Arylhydrazones of Barbituric Acid: synthesis, coordination ability and catalytic activity of their CoII/III and CuII complexes toward peroxidative oxidation of alkanes
Palmucci, Jessica; Mahmudov, Kamran T.; Guedes da Silva, M. Fátima C.; Martins, Luísa Margarida; Marchetti, Fabio; Pettinari, Claudio; Pombeiro, Armando J. L.; RSC Adv.  (2015) –; doi:10.1039/C5RA14078A

data_7222361
_publ_section_title
;
 Arylhydrazones of Barbituric Acid: synthesis, coordination ability and
 catalytic activity of their CoII/III and CuII complexes toward
 peroxidative oxidation of alkanes
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C5RA14078A
_journal_year                    2015
_chemical_formula_moiety         'C19 H18 Co N10 O6 S'
_chemical_formula_sum            'C19 H18 Co N10 O6 S'
_chemical_formula_weight         573.42
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-03-20 deposited with the CCDC.
2015-09-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.753(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.9274(10)
_cell_length_b                   8.6362(5)
_cell_length_c                   16.9906(10)
_cell_measurement_reflns_used    5120
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.28
_cell_measurement_theta_min      2.49
_cell_volume                     2673.0(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SIR97 (Giacovazzo et al, 1997)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Bruker APEX-II PHOTON 100'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1126
_diffrn_reflns_av_unetI/netI     0.0917
_diffrn_reflns_laue_measured_fraction_full 0.981
_diffrn_reflns_laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            29502
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.342
_diffrn_reflns_theta_min         2.236
_exptl_absorpt_coefficient_mu    0.773
_exptl_absorpt_correction_T_max  0.955
_exptl_absorpt_correction_T_min  0.928
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.425
_exptl_crystal_description       NEEDLE
_exptl_crystal_F_000             1172
_exptl_crystal_size_max          0.380
_exptl_crystal_size_mid          0.078
_exptl_crystal_size_min          0.062
_platon_squeeze_details
;
 There were disordered molecules present in the structure of 5.
 Since no obvious major site occupations were found for those molecules,
 it was not possible to model them. PLATON/SQUEEZE was used to correct
 the data but the assignement is dubious. Thus, they were simply
 removed from the model. 
;
_refine_diff_density_max         1.159
_refine_diff_density_min         -1.036
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         4798
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.1410
_refine_ls_R_factor_gt           0.0852
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1317P)^2^+2.7927P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2114
_refine_ls_wR_factor_ref         0.2386
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2949
_reflns_number_total             4798
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ra14078a2.cif
_cod_data_source_block           5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'MULTI-SCAN' changed to
'multi-scan' 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 3271 2015-04-21 07:52:19Z andrius 
;
_cod_database_code               7222361
_shelx_estimated_absorpt_t_min   0.758
_shelx_estimated_absorpt_t_max   0.954
_shelxl_version_number           2013-4
_shelx_res_checksum              87434