Oxidation of secondary alcohols by conventional and microwave-assisted methods using molybdenum complexes of ONO donor ligands
Maurya, Mannar R.; Dhaka, Sarita; Avecilla, Fernando; New J. Chem. 39 (2015) 2130–; doi:10.1039/C4NJ02208D

data_7054618
_publ_section_title
;
 Oxidation of secondary alcohols by conventional and microwave-assisted
 methods using molybdenum complexes of ONO donor ligands
;
_journal_issue                   3
_journal_name_full               'New J. Chem.'
_journal_page_first              2130
_journal_paper_doi               10.1039/C4NJ02208D
_journal_volume                  39
_journal_year                    2015
_chemical_formula_sum            'C25 H26 Mo N4 O7 S'
_chemical_formula_weight         622.50
_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
;
2014-12-02 deposited with the CCDC.
2015-01-07 downloaded from the CCDC.
;
_cell_angle_alpha                106.769(5)
_cell_angle_beta                 98.537(5)
_cell_angle_gamma                91.636(5)
_cell_formula_units_Z            2
_cell_length_a                   8.782(5)
_cell_length_b                   11.521(5)
_cell_length_c                   14.083(5)
_cell_measurement_temperature    293(2)
_cell_volume                     1345.3(11)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.945
_diffrn_measured_fraction_theta_max 0.682
_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  0.0386
_diffrn_reflns_av_sigmaI/netI    0.0530
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            17509
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         32.79
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    0.616
_exptl_absorpt_correction_T_max  0.9410
_exptl_absorpt_correction_T_min  0.8368
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'North et al., 1968'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.537
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             636
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.504
_refine_diff_density_min         -0.825
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         6817
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0719
_refine_ls_R_factor_gt           0.0460
_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^)+(0.0688P)^2^+0.2820P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1162
_refine_ls_wR_factor_ref         0.1421
_reflns_number_gt                4894
_reflns_number_total             6817
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4nj02208d2.cif
_cod_data_source_block           sar10b
_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 2935 2014-11-11 08:27:57Z andrius 

 Adding full bibliography for 7054618--7054619.cif.
;
_cod_original_sg_symbol_Hall     -P1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7054618