# Copyright The Royal Society of Chemistry, 1998 

data_rhen 

 

_audit_creation_method            SHELXL-97 

_chemical_name_systematic     
'Rhenium(I)tetracarbonyl(4-methyl-2phenylpyridinate)'
 

_chemical_name_common             ? 

_chemical_formula_moiety          ? 

_chemical_formula_sum 

 'C16 H10 N O4 Re' 

_chemical_formula_weight          466.45 

 

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' 

 'Re'  'Re'  -1.0185   7.2310 

 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 

 

_symmetry_cell_setting            orthorhombic

_symmetry_space_group_name_H-M    Pbca

 

loop_ 

 _symmetry_equiv_pos_as_xyz 

 'x, y, z' 

 '-x+1/2, -y, z+1/2' 

 'x+1/2, -y+1/2, -z' 

 '-x, y+1/2, -z+1/2' 

 '-x, -y, -z' 

 'x-1/2, y, -z-1/2' 

 '-x-1/2, y-1/2, z' 

 'x, -y-1/2, z-1/2' 

 

_cell_length_a                    12.3490(10) 

_cell_length_b                    12.9660(10) 

_cell_length_c                    19.6070(10) 

_cell_angle_alpha                 90.00 

_cell_angle_beta                  90.00 

_cell_angle_gamma                 90.00 

_cell_volume                      3139.4(4) 

_cell_formula_units_Z             8 

_cell_measurement_temperature     293(2) 

_cell_measurement_reflns_used     5550 

_cell_measurement_theta_min       2.08 

_cell_measurement_theta_max       26.54 

 

_exptl_crystal_description        plate 

_exptl_crystal_colour             yellow 

_exptl_crystal_size_max           '0.2 mm' 

_exptl_crystal_size_mid           '0.2 mm' 

_exptl_crystal_size_min           '0.1 mm' 

_exptl_crystal_density_meas       'not measured' 

_exptl_crystal_density_diffrn     1.974 

_exptl_crystal_density_method     'not measured' 

_exptl_crystal_F_000              1760 

_exptl_absorpt_coefficient_mu     7.757 

_exptl_absorpt_correction_type    empirical 

_exptl_absorpt_correction_T_min   0.0397

_exptl_absorpt_correction_T_max   0.0743 

 

_exptl_special_details 

; 

 ? 

; 

 

_diffrn_ambient_temperature       293(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   'Siemens SMART CCD' 

_diffrn_measurement_method        omega-scan 

_diffrn_detector_area_resol_mean  0.79 

_diffrn_reflns_number             14759 

_diffrn_reflns_av_R_equivalents   0.0523 

_diffrn_reflns_av_sigmaI/netI     0.0336 

_diffrn_reflns_limit_h_min        -14 

_diffrn_reflns_limit_h_max        10 

_diffrn_reflns_limit_k_min        -13 

_diffrn_reflns_limit_k_max        15 

_diffrn_reflns_limit_l_min        -24 

_diffrn_reflns_limit_l_max        24 

_diffrn_reflns_theta_min          2.08 

_diffrn_reflns_theta_max          26.54 

_reflns_number_total              3072 

_reflns_number_gt                 2143 

_reflns_threshold_expression      >2sigma(I) 

 

_computing_data_collection        'Siemens SMART' 

_computing_cell_refinement        'Siemens SMART' 

_computing_data_reduction        'SHELTXL XPREP' 

_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 

_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 

_computing_molecular_graphics     Diamond

_computing_publication_material   'SHELDRICK XCIF' 

 

_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^)+(0.0200P)^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          3072 

_refine_ls_number_parameters      201 

_refine_ls_number_restraints      0 

_refine_ls_R_factor_all           0.0622 

_refine_ls_R_factor_gt            0.0323 

_refine_ls_wR_factor_ref          0.0648 

_refine_ls_wR_factor_gt           0.0569 

_refine_ls_goodness_of_fit_ref    1.308 

_refine_ls_restrained_S_all       1.308 

_refine_ls_shift/su_max           0.011 

_refine_ls_shift/su_mean          0.001 

 

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 

Re1 Re 0.129632(16) 0.805543(17) 0.069797(10) 0.04864(9) Uani 1 d . . . 

N1 N 0.2207(3) 0.8570(3) 0.1599(2) 0.0495(11) Uani 1 d . . . 

C2 C 0.1823(4) 0.8314(4) 0.2235(3) 0.0525(14) Uani 1 d . . . 

C3 C 0.2356(5) 0.8726(5) 0.2804(3) 0.0629(16) Uani 1 d . . . 

C4 C 0.3257(5) 0.9347(5) 0.2702(4) 0.0761(19) Uani 1 d . . . 

H4 H 0.3611 0.9626 0.3078 0.077(6) Uiso 1 calc R . . 

C5 C 0.3633(5) 0.9556(5) 0.2072(4) 0.0805(19) Uani 1 d . . . 

H5 H 0.4244 0.9964 0.2008 0.077(6) Uiso 1 calc R . . 

C6 C 0.3087(5) 0.9150(5) 0.1530(3) 0.0634(16) Uani 1 d . . . 

H6 H 0.3342 0.9284 0.1092 0.077(6) Uiso 1 calc R . . 

C7 C 0.0853(4) 0.7637(4) 0.2214(3) 0.0495(13) Uani 1 d . . . 

C8 C 0.0436(4) 0.7404(4) 0.1560(3) 0.0503(14) Uani 1 d . . . 

C9 C -0.0496(5) 0.6793(5) 0.1530(3) 0.0656(17) Uani 1 d . . . 

H9 H -0.0781 0.6621 0.1106 0.077(6) Uiso 1 calc R . . 

C10 C -0.1005(5) 0.6436(5) 0.2113(4) 0.080(2) Uani 1 d . . . 

H10 H -0.1642 0.6056 0.2079 0.077(6) Uiso 1 calc R . . 

C11 C -0.0576(6) 0.6641(5) 0.2729(4) 0.081(2) Uani 1 d . . . 

H11 H -0.0901 0.6380 0.3120 0.077(6) Uiso 1 calc R . . 

C12 C 0.0336(5) 0.7232(5) 0.2781(3) 0.0730(19) Uani 1 d . . . 

H12 H 0.0620 0.7367 0.3212 0.077(6) Uiso 1 calc R . . 

C13 C 0.1999(6) 0.8551(6) 0.3529(3) 0.100(2) Uani 1 d . . . 

H13A H 0.2044 0.7829 0.3635 0.077(6) Uiso 1 calc R . . 

H13B H 0.1265 0.8780 0.3583 0.077(6) Uiso 1 calc R . . 

H13C H 0.2460 0.8932 0.3832 0.077(6) Uiso 1 calc R . . 

C14 C 0.0338(5) 0.7513(6) 0.0016(3) 0.072(2) Uani 1 d . . . 

O14 O -0.0248(4) 0.7162(5) -0.0376(3) 0.108(2) Uani 1 d . . . 

C15 C 0.2165(5) 0.8766(5) 0.0000(3) 0.0632(16) Uani 1 d . . . 

O15 O 0.2639(4) 0.9182(4) -0.0417(3) 0.0922(15) Uani 1 d . . . 

C16 C 0.2235(5) 0.6804(5) 0.0642(3) 0.0628(16) Uani 1 d . . . 

O16 O 0.2765(4) 0.6095(4) 0.0586(3) 0.1036(17) Uani 1 d . . . 

C17 C 0.0339(4) 0.9283(5) 0.0779(3) 0.0567(15) Uani 1 d . . . 

O17 O -0.0219(4) 0.9975(4) 0.0821(2) 0.0882(15) 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 0.04758(14) 0.05516(15) 0.04317(13) 0.00016(11) -0.00034(11) 0.00128(11) 

N1 0.051(3) 0.044(3) 0.054(3) -0.002(2) -0.007(2) 0.000(2) 

C2 0.056(3) 0.053(4) 0.049(4) 0.000(3) -0.004(3) 0.010(3) 

C3 0.080(4) 0.061(4) 0.048(4) -0.006(3) -0.010(3) 0.019(3) 

C4 0.070(4) 0.076(5) 0.082(5) -0.019(4) -0.025(4) -0.004(4) 

C5 0.060(4) 0.079(5) 0.102(5) 0.001(4) -0.020(4) -0.013(3) 

C6 0.058(4) 0.061(4) 0.071(4) 0.004(3) -0.006(3) -0.008(3) 

C7 0.051(3) 0.047(3) 0.050(4) -0.002(3) 0.003(3) 0.011(3) 

C8 0.047(3) 0.049(3) 0.055(3) 0.001(3) 0.005(3) 0.001(3) 

C9 0.056(4) 0.065(5) 0.077(4) -0.002(3) -0.002(3) -0.010(3) 

C10 0.058(4) 0.076(5) 0.106(6) 0.021(5) 0.017(4) -0.006(3) 

C11 0.083(5) 0.086(6) 0.073(5) 0.027(4) 0.029(4) 0.001(4) 

C12 0.078(5) 0.089(5) 0.053(4) 0.010(4) 0.007(3) 0.003(4) 

C13 0.119(6) 0.111(7) 0.070(5) -0.024(5) -0.019(4) -0.010(5) 

C14 0.070(5) 0.093(6) 0.054(4) -0.010(4) -0.005(3) -0.003(4) 

O14 0.084(3) 0.167(6) 0.074(3) -0.027(4) -0.014(3) -0.022(3) 

C15 0.065(4) 0.061(4) 0.064(4) 0.007(3) 0.007(3) 0.011(3) 

O15 0.095(3) 0.095(4) 0.086(3) 0.027(3) 0.039(3) 0.014(3) 

C16 0.067(4) 0.054(4) 0.067(4) -0.003(3) -0.002(3) -0.003(3) 

O16 0.111(4) 0.064(4) 0.136(5) -0.009(3) 0.002(3) 0.021(3) 

C17 0.056(3) 0.074(4) 0.040(3) 0.008(3) 0.008(3) 0.007(3) 

O17 0.089(3) 0.093(4) 0.083(3) 0.011(3) 0.016(3) 0.039(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 C14 1.919(7) . ? 

Re1 C15 1.967(6) . ? 

Re1 C17 1.989(7) . ? 

Re1 C16 1.997(7) . ? 

Re1 C8 2.168(5) . ? 

Re1 N1 2.198(4) . ? 

N1 C6 1.328(7) . ? 

N1 C2 1.373(6) . ? 

C2 C3 1.402(7) . ? 

C2 C7 1.485(8) . ? 

C3 C4 1.388(8) . ? 

C3 C13 1.505(8) . ? 

C4 C5 1.346(9) . ? 

C5 C6 1.364(8) . ? 

C7 C12 1.386(7) . ? 

C7 C8 1.415(7) . ? 

C8 C9 1.398(8) . ? 

C9 C10 1.385(8) . ? 

C10 C11 1.345(9) . ? 

C11 C12 1.367(9) . ? 

C14 O14 1.150(7) . ? 

C15 O15 1.141(6) . ? 

C16 O16 1.135(7) . ? 

C17 O17 1.134(6) . ? 

 

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 

C14 Re1 C15 91.3(3) . . ? 

C14 Re1 C17 89.0(3) . . ? 

C15 Re1 C17 90.3(2) . . ? 

C14 Re1 C16 91.3(3) . . ? 

C15 Re1 C16 91.5(2) . . ? 

C17 Re1 C16 178.2(2) . . ? 

C14 Re1 C8 95.6(2) . . ? 

C15 Re1 C8 172.7(2) . . ? 

C17 Re1 C8 87.6(2) . . ? 

C16 Re1 C8 90.6(2) . . ? 

C14 Re1 N1 170.6(2) . . ? 

C15 Re1 N1 98.0(2) . . ? 

C17 Re1 N1 89.81(19) . . ? 

C16 Re1 N1 89.6(2) . . ? 

C8 Re1 N1 75.06(19) . . ? 

C6 N1 C2 120.8(5) . . ? 

C6 N1 Re1 120.5(4) . . ? 

C2 N1 Re1 118.7(3) . . ? 

N1 C2 C3 117.9(5) . . ? 

N1 C2 C7 113.3(5) . . ? 

C3 C2 C7 128.7(5) . . ? 

C4 C3 C2 118.8(6) . . ? 

C4 C3 C13 117.3(6) . . ? 

C2 C3 C13 123.9(6) . . ? 

C5 C4 C3 121.7(6) . . ? 

C4 C5 C6 117.8(6) . . ? 

N1 C6 C5 122.9(6) . . ? 

C12 C7 C8 118.6(5) . . ? 

C12 C7 C2 125.0(5) . . ? 

C8 C7 C2 116.5(5) . . ? 

C9 C8 C7 117.4(5) . . ? 

C9 C8 Re1 126.2(4) . . ? 

C7 C8 Re1 116.4(4) . . ? 

C10 C9 C8 121.9(6) . . ? 

C11 C10 C9 119.7(6) . . ? 

C10 C11 C12 120.2(6) . . ? 

C11 C12 C7 122.1(6) . . ? 

O14 C14 Re1 177.6(7) . . ? 

O15 C15 Re1 177.8(6) . . ? 

O16 C16 Re1 177.6(6) . . ? 

O17 C17 Re1 178.9(6) . . ? 

 

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 

C14 Re1 N1 C6 -175.6(14) . . . . ? 

C15 Re1 N1 C6 -2.6(5) . . . . ? 

C17 Re1 N1 C6 -92.9(4) . . . . ? 

C16 Re1 N1 C6 88.8(5) . . . . ? 

C8 Re1 N1 C6 179.6(5) . . . . ? 

C14 Re1 N1 C2 1.9(16) . . . . ? 

C15 Re1 N1 C2 174.9(4) . . . . ? 

C17 Re1 N1 C2 84.6(4) . . . . ? 

C16 Re1 N1 C2 -93.7(4) . . . . ? 

C8 Re1 N1 C2 -3.0(4) . . . . ? 

C6 N1 C2 C3 3.2(8) . . . . ? 

Re1 N1 C2 C3 -174.3(4) . . . . ? 

C6 N1 C2 C7 -178.3(5) . . . . ? 

Re1 N1 C2 C7 4.2(6) . . . . ? 

N1 C2 C3 C4 -1.7(8) . . . . ? 

C7 C2 C3 C4 -179.9(6) . . . . ? 

N1 C2 C3 C13 177.3(6) . . . . ? 

C7 C2 C3 C13 -1.0(10) . . . . ? 

C2 C3 C4 C5 -0.4(9) . . . . ? 

C13 C3 C4 C5 -179.4(7) . . . . ? 

C3 C4 C5 C6 1.0(10) . . . . ? 

C2 N1 C6 C5 -2.7(9) . . . . ? 

Re1 N1 C6 C5 174.7(5) . . . . ? 

C4 C5 C6 N1 0.5(10) . . . . ? 

N1 C2 C7 C12 177.1(5) . . . . ? 

C3 C2 C7 C12 -4.6(10) . . . . ? 

N1 C2 C7 C8 -3.3(7) . . . . ? 

C3 C2 C7 C8 175.0(5) . . . . ? 

C12 C7 C8 C9 1.5(8) . . . . ? 

C2 C7 C8 C9 -178.2(5) . . . . ? 

C12 C7 C8 Re1 -179.5(4) . . . . ? 

C2 C7 C8 Re1 0.8(7) . . . . ? 

C14 Re1 C8 C9 0.7(6) . . . . ? 

C15 Re1 C8 C9 162.9(15) . . . . ? 

C17 Re1 C8 C9 89.5(5) . . . . ? 

C16 Re1 C8 C9 -90.6(5) . . . . ? 

N1 Re1 C8 C9 179.9(6) . . . . ? 

C14 Re1 C8 C7 -178.2(4) . . . . ? 

C15 Re1 C8 C7 -16.1(19) . . . . ? 

C17 Re1 C8 C7 -89.4(4) . . . . ? 

C16 Re1 C8 C7 90.5(4) . . . . ? 

N1 Re1 C8 C7 1.0(4) . . . . ? 

C7 C8 C9 C10 0.8(9) . . . . ? 

Re1 C8 C9 C10 -178.1(5) . . . . ? 

C8 C9 C10 C11 -2.8(10) . . . . ? 

C9 C10 C11 C12 2.5(11) . . . . ? 

C10 C11 C12 C7 -0.2(11) . . . . ? 

C8 C7 C12 C11 -1.8(9) . . . . ? 

C2 C7 C12 C11 177.8(6) . . . . ? 

C15 Re1 C14 O14 162(14) . . . . ? 

C17 Re1 C14 O14 -108(14) . . . . ? 

C16 Re1 C14 O14 70(14) . . . . ? 

C8 Re1 C14 O14 -20(14) . . . . ? 

N1 Re1 C14 O14 -25(15) . . . . ? 

C14 Re1 C15 O15 33(15) . . . . ? 

C17 Re1 C15 O15 -56(15) . . . . ? 

C16 Re1 C15 O15 125(15) . . . . ? 

C8 Re1 C15 O15 -129(14) . . . . ? 

N1 Re1 C15 O15 -145(15) . . . . ? 

C14 Re1 C16 O16 43(14) . . . . ? 

C15 Re1 C16 O16 -48(14) . . . . ? 

C17 Re1 C16 O16 142(12) . . . . ? 

C8 Re1 C16 O16 139(14) . . . . ? 

N1 Re1 C16 O16 -146(14) . . . . ? 

C14 Re1 C17 O17 19(25) . . . . ? 

C15 Re1 C17 O17 111(25) . . . . ? 

C16 Re1 C17 O17 -79(26) . . . . ? 

C8 Re1 C17 O17 -76(25) . . . . ? 

N1 Re1 C17 O17 -152(25) . . . . ? 


_refine_diff_density_max    0.508 

_refine_diff_density_min   -0.650 

_refine_diff_density_rms    0.111