#Supplementary Material (ESI) for Dalton Transactions #This journal is (c) The Royal Society of Chemistry 2001 data_[ReOCl(MePO)2] JCS Dalton Submission May 7, 2001. data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Michael S. Kovacs' 'Peter Hein' 'Sherwin Sattarzadeh' 'Brian O. Patrick' 'Thomas J. Emge' 'Chris Orvig' _publ_contact_author_name 'Prof Chris Orvig' _publ_contact_author_address ; Department of Chemistry University of British Columbia 2036 Main Mall Vancouver BC V6T 1Z1 CANADA ; _publ_contact_author_email 'ORVIG@CHEM.UBC.CA' _publ_section_title ; Complexes of Phosphine-Phenolate Ligands with the [Re=O]3+ and [Re(HNNC5H4N)(NNC5H4N)]2+ Cores ; data_[ReOCl(MePO)2] _database_code_CSD 168621 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety '[ReOCl(MePO)2]' _chemical_formula_sum 'C48 H56 Cl O3 P2 Re' _chemical_formula_weight 964.52 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Re' 'Re' -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 29.3712(10) _cell_length_b 16.9227(5) _cell_length_c 17.6075(9) _cell_angle_alpha 90.00 _cell_angle_beta 105.453(2) _cell_angle_gamma 90.00 _cell_volume 8435.3(6) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 18480 _cell_measurement_theta_min 2.9 _cell_measurement_theta_max 27.9 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.519 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3920 _exptl_absorpt_coefficient_mu 3.062 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7656 _exptl_absorpt_correction_T_max 1.0000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CCD _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36637 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0840 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.90 _diffrn_reflns_theta_max 27.89 _reflns_number_total 8423 _reflns_number_gt 6071 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness 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 threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) 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_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0502P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8423 _refine_ls_number_parameters 441 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0651 _refine_ls_R_factor_gt 0.0384 _refine_ls_wR_factor_ref 0.1109 _refine_ls_wR_factor_gt 0.0995 _refine_ls_goodness_of_fit_ref 0.968 _refine_ls_restrained_S_all 0.968 _refine_ls_shift/su_max 0.975 _refine_ls_shift/su_mean 0.026 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re 0.175375(8) 0.065975(13) 0.118581(12) 0.02220(8) Uani 1 d . . . Cl1 Cl 0.11857(12) 0.1409(3) 0.03849(17) 0.1186(13) Uani 1 d . . . P1 P 0.25134(5) 0.00473(9) 0.18252(8) 0.0216(3) Uani 1 d . . . P2 P 0.12158(6) -0.03807(9) 0.13235(8) 0.0246(3) Uani 1 d . . . O1 O 0.21745(16) 0.1330(2) 0.0714(2) 0.0304(10) Uani 1 d . . . O2 O 0.17762(15) -0.0079(2) 0.0278(2) 0.0276(9) Uani 1 d . . . O3 O 0.17062(15) 0.1010(2) 0.2054(2) 0.0298(9) Uani 1 d . . . C1 C 0.2849(2) 0.0490(3) 0.1220(3) 0.0265(13) Uani 1 d . . . C2 C 0.2623(2) 0.1102(3) 0.0734(3) 0.0279(13) Uani 1 d . . . C3 C 0.2858(3) 0.1481(4) 0.0247(4) 0.0389(16) Uani 1 d . . . H3 H 0.2710 0.1886 -0.0086 0.047 Uiso 1 calc R . . C4 C 0.3310(3) 0.1256(4) 0.0258(4) 0.0444(18) Uani 1 d . . . H4 H 0.3463 0.1521 -0.0065 0.053 Uiso 1 calc R . . C5 C 0.3548(3) 0.0645(4) 0.0735(4) 0.0411(16) Uani 1 d . . . C6 C 0.3303(2) 0.0264(4) 0.1215(4) 0.0339(14) Uani 1 d . . . H6 H 0.3447 -0.0150 0.1537 0.041 Uiso 1 calc R . . C7 C 0.4037(3) 0.0398(6) 0.0721(6) 0.069(3) Uani 1 d . . . H7A H 0.4144 0.0727 0.0359 0.103 Uiso 1 calc R . . H7B H 0.4032 -0.0143 0.0555 0.103 Uiso 1 calc R . . H7C H 0.4247 0.0452 0.1239 0.103 Uiso 1 calc R . . C8 C 0.2753(2) 0.0409(3) 0.2823(3) 0.0239(12) Uani 1 d . . . C9 C 0.3130(2) 0.0935(4) 0.3013(4) 0.0327(14) Uani 1 d . . . H9 H 0.3273 0.1101 0.2628 0.039 Uiso 1 calc R . . C10 C 0.3294(3) 0.1213(5) 0.3782(4) 0.0438(18) Uani 1 d . . . H10 H 0.3543 0.1570 0.3906 0.053 Uiso 1 calc R . . C11 C 0.3092(3) 0.0968(4) 0.4359(4) 0.0417(17) Uani 1 d . . . H11 H 0.3207 0.1154 0.4871 0.050 Uiso 1 calc R . . C12 C 0.2712(2) 0.0435(4) 0.4176(4) 0.0346(15) Uani 1 d . . . H12 H 0.2578 0.0258 0.4568 0.042 Uiso 1 calc R . . C13 C 0.2539(2) 0.0174(3) 0.3411(3) 0.0272(13) Uani 1 d . . . H13 H 0.2278 -0.0159 0.3283 0.033 Uiso 1 calc R . . C14 C 0.2649(2) -0.1004(4) 0.1859(3) 0.0243(12) Uani 1 d . . . C15 C 0.2829(3) -0.1403(4) 0.2558(4) 0.0383(17) Uani 1 d . . . H15 H 0.2902 -0.1128 0.3033 0.046 Uiso 1 calc R . . C16 C 0.2902(3) -0.2215(4) 0.2557(4) 0.0409(17) Uani 1 d . . . H16 H 0.3022 -0.2482 0.3030 0.049 Uiso 1 calc R . . C17 C 0.2797(3) -0.2625(4) 0.1856(4) 0.0361(15) Uani 1 d . . . H17 H 0.2844 -0.3168 0.1853 0.043 Uiso 1 calc R . . C18 C 0.2620(3) -0.2220(4) 0.1156(4) 0.0362(16) Uani 1 d . . . H18 H 0.2549 -0.2494 0.0681 0.043 Uiso 1 calc R . . C19 C 0.2549(2) -0.1414(3) 0.1154(3) 0.0265(13) Uani 1 d . . . H19 H 0.2434 -0.1147 0.0680 0.032 Uiso 1 calc R . . C20 C 0.1237(2) -0.1024(4) 0.0533(3) 0.0282(13) Uani 1 d . . . C21 C 0.1532(2) -0.0747(4) 0.0083(3) 0.0278(13) Uani 1 d . . . C22 C 0.1563(2) -0.1185(4) -0.0580(4) 0.0365(16) Uani 1 d . . . H22 H 0.1754 -0.1007 -0.0890 0.044 Uiso 1 calc R . . C23 C 0.1313(2) -0.1871(4) -0.0770(4) 0.0420(18) Uani 1 d . . . H23 H 0.1331 -0.2146 -0.1218 0.050 Uiso 1 calc R . . C24 C 0.1031(3) -0.2174(4) -0.0315(4) 0.0430(18) Uani 1 d . . . C25 C 0.0995(2) -0.1744(4) 0.0330(4) 0.0358(15) Uani 1 d . . . H25 H 0.0806 -0.1933 0.0639 0.043 Uiso 1 calc R . . C26 C 0.0763(3) -0.2944(5) -0.0541(5) 0.070(3) Uani 1 d . . . H26A H 0.0588 -0.3062 -0.0165 0.105 Uiso 1 calc R . . H26B H 0.0983 -0.3363 -0.0544 0.105 Uiso 1 calc R . . H26C H 0.0549 -0.2892 -0.1056 0.105 Uiso 1 calc R . . C27A C 0.0606(2) -0.0051(5) 0.1232(5) 0.0305(19) Uani 0.722(9) d PG A 1 C28A C 0.0535(2) 0.0684(4) 0.1532(6) 0.064(4) Uani 0.722(9) d PG A 1 H28A H 0.0791 0.1014 0.1740 0.077 Uiso 0.722(9) calc PR A 1 C29A C 0.0081(3) 0.0927(5) 0.1520(6) 0.076(4) Uani 0.722(9) d PG A 1 H29A H 0.0033 0.1419 0.1721 0.092 Uiso 0.722(9) calc PR A 1 C30A C -0.0302(2) 0.0433(6) 0.1208(6) 0.065(4) Uani 0.722(9) d PG A 1 H30A H -0.0605 0.0595 0.1201 0.078 Uiso 0.722(9) calc PR A 1 C31A C -0.0230(2) -0.0302(6) 0.0908(6) 0.080(5) Uani 0.722(9) d PG A 1 H31A H -0.0486 -0.0632 0.0700 0.095 Uiso 0.722(9) calc PR A 1 C32A C 0.0224(3) -0.0545(5) 0.0920(6) 0.071(4) Uani 0.722(9) d PG A 1 H32A H 0.0272 -0.1037 0.0719 0.085 Uiso 0.722(9) calc PR A 1 C27B C 0.0610(6) -0.0204(14) 0.1273(15) 0.0305(19) Uani 0.278(9) d PG A 2 C28B C 0.0438(8) 0.0531(13) 0.0981(16) 0.064(4) Uani 0.278(9) d PG A 2 H28B H 0.0635 0.0890 0.0824 0.077 Uiso 0.278(9) calc PR A 2 C29B C -0.0030(8) 0.0730(14) 0.0923(17) 0.076(4) Uani 0.278(9) d PG A 2 H29B H -0.0145 0.1222 0.0728 0.092 Uiso 0.278(9) calc PR A 2 C30B C -0.0324(6) 0.0194(17) 0.1157(17) 0.065(4) Uani 0.278(9) d PG A 2 H30B H -0.0637 0.0327 0.1118 0.078 Uiso 0.278(9) calc PR A 2 C31B C -0.0151(7) -0.0542(15) 0.1449(17) 0.080(5) Uani 0.278(9) d PG A 2 H31B H -0.0348 -0.0901 0.1605 0.095 Uiso 0.278(9) calc PR A 2 C32B C 0.0316(7) -0.0741(12) 0.1507(16) 0.071(4) Uani 0.278(9) d PG A 2 H32B H 0.0432 -0.1233 0.1702 0.085 Uiso 0.278(9) calc PR A 2 C33 C 0.1388(2) -0.0941(4) 0.2236(3) 0.0259(12) Uani 1 d . . . C34 C 0.1631(2) -0.1642(4) 0.2302(3) 0.0323(14) Uani 1 d . . . H34 H 0.1697 -0.1864 0.1860 0.039 Uiso 1 calc R . . C35 C 0.1778(3) -0.2020(5) 0.3026(4) 0.0446(17) Uani 1 d . . . H35 H 0.1944 -0.2493 0.3067 0.054 Uiso 1 calc R . . C36 C 0.1679(3) -0.1699(4) 0.3681(4) 0.0424(17) Uani 1 d . . . H36 H 0.1771 -0.1960 0.4163 0.051 Uiso 1 calc R . . C37 C 0.1442(3) -0.0985(5) 0.3620(4) 0.0431(17) Uani 1 d . . . H37 H 0.1386 -0.0759 0.4068 0.052 Uiso 1 calc R . . C38 C 0.1290(2) -0.0608(4) 0.2912(3) 0.0352(14) Uani 1 d . . . H38 H 0.1124 -0.0136 0.2874 0.042 Uiso 1 calc R . . C39 C 0.0565(12) 0.269(2) 0.2228(17) 0.275(14) Uiso 1 d . B 3 H39A H 0.0766 0.2251 0.2435 0.413 Uiso 1 calc . C 3 H39B H 0.0300 0.2508 0.1817 0.413 Uiso 1 calc . D 3 H39C H 0.0454 0.2926 0.2641 0.413 Uiso 1 calc . E 3 C40 C 0.0842(15) 0.330(3) 0.189(3) 0.333(19) Uiso 1 d D B 3 H40A H 0.1059 0.3005 0.1672 0.400 Uiso 1 calc . F 3 H40B H 0.1036 0.3586 0.2342 0.400 Uiso 1 calc . G 3 C41 C 0.062(2) 0.396(4) 0.126(3) 0.46(3) Uiso 1 d D B 3 H41A H 0.0303 0.3815 0.0957 0.554 Uiso 1 calc . H 3 H41B H 0.0815 0.4056 0.0904 0.554 Uiso 1 calc . I 3 C42 C 0.0618(14) 0.472(3) 0.186(3) 0.331(18) Uiso 1 d . B 3 H42A H 0.0932 0.4880 0.2156 0.398 Uiso 1 calc . J 3 H42B H 0.0415 0.4640 0.2205 0.398 Uiso 1 calc . K 3 C43 C 0.0388(14) 0.529(3) 0.111(3) 0.342(19) Uiso 1 d . B 3 H43A H 0.0346 0.5814 0.1295 0.512 Uiso 1 calc . L 3 H43B H 0.0087 0.5085 0.0821 0.512 Uiso 1 calc . M 3 H43C H 0.0595 0.5317 0.0770 0.512 Uiso 1 calc . N 3 C44 C 0.0326(17) 0.272(3) -0.029(3) 0.42(2) Uiso 1 d . O 4 H44A H 0.0076 0.2840 -0.0051 0.636 Uiso 1 calc . P 4 H44B H 0.0561 0.3131 -0.0163 0.636 Uiso 1 calc . Q 4 H44C H 0.0467 0.2225 -0.0097 0.636 Uiso 1 calc . R 4 C45 C 0.0092(14) 0.267(2) -0.133(2) 0.335(18) Uiso 1 d D O 4 H45A H -0.0150 0.2265 -0.1419 0.402 Uiso 1 calc . S 4 H45B H -0.0073 0.3166 -0.1481 0.402 Uiso 1 calc . T 4 C46 C 0.0384(13) 0.251(2) -0.199(2) 0.327(19) Uiso 1 d D O 4 H46A H 0.0702 0.2391 -0.1677 0.393 Uiso 1 calc . U 4 H46B H 0.0258 0.2011 -0.2227 0.393 Uiso 1 calc . V 4 C47 C 0.0450(13) 0.290(2) -0.256(2) 0.287(16) Uiso 1 d D O 4 H47A H 0.0120 0.3006 -0.2825 0.344 Uiso 1 calc . W 4 H47B H 0.0528 0.2461 -0.2858 0.344 Uiso 1 calc . X 4 C48 C 0.0677(13) 0.361(2) -0.300(2) 0.297(15) Uiso 1 d D O 4 H48A H 0.0642 0.3469 -0.3540 0.446 Uiso 1 calc . Y 4 H48B H 0.1006 0.3667 -0.2736 0.446 Uiso 1 calc . Z 4 H48C H 0.0515 0.4095 -0.2973 0.446 Uiso 1 calc . A 4 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.03091(13) 0.01605(12) 0.01820(11) -0.00067(9) 0.00405(8) 0.00509(11) Cl1 0.086(2) 0.202(4) 0.0636(17) -0.003(2) 0.0132(15) 0.000(2) P1 0.0264(8) 0.0163(7) 0.0201(7) -0.0007(5) 0.0029(6) 0.0015(6) P2 0.0272(8) 0.0255(8) 0.0191(7) -0.0014(5) 0.0025(6) 0.0017(6) O1 0.045(3) 0.021(2) 0.026(2) 0.0028(16) 0.0105(18) 0.004(2) O2 0.033(2) 0.029(2) 0.022(2) -0.0070(16) 0.0088(17) 0.0007(19) O3 0.040(3) 0.021(2) 0.027(2) -0.0069(16) 0.0070(18) 0.0038(19) C1 0.033(3) 0.022(3) 0.026(3) -0.006(2) 0.010(2) -0.005(2) C2 0.034(4) 0.020(3) 0.029(3) -0.003(2) 0.008(2) -0.005(3) C3 0.054(5) 0.031(4) 0.034(4) 0.002(3) 0.016(3) -0.003(3) C4 0.056(5) 0.037(4) 0.048(4) 0.003(3) 0.028(4) -0.010(4) C5 0.041(4) 0.042(4) 0.045(4) -0.004(3) 0.019(3) -0.004(4) C6 0.033(4) 0.027(3) 0.040(4) 0.001(3) 0.007(3) -0.002(3) C7 0.045(5) 0.080(7) 0.091(7) 0.005(5) 0.036(5) 0.004(5) C8 0.024(3) 0.020(3) 0.023(3) -0.001(2) -0.001(2) 0.002(2) C9 0.040(4) 0.029(3) 0.028(3) -0.001(2) 0.007(3) -0.007(3) C10 0.047(4) 0.047(4) 0.031(3) -0.010(3) -0.002(3) -0.015(4) C11 0.053(5) 0.042(4) 0.022(3) -0.007(3) -0.005(3) -0.003(3) C12 0.044(4) 0.031(4) 0.027(3) 0.003(2) 0.006(3) 0.009(3) C13 0.032(3) 0.022(3) 0.026(3) 0.002(2) 0.004(2) 0.000(3) C14 0.025(3) 0.023(3) 0.024(3) 0.002(2) 0.005(2) 0.007(3) C15 0.058(5) 0.023(3) 0.025(3) -0.002(2) -0.002(3) 0.010(3) C16 0.063(5) 0.027(4) 0.026(3) 0.003(2) 0.000(3) 0.013(3) C17 0.053(5) 0.020(3) 0.033(3) 0.000(2) 0.009(3) 0.009(3) C18 0.060(5) 0.023(3) 0.025(3) -0.005(2) 0.010(3) 0.007(3) C19 0.039(4) 0.022(3) 0.019(3) -0.001(2) 0.006(2) 0.008(3) C20 0.028(3) 0.028(3) 0.023(3) -0.006(2) -0.004(2) -0.001(3) C21 0.030(3) 0.026(4) 0.024(3) -0.010(2) 0.003(2) 0.003(3) C22 0.037(4) 0.040(4) 0.032(3) -0.017(3) 0.010(3) 0.006(3) C23 0.039(4) 0.044(4) 0.037(4) -0.024(3) 0.001(3) 0.007(3) C24 0.038(4) 0.034(4) 0.045(4) -0.015(3) -0.009(3) 0.002(3) C25 0.039(4) 0.029(4) 0.032(3) 0.000(3) -0.003(3) -0.001(3) C26 0.083(7) 0.043(5) 0.063(5) -0.016(4) -0.016(5) -0.022(5) C27A 0.036(4) 0.034(5) 0.019(3) 0.008(3) 0.003(2) 0.010(3) C28A 0.054(7) 0.038(6) 0.111(11) -0.009(7) 0.039(8) 0.007(5) C29A 0.044(7) 0.075(9) 0.120(13) 0.007(9) 0.039(8) 0.021(7) C30A 0.033(5) 0.099(12) 0.063(6) 0.020(7) 0.012(4) 0.024(6) C31A 0.030(6) 0.099(12) 0.105(12) -0.014(10) 0.011(7) 0.005(7) C32A 0.026(6) 0.077(9) 0.099(10) -0.009(8) 0.000(6) -0.010(6) C27B 0.036(4) 0.034(5) 0.019(3) 0.008(3) 0.003(2) 0.010(3) C28B 0.054(7) 0.038(6) 0.111(11) -0.009(7) 0.039(8) 0.007(5) C29B 0.044(7) 0.075(9) 0.120(13) 0.007(9) 0.039(8) 0.021(7) C30B 0.033(5) 0.099(12) 0.063(6) 0.020(7) 0.012(4) 0.024(6) C31B 0.030(6) 0.099(12) 0.105(12) -0.014(10) 0.011(7) 0.005(7) C32B 0.026(6) 0.077(9) 0.099(10) -0.009(8) 0.000(6) -0.010(6) C33 0.026(3) 0.026(3) 0.025(3) 0.000(2) 0.005(2) -0.003(3) C34 0.043(4) 0.028(3) 0.024(3) 0.000(2) 0.007(3) 0.005(3) C35 0.056(5) 0.040(4) 0.034(4) 0.009(3) 0.005(3) 0.012(4) C36 0.052(5) 0.048(5) 0.027(3) 0.012(3) 0.010(3) 0.002(4) C37 0.063(5) 0.045(4) 0.023(3) -0.003(3) 0.013(3) -0.001(4) C38 0.048(4) 0.028(3) 0.029(3) 0.001(3) 0.009(3) 0.005(3) _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 Re1 O3 1.680(4) . ? Re1 O1 2.013(4) . ? Re1 O2 2.044(4) . ? Re1 Cl1 2.264(4) . ? Re1 P2 2.4207(16) . ? Re1 P1 2.4457(15) . ? P1 C1 1.797(6) . ? P1 C8 1.817(6) . ? P1 C14 1.820(6) . ? P2 C27B 1.781(15) . ? P2 C20 1.780(6) . ? P2 C33 1.818(6) . ? P2 C27A 1.840(6) . ? O1 C2 1.364(7) . ? O2 C21 1.334(7) . ? C1 C6 1.387(9) . ? C1 C2 1.395(9) . ? C2 C3 1.393(8) . ? C3 C4 1.375(10) . ? C4 C5 1.396(10) . ? C5 C6 1.406(9) . ? C5 C7 1.501(10) . ? C8 C9 1.390(9) . ? C8 C13 1.404(8) . ? C9 C10 1.393(8) . ? C10 C11 1.368(10) . ? C11 C12 1.405(10) . ? C12 C13 1.379(8) . ? C14 C19 1.384(8) . ? C14 C15 1.381(8) . ? C15 C16 1.391(9) . ? C16 C17 1.377(8) . ? C17 C18 1.385(8) . ? C18 C19 1.379(8) . ? C20 C21 1.401(9) . ? C20 C25 1.408(9) . ? C21 C22 1.407(7) . ? C22 C23 1.368(10) . ? C23 C24 1.393(10) . ? C24 C25 1.378(9) . ? C24 C26 1.518(10) . ? C27A C28A 1.3900 . ? C27A C32A 1.3900 . ? C28A C29A 1.3900 . ? C29A C30A 1.3900 . ? C30A C31A 1.3900 . ? C31A C32A 1.3900 . ? C27B C28B 1.3900 . ? C27B C32B 1.3900 . ? C28B C29B 1.3900 . ? C29B C30B 1.3900 . ? C30B C31B 1.3900 . ? C31B C32B 1.3900 . ? C33 C34 1.373(9) . ? C33 C38 1.413(8) . ? C34 C35 1.388(8) . ? C35 C36 1.375(9) . ? C36 C37 1.384(10) . ? C37 C38 1.366(9) . ? C39 C40 1.53(4) . ? C40 C41 1.58(2) . ? C41 C42 1.67(6) . ? C42 C43 1.63(5) . ? C44 C45 1.78(5) . ? C45 C46 1.641(19) . ? C46 C47 1.27(4) . ? C47 C48 1.650(19) . ? 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 O3 Re1 O1 112.71(19) . . ? O3 Re1 O2 162.78(19) . . ? O1 Re1 O2 82.58(16) . . ? O3 Re1 Cl1 98.22(17) . . ? O1 Re1 Cl1 81.87(15) . . ? O2 Re1 Cl1 91.59(15) . . ? O3 Re1 P2 87.17(15) . . ? O1 Re1 P2 160.08(12) . . ? O2 Re1 P2 77.94(12) . . ? Cl1 Re1 P2 94.44(11) . . ? O3 Re1 P1 91.00(15) . . ? O1 Re1 P1 81.02(13) . . ? O2 Re1 P1 83.40(12) . . ? Cl1 Re1 P1 162.65(10) . . ? P2 Re1 P1 100.69(5) . . ? C1 P1 C8 107.4(3) . . ? C1 P1 C14 106.1(3) . . ? C8 P1 C14 105.8(3) . . ? C1 P1 Re1 97.4(2) . . ? C8 P1 Re1 111.94(19) . . ? C14 P1 Re1 126.4(2) . . ? C27B P2 C20 107.7(8) . . ? C27B P2 C33 99.9(9) . . ? C20 P2 C33 108.2(3) . . ? C27B P2 C27A 8.3(9) . . ? C20 P2 C27A 110.6(3) . . ? C33 P2 C27A 105.8(3) . . ? C27B P2 Re1 122.9(8) . . ? C20 P2 Re1 101.9(2) . . ? C33 P2 Re1 115.6(2) . . ? C27A P2 Re1 114.6(3) . . ? C2 O1 Re1 121.6(4) . . ? C21 O2 Re1 126.3(4) . . ? C6 C1 C2 120.2(6) . . ? C6 C1 P1 124.6(5) . . ? C2 C1 P1 115.2(5) . . ? O1 C2 C3 119.2(6) . . ? O1 C2 C1 121.7(5) . . ? C3 C2 C1 119.1(6) . . ? C4 C3 C2 119.8(6) . . ? C3 C4 C5 122.8(6) . . ? C4 C5 C6 116.4(6) . . ? C4 C5 C7 121.7(7) . . ? C6 C5 C7 121.9(7) . . ? C1 C6 C5 121.6(6) . . ? C9 C8 C13 119.3(5) . . ? C9 C8 P1 121.8(4) . . ? C13 C8 P1 118.8(4) . . ? C8 C9 C10 119.8(6) . . ? C11 C10 C9 120.9(7) . . ? C10 C11 C12 119.9(6) . . ? C13 C12 C11 119.6(6) . . ? C12 C13 C8 120.5(6) . . ? C19 C14 C15 119.6(6) . . ? C19 C14 P1 118.0(4) . . ? C15 C14 P1 122.4(4) . . ? C14 C15 C16 120.3(6) . . ? C17 C16 C15 120.1(6) . . ? C16 C17 C18 119.4(6) . . ? C19 C18 C17 120.8(6) . . ? C18 C19 C14 119.9(5) . . ? C21 C20 C25 119.5(6) . . ? C21 C20 P2 113.1(4) . . ? C25 C20 P2 127.4(5) . . ? O2 C21 C20 120.6(5) . . ? O2 C21 C22 120.7(6) . . ? C20 C21 C22 118.7(6) . . ? C23 C22 C21 120.0(6) . . ? C22 C23 C24 122.4(6) . . ? C25 C24 C23 117.9(6) . . ? C25 C24 C26 121.4(8) . . ? C23 C24 C26 120.7(7) . . ? C24 C25 C20 121.5(7) . . ? C28A C27A C32A 120.0 . . ? C28A C27A P2 118.7(4) . . ? C32A C27A P2 121.2(4) . . ? C27A C28A C29A 120.0 . . ? C30A C29A C28A 120.0 . . ? C29A C30A C31A 120.0 . . ? C30A C31A C32A 120.0 . . ? C31A C32A C27A 120.0 . . ? C28B C27B C32B 120.0 . . ? C28B C27B P2 115.5(13) . . ? C32B C27B P2 124.5(13) . . ? C29B C28B C27B 120.0 . . ? C28B C29B C30B 120.0 . . ? C31B C30B C29B 120.0 . . ? C30B C31B C32B 120.0 . . ? C31B C32B C27B 120.0 . . ? C34 C33 C38 119.4(5) . . ? C34 C33 P2 122.8(4) . . ? C38 C33 P2 117.7(5) . . ? C33 C34 C35 120.2(6) . . ? C36 C35 C34 120.3(7) . . ? C35 C36 C37 119.6(6) . . ? C38 C37 C36 120.9(6) . . ? C37 C38 C33 119.5(6) . . ? C39 C40 C41 126(4) . . ? C40 C41 C42 99(4) . . ? C41 C42 C43 91(3) . . ? C46 C45 C44 127(4) . . ? C47 C46 C45 134(4) . . ? C46 C47 C48 156(4) . . ? _diffrn_measured_fraction_theta_max 0.404 _diffrn_reflns_theta_full 27.89 _diffrn_measured_fraction_theta_full 0.404 _refine_diff_density_max 1.415 _refine_diff_density_min -1.292 _refine_diff_density_rms 0.135 #===END data_[ReO(Me2PO2)(H(Me2PO2))] _database_code_CSD 168622 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety '[ReO(Me2PO2)(H(Me2PO2))]' _chemical_formula_sum 'C44 H41 N2 O5 P2 Re' _chemical_formula_weight 925.93 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Re' 'Re' -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 9.5519(3) _cell_length_b 18.9971(6) _cell_length_c 21.8244(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3960.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 20525 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.9 _exptl_crystal_description needle _exptl_crystal_colour green _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.553 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1856 _exptl_absorpt_coefficient_mu 3.197 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7617 _exptl_absorpt_correction_T_max 1.0000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CCD _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33634 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1280 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 27.94 _reflns_number_total 8541 _reflns_number_gt 6871 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness 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 threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) 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_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.012(7) _refine_ls_number_reflns 8541 _refine_ls_number_parameters 497 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0488 _refine_ls_R_factor_gt 0.0319 _refine_ls_wR_factor_ref 0.0777 _refine_ls_wR_factor_gt 0.0692 _refine_ls_goodness_of_fit_ref 0.618 _refine_ls_restrained_S_all 0.618 _refine_ls_shift/su_max 0.274 _refine_ls_shift/su_mean 0.005 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re 0.03394(2) 0.988023(12) 0.091933(10) 0.01200(6) Uani 1 d . . . P1 P 0.14452(15) 1.09650(8) 0.06129(7) 0.0112(3) Uani 1 d . . . P2 P 0.14763(15) 0.94658(8) 0.18629(7) 0.0124(3) Uani 1 d . . . O1 O 0.2241(4) 0.9589(2) 0.05826(18) 0.0135(8) Uani 1 d . . . O2 O -0.0375(4) 0.9904(2) 0.00490(16) 0.0187(7) Uani 1 d . . . O3 O -0.0149(4) 0.88590(19) 0.08392(19) 0.0184(9) Uani 1 d . . . O4 O 0.3371(5) 1.0638(2) 0.2198(2) 0.0285(11) Uani 1 d . . . O5 O -0.0941(4) 1.0295(2) 0.1290(2) 0.0193(10) Uani 1 d . . . N1 N -0.1052(10) 0.7296(5) -0.0421(4) 0.059(2) Uani 1 d . . . N2 N 0.0653(13) 0.8781(5) -0.1694(4) 0.082(3) Uani 1 d . . . C1 C 0.3392(5) 0.9995(3) 0.0537(2) 0.0131(13) Uani 1 d . . . C2 C 0.3249(6) 1.0724(3) 0.0555(3) 0.0128(12) Uani 1 d . . . C3 C 0.4407(5) 1.1164(3) 0.0498(3) 0.0115(12) Uani 1 d . . . H3 H 0.4286 1.1649 0.0498 0.014 Uiso 1 calc R . . C4 C 0.5755(6) 1.0879(3) 0.0440(3) 0.0163(13) Uani 1 d . . . C5 C 0.5871(6) 1.0138(4) 0.0419(3) 0.0168(12) Uani 1 d . . . H5 H 0.6754 0.9939 0.0373 0.020 Uiso 1 calc R . . C6 C 0.4732(7) 0.9700(3) 0.0463(3) 0.0160(12) Uani 1 d . . . H6 H 0.4845 0.9214 0.0444 0.019 Uiso 1 calc R . . C7 C 0.7023(7) 1.1337(4) 0.0381(4) 0.0294(16) Uani 1 d . . . H7A H 0.6742 1.1822 0.0370 0.044 Uiso 1 calc R . . H7B H 0.7510 1.1222 0.0009 0.044 Uiso 1 calc R . . H7C H 0.7631 1.1260 0.0725 0.044 Uiso 1 calc R . . C8 C -0.0070(6) 1.0444(3) -0.0333(3) 0.0166(13) Uani 1 d . . . C9 C 0.0760(5) 1.1008(3) -0.0156(3) 0.0128(12) Uani 1 d . . . C10 C 0.1048(6) 1.1551(3) -0.0573(3) 0.0163(13) Uani 1 d . . . H10 H 0.1617 1.1923 -0.0452 0.020 Uiso 1 calc R . . C11 C 0.0505(7) 1.1547(3) -0.1164(3) 0.0184(13) Uani 1 d . . . C12 C -0.0322(8) 1.0975(3) -0.1333(3) 0.0266(13) Uani 1 d . . . H12 H -0.0701 1.0960 -0.1725 0.032 Uiso 1 calc R . . C13 C -0.0591(6) 1.0431(3) -0.0932(3) 0.0236(13) Uani 1 d . . . H13 H -0.1124 1.0049 -0.1062 0.028 Uiso 1 calc R . . C14 C 0.0778(7) 1.2146(4) -0.1602(4) 0.0317(17) Uani 1 d . . . H14A H 0.0122 1.2519 -0.1526 0.048 Uiso 1 calc R . . H14B H 0.0673 1.1982 -0.2016 0.048 Uiso 1 calc R . . H14C H 0.1714 1.2318 -0.1544 0.048 Uiso 1 calc R . . C15 C 0.1265(5) 1.1827(3) 0.0952(3) 0.0140(11) Uani 1 d . . . C16 C 0.2098(7) 1.2006(4) 0.1452(3) 0.0241(14) Uani 1 d . . . H16 H 0.2744 1.1685 0.1606 0.029 Uiso 1 calc R . . C17 C 0.1961(8) 1.2668(4) 0.1722(3) 0.0296(16) Uani 1 d . . . H17 H 0.2525 1.2789 0.2054 0.036 Uiso 1 calc R . . C18 C 0.1003(8) 1.3143(4) 0.1503(3) 0.0286(16) Uani 1 d . . . H18 H 0.0917 1.3583 0.1686 0.034 Uiso 1 calc R . . C19 C 0.0152(7) 1.2965(3) 0.1003(3) 0.0265(15) Uani 1 d . . . H19 H -0.0492 1.3288 0.0851 0.032 Uiso 1 calc R . . C20 C 0.0274(7) 1.2308(3) 0.0736(3) 0.0181(12) Uani 1 d . . . H20 H -0.0306 1.2186 0.0411 0.022 Uiso 1 calc R . . C21 C 0.0229(7) 0.8379(3) 0.1265(3) 0.0161(12) Uani 1 d . . . C22 C 0.0940(6) 0.8563(3) 0.1804(3) 0.0151(12) Uani 1 d . . . C23 C 0.1223(6) 0.8047(3) 0.2242(3) 0.0193(13) Uani 1 d . . . H23 H 0.1695 0.8173 0.2599 0.023 Uiso 1 calc R . . C24 C 0.0817(7) 0.7347(3) 0.2160(3) 0.0225(14) Uani 1 d . . . C25 C 0.0135(7) 0.7177(3) 0.1614(3) 0.0244(15) Uani 1 d . . . H25 H -0.0130 0.6713 0.1547 0.029 Uiso 1 calc R . . C26 C -0.0162(7) 0.7672(3) 0.1170(3) 0.0208(13) Uani 1 d . . . H26 H -0.0616 0.7540 0.0811 0.025 Uiso 1 calc R . . C27 C 0.1121(8) 0.6801(4) 0.2639(4) 0.0338(18) Uani 1 d . . . H27A H 0.1914 0.6525 0.2515 0.051 Uiso 1 calc R . . H27B H 0.0321 0.6500 0.2687 0.051 Uiso 1 calc R . . H27C H 0.1323 0.7029 0.3021 0.051 Uiso 1 calc R . . C28 C 0.4121(6) 1.0035(3) 0.2075(3) 0.0186(14) Uani 1 d . . . C29 C 0.3382(7) 0.9440(3) 0.1904(3) 0.0163(13) Uani 1 d . . . C30 C 0.4112(6) 0.8824(3) 0.1751(3) 0.0173(13) Uani 1 d . . . H30 H 0.3619 0.8426 0.1629 0.021 Uiso 1 calc R . . C31 C 0.5584(7) 0.8802(4) 0.1779(3) 0.0242(15) Uani 1 d . . . C32 C 0.6272(7) 0.9414(4) 0.1955(3) 0.0266(17) Uani 1 d . . . H32 H 0.7245 0.9411 0.1976 0.032 Uiso 1 calc R . . C33 C 0.5579(6) 1.0021(4) 0.2100(3) 0.0253(16) Uani 1 d . . . H33 H 0.6076 1.0422 0.2213 0.030 Uiso 1 calc R . . C34 C 0.6357(8) 0.8140(5) 0.1601(4) 0.043(2) Uani 1 d . . . H34A H 0.6432 0.8116 0.1163 0.064 Uiso 1 calc R . . H34B H 0.5854 0.7737 0.1749 0.064 Uiso 1 calc R . . H34C H 0.7277 0.8147 0.1778 0.064 Uiso 1 calc R . . C35 C 0.0901(6) 0.9735(3) 0.2623(3) 0.0164(13) Uani 1 d . . . C36 C -0.0411(7) 1.0022(3) 0.2704(3) 0.0183(13) Uani 1 d . . . H36 H -0.0968 1.0111 0.2363 0.022 Uiso 1 calc R . . C37 C -0.0920(7) 1.0181(4) 0.3282(3) 0.0276(14) Uani 1 d . . . H37 H -0.1807 1.0376 0.3328 0.033 Uiso 1 calc R . . C38 C -0.0091(7) 1.0046(3) 0.3797(3) 0.0316(17) Uani 1 d . . . H38 H -0.0426 1.0147 0.4187 0.038 Uiso 1 calc R . . C39 C 0.1230(7) 0.9762(4) 0.3721(3) 0.0310(17) Uani 1 d . . . H39 H 0.1787 0.9675 0.4062 0.037 Uiso 1 calc R . . C40 C 0.1730(7) 0.9607(4) 0.3142(3) 0.0232(14) Uani 1 d . . . H40 H 0.2621 0.9416 0.3096 0.028 Uiso 1 calc R . . C41 C -0.1695(10) 0.7800(5) -0.0399(4) 0.043(2) Uani 1 d . . . C42 C -0.2491(11) 0.8446(5) -0.0340(6) 0.063(3) Uani 1 d . . . H42A H -0.3264 0.8371 -0.0067 0.095 Uiso 1 calc R . . H42B H -0.2837 0.8584 -0.0735 0.095 Uiso 1 calc R . . H42C H -0.1899 0.8810 -0.0180 0.095 Uiso 1 calc R . . C43 C 0.1105(10) 0.8712(4) -0.1217(4) 0.043(2) Uani 1 d . . . C44 C 0.1664(10) 0.8624(5) -0.0621(4) 0.046(2) Uani 1 d . . . H44A H 0.2611 0.8794 -0.0612 0.069 Uiso 1 calc R . . H44B H 0.1651 0.8134 -0.0513 0.069 Uiso 1 calc R . . H44C H 0.1110 0.8885 -0.0332 0.069 Uiso 1 calc R . . H35 H 0.377(12) 1.094(6) 0.263(6) 0.11(4) Uiso 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.01077(8) 0.01312(9) 0.01211(9) -0.00022(10) -0.00179(10) -0.00147(9) P1 0.0088(7) 0.0125(8) 0.0123(7) -0.0018(6) -0.0006(5) 0.0010(5) P2 0.0136(7) 0.0108(8) 0.0128(8) -0.0007(6) -0.0023(6) -0.0014(5) O1 0.0124(19) 0.013(2) 0.016(2) -0.0060(17) 0.0017(16) -0.0018(15) O2 0.0178(17) 0.0172(19) 0.0210(19) -0.0019(17) -0.0032(18) -0.005(2) O3 0.023(2) 0.0169(19) 0.015(2) 0.0011(16) -0.0047(18) -0.0032(15) O4 0.035(3) 0.015(2) 0.035(3) 0.001(2) 0.001(2) -0.0066(19) O5 0.019(2) 0.018(3) 0.021(2) 0.0019(18) -0.0025(18) 0.0043(16) N1 0.076(6) 0.054(5) 0.048(5) -0.011(4) 0.002(4) -0.001(4) N2 0.153(11) 0.053(5) 0.041(5) 0.014(4) -0.004(6) -0.013(6) C1 0.014(2) 0.019(4) 0.006(2) -0.002(2) 0.0028(19) -0.003(2) C2 0.013(3) 0.014(3) 0.011(3) -0.002(2) -0.001(2) 0.001(2) C3 0.007(3) 0.011(3) 0.017(3) -0.001(2) -0.003(2) 0.002(2) C4 0.012(3) 0.021(3) 0.016(3) 0.004(3) -0.002(2) 0.000(2) C5 0.008(2) 0.027(3) 0.016(3) 0.005(3) 0.000(2) 0.002(3) C6 0.017(3) 0.014(3) 0.016(3) 0.000(2) -0.005(3) 0.004(3) C7 0.020(3) 0.023(4) 0.045(5) 0.005(3) 0.003(3) 0.000(3) C8 0.019(3) 0.017(3) 0.013(3) 0.002(2) 0.001(2) 0.004(2) C9 0.011(3) 0.011(3) 0.016(3) -0.003(2) -0.001(2) 0.0041(19) C10 0.016(3) 0.020(3) 0.012(3) -0.002(2) 0.001(2) 0.005(2) C11 0.020(3) 0.021(3) 0.014(3) 0.005(2) 0.007(3) 0.008(3) C12 0.037(3) 0.033(4) 0.010(3) -0.002(2) -0.007(3) 0.006(4) C13 0.032(4) 0.023(3) 0.016(3) 0.003(3) -0.014(3) -0.001(2) C14 0.032(4) 0.033(4) 0.030(4) 0.009(3) -0.001(3) 0.003(3) C15 0.009(2) 0.016(3) 0.017(3) -0.001(3) 0.001(2) -0.0004(18) C16 0.028(3) 0.023(4) 0.022(4) -0.004(3) -0.011(3) 0.003(3) C17 0.031(4) 0.030(4) 0.028(4) -0.013(3) -0.005(3) 0.003(3) C18 0.033(4) 0.019(4) 0.034(4) -0.010(3) 0.002(3) -0.001(3) C19 0.029(3) 0.019(3) 0.032(4) 0.002(3) 0.002(3) 0.007(2) C20 0.023(3) 0.014(3) 0.018(3) -0.004(2) 0.004(3) 0.005(3) C21 0.017(3) 0.014(3) 0.018(3) -0.004(2) -0.002(3) -0.001(3) C22 0.015(3) 0.014(3) 0.017(3) 0.000(2) 0.000(2) -0.002(2) C23 0.023(3) 0.015(3) 0.020(3) 0.000(3) 0.000(3) 0.001(2) C24 0.026(3) 0.013(3) 0.028(4) 0.003(3) 0.001(3) 0.000(2) C25 0.030(4) 0.014(3) 0.029(4) -0.006(3) 0.003(3) -0.004(3) C26 0.024(3) 0.015(3) 0.023(3) -0.007(2) -0.002(3) -0.008(2) C27 0.042(4) 0.018(4) 0.042(5) 0.003(3) -0.007(4) -0.004(3) C28 0.027(3) 0.016(4) 0.013(3) 0.005(2) -0.004(2) 0.002(2) C29 0.022(3) 0.011(3) 0.016(3) 0.004(2) -0.001(2) 0.001(2) C30 0.012(3) 0.022(3) 0.018(3) 0.000(3) -0.002(2) -0.004(2) C31 0.016(4) 0.030(4) 0.027(4) 0.002(3) -0.001(3) 0.004(3) C32 0.013(3) 0.049(5) 0.018(4) 0.003(3) 0.001(3) -0.003(3) C33 0.016(3) 0.033(5) 0.027(3) -0.004(3) -0.001(2) -0.012(3) C34 0.034(4) 0.047(5) 0.047(5) -0.007(4) -0.001(4) 0.015(4) C35 0.020(3) 0.014(4) 0.015(3) 0.004(2) 0.001(2) -0.006(2) C36 0.026(3) 0.015(4) 0.014(2) -0.002(2) 0.003(3) 0.003(3) C37 0.035(3) 0.028(4) 0.020(3) -0.004(3) 0.011(3) -0.003(3) C38 0.056(5) 0.025(4) 0.014(3) -0.003(3) 0.011(3) -0.006(3) C39 0.043(4) 0.033(5) 0.017(3) 0.003(3) -0.007(3) -0.005(3) C40 0.029(3) 0.023(3) 0.017(3) 0.001(3) -0.005(3) -0.004(3) C41 0.059(6) 0.042(5) 0.028(5) -0.005(4) 0.000(4) -0.002(4) C42 0.054(6) 0.051(6) 0.086(9) -0.011(6) -0.023(6) 0.001(5) C43 0.068(6) 0.022(4) 0.039(5) 0.007(4) 0.015(5) 0.000(4) C44 0.051(6) 0.046(6) 0.041(5) -0.012(4) 0.004(4) -0.002(4) _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 Re1 O5 1.665(4) . ? Re1 O3 2.003(4) . ? Re1 O2 2.019(4) . ? Re1 O1 2.036(4) . ? Re1 P1 2.4103(15) . ? Re1 P2 2.4577(15) . ? P1 C2 1.787(6) . ? P1 C9 1.803(6) . ? P1 C15 1.804(6) . ? P2 C22 1.795(6) . ? P2 C35 1.820(6) . ? P2 C29 1.823(7) . ? O1 C1 1.346(6) . ? O2 C8 1.353(7) . ? O3 C21 1.351(7) . ? O4 C28 1.377(8) . ? N1 C41 1.138(11) . ? N2 C43 1.133(12) . ? C1 C2 1.393(9) . ? C1 C6 1.407(8) . ? C2 C3 1.391(8) . ? C3 C4 1.402(7) . ? C4 C5 1.413(10) . ? C4 C7 1.497(9) . ? C5 C6 1.373(8) . ? C8 C9 1.387(8) . ? C8 C13 1.400(8) . ? C9 C10 1.404(8) . ? C10 C11 1.390(8) . ? C11 C12 1.393(9) . ? C11 C14 1.509(9) . ? C12 C13 1.379(9) . ? C15 C16 1.394(9) . ? C15 C20 1.398(8) . ? C16 C17 1.395(9) . ? C17 C18 1.371(10) . ? C18 C19 1.402(10) . ? C19 C20 1.382(8) . ? C21 C22 1.403(8) . ? C21 C26 1.409(8) . ? C22 C23 1.396(9) . ? C23 C24 1.397(9) . ? C24 C25 1.395(9) . ? C24 C27 1.501(9) . ? C25 C26 1.379(9) . ? C28 C29 1.385(9) . ? C28 C33 1.394(8) . ? C29 C30 1.402(9) . ? C30 C31 1.408(8) . ? C31 C32 1.391(10) . ? C31 C34 1.509(10) . ? C32 C33 1.366(10) . ? C35 C36 1.378(8) . ? C35 C40 1.404(8) . ? C36 C37 1.386(8) . ? C37 C38 1.397(9) . ? C38 C39 1.382(10) . ? C39 C40 1.384(9) . ? C41 C42 1.448(13) . ? C43 C44 1.418(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Re1 O3 109.26(19) . . ? O5 Re1 O2 101.46(18) . . ? O3 Re1 O2 82.00(16) . . ? O5 Re1 O1 163.62(17) . . ? O3 Re1 O1 85.00(16) . . ? O2 Re1 O1 88.17(16) . . ? O5 Re1 P1 92.98(15) . . ? O3 Re1 P1 154.96(13) . . ? O2 Re1 P1 82.41(12) . . ? O1 Re1 P1 75.02(12) . . ? O5 Re1 P2 93.94(15) . . ? O3 Re1 P2 82.29(12) . . ? O2 Re1 P2 160.90(12) . . ? O1 Re1 P2 79.70(12) . . ? P1 Re1 P2 108.22(5) . . ? C2 P1 C9 107.2(3) . . ? C2 P1 C15 110.7(3) . . ? C9 P1 C15 107.8(3) . . ? C2 P1 Re1 102.9(2) . . ? C9 P1 Re1 97.93(19) . . ? C15 P1 Re1 128.3(2) . . ? C22 P2 C35 104.4(3) . . ? C22 P2 C29 105.2(3) . . ? C35 P2 C29 105.3(3) . . ? C22 P2 Re1 96.9(2) . . ? C35 P2 Re1 122.7(2) . . ? C29 P2 Re1 119.4(2) . . ? C1 O1 Re1 126.8(3) . . ? C8 O2 Re1 121.5(3) . . ? C21 O3 Re1 122.1(3) . . ? O1 C1 C2 119.2(5) . . ? O1 C1 C6 121.5(5) . . ? C2 C1 C6 119.2(5) . . ? C3 C2 C1 121.1(5) . . ? C3 C2 P1 128.2(5) . . ? C1 C2 P1 110.5(4) . . ? C2 C3 C4 120.4(5) . . ? C3 C4 C5 117.3(5) . . ? C3 C4 C7 121.8(6) . . ? C5 C4 C7 120.8(5) . . ? C6 C5 C4 122.6(5) . . ? C5 C6 C1 119.2(5) . . ? O2 C8 C9 122.5(5) . . ? O2 C8 C13 119.0(5) . . ? C9 C8 C13 118.5(5) . . ? C8 C9 C10 119.9(5) . . ? C8 C9 P1 115.5(4) . . ? C10 C9 P1 124.5(5) . . ? C11 C10 C9 121.7(6) . . ? C10 C11 C12 117.5(6) . . ? C10 C11 C14 121.3(6) . . ? C12 C11 C14 121.3(6) . . ? C13 C12 C11 121.5(6) . . ? C12 C13 C8 120.8(6) . . ? C16 C15 C20 119.3(5) . . ? C16 C15 P1 119.3(4) . . ? C20 C15 P1 121.4(5) . . ? C15 C16 C17 119.9(6) . . ? C18 C17 C16 120.5(7) . . ? C17 C18 C19 120.0(6) . . ? C20 C19 C18 119.7(6) . . ? C19 C20 C15 120.4(6) . . ? O3 C21 C22 122.6(5) . . ? O3 C21 C26 118.2(5) . . ? C22 C21 C26 119.2(5) . . ? C23 C22 C21 119.6(5) . . ? C23 C22 P2 124.5(5) . . ? C21 C22 P2 115.9(4) . . ? C22 C23 C24 121.7(6) . . ? C25 C24 C23 117.4(6) . . ? C25 C24 C27 121.7(6) . . ? C23 C24 C27 120.9(6) . . ? C26 C25 C24 122.6(6) . . ? C25 C26 C21 119.5(6) . . ? O4 C28 C29 117.8(5) . . ? O4 C28 C33 121.8(6) . . ? C29 C28 C33 120.3(6) . . ? C28 C29 C30 119.5(6) . . ? C28 C29 P2 120.0(5) . . ? C30 C29 P2 120.5(5) . . ? C29 C30 C31 120.8(6) . . ? C32 C31 C30 117.3(6) . . ? C32 C31 C34 122.5(6) . . ? C30 C31 C34 120.2(7) . . ? C33 C32 C31 122.7(6) . . ? C32 C33 C28 119.4(6) . . ? C36 C35 C40 118.6(6) . . ? C36 C35 P2 120.2(4) . . ? C40 C35 P2 121.0(5) . . ? C35 C36 C37 121.5(6) . . ? C36 C37 C38 119.5(6) . . ? C39 C38 C37 119.5(6) . . ? C38 C39 C40 120.5(6) . . ? C39 C40 C35 120.3(6) . . ? N1 C41 C42 177.2(10) . . ? N2 C43 C44 179.7(12) . . ? 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 O5 Re1 P1 C2 151.1(2) . . . . ? O3 Re1 P1 C2 -55.8(3) . . . . ? O2 Re1 P1 C2 -107.8(2) . . . . ? O1 Re1 P1 C2 -17.6(2) . . . . ? P2 Re1 P1 C2 55.9(2) . . . . ? O5 Re1 P1 C9 -99.2(2) . . . . ? O3 Re1 P1 C9 53.9(3) . . . . ? O2 Re1 P1 C9 2.0(2) . . . . ? O1 Re1 P1 C9 92.1(2) . . . . ? P2 Re1 P1 C9 165.69(18) . . . . ? O5 Re1 P1 C15 21.1(3) . . . . ? O3 Re1 P1 C15 174.1(4) . . . . ? O2 Re1 P1 C15 122.2(3) . . . . ? O1 Re1 P1 C15 -147.6(3) . . . . ? P2 Re1 P1 C15 -74.1(3) . . . . ? O5 Re1 P2 C22 105.8(2) . . . . ? O3 Re1 P2 C22 -3.1(2) . . . . ? O2 Re1 P2 C22 -38.1(4) . . . . ? O1 Re1 P2 C22 -89.4(2) . . . . ? P1 Re1 P2 C22 -159.8(2) . . . . ? O5 Re1 P2 C35 -6.2(3) . . . . ? O3 Re1 P2 C35 -115.1(3) . . . . ? O2 Re1 P2 C35 -150.0(4) . . . . ? O1 Re1 P2 C35 158.6(3) . . . . ? P1 Re1 P2 C35 88.3(2) . . . . ? O5 Re1 P2 C29 -142.4(3) . . . . ? O3 Re1 P2 C29 108.7(3) . . . . ? O2 Re1 P2 C29 73.8(4) . . . . ? O1 Re1 P2 C29 22.4(3) . . . . ? P1 Re1 P2 C29 -47.9(2) . . . . ? O5 Re1 O1 C1 -21.2(9) . . . . ? O3 Re1 O1 C1 -172.5(4) . . . . ? O2 Re1 O1 C1 105.4(4) . . . . ? P1 Re1 O1 C1 22.8(4) . . . . ? P2 Re1 O1 C1 -89.4(4) . . . . ? O5 Re1 O2 C8 89.6(4) . . . . ? O3 Re1 O2 C8 -162.3(4) . . . . ? O1 Re1 O2 C8 -77.0(4) . . . . ? P1 Re1 O2 C8 -1.9(4) . . . . ? P2 Re1 O2 C8 -127.3(4) . . . . ? O5 Re1 O3 C21 -90.5(5) . . . . ? O2 Re1 O3 C21 170.1(5) . . . . ? O1 Re1 O3 C21 81.3(4) . . . . ? P1 Re1 O3 C21 118.1(4) . . . . ? P2 Re1 O3 C21 1.0(4) . . . . ? Re1 O1 C1 C2 -19.1(7) . . . . ? Re1 O1 C1 C6 161.8(4) . . . . ? O1 C1 C2 C3 -178.8(5) . . . . ? C6 C1 C2 C3 0.3(8) . . . . ? O1 C1 C2 P1 -2.0(6) . . . . ? C6 C1 C2 P1 177.1(4) . . . . ? C9 P1 C2 C3 89.6(6) . . . . ? C15 P1 C2 C3 -27.7(6) . . . . ? Re1 P1 C2 C3 -167.7(5) . . . . ? C9 P1 C2 C1 -86.8(5) . . . . ? C15 P1 C2 C1 155.8(4) . . . . ? Re1 P1 C2 C1 15.8(4) . . . . ? C1 C2 C3 C4 -2.1(9) . . . . ? P1 C2 C3 C4 -178.2(5) . . . . ? C2 C3 C4 C5 2.4(9) . . . . ? C2 C3 C4 C7 -179.7(6) . . . . ? C3 C4 C5 C6 -1.2(9) . . . . ? C7 C4 C5 C6 -179.0(6) . . . . ? C4 C5 C6 C1 -0.5(8) . . . . ? O1 C1 C6 C5 -180.0(5) . . . . ? C2 C1 C6 C5 0.9(8) . . . . ? Re1 O2 C8 C9 0.9(7) . . . . ? Re1 O2 C8 C13 179.7(4) . . . . ? O2 C8 C9 C10 179.6(5) . . . . ? C13 C8 C9 C10 0.7(8) . . . . ? O2 C8 C9 P1 1.4(7) . . . . ? C13 C8 C9 P1 -177.5(4) . . . . ? C2 P1 C9 C8 103.9(4) . . . . ? C15 P1 C9 C8 -136.9(4) . . . . ? Re1 P1 C9 C8 -2.3(4) . . . . ? C2 P1 C9 C10 -74.2(5) . . . . ? C15 P1 C9 C10 45.0(5) . . . . ? Re1 P1 C9 C10 179.6(5) . . . . ? C8 C9 C10 C11 0.9(9) . . . . ? P1 C9 C10 C11 178.9(4) . . . . ? C9 C10 C11 C12 -1.1(9) . . . . ? C9 C10 C11 C14 177.8(6) . . . . ? C10 C11 C12 C13 -0.2(10) . . . . ? C14 C11 C12 C13 -179.1(6) . . . . ? C11 C12 C13 C8 1.8(10) . . . . ? O2 C8 C13 C12 179.1(6) . . . . ? C9 C8 C13 C12 -2.0(9) . . . . ? C2 P1 C15 C16 -42.1(6) . . . . ? C9 P1 C15 C16 -159.1(5) . . . . ? Re1 P1 C15 C16 84.9(5) . . . . ? C2 P1 C15 C20 140.0(5) . . . . ? C9 P1 C15 C20 23.1(6) . . . . ? Re1 P1 C15 C20 -92.9(5) . . . . ? C20 C15 C16 C17 -1.6(10) . . . . ? P1 C15 C16 C17 -179.5(5) . . . . ? C15 C16 C17 C18 0.6(11) . . . . ? C16 C17 C18 C19 -0.1(11) . . . . ? C17 C18 C19 C20 0.6(11) . . . . ? C18 C19 C20 C15 -1.6(10) . . . . ? C16 C15 C20 C19 2.1(9) . . . . ? P1 C15 C20 C19 179.9(5) . . . . ? Re1 O3 C21 C22 2.6(8) . . . . ? Re1 O3 C21 C26 179.9(4) . . . . ? O3 C21 C22 C23 176.0(6) . . . . ? C26 C21 C22 C23 -1.2(9) . . . . ? O3 C21 C22 P2 -6.0(8) . . . . ? C26 C21 C22 P2 176.7(5) . . . . ? C35 P2 C22 C23 -50.4(6) . . . . ? C29 P2 C22 C23 60.2(6) . . . . ? Re1 P2 C22 C23 -176.7(5) . . . . ? C35 P2 C22 C21 131.7(5) . . . . ? C29 P2 C22 C21 -117.7(5) . . . . ? Re1 P2 C22 C21 5.4(5) . . . . ? C21 C22 C23 C24 0.0(9) . . . . ? P2 C22 C23 C24 -177.8(5) . . . . ? C22 C23 C24 C25 1.1(9) . . . . ? C22 C23 C24 C27 -179.5(6) . . . . ? C23 C24 C25 C26 -1.1(10) . . . . ? C27 C24 C25 C26 179.6(7) . . . . ? C24 C25 C26 C21 -0.1(10) . . . . ? O3 C21 C26 C25 -176.1(6) . . . . ? C22 C21 C26 C25 1.3(9) . . . . ? O4 C28 C29 C30 177.4(5) . . . . ? C33 C28 C29 C30 -0.6(9) . . . . ? O4 C28 C29 P2 -1.2(8) . . . . ? C33 C28 C29 P2 -179.2(5) . . . . ? C22 P2 C29 C28 -167.1(5) . . . . ? C35 P2 C29 C28 -57.1(6) . . . . ? Re1 P2 C29 C28 85.7(5) . . . . ? C22 P2 C29 C30 14.4(6) . . . . ? C35 P2 C29 C30 124.3(5) . . . . ? Re1 P2 C29 C30 -92.9(5) . . . . ? C28 C29 C30 C31 1.1(10) . . . . ? P2 C29 C30 C31 179.7(5) . . . . ? C29 C30 C31 C32 -0.9(10) . . . . ? C29 C30 C31 C34 -178.8(6) . . . . ? C30 C31 C32 C33 0.1(10) . . . . ? C34 C31 C32 C33 178.0(7) . . . . ? C31 C32 C33 C28 0.4(10) . . . . ? O4 C28 C33 C32 -178.0(6) . . . . ? C29 C28 C33 C32 -0.2(9) . . . . ? C22 P2 C35 C36 -90.2(5) . . . . ? C29 P2 C35 C36 159.3(5) . . . . ? Re1 P2 C35 C36 17.9(5) . . . . ? C22 P2 C35 C40 84.8(5) . . . . ? C29 P2 C35 C40 -25.8(6) . . . . ? Re1 P2 C35 C40 -167.1(4) . . . . ? C40 C35 C36 C37 -0.2(9) . . . . ? P2 C35 C36 C37 174.9(5) . . . . ? C35 C36 C37 C38 -0.3(10) . . . . ? C36 C37 C38 C39 0.6(10) . . . . ? C37 C38 C39 C40 -0.4(10) . . . . ? C38 C39 C40 C35 -0.1(10) . . . . ? C36 C35 C40 C39 0.4(9) . . . . ? P2 C35 C40 C39 -174.7(5) . . . . ? _diffrn_measured_fraction_theta_max 0.918 _diffrn_reflns_theta_full 27.94 _diffrn_measured_fraction_theta_full 0.918 _refine_diff_density_max 0.866 _refine_diff_density_min -1.332 _refine_diff_density_rms 0.121 #===END data_[(Hhypy)(hypy)(PO)(HPO)]Cl _database_code_CSD 168623 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety '[(Hhypy)(hypy)(PO)(HPO)]Cl' _chemical_formula_sum 'C46 H38 Cl N6 O2 P2 Re' _chemical_formula_weight 990.41 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Re' 'Re' -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.9440(8) _cell_length_b 16.1173(7) _cell_length_c 19.0034(14) _cell_angle_alpha 81.996(2) _cell_angle_beta 77.802(2) _cell_angle_gamma 78.955(2) _cell_volume 4367.6(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 22660 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.9 _exptl_crystal_description red _exptl_crystal_colour block _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.506 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1976 _exptl_absorpt_coefficient_mu 2.961 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6273 _exptl_absorpt_correction_T_max 1.0000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CCD _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37678 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0699 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.14 _diffrn_reflns_theta_max 27.89 _reflns_number_total 16741 _reflns_number_gt 13312 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness 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 threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) 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_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0176P)^2^+9.6197P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16741 _refine_ls_number_parameters 1051 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0569 _refine_ls_R_factor_gt 0.0418 _refine_ls_wR_factor_ref 0.1061 _refine_ls_wR_factor_gt 0.0985 _refine_ls_goodness_of_fit_ref 1.132 _refine_ls_restrained_S_all 1.132 _refine_ls_shift/su_max 0.259 _refine_ls_shift/su_mean 0.004 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re 0.515447(13) 0.261393(12) 0.714722(10) 0.01958(6) Uani 1 d . . . Re2 Re -0.013209(13) 0.255379(12) 0.216732(9) 0.01759(6) Uani 1 d . . . Cl1 Cl 0.69820(15) 0.10392(14) -0.01202(10) 0.0595(5) Uani 1 d . . . Cl2 Cl 0.19071(17) 0.11173(18) 0.49754(11) 0.0771(7) Uani 1 d . . . P1 P 0.39329(9) 0.20492(9) 0.68190(7) 0.0215(3) Uani 1 d . . . P2 P 0.64717(9) 0.33133(8) 0.71855(7) 0.0209(3) Uani 1 d . . . P3 P -0.12302(9) 0.19353(8) 0.17305(7) 0.0194(3) Uani 1 d . . . P4 P 0.10630(9) 0.33292(9) 0.23242(7) 0.0222(3) Uani 1 d . . . O1 O 0.5548(2) 0.2771(2) 0.60526(18) 0.0240(8) Uani 1 d . . . O2 O 0.6783(3) 0.2216(3) 0.8525(2) 0.0320(9) Uani 1 d . . . H93 H 0.6777 0.1893 0.8912 0.048 Uiso 1 calc R . . O3 O 0.0434(2) 0.2642(2) 0.10976(18) 0.0215(7) Uani 1 d . . . O4 O 0.1424(3) 0.2191(3) 0.3633(2) 0.0356(9) Uani 1 d . . . H94 H 0.1959 0.2258 0.3412 0.053 Uiso 1 calc R . . N1 N 0.4984(3) 0.2054(3) 0.8151(2) 0.0281(10) Uani 1 d . . . H95 H 0.436(5) 0.274(5) 0.830(4) 0.06(2) Uiso 1 d . . . N2 N 0.5281(3) 0.1263(3) 0.8352(3) 0.0327(11) Uani 1 d . . . N3 N 0.5927(3) 0.1338(3) 0.7123(2) 0.0246(9) Uani 1 d . . . N4 N 0.4421(3) 0.3553(3) 0.7453(2) 0.0233(9) Uani 1 d . . . N5 N 0.3911(3) 0.4190(3) 0.7699(2) 0.0260(10) Uani 1 d . . . N6 N 0.3832(4) 0.3446(4) 0.8869(3) 0.0439(14) Uani 1 d . . . N7 N -0.0440(3) 0.2053(3) 0.3184(2) 0.0230(9) Uani 1 d . . . H96 H -0.0826 0.2383 0.3486 0.028 Uiso 1 calc R . . N8 N -0.0134(3) 0.1289(3) 0.3453(2) 0.0264(10) Uani 1 d . . . N9 N 0.0673(3) 0.1300(3) 0.2252(2) 0.0226(9) Uani 1 d . . . N10 N -0.0931(3) 0.3512(3) 0.2362(2) 0.0203(8) Uani 1 d . . . N11 N -0.1461(3) 0.4165(3) 0.2534(2) 0.0240(9) Uani 1 d . . . N12 N -0.1790(3) 0.3465(3) 0.3717(2) 0.0290(10) Uani 1 d . . . C1 C 0.5112(4) 0.2471(4) 0.5604(3) 0.0267(11) Uani 1 d . . . C2 C 0.5497(5) 0.2505(4) 0.4859(3) 0.0349(14) Uani 1 d . . . H2 H 0.6045 0.2744 0.4675 0.042 Uiso 1 calc R . . C3 C 0.5079(5) 0.2192(5) 0.4399(3) 0.0441(17) Uani 1 d . . . H3 H 0.5342 0.2220 0.3898 0.053 Uiso 1 calc R . . C4 C 0.4284(5) 0.1836(5) 0.4650(3) 0.0424(16) Uani 1 d . . . H4 H 0.4005 0.1627 0.4320 0.051 Uiso 1 calc R . . C5 C 0.3897(5) 0.1784(4) 0.5375(3) 0.0342(13) Uani 1 d . . . H5 H 0.3358 0.1530 0.5550 0.041 Uiso 1 calc R . . C6 C 0.4309(4) 0.2113(4) 0.5856(3) 0.0272(11) Uani 1 d . . . C7 C 0.2765(4) 0.2656(3) 0.7046(3) 0.0275(12) Uani 1 d . . . C8 C 0.2182(4) 0.2887(4) 0.6548(3) 0.0323(13) Uani 1 d . . . H8 H 0.2389 0.2747 0.6065 0.039 Uiso 1 calc R . . C9 C 0.1282(4) 0.3332(4) 0.6766(4) 0.0468(18) Uani 1 d . . . H9 H 0.0874 0.3482 0.6430 0.056 Uiso 1 calc R . . C10 C 0.0986(4) 0.3552(4) 0.7462(4) 0.0492(19) Uani 1 d . . . H10 H 0.0377 0.3853 0.7605 0.059 Uiso 1 calc R . . C11 C 0.1572(4) 0.3337(4) 0.7948(4) 0.0447(16) Uani 1 d . . . H11 H 0.1371 0.3498 0.8426 0.054 Uiso 1 calc R . . C12 C 0.2460(4) 0.2883(4) 0.7745(3) 0.0326(13) Uani 1 d . . . H12 H 0.2859 0.2727 0.8087 0.039 Uiso 1 calc R . . C13 C 0.3862(4) 0.0950(3) 0.7156(3) 0.0249(11) Uani 1 d . . . C14 C 0.3428(4) 0.0756(4) 0.7872(3) 0.0317(12) Uani 1 d . . . H14 H 0.3134 0.1201 0.8164 0.038 Uiso 1 calc R . . C15 C 0.3425(4) -0.0084(4) 0.8158(3) 0.0397(15) Uani 1 d . . . H15 H 0.3128 -0.0216 0.8644 0.048 Uiso 1 calc R . . C16 C 0.3858(5) -0.0726(4) 0.7729(4) 0.0446(16) Uani 1 d . . . H16 H 0.3849 -0.1302 0.7917 0.054 Uiso 1 calc R . . C17 C 0.4298(5) -0.0536(4) 0.7039(4) 0.0452(16) Uani 1 d . . . H17 H 0.4609 -0.0986 0.6757 0.054 Uiso 1 calc R . . C18 C 0.4306(4) 0.0294(4) 0.6737(4) 0.0364(14) Uani 1 d . . . H18 H 0.4610 0.0415 0.6251 0.044 Uiso 1 calc R . . C19 C 0.5796(4) 0.0863(4) 0.7780(3) 0.0271(11) Uani 1 d . . . C20 C 0.6180(4) 0.0000(4) 0.7859(4) 0.0371(14) Uani 1 d . . . H20 H 0.6089 -0.0320 0.8320 0.045 Uiso 1 calc R . . C21 C 0.6687(4) -0.0375(4) 0.7264(4) 0.0422(15) Uani 1 d . . . H21 H 0.6952 -0.0961 0.7309 0.051 Uiso 1 calc R . . C22 C 0.6813(4) 0.0102(4) 0.6591(4) 0.0380(14) Uani 1 d . . . H22 H 0.7158 -0.0154 0.6174 0.046 Uiso 1 calc R . . C23 C 0.6429(4) 0.0951(4) 0.6540(3) 0.0308(12) Uani 1 d . . . H23 H 0.6520 0.1276 0.6082 0.037 Uiso 1 calc R . . C24 C 0.3565(4) 0.4157(4) 0.8449(3) 0.0303(12) Uani 1 d . . . C25 C 0.2954(5) 0.4847(5) 0.8704(4) 0.0453(16) Uani 1 d . . . H25 H 0.2775 0.5327 0.8382 0.054 Uiso 1 calc R . . C26 C 0.2605(6) 0.4831(5) 0.9441(4) 0.064(2) Uani 1 d . . . H26 H 0.2187 0.5301 0.9637 0.077 Uiso 1 calc R . . C27 C 0.2881(8) 0.4111(6) 0.9885(4) 0.075(3) Uani 1 d . . . H27 H 0.2648 0.4077 1.0391 0.090 Uiso 1 calc R . . C28 C 0.3497(7) 0.3446(6) 0.9583(4) 0.066(2) Uani 1 d . . . H28 H 0.3695 0.2963 0.9895 0.080 Uiso 1 calc R . . C29 C 0.6356(4) 0.3656(4) 0.8080(3) 0.0242(11) Uani 1 d . . . C30 C 0.6477(4) 0.3025(4) 0.8677(3) 0.0290(12) Uani 1 d . . . C31 C 0.6284(5) 0.3275(4) 0.9365(3) 0.0390(14) Uani 1 d . . . H31 H 0.6357 0.2864 0.9768 0.047 Uiso 1 calc R . . C32 C 0.5983(5) 0.4125(5) 0.9472(3) 0.0449(16) Uani 1 d . . . H32 H 0.5850 0.4290 0.9948 0.054 Uiso 1 calc R . . C33 C 0.5875(5) 0.4735(4) 0.8893(3) 0.0412(15) Uani 1 d . . . H33 H 0.5672 0.5315 0.8974 0.049 Uiso 1 calc R . . C34 C 0.6062(4) 0.4500(4) 0.8201(3) 0.0334(13) Uani 1 d . . . H34 H 0.5988 0.4919 0.7805 0.040 Uiso 1 calc R . . C35 C 0.7656(3) 0.2769(3) 0.6909(3) 0.0242(11) Uani 1 d . . . C36 C 0.8357(4) 0.2741(4) 0.7294(3) 0.0315(12) Uani 1 d . . . H36 H 0.8221 0.2955 0.7753 0.038 Uiso 1 calc R . . C37 C 0.9264(4) 0.2394(4) 0.6994(4) 0.0384(14) Uani 1 d . . . H37 H 0.9751 0.2385 0.7247 0.046 Uiso 1 calc R . . C38 C 0.9463(4) 0.2066(4) 0.6343(4) 0.0404(15) Uani 1 d . . . H38 H 1.0083 0.1824 0.6151 0.048 Uiso 1 calc R . . C39 C 0.8769(4) 0.2083(4) 0.5962(4) 0.0353(13) Uani 1 d . . . H39 H 0.8911 0.1857 0.5508 0.042 Uiso 1 calc R . . C40 C 0.7865(4) 0.2430(3) 0.6244(3) 0.0285(12) Uani 1 d . . . H40 H 0.7385 0.2439 0.5985 0.034 Uiso 1 calc R . . C41 C 0.6501(4) 0.4319(4) 0.6605(3) 0.0280(12) Uani 1 d . . . C42 C 0.7308(5) 0.4677(4) 0.6430(3) 0.0375(14) Uani 1 d . . . H42 H 0.7852 0.4382 0.6594 0.045 Uiso 1 calc R . . C43 C 0.7329(5) 0.5451(4) 0.6022(4) 0.0451(16) Uani 1 d . . . H43 H 0.7886 0.5683 0.5904 0.054 Uiso 1 calc R . . C44 C 0.6556(5) 0.5884(4) 0.5787(3) 0.0447(17) Uani 1 d . . . H44 H 0.6570 0.6426 0.5517 0.054 Uiso 1 calc R . . C45 C 0.5736(5) 0.5535(4) 0.5940(3) 0.0394(15) Uani 1 d . . . H45 H 0.5201 0.5832 0.5764 0.047 Uiso 1 calc R . . C46 C 0.5711(4) 0.4756(4) 0.6349(3) 0.0292(12) Uani 1 d . . . H46 H 0.5157 0.4518 0.6456 0.035 Uiso 1 calc R . . C47 C 0.0109(4) 0.2319(4) 0.0602(3) 0.0262(11) Uani 1 d . . . C48 C 0.0617(5) 0.2303(5) -0.0093(3) 0.0427(17) Uani 1 d . . . H48 H 0.1181 0.2526 -0.0216 0.051 Uiso 1 calc R . . C49 C 0.0314(6) 0.1967(6) -0.0609(4) 0.060(2) Uani 1 d . . . H49 H 0.0654 0.1981 -0.1092 0.072 Uiso 1 calc R . . C50 C -0.0491(6) 0.1606(6) -0.0427(4) 0.057(2) Uani 1 d . . . H50 H -0.0697 0.1375 -0.0786 0.068 Uiso 1 calc R . . C51 C -0.0985(5) 0.1581(4) 0.0263(3) 0.0373(14) Uani 1 d . . . H51 H -0.1526 0.1324 0.0385 0.045 Uiso 1 calc R . . C52 C -0.0696(4) 0.1936(4) 0.0793(3) 0.0272(12) Uani 1 d . . . C53 C -0.2402(4) 0.2529(3) 0.1836(3) 0.0230(10) Uani 1 d . . . C54 C -0.2907(4) 0.2700(4) 0.1283(3) 0.0335(13) Uani 1 d . . . H54 H -0.2642 0.2498 0.0826 0.040 Uiso 1 calc R . . C55 C -0.3797(4) 0.3165(5) 0.1395(4) 0.0430(16) Uani 1 d . . . H55 H -0.4143 0.3272 0.1017 0.052 Uiso 1 calc R . . C56 C -0.4179(4) 0.3472(4) 0.2048(4) 0.0455(17) Uani 1 d . . . H56 H -0.4784 0.3801 0.2116 0.055 Uiso 1 calc R . . C57 C -0.3690(4) 0.3308(4) 0.2615(3) 0.0350(13) Uani 1 d . . . H57 H -0.3957 0.3519 0.3069 0.042 Uiso 1 calc R . . C58 C -0.2806(4) 0.2830(4) 0.2501(3) 0.0261(11) Uani 1 d . . . H58 H -0.2468 0.2705 0.2885 0.031 Uiso 1 calc R . . C59 C -0.1330(3) 0.0854(3) 0.2121(3) 0.0233(10) Uani 1 d . . . C60 C -0.1823(4) 0.0734(4) 0.2818(3) 0.0316(12) Uani 1 d . . . H60 H -0.2149 0.1213 0.3060 0.038 Uiso 1 calc R . . C61 C -0.1848(4) -0.0088(4) 0.3172(4) 0.0372(14) Uani 1 d . . . H61 H -0.2202 -0.0169 0.3647 0.045 Uiso 1 calc R . . C62 C -0.1351(5) -0.0777(4) 0.2821(4) 0.0431(16) Uani 1 d . . . H62 H -0.1357 -0.1337 0.3057 0.052 Uiso 1 calc R . . C63 C -0.0845(5) -0.0654(4) 0.2126(4) 0.0467(17) Uani 1 d . . . H63 H -0.0502 -0.1131 0.1890 0.056 Uiso 1 calc R . . C64 C -0.0834(4) 0.0157(4) 0.1773(3) 0.0359(14) Uani 1 d . . . H64 H -0.0490 0.0237 0.1294 0.043 Uiso 1 calc R . . C65 C 0.0491(4) 0.0860(4) 0.2930(3) 0.0264(11) Uani 1 d . . . C66 C 0.0896(4) 0.0023(4) 0.3079(4) 0.0356(13) Uani 1 d . . . H66 H 0.0776 -0.0259 0.3554 0.043 Uiso 1 calc R . . C67 C 0.1473(4) -0.0391(4) 0.2527(4) 0.0395(15) Uani 1 d . . . H67 H 0.1747 -0.0969 0.2614 0.047 Uiso 1 calc R . . C68 C 0.1659(4) 0.0045(4) 0.1829(4) 0.0372(14) Uani 1 d . . . H68 H 0.2058 -0.0233 0.1442 0.045 Uiso 1 calc R . . C69 C 0.1250(4) 0.0887(4) 0.1719(3) 0.0279(12) Uani 1 d . . . H69 H 0.1381 0.1183 0.1250 0.034 Uiso 1 calc R . . C70 C -0.1932(4) 0.4174(3) 0.3257(3) 0.0245(11) Uani 1 d . . . C71 C -0.2542(4) 0.4909(4) 0.3444(3) 0.0314(12) Uani 1 d . . . H71 H -0.2616 0.5392 0.3100 0.038 Uiso 1 calc R . . C72 C -0.3036(5) 0.4915(4) 0.4143(4) 0.0419(15) Uani 1 d . . . H72 H -0.3460 0.5407 0.4289 0.050 Uiso 1 calc R . . C73 C -0.2914(5) 0.4210(5) 0.4627(3) 0.0454(17) Uani 1 d . . . H73 H -0.3250 0.4204 0.5111 0.055 Uiso 1 calc R . . C74 C -0.2279(4) 0.3496(4) 0.4390(3) 0.0377(14) Uani 1 d . . . H74 H -0.2192 0.3009 0.4728 0.045 Uiso 1 calc R . . C75 C 0.0776(4) 0.3598(4) 0.3253(3) 0.0270(11) Uani 1 d . . . C76 C 0.0942(4) 0.2932(4) 0.3825(3) 0.0303(12) Uani 1 d . . . C77 C 0.0569(5) 0.3111(5) 0.4527(3) 0.0423(16) Uani 1 d . . . H77 H 0.0689 0.2689 0.4914 0.051 Uiso 1 calc R . . C78 C 0.0031(5) 0.3880(5) 0.4687(3) 0.0467(17) Uani 1 d . . . H78 H -0.0235 0.3972 0.5175 0.056 Uiso 1 calc R . . C79 C -0.0124(5) 0.4513(5) 0.4142(3) 0.0438(16) Uani 1 d . . . H79 H -0.0485 0.5047 0.4256 0.053 Uiso 1 calc R . . C80 C 0.0244(4) 0.4375(4) 0.3428(3) 0.0365(14) Uani 1 d . . . H80 H 0.0132 0.4816 0.3053 0.044 Uiso 1 calc R . . C81 C 0.2286(4) 0.2870(4) 0.2118(3) 0.0275(11) Uani 1 d . . . C82 C 0.2906(4) 0.2938(5) 0.2557(4) 0.0409(15) Uani 1 d . . . H82 H 0.2698 0.3213 0.2987 0.049 Uiso 1 calc R . . C83 C 0.3840(5) 0.2587(6) 0.2343(5) 0.058(2) Uani 1 d . . . H83 H 0.4269 0.2618 0.2640 0.070 Uiso 1 calc R . . C84 C 0.4153(5) 0.2202(5) 0.1722(4) 0.052(2) Uani 1 d . . . H84 H 0.4793 0.1974 0.1586 0.063 Uiso 1 calc R . . C85 C 0.3536(4) 0.2148(4) 0.1294(4) 0.0435(16) Uani 1 d . . . H85 H 0.3753 0.1882 0.0859 0.052 Uiso 1 calc R . . C86 C 0.2603(4) 0.2475(4) 0.1487(3) 0.0307(12) Uani 1 d . . . H86 H 0.2181 0.2429 0.1189 0.037 Uiso 1 calc R . . C87 C 0.1027(4) 0.4349(3) 0.1762(3) 0.0256(11) Uani 1 d . . . C88 C 0.1634(4) 0.4885(4) 0.1810(3) 0.0365(14) Uani 1 d . . . H88 H 0.2045 0.4729 0.2143 0.044 Uiso 1 calc R . . C89 C 0.1640(5) 0.5647(4) 0.1370(4) 0.0409(15) Uani 1 d . . . H89 H 0.2070 0.6001 0.1396 0.049 Uiso 1 calc R . . C90 C 0.1038(5) 0.5897(4) 0.0901(3) 0.0355(14) Uani 1 d . . . H90 H 0.1046 0.6424 0.0606 0.043 Uiso 1 calc R . . C91 C 0.0420(4) 0.5382(4) 0.0858(3) 0.0335(13) Uani 1 d . . . H91 H -0.0005 0.5554 0.0536 0.040 Uiso 1 calc R . . C92 C 0.0418(4) 0.4605(4) 0.1289(3) 0.0266(11) Uani 1 d . . . H92 H -0.0007 0.4250 0.1256 0.032 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.01836(11) 0.02385(12) 0.01667(10) -0.00208(7) -0.00158(8) -0.00579(8) Re2 0.01676(11) 0.02076(11) 0.01600(10) -0.00340(7) -0.00077(7) -0.00651(7) Cl1 0.0724(13) 0.0649(13) 0.0519(10) 0.0212(9) -0.0367(9) -0.0299(10) Cl2 0.0785(15) 0.0983(19) 0.0456(11) 0.0133(11) -0.0197(10) 0.0011(13) P1 0.0202(6) 0.0251(7) 0.0191(6) -0.0004(5) -0.0012(5) -0.0076(5) P2 0.0204(6) 0.0213(7) 0.0218(6) -0.0028(5) -0.0046(5) -0.0048(5) P3 0.0171(6) 0.0237(7) 0.0183(6) -0.0028(5) -0.0015(5) -0.0073(5) P4 0.0217(6) 0.0275(7) 0.0196(6) -0.0041(5) -0.0028(5) -0.0100(5) O1 0.0230(18) 0.033(2) 0.0173(17) -0.0016(14) -0.0015(14) -0.0105(15) O2 0.042(2) 0.027(2) 0.030(2) 0.0019(16) -0.0158(18) -0.0078(17) O3 0.0219(18) 0.0269(19) 0.0180(17) -0.0060(13) 0.0016(14) -0.0131(14) O4 0.041(2) 0.044(3) 0.024(2) -0.0039(17) -0.0049(18) -0.0132(19) N1 0.023(2) 0.038(3) 0.021(2) -0.0005(19) 0.0012(18) -0.007(2) N2 0.034(3) 0.035(3) 0.028(2) 0.009(2) -0.009(2) -0.009(2) N3 0.021(2) 0.023(2) 0.031(2) -0.0031(18) -0.0057(19) -0.0042(17) N4 0.024(2) 0.032(3) 0.0134(19) -0.0016(16) 0.0034(17) -0.0123(18) N5 0.023(2) 0.023(2) 0.030(2) -0.0038(18) 0.0019(19) -0.0059(18) N6 0.061(4) 0.041(3) 0.023(3) -0.008(2) 0.003(2) -0.001(3) N7 0.025(2) 0.022(2) 0.022(2) -0.0013(16) -0.0028(18) -0.0064(17) N8 0.027(2) 0.028(3) 0.024(2) 0.0006(18) -0.0037(19) -0.0061(19) N9 0.017(2) 0.021(2) 0.030(2) -0.0030(17) -0.0017(18) -0.0063(16) N10 0.019(2) 0.026(2) 0.017(2) -0.0005(16) -0.0025(17) -0.0089(17) N11 0.024(2) 0.021(2) 0.026(2) -0.0030(17) -0.0002(18) -0.0026(17) N12 0.029(2) 0.034(3) 0.024(2) -0.0061(19) 0.001(2) -0.010(2) C1 0.039(3) 0.026(3) 0.017(2) -0.0045(19) -0.004(2) -0.008(2) C2 0.044(4) 0.039(3) 0.022(3) -0.004(2) 0.004(3) -0.020(3) C3 0.066(5) 0.052(4) 0.017(3) -0.003(3) 0.000(3) -0.026(4) C4 0.062(4) 0.050(4) 0.023(3) -0.004(3) -0.011(3) -0.025(3) C5 0.043(3) 0.036(3) 0.028(3) 0.001(2) -0.012(3) -0.014(3) C6 0.032(3) 0.032(3) 0.017(2) 0.001(2) -0.002(2) -0.010(2) C7 0.019(3) 0.024(3) 0.038(3) 0.002(2) 0.000(2) -0.008(2) C8 0.027(3) 0.029(3) 0.043(3) 0.005(2) -0.010(3) -0.011(2) C9 0.030(3) 0.036(4) 0.075(5) 0.017(3) -0.022(3) -0.011(3) C10 0.020(3) 0.038(4) 0.078(5) 0.005(3) 0.009(3) -0.004(3) C11 0.032(3) 0.039(4) 0.057(4) -0.004(3) 0.009(3) -0.009(3) C12 0.025(3) 0.035(3) 0.034(3) -0.003(2) 0.003(2) -0.008(2) C13 0.021(3) 0.026(3) 0.030(3) 0.002(2) -0.009(2) -0.009(2) C14 0.035(3) 0.035(3) 0.025(3) 0.004(2) -0.006(2) -0.009(2) C15 0.037(3) 0.045(4) 0.038(3) 0.015(3) -0.011(3) -0.019(3) C16 0.039(4) 0.030(4) 0.070(5) 0.012(3) -0.025(3) -0.014(3) C17 0.042(4) 0.026(3) 0.070(5) -0.010(3) -0.015(3) -0.005(3) C18 0.035(3) 0.035(3) 0.043(3) -0.011(3) -0.005(3) -0.012(3) C19 0.024(3) 0.029(3) 0.029(3) 0.006(2) -0.010(2) -0.007(2) C20 0.032(3) 0.030(3) 0.051(4) 0.009(3) -0.016(3) -0.010(2) C21 0.030(3) 0.028(3) 0.067(5) 0.003(3) -0.013(3) -0.002(2) C22 0.028(3) 0.030(3) 0.056(4) -0.010(3) -0.005(3) -0.005(2) C23 0.022(3) 0.032(3) 0.037(3) -0.008(2) 0.000(2) -0.006(2) C24 0.033(3) 0.033(3) 0.026(3) -0.006(2) 0.002(2) -0.012(2) C25 0.051(4) 0.038(4) 0.042(4) -0.012(3) 0.010(3) -0.010(3) C26 0.088(6) 0.044(4) 0.046(4) -0.018(3) 0.033(4) -0.016(4) C27 0.115(8) 0.057(5) 0.037(4) -0.012(4) 0.023(5) -0.013(5) C28 0.106(7) 0.059(5) 0.020(3) -0.006(3) 0.009(4) -0.003(5) C29 0.024(3) 0.029(3) 0.020(2) -0.003(2) -0.006(2) -0.004(2) C30 0.029(3) 0.031(3) 0.031(3) -0.003(2) -0.013(2) -0.005(2) C31 0.045(4) 0.047(4) 0.029(3) -0.005(3) -0.009(3) -0.013(3) C32 0.058(4) 0.054(4) 0.023(3) -0.010(3) -0.008(3) -0.004(3) C33 0.052(4) 0.034(4) 0.035(3) -0.013(3) -0.011(3) 0.007(3) C34 0.037(3) 0.031(3) 0.030(3) -0.006(2) -0.009(3) 0.002(2) C35 0.018(2) 0.023(3) 0.031(3) 0.000(2) -0.002(2) -0.009(2) C36 0.026(3) 0.031(3) 0.042(3) -0.008(2) -0.008(2) -0.010(2) C37 0.024(3) 0.031(3) 0.063(4) -0.001(3) -0.013(3) -0.010(2) C38 0.025(3) 0.040(4) 0.049(4) -0.001(3) 0.009(3) -0.006(2) C39 0.030(3) 0.028(3) 0.042(3) -0.002(2) 0.003(3) -0.005(2) C40 0.027(3) 0.025(3) 0.033(3) 0.001(2) 0.001(2) -0.010(2) C41 0.035(3) 0.030(3) 0.019(2) -0.006(2) 0.000(2) -0.009(2) C42 0.039(3) 0.034(3) 0.044(3) -0.001(3) -0.012(3) -0.014(3) C43 0.053(4) 0.032(4) 0.053(4) 0.004(3) -0.008(3) -0.023(3) C44 0.067(5) 0.027(3) 0.034(3) 0.001(2) 0.003(3) -0.009(3) C45 0.043(4) 0.033(3) 0.029(3) 0.005(2) 0.007(3) 0.004(3) C46 0.029(3) 0.030(3) 0.023(3) 0.000(2) 0.003(2) -0.002(2) C47 0.029(3) 0.029(3) 0.022(3) -0.004(2) -0.003(2) -0.009(2) C48 0.045(4) 0.064(5) 0.025(3) -0.016(3) 0.010(3) -0.034(3) C49 0.075(5) 0.091(6) 0.023(3) -0.026(3) 0.019(3) -0.052(5) C50 0.068(5) 0.088(6) 0.031(3) -0.023(4) -0.002(3) -0.047(5) C51 0.039(3) 0.052(4) 0.027(3) -0.011(3) -0.001(3) -0.023(3) C52 0.026(3) 0.039(3) 0.017(2) -0.006(2) 0.002(2) -0.012(2) C53 0.021(3) 0.023(3) 0.025(3) 0.0036(19) -0.003(2) -0.008(2) C54 0.036(3) 0.035(3) 0.030(3) 0.006(2) -0.012(2) -0.007(3) C55 0.034(3) 0.050(4) 0.043(4) 0.014(3) -0.017(3) -0.004(3) C56 0.026(3) 0.033(4) 0.068(5) 0.014(3) -0.007(3) 0.002(2) C57 0.027(3) 0.032(3) 0.041(3) -0.005(3) 0.006(3) -0.007(2) C58 0.017(2) 0.031(3) 0.031(3) -0.003(2) -0.003(2) -0.009(2) C59 0.019(2) 0.024(3) 0.029(3) 0.000(2) -0.008(2) -0.006(2) C60 0.029(3) 0.030(3) 0.034(3) 0.003(2) -0.008(2) -0.005(2) C61 0.034(3) 0.035(3) 0.043(3) 0.013(3) -0.012(3) -0.013(3) C62 0.038(3) 0.028(3) 0.067(5) 0.007(3) -0.018(3) -0.016(3) C63 0.049(4) 0.030(4) 0.063(5) -0.015(3) -0.006(3) -0.009(3) C64 0.038(3) 0.035(3) 0.038(3) -0.012(3) -0.002(3) -0.011(3) C65 0.022(3) 0.025(3) 0.035(3) -0.001(2) -0.008(2) -0.008(2) C66 0.031(3) 0.030(3) 0.045(3) 0.007(3) -0.011(3) -0.007(2) C67 0.030(3) 0.023(3) 0.065(4) -0.001(3) -0.014(3) -0.001(2) C68 0.024(3) 0.033(3) 0.055(4) -0.013(3) -0.003(3) -0.005(2) C69 0.020(3) 0.031(3) 0.033(3) -0.010(2) 0.001(2) -0.006(2) C70 0.025(3) 0.025(3) 0.025(3) -0.005(2) -0.003(2) -0.010(2) C71 0.032(3) 0.031(3) 0.030(3) -0.010(2) 0.001(2) -0.005(2) C72 0.040(4) 0.044(4) 0.038(3) -0.016(3) 0.001(3) 0.002(3) C73 0.053(4) 0.055(4) 0.024(3) -0.015(3) 0.011(3) -0.013(3) C74 0.042(4) 0.045(4) 0.024(3) -0.004(2) 0.000(3) -0.009(3) C75 0.031(3) 0.034(3) 0.020(2) -0.007(2) -0.004(2) -0.015(2) C76 0.035(3) 0.039(3) 0.022(3) -0.005(2) -0.007(2) -0.016(3) C77 0.049(4) 0.057(4) 0.026(3) -0.006(3) -0.003(3) -0.023(3) C78 0.061(5) 0.058(5) 0.025(3) -0.017(3) 0.000(3) -0.021(4) C79 0.052(4) 0.046(4) 0.035(3) -0.019(3) 0.002(3) -0.014(3) C80 0.044(4) 0.037(4) 0.035(3) -0.009(2) -0.008(3) -0.017(3) C81 0.021(3) 0.035(3) 0.028(3) 0.003(2) -0.006(2) -0.012(2) C82 0.032(3) 0.047(4) 0.050(4) 0.005(3) -0.019(3) -0.017(3) C83 0.032(4) 0.083(6) 0.065(5) 0.020(4) -0.025(4) -0.027(4) C84 0.023(3) 0.059(5) 0.065(5) 0.020(4) -0.004(3) -0.006(3) C85 0.030(3) 0.044(4) 0.046(4) 0.008(3) 0.007(3) -0.004(3) C86 0.026(3) 0.030(3) 0.034(3) 0.002(2) -0.002(2) -0.007(2) C87 0.029(3) 0.025(3) 0.025(3) -0.006(2) 0.001(2) -0.011(2) C88 0.038(3) 0.043(4) 0.034(3) -0.009(3) -0.004(3) -0.019(3) C89 0.049(4) 0.038(4) 0.043(4) -0.009(3) -0.003(3) -0.030(3) C90 0.049(4) 0.027(3) 0.029(3) -0.004(2) 0.005(3) -0.014(3) C91 0.036(3) 0.034(3) 0.026(3) 0.000(2) 0.002(2) -0.007(2) C92 0.028(3) 0.027(3) 0.025(3) -0.006(2) 0.000(2) -0.009(2) _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 Re1 N4 1.780(5) . ? Re1 N1 1.980(4) . ? Re1 O1 2.032(3) . ? Re1 N3 2.158(4) . ? Re1 P1 2.4137(13) . ? Re1 P2 2.4667(13) . ? Re2 N10 1.792(4) . ? Re2 N7 1.982(4) . ? Re2 O3 2.026(3) . ? Re2 N9 2.148(4) . ? Re2 P3 2.4101(13) . ? Re2 P4 2.4545(13) . ? P1 C6 1.791(5) . ? P1 C13 1.814(6) . ? P1 C7 1.826(6) . ? P2 C35 1.822(5) . ? P2 C29 1.824(5) . ? P2 C41 1.832(6) . ? P3 C52 1.791(5) . ? P3 C53 1.812(5) . ? P3 C59 1.818(5) . ? P4 C81 1.817(6) . ? P4 C75 1.819(5) . ? P4 C87 1.830(6) . ? O1 C1 1.362(6) . ? O2 C30 1.346(7) . ? O3 C47 1.350(6) . ? O4 C76 1.327(7) . ? N1 N2 1.299(7) . ? N2 C19 1.357(8) . ? N3 C23 1.358(7) . ? N3 C19 1.367(7) . ? N4 N5 1.240(6) . ? N5 C24 1.408(7) . ? N6 C28 1.343(8) . ? N6 C24 1.346(8) . ? N7 N8 1.301(7) . ? N8 C65 1.375(7) . ? N9 C69 1.347(7) . ? N9 C65 1.381(7) . ? N10 N11 1.229(6) . ? N11 C70 1.406(7) . ? N12 C74 1.336(7) . ? N12 C70 1.349(7) . ? C1 C6 1.397(8) . ? C1 C2 1.409(7) . ? C2 C3 1.371(9) . ? C3 C4 1.383(9) . ? C4 C5 1.375(8) . ? C5 C6 1.412(8) . ? C7 C8 1.385(8) . ? C7 C12 1.386(8) . ? C8 C9 1.404(9) . ? C9 C10 1.376(11) . ? C10 C11 1.370(11) . ? C11 C12 1.391(8) . ? C13 C18 1.391(8) . ? C13 C14 1.399(8) . ? C14 C15 1.387(9) . ? C15 C16 1.381(10) . ? C16 C17 1.358(10) . ? C17 C18 1.381(9) . ? C19 C20 1.399(9) . ? C20 C21 1.369(10) . ? C21 C22 1.393(10) . ? C22 C23 1.376(9) . ? C24 C25 1.371(9) . ? C25 C26 1.386(10) . ? C26 C27 1.385(13) . ? C27 C28 1.377(12) . ? C29 C34 1.382(8) . ? C29 C30 1.432(8) . ? C30 C31 1.378(8) . ? C31 C32 1.386(10) . ? C32 C33 1.384(10) . ? C33 C34 1.376(8) . ? C35 C36 1.391(8) . ? C35 C40 1.395(8) . ? C36 C37 1.396(8) . ? C37 C38 1.366(10) . ? C38 C39 1.378(10) . ? C39 C40 1.383(8) . ? C41 C42 1.394(8) . ? C41 C46 1.397(8) . ? C42 C43 1.376(9) . ? C43 C44 1.358(11) . ? C44 C45 1.403(10) . ? C45 C46 1.385(8) . ? C47 C48 1.378(8) . ? C47 C52 1.413(8) . ? C48 C49 1.376(9) . ? C49 C50 1.393(10) . ? C50 C51 1.361(9) . ? C51 C52 1.403(8) . ? C53 C54 1.388(8) . ? C53 C58 1.390(8) . ? C54 C55 1.384(9) . ? C55 C56 1.370(10) . ? C56 C57 1.393(10) . ? C57 C58 1.387(8) . ? C59 C60 1.380(8) . ? C59 C64 1.389(8) . ? C60 C61 1.403(8) . ? C61 C62 1.383(10) . ? C62 C63 1.384(10) . ? C63 C64 1.387(10) . ? C65 C66 1.385(8) . ? C66 C67 1.372(9) . ? C67 C68 1.410(9) . ? C68 C69 1.383(9) . ? C70 C71 1.387(8) . ? C71 C72 1.377(8) . ? C72 C73 1.366(10) . ? C73 C74 1.404(9) . ? C75 C80 1.390(9) . ? C75 C76 1.443(8) . ? C76 C77 1.381(8) . ? C77 C78 1.377(10) . ? C78 C79 1.372(11) . ? C79 C80 1.385(9) . ? C81 C86 1.387(8) . ? C81 C82 1.399(8) . ? C82 C83 1.399(10) . ? C83 C84 1.362(12) . ? C84 C85 1.375(11) . ? C85 C86 1.383(8) . ? C87 C92 1.380(8) . ? C87 C88 1.391(8) . ? C88 C89 1.387(9) . ? C89 C90 1.367(10) . ? C90 C91 1.376(9) . ? C91 C92 1.398(8) . ? 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 N4 Re1 N1 90.14(19) . . ? N4 Re1 O1 109.63(17) . . ? N1 Re1 O1 160.03(18) . . ? N4 Re1 N3 162.35(18) . . ? N1 Re1 N3 72.24(18) . . ? O1 Re1 N3 87.93(16) . . ? N4 Re1 P1 94.79(14) . . ? N1 Re1 P1 94.91(14) . . ? O1 Re1 P1 80.98(10) . . ? N3 Re1 P1 86.02(12) . . ? N4 Re1 P2 86.70(14) . . ? N1 Re1 P2 98.18(14) . . ? O1 Re1 P2 86.18(10) . . ? N3 Re1 P2 96.53(12) . . ? P1 Re1 P2 166.82(4) . . ? N10 Re2 N7 91.33(18) . . ? N10 Re2 O3 108.90(16) . . ? N7 Re2 O3 159.60(17) . . ? N10 Re2 N9 163.61(17) . . ? N7 Re2 N9 72.29(17) . . ? O3 Re2 N9 87.43(16) . . ? N10 Re2 P3 93.87(13) . . ? N7 Re2 P3 95.60(13) . . ? O3 Re2 P3 80.87(10) . . ? N9 Re2 P3 87.17(12) . . ? N10 Re2 P4 85.55(13) . . ? N7 Re2 P4 97.54(13) . . ? O3 Re2 P4 86.89(10) . . ? N9 Re2 P4 97.09(12) . . ? P3 Re2 P4 166.86(4) . . ? C6 P1 C13 108.4(3) . . ? C6 P1 C7 110.0(3) . . ? C13 P1 C7 106.9(2) . . ? C6 P1 Re1 99.90(19) . . ? C13 P1 Re1 115.51(18) . . ? C7 P1 Re1 115.72(19) . . ? C35 P2 C29 108.7(2) . . ? C35 P2 C41 100.8(2) . . ? C29 P2 C41 101.8(2) . . ? C35 P2 Re1 119.66(18) . . ? C29 P2 Re1 110.21(18) . . ? C41 P2 Re1 114.01(19) . . ? C52 P3 C53 110.8(3) . . ? C52 P3 C59 109.7(3) . . ? C53 P3 C59 106.4(2) . . ? C52 P3 Re2 99.88(18) . . ? C53 P3 Re2 115.57(18) . . ? C59 P3 Re2 114.39(17) . . ? C81 P4 C75 109.0(3) . . ? C81 P4 C87 102.2(2) . . ? C75 P4 C87 105.2(3) . . ? C81 P4 Re2 120.66(19) . . ? C75 P4 Re2 107.09(18) . . ? C87 P4 Re2 111.77(18) . . ? C1 O1 Re1 122.2(3) . . ? C47 O3 Re2 123.3(3) . . ? N2 N1 Re1 126.3(4) . . ? N1 N2 C19 110.7(4) . . ? C23 N3 C19 118.5(5) . . ? C23 N3 Re1 128.2(4) . . ? C19 N3 Re1 113.0(3) . . ? N5 N4 Re1 177.0(4) . . ? N4 N5 C24 118.4(5) . . ? C28 N6 C24 116.5(6) . . ? N8 N7 Re2 127.2(3) . . ? N7 N8 C65 110.1(4) . . ? C69 N9 C65 118.1(5) . . ? C69 N9 Re2 127.9(4) . . ? C65 N9 Re2 113.8(3) . . ? N11 N10 Re2 176.2(4) . . ? N10 N11 C70 117.6(4) . . ? C74 N12 C70 116.1(5) . . ? O1 C1 C6 122.5(5) . . ? O1 C1 C2 118.9(5) . . ? C6 C1 C2 118.6(5) . . ? C3 C2 C1 119.8(6) . . ? C2 C3 C4 121.6(5) . . ? C5 C4 C3 120.1(6) . . ? C4 C5 C6 119.3(6) . . ? C1 C6 C5 120.6(5) . . ? C1 C6 P1 114.1(4) . . ? C5 C6 P1 125.1(4) . . ? C8 C7 C12 119.6(5) . . ? C8 C7 P1 122.3(5) . . ? C12 C7 P1 118.1(5) . . ? C7 C8 C9 119.3(6) . . ? C10 C9 C8 120.5(6) . . ? C11 C10 C9 120.0(6) . . ? C10 C11 C12 120.2(7) . . ? C7 C12 C11 120.3(6) . . ? C18 C13 C14 119.5(5) . . ? C18 C13 P1 121.0(4) . . ? C14 C13 P1 119.2(4) . . ? C15 C14 C13 120.3(6) . . ? C16 C15 C14 119.3(6) . . ? C17 C16 C15 120.3(6) . . ? C16 C17 C18 121.7(6) . . ? C17 C18 C13 118.9(6) . . ? N2 C19 N3 117.3(5) . . ? N2 C19 C20 121.3(5) . . ? N3 C19 C20 121.4(5) . . ? C21 C20 C19 119.1(6) . . ? C20 C21 C22 119.8(6) . . ? C23 C22 C21 119.0(6) . . ? N3 C23 C22 122.2(6) . . ? N6 C24 C25 124.1(6) . . ? N6 C24 N5 118.4(5) . . ? C25 C24 N5 117.5(6) . . ? C24 C25 C26 118.6(7) . . ? C27 C26 C25 118.3(7) . . ? C28 C27 C26 119.2(7) . . ? N6 C28 C27 123.2(8) . . ? C34 C29 C30 119.8(5) . . ? C34 C29 P2 121.1(4) . . ? C30 C29 P2 118.8(4) . . ? O2 C30 C31 124.0(6) . . ? O2 C30 C29 117.2(5) . . ? C31 C30 C29 118.8(6) . . ? C30 C31 C32 120.2(6) . . ? C33 C32 C31 120.9(6) . . ? C34 C33 C32 119.9(6) . . ? C33 C34 C29 120.4(6) . . ? C36 C35 C40 119.8(5) . . ? C36 C35 P2 123.2(4) . . ? C40 C35 P2 116.8(4) . . ? C35 C36 C37 118.7(6) . . ? C38 C37 C36 121.0(6) . . ? C37 C38 C39 120.5(6) . . ? C38 C39 C40 119.7(6) . . ? C39 C40 C35 120.3(6) . . ? C42 C41 C46 118.7(5) . . ? C42 C41 P2 120.3(5) . . ? C46 C41 P2 121.0(4) . . ? C43 C42 C41 121.0(6) . . ? C44 C43 C42 120.3(6) . . ? C43 C44 C45 120.3(6) . . ? C46 C45 C44 119.6(6) . . ? C45 C46 C41 120.1(6) . . ? O3 C47 C48 118.9(5) . . ? O3 C47 C52 121.5(4) . . ? C48 C47 C52 119.4(5) . . ? C49 C48 C47 120.4(6) . . ? C48 C49 C50 120.3(6) . . ? C51 C50 C49 120.4(6) . . ? C50 C51 C52 120.1(6) . . ? C51 C52 C47 119.2(5) . . ? C51 C52 P3 126.6(4) . . ? C47 C52 P3 114.2(4) . . ? C54 C53 C58 118.8(5) . . ? C54 C53 P3 123.0(4) . . ? C58 C53 P3 118.2(4) . . ? C55 C54 C53 120.3(6) . . ? C56 C55 C54 120.2(6) . . ? C55 C56 C57 120.9(6) . . ? C58 C57 C56 118.4(6) . . ? C57 C58 C53 121.4(5) . . ? C60 C59 C64 119.9(5) . . ? C60 C59 P3 118.1(4) . . ? C64 C59 P3 121.6(4) . . ? C59 C60 C61 120.5(6) . . ? C62 C61 C60 119.1(6) . . ? C61 C62 C63 120.2(6) . . ? C62 C63 C64 120.6(6) . . ? C63 C64 C59 119.6(6) . . ? N8 C65 N9 116.5(5) . . ? N8 C65 C66 121.1(5) . . ? N9 C65 C66 122.3(5) . . ? C67 C66 C65 118.7(6) . . ? C66 C67 C68 119.7(6) . . ? C69 C68 C67 118.8(6) . . ? N9 C69 C68 122.3(6) . . ? N12 C70 C71 124.2(5) . . ? N12 C70 N11 118.5(5) . . ? C71 C70 N11 117.3(5) . . ? C72 C71 C70 118.0(6) . . ? C73 C72 C71 119.8(6) . . ? C72 C73 C74 118.3(6) . . ? N12 C74 C73 123.6(6) . . ? C80 C75 C76 119.3(5) . . ? C80 C75 P4 121.0(5) . . ? C76 C75 P4 118.4(4) . . ? O4 C76 C77 125.2(6) . . ? O4 C76 C75 117.4(5) . . ? C77 C76 C75 117.4(6) . . ? C78 C77 C76 122.1(7) . . ? C79 C78 C77 120.3(6) . . ? C78 C79 C80 120.1(7) . . ? C79 C80 C75 120.7(6) . . ? C86 C81 C82 120.3(6) . . ? C86 C81 P4 117.7(4) . . ? C82 C81 P4 121.9(5) . . ? C83 C82 C81 117.9(7) . . ? C84 C83 C82 121.9(7) . . ? C83 C84 C85 119.4(6) . . ? C84 C85 C86 120.9(7) . . ? C85 C86 C81 119.6(6) . . ? C92 C87 C88 118.7(5) . . ? C92 C87 P4 122.2(4) . . ? C88 C87 P4 119.1(5) . . ? C89 C88 C87 120.0(6) . . ? C90 C89 C88 121.1(6) . . ? C89 C90 C91 119.6(6) . . ? C90 C91 C92 119.8(6) . . ? C87 C92 C91 120.8(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 N4 Re1 P1 C6 112.9(2) . . . . ? N1 Re1 P1 C6 -156.5(2) . . . . ? O1 Re1 P1 C6 3.8(2) . . . . ? N3 Re1 P1 C6 -84.7(2) . . . . ? P2 Re1 P1 C6 17.0(3) . . . . ? N4 Re1 P1 C13 -131.0(2) . . . . ? N1 Re1 P1 C13 -40.5(2) . . . . ? O1 Re1 P1 C13 119.8(2) . . . . ? N3 Re1 P1 C13 31.3(2) . . . . ? P2 Re1 P1 C13 133.0(3) . . . . ? N4 Re1 P1 C7 -5.0(2) . . . . ? N1 Re1 P1 C7 85.5(2) . . . . ? O1 Re1 P1 C7 -114.2(2) . . . . ? N3 Re1 P1 C7 157.3(2) . . . . ? P2 Re1 P1 C7 -101.0(3) . . . . ? N4 Re1 P2 C35 -178.6(2) . . . . ? N1 Re1 P2 C35 91.8(2) . . . . ? O1 Re1 P2 C35 -68.6(2) . . . . ? N3 Re1 P2 C35 18.9(2) . . . . ? P1 Re1 P2 C35 -81.7(3) . . . . ? N4 Re1 P2 C29 54.4(2) . . . . ? N1 Re1 P2 C29 -35.2(2) . . . . ? O1 Re1 P2 C29 164.4(2) . . . . ? N3 Re1 P2 C29 -108.1(2) . . . . ? P1 Re1 P2 C29 151.3(2) . . . . ? N4 Re1 P2 C41 -59.2(2) . . . . ? N1 Re1 P2 C41 -148.9(2) . . . . ? O1 Re1 P2 C41 50.7(2) . . . . ? N3 Re1 P2 C41 138.2(2) . . . . ? P1 Re1 P2 C41 37.7(3) . . . . ? N10 Re2 P3 C52 112.5(2) . . . . ? N7 Re2 P3 C52 -155.7(2) . . . . ? O3 Re2 P3 C52 4.0(2) . . . . ? N9 Re2 P3 C52 -83.9(2) . . . . ? P4 Re2 P3 C52 25.5(3) . . . . ? N10 Re2 P3 C53 -6.3(2) . . . . ? N7 Re2 P3 C53 85.4(2) . . . . ? O3 Re2 P3 C53 -114.9(2) . . . . ? N9 Re2 P3 C53 157.3(2) . . . . ? P4 Re2 P3 C53 -93.4(3) . . . . ? N10 Re2 P3 C59 -130.5(2) . . . . ? N7 Re2 P3 C59 -38.7(2) . . . . ? O3 Re2 P3 C59 121.0(2) . . . . ? N9 Re2 P3 C59 33.1(2) . . . . ? P4 Re2 P3 C59 142.5(2) . . . . ? N10 Re2 P4 C81 -172.7(2) . . . . ? N7 Re2 P4 C81 96.5(2) . . . . ? O3 Re2 P4 C81 -63.5(2) . . . . ? N9 Re2 P4 C81 23.5(2) . . . . ? P3 Re2 P4 C81 -84.7(3) . . . . ? N10 Re2 P4 C75 62.0(2) . . . . ? N7 Re2 P4 C75 -28.7(2) . . . . ? O3 Re2 P4 C75 171.3(2) . . . . ? N9 Re2 P4 C75 -101.7(2) . . . . ? P3 Re2 P4 C75 150.0(3) . . . . ? N10 Re2 P4 C87 -52.7(2) . . . . ? N7 Re2 P4 C87 -143.4(2) . . . . ? O3 Re2 P4 C87 56.6(2) . . . . ? N9 Re2 P4 C87 143.6(2) . . . . ? P3 Re2 P4 C87 35.3(3) . . . . ? N4 Re1 O1 C1 -97.9(4) . . . . ? N1 Re1 O1 C1 73.5(6) . . . . ? N3 Re1 O1 C1 80.3(4) . . . . ? P1 Re1 O1 C1 -6.0(4) . . . . ? P2 Re1 O1 C1 177.0(4) . . . . ? N10 Re2 O3 C47 -95.8(4) . . . . ? N7 Re2 O3 C47 76.6(6) . . . . ? N9 Re2 O3 C47 82.7(4) . . . . ? P3 Re2 O3 C47 -4.9(4) . . . . ? P4 Re2 O3 C47 179.9(4) . . . . ? N4 Re1 N1 N2 173.4(5) . . . . ? O1 Re1 N1 N2 1.6(8) . . . . ? N3 Re1 N1 N2 -5.6(4) . . . . ? P1 Re1 N1 N2 78.6(5) . . . . ? P2 Re1 N1 N2 -99.9(4) . . . . ? Re1 N1 N2 C19 4.4(7) . . . . ? N4 Re1 N3 C23 175.3(5) . . . . ? N1 Re1 N3 C23 178.5(5) . . . . ? O1 Re1 N3 C23 0.9(4) . . . . ? P1 Re1 N3 C23 82.0(4) . . . . ? P2 Re1 N3 C23 -85.0(4) . . . . ? N4 Re1 N3 C19 2.1(8) . . . . ? N1 Re1 N3 C19 5.3(4) . . . . ? O1 Re1 N3 C19 -172.3(4) . . . . ? P1 Re1 N3 C19 -91.2(4) . . . . ? P2 Re1 N3 C19 101.8(3) . . . . ? N1 Re1 N4 N5 10(7) . . . . ? O1 Re1 N4 N5 -172(7) . . . . ? N3 Re1 N4 N5 13(8) . . . . ? P1 Re1 N4 N5 105(7) . . . . ? P2 Re1 N4 N5 -88(7) . . . . ? Re1 N4 N5 C24 -1(8) . . . . ? N10 Re2 N7 N8 175.9(4) . . . . ? O3 Re2 N7 N8 3.1(8) . . . . ? N9 Re2 N7 N8 -3.3(4) . . . . ? P3 Re2 N7 N8 81.9(4) . . . . ? P4 Re2 N7 N8 -98.4(4) . . . . ? Re2 N7 N8 C65 2.7(6) . . . . ? N10 Re2 N9 C69 173.9(5) . . . . ? N7 Re2 N9 C69 176.6(5) . . . . ? O3 Re2 N9 C69 -1.2(4) . . . . ? P3 Re2 N9 C69 79.8(4) . . . . ? P4 Re2 N9 C69 -87.7(4) . . . . ? N10 Re2 N9 C65 0.3(8) . . . . ? N7 Re2 N9 C65 3.0(3) . . . . ? O3 Re2 N9 C65 -174.7(4) . . . . ? P3 Re2 N9 C65 -93.8(3) . . . . ? P4 Re2 N9 C65 98.7(3) . . . . ? N7 Re2 N10 N11 41(6) . . . . ? O3 Re2 N10 N11 -141(6) . . . . ? N9 Re2 N10 N11 44(6) . . . . ? P3 Re2 N10 N11 137(6) . . . . ? P4 Re2 N10 N11 -56(6) . . . . ? Re2 N10 N11 C70 -42(6) . . . . ? Re1 O1 C1 C6 6.6(7) . . . . ? Re1 O1 C1 C2 -171.8(4) . . . . ? O1 C1 C2 C3 178.7(6) . . . . ? C6 C1 C2 C3 0.3(10) . . . . ? C1 C2 C3 C4 -0.4(11) . . . . ? C2 C3 C4 C5 -0.4(12) . . . . ? C3 C4 C5 C6 1.3(11) . . . . ? O1 C1 C6 C5 -177.9(5) . . . . ? C2 C1 C6 C5 0.5(9) . . . . ? O1 C1 C6 P1 -2.1(8) . . . . ? C2 C1 C6 P1 176.3(5) . . . . ? C4 C5 C6 C1 -1.3(10) . . . . ? C4 C5 C6 P1 -176.6(5) . . . . ? C13 P1 C6 C1 -123.4(4) . . . . ? C7 P1 C6 C1 120.0(5) . . . . ? Re1 P1 C6 C1 -2.2(5) . . . . ? C13 P1 C6 C5 52.1(6) . . . . ? C7 P1 C6 C5 -64.5(6) . . . . ? Re1 P1 C6 C5 173.4(5) . . . . ? C6 P1 C7 C8 18.3(5) . . . . ? C13 P1 C7 C8 -99.2(5) . . . . ? Re1 P1 C7 C8 130.5(4) . . . . ? C6 P1 C7 C12 -162.1(4) . . . . ? C13 P1 C7 C12 80.3(5) . . . . ? Re1 P1 C7 C12 -49.9(5) . . . . ? C12 C7 C8 C9 -1.5(8) . . . . ? P1 C7 C8 C9 178.1(4) . . . . ? C7 C8 C9 C10 1.4(9) . . . . ? C8 C9 C10 C11 -0.1(10) . . . . ? C9 C10 C11 C12 -1.1(10) . . . . ? C8 C7 C12 C11 0.3(9) . . . . ? P1 C7 C12 C11 -179.3(5) . . . . ? C10 C11 C12 C7 1.0(10) . . . . ? C6 P1 C13 C18 17.4(5) . . . . ? C7 P1 C13 C18 135.9(5) . . . . ? Re1 P1 C13 C18 -93.7(5) . . . . ? C6 P1 C13 C14 -168.7(4) . . . . ? C7 P1 C13 C14 -50.2(5) . . . . ? Re1 P1 C13 C14 80.2(5) . . . . ? C18 C13 C14 C15 -1.3(9) . . . . ? P1 C13 C14 C15 -175.2(5) . . . . ? C13 C14 C15 C16 0.3(9) . . . . ? C14 C15 C16 C17 1.3(10) . . . . ? C15 C16 C17 C18 -1.9(10) . . . . ? C16 C17 C18 C13 0.9(10) . . . . ? C14 C13 C18 C17 0.7(9) . . . . ? P1 C13 C18 C17 174.6(5) . . . . ? N1 N2 C19 N3 1.2(7) . . . . ? N1 N2 C19 C20 -178.9(5) . . . . ? C23 N3 C19 N2 -179.2(5) . . . . ? Re1 N3 C19 N2 -5.3(6) . . . . ? C23 N3 C19 C20 0.9(8) . . . . ? Re1 N3 C19 C20 174.8(4) . . . . ? N2 C19 C20 C21 179.3(5) . . . . ? N3 C19 C20 C21 -0.7(9) . . . . ? C19 C20 C21 C22 -0.1(9) . . . . ? C20 C21 C22 C23 0.6(9) . . . . ? C19 N3 C23 C22 -0.3(8) . . . . ? Re1 N3 C23 C22 -173.2(4) . . . . ? C21 C22 C23 N3 -0.4(9) . . . . ? C28 N6 C24 C25 -2.7(11) . . . . ? C28 N6 C24 N5 179.1(7) . . . . ? N4 N5 C24 N6 2.5(8) . . . . ? N4 N5 C24 C25 -175.8(5) . . . . ? N6 C24 C25 C26 1.8(11) . . . . ? N5 C24 C25 C26 -179.9(6) . . . . ? C24 C25 C26 C27 -0.8(13) . . . . ? C25 C26 C27 C28 0.8(15) . . . . ? C24 N6 C28 C27 2.7(13) . . . . ? C26 C27 C28 N6 -1.8(16) . . . . ? C35 P2 C29 C34 123.7(5) . . . . ? C41 P2 C29 C34 17.9(5) . . . . ? Re1 P2 C29 C34 -103.4(5) . . . . ? C35 P2 C29 C30 -63.0(5) . . . . ? C41 P2 C29 C30 -168.8(4) . . . . ? Re1 P2 C29 C30 69.9(5) . . . . ? C34 C29 C30 O2 -178.7(5) . . . . ? P2 C29 C30 O2 7.9(7) . . . . ? C34 C29 C30 C31 0.9(9) . . . . ? P2 C29 C30 C31 -172.5(4) . . . . ? O2 C30 C31 C32 179.2(6) . . . . ? C29 C30 C31 C32 -0.4(9) . . . . ? C30 C31 C32 C33 -0.2(11) . . . . ? C31 C32 C33 C34 0.4(11) . . . . ? C32 C33 C34 C29 0.1(10) . . . . ? C30 C29 C34 C33 -0.7(9) . . . . ? P2 C29 C34 C33 172.5(5) . . . . ? C29 P2 C35 C36 -7.8(5) . . . . ? C41 P2 C35 C36 98.6(5) . . . . ? Re1 P2 C35 C36 -135.6(4) . . . . ? C29 P2 C35 C40 177.6(4) . . . . ? C41 P2 C35 C40 -75.9(4) . . . . ? Re1 P2 C35 C40 49.9(5) . . . . ? C40 C35 C36 C37 1.7(8) . . . . ? P2 C35 C36 C37 -172.7(4) . . . . ? C35 C36 C37 C38 -1.6(9) . . . . ? C36 C37 C38 C39 0.9(10) . . . . ? C37 C38 C39 C40 -0.4(9) . . . . ? C38 C39 C40 C35 0.5(9) . . . . ? C36 C35 C40 C39 -1.2(8) . . . . ? P2 C35 C40 C39 173.5(4) . . . . ? C35 P2 C41 C42 -34.4(5) . . . . ? C29 P2 C41 C42 77.4(5) . . . . ? Re1 P2 C41 C42 -164.0(4) . . . . ? C35 P2 C41 C46 147.6(5) . . . . ? C29 P2 C41 C46 -100.5(5) . . . . ? Re1 P2 C41 C46 18.1(5) . . . . ? C46 C41 C42 C43 1.0(9) . . . . ? P2 C41 C42 C43 -177.0(5) . . . . ? C41 C42 C43 C44 0.5(11) . . . . ? C42 C43 C44 C45 -1.9(11) . . . . ? C43 C44 C45 C46 1.8(10) . . . . ? C44 C45 C46 C41 -0.3(9) . . . . ? C42 C41 C46 C45 -1.1(8) . . . . ? P2 C41 C46 C45 176.9(4) . . . . ? Re2 O3 C47 C48 -170.8(5) . . . . ? Re2 O3 C47 C52 3.9(7) . . . . ? O3 C47 C48 C49 179.0(7) . . . . ? C52 C47 C48 C49 4.2(11) . . . . ? C47 C48 C49 C50 -2.8(14) . . . . ? C48 C49 C50 C51 0.0(15) . . . . ? C49 C50 C51 C52 1.2(13) . . . . ? C50 C51 C52 C47 0.2(11) . . . . ? C50 C51 C52 P3 -177.9(6) . . . . ? O3 C47 C52 C51 -177.6(6) . . . . ? C48 C47 C52 C51 -3.0(10) . . . . ? O3 C47 C52 P3 0.7(7) . . . . ? C48 C47 C52 P3 175.4(5) . . . . ? C53 P3 C52 C51 -63.2(6) . . . . ? C59 P3 C52 C51 54.0(6) . . . . ? Re2 P3 C52 C51 174.5(6) . . . . ? C53 P3 C52 C47 118.7(5) . . . . ? C59 P3 C52 C47 -124.2(5) . . . . ? Re2 P3 C52 C47 -3.7(5) . . . . ? C52 P3 C53 C54 20.1(5) . . . . ? C59 P3 C53 C54 -99.0(5) . . . . ? Re2 P3 C53 C54 132.8(4) . . . . ? C52 P3 C53 C58 -159.4(4) . . . . ? C59 P3 C53 C58 81.5(5) . . . . ? Re2 P3 C53 C58 -46.7(5) . . . . ? C58 C53 C54 C55 0.2(9) . . . . ? P3 C53 C54 C55 -179.3(5) . . . . ? C53 C54 C55 C56 1.1(10) . . . . ? C54 C55 C56 C57 -1.4(10) . . . . ? C55 C56 C57 C58 0.3(9) . . . . ? C56 C57 C58 C53 1.0(9) . . . . ? C54 C53 C58 C57 -1.3(8) . . . . ? P3 C53 C58 C57 178.3(4) . . . . ? C52 P3 C59 C60 -172.5(4) . . . . ? C53 P3 C59 C60 -52.6(5) . . . . ? Re2 P3 C59 C60 76.3(4) . . . . ? C52 P3 C59 C64 15.4(5) . . . . ? C53 P3 C59 C64 135.3(5) . . . . ? Re2 P3 C59 C64 -95.8(5) . . . . ? C64 C59 C60 C61 -1.6(9) . . . . ? P3 C59 C60 C61 -173.8(4) . . . . ? C59 C60 C61 C62 1.7(9) . . . . ? C60 C61 C62 C63 -0.7(10) . . . . ? C61 C62 C63 C64 -0.5(11) . . . . ? C62 C63 C64 C59 0.6(10) . . . . ? C60 C59 C64 C63 0.5(9) . . . . ? P3 C59 C64 C63 172.4(5) . . . . ? N7 N8 C65 N9 0.5(6) . . . . ? N7 N8 C65 C66 -178.2(5) . . . . ? C69 N9 C65 N8 -177.1(5) . . . . ? Re2 N9 C65 N8 -2.9(6) . . . . ? C69 N9 C65 C66 1.6(8) . . . . ? Re2 N9 C65 C66 175.8(4) . . . . ? N8 C65 C66 C67 176.3(5) . . . . ? N9 C65 C66 C67 -2.3(9) . . . . ? C65 C66 C67 C68 1.5(9) . . . . ? C66 C67 C68 C69 0.0(9) . . . . ? C65 N9 C69 C68 0.0(8) . . . . ? Re2 N9 C69 C68 -173.3(4) . . . . ? C67 C68 C69 N9 -0.8(9) . . . . ? C74 N12 C70 C71 -0.2(8) . . . . ? C74 N12 C70 N11 -177.7(5) . . . . ? N10 N11 C70 N12 -1.2(7) . . . . ? N10 N11 C70 C71 -178.8(5) . . . . ? N12 C70 C71 C72 -0.1(9) . . . . ? N11 C70 C71 C72 177.4(5) . . . . ? C70 C71 C72 C73 0.2(10) . . . . ? C71 C72 C73 C74 0.1(11) . . . . ? C70 N12 C74 C73 0.4(9) . . . . ? C72 C73 C74 N12 -0.4(11) . . . . ? C81 P4 C75 C80 134.9(5) . . . . ? C87 P4 C75 C80 26.0(5) . . . . ? Re2 P4 C75 C80 -93.1(5) . . . . ? C81 P4 C75 C76 -57.8(5) . . . . ? C87 P4 C75 C76 -166.7(4) . . . . ? Re2 P4 C75 C76 74.2(5) . . . . ? C80 C75 C76 O4 177.6(5) . . . . ? P4 C75 C76 O4 10.1(7) . . . . ? C80 C75 C76 C77 -1.1(8) . . . . ? P4 C75 C76 C77 -168.6(4) . . . . ? O4 C76 C77 C78 -176.2(6) . . . . ? C75 C76 C77 C78 2.4(9) . . . . ? C76 C77 C78 C79 -2.6(11) . . . . ? C77 C78 C79 C80 1.4(11) . . . . ? C78 C79 C80 C75 -0.2(10) . . . . ? C76 C75 C80 C79 0.1(9) . . . . ? P4 C75 C80 C79 167.3(5) . . . . ? C75 P4 C81 C86 168.0(4) . . . . ? C87 P4 C81 C86 -81.1(5) . . . . ? Re2 P4 C81 C86 43.6(5) . . . . ? C75 P4 C81 C82 -14.7(6) . . . . ? C87 P4 C81 C82 96.2(5) . . . . ? Re2 P4 C81 C82 -139.1(4) . . . . ? C86 C81 C82 C83 -0.8(9) . . . . ? P4 C81 C82 C83 -178.0(5) . . . . ? C81 C82 C83 C84 1.1(11) . . . . ? C82 C83 C84 C85 -0.6(12) . . . . ? C83 C84 C85 C86 -0.3(11) . . . . ? C84 C85 C86 C81 0.6(9) . . . . ? C82 C81 C86 C85 0.0(9) . . . . ? P4 C81 C86 C85 177.3(5) . . . . ? C81 P4 C87 C92 127.4(5) . . . . ? C75 P4 C87 C92 -118.8(5) . . . . ? Re2 P4 C87 C92 -2.9(5) . . . . ? C81 P4 C87 C88 -52.3(5) . . . . ? C75 P4 C87 C88 61.5(5) . . . . ? Re2 P4 C87 C88 177.3(4) . . . . ? C92 C87 C88 C89 -2.0(9) . . . . ? P4 C87 C88 C89 177.7(5) . . . . ? C87 C88 C89 C90 1.9(10) . . . . ? C88 C89 C90 C91 -0.6(10) . . . . ? C89 C90 C91 C92 -0.5(9) . . . . ? C88 C87 C92 C91 0.9(8) . . . . ? P4 C87 C92 C91 -178.8(4) . . . . ? C90 C91 C92 C87 0.4(8) . . . . ? _diffrn_measured_fraction_theta_max 0.803 _diffrn_reflns_theta_full 27.89 _diffrn_measured_fraction_theta_full 0.803 _refine_diff_density_max 4.371 _refine_diff_density_min -2.188 _refine_diff_density_rms 0.146 #===END data_[ReCl(Hhypy)(hypy)(PO)] _database_code_CSD 168624 _audit_creation_method SHELXL-97 _chemical_formula_sum 'C28 H23 Cl N6 O P Re' _chemical_formula_weight 712.14 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Re' 'Re' -5.2083 5.8923 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P2(1)2(1)2(1)' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' _cell_length_a 12.294(2) _cell_length_b 14.500(4) _cell_length_c 14.999(5) _cell_angle_alpha 90.00(2) _cell_angle_beta 90.00(2) _cell_angle_gamma 90.00(2) _cell_volume 2673.8(12) _cell_formula_units_Z 4 _cell_measurement_temperature 153(5) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 27.3 _cell_measurement_theta_max 29.5 _exptl_crystal_description rod _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 1.769 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1392 _exptl_absorpt_coefficient_mu 10.651 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.4055 _exptl_absorpt_correction_T_max 0.7796 _exptl_absorpt_process_details SHELX-76 _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(5) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CAD4 diffractometer' _diffrn_measurement_method 'omega-theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_time 3600 _diffrn_standards_decay_% 1 _diffrn_reflns_number 4008 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0157 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 4.24 _diffrn_reflns_theta_max 70.04 _reflns_number_total 3982 _reflns_number_gt 3949 _reflns_threshold_expression >2sigma(I) _computing_data_collection CAD4 _computing_cell_refinement CAD4 _computing_data_reduction 'local program' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XPMA/ZORTEP (Zsolnai, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness 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 threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) 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_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+6.5000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00049(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.215(10) _refine_ls_number_reflns 3982 _refine_ls_number_parameters 431 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0260 _refine_ls_R_factor_gt 0.0257 _refine_ls_wR_factor_ref 0.0676 _refine_ls_wR_factor_gt 0.0675 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 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 Re1 Re 0.142696(17) 0.488335(14) 0.381549(14) 0.01525(9) Uani 1 1 d . . . Cl1 Cl 0.02186(11) 0.56723(10) 0.48288(9) 0.0241(3) Uani 1 1 d . . . N1 N 0.0342(4) 0.4414(3) 0.3175(3) 0.0193(10) Uani 1 1 d . . . N2 N -0.0447(4) 0.4160(4) 0.2726(3) 0.0230(11) Uani 1 1 d . . . N3 N -0.0109(4) 0.5379(3) 0.1695(3) 0.0225(10) Uani 1 1 d . . . N4 N 0.1631(4) 0.5858(3) 0.2943(3) 0.0195(10) Uani 1 1 d . . . H4N H 0.129(5) 0.585(4) 0.249(5) 0.023 Uiso 1 1 d . . . N5 N 0.2322(4) 0.6547(3) 0.2960(3) 0.0233(11) Uani 1 1 d . . . N6 N 0.2687(4) 0.5773(3) 0.4287(3) 0.0186(10) Uani 1 1 d . . . C1 C -0.0761(5) 0.4695(4) 0.1967(4) 0.0208(11) Uani 1 1 d . . . C2 C -0.1743(5) 0.4475(6) 0.1566(5) 0.0325(15) Uani 1 1 d . . . H2 H -0.198(6) 0.404(5) 0.170(4) 0.019(19) Uiso 1 1 d . . . C3 C -0.2102(5) 0.5012(6) 0.0874(4) 0.0392(17) Uani 1 1 d . . . H3 H -0.283(6) 0.494(6) 0.061(5) 0.040(19) Uiso 1 1 d . . . C4 C -0.1452(6) 0.5722(5) 0.0577(4) 0.0336(14) Uani 1 1 d . . . H4 H -0.169(6) 0.607(5) 0.008(5) 0.04(2) Uiso 1 1 d . . . C5 C -0.0470(5) 0.5868(5) 0.0997(4) 0.0273(13) Uani 1 1 d . . . H5 H -0.011(5) 0.634(5) 0.085(4) 0.024(18) Uiso 1 1 d . . . C6 C 0.2921(4) 0.6490(4) 0.3737(4) 0.0211(11) Uani 1 1 d . . . C7 C 0.3711(5) 0.7142(4) 0.3941(4) 0.0255(12) Uani 1 1 d . . . H7 H 0.387(5) 0.762(5) 0.362(5) 0.030(18) Uiso 1 1 d . . . C8 C 0.4258(5) 0.7059(4) 0.4737(4) 0.0280(14) Uani 1 1 d . . . H8 H 0.465(6) 0.751(5) 0.490(5) 0.034 Uiso 1 1 d . . . C9 C 0.4033(5) 0.6326(4) 0.5293(4) 0.0287(14) Uani 1 1 d . . . H9 H 0.435(5) 0.624(4) 0.583(4) 0.021(16) Uiso 1 1 d . . . C10 C 0.3248(5) 0.5706(4) 0.5068(4) 0.0215(12) Uani 1 1 d . . . H10 H 0.308(6) 0.523(6) 0.538(5) 0.04(2) Uiso 1 1 d . . . P1 P 0.28173(11) 0.38834(10) 0.32435(9) 0.0158(3) Uani 1 1 d . . . O1 O 0.1671(3) 0.4082(3) 0.4911(3) 0.0212(8) Uani 1 1 d . . . C11 C 0.2520(4) 0.3053(4) 0.2375(3) 0.0171(11) Uani 1 1 d . . . C12 C 0.1576(5) 0.2528(4) 0.2465(4) 0.0227(12) Uani 1 1 d . . . H12 H 0.102(6) 0.264(5) 0.296(5) 0.04(2) Uiso 1 1 d . . . C13 C 0.1329(5) 0.1837(4) 0.1846(4) 0.0245(12) Uani 1 1 d . . . H13 H 0.072(6) 0.150(5) 0.189(4) 0.029 Uiso 1 1 d . . . C14 C 0.2046(5) 0.1666(4) 0.1158(4) 0.0253(12) Uani 1 1 d . . . H14 H 0.184(5) 0.114(5) 0.073(5) 0.028(18) Uiso 1 1 d . . . C15 C 0.2978(5) 0.2186(4) 0.1067(4) 0.0273(13) Uani 1 1 d . . . H15 H 0.343(6) 0.207(5) 0.067(5) 0.033(19) Uiso 1 1 d . . . C16 C 0.3227(5) 0.2876(4) 0.1664(4) 0.0238(12) Uani 1 1 d . . . H16 H 0.392(6) 0.320(5) 0.160(4) 0.029 Uiso 1 1 d . . . C17 C 0.4028(4) 0.4492(4) 0.2918(4) 0.0192(11) Uani 1 1 d . . . C18 C 0.4022(4) 0.5004(4) 0.2120(3) 0.0229(12) Uani 1 1 d . . . H18 H 0.333(5) 0.493(5) 0.171(4) 0.028 Uiso 1 1 d . . . C19 C 0.4908(5) 0.5525(4) 0.1878(4) 0.0263(13) Uani 1 1 d . . . H19 H 0.485(5) 0.574(5) 0.135(5) 0.032(19) Uiso 1 1 d . . . C20 C 0.5812(5) 0.5563(5) 0.2426(4) 0.0311(14) Uani 1 1 d . . . H20 H 0.627(6) 0.590(5) 0.227(5) 0.03(2) Uiso 1 1 d . . . C21 C 0.5823(5) 0.5060(5) 0.3213(4) 0.0326(14) Uani 1 1 d . . . H21 H 0.641(5) 0.505(4) 0.345(5) 0.029(17) Uiso 1 1 d . . . C22 C 0.4954(5) 0.4520(4) 0.3455(4) 0.0260(13) Uani 1 1 d . . . H22 H 0.494(7) 0.412(6) 0.407(6) 0.06(3) Uiso 1 1 d . . . C23 C 0.3095(5) 0.3209(4) 0.4227(4) 0.0177(11) Uani 1 1 d . . . C24 C 0.3875(5) 0.2515(4) 0.4289(4) 0.0216(12) Uani 1 1 d . . . H24 H 0.432(6) 0.237(5) 0.389(5) 0.034(19) Uiso 1 1 d . . . C25 C 0.4005(5) 0.2025(4) 0.5081(4) 0.0266(13) Uani 1 1 d . . . H25 H 0.456(5) 0.155(4) 0.515(4) 0.019(15) Uiso 1 1 d . . . C26 C 0.3351(5) 0.2249(4) 0.5808(4) 0.0255(13) Uani 1 1 d . . . H26 H 0.345(7) 0.192(5) 0.632(6) 0.05(2) Uiso 1 1 d . . . C27 C 0.2575(5) 0.2934(4) 0.5750(4) 0.0235(12) Uani 1 1 d . . . H27 H 0.215(6) 0.309(5) 0.618(5) 0.032(18) Uiso 1 1 d . . . C28 C 0.2432(4) 0.3425(4) 0.4956(4) 0.0176(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.01807(13) 0.01560(13) 0.01207(13) 0.00228(8) -0.00060(8) 0.00074(8) Cl1 0.0257(6) 0.0268(7) 0.0197(7) 0.0008(6) 0.0029(5) 0.0092(6) N1 0.023(2) 0.020(2) 0.015(2) 0.0042(19) 0.0051(19) 0.0016(19) N2 0.018(2) 0.031(3) 0.020(2) 0.002(2) -0.0007(19) -0.006(2) N3 0.026(2) 0.027(3) 0.014(2) -0.002(2) 0.0008(19) 0.003(2) N4 0.023(2) 0.023(2) 0.013(2) -0.0013(19) -0.0023(19) 0.000(2) N5 0.030(3) 0.023(2) 0.017(2) 0.004(2) -0.003(2) -0.002(2) N6 0.020(2) 0.018(2) 0.018(2) -0.0003(19) -0.0007(19) 0.0008(19) C1 0.022(3) 0.025(3) 0.015(2) -0.002(2) -0.002(2) 0.004(2) C2 0.027(3) 0.044(4) 0.026(3) -0.001(3) -0.001(3) -0.004(3) C3 0.028(3) 0.073(5) 0.017(3) -0.006(3) -0.007(2) 0.001(4) C4 0.035(3) 0.046(4) 0.020(3) 0.001(3) 0.004(3) 0.014(3) C5 0.033(3) 0.034(3) 0.015(3) 0.003(3) 0.002(2) 0.004(3) C6 0.022(3) 0.023(3) 0.018(3) -0.002(2) 0.002(2) 0.003(2) C7 0.023(3) 0.025(3) 0.028(3) 0.000(2) -0.002(3) -0.005(2) C8 0.025(3) 0.023(3) 0.036(4) -0.010(3) -0.005(3) -0.002(3) C9 0.034(3) 0.029(3) 0.022(3) -0.010(3) -0.011(3) 0.006(3) C10 0.026(3) 0.022(3) 0.016(3) 0.000(2) -0.004(2) 0.002(2) P1 0.0181(6) 0.0173(6) 0.0121(6) 0.0003(5) -0.0004(5) -0.0002(5) O1 0.023(2) 0.0178(19) 0.022(2) 0.0003(16) 0.0008(16) 0.0049(16) C11 0.023(3) 0.016(2) 0.012(3) 0.001(2) -0.001(2) 0.001(2) C12 0.025(3) 0.023(3) 0.021(3) 0.003(2) 0.001(2) -0.007(2) C13 0.030(3) 0.020(3) 0.023(3) 0.000(2) -0.001(3) -0.007(3) C14 0.027(3) 0.025(3) 0.025(3) -0.006(3) -0.007(3) 0.003(2) C15 0.024(3) 0.034(3) 0.023(3) -0.008(3) 0.003(3) 0.001(2) C16 0.023(3) 0.028(3) 0.021(3) -0.004(2) 0.001(2) 0.000(2) C17 0.024(3) 0.018(3) 0.016(3) -0.002(2) -0.001(2) -0.004(2) C18 0.029(3) 0.022(3) 0.017(3) -0.001(2) 0.002(2) -0.003(2) C19 0.037(3) 0.028(3) 0.014(3) 0.000(3) 0.000(3) -0.006(3) C20 0.028(3) 0.033(3) 0.032(4) -0.001(3) 0.006(3) -0.010(3) C21 0.025(3) 0.043(4) 0.031(3) 0.010(3) -0.008(2) -0.011(3) C22 0.029(3) 0.032(3) 0.017(3) 0.003(3) -0.004(2) 0.000(3) C23 0.024(3) 0.017(3) 0.012(2) -0.002(2) 0.000(2) 0.000(2) C24 0.027(3) 0.022(3) 0.016(3) 0.000(2) -0.001(2) 0.003(2) C25 0.033(3) 0.023(3) 0.023(3) -0.002(2) -0.006(3) 0.008(3) C26 0.036(3) 0.025(3) 0.015(3) 0.006(2) -0.006(3) 0.005(3) C27 0.030(3) 0.024(3) 0.016(3) 0.003(2) -0.001(3) 0.002(3) C28 0.020(3) 0.013(2) 0.019(3) 0.000(2) -0.002(2) -0.002(2) _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 Re1 N1 1.779(5) . ? Re1 N4 1.942(5) . ? Re1 O1 2.035(4) . ? Re1 N6 2.137(5) . ? Re1 P1 2.4000(15) . ? Re1 Cl1 2.4136(15) . ? N1 N2 1.237(7) . ? N2 C1 1.431(7) . ? N3 C5 1.340(8) . ? N3 C1 1.340(8) . ? N4 N5 1.312(7) . ? N4 H4N 0.80(7) . ? N5 C6 1.382(8) . ? N6 C6 1.358(7) . ? N6 C10 1.363(7) . ? C1 C2 1.385(9) . ? C2 C3 1.371(10) . ? C2 H2 0.72(7) . ? C3 C4 1.378(11) . ? C3 H3 0.98(7) . ? C4 C5 1.377(9) . ? C4 H4 0.94(7) . ? C5 H5 0.84(7) . ? C6 C7 1.390(8) . ? C7 C8 1.375(9) . ? C7 H7 0.87(7) . ? C8 C9 1.379(9) . ? C8 H8 0.85(8) . ? C9 C10 1.361(9) . ? C9 H9 0.90(7) . ? C10 H10 0.86(8) . ? P1 C17 1.798(6) . ? P1 C23 1.803(6) . ? P1 C11 1.811(6) . ? O1 C28 1.337(7) . ? C11 C12 1.394(8) . ? C11 C16 1.399(8) . ? C12 C13 1.399(8) . ? C12 H12 1.02(7) . ? C13 C14 1.380(9) . ? C13 H13 0.90(7) . ? C14 C15 1.378(9) . ? C14 H14 1.03(7) . ? C15 C16 1.377(9) . ? C15 H15 0.84(7) . ? C16 H16 0.98(7) . ? C17 C22 1.394(8) . ? C17 C18 1.409(8) . ? C18 C19 1.374(8) . ? C18 H18 1.06(6) . ? C19 C20 1.384(9) . ? C19 H19 0.85(7) . ? C20 C21 1.387(9) . ? C20 H20 0.79(7) . ? C21 C22 1.374(9) . ? C21 H21 0.81(7) . ? C22 H22 1.09(8) . ? C23 C24 1.394(8) . ? C23 C28 1.399(8) . ? C24 C25 1.393(8) . ? C24 H24 0.84(7) . ? C25 C26 1.393(9) . ? C25 H25 0.97(6) . ? C26 C27 1.380(8) . ? C26 H26 0.91(8) . ? C27 C28 1.400(8) . ? C27 H27 0.86(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 N1 Re1 N4 90.7(2) . . ? N1 Re1 O1 109.15(18) . . ? N4 Re1 O1 160.13(18) . . ? N1 Re1 N6 162.45(17) . . ? N4 Re1 N6 71.94(19) . . ? O1 Re1 N6 88.30(17) . . ? N1 Re1 P1 96.30(15) . . ? N4 Re1 P1 96.14(14) . . ? O1 Re1 P1 80.74(11) . . ? N6 Re1 P1 88.12(13) . . ? N1 Re1 Cl1 93.44(15) . . ? N4 Re1 Cl1 99.13(14) . . ? O1 Re1 Cl1 81.51(11) . . ? N6 Re1 Cl1 87.20(13) . . ? P1 Re1 Cl1 161.77(5) . . ? N2 N1 Re1 174.7(4) . . ? N1 N2 C1 118.9(5) . . ? C5 N3 C1 115.6(5) . . ? N5 N4 Re1 128.7(4) . . ? N5 N4 H4N 112(5) . . ? Re1 N4 H4N 119(5) . . ? N4 N5 C6 108.4(5) . . ? C6 N6 C10 118.0(5) . . ? C6 N6 Re1 114.5(4) . . ? C10 N6 Re1 127.5(4) . . ? N3 C1 C2 124.0(6) . . ? N3 C1 N2 118.9(5) . . ? C2 C1 N2 117.2(6) . . ? C3 C2 C1 118.7(7) . . ? C3 C2 H2 126(6) . . ? C1 C2 H2 115(6) . . ? C2 C3 C4 118.8(6) . . ? C2 C3 H3 122(5) . . ? C4 C3 H3 119(5) . . ? C5 C4 C3 118.4(6) . . ? C5 C4 H4 123(4) . . ? C3 C4 H4 118(4) . . ? N3 C5 C4 124.5(6) . . ? N3 C5 H5 117(5) . . ? C4 C5 H5 118(5) . . ? N6 C6 N5 116.4(5) . . ? N6 C6 C7 122.4(5) . . ? N5 C6 C7 121.2(5) . . ? C8 C7 C6 118.2(6) . . ? C8 C7 H7 116(4) . . ? C6 C7 H7 125(4) . . ? C7 C8 C9 119.6(6) . . ? C7 C8 H8 117(5) . . ? C9 C8 H8 123(5) . . ? C10 C9 C8 120.1(6) . . ? C10 C9 H9 116(4) . . ? C8 C9 H9 123(4) . . ? N6 C10 C9 121.6(6) . . ? N6 C10 H10 114(5) . . ? C9 C10 H10 124(5) . . ? C17 P1 C23 109.4(3) . . ? C17 P1 C11 107.3(3) . . ? C23 P1 C11 105.4(2) . . ? C17 P1 Re1 112.97(19) . . ? C23 P1 Re1 99.80(19) . . ? C11 P1 Re1 120.99(18) . . ? C28 O1 Re1 123.4(3) . . ? C12 C11 C16 119.4(5) . . ? C12 C11 P1 117.4(4) . . ? C16 C11 P1 123.0(4) . . ? C11 C12 C13 120.5(5) . . ? C11 C12 H12 123(4) . . ? C13 C12 H12 117(4) . . ? C14 C13 C12 119.1(6) . . ? C14 C13 H13 119(4) . . ? C12 C13 H13 121(4) . . ? C15 C14 C13 120.5(6) . . ? C15 C14 H14 123(4) . . ? C13 C14 H14 117(4) . . ? C16 C15 C14 121.2(6) . . ? C16 C15 H15 118(5) . . ? C14 C15 H15 121(5) . . ? C15 C16 C11 119.4(5) . . ? C15 C16 H16 119(4) . . ? C11 C16 H16 122(4) . . ? C22 C17 C18 118.6(5) . . ? C22 C17 P1 122.3(4) . . ? C18 C17 P1 119.0(4) . . ? C19 C18 C17 120.7(5) . . ? C19 C18 H18 123(3) . . ? C17 C18 H18 116(4) . . ? C18 C19 C20 120.1(6) . . ? C18 C19 H19 113(5) . . ? C20 C19 H19 127(5) . . ? C19 C20 C21 119.5(6) . . ? C19 C20 H20 115(5) . . ? C21 C20 H20 126(5) . . ? C22 C21 C20 121.1(6) . . ? C22 C21 H21 125(5) . . ? C20 C21 H21 113(5) . . ? C21 C22 C17 120.0(6) . . ? C21 C22 H22 123(4) . . ? C17 C22 H22 117(4) . . ? C24 C23 C28 120.8(5) . . ? C24 C23 P1 125.2(4) . . ? C28 C23 P1 114.0(4) . . ? C25 C24 C23 120.2(6) . . ? C25 C24 H24 115(5) . . ? C23 C24 H24 125(5) . . ? C26 C25 C24 118.9(5) . . ? C26 C25 H25 119(4) . . ? C24 C25 H25 122(4) . . ? C27 C26 C25 121.2(5) . . ? C27 C26 H26 121(5) . . ? C25 C26 H26 117(5) . . ? C26 C27 C28 120.5(6) . . ? C26 C27 H27 124(5) . . ? C28 C27 H27 115(5) . . ? O1 C28 C27 119.6(5) . . ? O1 C28 C23 121.9(5) . . ? C27 C28 C23 118.5(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 N4 Re1 N1 N2 -48(4) . . . . ? O1 Re1 N1 N2 133(4) . . . . ? N6 Re1 N1 N2 -41(5) . . . . ? P1 Re1 N1 N2 -145(4) . . . . ? Cl1 Re1 N1 N2 51(4) . . . . ? Re1 N1 N2 C1 44(5) . . . . ? N1 Re1 N4 N5 178.1(5) . . . . ? O1 Re1 N4 N5 -5.8(9) . . . . ? N6 Re1 N4 N5 0.5(5) . . . . ? P1 Re1 N4 N5 -85.5(5) . . . . ? Cl1 Re1 N4 N5 84.5(5) . . . . ? Re1 N4 N5 C6 -0.6(7) . . . . ? N1 Re1 N6 C6 -8.3(8) . . . . ? N4 Re1 N6 C6 -0.3(4) . . . . ? O1 Re1 N6 C6 177.6(4) . . . . ? P1 Re1 N6 C6 96.8(4) . . . . ? Cl1 Re1 N6 C6 -100.8(4) . . . . ? N1 Re1 N6 C10 170.5(6) . . . . ? N4 Re1 N6 C10 178.5(5) . . . . ? O1 Re1 N6 C10 -3.6(5) . . . . ? P1 Re1 N6 C10 -84.4(5) . . . . ? Cl1 Re1 N6 C10 78.0(5) . . . . ? C5 N3 C1 C2 0.9(8) . . . . ? C5 N3 C1 N2 -178.1(5) . . . . ? N1 N2 C1 N3 9.0(8) . . . . ? N1 N2 C1 C2 -170.0(5) . . . . ? N3 C1 C2 C3 -3.1(10) . . . . ? N2 C1 C2 C3 175.8(6) . . . . ? C1 C2 C3 C4 2.9(10) . . . . ? C2 C3 C4 C5 -0.6(10) . . . . ? C1 N3 C5 C4 1.6(9) . . . . ? C3 C4 C5 N3 -1.8(10) . . . . ? C10 N6 C6 N5 -178.8(5) . . . . ? Re1 N6 C6 N5 0.1(6) . . . . ? C10 N6 C6 C7 0.5(8) . . . . ? Re1 N6 C6 C7 179.4(4) . . . . ? N4 N5 C6 N6 0.2(7) . . . . ? N4 N5 C6 C7 -179.1(5) . . . . ? N6 C6 C7 C8 -0.9(8) . . . . ? N5 C6 C7 C8 178.3(5) . . . . ? C6 C7 C8 C9 1.7(9) . . . . ? C7 C8 C9 C10 -2.1(9) . . . . ? C6 N6 C10 C9 -0.9(8) . . . . ? Re1 N6 C10 C9 -179.6(4) . . . . ? C8 C9 C10 N6 1.7(9) . . . . ? N1 Re1 P1 C17 132.6(2) . . . . ? N4 Re1 P1 C17 41.2(2) . . . . ? O1 Re1 P1 C17 -119.0(2) . . . . ? N6 Re1 P1 C17 -30.4(2) . . . . ? Cl1 Re1 P1 C17 -105.5(2) . . . . ? N1 Re1 P1 C23 -111.4(2) . . . . ? N4 Re1 P1 C23 157.2(2) . . . . ? O1 Re1 P1 C23 -3.0(2) . . . . ? N6 Re1 P1 C23 85.6(2) . . . . ? Cl1 Re1 P1 C23 10.5(3) . . . . ? N1 Re1 P1 C11 3.4(3) . . . . ? N4 Re1 P1 C11 -88.0(3) . . . . ? O1 Re1 P1 C11 111.8(2) . . . . ? N6 Re1 P1 C11 -159.6(3) . . . . ? Cl1 Re1 P1 C11 125.2(2) . . . . ? N1 Re1 O1 C28 97.2(4) . . . . ? N4 Re1 O1 C28 -78.7(6) . . . . ? N6 Re1 O1 C28 -84.7(4) . . . . ? P1 Re1 O1 C28 3.7(4) . . . . ? Cl1 Re1 O1 C28 -172.1(4) . . . . ? C17 P1 C11 C12 -176.9(4) . . . . ? C23 P1 C11 C12 66.5(5) . . . . ? Re1 P1 C11 C12 -45.3(5) . . . . ? C17 P1 C11 C16 7.7(5) . . . . ? C23 P1 C11 C16 -108.8(5) . . . . ? Re1 P1 C11 C16 139.3(4) . . . . ? C16 C11 C12 C13 -0.7(8) . . . . ? P1 C11 C12 C13 -176.3(4) . . . . ? C11 C12 C13 C14 1.6(9) . . . . ? C12 C13 C14 C15 -1.8(9) . . . . ? C13 C14 C15 C16 1.1(10) . . . . ? C14 C15 C16 C11 -0.2(9) . . . . ? C12 C11 C16 C15 0.0(9) . . . . ? P1 C11 C16 C15 175.3(5) . . . . ? C23 P1 C17 C22 -9.1(6) . . . . ? C11 P1 C17 C22 -123.0(5) . . . . ? Re1 P1 C17 C22 101.0(5) . . . . ? C23 P1 C17 C18 174.8(4) . . . . ? C11 P1 C17 C18 60.9(5) . . . . ? Re1 P1 C17 C18 -75.0(5) . . . . ? C22 C17 C18 C19 -0.3(9) . . . . ? P1 C17 C18 C19 175.9(5) . . . . ? C17 C18 C19 C20 -1.1(9) . . . . ? C18 C19 C20 C21 1.0(10) . . . . ? C19 C20 C21 C22 0.4(11) . . . . ? C20 C21 C22 C17 -1.8(11) . . . . ? C18 C17 C22 C21 1.8(9) . . . . ? P1 C17 C22 C21 -174.3(5) . . . . ? C17 P1 C23 C24 -59.7(6) . . . . ? C11 P1 C23 C24 55.4(6) . . . . ? Re1 P1 C23 C24 -178.4(5) . . . . ? C17 P1 C23 C28 121.4(4) . . . . ? C11 P1 C23 C28 -123.4(4) . . . . ? Re1 P1 C23 C28 2.7(4) . . . . ? C28 C23 C24 C25 0.0(9) . . . . ? P1 C23 C24 C25 -178.8(4) . . . . ? C23 C24 C25 C26 -0.7(9) . . . . ? C24 C25 C26 C27 0.9(10) . . . . ? C25 C26 C27 C28 -0.5(10) . . . . ? Re1 O1 C28 C27 177.2(4) . . . . ? Re1 O1 C28 C23 -3.0(7) . . . . ? C26 C27 C28 O1 179.6(5) . . . . ? C26 C27 C28 C23 -0.2(9) . . . . ? C24 C23 C28 O1 -179.4(5) . . . . ? P1 C23 C28 O1 -0.5(7) . . . . ? C24 C23 C28 C27 0.4(8) . . . . ? P1 C23 C28 C27 179.4(4) . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 70.04 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.765 _refine_diff_density_min -2.222 _refine_diff_density_rms 0.120 #===END