#------------------------------------------------------------------------------
#$Date: 2024-07-05 19:55:56 +0300 (Fri, 05 Jul 2024) $
#$Revision: 293134 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/61/7716100.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7716100
loop_
_publ_author_name
'Youssef, Khalil'
'Poidevin, Corentin'
'Vacher, Antoine'
'Fihey, Arnaud'
'Le Gal, Yann'
'Roisnel, Thierry'
'Lorcy, Dominique'
_publ_section_title
;
 Radical and diradical states of bis(molybdenocene dithiolene) complexes.
;
_journal_issue                   23
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9763
_journal_page_last               9776
_journal_paper_doi               10.1039/d4dt00694a
_journal_volume                  53
_journal_year                    2024
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C8 H2 O2 S4'
_chemical_formula_sum            'C8 H2 O2 S4'
_chemical_formula_weight         258.34
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_update_record
;
2024-02-15 deposited with the CCDC.	2024-05-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.310(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   3.8723(7)
_cell_length_b                   11.708(2)
_cell_length_c                   9.9274(17)
_cell_measurement_reflns_used    2518
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.5561
_cell_measurement_theta_min      2.6901
_cell_measurement_wavelength     0.710730
_cell_volume                     450.07(14)
_computing_cell_refinement       'APEX3 (Bruker, 2015)'
_computing_data_collection       'Bruker APEX3 (Bruker, 2015)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_molecular_graphics
;
   'SXGRAPH (L. Farrugia, 1999), Mercury (CSD, 2020)'
;
_computing_publication_material  'CRYSCALC (T. Roisnel, local program, 2023)'
_computing_structure_refinement  'SHELXL-2019_2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 CMOS-PHOTON70
_diffrn_detector_area_resol_mean 7.39
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'D8 VENTURE Bruker AXS'
_diffrn_measurement_method       'rotation images'
_diffrn_orient_matrix_UB_11      -0.1607493
_diffrn_orient_matrix_UB_12      0.0657956
_diffrn_orient_matrix_UB_13      0.0136080
_diffrn_orient_matrix_UB_21      0.0055770
_diffrn_orient_matrix_UB_22      -0.0136610
_diffrn_orient_matrix_UB_23      0.0994222
_diffrn_orient_matrix_UB_31      0.2020445
_diffrn_orient_matrix_UB_32      0.0527249
_diffrn_orient_matrix_UB_33      0.0087788
_diffrn_radiation_monochromator  'multilayer monochromator'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Incoatec microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0401
_diffrn_reflns_av_unetI/netI     0.0408
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            3667
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.610
_diffrn_reflns_theta_min         2.051
_diffrn_source_current           1.00
_diffrn_source_power             50.0
_diffrn_source_voltage           50.00
_exptl_absorpt_coefficient_mu    1.016
_exptl_absorpt_correction_T_max  0.980
_exptl_absorpt_correction_T_min  0.778
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  [Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.906
_exptl_crystal_description       stick
_exptl_crystal_F_000             260
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.430
_refine_diff_density_min         -0.384
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     65
_refine_ls_number_reflns         1019
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0376
_refine_ls_R_factor_gt           0.0344
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0399P)²+0.5000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0826
_refine_ls_wR_factor_ref         0.0846
_reflns_number_gt                963
_reflns_number_total             1019
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d4dt00694a2.cif
_cod_data_source_block           compound5
_cod_depositor_comments
'Adding full bibliography for 7716097--7716104.cif.'
_cod_original_cell_volume        450.06(14)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7716100
_shelx_res_file
;
TITL Y803 [Space group= P21/c]
    job.res
    created by SHELXL-2019/2 at 18:03:00 on 23-Jun-2023
REM Old TITL Y803
REM SHELXT solution in Pc: R1 0.145, Rweak 0.026, Alpha 0.017
REM <I/s>   0.671 for   44 systematic absences,  Orientation as input
REM Flack x =  0.451 ( 0.053 ) from   593 Parsons' quotients
REM Formula found by SHELXT:  C11 O3 S2

CELL  0.71073   3.8723  11.7076   9.9274   90.000   90.310   90.000
ZERR    2.000   0.0007   0.0020   0.0017    0.000    0.007    0.000
LATT   1
SYMM  - X, 1/2 + Y, 1/2 - Z
SFAC  C    H    O    S
UNIT  16   4    4    8
MERG   2
TWIN   -1.00  0.00  0.00  0.00 -1.00  0.00  0.02  0.00  1.00   2
FMAP   2
PLAN   20
ACTA
BOND   $H
CONF
LIST   4
WPDB  -2
L.S.   4
TEMP  -123.00
WGHT    0.039900    0.500000
BASF   0.28552
FVAR       0.80469
S1    4    0.636403    0.695557    0.292943    11.00000    0.02810    0.01778 =
         0.01521    0.00262    0.00475    0.00040
S2    4    0.832317    0.458965    0.217227    11.00000    0.02308    0.02112 =
         0.01317   -0.00125    0.00586    0.00011
O1    3    0.908257    0.639311    0.060393    11.00000    0.04211    0.02899 =
         0.01905    0.00309    0.01120   -0.00387
C2    1    0.811393    0.604737    0.167578    11.00000    0.02198    0.02415 =
         0.01530    0.00068    0.00395   -0.00463
C3    1    0.553480    0.588921    0.411551    11.00000    0.01618    0.01820 =
         0.01339    0.00149   -0.00183   -0.00250
C4    1    0.653176    0.478106    0.377150    11.00000    0.01354    0.02231 =
         0.01135   -0.00216    0.00085   -0.00099
C5    1    0.603273    0.387749    0.465804    11.00000    0.01860    0.01761 =
         0.01478   -0.00273    0.00140    0.00075
AFIX  43
H5    2    0.674019    0.312463    0.443307    11.00000   -1.20000
AFIX   0
HKLF    4




REM  Y803 [Space group= P21/c]
REM wR2 = 0.0846, GooF = S = 1.017, Restrained GooF = 1.017 for all data
REM R1 = 0.0344 for 963 Fo > 4sig(Fo) and 0.0376 for all 1019 data
REM 65 parameters refined using 0 restraints

END

WGHT      0.0321      0.3197

REM Highest difference peak  0.430,  deepest hole -0.384,  1-sigma level  0.093
Q1    1   0.7874  0.5481  0.1990  11.00000  0.05    0.43
Q2    1   0.5606  0.6415  0.3493  11.00000  0.05    0.39
Q3    1   0.8745  0.7082  0.3432  11.00000  0.05    0.35
Q4    1   0.6020  0.4523  0.1734  11.00000  0.05    0.35
Q5    1   0.6541  0.4461  0.4267  11.00000  0.05    0.32
Q6    1   0.7202  0.4714  0.3432  11.00000  0.05    0.30
Q7    1   0.7210  0.6400  0.2316  11.00000  0.05    0.29
Q8    1   0.7658  0.4382  0.1252  11.00000  0.05    0.29
Q9    1   0.7727  0.5017  0.1414  11.00000  0.05    0.29
Q10   1   0.5120  0.6087  0.4761  11.00000  0.05    0.29
Q11   1   0.9932  0.5427  0.0060  11.00000  0.05    0.28
Q12   1   0.6856  0.4657  0.2456  11.00000  0.05    0.28
Q13   1   1.0071  0.6055  0.1288  11.00000  0.05    0.26
Q14   1   0.8236  0.5776  0.0776  11.00000  0.05    0.25
Q15   1   0.5486  0.3838  0.3793  11.00000  0.05    0.25
Q16   1   0.5586  0.5110  0.1795  11.00000  0.05    0.24
Q17   1   0.9269  0.4534  0.3015  11.00000  0.05    0.24
Q18   1   0.6185  0.5292  0.3972  11.00000  0.05    0.23
Q19   1   0.8417  0.2506  0.2784  11.00000  0.05    0.22
Q20   1   0.8304  0.6014  0.0018  11.00000  0.05    0.22
;
_shelx_res_checksum              10403
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
S1 S 0.6364(2) 0.69556(6) 0.29294(7) 0.0203(2) Uani 1 1 d . . . . .
S2 S 0.8323(2) 0.45896(5) 0.21723(7) 0.01910(19) Uani 1 1 d . . . . .
O1 O 0.9083(7) 0.63931(19) 0.0604(2) 0.0300(6) Uani 1 1 d . . . . .
C2 C 0.8114(8) 0.6047(3) 0.1676(3) 0.0205(6) Uani 1 1 d . . . . .
C3 C 0.5535(8) 0.5889(2) 0.4116(3) 0.0159(6) Uani 1 1 d . . . . .
C4 C 0.6532(8) 0.4781(2) 0.3772(3) 0.0157(5) Uani 1 1 d . . . . .
C5 C 0.6033(8) 0.3877(2) 0.4658(3) 0.0170(6) Uani 1 1 d . . . . .
H5 H 0.674019 0.312463 0.443307 0.020 Uiso 1 1 calc R U . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
S1 0.0281(4) 0.0178(3) 0.0152(3) 0.0026(2) 0.0047(3) 0.0004(3)
S2 0.0231(4) 0.0211(3) 0.0132(3) -0.0012(3) 0.0059(3) 0.0001(3)
O1 0.0421(15) 0.0290(12) 0.0191(10) 0.0031(8) 0.0112(11) -0.0039(11)
C2 0.0220(15) 0.0242(15) 0.0153(12) 0.0007(10) 0.0040(12) -0.0046(13)
C3 0.0162(14) 0.0182(13) 0.0134(12) 0.0015(10) -0.0018(11) -0.0025(11)
C4 0.0135(14) 0.0223(14) 0.0113(11) -0.0022(10) 0.0009(11) -0.0010(12)
C5 0.0186(14) 0.0176(13) 0.0148(11) -0.0027(10) 0.0014(11) 0.0007(12)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
C3 S1 C2 96.71(13) . . ?
C4 S2 C2 96.36(13) . . ?
O1 C2 S1 122.8(2) . . ?
O1 C2 S2 123.7(2) . . ?
S1 C2 S2 113.44(14) . . ?
C5 C3 C4 121.3(3) 3_666 . ?
C5 C3 S1 122.2(2) 3_666 . ?
C4 C3 S1 116.55(19) . . ?
C5 C4 C3 120.8(2) . . ?
C5 C4 S2 122.3(2) . . ?
C3 C4 S2 116.9(2) . . ?
C4 C5 C3 117.9(3) . 3_666 ?
C4 C5 H5 121.1 . . ?
C3 C5 H5 121.1 3_666 . ?
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
S1 C3 1.747(3) . ?
S1 C2 1.774(3) . ?
S2 C4 1.750(3) . ?
S2 C2 1.778(3) . ?
O1 C2 1.200(3) . ?
C3 C5 1.390(3) 3_666 ?
C3 C4 1.397(4) . ?
C4 C5 1.390(4) . ?
C5 H5 0.9500 . ?
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
C3 S1 C2 O1 179.1(3) . . . . ?
C3 S1 C2 S2 -1.5(2) . . . . ?
C4 S2 C2 O1 179.9(3) . . . . ?
C4 S2 C2 S1 0.5(2) . . . . ?
C2 S1 C3 C5 -177.6(3) . . . 3_666 ?
C2 S1 C3 C4 2.4(3) . . . . ?
C5 C3 C4 C5 -1.0(5) 3_666 . . . ?
S1 C3 C4 C5 178.9(2) . . . . ?
C5 C3 C4 S2 177.6(2) 3_666 . . . ?
S1 C3 C4 S2 -2.5(3) . . . . ?
C2 S2 C4 C5 179.7(3) . . . . ?
C2 S2 C4 C3 1.2(3) . . . . ?
C3 C4 C5 C3 1.0(5) . . . 3_666 ?
S2 C4 C5 C3 -177.5(2) . . . 3_666 ?
