#------------------------------------------------------------------------------
#$Date: 2016-03-23 21:00:38 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179435 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/32/4333254.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4333254
loop_
_publ_author_name
'Sachse, Anna'
'Mösch-Zanetti, Nadia C'
'Lyashenko, Ganna'
'Wielandt, J. Wolfram'
'Most, Kerstin'
'Magull, Jörg'
'Dall'Antonia, Fabio'
'Pal, Aritra'
'Herbst-Irmer, Regine'
_publ_section_title
;
 Rhenium(V) oxo complexes with acetylacetone derived Schiff bases:
 structure and catalytic epoxidation.
;
_journal_issue                   17
_journal_name_full               'Inorganic chemistry'
_journal_page_first              7129
_journal_page_last               7135
_journal_paper_doi               10.1021/ic700381n
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C12 H15 N O S'
_chemical_formula_weight         221.31
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                112.79(3)
_cell_angle_beta                 106.59(3)
_cell_angle_gamma                92.62(3)
_cell_formula_units_Z            2
_cell_length_a                   7.828(2)
_cell_length_b                   8.018(2)
_cell_length_c                   10.210(2)
_cell_measurement_reflns_used    4747
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      27.589
_cell_measurement_theta_min      2.272
_cell_volume                     557.3(3)
_computing_cell_refinement       'Bruker SAINT (V. 7.12A, Siemens 2003)'
_computing_data_collection       'Siemens SMART (V. 4.202, Siemens 1996)'
_computing_data_reduction        'Bruker SAINT (V. 7.12A, Siemens 2003)'
_computing_molecular_graphics    'Bruker AXS SHELXTL (V. 6.12)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type
'Stoe-Siemens-Huber four circle diffractometer'
_diffrn_measurement_method       'phi scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0952
_diffrn_reflns_av_sigmaI/netI    0.0132
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            11768
_diffrn_reflns_theta_full        27.68
_diffrn_reflns_theta_max         27.68
_diffrn_reflns_theta_min         2.29
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.263
_exptl_absorpt_correction_T_max  0.8799
_exptl_absorpt_correction_T_min  0.8376
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    1.319
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             236
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.50
_refine_diff_density_max         0.533
_refine_diff_density_min         -0.534
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     144
_refine_ls_number_reflns         3305
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_gt           0.0560
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1177P)²+0.2722P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1583
_refine_ls_wR_factor_ref         0.1642
_reflns_number_gt                3047
_reflns_number_total             3305
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic700381nsup4.cif
_cod_data_source_block           snoh
_cod_depositor_comments
'Adding full bibliography for 4333253--4333254.cif.'
_cod_original_cell_volume        557.3(2)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4333254
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
S1 S 0.32873(6) 0.83122(7) 0.56751(5) 0.02254(18) Uani 1 1 d .
O1 O 0.58073(19) 0.5764(2) 0.82157(16) 0.0246(3) Uani 1 1 d .
N1 N 0.2849(2) 0.7290(2) 0.80206(18) 0.0190(4) Uani 1 1 d D
H1 H 0.359(4) 0.667(4) 0.756(3) 0.043(8) Uiso 1 1 d D
C1 C 0.7893(3) 0.6366(3) 1.0628(3) 0.0276(5) Uani 1 1 d .
H1B H 0.8503 0.5498 1.0023 0.041 Uiso 1 1 calc R
H1C H 0.7600 0.5907 1.1313 0.041 Uiso 1 1 calc R
H1D H 0.8693 0.7566 1.1214 0.041 Uiso 1 1 calc R
C2 C 0.6166(3) 0.6563(3) 0.9600(2) 0.0207(4) Uani 1 1 d .
C3 C 0.5056(3) 0.7708(3) 1.0308(2) 0.0207(4) Uani 1 1 d .
H3A H 0.5450 0.8280 1.1377 0.025 Uiso 1 1 calc R
C4 C 0.3449(3) 0.8033(3) 0.9535(2) 0.0190(4) Uani 1 1 d .
C5 C 0.2376(3) 0.9249(3) 1.0389(2) 0.0241(4) Uani 1 1 d .
H5A H 0.1731 0.9895 0.9812 0.036 Uiso 1 1 calc R
H5B H 0.3196 1.0148 1.1365 0.036 Uiso 1 1 calc R
H5C H 0.1499 0.8498 1.0547 0.036 Uiso 1 1 calc R
C6 C 0.1166(3) 0.7334(3) 0.7048(2) 0.0182(4) Uani 1 1 d .
C7 C -0.0471(3) 0.6865(3) 0.7212(2) 0.0221(4) Uani 1 1 d .
H7A H -0.0466 0.6592 0.8039 0.027 Uiso 1 1 calc R
C8 C -0.2108(3) 0.6789(3) 0.6187(2) 0.0243(4) Uani 1 1 d .
H8A H -0.3216 0.6482 0.6317 0.029 Uiso 1 1 calc R
C9 C -0.2114(3) 0.7163(3) 0.4974(2) 0.0246(5) Uani 1 1 d .
H9A H -0.3232 0.7087 0.4255 0.029 Uiso 1 1 calc R
C10 C -0.0489(3) 0.7652(3) 0.4798(2) 0.0221(4) Uani 1 1 d .
H10A H -0.0508 0.7937 0.3974 0.027 Uiso 1 1 calc R
C11 C 0.1166(3) 0.7725(3) 0.5823(2) 0.0187(4) Uani 1 1 d .
C12 C 0.2708(3) 0.8093(3) 0.3776(2) 0.0245(4) Uani 1 1 d .
H12A H 0.3817 0.8304 0.3556 0.037 Uiso 1 1 calc R
H12B H 0.1956 0.9002 0.3654 0.037 Uiso 1 1 calc R
H12C H 0.2035 0.6854 0.3081 0.037 Uiso 1 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
S1 0.0179(3) 0.0314(3) 0.0194(3) 0.0109(2) 0.0074(2) 0.00395(19)
O1 0.0242(7) 0.0311(8) 0.0207(7) 0.0105(6) 0.0098(6) 0.0120(6)
N1 0.0193(8) 0.0233(8) 0.0183(8) 0.0106(7) 0.0081(6) 0.0096(6)
C1 0.0215(10) 0.0367(12) 0.0284(11) 0.0188(10) 0.0057(8) 0.0094(8)
C2 0.0182(9) 0.0246(10) 0.0212(9) 0.0114(8) 0.0061(7) 0.0056(7)
C3 0.0211(9) 0.0244(10) 0.0172(9) 0.0082(8) 0.0077(7) 0.0044(7)
C4 0.0203(9) 0.0193(9) 0.0203(9) 0.0085(8) 0.0104(7) 0.0045(7)
C5 0.0240(9) 0.0257(10) 0.0221(10) 0.0063(8) 0.0113(8) 0.0081(8)
C6 0.0182(9) 0.0175(9) 0.0193(9) 0.0071(7) 0.0069(7) 0.0076(7)
C7 0.0230(10) 0.0228(10) 0.0249(10) 0.0110(8) 0.0119(8) 0.0079(8)
C8 0.0182(9) 0.0235(10) 0.0305(11) 0.0080(9) 0.0113(8) 0.0067(7)
C9 0.0194(9) 0.0256(11) 0.0243(10) 0.0068(8) 0.0052(8) 0.0094(8)
C10 0.0225(9) 0.0254(10) 0.0199(9) 0.0103(8) 0.0072(8) 0.0093(8)
C11 0.0171(8) 0.0202(9) 0.0183(9) 0.0066(7) 0.0066(7) 0.0062(7)
C12 0.0285(10) 0.0293(11) 0.0194(9) 0.0109(8) 0.0119(8) 0.0086(8)
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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
C11 S1 C12 103.18(10)
C4 N1 C6 128.03(16)
O1 C2 C3 123.98(18)
O1 C2 C1 119.28(18)
C3 C2 C1 116.73(18)
C4 C3 C2 123.90(18)
N1 C4 C3 120.48(18)
N1 C4 C5 119.83(18)
C3 C4 C5 119.69(18)
C7 C6 C11 119.73(18)
C7 C6 N1 121.86(18)
C11 C6 N1 118.22(17)
C8 C7 C6 121.0(2)
C9 C8 C7 119.40(19)
C8 C9 C10 120.41(19)
C9 C10 C11 120.50(19)
C10 C11 C6 118.91(18)
C10 C11 S1 123.41(16)
C6 C11 S1 117.68(14)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
S1 C11 1.769(2)
S1 C12 1.795(2)
O1 C2 1.242(3)
N1 C4 1.347(3)
N1 C6 1.417(2)
C1 C2 1.514(3)
C2 C3 1.427(3)
C3 C4 1.377(3)
C4 C5 1.500(3)
C6 C7 1.392(3)
C6 C11 1.402(3)
C7 C8 1.385(3)
C8 C9 1.382(3)
C9 C10 1.394(3)
C10 C11 1.396(3)
