#------------------------------------------------------------------------------
#$Date: 2021-04-05 17:57:43 +0300 (Mon, 05 Apr 2021) $
#$Revision: 263786 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/67/7706765.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_7706765
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(CH2)3SMe)]'
_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
_audit_creation_date             2020-06-12
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-12-17 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                   12.2610(2)
_cell_length_b                   12.7705(2)
_cell_length_c                   7.60850(10)
_cell_measurement_reflns_used    13406
_cell_measurement_temperature    99.98(18)
_cell_measurement_theta_max      31.4210
_cell_measurement_theta_min      4.2490
_cell_volume                     1191.33(3)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.98(18)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.945
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -72.00  17.00   1.00    1.00    --  -10.30 -60.00  30.00   89
  2  ω    -82.00   3.00   1.00    1.00    --  -10.30 -60.00-180.00   85
  3  ω    -65.00 -30.00   1.00    1.00    --  -10.30 -60.00   0.00   35
  4  ω    -98.00 -38.00   1.00    1.00    --  -10.30   0.00-180.00   60
  5  ω    -14.00  78.00   1.00    1.00    --  -10.30   0.00-180.00   92
  6  ω    -33.00  48.00   1.00    1.00    --  -10.30  57.00 -60.00   81
;
_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      -0.0345891000
_diffrn_orient_matrix_UB_12      -0.0014842000
_diffrn_orient_matrix_UB_13      0.0444754000
_diffrn_orient_matrix_UB_21      0.0463652000
_diffrn_orient_matrix_UB_22      -0.0002376000
_diffrn_orient_matrix_UB_23      0.0332200000
_diffrn_orient_matrix_UB_31      -0.0004705000
_diffrn_orient_matrix_UB_32      0.0932566000
_diffrn_orient_matrix_UB_33      0.0008005000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0365
_diffrn_reflns_av_unetI/netI     0.0182
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.945
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            18361
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.945
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.503
_diffrn_reflns_theta_min         3.151
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.080
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60274
_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 yellow'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.977
_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          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.375
_refine_diff_density_min         -0.530
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     62
_refine_ls_number_reflns         1948
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0194
_refine_ls_R_factor_gt           0.0187
_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)+(0.0158P)²+0.9071P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0424
_refine_ls_wR_factor_ref         0.0428
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1909
_reflns_number_total             1948
_reflns_threshold_expression     'I > 2σ(I)'
_iucr_refine_instructions_details
;
TITL jp20-1_a.res in Pnma
    jp20-1.res
    created by SHELXL-2018/3 at 11:09:56 on 12-Jun-2020
REM Old TITL JP20 - 1 in Pna2(1)
REM SHELXT solution in Pnma: R1 0.044, Rweak 0.007, Alpha 0.030
REM <I/s> 2.424 for 162 systematic absences, Orientation a'=-a, b'=c, c'=b
REM Formula found by SHELXT: C5 O Cl5 Mo
CELL 0.71073 12.261 12.7705 7.6085 90 90 90
ZERR 4 0.0002 0.0002 0.0001 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
PLAN  4
SIZE 0.2 0.3 0.3
BOND
LIST 4
MORE -1
BOND $H
CONF
fmap 2
acta
REM <olex2.extras>
REM <HklSrc "%.\\JP20%20-%201.hkl">
REM </olex2.extras>

WGHT    0.015800    0.907100
FVAR       0.42708
MO1   4    0.350626    0.750000    0.431711    10.50000    0.00963    0.00959 =
         0.00939    0.00000   -0.00039    0.00000
S1    6    0.278080    0.600024    0.246488    11.00000    0.01694    0.01017 =
         0.01227   -0.00072   -0.00170   -0.00033
CL1   3    0.155593    0.750000    0.504137    10.50000    0.01121    0.02127 =
         0.01320    0.00000    0.00100    0.00000
CL2   3    0.394798    0.882711    0.632501    11.00000    0.02310    0.01434 =
         0.01625   -0.00345   -0.00452   -0.00230
O1    5    0.459898    0.750000    0.299820    10.50000    0.01305    0.01847 =
         0.01911    0.00000    0.00229    0.00000
C2    1    0.198734    0.649451    0.063000    11.00000    0.01690    0.01368 =
         0.01486   -0.00211   -0.00524   -0.00008
AFIX  23
H2A   2    0.196098    0.595159   -0.026058    11.00000   -1.20000
H2B   2    0.124642    0.660430    0.103719    11.00000   -1.20000
AFIX   0
C3    1    0.236931    0.750000   -0.024851    10.50000    0.02213    0.01659 =
         0.01092    0.00000   -0.00135    0.00000
AFIX  23
H3A   2    0.316025    0.750000   -0.027588    10.50000   -1.20000
H3B   2    0.211518    0.750001   -0.145584    10.50000   -1.20000
AFIX   0
C1    1    0.395355    0.548109    0.133851    11.00000    0.02205    0.02110 =
         0.02490   -0.00870   -0.00249    0.00964
AFIX 137
H1A   2    0.427102    0.601725    0.061711    11.00000   -1.50000
H1B   2    0.373451    0.490298    0.061334    11.00000   -1.50000
H1C   2    0.448044    0.524622    0.218449    11.00000   -1.50000
AFIX   0
HKLF 4




REM  jp20-1_a.res in Pnma
REM wR2 = 0.0428, GooF = S = 1.106, Restrained GooF = 1.106 for all data
REM R1 = 0.0187 for 1909 Fo > 4sig(Fo) and 0.0194 for all 1948 data
REM 62 parameters refined using 0 restraints

END  
     
WGHT      0.0158      0.9071 

REM Highest difference peak  0.375,  deepest hole -0.530,  1-sigma level  0.081
Q1    1   0.3599  0.7500  0.6800  10.50000  0.05    0.37
Q2    1   0.4577  0.7500  0.4219  10.50000  0.05    0.37
Q3    1   0.4039  0.7359  0.2890  11.00000  0.05    0.33
Q4    1   0.4986  0.7500  0.3360  10.50000  0.05    0.32

  REM The information below was added by Olex2.
  REM
  REM R1 = 0.0187 for 1909 Fo > 4sig(Fo) and 0.0194 for all 19612 data
  REM n/a parameters refined using n/a restraints
  REM Highest difference peak 0.37, deepest hole -0.53
  REM Mean Shift 0, Max Shift 0.001.

  REM +++ Tabular Listing of Refinement Information +++
  REM R1_all = 0.0194
  REM R1_gt = 0.0187
  REM wR_ref = 0.0428
  REM GOOF = 1.106
  REM Shift_max = 0.001
  REM Shift_mean = 0
  REM Reflections_all = 19612
  REM Reflections_gt = 1909
  REM Parameters = n/a
  REM Hole = -0.53
  REM Peak = 0.37
  REM Flack = n/a

  
;
_cod_data_source_file            d1dt00038a2.cif
_cod_data_source_block           jp20-1
_cod_depositor_comments
'Adding full bibliography for 7706761--7706769.cif.'
_cod_database_code               7706765
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         MoOCl3C4H5P
_chemical_oxdiff_usercomment     'Green/Yellow Block Dichromic'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.681
_shelx_estimated_absorpt_t_min   0.574
_reflns_odcompleteness_completeness 99.45
_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 1.810
_oxdiff_exptl_absorpt_empirical_full_min 0.668
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 0.35063(2) 0.750000 0.43171(2) 0.00953(5) Uani 1 2 d S T P . .
S1 S 0.27808(3) 0.60002(2) 0.24649(4) 0.01313(7) Uani 1 1 d . . . . .
Cl1 Cl 0.15559(4) 0.750000 0.50414(6) 0.01522(9) Uani 1 2 d S T P . .
Cl2 Cl 0.39480(3) 0.88271(3) 0.63250(4) 0.01790(8) Uani 1 1 d . . . . .
O1 O 0.45990(12) 0.750000 0.29982(19) 0.0169(3) Uani 1 2 d S T P . .
C2 C 0.19873(12) 0.64945(11) 0.06300(17) 0.0151(3) Uani 1 1 d . . . . .
H2A H 0.196098 0.595159 -0.026058 0.018 Uiso 1 1 calc R . . . .
H2B H 0.124642 0.660430 0.103719 0.018 Uiso 1 1 calc R . . . .
C3 C 0.23693(17) 0.750000 -0.0249(2) 0.0165(4) Uani 1 2 d S T P . .
H3A H 0.316025 0.750000 -0.027588 0.020 Uiso 1 2 calc RS T P . .
H3B H 0.211518 0.750001 -0.145584 0.020 Uiso 1 2 calc RS T P . .
C1 C 0.39535(13) 0.54811(12) 0.1339(2) 0.0227(3) Uani 1 1 d . . . . .
H1A H 0.427102 0.601725 0.061711 0.034 Uiso 1 1 calc GR . . . .
H1B H 0.373451 0.490298 0.061334 0.034 Uiso 1 1 calc GR . . . .
H1C H 0.448044 0.524622 0.218449 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 0.00963(8) 0.00959(8) 0.00939(8) 0.000 -0.00039(5) 0.000
S1 0.01694(16) 0.01017(13) 0.01227(14) -0.00072(11) -0.00170(11) -0.00033(11)
Cl1 0.01121(19) 0.0213(2) 0.0132(2) 0.000 0.00100(15) 0.000
Cl2 0.02310(17) 0.01434(14) 0.01625(15) -0.00345(11) -0.00452(12) -0.00230(12)
O1 0.0130(6) 0.0185(6) 0.0191(7) 0.000 0.0023(5) 0.000
C2 0.0169(6) 0.0137(6) 0.0149(6) -0.0021(5) -0.0052(5) -0.0001(5)
C3 0.0221(10) 0.0166(8) 0.0109(8) 0.000 -0.0014(7) 0.000
C1 0.0221(7) 0.0211(7) 0.0249(7) -0.0087(6) -0.0025(6) 0.0096(6)
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 97.946(15) . 7_575 ?
Cl1 Mo1 S1 77.480(11) . 7_575 ?
Cl1 Mo1 S1 77.481(11) . . ?
Cl2 Mo1 S1 84.106(11) 7_575 . ?
Cl2 Mo1 S1 171.013(14) . . ?
Cl2 Mo1 S1 171.013(14) 7_575 7_575 ?
Cl2 Mo1 S1 84.107(11) . 7_575 ?
Cl2 Mo1 Cl1 94.517(12) . . ?
Cl2 Mo1 Cl1 94.517(12) 7_575 . ?
Cl2 Mo1 Cl2 92.555(17) . 7_575 ?
O1 Mo1 S1 87.00(3) . 7_575 ?
O1 Mo1 S1 87.00(3) . . ?
O1 Mo1 Cl1 156.14(5) . . ?
O1 Mo1 Cl2 101.87(4) . . ?
O1 Mo1 Cl2 101.87(4) . 7_575 ?
C2 S1 Mo1 110.64(4) . . ?
C1 S1 Mo1 105.20(5) . . ?
C1 S1 C2 100.95(7) . . ?
S1 C2 H2A 107.9 . . ?
S1 C2 H2B 107.9 . . ?
H2A C2 H2B 107.2 . . ?
C3 C2 S1 117.80(11) . . ?
C3 C2 H2A 107.9 . . ?
C3 C2 H2B 107.9 . . ?
C2 C3 C2 115.12(16) 7_575 . ?
C2 C3 H3A 108.5 . . ?
C2 C3 H3A 108.5 7_575 . ?
C2 C3 H3B 108.5 7_575 . ?
C2 C3 H3B 108.5 . . ?
H3A C3 H3B 107.5 . . ?
S1 C1 H1A 109.5 . . ?
S1 C1 H1B 109.5 . . ?
S1 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 S1 2.5388(3) . ?
Mo1 S1 2.5388(3) 7_575 ?
Mo1 Cl1 2.4540(5) . ?
Mo1 Cl2 2.3451(3) 7_575 ?
Mo1 Cl2 2.3451(3) . ?
Mo1 O1 1.6739(14) . ?
S1 C2 1.8149(13) . ?
S1 C1 1.8004(15) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C3 1.5215(17) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
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
Mo1 S1 C2 C3 36.54(12) . . . . ?
S1 C2 C3 C2 -84.45(18) . . . 7_575 ?
C1 S1 C2 C3 -74.45(13) . . . . ?
