Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'Isabel Santos' 'Susana Alves' 'Joao D. G. Correia' 'Angela Domingos' 'Antonio Paulo' _publ_contact_author_name 'Prof Isabel Santos' _publ_contact_author_address ; Departamento de Quimica ITN Estrada Nacional 10 2686-953 Sacavem Codex PORTUGAL ; _publ_contact_author_email 'ISANTOS@ITN1.ITN.PT' _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Coordination Capabilities of Pyrazolyl Containing Ligands Towards the fac-[Re(CO)3]+ Moiety ; data_pzNHpz _database_code_CSD 190654 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety [Re(CO)3(k3-pz(CH2)2NH(CH2)2pz)]Br _chemical_formula_sum 'C17 H23 Br N5 O3 Re' _chemical_formula_weight 611.51 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' 'Br' 'Br' -0.2901 2.4595 '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 8.6142(11) _cell_length_b 15.622(3) _cell_length_c 17.244(4) _cell_angle_alpha 114.52(2) _cell_angle_beta 92.647(15) _cell_angle_gamma 95.593(12) _cell_volume 2091.6(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 8.5 _cell_measurement_theta_max 14.0 _exptl_crystal_description 'irregular fragment' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.942 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1176 _exptl_absorpt_coefficient_mu 7.746 _exptl_absorpt_correction_type 'empirical via \y-scan North et al(1968)' _exptl_absorpt_correction_T_min 0.7192 _exptl_absorpt_correction_T_max 0.9996 _exptl_absorpt_process_details ? _exptl_special_details ; Crystals were obtained by slow evaporation of concentrated solution of the compound in acetonitrile. ; _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 'CAD4-Enraf-Nonius' _diffrn_measurement_method '\w/2\qscans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% none _diffrn_reflns_number 8701 _diffrn_reflns_av_R_equivalents 0.0297 _diffrn_reflns_av_sigmaI/netI 0.0536 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_theta_max 27.00 _reflns_number_total 8410 _reflns_number_gt 6060 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 software(Enraf-Nonius,1989)' _computing_cell_refinement 'CAD4 software(Enraf-Nonius,1989)' _computing_data_reduction 'process-MolEN(Fair,1990)' _computing_structure_solution 'SHELXS-97 (Sheldrick,1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3(Farrugia,1997)' _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^)+(0.0321P)^2^+6.6400P] 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 8410 _refine_ls_number_parameters 487 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0795 _refine_ls_R_factor_gt 0.0458 _refine_ls_wR_factor_ref 0.0943 _refine_ls_wR_factor_gt 0.0790 _refine_ls_goodness_of_fit_ref 1.114 _refine_ls_restrained_S_all 1.114 _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 0.37692(4) 0.23493(2) 0.03559(2) 0.03097(10) Uani 1 1 d . . . Re2 Re -0.04808(4) 0.28198(2) 0.49474(2) 0.03167(10) Uani 1 1 d . . . Br1 Br 0.74966(12) 0.33166(8) -0.10044(7) 0.0540(3) Uani 1 1 d . . . Br2 Br 0.28019(13) 0.16048(8) 0.60999(7) 0.0583(3) Uani 1 1 d . . . O1 O 0.3482(10) 0.1078(5) 0.1301(5) 0.077(3) Uani 1 1 d . . . O2 O 0.5872(9) 0.0904(6) -0.0680(5) 0.077(2) Uani 1 1 d . . . O3 O 0.6689(9) 0.3416(6) 0.1577(5) 0.077(2) Uani 1 1 d . . . O4 O 0.0162(10) 0.4189(5) 0.4127(5) 0.071(2) Uani 1 1 d . . . O5 O 0.2346(9) 0.1936(6) 0.4083(5) 0.070(2) Uani 1 1 d . . . O6 O 0.1726(8) 0.4360(5) 0.6388(5) 0.0582(19) Uani 1 1 d . . . N1 N 0.3895(8) 0.3177(5) -0.0440(4) 0.0355(17) Uani 1 1 d . . . H1 H 0.4940 0.3332 -0.0444 0.043 Uiso 1 1 calc R . . N2 N 0.2333(7) 0.3405(4) 0.1182(4) 0.0260(14) Uani 1 1 d . . . N3 N 0.1675(8) 0.1598(5) -0.0526(4) 0.0345(17) Uani 1 1 d . . . N4 N -0.0842(9) 0.1931(5) 0.5678(4) 0.0364(17) Uani 1 1 d . . . H4 H 0.0145 0.1832 0.5800 0.044 Uiso 1 1 calc R . . N5 N -0.2580(8) 0.3380(5) 0.5495(4) 0.0346(17) Uani 1 1 d . . . N6 N -0.2113(9) 0.1706(5) 0.3906(5) 0.0386(18) Uani 1 1 d . . . N21 N 0.1367(7) 0.3882(5) 0.0901(4) 0.0289(15) Uani 1 1 d . . . N31 N 0.1714(8) 0.1300(5) -0.1392(4) 0.0345(16) Uani 1 1 d . . . N51 N -0.2853(8) 0.3552(5) 0.6332(4) 0.0354(17) Uani 1 1 d . . . N61 N -0.3263(9) 0.1123(5) 0.4019(5) 0.0381(17) Uani 1 1 d . . . C1 C 0.3572(11) 0.1570(6) 0.0954(6) 0.044(2) Uani 1 1 d . . . C2 C 0.5048(11) 0.1468(7) -0.0313(6) 0.045(2) Uani 1 1 d . . . C3 C 0.5619(11) 0.3041(7) 0.1118(6) 0.044(2) Uani 1 1 d . . . C4 C -0.0126(12) 0.3660(7) 0.4405(6) 0.046(2) Uani 1 1 d . . . C5 C 0.1284(12) 0.2253(7) 0.4423(6) 0.046(2) Uani 1 1 d . . . C6 C 0.0884(11) 0.3762(7) 0.5846(6) 0.039(2) Uani 1 1 d . . . C7 C 0.1560(10) 0.3977(7) 0.0106(5) 0.037(2) Uani 1 1 d . . . H7A H 0.1090 0.4524 0.0125 0.045 Uiso 1 1 calc R . . H7B H 0.1016 0.3420 -0.0368 0.045 Uiso 1 1 calc R . . C8 C 0.3296(10) 0.4094(6) -0.0045(6) 0.036(2) Uani 1 1 d . . . H8A H 0.3420 0.4421 -0.0414 0.043 Uiso 1 1 calc R . . H8B H 0.3906 0.4482 0.0497 0.043 Uiso 1 1 calc R . . C9 C 0.3293(11) 0.2704(6) -0.1364(5) 0.043(2) Uani 1 1 d . . . H9A H 0.4030 0.2897 -0.1688 0.051 Uiso 1 1 calc R . . H9B H 0.2308 0.2928 -0.1435 0.051 Uiso 1 1 calc R . . C10 C 0.3035(10) 0.1630(7) -0.1742(6) 0.043(2) Uani 1 1 d . . . H10A H 0.2831 0.1378 -0.2359 0.052 Uiso 1 1 calc R . . H10B H 0.3974 0.1398 -0.1614 0.052 Uiso 1 1 calc R . . C11 C -0.1646(10) 0.0973(6) 0.5163(5) 0.038(2) Uani 1 1 d . . . H11A H -0.1717 0.0624 0.5515 0.046 Uiso 1 1 calc R . . H11B H -0.1033 0.0646 0.4695 0.046 Uiso 1 1 calc R . . C12 C -0.3267(12) 0.0981(7) 0.4803(6) 0.049(2) Uani 1 1 d . . . H12A H -0.3896 0.0383 0.4685 0.059 Uiso 1 1 calc R . . H12B H -0.3751 0.1483 0.5228 0.059 Uiso 1 1 calc R . . C13 C -0.1474(13) 0.2335(7) 0.6533(6) 0.053(3) Uani 1 1 d . . . H13A H -0.0755 0.2264 0.6946 0.063 Uiso 1 1 calc R . . H13B H -0.2464 0.1960 0.6497 0.063 Uiso 1 1 calc R . . C14 C -0.1733(11) 0.3361(7) 0.6869(5) 0.041(2) Uani 1 1 d . . . H14A H -0.2093 0.3555 0.7435 0.049 Uiso 1 1 calc R . . H14B H -0.0740 0.3743 0.6926 0.049 Uiso 1 1 calc R . . C21 C 0.0426(9) 0.4338(6) 0.1498(5) 0.0320(19) Uani 1 1 d . . . C22 C 0.0773(10) 0.4154(6) 0.2188(6) 0.039(2) Uani 1 1 d . . . H22 H 0.0303 0.4368 0.2698 0.047 Uiso 1 1 calc R . . C23 C 0.1964(10) 0.3585(6) 0.1978(5) 0.035(2) Uani 1 1 d . . . C24 C -0.0740(10) 0.4912(6) 0.1347(6) 0.042(2) Uani 1 1 d . . . H24A H -0.0691 0.4883 0.0781 0.062 Uiso 1 1 calc R . . H24B H -0.0505 0.5560 0.1761 0.062 Uiso 1 1 calc R . . H24C H -0.1773 0.4663 0.1400 0.062 Uiso 1 1 calc R . . C25 C 0.2803(13) 0.3260(8) 0.2568(6) 0.057(3) Uani 1 1 d . . . H25A H 0.3579 0.2876 0.2274 0.085 Uiso 1 1 calc R . . H25B H 0.2063 0.2895 0.2748 0.085 Uiso 1 1 calc R . . H25C H 0.3303 0.3802 0.3061 0.085 Uiso 1 1 calc R . . C31 C 0.0380(10) 0.0766(6) -0.1813(6) 0.039(2) Uani 1 1 d . . . C32 C -0.0568(11) 0.0694(7) -0.1215(7) 0.047(2) Uani 1 1 d . . . H32 H -0.1564 0.0357 -0.1321 0.057 Uiso 1 1 calc R . . C33 C 0.0270(10) 0.1228(6) -0.0421(6) 0.038(2) Uani 1 1 d . . . C34 C 0.0087(11) 0.0334(7) -0.2764(6) 0.052(3) Uani 1 1 d . . . H34A H 0.0975 0.0520 -0.3002 0.078 Uiso 1 1 calc R . . H34B H -0.0828 0.0548 -0.2928 0.078 Uiso 1 1 calc R . . H34C H -0.0074 -0.0345 -0.2977 0.078 Uiso 1 1 calc R . . C35 C -0.0278(11) 0.1412(8) 0.0432(6) 0.056(3) Uani 1 1 d . . . H35A H 0.0533 0.1806 0.0872 0.084 Uiso 1 1 calc R . . H35B H -0.0523 0.0821 0.0474 0.084 Uiso 1 1 calc R . . H35C H -0.1197 0.1729 0.0501 0.084 Uiso 1 1 calc R . . C51 C -0.4177(10) 0.3957(7) 0.6534(6) 0.042(2) Uani 1 1 d . . . C52 C -0.4784(11) 0.4026(7) 0.5836(6) 0.049(3) Uani 1 1 d . . . H52 H -0.5710 0.4267 0.5785 0.059 Uiso 1 1 calc R . . C53 C -0.3787(11) 0.3675(7) 0.5210(6) 0.045(2) Uani 1 1 d . . . C54 C -0.4772(11) 0.4204(8) 0.7398(7) 0.059(3) Uani 1 1 d . . . H54A H -0.4048 0.4059 0.7752 0.089 Uiso 1 1 calc R . . H54B H -0.5776 0.3842 0.7330 0.089 Uiso 1 1 calc R . . H54C H -0.4874 0.4868 0.7662 0.089 Uiso 1 1 calc R . . C55 C -0.3973(14) 0.3613(9) 0.4316(7) 0.068(3) Uani 1 1 d . . . H55A H -0.3115 0.3334 0.4012 0.101 Uiso 1 1 calc R . . H55B H -0.3983 0.4238 0.4342 0.101 Uiso 1 1 calc R . . H55C H -0.4941 0.3228 0.4025 0.101 Uiso 1 1 calc R . . C61 C -0.4223(12) 0.0631(7) 0.3295(7) 0.049(3) Uani 1 1 d . . . C62 C -0.3667(13) 0.0884(7) 0.2691(6) 0.052(3) Uani 1 1 d . . . H62 H -0.4089 0.0655 0.2125 0.063 Uiso 1 1 calc R . . C63 C -0.2366(13) 0.1542(7) 0.3063(6) 0.049(3) Uani 1 1 d . . . C64 C -0.5585(11) -0.0075(8) 0.3258(8) 0.065(3) Uani 1 1 d . . . H64A H -0.5633 -0.0083 0.3810 0.098 Uiso 1 1 calc R . . H64B H -0.5446 -0.0695 0.2842 0.098 Uiso 1 1 calc R . . H64C H -0.6542 0.0105 0.3099 0.098 Uiso 1 1 calc R . . C65 C -0.1358(15) 0.2019(9) 0.2639(7) 0.076(4) Uani 1 1 d . . . H65A H -0.0526 0.2445 0.3046 0.115 Uiso 1 1 calc R . . H65B H -0.1977 0.2370 0.2429 0.115 Uiso 1 1 calc R . . H65C H -0.0921 0.1550 0.2171 0.115 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 0.02393(18) 0.03151(19) 0.0385(2) 0.01554(16) 0.00376(15) 0.00449(14) Re2 0.0354(2) 0.0332(2) 0.02962(19) 0.01481(16) 0.00918(15) 0.00908(15) Br1 0.0380(5) 0.0722(7) 0.0521(6) 0.0281(6) 0.0073(5) -0.0028(5) Br2 0.0542(7) 0.0621(7) 0.0675(7) 0.0353(6) 0.0004(5) 0.0130(5) O1 0.096(7) 0.067(5) 0.098(7) 0.067(5) 0.000(5) 0.005(5) O2 0.061(5) 0.067(5) 0.086(6) 0.011(5) 0.009(4) 0.029(4) O3 0.047(5) 0.090(6) 0.087(6) 0.037(5) -0.024(4) -0.017(4) O4 0.116(7) 0.054(5) 0.058(5) 0.035(4) 0.031(5) 0.009(5) O5 0.061(5) 0.078(5) 0.073(5) 0.028(4) 0.034(4) 0.033(4) O6 0.039(4) 0.061(5) 0.055(5) 0.006(4) 0.006(3) 0.001(4) N1 0.027(4) 0.044(4) 0.038(4) 0.022(4) 0.002(3) -0.002(3) N2 0.033(4) 0.025(3) 0.022(3) 0.012(3) 0.006(3) 0.003(3) N3 0.026(4) 0.036(4) 0.039(4) 0.014(3) 0.010(3) -0.002(3) N4 0.043(4) 0.033(4) 0.038(4) 0.018(3) 0.009(3) 0.016(3) N5 0.040(4) 0.048(4) 0.032(4) 0.028(4) 0.014(3) 0.020(4) N6 0.041(4) 0.042(4) 0.036(4) 0.019(4) 0.007(3) 0.006(4) N21 0.028(4) 0.036(4) 0.027(4) 0.016(3) 0.004(3) 0.009(3) N31 0.030(4) 0.035(4) 0.036(4) 0.012(3) 0.002(3) 0.001(3) N51 0.031(4) 0.040(4) 0.034(4) 0.014(3) 0.009(3) 0.010(3) N61 0.037(4) 0.042(4) 0.038(4) 0.020(4) 0.003(3) 0.004(3) C1 0.037(5) 0.034(5) 0.053(6) 0.014(5) -0.006(5) 0.005(4) C2 0.039(5) 0.053(6) 0.035(5) 0.011(5) -0.002(4) 0.010(5) C3 0.034(5) 0.046(6) 0.050(6) 0.018(5) 0.004(5) 0.010(4) C4 0.070(7) 0.041(5) 0.035(5) 0.023(5) 0.018(5) 0.006(5) C5 0.056(6) 0.042(5) 0.055(6) 0.031(5) 0.019(5) 0.018(5) C6 0.034(5) 0.046(6) 0.044(6) 0.024(5) 0.022(4) 0.015(4) C7 0.033(5) 0.050(5) 0.034(5) 0.020(4) 0.011(4) 0.014(4) C8 0.039(5) 0.033(5) 0.037(5) 0.017(4) 0.007(4) -0.001(4) C9 0.044(6) 0.054(6) 0.034(5) 0.022(5) 0.009(4) -0.001(5) C10 0.032(5) 0.063(6) 0.032(5) 0.015(5) 0.010(4) 0.009(5) C11 0.049(6) 0.036(5) 0.034(5) 0.018(4) 0.010(4) 0.008(4) C12 0.052(6) 0.049(6) 0.043(6) 0.020(5) 0.005(5) -0.005(5) C13 0.078(8) 0.052(6) 0.031(5) 0.020(5) 0.007(5) 0.014(6) C14 0.041(5) 0.055(6) 0.030(5) 0.020(4) 0.002(4) 0.012(4) C21 0.030(5) 0.030(4) 0.039(5) 0.017(4) 0.012(4) 0.007(4) C22 0.039(5) 0.045(5) 0.040(5) 0.025(4) 0.009(4) 0.002(4) C23 0.041(5) 0.035(5) 0.036(5) 0.019(4) 0.007(4) 0.014(4) C24 0.040(5) 0.051(6) 0.042(5) 0.024(5) 0.016(4) 0.019(4) C25 0.070(7) 0.081(8) 0.038(6) 0.038(6) 0.007(5) 0.028(6) C31 0.035(5) 0.031(5) 0.048(6) 0.015(4) -0.005(4) 0.005(4) C32 0.029(5) 0.048(6) 0.064(7) 0.026(5) -0.001(5) -0.009(4) C33 0.029(5) 0.038(5) 0.055(6) 0.027(5) 0.012(4) 0.002(4) C34 0.042(6) 0.059(6) 0.048(6) 0.019(5) -0.016(5) -0.006(5) C35 0.038(6) 0.074(7) 0.054(6) 0.028(6) 0.009(5) -0.009(5) C51 0.035(5) 0.050(6) 0.038(5) 0.016(5) 0.012(4) 0.009(4) C52 0.042(6) 0.063(7) 0.050(6) 0.027(5) 0.009(5) 0.022(5) C53 0.044(6) 0.047(6) 0.040(5) 0.017(5) -0.002(4) 0.008(5) C54 0.036(6) 0.075(8) 0.061(7) 0.020(6) 0.019(5) 0.019(5) C55 0.069(8) 0.090(9) 0.063(7) 0.045(7) 0.005(6) 0.039(7) C61 0.043(6) 0.045(6) 0.057(7) 0.018(5) 0.001(5) 0.010(5) C62 0.067(7) 0.051(6) 0.038(6) 0.016(5) -0.005(5) 0.015(5) C63 0.067(7) 0.049(6) 0.026(5) 0.010(4) -0.001(5) 0.016(5) C64 0.031(6) 0.071(7) 0.084(9) 0.027(7) -0.010(5) -0.002(5) C65 0.100(10) 0.088(9) 0.045(7) 0.038(7) 0.002(7) -0.012(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re1 C2 1.880(9) . ? Re1 C1 1.896(10) . ? Re1 C3 1.931(10) . ? Re1 N3 2.190(7) . ? Re1 N2 2.211(6) . ? Re1 N1 2.242(7) . ? Re2 C6 1.885(10) . ? Re2 C5 1.908(10) . ? Re2 C4 1.913(9) . ? Re2 N5 2.170(7) . ? Re2 N6 2.219(7) . ? Re2 N4 2.240(7) . ? O1 C1 1.151(11) . ? O2 C2 1.175(11) . ? O3 C3 1.123(11) . ? O4 C4 1.129(10) . ? O5 C5 1.149(11) . ? O6 C6 1.163(11) . ? N1 C8 1.467(10) . ? N1 C9 1.492(10) . ? N2 C23 1.343(10) . ? N2 N21 1.366(8) . ? N3 C33 1.343(10) . ? N3 N31 1.371(9) . ? N4 C11 1.464(11) . ? N4 C13 1.496(11) . ? N5 C53 1.330(11) . ? N5 N51 1.389(9) . ? N6 N61 1.355(10) . ? N6 C63 1.370(11) . ? N21 C21 1.344(10) . ? N21 C7 1.455(10) . ? N31 C31 1.333(10) . ? N31 C10 1.460(11) . ? N51 C51 1.347(10) . ? N51 C14 1.442(10) . ? N61 C61 1.348(12) . ? N61 C12 1.458(11) . ? C7 C8 1.536(11) . ? C9 C10 1.515(13) . ? C11 C12 1.505(13) . ? C13 C14 1.506(12) . ? C21 C22 1.361(11) . ? C21 C24 1.492(11) . ? C22 C23 1.386(11) . ? C23 C25 1.499(11) . ? C31 C32 1.378(13) . ? C31 C34 1.490(12) . ? C32 C33 1.392(13) . ? C33 C35 1.486(12) . ? C51 C52 1.339(12) . ? C51 C54 1.504(12) . ? C52 C53 1.375(13) . ? C53 C55 1.504(13) . ? C61 C62 1.349(14) . ? C61 C64 1.509(14) . ? C62 C63 1.372(14) . ? C63 C65 1.493(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Re1 C1 84.4(4) . . ? C2 Re1 C3 87.9(4) . . ? C1 Re1 C3 88.2(4) . . ? C2 Re1 N3 92.5(3) . . ? C1 Re1 N3 93.6(3) . . ? C3 Re1 N3 178.2(3) . . ? C2 Re1 N2 177.9(3) . . ? C1 Re1 N2 95.0(3) . . ? C3 Re1 N2 90.1(3) . . ? N3 Re1 N2 89.5(2) . . ? C2 Re1 N1 93.9(4) . . ? C1 Re1 N1 175.5(3) . . ? C3 Re1 N1 95.9(3) . . ? N3 Re1 N1 82.3(3) . . ? N2 Re1 N1 86.9(2) . . ? C6 Re2 C5 89.6(4) . . ? C6 Re2 C4 83.6(4) . . ? C5 Re2 C4 86.7(4) . . ? C6 Re2 N5 93.9(3) . . ? C5 Re2 N5 176.4(4) . . ? C4 Re2 N5 94.8(3) . . ? C6 Re2 N6 178.9(3) . . ? C5 Re2 N6 91.1(4) . . ? C4 Re2 N6 97.3(4) . . ? N5 Re2 N6 85.4(3) . . ? C6 Re2 N4 92.4(3) . . ? C5 Re2 N4 94.9(3) . . ? C4 Re2 N4 175.6(3) . . ? N5 Re2 N4 83.8(2) . . ? N6 Re2 N4 86.8(3) . . ? C8 N1 C9 108.8(7) . . ? C8 N1 Re1 113.8(5) . . ? C9 N1 Re1 119.7(5) . . ? C23 N2 N21 104.7(6) . . ? C23 N2 Re1 129.6(5) . . ? N21 N2 Re1 124.5(5) . . ? C33 N3 N31 105.8(7) . . ? C33 N3 Re1 132.9(6) . . ? N31 N3 Re1 120.8(5) . . ? C11 N4 C13 109.8(7) . . ? C11 N4 Re2 114.0(5) . . ? C13 N4 Re2 119.9(5) . . ? C53 N5 N51 104.4(7) . . ? C53 N5 Re2 133.6(6) . . ? N51 N5 Re2 121.9(5) . . ? N61 N6 C63 104.7(8) . . ? N61 N6 Re2 125.1(5) . . ? C63 N6 Re2 129.6(7) . . ? C21 N21 N2 111.4(6) . . ? C21 N21 C7 126.3(7) . . ? N2 N21 C7 121.6(6) . . ? C31 N31 N3 110.8(7) . . ? C31 N31 C10 127.9(8) . . ? N3 N31 C10 121.0(7) . . ? C51 N51 N5 110.3(7) . . ? C51 N51 C14 129.1(7) . . ? N5 N51 C14 120.5(6) . . ? C61 N61 N6 111.5(8) . . ? C61 N61 C12 126.3(8) . . ? N6 N61 C12 121.7(7) . . ? O1 C1 Re1 177.9(9) . . ? O2 C2 Re1 175.0(9) . . ? O3 C3 Re1 177.0(9) . . ? O4 C4 Re2 175.4(10) . . ? O5 C5 Re2 176.6(8) . . ? O6 C6 Re2 177.9(8) . . ? N21 C7 C8 111.7(7) . . ? N1 C8 C7 111.8(7) . . ? N1 C9 C10 114.9(7) . . ? N31 C10 C9 110.7(7) . . ? N4 C11 C12 112.4(7) . . ? N61 C12 C11 112.6(8) . . ? N4 C13 C14 115.9(8) . . ? N51 C14 C13 113.8(8) . . ? N21 C21 C22 107.0(7) . . ? N21 C21 C24 121.8(7) . . ? C22 C21 C24 131.2(8) . . ? C21 C22 C23 106.3(8) . . ? N2 C23 C22 110.5(7) . . ? N2 C23 C25 124.1(8) . . ? C22 C23 C25 125.3(8) . . ? N31 C31 C32 107.6(8) . . ? N31 C31 C34 123.0(8) . . ? C32 C31 C34 129.4(9) . . ? C31 C32 C33 106.0(8) . . ? N3 C33 C32 109.8(8) . . ? N3 C33 C35 123.3(8) . . ? C32 C33 C35 126.8(8) . . ? C52 C51 N51 107.2(8) . . ? C52 C51 C54 131.1(9) . . ? N51 C51 C54 121.6(8) . . ? C51 C52 C53 107.4(8) . . ? N5 C53 C52 110.7(8) . . ? N5 C53 C55 122.5(9) . . ? C52 C53 C55 126.8(9) . . ? N61 C61 C62 106.9(9) . . ? N61 C61 C64 121.3(10) . . ? C62 C61 C64 131.8(10) . . ? C61 C62 C63 107.7(9) . . ? N6 C63 C62 109.3(9) . . ? N6 C63 C65 123.9(9) . . ? C62 C63 C65 126.8(9) . . ? _diffrn_measured_fraction_theta_max 0.924 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.924 _refine_diff_density_max 1.029 _refine_diff_density_min -0.975 _refine_diff_density_rms 0.170 data_pznhnh2 _database_code_CSD 190655 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety [Re(CO)3(k3-pz(CH2)2NH(CH2)2NH2)]Br _chemical_formula_sum 'C12 H18 Br N4 O3 Re' _chemical_formula_weight 532.41 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' 'Br' 'Br' -0.2901 2.4595 '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 8.6270(11) _cell_length_b 9.0940(15) _cell_length_c 10.7625(16) _cell_angle_alpha 88.582(18) _cell_angle_beta 85.696(13) _cell_angle_gamma 74.688(14) _cell_volume 812.1(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7.5 _cell_measurement_theta_max 13.8 _exptl_crystal_description irregular _exptl_crystal_colour colorless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.177 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 504 _exptl_absorpt_coefficient_mu 9.956 _exptl_absorpt_correction_type 'empirical via \y-scan North et al(1968)' _exptl_absorpt_correction_T_min 0.5474 _exptl_absorpt_correction_T_max 0.9948 _exptl_absorpt_process_details ? _exptl_special_details ; Crystals obtained by recrystallization of concentrated solution of the compound in methanol ; _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 'CAD4-Enraf-Nonius' _diffrn_measurement_method '\w/2\qscans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% none _diffrn_reflns_number 3747 _diffrn_reflns_av_R_equivalents 0.0140 _diffrn_reflns_av_sigmaI/netI 0.0231 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 27.04 _reflns_number_total 3507 _reflns_number_gt 3179 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 software(Enraf-Nonius,1989)' _computing_cell_refinement 'CAD4 software(Enraf-Nonius,1989)' _computing_data_reduction 'process-MolEN(Fair,1990)' _computing_structure_solution 'SHELXS-97(Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia,1997)' _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^)+(0.0426P)^2^+2.6865P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3507 _refine_ls_number_parameters 190 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0366 _refine_ls_R_factor_gt 0.0305 _refine_ls_wR_factor_ref 0.0734 _refine_ls_wR_factor_gt 0.0693 _refine_ls_goodness_of_fit_ref 0.987 _refine_ls_restrained_S_all 0.987 _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 0.69016(3) 0.80249(2) 0.79640(2) 0.03017(8) Uani 1 1 d . . . Br1 Br 0.24559(8) 0.82853(8) 0.54461(7) 0.04825(16) Uani 1 1 d . . . O1 O 0.8059(7) 0.9610(6) 1.0052(5) 0.0612(14) Uani 1 1 d . . . O2 O 0.4450(7) 1.1088(6) 0.7594(5) 0.0691(16) Uani 1 1 d . . . O3 O 0.4578(7) 0.7230(7) 0.9987(5) 0.0699(16) Uani 1 1 d . . . N1 N 0.8528(6) 0.8440(6) 0.6389(4) 0.0368(11) Uani 1 1 d . . . H1A H 0.8241 0.9433 0.6175 0.044 Uiso 1 1 calc R . . H1B H 0.9544 0.8214 0.6624 0.044 Uiso 1 1 calc R . . N2 N 0.6103(6) 0.6951(6) 0.6377(5) 0.0427(12) Uani 1 1 d . . . H2 H 0.5020 0.7367 0.6393 0.051 Uiso 1 1 calc R . . N3 N 0.8715(6) 0.5827(5) 0.8094(5) 0.0348(10) Uani 1 1 d . . . N31 N 0.8345(6) 0.4488(5) 0.7871(4) 0.0353(10) Uani 1 1 d . . . C1 C 0.7682(8) 0.8981(7) 0.9254(6) 0.0394(13) Uani 1 1 d . . . C2 C 0.5343(8) 0.9932(7) 0.7729(6) 0.0431(14) Uani 1 1 d . . . C3 C 0.5464(8) 0.7529(8) 0.9220(6) 0.0452(15) Uani 1 1 d . . . C4 C 0.6730(8) 0.4489(7) 0.7577(7) 0.0502(17) Uani 1 1 d . . . H4A H 0.5962 0.4991 0.8239 0.060 Uiso 1 1 calc R . . H4B H 0.6657 0.3446 0.7525 0.060 Uiso 1 1 calc R . . C5 C 0.6306(10) 0.5305(8) 0.6352(8) 0.063(2) Uani 1 1 d . . . H5A H 0.7149 0.4867 0.5716 0.076 Uiso 1 1 calc R . . H5B H 0.5315 0.5116 0.6111 0.076 Uiso 1 1 calc R . . C6 C 0.6769(9) 0.7543(10) 0.5194(7) 0.0569(18) Uani 1 1 d . . . H6A H 0.6687 0.6918 0.4497 0.068 Uiso 1 1 calc R . . H6B H 0.6151 0.8580 0.5038 0.068 Uiso 1 1 calc R . . C7 C 0.8463(10) 0.7509(10) 0.5309(7) 0.0588(19) Uani 1 1 d . . . H7A H 0.9098 0.6469 0.5426 0.071 Uiso 1 1 calc R . . H7B H 0.8896 0.7917 0.4559 0.071 Uiso 1 1 calc R . . C31 C 0.9648(9) 0.3295(7) 0.7933(6) 0.0425(14) Uani 1 1 d . . . C32 C 1.0895(8) 0.3876(8) 0.8202(6) 0.0454(15) Uani 1 1 d . . . H32 H 1.1952 0.3323 0.8297 0.055 Uiso 1 1 calc R . . C33 C 1.0285(7) 0.5450(7) 0.8306(5) 0.0363(12) Uani 1 1 d . . . C34 C 1.1171(8) 0.6560(8) 0.8622(6) 0.0472(15) Uani 1 1 d . . . H34A H 1.0462 0.7571 0.8617 0.071 Uiso 1 1 calc R . . H34B H 1.2063 0.6500 0.8019 0.071 Uiso 1 1 calc R . . H34C H 1.1562 0.6332 0.9435 0.071 Uiso 1 1 calc R . . C35 C 0.9598(11) 0.1700(8) 0.7749(7) 0.061(2) Uani 1 1 d . . . H35A H 0.8537 0.1686 0.7547 0.092 Uiso 1 1 calc R . . H35B H 0.9859 0.1127 0.8501 0.092 Uiso 1 1 calc R . . H35C H 1.0366 0.1253 0.7081 0.092 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 0.02861(12) 0.02935(12) 0.03046(12) 0.00226(8) -0.00304(8) -0.00392(8) Br1 0.0352(3) 0.0530(4) 0.0542(4) 0.0086(3) -0.0083(3) -0.0070(3) O1 0.081(4) 0.059(3) 0.049(3) -0.008(2) -0.016(3) -0.023(3) O2 0.068(4) 0.050(3) 0.066(3) 0.005(2) -0.004(3) 0.025(3) O3 0.069(4) 0.079(4) 0.064(3) -0.003(3) 0.025(3) -0.030(3) N1 0.036(3) 0.036(3) 0.038(3) 0.000(2) 0.002(2) -0.011(2) N2 0.033(3) 0.051(3) 0.046(3) 0.003(2) -0.011(2) -0.013(2) N3 0.035(3) 0.028(2) 0.042(3) 0.0041(19) -0.009(2) -0.0079(19) N31 0.041(3) 0.029(2) 0.037(3) 0.0044(19) -0.009(2) -0.010(2) C1 0.045(3) 0.038(3) 0.038(3) 0.007(2) 0.001(3) -0.017(3) C2 0.046(4) 0.044(4) 0.036(3) 0.001(3) -0.001(3) -0.007(3) C3 0.047(4) 0.047(4) 0.043(3) -0.004(3) -0.004(3) -0.014(3) C4 0.048(4) 0.035(3) 0.074(5) -0.005(3) -0.009(3) -0.020(3) C5 0.067(5) 0.049(4) 0.075(5) -0.007(4) -0.040(4) -0.009(4) C6 0.058(4) 0.071(5) 0.045(4) -0.002(3) -0.005(3) -0.022(4) C7 0.067(5) 0.070(5) 0.044(4) -0.013(3) 0.012(3) -0.031(4) C31 0.060(4) 0.031(3) 0.033(3) 0.007(2) -0.009(3) -0.005(3) C32 0.041(3) 0.049(4) 0.037(3) 0.006(3) -0.008(3) 0.006(3) C33 0.034(3) 0.043(3) 0.031(3) 0.005(2) -0.005(2) -0.008(2) C34 0.037(3) 0.058(4) 0.049(4) 0.005(3) -0.010(3) -0.015(3) C35 0.082(6) 0.042(4) 0.056(4) 0.002(3) -0.014(4) -0.007(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 1.893(7) . ? Re1 C1 1.909(6) . ? Re1 C2 1.918(6) . ? Re1 N1 2.208(5) . ? Re1 N3 2.198(5) . ? Re1 N2 2.227(5) . ? O1 C1 1.156(8) . ? O2 C2 1.141(8) . ? O3 C3 1.159(8) . ? N1 C7 1.468(8) . ? N2 C5 1.461(9) . ? N2 C6 1.504(9) . ? N3 C33 1.342(7) . ? N3 N31 1.369(6) . ? N31 C31 1.345(8) . ? N31 C4 1.451(8) . ? C4 C5 1.518(11) . ? C6 C7 1.468(10) . ? C31 C32 1.369(10) . ? C31 C35 1.481(9) . ? C32 C33 1.392(9) . ? C33 C34 1.477(9) . ? 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 C1 86.3(3) . . ? C3 Re1 C2 88.7(3) . . ? C1 Re1 C2 87.6(3) . . ? C3 Re1 N1 174.6(2) . . ? C1 Re1 N1 98.9(2) . . ? C2 Re1 N1 93.1(2) . . ? C3 Re1 N3 94.2(2) . . ? C1 Re1 N3 95.2(2) . . ? C2 Re1 N3 176.1(2) . . ? N1 Re1 N3 83.85(19) . . ? C3 Re1 N2 97.3(2) . . ? C1 Re1 N2 176.5(2) . . ? C2 Re1 N2 92.5(2) . . ? N1 Re1 N2 77.53(19) . . ? N3 Re1 N2 84.50(19) . . ? C7 N1 Re1 111.0(4) . . ? C5 N2 C6 112.6(6) . . ? C5 N2 Re1 120.6(4) . . ? C6 N2 Re1 107.5(4) . . ? C33 N3 N31 106.1(5) . . ? C33 N3 Re1 132.9(4) . . ? N31 N3 Re1 120.8(3) . . ? C31 N31 N3 111.0(5) . . ? C31 N31 C4 128.5(5) . . ? N3 N31 C4 120.6(5) . . ? O1 C1 Re1 175.8(6) . . ? O2 C2 Re1 178.0(7) . . ? O3 C3 Re1 179.7(7) . . ? N31 C4 C5 111.1(6) . . ? N2 C5 C4 114.7(6) . . ? C7 C6 N2 109.5(6) . . ? N1 C7 C6 107.7(6) . . ? N31 C31 C32 106.6(5) . . ? N31 C31 C35 122.8(6) . . ? C32 C31 C35 130.5(6) . . ? C33 C32 C31 107.2(5) . . ? N3 C33 C32 109.0(5) . . ? N3 C33 C34 124.0(6) . . ? C32 C33 C34 127.0(6) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.04 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.621 _refine_diff_density_min -1.169 _refine_diff_density_rms 0.137 data_pzsnh2 _database_code_CSD 190656 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety [Re(CO)3(k3-pz(CH2)2S(CH2)2NH2)]Br _chemical_formula_sum 'C12 H17 Br N3 O3 Re S' _chemical_formula_weight 549.46 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' 'Br' 'Br' -0.2901 2.4595 '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)/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 12.7828(15) _cell_length_b 9.3652(9) _cell_length_c 14.9315(19) _cell_angle_alpha 90.00 _cell_angle_beta 111.212(10) _cell_angle_gamma 90.00 _cell_volume 1666.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7.5 _cell_measurement_theta_max 11.4 _exptl_crystal_description 'irregular prism' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.190 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1040 _exptl_absorpt_coefficient_mu 9.826 _exptl_absorpt_correction_type 'empirical via \y-scan North et al(1968)' _exptl_absorpt_correction_T_min 0.4977 _exptl_absorpt_correction_T_max 0.9984 _exptl_absorpt_process_details ? _exptl_special_details ; Crystals were obtained from crystalization in methanol solution ; _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 'CAD4-Enraf-Nonius' _diffrn_measurement_method '\w/2\qscans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% none _diffrn_reflns_number 3743 _diffrn_reflns_av_R_equivalents 0.0438 _diffrn_reflns_av_sigmaI/netI 0.0491 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 26.99 _reflns_number_total 3607 _reflns_number_gt 2710 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 software(Enraf-Nonius,1989)' _computing_cell_refinement 'CAD4 software(Enraf-Nonius,1989)' _computing_data_reduction 'process-MolEN(Fair,1990)' _computing_structure_solution 'SHELXS-97 (Sheldrick,1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3(Farrugia,1997)' _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^)+(0.0459P)^2^+15.5522P] 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 0.00136(19) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3607 _refine_ls_number_parameters 191 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0734 _refine_ls_R_factor_gt 0.0467 _refine_ls_wR_factor_ref 0.1109 _refine_ls_wR_factor_gt 0.0938 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.068 _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 0.74977(3) 0.21981(4) 0.92736(3) 0.02514(14) Uani 1 1 d . . . Br1 Br 0.66491(10) 0.57857(13) 1.12532(8) 0.0437(3) Uani 1 1 d . . . S1 S 0.8017(2) 0.1087(3) 1.08829(18) 0.0306(5) Uani 1 1 d . . . N1 N 0.6095(7) 0.2969(9) 0.9683(6) 0.0279(17) Uani 1 1 d . . . H1A H 0.6270 0.3835 0.9959 0.033 Uiso 1 1 calc R . . H1B H 0.5478 0.3068 0.9150 0.033 Uiso 1 1 calc R . . N2 N 0.6433(7) 0.0306(9) 0.8692(6) 0.0281(18) Uani 1 1 d . . . N21 N 0.6757(7) -0.1065(8) 0.8963(6) 0.0257(17) Uani 1 1 d . . . C5 C 0.5836(9) 0.1975(11) 1.0368(8) 0.035(2) Uani 1 1 d . . . H5A H 0.5256 0.2384 1.0565 0.042 Uiso 1 1 calc R . . H5B H 0.5567 0.1069 1.0055 0.042 Uiso 1 1 calc R . . C23 C 0.5468(8) 0.0199(12) 0.7934(7) 0.033(2) Uani 1 1 d . . . C7 C 0.7748(8) -0.1400(11) 0.9800(7) 0.033(2) Uani 1 1 d . . . H7A H 0.8405 -0.1024 0.9701 0.039 Uiso 1 1 calc R . . H7B H 0.7829 -0.2429 0.9860 0.039 Uiso 1 1 calc R . . C6 C 0.7703(9) -0.0797(11) 1.0726(7) 0.034(2) Uani 1 1 d . . . H6A H 0.8234 -0.1312 1.1263 0.041 Uiso 1 1 calc R . . H6B H 0.6960 -0.0958 1.0740 0.041 Uiso 1 1 calc R . . C4 C 0.6880(9) 0.1749(13) 1.1225(8) 0.041(3) Uani 1 1 d . . . H4A H 0.6730 0.1070 1.1654 0.049 Uiso 1 1 calc R . . H4B H 0.7103 0.2645 1.1568 0.049 Uiso 1 1 calc R . . C21 C 0.6035(9) -0.2010(11) 0.8386(7) 0.031(2) Uani 1 1 d . . . O3 O 0.9594(7) 0.1078(11) 0.8975(6) 0.056(2) Uani 1 1 d . . . O2 O 0.8855(7) 0.4913(10) 1.0067(7) 0.056(2) Uani 1 1 d . . . C25 C 0.6180(11) -0.3601(12) 0.8493(9) 0.046(3) Uani 1 1 d . . . H25A H 0.6850 -0.3814 0.9032 0.069 Uiso 1 1 calc R . . H25B H 0.6240 -0.3995 0.7920 0.069 Uiso 1 1 calc R . . H25C H 0.5544 -0.4010 0.8595 0.069 Uiso 1 1 calc R . . C22 C 0.5211(9) -0.1238(12) 0.7725(8) 0.036(2) Uani 1 1 d . . . H22 H 0.4593 -0.1601 0.7228 0.043 Uiso 1 1 calc R . . C3 C 0.8785(10) 0.1489(12) 0.9064(8) 0.038(2) Uani 1 1 d . . . C2 C 0.8348(9) 0.3908(12) 0.9786(8) 0.034(2) Uani 1 1 d . . . C24 C 0.4784(11) 0.1435(14) 0.7401(9) 0.057(4) Uani 1 1 d . . . H24A H 0.5141 0.2311 0.7686 0.086 Uiso 1 1 calc R . . H24B H 0.4048 0.1388 0.7432 0.086 Uiso 1 1 calc R . . H24C H 0.4725 0.1399 0.6742 0.086 Uiso 1 1 calc R . . C1 C 0.7084(10) 0.3060(14) 0.8039(8) 0.046(3) Uani 1 1 d . . . O1 O 0.6879(8) 0.3607(11) 0.7304(6) 0.064(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 0.0256(2) 0.0230(2) 0.0268(2) 0.00169(18) 0.00946(15) 0.00059(18) Br1 0.0436(6) 0.0384(6) 0.0398(6) -0.0066(5) 0.0038(5) 0.0042(5) S1 0.0292(12) 0.0315(14) 0.0255(12) 0.0001(10) 0.0032(10) -0.0026(11) N1 0.029(4) 0.025(5) 0.025(4) -0.006(3) 0.003(3) -0.004(4) N2 0.023(4) 0.021(4) 0.029(4) 0.004(3) -0.004(3) 0.003(3) N21 0.028(4) 0.018(4) 0.031(4) -0.001(3) 0.010(4) 0.003(3) C5 0.034(5) 0.032(6) 0.041(6) 0.003(5) 0.017(5) -0.003(5) C23 0.026(5) 0.036(6) 0.030(5) -0.002(4) 0.002(4) 0.005(4) C7 0.030(5) 0.025(5) 0.030(5) -0.002(4) -0.005(4) 0.008(4) C6 0.041(6) 0.026(5) 0.023(5) 0.000(4) -0.002(5) -0.002(5) C4 0.043(6) 0.041(6) 0.037(6) -0.006(5) 0.014(5) -0.013(5) C21 0.034(5) 0.029(6) 0.030(5) -0.004(4) 0.011(4) 0.000(4) O3 0.035(4) 0.075(7) 0.062(6) -0.005(5) 0.024(4) 0.010(4) O2 0.050(5) 0.041(5) 0.071(6) -0.007(5) 0.017(5) -0.019(4) C25 0.059(8) 0.028(6) 0.049(7) -0.002(5) 0.015(6) 0.000(6) C22 0.028(5) 0.040(6) 0.033(6) -0.013(5) 0.005(5) -0.008(5) C3 0.042(6) 0.035(6) 0.040(6) 0.003(5) 0.016(5) 0.004(5) C2 0.027(5) 0.035(6) 0.037(6) 0.004(5) 0.007(5) 0.000(5) C24 0.051(8) 0.044(8) 0.052(8) -0.002(6) -0.011(6) 0.021(6) C1 0.040(6) 0.065(9) 0.038(6) 0.001(6) 0.020(5) 0.002(6) O1 0.087(7) 0.075(7) 0.038(5) 0.028(5) 0.033(5) 0.024(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re1 C3 1.903(11) . ? Re1 C1 1.904(12) . ? Re1 C2 1.931(11) . ? Re1 N2 2.212(8) . ? Re1 N1 2.215(8) . ? Re1 S1 2.479(3) . ? S1 C4 1.816(12) . ? S1 C6 1.806(11) . ? N1 C5 1.505(12) . ? N2 C23 1.343(12) . ? N2 N21 1.364(11) . ? N21 C21 1.343(13) . ? N21 C7 1.455(12) . ? C5 C4 1.492(15) . ? C23 C22 1.394(15) . ? C23 C24 1.494(15) . ? C7 C6 1.514(14) . ? C21 C22 1.362(15) . ? C21 C25 1.502(14) . ? O3 C3 1.155(13) . ? O2 C2 1.134(13) . ? C1 O1 1.152(13) . ? 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 C1 86.7(5) . . ? C3 Re1 C2 87.6(5) . . ? C1 Re1 C2 87.2(5) . . ? C3 Re1 N2 95.8(4) . . ? C1 Re1 N2 92.5(4) . . ? C2 Re1 N2 176.5(4) . . ? C3 Re1 N1 173.8(4) . . ? C1 Re1 N1 99.2(4) . . ? C2 Re1 N1 90.9(4) . . ? N2 Re1 N1 85.7(3) . . ? C3 Re1 S1 93.9(3) . . ? C1 Re1 S1 179.4(4) . . ? C2 Re1 S1 92.8(3) . . ? N2 Re1 S1 87.4(2) . . ? N1 Re1 S1 80.2(2) . . ? C4 S1 C6 102.0(5) . . ? C4 S1 Re1 99.7(4) . . ? C6 S1 Re1 108.4(3) . . ? C5 N1 Re1 112.6(6) . . ? C23 N2 N21 105.5(8) . . ? C23 N2 Re1 129.6(7) . . ? N21 N2 Re1 124.0(6) . . ? C21 N21 N2 111.5(8) . . ? C21 N21 C7 126.2(8) . . ? N2 N21 C7 122.3(8) . . ? C4 C5 N1 108.8(8) . . ? N2 C23 C22 109.3(9) . . ? N2 C23 C24 125.0(10) . . ? C22 C23 C24 125.7(10) . . ? N21 C7 C6 113.3(8) . . ? C7 C6 S1 113.7(8) . . ? C5 C4 S1 111.5(8) . . ? N21 C21 C22 106.7(9) . . ? N21 C21 C25 123.8(10) . . ? C22 C21 C25 129.5(10) . . ? C21 C22 C23 107.0(9) . . ? O3 C3 Re1 177.1(11) . . ? O2 C2 Re1 178.3(10) . . ? O1 C1 Re1 177.0(11) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.99 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 2.231 _refine_diff_density_min -1.741 _refine_diff_density_rms 0.228 _eof # End of Crystallographic Information File