#------------------------------------------------------------------------------
#$Date: 2020-10-06 12:32:11 +0300 (Tue, 06 Oct 2020) $
#$Revision: 257632 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/05/97/7059768.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7059768
loop_
_publ_author_name
'Parveen, Sheikdawood'
'Nguyen, Hung Huy'
'Premkumar, Thathan'
'Puschmann, Horst'
'Govindarajan, Subbiah'
_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
 α-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 Co0.67 N4 O12 Zn0.33'
_chemical_formula_sum            'C16 H22 Co0.66 N4 O12 Zn0.33'
_chemical_formula_weight         523.46
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-01-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-03-26 deposited with the CCDC.	2020-07-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.7590(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.6689(5)
_cell_length_b                   9.2368(3)
_cell_length_c                   11.2492(3)
_cell_measurement_reflns_used    9975
_cell_measurement_temperature    300.0
_cell_measurement_theta_max      28.283
_cell_measurement_theta_min      2.966
_cell_volume                     2136.80(10)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      300.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 Quest CMOS'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_av_unetI/netI     0.0165
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            23907
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.354
_diffrn_reflns_theta_min         2.966
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.991
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6628
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/2 (Bruker,2014/2) was used for absorption correction. wR2(int) was 0.0739 before and 0.0537 after correction. The Ratio of minimum to maximum transmission is 0.8888. The λ/2 correction factor is 0.00150.'
_exptl_crystal_colour            'clear light red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.627
_exptl_crystal_description       Block
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.295
_refine_diff_density_min         -0.378
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.170
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     152
_refine_ls_number_reflns         2667
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.170
_refine_ls_R_factor_all          0.0346
_refine_ls_R_factor_gt           0.0297
_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/[σ²(Fo²)+(0.0373P)²+1.4492P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0760
_refine_ls_wR_factor_ref         0.0783
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2395
_reflns_number_total             2667
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0nj01016b2.cif
_cod_data_source_block           nhindzckm_0m
_cod_depositor_comments
;Adding full bibliography for 7059765--7059769.cif.

 Adding full bibliography for 7059765--7059769.cif.
;
_cod_database_code               7059768
_shelx_shelxl_version_number     2016/6
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.826
_shelx_estimated_absorpt_t_min   0.755
_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, All O(H) groups
2. Shared sites
{Co, Zn}
3. Uiso/Uaniso restraints and constraints
Uanis(Co) = Uanis(Zn)
4. Others
 Fixed Sof: Zn(0.167) Co(0.333)
5.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C7(H7A,H7B)
5.b Aromatic/amide H refined with riding coordinates:
 N2(H2)
5.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C)
5.d Idealised tetrahedral OH refined as rotating group:
 O3(H3)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn Zn 0.500000 0.55170(3) 0.250000 0.02511(9) Uani 0.334 2 d S T P . .
Co Co 0.500000 0.55170(3) 0.250000 0.02511(9) Uani 0.666 2 d S T P . .
O1 O 0.57348(6) 0.40609(14) 0.22147(9) 0.0343(3) Uani 1 1 d . . . . .
N1 N 0.56260(6) 0.56526(13) 0.40435(10) 0.0240(2) Uani 1 1 d . . . . .
C1 C 0.61963(7) 0.39465(17) 0.30456(13) 0.0274(3) Uani 1 1 d . . . . .
O2 O 0.66586(6) 0.31105(14) 0.30593(11) 0.0421(3) Uani 1 1 d . . . . .
N2 N 0.54670(6) 0.66178(14) 0.48881(10) 0.0274(3) Uani 1 1 d . . . . .
H2 H 0.570421 0.676220 0.555022 0.033 Uiso 1 1 calc R . . . .
C2 C 0.61590(7) 0.49396(16) 0.41239(12) 0.0239(3) Uani 1 1 d . . . . .
O3 O 0.81033(6) 0.62086(18) 0.36411(13) 0.0508(4) Uani 1 1 d . . . . .
H3 H 0.813800 0.680191 0.310903 0.076 Uiso 1 1 calc GR . . . .
C3 C 0.66848(7) 0.5000(2) 0.51405(14) 0.0304(3) Uani 1 1 d . . . . .
H3A H 0.663556 0.417321 0.565538 0.037 Uiso 1 1 calc R . . . .
H3B H 0.662179 0.586498 0.560415 0.037 Uiso 1 1 calc R . . . .
O4 O 0.70723(8) 0.6881(2) 0.3387(2) 0.0828(7) Uani 1 1 d . . . . .
C4 C 0.73818(7) 0.5008(2) 0.47905(15) 0.0331(3) Uani 1 1 d . . . . .
H4A H 0.767939 0.518732 0.549792 0.040 Uiso 1 1 calc R . . . .
H4B H 0.748134 0.405992 0.448515 0.040 Uiso 1 1 calc R . . . .
O5 O 0.45781(6) 0.71991(13) 0.36135(10) 0.0356(3) Uani 1 1 d . . . . .
C5 C 0.74895(8) 0.6128(2) 0.38652(16) 0.0361(4) Uani 1 1 d . . . . .
O6 O 0.47510(6) 0.81702(13) 0.54657(10) 0.0355(3) Uani 1 1 d . . . . .
C6 C 0.48968(7) 0.73299(17) 0.45816(13) 0.0269(3) Uani 1 1 d . . . . .
C7 C 0.41868(8) 0.9128(2) 0.52366(17) 0.0385(4) Uani 1 1 d . . . . .
H7A H 0.379334 0.856651 0.504761 0.046 Uiso 1 1 calc R . . . .
H7B H 0.424274 0.977067 0.457268 0.046 Uiso 1 1 calc R . . . .
C8 C 0.41483(10) 0.9979(2) 0.63645(19) 0.0461(4) Uani 1 1 d . . . . .
H8A H 0.380586 1.068173 0.624170 0.069 Uiso 1 1 calc GR . . . .
H8B H 0.455436 1.046450 0.657453 0.069 Uiso 1 1 calc GR . . . .
H8C H 0.405993 0.933508 0.699825 0.069 Uiso 1 1 calc GR . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Co O1 99.31(7) . 2_655 ?
O1 Co O5 91.78(5) . 2_655 ?
O1 Co O5 150.68(4) 2_655 2_655 ?
O1 Co O5 150.67(4) . . ?
O1 Co O5 91.78(5) 2_655 . ?
N1 Co O1 108.41(4) 2_655 . ?
N1 Co O1 76.28(4) 2_655 2_655 ?
N1 Co O1 108.41(4) . 2_655 ?
N1 Co O1 76.28(4) . . ?
N1 Co N1 173.04(7) 2_655 . ?
N1 Co O5 74.47(4) . . ?
N1 Co O5 100.55(4) . 2_655 ?
N1 Co O5 100.55(4) 2_655 . ?
N1 Co O5 74.47(4) 2_655 2_655 ?
O5 Co O5 91.56(7) 2_655 . ?
C1 O1 Co 116.52(10) . . ?
N2 N1 Co 116.78(9) . . ?
C2 N1 Co 119.44(10) . . ?
C2 N1 N2 123.51(12) . . ?
O1 C1 C2 116.08(13) . . ?
O2 C1 O1 125.97(14) . . ?
O2 C1 C2 117.95(13) . . ?
N1 N2 H2 123.2 . . ?
C6 N2 N1 113.63(12) . . ?
C6 N2 H2 123.2 . . ?
N1 C2 C1 111.38(12) . . ?
N1 C2 C3 126.07(13) . . ?
C3 C2 C1 122.53(13) . . ?
C5 O3 H3 109.5 . . ?
C2 C3 H3A 108.4 . . ?
C2 C3 H3B 108.4 . . ?
C2 C3 C4 115.67(12) . . ?
H3A C3 H3B 107.4 . . ?
C4 C3 H3A 108.4 . . ?
C4 C3 H3B 108.4 . . ?
C3 C4 H4A 109.0 . . ?
C3 C4 H4B 109.0 . . ?
H4A C4 H4B 107.8 . . ?
C5 C4 C3 112.99(13) . . ?
C5 C4 H4A 109.0 . . ?
C5 C4 H4B 109.0 . . ?
C6 O5 Co 111.34(10) . . ?
O3 C5 C4 112.57(14) . . ?
O4 C5 O3 123.07(17) . . ?
O4 C5 C4 124.35(16) . . ?
C6 O6 C7 117.39(13) . . ?
O5 C6 N2 123.59(14) . . ?
O5 C6 O6 125.92(14) . . ?
O6 C6 N2 110.48(12) . . ?
O6 C7 H7A 110.5 . . ?
O6 C7 H7B 110.5 . . ?
O6 C7 C8 106.03(15) . . ?
H7A C7 H7B 108.7 . . ?
C8 C7 H7A 110.5 . . ?
C8 C7 H7B 110.5 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co O1 2.0776(12) 2_655 ?
Co O1 2.0776(12) . ?
Co N1 2.0624(12) . ?
Co N1 2.0623(12) 2_655 ?
Co O5 2.2278(12) 2_655 ?
Co O5 2.2278(12) . ?
O1 C1 1.2712(18) . ?
N1 N2 1.3668(17) . ?
N1 C2 1.2790(19) . ?
C1 O2 1.2274(19) . ?
C1 C2 1.529(2) . ?
N2 H2 0.8600 . ?
N2 C6 1.3634(19) . ?
C2 C3 1.498(2) . ?
O3 H3 0.8200 . ?
O3 C5 1.320(2) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.531(2) . ?
O4 C5 1.194(2) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 C5 1.500(2) . ?
O5 C6 1.2209(18) . ?
O6 C6 1.3201(18) . ?
O6 C7 1.466(2) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C8 1.501(3) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
