Preparation of organocobalt(iii) complexes via O<sub>2</sub> activation.
Møller, Mads Sondrup; Kongsted, Jacob; McKenzie, Christine J.; Dalton transactions (Cambridge, England : 2003) 50 (2021) 4819–4829; doi:10.1039/d1dt00563d

data_7706905
_publ_section_title
;
 Preparation of organocobalt(iii) complexes via O<sub>2</sub> activation.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4819
_journal_page_last               4829
_journal_paper_doi               10.1039/d1dt00563d
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C18 H16 Co F3 N2 O3, 2(C2 H3 F3 O)'
_chemical_formula_sum            'C22 H22 Co F9 N2 O5'
_chemical_formula_weight         624.34
_chemical_name_systematic
'(N,N'-Ethylene-bis(salicylideneiminato))-(2,2,2-trifluoroethoxy)-cobalt(iii) 2,2,2-trifluoroethanol solvate'
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-06-17
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2020-11-20 deposited with the CCDC.	2021-03-15 downloaded from the CCDC.
;
_cell_angle_alpha                105.961(2)
_cell_angle_beta                 102.9240(10)
_cell_angle_gamma                109.030(2)
_cell_formula_units_Z            2
_cell_length_a                   9.3662(2)
_cell_length_b                   11.9220(3)
_cell_length_c                   13.0281(2)
_cell_measurement_reflns_used    18968
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      74.5480
_cell_measurement_theta_min      3.7520
_cell_volume                     1241.20(5)
_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 2018/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2923
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.982
_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     26.00 123.00   1.00    7.18    --   54.00  80.00   8.98   97
  2  \w     73.00 169.00   1.00    7.18    --  100.40  77.00  60.00   96
  3  \w    137.00 168.00   1.00    7.18    --  100.40  61.00   0.00   31
  4  \w     88.00 169.00   1.00    7.18    --  100.40  30.00 150.00   81
  5  \w     82.00 107.00   1.00    7.18    --  100.40 -94.00   0.00   25
  6  \w     56.00 112.00   1.00    7.18    --  100.40-125.00 -30.00   56
  7  \w     54.00 109.00   1.00    7.18    --  100.40-107.00  -6.53   55
  8  \w     79.00 105.00   1.00    7.18    --  100.40 -94.00 120.00   26
  9  \w     77.00 104.00   1.00    7.18    --  100.40 -94.00 150.00   27
 10  \w     36.00  73.00   1.00    7.18    --  100.40 -94.00 150.00   37
 11  \w     28.00  71.00   1.00    7.18    --  100.40 -94.00 120.00   43
 12  \w     28.00 105.00   1.00    7.18    --  100.40 -94.00  60.00   77
 13  \w     27.00  66.00   1.00    7.18    --  100.40   0.00 120.00   39
 14  \w     30.00 127.00   1.00    7.18    --   58.00  80.00 122.45   97
 15  \w     73.00 169.00   1.00    7.18    --  100.40  77.00  90.00   96
 16  \w     74.00 155.00   1.00    7.18    --  100.40  77.00 -90.00   81
 17  \w     81.00 159.00   1.00    7.18    --  100.40  61.00-120.00   78
 18  \w     76.00 149.00   1.00    7.18    --  100.40  77.00-180.00   73
 19  \w     73.00 169.00   1.00    7.18    --  100.40  77.00-150.00   96
 20  \w     78.00 124.00   1.00    7.18    --  100.40  61.00   0.00   46
 21  \w     73.00 156.00   1.00    7.18    --  100.40  77.00  30.00   83
 22  \w     74.00 168.00   1.00    7.18    --  100.40  77.00 150.00   94
 23  \w     73.00 166.00   1.00    7.18    --  100.40  77.00 -60.00   93
 24  \w     46.00 143.00   1.00    7.18    --   74.00  80.00 -31.54   97
 25  \w     38.00 135.00   1.00    7.18    --   66.00  80.00  49.58   97
 26  \w     43.00 139.00   1.00    7.18    --   70.00  76.00 -65.41   96
 27  \w     34.00 131.00   1.00    7.18    --   62.00  79.00  18.87   97
 28  \w     27.00 123.00   1.00    7.18    --   54.00  78.00 -81.52   96
 29  \w     17.00  43.00   1.00    1.80    --   46.00  82.00 102.26   26
 30  \w     34.00 131.00   1.00    7.18    --   62.00  80.00 162.93   97
 31  \w     15.00  43.00   1.00    1.80    --   46.00  87.00 -19.56   28
 32  \w      0.00  32.00   1.00    1.80    --   34.00  95.00  31.87   32
 33  \w    -49.00 -23.00   1.00    1.80    --   14.00 145.00 140.31   26
 34  \w    -77.00  75.00   1.00    1.80    --   -0.75   0.00  90.00  152
 35  \w     33.00  65.00   1.00    7.18    --  100.40 -61.00-150.00   32
 36  \w     31.00 127.00   1.00    7.18    --  100.40 -77.00-180.00   96
 37  \w     29.00  69.00   1.00    7.18    --  100.40 -94.00   0.00   40
 38  \w    -41.00  44.00   1.00    1.80    --   26.00 -46.00-165.73   85
 39  \w    -11.00  15.00   1.00    1.80    --   26.00 102.00-130.48   26
 40  \w     14.00  42.00   1.00    1.80    --   46.00  91.00-157.78   28
 41  \w    -87.00 -15.00   1.00    7.18    --  -82.50 125.00 -30.00   72
 42  \w   -135.00 -38.00   1.00    7.18    --  -66.00 -79.00  48.26   97
 43  \w   -135.00 -38.00   1.00    7.18    --  -66.00 -80.00-100.10   97
 44  \w   -143.00 -47.00   1.00    7.18    --  -74.00 -76.00-174.28   96
 45  \w   -143.00 -47.00   1.00    7.18    --  -74.00 -76.00-142.85   96
 46  \w   -151.00 -58.00   1.00    7.18    --  -82.50 -68.00  26.04   93
 47  \w   -147.00 -52.00   1.00    7.18    --  -78.00 -74.00 147.79   95
 48  \w   -147.00 -50.00   1.00    7.18    --  -78.00 -79.00 129.13   97
 49  \w   -151.00 -54.00   1.00    7.18    --  -82.00 -79.00 175.98   97
 50  \w   -152.00 -55.00   1.00    7.18    --  -82.50 -78.00  87.50   97
 51  \w   -151.00 -57.00   1.00    7.18    --  -82.50 -71.00 -60.29   94
 52  \w   -152.00 -55.00   1.00    7.18    --  -82.50 -78.00-151.47   97
 53  \w   -151.00 -55.00   1.00    7.18    --  -82.50 -77.00  60.00   96
 54  \w   -151.00 -56.00   1.00    7.18    --  -82.50 -76.00-106.35   95
 55  \w   -151.00 -57.00   1.00    7.18    --  -82.50 -70.00 -20.98   94
 56  \w   -152.00 -55.00   1.00    7.18    --  -82.50 -78.00 -37.43   97
 57  \w   -152.00 -54.00   1.00    7.18    --  -82.50 -80.00 106.22   98
 58  \w   -151.00 -56.00   1.00    7.18    --  -82.50 -74.00   8.04   95
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0277736000
_diffrn_orient_matrix_UB_12      -0.0124763000
_diffrn_orient_matrix_UB_13      0.1166815000
_diffrn_orient_matrix_UB_21      0.1804833000
_diffrn_orient_matrix_UB_22      0.0856634000
_diffrn_orient_matrix_UB_23      0.0366929000
_diffrn_orient_matrix_UB_31      -0.0317657000
_diffrn_orient_matrix_UB_32      0.1195707000
_diffrn_orient_matrix_UB_33      0.0469621000
_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  0.0596
_diffrn_reflns_av_unetI/netI     0.0326
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            44153
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.456
_diffrn_reflns_theta_min         3.759
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.404
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.512
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
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            'intense red'
_exptl_crystal_density_diffrn    1.671
_exptl_crystal_description       Lath
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.152
_exptl_crystal_size_mid          0.032
_exptl_crystal_size_min          0.022
_refine_diff_density_max         0.294
_refine_diff_density_min         -0.348
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     356
_refine_ls_number_reflns         4979
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0374
_refine_ls_R_factor_gt           0.0327
_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^)+(0.0470P)^2^+0.4028P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0826
_refine_ls_wR_factor_ref         0.0849
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4574
_reflns_number_total             4979
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00563d2.cif
_cod_data_source_block           mads_a_CCDC3
_cod_depositor_comments
'Adding full bibliography for 7706901--7706909.cif.'
_cod_database_code               7706905
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'C22 H20 N2 O5 Co F9'
_reflns_odcompleteness_completeness 99.98
_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 O(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C17(H17A,H17B), C19(H19A,H19B), C21(H21A,H21B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C10(H10), C12(H12), C13(H13),
 C14(H14), C15(H15)
2.c Idealised tetrahedral OH refined as rotating group with stretchable bonds:
 O4(H4A), O5(H5A)
;
_shelx_res_checksum              11895
_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 1.659
_oxdiff_exptl_absorpt_empirical_full_min 0.783