Spin transitions in ferric catecholate complexes mediated by outer-sphere counteranions.
Chegerev, Maxim; Demidov, Oleg; Vasilyev, Pavel; Efimov, Nikolay; Kubrin, Stanislav; Starikov, Andrey; Vlasenko, Valery; Piskunov, Alexander; Shapovalova, Svetlana; Guda, Alexander; Rusalev, Yury; Soldatov, Alexander; Dalton transactions (Cambridge, England : 2003) 51 (2022) 10909–10919; doi:10.1039/d2dt01207c

data_7710601
_publ_section_title
;
 Spin transitions in ferric catecholate complexes mediated by outer-sphere
 counteranions.
;
_journal_issue                   29
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10909
_journal_page_last               10919
_journal_paper_doi               10.1039/d2dt01207c
_journal_volume                  51
_journal_year                    2022
_chemical_compound_source        'Rostov-on-Don, Russia'
_chemical_formula_moiety
'C32 H38 Fe N4 O2, 0.5(H2 O), B0.439 F2.242, B0.561 F1.758'
_chemical_formula_sum            'C32 H39 B F4 Fe N4 O2.5'
_chemical_formula_weight         662.33
_chemical_name_common
'(3,6-Di-tert-butylcatecholato)-(tris(2-pyridylmethyl)amine)-iron(iii) tetrafluoroborate'
_chemical_name_systematic
'(3,6-Di-tert-butylcatecholato)-(tris(2-pyridylmethyl)amine)-iron(iii) tetrafluoroborate'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-09-08
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2022-04-03 deposited with the CCDC.	2022-06-27 downloaded from the CCDC.
;
_cell_angle_alpha                97.060(2)
_cell_angle_beta                 93.064(3)
_cell_angle_gamma                106.882(3)
_cell_formula_units_Z            2
_cell_length_a                   8.3740(3)
_cell_length_b                   10.2623(3)
_cell_length_c                   19.6717(6)
_cell_measurement_reflns_used    10714
_cell_measurement_temperature    100.02(11)
_cell_measurement_theta_max      76.0130
_cell_measurement_theta_min      4.5000
_cell_volume                     1598.31(9)
_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 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.02(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2529
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_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    -69.00  33.00   1.00    5.16    --  -40.60  57.00-120.00  102
  2  \w   -113.00 -12.00   1.00    5.16    --  -40.60 -57.00  90.00  101
  3  \w    -21.00  73.00   1.00    5.16    --   40.60 -77.00 -60.00   94
  4  \w      7.00  42.00   1.00    5.16    --   40.60  82.00  70.40   35
  5  \w     16.00 115.00   1.00    5.16    --   40.60  38.00  30.00   99
  6  \w    -34.00  65.00   1.00    5.16    --   40.60 -38.00 -30.00   99
  7  \w      6.00  81.00   1.00    5.16    --   40.60 -99.00-120.00   75
  8  \w     86.00 178.00   1.00   20.63    --  112.00  45.00   0.00   92
  9  \w     30.00 106.00   1.00   20.63    --  112.00 -95.00-120.00   76
 10  \w     36.00 109.00   1.00   20.63    --  112.00-111.00-180.00   73
 11  \w    104.00 178.00   1.00   20.63    --  112.00 111.00-180.00   74
 12  \w    103.00 178.00   1.00   20.63    --  112.00  77.00  90.00   75
 13  \w    104.00 178.00   1.00   20.63    --  112.00 111.00 -60.00   74
 14  \w     36.00 109.00   1.00   20.63    --  112.00-111.00 -30.00   73
 15  \w     40.00 141.00   1.00   20.63    --  112.00 -61.00-180.00  101
 16  \w     86.00 178.00   1.00   20.63    --  112.00  45.00  30.00   92
 17  \w     36.00 109.00   1.00   20.63    --  112.00-111.00 -90.00   73
 18  \w    104.00 178.00   1.00   20.63    --  112.00 111.00  30.00   74
 19  \w     30.00 106.00   1.00   20.63    --  112.00 -95.00-180.00   76
 20  \w    104.00 178.00   1.00   20.63    --  112.00 111.00   0.00   74
 21  \w     36.00 109.00   1.00   20.63    --  112.00-111.00  60.00   73
 22  \w     39.00 138.00   1.00   20.63    --  112.00 -45.00-120.00   99
 23  \w     36.00 109.00   1.00   20.63    --  112.00-113.00  16.00   73
 24  \w     36.00 140.00   1.00   20.63    --  112.00 -30.00   0.00  104
 25  \w     40.00 141.00   1.00   20.63    --  112.00 -61.00-120.00  101
 26  \w     39.00 138.00   1.00   20.63    --  112.00 -45.00   0.00   99
 27  \w     84.00 178.00   1.00   20.63    --  112.00  30.00 -30.00   94
 28  \w    103.00 178.00   1.00   20.63    --  112.00  77.00-120.00   75
 29  \w     30.00 106.00   1.00   20.63    --  112.00 -95.00 150.00   76
 30  \w     36.00 109.00   1.00   20.63    --  112.00-111.00 -60.00   73
 31  \w     30.00 106.00   1.00   20.63    --  112.00 -95.00-150.00   76
 32  \w    104.00 178.00   1.00   20.63    --  112.00 111.00 -30.00   74
 33  \w     39.00 138.00   1.00   20.63    --  112.00 -45.00 -60.00   99
 34  \w     36.00 140.00   1.00   20.63    --  112.00 -30.00-150.00  104
 35  \w     40.00 141.00   1.00   20.63    --  112.00 -61.00 120.00  101
 36  \w     36.00 145.00   1.00   20.63    --  112.00 -77.00 -30.00  109
 37  \w     36.00 109.00   1.00   20.63    --  112.00-111.00-150.00   73
 38  \w     36.00 109.00   1.00   20.63    --  112.00-111.00-120.00   73
 39  \w     36.00 109.00   1.00   20.63    --  112.00-111.00 120.00   73
 40  \w     33.00 146.00   1.00   20.63    --  112.00 -83.00   4.78  113
 41  \w    113.00 141.00   1.00   20.63    --  112.00  77.00-180.00   28
 42  \w    120.00 145.00   1.00   20.63    --  112.00 -77.00  90.00   25
 43  \w     65.00  93.00   1.00   20.63    --  112.00  13.00  -8.88   28
 44  \w     76.00 112.00   1.00   20.63    --  112.00 -15.00 -30.00   36
 45  \w    123.00 164.00   1.00   20.63    --  112.00 -15.00 -30.00   41
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1621694000
_diffrn_orient_matrix_UB_12      0.0134370000
_diffrn_orient_matrix_UB_13      -0.0356976000
_diffrn_orient_matrix_UB_21      -0.0952548000
_diffrn_orient_matrix_UB_22      -0.0008109000
_diffrn_orient_matrix_UB_23      -0.0693278000
_diffrn_orient_matrix_UB_31      0.0437948000
_diffrn_orient_matrix_UB_32      0.1579791000
_diffrn_orient_matrix_UB_33      0.0142044000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0550
_diffrn_reflns_av_unetI/netI     0.0408
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            32634
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.451
_diffrn_reflns_theta_min         4.550
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.303
_exptl_absorpt_correction_T_max  0.971
_exptl_absorpt_correction_T_min  0.904
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.376
_exptl_crystal_description       plate
_exptl_crystal_F_000             692
_exptl_crystal_size_max          0.366
_exptl_crystal_size_mid          0.286
_exptl_crystal_size_min          0.101
_refine_diff_density_max         0.525
_refine_diff_density_min         -0.450
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     455
_refine_ls_number_reflns         6673
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0576
_refine_ls_R_factor_gt           0.0519
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0558P)^2^+1.8116P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1264
_refine_ls_wR_factor_ref         0.1317
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6087
_reflns_number_total             6673
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01207c2.cif
_cod_data_source_block           tpafe36bf4_100_2
_cod_depositor_comments
'Adding full bibliography for 7710599--7710604.cif.'
_cod_original_formula_sum        'C32 H39 B F4 Fe N4 O2.50'
_cod_database_code               7710601
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C32 H38 Fe N4 O2, B F4'
_shelx_estimated_absorpt_t_max   0.670
_shelx_estimated_absorpt_t_min   0.302
_reflns_odcompleteness_completeness 98.19
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     77.17
_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 C(H,H,H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(F2) = Uanis(F2A)
3. Others
 Sof(F4)=Sof(F1)=Sof(B1A)=Sof(F3)=Sof(F2)=1-FVAR(1)
 Sof(F2A)=Sof(F3A)=Sof(B1)=Sof(F1A)=Sof(F4A)=FVAR(1)
 Fixed Sof: O1S(0.5) H1SA(0.5) H1SB(0.5)
4.a Free rotating group:
 O1S(H1SA,H1SB)
4.b Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C20(H20A,H20B), C32(H32A,H32B)
4.c Aromatic/amide H refined with riding coordinates:
 C27(H27), C29(H29), C24(H24), C4(H4), C5(H5), C23(H23), C21(H21), C22(H22),
 C15(H15), C28(H28), C30(H30), C18(H18), C16(H16), C17(H17)
4.d Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C8(H8A,H8B,H8C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C),
 C10(H10A,H10B,H10C), C14(H14A,H14B,H14C)
;
_shelx_res_checksum              30125
_shelx_hkl_checksum              86324
_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 2.016
_oxdiff_exptl_absorpt_empirical_full_min 0.615