Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Julio Perez' _publ_contact_author_address ; Quimica Organica e Inorganica Universidad de Oviedo Julian Claveria, 8 Oviedo 33006 SPAIN ; _publ_contact_author_email JAPM@UNIOVI.ES _publ_section_title ; Second-sphere interaction of anions with a weakly binding metal complex host: probing the effect of counteranions ; loop_ _publ_author_name 'Julio Perez' 'Kirsty Anderson' 'Laura Ion' 'Daniel Miguel' 'Lucia Riera' 'Victor Riera' 'Jonathan Steed' data_Compound_1_(li418) _database_code_depnum_ccdc_archive 'CCDC 642013' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H18 N6 O3 Re, C F3 O3 S' _chemical_formula_sum 'C16 H18 F3 N6 O6 Re S' _chemical_formula_weight 665.62 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' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' _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 7.0294(8) _cell_length_b 12.1099(14) _cell_length_c 13.4786(16) _cell_angle_alpha 95.450(2) _cell_angle_beta 98.829(2) _cell_angle_gamma 90.805(2) _cell_volume 1128.2(2) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.959 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 644 _exptl_absorpt_coefficient_mu 5.548 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.560656 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABs _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 'SMART 1k' _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 15709 _diffrn_reflns_av_R_equivalents 0.0337 _diffrn_reflns_av_sigmaI/netI 0.0421 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 29.17 _reflns_number_total 6034 _reflns_number_gt 5375 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics X-Seed _computing_publication_material X-Seed _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^)+(0.0201P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6034 _refine_ls_number_parameters 301 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0307 _refine_ls_R_factor_gt 0.0234 _refine_ls_wR_factor_ref 0.0484 _refine_ls_wR_factor_gt 0.0467 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _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 0.437711(16) 0.230999(9) 0.135342(8) 0.01230(4) Uani 1 1 d . . . S1 S 0.30873(11) 0.27794(6) 0.62559(6) 0.01924(15) Uani 1 1 d . . . F1 F 0.6531(3) 0.2513(2) 0.72314(18) 0.0471(6) Uani 1 1 d . . . F2 F 0.4349(4) 0.2726(3) 0.81818(16) 0.0584(7) Uani 1 1 d . . . F3 F 0.4513(4) 0.1176(2) 0.7281(2) 0.0580(7) Uani 1 1 d . . . O1 O 0.7010(3) 0.0528(2) 0.05859(18) 0.0308(6) Uani 1 1 d . . . O2 O 0.6634(3) 0.3928(2) 0.03247(18) 0.0298(5) Uani 1 1 d . . . O3 O 0.1509(3) 0.17847(18) -0.05930(17) 0.0272(5) Uani 1 1 d . . . O4 O 0.3844(4) 0.2317(2) 0.53795(18) 0.0384(6) Uani 1 1 d . . . O5 O 0.3310(4) 0.39573(19) 0.6453(2) 0.0340(6) Uani 1 1 d . . . O6 O 0.1236(3) 0.2333(2) 0.63735(18) 0.0326(6) Uani 1 1 d . . . N1 N 0.2477(3) 0.3599(2) 0.18733(18) 0.0147(5) Uani 1 1 d . . . N2 N 0.0721(4) 0.5088(2) 0.18010(19) 0.0184(5) Uani 1 1 d . . . N3 N 0.2856(3) 0.1162(2) 0.21591(18) 0.0159(5) Uani 1 1 d . . . N4 N 0.2033(3) 0.0185(2) 0.33301(18) 0.0157(5) Uani 1 1 d . . . N5 N 0.6176(3) 0.2656(2) 0.28239(18) 0.0154(5) Uani 1 1 d . . . N6 N 0.7395(4) 0.3406(2) 0.43378(18) 0.0186(5) Uani 1 1 d . . . C1 C 0.6011(4) 0.1185(3) 0.0894(2) 0.0204(6) Uani 1 1 d . . . C2 C 0.5771(4) 0.3324(3) 0.0715(2) 0.0183(6) Uani 1 1 d . . . C3 C 0.2603(4) 0.1982(2) 0.0131(2) 0.0169(6) Uani 1 1 d . . . C11 C 0.2156(4) 0.4537(2) 0.1441(2) 0.0194(6) Uani 1 1 d . . . H11 H 0.2848 0.4784 0.0947 0.023 Uiso 1 1 calc R . . C12 C 0.1188(4) 0.3566(3) 0.2539(2) 0.0218(6) Uani 1 1 d . . . H12 H 0.1078 0.2993 0.2963 0.026 Uiso 1 1 calc R . . C13 C 0.0091(4) 0.4483(3) 0.2497(2) 0.0215(6) Uani 1 1 d . . . H13 H -0.0914 0.4665 0.2876 0.026 Uiso 1 1 calc R . . C14 C -0.0093(5) 0.6115(3) 0.1463(3) 0.0275(7) Uani 1 1 d . . . H14A H 0.0673 0.6399 0.0988 0.041 Uiso 1 1 calc R . . H14B H -0.0076 0.6666 0.2046 0.041 Uiso 1 1 calc R . . H14C H -0.1423 0.5968 0.1127 0.041 Uiso 1 1 calc R . . C21 C 0.3135(4) 0.1028(2) 0.3131(2) 0.0168(6) Uani 1 1 d . . . H21 H 0.4004 0.1470 0.3626 0.020 Uiso 1 1 calc R . . C22 C 0.1507(4) 0.0347(2) 0.1711(2) 0.0191(6) Uani 1 1 d . . . H22 H 0.1015 0.0232 0.1012 0.023 Uiso 1 1 calc R . . C23 C 0.1001(4) -0.0258(2) 0.2430(2) 0.0187(6) Uani 1 1 d . . . H23 H 0.0107 -0.0869 0.2330 0.022 Uiso 1 1 calc R . . C24 C 0.2111(5) -0.0254(3) 0.4307(2) 0.0242(7) Uani 1 1 d . . . H24A H 0.3096 -0.0818 0.4375 0.036 Uiso 1 1 calc R . . H24B H 0.0854 -0.0588 0.4354 0.036 Uiso 1 1 calc R . . H24C H 0.2434 0.0350 0.4847 0.036 Uiso 1 1 calc R . . C31 C 0.6105(4) 0.3505(2) 0.3512(2) 0.0168(6) Uani 1 1 d . . . H31 H 0.5253 0.4103 0.3431 0.020 Uiso 1 1 calc R . . C32 C 0.7588(4) 0.1973(2) 0.3242(2) 0.0188(6) Uani 1 1 d . . . H32 H 0.7966 0.1295 0.2924 0.023 Uiso 1 1 calc R . . C33 C 0.8344(4) 0.2437(3) 0.4184(2) 0.0202(6) Uani 1 1 d . . . H33 H 0.9330 0.2147 0.4643 0.024 Uiso 1 1 calc R . . C34 C 0.7674(5) 0.4171(3) 0.5262(2) 0.0274(7) Uani 1 1 d . . . H34A H 0.7555 0.4936 0.5086 0.041 Uiso 1 1 calc R . . H34B H 0.8958 0.4078 0.5641 0.041 Uiso 1 1 calc R . . H34C H 0.6695 0.4008 0.5677 0.041 Uiso 1 1 calc R . . C41 C 0.4697(5) 0.2269(3) 0.7293(3) 0.0311(8) 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 0.01548(6) 0.01114(6) 0.01064(5) 0.00174(4) 0.00272(4) 0.00099(4) S1 0.0204(4) 0.0192(4) 0.0175(4) 0.0009(3) 0.0018(3) -0.0012(3) F1 0.0179(10) 0.0693(17) 0.0548(15) 0.0146(13) 0.0021(10) 0.0057(10) F2 0.0490(15) 0.105(2) 0.0203(11) 0.0086(13) 0.0010(10) 0.0132(14) F3 0.0478(15) 0.0456(15) 0.089(2) 0.0403(14) 0.0159(14) 0.0181(12) O1 0.0272(13) 0.0299(13) 0.0334(13) -0.0076(11) 0.0038(10) 0.0121(10) O2 0.0365(14) 0.0295(13) 0.0268(13) 0.0083(10) 0.0131(11) -0.0074(11) O3 0.0365(13) 0.0212(12) 0.0206(12) 0.0016(9) -0.0059(10) 0.0034(10) O4 0.0483(16) 0.0439(16) 0.0225(13) -0.0070(11) 0.0111(12) -0.0051(13) O5 0.0394(15) 0.0181(12) 0.0459(16) 0.0041(11) 0.0103(12) 0.0032(10) O6 0.0206(12) 0.0422(15) 0.0335(14) 0.0064(11) -0.0014(10) -0.0076(11) N1 0.0139(11) 0.0153(12) 0.0151(12) 0.0015(9) 0.0034(9) -0.0004(9) N2 0.0203(13) 0.0164(12) 0.0193(12) 0.0018(10) 0.0054(10) 0.0041(10) N3 0.0170(12) 0.0156(12) 0.0152(12) 0.0021(9) 0.0026(9) -0.0007(9) N4 0.0167(12) 0.0159(12) 0.0158(12) 0.0048(9) 0.0051(9) -0.0010(9) N5 0.0160(12) 0.0166(12) 0.0140(12) 0.0039(9) 0.0027(9) -0.0031(9) N6 0.0210(13) 0.0204(13) 0.0142(12) 0.0017(10) 0.0025(10) -0.0043(10) C1 0.0200(15) 0.0206(15) 0.0193(15) 0.0000(12) -0.0001(12) -0.0014(12) C2 0.0201(15) 0.0208(15) 0.0144(14) -0.0010(12) 0.0052(11) 0.0002(12) C3 0.0218(15) 0.0141(14) 0.0162(14) 0.0037(11) 0.0059(12) 0.0035(11) C11 0.0249(16) 0.0153(14) 0.0207(15) 0.0042(12) 0.0099(12) 0.0050(12) C12 0.0228(16) 0.0212(16) 0.0248(16) 0.0076(13) 0.0107(13) 0.0003(12) C13 0.0191(15) 0.0247(16) 0.0223(15) 0.0024(13) 0.0075(12) 0.0006(12) C14 0.0319(18) 0.0206(16) 0.0321(18) 0.0071(14) 0.0078(15) 0.0124(14) C21 0.0180(14) 0.0155(14) 0.0163(14) 0.0013(11) 0.0014(11) -0.0028(11) C22 0.0207(15) 0.0179(15) 0.0170(14) -0.0018(11) -0.0002(12) -0.0024(12) C23 0.0178(15) 0.0180(15) 0.0199(15) 0.0026(12) 0.0014(11) -0.0045(11) C24 0.0319(18) 0.0240(17) 0.0187(15) 0.0078(13) 0.0075(13) -0.0068(13) C31 0.0143(14) 0.0182(14) 0.0177(14) 0.0020(11) 0.0020(11) -0.0020(11) C32 0.0205(15) 0.0169(15) 0.0191(15) 0.0044(12) 0.0020(12) 0.0026(12) C33 0.0166(14) 0.0249(16) 0.0196(15) 0.0071(12) 0.0012(12) -0.0007(12) C34 0.0329(19) 0.0336(19) 0.0131(14) -0.0039(13) -0.0007(13) -0.0046(15) C41 0.0193(16) 0.043(2) 0.0318(19) 0.0109(16) 0.0027(14) 0.0062(15) _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 1.906(3) . ? Re1 C3 1.912(3) . ? Re1 C1 1.914(3) . ? Re1 N5 2.182(2) . ? Re1 N1 2.202(2) . ? Re1 N3 2.204(2) . ? S1 O5 1.428(2) . ? S1 O4 1.438(2) . ? S1 O6 1.439(2) . ? S1 C41 1.821(4) . ? F1 C41 1.335(4) . ? F2 C41 1.330(4) . ? F3 C41 1.326(4) . ? O1 C1 1.158(4) . ? O2 C2 1.157(4) . ? O3 C3 1.150(4) . ? N1 C11 1.332(4) . ? N1 C12 1.372(4) . ? N2 C11 1.344(4) . ? N2 C13 1.364(4) . ? N2 C14 1.458(4) . ? N3 C21 1.320(4) . ? N3 C22 1.386(4) . ? N4 C21 1.344(4) . ? N4 C23 1.372(4) . ? N4 C24 1.460(4) . ? N5 C31 1.324(4) . ? N5 C32 1.388(4) . ? N6 C31 1.339(4) . ? N6 C33 1.373(4) . ? N6 C34 1.466(4) . ? C12 C13 1.362(4) . ? C22 C23 1.355(4) . ? C32 C33 1.364(4) . ? 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 C3 90.34(12) . . ? C2 Re1 C1 87.01(13) . . ? C3 Re1 C1 89.26(12) . . ? C2 Re1 N5 94.24(11) . . ? C3 Re1 N5 174.61(10) . . ? C1 Re1 N5 93.80(11) . . ? C2 Re1 N1 93.14(11) . . ? C3 Re1 N1 90.30(10) . . ? C1 Re1 N1 179.54(11) . . ? N5 Re1 N1 86.63(9) . . ? C2 Re1 N3 177.31(11) . . ? C3 Re1 N3 92.34(11) . . ? C1 Re1 N3 93.24(11) . . ? N5 Re1 N3 83.07(9) . . ? N1 Re1 N3 86.63(9) . . ? O5 S1 O4 114.72(16) . . ? O5 S1 O6 114.87(15) . . ? O4 S1 O6 115.27(15) . . ? O5 S1 C41 103.53(17) . . ? O4 S1 C41 103.11(16) . . ? O6 S1 C41 102.93(15) . . ? C11 N1 C12 105.8(2) . . ? C11 N1 Re1 123.26(19) . . ? C12 N1 Re1 130.1(2) . . ? C11 N2 C13 107.8(2) . . ? C11 N2 C14 126.0(3) . . ? C13 N2 C14 126.1(3) . . ? C21 N3 C22 105.7(2) . . ? C21 N3 Re1 128.50(19) . . ? C22 N3 Re1 125.59(19) . . ? C21 N4 C23 107.3(2) . . ? C21 N4 C24 125.7(3) . . ? C23 N4 C24 126.6(2) . . ? C31 N5 C32 106.1(2) . . ? C31 N5 Re1 128.4(2) . . ? C32 N5 Re1 125.44(19) . . ? C31 N6 C33 108.0(2) . . ? C31 N6 C34 126.0(3) . . ? C33 N6 C34 126.0(3) . . ? O1 C1 Re1 177.4(3) . . ? O2 C2 Re1 179.1(3) . . ? O3 C3 Re1 178.7(3) . . ? N1 C11 N2 110.7(3) . . ? C13 C12 N1 109.4(3) . . ? C12 C13 N2 106.3(3) . . ? N3 C21 N4 111.3(3) . . ? C23 C22 N3 109.2(3) . . ? C22 C23 N4 106.5(3) . . ? N5 C31 N6 110.9(3) . . ? C33 C32 N5 108.7(3) . . ? C32 C33 N6 106.3(3) . . ? F3 C41 F2 108.2(3) . . ? F3 C41 F1 107.8(3) . . ? F2 C41 F1 107.3(3) . . ? F3 C41 S1 111.2(3) . . ? F2 C41 S1 111.5(2) . . ? F1 C41 S1 110.7(2) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 29.17 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.873 _refine_diff_density_min -0.939 _refine_diff_density_rms 0.125 #===END data_Compound_2_(li453) _database_code_depnum_ccdc_archive 'CCDC 642014' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H18 N6 O3 Re, F6 P' _chemical_formula_sum 'C15 H18 F6 N6 O3 P Re' _chemical_formula_weight 661.52 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' 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' 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 P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 8.336(5) _cell_length_b 13.146(8) _cell_length_c 10.254(6) _cell_angle_alpha 90.00 _cell_angle_beta 96.923(11) _cell_angle_gamma 90.00 _cell_volume 1115.6(12) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description BLOCK _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.969 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 636 _exptl_absorpt_coefficient_mu 5.597 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.635814 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5003 _diffrn_reflns_av_R_equivalents 0.0202 _diffrn_reflns_av_sigmaI/netI 0.0248 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 23.30 _reflns_number_total 2999 _reflns_number_gt 2857 _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^)+(0.0404P)^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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0021(3) _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 0.022(10) _refine_ls_number_reflns 2999 _refine_ls_number_parameters 293 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0239 _refine_ls_R_factor_gt 0.0223 _refine_ls_wR_factor_ref 0.0547 _refine_ls_wR_factor_gt 0.0541 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _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 1.13951(2) 0.25750(3) 0.388955(19) 0.03658(11) Uani 1 1 d . . . C1 C 1.3434(10) 0.3205(6) 0.3850(9) 0.059(2) Uani 1 1 d . . . O1 O 1.4711(8) 0.3565(6) 0.3842(9) 0.099(2) Uani 1 1 d . . . C2 C 1.1638(8) 0.1921(6) 0.2263(8) 0.0481(17) Uani 1 1 d . . . O2 O 1.1791(7) 0.1507(5) 0.1303(5) 0.0687(16) Uani 1 1 d . . . C3 C 1.2463(8) 0.1466(6) 0.4813(6) 0.0407(16) Uani 1 1 d . . . O3 O 1.3062(6) 0.0770(4) 0.5361(6) 0.0605(14) Uani 1 1 d . . . N1 N 1.0979(7) 0.3337(4) 0.5714(5) 0.0408(13) Uani 1 1 d . . . N2 N 1.1157(8) 0.3702(5) 0.7810(6) 0.0543(16) Uani 1 1 d . . . N3 N 0.9016(6) 0.1879(4) 0.3984(5) 0.0372(12) Uani 1 1 d . . . N4 N 0.6831(7) 0.0984(5) 0.3438(6) 0.0466(14) Uani 1 1 d . . . N5 N 1.0063(7) 0.3841(4) 0.2876(5) 0.0413(13) Uani 1 1 d . . . N6 N 0.8164(8) 0.4792(5) 0.1869(6) 0.0519(15) Uani 1 1 d . . . C11 C 1.1769(9) 0.3182(5) 0.6882(7) 0.0498(18) Uani 1 1 d . . . H11 H 1.2660 0.2755 0.7041 0.060 Uiso 1 1 calc R . . C12 C 0.9881(10) 0.4238(6) 0.7196(8) 0.060(2) Uani 1 1 d . . . H12 H 0.9204 0.4672 0.7592 0.072 Uiso 1 1 calc R . . C13 C 0.9791(10) 0.4019(6) 0.5910(8) 0.0557(19) Uani 1 1 d . . . H13 H 0.9040 0.4288 0.5256 0.067 Uiso 1 1 calc R . . C14 C 1.1700(13) 0.3702(9) 0.9221(8) 0.080(3) Uani 1 1 d . . . H14A H 1.1048 0.3239 0.9655 0.119 Uiso 1 1 calc R . . H14B H 1.1597 0.4375 0.9565 0.119 Uiso 1 1 calc R . . H14C H 1.2810 0.3493 0.9368 0.119 Uiso 1 1 calc R . . C21 C 0.8073(9) 0.1451(6) 0.3024(8) 0.0425(19) Uani 1 1 d . . . H21 H 0.8259 0.1474 0.2149 0.051 Uiso 1 1 calc R . . C22 C 0.6988(9) 0.1108(6) 0.4763(8) 0.058(2) Uani 1 1 d . . . H22 H 0.6287 0.0865 0.5331 0.069 Uiso 1 1 calc R . . C23 C 0.8333(9) 0.1643(7) 0.5097(7) 0.057(2) Uani 1 1 d . . . H23 H 0.8743 0.1828 0.5948 0.069 Uiso 1 1 calc R . . C24 C 0.5521(9) 0.0452(8) 0.2620(10) 0.074(3) Uani 1 1 d . . . H24A H 0.5109 0.0880 0.1897 0.112 Uiso 1 1 calc R . . H24B H 0.4668 0.0297 0.3138 0.112 Uiso 1 1 calc R . . H24C H 0.5930 -0.0167 0.2289 0.112 Uiso 1 1 calc R . . C31 C 0.8511(10) 0.3954(6) 0.2570(8) 0.046(2) Uani 1 1 d . . . H31 H 0.7740 0.3503 0.2814 0.055 Uiso 1 1 calc R . . C32 C 0.9565(11) 0.5254(6) 0.1738(8) 0.063(2) Uani 1 1 d . . . H32 H 0.9689 0.5864 0.1303 0.076 Uiso 1 1 calc R . . C33 C 1.0758(10) 0.4679(6) 0.2348(7) 0.0532(18) Uani 1 1 d . . . H33 H 1.1858 0.4819 0.2406 0.064 Uiso 1 1 calc R . . C34 C 0.6523(12) 0.5117(7) 0.1354(9) 0.081(3) Uani 1 1 d . . . H34A H 0.5749 0.4671 0.1678 0.121 Uiso 1 1 calc R . . H34B H 0.6400 0.5092 0.0411 0.121 Uiso 1 1 calc R . . H34C H 0.6347 0.5800 0.1635 0.121 Uiso 1 1 calc R . . P1 P 1.6784(3) 0.2370(2) 0.9078(2) 0.0617(9) Uani 1 1 d . . . F1 F 1.5332(12) 0.2245(9) 0.8107(11) 0.224(8) Uani 1 1 d . . . F2 F 1.8018(10) 0.2241(5) 0.8066(7) 0.129(3) Uani 1 1 d . . . F3 F 1.6720(13) 0.3529(7) 0.8744(12) 0.160(5) Uani 1 1 d . . . F4 F 1.5667(11) 0.2491(11) 1.0191(10) 0.192(5) Uani 1 1 d . . . F5 F 1.6874(12) 0.1206(5) 0.9405(10) 0.123(3) Uani 1 1 d . . . F6 F 1.8259(8) 0.2575(12) 1.0149(5) 0.150(3) 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 0.03318(14) 0.03939(15) 0.03750(14) 0.0026(2) 0.00566(8) 0.0015(2) C1 0.062(5) 0.041(5) 0.077(6) 0.003(4) 0.017(4) -0.001(4) O1 0.048(3) 0.098(5) 0.152(7) 0.016(5) 0.019(4) -0.021(3) C2 0.037(4) 0.053(4) 0.055(5) 0.008(4) 0.004(3) 0.001(3) O2 0.075(4) 0.086(4) 0.047(3) -0.015(3) 0.017(3) 0.016(3) C3 0.037(3) 0.051(4) 0.036(4) -0.003(3) 0.010(3) -0.005(3) O3 0.052(3) 0.057(3) 0.071(4) 0.021(3) 0.000(3) 0.010(3) N1 0.044(3) 0.042(3) 0.036(3) 0.002(2) 0.003(3) -0.002(3) N2 0.055(4) 0.059(4) 0.047(4) -0.005(3) 0.002(3) -0.013(3) N3 0.039(3) 0.042(3) 0.031(3) 0.003(2) 0.006(2) 0.003(2) N4 0.032(3) 0.052(4) 0.056(4) -0.006(3) 0.003(3) 0.002(3) N5 0.043(3) 0.043(3) 0.039(3) 0.004(2) 0.008(3) 0.007(3) N6 0.062(4) 0.046(4) 0.046(3) 0.002(3) 0.000(3) 0.016(3) C11 0.049(4) 0.052(4) 0.048(5) -0.006(3) 0.004(4) 0.001(3) C12 0.069(5) 0.054(5) 0.061(5) -0.014(4) 0.021(4) 0.006(4) C13 0.062(5) 0.048(4) 0.057(5) -0.003(3) 0.010(4) 0.017(4) C14 0.092(7) 0.105(8) 0.041(5) -0.011(5) 0.006(5) -0.012(6) C21 0.036(4) 0.047(4) 0.045(5) 0.001(4) 0.007(4) 0.002(4) C22 0.046(4) 0.073(5) 0.055(5) 0.009(4) 0.013(4) -0.012(4) C23 0.053(4) 0.084(6) 0.035(4) 0.001(4) 0.011(3) -0.015(4) C24 0.036(4) 0.096(7) 0.090(7) -0.025(5) 0.000(4) -0.009(4) C31 0.050(5) 0.044(5) 0.044(5) 0.005(3) 0.008(4) 0.010(4) C32 0.084(6) 0.043(4) 0.062(5) 0.015(4) 0.001(5) 0.002(4) C33 0.063(5) 0.045(4) 0.052(4) 0.004(3) 0.006(4) -0.006(4) C34 0.082(6) 0.084(7) 0.071(6) -0.003(5) -0.012(5) 0.044(5) P1 0.0521(10) 0.069(3) 0.0647(12) -0.0033(11) 0.0089(9) -0.0061(12) F1 0.158(7) 0.207(15) 0.267(12) 0.121(11) -0.133(8) -0.082(8) F2 0.188(7) 0.116(7) 0.099(4) 0.007(3) 0.081(5) 0.021(5) F3 0.144(8) 0.068(6) 0.279(16) 0.026(7) 0.072(10) 0.003(6) F4 0.194(7) 0.183(9) 0.234(9) 0.082(11) 0.167(7) 0.079(10) F5 0.120(6) 0.068(5) 0.180(8) 0.013(5) 0.017(5) 0.006(4) F6 0.132(5) 0.223(8) 0.087(4) -0.021(9) -0.017(4) -0.075(9) _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 1.896(9) . ? Re1 C3 1.900(8) . ? Re1 C2 1.909(8) . ? Re1 N1 2.186(5) . ? Re1 N5 2.192(5) . ? Re1 N3 2.197(5) . ? C1 O1 1.166(10) . ? C2 O2 1.145(9) . ? C3 O3 1.156(8) . ? N3 C21 1.310(9) . ? N3 C23 1.371(8) . ? N4 C21 1.317(10) . ? N4 C22 1.359(10) . ? N4 C24 1.471(10) . ? N1 C11 1.311(9) . ? N1 C13 1.369(9) . ? N2 C11 1.323(9) . ? N2 C12 1.365(10) . ? N2 C14 1.463(10) . ? N5 C31 1.303(10) . ? N5 C33 1.385(9) . ? N6 C31 1.329(10) . ? N6 C32 1.337(11) . ? N6 C34 1.470(10) . ? C12 C13 1.343(11) . ? C22 C23 1.334(11) . ? C32 C33 1.343(11) . ? P1 F1 1.481(8) . ? P1 F2 1.556(7) . ? P1 F3 1.561(10) . ? P1 F5 1.565(7) . ? P1 F4 1.566(6) . ? P1 F6 1.570(6) . ? 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 C3 88.8(3) . . ? C1 Re1 C2 89.3(3) . . ? C3 Re1 C2 89.8(3) . . ? C1 Re1 N1 93.0(3) . . ? C3 Re1 N1 92.2(2) . . ? C2 Re1 N1 176.9(2) . . ? C1 Re1 N5 93.6(3) . . ? C3 Re1 N5 177.2(2) . . ? C2 Re1 N5 91.6(3) . . ? N1 Re1 N5 86.2(2) . . ? C1 Re1 N3 178.2(3) . . ? C3 Re1 N3 91.7(2) . . ? C2 Re1 N3 92.4(2) . . ? N1 Re1 N3 85.2(2) . . ? N5 Re1 N3 85.9(2) . . ? O1 C1 Re1 177.9(7) . . ? O2 C2 Re1 178.3(7) . . ? O3 C3 Re1 177.5(6) . . ? C21 N3 C23 104.9(6) . . ? C21 N3 Re1 127.5(5) . . ? C23 N3 Re1 126.7(5) . . ? C21 N4 C22 106.4(6) . . ? C21 N4 C24 126.6(7) . . ? C22 N4 C24 127.1(7) . . ? C11 N1 C13 105.0(6) . . ? C11 N1 Re1 126.6(4) . . ? C13 N1 Re1 128.2(5) . . ? C11 N2 C12 106.4(6) . . ? C11 N2 C14 127.7(8) . . ? C12 N2 C14 126.0(7) . . ? C31 N5 C33 105.5(6) . . ? C31 N5 Re1 129.2(5) . . ? C33 N5 Re1 125.2(5) . . ? C31 N6 C32 107.2(7) . . ? C31 N6 C34 124.6(8) . . ? C32 N6 C34 128.2(7) . . ? N1 C11 N2 112.5(6) . . ? C13 C12 N2 106.9(7) . . ? C12 C13 N1 109.2(7) . . ? N3 C21 N4 112.5(7) . . ? C23 C22 N4 107.3(6) . . ? C22 C23 N3 109.0(7) . . ? N5 C31 N6 111.7(7) . . ? N6 C32 C33 107.8(7) . . ? C32 C33 N5 107.9(7) . . ? F1 P1 F2 95.3(7) . . ? F1 P1 F3 87.5(7) . . ? F2 P1 F3 88.1(5) . . ? F1 P1 F5 92.9(6) . . ? F2 P1 F5 91.0(4) . . ? F3 P1 F5 179.1(5) . . ? F1 P1 F4 89.5(7) . . ? F2 P1 F4 175.1(6) . . ? F3 P1 F4 93.0(7) . . ? F5 P1 F4 87.8(6) . . ? F1 P1 F6 175.6(8) . . ? F2 P1 F6 87.7(4) . . ? F3 P1 F6 89.4(7) . . ? F5 P1 F6 90.2(7) . . ? F4 P1 F6 87.5(5) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 23.30 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.816 _refine_diff_density_min -0.568 _refine_diff_density_rms 0.080 #===END data_Compound_5_(li417) _database_code_depnum_ccdc_archive 'CCDC 642015' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C15 H18 N6 O3 Re), Cl6 Pt, 2(C H2 Cl2)' _chemical_formula_sum 'C32 H40 Cl10 N12 O6 Pt Re2' _chemical_formula_weight 1610.75 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' Cl Cl 0.3639 0.7018 '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' Re Re -5.2083 5.8923 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -4.5932 6.9264 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 18.384(4) _cell_length_b 9.2341(18) _cell_length_c 15.713(3) _cell_angle_alpha 90.00 _cell_angle_beta 111.20(3) _cell_angle_gamma 90.00 _cell_volume 2486.9(10) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description yellow _exptl_crystal_colour plate _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.151 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1524 _exptl_absorpt_coefficient_mu 19.864 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _exptl_absorpt_correction_T_min 0.645 _exptl_absorpt_correction_T_max 1.674 _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _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 KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4547 _diffrn_reflns_av_R_equivalents 0.0713 _diffrn_reflns_av_sigmaI/netI 0.0469 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.58 _diffrn_reflns_theta_max 68.48 _reflns_number_total 4547 _reflns_number_gt 3919 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2006)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor, 1997) ; _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^)+(0.0956P)^2^+34.9432P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4547 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0655 _refine_ls_R_factor_gt 0.0573 _refine_ls_wR_factor_ref 0.1651 _refine_ls_wR_factor_gt 0.1516 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _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 Pt1 Pt 0.5000 0.0000 1.0000 0.02356(19) Uani 1 2 d S . . Re1 Re 0.17728(2) 0.84294(5) 0.61448(3) 0.02866(19) Uani 1 1 d . . . Cl1 Cl 0.42822(19) 0.1720(4) 0.8974(3) 0.0635(10) Uani 1 1 d . . . Cl2 Cl 0.60630(15) 0.0558(3) 0.9593(2) 0.0402(6) Uani 1 1 d . . . Cl3 Cl 0.4609(2) -0.1726(4) 0.8861(3) 0.0652(11) Uani 1 1 d . . . Cl91 Cl 0.8996(3) 0.9590(6) 0.7372(4) 0.0898(14) Uani 1 1 d . . . Cl92 Cl 0.8799(5) 0.8509(11) 0.8997(7) 0.195(6) Uani 1 1 d . . . O1 O 0.0770(6) 1.0535(11) 0.4663(6) 0.056(2) Uani 1 1 d . . . O2 O 0.1925(6) 0.6713(10) 0.4548(6) 0.052(2) Uani 1 1 d . . . O3 O 0.0264(5) 0.6740(10) 0.5873(8) 0.057(3) Uani 1 1 d . . . N1 N 0.1673(5) 0.9700(9) 0.7278(6) 0.0292(18) Uani 1 1 d . . . N2 N 0.1899(5) 1.1077(10) 0.8483(6) 0.0330(19) Uani 1 1 d . . . N3 N 0.2857(5) 0.9641(10) 0.6419(6) 0.0308(18) Uani 1 1 d . . . N4 N 0.4086(5) 1.0157(10) 0.6678(6) 0.034(2) Uani 1 1 d . . . N5 N 0.2502(5) 0.6908(10) 0.7175(6) 0.0312(18) Uani 1 1 d . . . N6 N 0.3113(5) 0.5762(10) 0.8463(6) 0.0329(19) Uani 1 1 d . . . C1 C 0.1150(7) 0.9784(13) 0.5239(8) 0.039(3) Uani 1 1 d . . . C2 C 0.1880(6) 0.7352(13) 0.5171(8) 0.038(3) Uani 1 1 d . . . C3 C 0.0834(7) 0.7374(15) 0.5981(9) 0.046(3) Uani 1 1 d . . . C11 C 0.2210(7) 1.0405(12) 0.7943(7) 0.033(2) Uani 1 1 d . . . H11 H 0.2748 1.0430 0.8027 0.039 Uiso 1 1 calc R . . C12 C 0.0974(7) 0.9931(14) 0.7396(9) 0.046(3) Uani 1 1 d . . . H12 H 0.0484 0.9546 0.7017 0.055 Uiso 1 1 calc R . . C13 C 0.1091(7) 1.0788(14) 0.8133(9) 0.047(3) Uani 1 1 d . . . H13 H 0.0710 1.1122 0.8364 0.056 Uiso 1 1 calc R . . C14 C 0.2305(8) 1.1904(13) 0.9286(8) 0.042(3) Uani 1 1 d . . . H14A H 0.2866 1.1894 0.9398 0.063 Uiso 1 1 calc R . . H14B H 0.2214 1.1480 0.9810 0.063 Uiso 1 1 calc R . . H14C H 0.2115 1.2905 0.9199 0.063 Uiso 1 1 calc R . . C21 C 0.3562(6) 0.9104(12) 0.6626(7) 0.031(2) Uani 1 1 d . . . H21 H 0.3687 0.8105 0.6727 0.037 Uiso 1 1 calc R . . C22 C 0.2940(6) 1.1119(12) 0.6340(7) 0.031(2) Uani 1 1 d . . . H22 H 0.2526 1.1801 0.6203 0.038 Uiso 1 1 calc R . . C23 C 0.3679(7) 1.1452(12) 0.6482(8) 0.034(2) Uani 1 1 d . . . H23 H 0.3886 1.2387 0.6455 0.041 Uiso 1 1 calc R . . C24 C 0.4934(6) 0.9936(15) 0.6954(9) 0.046(3) Uani 1 1 d . . . H24A H 0.5042 0.8904 0.6910 0.070 Uiso 1 1 calc R . . H24B H 0.5195 1.0263 0.7584 0.070 Uiso 1 1 calc R . . H24C H 0.5129 1.0492 0.6550 0.070 Uiso 1 1 calc R . . C31 C 0.2717(6) 0.6935(11) 0.8078(7) 0.030(2) Uani 1 1 d . . . H31 H 0.2600 0.7705 0.8409 0.036 Uiso 1 1 calc R . . C32 C 0.2800(6) 0.5628(13) 0.6984(8) 0.040(3) Uani 1 1 d . . . H32 H 0.2753 0.5298 0.6394 0.048 Uiso 1 1 calc R . . C33 C 0.3171(7) 0.4917(14) 0.7783(8) 0.042(3) Uani 1 1 d . . . H33 H 0.3423 0.4003 0.7852 0.050 Uiso 1 1 calc R . . C34 C 0.3482(8) 0.5505(14) 0.9445(8) 0.045(3) Uani 1 1 d . . . H34A H 0.3810 0.6336 0.9733 0.067 Uiso 1 1 calc R . . H34B H 0.3805 0.4631 0.9551 0.067 Uiso 1 1 calc R . . H34C H 0.3078 0.5377 0.9709 0.067 Uiso 1 1 calc R . . C90 C 0.9413(15) 0.862(2) 0.8436(19) 0.120(10) Uani 1 1 d . . . H90A H 0.9557 0.7632 0.8311 0.144 Uiso 1 1 calc R . . H90B H 0.9896 0.9119 0.8826 0.144 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 Pt1 0.0172(3) 0.0276(3) 0.0268(3) 0.0014(2) 0.0090(2) 0.0005(2) Re1 0.0190(3) 0.0390(3) 0.0279(3) 0.00127(17) 0.0083(2) 0.00337(17) Cl1 0.0351(16) 0.068(2) 0.088(3) 0.0479(19) 0.0231(17) 0.0169(14) Cl2 0.0275(12) 0.0447(14) 0.0573(17) 0.0067(12) 0.0260(12) -0.0002(10) Cl3 0.083(3) 0.070(2) 0.058(2) -0.0324(17) 0.043(2) -0.0419(19) Cl91 0.072(3) 0.113(4) 0.082(3) -0.036(3) 0.025(2) -0.013(3) Cl92 0.094(5) 0.225(10) 0.207(9) 0.138(8) -0.016(5) -0.064(5) O1 0.052(5) 0.059(5) 0.045(5) 0.023(4) 0.003(4) 0.019(5) O2 0.054(6) 0.063(6) 0.041(5) -0.017(4) 0.021(4) 0.001(4) O3 0.024(4) 0.061(6) 0.079(7) 0.007(5) 0.010(4) -0.012(4) N1 0.026(4) 0.036(4) 0.032(4) 0.001(4) 0.018(4) 0.008(4) N2 0.025(4) 0.042(5) 0.035(5) -0.003(4) 0.015(4) 0.006(4) N3 0.024(4) 0.039(5) 0.032(5) 0.001(4) 0.013(4) 0.002(4) N4 0.024(5) 0.049(5) 0.026(4) 0.003(4) 0.007(4) -0.001(4) N5 0.019(4) 0.041(5) 0.033(5) 0.005(4) 0.009(4) 0.002(4) N6 0.032(5) 0.034(5) 0.031(5) -0.001(4) 0.010(4) -0.007(4) C1 0.038(6) 0.046(6) 0.037(6) -0.001(5) 0.019(5) 0.006(5) C2 0.016(5) 0.042(6) 0.044(6) 0.012(5) -0.005(4) 0.000(4) C3 0.036(7) 0.055(7) 0.045(7) -0.001(6) 0.012(5) 0.016(6) C11 0.036(6) 0.035(5) 0.035(6) 0.005(5) 0.023(5) 0.001(4) C12 0.018(5) 0.065(8) 0.052(7) -0.009(6) 0.009(5) 0.009(5) C13 0.023(5) 0.058(8) 0.061(8) 0.001(6) 0.018(6) 0.008(5) C14 0.044(7) 0.044(6) 0.039(6) -0.013(5) 0.016(5) 0.000(5) C21 0.021(5) 0.041(6) 0.032(5) 0.009(4) 0.011(4) 0.005(4) C22 0.028(5) 0.041(6) 0.026(5) 0.000(4) 0.010(4) 0.008(4) C23 0.034(6) 0.037(6) 0.036(6) -0.004(4) 0.018(5) -0.001(4) C24 0.016(5) 0.071(9) 0.050(7) 0.010(6) 0.009(5) 0.001(5) C31 0.036(6) 0.030(5) 0.021(5) 0.003(4) 0.007(4) -0.001(4) C32 0.028(5) 0.052(7) 0.036(6) 0.005(5) 0.006(5) 0.016(5) C33 0.031(6) 0.058(8) 0.039(6) -0.001(5) 0.016(5) 0.014(5) C34 0.058(8) 0.041(6) 0.035(6) 0.006(5) 0.016(6) -0.004(6) C90 0.098(17) 0.082(14) 0.14(2) -0.052(14) -0.003(16) 0.008(12) _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 Pt1 Cl1 2.307(3) . ? Pt1 Cl1 2.307(3) 3_657 ? Pt1 Cl3 2.309(3) . ? Pt1 Cl3 2.309(3) 3_657 ? Pt1 Cl2 2.323(2) . ? Pt1 Cl2 2.323(2) 3_657 ? Re1 C2 1.895(13) . ? Re1 C3 1.916(14) . ? Re1 C1 1.930(12) . ? Re1 N3 2.188(9) . ? Re1 N1 2.195(8) . ? Re1 N5 2.196(9) . ? Cl91 C90 1.80(3) . ? Cl92 C90 1.67(3) . ? O1 C1 1.154(15) . ? O2 C2 1.171(15) . ? O3 C3 1.158(16) . ? N1 C11 1.320(15) . ? N1 C12 1.380(14) . ? N2 C11 1.335(13) . ? N2 C13 1.410(14) . ? N2 C14 1.433(15) . ? N3 C21 1.315(13) . ? N3 C22 1.384(14) . ? N4 C21 1.350(14) . ? N4 C23 1.385(14) . ? N4 C24 1.474(14) . ? N5 C31 1.328(13) . ? N5 C32 1.380(15) . ? N6 C31 1.323(14) . ? N6 C33 1.358(15) . ? N6 C34 1.463(15) . ? C12 C13 1.354(19) . ? C22 C23 1.331(15) . ? C32 C33 1.361(17) . ? 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 Cl1 Pt1 Cl1 180.000(1) . 3_657 ? Cl1 Pt1 Cl3 89.67(17) . . ? Cl1 Pt1 Cl3 90.33(17) 3_657 . ? Cl1 Pt1 Cl3 90.33(17) . 3_657 ? Cl1 Pt1 Cl3 89.67(17) 3_657 3_657 ? Cl3 Pt1 Cl3 180.000(1) . 3_657 ? Cl1 Pt1 Cl2 88.89(11) . . ? Cl1 Pt1 Cl2 91.11(11) 3_657 . ? Cl3 Pt1 Cl2 89.82(11) . . ? Cl3 Pt1 Cl2 90.18(12) 3_657 . ? Cl1 Pt1 Cl2 91.11(11) . 3_657 ? Cl1 Pt1 Cl2 88.89(11) 3_657 3_657 ? Cl3 Pt1 Cl2 90.18(12) . 3_657 ? Cl3 Pt1 Cl2 89.82(11) 3_657 3_657 ? Cl2 Pt1 Cl2 180.000(1) . 3_657 ? C2 Re1 C3 88.6(5) . . ? C2 Re1 C1 87.2(5) . . ? C3 Re1 C1 88.0(5) . . ? C2 Re1 N3 94.2(4) . . ? C3 Re1 N3 176.6(4) . . ? C1 Re1 N3 94.0(4) . . ? C2 Re1 N1 178.8(4) . . ? C3 Re1 N1 92.6(4) . . ? C1 Re1 N1 92.9(4) . . ? N3 Re1 N1 84.5(3) . . ? C2 Re1 N5 92.6(4) . . ? C3 Re1 N5 93.1(4) . . ? C1 Re1 N5 178.9(4) . . ? N3 Re1 N5 85.0(3) . . ? N1 Re1 N5 87.2(3) . . ? C11 N1 C12 106.5(9) . . ? C11 N1 Re1 130.4(7) . . ? C12 N1 Re1 123.1(8) . . ? C11 N2 C13 107.2(10) . . ? C11 N2 C14 126.9(10) . . ? C13 N2 C14 125.8(9) . . ? C21 N3 C22 105.3(9) . . ? C21 N3 Re1 127.1(7) . . ? C22 N3 Re1 127.5(7) . . ? C21 N4 C23 107.1(9) . . ? C21 N4 C24 125.0(10) . . ? C23 N4 C24 127.9(10) . . ? C31 N5 C32 105.1(9) . . ? C31 N5 Re1 129.9(7) . . ? C32 N5 Re1 124.9(7) . . ? C31 N6 C33 107.3(9) . . ? C31 N6 C34 125.7(10) . . ? C33 N6 C34 126.8(10) . . ? O1 C1 Re1 176.3(11) . . ? O2 C2 Re1 177.7(10) . . ? O3 C3 Re1 179.4(13) . . ? N1 C11 N2 111.3(9) . . ? C13 C12 N1 109.7(11) . . ? C12 C13 N2 105.3(10) . . ? N3 C21 N4 111.2(9) . . ? C23 C22 N3 110.6(9) . . ? C22 C23 N4 105.9(10) . . ? N6 C31 N5 112.0(9) . . ? C33 C32 N5 108.6(10) . . ? N6 C33 C32 107.0(10) . . ? Cl92 C90 Cl91 112.2(14) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 68.48 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 3.243 _refine_diff_density_min -2.424 _refine_diff_density_rms 0.293 #===END data_Compound_6_(li387) _database_code_depnum_ccdc_archive 'CCDC 642016' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ' C15 H18 N6 O3 Re, H O4 S, C H2 Cl2' _chemical_formula_sum 'C16 H21 Cl2 N6 O7 Re S' _chemical_formula_weight 698.55 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' Cl Cl 0.3639 0.7018 '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' S S 0.3331 0.5567 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.1111(14) _cell_length_b 10.866(2) _cell_length_c 16.743(3) _cell_angle_alpha 97.15(3) _cell_angle_beta 96.72(3) _cell_angle_gamma 107.55(3) _cell_volume 1207.5(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.921 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 680 _exptl_absorpt_coefficient_mu 13.129 _exptl_absorpt_correction_type 'multi scan' _exptl_absorpt_correction_T_min 0.728 _exptl_absorpt_correction_T_max 1.467 _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _diffrn_ambient_temperature 293(2) _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 KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6292 _diffrn_reflns_av_R_equivalents 0.0966 _diffrn_reflns_av_sigmaI/netI 0.1031 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.70 _diffrn_reflns_theta_max 68.87 _reflns_number_total 4407 _reflns_number_gt 3963 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.1546P)^2^+3.7547P] 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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0047(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4407 _refine_ls_number_parameters 278 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0851 _refine_ls_R_factor_gt 0.0697 _refine_ls_wR_factor_ref 0.2310 _refine_ls_wR_factor_gt 0.1880 _refine_ls_goodness_of_fit_ref 1.122 _refine_ls_restrained_S_all 1.122 _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 0.60555(5) 0.10177(4) 0.32705(2) 0.0307(3) Uani 1 1 d . . . Cl91 Cl 0.4519(5) 0.6548(4) 0.4380(2) 0.0662(9) Uani 1 1 d . . . Cl92 Cl 0.0428(6) 0.4977(3) 0.3672(2) 0.0626(9) Uani 1 1 d . . . S2 S 0.4411(4) 0.3041(3) -0.00187(17) 0.0395(6) Uani 1 1 d . . . O1 O 0.4944(13) 0.3534(8) 0.3427(5) 0.0475(19) Uani 1 1 d . . . O2 O 0.3123(13) 0.0056(10) 0.4457(5) 0.051(2) Uani 1 1 d . . . O3 O 0.9364(13) 0.2399(8) 0.4742(5) 0.049(2) Uani 1 1 d . . . O11 O 0.4780(13) 0.3102(10) 0.0855(6) 0.054(2) Uani 1 1 d . . . O12 O 0.2948(11) 0.3664(8) -0.0269(5) 0.0413(17) Uani 1 1 d . . . O13 O 0.6397(8) 0.3863(4) -0.0277(2) 0.048(2) Uani 1 1 d G . . O14 O 0.3951(7) 0.1752(5) -0.04902(19) 0.062(3) Uani 1 1 d G . . N1 N 0.8143(4) 0.1720(3) 0.24303(18) 0.0344(19) Uani 1 1 d G . . N2 N 0.9864(5) 0.3102(4) 0.1741(2) 0.039(2) Uani 1 1 d G . . N3 N 0.3802(4) -0.0078(3) 0.22087(19) 0.0349(19) Uani 1 1 d G . . N4 N 0.2165(5) -0.0841(3) 0.0966(2) 0.0319(18) Uani 1 1 d G . . N5 N 0.6980(5) -0.0731(3) 0.3135(2) 0.038(2) Uani 1 1 d G . . N6 N 0.7231(8) -0.2675(4) 0.2744(3) 0.0339(18) Uani 1 1 d G . . C1 C 0.5322(6) 0.2549(3) 0.33584(19) 0.035(2) Uani 1 1 d G . . C2 C 0.4171(6) 0.0396(4) 0.3996(2) 0.041(3) Uani 1 1 d G . . C3 C 0.8125(6) 0.1892(4) 0.41774(17) 0.044(3) Uani 1 1 d G . . C11 C 0.8195(4) 0.2704(3) 0.2044(2) 0.030(2) Uani 1 1 d G . . H11 H 0.7156 0.3085 0.1989 0.036 Uiso 1 1 calc R . . C12 C 0.9896(17) 0.1445(12) 0.2350(8) 0.046(3) Uani 1 1 d . . . H12 H 1.0277 0.0771 0.2565 0.055 Uiso 1 1 calc R . . C13 C 1.0998(17) 0.2298(12) 0.1911(7) 0.042(2) Uani 1 1 d . . . H13 H 1.2255 0.2332 0.1757 0.051 Uiso 1 1 calc R . . C14 C 1.048(2) 0.4227(12) 0.1303(8) 0.047(3) Uani 1 1 d . . . H14A H 0.9303 0.4458 0.1100 0.071 Uiso 1 1 calc R . . H14B H 1.1105 0.3987 0.0842 0.071 Uiso 1 1 calc R . . H14C H 1.1439 0.4979 0.1676 0.071 Uiso 1 1 calc R . . C21 C 0.3722(15) 0.0048(9) 0.1435(6) 0.030(2) Uani 1 1 d . . . H21 H 0.4679 0.0706 0.1237 0.036 Uiso 1 1 calc R . . C22 C 0.2167(15) -0.1111(11) 0.2227(6) 0.037(2) Uani 1 1 d . . . H22 H 0.1807 -0.1440 0.2707 0.044 Uiso 1 1 calc R . . C23 C 0.1105(14) -0.1613(11) 0.1454(7) 0.040(2) Uani 1 1 d . . . H23 H -0.0093 -0.2334 0.1295 0.049 Uiso 1 1 calc R . . C24 C 0.1681(18) -0.1054(12) 0.0059(7) 0.043(3) Uani 1 1 d . . . H24A H 0.2305 -0.0237 -0.0137 0.064 Uiso 1 1 calc R . . H24B H 0.0229 -0.1327 -0.0108 0.064 Uiso 1 1 calc R . . H24C H 0.2193 -0.1737 -0.0175 0.064 Uiso 1 1 calc R . . C31 C 0.6452(16) -0.1727(10) 0.2546(6) 0.032(2) Uani 1 1 d . . . H31 H 0.5630 -0.1788 0.2043 0.039 Uiso 1 1 calc R . . C32 C 0.8204(15) -0.1054(10) 0.3751(7) 0.035(2) Uani 1 1 d . . . H32 H 0.8819 -0.0516 0.4264 0.042 Uiso 1 1 calc R . . C33 C 0.8363(17) -0.2229(11) 0.3501(7) 0.041(2) Uani 1 1 d . . . H33 H 0.9115 -0.2667 0.3793 0.049 Uiso 1 1 calc R . . C34 C 0.686(2) -0.3947(12) 0.2241(8) 0.048(3) Uani 1 1 d . . . H34A H 0.8132 -0.4051 0.2134 0.072 Uiso 1 1 calc R . . H34B H 0.6015 -0.4001 0.1722 0.072 Uiso 1 1 calc R . . H34C H 0.6175 -0.4642 0.2527 0.072 Uiso 1 1 calc R . . C90 C 0.2498(18) 0.5197(12) 0.4429(8) 0.047(3) Uani 1 1 d . . . H90A H 0.2095 0.5304 0.4973 0.057 Uiso 1 1 calc R . . H90B H 0.2912 0.4403 0.4367 0.057 Uiso 1 1 calc R . . H1S H 0.6794 0.4503 -0.0128 0.057 Uiso 1 1 d G . . 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 0.0289(4) 0.0317(4) 0.0289(4) 0.0020(2) -0.0018(2) 0.0095(2) Cl91 0.0522(19) 0.063(2) 0.070(2) 0.0041(17) 0.0106(16) 0.0017(15) Cl92 0.066(2) 0.0523(17) 0.0573(19) -0.0002(14) -0.0140(16) 0.0143(15) S2 0.0358(14) 0.0367(13) 0.0439(15) 0.0075(11) 0.0032(11) 0.0097(11) O1 0.053(5) 0.034(4) 0.053(5) 0.002(3) 0.003(4) 0.015(4) O2 0.043(5) 0.080(6) 0.027(4) 0.018(4) 0.009(3) 0.010(4) O3 0.046(5) 0.048(5) 0.037(4) -0.003(3) -0.021(4) 0.005(4) O11 0.041(5) 0.072(6) 0.049(5) 0.020(4) 0.002(4) 0.016(4) O12 0.031(4) 0.046(4) 0.044(4) 0.010(3) -0.002(3) 0.010(3) O13 0.039(5) 0.045(4) 0.063(6) 0.012(4) 0.013(4) 0.015(4) O14 0.064(6) 0.043(5) 0.075(7) -0.004(4) 0.023(5) 0.015(4) N1 0.026(4) 0.031(4) 0.037(5) -0.001(4) -0.002(4) 0.002(3) N2 0.036(5) 0.038(4) 0.033(5) 0.000(4) -0.002(4) 0.004(4) N3 0.027(4) 0.039(5) 0.032(5) -0.008(4) -0.004(3) 0.009(4) N4 0.034(4) 0.039(4) 0.023(4) 0.004(3) 0.000(3) 0.014(4) N5 0.035(5) 0.032(5) 0.041(5) 0.006(4) -0.008(4) 0.008(4) N6 0.039(5) 0.035(4) 0.028(4) 0.010(3) -0.002(4) 0.014(4) C1 0.033(6) 0.026(5) 0.044(6) 0.005(4) 0.005(5) 0.007(4) C2 0.043(6) 0.028(5) 0.044(6) -0.001(4) -0.025(5) 0.014(5) C3 0.036(6) 0.051(6) 0.052(7) 0.007(5) 0.003(5) 0.026(5) C11 0.022(4) 0.034(5) 0.031(5) 0.012(4) 0.000(4) 0.003(4) C12 0.036(6) 0.052(7) 0.055(7) 0.004(5) 0.014(5) 0.022(5) C13 0.038(6) 0.051(6) 0.036(6) 0.000(5) 0.007(5) 0.014(5) C14 0.051(7) 0.038(6) 0.045(7) 0.007(5) 0.012(6) 0.001(5) C21 0.031(5) 0.031(5) 0.026(5) -0.001(4) -0.009(4) 0.013(4) C22 0.028(5) 0.045(6) 0.035(5) 0.016(4) 0.002(4) 0.005(4) C23 0.016(4) 0.046(6) 0.050(7) 0.007(5) -0.008(4) 0.002(4) C24 0.041(6) 0.057(7) 0.028(6) 0.004(5) -0.009(5) 0.020(5) C31 0.039(6) 0.037(5) 0.026(5) 0.009(4) 0.005(4) 0.018(4) C32 0.033(5) 0.030(5) 0.039(6) 0.014(4) -0.006(4) 0.007(4) C33 0.039(6) 0.047(6) 0.038(6) 0.012(5) 0.001(5) 0.016(5) C34 0.053(7) 0.044(6) 0.050(7) 0.005(5) 0.001(6) 0.025(5) C90 0.041(6) 0.051(7) 0.047(7) 0.006(5) 0.004(5) 0.012(5) _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 1.882(3) . ? Re1 C3 1.910(3) . ? Re1 C2 1.941(3) . ? Re1 N5 2.185(3) . ? Re1 N3 2.191(3) . ? Re1 N1 2.199(3) . ? Cl91 C90 1.735(12) . ? Cl92 C90 1.762(12) . ? S2 O14 1.442(5) . ? S2 O11 1.445(9) . ? S2 O12 1.453(8) . ? S2 O13 1.568(5) . ? O1 C1 1.175(9) . ? O2 C2 1.152(8) . ? O3 C3 1.165(8) . ? N1 C11 1.3109 . ? N1 C12 1.384(11) . ? N2 C11 1.3185 . ? N2 C13 1.388(13) . ? N2 C14 1.484(12) . ? N3 C21 1.316(10) . ? N3 C22 1.357(10) . ? N4 C21 1.318(10) . ? N4 C23 1.369(12) . ? N4 C24 1.490(11) . ? N5 C31 1.299(11) . ? N5 C32 1.417(10) . ? N6 C31 1.365(10) . ? N6 C33 1.365(12) . ? N6 C34 1.459(13) . ? C12 C13 1.372(17) . ? C22 C23 1.375(15) . ? C32 C33 1.335(16) . ? 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 C3 87.06(12) . . ? C1 Re1 C2 87.20(13) . . ? C3 Re1 C2 91.11(12) . . ? C1 Re1 N5 177.82(17) . . ? C3 Re1 N5 93.02(13) . . ? C2 Re1 N5 94.97(13) . . ? C1 Re1 N3 96.70(13) . . ? C3 Re1 N3 175.98(18) . . ? C2 Re1 N3 90.49(13) . . ? N5 Re1 N3 83.17(11) . . ? C1 Re1 N1 92.36(12) . . ? C3 Re1 N1 89.87(13) . . ? C2 Re1 N1 178.90(16) . . ? N5 Re1 N1 85.47(11) . . ? N3 Re1 N1 88.56(10) . . ? O14 S2 O11 114.8(4) . . ? O14 S2 O12 111.5(4) . . ? O11 S2 O12 112.5(5) . . ? O14 S2 O13 104.4(3) . . ? O11 S2 O13 107.7(4) . . ? O12 S2 O13 105.0(4) . . ? C11 N1 C12 105.9(6) . . ? C11 N1 Re1 125.16(8) . . ? C12 N1 Re1 127.4(6) . . ? C11 N2 C13 108.5(5) . . ? C11 N2 C14 126.7(6) . . ? C13 N2 C14 124.7(8) . . ? C21 N3 C22 104.8(6) . . ? C21 N3 Re1 130.2(5) . . ? C22 N3 Re1 125.0(5) . . ? C21 N4 C23 108.0(7) . . ? C21 N4 C24 127.1(7) . . ? C23 N4 C24 124.8(7) . . ? C31 N5 C32 105.1(7) . . ? C31 N5 Re1 130.2(5) . . ? C32 N5 Re1 124.5(5) . . ? C31 N6 C33 107.6(7) . . ? C31 N6 C34 125.6(7) . . ? C33 N6 C34 126.7(7) . . ? O1 C1 Re1 177.3(6) . . ? O2 C2 Re1 176.8(5) . . ? O3 C3 Re1 178.1(6) . . ? N1 C11 N2 111.7 . . ? C13 C12 N1 109.3(10) . . ? C12 C13 N2 104.5(9) . . ? N3 C21 N4 112.4(8) . . ? N3 C22 C23 110.5(9) . . ? N4 C23 C22 104.4(8) . . ? N5 C31 N6 111.2(8) . . ? C33 C32 N5 109.7(9) . . ? C32 C33 N6 106.4(9) . . ? Cl91 C90 Cl92 112.7(7) . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 68.87 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 2.837 _refine_diff_density_min -2.946 _refine_diff_density_rms 0.363 #===END data_Compound_8_(Li478) _database_code_depnum_ccdc_archive 'CCDC 642017' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H24 N6 O3 Re, Br' _chemical_formula_sum 'C30 H24 Br N6 O3 Re' _chemical_formula_weight 782.66 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' Br Br -0.2901 2.4595 '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 Orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' _cell_length_a 19.1346(17) _cell_length_b 14.3590(13) _cell_length_c 10.2350(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2812.1(4) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.849 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1520 _exptl_absorpt_coefficient_mu 5.786 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.780904 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 'SMART 1k' _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 31396 _diffrn_reflns_av_R_equivalents 0.0400 _diffrn_reflns_av_sigmaI/netI 0.0221 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 29.16 _reflns_number_total 3931 _reflns_number_gt 3399 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics X-Seed _computing_publication_material X-Seed _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^)+(0.0126P)^2^+3.6478P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3931 _refine_ls_number_parameters 208 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0273 _refine_ls_R_factor_gt 0.0200 _refine_ls_wR_factor_ref 0.0412 _refine_ls_wR_factor_gt 0.0392 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _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 0.004197(6) 0.2500 0.147412(11) 0.01236(4) Uani 1 2 d S . . Br1 Br -0.036598(16) 0.2500 0.65157(3) 0.02092(7) Uani 1 2 d S . . O1 O -0.05739(9) 0.10154(12) -0.03382(16) 0.0259(4) Uani 1 1 d . . . O2 O -0.13046(12) 0.2500 0.3114(2) 0.0267(6) Uani 1 2 d S . . N1 N 0.05574(9) 0.14173(13) 0.26475(17) 0.0150(4) Uani 1 1 d . . . N2 N 0.09464(9) 0.05025(13) 0.42161(18) 0.0166(4) Uani 1 1 d . . . N3 N 0.10333(13) 0.2500 0.0403(2) 0.0155(5) Uani 1 2 d S . . N4 N 0.18104(13) 0.2500 -0.1181(2) 0.0156(5) Uani 1 2 d S . . C1 C -0.03502(11) 0.15681(16) 0.0355(2) 0.0171(4) Uani 1 1 d . . . C2 C -0.07960(16) 0.2500 0.2517(3) 0.0180(6) Uani 1 2 d S . . C11 C 0.05887(11) 0.12876(16) 0.3928(2) 0.0155(4) Uani 1 1 d . . . H11 H 0.0387 0.1692 0.4559 0.019 Uiso 1 1 calc R . . C12 C 0.09024(12) 0.06635(16) 0.2097(2) 0.0202(5) Uani 1 1 d . . . H12 H 0.0962 0.0561 0.1187 0.024 Uiso 1 1 calc R . . C13 C 0.11414(13) 0.00971(17) 0.3049(2) 0.0219(5) Uani 1 1 d . . . H13 H 0.1393 -0.0468 0.2938 0.026 Uiso 1 1 calc R . . C14 C 0.11550(11) 0.02198(16) 0.5506(2) 0.0180(4) Uani 1 1 d . . . C15 C 0.18009(12) -0.01976(18) 0.5677(2) 0.0250(5) Uani 1 1 d . . . H15 H 0.2092 -0.0326 0.4947 0.030 Uiso 1 1 calc R . . C16 C 0.20168(13) -0.0426(2) 0.6933(3) 0.0304(6) Uani 1 1 d . . . H16 H 0.2456 -0.0720 0.7063 0.036 Uiso 1 1 calc R . . C17 C 0.15965(13) -0.02297(19) 0.7991(3) 0.0274(5) Uani 1 1 d . . . H17 H 0.1750 -0.0379 0.8848 0.033 Uiso 1 1 calc R . . C18 C 0.09488(13) 0.01859(17) 0.7806(2) 0.0235(5) Uani 1 1 d . . . H18 H 0.0659 0.0320 0.8537 0.028 Uiso 1 1 calc R . . C19 C 0.07236(12) 0.04062(16) 0.6551(2) 0.0202(4) Uani 1 1 d . . . H19 H 0.0278 0.0682 0.6417 0.024 Uiso 1 1 calc R . . C21 C 0.11250(15) 0.2500 -0.0883(3) 0.0157(6) Uani 1 2 d S . . H21 H 0.0757 0.2500 -0.1507 0.019 Uiso 1 2 calc SR . . C22 C 0.16948(17) 0.2500 0.0947(3) 0.0220(7) Uani 1 2 d S . . H22 H 0.1794 0.2500 0.1857 0.026 Uiso 1 2 calc SR . . C23 C 0.21787(17) 0.2500 -0.0016(3) 0.0225(7) Uani 1 2 d S . . H23 H 0.2672 0.2500 0.0086 0.027 Uiso 1 2 calc SR . . C24 C 0.21111(16) 0.2500 -0.2469(3) 0.0179(6) Uani 1 2 d S . . C25 C 0.16914(16) 0.2500 -0.3563(3) 0.0211(7) Uani 1 2 d S . . H25 H 0.1197 0.2500 -0.3477 0.025 Uiso 1 2 calc SR . . C26 C 0.19985(18) 0.2500 -0.4796(3) 0.0251(7) Uani 1 2 d S . . H26 H 0.1711 0.2500 -0.5553 0.030 Uiso 1 2 calc SR . . C27 C 0.27189(18) 0.2500 -0.4931(3) 0.0287(8) Uani 1 2 d S . . H27 H 0.2926 0.2500 -0.5774 0.034 Uiso 1 2 calc SR . . C28 C 0.31315(19) 0.2500 -0.3824(4) 0.0343(9) Uani 1 2 d S . . H28 H 0.3626 0.2500 -0.3912 0.041 Uiso 1 2 calc SR . . C29 C 0.28375(17) 0.2500 -0.2594(4) 0.0275(8) Uani 1 2 d S . . H29 H 0.3126 0.2500 -0.1839 0.033 Uiso 1 2 calc SR . . 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 0.01312(6) 0.01389(6) 0.01007(5) 0.000 -0.00038(5) 0.000 Br1 0.01946(15) 0.02253(16) 0.02075(15) 0.000 0.00503(12) 0.000 O1 0.0354(10) 0.0247(9) 0.0176(8) -0.0034(7) -0.0047(7) -0.0073(8) O2 0.0203(12) 0.0375(15) 0.0223(12) 0.000 0.0054(10) 0.000 N1 0.0163(8) 0.0150(9) 0.0137(8) 0.0001(7) -0.0002(7) 0.0001(7) N2 0.0182(9) 0.0142(9) 0.0173(9) 0.0022(7) 0.0002(7) 0.0031(7) N3 0.0145(12) 0.0182(13) 0.0139(12) 0.000 -0.0015(9) 0.000 N4 0.0140(12) 0.0200(14) 0.0128(12) 0.000 -0.0005(9) 0.000 C1 0.0171(10) 0.0199(11) 0.0143(10) 0.0022(8) 0.0008(8) 0.0001(8) C2 0.0195(15) 0.0194(16) 0.0150(14) 0.000 -0.0028(12) 0.000 C11 0.0164(10) 0.0155(10) 0.0147(9) 0.0006(8) 0.0001(8) -0.0002(8) C12 0.0257(12) 0.0192(11) 0.0157(10) -0.0026(9) 0.0024(9) 0.0031(9) C13 0.0263(12) 0.0179(12) 0.0217(11) -0.0007(9) 0.0031(9) 0.0058(9) C14 0.0194(11) 0.0160(11) 0.0186(10) 0.0034(9) -0.0030(9) -0.0011(8) C15 0.0200(11) 0.0295(13) 0.0256(12) 0.0078(11) 0.0028(9) 0.0046(10) C16 0.0203(12) 0.0360(15) 0.0348(14) 0.0118(12) -0.0055(10) 0.0063(11) C17 0.0288(13) 0.0297(14) 0.0237(12) 0.0098(11) -0.0090(10) -0.0023(11) C18 0.0291(13) 0.0226(12) 0.0190(12) 0.0051(9) -0.0004(9) -0.0017(10) C19 0.0210(11) 0.0169(11) 0.0226(11) 0.0036(9) -0.0003(9) 0.0011(8) C21 0.0134(13) 0.0170(15) 0.0165(14) 0.000 0.0002(11) 0.000 C22 0.0181(15) 0.034(2) 0.0142(15) 0.000 -0.0049(12) 0.000 C23 0.0170(16) 0.032(2) 0.0182(16) 0.000 -0.0048(13) 0.000 C24 0.0173(15) 0.0188(16) 0.0177(15) 0.000 0.0045(12) 0.000 C25 0.0150(14) 0.0289(18) 0.0194(15) 0.000 0.0030(12) 0.000 C26 0.0217(17) 0.034(2) 0.0196(17) 0.000 0.0027(13) 0.000 C27 0.0257(19) 0.039(2) 0.0214(18) 0.000 0.0126(14) 0.000 C28 0.0164(16) 0.052(3) 0.034(2) 0.000 0.0096(15) 0.000 C29 0.0149(15) 0.045(2) 0.0230(17) 0.000 0.0000(13) 0.000 _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 1.914(2) . ? Re1 C1 1.914(2) 8_565 ? Re1 C2 1.926(3) . ? Re1 N3 2.191(3) . ? Re1 N1 2.1981(18) 8_565 ? Re1 N1 2.1981(18) . ? O1 C1 1.148(3) . ? O2 C2 1.149(4) . ? N1 C11 1.325(3) . ? N1 C12 1.387(3) . ? N2 C11 1.351(3) . ? N2 C13 1.380(3) . ? N2 C14 1.437(3) . ? N3 C21 1.328(4) . ? N3 C22 1.383(4) . ? N4 C21 1.347(4) . ? N4 C23 1.385(4) . ? N4 C24 1.438(4) . ? C12 C13 1.349(3) . ? C14 C19 1.378(3) . ? C14 C15 1.385(3) . ? C15 C16 1.390(3) . ? C16 C17 1.378(4) . ? C17 C18 1.389(3) . ? C18 C19 1.391(3) . ? C22 C23 1.353(4) . ? C24 C25 1.378(4) . ? C24 C29 1.396(4) . ? C25 C26 1.392(4) . ? C26 C27 1.385(5) . ? C27 C28 1.381(5) . ? C28 C29 1.379(5) . ? 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 C1 88.70(13) . 8_565 ? C1 Re1 C2 90.29(9) . . ? C1 Re1 C2 90.29(9) 8_565 . ? C1 Re1 N3 92.31(8) . . ? C1 Re1 N3 92.31(8) 8_565 . ? C2 Re1 N3 176.36(11) . . ? C1 Re1 N1 175.58(8) . 8_565 ? C1 Re1 N1 90.47(8) 8_565 8_565 ? C2 Re1 N1 94.06(8) . 8_565 ? N3 Re1 N1 83.38(6) . 8_565 ? C1 Re1 N1 90.47(8) . . ? C1 Re1 N1 175.58(8) 8_565 . ? C2 Re1 N1 94.06(8) . . ? N3 Re1 N1 83.38(6) . . ? N1 Re1 N1 90.02(9) 8_565 . ? C11 N1 C12 105.69(18) . . ? C11 N1 Re1 131.31(15) . . ? C12 N1 Re1 122.92(14) . . ? C11 N2 C13 107.46(18) . . ? C11 N2 C14 125.21(19) . . ? C13 N2 C14 126.90(19) . . ? C21 N3 C22 106.1(3) . . ? C21 N3 Re1 127.6(2) . . ? C22 N3 Re1 126.2(2) . . ? C21 N4 C23 107.5(3) . . ? C21 N4 C24 126.7(3) . . ? C23 N4 C24 125.8(3) . . ? O1 C1 Re1 178.3(2) . . ? O2 C2 Re1 178.5(3) . . ? N1 C11 N2 110.85(19) . . ? C13 C12 N1 109.8(2) . . ? C12 C13 N2 106.2(2) . . ? C19 C14 C15 121.4(2) . . ? C19 C14 N2 119.5(2) . . ? C15 C14 N2 119.1(2) . . ? C14 C15 C16 119.0(2) . . ? C17 C16 C15 120.3(2) . . ? C16 C17 C18 120.1(2) . . ? C17 C18 C19 120.0(2) . . ? C14 C19 C18 119.2(2) . . ? N3 C21 N4 110.7(3) . . ? C23 C22 N3 109.5(3) . . ? C22 C23 N4 106.2(3) . . ? C25 C24 C29 120.4(3) . . ? C25 C24 N4 120.8(3) . . ? C29 C24 N4 118.8(3) . . ? C24 C25 C26 119.4(3) . . ? C27 C26 C25 120.7(3) . . ? C28 C27 C26 119.2(3) . . ? C29 C28 C27 121.0(3) . . ? C28 C29 C24 119.3(3) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C11 H11 Br1 0.95 2.73 3.658(2) 166.9 . C19 H19 Br1 0.95 2.89 3.659(2) 139.0 . C21 H21 Br1 0.95 2.95 3.902(3) 179.0 1_554 C25 H25 Br1 0.95 2.99 3.938(3) 174.5 1_554 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 29.16 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.889 _refine_diff_density_min -1.059 _refine_diff_density_rms 0.095 #===END data_Compound_9_(li493) _database_code_depnum_ccdc_archive 'CCDC 642018' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H24 N6 O3 Re, N O3' _chemical_formula_sum 'C30 H24 N7 O6 Re' _chemical_formula_weight 764.76 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' 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 P21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.5765(14) _cell_length_b 24.603(3) _cell_length_c 11.3361(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.570(3) _cell_angle_gamma 90.00 _cell_volume 2949.6(6) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.722 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1504 _exptl_absorpt_coefficient_mu 4.176 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.812646 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 'SMART 1k' _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 34367 _diffrn_reflns_av_R_equivalents 0.0670 _diffrn_reflns_av_sigmaI/netI 0.1155 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 29.16 _reflns_number_total 15746 _reflns_number_gt 12480 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics X-Seed _computing_publication_material X-Seed _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^)+(0.0000P)^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 constr _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 -0.003(6) _refine_ls_number_reflns 15746 _refine_ls_number_parameters 793 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0707 _refine_ls_R_factor_gt 0.0467 _refine_ls_wR_factor_ref 0.0801 _refine_ls_wR_factor_gt 0.0733 _refine_ls_goodness_of_fit_ref 0.918 _refine_ls_restrained_S_all 0.918 _refine_ls_shift/su_max 0.038 _refine_ls_shift/su_mean 0.001 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 0.70555(2) 0.072033(10) 0.23300(2) 0.01356(7) Uani 1 1 d . . . Re2 Re 0.22284(3) -0.071993(9) -0.13419(2) 0.01283(7) Uani 1 1 d . . . O1 O 0.7294(5) 0.1955(2) 0.2361(5) 0.0236(13) Uani 1 1 d . . . O2 O 0.9871(5) 0.0638(2) 0.1760(4) 0.0259(12) Uani 1 1 d . . . O3 O 0.7516(6) 0.0764(3) 0.4999(5) 0.0397(15) Uani 1 1 d . . . O101 O 0.2452(5) -0.0478(2) -0.3993(5) 0.0271(13) Uani 1 1 d . . . O102 O 0.5091(5) -0.0550(2) -0.1160(5) 0.0295(13) Uani 1 1 d . . . O103 O 0.2793(6) -0.1924(2) -0.1786(5) 0.0337(14) Uani 1 1 d . . . O1N O 0.5365(5) 0.2851(2) -0.0738(5) 0.0321(14) Uani 1 1 d . . . O2N O 0.4907(5) 0.2201(2) 0.0461(5) 0.0315(14) Uani 1 1 d . . . O3N O 0.3731(6) 0.2925(2) 0.0386(5) 0.0387(15) Uani 1 1 d . . . O4N O 0.0410(6) 0.0291(2) -0.5760(6) 0.0469(17) Uani 1 1 d . . . O5N O -0.0079(6) 0.0223(2) -0.3921(5) 0.0337(14) Uani 1 1 d . . . O6N O -0.0325(5) -0.0464(2) -0.5087(4) 0.0210(11) Uani 1 1 d . . . N1 N 0.6652(5) 0.0685(3) 0.0433(5) 0.0145(12) Uani 1 1 d . . . N2 N 0.5863(6) 0.0850(2) -0.1331(5) 0.0191(14) Uani 1 1 d . . . N3 N 0.4991(5) 0.0790(2) 0.2568(5) 0.0135(12) Uani 1 1 d . . . N4 N 0.3120(5) 0.1175(2) 0.2762(5) 0.0173(13) Uani 1 1 d . . . N5 N 0.6815(6) -0.0169(3) 0.2248(5) 0.0157(14) Uani 1 1 d . . . N6 N 0.7232(6) -0.1039(2) 0.2468(5) 0.0150(13) Uani 1 1 d . . . N101 N 0.1797(6) 0.0135(2) -0.0985(5) 0.0156(13) Uani 1 1 d . . . N102 N 0.0838(6) 0.0929(2) -0.1010(5) 0.0159(13) Uani 1 1 d . . . N103 N 0.0165(6) -0.0860(2) -0.1410(5) 0.0171(14) Uani 1 1 d . . . N104 N -0.1753(5) -0.0968(2) -0.2139(5) 0.0160(12) Uani 1 1 d . . . N105 N 0.2056(6) -0.0818(2) 0.0577(5) 0.0179(13) Uani 1 1 d . . . N106 N 0.2151(6) -0.1171(2) 0.2358(5) 0.0180(13) Uani 1 1 d . . . N1N N 0.4667(6) 0.2661(2) 0.0048(5) 0.0223(15) Uani 1 1 d . . . N2N N 0.0013(6) 0.0020(2) -0.4921(5) 0.0199(13) Uani 1 1 d . . . C1 C 0.7209(6) 0.1489(3) 0.2335(6) 0.0146(17) Uani 1 1 d . . . C2 C 0.8805(7) 0.0673(3) 0.2006(6) 0.0167(15) Uani 1 1 d . . . C3 C 0.7345(6) 0.0737(3) 0.3975(7) 0.0217(16) Uani 1 1 d . . . C11 C 0.5817(7) 0.0970(3) -0.0179(6) 0.0185(16) Uani 1 1 d . . . H11 H 0.5255 0.1228 0.0154 0.022 Uiso 1 1 calc R . . C12 C 0.7276(7) 0.0372(3) -0.0380(6) 0.0207(17) Uani 1 1 d . . . H12 H 0.7947 0.0128 -0.0202 0.025 Uiso 1 1 calc R . . C13 C 0.6792(7) 0.0464(3) -0.1477(7) 0.0231(17) Uani 1 1 d . . . H13 H 0.7041 0.0297 -0.2193 0.028 Uiso 1 1 calc R . . C14 C 0.4996(8) 0.1053(3) -0.2216(6) 0.0256(17) Uani 1 1 d . . . C15 C 0.4465(7) 0.0693(4) -0.3006(6) 0.0325(18) Uani 1 1 d . . . H15 H 0.4686 0.0319 -0.2984 0.039 Uiso 1 1 calc R . . C16 C 0.3593(10) 0.0888(4) -0.3843(8) 0.047(3) Uani 1 1 d . . . H16 H 0.3240 0.0649 -0.4417 0.056 Uiso 1 1 calc R . . C17 C 0.3248(9) 0.1430(4) -0.3829(8) 0.045(2) Uani 1 1 d . . . H17 H 0.2637 0.1561 -0.4379 0.054 Uiso 1 1 calc R . . C18 C 0.3787(8) 0.1780(4) -0.3021(8) 0.040(2) Uani 1 1 d . . . H18 H 0.3549 0.2152 -0.3019 0.047 Uiso 1 1 calc R . . C19 C 0.4671(8) 0.1594(3) -0.2211(6) 0.0259(18) Uani 1 1 d . . . H19 H 0.5049 0.1836 -0.1659 0.031 Uiso 1 1 calc R . . C21 C 0.4344(6) 0.1251(3) 0.2498(6) 0.0140(14) Uani 1 1 d . . . H21 H 0.4701 0.1591 0.2288 0.017 Uiso 1 1 calc R . . C22 C 0.4117(7) 0.0404(3) 0.2900(6) 0.0201(17) Uani 1 1 d . . . H22 H 0.4297 0.0031 0.3031 0.024 Uiso 1 1 calc R . . C23 C 0.2968(7) 0.0638(3) 0.3010(6) 0.0189(16) Uani 1 1 d . . . H23 H 0.2204 0.0461 0.3220 0.023 Uiso 1 1 calc R . . C24 C 0.2152(6) 0.1592(3) 0.2739(6) 0.0159(15) Uani 1 1 d . . . C25 C 0.1088(7) 0.1521(3) 0.3453(6) 0.0203(16) Uani 1 1 d . . . H25 H 0.1018 0.1217 0.3966 0.024 Uiso 1 1 calc R . . C26 C 0.0150(7) 0.1908(3) 0.3383(6) 0.0230(17) Uani 1 1 d . . . H26 H -0.0581 0.1868 0.3855 0.028 Uiso 1 1 calc R . . C27 C 0.0242(7) 0.2358(3) 0.2635(6) 0.0232(17) Uani 1 1 d . . . H27 H -0.0425 0.2616 0.2586 0.028 Uiso 1 1 calc R . . C28 C 0.1323(7) 0.2421(3) 0.1969(7) 0.0219(16) Uani 1 1 d . . . H28 H 0.1407 0.2731 0.1476 0.026 Uiso 1 1 calc R . . C29 C 0.2280(7) 0.2039(3) 0.2010(6) 0.0180(15) Uani 1 1 d . . . H29 H 0.3015 0.2083 0.1544 0.022 Uiso 1 1 calc R . . C31 C 0.7555(7) -0.0530(3) 0.2794(6) 0.0188(17) Uani 1 1 d . . . H31 H 0.8216 -0.0441 0.3334 0.023 Uiso 1 1 calc R . . C32 C 0.6005(7) -0.0467(3) 0.1539(6) 0.0162(15) Uani 1 1 d . . . H32 H 0.5367 -0.0317 0.1041 0.019 Uiso 1 1 calc R . . C33 C 0.6252(7) -0.1004(3) 0.1656(6) 0.0191(16) Uani 1 1 d . . . H33 H 0.5838 -0.1296 0.1262 0.023 Uiso 1 1 calc R . . C34 C 0.7833(7) -0.1526(3) 0.2881(6) 0.0160(16) Uani 1 1 d . . . C35 C 0.8266(7) -0.1899(3) 0.2080(6) 0.0227(17) Uani 1 1 d . . . H35 H 0.8146 -0.1844 0.1257 0.027 Uiso 1 1 calc R . . C36 C 0.8885(8) -0.2360(3) 0.2500(7) 0.0253(18) Uani 1 1 d . . . H36 H 0.9205 -0.2617 0.1954 0.030 Uiso 1 1 calc R . . C37 C 0.9039(7) -0.2449(3) 0.3668(7) 0.0272(18) Uani 1 1 d . . . H37 H 0.9490 -0.2759 0.3937 0.033 Uiso 1 1 calc R . . C38 C 0.8539(7) -0.2086(3) 0.4475(7) 0.0255(17) Uani 1 1 d . . . H38 H 0.8603 -0.2158 0.5296 0.031 Uiso 1 1 calc R . . C39 C 0.7945(7) -0.1617(3) 0.4078(7) 0.0250(17) Uani 1 1 d . . . H39 H 0.7618 -0.1362 0.4624 0.030 Uiso 1 1 calc R . . C101 C 0.2343(6) -0.0577(2) -0.2994(7) 0.0158(16) Uani 1 1 d . . . C102 C 0.4002(8) -0.0610(3) -0.1215(6) 0.0184(18) Uani 1 1 d . . . C103 C 0.2575(7) -0.1468(3) -0.1636(6) 0.0202(17) Uani 1 1 d . . . C111 C 0.0802(7) 0.0407(3) -0.1363(6) 0.0165(16) Uani 1 1 d . . . H111 H 0.0139 0.0254 -0.1828 0.020 Uiso 1 1 calc R . . C112 C 0.2527(8) 0.0501(3) -0.0359(7) 0.0220(18) Uani 1 1 d . . . H112 H 0.3320 0.0423 0.0003 0.026 Uiso 1 1 calc R . . C113 C 0.1939(7) 0.0992(3) -0.0342(6) 0.0193(17) Uani 1 1 d . . . H113 H 0.2221 0.1312 0.0048 0.023 Uiso 1 1 calc R . . C114 C -0.0148(7) 0.1329(3) -0.1214(6) 0.0207(16) Uani 1 1 d . . . C115 C -0.0502(7) 0.1656(3) -0.0271(7) 0.0243(17) Uani 1 1 d . . . H115 H -0.0088 0.1630 0.0474 0.029 Uiso 1 1 calc R . . C116 C -0.1486(8) 0.2022(3) -0.0460(8) 0.031(2) Uani 1 1 d . . . H116 H -0.1743 0.2254 0.0164 0.037 Uiso 1 1 calc R . . C117 C -0.2089(7) 0.2054(3) -0.1536(8) 0.032(2) Uani 1 1 d . . . H117 H -0.2772 0.2300 -0.1650 0.038 Uiso 1 1 calc R . . C118 C -0.1694(8) 0.1724(3) -0.2459(8) 0.0304(19) Uani 1 1 d . . . H118 H -0.2100 0.1750 -0.3208 0.036 Uiso 1 1 calc R . . C119 C -0.0715(7) 0.1358(3) -0.2292(6) 0.0216(16) Uani 1 1 d . . . H119 H -0.0445 0.1132 -0.2920 0.026 Uiso 1 1 calc R . . C121 C -0.0547(6) -0.0827(2) -0.2361(6) 0.0156(15) Uani 1 1 d . . . H121 H -0.0250 -0.0719 -0.3113 0.019 Uiso 1 1 calc R . . C122 C -0.0619(7) -0.1038(3) -0.0527(6) 0.0203(16) Uani 1 1 d . . . H122 H -0.0368 -0.1104 0.0267 0.024 Uiso 1 1 calc R . . C123 C -0.1818(7) -0.1106(3) -0.0974(7) 0.0201(16) Uani 1 1 d . . . H123 H -0.2544 -0.1224 -0.0560 0.024 Uiso 1 1 calc R . . C124 C -0.2800(7) -0.0973(3) -0.2974(6) 0.0194(15) Uani 1 1 d . . . C125 C -0.2940(7) -0.0542(3) -0.3747(6) 0.0210(17) Uani 1 1 d . . . H125 H -0.2345 -0.0253 -0.3755 0.025 Uiso 1 1 calc R . . C126 C -0.3987(8) -0.0543(4) -0.4519(7) 0.033(2) Uani 1 1 d . . . H126 H -0.4114 -0.0253 -0.5061 0.039 Uiso 1 1 calc R . . C127 C -0.4815(8) -0.0966(4) -0.4480(8) 0.038(2) Uani 1 1 d . . . H127 H -0.5512 -0.0969 -0.5015 0.045 Uiso 1 1 calc R . . C128 C -0.4683(8) -0.1390(4) -0.3695(7) 0.038(2) Uani 1 1 d . . . H128 H -0.5292 -0.1674 -0.3680 0.045 Uiso 1 1 calc R . . C129 C -0.3649(7) -0.1401(3) -0.2923(7) 0.0265(19) Uani 1 1 d . . . H129 H -0.3532 -0.1691 -0.2380 0.032 Uiso 1 1 calc R . . C131 C 0.2476(7) -0.1234(3) 0.1226(6) 0.0188(16) Uani 1 1 d . . . H131 H 0.2942 -0.1533 0.0928 0.023 Uiso 1 1 calc R . . C132 C 0.1418(7) -0.0485(3) 0.1353(6) 0.0195(16) Uani 1 1 d . . . H132 H 0.1002 -0.0156 0.1141 0.023 Uiso 1 1 calc R . . C133 C 0.1472(7) -0.0693(3) 0.2446(6) 0.0226(15) Uani 1 1 d . . . H133 H 0.1117 -0.0542 0.3139 0.027 Uiso 1 1 calc R . . C134 C 0.2428(7) -0.1536(3) 0.3308(6) 0.0206(16) Uani 1 1 d . . . C135 C 0.1634(7) -0.1549(3) 0.4267(6) 0.0278(18) Uani 1 1 d . . . H135 H 0.0929 -0.1311 0.4305 0.033 Uiso 1 1 calc R . . C136 C 0.1875(9) -0.1913(4) 0.5173(8) 0.046(3) Uani 1 1 d . . . H136 H 0.1326 -0.1927 0.5830 0.055 Uiso 1 1 calc R . . C137 C 0.2903(9) -0.2255(3) 0.5129(7) 0.038(2) Uani 1 1 d . . . H137 H 0.3055 -0.2506 0.5752 0.046 Uiso 1 1 calc R . . C138 C 0.3712(10) -0.2234(3) 0.4186(7) 0.040(2) Uani 1 1 d . . . H138 H 0.4428 -0.2467 0.4163 0.048 Uiso 1 1 calc R . . C139 C 0.3478(8) -0.1872(3) 0.3267(7) 0.029(2) Uani 1 1 d . . . H139 H 0.4035 -0.1855 0.2616 0.034 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 0.01350(15) 0.01088(13) 0.01627(15) -0.00154(13) -0.00233(11) 0.00125(13) Re2 0.01342(15) 0.01180(13) 0.01328(14) -0.00115(13) 0.00017(11) 0.00040(13) O1 0.020(3) 0.014(3) 0.037(4) -0.004(2) -0.001(3) -0.003(2) O2 0.020(3) 0.029(3) 0.028(3) -0.005(2) 0.002(2) 0.002(2) O3 0.042(4) 0.050(4) 0.027(3) -0.012(4) -0.010(3) 0.005(4) O101 0.023(3) 0.040(3) 0.019(3) 0.005(3) 0.002(2) 0.003(3) O102 0.016(3) 0.043(4) 0.029(3) -0.003(3) -0.004(2) 0.000(2) O103 0.050(4) 0.014(3) 0.037(3) -0.009(2) 0.002(3) 0.005(3) O1N 0.035(4) 0.030(3) 0.032(3) 0.007(3) 0.012(3) 0.002(3) O2N 0.039(4) 0.020(3) 0.036(3) 0.009(3) 0.009(3) 0.011(3) O3N 0.049(4) 0.028(3) 0.040(4) 0.011(3) 0.023(3) 0.018(3) O4N 0.056(4) 0.033(3) 0.052(4) 0.020(3) 0.030(3) 0.007(3) O5N 0.051(4) 0.026(3) 0.023(3) -0.006(2) -0.015(3) 0.006(3) O6N 0.020(3) 0.027(3) 0.016(3) -0.002(2) 0.001(2) -0.008(2) N1 0.016(3) 0.009(3) 0.018(3) 0.001(3) 0.000(2) 0.002(3) N2 0.022(3) 0.022(3) 0.014(3) 0.000(2) -0.005(2) 0.001(2) N3 0.015(3) 0.007(3) 0.018(3) 0.000(2) -0.001(2) 0.003(2) N4 0.012(3) 0.022(3) 0.018(3) 0.001(3) 0.002(3) -0.001(3) N5 0.018(3) 0.019(3) 0.010(3) -0.009(3) -0.002(3) 0.004(3) N6 0.018(3) 0.014(3) 0.013(3) 0.001(2) -0.004(3) 0.001(2) N101 0.021(3) 0.014(3) 0.012(3) 0.004(2) 0.000(3) -0.001(2) N102 0.019(3) 0.010(3) 0.018(3) -0.002(2) 0.005(3) 0.003(2) N103 0.015(3) 0.020(3) 0.016(3) -0.002(2) -0.004(2) 0.006(2) N104 0.019(3) 0.021(3) 0.008(3) 0.000(2) 0.001(2) -0.003(2) N105 0.027(3) 0.013(3) 0.014(3) -0.002(2) 0.003(2) -0.001(2) N106 0.026(4) 0.020(3) 0.007(3) -0.005(2) 0.000(2) 0.003(3) N1N 0.030(4) 0.019(3) 0.018(3) -0.002(3) 0.004(3) 0.011(3) N2N 0.019(3) 0.024(3) 0.017(3) 0.006(3) -0.003(3) -0.001(3) C1 0.006(4) 0.022(4) 0.015(4) -0.002(3) -0.003(3) -0.005(3) C2 0.024(4) 0.014(3) 0.012(3) -0.006(3) -0.004(3) -0.003(3) C3 0.023(4) 0.011(3) 0.031(4) -0.008(4) -0.005(3) 0.008(4) C11 0.019(4) 0.016(3) 0.021(4) 0.000(3) -0.001(3) 0.001(3) C12 0.020(4) 0.019(4) 0.023(4) 0.004(3) -0.002(3) 0.004(3) C13 0.020(4) 0.015(4) 0.033(5) -0.006(3) 0.004(3) 0.009(3) C14 0.029(5) 0.032(4) 0.016(4) 0.002(3) 0.000(3) 0.000(4) C15 0.043(5) 0.029(4) 0.025(4) -0.002(4) -0.015(3) 0.001(5) C16 0.062(7) 0.044(6) 0.034(5) -0.006(4) -0.022(5) -0.005(5) C17 0.044(6) 0.044(6) 0.046(6) 0.004(5) -0.023(5) -0.004(5) C18 0.036(5) 0.039(5) 0.043(6) 0.008(4) -0.015(4) 0.008(4) C19 0.036(5) 0.020(4) 0.022(4) -0.002(3) -0.014(4) 0.003(3) C21 0.014(4) 0.011(3) 0.017(4) 0.000(3) 0.003(3) 0.002(3) C22 0.023(4) 0.013(4) 0.024(4) 0.005(3) 0.003(3) 0.001(3) C23 0.019(4) 0.016(4) 0.022(4) 0.000(3) -0.001(3) -0.004(3) C24 0.012(4) 0.014(3) 0.022(4) -0.005(3) 0.001(3) 0.006(3) C25 0.019(4) 0.022(4) 0.020(4) -0.003(3) -0.004(3) 0.001(3) C26 0.013(4) 0.035(4) 0.021(4) -0.011(3) 0.004(3) 0.002(3) C27 0.020(4) 0.028(4) 0.021(4) -0.010(3) -0.004(3) 0.009(3) C28 0.019(4) 0.020(4) 0.027(4) 0.001(3) -0.005(3) 0.002(3) C29 0.018(4) 0.019(4) 0.017(4) -0.007(3) 0.001(3) 0.002(3) C31 0.019(4) 0.025(4) 0.012(4) -0.002(3) -0.006(3) 0.004(3) C32 0.020(4) 0.016(4) 0.012(4) 0.001(3) -0.002(3) -0.002(3) C33 0.022(4) 0.016(4) 0.019(4) 0.004(3) -0.003(3) -0.005(3) C34 0.019(4) 0.010(3) 0.019(4) 0.006(3) 0.001(3) 0.001(3) C35 0.040(5) 0.016(3) 0.012(4) -0.001(3) 0.003(3) 0.008(3) C36 0.038(5) 0.012(3) 0.026(4) 0.002(3) 0.003(4) 0.006(3) C37 0.021(4) 0.022(4) 0.039(5) 0.004(4) -0.004(4) 0.002(3) C38 0.035(5) 0.021(4) 0.021(4) 0.001(3) -0.003(3) 0.005(3) C39 0.028(5) 0.025(4) 0.021(4) -0.005(3) 0.002(3) 0.004(3) C101 0.010(4) 0.005(3) 0.033(4) 0.003(3) 0.003(3) -0.004(2) C102 0.040(5) 0.008(4) 0.007(3) -0.003(3) 0.000(3) -0.004(3) C103 0.018(4) 0.031(5) 0.011(4) 0.001(3) -0.006(3) -0.005(3) C111 0.021(4) 0.016(4) 0.013(4) 0.001(3) -0.003(3) -0.001(3) C112 0.019(4) 0.021(4) 0.027(4) 0.001(3) -0.006(4) -0.002(3) C113 0.027(5) 0.011(3) 0.021(4) -0.009(3) -0.008(3) -0.001(3) C114 0.023(4) 0.011(3) 0.029(4) 0.003(3) 0.001(3) 0.004(3) C115 0.028(5) 0.020(4) 0.025(4) 0.003(3) 0.007(3) 0.001(3) C116 0.032(5) 0.018(4) 0.042(5) -0.001(4) 0.017(4) 0.002(3) C117 0.017(4) 0.022(4) 0.056(6) 0.007(4) 0.005(4) 0.006(3) C118 0.028(5) 0.026(4) 0.037(5) 0.004(4) -0.002(4) 0.006(3) C119 0.021(4) 0.016(4) 0.027(4) -0.002(3) 0.007(3) 0.002(3) C121 0.021(4) 0.012(4) 0.014(3) 0.001(3) 0.003(3) 0.001(3) C122 0.021(4) 0.026(4) 0.014(4) -0.001(3) 0.001(3) -0.009(3) C123 0.016(4) 0.029(4) 0.015(4) 0.004(3) 0.007(3) -0.005(3) C124 0.016(4) 0.031(4) 0.011(3) -0.003(3) 0.000(3) 0.003(3) C125 0.016(4) 0.030(4) 0.017(4) -0.008(3) 0.006(3) 0.001(3) C126 0.027(5) 0.048(6) 0.023(4) -0.015(4) -0.006(4) 0.017(4) C127 0.019(5) 0.059(6) 0.035(5) -0.014(5) -0.003(4) 0.003(4) C128 0.022(5) 0.058(6) 0.033(5) -0.014(5) 0.005(4) -0.010(4) C129 0.014(4) 0.034(4) 0.033(5) -0.013(4) 0.005(3) -0.007(3) C131 0.025(4) 0.016(3) 0.015(4) -0.004(3) -0.001(3) -0.004(3) C132 0.020(4) 0.024(4) 0.014(4) -0.001(3) 0.002(3) 0.001(3) C133 0.028(4) 0.023(4) 0.016(3) -0.013(4) 0.000(3) 0.006(4) C134 0.022(4) 0.021(4) 0.018(4) 0.001(3) -0.002(3) -0.006(3) C135 0.025(4) 0.038(5) 0.021(4) 0.014(4) 0.008(3) -0.003(4) C136 0.041(6) 0.066(7) 0.030(5) 0.021(5) 0.000(4) -0.019(5) C137 0.060(7) 0.031(5) 0.024(5) 0.007(4) -0.014(4) -0.027(5) C138 0.070(7) 0.028(4) 0.022(5) -0.001(4) -0.019(5) 0.005(4) C139 0.037(5) 0.026(4) 0.023(5) -0.004(4) 0.003(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 C3 1.887(7) . ? Re1 C2 1.893(7) . ? Re1 C1 1.899(8) . ? Re1 N1 2.190(5) . ? Re1 N5 2.205(6) . ? Re1 N3 2.209(6) . ? Re2 C102 1.899(8) . ? Re2 C103 1.906(8) . ? Re2 C101 1.910(8) . ? Re2 N101 2.191(6) . ? Re2 N105 2.199(5) . ? Re2 N103 2.210(6) . ? O1 C1 1.150(9) . ? O2 C2 1.168(8) . ? O3 C3 1.175(8) . ? O101 C101 1.166(8) . ? O102 C102 1.163(9) . ? O103 C103 1.158(9) . ? O1N N1N 1.254(8) . ? O2N N1N 1.250(7) . ? O3N N1N 1.246(8) . ? O4N N2N 1.236(7) . ? O5N N2N 1.243(7) . ? O6N N2N 1.258(7) . ? N1 C11 1.321(8) . ? N1 C12 1.375(9) . ? N2 C11 1.341(8) . ? N2 C13 1.377(8) . ? N2 C14 1.442(9) . ? N3 C21 1.326(8) . ? N3 C22 1.379(9) . ? N4 C21 1.345(9) . ? N4 C23 1.362(9) . ? N4 C24 1.449(8) . ? N5 C31 1.332(9) . ? N5 C32 1.380(9) . ? N6 C31 1.350(9) . ? N6 C33 1.382(9) . ? N6 C34 1.431(8) . ? N101 C111 1.316(9) . ? N101 C112 1.379(9) . ? N102 C111 1.346(8) . ? N102 C113 1.392(9) . ? N102 C114 1.450(8) . ? N103 C121 1.312(8) . ? N103 C122 1.378(9) . ? N104 C121 1.347(8) . ? N104 C123 1.366(9) . ? N104 C124 1.449(8) . ? N105 C131 1.333(8) . ? N105 C132 1.383(8) . ? N106 C131 1.340(8) . ? N106 C133 1.384(9) . ? N106 C134 1.429(9) . ? C12 C13 1.359(10) . ? C14 C19 1.372(10) . ? C14 C15 1.376(10) . ? C15 C16 1.401(11) . ? C16 C17 1.383(12) . ? C17 C18 1.378(12) . ? C18 C19 1.382(10) . ? C22 C23 1.351(10) . ? C24 C29 1.385(9) . ? C24 C25 1.403(10) . ? C25 C26 1.377(10) . ? C26 C27 1.399(10) . ? C27 C28 1.385(11) . ? C28 C29 1.381(9) . ? C32 C33 1.354(8) . ? C34 C35 1.374(9) . ? C34 C39 1.379(10) . ? C35 C36 1.390(9) . ? C36 C37 1.351(10) . ? C37 C38 1.386(10) . ? C38 C39 1.386(10) . ? C112 C113 1.357(9) . ? C114 C119 1.359(10) . ? C114 C115 1.392(10) . ? C115 C116 1.392(10) . ? C116 C117 1.373(11) . ? C117 C118 1.391(11) . ? C118 C119 1.384(10) . ? C122 C123 1.371(10) . ? C124 C125 1.383(10) . ? C124 C129 1.384(10) . ? C125 C126 1.405(10) . ? C126 C127 1.361(12) . ? C127 C128 1.378(12) . ? C128 C129 1.394(11) . ? C132 C133 1.341(9) . ? C134 C135 1.381(10) . ? C134 C139 1.387(11) . ? C135 C136 1.384(11) . ? C136 C137 1.376(13) . ? C137 C138 1.377(12) . ? C138 C139 1.391(11) . ? 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 C3 Re1 C2 92.5(3) . . ? C3 Re1 C1 87.8(3) . . ? C2 Re1 C1 88.7(3) . . ? C3 Re1 N1 177.8(3) . . ? C2 Re1 N1 89.3(2) . . ? C1 Re1 N1 93.4(3) . . ? C3 Re1 N5 94.6(3) . . ? C2 Re1 N5 92.5(3) . . ? C1 Re1 N5 177.2(3) . . ? N1 Re1 N5 84.1(2) . . ? C3 Re1 N3 91.6(2) . . ? C2 Re1 N3 175.7(2) . . ? C1 Re1 N3 90.4(3) . . ? N1 Re1 N3 86.5(2) . . ? N5 Re1 N3 88.2(2) . . ? C102 Re2 C103 87.7(3) . . ? C102 Re2 C101 88.6(3) . . ? C103 Re2 C101 89.6(3) . . ? C102 Re2 N101 93.2(3) . . ? C103 Re2 N101 178.9(3) . . ? C101 Re2 N101 91.1(2) . . ? C102 Re2 N105 91.8(3) . . ? C103 Re2 N105 94.9(3) . . ? C101 Re2 N105 175.5(2) . . ? N101 Re2 N105 84.4(2) . . ? C102 Re2 N103 177.5(3) . . ? C103 Re2 N103 92.0(3) . . ? C101 Re2 N103 93.8(2) . . ? N101 Re2 N103 87.1(2) . . ? N105 Re2 N103 85.8(2) . . ? C11 N1 C12 105.6(6) . . ? C11 N1 Re1 128.1(5) . . ? C12 N1 Re1 126.2(5) . . ? C11 N2 C13 107.6(6) . . ? C11 N2 C14 124.8(6) . . ? C13 N2 C14 127.3(6) . . ? C21 N3 C22 104.9(6) . . ? C21 N3 Re1 124.7(5) . . ? C22 N3 Re1 130.2(5) . . ? C21 N4 C23 107.2(6) . . ? C21 N4 C24 125.5(6) . . ? C23 N4 C24 127.3(6) . . ? C31 N5 C32 106.0(6) . . ? C31 N5 Re1 125.1(5) . . ? C32 N5 Re1 128.5(5) . . ? C31 N6 C33 108.1(6) . . ? C31 N6 C34 125.2(5) . . ? C33 N6 C34 126.7(6) . . ? C111 N101 C112 106.1(6) . . ? C111 N101 Re2 126.5(5) . . ? C112 N101 Re2 127.3(5) . . ? C111 N102 C113 106.8(6) . . ? C111 N102 C114 125.6(6) . . ? C113 N102 C114 127.4(6) . . ? C121 N103 C122 105.7(6) . . ? C121 N103 Re2 125.3(5) . . ? C122 N103 Re2 128.7(5) . . ? C121 N104 C123 107.5(6) . . ? C121 N104 C124 126.8(6) . . ? C123 N104 C124 125.7(6) . . ? C131 N105 C132 105.4(6) . . ? C131 N105 Re2 126.9(5) . . ? C132 N105 Re2 127.6(5) . . ? C131 N106 C133 107.7(6) . . ? C131 N106 C134 126.7(6) . . ? C133 N106 C134 125.6(6) . . ? O3N N1N O2N 121.0(6) . . ? O3N N1N O1N 119.9(6) . . ? O2N N1N O1N 119.1(6) . . ? O4N N2N O5N 121.1(7) . . ? O4N N2N O6N 119.5(6) . . ? O5N N2N O6N 119.3(6) . . ? O1 C1 Re1 178.7(6) . . ? O2 C2 Re1 177.3(6) . . ? O3 C3 Re1 178.0(7) . . ? N1 C11 N2 111.3(6) . . ? C13 C12 N1 109.9(6) . . ? C12 C13 N2 105.6(7) . . ? C19 C14 C15 121.7(7) . . ? C19 C14 N2 119.4(7) . . ? C15 C14 N2 118.8(7) . . ? C14 C15 C16 118.9(8) . . ? C17 C16 C15 119.6(8) . . ? C18 C17 C16 120.2(8) . . ? C17 C18 C19 120.5(8) . . ? C14 C19 C18 119.1(7) . . ? N3 C21 N4 111.4(6) . . ? C23 C22 N3 109.8(6) . . ? C22 C23 N4 106.6(6) . . ? C29 C24 C25 121.9(6) . . ? C29 C24 N4 120.0(6) . . ? C25 C24 N4 118.2(6) . . ? C26 C25 C24 117.5(7) . . ? C25 C26 C27 121.9(7) . . ? C28 C27 C26 118.8(7) . . ? C29 C28 C27 120.9(7) . . ? C28 C29 C24 119.0(7) . . ? N5 C31 N6 110.2(6) . . ? C33 C32 N5 110.1(7) . . ? C32 C33 N6 105.6(7) . . ? C35 C34 C39 121.0(6) . . ? C35 C34 N6 119.6(6) . . ? C39 C34 N6 119.4(6) . . ? C34 C35 C36 118.6(7) . . ? C37 C36 C35 121.3(7) . . ? C36 C37 C38 120.0(7) . . ? C37 C38 C39 119.7(7) . . ? C34 C39 C38 119.3(7) . . ? O101 C101 Re2 177.6(6) . . ? O102 C102 Re2 178.4(6) . . ? O103 C103 Re2 178.4(6) . . ? N101 C111 N102 111.6(6) . . ? C113 C112 N101 109.6(7) . . ? C112 C113 N102 105.9(6) . . ? C119 C114 C115 122.7(7) . . ? C119 C114 N102 119.3(6) . . ? C115 C114 N102 118.0(6) . . ? C116 C115 C114 117.6(7) . . ? C117 C116 C115 120.9(8) . . ? C116 C117 C118 119.6(7) . . ? C119 C118 C117 120.5(8) . . ? C114 C119 C118 118.7(7) . . ? N103 C121 N104 111.6(6) . . ? C123 C122 N103 109.3(6) . . ? N104 C123 C122 105.8(7) . . ? C125 C124 C129 122.9(7) . . ? C125 C124 N104 118.8(6) . . ? C129 C124 N104 118.2(6) . . ? C124 C125 C126 118.2(7) . . ? C127 C126 C125 119.0(8) . . ? C126 C127 C128 122.6(8) . . ? C127 C128 C129 119.6(8) . . ? C124 C129 C128 117.7(8) . . ? N105 C131 N106 110.7(6) . . ? C133 C132 N105 110.2(6) . . ? C132 C133 N106 106.0(6) . . ? C135 C134 C139 120.4(7) . . ? C135 C134 N106 119.1(7) . . ? C139 C134 N106 120.5(7) . . ? C134 C135 C136 119.4(8) . . ? C137 C136 C135 120.6(9) . . ? C136 C137 C138 120.2(8) . . ? C137 C138 C139 119.9(9) . . ? C134 C139 C138 119.6(8) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 29.16 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.281 _refine_diff_density_min -0.998 _refine_diff_density_rms 0.170 #===END