Dimeric μ-oxo bridged molybdenum(vi) dioxo complexes as catalysts in the epoxidation of internal and terminal alkenes
Judmaier, Martina E.; Sala, Chris H.; Belaj, Ferdinand; Volpe, Manuel; Mösch-Zanetti, Nadia C.; New Journal of Chemistry 37 (2013) 2139–; doi:10.1039/c3nj00115f

data_7053130
_publ_section_title
;
 Dimeric \m-oxo bridged molybdenum(vi) dioxo complexes as catalysts in the
 epoxidation of internal and terminal alkenes
;
_journal_issue                   7
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              2139
_journal_paper_doi               10.1039/c3nj00115f
_journal_volume                  37
_journal_year                    2013
_chemical_compound_source        'synthetical product'
_chemical_formula_moiety         'C38 H66 Mo2 N4 O7, 2.0(C2 H3 N)'
_chemical_formula_sum            'C42 H72 Mo2 N6 O7'
_chemical_formula_weight         964.94
_chemical_name_systematic
;
(mu2-oxo)-bis(2,4-di-tert-butyl-6-[{[2-(dimethylamino)ethyl]imino}methyl]phe-
nolato)-tetraoxo-di-molybdenum(VI) acetonitrile solvate (1:2)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'manual edited SHELXL-97 .cif file'
_cell_angle_alpha                90.00
_cell_angle_beta                 94.1130(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.8832(5)
_cell_length_b                   11.6611(4)
_cell_length_c                   30.2445(9)
_cell_measurement_reflns_used    9863
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.83
_cell_measurement_theta_min      2.21
_cell_volume                     4883.8(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'modified ORTEP (Johnson, 1965)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0216
_diffrn_reflns_av_sigmaI/netI    0.0229
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            44653
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         1.87
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.563
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6083
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.312
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2024
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.200
_refine_diff_density_min         -0.691
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     585
_refine_ls_number_reflns         14241
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0322
_refine_ls_R_factor_gt           0.0268
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0268P)^2^+4.6077P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0657
_refine_ls_wR_factor_ref         0.0686
_reflns_number_gt                12714
_reflns_number_total             14241
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3nj00115f.txt
_cod_data_source_block           MJ393
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7053130