Single-ion anisotropy and exchange coupling in cobalt(ii)-radical complexes: insights from magnetic and ab initio studies
Gransbury, Gemma K.; Boulon, Marie-Emmanuelle; Mole, Richard A.; Gable, Robert W.; Moubaraki, Boujemaa; Murray, Keith S.; Sorace, Lorenzo; Soncini, Alessandro; Boskovic, Colette; Chemical Science  (2019) –; doi:10.1039/C9SC00914K

data_1552222
_publ_section_title
;
 Single-ion anisotropy and exchange coupling in cobalt(ii)-radical
 complexes: insights from magnetic and ab initio studies
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C9SC00914K
_journal_year                    2019
_chemical_formula_moiety         'C35 H44 Co N4 O2, F6 P, C7 H8'
_chemical_formula_sum            'C42 H52 Co F6 N4 O2 P'
_chemical_formula_weight         848.77
_chemical_name_systematic
'(3,5-di-tert-butyl-catecholato)-(tris(6-methyl-2-pyridylmethyl)amine)-cobalt(II) hexafluorophosphate toluene solvate'
_chemical_properties_physical    paramagnetic
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc21n833
_audit_creation_date             2018-11-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-02-09 deposited with the CCDC.    2019-08-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.1148(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.57434(4)
_cell_length_b                   31.75314(10)
_cell_length_c                   22.05467(7)
_cell_measurement_reflns_used    175384
_cell_measurement_temperature    99.99(13)
_cell_measurement_theta_max      77.8210
_cell_measurement_theta_min      2.7780
_cell_volume                     8084.67(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(13)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_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     27.00  54.00   0.50    0.32    --   48.30  77.00 -30.00   54
  2  \w     27.00  53.00   0.50    0.32    --   48.30  77.00 -90.00   52
  3  \w     38.00  72.00   0.50    0.32    --   48.30  38.00-150.00   68
  4  \w     27.00  55.00   0.50    0.32    --   48.30  77.00-120.00   56
  5  \w     46.00 123.00   0.50    0.32    --   48.30  19.00 -60.00  154
  6  \w     82.00 118.00   0.50    0.32    --   48.30  19.00  30.00   72
  7  \w     60.00  87.00   0.50    0.32    --   48.30  77.00  90.00   54
  8  \w     47.00  80.00   0.50    0.32    --   48.30  19.00  30.00   66
  9  \w     38.00  97.00   0.50    0.32    --   48.30  38.00  60.00  118
 10  \w     94.00 178.00   0.50    1.26    --  107.75 122.00  40.00  168
 11  \w    145.00 177.00   0.50    1.26    --  107.75  64.00  61.23   64
 12  \w    142.00 178.00   0.50    1.26    --  107.75  77.00 -19.95   72
 13  \w    135.00 178.00   0.50    1.26    --  107.75  77.00  90.00   86
 14  \w    125.00 171.00   0.50    1.26    --  107.75  77.00  30.00   92
 15  \w    129.00 178.00   0.50    1.26    --  107.75  77.00   0.00   98
 16  \w    127.00 172.00   0.50    1.26    --  107.75  30.00   0.00   90
 17  \w     91.00 116.00   0.50    1.26    --  107.75  64.00  61.23   50
 18  \w     86.00 117.00   0.50    1.26    --  107.75  77.00 120.00   62
 19  \w    118.00 177.00   0.50    1.26    --  107.75  78.00 144.75  118
 20  \w     94.00 178.00   0.50    1.26    --  107.75  61.00 120.00  168
 21  \w     88.00 147.00   0.50    1.26    --  107.75  77.00  60.00  118
 22  \w     93.00 154.00   0.50    1.26    --  107.75  61.00  30.00  122
 23  \w     86.00 178.00   0.50    1.26    --  107.75  77.00 -60.00  184
 24  \w    142.00 168.00   0.50    1.26    --  107.75  79.00-159.30   52
 25  \w    108.00 134.00   0.50    1.26    --  107.75 150.00-157.00   52
 26  \w     86.00 124.00   0.50    1.26    --  107.75  79.00-159.30   76
 27  \w     93.00 175.00   0.50    1.26    --  107.75  61.00-180.00  164
 28  \w     94.00 159.00   0.50    1.26    --  107.75  61.00 -90.00  130
 29  \w     89.00 168.00   0.50    1.26    --  107.75  72.00-137.56  158
 30  \w    101.00 176.00   0.50    1.26    --  107.75  61.00-120.00  150
 31  \w     87.00 130.00   0.50    1.26    --  107.75  77.00 -19.95   86
 32  \w     86.00 172.00   0.50    1.26    --  107.75  77.00 -30.00  172
 33  \w     91.00 173.00   0.50    1.26    --  107.75  68.00  77.27  164
 34  \w     93.00 144.00   0.50    1.26    --  107.75  61.00 150.00  102
 35  \w     87.00 114.00   0.50    1.26    --  107.75  78.00 144.75   54
 36  \w     86.00 132.00   0.50    1.26    --  107.75  77.00 150.00   92
 37  \w     86.00 122.00   0.50    1.26    --  107.75  77.00  90.00   72
 38  \w     86.00 120.00   0.50    1.26    --  107.75  77.00  30.00   68
 39  \w     84.00 155.00   0.50    1.26    --  107.75  81.00 -52.99  142
 40  \w     86.00 176.00   0.50    1.26    --  107.75  77.00 -90.00  180
 41  \w     86.00 125.00   0.50    1.26    --  107.75  77.00   0.00   78
 42  \w     75.00 121.00   0.50    0.32    --   48.30 150.00-157.00   92
 43  \w     86.00 178.00   0.50    1.26    --  107.75  77.00-175.98  184
 44  \w    104.00 130.00   0.50    1.26    --  107.75 -77.00 -30.00   52
 45  \w     69.00 101.00   0.50    1.26    --  107.75-122.00 -40.00   64
 46  \w     47.00 116.00   0.50    1.26    --  107.75-125.00 -90.00  138
 47  \w     47.00  73.00   0.50    1.26    --  107.75 -61.00-180.00   52
 48  \w     37.00  62.00   0.50    1.26    --  107.75 -45.00-150.00   50
 49  \w     41.00 107.00   0.50    1.26    --  107.75 -94.00-180.00  132
 50  \w     40.00 107.00   0.50    1.26    --  107.75 -94.00 -60.00  134
 51  \w     51.00 127.00   0.50    1.26    --  107.75-138.00 -29.99  152
 52  \w     68.00 116.00   0.50    1.26    --  107.75-125.00  60.00   96
 53  \w     49.00 127.00   0.50    1.26    --  107.75-138.00 163.57  156
 54  \w     45.00 110.00   0.50    0.32    --   48.30-150.00 157.00  130
 55  \w     45.00 134.00   0.50    1.26    --  107.75-150.00 157.00  178
 56  \w     40.00  92.00   0.50    1.26    --  107.75 -94.00 -30.00  104
 57  \w     37.00  78.00   0.50    1.26    --  107.75 -94.00  60.00   82
 58  \w     36.00 106.00   0.50    1.26    --  107.75 -94.00 120.00  140
 59  \w     40.00 115.00   0.50    1.26    --  107.75-125.00 120.00  150
 60  \w     37.00  66.00   0.50    1.26    --  107.75 -77.00 -30.00   58
 61  \w     37.00 107.00   0.50    1.26    --  107.75 -94.00   0.00  140
 62  \w     29.00  93.00   0.50    0.32    --   48.30-122.00 -40.00  128
 63  \w     37.00 105.00   0.50    1.26    --  107.75 -94.00 150.00  136
 64  \w     27.00  54.00   0.50    0.32    --   48.30  77.00 150.00   54
 65  \w     27.00  55.00   0.50    0.32    --   48.30  77.00  90.00   56
 66  \w     27.00  69.00   0.50    0.32    --   48.30  77.00 120.00   84
 67  \w     27.00  53.00   0.50    0.32    --   48.30  77.00  60.00   52
 68  \w     27.00  53.00   0.50    0.32    --   48.30  77.00   0.00   52
 69  \w     27.00  57.00   0.50    0.32    --   48.30  77.00  30.00   60
 70  \w    -53.00 -27.00   0.50    0.32    --  -48.30 -77.00-180.00   52
 71  \w    -66.00 -28.00   0.50    0.32    --  -48.30 -77.00-120.00   76
 72  \w    -60.00 -34.00   0.50    0.32    --  -48.30 -57.00-180.00   52
 73  \w    -73.00 -27.00   0.50    0.32    --  -48.30 -77.00 -90.00   92
 74  \w    -69.00 -36.00   0.50    0.32    --  -48.30 -58.00 -15.66   66
 75  \w    -85.00 -34.00   0.50    0.32    --  -48.30 -57.00 -60.00  102
 76  \w    -88.00 -62.00   0.50    1.26    --  -86.25 -83.00-158.72   52
 77  \w    -88.00 -62.00   0.50    1.26    --  -86.25 -83.00 -97.28   52
 78  \w    -91.00 -66.00   0.50    1.26    --  -86.25 -73.00 -59.66   50
 79  \w    -93.00 -64.00   0.50    1.26    --  -86.25 -77.00 -30.00   58
 80  \w    -90.00 -64.00   0.50    1.26    --  -86.25 -77.00 -90.00   52
 81  \w    -88.00 -62.00   0.50    1.26    --  -86.25 -83.00 -70.54   52
 82  \w    -87.00 -62.00   0.50    1.26    --  -86.25 -83.00-112.06   50
 83  \w    -91.00 -65.00   0.50    1.26    --  -86.25 -76.00-156.81   52
 84  \w    -87.00 -62.00   0.50    1.26    --  -86.25 -83.00-128.64   50
 85  \w    -99.00 -39.00   0.50    0.32    --  -48.30 -38.00-150.00  120
 86  \w    -89.00 -64.00   0.50    1.26    --  -86.25 -77.00 -60.00   50
 87  \w    -87.00 -62.00   0.50    1.26    --  -86.25 -82.00  -3.05   50
 88  \w    -90.00 -64.00   0.50    1.26    --  -86.25 -77.00  60.00   52
 89  \w    -90.00 -64.00   0.50    1.26    --  -86.25 -77.00  90.00   52
 90  \w    -90.00 -64.00   0.50    1.26    --  -86.25 -83.00  89.08   52
 91  \w    -88.00 -63.00   0.50    1.26    --  -86.25 -81.00 113.97   50
 92  \w    -90.00 -64.00   0.50    1.26    --  -86.25 -77.00 150.00   52
 93  \w    -92.00 -66.00   0.50    1.26    --  -86.25 -72.00 119.21   52
 94  \w    -87.00 -62.00   0.50    1.26    --  -86.25 -83.00 169.80   50
 95  \w    -91.00 -65.00   0.50    1.26    --  -86.25 -75.00 137.34   52
 96  \w    -53.00 -28.00   0.50    0.32    --  -48.30 -77.00 150.00   50
 97  \w    -63.00 -34.00   0.50    0.32    --  -48.30 -57.00 120.00   58
 98  \w    -89.00 -63.00   0.50    1.26    --  -86.25 -80.00  49.31   52
 99  \w    -88.00 -62.00   0.50    1.26    --  -86.25 -83.00  25.89   52
100  \w    -93.00 -67.00   0.50    1.26    --  -86.25 -71.00  63.20   52
101  \w    -98.00 -64.00   0.50    1.26    --  -86.25 -77.00  30.00   68
102  \w    -97.00 -64.00   0.50    1.26    --  -86.25 -78.00   8.67   66
103  \w   -119.00 -72.00   0.50    0.32    --  -48.30-122.00 -40.00   94
104  \w    -89.00  -8.00   0.50    0.32    --  -48.30 122.00  40.00  162
105  \w    -89.00 -14.00   0.50    1.26    --  -86.25 122.00  40.00  150
106  \w   -108.00 -23.00   0.50    0.32    --  -48.30 150.00-157.00  170
107  \w   -108.00 -23.00   0.50    1.26    --  -86.25 150.00-157.00  170
108  \w   -121.00 -38.00   0.50    0.32    --  -48.30 -24.00  92.07  166
109  \w   -119.00 -35.00   0.50    0.32    --  -48.30 -57.00  60.00  168
110  \w   -119.00 -53.00   0.50    0.32    --  -48.30-150.00 157.00  132
111  \w   -158.00 -72.00   0.50    1.26    --  -86.25-122.00 -40.00  172
112  \w   -126.00 -66.00   0.50    1.26    --  -86.25 -74.00-147.73  120
113  \w   -107.00 -62.00   0.50    1.26    --  -86.25 -83.00-177.05   90
114  \w   -114.00 -88.00   0.50    0.32    --  -48.30 -77.00-180.00   52
115  \w   -149.00-123.00   0.50    1.26    --  -86.25 -77.00 -30.00   52
116  \w   -154.00 -53.00   0.50    1.26    --  -86.25-150.00 157.00  202
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0069339000
_diffrn_orient_matrix_UB_12      -0.0482866000
_diffrn_orient_matrix_UB_13      -0.0054370000
_diffrn_orient_matrix_UB_21      -0.1115002000
_diffrn_orient_matrix_UB_22      0.0000814000
_diffrn_orient_matrix_UB_23      -0.0425935000
_diffrn_orient_matrix_UB_31      0.0730013000
_diffrn_orient_matrix_UB_32      0.0046845000
_diffrn_orient_matrix_UB_33      -0.0553273000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0808
_diffrn_reflns_av_unetI/netI     0.0212
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            324842
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.115
_diffrn_reflns_theta_min         2.783
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.292
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.395
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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            'dark green'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.395
_exptl_crystal_description       plate
_exptl_crystal_F_000             3552
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene'
_exptl_crystal_size_max          0.359
_exptl_crystal_size_mid          0.344
_exptl_crystal_size_min          0.115
_refine_diff_density_max         0.688
_refine_diff_density_min         -0.692
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1083
_refine_ls_number_reflns         17195
_refine_ls_number_restraints     85
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0424
_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^)+(0.0646P)^2^+6.0308P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1157
_refine_ls_wR_factor_ref         0.1167
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16488
_reflns_number_total             17195
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc00914k2.cif
_cod_data_source_block           3pf6
_cod_database_code               1552222
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C42H52N4O2Co1P1F6
_chemical_oxdiff_usercomment
'Co-Me3tpa-dbsq-PF6-tol, dark green plate, recryst from toluene'
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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. Restrained distances
 P2A-F7A = P2A-F8A = P2A-F9A = P2A-F10A = P2A-F11A = P2A-F12A
 1.5823 with sigma of 0.001
 P2B-F7B = P2B-F8B = P2B-F9B = P2B-F10B = P2B-F11B = P2B-F12B
 1.5823 with sigma of 0.001
 F7A-F8A = F7A-F9A = F7A-F10A = F7A-F11A
 2.237372 with sigma of 0.001
 F7B-F8B = F7B-F9B = F7B-F10B = F7B-F11B
 2.237372 with sigma of 0.001
 F12A-F8A = F12A-F9A = F12A-F10A = F12A-F11A
 2.237372 with sigma of 0.001
 F12B-F8B = F12B-F9B = F12B-F10B = F12B-F11B
 2.237372 with sigma of 0.001
 F8A-F9A = F9A-F11A = F11A-F10A = F10A-F8A
 2.237372 with sigma of 0.001
 F8B-F9B = F9B-F11B = F11B-F10B = F10B-F8B
 2.237372 with sigma of 0.001
3. Restrained planarity
 F8B, F9B, F10B, F11B
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C12B \\sim C12C \\sim C13B \\sim C13C \\sim C14B \\sim C14C: within 2A with
sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(F11A) \\sim Ueq, Uanis(F11B) \\sim Ueq: with sigma of 0.004 and sigma for
terminal atoms of 0.008
Uanis(F7A) = Uanis(F7B)
Uanis(F8A) = Uanis(F8B)
Uanis(F9A) = Uanis(F9B)
Uanis(F10A) = Uanis(F10B)
Uanis(F11A) = Uanis(F11B)
Uanis(F12A) = Uanis(F12B)
Uanis(P2A) = Uanis(P2B)
5. Others
 Sof(C12C)=Sof(H12D)=Sof(H12E)=Sof(H12F)=Sof(C13C)=Sof(H13D)=Sof(H13E)=
 Sof(H13F)=Sof(C14C)=Sof(H14D)=Sof(H14E)=Sof(H14F)=1-FVAR(1)
 Sof(C12B)=Sof(H12A)=Sof(H12B)=Sof(H12C)=Sof(C13B)=Sof(H13A)=Sof(H13B)=
 Sof(H13C)=Sof(C14B)=Sof(H14A)=Sof(H14B)=Sof(H14C)=FVAR(1)
 Sof(P2B)=Sof(F7B)=Sof(F8B)=Sof(F9B)=Sof(F10B)=Sof(F11B)=Sof(F12B)=1-FVAR(2)
 Sof(P2A)=Sof(F7A)=Sof(F8A)=Sof(F9A)=Sof(F10A)=Sof(F11A)=Sof(F12A)=FVAR(2)
 1(DFIX)=1(DFIX)=FVAR(3)
 1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1.414*FVAR(4)
6.a Secondary CH2 refined with riding coordinates:
 C20A(H20C,H20D), C26A(H26C,H26D), C32A(H32C,H32D), C20B(H20A,H20B), C26B(H26A,
 H26B), C32B(H32A,H32B)
6.b Aromatic/amide H refined with riding coordinates:
 C4A(H4A), C6A(H6A), C16A(H16A), C17A(H17A), C18A(H18A), C22A(H22A),
 C23A(H23A), C24A(H24A), C28A(H28A), C29A(H29A), C30A(H30A), C4B(H4B), C6B(H6B),
  C16B(H16B), C17B(H17B), C18B(H18B), C22B(H22B), C23B(H23B), C24B(H24B),
 C28B(H28B), C29B(H29B), C30B(H30B), C1S(H1S), C2S(H2S), C3S(H3S), C4S(H4S),
 C5S(H5S), C8S(H8S), C9S(H9S), C10S(H10S), C11S(H11S), C12S(H12S)
6.c Idealised Me refined as rotating group:
 C8A(H8AA,H8AB,H8AC), C9A(H9AA,H9AB,H9AC), C10A(H10D,H10E,H10F), C12A(H12G,
 H12H,H12I), C13A(H13G,H13H,H13I), C14A(H14G,H14H,H14I), C33A(H33D,H33E,H33F),
 C34A(H34D,H34E,H34F), C35A(H35D,H35E,H35F), C8B(H8BA,H8BB,H8BC), C9B(H9BA,H9BB,
 H9BC), C10B(H10A,H10B,H10C), C12B(H12A,H12B,H12C), C12C(H12D,H12E,H12F),
 C13B(H13A,H13B,H13C), C13C(H13D,H13E,H13F), C14B(H14A,H14B,H14C), C14C(H14D,
 H14E,H14F), C33B(H33A,H33B,H33C), C34B(H34A,H34B,H34C), C35B(H35A,H35B,H35C),
 C7S(H7SA,H7SB,H7SC), C14S(H14J,H14K,H14L)
;
_shelx_res_checksum              95874
_olex2_exptl_crystal_mounting_method 'MiTeGen mount with cryoprotectant oil'
_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 2.381
_oxdiff_exptl_absorpt_empirical_full_min 0.493