Applying Na/Co(II) bimetallic partnerships to promote multiple Co-H exchanges in polyfluoroarenes.
Logallo, Alessandra; Hevia, Eva; Chemical communications (Cambridge, England) 59 (2023) 5383–5386; doi:10.1039/d3cc01216f

data_7131535
_publ_section_title
;
 Applying Na/Co(II) bimetallic partnerships to promote multiple Co-H
 exchanges in polyfluoroarenes.
;
_journal_issue                   36
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              5383
_journal_page_last               5386
_journal_paper_doi               10.1039/d3cc01216f
_journal_volume                  59
_journal_year                    2023
_chemical_formula_moiety         'C26 H55 Co F2 N2 Na O2 Si4'
_chemical_formula_sum            'C26 H55 Co F2 N2 Na O2 Si4'
_chemical_formula_weight         660.00
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-03-09
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-03-10 deposited with the CCDC.	2023-04-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.3623(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.5676(2)
_cell_length_b                   11.28947(11)
_cell_length_c                   20.1652(3)
_cell_measurement_reflns_used    30414
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      28.8230
_cell_measurement_theta_min      1.9360
_cell_volume                     3698.58(9)
_computing_cell_refinement       'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_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      173.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0965
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -44.00  42.00   1.00    5.00    --    0.31  77.00-150.00   86
  2  \w    -96.00 -39.00   1.00    5.00    --    0.31-178.00-150.00   57
  3  \w    -96.00 -37.00   1.00    5.00    --    0.31 178.00-150.00   59
  4  \w    -42.00   9.00   1.00   60.00    --  -35.55 -77.00  90.00   51
  5  \w    -42.00   9.00   1.00   60.00    --  -35.55 -77.00 150.00   51
  6  \w   -112.00   3.00   1.00   60.00    --  -35.55 -57.00-120.00  115
  7  \w   -104.00  -2.00   1.00   60.00    --  -35.55 121.00-121.00  102
  8  \w    -80.00  42.00   1.00   60.00    --  -35.55  77.00-180.00  122
  9  \w    -42.00   9.00   1.00   60.00    --  -35.55 -77.00   0.00   51
 10  \w     -2.00 113.00   1.00   60.00    --   36.17  57.00  30.00  115
 11  \w     -8.00  42.00   1.00   60.00    --   36.17  77.00  90.00   50
 12  \w     -8.00  42.00   1.00   60.00    --   36.17  77.00-120.00   50
 13  \w    -35.00  -7.00   1.00   60.00    --   36.17 126.00-130.04   28
 14  \w    -15.00  92.00   1.00   60.00    --   36.17 -99.00  30.00  107
 15  \w    -76.00  39.00   1.00    5.00    --    0.31 -57.00  60.00  115
 16  \w    -42.00  45.00   1.00    5.00    --    0.31 -77.00 -90.00   87
 17  \w   -124.00  51.00   1.00   60.00    --  -35.55 -19.00  60.00  175
 18  \w    -74.00  41.00   1.00   60.00    --  -35.55  57.00 -30.00  115
 19  \w    -95.00  48.00   1.00   60.00    --  -35.55  38.00 150.00  143
 20  \w    -34.00  -6.00   1.00   60.00    --   36.17 125.00 -34.93   28
 21  \w    -23.00 119.00   1.00   60.00    --   36.17  38.00 -30.00  142
 22  \w    -15.00  10.00   1.00   60.00    --   36.17 -99.00-120.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0106655000
_diffrn_orient_matrix_UB_12      -0.0176216000
_diffrn_orient_matrix_UB_13      0.0361941000
_diffrn_orient_matrix_UB_21      0.0324391000
_diffrn_orient_matrix_UB_22      0.0420344000
_diffrn_orient_matrix_UB_23      0.0109829000
_diffrn_orient_matrix_UB_31      -0.0271982000
_diffrn_orient_matrix_UB_32      0.0432388000
_diffrn_orient_matrix_UB_33      0.0040579000
_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  0.0505
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            110235
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.751
_diffrn_reflns_theta_min         1.951
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.639
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.562
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.73a (Rigaku Oxford Diffraction, 2022)
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            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.185
_exptl_crystal_description       plate
_exptl_crystal_F_000             1412
_exptl_crystal_size_max          0.459
_exptl_crystal_size_mid          0.233
_exptl_crystal_size_min          0.063
_refine_diff_density_max         0.292
_refine_diff_density_min         -0.275
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     512
_refine_ls_number_reflns         11548
_refine_ls_number_restraints     52
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.0402
_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^)+(0.0441P)^2^+1.1427P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0973
_refine_ls_wR_factor_ref         0.1078
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8471
_reflns_number_total             11548
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc01216f2.cif
_cod_data_source_block           22eh144_al579
_cod_depositor_comments
'Adding full bibliography for 7131535--7131539.cif.'
_cod_original_cell_volume        3698.58(8)
_cod_database_code               7131535
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C104  H220  Co4  F8  N8  Na4  O8  Si16  '
_shelx_estimated_absorpt_t_max   0.961
_shelx_estimated_absorpt_t_min   0.758
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N1A-Co1 \\sim N1-Co1
 with sigma of 0.002
 Si3-C8A \\sim Si3-C8 \\sim Si3-C7A \\sim Si3-C7 \\sim Si3-C9A \\sim Si3-C9
 with sigma of 0.002
3. Uiso/Uaniso restraints and constraints
Uanis(C22) \\sim Ueq, Uanis(C21) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C8) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C5A) \\sim Ueq, Uanis(C6A) \\sim Ueq, Uanis(C4A) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(C6A)=Sof(H6AA)=Sof(H6AB)=Sof(H6AC)=Sof(C5A)=Sof(H5AA)=Sof(H5AB)=Sof(H5AC)=
 Sof(Si2A)=Sof(C4A)=Sof(H4AA)=Sof(H4AB)=Sof(H4AC)=Sof(N1A)=Sof(Si1A)=Sof(C1A)=
 Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(H2AC)=Sof(C3A)=
 Sof(H3AA)=Sof(H3AB)=Sof(H3AC)=1-FVAR(1)
 Sof(Si1)=Sof(Si2)=Sof(N1)=Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=Sof(C6)=Sof(H6A)=
 Sof(H6B)=Sof(H6C)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(H5C)=Sof(C2)=Sof(H2A)=Sof(H2B)=
 Sof(H2C)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(H4C)=
 FVAR(1)
 Sof(C20A)=Sof(H20C)=Sof(H20D)=Sof(C21A)=Sof(H21C)=Sof(H21D)=Sof(C22A)=
 Sof(H22C)=Sof(H22D)=Sof(C19A)=Sof(H19C)=Sof(H19D)=1-FVAR(2)
 Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(C20)=Sof(H20A)=
 Sof(H20B)=Sof(C22)=Sof(H22A)=Sof(H22B)=FVAR(2)
 Sof(H25C)=Sof(H25D)=Sof(C26A)=Sof(H26C)=Sof(H26D)=1-FVAR(3)
 Sof(H25A)=Sof(H25B)=Sof(C26)=Sof(H26A)=Sof(H26B)=FVAR(3)
 Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(H8AC)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=
 Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(H7AC)=1-FVAR(4)
 Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(H7C)=Sof(C8)=
 Sof(H8C)=Sof(H8A)=Sof(H8B)=FVAR(4)
5.a Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C25(H25A,H25B), C25(H25C,H25D), C23(H23A,H23B), C24(H24A,
 H24B), C21(H21A,H21B), C20(H20A,H20B), C22(H22A,H22B), C26(H26A,H26B),
 C20A(H20C,H20D), C21A(H21C,H21D), C22A(H22C,H22D), C19A(H19C,H19D), C26A(H26C,
 H26D)
5.b Me refined with riding coordinates:
 C10(H10A,H10B,H10C), C9(H9A,H9B,H9C), C7(H7A,H7B,H7C), C8(H8C,H8A,H8B),
 C2A(H2AA,H2AB,H2AC), C3A(H3AA,H3AB,H3AC), C8A(H8AA,H8AB,H8AC), C9A(H9AA,H9AB,
 H9AC), C7A(H7AA,H7AB,H7AC)
5.c Aromatic/amide H refined with riding coordinates:
 C18(H18), C16(H16), C15(H15)
5.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C1(H1A,H1B,H1C), C6(H6A,H6B,H6C),
 C5(H5A,H5B,H5C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C6A(H6AA,
 H6AB,H6AC), C5A(H5AA,H5AB,H5AC), C4A(H4AA,H4AB,H4AC), C1A(H1AA,H1AB,H1AC)
;
_shelx_res_checksum              80983
_shelx_hkl_checksum              87889
_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 1.339
_oxdiff_exptl_absorpt_empirical_full_min 0.807