Synthesis and Catalytic Epoxidation Activity with TBHP and H2O2of Dioxo-, Oxoperoxo-, and Oxodiperoxo Molybdenum(VI) and Tungsten(VI) Compounds Containing Monodentate or Bidentate Phosphine Oxide Ligands: Crystal Structures of WCl2(O)2(OPMePh2)2, WCl2(O)(O2)(OPMePh2)2, MoCl2(O)2dppmO2·C4H10O, WCl2(O)2dppmO2, Mo(O)(O2)2dppmO2, and W(O)(O2)2dppmO2
Jimtaisong, Ampa; Luck, Rudy L.; Inorganic Chemistry 45 (2006) 10391–10402; doi:10.1021/ic061455d

data_4333123
_publ_section_title
;
 Synthesis and Catalytic Epoxidation Activity with TBHP and H2O2of Dioxo-,
 Oxoperoxo-, and Oxodiperoxo Molybdenum(VI) and Tungsten(VI) Compounds
 Containing Monodentate or Bidentate Phosphine Oxide Ligands:&#x00A0;
 Crystal Structures of WCl2(O)2(OPMePh2)2, WCl2(O)(O2)(OPMePh2)2,
 MoCl2(O)2dppmO2&#x00B7;C4H10O, WCl2(O)2dppmO2, Mo(O)(O2)2dppmO2, and
 W(O)(O2)2dppmO2
;
_journal_issue                   25
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10391
_journal_page_last               10402
_journal_paper_doi               10.1021/ic061455d
_journal_volume                  45
_journal_year                    2006
_chemical_absolute_configuration unk
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C100 H88 Cl8 O16 P8 W4'
_chemical_formula_sum            'C100 H88 Cl8 O16 P8 W4'
_chemical_formula_weight         2812.46
_space_group_IT_number           80
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      80
_symmetry_space_group_name_Hall  'I 4bw'
_symmetry_space_group_name_H-M   'I 41'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2006-06-06T18:02:43-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.268(2)
_cell_length_b                   19.268(4)
_cell_length_c                   28.587(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      10
_cell_measurement_wavelength     0.71073
_cell_volume                     10613(3)
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Giacovazzo et al, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'scintillation LiI'
_diffrn_detector_dtime           1.195
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf Nonius TurboCAD4'
_diffrn_measurement_method       'non-profiled omega scans'
_diffrn_orient_matrix_type
;
  x-axis points to radiation source
  the matrix is specified in reciprocal space
;
_diffrn_orient_matrix_UB_11      0.008122
_diffrn_orient_matrix_UB_12      0.014137
_diffrn_orient_matrix_UB_13      0.056561
_diffrn_orient_matrix_UB_21      0.012158
_diffrn_orient_matrix_UB_22      0.04535
_diffrn_orient_matrix_UB_23      -0.005555
_diffrn_orient_matrix_UB_31      -0.031779
_diffrn_orient_matrix_UB_32      0.020958
_diffrn_orient_matrix_UB_33      -0.026188
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0697
_diffrn_reflns_av_unetI/netI     0.0628
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7331
_diffrn_reflns_theta_full        22.47
_diffrn_reflns_theta_max         22.47
_diffrn_reflns_theta_min         1.27
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_decay_%        3
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.705
_exptl_absorpt_correction_T_max  0.7895
_exptl_absorpt_correction_T_min  0.5366
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351
        Number of psi-scan sets used was   5
        Theta correction was applied.
        Averaged transmission function was used.
        No Fourier smoothing was applied.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.76
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             5472
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.318
_refine_diff_density_min         -0.643
_refine_diff_density_rms         0.109
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.007(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     613
_refine_ls_number_reflns         4903
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0564
_refine_ls_R_factor_gt           0.0379
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0622P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0916
_refine_ls_wR_factor_ref         0.099
_reflns_number_gt                4217
_reflns_number_total             4903
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061455dsup1.cif
_cod_data_source_block           new
_cod_database_code               4333123