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_7706768
_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         'C6 H16 Cl3 Mo O P2'
_chemical_formula_sum            'C6 H16 Cl3 Mo O P2'
_chemical_formula_weight         368.42
_chemical_name_systematic        MoOCl3(dmpe)
_chemical_properties_physical    Air-sensitive,Moisture-sensitive,Hygroscopic
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-05-10
_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                 93.989(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   7.37160(10)
_cell_length_b                   29.8674(6)
_cell_length_c                   12.4489(2)
_cell_measurement_reflns_used    30241
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.8010
_cell_measurement_theta_min      2.1310
_cell_volume                     2734.24(8)
_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_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.787
_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    -98.00  21.32   0.38    1.07    --   -8.30 -60.00  30.00  314
  2  \w    -98.00  20.18   0.38    1.07    --   -8.30 -57.00 150.00  311
  3  \w    -98.00  21.32   0.38    1.07    --   -8.30 -60.00 -90.00  314
  4  \w    -98.00  80.22   0.38    1.07    --   -8.30   0.00   0.00  469
  5  \w    -39.00  43.08   0.38    1.07    --   -8.30  38.00  30.00  216
  6  \w    -38.00  80.18   0.38    1.07    --   -8.30  57.00 120.00  311
;
_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      -0.0041237000
_diffrn_orient_matrix_UB_12      -0.0039418000
_diffrn_orient_matrix_UB_13      0.0559725000
_diffrn_orient_matrix_UB_21      0.0846703000
_diffrn_orient_matrix_UB_22      -0.0113518000
_diffrn_orient_matrix_UB_23      0.0010796000
_diffrn_orient_matrix_UB_31      0.0460551000
_diffrn_orient_matrix_UB_32      0.0204752000
_diffrn_orient_matrix_UB_33      0.0113462000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0532
_diffrn_reflns_av_unetI/netI     0.0470
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.787
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            24936
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.787
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.852
_diffrn_reflns_theta_min         2.133
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.745
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50112
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.790
_exptl_crystal_description       plate
_exptl_crystal_F_000             1464
_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          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         3.853
_refine_diff_density_min         -1.381
_refine_diff_density_rms         0.169
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     243
_refine_ls_number_reflns         8018
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0417
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0616P)^2^+4.7250P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1072
_refine_ls_wR_factor_ref         0.1117
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7053
_reflns_number_total             8018
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00038a2.cif
_cod_data_source_block           moocl3dmpe
_cod_depositor_comments
'Adding full bibliography for 7706761--7706769.cif.'
_cod_database_code               7706768
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         MoOCl3P2C6H9
_chemical_oxdiff_usercomment     'Yellow Block'
_reflns_odcompleteness_completeness 96.49
_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:
 C00G(H00D,H00E), C00H(H00F,H00G), C00I(H00Q,H00R), C00J(H00S,H00T)
2.b Idealised Me refined as rotating group:
 C00F(H00A,H00B,H00C), C00K(H00U,H00V,H00W), C00L(H00H,H00I,H00J), C00M(H00K,
 H00L,H00M), C00N(H00X,H00Y,H), C00O(H00Z,HA,HB), C00P(H00,HC,HD), C00Q(H00N,
 H00O,H00P)
;
_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 3.134
_oxdiff_exptl_absorpt_empirical_full_min 0.571