# Copyright The Royal Society of Chemistry, 1998 # Paper 8/03301C data_[ReO3(Hpin)].H2pin _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety '[ReO3(C6H13O2)].C6H14O2' _chemical_formula_sum 'C12 H27 O7 Re' _chemical_formula_weight 469.54 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' '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 'P 1 21/c 1' 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 12.184(8) _cell_length_b 11.217(7) _cell_length_c 13.864(9) _cell_angle_alpha 90.00 _cell_angle_beta 111.34(5) _cell_angle_gamma 90.00 _cell_volume 1765(2) _cell_formula_units_Z 4 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 18.4 _cell_measurement_theta_max 20.5 _exptl_crystal_description cube _exptl_crystal_colour colourless _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.767 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 920 _exptl_absorpt_coefficient_mu 6.909 _exptl_absorpt_correction_type ; empirical via \y scans (North, Phillips & Mathews, 1968) ; _exptl_absorpt_correction_T_min 0.2023 _exptl_absorpt_correction_T_max 0.4911 _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC5S' _diffrn_measurement_method '\w--2\q' _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% -6.8% _diffrn_reflns_number 3276 _diffrn_reflns_av_R_equivalents 0.0425 _diffrn_reflns_av_sigmaI/netI 0.0892 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 25.05 _reflns_number_total 3122 _reflns_number_gt 1906 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; MSC/AFC Control Program (Molecular Structure Corporation, 1995) ; _computing_cell_refinement ; MSC/AFC5S Control Program (Molecular Structure Corporation, 1995) ; _computing_data_reduction ; TEXSAN (Molecular Structure Corporation, 1989) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 for WINDOWS (Farrugia, 1997)' _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 w=1/[\s^2^(Fo^2^)+(0.0298P)^2^+4.2000P] 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 3122 _refine_ls_number_parameters 190 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1111 _refine_ls_R_factor_gt 0.0432 _refine_ls_wR_factor_ref 0.0969 _refine_ls_wR_factor_gt 0.0807 _refine_ls_goodness_of_fit_ref 0.992 _refine_ls_restrained_S_all 0.995 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re Re 0.69327(4) 0.06236(4) 0.67854(3) 0.05711(16) Uani 1 d . . . O1 O 0.7429(7) -0.0354(7) 0.6108(6) 0.087(3) Uani 1 d . . . O2 O 0.8055(7) 0.1149(8) 0.7828(5) 0.082(2) Uani 1 d . . . O3 O 0.6132(7) -0.0248(7) 0.7303(6) 0.089(3) Uani 1 d . . . O4 O 0.7615(6) 0.2054(7) 0.5982(5) 0.057(2) Uani 1 d . . . H1 H 0.804(10) 0.194(12) 0.577(9) 0.086 Uiso 1 d . . . O5 O 0.5658(6) 0.1593(6) 0.6046(5) 0.0628(19) Uani 1 d . . . O6 O 0.9473(6) 0.1631(7) 0.5552(6) 0.071(2) Uani 1 d D . . H2 H 0.927(11) 0.104(11) 0.524(9) 0.107 Uiso 1 d . . . O7 O 1.1339(6) 0.0590(8) 0.5322(7) 0.089(3) Uani 1 d D . . H3 H 1.178(11) 0.056(14) 0.505(10) 0.133 Uiso 1 d D . . C1 C 0.6395(10) 0.1827(11) 0.4174(7) 0.077(3) Uani 1 d . . . H1A H 0.6104 0.1079 0.4320 0.115 Uiso 1 calc R . . H1B H 0.7086 0.1692 0.4011 0.115 Uiso 1 calc R . . H1C H 0.5800 0.2202 0.3597 0.115 Uiso 1 calc R . . C2 C 0.6709(9) 0.2645(9) 0.5133(7) 0.059(3) Uani 1 d . . . C3 C 0.5702(9) 0.2739(9) 0.5576(8) 0.057(3) Uani 1 d . . . C4 C 0.5960(11) 0.3686(9) 0.6400(8) 0.076(3) Uani 1 d . . . H4A H 0.6720 0.3544 0.6924 0.113 Uiso 1 calc R . . H4B H 0.5368 0.3664 0.6705 0.113 Uiso 1 calc R . . H4C H 0.5955 0.4455 0.6094 0.113 Uiso 1 calc R . . C5 C 0.7170(10) 0.3831(9) 0.4923(8) 0.075(3) Uani 1 d . . . H5A H 0.7358 0.4330 0.5524 0.113 Uiso 1 calc R . . H5B H 0.6578 0.4212 0.4346 0.113 Uiso 1 calc R . . H5C H 0.7865 0.3704 0.4764 0.113 Uiso 1 calc R . . C6 C 0.4490(9) 0.2928(11) 0.4714(9) 0.086(4) Uani 1 d . . . H6A H 0.4357 0.2315 0.4200 0.129 Uiso 1 calc R . . H6B H 0.4471 0.3693 0.4399 0.129 Uiso 1 calc R . . H6C H 0.3886 0.2892 0.5005 0.129 Uiso 1 calc R . . C7 C 1.0900(12) 0.0609(12) 0.7136(9) 0.096(4) Uani 1 d . . . H7A H 1.0338 0.0597 0.7474 0.144 Uiso 1 calc R . . H7B H 1.1681 0.0670 0.7646 0.144 Uiso 1 calc R . . H7C H 1.0833 -0.0112 0.6746 0.144 Uiso 1 calc R . . C8 C 1.0645(9) 0.1735(14) 0.6369(9) 0.105(5) Uani 1 d D . . C9 C 1.1534(8) 0.1721(10) 0.5877(9) 0.094(4) Uani 1 d D . . C10 C 1.1242(12) 0.2811(11) 0.5099(10) 0.105(5) Uani 1 d D . . H10A H 1.1798 0.2831 0.4755 0.158 Uiso 1 calc R . . H10B H 1.1293 0.3540 0.5476 0.158 Uiso 1 calc R . . H10C H 1.0460 0.2723 0.4596 0.158 Uiso 1 calc R . . C11 C 1.0583(12) 0.2914(13) 0.6912(11) 0.120(6) Uani 1 d . . . H11A H 0.9981 0.2860 0.7204 0.180 Uiso 1 calc R . . H11B H 1.0401 0.3553 0.6418 0.180 Uiso 1 calc R . . H11C H 1.1329 0.3064 0.7453 0.180 Uiso 1 calc R . . C12 C 1.2808(8) 0.1720(11) 0.6633(8) 0.082(4) Uani 1 d D . . H12A H 1.3328 0.1684 0.6254 0.124 Uiso 1 calc R . . H12B H 1.2940 0.1039 0.7081 0.124 Uiso 1 calc R . . H12C H 1.2960 0.2435 0.7041 0.124 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re 0.0713(3) 0.0511(2) 0.0526(2) 0.0096(3) 0.02686(19) 0.0123(3) O1 0.114(6) 0.067(6) 0.080(5) 0.001(4) 0.034(5) 0.018(5) O2 0.090(6) 0.104(6) 0.053(4) 0.009(4) 0.028(4) -0.009(5) O3 0.116(7) 0.072(6) 0.087(6) 0.041(4) 0.047(5) 0.000(5) O4 0.060(5) 0.066(5) 0.051(4) 0.000(4) 0.026(3) 0.007(4) O5 0.066(4) 0.051(4) 0.080(5) 0.013(4) 0.036(4) 0.010(3) O6 0.054(4) 0.082(6) 0.078(5) -0.047(4) 0.026(4) -0.014(4) O7 0.065(5) 0.089(6) 0.126(7) -0.067(6) 0.050(5) -0.018(5) C1 0.085(8) 0.087(8) 0.051(6) -0.006(6) 0.017(6) 0.015(7) C2 0.071(7) 0.056(7) 0.049(6) 0.006(5) 0.021(5) 0.021(6) C3 0.061(7) 0.054(7) 0.060(6) 0.021(5) 0.027(6) 0.018(5) C4 0.110(10) 0.053(7) 0.082(8) 0.013(6) 0.057(7) 0.018(7) C5 0.107(9) 0.060(7) 0.074(8) 0.013(6) 0.052(7) 0.000(7) C6 0.069(8) 0.089(9) 0.101(9) 0.039(8) 0.032(7) 0.025(7) C7 0.128(11) 0.092(9) 0.073(8) 0.021(8) 0.041(8) -0.010(9) C8 0.068(9) 0.143(13) 0.105(10) -0.082(11) 0.032(8) -0.039(9) C9 0.056(8) 0.113(11) 0.105(10) -0.058(10) 0.022(7) -0.017(8) C10 0.137(13) 0.088(10) 0.106(10) 0.024(9) 0.063(10) 0.002(9) C11 0.106(10) 0.139(13) 0.133(12) -0.105(11) 0.064(9) -0.045(10) C12 0.054(7) 0.090(9) 0.091(8) -0.017(7) 0.012(6) -0.017(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re O1 1.692(8) . y Re O2 1.694(7) . y Re O3 1.713(7) . y Re O5 1.866(6) . y Re O4 2.277(8) . y O4 C2 1.447(11) . y O4 H1 0.70(11) . y O5 C3 1.451(11) . y O6 C8 1.469(10) . y O6 H2 0.78(12) . y O7 C9 1.458(10) . y O7 H3 0.77(8) . y C1 C2 1.544(13) . y C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C5 1.513(14) . y C2 C3 1.563(14) . y C3 C4 1.507(13) . y C3 C6 1.540(13) . y C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 C8 1.606(18) . y C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 C9 1.476(11) . y C8 C11 1.537(16) . y C9 C12 1.525(10) . y C9 C10 1.583(11) . y C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? 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 Re O2 111.0(4) . . y O1 Re O3 103.7(4) . . y O2 Re O3 104.3(4) . . y O1 Re O5 117.8(3) . . y O2 Re O5 121.2(4) . . y O3 Re O5 94.3(3) . . y O1 Re O4 85.2(3) . . y O2 Re O4 81.2(3) . . y O3 Re O4 166.6(3) . . y O5 Re O4 72.5(3) . . y C2 O4 Re 114.5(6) . . y C2 O4 H1 102(10) . . y Re O4 H1 122(10) . . y C3 O5 Re 127.1(6) . . y C8 O6 H2 121(10) . . y C9 O7 H3 107(10) . . y C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O4 C2 C5 109.4(9) . . y O4 C2 C1 107.7(8) . . y C5 C2 C1 110.5(9) . . y O4 C2 C3 100.8(7) . . y C5 C2 C3 114.6(8) . . y C1 C2 C3 113.2(9) . . y O5 C3 C4 108.4(8) . . y O5 C3 C6 106.8(8) . . y C4 C3 C6 111.6(9) . . y O5 C3 C2 106.2(7) . . y C4 C3 C2 111.6(9) . . y C6 C3 C2 111.9(8) . . y C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C2 C5 H5A 109.5 . . ? C2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C3 C6 H6A 109.5 . . ? C3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 H7A 109.5 . . ? C8 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C8 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O6 C8 C9 108.3(9) . . y O6 C8 C11 103.8(10) . . y C9 C8 C11 114.2(11) . . y O6 C8 C7 110.4(10) . . y C9 C8 C7 107.4(11) . . y C11 C8 C7 112.6(10) . . y O7 C9 C8 104.3(9) . . y O7 C9 C12 107.0(9) . . y C8 C9 C12 114.7(9) . . y O7 C9 C10 111.0(9) . . y C8 C9 C10 106.6(11) . . y C12 C9 C10 112.9(10) . . y C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Re O4 C2 102.8(6) . . . . ? O2 Re O4 C2 -145.1(7) . . . . ? O3 Re O4 C2 -29.6(17) . . . . ? O5 Re O4 C2 -18.4(6) . . . . ? O1 Re O5 C3 -87.1(8) . . . . ? O2 Re O5 C3 55.4(8) . . . . ? O3 Re O5 C3 165.0(8) . . . . ? O4 Re O5 C3 -12.4(7) . . . . ? Re O4 C2 C5 159.4(6) . . . . ? Re O4 C2 C1 -80.4(9) . . . . ? Re O4 C2 C3 38.4(8) . . . . ? Re O5 C3 C4 -82.6(9) . . . . ? Re O5 C3 C6 157.1(7) . . . . ? Re O5 C3 C2 37.6(10) . . . . ? O4 C2 C3 O5 -43.8(10) . . . . y C5 C2 C3 O5 -161.2(8) . . . . ? C1 C2 C3 O5 71.0(10) . . . . ? O4 C2 C3 C4 74.2(9) . . . . ? C5 C2 C3 C4 -43.1(11) . . . . ? C1 C2 C3 C4 -171.0(8) . . . . ? O4 C2 C3 C6 -160.0(8) . . . . ? C5 C2 C3 C6 82.7(11) . . . . ? C1 C2 C3 C6 -45.2(12) . . . . ? O6 C8 C9 O7 -58.6(13) . . . . y C11 C8 C9 O7 -173.7(11) . . . . ? C7 C8 C9 O7 60.6(10) . . . . ? O6 C8 C9 C12 -175.2(10) . . . . ? C11 C8 C9 C12 69.7(16) . . . . ? C7 C8 C9 C12 -56.0(13) . . . . ? O6 C8 C9 C10 59.0(13) . . . . ? C11 C8 C9 C10 -56.1(13) . . . . ? C7 C8 C9 C10 178.2(9) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O4 H1 O6 0.70(11) 1.90(11) 2.585(10) 165(13) . O6 H2 O7 0.78(12) 2.03(12) 2.790(11) 169(14) 3_756 O7 H3 O1 0.77(8) 2.16(9) 2.901(11) 163(15) 3_756 _refine_diff_density_max 1.015 _refine_diff_density_min -0.933 _refine_diff_density_rms 0.141 #===END data_[ReO(pin)2] _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety '[ReO(C6H12O2)]' _chemical_formula_sum 'C12 H24 O5 Re' _chemical_formula_weight 434.51 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Re' 'Re' -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P42nm' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, x, z' '-y, -x, z' 'x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' _cell_length_a 10.315(2) _cell_length_b 10.315(2) _cell_length_c 7.2700(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 773.5(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 20.9 _cell_measurement_theta_max 21.7 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max .38 _exptl_crystal_size_mid .32 _exptl_crystal_size_min .24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.866 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 422 _exptl_absorpt_coefficient_mu 7.864 _exptl_absorpt_correction_type ; empirical via \y scans (North, Phillips & Mathews, 1968) ; _exptl_absorpt_correction_T_min 0.154 _exptl_absorpt_correction_T_max 0.254 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC5S' _diffrn_measurement_method '\w--2\q' _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 743 _diffrn_reflns_av_R_equivalents 0.0263 _diffrn_reflns_av_sigmaI/netI 0.0348 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.79 _diffrn_reflns_theta_max 24.98 _reflns_number_total 403 _reflns_number_gt 295 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; MSC/AFC Control Program (Molecular Structure Corporation, 1995) ; _computing_cell_refinement ; MSC/AFC5S Control Program (Molecular Structure Corporation, 1995) ; _computing_data_reduction ; TEXSAN (Molecular Structure Corporation, 1989) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 for WINDOWS (Farrugia, 1997)' _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 w=1/[\s^2^(Fo^2^)+(0.0288P)^2^+2.2700P] 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 none _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0102(11) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.02(6) _refine_ls_number_reflns 403 _refine_ls_number_parameters 61 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.0525 _refine_ls_R_factor_gt 0.0311 _refine_ls_wR_factor_ref 0.0720 _refine_ls_wR_factor_gt 0.0653 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.062 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re Re 0.5000 0.5000 0.0000 0.0574(4) Uani 1 d SD . . O1 O 0.543(2) 0.543(2) -0.217(2) 0.078(10) Uani 0.50 d SPD . . O2A O 0.5105(18) 0.3246(8) 0.047(2) 0.040(5) Uiso 0.50 d PD . . O2B O 0.509(2) 0.3347(12) 0.116(3) 0.050(5) Uiso 0.50 d PD . . C1A C 0.6399(19) 0.2722(17) 0.079(3) 0.057(9) Uani 0.50 d PD . . C1B C 0.630(2) 0.2922(15) 0.202(3) 0.044(7) Uani 0.50 d PD . . C2A C 0.703(3) 0.253(3) -0.110(4) 0.055(12) Uani 0.50 d PD . . C2B C 0.6414(19) 0.3586(19) 0.390(3) 0.112(11) Uani 1 d SD . . C3 C 0.6266(14) 0.1446(11) 0.182(3) 0.080(5) Uani 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re 0.0668(5) 0.0668(5) 0.0386(5) 0.000 0.000 0.0223(6) O1 0.093(14) 0.093(14) 0.048(17) 0.009(10) 0.009(10) 0.008(15) C1A 0.030(14) 0.052(15) 0.09(3) -0.004(17) -0.010(15) -0.007(11) C1B 0.042(15) 0.050(14) 0.042(14) -0.006(13) -0.019(14) -0.012(11) C2A 0.039(16) 0.09(3) 0.040(12) -0.008(15) 0.018(14) 0.001(19) C2B 0.143(17) 0.143(17) 0.050(14) -0.010(12) 0.010(12) 0.05(2) C3 0.081(11) 0.041(7) 0.119(14) 0.020(11) 0.008(12) -0.005(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re O1 1.699(10) . y Re O2A 1.845(8) 4_665 ? Re O2A 1.845(8) 2_665 ? Re O2A 1.845(8) . y Re O2A 1.845(8) 3 ? Re O2B 1.904(9) 4_665 ? Re O2B 1.904(9) 2_665 ? Re O2B 1.904(9) 3 ? Re O2B 1.904(9) . y O1 O1 1.27(6) 2_665 ? O2A C1A 1.458(10) . y O2B C1B 1.464(10) . y C1A C1B 1.520(11) 4_665 y C1A C3 1.523(14) . y C1A C2A 1.532(15) . y C1B C1A 1.520(11) 4_665 ? C1B C3 1.529(14) . y C1B C2B 1.534(15) . y C2B C1B 1.534(15) 4_665 ? 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 Re O2A 85.9(9) . 4_665 ? O1 Re O2A 85.9(9) . 2_665 ? O2A Re O2A 94.6(11) 4_665 2_665 ? O1 Re O2A 114.6(8) . . y O2A Re O2A 81.4(11) 4_665 . y O2A Re O2A 158.6(11) 2_665 . ? O1 Re O2A 114.6(8) . 3 ? O2A Re O2A 158.6(11) 4_665 3 ? O2A Re O2A 81.4(11) 2_665 3 ? O2A Re O2A 94.6(11) . 3 ? O1 Re O2B 100.7(10) . 4_665 y O2A Re O2B 15.5(6) 4_665 4_665 ? O2A Re O2B 91.1(6) 2_665 4_665 ? O2A Re O2B 79.4(5) . 4_665 y O2A Re O2B 143.1(10) 3 4_665 ? O1 Re O2B 100.7(10) . 2_665 ? O2A Re O2B 91.1(6) 4_665 2_665 ? O2A Re O2B 15.5(6) 2_665 2_665 ? O2A Re O2B 143.1(10) . 2_665 y O2A Re O2B 79.4(5) 3 2_665 ? O2B Re O2B 84.0(13) 4_665 2_665 y O1 Re O2B 129.3(8) . 3 ? O2A Re O2B 143.1(10) 4_665 3 ? O2A Re O2B 79.4(5) 2_665 3 ? O2A Re O2B 91.1(6) . 3 ? O2A Re O2B 15.5(6) 3 3 ? O2B Re O2B 127.6(12) 4_665 3 ? O2B Re O2B 73.5(12) 2_665 3 ? O1 Re O2B 129.3(8) . . ? O2A Re O2B 79.4(5) 4_665 . ? O2A Re O2B 143.1(10) 2_665 . ? O2A Re O2B 15.5(6) . . ? O2A Re O2B 91.1(6) 3 . ? O2B Re O2B 73.5(12) 4_665 . ? O2B Re O2B 127.6(12) 2_665 . ? O2B Re O2B 84.0(13) 3 . ? O1 O1 Re 68.1(11) 2_665 . ? C1A O2A Re 116.5(11) . . y C1B O2B Re 120.1(12) . . y O2A C1A C1B 105.6(16) . 4_665 ? O2A C1A C3 108.4(13) . . ? C1B C1A C3 108.8(16) 4_665 . ? O2A C1A C2A 107.0(17) . . ? C1B C1A C2A 114.8(18) 4_665 . ? C3 C1A C2A 111.9(19) . . ? O2B C1B C1A 99.9(16) . 4_665 ? O2B C1B C3 103.7(12) . . ? C1A C1B C3 114.8(17) 4_665 . ? O2B C1B C2B 108.3(18) . . ? C1A C1B C2B 105.7(13) 4_665 . ? C3 C1B C2B 122.0(17) . . ? C1B C2B C1B 43.4(15) . 4_665 ? C1A C3 C1B 35.3(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2A Re O1 O1 132.5(6) 4_665 . . 2_665 ? O2A Re O1 O1 -132.5(6) 2_665 . . 2_665 ? O2A Re O1 O1 53.9(7) . . . 2_665 ? O2A Re O1 O1 -53.9(7) 3 . . 2_665 ? O2B Re O1 O1 137.1(7) 4_665 . . 2_665 ? O2B Re O1 O1 -137.1(7) 2_665 . . 2_665 ? O2B Re O1 O1 -59.7(11) 3 . . 2_665 ? O2B Re O1 O1 59.7(11) . . . 2_665 ? O1 Re O2A C1A 77.0(19) . . . . ? O2A Re O2A C1A -4.5(19) 4_665 . . . ? O2A Re O2A C1A -85.1(15) 2_665 . . . ? O2A Re O2A C1A -163.3(12) 3 . . . ? O2B Re O2A C1A -20.1(18) 4_665 . . . ? O2B Re O2A C1A -85(2) 2_665 . . . ? O2B Re O2A C1A -148.2(15) 3 . . . ? O2B Re O2A C1A -86(4) . . . . ? O1 Re O2B C1B 85(2) . . . . ? O2A Re O2B C1B 8.8(17) 4_665 . . . ? O2A Re O2B C1B -75(2) 2_665 . . . ? O2A Re O2B C1B 105(5) . . . . ? O2A Re O2B C1B -151.9(15) 3 . . . ? O2B Re O2B C1B -6(2) 4_665 . . . ? O2B Re O2B C1B -74.4(16) 2_665 . . . ? O2B Re O2B C1B -138.1(13) 3 . . . ? Re O2A C1A C1B 42.7(19) . . . 4_665 ? Re O2A C1A C3 159.1(13) . . . . ? Re O2A C1A C2A -80(2) . . . . ? Re O2B C1B C1A -31.5(18) . . . 4_665 ? Re O2B C1B C3 -150.3(15) . . . . ? Re O2B C1B C2B 78.7(17) . . . . ? O2B C1B C2B C1B -108.1(11) . . . 4_665 ? C1A C1B C2B C1B -1.8(17) 4_665 . . 4_665 ? C3 C1B C2B C1B 131.8(14) . . . 4_665 ? O2A C1A C3 C1B -82(2) . . . . ? C1B C1A C3 C1B 32.2(16) 4_665 . . . ? C2A C1A C3 C1B 160(3) . . . . ? O2B C1B C3 C1A 69(2) . . . . ? C1A C1B C3 C1A -38.9(19) 4_665 . . . ? C2B C1B C3 C1A -169(4) . . . . ? O2A C1A C1B O2B -42.1(16) . . 4_665 4_665 y _refine_diff_density_max 0.825 _refine_diff_density_min -0.962 _refine_diff_density_rms 0.100 #===END