Effect of N-based additive on the optimization of liquid phase oxidation of bicyclic, cyclic and aromatic alcohols catalyzed by dioxidomolybdenum(VI) and oxidoperoxidomolybdenum(VI) complexes
Maurya, Mannar R.; Saini, Neeraj; Avecilla, Fernando; RSC Adv.  (2015) –; doi:10.1039/C5RA16490G

data_7223298
_publ_section_title
;
 Effect of N-based additive on the optimization of liquid phase oxidation
 of bicyclic, cyclic and aromatic alcohols catalyzed by
 dioxidomolybdenum(VI) and oxidoperoxidomolybdenum(VI) complexes
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C5RA16490G
_journal_year                    2015
_chemical_formula_moiety         'C21 H17 Mo N3 O5, C H4 O'
_chemical_formula_sum            'C22 H21 Mo N3 O6'
_chemical_formula_weight         519.36
_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
_audit_update_record
;
2015-07-22 deposited with the CCDC.
2015-11-16 downloaded from the CCDC.
;
_cell_angle_alpha                90.030(2)
_cell_angle_beta                 100.548(2)
_cell_angle_gamma                99.031(2)
_cell_formula_units_Z            2
_cell_length_a                   7.7600(3)
_cell_length_b                   9.9273(4)
_cell_length_c                   14.1328(6)
_cell_measurement_reflns_used    48101
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      51.544
_cell_measurement_theta_min      5.015
_cell_volume                     1056.59(7)
_computing_cell_refinement
' SAINT V7.68A (Bruker: Madison, 2009 ) in Apex2 suite.'
_computing_data_collection       'Apex2, Bruker Instrument Service v2010, 1-2'
_computing_data_reduction
'SAINT and XPREP Version 2008/2 (Sheldrick, Bruker AXS Inc.)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement
'XL Version 2008/4 (George M. Sheldrick, Acta Cryst. (2008). A64, 112-122)'
_computing_structure_solution
'XS Version 2008/1 (George M. Sheldrick, Acta Cryst. (2008). A64, 112-122) '
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and 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  0.0678
_diffrn_reflns_av_unetI/netI     0.0535
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            56836
_diffrn_reflns_theta_full        34.79
_diffrn_reflns_theta_max         34.79
_diffrn_reflns_theta_min         1.47
_exptl_absorpt_coefficient_mu    0.666
_exptl_absorpt_correction_T_max  0.9243
_exptl_absorpt_correction_T_min  0.8052
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.632
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             528
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.702
_refine_diff_density_min         -0.828
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     351
_refine_ls_number_reflns         8936
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0362
_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^)+(0.0336P)^2^+0.3225P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0773
_refine_ls_wR_factor_ref         0.0829
_reflns_number_gt                7391
_reflns_number_total             8936
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ra16490g2.cif
_cod_data_source_block           manar183
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 
;
_cod_original_sg_symbol_Hall     -P1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7223298