Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'Animesh Chakravorty' 'Sangeeta Banerjee' 'Indranil Chakraborty' 'Samir Das' 'Suman Sengupta' _publ_contact_author_name 'Prof Animesh Chakravorty' _publ_contact_author_address ; Department of Inorganic Chemistry Indian Association for the Cultivation of Science Jadavpur Kolkata 700032 INDIA ; _publ_contact_author_email 'ICAC@MAHENDRA.IACS.RES.IN' _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Chemistry of monovalent and bivalent rhenium : synthesis, structure, isomer specificity and metal redox of azoheterocycle complexes ; data_559re _database_code_CSD 192365 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C22 H24 Cl2 N8 Re' _chemical_formula_weight 657.59 _chemical_melting_point ? _chemical_compound_source ? 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Re' 'Re' -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 28.740(16) _cell_length_b 13.454(4) _cell_length_c 13.427(5) _cell_angle_alpha 90.00 _cell_angle_beta 110.86(4) _cell_angle_gamma 90.00 _cell_volume 4851.5(36) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 30 _cell_measurement_theta_min 7 _cell_measurement_theta_max 15 _exptl_crystal_description parallelopiped _exptl_crystal_colour 'dark orange' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.801 _exptl_crystal_density_method ? _exptl_crystal_F_000 2568 _exptl_absorpt_coefficient_mu 5.257 _exptl_absorpt_correction_type 'semi-empirical' _exptl_absorpt_correction_T_min 0.136 _exptl_absorpt_correction_T_max 0.208 _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 'Siemens R3m/V' _diffrn_measurement_method '\w scans' _diffrn_standards_number 2 _diffrn_standards_interval_count 198 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 3750 _diffrn_reflns_av_R_equivalents 0.0476 _diffrn_reflns_av_sigmaI/netI 0.0466 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 23.54 _reflns_number_total 3604 _reflns_number_observed 2718 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens P3/P4-PC V4.27' _computing_cell_refinement 'Siemens P3/P4-PC V4.27' _computing_data_reduction 'Siemens P3/P4-PC V4.27' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL V5.03 PC' _computing_publication_material 'Siemens SHELXTL V5.03 PC' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'Heavy atom method' _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3604 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0642 _refine_ls_R_factor_obs 0.0399 _refine_ls_wR_factor_all 0.1297 _refine_ls_wR_factor_obs 0.1049 _refine_ls_goodness_of_fit_all 0.921 _refine_ls_goodness_of_fit_obs 0.868 _refine_ls_restrained_S_all 0.921 _refine_ls_restrained_S_obs 0.868 _refine_ls_shift/esd_max -0.008 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Re Re 0.376787(14) 0.28869(3) 0.40822(3) 0.0343(2) Uani 1 d . . Cl1 Cl 0.42259(11) 0.3352(2) 0.5876(2) 0.0564(8) Uani 1 d . . Cl2 Cl 0.31968(11) 0.4241(2) 0.3855(2) 0.0515(7) Uani 1 d . . N1 N 0.3345(3) 0.2030(6) 0.4706(7) 0.037(2) Uani 1 d . . N4 N 0.3286(3) 0.2155(6) 0.2838(7) 0.038(2) Uani 1 d . . N5 N 0.4200(3) 0.3862(6) 0.3622(6) 0.039(2) Uani 1 d . . N8 N 0.4321(3) 0.2058(6) 0.3954(7) 0.039(2) Uani 1 d . . N3 N 0.2929(3) 0.1574(7) 0.2922(7) 0.042(2) Uani 1 d . . N2 N 0.2668(3) 0.1150(7) 0.4390(7) 0.047(2) Uani 1 d . . N7 N 0.4730(3) 0.2461(7) 0.3850(7) 0.042(2) Uani 1 d . . N6 N 0.4984(3) 0.4162(7) 0.3732(7) 0.044(2) Uani 1 d . . C1 C 0.3271(4) 0.1875(8) 0.5637(8) 0.045(3) Uani 1 d . . H1A H 0.3474(4) 0.2111(8) 0.6301(8) 0.054 Uiso 1 calc R . C2 C 0.2858(4) 0.1327(9) 0.5447(9) 0.051(3) Uani 1 d . . H2A H 0.2728(4) 0.1110(9) 0.5951(9) 0.061 Uiso 1 calc R . C3 C 0.2967(3) 0.1560(7) 0.3945(8) 0.036(2) Uani 1 d . . C4 C 0.2219(4) 0.0600(10) 0.3817(10) 0.063(3) Uani 1 d . . H4A H 0.2065(4) 0.0382(10) 0.4306(10) 0.094 Uiso 1 calc R . H4B H 0.2303(4) 0.0032(10) 0.3480(10) 0.094 Uiso 1 calc R . H4C H 0.1993(4) 0.1020(10) 0.3285(10) 0.094 Uiso 1 calc R . C5 C 0.3273(4) 0.2144(8) 0.1762(8) 0.039(2) Uani 1 d . . C6 C 0.3220(4) 0.1246(9) 0.1199(9) 0.057(3) Uani 1 d . . H6A H 0.3212(4) 0.0640(9) 0.1526(9) 0.069 Uiso 1 calc R . C7 C 0.3179(5) 0.1292(11) 0.0143(9) 0.064(3) Uani 1 d . . H7A H 0.3144(5) 0.0700(11) -0.0234(9) 0.077 Uiso 1 calc R . C8 C 0.3188(5) 0.2161(11) -0.0376(10) 0.058(3) Uani 1 d . . C9 C 0.3263(4) 0.3022(10) 0.0187(11) 0.060(4) Uani 1 d . . H9A H 0.3284(4) 0.3620(10) -0.0142(11) 0.072 Uiso 1 calc R . C10 C 0.3309(4) 0.3016(9) 0.1259(10) 0.053(3) Uani 1 d . . H10A H 0.3366(4) 0.3610(9) 0.1637(10) 0.064 Uiso 1 calc R . C11 C 0.3109(6) 0.2128(13) -0.1546(10) 0.088(5) Uani 1 d . . H11A H 0.3059(6) 0.1452(13) -0.1790(10) 0.132 Uiso 1 calc R . H11B H 0.3396(6) 0.2394(13) -0.1657(10) 0.132 Uiso 1 calc R . H11C H 0.2822(6) 0.2517(13) -0.1935(10) 0.132 Uiso 1 calc R . C12 C 0.4252(4) 0.4875(7) 0.3514(9) 0.044(3) Uani 1 d . . H12A H 0.4005(4) 0.5350(7) 0.3416(9) 0.052 Uiso 1 calc R . C13 C 0.4735(4) 0.5057(9) 0.3577(9) 0.051(3) Uani 1 d . . H13A H 0.4869(4) 0.5676(9) 0.3524(9) 0.061 Uiso 1 calc R . C14 C 0.4648(4) 0.3456(8) 0.3760(8) 0.041(3) Uani 1 d . . C15 C 0.5521(4) 0.3964(9) 0.3929(10) 0.056(3) Uani 1 d . . H15A H 0.5682(4) 0.4574(9) 0.3870(10) 0.084 Uiso 1 calc R . H15B H 0.5548(4) 0.3497(9) 0.3413(10) 0.084 Uiso 1 calc R . H15C H 0.5677(4) 0.3695(9) 0.4632(10) 0.084 Uiso 1 calc R . C16 C 0.4325(4) 0.0999(7) 0.3851(8) 0.039(2) Uani 1 d . . C17 C 0.4239(4) 0.0382(8) 0.4582(9) 0.050(3) Uani 1 d . . H17A H 0.4158(4) 0.0654(8) 0.5136(9) 0.060 Uiso 1 calc R . C18 C 0.4270(4) -0.0627(9) 0.4504(10) 0.058(3) Uani 1 d . . H18A H 0.4215(4) -0.1032(9) 0.5013(10) 0.069 Uiso 1 calc R . C19 C 0.4383(4) -0.1055(8) 0.3677(9) 0.050(3) Uani 1 d . . C20 C 0.4448(4) -0.0425(9) 0.2914(9) 0.055(3) Uani 1 d . . H20A H 0.4508(4) -0.0698(9) 0.2335(9) 0.066 Uiso 1 calc R . C21 C 0.4426(5) 0.0578(10) 0.2996(9) 0.059(3) Uani 1 d . . H21A H 0.4477(5) 0.0985(10) 0.2485(9) 0.071 Uiso 1 calc R . C22 C 0.4436(6) -0.2162(9) 0.3599(13) 0.079(5) Uani 1 d . . H22A H 0.4516(6) -0.2315(9) 0.2981(13) 0.118 Uiso 1 calc R . H22B H 0.4128(6) -0.2479(9) 0.3543(13) 0.118 Uiso 1 calc R . H22C H 0.4697(6) -0.2398(9) 0.4226(13) 0.118 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re 0.0331(3) 0.0355(3) 0.0374(3) -0.0010(2) 0.0162(2) -0.0069(2) Cl1 0.056(2) 0.068(2) 0.044(2) -0.0062(14) 0.0169(13) -0.0258(15) Cl2 0.053(2) 0.044(2) 0.068(2) 0.0030(14) 0.0352(15) 0.0023(13) N1 0.027(4) 0.035(5) 0.050(5) 0.012(4) 0.017(4) -0.004(4) N4 0.040(5) 0.035(5) 0.039(5) 0.001(4) 0.016(4) 0.001(4) N5 0.039(5) 0.041(5) 0.040(5) 0.007(4) 0.018(4) 0.002(4) N8 0.040(5) 0.034(5) 0.040(5) -0.003(4) 0.012(4) -0.005(4) N3 0.039(5) 0.045(5) 0.049(5) 0.002(4) 0.021(4) -0.008(4) N2 0.048(6) 0.050(6) 0.051(6) -0.001(5) 0.027(5) -0.013(4) N7 0.030(5) 0.046(5) 0.053(5) -0.003(4) 0.020(4) -0.012(4) N6 0.035(5) 0.052(6) 0.052(5) 0.001(4) 0.026(4) -0.013(4) C1 0.039(6) 0.058(7) 0.036(6) 0.010(5) 0.010(5) -0.009(5) C2 0.054(7) 0.056(7) 0.053(7) 0.006(6) 0.032(6) -0.012(6) C3 0.029(5) 0.028(6) 0.052(7) -0.002(5) 0.014(5) -0.006(4) C4 0.054(7) 0.071(9) 0.070(8) -0.008(7) 0.029(6) -0.029(7) C5 0.039(6) 0.042(6) 0.036(6) -0.002(5) 0.012(5) 0.000(5) C6 0.077(8) 0.055(8) 0.041(6) -0.009(6) 0.023(6) -0.015(7) C7 0.075(9) 0.072(9) 0.043(7) -0.021(7) 0.017(6) -0.003(7) C8 0.047(7) 0.084(10) 0.049(7) 0.011(7) 0.026(6) 0.011(7) C9 0.052(7) 0.064(9) 0.067(9) 0.034(7) 0.023(6) 0.014(6) C10 0.050(7) 0.054(8) 0.058(8) 0.005(6) 0.023(6) 0.005(6) C11 0.088(11) 0.139(16) 0.036(7) 0.014(8) 0.022(7) 0.034(10) C12 0.055(7) 0.028(6) 0.053(7) -0.003(5) 0.025(6) -0.008(5) C13 0.065(8) 0.047(7) 0.045(7) -0.003(5) 0.025(6) -0.019(6) C14 0.046(7) 0.046(7) 0.033(6) 0.007(5) 0.018(5) -0.005(5) C15 0.042(6) 0.069(8) 0.063(8) 0.004(6) 0.025(6) -0.015(6) C16 0.040(6) 0.036(6) 0.044(6) 0.002(5) 0.017(5) 0.004(5) C17 0.060(7) 0.047(7) 0.050(7) 0.000(5) 0.028(6) -0.003(6) C18 0.071(8) 0.043(7) 0.064(8) -0.001(6) 0.029(7) -0.001(6) C19 0.044(6) 0.034(6) 0.057(7) 0.002(5) 0.000(5) 0.002(5) C20 0.074(8) 0.049(8) 0.050(7) -0.010(6) 0.032(6) 0.013(6) C21 0.070(8) 0.065(9) 0.045(7) 0.011(6) 0.025(6) 0.003(7) C22 0.087(11) 0.045(8) 0.082(10) -0.014(7) 0.004(8) 0.025(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 Re N8 1.999(8) . y Re N4 2.007(8) . y Re N5 2.046(8) . y Re N1 2.057(7) . y Re Cl1 2.381(3) . y Re Cl2 2.398(3) . y N1 C3 1.356(12) . ? N1 C1 1.357(13) . ? N4 N3 1.328(11) . y N4 C5 1.431(13) . ? N5 C14 1.351(13) . ? N5 C12 1.384(12) . ? N8 N7 1.345(11) . y N8 C16 1.432(13) . ? N3 C3 1.338(13) . ? N2 C3 1.329(12) . ? N2 C2 1.348(14) . ? N2 C4 1.447(13) . ? N7 C14 1.357(14) . ? N6 C14 1.364(13) . ? N6 C13 1.379(14) . ? N6 C15 1.493(13) . ? C1 C2 1.342(14) . ? C5 C10 1.376(15) . ? C5 C6 1.405(15) . ? C6 C7 1.38(2) . ? C7 C8 1.37(2) . ? C8 C9 1.36(2) . ? C8 C11 1.50(2) . ? C9 C10 1.40(2) . ? C12 C13 1.38(2) . ? C16 C17 1.374(14) . ? C16 C21 1.40(2) . ? C17 C18 1.37(2) . ? C18 C19 1.39(2) . ? C19 C20 1.39(2) . ? C19 C22 1.505(15) . ? C20 C21 1.36(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N8 Re N4 89.4(3) . . y N8 Re N5 75.2(3) . . y N4 Re N5 112.0(3) . . y N8 Re N1 109.0(3) . . y N4 Re N1 74.5(3) . . y N5 Re N1 172.6(3) . . y N8 Re Cl1 93.6(3) . . y N4 Re Cl1 160.1(2) . . y N5 Re Cl1 87.8(2) . . y N1 Re Cl1 85.9(2) . . y N8 Re Cl2 160.4(2) . . y N4 Re Cl2 91.7(2) . . y N5 Re Cl2 86.3(2) . . y N1 Re Cl2 90.1(2) . . y Cl1 Re Cl2 92.04(12) . . y C3 N1 C1 106.0(8) . . ? C3 N1 Re 112.7(7) . . ? C1 N1 Re 140.4(7) . . ? N3 N4 C5 109.7(8) . . ? N3 N4 Re 122.9(6) . . ? C5 N4 Re 127.4(7) . . ? C14 N5 C12 106.1(9) . . ? C14 N5 Re 110.6(6) . . ? C12 N5 Re 139.7(7) . . ? N7 N8 C16 110.6(8) . . ? N7 N8 Re 122.3(6) . . ? C16 N8 Re 126.7(7) . . ? N4 N3 C3 108.3(8) . . ? C3 N2 C2 108.4(9) . . ? C3 N2 C4 124.7(9) . . ? C2 N2 C4 127.0(9) . . ? N8 N7 C14 106.1(8) . . ? C14 N6 C13 106.1(8) . . ? C14 N6 C15 124.6(9) . . ? C13 N6 C15 129.1(9) . . ? N1 C1 C2 109.1(10) . . ? N2 C2 C1 107.3(9) . . ? N2 C3 N3 129.6(9) . . ? N2 C3 N1 109.2(9) . . ? N3 C3 N1 121.1(9) . . ? C10 C5 C6 118.8(10) . . ? C10 C5 N4 120.5(9) . . ? C6 C5 N4 120.7(9) . . ? C7 C6 C5 117.8(11) . . ? C6 C7 C8 123.5(12) . . ? C9 C8 C7 118.3(11) . . ? C9 C8 C11 122.8(13) . . ? C7 C8 C11 118.9(13) . . ? C8 C9 C10 120.4(11) . . ? C5 C10 C9 121.0(12) . . ? N5 C12 C13 108.3(10) . . ? N6 C13 C12 108.0(9) . . ? N5 C14 N7 122.4(9) . . ? N5 C14 N6 111.5(9) . . ? N7 C14 N6 126.0(9) . . ? C17 C16 C21 119.0(10) . . ? C17 C16 N8 121.4(10) . . ? C21 C16 N8 119.6(10) . . ? C16 C17 C18 120.8(11) . . ? C19 C18 C17 120.9(12) . . ? C18 C19 C20 117.8(10) . . ? C18 C19 C22 121.6(12) . . ? C20 C19 C22 120.6(12) . . ? C21 C20 C19 121.5(11) . . ? C20 C21 C16 119.9(11) . . ? _refine_diff_density_max 2.238 _refine_diff_density_min -0.616 _refine_diff_density_rms 0.134 #end# data_647re _database_code_CSD 192366 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C34 H32 I2 N8 Re' _chemical_formula_weight 992.68 _chemical_melting_point ? _chemical_compound_source ? 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' 'I' 'I' -0.4742 1.8119 '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)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.946(2) _cell_length_b 18.790(4) _cell_length_c 17.394(4) _cell_angle_alpha 90.00 _cell_angle_beta 99.60(3) _cell_angle_gamma 90.00 _cell_volume 3527.4(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 30 _cell_measurement_theta_min 7 _cell_measurement_theta_max 15 _exptl_crystal_description parallelopiped _exptl_crystal_colour 'dark orange' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.869 _exptl_crystal_density_method ? _exptl_crystal_F_000 1892 _exptl_absorpt_coefficient_mu 5.231 _exptl_absorpt_correction_type 'semi-empirical' _exptl_absorpt_correction_T_min 0.195 _exptl_absorpt_correction_T_max 0.254 _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 'Siemens R3m/V' _diffrn_measurement_method '\w scans' _diffrn_standards_number 2 _diffrn_standards_interval_count 198 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 5684 _diffrn_reflns_av_R_equivalents 0.0376 _diffrn_reflns_av_sigmaI/netI 0.0630 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 23.55 _reflns_number_total 5257 _reflns_number_observed 3631 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens P3/P4-PC V4.27' _computing_cell_refinement 'Siemens P3/P4-PC V4.27' _computing_data_reduction 'Siemens P3/P4-PC V4.27' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL V5.03 PC' _computing_publication_material 'Siemens SHELXTL V5.03 PC' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 2 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0482P)^2^+6.8352P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'Heavy atom method' _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5255 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0876 _refine_ls_R_factor_obs 0.0483 _refine_ls_wR_factor_all 0.1206 _refine_ls_wR_factor_obs 0.0955 _refine_ls_goodness_of_fit_all 1.044 _refine_ls_goodness_of_fit_obs 1.093 _refine_ls_restrained_S_all 1.128 _refine_ls_restrained_S_obs 1.093 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Re Re 0.86780(4) 0.15984(2) 0.15158(3) 0.0433(2) Uani 1 d . . I2 I 0.68059(7) 0.07996(4) 0.06952(5) 0.0616(3) Uani 1 d . . I1 I 0.92174(10) 0.06727(5) 0.27282(5) 0.0839(3) Uani 1 d . . N1 N 0.9956(7) 0.1072(4) 0.0974(5) 0.044(2) Uani 1 d . . N2 N 1.0854(9) 0.0974(5) -0.0069(6) 0.056(3) Uani 1 d . . N3 N 0.9481(8) 0.1956(4) 0.0013(5) 0.043(2) Uani 1 d . . N4 N 0.8803(8) 0.2178(4) 0.0540(5) 0.043(2) Uani 1 d . . N5 N 0.7386(7) 0.2048(4) 0.2098(5) 0.043(2) Uani 1 d . . N6 N 0.7034(9) 0.2805(5) 0.3023(5) 0.054(2) Uani 1 d . . N7 N 0.9010(8) 0.2815(5) 0.2600(5) 0.047(2) Uani 1 d . . N8 N 0.9570(8) 0.2411(5) 0.2106(5) 0.046(2) Uani 1 d . . C1 C 1.0737(11) 0.0503(6) 0.1076(7) 0.060(3) Uani 1 d . . H1A H 1.0879(11) 0.0206(6) 0.1509(7) 0.072 Uiso 1 calc R . C2 C 1.1271(12) 0.0450(7) 0.0425(8) 0.066(4) Uani 1 d . . H2A H 1.1837(12) 0.0103(7) 0.0338(8) 0.079 Uiso 1 calc R . C3 C 1.0060(10) 0.1354(6) 0.0282(6) 0.046(3) Uani 1 d . . C4 C 0.8357(9) 0.2890(5) 0.0386(6) 0.038(2) Uani 1 d . . C5 C 0.9084(12) 0.3360(6) 0.0048(7) 0.070(4) Uani 1 d . . H5A H 0.9838(12) 0.3216(6) -0.0079(7) 0.084 Uiso 1 calc R . C6 C 0.8655(16) 0.4054(7) -0.0098(8) 0.095(5) Uani 1 d . . H6A H 0.9099(16) 0.4366(7) -0.0362(8) 0.114 Uiso 1 calc R . C7 C 0.7609(16) 0.4281(7) 0.0137(9) 0.090(5) Uani 1 d . . C8 C 0.6900(13) 0.3809(6) 0.0477(8) 0.076(4) Uani 1 d . . H8A H 0.6157(13) 0.3958(6) 0.0618(8) 0.091 Uiso 1 calc R . C9 C 0.7294(11) 0.3110(6) 0.0609(7) 0.057(3) Uani 1 d . . H9A H 0.6827(11) 0.2794(6) 0.0852(7) 0.068 Uiso 1 calc R . C10 C 0.7106(20) 0.5036(8) -0.0052(11) 0.164(10) Uani 1 d . . H10A H 0.6360(20) 0.5101(8) 0.0162(11) 0.246 Uiso 1 calc R . H10B H 0.6930(20) 0.5099(8) -0.0607(11) 0.246 Uiso 1 calc R . H10C H 0.7713(20) 0.5379(8) 0.0172(11) 0.246 Uiso 1 calc R . C11 C 1.1246(11) 0.1146(6) -0.0812(6) 0.062(3) Uani 1 d . . H11A H 1.0523(11) 0.1268(6) -0.1191(6) 0.075 Uiso 1 calc R . H11B H 1.1622(11) 0.0728(6) -0.1001(6) 0.075 Uiso 1 calc R . C12 C 1.2153(11) 0.1751(6) -0.0748(6) 0.048(3) Uani 1 d . . C13 C 1.1770(13) 0.2411(8) -0.1021(7) 0.073(4) Uani 1 d . . H13A H 1.0944(13) 0.2493(8) -0.1233(7) 0.088 Uiso 1 calc R . C14 C 1.2623(17) 0.2952(8) -0.0978(9) 0.089(4) Uani 1 d . . H14A H 1.2365(17) 0.3399(8) -0.1172(9) 0.106 Uiso 1 calc R . C15 C 1.3838(17) 0.2854(10) -0.0660(9) 0.091(5) Uani 1 d . . H15A H 1.4395(17) 0.3230(10) -0.0636(9) 0.110 Uiso 1 calc R . C16 C 1.4232(14) 0.2202(11) -0.0375(9) 0.091(5) Uani 1 d . . H16A H 1.5056(14) 0.2133(11) -0.0151(9) 0.109 Uiso 1 calc R . C17 C 1.3387(13) 0.1635(8) -0.0421(8) 0.080(4) Uani 1 d . . H17A H 1.3648(13) 0.1186(8) -0.0236(8) 0.095 Uiso 1 calc R . C18 C 0.5996(12) 0.2410(7) 0.2797(7) 0.063(3) Uani 1 d . . H18A H 0.5258(12) 0.2455(7) 0.2991(7) 0.075 Uiso 1 calc R . C19 C 0.6205(10) 0.1942(6) 0.2248(7) 0.054(3) Uani 1 d . . H19A H 0.5646(10) 0.1604(6) 0.2010(7) 0.065 Uiso 1 calc R . C20 C 0.7880(10) 0.2572(6) 0.2590(6) 0.047(3) Uani 1 d . . C21 C 1.0721(11) 0.2698(6) 0.1982(6) 0.051(3) Uani 1 d . . C22 C 1.1658(10) 0.2244(6) 0.1862(6) 0.056(3) Uani 1 d . . H22A H 1.1558(10) 0.1754(6) 0.1902(6) 0.068 Uiso 1 calc R . C23 C 1.2739(11) 0.2516(8) 0.1684(7) 0.066(4) Uani 1 d . . H23A H 1.3363(11) 0.2204(8) 0.1599(7) 0.080 Uiso 1 calc R . C24 C 1.2922(11) 0.3225(8) 0.1628(7) 0.063(4) Uani 1 d . . C25 C 1.1994(12) 0.3682(7) 0.1787(7) 0.062(3) Uani 1 d . . H25A H 1.2123(12) 0.4171(7) 0.1781(7) 0.074 Uiso 1 calc R . C26 C 1.0892(11) 0.3425(7) 0.1954(7) 0.063(3) Uani 1 d . . H26A H 1.0272(11) 0.3736(7) 0.2046(7) 0.075 Uiso 1 calc R . C27 C 1.4095(11) 0.3516(8) 0.1391(8) 0.083(4) Uani 1 d . . H27A H 1.4063(11) 0.4026(8) 0.1384(8) 0.124 Uiso 1 calc R . H27B H 1.4167(11) 0.3343(8) 0.0881(8) 0.124 Uiso 1 calc R . H27C H 1.4799(11) 0.3362(8) 0.1759(8) 0.124 Uiso 1 calc R . C28 C 0.7151(12) 0.3429(7) 0.3524(7) 0.071(4) Uani 1 d . . H28A H 0.8017(12) 0.3496(7) 0.3746(7) 0.086 Uiso 1 calc R . H28B H 0.6697(12) 0.3349(7) 0.3949(7) 0.086 Uiso 1 calc R . C29 C 0.6672(12) 0.4091(7) 0.3094(7) 0.063(3) Uani 1 d . . C30 C 0.7332(14) 0.4389(8) 0.2570(9) 0.080(4) Uani 1 d . . H30A H 0.8065(14) 0.4178(8) 0.2481(9) 0.096 Uiso 1 calc R . C31 C 0.6916(19) 0.4992(9) 0.2181(10) 0.110(6) Uani 1 d . . H31A H 0.7361(19) 0.5186(9) 0.1820(10) 0.132 Uiso 1 calc R . C32 C 0.5862(22) 0.5317(9) 0.2310(12) 0.133(8) Uani 1 d . . H32A H 0.5594(22) 0.5735(9) 0.2050(12) 0.160 Uiso 1 calc R . C33 C 0.5213(20) 0.5023(11) 0.2819(11) 0.131(7) Uani 1 d . . H33A H 0.4470(20) 0.5231(11) 0.2893(11) 0.157 Uiso 1 calc R . C34 C 0.5626(16) 0.4419(9) 0.3234(9) 0.099(5) Uani 1 d . . H34A H 0.5191(16) 0.4237(9) 0.3606(9) 0.119 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re 0.0504(3) 0.0382(2) 0.0457(3) 0.0054(2) 0.0205(2) 0.0080(2) I2 0.0632(5) 0.0527(5) 0.0746(6) -0.0115(4) 0.0285(4) -0.0042(4) I1 0.1086(8) 0.0783(6) 0.0733(6) 0.0371(5) 0.0398(6) 0.0332(6) N1 0.043(5) 0.044(5) 0.048(6) 0.001(4) 0.016(4) 0.007(4) N2 0.070(7) 0.040(5) 0.064(6) -0.011(5) 0.026(6) 0.007(5) N3 0.049(6) 0.043(5) 0.042(5) -0.005(4) 0.020(5) 0.000(5) N4 0.044(5) 0.047(5) 0.041(5) 0.005(4) 0.012(4) -0.002(4) N5 0.039(5) 0.045(5) 0.048(5) 0.005(5) 0.018(4) 0.005(4) N6 0.050(6) 0.061(6) 0.053(6) 0.000(5) 0.016(5) 0.008(5) N7 0.036(5) 0.063(6) 0.041(5) -0.010(5) 0.007(4) 0.005(5) N8 0.043(5) 0.059(6) 0.040(5) 0.006(4) 0.015(4) 0.013(5) C1 0.070(8) 0.039(6) 0.078(9) 0.019(6) 0.032(7) 0.016(6) C2 0.069(9) 0.052(8) 0.083(10) -0.014(7) 0.030(8) 0.015(7) C3 0.051(7) 0.042(6) 0.049(7) -0.003(5) 0.018(6) 0.005(6) C4 0.048(7) 0.033(6) 0.035(6) 0.011(5) 0.011(5) 0.004(5) C5 0.078(9) 0.057(8) 0.083(9) 0.009(7) 0.040(8) 0.019(7) C6 0.160(16) 0.050(8) 0.095(11) 0.029(8) 0.078(11) 0.023(9) C7 0.141(14) 0.051(8) 0.089(11) 0.029(8) 0.051(10) 0.028(9) C8 0.086(10) 0.061(9) 0.086(10) 0.023(7) 0.031(8) 0.041(8) C9 0.063(8) 0.057(7) 0.059(8) 0.013(6) 0.034(6) 0.010(6) C10 0.250(25) 0.085(12) 0.183(20) 0.076(13) 0.111(19) 0.094(15) C11 0.067(8) 0.077(9) 0.055(8) -0.024(7) 0.041(7) 0.001(7) C12 0.052(7) 0.058(8) 0.038(6) -0.005(5) 0.013(6) 0.010(6) C13 0.081(10) 0.088(11) 0.054(8) -0.003(8) 0.017(7) 0.000(9) C14 0.108(13) 0.081(11) 0.077(11) 0.017(9) 0.017(10) -0.006(11) C15 0.101(14) 0.110(14) 0.066(10) -0.015(10) 0.023(10) -0.048(12) C16 0.054(9) 0.134(15) 0.089(12) -0.015(11) 0.022(8) -0.007(11) C17 0.068(9) 0.094(11) 0.079(10) 0.000(9) 0.020(8) 0.018(9) C18 0.067(9) 0.070(9) 0.059(8) 0.009(7) 0.032(7) 0.020(7) C19 0.052(7) 0.059(7) 0.057(8) 0.003(6) 0.024(6) 0.005(6) C20 0.042(7) 0.055(7) 0.047(7) 0.005(6) 0.014(6) 0.011(6) C21 0.059(8) 0.053(7) 0.040(7) -0.006(5) 0.009(6) -0.003(6) C22 0.049(7) 0.060(8) 0.061(8) 0.000(6) 0.010(6) 0.002(6) C23 0.046(8) 0.084(10) 0.069(9) 0.004(7) 0.007(7) 0.005(7) C24 0.040(7) 0.087(11) 0.058(8) 0.007(7) -0.001(6) 0.000(7) C25 0.070(9) 0.054(7) 0.059(8) 0.005(6) 0.005(7) -0.004(7) C26 0.064(8) 0.066(8) 0.063(8) -0.005(7) 0.026(6) 0.003(7) C27 0.054(8) 0.112(12) 0.083(10) 0.017(9) 0.011(7) -0.007(8) C28 0.075(9) 0.093(10) 0.050(7) -0.045(8) 0.019(6) 0.008(8) C29 0.082(10) 0.057(8) 0.052(8) -0.014(6) 0.019(7) 0.015(7) C30 0.087(11) 0.066(10) 0.091(11) -0.014(8) 0.025(9) -0.008(8) C31 0.146(17) 0.082(12) 0.116(14) -0.013(11) 0.061(13) -0.016(12) C32 0.212(25) 0.076(12) 0.122(16) 0.006(11) 0.060(17) 0.031(14) C33 0.177(20) 0.119(16) 0.112(15) 0.002(13) 0.072(15) 0.057(15) C34 0.141(15) 0.088(11) 0.080(11) -0.009(9) 0.053(11) 0.036(11) _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 Re N8 2.000(9) . y Re N4 2.041(8) . y Re N5 2.053(8) . y Re N1 2.065(8) . y Re I1 2.7214(10) . y Re I2 2.7412(12) . y N1 C3 1.338(12) . ? N1 C1 1.362(12) . ? N2 C3 1.347(12) . ? N2 C2 1.337(14) . ? N2 C11 1.463(13) . ? N3 C3 1.341(12) . ? N3 N4 1.339(10) . y N4 C4 1.433(12) . ? N5 C20 1.358(13) . ? N5 C19 1.375(12) . ? N6 C20 1.361(12) . ? N6 C18 1.360(15) . ? N6 C28 1.452(13) . ? N7 C20 1.315(13) . ? N7 N8 1.366(11) . y N8 C21 1.420(13) . ? C1 C2 1.361(15) . ? C4 C9 1.351(13) . ? C4 C5 1.383(14) . ? C5 C6 1.40(2) . ? C6 C7 1.35(2) . ? C7 C8 1.38(2) . ? C7 C10 1.54(2) . ? C8 C9 1.390(15) . ? C11 C12 1.501(15) . ? C12 C13 1.37(2) . ? C12 C17 1.39(2) . ? C13 C14 1.37(2) . ? C14 C15 1.37(2) . ? C15 C16 1.36(2) . ? C16 C17 1.41(2) . ? C18 C19 1.346(15) . ? C21 C22 1.377(15) . ? C21 C26 1.38(2) . ? C22 C23 1.37(2) . ? C23 C24 1.35(2) . ? C24 C25 1.39(2) . ? C24 C27 1.51(2) . ? C25 C26 1.37(2) . ? C28 C29 1.50(2) . ? C29 C34 1.36(2) . ? C29 C30 1.37(2) . ? C30 C31 1.36(2) . ? C31 C32 1.36(2) . ? C32 C33 1.34(2) . ? C33 C34 1.38(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N8 Re N4 85.7(3) . . y N8 Re N5 75.6(3) . . y N4 Re N5 109.7(3) . . y N8 Re N1 106.8(3) . . y N4 Re N1 74.4(3) . . y N5 Re N1 175.5(3) . . y N8 Re I1 93.8(2) . . y N4 Re I1 161.8(2) . . y N5 Re I1 87.6(2) . . y N1 Re I1 88.4(2) . . y N8 Re I2 160.6(2) . . y N4 Re I2 90.4(2) . . y N5 Re I2 88.0(3) . . y N1 Re I2 90.3(2) . . y I1 Re I2 95.75(4) . . y C3 N1 C1 106.4(8) . . ? C3 N1 Re 112.7(7) . . ? C1 N1 Re 140.8(7) . . ? C3 N2 C2 106.0(9) . . ? C3 N2 C11 126.2(10) . . ? C2 N2 C11 127.7(10) . . ? C3 N3 N4 108.0(8) . . ? N3 N4 C4 112.0(8) . . ? N3 N4 Re 121.6(6) . . ? C4 N4 Re 125.8(6) . . ? C20 N5 C19 105.9(9) . . ? C20 N5 Re 112.0(6) . . ? C19 N5 Re 141.3(8) . . ? C20 N6 C18 106.1(10) . . ? C20 N6 C28 126.3(10) . . ? C18 N6 C28 126.9(10) . . ? C20 N7 N8 108.6(9) . . ? N7 N8 C21 112.8(9) . . ? N7 N8 Re 121.0(7) . . ? C21 N8 Re 125.6(7) . . ? N1 C1 C2 107.2(10) . . ? N2 C2 C1 109.5(10) . . ? N3 C3 N1 122.8(9) . . ? N3 C3 N2 126.3(10) . . ? N1 C3 N2 110.9(10) . . ? C9 C4 C5 120.7(10) . . ? C9 C4 N4 121.0(9) . . ? C5 C4 N4 118.2(9) . . ? C4 C5 C6 118.3(11) . . ? C7 C6 C5 121.2(12) . . ? C6 C7 C8 119.7(12) . . ? C6 C7 C10 121.3(13) . . ? C8 C7 C10 118.6(14) . . ? C7 C8 C9 119.9(12) . . ? C4 C9 C8 120.0(11) . . ? N2 C11 C12 112.9(9) . . ? C13 C12 C17 120.2(12) . . ? C13 C12 C11 120.0(11) . . ? C17 C12 C11 119.7(12) . . ? C12 C13 C14 119.1(13) . . ? C15 C14 C13 121.9(15) . . ? C16 C15 C14 119.8(15) . . ? C15 C16 C17 119.7(14) . . ? C16 C17 C12 119.3(14) . . ? C19 C18 N6 109.2(10) . . ? C18 C19 N5 108.5(11) . . ? N7 C20 N5 122.3(9) . . ? N7 C20 N6 127.4(11) . . ? N5 C20 N6 110.3(9) . . ? C22 C21 C26 119.9(11) . . ? C22 C21 N8 119.3(10) . . ? C26 C21 N8 120.7(10) . . ? C21 C22 C23 119.7(12) . . ? C24 C23 C22 121.9(12) . . ? C23 C24 C25 118.0(12) . . ? C23 C24 C27 121.2(12) . . ? C25 C24 C27 120.8(12) . . ? C26 C25 C24 121.4(12) . . ? C25 C26 C21 118.9(11) . . ? N6 C28 C29 112.4(10) . . ? C34 C29 C30 119.2(14) . . ? C34 C29 C28 121.4(13) . . ? C30 C29 C28 119.3(12) . . ? C31 C30 C29 120.0(14) . . ? C30 C31 C32 121.1(17) . . ? C33 C32 C31 118.9(19) . . ? C32 C33 C34 121.3(18) . . ? C29 C34 C33 119.4(16) . . ? _refine_diff_density_max 1.031 _refine_diff_density_min -0.774 _refine_diff_density_rms 0.137 #end# data_802re _database_code_CSD 192367 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C22 H16 Cl4 N6 Re' _chemical_formula_weight 692.41 _chemical_melting_point ? _chemical_compound_source ? 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Re' 'Re' -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 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 8.532(6) _cell_length_b 22.793(8) _cell_length_c 12.417(3) _cell_angle_alpha 90.00 _cell_angle_beta 100.22(4) _cell_angle_gamma 90.00 _cell_volume 2376.5(20) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 30 _cell_measurement_theta_min 7 _cell_measurement_theta_max 15 _exptl_crystal_description parallelopiped _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.935 _exptl_crystal_density_method ? _exptl_crystal_F_000 1332 _exptl_absorpt_coefficient_mu 5.587 _exptl_absorpt_correction_type 'semi-empirical' _exptl_absorpt_correction_T_min 0.167 _exptl_absorpt_correction_T_max 0.277 _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 'Siemens R3m/V' _diffrn_measurement_method '\w scans' _diffrn_standards_number 2 _diffrn_standards_interval_count 198 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 4464 _diffrn_reflns_av_R_equivalents 0.0658 _diffrn_reflns_av_sigmaI/netI 0.0807 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -4 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 24.99 _reflns_number_total 4165 _reflns_number_observed 2829 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens P3/P4-PC V4.27' _computing_cell_refinement 'Siemens P3/P4-PC V4.27' _computing_data_reduction 'Siemens P3/P4-PC V4.27' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL V5.03 PC' _computing_publication_material 'Siemens SHELXTL V5.03 PC' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 3 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0840P)^2^+11.1090P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4162 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1040 _refine_ls_R_factor_obs 0.0616 _refine_ls_wR_factor_all 0.1687 _refine_ls_wR_factor_obs 0.1386 _refine_ls_goodness_of_fit_all 1.063 _refine_ls_goodness_of_fit_obs 1.090 _refine_ls_restrained_S_all 1.079 _refine_ls_restrained_S_obs 1.090 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Re1 Re -0.06513(7) 1.18468(2) -0.43001(4) 0.0311(2) Uani 1 d . . Cl1 Cl -0.2156(5) 1.2697(2) -0.4938(3) 0.0502(10) Uani 1 d . . Cl2 Cl 0.1559(5) 1.2444(2) -0.3545(3) 0.0499(10) Uani 1 d . . Cl3 Cl -0.5455(6) 1.0139(2) -0.8652(3) 0.0694(13) Uani 1 d . . Cl4 Cl 0.1314(7) 0.9460(2) -0.0454(4) 0.083(2) Uani 1 d . . N1 N -0.1506(14) 1.1830(5) -0.2842(9) 0.037(3) Uani 1 d . . N2 N -0.3460(14) 1.1236(5) -0.3809(9) 0.042(3) Uani 1 d . . N3 N -0.2589(13) 1.1333(5) -0.4568(9) 0.032(3) Uani 1 d . . N4 N 0.0288(12) 1.1783(5) -0.5719(8) 0.031(3) Uani 1 d . . N5 N 0.1760(14) 1.1020(5) -0.4767(10) 0.045(3) Uani 1 d . . N6 N 0.0756(12) 1.1159(5) -0.4106(9) 0.035(3) Uani 1 d . . C1 C -0.0922(20) 1.2084(7) -0.1873(12) 0.048(4) Uani 1 d . . H1A H -0.0026(20) 1.2320(7) -0.1835(12) 0.058 Uiso 1 calc R . C2 C -0.1543(22) 1.2021(8) -0.0957(12) 0.055(5) Uani 1 d . . H2A H -0.1022(22) 1.2179(8) -0.0299(12) 0.066 Uiso 1 calc R . C3 C -0.2946(21) 1.1723(7) -0.0996(11) 0.050(4) Uani 1 d . . H3A H -0.3444(21) 1.1706(7) -0.0388(11) 0.060 Uiso 1 calc R . C4 C -0.3584(21) 1.1453(8) -0.1941(13) 0.057(4) Uani 1 d . . H4A H -0.4512(21) 1.1234(8) -0.1983(13) 0.068 Uiso 1 calc R . C5 C -0.2838(20) 1.1507(7) -0.2863(11) 0.045(4) Uani 1 d . . C6 C -0.3161(17) 1.1032(7) -0.5555(12) 0.040(3) Uani 1 d . . C7 C -0.3374(16) 1.1335(7) -0.6541(11) 0.038(3) Uani 1 d . . H7A H -0.3080(16) 1.1727(7) -0.6557(11) 0.046 Uiso 1 calc R . C8 C -0.4022(18) 1.1051(7) -0.7495(13) 0.045(4) Uani 1 d . . H8A H -0.4146(18) 1.1249(7) -0.8159(13) 0.054 Uiso 1 calc R . C9 C -0.4491(17) 1.0471(7) -0.7465(11) 0.043(4) Uani 1 d . . C10 C -0.4258(17) 1.0161(7) -0.6517(12) 0.044(4) Uani 1 d . . H10A H -0.4542(17) 0.9767(7) -0.6513(12) 0.052 Uiso 1 calc R . C11 C -0.3587(16) 1.0443(6) -0.5552(12) 0.040(3) Uani 1 d . . H11A H -0.3422(16) 1.0236(6) -0.4896(12) 0.048 Uiso 1 calc R . C12 C -0.0091(19) 1.2094(7) -0.6675(11) 0.045(4) Uani 1 d . . H12A H -0.0913(19) 1.2367(7) -0.6738(11) 0.054 Uiso 1 calc R . C13 C 0.0685(21) 1.2021(8) -0.7543(12) 0.059(5) Uani 1 d . . H13A H 0.0365(21) 1.2220(8) -0.8199(12) 0.070 Uiso 1 calc R . C14 C 0.2007(19) 1.1627(8) -0.7397(13) 0.052(4) Uani 1 d . . H14A H 0.2612(19) 1.1592(8) -0.7947(13) 0.063 Uiso 1 calc R . C15 C 0.2395(18) 1.1306(8) -0.6483(14) 0.052(4) Uani 1 d . . H15A H 0.3223(18) 1.1035(8) -0.6408(14) 0.062 Uiso 1 calc R . C16 C 0.1521(17) 1.1391(6) -0.5649(11) 0.038(3) Uani 1 d . . C17 C 0.0872(16) 1.0742(7) -0.3192(11) 0.038(3) Uani 1 d . . C22 C 0.1565(20) 1.0917(8) -0.2163(12) 0.055(5) Uani 1 d . . H22A H 0.1973(20) 1.1294(8) -0.2039(12) 0.067 Uiso 1 calc R . C21 C 0.1645(22) 1.0518(8) -0.1304(13) 0.060(5) Uani 1 d . . H21A H 0.2080(22) 1.0630(8) -0.0594(13) 0.072 Uiso 1 calc R . C20 C 0.1100(20) 0.9978(8) -0.1504(13) 0.053(4) Uani 1 d . . C19 C 0.0405(21) 0.9803(7) -0.2530(13) 0.056(5) Uani 1 d . . H19A H 0.0009(21) 0.9423(7) -0.2645(13) 0.068 Uiso 1 calc R . C18 C 0.0293(18) 1.0184(7) -0.3385(12) 0.049(4) Uani 1 d . . H18A H -0.0169(18) 1.0068(7) -0.4087(12) 0.059 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.0378(3) 0.0303(3) 0.0258(3) -0.0012(3) 0.0071(2) 0.0002(3) Cl1 0.067(3) 0.042(2) 0.043(2) 0.000(2) 0.013(2) 0.014(2) Cl2 0.057(2) 0.053(2) 0.037(2) -0.003(2) 0.002(2) -0.018(2) Cl3 0.086(3) 0.070(3) 0.047(2) -0.018(2) -0.004(2) -0.010(3) Cl4 0.114(4) 0.073(3) 0.062(3) 0.038(3) 0.013(3) 0.004(3) N1 0.050(7) 0.033(6) 0.029(6) 0.006(5) 0.005(5) 0.011(6) N2 0.053(8) 0.035(7) 0.042(7) -0.016(6) 0.020(6) -0.012(6) N3 0.047(7) 0.023(6) 0.032(6) 0.000(5) 0.019(5) 0.002(5) N4 0.034(6) 0.031(6) 0.027(5) -0.004(5) -0.001(5) -0.004(5) N5 0.051(8) 0.038(7) 0.050(7) 0.011(6) 0.021(6) -0.002(6) N6 0.024(6) 0.045(7) 0.040(6) -0.001(6) 0.019(5) -0.013(5) C1 0.065(11) 0.049(9) 0.033(8) -0.002(7) 0.012(7) 0.002(8) C2 0.069(12) 0.067(12) 0.031(8) 0.000(8) 0.013(8) 0.011(9) C3 0.079(12) 0.049(10) 0.026(7) -0.003(7) 0.023(8) 0.009(9) C4 0.061(11) 0.062(12) 0.051(10) -0.006(9) 0.020(8) 0.003(9) C5 0.063(11) 0.045(10) 0.029(7) 0.004(7) 0.012(7) -0.001(8) C6 0.042(8) 0.037(8) 0.044(8) -0.009(7) 0.013(7) -0.003(7) C7 0.037(8) 0.043(9) 0.034(7) -0.004(7) 0.005(6) -0.009(7) C8 0.046(9) 0.044(9) 0.046(9) -0.004(7) 0.009(7) 0.005(7) C9 0.044(9) 0.051(10) 0.035(8) -0.008(7) 0.007(6) -0.001(7) C10 0.047(9) 0.036(8) 0.046(9) -0.010(7) 0.003(7) 0.000(7) C11 0.039(8) 0.035(8) 0.045(8) 0.002(7) 0.002(6) -0.002(7) C12 0.051(9) 0.049(9) 0.035(8) 0.008(7) 0.005(7) -0.002(8) C13 0.067(12) 0.076(13) 0.030(8) 0.009(8) 0.003(8) -0.017(10) C14 0.047(10) 0.069(12) 0.041(9) -0.002(8) 0.013(7) 0.000(9) C15 0.039(9) 0.058(11) 0.066(11) 0.003(9) 0.028(8) 0.002(8) C16 0.045(9) 0.036(8) 0.035(8) -0.005(6) 0.010(6) 0.001(7) C17 0.034(8) 0.045(9) 0.035(7) 0.000(7) 0.005(6) 0.004(7) C22 0.070(12) 0.053(11) 0.036(8) 0.005(8) -0.010(8) -0.011(9) C21 0.081(13) 0.057(11) 0.035(8) 0.010(8) -0.006(8) 0.002(10) C20 0.058(10) 0.055(11) 0.049(10) 0.032(9) 0.013(8) 0.004(9) C19 0.072(12) 0.039(9) 0.054(10) 0.017(8) 0.001(9) -0.018(8) C18 0.048(9) 0.063(11) 0.035(8) 0.005(8) 0.002(7) -0.013(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 N6 1.964(12) . y Re1 N3 2.006(11) . y Re1 N4 2.066(10) . y Re1 N1 2.069(11) . y Re1 Cl2 2.380(4) . y Re1 Cl1 2.382(4) . y Cl3 C9 1.729(14) . ? Cl4 C20 1.744(14) . ? N1 C5 1.35(2) . ? N1 C1 1.35(2) . ? N2 N3 1.319(14) . y N2 C5 1.35(2) . ? N3 C6 1.41(2) . ? N4 C16 1.37(2) . ? N4 C12 1.37(2) . ? N5 N6 1.325(15) . y N5 C16 1.37(2) . ? N6 C17 1.47(2) . ? C1 C2 1.35(2) . ? C2 C3 1.37(2) . ? C3 C4 1.35(2) . ? C4 C5 1.41(2) . ? C6 C7 1.39(2) . ? C6 C11 1.39(2) . ? C7 C8 1.38(2) . ? C8 C9 1.38(2) . ? C9 C10 1.36(2) . ? C10 C11 1.39(2) . ? C12 C13 1.37(2) . ? C13 C14 1.43(2) . ? C14 C15 1.34(2) . ? C15 C16 1.39(2) . ? C17 C22 1.37(2) . ? C17 C18 1.37(2) . ? C22 C21 1.39(2) . ? C21 C20 1.32(2) . ? C20 C19 1.37(2) . ? C19 C18 1.36(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N6 Re1 N3 91.3(4) . . y N6 Re1 N4 74.1(4) . . y N3 Re1 N4 104.5(4) . . y N6 Re1 N1 100.4(4) . . y N3 Re1 N1 74.1(4) . . y N4 Re1 N1 174.4(4) . . y N6 Re1 Cl2 89.1(3) . . y N3 Re1 Cl2 166.4(3) . . y N4 Re1 Cl2 88.7(3) . . y N1 Re1 Cl2 92.5(4) . . y N6 Re1 Cl1 166.5(3) . . y N3 Re1 Cl1 92.3(3) . . y N4 Re1 Cl1 92.4(3) . . y N1 Re1 Cl1 93.1(3) . . y Cl2 Re1 Cl1 90.5(2) . . y C5 N1 C1 115.4(12) . . ? C5 N1 Re1 114.8(9) . . ? C1 N1 Re1 129.9(11) . . ? N3 N2 C5 111.1(12) . . ? N2 N3 C6 112.8(11) . . ? N2 N3 Re1 122.1(9) . . ? C6 N3 Re1 125.1(9) . . ? C16 N4 C12 116.9(12) . . ? C16 N4 Re1 113.7(8) . . ? C12 N4 Re1 129.3(10) . . ? N6 N5 C16 109.0(12) . . ? N5 N6 C17 111.1(11) . . ? N5 N6 Re1 124.3(9) . . ? C17 N6 Re1 124.5(8) . . ? C2 C1 N1 124.7(16) . . ? C1 C2 C3 119.7(16) . . ? C4 C3 C2 118.1(14) . . ? C3 C4 C5 119.7(16) . . ? N1 C5 N2 117.8(12) . . ? N1 C5 C4 122.0(14) . . ? N2 C5 C4 120.1(15) . . ? C7 C6 C11 119.2(13) . . ? C7 C6 N3 119.6(13) . . ? C11 C6 N3 121.1(13) . . ? C8 C7 C6 119.6(14) . . ? C7 C8 C9 120.0(15) . . ? C10 C9 C8 121.5(14) . . ? C10 C9 Cl3 119.1(12) . . ? C8 C9 Cl3 119.4(12) . . ? C9 C10 C11 118.8(14) . . ? C10 C11 C6 120.8(14) . . ? C13 C12 N4 123.0(15) . . ? C12 C13 C14 117.2(15) . . ? C15 C14 C13 121.5(15) . . ? C14 C15 C16 117.9(15) . . ? N4 C16 N5 117.1(12) . . ? N4 C16 C15 123.4(14) . . ? N5 C16 C15 119.0(14) . . ? C22 C17 C18 121.1(14) . . ? C22 C17 N6 119.4(13) . . ? C18 C17 N6 119.5(12) . . ? C17 C22 C21 118.6(16) . . ? C20 C21 C22 119.7(15) . . ? C21 C20 C19 121.8(14) . . ? C21 C20 Cl4 120.2(14) . . ? C19 C20 Cl4 118.0(13) . . ? C20 C19 C18 119.9(15) . . ? C19 C18 C17 118.9(14) . . ? _refine_diff_density_max 2.687 _refine_diff_density_min -1.353 _refine_diff_density_rms 0.224 #end# data_papt _database_code_CSD 192368 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C33 H27 N9 O4 Re2' _chemical_formula_weight 986.04 _chemical_melting_point ? _chemical_compound_source ? 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 Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 12.876(10) _cell_length_b 22.313(10) _cell_length_c 10.938(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.08(6) _cell_angle_gamma 90.00 _cell_volume 3142.5(33) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 30 _cell_measurement_theta_min 7 _cell_measurement_theta_max 15 _exptl_crystal_description parallelopiped _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.084 _exptl_crystal_density_method ? _exptl_crystal_F_000 1880 _exptl_absorpt_coefficient_mu 7.752 _exptl_absorpt_correction_type 'semi-empirical' _exptl_absorpt_correction_T_min 0.166 _exptl_absorpt_correction_T_max 0.259 _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 'Siemens R3m/V' _diffrn_measurement_method '\w scans' _diffrn_standards_number 2 _diffrn_standards_interval_count 198 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 7382 _diffrn_reflns_av_R_equivalents 0.0435 _diffrn_reflns_av_sigmaI/netI 0.0441 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 27.51 _reflns_number_total 3733 _reflns_number_observed 3106 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens P3/P4-PC V4.27' _computing_cell_refinement 'Siemens P3/P4-PC V4.27' _computing_data_reduction 'Siemens P3/P4-PC V4.27' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL V5.03 PC' _computing_publication_material 'Siemens SHELXTL V5.03 PC' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 17 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0293P)^2^+3.2556P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'Heavy atom method' _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00148(5) _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 -0.003(12) _refine_ls_number_reflns 3716 _refine_ls_number_parameters 432 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0388 _refine_ls_R_factor_obs 0.0243 _refine_ls_wR_factor_all 0.1160 _refine_ls_wR_factor_obs 0.0557 _refine_ls_goodness_of_fit_all 1.171 _refine_ls_goodness_of_fit_obs 1.140 _refine_ls_restrained_S_all 2.139 _refine_ls_restrained_S_obs 1.140 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Re1 Re 0.0000 0.166669(14) 0.0000 0.02602(8) Uani 1 d . . Re2 Re 0.00001(7) 0.50000(2) 0.01650(5) 0.03577(10) Uani 1 d . . N1 N -0.1045(6) 0.1137(3) -0.1023(7) 0.031(2) Uani 1 d . . N2 N -0.0853(6) 0.0489(3) 0.0644(8) 0.033(2) Uani 1 d . . N3 N -0.0149(5) 0.0908(3) 0.0922(6) 0.028(2) Uani 1 d . . N4 N -0.0259(5) 0.2450(3) -0.1005(7) 0.030(2) Uani 1 d . . N5 N -0.1340(6) 0.2679(3) 0.0669(8) 0.035(2) Uani 1 d . . N6 N -0.1070(5) 0.2125(3) 0.0921(7) 0.029(2) Uani 1 d . . N7 N 0.1312(6) 0.1409(3) -0.1015(7) 0.0289(15) Uani 1 d . . N8 N 0.2194(6) 0.1830(4) 0.0660(8) 0.035(2) Uani 1 d . . N9 N 0.1223(5) 0.1974(3) 0.0914(6) 0.0268(14) Uani 1 d . . O1 O 0.0774(8) 0.4434(5) 0.0681(10) 0.087(3) Uani 1 d . . O2 O -0.0006(9) 0.5000(6) -0.1391(8) 0.099(3) Uani 1 d . . O3 O 0.0472(9) 0.5669(4) 0.0684(10) 0.087(3) Uani 1 d . . O4 O -0.1235(6) 0.4901(6) 0.0677(10) 0.092(4) Uani 1 d . . C1 C -0.1428(8) 0.1239(5) -0.2164(10) 0.040(2) Uani 1 d . . H1 H -0.1229(8) 0.1584(5) -0.2580(10) 0.080 Uiso 1 calc R . C2 C -0.2097(8) 0.0850(5) -0.2714(10) 0.046(2) Uani 1 d . . H2 H -0.2313(8) 0.0919(5) -0.3513(10) 0.080 Uiso 1 calc R . C3 C -0.2455(8) 0.0355(5) -0.2096(11) 0.045(3) Uani 1 d . . H3 H -0.2953(8) 0.0107(5) -0.2444(11) 0.080 Uiso 1 calc R . C4 C -0.2058(7) 0.0233(4) -0.0940(10) 0.041(2) Uani 1 d . . H4 H -0.2268(7) -0.0105(4) -0.0509(10) 0.080 Uiso 1 calc R . C5 C -0.1342(7) 0.0626(4) -0.0450(8) 0.034(2) Uani 1 d . . C6 C 0.0446(8) 0.0736(4) 0.2000(10) 0.036(2) Uani 1 d . . C7 C 0.1485(8) 0.0580(4) 0.1853(9) 0.038(2) Uani 1 d . . H7 H 0.1793(8) 0.0588(4) 0.1085(9) 0.080 Uiso 1 calc R . C8 C 0.2039(8) 0.0415(5) 0.2851(11) 0.043(2) Uani 1 d . . H8 H 0.2732(8) 0.0308(5) 0.2760(11) 0.080 Uiso 1 calc R . C9 C 0.1598(9) 0.0402(5) 0.3999(9) 0.048(3) Uani 1 d . . H9 H 0.1991(9) 0.0289(5) 0.4675(9) 0.080 Uiso 1 calc R . C10 C 0.0555(9) 0.0560(5) 0.4136(10) 0.053(3) Uani 1 d . . H10 H 0.0251(9) 0.0559(5) 0.4906(10) 0.080 Uiso 1 calc R . C11 C -0.0022(9) 0.0717(5) 0.3121(10) 0.046(3) Uani 1 d . . H11 H -0.0723(9) 0.0810(5) 0.3199(10) 0.080 Uiso 1 calc R . C12 C 0.0062(11) 0.2590(4) -0.2163(12) 0.042(2) Uani 1 d . . H12 H 0.0456(11) 0.2312(4) -0.2593(12) 0.080 Uiso 1 calc R . C13 C -0.0173(8) 0.3117(5) -0.2706(9) 0.044(2) Uani 1 d . . H13 H 0.0062(8) 0.3194(5) -0.3494(9) 0.080 Uiso 1 calc R . C14 C -0.0766(10) 0.3548(5) -0.2095(12) 0.050(3) Uani 1 d . . H14 H -0.0910(10) 0.3917(5) -0.2454(12) 0.080 Uiso 1 calc R . C15 C -0.1129(9) 0.3411(4) -0.0953(11) 0.047(2) Uani 1 d . . H15 H -0.1525(9) 0.3687(4) -0.0520(11) 0.080 Uiso 1 calc R . C16 C -0.0896(7) 0.2850(4) -0.0441(8) 0.033(2) Uani 1 d . . C17 C -0.1625(6) 0.1911(4) 0.1997(8) 0.029(2) Uani 1 d . . C18 C -0.1410(8) 0.2148(5) 0.3121(10) 0.043(2) Uani 1 d . . H18 H -0.0906(8) 0.2444(5) 0.3205(10) 0.080 Uiso 1 calc R . C19 C -0.1944(10) 0.1946(6) 0.4126(10) 0.055(3) Uani 1 d . . H19 H -0.1807(10) 0.2109(6) 0.4893(10) 0.080 Uiso 1 calc R . C20 C -0.2695(9) 0.1498(5) 0.4000(9) 0.049(3) Uani 1 d . . H20 H -0.3048(9) 0.1356(5) 0.4682(9) 0.080 Uiso 1 calc R . C21 C -0.2909(8) 0.1266(5) 0.2846(10) 0.041(2) Uani 1 d . . H21 H -0.3413(8) 0.0971(5) 0.2758(10) 0.080 Uiso 1 calc R . C22 C -0.2380(7) 0.1470(4) 0.1831(9) 0.035(2) Uani 1 d . . H22 H -0.2522(7) 0.1317(4) 0.1057(9) 0.080 Uiso 1 calc R . C23 C 0.1358(9) 0.1164(5) -0.2157(10) 0.039(2) Uani 1 d . . H23 H 0.0740(9) 0.1089(5) -0.2571(10) 0.080 Uiso 1 calc R . C24 C 0.2269(9) 0.1027(5) -0.2713(10) 0.050(3) Uani 1 d . . H24 H 0.2272(9) 0.0882(5) -0.3510(10) 0.080 Uiso 1 calc R . C25 C 0.3206(10) 0.1105(6) -0.2078(12) 0.054(3) Uani 1 d . . H25 H 0.3835(10) 0.0989(6) -0.2420(12) 0.080 Uiso 1 calc R . C26 C 0.3167(7) 0.1353(5) -0.0959(10) 0.043(2) Uani 1 d . . H26 H 0.3778(7) 0.1410(5) -0.0521(10) 0.080 Uiso 1 calc R . C27 C 0.2212(8) 0.1527(4) -0.0439(8) 0.035(2) Uani 1 d . . C28 C 0.1176(7) 0.2359(4) 0.1994(9) 0.033(2) Uani 1 d . . C29 C 0.1421(8) 0.2134(5) 0.3122(10) 0.044(3) Uani 1 d . . H29 H 0.1604(8) 0.1733(5) 0.3212(10) 0.080 Uiso 1 calc R . C30 C 0.1394(9) 0.2510(6) 0.4131(10) 0.056(3) Uani 1 d . . H30 H 0.1576(9) 0.2366(6) 0.4899(10) 0.080 Uiso 1 calc R . C31 C 0.1095(8) 0.3100(6) 0.3987(10) 0.050(3) Uani 1 d . . H31 H 0.1061(8) 0.3352(6) 0.4663(10) 0.080 Uiso 1 calc R . C32 C 0.0850(9) 0.3313(5) 0.2860(11) 0.046(3) Uani 1 d . . H32 H 0.0656(9) 0.3712(5) 0.2773(11) 0.080 Uiso 1 calc R . C33 C 0.0884(7) 0.2948(4) 0.1842(9) 0.035(2) Uani 1 d . . H33 H 0.0715(7) 0.3097(4) 0.1073(9) 0.080 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.02798(13) 0.02823(13) 0.02184(13) -0.00023(12) 0.00006(10) 0.0002(2) Re2 0.0355(2) 0.0360(2) 0.0358(2) 0.0000(2) -0.0012(2) 0.0003(3) N1 0.028(3) 0.036(4) 0.029(4) -0.003(3) -0.002(3) 0.002(3) N2 0.035(4) 0.029(4) 0.036(4) -0.001(3) 0.000(3) -0.003(3) N3 0.031(4) 0.030(4) 0.024(3) 0.004(3) -0.003(3) 0.003(3) N4 0.028(4) 0.033(4) 0.029(4) 0.003(3) -0.005(3) -0.002(3) N5 0.033(4) 0.031(4) 0.039(4) 0.002(4) 0.001(3) 0.003(3) N6 0.027(3) 0.030(4) 0.029(3) -0.002(3) -0.011(3) -0.003(3) N7 0.031(4) 0.028(3) 0.028(3) -0.003(3) 0.000(3) 0.002(3) N8 0.029(4) 0.036(4) 0.040(4) -0.006(4) -0.005(3) -0.001(3) N9 0.022(3) 0.032(4) 0.026(3) -0.003(3) -0.006(3) 0.001(3) O1 0.095(7) 0.078(7) 0.087(7) -0.007(6) -0.016(6) 0.047(6) O2 0.130(9) 0.118(8) 0.047(5) 0.001(7) -0.027(6) 0.012(10) O3 0.127(9) 0.056(5) 0.076(7) -0.013(5) 0.013(6) -0.036(6) O4 0.038(4) 0.154(11) 0.085(7) 0.022(8) 0.011(4) -0.013(6) C1 0.043(6) 0.044(6) 0.033(5) 0.001(5) -0.007(4) -0.003(5) C2 0.040(5) 0.058(7) 0.039(5) -0.008(5) -0.011(4) 0.004(5) C3 0.036(5) 0.045(6) 0.055(6) -0.010(5) -0.018(5) -0.008(5) C4 0.034(5) 0.041(5) 0.049(5) -0.003(4) -0.002(4) -0.003(4) C5 0.031(4) 0.032(4) 0.039(4) -0.003(4) -0.002(4) 0.006(4) C6 0.043(5) 0.026(4) 0.039(5) 0.004(4) -0.004(4) 0.002(4) C7 0.045(5) 0.033(5) 0.036(5) -0.001(4) 0.000(4) 0.003(4) C8 0.035(5) 0.035(5) 0.058(6) 0.009(5) -0.012(5) 0.000(4) C9 0.053(6) 0.050(6) 0.041(5) 0.008(5) -0.018(5) -0.007(5) C10 0.061(7) 0.066(7) 0.032(5) 0.011(5) -0.003(5) -0.016(6) C11 0.036(5) 0.057(6) 0.044(6) 0.003(5) -0.009(5) -0.006(5) C12 0.056(6) 0.038(5) 0.031(5) 0.004(5) 0.009(4) 0.004(6) C13 0.044(5) 0.052(6) 0.036(4) 0.009(5) 0.001(4) -0.010(5) C14 0.052(6) 0.035(5) 0.063(7) 0.017(5) -0.012(6) -0.007(5) C15 0.048(6) 0.034(5) 0.059(6) 0.008(5) -0.006(5) -0.001(5) C16 0.031(4) 0.033(5) 0.036(4) 0.000(4) -0.005(3) -0.001(4) C17 0.021(4) 0.037(5) 0.029(4) 0.001(4) -0.002(3) 0.004(4) C18 0.051(6) 0.043(6) 0.036(6) 0.001(5) 0.008(5) -0.002(5) C19 0.076(8) 0.059(7) 0.029(5) -0.001(5) 0.018(5) 0.009(6) C20 0.057(6) 0.056(6) 0.035(5) 0.012(5) 0.008(4) 0.017(5) C21 0.029(5) 0.042(6) 0.052(6) 0.010(5) 0.012(4) 0.005(4) C22 0.026(4) 0.039(5) 0.039(5) 0.001(4) 0.009(4) 0.001(4) C23 0.046(6) 0.037(5) 0.033(5) -0.008(4) 0.001(4) -0.003(5) C24 0.066(7) 0.044(6) 0.041(5) -0.008(5) 0.013(5) 0.006(6) C25 0.049(6) 0.050(7) 0.062(7) 0.000(6) 0.020(6) 0.001(6) C26 0.032(5) 0.047(6) 0.051(5) -0.004(5) 0.003(4) 0.009(4) C27 0.041(5) 0.027(4) 0.037(4) -0.002(4) 0.012(4) -0.003(4) C28 0.032(4) 0.036(5) 0.030(5) -0.009(4) 0.008(4) -0.009(4) C29 0.049(6) 0.047(6) 0.036(5) -0.007(5) -0.007(5) 0.007(5) C30 0.060(7) 0.081(8) 0.027(5) -0.008(6) -0.007(5) -0.003(6) C31 0.047(6) 0.058(6) 0.044(5) -0.025(5) 0.003(4) -0.006(5) C32 0.042(5) 0.036(5) 0.061(6) -0.020(5) 0.007(5) -0.012(5) C33 0.032(4) 0.034(5) 0.039(5) 0.001(4) -0.002(4) -0.005(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 N3 1.979(7) . y Re1 N9 1.986(7) . y Re1 N6 1.991(8) . y Re1 N4 2.092(7) . y Re1 N7 2.103(7) . y Re1 N1 2.111(7) . y Re2 O4 1.702(8) . y Re2 O2 1.702(8) . y Re2 O1 1.705(9) . y Re2 O3 1.709(9) . y N1 C5 1.356(12) . ? N1 C1 1.361(13) . ? N2 N3 1.337(10) . y N2 C5 1.386(11) . ? N3 C6 1.458(11) . ? N4 C16 1.359(12) . ? N4 C12 1.370(14) . ? N5 N6 1.313(10) . y N5 C16 1.396(12) . ? N6 C17 1.458(11) . ? N7 C27 1.344(12) . ? N7 C23 1.364(12) . ? N8 N9 1.321(10) . y N8 C27 1.380(12) . ? N9 C28 1.461(11) . ? C1 C2 1.363(14) . ? C2 C3 1.37(2) . ? C3 C4 1.389(15) . ? C4 C5 1.380(13) . ? C6 C11 1.37(2) . ? C6 C7 1.391(14) . ? C7 C8 1.353(13) . ? C8 C9 1.38(2) . ? C9 C10 1.40(2) . ? C10 C11 1.380(14) . ? C12 C13 1.350(14) . ? C13 C14 1.40(2) . ? C14 C15 1.37(2) . ? C15 C16 1.404(13) . ? C17 C18 1.366(13) . ? C17 C22 1.395(14) . ? C18 C19 1.374(15) . ? C19 C20 1.40(2) . ? C20 C21 1.39(2) . ? C21 C22 1.381(13) . ? C23 C24 1.357(15) . ? C24 C25 1.40(2) . ? C25 C26 1.34(2) . ? C26 C27 1.411(13) . ? C28 C29 1.369(14) . ? C28 C33 1.378(14) . ? C29 C30 1.39(2) . ? C30 C31 1.38(2) . ? C31 C32 1.36(2) . ? C32 C33 1.380(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 N3 Re1 N9 96.7(3) . . y N3 Re1 N6 96.5(3) . . y N9 Re1 N6 96.7(3) . . y N3 Re1 N4 165.2(3) . . y N9 Re1 N4 95.8(3) . . y N6 Re1 N4 74.1(3) . . y N3 Re1 N7 96.5(3) . . y N9 Re1 N7 73.9(3) . . y N6 Re1 N7 164.7(3) . . y N4 Re1 N7 94.6(3) . . y N3 Re1 N1 74.3(3) . . y N9 Re1 N1 164.7(3) . . y N6 Re1 N1 96.6(3) . . y N4 Re1 N1 95.1(3) . . y N7 Re1 N1 94.5(3) . . y O4 Re2 O2 109.0(5) . . y O4 Re2 O1 109.9(6) . . y O2 Re2 O1 109.4(6) . . y O4 Re2 O3 109.7(6) . . y O2 Re2 O3 109.5(6) . . y O1 Re2 O3 109.3(5) . . y C5 N1 C1 117.5(8) . . ? C5 N1 Re1 113.9(6) . . ? C1 N1 Re1 128.5(7) . . ? N3 N2 C5 110.4(7) . . ? N2 N3 C6 110.8(7) . . ? N2 N3 Re1 123.3(5) . . ? C6 N3 Re1 126.0(6) . . ? C16 N4 C12 116.9(8) . . ? C16 N4 Re1 114.0(6) . . ? C12 N4 Re1 128.9(6) . . ? N6 N5 C16 109.3(8) . . ? N5 N6 C17 110.4(8) . . ? N5 N6 Re1 124.1(6) . . ? C17 N6 Re1 125.5(6) . . ? C27 N7 C23 118.0(8) . . ? C27 N7 Re1 113.0(6) . . ? C23 N7 Re1 128.9(6) . . ? N9 N8 C27 108.6(7) . . ? N8 N9 C28 110.6(7) . . ? N8 N9 Re1 124.1(6) . . ? C28 N9 Re1 125.2(5) . . ? N1 C1 C2 121.8(10) . . ? C1 C2 C3 120.4(10) . . ? C2 C3 C4 118.8(9) . . ? C5 C4 C3 118.3(10) . . ? N1 C5 C4 122.9(9) . . ? N1 C5 N2 117.2(8) . . ? C4 C5 N2 119.8(9) . . ? C11 C6 C7 121.4(9) . . ? C11 C6 N3 120.0(8) . . ? C7 C6 N3 118.5(9) . . ? C8 C7 C6 118.7(10) . . ? C7 C8 C9 121.5(10) . . ? C8 C9 C10 119.3(9) . . ? C11 C10 C9 119.7(10) . . ? C6 C11 C10 119.4(10) . . ? C13 C12 N4 122.5(10) . . ? C12 C13 C14 120.7(10) . . ? C15 C14 C13 118.0(10) . . ? C14 C15 C16 119.4(11) . . ? N4 C16 N5 117.6(8) . . ? N4 C16 C15 122.2(9) . . ? N5 C16 C15 120.2(9) . . ? C18 C17 C22 122.1(9) . . ? C18 C17 N6 120.1(8) . . ? C22 C17 N6 117.9(8) . . ? C17 C18 C19 119.5(10) . . ? C18 C19 C20 120.2(11) . . ? C21 C20 C19 119.5(10) . . ? C22 C21 C20 120.7(10) . . ? C21 C22 C17 118.2(9) . . ? C24 C23 N7 122.6(10) . . ? C23 C24 C25 119.6(11) . . ? C26 C25 C24 117.9(10) . . ? C25 C26 C27 121.0(10) . . ? N7 C27 N8 119.3(8) . . ? N7 C27 C26 120.5(8) . . ? N8 C27 C26 120.1(9) . . ? C29 C28 C33 121.4(9) . . ? C29 C28 N9 120.3(9) . . ? C33 C28 N9 118.3(9) . . ? C28 C29 C30 119.3(10) . . ? C31 C30 C29 119.6(10) . . ? C32 C31 C30 120.1(10) . . ? C31 C32 C33 121.2(10) . . ? C28 C33 C32 118.3(10) . . ? _refine_diff_density_max 2.346 _refine_diff_density_min -2.375 _refine_diff_density_rms 0.179 #end#