#------------------------------------------------------------------------------
#$Date: 2016-03-23 04:03:07 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179275 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/95/4319594.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_4319594
loop_
_publ_author_name
'Cungen Zhang'
'Ilia A. Guzei'
'James H. Espenson'
_publ_section_title
;
 Synthesis, Structure, and Catalytic Reactivity of N,N,S- and
 O,N,S-Tridentate Oxorhenium(V) Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2437
_journal_page_last               2438
_journal_paper_doi               10.1021/ic001087s
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C13 H13 N2 O Re S'
_chemical_formula_weight         431.51
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.0700(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.2770(5)
_cell_length_b                   12.6460(9)
_cell_length_c                   13.9716(9)
_cell_measurement_temperature    173(2)
_cell_volume                     1280.71(15)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0277
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2611
_diffrn_reflns_theta_full        26.42
_diffrn_reflns_theta_max         26.42
_diffrn_reflns_theta_min         2.18
_exptl_absorpt_coefficient_mu    9.639
_exptl_absorpt_correction_T_max  0.2487
_exptl_absorpt_correction_T_min  0.1134
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    2.238
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.732
_refine_diff_density_min         -0.911
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         2611
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0353
_refine_ls_R_factor_gt           0.0244
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0400P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0598
_refine_ls_wR_factor_ref         0.0652
_reflns_number_gt                2180
_reflns_number_total             2611
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic001087s.cif
_cod_data_source_block           IC001087S
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4319594
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Re Re 0.21266(3) 0.266811(16) 0.052825(13) 0.02363(9) Uani 1 1 d . . .
S S 0.13152(19) 0.26745(10) -0.10850(9) 0.0283(3) Uani 1 1 d . . .
O O 0.4088(5) 0.1967(3) 0.0735(2) 0.0321(8) Uani 1 1 d . . .
N1 N 0.2249(5) 0.4215(3) 0.0305(3) 0.0245(9) Uani 1 1 d . . .
N2 N 0.1527(5) 0.3301(3) 0.1867(3) 0.0263(9) Uani 1 1 d . . .
C1 C -0.0224(7) 0.1670(5) 0.0597(4) 0.0376(13) Uani 1 1 d . . .
H1A H -0.0347 0.1475 0.1267 0.056 Uiso 1 1 calc R . .
H1B H -0.0070 0.1030 0.0218 0.056 Uiso 1 1 calc R . .
H1C H -0.1335 0.2048 0.0338 0.056 Uiso 1 1 calc R . .
C2 C 0.2151(6) 0.3931(4) -0.1384(3) 0.0247(11) Uani 1 1 d . . .
C3 C 0.2390(7) 0.4256(4) -0.2303(3) 0.0293(12) Uani 1 1 d . . .
H3 H 0.2170 0.3777 -0.2825 0.035 Uiso 1 1 calc R . .
C4 C 0.2954(7) 0.5283(4) -0.2470(4) 0.0324(12) Uani 1 1 d . . .
H4 H 0.3143 0.5506 -0.3104 0.039 Uiso 1 1 calc R . .
C5 C 0.3239(7) 0.5982(4) -0.1707(4) 0.0322(12) Uani 1 1 d . . .
H5 H 0.3607 0.6687 -0.1825 0.039 Uiso 1 1 calc R . .
C6 C 0.2998(6) 0.5673(4) -0.0782(3) 0.0271(11) Uani 1 1 d . . .
H6 H 0.3181 0.6167 -0.0271 0.033 Uiso 1 1 calc R . .
C7 C 0.2485(6) 0.4634(4) -0.0594(3) 0.0226(10) Uani 1 1 d . . .
C8 C 0.2335(7) 0.4938(4) 0.1115(3) 0.0260(11) Uani 1 1 d . . .
H8A H 0.1453 0.5527 0.0979 0.031 Uiso 1 1 calc R . .
H8B H 0.3591 0.5241 0.1225 0.031 Uiso 1 1 calc R . .
C9 C 0.1864(6) 0.4348(4) 0.1991(3) 0.0268(11) Uani 1 1 d . . .
C10 C 0.1758(7) 0.4830(5) 0.2876(4) 0.0342(13) Uani 1 1 d . . .
H10 H 0.1984 0.5566 0.2954 0.041 Uiso 1 1 calc R . .
C11 C 0.1317(7) 0.4217(5) 0.3645(4) 0.0400(14) Uani 1 1 d . . .
H11 H 0.1241 0.4528 0.4259 0.048 Uiso 1 1 calc R . .
C12 C 0.0994(7) 0.3164(5) 0.3513(4) 0.0369(13) Uani 1 1 d . . .
H12 H 0.0717 0.2733 0.4039 0.044 Uiso 1 1 calc R . .
C13 C 0.1071(8) 0.2728(5) 0.2621(4) 0.0349(13) Uani 1 1 d . . .
H13 H 0.0793 0.1999 0.2531 0.042 Uiso 1 1 calc R . .
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'
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
O Re N1 119.83(17) . . ?
O Re N2 106.58(16) . . ?
N1 Re N2 77.39(16) . . ?
O Re C1 110.6(2) . . ?
N1 Re C1 129.57(19) . . ?
N2 Re C1 87.42(19) . . ?
O Re S 108.26(12) . . ?
N1 Re S 81.50(11) . . ?
N2 Re S 144.85(11) . . ?
C1 Re S 84.73(15) . . ?
C2 S Re 99.93(16) . . ?
C7 N1 C8 117.7(4) . . ?
C7 N1 Re 122.0(3) . . ?
C8 N1 Re 119.9(3) . . ?
C13 N2 C9 118.8(4) . . ?
C13 N2 Re 125.0(4) . . ?
C9 N2 Re 115.7(3) . . ?
C3 C2 C7 120.8(5) . . ?
C3 C2 S 124.4(4) . . ?
C7 C2 S 114.7(4) . . ?
C2 C3 C4 120.0(5) . . ?
C5 C4 C3 119.6(5) . . ?
C4 C5 C6 121.2(5) . . ?
C5 C6 C7 120.1(5) . . ?
N1 C7 C6 125.8(4) . . ?
N1 C7 C2 116.0(4) . . ?
C6 C7 C2 118.2(4) . . ?
N1 C8 C9 109.0(4) . . ?
N2 C9 C10 121.2(5) . . ?
N2 C9 C8 115.8(4) . . ?
C10 C9 C8 123.0(5) . . ?
C11 C10 C9 118.8(5) . . ?
C12 C11 C10 119.4(5) . . ?
C13 C12 C11 119.8(5) . . ?
N2 C13 C12 122.0(5) . . ?
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 O 1.684(3) . ?
Re N1 1.984(4) . ?
Re N2 2.115(4) . ?
Re C1 2.135(5) . ?
Re S 2.2790(13) . ?
S C2 1.765(5) . ?
N1 C7 1.388(6) . ?
N1 C8 1.453(6) . ?
N2 C13 1.344(6) . ?
N2 C9 1.355(7) . ?
C2 C3 1.375(6) . ?
C2 C7 1.420(6) . ?
C3 C4 1.388(8) . ?
C4 C5 1.386(7) . ?
C5 C6 1.376(6) . ?
C6 C7 1.397(7) . ?
C8 C9 1.498(6) . ?
C9 C10 1.387(7) . ?
C10 C11 1.385(8) . ?
C11 C12 1.362(8) . ?
C12 C13 1.369(7) . ?
