#------------------------------------------------------------------------------
#$Date: 2020-10-06 12:32:11 +0300 (Tue, 06 Oct 2020) $
#$Revision: 257632 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/05/97/7059767.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_7059767
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 Ni0.33 O12'
_chemical_formula_sum            'C16 H22 Co0.66 N4 Ni0.33 O12'
_chemical_formula_weight         521.23
_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
;
2019-02-01 deposited with the CCDC.	2020-07-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.7330(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.6312(8)
_cell_length_b                   9.2643(4)
_cell_length_c                   11.2605(4)
_cell_measurement_reflns_used    9636
_cell_measurement_temperature    298.0
_cell_measurement_theta_max      28.311
_cell_measurement_theta_min      2.961
_cell_volume                     2141.50(15)
_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      298.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0279
_diffrn_reflns_av_unetI/netI     0.0120
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_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       -13
_diffrn_reflns_number            34629
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.329
_diffrn_reflns_theta_min         2.960
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.908
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.7115
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/2 (Bruker,2014/2) was used for absorption correction. wR2(int) was 0.0523 before and 0.0451 after correction. The Ratio of minimum to maximum transmission is 0.9541. The λ/2 correction factor is 0.00150.'
_exptl_crystal_colour            'clear greenish green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.617
_exptl_crystal_description       Block
_exptl_crystal_F_000             1077
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.430
_refine_diff_density_min         -0.434
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     157
_refine_ls_number_reflns         2671
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0316
_refine_ls_R_factor_gt           0.0276
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0322P)²+2.2512P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0676
_refine_ls_wR_factor_ref         0.0697
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2440
_reflns_number_total             2671
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0nj01016b2.cif
_cod_data_source_block           nhindncke_0m
_cod_depositor_comments
;Adding full bibliography for 7059765--7059769.cif.

 Adding full bibliography for 7059765--7059769.cif.
;
_cod_database_code               7059767
_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   0.805
_shelx_estimated_absorpt_t_min   0.760
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All H(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{Ni, Co}
3. Uiso/Uaniso restraints and constraints
Uanis(Ni) = Uanis(Co)
4. Others
 Fixed Sof: Ni(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
Ni Ni 0.500000 0.43641(3) 0.750000 0.02277(8) Uani 0.334 2 d S T P . .
Co Co 0.500000 0.43641(3) 0.750000 0.02277(8) Uani 0.666 2 d S T P . .
O1 O 0.42934(5) 0.58466(12) 0.78349(9) 0.0308(2) Uani 1 1 d . . . . .
N1 N 0.43897(5) 0.43194(12) 0.59862(9) 0.0214(2) Uani 1 1 d . . . . .
C1 C 0.38298(7) 0.60064(16) 0.70046(12) 0.0251(3) Uani 1 1 d . . . . .
O2 O 0.33756(5) 0.68630(13) 0.70108(10) 0.0392(3) Uani 1 1 d . . . . .
N2 N 0.45503(5) 0.33728(13) 0.51282(9) 0.0246(2) Uani 1 1 d . . . . .
H2 H 0.431700 0.324853 0.445945 0.030 Uiso 1 1 calc R . . . .
C2 C 0.38597(6) 0.50452(15) 0.59111(11) 0.0218(3) Uani 1 1 d . . . . .
O3 O 0.18989(6) 0.38000(16) 0.63400(13) 0.0487(3) Uani 1 1 d . . . . .
H3 H 0.185597 0.318172 0.684733 0.069(8) Uiso 1 1 calc GR . . . .
C3 C 0.33338(6) 0.50180(17) 0.48918(12) 0.0281(3) Uani 1 1 d . . . . .
H3A H 0.339255 0.416315 0.441687 0.034(5) Uiso 1 1 calc R . . . .
H3B H 0.338879 0.585094 0.438969 0.041 Uiso 1 1 calc R . . . .
O4 O 0.29256(7) 0.3086(2) 0.65874(18) 0.0813(6) Uani 1 1 d . . . . .
C4 C 0.26354(7) 0.50214(17) 0.52387(13) 0.0304(3) Uani 1 1 d . . . . .
H4A H 0.254403 0.595570 0.557324 0.037(5) Uiso 1 1 calc R . . . .
H4B H 0.233661 0.488483 0.452624 0.040(5) Uiso 1 1 calc R . . . .
O5 O 0.54257(5) 0.27438(12) 0.64250(9) 0.0316(2) Uani 1 1 d . . . . .
C5 C 0.25162(7) 0.38682(18) 0.61267(14) 0.0338(3) Uani 1 1 d . . . . .
O6 O 0.52693(5) 0.18276(12) 0.45530(9) 0.0332(2) Uani 1 1 d . . . . .
C6 C 0.51162(7) 0.26476(15) 0.54398(12) 0.0247(3) Uani 1 1 d . . . . .
C7 C 0.58282(8) 0.08542(18) 0.47872(16) 0.0372(4) Uani 1 1 d . . . . .
H7A H 0.576414 0.020968 0.544425 0.047(5) Uiso 1 1 calc R . . . .
H7B H 0.622514 0.140085 0.498703 0.056 Uiso 1 1 calc R . . . .
C8 C 0.58679(9) 0.00140(19) 0.36560(17) 0.0436(4) Uani 1 1 d . . . . .
H8A H 0.596840 0.065737 0.303170 0.065 Uiso 1 1 calc GR . . . .
H8B H 0.545755 -0.044844 0.343137 0.065 Uiso 1 1 calc GR . . . .
H8C H 0.620326 -0.070405 0.378201 0.065 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'
Ni Ni 0.3393 1.1124 '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'
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 Ni O1 96.61(6) . 2_656 ?
O1 Ni O5 91.48(4) . 2_656 ?
O1 Ni O5 153.52(4) 2_656 2_656 ?
O1 Ni O5 153.52(4) . . ?
O1 Ni O5 91.48(4) 2_656 . ?
N1 Ni O1 104.59(4) 2_656 . ?
N1 Ni O1 77.02(4) 2_656 2_656 ?
N1 Ni O1 104.59(4) . 2_656 ?
N1 Ni O1 77.02(4) . . ?
N1 Ni N1 177.64(7) 2_656 . ?
N1 Ni O5 76.54(4) . . ?
N1 Ni O5 101.78(4) . 2_656 ?
N1 Ni O5 101.79(4) 2_656 . ?
N1 Ni O5 76.54(4) 2_656 2_656 ?
O5 Ni O5 92.39(6) 2_656 . ?
C1 O1 Ni 115.72(9) . . ?
N2 N1 Ni 115.78(8) . . ?
C2 N1 Ni 120.17(9) . . ?
C2 N1 N2 123.73(11) . . ?
O1 C1 C2 115.80(12) . . ?
O2 C1 O1 125.90(13) . . ?
O2 C1 C2 118.29(12) . . ?
N1 N2 H2 123.4 . . ?
C6 N2 N1 113.30(11) . . ?
C6 N2 H2 123.4 . . ?
N1 C2 C1 110.90(11) . . ?
N1 C2 C3 126.19(12) . . ?
C3 C2 C1 122.90(12) . . ?
C5 O3 H3 109.5 . . ?
C2 C3 H3A 108.4 . . ?
C2 C3 H3B 108.4 . . ?
C2 C3 C4 115.63(11) . . ?
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 112.95(12) . . ?
C5 C4 H4A 109.0 . . ?
C5 C4 H4B 109.0 . . ?
C6 O5 Ni 110.60(9) . . ?
O3 C5 C4 112.36(13) . . ?
O4 C5 O3 123.10(16) . . ?
O4 C5 C4 124.54(14) . . ?
C6 O6 C7 117.50(12) . . ?
O5 C6 N2 123.53(12) . . ?
O5 C6 O6 125.76(13) . . ?
O6 C6 N2 110.69(11) . . ?
O6 C7 H7A 110.5 . . ?
O6 C7 H7B 110.5 . . ?
O6 C7 C8 105.94(13) . . ?
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
Ni O1 2.0649(10) 2_656 ?
Ni O1 2.0648(10) . ?
Ni N1 2.0159(11) . ?
Ni N1 2.0159(11) 2_656 ?
Ni O5 2.1685(10) 2_656 ?
Ni O5 2.1685(10) . ?
O1 C1 1.2777(17) . ?
N1 N2 1.3697(15) . ?
N1 C2 1.2793(17) . ?
C1 O2 1.2286(17) . ?
C1 C2 1.5258(18) . ?
N2 H2 0.8600 . ?
N2 C6 1.3622(17) . ?
C2 C3 1.4988(17) . ?
O3 H3 0.8200 . ?
O3 C5 1.3209(18) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.5300(18) . ?
O4 C5 1.192(2) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 C5 1.500(2) . ?
O5 C6 1.2268(17) . ?
O6 C6 1.3180(17) . ?
O6 C7 1.4669(18) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C8 1.502(2) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
