.8321 0.7862 0.4816 0.1030 Uiso calc H(412) 0.2954 0.2647 0.4039 0.0850 Uiso calc H(413) 0.1112 0.1677 0.3337 0.1030 Uiso calc H(414) 0.1416 0.2140 0.2483 0.0930 Uiso calc H(415) 0.3626 0.3426 0.2286 0.0950 Uiso calc H(416) 0.5531 0.4374 0.2983 0.0740 Uiso calc H(41A) 0.8028 0.5850 0.4194 0.0720 Uiso calc H(41B) 0.7469 0.5349 0.3581 0.0720 Uiso calc H(422) 0.8420 0.4428 0.4778 0.1200 Uiso calc H(423) 0.9929 0.3371 0.4841 0.1630 Uiso calc H(424) 0.9471 0.1800 0.4213 0.1980 Uiso calc H(425) 0.7268 0.1059 0.3647 0.1910 Uiso calc H(426) 0.5818 0.2198 0.3565 0.1510 Uiso calc H(91A) 0.7442 0.7816 0.2741 0.1520 Uiso calc H(91B) 0.8168 0.8945 0.2518 0.1520 Uiso calc H(92A) 1.1980 0.7945 0.2161 0.1300 Uiso calc H(92B) 1.0621 0.7920 0.2509 0.1300 Uiso calc H(93A) 0.2272 0.6234 0.7505 0.2310 Uiso calc H(93B) 0.1342 0.6898 0.7270 0.2310 Uiso calc loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Re(1) 0.0214(2) 0.0157(2) 0.0265(3) 0.00262(19) 0.00165(19) 0.00382(18) Re(2) 0.0355(3) 0.0417(3) 0.0282(3) 0.0146(3) 0.0068(2) 0.0061(2) Cl(1) 0.0502(14) 0.0525(14) 0.0331(12) 0.0121(11) 0.0045(10) 0.0097(10) Cl(91) 0.122(4) 0.067(2) 0.171(5) 0.017(2) -0.027(3) 0.001(3) Cl(92) 0.131(4) 0.151(5) 0.118(4) 0.029(4) -0.005(3) -0.037(3) Cl(93) 0.202(6) 0.082(3) 0.145(4) 0.007(3) -0.052(4) 0.024(3) Cl(94) 0.185(5) 0.072(2) 0.096(3) -0.039(3) -0.029(3) 0.035(2) Cl(95) 0.144(4) 0.083(3) 0.159(4) 0.061(3) 0.053(3) 0.019(3) Cl(96) 0.236(8) 0.180(6) 0.124(4) 0.042(6) 0.059(5) -0.034(4) P(1) 0.0277(11) 0.0184(10) 0.0283(11) 0.0044(8) 0.0007(9) 0.0018(8) P(2) 0.0224(10) 0.0205(10) 0.0301(11) 0.0040(9) 0.0017(9) 0.0062(8) P(3) 0.0402(14) 0.0430(14) 0.0386(14) 0.0119(12) 0.0036(11) 0.0109(11) P(4) 0.0477(15) 0.0522(15) 0.0360(13) 0.0232(13) 0.0133(11) 0.0047(11) O(1) 0.038(3) 0.017(3) 0.025(3) 0.004(2) -0.002(2) 0.005(2) O(2) 0.090(5) 0.049(4) 0.018(3) -0.001(4) 0.014(3) 0.009(3) C(11) 0.025(4) 0.018(4) 0.040(5) 0.004(3) 0.004(4) 0.004(3) C(21) 0.044(5) 0.029(4) 0.026(4) 0.012(4) -0.003(4) 0.007(3) C(31) 0.058(6) 0.052(6) 0.046(6) 0.015(5) 0.011(5) 0.018(5) C(41) 0.049(6) 0.069(7) 0.037(6) 0.006(5) 0.016(5) 0.008(5) C(111) 0.030(4) 0.018(4) 0.035(5) -0.001(3) -0.002(4) 0.001(3) C(112) 0.033(5) 0.041(5) 0.039(5) 0.011(4) 0.004(4) 0.001(4) C(113) 0.030(5) 0.057(6) 0.056(6) 0.016(5) 0.006(4) -0.004(5) C(114) 0.043(6) 0.050(6) 0.051(6) 0.009(5) 0.016(5) 0.006(5) C(115) 0.055(6) 0.048(6) 0.040(5) 0.014(5) 0.015(5) 0.011(4) C(116) 0.040(5) 0.039(5) 0.043(5) 0.014(4) 0.008(4) 0.009(4) C(121) 0.031(4) 0.015(4) 0.039(5) 0.004(3) -0.007(4) 0.000(3) C(122) 0.029(4) 0.026(4) 0.049(5) 0.003(4) 0.003(4) 0.005(4) C(123) 0.032(5) 0.030(5) 0.063(6) -0.004(4) 0.008(4) 0.016(5) C(124) 0.050(6) 0.017(4) 0.083(8) 0.005(4) 0.001(6) 0.005(5) C(125) 0.066(7) 0.022(5) 0.062(7) 0.018(5) -0.002(5) -0.009(4) C(126) 0.048(6) 0.028(5) 0.046(6) 0.007(4) 0.004(4) 0.000(4) C(211) 0.032(4) 0.024(4) 0.026(4) 0.003(4) 0.008(3) 0.006(3) C(212) 0.039(5) 0.037(5) 0.052(6) 0.010(4) 0.011(4) 0.014(4) C(213) 0.035(5) 0.050(6) 0.067(7) 0.003(5) 0.020(5) 0.018(5) C(214) 0.056(7) 0.034(5) 0.051(6) -0.016(5) 0.021(5) 0.013(5) C(215) 0.058(7) 0.031(5) 0.067(7) 0.006(5) 0.024(5) 0.026(5) C(216) 0.047(5) 0.039(5) 0.047(6) 0.018(5) 0.009(4) 0.011(4) C(221) 0.027(4) 0.032(4) 0.031(4) 0.012(4) 0.003(3) 0.010(4) C(222) 0.042(5) 0.030(5) 0.041(5) 0.016(4) 0.006(4) 0.005(4) C(223) 0.056(6) 0.042(5) 0.049(6) 0.027(5) 0.004(5) 0.004(4) C(224) 0.037(5) 0.052(6) 0.064(7) 0.025(5) 0.012(5) 0.012(5) C(225) 0.034(5) 0.052(6) 0.058(6) 0.021(5) 0.012(5) 0.024(5) C(226) 0.024(4) 0.037(5) 0.047(5) 0.007(4) 0.005(4) 0.013(4) C(311) 0.051(6) 0.042(6) 0.058(6) 0.015(5) 0.001(5) 0.018(5) C(312) 0.065(8) 0.068(8) 0.074(8) 0.025(7) -0.011(6) -0.003(6) C(313) 0.069(8) 0.109(11) 0.066(8) 0.042(8) -0.011(7) 0.007(8) C(314) 0.092(11) 0.115(13) 0.077(10) 0.040(10) -0.018(8) 0.013(9) C(315) 0.099(12) 0.113(12) 0.080(10) 0.039(10) -0.024(9) 0.012(9) C(316) 0.096(10) 0.080(9) 0.079(9) 0.020(8) -0.035(8) 0.015(7) C(321) 0.067(7) 0.040(6) 0.045(6) 0.014(5) -0.008(5) 0.007(5) C(322) 0.088(10) 0.059(8) 0.097(10) 0.024(7) -0.031(8) 0.005(7) C(323) 0.109(13) 0.081(11) 0.156(16) 0.047(10) -0.053(12) -0.032(10) C(324) 0.126(15) 0.085(11) 0.127(14) 0.057(11) -0.053(12) -0.039(10) C(325) 0.082(10) 0.074(10) 0.094(11) -0.014(8) -0.035(8) 0.021(8) C(326) 0.089(10) 0.051(7) 0.082(9) 0.008(7) -0.006(7) 0.010(6) C(411) 0.053(6) 0.057(6) 0.036(5) 0.018(5) 0.004(5) -0.006(5) C(412) 0.069(8) 0.063(7) 0.049(7) 0.008(6) 0.010(6) -0.007(6) C(413) 0.088(9) 0.071(8) 0.057(8) 0.003(7) 0.016(7) 0.000(6) C(414) 0.073(8) 0.072(8) 0.050(7) 0.011(7) -0.007(6) -0.011(6) C(415) 0.095(10) 0.073(8) 0.045(7) 0.020(8) -0.002(6) 0.013(6) C(416) 0.063(7) 0.069(7) 0.041(6) 0.021(6) 0.012(5) 0.018(5) C(421) 0.084(9) 0.071(8) 0.042(6) 0.043(7) 0.004(6) 0.000(5) C(422) 0.064(8) 0.098(11) 0.128(13) 0.055(8) -0.005(8) -0.008(9) C(423) 0.098(12) 0.151(16) 0.146(16) 0.092(13) -0.027(11) -0.028(13) C(424) 0.18(2) 0.22(3) 0.096(14) 0.14(2) 0.000(14) -0.018(15) C(425) 0.24(2) 0.155(17) 0.086(11) 0.158(18) -0.051(14) -0.056(11) C(426) 0.162(16) 0.146(15) 0.072(9) 0.117(14) -0.032(10) -0.032(10) C(910) 0.159(17) 0.122(14) 0.092(12) 0.078(13) 0.025(11) 0.016(10) C(920) 0.122(13) 0.057(8) 0.104(12) 0.011(8) 0.004(10) 0.011(8) C(930) 0.25(3) 0.080(13) 0.18(2) 0.060(16) 0.040(19) -0.038(13) # 10. MOLECULAR GEOMETRY _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_publ_flag Re(1) O(1) 1.777(5) ? Re(1) O(1) 1.777(5) ? Re(1) P(1) 2.474(2) ? Re(1) P(1) 2.474(2) ? Re(1) P(2) 2.4865(19) ? Re(1) P(2) 2.4866(19) ? Re(2) O(2) 1.900(7) ? Re(2) O(2) 1.900(8) ? Re(2) P(4) 2.466(2) ? Re(2) P(4) 2.466(2) ? Re(2) P(3) 2.476(2) ? Re(2) P(3) 2.476(2) ? Cl(91) C(910) 1.741(17) ? Cl(92) C(910) 1.761(17) ? Cl(93) C(920) 1.724(14) ? Cl(94) C(920) 1.718(15) ? Cl(95) C(930) 1.80(2) ? Cl(96) C(930) 1.79(2) ? P(1) C(121) 1.816(7) ? P(1) C(11) 1.819(8) ? P(1) C(111) 1.822(8) ? P(2) C(211) 1.810(8) ? P(2) C(221) 1.824(8) ? P(2) C(21) 1.854(8) ? P(3) C(321) 1.797(10) ? P(3) C(311) 1.798(10) ? P(3) C(31) 1.851(10) ? P(4) C(411) 1.812(10) ? P(4) C(421) 1.821(11) ? P(4) C(41) 1.829(10) ? C(11) C(21) 1.542(10) ? C(31) C(41) 1.501(14) ? C(111) C(112) 1.377(12) ? C(111) C(116) 1.389(12) ? C(112) C(113) 1.406(12) ? C(113) C(114) 1.374(13) ? C(114) C(115) 1.389(14) ? C(115) C(116) 1.388(12) ? C(121) C(122) 1.388(12) ? C(121) C(126) 1.392(12) ? C(122) C(123) 1.395(12) ? C(123) C(124) 1.365(13) ? C(124) C(125) 1.368(14) ? C(125) C(126) 1.415(12) ? C(211) C(212) 1.361(12) ? C(211) C(216) 1.422(12) ? C(212) C(213) 1.388(12) ? C(213) C(214) 1.378(14) ? C(214) C(215) 1.364(14) ? C(215) C(216) 1.370(12) ? C(221) C(226) 1.390(11) ? C(221) C(222) 1.391(11) ? C(222) C(223) 1.395(12) ? C(223) C(224) 1.377(13) ? C(224) C(225) 1.390(14) ? C(225) C(226) 1.385(12) ? C(311) C(312) 1.380(15) ? C(311) C(316) 1.402(15) ? C(312) C(313) 1.378(16) ? C(313) C(314) 1.307(19) ? C(314) C(315) 1.39(2) ? C(315) C(316) 1.376(17) ? C(321) C(322) 1.358(16) ? C(321) C(326) 1.380(16) ? C(322) C(323) 1.386(18) ? C(323) C(324) 1.37(2) ? C(324) C(325) 1.32(2) ? C(325) C(326) 1.423(18) ? C(411) C(416) 1.379(13) ? C(411) C(412) 1.389(15) ? C(412) C(413) 1.382(16) ? C(413) C(414) 1.365(16) ? C(414) C(415) 1.376(16) ? C(415) C(416) 1.398(15) ? C(421) C(426) 1.349(17) ? C(421) C(422) 1.382(17) ? C(422) C(423) 1.377(18) ? C(423) C(424) 1.36(2) ? C(424) C(425) 1.38(2) ? C(425) C(426) 1.413(19) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag O(1) Re(1) O(1) 179.996(2) ? O(1) Re(1) P(1) 94.78(17) ? O(1) Re(1) P(1) 85.23(17) ? O(1) Re(1) P(1) 85.22(17) ? O(1) Re(1) P(1) 94.77(17) ? P(1) Re(1) P(1) 180.00(17) ? O(1) Re(1) P(2) 95.78(16) ? O(1) Re(1) P(2) 84.22(16) ? P(1) Re(1) P(2) 79.56(7) ? P(1) Re(1) P(2) 100.44(7) ? O(1) Re(1) P(2) 84.22(16) ? O(1) Re(1) P(2) 95.78(16) ? P(1) Re(1) P(2) 100.44(7) ? P(1) Re(1) P(2) 79.56(7) ? P(2) Re(1) P(2) 180.00(7) ? O(2) Re(2) O(2) 179.9970(10) ? O(2) Re(2) P(4) 95.7(2) ? O(2) Re(2) P(4) 84.3(2) ? O(2) Re(2) P(4) 84.3(2) ? O(2) Re(2) P(4) 95.7(2) ? P(4) Re(2) P(4) 179.9990(10) ? O(2) Re(2) P(3) 94.6(2) ? O(2) Re(2) P(3) 85.4(2) ? P(4) Re(2) P(3) 79.25(8) ? P(4) Re(2) P(3) 100.75(8) ? O(2) Re(2) P(3) 85.4(2) ? O(2) Re(2) P(3) 94.6(2) ? P(4) Re(2) P(3) 100.76(8) ? P(4) Re(2) P(3) 79.24(8) ? P(3) Re(2) P(3) 179.9970(10) ? C(121) P(1) C(11) 104.0(3) ? C(121) P(1) C(111) 105.2(4) ? C(11) P(1) C(111) 108.3(4) ? C(121) P(1) Re(1) 119.1(3) ? C(11) P(1) Re(1) 102.8(3) ? C(111) P(1) Re(1) 116.4(3) ? C(211) P(2) C(221) 107.1(4) ? C(211) P(2) C(21) 102.7(4) ? C(221) P(2) C(21) 105.4(4) ? C(211) P(2) Re(1) 119.6(3) ? C(221) P(2) Re(1) 112.5(3) ? C(21) P(2) Re(1) 108.2(3) ? C(321) P(3) C(311) 105.9(5) ? C(321) P(3) C(31) 105.9(5) ? C(311) P(3) C(31) 102.3(5) ? C(321) P(3) Re(2) 113.0(3) ? C(311) P(3) Re(2) 120.3(3) ? C(31) P(3) Re(2) 108.1(3) ? C(411) P(4) C(421) 105.4(5) ? C(411) P(4) C(41) 106.7(5) ? C(421) P(4) C(41) 102.4(6) ? C(411) P(4) Re(2) 118.0(3) ? C(421) P(4) Re(2) 119.1(4) ? C(41) P(4) Re(2) 103.5(3) ? C(21) C(11) P(1) 111.2(5) ? C(11) C(21) P(2) 113.0(5) ? C(41) C(31) P(3) 114.2(7) ? C(31) C(41) P(4) 110.9(7) ? C(112) C(111) C(116) 120.1(8) ? C(112) C(111) P(1) 118.1(6) ? C(116) C(111) P(1) 121.8(6) ? C(111) C(112) C(113) 119.8(9) ? C(114) C(113) C(112) 120.8(9) ? C(113) C(114) C(115) 118.4(9) ? C(116) C(115) C(114) 121.7(9) ? C(115) C(116) C(111) 119.2(9) ? C(122) C(121) C(126) 119.6(7) ? C(122) C(121) P(1) 118.6(6) ? C(126) C(121) P(1) 121.8(7) ? C(121) C(122) C(123) 119.9(8) ? C(124) C(123) C(122) 120.7(9) ? C(123) C(124) C(125) 120.4(8) ? C(124) C(125) C(126) 120.2(9) ? C(121) C(126) C(125) 119.2(9) ? C(212) C(211) C(216) 118.2(8) ? C(212) C(211) P(2) 120.5(6) ? C(216) C(211) P(2) 121.2(7) ? C(211) C(212) C(213) 121.2(9) ? C(214) C(213) C(212) 120.1(10) ? C(215) C(214) C(213) 119.5(8) ? C(214) C(215) C(216) 121.2(9) ? C(215) C(216) C(211) 119.8(9) ? C(226) C(221) C(222) 119.4(8) ? C(226) C(221) P(2) 119.8(6) ? C(222) C(221) P(2) 120.6(6) ? C(221) C(222) C(223) 119.8(9) ? C(224) C(223) C(222) 120.7(9) ? C(223) C(224) C(225) 119.6(9) ? C(226) C(225) C(224) 120.1(9) ? C(225) C(226) C(221) 120.5(8) ? C(312) C(311) C(316) 115.3(10) ? C(312) C(311) P(3) 122.9(8) ? C(316) C(311) P(3) 120.8(9) ? C(313) C(312) C(311) 122.3(13) ? C(314) C(313) C(312) 121.1(15) ? C(313) C(314) C(315) 120.0(14) ? C(316) C(315) C(314) 119.2(15) ? C(315) C(316) C(311) 121.7(14) ? C(322) C(321) C(326) 118.0(11) ? C(322) C(321) P(3) 121.1(9) ? C(326) C(321) P(3) 120.0(9) ? C(321) C(322) C(323) 121.0(14) ? C(324) C(323) C(322) 121.0(16) ? C(325) C(324) C(323) 119.0(15) ? C(324) C(325) C(326) 121.0(15) ? C(321) C(326) C(325) 119.9(14) ? C(416) C(411) C(412) 120.7(10) ? C(416) C(411) P(4) 122.5(8) ? C(412) C(411) P(4) 116.8(8) ? C(413) C(412) C(411) 119.8(11) ? C(414) C(413) C(412) 119.5(12) ? C(413) C(414) C(415) 121.6(11) ? C(414) C(415) C(416) 119.4(11) ? C(411) C(416) C(415) 119.0(11) ? C(426) C(421) C(422) 119.7(12) ? C(426) C(421) P(4) 121.8(10) ? C(422) C(421) P(4) 118.5(9) ? C(423) C(422) C(421) 121.6(14) ? C(424) C(423) C(422) 117.8(17) ? C(423) C(424) C(425) 122.5(18) ? C(424) C(425) C(426) 117.7(16) ? C(421) C(426) C(425) 120.2(14) ? Cl(91) C(910) Cl(92) 111.3(9) ? Cl(94) C(920) Cl(93) 111.2(8) ? Cl(96) C(930) Cl(95) 105.0(10) ? #===END data_RX473_ # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description brick _exptl_crystal_colour brown _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.10 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C86 H92 Cl4 O18 P4 Re4' _chemical_formula_structural ? _chemical_formula_weight 2424.19 _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+1/2, -z+1/2' '-x, -y, -z' 'x, -y+1/2, z+1/2' _cell_length_a 13.9995(7) _cell_length_b 23.5126(7) _cell_length_c 14.3633(7) _cell_angle_alpha 90.00 _cell_angle_beta 114.1998(16) _cell_angle_gamma 90.00 _cell_volume 4312.4(6) _cell_measurement_reflns_used 35082 _cell_measurement_theta_min 4 _cell_measurement_theta_max 31 _cell_formula_units_z 2 _exptl_crystal_density_diffrn 1.87 _exptl_crystal_density_meas ? _diffrn_radiation_type MO-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 5.937 _cell_measurement_temperature 296 _exptl_crystal_F_000 2360 # 6. DATA COLLECTION _diffrn_ambient_temperature 296 _diffrn_measurement_device_type ? _exptl_absorpt_correction_type refined_empirical_(Spek,_1997 _exptl_absorpt_correction_T_min 0.3540 _exptl_absorpt_correction_T_max 0.7710 _diffrn_reflns_number 35082 _reflns_number_total 10854 _reflns_number_gt 7175 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.101 _diffrn_reflns_theta_min 4.00 _diffrn_reflns_theta_max 31.02 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_max 18 # 7. REFINEMENT DATA _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R_factor_obs 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_R_factor_gt 0.062 _refine_ls_wR_factor_ref 0.104 _refine_ls_hydrogen_treatment H_atoms_riding _refine_ls_number_reflns 10854 _refine_ls_number_parameters 550 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 1.138 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0359P)^2^+7.4940P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.074 _refine_diff_density_max 1.97 _refine_diff_density_min -2.55 _refine_ls_extinction_method none _atom_type_scat_source 'International Tables for Crystallography (Vol C)' # 8. COMPUTING DATA _computing_data_collection Collect_(Nonius,_1998) _computing_cell_refinement DENZO/SCALEPACK_(Otwinowski,_1996) _computing_data_reduction DENZO/SCALEPACK_(Otwinowski,_1996) _computing_structure_solution Direct_methods_(SIR97,_Altomare_et_al.,_1997) _computing_structure_refinement SHELX97_(Sheldrick,_1997) _computing_molecular_graphics ; ORTEP (Johnson, 1976) Xtal_GX (Hall, 1995) PLUTON (Spek, 1991) ; _computing_publication_material CIF_VAX_MolEN_(Fair,_1990) # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag Re(1) 0.01528(2) 0.001175(12) 0.12737(3) 0.03960(11) Uani ? Re(2) 0.12671(2) 0.016012(13) 0.05234(3) 0.03928(11) Uani ? Re(3) 0.1044(4) -0.0352(2) 0.0837(5) 0.037(2) Uani ? Re(4) 0.0397(5) 0.0518(2) 0.0938(5) 0.038(2) Uani ? Cl(1) 0.04253(18) 0.06338(9) 0.26776(17) 0.0575(8) Uani ? Cl(2) 0.28907(15) -0.02300(9) 0.15233(18) 0.0564(8) Uani ? P(1) 0.09463(17) -0.07196(9) 0.26944(17) 0.0489(8) Uani ? P(2) 0.21218(16) 0.10982(9) 0.12395(17) 0.0459(7) Uani ? O(1) -0.0465(4) -0.0694(2) 0.0582(4) 0.0478(19) Uani ? O(2) -0.1011(4) 0.0512(2) 0.0412(4) 0.051(2) Uani ? O(117) -0.2803(6) -0.1451(4) 0.3252(7) 0.096(4) Uani ? O(127) 0.3092(6) -0.2794(3) 0.2192(6) 0.084(3) Uani ? O(137) 0.4161(6) -0.0084(3) 0.6875(6) 0.086(3) Uani ? O(217) -0.0685(5) 0.3083(3) -0.0362(5) 0.068(3) Uani ? O(227) 0.4758(6) 0.1592(3) 0.5748(6) 0.094(3) Uani ? O(237) 0.5251(6) 0.1515(4) -0.0491(7) 0.101(4) Uani ? O(901) 0.7965(10) 0.1358(5) 0.0944(11) 0.147(6) Uani ? C(111) -0.0170(6) -0.0964(3) 0.2902(7) 0.050(3) Uani ? C(112) -0.0609(8) -0.0619(4) 0.3417(9) 0.074(4) Uani ? C(113) -0.1482(9) -0.0795(5) 0.3511(10) 0.087(6) Uani ? C(114) -0.1921(8) -0.1311(4) 0.3111(9) 0.071(4) Uani ? C(115) -0.1493(7) -0.1650(4) 0.2570(8) 0.068(4) Uani ? C(116) -0.0628(7) -0.1466(4) 0.2466(7) 0.059(4) Uani ? C(117) -0.3257(9) -0.1980(6) 0.2901(11) 0.100(6) Uani ? C(121) 0.1510(6) -0.1368(3) 0.2442(7) 0.053(3) Uani ? C(122) 0.1835(8) -0.1799(4) 0.3213(8) 0.069(4) Uani ? C(123) 0.2338(8) -0.2271(4) 0.3080(9) 0.078(5) Uani ? C(124) 0.2542(7) -0.2323(4) 0.2213(8) 0.061(4) Uani ? C(125) 0.2189(7) -0.1906(4) 0.1443(7) 0.059(4) Uani ? C(126) 0.1669(7) -0.1446(3) 0.1556(7) 0.052(3) Uani ? C(127) 0.3434(10) -0.2844(5) 0.1376(10) 0.098(6) Uani ? C(131) 0.1871(6) -0.0498(3) 0.3988(6) 0.051(3) Uani ? C(132) 0.2634(7) -0.0123(4) 0.4089(7) 0.064(4) Uani ? C(133) 0.3378(9) 0.0010(4) 0.5052(9) 0.079(5) Uani ? C(134) 0.3378(8) -0.0232(4) 0.5954(7) 0.062(4) Uani ? C(135) 0.2606(8) -0.0606(4) 0.5872(7) 0.071(4) Uani ? C(136) 0.1844(8) -0.0735(4) 0.4898(7) 0.069(4) Uani ? C(137) 0.4213(9) -0.0351(5) 0.7798(8) 0.094(5) Uani ? C(211) 0.1290(6) 0.1709(3) 0.0754(6) 0.049(3) Uani ? C(212) 0.1436(7) 0.2091(4) 0.0061(7) 0.057(4) Uani ? C(213) 0.0797(7) 0.2556(4) -0.0321(7) 0.058(4) Uani ? C(214) -0.0010(7) 0.2646(4) -0.0017(7) 0.057(3) Uani ? C(215) -0.0150(7) 0.2266(4) 0.0665(7) 0.056(3) Uani ? C(216) 0.0467(7) 0.1802(3) 0.1038(7) 0.054(4) Uani ? C(217) -0.0586(10) 0.3454(5) -0.1139(9) 0.094(6) Uani ? C(221) 0.2879(6) 0.1228(3) 0.2623(6) 0.050(3) Uani ? C(222) 0.2590(8) 0.1611(4) 0.3221(8) 0.070(4) Uani ? C(223) 0.3216(8) 0.1723(5) 0.4256(8) 0.081(4) Uani ? C(224) 0.4181(8) 0.1463(5) 0.4724(8) 0.070(4) Uani ? C(225) 0.4469(7) 0.1075(4) 0.4141(7) 0.060(4) Uani ? C(226) 0.3822(6) 0.0969(4) 0.3120(7) 0.057(3) Uani ? C(227) 0.5663(9) 0.1263(6) 0.6277(9) 0.111(6) Uani ? C(231) 0.3073(6) 0.1201(3) 0.0708(7) 0.049(3) Uani ? C(232) 0.3047(7) 0.0882(4) -0.0137(8) 0.061(4) Uani ? C(233) 0.3783(8) 0.0973(5) -0.0548(8) 0.075(5) Uani ? C(234) 0.4505(8) 0.1383(5) -0.0140(9) 0.070(4) Uani ? C(235) 0.4515(9) 0.1711(4) 0.0688(9) 0.074(4) Uani ? C(236) 0.3822(7) 0.1609(4) 0.1105(8) 0.065(4) Uani ? C(237) 0.5378(12) 0.1138(6) -0.1171(13) 0.127(9) Uani ? C(902) 0.7434(18) 0.0997(12) 0.1344(18) 0.26(2) Uani ? H(112) -0.0313 -0.0271 0.3696 0.0960 Uiso calc H(113) -0.1778 -0.0563 0.3848 0.1140 Uiso calc H(115) -0.1791 -0.1996 0.2284 0.0880 Uiso calc H(116) -0.0353 -0.1686 0.2094 0.0760 Uiso calc H(11A) -0.3503 -0.1998 0.2152 0.1310 Uiso calc H(11B) -0.3818 -0.2030 0.3099 0.1310 Uiso calc H(11C) -0.2763 -0.2276 0.3210 0.1310 Uiso calc H(122) 0.1709 -0.1764 0.3811 0.0900 Uiso calc H(123) 0.2540 -0.2556 0.3585 0.1020 Uiso calc H(125) 0.2310 -0.1942 0.0842 0.0770 Uiso calc H(126) 0.1416 -0.1181 0.1019 0.0670 Uiso calc H(12A) 0.2855 -0.2882 0.0716 0.1280 Uiso calc H(12B) 0.3862 -0.3174 0.1496 0.1280 Uiso calc H(12C) 0.3814 -0.2511 0.1363 0.1280 Uiso calc H(132) 0.2648 0.0044 0.3493 0.0830 Uiso calc H(133) 0.3889 0.0265 0.5101 0.1030 Uiso calc H(135) 0.2598 -0.0772 0.6472 0.0920 Uiso calc H(136) 0.1315 -0.0978 0.4847 0.0900 Uiso calc H(13A) 0.3609 -0.0263 0.7903 0.1230 Uiso calc H(13B) 0.4802 -0.0216 0.8384 0.1230 Uiso calc H(13C) 0.4263 -0.0755 0.7734 0.1230 Uiso calc H(212) 0.1967 0.2032 -0.0146 0.0740 Uiso calc H(213) 0.0902 0.2808 -0.0779 0.0750 Uiso calc H(215) -0.0678 0.2327 0.0875 0.0720 Uiso calc H(216) 0.0344 0.1547 0.1481 0.0700 Uiso calc H(21A) 0.0071 0.3636 -0.0850 0.1220 Uiso calc H(21B) -0.1112 0.3738 -0.1342 0.1220 Uiso calc H(21C) -0.0650 0.3235 -0.1742 0.1220 Uiso calc H(222) 0.1963 0.1795 0.2912 0.0910 Uiso calc H(223) 0.2999 0.1970 0.4643 0.1060 Uiso calc H(225) 0.5095 0.0890 0.4442 0.0780 Uiso calc H(226) 0.4027 0.0709 0.2743 0.0740 Uiso calc H(22A) 0.5515 0.0868 0.6110 0.1450 Uiso calc H(22B) 0.5899 0.1316 0.7020 0.1450 Uiso calc H(22C) 0.6182 0.1385 0.6057 0.1450 Uiso calc H(232) 0.2544 0.0607 -0.0433 0.0800 Uiso calc H(233) 0.3774 0.0750 -0.1101 0.0970 Uiso calc H(235) 0.4993 0.2000 0.0959 0.0960 Uiso calc H(236) 0.3858 0.1822 0.1679 0.0840 Uiso calc H(23A) 0.5588 0.0777 -0.0832 0.1650 Uiso calc H(23B) 0.5891 0.1279 -0.1385 0.1650 Uiso calc H(23C) 0.4745 0.1095 -0.1775 0.1650 Uiso calc H(901) 0.8390 0.1174 0.0825 0.1920 Uiso calc H(90A) 0.7783 0.0638 0.1533 0.3370 Uiso calc H(90B) 0.6755 0.0937 0.0821 0.3370 Uiso calc H(90C) 0.7401 0.1167 0.1952 0.3370 Uiso calc loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Re(1) 0.03962(18) 0.03810(18) 0.03766(18) 0.00205(12) 0.01238(14) 0.00096(12) Re(2) 0.03662(18) 0.03834(18) 0.03926(18) 0.00182(12) 0.01188(14) 0.00006(12) Re(3) 0.041(4) 0.031(3) 0.037(3) 0.004(2) 0.013(3) -0.004(2) Re(4) 0.041(4) 0.035(3) 0.038(4) 0.001(2) 0.017(3) 0.000(2) Cl(1) 0.0767(15) 0.0500(12) 0.0468(12) 0.0097(10) 0.0262(11) -0.0037(8) Cl(2) 0.0403(11) 0.0586(12) 0.0630(14) 0.0087(9) 0.0137(10) 0.0031(10) P(1) 0.0513(13) 0.0444(12) 0.0446(13) -0.0003(9) 0.0132(11) 0.0055(8) P(2) 0.0415(12) 0.0446(11) 0.0462(13) -0.0019(8) 0.0125(10) -0.0002(8) O(1) 0.047(3) 0.043(3) 0.043(3) -0.003(2) 0.008(3) 0.003(2) O(2) 0.043(3) 0.064(4) 0.034(3) 0.009(2) 0.004(2) -0.002(2) O(117) 0.081(6) 0.101(6) 0.124(7) -0.002(4) 0.059(5) 0.009(5) O(127) 0.096(6) 0.071(5) 0.083(5) 0.029(4) 0.034(5) 0.006(4) O(137) 0.083(5) 0.094(5) 0.053(4) -0.010(4) -0.002(4) 0.002(4) O(217) 0.080(5) 0.063(4) 0.070(5) 0.022(3) 0.041(4) 0.017(3) O(227) 0.083(6) 0.123(6) 0.048(4) 0.000(5) -0.002(4) -0.026(4) O(237) 0.089(6) 0.119(7) 0.121(8) 0.004(5) 0.070(6) -0.001(5) O(901) 0.147(10) 0.136(9) 0.164(11) 0.059(7) 0.069(9) -0.017(7) C(111) 0.050(5) 0.051(5) 0.049(5) 0.002(4) 0.019(4) 0.002(4) C(112) 0.078(7) 0.065(6) 0.089(8) -0.009(5) 0.044(6) -0.010(5) C(113) 0.093(9) 0.073(7) 0.120(11) 0.002(6) 0.069(8) -0.012(6) C(114) 0.066(7) 0.065(6) 0.079(8) 0.011(5) 0.027(6) 0.018(5) C(115) 0.061(6) 0.060(6) 0.073(7) 0.000(4) 0.018(5) 0.001(5) C(116) 0.050(6) 0.068(6) 0.062(6) 0.000(4) 0.027(5) -0.003(4) C(117) 0.071(8) 0.112(10) 0.121(11) -0.005(7) 0.042(8) 0.024(8) C(121) 0.052(5) 0.045(5) 0.057(6) -0.003(3) 0.017(4) 0.009(4) C(122) 0.081(7) 0.074(7) 0.065(7) 0.012(5) 0.043(6) 0.017(5) C(123) 0.088(8) 0.068(7) 0.085(8) 0.023(5) 0.042(7) 0.028(5) C(124) 0.059(6) 0.058(6) 0.066(7) 0.007(4) 0.025(5) -0.001(4) C(125) 0.058(6) 0.060(6) 0.055(6) -0.004(4) 0.019(5) -0.003(4) C(126) 0.057(6) 0.048(5) 0.049(5) 0.001(4) 0.020(4) 0.003(4) C(127) 0.103(10) 0.096(9) 0.099(10) 0.030(7) 0.045(8) -0.013(7) C(131) 0.052(5) 0.051(5) 0.039(5) 0.002(4) 0.009(4) 0.002(3) C(132) 0.063(6) 0.073(6) 0.044(5) -0.006(5) 0.011(5) 0.005(4) C(133) 0.072(7) 0.078(7) 0.077(8) -0.012(5) 0.019(6) 0.008(5) C(134) 0.069(6) 0.059(6) 0.047(5) 0.006(4) 0.012(5) -0.007(4) C(135) 0.071(7) 0.093(7) 0.039(5) -0.007(5) 0.012(5) 0.008(5) C(136) 0.069(7) 0.076(7) 0.050(6) -0.019(5) 0.012(5) 0.003(5) C(137) 0.104(10) 0.106(9) 0.054(7) -0.001(7) 0.014(6) -0.014(6) C(211) 0.051(5) 0.045(5) 0.046(5) -0.003(3) 0.015(4) 0.003(3) C(212) 0.054(6) 0.058(5) 0.057(6) 0.004(4) 0.021(5) 0.006(4) C(213) 0.060(6) 0.057(5) 0.055(6) -0.003(4) 0.022(5) 0.007(4) C(214) 0.062(6) 0.051(5) 0.053(5) 0.007(4) 0.019(5) 0.003(4) C(215) 0.054(5) 0.058(5) 0.057(6) 0.007(4) 0.025(5) 0.005(4) C(216) 0.055(6) 0.047(5) 0.061(6) 0.000(4) 0.025(5) 0.009(4) C(217) 0.126(11) 0.086(8) 0.081(8) 0.045(7) 0.055(8) 0.033(6) C(221) 0.053(5) 0.047(5) 0.043(5) -0.002(4) 0.012(4) 0.002(3) C(222) 0.064(6) 0.067(6) 0.059(6) 0.013(5) 0.006(5) -0.012(5) C(223) 0.074(7) 0.104(8) 0.051(6) 0.019(6) 0.012(6) -0.027(5) C(224) 0.062(6) 0.090(7) 0.046(6) -0.007(5) 0.009(5) -0.013(5) C(225) 0.037(5) 0.083(7) 0.055(6) 0.000(4) 0.013(4) 0.002(4) C(226) 0.046(5) 0.069(6) 0.050(6) 0.006(4) 0.015(4) -0.005(4) C(227) 0.069(8) 0.176(14) 0.047(7) 0.006(8) -0.019(6) -0.016(7) C(231) 0.046(5) 0.051(5) 0.050(5) 0.002(3) 0.019(4) -0.005(4) C(232) 0.058(6) 0.067(6) 0.065(6) -0.004(4) 0.031(5) 0.000(4) C(233) 0.080(8) 0.088(8) 0.072(7) 0.007(6) 0.047(6) -0.006(5) C(234) 0.055(6) 0.080(7) 0.087(8) 0.000(5) 0.040(6) 0.011(6) C(235) 0.086(8) 0.066(6) 0.069(7) -0.011(5) 0.031(6) -0.005(5) C(236) 0.067(7) 0.064(6) 0.067(7) -0.003(5) 0.031(6) -0.001(5) C(237) 0.125(13) 0.132(13) 0.172(17) 0.002(9) 0.110(13) -0.013(11) C(902) 0.24(3) 0.42(4) 0.23(3) -0.13(3) 0.21(2) -0.08(2) # 10. MOLECULAR GEOMETRY _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_publ_flag Re(1) Re(4) 1.376(6) ? Re(1) Re(3) 1.840(6) ? Re(1) O(1) 1.943(5) ? Re(1) O(2) 1.995(5) ? Re(1) Re(2) 2.2726(5) ? Re(1) Cl(1) 2.350(2) ? Re(1) P(1) 2.521(2) ? Re(1) Re(2) 2.5388(5) ? Re(1) Re(3) 2.857(6) ? Re(1) Re(4) 3.123(6) ? Re(2) Re(3) 1.364(6) ? Re(2) Re(4) 1.789(6) ? Re(2) O(1) 1.960(5) ? Re(2) O(2) 1.988(5) ? Re(2) Cl(2) 2.359(2) ? Re(2) P(2) 2.524(2) ? Re(2) Re(1) 2.5389(5) ? Re(2) Re(4) 2.903(6) ? Re(2) Re(3) 3.109(6) ? Re(3) O(2) 1.770(8) ? Re(3) O(1) 2.199(8) ? Re(3) Re(4) 2.275(8) ? Re(3) Cl(2) 2.440(6) ? Re(3) Re(4) 2.528(8) ? Re(3) P(1) 2.798(7) ? Re(3) Re(1) 2.857(6) ? Re(3) Re(2) 3.109(6) ? Re(4) O(2) 1.846(8) ? Re(4) O(1) 2.210(8) ? Re(4) Cl(1) 2.434(6) ? Re(4) Re(3) 2.528(8) ? Re(4) P(2) 2.706(6) ? Re(4) Re(2) 2.903(6) ? Re(4) Re(1) 3.123(6) ? P(1) C(121) 1.827(9) ? P(1) C(131) 1.829(8) ? P(1) C(111) 1.835(9) ? P(2) C(211) 1.813(8) ? P(2) C(221) 1.817(8) ? P(2) C(231) 1.820(9) ? O(1) Re(2) 1.960(5) ? O(1) Re(4) 2.210(8) ? O(2) Re(3) 1.770(8) ? O(2) Re(2) 1.988(5) ? O(117) C(117) 1.398(14) ? O(117) C(114) 1.400(12) ? O(127) C(124) 1.367(10) ? O(127) C(127) 1.422(13) ? O(137) C(134) 1.363(11) ? O(137) C(137) 1.411(13) ? O(217) C(214) 1.359(10) ? O(217) C(217) 1.446(12) ? O(227) C(224) 1.364(11) ? O(227) C(227) 1.431(13) ? O(237) C(237) 1.366(14) ? O(237) C(234) 1.385(12) ? C(111) C(116) 1.367(12) ? C(111) C(112) 1.397(12) ? C(112) C(113) 1.377(14) ? C(113) C(114) 1.376(14) ? C(114) C(115) 1.402(14) ? C(115) C(116) 1.379(13) ? C(121) C(126) 1.362(12) ? C(121) C(122) 1.413(12) ? C(122) C(123) 1.379(13) ? C(123) C(124) 1.366(14) ? C(124) C(125) 1.389(12) ? C(125) C(126) 1.360(12) ? C(131) C(132) 1.367(12) ? C(131) C(136) 1.405(12) ? C(132) C(133) 1.370(14) ? C(133) C(134) 1.384(14) ? C(134) C(135) 1.383(13) ? C(135) C(136) 1.388(12) ? C(211) C(212) 1.400(11) ? C(211) C(216) 1.410(12) ? C(212) C(213) 1.386(11) ? C(213) C(214) 1.404(12) ? C(214) C(215) 1.382(12) ? C(215) C(216) 1.367(11) ? C(221) C(226) 1.386(11) ? C(221) C(222) 1.402(12) ? C(222) C(223) 1.382(13) ? C(223) C(224) 1.407(14) ? C(224) C(225) 1.396(13) ? C(225) C(226) 1.370(12) ? C(231) C(236) 1.377(12) ? C(231) C(232) 1.390(12) ? C(232) C(233) 1.412(13) ? C(233) C(234) 1.359(14) ? C(234) C(235) 1.387(15) ? C(235) C(236) 1.366(14) ? O(901) C(902) 1.403(19) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag Re(4) Re(1) Re(3) 88.8(3) ? Re(4) Re(1) O(1) 134.2(3) ? Re(3) Re(1) O(1) 71.0(2) ? Re(4) Re(1) O(2) 63.3(3) ? Re(3) Re(1) O(2) 126.7(2) ? O(1) Re(1) O(2) 96.0(2) ? Re(4) Re(1) Re(2) 51.9(2) ? Re(3) Re(1) Re(2) 36.89(18) ? O(1) Re(1) Re(2) 99.50(17) ? O(2) Re(1) Re(2) 101.77(17) ? Re(4) Re(1) Cl(1) 76.7(3) ? Re(3) Re(1) Cl(1) 131.86(18) ? O(1) Re(1) Cl(1) 146.48(17) ? O(2) Re(1) Cl(1) 87.12(16) ? Re(2) Re(1) Cl(1) 112.55(6) ? Re(4) Re(1) P(1) 139.8(3) ? Re(3) Re(1) P(1) 78.11(19) ? O(1) Re(1) P(1) 77.08(15) ? O(2) Re(1) P(1) 151.08(18) ? Re(2) Re(1) P(1) 107.04(6) ? Cl(1) Re(1) P(1) 84.16(7) ? Re(4) Re(1) Re(2) 90.7(2) ? Re(3) Re(1) Re(2) 88.98(18) ? O(1) Re(1) Re(2) 49.71(14) ? O(2) Re(1) Re(2) 50.29(15) ? Re(2) Re(1) Re(2) 89.901(16) ? Cl(1) Re(1) Re(2) 135.92(6) ? P(1) Re(1) Re(2) 126.38(5) ? Re(4) Re(1) Re(3) 62.2(3) ? Re(3) Re(1) Re(3) 89.5(2) ? O(1) Re(1) Re(3) 76.47(18) ? O(2) Re(1) Re(3) 37.78(19) ? Re(2) Re(1) Re(3) 73.62(13) ? Cl(1) Re(1) Re(3) 120.92(12) ? P(1) Re(1) Re(3) 153.25(12) ? Re(2) Re(1) Re(3) 28.52(11) ? Re(4) Re(1) Re(4) 90.1(3) ? Re(3) Re(1) Re(4) 54.0(2) ? O(1) Re(1) Re(4) 44.56(19) ? O(2) Re(1) Re(4) 80.04(18) ? Re(2) Re(1) Re(4) 62.78(11) ? Cl(1) Re(1) Re(4) 164.73(11) ? P(1) Re(1) Re(4) 111.04(11) ? Re(2) Re(1) Re(4) 34.95(11) ? Re(3) Re(1) Re(4) 44.44(15) ? Re(3) Re(2) Re(4) 91.3(3) ? Re(3) Re(2) O(1) 132.9(3) ? Re(4) Re(2) O(1) 72.1(3) ? Re(3) Re(2) O(2) 60.4(3) ? Re(4) Re(2) O(2) 128.4(2) ? O(1) Re(2) O(2) 95.7(2) ? Re(3) Re(2) Re(1) 54.0(2) ? Re(4) Re(2) Re(1) 37.27(18) ? O(1) Re(2) Re(1) 99.55(16) ? O(2) Re(2) Re(1) 101.94(17) ? Re(3) Re(2) Cl(2) 76.8(2) ? Re(4) Re(2) Cl(2) 130.0(2) ? O(1) Re(2) Cl(2) 146.77(17) ? O(2) Re(2) Cl(2) 87.30(15) ? Re(1) Re(2) Cl(2) 112.23(6) ? Re(3) Re(2) P(2) 141.6(2) ? Re(4) Re(2) P(2) 75.60(19) ? O(1) Re(2) P(2) 77.66(15) ? O(2) Re(2) P(2) 152.26(18) ? Re(1) Re(2) P(2) 105.70(5) ? Cl(2) Re(2) P(2) 84.41(7) ? Re(3) Re(2) Re(1) 88.8(2) ? Re(4) Re(2) Re(1) 90.68(19) ? O(1) Re(2) Re(1) 49.14(14) ? O(2) Re(2) Re(1) 50.51(14) ? Re(1) Re(2) Re(1) 90.099(16) ? Cl(2) Re(2) Re(1) 136.34(6) ? P(2) Re(2) Re(1) 126.52(5) ? Re(3) Re(2) Re(4) 60.5(3) ? Re(4) Re(2) Re(4) 90.2(2) ? O(1) Re(2) Re(4) 75.38(18) ? O(2) Re(2) Re(4) 38.98(19) ? Re(1) Re(2) Re(4) 73.10(12) ? Cl(2) Re(2) Re(4) 122.19(12) ? P(2) Re(2) Re(4) 152.33(12) ? Re(1) Re(2) Re(4) 28.29(11) ? Re(3) Re(2) Re(3) 89.6(3) ? Re(4) Re(2) Re(3) 54.4(2) ? O(1) Re(2) Re(3) 44.64(19) ? O(2) Re(2) Re(3) 81.31(18) ? Re(1) Re(2) Re(3) 61.84(12) ? Cl(2) Re(2) Re(3) 165.38(11) ? P(2) Re(2) Re(3) 109.86(11) ? Re(1) Re(2) Re(3) 36.28(11) ? Re(4) Re(2) Re(3) 44.30(15) ? Re(2) Re(3) O(2) 77.6(3) ? Re(2) Re(3) Re(1) 89.1(3) ? O(2) Re(3) Re(1) 133.4(4) ? Re(2) Re(3) O(1) 128.1(4) ? O(2) Re(3) O(1) 97.8(3) ? Re(1) Re(3) O(1) 56.7(2) ? Re(2) Re(3) Re(4) 51.9(2) ? O(2) Re(3) Re(4) 114.0(4) ? Re(1) Re(3) Re(4) 37.22(19) ? O(1) Re(3) Re(4) 86.5(3) ? Re(2) Re(3) Cl(2) 70.2(3) ? O(2) Re(3) Cl(2) 89.9(3) ? Re(1) Re(3) Cl(2) 127.3(3) ? O(1) Re(3) Cl(2) 161.2(3) ? Re(4) Re(3) Cl(2) 106.0(3) ? Re(2) Re(3) Re(4) 91.5(3) ? O(2) Re(3) Re(4) 46.9(3) ? Re(1) Re(3) Re(4) 89.9(3) ? O(1) Re(3) Re(4) 55.2(2) ? Re(4) Re(3) Re(4) 90.5(3) ? Cl(2) Re(3) Re(4) 136.5(3) ? Re(2) Re(3) P(1) 132.8(3) ? O(2) Re(3) P(1) 149.5(3) ? Re(1) Re(3) P(1) 61.84(18) ? O(1) Re(3) P(1) 67.4(2) ? Re(4) Re(3) P(1) 92.4(3) ? Cl(2) Re(3) P(1) 97.5(2) ? Re(4) Re(3) P(1) 122.2(3) ? Re(2) Re(3) Re(1) 62.7(2) ? O(2) Re(3) Re(1) 43.7(2) ? Re(1) Re(3) Re(1) 90.5(2) ? O(1) Re(3) Re(1) 78.5(2) ? Re(4) Re(3) Re(1) 74.0(2) ? Cl(2) Re(3) Re(1) 118.1(2) ? Re(4) Re(3) Re(1) 28.79(14) ? P(1) Re(3) Re(1) 144.1(2) ? Re(2) Re(3) Re(2) 90.4(3) ? O(2) Re(3) Re(2) 80.6(3) ? Re(1) Re(3) Re(2) 54.74(15) ? O(1) Re(3) Re(2) 38.78(16) ? Re(4) Re(3) Re(2) 63.0(2) ? Cl(2) Re(3) Re(2) 160.0(3) ? Re(4) Re(3) Re(2) 35.14(15) ? P(1) Re(3) Re(2) 99.60(19) ? Re(1) Re(3) Re(2) 44.54(8) ? Re(1) Re(4) Re(2) 90.8(3) ? Re(1) Re(4) O(2) 74.9(3) ? Re(2) Re(4) O(2) 131.6(4) ? Re(1) Re(4) O(1) 127.6(4) ? Re(2) Re(4) O(1) 57.5(2) ? O(2) Re(4) O(1) 95.2(3) ? Re(1) Re(4) Re(3) 54.0(2) ? Re(2) Re(4) Re(3) 36.8(2) ? O(2) Re(4) Re(3) 112.2(3) ? O(1) Re(4) Re(3) 85.9(3) ? Re(1) Re(4) Cl(1) 70.0(2) ? Re(2) Re(4) Cl(1) 130.5(3) ? O(2) Re(4) Cl(1) 88.1(3) ? O(1) Re(4) Cl(1) 162.4(3) ? Re(3) Re(4) Cl(1) 108.9(3) ? Re(1) Re(4) Re(3) 89.0(3) ? Re(2) Re(4) Re(3) 90.5(3) ? O(2) Re(4) Re(3) 44.4(3) ? O(1) Re(4) Re(3) 54.8(2) ? Re(3) Re(4) Re(3) 89.5(3) ? Cl(1) Re(4) Re(3) 132.2(3) ? Re(1) Re(4) P(2) 136.7(3) ? Re(2) Re(4) P(2) 64.58(19) ? O(2) Re(4) P(2) 148.1(3) ? O(1) Re(4) P(2) 69.9(2) ? Re(3) Re(4) P(2) 95.3(3) ? Cl(1) Re(4) P(2) 98.5(2) ? Re(3) Re(4) P(2) 124.0(3) ? Re(1) Re(4) Re(2) 61.0(2) ? Re(2) Re(4) Re(2) 89.8(2) ? O(2) Re(4) Re(2) 42.7(2) ? O(1) Re(4) Re(2) 76.9(2) ? Re(3) Re(4) Re(2) 72.7(2) ? Cl(1) Re(4) Re(2) 116.0(2) ? Re(3) Re(4) Re(2) 28.02(15) ? P(2) Re(4) Re(2) 145.4(2) ? Re(1) Re(4) Re(1) 89.9(3) ? Re(2) Re(4) Re(1) 54.37(15) ? O(2) Re(4) Re(1) 79.1(3) ? O(1) Re(4) Re(1) 38.10(16) ? Re(3) Re(4) Re(1) 61.6(2) ? Cl(1) Re(4) Re(1) 158.5(2) ? Re(3) Re(4) Re(1) 36.09(15) ? P(2) Re(4) Re(1) 101.47(19) ? Re(2) Re(4) Re(1) 44.12(8) ? Re(1) Cl(1) Re(4) 33.37(13) ? Re(2) Cl(2) Re(3) 32.98(14) ? C(121) P(1) C(131) 103.3(4) ? C(121) P(1) C(111) 104.7(4) ? C(131) P(1) C(111) 105.0(4) ? C(121) P(1) Re(1) 120.6(3) ? C(131) P(1) Re(1) 119.8(3) ? C(111) P(1) Re(1) 101.4(3) ? C(121) P(1) Re(3) 83.3(3) ? C(131) P(1) Re(3) 122.7(3) ? C(111) P(1) Re(3) 128.6(3) ? Re(1) P(1) Re(3) 40.05(12) ? C(211) P(2) C(221) 106.3(4) ? C(211) P(2) C(231) 103.4(4) ? C(221) P(2) C(231) 101.1(4) ? C(211) P(2) Re(2) 113.9(3) ? C(221) P(2) Re(2) 123.5(3) ? C(231) P(2) Re(2) 106.2(3) ? C(211) P(2) Re(4) 85.4(3) ? C(221) P(2) Re(4) 111.1(3) ? C(231) P(2) Re(4) 142.8(3) ? Re(2) P(2) Re(4) 39.82(13) ? Re(1) O(1) Re(2) 81.15(19) ? Re(1) O(1) Re(3) 52.30(19) ? Re(2) O(1) Re(3) 96.6(3) ? Re(1) O(1) Re(4) 97.3(3) ? Re(2) O(1) Re(4) 50.39(19) ? Re(3) O(1) Re(4) 70.0(3) ? Re(3) O(2) Re(4) 88.7(4) ? Re(3) O(2) Re(2) 42.1(2) ? Re(4) O(2) Re(2) 98.4(3) ? Re(3) O(2) Re(1) 98.5(3) ? Re(4) O(2) Re(1) 41.8(2) ? Re(2) O(2) Re(1) 79.19(19) ? C(117) O(117) C(114) 118.6(9) ? C(124) O(127) C(127) 118.5(8) ? C(134) O(137) C(137) 117.7(9) ? C(214) O(217) C(217) 116.6(8) ? C(224) O(227) C(227) 117.1(9) ? C(237) O(237) C(234) 116.5(10) ? C(116) C(111) C(112) 119.7(9) ? C(116) C(111) P(1) 119.4(7) ? C(112) C(111) P(1) 120.6(7) ? C(113) C(112) C(111) 119.8(9) ? C(114) C(113) C(112) 120.5(10) ? C(113) C(114) O(117) 116.1(10) ? C(113) C(114) C(115) 119.5(10) ? O(117) C(114) C(115) 124.4(10) ? C(116) C(115) C(114) 119.5(9) ? C(111) C(116) C(115) 120.9(9) ? C(126) C(121) C(122) 118.2(8) ? C(126) C(121) P(1) 122.8(6) ? C(122) C(121) P(1) 119.0(8) ? C(123) C(122) C(121) 120.1(10) ? C(124) C(123) C(122) 120.5(9) ? C(123) C(124) O(127) 115.3(9) ? C(123) C(124) C(125) 118.9(9) ? O(127) C(124) C(125) 125.8(9) ? C(126) C(125) C(124) 120.9(9) ? C(125) C(126) C(121) 121.3(8) ? C(132) C(131) C(136) 118.7(8) ? C(132) C(131) P(1) 120.8(7) ? C(136) C(131) P(1) 120.4(7) ? C(131) C(132) C(133) 121.2(9) ? C(132) C(133) C(134) 120.8(10) ? O(137) C(134) C(135) 124.3(9) ? O(137) C(134) C(133) 116.7(10) ? C(135) C(134) C(133) 119.0(9) ? C(134) C(135) C(136) 120.2(9) ? C(135) C(136) C(131) 120.0(9) ? C(212) C(211) C(216) 118.5(8) ? C(212) C(211) P(2) 120.3(7) ? C(216) C(211) P(2) 121.1(6) ? C(213) C(212) C(211) 120.7(9) ? C(212) C(213) C(214) 120.0(8) ? O(217) C(214) C(215) 116.7(9) ? O(217) C(214) C(213) 124.3(8) ? C(215) C(214) C(213) 118.9(8) ? C(216) C(215) C(214) 121.6(9) ? C(215) C(216) C(211) 120.2(8) ? C(226) C(221) C(222) 116.8(8) ? C(226) C(221) P(2) 119.7(7) ? C(222) C(221) P(2) 123.4(7) ? C(223) C(222) C(221) 121.6(9) ? C(222) C(223) C(224) 119.9(9) ? O(227) C(224) C(225) 124.2(9) ? O(227) C(224) C(223) 116.8(9) ? C(225) C(224) C(223) 118.9(9) ? C(226) C(225) C(224) 119.5(9) ? C(225) C(226) C(221) 123.3(9) ? C(236) C(231) C(232) 117.7(9) ? C(236) C(231) P(2) 121.4(7) ? C(232) C(231) P(2) 120.9(7) ? C(231) C(232) C(233) 120.1(9) ? C(234) C(233) C(232) 120.4(10) ? C(233) C(234) O(237) 125.3(11) ? C(233) C(234) C(235) 119.4(10) ? O(237) C(234) C(235) 115.3(10) ? C(236) C(235) C(234) 120.0(10) ? C(235) C(236) C(231) 122.4(10) ? #===END data_J03F02 # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description needle _exptl_crystal_colour green _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.17 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C44 H48 Cl8 O6 P2 Re2' _chemical_formula_structural ? _chemical_formula_weight 1390.86 _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+1/2, -z+1/2' '-x, -y, -z' 'x, -y+1/2, z+1/2' _cell_length_a 16.5256(3) _cell_length_b 18.6675(4) _cell_length_c 33.0129(4) _cell_angle_alpha 90.00 _cell_angle_beta 100.5122(11) _cell_angle_gamma 90.00 _cell_volume 10013.3(6) _cell_measurement_reflns_used 75534 _cell_measurement_theta_min 4 _cell_measurement_theta_max 28 _cell_formula_units_z 8 _exptl_crystal_density_diffrn 1.85 _exptl_crystal_density_meas ? _diffrn_radiation_type MO-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 5.436 _cell_measurement_temperature 193 _exptl_crystal_F_000 5408 # 6. DATA COLLECTION _diffrn_ambient_temperature 193 _diffrn_measurement_device_type ? _exptl_absorpt_correction_type refined_empirical_(Otwinowski_&_Minor,_1996 _exptl_absorpt_correction_T_min 0.0795 _exptl_absorpt_correction_T_max 0.3863 _diffrn_reflns_number 75534 _reflns_number_total 15630 _reflns_number_gt 8019 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.100 _diffrn_reflns_theta_min 4.00 _diffrn_reflns_theta_max 28.74 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_min -44 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_max 43 # 7. REFINEMENT DATA _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R_factor_obs 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_R_factor_gt 0.053 _refine_ls_wR_factor_ref 0.122 _refine_ls_hydrogen_treatment H_atoms_riding _refine_ls_number_reflns 15630 _refine_ls_number_parameters 1171 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 0.946 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0738P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.003 _refine_diff_density_max 2.67 _refine_diff_density_min -1.36 _refine_ls_extinction_method none _atom_type_scat_source 'International Tables for Crystallography (Vol C) ' # 8. COMPUTING DATA _computing_data_collection Collect_(Nonius,_1998) _computing_cell_refinement DENZO/SCALEPACK_(Otwinowski,_1996) _computing_data_reduction DENZO/SCALEPACK_(Otwinowski,_1996) _computing_structure_solution Direct_methods_(Shelxs97,_Sheldrick,_1997) _computing_structure_refinement SHELX97_(Sheldrick,_1997) _computing_molecular_graphics ; ORTEP (Johnson, 1976) Xtal_GX (Hall, 1995) PLUTON (Spek, 1991) ; _computing_publication_material CIF_VAX_MolEN_(Fair,_1990) # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag Re(1A) 0.35438(3) 0.53841(2) 0.096701(13) 0.03007(16) Uani ? Re(1B) 0.3204(5) 0.4834(4) 0.1241(2) 0.026(2) Uani ? Re(2A) 0.40884(3) 0.46883(2) 0.149302(13) 0.02962(16) Uani ? Re(2B) 0.4437(5) 0.5272(4) 0.1222(2) 0.033(3) Uani ? Re(3A) 0.16577(4) 1.02737(3) -0.099752(15) 0.03703(19) Uani ? Re(3B) 0.1432(2) 1.04690(18) -0.14372(9) 0.0389(12) Uani ? Re(4A) 0.10353(4) 0.96855(3) -0.155018(15) 0.03567(19) Uani ? Re(4B) 0.1274(2) 0.94790(18) -0.11090(10) 0.0396(12) Uani ? Cl(11) 0.4148(2) 0.64933(15) 0.11298(9) 0.0492(10) Uani ? Cl(12) 0.23645(19) 0.58349(15) 0.11625(8) 0.0461(10) Uani ? Cl(13) 0.26572(18) 0.46231(14) 0.05307(8) 0.0416(9) Uani ? Cl(14) 0.44557(18) 0.52427(15) 0.05137(7) 0.0395(9) Uani ? Cl(21) 0.34789(18) 0.35776(14) 0.13315(8) 0.0398(9) Uani ? Cl(22) 0.52628(18) 0.42164(16) 0.12984(8) 0.0460(10) Uani ? Cl(23) 0.4966(2) 0.54505(15) 0.19255(8) 0.0450(10) Uani ? Cl(24) 0.31685(18) 0.48327(15) 0.19444(7) 0.0391(9) Uani ? Cl(31) 0.2606(3) 0.9434(2) -0.06752(11) 0.1013(16) Uani ? Cl(32) 0.0880(2) 0.99509(18) -0.05035(8) 0.0610(12) Uani ? Cl(33) 0.1018(2) 1.13771(16) -0.10316(10) 0.0590(12) Uani ? Cl(34) 0.2750(2) 1.0838(2) -0.12067(11) 0.0840(16) Uani ? Cl(41) 0.1663(2) 0.85799(17) -0.15143(11) 0.0771(14) Uani ? Cl(42) 0.1827(3) 0.9994(2) -0.20392(9) 0.0783(14) Uani ? Cl(43) 0.0091(3) 1.0520(2) -0.18708(11) 0.0887(14) Uani ? Cl(44) -0.0056(2) 0.9131(2) -0.13359(11) 0.0825(14) Uani ? P(1) 0.1746(2) 0.23311(16) 0.72019(9) 0.0403(10) Uani ? P(2) 0.6312(2) 0.21266(16) 0.21909(9) 0.0456(10) Uani ? P(3) 0.3825(2) 0.21467(16) 0.47722(9) 0.0394(10) Uani ? P(4) 0.9223(2) 0.22550(16) 0.96314(9) 0.0410(10) Uani ? O(117) -0.0775(6) 0.3410(5) 0.8100(2) 0.058(3) Uani ? O(127) 0.4003(5) 0.4536(4) 0.6756(2) 0.056(3) Uani ? O(137) -0.0140(6) 0.1147(5) 0.5651(2) 0.061(3) Uani ? O(217) 0.4306(5) 0.3804(4) 0.3163(2) 0.052(3) Uani ? O(227) 0.8928(6) 0.3996(5) 0.1785(2) 0.058(3) Uani ? O(237) 0.4421(6) 0.1138(4) 0.0591(2) 0.062(3) Uani ? O(317) 0.1501(5) 0.3651(4) 0.5646(2) 0.043(2) Uani ? O(327) 0.2201(6) 0.1072(5) 0.3135(3) 0.065(3) Uani ? O(337) 0.6392(6) 0.4032(4) 0.4337(2) 0.060(3) Uani ? O(417) 1.1510(6) 0.4504(5) 0.9258(2) 0.062(3) Uani ? O(427) 0.7116(6) 0.1236(5) 0.8090(3) 0.073(4) Uani ? O(437) 0.6964(6) 0.3567(6) 1.0620(2) 0.072(4) Uani ? C(111) 0.1044(7) 0.2701(6) 0.7497(3) 0.036(4) Uani ? C(112) 0.0778(8) 0.2288(6) 0.7804(3) 0.052(5) Uani ? C(113) 0.0186(8) 0.2550(7) 0.8007(3) 0.050(5) Uani ? C(114) -0.0157(8) 0.3201(8) 0.7900(3) 0.049(5) Uani ? C(115) 0.0094(8) 0.3628(7) 0.7603(3) 0.046(4) Uani ? C(116) 0.0698(7) 0.3369(6) 0.7407(3) 0.038(4) Uani ? C(117) -0.1139(8) 0.4093(8) 0.8013(3) 0.071(6) Uani ? C(121) 0.2408(7) 0.2999(6) 0.7055(4) 0.042(4) Uani ? C(122) 0.3159(7) 0.3185(6) 0.7320(3) 0.044(4) Uani ? C(123) 0.3650(7) 0.3692(6) 0.7210(3) 0.043(4) Uani ? C(124) 0.3463(7) 0.4037(6) 0.6839(3) 0.040(4) Uani ? C(125) 0.2746(8) 0.3851(6) 0.6572(3) 0.046(4) Uani ? C(126) 0.2241(8) 0.3352(6) 0.6685(3) 0.044(4) Uani ? C(127) 0.3787(7) 0.4945(6) 0.6378(3) 0.054(5) Uani ? C(131) 0.1164(7) 0.1947(6) 0.6739(3) 0.039(4) Uani ? C(132) 0.0409(8) 0.2235(6) 0.6561(3) 0.048(4) Uani ? C(133) 0.0001(8) 0.1960(6) 0.6195(3) 0.049(4) Uani ? C(134) 0.0316(8) 0.1389(7) 0.6012(3) 0.046(4) Uani ? C(135) 0.1477(8) 0.1371(6) 0.6551(4) 0.046(4) Uani ? C(136) 0.1080(8) 0.1089(6) 0.6195(3) 0.047(5) Uani ? C(137) 0.0141(9) 0.0555(7) 0.5459(4) 0.074(6) Uani ? C(141) 0.2380(7) 0.1655(6) 0.7497(3) 0.055(4) Uani ? C(211) 0.5708(7) 0.2638(6) 0.2476(3) 0.039(4) Uani ? C(212) 0.5482(7) 0.3337(6) 0.2363(3) 0.040(4) Uani ? C(213) 0.5020(8) 0.3754(6) 0.2579(3) 0.047(4) Uani ? C(214) 0.4753(8) 0.3460(7) 0.2922(3) 0.043(4) Uani ? C(215) 0.4975(8) 0.2757(6) 0.3042(3) 0.048(5) Uani ? C(216) 0.5428(7) 0.2343(6) 0.2818(3) 0.044(4) Uani ? C(217) 0.4075(7) 0.4524(6) 0.3054(3) 0.050(4) Uani ? C(221) 0.7135(7) 0.2659(6) 0.2078(3) 0.042(4) Uani ? C(222) 0.7077(8) 0.2988(6) 0.1703(3) 0.050(5) Uani ? C(223) 0.7673(9) 0.3437(6) 0.1609(3) 0.054(5) Uani ? C(224) 0.8375(8) 0.3549(6) 0.1910(4) 0.045(4) Uani ? C(225) 0.8461(9) 0.3203(6) 0.2271(4) 0.049(5) Uani ? C(226) 0.7857(8) 0.2781(7) 0.2363(3) 0.053(5) Uani ? C(227) 0.9625(8) 0.4181(7) 0.2071(4) 0.068(5) Uani ? C(231) 0.5743(7) 0.1817(6) 0.1712(3) 0.041(4) Uani ? C(232) 0.5001(8) 0.2106(6) 0.1551(3) 0.049(5) Uani ? C(233) 0.4565(8) 0.1890(6) 0.1167(3) 0.042(4) Uani ? C(234) 0.4887(10) 0.1346(7) 0.0962(4) 0.057(5) Uani ? C(235) 0.5646(9) 0.1046(7) 0.1116(4) 0.058(5) Uani ? C(236) 0.6078(8) 0.1294(6) 0.1495(4) 0.056(5) Uani ? C(237) 0.4705(10) 0.0568(7) 0.0378(4) 0.079(6) Uani ? C(241) 0.6713(8) 0.1372(6) 0.2494(3) 0.064(5) Uani ? C(311) 0.3122(7) 0.2633(6) 0.5033(3) 0.040(4) Uani ? C(312) 0.2869(7) 0.3309(6) 0.4917(3) 0.041(4) Uani ? C(313) 0.2346(7) 0.3676(6) 0.5113(3) 0.039(4) Uani ? C(314) 0.2051(7) 0.3352(6) 0.5441(3) 0.036(4) Uani ? C(315) 0.2282(7) 0.2673(6) 0.5556(3) 0.043(4) Uani ? C(316) 0.2830(7) 0.2299(6) 0.5355(3) 0.041(4) Uani ? C(317) 0.1312(8) 0.4393(6) 0.5588(3) 0.052(5) Uani ? C(321) 0.3294(7) 0.1796(5) 0.4290(3) 0.033(3) Uani ? C(322) 0.2565(7) 0.2088(6) 0.4080(4) 0.047(4) Uani ? C(323) 0.2220(8) 0.1841(7) 0.3689(4) 0.056(5) Uani ? C(324) 0.2594(8) 0.1281(6) 0.3513(4) 0.045(4) Uani ? C(325) 0.3331(8) 0.0999(6) 0.3720(4) 0.050(5) Uani ? C(326) 0.3673(7) 0.1249(6) 0.4102(4) 0.047(4) Uani ? C(327) 0.2496(9) 0.0462(7) 0.2958(4) 0.071(6) Uani ? C(331) 0.4607(7) 0.2715(6) 0.4656(3) 0.042(4) Uani ? C(332) 0.4496(8) 0.3075(6) 0.4280(3) 0.049(4) Uani ? C(333) 0.5111(8) 0.3505(7) 0.4190(4) 0.054(5) Uani ? C(334) 0.5821(8) 0.3598(6) 0.4463(4) 0.045(4) Uani ? C(335) 0.5949(8) 0.3250(6) 0.4840(3) 0.050(4) Uani ? C(336) 0.5330(8) 0.2814(6) 0.4933(3) 0.049(4) Uani ? C(337) 0.7149(8) 0.4128(7) 0.4606(4) 0.075(6) Uani ? C(341) 0.4286(7) 0.1432(6) 0.5103(3) 0.055(4) Uani ? C(411) 0.9921(7) 0.2901(6) 0.9498(3) 0.034(3) Uani ? C(412) 0.9790(8) 0.3234(6) 0.9122(4) 0.048(4) Uani ? C(413) 1.0302(8) 0.3761(6) 0.9019(3) 0.044(4) Uani ? C(414) 1.0976(8) 0.3967(7) 0.9316(4) 0.046(4) Uani ? C(415) 1.1128(8) 0.3617(6) 0.9694(3) 0.051(5) Uani ? C(416) 1.0611(7) 0.3091(6) 0.9780(3) 0.045(4) Uani ? C(417) 1.1317(8) 0.4912(7) 0.8884(4) 0.072(6) Uani ? C(421) 0.8583(7) 0.1930(6) 0.9172(3) 0.035(4) Uani ? C(422) 0.8849(8) 0.1370(7) 0.8955(4) 0.054(5) Uani ? C(423) 0.8365(10) 0.1122(7) 0.8595(4) 0.067(6) Uani ? C(424) 0.7625(10) 0.1431(7) 0.8444(4) 0.055(5) Uani ? C(425) 0.7352(8) 0.1999(7) 0.8649(4) 0.052(5) Uani ? C(426) 0.7832(8) 0.2240(6) 0.9010(3) 0.053(5) Uani ? C(427) 0.7353(10) 0.0671(7) 0.7856(4) 0.080(6) Uani ? C(431) 0.8604(7) 0.2666(6) 0.9954(3) 0.041(4) Uani ? C(432) 0.8345(7) 0.2301(6) 1.0272(3) 0.043(4) Uani ? C(433) 0.7803(8) 0.2635(7) 1.0489(3) 0.055(5) Uani ? C(434) 0.7502(8) 0.3313(7) 1.0392(3) 0.050(5) Uani ? C(435) 0.7774(8) 0.3693(7) 1.0082(3) 0.050(4) Uani ? C(436) 0.8319(8) 0.3358(6) 0.9867(3) 0.051(5) Uani ? C(437) 0.6622(9) 0.4269(8) 1.0522(4) 0.077(6) Uani ? C(441) 0.9794(7) 0.1528(6) 0.9901(3) 0.055(5) Uani ? H(112) 0.1003 0.1837 0.7869 0.0670 Uiso calc H(113) 0.0021 0.2284 0.8215 0.0650 Uiso calc H(115) -0.0140 0.4076 0.7537 0.0590 Uiso calc H(116) 0.0880 0.3651 0.7209 0.0490 Uiso calc H(11A) -0.0722 0.4456 0.8068 0.0920 Uiso calc H(11B) -0.1542 0.4171 0.8185 0.0920 Uiso calc H(11C) -0.1401 0.4115 0.7729 0.0920 Uiso calc H(122) 0.3309 0.2954 0.7572 0.0570 Uiso calc H(123) 0.4132 0.3812 0.7390 0.0560 Uiso calc H(125) 0.2614 0.4069 0.6315 0.0600 Uiso calc H(126) 0.1757 0.3242 0.6503 0.0570 Uiso calc H(12A) 0.3706 0.4625 0.6147 0.0710 Uiso calc H(12B) 0.4224 0.5274 0.6356 0.0710 Uiso calc H(12C) 0.3290 0.5208 0.6383 0.0710 Uiso calc H(132) 0.0183 0.2610 0.6688 0.0640 Uiso calc H(133) -0.0496 0.2162 0.6069 0.0640 Uiso calc H(135) 0.1978 0.1174 0.6675 0.0600 Uiso calc H(136) 0.1303 0.0705 0.6072 0.0600 Uiso calc H(13A) 0.0658 0.0669 0.5381 0.0960 Uiso calc H(13B) -0.0254 0.0433 0.5218 0.0960 Uiso calc H(13C) 0.0211 0.0156 0.5646 0.0960 Uiso calc H(14A) 0.2646 0.1854 0.7755 0.0710 Uiso calc H(14B) 0.2788 0.1492 0.7345 0.0710 Uiso calc H(14C) 0.2042 0.1258 0.7547 0.0710 Uiso calc H(212) 0.5649 0.3531 0.2132 0.0520 Uiso calc H(213) 0.4888 0.4223 0.2499 0.0610 Uiso calc H(215) 0.4816 0.2567 0.3276 0.0620 Uiso calc H(216) 0.5549 0.1869 0.2893 0.0580 Uiso calc H(21A) 0.4557 0.4798 0.3033 0.0660 Uiso calc H(21B) 0.3809 0.4730 0.3262 0.0660 Uiso calc H(21C) 0.3704 0.4529 0.2794 0.0660 Uiso calc H(222) 0.6614 0.2901 0.1503 0.0650 Uiso calc H(223) 0.7611 0.3662 0.1354 0.0690 Uiso calc H(225) 0.8947 0.3256 0.2462 0.0640 Uiso calc H(226) 0.7922 0.2568 0.2622 0.0690 Uiso calc H(22A) 0.9461 0.4417 0.2302 0.0880 Uiso calc H(22B) 0.9963 0.4498 0.1945 0.0880 Uiso calc H(22C) 0.9931 0.3756 0.2164 0.0880 Uiso calc H(232) 0.4778 0.2455 0.1699 0.0640 Uiso calc H(233) 0.4070 0.2108 0.1053 0.0550 Uiso calc H(235) 0.5863 0.0688 0.0972 0.0750 Uiso calc H(236) 0.6595 0.1106 0.1601 0.0730 Uiso calc H(23A) 0.5235 0.0686 0.0317 0.1020 Uiso calc H(23B) 0.4325 0.0484 0.0126 0.1020 Uiso calc H(23C) 0.4749 0.0144 0.0545 0.1020 Uiso calc H(24A) 0.6906 0.1521 0.2773 0.0830 Uiso calc H(24B) 0.7162 0.1170 0.2384 0.0830 Uiso calc H(24C) 0.6288 0.1019 0.2487 0.0830 Uiso calc H(312) 0.3060 0.3524 0.4699 0.0540 Uiso calc H(313) 0.2183 0.4138 0.5031 0.0510 Uiso calc H(315) 0.2077 0.2455 0.5770 0.0570 Uiso calc H(316) 0.2995 0.1836 0.5436 0.0540 Uiso calc H(31A) 0.1804 0.4671 0.5670 0.0680 Uiso calc H(31B) 0.0914 0.4527 0.5753 0.0680 Uiso calc H(31C) 0.1090 0.4482 0.5303 0.0680 Uiso calc H(322) 0.2306 0.2451 0.4202 0.0610 Uiso calc H(323) 0.1740 0.2048 0.3546 0.0730 Uiso calc H(325) 0.3592 0.0638 0.3599 0.0640 Uiso calc H(326) 0.4165 0.1053 0.4239 0.0610 Uiso calc H(32A) 0.3043 0.0554 0.2910 0.0920 Uiso calc H(32B) 0.2141 0.0356 0.2701 0.0920 Uiso calc H(32C) 0.2506 0.0062 0.3141 0.0920 Uiso calc H(332) 0.4008 0.3023 0.4092 0.0630 Uiso calc H(333) 0.5041 0.3737 0.3936 0.0700 Uiso calc H(335) 0.6440 0.3307 0.5026 0.0650 Uiso calc H(336) 0.5403 0.2583 0.5187 0.0630 Uiso calc H(33A) 0.7061 0.4384 0.4846 0.0980 Uiso calc H(33B) 0.7515 0.4397 0.4469 0.0980 Uiso calc H(33C) 0.7388 0.3669 0.4686 0.0980 Uiso calc H(34A) 0.4742 0.1236 0.4997 0.0720 Uiso calc H(34B) 0.3885 0.1063 0.5113 0.0720 Uiso calc H(34C) 0.4475 0.1615 0.5376 0.0720 Uiso calc H(412) 0.9336 0.3098 0.8927 0.0620 Uiso calc H(413) 1.0201 0.3973 0.8760 0.0570 Uiso calc H(415) 1.1585 0.3742 0.9890 0.0670 Uiso calc H(416) 1.0725 0.2856 1.0032 0.0580 Uiso calc H(41A) 1.1276 0.4595 0.8652 0.0930 Uiso calc H(41B) 1.1745 0.5257 0.8875 0.0930 Uiso calc H(41C) 1.0803 0.5156 0.8875 0.0930 Uiso calc H(422) 0.9357 0.1159 0.9051 0.0700 Uiso calc H(423) 0.8548 0.0740 0.8455 0.0870 Uiso calc H(425) 0.6851 0.2218 0.8546 0.0680 Uiso calc H(426) 0.7646 0.2622 0.9149 0.0690 Uiso calc H(42A) 0.7877 0.0779 0.7785 0.1040 Uiso calc H(42B) 0.6949 0.0612 0.7609 0.1040 Uiso calc H(42C) 0.7393 0.0237 0.8014 0.1040 Uiso calc H(432) 0.8531 0.1839 1.0340 0.0560 Uiso calc H(433) 0.7639 0.2393 1.0707 0.0710 Uiso calc H(435) 0.7598 0.4160 1.0019 0.0650 Uiso calc H(436) 0.8497 0.3608 0.9656 0.0660 Uiso calc H(43A) 0.7054 0.4620 1.0572 0.1000 Uiso calc H(43B) 0.6222 0.4371 1.0692 0.1000 Uiso calc H(43C) 0.6363 0.4284 1.0237 0.1000 Uiso calc H(44A) 1.0068 0.1690 1.0167 0.0720 Uiso calc H(44B) 1.0196 0.1361 0.9747 0.0720 Uiso calc H(44C) 0.9426 0.1144 0.9935 0.0720 Uiso calc loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Re(1A) 0.0325(3) 0.0281(3) 0.0294(3) 0.0003(2) 0.0051(2) -0.0006(2) Re(1B) 0.024(5) 0.032(5) 0.024(4) -0.001(4) 0.008(3) -0.002(4) Re(2A) 0.0314(3) 0.0289(3) 0.0281(3) 0.0005(2) 0.0042(2) -0.0020(2) Re(2B) 0.027(5) 0.025(5) 0.045(5) -0.012(4) 0.005(4) -0.009(4) Re(3A) 0.0338(4) 0.0451(4) 0.0334(3) -0.0072(3) 0.0093(3) -0.0077(3) Re(3B) 0.048(3) 0.040(2) 0.0314(19) -0.0101(18) 0.0142(17) -0.0005(15) Re(4A) 0.0402(4) 0.0361(4) 0.0325(3) -0.0082(3) 0.0114(3) -0.0065(2) Re(4B) 0.047(3) 0.042(2) 0.032(2) 0.0000(18) 0.0128(17) 0.0009(15) Cl(11) 0.065(2) 0.0278(16) 0.0559(19) -0.0082(15) 0.0137(16) -0.0072(14) Cl(12) 0.041(2) 0.0483(19) 0.0514(18) 0.0167(15) 0.0146(15) 0.0066(15) Cl(13) 0.043(2) 0.0419(18) 0.0350(15) -0.0089(14) -0.0056(13) -0.0036(13) Cl(14) 0.0437(19) 0.0446(18) 0.0323(14) -0.0094(15) 0.0128(13) -0.0055(13) Cl(21) 0.047(2) 0.0251(15) 0.0478(17) -0.0042(13) 0.0099(14) -0.0051(12) Cl(22) 0.036(2) 0.052(2) 0.0522(18) 0.0138(15) 0.0140(15) 0.0077(15) Cl(23) 0.046(2) 0.051(2) 0.0334(16) -0.0116(15) -0.0048(14) -0.0092(13) Cl(24) 0.049(2) 0.0385(16) 0.0322(15) -0.0017(14) 0.0135(13) -0.0029(13) Cl(31) 0.082(3) 0.143(4) 0.070(2) 0.057(3) -0.010(2) 0.003(2) Cl(32) 0.083(3) 0.071(2) 0.0365(17) -0.023(2) 0.0304(17) -0.0120(16) Cl(33) 0.066(3) 0.0391(19) 0.075(2) -0.0027(17) 0.0208(19) -0.0112(16) Cl(34) 0.065(3) 0.104(3) 0.096(3) -0.051(2) 0.049(2) -0.053(2) Cl(41) 0.092(3) 0.046(2) 0.097(3) 0.016(2) 0.027(2) -0.0156(19) Cl(42) 0.111(3) 0.084(3) 0.052(2) -0.044(2) 0.047(2) -0.0230(19) Cl(43) 0.090(3) 0.097(3) 0.065(2) 0.032(3) -0.023(2) -0.001(2) Cl(44) 0.086(3) 0.091(3) 0.085(2) -0.057(2) 0.054(2) -0.046(2) P(1) 0.038(2) 0.0404(19) 0.0401(17) 0.0006(16) 0.0008(15) 0.0018(14) P(2) 0.051(2) 0.0365(19) 0.0488(19) 0.0110(17) 0.0076(17) 0.0079(15) P(3) 0.038(2) 0.0339(18) 0.0452(18) 0.0059(15) 0.0045(15) 0.0069(14) P(4) 0.041(2) 0.0385(19) 0.0426(18) 0.0011(16) 0.0053(15) 0.0047(15) O(117) 0.053(7) 0.077(7) 0.046(5) -0.002(5) 0.018(5) 0.001(5) O(127) 0.055(6) 0.063(6) 0.051(5) -0.015(5) 0.012(4) 0.021(4) O(137) 0.072(7) 0.057(6) 0.051(5) -0.012(5) 0.004(5) -0.021(5) O(217) 0.060(6) 0.059(6) 0.042(5) 0.012(5) 0.022(4) 0.007(4) O(227) 0.059(7) 0.070(6) 0.043(5) -0.010(5) 0.007(5) -0.013(4) O(237) 0.079(7) 0.056(6) 0.050(5) 0.000(5) 0.013(5) -0.004(5) O(317) 0.037(5) 0.050(5) 0.040(4) 0.008(4) 0.003(4) -0.002(4) O(327) 0.076(8) 0.060(6) 0.056(6) 0.013(5) 0.001(5) -0.017(5) O(337) 0.062(7) 0.062(6) 0.058(5) -0.011(5) 0.020(5) -0.001(5) O(417) 0.061(7) 0.067(6) 0.061(6) -0.014(5) 0.016(5) 0.011(5) O(427) 0.096(9) 0.067(7) 0.052(6) 0.000(6) -0.001(6) -0.020(5) O(437) 0.066(7) 0.119(9) 0.036(5) 0.023(6) 0.022(5) 0.008(5) C(111) 0.038(8) 0.041(7) 0.027(6) -0.009(6) 0.004(5) -0.001(5) C(112) 0.063(10) 0.044(8) 0.047(8) -0.004(7) 0.005(7) -0.001(6) C(113) 0.054(10) 0.055(9) 0.038(7) -0.010(7) 0.000(7) 0.014(7) C(114) 0.045(9) 0.079(11) 0.020(6) -0.025(8) 0.001(6) -0.017(7) C(115) 0.044(9) 0.052(8) 0.041(7) 0.003(7) 0.008(6) 0.003(6) C(116) 0.033(8) 0.038(7) 0.040(7) 0.003(6) -0.001(6) 0.009(6) C(117) 0.050(10) 0.124(14) 0.039(8) 0.024(9) 0.008(7) 0.006(8) C(121) 0.031(8) 0.042(8) 0.055(8) 0.002(6) 0.013(6) 0.001(6) C(122) 0.030(8) 0.055(8) 0.041(7) 0.006(6) -0.011(6) 0.015(6) C(123) 0.029(8) 0.057(8) 0.037(7) -0.003(6) -0.010(6) 0.002(6) C(124) 0.035(8) 0.041(8) 0.040(7) -0.006(6) -0.005(6) -0.008(6) C(125) 0.056(10) 0.047(8) 0.034(7) 0.005(7) 0.006(7) 0.010(6) C(126) 0.034(8) 0.048(8) 0.043(7) 0.009(6) -0.013(6) 0.007(6) C(127) 0.048(9) 0.062(9) 0.053(8) -0.016(7) 0.010(7) 0.011(7) C(131) 0.031(8) 0.048(8) 0.038(6) -0.010(6) 0.009(6) 0.001(6) C(132) 0.056(10) 0.030(7) 0.052(8) -0.007(7) -0.010(7) -0.013(6) C(133) 0.069(10) 0.031(7) 0.045(8) 0.008(7) 0.002(7) -0.005(6) C(134) 0.044(9) 0.047(8) 0.042(7) -0.013(7) -0.003(7) 0.001(6) C(135) 0.038(8) 0.051(8) 0.051(8) 0.005(6) 0.013(6) 0.000(6) C(136) 0.057(10) 0.041(8) 0.047(8) 0.010(7) 0.023(7) 0.007(6) C(137) 0.097(13) 0.062(10) 0.061(9) -0.027(9) 0.010(8) -0.017(8) C(141) 0.049(9) 0.044(8) 0.064(8) 0.008(7) -0.008(7) 0.015(6) C(211) 0.042(8) 0.043(8) 0.032(6) 0.017(6) 0.006(6) 0.005(5) C(212) 0.056(9) 0.036(7) 0.029(6) 0.007(6) 0.010(6) 0.015(5) C(213) 0.073(10) 0.036(7) 0.033(7) -0.002(7) 0.013(7) 0.012(6) C(214) 0.035(8) 0.057(9) 0.033(7) -0.010(6) -0.002(6) -0.003(6) C(215) 0.059(10) 0.051(9) 0.031(7) 0.002(7) 0.001(6) 0.011(6) C(216) 0.035(8) 0.049(8) 0.047(7) -0.010(6) 0.002(6) 0.000(6) C(217) 0.036(8) 0.070(10) 0.043(7) 0.001(7) 0.002(6) -0.004(6) C(221) 0.034(8) 0.056(8) 0.032(7) 0.015(6) -0.007(6) -0.010(6) C(222) 0.051(10) 0.048(8) 0.044(8) -0.003(7) -0.011(6) 0.001(6) C(223) 0.071(11) 0.049(9) 0.034(7) -0.005(8) -0.009(7) 0.010(6) C(224) 0.034(8) 0.048(8) 0.054(8) -0.005(6) 0.011(7) -0.008(7) C(225) 0.055(10) 0.044(8) 0.046(8) 0.005(7) 0.000(7) 0.005(6) C(226) 0.058(10) 0.059(9) 0.042(7) 0.016(7) 0.008(7) 0.006(6) C(227) 0.064(11) 0.070(10) 0.069(9) -0.017(8) 0.008(8) -0.007(7) C(231) 0.031(8) 0.034(7) 0.060(8) 0.002(6) 0.013(6) 0.007(6) C(232) 0.052(10) 0.051(8) 0.049(8) 0.002(7) 0.024(7) -0.008(6) C(233) 0.047(9) 0.033(7) 0.048(7) 0.011(6) 0.012(6) 0.003(6) C(234) 0.070(12) 0.045(9) 0.055(9) -0.011(8) 0.012(8) 0.012(7) C(235) 0.063(11) 0.053(9) 0.060(9) 0.001(8) 0.020(8) -0.014(7) C(236) 0.050(10) 0.027(7) 0.094(11) -0.002(6) 0.022(8) -0.004(7) C(237) 0.115(15) 0.060(10) 0.070(9) 0.003(9) 0.039(9) -0.020(8) C(241) 0.079(11) 0.035(8) 0.074(9) 0.024(7) 0.004(8) 0.006(6) C(311) 0.058(9) 0.023(7) 0.043(7) 0.007(6) 0.019(6) 0.009(5) C(312) 0.038(8) 0.046(8) 0.042(7) -0.001(6) 0.013(6) 0.012(6) C(313) 0.052(9) 0.023(6) 0.040(7) 0.006(6) 0.006(6) 0.013(5) C(314) 0.036(8) 0.034(7) 0.035(7) -0.006(6) 0.002(6) -0.002(5) C(315) 0.037(8) 0.052(8) 0.041(7) -0.013(6) 0.006(6) 0.001(6) C(316) 0.050(9) 0.026(7) 0.043(7) -0.007(6) -0.003(6) 0.003(5) C(317) 0.057(10) 0.056(9) 0.046(7) -0.005(7) 0.015(7) -0.007(6) C(321) 0.028(7) 0.028(7) 0.040(6) 0.006(5) 0.001(5) -0.005(5) C(322) 0.041(9) 0.035(7) 0.067(9) 0.013(6) 0.014(7) 0.002(6) C(323) 0.050(10) 0.063(9) 0.053(8) 0.015(7) 0.002(7) 0.003(7) C(324) 0.048(9) 0.038(8) 0.051(8) 0.016(7) 0.014(7) 0.010(6) C(325) 0.059(10) 0.039(8) 0.054(8) 0.012(7) 0.019(7) -0.009(6) C(326) 0.035(8) 0.040(8) 0.063(8) 0.013(6) 0.003(6) -0.006(6) C(327) 0.083(12) 0.054(10) 0.078(10) 0.000(8) 0.021(9) -0.012(8) C(331) 0.039(9) 0.034(7) 0.050(7) 0.006(6) -0.001(6) -0.007(6) C(332) 0.052(9) 0.049(8) 0.040(7) -0.002(7) -0.005(6) 0.017(6) C(333) 0.049(10) 0.058(9) 0.051(8) -0.011(7) 0.000(7) 0.011(7) C(334) 0.038(9) 0.036(7) 0.065(9) -0.004(6) 0.023(7) 0.006(6) C(335) 0.040(9) 0.063(9) 0.043(7) 0.000(7) -0.002(6) 0.004(7) C(336) 0.039(9) 0.071(9) 0.040(7) 0.002(7) 0.019(6) 0.009(6) C(337) 0.052(11) 0.080(11) 0.096(11) -0.031(8) 0.018(9) -0.002(9) C(341) 0.054(9) 0.044(8) 0.066(8) 0.015(7) 0.005(7) 0.016(6) C(411) 0.018(7) 0.048(7) 0.033(6) 0.009(6) -0.002(5) -0.002(6) C(412) 0.041(9) 0.047(8) 0.055(8) -0.004(7) 0.006(7) -0.001(6) C(413) 0.044(9) 0.043(8) 0.047(7) 0.003(6) 0.016(7) 0.013(6) C(414) 0.044(9) 0.046(8) 0.051(8) 0.006(7) 0.015(7) 0.002(7) C(415) 0.059(10) 0.053(9) 0.036(7) -0.007(7) -0.005(6) 0.001(6) C(416) 0.034(9) 0.053(8) 0.050(8) 0.000(6) 0.016(7) 0.015(6) C(417) 0.067(11) 0.062(10) 0.090(11) 0.002(8) 0.025(9) 0.020(9) C(421) 0.037(8) 0.032(7) 0.037(6) 0.004(6) 0.013(6) 0.003(5) C(422) 0.043(9) 0.049(8) 0.071(9) -0.006(7) 0.015(7) 0.003(7) C(423) 0.076(12) 0.058(10) 0.074(10) -0.005(9) 0.031(9) -0.028(8) C(424) 0.082(13) 0.038(8) 0.051(9) -0.013(8) 0.032(9) 0.003(7) C(425) 0.053(10) 0.058(9) 0.041(7) 0.010(7) -0.001(7) 0.002(7) C(426) 0.066(11) 0.046(8) 0.045(8) 0.019(7) 0.007(7) 0.015(6) C(427) 0.127(16) 0.065(10) 0.049(8) -0.009(10) 0.021(9) -0.013(7) C(431) 0.033(8) 0.041(8) 0.044(7) -0.003(6) -0.005(6) 0.000(6) C(432) 0.047(9) 0.040(7) 0.039(7) -0.004(6) -0.003(6) 0.006(6) C(433) 0.066(11) 0.064(10) 0.035(7) -0.013(8) 0.011(7) 0.003(7) C(434) 0.053(10) 0.064(10) 0.032(7) -0.002(7) 0.005(7) -0.006(7) C(435) 0.061(10) 0.051(8) 0.039(7) 0.019(7) 0.012(7) 0.002(6) C(436) 0.061(10) 0.052(9) 0.042(7) 0.011(7) 0.015(7) 0.007(6) C(437) 0.068(12) 0.107(13) 0.058(9) 0.047(10) 0.019(8) 0.017(8) C(441) 0.054(10) 0.043(8) 0.068(8) 0.015(7) 0.011(7) 0.021(6) # 10. MOLECULAR GEOMETRY _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_publ_flag Re(1A) Re(2A) 2.2231(6) ? Re(1A) Cl(11) 2.319(3) ? Re(1A) Cl(12) 2.320(3) ? Re(1A) Cl(14) 2.325(3) ? Re(1A) Cl(13) 2.339(3) ? Re(2A) Cl(21) 2.324(3) ? Re(2A) Cl(23) 2.326(3) ? Re(2A) Cl(22) 2.326(3) ? Re(2A) Cl(24) 2.330(3) ? Re(1B) Re(2B) 2.207(11) ? Re(1B) Cl(12) 2.314(9) ? Re(1B) Cl(24) 2.332(7) ? Re(1B) Cl(13) 2.388(7) ? Re(1B) Cl(21) 2.397(8) ? Re(2B) Cl(11) 2.339(8) ? Re(2B) Cl(14) 2.345(8) ? Re(2B) Cl(23) 2.351(8) ? Re(2B) Cl(22) 2.383(9) ? Re(3A) Re(4A) 2.2153(7) ? Re(3A) Cl(34) 2.302(3) ? Re(3A) Cl(33) 2.309(3) ? Re(3A) Cl(31) 2.331(4) ? Re(3A) Cl(32) 2.333(3) ? Re(4A) Cl(44) 2.300(3) ? Re(4A) Cl(41) 2.303(3) ? Re(4A) Cl(43) 2.319(4) ? Re(4A) Cl(42) 2.328(3) ? Re(3B) Re(4B) 2.182(5) ? Re(3B) Cl(34) 2.279(5) ? Re(3B) Cl(33) 2.339(5) ? Re(3B) Cl(42) 2.374(4) ? Re(3B) Cl(43) 2.410(5) ? Re(4B) Cl(44) 2.283(5) ? Re(4B) Cl(41) 2.310(5) ? Re(4B) Cl(32) 2.381(4) ? Re(4B) Cl(31) 2.399(5) ? P(1) C(121) 1.784(12) ? P(1) C(111) 1.784(11) ? P(1) C(131) 1.800(11) ? P(1) C(141) 1.808(10) ? P(2) C(211) 1.770(11) ? P(2) C(221) 1.778(13) ? P(2) C(231) 1.783(12) ? P(2) C(241) 1.783(10) ? P(3) C(331) 1.768(12) ? P(3) C(321) 1.795(10) ? P(3) C(341) 1.804(10) ? P(3) C(311) 1.810(11) ? P(4) C(431) 1.779(12) ? P(4) C(411) 1.779(11) ? P(4) C(421) 1.790(11) ? P(4) C(441) 1.795(10) ? O(117) C(114) 1.369(14) ? O(117) C(117) 1.417(14) ? O(127) C(124) 1.352(13) ? O(127) C(127) 1.450(11) ? O(137) C(134) 1.365(13) ? O(137) C(137) 1.394(14) ? O(217) C(214) 1.346(13) ? O(217) C(217) 1.426(12) ? O(227) C(224) 1.356(13) ? O(227) C(227) 1.393(13) ? O(237) C(234) 1.379(14) ? O(237) C(237) 1.402(13) ? O(317) C(314) 1.349(12) ? O(317) C(317) 1.426(12) ? O(327) C(324) 1.356(13) ? O(327) C(327) 1.407(13) ? O(337) C(334) 1.366(13) ? O(337) C(337) 1.408(13) ? O(417) C(414) 1.372(14) ? O(417) C(417) 1.436(12) ? O(427) C(424) 1.358(15) ? O(427) C(427) 1.404(14) ? O(437) C(434) 1.351(14) ? O(437) C(437) 1.439(14) ? C(111) C(116) 1.382(14) ? C(111) C(112) 1.404(14) ? C(112) C(113) 1.373(16) ? C(113) C(114) 1.360(16) ? C(114) C(115) 1.385(15) ? C(115) C(116) 1.372(15) ? C(121) C(126) 1.373(14) ? C(121) C(122) 1.424(15) ? C(122) C(123) 1.339(15) ? C(123) C(124) 1.369(14) ? C(124) C(125) 1.386(15) ? C(125) C(126) 1.348(15) ? C(131) C(132) 1.386(15) ? C(131) C(135) 1.388(14) ? C(132) C(133) 1.371(14) ? C(133) C(134) 1.375(15) ? C(134) C(136) 1.412(16) ? C(135) C(136) 1.345(14) ? C(211) C(212) 1.388(14) ? C(211) C(216) 1.410(14) ? C(212) C(213) 1.378(15) ? C(213) C(214) 1.398(14) ? C(214) C(215) 1.400(15) ? C(215) C(216) 1.381(15) ? C(221) C(222) 1.370(14) ? C(221) C(226) 1.396(15) ? C(222) C(223) 1.371(16) ? C(223) C(224) 1.398(15) ? C(224) C(225) 1.341(15) ? C(225) C(226) 1.350(16) ? C(231) C(232) 1.355(15) ? C(231) C(236) 1.385(15) ? C(232) C(233) 1.398(14) ? C(233) C(234) 1.381(16) ? C(234) C(235) 1.383(17) ? C(235) C(236) 1.400(16) ? C(311) C(312) 1.361(14) ? C(311) C(316) 1.394(13) ? C(312) C(313) 1.356(14) ? C(313) C(314) 1.402(14) ? C(314) C(315) 1.357(14) ? C(315) C(316) 1.403(15) ? C(321) C(322) 1.387(14) ? C(321) C(326) 1.402(14) ? C(322) C(323) 1.392(15) ? C(323) C(324) 1.394(15) ? C(324) C(325) 1.386(16) ? C(325) C(326) 1.365(14) ? C(331) C(336) 1.377(15) ? C(331) C(332) 1.394(13) ? C(332) C(333) 1.371(15) ? C(333) C(334) 1.355(16) ? C(334) C(335) 1.385(14) ? C(335) C(336) 1.386(15) ? C(411) C(412) 1.370(14) ? C(411) C(416) 1.380(14) ? C(412) C(413) 1.380(15) ? C(413) C(414) 1.397(15) ? C(414) C(415) 1.392(14) ? C(415) C(416) 1.365(15) ? C(421) C(422) 1.383(15) ? C(421) C(426) 1.384(15) ? C(422) C(423) 1.385(16) ? C(423) C(424) 1.361(18) ? C(424) C(425) 1.379(16) ? C(425) C(426) 1.380(15) ? C(431) C(432) 1.384(14) ? C(431) C(436) 1.387(15) ? C(432) C(433) 1.393(15) ? C(433) C(434) 1.376(16) ? C(434) C(435) 1.386(15) ? C(435) C(436) 1.393(15) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag Re(2A) Re(1A) Cl(11) 104.17(8) ? Re(2A) Re(1A) Cl(12) 103.62(7) ? Cl(11) Re(1A) Cl(12) 87.69(11) ? Re(2A) Re(1A) Cl(14) 102.65(7) ? Cl(11) Re(1A) Cl(14) 87.04(10) ? Cl(12) Re(1A) Cl(14) 153.71(10) ? Re(2A) Re(1A) Cl(13) 104.18(7) ? Cl(11) Re(1A) Cl(13) 151.64(10) ? Cl(12) Re(1A) Cl(13) 85.87(11) ? Cl(14) Re(1A) Cl(13) 86.64(10) ? Re(1A) Re(2A) Cl(21) 104.20(7) ? Re(1A) Re(2A) Cl(23) 103.90(7) ? Cl(21) Re(2A) Cl(23) 151.89(10) ? Re(1A) Re(2A) Cl(22) 104.17(7) ? Cl(21) Re(2A) Cl(22) 86.97(10) ? Cl(23) Re(2A) Cl(22) 86.74(11) ? Re(1A) Re(2A) Cl(24) 102.33(7) ? Cl(21) Re(2A) Cl(24) 86.79(10) ? Cl(23) Re(2A) Cl(24) 86.73(10) ? Cl(22) Re(2A) Cl(24) 153.50(10) ? Re(2B) Re(1B) Cl(12) 103.6(4) ? Re(2B) Re(1B) Cl(24) 102.7(4) ? Cl(12) Re(1B) Cl(24) 89.4(3) ? Re(2B) Re(1B) Cl(13) 102.6(4) ? Cl(12) Re(1B) Cl(13) 84.9(3) ? Cl(24) Re(1B) Cl(13) 154.6(4) ? Re(2B) Re(1B) Cl(21) 102.2(4) ? Cl(12) Re(1B) Cl(21) 154.2(4) ? Cl(24) Re(1B) Cl(21) 85.1(3) ? Cl(13) Re(1B) Cl(21) 89.4(3) ? Re(1B) Re(2B) Cl(11) 101.4(4) ? Re(1B) Re(2B) Cl(14) 101.6(3) ? Cl(11) Re(2B) Cl(14) 86.1(3) ? Re(1B) Re(2B) Cl(23) 101.7(4) ? Cl(11) Re(2B) Cl(23) 91.2(3) ? Cl(14) Re(2B) Cl(23) 156.7(4) ? Re(1B) Re(2B) Cl(22) 101.8(4) ? Cl(11) Re(2B) Cl(22) 156.8(4) ? Cl(14) Re(2B) Cl(22) 88.6(3) ? Cl(23) Re(2B) Cl(22) 84.9(3) ? Re(4A) Re(3A) Cl(34) 104.56(9) ? Re(4A) Re(3A) Cl(33) 105.21(9) ? Cl(34) Re(3A) Cl(33) 87.37(14) ? Re(4A) Re(3A) Cl(31) 102.42(11) ? Cl(34) Re(3A) Cl(31) 86.93(17) ? Cl(33) Re(3A) Cl(31) 152.34(13) ? Re(4A) Re(3A) Cl(32) 102.44(8) ? Cl(34) Re(3A) Cl(32) 152.91(12) ? Cl(33) Re(3A) Cl(32) 87.63(12) ? Cl(31) Re(3A) Cl(32) 85.26(14) ? Re(3A) Re(4A) Cl(44) 104.01(8) ? Re(3A) Re(4A) Cl(41) 105.35(10) ? Cl(44) Re(4A) Cl(41) 87.24(15) ? Re(3A) Re(4A) Cl(43) 102.45(10) ? Cl(44) Re(4A) Cl(43) 86.72(17) ? Cl(41) Re(4A) Cl(43) 152.19(14) ? Re(3A) Re(4A) Cl(42) 102.31(9) ? Cl(44) Re(4A) Cl(42) 153.64(12) ? Cl(41) Re(4A) Cl(42) 87.28(14) ? Cl(43) Re(4A) Cl(42) 86.20(16) ? Re(4B) Re(3B) Cl(34) 106.5(2) ? Re(4B) Re(3B) Cl(33) 104.81(17) ? Cl(34) Re(3B) Cl(33) 87.21(16) ? Re(4B) Re(3B) Cl(42) 100.11(18) ? Cl(34) Re(3B) Cl(42) 90.02(18) ? Cl(33) Re(3B) Cl(42) 154.68(19) ? Re(4B) Re(3B) Cl(43) 98.51(19) ? Cl(34) Re(3B) Cl(43) 154.9(2) ? Cl(33) Re(3B) Cl(43) 88.75(18) ? Cl(42) Re(3B) Cl(43) 83.16(17) ? Re(3B) Re(4B) Cl(44) 105.9(2) ? Re(3B) Re(4B) Cl(41) 104.87(18) ? Cl(44) Re(4B) Cl(41) 87.49(18) ? Re(3B) Re(4B) Cl(32) 100.34(18) ? Cl(44) Re(4B) Cl(32) 89.21(17) ? Cl(41) Re(4B) Cl(32) 154.5(2) ? Re(3B) Re(4B) Cl(31) 98.4(2) ? Cl(44) Re(4B) Cl(31) 155.4(2) ? Cl(41) Re(4B) Cl(31) 89.91(19) ? Cl(32) Re(4B) Cl(31) 82.73(16) ? Re(1A) Cl(11) Re(2B) 39.5(2) ? Re(1B) Cl(12) Re(1A) 38.86(19) ? Re(1A) Cl(13) Re(1B) 38.05(19) ? Re(1A) Cl(14) Re(2B) 39.4(2) ? Re(2A) Cl(21) Re(1B) 38.73(19) ? Re(2A) Cl(22) Re(2B) 39.3(2) ? Re(2A) Cl(23) Re(2B) 39.56(19) ? Re(2A) Cl(24) Re(1B) 39.3(2) ? Re(3A) Cl(31) Re(4B) 40.26(10) ? Re(3A) Cl(32) Re(4B) 40.41(10) ? Re(3A) Cl(33) Re(3B) 37.05(10) ? Re(3B) Cl(34) Re(3A) 37.61(10) ? Re(4A) Cl(41) Re(4B) 37.65(10) ? Re(4A) Cl(42) Re(3B) 40.24(9) ? Re(4A) Cl(43) Re(3B) 39.96(10) ? Re(4B) Cl(44) Re(4A) 37.90(10) ? C(121) P(1) C(111) 111.7(5) ? C(121) P(1) C(131) 107.9(5) ? C(111) P(1) C(131) 108.6(5) ? C(121) P(1) C(141) 108.1(6) ? C(111) P(1) C(141) 110.3(5) ? C(131) P(1) C(141) 110.3(5) ? C(211) P(2) C(221) 109.6(5) ? C(211) P(2) C(231) 112.9(6) ? C(221) P(2) C(231) 107.2(5) ? C(211) P(2) C(241) 108.5(5) ? C(221) P(2) C(241) 109.8(6) ? C(231) P(2) C(241) 108.9(5) ? C(331) P(3) C(321) 106.6(5) ? C(331) P(3) C(341) 109.3(6) ? C(321) P(3) C(341) 110.6(5) ? C(331) P(3) C(311) 111.1(5) ? C(321) P(3) C(311) 110.6(5) ? C(341) P(3) C(311) 108.6(5) ? C(431) P(4) C(411) 109.0(5) ? C(431) P(4) C(421) 109.8(5) ? C(411) P(4) C(421) 109.2(5) ? C(431) P(4) C(441) 109.7(5) ? C(411) P(4) C(441) 109.2(6) ? C(421) P(4) C(441) 109.9(5) ? C(114) O(117) C(117) 119.0(10) ? C(124) O(127) C(127) 118.0(9) ? C(134) O(137) C(137) 118.8(10) ? C(214) O(217) C(217) 116.8(9) ? C(224) O(227) C(227) 117.8(9) ? C(234) O(237) C(237) 118.4(11) ? C(314) O(317) C(317) 119.1(9) ? C(324) O(327) C(327) 118.2(10) ? C(334) O(337) C(337) 117.8(10) ? C(414) O(417) C(417) 117.3(10) ? C(424) O(427) C(427) 118.9(12) ? C(434) O(437) C(437) 117.8(10) ? C(116) C(111) C(112) 118.6(11) ? C(116) C(111) P(1) 121.1(8) ? C(112) C(111) P(1) 120.1(9) ? C(113) C(112) C(111) 120.1(12) ? C(114) C(113) C(112) 119.5(12) ? C(113) C(114) O(117) 116.2(12) ? C(113) C(114) C(115) 122.2(13) ? O(117) C(114) C(115) 121.6(13) ? C(116) C(115) C(114) 117.9(12) ? C(115) C(116) C(111) 121.7(11) ? C(126) C(121) C(122) 116.2(11) ? C(126) C(121) P(1) 122.9(10) ? C(122) C(121) P(1) 120.9(9) ? C(123) C(122) C(121) 120.5(10) ? C(122) C(123) C(124) 121.8(11) ? O(127) C(124) C(123) 117.1(10) ? O(127) C(124) C(125) 124.3(11) ? C(123) C(124) C(125) 118.6(11) ? C(126) C(125) C(124) 119.9(11) ? C(125) C(126) C(121) 123.0(11) ? C(132) C(131) C(135) 119.4(11) ? C(132) C(131) P(1) 120.3(9) ? C(135) C(131) P(1) 120.2(9) ? C(133) C(132) C(131) 119.2(11) ? C(132) C(133) C(134) 120.8(12) ? O(137) C(134) C(133) 116.5(12) ? O(137) C(134) C(136) 123.4(12) ? C(133) C(134) C(136) 120.1(11) ? C(136) C(135) C(131) 122.2(12) ? C(135) C(136) C(134) 118.3(11) ? C(212) C(211) C(216) 118.1(10) ? C(212) C(211) P(2) 121.0(9) ? C(216) C(211) P(2) 120.9(9) ? C(213) C(212) C(211) 122.6(10) ? C(212) C(213) C(214) 119.0(11) ? O(217) C(214) C(213) 125.5(11) ? O(217) C(214) C(215) 115.0(10) ? C(213) C(214) C(215) 119.5(12) ? C(216) C(215) C(214) 120.8(11) ? C(215) C(216) C(211) 120.0(11) ? C(222) C(221) C(226) 116.5(12) ? C(222) C(221) P(2) 120.6(9) ? C(226) C(221) P(2) 122.8(9) ? C(221) C(222) C(223) 122.9(12) ? C(222) C(223) C(224) 117.9(11) ? C(225) C(224) O(227) 126.7(12) ? C(225) C(224) C(223) 120.1(12) ? O(227) C(224) C(223) 113.2(11) ? C(224) C(225) C(226) 121.1(13) ? C(225) C(226) C(221) 121.3(12) ? C(232) C(231) C(236) 119.9(12) ? C(232) C(231) P(2) 120.7(9) ? C(236) C(231) P(2) 119.4(10) ? C(231) C(232) C(233) 121.3(11) ? C(234) C(233) C(232) 118.4(12) ? O(237) C(234) C(233) 116.1(13) ? O(237) C(234) C(235) 122.4(13) ? C(233) C(234) C(235) 121.4(13) ? C(234) C(235) C(236) 118.5(13) ? C(231) C(236) C(235) 120.4(13) ? C(312) C(311) C(316) 119.8(10) ? C(312) C(311) P(3) 121.5(8) ? C(316) C(311) P(3) 118.7(8) ? C(313) C(312) C(311) 121.7(10) ? C(312) C(313) C(314) 119.4(10) ? O(317) C(314) C(315) 115.2(10) ? O(317) C(314) C(313) 124.7(10) ? C(315) C(314) C(313) 120.0(11) ? C(314) C(315) C(316) 120.3(11) ? C(311) C(316) C(315) 118.8(10) ? C(322) C(321) C(326) 118.9(10) ? C(322) C(321) P(3) 122.6(8) ? C(326) C(321) P(3) 118.3(9) ? C(321) C(322) C(323) 120.3(11) ? C(322) C(323) C(324) 119.8(12) ? O(327) C(324) C(325) 125.1(11) ? O(327) C(324) C(323) 115.1(11) ? C(325) C(324) C(323) 119.8(12) ? C(326) C(325) C(324) 120.3(11) ? C(325) C(326) C(321) 120.9(11) ? C(336) C(331) C(332) 119.0(11) ? C(336) C(331) P(3) 121.0(9) ? C(332) C(331) P(3) 120.0(9) ? C(333) C(332) C(331) 119.6(12) ? C(334) C(333) C(332) 121.0(12) ? C(333) C(334) O(337) 115.7(11) ? C(333) C(334) C(335) 120.7(12) ? O(337) C(334) C(335) 123.5(12) ? C(334) C(335) C(336) 118.5(12) ? C(331) C(336) C(335) 121.1(11) ? C(412) C(411) C(416) 118.0(11) ? C(412) C(411) P(4) 122.0(9) ? C(416) C(411) P(4) 120.0(8) ? C(411) C(412) C(413) 123.0(12) ? C(412) C(413) C(414) 118.0(11) ? O(417) C(414) C(415) 116.9(12) ? O(417) C(414) C(413) 123.7(11) ? C(415) C(414) C(413) 119.4(12) ? C(416) C(415) C(414) 120.4(12) ? C(415) C(416) C(411) 121.1(11) ? C(422) C(421) C(426) 117.6(11) ? C(422) C(421) P(4) 120.0(10) ? C(426) C(421) P(4) 122.3(9) ? C(421) C(422) C(423) 120.6(13) ? C(424) C(423) C(422) 120.8(13) ? O(427) C(424) C(423) 125.1(13) ? O(427) C(424) C(425) 114.9(14) ? C(423) C(424) C(425) 119.9(14) ? C(424) C(425) C(426) 119.1(13) ? C(425) C(426) C(421) 122.1(12) ? C(432) C(431) C(436) 118.4(11) ? C(432) C(431) P(4) 122.2(9) ? C(436) C(431) P(4) 119.2(9) ? C(431) C(432) C(433) 119.2(11) ? C(434) C(433) C(432) 122.1(11) ? O(437) C(434) C(433) 116.1(12) ? O(437) C(434) C(435) 124.5(12) ? C(433) C(434) C(435) 119.4(12) ? C(434) C(435) C(436) 118.3(12) ? C(431) C(436) C(435) 122.6(11) ? #===END