Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_section_title ;Rhenium Oxohalides. Synthesis and Crystal Structures of ReO3Cl(THF)2, ReOCl4(THF), Re2O3Cl6(THF)2, and Re2O3Cl6(H2O)2 ; _publ_contact_author_name 'Prof. Gregory Girolami' _publ_contact_author_email GIROLAMI@SCS.UIUC.EDU loop_ _publ_author_name G.Girolami W.Noh # Attachment 'f57xell.cif' data_f57xell _database_code_depnum_ccdc_archive 'CCDC 626967' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H36 Cl6 O9 Re2' _chemical_formula_weight 957.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.528(5) _cell_length_b 10.051(5) _cell_length_c 10.707(6) _cell_angle_alpha 66.006(8) _cell_angle_beta 67.762(8) _cell_angle_gamma 67.683(8) _cell_volume 747.9(7) _cell_formula_units_Z 1 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.126 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 456 _exptl_absorpt_coefficient_mu 8.660 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.400 _exptl_absorpt_correction_T_max 0.757 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 7745 _diffrn_reflns_av_R_equivalents 0.1201 _diffrn_reflns_av_sigmaI/netI 0.0992 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.63 _diffrn_reflns_theta_max 25.38 _reflns_number_total 2741 _reflns_number_gt 2184 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0180P)^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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2741 _refine_ls_number_parameters 157 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0561 _refine_ls_R_factor_gt 0.0388 _refine_ls_wR_factor_ref 0.0655 _refine_ls_wR_factor_gt 0.0610 _refine_ls_goodness_of_fit_ref 0.991 _refine_ls_restrained_S_all 0.990 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re 0.66555(4) 0.59313(3) 0.85836(3) 0.03644(11) Uani 1 1 d . . . O1 O 0.5000 0.5000 1.0000 0.0428(17) Uani 1 2 d S . . O2 O 0.8050(6) 0.5488(6) 0.9523(6) 0.0572(14) Uani 1 1 d . . . O3 O 0.4894(6) 0.6474(6) 0.7372(6) 0.0490(14) Uani 1 1 d D . . H34 H 0.374(6) 0.685(5) 0.756(8) 0.059 Uiso 1 1 d D . . H35 H 0.533(8) 0.651(8) 0.647(5) 0.059 Uiso 1 1 d D . . Cl1 Cl 0.7914(2) 0.38804(18) 0.7719(2) 0.0473(5) Uani 1 1 d . . . Cl2 Cl 0.8271(3) 0.7243(2) 0.6469(2) 0.0638(6) Uani 1 1 d . . . Cl3 Cl 0.4989(3) 0.8240(2) 0.8958(2) 0.0662(6) Uani 1 1 d . . . O4 O 0.1713(7) 0.8130(8) 0.7643(8) 0.103(3) Uani 1 1 d D . . C1 C 0.1357(12) 0.9359(11) 0.6509(12) 0.107(4) Uani 1 1 d . . . H1A H 0.1409 0.9032 0.5734 0.129 Uiso 1 1 calc R . . H1B H 0.2230 0.9944 0.6150 0.129 Uiso 1 1 calc R . . C2 C -0.0399(13) 1.0281(10) 0.6990(12) 0.091(3) Uani 1 1 d . . . H2A H -0.0406 1.1356 0.6677 0.109 Uiso 1 1 calc R . . H2B H -0.1246 1.0202 0.6614 0.109 Uiso 1 1 calc R . . C3 C -0.0839(13) 0.9685(10) 0.8511(12) 0.095(4) Uani 1 1 d . . . H3A H -0.2074 0.9628 0.8886 0.114 Uiso 1 1 calc R . . H3B H -0.0706 1.0349 0.8918 0.114 Uiso 1 1 calc R . . C4 C 0.0332(11) 0.8198(9) 0.8890(10) 0.071(3) Uani 1 1 d . . . H4A H 0.0785 0.8060 0.9673 0.086 Uiso 1 1 calc R . . H4B H -0.0275 0.7409 0.9188 0.086 Uiso 1 1 calc R . . O5 O 0.5839(7) 0.6560(7) 0.4751(7) 0.0802(19) Uani 1 1 d D . . C5 C 0.7347(12) 0.5552(11) 0.4142(11) 0.085(3) Uani 1 1 d . . . H5B H 0.7242 0.4502 0.4596 0.102 Uiso 1 1 calc R . . H5C H 0.8422 0.5592 0.4262 0.102 Uiso 1 1 calc R . . C6 C 0.7421(12) 0.6061(12) 0.2623(11) 0.076(3) Uani 1 1 d . . . H6B H 0.8646 0.6010 0.2032 0.091 Uiso 1 1 calc R . . H6C H 0.6954 0.5422 0.2428 0.091 Uiso 1 1 calc R . . C7 C 0.638(2) 0.7553(14) 0.2340(13) 0.155(7) Uani 1 1 d . . . H7B H 0.5608 0.7716 0.1766 0.186 Uiso 1 1 calc R . . H7C H 0.7133 0.8257 0.1799 0.186 Uiso 1 1 calc R . . C8 C 0.5325(14) 0.7833(13) 0.3676(12) 0.104(4) Uani 1 1 d . . . H8A H 0.5507 0.8723 0.3728 0.125 Uiso 1 1 calc R . . H8B H 0.4062 0.8036 0.3768 0.125 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 0.04238(18) 0.03530(16) 0.0273(2) -0.00770(11) -0.00564(13) -0.01153(11) O1 0.045(4) 0.033(3) 0.041(5) -0.016(3) 0.002(3) -0.010(3) O2 0.064(3) 0.073(3) 0.046(4) -0.027(3) -0.019(3) -0.015(3) O3 0.036(3) 0.065(3) 0.033(4) -0.020(3) -0.004(3) 0.001(2) Cl1 0.0528(11) 0.0423(9) 0.0360(13) -0.0160(8) -0.0031(9) -0.0060(7) Cl2 0.0694(13) 0.0579(11) 0.0483(16) -0.0099(10) 0.0107(11) -0.0339(9) Cl3 0.0882(15) 0.0370(10) 0.0547(16) -0.0194(10) 0.0024(12) -0.0129(9) O4 0.052(4) 0.129(6) 0.054(6) -0.013(4) -0.006(4) 0.028(4) C1 0.080(7) 0.099(8) 0.057(9) 0.003(6) -0.007(6) 0.025(6) C2 0.096(8) 0.065(6) 0.080(10) -0.033(6) -0.028(7) 0.028(5) C3 0.087(7) 0.070(6) 0.059(9) -0.004(5) 0.007(6) 0.008(5) C4 0.064(6) 0.081(6) 0.040(7) -0.005(5) -0.005(5) -0.013(4) O5 0.059(4) 0.115(5) 0.040(5) -0.028(4) -0.012(3) 0.007(3) C5 0.080(7) 0.090(7) 0.051(8) -0.027(6) -0.009(6) 0.009(5) C6 0.069(6) 0.126(8) 0.029(7) -0.036(6) -0.001(5) -0.021(5) C7 0.230(15) 0.093(9) 0.045(9) -0.025(7) -0.013(9) 0.039(9) C8 0.114(8) 0.110(8) 0.042(8) -0.027(6) -0.025(7) 0.028(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 O2 1.662(5) . ? Re1 O1 1.8434(7) . ? Re1 O3 2.125(6) . ? Re1 Cl2 2.314(2) . ? Re1 Cl1 2.3189(19) . ? Re1 Cl3 2.321(2) . ? O1 Re1 1.8434(7) 2_667 ? O3 H34 0.88(5) . ? O3 H35 0.88(5) . ? O4 C1 1.366(11) . ? O4 C4 1.413(10) . ? C1 C2 1.456(11) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.437(13) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.441(11) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? O5 C8 1.382(11) . ? O5 C5 1.421(9) . ? C5 C6 1.476(13) . ? C5 H5B 0.9900 . ? C5 H5C 0.9900 . ? C6 C7 1.398(13) . ? C6 H6B 0.9900 . ? C6 H6C 0.9900 . ? C7 C8 1.448(13) . ? C7 H7B 0.9900 . ? C7 H7C 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? 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 O2 Re1 O1 98.1(2) . . ? O2 Re1 O3 179.2(2) . . ? O1 Re1 O3 81.99(14) . . ? O2 Re1 Cl2 96.1(2) . . ? O1 Re1 Cl2 165.76(6) . . ? O3 Re1 Cl2 83.77(15) . . ? O2 Re1 Cl1 97.92(17) . . ? O1 Re1 Cl1 90.99(6) . . ? O3 Re1 Cl1 81.32(14) . . ? Cl2 Re1 Cl1 86.64(8) . . ? O2 Re1 Cl3 97.71(18) . . ? O1 Re1 Cl3 90.64(6) . . ? O3 Re1 Cl3 83.04(14) . . ? Cl2 Re1 Cl3 87.85(8) . . ? Cl1 Re1 Cl3 163.89(8) . . ? Re1 O1 Re1 180.00(3) 2_667 . ? Re1 O3 H34 131(5) . . ? Re1 O3 H35 118(4) . . ? H34 O3 H35 110(7) . . ? C1 O4 C4 111.7(6) . . ? O4 C1 C2 107.4(9) . . ? O4 C1 H1A 110.2 . . ? C2 C1 H1A 110.2 . . ? O4 C1 H1B 110.2 . . ? C2 C1 H1B 110.2 . . ? H1A C1 H1B 108.5 . . ? C3 C2 C1 105.1(8) . . ? C3 C2 H2A 110.7 . . ? C1 C2 H2A 110.7 . . ? C3 C2 H2B 110.7 . . ? C1 C2 H2B 110.7 . . ? H2A C2 H2B 108.8 . . ? C2 C3 C4 107.9(8) . . ? C2 C3 H3A 110.1 . . ? C4 C3 H3A 110.1 . . ? C2 C3 H3B 110.1 . . ? C4 C3 H3B 110.1 . . ? H3A C3 H3B 108.4 . . ? O4 C4 C3 104.8(8) . . ? O4 C4 H4A 110.8 . . ? C3 C4 H4A 110.8 . . ? O4 C4 H4B 110.8 . . ? C3 C4 H4B 110.8 . . ? H4A C4 H4B 108.9 . . ? C8 O5 C5 108.8(7) . . ? O5 C5 C6 105.9(7) . . ? O5 C5 H5B 110.5 . . ? C6 C5 H5B 110.5 . . ? O5 C5 H5C 110.5 . . ? C6 C5 H5C 110.5 . . ? H5B C5 H5C 108.7 . . ? C7 C6 C5 105.5(8) . . ? C7 C6 H6B 110.6 . . ? C5 C6 H6B 110.6 . . ? C7 C6 H6C 110.6 . . ? C5 C6 H6C 110.6 . . ? H6B C6 H6C 108.8 . . ? C6 C7 C8 108.4(10) . . ? C6 C7 H7B 110.0 . . ? C8 C7 H7B 110.0 . . ? C6 C7 H7C 110.0 . . ? C8 C7 H7C 110.0 . . ? H7B C7 H7C 108.4 . . ? O5 C8 C7 107.7(8) . . ? O5 C8 H8A 110.2 . . ? C7 C8 H8A 110.2 . . ? O5 C8 H8B 110.2 . . ? C7 C8 H8B 110.2 . . ? H8A C8 H8B 108.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.38 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.234 _refine_diff_density_min -1.638 _refine_diff_density_rms 0.187 # Attachment 'f66yell.cif' data_f66yell _database_code_depnum_ccdc_archive 'CCDC 626968' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H16 Cl O5 Re' _chemical_formula_weight 413.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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)/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 7.724(2) _cell_length_b 12.795(3) _cell_length_c 12.204(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.412(4) _cell_angle_gamma 90.00 _cell_volume 1193.0(5) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.304 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 784 _exptl_absorpt_coefficient_mu 10.408 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.057 _exptl_absorpt_correction_T_max 0.125 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 10983 _diffrn_reflns_av_R_equivalents 0.0815 _diffrn_reflns_av_sigmaI/netI 0.0557 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_theta_max 28.33 _reflns_number_total 2919 _reflns_number_gt 2386 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0400P)^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 0.0041(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2919 _refine_ls_number_parameters 137 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0404 _refine_ls_R_factor_gt 0.0297 _refine_ls_wR_factor_ref 0.0749 _refine_ls_wR_factor_gt 0.0714 _refine_ls_goodness_of_fit_ref 0.956 _refine_ls_restrained_S_all 0.956 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re 0.27865(3) 1.033409(13) 0.267984(16) 0.02506(10) Uani 1 1 d . . . O1 O 0.0691(5) 1.0692(3) 0.2163(3) 0.0370(9) Uani 1 1 d . . . O2 O 0.3541(5) 1.1358(3) 0.3513(3) 0.0377(9) Uani 1 1 d . . . O3 O 0.2514(5) 0.9376(3) 0.3628(3) 0.0281(8) Uani 1 1 d . . . Cl1 Cl 0.38866(19) 1.10951(10) 0.10953(11) 0.0387(3) Uani 1 1 d . . . O4 O 0.5519(5) 0.9651(2) 0.2893(3) 0.0305(8) Uani 1 1 d . . . C1 C 0.6266(7) 0.9242(4) 0.3978(4) 0.0362(12) Uani 1 1 d . . . H1A H 0.5631 0.8607 0.4157 0.043 Uiso 1 1 calc R . . H1B H 0.6196 0.9770 0.4562 0.043 Uiso 1 1 calc R . . C2 C 0.8144(7) 0.8987(5) 0.3894(5) 0.0415(13) Uani 1 1 d . . . H2A H 0.8567 0.8392 0.4378 0.050 Uiso 1 1 calc R . . H2B H 0.8913 0.9598 0.4091 0.050 Uiso 1 1 calc R . . C3 C 0.8060(7) 0.8705(5) 0.2677(5) 0.0404(15) Uani 1 1 d . . . H3A H 0.7647 0.7978 0.2535 0.048 Uiso 1 1 calc R . . H3B H 0.9218 0.8786 0.2431 0.048 Uiso 1 1 calc R . . C4 C 0.6739(8) 0.9493(4) 0.2097(5) 0.0365(13) Uani 1 1 d . . . H4A H 0.7322 1.0156 0.1947 0.044 Uiso 1 1 calc R . . H4B H 0.6129 0.9207 0.1391 0.044 Uiso 1 1 calc R . . O5 O 0.2506(5) 0.8945(2) 0.1521(3) 0.0326(8) Uani 1 1 d . . . C5 C 0.1614(8) 0.8930(4) 0.0372(4) 0.0398(13) Uani 1 1 d . . . H5A H 0.2123 0.9460 -0.0078 0.048 Uiso 1 1 calc R . . H5B H 0.0350 0.9077 0.0345 0.048 Uiso 1 1 calc R . . C6 C 0.1886(10) 0.7866(5) -0.0045(5) 0.0549(18) Uani 1 1 d . . . H6A H 0.2985 0.7829 -0.0372 0.066 Uiso 1 1 calc R . . H6B H 0.0897 0.7656 -0.0612 0.066 Uiso 1 1 calc R . . C7 C 0.1987(9) 0.7179(4) 0.0960(6) 0.0486(16) Uani 1 1 d . . . H7A H 0.2676 0.6540 0.0871 0.058 Uiso 1 1 calc R . . H7B H 0.0804 0.6974 0.1102 0.058 Uiso 1 1 calc R . . C8 C 0.2888(8) 0.7853(4) 0.1882(5) 0.0382(13) Uani 1 1 d . . . H8A H 0.2426 0.7708 0.2582 0.046 Uiso 1 1 calc R . . H8B H 0.4165 0.7723 0.1999 0.046 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 0.02689(15) 0.02489(13) 0.02347(14) 0.00065(8) 0.00392(10) 0.00036(7) O1 0.033(2) 0.0379(19) 0.039(2) 0.0044(18) 0.0012(18) 0.0079(16) O2 0.045(2) 0.0316(18) 0.037(2) -0.0059(16) 0.0055(19) -0.0040(16) O3 0.029(2) 0.0321(17) 0.0238(18) 0.0049(15) 0.0067(16) -0.0019(14) Cl1 0.0498(9) 0.0364(7) 0.0309(7) 0.0081(6) 0.0093(6) -0.0053(6) O4 0.025(2) 0.043(2) 0.024(2) 0.0034(15) 0.0051(16) 0.0019(14) C1 0.037(3) 0.047(3) 0.024(3) 0.004(2) 0.000(2) 0.008(2) C2 0.029(3) 0.046(3) 0.046(4) -0.001(3) -0.003(3) 0.003(3) C3 0.026(3) 0.041(3) 0.056(4) -0.009(3) 0.016(3) 0.000(2) C4 0.034(3) 0.046(3) 0.031(3) 0.002(2) 0.009(3) -0.002(2) O5 0.041(2) 0.0264(17) 0.0281(19) 0.0019(15) -0.0037(17) 0.0026(15) C5 0.057(4) 0.038(3) 0.023(3) 0.000(2) -0.001(3) 0.003(3) C6 0.081(5) 0.044(3) 0.041(4) -0.015(3) 0.011(4) -0.016(3) C7 0.056(4) 0.036(3) 0.051(4) -0.008(3) -0.001(3) -0.009(3) C8 0.049(4) 0.023(2) 0.039(3) -0.001(2) -0.006(3) 0.006(2) _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 O2 1.708(4) . ? Re1 O1 1.711(4) . ? Re1 O3 1.719(3) . ? Re1 O5 2.262(3) . ? Re1 O4 2.264(4) . ? Re1 Cl1 2.4269(13) . ? O4 C1 1.461(7) . ? O4 C4 1.463(6) . ? C1 C2 1.504(7) . ? C2 C3 1.520(8) . ? C3 C4 1.532(8) . ? O5 C5 1.469(6) . ? O5 C8 1.482(6) . ? C5 C6 1.480(8) . ? C6 C7 1.501(9) . ? C7 C8 1.505(7) . ? 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 O2 Re1 O1 103.66(18) . . ? O2 Re1 O3 102.17(18) . . ? O1 Re1 O3 103.68(18) . . ? O2 Re1 O5 165.49(16) . . ? O1 Re1 O5 88.91(16) . . ? O3 Re1 O5 81.44(15) . . ? O2 Re1 O4 89.78(16) . . ? O1 Re1 O4 164.00(16) . . ? O3 Re1 O4 81.46(15) . . ? O5 Re1 O4 76.77(13) . . ? O2 Re1 Cl1 92.15(13) . . ? O1 Re1 Cl1 91.23(13) . . ? O3 Re1 Cl1 156.04(12) . . ? O5 Re1 Cl1 80.19(9) . . ? O4 Re1 Cl1 79.47(9) . . ? C1 O4 C4 110.2(4) . . ? C1 O4 Re1 118.7(3) . . ? C4 O4 Re1 131.1(3) . . ? O4 C1 C2 105.8(4) . . ? C1 C2 C3 102.4(5) . . ? C2 C3 C4 103.0(4) . . ? O4 C4 C3 103.5(4) . . ? C5 O5 C8 108.5(4) . . ? C5 O5 Re1 126.6(3) . . ? C8 O5 Re1 123.9(3) . . ? O5 C5 C6 105.7(5) . . ? C5 C6 C7 104.5(5) . . ? C6 C7 C8 103.8(5) . . ? O5 C8 C7 105.5(4) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 28.33 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 1.008 _refine_diff_density_min -1.284 _refine_diff_density_rms 0.168 # Attachment 'f75yface.cif' data_f75yface _database_code_depnum_ccdc_archive 'CCDC 626969' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H8 Cl4 O2 Re' _chemical_formula_weight 416.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 I2/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x, -y+1/2, z+1/2' _cell_length_a 15.220(4) _cell_length_b 7.996(2) _cell_length_c 16.717(7) _cell_angle_alpha 90.00 _cell_angle_beta 91.089(3) _cell_angle_gamma 90.00 _cell_volume 2034.0(11) _cell_formula_units_Z 8 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.718 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1528 _exptl_absorpt_coefficient_mu 12.951 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.156 _exptl_absorpt_correction_T_max 0.675 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 6260 _diffrn_reflns_av_R_equivalents 0.1150 _diffrn_reflns_av_sigmaI/netI 0.0758 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.44 _diffrn_reflns_theta_max 25.35 _reflns_number_total 1850 _reflns_number_gt 1518 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0300P)^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 0.00043(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1850 _refine_ls_number_parameters 101 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0455 _refine_ls_R_factor_gt 0.0361 _refine_ls_wR_factor_ref 0.0789 _refine_ls_wR_factor_gt 0.0752 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re 0.628330(16) 0.18404(3) 0.133601(16) 0.02946(15) Uani 1 1 d . . . Cl1 Cl 0.63491(11) 0.4716(2) 0.13684(12) 0.0433(5) Uani 1 1 d . . . Cl2 Cl 0.59924(14) 0.1869(2) 0.26829(11) 0.0433(5) Uani 1 1 d . . . Cl3 Cl 0.58389(12) -0.0911(2) 0.12725(13) 0.0452(5) Uani 1 1 d . . . Cl4 Cl 0.62215(14) 0.1977(2) -0.00396(12) 0.0480(5) Uani 1 1 d . . . O1 O 0.7353(3) 0.1447(7) 0.1420(4) 0.0499(14) Uani 1 1 d . . . O2 O 0.4846(3) 0.2321(6) 0.1230(3) 0.0302(10) Uani 1 1 d . . . C1 C 0.4412(5) 0.3580(10) 0.0703(5) 0.0422(18) Uani 1 1 d . . . H1A H 0.4554 0.4727 0.0888 0.051 Uiso 1 1 calc R . . H1B H 0.4608 0.3454 0.0145 0.051 Uiso 1 1 calc R . . C2 C 0.3461(6) 0.3258(11) 0.0755(6) 0.057(3) Uani 1 1 d . . . H2A H 0.3260 0.2493 0.0323 0.069 Uiso 1 1 calc R . . H2B H 0.3124 0.4314 0.0713 0.069 Uiso 1 1 calc R . . C3 C 0.3347(5) 0.2461(12) 0.1566(5) 0.052(2) Uani 1 1 d . . . H3A H 0.3329 0.3315 0.1994 0.062 Uiso 1 1 calc R . . H3B H 0.2805 0.1778 0.1580 0.062 Uiso 1 1 calc R . . C4 C 0.4154(5) 0.1391(10) 0.1644(5) 0.0441(19) Uani 1 1 d . . . H4A H 0.4317 0.1220 0.2215 0.053 Uiso 1 1 calc R . . H4B H 0.4054 0.0286 0.1391 0.053 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 0.0257(2) 0.0282(2) 0.0344(2) -0.00417(12) -0.00030(12) 0.00015(11) Cl1 0.0396(11) 0.0306(10) 0.0600(12) -0.0026(8) 0.0099(9) -0.0089(7) Cl2 0.0547(13) 0.0434(11) 0.0315(10) 0.0003(8) -0.0055(8) 0.0014(8) Cl3 0.0437(12) 0.0263(9) 0.0654(13) -0.0085(9) -0.0034(9) 0.0021(7) Cl4 0.0472(13) 0.0647(14) 0.0324(10) -0.0074(9) 0.0075(8) 0.0089(9) O1 0.034(3) 0.052(3) 0.064(4) -0.011(3) -0.001(3) 0.005(2) O2 0.026(3) 0.033(2) 0.032(3) 0.005(2) 0.0036(19) -0.001(2) C1 0.032(4) 0.046(4) 0.048(5) 0.014(4) 0.004(3) 0.007(3) C2 0.030(5) 0.080(7) 0.062(6) 0.004(5) -0.006(4) 0.018(4) C3 0.038(5) 0.058(5) 0.061(6) -0.009(5) 0.004(4) -0.004(4) C4 0.034(5) 0.048(4) 0.050(5) 0.007(4) -0.003(4) -0.010(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re1 O1 1.662(5) . ? Re1 O2 2.224(4) . ? Re1 Cl1 2.302(2) . ? Re1 Cl4 2.302(2) . ? Re1 Cl2 2.303(2) . ? Re1 Cl3 2.3034(18) . ? O2 C4 1.474(9) . ? O2 C1 1.484(8) . ? C1 C2 1.475(11) . ? C2 C3 1.511(13) . ? C3 C4 1.500(11) . ? 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 O1 Re1 O2 179.0(2) . . ? O1 Re1 Cl1 98.34(19) . . ? O2 Re1 Cl1 82.62(13) . . ? O1 Re1 Cl4 96.6(2) . . ? O2 Re1 Cl4 83.72(13) . . ? Cl1 Re1 Cl4 88.69(7) . . ? O1 Re1 Cl2 97.2(2) . . ? O2 Re1 Cl2 82.50(13) . . ? Cl1 Re1 Cl2 88.64(7) . . ? Cl4 Re1 Cl2 166.19(8) . . ? O1 Re1 Cl3 96.28(19) . . ? O2 Re1 Cl3 82.76(13) . . ? Cl1 Re1 Cl3 165.38(6) . . ? Cl4 Re1 Cl3 89.59(7) . . ? Cl2 Re1 Cl3 89.58(7) . . ? C4 O2 C1 107.9(5) . . ? C4 O2 Re1 125.9(4) . . ? C1 O2 Re1 126.2(4) . . ? C2 C1 O2 105.9(6) . . ? C1 C2 C3 104.8(6) . . ? C4 C3 C2 102.2(7) . . ? O2 C4 C3 105.2(6) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.518 _refine_diff_density_min -2.130 _refine_diff_density_rms 0.242 # Attachment 'f95a81f_face.cif' data_f95a81f_face _database_code_depnum_ccdc_archive 'CCDC 626970' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H16 Cl6 O5 Re2' _chemical_formula_weight 777.31 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.285(2) _cell_length_b 9.252(3) _cell_length_c 12.070(3) _cell_angle_alpha 91.525(4) _cell_angle_beta 90.116(4) _cell_angle_gamma 92.490(4) _cell_volume 924.0(4) _cell_formula_units_Z 2 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.794 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 712 _exptl_absorpt_coefficient_mu 13.967 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.125 _exptl_absorpt_correction_T_max 0.346 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 6759 _diffrn_reflns_av_R_equivalents 0.0754 _diffrn_reflns_av_sigmaI/netI 0.0788 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 25.36 _reflns_number_total 3341 _reflns_number_gt 2434 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0388P)^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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3341 _refine_ls_number_parameters 190 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0574 _refine_ls_R_factor_gt 0.0364 _refine_ls_wR_factor_ref 0.0862 _refine_ls_wR_factor_gt 0.0803 _refine_ls_goodness_of_fit_ref 0.945 _refine_ls_restrained_S_all 0.945 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re 0.34889(4) 0.63406(4) 0.31263(3) 0.02724(13) Uani 1 1 d . . . Re2 Re 0.15990(4) 0.32808(4) 0.15047(3) 0.02962(14) Uani 1 1 d . . . O1 O 0.2330(7) 0.4875(7) 0.2348(4) 0.0314(16) Uani 1 1 d . . . O2 O 0.5323(8) 0.5685(9) 0.3000(6) 0.049(2) Uani 1 1 d . . . Cl1 Cl 0.2739(3) 0.5330(3) 0.4803(2) 0.0423(7) Uani 1 1 d . . . Cl2 Cl 0.4280(3) 0.8411(3) 0.4149(2) 0.0414(7) Uani 1 1 d . . . Cl3 Cl 0.3576(4) 0.7818(4) 0.1613(2) 0.0585(8) Uani 1 1 d . . . O4 O -0.0260(8) 0.3758(9) 0.1237(6) 0.054(2) Uani 1 1 d . . . Cl4 Cl 0.0946(3) 0.1981(3) 0.3080(2) 0.0447(7) Uani 1 1 d . . . Cl5 Cl 0.1432(4) 0.1108(3) 0.0524(2) 0.0502(8) Uani 1 1 d . . . Cl6 Cl 0.2864(4) 0.4223(3) -0.0038(2) 0.0499(7) Uani 1 1 d . . . O3 O 0.1003(7) 0.7208(8) 0.3258(5) 0.0323(17) Uani 1 1 d . . . C1 C -0.0243(14) 0.7013(17) 0.2401(9) 0.063(4) Uani 1 1 d . . . H1A H -0.0770 0.6034 0.2431 0.076 Uiso 1 1 calc R . . H1B H 0.0232 0.7140 0.1657 0.076 Uiso 1 1 calc R . . C2 C -0.1420(14) 0.8128(15) 0.2639(9) 0.053(3) Uani 1 1 d . . . H2A H -0.2520 0.7793 0.2400 0.063 Uiso 1 1 calc R . . H2B H -0.1118 0.9039 0.2263 0.063 Uiso 1 1 calc R . . C3 C -0.1325(12) 0.8334(12) 0.3888(8) 0.038(3) Uani 1 1 d . . . H3A H -0.1609 0.9326 0.4117 0.046 Uiso 1 1 calc R . . H3B H -0.2062 0.7630 0.4259 0.046 Uiso 1 1 calc R . . C4 C 0.0378(13) 0.8082(16) 0.4158(9) 0.056(4) Uani 1 1 d . . . H4A H 0.1007 0.9014 0.4232 0.067 Uiso 1 1 calc R . . H4B H 0.0449 0.7570 0.4865 0.067 Uiso 1 1 calc R . . O5 O 0.4101(7) 0.2577(7) 0.1899(5) 0.0292(16) Uani 1 1 d . . . C5 C 0.4727(11) 0.2197(12) 0.2997(7) 0.034(2) Uani 1 1 d . . . H5A H 0.4549 0.2981 0.3552 0.040 Uiso 1 1 calc R . . H5B H 0.4187 0.1291 0.3253 0.040 Uiso 1 1 calc R . . C6 C 0.6472(12) 0.2008(13) 0.2828(8) 0.041(3) Uani 1 1 d . . . H6A H 0.6910 0.1366 0.3387 0.049 Uiso 1 1 calc R . . H6B H 0.7087 0.2950 0.2862 0.049 Uiso 1 1 calc R . . C7 C 0.6522(12) 0.1317(12) 0.1672(8) 0.039(3) Uani 1 1 d . . . H7A H 0.7607 0.1451 0.1337 0.047 Uiso 1 1 calc R . . H7B H 0.6219 0.0271 0.1684 0.047 Uiso 1 1 calc R . . C8 C 0.5299(13) 0.2127(14) 0.1065(8) 0.042(3) Uani 1 1 d . . . H8A H 0.5815 0.2984 0.0715 0.050 Uiso 1 1 calc R . . H8B H 0.4771 0.1500 0.0481 0.050 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 0.0258(2) 0.0305(3) 0.0256(2) 0.00212(18) -0.00236(15) 0.00295(16) Re2 0.0262(2) 0.0314(3) 0.0311(2) 0.00078(19) -0.00764(16) 0.00099(17) O1 0.043(4) 0.035(4) 0.017(3) 0.006(3) -0.005(3) 0.010(3) O2 0.028(4) 0.073(6) 0.047(4) 0.010(4) -0.004(3) 0.007(4) Cl1 0.0508(17) 0.0440(18) 0.0325(13) 0.0080(12) -0.0035(11) 0.0016(13) Cl2 0.0437(16) 0.0393(16) 0.0400(14) -0.0036(12) -0.0097(12) -0.0077(12) Cl3 0.077(2) 0.055(2) 0.0427(16) 0.0105(15) 0.0034(14) -0.0059(16) O4 0.033(4) 0.072(6) 0.057(5) 0.000(4) -0.018(4) 0.003(4) Cl4 0.0365(15) 0.0525(19) 0.0450(15) 0.0087(14) 0.0087(11) -0.0036(12) Cl5 0.0581(19) 0.0413(18) 0.0497(16) -0.0119(14) -0.0138(13) -0.0073(13) Cl6 0.064(2) 0.0492(19) 0.0364(14) 0.0079(13) -0.0075(13) -0.0011(14) O3 0.025(4) 0.050(5) 0.022(3) -0.011(3) -0.005(3) 0.011(3) C1 0.051(8) 0.105(12) 0.036(6) -0.024(7) -0.026(6) 0.041(7) C2 0.046(7) 0.070(10) 0.043(7) -0.002(6) -0.012(5) 0.015(6) C3 0.036(6) 0.035(7) 0.044(6) -0.005(5) 0.007(5) 0.013(5) C4 0.040(7) 0.092(11) 0.036(6) -0.020(7) -0.001(5) 0.017(7) O5 0.029(4) 0.040(4) 0.019(3) 0.001(3) 0.003(3) 0.008(3) C5 0.035(6) 0.041(7) 0.026(5) 0.012(5) -0.006(4) 0.005(5) C6 0.033(6) 0.052(8) 0.039(6) -0.004(6) -0.006(5) 0.011(5) C7 0.032(6) 0.035(7) 0.051(7) -0.012(5) 0.001(5) 0.008(5) C8 0.047(7) 0.059(8) 0.021(5) 0.000(5) 0.005(5) 0.015(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 O2 1.667(7) . ? Re1 O1 1.860(6) . ? Re1 O3 2.247(6) . ? Re1 Cl3 2.309(3) . ? Re1 Cl2 2.320(3) . ? Re1 Cl1 2.326(3) . ? Re2 O4 1.654(7) . ? Re2 O1 1.849(7) . ? Re2 O5 2.253(6) . ? Re2 Cl5 2.304(3) . ? Re2 Cl6 2.311(3) . ? Re2 Cl4 2.328(3) . ? O3 C4 1.447(13) . ? O3 C1 1.462(11) . ? C1 C2 1.473(16) . ? C2 C3 1.516(14) . ? C3 C4 1.478(13) . ? O5 C8 1.479(11) . ? O5 C5 1.479(10) . ? C5 C6 1.478(13) . ? C6 C7 1.521(13) . ? C7 C8 1.489(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Re1 O1 98.3(3) . . ? O2 Re1 O3 178.7(3) . . ? O1 Re1 O3 80.7(3) . . ? O2 Re1 Cl3 98.2(3) . . ? O1 Re1 Cl3 92.41(19) . . ? O3 Re1 Cl3 81.09(19) . . ? O2 Re1 Cl2 96.5(3) . . ? O1 Re1 Cl2 165.2(2) . . ? O3 Re1 Cl2 84.48(18) . . ? Cl3 Re1 Cl2 85.54(11) . . ? O2 Re1 Cl1 99.2(3) . . ? O1 Re1 Cl1 90.79(19) . . ? O3 Re1 Cl1 81.66(18) . . ? Cl3 Re1 Cl1 161.70(12) . . ? Cl2 Re1 Cl1 86.77(10) . . ? O4 Re2 O1 99.8(3) . . ? O4 Re2 O5 178.3(3) . . ? O1 Re2 O5 80.9(2) . . ? O4 Re2 Cl5 96.5(3) . . ? O1 Re2 Cl5 163.7(2) . . ? O5 Re2 Cl5 82.85(18) . . ? O4 Re2 Cl6 98.5(3) . . ? O1 Re2 Cl6 90.2(2) . . ? O5 Re2 Cl6 82.99(17) . . ? Cl5 Re2 Cl6 86.43(11) . . ? O4 Re2 Cl4 96.1(3) . . ? O1 Re2 Cl4 91.91(19) . . ? O5 Re2 Cl4 82.34(17) . . ? Cl5 Re2 Cl4 87.32(11) . . ? Cl6 Re2 Cl4 164.67(11) . . ? Re2 O1 Re1 168.0(4) . . ? C4 O3 C1 108.6(7) . . ? C4 O3 Re1 127.0(5) . . ? C1 O3 Re1 124.4(6) . . ? O3 C1 C2 106.0(9) . . ? C1 C2 C3 103.4(8) . . ? C4 C3 C2 104.2(8) . . ? O3 C4 C3 106.9(8) . . ? C8 O5 C5 107.1(7) . . ? C8 O5 Re2 124.9(5) . . ? C5 O5 Re2 126.9(5) . . ? C6 C5 O5 105.1(7) . . ? C5 C6 C7 102.6(7) . . ? C8 C7 C6 102.3(8) . . ? O5 C8 C7 106.4(8) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.36 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.728 _refine_diff_density_min -1.855 _refine_diff_density_rms 0.234