Synthesis, properties and structural features of molybdenum(v) oxide trichloride complexes with neutral chalcogenoether ligands.
Smith, Danielle E.; Levason, William; Powell, James; Reid, Gillian; Dalton transactions (Cambridge, England : 2003) 50 (2021) 4380–4389; doi:10.1039/d1dt00038a

data_7706761
_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  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -43.00 -16.00   0.50    0.50    --    5.00 -38.00 -30.00   54
  2  \w    -94.00   1.00   0.50    0.50    --   -8.40 -60.00 150.00  190
  3  \w    -35.00  19.00   0.50    0.50    --   -8.40 -60.00   0.00  108
  4  \w    -69.00  21.00   0.50    0.50    --   -8.40 -57.00-120.00  180
  5  \w    -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       '\w 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/[\s^2^(Fo^2^)+(0.0120P)^2^+0.6276P] where P=(Fo^2^+2Fc^2^)/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 > 2\s(I)'
_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_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