# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Coogan, Michael' _publ_contact_author_name 'Coogan, Michael' _publ_contact_author_email cooganmp@cf.ac.uk _publ_section_title ; Fluxionality and Lability in Rhenium 4\^a -Hydroxyterpyridine complexes: Evidence for an Associative Mechanism and Correlated Fluxionality and Lability. ; # Attachment '- C18H11BrN3O4Re.cif.CIF' data_C18H11BrN3O4Re _database_code_depnum_ccdc_archive 'CCDC 767719' #TrackingRef '- C18H11BrN3O4Re.cif.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Re hysroxy terpy Br ; _chemical_name_common ; Re hydroxy terpy Br ; _chemical_melting_point ? _chemical_formula_moiety 'C18 H18 Br N3 O4 Re' _chemical_formula_sum 'C18 H11 Br N3 O4 Re' _chemical_formula_weight 599.41 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.8310(2) _cell_length_b 8.8580(2) _cell_length_c 13.3900(3) _cell_angle_alpha 98.9970(10) _cell_angle_beta 92.2700(10) _cell_angle_gamma 102.5940(10) _cell_volume 892.70(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 yellow _exptl_crystal_colour needle _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.230 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 564 _exptl_absorpt_coefficient_mu 9.074 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1716 _exptl_absorpt_correction_T_max 0.2641 _exptl_absorpt_process_details ? _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 _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6291 _diffrn_reflns_av_R_equivalents 0.0302 _diffrn_reflns_av_sigmaI/netI 0.0459 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.62 _diffrn_reflns_theta_max 27.54 _reflns_number_total 4069 _reflns_number_gt 3872 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0248P)^2^+2.0391P] 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 0.0120(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4069 _refine_ls_number_parameters 246 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0301 _refine_ls_R_factor_gt 0.0282 _refine_ls_wR_factor_ref 0.0677 _refine_ls_wR_factor_gt 0.0667 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _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 C1 C 0.5516(6) 0.8136(5) 0.4679(3) 0.0202(8) Uani 1 1 d . . . H1 H 0.6197 0.8786 0.4293 0.024 Uiso 1 1 calc R . . C2 C 0.5795(6) 0.8508(5) 0.5728(3) 0.0204(8) Uani 1 1 d . . . H2 H 0.6645 0.9383 0.6034 0.024 Uiso 1 1 calc R . . C3 C 0.4780(5) 0.7547(5) 0.6311(3) 0.0188(8) Uani 1 1 d . . . H3 H 0.4933 0.7767 0.7015 0.023 Uiso 1 1 calc R . . C4 C 0.3529(5) 0.6248(5) 0.5819(3) 0.0186(8) Uani 1 1 d . . . H4 H 0.2832 0.5589 0.6194 0.022 Uiso 1 1 calc R . . C5 C 0.3323(5) 0.5936(5) 0.4761(3) 0.0141(7) Uani 1 1 d . . . C6 C 0.2087(5) 0.4545(5) 0.4192(3) 0.0150(8) Uani 1 1 d . . . C7 C 0.1004(5) 0.3504(5) 0.4690(3) 0.0169(8) Uani 1 1 d . . . H7 H 0.1010 0.3699 0.5394 0.020 Uiso 1 1 calc R . . C8 C -0.0099(5) 0.2160(5) 0.4132(3) 0.0174(8) Uani 1 1 d . . . C9 C -0.0044(6) 0.1897(5) 0.3079(3) 0.0197(8) Uani 1 1 d . . . H9 H -0.0759 0.1009 0.2686 0.024 Uiso 1 1 calc R . . C10 C 0.1093(5) 0.2980(5) 0.2627(3) 0.0187(8) Uani 1 1 d . . . C11 C 0.1251(6) 0.2598(5) 0.1514(3) 0.0190(8) Uani 1 1 d . . . C12 C -0.0193(6) 0.2410(6) 0.0834(3) 0.0260(10) Uani 1 1 d . . . H12 H -0.1267 0.2544 0.1058 0.031 Uiso 1 1 calc R . . C13 C 0.0017(7) 0.2013(6) -0.0193(3) 0.0319(11) Uani 1 1 d . . . H13 H -0.0909 0.1904 -0.0674 0.038 Uiso 1 1 calc R . . C14 C 0.1613(7) 0.1785(6) -0.0483(3) 0.0340(11) Uani 1 1 d . . . H14 H 0.1784 0.1502 -0.1164 0.041 Uiso 1 1 calc R . . C15 C 0.2962(7) 0.1982(6) 0.0254(4) 0.0313(11) Uani 1 1 d . . . H15 H 0.4041 0.1827 0.0048 0.038 Uiso 1 1 calc R . . C16 C 0.4964(6) 0.8313(5) 0.2288(3) 0.0218(9) Uani 1 1 d . . . C17 C 0.5591(6) 0.5440(5) 0.2229(3) 0.0231(9) Uani 1 1 d . . . C18 C 0.2914(6) 0.5863(5) 0.1141(3) 0.0239(9) Uani 1 1 d . . . O1 O -0.1185(4) 0.1096(4) 0.4558(2) 0.0233(6) Uani 1 1 d . . . H1A H -0.1122 0.1390 0.5173 0.035 Uiso 1 1 calc R . . O2 O 0.5748(5) 0.9501(4) 0.2125(3) 0.0372(9) Uani 1 1 d . . . O3 O 0.6736(4) 0.4887(4) 0.1996(2) 0.0296(7) Uani 1 1 d . . . O4 O 0.2560(5) 0.5627(4) 0.0286(2) 0.0370(9) Uani 1 1 d . . . N1 N 0.4312(4) 0.6888(4) 0.4193(2) 0.0165(7) Uani 1 1 d . . . N2 N 0.2140(4) 0.4322(4) 0.3163(2) 0.0154(7) Uani 1 1 d . . . N3 N 0.2813(5) 0.2382(5) 0.1247(3) 0.0248(8) Uani 1 1 d . . . Br1 Br 0.09344(6) 0.76123(5) 0.30082(3) 0.02059(11) Uani 1 1 d . . . Re1 Re 0.36640(2) 0.636529(18) 0.257025(10) 0.01675(9) 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 C1 0.019(2) 0.019(2) 0.023(2) 0.0063(16) 0.0055(16) 0.0014(16) C2 0.017(2) 0.016(2) 0.026(2) 0.0019(16) -0.0016(16) 0.0010(16) C3 0.020(2) 0.019(2) 0.0168(18) 0.0005(15) 0.0032(15) 0.0044(16) C4 0.018(2) 0.020(2) 0.0180(18) 0.0050(16) 0.0025(15) 0.0026(16) C5 0.0140(19) 0.0175(19) 0.0124(17) 0.0066(14) 0.0024(14) 0.0039(15) C6 0.0144(19) 0.0166(19) 0.0150(17) 0.0038(15) 0.0029(14) 0.0045(15) C7 0.0143(19) 0.019(2) 0.0171(18) 0.0053(15) 0.0035(14) 0.0010(16) C8 0.019(2) 0.018(2) 0.0172(18) 0.0076(15) 0.0045(15) 0.0061(16) C9 0.020(2) 0.021(2) 0.0179(19) 0.0040(16) 0.0038(15) 0.0024(16) C10 0.018(2) 0.020(2) 0.0186(19) 0.0036(16) 0.0024(15) 0.0054(16) C11 0.022(2) 0.019(2) 0.0150(18) 0.0026(15) 0.0038(15) 0.0025(16) C12 0.025(2) 0.032(3) 0.021(2) 0.0020(18) 0.0019(17) 0.009(2) C13 0.041(3) 0.035(3) 0.019(2) 0.0040(19) -0.0039(19) 0.010(2) C14 0.049(3) 0.036(3) 0.017(2) 0.0026(19) 0.011(2) 0.009(2) C15 0.032(3) 0.034(3) 0.028(2) 0.000(2) 0.0107(19) 0.007(2) C16 0.024(2) 0.019(2) 0.021(2) 0.0037(17) 0.0090(17) 0.0027(18) C17 0.021(2) 0.026(2) 0.0176(19) 0.0067(17) 0.0013(16) -0.0053(18) C18 0.032(2) 0.021(2) 0.020(2) 0.0079(17) 0.0046(17) 0.0042(19) O1 0.0235(16) 0.0221(16) 0.0214(14) 0.0062(12) 0.0044(12) -0.0032(13) O2 0.051(2) 0.0239(18) 0.0367(19) 0.0101(15) 0.0240(17) 0.0015(16) O3 0.0254(17) 0.043(2) 0.0274(16) 0.0142(15) 0.0132(13) 0.0155(16) O4 0.060(3) 0.036(2) 0.0167(15) 0.0087(14) 0.0039(15) 0.0123(18) N1 0.0147(17) 0.0181(17) 0.0155(15) 0.0022(13) 0.0016(13) 0.0014(13) N2 0.0168(17) 0.0162(17) 0.0140(15) 0.0056(13) 0.0043(12) 0.0029(13) N3 0.023(2) 0.026(2) 0.0218(17) 0.0019(15) 0.0052(14) 0.0005(16) Br1 0.0214(2) 0.0241(2) 0.01722(19) 0.00572(16) 0.00368(15) 0.00527(17) Re1 0.01895(12) 0.01742(12) 0.01389(11) 0.00500(6) 0.00585(6) 0.00167(7) _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 C1 N1 1.345(5) . ? C1 C2 1.389(6) . ? C1 H1 0.9300 . ? C2 C3 1.388(6) . ? C2 H2 0.9300 . ? C3 C4 1.393(6) . ? C3 H3 0.9300 . ? C4 C5 1.397(5) . ? C4 H4 0.9300 . ? C5 N1 1.360(5) . ? C5 C6 1.470(6) . ? C6 N2 1.365(5) . ? C6 C7 1.383(5) . ? C7 C8 1.394(6) . ? C7 H7 0.9300 . ? C8 O1 1.339(5) . ? C8 C9 1.396(5) . ? C9 C10 1.390(6) . ? C9 H9 0.9300 . ? C10 N2 1.365(5) . ? C10 C11 1.493(5) . ? C11 N3 1.333(6) . ? C11 C12 1.386(6) . ? C12 C13 1.391(6) . ? C12 H12 0.9300 . ? C13 C14 1.370(7) . ? C13 H13 0.9300 . ? C14 C15 1.379(7) . ? C14 H14 0.9300 . ? C15 N3 1.338(6) . ? C15 H15 0.9300 . ? C16 O2 1.154(5) . ? C16 Re1 1.904(4) . ? C17 O3 1.144(6) . ? C17 Re1 1.906(5) . ? C18 O4 1.143(5) . ? C18 Re1 1.933(4) . ? O1 H1A 0.8200 . ? N1 Re1 2.165(3) . ? N2 Re1 2.216(3) . ? Br1 Re1 2.6570(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 N1 C1 C2 123.5(4) . . ? N1 C1 H1 118.3 . . ? C2 C1 H1 118.3 . . ? C3 C2 C1 118.6(4) . . ? C3 C2 H2 120.7 . . ? C1 C2 H2 120.7 . . ? C2 C3 C4 118.6(4) . . ? C2 C3 H3 120.7 . . ? C4 C3 H3 120.7 . . ? C3 C4 C5 119.8(4) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? N1 C5 C4 121.3(4) . . ? N1 C5 C6 116.0(3) . . ? C4 C5 C6 122.7(3) . . ? N2 C6 C7 122.9(4) . . ? N2 C6 C5 116.0(3) . . ? C7 C6 C5 121.0(3) . . ? C6 C7 C8 119.6(4) . . ? C6 C7 H7 120.2 . . ? C8 C7 H7 120.2 . . ? O1 C8 C7 123.2(3) . . ? O1 C8 C9 118.5(4) . . ? C7 C8 C9 118.4(4) . . ? C10 C9 C8 119.1(4) . . ? C10 C9 H9 120.4 . . ? C8 C9 H9 120.4 . . ? N2 C10 C9 123.0(4) . . ? N2 C10 C11 118.8(4) . . ? C9 C10 C11 118.0(4) . . ? N3 C11 C12 124.2(4) . . ? N3 C11 C10 115.5(4) . . ? C12 C11 C10 120.3(4) . . ? C11 C12 C13 117.9(4) . . ? C11 C12 H12 121.1 . . ? C13 C12 H12 121.1 . . ? C14 C13 C12 118.9(4) . . ? C14 C13 H13 120.6 . . ? C12 C13 H13 120.6 . . ? C13 C14 C15 118.8(4) . . ? C13 C14 H14 120.6 . . ? C15 C14 H14 120.6 . . ? N3 C15 C14 123.9(5) . . ? N3 C15 H15 118.0 . . ? C14 C15 H15 118.0 . . ? O2 C16 Re1 179.4(4) . . ? O3 C17 Re1 178.0(4) . . ? O4 C18 Re1 175.9(4) . . ? C8 O1 H1A 109.5 . . ? C1 N1 C5 118.1(3) . . ? C1 N1 Re1 125.0(3) . . ? C5 N1 Re1 116.7(2) . . ? C10 N2 C6 116.9(3) . . ? C10 N2 Re1 128.1(3) . . ? C6 N2 Re1 114.5(3) . . ? C11 N3 C15 116.4(4) . . ? C16 Re1 C17 89.63(19) . . ? C16 Re1 C18 86.34(19) . . ? C17 Re1 C18 86.58(19) . . ? C16 Re1 N1 96.10(16) . . ? C17 Re1 N1 96.62(15) . . ? C18 Re1 N1 175.97(16) . . ? C16 Re1 N2 170.18(15) . . ? C17 Re1 N2 95.33(16) . . ? C18 Re1 N2 102.38(16) . . ? N1 Re1 N2 74.94(13) . . ? C16 Re1 Br1 90.91(13) . . ? C17 Re1 Br1 178.67(13) . . ? C18 Re1 Br1 92.24(14) . . ? N1 Re1 Br1 84.53(9) . . ? N2 Re1 Br1 84.31(9) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 -0.2(6) . . . . ? C1 C2 C3 C4 0.2(6) . . . . ? C2 C3 C4 C5 0.1(6) . . . . ? C3 C4 C5 N1 -0.6(6) . . . . ? C3 C4 C5 C6 177.0(4) . . . . ? N1 C5 C6 N2 3.4(5) . . . . ? C4 C5 C6 N2 -174.4(4) . . . . ? N1 C5 C6 C7 -179.4(4) . . . . ? C4 C5 C6 C7 2.9(6) . . . . ? N2 C6 C7 C8 -0.1(6) . . . . ? C5 C6 C7 C8 -177.2(4) . . . . ? C6 C7 C8 O1 180.0(4) . . . . ? C6 C7 C8 C9 1.2(6) . . . . ? O1 C8 C9 C10 -179.2(4) . . . . ? C7 C8 C9 C10 -0.3(6) . . . . ? C8 C9 C10 N2 -1.6(6) . . . . ? C8 C9 C10 C11 174.3(4) . . . . ? N2 C10 C11 N3 61.8(5) . . . . ? C9 C10 C11 N3 -114.2(4) . . . . ? N2 C10 C11 C12 -121.4(5) . . . . ? C9 C10 C11 C12 62.5(6) . . . . ? N3 C11 C12 C13 -1.9(7) . . . . ? C10 C11 C12 C13 -178.3(4) . . . . ? C11 C12 C13 C14 1.8(7) . . . . ? C12 C13 C14 C15 -1.0(8) . . . . ? C13 C14 C15 N3 0.2(8) . . . . ? C2 C1 N1 C5 -0.3(6) . . . . ? C2 C1 N1 Re1 174.4(3) . . . . ? C4 C5 N1 C1 0.7(6) . . . . ? C6 C5 N1 C1 -177.1(4) . . . . ? C4 C5 N1 Re1 -174.4(3) . . . . ? C6 C5 N1 Re1 7.8(4) . . . . ? C9 C10 N2 C6 2.6(6) . . . . ? C11 C10 N2 C6 -173.3(3) . . . . ? C9 C10 N2 Re1 -168.2(3) . . . . ? C11 C10 N2 Re1 15.9(5) . . . . ? C7 C6 N2 C10 -1.7(6) . . . . ? C5 C6 N2 C10 175.5(3) . . . . ? C7 C6 N2 Re1 170.4(3) . . . . ? C5 C6 N2 Re1 -12.4(4) . . . . ? C12 C11 N3 C15 1.0(7) . . . . ? C10 C11 N3 C15 177.7(4) . . . . ? C14 C15 N3 C11 -0.2(7) . . . . ? O2 C16 Re1 C17 -132(49) . . . . ? O2 C16 Re1 C18 141(49) . . . . ? O2 C16 Re1 N1 -36(49) . . . . ? O2 C16 Re1 N2 -12(50) . . . . ? O2 C16 Re1 Br1 49(49) . . . . ? O3 C17 Re1 C16 -71(11) . . . . ? O3 C17 Re1 C18 16(11) . . . . ? O3 C17 Re1 N1 -167(11) . . . . ? O3 C17 Re1 N2 118(11) . . . . ? O3 C17 Re1 Br1 43(16) . . . . ? O4 C18 Re1 C16 26(6) . . . . ? O4 C18 Re1 C17 -64(6) . . . . ? O4 C18 Re1 N1 153(5) . . . . ? O4 C18 Re1 N2 -159(6) . . . . ? O4 C18 Re1 Br1 116(6) . . . . ? C1 N1 Re1 C16 -9.5(4) . . . . ? C5 N1 Re1 C16 165.2(3) . . . . ? C1 N1 Re1 C17 80.8(4) . . . . ? C5 N1 Re1 C17 -104.4(3) . . . . ? C1 N1 Re1 C18 -137(2) . . . . ? C5 N1 Re1 C18 38(2) . . . . ? C1 N1 Re1 N2 174.6(4) . . . . ? C5 N1 Re1 N2 -10.7(3) . . . . ? C1 N1 Re1 Br1 -99.9(3) . . . . ? C5 N1 Re1 Br1 74.9(3) . . . . ? C10 N2 Re1 C16 158.6(9) . . . . ? C6 N2 Re1 C16 -12.4(10) . . . . ? C10 N2 Re1 C17 -81.3(4) . . . . ? C6 N2 Re1 C17 107.7(3) . . . . ? C10 N2 Re1 C18 6.4(4) . . . . ? C6 N2 Re1 C18 -164.6(3) . . . . ? C10 N2 Re1 N1 -176.7(4) . . . . ? C6 N2 Re1 N1 12.3(3) . . . . ? C10 N2 Re1 Br1 97.4(3) . . . . ? C6 N2 Re1 Br1 -73.6(3) . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.401 _refine_diff_density_min -1.491 _refine_diff_density_rms 0.166 # Attachment '- C18H11ClN3O4Re.CIF' data_C18H11ClN3O4Re _database_code_depnum_ccdc_archive 'CCDC 767720' #TrackingRef '- C18H11ClN3O4Re.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Re terpy Cl ; _chemical_name_common ; Re terpy Cl ; _chemical_melting_point ? _chemical_formula_moiety C18H11ClN3O4Re _chemical_formula_sum 'C18 H11 Cl N3 O4 Re' _chemical_formula_weight 554.95 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' Cl Cl 0.1484 0.1585 '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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.5227(2) _cell_length_b 10.4890(3) _cell_length_c 13.3433(4) _cell_angle_alpha 100.6910(10) _cell_angle_beta 92.6110(10) _cell_angle_gamma 100.2530(10) _cell_volume 879.81(5) _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 needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.095 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 528 _exptl_absorpt_coefficient_mu 7.088 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.3314 _exptl_absorpt_correction_T_max 0.3314 _exptl_absorpt_process_details ? _exptl_special_details ; Absolute value of parameter shift to su high at 0.3 but refinement stable at these values ; _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 _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13815 _diffrn_reflns_av_R_equivalents 0.1758 _diffrn_reflns_av_sigmaI/netI 0.1098 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 27.46 _reflns_number_total 4013 _reflns_number_gt 3685 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0863P)^2^+1.1655P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4013 _refine_ls_number_parameters 248 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0615 _refine_ls_R_factor_gt 0.0565 _refine_ls_wR_factor_ref 0.1469 _refine_ls_wR_factor_gt 0.1416 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.301 _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 0.71126(4) 0.87235(2) 0.741086(19) 0.01268(14) Uani 1 1 d . . . Cl1 Cl 0.3457(3) 0.75347(19) 0.67608(15) 0.0174(4) Uani 1 1 d . . . O2 O 1.1564(9) 1.0115(6) 0.8218(5) 0.0266(14) Uani 1 1 d . . . O4 O 0.6104(10) 1.1504(6) 0.7786(5) 0.0260(14) Uani 1 1 d . . . N5 N 0.7514(10) 0.8589(7) 0.5806(5) 0.0157(13) Uani 1 1 d . . . O6 O 0.6005(11) 0.8654(7) 0.9629(5) 0.0319(15) Uani 1 1 d . . . N7 N 0.7841(10) 0.6734(6) 0.6883(5) 0.0129(13) Uani 1 1 d . . . C8 C 0.6472(13) 0.8653(9) 0.8799(7) 0.0198(17) Uani 1 1 d . . . C9 C 0.9906(13) 0.9572(8) 0.7907(6) 0.0184(16) Uani 1 1 d . . . C10 C 0.7956(11) 0.5822(8) 0.7455(6) 0.0138(14) Uani 1 1 d . . . C11 C 0.7634(12) 0.7384(7) 0.5247(6) 0.0153(14) Uani 1 1 d . . . C12 C 0.6415(13) 1.0436(8) 0.7650(6) 0.0205(17) Uani 1 1 d . . . C13 C 0.7713(11) 0.7174(8) 0.4188(6) 0.0167(15) Uani 1 1 d . . . H13 H 0.7852 0.6351 0.3825 0.020 Uiso 1 1 calc R . . C14 C 0.8459(12) 0.6211(8) 0.8584(6) 0.0170(16) Uani 1 1 d . . . C15 C 0.7765(11) 0.4472(7) 0.7025(6) 0.0149(14) Uani 1 1 d . . . H15 H 0.7801 0.3856 0.7442 0.018 Uiso 1 1 calc R . . C16 C 0.7534(11) 0.5030(7) 0.5372(6) 0.0154(14) Uani 1 1 d . . . H16 H 0.7445 0.4797 0.4662 0.018 Uiso 1 1 calc R . . C17 C 0.7679(11) 0.6333(7) 0.5845(6) 0.0146(14) Uani 1 1 d . . . N18 N 0.7103(11) 0.5638(8) 0.9167(6) 0.0242(15) Uani 1 1 d . . . C19 C 0.7469(12) 0.9422(7) 0.4244(6) 0.0171(15) Uani 1 1 d . . . H19 H 0.7416 1.0125 0.3914 0.020 Uiso 1 1 calc R . . C20 C 0.7434(12) 0.9593(7) 0.5288(6) 0.0169(15) Uani 1 1 d . . . H20 H 0.7354 1.0424 0.5658 0.020 Uiso 1 1 calc R . . C21 C 1.0321(13) 0.7065(7) 0.8972(6) 0.0192(16) Uani 1 1 d . . . H21 H 1.1221 0.7434 0.8537 0.023 Uiso 1 1 calc R . . C22 C 0.9404(14) 0.6798(9) 1.0636(6) 0.0235(18) Uani 1 1 d . . . H22 H 0.9677 0.6991 1.1343 0.028 Uiso 1 1 calc R . . C23 C 0.7584(12) 0.8178(8) 0.3686(6) 0.0198(16) Uani 1 1 d . . . H23 H 0.7572 0.8035 0.2977 0.024 Uiso 1 1 calc R . . C24 C 1.0807(14) 0.7355(9) 1.0019(7) 0.0252(18) Uani 1 1 d . . . H24 H 1.2052 0.7912 1.0303 0.030 Uiso 1 1 calc R . . C25 C 0.7570(15) 0.5943(9) 1.0183(7) 0.0271(18) Uani 1 1 d . . . H25 H 0.6636 0.5570 1.0602 0.033 Uiso 1 1 calc R . . O1 O 0.7345(9) 0.2776(5) 0.5550(5) 0.0186(11) Uani 1 1 d . . . C2 C 0.7520(11) 0.4070(7) 0.5960(6) 0.0159(15) Uani 1 1 d . . . H1 H 0.692(12) 0.271(7) 0.494(6) 0.000(17) Uiso 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 0.0109(2) 0.01089(19) 0.0144(2) 0.00091(13) -0.00227(12) -0.00034(12) Cl1 0.0119(9) 0.0173(9) 0.0201(9) 0.0008(7) -0.0009(7) -0.0010(7) O2 0.015(3) 0.028(3) 0.030(3) 0.000(3) -0.002(2) -0.005(2) O4 0.028(3) 0.013(3) 0.038(4) 0.005(3) -0.005(3) 0.008(2) N5 0.008(3) 0.019(3) 0.018(3) 0.004(3) -0.003(2) -0.001(2) O6 0.039(4) 0.034(4) 0.021(3) 0.001(3) 0.007(3) 0.009(3) N7 0.015(3) 0.007(3) 0.015(3) -0.003(2) -0.001(2) 0.002(2) C8 0.013(4) 0.026(4) 0.019(4) 0.004(3) -0.004(3) 0.002(3) C9 0.019(4) 0.018(4) 0.020(4) 0.010(3) 0.002(3) 0.001(3) C10 0.007(3) 0.017(4) 0.017(4) 0.004(3) -0.004(3) 0.001(3) C11 0.011(4) 0.014(3) 0.018(4) 0.001(3) -0.002(3) -0.001(3) C12 0.015(4) 0.024(4) 0.018(4) -0.003(3) -0.008(3) 0.001(3) C13 0.011(4) 0.024(4) 0.016(4) 0.003(3) 0.002(3) 0.007(3) C14 0.010(3) 0.020(4) 0.025(4) 0.010(3) 0.002(3) 0.005(3) C15 0.005(3) 0.018(3) 0.021(4) 0.004(3) -0.001(3) 0.001(3) C16 0.013(3) 0.018(4) 0.013(3) 0.001(3) -0.004(3) 0.001(3) C17 0.010(3) 0.012(3) 0.019(4) 0.003(3) -0.006(3) -0.005(3) N18 0.017(3) 0.030(4) 0.022(4) 0.008(3) 0.001(3) -0.006(3) C19 0.018(4) 0.016(3) 0.019(4) 0.009(3) 0.002(3) 0.002(3) C20 0.017(4) 0.010(3) 0.027(4) 0.010(3) 0.000(3) 0.003(3) C21 0.022(4) 0.014(3) 0.018(4) 0.001(3) -0.002(3) -0.004(3) C22 0.027(5) 0.037(5) 0.005(3) 0.000(3) -0.003(3) 0.008(4) C23 0.013(4) 0.028(4) 0.017(4) 0.006(3) 0.003(3) 0.000(3) C24 0.024(5) 0.026(4) 0.022(4) -0.001(3) -0.005(3) 0.001(3) C25 0.031(5) 0.032(5) 0.019(4) 0.012(4) 0.008(4) 0.000(4) O1 0.021(3) 0.010(2) 0.021(3) 0.000(2) -0.006(2) 0.000(2) C2 0.009(3) 0.008(3) 0.027(4) -0.001(3) -0.003(3) -0.003(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re1 C12 1.905(8) . ? Re1 C9 1.909(8) . ? Re1 C8 1.929(9) . ? Re1 N5 2.151(7) . ? Re1 N7 2.217(6) . ? Re1 Cl1 2.5190(19) . ? O2 C9 1.148(10) . ? O4 C12 1.156(10) . ? N5 C11 1.360(10) . ? N5 C20 1.370(10) . ? O6 C8 1.162(11) . ? N7 C10 1.340(10) . ? N7 C17 1.364(10) . ? C10 C15 1.407(10) . ? C10 C14 1.491(11) . ? C11 C13 1.394(11) . ? C11 C17 1.479(10) . ? C13 C23 1.361(11) . ? C13 H13 0.9300 . ? C14 N18 1.340(10) . ? C14 C21 1.389(11) . ? C15 C2 1.398(11) . ? C15 H15 0.9300 . ? C16 C17 1.379(10) . ? C16 C2 1.386(11) . ? C16 H16 0.9300 . ? N18 C25 1.341(11) . ? C19 C20 1.373(11) . ? C19 C23 1.394(11) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C21 C24 1.384(11) . ? C21 H21 0.9300 . ? C22 C24 1.383(13) . ? C22 C25 1.397(13) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? O1 C2 1.348(8) . ? O1 H1 0.84(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C12 Re1 C9 87.1(3) . . ? C12 Re1 C8 86.8(4) . . ? C9 Re1 C8 89.2(3) . . ? C12 Re1 N5 96.7(3) . . ? C9 Re1 N5 97.3(3) . . ? C8 Re1 N5 172.8(3) . . ? C12 Re1 N7 171.3(3) . . ? C9 Re1 N7 96.0(3) . . ? C8 Re1 N7 101.4(3) . . ? N5 Re1 N7 74.9(3) . . ? C12 Re1 Cl1 94.7(2) . . ? C9 Re1 Cl1 178.2(2) . . ? C8 Re1 Cl1 90.5(3) . . ? N5 Re1 Cl1 82.92(18) . . ? N7 Re1 Cl1 82.35(18) . . ? C11 N5 C20 117.5(7) . . ? C11 N5 Re1 117.5(5) . . ? C20 N5 Re1 124.6(6) . . ? C10 N7 C17 117.8(6) . . ? C10 N7 Re1 126.3(5) . . ? C17 N7 Re1 114.1(5) . . ? O6 C8 Re1 176.2(7) . . ? O2 C9 Re1 178.0(7) . . ? N7 C10 C15 122.4(7) . . ? N7 C10 C14 121.0(7) . . ? C15 C10 C14 116.5(6) . . ? N5 C11 C13 121.7(7) . . ? N5 C11 C17 115.2(7) . . ? C13 C11 C17 123.1(7) . . ? O4 C12 Re1 176.2(8) . . ? C23 C13 C11 119.8(7) . . ? C23 C13 H13 120.1 . . ? C11 C13 H13 120.1 . . ? N18 C14 C21 123.8(8) . . ? N18 C14 C10 116.6(7) . . ? C21 C14 C10 119.6(7) . . ? C2 C15 C10 119.0(7) . . ? C2 C15 H15 120.5 . . ? C10 C15 H15 120.5 . . ? C17 C16 C2 119.7(7) . . ? C17 C16 H16 120.1 . . ? C2 C16 H16 120.1 . . ? N7 C17 C16 122.7(7) . . ? N7 C17 C11 115.8(6) . . ? C16 C17 C11 121.6(7) . . ? C14 N18 C25 117.3(7) . . ? C20 C19 C23 118.8(7) . . ? C20 C19 H19 120.6 . . ? C23 C19 H19 120.6 . . ? N5 C20 C19 122.6(7) . . ? N5 C20 H20 118.7 . . ? C19 C20 H20 118.7 . . ? C24 C21 C14 118.5(8) . . ? C24 C21 H21 120.7 . . ? C14 C21 H21 120.7 . . ? C24 C22 C25 119.2(7) . . ? C24 C22 H22 120.4 . . ? C25 C22 H22 120.4 . . ? C13 C23 C19 119.5(7) . . ? C13 C23 H23 120.3 . . ? C19 C23 H23 120.3 . . ? C22 C24 C21 118.6(8) . . ? C22 C24 H24 120.7 . . ? C21 C24 H24 120.7 . . ? N18 C25 C22 122.6(8) . . ? N18 C25 H25 118.7 . . ? C22 C25 H25 118.7 . . ? C2 O1 H1 105(5) . . ? O1 C2 C16 122.9(7) . . ? O1 C2 C15 118.9(7) . . ? C16 C2 C15 118.3(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C12 Re1 N5 C11 -167.2(6) . . . . ? C9 Re1 N5 C11 104.9(6) . . . . ? C8 Re1 N5 C11 -49(2) . . . . ? N7 Re1 N5 C11 10.7(5) . . . . ? Cl1 Re1 N5 C11 -73.3(5) . . . . ? C12 Re1 N5 C20 5.6(7) . . . . ? C9 Re1 N5 C20 -82.3(6) . . . . ? C8 Re1 N5 C20 124(2) . . . . ? N7 Re1 N5 C20 -176.6(7) . . . . ? Cl1 Re1 N5 C20 99.5(6) . . . . ? C12 Re1 N7 C10 -164.6(17) . . . . ? C9 Re1 N7 C10 85.1(7) . . . . ? C8 Re1 N7 C10 -5.2(7) . . . . ? N5 Re1 N7 C10 -178.9(7) . . . . ? Cl1 Re1 N7 C10 -94.2(6) . . . . ? C12 Re1 N7 C17 0(2) . . . . ? C9 Re1 N7 C17 -110.4(6) . . . . ? C8 Re1 N7 C17 159.3(5) . . . . ? N5 Re1 N7 C17 -14.4(5) . . . . ? Cl1 Re1 N7 C17 70.3(5) . . . . ? C12 Re1 C8 O6 31(12) . . . . ? C9 Re1 C8 O6 118(12) . . . . ? N5 Re1 C8 O6 -88(13) . . . . ? N7 Re1 C8 O6 -146(12) . . . . ? Cl1 Re1 C8 O6 -63(12) . . . . ? C12 Re1 C9 O2 16(21) . . . . ? C8 Re1 C9 O2 -71(21) . . . . ? N5 Re1 C9 O2 112(21) . . . . ? N7 Re1 C9 O2 -172(21) . . . . ? Cl1 Re1 C9 O2 -150(16) . . . . ? C17 N7 C10 C15 -4.7(11) . . . . ? Re1 N7 C10 C15 159.3(5) . . . . ? C17 N7 C10 C14 170.6(7) . . . . ? Re1 N7 C10 C14 -25.4(10) . . . . ? C20 N5 C11 C13 1.1(11) . . . . ? Re1 N5 C11 C13 174.4(6) . . . . ? C20 N5 C11 C17 -179.0(7) . . . . ? Re1 N5 C11 C17 -5.7(8) . . . . ? C9 Re1 C12 O4 29(11) . . . . ? C8 Re1 C12 O4 118(11) . . . . ? N5 Re1 C12 O4 -68(11) . . . . ? N7 Re1 C12 O4 -82(11) . . . . ? Cl1 Re1 C12 O4 -152(11) . . . . ? N5 C11 C13 C23 -2.6(12) . . . . ? C17 C11 C13 C23 177.5(7) . . . . ? N7 C10 C14 N18 125.4(8) . . . . ? C15 C10 C14 N18 -59.0(9) . . . . ? N7 C10 C14 C21 -58.4(10) . . . . ? C15 C10 C14 C21 117.2(8) . . . . ? N7 C10 C15 C2 2.4(11) . . . . ? C14 C10 C15 C2 -173.2(7) . . . . ? C10 N7 C17 C16 3.1(11) . . . . ? Re1 N7 C17 C16 -162.8(6) . . . . ? C10 N7 C17 C11 -177.8(7) . . . . ? Re1 N7 C17 C11 16.3(8) . . . . ? C2 C16 C17 N7 0.9(11) . . . . ? C2 C16 C17 C11 -178.1(7) . . . . ? N5 C11 C17 N7 -7.4(10) . . . . ? C13 C11 C17 N7 172.5(7) . . . . ? N5 C11 C17 C16 171.7(7) . . . . ? C13 C11 C17 C16 -8.4(12) . . . . ? C21 C14 N18 C25 1.7(12) . . . . ? C10 C14 N18 C25 177.7(7) . . . . ? C11 N5 C20 C19 0.1(11) . . . . ? Re1 N5 C20 C19 -172.6(6) . . . . ? C23 C19 C20 N5 0.2(12) . . . . ? N18 C14 C21 C24 -0.5(12) . . . . ? C10 C14 C21 C24 -176.5(7) . . . . ? C11 C13 C23 C19 2.9(12) . . . . ? C20 C19 C23 C13 -1.7(11) . . . . ? C25 C22 C24 C21 1.4(13) . . . . ? C14 C21 C24 C22 -1.0(12) . . . . ? C14 N18 C25 C22 -1.3(13) . . . . ? C24 C22 C25 N18 -0.2(14) . . . . ? C17 C16 C2 O1 178.8(7) . . . . ? C17 C16 C2 C15 -3.2(11) . . . . ? C10 C15 C2 O1 179.8(6) . . . . ? C10 C15 C2 C16 1.7(10) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 3.755 _refine_diff_density_min -4.883 _refine_diff_density_rms 0.355 # Attachment '- C19H12BrN2O4Re.CIF' data_C19H12BrN2O4Re _database_code_depnum_ccdc_archive 'CCDC 767721' #TrackingRef '- C19H12BrN2O4Re.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Re hydroxy bipy Ph ; _chemical_name_common ; Re hydroxy bipy Ph ; _chemical_melting_point ? _chemical_formula_moiety 'C19 H12 Br N2 O4 Re' _chemical_formula_sum 'C19 H12 Br N2 O4 Re' _chemical_formula_weight 598.42 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 monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 6.7559(2) _cell_length_b 30.9785(9) _cell_length_c 10.5040(3) _cell_angle_alpha 90.00 _cell_angle_beta 106.7710(10) _cell_angle_gamma 90.00 _cell_volume 2104.85(11) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.888 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1128 _exptl_absorpt_coefficient_mu 7.696 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8054 _diffrn_reflns_av_R_equivalents 0.0369 _diffrn_reflns_av_sigmaI/netI 0.0478 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -40 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 27.49 _reflns_number_total 4649 _reflns_number_gt 4015 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1424P)^2^+3.9035P] 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 0.0071(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4649 _refine_ls_number_parameters 246 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0663 _refine_ls_R_factor_gt 0.0596 _refine_ls_wR_factor_ref 0.1940 _refine_ls_wR_factor_gt 0.1857 _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_restrained_S_all 1.094 _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 0.63800(5) 0.390777(10) 0.81129(3) 0.0187(2) Uani 1 1 d . . . Br2 Br 0.26520(12) 0.42069(3) 0.68826(8) 0.0233(2) Uani 1 1 d . . . N1 N 0.7112(10) 0.4146(2) 0.6308(7) 0.0186(13) Uani 1 1 d . . . O3 O 0.5328(11) 0.3731(3) 1.0717(7) 0.0381(17) Uani 1 1 d . . . C4 C 0.7144(14) 0.4124(3) 0.4049(8) 0.028(2) Uani 1 1 d . . . H4 H 0.7059 0.3958 0.3274 0.034 Uiso 1 1 calc R . . N5 N 0.7157(10) 0.4577(2) 0.8518(6) 0.0205(14) Uani 1 1 d . . . O6 O 1.0637(10) 0.3524(2) 0.9420(7) 0.0346(15) Uani 1 1 d . . . C7 C 0.7083(14) 0.3922(2) 0.5205(9) 0.0205(18) Uani 1 1 d . . . O9 O 0.4743(14) 0.2990(2) 0.7376(9) 0.051(2) Uani 1 1 d . . . C12 C 0.5721(14) 0.3801(3) 0.9730(10) 0.0272(18) Uani 1 1 d . . . C13 C 0.8884(16) 0.3218(3) 0.6000(10) 0.036(2) Uani 1 1 d . . . H13 H 1.0007 0.3377 0.6555 0.044 Uiso 1 1 calc R . . C15 C 0.7117(14) 0.3445(3) 0.5239(9) 0.0240(17) Uani 1 1 d . . . C16 C 0.7268(13) 0.4779(3) 0.9671(8) 0.0232(17) Uani 1 1 d . . . H16 H 0.7153 0.4608 1.0398 0.028 Uiso 1 1 calc R . . C17 C 0.5416(15) 0.3343(3) 0.7624(10) 0.0279(19) Uani 1 1 d . . . C18 C 0.7455(12) 0.4825(3) 0.7510(8) 0.0186(15) Uani 1 1 d . . . C19 C 0.7328(11) 0.4582(3) 0.6274(8) 0.0188(15) Uani 1 1 d . . . C20 C 0.9030(19) 0.2787(3) 0.5967(12) 0.041(2) Uani 1 1 d . . . H20 H 1.0266 0.2650 0.6473 0.049 Uiso 1 1 calc R . . C22 C 0.5517(16) 0.3204(4) 0.4431(11) 0.040(2) Uani 1 1 d . . . H22 H 0.4334 0.3346 0.3878 0.047 Uiso 1 1 calc R . . C23 C 0.9070(15) 0.3677(3) 0.8910(9) 0.0274(19) Uani 1 1 d . . . C24 C 0.563(2) 0.2746(4) 0.4423(12) 0.050(3) Uani 1 1 d . . . H24 H 0.4502 0.2583 0.3886 0.060 Uiso 1 1 calc R . . C25 C 0.739(2) 0.2532(4) 0.5199(12) 0.046(3) Uani 1 1 d . . . H25 H 0.7477 0.2226 0.5208 0.056 Uiso 1 1 calc R . . O1 O 0.7401(10) 0.4757(2) 0.2863(6) 0.0318(15) Uani 1 1 d . . . H1 H 0.6436 0.4663 0.2227 0.038 Uiso 1 1 calc R . . C2 C 0.7328(12) 0.4563(3) 0.4017(8) 0.0199(16) Uani 1 1 d . . . C1 C 0.7466(12) 0.4798(3) 0.5148(8) 0.0181(15) Uani 1 1 d . . . H2 H 0.7652 0.5102 0.5158 0.022 Uiso 1 1 calc R . . C8 C 0.7784(13) 0.5468(3) 0.8813(9) 0.0240(17) Uani 1 1 d . . . H8 H 0.7957 0.5771 0.8903 0.029 Uiso 1 1 calc R . . C5 C 0.7539(13) 0.5220(3) 0.9861(9) 0.0240(17) Uani 1 1 d . . . H5 H 0.7557 0.5349 1.0684 0.029 Uiso 1 1 calc R . . C3 C 0.7774(13) 0.5266(3) 0.7646(9) 0.0245(17) Uani 1 1 d . . . H3 H 0.7985 0.5429 0.6931 0.029 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 0.0227(3) 0.0132(3) 0.0202(3) 0.00027(10) 0.00619(16) 0.00082(10) Br2 0.0210(4) 0.0204(5) 0.0276(5) -0.0005(3) 0.0055(3) -0.0011(3) N1 0.017(3) 0.015(4) 0.023(3) -0.002(3) 0.004(2) 0.001(3) O3 0.042(4) 0.053(5) 0.024(3) 0.004(3) 0.017(3) 0.002(4) C4 0.031(4) 0.038(5) 0.020(4) -0.009(4) 0.012(3) 0.005(4) N5 0.015(3) 0.030(4) 0.016(3) 0.002(3) 0.005(2) 0.007(3) O6 0.029(3) 0.030(4) 0.042(4) 0.004(3) 0.006(3) 0.010(3) C7 0.021(4) 0.019(5) 0.020(4) -0.004(3) 0.004(3) -0.003(3) O9 0.072(6) 0.027(4) 0.058(5) -0.001(4) 0.028(4) -0.009(4) C12 0.029(5) 0.019(4) 0.035(5) 0.005(4) 0.011(4) 0.006(4) C13 0.039(5) 0.036(6) 0.037(5) -0.011(4) 0.016(4) 0.005(4) C15 0.033(4) 0.015(4) 0.027(4) -0.005(3) 0.012(3) 0.002(3) C16 0.026(4) 0.024(5) 0.019(4) -0.006(3) 0.005(3) 0.005(3) C17 0.039(5) 0.010(4) 0.038(5) 0.004(3) 0.015(4) -0.004(4) C18 0.019(4) 0.018(4) 0.018(4) -0.005(3) 0.004(3) -0.002(3) C19 0.014(3) 0.025(4) 0.018(4) -0.002(3) 0.005(3) 0.001(3) C20 0.060(7) 0.015(5) 0.054(6) 0.001(4) 0.026(5) 0.010(5) C22 0.033(5) 0.038(6) 0.043(6) -0.015(4) 0.002(4) -0.010(4) C23 0.040(5) 0.020(5) 0.026(4) -0.002(3) 0.014(4) -0.001(4) C24 0.066(8) 0.036(6) 0.055(7) -0.028(5) 0.027(6) -0.027(6) C25 0.073(8) 0.021(5) 0.051(7) -0.015(5) 0.027(6) -0.004(5) O1 0.041(4) 0.038(4) 0.019(3) -0.001(3) 0.012(3) 0.003(3) C2 0.020(4) 0.018(4) 0.023(4) 0.000(3) 0.007(3) -0.001(3) C1 0.021(4) 0.010(4) 0.021(4) 0.002(3) 0.002(3) 0.002(3) C8 0.033(4) 0.004(3) 0.039(5) -0.003(3) 0.017(4) -0.002(3) C5 0.025(4) 0.023(4) 0.027(4) -0.004(3) 0.012(3) 0.001(3) C3 0.027(4) 0.017(4) 0.032(4) -0.005(3) 0.012(3) -0.001(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re1 C17 1.886(9) . ? Re1 C12 1.905(9) . ? Re1 C23 1.907(10) . ? Re1 N5 2.151(8) . ? Re1 N1 2.219(7) . ? Re1 Br2 2.6445(9) . ? N1 C7 1.346(11) . ? N1 C19 1.360(11) . ? O3 C12 1.162(11) . ? C4 C2 1.366(13) . ? C4 C7 1.377(13) . ? C4 H4 0.9500 . ? N5 C16 1.345(10) . ? N5 C18 1.369(10) . ? O6 C23 1.142(11) . ? C7 C15 1.477(11) . ? O9 C17 1.183(12) . ? C13 C20 1.339(14) . ? C13 C15 1.418(14) . ? C13 H13 0.9500 . ? C15 C22 1.384(13) . ? C16 C5 1.386(12) . ? C16 H16 0.9500 . ? C18 C3 1.384(11) . ? C18 C19 1.481(10) . ? C19 C1 1.386(11) . ? C20 C25 1.409(17) . ? C20 H20 0.9500 . ? C22 C24 1.424(17) . ? C22 H22 0.9500 . ? C24 C25 1.399(19) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? O1 C2 1.368(10) . ? O1 H1 0.8400 . ? C2 C1 1.374(11) . ? C1 H2 0.9500 . ? C8 C3 1.375(12) . ? C8 C5 1.390(12) . ? C8 H8 0.9500 . ? C5 H5 0.9500 . ? C3 H3 0.9500 . ? 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 C17 Re1 C12 86.0(4) . . ? C17 Re1 C23 89.0(4) . . ? C12 Re1 C23 89.0(4) . . ? C17 Re1 N5 173.5(3) . . ? C12 Re1 N5 95.6(3) . . ? C23 Re1 N5 97.3(3) . . ? C17 Re1 N1 102.7(3) . . ? C12 Re1 N1 170.6(3) . . ? C23 Re1 N1 94.6(3) . . ? N5 Re1 N1 75.4(2) . . ? C17 Re1 Br2 89.2(3) . . ? C12 Re1 Br2 93.5(3) . . ? C23 Re1 Br2 176.8(3) . . ? N5 Re1 Br2 84.40(17) . . ? N1 Re1 Br2 83.20(17) . . ? C7 N1 C19 117.7(7) . . ? C7 N1 Re1 127.8(6) . . ? C19 N1 Re1 113.9(5) . . ? C2 C4 C7 120.0(8) . . ? C2 C4 H4 120.0 . . ? C7 C4 H4 120.0 . . ? C16 N5 C18 117.0(8) . . ? C16 N5 Re1 124.9(6) . . ? C18 N5 Re1 118.0(5) . . ? N1 C7 C4 121.9(8) . . ? N1 C7 C15 119.9(8) . . ? C4 C7 C15 118.1(8) . . ? O3 C12 Re1 179.3(9) . . ? C20 C13 C15 122.5(10) . . ? C20 C13 H13 118.8 . . ? C15 C13 H13 118.8 . . ? C22 C15 C13 117.3(9) . . ? C22 C15 C7 121.3(9) . . ? C13 C15 C7 121.0(8) . . ? N5 C16 C5 124.0(8) . . ? N5 C16 H16 118.0 . . ? C5 C16 H16 118.0 . . ? O9 C17 Re1 175.8(8) . . ? N5 C18 C3 121.8(7) . . ? N5 C18 C19 114.1(7) . . ? C3 C18 C19 124.1(8) . . ? N1 C19 C1 122.5(7) . . ? N1 C19 C18 117.5(7) . . ? C1 C19 C18 120.1(8) . . ? C13 C20 C25 121.4(11) . . ? C13 C20 H20 119.3 . . ? C25 C20 H20 119.3 . . ? C15 C22 C24 120.6(11) . . ? C15 C22 H22 119.7 . . ? C24 C22 H22 119.7 . . ? O6 C23 Re1 176.6(8) . . ? C25 C24 C22 120.4(10) . . ? C25 C24 H24 119.8 . . ? C22 C24 H24 119.8 . . ? C24 C25 C20 117.7(10) . . ? C24 C25 H25 121.1 . . ? C20 C25 H25 121.1 . . ? C2 O1 H1 109.5 . . ? C4 C2 O1 119.2(7) . . ? C4 C2 C1 119.4(8) . . ? O1 C2 C1 121.4(8) . . ? C2 C1 C19 118.5(8) . . ? C2 C1 H2 120.8 . . ? C19 C1 H2 120.8 . . ? C3 C8 C5 119.0(8) . . ? C3 C8 H8 120.5 . . ? C5 C8 H8 120.5 . . ? C16 C5 C8 118.1(8) . . ? C16 C5 H5 121.0 . . ? C8 C5 H5 121.0 . . ? C8 C3 C18 120.1(8) . . ? C8 C3 H3 119.9 . . ? C18 C3 H3 119.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C17 Re1 N1 C7 -6.5(8) . . . . ? C12 Re1 N1 C7 -164.4(19) . . . . ? C23 Re1 N1 C7 83.5(7) . . . . ? N5 Re1 N1 C7 179.9(7) . . . . ? Br2 Re1 N1 C7 -94.2(7) . . . . ? C17 Re1 N1 C19 163.7(6) . . . . ? C12 Re1 N1 C19 6(2) . . . . ? C23 Re1 N1 C19 -106.2(6) . . . . ? N5 Re1 N1 C19 -9.9(5) . . . . ? Br2 Re1 N1 C19 76.1(5) . . . . ? C17 Re1 N5 C16 110(3) . . . . ? C12 Re1 N5 C16 6.2(7) . . . . ? C23 Re1 N5 C16 -83.5(7) . . . . ? N1 Re1 N5 C16 -176.4(7) . . . . ? Br2 Re1 N5 C16 99.2(6) . . . . ? C17 Re1 N5 C18 -66(3) . . . . ? C12 Re1 N5 C18 -170.1(6) . . . . ? C23 Re1 N5 C18 100.2(6) . . . . ? N1 Re1 N5 C18 7.3(5) . . . . ? Br2 Re1 N5 C18 -77.1(5) . . . . ? C19 N1 C7 C4 -3.8(12) . . . . ? Re1 N1 C7 C4 166.1(6) . . . . ? C19 N1 C7 C15 172.3(8) . . . . ? Re1 N1 C7 C15 -17.8(12) . . . . ? C2 C4 C7 N1 2.8(14) . . . . ? C2 C4 C7 C15 -173.3(8) . . . . ? C17 Re1 C12 O3 42(95) . . . . ? C23 Re1 C12 O3 -47(95) . . . . ? N5 Re1 C12 O3 -144(95) . . . . ? N1 Re1 C12 O3 -159(94) . . . . ? Br2 Re1 C12 O3 131(95) . . . . ? C20 C13 C15 C22 -0.6(14) . . . . ? C20 C13 C15 C7 -174.4(9) . . . . ? N1 C7 C15 C22 119.2(10) . . . . ? C4 C7 C15 C22 -64.6(12) . . . . ? N1 C7 C15 C13 -67.3(12) . . . . ? C4 C7 C15 C13 108.9(10) . . . . ? C18 N5 C16 C5 4.0(12) . . . . ? Re1 N5 C16 C5 -172.4(6) . . . . ? C12 Re1 C17 O9 21(12) . . . . ? C23 Re1 C17 O9 110(12) . . . . ? N5 Re1 C17 O9 -83(13) . . . . ? N1 Re1 C17 O9 -155(12) . . . . ? Br2 Re1 C17 O9 -72(12) . . . . ? C16 N5 C18 C3 -2.6(11) . . . . ? Re1 N5 C18 C3 174.0(6) . . . . ? C16 N5 C18 C19 179.6(7) . . . . ? Re1 N5 C18 C19 -3.8(8) . . . . ? C7 N1 C19 C1 1.6(11) . . . . ? Re1 N1 C19 C1 -169.8(6) . . . . ? C7 N1 C19 C18 -177.3(7) . . . . ? Re1 N1 C19 C18 11.4(8) . . . . ? N5 C18 C19 N1 -5.3(10) . . . . ? C3 C18 C19 N1 176.8(7) . . . . ? N5 C18 C19 C1 175.8(7) . . . . ? C3 C18 C19 C1 -2.0(12) . . . . ? C15 C13 C20 C25 -2.1(16) . . . . ? C13 C15 C22 C24 2.7(15) . . . . ? C7 C15 C22 C24 176.4(9) . . . . ? C17 Re1 C23 O6 -49(14) . . . . ? C12 Re1 C23 O6 37(14) . . . . ? N5 Re1 C23 O6 132(14) . . . . ? N1 Re1 C23 O6 -152(14) . . . . ? Br2 Re1 C23 O6 -105(14) . . . . ? C15 C22 C24 C25 -2.1(17) . . . . ? C22 C24 C25 C20 -0.6(17) . . . . ? C13 C20 C25 C24 2.7(17) . . . . ? C7 C4 C2 O1 179.5(8) . . . . ? C7 C4 C2 C1 0.5(13) . . . . ? C4 C2 C1 C19 -2.6(12) . . . . ? O1 C2 C1 C19 178.4(7) . . . . ? N1 C19 C1 C2 1.6(12) . . . . ? C18 C19 C1 C2 -179.6(7) . . . . ? N5 C16 C5 C8 -2.4(13) . . . . ? C3 C8 C5 C16 -0.8(13) . . . . ? C5 C8 C3 C18 2.1(13) . . . . ? N5 C18 C3 C8 -0.4(13) . . . . ? C19 C18 C3 C8 177.3(8) . . . . ? _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.963 _refine_diff_density_max 3.759 _refine_diff_density_min -5.174 _refine_diff_density_rms 0.417