Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_etreo3 _database_code_CSD 185060 _audit_creation_date 99-30-10 _audit_creation_method CRYSTALS_ver_12-03-99 _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Downs, A.' 'Geisberger, Martin R.' 'Green, Jennifer C.' 'Greene, T. M.' 'Haarland, Arne' 'Herrmann, Wolfgang' 'Morris, Leigh J.' 'Parsons, Simon' 'Scherer, Wolfgang' 'Volden, Hans Vidar' _publ_contact_author_name 'Prof A Downs' _publ_contact_author_address ; Inorganic Chemistry Laboratory University of Oxford South Parks Road Oxford OX1 3QR UNITED KINGDOM ; _publ_contact_author_email 'TONY.DOWNS@CHEM.OX.AC.UK' _publ_section_title ; Structure and vibrational properties of ethyltrioxorhenium(VII), C2H5ReO3, investigated by gas electron diffraction, single crystal X-ray diffraction, IR spectroscopy and quantum chemical calculations ; _diffrn_measurement_device_type 'Stoe Stadi-4 diffractometer' _diffrn_radiation_monochromator graphite _computing_data_collection 'Stoe DIF4' _computing_data_reduction 'Stoe REDU4' _computing_cell_refinement 'Stoe DIF4' #========================================================================== # General computing #========================================================================== _computing_structure_refinement ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_publication_material ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_molecular_graphics ; CAMERON (Watkin, Prout & Pearce, 1996) ; # choose one of the following two lines _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point 'not measured' _refine_ls_matrix_type full _atom_sites_solution_primary direct _atom_sites_solution_hydrogens geometric _refine_ls_hydrogen_treatment noref _cell_length_a 6.421(3) _cell_angle_alpha 90 _cell_length_b 5.111(2) _cell_angle_beta 98.01(4) _cell_length_c 15.108(5) _cell_angle_gamma 90 _cell_volume 491.0(3) _symmetry_cell_setting 'Monoclinic ' _symmetry_space_group_name_H-M 'P 1 21/n 1 ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' '-x+1/2,y+1/2,-z+1/2' 'x+1/2,-y+1/2,z+1/2' loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International_Tables_Vol_IV_Table_2.2B' 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 'International_Tables_Vol_IV_Table_2.2B' 'O ' 0.0080 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International_Tables_Vol_IV_Table_2.2B' 'Re ' -1.5980 7.2320 28.7621 1.6719 15.7189 9.0923 14.5564 0.3505 5.4417 52.0861 10.4720 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum ' C2 H5 O3 Re1 ' _chemical_formula_moiety EtReO3 _chemical_compound_source ; ? ; _chemical_formula_weight 263.26 _cell_measurement_reflns_used 54 _cell_measurement_theta_min 12 _cell_measurement_theta_max 16 _cell_measurement_temperature 150 _cell_formula_units_Z 4 _exptl_crystal_description ' cylinder ' _exptl_crystal_colour ' colourless ' _exptl_crystal_size_min 0.08 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_max 0.11 _exptl_crystal_density_diffrn 3.56 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 458.43 _exptl_absorpt_coefficient_mu 24.97 _exptl_absorpt_correction_type 'Optimised numerical' _exptl_absorpt_correction_T_min 0.0432 _exptl_absorpt_correction_T_max 0.0939 _diffrn_standards_interval_time 60 _diffrn_standards_interval_count 0 _diffrn_standards_number 3 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 150 _diffrn_reflns_number 5095 _reflns_number_total 1422 _diffrn_reflns_av_R_equivalents 0.0734 # Number of reflections with Friedels Law is 1422 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 1434 _diffrn_measured_fraction_theta_max 0.992 _reflns_number_gt 658 _diffrn_reflns_theta_min 2.72 _diffrn_reflns_theta_max 25.00 # Data collected to 2theta=60, but shell from 50-60 deg # omitted from refinement _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -3 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_limit_l_max 21 _reflns_limit_h_min -9 _reflns_limit_h_max 8 _reflns_limit_k_min 0 _reflns_limit_k_max 7 _reflns_limit_l_min 0 _reflns_limit_l_max 21 _refine_diff_density_min -2.68 _refine_diff_density_max 2.51 _reflns_threshold_expression >2.00\s(I) _refine_ls_number_reflns 658 _refine_ls_number_parameters 56 _refine_ls_R_factor_gt 0.0406 _refine_ls_wR_factor_ref 0.0435 _refine_ls_goodness_of_fit_ref 1.0598 _refine_ls_shift/su_max 0.000127 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 3 parameters, Carruthers & Watkin , 1979, 1.67 -.750 1.27 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method Omega-theta # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type Re1 0.50117(8) 0.18763(13) 0.18711(3) 0.0183 1.0000 Uani C1 0.235(2) 0.316(3) 0.101(1) 0.0233 1.0000 Uani C2 0.239(3) 0.205(4) 0.009(1) 0.0417 1.0000 Uani O1 0.4756(19) 0.308(2) 0.2879(7) 0.0324 1.0000 Uani O2 0.4889(16) -0.145(2) 0.1810(6) 0.0298 1.0000 Uani O3 0.7093(17) 0.314(2) 0.1423(7) 0.0325 1.0000 Uani H11 0.2372 0.5119 0.0982 0.0281 1.0000 Uiso H12 0.1058 0.2571 0.1250 0.0281 1.0000 Uiso H21 0.1111 0.2667 -0.0319 0.0396 1.0000 Uiso H22 0.3680 0.2638 -0.0152 0.0396 1.0000 Uiso H23 0.2365 0.0090 0.0115 0.0396 1.0000 Uiso 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 0.0229(4) 0.0213(4) 0.0084(4) 0.0002(2) -0.0056(2) -0.0001(3) C1 0.022(6) 0.025(7) 0.020(7) 0.004(6) -0.004(5) 0.001(6) C2 0.064(12) 0.051(11) 0.008(7) 0.004(7) -0.002(7) 0.011(9) O1 0.049(6) 0.034(6) 0.011(5) -0.005(4) -0.005(4) -0.015(5) O2 0.033(5) 0.036(9) 0.016(5) -0.009(4) -0.011(4) -0.006(4) O3 0.027(5) 0.041(7) 0.028(6) 0.000(5) -0.001(4) -0.002(5) _refine_ls_extinction_coef 9.5(16) _refine_ls_extinction_method 'Larson 1970 Crystallographic Computing eq 22' loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Re1 . C1 . 2.098(14) yes Re1 . O1 . 1.671(11) yes Re1 . O2 . 1.702(12) yes Re1 . O3 . 1.707(11) yes C1 . C2 . 1.51(2) yes C1 . H11 . 1.003(15) no C1 . H12 . 0.995(14) no C2 . H21 . 1.002(18) no C2 . H22 . 1.00(2) no C2 . H23 . 1.00(2) no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C1 . Re1 . O1 . 105.8(6) yes C1 . Re1 . O2 . 104.5(5) yes O1 . Re1 . O2 . 114.0(6) yes C1 . Re1 . O3 . 104.6(5) yes O1 . Re1 . O3 . 113.8(5) yes O2 . Re1 . O3 . 112.9(5) yes Re1 . C1 . C2 . 109.8(11) yes Re1 . C1 . H11 . 109.1(10) no C2 . C1 . H11 . 109.0(13) no Re1 . C1 . H12 . 109.5(10) no C2 . C1 . H12 . 109.8(14) no H11 . C1 . H12 . 109.6(14) no C1 . C2 . H21 . 109.5(16) no C1 . C2 . H22 . 110.1(17) no H21 . C2 . H22 . 109.5(15) no C1 . C2 . H23 . 109.3(14) no H21 . C2 . H23 . 109.0(19) no H22 . C2 . H23 . 109.4(18) no