#------------------------------------------------------------------------------
#$Date: 2021-04-05 16:57:43 +0200 (lun 05 de abr de 2021) $
#$Revision: 263786 $
#$URL: svn://www.crystallography.net/cod/cif/7/70/67/7706761.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_7706761
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 Se2'
_chemical_formula_sum            'C4 H12 Cl6 Mo2 O2 Se2'
_chemical_formula_weight         654.64
_chemical_name_systematic        '[MoOCl2(SeMe2)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                 105.647(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.8374(2)
_cell_length_b                   9.6744(2)
_cell_length_c                   11.2666(3)
_cell_measurement_reflns_used    7885
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.1600
_cell_measurement_theta_min      2.6810
_cell_volume                     822.60(4)
_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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.9991
_diffrn_measured_fraction_theta_max 0.8691
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -43.00 -16.00   0.50    0.50    --    5.00 -38.00 -30.00   54
  2  ω    -94.00   1.00   0.50    0.50    --   -8.40 -60.00 150.00  190
  3  ω    -35.00  19.00   0.50    0.50    --   -8.40 -60.00   0.00  108
  4  ω    -69.00  21.00   0.50    0.50    --   -8.40 -57.00-120.00  180
  5  ω    -97.00  40.00   0.50    0.50    --   -8.40 -19.00 -30.00  274
;
_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      -0.0865456000
_diffrn_orient_matrix_UB_12      -0.0206024000
_diffrn_orient_matrix_UB_13      0.0008933000
_diffrn_orient_matrix_UB_21      -0.0367748000
_diffrn_orient_matrix_UB_22      0.0474389000
_diffrn_orient_matrix_UB_23      -0.0481164000
_diffrn_orient_matrix_UB_31      0.0007532000
_diffrn_orient_matrix_UB_32      -0.0519446000
_diffrn_orient_matrix_UB_33      -0.0442256000
_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  0.0261
_diffrn_reflns_av_unetI/netI     0.0215
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.869
_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       -14
_diffrn_reflns_number            11835
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.869
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.664
_diffrn_reflns_theta_min         2.699
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.907
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60017
_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    2.643
_exptl_crystal_description       block
_exptl_crystal_F_000             612
_exptl_crystal_preparation       'Slow evporation from Toluene'
_exptl_crystal_recrystallization_method 'Slow evporation from Toluene`'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.637
_refine_diff_density_min         -0.651
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     75
_refine_ls_number_reflns         2616
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0194
_refine_ls_R_factor_gt           0.0167
_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)+(0.0120P)²+0.6276P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0348
_refine_ls_wR_factor_ref         0.0354
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2452
_reflns_number_total             2616
_reflns_threshold_expression     'I > 2σ(I)'
_iucr_refine_instructions_details
;
TITL moocl3(seme)2-1_a.res in P2(1)/c
    moocl3(seme)2-1.res
    created by SHELXL-2018/3 at 12:12:58 on 10-Feb-2020
REM Old TITL MoOCl3(SeMe)2-1 in P2(1)/c
REM SHELXT solution in P2(1)/c: R1 0.030, Rweak 0.009, Alpha 0.013
REM <I/s> 0.782 for 109 systematic absences, Orientation as input
REM Formula found by SHELXT: C2 O Cl3 Se Mo
CELL 0.71073 7.8374 9.6744 11.2666 90 105.647 90
ZERR 2 0.0002 0.0002 0.0003 0 0.003 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H Cl Mo O Se
UNIT 8 24 12 4 4 4

L.S. 4
PLAN  20
SIZE 0.3 0.3 0.3
BOND
list 4
fmap 2
ACTA
REM <olex2.extras>
REM <HklSrc "%.\\MoOCl3(SeMe)2-1.hkl">
REM </olex2.extras>

WGHT    0.012000    0.627600
FVAR       0.38220
MO1   4    0.659127    0.657736    0.580976    11.00000    0.00934    0.00855 =
         0.01001   -0.00020    0.00266   -0.00123
SE1   6    0.843904    0.446712    0.703870    11.00000    0.01042    0.00992 =
         0.01168   -0.00070    0.00284    0.00058
CL1   3    0.396933    0.543877    0.602929    11.00000    0.01027    0.01207 =
         0.01175   -0.00144    0.00464   -0.00137
CL2   3    0.480862    0.798319    0.428162    11.00000    0.01549    0.01219 =
         0.01591    0.00392    0.00276    0.00090
CL3   3    0.907060    0.695345    0.508586    11.00000    0.01220    0.01811 =
         0.01648    0.00038    0.00578   -0.00423
O1    5    0.700267    0.756851    0.705000    11.00000    0.01767    0.01397 =
         0.01434   -0.00291    0.00429   -0.00230
C2    1    1.055559    0.543795    0.797840    11.00000    0.01181    0.01818 =
         0.01664   -0.00207    0.00052   -0.00087
AFIX 137
H2A   2    1.021583    0.627519    0.831138    11.00000   -1.50000
H2B   2    1.129045    0.565762    0.744683    11.00000   -1.50000
H2C   2    1.120183    0.485869    0.863931    11.00000   -1.50000
AFIX   0
C1    1    0.732570    0.424411    0.838126    11.00000    0.01640    0.02088 =
         0.01533    0.00525    0.00643    0.00332
AFIX 137
H1A   2    0.804256    0.364995    0.900069    11.00000   -1.50000
H1B   2    0.617189    0.384192    0.806771    11.00000   -1.50000
H1C   2    0.721494    0.513073    0.873586    11.00000   -1.50000
AFIX   0
HKLF 4




REM  moocl3(seme)2-1_a.res in P2(1)/c
REM wR2 = 0.0354, GooF = S = 1.035, Restrained GooF = 1.035 for all data
REM R1 = 0.0167 for 2452 Fo > 4sig(Fo) and 0.0194 for all 2616 data
REM 75 parameters refined using 0 restraints

END  
     
WGHT      0.0120      0.6276 

REM Highest difference peak  0.637,  deepest hole -0.651,  1-sigma level  0.099
Q1    1   0.6506  0.6044  0.5378  11.00000  0.05    0.64
Q2    1   0.6768  0.7184  0.6367  11.00000  0.05    0.57
Q3    1   0.8466  0.3845  0.6645  11.00000  0.05    0.53
Q4    1   0.6538  0.7176  0.5373  11.00000  0.05    0.47
Q5    1   0.9714  0.4559  0.7336  11.00000  0.05    0.45
Q6    1   0.9120  0.3868  0.6840  11.00000  0.05    0.42
Q7    1   0.8150  0.4889  0.6511  11.00000  0.05    0.42
Q8    1   0.7507  0.4401  0.7861  11.00000  0.05    0.42
Q9    1   1.0643  0.4992  0.8700  11.00000  0.05    0.39
Q10   1   0.7584  0.6622  0.5012  11.00000  0.05    0.38
Q11   1   0.5168  0.5608  0.5857  11.00000  0.05    0.38
Q12   1   0.7663  0.4560  0.7113  11.00000  0.05    0.37
Q13   1   0.9563  0.4949  0.8042  11.00000  0.05    0.36
Q14   1   0.7439  0.6508  0.5790  11.00000  0.05    0.34
Q15   1   0.8300  0.7002  0.5269  11.00000  0.05    0.33
Q16   1   1.0559  0.6042  0.5522  11.00000  0.05    0.32
Q17   1   0.3527  0.5943  0.5397  11.00000  0.05    0.32
Q18   1   0.9388  0.7246  0.5836  11.00000  0.05    0.32
Q19   1   0.8483  0.7343  0.4147  11.00000  0.05    0.31
Q20   1   0.8639  0.5041  0.7524  11.00000  0.05    0.31

  REM The information below was added by Olex2.
  REM
  REM R1 = 0.0167 for 2452 Fo > 4sig(Fo) and 0.0194 for all 12252 data
  REM n/a parameters refined using n/a restraints
  REM Highest difference peak 0.64, deepest hole -0.65
  REM Mean Shift 0, Max Shift 0.001.

  REM +++ Tabular Listing of Refinement Information +++
  REM R1_all = 0.0194
  REM R1_gt = 0.0167
  REM wR_ref = 0.0354
  REM GOOF = 1.035
  REM Shift_max = 0.001
  REM Shift_mean = 0
  REM Reflections_all = 12252
  REM Reflections_gt = 2452
  REM Parameters = n/a
  REM Hole = -0.65
  REM Peak = 0.64
  REM Flack = n/a
;
_cod_data_source_file            d1dt00038a2.cif
_cod_data_source_block           moocl3(seme)2-1
_cod_depositor_comments
'Adding full bibliography for 7706761--7706769.cif.'
_cod_database_code               7706761
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         MoOCl3SeCH
_chemical_oxdiff_usercomment     'Yellow Plate'
_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   0.231
_shelx_estimated_absorpt_t_min   0.231
_reflns_odcompleteness_completeness 99.91
_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:
 C2(H2a,H2b,H2c), 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 1.326
_oxdiff_exptl_absorpt_empirical_full_min 0.727
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 0.65913(2) 0.65774(2) 0.58098(2) 0.00929(4) Uani 1 1 d . . . . .
Se1 Se 0.84390(2) 0.44671(2) 0.70387(2) 0.01070(4) Uani 1 1 d . . . . .
Cl1 Cl 0.39693(5) 0.54388(4) 0.60293(3) 0.01104(7) Uani 1 1 d . . . . .
Cl2 Cl 0.48086(5) 0.79832(4) 0.42816(4) 0.01482(8) Uani 1 1 d . . . . .
Cl3 Cl 0.90706(5) 0.69535(4) 0.50859(4) 0.01523(8) Uani 1 1 d . . . . .
O1 O 0.70027(15) 0.75685(13) 0.70500(11) 0.0153(2) Uani 1 1 d . . . . .
C2 C 1.0556(2) 0.54380(18) 0.79784(16) 0.0162(3) Uani 1 1 d . . . . .
H2A H 1.021583 0.627519 0.831138 0.024 Uiso 1 1 calc GR . . . .
H2B H 1.129045 0.565762 0.744683 0.024 Uiso 1 1 calc GR . . . .
H2C H 1.120183 0.485869 0.863931 0.024 Uiso 1 1 calc GR . . . .
C1 C 0.7326(2) 0.42441(19) 0.83813(16) 0.0171(3) Uani 1 1 d . . . . .
H1A H 0.804256 0.364995 0.900069 0.026 Uiso 1 1 calc GR . . . .
H1B H 0.617189 0.384192 0.806771 0.026 Uiso 1 1 calc GR . . . .
H1C H 0.721494 0.513073 0.873586 0.026 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 0.00934(6) 0.00855(7) 0.01001(6) -0.00020(4) 0.00266(5) -0.00123(4)
Se1 0.01042(7) 0.00992(8) 0.01168(8) -0.00070(5) 0.00284(6) 0.00058(5)
Cl1 0.01027(15) 0.01207(17) 0.01175(16) -0.00144(12) 0.00464(13) -0.00137(12)
Cl2 0.01549(17) 0.01219(17) 0.01591(18) 0.00392(14) 0.00276(14) 0.00090(13)
Cl3 0.01220(16) 0.01811(19) 0.01648(18) 0.00038(14) 0.00578(14) -0.00423(14)
O1 0.0177(5) 0.0140(6) 0.0143(5) -0.0029(4) 0.0043(5) -0.0023(4)
C2 0.0118(7) 0.0182(8) 0.0166(8) -0.0021(6) 0.0005(6) -0.0009(6)
C1 0.0164(7) 0.0209(8) 0.0153(8) 0.0053(6) 0.0064(6) 0.0033(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'
Se Se -0.0929 2.2259 '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
Se1 Mo1 Cl1 78.763(9) . 3_666 ?
Cl1 Mo1 Se1 87.438(10) . . ?
Cl1 Mo1 Cl1 77.783(13) . 3_666 ?
Cl2 Mo1 Se1 163.988(12) . . ?
Cl2 Mo1 Cl1 85.225(13) . 3_666 ?
Cl2 Mo1 Cl1 89.123(14) . . ?
Cl3 Mo1 Se1 85.058(12) . . ?
Cl3 Mo1 Cl1 157.663(15) . . ?
Cl3 Mo1 Cl1 80.126(13) . 3_666 ?
Cl3 Mo1 Cl2 92.323(15) . . ?
O1 Mo1 Se1 92.89(4) . . ?
O1 Mo1 Cl1 171.11(4) . 3_666 ?
O1 Mo1 Cl1 98.98(4) . . ?
O1 Mo1 Cl2 103.09(4) . . ?
O1 Mo1 Cl3 102.38(4) . . ?
C2 Se1 Mo1 100.17(5) . . ?
C2 Se1 C1 97.19(8) . . ?
C1 Se1 Mo1 101.16(5) . . ?
Mo1 Cl1 Mo1 102.218(13) . 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
Mo1 Se1 2.6647(2) . ?
Mo1 Cl1 2.7927(4) 3_666 ?
Mo1 Cl1 2.4024(4) . ?
Mo1 Cl2 2.3385(4) . ?
Mo1 Cl3 2.3299(4) . ?
Mo1 O1 1.6532(12) . ?
Se1 C2 1.9513(16) . ?
Se1 C1 1.9514(17) . ?
