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_7059765
_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 Co N4 O12'
_chemical_formula_sum            'C16 H22 Co N4 O12'
_chemical_formula_weight         521.30
_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             2015-10-07
_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                 96.0872(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.6210(2)
_cell_length_b                   9.05593(12)
_cell_length_c                   11.20988(13)
_cell_measurement_reflns_used    22533
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      32.5460
_cell_measurement_theta_min      2.4560
_cell_volume                     2081.56(4)
_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 16.1511
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_details
;
  1 omega  -52.00   46.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.4992   38.0000  -60.0000 98

  2 omega  -99.00   18.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.4992  -19.0000  -60.0000 117

  3 omega  -48.00   42.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.4992   57.0000  120.0000 90

  4 omega   -6.00   83.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       27.1242 -122.0000 -131.0000 89

  5 omega   15.00  102.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       27.1242 -154.0000   69.0000 87

  6 omega   32.00  104.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       27.1242 -178.0000 -180.0000 72

  7 omega  -42.00   48.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       27.1242  -57.0000 -120.0000 90

  8 omega  -95.00   -5.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.4992  -57.0000 -120.0000 90

  9 omega   -3.00   97.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       27.1242   77.0000   60.0000 100

 10 omega    6.00   96.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       27.1242   57.0000  150.0000 90

 11 omega   -3.00   97.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       27.1242   77.0000  -60.0000 100

 12 omega   35.00  103.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       27.1242  178.0000  150.0000 68

 13 omega   -3.00   97.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       27.1242   77.0000 -180.0000 100

 14 omega  -95.00   -5.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.4992  -57.0000  150.0000 90

 15 omega  -46.00  100.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       27.1242    0.0000 -150.0000 146

 16 omega    2.00  100.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       27.1242   38.0000 -180.0000 98

 17 omega  -46.00  100.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       27.1242    0.0000 -180.0000 146

 18 omega    6.00   96.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       27.1242   57.0000    0.0000 90

 19 omega    6.00   96.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       27.1242   57.0000 -120.0000 90

 20 omega  -46.00  100.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       27.1242    0.0000 -120.0000 146
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0004793000
_diffrn_orient_matrix_UB_12      -0.0565898000
_diffrn_orient_matrix_UB_13      0.0436272000
_diffrn_orient_matrix_UB_21      -0.0344009000
_diffrn_orient_matrix_UB_22      0.0065016000
_diffrn_orient_matrix_UB_23      -0.0024845000
_diffrn_orient_matrix_UB_31      -0.0036588000
_diffrn_orient_matrix_UB_32      -0.0537332000
_diffrn_orient_matrix_UB_33      -0.0462625000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0307
_diffrn_reflns_av_unetI/netI     0.0125
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            52185
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         32.737
_diffrn_reflns_theta_min         3.000
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_source_current           35
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.899
_exptl_absorpt_correction_T_max  0.841
_exptl_absorpt_correction_T_min  0.678
_exptl_absorpt_correction_type   analytical
_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)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.663
_exptl_crystal_description       block
_exptl_crystal_F_000             1076
_exptl_crystal_recrystallization_method
'The material was recrystallised from water by slow evaporation'
_exptl_crystal_size_max          0.6063
_exptl_crystal_size_mid          0.2714
_exptl_crystal_size_min          0.2263
_refine_diff_density_max         0.472
_refine_diff_density_min         -0.498
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       0.0019(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     156
_refine_ls_number_reflns         3735
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0285
_refine_ls_R_factor_gt           0.0266
_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^)+(0.0308P)^2^+2.6088P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0664
_refine_ls_wR_factor_ref         0.0675
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3552
_reflns_number_total             3735
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj01016b2.cif
_cod_data_source_block           sp_coznkgec
_cod_depositor_comments
;Adding full bibliography for 7059765--7059769.cif.

 Adding full bibliography for 7059765--7059769.cif.
;
_cod_database_code               7059765
_chemical_oxdiff_formula         C16CoN4O12
_reflns_odcompleteness_completeness 99.96
_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, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C21(H21A,H21B), C22(H22A,H22B)
2.b Aromatic/amide H refined with riding coordinates:
 N2(H2)
2.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C)
;
_shelx_res_checksum              74706
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2015-10-06
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems 700 PlusSeries'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in perfluoroether oil'
_olex2_submission_original_sample_id CoZnKGEC
_olex2_submission_special_instructions 'No special instructions were received'