Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Richard A. Walton' 'Swarup K. Chattopadhyay' 'P. Fanwick' _publ_contact_author_name 'Prof Richard A Walton' _publ_contact_author_address ; Department of Chemistry Purdue University 425 Central Drive West Lafayette Indiana 47907-2018 UNITED STATES OF AMERICA ; _publ_contact_author_email RAWALTON@PURDUE.EDU _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Reactions of the triply-bonded complex cis-Re2(u-O2CCH3)2Cl2(u-dppm)2 with pyridine carboxylic acids. The isolation and structural characterization of a third structural isomer of Re2(dipic)Cl2(u-dppm)2 (dipic = pyridine-2,6-dicarboxylate) ; _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 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_SWCH6 _database_code_CSD 212135 _audit_creation_date 23-09-02 _audit_creation_method from_MolEN_and_SHELXL _audit_update_record ; ? ; # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description needle _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.13 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C59 H51 Cl6 N1 O4 P4 Re2' _chemical_formula_moiety 'C57 H47 Cl2 N1 O4 P4 Re2,2(C1 H2 Cl2)' _chemical_formula_structural ? _chemical_formula_weight 1547.08 _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 19.4967(4) _cell_length_b 15.3146(3) _cell_length_c 19.7094(4) _cell_angle_alpha 90.00 _cell_angle_beta 93.0862(8) _cell_angle_gamma 90.00 _cell_volume 5876.4(2) _cell_measurement_reflns_used 45465 _cell_measurement_theta_min 2 _cell_measurement_theta_max 27 _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.75 _exptl_crystal_density_meas ? _diffrn_radiation_type MO-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 4.601 _cell_measurement_temperature 150 _exptl_crystal_F_000 3024 # 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 0.3383 _exptl_absorpt_correction_T_max 0.5626 _diffrn_reflns_number 45465 _diffrn_measured_fraction_theta_max 0.9980 _diffrn_reflns_theta_full 27.9 _diffrn_measured_fraction_theta_full 0.9980 _reflns_number_total 13990 _reflns_number_gt 11630 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.072 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 27.89 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_max 25 # 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 0.044 _refine_ls_wR_factor_ref 0.104 _refine_ls_hydrogen_treatment H_atoms_riding _refine_ls_number_reflns 13932 _refine_ls_number_parameters 685 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 0.982 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details '1/[\s^2^(Fo^2^)+(0.0672P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3 ' _refine_ls_shift/su_max 0.000 _refine_diff_density_max 1.79 _refine_diff_density_min -2.56 _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_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re(1) Re 0.071352(11) 0.198105(13) 0.170863(10) 0.01934(7) Uani 1 1 d . . . Re(2) Re 0.120871(11) 0.157153(13) 0.272108(10) 0.02120(7) Uani 1 1 d . . . Cl(1) Cl -0.00446(7) 0.22201(9) 0.06137(7) 0.0263(3) Uani 1 1 d . . . Cl(2) Cl 0.19565(8) 0.03751(9) 0.25804(8) 0.0347(3) Uani 1 1 d . . . Cl(91) Cl 0.24570(13) 0.19998(15) 0.86071(11) 0.0699(6) Uani 1 1 d . . . Cl(92) Cl 0.36814(14) 0.14174(19) 0.93745(12) 0.0820(8) Uani 1 1 d . . . Cl(93) Cl 0.59196(17) 0.21736(18) 0.26070(15) 0.0929(9) Uani 1 1 d . . . Cl(94) Cl 0.6109(4) 0.1952(3) 0.12312(19) 0.227(4) Uani 1 1 d . . . P(1) P 0.11991(7) 0.34595(9) 0.16476(7) 0.0214(3) Uani 1 1 d . . . P(2) P 0.21116(7) 0.26014(9) 0.27134(7) 0.0222(3) Uani 1 1 d . . . P(3) P -0.03983(7) 0.22729(9) 0.21775(7) 0.0231(3) Uani 1 1 d . . . P(4) P 0.05062(8) 0.23045(9) 0.34783(7) 0.0247(3) Uani 1 1 d . . . O(71) O 0.14124(19) 0.1701(2) 0.09911(18) 0.0222(8) Uani 1 1 d . . . O(72) O 0.1542(3) 0.0886(3) 0.0071(2) 0.0433(12) Uani 1 1 d . . . O(81) O 0.0499(2) 0.0601(2) 0.29708(19) 0.0286(9) Uani 1 1 d . . . O(82) O -0.0300(2) -0.0421(3) 0.2855(2) 0.0379(11) Uani 1 1 d . . . N(1) N 0.0571(2) 0.0587(3) 0.1511(2) 0.0198(9) Uani 1 1 d . . . C(2) C 0.0794(3) 0.0371(3) 0.0893(3) 0.0244(12) Uani 1 1 d . . . C(3) C 0.0662(3) -0.0419(4) 0.0584(3) 0.0335(14) Uani 1 1 d . . . C(4) C 0.0301(4) -0.1045(4) 0.0924(3) 0.0380(15) Uani 1 1 d . . . C(5) C 0.0129(3) -0.0868(4) 0.1584(3) 0.0329(14) Uani 1 1 d . . . C(6) C 0.0275(3) -0.0060(3) 0.1869(3) 0.0256(12) Uani 1 1 d . . . C(7) C 0.1274(3) 0.1028(3) 0.0600(3) 0.0269(12) Uani 1 1 d . . . C(8) C 0.0132(3) 0.0055(3) 0.2617(3) 0.0267(12) Uani 1 1 d . . . C(1B) C 0.1768(3) 0.3649(3) 0.2410(3) 0.0216(11) Uani 1 1 d . . . C(2B) C -0.0374(3) 0.2187(4) 0.3114(3) 0.0268(12) Uani 1 1 d . . . C(111) C 0.0722(3) 0.4493(3) 0.1553(3) 0.0214(11) Uani 1 1 d . . . C(112) C 0.0940(3) 0.5248(3) 0.1880(3) 0.0286(13) Uani 1 1 d . . . C(113) C 0.0612(4) 0.6045(4) 0.1734(4) 0.0404(16) Uani 1 1 d . . . C(114) C 0.0084(4) 0.6080(4) 0.1234(4) 0.0409(16) Uani 1 1 d . . . C(115) C -0.0127(3) 0.5321(4) 0.0897(3) 0.0374(15) Uani 1 1 d . . . C(116) C 0.0186(3) 0.4542(4) 0.1052(3) 0.0335(14) Uani 1 1 d . . . C(121) C 0.1751(3) 0.3603(3) 0.0926(3) 0.0227(11) Uani 1 1 d . . . C(122) C 0.1471(3) 0.3420(3) 0.0269(3) 0.0256(12) Uani 1 1 d . . . C(123) C 0.1843(4) 0.3596(4) -0.0291(3) 0.0364(15) Uani 1 1 d . . . C(124) C 0.2491(3) 0.3955(4) -0.0219(3) 0.0382(15) Uani 1 1 d . . . C(125) C 0.2772(3) 0.4132(4) 0.0429(3) 0.0363(15) Uani 1 1 d . . . C(126) C 0.2401(3) 0.3966(4) 0.1000(3) 0.0327(14) Uani 1 1 d . . . C(211) C 0.2483(3) 0.2820(4) 0.3564(3) 0.0264(12) Uani 1 1 d . . . C(212) C 0.2878(3) 0.2147(4) 0.3880(3) 0.0345(14) Uani 1 1 d . . . C(213) C 0.3166(4) 0.2264(5) 0.4531(3) 0.0457(17) Uani 1 1 d . . . C(214) C 0.3055(4) 0.3021(5) 0.4891(3) 0.0480(18) Uani 1 1 d . . . C(215) C 0.2672(4) 0.3692(5) 0.4574(3) 0.0474(18) Uani 1 1 d . . . C(216) C 0.2397(3) 0.3591(4) 0.3916(3) 0.0350(14) Uani 1 1 d . . . C(221) C 0.2874(3) 0.2464(3) 0.2225(3) 0.0244(11) Uani 1 1 d . . . C(222) C 0.2861(3) 0.1857(4) 0.1687(3) 0.0305(13) Uani 1 1 d . . . C(223) C 0.3413(4) 0.1813(4) 0.1274(3) 0.0377(15) Uani 1 1 d . . . C(224) C 0.3966(3) 0.2360(4) 0.1384(3) 0.0378(15) Uani 1 1 d . . . C(225) C 0.3976(3) 0.2950(4) 0.1905(3) 0.0358(14) Uani 1 1 d . . . C(226) C 0.3442(3) 0.3003(4) 0.2332(3) 0.0300(13) Uani 1 1 d . . . C(311) C -0.0893(3) 0.3285(4) 0.1999(3) 0.0296(13) Uani 1 1 d . . . C(312) C -0.0985(3) 0.3929(4) 0.2483(3) 0.0306(13) Uani 1 1 d . . . C(313) C -0.1367(4) 0.4677(4) 0.2333(3) 0.0391(15) Uani 1 1 d . . . C(314) C -0.1679(4) 0.4770(5) 0.1698(4) 0.0468(18) Uani 1 1 d . . . C(315) C -0.1622(4) 0.4123(5) 0.1210(3) 0.0492(19) Uani 1 1 d . . . C(316) C -0.1223(4) 0.3392(4) 0.1359(3) 0.0380(15) Uani 1 1 d . . . C(321) C -0.1107(3) 0.1506(4) 0.1957(3) 0.0309(13) Uani 1 1 d . . . C(322) C -0.1703(4) 0.1582(5) 0.2318(4) 0.0486(19) Uani 1 1 d . . . C(323) C -0.2249(4) 0.1051(5) 0.2185(4) 0.060(2) Uani 1 1 d . . . C(324) C -0.2226(4) 0.0410(5) 0.1679(4) 0.054(2) Uani 1 1 d . . . C(325) C -0.1652(3) 0.0330(4) 0.1313(3) 0.0385(15) Uani 1 1 d . . . C(326) C -0.1087(3) 0.0892(4) 0.1443(3) 0.0299(13) Uani 1 1 d . . . C(411) C 0.0566(3) 0.3423(4) 0.3786(3) 0.0270(12) Uani 1 1 d . . . C(412) C 0.0438(3) 0.4115(4) 0.3343(3) 0.0294(13) Uani 1 1 d . . . C(413) C 0.0430(3) 0.4976(4) 0.3575(3) 0.0366(15) Uani 1 1 d . . . C(414) C 0.0561(4) 0.5145(4) 0.4246(4) 0.0434(17) Uani 1 1 d . . . C(415) C 0.0720(4) 0.4473(4) 0.4701(3) 0.0388(15) Uani 1 1 d . . . C(416) C 0.0722(4) 0.3618(4) 0.4466(3) 0.0366(15) Uani 1 1 d . . . C(421) C 0.0538(3) 0.1681(4) 0.4274(3) 0.0295(13) Uani 1 1 d . . . C(422) C 0.1172(4) 0.1409(4) 0.4548(3) 0.0418(16) Uani 1 1 d . . . C(423) C 0.1219(5) 0.0967(5) 0.5168(3) 0.055(2) Uani 1 1 d . . . C(424) C 0.0649(5) 0.0819(5) 0.5520(3) 0.053(2) Uani 1 1 d . . . C(425) C 0.0025(5) 0.1099(5) 0.5262(3) 0.051(2) Uani 1 1 d . . . C(426) C -0.0042(4) 0.1534(4) 0.4636(3) 0.0412(16) Uani 1 1 d . . . C(910) C 0.2819(4) 0.1729(6) 0.9413(4) 0.057(2) Uani 1 1 d . . . C(920) C 0.6153(7) 0.2700(8) 0.1907(5) 0.107(4) Uani 1 1 d . . . H(3) H 0.0816 -0.0534 0.0144 0.040 Uiso 1 1 calc R . . H(4) H 0.0174 -0.1582 0.0711 0.046 Uiso 1 1 calc R . . H(5) H -0.0089 -0.1303 0.1840 0.039 Uiso 1 1 calc R . . H(112) H 0.1316 0.5227 0.2207 0.034 Uiso 1 1 calc R . . H(113) H 0.0750 0.6558 0.1975 0.049 Uiso 1 1 calc R . . H(114) H -0.0133 0.6621 0.1122 0.049 Uiso 1 1 calc R . . H(115) H -0.0491 0.5343 0.0557 0.045 Uiso 1 1 calc R . . H(116) H 0.0038 0.4028 0.0818 0.040 Uiso 1 1 calc R . . H(122) H 0.1024 0.3175 0.0210 0.031 Uiso 1 1 calc R . . H(123) H 0.1650 0.3468 -0.0733 0.044 Uiso 1 1 calc R . . H(124) H 0.2742 0.4081 -0.0608 0.046 Uiso 1 1 calc R . . H(125) H 0.3223 0.4367 0.0484 0.044 Uiso 1 1 calc R . . H(126) H 0.2594 0.4102 0.1440 0.039 Uiso 1 1 calc R . . H(1B1) H 0.2149 0.4042 0.2298 0.026 Uiso 1 1 calc R . . H(1B2) H 0.1507 0.3930 0.2768 0.026 Uiso 1 1 calc R . . H(212) H 0.2947 0.1614 0.3647 0.041 Uiso 1 1 calc R . . H(213) H 0.3444 0.1815 0.4734 0.055 Uiso 1 1 calc R . . H(214) H 0.3237 0.3084 0.5345 0.058 Uiso 1 1 calc R . . H(215) H 0.2599 0.4221 0.4812 0.057 Uiso 1 1 calc R . . H(216) H 0.2147 0.4057 0.3703 0.042 Uiso 1 1 calc R . . H(222) H 0.2477 0.1482 0.1608 0.037 Uiso 1 1 calc R . . H(223) H 0.3410 0.1402 0.0913 0.045 Uiso 1 1 calc R . . H(224) H 0.4342 0.2328 0.1097 0.045 Uiso 1 1 calc R . . H(225) H 0.4358 0.3331 0.1973 0.043 Uiso 1 1 calc R . . H(226) H 0.3462 0.3406 0.2698 0.036 Uiso 1 1 calc R . . H(2B1) H -0.0668 0.2648 0.3299 0.032 Uiso 1 1 calc R . . H(2B2) H -0.0560 0.1613 0.3245 0.032 Uiso 1 1 calc R . . H(312) H -0.0781 0.3856 0.2928 0.037 Uiso 1 1 calc R . . H(313) H -0.1411 0.5118 0.2666 0.047 Uiso 1 1 calc R . . H(314) H -0.1937 0.5283 0.1590 0.056 Uiso 1 1 calc R . . H(315) H -0.1857 0.4181 0.0777 0.059 Uiso 1 1 calc R . . H(316) H -0.1172 0.2959 0.1020 0.046 Uiso 1 1 calc R . . H(322) H -0.1725 0.2014 0.2663 0.058 Uiso 1 1 calc R . . H(323) H -0.2649 0.1113 0.2435 0.072 Uiso 1 1 calc R . . H(324) H -0.2608 0.0033 0.1590 0.065 Uiso 1 1 calc R . . H(325) H -0.1634 -0.0105 0.0971 0.046 Uiso 1 1 calc R . . H(326) H -0.0694 0.0849 0.1180 0.036 Uiso 1 1 calc R . . H(412) H 0.0353 0.4001 0.2872 0.035 Uiso 1 1 calc R . . H(413) H 0.0334 0.5441 0.3265 0.044 Uiso 1 1 calc R . . H(414) H 0.0544 0.5729 0.4405 0.052 Uiso 1 1 calc R . . H(415) H 0.0826 0.4596 0.5167 0.047 Uiso 1 1 calc R . . H(416) H 0.0832 0.3158 0.4775 0.044 Uiso 1 1 calc R . . H(422) H 0.1575 0.1524 0.4314 0.050 Uiso 1 1 calc R . . H(423) H 0.1654 0.0767 0.5346 0.066 Uiso 1 1 calc R . . H(424) H 0.0686 0.0522 0.5943 0.063 Uiso 1 1 calc R . . H(425) H -0.0371 0.0997 0.5511 0.062 Uiso 1 1 calc R . . H(426) H -0.0480 0.1727 0.4462 0.049 Uiso 1 1 calc R . . H(91A) H 0.2555 0.1244 0.9604 0.068 Uiso 1 1 calc R . . H(91B) H 0.2788 0.2239 0.9719 0.068 Uiso 1 1 calc R . . H(92A) H 0.6627 0.2928 0.1977 0.129 Uiso 1 1 calc R . . H(92B) H 0.5841 0.3198 0.1805 0.129 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Re(1) 0.02351(12) 0.01599(11) 0.01860(11) -0.00018(8) 0.00182(8) -0.00076(8) Re(2) 0.02795(13) 0.01638(11) 0.01925(11) 0.00111(8) 0.00111(8) -0.00002(8) Cl(1) 0.0295(7) 0.0256(6) 0.0236(6) -0.0010(5) -0.0015(5) -0.0007(5) Cl(2) 0.0386(9) 0.0202(6) 0.0451(8) 0.0104(6) 0.0010(7) 0.0007(6) Cl(91) 0.0831(17) 0.0745(15) 0.0521(12) 0.0106(12) 0.0033(11) 0.0020(11) Cl(92) 0.0778(17) 0.111(2) 0.0595(13) 0.0272(14) 0.0245(12) 0.0301(13) Cl(93) 0.105(2) 0.0745(16) 0.102(2) 0.0303(16) 0.0260(17) 0.0194(15) Cl(94) 0.439(10) 0.167(4) 0.072(2) 0.159(5) -0.031(4) -0.015(2) P(1) 0.0247(7) 0.0180(6) 0.0215(7) -0.0001(5) 0.0004(6) 0.0016(5) P(2) 0.0249(7) 0.0191(6) 0.0223(7) 0.0014(5) 0.0000(6) -0.0003(6) P(3) 0.0254(8) 0.0203(7) 0.0239(7) -0.0011(6) 0.0027(6) -0.0028(6) P(4) 0.0319(8) 0.0204(7) 0.0221(7) -0.0001(6) 0.0042(6) -0.0011(6) O(71) 0.026(2) 0.0205(18) 0.0202(18) -0.0020(15) 0.0044(15) -0.0033(15) O(72) 0.061(3) 0.037(2) 0.034(2) -0.016(2) 0.026(2) -0.013(2) O(81) 0.038(2) 0.0225(19) 0.026(2) -0.0077(17) 0.0075(17) 0.0000(17) O(82) 0.051(3) 0.032(2) 0.032(2) -0.014(2) 0.015(2) 0.0002(19) N(1) 0.028(2) 0.0116(19) 0.020(2) 0.0000(17) 0.0026(18) -0.0029(18) C(2) 0.027(3) 0.019(3) 0.028(3) 0.000(2) 0.004(2) 0.000(2) C(3) 0.047(4) 0.027(3) 0.027(3) -0.002(3) 0.005(3) -0.005(3) C(4) 0.055(4) 0.022(3) 0.037(3) -0.009(3) 0.003(3) -0.004(3) C(5) 0.046(4) 0.019(3) 0.034(3) -0.007(3) 0.006(3) -0.002(2) C(6) 0.033(3) 0.021(3) 0.023(3) 0.002(2) 0.002(2) -0.002(2) C(7) 0.035(3) 0.020(3) 0.026(3) 0.002(2) 0.005(2) 0.001(2) C(8) 0.039(3) 0.018(3) 0.023(3) -0.001(2) 0.005(2) 0.000(2) C(1B) 0.024(3) 0.021(2) 0.021(3) 0.003(2) 0.004(2) -0.002(2) C(2B) 0.028(3) 0.026(3) 0.027(3) -0.002(2) 0.007(2) -0.001(2) C(111) 0.028(3) 0.012(2) 0.025(3) 0.000(2) 0.002(2) 0.003(2) C(112) 0.033(3) 0.015(3) 0.038(3) -0.001(2) 0.003(3) -0.002(2) C(113) 0.047(4) 0.020(3) 0.054(4) 0.002(3) 0.002(3) -0.003(3) C(114) 0.045(4) 0.024(3) 0.055(4) 0.007(3) 0.006(3) -0.001(3) C(115) 0.034(4) 0.033(3) 0.044(4) 0.006(3) -0.006(3) 0.004(3) C(116) 0.033(3) 0.028(3) 0.040(3) 0.005(3) -0.001(3) -0.002(3) C(121) 0.027(3) 0.020(3) 0.021(3) 0.003(2) 0.003(2) 0.001(2) C(122) 0.030(3) 0.022(3) 0.025(3) 0.001(2) -0.001(2) 0.003(2) C(123) 0.045(4) 0.038(3) 0.026(3) 0.000(3) 0.002(3) 0.004(3) C(124) 0.037(4) 0.048(4) 0.031(3) -0.002(3) 0.010(3) 0.010(3) C(125) 0.029(3) 0.044(4) 0.037(3) -0.004(3) 0.008(3) 0.007(3) C(126) 0.034(4) 0.034(3) 0.030(3) -0.007(3) 0.001(3) 0.004(3) C(211) 0.032(3) 0.028(3) 0.019(3) -0.001(2) 0.002(2) 0.002(2) C(212) 0.045(4) 0.030(3) 0.027(3) 0.007(3) -0.005(3) 0.001(3) C(213) 0.056(5) 0.047(4) 0.032(3) 0.015(4) -0.010(3) 0.002(3) C(214) 0.055(5) 0.059(5) 0.029(3) 0.006(4) -0.012(3) -0.006(3) C(215) 0.061(5) 0.041(4) 0.040(4) 0.007(3) -0.008(3) -0.015(3) C(216) 0.044(4) 0.031(3) 0.030(3) 0.005(3) -0.002(3) -0.002(3) C(221) 0.028(3) 0.021(3) 0.025(3) -0.001(2) 0.000(2) 0.004(2) C(222) 0.030(3) 0.029(3) 0.032(3) 0.004(2) -0.003(3) -0.005(3) C(223) 0.043(4) 0.035(3) 0.035(3) 0.007(3) 0.006(3) -0.007(3) C(224) 0.035(4) 0.036(3) 0.043(4) 0.005(3) 0.007(3) 0.000(3) C(225) 0.034(4) 0.030(3) 0.044(4) -0.003(3) 0.006(3) 0.006(3) C(226) 0.035(3) 0.019(3) 0.037(3) 0.000(2) 0.005(3) 0.000(2) C(311) 0.031(3) 0.029(3) 0.029(3) 0.006(2) 0.004(3) -0.003(3) C(312) 0.032(3) 0.030(3) 0.029(3) 0.002(3) 0.001(2) -0.002(3) C(313) 0.045(4) 0.033(3) 0.040(4) 0.005(3) 0.007(3) -0.003(3) C(314) 0.050(4) 0.041(4) 0.049(4) 0.021(3) 0.004(3) 0.002(3) C(315) 0.058(5) 0.060(5) 0.028(3) 0.025(4) -0.001(3) -0.001(3) C(316) 0.044(4) 0.043(4) 0.027(3) 0.012(3) 0.001(3) -0.008(3) C(321) 0.036(4) 0.026(3) 0.031(3) -0.005(3) 0.008(3) -0.004(2) C(322) 0.047(4) 0.046(4) 0.055(4) -0.011(3) 0.016(4) -0.021(4) C(323) 0.048(5) 0.061(5) 0.073(5) -0.023(4) 0.032(4) -0.029(4) C(324) 0.049(5) 0.054(5) 0.060(5) -0.023(4) 0.016(4) -0.022(4) C(325) 0.041(4) 0.036(3) 0.039(3) -0.012(3) 0.011(3) -0.012(3) C(326) 0.030(3) 0.030(3) 0.030(3) -0.002(2) 0.005(3) -0.002(3) C(411) 0.027(3) 0.023(3) 0.032(3) 0.000(2) 0.010(2) -0.004(2) C(412) 0.028(3) 0.029(3) 0.031(3) -0.002(2) 0.004(2) 0.001(3) C(413) 0.042(4) 0.022(3) 0.047(4) -0.002(3) 0.014(3) 0.001(3) C(414) 0.055(4) 0.026(3) 0.052(4) -0.009(3) 0.023(4) -0.010(3) C(415) 0.048(4) 0.032(3) 0.038(3) -0.009(3) 0.009(3) -0.012(3) C(416) 0.046(4) 0.027(3) 0.037(3) -0.005(3) 0.007(3) -0.007(3) C(421) 0.041(4) 0.026(3) 0.022(3) 0.005(3) 0.002(3) -0.005(2) C(422) 0.054(4) 0.042(4) 0.030(3) 0.014(3) 0.007(3) 0.006(3) C(423) 0.086(6) 0.053(5) 0.025(3) 0.022(4) -0.003(4) 0.002(3) C(424) 0.101(7) 0.035(4) 0.023(3) -0.006(4) 0.009(4) 0.004(3) C(425) 0.080(6) 0.044(4) 0.032(4) -0.020(4) 0.020(4) -0.004(3) C(426) 0.052(4) 0.040(4) 0.033(3) -0.006(3) 0.011(3) 0.001(3) C(910) 0.049(5) 0.074(5) 0.049(4) -0.001(4) 0.019(4) 0.010(4) C(920) 0.151(12) 0.110(9) 0.062(6) 0.054(9) 0.011(7) 0.007(6) # 10. MOLECULAR GEOMETRY _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Re(1) O(71) 2.061(4) YES Re(1) N(1) 2.185(4) YES Re(1) Re(2) 2.2583(3) YES Re(1) P(3) 2.4430(14) YES Re(1) P(1) 2.4596(13) YES Re(1) Cl(1) 2.5753(13) YES Re(2) O(81) 2.107(4) YES Re(2) P(4) 2.3630(14) YES Re(2) P(2) 2.3642(14) YES Re(2) Cl(2) 2.3672(14) YES Cl(91) C(910) 1.752(8) YES Cl(92) C(910) 1.753(8) YES Cl(93) C(920) 1.683(11) YES Cl(94) C(920) 1.755(12) YES P(1) C(111) 1.840(5) YES P(1) C(1B) 1.841(6) YES P(1) C(121) 1.843(5) YES P(2) C(211) 1.821(6) YES P(2) C(221) 1.826(6) YES P(2) C(1B) 1.827(5) YES P(3) C(321) 1.848(6) YES P(3) C(311) 1.849(6) YES P(3) C(2B) 1.849(6) YES P(4) C(411) 1.819(6) YES P(4) C(2B) 1.833(6) YES P(4) C(421) 1.835(6) YES O(71) C(7) 1.307(6) YES O(72) C(7) 1.211(6) YES O(81) C(8) 1.281(7) YES O(82) C(8) 1.228(7) YES N(1) C(2) 1.355(6) YES N(1) C(6) 1.363(7) YES C(2) C(3) 1.372(8) YES C(2) C(7) 1.510(7) YES C(3) C(4) 1.384(8) YES C(4) C(5) 1.387(8) YES C(5) C(6) 1.383(8) YES C(6) C(8) 1.525(7) YES C(111) C(112) 1.380(7) YES C(111) C(116) 1.400(8) YES C(112) C(113) 1.400(8) YES C(113) C(114) 1.387(10) YES C(114) C(115) 1.390(9) YES C(115) C(116) 1.367(8) YES C(121) C(126) 1.384(8) YES C(121) C(122) 1.406(8) YES C(122) C(123) 1.379(8) YES C(123) C(124) 1.378(9) YES C(124) C(125) 1.390(9) YES C(125) C(126) 1.392(8) YES C(211) C(216) 1.385(8) YES C(211) C(212) 1.411(8) YES C(212) C(213) 1.383(9) YES C(213) C(214) 1.382(10) YES C(214) C(215) 1.398(10) YES C(215) C(216) 1.385(9) YES C(221) C(226) 1.389(8) YES C(221) C(222) 1.408(8) YES C(222) C(223) 1.387(8) YES C(223) C(224) 1.372(9) YES C(224) C(225) 1.367(9) YES C(225) C(226) 1.375(8) YES C(311) C(312) 1.390(8) YES C(311) C(316) 1.395(9) YES C(312) C(313) 1.389(9) YES C(313) C(314) 1.369(10) YES C(314) C(315) 1.389(10) YES C(315) C(316) 1.386(9) YES C(321) C(326) 1.383(8) YES C(321) C(322) 1.400(9) YES C(322) C(323) 1.354(10) YES C(323) C(324) 1.402(10) YES C(324) C(325) 1.369(9) YES C(325) C(326) 1.411(8) YES C(411) C(412) 1.388(8) YES C(411) C(416) 1.390(8) YES C(412) C(413) 1.395(8) YES C(413) C(414) 1.358(9) YES C(414) C(415) 1.390(9) YES C(415) C(416) 1.389(8) YES C(421) C(422) 1.386(9) YES C(421) C(426) 1.387(9) YES C(422) C(423) 1.396(9) YES C(423) C(424) 1.359(11) YES C(424) C(425) 1.362(12) YES C(425) C(426) 1.402(10) YES 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(71) Re(1) N(1) 75.91(15) YES O(71) Re(1) Re(2) 106.35(11) YES N(1) Re(1) Re(2) 86.02(11) YES O(71) Re(1) P(3) 158.51(11) YES N(1) Re(1) P(3) 98.03(12) YES Re(2) Re(1) P(3) 93.58(3) YES O(71) Re(1) P(1) 83.53(10) YES N(1) Re(1) P(1) 159.40(12) YES Re(2) Re(1) P(1) 98.71(3) YES P(3) Re(1) P(1) 101.64(5) YES O(71) Re(1) Cl(1) 79.94(11) YES N(1) Re(1) Cl(1) 85.85(12) YES Re(2) Re(1) Cl(1) 168.15(3) YES P(3) Re(1) Cl(1) 79.05(5) YES P(1) Re(1) Cl(1) 91.90(4) YES O(81) Re(2) Re(1) 98.46(11) YES O(81) Re(2) P(4) 77.11(11) YES Re(1) Re(2) P(4) 101.03(4) YES O(81) Re(2) P(2) 166.10(11) YES Re(1) Re(2) P(2) 95.28(3) YES P(4) Re(2) P(2) 98.30(5) YES O(81) Re(2) Cl(2) 84.15(12) YES Re(1) Re(2) Cl(2) 110.37(4) YES P(4) Re(2) Cl(2) 145.42(5) YES P(2) Re(2) Cl(2) 92.99(5) YES C(111) P(1) C(1B) 103.1(2) YES C(111) P(1) C(121) 97.7(2) YES C(1B) P(1) C(121) 105.0(3) YES C(111) P(1) Re(1) 127.04(18) YES C(1B) P(1) Re(1) 108.76(17) YES C(121) P(1) Re(1) 112.93(18) YES C(211) P(2) C(221) 102.2(3) YES C(211) P(2) C(1B) 105.1(3) YES C(221) P(2) C(1B) 102.9(2) YES C(211) P(2) Re(2) 112.10(19) YES C(221) P(2) Re(2) 123.61(18) YES C(1B) P(2) Re(2) 109.14(19) YES C(321) P(3) C(311) 96.4(3) YES C(321) P(3) C(2B) 99.7(3) YES C(311) P(3) C(2B) 103.5(3) YES C(321) P(3) Re(1) 117.52(19) YES C(311) P(3) Re(1) 123.1(2) YES C(2B) P(3) Re(1) 112.93(19) YES C(411) P(4) C(2B) 105.3(3) YES C(411) P(4) C(421) 101.9(3) YES C(2B) P(4) C(421) 105.7(3) YES C(411) P(4) Re(2) 129.00(19) YES C(2B) P(4) Re(2) 105.59(18) YES C(421) P(4) Re(2) 107.39(19) YES C(7) O(71) Re(1) 116.4(3) YES C(8) O(81) Re(2) 133.4(3) YES C(2) N(1) C(6) 116.9(4) YES C(2) N(1) Re(1) 110.8(3) YES C(6) N(1) Re(1) 132.1(3) YES N(1) C(2) C(3) 123.5(5) YES N(1) C(2) C(7) 114.6(5) YES C(3) C(2) C(7) 121.5(5) YES C(2) C(3) C(4) 119.0(5) YES C(3) C(4) C(5) 118.2(5) YES C(6) C(5) C(4) 120.1(5) YES N(1) C(6) C(5) 121.6(5) YES N(1) C(6) C(8) 121.4(5) YES C(5) C(6) C(8) 116.9(5) YES O(72) C(7) O(71) 124.4(5) YES O(72) C(7) C(2) 121.0(5) YES O(71) C(7) C(2) 114.3(5) YES O(82) C(8) O(81) 123.6(5) YES O(82) C(8) C(6) 117.8(5) YES O(81) C(8) C(6) 118.4(5) YES P(2) C(1B) P(1) 108.8(3) YES P(4) C(2B) P(3) 110.9(3) YES C(112) C(111) C(116) 118.9(5) YES C(112) C(111) P(1) 122.1(4) YES C(116) C(111) P(1) 118.2(4) YES C(111) C(112) C(113) 120.6(6) YES C(114) C(113) C(112) 119.6(6) YES C(113) C(114) C(115) 119.7(6) YES C(116) C(115) C(114) 120.4(6) YES C(115) C(116) C(111) 120.8(6) YES C(126) C(121) C(122) 119.0(5) YES C(126) C(121) P(1) 122.5(4) YES C(122) C(121) P(1) 118.2(4) YES C(123) C(122) C(121) 120.2(6) YES C(124) C(123) C(122) 121.0(6) YES C(123) C(124) C(125) 119.1(6) YES C(124) C(125) C(126) 120.7(6) YES C(121) C(126) C(125) 120.1(6) YES C(216) C(211) C(212) 118.6(5) YES C(216) C(211) P(2) 124.4(5) YES C(212) C(211) P(2) 117.0(4) YES C(213) C(212) C(211) 120.0(6) YES C(214) C(213) C(212) 121.1(6) YES C(213) C(214) C(215) 118.9(6) YES C(216) C(215) C(214) 120.4(6) YES C(211) C(216) C(215) 120.9(6) YES C(226) C(221) C(222) 119.2(5) YES C(226) C(221) P(2) 121.1(4) YES C(222) C(221) P(2) 119.4(4) YES C(223) C(222) C(221) 119.4(6) YES C(224) C(223) C(222) 120.4(6) YES C(225) C(224) C(223) 120.0(6) YES C(224) C(225) C(226) 121.2(6) YES C(225) C(226) C(221) 119.7(6) YES C(312) C(311) C(316) 117.8(6) YES C(312) C(311) P(3) 123.4(5) YES C(316) C(311) P(3) 118.7(5) YES C(313) C(312) C(311) 121.8(6) YES C(314) C(313) C(312) 119.1(6) YES C(313) C(314) C(315) 120.7(6) YES C(316) C(315) C(314) 119.6(6) YES C(315) C(316) C(311) 120.8(6) YES C(326) C(321) C(322) 119.1(6) YES C(326) C(321) P(3) 123.6(5) YES C(322) C(321) P(3) 117.2(5) YES C(323) C(322) C(321) 121.1(6) YES C(322) C(323) C(324) 120.3(7) YES C(325) C(324) C(323) 119.7(7) YES C(324) C(325) C(326) 120.2(6) YES C(321) C(326) C(325) 119.6(6) YES C(412) C(411) C(416) 117.7(5) YES C(412) C(411) P(4) 120.2(5) YES C(416) C(411) P(4) 122.1(5) YES C(411) C(412) C(413) 121.4(6) YES C(414) C(413) C(412) 119.6(6) YES C(413) C(414) C(415) 120.8(6) YES C(416) C(415) C(414) 119.1(6) YES C(415) C(416) C(411) 121.3(6) YES C(422) C(421) C(426) 119.0(6) YES C(422) C(421) P(4) 118.6(5) YES C(426) C(421) P(4) 122.2(5) YES C(421) C(422) C(423) 120.2(7) YES C(424) C(423) C(422) 120.6(8) YES C(423) C(424) C(425) 119.8(7) YES C(424) C(425) C(426) 121.1(7) YES C(421) C(426) C(425) 119.3(7) YES Cl(91) C(910) Cl(92) 111.5(4) YES Cl(93) C(920) Cl(94) 107.8(7) YES #===END #============================================================================== data_SWCH12 _database_code_CSD 212136 _audit_creation_date 25-02-03 _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 0.25 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.10 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C62 H52 Cl2 N2 O6 P4 Re2' _chemical_formula_moiety Re2(HnicO)2Cl2(dppm)2 _chemical_formula_structural ? _chemical_formula_weight 1488.32 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y+1/2, z+1/2' _cell_length_a 13.0405(3) _cell_length_b 22.9844(5) _cell_length_c 19.7779(3) _cell_angle_alpha 90.00 _cell_angle_beta 107.5243(15) _cell_angle_gamma 90.00 _cell_volume 5652.9(2) _cell_measurement_reflns_used 43144 _cell_measurement_theta_min 2 _cell_measurement_theta_max 27 _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.75 _exptl_crystal_density_meas ? _diffrn_radiation_type MO-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 4.597 _cell_measurement_temperature 150 _exptl_crystal_F_000 2920 # 6. DATA COLLECTION _diffrn_ambient_temperature 150 _diffrn_measurement_device_type Nonius_KappaCCD _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan_(Otwinowski_&_Minor,_ _exptl_absorpt_correction_T_min 0.3986 _exptl_absorpt_correction_T_max 0.6315 _diffrn_reflns_number 43144 _diffrn_measured_fraction_theta_max 0.8367 _reflns_number_total 13025 _reflns_number_gt 9326 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.090 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 27.88 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_max 22 _diffrn_special_details 'mosaicity from Denzo/Scalepack is 0.47' # 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 0.045 _refine_ls_wR_factor_ref 0.117 _refine_ls_hydrogen_treatment H_atoms_riding _refine_ls_number_reflns 9829 _refine_ls_number_parameters 703 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details '1/[\s^2^(Fo^2^)+(0.1219P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3 ' _refine_ls_shift/su_max 0.002 _refine_diff_density_max 1.82 _refine_diff_density_min -3.19 _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_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re(1) Re 0.29564(4) 0.156284(19) 0.19589(2) 0.02309(16) Uani 1 1 d . . . Re(2) Re 0.18598(4) 0.081608(19) 0.20989(2) 0.02452(16) Uani 1 1 d . . . Cl(1) Cl 0.3963(3) 0.24023(14) 0.15877(15) 0.0361(7) Uani 1 1 d . . . Cl(2) Cl 0.0634(3) -0.00483(14) 0.20698(17) 0.0390(8) Uani 1 1 d . . . P(1) P 0.4557(2) 0.11602(13) 0.27835(15) 0.0244(7) Uani 1 1 d . . . P(2) P 0.2924(2) 0.04479(13) 0.32334(14) 0.0240(7) Uani 1 1 d . . . P(3) P 0.2644(2) 0.22460(12) 0.28012(14) 0.0220(6) Uani 1 1 d . . . P(4) P 0.0792(2) 0.14358(13) 0.26117(16) 0.0257(7) Uani 1 1 d . . . O(12) O 0.2654(8) 0.0241(3) 0.1534(4) 0.035(2) Uani 1 1 d . . . O(22) O 0.1654(7) 0.1892(3) 0.1092(4) 0.033(2) Uani 1 1 d . . . O(171) O 0.2893(12) -0.0755(4) 0.1046(5) 0.074(4) Uani 1 1 d . . . O(172) O 0.3254(16) -0.0804(5) 0.0028(7) 0.109(6) Uani 1 1 d . . . O(271) O 0.1493(8) 0.2507(4) -0.0029(5) 0.051(3) Uani 1 1 d . . . O(272) O 0.0260(9) 0.2234(5) -0.1014(5) 0.065(3) Uani 1 1 d . . . N(11) N 0.3211(9) 0.1052(4) 0.1064(5) 0.033(2) Uani 1 1 d . . . N(21) N 0.0847(9) 0.0995(4) 0.1001(5) 0.036(3) Uani 1 1 d . . . C(12) C 0.3024(12) 0.0472(6) 0.1057(6) 0.039(3) Uani 1 1 d . . . C(13) C 0.3188(16) 0.0154(6) 0.0509(8) 0.061(5) Uani 1 1 d . . . C(14) C 0.350(2) 0.0426(8) -0.0016(10) 0.107(9) Uani 1 1 d . . . C(15) C 0.369(2) 0.0979(7) -0.0002(10) 0.094(8) Uani 1 1 d . . . C(16) C 0.3485(16) 0.1282(7) 0.0529(7) 0.063(5) Uani 1 1 d . . . C(17) C 0.3091(17) -0.0490(7) 0.0508(9) 0.072(6) Uani 1 1 d . . . C(1B) C 0.4195(10) 0.0876(5) 0.3531(6) 0.025(3) Uani 1 1 d . . . C(22) C 0.1004(11) 0.1510(5) 0.0705(6) 0.035(3) Uani 1 1 d . . . C(23) C 0.0467(12) 0.1615(6) -0.0021(6) 0.045(4) Uani 1 1 d . . . C(24) C -0.0286(14) 0.1225(7) -0.0421(9) 0.068(5) Uani 1 1 d . . . C(25) C -0.0435(18) 0.0729(9) -0.0106(10) 0.094(7) Uani 1 1 d . . . C(26) C 0.0124(17) 0.0624(8) 0.0607(8) 0.083(7) Uani 1 1 d . . . C(27) C 0.0707(13) 0.2142(7) -0.0392(7) 0.051(4) Uani 1 1 d . . . C(2B) C 0.1695(9) 0.1943(5) 0.3209(6) 0.025(3) Uani 1 1 d . . . C(111) C 0.5195(11) 0.0589(6) 0.2445(7) 0.038(3) Uani 1 1 d . . . C(112) C 0.552(2) 0.0715(9) 0.1852(10) 0.104(9) Uani 1 1 d . . . C(113) C 0.601(2) 0.0280(12) 0.1559(10) 0.128(12) Uani 1 1 d . . . C(114) C 0.6227(19) -0.0257(9) 0.1832(9) 0.089(7) Uani 1 1 d . . . C(115) C 0.5967(12) -0.0405(7) 0.2424(9) 0.057(4) Uani 1 1 d . . . C(116) C 0.5464(11) 0.0048(6) 0.2729(8) 0.045(3) Uani 1 1 d . . . C(121) C 0.5712(10) 0.1594(5) 0.3208(7) 0.033(3) Uani 1 1 d . . . C(122) C 0.6153(11) 0.1629(6) 0.3933(8) 0.045(4) Uani 1 1 d . . . C(123) C 0.7124(13) 0.1971(8) 0.4246(10) 0.064(5) Uani 1 1 d . . . C(124) C 0.7617(14) 0.2241(7) 0.3848(11) 0.069(5) Uani 1 1 d . . . C(125) C 0.7227(13) 0.2225(7) 0.3112(13) 0.082(7) Uani 1 1 d . . . C(126) C 0.6244(12) 0.1883(7) 0.2768(9) 0.060(5) Uani 1 1 d . . . C(211) C 0.3353(10) -0.0322(5) 0.3304(6) 0.031(3) Uani 1 1 d . . . C(212) C 0.3041(12) -0.0693(6) 0.2717(7) 0.041(3) Uani 1 1 d . . . C(213) C 0.3437(12) -0.1272(6) 0.2787(9) 0.050(4) Uani 1 1 d . . . C(214) C 0.4112(12) -0.1454(6) 0.3428(9) 0.055(4) Uani 1 1 d . . . C(215) C 0.4380(11) -0.1095(6) 0.4008(8) 0.048(4) Uani 1 1 d . . . C(216) C 0.4002(11) -0.0554(6) 0.3955(7) 0.046(4) Uani 1 1 d . . . C(221) C 0.2426(9) 0.0455(5) 0.4009(6) 0.027(3) Uani 1 1 d . . . C(222) C 0.1606(11) 0.0082(5) 0.4007(6) 0.034(3) Uani 1 1 d . . . C(223) C 0.1247(12) 0.0035(6) 0.4597(7) 0.043(3) Uani 1 1 d . . . C(224) C 0.1694(12) 0.0375(6) 0.5191(7) 0.044(4) Uani 1 1 d . . . C(225) C 0.2487(12) 0.0763(6) 0.5187(7) 0.046(4) Uani 1 1 d . . . C(226) C 0.2872(11) 0.0818(6) 0.4583(6) 0.037(3) Uani 1 1 d . . . C(311) C 0.2039(9) 0.2942(5) 0.2500(6) 0.028(3) Uani 1 1 d . . . C(312) C 0.1833(10) 0.3332(5) 0.2994(6) 0.034(3) Uani 1 1 d . . . C(313) C 0.1288(11) 0.3859(5) 0.2784(7) 0.038(3) Uani 1 1 d . . . C(314) C 0.0966(11) 0.4018(6) 0.2081(8) 0.045(4) Uani 1 1 d . . . C(315) C 0.1164(12) 0.3646(7) 0.1583(8) 0.052(4) Uani 1 1 d . . . C(316) C 0.1718(12) 0.3106(6) 0.1797(7) 0.042(3) Uani 1 1 d . . . C(321) C 0.3732(9) 0.2496(5) 0.3562(6) 0.026(3) Uani 1 1 d . . . C(322) C 0.3825(10) 0.2358(6) 0.4278(6) 0.036(3) Uani 1 1 d . . . C(323) C 0.4660(12) 0.2575(7) 0.4807(7) 0.051(4) Uani 1 1 d . . . C(324) C 0.5407(11) 0.2964(7) 0.4668(7) 0.049(4) Uani 1 1 d . . . C(325) C 0.5340(11) 0.3112(6) 0.3980(7) 0.043(3) Uani 1 1 d . . . C(326) C 0.4501(10) 0.2873(5) 0.3419(7) 0.033(3) Uani 1 1 d . . . C(411) C -0.0218(10) 0.1897(6) 0.2041(6) 0.033(3) Uani 1 1 d . . . C(412) C -0.0434(9) 0.2452(5) 0.2211(6) 0.028(3) Uani 1 1 d . . . C(413) C -0.1290(11) 0.2787(6) 0.1798(7) 0.043(3) Uani 1 1 d . . . C(414) C -0.1978(14) 0.2526(10) 0.1192(9) 0.082(7) Uani 1 1 d . . . C(415) C -0.1838(14) 0.1971(10) 0.0992(9) 0.084(7) Uani 1 1 d . . . C(416) C -0.0935(13) 0.1617(8) 0.1427(9) 0.067(5) Uani 1 1 d . . . C(421) C -0.0041(10) 0.1148(6) 0.3134(7) 0.040(3) Uani 1 1 d . . . C(422) C 0.0117(11) 0.1321(7) 0.3833(8) 0.049(4) Uani 1 1 d . . . C(423) C -0.0584(14) 0.1160(8) 0.4198(9) 0.065(5) Uani 1 1 d . . . C(424) C -0.1484(15) 0.0802(7) 0.3839(12) 0.073(6) Uani 1 1 d . . . C(425) C -0.1611(13) 0.0620(7) 0.3190(10) 0.058(4) Uani 1 1 d . . . C(426) C -0.0911(12) 0.0782(6) 0.2815(9) 0.053(4) Uani 1 1 d . . . H(14) H 0.3579 0.0201 -0.0400 0.128 Uiso 1 1 calc R . . H(15) H 0.3965 0.1162 -0.0343 0.113 Uiso 1 1 calc R . . H(16) H 0.3539 0.1693 0.0517 0.076 Uiso 1 1 calc R . . H(24) H -0.0681 0.1307 -0.0899 0.081 Uiso 1 1 calc R . . H(25) H -0.0924 0.0446 -0.0370 0.113 Uiso 1 1 calc R . . H(26) H -0.0017 0.0275 0.0819 0.100 Uiso 1 1 calc R . . H(112) H 0.5416 0.1093 0.1648 0.125 Uiso 1 1 calc R . . H(113) H 0.6202 0.0371 0.1144 0.154 Uiso 1 1 calc R . . H(114) H 0.6562 -0.0534 0.1611 0.107 Uiso 1 1 calc R . . H(115) H 0.6105 -0.0782 0.2627 0.069 Uiso 1 1 calc R . . H(116) H 0.5311 -0.0039 0.3158 0.054 Uiso 1 1 calc R . . H(122) H 0.5821 0.1430 0.4233 0.054 Uiso 1 1 calc R . . H(123) H 0.7405 0.1997 0.4747 0.077 Uiso 1 1 calc R . . H(124) H 0.8256 0.2453 0.4069 0.083 Uiso 1 1 calc R . . H(125) H 0.7587 0.2430 0.2833 0.098 Uiso 1 1 calc R . . H(126) H 0.5974 0.1857 0.2266 0.072 Uiso 1 1 calc R . . H(1B1) H 0.4103 0.1202 0.3835 0.030 Uiso 1 1 calc R . . H(1B2) H 0.4781 0.0624 0.3818 0.030 Uiso 1 1 calc R . . H(212) H 0.2572 -0.0560 0.2279 0.049 Uiso 1 1 calc R . . H(213) H 0.3235 -0.1531 0.2395 0.060 Uiso 1 1 calc R . . H(214) H 0.4400 -0.1837 0.3470 0.066 Uiso 1 1 calc R . . H(215) H 0.4836 -0.1233 0.4449 0.057 Uiso 1 1 calc R . . H(216) H 0.4173 -0.0317 0.4366 0.055 Uiso 1 1 calc R . . H(222) H 0.1281 -0.0147 0.3599 0.041 Uiso 1 1 calc R . . H(223) H 0.0690 -0.0232 0.4594 0.051 Uiso 1 1 calc R . . H(224) H 0.1452 0.0339 0.5597 0.053 Uiso 1 1 calc R . . H(225) H 0.2788 0.1000 0.5592 0.055 Uiso 1 1 calc R . . H(226) H 0.3412 0.1093 0.4576 0.045 Uiso 1 1 calc R . . H(2B1) H 0.1272 0.2261 0.3333 0.030 Uiso 1 1 calc R . . H(2B2) H 0.2090 0.1739 0.3652 0.030 Uiso 1 1 calc R . . H(312) H 0.2071 0.3235 0.3483 0.041 Uiso 1 1 calc R . . H(313) H 0.1141 0.4107 0.3129 0.045 Uiso 1 1 calc R . . H(314) H 0.0611 0.4379 0.1939 0.054 Uiso 1 1 calc R . . H(315) H 0.0931 0.3750 0.1096 0.062 Uiso 1 1 calc R . . H(316) H 0.1866 0.2860 0.1452 0.050 Uiso 1 1 calc R . . H(322) H 0.3306 0.2115 0.4386 0.043 Uiso 1 1 calc R . . H(323) H 0.4742 0.2463 0.5282 0.061 Uiso 1 1 calc R . . H(324) H 0.5961 0.3125 0.5051 0.059 Uiso 1 1 calc R . . H(325) H 0.5848 0.3371 0.3885 0.052 Uiso 1 1 calc R . . H(326) H 0.4453 0.2965 0.2942 0.039 Uiso 1 1 calc R . . H(412) H 0.0024 0.2619 0.2633 0.034 Uiso 1 1 calc R . . H(413) H -0.1399 0.3176 0.1924 0.052 Uiso 1 1 calc R . . H(414) H -0.2570 0.2744 0.0907 0.098 Uiso 1 1 calc R . . H(415) H -0.2321 0.1813 0.0573 0.100 Uiso 1 1 calc R . . H(416) H -0.0831 0.1225 0.1308 0.080 Uiso 1 1 calc R . . H(422) H 0.0721 0.1556 0.4062 0.059 Uiso 1 1 calc R . . H(423) H -0.0475 0.1283 0.4673 0.078 Uiso 1 1 calc R . . H(424) H -0.1993 0.0696 0.4074 0.088 Uiso 1 1 calc R . . H(425) H -0.2197 0.0370 0.2971 0.069 Uiso 1 1 calc R . . H(426) H -0.1022 0.0645 0.2345 0.063 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Re(1) 0.0273(3) 0.0198(3) 0.0246(3) -0.0014(2) 0.01155(19) 0.00056(17) Re(2) 0.0276(3) 0.0191(3) 0.0267(3) -0.0027(2) 0.00787(19) 0.00003(17) Cl(1) 0.042(2) 0.0327(17) 0.0406(16) -0.0071(15) 0.0231(14) 0.0035(13) Cl(2) 0.0380(19) 0.0284(17) 0.0508(18) -0.0110(14) 0.0138(15) 0.0001(13) P(1) 0.0239(17) 0.0243(16) 0.0283(15) 0.0016(13) 0.0129(12) -0.0002(12) P(2) 0.0241(17) 0.0221(16) 0.0264(14) 0.0009(13) 0.0084(12) 0.0043(11) P(3) 0.0204(16) 0.0190(15) 0.0284(14) 0.0003(12) 0.0100(12) -0.0009(11) P(4) 0.0192(16) 0.0241(16) 0.0330(15) -0.0003(13) 0.0068(12) 0.0014(12) O(12) 0.058(6) 0.016(4) 0.037(5) 0.003(4) 0.024(4) -0.001(3) O(22) 0.040(5) 0.023(4) 0.030(4) -0.004(4) 0.003(4) 0.002(3) O(171) 0.152(13) 0.031(6) 0.051(6) 0.003(7) 0.049(7) 0.006(5) O(172) 0.23(2) 0.041(7) 0.094(10) -0.006(9) 0.103(12) -0.013(6) O(271) 0.056(7) 0.050(6) 0.043(5) -0.011(5) 0.011(5) 0.012(4) O(272) 0.058(8) 0.097(9) 0.035(6) 0.003(7) 0.006(5) 0.021(5) N(11) 0.056(8) 0.020(5) 0.027(5) -0.006(5) 0.019(5) -0.005(4) N(21) 0.049(7) 0.029(6) 0.023(5) -0.007(5) 0.000(5) 0.001(4) C(12) 0.055(10) 0.029(7) 0.036(7) -0.003(7) 0.017(6) -0.007(5) C(13) 0.125(16) 0.026(8) 0.048(9) 0.002(9) 0.049(10) -0.005(6) C(14) 0.23(3) 0.046(11) 0.073(12) -0.004(15) 0.094(16) -0.010(9) C(15) 0.19(3) 0.043(11) 0.078(13) -0.005(13) 0.085(15) -0.004(9) C(16) 0.117(16) 0.042(9) 0.044(8) -0.011(10) 0.046(9) -0.001(7) C(17) 0.118(17) 0.045(10) 0.064(11) -0.008(10) 0.045(11) -0.023(8) C(1B) 0.029(7) 0.019(6) 0.027(6) 0.001(5) 0.008(5) 0.007(4) C(22) 0.034(8) 0.033(7) 0.037(7) 0.003(6) 0.011(6) 0.001(5) C(23) 0.046(9) 0.058(10) 0.025(6) 0.002(7) -0.001(6) 0.003(6) C(24) 0.070(13) 0.056(11) 0.060(10) -0.020(9) -0.006(9) 0.010(8) C(25) 0.095(18) 0.087(16) 0.075(13) -0.032(13) -0.014(11) 0.001(11) C(26) 0.103(17) 0.076(13) 0.045(9) -0.046(12) -0.016(9) 0.017(8) C(27) 0.048(10) 0.066(11) 0.036(8) 0.008(8) 0.010(7) 0.008(7) C(2B) 0.022(6) 0.025(6) 0.034(6) 0.005(5) 0.018(5) -0.003(5) C(111) 0.036(8) 0.039(8) 0.042(7) 0.006(6) 0.014(6) 0.000(6) C(112) 0.16(2) 0.109(17) 0.085(13) 0.097(16) 0.094(15) 0.047(12) C(113) 0.17(3) 0.17(3) 0.060(12) 0.11(2) 0.052(14) 0.023(14) C(114) 0.124(19) 0.090(16) 0.058(11) 0.051(14) 0.035(12) -0.010(10) C(115) 0.037(9) 0.046(9) 0.086(12) 0.009(7) 0.016(8) -0.011(8) C(116) 0.031(8) 0.041(9) 0.069(9) -0.013(7) 0.025(7) -0.010(7) C(121) 0.022(7) 0.025(7) 0.059(8) 0.010(5) 0.020(6) 0.001(6) C(122) 0.025(8) 0.050(9) 0.057(9) 0.004(7) 0.006(6) -0.005(7) C(123) 0.034(9) 0.062(11) 0.089(12) 0.001(8) 0.006(9) -0.024(10) C(124) 0.034(10) 0.046(11) 0.113(16) 0.001(8) -0.001(10) 0.001(10) C(125) 0.032(10) 0.033(9) 0.19(2) 0.010(7) 0.052(13) 0.043(12) C(126) 0.026(8) 0.073(12) 0.084(11) 0.015(8) 0.019(8) 0.026(9) C(211) 0.019(7) 0.027(7) 0.052(7) -0.005(5) 0.019(6) -0.001(6) C(212) 0.047(9) 0.032(8) 0.052(8) -0.001(6) 0.028(7) 0.000(6) C(213) 0.051(10) 0.024(7) 0.086(11) 0.011(7) 0.038(9) 0.003(7) C(214) 0.037(9) 0.030(8) 0.101(13) 0.013(7) 0.025(9) 0.029(8) C(215) 0.030(8) 0.037(8) 0.063(9) 0.001(7) -0.005(7) 0.015(7) C(216) 0.034(8) 0.039(8) 0.053(8) -0.001(7) -0.007(6) 0.007(6) C(221) 0.022(7) 0.031(7) 0.027(6) 0.003(5) 0.007(5) 0.006(5) C(222) 0.036(8) 0.037(8) 0.035(7) -0.003(6) 0.019(6) 0.002(5) C(223) 0.043(9) 0.044(8) 0.051(8) -0.002(7) 0.029(7) 0.010(6) C(224) 0.057(10) 0.040(8) 0.048(8) -0.001(7) 0.035(7) 0.010(6) C(225) 0.050(10) 0.054(9) 0.042(8) 0.000(8) 0.024(7) 0.000(6) C(226) 0.034(8) 0.041(8) 0.039(7) 0.012(6) 0.014(6) 0.007(6) C(311) 0.020(6) 0.033(7) 0.035(6) 0.001(5) 0.014(5) 0.007(5) C(312) 0.026(7) 0.038(8) 0.037(7) -0.002(6) 0.009(5) -0.011(5) C(313) 0.033(8) 0.030(7) 0.051(8) 0.004(6) 0.015(6) -0.009(6) C(314) 0.038(9) 0.023(7) 0.074(10) 0.017(6) 0.017(7) 0.009(7) C(315) 0.053(10) 0.051(9) 0.054(9) 0.025(8) 0.019(7) 0.031(7) C(316) 0.053(9) 0.035(8) 0.044(7) 0.010(7) 0.026(7) 0.011(6) C(321) 0.021(6) 0.019(6) 0.038(6) -0.001(5) 0.009(5) -0.006(5) C(322) 0.019(7) 0.050(8) 0.041(7) -0.008(6) 0.014(5) -0.014(6) C(323) 0.042(9) 0.073(11) 0.031(7) 0.021(8) 0.002(6) -0.005(7) C(324) 0.021(8) 0.072(11) 0.053(9) -0.008(7) 0.009(6) -0.023(7) C(325) 0.023(7) 0.041(8) 0.069(9) -0.009(6) 0.018(7) -0.013(7) C(326) 0.022(7) 0.031(7) 0.042(7) -0.004(5) 0.005(5) -0.009(5) C(411) 0.025(7) 0.036(7) 0.032(6) 0.004(6) 0.002(5) -0.002(5) C(412) 0.022(7) 0.033(7) 0.030(6) -0.004(5) 0.008(5) -0.005(5) C(413) 0.036(8) 0.039(8) 0.055(8) 0.013(7) 0.014(7) 0.003(6) C(414) 0.051(12) 0.134(19) 0.054(10) 0.058(12) 0.005(8) 0.017(11) C(415) 0.038(10) 0.129(18) 0.059(10) 0.024(11) -0.022(8) -0.039(11) C(416) 0.037(10) 0.075(12) 0.069(11) 0.013(9) -0.012(8) -0.031(9) C(421) 0.018(7) 0.044(8) 0.064(9) -0.004(6) 0.023(6) 0.003(7) C(422) 0.028(8) 0.068(10) 0.058(9) 0.001(7) 0.025(7) 0.015(8) C(423) 0.061(12) 0.069(12) 0.080(11) 0.005(10) 0.046(10) 0.030(9) C(424) 0.062(13) 0.038(10) 0.146(19) 0.024(9) 0.070(13) 0.035(11) C(425) 0.033(9) 0.036(9) 0.114(14) -0.002(7) 0.037(9) -0.003(9) C(426) 0.028(8) 0.044(9) 0.095(12) -0.007(7) 0.031(8) -0.011(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_site_symmetry_2 _geom_bond_publ_flag Re(1) O(22) 2.154(8) . ? Re(1) N(11) 2.231(9) . ? Re(1) Re(2) 2.3035(6) . ? Re(1) P(3) 2.411(3) . ? Re(1) P(1) 2.413(3) . ? Re(1) Cl(1) 2.562(3) . ? Re(2) O(12) 2.184(8) . ? Re(2) N(21) 2.214(9) . ? Re(2) P(2) 2.409(3) . ? Re(2) P(4) 2.418(3) . ? Re(2) Cl(2) 2.539(3) . ? P(1) C(111) 1.790(13) . ? P(1) C(121) 1.791(13) . ? P(1) C(1B) 1.805(11) . ? P(2) C(221) 1.837(11) . ? P(2) C(211) 1.848(12) . ? P(2) C(1B) 1.863(12) . ? P(3) C(311) 1.803(12) . ? P(3) C(2B) 1.809(11) . ? P(3) C(321) 1.823(11) . ? P(4) C(411) 1.799(12) . ? P(4) C(2B) 1.818(12) . ? P(4) C(421) 1.832(13) . ? O(12) C(12) 1.296(15) . ? O(22) C(22) 1.299(15) . ? O(171) C(17) 1.317(19) . ? O(172) C(17) 1.260(18) . ? O(271) C(27) 1.351(18) . ? O(272) C(27) 1.209(15) . ? N(11) C(16) 1.323(16) . ? N(11) C(12) 1.356(16) . ? N(21) C(26) 1.334(18) . ? N(21) C(22) 1.363(16) . ? C(12) C(13) 1.375(17) . ? C(13) C(14) 1.38(2) . ? C(13) C(17) 1.49(2) . ? C(14) C(15) 1.29(2) . ? C(15) C(16) 1.35(2) . ? C(22) C(23) 1.416(17) . ? C(23) C(24) 1.39(2) . ? C(23) C(27) 1.50(2) . ? C(24) C(25) 1.34(2) . ? C(25) C(26) 1.40(2) . ? C(111) C(116) 1.366(19) . ? C(111) C(112) 1.39(2) . ? C(112) C(113) 1.40(2) . ? C(113) C(114) 1.34(3) . ? C(114) C(115) 1.36(2) . ? C(115) C(116) 1.45(2) . ? C(121) C(122) 1.378(19) . ? C(121) C(126) 1.43(2) . ? C(122) C(123) 1.46(2) . ? C(123) C(124) 1.31(2) . ? C(124) C(125) 1.39(3) . ? C(125) C(126) 1.48(2) . ? C(211) C(212) 1.399(17) . ? C(211) C(216) 1.414(17) . ? C(212) C(213) 1.419(18) . ? C(213) C(214) 1.37(2) . ? C(214) C(215) 1.37(2) . ? C(215) C(216) 1.330(19) . ? C(221) C(222) 1.370(17) . ? C(221) C(226) 1.388(17) . ? C(222) C(223) 1.386(16) . ? C(223) C(224) 1.384(19) . ? C(224) C(225) 1.37(2) . ? C(225) C(226) 1.434(18) . ? C(311) C(316) 1.378(17) . ? C(311) C(312) 1.411(16) . ? C(312) C(313) 1.402(17) . ? C(313) C(314) 1.376(19) . ? C(314) C(315) 1.39(2) . ? C(315) C(316) 1.435(18) . ? C(321) C(326) 1.416(17) . ? C(321) C(322) 1.419(16) . ? C(322) C(323) 1.358(18) . ? C(323) C(324) 1.41(2) . ? C(324) C(325) 1.380(19) . ? C(325) C(326) 1.414(17) . ? C(411) C(412) 1.369(17) . ? C(411) C(416) 1.443(18) . ? C(412) C(413) 1.400(17) . ? C(413) C(414) 1.40(2) . ? C(414) C(415) 1.36(2) . ? C(415) C(416) 1.48(2) . ? C(421) C(422) 1.393(19) . ? C(421) C(426) 1.401(19) . ? C(422) C(423) 1.375(19) . ? C(423) C(424) 1.43(3) . ? C(424) C(425) 1.31(2) . ? C(425) C(426) 1.39(2) . ? 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 O(22) Re(1) N(11) 79.8(4) . . ? O(22) Re(1) Re(2) 89.3(2) . . ? N(11) Re(1) Re(2) 87.1(3) . . ? O(22) Re(1) P(3) 93.7(2) . . ? N(11) Re(1) P(3) 170.9(3) . . ? Re(2) Re(1) P(3) 99.33(7) . . ? O(22) Re(1) P(1) 170.6(2) . . ? N(11) Re(1) P(1) 91.7(3) . . ? Re(2) Re(1) P(1) 94.29(7) . . ? P(3) Re(1) P(1) 94.27(10) . . ? O(22) Re(1) Cl(1) 81.8(2) . . ? N(11) Re(1) Cl(1) 87.5(3) . . ? Re(2) Re(1) Cl(1) 170.29(7) . . ? P(3) Re(1) Cl(1) 85.13(10) . . ? P(1) Re(1) Cl(1) 93.97(10) . . ? O(12) Re(2) N(21) 81.1(4) . . ? O(12) Re(2) Re(1) 89.0(2) . . ? N(21) Re(2) Re(1) 87.3(3) . . ? O(12) Re(2) P(2) 92.0(2) . . ? N(21) Re(2) P(2) 170.1(3) . . ? Re(1) Re(2) P(2) 99.74(7) . . ? O(12) Re(2) P(4) 173.4(2) . . ? N(21) Re(2) P(4) 93.1(3) . . ? Re(1) Re(2) P(4) 93.92(7) . . ? P(2) Re(2) P(4) 93.41(10) . . ? O(12) Re(2) Cl(2) 84.7(2) . . ? N(21) Re(2) Cl(2) 86.4(3) . . ? Re(1) Re(2) Cl(2) 171.67(8) . . ? P(2) Re(2) Cl(2) 85.90(10) . . ? P(4) Re(2) Cl(2) 91.85(11) . . ? C(111) P(1) C(121) 99.4(6) . . ? C(111) P(1) C(1B) 107.9(6) . . ? C(121) P(1) C(1B) 102.0(6) . . ? C(111) P(1) Re(1) 115.7(4) . . ? C(121) P(1) Re(1) 122.5(4) . . ? C(1B) P(1) Re(1) 107.8(4) . . ? C(221) P(2) C(211) 96.9(5) . . ? C(221) P(2) C(1B) 103.6(5) . . ? C(211) P(2) C(1B) 105.1(5) . . ? C(221) P(2) Re(2) 121.7(4) . . ? C(211) P(2) Re(2) 118.9(4) . . ? C(1B) P(2) Re(2) 108.5(3) . . ? C(311) P(3) C(2B) 101.4(5) . . ? C(311) P(3) C(321) 98.5(5) . . ? C(2B) P(3) C(321) 102.7(5) . . ? C(311) P(3) Re(1) 119.8(4) . . ? C(2B) P(3) Re(1) 109.8(4) . . ? C(321) P(3) Re(1) 121.6(4) . . ? C(411) P(4) C(2B) 103.8(6) . . ? C(411) P(4) C(421) 96.9(6) . . ? C(2B) P(4) C(421) 104.1(6) . . ? C(411) P(4) Re(2) 119.3(4) . . ? C(2B) P(4) Re(2) 107.9(4) . . ? C(421) P(4) Re(2) 122.5(5) . . ? C(12) O(12) Re(2) 117.5(7) . . ? C(22) O(22) Re(1) 116.8(7) . . ? C(16) N(11) C(12) 118.4(11) . . ? C(16) N(11) Re(1) 124.4(9) . . ? C(12) N(11) Re(1) 117.1(8) . . ? C(26) N(21) C(22) 118.3(11) . . ? C(26) N(21) Re(2) 124.2(9) . . ? C(22) N(21) Re(2) 117.4(8) . . ? O(12) C(12) N(11) 120.1(11) . . ? O(12) C(12) C(13) 122.4(12) . . ? N(11) C(12) C(13) 117.4(12) . . ? C(12) C(13) C(14) 120.3(14) . . ? C(12) C(13) C(17) 119.8(13) . . ? C(14) C(13) C(17) 119.8(14) . . ? C(15) C(14) C(13) 122.0(16) . . ? C(14) C(15) C(16) 116.0(17) . . ? N(11) C(16) C(15) 125.5(15) . . ? O(172) C(17) O(171) 117.5(15) . . ? O(172) C(17) C(13) 122.5(15) . . ? O(171) C(17) C(13) 119.8(13) . . ? P(1) C(1B) P(2) 111.0(6) . . ? O(22) C(22) N(21) 119.3(11) . . ? O(22) C(22) C(23) 121.2(12) . . ? N(21) C(22) C(23) 119.5(12) . . ? C(24) C(23) C(22) 121.0(14) . . ? C(24) C(23) C(27) 117.3(12) . . ? C(22) C(23) C(27) 121.6(13) . . ? C(25) C(24) C(23) 117.5(16) . . ? C(24) C(25) C(26) 120.6(18) . . ? N(21) C(26) C(25) 122.8(16) . . ? O(272) C(27) O(271) 119.2(14) . . ? O(272) C(27) C(23) 122.2(15) . . ? O(271) C(27) C(23) 118.6(11) . . ? P(3) C(2B) P(4) 110.7(6) . . ? C(116) C(111) C(112) 115.4(13) . . ? C(116) C(111) P(1) 127.2(11) . . ? C(112) C(111) P(1) 117.2(11) . . ? C(111) C(112) C(113) 119.5(18) . . ? C(114) C(113) C(112) 123.8(19) . . ? C(113) C(114) C(115) 120.0(17) . . ? C(114) C(115) C(116) 116.1(16) . . ? C(111) C(116) C(115) 124.9(14) . . ? C(122) C(121) C(126) 118.7(14) . . ? C(122) C(121) P(1) 123.3(11) . . ? C(126) C(121) P(1) 117.9(11) . . ? C(121) C(122) C(123) 120.6(15) . . ? C(124) C(123) C(122) 121.3(17) . . ? C(123) C(124) C(125) 121.6(17) . . ? C(124) C(125) C(126) 119.2(16) . . ? C(121) C(126) C(125) 118.5(16) . . ? C(212) C(211) C(216) 118.0(12) . . ? C(212) C(211) P(2) 121.0(10) . . ? C(216) C(211) P(2) 121.0(10) . . ? C(211) C(212) C(213) 119.0(13) . . ? C(214) C(213) C(212) 119.3(14) . . ? C(215) C(214) C(213) 121.3(13) . . ? C(216) C(215) C(214) 120.1(13) . . ? C(215) C(216) C(211) 122.1(13) . . ? C(222) C(221) C(226) 120.9(11) . . ? C(222) C(221) P(2) 117.7(9) . . ? C(226) C(221) P(2) 121.4(9) . . ? C(221) C(222) C(223) 120.5(12) . . ? C(224) C(223) C(222) 120.6(13) . . ? C(225) C(224) C(223) 119.3(12) . . ? C(224) C(225) C(226) 121.1(13) . . ? C(221) C(226) C(225) 117.6(13) . . ? C(316) C(311) C(312) 117.4(11) . . ? C(316) C(311) P(3) 123.1(10) . . ? C(312) C(311) P(3) 119.4(9) . . ? C(313) C(312) C(311) 122.0(12) . . ? C(314) C(313) C(312) 120.1(12) . . ? C(313) C(314) C(315) 119.3(12) . . ? C(314) C(315) C(316) 120.6(12) . . ? C(311) C(316) C(315) 120.5(12) . . ? C(326) C(321) C(322) 118.9(10) . . ? C(326) C(321) P(3) 116.7(9) . . ? C(322) C(321) P(3) 124.3(9) . . ? C(323) C(322) C(321) 119.6(13) . . ? C(322) C(323) C(324) 121.6(13) . . ? C(325) C(324) C(323) 120.5(12) . . ? C(324) C(325) C(326) 118.8(13) . . ? C(325) C(326) C(321) 120.5(12) . . ? C(412) C(411) C(416) 119.6(12) . . ? C(412) C(411) P(4) 124.1(9) . . ? C(416) C(411) P(4) 115.5(10) . . ? C(411) C(412) C(413) 123.8(11) . . ? C(414) C(413) C(412) 117.2(13) . . ? C(415) C(414) C(413) 122.8(14) . . ? C(414) C(415) C(416) 120.1(14) . . ? C(411) C(416) C(415) 116.4(14) . . ? C(422) C(421) C(426) 118.4(13) . . ? C(422) C(421) P(4) 121.4(10) . . ? C(426) C(421) P(4) 120.0(11) . . ? C(423) C(422) C(421) 121.4(16) . . ? C(422) C(423) C(424) 118.0(17) . . ? C(425) C(424) C(423) 120.7(16) . . ? C(424) C(425) C(426) 121.8(17) . . ? C(425) C(426) C(421) 119.6(16) . . ? #===END #============================================================================== data_SWCH16 _database_code_CSD 212137 _audit_creation_date 23-05-03 _audit_creation_method from_MolEN_and_SHELXL _audit_update_record ; ? ; # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description plate _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.43 _exptl_crystal_size_min 0.28 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C62 H50 N2 O6 P4 Re2' _chemical_formula_moiety Re2(picO)2(dppm)2 _chemical_formula_structural ? _chemical_formula_weight 1415.40 _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 12.1326(3) _cell_length_b 21.4366(5) _cell_length_c 23.4676(6) _cell_angle_alpha 90.00 _cell_angle_beta 104.9374(11) _cell_angle_gamma 90.00 _cell_volume 5897.2(3) _cell_measurement_reflns_used 24531 _cell_measurement_theta_min 2 _cell_measurement_theta_max 27 _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.59 _exptl_crystal_density_meas ? _diffrn_radiation_type MO-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 4.313 _cell_measurement_temperature 150 _exptl_crystal_F_000 2776 # 6. DATA COLLECTION _diffrn_ambient_temperature 150 _diffrn_measurement_device_type Nonius_KappaCCD _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan_(Otwinowski_&_Minor,_1 _exptl_absorpt_correction_T_min 0.1362 _exptl_absorpt_correction_T_max 0.3054 _diffrn_reflns_number 24531 _diffrn_measured_fraction_theta_max 0.5205 _reflns_number_total 13040 _reflns_number_gt 10096 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.047 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 27.87 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_max 29 _diffrn_special_details 'mosaicity from Denzo/Scalepack is 0.77' # 7. REFINEMENT DATA _refine_special_details ; Residual electron density was adjusted using the SQUEEZE option in program PLATON (Spek, 1997). 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 0.076 _refine_ls_hydrogen_treatment H_atoms_riding _refine_ls_number_reflns 13001 _refine_ls_number_parameters 685 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 0.913 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details '1/[\s^2^(Fo^2^)+(0.0296P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3 ' _refine_ls_shift/su_max 0.001 _refine_diff_density_max 1.26 _refine_diff_density_min -2.54 _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) PLATON (Spek, 1997) ; _computing_publication_material CIF_VAX_MolEN_(Fair,_1990) # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re(1) Re 0.140371(17) 0.220887(10) 0.393067(10) 0.02092(6) Uani 1 1 d . . . Re(2) Re 0.292104(17) 0.257843(10) 0.359589(10) 0.02089(6) Uani 1 1 d . . . P(1) P 0.22249(11) 0.11926(6) 0.41098(6) 0.0221(3) Uani 1 1 d . . . P(2) P 0.39159(11) 0.16546(6) 0.34342(6) 0.0229(3) Uani 1 1 d . . . P(3) P -0.00741(11) 0.20105(6) 0.30438(6) 0.0232(3) Uani 1 1 d . . . P(4) P 0.17433(12) 0.27350(6) 0.26243(6) 0.0229(3) Uani 1 1 d . . . O(16) O 0.4016(3) 0.26805(15) 0.44508(16) 0.0246(8) Uani 1 1 d . . . O(26) O 0.0740(3) 0.30998(16) 0.40033(16) 0.0271(9) Uani 1 1 d . . . O(171) O 0.0445(3) 0.19578(17) 0.45626(17) 0.0297(9) Uani 1 1 d . . . O(172) O 0.0237(4) 0.2152(2) 0.54668(19) 0.0467(12) Uani 1 1 d . . . O(271) O 0.4050(3) 0.32509(17) 0.33455(16) 0.0318(9) Uani 1 1 d . . . O(272) O 0.4688(4) 0.4232(2) 0.3445(2) 0.0601(14) Uani 1 1 d . . . N(1) N 0.2435(3) 0.24981(19) 0.47804(18) 0.0209(10) Uani 1 1 d . . . N(21) N 0.2385(4) 0.34841(19) 0.3822(2) 0.0261(11) Uani 1 1 d . . . C(11) C 0.1362(4) 0.0477(2) 0.4068(2) 0.0235(12) Uani 1 1 d . . . C(12) C 0.1891(5) 0.2532(2) 0.5225(2) 0.0271(13) Uani 1 1 d . . . C(13) C 0.2345(5) 0.2820(3) 0.5740(3) 0.0366(15) Uani 1 1 d . . . C(14) C 0.3433(5) 0.3112(3) 0.5837(3) 0.0379(15) Uani 1 1 d . . . C(15) C 0.4012(5) 0.3054(3) 0.5399(3) 0.0318(14) Uani 1 1 d . . . C(16) C 0.3506(5) 0.2743(2) 0.4873(2) 0.0246(12) Uani 1 1 d . . . C(17) C 0.0771(5) 0.2200(3) 0.5081(3) 0.0297(14) Uani 1 1 d . . . C(1B) C 0.3139(4) 0.0985(2) 0.3626(2) 0.0264(13) Uani 1 1 d . . . C(22) C 0.3072(5) 0.3973(2) 0.3789(2) 0.0314(14) Uani 1 1 d . . . C(23) C 0.2859(6) 0.4555(3) 0.3971(3) 0.0473(18) Uani 1 1 d . . . C(24) C 0.1903(6) 0.4644(3) 0.4182(3) 0.0520(19) Uani 1 1 d . . . C(25) C 0.1194(6) 0.4167(3) 0.4212(3) 0.0411(16) Uani 1 1 d . . . C(26) C 0.1426(5) 0.3565(3) 0.4017(2) 0.0282(13) Uani 1 1 d . . . C(27) C 0.4019(5) 0.3820(3) 0.3512(3) 0.0362(15) Uani 1 1 d . . . C(2B) C 0.0479(4) 0.2220(2) 0.2414(2) 0.0271(13) Uani 1 1 d . . . C(112) C 0.1846(5) -0.0103(2) 0.4018(3) 0.0363(15) Uani 1 1 d . . . C(113) C 0.1247(5) -0.0639(3) 0.4034(3) 0.0408(16) Uani 1 1 d . . . C(114) C 0.0161(5) -0.0620(3) 0.4114(3) 0.0422(16) Uani 1 1 d . . . C(115) C -0.0318(5) -0.0057(3) 0.4162(3) 0.0428(17) Uani 1 1 d . . . C(116) C 0.0275(5) 0.0494(3) 0.4142(3) 0.0326(14) Uani 1 1 d . . . C(121) C 0.3098(4) 0.1103(2) 0.4871(2) 0.0246(13) Uani 1 1 d . . . C(122) C 0.4258(5) 0.1165(3) 0.5025(3) 0.0338(14) Uani 1 1 d . . . C(123) C 0.4864(6) 0.1113(3) 0.5614(3) 0.0489(18) Uani 1 1 d . . . C(124) C 0.4304(6) 0.1013(3) 0.6049(3) 0.0434(16) Uani 1 1 d . . . C(125) C 0.3118(6) 0.0955(3) 0.5886(3) 0.0423(16) Uani 1 1 d . . . C(126) C 0.2531(5) 0.0995(3) 0.5306(3) 0.0316(14) Uani 1 1 d . . . C(211) C 0.4090(4) 0.1445(2) 0.2701(2) 0.0231(12) Uani 1 1 d . . . C(212) C 0.3154(5) 0.1242(2) 0.2254(3) 0.0289(14) Uani 1 1 d . . . C(213) C 0.3261(5) 0.1124(3) 0.1691(3) 0.0370(15) Uani 1 1 d . . . C(214) C 0.4324(5) 0.1187(3) 0.1568(3) 0.0379(16) Uani 1 1 d . . . C(215) C 0.5241(5) 0.1378(3) 0.2005(3) 0.0329(14) Uani 1 1 d . . . C(216) C 0.5149(4) 0.1506(2) 0.2567(2) 0.0262(13) Uani 1 1 d . . . C(221) C 0.5387(4) 0.1560(3) 0.3875(2) 0.0267(13) Uani 1 1 d . . . C(222) C 0.6017(4) 0.2098(3) 0.4086(2) 0.0294(13) Uani 1 1 d . . . C(223) C 0.7147(5) 0.2041(3) 0.4419(2) 0.0351(15) Uani 1 1 d . . . C(224) C 0.7641(5) 0.1461(3) 0.4540(3) 0.0366(15) Uani 1 1 d . . . C(225) C 0.7023(5) 0.0934(3) 0.4326(3) 0.0388(16) Uani 1 1 d . . . C(226) C 0.5907(4) 0.0978(3) 0.3988(3) 0.0324(14) Uani 1 1 d . . . C(311) C -0.0699(4) 0.1231(2) 0.2842(2) 0.0279(13) Uani 1 1 d . . . C(312) C -0.0127(5) 0.0770(3) 0.2613(3) 0.0343(15) Uani 1 1 d . . . C(313) C -0.0565(5) 0.0179(3) 0.2495(3) 0.0464(18) Uani 1 1 d . . . C(314) C -0.1596(5) 0.0030(3) 0.2624(3) 0.0511(19) Uani 1 1 d . . . C(315) C -0.2159(5) 0.0474(3) 0.2859(3) 0.0469(18) Uani 1 1 d . . . C(316) C -0.1721(5) 0.1074(3) 0.2973(3) 0.0337(15) Uani 1 1 d . . . C(321) C -0.1379(4) 0.2475(2) 0.2933(2) 0.0233(12) Uani 1 1 d . . . C(322) C -0.1695(5) 0.2739(3) 0.3406(3) 0.0321(14) Uani 1 1 d . . . C(323) C -0.2681(5) 0.3110(3) 0.3300(3) 0.0411(17) Uani 1 1 d . . . C(324) C -0.3343(5) 0.3208(3) 0.2738(3) 0.0397(16) Uani 1 1 d . . . C(325) C -0.3035(5) 0.2941(3) 0.2260(3) 0.0407(16) Uani 1 1 d . . . C(326) C -0.2078(5) 0.2572(3) 0.2363(3) 0.0320(14) Uani 1 1 d . . . C(411) C 0.2288(5) 0.2684(2) 0.1966(2) 0.0251(13) Uani 1 1 d . . . C(412) C 0.1539(5) 0.2611(3) 0.1420(3) 0.0310(14) Uani 1 1 d . . . C(413) C 0.1944(5) 0.2592(3) 0.0908(3) 0.0348(15) Uani 1 1 d . . . C(414) C 0.3101(5) 0.2637(3) 0.0959(3) 0.0315(14) Uani 1 1 d . . . C(415) C 0.3851(4) 0.2723(2) 0.1507(2) 0.0266(13) Uani 1 1 d . . . C(416) C 0.3449(5) 0.2742(2) 0.2012(2) 0.0263(13) Uani 1 1 d . . . C(421) C 0.1177(4) 0.3531(2) 0.2521(2) 0.0241(12) Uani 1 1 d . . . C(422) C 0.0173(5) 0.3712(3) 0.2674(2) 0.0271(13) Uani 1 1 d . . . C(423) C -0.0157(5) 0.4326(3) 0.2645(3) 0.0346(15) Uani 1 1 d . . . C(424) C 0.0490(5) 0.4784(3) 0.2469(3) 0.0378(15) Uani 1 1 d . . . C(425) C 0.1487(5) 0.4613(3) 0.2321(3) 0.0382(16) Uani 1 1 d . . . C(426) C 0.1826(5) 0.3993(3) 0.2346(3) 0.0323(14) Uani 1 1 d . . . H(13) H 0.1943 0.2830 0.6038 0.044 Uiso 1 1 calc R . . H(14) H 0.3753 0.3339 0.6188 0.045 Uiso 1 1 calc R . . H(15) H 0.4754 0.3227 0.5458 0.038 Uiso 1 1 calc R . . H(23) H 0.3357 0.4893 0.3954 0.057 Uiso 1 1 calc R . . H(24) H 0.1743 0.5048 0.4307 0.062 Uiso 1 1 calc R . . H(25) H 0.0548 0.4233 0.4362 0.049 Uiso 1 1 calc R . . H(112) H 0.2600 -0.0125 0.3972 0.044 Uiso 1 1 calc R . . H(113) H 0.1583 -0.1031 0.3989 0.049 Uiso 1 1 calc R . . H(114) H -0.0245 -0.0995 0.4136 0.051 Uiso 1 1 calc R . . H(115) H -0.1072 -0.0039 0.4209 0.051 Uiso 1 1 calc R . . H(116) H -0.0073 0.0884 0.4180 0.039 Uiso 1 1 calc R . . H(122) H 0.4651 0.1243 0.4731 0.041 Uiso 1 1 calc R . . H(123) H 0.5672 0.1147 0.5717 0.059 Uiso 1 1 calc R . . H(124) H 0.4718 0.0985 0.6452 0.052 Uiso 1 1 calc R . . H(125) H 0.2718 0.0886 0.6179 0.051 Uiso 1 1 calc R . . H(126) H 0.1725 0.0949 0.5199 0.038 Uiso 1 1 calc R . . H(1B1) H 0.2662 0.0798 0.3259 0.032 Uiso 1 1 calc R . . H(1B2) H 0.3697 0.0665 0.3825 0.032 Uiso 1 1 calc R . . H(212) H 0.2436 0.1186 0.2339 0.035 Uiso 1 1 calc R . . H(213) H 0.2615 0.1000 0.1388 0.044 Uiso 1 1 calc R . . H(214) H 0.4408 0.1098 0.1185 0.046 Uiso 1 1 calc R . . H(215) H 0.5961 0.1423 0.1920 0.039 Uiso 1 1 calc R . . H(216) H 0.5800 0.1635 0.2864 0.031 Uiso 1 1 calc R . . H(222) H 0.5678 0.2498 0.4003 0.035 Uiso 1 1 calc R . . H(223) H 0.7578 0.2404 0.4562 0.042 Uiso 1 1 calc R . . H(224) H 0.8407 0.1425 0.4771 0.044 Uiso 1 1 calc R . . H(225) H 0.7366 0.0535 0.4411 0.047 Uiso 1 1 calc R . . H(226) H 0.5496 0.0612 0.3834 0.039 Uiso 1 1 calc R . . H(2B1) H -0.0128 0.2433 0.2113 0.032 Uiso 1 1 calc R . . H(2B2) H 0.0687 0.1834 0.2234 0.032 Uiso 1 1 calc R . . H(312) H 0.0586 0.0866 0.2537 0.041 Uiso 1 1 calc R . . H(313) H -0.0172 -0.0124 0.2327 0.056 Uiso 1 1 calc R . . H(314) H -0.1903 -0.0379 0.2549 0.061 Uiso 1 1 calc R . . H(315) H -0.2860 0.0371 0.2945 0.056 Uiso 1 1 calc R . . H(316) H -0.2117 0.1376 0.3141 0.040 Uiso 1 1 calc R . . H(322) H -0.1249 0.2670 0.3797 0.039 Uiso 1 1 calc R . . H(323) H -0.2893 0.3297 0.3623 0.049 Uiso 1 1 calc R . . H(324) H -0.4011 0.3457 0.2674 0.048 Uiso 1 1 calc R . . H(325) H -0.3481 0.3013 0.1869 0.049 Uiso 1 1 calc R . . H(326) H -0.1884 0.2377 0.2039 0.038 Uiso 1 1 calc R . . H(412) H 0.0745 0.2572 0.1388 0.037 Uiso 1 1 calc R . . H(413) H 0.1424 0.2549 0.0531 0.042 Uiso 1 1 calc R . . H(414) H 0.3382 0.2610 0.0617 0.038 Uiso 1 1 calc R . . H(415) H 0.4644 0.2769 0.1539 0.032 Uiso 1 1 calc R . . H(416) H 0.3969 0.2794 0.2388 0.032 Uiso 1 1 calc R . . H(422) H -0.0280 0.3406 0.2798 0.033 Uiso 1 1 calc R . . H(423) H -0.0840 0.4438 0.2747 0.041 Uiso 1 1 calc R . . H(424) H 0.0257 0.5208 0.2450 0.045 Uiso 1 1 calc R . . H(425) H 0.1940 0.4923 0.2202 0.046 Uiso 1 1 calc R . . H(426) H 0.2508 0.3884 0.2243 0.039 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Re(1) 0.01850(11) 0.01849(12) 0.02798(13) 0.00067(9) 0.00996(10) 0.00050(9) Re(2) 0.01885(11) 0.01846(12) 0.02691(13) -0.00077(9) 0.00873(10) 0.00100(9) P(1) 0.0201(7) 0.0178(7) 0.0303(9) -0.0002(6) 0.0098(7) 0.0004(6) P(2) 0.0190(7) 0.0202(8) 0.0313(9) 0.0018(6) 0.0094(7) 0.0004(6) P(3) 0.0177(7) 0.0215(8) 0.0318(9) 0.0013(6) 0.0091(7) 0.0002(6) P(4) 0.0208(7) 0.0203(8) 0.0292(9) 0.0004(6) 0.0093(7) 0.0015(6) O(16) 0.0211(19) 0.022(2) 0.031(2) -0.0010(15) 0.0081(18) -0.0001(17) O(26) 0.025(2) 0.018(2) 0.042(2) -0.0005(16) 0.0146(19) -0.0016(17) O(171) 0.028(2) 0.033(2) 0.033(2) -0.0014(17) 0.016(2) 0.0016(19) O(172) 0.049(3) 0.052(3) 0.050(3) -0.007(2) 0.033(2) -0.004(2) O(271) 0.028(2) 0.032(2) 0.038(3) -0.0080(17) 0.013(2) 0.0023(19) O(272) 0.074(4) 0.039(3) 0.081(4) -0.029(2) 0.045(3) -0.006(3) N(1) 0.022(2) 0.022(2) 0.021(3) -0.0021(19) 0.011(2) -0.0039(19) N(21) 0.027(3) 0.016(2) 0.038(3) -0.004(2) 0.013(2) -0.006(2) C(11) 0.025(3) 0.020(3) 0.025(3) -0.001(2) 0.005(3) 0.002(2) C(12) 0.032(3) 0.028(3) 0.026(3) 0.001(3) 0.017(3) 0.000(3) C(13) 0.034(3) 0.045(4) 0.035(4) 0.005(3) 0.017(3) -0.006(3) C(14) 0.032(4) 0.046(4) 0.033(4) -0.006(3) 0.005(3) -0.007(3) C(15) 0.023(3) 0.035(3) 0.036(4) 0.001(3) 0.005(3) -0.005(3) C(16) 0.026(3) 0.022(3) 0.026(3) 0.005(2) 0.006(3) 0.004(2) C(17) 0.022(3) 0.035(3) 0.035(4) 0.002(3) 0.011(3) 0.001(3) C(1B) 0.023(3) 0.021(3) 0.034(4) -0.003(2) 0.007(3) 0.002(3) C(22) 0.048(4) 0.017(3) 0.028(3) -0.002(3) 0.007(3) 0.002(2) C(23) 0.059(5) 0.025(4) 0.059(5) -0.012(3) 0.017(4) -0.009(3) C(24) 0.072(5) 0.021(4) 0.067(5) 0.000(3) 0.024(4) -0.013(3) C(25) 0.052(4) 0.026(3) 0.048(4) 0.010(3) 0.017(4) -0.001(3) C(26) 0.039(4) 0.023(3) 0.023(3) 0.010(3) 0.010(3) 0.004(2) C(27) 0.049(4) 0.023(3) 0.039(4) -0.017(3) 0.016(3) 0.002(3) C(2B) 0.023(3) 0.029(3) 0.031(3) 0.007(2) 0.009(3) 0.000(3) C(112) 0.029(3) 0.022(3) 0.062(5) 0.000(3) 0.020(3) 0.006(3) C(113) 0.039(4) 0.022(3) 0.063(5) 0.001(3) 0.015(4) 0.001(3) C(114) 0.044(4) 0.025(3) 0.061(5) -0.009(3) 0.019(4) 0.003(3) C(115) 0.025(3) 0.038(4) 0.069(5) -0.012(3) 0.018(3) 0.000(3) C(116) 0.025(3) 0.028(3) 0.048(4) 0.004(3) 0.016(3) 0.001(3) C(121) 0.024(3) 0.019(3) 0.030(3) -0.001(2) 0.006(3) 0.003(2) C(122) 0.031(3) 0.040(4) 0.029(4) -0.008(3) 0.006(3) 0.005(3) C(123) 0.039(4) 0.056(5) 0.051(5) -0.011(3) 0.010(4) 0.004(4) C(124) 0.049(4) 0.044(4) 0.028(4) -0.006(3) -0.005(3) 0.002(3) C(125) 0.047(4) 0.044(4) 0.040(4) -0.001(3) 0.018(4) 0.005(3) C(126) 0.028(3) 0.036(4) 0.033(4) -0.002(3) 0.011(3) 0.003(3) C(211) 0.028(3) 0.008(3) 0.036(4) 0.002(2) 0.012(3) 0.003(2) C(212) 0.027(3) 0.018(3) 0.043(4) 0.000(2) 0.011(3) 0.000(3) C(213) 0.040(4) 0.033(3) 0.038(4) 0.002(3) 0.008(3) -0.002(3) C(214) 0.046(4) 0.033(4) 0.041(4) 0.003(3) 0.022(4) -0.006(3) C(215) 0.034(3) 0.029(3) 0.041(4) 0.001(3) 0.019(3) 0.004(3) C(216) 0.022(3) 0.023(3) 0.035(4) -0.001(2) 0.010(3) 0.002(3) C(221) 0.021(3) 0.034(3) 0.028(3) 0.001(2) 0.011(3) 0.005(3) C(222) 0.017(3) 0.039(4) 0.032(4) 0.002(2) 0.005(3) 0.001(3) C(223) 0.029(3) 0.046(4) 0.032(4) -0.004(3) 0.010(3) -0.002(3) C(224) 0.024(3) 0.050(4) 0.037(4) 0.003(3) 0.010(3) 0.007(3) C(225) 0.031(3) 0.043(4) 0.046(4) 0.011(3) 0.017(3) 0.007(3) C(226) 0.015(3) 0.035(3) 0.047(4) 0.007(2) 0.008(3) 0.001(3) C(311) 0.023(3) 0.021(3) 0.038(4) -0.004(2) 0.007(3) -0.005(3) C(312) 0.024(3) 0.028(3) 0.051(4) 0.002(3) 0.010(3) -0.003(3) C(313) 0.040(4) 0.032(4) 0.068(5) -0.001(3) 0.016(4) -0.015(3) C(314) 0.038(4) 0.022(3) 0.091(6) -0.008(3) 0.013(4) -0.010(3) C(315) 0.021(3) 0.027(4) 0.094(6) -0.004(3) 0.018(4) -0.007(4) C(316) 0.021(3) 0.029(3) 0.054(4) -0.004(2) 0.015(3) -0.001(3) C(321) 0.013(3) 0.021(3) 0.034(4) 0.001(2) 0.004(3) 0.000(2) C(322) 0.027(3) 0.036(4) 0.037(4) 0.006(3) 0.015(3) 0.002(3) C(323) 0.030(3) 0.037(4) 0.066(5) 0.006(3) 0.029(4) -0.001(3) C(324) 0.023(3) 0.027(3) 0.070(5) 0.007(3) 0.014(4) 0.013(3) C(325) 0.018(3) 0.051(4) 0.052(4) -0.004(3) 0.007(3) 0.005(3) C(326) 0.023(3) 0.032(3) 0.042(4) 0.003(3) 0.010(3) -0.002(3) C(411) 0.024(3) 0.022(3) 0.029(3) -0.002(2) 0.007(3) 0.005(2) C(412) 0.020(3) 0.040(4) 0.036(4) 0.002(3) 0.013(3) 0.005(3) C(413) 0.031(3) 0.045(4) 0.027(3) -0.008(3) 0.006(3) -0.003(3) C(414) 0.026(3) 0.037(3) 0.039(4) 0.001(3) 0.020(3) 0.006(3) C(415) 0.020(3) 0.027(3) 0.033(4) -0.002(2) 0.009(3) 0.002(3) C(416) 0.025(3) 0.024(3) 0.031(3) -0.002(2) 0.010(3) 0.004(3) C(421) 0.026(3) 0.022(3) 0.021(3) 0.003(2) -0.001(3) 0.007(2) C(422) 0.028(3) 0.025(3) 0.030(3) -0.002(2) 0.011(3) -0.001(3) C(423) 0.033(3) 0.030(3) 0.043(4) 0.007(3) 0.014(3) 0.006(3) C(424) 0.039(4) 0.024(3) 0.049(4) 0.009(3) 0.008(3) 0.002(3) C(425) 0.043(4) 0.020(3) 0.053(4) -0.004(3) 0.015(3) 0.005(3) C(426) 0.025(3) 0.026(3) 0.046(4) 0.003(3) 0.011(3) 0.006(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_site_symmetry_2 _geom_bond_publ_flag Re(1) O(26) 2.096(3) . ? Re(1) N(1) 2.154(4) . ? Re(1) O(171) 2.175(3) . ? Re(1) Re(2) 2.3194(3) . ? Re(1) P(1) 2.3873(13) . ? Re(1) P(3) 2.4091(15) . ? Re(2) O(16) 2.113(4) . ? Re(2) N(21) 2.157(4) . ? Re(2) O(271) 2.171(3) . ? Re(2) P(4) 2.3820(15) . ? Re(2) P(2) 2.3998(13) . ? P(1) C(1B) 1.835(5) . ? P(1) C(121) 1.837(6) . ? P(1) C(11) 1.845(5) . ? P(2) C(221) 1.829(5) . ? P(2) C(1B) 1.836(5) . ? P(2) C(211) 1.842(5) . ? P(3) C(2B) 1.830(5) . ? P(3) C(321) 1.831(5) . ? P(3) C(311) 1.845(5) . ? P(4) C(421) 1.831(5) . ? P(4) C(411) 1.833(5) . ? P(4) C(2B) 1.851(5) . ? O(16) C(16) 1.304(6) . ? O(26) C(26) 1.294(6) . ? O(171) C(17) 1.287(6) . ? O(172) C(17) 1.247(6) . ? O(271) C(27) 1.284(6) . ? O(272) C(27) 1.238(6) . ? N(1) C(16) 1.366(6) . ? N(1) C(12) 1.373(6) . ? N(21) C(22) 1.353(7) . ? N(21) C(26) 1.366(6) . ? C(11) C(116) 1.375(7) . ? C(11) C(112) 1.392(7) . ? C(12) C(13) 1.342(8) . ? C(12) C(17) 1.493(8) . ? C(13) C(14) 1.426(8) . ? C(14) C(15) 1.391(7) . ? C(15) C(16) 1.399(8) . ? C(22) C(23) 1.366(8) . ? C(22) C(27) 1.495(8) . ? C(23) C(24) 1.387(8) . ? C(24) C(25) 1.349(8) . ? C(25) C(26) 1.421(7) . ? C(112) C(113) 1.367(7) . ? C(113) C(114) 1.379(8) . ? C(114) C(115) 1.357(8) . ? C(115) C(116) 1.390(7) . ? C(121) C(122) 1.366(7) . ? C(121) C(126) 1.390(7) . ? C(122) C(123) 1.392(8) . ? C(123) C(124) 1.382(8) . ? C(124) C(125) 1.396(8) . ? C(125) C(126) 1.367(8) . ? C(211) C(212) 1.401(7) . ? C(211) C(216) 1.405(6) . ? C(212) C(213) 1.385(7) . ? C(213) C(214) 1.398(7) . ? C(214) C(215) 1.367(8) . ? C(215) C(216) 1.380(7) . ? C(221) C(226) 1.392(7) . ? C(221) C(222) 1.400(7) . ? C(222) C(223) 1.398(8) . ? C(223) C(224) 1.377(8) . ? C(224) C(225) 1.377(8) . ? C(225) C(226) 1.385(8) . ? C(311) C(312) 1.392(7) . ? C(311) C(316) 1.394(7) . ? C(312) C(313) 1.373(8) . ? C(313) C(314) 1.398(8) . ? C(314) C(315) 1.368(8) . ? C(315) C(316) 1.391(8) . ? C(321) C(322) 1.384(7) . ? C(321) C(326) 1.402(8) . ? C(322) C(323) 1.405(8) . ? C(323) C(324) 1.373(9) . ? C(324) C(325) 1.392(8) . ? C(325) C(326) 1.374(8) . ? C(411) C(412) 1.375(8) . ? C(411) C(416) 1.390(7) . ? C(412) C(413) 1.410(7) . ? C(413) C(414) 1.382(7) . ? C(414) C(415) 1.383(8) . ? C(415) C(416) 1.395(7) . ? C(421) C(426) 1.393(7) . ? C(421) C(422) 1.409(7) . ? C(422) C(423) 1.372(7) . ? C(423) C(424) 1.385(8) . ? C(424) C(425) 1.391(8) . ? C(425) C(426) 1.386(7) . ? 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 O(26) Re(1) N(1) 78.82(15) . . ? O(26) Re(1) O(171) 83.46(13) . . ? N(1) Re(1) O(171) 74.04(14) . . ? O(26) Re(1) Re(2) 94.08(9) . . ? N(1) Re(1) Re(2) 83.85(10) . . ? O(171) Re(1) Re(2) 157.82(11) . . ? O(26) Re(1) P(1) 165.59(11) . . ? N(1) Re(1) P(1) 89.04(11) . . ? O(171) Re(1) P(1) 85.77(10) . . ? Re(2) Re(1) P(1) 92.27(3) . . ? O(26) Re(1) P(3) 90.87(11) . . ? N(1) Re(1) P(3) 167.41(11) . . ? O(171) Re(1) P(3) 97.81(11) . . ? Re(2) Re(1) P(3) 104.28(3) . . ? P(1) Re(1) P(3) 100.08(5) . . ? O(16) Re(2) N(21) 80.17(15) . . ? O(16) Re(2) O(271) 84.39(14) . . ? N(21) Re(2) O(271) 73.74(14) . . ? O(16) Re(2) Re(1) 94.20(9) . . ? N(21) Re(2) Re(1) 84.73(11) . . ? O(271) Re(2) Re(1) 158.37(10) . . ? O(16) Re(2) P(4) 165.84(10) . . ? N(21) Re(2) P(4) 87.92(13) . . ? O(271) Re(2) P(4) 84.95(11) . . ? Re(1) Re(2) P(4) 92.28(3) . . ? O(16) Re(2) P(2) 90.97(10) . . ? N(21) Re(2) P(2) 167.87(12) . . ? O(271) Re(2) P(2) 97.30(10) . . ? Re(1) Re(2) P(2) 104.31(3) . . ? P(4) Re(2) P(2) 99.61(5) . . ? C(1B) P(1) C(121) 106.6(2) . . ? C(1B) P(1) C(11) 100.9(2) . . ? C(121) P(1) C(11) 98.2(2) . . ? C(1B) P(1) Re(1) 113.85(17) . . ? C(121) P(1) Re(1) 112.14(17) . . ? C(11) P(1) Re(1) 122.95(17) . . ? C(221) P(2) C(1B) 105.2(2) . . ? C(221) P(2) C(211) 99.9(2) . . ? C(1B) P(2) C(211) 103.2(2) . . ? C(221) P(2) Re(2) 117.32(19) . . ? C(1B) P(2) Re(2) 107.21(17) . . ? C(211) P(2) Re(2) 122.17(17) . . ? C(2B) P(3) C(321) 103.7(2) . . ? C(2B) P(3) C(311) 103.1(2) . . ? C(321) P(3) C(311) 99.9(2) . . ? C(2B) P(3) Re(1) 107.97(18) . . ? C(321) P(3) Re(1) 116.78(19) . . ? C(311) P(3) Re(1) 123.15(19) . . ? C(421) P(4) C(411) 98.6(2) . . ? C(421) P(4) C(2B) 105.3(2) . . ? C(411) P(4) C(2B) 101.1(2) . . ? C(421) P(4) Re(2) 111.68(18) . . ? C(411) P(4) Re(2) 122.73(18) . . ? C(2B) P(4) Re(2) 115.02(18) . . ? C(16) O(16) Re(2) 115.3(3) . . ? C(26) O(26) Re(1) 116.5(3) . . ? C(17) O(171) Re(1) 117.2(3) . . ? C(27) O(271) Re(2) 118.6(3) . . ? C(16) N(1) C(12) 118.9(5) . . ? C(16) N(1) Re(1) 124.1(3) . . ? C(12) N(1) Re(1) 116.1(3) . . ? C(22) N(21) C(26) 120.7(4) . . ? C(22) N(21) Re(2) 117.0(3) . . ? C(26) N(21) Re(2) 122.2(3) . . ? C(116) C(11) C(112) 118.2(5) . . ? C(116) C(11) P(1) 121.4(4) . . ? C(112) C(11) P(1) 120.1(4) . . ? C(13) C(12) N(1) 122.8(5) . . ? C(13) C(12) C(17) 124.2(5) . . ? N(1) C(12) C(17) 112.9(5) . . ? C(12) C(13) C(14) 119.6(5) . . ? C(15) C(14) C(13) 117.8(5) . . ? C(14) C(15) C(16) 120.2(5) . . ? O(16) C(16) N(1) 117.2(5) . . ? O(16) C(16) C(15) 122.3(5) . . ? N(1) C(16) C(15) 120.5(5) . . ? O(172) C(17) O(171) 124.3(5) . . ? O(172) C(17) C(12) 119.1(5) . . ? O(171) C(17) C(12) 116.5(4) . . ? P(1) C(1B) P(2) 113.1(3) . . ? N(21) C(22) C(23) 121.4(5) . . ? N(21) C(22) C(27) 114.1(5) . . ? C(23) C(22) C(27) 124.4(5) . . ? C(22) C(23) C(24) 118.6(6) . . ? C(25) C(24) C(23) 121.2(6) . . ? C(24) C(25) C(26) 119.3(6) . . ? O(26) C(26) N(21) 119.4(4) . . ? O(26) C(26) C(25) 121.9(5) . . ? N(21) C(26) C(25) 118.7(5) . . ? O(272) C(27) O(271) 124.6(5) . . ? O(272) C(27) C(22) 120.1(5) . . ? O(271) C(27) C(22) 115.3(5) . . ? P(3) C(2B) P(4) 112.4(3) . . ? C(113) C(112) C(11) 120.7(5) . . ? C(112) C(113) C(114) 120.8(5) . . ? C(115) C(114) C(113) 118.8(5) . . ? C(114) C(115) C(116) 121.1(5) . . ? C(11) C(116) C(115) 120.2(5) . . ? C(122) C(121) C(126) 119.5(5) . . ? C(122) C(121) P(1) 123.0(4) . . ? C(126) C(121) P(1) 117.4(4) . . ? C(121) C(122) C(123) 120.0(5) . . ? C(124) C(123) C(122) 120.8(6) . . ? C(123) C(124) C(125) 118.6(6) . . ? C(126) C(125) C(124) 120.3(6) . . ? C(125) C(126) C(121) 120.8(5) . . ? C(212) C(211) C(216) 118.2(5) . . ? C(212) C(211) P(2) 120.6(4) . . ? C(216) C(211) P(2) 121.2(4) . . ? C(213) C(212) C(211) 121.0(5) . . ? C(212) C(213) C(214) 119.8(6) . . ? C(215) C(214) C(213) 119.4(5) . . ? C(214) C(215) C(216) 121.7(5) . . ? C(215) C(216) C(211) 120.0(5) . . ? C(226) C(221) C(222) 119.4(5) . . ? C(226) C(221) P(2) 122.3(4) . . ? C(222) C(221) P(2) 118.3(4) . . ? C(223) C(222) C(221) 119.5(5) . . ? C(224) C(223) C(222) 120.5(6) . . ? C(223) C(224) C(225) 119.8(6) . . ? C(224) C(225) C(226) 120.9(6) . . ? C(225) C(226) C(221) 119.9(6) . . ? C(312) C(311) C(316) 118.3(5) . . ? C(312) C(311) P(3) 122.0(4) . . ? C(316) C(311) P(3) 119.4(4) . . ? C(313) C(312) C(311) 121.8(5) . . ? C(312) C(313) C(314) 119.3(6) . . ? C(315) C(314) C(313) 119.7(6) . . ? C(314) C(315) C(316) 121.0(5) . . ? C(315) C(316) C(311) 119.9(5) . . ? C(322) C(321) C(326) 118.6(5) . . ? C(322) C(321) P(3) 121.1(4) . . ? C(326) C(321) P(3) 120.3(4) . . ? C(321) C(322) C(323) 119.3(6) . . ? C(324) C(323) C(322) 121.1(6) . . ? C(323) C(324) C(325) 120.0(5) . . ? C(326) C(325) C(324) 119.0(6) . . ? C(325) C(326) C(321) 122.0(5) . . ? C(412) C(411) C(416) 119.7(5) . . ? C(412) C(411) P(4) 119.8(4) . . ? C(416) C(411) P(4) 120.5(4) . . ? C(411) C(412) C(413) 120.4(5) . . ? C(414) C(413) C(412) 119.6(5) . . ? C(413) C(414) C(415) 119.9(5) . . ? C(414) C(415) C(416) 120.3(5) . . ? C(411) C(416) C(415) 120.1(5) . . ? C(426) C(421) C(422) 117.9(5) . . ? C(426) C(421) P(4) 118.7(4) . . ? C(422) C(421) P(4) 122.9(4) . . ? C(423) C(422) C(421) 120.9(5) . . ? C(422) C(423) C(424) 120.9(5) . . ? C(423) C(424) C(425) 118.9(5) . . ? C(426) C(425) C(424) 120.6(5) . . ? C(425) C(426) C(421) 120.7(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O(26) Re(1) Re(2) O(16) 89.06(14) . . . . ? N(1) Re(1) Re(2) O(16) 10.79(14) . . . . ? O(171) Re(1) Re(2) O(16) 6.4(3) . . . . ? P(1) Re(1) Re(2) O(16) -77.99(10) . . . . ? P(3) Re(1) Re(2) O(16) -178.99(10) . . . . ? O(26) Re(1) Re(2) N(21) 9.36(16) . . . . ? N(1) Re(1) Re(2) N(21) -68.91(16) . . . . ? O(171) Re(1) Re(2) N(21) -73.3(3) . . . . ? P(1) Re(1) Re(2) N(21) -157.70(13) . . . . ? P(3) Re(1) Re(2) N(21) 101.30(13) . . . . ? O(26) Re(1) Re(2) O(271) 3.7(3) . . . . ? N(1) Re(1) Re(2) O(271) -74.6(3) . . . . ? O(171) Re(1) Re(2) O(271) -79.0(4) . . . . ? P(1) Re(1) Re(2) O(271) -163.4(3) . . . . ? P(3) Re(1) Re(2) O(271) 95.6(3) . . . . ? O(26) Re(1) Re(2) P(4) -78.34(11) . . . . ? N(1) Re(1) Re(2) P(4) -156.61(11) . . . . ? O(171) Re(1) Re(2) P(4) -161.0(3) . . . . ? P(1) Re(1) Re(2) P(4) 114.60(5) . . . . ? P(3) Re(1) Re(2) P(4) 13.61(5) . . . . ? O(26) Re(1) Re(2) P(2) -178.86(11) . . . . ? N(1) Re(1) Re(2) P(2) 102.87(12) . . . . ? O(171) Re(1) Re(2) P(2) 98.5(3) . . . . ? P(1) Re(1) Re(2) P(2) 14.08(5) . . . . ? P(3) Re(1) Re(2) P(2) -86.92(5) . . . . ? O(26) Re(1) P(1) C(1B) -144.8(4) . . . . ? N(1) Re(1) P(1) C(1B) -112.5(2) . . . . ? O(171) Re(1) P(1) C(1B) 173.5(2) . . . . ? Re(2) Re(1) P(1) C(1B) -28.7(2) . . . . ? P(3) Re(1) P(1) C(1B) 76.3(2) . . . . ? O(26) Re(1) P(1) C(121) -23.6(4) . . . . ? N(1) Re(1) P(1) C(121) 8.7(2) . . . . ? O(171) Re(1) P(1) C(121) -65.4(2) . . . . ? Re(2) Re(1) P(1) C(121) 92.52(18) . . . . ? P(3) Re(1) P(1) C(121) -162.54(18) . . . . ? O(26) Re(1) P(1) C(11) 92.9(4) . . . . ? N(1) Re(1) P(1) C(11) 125.3(2) . . . . ? O(171) Re(1) P(1) C(11) 51.2(2) . . . . ? Re(2) Re(1) P(1) C(11) -150.9(2) . . . . ? P(3) Re(1) P(1) C(11) -46.0(2) . . . . ? O(16) Re(2) P(2) C(221) -23.2(2) . . . . ? N(21) Re(2) P(2) C(221) 19.6(6) . . . . ? O(271) Re(2) P(2) C(221) 61.3(2) . . . . ? Re(1) Re(2) P(2) C(221) -117.80(18) . . . . ? P(4) Re(2) P(2) C(221) 147.34(18) . . . . ? O(16) Re(2) P(2) C(1B) 94.8(2) . . . . ? N(21) Re(2) P(2) C(1B) 137.6(6) . . . . ? O(271) Re(2) P(2) C(1B) 179.3(2) . . . . ? Re(1) Re(2) P(2) C(1B) 0.2(2) . . . . ? P(4) Re(2) P(2) C(1B) -94.7(2) . . . . ? O(16) Re(2) P(2) C(211) -146.8(2) . . . . ? N(21) Re(2) P(2) C(211) -104.0(6) . . . . ? O(271) Re(2) P(2) C(211) -62.3(2) . . . . ? Re(1) Re(2) P(2) C(211) 118.6(2) . . . . ? P(4) Re(2) P(2) C(211) 23.8(2) . . . . ? O(26) Re(1) P(3) C(2B) 94.0(2) . . . . ? N(1) Re(1) P(3) C(2B) 128.8(5) . . . . ? O(171) Re(1) P(3) C(2B) 177.5(2) . . . . ? Re(2) Re(1) P(3) C(2B) -0.44(18) . . . . ? P(1) Re(1) P(3) C(2B) -95.42(18) . . . . ? O(26) Re(1) P(3) C(321) -22.2(2) . . . . ? N(1) Re(1) P(3) C(321) 12.6(6) . . . . ? O(171) Re(1) P(3) C(321) 61.3(2) . . . . ? Re(2) Re(1) P(3) C(321) -116.65(19) . . . . ? P(1) Re(1) P(3) C(321) 148.37(19) . . . . ? O(26) Re(1) P(3) C(311) -146.3(2) . . . . ? N(1) Re(1) P(3) C(311) -111.5(5) . . . . ? O(171) Re(1) P(3) C(311) -62.8(2) . . . . ? Re(2) Re(1) P(3) C(311) 119.3(2) . . . . ? P(1) Re(1) P(3) C(311) 24.3(2) . . . . ? O(16) Re(2) P(4) C(421) -24.5(4) . . . . ? N(21) Re(2) P(4) C(421) 8.1(2) . . . . ? O(271) Re(2) P(4) C(421) -65.8(2) . . . . ? Re(1) Re(2) P(4) C(421) 92.74(18) . . . . ? P(2) Re(2) P(4) C(421) -162.33(18) . . . . ? O(16) Re(2) P(4) C(411) 92.0(4) . . . . ? N(21) Re(2) P(4) C(411) 124.6(2) . . . . ? O(271) Re(2) P(4) C(411) 50.7(2) . . . . ? Re(1) Re(2) P(4) C(411) -150.8(2) . . . . ? P(2) Re(2) P(4) C(411) -45.9(2) . . . . ? O(16) Re(2) P(4) C(2B) -144.4(4) . . . . ? N(21) Re(2) P(4) C(2B) -111.8(2) . . . . ? O(271) Re(2) P(4) C(2B) 174.3(2) . . . . ? Re(1) Re(2) P(4) C(2B) -27.18(18) . . . . ? P(2) Re(2) P(4) C(2B) 77.75(18) . . . . ? N(21) Re(2) O(16) C(16) 60.6(3) . . . . ? O(271) Re(2) O(16) C(16) 135.0(3) . . . . ? Re(1) Re(2) O(16) C(16) -23.4(3) . . . . ? P(4) Re(2) O(16) C(16) 93.7(5) . . . . ? P(2) Re(2) O(16) C(16) -127.8(3) . . . . ? N(1) Re(1) O(26) C(26) 64.8(4) . . . . ? O(171) Re(1) O(26) C(26) 139.7(4) . . . . ? Re(2) Re(1) O(26) C(26) -18.1(4) . . . . ? P(1) Re(1) O(26) C(26) 97.8(5) . . . . ? P(3) Re(1) O(26) C(26) -122.5(4) . . . . ? O(26) Re(1) O(171) C(17) -65.9(4) . . . . ? N(1) Re(1) O(171) C(17) 14.3(4) . . . . ? Re(2) Re(1) O(171) C(17) 18.9(6) . . . . ? P(1) Re(1) O(171) C(17) 104.5(4) . . . . ? P(3) Re(1) O(171) C(17) -155.9(4) . . . . ? O(16) Re(2) O(271) C(27) -71.3(4) . . . . ? N(21) Re(2) O(271) C(27) 10.1(4) . . . . ? Re(1) Re(2) O(271) C(27) 16.0(6) . . . . ? P(4) Re(2) O(271) C(27) 99.4(4) . . . . ? P(2) Re(2) O(271) C(27) -161.6(4) . . . . ? O(26) Re(1) N(1) C(16) -98.2(4) . . . . ? O(171) Re(1) N(1) C(16) 175.5(4) . . . . ? Re(2) Re(1) N(1) C(16) -2.8(4) . . . . ? P(1) Re(1) N(1) C(16) 89.6(4) . . . . ? P(3) Re(1) N(1) C(16) -133.7(4) . . . . ? O(26) Re(1) N(1) C(12) 70.5(4) . . . . ? O(171) Re(1) N(1) C(12) -15.8(3) . . . . ? Re(2) Re(1) N(1) C(12) 165.9(4) . . . . ? P(1) Re(1) N(1) C(12) -101.7(4) . . . . ? P(3) Re(1) N(1) C(12) 35.0(8) . . . . ? O(16) Re(2) N(21) C(22) 77.2(4) . . . . ? O(271) Re(2) N(21) C(22) -9.8(4) . . . . ? Re(1) Re(2) N(21) C(22) 172.4(4) . . . . ? P(4) Re(2) N(21) C(22) -95.1(4) . . . . ? P(2) Re(2) N(21) C(22) 33.6(9) . . . . ? O(16) Re(2) N(21) C(26) -99.7(4) . . . . ? O(271) Re(2) N(21) C(26) 173.3(5) . . . . ? Re(1) Re(2) N(21) C(26) -4.5(4) . . . . ? P(4) Re(2) N(21) C(26) 88.0(4) . . . . ? P(2) Re(2) N(21) C(26) -143.3(5) . . . . ? C(1B) P(1) C(11) C(116) -151.8(5) . . . . ? C(121) P(1) C(11) C(116) 99.4(5) . . . . ? Re(1) P(1) C(11) C(116) -23.8(5) . . . . ? C(1B) P(1) C(11) C(112) 34.6(5) . . . . ? C(121) P(1) C(11) C(112) -74.2(5) . . . . ? Re(1) P(1) C(11) C(112) 162.6(4) . . . . ? C(16) N(1) C(12) C(13) 3.1(8) . . . . ? Re(1) N(1) C(12) C(13) -166.2(5) . . . . ? C(16) N(1) C(12) C(17) -175.2(5) . . . . ? Re(1) N(1) C(12) C(17) 15.5(6) . . . . ? N(1) C(12) C(13) C(14) 0.5(9) . . . . ? C(17) C(12) C(13) C(14) 178.7(5) . . . . ? C(12) C(13) C(14) C(15) -3.5(9) . . . . ? C(13) C(14) C(15) C(16) 2.9(9) . . . . ? Re(2) O(16) C(16) N(1) 25.3(6) . . . . ? Re(2) O(16) C(16) C(15) -153.6(4) . . . . ? C(12) N(1) C(16) O(16) 177.3(4) . . . . ? Re(1) N(1) C(16) O(16) -14.3(6) . . . . ? C(12) N(1) C(16) C(15) -3.8(8) . . . . ? Re(1) N(1) C(16) C(15) 164.6(4) . . . . ? C(14) C(15) C(16) O(16) 179.6(5) . . . . ? C(14) C(15) C(16) N(1) 0.8(8) . . . . ? Re(1) O(171) C(17) O(172) 172.1(4) . . . . ? Re(1) O(171) C(17) C(12) -10.8(6) . . . . ? C(13) C(12) C(17) O(172) -4.1(9) . . . . ? N(1) C(12) C(17) O(172) 174.2(5) . . . . ? C(13) C(12) C(17) O(171) 178.6(5) . . . . ? N(1) C(12) C(17) O(171) -3.1(7) . . . . ? C(121) P(1) C(1B) P(2) -90.3(3) . . . . ? C(11) P(1) C(1B) P(2) 167.6(3) . . . . ? Re(1) P(1) C(1B) P(2) 33.9(3) . . . . ? C(221) P(2) C(1B) P(1) 105.1(3) . . . . ? C(211) P(2) C(1B) P(1) -150.6(3) . . . . ? Re(2) P(2) C(1B) P(1) -20.5(3) . . . . ? C(26) N(21) C(22) C(23) 2.6(9) . . . . ? Re(2) N(21) C(22) C(23) -174.3(5) . . . . ? C(26) N(21) C(22) C(27) -174.3(5) . . . . ? Re(2) N(21) C(22) C(27) 8.7(7) . . . . ? N(21) C(22) C(23) C(24) -1.3(10) . . . . ? C(27) C(22) C(23) C(24) 175.3(6) . . . . ? C(22) C(23) C(24) C(25) 0.5(11) . . . . ? C(23) C(24) C(25) C(26) -0.9(11) . . . . ? Re(1) O(26) C(26) N(21) 18.3(7) . . . . ? Re(1) O(26) C(26) C(25) -163.7(4) . . . . ? C(22) N(21) C(26) O(26) 175.0(5) . . . . ? Re(2) N(21) C(26) O(26) -8.2(7) . . . . ? C(22) N(21) C(26) C(25) -3.0(8) . . . . ? Re(2) N(21) C(26) C(25) 173.8(4) . . . . ? C(24) C(25) C(26) O(26) -175.8(6) . . . . ? C(24) C(25) C(26) N(21) 2.1(9) . . . . ? Re(2) O(271) C(27) O(272) 173.0(5) . . . . ? Re(2) O(271) C(27) C(22) -8.7(7) . . . . ? N(21) C(22) C(27) O(272) 178.3(6) . . . . ? C(23) C(22) C(27) O(272) 1.4(10) . . . . ? N(21) C(22) C(27) O(271) -0.1(8) . . . . ? C(23) C(22) C(27) O(271) -176.9(6) . . . . ? C(321) P(3) C(2B) P(4) 106.2(3) . . . . ? C(311) P(3) C(2B) P(4) -150.0(3) . . . . ? Re(1) P(3) C(2B) P(4) -18.3(3) . . . . ? C(421) P(4) C(2B) P(3) -92.0(3) . . . . ? C(411) P(4) C(2B) P(3) 165.9(3) . . . . ? Re(2) P(4) C(2B) P(3) 31.4(3) . . . . ? C(116) C(11) C(112) C(113) 0.9(9) . . . . ? P(1) C(11) C(112) C(113) 174.7(5) . . . . ? C(11) C(112) C(113) C(114) -1.6(10) . . . . ? C(112) C(113) C(114) C(115) 1.7(10) . . . . ? C(113) C(114) C(115) C(116) -1.2(10) . . . . ? C(112) C(11) C(116) C(115) -0.4(9) . . . . ? P(1) C(11) C(116) C(115) -174.1(5) . . . . ? C(114) C(115) C(116) C(11) 0.6(10) . . . . ? C(1B) P(1) C(121) C(122) 27.3(5) . . . . ? C(11) P(1) C(121) C(122) 131.4(5) . . . . ? Re(1) P(1) C(121) C(122) -98.0(5) . . . . ? C(1B) P(1) C(121) C(126) -155.7(4) . . . . ? C(11) P(1) C(121) C(126) -51.6(5) . . . . ? Re(1) P(1) C(121) C(126) 79.1(4) . . . . ? C(126) C(121) C(122) C(123) 0.7(9) . . . . ? P(1) C(121) C(122) C(123) 177.7(5) . . . . ? C(121) C(122) C(123) C(124) -1.5(10) . . . . ? C(122) C(123) C(124) C(125) 1.1(10) . . . . ? C(123) C(124) C(125) C(126) 0.1(9) . . . . ? C(124) C(125) C(126) C(121) -0.8(9) . . . . ? C(122) C(121) C(126) C(125) 0.4(8) . . . . ? P(1) C(121) C(126) C(125) -176.7(4) . . . . ? C(221) P(2) C(211) C(212) 158.0(4) . . . . ? C(1B) P(2) C(211) C(212) 49.7(5) . . . . ? Re(2) P(2) C(211) C(212) -70.7(4) . . . . ? C(221) P(2) C(211) C(216) -24.5(5) . . . . ? C(1B) P(2) C(211) C(216) -132.8(4) . . . . ? Re(2) P(2) C(211) C(216) 106.8(4) . . . . ? C(216) C(211) C(212) C(213) -1.9(8) . . . . ? P(2) C(211) C(212) C(213) 175.6(4) . . . . ? C(211) C(212) C(213) C(214) 2.0(8) . . . . ? C(212) C(213) C(214) C(215) -1.3(9) . . . . ? C(213) C(214) C(215) C(216) 0.5(9) . . . . ? C(214) C(215) C(216) C(211) -0.4(8) . . . . ? C(212) C(211) C(216) C(215) 1.0(7) . . . . ? P(2) C(211) C(216) C(215) -176.5(4) . . . . ? C(1B) P(2) C(221) C(226) 36.8(5) . . . . ? C(211) P(2) C(221) C(226) -69.8(5) . . . . ? Re(2) P(2) C(221) C(226) 155.9(4) . . . . ? C(1B) P(2) C(221) C(222) -145.4(4) . . . . ? C(211) P(2) C(221) C(222) 107.9(4) . . . . ? Re(2) P(2) C(221) C(222) -26.4(5) . . . . ? C(226) C(221) C(222) C(223) -1.5(8) . . . . ? P(2) C(221) C(222) C(223) -179.3(4) . . . . ? C(221) C(222) C(223) C(224) -0.1(8) . . . . ? C(222) C(223) C(224) C(225) 0.9(9) . . . . ? C(223) C(224) C(225) C(226) 0.1(9) . . . . ? C(224) C(225) C(226) C(221) -1.7(9) . . . . ? C(222) C(221) C(226) C(225) 2.5(8) . . . . ? P(2) C(221) C(226) C(225) -179.9(4) . . . . ? C(2B) P(3) C(311) C(312) 45.4(5) . . . . ? C(321) P(3) C(311) C(312) 152.1(5) . . . . ? Re(1) P(3) C(311) C(312) -76.6(5) . . . . ? C(2B) P(3) C(311) C(316) -141.0(5) . . . . ? C(321) P(3) C(311) C(316) -34.3(5) . . . . ? Re(1) P(3) C(311) C(316) 97.0(5) . . . . ? C(316) C(311) C(312) C(313) 2.6(9) . . . . ? P(3) C(311) C(312) C(313) 176.2(5) . . . . ? C(311) C(312) C(313) C(314) -2.1(10) . . . . ? C(312) C(313) C(314) C(315) 0.9(11) . . . . ? C(313) C(314) C(315) C(316) -0.2(11) . . . . ? C(314) C(315) C(316) C(311) 0.7(10) . . . . ? C(312) C(311) C(316) C(315) -1.9(9) . . . . ? P(3) C(311) C(316) C(315) -175.7(5) . . . . ? C(2B) P(3) C(321) C(322) -142.4(4) . . . . ? C(311) P(3) C(321) C(322) 111.4(5) . . . . ? Re(1) P(3) C(321) C(322) -23.9(5) . . . . ? C(2B) P(3) C(321) C(326) 37.2(5) . . . . ? C(311) P(3) C(321) C(326) -69.0(5) . . . . ? Re(1) P(3) C(321) C(326) 155.7(4) . . . . ? C(326) C(321) C(322) C(323) -1.9(8) . . . . ? P(3) C(321) C(322) C(323) 177.8(4) . . . . ? C(321) C(322) C(323) C(324) 0.9(9) . . . . ? C(322) C(323) C(324) C(325) -0.5(9) . . . . ? C(323) C(324) C(325) C(326) 1.2(9) . . . . ? C(324) C(325) C(326) C(321) -2.3(9) . . . . ? C(322) C(321) C(326) C(325) 2.7(8) . . . . ? P(3) C(321) C(326) C(325) -177.0(4) . . . . ? C(421) P(4) C(411) C(412) -74.8(5) . . . . ? C(2B) P(4) C(411) C(412) 32.7(5) . . . . ? Re(2) P(4) C(411) C(412) 162.5(4) . . . . ? C(421) P(4) C(411) C(416) 102.9(4) . . . . ? C(2B) P(4) C(411) C(416) -149.6(4) . . . . ? Re(2) P(4) C(411) C(416) -19.8(5) . . . . ? C(416) C(411) C(412) C(413) 0.1(8) . . . . ? P(4) C(411) C(412) C(413) 177.9(4) . . . . ? C(411) C(412) C(413) C(414) 1.1(9) . . . . ? C(412) C(413) C(414) C(415) -2.3(8) . . . . ? C(413) C(414) C(415) C(416) 2.2(8) . . . . ? C(412) C(411) C(416) C(415) -0.2(8) . . . . ? P(4) C(411) C(416) C(415) -177.9(4) . . . . ? C(414) C(415) C(416) C(411) -0.9(8) . . . . ? C(411) P(4) C(421) C(426) -43.2(5) . . . . ? C(2B) P(4) C(421) C(426) -147.3(4) . . . . ? Re(2) P(4) C(421) C(426) 87.2(4) . . . . ? C(411) P(4) C(421) C(422) 144.0(5) . . . . ? C(2B) P(4) C(421) C(422) 39.9(5) . . . . ? Re(2) P(4) C(421) C(422) -85.6(5) . . . . ? C(426) C(421) C(422) C(423) 0.5(8) . . . . ? P(4) C(421) C(422) C(423) 173.4(5) . . . . ? C(421) C(422) C(423) C(424) -0.4(9) . . . . ? C(422) C(423) C(424) C(425) 0.0(9) . . . . ? C(423) C(424) C(425) C(426) 0.3(10) . . . . ? C(424) C(425) C(426) C(421) -0.1(10) . . . . ? C(422) C(421) C(426) C(425) -0.3(9) . . . . ? P(4) C(421) C(426) C(425) -173.4(5) . . . . ? #===END #============================================================================== data_SWCH15 _database_code_CSD 212138 _audit_creation_date 5-05-03 _audit_creation_method from_MolEN_and_SHELXL _audit_update_record ; ? ; # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description chunk _exptl_crystal_colour 'dark orange' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.25 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C62 H50 N2 O7 P4 Re2' _chemical_formula_moiety 'C62 H50 N2 O6 P4 Re2,H2 O1' _chemical_formula_structural ? _chemical_formula_weight 1431.40 _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 12.1609(2) _cell_length_b 21.3705(4) _cell_length_c 23.4450(5) _cell_angle_alpha 90.00 _cell_angle_beta 104.8157(10) _cell_angle_gamma 90.00 _cell_volume 5890.42(19) _cell_measurement_reflns_used 44542 _cell_measurement_theta_min 2 _cell_measurement_theta_max 27 _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.61 _exptl_crystal_density_meas ? _diffrn_radiation_type MO-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 4.320 _cell_measurement_temperature 150 _exptl_crystal_F_000 2816 # 6. DATA COLLECTION _diffrn_ambient_temperature 150 _diffrn_measurement_device_type Nonius_KappaCCD _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan_(Otwinowski_&_Minor,_ _exptl_absorpt_correction_T_min 0.2374 _exptl_absorpt_correction_T_max 0.3396 _diffrn_reflns_number 44542 _diffrn_measured_fraction_theta_max 0.8568 _diffrn_reflns_theta_full 15.9 _diffrn_measured_fraction_theta_full 0.9580 _reflns_number_total 13920 _reflns_number_gt 11304 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.056 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 27.89 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_max 29 _diffrn_special_details 'mosaicity from Denzo/Scalepack is 1.26' # 7. REFINEMENT DATA _refine_special_details ; Residual electron density was adjusted using the SQUEEZE option in program PLATON (Spek, 1997). 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 0.040 _refine_ls_wR_factor_ref 0.084 _refine_ls_hydrogen_treatment H_atoms_riding _refine_ls_number_reflns 13840 _refine_ls_number_parameters 694 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 0.951 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details '1/[\s^2^(Fo^2^)+(0.0488P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3 ' _refine_ls_shift/su_max 0.002 _refine_diff_density_max 1.52 _refine_diff_density_min -2.12 _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) PLATON (Spek, 1997) ; _computing_publication_material CIF_VAX_MolEN_(Fair,_1990) # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re(1) Re 0.289975(16) 0.259500(9) 0.360507(8) 0.02084(6) Uani 1 1 d . . . Re(5B) Re 0.140019(15) 0.221518(8) 0.394355(8) 0.02032(6) Uani 1 1 d . . . P(1) P 0.39131(10) 0.16725(6) 0.34431(6) 0.0232(3) Uani 1 1 d . . . P(2) P 0.22285(10) 0.11969(6) 0.41196(6) 0.0219(3) Uani 1 1 d . . . P(3) P 0.17251(10) 0.27383(6) 0.26293(6) 0.0221(3) Uani 1 1 d . . . P(4) P -0.00810(10) 0.20123(6) 0.30601(5) 0.0224(3) Uani 1 1 d . . . O(12) O 0.0717(3) 0.31098(15) 0.40165(14) 0.0271(8) Uani 1 1 d . . . O(1W) O 0.0425(4) 0.06634(18) 0.1332(2) 0.0566(12) Uani 1 1 d . . . O(22) O 0.3999(3) 0.27095(15) 0.44589(15) 0.0257(8) Uani 1 1 d . . . O(171) O 0.4021(3) 0.32981(16) 0.33492(16) 0.0319(8) Uani 1 1 d . . . O(172) O 0.4659(4) 0.4275(2) 0.3464(2) 0.0579(13) Uani 1 1 d . . . O(271) O 0.0456(3) 0.19554(15) 0.45805(14) 0.0251(7) Uani 1 1 d . . . O(272) O 0.0246(3) 0.21513(19) 0.54860(17) 0.0426(10) Uani 1 1 d . . . N(11) N 0.2341(4) 0.35024(18) 0.38308(18) 0.0263(9) Uani 1 1 d . . . N(21) N 0.2433(3) 0.25100(17) 0.47997(17) 0.0214(8) Uani 1 1 d . . . C(12) C 0.1401(4) 0.3575(2) 0.4028(2) 0.0258(11) Uani 1 1 d . . . C(13) C 0.1144(5) 0.4177(2) 0.4233(3) 0.0404(14) Uani 1 1 d . . . C(14) C 0.1847(6) 0.4664(3) 0.4211(3) 0.0496(17) Uani 1 1 d . . . C(15) C 0.2809(6) 0.4585(3) 0.3998(3) 0.0468(16) Uani 1 1 d . . . C(16) C 0.3018(5) 0.4003(2) 0.3810(2) 0.0335(13) Uani 1 1 d . . . C(17) C 0.3974(5) 0.3856(3) 0.3529(2) 0.0398(14) Uani 1 1 d . . . C(1B) C 0.3148(4) 0.0994(2) 0.3632(2) 0.0258(11) Uani 1 1 d . . . C(22) C 0.3484(4) 0.2761(2) 0.4878(2) 0.0265(11) Uani 1 1 d . . . C(23) C 0.3976(4) 0.3081(2) 0.5408(2) 0.0314(12) Uani 1 1 d . . . C(24) C 0.3398(5) 0.3133(3) 0.5841(2) 0.0353(13) Uani 1 1 d . . . C(25) C 0.2332(4) 0.2839(2) 0.5755(2) 0.0327(12) Uani 1 1 d . . . C(26) C 0.1882(4) 0.2541(2) 0.5237(2) 0.0254(11) Uani 1 1 d . . . C(27) C 0.0763(4) 0.2202(2) 0.5103(2) 0.0268(11) Uani 1 1 d . . . C(2B) C 0.0483(4) 0.2214(2) 0.2429(2) 0.0264(11) Uani 1 1 d . . . C(111) C 0.5378(4) 0.1590(2) 0.3888(2) 0.0272(11) Uani 1 1 d . . . C(112) C 0.5999(4) 0.2132(3) 0.4107(2) 0.0319(12) Uani 1 1 d . . . C(113) C 0.7129(4) 0.2075(3) 0.4433(2) 0.0352(13) Uani 1 1 d . . . C(114) C 0.7635(5) 0.1496(3) 0.4554(2) 0.0394(14) Uani 1 1 d . . . C(115) C 0.7020(4) 0.0965(3) 0.4334(3) 0.0414(15) Uani 1 1 d . . . C(116) C 0.5915(4) 0.1006(3) 0.4001(2) 0.0340(13) Uani 1 1 d . . . C(121) C 0.4098(4) 0.1459(2) 0.2711(2) 0.0263(11) Uani 1 1 d . . . C(122) C 0.5157(4) 0.1530(2) 0.2584(2) 0.0307(12) Uani 1 1 d . . . C(123) C 0.5277(5) 0.1392(3) 0.2020(2) 0.0349(13) Uani 1 1 d . . . C(124) C 0.4369(5) 0.1195(2) 0.1587(3) 0.0380(14) Uani 1 1 d . . . C(125) C 0.3311(5) 0.1131(2) 0.1701(2) 0.0336(12) Uani 1 1 d . . . C(126) C 0.3175(4) 0.1258(2) 0.2259(2) 0.0287(11) Uani 1 1 d . . . C(211) C 0.1375(4) 0.0480(2) 0.4076(2) 0.0260(11) Uani 1 1 d . . . C(212) C 0.1863(5) -0.0104(2) 0.4027(3) 0.0356(13) Uani 1 1 d . . . C(213) C 0.1262(5) -0.0655(2) 0.4038(3) 0.0408(14) Uani 1 1 d . . . C(214) C 0.0160(5) -0.0623(3) 0.4113(3) 0.0433(15) Uani 1 1 d . . . C(215) C -0.0312(5) -0.0050(3) 0.4172(3) 0.0394(14) Uani 1 1 d . . . C(216) C 0.0289(4) 0.0506(2) 0.4152(2) 0.0316(12) Uani 1 1 d . . . C(221) C 0.3101(4) 0.1107(2) 0.4884(2) 0.0256(11) Uani 1 1 d . . . C(222) C 0.4265(5) 0.1182(3) 0.5047(2) 0.0371(13) Uani 1 1 d . . . C(223) C 0.4857(5) 0.1130(3) 0.5639(3) 0.0482(16) Uani 1 1 d . . . C(224) C 0.4298(5) 0.1015(3) 0.6068(3) 0.0458(16) Uani 1 1 d . . . C(225) C 0.3118(5) 0.0945(3) 0.5904(3) 0.0426(14) Uani 1 1 d . . . C(226) C 0.2528(5) 0.0988(2) 0.5317(2) 0.0338(12) Uani 1 1 d . . . C(311) C 0.2278(4) 0.2678(2) 0.1969(2) 0.0243(10) Uani 1 1 d . . . C(312) C 0.1532(5) 0.2587(3) 0.1415(2) 0.0353(13) Uani 1 1 d . . . C(313) C 0.1944(5) 0.2554(3) 0.0914(2) 0.0382(14) Uani 1 1 d . . . C(314) C 0.3091(4) 0.2626(2) 0.0962(2) 0.0312(12) Uani 1 1 d . . . C(315) C 0.3830(4) 0.2735(2) 0.1512(2) 0.0289(11) Uani 1 1 d . . . C(316) C 0.3436(4) 0.2760(2) 0.2016(2) 0.0275(11) Uani 1 1 d . . . C(321) C 0.1160(4) 0.3544(2) 0.2526(2) 0.0257(11) Uani 1 1 d . . . C(322) C 0.0176(4) 0.3722(2) 0.2690(2) 0.0288(11) Uani 1 1 d . . . C(323) C -0.0160(4) 0.4343(2) 0.2653(2) 0.0312(12) Uani 1 1 d . . . C(324) C 0.0486(5) 0.4795(2) 0.2469(2) 0.0343(13) Uani 1 1 d . . . C(325) C 0.1460(5) 0.4625(2) 0.2314(3) 0.0387(14) Uani 1 1 d . . . C(326) C 0.1800(5) 0.4005(2) 0.2334(2) 0.0341(13) Uani 1 1 d . . . C(411) C -0.0699(4) 0.1229(2) 0.2870(2) 0.0295(12) Uani 1 1 d . . . C(412) C -0.0130(5) 0.0769(2) 0.2647(3) 0.0372(13) Uani 1 1 d . . . C(413) C -0.0596(5) 0.0172(3) 0.2526(3) 0.0513(18) Uani 1 1 d . . . C(414) C -0.1622(5) 0.0031(3) 0.2650(3) 0.057(2) Uani 1 1 d . . . C(415) C -0.2187(5) 0.0487(3) 0.2879(3) 0.0502(17) Uani 1 1 d . . . C(416) C -0.1737(4) 0.1083(3) 0.2987(3) 0.0379(14) Uani 1 1 d . . . C(421) C -0.1379(4) 0.2481(2) 0.2948(2) 0.0274(11) Uani 1 1 d . . . C(422) C -0.1690(4) 0.2765(2) 0.3424(3) 0.0324(12) Uani 1 1 d . . . C(423) C -0.2671(5) 0.3131(3) 0.3318(3) 0.0409(14) Uani 1 1 d . . . C(424) C -0.3334(5) 0.3230(2) 0.2741(3) 0.0403(14) Uani 1 1 d . . . C(425) C -0.3030(4) 0.2957(3) 0.2277(3) 0.0404(14) Uani 1 1 d . . . C(426) C -0.2074(4) 0.2574(3) 0.2370(3) 0.0328(12) Uani 1 1 d . . . H(13) H 0.0494 0.4234 0.4382 0.048 Uiso 1 1 calc R . . H(14) H 0.1681 0.5065 0.4342 0.060 Uiso 1 1 calc R . . H(15) H 0.3303 0.4926 0.3984 0.056 Uiso 1 1 calc R . . H(23) H 0.4711 0.3261 0.5468 0.038 Uiso 1 1 calc R . . H(24) H 0.3714 0.3364 0.6191 0.042 Uiso 1 1 calc R . . H(25) H 0.1934 0.2850 0.6055 0.039 Uiso 1 1 calc R . . H(112) H 0.5654 0.2533 0.4034 0.038 Uiso 1 1 calc R . . H(113) H 0.7556 0.2441 0.4573 0.042 Uiso 1 1 calc R . . H(114) H 0.8398 0.1462 0.4786 0.047 Uiso 1 1 calc R . . H(115) H 0.7368 0.0566 0.4415 0.050 Uiso 1 1 calc R . . H(116) H 0.5512 0.0636 0.3846 0.041 Uiso 1 1 calc R . . H(122) H 0.5795 0.1671 0.2882 0.037 Uiso 1 1 calc R . . H(123) H 0.5998 0.1437 0.1937 0.042 Uiso 1 1 calc R . . H(124) H 0.4460 0.1101 0.1205 0.046 Uiso 1 1 calc R . . H(125) H 0.2677 0.0999 0.1396 0.040 Uiso 1 1 calc R . . H(126) H 0.2449 0.1208 0.2336 0.034 Uiso 1 1 calc R . . H(1B1) H 0.3708 0.0675 0.3830 0.031 Uiso 1 1 calc R . . H(1B2) H 0.2675 0.0807 0.3265 0.031 Uiso 1 1 calc R . . H(212) H 0.2619 -0.0125 0.3985 0.043 Uiso 1 1 calc R . . H(213) H 0.1596 -0.1048 0.3995 0.049 Uiso 1 1 calc R . . H(214) H -0.0261 -0.0996 0.4124 0.052 Uiso 1 1 calc R . . H(215) H -0.1058 -0.0030 0.4228 0.047 Uiso 1 1 calc R . . H(216) H -0.0051 0.0899 0.4190 0.038 Uiso 1 1 calc R . . H(222) H 0.4664 0.1269 0.4757 0.045 Uiso 1 1 calc R . . H(223) H 0.5661 0.1176 0.5747 0.058 Uiso 1 1 calc R . . H(224) H 0.4709 0.0983 0.6471 0.055 Uiso 1 1 calc R . . H(225) H 0.2719 0.0868 0.6197 0.051 Uiso 1 1 calc R . . H(226) H 0.1726 0.0935 0.5209 0.041 Uiso 1 1 calc R . . H(2B1) H -0.0124 0.2418 0.2123 0.032 Uiso 1 1 calc R . . H(2B2) H 0.0703 0.1824 0.2258 0.032 Uiso 1 1 calc R . . H(312) H 0.0739 0.2547 0.1380 0.042 Uiso 1 1 calc R . . H(313) H 0.1435 0.2482 0.0539 0.046 Uiso 1 1 calc R . . H(314) H 0.3374 0.2601 0.0621 0.037 Uiso 1 1 calc R . . H(315) H 0.4618 0.2792 0.1543 0.035 Uiso 1 1 calc R . . H(316) H 0.3949 0.2833 0.2390 0.033 Uiso 1 1 calc R . . H(322) H -0.0263 0.3416 0.2826 0.035 Uiso 1 1 calc R . . H(323) H -0.0839 0.4459 0.2754 0.037 Uiso 1 1 calc R . . H(324) H 0.0258 0.5221 0.2451 0.041 Uiso 1 1 calc R . . H(325) H 0.1906 0.4937 0.2191 0.046 Uiso 1 1 calc R . . H(326) H 0.2467 0.3892 0.2218 0.041 Uiso 1 1 calc R . . H(412) H 0.0588 0.0859 0.2575 0.045 Uiso 1 1 calc R . . H(413) H -0.0211 -0.0137 0.2359 0.062 Uiso 1 1 calc R . . H(414) H -0.1935 -0.0377 0.2577 0.069 Uiso 1 1 calc R . . H(415) H -0.2892 0.0391 0.2964 0.060 Uiso 1 1 calc R . . H(416) H -0.2138 0.1394 0.3142 0.045 Uiso 1 1 calc R . . H(422) H -0.1236 0.2708 0.3815 0.039 Uiso 1 1 calc R . . H(423) H -0.2892 0.3317 0.3640 0.049 Uiso 1 1 calc R . . H(424) H -0.3994 0.3485 0.2673 0.048 Uiso 1 1 calc R . . H(425) H -0.3476 0.3029 0.1887 0.048 Uiso 1 1 calc R . . H(426) H -0.1888 0.2376 0.2044 0.039 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Re(1) 0.01964(10) 0.02007(10) 0.02271(10) -0.00227(7) 0.00524(8) 0.00084(7) Re(5B) 0.01836(10) 0.01924(10) 0.02383(10) -0.00028(7) 0.00623(8) 0.00039(7) P(1) 0.0193(6) 0.0235(6) 0.0267(7) -0.0001(5) 0.0057(5) 0.0009(5) P(2) 0.0193(6) 0.0201(6) 0.0263(7) 0.0000(5) 0.0056(5) 0.0015(5) P(3) 0.0195(6) 0.0235(6) 0.0227(6) -0.0001(5) 0.0046(5) 0.0005(5) P(4) 0.0179(6) 0.0231(6) 0.0260(7) 0.0003(5) 0.0052(5) 0.0002(5) O(12) 0.0264(18) 0.0241(18) 0.0299(19) 0.0057(15) 0.0056(15) -0.0022(14) O(1W) 0.062(3) 0.031(2) 0.085(3) 0.020(2) 0.034(3) 0.016(2) O(22) 0.0207(17) 0.0315(19) 0.0231(18) -0.0042(14) 0.0024(15) -0.0030(14) O(171) 0.031(2) 0.032(2) 0.036(2) -0.0142(16) 0.0131(17) 0.0031(16) O(172) 0.068(3) 0.051(3) 0.063(3) -0.033(2) 0.031(3) -0.008(2) O(271) 0.0219(17) 0.0299(18) 0.0256(18) -0.0025(14) 0.0099(14) -0.0012(15) O(272) 0.041(2) 0.054(3) 0.041(2) -0.0094(19) 0.024(2) -0.0073(19) N(11) 0.030(2) 0.021(2) 0.026(2) 0.0024(18) 0.0064(19) -0.0019(17) N(21) 0.023(2) 0.022(2) 0.018(2) -0.0023(16) 0.0031(17) -0.0019(16) C(12) 0.029(3) 0.022(2) 0.023(3) 0.003(2) 0.000(2) 0.0020(19) C(13) 0.055(4) 0.024(3) 0.042(3) 0.007(3) 0.012(3) -0.006(2) C(14) 0.069(5) 0.028(3) 0.052(4) 0.002(3) 0.016(4) -0.009(3) C(15) 0.068(4) 0.026(3) 0.045(4) -0.013(3) 0.011(3) -0.001(3) C(16) 0.043(3) 0.023(3) 0.034(3) -0.008(2) 0.008(3) 0.001(2) C(17) 0.051(4) 0.032(3) 0.036(3) -0.022(3) 0.011(3) 0.004(2) C(1B) 0.025(3) 0.023(2) 0.030(3) 0.002(2) 0.008(2) 0.002(2) C(22) 0.029(3) 0.026(3) 0.023(3) -0.003(2) 0.003(2) 0.004(2) C(23) 0.032(3) 0.030(3) 0.028(3) -0.006(2) -0.001(2) -0.002(2) C(24) 0.039(3) 0.038(3) 0.027(3) -0.003(2) 0.005(2) -0.010(2) C(25) 0.031(3) 0.040(3) 0.030(3) -0.001(2) 0.014(2) -0.004(2) C(26) 0.026(3) 0.028(3) 0.023(3) 0.003(2) 0.007(2) 0.001(2) C(27) 0.026(3) 0.030(3) 0.025(3) 0.002(2) 0.008(2) -0.002(2) C(2B) 0.019(2) 0.033(3) 0.027(3) 0.001(2) 0.006(2) -0.003(2) C(111) 0.021(2) 0.037(3) 0.025(3) -0.001(2) 0.009(2) 0.002(2) C(112) 0.024(3) 0.040(3) 0.033(3) -0.002(2) 0.010(2) 0.005(2) C(113) 0.025(3) 0.052(4) 0.031(3) -0.010(2) 0.012(2) -0.004(3) C(114) 0.025(3) 0.062(4) 0.032(3) 0.003(3) 0.008(2) 0.009(3) C(115) 0.025(3) 0.051(4) 0.047(4) 0.015(3) 0.007(3) 0.008(3) C(116) 0.022(3) 0.040(3) 0.041(3) 0.004(2) 0.010(2) 0.000(3) C(121) 0.025(3) 0.022(2) 0.034(3) 0.004(2) 0.012(2) 0.003(2) C(122) 0.026(3) 0.027(3) 0.039(3) -0.001(2) 0.008(2) 0.003(2) C(123) 0.035(3) 0.037(3) 0.038(3) 0.003(2) 0.019(3) 0.002(2) C(124) 0.051(4) 0.032(3) 0.035(3) 0.004(3) 0.018(3) -0.002(2) C(125) 0.040(3) 0.027(3) 0.033(3) -0.002(2) 0.008(3) -0.003(2) C(126) 0.025(3) 0.030(3) 0.030(3) 0.001(2) 0.007(2) 0.001(2) C(211) 0.027(3) 0.024(3) 0.025(3) -0.004(2) 0.004(2) 0.001(2) C(212) 0.032(3) 0.026(3) 0.052(4) -0.003(2) 0.015(3) 0.001(2) C(213) 0.045(3) 0.021(3) 0.060(4) -0.002(2) 0.020(3) 0.001(3) C(214) 0.042(3) 0.031(3) 0.057(4) -0.012(3) 0.012(3) 0.005(3) C(215) 0.030(3) 0.033(3) 0.058(4) -0.008(2) 0.016(3) 0.003(3) C(216) 0.028(3) 0.024(3) 0.044(3) -0.001(2) 0.011(3) 0.001(2) C(221) 0.026(3) 0.018(2) 0.034(3) 0.0007(19) 0.009(2) 0.002(2) C(222) 0.030(3) 0.052(4) 0.027(3) -0.006(3) 0.005(2) 0.006(3) C(223) 0.030(3) 0.068(4) 0.041(4) -0.010(3) -0.001(3) 0.005(3) C(224) 0.051(4) 0.049(4) 0.030(3) -0.016(3) -0.003(3) 0.008(3) C(225) 0.048(4) 0.046(4) 0.034(3) -0.009(3) 0.011(3) 0.004(3) C(226) 0.030(3) 0.039(3) 0.030(3) -0.006(2) 0.004(2) 0.004(2) C(311) 0.022(2) 0.026(3) 0.024(2) -0.001(2) 0.004(2) 0.002(2) C(312) 0.022(3) 0.053(3) 0.032(3) 0.001(2) 0.010(2) 0.003(3) C(313) 0.034(3) 0.056(4) 0.023(3) -0.006(3) 0.006(2) 0.003(3) C(314) 0.031(3) 0.037(3) 0.030(3) -0.002(2) 0.016(2) 0.002(2) C(315) 0.023(3) 0.029(3) 0.035(3) 0.000(2) 0.010(2) 0.001(2) C(316) 0.025(3) 0.027(3) 0.031(3) -0.002(2) 0.009(2) 0.003(2) C(321) 0.023(2) 0.026(3) 0.027(3) 0.003(2) 0.005(2) 0.001(2) C(322) 0.029(3) 0.026(3) 0.030(3) 0.003(2) 0.007(2) 0.000(2) C(323) 0.028(3) 0.030(3) 0.035(3) 0.005(2) 0.006(2) -0.001(2) C(324) 0.041(3) 0.022(3) 0.036(3) 0.004(2) 0.004(3) 0.003(2) C(325) 0.041(3) 0.026(3) 0.049(4) 0.000(2) 0.013(3) 0.011(3) C(326) 0.030(3) 0.030(3) 0.042(3) -0.003(2) 0.009(3) 0.004(2) C(411) 0.020(2) 0.028(3) 0.038(3) -0.002(2) 0.002(2) -0.005(2) C(412) 0.027(3) 0.032(3) 0.052(4) 0.000(2) 0.010(3) -0.010(3) C(413) 0.045(4) 0.029(3) 0.074(5) 0.003(3) 0.004(3) -0.018(3) C(414) 0.039(4) 0.030(3) 0.093(6) -0.008(3) -0.003(4) -0.019(3) C(415) 0.032(3) 0.030(3) 0.085(5) -0.011(2) 0.007(3) -0.004(3) C(416) 0.026(3) 0.030(3) 0.059(4) 0.002(2) 0.013(3) 0.002(3) C(421) 0.025(3) 0.023(3) 0.039(3) 0.001(2) 0.016(2) 0.001(2) C(422) 0.025(3) 0.032(3) 0.041(3) 0.003(2) 0.010(2) 0.007(2) C(423) 0.032(3) 0.037(3) 0.061(4) 0.004(2) 0.024(3) -0.004(3) C(424) 0.027(3) 0.025(3) 0.070(4) 0.005(2) 0.015(3) 0.011(3) C(425) 0.023(3) 0.043(3) 0.049(4) 0.003(2) -0.001(3) 0.013(3) C(426) 0.022(3) 0.038(3) 0.038(3) 0.002(2) 0.007(2) 0.001(2) # 10. MOLECULAR GEOMETRY _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re(1) O(22) 2.118(3) . ? Re(1) N(11) 2.165(4) . ? Re(1) O(171) 2.213(3) . ? Re(1) Re(5B) 2.3139(3) . ? Re(1) P(3) 2.3867(12) . ? Re(1) P(1) 2.4059(13) . ? Re(5B) O(12) 2.109(3) . ? Re(5B) N(21) 2.171(4) . ? Re(5B) O(271) 2.176(3) . ? Re(5B) P(2) 2.3892(12) . ? Re(5B) P(4) 2.4114(12) . ? P(1) C(111) 1.829(5) . ? P(1) C(1B) 1.838(5) . ? P(1) C(121) 1.846(5) . ? P(2) C(211) 1.839(5) . ? P(2) C(1B) 1.843(5) . ? P(2) C(221) 1.844(5) . ? P(3) C(311) 1.842(5) . ? P(3) C(2B) 1.843(5) . ? P(3) C(321) 1.846(5) . ? P(4) C(421) 1.831(5) . ? P(4) C(2B) 1.833(5) . ? P(4) C(411) 1.842(5) . ? O(12) C(12) 1.292(6) . ? O(22) C(22) 1.298(6) . ? O(171) C(17) 1.271(7) . ? O(172) C(17) 1.258(6) . ? O(271) C(27) 1.298(6) . ? O(272) C(27) 1.225(6) . ? N(11) C(12) 1.348(6) . ? N(11) C(16) 1.359(6) . ? N(21) C(22) 1.355(6) . ? N(21) C(26) 1.361(6) . ? C(12) C(13) 1.436(7) . ? C(13) C(14) 1.355(8) . ? C(14) C(15) 1.394(9) . ? C(15) C(16) 1.366(8) . ? C(16) C(17) 1.508(8) . ? C(22) C(23) 1.411(7) . ? C(23) C(24) 1.378(7) . ? C(24) C(25) 1.409(7) . ? C(25) C(26) 1.358(7) . ? C(26) C(27) 1.501(7) . ? C(111) C(116) 1.403(7) . ? C(111) C(112) 1.406(7) . ? C(112) C(113) 1.396(7) . ? C(113) C(114) 1.379(8) . ? C(114) C(115) 1.385(8) . ? C(115) C(116) 1.374(7) . ? C(121) C(126) 1.399(7) . ? C(121) C(122) 1.402(7) . ? C(122) C(123) 1.398(7) . ? C(123) C(124) 1.362(7) . ? C(124) C(125) 1.386(8) . ? C(125) C(126) 1.387(7) . ? C(211) C(216) 1.378(7) . ? C(211) C(212) 1.400(7) . ? C(212) C(213) 1.388(7) . ? C(213) C(214) 1.398(8) . ? C(214) C(215) 1.375(8) . ? C(215) C(216) 1.402(7) . ? C(221) C(222) 1.378(7) . ? C(221) C(226) 1.395(7) . ? C(222) C(223) 1.394(7) . ? C(223) C(224) 1.373(8) . ? C(224) C(225) 1.395(8) . ? C(225) C(226) 1.383(7) . ? C(311) C(316) 1.395(7) . ? C(311) C(312) 1.395(7) . ? C(312) C(313) 1.391(8) . ? C(313) C(314) 1.379(7) . ? C(314) C(315) 1.390(7) . ? C(315) C(316) 1.386(7) . ? C(321) C(326) 1.399(7) . ? C(321) C(322) 1.399(7) . ? C(322) C(323) 1.385(7) . ? C(323) C(324) 1.381(7) . ? C(324) C(325) 1.374(8) . ? C(325) C(326) 1.386(7) . ? C(411) C(412) 1.381(7) . ? C(411) C(416) 1.394(7) . ? C(412) C(413) 1.394(8) . ? C(413) C(414) 1.385(9) . ? C(414) C(415) 1.377(9) . ? C(415) C(416) 1.384(7) . ? C(421) C(422) 1.402(7) . ? C(421) C(426) 1.417(7) . ? C(422) C(423) 1.396(7) . ? C(423) C(424) 1.401(8) . ? C(424) C(425) 1.365(8) . ? C(425) C(426) 1.391(7) . ? 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 O(22) Re(1) N(11) 80.03(14) . . ? O(22) Re(1) O(171) 83.92(13) . . ? N(11) Re(1) O(171) 73.24(15) . . ? O(22) Re(1) Re(5B) 94.50(9) . . ? N(11) Re(1) Re(5B) 84.63(11) . . ? O(171) Re(1) Re(5B) 157.77(10) . . ? O(22) Re(1) P(3) 165.82(9) . . ? N(11) Re(1) P(3) 88.35(11) . . ? O(171) Re(1) P(3) 84.97(9) . . ? Re(5B) Re(1) P(3) 92.45(3) . . ? O(22) Re(1) P(1) 91.09(10) . . ? N(11) Re(1) P(1) 167.96(11) . . ? O(171) Re(1) P(1) 97.90(10) . . ? Re(5B) Re(1) P(1) 104.31(3) . . ? P(3) Re(1) P(1) 99.15(4) . . ? O(12) Re(5B) N(21) 78.96(13) . . ? O(12) Re(5B) O(271) 83.55(13) . . ? N(21) Re(5B) O(271) 73.82(14) . . ? O(12) Re(5B) Re(1) 94.07(9) . . ? N(21) Re(5B) Re(1) 83.98(11) . . ? O(271) Re(5B) Re(1) 157.73(8) . . ? O(12) Re(5B) P(2) 165.74(10) . . ? N(21) Re(5B) P(2) 89.20(10) . . ? O(271) Re(5B) P(2) 85.54(9) . . ? Re(1) Re(5B) P(2) 92.54(3) . . ? O(12) Re(5B) P(4) 90.54(9) . . ? N(21) Re(5B) P(4) 167.09(11) . . ? O(271) Re(5B) P(4) 97.72(9) . . ? Re(1) Re(5B) P(4) 104.45(3) . . ? P(2) Re(5B) P(4) 100.02(4) . . ? C(111) P(1) C(1B) 105.4(2) . . ? C(111) P(1) C(121) 100.1(2) . . ? C(1B) P(1) C(121) 102.6(2) . . ? C(111) P(1) Re(1) 116.89(17) . . ? C(1B) P(1) Re(1) 107.29(16) . . ? C(121) P(1) Re(1) 122.61(16) . . ? C(211) P(2) C(1B) 101.1(2) . . ? C(211) P(2) C(221) 98.3(2) . . ? C(1B) P(2) C(221) 106.8(2) . . ? C(211) P(2) Re(5B) 122.84(17) . . ? C(1B) P(2) Re(5B) 113.78(16) . . ? C(221) P(2) Re(5B) 112.00(16) . . ? C(311) P(3) C(2B) 101.3(2) . . ? C(311) P(3) C(321) 99.1(2) . . ? C(2B) P(3) C(321) 106.3(2) . . ? C(311) P(3) Re(1) 122.58(16) . . ? C(2B) P(3) Re(1) 114.61(17) . . ? C(321) P(3) Re(1) 110.88(16) . . ? C(421) P(4) C(2B) 104.1(2) . . ? C(421) P(4) C(411) 100.3(2) . . ? C(2B) P(4) C(411) 103.4(2) . . ? C(421) P(4) Re(5B) 116.84(18) . . ? C(2B) P(4) Re(5B) 107.41(16) . . ? C(411) P(4) Re(5B) 122.67(17) . . ? C(12) O(12) Re(5B) 115.7(3) . . ? C(22) O(22) Re(1) 114.6(3) . . ? C(17) O(171) Re(1) 117.7(3) . . ? C(27) O(271) Re(5B) 118.0(3) . . ? C(12) N(11) C(16) 119.8(4) . . ? C(12) N(11) Re(1) 122.3(3) . . ? C(16) N(11) Re(1) 117.8(4) . . ? C(22) N(21) C(26) 120.5(4) . . ? C(22) N(21) Re(5B) 122.9(3) . . ? C(26) N(21) Re(5B) 115.5(3) . . ? O(12) C(12) N(11) 120.2(4) . . ? O(12) C(12) C(13) 120.2(5) . . ? N(11) C(12) C(13) 119.6(5) . . ? C(14) C(13) C(12) 118.8(6) . . ? C(13) C(14) C(15) 121.1(6) . . ? C(16) C(15) C(14) 118.0(6) . . ? N(11) C(16) C(15) 122.7(6) . . ? N(11) C(16) C(17) 113.2(4) . . ? C(15) C(16) C(17) 124.0(5) . . ? O(172) C(17) O(171) 122.8(6) . . ? O(172) C(17) C(16) 120.8(5) . . ? O(171) C(17) C(16) 116.4(4) . . ? P(1) C(1B) P(2) 112.9(3) . . ? O(22) C(22) N(21) 119.0(4) . . ? O(22) C(22) C(23) 122.0(5) . . ? N(21) C(22) C(23) 119.0(5) . . ? C(24) C(23) C(22) 120.4(5) . . ? C(23) C(24) C(25) 118.9(5) . . ? C(26) C(25) C(24) 118.8(5) . . ? C(25) C(26) N(21) 122.2(5) . . ? C(25) C(26) C(27) 123.3(5) . . ? N(21) C(26) C(27) 114.4(4) . . ? O(272) C(27) O(271) 125.3(5) . . ? O(272) C(27) C(26) 119.8(5) . . ? O(271) C(27) C(26) 114.8(4) . . ? P(4) C(2B) P(3) 112.9(3) . . ? C(116) C(111) C(112) 119.0(5) . . ? C(116) C(111) P(1) 122.1(4) . . ? C(112) C(111) P(1) 118.9(4) . . ? C(113) C(112) C(111) 119.3(5) . . ? C(114) C(113) C(112) 121.1(5) . . ? C(113) C(114) C(115) 119.2(5) . . ? C(116) C(115) C(114) 121.2(5) . . ? C(115) C(116) C(111) 120.2(5) . . ? C(126) C(121) C(122) 118.4(5) . . ? C(126) C(121) P(1) 121.0(4) . . ? C(122) C(121) P(1) 120.5(4) . . ? C(123) C(122) C(121) 120.0(5) . . ? C(124) C(123) C(122) 120.7(5) . . ? C(123) C(124) C(125) 120.1(5) . . ? C(124) C(125) C(126) 120.3(5) . . ? C(125) C(126) C(121) 120.5(5) . . ? C(216) C(211) C(212) 119.2(5) . . ? C(216) C(211) P(2) 120.4(4) . . ? C(212) C(211) P(2) 120.2(4) . . ? C(213) C(212) C(211) 121.2(5) . . ? C(212) C(213) C(214) 119.2(5) . . ? C(215) C(214) C(213) 119.6(5) . . ? C(214) C(215) C(216) 121.1(5) . . ? C(211) C(216) C(215) 119.7(5) . . ? C(222) C(221) C(226) 119.2(5) . . ? C(222) C(221) P(2) 123.6(4) . . ? C(226) C(221) P(2) 117.2(4) . . ? C(221) C(222) C(223) 119.9(5) . . ? C(224) C(223) C(222) 121.2(6) . . ? C(223) C(224) C(225) 118.9(5) . . ? C(226) C(225) C(224) 120.2(6) . . ? C(225) C(226) C(221) 120.5(5) . . ? C(316) C(311) C(312) 119.6(5) . . ? C(316) C(311) P(3) 120.2(4) . . ? C(312) C(311) P(3) 120.1(4) . . ? C(313) C(312) C(311) 120.3(5) . . ? C(314) C(313) C(312) 120.1(5) . . ? C(313) C(314) C(315) 119.6(5) . . ? C(316) C(315) C(314) 121.0(5) . . ? C(315) C(316) C(311) 119.4(5) . . ? C(326) C(321) C(322) 118.8(5) . . ? C(326) C(321) P(3) 118.7(4) . . ? C(322) C(321) P(3) 122.3(4) . . ? C(323) C(322) C(321) 120.2(5) . . ? C(324) C(323) C(322) 120.5(5) . . ? C(325) C(324) C(323) 119.7(5) . . ? C(324) C(325) C(326) 120.9(5) . . ? C(325) C(326) C(321) 119.9(5) . . ? C(412) C(411) C(416) 118.8(5) . . ? C(412) C(411) P(4) 121.7(4) . . ? C(416) C(411) P(4) 119.3(4) . . ? C(411) C(412) C(413) 120.8(6) . . ? C(414) C(413) C(412) 119.8(6) . . ? C(415) C(414) C(413) 119.7(5) . . ? C(414) C(415) C(416) 120.5(6) . . ? C(415) C(416) C(411) 120.4(5) . . ? C(422) C(421) C(426) 118.9(5) . . ? C(422) C(421) P(4) 121.4(4) . . ? C(426) C(421) P(4) 119.7(4) . . ? C(423) C(422) C(421) 119.5(5) . . ? C(422) C(423) C(424) 120.7(6) . . ? C(425) C(424) C(423) 119.9(5) . . ? C(424) C(425) C(426) 120.8(5) . . ? C(425) C(426) C(421) 120.1(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O(22) Re(1) Re(5B) O(12) 88.82(12) . . . . ? N(11) Re(1) Re(5B) O(12) 9.29(13) . . . . ? O(171) Re(1) Re(5B) O(12) 3.9(3) . . . . ? P(3) Re(1) Re(5B) O(12) -78.82(9) . . . . ? P(1) Re(1) Re(5B) O(12) -178.91(9) . . . . ? O(22) Re(1) Re(5B) N(21) 10.38(13) . . . . ? N(11) Re(1) Re(5B) N(21) -69.15(15) . . . . ? O(171) Re(1) Re(5B) N(21) -74.6(3) . . . . ? P(3) Re(1) Re(5B) N(21) -157.25(10) . . . . ? P(1) Re(1) Re(5B) N(21) 102.66(10) . . . . ? O(22) Re(1) Re(5B) O(271) 5.9(2) . . . . ? N(11) Re(1) Re(5B) O(271) -73.6(3) . . . . ? O(171) Re(1) Re(5B) O(271) -79.1(3) . . . . ? P(3) Re(1) Re(5B) O(271) -161.7(2) . . . . ? P(1) Re(1) Re(5B) O(271) 98.2(2) . . . . ? O(22) Re(1) Re(5B) P(2) -78.55(9) . . . . ? N(11) Re(1) Re(5B) P(2) -158.07(11) . . . . ? O(171) Re(1) Re(5B) P(2) -163.5(2) . . . . ? P(3) Re(1) Re(5B) P(2) 113.82(4) . . . . ? P(1) Re(1) Re(5B) P(2) 13.73(4) . . . . ? O(22) Re(1) Re(5B) P(4) -179.57(9) . . . . ? N(11) Re(1) Re(5B) P(4) 100.90(11) . . . . ? O(171) Re(1) Re(5B) P(4) 95.5(2) . . . . ? P(3) Re(1) Re(5B) P(4) 12.80(4) . . . . ? P(1) Re(1) Re(5B) P(4) -87.29(4) . . . . ? O(22) Re(1) P(1) C(111) -22.4(2) . . . . ? N(11) Re(1) P(1) C(111) 19.8(6) . . . . ? O(171) Re(1) P(1) C(111) 61.6(2) . . . . ? Re(5B) Re(1) P(1) C(111) -117.35(18) . . . . ? P(3) Re(1) P(1) C(111) 147.73(19) . . . . ? O(22) Re(1) P(1) C(1B) 95.62(19) . . . . ? N(11) Re(1) P(1) C(1B) 137.8(6) . . . . ? O(171) Re(1) P(1) C(1B) 179.63(19) . . . . ? Re(5B) Re(1) P(1) C(1B) 0.69(17) . . . . ? P(3) Re(1) P(1) C(1B) -94.22(17) . . . . ? O(22) Re(1) P(1) C(121) -146.3(2) . . . . ? N(11) Re(1) P(1) C(121) -104.1(6) . . . . ? O(171) Re(1) P(1) C(121) -62.2(2) . . . . ? Re(5B) Re(1) P(1) C(121) 118.81(19) . . . . ? P(3) Re(1) P(1) C(121) 23.89(19) . . . . ? O(12) Re(5B) P(2) C(211) 91.6(4) . . . . ? N(21) Re(5B) P(2) C(211) 125.3(2) . . . . ? O(271) Re(5B) P(2) C(211) 51.4(2) . . . . ? Re(1) Re(5B) P(2) C(211) -150.8(2) . . . . ? P(4) Re(5B) P(2) C(211) -45.6(2) . . . . ? O(12) Re(5B) P(2) C(1B) -146.0(4) . . . . ? N(21) Re(5B) P(2) C(1B) -112.4(2) . . . . ? O(271) Re(5B) P(2) C(1B) 173.81(19) . . . . ? Re(1) Re(5B) P(2) C(1B) -28.42(18) . . . . ? P(4) Re(5B) P(2) C(1B) 76.74(18) . . . . ? O(12) Re(5B) P(2) C(221) -24.8(4) . . . . ? N(21) Re(5B) P(2) C(221) 8.8(2) . . . . ? O(271) Re(5B) P(2) C(221) -64.99(19) . . . . ? Re(1) Re(5B) P(2) C(221) 92.78(17) . . . . ? P(4) Re(5B) P(2) C(221) -162.06(18) . . . . ? O(22) Re(1) P(3) C(311) 90.6(4) . . . . ? N(11) Re(1) P(3) C(311) 125.4(2) . . . . ? O(171) Re(1) P(3) C(311) 52.1(2) . . . . ? Re(5B) Re(1) P(3) C(311) -150.04(18) . . . . ? P(1) Re(1) P(3) C(311) -45.13(19) . . . . ? O(22) Re(1) P(3) C(2B) -146.2(4) . . . . ? N(11) Re(1) P(3) C(2B) -111.4(2) . . . . ? O(171) Re(1) P(3) C(2B) 175.3(2) . . . . ? Re(5B) Re(1) P(3) C(2B) -26.82(18) . . . . ? P(1) Re(1) P(3) C(2B) 78.09(18) . . . . ? O(22) Re(1) P(3) C(321) -25.8(4) . . . . ? N(11) Re(1) P(3) C(321) 9.0(2) . . . . ? O(171) Re(1) P(3) C(321) -64.4(2) . . . . ? Re(5B) Re(1) P(3) C(321) 93.52(18) . . . . ? P(1) Re(1) P(3) C(321) -161.57(18) . . . . ? O(12) Re(5B) P(4) C(421) -21.2(2) . . . . ? N(21) Re(5B) P(4) C(421) 14.2(5) . . . . ? O(271) Re(5B) P(4) C(421) 62.4(2) . . . . ? Re(1) Re(5B) P(4) C(421) -115.54(18) . . . . ? P(2) Re(5B) P(4) C(421) 149.18(19) . . . . ? O(12) Re(5B) P(4) C(2B) 95.2(2) . . . . ? N(21) Re(5B) P(4) C(2B) 130.6(5) . . . . ? O(271) Re(5B) P(4) C(2B) 178.74(19) . . . . ? Re(1) Re(5B) P(4) C(2B) 0.82(17) . . . . ? P(2) Re(5B) P(4) C(2B) -94.45(17) . . . . ? O(12) Re(5B) P(4) C(411) -145.5(2) . . . . ? N(21) Re(5B) P(4) C(411) -110.1(5) . . . . ? O(271) Re(5B) P(4) C(411) -61.9(2) . . . . ? Re(1) Re(5B) P(4) C(411) 120.2(2) . . . . ? P(2) Re(5B) P(4) C(411) 24.9(2) . . . . ? N(21) Re(5B) O(12) C(12) 64.7(3) . . . . ? O(271) Re(5B) O(12) C(12) 139.5(3) . . . . ? Re(1) Re(5B) O(12) C(12) -18.3(3) . . . . ? P(2) Re(5B) O(12) C(12) 99.1(5) . . . . ? P(4) Re(5B) O(12) C(12) -122.8(3) . . . . ? N(11) Re(1) O(22) C(22) 61.2(3) . . . . ? O(171) Re(1) O(22) C(22) 135.2(3) . . . . ? Re(5B) Re(1) O(22) C(22) -22.5(3) . . . . ? P(3) Re(1) O(22) C(22) 96.6(5) . . . . ? P(1) Re(1) O(22) C(22) -126.9(3) . . . . ? O(22) Re(1) O(171) C(17) -70.0(4) . . . . ? N(11) Re(1) O(171) C(17) 11.4(4) . . . . ? Re(5B) Re(1) O(171) C(17) 17.0(5) . . . . ? P(3) Re(1) O(171) C(17) 101.2(4) . . . . ? P(1) Re(1) O(171) C(17) -160.3(4) . . . . ? O(12) Re(5B) O(271) C(27) -65.2(3) . . . . ? N(21) Re(5B) O(271) C(27) 15.2(3) . . . . ? Re(1) Re(5B) O(271) C(27) 19.8(5) . . . . ? P(2) Re(5B) O(271) C(27) 105.6(3) . . . . ? P(4) Re(5B) O(271) C(27) -154.8(3) . . . . ? O(22) Re(1) N(11) C(12) -99.7(4) . . . . ? O(171) Re(1) N(11) C(12) 173.7(4) . . . . ? Re(5B) Re(1) N(11) C(12) -4.1(3) . . . . ? P(3) Re(1) N(11) C(12) 88.5(4) . . . . ? P(1) Re(1) N(11) C(12) -142.6(4) . . . . ? O(22) Re(1) N(11) C(16) 75.6(4) . . . . ? O(171) Re(1) N(11) C(16) -11.0(4) . . . . ? Re(5B) Re(1) N(11) C(16) 171.1(4) . . . . ? P(3) Re(1) N(11) C(16) -96.3(4) . . . . ? P(1) Re(1) N(11) C(16) 32.6(8) . . . . ? O(12) Re(5B) N(21) C(22) -97.8(4) . . . . ? O(271) Re(5B) N(21) C(22) 175.8(4) . . . . ? Re(1) Re(5B) N(21) C(22) -2.4(4) . . . . ? P(2) Re(5B) N(21) C(22) 90.2(4) . . . . ? P(4) Re(5B) N(21) C(22) -134.0(4) . . . . ? O(12) Re(5B) N(21) C(26) 70.0(3) . . . . ? O(271) Re(5B) N(21) C(26) -16.4(3) . . . . ? Re(1) Re(5B) N(21) C(26) 165.4(3) . . . . ? P(2) Re(5B) N(21) C(26) -102.0(3) . . . . ? P(4) Re(5B) N(21) C(26) 33.9(7) . . . . ? Re(5B) O(12) C(12) N(11) 19.0(5) . . . . ? Re(5B) O(12) C(12) C(13) -163.2(4) . . . . ? C(16) N(11) C(12) O(12) 175.8(4) . . . . ? Re(1) N(11) C(12) O(12) -9.1(6) . . . . ? C(16) N(11) C(12) C(13) -2.1(7) . . . . ? Re(1) N(11) C(12) C(13) 173.0(4) . . . . ? O(12) C(12) C(13) C(14) -176.5(5) . . . . ? N(11) C(12) C(13) C(14) 1.4(8) . . . . ? C(12) C(13) C(14) C(15) -0.5(9) . . . . ? C(13) C(14) C(15) C(16) 0.3(9) . . . . ? C(12) N(11) C(16) C(15) 2.0(8) . . . . ? Re(1) N(11) C(16) C(15) -173.4(4) . . . . ? C(12) N(11) C(16) C(17) -174.9(4) . . . . ? Re(1) N(11) C(16) C(17) 9.8(6) . . . . ? C(14) C(15) C(16) N(11) -1.1(9) . . . . ? C(14) C(15) C(16) C(17) 175.5(5) . . . . ? Re(1) O(171) C(17) O(172) 171.9(4) . . . . ? Re(1) O(171) C(17) C(16) -10.0(6) . . . . ? N(11) C(16) C(17) O(172) 178.4(5) . . . . ? C(15) C(16) C(17) O(172) 1.6(9) . . . . ? N(11) C(16) C(17) O(171) 0.3(7) . . . . ? C(15) C(16) C(17) O(171) -176.5(5) . . . . ? C(111) P(1) C(1B) P(2) 104.5(3) . . . . ? C(121) P(1) C(1B) P(2) -151.2(3) . . . . ? Re(1) P(1) C(1B) P(2) -20.8(3) . . . . ? C(211) P(2) C(1B) P(1) 167.5(3) . . . . ? C(221) P(2) C(1B) P(1) -90.2(3) . . . . ? Re(5B) P(2) C(1B) P(1) 33.9(3) . . . . ? Re(1) O(22) C(22) N(21) 25.0(5) . . . . ? Re(1) O(22) C(22) C(23) -153.7(4) . . . . ? C(26) N(21) C(22) O(22) 178.3(4) . . . . ? Re(5B) N(21) C(22) O(22) -14.5(6) . . . . ? C(26) N(21) C(22) C(23) -3.0(7) . . . . ? Re(5B) N(21) C(22) C(23) 164.2(3) . . . . ? O(22) C(22) C(23) C(24) 179.1(5) . . . . ? N(21) C(22) C(23) C(24) 0.4(8) . . . . ? C(22) C(23) C(24) C(25) 2.7(8) . . . . ? C(23) C(24) C(25) C(26) -3.3(8) . . . . ? C(24) C(25) C(26) N(21) 0.8(8) . . . . ? C(24) C(25) C(26) C(27) 178.8(5) . . . . ? C(22) N(21) C(26) C(25) 2.4(7) . . . . ? Re(5B) N(21) C(26) C(25) -165.7(4) . . . . ? C(22) N(21) C(26) C(27) -175.7(4) . . . . ? Re(5B) N(21) C(26) C(27) 16.1(5) . . . . ? Re(5B) O(271) C(27) O(272) 172.2(4) . . . . ? Re(5B) O(271) C(27) C(26) -11.5(5) . . . . ? C(25) C(26) C(27) O(272) -4.9(8) . . . . ? N(21) C(26) C(27) O(272) 173.3(4) . . . . ? C(25) C(26) C(27) O(271) 178.7(5) . . . . ? N(21) C(26) C(27) O(271) -3.2(6) . . . . ? C(421) P(4) C(2B) P(3) 104.9(3) . . . . ? C(411) P(4) C(2B) P(3) -150.7(3) . . . . ? Re(5B) P(4) C(2B) P(3) -19.6(3) . . . . ? C(311) P(3) C(2B) P(4) 166.1(3) . . . . ? C(321) P(3) C(2B) P(4) -90.8(3) . . . . ? Re(1) P(3) C(2B) P(4) 32.1(3) . . . . ? C(1B) P(1) C(111) C(116) 37.3(5) . . . . ? C(121) P(1) C(111) C(116) -68.9(5) . . . . ? Re(1) P(1) C(111) C(116) 156.3(4) . . . . ? C(1B) P(1) C(111) C(112) -145.0(4) . . . . ? C(121) P(1) C(111) C(112) 108.7(4) . . . . ? Re(1) P(1) C(111) C(112) -26.0(5) . . . . ? C(116) C(111) C(112) C(113) -0.4(8) . . . . ? P(1) C(111) C(112) C(113) -178.1(4) . . . . ? C(111) C(112) C(113) C(114) -1.5(8) . . . . ? C(112) C(113) C(114) C(115) 1.9(9) . . . . ? C(113) C(114) C(115) C(116) -0.4(9) . . . . ? C(114) C(115) C(116) C(111) -1.5(9) . . . . ? C(112) C(111) C(116) C(115) 1.9(8) . . . . ? P(1) C(111) C(116) C(115) 179.5(4) . . . . ? C(111) P(1) C(121) C(126) 159.1(4) . . . . ? C(1B) P(1) C(121) C(126) 50.6(4) . . . . ? Re(1) P(1) C(121) C(126) -69.7(4) . . . . ? C(111) P(1) C(121) C(122) -24.7(4) . . . . ? C(1B) P(1) C(121) C(122) -133.1(4) . . . . ? Re(1) P(1) C(121) C(122) 106.5(4) . . . . ? C(126) C(121) C(122) C(123) -0.9(7) . . . . ? P(1) C(121) C(122) C(123) -177.2(4) . . . . ? C(121) C(122) C(123) C(124) 0.6(8) . . . . ? C(122) C(123) C(124) C(125) 0.3(8) . . . . ? C(123) C(124) C(125) C(126) -1.0(8) . . . . ? C(124) C(125) C(126) C(121) 0.7(8) . . . . ? C(122) C(121) C(126) C(125) 0.2(7) . . . . ? P(1) C(121) C(126) C(125) 176.5(4) . . . . ? C(1B) P(2) C(211) C(216) -151.6(4) . . . . ? C(221) P(2) C(211) C(216) 99.4(4) . . . . ? Re(5B) P(2) C(211) C(216) -23.6(5) . . . . ? C(1B) P(2) C(211) C(212) 34.9(5) . . . . ? C(221) P(2) C(211) C(212) -74.1(5) . . . . ? Re(5B) P(2) C(211) C(212) 163.0(4) . . . . ? C(216) C(211) C(212) C(213) 1.6(8) . . . . ? P(2) C(211) C(212) C(213) 175.2(4) . . . . ? C(211) C(212) C(213) C(214) -1.5(9) . . . . ? C(212) C(213) C(214) C(215) 0.3(9) . . . . ? C(213) C(214) C(215) C(216) 0.7(9) . . . . ? C(212) C(211) C(216) C(215) -0.6(8) . . . . ? P(2) C(211) C(216) C(215) -174.1(4) . . . . ? C(214) C(215) C(216) C(211) -0.5(9) . . . . ? C(211) P(2) C(221) C(222) 132.6(5) . . . . ? C(1B) P(2) C(221) C(222) 28.2(5) . . . . ? Re(5B) P(2) C(221) C(222) -96.9(4) . . . . ? C(211) P(2) C(221) C(226) -50.7(4) . . . . ? C(1B) P(2) C(221) C(226) -155.0(4) . . . . ? Re(5B) P(2) C(221) C(226) 79.9(4) . . . . ? C(226) C(221) C(222) C(223) 0.8(8) . . . . ? P(2) C(221) C(222) C(223) 177.5(5) . . . . ? C(221) C(222) C(223) C(224) -1.0(10) . . . . ? C(222) C(223) C(224) C(225) 0.4(10) . . . . ? C(223) C(224) C(225) C(226) 0.5(9) . . . . ? C(224) C(225) C(226) C(221) -0.7(8) . . . . ? C(222) C(221) C(226) C(225) 0.1(8) . . . . ? P(2) C(221) C(226) C(225) -176.9(4) . . . . ? C(2B) P(3) C(311) C(316) -151.3(4) . . . . ? C(321) P(3) C(311) C(316) 100.0(4) . . . . ? Re(1) P(3) C(311) C(316) -22.1(5) . . . . ? C(2B) P(3) C(311) C(312) 32.5(5) . . . . ? C(321) P(3) C(311) C(312) -76.3(4) . . . . ? Re(1) P(3) C(311) C(312) 161.6(4) . . . . ? C(316) C(311) C(312) C(313) 2.4(8) . . . . ? P(3) C(311) C(312) C(313) 178.7(4) . . . . ? C(311) C(312) C(313) C(314) -1.5(9) . . . . ? C(312) C(313) C(314) C(315) -0.4(8) . . . . ? C(313) C(314) C(315) C(316) 1.3(8) . . . . ? C(314) C(315) C(316) C(311) -0.3(7) . . . . ? C(312) C(311) C(316) C(315) -1.5(7) . . . . ? P(3) C(311) C(316) C(315) -177.8(4) . . . . ? C(311) P(3) C(321) C(326) -41.4(4) . . . . ? C(2B) P(3) C(321) C(326) -146.1(4) . . . . ? Re(1) P(3) C(321) C(326) 88.8(4) . . . . ? C(311) P(3) C(321) C(322) 145.2(4) . . . . ? C(2B) P(3) C(321) C(322) 40.5(5) . . . . ? Re(1) P(3) C(321) C(322) -84.7(4) . . . . ? C(326) C(321) C(322) C(323) 0.8(7) . . . . ? P(3) C(321) C(322) C(323) 174.3(4) . . . . ? C(321) C(322) C(323) C(324) -1.7(8) . . . . ? C(322) C(323) C(324) C(325) 1.0(8) . . . . ? C(323) C(324) C(325) C(326) 0.5(9) . . . . ? C(324) C(325) C(326) C(321) -1.3(9) . . . . ? C(322) C(321) C(326) C(325) 0.6(8) . . . . ? P(3) C(321) C(326) C(325) -173.1(4) . . . . ? C(421) P(4) C(411) C(412) 152.0(5) . . . . ? C(2B) P(4) C(411) C(412) 44.7(5) . . . . ? Re(5B) P(4) C(411) C(412) -76.5(5) . . . . ? C(421) P(4) C(411) C(416) -31.9(5) . . . . ? C(2B) P(4) C(411) C(416) -139.2(5) . . . . ? Re(5B) P(4) C(411) C(416) 99.6(4) . . . . ? C(416) C(411) C(412) C(413) 1.6(9) . . . . ? P(4) C(411) C(412) C(413) 177.7(5) . . . . ? C(411) C(412) C(413) C(414) -2.3(10) . . . . ? C(412) C(413) C(414) C(415) 1.5(11) . . . . ? C(413) C(414) C(415) C(416) 0.0(11) . . . . ? C(414) C(415) C(416) C(411) -0.7(10) . . . . ? C(412) C(411) C(416) C(415) -0.1(9) . . . . ? P(4) C(411) C(416) C(415) -176.3(5) . . . . ? C(2B) P(4) C(421) C(422) -141.2(4) . . . . ? C(411) P(4) C(421) C(422) 112.0(4) . . . . ? Re(5B) P(4) C(421) C(422) -23.0(5) . . . . ? C(2B) P(4) C(421) C(426) 37.3(5) . . . . ? C(411) P(4) C(421) C(426) -69.5(4) . . . . ? Re(5B) P(4) C(421) C(426) 155.5(3) . . . . ? C(426) C(421) C(422) C(423) -0.1(8) . . . . ? P(4) C(421) C(422) C(423) 178.4(4) . . . . ? C(421) C(422) C(423) C(424) -1.4(8) . . . . ? C(422) C(423) C(424) C(425) 1.0(8) . . . . ? C(423) C(424) C(425) C(426) 0.8(9) . . . . ? C(424) C(425) C(426) C(421) -2.3(8) . . . . ? C(422) C(421) C(426) C(425) 1.9(8) . . . . ? P(4) C(421) C(426) C(425) -176.6(4) . . . . ?