Catalytic oxidation of benzyl-alcohol with H2O2 in the presence of a dioxidomolybdenum(VI) complex
Balapoor, Leila; Bikas, Rahman; Dargahi, Maryam; Inorganica Chimica Acta 510 (2020) 119734–; doi:10.1016/j.ica.2020.119734

data_1564214
_publ_section_title
;
 Catalytic oxidation of benzyl-alcohol with H2O2 in the presence of a
 dioxidomolybdenum(VI) complex
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119734
_journal_paper_doi               10.1016/j.ica.2020.119734
_journal_volume                  510
_journal_year                    2020
_chemical_formula_sum            'C16 H16 Mo N2 O6'
_chemical_formula_weight         428.25
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   23.8478(16)
_cell_length_b                   9.7286(8)
_cell_length_c                   15.1467(11)
_cell_measurement_reflns_used    5372
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      65.977
_cell_measurement_theta_min      4.720
_cell_volume                     3514.1(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker X8 Proteum'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'graded multilayer optics'
_diffrn_radiation_source         'fine-focus rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0596
_diffrn_reflns_av_sigmaI/netI    0.0469
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6300
_diffrn_reflns_theta_full        66.47
_diffrn_reflns_theta_max         66.47
_diffrn_reflns_theta_min         4.72
_exptl_absorpt_coefficient_mu    6.424
_exptl_absorpt_correction_T_max  0.6275
_exptl_absorpt_correction_T_min  0.5128
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS, 2010'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.619
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1728
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.311
_refine_diff_density_min         -1.717
_refine_diff_density_rms         0.175
_refine_ls_abs_structure_details
'Flack H D (1983), Acta Cryst. A39, 876-881, 3598 Friedel pairs''
_refine_ls_abs_structure_Flack   0.48(3)
_refine_ls_extinction_coef       0.00087(17)
_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   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     457
_refine_ls_number_reflns         6054
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0950
_refine_ls_R_factor_gt           0.0821
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2329
_refine_ls_wR_factor_ref         0.2519
_reflns_number_gt                4909
_reflns_number_total             6054
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2020-510-119734.cif
_cod_data_source_block           d4a
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'MULTI-SCAN' was
changed to 'multi-scan' in accordance with the built-in table derived
from the CIF Core dictionary named 'cif_core.dic' version 2.4.5 last
updated on 2014-11-21.

data item '_symmetry_cell_setting' value 'Orthorhombic' was changed
to 'orthorhombic' in accordance with the built-in table derived from
the CIF Core dictionary named 'cif_core.dic' version 2.4.5 last
updated on 2014-11-21.

Automatic conversion script
Id: cif_fix_values 8369 2020-08-20 11:38:08Z andrius 
;
_cod_original_sg_symbol_H-M      Pna2(1)
_cod_database_code               1564214