#------------------------------------------------------------------------------
#$Date: 2026-02-13 02:24:13 +0100 (Fri 13 de Feb de 2026) $
#$Revision: 304355 $
#$URL: svn://www.crystallography.net/cod/cif/7/06/42/7064235.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_7064235
loop_
_publ_author_name
'Pandey, Sharmila'
'Mukhopadhyay, Narottam'
'Lloret, Francesc'
'Mukherjee, Rabindranath'
_publ_section_title
;
 Hetero-bimetallic complexes of pyridine-/pyrazine-2-carboxamide ligands:
 synthesis, structure, redox properties and magnetism
;
_journal_issue                   6
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              2721
_journal_page_last               2731
_journal_paper_doi               10.1039/D5NJ03831F
_journal_volume                  50
_journal_year                    2026
_chemical_formula_moiety         'C36 H30 Cl Co N9 Ni O3, 6[H2O]'
_chemical_formula_sum            'C36 H42 Cl Co N9 Ni O9'
_chemical_formula_weight         897.87
_space_group_crystal_system      trigonal
_space_group_IT_number           147
_space_group_name_Hall           '-P 3'
_space_group_name_H-M_alt        'P -3'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2025-12-07
_audit_creation_method
;
Olex2 1.5
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7314)
;
_audit_update_record
;
2025-12-14 deposited with the CCDC.	2025-12-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   15.380(2)
_cell_length_b                   15.380(2)
_cell_length_c                   10.4419(17)
_cell_measurement_reflns_used    2187
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      23.76
_cell_measurement_theta_min      2.48
_cell_volume                     2139.1(5)
_computing_cell_refinement       'SAINT v6.45A (Bruker, 2003)'
_computing_data_collection       'Bruker SMART APEX'
_computing_data_reduction        'SAINT v6.45A (Bruker, 2003)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0700
_diffrn_reflns_av_unetI/netI     0.0578
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            11101
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.012
_diffrn_reflns_theta_max         25.012
_diffrn_reflns_theta_min         2.478
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.951
_exptl_absorpt_correction_T_max  0.827
_exptl_absorpt_correction_T_min  0.677
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS v.2.10 (Bruker,2003) was used for absorption correction.
R(int) was 0.0521 before and 0.0360 after correction.
The Ratio of minimum to maximum transmission is 0.6110.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_description       block
_exptl_crystal_F_000             930
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.006
_refine_diff_density_min         -0.393
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         2512
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0576
_refine_ls_R_factor_gt           0.0435
_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)+(0.0724P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1131
_refine_ls_wR_factor_ref         0.1228
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1988
_reflns_number_total             2512
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d5nj03831f2.cif
_cod_data_source_block           17janc
_cod_original_cell_volume        2139.1(7)
_cod_database_code               7064235
_shelx_shelxl_version_number     2018/3
_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   0.827
_shelx_estimated_absorpt_t_min   0.677
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C8(H8), C11(H11), C2(H2), C4(H4), C10(H10), C3(H3)
2.b Idealised Me refined as rotating group:
 C00J(H00a,H00b,H00c)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 119 electrons were 
found in a volume of 558Å³ in 1 void per unit cell. 
This is consistent with the presence of 
6[H2O] per Asymmetric Unit 
which account for 120 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
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
Ni1 Ni 0.666667 0.333333 0.14241(5) 0.0223(2) Uani 1 3 d S T P . .
Co1 Co 0.666667 0.333333 0.48207(6) 0.0266(2) Uani 1 3 d S T P . .
Cl1 Cl 0.666667 0.333333 0.69878(11) 0.0352(3) Uani 1 3 d S T P . .
O004 O 0.70223(14) 0.09340(14) 0.25089(19) 0.0311(5) Uani 1 1 d . . . . .
N2 N 0.64740(16) 0.20840(16) 0.2430(2) 0.0233(5) Uani 1 1 d . . . . .
N1 N 0.76270(17) 0.29793(17) 0.0428(2) 0.0249(5) Uani 1 1 d . . . . .
N3 N 0.56332(18) 0.19087(17) 0.4357(2) 0.0264(6) Uani 1 1 d . . . . .
C7 C 0.5651(2) 0.1505(2) 0.3232(3) 0.0245(6) Uani 1 1 d . . . . .
C6 C 0.7030(2) 0.1688(2) 0.2070(3) 0.0247(6) Uani 1 1 d . . . . .
C5 C 0.7731(2) 0.2249(2) 0.0968(3) 0.0264(6) Uani 1 1 d . . . . .
C1 C 0.8224(2) 0.3474(2) -0.0566(3) 0.0288(7) Uani 1 1 d . . . . .
H1 H 0.815634 0.399553 -0.095466 0.035 Uiso 1 1 calc R U . . .
C9 C 0.4025(2) 0.0050(2) 0.3620(3) 0.0318(7) Uani 1 1 d . . . . .
C8 C 0.4847(2) 0.0587(2) 0.2837(3) 0.0288(7) Uani 1 1 d . . . . .
H8 H 0.486476 0.032806 0.201748 0.035 Uiso 1 1 calc R U . . .
C11 C 0.4837(2) 0.1370(2) 0.5153(3) 0.0312(7) Uani 1 1 d . . . . .
H11 H 0.483544 0.164064 0.597042 0.037 Uiso 1 1 calc R U . . .
C2 C 0.8925(2) 0.3261(2) -0.1048(3) 0.0337(7) Uani 1 1 d . . . . .
H2 H 0.933127 0.362487 -0.175708 0.040 Uiso 1 1 calc R U . . .
C4 C 0.8425(2) 0.1994(2) 0.0536(3) 0.0345(7) Uani 1 1 d . . . . .
H4 H 0.848292 0.147015 0.093619 0.041 Uiso 1 1 calc R U . . .
C10 C 0.4039(2) 0.0454(2) 0.4823(3) 0.0346(7) Uani 1 1 d . . . . .
H10 H 0.350135 0.009811 0.540658 0.041 Uiso 1 1 calc R U . . .
C3 C 0.9031(2) 0.2512(2) -0.0486(3) 0.0381(8) Uani 1 1 d . . . . .
H3 H 0.951608 0.235350 -0.079654 0.046 Uiso 1 1 calc R U . . .
C00J C 0.3152(2) -0.0926(2) 0.3194(4) 0.0451(9) Uani 1 1 d . . . . .
H00A H 0.294471 -0.084811 0.233373 0.068 Uiso 1 1 calc R U . . .
H00B H 0.259167 -0.112721 0.379087 0.068 Uiso 1 1 calc R U . . .
H00C H 0.334731 -0.144271 0.317686 0.068 Uiso 1 1 calc R U . . .
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'
Cl Cl 0.1484 0.1585 '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
N2 Ni1 N2 96.69(8) . 2_655 ?
N2 Ni1 N2 96.69(8) . 3_665 ?
N2 Ni1 N2 96.68(8) 2_655 3_665 ?
N2 Ni1 N1 78.64(9) 3_665 3_665 ?
N2 Ni1 N1 174.05(8) . 2_655 ?
N2 Ni1 N1 78.64(9) 2_655 2_655 ?
N2 Ni1 N1 78.64(9) . . ?
N2 Ni1 N1 174.04(8) 2_655 3_665 ?
N2 Ni1 N1 87.57(8) 3_665 2_655 ?
N2 Ni1 N1 174.05(8) 3_665 . ?
N2 Ni1 N1 87.58(8) . 3_665 ?
N2 Ni1 N1 87.58(8) 2_655 . ?
N1 Ni1 N1 97.37(8) . 2_655 ?
N1 Ni1 N1 97.36(8) 3_665 2_655 ?
N1 Ni1 N1 97.37(8) . 3_665 ?
N3 Co1 Cl1 103.88(7) . . ?
N3 Co1 Cl1 103.88(7) 3_665 . ?
N3 Co1 Cl1 103.88(7) 2_655 . ?
N3 Co1 N3 114.44(5) 3_665 . ?
N3 Co1 N3 114.44(5) 2_655 3_665 ?
N3 Co1 N3 114.44(5) 2_655 . ?
C7 N2 Ni1 123.74(18) . . ?
C6 N2 Ni1 117.04(18) . . ?
C6 N2 C7 117.4(2) . . ?
C5 N1 Ni1 114.00(18) . . ?
C5 N1 C1 117.9(2) . . ?
C1 N1 Ni1 127.6(2) . . ?
C7 N3 Co1 121.85(19) . . ?
C7 N3 C11 118.3(3) . . ?
C11 N3 Co1 119.54(19) . . ?
N3 C7 N2 116.8(2) . . ?
N3 C7 C8 121.1(3) . . ?
C8 C7 N2 121.9(3) . . ?
O004 C6 N2 128.1(3) . . ?
O004 C6 C5 118.8(2) . . ?
N2 C6 C5 113.1(2) . . ?
N1 C5 C6 116.6(2) . . ?
N1 C5 C4 122.3(3) . . ?
C4 C5 C6 121.1(3) . . ?
N1 C1 H1 118.5 . . ?
N1 C1 C2 123.1(3) . . ?
C2 C1 H1 118.5 . . ?
C8 C9 C10 117.5(3) . . ?
C8 C9 C00J 121.2(3) . . ?
C10 C9 C00J 121.4(3) . . ?
C7 C8 H8 119.6 . . ?
C9 C8 C7 120.9(3) . . ?
C9 C8 H8 119.6 . . ?
N3 C11 H11 118.6 . . ?
N3 C11 C10 122.7(3) . . ?
C10 C11 H11 118.6 . . ?
C1 C2 H2 120.6 . . ?
C1 C2 C3 118.8(3) . . ?
C3 C2 H2 120.6 . . ?
C5 C4 H4 120.6 . . ?
C3 C4 C5 118.9(3) . . ?
C3 C4 H4 120.6 . . ?
C9 C10 H10 120.3 . . ?
C11 C10 C9 119.3(3) . . ?
C11 C10 H10 120.3 . . ?
C2 C3 C4 119.1(3) . . ?
C2 C3 H3 120.4 . . ?
C4 C3 H3 120.4 . . ?
C9 C00J H00A 109.5 . . ?
C9 C00J H00B 109.5 . . ?
C9 C00J H00C 109.5 . . ?
H00A C00J H00B 109.5 . . ?
H00A C00J H00C 109.5 . . ?
H00B C00J H00C 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
Ni1 N2 2.077(2) . ?
Ni1 N2 2.077(2) 2_655 ?
Ni1 N2 2.077(2) 3_665 ?
Ni1 N1 2.089(2) . ?
Ni1 N1 2.089(2) 2_655 ?
Ni1 N1 2.089(2) 3_665 ?
Co1 Cl1 2.2628(14) . ?
Co1 N3 2.020(2) . ?
Co1 N3 2.020(2) 2_655 ?
Co1 N3 2.020(2) 3_665 ?
O004 C6 1.242(3) . ?
N2 C7 1.403(3) . ?
N2 C6 1.328(3) . ?
N1 C5 1.337(4) . ?
N1 C1 1.342(3) . ?
N3 C7 1.336(4) . ?
N3 C11 1.365(4) . ?
C7 C8 1.395(4) . ?
C6 C5 1.517(4) . ?
C5 C4 1.384(4) . ?
C1 H1 0.9500 . ?
C1 C2 1.370(4) . ?
C9 C8 1.380(4) . ?
C9 C10 1.396(4) . ?
C9 C00J 1.497(4) . ?
C8 H8 0.9500 . ?
C11 H11 0.9500 . ?
C11 C10 1.371(4) . ?
C2 H2 0.9500 . ?
C2 C3 1.373(4) . ?
C4 H4 0.9500 . ?
C4 C3 1.378(4) . ?
C10 H10 0.9500 . ?
C3 H3 0.9500 . ?
C00J H00A 0.9800 . ?
C00J H00B 0.9800 . ?
C00J H00C 0.9800 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 N2 C7 N3 -73.6(3) . . . . ?
Ni1 N2 C7 C8 101.2(3) . . . . ?
Ni1 N2 C6 O004 -178.1(2) . . . . ?
Ni1 N2 C6 C5 0.7(3) . . . . ?
Ni1 N1 C5 C6 9.3(3) . . . . ?
Ni1 N1 C5 C4 -172.1(2) . . . . ?
Ni1 N1 C1 C2 171.0(2) . . . . ?
Co1 N3 C7 N2 5.6(3) . . . . ?
Co1 N3 C7 C8 -169.2(2) . . . . ?
Co1 N3 C11 C10 171.0(2) . . . . ?
O004 C6 C5 N1 172.2(2) . . . . ?
O004 C6 C5 C4 -6.5(4) . . . . ?
N2 C7 C8 C9 -177.2(3) . . . . ?
N2 C6 C5 N1 -6.7(3) . . . . ?
N2 C6 C5 C4 174.6(3) . . . . ?
N1 C5 C4 C3 0.1(4) . . . . ?
N1 C1 C2 C3 -0.4(4) . . . . ?
N3 C7 C8 C9 -2.6(4) . . . . ?
N3 C11 C10 C9 -0.6(4) . . . . ?
C7 N2 C6 O004 -12.8(4) . . . . ?
C7 N2 C6 C5 166.0(2) . . . . ?
C7 N3 C11 C10 -2.8(4) . . . . ?
C6 N2 C7 N3 122.2(3) . . . . ?
C6 N2 C7 C8 -63.0(4) . . . . ?
C6 C5 C4 C3 178.7(3) . . . . ?
C5 N1 C1 C2 0.2(4) . . . . ?
C5 C4 C3 C2 -0.4(5) . . . . ?
C1 N1 C5 C6 -178.6(2) . . . . ?
C1 N1 C5 C4 0.0(4) . . . . ?
C1 C2 C3 C4 0.5(5) . . . . ?
C8 C9 C10 C11 2.4(4) . . . . ?
C11 N3 C7 N2 179.2(2) . . . . ?
C11 N3 C7 C8 4.4(4) . . . . ?
C10 C9 C8 C7 -0.9(4) . . . . ?
C00J C9 C8 C7 178.9(3) . . . . ?
C00J C9 C10 C11 -177.4(3) . . . . ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 -0.325 557.8 118.7 '12 H2O'
