#------------------------------------------------------------------------------
#$Date: 2025-11-29 22:06:05 +0100 (Sat 29 de Nov de 2025) $
#$Revision: 303818 $
#$URL: svn://www.crystallography.net/cod/cif/7/71/96/7719621.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_7719621
loop_
_publ_author_name
'Malik, Magdalena'
'Bieńko, Alina'
'Boča, Roman'
'Titiš, Ján'
'Rajnák, Cyril'
'Świtlicka, Anna'
'Bieńko, Dariusz C'
'Ozerov, Mykhaylo'
'Ozarowski, Andrew'
_publ_section_title
;
 Effect of the counter anion to slow magnetic relaxation of hexacoordinate
 Co(II) complexes.
;
_journal_issue                   45
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16955
_journal_page_last               16965
_journal_paper_doi               10.1039/d5dt01360g
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C14 H22 Co N2 O4, 2(N O3)'
_chemical_formula_sum            'C14 H22 Co N4 O10'
_chemical_formula_weight         465.28
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-06-26
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2021-12-01 deposited with the CCDC.	2025-10-09 downloaded from the CCDC.
;
_cell_angle_alpha                96.668(5)
_cell_angle_beta                 112.960(7)
_cell_angle_gamma                109.626(8)
_cell_formula_units_Z            1
_cell_length_a                   7.8857(8)
_cell_length_b                   8.2193(6)
_cell_length_c                   8.8245(5)
_cell_measurement_reflns_used    2397
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      28.4940
_cell_measurement_theta_min      4.3010
_cell_volume                     475.49(8)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_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)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4015
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -22.00  39.00   1.00    1.00    --   10.22  77.00  60.00   61
  2  ω    -18.00  43.00   1.00    1.00    --   10.22 -77.00 -60.00   61
  3  ω    -44.00  39.00   1.00    1.00    --  -11.31  77.00-150.00   83
  4  ω    -78.00   3.00   1.00    1.00    --  -11.31 -38.00  90.00   81
  5  ω    -84.00  13.00   1.00    1.00    --  -11.31 -38.00  30.00   97
;
_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      -0.0737677000
_diffrn_orient_matrix_UB_12      -0.0896316000
_diffrn_orient_matrix_UB_13      -0.0255966000
_diffrn_orient_matrix_UB_21      -0.0700473000
_diffrn_orient_matrix_UB_22      0.0331995000
_diffrn_orient_matrix_UB_23      0.0060032000
_diffrn_orient_matrix_UB_31      -0.0346484000
_diffrn_orient_matrix_UB_32      0.0001511000
_diffrn_orient_matrix_UB_33      -0.0871924000
_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  0.0361
_diffrn_reflns_av_unetI/netI     0.0419
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            4253
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.043
_diffrn_reflns_theta_max         25.043
_diffrn_reflns_theta_min         3.679
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.965
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59179
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.625
_exptl_crystal_description       plate
_exptl_crystal_F_000             241
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.294
_refine_diff_density_min         -0.402
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     135
_refine_ls_number_reflns         1677
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0385
_refine_ls_R_factor_gt           0.0326
_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)+(0.0429P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0754
_refine_ls_wR_factor_ref         0.0780
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1546
_reflns_number_total             1677
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d5dt01360g2.cif
_cod_data_source_block           co1mm
_cod_depositor_comments
'Adding full bibliography for 7719621--7719623.cif.'
_cod_original_cell_volume        475.49(7)
_cod_database_code               7719621
_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 99.69
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2.a Rotating group:
 O2(H2A,H2B)
2.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B)
2.c Aromatic/amide H refined with riding coordinates:
 C1(H1A), C2(H2), C3(H3), C4(H4)
2.d Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_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 1.570
_oxdiff_exptl_absorpt_empirical_full_min 0.705
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -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
Co1 Co 1.000000 0.500000 0.500000 0.02067(15) Uani 1 2 d S . P . .
O1 O 0.8604(2) 0.21855(18) 0.42222(17) 0.0302(4) Uani 1 1 d . . . . .
H1 H 0.813980 0.165116 0.479644 0.045 Uiso 1 1 calc R U . . .
O2 O 0.7371(2) 0.50201(19) 0.50929(17) 0.0305(4) Uani 1 1 d . . . . .
H2A H 0.720686 0.594098 0.483244 0.046 Uiso 1 1 d R U . . .
H2B H 0.633170 0.412758 0.430602 0.046 Uiso 1 1 d R U . . .
N1 N 0.8676(3) 0.4886(2) 0.2335(2) 0.0245(4) Uani 1 1 d . . . . .
C1 C 0.8254(3) 0.6265(3) 0.1916(3) 0.0295(5) Uani 1 1 d . . . . .
H1A H 0.851527 0.720065 0.279448 0.035 Uiso 1 1 calc R U . . .
C2 C 0.7456(4) 0.6381(3) 0.0263(3) 0.0359(6) Uani 1 1 d . . . . .
H2 H 0.721568 0.737994 0.003232 0.043 Uiso 1 1 calc R U . . .
C3 C 0.7023(4) 0.4974(3) -0.1042(3) 0.0380(6) Uani 1 1 d . . . . .
H3 H 0.649067 0.500925 -0.217593 0.046 Uiso 1 1 calc R U . . .
C4 C 0.7388(3) 0.3524(3) -0.0644(3) 0.0344(6) Uani 1 1 d . . . . .
H4 H 0.707190 0.255293 -0.151511 0.041 Uiso 1 1 calc R U . . .
C5 C 0.8221(3) 0.3497(3) 0.1042(3) 0.0265(5) Uani 1 1 d . . . . .
C6 C 0.8655(4) 0.1930(3) 0.1498(3) 0.0345(5) Uani 1 1 d . . . . .
H6A H 1.010848 0.234110 0.216287 0.041 Uiso 1 1 calc R U . . .
H6B H 0.822091 0.103737 0.044732 0.041 Uiso 1 1 calc R U . . .
C7 C 0.7646(4) 0.1035(3) 0.2506(3) 0.0384(6) Uani 1 1 d . . . . .
H7A H 0.622099 0.079721 0.195553 0.046 Uiso 1 1 calc R U . . .
H7B H 0.774804 -0.010555 0.253338 0.046 Uiso 1 1 calc R U . . .
O3 O 0.3886(3) 0.1847(2) 0.3087(2) 0.0446(4) Uani 1 1 d . . . . .
O4 O 0.2701(3) -0.0630(2) 0.3669(2) 0.0560(5) Uani 1 1 d . . . . .
O5 O 0.3132(3) 0.1838(2) 0.5187(2) 0.0491(5) Uani 1 1 d . . . . .
N2 N 0.3235(3) 0.1023(2) 0.3977(2) 0.0305(4) 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'
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'
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 Co1 O1 180.00(10) 2_766 . ?
O1 Co1 O2 88.89(6) . . ?
O1 Co1 O2 91.11(6) 2_766 . ?
O1 Co1 O2 91.11(6) . 2_766 ?
O1 Co1 O2 88.89(6) 2_766 2_766 ?
O1 Co1 N1 92.64(6) . 2_766 ?
O1 Co1 N1 87.36(6) 2_766 2_766 ?
O1 Co1 N1 92.64(6) 2_766 . ?
O1 Co1 N1 87.36(6) . . ?
O2 Co1 O2 180.0 2_766 . ?
O2 Co1 N1 89.39(6) 2_766 2_766 ?
O2 Co1 N1 90.61(6) 2_766 . ?
O2 Co1 N1 90.61(6) . 2_766 ?
O2 Co1 N1 89.39(6) . . ?
N1 Co1 N1 180.0 2_766 . ?
Co1 O1 H1 119.5 . . ?
C7 O1 Co1 126.65(13) . . ?
C7 O1 H1 109.5 . . ?
Co1 O2 H2A 109.5 . . ?
Co1 O2 H2B 109.3 . . ?
H2A O2 H2B 104.4 . . ?
C1 N1 Co1 118.04(13) . . ?
C1 N1 C5 117.70(17) . . ?
C5 N1 Co1 124.26(13) . . ?
N1 C1 H1A 118.1 . . ?
N1 C1 C2 123.8(2) . . ?
C2 C1 H1A 118.1 . . ?
C1 C2 H2 121.0 . . ?
C1 C2 C3 118.1(2) . . ?
C3 C2 H2 121.0 . . ?
C2 C3 H3 120.5 . . ?
C4 C3 C2 118.95(19) . . ?
C4 C3 H3 120.5 . . ?
C3 C4 H4 119.8 . . ?
C3 C4 C5 120.3(2) . . ?
C5 C4 H4 119.8 . . ?
N1 C5 C4 121.1(2) . . ?
N1 C5 C6 118.05(17) . . ?
C4 C5 C6 120.88(19) . . ?
C5 C6 H6A 108.6 . . ?
C5 C6 H6B 108.6 . . ?
C5 C6 C7 114.7(2) . . ?
H6A C6 H6B 107.6 . . ?
C7 C6 H6A 108.6 . . ?
C7 C6 H6B 108.6 . . ?
O1 C7 C6 109.71(18) . . ?
O1 C7 H7A 109.7 . . ?
O1 C7 H7B 109.7 . . ?
C6 C7 H7A 109.7 . . ?
C6 C7 H7B 109.7 . . ?
H7A C7 H7B 108.2 . . ?
O4 N2 O3 119.96(18) . . ?
O5 N2 O3 120.70(19) . . ?
O5 N2 O4 119.34(18) . . ?
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
Co1 O1 2.0894(13) 2_766 ?
Co1 O1 2.0894(13) . ?
Co1 O2 2.1122(15) 2_766 ?
Co1 O2 2.1122(15) . ?
Co1 N1 2.1439(16) 2_766 ?
Co1 N1 2.1439(16) . ?
O1 H1 0.8200 . ?
O1 C7 1.433(3) . ?
O2 H2A 0.8516 . ?
O2 H2B 0.8518 . ?
N1 C1 1.337(3) . ?
N1 C5 1.355(3) . ?
C1 H1A 0.9300 . ?
C1 C2 1.375(3) . ?
C2 H2 0.9300 . ?
C2 C3 1.378(3) . ?
C3 H3 0.9300 . ?
C3 C4 1.370(3) . ?
C4 H4 0.9300 . ?
C4 C5 1.379(3) . ?
C5 C6 1.500(3) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 C7 1.509(3) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
O3 N2 1.242(2) . ?
O4 N2 1.240(2) . ?
O5 N2 1.238(2) . ?
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
Co1 O1 C7 C6 30.1(3) . . . . ?
Co1 N1 C1 C2 178.16(19) . . . . ?
Co1 N1 C5 C4 -179.36(16) . . . . ?
Co1 N1 C5 C6 0.5(3) . . . . ?
N1 C1 C2 C3 1.5(4) . . . . ?
N1 C5 C6 C7 56.9(3) . . . . ?
C1 N1 C5 C4 1.2(3) . . . . ?
C1 N1 C5 C6 -178.9(2) . . . . ?
C1 C2 C3 C4 0.5(4) . . . . ?
C2 C3 C4 C5 -1.5(4) . . . . ?
C3 C4 C5 N1 0.7(3) . . . . ?
C3 C4 C5 C6 -179.1(2) . . . . ?
C4 C5 C6 C7 -123.3(2) . . . . ?
C5 N1 C1 C2 -2.4(3) . . . . ?
C5 C6 C7 O1 -71.8(3) . . . . ?
