Spin canting and slow magnetic relaxation in mononuclear cobalt(II) sulfadiazine ternary complexes.
Villa-Pérez, Cristian; Zabala-Lekuona, Andoni; Vitorica-Yrezabal, Iñigo J; Seco, José Manuel; Cepeda, Javier; Echeverría, Gustavo Alberto; Soria, Delia Beatriz; Dalton transactions (Cambridge, England : 2003) 53 (2024) 3254–3266; doi:10.1039/d3dt02359a

data_7714964
_publ_section_title
;
 Spin canting and slow magnetic relaxation in mononuclear cobalt(II)
 sulfadiazine ternary complexes.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3254
_journal_page_last               3266
_journal_paper_doi               10.1039/d3dt02359a
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C28 H21 Cl N6 Ni O2 S'
_chemical_formula_sum            'C28 H21 Cl N6 Ni O2 S'
_chemical_formula_weight         599.73
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-11-14
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-11-21 deposited with the CCDC.	2024-01-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.955(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.1866(3)
_cell_length_b                   28.6498(10)
_cell_length_c                   10.0473(4)
_cell_measurement_reflns_used    10388
_cell_measurement_temperature    232(80)
_cell_measurement_theta_max      29.7310
_cell_measurement_theta_min      2.1790
_cell_volume                     2604.58(17)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_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_environment      N~2~
_diffrn_ambient_temperature      232(80)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.843
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     29.00  66.00   0.50   50.00    --   15.42-140.00 169.00   74
  2  \w     20.00  46.00   0.50   50.00    --   15.42-130.00 -16.00   52
  3  \w    -22.00  21.00   0.50   50.00    --  -14.80 -99.00-120.00   86
  4  \w    -62.00  39.00   0.50   50.00    --   15.42 -57.00 150.00  202
  5  \w     15.00  40.00   0.50   50.00    --   15.42 -99.00-180.00   50
  6  \w    -42.00  42.00   0.50   50.00    --   15.42 -57.00-120.00  168
  7  \w     -4.00  54.00   0.50   50.00    --  -14.80  57.00 -30.00  116
  8  \w    -89.00 -49.00   0.50   50.00    --  -14.80 -57.00  30.00   80
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0094584000
_diffrn_orient_matrix_UB_12      -0.0233381000
_diffrn_orient_matrix_UB_13      0.0204416000
_diffrn_orient_matrix_UB_21      0.0337377000
_diffrn_orient_matrix_UB_22      -0.0082099000
_diffrn_orient_matrix_UB_23      -0.0539474000
_diffrn_orient_matrix_UB_31      0.0701132000
_diffrn_orient_matrix_UB_32      0.0007943000
_diffrn_orient_matrix_UB_33      0.0425684000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0535
_diffrn_reflns_av_unetI/netI     0.0687
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.843
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            23391
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.843
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.009
_diffrn_reflns_theta_min         2.177
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.967
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97289
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dull green'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.529
_exptl_crystal_description       plate
_exptl_crystal_F_000             1232
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Ethanol'
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.368
_refine_diff_density_min         -0.423
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         6403
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0810
_refine_ls_R_factor_gt           0.0451
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0467P)^2^+0.0974P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0965
_refine_ls_wR_factor_ref         0.1068
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4382
_reflns_number_total             6403
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02359a2.cif
_cod_data_source_block           Compound3
_cod_depositor_comments
'Adding full bibliography for 7714962--7714964.cif.'
_cod_database_code               7714964
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         Cu2Dy1C20H20N2O4Cl2
_shelx_estimated_absorpt_t_max   0.990
_shelx_estimated_absorpt_t_min   0.972
_reflns_odcompleteness_completeness 99.96
_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 N(H,H) groups
2.a Riding coordinates:
 N117(H11A,H11B)
2.b Aromatic/amide H refined with riding coordinates:
 C112(H112), C115(H115), C14(H14), C113(H113), C116(H116), C15(H15), C39(H39),
 C33(H33), C24(H24), C30(H30), C16(H16), C34(H34), C27(H27), C25(H25), C29(H29),
  C26(H26), C38(H38), C36(H36), C37(H37)
;
_shelx_res_checksum              52948
_shelx_hkl_checksum              60322
_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 1.333
_oxdiff_exptl_absorpt_empirical_full_min 0.886