#------------------------------------------------------------------------------
#$Date: 2021-04-05 16:57:43 +0200 (lun 05 de abr de 2021) $
#$Revision: 263786 $
#$URL: svn://www.crystallography.net/cod/cif/7/70/67/7706763.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_7706763
loop_
_publ_author_name
'Smith, Danielle E.'
'Levason, William'
'Powell, James'
'Reid, Gillian'
_publ_section_title
;
 Synthesis, properties and structural features of molybdenum(v) oxide
 trichloride complexes with neutral chalcogenoether ligands.
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4380
_journal_page_last               4389
_journal_paper_doi               10.1039/d1dt00038a
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C5 H12 Cl3 Mo O S2'
_chemical_formula_sum            'C5 H12 Cl3 Mo O S2'
_chemical_formula_weight         354.56
_chemical_name_systematic        '[MoOCl3(MeS(CH3)2SMe)]'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive,Hygroscopic
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-12-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-12-16 deposited with the CCDC.	2021-02-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.2795(2)
_cell_length_b                   12.7576(3)
_cell_length_c                   7.6118(2)
_cell_measurement_reflns_used    4060
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      30.6270
_cell_measurement_theta_min      3.5160
_cell_volume                     1192.44(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.916
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -44.00  52.00   1.00    4.00    --  -15.60  38.00-150.00   96
  2  ω    -47.00  71.00   1.00    4.00    --  -15.60  57.00 120.00  118
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RCD3): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0304818000
_diffrn_orient_matrix_UB_12      -0.0305080000
_diffrn_orient_matrix_UB_13      -0.0603815000
_diffrn_orient_matrix_UB_21      0.0009210000
_diffrn_orient_matrix_UB_22      -0.0420640000
_diffrn_orient_matrix_UB_23      0.0609997000
_diffrn_orient_matrix_UB_31      -0.0490734000
_diffrn_orient_matrix_UB_32      -0.0197022000
_diffrn_orient_matrix_UB_33      -0.0363339000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_av_unetI/netI     0.0316
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.916
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            6824
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.916
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.010
_diffrn_reflns_theta_min         3.116
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.078
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62022
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark green'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.975
_exptl_crystal_description       block
_exptl_crystal_F_000             700
_exptl_crystal_preparation       'Slow evporation from DCM'
_exptl_crystal_recrystallization_method 'Slow evporation from DCM'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.686
_refine_diff_density_min         -0.593
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     62
_refine_ls_number_reflns         1807
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0357
_refine_ls_R_factor_gt           0.0290
_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)+(0.0253P)²+0.7877P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0580
_refine_ls_wR_factor_ref         0.0605
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1624
_reflns_number_total             1807
_reflns_threshold_expression     'I > 2σ(I)'
_iucr_refine_instructions_details
;
TITL des_moocl3dithiahept-1_a.res in Pnma
    des_moocl3dithiahept-1.res
    created by SHELXL-2018/3 at 11:34:36 on 23-Nov-2020
REM Old TITL DES_MoOCl3dithiahept-1 in Pnma
REM SHELXT solution in Pnma: R1 0.054, Rweak 0.083, Alpha 0.023
REM <I/s> 0.887 for 158 systematic absences, Orientation as input
REM Formula found by SHELXT: C5 O S2 Cl3 Mo
CELL 0.71073 12.2795 12.7576 7.6118 90 90 90
ZERR 4 0.0002 0.0003 0.0002 0 0 0
LATT 1
SYMM 0.5-X,-Y,0.5+Z
SYMM -X,0.5+Y,-Z
SYMM 0.5+X,0.5-Y,0.5-Z
SFAC C H Cl Mo O S
UNIT 20 48 12 4 4 8

L.S. 4 0 0
PLAN  20
BOND
list 4
fmap 2 53
acta
REM <olex2.extras>
REM <HklSrc "%.\\DES_MoOCl3dithiahept-1.hkl">
REM </olex2.extras>

WGHT    0.025300    0.787700
FVAR       0.35939
MO1   4    0.649161    0.250000    0.568498    10.50000    0.01196    0.00847 =
         0.01173    0.00000   -0.00055    0.00000
S1    6    0.721669    0.400180    0.753669    11.00000    0.01859    0.00898 =
         0.01468   -0.00067   -0.00184    0.00007
CL2   3    0.844047    0.250000    0.496210    10.50000    0.01317    0.01913 =
         0.01511    0.00000    0.00107    0.00000
CL1   3    0.604865    0.117158    0.367585    11.00000    0.02493    0.01276 =
         0.01819   -0.00325   -0.00447   -0.00231
O1    5    0.540273    0.250000    0.700493    10.50000    0.01539    0.01666 =
         0.02011    0.00000    0.00101    0.00000
C2    1    0.801191    0.350548    0.937158    11.00000    0.01958    0.01138 =
         0.01762   -0.00281   -0.00585    0.00074
AFIX  23
H2A   2    0.875138    0.339628    0.896247    11.00000   -1.20000
H2B   2    0.803886    0.404883    1.026193    11.00000   -1.20000
AFIX   0
C3    1    0.763376    0.250000    1.025031    10.50000    0.02086    0.01216 =
         0.01471    0.00000   -0.00261    0.00000
AFIX  23
H3A   2    0.789066    0.250000    1.145538    10.50000   -1.20000
H3B   2    0.684409    0.249999    1.028325    10.50000   -1.20000
AFIX   0
C1    1    0.604562    0.451874    0.866587    11.00000    0.02430    0.01893 =
         0.02541   -0.00798   -0.00190    0.00986
AFIX 137
H1A   2    0.551597    0.474828    0.782175    11.00000   -1.50000
H1B   2    0.626282    0.510091    0.938404    11.00000   -1.50000
H1C   2    0.573365    0.398264    0.939389    11.00000   -1.50000
AFIX   0
HKLF 4




REM  des_moocl3dithiahept-1_a.res in Pnma
REM wR2 = 0.0605, GooF = S = 1.074, Restrained GooF = 1.074 for all data
REM R1 = 0.0290 for 1624 Fo > 4sig(Fo) and 0.0357 for all 1807 data
REM 62 parameters refined using 0 restraints

END  
     
WGHT      0.0253      0.7878 

REM Highest difference peak  0.686,  deepest hole -0.593,  1-sigma level  0.121
Q1    1   0.5634  0.2500  0.6176  10.50000  0.05    0.69
Q2    1   0.6425  0.1815  0.4572  11.00000  0.05    0.57
Q3    1   0.6049  0.2500  0.4868  10.50000  0.05    0.57
Q4    1   0.7665  0.3917  0.8342  11.00000  0.05    0.54
Q5    1   0.7013  0.2500  0.6612  10.50000  0.05    0.53
Q6    1   0.7445  0.2500  0.5251  10.50000  0.05    0.51
Q7    1   0.6585  0.2049  0.6960  11.00000  0.05    0.51
Q8    1   0.8354  0.2500  0.3768  10.50000  0.05    0.51
Q9    1   0.7544  0.2500  0.5644  10.50000  0.05    0.50
Q10   1   0.6829  0.2500  0.4916  10.50000  0.05    0.47
Q11   1   0.6064  0.1233  0.4711  11.00000  0.05    0.47
Q12   1   0.6782  0.1208  0.4142  11.00000  0.05    0.46
Q13   1   0.8216  0.2500  0.6128  10.50000  0.05    0.46
Q14   1   0.8874  0.2500  0.5802  10.50000  0.05    0.46
Q15   1   0.6148  0.2500  0.6941  10.50000  0.05    0.46
Q16   1   0.6796  0.4167  0.8386  11.00000  0.05    0.46
Q17   1   0.6021  0.3862  1.1385  11.00000  0.05    0.43
Q18   1   0.4916  0.2500  0.6295  10.50000  0.05    0.43
Q19   1   0.5407  0.2500  0.9391  10.50000  0.05    0.43
Q20   1   0.6469  0.2500  0.9227  10.50000  0.05    0.42

  REM The information below was added by Olex2.
  REM
  REM R1 = 0.0290 for 1624 Fo > 4sig(Fo) and 0.0357 for all 7322 data
  REM n/a parameters refined using n/a restraints
  REM Highest difference peak 0.69, deepest hole -0.59
  REM Mean Shift 0, Max Shift -0.001.

  REM +++ Tabular Listing of Refinement Information +++
  REM R1_all = 0.0357
  REM R1_gt = 0.0290
  REM wR_ref = 0.0605
  REM GOOF = 1.074
  REM Shift_max = -0.001
  REM Shift_mean = 0
  REM Reflections_all = 7322
  REM Reflections_gt = 1624
  REM Parameters = n/a
  REM Hole = -0.59
  REM Peak = 0.69
  REM Flack = n/a

  
;
_cod_data_source_file            d1dt00038a2.cif
_cod_data_source_block           des_moocl3dithiahept-1
_cod_depositor_comments
'Adding full bibliography for 7706761--7706769.cif.'
_cod_database_code               7706763
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         MoOCl3C5H15S2
_chemical_oxdiff_usercomment     'Small green crystal'
_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.
;
_reflns_odcompleteness_completeness 99.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.64
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C2(H2a,H2b), C3(H3a,H3b)
2.b Idealised Me refined as rotating group:
 C1(H1a,H1b,H1c)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.838
_oxdiff_exptl_absorpt_empirical_full_min 0.718
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.64916(2) 0.250000 0.56850(3) 0.01072(8) Uani 1 2 d S T P . .
S1 S 0.72167(4) 0.40018(5) 0.75367(7) 0.01408(12) Uani 1 1 d . . . . .
Cl2 Cl 0.84405(5) 0.250000 0.49621(10) 0.01580(16) Uani 1 2 d S T P . .
Cl1 Cl 0.60486(4) 0.11716(5) 0.36758(7) 0.01863(13) Uani 1 1 d . . . . .
O1 O 0.54027(16) 0.250000 0.7005(3) 0.0174(5) Uani 1 2 d S T P . .
C2 C 0.80119(17) 0.35055(19) 0.9372(3) 0.0162(5) Uani 1 1 d . . . . .
H2A H 0.875138 0.339628 0.896247 0.019 Uiso 1 1 calc R . . . .
H2B H 0.803886 0.404883 1.026193 0.019 Uiso 1 1 calc R . . . .
C3 C 0.7634(2) 0.250000 1.0250(4) 0.0159(6) Uani 1 2 d S T P . .
H3A H 0.789066 0.250000 1.145538 0.019 Uiso 1 2 calc RS T P . .
H3B H 0.684409 0.249999 1.028325 0.019 Uiso 1 2 calc RS T P . .
C1 C 0.60456(19) 0.4519(2) 0.8666(3) 0.0229(5) Uani 1 1 d . . . . .
H1A H 0.551597 0.474828 0.782175 0.034 Uiso 1 1 calc GR . . . .
H1B H 0.626282 0.510091 0.938404 0.034 Uiso 1 1 calc GR . . . .
H1C H 0.573365 0.398264 0.939389 0.034 Uiso 1 1 calc GR . . . .
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
Mo1 0.01196(12) 0.00847(15) 0.01173(13) 0.000 -0.00055(9) 0.000
S1 0.0186(2) 0.0090(3) 0.0147(2) -0.0007(2) -0.00184(19) 0.0001(2)
Cl2 0.0132(3) 0.0191(4) 0.0151(3) 0.000 0.0011(3) 0.000
Cl1 0.0249(3) 0.0128(3) 0.0182(2) -0.0033(2) -0.0045(2) -0.0023(2)
O1 0.0154(10) 0.0167(13) 0.0201(11) 0.000 0.0010(9) 0.000
C2 0.0196(10) 0.0114(12) 0.0176(10) -0.0028(9) -0.0058(8) 0.0007(9)
C3 0.0209(14) 0.0122(17) 0.0147(13) 0.000 -0.0026(12) 0.000
C1 0.0243(11) 0.0189(14) 0.0254(12) -0.0080(11) -0.0019(10) 0.0099(10)
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'
Mo Mo -1.6832 0.6857 '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
S1 Mo1 S1 97.94(3) 7_565 . ?
Cl2 Mo1 S1 77.449(17) . . ?
Cl2 Mo1 S1 77.449(17) . 7_565 ?
Cl1 Mo1 S1 84.153(19) . 7_565 ?
Cl1 Mo1 S1 171.02(2) . . ?
Cl1 Mo1 S1 171.02(2) 7_565 7_565 ?
Cl1 Mo1 S1 84.152(19) 7_565 . ?
Cl1 Mo1 Cl2 94.581(19) . . ?
Cl1 Mo1 Cl2 94.581(19) 7_565 . ?
Cl1 Mo1 Cl1 92.47(3) . 7_565 ?
O1 Mo1 S1 86.95(5) . . ?
O1 Mo1 S1 86.96(5) . 7_565 ?
O1 Mo1 Cl2 156.03(8) . . ?
O1 Mo1 Cl1 101.90(5) . 7_565 ?
O1 Mo1 Cl1 101.90(5) . . ?
C2 S1 Mo1 110.60(8) . . ?
C1 S1 Mo1 105.14(9) . . ?
C1 S1 C2 100.94(11) . . ?
C3 C2 S1 117.91(17) . . ?
C2 C3 C2 115.2(3) 7_565 . ?
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
Mo1 S1 2.5397(6) 7_565 ?
Mo1 S1 2.5397(6) . ?
Mo1 Cl2 2.4555(7) . ?
Mo1 Cl1 2.3467(6) 7_565 ?
Mo1 Cl1 2.3467(6) . ?
Mo1 O1 1.673(2) . ?
S1 C2 1.818(2) . ?
S1 C1 1.800(2) . ?
C2 C3 1.519(3) . ?
