# ic970415u.cif # 5. DATA # data_rhen.acta _audit_creation_method SHELXL _chemical_name_systematic ; 2-(2-thienyl)pyridine)-tetracarbonyl-rhenium(I) ; _chemical_name_common ? _chemical_formula_moiety 'C4 O4 Re 1+, C9 H6 N S 1-' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C13 H6 N O4 Re S' _chemical_formula_weight 458.45 _chemical_melting_point ? _chemical_compound_source ; Give summary of chemical and crystal preparation in sufficent detail to reproduce experiment ; loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Re' 'Re' -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 '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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _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 10.64(7) _cell_length_b 11.70(13) _cell_length_c 12.23(6) _cell_angle_alpha 90.00 _cell_angle_beta 110.33(4) _cell_angle_gamma 90.00 _cell_volume 1430(20) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 21 _cell_measurement_theta_min 2.04 _cell_measurement_theta_max 27.97 _exptl_crystal_colour orange _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.5 _exptl_crystal_size_min 0.4 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.132 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 856 _exptl_absorpt_coefficient_mu 8.664 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.6991 _exptl_absorpt_correction_T_max 0.9995 _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 'Enraf-Nonius CAD-4' _diffrn_measurement_method '\w/2\q scans' _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 4265 _diffrn_reflns_av_R_equivalents 0.0280 _diffrn_reflns_av_sigmaI/netI 0.0406 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 27.97 _reflns_number_total 3429 _reflns_number_observed 2489 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'CAD4 Software (Enraf-Nonius, 1989)' _computing_cell_refinement 'CAD4 Software (Enraf-Nonius, 1989)' _computing_data_reduction 'SHELXTL PC^TM^ (Sheldrick, 1990)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 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 w=1/[\s^2^(Fo^2^)+(0.0225P)^2^+1.7346P] 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 SHELXL _refine_ls_extinction_coef 0.0067(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3429 _refine_ls_number_parameters 183 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0600 _refine_ls_R_factor_obs 0.0260 _refine_ls_wR_factor_all 0.0611 _refine_ls_wR_factor_obs 0.0534 _refine_ls_goodness_of_fit_all 1.023 _refine_ls_goodness_of_fit_obs 1.062 _refine_ls_restrained_S_all 1.023 _refine_ls_restrained_S_obs 1.062 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_mean 0.000 _refine_diff_density_max 0.897 _refine_diff_density_min -0.952 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 0.14364(2) 0.16279(2) 0.34309(2) 0.03986(8) Uani 1 d . . N N 0.2723(4) 0.0605(3) 0.2718(3) 0.0364(8) Uani 1 d . . S S 0.60339(13) 0.18291(12) 0.51532(12) 0.0480(3) Uani 1 d . . C1 C 0.4075(5) 0.0690(4) 0.3300(4) 0.0353(10) Uani 1 d . . C2 C 0.4959(5) 0.0070(4) 0.2925(4) 0.0447(11) Uani 1 d . . H2 H 0.5877(5) 0.0139(4) 0.3313(4) 0.065(7) Uiso 1 calc R . C3 C 0.4483(6) -0.0644(5) 0.1986(5) 0.0586(15) Uani 1 d . . H3 H 0.5071(6) -0.1066(5) 0.1735(5) 0.065(7) Uiso 1 calc R . C4 C 0.3117(6) -0.0730(5) 0.1415(5) 0.0589(15) Uani 1 d . . H4 H 0.2773(6) -0.1214(5) 0.0778(5) 0.065(7) Uiso 1 calc R . C5 C 0.2281(5) -0.0097(5) 0.1797(4) 0.0481(12) Uani 1 d . . H5 H 0.1363(5) -0.0154(5) 0.1403(4) 0.065(7) Uiso 1 calc R . C6 C 0.4416(4) 0.1467(4) 0.4270(4) 0.0348(10) Uani 1 d . . C7 C 0.3445(5) 0.2015(4) 0.4573(4) 0.0387(11) Uani 1 d . . C8 C 0.4063(5) 0.2771(4) 0.5553(4) 0.0452(12) Uani 1 d . . H8 H 0.3581(5) 0.3225(4) 0.5892(4) 0.065(7) Uiso 1 calc R . C9 C 0.5427(6) 0.2742(5) 0.5923(5) 0.0557(14) Uani 1 d . . H9 H 0.5972(6) 0.3182(5) 0.6538(5) 0.065(7) Uiso 1 calc R . C1' C -0.0286(6) 0.1209(6) 0.2267(5) 0.060(2) Uani 1 d . . O1' O -0.1306(5) 0.0976(6) 0.1599(4) 0.099(2) Uani 1 d . . C2' C 0.0598(6) 0.2559(5) 0.4260(5) 0.0538(14) Uani 1 d . . O2' O 0.0140(5) 0.3142(4) 0.4788(4) 0.0810(15) Uani 1 d . . C3' C 0.1632(6) 0.2967(5) 0.2509(5) 0.0548(14) Uani 1 d . . O3' O 0.1770(6) 0.3743(4) 0.1998(5) 0.091(2) Uani 1 d . . C4' C 0.1366(5) 0.0299(5) 0.4419(5) 0.0481(13) Uani 1 d . . O4' O 0.1327(4) -0.0456(4) 0.4990(4) 0.0701(12) Uani 1 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 Re1 0.03208(11) 0.04844(13) 0.03840(11) 0.00118(11) 0.01141(7) 0.00552(11) N 0.035(2) 0.036(2) 0.038(2) 0.001(2) 0.012(2) 0.002(2) S 0.0374(6) 0.0503(8) 0.0531(7) 0.0013(6) 0.0115(6) -0.0020(6) C1 0.038(2) 0.032(2) 0.035(2) 0.006(2) 0.013(2) 0.005(2) C2 0.042(3) 0.042(3) 0.051(3) 0.002(2) 0.018(2) 0.006(2) C3 0.063(4) 0.058(4) 0.060(4) 0.000(3) 0.029(3) 0.019(3) C4 0.071(4) 0.052(3) 0.054(3) -0.014(3) 0.022(3) 0.002(3) C5 0.048(3) 0.043(3) 0.049(3) -0.004(2) 0.012(2) 0.001(2) C6 0.033(2) 0.033(2) 0.039(2) 0.008(2) 0.013(2) 0.004(2) C7 0.038(2) 0.039(2) 0.039(2) 0.003(2) 0.014(2) 0.006(2) C8 0.045(3) 0.043(3) 0.046(3) -0.008(2) 0.013(2) 0.000(2) C9 0.049(3) 0.049(3) 0.058(3) -0.012(3) 0.006(3) -0.008(3) C1' 0.043(3) 0.081(4) 0.053(3) 0.006(3) 0.011(3) -0.002(3) O1' 0.051(3) 0.147(5) 0.077(3) 0.007(3) -0.005(3) -0.020(3) C2' 0.046(3) 0.065(4) 0.049(3) 0.010(3) 0.014(3) 0.016(3) O2' 0.088(3) 0.092(4) 0.074(3) 0.005(3) 0.043(3) 0.042(3) C3' 0.058(3) 0.057(3) 0.047(3) 0.001(3) 0.015(3) 0.016(3) O3' 0.130(5) 0.069(3) 0.078(3) 0.025(3) 0.041(3) 0.008(3) C4' 0.042(3) 0.059(3) 0.049(3) 0.002(3) 0.023(2) 0.005(3) O4' 0.063(3) 0.070(3) 0.091(3) 0.019(3) 0.043(3) 0.012(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 C2' 1.907(11) . yes Re1 C1' 1.954(14) . yes Re1 C3' 1.98(2) . yes Re1 C4' 1.99(2) . yes Re1 C7 2.16(2) . yes Re1 N 2.213(12) . yes N C5 1.340(10) . yes N C1 1.370(11) . yes S C9 1.693(11) . yes S C6 1.738(13) . yes C1 C2 1.386(9) . yes C1 C6 1.437(10) . yes C2 C3 1.367(11) . yes C2 H2 0.93 . yes C3 C4 1.381(13) . yes C3 H3 0.93 . yes C4 C5 1.359(10) . yes C4 H4 0.93 . yes C5 H5 0.93 . yes C6 C7 1.373(9) . yes C7 C8 1.450(11) . yes C8 C9 1.364(12) . yes C8 H8 0.93 . yes C9 H9 0.93 . yes C1' O1' 1.142(10) . yes C2' O2' 1.157(9) . yes C3' O3' 1.140(11) . yes C4' O4' 1.135(10) . yes 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 C2' Re1 C1' 92.1(5) . . yes C2' Re1 C3' 90.7(7) . . yes C1' Re1 C3' 92.4(5) . . yes C2' Re1 C4' 90.0(7) . . yes C1' Re1 C4' 91.3(5) . . yes C3' Re1 C4' 176.3(2) . . yes C2' Re1 C7 94.4(5) . . yes C1' Re1 C7 173.2(2) . . yes C3' Re1 C7 85.8(4) . . yes C4' Re1 C7 90.5(4) . . yes C2' Re1 N 170.4(2) . . yes C1' Re1 N 97.4(5) . . yes C3' Re1 N 90.1(6) . . yes C4' Re1 N 88.6(6) . . yes C7 Re1 N 76.1(5) . . yes C5 N C1 118.7(5) . . yes C5 N Re1 125.3(5) . . yes C1 N Re1 116.0(5) . . yes C9 S C6 90.7(5) . . yes N C1 C2 120.1(6) . . yes N C1 C6 113.2(5) . . yes C2 C1 C6 126.7(6) . . yes C3 C2 C1 120.1(7) . . yes C3 C2 H2 120.0(5) . . yes C1 C2 H2 120.0(5) . . yes C2 C3 C4 119.2(6) . . yes C2 C3 H3 120.4(6) . . yes C4 C3 H3 120.4(5) . . yes C5 C4 C3 119.1(7) . . yes C5 C4 H4 120.5(6) . . yes C3 C4 H4 120.5(5) . . yes N C5 C4 122.8(7) . . yes N C5 H5 118.6(4) . . yes C4 C5 H5 118.6(5) . . yes C7 C6 C1 121.4(6) . . yes C7 C6 S 113.3(6) . . yes C1 C6 S 125.4(5) . . yes C6 C7 C8 109.9(6) . . yes C6 C7 Re1 113.4(6) . . yes C8 C7 Re1 136.6(4) . . yes C9 C8 C7 112.6(6) . . yes C9 C8 H8 123.7(5) . . yes C7 C8 H8 123.7(5) . . yes C8 C9 S 113.5(5) . . yes C8 C9 H9 123.3(5) . . yes S C9 H9 123.3(5) . . yes O1' C1' Re1 178.6(6) . . yes O2' C2' Re1 177.2(6) . . yes O3' C3' Re1 178.5(6) . . yes O4' C4' Re1 179.5(5) . . yes