Molybdenum(VI) Dioxo Complexes Employing Schiff Base Ligands with an Intramolecular Donor for Highly Selective Olefin Epoxidation
Martina E. Judmaier; Christof Holzer; Manuel Volpe; Nadia C. Mösch-Zanetti; Inorganic Chemistry 51 (2012) 9956–9966; doi:10.1021/ic301464w

data_4330397
_publ_section_title
;
 Molybdenum(VI) Dioxo Complexes Employing Schiff Base Ligands with an
 Intramolecular Donor for Highly Selective Olefin Epoxidation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9956
_journal_page_last               9966
_journal_paper_doi               10.1021/ic301464w
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C36 H56 Mo N2 O6'
_chemical_formula_sum            'C36 H56 Mo N2 O6'
_chemical_formula_weight         708.77
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 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                 107.044(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   31.098(3)
_cell_length_b                   10.1937(8)
_cell_length_c                   11.9756(9)
_cell_measurement_reflns_used    9658
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.00
_cell_measurement_theta_min      2.74
_cell_volume                     3629.6(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    ORTEP
_computing_publication_material  enCIFer
_computing_structure_refinement  'SIR-92 (Giacovazzo, 1992)'
_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         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0233
_diffrn_reflns_av_sigmaI/netI    0.0200
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            36836
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.11
_diffrn_standards_decay_%        none
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.406
_exptl_absorpt_correction_T_max  0.7643
_exptl_absorpt_correction_T_min  0.6477
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.297
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.033
_refine_diff_density_min         -0.576
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(1)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     421
_refine_ls_number_reflns         9485
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0225
_refine_ls_R_factor_gt           0.0221
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0373P)^2^+1.6497P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0576
_refine_ls_wR_factor_ref         0.0579
_reflns_number_gt                9350
_reflns_number_total             9485
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301464w_si_001.cif
_cod_data_source_block           motbun
_cod_original_cell_volume        3629.5(5)
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               4330397