#Supplementary Material (ESI) for Dalton Transactions #This journal is (c) The Royal Society of Chemistry 2001 data_ic8222 _database_code_CSD 160973 _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Chen, Po-Jui' 'Chen, Yu-Ju' 'Lee, Gene-Hsiung' 'Lee, Fang-Yuan' 'Lin, Su-Ching' 'Lu, Kuang-Lieh' 'Manimaran, Bala' 'Peng, Shie-ming' 'Rajendran, T.' _publ_contact_author_name 'Prof Kuang-Lieh Lu' _publ_contact_author_address ; Institute of Chemistry Academia Sinica Taipei 115 TAIWAN ; _publ_contact_author_email 'LU@CHEM.SINICA.EDU.TW' _publ_section_title ; Self-assembly of tetrametallic square [Re4(CO)12Br4(mu-pz)4- from [Re(CO)4Br(pz)]. A mechanistic approach ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H28 Br4 N8 O14 Re4' _chemical_formula_weight 1837.08 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Re' 'Re' -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I4(1)/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 21.3363(5) _cell_length_b 21.3363(5) _cell_length_c 15.5207(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7065.6(4) _cell_formula_units_Z 4 _cell_measurement_temperature 200(1) _cell_measurement_reflns_used all _cell_measurement_theta_min 2.51 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour orange-yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.727 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3360 _exptl_absorpt_coefficient_mu 9.138 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.157 _exptl_absorpt_correction_T_max 0.228 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(1) _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 'NONIUS KappaCCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 16937 _diffrn_reflns_av_R_equivalents 0.0556 _diffrn_reflns_av_sigmaI/netI 0.0395 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4030 _reflns_number_gt 2965 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'NONIUS KappaCCD' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0931P)^2^+42.4831P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4030 _refine_ls_number_parameters 162 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0713 _refine_ls_R_factor_gt 0.0483 _refine_ls_wR_factor_ref 0.1674 _refine_ls_wR_factor_gt 0.1404 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_restrained_S_all 1.092 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re 0.286176(15) 0.854302(15) 0.11399(3) 0.04994(17) Uani 1 1 d D . . Br1 Br 0.28680(11) 0.85066(14) 0.2801(2) 0.0602(5) Uani 0.67 1 d PD A 1 C3 C 0.2899(12) 0.8558(10) -0.0094(9) 0.053(5) Uani 0.67 1 d PD A 1 O3 O 0.2925(14) 0.8494(14) -0.0857(11) 0.111(10) Uani 0.67 1 d PD A 1 Br1' Br 0.2963(3) 0.8473(3) -0.0505(4) 0.0716(15) Uani 0.33 1 d PD A 2 C3' C 0.2738(17) 0.8568(15) 0.2389(12) 0.051(8) Uani 0.33 1 d PD A 2 O3' O 0.280(2) 0.857(2) 0.3090(17) 0.103(19) Uani 0.33 1 d PD A 2 N1 N 0.3843(3) 0.8846(3) 0.1250(5) 0.0429(15) Uani 1 1 d . A . N2 N 0.5086(3) 0.9258(3) 0.1321(4) 0.0425(14) Uani 1 1 d . . . C1 C 0.2004(5) 0.8251(5) 0.1081(7) 0.064(3) Uani 1 1 d . A . C2 C 0.2573(5) 0.9412(5) 0.1106(9) 0.075(3) Uani 1 1 d . A . C4 C 0.4030(4) 0.9246(4) 0.1823(6) 0.0498(19) Uani 1 1 d . . . H4A H 0.3735 0.9396 0.2233 0.060 Uiso 1 1 calc R A . C5 C 0.4638(4) 0.9465(4) 0.1865(6) 0.052(2) Uani 1 1 d . A . H5A H 0.4744 0.9770 0.2287 0.063 Uiso 1 1 calc R . . C6 C 0.4898(4) 0.8840(4) 0.0736(6) 0.0491(19) Uani 1 1 d . A . H6A H 0.5193 0.8681 0.0334 0.059 Uiso 1 1 calc R . . C7 C 0.4288(4) 0.8633(4) 0.0699(6) 0.0486(19) Uani 1 1 d . . . H7A H 0.4175 0.8332 0.0276 0.058 Uiso 1 1 calc R A . O1 O 0.1503(3) 0.8075(4) 0.1080(6) 0.081(3) Uani 1 1 d . . . O2 O 0.2411(4) 0.9904(4) 0.1081(8) 0.105(3) Uani 1 1 d . . . O4 O 0.5000 0.7500 -0.014(2) 0.222(13) Uiso 1 2 d S . . C8 C 0.5000 0.7500 -0.103(3) 0.155(12) Uiso 1 2 d S . . C9 C 0.5665(16) 0.7757(16) -0.136(2) 0.235(16) Uiso 1 1 d . . . H9A H 0.5929 0.7859 -0.0859 0.352 Uiso 1 1 calc R . . H9B H 0.5601 0.8134 -0.1705 0.352 Uiso 1 1 calc R . . H9C H 0.5871 0.7435 -0.1705 0.352 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 0.0367(2) 0.0413(2) 0.0718(3) 0.00668(15) 0.00554(14) 0.00232(12) Br1 0.0590(11) 0.0549(12) 0.0666(15) -0.0022(12) 0.0214(11) -0.0017(8) C3 0.058(11) 0.039(7) 0.062(13) -0.004(9) -0.018(11) 0.002(7) O3 0.103(14) 0.15(2) 0.076(16) 0.011(13) -0.023(12) -0.022(12) Br1' 0.062(2) 0.076(3) 0.076(5) 0.017(3) -0.007(4) -0.007(2) C3' 0.063(19) 0.043(14) 0.048(18) 0.020(14) -0.008(16) 0.002(12) O3' 0.15(4) 0.058(18) 0.10(4) -0.01(2) 0.05(3) 0.014(19) N1 0.032(3) 0.035(3) 0.061(4) 0.009(3) 0.000(3) -0.004(2) N2 0.037(3) 0.042(3) 0.049(4) 0.006(3) -0.002(3) 0.002(3) C1 0.049(5) 0.058(6) 0.085(7) 0.001(5) 0.002(5) 0.008(4) C2 0.046(5) 0.054(6) 0.124(10) 0.011(6) 0.012(6) 0.001(4) C4 0.045(4) 0.049(4) 0.055(5) 0.001(4) 0.010(4) 0.005(4) C5 0.052(5) 0.043(4) 0.062(5) -0.002(4) -0.002(4) -0.002(4) C6 0.045(4) 0.044(4) 0.059(5) 0.001(4) 0.008(4) -0.002(3) C7 0.038(4) 0.051(5) 0.057(5) -0.002(4) 0.004(3) -0.006(3) O1 0.042(4) 0.070(5) 0.132(8) 0.005(5) 0.004(4) -0.013(3) O2 0.072(5) 0.051(5) 0.193(11) 0.024(5) 0.013(6) 0.020(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re1 C3 1.918(15) . ? Re1 C1 1.935(11) . ? Re1 C2 1.954(11) . ? Re1 C3' 1.957(18) . ? Re1 N1 2.197(6) . ? Re1 N2 2.198(7) 12_766 ? Re1 Br1' 2.567(7) . ? Re1 Br1 2.580(3) . ? C3 O3 1.193(16) . ? C3' O3' 1.096(19) . ? N1 C4 1.297(11) . ? N1 C7 1.356(11) . ? N2 C6 1.335(11) . ? N2 C5 1.349(11) . ? N2 Re1 2.198(7) 15_565 ? C1 O1 1.135(12) . ? C2 O2 1.107(13) . ? C4 C5 1.382(12) . ? C6 C7 1.375(11) . ? O4 C8 1.38(5) . ? C8 C9 1.60(3) 6_564 ? C8 C9 1.60(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 C3 Re1 C1 89.9(8) . . ? C3 Re1 C2 88.3(8) . . ? C1 Re1 C2 90.3(4) . . ? C3 Re1 C3' 174.1(13) . . ? C1 Re1 C3' 85.9(11) . . ? C2 Re1 C3' 87.6(10) . . ? C3 Re1 N1 91.9(8) . . ? C1 Re1 N1 177.6(4) . . ? C2 Re1 N1 91.3(3) . . ? C3' Re1 N1 92.5(11) . . ? C3 Re1 N2 91.6(7) . 12_766 ? C1 Re1 N2 92.9(3) . 12_766 ? C2 Re1 N2 176.7(3) . 12_766 ? C3' Re1 N2 92.8(9) . 12_766 ? N1 Re1 N2 85.4(2) . 12_766 ? C3 Re1 Br1' 4.9(7) . . ? C1 Re1 Br1' 90.8(4) . . ? C2 Re1 Br1' 93.2(4) . . ? C3' Re1 Br1' 176.6(11) . . ? N1 Re1 Br1' 90.8(2) . . ? N2 Re1 Br1' 86.7(2) 12_766 . ? C3 Re1 Br1 177.2(8) . . ? C1 Re1 Br1 92.4(3) . . ? C2 Re1 Br1 93.3(4) . . ? C3' Re1 Br1 8.7(10) . . ? N1 Re1 Br1 85.77(19) . . ? N2 Re1 Br1 86.73(19) 12_766 . ? Br1' Re1 Br1 172.78(16) . . ? O3 C3 Re1 172(3) . . ? O3' C3' Re1 165(4) . . ? C4 N1 C7 116.0(7) . . ? C4 N1 Re1 122.7(6) . . ? C7 N1 Re1 121.3(6) . . ? C6 N2 C5 115.6(7) . . ? C6 N2 Re1 123.0(6) . 15_565 ? C5 N2 Re1 121.3(6) . 15_565 ? O1 C1 Re1 177.3(11) . . ? O2 C2 Re1 179.5(14) . . ? N1 C4 C5 123.0(8) . . ? N2 C5 C4 121.7(8) . . ? N2 C6 C7 121.8(8) . . ? N1 C7 C6 121.9(8) . . ? O4 C8 C9 108.5(19) . 6_564 ? O4 C8 C9 108.5(19) . . ? C9 C8 C9 143(4) 6_564 . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.287 _refine_diff_density_min -1.685 _refine_diff_density_rms 0.191