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_7131537
_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_absolute_configuration unk
_chemical_formula_moiety         'C36 H91 Co2 N5 Si10'
_chemical_formula_sum            'C36 H91 Co2 N5 Si10'
_chemical_formula_weight         992.89
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-05-31T23:15:55-00:00
_audit_update_record
;
2023-03-10 deposited with the CCDC.	2023-04-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.7961(6)
_cell_angle_gamma                90
_cell_formula_units_Z            6
_cell_length_a                   9.10611(6)
_cell_length_b                   29.0863(2)
_cell_length_c                   32.9649(2)
_cell_measurement_reflns_used    86504
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      79.444
_cell_measurement_theta_min      2.682
_cell_volume                     8686.55(10)
_computing_cell_refinement       'CrysAlisPro 1.171.41.117a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.117a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.117a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 0.998
_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    -82.00 -23.00   0.50    1.20    --  -23.00 145.00   7.00  118
  2  \w    -71.00 -13.00   0.50    1.20    --  -23.00 126.00-160.00  116
  3  \w    -20.00   6.00   0.50    1.20    --  -23.00 -91.00 -74.99   52
  4  \w    -95.00   0.00   0.50    1.20    --  -23.00 -77.00 120.00  190
  5  \w    -95.00 -10.00   0.50    1.20    --  -23.00 -45.00 150.00  170
  6  \w    -95.00  -6.00   0.50    1.20    --  -23.00 -61.00 -90.00  178
  7  \w    -70.00 -12.00   0.50    1.20    --  -23.00 125.00-120.00  116
  8  \w    -70.00 -12.00   0.50    1.20    --  -23.00 125.00  90.00  116
  9  \w    -26.00  23.00   0.50    1.20    --   47.92 -19.00-120.00   98
 10  \w    -26.00  23.00   0.50    1.20    --   47.92 -19.00 -30.00   98
 11  \w    -26.00  23.00   0.50    1.20    --   47.92 -19.00  30.00   98
 12  \w    -26.00  23.00   0.50    1.20    --   47.92 -19.00 150.00   98
 13  \w    -23.00  63.00   0.50    1.20    --   47.92 -57.00-120.00  172
 14  \w    -25.00  40.00   0.50    1.20    --   47.92 -38.00 150.00  130
 15  \w     42.00 106.00   0.50    7.00    --  113.25 -94.00  60.00  128
 16  \w     42.00 106.00   0.50    7.00    --  113.25 -94.00 -60.00  128
 17  \w     42.00  68.00   0.50    7.00    --  113.25 -61.00  60.00   52
 18  \w     42.00 106.00   0.50    7.00    --  113.25 -94.00-180.00  128
 19  \w    101.00 177.00   0.50    7.00    --  113.25  42.00  39.36  152
 20  \w     42.00  68.00   0.50    7.00    --  113.25 -61.00 -60.00   52
 21  \w     42.00 106.00   0.50    7.00    --  113.25 -94.00-120.00  128
 22  \w     42.00 106.00   0.50    7.00    --  113.25 -97.00-149.26  128
 23  \w     96.00 177.00   0.50    7.00    --  113.25  63.00 -94.40  162
 24  \w     42.00  68.00   0.50    7.00    --  113.25 -61.00-150.00   52
 25  \w     97.00 177.00   0.50    7.00    --  113.25  61.00-150.00  160
 26  \w     97.00 177.00   0.50    7.00    --  113.25  61.00   0.00  160
 27  \w     42.00 106.00   0.50    7.00    --  113.25 -94.00 120.00  128
 28  \w     42.00 106.00   0.50    7.00    --  113.25 -94.00  30.00  128
 29  \w     42.00 106.00   0.50    7.00    --  113.25 -94.00 150.00  128
 30  \w     42.00  68.00   0.50    7.00    --  113.25 -61.00-180.00   52
 31  \w     42.00 106.00   0.50    7.00    --  113.25 -94.00   0.00  128
 32  \w     42.00 102.00   0.50    7.00    --  113.25 -77.00 150.00  120
 33  \w     42.00  68.00   0.50    7.00    --  113.25 -61.00  30.00   52
 34  \w     42.00 106.00   0.50    7.00    --  113.25 -94.00 -30.00  128
 35  \w    106.00 177.00   0.50    7.00    --  113.25  98.00 -45.53  142
 36  \w    101.00 177.00   0.50    7.00    --  113.25  45.00 150.00  152
 37  \w     42.00  68.00   0.50    7.00    --  113.25 -61.00 -30.00   52
 38  \w    101.00 177.00   0.50    7.00    --  113.25  45.00  60.00  152
 39  \w     42.00 102.00   0.50    7.00    --  113.25 -77.00  60.00  120
 40  \w    101.00 177.00   0.50    7.00    --  113.25  30.00 120.00  152
 41  \w     42.00 106.00   0.50    7.00    --  113.25 -94.00  90.00  128
 42  \w     42.00  68.00   0.50    7.00    --  113.25 -61.00 -90.00   52
 43  \w     42.00 106.00   0.50    7.00    --  113.25 -94.00 -90.00  128
 44  \w    101.00 177.00   0.50    7.00    --  113.25  45.00 -30.00  152
 45  \w     42.00  68.00   0.50    7.00    --  113.25 -61.00 120.00   52
 46  \w    101.00 177.00   0.50    7.00    --  113.25  45.00   0.00  152
 47  \w    100.00 177.00   0.50    7.00    --  113.25  15.00-150.00  154
 48  \w     42.00 102.00   0.50    7.00    --  113.25 -77.00-120.00  120
 49  \w     42.00  68.00   0.50    7.00    --  113.25 -61.00  90.00   52
 50  \w     25.00 121.00   0.50    1.20    --   47.92  77.00-120.00  192
 51  \w     25.00 121.00   0.50    1.20    --   47.92  77.00 120.00  192
 52  \w     25.00  82.00   0.50    1.20    --   47.92  77.00 -60.00  114
 53  \w     25.00 121.00   0.50    1.20    --   47.92  77.00   0.00  192
;
_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      -0.0358453
_diffrn_orient_matrix_UB_12      -0.0499796
_diffrn_orient_matrix_UB_13      -0.0129376
_diffrn_orient_matrix_UB_21      -0.0766902
_diffrn_orient_matrix_UB_22      0.0172531
_diffrn_orient_matrix_UB_23      -0.0409721
_diffrn_orient_matrix_UB_31      0.1474771
_diffrn_orient_matrix_UB_32      -0.003176
_diffrn_orient_matrix_UB_33      -0.0189783
_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  0.0802
_diffrn_reflns_av_unetI/netI     0.0744
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            176467
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.504
_diffrn_reflns_theta_min         2.695
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.677
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.57662
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlisPro 1.171.41.117a (Rigaku Oxford Diffraction, 2021)
        Empirical absorption correction using spherical harmonics,
        implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.139
_exptl_crystal_description       block
_exptl_crystal_F_000             3216
_exptl_crystal_size_max          0.276
_exptl_crystal_size_mid          0.201
_exptl_crystal_size_min          0.157
_refine_diff_density_max         1.66
_refine_diff_density_min         -0.687
_refine_diff_density_rms         0.103
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.463(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1453
_refine_ls_number_reflns         35452
_refine_ls_number_restraints     71
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0767
_refine_ls_R_factor_gt           0.0722
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1324P)^2^+8.6164P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1989
_refine_ls_wR_factor_ref         0.2051
_reflns_Friedel_coverage         0.958
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                32636
_reflns_number_total             35452
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc01216f2.cif
_cod_data_source_block           22EH069_AL453
_cod_depositor_comments
'Adding full bibliography for 7131535--7131539.cif.'
_cod_original_cell_volume        8686.54(11)
_cod_database_code               7131537
_shelx_estimated_absorpt_t_min   0.256
_shelx_estimated_absorpt_t_max   0.415
_oxdiff_exptl_absorpt_empirical_details
;
        Empirical correction (ABSPACK) includes:
        - Absorption correction using spherical harmonics
        - Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.562
_oxdiff_exptl_absorpt_empirical_full_min 0.696
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
        1. Twinned data refinement
 Scales: 0.537(4)
 0.463(4)
        2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
        3. Rigid bond restraints
 C64, C63, Si21, C62, N11
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
        4. Uiso/Uaniso restraints and constraints
Uanis(C64) \\sim Ueq, Uanis(C56) \\sim Ueq, Uanis(C69) \\sim Ueq, Uanis(C62)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C53) \\sim Ueq, Uanis(C68) \\sim Ueq, Uanis(C70) \\sim Ueq, Uanis(C11)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C63) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(Co6A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
        5. Others
 Sof(Co5A)=1-FVAR(1)
 Sof(Co5)=FVAR(1)
 Sof(Co6A)=1-FVAR(2)
 Sof(Co6)=FVAR(2)
        6.a Me refined with riding coordinates:
 C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C24(H24A,H24B,H24C), C73(H73A,H73B,
 H73C), C55(H55A,H55B,H55C), C40(H40A,H40B,H40C), C50(H50A,H50B,H50C), C30(H30A,
 H30B,H30C), C41(H41A,H41B,H41C), C25(H25A,H25B,H25C), C28(H28A,H28B,H28C),
 C18(H18A,H18B,H18C), C80(H80A,H80B,H80C), C51(H51A,H51B,H51C), C36(H36A,H36B,
 H36C), C42(H42A,H42B,H42C), C37(H37A,H37B,H37C), C61(H61A,H61B,H61C), C60(H60A,
 H60B,H60C), C85(H85A,H85B,H85C), C49(H49A,H49B,H49C), C3(H3A,H3B,H3C),
 C79(H79A,H79B,H79C), C58(H58A,H58B,H58C), C87(H87A,H87B,H87C), C12(H12A,H12B,
 H12C), C39(H39A,H39B,H39C), C8(H8A,H8B,H8C), C29(H29A,H29B,H29C), C89(H89A,
 H89B,H89C), C91(H91A,H91B,H91C), C13(H13A,H13B,H13C), C7(H7A,H7B,H7C),
 C52(H52A,H52B,H52C), C33(H33A,H33B,H33C), C43(H43A,H43B,H43C), C35(H35A,H35B,
 H35C), C16(H16A,H16B,H16C), C23(H23A,H23B,H23C), C1(H1A,H1B,H1C), C90(H90A,
 H90B,H90C), C5(H5A,H5B,H5C), C59(H59A,H59B,H59C), C22(H22A,H22B,H22C),
 C44(H44A,H44B,H44C), C46(H46A,H46B,H46C), C71(H71A,H71B,H71C), C54(H54A,H54B,
 H54C), C10(H10A,H10B,H10C), C21(H21A,H21B,H21C), C81(H81A,H81B,H81C), C47(H47A,
 H47B,H47C), C82(H82A,H82B,H82C), C86(H86A,H86B,H86C), C45(H45A,H45B,H45C),
 C57(H57A,H57B,H57C), C48(H48A,H48B,H48C), C31(H31A,H31B,H31C), C83(H83A,H83B,
 H83C), C2(H2A,H2B,H2C), C88(H88A,H88B,H88C), C72(H72A,H72B,H72C), C20(H20A,
 H20B,H20C), C17(H17A,H17B,H17C), C76(H76A,H76B,H76C), C15(H15A,H15B,H15C),
 C32(H32A,H32B,H32C), C53(H53A,H53B,H53C), C6(H6A,H6B,H6C), C9(H9A,H9B,H9C),
 C75(H75A,H75B,H75C), C14(H14A,H14B,H14C), C67(H67A,H67B,H67C), C56(H56A,H56B,
 H56C), C65(H65A,H65B,H65C), C84(H84A,H84B,H84C), C4(H4A,H4B,H4C), C66(H66A,
 H66B,H66C), C69(H69A,H69B,H69C), C78(H78A,H78B,H78C), C62(H62A,H62B,H62C),
 C77(H77A,H77B,H77C), C34(H34A,H34B,H34C), C11(H11A,H11B,H11C), C19(H19A,H19B,
 H19C), C74(H74A,H74B,H74C), C68(H68A,H68B,H68C), C70(H70A,H70B,H70C), C63(H63A,
 H63B,H63C), C64(H64A,H64B,H64C)
        6.b Aromatic/amide H refined with riding coordinates:
 C01Q(H01Q), C01T(H01T), C01U(H01U)
;
_shelx_res_checksum              3719
_shelx_hkl_checksum              58224