Nano spinel cobaltites and their catalytic and electrochemical properties: facile synthesis of metal (Co, Ni, and Zn) and mixed metal (Co–Ni and Co–Zn) complexes of Schiff bases prepared from α-ketoglutaric acid and ethyl carbazate
Parveen, Sheikdawood; Nguyen, Hung Huy; Premkumar, Thathan; Puschmann, Horst; Govindarajan, Subbiah; New Journal of Chemistry 44 (2020) 12729–12740; doi:10.1039/D0NJ01016B

data_7059766
_publ_section_title
;
 Nano spinel cobaltites and their catalytic and electrochemical
 properties: facile synthesis of metal (Co, Ni, and Zn) and mixed metal
 (Co--Ni and Co--Zn) complexes of Schiff bases prepared from
 \a-ketoglutaric acid and ethyl carbazate
;
_journal_issue                   29
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              12729
_journal_page_last               12740
_journal_paper_doi               10.1039/D0NJ01016B
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety         'C16 H22 N4 O12 Zn'
_chemical_formula_sum            'C16 H22 N4 O12 Zn'
_chemical_formula_weight         527.74
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-10-05
_audit_creation_method
;
Olex2 1.2-dev
(compiled 2015.09.07 svn.r3215 for OlexSys, GUI svn.r3563)
;
_audit_update_record
;
2018-12-06 deposited with the CCDC.	2020-07-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.230(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.6603(9)
_cell_length_b                   9.0466(4)
_cell_length_c                   11.1969(5)
_cell_measurement_reflns_used    4267
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.7550
_cell_measurement_theta_min      2.9770
_cell_volume                     2080.40(16)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0756
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -94.00 -35.00   1.00    4.00    --  -18.25-178.00-150.00   59
  2  \w    -24.00  24.00   1.00    4.00    --  -18.25-100.00  60.00   48
  3  \w    -91.00  26.00   1.00    4.00    --  -18.25 -19.00  60.00  117
  4  \w    -24.00  24.00   1.00    4.00    --  -18.25-100.00-150.00   48
  5  \w    -50.00  29.00   1.00    4.00    --   18.72 -57.00  30.00   79
  6  \w    -51.00 -26.00   1.00    4.00    --   18.72 -77.00 150.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0018672000
_diffrn_orient_matrix_UB_12      0.0776736000
_diffrn_orient_matrix_UB_13      0.0076041000
_diffrn_orient_matrix_UB_21      0.0343397000
_diffrn_orient_matrix_UB_22      0.0032650000
_diffrn_orient_matrix_UB_23      0.0127096000
_diffrn_orient_matrix_UB_31      0.0030429000
_diffrn_orient_matrix_UB_32      0.0102965000
_diffrn_orient_matrix_UB_33      -0.0619476000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0286
_diffrn_reflns_av_unetI/netI     0.0279
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7565
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        27.496
_diffrn_reflns_theta_max         27.496
_diffrn_reflns_theta_min         3.002
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_source_current           35
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    1.255
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80790
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.685
_exptl_crystal_description       block
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.587
_exptl_crystal_size_mid          0.309
_exptl_crystal_size_min          0.309
_refine_diff_density_max         0.420
_refine_diff_density_min         -0.346
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     156
_refine_ls_number_reflns         2352
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0271
_refine_ls_R_factor_gt           0.0251
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0245P)^2^+2.5548P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0609
_refine_ls_wR_factor_ref         0.0619
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2214
_reflns_number_total             2352
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj01016b2.cif
_cod_data_source_block           sp_znkgec
_cod_depositor_comments
;Adding full bibliography for 7059765--7059769.cif.

 Adding full bibliography for 7059765--7059769.cif.
;
_cod_database_code               7059766
_chemical_oxdiff_formula         C16H22N4O12Zn
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C6(H6A,H6B), C7(H7A,H7B)
2.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C)
2.c Idealised tetrahedral OH refined as rotating group:
 O5(H5)
;
_shelx_res_checksum              67147
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2015-10-05
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems 700 Series'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in perfluoroether oil'
_olex2_submission_original_sample_id ZnKGEC
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.184
_oxdiff_exptl_absorpt_empirical_full_min 0.885