Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 Title: "An unusual dirhenium complex that contains the bridging 6-diphenylphosphino-2-pyridonaten ligand" Authors: Shan-Ming Kuang, Phillip E. Fanwick, Richard A. Walton #============================================================================== data_global #============================================================================== _audit_creation_date 7-09-01 _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 11 _journal_year 2001 _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 ; ; ? ; 'KUANG' ; 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 'KSM99Q' _publ_section_experimental ; ? ; _publ_section_references ; P. T. Beurskens, G. Beurskens, R. deGelder,S. Garcia-Granda, R. O. Gould, R. Israel, J. M. M. Smits, '(1999). The DIRDIF-99 Program System. 'Crystallography Laboratory, Univ. of Nijmegen, The Netherlands. Enraf-Nonius (1993), CAD4 Express, Enraf-Nonius, Delft, The Netherlands. 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. (1997). 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_KSM99 # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.10 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C53 H43 Cl2 N4 O3 P3 Re2' _chemical_formula_moiety 'C51 H40 Cl2 N3 O3 P3 Re2, C2 H3 N1' _chemical_formula_structural ? _chemical_formula_weight 1320.19 _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 11.7392(4) _cell_length_b 13.4032(5) _cell_length_c 15.4780(6) _cell_angle_alpha 84.3933(15) _cell_angle_beta 89.5143(14) _cell_angle_gamma 83.296(2) _cell_volume 2407.1(2) _cell_measurement_reflns_used 25823 _cell_measurement_theta_min 5 _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 5.351 _cell_measurement_temperature 150 _exptl_crystal_F_000 1282 # 6. DATA COLLECTION _diffrn_ambient_temperature 150 _diffrn_measurement_device_type Nonius_KappaCCD _exptl_absorpt_correction_type refined_empirical_(Otwinowski_&_Minor,_1996 _exptl_absorpt_correction_T_min 0.2303 _exptl_absorpt_correction_T_max 0.5856 _diffrn_reflns_number 25823 _diffrn_measured_fraction_theta_max 0.9971 _diffrn_reflns_theta_full 27.5 _diffrn_measured_fraction_theta_full 0.9971 _reflns_number_total 10901 _reflns_number_gt 8776 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.055 _diffrn_reflns_theta_min 5.00 _diffrn_reflns_theta_max 27.46 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_max 20 # 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 0.039 _refine_ls_wR_factor_ref 0.083 _refine_ls_hydrogen_treatment H_atoms_riding _refine_ls_number_reflns 10901 _refine_ls_number_parameters 605 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 0.985 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details '1/[\s^2^(Fo^2^)+(0.0362P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3 ' _refine_ls_shift/su_max 0.003 _refine_diff_density_max 2.31 _refine_diff_density_min -2.62 _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_(DIRDIF99,_Beurskins,_1999) _computing_structure_refinement SHELX97_(Sheldrick,_1997) _computing_molecular_graphics ; ORTEP (Johnson, 1976) 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 Re 0.023307(17) 0.340513(17) 0.196693(14) 0.01771(7) Uani 1 1 d . . . Re2 Re 0.063810(17) 0.226086(17) 0.313507(14) 0.01741(7) Uani 1 1 d . . . Cl1 Cl 0.02794(12) 0.49667(11) 0.25943(10) 0.0271(3) Uani 1 1 d . . . Cl2 Cl 0.10780(11) 0.29260(11) 0.44412(9) 0.0244(3) Uani 1 1 d . . . P1 P 0.26536(12) 0.21593(12) 0.28133(10) 0.0198(3) Uani 1 1 d . . . P2 P 0.00061(12) 0.21735(12) 0.09787(10) 0.0213(3) Uani 1 1 d . . . P3 P -0.13482(12) 0.23464(11) 0.36672(10) 0.0197(3) Uani 1 1 d . . . O16 O 0.1077(3) 0.4773(3) 0.0537(3) 0.0265(10) Uani 1 1 d . . . H16 H 0.117(9) 0.482(9) -0.002(7) 0.12(4) Uiso 1 1 d . . . O26 O 0.0855(3) 0.0537(3) 0.3800(3) 0.0229(9) Uani 1 1 d . . . O36 O -0.1255(3) 0.4522(3) 0.1000(3) 0.0271(10) Uani 1 1 d . . . N11 N 0.1939(4) 0.3592(4) 0.1541(3) 0.0206(10) Uani 1 1 d . . . N21 N 0.0407(4) 0.1053(4) 0.2446(3) 0.0213(11) Uani 1 1 d . . . N31 N -0.1544(4) 0.3591(3) 0.2229(3) 0.0188(10) Uani 1 1 d . . . N901 N 0.4331(7) 0.3135(6) 0.7128(5) 0.061(2) Uani 1 1 d . . . C12 C 0.2900(5) 0.3078(5) 0.1930(4) 0.0226(12) Uani 1 1 d . . . C13 C 0.3984(5) 0.3286(5) 0.1659(4) 0.0268(14) Uani 1 1 d . . . H13 H 0.4633 0.2923 0.1923 0.032 Uiso 1 1 calc R . . C14 C 0.4096(5) 0.4032(5) 0.0995(4) 0.0351(16) Uani 1 1 d . . . H14 H 0.4819 0.4178 0.0811 0.042 Uiso 1 1 calc R . . C15 C 0.3129(5) 0.4558(5) 0.0608(4) 0.0313(15) Uani 1 1 d . . . H15 H 0.3190 0.5069 0.0163 0.038 Uiso 1 1 calc R . . C16 C 0.2044(5) 0.4314(5) 0.0894(4) 0.0220(12) Uani 1 1 d . . . C22 C 0.0115(5) 0.0972(5) 0.1615(4) 0.0262(14) Uani 1 1 d . . . C23 C -0.0075(5) 0.0021(5) 0.1389(5) 0.0336(15) Uani 1 1 d . . . H23 H -0.0278 -0.0062 0.0824 0.040 Uiso 1 1 calc R . . C24 C 0.0042(6) -0.0805(5) 0.2020(5) 0.0368(16) Uani 1 1 d . . . H24 H -0.0089 -0.1438 0.1870 0.044 Uiso 1 1 calc R . . C25 C 0.0349(5) -0.0695(5) 0.2861(5) 0.0347(15) Uani 1 1 d . . . H25 H 0.0421 -0.1246 0.3280 0.042 Uiso 1 1 calc R . . C26 C 0.0550(5) 0.0263(5) 0.3073(4) 0.0238(13) Uani 1 1 d . . . C32 C -0.2163(5) 0.3273(4) 0.2909(4) 0.0212(12) Uani 1 1 d . . . C33 C -0.3295(5) 0.3669(5) 0.3004(4) 0.0246(13) Uani 1 1 d . . . H33 H -0.3732 0.3428 0.3465 0.029 Uiso 1 1 calc R . . C34 C -0.3764(5) 0.4434(5) 0.2394(4) 0.0263(13) Uani 1 1 d . . . H34 H -0.4512 0.4730 0.2461 0.032 Uiso 1 1 calc R . . C35 C -0.3122(5) 0.4759(5) 0.1687(4) 0.0268(13) Uani 1 1 d . . . H35 H -0.3435 0.5272 0.1280 0.032 Uiso 1 1 calc R . . C36 C -0.1989(5) 0.4304(5) 0.1594(4) 0.0244(13) Uani 1 1 d . . . C111 C 0.3324(4) 0.0955(5) 0.2478(4) 0.0245(13) Uani 1 1 d . . . C112 C 0.3738(5) 0.0858(5) 0.1638(4) 0.0286(14) Uani 1 1 d . . . H112 H 0.3712 0.1420 0.1233 0.034 Uiso 1 1 calc R . . C113 C 0.4191(5) -0.0092(6) 0.1412(5) 0.0374(17) Uani 1 1 d . . . H113 H 0.4446 -0.0163 0.0848 0.045 Uiso 1 1 calc R . . C114 C 0.4266(5) -0.0930(5) 0.2020(5) 0.0362(17) Uani 1 1 d . . . H114 H 0.4590 -0.1556 0.1869 0.043 Uiso 1 1 calc R . . C115 C 0.3857(5) -0.0829(5) 0.2852(5) 0.0315(15) Uani 1 1 d . . . H115 H 0.3914 -0.1385 0.3265 0.038 Uiso 1 1 calc R . . C116 C 0.3361(5) 0.0108(5) 0.3069(5) 0.0293(14) Uani 1 1 d . . . H116 H 0.3050 0.0166 0.3619 0.035 Uiso 1 1 calc R . . C121 C 0.3629(4) 0.2501(5) 0.3627(4) 0.0249(13) Uani 1 1 d . . . C122 C 0.4390(5) 0.1810(5) 0.4128(4) 0.0302(15) Uani 1 1 d . . . H122 H 0.4457 0.1129 0.4042 0.036 Uiso 1 1 calc R . . C123 C 0.5048(5) 0.2141(6) 0.4757(4) 0.0363(16) Uani 1 1 d . . . H123 H 0.5569 0.1680 0.5082 0.044 Uiso 1 1 calc R . . C124 C 0.4943(5) 0.3143(6) 0.4909(4) 0.0389(18) Uani 1 1 d . . . H124 H 0.5384 0.3352 0.5339 0.047 Uiso 1 1 calc R . . C125 C 0.4194(5) 0.3826(6) 0.4431(4) 0.0354(16) Uani 1 1 d . . . H125 H 0.4131 0.4504 0.4528 0.042 Uiso 1 1 calc R . . C126 C 0.3519(5) 0.3510(5) 0.3792(4) 0.0282(14) Uani 1 1 d . . . H126 H 0.2995 0.3977 0.3477 0.034 Uiso 1 1 calc R . . C211 C -0.1396(5) 0.2245(5) 0.0434(4) 0.0274(14) Uani 1 1 d . . . C212 C -0.2296(6) 0.1898(6) 0.0928(5) 0.0440(19) Uani 1 1 d . . . H212 H -0.2154 0.1599 0.1490 0.053 Uiso 1 1 calc R . . C213 C -0.3391(5) 0.1991(7) 0.0593(6) 0.054(2) Uani 1 1 d . . . H213 H -0.3987 0.1767 0.0931 0.065 Uiso 1 1 calc R . . C214 C -0.3600(6) 0.2419(7) -0.0246(6) 0.057(3) Uani 1 1 d . . . H214 H -0.4340 0.2487 -0.0471 0.068 Uiso 1 1 calc R . . C215 C -0.2733(7) 0.2742(7) -0.0747(6) 0.060(3) Uani 1 1 d . . . H215 H -0.2883 0.3017 -0.1315 0.072 Uiso 1 1 calc R . . C216 C -0.1604(6) 0.2663(6) -0.0413(5) 0.0441(19) Uani 1 1 d . . . H216 H -0.1012 0.2888 -0.0755 0.053 Uiso 1 1 calc R . . C221 C 0.1055(5) 0.2026(5) 0.0099(4) 0.0267(14) Uani 1 1 d . . . C222 C 0.1144(6) 0.2847(5) -0.0508(4) 0.0332(15) Uani 1 1 d . . . H222 H 0.0664 0.3444 -0.0470 0.040 Uiso 1 1 calc R . . C223 C 0.1943(6) 0.2783(6) -0.1173(5) 0.0446(19) Uani 1 1 d . . . H223 H 0.2005 0.3339 -0.1573 0.054 Uiso 1 1 calc R . . C224 C 0.2655(6) 0.1879(6) -0.1239(5) 0.0429(19) Uani 1 1 d . . . H224 H 0.3183 0.1827 -0.1689 0.051 Uiso 1 1 calc R . . C225 C 0.2567(6) 0.1071(6) -0.0634(5) 0.0424(19) Uani 1 1 d . . . H225 H 0.3040 0.0471 -0.0680 0.051 Uiso 1 1 calc R . . C226 C 0.1782(5) 0.1130(5) 0.0050(4) 0.0299(15) Uani 1 1 d . . . H226 H 0.1743 0.0582 0.0463 0.036 Uiso 1 1 calc R . . C311 C -0.2065(4) 0.1211(4) 0.3693(4) 0.0222(12) Uani 1 1 d . . . C312 C -0.1702(5) 0.0381(5) 0.4266(4) 0.0253(13) Uani 1 1 d . . . H312 H -0.1098 0.0416 0.4642 0.030 Uiso 1 1 calc R . . C313 C -0.2210(5) -0.0497(5) 0.4295(4) 0.0321(15) Uani 1 1 d . . . H313 H -0.1972 -0.1038 0.4701 0.038 Uiso 1 1 calc R . . C314 C -0.3083(5) -0.0566(5) 0.3711(5) 0.0328(15) Uani 1 1 d . . . H314 H -0.3421 -0.1161 0.3713 0.039 Uiso 1 1 calc R . . C315 C -0.3447(5) 0.0256(5) 0.3125(4) 0.0319(15) Uani 1 1 d . . . H315 H -0.4033 0.0209 0.2735 0.038 Uiso 1 1 calc R . . C316 C -0.2959(5) 0.1137(5) 0.3110(4) 0.0238(13) Uani 1 1 d . . . H316 H -0.3217 0.1684 0.2717 0.029 Uiso 1 1 calc R . . C321 C -0.1672(4) 0.2876(4) 0.4700(4) 0.0204(12) Uani 1 1 d . . . C322 C -0.1463(5) 0.3872(5) 0.4732(4) 0.0267(13) Uani 1 1 d . . . H322 H -0.1208 0.4235 0.4239 0.032 Uiso 1 1 calc R . . C323 C -0.1633(5) 0.4321(5) 0.5493(4) 0.0319(15) Uani 1 1 d . . . H323 H -0.1483 0.4984 0.5515 0.038 Uiso 1 1 calc R . . C324 C -0.2025(5) 0.3792(5) 0.6222(4) 0.0340(16) Uani 1 1 d . . . H324 H -0.2152 0.4103 0.6731 0.041 Uiso 1 1 calc R . . C325 C -0.2226(5) 0.2812(5) 0.6197(4) 0.0314(15) Uani 1 1 d . . . H325 H -0.2481 0.2456 0.6693 0.038 Uiso 1 1 calc R . . C326 C -0.2052(5) 0.2338(5) 0.5432(4) 0.0252(13) Uani 1 1 d . . . H326 H -0.2191 0.1671 0.5416 0.030 Uiso 1 1 calc R . . C902 C 0.3442(8) 0.3302(6) 0.6811(5) 0.0469(19) Uani 1 1 d . . . C903 C 0.2311(8) 0.3510(8) 0.6424(6) 0.072(3) Uani 1 1 d . . . H90A H 0.2380 0.3589 0.5803 0.108 Uiso 1 1 calc R . . H90B H 0.1928 0.4119 0.6620 0.108 Uiso 1 1 calc R . . H90C H 0.1876 0.2959 0.6593 0.108 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.01588(11) 0.02093(13) 0.01632(13) -0.00026(10) 0.00002(8) -0.00348(8) Re2 0.01623(11) 0.01978(13) 0.01629(13) -0.00098(10) -0.00036(9) -0.00307(8) Cl1 0.0301(7) 0.0221(8) 0.0297(8) -0.0042(6) -0.0005(6) -0.0045(6) Cl2 0.0235(7) 0.0313(8) 0.0198(7) -0.0054(6) -0.0002(5) -0.0058(6) P1 0.0158(7) 0.0234(8) 0.0201(8) -0.0014(6) -0.0003(6) -0.0020(6) P2 0.0195(7) 0.0274(8) 0.0178(8) -0.0039(7) 0.0012(6) -0.0047(6) P3 0.0191(7) 0.0202(8) 0.0198(8) -0.0001(6) 0.0005(6) -0.0035(6) O16 0.028(2) 0.031(3) 0.020(2) 0.004(2) -0.0012(18) -0.0054(18) O26 0.025(2) 0.020(2) 0.023(2) -0.0004(18) -0.0019(17) -0.0010(16) O36 0.022(2) 0.033(3) 0.023(2) 0.0103(19) 0.0030(17) -0.0030(18) N11 0.019(2) 0.030(3) 0.016(2) -0.006(2) -0.0020(19) -0.010(2) N21 0.016(2) 0.027(3) 0.022(3) -0.004(2) 0.0021(19) -0.0081(19) N31 0.021(2) 0.016(2) 0.020(3) -0.007(2) -0.0078(19) 0.0011(18) N901 0.073(5) 0.050(5) 0.058(5) -0.005(4) 0.012(4) 0.001(4) C12 0.020(3) 0.027(3) 0.020(3) 0.001(3) -0.002(2) -0.002(2) C13 0.018(3) 0.036(4) 0.026(3) 0.004(3) -0.001(2) -0.006(2) C14 0.024(3) 0.049(4) 0.034(4) -0.001(3) 0.000(3) -0.013(3) C15 0.029(3) 0.040(4) 0.026(4) 0.006(3) 0.001(3) -0.014(3) C16 0.019(3) 0.030(3) 0.017(3) 0.002(3) 0.000(2) -0.007(2) C22 0.021(3) 0.034(4) 0.026(3) -0.012(3) 0.005(2) -0.007(2) C23 0.040(4) 0.034(4) 0.031(4) -0.013(3) 0.000(3) -0.013(3) C24 0.049(4) 0.026(4) 0.039(4) -0.009(3) 0.003(3) -0.015(3) C25 0.040(4) 0.026(4) 0.038(4) 0.004(3) -0.002(3) -0.006(3) C26 0.022(3) 0.025(3) 0.024(3) -0.001(3) 0.003(2) -0.001(2) C32 0.020(3) 0.025(3) 0.021(3) -0.003(3) 0.004(2) -0.008(2) C33 0.019(3) 0.031(3) 0.022(3) 0.003(3) 0.003(2) -0.003(2) C34 0.022(3) 0.027(3) 0.029(4) -0.002(3) -0.002(3) 0.000(2) C35 0.025(3) 0.022(3) 0.032(4) 0.005(3) -0.006(3) -0.003(2) C36 0.024(3) 0.027(3) 0.022(3) 0.005(3) -0.001(2) -0.009(2) C111 0.017(3) 0.028(3) 0.029(3) -0.007(3) -0.001(2) -0.002(2) C112 0.023(3) 0.033(4) 0.029(4) -0.007(3) 0.000(3) 0.002(3) C113 0.034(4) 0.046(4) 0.033(4) -0.018(4) 0.000(3) 0.005(3) C114 0.029(3) 0.028(4) 0.053(5) -0.013(3) -0.010(3) 0.001(3) C115 0.027(3) 0.020(3) 0.047(4) -0.001(3) 0.000(3) -0.004(2) C116 0.023(3) 0.028(3) 0.038(4) -0.002(3) -0.001(3) -0.006(2) C121 0.016(3) 0.037(4) 0.022(3) -0.001(3) -0.002(2) -0.002(2) C122 0.021(3) 0.043(4) 0.025(3) 0.004(3) 0.002(2) -0.006(3) C123 0.025(3) 0.051(5) 0.030(4) 0.003(3) -0.004(3) -0.001(3) C124 0.024(3) 0.070(6) 0.028(4) -0.016(4) 0.005(3) -0.017(3) C125 0.025(3) 0.047(4) 0.038(4) -0.017(3) 0.005(3) -0.012(3) C126 0.019(3) 0.037(4) 0.029(4) -0.007(3) 0.000(2) -0.002(3) C211 0.021(3) 0.038(4) 0.025(3) -0.009(3) -0.001(2) -0.003(3) C212 0.034(4) 0.053(5) 0.047(5) -0.013(4) 0.012(3) -0.009(3) C213 0.017(3) 0.075(6) 0.075(6) -0.031(5) 0.005(4) -0.005(3) C214 0.030(4) 0.068(6) 0.076(7) -0.039(5) -0.017(4) 0.004(4) C215 0.060(5) 0.069(6) 0.051(5) -0.017(5) -0.031(4) 0.006(5) C216 0.044(4) 0.054(5) 0.034(4) -0.007(4) -0.017(3) 0.003(3) C221 0.019(3) 0.035(4) 0.026(3) -0.008(3) -0.003(2) -0.003(2) C222 0.041(4) 0.032(4) 0.028(4) -0.008(3) 0.006(3) -0.006(3) C223 0.060(5) 0.045(5) 0.033(4) -0.011(4) 0.020(4) -0.020(4) C224 0.042(4) 0.059(5) 0.032(4) -0.014(4) 0.018(3) -0.015(4) C225 0.031(4) 0.051(5) 0.046(5) -0.017(4) 0.008(3) 0.004(3) C226 0.021(3) 0.042(4) 0.028(4) -0.008(3) -0.001(3) -0.005(3) C311 0.019(3) 0.018(3) 0.029(3) 0.000(3) 0.004(2) -0.004(2) C312 0.027(3) 0.025(3) 0.022(3) 0.004(3) -0.003(2) -0.001(2) C313 0.038(4) 0.022(3) 0.034(4) 0.006(3) 0.006(3) -0.004(3) C314 0.033(3) 0.023(3) 0.044(4) -0.003(3) 0.004(3) -0.010(3) C315 0.024(3) 0.039(4) 0.034(4) -0.007(3) 0.001(3) -0.006(3) C316 0.019(3) 0.030(3) 0.024(3) -0.001(3) 0.001(2) -0.010(2) C321 0.016(3) 0.024(3) 0.021(3) -0.003(3) 0.000(2) -0.003(2) C322 0.027(3) 0.031(4) 0.022(3) -0.003(3) 0.002(2) -0.003(3) C323 0.034(3) 0.025(3) 0.039(4) -0.011(3) 0.007(3) -0.005(3) C324 0.032(3) 0.041(4) 0.031(4) -0.016(3) 0.003(3) -0.005(3) C325 0.032(3) 0.042(4) 0.022(3) -0.001(3) 0.004(3) -0.012(3) C326 0.028(3) 0.024(3) 0.024(3) -0.003(3) 0.001(2) -0.007(2) C902 0.072(6) 0.037(4) 0.029(4) -0.003(3) 0.009(4) 0.003(4) C903 0.083(7) 0.074(7) 0.054(6) -0.019(5) -0.006(5) 0.023(5) # 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 Re1 N31 2.113(4) . ? Re1 N11 2.138(4) . ? Re1 Re2 2.2693(3) . ? Re1 P2 2.3956(15) . ? Re1 Cl1 2.3981(14) . ? Re1 O36 2.555(4) . ? Re1 O16 2.973(4) . ? Re2 N21 2.068(5) . ? Re2 Cl2 2.3718(14) . ? Re2 P1 2.4047(14) . ? Re2 O26 2.422(4) . ? Re2 P3 2.4601(14) . ? P1 C12 1.793(6) . ? P1 C111 1.832(6) . ? P1 C121 1.835(6) . ? P2 C22 1.796(7) . ? P2 C221 1.837(6) . ? P2 C211 1.844(6) . ? P3 C32 1.813(6) . ? P3 C311 1.819(6) . ? P3 C321 1.830(6) . ? O16 C16 1.324(7) . ? O26 C26 1.283(7) . ? O36 C36 1.291(7) . ? N11 C16 1.338(8) . ? N11 C12 1.363(7) . ? N21 C22 1.352(7) . ? N21 C26 1.361(8) . ? N31 C32 1.338(7) . ? N31 C36 1.364(8) . ? N901 C902 1.146(10) . ? C12 C13 1.387(7) . ? C13 C14 1.379(9) . ? C14 C15 1.373(9) . ? C15 C16 1.409(7) . ? C22 C23 1.397(8) . ? C23 C24 1.397(10) . ? C24 C25 1.380(9) . ? C25 C26 1.403(8) . ? C32 C33 1.384(7) . ? C33 C34 1.391(8) . ? C34 C35 1.387(8) . ? C35 C36 1.409(8) . ? C111 C116 1.382(9) . ? C111 C112 1.397(8) . ? C112 C113 1.397(8) . ? C113 C114 1.388(10) . ? C114 C115 1.384(9) . ? C115 C116 1.392(8) . ? C121 C122 1.391(8) . ? C121 C126 1.392(8) . ? C122 C123 1.385(9) . ? C123 C124 1.376(10) . ? C124 C125 1.360(10) . ? C125 C126 1.399(8) . ? C211 C216 1.386(10) . ? C211 C212 1.395(9) . ? C212 C213 1.378(10) . ? C213 C214 1.380(12) . ? C214 C215 1.359(12) . ? C215 C216 1.416(10) . ? C221 C222 1.389(9) . ? C221 C226 1.398(8) . ? C222 C223 1.388(9) . ? C223 C224 1.402(10) . ? C224 C225 1.374(11) . ? C225 C226 1.400(9) . ? C311 C312 1.382(8) . ? C311 C316 1.408(8) . ? C312 C313 1.376(8) . ? C313 C314 1.389(9) . ? C314 C315 1.386(9) . ? C315 C316 1.370(8) . ? C321 C326 1.382(8) . ? C321 C322 1.391(8) . ? C322 C323 1.378(8) . ? C323 C324 1.377(9) . ? C324 C325 1.366(9) . ? C325 C326 1.400(8) . ? C902 C903 1.446(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N31 Re1 N11 165.55(19) . . ? N31 Re1 Re2 93.58(13) . . ? N11 Re1 Re2 99.46(14) . . ? N31 Re1 P2 91.79(12) . . ? N11 Re1 P2 93.24(12) . . ? Re2 Re1 P2 95.03(4) . . ? N31 Re1 Cl1 85.67(12) . . ? N11 Re1 Cl1 85.63(13) . . ? Re2 Re1 Cl1 101.59(4) . . ? P2 Re1 Cl1 163.30(6) . . ? N31 Re1 O36 55.75(16) . . ? N11 Re1 O36 111.34(16) . . ? Re2 Re1 O36 149.20(9) . . ? P2 Re1 O36 84.20(10) . . ? Cl1 Re1 O36 80.73(10) . . ? N31 Re1 O16 117.15(16) . . ? N11 Re1 O16 49.29(16) . . ? Re2 Re1 O16 148.57(8) . . ? P2 Re1 O16 90.64(9) . . ? Cl1 Re1 O16 75.99(9) . . ? O36 Re1 O16 62.11(12) . . ? N21 Re2 Re1 93.05(14) . . ? N21 Re2 Cl2 150.93(15) . . ? Re1 Re2 Cl2 116.02(4) . . ? N21 Re2 P1 93.01(12) . . ? Re1 Re2 P1 90.91(4) . . ? Cl2 Re2 P1 86.99(5) . . ? N21 Re2 O26 57.73(17) . . ? Re1 Re2 O26 150.78(9) . . ? Cl2 Re2 O26 93.20(10) . . ? P1 Re2 O26 91.17(9) . . ? N21 Re2 P3 91.31(12) . . ? Re1 Re2 P3 95.07(4) . . ? Cl2 Re2 P3 86.21(5) . . ? P1 Re2 P3 172.42(5) . . ? O26 Re2 P3 85.88(9) . . ? C12 P1 C111 105.0(3) . . ? C12 P1 C121 99.9(3) . . ? C111 P1 C121 105.2(3) . . ? C12 P1 Re2 109.83(19) . . ? C111 P1 Re2 116.31(19) . . ? C121 P1 Re2 118.56(19) . . ? C22 P2 C221 105.8(3) . . ? C22 P2 C211 103.2(3) . . ? C221 P2 C211 104.2(3) . . ? C22 P2 Re1 106.5(2) . . ? C221 P2 Re1 118.3(2) . . ? C211 P2 Re1 117.3(2) . . ? C32 P3 C311 105.8(3) . . ? C32 P3 C321 101.5(3) . . ? C311 P3 C321 106.5(3) . . ? C32 P3 Re2 105.05(18) . . ? C311 P3 Re2 117.90(18) . . ? C321 P3 Re2 118.20(17) . . ? C16 O16 Re1 77.7(3) . . ? C26 O26 Re2 88.1(3) . . ? C36 O36 Re1 86.1(3) . . ? C16 N11 C12 119.5(5) . . ? C16 N11 Re1 116.4(4) . . ? C12 N11 Re1 123.8(4) . . ? C22 N21 C26 124.1(5) . . ? C22 N21 Re2 133.7(4) . . ? C26 N21 Re2 102.1(4) . . ? C32 N31 C36 122.4(5) . . ? C32 N31 Re1 132.4(4) . . ? C36 N31 Re1 104.3(4) . . ? N11 C12 C13 120.9(6) . . ? N11 C12 P1 115.6(4) . . ? C13 C12 P1 123.6(5) . . ? C14 C13 C12 119.8(6) . . ? C15 C14 C13 119.4(6) . . ? C14 C15 C16 119.1(6) . . ? O16 C16 N11 116.4(5) . . ? O16 C16 C15 122.3(6) . . ? N11 C16 C15 121.3(6) . . ? N21 C22 C23 118.0(6) . . ? N21 C22 P2 111.4(4) . . ? C23 C22 P2 130.6(5) . . ? C22 C23 C24 119.6(6) . . ? C25 C24 C23 120.9(6) . . ? C24 C25 C26 118.7(6) . . ? O26 C26 N21 111.8(5) . . ? O26 C26 C25 129.5(6) . . ? N21 C26 C25 118.7(6) . . ? N31 C32 C33 120.8(6) . . ? N31 C32 P3 113.1(4) . . ? C33 C32 P3 126.0(5) . . ? C32 C33 C34 118.6(6) . . ? C35 C34 C33 120.4(5) . . ? C34 C35 C36 119.2(6) . . ? O36 C36 N31 113.2(5) . . ? O36 C36 C35 128.1(6) . . ? N31 C36 C35 118.5(5) . . ? C116 C111 C112 119.4(6) . . ? C116 C111 P1 118.3(5) . . ? C112 C111 P1 122.2(5) . . ? C113 C112 C111 119.4(7) . . ? C114 C113 C112 120.7(6) . . ? C115 C114 C113 119.6(6) . . ? C114 C115 C116 119.8(7) . . ? C111 C116 C115 121.0(6) . . ? C122 C121 C126 118.8(6) . . ? C122 C121 P1 124.3(5) . . ? C126 C121 P1 116.7(4) . . ? C123 C122 C121 119.7(6) . . ? C124 C123 C122 121.0(7) . . ? C125 C124 C123 120.0(6) . . ? C124 C125 C126 120.1(7) . . ? C121 C126 C125 120.4(6) . . ? C216 C211 C212 119.4(6) . . ? C216 C211 P2 123.5(5) . . ? C212 C211 P2 117.0(5) . . ? C213 C212 C211 120.9(8) . . ? C212 C213 C214 119.6(8) . . ? C215 C214 C213 120.6(7) . . ? C214 C215 C216 120.7(8) . . ? C211 C216 C215 118.7(8) . . ? C222 C221 C226 120.0(6) . . ? C222 C221 P2 118.3(5) . . ? C226 C221 P2 121.7(5) . . ? C223 C222 C221 120.5(6) . . ? C222 C223 C224 119.8(7) . . ? C225 C224 C223 119.4(6) . . ? C224 C225 C226 121.4(7) . . ? C221 C226 C225 118.8(7) . . ? C312 C311 C316 118.4(5) . . ? C312 C311 P3 120.2(4) . . ? C316 C311 P3 121.4(5) . . ? C313 C312 C311 121.9(6) . . ? C312 C313 C314 119.3(6) . . ? C313 C314 C315 119.6(6) . . ? C316 C315 C314 121.1(6) . . ? C315 C316 C311 119.8(6) . . ? C326 C321 C322 119.9(5) . . ? C326 C321 P3 124.2(4) . . ? C322 C321 P3 115.8(4) . . ? C323 C322 C321 120.0(6) . . ? C324 C323 C322 120.3(6) . . ? C325 C324 C323 120.1(6) . . ? C324 C325 C326 120.6(6) . . ? C321 C326 C325 119.1(6) . . ? N901 C902 C903 179.1(10) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 2.312 _refine_diff_density_min -2.623 _refine_diff_density_rms 0.187 ===END