#------------------------------------------------------------------------------
#$Date: 2024-07-05 18:55:56 +0200 (Fri 05 de Jul de 2024) $
#$Revision: 293134 $
#$URL: svn://www.crystallography.net/cod/cif/7/71/60/7716097.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_7716097
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_absolute_configuration rm/ad/rmad/syn/unk/.
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C6 O2 S6'
_chemical_formula_sum            'C6 O2 S6'
_chemical_formula_weight         296.42
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_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
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.925(2)
_cell_length_b                   26.902(3)
_cell_length_c                   3.9069(4)
_cell_measurement_reflns_used    985
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.9289
_cell_measurement_theta_min      2.7309
_cell_measurement_wavelength     0.710730
_cell_volume                     1884.0(4)
_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, 2020)'
_computing_structure_refinement  'SHELXL-2018_3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018_2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'APEXII Bruker-AXS'
_diffrn_measurement_method       'CCD rotation images, thin slices'
_diffrn_orient_matrix_UB_11      -0.0900387
_diffrn_orient_matrix_UB_12      0.0434120
_diffrn_orient_matrix_UB_13      -0.0193405
_diffrn_orient_matrix_UB_21      0.1810534
_diffrn_orient_matrix_UB_22      -0.0079811
_diffrn_orient_matrix_UB_23      -0.0257313
_diffrn_orient_matrix_UB_31      -0.1569256
_diffrn_orient_matrix_UB_32      -0.0341166
_diffrn_orient_matrix_UB_33      -0.0185906
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0216
_diffrn_reflns_av_unetI/netI     0.0396
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_number            1909
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.429
_diffrn_reflns_theta_min         2.731
_diffrn_source_current           1.0
_diffrn_source_power             50.0
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.412
_exptl_absorpt_correction_T_max  0.932
_exptl_absorpt_correction_T_min  0.744
_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    2.090
_exptl_crystal_description       stick
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.720
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.373
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details
;
Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.0(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_matrix_type           full
_refine_ls_number_parameters     65
_refine_ls_number_reflns         1020
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0340
_refine_ls_R_factor_gt           0.0312
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0384P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0679
_refine_ls_wR_factor_ref         0.0692
_reflns_Friedel_coverage         0.686
_reflns_Friedel_fraction_full    0.924
_reflns_Friedel_fraction_max     0.916
_reflns_number_gt                957
_reflns_number_total             1020
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d4dt00694a2.cif
_cod_data_source_block           compound2
_cod_depositor_comments
'Adding full bibliography for 7716097--7716104.cif.'
_cod_database_code               7716097
_shelx_res_file
;
TITL KY097 [Space group= Fdd2]
    job.res
    created by SHELXL-2018/3 at 12:03:14 on 16-Jun-2021
REM Old TITL KY097
REM SHELXT solution in Fdd2: R1 0.055, Rweak 0.019, Alpha 0.000
REM <I/s>   0.591 for   33 systematic absences,  Orientation a'=b, b'=c, c'=a
REM Flack x =  0.420 ( 0.186 ) from   345 Parsons' quotients
REM Formula found by SHELXT:  C3 O S3

CELL  0.71073  17.9252  26.9019   3.9069   90.000   90.000   90.000
ZERR    8.000   0.0020   0.0030   0.0004    0.000    0.000    0.000
LATT  -4
SYMM  - X, - Y,   Z
SYMM  1/4 + X, 1/4 - Y, 1/4 + Z
SYMM  1/4 - X, 1/4 + Y, 1/4 + Z
SFAC  C    O    S
UNIT   48.00   16.00   48.00
MERG   2
FMAP   2
twin
SIZE     0.05   0.09   0.72
ACTA
CONF
LIST   4
WPDB  -2
L.S.   4
TEMP  -123.00
WGHT    0.038400
BASF   0.03739
FVAR       0.28000
O1    2    0.725213    0.587736    0.208423    11.00000    0.02107    0.02048 =
         0.04063    0.00298    0.00887   -0.00117
C2    1    0.672531    0.567670    0.344776    11.00000    0.01714    0.01727 =
         0.02262    0.00222   -0.00196   -0.00041
C3    1    0.545011    0.547228    0.636378    11.00000    0.01488    0.01517 =
         0.01785   -0.00105    0.00058   -0.00508
C4    1    0.581949    0.504078    0.633366    11.00000    0.01076    0.01792 =
         0.01661    0.00141   -0.00283   -0.00328
S1    3    0.588921    0.599178    0.460337    11.00000    0.01523    0.01349 =
         0.02544    0.00101    0.00056   -0.00134
S2    3    0.670186    0.502948    0.445005    11.00000    0.01183    0.01577 =
         0.02518    0.00239   -0.00028   -0.00032
S3    3    0.547054    0.447397    0.792420    11.00000    0.01440    0.01640 =
         0.02338    0.00568   -0.00233   -0.00240
HKLF    4




REM  KY097 [Space group= Fdd2]
REM wR2 = 0.0692, GooF = S = 1.056, Restrained GooF = 1.055 for all data
REM R1 = 0.0312 for 957 Fo > 4sig(Fo) and 0.0340 for all 1020 data
REM 65 parameters refined using 1 restraints

END

WGHT      0.0432      0.0000

REM Highest difference peak  0.373,  deepest hole -0.323,  1-sigma level  0.075
Q1    1   0.5656  0.4773  0.6840  11.00000  0.05    0.37
Q2    1   0.6737  0.5278  0.2905  11.00000  0.05    0.34
Q3    1   0.6842  0.5005  0.1786  11.00000  0.05    0.29
Q4    1   0.5611  0.5690  0.5514  11.00000  0.05    0.27
Q5    1   0.5492  0.4466  1.0642  11.00000  0.05    0.27
Q6    1   0.5486  0.4409  0.5541  11.00000  0.05    0.26
Q7    1   0.6745  0.5395  0.5068  11.00000  0.05    0.26
Q8    1   0.5477  0.5210  0.5479  11.00000  0.05    0.26
Q9    1   0.5822  0.5784  0.6754  11.00000  0.05    0.26
Q10   1   0.5486  0.5316  0.4896  11.00000  0.05    0.25
Q11   1   0.5430  0.4713  0.9646  11.00000  0.05    0.25
Q12   1   0.7573  0.5705  0.1997  11.00000  0.05    0.24
Q13   1   0.6767  0.4993  0.6980  11.00000  0.05    0.23
Q14   1   0.5802  0.5120  0.8056  11.00000  0.05    0.23
Q15   1   0.5878  0.5989  0.2091  11.00000  0.05    0.23
Q16   1   0.5917  0.5998  0.7048  11.00000  0.05    0.23
Q17   1   0.6658  0.4829  0.2638  11.00000  0.05    0.22
Q18   1   0.5500  0.4196  0.6396  11.00000  0.05    0.22
Q19   1   0.6876  0.5884 -0.2107  11.00000  0.05    0.21
Q20   1   0.6073  0.6290  0.5885  11.00000  0.05    0.20
;
_shelx_res_checksum              42810
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'x+1/4, -y+1/4, z+1/4'
'-x+1/4, y+1/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'x+1/4, -y+3/4, z+3/4'
'-x+1/4, y+3/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'x+3/4, -y+1/4, z+3/4'
'-x+3/4, y+1/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'x+3/4, -y+3/4, z+1/4'
'-x+3/4, y+3/4, z+1/4'
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
O1 O 0.72521(16) 0.58774(11) 0.2084(10) 0.0274(8) Uani 1 1 d . . . . .
C2 C 0.6725(2) 0.56767(16) 0.3448(13) 0.0190(9) Uani 1 1 d . . . . .
C3 C 0.5450(2) 0.54723(15) 0.6364(11) 0.0160(9) Uani 1 1 d . . . . .
C4 C 0.5819(2) 0.50408(15) 0.6334(12) 0.0151(9) Uani 1 1 d . . . . .
S1 S 0.58892(5) 0.59918(4) 0.4603(3) 0.0181(3) Uani 1 1 d . . . . .
S2 S 0.67019(5) 0.50295(4) 0.4450(3) 0.0176(3) Uani 1 1 d . . . . .
S3 S 0.54705(6) 0.44740(4) 0.7924(3) 0.0181(3) Uani 1 1 d . . . . .
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
O1 0.0211(16) 0.0205(16) 0.041(2) 0.0030(17) 0.0089(18) -0.0012(13)
C2 0.017(2) 0.017(2) 0.023(2) 0.0022(19) -0.0020(18) -0.0004(16)
C3 0.0149(19) 0.015(2) 0.018(2) -0.0011(18) 0.0006(17) -0.0051(16)
C4 0.0108(19) 0.018(2) 0.017(2) 0.0014(17) -0.0028(17) -0.0033(15)
S1 0.0152(5) 0.0135(5) 0.0254(6) 0.0010(5) 0.0006(5) -0.0013(4)
S2 0.0118(5) 0.0158(5) 0.0252(5) 0.0024(5) -0.0003(5) -0.0003(4)
S3 0.0144(5) 0.0164(5) 0.0234(5) 0.0057(4) -0.0023(5) -0.0024(4)
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'
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
O1 C2 S1 123.8(3) . . ?
O1 C2 S2 123.3(3) . . ?
S1 C2 S2 112.9(2) . . ?
C4 C3 S1 117.9(3) . . ?
C4 C3 S3 122.5(3) . 2_665 ?
S1 C3 S3 119.5(2) . 2_665 ?
C3 C4 S2 117.9(3) . . ?
C3 C4 S3 125.0(3) . . ?
S2 C4 S3 117.1(2) . . ?
C3 S1 C2 95.6(2) . . ?
C4 S2 C2 95.6(2) . . ?
C4 S3 C3 98.00(19) . 2_665 ?
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
O1 C2 1.211(5) . ?
C2 S1 1.780(4) . ?
C2 S2 1.785(4) . ?
C3 C4 1.336(6) . ?
C3 S1 1.745(4) . ?
C3 S3 1.765(4) 2_665 ?
C4 S2 1.745(4) . ?
C4 S3 1.761(4) . ?
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
S1 C3 C4 S2 -1.4(5) . . . . ?
S3 C3 C4 S2 175.6(3) 2_665 . . . ?
S1 C3 C4 S3 -179.1(3) . . . . ?
S3 C3 C4 S3 -2.1(6) 2_665 . . . ?
C4 C3 S1 C2 -0.2(4) . . . . ?
S3 C3 S1 C2 -177.3(3) 2_665 . . . ?
O1 C2 S1 C3 -179.3(4) . . . . ?
S2 C2 S1 C3 1.6(3) . . . . ?
C3 C4 S2 C2 2.2(4) . . . . ?
S3 C4 S2 C2 -179.9(3) . . . . ?
O1 C2 S2 C4 178.7(4) . . . . ?
S1 C2 S2 C4 -2.2(3) . . . . ?
C3 C4 S3 C3 41.2(4) . . . 2_665 ?
S2 C4 S3 C3 -136.5(3) . . . 2_665 ?
