#------------------------------------------------------------------------------
#$Date: 2025-10-06 11:23:24 +0200 (Mon 06 de Oct de 2025) $
#$Revision: 302641 $
#$URL: svn://www.crystallography.net/cod/cif/7/71/93/7719349.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_7719349
loop_
_publ_author_name
'Sawka, Jacek'
'Bieńko, Alina'
'Świtlicka, Anna'
'Penkala, Mateusz'
'Bieńko, Dariusz'
'Rajnák, Cyril'
'Titiš, Ján'
'Boča, Roman'
'Ozarowski, Andrew'
_publ_section_title
;
 Large magnetic anisotropy of Ni(II) polynuclear complexes confirmed by
 very unusual HFEPR spectra: relaxation behaviour of six-coordinate Ni(II)
 dimers.
;
_journal_issue                   36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13421
_journal_page_last               13425
_journal_paper_doi               10.1039/d5dt01264c
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C13 H11 N8 Ni O, C2 N3'
_chemical_formula_sum            'C15 H11 N11 Ni O'
_chemical_formula_weight         420.06
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2025-05-15
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2025-05-15 deposited with the CCDC.	2025-07-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.668(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.0526(5)
_cell_length_b                   8.7823(4)
_cell_length_c                   28.8665(13)
_cell_measurement_reflns_used    4243
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.5400
_cell_measurement_theta_min      3.9450
_cell_volume                     3488.9(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4015
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -44.00  64.00   1.00    5.54    --  -11.86  77.00-150.00  108
  2  ω    -88.00  21.00   1.00    5.54    --  -11.86 -77.00  60.00  109
  3  ω   -100.00 -75.00   1.00    5.54    --  -11.86-179.00   0.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0080022000
_diffrn_orient_matrix_UB_12      -0.0792526000
_diffrn_orient_matrix_UB_13      0.0020216000
_diffrn_orient_matrix_UB_21      0.0095812000
_diffrn_orient_matrix_UB_22      -0.0115339000
_diffrn_orient_matrix_UB_23      -0.0229466000
_diffrn_orient_matrix_UB_31      0.0499964000
_diffrn_orient_matrix_UB_32      -0.0104822000
_diffrn_orient_matrix_UB_33      0.0099483000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0186
_diffrn_reflns_av_unetI/netI     0.0196
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            9341
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.048
_diffrn_reflns_theta_max         25.048
_diffrn_reflns_theta_min         3.545
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.146
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71806
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.599
_exptl_crystal_description       prism
_exptl_crystal_F_000             1712
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.467
_refine_diff_density_min         -0.526
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         3093
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0345
_refine_ls_R_factor_gt           0.0286
_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)+(0.0388P)²+3.1081P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0746
_refine_ls_wR_factor_ref         0.0774
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2745
_reflns_number_total             3093
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d5dt01264c3.cif
_cod_data_source_block           ni23
_cod_depositor_comments
'Adding full bibliography for 7719348--7719349.cif.'
_cod_database_code               7719349
_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.
;
_reflns_odcompleteness_completeness 99.66
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Rotating group:
 O1(H1A,H1B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11)
;
_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 1.344
_oxdiff_exptl_absorpt_empirical_full_min 0.889
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -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
Ni1 Ni 0.15423(2) 0.30079(3) 0.09865(2) 0.02920(11) Uani 1 1 d . . . . .
O1 O 0.30089(10) 0.22827(17) 0.11395(6) 0.0403(4) Uani 1 1 d . . . . .
H1A H 0.335161 0.289347 0.133987 0.060 Uiso 1 1 d R U . . .
H1B H 0.325754 0.236730 0.089106 0.060 Uiso 1 1 d R U . . .
N1 N 0.15942(13) 0.3572(2) 0.17019(6) 0.0382(4) Uani 1 1 d . . . . .
N2 N 0.12849(13) 0.2406(2) 0.19442(6) 0.0394(4) Uani 1 1 d . . . . .
N3 N 0.11742(12) 0.1033(2) 0.12674(6) 0.0336(4) Uani 1 1 d . . . . .
N4 N 0.13308(12) 0.1472(2) 0.04078(6) 0.0374(4) Uani 1 1 d . . . . .
N5 N 0.11782(13) 0.0014(2) 0.05476(7) 0.0403(4) Uani 1 1 d . . . . .
N6 N 0.01273(13) 0.3697(2) 0.07913(7) 0.0434(5) Uani 1 1 d . . . . .
N8 N 0.20829(14) 0.4934(2) 0.07533(7) 0.0447(5) Uani 1 1 d . . . . .
N9 N 0.34121(15) 0.6008(4) 0.04445(8) 0.0752(9) Uani 1 1 d . . . . .
C1 C 0.17520(17) 0.4722(3) 0.20044(9) 0.0492(6) Uani 1 1 d . . . . .
H1 H 0.196644 0.568098 0.193500 0.059 Uiso 1 1 calc R U . . .
C2 C 0.1554(2) 0.4302(4) 0.24413(9) 0.0606(7) Uani 1 1 d . . . . .
H2 H 0.161376 0.490835 0.270982 0.073 Uiso 1 1 calc R U . . .
C3 C 0.1258(2) 0.2846(3) 0.23960(8) 0.0550(7) Uani 1 1 d . . . . .
H3 H 0.107107 0.224896 0.262821 0.066 Uiso 1 1 calc R U . . .
C4 C 0.10857(15) 0.0995(3) 0.17178(8) 0.0384(5) Uani 1 1 d . . . . .
C5 C 0.08322(18) -0.0307(3) 0.19274(9) 0.0531(6) Uani 1 1 d . . . . .
H5 H 0.076896 -0.031744 0.224186 0.064 Uiso 1 1 calc R U . . .
C6 C 0.0677(2) -0.1592(3) 0.16521(11) 0.0600(7) Uani 1 1 d . . . . .
H6 H 0.049425 -0.248808 0.178196 0.072 Uiso 1 1 calc R U . . .
C7 C 0.07849(19) -0.1587(3) 0.11843(11) 0.0543(7) Uani 1 1 d . . . . .
H7 H 0.068963 -0.246175 0.099913 0.065 Uiso 1 1 calc R U . . .
C8 C 0.10405(15) -0.0221(2) 0.10083(8) 0.0386(5) Uani 1 1 d . . . . .
C9 C 0.11318(18) -0.0973(3) 0.01799(10) 0.0561(7) Uani 1 1 d . . . . .
H9 H 0.103726 -0.201995 0.018834 0.067 Uiso 1 1 calc R U . . .
C10 C 0.12490(19) -0.0145(4) -0.02005(10) 0.0610(8) Uani 1 1 d . . . . .
H10 H 0.124966 -0.050552 -0.050340 0.073 Uiso 1 1 calc R U . . .
C11 C 0.13687(16) 0.1359(3) -0.00440(8) 0.0475(6) Uani 1 1 d . . . . .
H11 H 0.146308 0.217821 -0.023395 0.057 Uiso 1 1 calc R U . . .
C12 C -0.06835(16) 0.3881(3) 0.06538(7) 0.0400(5) Uani 1 1 d . . . . .
C13 C 0.27419(15) 0.5428(2) 0.06296(7) 0.0360(5) Uani 1 1 d . . . . .
N10 N 0.1607(2) 0.5747(3) 0.36426(9) 0.0674(7) Uani 1 1 d . . . . .
N11 N 0.1202(3) 0.7887(3) 0.31108(9) 0.0825(9) Uani 1 1 d . . . . .
N12 N 0.08401(15) 1.0518(2) 0.32697(8) 0.0525(5) Uani 1 1 d . . . . .
C14 C 0.14153(18) 0.6809(3) 0.34157(9) 0.0441(6) Uani 1 1 d . . . . .
C15 C 0.10116(18) 0.9265(3) 0.32251(8) 0.0430(5) Uani 1 1 d . . . . .
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'
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 Ni1 N4 87.05(6) . . ?
N1 Ni1 O1 91.54(7) . . ?
N1 Ni1 N4 153.08(7) . . ?
N3 Ni1 O1 88.59(6) . . ?
N3 Ni1 N1 76.72(7) . . ?
N3 Ni1 N4 76.37(7) . . ?
N3 Ni1 N6 92.91(7) . . ?
N6 Ni1 O1 176.15(7) . . ?
N6 Ni1 N1 92.26(7) . . ?
N6 Ni1 N4 89.86(7) . . ?
N8 Ni1 O1 84.60(7) . . ?
N8 Ni1 N1 100.85(8) . . ?
N8 Ni1 N3 172.72(7) . . ?
N8 Ni1 N4 105.76(8) . . ?
N8 Ni1 N6 94.04(8) . . ?
Ni1 O1 H1A 110.0 . . ?
Ni1 O1 H1B 110.0 . . ?
H1A O1 H1B 103.8 . . ?
N2 N1 Ni1 112.03(13) . . ?
C1 N1 Ni1 142.41(17) . . ?
C1 N1 N2 105.27(19) . . ?
N1 N2 C3 110.5(2) . . ?
N1 N2 C4 118.70(17) . . ?
C3 N2 C4 130.7(2) . . ?
C4 N3 Ni1 119.63(15) . . ?
C8 N3 Ni1 120.33(15) . . ?
C8 N3 C4 120.02(19) . . ?
N5 N4 Ni1 111.53(13) . . ?
C11 N4 Ni1 143.05(18) . . ?
C11 N4 N5 105.09(19) . . ?
N4 N5 C8 118.52(17) . . ?
C9 N5 N4 110.5(2) . . ?
C9 N5 C8 130.9(2) . . ?
C12 N6 Ni1 170.2(2) . . ?
C13 N8 Ni1 143.42(18) . . ?
C13 N9 C12 124.8(2) . 6_665 ?
N1 C1 H1 124.5 . . ?
N1 C1 C2 110.9(2) . . ?
C2 C1 H1 124.5 . . ?
C1 C2 H2 126.9 . . ?
C3 C2 C1 106.1(2) . . ?
C3 C2 H2 126.9 . . ?
N2 C3 H3 126.4 . . ?
C2 C3 N2 107.1(2) . . ?
C2 C3 H3 126.4 . . ?
N3 C4 N2 112.54(18) . . ?
N3 C4 C5 122.3(2) . . ?
C5 C4 N2 125.1(2) . . ?
C4 C5 H5 121.5 . . ?
C6 C5 C4 117.0(2) . . ?
C6 C5 H5 121.5 . . ?
C5 C6 H6 119.2 . . ?
C5 C6 C7 121.7(2) . . ?
C7 C6 H6 119.2 . . ?
C6 C7 H7 121.7 . . ?
C8 C7 C6 116.7(2) . . ?
C8 C7 H7 121.7 . . ?
N3 C8 N5 112.59(19) . . ?
N3 C8 C7 122.3(2) . . ?
C7 C8 N5 125.1(2) . . ?
N5 C9 H9 126.4 . . ?
C10 C9 N5 107.2(2) . . ?
C10 C9 H9 126.4 . . ?
C9 C10 H10 127.1 . . ?
C9 C10 C11 105.8(2) . . ?
C11 C10 H10 127.1 . . ?
N4 C11 C10 111.4(2) . . ?
N4 C11 H11 124.3 . . ?
C10 C11 H11 124.3 . . ?
N6 C12 N9 172.0(2) . 6_565 ?
N8 C13 N9 173.3(2) . . ?
C14 N11 C15 123.0(2) . . ?
N10 C14 N11 172.1(3) . . ?
N12 C15 N11 171.7(3) . . ?
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 O1 2.1166(14) . ?
Ni1 N1 2.1106(18) . ?
Ni1 N3 2.0256(17) . ?
Ni1 N4 2.1205(18) . ?
Ni1 N6 2.0455(18) . ?
Ni1 N8 2.0246(19) . ?
O1 H1A 0.8610 . ?
O1 H1B 0.8623 . ?
N1 N2 1.360(3) . ?
N1 C1 1.324(3) . ?
N2 C3 1.368(3) . ?
N2 C4 1.403(3) . ?
N3 C4 1.331(3) . ?
N3 C8 1.323(3) . ?
N4 N5 1.373(3) . ?
N4 C11 1.320(3) . ?
N5 C8 1.397(3) . ?
N5 C9 1.362(3) . ?
N6 C12 1.140(3) . ?
N8 C13 1.143(3) . ?
N9 C12 1.296(3) 6_665 ?
N9 C13 1.279(3) . ?
C1 H1 0.9300 . ?
C1 C2 1.395(4) . ?
C2 H2 0.9300 . ?
C2 C3 1.342(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.374(3) . ?
C5 H5 0.9300 . ?
C5 C6 1.371(4) . ?
C6 H6 0.9300 . ?
C6 C7 1.389(4) . ?
C7 H7 0.9300 . ?
C7 C8 1.379(3) . ?
C9 H9 0.9300 . ?
C9 C10 1.354(4) . ?
C10 H10 0.9300 . ?
C10 C11 1.396(4) . ?
C11 H11 0.9300 . ?
N10 C14 1.141(3) . ?
N11 C14 1.286(3) . ?
N11 C15 1.297(3) . ?
N12 C15 1.139(3) . ?
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 N1 N2 C3 -175.47(15) . . . . ?
Ni1 N1 N2 C4 6.8(2) . . . . ?
Ni1 N1 C1 C2 173.18(19) . . . . ?
Ni1 N3 C4 N2 -0.8(2) . . . . ?
Ni1 N3 C4 C5 179.59(18) . . . . ?
Ni1 N3 C8 N5 -0.2(2) . . . . ?
Ni1 N3 C8 C7 -179.67(17) . . . . ?
Ni1 N4 N5 C8 9.2(2) . . . . ?
Ni1 N4 N5 C9 -174.52(15) . . . . ?
Ni1 N4 C11 C10 171.86(19) . . . . ?
N1 N2 C3 C2 0.0(3) . . . . ?
N1 N2 C4 N3 -4.2(3) . . . . ?
N1 N2 C4 C5 175.4(2) . . . . ?
N1 C1 C2 C3 -0.5(3) . . . . ?
N2 N1 C1 C2 0.4(3) . . . . ?
N2 C4 C5 C6 -179.1(2) . . . . ?
N3 C4 C5 C6 0.4(4) . . . . ?
N4 N5 C8 N3 -6.2(3) . . . . ?
N4 N5 C8 C7 173.2(2) . . . . ?
N4 N5 C9 C10 -0.4(3) . . . . ?
N5 N4 C11 C10 -0.3(3) . . . . ?
N5 C9 C10 C11 0.2(3) . . . . ?
C1 N1 N2 C3 -0.3(2) . . . . ?
C1 N1 N2 C4 -177.99(19) . . . . ?
C1 C2 C3 N2 0.3(3) . . . . ?
C3 N2 C4 N3 178.6(2) . . . . ?
C3 N2 C4 C5 -1.8(4) . . . . ?
C4 N2 C3 C2 177.3(2) . . . . ?
C4 N3 C8 N5 -178.91(18) . . . . ?
C4 N3 C8 C7 1.6(3) . . . . ?
C4 C5 C6 C7 1.0(4) . . . . ?
C5 C6 C7 C8 -1.0(4) . . . . ?
C6 C7 C8 N3 -0.3(4) . . . . ?
C6 C7 C8 N5 -179.7(2) . . . . ?
C8 N3 C4 N2 177.87(18) . . . . ?
C8 N3 C4 C5 -1.7(3) . . . . ?
C8 N5 C9 C10 175.3(2) . . . . ?
C9 N5 C8 N3 178.4(2) . . . . ?
C9 N5 C8 C7 -2.2(4) . . . . ?
C9 C10 C11 N4 0.1(3) . . . . ?
C11 N4 N5 C8 -175.85(18) . . . . ?
C11 N4 N5 C9 0.4(2) . . . . ?
