##############################################################################
###                                                                        ###
###        Electronic paper (Acta Crystallographica Section E)             ###
###                                                                        ###
##############################################################################
#                                                                            #
# This CIF contains the data in a paper accepted for publication in Acta     #
# Crystallographica Section E. It conforms to the requirements of Notes      #
# for Authors for Section E, and has been peer reviewed under the auspices   #
# of the IUCr Commission on Journals.                                        #
#                                                                            #
# Full details of the Crystallographic Information File format               #
# are given in the paper "The Crystallographic Information File (CIF):       #
# a New Standard Archive File for Crystallography" by S. R. Hall, F. H.      #
# Allen and I. D. Brown [Acta Cryst. (1991), A47, 655-685].                  #
#                                                                            #
# The current version of the core CIF dictionary is obtainable from          #
# ftp://ftp.iucr.org/pub/cif_core.dic. The current version number is 2.1.    #
#                                                                            #
# Software is freely available for graphical display of the structure(s) in  #
# this CIF.  For information consult the CIF home page http://www.iucr.org/  #
# cif/home.html                                                              #
#                                                                            #
#            Copyright International Union of Crystallography                #
#                                                                            #
##############################################################################
                                             
data_I
_audit_creation_method     SHELXL-97
_chemical_name_systematic
;
(4-Methoxybenzenethiolato-\kS)oxido[2,2'-(propylimino)bis(ethanethiolato)-
κ³S,N,S']rhenium(V)
;
_chemical_name_common     ?
_chemical_formula_moiety     'C14 H22 N O2 Re S3'
_chemical_formula_sum     'C14 H22 N O2 Re S3'
_chemical_formula_weight     518.71
_chemical_melting_point     ?
_symmetry_cell_setting     monoclinic
_symmetry_space_group_name_H-M     'P 21/c'
_symmetry_space_group_name_Hall     '-P 2ybc'
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     12.160(3)
_cell_length_b     16.809(4)
_cell_length_c     9.441(2)
_cell_angle_alpha     90.00
_cell_angle_beta     111.459(4)
_cell_angle_gamma     90.00
_cell_volume     1796.0(7)
_cell_formula_units_Z     4
_cell_measurement_reflns_used     1013
_cell_measurement_theta_min     2.651
_cell_measurement_theta_max     27.91
_cell_measurement_temperature     295(2)
_exptl_crystal_description     needle
_exptl_crystal_colour     red
_exptl_crystal_size_max     0.45
_exptl_crystal_size_mid     0.4
_exptl_crystal_size_min     0.2
_exptl_crystal_density_diffrn     1.918
_exptl_crystal_density_meas     ?
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000     1008
_exptl_absorpt_coefficient_mu     7.117
_exptl_absorpt_correction_type     multi-scan
_exptl_absorpt_process_details     '(SADABS; Sheldrick, 1996)'
_exptl_absorpt_correction_T_min     0.058
_exptl_absorpt_correction_T_max     0.247
_exptl_special_details
;
 ?
;
_diffrn_ambient_temperature     295(2)
_diffrn_radiation_type     MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_source     'fine-focus sealed tube'
_diffrn_radiation_monochromator     graphite
_diffrn_measurement_device_type     'Bruker SMART CCD diffractometer'
_diffrn_measurement_method     ω-scan
_diffrn_detector_area_resol_mean     ?
_diffrn_reflns_number     10348
_diffrn_reflns_av_R_equivalents     0.0597
_diffrn_reflns_av_sigmaI/netI     0.0617
_diffrn_reflns_theta_min     2.17
_diffrn_reflns_theta_max     27.50
_diffrn_reflns_theta_full     27.50
_diffrn_measured_fraction_theta_max     0.974
_diffrn_measured_fraction_theta_full     0.994
_diffrn_reflns_limit_h_min     -12
_diffrn_reflns_limit_h_max     15
_diffrn_reflns_limit_k_min     -18
_diffrn_reflns_limit_k_max     21
_diffrn_reflns_limit_l_min     -12
_diffrn_reflns_limit_l_max     11
_diffrn_standards_number     0
_diffrn_standards_interval_count     .
_diffrn_standards_interval_time     .
_diffrn_standards_decay_%     .
_refine_special_details
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_reflns_number_total     4013
_reflns_number_gt     2835
_reflns_threshold_expression     >2sigma(I)
_refine_ls_structure_factor_coef     Fsqd
_refine_ls_matrix_type     full
_refine_ls_R_factor_all     0.0579
_refine_ls_R_factor_gt     0.0348
_refine_ls_wR_factor_gt     0.0738
_refine_ls_wR_factor_ref     0.0775
_refine_ls_goodness_of_fit_ref     0.892
_refine_ls_restrained_S_all     0.892
_refine_ls_number_reflns     4013
_refine_ls_number_parameters     190
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment     constr
_refine_ls_weighting_scheme     calc
_refine_ls_weighting_details
         'calc w=1/[σ²(Fo²)+(0.0372P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens     geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary     difmap
_refine_ls_shift/su_max     0.001
_refine_ls_shift/su_mean     0.000
_refine_diff_density_max     1.679
_refine_diff_density_min     -1.239
_refine_ls_extinction_method     none
_refine_ls_extinction_coef     ?
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'
    'S' 'S' 0.1246 0.1234
                         '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'
_computing_data_collection     'SMART (Bruker, 1997)'
_computing_cell_refinement     'SAINT (Bruker, 1997)'
_computing_data_reduction     'SAINT (Bruker, 1997)'
_computing_structure_solution     'SHELXS97 (Sheldrick, 1997)'
_computing_structure_refinement     'SHELXL97 (Sheldrick, 1997)'
_computing_molecular_graphics     'SHELXTL (Bruker, 1997)'
_computing_publication_material     'SHELXTL (Bruker, 1997)'
loop_
    _atom_site_type_symbol
    _atom_site_label
    _atom_site_fract_x
    _atom_site_fract_y
    _atom_site_fract_z
    _atom_site_U_iso_or_equiv
    _atom_site_adp_type
    _atom_site_calc_flag
    _atom_site_refinement_flags
    _atom_site_occupancy
    _atom_site_disorder_assembly
    _atom_site_disorder_group
    Re Re 0.700310(19) 0.893135(12) 0.01570(2) 0.04417(9) Uani d . 1 . .
    S S2 0.72046(17) 1.02603(9) 0.06904(18) 0.0645(5) Uani d . 1 . .
    S S1 0.52443(14) 0.82875(9) -0.04378(17) 0.0609(4) Uani d . 1 . .
    S S3 0.63447(14) 0.92485(10) -0.23912(16) 0.0575(4) Uani d . 1 . .
    N N 0.7014(4) 0.8856(2) 0.2477(5) 0.0473(11) Uani d . 1 . .
    O O1 0.8211(3) 0.8372(2) 0.0448(4) 0.0608(11) Uani d . 1 . .
    O O2 0.8870(4) 1.2026(3) -0.3639(5) 0.0802(14) Uani d . 1 . .
    C C1 0.5151(6) 0.8080(4) 0.1407(6) 0.0689(18) Uani d . 1 . .
    H H1B 0.4615 0.8455 0.1597 0.083 Uiso calc R 1 . .
    H H1C 0.4837 0.7549 0.1402 0.083 Uiso calc R 1 . .
    C C2 0.6344(6) 0.8141(4) 0.2648(7) 0.0703(19) Uani d . 1 . .
    H H2A 0.6249 0.8166 0.3623 0.084 Uiso calc R 1 . .
    H H2B 0.6797 0.7667 0.2641 0.084 Uiso calc R 1 . .
    C C3 0.7113(6) 1.0310(3) 0.2570(6) 0.0638(17) Uani d . 1 . .
    H H3A 0.7902 1.0329 0.3343 0.077 Uiso calc R 1 . .
    H H3B 0.6696 1.0789 0.2655 0.077 Uiso calc R 1 . .
    C C4 0.6471(5) 0.9593(3) 0.2808(6) 0.0544(15) Uani d . 1 . .
    H H4A 0.6508 0.9581 0.3852 0.065 Uiso calc R 1 . .
    H H4B 0.5647 0.9621 0.2143 0.065 Uiso calc R 1 . .
    C C5 0.7100(5) 1.0101(3) -0.2697(6) 0.0483(14) Uani d . 1 . .
    C C6 0.8320(5) 1.0194(4) -0.2006(6) 0.0553(15) Uani d . 1 . .
    H H6A 0.8766 0.9817 -0.1313 0.066 Uiso calc R 1 . .
    C C7 0.8863(6) 1.0841(4) -0.2349(7) 0.0605(16) Uani d . 1 . .
    H H7A 0.9677 1.0898 -0.1882 0.073 Uiso calc R 1 . .
    C C8 0.8217(6) 1.1413(4) -0.3381(7) 0.0573(15) Uani d . 1 . .
    C C9 0.7015(6) 1.1325(4) -0.4051(7) 0.0582(16) Uani d . 1 . .
    H H9A 0.6569 1.1704 -0.4739 0.070 Uiso calc R 1 . .
    C C10 0.6463(5) 1.0677(4) -0.3710(6) 0.0570(15) Uani d . 1 . .
    H H10A 0.5647 1.0627 -0.4169 0.068 Uiso calc R 1 . .
    C C11 0.8255(7) 1.2612(4) -0.4715(9) 0.101(3) Uani d . 1 . .
    H H11A 0.8803 1.3004 -0.4794 0.151 Uiso calc R 1 . .
    H H11B 0.7677 1.2862 -0.4391 0.151 Uiso calc R 1 . .
    H H11C 0.7867 1.2366 -0.5689 0.151 Uiso calc R 1 . .
    C C12 0.8277(5) 0.8757(3) 0.3550(6) 0.0576(16) Uani d . 1 . .
    H H12A 0.8746 0.9178 0.3351 0.069 Uiso calc R 1 . .
    H H12B 0.8572 0.8256 0.3320 0.069 Uiso calc R 1 . .
    C C13 0.8477(7) 0.8768(4) 0.5254(7) 0.074(2) Uani d . 1 . .
    H H13A 0.8189 0.9267 0.5500 0.088 Uiso calc R 1 . .
    H H13B 0.8027 0.8341 0.5473 0.088 Uiso calc R 1 . .
    C C14 0.9746(8) 0.8674(6) 0.6222(8) 0.124(3) Uani d . 1 . .
    H H14A 0.9835 0.8685 0.7275 0.186 Uiso calc R 1 . .
    H H14B 1.0192 0.9100 0.6019 0.186 Uiso calc R 1 . .
    H H14C 1.0029 0.8175 0.5996 0.186 Uiso calc R 1 . .
loop_
    _atom_site_aniso_label
    _atom_site_aniso_U_11
    _atom_site_aniso_U_22
    _atom_site_aniso_U_33
    _atom_site_aniso_U_12
    _atom_site_aniso_U_13
    _atom_site_aniso_U_23
    Re 0.04516(15) 0.04144(14) 0.04578(15) 0.00048(10) 0.01648(10) -0.00574(10)
    S2 0.1001(14) 0.0421(8) 0.0571(9) -0.0062(8) 0.0356(9) -0.0031(7)
    S1 0.0518(9) 0.0694(10) 0.0571(9) -0.0097(8) 0.0146(7) -0.0114(8)
    S3 0.0595(10) 0.0647(9) 0.0461(8) -0.0043(8) 0.0166(7) -0.0062(7)
    N 0.045(3) 0.040(3) 0.053(3) 0.000(2) 0.014(2) -0.003(2)
    O1 0.062(3) 0.056(3) 0.064(2) 0.004(2) 0.023(2) -0.008(2)
    O2 0.087(4) 0.069(3) 0.079(3) -0.009(3) 0.024(3) 0.015(2)
    C1 0.070(5) 0.076(4) 0.062(4) -0.028(4) 0.028(3) -0.008(3)
    C2 0.079(5) 0.065(4) 0.062(4) -0.021(4) 0.019(3) 0.002(3)
    C3 0.088(5) 0.051(4) 0.054(4) 0.010(3) 0.027(3) -0.007(3)
    C4 0.056(4) 0.059(4) 0.049(3) 0.005(3) 0.021(3) -0.005(3)
    C5 0.052(4) 0.061(4) 0.033(3) 0.005(3) 0.016(2) -0.004(3)
    C6 0.055(4) 0.064(4) 0.045(3) 0.008(3) 0.017(3) 0.007(3)
    C7 0.045(4) 0.077(4) 0.054(4) 0.006(3) 0.012(3) 0.005(3)
    C8 0.065(4) 0.058(4) 0.053(4) 0.004(3) 0.026(3) 0.002(3)
    C9 0.059(4) 0.060(4) 0.051(4) 0.011(3) 0.014(3) 0.008(3)
    C10 0.049(4) 0.070(4) 0.049(3) 0.006(3) 0.013(3) -0.003(3)
    C11 0.124(7) 0.067(5) 0.104(6) -0.001(4) 0.034(5) 0.028(4)
    C12 0.056(4) 0.058(4) 0.055(4) -0.001(3) 0.016(3) 0.001(3)
    C13 0.079(5) 0.089(5) 0.048(4) 0.002(4) 0.018(3) 0.001(3)
    C14 0.088(6) 0.193(9) 0.062(5) 0.030(7) -0.007(4) -0.010(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_site_symmetry_2
    _geom_bond_distance
    _geom_bond_publ_flag
    Re O1 . 1.679(4) ?
    Re N . 2.189(5) ?
    Re S1 . 2.2762(16) ?
    Re S2 . 2.2833(16) ?
    Re S3 . 2.3030(16) ?
    S2 C3 . 1.820(6) ?
    S1 C1 . 1.820(6) ?
    S3 C5 . 1.782(6) ?
    N C4 . 1.489(6) ?
    N C2 . 1.493(7) ?
    N C12 . 1.509(7) ?
    O2 C8 . 1.376(7) ?
    O2 C11 . 1.416(7) ?
    C1 C2 . 1.498(8) ?
    C1 H1B . 0.9700 ?
    C1 H1C . 0.9700 ?
    C2 H2A . 0.9700 ?
    C2 H2B . 0.9700 ?
    C3 C4 . 1.497(8) ?
    C3 H3A . 0.9700 ?
    C3 H3B . 0.9700 ?
    C4 H4A . 0.9700 ?
    C4 H4B . 0.9700 ?
    C5 C10 . 1.382(7) ?
    C5 C6 . 1.393(7) ?
    C6 C7 . 1.370(8) ?
    C6 H6A . 0.9300 ?
    C7 C8 . 1.390(8) ?
    C7 H7A . 0.9300 ?
    C8 C9 . 1.372(8) ?
    C9 C10 . 1.377(8) ?
    C9 H9A . 0.9300 ?
    C10 H10A . 0.9300 ?
    C11 H11A . 0.9600 ?
    C11 H11B . 0.9600 ?
    C11 H11C . 0.9600 ?
    C12 C13 . 1.536(8) ?
    C12 H12A . 0.9700 ?
    C12 H12B . 0.9700 ?
    C13 C14 . 1.486(10) ?
    C13 H13A . 0.9700 ?
    C13 H13B . 0.9700 ?
    C14 H14A . 0.9600 ?
    C14 H14B . 0.9600 ?
    C14 H14C . 0.9600 ?
loop_
    _geom_angle_atom_site_label_1
    _geom_angle_atom_site_label_2
    _geom_angle_atom_site_label_3
    _geom_angle_site_symmetry_1
    _geom_angle_site_symmetry_3
    _geom_angle
    _geom_angle_publ_flag
    O1 Re N . . 96.85(18) ?
    O1 Re S1 . . 117.42(14) ?
    N Re S1 . . 83.14(12) ?
    O1 Re S2 . . 119.65(14) ?
    N Re S2 . . 82.81(11) ?
    S1 Re S2 . . 122.34(6) ?
    O1 Re S3 . . 104.45(14) ?
    N Re S3 . . 158.59(13) ?
    S1 Re S3 . . 85.19(6) ?
    S2 Re S3 . . 88.41(6) ?
    C3 S2 Re . . 102.7(2) ?
    C1 S1 Re . . 103.7(2) ?
    C5 S3 Re . . 110.64(18) ?
    C4 N C2 . . 110.2(5) ?
    C4 N C12 . . 111.8(4) ?
    C2 N C12 . . 107.4(4) ?
    C4 N Re . . 108.7(3) ?
    C2 N Re . . 110.5(3) ?
    C12 N Re . . 108.1(4) ?
    C8 O2 C11 . . 117.4(6) ?
    C2 C1 S1 . . 110.7(5) ?
    C2 C1 H1B . . 109.5 ?
    S1 C1 H1B . . 109.5 ?
    C2 C1 H1C . . 109.5 ?
    S1 C1 H1C . . 109.5 ?
    H1B C1 H1C . . 108.1 ?
    N C2 C1 . . 112.4(5) ?
    N C2 H2A . . 109.1 ?
    C1 C2 H2A . . 109.1 ?
    N C2 H2B . . 109.1 ?
    C1 C2 H2B . . 109.1 ?
    H2A C2 H2B . . 107.9 ?
    C4 C3 S2 . . 109.3(4) ?
    C4 C3 H3A . . 109.8 ?
    S2 C3 H3A . . 109.8 ?
    C4 C3 H3B . . 109.8 ?
    S2 C3 H3B . . 109.8 ?
    H3A C3 H3B . . 108.3 ?
    N C4 C3 . . 110.0(5) ?
    N C4 H4A . . 109.7 ?
    C3 C4 H4A . . 109.7 ?
    N C4 H4B . . 109.7 ?
    C3 C4 H4B . . 109.7 ?
    H4A C4 H4B . . 108.2 ?
    C10 C5 C6 . . 118.4(5) ?
    C10 C5 S3 . . 118.9(5) ?
    C6 C5 S3 . . 122.6(4) ?
    C7 C6 C5 . . 120.0(5) ?
    C7 C6 H6A . . 120.0 ?
    C5 C6 H6A . . 120.0 ?
    C6 C7 C8 . . 121.2(6) ?
    C6 C7 H7A . . 119.4 ?
    C8 C7 H7A . . 119.4 ?
    C9 C8 O2 . . 125.9(6) ?
    C9 C8 C7 . . 118.8(6) ?
    O2 C8 C7 . . 115.3(6) ?
    C8 C9 C10 . . 120.4(6) ?
    C8 C9 H9A . . 119.8 ?
    C10 C9 H9A . . 119.8 ?
    C9 C10 C5 . . 121.2(6) ?
    C9 C10 H10A . . 119.4 ?
    C5 C10 H10A . . 119.4 ?
    O2 C11 H11A . . 109.5 ?
    O2 C11 H11B . . 109.5 ?
    H11A C11 H11B . . 109.5 ?
    O2 C11 H11C . . 109.5 ?
    H11A C11 H11C . . 109.5 ?
    H11B C11 H11C . . 109.5 ?
    N C12 C13 . . 115.7(5) ?
    N C12 H12A . . 108.4 ?
    C13 C12 H12A . . 108.4 ?
    N C12 H12B . . 108.4 ?
    C13 C12 H12B . . 108.4 ?
    H12A C12 H12B . . 107.4 ?
    C14 C13 C12 . . 111.9(6) ?
    C14 C13 H13A . . 109.2 ?
    C12 C13 H13A . . 109.2 ?
    C14 C13 H13B . . 109.2 ?
    C12 C13 H13B . . 109.2 ?
    H13A C13 H13B . . 107.9 ?
    C13 C14 H14A . . 109.5 ?
    C13 C14 H14B . . 109.5 ?
    H14A C14 H14B . . 109.5 ?
    C13 C14 H14C . . 109.5 ?
    H14A C14 H14C . . 109.5 ?
    H14B C14 H14C . . 109.5 ?
loop_
    _geom_hbond_atom_site_label_D
    _geom_hbond_atom_site_label_H
    _geom_hbond_atom_site_label_A
    _geom_hbond_site_symmetry_A
    _geom_hbond_distance_DH
    _geom_hbond_distance_HA
    _geom_hbond_distance_DA
    _geom_hbond_angle_DHA
    C12 H12B O1 . 0.97 2.59 2.971(7) 103.5
data_global
_journal_date_recd_electronic     2007-10-23
_journal_date_accepted     2007-11-07
_journal_name_full     'Acta Crystallographica, Section E'
_journal_year     2007
_journal_volume     63
_journal_issue     12
_journal_page_first     m3018
_journal_page_last     m3018
_journal_paper_category     QM
_journal_coeditor_code     ZL2076
_publ_contact_author
;
      Kraus, Werner
      Bundesanstalt für Materialforschung und -prüfung
      Richard-Willstätter-Str. 11
      D-12489 Berlin
      Germany
;
_publ_contact_author_email     w.kraus@bam.de
_publ_contact_author_fax     ' '
_publ_contact_author_phone     '+49 30 8104-5845'
_publ_section_title
;\
(4-Methoxybenzenethiolato-κS)oxido[2,2'-(propylimino)\
bis(ethanethiolato)-κ³S,N,S']rhenium(V)
;
loop_
    _publ_author_name
    _publ_author_address
    'Werner Kraus'
;     Bundesanstalt für Materialforschung und -prüfung
      Richard-Willstätter-Strasse 11
      D-12489 Berlin
      Germany
;
    'Franziska Emmerling'
;     Bundesanstalt für Materialforschung und -prüfung
      Richard-Willstätter-Strasse 11
      D-12489 Berlin
      Germany
;
    'Bernhard Noll'
;     Forschungszentrum Rossendorf,
      Institut für Radiopharmazie,
      Postfach 510119, D-01314 Dresden, Germany
;
    'Steffi Noll'
;     Forschungszentrum Rossendorf,
      Institut für Radiopharmazie,
      Postfach 510119, D-01314 Dresden, Germany
;
    'Hans-Jürgen Pietzsch'
;     Forschungszentrum Rossendorf,
      Institut für Radiopharmazie,
      Postfach 510119, D-01314 Dresden, Germany
;
