Synthesis and Full Characterization of Molybdenum and Antimony Corroles and Utilization of the Latter Complexes as Very Efficient Catalysts for Highly Selective Aerobic Oxygenation Reactions
Luobeznova, Inna; Raizman, Marina; Goldberg, Israel; Gross, Zeev; Inorganic Chemistry 45 (2006) 386–394; doi:10.1021/ic051483g

data_4331738
_publ_section_title
;
 Synthesis and Full Characterization of Molybdenum and Antimony Corroles
 and Utilization of the Latter Complexes as Very Efficient Catalysts for
 Highly Selective Aerobic Oxygenation Reactions
;
_journal_issue                   1
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              386
_journal_page_last               394
_journal_paper_doi               10.1021/ic051483g
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety         '(C37 H8 F15 N4 Mo O), 2(C6 H6)'
_chemical_formula_sum            'C49 H20 F15 Mo N4 O'
_chemical_formula_weight         1061.63
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                70.7720(11)
_cell_angle_beta                 84.5440(15)
_cell_angle_gamma                72.6970(14)
_cell_formula_units_Z            2
_cell_length_a                   8.4738(1)
_cell_length_b                   13.6757(3)
_cell_length_c                   19.5250(5)
_cell_measurement_reflns_used    7629
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      28.19
_cell_measurement_theta_min      2.75
_cell_volume                     2039.74(8)
_computing_cell_refinement       Denzo
_computing_data_collection       'Collect, Nonius B.V.'
_computing_data_reduction        Denzo
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-92
_diffrn_ambient_temperature      110(2)
_diffrn_detector_area_resol_mean '56 microns'
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '1 deg. Phi & Omega 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  0.0280
_diffrn_reflns_av_sigmaI/netI    0.0529
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            17386
_diffrn_reflns_theta_full        28.19
_diffrn_reflns_theta_max         28.19
_diffrn_reflns_theta_min         2.75
_exptl_absorpt_coefficient_mu    0.437
_exptl_absorpt_correction_T_max  0.9373
_exptl_absorpt_correction_T_min  0.8800
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.728
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prisms
_exptl_crystal_F_000             1054
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.835
_refine_diff_density_min         -0.864
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     631
_refine_ls_number_reflns         9397
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0413
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0507P)^2^+1.4101P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0956
_refine_ls_wR_factor_ref         0.1049
_reflns_number_gt                7629
_reflns_number_total             9397
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic051483gsup1.cif
_cod_data_source_block           Compound-1a
_cod_original_cell_volume        2039.74(7)
_cod_database_code               4331738