Synthesis and Structural Characterization of Molybdenum(VI) and Iron(II) Coordination Compounds with S-Alkyl-N-methyl-S-(2-pyridyl)sulfoximines and Catalytic Epoxidation Activity of the Molybdenum Complexes
Yvonne Brussaard; Falk Olbrich; Ernst Schaumann; Inorganic Chemistry 52 (2013) 13160–13166; doi:10.1021/ic4020306

data_4336738
_publ_contact_author
;
      Schaumann, Ernst
      Institute of Organic Chemistry
      Clausthal University of Technology
      Leibnizstrasse 6
      D-38678 Clausthal-Zellerfeld
      Germany
;
_publ_contact_author_email       ernst.schaumann@tu.clausthal.de
_publ_contact_author_fax         '+49 5323 72 2858'
_publ_contact_author_phone       '+49 5323 72 2519'
_publ_section_title
;
 Synthesis and Structural Characterization of Molybdenum(VI) and Iron(II)
 Coordination Compounds with S-Alkyl-N-methyl-S-(2-pyridyl)sulfoximines
 and Catalytic Epoxidation Activity of the Molybdenum Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              13160
_journal_page_last               13166
_journal_paper_doi               10.1021/ic4020306
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C10 H16 Mo N2 O6 S'
_chemical_formula_sum            'C10 H16 Mo N2 O6 S'
_chemical_formula_weight         388.25
_chemical_name_common            '[MoO(O2)2{SO(NMe)Bu(NC5H4)}]'
_chemical_name_systematic
; 
 (S-Butyl-N-methyl-S-2-pyridyl sulfoximine)(oxo)(diperoxo)molybdenum(VI)
;
_chemical_temperature_decomposition 668
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.701(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.5057(1)
_cell_length_b                   18.5753(2)
_cell_length_c                   9.4720(1)
_cell_measurement_reflns_used    100
_cell_measurement_temperature    173
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.00
_cell_volume                     1470.51(3)
_computing_cell_refinement       'SAINT (Bruker AXS, 1998)'
_computing_data_collection       'SMART (Bruker AXS, 1998)'
_computing_data_reduction        'SAINT (Bruker AXS, 1998)'
_computing_molecular_graphics    'SHELXTL (Bruker AXS, 1998)'
_computing_publication_material  'SHELXTL (Bruker AXS, 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker AXS, 1998'
_diffrn_measurement_method       omega-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0245
_diffrn_reflns_av_sigmaI/netI    0.0288
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            9183
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.19
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    1.058
_exptl_absorpt_correction_T_max  0.6768
_exptl_absorpt_correction_T_min  0.6197
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 1998)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.754
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             784
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.608
_refine_diff_density_min         -0.637
_refine_diff_density_rms         0.068
_refine_ls_extinction_coef       0.0054(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         3357
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0259
_refine_ls_R_factor_gt           0.0222
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0382P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0577
_refine_ls_wR_factor_ref         0.0593
_reflns_number_gt                3031
_reflns_number_total             3357
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4020306_si_002_2.cif
_cod_data_source_block           13_98md
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4336738