#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:57:40 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179872 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/68/7016811.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_7016811
loop_
_publ_author_name
'Lotz, Simon'
'Landman, Marilé'
'Olivier, Andrew J.'
'Bezuidenhout, Daniela I.'
'Liles, David C.'
'Palmer, Eric R.'
_publ_section_title
;
 Rhenium ethoxy- and hydroxycarbene complexes with thiophene
 substituents.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9394
_journal_page_last               9403
_journal_paper_doi               10.1039/c1dt10824g
_journal_volume                  40
_journal_year                    2011
_chemical_formula_moiety         'C16 H8 O10 Re2 S'
_chemical_formula_sum            'C16 H8 O10 Re2 S'
_chemical_formula_weight         764.68
_chemical_name_systematic
;
nonacarbonyl-(ethoxy-thien-2-yl-methylidene)-di-rhenium
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 101.206(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.5491(6)
_cell_length_b                   13.0140(8)
_cell_length_c                   16.4648(10)
_cell_measurement_reflns_used    8379
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.492
_cell_measurement_theta_min      2.522
_cell_volume                     2007.1(2)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        SAINT
_computing_molecular_graphics
' ORTEP-3 for Windows (Farrugia, 1997), POV-Ray (Cason, 2004)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXTL and SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXTL (Bruker, 2001)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'SMART 1000 CCD'
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.918
_diffrn_measurement_device_type  'Bruker (Seimens) P4'
_diffrn_measurement_method       'φ and ω 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  0.0365
_diffrn_reflns_av_sigmaI/netI    0.0368
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10576
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.53
_diffrn_reflns_theta_min         2.68
_exptl_absorpt_coefficient_mu    12.206
_exptl_absorpt_correction_T_max  0.231
_exptl_absorpt_correction_T_min  0.067
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2001)'
_exptl_crystal_colour            dark-yellow
_exptl_crystal_density_diffrn    2.531
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1400
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.444
_refine_diff_density_min         -1.213
_refine_diff_density_rms         0.162
_refine_ls_extinction_coef       0.00126(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     264
_refine_ls_number_reflns         3829
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.0297
_refine_ls_R_factor_gt           0.0274
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0362P)²+1.1668P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0690
_refine_ls_wR_factor_ref         0.0705
_reflns_number_gt                3545
_reflns_number_total             3829
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            c1dt10824g.txt
_cod_data_source_block           dbmc9f2_complex_1a
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7016811
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'
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
Re1 Re 0.53349(2) 0.065068(15) 0.193204(11) 0.03538(9) Uani 1 1 d .
Re2 Re 0.85693(2) 0.019919(14) 0.238859(11) 0.03368(9) Uani 1 1 d .
C1 C 0.3325(6) 0.0920(4) 0.1569(3) 0.0453(12) Uani 1 1 d .
O1 O 0.2145(5) 0.1080(4) 0.1333(3) 0.0647(11) Uani 1 1 d .
C2 C 0.5469(6) 0.1636(4) 0.2864(3) 0.0455(12) Uani 1 1 d .
O2 O 0.5504(5) 0.2171(4) 0.3407(3) 0.0685(12) Uani 1 1 d .
C3 C 0.5923(6) 0.1736(4) 0.1205(3) 0.0428(12) Uani 1 1 d .
O3 O 0.6273(5) 0.2339(3) 0.0798(3) 0.0626(11) Uani 1 1 d .
C4 C 0.5354(6) -0.0399(4) 0.1066(3) 0.0477(13) Uani 1 1 d .
O4 O 0.5369(6) -0.1011(3) 0.0575(3) 0.0696(13) Uani 1 1 d .
C5 C 0.5049(6) -0.0466(4) 0.2707(4) 0.0469(12) Uani 1 1 d .
O5 O 0.4891(5) -0.1108(4) 0.3143(3) 0.0691(13) Uani 1 1 d .
C6 C 1.0549(6) -0.0180(4) 0.2687(3) 0.0477(13) Uani 1 1 d .
O6 O 1.1728(5) -0.0413(4) 0.2855(4) 0.0735(14) Uani 1 1 d .
C7 C 0.9058(6) 0.1613(4) 0.2083(3) 0.0472(12) Uani 1 1 d .
O7 O 0.9359(5) 0.2356(3) 0.1815(3) 0.0636(11) Uani 1 1 d .
C8 C 0.8473(7) -0.0055(4) 0.1192(4) 0.0491(13) Uani 1 1 d .
O8 O 0.8423(6) -0.0180(4) 0.0509(3) 0.0744(14) Uani 1 1 d .
C9 C 0.7896(6) -0.1237(4) 0.2400(3) 0.0428(11) Uani 1 1 d .
O9 O 0.7531(5) -0.2071(3) 0.2304(3) 0.0630(11) Uani 1 1 d .
C10 C 0.8385(5) 0.0505(4) 0.3631(3) 0.0385(11) Uani 1 1 d .
O10 O 0.8493(4) 0.1392(3) 0.4045(2) 0.0474(9) Uani 1 1 d .
S1 S 0.7169(3) 0.01201(16) 0.49851(12) 0.0838(6) Uani 1 1 d .
C11 C 0.8034(6) -0.0261(4) 0.4209(3) 0.0420(12) Uani 1 1 d .
C12 C 0.8270(7) -0.1323(4) 0.4250(3) 0.0502(13) Uani 1 1 d .
H12 H 0.8717 -0.1685 0.3885 0.060 Uiso 1 1 calc R
C13 C 0.7751(8) -0.1774(5) 0.4907(4) 0.0670(18) Uani 1 1 d .
H13 H 0.7841 -0.2470 0.5035 0.080 Uiso 1 1 calc R
C14 C 0.7121(10) -0.1106(7) 0.5326(5) 0.087(2) Uani 1 1 d .
H14 H 0.6692 -0.1292 0.5766 0.105 Uiso 1 1 calc R
C15 C 0.8825(7) 0.2359(4) 0.3710(4) 0.0560(15) Uani 1 1 d .
H15A H 0.8167 0.2500 0.3194 0.067 Uiso 1 1 calc R
H15B H 0.9789 0.2351 0.3603 0.067 Uiso 1 1 calc R
C16 C 0.8685(8) 0.3168(5) 0.4350(4) 0.0715(19) Uani 1 1 d .
H16A H 0.7714 0.3195 0.4425 0.107 Uiso 1 1 calc R
H16B H 0.8955 0.3826 0.4165 0.107 Uiso 1 1 calc R
H16C H 0.9299 0.2996 0.4866 0.107 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'
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
C1 Re1 C4 92.9(2)
C1 Re1 C2 91.9(2)
C4 Re1 C2 174.7(2)
C1 Re1 C5 94.5(2)
C4 Re1 C5 88.8(2)
C2 Re1 C5 88.4(2)
C1 Re1 C3 93.7(2)
C4 Re1 C3 90.7(2)
C2 Re1 C3 91.3(2)
C5 Re1 C3 171.8(2)
C1 Re1 Re2 176.09(15)
C4 Re1 Re2 83.98(18)
C2 Re1 Re2 91.34(15)
C5 Re1 Re2 87.73(16)
C3 Re1 Re2 84.04(16)
C6 Re2 C9 93.4(2)
C6 Re2 C8 93.7(2)
C9 Re2 C8 84.2(2)
C6 Re2 C7 92.0(2)
C9 Re2 C7 166.0(2)
C8 Re2 C7 82.6(2)
C6 Re2 C10 93.6(2)
C9 Re2 C10 94.6(2)
C8 Re2 C10 172.6(2)
C7 Re2 C10 97.9(2)
C6 Re2 Re1 175.97(17)
C9 Re2 Re1 82.58(15)
C8 Re2 Re1 86.49(18)
C7 Re2 Re1 92.02(17)
C10 Re2 Re1 86.14(14)
O1 C1 Re1 178.1(5)
O2 C2 Re1 177.0(5)
O3 C3 Re1 179.0(5)
O4 C4 Re1 179.2(5)
O5 C5 Re1 179.3(6)
O6 C6 Re2 179.1(6)
O7 C7 Re2 170.8(5)
O8 C8 Re2 178.7(6)
O9 C9 Re2 171.2(5)
O10 C10 C11 105.2(4)
O10 C10 Re2 129.9(4)
C11 C10 Re2 124.9(4)
C10 O10 C15 124.3(4)
C14 S1 C11 91.3(3)
C12 C11 C10 130.4(5)
C12 C11 S1 110.2(4)
C10 C11 S1 119.4(4)
C11 C12 C13 111.9(5)
C11 C12 H12 124.1
C13 C12 H12 124.1
C14 C13 C12 113.0(6)
C14 C13 H13 123.5
C12 C13 H13 123.5
C13 C14 S1 113.6(5)
C13 C14 H14 123.2
S1 C14 H14 123.2
O10 C15 C16 106.6(5)
O10 C15 H15A 110.4
C16 C15 H15A 110.4
O10 C15 H15B 110.4
C16 C15 H15B 110.4
H15A C15 H15B 108.6
C15 C16 H16A 109.5
C15 C16 H16B 109.5
H16A C16 H16B 109.5
C15 C16 H16C 109.5
H16A C16 H16C 109.5
H16B C16 H16C 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Re1 C1 1.928(6)
Re1 C4 1.977(6)
Re1 C2 1.984(6)
Re1 C5 1.988(6)
Re1 C3 2.002(5)
Re1 Re2 3.0899(3)
Re2 C6 1.923(6)
Re2 C9 1.978(5)
Re2 C8 1.982(6)
Re2 C7 1.987(6)
Re2 C10 2.125(5)
C1 O1 1.137(6)
C2 O2 1.129(7)
C3 O3 1.123(6)
C4 O4 1.136(7)
C5 O5 1.129(7)
C6 O6 1.146(7)
C7 O7 1.123(6)
C8 O8 1.129(7)
C9 O9 1.141(6)
C10 O10 1.335(6)
C10 C11 1.461(7)
O10 C15 1.434(7)
S1 C14 1.695(8)
S1 C11 1.723(5)
C11 C12 1.400(8)
C12 C13 1.403(8)
C12 H12 0.9300
C13 C14 1.326(11)
C13 H13 0.9300
C14 H14 0.9300
C15 C16 1.514(8)
C15 H15A 0.9700
C15 H15B 0.9700
C16 H16A 0.9600
C16 H16B 0.9600
C16 H16C 0.9600
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
C4 Re1 Re2 C9 -51.7(2)
C2 Re1 Re2 C9 125.7(2)
C5 Re1 Re2 C9 37.3(2)
C3 Re1 Re2 C9 -143.1(2)
C4 Re1 Re2 C8 32.9(2)
C2 Re1 Re2 C8 -149.7(2)
C5 Re1 Re2 C8 122.0(2)
C3 Re1 Re2 C8 -58.5(2)
C4 Re1 Re2 C7 115.3(2)
C2 Re1 Re2 C7 -67.2(2)
C5 Re1 Re2 C7 -155.6(2)
C3 Re1 Re2 C7 23.9(2)
C4 Re1 Re2 C10 -146.9(2)
C2 Re1 Re2 C10 30.6(2)
C5 Re1 Re2 C10 -57.8(2)
C3 Re1 Re2 C10 121.8(2)
C6 Re2 C10 O10 95.7(5)
C9 Re2 C10 O10 -170.5(5)
C7 Re2 C10 O10 3.2(5)
Re1 Re2 C10 O10 -88.3(5)
C6 Re2 C10 C11 -87.3(5)
C9 Re2 C10 C11 6.5(5)
C7 Re2 C10 C11 -179.8(5)
Re1 Re2 C10 C11 88.7(4)
C11 C10 O10 C15 -179.9(5)
Re2 C10 O10 C15 -2.4(8)
O10 C10 C11 C12 -154.7(6)
Re2 C10 C11 C12 27.7(9)
O10 C10 C11 S1 26.1(6)
Re2 C10 C11 S1 -151.5(3)
C14 S1 C11 C12 -0.8(5)
C14 S1 C11 C10 178.6(5)
C10 C11 C12 C13 -179.6(6)
S1 C11 C12 C13 -0.4(7)
C11 C12 C13 C14 1.8(9)
C12 C13 C14 S1 -2.4(10)
C11 S1 C14 C13 1.9(7)
C10 O10 C15 C16 174.2(5)
