#------------------------------------------------------------------------------
#$Date: 2021-04-05 16:57:43 +0200 (lun 05 de abr de 2021) $
#$Revision: 263786 $
#$URL: svn://www.crystallography.net/cod/cif/7/70/67/7706762.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_7706762
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         'C4 H12 Cl6 Mo2 O2 S2'
_chemical_formula_sum            'C4 H12 Cl6 Mo2 O2 S2'
_chemical_formula_weight         560.84
_chemical_name_systematic        '[MoOCl2(SMe)2)(Cl)2]'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive,Hygroscopic
_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_creation_date             2020-05-04
_audit_creation_method
;
Olex2 1.3
(compiled Sep 10 2019 10:52:38 for OlexSys, GUI svn.r5938)
;
_audit_update_record
;
2020-12-16 deposited with the CCDC.	2021-02-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.1720(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.81110(10)
_cell_length_b                   9.50630(10)
_cell_length_c                   11.2487(2)
_cell_measurement_reflns_used    18670
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.7760
_cell_measurement_theta_min      2.8270
_cell_volume                     806.15(2)
_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 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.9955
_diffrn_measured_fraction_theta_max 0.8997
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -98.00  22.00   0.50    0.50    --   -8.30 -60.00-150.00  240
  2  ω    -98.00  22.00   0.50    0.50    --   -8.30 -60.00 -30.00  240
  3  ω    -98.00  21.00   0.50    0.50    --   -8.30 -57.00  60.00  238
  4  ω    -98.00  81.00   0.50    0.50    --   -8.30   0.00-180.00  358
  5  ω    -39.00  32.00   0.50    0.50    --   -8.30  60.00  30.00  142
  6  ω    -39.00  81.00   0.50    0.50    --   -8.30  60.00 -90.00  240
;
_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      -0.0250907000
_diffrn_orient_matrix_UB_12      -0.0192916000
_diffrn_orient_matrix_UB_13      -0.0631257000
_diffrn_orient_matrix_UB_21      0.0900971000
_diffrn_orient_matrix_UB_22      0.0030738000
_diffrn_orient_matrix_UB_23      -0.0016747000
_diffrn_orient_matrix_UB_31      0.0105303000
_diffrn_orient_matrix_UB_32      -0.0719789000
_diffrn_orient_matrix_UB_33      0.0167839000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0175
_diffrn_reflns_av_unetI/netI     0.0086
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.898
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            21532
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.898
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.807
_diffrn_reflns_theta_min         3.754
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.791
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68702
_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    2.310
_exptl_crystal_description       block
_exptl_crystal_F_000             540
_exptl_crystal_preparation       'Slow evporation from Toluene'
_exptl_crystal_recrystallization_method 'Slow evporation from Toluene'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.302
_refine_diff_density_min         -0.483
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.208
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     75
_refine_ls_number_reflns         2693
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.208
_refine_ls_R_factor_all          0.0122
_refine_ls_R_factor_gt           0.0119
_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)+(0.0094P)²+0.3552P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0276
_refine_ls_wR_factor_ref         0.0277
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2654
_reflns_number_total             2693
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1dt00038a2.cif
_cod_data_source_block           moocl3(sme2)2-1
_cod_depositor_comments
'Adding full bibliography for 7706761--7706769.cif.'
_cod_database_code               7706762
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         MoOCl3S2C4H12
_chemical_oxdiff_usercomment     'Dark Green Block'
_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   0.488
_shelx_estimated_absorpt_t_min   0.401
_reflns_odcompleteness_completeness 99.55
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.64
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C)
;
_shelx_res_file
;
TITL moocl3(sme2)2-1_a.res in P2(1)/c
    moocl3(sme2)2-1.res
    created by SHELXL-2018/3 at 16:31:25 on 04-May-2020
REM Old TITL MoOCl3(SMe2)2-1 in P2(1)/c
REM SHELXT solution in P2(1)/c: R1 0.032, Rweak 0.009, Alpha 0.022
REM <I/s> 3.892 for 108 systematic absences, Orientation as input
REM Formula found by SHELXT: C2 O S Cl3 Mo
CELL 0.71073 7.8111 9.5063 11.2487 90 105.172 90
ZERR 2 0.0001 0.0001 0.0002 0 0.001 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H Cl Mo O S
UNIT 8 24 12 4 4 4

L.S. 4
PLAN  5
SIZE 0.4 0.3 0.3
BOND
list 4
fmap 2
acta
MORE -1
BOND $H
CONF
OMIT 2 0 2
REM <olex2.extras>
REM <HklSrc "%./MoOCl3(SMe2)2-1.hkl">
REM </olex2.extras>

WGHT    0.009400    0.355200
FVAR       0.62036
MO1   4    0.346060    0.336112    0.420554    11.00000    0.00845    0.00929 =
         0.00973   -0.00034    0.00260   -0.00124
CL3   3    0.604928    0.456476    0.397627    11.00000    0.00970    0.01275 =
         0.01183   -0.00174    0.00504   -0.00163
CL2   3    0.528355    0.195999    0.572471    11.00000    0.01483    0.01318 =
         0.01606    0.00366    0.00239    0.00103
S1    6    0.162121    0.536113    0.298958    11.00000    0.01041    0.01189 =
         0.01227   -0.00065    0.00311    0.00078
CL1   3    0.100426    0.295562    0.496318    11.00000    0.01162    0.01954 =
         0.01530    0.00028    0.00536   -0.00502
O1    5    0.308736    0.232535    0.298583    11.00000    0.01708    0.01545 =
         0.01428   -0.00261    0.00378   -0.00155
C1    1   -0.041205    0.450071    0.216898    11.00000    0.01032    0.01875 =
         0.01825   -0.00076    0.00104   -0.00058
AFIX 137
H1A   2   -0.106090    0.510654    0.152464    11.00000   -1.50000
H1B   2   -0.111970    0.430155    0.272964    11.00000   -1.50000
H1C   2   -0.013397    0.363770    0.181742    11.00000   -1.50000
AFIX   0
C2    1    0.260289    0.568507    0.172814    11.00000    0.01470    0.02037 =
         0.01502    0.00534    0.00554    0.00245
AFIX 137
H2A   2    0.273063    0.481098    0.133261    11.00000   -1.50000
H2B   2    0.374747    0.611105    0.203770    11.00000   -1.50000
H2C   2    0.185206    0.630526    0.114399    11.00000   -1.50000
AFIX   0
HKLF 4




REM  moocl3(sme2)2-1_a.res in P2(1)/c
REM wR2 = 0.0277, GooF = S = 1.208, Restrained GooF = 1.208 for all data
REM R1 = 0.0119 for 2654 Fo > 4sig(Fo) and 0.0122 for all 2693 data
REM 75 parameters refined using 0 restraints

END

WGHT      0.0094      0.3552

REM Highest difference peak  0.302,  deepest hole -0.483,  1-sigma level  0.064
Q1    1   0.2602  0.4474  0.3482  11.00000  0.05    0.30
Q2    1   0.2807  0.2487  0.3463  11.00000  0.05    0.29
Q3    1   0.3240  0.3103  0.3112  11.00000  0.05    0.26
Q4    1   0.2013  0.5462  0.2248  11.00000  0.05    0.24
Q5    1   0.5467  0.2760  0.5954  11.00000  0.05    0.23
;
_shelx_res_checksum              4806
_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 1.727
_oxdiff_exptl_absorpt_empirical_full_min 0.609
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
Mo1 Mo 0.34606(2) 0.33611(2) 0.42055(2) 0.00912(3) Uani 1 1 d . . . . .
Cl3 Cl 0.60493(3) 0.45648(2) 0.39763(2) 0.01101(4) Uani 1 1 d . . . . .
Cl2 Cl 0.52835(3) 0.19600(3) 0.57247(2) 0.01500(5) Uani 1 1 d . . . . .
S1 S 0.16212(3) 0.53611(3) 0.29896(2) 0.01150(5) Uani 1 1 d . . . . .
Cl1 Cl 0.10043(3) 0.29556(3) 0.49632(2) 0.01515(5) Uani 1 1 d . . . . .
O1 O 0.30874(10) 0.23253(8) 0.29858(7) 0.01566(14) Uani 1 1 d . . . . .
C1 C -0.04121(13) 0.45007(12) 0.21690(10) 0.01628(19) Uani 1 1 d . . . . .
H1A H -0.106090 0.510654 0.152464 0.024 Uiso 1 1 calc R U . . .
H1B H -0.111970 0.430155 0.272964 0.024 Uiso 1 1 calc R U . . .
H1C H -0.013397 0.363770 0.181742 0.024 Uiso 1 1 calc R U . . .
C2 C 0.26029(14) 0.56851(12) 0.17281(10) 0.01639(19) Uani 1 1 d . . . . .
H2A H 0.273063 0.481098 0.133261 0.025 Uiso 1 1 calc R U . . .
H2B H 0.374747 0.611105 0.203770 0.025 Uiso 1 1 calc R U . . .
H2C H 0.185206 0.630526 0.114399 0.025 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
Mo1 0.00845(4) 0.00929(4) 0.00973(4) -0.00034(3) 0.00260(3) -0.00124(2)
Cl3 0.00970(9) 0.01275(10) 0.01183(9) -0.00174(7) 0.00504(7) -0.00163(7)
Cl2 0.01483(10) 0.01318(10) 0.01606(11) 0.00366(8) 0.00239(8) 0.00103(8)
S1 0.01041(9) 0.01189(10) 0.01227(10) -0.00065(8) 0.00311(8) 0.00078(8)
Cl1 0.01162(10) 0.01954(11) 0.01530(10) 0.00028(9) 0.00536(8) -0.00502(8)
O1 0.0171(3) 0.0154(3) 0.0143(3) -0.0026(3) 0.0038(3) -0.0015(3)
C1 0.0103(4) 0.0188(5) 0.0182(5) -0.0008(4) 0.0010(3) -0.0006(3)
C2 0.0147(4) 0.0204(5) 0.0150(4) 0.0053(4) 0.0055(3) 0.0025(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'
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
Cl3 Mo1 Cl3 77.520(8) . 3_666 ?
Cl3 Mo1 S1 87.659(8) . . ?
Cl2 Mo1 Cl3 88.911(9) . . ?
Cl2 Mo1 Cl3 85.774(8) . 3_666 ?
Cl2 Mo1 S1 165.215(9) . . ?
S1 Mo1 Cl3 79.443(8) . 3_666 ?
Cl1 Mo1 Cl3 156.780(9) . . ?
Cl1 Mo1 Cl3 79.451(8) . 3_666 ?
Cl1 Mo1 Cl2 92.340(9) . . ?
Cl1 Mo1 S1 85.253(9) . . ?
O1 Mo1 Cl3 171.64(3) . 3_666 ?
O1 Mo1 Cl3 99.54(3) . . ?
O1 Mo1 Cl2 102.08(3) . . ?
O1 Mo1 S1 92.67(3) . . ?
O1 Mo1 Cl1 102.85(3) . . ?
Mo1 Cl3 Mo1 102.479(8) . 3_666 ?
C1 S1 Mo1 103.43(4) . . ?
C2 S1 Mo1 104.63(4) . . ?
C2 S1 C1 99.94(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 . . ?
S1 C2 H2A 109.5 . . ?
S1 C2 H2B 109.5 . . ?
S1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 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 Cl3 2.7942(2) 3_666 ?
Mo1 Cl3 2.3953(2) . ?
Mo1 Cl2 2.3341(3) . ?
Mo1 S1 2.5537(3) . ?
Mo1 Cl1 2.3264(2) . ?
Mo1 O1 1.6515(8) . ?
S1 C1 1.8100(10) . ?
S1 C2 1.8071(11) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
