Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2002 data_global #==================================================================== _audit_creation_date 3-03-00 _audit_creation_method from_MolEN_and_SHELXL _audit_update_record ; ? ; _journal_coden_Cambridge 186 loop_ _publ_author_name 'Walton, Richard A.' 'Bera, Jitendra K.' 'Clerac, Rodolphe' 'Fanwick, P.' _publ_contact_author_name 'Prof Richard A Walton' _publ_contact_author_address ; Department of Chemistry Purdue University 1393 Brown Building, West Lafayette Indiana 47907-1393 UNITED STATES OF AMERICA ; _publ_contact_author_email 'RAWALTON@PURDUE.EDU' _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Assemblies of multiply bonded [Re2]n+ cores possessing bond orders of 3 or 3.5 that are linked by dicarboxylate bridges ; _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 Gottingen, 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 ; data_MD21PX _database_code_CSD 178305 # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description cube _exptl_crystal_colour orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C56 H48 Cl4 N O2 P4 Re2' _chemical_formula_structural ? _chemical_formula_weight 1405.12 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'p 1 21/n 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 17.8053(5) _cell_length_b 14.4632(2) _cell_length_c 21.1278(5) _cell_angle_alpha 90.00 _cell_angle_beta 105.9273(9) _cell_angle_gamma 90.00 _cell_volume 5232.0(4) _cell_measurement_reflns_used 42362 _cell_measurement_theta_min 4 _cell_measurement_theta_max 27 _cell_formula_units_z 4 _exptl_crystal_density_diffrn 1.78 _exptl_crystal_density_meas ? _diffrn_radiation_type MO-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 5.056 _cell_measurement_temperature 173 _exptl_crystal_F_000 2740 # 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 0.2821 _exptl_absorpt_correction_T_max 0.3638 _diffrn_reflns_number 42362 _reflns_number_total 12282 _reflns_number_gt 10483 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.052 _diffrn_reflns_theta_min 4.00 _diffrn_reflns_theta_max 27.50 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_max 26 # 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 0.036 _refine_ls_wR_factor_ref 0.080 _refine_ls_hydrogen_treatment H_atoms_riding _refine_ls_number_reflns 11806 _refine_ls_number_parameters 622 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0417P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.001 _refine_diff_density_max 1.21 _refine_diff_density_min -1.85 _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) 0.130452(11) 0.139360(11) 0.384469(9) 0.01934(5) Uani ? Re(2) 0.257628(10) 0.184499(11) 0.395707(9) 0.01915(5) Uani ? Cl(11) 0.06743(7) 0.17672(8) 0.27439(6) 0.0286(3) Uani ? Cl(12) -0.00272(7) 0.10583(8) 0.40632(6) 0.0306(3) Uani ? Cl(21) 0.23987(7) 0.27983(8) 0.30178(6) 0.0276(3) Uani ? Cl(22) 0.40594(7) 0.19727(8) 0.41202(6) 0.0280(3) Uani ? P(1) 0.09632(7) 0.29212(8) 0.42217(6) 0.0236(4) Uani ? P(2) 0.26876(7) 0.33270(8) 0.45758(6) 0.0239(4) Uani ? P(3) 0.12852(7) -0.02071(8) 0.34135(6) 0.0218(3) Uani ? P(4) 0.28473(7) 0.05294(8) 0.33059(6) 0.0205(3) Uani ? O(1) 0.16722(18) 0.0789(2) 0.47667(15) 0.0228(9) Uani ? O(2) 0.29136(19) 0.1115(2) 0.48448(15) 0.0232(9) Uani ? N(14) 0.3005(4) -0.1098(3) 0.6719(2) 0.0527(19) Uani ? C(10) 0.2393(3) 0.0733(3) 0.5065(2) 0.0226(13) Uani ? C(11) 0.2616(3) 0.0142(3) 0.5667(2) 0.0280(13) Uani ? C(12) 0.2051(4) -0.0185(4) 0.5948(3) 0.0388(19) Uani ? C(13) 0.2274(4) -0.0792(4) 0.6479(3) 0.047(2) Uani ? C(15) 0.3540(4) -0.0774(4) 0.6446(3) 0.0461(19) Uani ? C(16) 0.3386(3) -0.0142(3) 0.5927(3) 0.0362(16) Uani ? C(1B) 0.1713(3) 0.3823(3) 0.4273(2) 0.0256(15) Uani ? C(2B) 0.2003(3) -0.0209(3) 0.2943(2) 0.0246(13) Uani ? C(111) 0.0092(3) 0.3429(3) 0.3661(3) 0.0285(15) Uani ? C(112) 0.0138(3) 0.3830(3) 0.3085(3) 0.0341(16) Uani ? C(113) -0.0522(4) 0.4181(4) 0.2631(3) 0.0458(19) Uani ? C(114) -0.1236(4) 0.4104(4) 0.2758(3) 0.051(2) Uani ? C(115) -0.1297(3) 0.3699(4) 0.3328(3) 0.048(2) Uani ? C(116) -0.0626(3) 0.3364(4) 0.3791(3) 0.0378(19) Uani ? C(121) 0.0784(3) 0.3002(3) 0.5037(2) 0.0285(16) Uani ? C(122) 0.0572(3) 0.3837(3) 0.5256(3) 0.0340(17) Uani ? C(123) 0.0528(4) 0.3948(4) 0.5890(3) 0.046(2) Uani ? C(124) 0.0720(4) 0.3206(4) 0.6331(3) 0.045(2) Uani ? C(125) 0.0900(4) 0.2368(4) 0.6112(3) 0.0416(19) Uani ? C(126) 0.0934(3) 0.2258(3) 0.5467(3) 0.0331(16) Uani ? C(211) 0.3346(3) 0.4253(3) 0.4466(3) 0.0285(15) Uani ? C(212) 0.3724(3) 0.4242(3) 0.3969(3) 0.0327(16) Uani ? C(213) 0.4231(3) 0.4942(3) 0.3920(3) 0.0410(19) Uani ? C(214) 0.4376(3) 0.5670(4) 0.4363(3) 0.0442(19) Uani ? C(215) 0.4011(4) 0.5691(4) 0.4857(3) 0.046(2) Uani ? C(216) 0.3495(3) 0.4985(3) 0.4914(3) 0.0387(19) Uani ? C(221) 0.2933(3) 0.3229(3) 0.5467(2) 0.0272(16) Uani ? C(222) 0.2548(3) 0.3696(4) 0.5863(3) 0.0411(17) Uani ? C(223) 0.2814(4) 0.3628(4) 0.6543(3) 0.051(2) Uani ? C(224) 0.3473(4) 0.3117(4) 0.6832(3) 0.051(2) Uani ? C(225) 0.3866(4) 0.2657(4) 0.6447(3) 0.0439(19) Uani ? C(226) 0.3594(3) 0.2705(3) 0.5771(3) 0.0345(16) Uani ? C(311) 0.0433(3) -0.0704(3) 0.2829(2) 0.0250(13) Uani ? C(312) -0.0296(3) -0.0304(4) 0.2684(3) 0.0413(19) Uani ? C(313) -0.0924(4) -0.0727(4) 0.2225(4) 0.059(2) Uani ? C(314) -0.0823(4) -0.1534(4) 0.1919(3) 0.053(2) Uani ? C(315) -0.0099(3) -0.1933(4) 0.2065(3) 0.047(2) Uani ? C(316) 0.0533(3) -0.1529(3) 0.2521(3) 0.0369(19) Uani ? C(321) 0.1550(3) -0.1073(3) 0.4064(2) 0.0252(15) Uani ? C(322) 0.0999(3) -0.1250(3) 0.4405(3) 0.0395(19) Uani ? C(323) 0.1174(4) -0.1870(4) 0.4925(3) 0.044(2) Uani ? C(324) 0.1893(4) -0.2288(4) 0.5123(3) 0.0426(19) Uani ? C(325) 0.2441(3) -0.2096(3) 0.4793(3) 0.0360(17) Uani ? C(326) 0.2274(3) -0.1504(3) 0.4257(3) 0.0279(15) Uani ? C(411) 0.3152(3) 0.0850(3) 0.2583(2) 0.0256(15) Uani ? C(412) 0.3938(3) 0.0838(4) 0.2597(3) 0.0351(17) Uani ? C(413) 0.4163(4) 0.1061(4) 0.2036(3) 0.048(2) Uani ? C(414) 0.3617(4) 0.1318(4) 0.1464(3) 0.046(2) Uani ? C(415) 0.2844(4) 0.1329(4) 0.1454(3) 0.0439(19) Uani ? C(416) 0.2603(3) 0.1110(3) 0.2003(3) 0.0356(16) Uani ? C(421) 0.3583(3) -0.0314(3) 0.3718(2) 0.0235(11) Uani ? C(422) 0.3712(3) -0.1081(3) 0.3359(3) 0.0286(16) Uani ? C(423) 0.4170(3) -0.1809(3) 0.3677(3) 0.0332(16) Uani ? C(424) 0.4517(3) -0.1772(3) 0.4348(3) 0.0335(16) Uani ? C(425) 0.4420(3) -0.0998(3) 0.4701(2) 0.0285(15) Uani ? C(426) 0.3956(3) -0.0269(3) 0.4387(2) 0.0252(15) Uani ? H(12) 0.1533 -0.0004 0.5785 0.0510 Uiso calc H(13) 0.1895 -0.0993 0.6676 0.0610 Uiso calc H(15) 0.4051 -0.0981 0.6611 0.0600 Uiso calc H(16) 0.3784 0.0081 0.5761 0.0470 Uiso calc H(112) 0.0620 0.3868 0.2995 0.0440 Uiso calc H(113) -0.0479 0.4463 0.2246 0.0590 Uiso calc H(114) -0.1681 0.4329 0.2455 0.0660 Uiso calc H(115) -0.1783 0.3646 0.3409 0.0620 Uiso calc H(116) -0.0665 0.3100 0.4182 0.0490 Uiso calc H(122) 0.0457 0.4336 0.4968 0.0440 Uiso calc H(123) 0.0372 0.4510 0.6025 0.0600 Uiso calc H(124) 0.0726 0.3284 0.6770 0.0590 Uiso calc H(125) 0.1001 0.1866 0.6398 0.0540 Uiso calc H(126) 0.1056 0.1684 0.5323 0.0430 Uiso calc H(1B1) 0.1653 0.4092 0.3842 0.0330 Uiso calc H(1B2) 0.1645 0.4311 0.4568 0.0330 Uiso calc H(212) 0.3634 0.3758 0.3668 0.0430 Uiso calc H(213) 0.4478 0.4925 0.3586 0.0530 Uiso calc H(214) 0.4717 0.6140 0.4326 0.0570 Uiso calc H(215) 0.4107 0.6178 0.5156 0.0600 Uiso calc H(216) 0.3252 0.5003 0.5251 0.0500 Uiso calc H(222) 0.2112 0.4056 0.5671 0.0530 Uiso calc H(223) 0.2547 0.3927 0.6805 0.0660 Uiso calc H(224) 0.3653 0.3082 0.7288 0.0670 Uiso calc H(225) 0.4312 0.2317 0.6644 0.0570 Uiso calc H(226) 0.3854 0.2383 0.5514 0.0450 Uiso calc H(2B1) 0.1755 0.0002 0.2499 0.0320 Uiso calc H(2B2) 0.2182 -0.0837 0.2915 0.0320 Uiso calc H(312) -0.0372 0.0243 0.2890 0.0540 Uiso calc H(313) -0.1416 -0.0454 0.2126 0.0780 Uiso calc H(314) -0.1243 -0.1808 0.1615 0.0690 Uiso calc H(315) -0.0028 -0.2481 0.1858 0.0600 Uiso calc H(316) 0.1021 -0.1809 0.2619 0.0480 Uiso calc H(322) 0.0516 -0.0955 0.4284 0.0510 Uiso calc H(323) 0.0799 -0.2004 0.5143 0.0570 Uiso calc H(324) 0.2007 -0.2697 0.5476 0.0560 Uiso calc H(325) 0.2932 -0.2368 0.4932 0.0470 Uiso calc H(326) 0.2643 -0.1397 0.4028 0.0370 Uiso calc H(412) 0.4313 0.0680 0.2983 0.0460 Uiso calc H(413) 0.4688 0.1038 0.2047 0.0620 Uiso calc H(414) 0.3770 0.1480 0.1092 0.0590 Uiso calc H(415) 0.2472 0.1489 0.1066 0.0570 Uiso calc H(416) 0.2076 0.1136 0.1987 0.0460 Uiso calc H(422) 0.3490 -0.1103 0.2906 0.0370 Uiso calc H(423) 0.4245 -0.2324 0.3438 0.0430 Uiso calc H(424) 0.4814 -0.2268 0.4562 0.0440 Uiso calc H(425) 0.4667 -0.0964 0.5149 0.0370 Uiso calc H(426) 0.3895 0.0251 0.4626 0.0330 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) 0.01952(10) 0.02043(10) 0.01820(10) 0.00140(7) 0.00541(7) 0.00128(7) Re(2) 0.01957(10) 0.01993(10) 0.01735(10) 0.00055(7) 0.00406(7) 0.00124(7) Cl(11) 0.0263(6) 0.0360(6) 0.0205(6) 0.0010(5) 0.0013(5) 0.0037(5) Cl(12) 0.0266(6) 0.0337(6) 0.0348(7) -0.0003(5) 0.0139(5) -0.0013(5) Cl(21) 0.0295(6) 0.0283(6) 0.0231(6) -0.0018(5) 0.0042(5) 0.0078(5) Cl(22) 0.0228(6) 0.0285(6) 0.0311(7) -0.0002(4) 0.0048(5) 0.0036(5) P(1) 0.0244(7) 0.0217(6) 0.0242(7) 0.0026(5) 0.0058(5) 0.0029(5) P(2) 0.0237(7) 0.0222(6) 0.0240(7) 0.0018(5) 0.0036(5) 0.0003(5) P(3) 0.0221(6) 0.0222(6) 0.0221(6) -0.0007(5) 0.0078(5) -0.0011(5) P(4) 0.0203(6) 0.0226(6) 0.0181(6) -0.0014(5) 0.0045(5) -0.0005(4) O(1) 0.0259(18) 0.0257(16) 0.0173(16) 0.0026(13) 0.0069(14) 0.0037(13) O(2) 0.0269(18) 0.0237(16) 0.0185(17) 0.0022(13) 0.0054(14) 0.0014(13) N(14) 0.075(4) 0.043(3) 0.031(3) -0.008(3) -0.001(3) 0.009(2) C(10) 0.031(3) 0.020(2) 0.017(2) -0.0003(19) 0.007(2) 0.0011(17) C(11) 0.040(3) 0.025(2) 0.019(2) 0.006(2) 0.008(2) 0.0024(19) C(12) 0.047(4) 0.041(3) 0.031(3) -0.001(3) 0.015(3) 0.009(2) C(13) 0.055(4) 0.053(4) 0.032(3) -0.001(3) 0.011(3) 0.013(3) C(15) 0.055(4) 0.044(3) 0.030(3) 0.004(3) -0.004(3) 0.008(3) C(16) 0.038(3) 0.034(3) 0.032(3) 0.002(2) 0.002(2) 0.002(2) C(1B) 0.026(3) 0.018(2) 0.031(3) 0.0005(18) 0.005(2) 0.0022(19) C(2B) 0.021(2) 0.027(2) 0.025(3) -0.0038(19) 0.005(2) -0.0033(19) C(111) 0.030(3) 0.021(2) 0.033(3) 0.005(2) 0.006(2) 0.006(2) C(112) 0.029(3) 0.037(3) 0.032(3) 0.001(2) 0.001(2) 0.000(2) C(113) 0.046(4) 0.047(3) 0.036(3) 0.003(3) -0.003(3) 0.010(3) C(114) 0.036(4) 0.048(4) 0.056(4) 0.011(3) -0.009(3) 0.012(3) C(115) 0.026(3) 0.059(4) 0.054(4) 0.005(3) 0.005(3) 0.024(3) C(116) 0.031(3) 0.037(3) 0.045(4) 0.008(2) 0.010(3) 0.017(2) C(121) 0.028(3) 0.033(3) 0.025(3) 0.003(2) 0.008(2) 0.001(2) C(122) 0.039(3) 0.027(3) 0.038(3) 0.010(2) 0.014(3) 0.000(2) C(123) 0.050(4) 0.046(3) 0.051(4) 0.013(3) 0.027(3) -0.007(3) C(124) 0.057(4) 0.062(4) 0.025(3) 0.013(3) 0.024(3) -0.006(3) C(125) 0.054(4) 0.045(3) 0.028(3) 0.011(3) 0.015(3) 0.002(2) C(126) 0.041(3) 0.033(3) 0.028(3) 0.013(2) 0.014(2) 0.004(2) C(211) 0.026(3) 0.018(2) 0.038(3) -0.0017(19) 0.003(2) 0.002(2) C(212) 0.035(3) 0.028(3) 0.031(3) -0.003(2) 0.002(2) 0.004(2) C(213) 0.038(3) 0.029(3) 0.051(4) -0.001(2) 0.004(3) 0.013(2) C(214) 0.035(3) 0.029(3) 0.064(4) -0.004(2) 0.006(3) 0.005(3) C(215) 0.043(4) 0.022(3) 0.065(4) -0.007(2) 0.000(3) -0.007(3) C(216) 0.034(3) 0.031(3) 0.047(4) -0.004(2) 0.004(3) -0.003(2) C(221) 0.028(3) 0.031(3) 0.021(3) -0.003(2) 0.004(2) -0.002(2) C(222) 0.036(3) 0.050(3) 0.033(3) 0.005(3) 0.002(3) -0.013(3) C(223) 0.048(4) 0.071(4) 0.035(4) -0.010(3) 0.015(3) -0.023(3) C(224) 0.057(4) 0.071(4) 0.019(3) -0.003(3) -0.001(3) -0.008(3) C(225) 0.047(4) 0.047(3) 0.028(3) 0.006(3) -0.006(3) -0.001(3) C(226) 0.036(3) 0.034(3) 0.031(3) 0.001(2) 0.005(2) 0.000(2) C(311) 0.018(2) 0.024(2) 0.032(3) -0.0055(18) 0.005(2) -0.0032(19) C(312) 0.026(3) 0.039(3) 0.053(4) -0.001(2) 0.001(3) -0.016(3) C(313) 0.028(3) 0.052(4) 0.086(6) 0.002(3) -0.005(3) -0.016(4) C(314) 0.032(3) 0.054(4) 0.063(5) -0.006(3) -0.004(3) -0.024(3) C(315) 0.042(4) 0.032(3) 0.058(4) -0.012(2) 0.000(3) -0.019(3) C(316) 0.032(3) 0.030(3) 0.047(4) 0.000(2) 0.008(3) -0.009(2) C(321) 0.032(3) 0.022(2) 0.023(3) -0.003(2) 0.010(2) -0.0032(19) C(322) 0.043(3) 0.034(3) 0.051(4) 0.008(2) 0.029(3) 0.009(3) C(323) 0.057(4) 0.036(3) 0.053(4) 0.009(3) 0.039(3) 0.015(3) C(324) 0.066(4) 0.029(3) 0.037(3) 0.000(3) 0.021(3) 0.008(2) C(325) 0.038(3) 0.027(3) 0.038(3) 0.007(2) 0.002(3) 0.004(2) C(326) 0.026(3) 0.026(2) 0.034(3) -0.003(2) 0.012(2) 0.003(2) C(411) 0.028(3) 0.026(2) 0.024(3) -0.002(2) 0.009(2) -0.0013(19) C(412) 0.033(3) 0.040(3) 0.039(3) 0.003(2) 0.021(3) 0.011(2) C(413) 0.049(4) 0.045(3) 0.061(4) 0.005(3) 0.036(3) 0.009(3) C(414) 0.073(5) 0.039(3) 0.036(3) -0.007(3) 0.034(3) 0.005(3) C(415) 0.066(4) 0.042(3) 0.022(3) -0.018(3) 0.009(3) 0.003(2) C(416) 0.036(3) 0.039(3) 0.029(3) -0.010(2) 0.004(2) 0.003(2) C(421) 0.021(2) 0.026(2) 0.022(2) -0.0031(19) 0.0036(19) 0.0009(19) C(422) 0.027(3) 0.031(3) 0.028(3) -0.001(2) 0.008(2) -0.007(2) C(423) 0.031(3) 0.027(3) 0.039(3) 0.008(2) 0.005(2) -0.014(2) C(424) 0.031(3) 0.026(3) 0.039(3) 0.007(2) 0.002(2) 0.000(2) C(425) 0.030(3) 0.026(2) 0.024(3) 0.000(2) -0.002(2) 0.0006(19) C(426) 0.026(3) 0.023(2) 0.026(3) 0.0046(19) 0.006(2) -0.0002(19) # 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) 2.071(3) ? Re(1) Re(2) 2.3055(3) ? Re(1) Cl(11) 2.3511(12) ? Re(1) P(1) 2.4801(12) ? Re(1) P(3) 2.4848(11) ? Re(1) Cl(12) 2.5829(12) ? Re(2) O(2) 2.092(3) ? Re(2) Cl(21) 2.3653(11) ? Re(2) P(4) 2.4720(12) ? Re(2) P(2) 2.4901(12) ? Re(2) Cl(22) 2.5743(12) ? P(1) C(111) 1.827(5) ? P(1) C(121) 1.839(5) ? P(1) C(1B) 1.848(5) ? P(2) C(221) 1.818(5) ? P(2) C(1B) 1.824(5) ? P(2) C(211) 1.836(5) ? P(3) C(311) 1.821(5) ? P(3) C(2B) 1.822(5) ? P(3) C(321) 1.824(5) ? P(4) C(411) 1.817(5) ? P(4) C(421) 1.826(5) ? P(4) C(2B) 1.832(5) ? O(1) C(10) 1.268(6) ? O(2) C(10) 1.272(5) ? N(14) C(15) 1.328(8) ? N(14) C(13) 1.337(8) ? C(10) C(11) 1.493(6) ? C(11) C(12) 1.383(7) ? C(11) C(16) 1.393(7) ? C(12) C(13) 1.393(7) ? C(15) C(16) 1.394(7) ? C(111) C(112) 1.372(7) ? C(111) C(116) 1.382(7) ? C(112) C(113) 1.392(7) ? C(113) C(114) 1.375(9) ? C(114) C(115) 1.371(9) ? C(115) C(116) 1.407(7) ? C(121) C(122) 1.384(7) ? C(121) C(126) 1.386(7) ? C(122) C(123) 1.372(8) ? C(123) C(124) 1.400(8) ? C(124) C(125) 1.368(7) ? C(125) C(126) 1.389(7) ? C(211) C(212) 1.393(7) ? C(211) C(216) 1.396(7) ? C(212) C(213) 1.379(7) ? C(213) C(214) 1.384(8) ? C(214) C(215) 1.373(9) ? C(215) C(216) 1.401(7) ? C(221) C(222) 1.393(7) ? C(221) C(226) 1.399(7) ? C(222) C(223) 1.388(8) ? C(223) C(224) 1.379(9) ? C(224) C(225) 1.379(8) ? C(225) C(226) 1.378(7) ? C(311) C(312) 1.376(7) ? C(311) C(316) 1.394(7) ? C(312) C(313) 1.404(8) ? C(313) C(314) 1.370(8) ? C(314) C(315) 1.368(8) ? C(315) C(316) 1.393(7) ? C(321) C(322) 1.390(7) ? C(321) C(326) 1.388(7) ? C(322) C(323) 1.386(7) ? C(323) C(324) 1.373(8) ? C(324) C(325) 1.374(8) ? C(325) C(326) 1.386(7) ? C(411) C(412) 1.391(7) ? C(411) C(416) 1.393(7) ? C(412) C(413) 1.389(7) ? C(413) C(414) 1.378(9) ? C(414) C(415) 1.372(9) ? C(415) C(416) 1.380(7) ? C(421) C(426) 1.388(6) ? C(421) C(422) 1.398(6) ? C(422) C(423) 1.387(7) ? C(423) C(424) 1.383(7) ? C(424) C(425) 1.381(7) ? C(425) C(426) 1.391(6) ? 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) 88.55(9) ? O(1) Re(1) Cl(11) 165.81(9) ? Re(2) Re(1) Cl(11) 103.03(3) ? O(1) Re(1) P(1) 96.66(9) ? Re(2) Re(1) P(1) 92.00(3) ? Cl(11) Re(1) P(1) 91.17(4) ? O(1) Re(1) P(3) 85.44(9) ? Re(2) Re(1) P(3) 102.47(3) ? Cl(11) Re(1) P(3) 84.07(4) ? P(1) Re(1) P(3) 165.43(4) ? O(1) Re(1) Cl(12) 79.71(9) ? Re(2) Re(1) Cl(12) 163.47(3) ? Cl(11) Re(1) Cl(12) 90.43(4) ? P(1) Re(1) Cl(12) 78.00(4) ? P(3) Re(1) Cl(12) 88.26(4) ? O(2) Re(2) Re(1) 88.95(9) ? O(2) Re(2) Cl(21) 170.38(9) ? Re(1) Re(2) Cl(21) 100.21(3) ? O(2) Re(2) P(4) 93.35(9) ? Re(1) Re(2) P(4) 93.49(3) ? Cl(21) Re(2) P(4) 89.05(4) ? O(2) Re(2) P(2) 90.11(9) ? Re(1) Re(2) P(2) 103.43(3) ? Cl(21) Re(2) P(2) 84.94(4) ? P(4) Re(2) P(2) 162.79(4) ? O(2) Re(2) Cl(22) 83.37(9) ? Re(1) Re(2) Cl(22) 167.58(3) ? Cl(21) Re(2) Cl(22) 88.08(4) ? P(4) Re(2) Cl(22) 77.29(4) ? P(2) Re(2) Cl(22) 86.39(4) ? C(111) P(1) C(121) 104.3(2) ? C(111) P(1) C(1B) 103.0(2) ? C(121) P(1) C(1B) 102.0(2) ? C(111) P(1) Re(1) 112.92(17) ? C(121) P(1) Re(1) 118.53(16) ? C(1B) P(1) Re(1) 114.27(16) ? C(221) P(2) C(1B) 109.2(2) ? C(221) P(2) C(211) 102.0(2) ? C(1B) P(2) C(211) 104.4(2) ? C(221) P(2) Re(2) 116.01(16) ? C(1B) P(2) Re(2) 102.93(15) ? C(211) P(2) Re(2) 121.53(17) ? C(311) P(3) C(2B) 102.0(2) ? C(311) P(3) C(321) 103.6(2) ? C(2B) P(3) C(321) 109.6(2) ? C(311) P(3) Re(1) 122.76(16) ? C(2B) P(3) Re(1) 105.07(15) ? C(321) P(3) Re(1) 112.87(15) ? C(411) P(4) C(421) 103.3(2) ? C(411) P(4) C(2B) 101.4(2) ? C(421) P(4) C(2B) 102.1(2) ? C(411) P(4) Re(2) 114.87(15) ? C(421) P(4) Re(2) 118.22(16) ? C(2B) P(4) Re(2) 114.74(16) ? C(10) O(1) Re(1) 120.7(3) ? C(10) O(2) Re(2) 119.2(3) ? C(15) N(14) C(13) 117.3(5) ? O(1) C(10) O(2) 122.0(4) ? O(1) C(10) C(11) 117.1(4) ? O(2) C(10) C(11) 120.7(4) ? C(12) C(11) C(16) 118.9(5) ? C(12) C(11) C(10) 120.5(5) ? C(16) C(11) C(10) 120.5(5) ? C(11) C(12) C(13) 118.8(6) ? N(14) C(13) C(12) 123.1(6) ? N(14) C(15) C(16) 124.3(6) ? C(11) C(16) C(15) 117.6(5) ? P(2) C(1B) P(1) 110.2(2) ? P(3) C(2B) P(4) 112.9(2) ? C(112) C(111) C(116) 119.2(5) ? C(112) C(111) P(1) 119.9(4) ? C(116) C(111) P(1) 120.7(4) ? C(111) C(112) C(113) 121.5(6) ? C(114) C(113) C(112) 119.1(6) ? C(115) C(114) C(113) 120.5(5) ? C(114) C(115) C(116) 120.1(6) ? C(111) C(116) C(115) 119.6(5) ? C(122) C(121) C(126) 118.6(5) ? C(122) C(121) P(1) 120.2(4) ? C(126) C(121) P(1) 120.9(4) ? C(123) C(122) C(121) 121.5(5) ? C(122) C(123) C(124) 119.5(5) ? C(125) C(124) C(123) 119.4(5) ? C(124) C(125) C(126) 120.7(5) ? C(121) C(126) C(125) 120.1(5) ? C(212) C(211) C(216) 118.6(5) ? C(212) C(211) P(2) 123.0(4) ? C(216) C(211) P(2) 118.4(4) ? C(213) C(212) C(211) 120.6(5) ? C(212) C(213) C(214) 120.8(6) ? C(215) C(214) C(213) 119.4(5) ? C(214) C(215) C(216) 120.5(5) ? C(211) C(216) C(215) 120.1(6) ? C(222) C(221) C(226) 118.5(5) ? C(222) C(221) P(2) 124.5(4) ? C(226) C(221) P(2) 116.8(4) ? C(223) C(222) C(221) 120.2(5) ? C(224) C(223) C(222) 120.2(6) ? C(223) C(224) C(225) 120.3(6) ? C(226) C(225) C(224) 119.7(6) ? C(225) C(226) C(221) 121.0(5) ? C(312) C(311) C(316) 119.3(5) ? C(312) C(311) P(3) 123.0(4) ? C(316) C(311) P(3) 117.7(4) ? C(311) C(312) C(313) 119.6(5) ? C(314) C(313) C(312) 121.0(6) ? C(315) C(314) C(313) 119.4(5) ? C(314) C(315) C(316) 120.8(5) ? C(315) C(316) C(311) 120.0(5) ? C(322) C(321) C(326) 119.7(5) ? C(322) C(321) P(3) 116.3(4) ? C(326) C(321) P(3) 123.8(4) ? C(323) C(322) C(321) 119.5(5) ? C(324) C(323) C(322) 121.0(5) ? C(323) C(324) C(325) 119.3(5) ? C(324) C(325) C(326) 121.1(5) ? C(325) C(326) C(321) 119.4(5) ? C(412) C(411) C(416) 118.8(5) ? C(412) C(411) P(4) 120.6(4) ? C(416) C(411) P(4) 120.5(4) ? C(413) C(412) C(411) 120.1(5) ? C(414) C(413) C(412) 120.9(6) ? C(415) C(414) C(413) 118.6(5) ? C(414) C(415) C(416) 121.8(6) ? C(415) C(416) C(411) 119.7(5) ? C(426) C(421) C(422) 119.0(4) ? C(426) C(421) P(4) 122.3(4) ? C(422) C(421) P(4) 118.3(4) ? C(423) C(422) C(421) 120.1(5) ? C(424) C(423) C(422) 120.4(4) ? C(425) C(424) C(423) 119.8(4) ? C(424) C(425) C(426) 120.2(5) ? C(421) C(426) C(425) 120.4(4) ? #===END #CIFFILE FOR COMPLEX 14. #==================================================================== data_DFC36X _database_code_CSD 178306 _audit_creation_date 10-05-00 _audit_creation_method from_MolEN_and_SHELXL _audit_update_record ; ? ; # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.22 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C64.87 H60.60 Cl2 Fe O5.43 P4 Re2' _chemical_formula_structural ? _chemical_formula_weight 1550.17 _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 12.4909(2) _cell_length_b 17.7630(3) _cell_length_c 27.8096(6) _cell_angle_alpha 90.00 _cell_angle_beta 96.7556(12) _cell_angle_gamma 90.00 _cell_volume 6127.4(3) _cell_measurement_reflns_used 54835 _cell_measurement_theta_min 4 _cell_measurement_theta_max 28 _cell_formula_units_z 4 _exptl_crystal_density_diffrn 1.68 _exptl_crystal_density_meas ? _diffrn_radiation_type MO-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 4.468 _cell_measurement_temperature 173 _exptl_crystal_F_000 3044 # 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 0.1481 _exptl_absorpt_correction_T_max 0.3659 _diffrn_reflns_number 54835 _reflns_number_total 15590 _reflns_number_gt 12301 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.066 _diffrn_reflns_theta_min 4.00 _diffrn_reflns_theta_max 28.71 _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 23 _diffrn_reflns_limit_l_max 36 # 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 0.046 _refine_ls_wR_factor_ref 0.098 _refine_ls_hydrogen_treatment H_atoms_riding _refine_ls_number_reflns 15087 _refine_ls_number_parameters 705 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0532P)^2^+4.4513P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.022 _refine_diff_density_max 1.22 _refine_diff_density_min -2.02 _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) 0.200726(16) 0.177327(11) 0.133640(8) 0.02640(6) Uani ? Re(2) 0.265258(15) 0.104100(11) 0.199932(8) 0.02414(6) Uani ? Fe 0.04542(6) -0.07805(4) 0.08764(3) 0.0286(2) Uani ? Cl(1) 0.09242(13) 0.23544(8) 0.05903(6) 0.0468(5) Uani ? Cl(2) 0.34124(11) 0.00237(8) 0.25898(5) 0.0346(4) Uani ? P(1) 0.15158(11) 0.28600(8) 0.17664(6) 0.0288(4) Uani ? P(2) 0.20302(11) 0.18277(8) 0.26081(5) 0.0279(4) Uani ? P(3) 0.37064(12) 0.22556(8) 0.11420(6) 0.0323(4) Uani ? P(4) 0.44474(11) 0.15303(8) 0.21112(6) 0.0299(4) Uani ? O(11) 0.0514(3) 0.1164(2) 0.13424(14) 0.0301(10) Uani ? O(12) 0.1223(3) 0.0392(2) 0.19321(13) 0.0268(10) Uani ? O(21) 0.2142(3) 0.0866(2) 0.08620(14) 0.0319(10) Uani ? O(22) 0.2897(3) 0.01633(19) 0.14764(13) 0.0263(10) Uani ? O(901) 0.0400(16) 0.1491(10) 0.4283(6) 0.196(8) Uiso ? O(911) 0.786(2) 0.1828(16) 0.5330(11) 0.372(18) Uiso ? C(10) 0.0562(4) 0.0537(3) 0.1564(2) 0.0254(15) Uani ? C(11) -0.0159(4) -0.0080(3) 0.1362(2) 0.0281(15) Uani ? C(12) -0.0119(4) -0.0843(3) 0.1536(2) 0.0293(15) Uani ? C(13) -0.0766(4) -0.1285(3) 0.1189(2) 0.0347(17) Uani ? C(14) -0.1198(5) -0.0802(3) 0.0804(2) 0.0378(17) Uani ? C(15) -0.0830(4) -0.0060(3) 0.0907(2) 0.0327(15) Uani ? C(1B) 0.2088(4) 0.2805(3) 0.2402(2) 0.0329(17) Uani ? C(20) 0.2394(4) 0.0233(3) 0.1058(2) 0.0250(15) Uani ? C(21) 0.1987(4) -0.0444(3) 0.0791(2) 0.0290(15) Uani ? C(22) 0.1986(4) -0.1196(3) 0.0972(2) 0.0359(17) Uani ? C(23) 0.1358(5) -0.1642(3) 0.0631(2) 0.0436(19) Uani ? C(24) 0.0925(5) -0.1175(3) 0.0234(2) 0.043(2) Uani ? C(25) 0.1315(4) -0.0429(3) 0.0335(2) 0.0360(17) Uani ? C(2B) 0.4598(4) 0.2316(3) 0.1698(2) 0.0363(17) Uani ? C(111) 0.0081(4) 0.3067(3) 0.1796(2) 0.0334(17) Uani ? C(112) -0.0736(4) 0.2605(3) 0.1575(2) 0.0369(17) Uani ? C(113) -0.1796(5) 0.2784(4) 0.1622(3) 0.050(2) Uani ? C(114) -0.2066(5) 0.3386(4) 0.1883(3) 0.052(2) Uani ? C(115) -0.1260(5) 0.3851(3) 0.2107(3) 0.044(2) Uani ? C(116) -0.0198(4) 0.3699(3) 0.2055(2) 0.0366(17) Uani ? C(121) 0.1951(5) 0.3800(3) 0.1590(3) 0.0388(19) Uani ? C(122) 0.1397(7) 0.4139(4) 0.1195(3) 0.057(2) Uani ? C(123) 0.1720(8) 0.4825(4) 0.1026(3) 0.073(3) Uani ? C(124) 0.2582(8) 0.5185(4) 0.1265(4) 0.077(3) Uani ? C(125) 0.3135(7) 0.4864(4) 0.1662(5) 0.097(4) Uani ? C(126) 0.2828(6) 0.4161(4) 0.1844(4) 0.069(3) Uani ? C(211) 0.0654(4) 0.1702(3) 0.2754(2) 0.0294(15) Uani ? C(212) 0.0253(5) 0.0975(3) 0.2802(2) 0.0363(17) Uani ? C(213) -0.0767(5) 0.0863(4) 0.2962(3) 0.046(2) Uani ? C(214) -0.1375(5) 0.1481(4) 0.3058(2) 0.046(2) Uani ? C(215) -0.0976(5) 0.2197(4) 0.3017(2) 0.045(2) Uani ? C(216) 0.0036(4) 0.2302(3) 0.2866(2) 0.0352(17) Uani ? C(221) 0.2692(4) 0.1864(3) 0.3231(2) 0.0366(17) Uani ? C(222) 0.3010(5) 0.2544(4) 0.3462(2) 0.050(2) Uani ? C(223) 0.3422(6) 0.2550(5) 0.3944(3) 0.064(3) Uani ? C(224) 0.3524(6) 0.1894(5) 0.4211(3) 0.068(3) Uani ? C(225) 0.3216(6) 0.1223(5) 0.3994(3) 0.061(3) Uani ? C(226) 0.2789(5) 0.1195(4) 0.3499(2) 0.049(2) Uani ? C(311) 0.4395(5) 0.1678(3) 0.0725(2) 0.0401(19) Uani ? C(312) 0.5476(5) 0.1491(4) 0.0811(3) 0.057(2) Uani ? C(313) 0.5977(7) 0.1124(5) 0.0461(3) 0.073(3) Uani ? C(314) 0.5387(7) 0.0918(4) 0.0022(3) 0.066(3) Uani ? C(315) 0.4315(6) 0.1085(4) -0.0061(3) 0.054(2) Uani ? C(316) 0.3814(6) 0.1464(3) 0.0284(2) 0.0444(19) Uani ? C(321) 0.3924(5) 0.3188(3) 0.0877(2) 0.0410(19) Uani ? C(322) 0.3205(7) 0.3480(4) 0.0519(3) 0.063(3) Uani ? C(323) 0.3397(8) 0.4167(5) 0.0311(3) 0.075(3) Uani ? C(324) 0.4284(9) 0.4569(5) 0.0453(4) 0.086(4) Uani ? C(325) 0.5036(11) 0.4280(6) 0.0815(5) 0.138(6) Uani ? C(326) 0.4811(8) 0.3592(6) 0.1014(5) 0.131(5) Uani ? C(411) 0.5549(4) 0.0894(3) 0.1990(2) 0.0330(17) Uani ? C(412) 0.6612(5) 0.1147(4) 0.2053(2) 0.0446(19) Uani ? C(413) 0.7435(5) 0.0697(4) 0.1922(3) 0.051(2) Uani ? C(414) 0.7215(5) -0.0016(4) 0.1753(3) 0.052(2) Uani ? C(415) 0.6174(5) -0.0274(4) 0.1699(3) 0.047(2) Uani ? C(416) 0.5335(5) 0.0181(3) 0.1818(2) 0.0407(17) Uani ? C(421) 0.5033(4) 0.1954(3) 0.2691(2) 0.0343(17) Uani ? C(422) 0.5382(5) 0.2704(3) 0.2737(3) 0.0432(19) Uani ? C(423) 0.5823(5) 0.2982(4) 0.3186(3) 0.057(2) Uani ? C(424) 0.5946(5) 0.2521(4) 0.3583(3) 0.057(2) Uani ? C(425) 0.5613(5) 0.1779(4) 0.3544(3) 0.0458(19) Uani ? C(426) 0.5150(4) 0.1493(3) 0.3099(2) 0.0376(17) Uani ? C(902) 0.0617(19) 0.0903(13) 0.4638(8) 0.181(11) Uiso ? C(903) -0.0127(14) 0.1210(10) 0.4975(6) 0.125(7) Uiso ? C(912) 0.6892(18) 0.1845(13) 0.5009(8) 0.172(11) Uiso ? C(913) 0.7564(18) 0.1459(13) 0.4674(8) 0.189(12) Uiso ? H(12) 0.0261 -0.1015 0.1823 0.0380 Uiso calc H(13) -0.0887 -0.1800 0.1209 0.0450 Uiso calc H(14) -0.1649 -0.0951 0.0530 0.0490 Uiso calc H(15) -0.0992 0.0362 0.0715 0.0420 Uiso calc H(22) 0.2341 -0.1362 0.1266 0.0470 Uiso calc H(23) 0.1240 -0.2156 0.0658 0.0570 Uiso calc H(24) 0.0475 -0.1330 -0.0038 0.0570 Uiso calc H(25) 0.1160 -0.0008 0.0141 0.0470 Uiso calc H(112) -0.0571 0.2184 0.1398 0.0480 Uiso calc H(113) -0.2342 0.2481 0.1470 0.0640 Uiso calc H(114) -0.2786 0.3487 0.1913 0.0670 Uiso calc H(115) -0.1436 0.4262 0.2289 0.0570 Uiso calc H(116) 0.0340 0.4020 0.2195 0.0480 Uiso calc H(122) 0.0792 0.3902 0.1036 0.0730 Uiso calc H(123) 0.1347 0.5039 0.0751 0.0960 Uiso calc H(124) 0.2794 0.5651 0.1157 0.1000 Uiso calc H(125) 0.3731 0.5113 0.1820 0.1260 Uiso calc H(126) 0.3200 0.3950 0.2121 0.0890 Uiso calc H(1B1) 0.1683 0.3126 0.2597 0.0430 Uiso calc H(1B2) 0.2830 0.2977 0.2437 0.0430 Uiso calc H(212) 0.0662 0.0562 0.2730 0.0470 Uiso calc H(213) -0.1026 0.0379 0.3001 0.0600 Uiso calc H(214) -0.2060 0.1414 0.3152 0.0600 Uiso calc H(215) -0.1383 0.2611 0.3089 0.0580 Uiso calc H(216) 0.0299 0.2788 0.2841 0.0460 Uiso calc H(222) 0.2943 0.2993 0.3288 0.0660 Uiso calc H(223) 0.3635 0.3005 0.4092 0.0830 Uiso calc H(224) 0.3801 0.1907 0.4536 0.0880 Uiso calc H(225) 0.3288 0.0780 0.4174 0.0790 Uiso calc H(226) 0.2576 0.0739 0.3354 0.0640 Uiso calc H(2B1) 0.4461 0.2783 0.1860 0.0480 Uiso calc H(2B2) 0.5337 0.2329 0.1623 0.0480 Uiso calc H(312) 0.5868 0.1613 0.1107 0.0740 Uiso calc H(313) 0.6709 0.1014 0.0517 0.0950 Uiso calc H(314) 0.5725 0.0667 -0.0212 0.0860 Uiso calc H(315) 0.3920 0.0943 -0.0352 0.0710 Uiso calc H(316) 0.3085 0.1579 0.0223 0.0580 Uiso calc H(322) 0.2579 0.3215 0.0414 0.0820 Uiso calc H(323) 0.2897 0.4354 0.0066 0.0990 Uiso calc H(324) 0.4396 0.5033 0.0312 0.1120 Uiso calc H(325) 0.5666 0.4540 0.0920 0.1800 Uiso calc H(326) 0.5309 0.3398 0.1258 0.1700 Uiso calc H(412) 0.6769 0.1622 0.2183 0.0580 Uiso calc H(413) 0.8137 0.0879 0.1950 0.0670 Uiso calc H(414) 0.7771 -0.0325 0.1674 0.0670 Uiso calc H(415) 0.6026 -0.0758 0.1582 0.0620 Uiso calc H(416) 0.4631 0.0000 0.1782 0.0530 Uiso calc H(422) 0.5318 0.3018 0.2467 0.0570 Uiso calc H(423) 0.6035 0.3483 0.3216 0.0730 Uiso calc H(424) 0.6255 0.2708 0.3880 0.0740 Uiso calc H(425) 0.5696 0.1469 0.3816 0.0590 Uiso calc H(426) 0.4921 0.0995 0.3075 0.0490 Uiso calc H(901) 0.0426 0.1901 0.4419 0.2550 Uiso calc H(90A) 0.1364 0.0893 0.4781 0.2350 Uiso calc H(90B) 0.0400 0.0409 0.4512 0.2350 Uiso calc H(90C) 0.0285 0.1472 0.5237 0.1630 Uiso calc H(90D) -0.0513 0.0803 0.5103 0.1630 Uiso calc H(90E) -0.0630 0.1551 0.4803 0.1630 Uiso calc H(911) 0.7855 0.2175 0.5525 0.4830 Uiso calc H(91A) 0.6648 0.2345 0.4907 0.2240 Uiso calc H(91B) 0.6310 0.1542 0.5108 0.2240 Uiso calc H(91C) 0.8081 0.1808 0.4573 0.2460 Uiso calc H(91D) 0.7109 0.1279 0.4395 0.2460 Uiso calc H(91E) 0.7934 0.1042 0.4838 0.2460 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) 0.02805(12) 0.01996(11) 0.03085(14) -0.00205(8) 0.00202(9) -0.00129(9) Re(2) 0.02230(11) 0.02140(11) 0.02856(13) -0.00103(8) 0.00238(8) -0.00291(9) Fe 0.0299(4) 0.0234(4) 0.0323(5) -0.0028(3) 0.0022(3) -0.0045(3) Cl(1) 0.0629(10) 0.0331(8) 0.0406(9) -0.0038(7) -0.0098(7) 0.0036(7) Cl(2) 0.0339(7) 0.0305(7) 0.0385(9) -0.0022(6) 0.0009(6) 0.0047(6) P(1) 0.0269(7) 0.0202(7) 0.0395(9) -0.0017(6) 0.0052(6) -0.0026(6) P(2) 0.0271(7) 0.0258(7) 0.0301(8) 0.0018(6) 0.0010(6) -0.0057(6) P(3) 0.0341(8) 0.0255(8) 0.0381(9) -0.0029(6) 0.0076(6) 0.0034(7) P(4) 0.0244(7) 0.0265(7) 0.0384(9) -0.0017(6) 0.0024(6) -0.0037(7) O(11) 0.0282(19) 0.024(2) 0.037(2) 0.0019(15) -0.0009(16) -0.0028(17) O(12) 0.0222(18) 0.029(2) 0.029(2) -0.0009(15) 0.0021(15) -0.0014(17) O(21) 0.044(2) 0.020(2) 0.032(2) -0.0017(16) 0.0051(18) -0.0027(17) O(22) 0.0266(19) 0.025(2) 0.027(2) 0.0015(15) 0.0018(16) -0.0052(16) C(10) 0.025(3) 0.023(3) 0.029(3) 0.000(2) 0.007(2) -0.007(2) C(11) 0.021(3) 0.032(3) 0.031(3) -0.003(2) 0.002(2) -0.007(2) C(12) 0.032(3) 0.025(3) 0.031(3) -0.004(2) 0.004(2) 0.000(2) C(13) 0.033(3) 0.030(3) 0.041(4) -0.003(2) 0.004(3) -0.004(3) C(14) 0.035(3) 0.039(3) 0.039(4) -0.010(3) 0.003(3) -0.005(3) C(15) 0.028(3) 0.034(3) 0.036(3) -0.002(2) 0.003(2) 0.002(3) C(1B) 0.029(3) 0.028(3) 0.041(4) -0.004(2) 0.001(2) -0.005(3) C(20) 0.022(3) 0.027(3) 0.027(3) -0.001(2) 0.007(2) -0.003(2) C(21) 0.025(3) 0.030(3) 0.033(3) 0.004(2) 0.007(2) -0.004(3) C(22) 0.033(3) 0.026(3) 0.049(4) 0.006(2) 0.006(3) -0.004(3) C(23) 0.045(4) 0.032(3) 0.054(4) 0.001(3) 0.007(3) -0.017(3) C(24) 0.048(4) 0.042(4) 0.041(4) -0.007(3) 0.008(3) -0.023(3) C(25) 0.039(3) 0.036(3) 0.034(4) -0.001(3) 0.009(3) -0.007(3) C(2B) 0.029(3) 0.029(3) 0.052(4) -0.008(2) 0.009(3) -0.004(3) C(111) 0.033(3) 0.029(3) 0.039(4) 0.002(2) 0.007(3) 0.005(3) C(112) 0.028(3) 0.033(3) 0.049(4) -0.002(2) 0.001(3) 0.000(3) C(113) 0.034(3) 0.043(4) 0.071(5) -0.005(3) 0.002(3) -0.006(4) C(114) 0.033(3) 0.044(4) 0.078(5) 0.003(3) 0.007(3) 0.006(4) C(115) 0.044(4) 0.030(3) 0.060(5) 0.007(3) 0.013(3) 0.001(3) C(116) 0.031(3) 0.033(3) 0.046(4) -0.002(2) 0.005(3) 0.004(3) C(121) 0.044(3) 0.016(3) 0.060(5) -0.003(2) 0.021(3) -0.008(3) C(122) 0.082(5) 0.043(4) 0.047(5) -0.003(4) 0.017(4) 0.001(3) C(123) 0.135(8) 0.031(4) 0.062(6) 0.000(5) 0.044(5) 0.004(4) C(124) 0.108(7) 0.026(4) 0.111(8) -0.004(4) 0.072(6) -0.006(5) C(125) 0.058(5) 0.034(4) 0.204(13) -0.018(4) 0.035(7) -0.001(6) C(126) 0.043(4) 0.028(4) 0.134(8) -0.007(3) 0.006(4) 0.002(4) C(211) 0.031(3) 0.027(3) 0.030(3) 0.003(2) 0.003(2) -0.002(2) C(212) 0.040(3) 0.027(3) 0.043(4) 0.004(2) 0.009(3) -0.005(3) C(213) 0.039(3) 0.038(4) 0.063(5) -0.001(3) 0.017(3) 0.001(3) C(214) 0.040(4) 0.047(4) 0.055(5) 0.004(3) 0.024(3) 0.007(3) C(215) 0.048(4) 0.042(4) 0.048(4) 0.016(3) 0.022(3) 0.003(3) C(216) 0.037(3) 0.032(3) 0.038(4) 0.000(3) 0.010(3) 0.001(3) C(221) 0.031(3) 0.045(4) 0.032(3) 0.012(3) -0.004(2) -0.011(3) C(222) 0.047(4) 0.056(4) 0.045(4) 0.014(3) -0.007(3) -0.016(4) C(223) 0.058(4) 0.080(6) 0.049(5) 0.011(4) -0.014(4) -0.031(4) C(224) 0.068(5) 0.099(7) 0.031(4) 0.020(5) -0.014(4) -0.016(4) C(225) 0.061(5) 0.074(5) 0.046(5) 0.026(4) 0.004(4) 0.002(4) C(226) 0.047(4) 0.058(4) 0.040(4) 0.015(3) -0.004(3) -0.006(3) C(311) 0.050(4) 0.036(3) 0.037(4) 0.000(3) 0.016(3) 0.013(3) C(312) 0.041(4) 0.074(5) 0.061(5) 0.007(4) 0.021(3) 0.003(4) C(313) 0.060(5) 0.085(6) 0.079(7) 0.023(4) 0.029(5) 0.019(5) C(314) 0.085(6) 0.049(5) 0.071(6) 0.017(4) 0.042(5) 0.008(4) C(315) 0.084(6) 0.039(4) 0.045(4) 0.007(4) 0.028(4) 0.004(3) C(316) 0.061(4) 0.034(3) 0.040(4) 0.001(3) 0.014(3) 0.008(3) C(321) 0.050(4) 0.030(3) 0.047(4) -0.005(3) 0.022(3) 0.010(3) C(322) 0.092(6) 0.049(4) 0.052(5) -0.002(4) 0.024(4) 0.019(4) C(323) 0.114(8) 0.067(6) 0.051(5) 0.020(5) 0.034(5) 0.032(4) C(324) 0.124(8) 0.035(5) 0.115(9) 0.024(5) 0.079(7) 0.022(5) C(325) 0.145(11) 0.082(8) 0.183(14) -0.064(7) -0.001(10) 0.062(9) C(326) 0.092(7) 0.090(7) 0.199(13) -0.063(6) -0.036(7) 0.090(8) C(411) 0.024(3) 0.036(3) 0.039(4) -0.001(2) 0.004(2) 0.005(3) C(412) 0.032(3) 0.047(4) 0.056(4) -0.007(3) 0.010(3) -0.007(3) C(413) 0.023(3) 0.062(5) 0.070(5) 0.003(3) 0.009(3) 0.003(4) C(414) 0.039(4) 0.057(5) 0.062(5) 0.006(3) 0.019(3) 0.001(4) C(415) 0.038(3) 0.040(4) 0.065(5) 0.005(3) 0.010(3) -0.012(3) C(416) 0.031(3) 0.035(3) 0.055(4) 0.004(3) 0.001(3) -0.002(3) C(421) 0.022(3) 0.037(3) 0.043(4) 0.001(2) 0.000(2) -0.007(3) C(422) 0.037(3) 0.037(4) 0.052(4) -0.007(3) -0.010(3) -0.009(3) C(423) 0.049(4) 0.044(4) 0.073(6) -0.014(3) -0.008(4) -0.018(4) C(424) 0.045(4) 0.068(5) 0.054(5) -0.004(4) -0.010(3) -0.011(4) C(425) 0.036(3) 0.049(4) 0.050(4) 0.002(3) -0.005(3) -0.003(3) C(426) 0.029(3) 0.036(3) 0.047(4) 0.000(3) 0.001(3) -0.007(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(1) O(21) 2.102(4) ? Re(1) O(11) 2.158(3) ? Re(1) Re(2) 2.3218(3) ? Re(1) P(1) 2.3887(14) ? Re(1) P(3) 2.4085(14) ? Re(1) Cl(1) 2.5574(15) ? Re(2) O(12) 2.115(3) ? Re(2) O(22) 2.178(3) ? Re(2) P(4) 2.3904(14) ? Re(2) P(2) 2.3945(14) ? Re(2) Cl(2) 2.5486(14) ? Fe C(22) 2.039(5) ? Fe C(21) 2.046(5) ? Fe C(25) 2.046(6) ? Fe C(13) 2.048(6) ? Fe C(12) 2.049(6) ? Fe C(11) 2.050(5) ? Fe C(14) 2.051(6) ? Fe C(15) 2.061(5) ? Fe C(23) 2.064(6) ? Fe C(24) 2.067(6) ? P(1) C(1B) 1.829(6) ? P(1) C(121) 1.840(6) ? P(1) C(111) 1.841(6) ? P(2) C(211) 1.826(5) ? P(2) C(221) 1.831(6) ? P(2) C(1B) 1.832(6) ? P(3) C(2B) 1.800(6) ? P(3) C(311) 1.836(6) ? P(3) C(321) 1.845(6) ? P(4) C(2B) 1.831(6) ? P(4) C(411) 1.843(6) ? P(4) C(421) 1.851(6) ? O(11) C(10) 1.271(6) ? O(12) C(10) 1.264(6) ? O(21) C(20) 1.273(6) ? O(22) C(20) 1.261(6) ? C(10) C(11) 1.486(7) ? C(11) C(15) 1.434(8) ? C(11) C(12) 1.438(7) ? C(12) C(13) 1.420(8) ? C(13) C(14) 1.428(9) ? C(14) C(15) 1.413(8) ? C(20) C(21) 1.472(7) ? C(21) C(22) 1.428(8) ? C(21) C(25) 1.436(8) ? C(22) C(23) 1.402(8) ? C(23) C(24) 1.435(9) ? C(24) C(25) 1.428(8) ? C(111) C(112) 1.396(8) ? C(111) C(116) 1.400(8) ? C(112) C(113) 1.382(8) ? C(113) C(114) 1.357(9) ? C(114) C(115) 1.392(9) ? C(115) C(116) 1.377(8) ? C(121) C(122) 1.368(10) ? C(121) C(126) 1.388(9) ? C(122) C(123) 1.383(10) ? C(123) C(124) 1.357(12) ? C(124) C(125) 1.357(13) ? C(125) C(126) 1.416(11) ? C(211) C(216) 1.374(7) ? C(211) C(212) 1.397(7) ? C(212) C(213) 1.412(8) ? C(213) C(214) 1.379(8) ? C(214) C(215) 1.375(9) ? C(215) C(216) 1.390(8) ? C(221) C(226) 1.401(9) ? C(221) C(222) 1.402(8) ? C(222) C(223) 1.379(9) ? C(223) C(224) 1.379(11) ? C(224) C(225) 1.371(11) ? C(225) C(226) 1.417(10) ? C(311) C(312) 1.384(9) ? C(311) C(316) 1.403(9) ? C(312) C(313) 1.382(10) ? C(313) C(314) 1.398(12) ? C(314) C(315) 1.365(11) ? C(315) C(316) 1.381(9) ? C(321) C(326) 1.337(10) ? C(321) C(322) 1.364(10) ? C(322) C(323) 1.383(10) ? C(323) C(324) 1.338(13) ? C(324) C(325) 1.393(15) ? C(325) C(326) 1.383(12) ? C(411) C(416) 1.368(8) ? C(411) C(412) 1.393(8) ? C(412) C(413) 1.384(9) ? C(413) C(414) 1.369(9) ? C(414) C(415) 1.370(9) ? C(415) C(416) 1.394(8) ? C(421) C(426) 1.393(8) ? C(421) C(422) 1.403(8) ? C(422) C(423) 1.394(9) ? C(423) C(424) 1.368(10) ? C(424) C(425) 1.384(9) ? C(425) C(426) 1.399(9) ? O(901) C(902) 1.44(2) ? C(902) C(903) 1.499(19) ? O(911) C(912) 1.41(2) ? C(912) C(913) 1.49(2) ? 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(21) Re(1) O(11) 75.72(14) ? O(21) Re(1) Re(2) 91.30(10) ? O(11) Re(1) Re(2) 86.15(10) ? O(21) Re(1) P(1) 167.97(11) ? O(11) Re(1) P(1) 97.35(10) ? Re(2) Re(1) P(1) 98.10(4) ? O(21) Re(1) P(3) 89.69(11) ? O(11) Re(1) P(3) 164.87(11) ? Re(2) Re(1) P(3) 98.32(4) ? P(1) Re(1) P(3) 96.31(5) ? O(21) Re(1) Cl(1) 82.77(11) ? O(11) Re(1) Cl(1) 80.40(11) ? Re(2) Re(1) Cl(1) 166.27(4) ? P(1) Re(1) Cl(1) 86.41(5) ? P(3) Re(1) Cl(1) 94.03(5) ? O(12) Re(2) O(22) 74.59(13) ? O(12) Re(2) Re(1) 91.40(10) ? O(22) Re(2) Re(1) 86.20(9) ? O(12) Re(2) P(4) 168.17(10) ? O(22) Re(2) P(4) 98.28(9) ? Re(1) Re(2) P(4) 97.60(4) ? O(12) Re(2) P(2) 92.27(10) ? O(22) Re(2) P(2) 166.57(10) ? Re(1) Re(2) P(2) 97.08(4) ? P(4) Re(2) P(2) 94.20(5) ? O(12) Re(2) Cl(2) 85.24(10) ? O(22) Re(2) Cl(2) 81.48(10) ? Re(1) Re(2) Cl(2) 167.68(3) ? P(4) Re(2) Cl(2) 84.35(5) ? P(2) Re(2) Cl(2) 94.90(5) ? C(22) Fe C(21) 40.9(2) ? C(22) Fe C(25) 68.9(2) ? C(21) Fe C(25) 41.1(2) ? C(22) Fe C(13) 121.3(2) ? C(21) Fe C(13) 158.5(2) ? C(25) Fe C(13) 158.0(2) ? C(22) Fe C(12) 106.5(2) ? C(21) Fe C(12) 123.3(2) ? C(25) Fe C(12) 160.7(2) ? C(13) Fe C(12) 40.6(2) ? C(22) Fe C(11) 123.4(2) ? C(21) Fe C(11) 109.0(2) ? C(25) Fe C(11) 124.6(2) ? C(13) Fe C(11) 68.4(2) ? C(12) Fe C(11) 41.1(2) ? C(22) Fe C(14) 157.6(2) ? C(21) Fe C(14) 159.9(2) ? C(25) Fe C(14) 122.9(2) ? C(13) Fe C(14) 40.8(2) ? C(12) Fe C(14) 68.5(2) ? C(11) Fe C(14) 68.1(2) ? C(22) Fe C(15) 160.4(2) ? C(21) Fe C(15) 124.5(2) ? C(25) Fe C(15) 108.6(2) ? C(13) Fe C(15) 68.4(2) ? C(12) Fe C(15) 69.0(2) ? C(11) Fe C(15) 40.8(2) ? C(14) Fe C(15) 40.2(2) ? C(22) Fe C(23) 40.0(2) ? C(21) Fe C(23) 67.8(2) ? C(25) Fe C(23) 68.2(3) ? C(13) Fe C(23) 106.2(2) ? C(12) Fe C(23) 121.2(2) ? C(11) Fe C(23) 158.2(3) ? C(14) Fe C(23) 122.5(2) ? C(15) Fe C(23) 158.8(2) ? C(22) Fe C(24) 68.4(3) ? C(21) Fe C(24) 68.5(2) ? C(25) Fe C(24) 40.6(2) ? C(13) Fe C(24) 121.3(2) ? C(12) Fe C(24) 156.9(2) ? C(11) Fe C(24) 160.3(3) ? C(14) Fe C(24) 107.1(3) ? C(15) Fe C(24) 123.2(3) ? C(23) Fe C(24) 40.6(3) ? C(1B) P(1) C(121) 102.2(3) ? C(1B) P(1) C(111) 103.8(3) ? C(121) P(1) C(111) 98.6(3) ? C(1B) P(1) Re(1) 110.26(19) ? C(121) P(1) Re(1) 119.93(19) ? C(111) P(1) Re(1) 119.54(19) ? C(211) P(2) C(221) 97.3(3) ? C(211) P(2) C(1B) 105.0(3) ? C(221) P(2) C(1B) 103.4(3) ? C(211) P(2) Re(2) 118.54(18) ? C(221) P(2) Re(2) 122.81(18) ? C(1B) P(2) Re(2) 107.7(2) ? C(2B) P(3) C(311) 106.7(3) ? C(2B) P(3) C(321) 100.6(3) ? C(311) P(3) C(321) 98.5(3) ? C(2B) P(3) Re(1) 107.52(19) ? C(311) P(3) Re(1) 115.7(2) ? C(321) P(3) Re(1) 125.7(2) ? C(2B) P(4) C(411) 102.6(3) ? C(2B) P(4) C(421) 100.2(3) ? C(411) P(4) C(421) 100.5(3) ? C(2B) P(4) Re(2) 111.08(18) ? C(411) P(4) Re(2) 117.53(18) ? C(421) P(4) Re(2) 121.99(18) ? C(10) O(11) Re(1) 116.8(3) ? C(10) O(12) Re(2) 115.1(3) ? C(20) O(21) Re(1) 116.2(3) ? C(20) O(22) Re(2) 116.8(3) ? O(12) C(10) O(11) 124.1(5) ? O(12) C(10) C(11) 117.7(5) ? O(11) C(10) C(11) 118.1(5) ? C(15) C(11) C(12) 108.3(5) ? C(15) C(11) C(10) 125.5(5) ? C(12) C(11) C(10) 124.9(5) ? C(15) C(11) Fe 70.0(3) ? C(12) C(11) Fe 69.5(3) ? C(10) C(11) Fe 116.1(3) ? C(13) C(12) C(11) 107.3(5) ? C(13) C(12) Fe 69.7(3) ? C(11) C(12) Fe 69.5(3) ? C(12) C(13) C(14) 108.2(5) ? C(12) C(13) Fe 69.8(3) ? C(14) C(13) Fe 69.7(3) ? C(15) C(14) C(13) 108.8(5) ? C(15) C(14) Fe 70.3(3) ? C(13) C(14) Fe 69.5(3) ? C(14) C(15) C(11) 107.4(5) ? C(14) C(15) Fe 69.5(3) ? C(11) C(15) Fe 69.2(3) ? P(1) C(1B) P(2) 109.1(3) ? O(22) C(20) O(21) 123.6(5) ? O(22) C(20) C(21) 119.4(5) ? O(21) C(20) C(21) 116.8(5) ? C(22) C(21) C(25) 107.7(5) ? C(22) C(21) C(20) 126.9(5) ? C(25) C(21) C(20) 124.2(5) ? C(22) C(21) Fe 69.3(3) ? C(25) C(21) Fe 69.5(3) ? C(20) C(21) Fe 116.9(3) ? C(23) C(22) C(21) 108.2(6) ? C(23) C(22) Fe 71.0(3) ? C(21) C(22) Fe 69.8(3) ? C(22) C(23) C(24) 109.0(5) ? C(22) C(23) Fe 69.1(3) ? C(24) C(23) Fe 69.8(3) ? C(25) C(24) C(23) 107.2(5) ? C(25) C(24) Fe 68.9(3) ? C(23) C(24) Fe 69.5(3) ? C(24) C(25) C(21) 107.9(5) ? C(24) C(25) Fe 70.5(3) ? C(21) C(25) Fe 69.4(3) ? P(3) C(2B) P(4) 113.3(3) ? C(112) C(111) C(116) 119.0(5) ? C(112) C(111) P(1) 121.9(4) ? C(116) C(111) P(1) 119.1(4) ? C(113) C(112) C(111) 118.8(6) ? C(114) C(113) C(112) 122.3(6) ? C(113) C(114) C(115) 119.6(6) ? C(116) C(115) C(114) 119.5(6) ? C(115) C(116) C(111) 120.8(6) ? C(122) C(121) C(126) 119.9(6) ? C(122) C(121) P(1) 118.4(5) ? C(126) C(121) P(1) 121.7(6) ? C(121) C(122) C(123) 121.4(8) ? C(124) C(123) C(122) 119.7(9) ? C(123) C(124) C(125) 120.0(8) ? C(124) C(125) C(126) 121.8(9) ? C(121) C(126) C(125) 117.2(9) ? C(216) C(211) C(212) 118.5(5) ? C(216) C(211) P(2) 121.6(4) ? C(212) C(211) P(2) 119.5(4) ? C(211) C(212) C(213) 120.5(5) ? C(214) C(213) C(212) 119.2(6) ? C(215) C(214) C(213) 120.4(6) ? C(214) C(215) C(216) 120.1(5) ? C(211) C(216) C(215) 121.3(5) ? C(226) C(221) C(222) 119.0(6) ? C(226) C(221) P(2) 118.3(5) ? C(222) C(221) P(2) 122.4(5) ? C(223) C(222) C(221) 120.3(7) ? C(222) C(223) C(224) 121.1(7) ? C(225) C(224) C(223) 119.7(7) ? C(224) C(225) C(226) 120.7(7) ? C(221) C(226) C(225) 119.1(7) ? C(312) C(311) C(316) 118.7(6) ? C(312) C(311) P(3) 123.0(5) ? C(316) C(311) P(3) 118.1(5) ? C(313) C(312) C(311) 120.3(8) ? C(312) C(313) C(314) 120.2(7) ? C(315) C(314) C(313) 119.8(7) ? C(314) C(315) C(316) 120.3(8) ? C(315) C(316) C(311) 120.7(7) ? C(326) C(321) C(322) 117.1(7) ? C(326) C(321) P(3) 121.7(6) ? C(322) C(321) P(3) 121.2(5) ? C(321) C(322) C(323) 120.6(8) ? C(324) C(323) C(322) 121.7(9) ? C(323) C(324) C(325) 118.7(8) ? C(326) C(325) C(324) 117.6(10) ? C(321) C(326) C(325) 124.1(10) ? C(416) C(411) C(412) 119.2(5) ? C(416) C(411) P(4) 120.8(4) ? C(412) C(411) P(4) 120.0(5) ? C(413) C(412) C(411) 120.4(6) ? C(414) C(413) C(412) 120.0(6) ? C(413) C(414) C(415) 119.7(6) ? C(414) C(415) C(416) 120.8(6) ? C(411) C(416) C(415) 119.8(6) ? C(426) C(421) C(422) 118.9(6) ? C(426) C(421) P(4) 117.6(4) ? C(422) C(421) P(4) 123.5(5) ? C(423) C(422) C(421) 120.2(7) ? C(424) C(423) C(422) 120.4(6) ? C(423) C(424) C(425) 120.2(7) ? C(424) C(425) C(426) 120.3(7) ? C(421) C(426) C(425) 120.0(6) ? O(901) C(902) C(903) 94.9(15) ? O(911) C(912) C(913) 83.3(16) ? #===END #CIFFILE FOR COMPLEX 11. data_CYL26X _database_code_CSD 178307 _audit_creation_date 22-03-00 _audit_creation_method from_MolEN_and_SHELXL _audit_update_record ; ? ; # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description chunk _exptl_crystal_colour orange _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.28 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C74 H86 Cl2 O10 P4 Re2' _chemical_formula_structural ? _chemical_formula_weight 1702.71 _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 22.1984(10) _cell_length_b 12.4860(4) _cell_length_c 25.8565(12) _cell_angle_alpha 90.00 _cell_angle_beta 99.5236(18) _cell_angle_gamma 90.00 _cell_volume 7067.9(9) _cell_measurement_reflns_used 22575 _cell_measurement_theta_min 4 _cell_measurement_theta_max 27 _cell_formula_units_z 4 _exptl_crystal_density_diffrn 1.60 _exptl_crystal_density_meas ? _diffrn_radiation_type MO-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 3.690 _cell_measurement_temperature 173 _exptl_crystal_F_000 3416 # 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 0.2170 _exptl_absorpt_correction_T_max 0.3625 _diffrn_reflns_number 22575 _reflns_number_total 14030 _reflns_number_gt 9977 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.080 _diffrn_reflns_theta_min 4.00 _diffrn_reflns_theta_max 27.53 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_max 33 # 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 0.046 _refine_ls_wR_factor_ref 0.082 _refine_ls_hydrogen_treatment H_atoms_riding _refine_ls_number_reflns 7844 _refine_ls_number_parameters 418 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 0.936 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0277P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.003 _refine_diff_density_max 1.85 _refine_diff_density_min -1.82 _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 0.042461(11) 0.069509(17) 0.282610(9) 0.02411(7) Uani ? Cl 0.13715(7) 0.02367(13) 0.34806(6) 0.0396(5) Uani ? P(1) 0.09764(7) 0.21684(12) 0.25526(6) 0.0257(4) Uani ? P(2) -0.00541(7) 0.17760(12) 0.34156(6) 0.0265(4) Uani ? O(11) 0.08226(17) -0.0483(3) 0.23704(16) 0.0291(12) Uani ? O(12) 0.00893(17) -0.0718(3) 0.31278(15) 0.0297(10) Uani ? O(17) -0.1330(2) -0.5619(4) 0.3741(2) 0.067(2) Uani ? O(18) -0.2000(2) -0.4551(4) 0.40247(19) 0.0496(16) Uani ? O(901) 0.0999(4) -0.2352(5) 0.3758(3) 0.112(3) Uani ? C(10) -0.0471(3) -0.0973(5) 0.2985(2) 0.0301(19) Uani ? C(11) -0.0706(3) -0.1912(4) 0.3261(2) 0.0284(17) Uani ? C(12) -0.1370(3) -0.1826(5) 0.3316(3) 0.036(2) Uani ? C(13) -0.1550(3) -0.2738(5) 0.3647(3) 0.039(2) Uani ? C(14) -0.1424(3) -0.3821(5) 0.3415(2) 0.0354(19) Uani ? C(15) -0.0768(3) -0.3902(5) 0.3317(3) 0.047(2) Uani ? C(16) -0.0597(3) -0.2965(4) 0.2995(3) 0.047(2) Uani ? C(17) -0.1569(3) -0.4771(5) 0.3739(3) 0.037(2) Uani ? C(19) -0.2188(4) -0.5443(6) 0.4332(3) 0.057(3) Uani ? C(1B) 0.0541(3) 0.2776(4) 0.1965(2) 0.0277(17) Uani ? C(20) -0.2520(4) -0.4978(7) 0.4730(3) 0.074(3) Uani ? C(111) 0.1726(3) 0.1968(4) 0.2354(2) 0.0292(17) Uani ? C(112) 0.1971(3) 0.0976(5) 0.2303(3) 0.037(2) Uani ? C(113) 0.2506(3) 0.0867(5) 0.2096(3) 0.040(2) Uani ? C(114) 0.2805(3) 0.1761(5) 0.1947(3) 0.041(2) Uani ? C(115) 0.2566(3) 0.2775(6) 0.2008(3) 0.043(2) Uani ? C(116) 0.2030(3) 0.2885(5) 0.2215(2) 0.034(2) Uani ? C(121) 0.1169(3) 0.3288(4) 0.3006(2) 0.0282(17) Uani ? C(122) 0.1641(3) 0.3125(5) 0.3425(3) 0.039(2) Uani ? C(123) 0.1798(3) 0.3911(6) 0.3798(3) 0.048(2) Uani ? C(124) 0.1496(3) 0.4877(5) 0.3758(3) 0.048(2) Uani ? C(125) 0.1033(3) 0.5067(5) 0.3347(3) 0.044(2) Uani ? C(126) 0.0875(3) 0.4283(5) 0.2967(3) 0.0344(19) Uani ? C(211) -0.0544(3) 0.1076(5) 0.3814(2) 0.0297(17) Uani ? C(212) -0.1118(3) 0.1414(5) 0.3881(2) 0.037(2) Uani ? C(213) -0.1428(3) 0.0885(6) 0.4231(3) 0.048(2) Uani ? C(214) -0.1171(3) 0.0049(5) 0.4524(3) 0.046(2) Uani ? C(215) -0.0593(3) -0.0302(5) 0.4467(3) 0.040(2) Uani ? C(216) -0.0288(3) 0.0194(5) 0.4109(2) 0.0350(19) Uani ? C(221) 0.0368(3) 0.2551(5) 0.3967(3) 0.0319(19) Uani ? C(222) 0.0854(3) 0.2108(5) 0.4298(3) 0.043(2) Uani ? C(223) 0.1113(3) 0.2636(6) 0.4750(3) 0.049(2) Uani ? C(224) 0.0894(4) 0.3605(6) 0.4881(3) 0.051(3) Uani ? C(225) 0.0423(4) 0.4068(5) 0.4555(3) 0.049(2) Uani ? C(226) 0.0150(3) 0.3554(5) 0.4093(3) 0.042(2) Uani ? C(902) 0.1093(6) -0.2113(8) 0.4293(5) 0.118(5) Uani ? C(903) 0.0828(7) -0.2794(9) 0.4609(5) 0.161(7) Uani ? H(11) -0.0469 -0.1938 0.3616 0.0370 Uiso calc H(14) -0.1690 -0.3875 0.3073 0.0460 Uiso calc H(112) 0.1778 0.0372 0.2407 0.0490 Uiso calc H(113) 0.2664 0.0188 0.2057 0.0520 Uiso calc H(114) 0.3163 0.1683 0.1808 0.0530 Uiso calc H(115) 0.2764 0.3379 0.1909 0.0570 Uiso calc H(116) 0.1874 0.3562 0.2263 0.0440 Uiso calc H(122) 0.1852 0.2479 0.3455 0.0510 Uiso calc H(123) 0.2111 0.3787 0.4079 0.0630 Uiso calc H(124) 0.1607 0.5403 0.4010 0.0630 Uiso calc H(125) 0.0825 0.5717 0.3322 0.0580 Uiso calc H(126) 0.0569 0.4421 0.2683 0.0440 Uiso calc H(12A) -0.1622 -0.1845 0.2972 0.0460 Uiso calc H(12B) -0.1441 -0.1148 0.3479 0.0460 Uiso calc H(13A) -0.1982 -0.2683 0.3667 0.0500 Uiso calc H(13B) -0.1323 -0.2683 0.4000 0.0500 Uiso calc H(15A) -0.0494 -0.3920 0.3651 0.0620 Uiso calc H(15B) -0.0717 -0.4565 0.3134 0.0620 Uiso calc H(16A) -0.0841 -0.2986 0.2647 0.0610 Uiso calc H(16B) -0.0170 -0.3020 0.2958 0.0610 Uiso calc H(19A) -0.1832 -0.5836 0.4501 0.0750 Uiso calc H(19B) -0.2450 -0.5930 0.4106 0.0750 Uiso calc H(1B1) 0.0290 0.3352 0.2064 0.0360 Uiso calc H(1B2) 0.0820 0.3078 0.1751 0.0360 Uiso calc H(20A) -0.2245 -0.4552 0.4972 0.0960 Uiso calc H(20B) -0.2683 -0.5545 0.4917 0.0960 Uiso calc H(20C) -0.2848 -0.4537 0.4560 0.0960 Uiso calc H(212) -0.1297 0.1997 0.3691 0.0480 Uiso calc H(213) -0.1819 0.1109 0.4264 0.0620 Uiso calc H(214) -0.1382 -0.0285 0.4762 0.0590 Uiso calc H(215) -0.0412 -0.0869 0.4668 0.0510 Uiso calc H(216) 0.0093 -0.0059 0.4062 0.0460 Uiso calc H(222) 0.1008 0.1448 0.4217 0.0560 Uiso calc H(223) 0.1443 0.2328 0.4969 0.0640 Uiso calc H(224) 0.1066 0.3944 0.5191 0.0660 Uiso calc H(225) 0.0280 0.4734 0.4639 0.0640 Uiso calc H(226) -0.0172 0.3876 0.3872 0.0540 Uiso calc H(901) 0.1048 -0.1809 0.3591 0.1450 Uiso calc H(90A) 0.1530 -0.2103 0.4418 0.1540 Uiso calc H(90B) 0.0941 -0.1396 0.4336 0.1540 Uiso calc H(90C) 0.0709 -0.3445 0.4423 0.2090 Uiso calc H(90D) 0.0474 -0.2458 0.4706 0.2090 Uiso calc H(90E) 0.1116 -0.2954 0.4920 0.2090 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 0.02705(14) 0.02231(13) 0.02326(14) -0.00033(11) 0.00504(9) -0.00018(11) Cl 0.0339(9) 0.0480(9) 0.0339(9) -0.0015(8) -0.0031(7) 0.0009(8) P(1) 0.0280(9) 0.0256(8) 0.0245(9) -0.0016(7) 0.0075(7) -0.0013(7) P(2) 0.0303(9) 0.0265(8) 0.0237(9) -0.0016(7) 0.0073(7) 0.0001(7) O(11) 0.027(2) 0.027(2) 0.033(3) 0.0000(18) 0.004(2) -0.0065(18) O(12) 0.029(2) 0.029(2) 0.031(2) -0.002(2) 0.0043(19) 0.0056(19) O(17) 0.083(4) 0.033(3) 0.100(5) 0.008(3) 0.061(4) 0.017(3) O(18) 0.041(3) 0.056(3) 0.059(3) -0.002(2) 0.029(3) 0.016(3) O(901) 0.178(8) 0.047(4) 0.117(7) 0.023(5) 0.046(6) 0.012(4) C(10) 0.032(4) 0.031(3) 0.029(4) 0.002(3) 0.010(3) -0.002(3) C(11) 0.028(3) 0.025(3) 0.032(4) -0.004(3) 0.004(3) 0.008(3) C(12) 0.031(4) 0.034(4) 0.044(4) 0.007(3) 0.011(3) 0.009(3) C(13) 0.038(4) 0.036(4) 0.046(4) 0.005(3) 0.019(3) 0.004(3) C(14) 0.042(4) 0.035(3) 0.030(4) -0.009(3) 0.008(3) -0.001(3) C(15) 0.060(5) 0.026(3) 0.065(5) 0.004(3) 0.038(4) 0.004(3) C(16) 0.058(5) 0.027(3) 0.067(5) -0.005(3) 0.043(4) -0.002(3) C(17) 0.039(4) 0.038(4) 0.037(4) -0.008(3) 0.015(3) 0.001(3) C(19) 0.056(5) 0.061(5) 0.062(5) -0.004(4) 0.029(4) 0.020(4) C(1B) 0.026(3) 0.023(3) 0.037(4) 0.003(3) 0.014(3) -0.003(3) C(20) 0.068(6) 0.110(7) 0.047(5) -0.021(5) 0.020(5) 0.000(5) C(111) 0.034(4) 0.029(3) 0.025(3) -0.001(3) 0.006(3) -0.002(3) C(112) 0.040(4) 0.040(4) 0.033(4) -0.003(3) 0.009(3) -0.002(3) C(113) 0.034(4) 0.049(4) 0.037(4) 0.012(3) 0.006(3) -0.001(3) C(114) 0.033(4) 0.060(5) 0.033(4) -0.001(3) 0.014(3) -0.003(3) C(115) 0.040(4) 0.049(4) 0.043(4) -0.010(4) 0.012(3) 0.000(4) C(116) 0.030(4) 0.042(4) 0.032(4) -0.001(3) 0.011(3) -0.005(3) C(121) 0.035(4) 0.029(3) 0.023(3) -0.007(3) 0.012(3) -0.003(3) C(122) 0.048(4) 0.036(4) 0.035(4) -0.010(3) 0.012(3) -0.002(3) C(123) 0.058(5) 0.057(5) 0.030(4) -0.025(4) 0.008(4) -0.004(3) C(124) 0.065(5) 0.039(4) 0.048(5) -0.018(4) 0.031(4) -0.015(4) C(125) 0.048(5) 0.034(4) 0.054(5) -0.008(3) 0.017(4) -0.012(4) C(126) 0.039(4) 0.034(3) 0.033(4) -0.002(3) 0.014(3) -0.002(3) C(211) 0.032(4) 0.036(3) 0.022(3) 0.000(3) 0.007(3) -0.001(3) C(212) 0.038(4) 0.045(4) 0.030(4) -0.003(3) 0.010(3) -0.001(3) C(213) 0.045(4) 0.061(5) 0.044(4) 0.001(4) 0.025(4) 0.001(4) C(214) 0.059(5) 0.045(4) 0.039(4) -0.010(4) 0.024(4) 0.011(4) C(215) 0.058(5) 0.033(3) 0.030(4) -0.003(3) 0.012(3) 0.007(3) C(216) 0.045(4) 0.032(3) 0.028(4) 0.002(3) 0.006(3) 0.007(3) C(221) 0.035(4) 0.030(3) 0.034(4) -0.005(3) 0.015(3) -0.003(3) C(222) 0.042(4) 0.045(4) 0.041(4) 0.000(3) 0.007(3) 0.005(4) C(223) 0.064(5) 0.051(4) 0.026(4) -0.014(4) -0.007(4) -0.001(3) C(224) 0.071(6) 0.054(5) 0.029(4) -0.024(4) 0.010(4) -0.003(4) C(225) 0.073(5) 0.039(4) 0.039(4) -0.012(4) 0.021(4) -0.012(3) C(226) 0.051(4) 0.039(4) 0.035(4) -0.007(3) 0.007(3) -0.006(3) C(902) 0.189(13) 0.069(7) 0.091(9) -0.033(8) 0.005(9) 0.002(7) C(903) 0.286(19) 0.088(8) 0.123(11) -0.004(11) 0.079(13) 0.004(8) # 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(12) 2.114(4) ? Re O(11) 2.163(4) ? Re Re 2.3120(5) ? Re P(1) 2.3814(15) ? Re P(2) 2.4104(15) ? Re Cl 2.5362(16) ? P(1) C(1B) 1.826(6) ? P(1) C(121) 1.828(6) ? P(1) C(111) 1.838(6) ? P(2) C(1B) 1.829(6) ? P(2) C(211) 1.838(6) ? P(2) C(221) 1.846(6) ? O(11) C(10) 1.262(7) ? O(12) C(10) 1.277(7) ? O(17) C(17) 1.185(7) ? O(18) C(17) 1.330(7) ? O(18) C(19) 1.467(7) ? O(901) C(902) 1.398(12) ? C(10) O(11) 1.262(7) ? C(10) C(11) 1.509(8) ? C(11) C(12) 1.509(8) ? C(11) C(16) 1.522(8) ? C(12) C(13) 1.517(8) ? C(13) C(14) 1.523(8) ? C(14) C(17) 1.518(8) ? C(14) C(15) 1.524(8) ? C(15) C(16) 1.521(8) ? C(19) C(20) 1.482(10) ? C(1B) P(2) 1.828(6) ? C(111) C(112) 1.368(8) ? C(111) C(116) 1.405(8) ? C(112) C(113) 1.387(8) ? C(113) C(114) 1.386(9) ? C(114) C(115) 1.392(9) ? C(115) C(116) 1.390(8) ? C(121) C(122) 1.393(8) ? C(121) C(126) 1.400(8) ? C(122) C(123) 1.380(9) ? C(123) C(124) 1.375(10) ? C(124) C(125) 1.372(10) ? C(125) C(126) 1.390(8) ? C(211) C(212) 1.379(8) ? C(211) C(216) 1.404(8) ? C(212) C(213) 1.391(8) ? C(213) C(214) 1.360(9) ? C(214) C(215) 1.388(9) ? C(215) C(216) 1.380(8) ? C(221) C(222) 1.375(9) ? C(221) C(226) 1.400(8) ? C(222) C(223) 1.383(9) ? C(223) C(224) 1.367(9) ? C(224) C(225) 1.360(10) ? C(225) C(226) 1.402(9) ? C(902) C(903) 1.378(14) ? 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(12) Re O(11) 80.44(15) ? O(12) Re Re 88.55(11) ? O(11) Re Re 87.70(10) ? O(12) Re P(1) 169.81(11) ? O(11) Re P(1) 95.00(11) ? Re Re P(1) 100.42(4) ? O(12) Re P(2) 90.85(11) ? O(11) Re P(2) 171.10(10) ? Re Re P(2) 93.99(4) ? P(1) Re P(2) 93.30(5) ? O(12) Re Cl 82.47(11) ? O(11) Re Cl 80.90(11) ? Re Re Cl 166.50(4) ? P(1) Re Cl 87.83(5) ? P(2) Re Cl 96.19(5) ? C(1B) P(1) C(121) 104.6(3) ? C(1B) P(1) C(111) 101.7(3) ? C(121) P(1) C(111) 99.0(3) ? C(1B) P(1) Re 109.93(19) ? C(121) P(1) Re 118.53(19) ? C(111) P(1) Re 120.80(19) ? C(1B) P(2) C(211) 105.9(3) ? C(1B) P(2) C(221) 103.7(3) ? C(211) P(2) C(221) 95.1(3) ? C(1B) P(2) Re 109.01(19) ? C(211) P(2) Re 116.84(19) ? C(221) P(2) Re 124.1(2) ? C(10) O(11) Re 117.9(4) ? C(10) O(12) Re 119.1(4) ? C(17) O(18) C(19) 115.9(5) ? O(11) C(10) O(12) 123.0(5) ? O(11) C(10) C(11) 120.0(5) ? O(12) C(10) C(11) 117.0(5) ? C(10) C(11) C(12) 114.1(5) ? C(10) C(11) C(16) 111.3(5) ? C(12) C(11) C(16) 109.6(5) ? C(11) C(12) C(13) 110.6(5) ? C(12) C(13) C(14) 111.2(5) ? C(17) C(14) C(13) 114.0(5) ? C(17) C(14) C(15) 109.6(5) ? C(13) C(14) C(15) 111.6(5) ? C(16) C(15) C(14) 111.9(5) ? C(15) C(16) C(11) 110.1(5) ? O(17) C(17) O(18) 123.2(6) ? O(17) C(17) C(14) 124.4(6) ? O(18) C(17) C(14) 112.5(6) ? O(18) C(19) C(20) 107.3(6) ? P(2) C(1B) P(1) 110.4(3) ? C(112) C(111) C(116) 119.8(6) ? C(112) C(111) P(1) 122.9(5) ? C(116) C(111) P(1) 117.1(4) ? C(111) C(112) C(113) 120.3(6) ? C(114) C(113) C(112) 120.6(6) ? C(113) C(114) C(115) 119.4(6) ? C(114) C(115) C(116) 120.0(6) ? C(115) C(116) C(111) 119.7(6) ? C(122) C(121) C(126) 117.9(6) ? C(122) C(121) P(1) 117.0(4) ? C(126) C(121) P(1) 125.1(5) ? C(123) C(122) C(121) 120.8(6) ? C(124) C(123) C(122) 120.4(7) ? C(125) C(124) C(123) 120.3(7) ? C(124) C(125) C(126) 119.6(6) ? C(125) C(126) C(121) 121.0(6) ? C(212) C(211) C(216) 118.1(6) ? C(212) C(211) P(2) 124.6(5) ? C(216) C(211) P(2) 117.0(4) ? C(211) C(212) C(213) 120.2(6) ? C(214) C(213) C(212) 121.4(6) ? C(213) C(214) C(215) 119.5(6) ? C(216) C(215) C(214) 119.7(6) ? C(215) C(216) C(211) 121.1(6) ? C(222) C(221) C(226) 118.8(6) ? C(222) C(221) P(2) 121.0(5) ? C(226) C(221) P(2) 119.7(5) ? C(221) C(222) C(223) 120.5(7) ? C(224) C(223) C(222) 121.1(7) ? C(223) C(224) C(225) 119.4(7) ? C(224) C(225) C(226) 120.9(7) ? C(225) C(226) C(221) 119.3(7) ? C(903) C(902) O(901) 116.6(10) ? #===END