#------------------------------------------------------------------------------
#$Date: 2024-12-24 04:15:53 +0200 (Tue, 24 Dec 2024) $
#$Revision: 296957 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/97/7249710.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_7249710
loop_
_publ_author_name
'Gradenegger, A.'
'Schachner, J. A.'
'Belaj, F.'
'Mösch-Zanetti, N. C.'
_publ_section_title
;
 An oxidorhenium(v) complex with an electron-withdrawing ligand: benefits
 and drawbacks for a dual role catalyst
;
_journal_issue                   54
_journal_name_full               'RSC Advances'
_journal_page_first              40058
_journal_page_last               40068
_journal_paper_doi               10.1039/D4RA07391F
_journal_volume                  14
_journal_year                    2024
_chemical_absolute_configuration ad
_chemical_compound_source        'synthetical product'
_chemical_formula_moiety         'C13 H16 Cl4 N O3 Re S'
_chemical_formula_sum            'C13 H16 Cl4 N O3 Re S'
_chemical_formula_weight         594.33
_chemical_name_common
trans-dichloro-[2,4-dichloro-6-(4,4-dimethyl-4,5-dihydro-1,3-oxa-zol-2-yl)phenolato-N,O]-dimethylthio-oxo-rhenium(V)
_chemical_name_systematic
trans-dichloro-[2,4-dichloro-6-(4,4-dimethyl-4,5-dihydro-1,3-oxa-zol-2-yl)phenolato-N,O]-dimethylthio-oxo-rhenium(V)
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'manual edited SHELXL-2014/6.cif file'
_audit_update_record
;
2018-07-10 deposited with the CCDC.	2024-12-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.071(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.3972(12)
_cell_length_b                   32.451(5)
_cell_length_c                   6.6411(11)
_cell_measurement_reflns_used    9365
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      35.74
_cell_measurement_theta_min      2.51
_cell_volume                     1805.1(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'modified ORTEP (Johnson, 1965)'
_computing_publication_material  'SHELXL-2014/6 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  'multilayer monochromator'
_diffrn_radiation_source         'Incoatec microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0417
_diffrn_reflns_av_unetI/netI     0.0475
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       52
_diffrn_reflns_limit_k_min       -52
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            16795
_diffrn_reflns_point_group_measured_fraction_full 0.845
_diffrn_reflns_point_group_measured_fraction_max 0.845
_diffrn_reflns_theta_full        35.00
_diffrn_reflns_theta_max         35.00
_diffrn_reflns_theta_min         2.51
_exptl_absorpt_coefficient_mu    7.450
_exptl_absorpt_correction_T_max  0.747
_exptl_absorpt_correction_T_min  0.455
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Bruker (2001). SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.187
_exptl_crystal_description       block
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.150
_refine_diff_density_max         1.847
_refine_diff_density_min         -1.429
_refine_diff_density_rms         0.194
_refine_ls_abs_structure_details
;
 Flack x determined by classical fit to all intensities.
;
_refine_ls_abs_structure_Flack   0.013(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         6728
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0349
_refine_ls_R_factor_gt           0.0298
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0381P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0663
_refine_ls_wR_factor_ref         0.0690
_reflns_Friedel_coverage         0.685
_reflns_Friedel_fraction_full    0.689
_reflns_Friedel_fraction_max     0.689
_reflns_number_gt                6295
_reflns_number_total             6728
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4ra07391f2.cif
_cod_data_source_block           JS76IV
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               7249710
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.268
_shelx_estimated_absorpt_t_max   0.401
_shelxl_version_number           2014/6
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, 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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Re1 Re 0.48551(4) 0.65805(2) 0.68624(4) 0.01853(5) Uani 1 1 d . . . . .
O1 O 0.5108(5) 0.70450(12) 0.5826(8) 0.0341(9) Uani 1 1 d . . . . .
Cl1 Cl 0.32181(17) 0.68143(4) 0.9422(3) 0.0334(3) Uani 1 1 d . . . . .
Cl2 Cl 0.65472(17) 0.62512(5) 0.4569(2) 0.0317(2) Uani 1 1 d . . . . .
O11 O 0.9049(5) 0.63720(12) 1.0763(7) 0.0267(7) Uani 1 1 d . . . . .
C12 C 0.7706(5) 0.62897(14) 0.9622(8) 0.0191(8) Uani 1 1 d . . . . .
N13 N 0.6889(5) 0.66043(11) 0.8923(7) 0.0182(7) Uani 1 1 d . . . . .
C14 C 0.7801(6) 0.69890(14) 0.9572(9) 0.0237(9) Uani 1 1 d . . . . .
C15 C 0.9043(7) 0.68126(18) 1.1133(10) 0.0292(10) Uani 1 1 d . . . . .
H151 H 1.0109 0.6932 1.0960 0.048(18) Uiso 1 1 calc R U . . .
H152 H 0.8745 0.6872 1.2520 0.048(18) Uiso 1 1 calc R U . . .
C16 C 0.6733(7) 0.72971(19) 1.0562(12) 0.0379(14) Uani 1 1 d . . . . .
H161 H 0.5930 0.7403 0.9553 0.042(13) Uiso 1 1 calc R U . . .
H162 H 0.7384 0.7526 1.1127 0.042(13) Uiso 1 1 calc R U . . .
H163 H 0.6200 0.7160 1.1645 0.042(13) Uiso 1 1 calc R U . . .
C17 C 0.8568(8) 0.71721(19) 0.7773(11) 0.0365(13) Uani 1 1 d . . . . .
H171 H 0.9156 0.6957 0.7103 0.041(13) Uiso 1 1 calc R U . . .
H172 H 0.9307 0.7392 0.8235 0.041(13) Uiso 1 1 calc R U . . .
H173 H 0.7738 0.7286 0.6820 0.041(13) Uiso 1 1 calc R U . . .
O21 O 0.4675(4) 0.60197(10) 0.8033(6) 0.0202(6) Uani 1 1 d . . . . .
C21 C 0.5778(5) 0.57423(13) 0.8558(7) 0.0181(7) Uani 1 1 d . . . . .
C22 C 0.5423(6) 0.53194(14) 0.8401(8) 0.0222(8) Uani 1 1 d . . . . .
C23 C 0.6583(7) 0.50213(15) 0.8830(8) 0.0259(9) Uani 1 1 d . . . . .
H23 H 0.6336 0.4737 0.8683 0.035(15) Uiso 1 1 calc R U . . .
C24 C 0.8107(7) 0.51477(15) 0.9476(8) 0.0253(9) Uani 1 1 d . . . . .
C25 C 0.8493(6) 0.55580(15) 0.9764(8) 0.0234(8) Uani 1 1 d . . . . .
H25 H 0.9537 0.5636 1.0268 0.035(15) Uiso 1 1 calc R U . . .
C26 C 0.7323(6) 0.58570(13) 0.9302(7) 0.0195(7) Uani 1 1 d . . . . .
Cl22 Cl 0.35236(18) 0.51747(4) 0.7553(2) 0.0327(3) Uani 1 1 d . . . . .
Cl24 Cl 0.9590(2) 0.47784(5) 0.9878(2) 0.0371(3) Uani 1 1 d . . . . .
S1 S 0.24625(17) 0.64219(4) 0.4747(3) 0.0303(3) Uani 1 1 d . . . . .
C1 C 0.1089(8) 0.6177(2) 0.6338(15) 0.0444(16) Uani 1 1 d . . . . .
H1 H 0.0078 0.6123 0.5553 0.07(2) Uiso 1 1 calc R U . . .
H2 H 0.0898 0.6359 0.7475 0.07(2) Uiso 1 1 calc R U . . .
H3 H 0.1545 0.5916 0.6850 0.07(2) Uiso 1 1 calc R U . . .
C2 C 0.2832(10) 0.5998(2) 0.3095(12) 0.0435(15) Uani 1 1 d . . . . .
H4 H 0.3184 0.5758 0.3901 0.054(17) Uiso 1 1 calc R U . . .
H5 H 0.3665 0.6076 0.2205 0.054(17) Uiso 1 1 calc R U . . .
H6 H 0.1849 0.5931 0.2279 0.054(17) Uiso 1 1 calc R U . . .
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'
Cl Cl 0.1484 0.1585 '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'
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Re1 O21 176.68(19) . . yes
O1 Re1 N13 96.48(19) . . ?
O21 Re1 N13 81.99(14) . . ?
O1 Re1 Cl1 95.91(18) . . ?
O21 Re1 Cl1 87.07(11) . . ?
N13 Re1 Cl1 90.40(13) . . ?
O1 Re1 Cl2 92.39(18) . . ?
O21 Re1 Cl2 84.59(11) . . ?
N13 Re1 Cl2 86.54(13) . . ?
Cl1 Re1 Cl2 171.43(5) . . yes
O1 Re1 S1 94.41(17) . . ?
O21 Re1 S1 87.10(11) . . ?
N13 Re1 S1 169.08(11) . . yes
Cl1 Re1 S1 89.12(6) . . ?
Cl2 Re1 S1 92.36(5) . . ?
C12 O11 C15 106.2(4) . . ?
N13 C12 O11 116.6(4) . . ?
N13 C12 C26 127.0(4) . . ?
O11 C12 C26 116.4(4) . . ?
C12 N13 C14 107.7(4) . . yes
C12 N13 Re1 125.8(3) . . yes
C14 N13 Re1 125.8(3) . . yes
N13 C14 C17 109.5(5) . . ?
N13 C14 C16 111.3(4) . . ?
C17 C14 C16 112.3(5) . . ?
N13 C14 C15 101.1(4) . . ?
C17 C14 C15 111.9(5) . . ?
C16 C14 C15 110.3(5) . . ?
O11 C15 C14 105.3(4) . . ?
O11 C15 H151 110.7 . . ?
C14 C15 H151 110.7 . . ?
O11 C15 H152 110.7 . . ?
C14 C15 H152 110.7 . . ?
H151 C15 H152 108.8 . . ?
C14 C16 H161 109.5 . . ?
C14 C16 H162 109.5 . . ?
H161 C16 H162 109.5 . . ?
C14 C16 H163 109.5 . . ?
H161 C16 H163 109.5 . . ?
H162 C16 H163 109.5 . . ?
C14 C17 H171 109.5 . . ?
C14 C17 H172 109.5 . . ?
H171 C17 H172 109.5 . . ?
C14 C17 H173 109.5 . . ?
H171 C17 H173 109.5 . . ?
H172 C17 H173 109.5 . . ?
C21 O21 Re1 131.0(3) . . yes
O21 C21 C26 121.7(4) . . ?
O21 C21 C22 120.3(4) . . ?
C26 C21 C22 118.0(4) . . ?
C23 C22 C21 121.5(5) . . ?
C23 C22 Cl22 119.9(4) . . ?
C21 C22 Cl22 118.5(4) . . ?
C24 C23 C22 118.5(5) . . ?
C24 C23 H23 120.7 . . ?
C22 C23 H23 120.7 . . ?
C25 C24 C23 122.1(5) . . ?
C25 C24 Cl24 119.1(4) . . ?
C23 C24 Cl24 118.8(4) . . ?
C24 C25 C26 119.0(5) . . ?
C24 C25 H25 120.5 . . ?
C26 C25 H25 120.5 . . ?
C25 C26 C21 120.7(4) . . ?
C25 C26 C12 119.6(4) . . ?
C21 C26 C12 119.8(4) . . ?
C1 S1 C2 99.5(4) . . yes
C1 S1 Re1 107.0(3) . . yes
C2 S1 Re1 110.1(3) . . yes
S1 C1 H1 109.5 . . ?
S1 C1 H2 109.5 . . ?
H1 C1 H2 109.5 . . ?
S1 C1 H3 109.5 . . ?
H1 C1 H3 109.5 . . ?
H2 C1 H3 109.5 . . ?
S1 C2 H4 109.5 . . ?
S1 C2 H5 109.5 . . ?
H4 C2 H5 109.5 . . ?
S1 C2 H6 109.5 . . ?
H4 C2 H6 109.5 . . ?
H5 C2 H6 109.5 . . ?
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
Re1 O1 1.677(4) . yes
Re1 N13 2.113(5) . yes
Re1 O21 1.989(3) . yes
Re1 Cl1 2.3846(15) . yes
Re1 Cl2 2.4057(14) . yes
Re1 S1 2.4238(15) . yes
O11 C12 1.340(6) . ?
O11 C15 1.451(8) . ?
C12 N13 1.298(6) . ?
C12 C26 1.453(6) . ?
N13 C14 1.511(6) . ?
C14 C17 1.518(8) . ?
C14 C16 1.523(8) . ?
C14 C15 1.529(9) . ?
C15 H151 0.99 . ?
C15 H152 0.99 . ?
C16 H161 0.98 . ?
C16 H162 0.98 . ?
C16 H163 0.98 . ?
C17 H171 0.98 . ?
C17 H172 0.98 . ?
C17 H173 0.98 . ?
O21 C21 1.321(5) . ?
C21 C26 1.405(7) . ?
C21 C22 1.407(6) . ?
C22 C23 1.388(7) . ?
C22 Cl22 1.719(5) . ?
C23 C24 1.383(8) . ?
C23 H23 0.95 . ?
C24 C25 1.380(7) . ?
C24 Cl24 1.735(5) . ?
C25 C26 1.399(6) . ?
C25 H25 0.95 . ?
S1 C2 1.799(8) . yes
S1 C1 1.803(8) . yes
C1 H1 0.98 . ?
C1 H2 0.98 . ?
C1 H3 0.98 . ?
C2 H4 0.98 . ?
C2 H5 0.98 . ?
C2 H6 0.98 . ?
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
C15 O11 C12 N13 9.0(6) . . . . ?
C15 O11 C12 C26 -171.0(4) . . . . ?
O11 C12 N13 C14 2.7(6) . . . . ?
C26 C12 N13 C14 -177.2(5) . . . . ?
O11 C12 N13 Re1 173.7(3) . . . . ?
C26 C12 N13 Re1 -6.3(8) . . . . ?
C12 N13 C14 C17 105.8(5) . . . . ?
Re1 N13 C14 C17 -65.1(6) . . . . ?
C12 N13 C14 C16 -129.5(5) . . . . ?
Re1 N13 C14 C16 59.6(6) . . . . ?
C12 N13 C14 C15 -12.4(6) . . . . ?
Re1 N13 C14 C15 176.7(4) . . . . ?
C12 O11 C15 C14 -16.3(5) . . . . ?
N13 C14 C15 O11 17.0(5) . . . . ?
C17 C14 C15 O11 -99.4(5) . . . . ?
C16 C14 C15 O11 134.9(4) . . . . ?
Re1 O21 C21 C26 32.4(7) . . . . ?
Re1 O21 C21 C22 -148.3(4) . . . . ?
O21 C21 C22 C23 176.2(5) . . . . ?
C26 C21 C22 C23 -4.4(7) . . . . ?
O21 C21 C22 Cl22 -1.0(6) . . . . ?
C26 C21 C22 Cl22 178.4(4) . . . . ?
C21 C22 C23 C24 1.7(8) . . . . ?
Cl22 C22 C23 C24 178.9(4) . . . . ?
C22 C23 C24 C25 2.0(8) . . . . ?
C22 C23 C24 Cl24 -176.4(4) . . . . ?
C23 C24 C25 C26 -2.9(8) . . . . ?
Cl24 C24 C25 C26 175.5(4) . . . . ?
C24 C25 C26 C21 0.1(8) . . . . ?
C24 C25 C26 C12 179.2(5) . . . . ?
O21 C21 C26 C25 -177.1(5) . . . . ?
C22 C21 C26 C25 3.5(7) . . . . ?
O21 C21 C26 C12 3.7(7) . . . . ?
C22 C21 C26 C12 -175.7(4) . . . . ?
N13 C12 C26 C25 165.5(5) . . . . ?
O11 C12 C26 C25 -14.5(7) . . . . ?
N13 C12 C26 C21 -15.4(8) . . . . ?
O11 C12 C26 C21 164.7(4) . . . . ?
