# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2001 # CCDC Number: 186/2294 data_global #==================================================================== _audit_creation_date 19-09-00 _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 10 _journal_year 2000 _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 'WALTON' ; Department of Chemistry Purdue University W. Lafayette IN 47907 USA ; ; ? ; '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 'J0134Q' _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_J0134Q # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description chunk _exptl_crystal_colour green _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.25 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C52 H46 Cl5 P4 Re2' _chemical_formula_structural ? _chemical_formula_weight 1344.51 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'c 1 2/c 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 22.9626(4) _cell_length_b 10.8638(3) _cell_length_c 21.7099(6) _cell_angle_alpha 90.00 _cell_angle_beta 118.7103(12) _cell_angle_gamma 90.00 _cell_volume 4750.0(4) _cell_measurement_reflns_used 20529 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_formula_units_z 4 _exptl_crystal_density_diffrn 1.88 _exptl_crystal_density_meas ? _diffrn_radiation_type MO-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 5.616 _cell_measurement_temperature 150 _exptl_crystal_F_000 2612 # 6. DATA COLLECTION _diffrn_ambient_temperature 150 _diffrn_measurement_device_type ? _exptl_absorpt_correction_type refined_empirical_(Otwinowski_&_Minor,_1996 _exptl_absorpt_correction_T_min 0.1529 _exptl_absorpt_correction_T_max 0.2456 _diffrn_reflns_number 20529 _reflns_number_total 5025 _reflns_number_gt 4162 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.058 _diffrn_reflns_theta_min 5.00 _diffrn_reflns_theta_max 27.47 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_max 28 # 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 0.088 _refine_ls_hydrogen_treatment ; Chemically significant hydrogens refined isotropically Others riding, U=1.3*Ueq of bonding atom ; _refine_ls_number_reflns 5024 _refine_ls_number_parameters 305 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0382P)^2^+12.6138P] where P=(Fo^2^+2Fc^2^)/' _refine_ls_shift/su_max 0.002 _refine_diff_density_max 1.07 _refine_diff_density_min -1.30 _refine_ls_extinction_method SHELXL97_(Sheldrick_1997) _refine_ls_extinction_coef 0.99E-03 _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 0.212943(11) 0.20102(2) 0.025463(13) 0.03937(12) Uani ? Cl(1) 0.16586(12) 0.2589(3) 0.09864(12) 0.0824(10) Uani ? Cl(2) 0.15947(9) 0.00748(19) 0.01928(15) 0.0837(10) Uani ? Cl(12) 0.2406(3) 0.1046(5) -0.0540(3) 0.037(2) Uani ? P(1) 0.30860(8) 0.11463(15) 0.13117(8) 0.0381(6) Uani ? P(2) 0.10623(7) 0.27173(15) -0.07243(9) 0.0372(6) Uani ? C(1) 0.2278(8) 0.3988(14) 0.0150(9) 0.037(5) Uani ? C(2) 0.2827(10) 0.3613(19) 0.0691(11) 0.033(7) Uani ? C(1B) 0.3853(4) 0.1976(7) 0.1506(4) 0.054(3) Uani ? C(111) 0.3028(3) 0.1284(6) 0.2121(3) 0.043(2) Uani ? C(112) 0.3300(3) 0.2248(6) 0.2586(4) 0.050(3) Uani ? C(113) 0.3207(4) 0.2319(8) 0.3172(4) 0.059(3) Uani ? C(114) 0.2856(4) 0.1442(10) 0.3299(4) 0.072(4) Uani ? C(115) 0.2601(6) 0.0473(12) 0.2838(5) 0.110(6) Uani ? C(116) 0.2676(5) 0.0397(11) 0.2257(5) 0.096(5) Uani ? C(121) 0.3341(3) -0.0460(7) 0.1346(4) 0.055(3) Uani ? C(122) 0.3067(4) -0.1248(8) 0.0804(5) 0.081(4) Uani ? C(123) 0.3302(6) -0.2449(9) 0.0868(7) 0.103(6) Uani ? C(124) 0.3793(7) -0.2858(10) 0.1431(9) 0.127(7) Uani ? C(125) 0.4119(10) -0.2054(14) 0.1963(9) 0.189(10) Uani ? C(126) 0.3911(6) -0.0859(11) 0.1916(7) 0.140(6) Uani ? C(211) 0.0391(3) 0.1569(6) -0.1034(3) 0.042(2) Uani ? C(212) 0.0070(4) 0.1421(8) -0.0638(4) 0.066(3) Uani ? C(213) -0.0432(4) 0.0542(8) -0.0842(5) 0.069(4) Uani ? C(214) -0.0602(4) -0.0186(8) -0.1414(5) 0.064(3) Uani ? C(215) -0.0292(4) -0.0045(7) -0.1792(5) 0.067(4) Uani ? C(216) 0.0222(4) 0.0838(7) -0.1604(4) 0.054(3) Uani ? C(221) 0.0637(3) 0.4101(6) -0.0667(3) 0.043(2) Uani ? C(222) 0.0917(3) 0.4946(6) -0.0131(4) 0.048(2) Uani ? C(223) 0.0587(4) 0.6038(7) -0.0153(4) 0.060(3) Uani ? C(224) -0.0040(4) 0.6256(9) -0.0701(5) 0.072(4) Uani ? C(225) -0.0333(4) 0.5407(10) -0.1221(5) 0.083(4) Uani ? C(226) -0.0013(4) 0.4328(8) -0.1218(4) 0.068(3) Uani ? H(1) 0.207(7) 0.469(14) 0.005(7) 0.0480 Uiso ? H(2) 0.310(7) 0.375(13) 0.106(7) 0.0420 Uiso ? H(112) 0.3544 0.2850 0.2508 0.0650 Uiso calc H(113) 0.3388 0.2975 0.3482 0.0770 Uiso calc H(114) 0.2790 0.1497 0.3688 0.0940 Uiso calc H(115) 0.2371 -0.0145 0.2927 0.1440 Uiso calc H(116) 0.2490 -0.0259 0.1948 0.1250 Uiso calc H(122) 0.2715 -0.0988 0.0380 0.1050 Uiso calc H(123) 0.3093 -0.2976 0.0486 0.1340 Uiso calc H(124) 0.3922 -0.3678 0.1472 0.1650 Uiso calc H(125) 0.4490 -0.2318 0.2370 0.2460 Uiso calc H(126) 0.4161 -0.0310 0.2276 0.1820 Uiso calc H(1B1) 0.3861 0.2752 0.1731 0.0710 Uiso calc H(1B2) 0.4231 0.1495 0.1835 0.0710 Uiso calc H(212) 0.0187 0.1902 -0.0241 0.0860 Uiso calc H(213) -0.0655 0.0451 -0.0583 0.0900 Uiso calc H(214) -0.0932 -0.0778 -0.1539 0.0820 Uiso calc H(215) -0.0415 -0.0533 -0.2188 0.0870 Uiso calc H(216) 0.0441 0.0916 -0.1868 0.0700 Uiso calc H(222) 0.1331 0.4788 0.0251 0.0620 Uiso calc H(223) 0.0790 0.6618 0.0203 0.0780 Uiso calc H(224) -0.0262 0.6980 -0.0714 0.0940 Uiso calc H(225) -0.0757 0.5557 -0.1588 0.1070 Uiso calc H(226) -0.0223 0.3755 -0.1576 0.0890 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 0.03259(16) 0.04193(18) 0.04734(19) 0.01145(11) 0.02219(12) 0.00933(13) Cl(1) 0.0875(15) 0.1157(18) 0.0732(14) 0.0606(14) 0.0619(13) 0.0405(13) Cl(2) 0.0490(10) 0.0541(12) 0.160(2) 0.0142(9) 0.0597(13) 0.0430(13) Cl(12) 0.028(3) 0.033(2) 0.048(3) 0.0060(18) 0.017(3) -0.003(2) P(1) 0.0360(8) 0.0337(9) 0.0403(9) 0.0025(6) 0.0150(7) 0.0018(7) P(2) 0.0286(7) 0.0409(10) 0.0419(9) 0.0036(6) 0.0168(7) -0.0040(7) C(1) 0.023(7) 0.039(8) 0.034(8) 0.005(6) 0.001(6) -0.010(7) C(2) 0.026(10) 0.042(11) 0.032(10) -0.005(7) 0.015(9) -0.014(8) C(1B) 0.052(4) 0.067(5) 0.051(4) -0.015(4) 0.030(3) -0.005(4) C(111) 0.036(3) 0.045(4) 0.045(4) -0.004(3) 0.016(3) 0.007(3) C(112) 0.051(4) 0.046(4) 0.059(4) -0.002(3) 0.031(4) 0.003(3) C(113) 0.060(5) 0.070(5) 0.049(4) 0.000(4) 0.028(4) -0.007(4) C(114) 0.066(5) 0.113(8) 0.044(4) -0.015(5) 0.032(4) 0.004(5) C(115) 0.132(9) 0.149(11) 0.069(6) -0.078(8) 0.064(6) -0.012(7) C(116) 0.110(7) 0.119(8) 0.060(6) -0.075(6) 0.042(5) -0.014(5) C(121) 0.048(4) 0.041(4) 0.056(4) 0.007(3) 0.010(3) 0.005(3) C(122) 0.074(6) 0.053(5) 0.085(6) 0.022(4) 0.014(5) -0.012(5) C(123) 0.099(8) 0.044(5) 0.144(10) 0.017(5) 0.041(8) -0.021(6) C(124) 0.124(10) 0.050(6) 0.171(13) 0.050(7) 0.043(10) 0.018(8) C(125) 0.207(18) 0.086(10) 0.159(15) 0.090(11) -0.005(13) 0.015(10) C(126) 0.118(9) 0.069(7) 0.131(10) 0.034(7) -0.021(8) 0.013(7) C(211) 0.033(3) 0.049(4) 0.042(4) 0.002(3) 0.016(3) 0.003(3) C(212) 0.054(4) 0.086(6) 0.075(5) -0.018(4) 0.045(4) -0.021(5) C(213) 0.052(4) 0.081(6) 0.088(6) -0.001(4) 0.045(5) 0.012(5) C(214) 0.050(4) 0.066(5) 0.071(5) -0.006(4) 0.026(4) 0.014(4) C(215) 0.076(5) 0.048(5) 0.070(5) -0.021(4) 0.029(5) -0.009(4) C(216) 0.058(4) 0.052(4) 0.061(5) -0.014(3) 0.035(4) -0.008(4) C(221) 0.037(3) 0.050(4) 0.043(4) 0.013(3) 0.020(3) 0.004(3) C(222) 0.040(3) 0.051(4) 0.049(4) 0.008(3) 0.019(3) -0.004(3) C(223) 0.060(4) 0.046(4) 0.076(5) 0.018(4) 0.035(4) -0.008(4) C(224) 0.081(6) 0.076(6) 0.069(6) 0.039(5) 0.043(5) 0.014(5) C(225) 0.055(5) 0.099(7) 0.082(6) 0.048(5) 0.023(5) 0.022(6) C(226) 0.053(4) 0.080(6) 0.048(4) 0.021(4) 0.005(4) -0.004(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 C(1) 2.205(15) ? Re C(2) 2.208(19) ? Re C(1) 2.224(14) ? Re C(2) 2.24(2) ? Re Cl(12) 2.312(5) ? Re Cl(12) 2.351(5) ? Re Cl(1) 2.3954(18) ? Re Cl(2) 2.4058(19) ? Re P(2) 2.4714(16) ? Re P(1) 2.4757(16) ? Re Re 2.6567(5) ? Cl(12) C(2) 0.603(18) ? Cl(12) C(1) 0.808(15) ? Cl(12) H(2) 1.19(14) ? Cl(12) H(1) 1.42(14) ? Cl(12) Re 2.312(5) ? P(1) C(121) 1.831(7) ? P(1) C(111) 1.832(7) ? P(1) C(1B) 1.839(7) ? P(2) C(1B) 1.829(7) ? P(2) C(221) 1.829(6) ? P(2) C(211) 1.840(7) ? C(1) Cl(12) 0.808(15) ? C(1) H(1) 0.88(15) ? C(1) C(2) 1.31(2) ? C(1) Re 2.224(14) ? H(1) Cl(12) 1.42(14) ? C(2) Cl(12) 0.602(18) ? C(2) H(2) 0.76(14) ? C(2) Re 2.208(19) ? H(2) Cl(12) 1.19(14) ? C(1B) P(2) 1.829(7) ? C(111) C(116) 1.377(9) ? C(111) C(112) 1.378(9) ? C(112) C(113) 1.388(10) ? C(113) C(114) 1.359(11) ? C(114) C(115) 1.375(13) ? C(115) C(116) 1.356(13) ? C(121) C(122) 1.341(11) ? C(121) C(126) 1.370(12) ? C(122) C(123) 1.393(12) ? C(123) C(124) 1.279(16) ? C(124) C(125) 1.352(18) ? C(125) C(126) 1.369(15) ? C(211) C(216) 1.360(9) ? C(211) C(212) 1.385(9) ? C(212) C(213) 1.396(11) ? C(213) C(214) 1.361(11) ? C(214) C(215) 1.329(11) ? C(215) C(216) 1.421(10) ? C(221) C(222) 1.375(9) ? C(221) C(226) 1.416(9) ? C(222) C(223) 1.396(9) ? C(223) C(224) 1.377(11) ? C(224) C(225) 1.360(12) ? C(225) C(226) 1.381(11) ? 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 C(1) Re C(2) 97.2(7) ? C(1) Re C(1) 106.3(4) ? C(2) Re C(1) 34.3(5) ? C(1) Re C(2) 34.2(5) ? C(2) Re C(2) 106.7(6) ? C(1) Re C(2) 95.6(6) ? C(1) Re Cl(12) 20.4(4) ? C(2) Re Cl(12) 107.9(6) ? C(1) Re Cl(12) 105.1(4) ? C(2) Re Cl(12) 15.1(5) ? C(1) Re Cl(12) 104.4(4) ? C(2) Re Cl(12) 14.8(5) ? C(1) Re Cl(12) 20.1(4) ? C(2) Re Cl(12) 105.4(5) ? Cl(12) Re Cl(12) 110.54(15) ? C(1) Re Cl(1) 87.4(4) ? C(2) Re Cl(1) 158.9(5) ? C(1) Re Cl(1) 161.2(5) ? C(2) Re Cl(1) 88.6(5) ? Cl(12) Re Cl(1) 83.12(15) ? Cl(12) Re Cl(1) 166.02(15) ? C(1) Re Cl(2) 161.1(4) ? C(2) Re Cl(2) 86.0(5) ? C(1) Re Cl(2) 86.8(4) ? C(2) Re Cl(2) 160.6(6) ? Cl(12) Re Cl(2) 166.07(15) ? Cl(12) Re Cl(2) 83.10(14) ? Cl(1) Re Cl(2) 83.42(10) ? C(1) Re P(2) 75.4(5) ? C(2) Re P(2) 76.4(6) ? C(1) Re P(2) 110.7(5) ? C(2) Re P(2) 109.5(6) ? Cl(12) Re P(2) 94.93(15) ? Cl(12) Re P(2) 90.75(15) ? Cl(1) Re P(2) 84.94(6) ? Cl(2) Re P(2) 87.42(6) ? C(1) Re P(1) 110.6(5) ? C(2) Re P(1) 109.2(6) ? C(1) Re P(1) 75.1(5) ? C(2) Re P(1) 76.5(6) ? Cl(12) Re P(1) 90.47(16) ? Cl(12) Re P(1) 94.54(15) ? Cl(1) Re P(1) 88.10(6) ? Cl(2) Re P(1) 85.54(7) ? P(2) Re P(1) 170.62(5) ? C(1) Re Re 53.5(4) ? C(2) Re Re 54.0(5) ? C(1) Re Re 52.8(4) ? C(2) Re Re 52.7(5) ? Cl(12) Re Re 55.95(13) ? Cl(12) Re Re 54.60(13) ? Cl(1) Re Re 138.96(7) ? Cl(2) Re Re 137.61(6) ? P(2) Re Re 94.96(4) ? P(1) Re Re 94.42(4) ? C(2) Cl(12) C(1) 136(3) ? C(2) Cl(12) H(2) 33(7) ? C(1) Cl(12) H(2) 168(7) ? C(2) Cl(12) H(1) 167(6) ? C(1) Cl(12) H(1) 34(6) ? H(2) Cl(12) H(1) 156(9) ? C(2) Cl(12) Re 76(2) ? C(1) Cl(12) Re 72.3(12) ? H(2) Cl(12) Re 102(7) ? H(1) Cl(12) Re 101(6) ? C(2) Cl(12) Re 69(2) ? C(1) Cl(12) Re 71.1(11) ? H(2) Cl(12) Re 98(7) ? H(1) Cl(12) Re 98(5) ? Re Cl(12) Re 69.46(15) ? C(121) P(1) C(111) 102.0(3) ? C(121) P(1) C(1B) 101.8(4) ? C(111) P(1) C(1B) 104.1(3) ? C(121) P(1) Re 121.5(2) ? C(111) P(1) Re 114.6(2) ? C(1B) P(1) Re 110.6(3) ? C(1B) P(2) C(221) 102.2(3) ? C(1B) P(2) C(211) 103.2(3) ? C(221) P(2) C(211) 101.6(3) ? C(1B) P(2) Re 110.6(3) ? C(221) P(2) Re 122.6(2) ? C(211) P(2) Re 114.4(2) ? Cl(12) C(1) H(1) 115(9) ? Cl(12) C(1) C(2) 18.8(11) ? H(1) C(1) C(2) 133(9) ? Cl(12) C(1) Re 87.3(13) ? H(1) C(1) Re 141(9) ? C(2) C(1) Re 74.6(12) ? Cl(12) C(1) Re 88.8(11) ? H(1) C(1) Re 134(9) ? C(2) C(1) Re 72.2(10) ? Re C(1) Re 73.7(4) ? C(1) H(1) Cl(12) 31(5) ? Cl(12) C(2) H(2) 121(10) ? Cl(12) C(2) C(1) 25.6(18) ? H(2) C(2) C(1) 147(10) ? Cl(12) C(2) Re 96(2) ? H(2) C(2) Re 131(10) ? C(1) C(2) Re 73.5(10) ? Cl(12) C(2) Re 89(2) ? H(2) C(2) Re 131(10) ? C(1) C(2) Re 71.2(11) ? Re C(2) Re 73.3(6) ? C(2) H(2) Cl(12) 26(6) ? P(2) C(1B) P(1) 113.2(4) ? C(116) C(111) C(112) 118.8(7) ? C(116) C(111) P(1) 117.9(6) ? C(112) C(111) P(1) 123.3(5) ? C(111) C(112) C(113) 119.9(7) ? C(114) C(113) C(112) 120.9(8) ? C(113) C(114) C(115) 118.5(7) ? C(116) C(115) C(114) 121.5(8) ? C(115) C(116) C(111) 120.4(9) ? C(122) C(121) C(126) 115.6(8) ? C(122) C(121) P(1) 124.5(6) ? C(126) C(121) P(1) 119.1(7) ? C(121) C(122) C(123) 120.9(9) ? C(124) C(123) C(122) 122.8(11) ? C(123) C(124) C(125) 117.6(10) ? C(124) C(125) C(126) 121.2(13) ? C(125) C(126) C(121) 121.0(12) ? C(216) C(211) C(212) 119.5(7) ? C(216) C(211) P(2) 123.5(5) ? C(212) C(211) P(2) 117.0(5) ? C(211) C(212) C(213) 119.2(8) ? C(214) C(213) C(212) 121.2(8) ? C(215) C(214) C(213) 119.5(8) ? C(214) C(215) C(216) 121.2(8) ? C(211) C(216) C(215) 119.4(7) ? C(222) C(221) C(226) 118.2(6) ? C(222) C(221) P(2) 124.0(5) ? C(226) C(221) P(2) 117.8(5) ? C(221) C(222) C(223) 120.9(6) ? C(224) C(223) C(222) 120.0(7) ? C(225) C(224) C(223) 119.7(7) ? C(224) C(225) C(226) 121.5(8) ? C(225) C(226) C(221) 119.6(8) ? #= = = = END data_COMPLEX3 # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description needle _exptl_crystal_colour green _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.16 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C57 H58.32 Cl13 O0.66 P4 Re2' _chemical_formula_structural ? _chemical_formula_weight 1711.15 _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 12.4448(3) _cell_length_b 18.7581(5) _cell_length_c 27.8011(8) _cell_angle_alpha 90.00 _cell_angle_beta 101.5817(19) _cell_angle_gamma 90.00 _cell_volume 6357.8(5) _cell_measurement_reflns_used 54443 _cell_measurement_theta_min 4 _cell_measurement_theta_max 28 _cell_formula_units_z 4 _exptl_crystal_density_diffrn 1.79 _exptl_crystal_density_meas ? _diffrn_radiation_type MO-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 4.546 _cell_measurement_temperature 173 _exptl_crystal_F_000 3348 # 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 0.1877 _exptl_absorpt_correction_T_max 0.4777 _diffrn_reflns_number 54443 _reflns_number_total 16031 _reflns_number_gt 12134 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.073 _diffrn_reflns_theta_min 4.00 _diffrn_reflns_theta_max 28.68 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_max 35 # 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 0.081 _refine_ls_wR_factor_ref 0.168 _refine_ls_hydrogen_treatment H_atoms_riding _refine_ls_number_reflns 15596 _refine_ls_number_parameters 705 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0346P)^2^+154.5642P] where P=(Fo^2^+2Fc^2^)' _refine_ls_shift/su_max 0.001 _refine_diff_density_max 2.77 _refine_diff_density_min -3.39 _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 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(1) 0.06769(4) 0.26405(2) 0.186245(15) 0.03407(12) Uani ? Re(2) -0.05863(4) 0.27207(2) 0.102998(15) 0.03462(12) Uani ? Cl(B) 0.0107(3) 0.37762(15) 0.14834(10) 0.0391(8) Uani ? Cl(11) 0.1659(3) 0.33190(17) 0.25790(10) 0.0423(8) Uani ? Cl(12) 0.1542(3) 0.16382(16) 0.23453(11) 0.0450(9) Uani ? Cl(21) -0.1492(3) 0.35179(16) 0.03659(10) 0.0423(9) Uani ? Cl(22) -0.1569(3) 0.18271(17) 0.04817(11) 0.0474(9) Uani ? Cl(8A) 0.4658(13) 0.0613(9) 0.8544(6) 0.118(5) Uani ? Cl(8B) 0.4730(12) 0.0789(7) 0.8212(6) 0.104(5) Uani ? Cl(91) 0.7454(4) 0.3238(2) 0.89098(16) 0.0745(14) Uani ? Cl(92) 0.6152(4) 0.2011(2) 0.90899(15) 0.0703(13) Uani ? Cl(93) 0.4082(4) 0.3346(2) 0.87708(15) 0.0708(13) Uani ? Cl(94) 0.2805(4) 0.2112(3) 0.89672(14) 0.0760(14) Uani ? Cl(95) 0.3476(6) 0.4844(3) 0.4698(2) 0.107(2) Uani ? Cl(96) 0.2909(7) 0.5115(3) 0.5641(2) 0.127(3) Uani ? Cl(97) 0.2996(5) -0.0162(3) 0.7892(2) 0.112(2) Uani ? P(1) 0.2402(3) 0.27195(17) 0.15525(10) 0.0372(8) Uani ? P(2) 0.0905(3) 0.26386(17) 0.05624(10) 0.0374(8) Uani ? P(3) -0.0797(3) 0.25622(16) 0.23396(10) 0.0350(8) Uani ? P(4) -0.2298(3) 0.27949(17) 0.13623(10) 0.0354(8) Uani ? O(1W) 0.468(2) 0.5652(9) 0.0191(6) 0.104(10) Uani ? C(11) 0.0013(10) 0.1896(6) 0.1412(4) 0.034(3) Uani ? C(12) 0.0142(15) 0.1089(8) 0.1330(5) 0.071(5) Uani ? C(13) -0.0771(17) 0.0696(11) 0.1483(7) 0.091(8) Uani ? C(1B) 0.2161(10) 0.2267(7) 0.0952(4) 0.037(3) Uani ? C(2B) -0.2065(10) 0.2275(6) 0.1929(4) 0.039(3) Uani ? C(111) 0.3610(11) 0.2261(7) 0.1911(4) 0.042(4) Uani ? C(112) 0.3785(12) 0.1547(8) 0.1865(5) 0.056(5) Uani ? C(113) 0.4656(14) 0.1204(9) 0.2161(6) 0.073(6) Uani ? C(114) 0.5297(13) 0.1598(10) 0.2537(6) 0.071(6) Uani ? C(115) 0.5100(12) 0.2299(9) 0.2606(5) 0.056(4) Uani ? C(116) 0.4243(11) 0.2640(8) 0.2299(4) 0.047(4) Uani ? C(121) 0.2969(11) 0.3579(6) 0.1432(4) 0.041(4) Uani ? C(122) 0.3701(11) 0.3622(8) 0.1111(4) 0.045(4) Uani ? C(123) 0.4096(12) 0.4264(9) 0.0998(5) 0.057(5) Uani ? C(124) 0.3798(12) 0.4892(8) 0.1204(5) 0.057(5) Uani ? C(125) 0.3124(12) 0.4862(8) 0.1536(5) 0.054(5) Uani ? C(126) 0.2704(11) 0.4195(7) 0.1654(4) 0.045(4) Uani ? C(211) 0.0619(11) 0.2032(7) 0.0043(4) 0.044(4) Uani ? C(212) -0.0118(12) 0.2267(8) -0.0367(4) 0.053(4) Uani ? C(213) -0.0408(14) 0.1824(9) -0.0774(5) 0.068(5) Uani ? C(214) -0.0009(16) 0.1129(11) -0.0760(6) 0.093(7) Uani ? C(215) 0.069(2) 0.0905(12) -0.0350(8) 0.134(9) Uani ? C(216) 0.1015(15) 0.1341(9) 0.0049(5) 0.076(6) Uani ? C(221) 0.1389(11) 0.3444(7) 0.0291(4) 0.041(4) Uani ? C(222) 0.1075(12) 0.4113(7) 0.0401(4) 0.045(4) Uani ? C(223) 0.1474(12) 0.4696(8) 0.0185(5) 0.053(5) Uani ? C(224) 0.2134(15) 0.4609(9) -0.0151(5) 0.069(6) Uani ? C(225) 0.2462(14) 0.3935(9) -0.0258(5) 0.062(5) Uani ? C(226) 0.2103(11) 0.3348(7) -0.0041(4) 0.045(4) Uani ? C(311) -0.0543(11) 0.1901(6) 0.2833(4) 0.042(4) Uani ? C(312) 0.0139(12) 0.2084(7) 0.3268(4) 0.048(4) Uani ? C(313) 0.0427(13) 0.1580(9) 0.3641(5) 0.060(5) Uani ? C(314) 0.0016(14) 0.0906(9) 0.3569(6) 0.065(5) Uani ? C(315) -0.0680(13) 0.0714(8) 0.3143(6) 0.058(5) Uani ? C(316) -0.0972(13) 0.1218(7) 0.2770(5) 0.056(5) Uani ? C(321) -0.1216(10) 0.3345(6) 0.2653(4) 0.036(3) Uani ? C(322) -0.0897(11) 0.4031(6) 0.2562(4) 0.043(4) Uani ? C(323) -0.1311(12) 0.4621(7) 0.2769(5) 0.048(4) Uani ? C(324) -0.2030(12) 0.4503(7) 0.3071(4) 0.048(4) Uani ? C(325) -0.2364(11) 0.3831(8) 0.3172(4) 0.049(4) Uani ? C(326) -0.1957(11) 0.3245(7) 0.2961(4) 0.046(4) Uani ? C(411) -0.3523(10) 0.2418(7) 0.0985(5) 0.045(4) Uani ? C(412) -0.3967(12) 0.1763(8) 0.1088(6) 0.061(5) Uani ? C(413) -0.4874(15) 0.1483(10) 0.0755(8) 0.086(7) Uani ? C(414) -0.5363(12) 0.1856(9) 0.0353(6) 0.059(5) Uani ? C(415) -0.4950(11) 0.2519(10) 0.0250(5) 0.059(5) Uani ? C(416) -0.4034(10) 0.2795(8) 0.0571(4) 0.048(4) Uani ? C(421) -0.2786(10) 0.3659(6) 0.1531(4) 0.036(3) Uani ? C(422) -0.2440(12) 0.4291(6) 0.1354(4) 0.044(4) Uani ? C(423) -0.2816(12) 0.4932(7) 0.1504(5) 0.048(4) Uani ? C(424) -0.3517(12) 0.4947(8) 0.1832(5) 0.053(5) Uani ? C(425) -0.3879(11) 0.4328(7) 0.1993(4) 0.046(4) Uani ? C(426) -0.3533(11) 0.3686(7) 0.1846(4) 0.044(4) Uani ? C(901) 0.6915(14) 0.2754(9) 0.9345(5) 0.068(5) Uani ? C(902) 0.3305(16) 0.2610(10) 0.8524(5) 0.078(6) Uani ? C(903) 0.3348(19) 0.5473(10) 0.5127(7) 0.095(8) Uani ? C(904) 0.335(2) 0.0439(14) 0.8346(8) 0.122(9) Uani ? H(112) 0.3308 0.1286 0.1629 0.0730 Uiso calc H(113) 0.4809 0.0727 0.2112 0.0950 Uiso calc H(114) 0.5876 0.1375 0.2747 0.0930 Uiso calc H(115) 0.5541 0.2549 0.2861 0.0720 Uiso calc H(116) 0.4090 0.3116 0.2349 0.0610 Uiso calc H(122) 0.3919 0.3208 0.0974 0.0590 Uiso calc H(123) 0.4572 0.4283 0.0780 0.0740 Uiso calc H(124) 0.4056 0.5329 0.1116 0.0740 Uiso calc H(125) 0.2941 0.5278 0.1684 0.0700 Uiso calc H(126) 0.2249 0.4174 0.1881 0.0590 Uiso calc H(12A) 0.0116 0.1001 0.0990 0.0847 Uiso calc H(12B) 0.0819 0.0929 0.1524 0.0847 Uiso calc H(13A) -0.0792 0.0813 0.1817 0.1190 Uiso calc H(13B) -0.0658 0.0193 0.1456 0.1190 Uiso calc H(13C) -0.1453 0.0829 0.1274 0.1190 Uiso calc H(1B1) 0.2073 0.1759 0.0996 0.0480 Uiso calc H(1B2) 0.2783 0.2339 0.0796 0.0480 Uiso calc H(212) -0.0420 0.2721 -0.0370 0.0690 Uiso calc H(213) -0.0871 0.1992 -0.1056 0.0880 Uiso calc H(214) -0.0216 0.0826 -0.1027 0.1210 Uiso calc H(215) 0.0951 0.0440 -0.0338 0.1750 Uiso calc H(216) 0.1503 0.1173 0.0324 0.0980 Uiso calc H(222) 0.0602 0.4176 0.0617 0.0590 Uiso calc H(223) 0.1291 0.5154 0.0269 0.0680 Uiso calc H(224) 0.2361 0.5004 -0.0307 0.0900 Uiso calc H(225) 0.2928 0.3878 -0.0478 0.0800 Uiso calc H(226) 0.2326 0.2893 -0.0111 0.0580 Uiso calc H(2B1) -0.2013 0.1773 0.1852 0.0520 Uiso calc H(2B2) -0.2679 0.2336 0.2091 0.0520 Uiso calc H(312) 0.0411 0.2546 0.3313 0.0630 Uiso calc H(313) 0.0893 0.1702 0.3935 0.0780 Uiso calc H(314) 0.0213 0.0568 0.3816 0.0840 Uiso calc H(315) -0.0956 0.0252 0.3102 0.0750 Uiso calc H(316) -0.1452 0.1095 0.2480 0.0730 Uiso calc H(322) -0.0396 0.4099 0.2359 0.0560 Uiso calc H(323) -0.1103 0.5081 0.2703 0.0620 Uiso calc H(324) -0.2305 0.4893 0.3214 0.0630 Uiso calc H(325) -0.2858 0.3769 0.3380 0.0630 Uiso calc H(326) -0.2179 0.2788 0.3026 0.0600 Uiso calc H(412) -0.3667 0.1515 0.1374 0.0790 Uiso calc H(413) -0.5141 0.1034 0.0811 0.1120 Uiso calc H(414) -0.5978 0.1670 0.0145 0.0760 Uiso calc H(415) -0.5279 0.2772 -0.0029 0.0770 Uiso calc H(416) -0.3763 0.3239 0.0507 0.0630 Uiso calc H(422) -0.1960 0.4284 0.1137 0.0570 Uiso calc H(423) -0.2596 0.5358 0.1382 0.0630 Uiso calc H(424) -0.3738 0.5380 0.1942 0.0690 Uiso calc H(425) -0.4368 0.4338 0.2205 0.0600 Uiso calc H(426) -0.3795 0.3265 0.1956 0.0570 Uiso calc H(90A) 0.6448 0.3064 0.9493 0.0880 Uiso calc H(90B) 0.7512 0.2595 0.9603 0.0880 Uiso calc H(90C) 0.3754 0.2304 0.8364 0.1020 Uiso calc H(90D) 0.2691 0.2773 0.8277 0.1020 Uiso calc H(90E) 0.2825 0.5832 0.4976 0.1230 Uiso calc H(90F) 0.4050 0.5707 0.5235 0.1230 Uiso calc H(90G) 0.2988 0.0884 0.8235 0.1600 Uiso calc H(90H) 0.3055 0.0277 0.8624 0.1600 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) 0.0464(3) 0.0369(2) 0.0165(2) -0.0001(2) 0.00052(18) 0.00078(18) Re(2) 0.0472(3) 0.0366(2) 0.0171(2) 0.0028(2) -0.00065(18) -0.00222(17) Cl(B) 0.0569(18) 0.0381(15) 0.0208(12) 0.0005(13) 0.0045(12) -0.0015(11) Cl(11) 0.0518(18) 0.0501(17) 0.0229(13) -0.0067(14) 0.0022(13) -0.0011(12) Cl(12) 0.058(2) 0.0436(17) 0.0305(15) 0.0031(14) 0.0016(14) 0.0099(12) Cl(21) 0.0540(19) 0.0484(17) 0.0205(13) 0.0071(14) -0.0022(12) 0.0031(11) Cl(22) 0.059(2) 0.0508(18) 0.0283(14) -0.0011(15) -0.0013(14) -0.0104(13) Cl(8A) 0.109(10) 0.125(11) 0.105(10) -0.034(8) -0.015(9) -0.044(9) Cl(8B) 0.107(9) 0.083(8) 0.116(10) -0.013(6) 0.009(9) -0.009(8) Cl(91) 0.094(3) 0.070(3) 0.059(2) 0.010(2) 0.014(2) 0.011(2) Cl(92) 0.088(3) 0.062(2) 0.057(2) 0.002(2) 0.005(2) -0.0110(19) Cl(93) 0.086(3) 0.065(2) 0.059(2) 0.009(2) 0.009(2) -0.0082(19) Cl(94) 0.097(3) 0.088(3) 0.043(2) -0.001(2) 0.014(2) -0.0087(19) Cl(95) 0.141(5) 0.098(4) 0.080(3) -0.005(4) 0.018(3) -0.004(3) Cl(96) 0.181(7) 0.100(4) 0.106(5) -0.036(4) 0.043(5) -0.040(4) Cl(97) 0.113(4) 0.089(4) 0.120(5) -0.006(3) -0.011(4) -0.013(3) P(1) 0.0472(18) 0.0402(17) 0.0211(13) 0.0055(14) -0.0006(13) -0.0005(12) P(2) 0.0460(18) 0.0447(17) 0.0184(13) 0.0074(15) -0.0011(12) -0.0049(12) P(3) 0.0476(18) 0.0367(16) 0.0196(13) -0.0020(13) 0.0041(12) 0.0026(11) P(4) 0.0439(18) 0.0421(17) 0.0186(13) 0.0003(14) 0.0028(12) -0.0015(12) O(1W) 0.22(3) 0.064(12) 0.053(12) 0.003(13) 0.086(14) 0.016(8) C(11) 0.050(7) 0.033(6) 0.020(5) -0.001(5) 0.007(5) -0.003(4) C(12) 0.098(13) 0.058(9) 0.045(8) -0.036(9) -0.013(8) 0.020(7) C(13) 0.111(17) 0.088(14) 0.071(12) 0.019(12) 0.010(11) -0.010(10) C(1B) 0.044(7) 0.057(7) 0.012(5) 0.007(6) 0.013(5) -0.007(5) C(2B) 0.043(7) 0.036(6) 0.034(6) -0.004(5) -0.005(5) -0.002(5) C(111) 0.049(7) 0.059(8) 0.017(5) 0.014(6) 0.004(5) 0.007(5) C(112) 0.052(9) 0.063(9) 0.048(8) 0.002(7) -0.004(7) 0.002(7) C(113) 0.082(12) 0.075(11) 0.056(10) 0.036(9) -0.002(9) -0.002(8) C(114) 0.053(10) 0.100(14) 0.054(10) 0.010(9) -0.006(8) 0.031(9) C(115) 0.051(8) 0.082(11) 0.027(6) 0.007(8) -0.011(6) -0.001(7) C(116) 0.044(7) 0.065(8) 0.028(6) -0.014(7) 0.001(5) 0.006(6) C(121) 0.054(8) 0.038(7) 0.029(6) -0.004(6) 0.003(6) 0.005(5) C(122) 0.046(8) 0.058(8) 0.030(6) 0.002(6) 0.002(6) -0.004(6) C(123) 0.057(9) 0.079(11) 0.035(7) 0.007(8) 0.006(7) 0.005(7) C(124) 0.062(10) 0.063(9) 0.045(8) -0.003(8) 0.008(7) 0.011(7) C(125) 0.071(10) 0.050(8) 0.040(8) 0.004(7) 0.011(7) -0.003(6) C(126) 0.056(8) 0.045(7) 0.030(6) 0.001(6) 0.000(6) -0.001(5) C(211) 0.055(8) 0.069(9) 0.010(5) 0.013(7) 0.008(5) -0.021(5) C(212) 0.068(9) 0.062(9) 0.021(6) 0.004(7) -0.010(6) -0.007(6) C(213) 0.081(12) 0.087(12) 0.027(7) 0.014(9) -0.012(7) -0.017(7) C(214) 0.103(15) 0.113(15) 0.050(10) 0.040(12) -0.017(9) -0.055(10) C(215) 0.16(2) 0.117(17) 0.090(15) 0.080(16) -0.062(15) -0.075(13) C(216) 0.100(13) 0.072(10) 0.044(8) 0.048(10) -0.013(8) -0.030(7) C(221) 0.052(8) 0.053(8) 0.017(5) 0.006(6) 0.002(5) 0.003(5) C(222) 0.059(9) 0.048(8) 0.025(6) 0.005(6) 0.000(6) 0.001(5) C(223) 0.070(10) 0.057(9) 0.033(7) 0.008(7) 0.016(7) 0.003(6) C(224) 0.093(13) 0.067(10) 0.043(8) 0.007(9) 0.002(8) 0.023(7) C(225) 0.080(11) 0.085(11) 0.020(6) 0.016(9) 0.009(7) 0.005(7) C(226) 0.054(8) 0.057(8) 0.025(6) 0.010(6) 0.013(6) 0.000(5) C(311) 0.055(8) 0.035(6) 0.033(6) 0.003(6) 0.005(6) 0.012(5) C(312) 0.064(9) 0.054(8) 0.028(6) -0.006(7) 0.011(6) 0.007(5) C(313) 0.071(10) 0.074(11) 0.034(7) 0.009(8) 0.009(7) 0.022(7) C(314) 0.070(10) 0.072(11) 0.056(9) 0.024(9) 0.021(8) 0.039(8) C(315) 0.072(10) 0.044(8) 0.062(10) -0.003(7) 0.026(8) 0.018(7) C(316) 0.069(10) 0.051(8) 0.045(8) 0.011(7) 0.004(7) 0.009(6) C(321) 0.041(7) 0.043(7) 0.024(5) 0.003(5) 0.010(5) 0.005(5) C(322) 0.055(8) 0.043(7) 0.026(6) -0.013(6) -0.002(6) -0.001(5) C(323) 0.065(9) 0.040(7) 0.034(7) -0.002(6) -0.003(6) -0.006(5) C(324) 0.065(9) 0.051(8) 0.028(6) -0.002(7) 0.006(6) -0.004(5) C(325) 0.056(9) 0.070(9) 0.026(6) 0.006(7) 0.020(6) -0.002(6) C(326) 0.057(8) 0.055(8) 0.025(6) 0.004(7) 0.003(6) 0.004(5) C(411) 0.038(7) 0.050(8) 0.041(7) -0.001(6) -0.006(6) -0.008(6) C(412) 0.054(9) 0.061(9) 0.060(9) -0.017(7) -0.008(7) -0.006(7) C(413) 0.069(12) 0.068(11) 0.107(16) -0.003(9) -0.017(11) -0.025(11) C(414) 0.038(8) 0.083(11) 0.055(9) -0.005(8) 0.008(7) -0.024(8) C(415) 0.042(8) 0.112(14) 0.024(6) 0.016(8) 0.009(6) -0.014(7) C(416) 0.036(7) 0.080(10) 0.027(6) -0.003(7) 0.002(5) -0.002(6) C(421) 0.048(7) 0.043(7) 0.017(5) 0.003(5) 0.006(5) 0.003(4) C(422) 0.067(9) 0.038(7) 0.025(6) 0.006(6) 0.006(6) 0.003(5) C(423) 0.061(9) 0.044(7) 0.040(7) 0.006(6) 0.014(7) 0.012(6) C(424) 0.064(10) 0.055(9) 0.035(7) 0.015(7) -0.001(7) -0.011(6) C(425) 0.048(8) 0.063(9) 0.027(6) 0.001(7) 0.009(6) 0.002(6) C(426) 0.054(8) 0.046(7) 0.026(6) 0.005(6) -0.004(6) 0.005(5) C(901) 0.071(11) 0.091(12) 0.044(8) -0.013(9) 0.016(8) -0.010(8) C(902) 0.104(14) 0.097(13) 0.034(8) -0.022(11) 0.013(8) -0.005(8) C(903) 0.118(17) 0.080(13) 0.086(14) 0.007(12) 0.021(13) 0.024(11) C(904) 0.13(2) 0.15(2) 0.074(14) 0.050(17) -0.011(14) -0.046(14) # 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) C(11) 1.946(11) ? Re(1) Cl(B) 2.419(3) ? Re(1) Cl(12) 2.432(3) ? Re(1) Cl(11) 2.471(3) ? Re(1) P(1) 2.473(4) ? Re(1) P(3) 2.475(3) ? Re(1) Re(2) 2.5277(6) ? Re(2) C(11) 1.938(11) ? Re(2) Cl(B) 2.412(3) ? Re(2) Cl(22) 2.425(3) ? Re(2) Cl(21) 2.466(3) ? Re(2) P(2) 2.475(3) ? Re(2) P(4) 2.490(3) ? Cl(91) C(901) 1.751(16) ? Cl(92) C(901) 1.753(16) ? Cl(93) C(902) 1.744(17) ? Cl(94) C(902) 1.756(17) ? Cl(95) C(903) 1.71(2) ? Cl(96) C(903) 1.76(2) ? Cl(97) C(904) 1.68(2) ? Cl(8A) C(904) 1.64(3) ? Cl(8B) C(904) 1.94(3) ? P(1) C(121) 1.817(12) ? P(1) C(111) 1.842(12) ? P(1) C(1B) 1.843(10) ? P(2) C(211) 1.816(11) ? P(2) C(221) 1.842(13) ? P(2) C(1B) 1.850(12) ? P(3) C(311) 1.829(11) ? P(3) C(2B) 1.833(11) ? P(3) C(321) 1.836(12) ? P(4) C(411) 1.811(12) ? P(4) C(2B) 1.825(12) ? P(4) C(421) 1.825(12) ? C(11) C(12) 1.544(19) ? C(12) C(13) 1.49(2) ? C(111) C(112) 1.368(19) ? C(111) C(116) 1.394(17) ? C(112) C(113) 1.382(19) ? C(113) C(114) 1.39(2) ? C(114) C(115) 1.36(2) ? C(115) C(116) 1.384(18) ? C(121) C(126) 1.381(17) ? C(121) C(122) 1.400(18) ? C(122) C(123) 1.36(2) ? C(123) C(124) 1.39(2) ? C(124) C(125) 1.37(2) ? C(125) C(126) 1.420(19) ? C(211) C(212) 1.383(16) ? C(211) C(216) 1.385(19) ? C(212) C(213) 1.392(17) ? C(213) C(214) 1.39(2) ? C(214) C(215) 1.35(2) ? C(215) C(216) 1.37(2) ? C(221) C(222) 1.368(17) ? C(221) C(226) 1.415(17) ? C(222) C(223) 1.387(19) ? C(223) C(224) 1.37(2) ? C(224) C(225) 1.38(2) ? C(225) C(226) 1.37(2) ? C(311) C(312) 1.373(17) ? C(311) C(316) 1.387(18) ? C(312) C(313) 1.398(17) ? C(313) C(314) 1.36(2) ? C(314) C(315) 1.37(2) ? C(315) C(316) 1.396(18) ? C(321) C(322) 1.386(16) ? C(321) C(326) 1.391(17) ? C(322) C(323) 1.393(18) ? C(323) C(324) 1.362(19) ? C(324) C(325) 1.376(19) ? C(325) C(326) 1.388(18) ? C(411) C(416) 1.392(18) ? C(411) C(412) 1.400(19) ? C(412) C(413) 1.41(2) ? C(413) C(414) 1.35(2) ? C(414) C(415) 1.40(2) ? C(415) C(416) 1.399(18) ? C(421) C(422) 1.383(17) ? C(421) C(426) 1.401(18) ? C(422) C(423) 1.385(18) ? C(423) C(424) 1.385(19) ? C(424) C(425) 1.353(19) ? C(425) C(426) 1.367(18) ? 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 C(11) Re(1) Cl(B) 107.6(3) ? C(11) Re(1) Cl(12) 83.4(3) ? Cl(B) Re(1) Cl(12) 168.46(11) ? C(11) Re(1) Cl(11) 165.1(3) ? Cl(B) Re(1) Cl(11) 87.24(10) ? Cl(12) Re(1) Cl(11) 82.00(10) ? C(11) Re(1) P(1) 96.0(4) ? Cl(B) Re(1) P(1) 89.69(11) ? Cl(12) Re(1) P(1) 85.40(11) ? Cl(11) Re(1) P(1) 85.79(10) ? C(11) Re(1) P(3) 92.2(4) ? Cl(B) Re(1) P(3) 95.84(11) ? Cl(12) Re(1) P(3) 87.23(11) ? Cl(11) Re(1) P(3) 84.17(10) ? P(1) Re(1) P(3) 168.28(10) ? C(11) Re(1) Re(2) 49.3(3) ? Cl(B) Re(1) Re(2) 58.32(7) ? Cl(12) Re(1) Re(2) 132.55(8) ? Cl(11) Re(1) Re(2) 145.45(8) ? P(1) Re(1) Re(2) 95.81(7) ? P(3) Re(1) Re(2) 95.89(7) ? C(11) Re(2) Cl(B) 108.1(3) ? C(11) Re(2) Cl(22) 83.3(3) ? Cl(B) Re(2) Cl(22) 168.05(11) ? C(11) Re(2) Cl(21) 164.1(3) ? Cl(B) Re(2) Cl(21) 87.44(10) ? Cl(22) Re(2) Cl(21) 81.46(10) ? C(11) Re(2) P(2) 89.5(4) ? Cl(B) Re(2) P(2) 95.63(11) ? Cl(22) Re(2) P(2) 87.92(11) ? Cl(21) Re(2) P(2) 85.57(10) ? C(11) Re(2) P(4) 96.1(4) ? Cl(B) Re(2) P(4) 90.18(11) ? Cl(22) Re(2) P(4) 84.88(11) ? Cl(21) Re(2) P(4) 86.98(10) ? P(2) Re(2) P(4) 170.33(9) ? C(11) Re(2) Re(1) 49.5(3) ? Cl(B) Re(2) Re(1) 58.59(7) ? Cl(22) Re(2) Re(1) 132.61(8) ? Cl(21) Re(2) Re(1) 145.94(7) ? P(2) Re(2) Re(1) 94.76(7) ? P(4) Re(2) Re(1) 94.86(7) ? Re(2) Cl(B) Re(1) 63.10(7) ? C(121) P(1) C(111) 102.1(6) ? C(121) P(1) C(1B) 104.0(6) ? C(111) P(1) C(1B) 104.0(5) ? C(121) P(1) Re(1) 120.9(5) ? C(111) P(1) Re(1) 117.0(4) ? C(1B) P(1) Re(1) 107.0(4) ? C(211) P(2) C(221) 102.5(6) ? C(211) P(2) C(1B) 103.7(5) ? C(221) P(2) C(1B) 104.0(6) ? C(211) P(2) Re(2) 114.1(5) ? C(221) P(2) Re(2) 120.3(4) ? C(1B) P(2) Re(2) 110.5(4) ? C(311) P(3) C(2B) 105.4(6) ? C(311) P(3) C(321) 102.0(6) ? C(2B) P(3) C(321) 103.9(6) ? C(311) P(3) Re(1) 114.0(5) ? C(2B) P(3) Re(1) 108.7(4) ? C(321) P(3) Re(1) 121.3(4) ? C(411) P(4) C(2B) 105.1(6) ? C(411) P(4) C(421) 102.2(6) ? C(2B) P(4) C(421) 104.9(5) ? C(411) P(4) Re(2) 116.5(5) ? C(2B) P(4) Re(2) 106.9(4) ? C(421) P(4) Re(2) 119.9(4) ? C(12) C(11) Re(2) 137.9(8) ? C(12) C(11) Re(1) 139.0(9) ? Re(2) C(11) Re(1) 81.2(4) ? C(13) C(12) C(11) 109.7(16) ? P(1) C(1B) P(2) 108.8(6) ? P(4) C(2B) P(3) 110.4(6) ? C(112) C(111) C(116) 119.8(12) ? C(112) C(111) P(1) 122.3(10) ? C(116) C(111) P(1) 116.9(10) ? C(111) C(112) C(113) 121.3(14) ? C(112) C(113) C(114) 117.6(15) ? C(115) C(114) C(113) 121.8(14) ? C(114) C(115) C(116) 119.9(13) ? C(115) C(116) C(111) 119.2(14) ? C(126) C(121) C(122) 118.7(12) ? C(126) C(121) P(1) 121.7(10) ? C(122) C(121) P(1) 119.6(10) ? C(123) C(122) C(121) 120.7(13) ? C(122) C(123) C(124) 121.0(14) ? C(125) C(124) C(123) 119.5(14) ? C(124) C(125) C(126) 119.8(14) ? C(121) C(126) C(125) 120.2(13) ? C(212) C(211) C(216) 118.9(11) ? C(212) C(211) P(2) 116.6(10) ? C(216) C(211) P(2) 124.3(10) ? C(211) C(212) C(213) 120.1(14) ? C(212) C(213) C(214) 120.3(14) ? C(215) C(214) C(213) 118.5(14) ? C(214) C(215) C(216) 122.2(18) ? C(215) C(216) C(211) 120.0(15) ? C(222) C(221) C(226) 120.5(12) ? C(222) C(221) P(2) 122.0(10) ? C(226) C(221) P(2) 117.5(10) ? C(221) C(222) C(223) 118.9(13) ? C(224) C(223) C(222) 121.1(14) ? C(223) C(224) C(225) 120.0(15) ? C(226) C(225) C(224) 120.3(15) ? C(225) C(226) C(221) 119.1(13) ? C(312) C(311) C(316) 119.8(11) ? C(312) C(311) P(3) 118.3(10) ? C(316) C(311) P(3) 121.9(10) ? C(311) C(312) C(313) 120.4(13) ? C(314) C(313) C(312) 119.0(14) ? C(313) C(314) C(315) 121.7(13) ? C(314) C(315) C(316) 119.3(14) ? C(311) C(316) C(315) 119.8(14) ? C(322) C(321) C(326) 119.2(12) ? C(322) C(321) P(3) 122.5(10) ? C(326) C(321) P(3) 118.2(10) ? C(321) C(322) C(323) 121.2(13) ? C(324) C(323) C(322) 118.0(13) ? C(323) C(324) C(325) 122.6(13) ? C(324) C(325) C(326) 119.2(13) ? C(325) C(326) C(321) 119.8(13) ? C(416) C(411) C(412) 118.8(12) ? C(416) C(411) P(4) 118.2(10) ? C(412) C(411) P(4) 123.0(10) ? C(411) C(412) C(413) 119.2(15) ? C(414) C(413) C(412) 121.2(17) ? C(413) C(414) C(415) 120.4(14) ? C(414) C(415) C(416) 119.0(14) ? C(411) C(416) C(415) 121.2(14) ? C(422) C(421) C(426) 118.9(12) ? C(422) C(421) P(4) 121.8(10) ? C(426) C(421) P(4) 119.3(9) ? C(421) C(422) C(423) 119.3(13) ? C(424) C(423) C(422) 120.7(13) ? C(425) C(424) C(423) 119.7(13) ? C(424) C(425) C(426) 120.8(13) ? C(425) C(426) C(421) 120.4(12) ? Cl(91) C(901) Cl(92) 112.6(8) ? Cl(93) C(902) Cl(94) 113.1(8) ? Cl(95) C(903) Cl(96) 113.0(11) ? Cl(8A) C(904) Cl(97) 118.6(14) ? Cl(8A) C(904) Cl(8B) 31.0(8) ? Cl(97) C(904) Cl(8B) 101.2(12) ? #= = = = END