# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2001 data_paper _journal_coden_Cambridge 440 _publ_contact_author ; Dr Patrick Batail Laboratoire Sciences Mol\'eculaires aux Interfaces Institut Jean Rouxel CNRS FRE 2068, 2, rue de la Houssini\`ere 44322 Nantes cedex 03, France ; _publ_contact_author_email batail@cnrs-imn.fr _publ_contact_author_fax '33 2 40 37 64 34' _publ_contact_author_phone '33 2 40 37 39 51' _publ_requested_journal 'New Journal of Chemistry' _publ_requested_category FM loop_ _publ_author_name _publ_author_address 'Uriel, Santiago' ; Laboratoire Sciences Mol\'eculaires aux Interfaces Institut Jean Rouxel CNRS FRE 2068, 2, rue de la Houssini\`ere 44322 Nantes cedex 03, France ; 'Boubekeur, Kamal' ; Laboratoire Sciences Mol\'eculaires aux Interfaces Institut Jean Rouxel CNRS FRE 2068, 2, rue de la Houssini\`ere 44322 Nantes cedex 03, France ; 'Batail, Patrick' ; Laboratoire Sciences Mol\'eculaires aux Interfaces Institut Jean Rouxel CNRS FRE 2068, 2, rue de la Houssini\`ere 44322 Nantes cedex 03, France ; 'Orduna, Jesus' ; Instituto de Ciencia de Materiales de Aragon Universidad de Zaragoza 50009 Zaragoza, Spain ; 'Perrin, Andre' ; Laboratoire de Chimie Min\'erale B CNRS UMR6511, Universit\'e de Rennes 1 35042 Rennes, France ; _publ_section_title ; Inertness of the [Re6Se5Cl3]5+ cluster core to substitution with OH- in organic solutions: synthesis, structural and liquid secondary ion mass spectroscopy characterisation of K(H2O)2[Re6Se5Cl9] and (nBu4N)[Re6Se5Cl9], and the crystal structure of (nBu4N)2[Re6Se6Cl8] ; #################### Material relevant to compound 1 #################### data_kreoh _database_code_CSD 146272 _audit_creation_method SHELXL-97 _chemical_name_systematic ; potassium penta-\m~eq~3-seleno-tri-\m~eq~3-chloro- hexachloro-octahedro-hexarhenate(III) dihydrate ; _chemical_name_common 'K[Re6Se5Cl9](H2O)2' _chemical_formula_moiety 'K 1+, Re6 Se5 Cl9 1-, (H2O)2' _chemical_formula_structural 'K (Re6Se5Cl9)(H2O)2' _chemical_formula_sum 'H4 Cl9 K O2 Re6 Se5' _chemical_formula_weight 1906.18 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'K' 'K' 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Se' 'Se' -0.0929 2.2259 '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 Rhombohedral _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'z, x, y' 'y, z, x' '-x, -y, -z' '-z, -x, -y' '-y, -z, -x' _cell_length_a 8.8920(10) _cell_length_b 8.8920(10) _cell_length_c 8.8920(10) _cell_angle_alpha 65.630(17) _cell_angle_beta 65.630(17) _cell_angle_gamma 65.630(17) _cell_volume 557.92(26) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 6.3 _cell_measurement_theta_max 12.4 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 5.673 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 812 _exptl_absorpt_coefficient_mu 41.828 _exptl_absorpt_correction_type 'psi-scan' _exptl_absorpt_correction_T_min 0.0479 _exptl_absorpt_correction_T_max 0.9399 _exptl_absorpt_process_details 'SHELXTL, V5.04' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf-Nonius CAD4' _diffrn_measurement_method \w--2\q _diffrn_refln_scan_width 1.00 _diffrn_standards_number 3 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% ? _diffrn_reflns_number 2791 _diffrn_reflns_av_R_equivalents 0.0268 _diffrn_reflns_av_sigmaI/netI 0.0663 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.63 _diffrn_reflns_theta_max 27.95 _reflns_number_total 904 _reflns_number_gt 684 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 EXPRESS' _computing_cell_refinement 'CAD4 EXPRESS' _computing_data_reduction 'XCAD4 (Harms, 1993)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00090(10) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 904 _refine_ls_number_parameters 41 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0577 _refine_ls_R_factor_gt 0.0401 _refine_ls_wR_factor_ref 0.0558 _refine_ls_wR_factor_gt 0.0489 _refine_ls_goodness_of_fit_ref 0.872 _refine_ls_restrained_S_all 0.871 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re -0.05720(4) 0.10752(4) 0.79599(4) 0.01135(15) Uani 1 1 d . . . Se1 Se 0.03719(15) 0.35384(14) 0.75677(15) 0.0174(4) Uani 0.629(11) 1 d P A 1 Se2 Se 0.14703(7) 0.14703(7) 0.14703(7) 0.0153(6) Uani 0.652(13) 3 d SP . 1 Cl1 Cl 0.03719(15) 0.35384(14) 0.75677(15) 0.0174(4) Uani 0.370(19) 1 d P A 2 Cl2 Cl 0.14703(7) 0.14703(7) 0.14703(7) 0.0153(6) Uani 0.34(2) 3 d SP . 2 Cl3 Cl 0.8739(3) 0.2485(3) 0.5321(3) 0.0268(5) Uani 1 1 d . . . K1 K 0.5000 0.5000 0.5000 0.125(5) Uani 1 6 d S . . O1 O 0.3446(13) 0.3446(13) 0.3446(13) 0.145(9) Uani 1 3 d S . . 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 0.0133(2) 0.01196(19) 0.0103(2) -0.00261(13) -0.00495(12) -0.00425(13) Se1 0.0223(7) 0.0133(6) 0.0179(6) -0.0001(4) -0.0083(5) -0.0083(5) Se2 0.0174(6) 0.0174(6) 0.0174(6) -0.0070(3) -0.0070(3) -0.0070(3) Cl1 0.0223(7) 0.0133(6) 0.0179(6) -0.0001(4) -0.0083(5) -0.0083(5) Cl2 0.0174(6) 0.0174(6) 0.0174(6) -0.0070(3) -0.0070(3) -0.0070(3) Cl3 0.0329(13) 0.0292(12) 0.0170(11) 0.0009(10) -0.0149(9) -0.0081(10) K1 0.070(2) 0.070(2) 0.070(2) 0.030(2) 0.030(2) 0.030(2) O1 0.108(10) 0.108(10) 0.108(10) 0.002(7) 0.002(7) 0.002(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 Re1 Cl3 2.362(2) 1_455 ? Re1 Cl1 2.4916(14) 5_656 ? Re1 Se1 2.4916(14) 5_656 ? Re1 Cl2 2.4960(12) 4_556 ? Re1 Se2 2.4960(12) 4_556 ? Re1 Cl1 2.4971(13) 6_566 ? Re1 Se1 2.4971(13) 6_566 ? Re1 Se1 2.5037(10) . ? Re1 Re1 2.6015(9) 2_456 ? Re1 Re1 2.6015(9) 3_546 ? Re1 Re1 2.6078(5) 5_656 ? Se1 Re1 2.4916(14) 6_566 ? Se1 Re1 2.4971(13) 5_656 ? Se2 Re1 2.4960(12) 6_565 ? Se2 Re1 2.4960(12) 4_556 ? Se2 Re1 2.4960(12) 5_655 ? Cl3 Re1 2.362(2) 1_655 ? Cl3 K1 3.203(3) . ? K1 Cl3 3.203(3) 3 ? K1 Cl3 3.203(3) 2 ? K1 Cl3 3.203(3) 6_666 ? K1 Cl3 3.203(3) 4_666 ? K1 Cl3 3.203(3) 5_666 ? K1 O1 3.23(3) 4_666 ? K1 O1 3.23(3) . ? 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 Cl3 Re1 Cl1 91.06(7) 1_455 5_656 ? Cl3 Re1 Se1 91.06(7) 1_455 5_656 ? Cl1 Re1 Se1 0.00(6) 5_656 5_656 ? Cl3 Re1 Cl2 92.71(6) 1_455 4_556 ? Cl1 Re1 Cl2 89.95(2) 5_656 4_556 ? Se1 Re1 Cl2 89.95(2) 5_656 4_556 ? Cl3 Re1 Se2 92.71(6) 1_455 4_556 ? Cl1 Re1 Se2 89.95(2) 5_656 4_556 ? Se1 Re1 Se2 89.95(2) 5_656 4_556 ? Cl2 Re1 Se2 0.00(2) 4_556 4_556 ? Cl3 Re1 Cl1 92.37(7) 1_455 6_566 ? Cl1 Re1 Cl1 176.57(3) 5_656 6_566 ? Se1 Re1 Cl1 176.57(3) 5_656 6_566 ? Cl2 Re1 Cl1 89.82(3) 4_556 6_566 ? Se2 Re1 Cl1 89.82(3) 4_556 6_566 ? Cl3 Re1 Se1 92.37(7) 1_455 6_566 ? Cl1 Re1 Se1 176.57(3) 5_656 6_566 ? Se1 Re1 Se1 176.57(3) 5_656 6_566 ? Cl2 Re1 Se1 89.82(3) 4_556 6_566 ? Se2 Re1 Se1 89.82(3) 4_556 6_566 ? Cl1 Re1 Se1 0.00(5) 6_566 6_566 ? Cl3 Re1 Se1 90.93(6) 1_455 . ? Cl1 Re1 Se1 90.07(3) 5_656 . ? Se1 Re1 Se1 90.07(3) 5_656 . ? Cl2 Re1 Se1 176.37(3) 4_556 . ? Se2 Re1 Se1 176.37(3) 4_556 . ? Cl1 Re1 Se1 89.94(2) 6_566 . ? Se1 Re1 Se1 89.94(2) 6_566 . ? Cl3 Re1 Re1 136.09(6) 1_455 2_456 ? Cl1 Re1 Re1 118.66(3) 5_656 2_456 ? Se1 Re1 Re1 118.66(3) 5_656 2_456 ? Cl2 Re1 Re1 58.591(19) 4_556 2_456 ? Se2 Re1 Re1 58.591(19) 4_556 2_456 ? Cl1 Re1 Re1 58.46(3) 6_566 2_456 ? Se1 Re1 Re1 58.46(3) 6_566 2_456 ? Se1 Re1 Re1 118.37(3) . 2_456 ? Cl3 Re1 Re1 135.28(7) 1_455 3_546 ? Cl1 Re1 Re1 58.67(3) 5_656 3_546 ? Se1 Re1 Re1 58.67(3) 5_656 3_546 ? Cl2 Re1 Re1 58.591(19) 4_556 3_546 ? Se2 Re1 Re1 58.591(19) 4_556 3_546 ? Cl1 Re1 Re1 118.45(3) 6_566 3_546 ? Se1 Re1 Re1 118.45(3) 6_566 3_546 ? Se1 Re1 Re1 118.51(3) . 3_546 ? Re1 Re1 Re1 60.0 2_456 3_546 ? Cl3 Re1 Re1 133.91(6) 1_455 5_656 ? Cl1 Re1 Re1 58.76(2) 5_656 5_656 ? Se1 Re1 Re1 58.76(2) 5_656 5_656 ? Cl2 Re1 Re1 118.66(3) 4_556 5_656 ? Se2 Re1 Re1 118.66(3) 4_556 5_656 ? Cl1 Re1 Re1 118.52(3) 6_566 5_656 ? Se1 Re1 Re1 118.52(3) 6_566 5_656 ? Se1 Re1 Re1 58.45(3) . 5_656 ? Re1 Re1 Re1 90.0 2_456 5_656 ? Re1 Re1 Re1 60.080(11) 3_546 5_656 ? Re1 Se1 Re1 62.86(3) 6_566 5_656 ? Re1 Se1 Re1 62.94(3) 6_566 . ? Re1 Se1 Re1 62.86(3) 5_656 . ? Re1 Se2 Re1 62.82(4) 6_565 4_556 ? Re1 Se2 Re1 62.82(4) 6_565 5_655 ? Re1 Se2 Re1 62.82(4) 4_556 5_655 ? Re1 Cl3 K1 123.76(10) 1_655 . ? Cl3 K1 Cl3 109.40(4) 3 2 ? Cl3 K1 Cl3 109.40(4) 3 . ? Cl3 K1 Cl3 109.40(4) 2 . ? Cl3 K1 Cl3 180.0 3 6_666 ? Cl3 K1 Cl3 70.60(4) 2 6_666 ? Cl3 K1 Cl3 70.60(4) . 6_666 ? Cl3 K1 Cl3 70.60(4) 3 4_666 ? Cl3 K1 Cl3 70.60(4) 2 4_666 ? Cl3 K1 Cl3 180.0 . 4_666 ? Cl3 K1 Cl3 109.40(4) 6_666 4_666 ? Cl3 K1 Cl3 70.60(4) 3 5_666 ? Cl3 K1 Cl3 180.0 2 5_666 ? Cl3 K1 Cl3 70.60(4) . 5_666 ? Cl3 K1 Cl3 109.40(4) 6_666 5_666 ? Cl3 K1 Cl3 109.40(4) 4_666 5_666 ? Cl3 K1 O1 70.45(4) 3 4_666 ? Cl3 K1 O1 70.45(4) 2 4_666 ? Cl3 K1 O1 70.45(4) . 4_666 ? Cl3 K1 O1 109.55(4) 6_666 4_666 ? Cl3 K1 O1 109.55(4) 4_666 4_666 ? Cl3 K1 O1 109.55(4) 5_666 4_666 ? Cl3 K1 O1 109.55(4) 3 . ? Cl3 K1 O1 109.55(4) 2 . ? Cl3 K1 O1 109.55(4) . . ? Cl3 K1 O1 70.45(4) 6_666 . ? Cl3 K1 O1 70.45(4) 4_666 . ? Cl3 K1 O1 70.45(4) 5_666 . ? O1 K1 O1 180.0 4_666 . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.95 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 4.522 _refine_diff_density_min -2.852 _refine_diff_density_rms 0.506 #################### Material relevant to compound 2 #################### data_tbarese _database_code_CSD 146273 _audit_creation_method SHELXL _chemical_name_systematic ; tetra-n-butylammonium penta-\m~eq~3-seleno-tri-\m~eq~3-chloro- hexachloro-octahedro-hexarhenate(III) ; _chemical_name_common '(nBu4N)[Re6Se5Cl9]' _chemical_formula_moiety '(C16 H36 N 1+, Re6 Se5 Cl9 1-' _chemical_formula_structural '((C4H9)4N) (Re6Se5Cl9)' _chemical_formula_sum 'C16 H36 Cl9 N Re6 Se5' _chemical_formula_weight 2073.51 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' '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' 'Se' 'Se' -0.0929 2.2259 '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 10.775(2) _cell_length_b 17.101(3) _cell_length_c 10.602(2) _cell_angle_alpha 100.83(3) _cell_angle_beta 99.62(3) _cell_angle_gamma 87.51(3) _cell_volume 1891.6(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10.1 _cell_measurement_theta_max 15.4 _exptl_crystal_description paralelepipedic _exptl_crystal_colour 'intense red' _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 3.640 _exptl_crystal_density_method 'none' _exptl_crystal_F_000 1824 _exptl_absorpt_coefficient_mu 24.580 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details 'SHELXTL (Sheldrick, 1995)' _exptl_absorpt_correction_T_min 0.3135 _exptl_absorpt_correction_T_max 0.6319 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf Nonius CAD4' _diffrn_measurement_method \w--2\q _diffrn_refln_scan_width 1.00 _diffrn_standards_number 3 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0 _diffrn_reflns_number 6715 _diffrn_reflns_av_R_equivalents 0.0170 _diffrn_reflns_av_sigmaI/netI 0.0755 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.21 _diffrn_reflns_theta_max 24.97 _reflns_number_total 6334 _reflns_number_gt 3946 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'CAD4 EXPRESS' _computing_cell_refinement 'CAD4 EXPRESS' _computing_data_reduction 'XCAD4 (Harms, 1993)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'ORTEP (Johnson, 1976)' _computing_publication_material 'SHELXL-93 (Sheldrick, 1993)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1 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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0807P)^2^+5.6379P] 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 6333 _refine_ls_number_parameters 350 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.1000 _refine_ls_R_factor_gt 0.0345 _refine_ls_wR_factor_all 0.1545 _refine_ls_wR_factor_ref 0.1295 _refine_ls_goodness_of_fit_all 1.188 _refine_ls_goodness_of_fit_ref 1.311 _refine_ls_restrained_S_all 1.215 _refine_ls_restrained_S_obs 1.309 _refine_ls_shift/su_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 -0.07095(7) 0.08809(4) 0.59226(8) 0.0277(2) Uani 1 d . . Re2 Re -0.10200(7) 0.01684(5) 0.34947(8) 0.0287(2) Uani 1 d . . Re3 Re 0.12110(7) 0.06371(4) 0.46911(8) 0.0275(2) Uani 1 d . . Re4 Re 0.14001(8) 0.48479(5) 0.41875(9) 0.0320(2) Uani 1 d . . Re5 Re 0.06915(8) 0.43244(5) 0.61049(9) 0.0323(2) Uani 1 d . . Re6 Re -0.07620(8) 0.41496(5) 0.38497(9) 0.0309(2) Uani 1 d . . Se1 Se 0.1467(3) 0.1291(2) 0.7010(3) 0.0381(11) Uani 0.64(2) d P 1 Se2 Se -0.0502(2) 0.16146(14) 0.4152(3) 0.0378(10) Uani 0.74(2) d P 1 Se3 Se 0.2817(2) -0.0393(2) 0.5277(3) 0.0400(11) Uani 0.66(2) d P 1 Se4 Se 0.0864(3) -0.0063(2) 0.2375(3) 0.0382(12) Uani 0.51(2) d P 1 Se5 Se -0.0051(3) 0.4687(2) 0.2054(3) 0.0425(12) Uani 0.65(2) d P 1 Se6 Se 0.1279(3) 0.3392(2) 0.4181(3) 0.0400(11) Uani 0.67(2) d P 1 Se7 Se 0.2738(3) 0.5017(2) 0.6386(3) 0.0410(12) Uani 0.63(2) d P 1 Se8 Se 0.1397(3) 0.6322(2) 0.4261(3) 0.0364(13) Uani 0.45(2) d P 1 Cl1 Cl 0.1467(3) 0.1291(2) 0.7010(3) 0.0381(11) Uani 0.36(2) d P 2 Cl2 Cl -0.0502(2) 0.16146(14) 0.4152(3) 0.0378(10) Uani 0.26(2) d P 2 Cl3 Cl 0.2817(2) -0.0393(2) 0.5277(3) 0.0400(11) Uani 0.34(2) d P 2 Cl4 Cl 0.0864(3) -0.0063(2) 0.2375(3) 0.0382(12) Uani 0.49(2) d P 2 Cl5 Cl -0.0051(3) 0.4687(2) 0.2054(3) 0.0425(12) Uani 0.35(2) d P 2 Cl6 Cl 0.1279(3) 0.3392(2) 0.4181(3) 0.0400(11) Uani 0.33(2) d P 2 Cl7 Cl 0.2738(3) 0.5017(2) 0.6386(3) 0.0410(12) Uani 0.37(2) d P 2 Cl8 Cl 0.1397(3) 0.6322(2) 0.4261(3) 0.0364(13) Uani 0.55(2) d P 2 Cl10 Cl -0.1601(6) 0.1993(3) 0.7123(6) 0.0472(15) Uani 1 d . . Cl20 Cl -0.2294(7) 0.0360(4) 0.1541(7) 0.067(2) Uani 1 d . . Cl30 Cl 0.2757(6) 0.1442(4) 0.4273(7) 0.059(2) Uani 1 d . . Cl40 Cl 0.3206(6) 0.4671(4) 0.3168(7) 0.058(2) Uani 1 d . . Cl50 Cl 0.1536(7) 0.3452(4) 0.7502(7) 0.064(2) Uani 1 d . . Cl60 Cl -0.1749(5) 0.3055(3) 0.2407(6) 0.048(2) Uani 1 d . . N1 N 0.4514(16) 0.2472(10) 0.0545(16) 0.033(4) Uani 1 d . . C1 C 0.5264(21) 0.3185(14) 0.0443(20) 0.041(6) Uani 1 d . . H1A H 0.5145(21) 0.3611(14) 0.1159(20) 0.049 Uiso 1 calc R . H1B H 0.6149(21) 0.3037(14) 0.0560(20) 0.049 Uiso 1 calc R . C2 C 0.4956(23) 0.3506(17) -0.0795(30) 0.064(8) Uani 1 d . . H2A H 0.4108(23) 0.3728(17) -0.0881(30) 0.077 Uiso 1 calc R . H2B H 0.5007(23) 0.3084(17) -0.1537(30) 0.077 Uiso 1 calc R . C3 C 0.5920(27) 0.4161(17) -0.0738(29) 0.064(8) Uani 1 d . . H3A H 0.5617(27) 0.4455(17) -0.1429(29) 0.077 Uiso 1 calc R . H3B H 0.5939(27) 0.4529(17) 0.0081(29) 0.077 Uiso 1 calc R . C4 C 0.7241(26) 0.3887(18) -0.0860(30) 0.073(9) Uani 1 d . . H4A H 0.7755(26) 0.4340(18) -0.0812(30) 0.109 Uiso 1 calc R . H4B H 0.7246(26) 0.3536(18) -0.1680(30) 0.109 Uiso 1 calc R . H4C H 0.7569(26) 0.3610(18) -0.0165(30) 0.109 Uiso 1 calc R . C5 C 0.5046(19) 0.2191(13) 0.1825(19) 0.035(5) Uani 1 d . . H5A H 0.4632(19) 0.1699(13) 0.1831(19) 0.042 Uiso 1 calc R . H5B H 0.5933(19) 0.2067(13) 0.1827(19) 0.042 Uiso 1 calc R . C6 C 0.4915(22) 0.2756(14) 0.3059(22) 0.044(6) Uani 1 d . . H6A H 0.4032(22) 0.2838(14) 0.3133(22) 0.053 Uiso 1 calc R . H6B H 0.5270(22) 0.3266(14) 0.3050(22) 0.053 Uiso 1 calc R . C7 C 0.5593(21) 0.2417(14) 0.4196(19) 0.043(6) Uani 1 d . . H7A H 0.6491(21) 0.2393(14) 0.4178(19) 0.052 Uiso 1 calc R . H7B H 0.5307(21) 0.1880(14) 0.4149(19) 0.052 Uiso 1 calc R . C8 C 0.5331(24) 0.2939(18) 0.5443(23) 0.062(8) Uani 1 d . . H8A H 0.5762(24) 0.2725(18) 0.6174(23) 0.093 Uiso 1 calc R . H8B H 0.4442(24) 0.2957(18) 0.5459(23) 0.093 Uiso 1 calc R . H8C H 0.5623(24) 0.3468(18) 0.5488(23) 0.093 Uiso 1 calc R . C9 C 0.4641(23) 0.1808(14) -0.0619(27) 0.053(7) Uani 1 d . . H9A H 0.4213(23) 0.1342(14) -0.0515(27) 0.063 Uiso 1 calc R . H9B H 0.4206(23) 0.1978(14) -0.1401(27) 0.063 Uiso 1 calc R . C10 C 0.5932(22) 0.1572(14) -0.0812(28) 0.057(8) Uani 1 d . . H10A H 0.6386(22) 0.1377(14) -0.0061(28) 0.068 Uiso 1 calc R . H10B H 0.6381(22) 0.2020(14) -0.0950(28) 0.068 Uiso 1 calc R . C11 C 0.5797(30) 0.0897(18) -0.2046(34) 0.080(10) Uani 1 d . . H11A H 0.5078(30) 0.1024(18) -0.2659(34) 0.096 Uiso 1 calc R . H11B H 0.6539(30) 0.0898(18) -0.2453(34) 0.096 Uiso 1 calc R . C12 C 0.5652(39) 0.0152(26) -0.1830(47) 0.135(17) Uani 1 d . . H12A H 0.5579(39) -0.0218(26) -0.2640(47) 0.202 Uiso 1 calc R . H12B H 0.4904(39) 0.0137(26) -0.1454(47) 0.202 Uiso 1 calc R . H12C H 0.6369(39) 0.0011(26) -0.1244(47) 0.202 Uiso 1 calc R . C13 C 0.3163(20) 0.2705(14) 0.0453(23) 0.043(6) Uani 1 d . . H13A H 0.2873(20) 0.2839(14) -0.0398(23) 0.051 Uiso 1 calc R . H13B H 0.3082(20) 0.3180(14) 0.1098(23) 0.051 Uiso 1 calc R . C14 C 0.2298(18) 0.2057(14) 0.0659(23) 0.040(6) Uani 1 d . . H14A H 0.2413(18) 0.1567(14) 0.0060(23) 0.048 Uiso 1 calc R . H14B H 0.2525(18) 0.1955(14) 0.1539(23) 0.048 Uiso 1 calc R . C15 C 0.0937(21) 0.2321(13) 0.0438(21) 0.042(6) Uani 1 d . . H15A H 0.0741(21) 0.2475(13) -0.0410(21) 0.051 Uiso 1 calc R . H15B H 0.0813(21) 0.2785(13) 0.1089(21) 0.051 Uiso 1 calc R . C16 C 0.0024(22) 0.1663(15) 0.0504(22) 0.049(6) Uani 1 d . . H16A H -0.0827(22) 0.1858(15) 0.0356(22) 0.073 Uiso 1 calc R . H16B H 0.0202(22) 0.1517(15) 0.1348(22) 0.073 Uiso 1 calc R . H16C H 0.0131(22) 0.1206(15) -0.0151(22) 0.073 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 0.0294(4) 0.0199(4) 0.0353(5) 0.0069(3) 0.0085(4) 0.0041(3) Re2 0.0283(4) 0.0257(4) 0.0328(5) 0.0097(4) 0.0026(3) 0.0036(3) Re3 0.0266(4) 0.0209(4) 0.0370(5) 0.0080(4) 0.0083(3) 0.0010(3) Re4 0.0301(4) 0.0261(4) 0.0425(5) 0.0138(4) 0.0054(4) 0.0005(3) Re5 0.0327(5) 0.0260(4) 0.0398(5) 0.0178(4) -0.0026(4) -0.0003(3) Re6 0.0302(4) 0.0243(4) 0.0387(5) 0.0123(4) -0.0010(4) -0.0013(3) Se1 0.037(2) 0.030(2) 0.043(2) -0.0020(13) 0.0014(13) -0.0063(12) Se2 0.045(2) 0.0237(15) 0.049(2) 0.0133(12) 0.0127(13) 0.0086(11) Se3 0.0255(15) 0.039(2) 0.057(2) 0.0125(14) 0.0074(13) 0.0081(11) Se4 0.044(2) 0.035(2) 0.040(2) 0.0118(14) 0.0149(14) 0.0039(14) Se5 0.053(2) 0.039(2) 0.036(2) 0.0101(13) 0.0043(14) -0.0050(14) Se6 0.036(2) 0.026(2) 0.059(2) 0.0144(13) 0.0027(13) 0.0031(11) Se7 0.030(2) 0.036(2) 0.056(2) 0.0165(14) -0.0066(13) 0.0002(12) Se8 0.036(2) 0.026(2) 0.052(2) 0.018(2) 0.0055(15) -0.0049(13) Cl1 0.037(2) 0.030(2) 0.043(2) -0.0020(13) 0.0014(13) -0.0063(12) Cl2 0.045(2) 0.0237(15) 0.049(2) 0.0133(12) 0.0127(13) 0.0086(11) Cl3 0.0255(15) 0.039(2) 0.057(2) 0.0125(14) 0.0074(13) 0.0081(11) Cl4 0.044(2) 0.035(2) 0.040(2) 0.0118(14) 0.0149(14) 0.0039(14) Cl5 0.053(2) 0.039(2) 0.036(2) 0.0101(13) 0.0043(14) -0.0050(14) Cl6 0.036(2) 0.026(2) 0.059(2) 0.0144(13) 0.0027(13) 0.0031(11) Cl7 0.030(2) 0.036(2) 0.056(2) 0.0165(14) -0.0066(13) 0.0002(12) Cl8 0.036(2) 0.026(2) 0.052(2) 0.018(2) 0.0055(15) -0.0049(13) Cl10 0.058(4) 0.025(3) 0.062(4) 0.002(3) 0.028(3) 0.014(3) Cl20 0.062(4) 0.073(5) 0.064(5) 0.031(4) -0.020(4) 0.001(4) Cl30 0.047(4) 0.048(4) 0.092(5) 0.023(4) 0.022(3) -0.014(3) Cl40 0.051(4) 0.050(4) 0.080(5) 0.011(3) 0.034(3) 0.004(3) Cl50 0.068(4) 0.052(4) 0.077(5) 0.044(4) -0.012(4) 0.003(3) Cl60 0.044(3) 0.039(3) 0.055(4) 0.009(3) -0.012(3) -0.011(3) N1 0.036(10) 0.036(10) 0.024(9) 0.000(8) 0.003(7) -0.008(8) C1 0.049(14) 0.046(14) 0.025(12) 0.000(10) 0.007(10) 0.000(11) C2 0.040(14) 0.066(19) 0.095(23) 0.055(17) -0.013(14) -0.002(13) C3 0.076(19) 0.064(18) 0.063(19) 0.042(15) 0.013(15) 0.011(15) C4 0.072(20) 0.082(22) 0.085(23) 0.045(18) 0.045(18) 0.024(17) C5 0.027(11) 0.050(14) 0.022(11) 0.000(10) 0.001(8) 0.010(10) C6 0.046(13) 0.046(14) 0.048(15) 0.027(12) 0.011(11) 0.009(11) C7 0.043(13) 0.055(15) 0.021(12) -0.015(11) -0.002(10) 0.007(11) C8 0.057(17) 0.093(22) 0.033(15) 0.003(14) 0.011(12) 0.002(15) C9 0.053(15) 0.041(14) 0.068(18) 0.012(13) 0.021(13) 0.000(12) C10 0.037(13) 0.042(15) 0.087(21) -0.016(14) 0.024(13) -0.011(11) C11 0.071(21) 0.063(20) 0.115(29) 0.012(20) 0.054(20) 0.026(17) C12 0.107(34) 0.116(38) 0.189(53) 0.024(35) 0.052(34) 0.015(28) C13 0.036(12) 0.049(14) 0.043(14) 0.023(11) -0.007(10) 0.003(10) C14 0.025(11) 0.052(14) 0.042(14) 0.012(11) -0.001(9) -0.015(10) C15 0.057(15) 0.042(13) 0.030(13) -0.011(10) 0.035(11) -0.001(11) C16 0.045(14) 0.069(17) 0.035(14) 0.001(12) 0.020(11) -0.008(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re1 Cl10 2.345(5) . ? Re1 Cl2 2.490(3) . ? Re1 Se2 2.490(3) . ? Re1 Cl1 2.501(3) . ? Re1 Se1 2.501(3) . ? Re1 Cl3 2.504(3) 2_556 ? Re1 Se3 2.504(3) 2_556 ? Re1 Cl4 2.513(3) 2_556 ? Re1 Se4 2.513(3) 2_556 ? Re1 Re3 2.6046(13) . ? Re1 Re2 2.6060(14) . ? Re1 Re2 2.6106(14) 2_556 ? Re2 Cl20 2.355(6) . ? Re2 Cl3 2.486(3) 2_556 ? Re2 Se3 2.486(3) 2_556 ? Re2 Cl4 2.500(3) . ? Re2 Se4 2.500(3) . ? Re2 Se2 2.501(3) . ? Re2 Cl2 2.501(3) . ? Re2 Cl1 2.502(3) 2_556 ? Re2 Se1 2.502(3) 2_556 ? Re2 Re3 2.6061(13) 2_556 ? Re2 Re3 2.6070(14) . ? Re3 Cl30 2.354(6) . ? Re3 Cl1 2.477(3) . ? Re3 Se1 2.477(3) . ? Re3 Cl4 2.496(3) . ? Re3 Se4 2.496(3) . ? Re3 Se2 2.504(3) . ? Re3 Cl2 2.504(3) . ? Re3 Se3 2.505(3) . ? Re3 Cl3 2.505(3) . ? Re3 Re2 2.6060(13) 2_556 ? Re4 Cl40 2.362(6) . ? Re4 Cl6 2.498(3) . ? Re4 Se6 2.498(3) . ? Re4 Cl7 2.501(3) . ? Re4 Se7 2.501(3) . ? Re4 Se5 2.501(3) . ? Re4 Cl5 2.501(3) . ? Re4 Cl8 2.507(3) . ? Re4 Se8 2.507(3) . ? Re4 Re6 2.603(2) 2_566 ? Re4 Re5 2.6035(14) . ? Re4 Re6 2.6045(13) . ? Re5 Cl50 2.347(6) . ? Re5 Cl8 2.490(3) 2_566 ? Re5 Se8 2.490(3) 2_566 ? Re5 Se6 2.495(3) . ? Re5 Cl6 2.495(3) . ? Re5 Se7 2.496(3) . ? Re5 Cl7 2.496(3) . ? Re5 Cl5 2.501(3) 2_566 ? Re5 Se5 2.501(3) 2_566 ? Re5 Re6 2.6038(15) . ? Re5 Re6 2.6051(12) 2_566 ? Re6 Cl60 2.351(5) . ? Re6 Cl8 2.499(3) 2_566 ? Re6 Se8 2.499(3) 2_566 ? Re6 Se5 2.502(3) . ? Re6 Cl5 2.502(3) . ? Re6 Se6 2.511(3) . ? Re6 Cl6 2.511(3) . ? Re6 Cl7 2.514(3) 2_566 ? Re6 Se7 2.514(3) 2_566 ? Re6 Re4 2.603(2) 2_566 ? Se1 Re2 2.502(3) 2_556 ? Se3 Re2 2.486(3) 2_556 ? Se3 Re1 2.504(3) 2_556 ? Se4 Re1 2.513(3) 2_556 ? Se5 Re5 2.501(3) 2_566 ? Se7 Re6 2.514(3) 2_566 ? Se8 Re5 2.490(3) 2_566 ? Se8 Re6 2.499(3) 2_566 ? Cl1 Re2 2.502(3) 2_556 ? Cl3 Re2 2.486(3) 2_556 ? Cl3 Re1 2.504(3) 2_556 ? Cl4 Re1 2.513(3) 2_556 ? Cl5 Re5 2.501(3) 2_566 ? Cl7 Re6 2.514(3) 2_566 ? Cl8 Re5 2.490(3) 2_566 ? Cl8 Re6 2.499(3) 2_566 ? N1 C13 1.48(3) . ? N1 C1 1.52(3) . ? N1 C9 1.53(3) . ? N1 C5 1.54(3) . ? C1 C2 1.50(3) . ? C2 C3 1.55(3) . ? C3 C4 1.50(4) . ? C5 C6 1.50(3) . ? C6 C7 1.50(3) . ? C7 C8 1.51(3) . ? C9 C10 1.47(3) . ? C10 C11 1.56(4) . ? C11 C12 1.36(5) . ? C13 C14 1.55(3) . ? C14 C15 1.51(3) . ? C15 C16 1.55(3) . ? 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 Cl10 Re1 Cl2 92.2(2) . . ? Cl10 Re1 Se2 92.2(2) . . ? Cl10 Re1 Cl1 91.8(2) . . ? Cl2 Re1 Cl1 89.63(10) . . ? Cl10 Re1 Se1 91.8(2) . . ? Se2 Re1 Se1 89.63(10) . . ? Cl10 Re1 Cl3 92.4(2) . 2_556 ? Cl2 Re1 Cl3 89.59(10) . 2_556 ? Cl1 Re1 Cl3 175.80(10) . 2_556 ? Cl10 Re1 Se3 92.4(2) . 2_556 ? Se2 Re1 Se3 89.59(10) . 2_556 ? Se1 Re1 Se3 175.80(10) . 2_556 ? Cl10 Re1 Cl4 91.4(2) . 2_556 ? Cl2 Re1 Cl4 176.35(10) . 2_556 ? Cl1 Re1 Cl4 90.43(11) . 2_556 ? Cl3 Re1 Cl4 90.09(11) 2_556 2_556 ? Cl10 Re1 Se4 91.4(2) . 2_556 ? Se2 Re1 Se4 176.35(10) . 2_556 ? Se1 Re1 Se4 90.43(11) . 2_556 ? Se3 Re1 Se4 90.09(11) 2_556 2_556 ? Cl10 Re1 Re3 135.2(2) . . ? Cl2 Re1 Re3 58.82(7) . . ? Se2 Re1 Re3 58.82(7) . . ? Cl1 Re1 Re3 58.01(8) . . ? Se1 Re1 Re3 58.01(8) . . ? Cl3 Re1 Re3 118.22(8) 2_556 . ? Se3 Re1 Re3 118.22(8) 2_556 . ? Cl4 Re1 Re3 118.31(8) 2_556 . ? Se4 Re1 Re3 118.31(8) 2_556 . ? Cl10 Re1 Re2 135.8(2) . . ? Cl2 Re1 Re2 58.74(7) . . ? Se2 Re1 Re2 58.74(7) . . ? Cl1 Re1 Re2 118.04(8) . . ? Se1 Re1 Re2 118.04(8) . . ? Cl3 Re1 Re2 58.19(8) 2_556 . ? Se3 Re1 Re2 58.19(8) 2_556 . ? Cl4 Re1 Re2 118.18(8) 2_556 . ? Se4 Re1 Re2 118.18(8) 2_556 . ? Re3 Re1 Re2 60.04(4) . . ? Cl10 Re1 Re2 134.3(2) . 2_556 ? Cl2 Re1 Re2 118.77(7) . 2_556 ? Se2 Re1 Re2 118.77(7) . 2_556 ? Cl1 Re1 Re2 58.56(7) . 2_556 ? Se1 Re1 Re2 58.56(7) . 2_556 ? Cl3 Re1 Re2 118.44(8) 2_556 2_556 ? Se3 Re1 Re2 118.44(8) 2_556 2_556 ? Cl4 Re1 Re2 58.37(8) 2_556 2_556 ? Se4 Re1 Re2 58.37(8) 2_556 2_556 ? Re3 Re1 Re2 59.96(4) . 2_556 ? Re2 Re1 Re2 89.92(5) . 2_556 ? Cl20 Re2 Cl3 92.6(2) . 2_556 ? Cl20 Re2 Se3 92.6(2) . 2_556 ? Cl20 Re2 Cl4 90.5(2) . . ? Cl3 Re2 Cl4 176.86(11) 2_556 . ? Cl20 Re2 Se4 90.5(2) . . ? Se3 Re2 Se4 176.86(11) 2_556 . ? Cl20 Re2 Se2 92.6(2) . . ? Se3 Re2 Se2 89.74(10) 2_556 . ? Se4 Re2 Se2 89.88(10) . . ? Cl20 Re2 Cl2 92.6(2) . . ? Cl3 Re2 Cl2 89.74(10) 2_556 . ? Cl4 Re2 Cl2 89.88(10) . . ? Cl20 Re2 Cl1 91.3(2) . 2_556 ? Cl3 Re2 Cl1 89.46(10) 2_556 2_556 ? Cl4 Re2 Cl1 90.71(11) . 2_556 ? Cl2 Re2 Cl1 176.07(10) . 2_556 ? Cl20 Re2 Se1 91.3(2) . 2_556 ? Se3 Re2 Se1 89.46(10) 2_556 2_556 ? Se4 Re2 Se1 90.71(11) . 2_556 ? Se2 Re2 Se1 176.07(10) . 2_556 ? Cl20 Re2 Re1 136.3(2) . . ? Cl3 Re2 Re1 58.86(8) 2_556 . ? Se3 Re2 Re1 58.86(8) 2_556 . ? Cl4 Re2 Re1 118.43(9) . . ? Se4 Re2 Re1 118.43(9) . . ? Se2 Re2 Re1 58.31(7) . . ? Cl2 Re2 Re1 58.31(7) . . ? Cl1 Re2 Re1 118.13(8) 2_556 . ? Se1 Re2 Re1 118.13(8) 2_556 . ? Cl20 Re2 Re3 135.2(2) . 2_556 ? Cl3 Re2 Re3 58.87(7) 2_556 2_556 ? Se3 Re2 Re3 58.87(7) 2_556 2_556 ? Cl4 Re2 Re3 118.74(8) . 2_556 ? Se4 Re2 Re3 118.74(8) . 2_556 ? Se2 Re2 Re3 118.45(8) . 2_556 ? Cl2 Re2 Re3 118.45(8) . 2_556 ? Cl1 Re2 Re3 57.98(8) 2_556 2_556 ? Se1 Re2 Re3 57.98(8) 2_556 2_556 ? Re1 Re2 Re3 60.15(3) . 2_556 ? Cl20 Re2 Re3 134.7(2) . . ? Cl3 Re2 Re3 118.80(8) 2_556 . ? Se3 Re2 Re3 118.80(8) 2_556 . ? Cl4 Re2 Re3 58.48(8) . . ? Se4 Re2 Re3 58.48(8) . . ? Se2 Re2 Re3 58.65(7) . . ? Cl2 Re2 Re3 58.65(7) . . ? Cl1 Re2 Re3 118.59(8) 2_556 . ? Se1 Re2 Re3 118.59(8) 2_556 . ? Re1 Re2 Re3 59.95(4) . . ? Re3 Re2 Re3 90.00(4) 2_556 . ? Cl30 Re3 Cl1 92.0(2) . . ? Cl30 Re3 Se1 92.0(2) . . ? Cl30 Re3 Cl4 91.0(2) . . ? Cl1 Re3 Cl4 177.05(10) . . ? Cl30 Re3 Se4 91.0(2) . . ? Se1 Re3 Se4 177.05(10) . . ? Cl30 Re3 Se2 91.9(2) . . ? Se1 Re3 Se2 89.85(10) . . ? Se4 Re3 Se2 89.90(11) . . ? Cl30 Re3 Cl2 91.9(2) . . ? Cl1 Re3 Cl2 89.85(10) . . ? Cl4 Re3 Cl2 89.90(11) . . ? Cl30 Re3 Se3 91.9(2) . . ? Se1 Re3 Se3 89.60(11) . . ? Se4 Re3 Se3 90.46(11) . . ? Se2 Re3 Se3 176.14(9) . . ? Cl30 Re3 Cl3 91.9(2) . . ? Cl1 Re3 Cl3 89.60(11) . . ? Cl4 Re3 Cl3 90.46(11) . . ? Cl2 Re3 Cl3 176.14(9) . . ? Cl30 Re3 Re1 135.4(2) . . ? Cl1 Re3 Re1 58.90(7) . . ? Se1 Re3 Re1 58.90(7) . . ? Cl4 Re3 Re1 118.61(9) . . ? Se4 Re3 Re1 118.61(9) . . ? Se2 Re3 Re1 58.30(7) . . ? Cl2 Re3 Re1 58.30(7) . . ? Se3 Re3 Re1 118.31(8) . . ? Cl3 Re3 Re1 118.31(8) . . ? Cl30 Re3 Re2 135.4(2) . 2_556 ? Cl1 Re3 Re2 58.90(7) . 2_556 ? Se1 Re3 Re2 58.90(7) . 2_556 ? Cl4 Re3 Re2 118.79(8) . 2_556 ? Se4 Re3 Re2 118.79(8) . 2_556 ? Se2 Re3 Re2 118.42(8) . 2_556 ? Cl2 Re3 Re2 118.42(8) . 2_556 ? Se3 Re3 Re2 58.18(8) . 2_556 ? Cl3 Re3 Re2 58.18(8) . 2_556 ? Re1 Re3 Re2 60.14(4) . 2_556 ? Cl30 Re3 Re2 134.6(2) . . ? Cl1 Re3 Re2 118.89(8) . . ? Se1 Re3 Re2 118.89(8) . . ? Cl4 Re3 Re2 58.61(8) . . ? Se4 Re3 Re2 58.61(8) . . ? Se2 Re3 Re2 58.56(7) . . ? Cl2 Re3 Re2 58.56(7) . . ? Se3 Re3 Re2 118.57(8) . . ? Cl3 Re3 Re2 118.57(8) . . ? Re1 Re3 Re2 60.01(4) . . ? Re2 Re3 Re2 90.00(4) 2_556 . ? Cl40 Re4 Cl6 92.2(2) . . ? Cl40 Re4 Se6 92.2(2) . . ? Cl40 Re4 Cl7 91.0(2) . . ? Cl6 Re4 Cl7 89.43(10) . . ? Cl40 Re4 Se7 91.0(2) . . ? Se6 Re4 Se7 89.43(10) . . ? Cl40 Re4 Se5 92.4(2) . . ? Se6 Re4 Se5 90.30(10) . . ? Se7 Re4 Se5 176.59(11) . . ? Cl40 Re4 Cl5 92.4(2) . . ? Cl6 Re4 Cl5 90.30(10) . . ? Cl7 Re4 Cl5 176.59(11) . . ? Cl40 Re4 Cl8 91.4(2) . . ? Cl6 Re4 Cl8 176.33(11) . . ? Cl7 Re4 Cl8 90.56(11) . . ? Cl5 Re4 Cl8 89.49(11) . . ? Cl40 Re4 Se8 91.4(2) . . ? Se6 Re4 Se8 176.33(11) . . ? Se7 Re4 Se8 90.56(11) . . ? Se5 Re4 Se8 89.49(11) . . ? Cl40 Re4 Re6 134.2(2) . 2_566 ? Cl6 Re4 Re6 118.56(9) . 2_566 ? Se6 Re4 Re6 118.56(9) . 2_566 ? Cl7 Re4 Re6 58.96(8) . 2_566 ? Se7 Re4 Re6 58.96(8) . 2_566 ? Se5 Re4 Re6 118.35(8) . 2_566 ? Cl5 Re4 Re6 118.35(8) . 2_566 ? Cl8 Re4 Re6 58.50(9) . 2_566 ? Se8 Re4 Re6 58.50(9) . 2_566 ? Cl40 Re4 Re5 134.9(2) . . ? Cl6 Re4 Re5 58.52(8) . . ? Se6 Re4 Re5 58.52(8) . . ? Cl7 Re4 Re5 58.50(8) . . ? Se7 Re4 Re5 58.50(8) . . ? Se5 Re4 Re5 118.62(8) . . ? Cl5 Re4 Re5 118.62(8) . . ? Cl8 Re4 Re5 118.53(9) . . ? Se8 Re4 Re5 118.53(9) . . ? Re6 Re4 Re5 60.04(4) 2_566 . ? Cl40 Re4 Re6 136.0(2) . . ? Cl6 Re4 Re6 58.92(7) . . ? Se6 Re4 Re6 58.92(7) . . ? Cl7 Re4 Re6 118.49(8) . . ? Se7 Re4 Re6 118.49(8) . . ? Se5 Re4 Re6 58.63(8) . . ? Cl5 Re4 Re6 58.63(8) . . ? Cl8 Re4 Re6 118.03(8) . . ? Se8 Re4 Re6 118.03(8) . . ? Re6 Re4 Re6 89.81(5) 2_566 . ? Re5 Re4 Re6 59.99(4) . . ? Cl50 Re5 Cl8 90.6(2) . 2_566 ? Cl50 Re5 Se8 90.6(2) . 2_566 ? Cl50 Re5 Se6 91.4(2) . . ? Se8 Re5 Se6 90.10(11) 2_566 . ? Cl50 Re5 Cl6 91.4(2) . . ? Cl8 Re5 Cl6 90.10(11) 2_566 . ? Cl50 Re5 Se7 92.5(2) . . ? Se8 Re5 Se7 176.97(11) 2_566 . ? Se6 Re5 Se7 89.61(11) . . ? Cl50 Re5 Cl7 92.5(2) . . ? Cl8 Re5 Cl7 176.97(11) 2_566 . ? Cl6 Re5 Cl7 89.61(11) . . ? Cl50 Re5 Cl5 91.9(2) . 2_566 ? Cl8 Re5 Cl5 89.89(11) 2_566 2_566 ? Cl6 Re5 Cl5 176.66(10) . 2_566 ? Cl7 Re5 Cl5 90.22(11) . 2_566 ? Cl50 Re5 Se5 91.9(2) . 2_566 ? Se8 Re5 Se5 89.89(11) 2_566 2_566 ? Se6 Re5 Se5 176.66(10) . 2_566 ? Se7 Re5 Se5 90.22(11) . 2_566 ? Cl50 Re5 Re4 135.6(2) . . ? Cl8 Re5 Re4 118.72(9) 2_566 . ? Se8 Re5 Re4 118.72(9) 2_566 . ? Se6 Re5 Re4 58.63(7) . . ? Cl6 Re5 Re4 58.63(7) . . ? Se7 Re5 Re4 58.70(8) . . ? Cl7 Re5 Re4 58.70(8) . . ? Cl5 Re5 Re4 118.59(8) 2_566 . ? Se5 Re5 Re4 118.59(8) 2_566 . ? Cl50 Re5 Re6 134.3(2) . . ? Cl8 Re5 Re6 58.70(9) 2_566 . ? Se8 Re5 Re6 58.70(9) 2_566 . ? Se6 Re5 Re6 58.97(7) . . ? Cl6 Re5 Re6 58.97(7) . . ? Se7 Re5 Re6 118.71(9) . . ? Cl7 Re5 Re6 118.71(9) . . ? Cl5 Re5 Re6 118.36(8) 2_566 . ? Se5 Re5 Re6 118.36(8) 2_566 . ? Re4 Re5 Re6 60.02(4) . . ? Cl50 Re5 Re6 135.9(2) . 2_566 ? Cl8 Re5 Re6 118.65(8) 2_566 2_566 ? Se8 Re5 Re6 118.65(8) 2_566 2_566 ? Se6 Re5 Re6 118.59(8) . 2_566 ? Cl6 Re5 Re6 118.59(8) . 2_566 ? Se7 Re5 Re6 59.00(7) . 2_566 ? Cl7 Re5 Re6 59.00(7) . 2_566 ? Cl5 Re5 Re6 58.63(8) 2_566 2_566 ? Se5 Re5 Re6 58.63(8) 2_566 2_566 ? Re4 Re5 Re6 59.97(4) . 2_566 ? Re6 Re5 Re6 89.79(5) . 2_566 ? Cl60 Re6 Cl8 90.8(2) . 2_566 ? Cl60 Re6 Se8 90.8(2) . 2_566 ? Cl60 Re6 Se5 92.7(2) . . ? Se8 Re6 Se5 176.52(10) 2_566 . ? Cl60 Re6 Cl5 92.7(2) . . ? Cl8 Re6 Cl5 176.52(10) 2_566 . ? Cl60 Re6 Se6 91.9(2) . . ? Se8 Re6 Se6 89.54(11) 2_566 . ? Se5 Re6 Se6 89.99(11) . . ? Cl60 Re6 Cl6 91.9(2) . . ? Cl8 Re6 Cl6 89.54(11) 2_566 . ? Cl5 Re6 Cl6 89.99(11) . . ? Cl60 Re6 Cl7 91.8(2) . 2_566 ? Cl8 Re6 Cl7 90.46(11) 2_566 2_566 ? Cl5 Re6 Cl7 89.79(11) . 2_566 ? Cl6 Re6 Cl7 176.36(10) . 2_566 ? Cl60 Re6 Se7 91.8(2) . 2_566 ? Se8 Re6 Se7 90.46(11) 2_566 2_566 ? Se5 Re6 Se7 89.79(11) . 2_566 ? Se6 Re6 Se7 176.36(10) . 2_566 ? Cl60 Re6 Re4 134.2(2) . 2_566 ? Cl8 Re6 Re4 58.83(8) 2_566 2_566 ? Se8 Re6 Re4 58.83(8) 2_566 2_566 ? Se5 Re6 Re4 118.57(8) . 2_566 ? Cl5 Re6 Re4 118.57(8) . 2_566 ? Se6 Re6 Re4 118.62(8) . 2_566 ? Cl6 Re6 Re4 118.62(8) . 2_566 ? Cl7 Re6 Re4 58.48(8) 2_566 2_566 ? Se7 Re6 Re4 58.48(8) 2_566 2_566 ? Cl60 Re6 Re5 134.3(2) . . ? Cl8 Re6 Re5 58.38(8) 2_566 . ? Se8 Re6 Re5 58.38(8) 2_566 . ? Se5 Re6 Re5 118.60(8) . . ? Cl5 Re6 Re5 118.60(8) . . ? Se6 Re6 Re5 58.36(8) . . ? Cl6 Re6 Re5 58.36(8) . . ? Cl7 Re6 Re5 118.74(9) 2_566 . ? Se7 Re6 Re5 118.74(9) 2_566 . ? Re4 Re6 Re5 60.26(4) 2_566 . ? Cl60 Re6 Re4 135.6(2) . . ? Cl8 Re6 Re4 118.35(8) 2_566 . ? Se8 Re6 Re4 118.35(8) 2_566 . ? Se5 Re6 Re4 58.62(8) . . ? Cl5 Re6 Re4 58.62(8) . . ? Se6 Re6 Re4 58.42(7) . . ? Cl6 Re6 Re4 58.42(7) . . ? Cl7 Re6 Re4 118.55(7) 2_566 . ? Se7 Re6 Re4 118.55(7) 2_566 . ? Re4 Re6 Re4 90.19(5) 2_566 . ? Re5 Re6 Re4 59.98(4) . . ? Re3 Se1 Re1 63.09(7) . . ? Re3 Se1 Re2 63.12(7) . 2_556 ? Re1 Se1 Re2 62.91(7) . 2_556 ? Re1 Se2 Re2 62.96(7) . . ? Re1 Se2 Re3 62.88(7) . . ? Re2 Se2 Re3 62.79(7) . . ? Re2 Se3 Re1 62.96(7) 2_556 2_556 ? Re2 Se3 Re3 62.95(7) 2_556 . ? Re1 Se3 Re3 62.86(7) 2_556 . ? Re3 Se4 Re2 62.91(9) . . ? Re3 Se4 Re1 62.86(8) . 2_556 ? Re2 Se4 Re1 62.78(8) . 2_556 ? Re5 Se5 Re4 63.01(8) 2_566 . ? Re5 Se5 Re6 62.77(8) 2_566 . ? Re4 Se5 Re6 62.75(8) . . ? Re5 Se6 Re4 62.85(8) . . ? Re5 Se6 Re6 62.67(8) . . ? Re4 Se6 Re6 62.65(7) . . ? Re5 Se7 Re4 62.81(7) . . ? Re5 Se7 Re6 62.67(7) . 2_566 ? Re4 Se7 Re6 62.55(7) . 2_566 ? Re5 Se8 Re6 62.92(8) 2_566 2_566 ? Re5 Se8 Re4 63.08(8) 2_566 . ? Re6 Se8 Re4 62.67(8) 2_566 . ? Re3 Cl1 Re1 63.09(7) . . ? Re3 Cl1 Re2 63.12(7) . 2_556 ? Re1 Cl1 Re2 62.91(7) . 2_556 ? Re1 Cl2 Re2 62.96(7) . . ? Re1 Cl2 Re3 62.88(7) . . ? Re2 Cl2 Re3 62.79(7) . . ? Re2 Cl3 Re1 62.96(7) 2_556 2_556 ? Re2 Cl3 Re3 62.95(7) 2_556 . ? Re1 Cl3 Re3 62.86(7) 2_556 . ? Re3 Cl4 Re2 62.91(9) . . ? Re3 Cl4 Re1 62.86(8) . 2_556 ? Re2 Cl4 Re1 62.78(8) . 2_556 ? Re5 Cl5 Re4 63.01(8) 2_566 . ? Re5 Cl5 Re6 62.77(8) 2_566 . ? Re4 Cl5 Re6 62.75(8) . . ? Re5 Cl6 Re4 62.85(8) . . ? Re5 Cl6 Re6 62.67(8) . . ? Re4 Cl6 Re6 62.65(7) . . ? Re5 Cl7 Re4 62.81(7) . . ? Re5 Cl7 Re6 62.67(7) . 2_566 ? Re4 Cl7 Re6 62.55(7) . 2_566 ? Re5 Cl8 Re6 62.92(8) 2_566 2_566 ? Re5 Cl8 Re4 63.08(8) 2_566 . ? Re6 Cl8 Re4 62.67(8) 2_566 . ? C13 N1 C1 108.8(17) . . ? C13 N1 C9 107.5(17) . . ? C1 N1 C9 108.7(16) . . ? C13 N1 C5 112.9(16) . . ? C1 N1 C5 108.8(15) . . ? C9 N1 C5 110.2(17) . . ? C2 C1 N1 116.8(18) . . ? C1 C2 C3 107.6(21) . . ? C4 C3 C2 116.6(25) . . ? C6 C5 N1 116.7(17) . . ? C5 C6 C7 109.2(18) . . ? C6 C7 C8 109.1(20) . . ? C10 C9 N1 115.9(20) . . ? C9 C10 C11 105.6(21) . . ? C12 C11 C10 115.6(35) . . ? N1 C13 C14 114.5(18) . . ? C15 C14 C13 110.5(19) . . ? C14 C15 C16 112.5(20) . . ? _refine_diff_density_max 2.050 _refine_diff_density_min -2.605 _refine_diff_density_rms 0.531 #################### Material relevant to compound 3 #################### data_tba2rese _database_code_CSD 146274 _audit_creation_method SHELXL-97 _chemical_name_systematic ; bis-tetra-n-butylammonium hexa-\m~eq~3-seleno-di-\m~eq~3-chloro- hexachloro-octahedro-hexarhenate(III) ; _chemical_name_common '(nBu4N)2[Re6Se6Cl8]' _chemical_formula_moiety '(C16 H36 N 1+)2, Re6 Se6 Cl8 2-' _chemical_formula_structural '((C4H9)4N)2 (Re6Se6Cl8)' _chemical_formula_sum 'C32 H72 Cl8 N2 Re6 Se6' _chemical_formula_weight 2359.48 _chemical_melting_point ? 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' 'Se' 'Se' -0.0929 2.2259 '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 12.833(3) _cell_length_b 11.588(2) _cell_length_c 18.563(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.04(3) _cell_angle_gamma 90.00 _cell_volume 2760.3(10) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 6.2 _cell_measurement_theta_max 11.1 _exptl_crystal_description octahedron _exptl_crystal_colour 'intense red' _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.839 _exptl_crystal_density_method 'none' _exptl_crystal_F_000 2136 _exptl_absorpt_coefficient_mu 17.472 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.2740 _exptl_absorpt_correction_T_max 0.2740 _exptl_absorpt_process_details 'SHELXTL (Sheldrick, 1995)' _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 'Enraf-Nonius CAD4' _diffrn_measurement_method \w--2\q _diffrn_refln_scan_width 1.00 _diffrn_standards_number 3 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% ? _diffrn_reflns_number 4605 _diffrn_reflns_av_R_equivalents 0.0240 _diffrn_reflns_av_sigmaI/netI 0.0528 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 24.97 _reflns_number_total 4605 _reflns_number_gt 2657 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 EXPRESS' _computing_cell_refinement 'CAD4 EXPRESS' _computing_data_reduction 'XCAD4 (Harms, 1993)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'ORTEP (Johnson, 1976)' _computing_publication_material 'SHELXL-93 (Sheldrick, 1993)' _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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4605 _refine_ls_number_parameters 252 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1272 _refine_ls_R_factor_gt 0.0539 _refine_ls_wR_factor_ref 0.1885 _refine_ls_wR_factor_gt 0.1588 _refine_ls_goodness_of_fit_ref 1.201 _refine_ls_restrained_S_all 1.201 _refine_ls_shift/su_max 0.051 _refine_ls_shift/su_mean 0.003 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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re 0.05161(6) 0.06382(7) 0.08351(4) 0.0370(3) Uani 1 1 d . . . Re2 Re -0.13055(5) 0.05751(7) 0.02087(4) 0.0387(3) Uani 1 1 d . . . Re3 Re -0.03170(6) -0.13413(7) 0.04904(4) 0.0380(3) Uani 1 1 d . . . Se1 Se -0.04557(19) 0.2450(2) 0.05243(13) 0.0510(10) Uani 0.854(17) 1 d P . . Se2 Se 0.14473(16) -0.1233(2) 0.10622(12) 0.0438(9) Uani 0.828(16) 1 d P . . Se3 Se 0.20423(18) 0.1352(2) 0.01352(14) 0.0517(11) Uani 0.722(17) 1 d P . . Se4 Se -0.1048(2) -0.0094(3) 0.14725(14) 0.0503(12) Uani 0.520(17) 1 d P . . Cl1 Cl -0.04557(19) 0.2450(2) 0.05243(13) 0.0510(10) Uani 0.14(2) 1 d P . . Cl2 Cl 0.14473(16) -0.1233(2) 0.10622(12) 0.0438(9) Uani 0.17(2) 1 d P . . Cl3 Cl 0.20423(18) 0.1352(2) 0.01352(14) 0.0517(11) Uani 0.28(2) 1 d P . . Cl4 Cl -0.1048(2) -0.0094(3) 0.14725(14) 0.0503(12) Uani 0.48(2) 1 d P . . Cl10 Cl 0.1171(5) 0.1427(5) 0.1928(3) 0.0612(16) Uani 1 1 d . . . Cl20 Cl -0.3009(4) 0.1259(7) 0.0486(3) 0.073(2) Uani 1 1 d . . . Cl30 Cl -0.0776(5) -0.3031(6) 0.1142(3) 0.0686(17) Uani 1 1 d . . . N1 N 0.0265(14) 0.4710(18) 0.2915(9) 0.059(5) Uani 1 1 d . . . C1 C 0.1338(18) 0.453(2) 0.2567(14) 0.072(7) Uani 1 1 d . . . H1A H 0.1872 0.4701 0.2921 0.086 Uiso 1 1 calc R . . H1B H 0.1408 0.3718 0.2439 0.086 Uiso 1 1 calc R . . C2 C 0.154(2) 0.528(3) 0.1872(15) 0.094(10) Uani 1 1 d . . . H2A H 0.0920 0.5723 0.1769 0.113 Uiso 1 1 calc R . . H2B H 0.2098 0.5823 0.1978 0.113 Uiso 1 1 calc R . . C3 C 0.182(4) 0.465(3) 0.1249(17) 0.20(3) Uani 1 1 d . . . H3A H 0.1251 0.4113 0.1166 0.237 Uiso 1 1 calc R . . H3B H 0.2416 0.4185 0.1383 0.237 Uiso 1 1 calc R . . C4 C 0.206(3) 0.512(3) 0.0572(16) 0.125(14) Uani 1 1 d . . . H4A H 0.2162 0.4509 0.0231 0.188 Uiso 1 1 calc R . . H4B H 0.2683 0.5574 0.0608 0.188 Uiso 1 1 calc R . . H4C H 0.1494 0.5603 0.0414 0.188 Uiso 1 1 calc R . . C5 C -0.0528(16) 0.429(3) 0.2407(13) 0.074(8) Uani 1 1 d . . . H5A H -0.0492 0.4775 0.1980 0.089 Uiso 1 1 calc R . . H5B H -0.0333 0.3519 0.2262 0.089 Uiso 1 1 calc R . . C6 C -0.1605(16) 0.426(4) 0.2636(18) 0.126(16) Uani 1 1 d . . . H6A H -0.1905 0.5025 0.2590 0.151 Uiso 1 1 calc R . . H6B H -0.1633 0.4044 0.3141 0.151 Uiso 1 1 calc R . . C7 C -0.232(3) 0.332(6) 0.2151(18) 0.20(4) Uani 1 1 d . . . H7A H -0.1929 0.2660 0.1974 0.241 Uiso 1 1 calc R . . H7B H -0.2957 0.3071 0.2389 0.241 Uiso 1 1 calc R . . C8 C -0.247(4) 0.418(5) 0.164(3) 0.22(4) Uani 1 1 d . . . H8A H -0.2891 0.3887 0.1253 0.337 Uiso 1 1 calc R . . H8B H -0.1809 0.4425 0.1457 0.337 Uiso 1 1 calc R . . H8C H -0.2819 0.4823 0.1860 0.337 Uiso 1 1 calc R . . C9 C 0.005(2) 0.596(2) 0.3054(11) 0.072(8) Uani 1 1 d . . . H9A H 0.0018 0.6348 0.2591 0.086 Uiso 1 1 calc R . . H9B H -0.0633 0.6018 0.3271 0.086 Uiso 1 1 calc R . . C10 C 0.0809(19) 0.663(2) 0.3527(14) 0.075(8) Uani 1 1 d . . . H10A H 0.1498 0.6609 0.3312 0.090 Uiso 1 1 calc R . . H10B H 0.0850 0.6264 0.3997 0.090 Uiso 1 1 calc R . . C11 C 0.045(2) 0.790(3) 0.3611(14) 0.083(8) Uani 1 1 d . . . H11A H -0.0261 0.7897 0.3796 0.099 Uiso 1 1 calc R . . H11B H 0.0885 0.8270 0.3966 0.099 Uiso 1 1 calc R . . C12 C 0.047(3) 0.857(3) 0.2951(17) 0.123(13) Uani 1 1 d . . . H12A H 0.0253 0.9349 0.3052 0.185 Uiso 1 1 calc R . . H12B H 0.0006 0.8237 0.2603 0.185 Uiso 1 1 calc R . . H12C H 0.1166 0.8581 0.2761 0.185 Uiso 1 1 calc R . . C13 C 0.023(2) 0.412(3) 0.3633(13) 0.093(10) Uani 1 1 d . . . H13A H -0.0425 0.4307 0.3862 0.111 Uiso 1 1 calc R . . H13B H 0.0783 0.4443 0.3931 0.111 Uiso 1 1 calc R . . C14 C 0.036(3) 0.279(3) 0.3615(18) 0.112(12) Uani 1 1 d . . . H14A H -0.0018 0.2485 0.3204 0.135 Uiso 1 1 calc R . . H14B H 0.1088 0.2599 0.3560 0.135 Uiso 1 1 calc R . . C15 C -0.006(4) 0.225(3) 0.4300(14) 0.138(16) Uani 1 1 d . . . H15A H 0.0489 0.2305 0.4659 0.165 Uiso 1 1 calc R . . H15B H -0.0628 0.2733 0.4467 0.165 Uiso 1 1 calc R . . C16 C -0.036(5) 0.130(4) 0.430(2) 0.24(4) Uani 1 1 d . . . H16A H -0.0575 0.1089 0.4779 0.367 Uiso 1 1 calc R . . H16B H 0.0194 0.0792 0.4150 0.367 Uiso 1 1 calc R . . H16C H -0.0936 0.1225 0.3977 0.367 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 0.0390(4) 0.0433(5) 0.0287(4) 0.0014(3) -0.0034(3) 0.0000(3) Re2 0.0331(4) 0.0509(6) 0.0320(5) 0.0038(4) 0.0013(3) 0.0052(4) Re3 0.0388(4) 0.0432(5) 0.0321(5) 0.0064(3) -0.0017(3) -0.0026(4) Se1 0.0649(17) 0.0457(16) 0.0424(15) -0.0046(11) -0.0061(11) 0.0123(12) Se2 0.0418(14) 0.0517(17) 0.0380(15) 0.0057(10) -0.0084(10) 0.0050(10) Se3 0.0395(15) 0.065(2) 0.0505(18) 0.0098(13) -0.0072(11) -0.0141(12) Se4 0.0488(18) 0.070(2) 0.0315(17) 0.0062(15) 0.0087(12) 0.0084(16) Cl1 0.0649(17) 0.0457(16) 0.0424(15) -0.0046(11) -0.0061(11) 0.0123(12) Cl2 0.0418(14) 0.0517(17) 0.0380(15) 0.0057(10) -0.0084(10) 0.0050(10) Cl3 0.0395(15) 0.065(2) 0.0505(18) 0.0098(13) -0.0072(11) -0.0141(12) Cl4 0.0488(18) 0.070(2) 0.0315(17) 0.0062(15) 0.0087(12) 0.0084(16) Cl10 0.082(4) 0.062(4) 0.040(3) -0.009(3) -0.021(3) 0.005(3) Cl20 0.047(3) 0.110(6) 0.063(4) 0.006(4) 0.011(3) 0.026(3) Cl30 0.086(4) 0.059(4) 0.061(4) 0.027(3) -0.005(3) -0.024(3) N1 0.051(10) 0.087(15) 0.040(10) -0.010(10) 0.007(8) 0.004(10) C1 0.065(15) 0.076(19) 0.075(17) 0.016(15) -0.016(13) 0.017(14) C2 0.053(15) 0.14(3) 0.09(2) 0.02(2) 0.021(14) -0.003(17) C3 0.37(7) 0.15(4) 0.07(2) 0.03(2) 0.07(3) 0.17(5) C4 0.17(3) 0.12(3) 0.09(2) 0.02(2) 0.06(2) 0.03(3) C5 0.049(13) 0.11(2) 0.061(16) 0.002(16) -0.001(12) -0.012(14) C6 0.024(12) 0.24(5) 0.11(3) -0.07(3) -0.005(13) 0.009(19) C7 0.07(2) 0.47(12) 0.05(2) -0.06(4) -0.011(18) 0.03(4) C8 0.13(4) 0.26(8) 0.29(8) -0.20(7) -0.04(5) 0.02(4) C9 0.101(19) 0.092(19) 0.023(11) -0.024(12) -0.006(12) 0.045(16) C10 0.070(16) 0.09(2) 0.067(17) -0.028(15) -0.028(13) 0.012(14) C11 0.11(2) 0.09(2) 0.054(16) 0.000(15) 0.002(15) -0.011(18) C12 0.15(3) 0.12(3) 0.10(3) 0.03(2) 0.00(2) 0.01(3) C13 0.08(2) 0.15(3) 0.048(16) 0.006(18) -0.007(14) -0.01(2) C14 0.16(3) 0.08(2) 0.10(3) -0.01(2) -0.02(2) 0.01(2) C15 0.28(5) 0.11(3) 0.024(15) 0.008(17) -0.01(2) -0.02(3) C16 0.50(10) 0.11(4) 0.12(4) -0.01(3) 0.09(5) -0.14(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 Cl10 2.379(5) . ? Re1 Se4 2.480(3) . ? Re1 Se3 2.492(3) . ? Re1 Se1 2.509(3) . ? Re1 Se2 2.511(2) . ? Re1 Re2 2.5999(12) 3 ? Re1 Re3 2.6043(11) 3 ? Re1 Re3 2.6101(12) . ? Re2 Cl20 2.382(5) . ? Re2 Cl2 2.486(2) 3 ? Re2 Se2 2.486(2) 3 ? Re2 Se4 2.492(3) . ? Re2 Se1 2.500(3) . ? Re2 Cl3 2.508(3) 3 ? Re2 Se3 2.508(3) 3 ? Re2 Re1 2.5999(12) 3 ? Re2 Re3 2.6099(12) 3 ? Re2 Re3 2.6102(12) . ? Re3 Cl30 2.376(5) . ? Re3 Cl1 2.487(3) 3 ? Re3 Se1 2.487(3) 3 ? Re3 Cl3 2.499(3) 3 ? Re3 Se3 2.499(3) 3 ? Re3 Se2 2.503(2) . ? Re3 Se4 2.509(3) . ? Re3 Re1 2.6043(11) 3 ? Re3 Re2 2.6099(12) 3 ? Se1 Re3 2.487(3) 3 ? Se2 Re2 2.486(2) 3 ? Se3 Re3 2.499(3) 3 ? Se3 Re2 2.508(3) 3 ? N1 C5 1.47(3) . ? N1 C13 1.50(3) . ? N1 C9 1.50(3) . ? N1 C1 1.54(3) . ? C1 C2 1.58(4) . ? C2 C3 1.41(4) . ? C3 C4 1.40(4) . ? C5 C6 1.45(3) . ? C6 C7 1.69(6) . ? C7 C8 1.39(8) . ? C9 C10 1.52(3) . ? C10 C11 1.55(4) . ? C11 C12 1.46(3) . ? C13 C14 1.55(4) . ? C14 C15 1.52(4) . ? C15 C16 1.17(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl10 Re1 Se4 90.57(17) . . ? Cl10 Re1 Se3 92.29(17) . . ? Se4 Re1 Se3 177.07(9) . . ? Cl10 Re1 Se1 92.84(16) . . ? Se4 Re1 Se1 89.63(10) . . ? Se3 Re1 Se1 89.60(9) . . ? Cl10 Re1 Se2 91.21(15) . . ? Se4 Re1 Se2 90.55(9) . . ? Se3 Re1 Se2 90.01(9) . . ? Se1 Re1 Se2 175.94(8) . . ? Cl10 Re1 Re2 134.93(15) . 3 ? Se4 Re1 Re2 119.10(8) . 3 ? Se3 Re1 Re2 58.96(7) . 3 ? Se1 Re1 Re2 118.36(6) . 3 ? Se2 Re1 Re2 58.17(6) . 3 ? Cl10 Re1 Re3 136.06(16) . 3 ? Se4 Re1 Re3 118.61(7) . 3 ? Se3 Re1 Re3 58.68(6) . 3 ? Se1 Re1 Re3 58.17(6) . 3 ? Se2 Re1 Re3 118.37(6) . 3 ? Re2 Re1 Re3 60.21(3) 3 3 ? Cl10 Re1 Re3 133.74(16) . . ? Se4 Re1 Re3 58.99(8) . . ? Se3 Re1 Re3 119.07(8) . . ? Se1 Re1 Re3 118.39(7) . . ? Se2 Re1 Re3 58.48(6) . . ? Re2 Re1 Re3 60.12(3) 3 . ? Re3 Re1 Re3 90.20(4) 3 . ? Cl20 Re2 Cl2 92.07(17) . 3 ? Cl20 Re2 Se2 92.07(17) . 3 ? Cl2 Re2 Se2 0.00(11) 3 3 ? Cl20 Re2 Se4 91.23(17) . . ? Cl2 Re2 Se4 176.56(8) 3 . ? Se2 Re2 Se4 176.56(8) 3 . ? Cl20 Re2 Se1 93.5(2) . . ? Cl2 Re2 Se1 89.28(8) 3 . ? Se2 Re2 Se1 89.28(8) 3 . ? Se4 Re2 Se1 89.56(10) . . ? Cl20 Re2 Cl3 90.3(2) . 3 ? Cl2 Re2 Cl3 90.25(8) 3 3 ? Se2 Re2 Cl3 90.25(8) 3 3 ? Se4 Re2 Cl3 90.70(10) . 3 ? Se1 Re2 Cl3 176.21(8) . 3 ? Cl20 Re2 Se3 90.3(2) . 3 ? Cl2 Re2 Se3 90.25(8) 3 3 ? Se2 Re2 Se3 90.25(8) 3 3 ? Se4 Re2 Se3 90.70(10) . 3 ? Se1 Re2 Se3 176.21(8) . 3 ? Cl3 Re2 Se3 0.00(16) 3 3 ? Cl20 Re2 Re1 134.34(17) . 3 ? Cl2 Re2 Re1 59.13(6) 3 3 ? Se2 Re2 Re1 59.13(6) 3 3 ? Se4 Re2 Re1 118.80(8) . 3 ? Se1 Re2 Re1 118.32(6) . 3 ? Cl3 Re2 Re1 58.38(7) 3 3 ? Se3 Re2 Re1 58.38(7) 3 3 ? Cl20 Re2 Re3 136.61(18) . 3 ? Cl2 Re2 Re3 58.78(6) 3 3 ? Se2 Re2 Re3 58.78(6) 3 3 ? Se4 Re2 Re3 117.94(8) . 3 ? Se1 Re2 Re3 58.19(6) . 3 ? Cl3 Re2 Re3 118.50(7) 3 3 ? Se3 Re2 Re3 118.50(7) 3 3 ? Re1 Re2 Re3 60.13(3) 3 3 ? Cl20 Re2 Re3 133.31(18) . . ? Cl2 Re2 Re3 119.10(7) 3 . ? Se2 Re2 Re3 119.10(7) 3 . ? Se4 Re2 Re3 58.85(8) . . ? Se1 Re2 Re3 118.71(6) . . ? Cl3 Re2 Re3 58.42(7) 3 . ? Se3 Re2 Re3 58.42(7) 3 . ? Re1 Re2 Re3 59.98(3) 3 . ? Re3 Re2 Re3 90.07(3) 3 . ? Cl30 Re3 Cl1 93.39(18) . 3 ? Cl30 Re3 Se1 93.39(18) . 3 ? Cl1 Re3 Se1 0.00(15) 3 3 ? Cl30 Re3 Cl3 90.71(16) . 3 ? Cl1 Re3 Cl3 89.94(9) 3 3 ? Se1 Re3 Cl3 89.94(9) 3 3 ? Cl30 Re3 Se3 90.71(16) . 3 ? Cl1 Re3 Se3 89.94(9) 3 3 ? Se1 Re3 Se3 89.94(9) 3 3 ? Cl3 Re3 Se3 0.00(11) 3 3 ? Cl30 Re3 Se2 92.87(16) . . ? Cl1 Re3 Se2 89.20(8) 3 . ? Se1 Re3 Se2 89.20(8) 3 . ? Cl3 Re3 Se2 176.36(9) 3 . ? Se3 Re3 Se2 176.36(9) 3 . ? Cl30 Re3 Se4 90.68(19) . . ? Cl1 Re3 Se4 175.90(10) 3 . ? Se1 Re3 Se4 175.90(10) 3 . ? Cl3 Re3 Se4 90.51(10) 3 . ? Se3 Re3 Se4 90.51(10) 3 . ? Se2 Re3 Se4 90.09(9) . . ? Cl30 Re3 Re1 135.60(16) . 3 ? Cl1 Re3 Re1 58.99(6) 3 3 ? Se1 Re3 Re1 58.99(6) 3 3 ? Cl3 Re3 Re1 58.42(7) 3 3 ? Se3 Re3 Re1 58.42(7) 3 3 ? Se2 Re3 Re1 118.23(7) . 3 ? Se4 Re3 Re1 118.02(8) . 3 ? Cl30 Re3 Re2 137.03(17) . 3 ? Cl1 Re3 Re2 58.69(7) 3 3 ? Se1 Re3 Re2 58.69(7) 3 3 ? Cl3 Re3 Re2 118.52(7) 3 3 ? Se3 Re3 Re2 118.52(7) 3 3 ? Se2 Re3 Re2 58.14(6) . 3 ? Se4 Re3 Re2 117.66(8) . 3 ? Re1 Re3 Re2 60.10(3) 3 3 ? Cl30 Re3 Re2 133.04(17) . . ? Cl1 Re3 Re2 118.79(6) 3 . ? Se1 Re3 Re2 118.79(6) 3 . ? Cl3 Re3 Re2 58.74(7) 3 . ? Se3 Re3 Re2 58.74(7) 3 . ? Se2 Re3 Re2 118.79(7) . . ? Se4 Re3 Re2 58.23(7) . . ? Re1 Re3 Re2 59.81(3) 3 . ? Re2 Re3 Re2 89.93(3) 3 . ? Re3 Se1 Re2 63.12(6) 3 . ? Re3 Se1 Re1 62.84(6) 3 . ? Re2 Se1 Re1 62.84(7) . . ? Re2 Se2 Re3 63.09(6) 3 . ? Re2 Se2 Re1 62.70(6) 3 . ? Re3 Se2 Re1 62.74(5) . . ? Re1 Se3 Re3 62.90(6) . 3 ? Re1 Se3 Re2 62.66(6) . 3 ? Re3 Se3 Re2 62.84(6) 3 3 ? Re1 Se4 Re2 63.35(7) . . ? Re1 Se4 Re3 63.09(7) . . ? Re2 Se4 Re3 62.92(7) . . ? C5 N1 C13 114(2) . . ? C5 N1 C9 108(2) . . ? C13 N1 C9 106(2) . . ? C5 N1 C1 107.8(17) . . ? C13 N1 C1 109.7(19) . . ? C9 N1 C1 111.8(19) . . ? C2 C1 N1 114.6(18) . . ? C3 C2 C1 115(3) . . ? C2 C3 C4 126(4) . . ? C6 C5 N1 119(2) . . ? C5 C6 C7 112(3) . . ? C8 C7 C6 88(5) . . ? C10 C9 N1 118(2) . . ? C9 C10 C11 110(2) . . ? C12 C11 C10 115(2) . . ? N1 C13 C14 115(2) . . ? C15 C14 C13 111(3) . . ? C16 C15 C14 121(4) . . ? _diffrn_measured_fraction_theta_max 0.949 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 0.949 _refine_diff_density_max 2.069 _refine_diff_density_min -3.293 _refine_diff_density_rms 0.674 #########################################################################