Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Burns, Carol' 'Harmjanz, Michael' 'Scott, Brian L.' _publ_contact_author_name 'Dr Carol Burns' _publ_contact_author_address ; Chemistry Division Los Alamos National Laboratory MSJ514 Los Alamos NM 87545 UNITED STATES OF AMERICA ; _publ_contact_author_email 'CJB@LANL.GOV' _publ_requested_journal ' ChemComm' _publ_section_title ; First rhenium complexes based on cyclotriphosphazene scaffolds with exocyclic pyrazolyl substituents ; data_1a _database_code_CSD 183233 _audit_creation_method SHELXL-97 _chemical_name_common 'Compound 1a' _chemical_formula_sum 'C43 H52 Cl3 N15 O10 P3 Re3' _chemical_formula_weight 1696.86 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' '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 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.987(3) _cell_length_b 24.360(6) _cell_length_c 21.664(5) _cell_angle_alpha 90.00 _cell_angle_beta 101.356(4) _cell_angle_gamma 90.00 _cell_volume 5685(2) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'irregular plate' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.983 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3264 _exptl_absorpt_coefficient_mu 6.664 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4153 _exptl_absorpt_correction_T_max 0.6906 _exptl_absorpt_process_details 'DIFABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4/CCD' _diffrn_measurement_method '\f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% '< 2' _diffrn_reflns_number 9845 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1122 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.27 _diffrn_reflns_theta_max 25.35 _reflns_number_total 9845 _reflns_number_gt 6469 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. The program PLATON/SQUEEZE (A.L. Spek, 2001) was used to remove the electron density of four disordered ether molecules per unit cell; 148 electrons, 625\%A^3^. ; _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^)+(0.0735P)^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 9845 _refine_ls_number_parameters 649 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1264 _refine_ls_R_factor_gt 0.0732 _refine_ls_wR_factor_ref 0.1595 _refine_ls_wR_factor_gt 0.1458 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.084 _refine_ls_shift/su_max 0.001 _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 0.44633(5) 0.66621(2) 0.37086(3) 0.03146(18) Uani 1 1 d . . . Re2 Re 0.70400(6) 0.41689(3) 0.21021(3) 0.03402(18) Uani 1 1 d . . . Re3 Re 0.80631(6) 0.44803(3) 0.07716(3) 0.03810(19) Uani 1 1 d . . . Cl1 Cl 0.8443(3) 0.36659(16) 0.15030(19) 0.0415(10) Uani 1 1 d . . . Cl2 Cl 0.5934(3) 0.43491(16) 0.09910(19) 0.0405(10) Uani 1 1 d . . . Cl3 Cl 0.8315(4) 0.49482(16) 0.1824(2) 0.0466(11) Uani 1 1 d . . . P1 P 0.6807(3) 0.71659(15) 0.32225(17) 0.0262(9) Uani 1 1 d . . . P2 P 0.4835(3) 0.68758(15) 0.22513(18) 0.0277(9) Uani 1 1 d . . . P3 P 0.6759(3) 0.75298(16) 0.20075(18) 0.0281(9) Uani 1 1 d . . . O1 O 0.2894(12) 0.6592(6) 0.4731(7) 0.078(4) Uani 1 1 d . . . O2 O 0.3426(11) 0.5491(5) 0.3430(6) 0.065(4) Uani 1 1 d . . . O3 O 0.6453(11) 0.6079(5) 0.4671(6) 0.054(3) Uani 1 1 d . . . O4 O 0.7822(12) 0.3766(5) -0.0400(6) 0.066(4) Uani 1 1 d . . . O5 O 0.7235(14) 0.5497(6) -0.0010(7) 0.084(5) Uani 1 1 d . . . O6 O 1.0700(11) 0.4659(6) 0.0618(6) 0.075(4) Uani 1 1 d . . . O7 O 0.5302(10) 0.3229(4) 0.2260(5) 0.047(3) Uani 1 1 d . . . O8 O 0.5453(11) 0.4900(5) 0.2755(6) 0.063(4) Uani 1 1 d . . . O9 O 0.8584(12) 0.3897(6) 0.3404(6) 0.071(4) Uani 1 1 d . . . N1 N 0.5611(10) 0.6797(4) 0.2971(5) 0.029(3) Uani 1 1 d . . . N2 N 0.5484(10) 0.7208(5) 0.1795(6) 0.030(3) Uani 1 1 d . . . N3 N 0.7405(9) 0.7485(5) 0.2726(6) 0.030(3) Uani 1 1 d . . . N4 N 0.3136(10) 0.7068(4) 0.2942(6) 0.029(3) Uani 1 1 d . . . N5 N 0.3494(10) 0.7163(4) 0.2378(6) 0.028(3) Uani 1 1 d . . . N6 N 0.5294(10) 0.7468(5) 0.3944(5) 0.028(3) Uani 1 1 d . . . N7 N 0.6349(10) 0.7606(4) 0.3737(5) 0.026(3) Uani 1 1 d . . . N8 N 0.7843(10) 0.6773(4) 0.3688(5) 0.025(3) Uani 1 1 d . . . N9 N 0.8478(10) 0.7013(5) 0.4242(5) 0.034(3) Uani 1 1 d . . . N10 N 0.4365(10) 0.6290(5) 0.1906(6) 0.035(3) Uani 1 1 d . . . N11 N 0.3402(11) 0.6025(5) 0.2115(7) 0.046(4) Uani 1 1 d . . . N12 N 0.6562(10) 0.8189(5) 0.1786(5) 0.029(3) Uani 1 1 d . . . N13 N 0.5401(11) 0.8352(5) 0.1432(6) 0.040(3) Uani 1 1 d . . . N14 N 0.7838(9) 0.7304(5) 0.1606(6) 0.031(3) Uani 1 1 d . . . N15 N 0.8579(10) 0.6866(5) 0.1853(6) 0.040(3) Uani 1 1 d . . . C1 C 0.3508(14) 0.6636(7) 0.4338(9) 0.047(4) Uani 1 1 d . . . C2 C 0.3833(16) 0.5939(6) 0.3492(9) 0.049(5) Uani 1 1 d . . . C3 C 0.5735(15) 0.6297(7) 0.4320(8) 0.043(4) Uani 1 1 d . . . C4 C 0.1955(14) 0.7236(6) 0.2865(8) 0.038(4) Uani 1 1 d . . . C5 C 0.1587(14) 0.7444(6) 0.2250(7) 0.038(4) Uani 1 1 d . . . H5 H 0.0822 0.7602 0.2084 0.046 Uiso 1 1 calc R . . C6 C 0.2554(13) 0.7373(6) 0.1938(8) 0.040(4) Uani 1 1 d . . . C7 C 0.1194(13) 0.7185(7) 0.3364(8) 0.052(5) Uani 1 1 d . . . H7A H 0.1692 0.7029 0.3736 0.079 Uiso 1 1 calc R . . H7B H 0.0493 0.6952 0.3215 0.079 Uiso 1 1 calc R . . H7C H 0.0909 0.7542 0.3459 0.079 Uiso 1 1 calc R . . C8 C 0.2658(14) 0.7510(7) 0.1272(8) 0.051(5) Uani 1 1 d . . . H8A H 0.3464 0.7406 0.1204 0.077 Uiso 1 1 calc R . . H8B H 0.2543 0.7898 0.1204 0.077 Uiso 1 1 calc R . . H8C H 0.2032 0.7314 0.0983 0.077 Uiso 1 1 calc R . . C9 C 0.5133(13) 0.7873(7) 0.4326(7) 0.038(4) Uani 1 1 d . . . C10 C 0.6069(15) 0.8269(6) 0.4352(7) 0.040(4) Uani 1 1 d . . . H10 H 0.6144 0.8597 0.4577 0.049 Uiso 1 1 calc R . . C11 C 0.6825(14) 0.8083(6) 0.3992(7) 0.037(4) Uani 1 1 d . . . C12 C 0.4061(15) 0.7900(7) 0.4655(8) 0.059(5) Uani 1 1 d . . . H12A H 0.3556 0.7578 0.4555 0.088 Uiso 1 1 calc R . . H12B H 0.3575 0.8221 0.4519 0.088 Uiso 1 1 calc R . . H12C H 0.4364 0.7918 0.5101 0.088 Uiso 1 1 calc R . . C13 C 0.7984(15) 0.8356(7) 0.3836(9) 0.056(5) Uani 1 1 d . . . H13A H 0.8333 0.8123 0.3559 0.084 Uiso 1 1 calc R . . H13B H 0.8584 0.8414 0.4217 0.084 Uiso 1 1 calc R . . H13C H 0.7760 0.8703 0.3634 0.084 Uiso 1 1 calc R . . C14 C 0.9272(13) 0.6605(7) 0.4468(7) 0.040(4) Uani 1 1 d . . . C15 C 0.9220(13) 0.6153(6) 0.4097(7) 0.037(4) Uani 1 1 d . . . H15 H 0.9713 0.5840 0.4170 0.045 Uiso 1 1 calc R . . C16 C 0.8320(13) 0.6252(6) 0.3611(8) 0.034(4) Uani 1 1 d . . . C17 C 1.0127(16) 0.6723(8) 0.5113(8) 0.068(6) Uani 1 1 d . . . H17A H 0.9925 0.7075 0.5263 0.102 Uiso 1 1 calc R . . H17B H 1.0977 0.6722 0.5066 0.102 Uiso 1 1 calc R . . H17C H 1.0007 0.6445 0.5409 0.102 Uiso 1 1 calc R . . C18 C 0.7811(17) 0.5929(7) 0.3044(9) 0.073(7) Uani 1 1 d . . . H18A H 0.7145 0.6129 0.2787 0.110 Uiso 1 1 calc R . . H18B H 0.7505 0.5585 0.3165 0.110 Uiso 1 1 calc R . . H18C H 0.8452 0.5863 0.2809 0.110 Uiso 1 1 calc R . . C19 C 0.4836(14) 0.5944(6) 0.1496(8) 0.038(4) Uani 1 1 d . . . C20 C 0.4138(18) 0.5492(7) 0.1452(8) 0.059(6) Uani 1 1 d . . . H20 H 0.4198 0.5195 0.1190 0.070 Uiso 1 1 calc R . . C21 C 0.3284(15) 0.5534(7) 0.1869(8) 0.046(4) Uani 1 1 d . . . C22 C 0.5867(17) 0.6097(7) 0.1184(7) 0.062(6) Uani 1 1 d . . . H22A H 0.6182 0.6451 0.1331 0.093 Uiso 1 1 calc R . . H22B H 0.5572 0.6110 0.0736 0.093 Uiso 1 1 calc R . . H22C H 0.6517 0.5829 0.1281 0.093 Uiso 1 1 calc R . . C23 C 0.2372(16) 0.5140(7) 0.2005(10) 0.070(6) Uani 1 1 d . . . H23A H 0.1943 0.5293 0.2310 0.105 Uiso 1 1 calc R . . H23B H 0.2787 0.4809 0.2169 0.105 Uiso 1 1 calc R . . H23C H 0.1787 0.5059 0.1625 0.105 Uiso 1 1 calc R . . C24 C 0.7405(15) 0.8625(6) 0.1842(7) 0.039(4) Uani 1 1 d . . . C25 C 0.6801(17) 0.9048(7) 0.1586(9) 0.054(5) Uani 1 1 d . . . H25 H 0.7114 0.9403 0.1583 0.065 Uiso 1 1 calc R . . C26 C 0.5553(16) 0.8879(6) 0.1304(7) 0.039(4) Uani 1 1 d . . . C27 C 0.8745(13) 0.8578(7) 0.2171(9) 0.055(5) Uani 1 1 d . . . H27A H 0.8913 0.8208 0.2316 0.083 Uiso 1 1 calc R . . H27B H 0.8902 0.8824 0.2524 0.083 Uiso 1 1 calc R . . H27C H 0.9274 0.8671 0.1883 0.083 Uiso 1 1 calc R . . C28 C 0.4488(16) 0.9189(7) 0.0913(9) 0.064(6) Uani 1 1 d . . . H28A H 0.3780 0.8951 0.0810 0.095 Uiso 1 1 calc R . . H28B H 0.4722 0.9315 0.0533 0.095 Uiso 1 1 calc R . . H28C H 0.4284 0.9498 0.1148 0.095 Uiso 1 1 calc R . . C29 C 0.7875(13) 0.7387(6) 0.0957(7) 0.032(4) Uani 1 1 d . . . C30 C 0.8665(14) 0.6972(7) 0.0818(9) 0.047(4) Uani 1 1 d . . . H30 H 0.8867 0.6900 0.0429 0.057 Uiso 1 1 calc R . . C31 C 0.9097(14) 0.6683(6) 0.1392(9) 0.042(4) Uani 1 1 d . . . C32 C 0.7169(14) 0.7798(7) 0.0553(6) 0.046(5) Uani 1 1 d . . . H32A H 0.6708 0.8017 0.0795 0.070 Uiso 1 1 calc R . . H32B H 0.6606 0.7620 0.0218 0.070 Uiso 1 1 calc R . . H32C H 0.7726 0.8028 0.0380 0.070 Uiso 1 1 calc R . . C33 C 0.9973(14) 0.6211(8) 0.1503(10) 0.069(6) Uani 1 1 d . . . H33A H 1.0092 0.6101 0.1937 0.103 Uiso 1 1 calc R . . H33B H 1.0756 0.6318 0.1407 0.103 Uiso 1 1 calc R . . H33C H 0.9637 0.5910 0.1238 0.103 Uiso 1 1 calc R . . C34 C 0.7893(15) 0.4049(7) 0.0047(8) 0.044(4) Uani 1 1 d . . . C35 C 0.7593(16) 0.5109(7) 0.0278(9) 0.053(5) Uani 1 1 d . . . C36 C 0.9681(17) 0.4578(8) 0.0667(8) 0.052(5) Uani 1 1 d . . . C37 C 0.6016(14) 0.3579(6) 0.2194(7) 0.035(4) Uani 1 1 d . . . C38 C 0.6040(13) 0.4627(6) 0.2505(8) 0.038(4) Uani 1 1 d . . . C39 C 0.8001(14) 0.4012(6) 0.2907(8) 0.037(4) 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 0.0297(3) 0.0297(3) 0.0356(4) 0.0053(3) 0.0082(3) 0.0003(3) Re2 0.0355(4) 0.0343(3) 0.0317(4) 0.0008(3) 0.0051(3) -0.0002(3) Re3 0.0398(4) 0.0395(4) 0.0359(4) 0.0057(3) 0.0095(3) 0.0059(3) Cl1 0.044(2) 0.041(2) 0.038(3) 0.0020(19) 0.0070(18) 0.0131(18) Cl2 0.039(2) 0.042(2) 0.041(3) 0.0028(19) 0.0075(18) 0.0012(17) Cl3 0.051(2) 0.043(2) 0.049(3) -0.007(2) 0.017(2) -0.0101(19) P1 0.0268(19) 0.030(2) 0.019(2) -0.0001(17) -0.0016(16) 0.0008(16) P2 0.0176(18) 0.033(2) 0.030(2) -0.0046(18) -0.0023(16) 0.0014(15) P3 0.025(2) 0.035(2) 0.022(2) 0.0032(18) 0.0006(16) 0.0042(16) O1 0.068(9) 0.092(11) 0.082(11) 0.032(9) 0.036(8) 0.023(8) O2 0.075(9) 0.035(7) 0.086(10) 0.006(7) 0.023(8) -0.009(6) O3 0.054(8) 0.058(8) 0.044(8) 0.016(6) -0.005(6) 0.008(6) O4 0.092(10) 0.069(9) 0.037(9) 0.002(7) 0.015(7) 0.006(8) O5 0.123(12) 0.066(9) 0.078(11) 0.035(8) 0.060(9) 0.062(9) O6 0.047(8) 0.122(13) 0.056(9) 0.025(8) 0.007(7) 0.014(8) O7 0.059(7) 0.045(7) 0.036(7) 0.005(5) 0.005(6) -0.008(6) O8 0.064(8) 0.069(9) 0.059(9) 0.003(7) 0.018(7) 0.026(7) O9 0.071(9) 0.097(11) 0.042(9) 0.000(8) 0.001(7) 0.004(8) N1 0.023(6) 0.026(7) 0.033(8) 0.007(5) -0.005(5) -0.004(5) N2 0.022(6) 0.036(7) 0.031(8) -0.003(6) 0.003(5) -0.001(5) N3 0.016(6) 0.037(7) 0.035(8) -0.002(6) 0.002(5) -0.011(5) N4 0.031(7) 0.017(6) 0.038(8) -0.008(6) 0.007(6) -0.004(5) N5 0.026(6) 0.026(7) 0.034(8) -0.003(6) 0.009(6) 0.001(5) N6 0.026(6) 0.035(7) 0.023(7) 0.006(6) 0.007(5) 0.002(5) N7 0.023(6) 0.025(6) 0.026(7) -0.009(5) -0.003(5) 0.001(5) N8 0.026(6) 0.033(7) 0.013(7) 0.001(5) -0.004(5) 0.008(5) N9 0.028(7) 0.045(8) 0.023(8) 0.005(6) -0.009(5) 0.001(6) N10 0.024(6) 0.035(7) 0.040(8) -0.015(6) -0.012(6) -0.001(6) N11 0.032(7) 0.031(7) 0.067(11) -0.012(7) -0.006(7) -0.010(6) N12 0.031(7) 0.030(7) 0.022(7) 0.005(5) -0.003(5) 0.006(5) N13 0.035(7) 0.045(8) 0.040(9) 0.020(7) 0.008(6) 0.011(6) N14 0.018(6) 0.039(7) 0.036(8) -0.003(6) 0.005(5) 0.005(5) N15 0.023(7) 0.048(8) 0.048(9) 0.001(7) 0.003(6) -0.008(6) C1 0.038(9) 0.045(10) 0.058(13) 0.004(9) 0.012(9) 0.012(8) C2 0.059(11) 0.029(9) 0.071(14) 0.022(9) 0.042(10) 0.003(8) C3 0.042(10) 0.049(11) 0.041(12) 0.003(9) 0.015(9) -0.004(8) C4 0.042(10) 0.030(8) 0.042(11) -0.006(8) 0.006(8) 0.003(7) C5 0.039(9) 0.034(9) 0.034(11) -0.001(7) -0.010(8) 0.010(7) C6 0.019(8) 0.027(8) 0.066(13) -0.002(8) -0.016(8) 0.013(6) C7 0.031(9) 0.066(12) 0.067(13) 0.015(10) 0.025(9) 0.002(8) C8 0.037(10) 0.058(12) 0.051(13) 0.015(10) -0.011(8) -0.007(8) C9 0.027(8) 0.053(11) 0.035(10) 0.001(8) 0.006(7) 0.004(7) C10 0.060(11) 0.022(8) 0.037(11) -0.008(7) 0.004(8) 0.003(8) C11 0.042(9) 0.033(9) 0.031(10) -0.001(7) -0.006(7) 0.000(7) C12 0.053(11) 0.062(13) 0.058(13) -0.022(10) 0.003(9) 0.010(9) C13 0.056(11) 0.052(11) 0.065(14) -0.009(10) 0.023(10) -0.019(9) C14 0.032(8) 0.062(11) 0.028(10) -0.002(9) 0.009(7) 0.001(8) C15 0.029(8) 0.037(9) 0.041(11) -0.004(8) -0.001(7) 0.013(7) C16 0.028(8) 0.025(8) 0.052(11) -0.017(7) 0.012(7) 0.005(6) C17 0.060(12) 0.098(16) 0.034(12) -0.016(11) -0.018(9) 0.032(11) C18 0.075(14) 0.046(12) 0.088(17) -0.027(11) -0.012(12) 0.019(10) C19 0.042(9) 0.026(9) 0.045(11) -0.013(8) 0.005(8) 0.010(7) C20 0.092(15) 0.031(10) 0.038(12) -0.014(8) -0.024(10) 0.019(10) C21 0.039(10) 0.047(11) 0.043(12) -0.010(9) -0.014(8) 0.005(8) C22 0.095(15) 0.068(13) 0.018(11) -0.021(9) -0.004(9) 0.042(11) C23 0.059(12) 0.042(11) 0.103(18) -0.006(11) 0.000(12) -0.021(9) C24 0.052(10) 0.030(9) 0.034(10) -0.001(8) 0.009(8) 0.008(8) C25 0.074(13) 0.031(10) 0.059(13) 0.000(9) 0.020(10) 0.008(9) C26 0.062(11) 0.041(10) 0.013(9) -0.003(7) 0.009(7) 0.019(8) C27 0.034(9) 0.048(11) 0.080(15) 0.015(10) 0.003(9) -0.010(8) C28 0.063(12) 0.045(11) 0.076(15) -0.004(10) -0.003(10) 0.035(10) C29 0.040(9) 0.023(8) 0.033(10) -0.012(7) 0.010(7) -0.004(7) C30 0.048(10) 0.039(10) 0.057(13) -0.001(9) 0.017(9) -0.001(8) C31 0.034(9) 0.031(9) 0.061(13) -0.006(9) 0.010(8) 0.001(7) C32 0.053(10) 0.076(13) 0.004(9) 0.008(8) -0.008(7) -0.002(9) C33 0.033(10) 0.072(14) 0.106(18) -0.008(13) 0.025(11) 0.012(9) C34 0.048(10) 0.055(12) 0.029(11) 0.000(9) 0.010(8) -0.005(8) C35 0.051(11) 0.053(12) 0.066(14) 0.003(10) 0.035(10) 0.015(9) C36 0.049(11) 0.080(14) 0.026(11) 0.018(9) 0.008(8) 0.004(10) C37 0.039(9) 0.033(9) 0.033(10) 0.000(7) 0.005(7) -0.004(7) C38 0.020(8) 0.037(9) 0.056(12) 0.006(8) 0.003(8) 0.002(7) C39 0.045(10) 0.039(9) 0.027(10) -0.010(8) 0.007(8) 0.005(8) _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 C1 1.879(18) . ? Re1 C2 1.918(17) . ? Re1 C3 1.941(18) . ? Re1 N6 2.183(11) . ? Re1 N4 2.216(11) . ? Re1 N1 2.247(12) . ? Re2 C37 1.860(15) . ? Re2 C39 1.891(17) . ? Re2 C38 1.896(17) . ? Re2 Cl3 2.502(4) . ? Re2 Cl2 2.512(4) . ? Re2 Cl1 2.519(4) . ? Re3 C36 1.851(18) . ? Re3 C34 1.868(18) . ? Re3 C35 1.880(19) . ? Re3 Cl2 2.497(4) . ? Re3 Cl3 2.515(4) . ? Re3 Cl1 2.522(4) . ? P1 N3 1.573(12) . ? P1 N1 1.596(11) . ? P1 N8 1.666(11) . ? P1 N7 1.693(11) . ? P2 N2 1.555(12) . ? P2 N1 1.634(12) . ? P2 N10 1.645(12) . ? P2 N5 1.702(11) . ? P3 N3 1.583(12) . ? P3 N2 1.592(11) . ? P3 N12 1.678(11) . ? P3 N14 1.695(12) . ? O1 C1 1.190(19) . ? O2 C2 1.176(17) . ? O3 C3 1.117(17) . ? O4 C34 1.179(18) . ? O5 C35 1.159(19) . ? O6 C36 1.162(19) . ? O7 C37 1.186(16) . ? O8 C38 1.136(18) . ? O9 C39 1.174(17) . ? N4 C4 1.338(17) . ? N4 N5 1.375(15) . ? N5 C6 1.359(17) . ? N6 C9 1.321(18) . ? N6 N7 1.365(15) . ? N7 C11 1.347(17) . ? N8 N9 1.392(15) . ? N8 C16 1.397(16) . ? N9 C14 1.349(18) . ? N10 C19 1.397(18) . ? N10 N11 1.389(17) . ? N11 C21 1.305(19) . ? N12 C24 1.399(18) . ? N12 N13 1.409(15) . ? N13 C26 1.332(18) . ? N14 N15 1.385(16) . ? N14 C29 1.429(18) . ? N15 C31 1.321(19) . ? C4 C5 1.41(2) . ? C4 C7 1.50(2) . ? C5 C6 1.38(2) . ? C6 C8 1.51(2) . ? C9 C10 1.40(2) . ? C9 C12 1.49(2) . ? C10 C11 1.33(2) . ? C11 C13 1.53(2) . ? C14 C15 1.36(2) . ? C14 C17 1.55(2) . ? C15 C16 1.316(19) . ? C16 C18 1.47(2) . ? C19 C20 1.33(2) . ? C19 C22 1.48(2) . ? C20 C21 1.43(2) . ? C21 C23 1.46(2) . ? C24 C25 1.29(2) . ? C24 C27 1.51(2) . ? C25 C26 1.45(2) . ? C26 C28 1.50(2) . ? C29 C30 1.40(2) . ? C29 C32 1.450(19) . ? C30 C31 1.43(2) . ? C31 C33 1.49(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Re1 C2 85.4(7) . . ? C1 Re1 C3 85.4(7) . . ? C2 Re1 C3 85.6(7) . . ? C1 Re1 N6 97.4(6) . . ? C2 Re1 N6 176.4(6) . . ? C3 Re1 N6 92.4(6) . . ? C1 Re1 N4 100.3(6) . . ? C2 Re1 N4 94.3(6) . . ? C3 Re1 N4 174.3(6) . . ? N6 Re1 N4 87.5(4) . . ? C1 Re1 N1 173.4(6) . . ? C2 Re1 N1 100.8(6) . . ? C3 Re1 N1 97.1(5) . . ? N6 Re1 N1 76.5(4) . . ? N4 Re1 N1 77.3(4) . . ? C37 Re2 C39 89.1(7) . . ? C37 Re2 C38 89.3(6) . . ? C39 Re2 C38 87.9(6) . . ? C37 Re2 Cl3 172.3(5) . . ? C39 Re2 Cl3 97.9(5) . . ? C38 Re2 Cl3 93.8(5) . . ? C37 Re2 Cl2 92.8(5) . . ? C39 Re2 Cl2 174.6(5) . . ? C38 Re2 Cl2 97.1(5) . . ? Cl3 Re2 Cl2 79.90(13) . . ? C37 Re2 Cl1 97.1(5) . . ? C39 Re2 Cl1 95.1(5) . . ? C38 Re2 Cl1 172.9(5) . . ? Cl3 Re2 Cl1 79.44(13) . . ? Cl2 Re2 Cl1 79.68(13) . . ? C36 Re3 C34 84.8(7) . . ? C36 Re3 C35 89.4(7) . . ? C34 Re3 C35 90.5(8) . . ? C36 Re3 Cl2 176.1(5) . . ? C34 Re3 Cl2 98.4(5) . . ? C35 Re3 Cl2 92.9(5) . . ? C36 Re3 Cl3 96.6(6) . . ? C34 Re3 Cl3 172.7(5) . . ? C35 Re3 Cl3 96.6(6) . . ? Cl2 Re3 Cl3 79.95(13) . . ? C36 Re3 Cl1 97.7(5) . . ? C34 Re3 Cl1 93.6(5) . . ? C35 Re3 Cl1 172.1(5) . . ? Cl2 Re3 Cl1 79.92(13) . . ? Cl3 Re3 Cl1 79.16(13) . . ? Re2 Cl1 Re3 84.20(11) . . ? Re3 Cl2 Re2 84.85(12) . . ? Re2 Cl3 Re3 84.70(12) . . ? N3 P1 N1 118.1(6) . . ? N3 P1 N8 111.7(6) . . ? N1 P1 N8 107.6(6) . . ? N3 P1 N7 110.8(6) . . ? N1 P1 N7 104.5(6) . . ? N8 P1 N7 102.8(6) . . ? N2 P2 N1 116.7(6) . . ? N2 P2 N10 107.7(7) . . ? N1 P2 N10 113.0(6) . . ? N2 P2 N5 114.2(6) . . ? N1 P2 N5 101.5(6) . . ? N10 P2 N5 103.0(6) . . ? N3 P3 N2 116.7(6) . . ? N3 P3 N12 110.8(6) . . ? N2 P3 N12 109.4(6) . . ? N3 P3 N14 105.0(6) . . ? N2 P3 N14 110.8(6) . . ? N12 P3 N14 103.1(6) . . ? P1 N1 P2 120.0(7) . . ? P1 N1 Re1 112.3(6) . . ? P2 N1 Re1 115.8(5) . . ? P2 N2 P3 124.0(8) . . ? P1 N3 P3 122.6(7) . . ? C4 N4 N5 106.1(12) . . ? C4 N4 Re1 135.1(11) . . ? N5 N4 Re1 118.6(8) . . ? C6 N5 N4 112.0(12) . . ? C6 N5 P2 127.1(11) . . ? N4 N5 P2 118.9(9) . . ? C9 N6 N7 104.4(11) . . ? C9 N6 Re1 135.8(10) . . ? N7 N6 Re1 119.2(8) . . ? C11 N7 N6 111.3(12) . . ? C11 N7 P1 132.5(11) . . ? N6 N7 P1 116.2(9) . . ? N9 N8 C16 110.3(10) . . ? N9 N8 P1 116.7(9) . . ? C16 N8 P1 132.7(10) . . ? C14 N9 N8 100.5(12) . . ? C19 N10 N11 109.2(12) . . ? C19 N10 P2 133.6(11) . . ? N11 N10 P2 116.5(10) . . ? C21 N11 N10 108.3(14) . . ? C24 N12 N13 110.3(11) . . ? C24 N12 P3 131.0(10) . . ? N13 N12 P3 118.5(9) . . ? C26 N13 N12 104.3(12) . . ? N15 N14 C29 111.2(11) . . ? N15 N14 P3 118.0(10) . . ? C29 N14 P3 128.2(10) . . ? C31 N15 N14 106.0(13) . . ? O1 C1 Re1 176.6(16) . . ? O2 C2 Re1 172.3(15) . . ? O3 C3 Re1 178.7(15) . . ? N4 C4 C5 108.6(14) . . ? N4 C4 C7 123.3(14) . . ? C5 C4 C7 128.0(14) . . ? C6 C5 C4 108.2(14) . . ? N5 C6 C5 104.8(15) . . ? N5 C6 C8 124.3(14) . . ? C5 C6 C8 130.7(13) . . ? N6 C9 C10 110.6(13) . . ? N6 C9 C12 123.1(14) . . ? C10 C9 C12 126.2(15) . . ? C11 C10 C9 106.2(14) . . ? C10 C11 N7 107.4(14) . . ? C10 C11 C13 128.7(15) . . ? N7 C11 C13 123.8(14) . . ? N9 C14 C15 115.7(14) . . ? N9 C14 C17 115.1(14) . . ? C15 C14 C17 129.2(15) . . ? C16 C15 C14 105.2(13) . . ? C15 C16 N8 108.2(13) . . ? C15 C16 C18 132.1(14) . . ? N8 C16 C18 119.7(13) . . ? C20 C19 N10 105.2(15) . . ? C20 C19 C22 131.1(16) . . ? N10 C19 C22 123.6(14) . . ? C19 C20 C21 109.7(15) . . ? N11 C21 C20 107.3(16) . . ? N11 C21 C23 122.6(17) . . ? C20 C21 C23 130.0(17) . . ? C25 C24 N12 107.0(14) . . ? C25 C24 C27 129.5(16) . . ? N12 C24 C27 123.4(13) . . ? C24 C25 C26 108.6(15) . . ? N13 C26 C25 109.5(13) . . ? N13 C26 C28 119.1(16) . . ? C25 C26 C28 131.5(16) . . ? C30 C29 N14 104.4(13) . . ? C30 C29 C32 130.4(15) . . ? N14 C29 C32 125.1(13) . . ? C29 C30 C31 106.4(15) . . ? N15 C31 C30 111.9(14) . . ? N15 C31 C33 120.0(16) . . ? C30 C31 C33 128.0(16) . . ? O4 C34 Re3 177.6(15) . . ? O5 C35 Re3 175.6(15) . . ? O6 C36 Re3 177.1(18) . . ? O7 C37 Re2 175.3(13) . . ? O8 C38 Re2 179.0(15) . . ? O9 C39 Re2 177.8(15) . . ? _refine_diff_density_max 0.976 _refine_diff_density_min -1.025 _refine_diff_density_rms 0.213 #===END data_2a _database_code_CSD 183234 _audit_creation_method SHELXL-97 _chemical_name_common 'Compound 2a' _chemical_formula_sum 'C17 H26 F6 N11 O3 P3 Re Sb' _chemical_formula_weight 947.35 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' 'F' 'F' 0.0171 0.0103 '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' 'Sb' 'Sb' -0.5866 1.5461 '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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.838(3) _cell_length_b 13.475(5) _cell_length_c 13.819(5) _cell_angle_alpha 97.523(5) _cell_angle_beta 108.543(5) _cell_angle_gamma 91.604(6) _cell_volume 1542.8(9) _cell_formula_units_Z 2 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description slab _exptl_crystal_colour colorless _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.29 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.039 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 908 _exptl_absorpt_coefficient_mu 5.028 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5715 _exptl_absorpt_correction_T_max 0.9280 _exptl_absorpt_process_details 'DIFABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4/CCD' _diffrn_measurement_method '\f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7230 _diffrn_reflns_av_R_equivalents 0.0253 _diffrn_reflns_av_sigmaI/netI 0.0359 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 23.23 _reflns_number_total 4123 _reflns_number_gt 3614 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0612P)^2^+3.7978P] 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 4123 _refine_ls_number_parameters 379 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0495 _refine_ls_R_factor_gt 0.0418 _refine_ls_wR_factor_ref 0.1035 _refine_ls_wR_factor_gt 0.1007 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_restrained_S_all 1.085 _refine_ls_shift/su_max 0.000 _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 0.31688(4) 0.43230(2) 0.66217(3) 0.03192(15) Uani 1 1 d . . . Sb1 Sb -0.05721(8) 0.71889(4) 0.88727(5) 0.03933(19) Uani 1 1 d . . . P1 P 0.4316(3) 0.27055(15) 0.79851(16) 0.0267(5) Uani 1 1 d . . . P2 P 0.2251(3) 0.16581(16) 0.61114(18) 0.0342(6) Uani 1 1 d . . . P3 P 0.3950(3) 0.06568(15) 0.78527(18) 0.0310(5) Uani 1 1 d . . . F1 F -0.0282(10) 0.6564(6) 0.7654(5) 0.089(2) Uani 1 1 d . . . F2 F -0.1009(9) 0.8369(5) 0.8313(7) 0.091(2) Uani 1 1 d . . . F3 F -0.0805(9) 0.7774(5) 1.0107(5) 0.078(2) Uani 1 1 d . . . F4 F -0.0108(7) 0.6007(4) 0.9429(5) 0.0541(15) Uani 1 1 d . . . F5 F -0.2748(6) 0.6777(4) 0.8363(5) 0.0578(16) Uani 1 1 d . . . F6 F 0.1613(7) 0.7588(6) 0.9421(6) 0.081(2) Uani 1 1 d . . . O1 O 0.3574(10) 0.6583(5) 0.6608(7) 0.074(2) Uani 1 1 d . . . O2 O -0.0468(9) 0.4412(6) 0.5797(6) 0.061(2) Uani 1 1 d . . . O3 O 0.3384(11) 0.4002(6) 0.4433(6) 0.069(2) Uani 1 1 d . . . N1 N 0.3078(9) 0.2719(5) 0.6879(5) 0.0342(18) Uani 1 1 d . . . N2 N 0.2788(9) 0.0749(5) 0.6723(6) 0.0378(18) Uani 1 1 d . . . N3 N 0.4691(8) 0.1761(5) 0.8515(5) 0.0294(16) Uani 1 1 d . . . N5 N 0.3721(8) 0.3624(5) 0.8724(5) 0.0290(16) Uani 1 1 d . . . N4 N 0.3202(9) 0.4440(5) 0.8236(6) 0.0354(18) Uani 1 1 d . . . N7 N 0.6007(8) 0.3304(5) 0.7913(5) 0.0291(16) Uani 1 1 d . . . N6 N 0.5704(8) 0.4079(5) 0.7321(5) 0.0294(16) Uani 1 1 d . . . N8 N 0.0334(11) 0.1688(7) 0.5608(7) 0.057(2) Uani 1 1 d . . . N9 N 0.2609(12) 0.1618(6) 0.5021(6) 0.053(2) Uani 1 1 d . . . N10 N 0.3147(10) 0.0035(5) 0.8513(6) 0.0396(19) Uani 1 1 d . . . N11 N 0.5369(10) -0.0104(5) 0.7834(6) 0.0400(19) Uani 1 1 d . . . C1 C 0.3442(13) 0.5738(8) 0.6606(8) 0.053(3) Uani 1 1 d . . . C2 C 0.0906(12) 0.4395(7) 0.6107(7) 0.040(2) Uani 1 1 d . . . C3 C 0.3281(12) 0.4118(7) 0.5244(9) 0.049(3) Uani 1 1 d . . . C4 C 0.2750(10) 0.5052(6) 0.8900(7) 0.037(2) Uani 1 1 d . . . H4A H 0.2348 0.5671 0.8777 0.044 Uiso 1 1 calc R . . C5 C 0.2950(11) 0.4657(6) 0.9807(7) 0.037(2) Uani 1 1 d . . . H5A H 0.2707 0.4945 1.0385 0.045 Uiso 1 1 calc R . . C6 C 0.3578(10) 0.3758(6) 0.9671(7) 0.034(2) Uani 1 1 d . . . H6A H 0.3859 0.3314 1.0150 0.040 Uiso 1 1 calc R . . C7 C 0.7140(11) 0.4445(6) 0.7365(7) 0.034(2) Uani 1 1 d . . . H7A H 0.7326 0.4973 0.7036 0.041 Uiso 1 1 calc R . . C8 C 0.8322(11) 0.3924(6) 0.7972(7) 0.039(2) Uani 1 1 d . . . H8A H 0.9419 0.4042 0.8118 0.046 Uiso 1 1 calc R . . C9 C 0.7602(10) 0.3222(6) 0.8309(6) 0.032(2) Uani 1 1 d . . . H9A H 0.8101 0.2765 0.8735 0.038 Uiso 1 1 calc R . . C10 C -0.0221(17) 0.1710(10) 0.4504(10) 0.081(4) Uani 1 1 d . . . H10A H -0.0594 0.2361 0.4358 0.098 Uiso 1 1 calc R . . H10B H -0.1091 0.1201 0.4158 0.098 Uiso 1 1 calc R . . C11 C 0.121(2) 0.1503(13) 0.4148(10) 0.104(6) Uani 1 1 d . . . H11A H 0.1076 0.0826 0.3779 0.125 Uiso 1 1 calc R . . H11B H 0.1291 0.1967 0.3684 0.125 Uiso 1 1 calc R . . C12 C -0.0760(15) 0.1782(10) 0.6175(12) 0.085(4) Uani 1 1 d . . . H12A H -0.1824 0.1802 0.5709 0.128 Uiso 1 1 calc R . . H12B H -0.0475 0.2391 0.6660 0.128 Uiso 1 1 calc R . . H12C H -0.0718 0.1219 0.6540 0.128 Uiso 1 1 calc R . . C13 C 0.4186(17) 0.1538(9) 0.4934(10) 0.075(4) Uani 1 1 d . . . H13A H 0.4133 0.1559 0.4233 0.112 Uiso 1 1 calc R . . H13B H 0.4584 0.0915 0.5137 0.112 Uiso 1 1 calc R . . H13C H 0.4890 0.2087 0.5376 0.112 Uiso 1 1 calc R . . C14 C 0.3756(14) -0.0990(7) 0.8584(9) 0.055(3) Uani 1 1 d . . . H14A H 0.3095 -0.1476 0.8014 0.065 Uiso 1 1 calc R . . H14B H 0.3770 -0.1209 0.9228 0.065 Uiso 1 1 calc R . . C15 C 0.5432(14) -0.0865(7) 0.8534(9) 0.055(3) Uani 1 1 d . . . H15A H 0.6189 -0.0633 0.9214 0.066 Uiso 1 1 calc R . . H15B H 0.5749 -0.1496 0.8261 0.066 Uiso 1 1 calc R . . C16 C 0.1533(13) 0.0168(7) 0.8540(8) 0.052(3) Uani 1 1 d . . . H16A H 0.1278 -0.0284 0.8958 0.078 Uiso 1 1 calc R . . H16B H 0.0788 0.0028 0.7851 0.078 Uiso 1 1 calc R . . H16C H 0.1468 0.0847 0.8828 0.078 Uiso 1 1 calc R . . C17 C 0.6891(14) 0.0287(8) 0.7783(10) 0.066(3) Uani 1 1 d . . . H17A H 0.7580 -0.0251 0.7778 0.098 Uiso 1 1 calc R . . H17B H 0.7388 0.0785 0.8373 0.098 Uiso 1 1 calc R . . H17C H 0.6709 0.0584 0.7165 0.098 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.0345(2) 0.0269(2) 0.0363(2) 0.00977(14) 0.01154(17) 0.00911(14) Sb1 0.0377(4) 0.0384(4) 0.0469(4) 0.0150(3) 0.0170(3) 0.0070(3) P1 0.0287(12) 0.0228(10) 0.0294(12) 0.0043(9) 0.0103(10) 0.0033(9) P2 0.0366(14) 0.0287(12) 0.0317(13) -0.0012(10) 0.0055(11) 0.0041(10) P3 0.0356(13) 0.0225(11) 0.0373(13) 0.0047(9) 0.0151(11) 0.0044(9) F1 0.093(6) 0.130(7) 0.056(4) 0.013(4) 0.041(4) 0.035(5) F2 0.093(6) 0.058(4) 0.129(7) 0.057(4) 0.030(5) 0.011(4) F3 0.095(5) 0.063(4) 0.076(5) -0.016(3) 0.039(4) 0.006(4) F4 0.054(4) 0.040(3) 0.074(4) 0.021(3) 0.023(3) 0.019(3) F5 0.032(3) 0.067(4) 0.075(4) 0.020(3) 0.014(3) 0.010(3) F6 0.044(4) 0.102(5) 0.099(5) 0.051(4) 0.013(4) -0.018(4) O1 0.085(6) 0.031(4) 0.103(7) 0.027(4) 0.022(5) 0.011(4) O2 0.038(5) 0.075(5) 0.072(5) 0.041(4) 0.010(4) 0.014(4) O3 0.096(7) 0.082(6) 0.040(5) 0.020(4) 0.029(4) 0.029(5) N1 0.045(5) 0.021(4) 0.033(4) 0.006(3) 0.008(4) 0.000(3) N2 0.047(5) 0.028(4) 0.033(4) -0.005(3) 0.008(4) 0.002(3) N3 0.032(4) 0.028(4) 0.032(4) 0.010(3) 0.014(3) 0.004(3) N5 0.032(4) 0.025(4) 0.036(4) 0.005(3) 0.019(3) 0.002(3) N4 0.038(5) 0.029(4) 0.040(4) 0.005(3) 0.014(4) 0.010(3) N7 0.030(4) 0.028(4) 0.029(4) 0.005(3) 0.008(3) 0.008(3) N6 0.032(4) 0.027(4) 0.034(4) 0.008(3) 0.016(3) 0.006(3) N8 0.039(5) 0.065(6) 0.051(6) 0.004(4) -0.006(5) 0.003(4) N9 0.073(7) 0.058(5) 0.029(4) 0.001(4) 0.016(4) 0.019(5) N10 0.053(5) 0.025(4) 0.047(5) 0.007(3) 0.023(4) 0.003(3) N11 0.049(5) 0.027(4) 0.054(5) 0.016(3) 0.025(4) 0.016(3) C1 0.060(7) 0.035(6) 0.061(7) 0.021(5) 0.010(6) 0.015(5) C2 0.039(6) 0.045(5) 0.044(6) 0.026(4) 0.017(5) 0.015(4) C3 0.044(6) 0.045(6) 0.057(7) 0.014(5) 0.013(5) 0.013(5) C4 0.031(5) 0.027(5) 0.059(6) -0.004(4) 0.027(5) 0.005(4) C5 0.030(5) 0.041(5) 0.046(6) -0.009(4) 0.027(5) -0.008(4) C6 0.031(5) 0.040(5) 0.035(5) 0.003(4) 0.020(4) -0.004(4) C7 0.037(6) 0.029(5) 0.040(5) 0.005(4) 0.018(5) 0.002(4) C8 0.028(5) 0.036(5) 0.056(6) 0.004(4) 0.019(5) 0.001(4) C9 0.032(5) 0.032(5) 0.029(5) 0.004(4) 0.006(4) 0.011(4) C10 0.076(10) 0.062(8) 0.078(9) -0.003(7) -0.012(8) 0.014(7) C11 0.128(15) 0.121(13) 0.035(7) -0.007(7) -0.008(8) 0.022(11) C12 0.048(8) 0.079(9) 0.123(12) 0.023(8) 0.017(9) 0.006(6) C13 0.111(12) 0.069(8) 0.070(8) 0.018(6) 0.061(8) 0.032(7) C14 0.077(8) 0.030(5) 0.069(7) 0.018(5) 0.036(6) 0.011(5) C15 0.077(8) 0.032(5) 0.065(7) 0.017(5) 0.032(6) 0.022(5) C16 0.054(7) 0.045(6) 0.062(7) 0.004(5) 0.026(6) -0.002(5) C17 0.069(8) 0.060(7) 0.100(10) 0.030(7) 0.061(8) 0.034(6) _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 C2 1.908(10) . ? Re1 C1 1.919(10) . ? Re1 C3 1.922(12) . ? Re1 N6 2.193(7) . ? Re1 N4 2.206(7) . ? Re1 N1 2.239(6) . ? Sb1 F2 1.856(6) . ? Sb1 F4 1.858(5) . ? Sb1 F3 1.858(6) . ? Sb1 F5 1.866(6) . ? Sb1 F6 1.870(6) . ? Sb1 F1 1.878(6) . ? P1 N3 1.542(7) . ? P1 N1 1.574(7) . ? P1 N5 1.703(7) . ? P1 N7 1.715(7) . ? P2 N2 1.578(8) . ? P2 N8 1.618(9) . ? P2 N9 1.630(9) . ? P2 N1 1.660(7) . ? P3 N2 1.596(8) . ? P3 N10 1.618(8) . ? P3 N3 1.640(7) . ? P3 N11 1.647(7) . ? O1 C1 1.140(11) . ? O2 C2 1.153(11) . ? O3 C3 1.144(12) . ? N5 C6 1.344(11) . ? N5 N4 1.378(9) . ? N4 C4 1.318(11) . ? N7 C9 1.353(11) . ? N7 N6 1.390(9) . ? N6 C7 1.328(11) . ? N8 C12 1.424(17) . ? N8 C10 1.451(16) . ? N9 C11 1.416(15) . ? N9 C13 1.442(15) . ? N10 C16 1.454(13) . ? N10 C14 1.500(11) . ? N11 C17 1.457(13) . ? N11 C15 1.490(12) . ? C4 C5 1.388(14) . ? C5 C6 1.362(12) . ? C7 C8 1.388(12) . ? C8 C9 1.338(12) . ? C10 C11 1.51(2) . ? C14 C15 1.510(15) . ? 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 C2 Re1 C1 89.4(4) . . ? C2 Re1 C3 91.2(4) . . ? C1 Re1 C3 87.6(4) . . ? C2 Re1 N6 172.3(3) . . ? C1 Re1 N6 97.2(4) . . ? C3 Re1 N6 93.1(4) . . ? C2 Re1 N4 92.9(3) . . ? C1 Re1 N4 96.4(4) . . ? C3 Re1 N4 174.3(3) . . ? N6 Re1 N4 82.4(3) . . ? C2 Re1 N1 95.6(3) . . ? C1 Re1 N1 171.7(4) . . ? C3 Re1 N1 98.9(3) . . ? N6 Re1 N1 77.4(3) . . ? N4 Re1 N1 76.8(3) . . ? F2 Sb1 F4 179.2(3) . . ? F2 Sb1 F3 91.4(4) . . ? F4 Sb1 F3 89.1(3) . . ? F2 Sb1 F5 89.7(3) . . ? F4 Sb1 F5 90.9(3) . . ? F3 Sb1 F5 90.2(3) . . ? F2 Sb1 F6 91.5(3) . . ? F4 Sb1 F6 87.8(3) . . ? F3 Sb1 F6 88.7(3) . . ? F5 Sb1 F6 178.3(3) . . ? F2 Sb1 F1 90.6(4) . . ? F4 Sb1 F1 89.0(3) . . ? F3 Sb1 F1 177.8(3) . . ? F5 Sb1 F1 90.9(3) . . ? F6 Sb1 F1 90.3(4) . . ? N3 P1 N1 124.8(4) . . ? N3 P1 N5 111.6(4) . . ? N1 P1 N5 102.5(4) . . ? N3 P1 N7 112.0(4) . . ? N1 P1 N7 102.7(4) . . ? N5 P1 N7 100.3(3) . . ? N2 P2 N8 114.4(5) . . ? N2 P2 N9 116.3(4) . . ? N8 P2 N9 95.0(5) . . ? N2 P2 N1 108.9(4) . . ? N8 P2 N1 111.7(4) . . ? N9 P2 N1 110.0(4) . . ? N2 P3 N10 114.3(4) . . ? N2 P3 N3 111.6(4) . . ? N10 P3 N3 109.7(4) . . ? N2 P3 N11 112.4(4) . . ? N10 P3 N11 96.4(4) . . ? N3 P3 N11 111.6(4) . . ? P1 N1 P2 120.9(4) . . ? P1 N1 Re1 105.0(3) . . ? P2 N1 Re1 133.2(4) . . ? P2 N2 P3 134.0(4) . . ? P1 N3 P3 119.2(4) . . ? C6 N5 N4 109.9(7) . . ? C6 N5 P1 136.4(6) . . ? N4 N5 P1 113.7(5) . . ? C4 N4 N5 105.4(7) . . ? C4 N4 Re1 138.6(6) . . ? N5 N4 Re1 115.8(5) . . ? C9 N7 N6 110.4(7) . . ? C9 N7 P1 135.7(6) . . ? N6 N7 P1 113.9(5) . . ? C7 N6 N7 104.8(7) . . ? C7 N6 Re1 139.9(6) . . ? N7 N6 Re1 115.3(5) . . ? C12 N8 C10 120.2(10) . . ? C12 N8 P2 125.0(8) . . ? C10 N8 P2 114.5(9) . . ? C11 N9 C13 122.5(11) . . ? C11 N9 P2 113.6(10) . . ? C13 N9 P2 123.2(8) . . ? C16 N10 C14 118.1(8) . . ? C16 N10 P3 122.7(6) . . ? C14 N10 P3 111.6(6) . . ? C17 N11 C15 117.0(8) . . ? C17 N11 P3 120.0(6) . . ? C15 N11 P3 110.9(6) . . ? O1 C1 Re1 178.2(11) . . ? O2 C2 Re1 178.2(8) . . ? O3 C3 Re1 178.5(10) . . ? N4 C4 C5 111.4(8) . . ? C6 C5 C4 105.2(8) . . ? N5 C6 C5 108.1(8) . . ? N6 C7 C8 110.1(8) . . ? C9 C8 C7 107.8(8) . . ? C8 C9 N7 106.9(8) . . ? N8 C10 C11 105.9(10) . . ? N9 C11 C10 108.9(11) . . ? N10 C14 C15 104.4(8) . . ? N11 C15 C14 105.5(8) . . ? _diffrn_measured_fraction_theta_max 0.933 _diffrn_reflns_theta_full 23.23 _diffrn_measured_fraction_theta_full 0.933 _refine_diff_density_max 1.778 _refine_diff_density_min -1.699 _refine_diff_density_rms 0.146