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_7710603
_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, 2.002(F3 P0.5)'
_chemical_formula_sum            'C32 H38 F6.01 Fe N4 O2 P'
_chemical_formula_weight         711.60
_chemical_name_common
'(3,6-Di-tert-butylcatecholato)-(tris(2-pyridylmethyl)amine)-iron(iii) hexafluorophosphate'
_chemical_name_systematic
'(3,6-Di-tert-butylcatecholato)-(tris(2-pyridylmethyl)amine)-iron(iii) hexafluorophosphate'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      60
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-09-09
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.8272(3)
_cell_length_b                   18.6423(2)
_cell_length_c                   15.0968(2)
_cell_measurement_reflns_used    16830
_cell_measurement_temperature    100.01(15)
_cell_measurement_theta_max      76.1430
_cell_measurement_theta_min      3.6700
_cell_volume                     6705.91(14)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (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 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(15)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2529
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_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    -74.00  34.00   1.00    7.00    --  -41.72  77.00-120.00  108
  2  \w      9.00  42.00   1.00    7.00    --   41.72  76.00-167.26   33
  3  \w      8.00  42.00   1.00    7.00    --   41.72  81.00 -68.41   34
  4  \w      7.00  34.00   1.00    7.00    --   41.72  83.00  -5.86   27
  5  \w     27.00  98.00   1.00    7.00    --   41.72-125.00  90.00   71
  6  \w     36.00 109.00   1.00   28.00    --  112.00-111.00  60.00   73
  7  \w     83.00 178.00   1.00   28.00    --  112.00  61.00   0.00   95
  8  \w     36.00 109.00   1.00   28.00    --  112.00-111.00   0.00   73
  9  \w     36.00 104.00   1.00   28.00    --  112.00-111.00-150.00   68
 10  \w     63.00 118.00   1.00   28.00    --  112.00 178.00   0.00   55
 11  \w    117.00 154.00   1.00   28.00    --  112.00 111.00 -90.00   37
 12  \w    103.00 174.00   1.00   28.00    --  112.00  77.00 120.00   71
 13  \w    114.00 141.00   1.00   28.00    --  112.00 178.00 -30.00   27
 14  \w     91.00 123.00   1.00   28.00    --  112.00 178.00-150.00   32
 15  \w     80.00 109.00   1.00   28.00    --  112.00-111.00 150.00   29
 16  \w    116.00 142.00   1.00   28.00    --  112.00  77.00  30.00   26
 17  \w     83.00 177.00   1.00   28.00    --  112.00  61.00  90.00   94
 18  \w     52.00  80.00   1.00   28.00    --  112.00 -95.00 -60.00   28
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0490831000
_diffrn_orient_matrix_UB_12      0.0187229000
_diffrn_orient_matrix_UB_13      -0.0624056000
_diffrn_orient_matrix_UB_21      0.0169875000
_diffrn_orient_matrix_UB_22      0.0796152000
_diffrn_orient_matrix_UB_23      0.0033128000
_diffrn_orient_matrix_UB_31      0.0385352000
_diffrn_orient_matrix_UB_32      -0.0112674000
_diffrn_orient_matrix_UB_33      -0.0807587000
_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  0.0274
_diffrn_reflns_av_unetI/netI     0.0198
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            37644
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.412
_diffrn_reflns_theta_min         3.010
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.661
_exptl_absorpt_correction_T_max  0.969
_exptl_absorpt_correction_T_min  0.891
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
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    1.410
_exptl_crystal_description       block
_exptl_crystal_F_000             2952
_exptl_crystal_size_max          0.362
_exptl_crystal_size_mid          0.086
_exptl_crystal_size_min          0.067
_refine_diff_density_max         0.621
_refine_diff_density_min         -0.652
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         7007
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0339
_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^)+(0.0401P)^2^+4.8656P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0842
_refine_ls_wR_factor_ref         0.0877
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6453
_reflns_number_total             7007
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01207c2.cif
_cod_data_source_block           tpa36fepf6_100_2
_cod_depositor_comments
'Adding full bibliography for 7710599--7710604.cif.'
_cod_database_code               7710603
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C32 H38 F6 Fe N4 O2 P'
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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
2. Others
 Sof(F9)=1-FVAR(1)
 Sof(F8)=Sof(F5)=Sof(F7)=Sof(F10)=Sof(F6)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C20(H20A,H20B), C32(H32A,H32B)
3.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C24(H24), C5(H5), C16(H16), C21(H21), C4(H4), C27(H27), C23(H23),
 C18(H18), C22(H22), C28(H28), C17(H17), C30(H30), C29(H29)
3.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C12(H12A,H12B,H12C),
 C10(H10A,H10B,H10C), C14(H14A,H14B,H14C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              70509
_shelx_hkl_checksum              5550
_shelx_fab_checksum              41709
_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 1.707
_oxdiff_exptl_absorpt_empirical_full_min 0.589