# Supplementary Information (SI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_JS76IV
_database_code_depnum_ccdc_archive 'CCDC 1854790'
loop_
_audit_author_name
_audit_author_address
'Ferdinand Belaj'
;University of Graz
Austria
;
_audit_update_record             
;
2018-07-10 deposited with the CCDC.	2024-12-12 downloaded from the CCDC.
;
_audit_creation_method           'manual edited SHELXL-2014/6.cif file'

_chemical_compound_source        'synthetical product'

_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)
_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_melting_point          ?
_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

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_H-M_alt        'C c'
_space_group_name_Hall           'C -2yc'

_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.
;

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'

_cell_length_a                   8.3972(12)
_cell_length_b                   32.451(5)
_cell_length_c                   6.6411(11)
_cell_angle_alpha                90
_cell_angle_beta                 94.071(5)
_cell_angle_gamma                90
_cell_volume                     1805.1(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9365
_cell_measurement_theta_min      2.51
_cell_measurement_theta_max      35.74

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.187
_exptl_crystal_F_000             1136
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    7.450
_shelx_estimated_absorpt_T_min   0.268
_shelx_estimated_absorpt_T_max   0.401
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.455
_exptl_absorpt_correction_T_max  0.747
_exptl_absorpt_process_details   
'Bruker (2001). SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.'

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_source         'Incoatec microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  'multilayer monochromator'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            16795
_diffrn_reflns_av_unetI/netI     0.0475
_diffrn_reflns_av_R_equivalents  0.0417
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -52
_diffrn_reflns_limit_k_max       52
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         2.51
_diffrn_reflns_theta_max         35.00
_diffrn_reflns_theta_full        35.00
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.845
_diffrn_reflns_point_group_measured_fraction_full 0.845
_reflns_number_total             6728
_reflns_number_gt                6295
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.685
_reflns_Friedel_fraction_max     0.689
_reflns_Friedel_fraction_full    0.689

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2015)'
_computing_molecular_graphics    'modified ORTEP (Johnson, 1965)'
_computing_publication_material  'SHELXL-2014/6 (Sheldrick, 2015)'

_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.
 
 The absolute configuration was determined by anomalous dispersion effects in
 the diffraction measurements on the crystal.
 
 The non-hydrogen atoms were refined with anisotropic displacement parameters
 without any constraints.
 
 The H atoms of the phenyl ring were put at the external bisectors of the
 C-C-C angles at C-H distances of 0.95 Å and a common isotropic displacement
 parameter was refined for these H atoms (AFIX 43 of SHELXL).
 
 The H atoms of the CH₂ group were refined with common isotropic
 displacement parameters and idealized geometry with approximately
 tetrahedral angles and C-H distances of 0.99 Å (AFIX 23 of SHELXL).
 
 The H atoms of the methyl groups were refined with common isotropic
 displacement parameters for the H atoms of the same group and idealized
 geometries with tetrahedral angles, enabling rotation around the C-C bonds,
 and C-H distances of 0.98 Å (AFIX 137 of SHELXL).
 
 The largest peaks in a final difference Fourier map (0.97 - 1.85 eÅ⁻³)
 were in the vicinity (0.80 - 0.89 Å) of the Re atom.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0381P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    refU
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 
;
 Flack x determined by classical fit to all intensities.
;
_refine_ls_abs_structure_Flack   0.013(7)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         6728
_refine_ls_number_parameters     218
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0349
_refine_ls_R_factor_gt           0.0298
_refine_ls_wR_factor_ref         0.0690
_refine_ls_wR_factor_gt          0.0663
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.034
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

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 . . .


_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_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_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_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) . . . . ?

_refine_diff_density_max         1.847
_refine_diff_density_min         -1.429
_refine_diff_density_rms         0.194

_shelxl_version_number           2014/6

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_JS76
_database_code_depnum_ccdc_archive 'CCDC 1854791'
loop_
_audit_author_name
_audit_author_address
'Ferdinand Belaj'
;University of Graz
Austria
;
_audit_update_record             
;
2018-07-10 deposited with the CCDC.	2024-12-12 downloaded from the CCDC.
;
_audit_creation_method           'manual edited SHELXL-2014/6.cif file'

_chemical_compound_source        'synthetical product'

_chemical_name_systematic        
'cis-dichloro-[2,4-dichloro-6-(4,4-dimethyl-4,5-dihydro-1,3-oxa-zol-2-yl)phenolato-N,O]-oxo-(triphenylphosphine oxide-O)-rhenium(V)'
_chemical_name_common            
'cis-dichloro-[2,4-dichloro-6-(4,4-dimethyl-4,5-dihydro-1,3-oxa-zol-2-yl)phenolato-N,O]-oxo-(triphenylphosphine oxide-O)-rhenium(V)'
_chemical_melting_point          ?
_chemical_formula_moiety         'C29 H25 Cl4 N O4 P Re'
_chemical_formula_sum            'C29 H25 Cl4 N O4 P Re'
_chemical_formula_weight         810.47

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'
P P 0.1023 0.0942 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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.
;

loop_
_space_group_symop_operation_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'

_cell_length_a                   11.6314(5)
_cell_length_b                   20.2311(9)
_cell_length_c                   12.6581(6)
_cell_angle_alpha                90
_cell_angle_beta                 101.269(2)
_cell_angle_gamma                90
_cell_volume                     2921.2(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    8513
_cell_measurement_theta_min      2.40
_cell_measurement_theta_max      30.49

_exptl_crystal_description       plate
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.843
_exptl_crystal_F_000             1584
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.070
_exptl_absorpt_coefficient_mu    4.617
_shelx_estimated_absorpt_T_min   0.391
_shelx_estimated_absorpt_T_max   0.738
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.719
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
'Bruker (2001). SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.'

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_source         'Incoatec microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  'multilayer monochromator'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            26705
_diffrn_reflns_av_unetI/netI     0.0558
_diffrn_reflns_av_R_equivalents  0.0505
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.92
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_full        30.00
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             8522
_reflns_number_gt                6802
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     ?
_reflns_Friedel_fraction_full    ?

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2015)'
_computing_molecular_graphics    'modified ORTEP (Johnson, 1965)'
_computing_publication_material  'SHELXL-2014/6 (Sheldrick, 2015)'

_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.
 
 The non-hydrogen atoms were refined with anisotropic displacement parameters
 without any constraints.
 
 The H atoms of the phenyl rings were put at the external bisectors of the
 C-C-C angles at C-H distances of 0.95 Å and common isotropic displacement
 parameters were refined for the H atoms of the same ring
 (AFIX 43 of SHELXL).
 
 The H atoms of the CH₂ group were refined with common isotropic
 displacement parameters and idealized geometry with approximately
 tetrahedral angles and C-H distances of 0.99 Å (AFIX 23 of SHELXL).
 
 The H atoms of the methyl groups were refined with common isotropic
 displacement parameters for the H atoms of the same group and idealized
 geometries with tetrahedral angles, enabling rotation around the C-C bonds,
 and C-H distances of 0.98 Å (AFIX 137 of SHELXL).
 
 The largest peaks in a final difference Fourier map (0.92 - 1.98 eÅ⁻³)
 were in the vicinity (0.64 - 1.08 Å) of the Re atom.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0305P)²+2.1365P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    refU
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8522
_refine_ls_number_parameters     370
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_gt           0.0343
_refine_ls_wR_factor_ref         0.0789
_refine_ls_wR_factor_gt          0.0732
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_restrained_S_all      1.014
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000

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 0.18430(2) 0.65112(2) 0.81667(2) 0.01657(5) Uani 1 1 d . . . . .
O1 O 0.0622(2) 0.62186(16) 0.8544(2) 0.0303(7) Uani 1 1 d . . . . .
Cl1 Cl 0.32295(8) 0.62588(5) 0.97471(7) 0.02347(19) Uani 1 1 d . . . . .
Cl2 Cl 0.17194(9) 0.75953(5) 0.88781(8) 0.0256(2) Uani 1 1 d . . . . .
O11 O 0.0196(2) 0.65132(12) 0.4860(2) 0.0218(6) Uani 1 1 d . . . . .
C12 C 0.0875(3) 0.63160(17) 0.5791(3) 0.0170(7) Uani 1 1 d . . . . .
N13 N 0.0922(3) 0.67242(14) 0.6599(2) 0.0160(6) Uani 1 1 d . . . . .
C14 C 0.0180(3) 0.73236(17) 0.6209(3) 0.0182(7) Uani 1 1 d . . . . .
C15 C -0.0416(4) 0.7104(2) 0.5076(3) 0.0331(10) Uani 1 1 d . . . . .
H151 H -0.1257 0.7009 0.5049 0.042(10) Uiso 1 1 calc R U . . .
H152 H -0.0351 0.7452 0.4542 0.042(10) Uiso 1 1 calc R U . . .
C16 C 0.0961(3) 0.79235(18) 0.6163(3) 0.0240(8) Uani 1 1 d . . . . .
H161 H 0.1413 0.8017 0.6886 0.029(7) Uiso 1 1 calc R U . . .
H162 H 0.0474 0.8307 0.5901 0.029(7) Uiso 1 1 calc R U . . .
H163 H 0.1499 0.7832 0.5674 0.029(7) Uiso 1 1 calc R U . . .
C17 C -0.0740(3) 0.7447(2) 0.6896(3) 0.0254(8) Uani 1 1 d . . . . .
H171 H -0.1141 0.7031 0.6991 0.039(8) Uiso 1 1 calc R U . . .
H172 H -0.1313 0.7770 0.6536 0.039(8) Uiso 1 1 calc R U . . .
H173 H -0.0358 0.7618 0.7601 0.039(8) Uiso 1 1 calc R U . . .
O21 O 0.2398(3) 0.56628(12) 0.7632(2) 0.0238(6) Uani 1 1 d . . . . .
C21 C 0.2173(3) 0.54009(17) 0.6653(3) 0.0195(7) Uani 1 1 d . . . . .
C22 C 0.2696(3) 0.47795(17) 0.6512(3) 0.0212(8) Uani 1 1 d . . . . .
C23 C 0.2514(4) 0.44582(17) 0.5535(3) 0.0230(8) Uani 1 1 d . . . . .
H23 H 0.2862 0.4040 0.5467 0.023(8) Uiso 1 1 calc R U . . .
C24 C 0.1808(4) 0.47593(18) 0.4647(3) 0.0233(8) Uani 1 1 d . . . . .
C25 C 0.1276(3) 0.53564(18) 0.4738(3) 0.0214(8) Uani 1 1 d . . . . .
H25 H 0.0796 0.5552 0.4124 0.023(8) Uiso 1 1 calc R U . . .
C26 C 0.1444(3) 0.56778(17) 0.5742(3) 0.0193(7) Uani 1 1 d . . . . .
Cl22 Cl 0.35898(10) 0.44247(5) 0.76195(9) 0.0332(2) Uani 1 1 d . . . . .
Cl24 Cl 0.16327(11) 0.43750(5) 0.33943(9) 0.0370(3) Uani 1 1 d . . . . .
O2 O 0.3270(2) 0.69141(13) 0.7533(2) 0.0217(6) Uani 1 1 d . . . . .
P1 P 0.43595(8) 0.69408(5) 0.70533(8) 0.01790(19) Uani 1 1 d . . . . .
C31 C 0.4727(3) 0.77917(18) 0.6881(3) 0.0185(7) Uani 1 1 d . . . . .
C32 C 0.5555(4) 0.7964(2) 0.6266(3) 0.0245(8) Uani 1 1 d . . . . .
H32 H 0.5929 0.7628 0.5932 0.033(6) Uiso 1 1 calc R U . . .
C33 C 0.5836(4) 0.8621(2) 0.6140(3) 0.0292(9) Uani 1 1 d . . . . .
H33 H 0.6419 0.8736 0.5742 0.033(6) Uiso 1 1 calc R U . . .
C34 C 0.5255(4) 0.9111(2) 0.6603(3) 0.0294(9) Uani 1 1 d . . . . .
H34 H 0.5440 0.9562 0.6513 0.033(6) Uiso 1 1 calc R U . . .
C35 C 0.4413(4) 0.8948(2) 0.7192(3) 0.0267(9) Uani 1 1 d . . . . .
H35 H 0.4017 0.9287 0.7499 0.033(6) Uiso 1 1 calc R U . . .
C36 C 0.4149(3) 0.82877(18) 0.7334(3) 0.0200(7) Uani 1 1 d . . . . .
H36 H 0.3572 0.8175 0.7741 0.033(6) Uiso 1 1 calc R U . . .
C41 C 0.5572(3) 0.65225(18) 0.7906(3) 0.0201(7) Uani 1 1 d . . . . .
C42 C 0.5340(4) 0.5913(2) 0.8356(3) 0.0287(9) Uani 1 1 d . . . . .
H42 H 0.4571 0.5733 0.8208 0.036(6) Uiso 1 1 calc R U . . .
C43 C 0.6247(4) 0.5575(2) 0.9019(4) 0.0357(10) Uani 1 1 d . . . . .
H43 H 0.6098 0.5160 0.9315 0.036(6) Uiso 1 1 calc R U . . .
C44 C 0.7365(4) 0.5841(2) 0.9247(4) 0.0344(10) Uani 1 1 d . . . . .
H44 H 0.7974 0.5612 0.9714 0.036(6) Uiso 1 1 calc R U . . .
C45 C 0.7597(4) 0.6433(2) 0.8806(3) 0.0324(10) Uani 1 1 d . . . . .
H45 H 0.8370 0.6609 0.8961 0.036(6) Uiso 1 1 calc R U . . .
C46 C 0.6701(3) 0.6782(2) 0.8122(3) 0.0255(8) Uani 1 1 d . . . . .
H46 H 0.6865 0.7191 0.7813 0.036(6) Uiso 1 1 calc R U . . .
C51 C 0.4115(3) 0.65800(17) 0.5723(3) 0.0201(7) Uani 1 1 d . . . . .
C52 C 0.3250(4) 0.6839(2) 0.4934(3) 0.0259(9) Uani 1 1 d . . . . .
H52 H 0.2818 0.7212 0.5095 0.032(5) Uiso 1 1 calc R U . . .
C53 C 0.2996(4) 0.6566(2) 0.3906(3) 0.0307(9) Uani 1 1 d . . . . .
H53 H 0.2380 0.6744 0.3377 0.032(5) Uiso 1 1 calc R U . . .
C54 C 0.3642(4) 0.6033(2) 0.3656(3) 0.0286(9) Uani 1 1 d . . . . .
H54 H 0.3481 0.5847 0.2953 0.032(5) Uiso 1 1 calc R U . . .
C55 C 0.4532(4) 0.5772(2) 0.4445(3) 0.0298(9) Uani 1 1 d . . . . .
H55 H 0.4980 0.5408 0.4276 0.032(5) Uiso 1 1 calc R U . . .
C56 C 0.4769(4) 0.60376(19) 0.5472(3) 0.0255(8) Uani 1 1 d . . . . .
H56 H 0.5372 0.5854 0.6007 0.032(5) Uiso 1 1 calc R U . . .


_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_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Re1 O1 1.692(3) . yes
Re1 O2 2.141(3) . yes
Re1 N13 2.107(3) . yes
Re1 O21 1.998(2) . yes
Re1 Cl1 2.3670(9) . yes
Re1 Cl2 2.3858(10) . yes
O11 C12 1.345(4) . ?
O11 C15 1.445(4) . ?
C12 N13 1.308(5) . ?
C12 C26 1.457(5) . ?
N13 C14 1.514(4) . ?
C14 C16 1.524(5) . ?
C14 C17 1.525(5) . ?
C14 C15 1.531(5) . ?
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 1.326(4) . ?
C21 C26 1.407(5) . ?
C21 C22 1.423(5) . ?
C22 C23 1.377(5) . ?
C22 Cl22 1.729(4) . ?
C23 C24 1.396(6) . ?
C23 H23 0.95 . ?
C24 C25 1.372(5) . ?
C24 Cl24 1.741(4) . ?
C25 C26 1.408(5) . ?
C25 H25 0.95 . ?
O2 P1 1.510(3) . yes
P1 C31 1.797(4) . ?
P1 C51 1.806(4) . ?
P1 C41 1.810(4) . ?
C31 C36 1.392(5) . ?
C31 C32 1.395(5) . ?
C32 C33 1.386(5) . ?
C32 H32 0.95 . ?
C33 C34 1.391(6) . ?
C33 H33 0.95 . ?
C34 C35 1.381(6) . ?
C34 H34 0.95 . ?
C35 C36 1.391(5) . ?
C35 H35 0.95 . ?
C36 H36 0.95 . ?
C41 C46 1.391(5) . ?
C41 C42 1.407(5) . ?
C42 C43 1.392(6) . ?
C42 H42 0.95 . ?
C43 C44 1.385(7) . ?
C43 H43 0.95 . ?
C44 C45 1.370(6) . ?
C44 H44 0.95 . ?
C45 C46 1.408(6) . ?
C45 H45 0.95 . ?
C46 H46 0.95 . ?
C51 C52 1.375(5) . ?
C51 C56 1.406(5) . ?
C52 C53 1.392(6) . ?
C52 H52 0.95 . ?
C53 C54 1.386(6) . ?
C53 H53 0.95 . ?
C54 C55 1.394(6) . ?
C54 H54 0.95 . ?
C55 C56 1.384(6) . ?
C55 H55 0.95 . ?
C56 H56 0.95 . ?

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 98.04(14) . . ?
O1 Re1 N13 92.12(13) . . ?
O21 Re1 N13 89.72(11) . . ?
O1 Re1 O2 173.90(12) . . yes
O21 Re1 O2 82.79(11) . . ?
N13 Re1 O2 81.83(11) . . ?
O1 Re1 Cl1 99.03(10) . . ?
O21 Re1 Cl1 83.62(8) . . ?
N13 Re1 Cl1 167.70(9) . . yes
O2 Re1 Cl1 87.06(7) . . ?
O1 Re1 Cl2 95.70(11) . . ?
O21 Re1 Cl2 164.76(9) . . yes
N13 Re1 Cl2 96.34(8) . . ?
O2 Re1 Cl2 84.24(7) . . ?
Cl1 Re1 Cl2 87.75(3) . . yes
C12 O11 C15 107.8(3) . . ?
N13 C12 O11 115.2(3) . . ?
N13 C12 C26 130.0(3) . . ?
O11 C12 C26 114.8(3) . . ?
C12 N13 C14 108.5(3) . . yes
C12 N13 Re1 122.9(2) . . yes
C14 N13 Re1 128.5(2) . . yes
N13 C14 C16 110.1(3) . . ?
N13 C14 C17 111.3(3) . . ?
C16 C14 C17 112.4(3) . . ?
N13 C14 C15 101.4(3) . . ?
C16 C14 C15 111.1(3) . . ?
C17 C14 C15 109.9(3) . . ?
O11 C15 C14 105.5(3) . . ?
O11 C15 H151 110.6 . . ?
C14 C15 H151 110.6 . . ?
O11 C15 H152 110.6 . . ?
C14 C15 H152 110.6 . . ?
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 129.9(2) . . yes
O21 C21 C26 125.7(3) . . ?
O21 C21 C22 117.3(3) . . ?
C26 C21 C22 117.0(3) . . ?
C23 C22 C21 122.3(4) . . ?
C23 C22 Cl22 119.7(3) . . ?
C21 C22 Cl22 118.0(3) . . ?
C22 C23 C24 118.8(3) . . ?
C22 C23 H23 120.6 . . ?
C24 C23 H23 120.6 . . ?
C25 C24 C23 121.3(4) . . ?
C25 C24 Cl24 119.7(3) . . ?
C23 C24 Cl24 119.0(3) . . ?
C24 C25 C26 119.8(4) . . ?
C24 C25 H25 120.1 . . ?
C26 C25 H25 120.1 . . ?
C21 C26 C25 120.7(3) . . ?
C21 C26 C12 121.6(3) . . ?
C25 C26 C12 117.6(3) . . ?
P1 O2 Re1 159.66(17) . . yes
O2 P1 C31 108.74(16) . . ?
O2 P1 C51 111.67(16) . . ?
C31 P1 C51 105.76(17) . . ?
O2 P1 C41 111.15(16) . . ?
C31 P1 C41 110.15(18) . . ?
C51 P1 C41 109.24(17) . . ?
C36 C31 C32 119.4(3) . . ?
C36 C31 P1 119.7(3) . . ?
C32 C31 P1 120.9(3) . . ?
C33 C32 C31 120.5(4) . . ?
C33 C32 H32 119.7 . . ?
C31 C32 H32 119.7 . . ?
C32 C33 C34 119.3(4) . . ?
C32 C33 H33 120.3 . . ?
C34 C33 H33 120.3 . . ?
C35 C34 C33 120.8(4) . . ?
C35 C34 H34 119.6 . . ?
C33 C34 H34 119.6 . . ?
C34 C35 C36 119.7(4) . . ?
C34 C35 H35 120.1 . . ?
C36 C35 H35 120.1 . . ?
C35 C36 C31 120.2(4) . . ?
C35 C36 H36 119.9 . . ?
C31 C36 H36 119.9 . . ?
C46 C41 C42 120.0(4) . . ?
C46 C41 P1 122.4(3) . . ?
C42 C41 P1 117.6(3) . . ?
C43 C42 C41 119.4(4) . . ?
C43 C42 H42 120.3 . . ?
C41 C42 H42 120.3 . . ?
C44 C43 C42 120.4(4) . . ?
C44 C43 H43 119.8 . . ?
C42 C43 H43 119.8 . . ?
C45 C44 C43 120.4(4) . . ?
C45 C44 H44 119.8 . . ?
C43 C44 H44 119.8 . . ?
C44 C45 C46 120.5(4) . . ?
C44 C45 H45 119.8 . . ?
C46 C45 H45 119.8 . . ?
C41 C46 C45 119.3(4) . . ?
C41 C46 H46 120.4 . . ?
C45 C46 H46 120.4 . . ?
C52 C51 C56 119.0(4) . . ?
C52 C51 P1 118.8(3) . . ?
C56 C51 P1 122.2(3) . . ?
C51 C52 C53 121.3(4) . . ?
C51 C52 H52 119.3 . . ?
C53 C52 H52 119.3 . . ?
C54 C53 C52 119.8(4) . . ?
C54 C53 H53 120.1 . . ?
C52 C53 H53 120.1 . . ?
C53 C54 C55 119.4(4) . . ?
C53 C54 H54 120.3 . . ?
C55 C54 H54 120.3 . . ?
C56 C55 C54 120.6(4) . . ?
C56 C55 H55 119.7 . . ?
C54 C55 H55 119.7 . . ?
C55 C56 C51 119.9(4) . . ?
C55 C56 H56 120.1 . . ?
C51 C56 H56 120.1 . . ?

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 -7.2(5) . . . . ?
C15 O11 C12 C26 172.6(3) . . . . ?
O11 C12 N13 C14 -1.1(4) . . . . ?
C26 C12 N13 C14 179.2(4) . . . . ?
O11 C12 N13 Re1 176.4(2) . . . . ?
C26 C12 N13 Re1 -3.3(6) . . . . ?
C12 N13 C14 C16 -109.5(3) . . . . ?
Re1 N13 C14 C16 73.1(4) . . . . ?
C12 N13 C14 C17 125.0(3) . . . . ?
Re1 N13 C14 C17 -52.3(4) . . . . ?
C12 N13 C14 C15 8.1(4) . . . . ?
Re1 N13 C14 C15 -169.2(3) . . . . ?
C12 O11 C15 C14 11.9(4) . . . . ?
N13 C14 C15 O11 -11.8(4) . . . . ?
C16 C14 C15 O11 105.2(4) . . . . ?
C17 C14 C15 O11 -129.7(4) . . . . ?
Re1 O21 C21 C26 -0.9(6) . . . . ?
Re1 O21 C21 C22 -179.7(3) . . . . ?
O21 C21 C22 C23 179.3(4) . . . . ?
C26 C21 C22 C23 0.4(6) . . . . ?
O21 C21 C22 Cl22 -0.7(5) . . . . ?
C26 C21 C22 Cl22 -179.6(3) . . . . ?
C21 C22 C23 C24 1.2(6) . . . . ?
Cl22 C22 C23 C24 -178.7(3) . . . . ?
C22 C23 C24 C25 -1.6(6) . . . . ?
C22 C23 C24 Cl24 176.9(3) . . . . ?
C23 C24 C25 C26 0.3(6) . . . . ?
Cl24 C24 C25 C26 -178.2(3) . . . . ?
O21 C21 C26 C25 179.5(4) . . . . ?
C22 C21 C26 C25 -1.8(5) . . . . ?
O21 C21 C26 C12 2.0(6) . . . . ?
C22 C21 C26 C12 -179.2(3) . . . . ?
C24 C25 C26 C21 1.4(6) . . . . ?
C24 C25 C26 C12 179.0(4) . . . . ?
N13 C12 C26 C21 0.4(6) . . . . ?
O11 C12 C26 C21 -179.4(3) . . . . ?
N13 C12 C26 C25 -177.1(4) . . . . ?
O11 C12 C26 C25 3.1(5) . . . . ?
Re1 O2 P1 C31 -179.9(5) . . . . ?
Re1 O2 P1 C51 63.7(5) . . . . ?
Re1 O2 P1 C41 -58.5(5) . . . . ?
O2 P1 C31 C36 10.2(4) . . . . ?
C51 P1 C31 C36 130.2(3) . . . . ?
C41 P1 C31 C36 -111.8(3) . . . . ?
O2 P1 C31 C32 -167.5(3) . . . . ?
C51 P1 C31 C32 -47.5(4) . . . . ?
C41 P1 C31 C32 70.4(4) . . . . ?
C36 C31 C32 C33 2.5(6) . . . . ?
P1 C31 C32 C33 -179.8(3) . . . . ?
C31 C32 C33 C34 -2.1(6) . . . . ?
C32 C33 C34 C35 0.6(7) . . . . ?
C33 C34 C35 C36 0.6(6) . . . . ?
C34 C35 C36 C31 -0.2(6) . . . . ?
C32 C31 C36 C35 -1.3(6) . . . . ?
P1 C31 C36 C35 -179.0(3) . . . . ?
O2 P1 C41 C46 -137.0(3) . . . . ?
C31 P1 C41 C46 -16.4(4) . . . . ?
C51 P1 C41 C46 99.4(3) . . . . ?
O2 P1 C41 C42 43.1(3) . . . . ?
C31 P1 C41 C42 163.7(3) . . . . ?
C51 P1 C41 C42 -80.5(3) . . . . ?
C46 C41 C42 C43 0.2(6) . . . . ?
P1 C41 C42 C43 -179.9(3) . . . . ?
C41 C42 C43 C44 1.0(7) . . . . ?
C42 C43 C44 C45 -1.4(7) . . . . ?
C43 C44 C45 C46 0.7(7) . . . . ?
C42 C41 C46 C45 -0.9(6) . . . . ?
P1 C41 C46 C45 179.2(3) . . . . ?
C44 C45 C46 C41 0.5(6) . . . . ?
O2 P1 C51 C52 58.5(3) . . . . ?
C31 P1 C51 C52 -59.6(3) . . . . ?
C41 P1 C51 C52 -178.1(3) . . . . ?
O2 P1 C51 C56 -120.5(3) . . . . ?
C31 P1 C51 C56 121.3(3) . . . . ?
C41 P1 C51 C56 2.8(4) . . . . ?
C56 C51 C52 C53 1.4(6) . . . . ?
P1 C51 C52 C53 -177.7(3) . . . . ?
C51 C52 C53 C54 -1.7(7) . . . . ?
C52 C53 C54 C55 0.8(7) . . . . ?
C53 C54 C55 C56 0.3(7) . . . . ?
C54 C55 C56 C51 -0.6(6) . . . . ?
C52 C51 C56 C55 -0.3(6) . . . . ?
P1 C51 C56 C55 178.8(3) . . . . ?

_refine_diff_density_max         1.982
_refine_diff_density_min         -1.204
_refine_diff_density_rms         0.148

_shelxl_version_number           2014/6

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_JSJZ15
_database_code_depnum_ccdc_archive 'CCDC 1913789'
loop_
_audit_author_name
_audit_author_address
'Ferdinand Belaj'
;University of Graz
Austria
;
_audit_update_record             
;
2019-05-03 deposited with the CCDC.	2024-12-12 downloaded from the CCDC.
;
_audit_creation_method           'manual edited SHELXL-2014/6.cif file'

_chemical_compound_source        'synthetical product'

_chemical_name_systematic        
; 2,4-dichloro-6-(4,4-dimethyl-4,5-dihydro-1,3-oxazol-2-yl)phenol
;
_chemical_name_common            
; 2,4-dichloro-6-(4,4-dimethyl-4,5-dihydro-1,3-oxazol-2-yl)phenol
;
_chemical_melting_point          ?
_chemical_formula_moiety         'C11 H11 Cl2 N O2'
_chemical_formula_sum            'C11 H11 Cl2 N O2'
_chemical_formula_weight         260.11

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_H-M_alt        'C c'
_space_group_name_Hall           'C -2yc'

_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.
;

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'

_cell_length_a                   7.4471(9)
_cell_length_b                   23.852(4)
_cell_length_c                   6.8468(8)
_cell_angle_alpha                90
_cell_angle_beta                 107.136(7)
_cell_angle_gamma                90
_cell_volume                     1162.2(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4813
_cell_measurement_theta_min      2.99
_cell_measurement_theta_max      28.73

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.487
_exptl_crystal_F_000             536
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    0.542
_shelx_estimated_absorpt_T_min   0.829
_shelx_estimated_absorpt_T_max   0.984
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.613
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
'Bruker (2001). SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.'

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_source         'Incoatec microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  'multilayer monochromator'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            17577
_diffrn_reflns_av_unetI/netI     0.0675
_diffrn_reflns_av_R_equivalents  0.0857
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.99
_diffrn_reflns_theta_max         29.99
_diffrn_reflns_theta_full        30.00
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             3384
_reflns_number_gt                2846
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.991
_reflns_Friedel_fraction_max     0.999
_reflns_Friedel_fraction_full    0.999

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2015)'
_computing_molecular_graphics    'modified ORTEP (Johnson, 1965)'
_computing_publication_material  'SHELXL-2014/6 (Sheldrick, 2015)'

_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.
 
 The absolute configuration was established by anomalous dispersion effects in
 the diffraction measurements on the crystal.
 
 The non-hydrogen atoms were refined with anisotropic displacement parameters
 without any constraints.
 
 The position of the H atom of the OH group was taken from a difference
 Fourier map, the O-H distance was fixed to 0.84 Å, and the H atom was
 refined with an individual isotropic displacement parameter without any
 constraints to the bond angles (DFIX of SHELXL).
 
 The H atoms of the CH₂ group were refined with common isotropic
 displacement parameters and idealized geometry with approximately
 tetrahedral angles and C-H distances of 0.99 Å (AFIX 23 of SHELXL).
 
 The H atoms of the phenyl ring were put at the external bisectors of the
 C-C-C angles at C-H distances of 0.95 Å and a common isotropic displacement
 parameter was refined for these H atoms (AFIX 43 of SHELXL).
 
 The H atoms of the methyl groups were refined with common isotropic
 displacement parameters for the H atoms of the same group and idealized
 geometries with tetrahedral angles, enabling rotations around the C-C bonds,
 and C-H distances of 0.98 Å (AFIX 137 of SHELXL).
;

# start Validation Reply Form
_vrf_PLAT172_JSJZ15              
;
PROBLEM: The CIF-Embedded .res File Contains DFIX Records ....... 1 Report
RESPONSE:
 The position of the H atom of the OH group was taken from a difference
 Fourier map, the O-H distance was fixed to 0.84A, and the H atom was
 refined with an individual isotropic displacement parameter without any
 constraints to the bond angles (DFIX of SHELXL).
 The non-hydrogen atoms were refined with anisotropic displacement parameters
 without any constraints.
;
# end Validation Reply Form

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0257P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    refU
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 
;
 Flack x determined using 1228 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.03(5)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         3384
_refine_ls_number_parameters     155
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0505
_refine_ls_R_factor_gt           0.0365
_refine_ls_wR_factor_ref         0.0762
_refine_ls_wR_factor_gt          0.0713
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_restrained_S_all      1.008
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
O11 O 0.8783(4) 0.59340(9) 0.6223(5) 0.0218(5) Uani 1 1 d . . . . .
C12 C 0.7050(5) 0.61298(14) 0.5225(5) 0.0163(6) Uani 1 1 d . . . . .
N13 N 0.6813(4) 0.66574(11) 0.5083(5) 0.0192(6) Uani 1 1 d . . . . .
C14 C 0.8611(5) 0.69260(13) 0.6287(6) 0.0200(6) Uani 1 1 d . . . . .
C15 C 0.9979(6) 0.64295(13) 0.6658(6) 0.0233(6) Uani 1 1 d . . . . .
H151 H 1.0780 0.6449 0.5735 0.031(7) Uiso 1 1 calc R U . . .
H152 H 1.0795 0.6426 0.8090 0.031(7) Uiso 1 1 calc R U . . .
C16 C 0.8351(6) 0.71422(15) 0.8286(6) 0.0269(7) Uani 1 1 d . . . . .
H161 H 0.7377 0.7433 0.7988 0.041(6) Uiso 1 1 calc R U . . .
H162 H 0.9537 0.7301 0.9138 0.041(6) Uiso 1 1 calc R U . . .
H163 H 0.7971 0.6832 0.9016 0.041(6) Uiso 1 1 calc R U . . .
C17 C 0.9151(5) 0.73938(15) 0.5063(6) 0.0305(8) Uani 1 1 d . . . . .
H171 H 0.9265 0.7242 0.3774 0.035(6) Uiso 1 1 calc R U . . .
H172 H 1.0355 0.7556 0.5852 0.035(6) Uiso 1 1 calc R U . . .
H173 H 0.8179 0.7685 0.4772 0.035(6) Uiso 1 1 calc R U . . .
O21 O 0.32681(2) 0.64586(9) 0.33599(2) 0.0219(5) Uani 1 1 d D . . . .
H21 H 0.4186(9) 0.6657(3) 0.400(2) 0.062(15) Uiso 1 1 d D . . . .
C21 C 0.3715(5) 0.59158(14) 0.3558(5) 0.0146(6) Uani 1 1 d . . . . .
C22 C 0.5559(5) 0.57147(13) 0.4429(5) 0.0153(6) Uani 1 1 d . . . . .
C23 C 0.5936(5) 0.51418(14) 0.4592(5) 0.0177(7) Uani 1 1 d . . . . .
H23 H 0.7184 0.5011 0.5176 0.027(7) Uiso 1 1 calc R U . . .
C24 C 0.4483(5) 0.47671(14) 0.3898(6) 0.0176(6) Uani 1 1 d . . . . .
C25 C 0.2648(5) 0.49450(14) 0.3024(5) 0.0177(6) Uani 1 1 d . . . . .
H25 H 0.1659 0.4681 0.2548 0.027(7) Uiso 1 1 calc R U . . .
C26 C 0.2292(5) 0.55124(14) 0.2863(5) 0.0165(6) Uani 1 1 d . . . . .
Cl24 Cl 0.4959(3) 0.40493(3) 0.4123(3) 0.02213(17) Uani 1 1 d . . . . .
Cl26 Cl 0.0013(3) 0.57500(4) 0.1728(4) 0.02665(19) Uani 1 1 d . . . . .


_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_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O11 C12 1.353(4) . ?
O11 C15 1.457(4) . ?
C12 N13 1.270(4) . ?
C12 C22 1.467(4) . ?
N13 C14 1.494(4) . ?
C14 C17 1.519(4) . ?
C14 C16 1.528(4) . ?
C14 C15 1.533(5) . ?
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 1.334(4) . ?
O21 H21 0.84 . ?
C21 C26 1.406(4) . ?
C21 C22 1.411(4) . ?
C22 C23 1.393(4) . ?
C23 C24 1.375(4) . ?
C23 H23 0.95 . ?
C24 C25 1.387(4) . ?
C24 Cl24 1.746(3) . ?
C25 C26 1.377(5) . ?
C25 H25 0.95 . ?
C26 Cl26 1.740(3) . ?

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
C12 O11 C15 104.9(3) . . ?
N13 C12 O11 118.1(3) . . ?
N13 C12 C22 124.6(3) . . ?
O11 C12 C22 117.3(3) . . ?
C12 N13 C14 107.5(3) . . ?
N13 C14 C17 110.5(3) . . ?
N13 C14 C16 108.0(2) . . ?
C17 C14 C16 111.8(3) . . ?
N13 C14 C15 101.7(3) . . ?
C17 C14 C15 112.8(3) . . ?
C16 C14 C15 111.5(3) . . ?
O11 C15 C14 104.9(3) . . ?
O11 C15 H151 110.8 . . ?
C14 C15 H151 110.8 . . ?
O11 C15 H152 110.8 . . ?
C14 C15 H152 110.8 . . ?
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 H21 110.6(7) . . ?
O21 C21 C26 119.3(3) . . ?
O21 C21 C22 123.8(3) . . ?
C26 C21 C22 116.9(3) . . ?
C23 C22 C21 121.0(3) . . ?
C23 C22 C12 121.3(3) . . ?
C21 C22 C12 117.6(3) . . ?
C24 C23 C22 119.4(3) . . ?
C24 C23 H23 120.3 . . ?
C22 C23 H23 120.3 . . ?
C23 C24 C25 121.7(3) . . ?
C23 C24 Cl24 119.2(2) . . ?
C25 C24 Cl24 119.1(2) . . ?
C26 C25 C24 118.5(3) . . ?
C26 C25 H25 120.7 . . ?
C24 C25 H25 120.7 . . ?
C25 C26 C21 122.5(3) . . ?
C25 C26 Cl26 119.7(2) . . ?
C21 C26 Cl26 117.8(2) . . ?

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 -6.7(3) . . . . ?
C15 O11 C12 C22 174.9(2) . . . . ?
O11 C12 N13 C14 -4.7(3) . . . . ?
C22 C12 N13 C14 173.6(2) . . . . ?
C12 N13 C14 C17 133.2(3) . . . . ?
C12 N13 C14 C16 -104.3(3) . . . . ?
C12 N13 C14 C15 13.1(3) . . . . ?
C12 O11 C15 C14 14.5(3) . . . . ?
N13 C14 C15 O11 -16.5(3) . . . . ?
C17 C14 C15 O11 -134.9(3) . . . . ?
C16 C14 C15 O11 98.4(3) . . . . ?
O21 C21 C22 C23 -179.9(2) . . . . ?
C26 C21 C22 C23 -0.2(4) . . . . ?
O21 C21 C22 C12 2.3(4) . . . . ?
C26 C21 C22 C12 -178.0(2) . . . . ?
N13 C12 C22 C23 178.2(3) . . . . ?
O11 C12 C22 C23 -3.6(4) . . . . ?
N13 C12 C22 C21 -4.1(4) . . . . ?
O11 C12 C22 C21 174.2(2) . . . . ?
C21 C22 C23 C24 -0.2(4) . . . . ?
C12 C22 C23 C24 177.4(3) . . . . ?
C22 C23 C24 C25 0.5(4) . . . . ?
C22 C23 C24 Cl24 -179.5(2) . . . . ?
C23 C24 C25 C26 -0.2(4) . . . . ?
Cl24 C24 C25 C26 179.77(19) . . . . ?
C24 C25 C26 C21 -0.3(4) . . . . ?
C24 C25 C26 Cl26 178.7(2) . . . . ?
O21 C21 C26 C25 -179.8(2) . . . . ?
C22 C21 C26 C25 0.5(4) . . . . ?
O21 C21 C26 Cl26 1.2(3) . . . . ?
C22 C21 C26 Cl26 -178.5(2) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O21 H21 N13 0.84 1.877(6) 2.598(3) 143.1(9) .

_refine_diff_density_max         0.277
_refine_diff_density_min         -0.258
_refine_diff_density_rms         0.057

_shelxl_version_number           2014/6

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_JSJZ2B
_database_code_depnum_ccdc_archive 'CCDC 1913787'
loop_
_audit_author_name
_audit_author_address
'Ferdinand Belaj'
;University of Graz
Austria
;
_audit_update_record             
;
2019-05-03 deposited with the CCDC.	2024-12-12 downloaded from the CCDC.
;
_audit_creation_method           'manual edited SHELXL-2014/6.cif file'

_chemical_compound_source        'synthetical product'

_chemical_name_systematic        
chloro-bis[2-(4,4-dimethyl-4,5-dihydro-1,3-oxazol-2-yl)-4,6-dichlo-rophenolato-N,O]-oxo-rhenium(V)
_chemical_name_common            
chloro-bis[2-(4,4-dimethyl-4,5-dihydro-1,3-oxazol-2-yl)-4,6-dichlo-rophenolato-N,O]-oxo-rhenium(V)
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H20 Cl5 N2 O5 Re'
_chemical_formula_sum            'C22 H20 Cl5 N2 O5 Re'
_chemical_formula_weight         755.85

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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.
;

loop_
_space_group_symop_operation_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'

_cell_length_a                   11.0483(15)
_cell_length_b                   12.4028(17)
_cell_length_c                   37.115(5)
_cell_angle_alpha                90
_cell_angle_beta                 93.108(6)
_cell_angle_gamma                90
_cell_volume                     5078.4(12)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9774
_cell_measurement_theta_min      2.47
_cell_measurement_theta_max      26.84

_exptl_crystal_description       plate
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.977
_exptl_crystal_F_000             2928
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.270
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    5.349
_shelx_estimated_absorpt_T_min   0.288
_shelx_estimated_absorpt_T_max   0.814
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.640
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
'Bruker (2001). SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.'

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_source         'Incoatec microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  'multilayer monochromator'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            25840
_diffrn_reflns_av_unetI/netI     0.0676
_diffrn_reflns_av_R_equivalents  0.0378
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_theta_min         1.73
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             9991
_reflns_number_gt                7907
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     ?
_reflns_Friedel_fraction_full    ?

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2015)'
_computing_molecular_graphics    'modified ORTEP (Johnson, 1965)'
_computing_publication_material  'SHELXL-2014/6 (Sheldrick, 2015)'

_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.
 
 The non-hydrogen atoms were refined with anisotropic displacement parameters
 without any constraints.
 
 The H atoms of the CH₂ groups were refined with common isotropic
 displacement parameters for the H atoms of the same group and idealized
 geometries with approximately tetrahedral angles and C-H distances of 0.99 Å
 (AFIX 23 of SHELXL).
 
 The H atoms of the phenyl rings were put at the external bisectors of the
 C-C-C angles at C-H distances of 0.95 Å and common isotropic displacement
 parameters were refined for the H atoms of the same ring
 (AFIX 43 of SHELXL).
 
 The H atoms of the methyl groups were refined with common isotropic
 displacement parameters for the H atoms of the same group and idealized
 geometries with tetrahedral angles, enabling rotation around the C-C bonds,
 and C-H distances of 0.98 Å (AFIX 137 of SHELXL).
 
 The largest peaks in a final difference Fourier map (1.79 eÅ⁻³)
 was in the vicinity (0.69 Å) of a Re atom.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0650P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    refU
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9991
_refine_ls_number_parameters     655
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0546
_refine_ls_R_factor_gt           0.0447
_refine_ls_wR_factor_ref         0.1147
_refine_ls_wR_factor_gt          0.1110
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_restrained_S_all      1.007
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

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 0.71574(2) 0.50673(2) 0.32497(2) 0.01524(10) Uani 1 1 d . . . . .
O1 O 0.6515(4) 0.4261(4) 0.29218(12) 0.0234(11) Uani 1 1 d . . . . .
Cl1 Cl 0.75692(14) 0.65327(14) 0.28539(5) 0.0249(4) Uani 1 1 d . . . . .
O11 O 1.0902(4) 0.4199(4) 0.33725(12) 0.0207(11) Uani 1 1 d . . . . .
C12 C 0.9847(5) 0.4639(5) 0.34490(18) 0.0196(15) Uani 1 1 d . . . . .
N13 N 0.8961(4) 0.4559(4) 0.32027(14) 0.0184(13) Uani 1 1 d . . . . .
C14 C 0.9397(6) 0.3787(6) 0.29181(18) 0.0227(16) Uani 1 1 d . . . . .
C15 C 1.0754(6) 0.3906(6) 0.29876(17) 0.0246(17) Uani 1 1 d . . . . .
H151 H 1.1176 0.3221 0.2940 0.029(14) Uiso 1 1 calc R U . . .
H152 H 1.1077 0.4479 0.2834 0.029(14) Uiso 1 1 calc R U . . .
C16 C 0.9008(6) 0.4159(6) 0.25384(18) 0.0254(17) Uani 1 1 d . . . . .
H161 H 0.9517 0.3810 0.2364 0.027(11) Uiso 1 1 calc R U . . .
H162 H 0.9099 0.4943 0.2522 0.027(11) Uiso 1 1 calc R U . . .
H163 H 0.8158 0.3963 0.2484 0.027(11) Uiso 1 1 calc R U . . .
C17 C 0.8924(6) 0.2685(6) 0.29969(19) 0.0265(17) Uani 1 1 d . . . . .
H171 H 0.8053 0.2656 0.2931 0.033(12) Uiso 1 1 calc R U . . .
H172 H 0.9060 0.2530 0.3255 0.033(12) Uiso 1 1 calc R U . . .
H173 H 0.9348 0.2149 0.2856 0.033(12) Uiso 1 1 calc R U . . .
O21 O 0.7918(4) 0.5973(4) 0.36520(12) 0.0215(11) Uani 1 1 d . . . . .
C21 C 0.8815(5) 0.5779(5) 0.38906(17) 0.0178(15) Uani 1 1 d . . . . .
C22 C 0.9804(6) 0.5136(5) 0.38052(19) 0.0201(15) Uani 1 1 d . . . . .
C23 C 1.0772(6) 0.4972(5) 0.40618(18) 0.0192(16) Uani 1 1 d . . . . .
H23 H 1.1452 0.4552 0.4002 0.028(14) Uiso 1 1 calc R U . . .
C24 C 1.0726(6) 0.5421(5) 0.43966(18) 0.0196(15) Uani 1 1 d . . . . .
C25 C 0.9758(5) 0.6052(5) 0.44931(17) 0.0193(15) Uani 1 1 d . . . . .
H25 H 0.9738 0.6352 0.4728 0.028(14) Uiso 1 1 calc R U . . .
C26 C 0.8833(6) 0.6230(5) 0.42398(18) 0.0223(16) Uani 1 1 d . . . . .
Cl24 Cl 1.19094(17) 0.51760(16) 0.47242(5) 0.0331(5) Uani 1 1 d . . . . .
Cl26 Cl 0.75988(16) 0.70258(15) 0.43499(5) 0.0308(4) Uani 1 1 d . . . . .
O31 O 0.4039(4) 0.5780(4) 0.38250(12) 0.0212(11) Uani 1 1 d . . . . .
C32 C 0.5103(6) 0.5326(5) 0.37458(18) 0.0195(15) Uani 1 1 d . . . . .
N33 N 0.5520(4) 0.5624(5) 0.34411(15) 0.0207(13) Uani 1 1 d . . . . .
C34 C 0.4679(6) 0.6490(5) 0.32790(18) 0.0215(16) Uani 1 1 d . . . . .
C35 C 0.3570(6) 0.6318(6) 0.35067(18) 0.0255(17) Uani 1 1 d . . . . .
H351 H 0.3200 0.7017 0.3568 0.026(13) Uiso 1 1 calc R U . . .
H352 H 0.2951 0.5869 0.3375 0.026(13) Uiso 1 1 calc R U . . .
C36 C 0.4383(6) 0.6326(5) 0.28856(17) 0.0208(15) Uani 1 1 d . . . . .
H361 H 0.3966 0.5634 0.2848 0.033(12) Uiso 1 1 calc R U . . .
H362 H 0.5133 0.6324 0.2756 0.033(12) Uiso 1 1 calc R U . . .
H363 H 0.3856 0.6911 0.2794 0.033(12) Uiso 1 1 calc R U . . .
C37 C 0.5281(5) 0.7595(5) 0.33579(19) 0.0237(16) Uani 1 1 d . . . . .
H371 H 0.6067 0.7622 0.3248 0.026(11) Uiso 1 1 calc R U . . .
H372 H 0.5399 0.7696 0.3619 0.026(11) Uiso 1 1 calc R U . . .
H373 H 0.4757 0.8170 0.3256 0.026(11) Uiso 1 1 calc R U . . .
O41 O 0.7178(4) 0.3908(3) 0.36270(11) 0.0194(10) Uani 1 1 d . . . . .
C41 C 0.6608(6) 0.3902(5) 0.39345(17) 0.0188(15) Uani 1 1 d . . . . .
C42 C 0.5622(6) 0.4565(5) 0.40082(17) 0.0173(14) Uani 1 1 d . . . . .
C43 C 0.5096(6) 0.4483(5) 0.43450(18) 0.0201(15) Uani 1 1 d . . . . .
H43 H 0.4424 0.4925 0.4395 0.033(15) Uiso 1 1 calc R U . . .
C44 C 0.5545(6) 0.3775(5) 0.45986(18) 0.0233(16) Uani 1 1 d . . . . .
C45 C 0.6546(6) 0.3125(5) 0.45294(18) 0.0212(15) Uani 1 1 d . . . . .
H45 H 0.6854 0.2641 0.4711 0.033(15) Uiso 1 1 calc R U . . .
C46 C 0.7082(5) 0.3171(5) 0.42098(18) 0.0189(15) Uani 1 1 d . . . . .
Cl44 Cl 0.48655(16) 0.36248(15) 0.50087(5) 0.0295(4) Uani 1 1 d . . . . .
Cl46 Cl 0.82763(15) 0.23975(15) 0.41130(5) 0.0301(4) Uani 1 1 d . . . . .
Re2 Re 0.78254(2) 0.96933(2) 0.66915(2) 0.01446(9) Uani 1 1 d . . . . .
O2 O 0.8464(4) 0.8802(4) 0.69892(12) 0.0241(11) Uani 1 1 d . . . . .
Cl2 Cl 0.73519(14) 1.09779(14) 0.71504(4) 0.0257(4) Uani 1 1 d . . . . .
O51 O 0.4099(4) 0.8792(4) 0.65095(12) 0.0284(12) Uani 1 1 d . . . . .
C52 C 0.5140(6) 0.9293(5) 0.64571(18) 0.0194(15) Uani 1 1 d . . . . .
N53 N 0.6033(5) 0.9118(5) 0.67025(14) 0.0225(13) Uani 1 1 d . . . . .
C54 C 0.5608(6) 0.8184(6) 0.69333(18) 0.0237(16) Uani 1 1 d . . . . .
C55 C 0.4264(6) 0.8266(6) 0.68592(18) 0.0239(16) Uani 1 1 d . . . . .
H551 H 0.3890 0.7541 0.6852 0.026(13) Uiso 1 1 calc R U . . .
H552 H 0.3892 0.8698 0.7048 0.026(13) Uiso 1 1 calc R U . . .
C56 C 0.6008(6) 0.8297(6) 0.73284(17) 0.0279(18) Uani 1 1 d . . . . .
H561 H 0.6019 0.9061 0.7395 0.031(11) Uiso 1 1 calc R U . . .
H562 H 0.6822 0.7993 0.7370 0.031(11) Uiso 1 1 calc R U . . .
H563 H 0.5440 0.7909 0.7476 0.031(11) Uiso 1 1 calc R U . . .
C57 C 0.6088(6) 0.7137(6) 0.6766(2) 0.0317(18) Uani 1 1 d . . . . .
H571 H 0.5811 0.6514 0.6902 0.042(13) Uiso 1 1 calc R U . . .
H572 H 0.6976 0.7152 0.6777 0.042(13) Uiso 1 1 calc R U . . .
H573 H 0.5781 0.7082 0.6514 0.042(13) Uiso 1 1 calc R U . . .
O61 O 0.7075(4) 1.0759(3) 0.63368(12) 0.0189(10) Uani 1 1 d . . . . .
C61 C 0.6173(5) 1.0644(5) 0.60840(17) 0.0169(14) Uani 1 1 d . . . . .
C62 C 0.5212(6) 0.9955(5) 0.61394(19) 0.0205(16) Uani 1 1 d . . . . .
C63 C 0.4232(6) 0.9881(5) 0.58711(19) 0.0212(16) Uani 1 1 d . . . . .
H63 H 0.3532 0.9465 0.5913 0.041(16) Uiso 1 1 calc R U . . .
C64 C 0.4329(6) 1.0418(6) 0.55561(19) 0.0265(17) Uani 1 1 d . . . . .
C65 C 0.5277(6) 1.1101(6) 0.54912(19) 0.0282(17) Uani 1 1 d . . . . .
H65 H 0.5297 1.1488 0.5271 0.041(16) Uiso 1 1 calc R U . . .
C66 C 0.6207(6) 1.1208(5) 0.57589(18) 0.0230(16) Uani 1 1 d . . . . .
Cl64 Cl 0.31506(16) 1.03020(15) 0.52164(5) 0.0316(4) Uani 1 1 d . . . . .
Cl66 Cl 0.74268(15) 1.20457(15) 0.56867(5) 0.0281(4) Uani 1 1 d . . . . .
O71 O 1.0927(4) 1.0684(4) 0.61593(12) 0.0213(11) Uani 1 1 d . . . . .
C72 C 0.9901(6) 1.0165(5) 0.62220(19) 0.0195(16) Uani 1 1 d . . . . .
N73 N 0.9443(5) 1.0351(4) 0.65399(16) 0.0233(14) Uani 1 1 d . . . . .
C74 C 1.0234(5) 1.1239(5) 0.67194(17) 0.0174(15) Uani 1 1 d . . . . .
C75 C 1.1368(6) 1.1196(6) 0.64976(18) 0.0244(17) Uani 1 1 d . . . . .
H751 H 1.1683 1.1929 0.6454 0.039(15) Uiso 1 1 calc R U . . .
H752 H 1.2016 1.0760 0.6622 0.039(15) Uiso 1 1 calc R U . . .
C76 C 1.0536(5) 1.0941(6) 0.71070(17) 0.0218(16) Uani 1 1 d . . . . .
H761 H 0.9785 1.0860 0.7233 0.029(11) Uiso 1 1 calc R U . . .
H762 H 1.1034 1.1510 0.7223 0.029(11) Uiso 1 1 calc R U . . .
H763 H 1.0985 1.0260 0.7117 0.029(11) Uiso 1 1 calc R U . . .
C77 C 0.9564(6) 1.2299(5) 0.66793(18) 0.0208(15) Uani 1 1 d . . . . .
H771 H 0.8821 1.2266 0.6812 0.027(11) Uiso 1 1 calc R U . . .
H772 H 0.9354 1.2434 0.6423 0.027(11) Uiso 1 1 calc R U . . .
H773 H 1.0081 1.2883 0.6777 0.027(11) Uiso 1 1 calc R U . . .
O81 O 0.7813(4) 0.8719(4) 0.62672(12) 0.0208(11) Uani 1 1 d . . . . .
C81 C 0.8467(5) 0.8762(5) 0.59801(18) 0.0176(15) Uani 1 1 d . . . . .
C82 C 0.9454(6) 0.9445(5) 0.59347(18) 0.0203(15) Uani 1 1 d . . . . .
C83 C 1.0070(6) 0.9419(5) 0.56131(18) 0.0198(15) Uani 1 1 d . . . . .
H83 H 1.0735 0.9890 0.5582 0.025(14) Uiso 1 1 calc R U . . .
C84 C 0.9710(5) 0.8719(5) 0.53461(18) 0.0193(15) Uani 1 1 d . . . . .
C85 C 0.8688(5) 0.8061(5) 0.53778(18) 0.0216(16) Uani 1 1 d . . . . .
H85 H 0.8417 0.7603 0.5185 0.025(14) Uiso 1 1 calc R U . . .
C86 C 0.8096(5) 0.8087(5) 0.56852(18) 0.0174(15) Uani 1 1 d . . . . .
Cl84 Cl 1.05463(15) 0.85862(15) 0.49644(5) 0.0275(4) Uani 1 1 d . . . . .
Cl86 Cl 0.68415(15) 0.72904(16) 0.57387(5) 0.0326(5) Uani 1 1 d . . . . .


_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_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Re1 O1 1.700(5) . yes
Re1 O21 2.016(4) . yes
Re1 O41 2.006(4) . yes
Re1 N13 2.106(5) . yes
Re1 N33 2.096(5) . yes
Re1 Cl1 2.3960(17) . yes
O11 C12 1.330(7) . ?
O11 C15 1.474(7) . ?
C12 N13 1.307(8) . ?
C12 C22 1.462(9) . ?
N13 C14 1.523(8) . ?
C14 C17 1.497(9) . ?
C14 C15 1.514(9) . ?
C14 C16 1.522(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 1.314(7) . ?
C21 C22 1.403(9) . ?
C21 C26 1.411(9) . ?
C22 C23 1.408(9) . ?
C23 C24 1.365(9) . ?
C23 H23 0.95 . ?
C24 C25 1.388(9) . ?
C24 Cl24 1.763(7) . ?
C25 C26 1.368(9) . ?
C25 H25 0.95 . ?
C26 Cl26 1.749(6) . ?
O31 C32 1.350(7) . ?
O31 C35 1.430(8) . ?
C32 N33 1.298(8) . ?
C32 C42 1.451(9) . ?
N33 C34 1.523(8) . ?
C34 C36 1.493(9) . ?
C34 C35 1.541(9) . ?
C34 C37 1.544(9) . ?
C35 H351 0.99 . ?
C35 H352 0.99 . ?
C36 H361 0.98 . ?
C36 H362 0.98 . ?
C36 H363 0.98 . ?
C37 H371 0.98 . ?
C37 H372 0.98 . ?
C37 H373 0.98 . ?
O41 C41 1.333(7) . ?
C41 C42 1.404(9) . ?
C41 C46 1.443(9) . ?
C42 C43 1.410(9) . ?
C43 C44 1.361(9) . ?
C43 H43 0.95 . ?
C44 C45 1.404(9) . ?
C44 Cl44 1.743(7) . ?
C45 C46 1.356(9) . ?
C45 H45 0.95 . ?
C46 Cl46 1.686(7) . ?
Re2 O2 1.690(5) . yes
Re2 O61 2.012(4) . yes
Re2 O81 1.985(4) . yes
Re2 N53 2.107(5) . yes
Re2 N73 2.070(5) . yes
Re2 Cl2 2.4103(17) . yes
O51 C52 1.331(8) . ?
O51 C55 1.455(8) . ?
C52 N53 1.324(8) . ?
C52 C62 1.443(9) . ?
N53 C54 1.530(8) . ?
C54 C55 1.499(9) . ?
C54 C56 1.515(9) . ?
C54 C57 1.545(10) . ?
C55 H551 0.99 . ?
C55 H552 0.99 . ?
C56 H561 0.98 . ?
C56 H562 0.98 . ?
C56 H563 0.98 . ?
C57 H571 0.98 . ?
C57 H572 0.98 . ?
C57 H573 0.98 . ?
O61 C61 1.339(8) . ?
C61 C62 1.386(9) . ?
C61 C66 1.397(9) . ?
C62 C63 1.434(10) . ?
C63 C64 1.355(10) . ?
C63 H63 0.95 . ?
C64 C65 1.379(10) . ?
C64 Cl64 1.768(7) . ?
C65 C66 1.397(10) . ?
C65 H65 0.95 . ?
C66 Cl66 1.734(7) . ?
O71 C72 1.334(7) . ?
O71 C75 1.467(8) . ?
C72 N73 1.329(9) . ?
C72 C82 1.457(9) . ?
N73 C74 1.536(8) . ?
C74 C76 1.505(9) . ?
C74 C77 1.512(9) . ?
C74 C75 1.537(9) . ?
C75 H751 0.99 . ?
C75 H752 0.99 . ?
C76 H761 0.98 . ?
C76 H762 0.98 . ?
C76 H763 0.98 . ?
C77 H771 0.98 . ?
C77 H772 0.98 . ?
C77 H773 0.98 . ?
O81 C81 1.321(7) . ?
C81 C82 1.398(9) . ?
C81 C86 1.421(9) . ?
C82 C83 1.406(9) . ?
C83 C84 1.361(9) . ?
C83 H83 0.95 . ?
C84 C85 1.404(9) . ?
C84 Cl84 1.740(6) . ?
C85 C86 1.346(9) . ?
C85 H85 0.95 . ?
C86 Cl86 1.722(6) . ?

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 O41 93.8(2) . . ?
O1 Re1 O21 177.7(2) . . yes
O41 Re1 O21 83.90(18) . . ?
O1 Re1 N33 95.8(2) . . ?
O41 Re1 N33 88.67(19) . . ?
O21 Re1 N33 84.16(19) . . ?
O1 Re1 N13 97.2(2) . . ?
O41 Re1 N13 82.43(19) . . ?
O21 Re1 N13 82.52(18) . . ?
N13 Re1 N33 164.7(2) . . yes
O1 Re1 Cl1 95.34(16) . . ?
O41 Re1 Cl1 167.46(13) . . yes
O21 Re1 Cl1 86.90(13) . . ?
N33 Re1 Cl1 98.86(16) . . ?
N13 Re1 Cl1 87.96(16) . . ?
C12 O11 C15 104.8(5) . . ?
N13 C12 O11 116.8(6) . . ?
N13 C12 C22 127.2(6) . . ?
O11 C12 C22 116.0(5) . . ?
C12 N13 C14 106.2(5) . . yes
C12 N13 Re1 126.6(4) . . yes
C14 N13 Re1 125.6(4) . . yes
C17 C14 C15 114.1(6) . . ?
C17 C14 C16 111.9(6) . . ?
C15 C14 C16 110.8(5) . . ?
C17 C14 N13 108.1(5) . . ?
C15 C14 N13 99.6(5) . . ?
C16 C14 N13 111.5(6) . . ?
O11 C15 C14 104.2(5) . . ?
O11 C15 H151 110.9 . . ?
C14 C15 H151 110.9 . . ?
O11 C15 H152 110.9 . . ?
C14 C15 H152 110.9 . . ?
H151 C15 H152 108.9 . . ?
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 131.8(4) . . yes
O21 C21 C22 121.3(6) . . ?
O21 C21 C26 121.3(5) . . ?
C22 C21 C26 117.4(6) . . ?
C21 C22 C23 120.1(6) . . ?
C21 C22 C12 120.6(6) . . ?
C23 C22 C12 119.3(6) . . ?
C24 C23 C22 119.5(6) . . ?
C24 C23 H23 120.3 . . ?
C22 C23 H23 120.3 . . ?
C23 C24 C25 122.1(6) . . ?
C23 C24 Cl24 119.7(5) . . ?
C25 C24 Cl24 118.2(5) . . ?
C26 C25 C24 118.1(6) . . ?
C26 C25 H25 120.9 . . ?
C24 C25 H25 120.9 . . ?
C25 C26 C21 122.7(6) . . ?
C25 C26 Cl26 119.6(5) . . ?
C21 C26 Cl26 117.7(5) . . ?
C32 O31 C35 107.2(5) . . ?
N33 C32 O31 115.1(6) . . ?
N33 C32 C42 128.7(6) . . ?
O31 C32 C42 116.2(6) . . ?
C32 N33 C34 107.9(5) . . yes
C32 N33 Re1 123.7(4) . . yes
C34 N33 Re1 128.1(4) . . yes
C36 C34 N33 112.7(5) . . ?
C36 C34 C35 112.3(6) . . ?
N33 C34 C35 99.9(5) . . ?
C36 C34 C37 112.1(6) . . ?
N33 C34 C37 107.7(5) . . ?
C35 C34 C37 111.5(6) . . ?
O31 C35 C34 104.7(5) . . ?
O31 C35 H351 110.8 . . ?
C34 C35 H351 110.8 . . ?
O31 C35 H352 110.8 . . ?
C34 C35 H352 110.8 . . ?
H351 C35 H352 108.9 . . ?
C34 C36 H361 109.5 . . ?
C34 C36 H362 109.5 . . ?
H361 C36 H362 109.5 . . ?
C34 C36 H363 109.5 . . ?
H361 C36 H363 109.5 . . ?
H362 C36 H363 109.5 . . ?
C34 C37 H371 109.5 . . ?
C34 C37 H372 109.5 . . ?
H371 C37 H372 109.5 . . ?
C34 C37 H373 109.5 . . ?
H371 C37 H373 109.5 . . ?
H372 C37 H373 109.5 . . ?
C41 O41 Re1 127.9(4) . . yes
O41 C41 C42 124.8(6) . . ?
O41 C41 C46 116.1(5) . . ?
C42 C41 C46 119.1(6) . . ?
C41 C42 C43 119.4(6) . . ?
C41 C42 C32 122.1(6) . . ?
C43 C42 C32 118.4(6) . . ?
C44 C43 C42 120.5(6) . . ?
C44 C43 H43 119.7 . . ?
C42 C43 H43 119.7 . . ?
C43 C44 C45 120.3(6) . . ?
C43 C44 Cl44 121.0(5) . . ?
C45 C44 Cl44 118.6(5) . . ?
C46 C45 C44 121.4(6) . . ?
C46 C45 H45 119.3 . . ?
C44 C45 H45 119.3 . . ?
C45 C46 C41 119.2(6) . . ?
C45 C46 Cl46 123.1(5) . . ?
C41 C46 Cl46 117.7(5) . . ?
O2 Re2 O81 96.0(2) . . ?
O2 Re2 O61 179.66(19) . . yes
O81 Re2 O61 84.04(18) . . ?
O2 Re2 N73 95.7(2) . . ?
O81 Re2 N73 89.6(2) . . ?
O61 Re2 N73 84.0(2) . . ?
O2 Re2 N53 97.2(2) . . ?
O81 Re2 N53 80.98(19) . . ?
O61 Re2 N53 83.13(19) . . ?
N53 Re2 N73 164.7(2) . . yes
O2 Re2 Cl2 93.98(16) . . ?
O81 Re2 Cl2 166.14(13) . . yes
O61 Re2 Cl2 86.02(13) . . ?
N73 Re2 Cl2 98.93(16) . . ?
N53 Re2 Cl2 88.28(16) . . ?
C52 O51 C55 105.8(5) . . ?
N53 C52 O51 116.2(6) . . ?
N53 C52 C62 125.6(6) . . ?
O51 C52 C62 118.2(6) . . ?
C52 N53 C54 105.6(5) . . yes
C52 N53 Re2 126.7(4) . . yes
C54 N53 Re2 125.8(4) . . yes
C55 C54 C56 113.9(6) . . ?
C55 C54 N53 100.2(5) . . ?
C56 C54 N53 113.0(6) . . ?
C55 C54 C57 109.9(6) . . ?
C56 C54 C57 112.2(6) . . ?
N53 C54 C57 106.8(5) . . ?
O51 C55 C54 105.6(5) . . ?
O51 C55 H551 110.6 . . ?
C54 C55 H551 110.6 . . ?
O51 C55 H552 110.6 . . ?
C54 C55 H552 110.6 . . ?
H551 C55 H552 108.7 . . ?
C54 C56 H561 109.5 . . ?
C54 C56 H562 109.5 . . ?
H561 C56 H562 109.5 . . ?
C54 C56 H563 109.5 . . ?
H561 C56 H563 109.5 . . ?
H562 C56 H563 109.5 . . ?
C54 C57 H571 109.5 . . ?
C54 C57 H572 109.5 . . ?
H571 C57 H572 109.5 . . ?
C54 C57 H573 109.5 . . ?
H571 C57 H573 109.5 . . ?
H572 C57 H573 109.5 . . ?
C61 O61 Re2 130.8(4) . . yes
O61 C61 C62 120.5(6) . . ?
O61 C61 C66 119.9(6) . . ?
C62 C61 C66 119.6(6) . . ?
C61 C62 C63 119.5(6) . . ?
C61 C62 C52 123.3(6) . . ?
C63 C62 C52 117.2(6) . . ?
C64 C63 C62 118.4(6) . . ?
C64 C63 H63 120.8 . . ?
C62 C63 H63 120.8 . . ?
C63 C64 C65 123.3(7) . . ?
C63 C64 Cl64 119.1(6) . . ?
C65 C64 Cl64 117.6(6) . . ?
C64 C65 C66 118.1(7) . . ?
C64 C65 H65 120.9 . . ?
C66 C65 H65 120.9 . . ?
C65 C66 C61 120.9(6) . . ?
C65 C66 Cl66 119.7(5) . . ?
C61 C66 Cl66 119.4(5) . . ?
C72 O71 C75 107.8(5) . . ?
N73 C72 O71 116.1(6) . . ?
N73 C72 C82 128.7(6) . . ?
O71 C72 C82 115.2(6) . . ?
C72 N73 C74 105.9(5) . . yes
C72 N73 Re2 123.3(4) . . yes
C74 N73 Re2 130.1(4) . . yes
C76 C74 C77 112.9(5) . . ?
C76 C74 N73 109.3(5) . . ?
C77 C74 N73 108.4(5) . . ?
C76 C74 C75 111.0(5) . . ?
C77 C74 C75 112.8(6) . . ?
N73 C74 C75 101.8(5) . . ?
O71 C75 C74 103.4(5) . . ?
O71 C75 H751 111.1 . . ?
C74 C75 H751 111.1 . . ?
O71 C75 H752 111.1 . . ?
C74 C75 H752 111.1 . . ?
H751 C75 H752 109.1 . . ?
C74 C76 H761 109.5 . . ?
C74 C76 H762 109.5 . . ?
H761 C76 H762 109.5 . . ?
C74 C76 H763 109.5 . . ?
H761 C76 H763 109.5 . . ?
H762 C76 H763 109.5 . . ?
C74 C77 H771 109.5 . . ?
C74 C77 H772 109.5 . . ?
H771 C77 H772 109.5 . . ?
C74 C77 H773 109.5 . . ?
H771 C77 H773 109.5 . . ?
H772 C77 H773 109.5 . . ?
C81 O81 Re2 129.4(4) . . yes
O81 C81 C82 125.9(6) . . ?
O81 C81 C86 116.7(6) . . ?
C82 C81 C86 117.3(6) . . ?
C81 C82 C83 120.3(6) . . ?
C81 C82 C72 121.3(6) . . ?
C83 C82 C72 118.3(6) . . ?
C84 C83 C82 119.8(6) . . ?
C84 C83 H83 120.1 . . ?
C82 C83 H83 120.1 . . ?
C83 C84 C85 121.0(6) . . ?
C83 C84 Cl84 120.4(5) . . ?
C85 C84 Cl84 118.6(5) . . ?
C86 C85 C84 119.2(6) . . ?
C86 C85 H85 120.4 . . ?
C84 C85 H85 120.4 . . ?
C85 C86 C81 122.2(6) . . ?
C85 C86 Cl86 121.0(5) . . ?
C81 C86 Cl86 116.7(5) . . ?

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 9.4(8) . . . . ?
C15 O11 C12 C22 -172.0(6) . . . . ?
O11 C12 N13 C14 9.5(8) . . . . ?
C22 C12 N13 C14 -168.9(7) . . . . ?
O11 C12 N13 Re1 175.6(4) . . . . ?
C22 C12 N13 Re1 -2.8(10) . . . . ?
C12 N13 C14 C17 96.4(6) . . . . ?
Re1 N13 C14 C17 -69.9(7) . . . . ?
C12 N13 C14 C15 -23.1(7) . . . . ?
Re1 N13 C14 C15 170.7(4) . . . . ?
C12 N13 C14 C16 -140.1(6) . . . . ?
Re1 N13 C14 C16 53.7(7) . . . . ?
C12 O11 C15 C14 -24.0(7) . . . . ?
C17 C14 C15 O11 -87.2(7) . . . . ?
C16 C14 C15 O11 145.4(6) . . . . ?
N13 C14 C15 O11 27.8(6) . . . . ?
Re1 O21 C21 C22 33.5(9) . . . . ?
Re1 O21 C21 C26 -148.0(5) . . . . ?
O21 C21 C22 C23 177.8(6) . . . . ?
C26 C21 C22 C23 -0.8(10) . . . . ?
O21 C21 C22 C12 -1.6(10) . . . . ?
C26 C21 C22 C12 179.8(6) . . . . ?
N13 C12 C22 C21 -12.6(11) . . . . ?
O11 C12 C22 C21 169.1(6) . . . . ?
N13 C12 C22 C23 168.0(7) . . . . ?
O11 C12 C22 C23 -10.3(10) . . . . ?
C21 C22 C23 C24 1.6(10) . . . . ?
C12 C22 C23 C24 -179.0(6) . . . . ?
C22 C23 C24 C25 -0.9(10) . . . . ?
C22 C23 C24 Cl24 177.6(5) . . . . ?
C23 C24 C25 C26 -0.6(10) . . . . ?
Cl24 C24 C25 C26 -179.2(5) . . . . ?
C24 C25 C26 C21 1.5(11) . . . . ?
C24 C25 C26 Cl26 -179.8(5) . . . . ?
O21 C21 C26 C25 -179.4(6) . . . . ?
C22 C21 C26 C25 -0.8(10) . . . . ?
O21 C21 C26 Cl26 1.9(9) . . . . ?
C22 C21 C26 Cl26 -179.6(5) . . . . ?
C35 O31 C32 N33 10.9(8) . . . . ?
C35 O31 C32 C42 -168.5(6) . . . . ?
O31 C32 N33 C34 4.3(8) . . . . ?
C42 C32 N33 C34 -176.4(7) . . . . ?
O31 C32 N33 Re1 179.3(4) . . . . ?
C42 C32 N33 Re1 -1.4(10) . . . . ?
C32 N33 C34 C36 -135.4(6) . . . . ?
Re1 N33 C34 C36 49.8(7) . . . . ?
C32 N33 C34 C35 -16.1(7) . . . . ?
Re1 N33 C34 C35 169.2(4) . . . . ?
C32 N33 C34 C37 100.4(6) . . . . ?
Re1 N33 C34 C37 -74.4(7) . . . . ?
C32 O31 C35 C34 -20.6(7) . . . . ?
C36 C34 C35 O31 141.3(6) . . . . ?
N33 C34 C35 O31 21.6(7) . . . . ?
C37 C34 C35 O31 -92.0(6) . . . . ?
Re1 O41 C41 C42 18.7(9) . . . . ?
Re1 O41 C41 C46 -159.6(4) . . . . ?
O41 C41 C42 C43 -179.9(6) . . . . ?
C46 C41 C42 C43 -1.7(9) . . . . ?
O41 C41 C42 C32 1.2(10) . . . . ?
C46 C41 C42 C32 179.5(6) . . . . ?
N33 C32 C42 C41 -10.1(11) . . . . ?
O31 C32 C42 C41 169.1(6) . . . . ?
N33 C32 C42 C43 171.0(7) . . . . ?
O31 C32 C42 C43 -9.7(9) . . . . ?
C41 C42 C43 C44 0.6(10) . . . . ?
C32 C42 C43 C44 179.5(6) . . . . ?
C42 C43 C44 C45 0.7(10) . . . . ?
C42 C43 C44 Cl44 -177.3(5) . . . . ?
C43 C44 C45 C46 -0.8(10) . . . . ?
Cl44 C44 C45 C46 177.2(5) . . . . ?
C44 C45 C46 C41 -0.3(10) . . . . ?
C44 C45 C46 Cl46 -179.3(5) . . . . ?
O41 C41 C46 C45 179.9(6) . . . . ?
C42 C41 C46 C45 1.6(9) . . . . ?
O41 C41 C46 Cl46 -1.0(8) . . . . ?
C42 C41 C46 Cl46 -179.4(5) . . . . ?
C55 O51 C52 N53 5.6(8) . . . . ?
C55 O51 C52 C62 -175.6(6) . . . . ?
O51 C52 N53 C54 11.1(8) . . . . ?
C62 C52 N53 C54 -167.6(6) . . . . ?
O51 C52 N53 Re2 175.9(4) . . . . ?
C62 C52 N53 Re2 -2.7(10) . . . . ?
C52 N53 C54 C55 -21.9(7) . . . . ?
Re2 N53 C54 C55 173.0(4) . . . . ?
C52 N53 C54 C56 -143.5(6) . . . . ?
Re2 N53 C54 C56 51.5(7) . . . . ?
C52 N53 C54 C57 92.7(6) . . . . ?
Re2 N53 C54 C57 -72.4(7) . . . . ?
C52 O51 C55 C54 -20.1(7) . . . . ?
C56 C54 C55 O51 145.9(6) . . . . ?
N53 C54 C55 O51 25.0(7) . . . . ?
C57 C54 C55 O51 -87.2(7) . . . . ?
Re2 O61 C61 C62 33.8(8) . . . . ?
Re2 O61 C61 C66 -145.2(5) . . . . ?
O61 C61 C62 C63 177.4(6) . . . . ?
C66 C61 C62 C63 -3.7(10) . . . . ?
O61 C61 C62 C52 -2.8(10) . . . . ?
C66 C61 C62 C52 176.2(6) . . . . ?
N53 C52 C62 C61 -11.7(11) . . . . ?
O51 C52 C62 C61 169.7(6) . . . . ?
N53 C52 C62 C63 168.2(6) . . . . ?
O51 C52 C62 C63 -10.5(9) . . . . ?
C61 C62 C63 C64 5.7(10) . . . . ?
C52 C62 C63 C64 -174.1(6) . . . . ?
C62 C63 C64 C65 -5.3(11) . . . . ?
C62 C63 C64 Cl64 178.0(5) . . . . ?
C63 C64 C65 C66 2.7(11) . . . . ?
Cl64 C64 C65 C66 179.4(5) . . . . ?
C64 C65 C66 C61 -0.4(10) . . . . ?
C64 C65 C66 Cl66 179.2(5) . . . . ?
O61 C61 C66 C65 -180.0(6) . . . . ?
C62 C61 C66 C65 1.0(10) . . . . ?
O61 C61 C66 Cl66 0.4(9) . . . . ?
C62 C61 C66 Cl66 -178.6(5) . . . . ?
C75 O71 C72 N73 9.2(8) . . . . ?
C75 O71 C72 C82 -169.1(6) . . . . ?
O71 C72 N73 C74 5.9(8) . . . . ?
C82 C72 N73 C74 -176.1(7) . . . . ?
O71 C72 N73 Re2 177.4(4) . . . . ?
C82 C72 N73 Re2 -4.6(10) . . . . ?
C72 N73 C74 C76 -134.8(6) . . . . ?
Re2 N73 C74 C76 54.5(7) . . . . ?
C72 N73 C74 C77 101.7(6) . . . . ?
Re2 N73 C74 C77 -69.0(7) . . . . ?
C72 N73 C74 C75 -17.4(7) . . . . ?
Re2 N73 C74 C75 171.9(5) . . . . ?
C72 O71 C75 C74 -19.8(7) . . . . ?
C76 C74 C75 O71 138.0(5) . . . . ?
C77 C74 C75 O71 -94.1(6) . . . . ?
N73 C74 C75 O71 21.8(7) . . . . ?
Re2 O81 C81 C82 9.3(9) . . . . ?
Re2 O81 C81 C86 -167.6(4) . . . . ?
O81 C81 C82 C83 -179.4(6) . . . . ?
C86 C81 C82 C83 -2.5(9) . . . . ?
O81 C81 C82 C72 3.2(10) . . . . ?
C86 C81 C82 C72 -180.0(6) . . . . ?
N73 C72 C82 C81 -5.3(11) . . . . ?
O71 C72 C82 C81 172.8(6) . . . . ?
N73 C72 C82 C83 177.2(6) . . . . ?
O71 C72 C82 C83 -4.7(9) . . . . ?
C81 C82 C83 C84 -0.6(10) . . . . ?
C72 C82 C83 C84 176.9(6) . . . . ?
C82 C83 C84 C85 3.6(10) . . . . ?
C82 C83 C84 Cl84 -174.0(5) . . . . ?
C83 C84 C85 C86 -3.5(10) . . . . ?
Cl84 C84 C85 C86 174.2(5) . . . . ?
C84 C85 C86 C81 0.2(10) . . . . ?
C84 C85 C86 Cl86 -179.7(5) . . . . ?
O81 C81 C86 C85 179.9(6) . . . . ?
C82 C81 C86 C85 2.7(10) . . . . ?
O81 C81 C86 Cl86 -0.3(8) . . . . ?
C82 C81 C86 Cl86 -177.4(5) . . . . ?

_refine_diff_density_max         1.794
_refine_diff_density_min         -1.740
_refine_diff_density_rms         0.197

_shelxl_version_number           2014/6

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_JSJZ21
_database_code_depnum_ccdc_archive 'CCDC 1995752'
loop_
_audit_author_name
_audit_author_address
'Ferdinand Belaj'
;University of Graz
Austria
;
_audit_update_record             
;
2020-04-08 deposited with the CCDC.	2024-12-12 downloaded from the CCDC.
;
_audit_creation_method           'manual edited SHELXL-2014/6.cif file'

_chemical_compound_source        'synthetical product'

_chemical_name_systematic        
bis[2-(4,4-dimethyl-4,5-dihydro-1,3-oxazol-2-yl)-4,6-dichlo-rophenolato-N,O]-dioxo-rhenium(VI)
_chemical_name_common            
bis[2-(4,4-dimethyl-4,5-dihydro-1,3-oxazol-2-yl)-4,6-dichlo-rophenolato-N,O]-dioxo-rhenium(VI)
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H20 Cl4 N2 O6 Re'
_chemical_formula_sum            'C22 H20 Cl4 N2 O6 Re'
_chemical_formula_weight         736.40

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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_H-M_alt        'P c c n'
_space_group_name_Hall           '-P 2ab 2ac'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-x, y+1/2, -z+1/2'
'x+1/2, -y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'x, -y-1/2, z-1/2'
'-x-1/2, y, z-1/2'

_cell_length_a                   16.202(3)
_cell_length_b                   16.335(3)
_cell_length_c                   18.805(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4976.9(15)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9744
_cell_measurement_theta_min      2.50
_cell_measurement_theta_max      40.71

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.966
_exptl_crystal_F_000             2856
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.090
_exptl_absorpt_coefficient_mu    5.355
_shelx_estimated_absorpt_T_min   0.316
_shelx_estimated_absorpt_T_max   0.644
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.593
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
'Bruker (2001). SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.'

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_source         'Incoatec microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  'multilayer monochromator'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            77915
_diffrn_reflns_av_unetI/netI     0.0424
_diffrn_reflns_av_R_equivalents  0.0542
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         1.77
_diffrn_reflns_theta_max         40.00
_diffrn_reflns_theta_full        40.00
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             15402
_reflns_number_gt                10723
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     ?
_reflns_Friedel_fraction_full    ?

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2015)'
_computing_molecular_graphics    'modified ORTEP (Johnson, 1965)'
_computing_publication_material  'SHELXL-2014/6 (Sheldrick, 2015)'

_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.
 
 The non-hydrogen atoms were refined with anisotropic displacement parameters
 without any constraints.
 
 The H atoms of the CH₂ groups were refined with common isotropic
 displacement parameters for the H atoms of the same group and idealized
 geometries with approximately tetrahedral angles and C-H distances of 0.99 Å
 (AFIX 23 of SHELXL).
 
 The H atoms of the phenyl rings were put at the external bisectors of the
 C-C-C angles at C-H distances of 0.95 Å and common isotropic displacement
 parameters were refined for the H atoms of the same ring
 (AFIX 43 of SHELXL).
 
 The H atoms of the methyl groups were refined with common isotropic
 displacement parameters for the H atoms of the same group and idealized
 geometries with tetrahedral angles, enabling rotation around the C-C bonds,
 and C-H distances of 0.98 Å (AFIX 137 of SHELXL).
 
 The largest peaks in a final difference Fourier map (1.28 - 1.78 eÅ⁻³)
 were in the vicinity (0.65 - 0.72 Å) of the Re atom.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0217P)²+2.4883P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    refU
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         15402
_refine_ls_number_parameters     330
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0501
_refine_ls_R_factor_gt           0.0283
_refine_ls_wR_factor_ref         0.0686
_refine_ls_wR_factor_gt          0.0605
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_restrained_S_all      1.018
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

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 0.2500 0.2500 0.24920(2) 0.00892(2) Uani 1 2 d S T P . .
O1 O 0.28084(8) 0.16907(8) 0.19524(7) 0.0140(2) Uani 1 1 d . . . . .
O11 O 0.48009(8) 0.35395(8) 0.31044(7) 0.0166(2) Uani 1 1 d . . . . .
C12 C 0.40045(10) 0.33195(10) 0.31546(8) 0.0121(2) Uani 1 1 d . . . . .
N13 N 0.37109(9) 0.29352(9) 0.25984(7) 0.0109(2) Uani 1 1 d . . . . .
C14 C 0.44147(10) 0.27741(11) 0.20937(8) 0.0130(3) Uani 1 1 d . . . . .
C15 C 0.50422(11) 0.33940(12) 0.23696(9) 0.0168(3) Uani 1 1 d . . . . .
H151 H 0.5609 0.3169 0.2344 0.021(5) Uiso 1 1 calc R U . . .
H152 H 0.5019 0.3907 0.2090 0.021(5) Uiso 1 1 calc R U . . .
C16 C 0.41736(12) 0.29449(13) 0.13300(9) 0.0188(3) Uani 1 1 d . . . . .
H161 H 0.3757 0.2547 0.1177 0.019(4) Uiso 1 1 calc R U . . .
H162 H 0.4662 0.2899 0.1025 0.019(4) Uiso 1 1 calc R U . . .
H163 H 0.3946 0.3499 0.1294 0.019(4) Uiso 1 1 calc R U . . .
C17 C 0.47218(11) 0.18972(11) 0.22088(10) 0.0171(3) Uani 1 1 d . . . . .
H171 H 0.4278 0.1511 0.2096 0.028(4) Uiso 1 1 calc R U . . .
H172 H 0.4888 0.1827 0.2706 0.028(4) Uiso 1 1 calc R U . . .
H173 H 0.5196 0.1793 0.1898 0.028(4) Uiso 1 1 calc R U . . .
O21 O 0.22453(8) 0.32512(8) 0.33496(6) 0.01250(19) Uani 1 1 d . . . . .
C21 C 0.27326(11) 0.34577(10) 0.38760(8) 0.0115(2) Uani 1 1 d . . . . .
C22 C 0.35948(10) 0.35298(10) 0.38161(8) 0.0133(3) Uani 1 1 d . . . . .
C23 C 0.40782(11) 0.38228(11) 0.43810(8) 0.0150(3) Uani 1 1 d . . . . .
H23 H 0.4658 0.3884 0.4327 0.018(5) Uiso 1 1 calc R U . . .
C24 C 0.37020(13) 0.40205(11) 0.50147(8) 0.0166(3) Uani 1 1 d . . . . .
C25 C 0.28522(12) 0.39204(11) 0.51105(9) 0.0170(3) Uani 1 1 d . . . . .
H25 H 0.2603 0.4038 0.5556 0.018(5) Uiso 1 1 calc R U . . .
C26 C 0.23805(10) 0.36477(11) 0.45472(8) 0.0142(3) Uani 1 1 d . . . . .
Cl24 Cl 0.42959(3) 0.43951(3) 0.57115(2) 0.02192(8) Uani 1 1 d . . . . .
Cl26 Cl 0.13268(3) 0.35296(3) 0.46435(2) 0.01821(7) Uani 1 1 d . . . . .
Re2 Re 0.7500 0.2500 0.70933(2) 0.00946(2) Uani 1 2 d S T P . .
O2 O 0.66792(8) 0.27893(8) 0.76292(7) 0.0151(2) Uani 1 1 d . . . . .
O31 O 0.85280(9) 0.48092(8) 0.65306(7) 0.0175(2) Uani 1 1 d . . . . .
C32 C 0.83001(10) 0.40237(10) 0.64604(8) 0.0128(3) Uani 1 1 d . . . . .
N33 N 0.79002(9) 0.37168(9) 0.69981(7) 0.0119(2) Uani 1 1 d . . . . .
C34 C 0.77232(12) 0.44072(11) 0.75104(9) 0.0145(3) Uani 1 1 d . . . . .
C35 C 0.83716(12) 0.50282(10) 0.72719(9) 0.0165(3) Uani 1 1 d . . . . .
H351 H 0.8158 0.5594 0.7310 0.021(5) Uiso 1 1 calc R U . . .
H352 H 0.8880 0.4980 0.7560 0.021(5) Uiso 1 1 calc R U . . .
C36 C 0.78468(13) 0.41502(12) 0.82806(9) 0.0193(3) Uani 1 1 d . . . . .
H361 H 0.7424 0.3749 0.8413 0.026(4) Uiso 1 1 calc R U . . .
H362 H 0.7802 0.4631 0.8590 0.026(4) Uiso 1 1 calc R U . . .
H363 H 0.8395 0.3904 0.8336 0.026(4) Uiso 1 1 calc R U . . .
C37 C 0.68493(12) 0.47186(12) 0.73624(10) 0.0194(3) Uani 1 1 d . . . . .
H371 H 0.6805 0.4883 0.6863 0.025(4) Uiso 1 1 calc R U . . .
H372 H 0.6733 0.5191 0.7668 0.025(4) Uiso 1 1 calc R U . . .
H373 H 0.6451 0.4282 0.7462 0.025(4) Uiso 1 1 calc R U . . .
O41 O 0.82700(8) 0.22749(8) 0.62377(7) 0.0146(2) Uani 1 1 d . . . . .
C41 C 0.84830(10) 0.27728(11) 0.57227(8) 0.0126(2) Uani 1 1 d . . . . .
C42 C 0.85324(10) 0.36320(10) 0.57990(8) 0.0133(3) Uani 1 1 d . . . . .
C43 C 0.88356(11) 0.41319(12) 0.52441(9) 0.0160(3) Uani 1 1 d . . . . .
H43 H 0.8885 0.4707 0.5308 0.023(5) Uiso 1 1 calc R U . . .
C44 C 0.90570(12) 0.37752(12) 0.46115(9) 0.0180(3) Uani 1 1 d . . . . .
C45 C 0.89957(12) 0.29307(13) 0.45038(9) 0.0194(3) Uani 1 1 d . . . . .
H45 H 0.9144 0.2695 0.4060 0.023(5) Uiso 1 1 calc R U . . .
C46 C 0.87154(12) 0.24457(11) 0.50546(9) 0.0163(3) Uani 1 1 d . . . . .
Cl44 Cl 0.94325(3) 0.43934(3) 0.39281(2) 0.02583(10) Uani 1 1 d . . . . .
Cl46 Cl 0.86473(3) 0.13911(3) 0.49438(2) 0.02269(9) Uani 1 1 d . . . . .


_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_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Re1 O1 1.7397(13) . yes
Re1 O21 2.0680(12) . yes
Re1 N13 2.0963(14) . yes
O11 C12 1.343(2) . ?
O11 C15 1.455(2) . ?
C12 N13 1.309(2) . ?
C12 C22 1.451(2) . ?
N13 C14 1.507(2) . ?
C14 C16 1.514(2) . ?
C14 C15 1.526(2) . ?
C14 C17 1.532(3) . ?
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 1.310(2) . ?
C21 C22 1.406(2) . ?
C21 C26 1.419(2) . ?
C22 C23 1.404(2) . ?
C23 C24 1.377(2) . ?
C23 H23 0.95 . ?
C24 C25 1.398(3) . ?
C24 Cl24 1.7371(17) . ?
C25 C26 1.380(2) . ?
C25 H25 0.95 . ?
C26 Cl26 1.7277(17) . ?
Re2 O2 1.7342(13) . yes
Re2 O41 2.0689(12) . yes
Re2 N33 2.0984(15) . yes
O31 C32 1.342(2) . ?
O31 C35 1.461(2) . ?
C32 N33 1.301(2) . ?
C32 C42 1.448(2) . ?
N33 C34 1.511(2) . ?
C34 C36 1.521(2) . ?
C34 C35 1.528(3) . ?
C34 C37 1.530(3) . ?
C35 H351 0.99 . ?
C35 H352 0.99 . ?
C36 H361 0.98 . ?
C36 H362 0.98 . ?
C36 H363 0.98 . ?
C37 H371 0.98 . ?
C37 H372 0.98 . ?
C37 H373 0.98 . ?
O41 C41 1.311(2) . ?
C41 C42 1.413(2) . ?
C41 C46 1.416(2) . ?
C42 C43 1.413(2) . ?
C43 C44 1.372(3) . ?
C43 H43 0.95 . ?
C44 C45 1.398(3) . ?
C44 Cl44 1.7439(18) . ?
C45 C46 1.381(3) . ?
C45 H45 0.95 . ?
C46 Cl46 1.7388(19) . ?

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 O1 108.65(8) . 2 ?
O1 Re1 O21 164.36(5) . . yes
O1 Re1 O21 86.94(5) . 2 ?
O21 Re1 O21 77.51(7) . 2 ?
O1 Re1 N13 93.83(6) . 2 ?
O21 Re1 N13 86.56(5) . 2 ?
O1 Re1 N13 92.55(6) . . ?
O21 Re1 N13 84.90(5) . . ?
N13 Re1 N13 169.04(7) . 2 yes
C12 O11 C15 106.33(13) . . ?
N13 C12 O11 114.91(14) . . ?
N13 C12 C22 129.20(15) . . ?
O11 C12 C22 115.88(14) . . ?
C12 N13 C14 108.18(13) . . yes
C12 N13 Re1 125.37(11) . . yes
C14 N13 Re1 126.08(10) . . yes
N13 C14 C16 111.72(14) . . ?
N13 C14 C15 100.03(13) . . ?
C16 C14 C15 111.85(15) . . ?
N13 C14 C17 108.67(14) . . ?
C16 C14 C17 112.96(15) . . ?
C15 C14 C17 110.86(15) . . ?
O11 C15 C14 104.60(13) . . ?
O11 C15 H151 110.8 . . ?
C14 C15 H151 110.8 . . ?
O11 C15 H152 110.8 . . ?
C14 C15 H152 110.8 . . ?
H151 C15 H152 108.9 . . ?
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 128.44(11) . . yes
O21 C21 C22 124.02(14) . . ?
O21 C21 C26 119.07(15) . . ?
C22 C21 C26 116.88(14) . . ?
C23 C22 C21 121.47(15) . . ?
C23 C22 C12 118.30(15) . . ?
C21 C22 C12 120.21(14) . . ?
C24 C23 C22 119.20(17) . . ?
C24 C23 H23 120.4 . . ?
C22 C23 H23 120.4 . . ?
C23 C24 C25 121.34(16) . . ?
C23 C24 Cl24 119.36(15) . . ?
C25 C24 Cl24 119.30(13) . . ?
C26 C25 C24 118.96(16) . . ?
C26 C25 H25 120.5 . . ?
C24 C25 H25 120.5 . . ?
C25 C26 C21 122.04(16) . . ?
C25 C26 Cl26 120.19(13) . . ?
C21 C26 Cl26 117.77(13) . . ?
O2 Re2 O2 108.94(9) . 2_655 ?
O2 Re2 O41 86.62(6) . 2_655 ?
O2 Re2 O41 164.32(6) . . yes
O41 Re2 O41 77.90(7) . 2_655 ?
O2 Re2 N33 94.05(6) . 2_655 ?
O41 Re2 N33 87.23(5) . 2_655 ?
O2 Re2 N33 91.63(6) . . ?
O41 Re2 N33 85.16(5) . . ?
N33 Re2 N33 170.21(7) . 2_655 yes
C32 O31 C35 106.28(13) . . ?
N33 C32 O31 115.40(15) . . ?
N33 C32 C42 128.78(15) . . ?
O31 C32 C42 115.81(14) . . ?
C32 N33 C34 107.60(14) . . yes
C32 N33 Re2 125.81(11) . . yes
C34 N33 Re2 126.44(11) . . yes
N33 C34 C36 112.10(15) . . ?
N33 C34 C35 100.25(13) . . ?
C36 C34 C35 111.85(16) . . ?
N33 C34 C37 107.93(14) . . ?
C36 C34 C37 112.76(16) . . ?
C35 C34 C37 111.23(16) . . ?
O31 C35 C34 103.69(13) . . ?
O31 C35 H351 111.0 . . ?
C34 C35 H351 111.0 . . ?
O31 C35 H352 111.0 . . ?
C34 C35 H352 111.0 . . ?
H351 C35 H352 109.0 . . ?
C34 C36 H361 109.5 . . ?
C34 C36 H362 109.5 . . ?
H361 C36 H362 109.5 . . ?
C34 C36 H363 109.5 . . ?
H361 C36 H363 109.5 . . ?
H362 C36 H363 109.5 . . ?
C34 C37 H371 109.5 . . ?
C34 C37 H372 109.5 . . ?
H371 C37 H372 109.5 . . ?
C34 C37 H373 109.5 . . ?
H371 C37 H373 109.5 . . ?
H372 C37 H373 109.5 . . ?
C41 O41 Re2 128.54(11) . . yes
O41 C41 C42 123.79(15) . . ?
O41 C41 C46 119.43(16) . . ?
C42 C41 C46 116.73(15) . . ?
C43 C42 C41 121.24(15) . . ?
C43 C42 C32 117.98(15) . . ?
C41 C42 C32 120.74(14) . . ?
C44 C43 C42 119.05(17) . . ?
C44 C43 H43 120.5 . . ?
C42 C43 H43 120.5 . . ?
C43 C44 C45 121.73(16) . . ?
C43 C44 Cl44 118.95(15) . . ?
C45 C44 Cl44 119.32(14) . . ?
C46 C45 C44 118.75(16) . . ?
C46 C45 H45 120.6 . . ?
C44 C45 H45 120.6 . . ?
C45 C46 C41 122.44(17) . . ?
C45 C46 Cl46 119.96(13) . . ?
C41 C46 Cl46 117.60(13) . . ?

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 9.9(2) . . . . ?
C15 O11 C12 C22 -170.88(15) . . . . ?
O11 C12 N13 C14 6.4(2) . . . . ?
C22 C12 N13 C14 -172.68(16) . . . . ?
O11 C12 N13 Re1 179.79(11) . . . . ?
C22 C12 N13 Re1 0.7(3) . . . . ?
C12 N13 C14 C16 -137.20(16) . . . . ?
Re1 N13 C14 C16 49.52(19) . . . . ?
C12 N13 C14 C15 -18.69(17) . . . . ?
Re1 N13 C14 C15 168.03(11) . . . . ?
C12 N13 C14 C17 97.51(16) . . . . ?
Re1 N13 C14 C17 -75.78(16) . . . . ?
C12 O11 C15 C14 -21.36(18) . . . . ?
N13 C14 C15 O11 23.53(17) . . . . ?
C16 C14 C15 O11 141.94(15) . . . . ?
C17 C14 C15 O11 -91.01(17) . . . . ?
Re1 O21 C21 C22 30.6(2) . . . . ?
Re1 O21 C21 C26 -151.43(13) . . . . ?
O21 C21 C22 C23 174.31(16) . . . . ?
C26 C21 C22 C23 -3.7(2) . . . . ?
O21 C21 C22 C12 -4.1(3) . . . . ?
C26 C21 C22 C12 177.88(15) . . . . ?
N13 C12 C22 C23 169.52(17) . . . . ?
O11 C12 C22 C23 -9.6(2) . . . . ?
N13 C12 C22 C21 -12.0(3) . . . . ?
O11 C12 C22 C21 168.88(15) . . . . ?
C21 C22 C23 C24 2.0(3) . . . . ?
C12 C22 C23 C24 -179.56(16) . . . . ?
C22 C23 C24 C25 1.2(3) . . . . ?
C22 C23 C24 Cl24 -179.21(13) . . . . ?
C23 C24 C25 C26 -2.5(3) . . . . ?
Cl24 C24 C25 C26 177.91(14) . . . . ?
C24 C25 C26 C21 0.7(3) . . . . ?
C24 C25 C26 Cl26 -179.17(14) . . . . ?
O21 C21 C26 C25 -175.74(16) . . . . ?
C22 C21 C26 C25 2.4(3) . . . . ?
O21 C21 C26 Cl26 4.1(2) . . . . ?
C22 C21 C26 Cl26 -177.79(13) . . . . ?
C35 O31 C32 N33 10.2(2) . . . . ?
C35 O31 C32 C42 -169.74(15) . . . . ?
O31 C32 N33 C34 7.2(2) . . . . ?
C42 C32 N33 C34 -172.86(17) . . . . ?
O31 C32 N33 Re2 -176.93(11) . . . . ?
C42 C32 N33 Re2 3.0(3) . . . . ?
C32 N33 C34 C36 -139.02(16) . . . . ?
Re2 N33 C34 C36 45.2(2) . . . . ?
C32 N33 C34 C35 -20.23(17) . . . . ?
Re2 N33 C34 C35 163.97(11) . . . . ?
C32 N33 C34 C37 96.21(17) . . . . ?
Re2 N33 C34 C37 -79.58(16) . . . . ?
C32 O31 C35 C34 -22.48(18) . . . . ?
N33 C34 C35 O31 25.05(16) . . . . ?
C36 C34 C35 O31 144.02(15) . . . . ?
C37 C34 C35 O31 -88.90(17) . . . . ?
Re2 O41 C41 C42 29.1(2) . . . . ?
Re2 O41 C41 C46 -153.78(13) . . . . ?
O41 C41 C42 C43 174.32(16) . . . . ?
C46 C41 C42 C43 -2.8(2) . . . . ?
O41 C41 C42 C32 -3.4(3) . . . . ?
C46 C41 C42 C32 179.41(16) . . . . ?
N33 C32 C42 C43 168.92(17) . . . . ?
O31 C32 C42 C43 -11.2(2) . . . . ?
N33 C32 C42 C41 -13.2(3) . . . . ?
O31 C32 C42 C41 166.66(15) . . . . ?
C41 C42 C43 C44 2.4(3) . . . . ?
C32 C42 C43 C44 -179.78(16) . . . . ?
C42 C43 C44 C45 -0.4(3) . . . . ?
C42 C43 C44 Cl44 -179.90(14) . . . . ?
C43 C44 C45 C46 -0.9(3) . . . . ?
Cl44 C44 C45 C46 178.52(15) . . . . ?
C44 C45 C46 C41 0.4(3) . . . . ?
C44 C45 C46 Cl46 -178.96(15) . . . . ?
O41 C41 C46 C45 -175.85(17) . . . . ?
C42 C41 C46 C45 1.4(3) . . . . ?
O41 C41 C46 Cl46 3.5(2) . . . . ?
C42 C41 C46 Cl46 -179.19(13) . . . . ?

_refine_diff_density_max         1.776
_refine_diff_density_min         -1.583
_refine_diff_density_rms         0.168

_shelxl_version_number           2014/6

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_JS76V
_database_code_depnum_ccdc_archive 'CCDC 1854792'
loop_
_audit_author_name
_audit_author_address
'Ferdinand Belaj'
;University of Graz
Austria
;
_audit_update_record             
;
2018-07-10 deposited with the CCDC.	2024-12-12 downloaded from the CCDC.
;
_audit_creation_method           'manual edited SHELXL-2014/6.cif file'

_chemical_compound_source        'synthetical product'

_chemical_name_systematic        
'trichloro-[2,4-dichloro-6-(4,4-dimethyl-4,5-dihydro-1,3-oxa-zol-2-yl)phenolato-N,O]-(triphenylphosphine oxide-O)-rhenium(IV)'
_chemical_name_common            
'trichloro-[2,4-dichloro-6-(4,4-dimethyl-4,5-dihydro-1,3-oxa-zol-2-yl)phenolato-N,O]-(triphenylphosphine oxide-O)-rhenium(IV)'
_chemical_melting_point          ?
_chemical_formula_moiety         'C29 H25 Cl5 N O3 P Re'
_chemical_formula_sum            'C29 H25 Cl5 N O3 P Re'
_chemical_formula_weight         829.92

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'
P P 0.1023 0.0942 '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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.9619(18)
_cell_length_b                   10.0674(18)
_cell_length_c                   17.161(3)
_cell_angle_alpha                73.649(5)
_cell_angle_beta                 76.698(5)
_cell_angle_gamma                71.136(6)
_cell_volume                     1544.3(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5384
_cell_measurement_theta_min      2.35
_cell_measurement_theta_max      23.47

_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.785
_exptl_crystal_F_000             810
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    4.451
_shelx_estimated_absorpt_T_min   0.536
_shelx_estimated_absorpt_T_max   0.842
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.624
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
'Bruker (2001). SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.'

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_source         'Incoatec microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  'multilayer monochromator'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            27366
_diffrn_reflns_av_unetI/netI     0.0721
_diffrn_reflns_av_R_equivalents  0.0893
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.19
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             6063
_reflns_number_gt                4977
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     ?
_reflns_Friedel_fraction_full    ?

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2015)'
_computing_molecular_graphics    'modified ORTEP (Johnson, 1965)'
_computing_publication_material  'SHELXL-2014/6 (Sheldrick, 2015)'

_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.
 
 The non-hydrogen atoms were refined with anisotropic displacement parameters
 without any constraints.
 
 The H atoms of the phenyl rings were put at the external bisectors of the
 C-C-C angles at C-H distances of 0.95 Å and common isotropic displacement
 parameters were refined for the H atoms of the same ring
 (AFIX 43 of SHELXL).
 
 The H atoms of the CH₂ group were refined with common isotropic
 displacement parameters and idealized geometry with approximately
 tetrahedral angles and C-H distances of 0.99 Å (AFIX 23 of SHELXL).
 
 The H atoms of the methyl groups were refined with common isotropic
 displacement parameters for the H atoms of the same group and idealized
 geometries with tetrahedral angles, enabling rotation around the C-C bonds,
 and C-H distances of 0.98 Å (AFIX 137 of SHELXL).
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0174P)²+1.0201P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    refU
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6063
_refine_ls_number_parameters     370
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0359
_refine_ls_wR_factor_ref         0.0685
_refine_ls_wR_factor_gt          0.0630
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.029
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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 0.74354(2) 0.57065(2) 0.72819(2) 0.01159(7) Uani 1 1 d . . . . .
Cl1 Cl 0.51746(12) 0.53845(14) 0.79088(8) 0.0186(3) Uani 1 1 d . . . . .
Cl2 Cl 0.96769(12) 0.59895(13) 0.65641(8) 0.0188(3) Uani 1 1 d . . . . .
Cl3 Cl 0.78492(12) 0.61992(13) 0.84380(7) 0.0176(3) Uani 1 1 d . . . . .
O11 O 0.5972(4) 0.6090(4) 0.5064(2) 0.0238(9) Uani 1 1 d . . . . .
C12 C 0.6113(5) 0.6420(5) 0.5745(3) 0.0163(11) Uani 1 1 d . . . . .
N13 N 0.7019(4) 0.5452(4) 0.6192(2) 0.0148(9) Uani 1 1 d . . . . .
C14 C 0.7510(5) 0.4131(5) 0.5838(3) 0.0185(12) Uani 1 1 d . . . . .
C15 C 0.7129(5) 0.4794(6) 0.4977(3) 0.0228(12) Uani 1 1 d . . . . .
H151 H 0.7963 0.5034 0.4586 0.029(11) Uiso 1 1 calc R U . . .
H152 H 0.6808 0.4129 0.4781 0.029(11) Uiso 1 1 calc R U . . .
C16 C 0.6580(6) 0.3143(6) 0.6337(3) 0.0252(13) Uani 1 1 d . . . . .
H161 H 0.6601 0.2997 0.6924 0.028(8) Uiso 1 1 calc R U . . .
H162 H 0.6952 0.2213 0.6179 0.028(8) Uiso 1 1 calc R U . . .
H163 H 0.5590 0.3587 0.6228 0.028(8) Uiso 1 1 calc R U . . .
C17 C 0.9092(5) 0.3375(6) 0.5820(3) 0.0220(12) Uani 1 1 d . . . . .
H171 H 0.9647 0.4064 0.5532 0.028(9) Uiso 1 1 calc R U . . .
H172 H 0.9354 0.2591 0.5532 0.028(9) Uiso 1 1 calc R U . . .
H173 H 0.9302 0.2978 0.6384 0.028(9) Uiso 1 1 calc R U . . .
O21 O 0.6492(3) 0.7780(3) 0.6917(2) 0.0192(8) Uani 1 1 d . . . . .
C21 C 0.5419(5) 0.8379(5) 0.6485(3) 0.0208(12) Uani 1 1 d . . . . .
C22 C 0.4485(6) 0.9750(6) 0.6575(3) 0.0248(13) Uani 1 1 d . . . . .
C23 C 0.3361(6) 1.0440(6) 0.6131(4) 0.0330(15) Uani 1 1 d . . . . .
H23 H 0.2722 1.1335 0.6220 0.036(12) Uiso 1 1 calc R U . . .
C24 C 0.3176(6) 0.9815(6) 0.5556(3) 0.0294(14) Uani 1 1 d . . . . .
C25 C 0.4071(5) 0.8521(6) 0.5430(3) 0.0273(13) Uani 1 1 d . . . . .
H25 H 0.3940 0.8113 0.5026 0.036(12) Uiso 1 1 calc R U . . .
C26 C 0.5189(5) 0.7789(6) 0.5899(3) 0.0219(12) Uani 1 1 d . . . . .
Cl22 Cl 0.47414(16) 1.05324(15) 0.72867(9) 0.0346(4) Uani 1 1 d . . . . .
Cl24 Cl 0.18106(16) 1.07174(19) 0.49582(10) 0.0515(5) Uani 1 1 d . . . . .
O1 O 0.8335(3) 0.3541(3) 0.76927(19) 0.0107(7) Uani 1 1 d . . . . .
P1 P 0.89496(12) 0.23753(13) 0.84146(8) 0.0120(3) Uani 1 1 d . . . . .
C31 C 1.0250(5) 0.2866(5) 0.8758(3) 0.0152(11) Uani 1 1 d . . . . .
C32 C 1.0175(6) 0.2836(6) 0.9590(3) 0.0243(13) Uani 1 1 d . . . . .
H32 H 0.9447 0.2516 0.9992 0.040(8) Uiso 1 1 calc R U . . .
C33 C 1.1182(6) 0.3280(6) 0.9813(4) 0.0355(15) Uani 1 1 d . . . . .
H33 H 1.1134 0.3278 1.0373 0.040(8) Uiso 1 1 calc R U . . .
C34 C 1.2253(6) 0.3725(6) 0.9232(4) 0.0401(17) Uani 1 1 d . . . . .
H34 H 1.2927 0.4046 0.9391 0.040(8) Uiso 1 1 calc R U . . .
C35 C 1.2347(6) 0.3706(6) 0.8414(4) 0.0340(15) Uani 1 1 d . . . . .
H35 H 1.3113 0.3968 0.8019 0.040(8) Uiso 1 1 calc R U . . .
C36 C 1.1332(5) 0.3306(6) 0.8175(4) 0.0254(13) Uani 1 1 d . . . . .
H36 H 1.1374 0.3333 0.7613 0.040(8) Uiso 1 1 calc R U . . .
C41 C 0.7583(5) 0.2023(5) 0.9265(3) 0.0143(11) Uani 1 1 d . . . . .
C42 C 0.7416(5) 0.0637(6) 0.9585(3) 0.0199(12) Uani 1 1 d . . . . .
H42 H 0.8018 -0.0137 0.9344 0.034(7) Uiso 1 1 calc R U . . .
C43 C 0.6368(6) 0.0395(6) 1.0254(3) 0.0283(14) Uani 1 1 d . . . . .
H43 H 0.6250 -0.0546 1.0469 0.034(7) Uiso 1 1 calc R U . . .
C44 C 0.5496(5) 0.1511(6) 1.0609(3) 0.0267(13) Uani 1 1 d . . . . .
H44 H 0.4779 0.1336 1.1066 0.034(7) Uiso 1 1 calc R U . . .
C45 C 0.5660(5) 0.2881(6) 1.0303(3) 0.0235(13) Uani 1 1 d . . . . .
H45 H 0.5056 0.3649 1.0547 0.034(7) Uiso 1 1 calc R U . . .
C46 C 0.6712(5) 0.3133(6) 0.9636(3) 0.0199(12) Uani 1 1 d . . . . .
H46 H 0.6836 0.4073 0.9432 0.034(7) Uiso 1 1 calc R U . . .
C51 C 0.9818(5) 0.0723(5) 0.8073(3) 0.0169(11) Uani 1 1 d . . . . .
C52 C 1.1144(5) -0.0147(6) 0.8287(3) 0.0203(12) Uani 1 1 d . . . . .
H52 H 1.1634 0.0155 0.8591 0.036(7) Uiso 1 1 calc R U . . .
C53 C 1.1745(6) -0.1451(6) 0.8058(4) 0.0297(14) Uani 1 1 d . . . . .
H53 H 1.2654 -0.2042 0.8198 0.036(7) Uiso 1 1 calc R U . . .
C54 C 1.1019(6) -0.1895(6) 0.7622(4) 0.0327(15) Uani 1 1 d . . . . .
H54 H 1.1432 -0.2792 0.7465 0.036(7) Uiso 1 1 calc R U . . .
C55 C 0.9704(6) -0.1043(6) 0.7415(3) 0.0312(14) Uani 1 1 d . . . . .
H55 H 0.9213 -0.1353 0.7117 0.036(7) Uiso 1 1 calc R U . . .
C56 C 0.9099(6) 0.0262(6) 0.7639(3) 0.0242(13) Uani 1 1 d . . . . .
H56 H 0.8189 0.0847 0.7497 0.036(7) Uiso 1 1 calc R U . . .


_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_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Re1 O1 2.053(3) . yes
Re1 N13 2.105(4) . yes
Re1 O21 1.974(3) . yes
Re1 Cl1 2.3443(12) . yes
Re1 Cl2 2.3522(12) . yes
Re1 Cl3 2.3268(12) . yes
O11 C12 1.349(6) . ?
O11 C15 1.453(6) . ?
C12 N13 1.296(6) . ?
C12 C26 1.446(7) . ?
N13 C14 1.508(6) . ?
C14 C17 1.509(7) . ?
C14 C15 1.521(7) . ?
C14 C16 1.527(7) . ?
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 1.323(6) . ?
C21 C26 1.396(7) . ?
C21 C22 1.421(7) . ?
C22 C23 1.382(8) . ?
C22 Cl22 1.730(6) . ?
C23 C24 1.383(8) . ?
C23 H23 0.95 . ?
C24 C25 1.363(8) . ?
C24 Cl24 1.745(6) . ?
C25 C26 1.406(7) . ?
C25 H25 0.95 . ?
O1 P1 1.534(3) . yes
P1 C31 1.788(5) . ?
P1 C41 1.793(5) . ?
P1 C51 1.802(5) . ?
C31 C36 1.386(7) . ?
C31 C32 1.405(7) . ?
C32 C33 1.384(7) . ?
C32 H32 0.95 . ?
C33 C34 1.379(8) . ?
C33 H33 0.95 . ?
C34 C35 1.391(8) . ?
C34 H34 0.95 . ?
C35 C36 1.378(7) . ?
C35 H35 0.95 . ?
C36 H36 0.95 . ?
C41 C46 1.388(7) . ?
C41 C42 1.398(7) . ?
C42 C43 1.387(7) . ?
C42 H42 0.95 . ?
C43 C44 1.378(8) . ?
C43 H43 0.95 . ?
C44 C45 1.380(7) . ?
C44 H44 0.95 . ?
C45 C46 1.388(7) . ?
C45 H45 0.95 . ?
C46 H46 0.95 . ?
C51 C56 1.392(7) . ?
C51 C52 1.394(7) . ?
C52 C53 1.382(7) . ?
C52 H52 0.95 . ?
C53 C54 1.390(8) . ?
C53 H53 0.95 . ?
C54 C55 1.376(8) . ?
C54 H54 0.95 . ?
C55 C56 1.379(7) . ?
C55 H55 0.95 . ?
C56 H56 0.95 . ?

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 177.55(13) . . yes
O21 Re1 N13 86.75(15) . . ?
O1 Re1 N13 93.58(14) . . ?
O21 Re1 Cl3 88.48(10) . . ?
O1 Re1 Cl3 91.24(9) . . ?
N13 Re1 Cl3 175.08(11) . . yes
O21 Re1 Cl1 88.45(10) . . ?
O1 Re1 Cl1 89.14(9) . . ?
N13 Re1 Cl1 87.75(10) . . ?
Cl3 Re1 Cl1 93.32(4) . . ?
O21 Re1 Cl2 91.74(10) . . ?
O1 Re1 Cl2 90.70(9) . . ?
N13 Re1 Cl2 87.94(10) . . ?
Cl3 Re1 Cl2 91.01(4) . . ?
Cl1 Re1 Cl2 175.67(4) . . yes
C12 O11 C15 105.4(4) . . ?
N13 C12 O11 116.1(4) . . ?
N13 C12 C26 128.4(5) . . ?
O11 C12 C26 115.5(4) . . ?
C12 N13 C14 107.0(4) . . yes
C12 N13 Re1 123.5(3) . . yes
C14 N13 Re1 129.1(3) . . yes
N13 C14 C17 113.9(4) . . ?
N13 C14 C15 100.5(4) . . ?
C17 C14 C15 111.7(4) . . ?
N13 C14 C16 106.8(4) . . ?
C17 C14 C16 112.1(4) . . ?
C15 C14 C16 111.2(4) . . ?
O11 C15 C14 104.2(4) . . ?
O11 C15 H151 110.9 . . ?
C14 C15 H151 110.9 . . ?
O11 C15 H152 110.9 . . ?
C14 C15 H152 110.9 . . ?
H151 C15 H152 108.9 . . ?
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 127.6(3) . . yes
O21 C21 C26 124.0(4) . . ?
O21 C21 C22 119.1(5) . . ?
C26 C21 C22 116.8(5) . . ?
C23 C22 C21 121.7(5) . . ?
C23 C22 Cl22 119.8(4) . . ?
C21 C22 Cl22 118.4(4) . . ?
C22 C23 C24 119.4(5) . . ?
C22 C23 H23 120.3 . . ?
C24 C23 H23 120.3 . . ?
C25 C24 C23 121.0(5) . . ?
C25 C24 Cl24 119.3(5) . . ?
C23 C24 Cl24 119.7(4) . . ?
C24 C25 C26 119.9(5) . . ?
C24 C25 H25 120.0 . . ?
C26 C25 H25 120.0 . . ?
C21 C26 C25 121.1(5) . . ?
C21 C26 C12 120.8(5) . . ?
C25 C26 C12 118.1(5) . . ?
P1 O1 Re1 144.71(19) . . yes
O1 P1 C31 110.9(2) . . ?
O1 P1 C41 112.42(19) . . ?
C31 P1 C41 109.1(2) . . ?
O1 P1 C51 108.5(2) . . ?
C31 P1 C51 108.4(2) . . ?
C41 P1 C51 107.3(2) . . ?
C36 C31 C32 120.4(5) . . ?
C36 C31 P1 118.1(4) . . ?
C32 C31 P1 121.5(4) . . ?
C33 C32 C31 118.8(5) . . ?
C33 C32 H32 120.6 . . ?
C31 C32 H32 120.6 . . ?
C34 C33 C32 120.8(6) . . ?
C34 C33 H33 119.6 . . ?
C32 C33 H33 119.6 . . ?
C33 C34 C35 120.0(5) . . ?
C33 C34 H34 120.0 . . ?
C35 C34 H34 120.0 . . ?
C36 C35 C34 120.2(6) . . ?
C36 C35 H35 119.9 . . ?
C34 C35 H35 119.9 . . ?
C35 C36 C31 119.9(5) . . ?
C35 C36 H36 120.1 . . ?
C31 C36 H36 120.1 . . ?
C46 C41 C42 119.2(5) . . ?
C46 C41 P1 119.5(4) . . ?
C42 C41 P1 121.2(4) . . ?
C43 C42 C41 119.8(5) . . ?
C43 C42 H42 120.1 . . ?
C41 C42 H42 120.1 . . ?
C44 C43 C42 120.4(5) . . ?
C44 C43 H43 119.8 . . ?
C42 C43 H43 119.8 . . ?
C43 C44 C45 120.3(5) . . ?
C43 C44 H44 119.9 . . ?
C45 C44 H44 119.9 . . ?
C44 C45 C46 119.8(5) . . ?
C44 C45 H45 120.1 . . ?
C46 C45 H45 120.1 . . ?
C41 C46 C45 120.5(5) . . ?
C41 C46 H46 119.7 . . ?
C45 C46 H46 119.7 . . ?
C56 C51 C52 119.7(5) . . ?
C56 C51 P1 119.1(4) . . ?
C52 C51 P1 121.0(4) . . ?
C53 C52 C51 119.8(5) . . ?
C53 C52 H52 120.1 . . ?
C51 C52 H52 120.1 . . ?
C52 C53 C54 119.9(5) . . ?
C52 C53 H53 120.0 . . ?
C54 C53 H53 120.0 . . ?
C55 C54 C53 120.4(5) . . ?
C55 C54 H54 119.8 . . ?
C53 C54 H54 119.8 . . ?
C54 C55 C56 120.1(5) . . ?
C54 C55 H55 120.0 . . ?
C56 C55 H55 120.0 . . ?
C55 C56 C51 120.1(5) . . ?
C55 C56 H56 119.9 . . ?
C51 C56 H56 119.9 . . ?

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 -10.3(6) . . . . ?
C15 O11 C12 C26 172.1(4) . . . . ?
O11 C12 N13 C14 -7.1(6) . . . . ?
C26 C12 N13 C14 170.2(5) . . . . ?
O11 C12 N13 Re1 180.0(3) . . . . ?
C26 C12 N13 Re1 -2.7(7) . . . . ?
C12 N13 C14 C17 139.7(4) . . . . ?
Re1 N13 C14 C17 -47.9(6) . . . . ?
C12 N13 C14 C15 20.2(5) . . . . ?
Re1 N13 C14 C15 -167.4(3) . . . . ?
C12 N13 C14 C16 -95.9(5) . . . . ?
Re1 N13 C14 C16 76.4(5) . . . . ?
C12 O11 C15 C14 22.6(5) . . . . ?
N13 C14 C15 O11 -25.4(5) . . . . ?
C17 C14 C15 O11 -146.5(4) . . . . ?
C16 C14 C15 O11 87.4(5) . . . . ?
Re1 O21 C21 C26 -31.5(7) . . . . ?
Re1 O21 C21 C22 152.8(4) . . . . ?
O21 C21 C22 C23 178.9(5) . . . . ?
C26 C21 C22 C23 2.9(8) . . . . ?
O21 C21 C22 Cl22 -3.3(6) . . . . ?
C26 C21 C22 Cl22 -179.3(4) . . . . ?
C21 C22 C23 C24 -3.1(8) . . . . ?
Cl22 C22 C23 C24 179.2(4) . . . . ?
C22 C23 C24 C25 1.0(8) . . . . ?
C22 C23 C24 Cl24 -177.1(4) . . . . ?
C23 C24 C25 C26 1.1(8) . . . . ?
Cl24 C24 C25 C26 179.1(4) . . . . ?
O21 C21 C26 C25 -176.5(5) . . . . ?
C22 C21 C26 C25 -0.7(7) . . . . ?
O21 C21 C26 C12 2.2(8) . . . . ?
C22 C21 C26 C12 178.0(5) . . . . ?
C24 C25 C26 C21 -1.2(8) . . . . ?
C24 C25 C26 C12 -180.0(5) . . . . ?
N13 C12 C26 C21 15.1(8) . . . . ?
O11 C12 C26 C21 -167.6(4) . . . . ?
N13 C12 C26 C25 -166.1(5) . . . . ?
O11 C12 C26 C25 11.2(7) . . . . ?
Re1 O1 P1 C31 -50.1(4) . . . . ?
Re1 O1 P1 C41 72.4(4) . . . . ?
Re1 O1 P1 C51 -169.0(3) . . . . ?
O1 P1 C31 C36 -50.0(4) . . . . ?
C41 P1 C31 C36 -174.4(4) . . . . ?
C51 P1 C31 C36 69.0(4) . . . . ?
O1 P1 C31 C32 128.9(4) . . . . ?
C41 P1 C31 C32 4.5(5) . . . . ?
C51 P1 C31 C32 -112.1(4) . . . . ?
C36 C31 C32 C33 1.3(7) . . . . ?
P1 C31 C32 C33 -177.6(4) . . . . ?
C31 C32 C33 C34 -0.9(8) . . . . ?
C32 C33 C34 C35 -1.2(9) . . . . ?
C33 C34 C35 C36 3.1(9) . . . . ?
C34 C35 C36 C31 -2.7(8) . . . . ?
C32 C31 C36 C35 0.5(7) . . . . ?
P1 C31 C36 C35 179.4(4) . . . . ?
O1 P1 C41 C46 -59.0(4) . . . . ?
C31 P1 C41 C46 64.5(4) . . . . ?
C51 P1 C41 C46 -178.2(4) . . . . ?
O1 P1 C41 C42 123.7(4) . . . . ?
C31 P1 C41 C42 -112.8(4) . . . . ?
C51 P1 C41 C42 4.5(5) . . . . ?
C46 C41 C42 C43 1.3(7) . . . . ?
P1 C41 C42 C43 178.7(4) . . . . ?
C41 C42 C43 C44 -0.4(8) . . . . ?
C42 C43 C44 C45 -0.2(8) . . . . ?
C43 C44 C45 C46 -0.2(8) . . . . ?
C42 C41 C46 C45 -1.7(7) . . . . ?
P1 C41 C46 C45 -179.1(4) . . . . ?
C44 C45 C46 C41 1.2(8) . . . . ?
O1 P1 C51 C56 -47.8(5) . . . . ?
C31 P1 C51 C56 -168.3(4) . . . . ?
C41 P1 C51 C56 73.9(4) . . . . ?
O1 P1 C51 C52 137.0(4) . . . . ?
C31 P1 C51 C52 16.5(5) . . . . ?
C41 P1 C51 C52 -101.3(4) . . . . ?
C56 C51 C52 C53 1.0(8) . . . . ?
P1 C51 C52 C53 176.1(4) . . . . ?
C51 C52 C53 C54 -0.7(8) . . . . ?
C52 C53 C54 C55 0.2(9) . . . . ?
C53 C54 C55 C56 0.1(9) . . . . ?
C54 C55 C56 C51 0.3(8) . . . . ?
C52 C51 C56 C55 -0.8(8) . . . . ?
P1 C51 C56 C55 -176.0(4) . . . . ?

_refine_diff_density_max         0.973
_refine_diff_density_min         -1.207
_refine_diff_density_rms         0.167

_shelxl_version_number           2014/6

