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_7131538
_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         'C18 H38 Co F3 Li N2 Si4'
_chemical_formula_sum            'C18 H38 Co F3 Li N2 Si4'
_chemical_formula_weight         517.73
_space_group_crystal_system      orthorhombic
_space_group_IT_number           37
_space_group_name_Hall           'C 2 -2c'
_space_group_name_H-M_alt        'C c c 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-03-10
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.3832(2)
_cell_length_b                   18.7778(3)
_cell_length_c                   10.86351(14)
_cell_measurement_reflns_used    31139
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      33.2960
_cell_measurement_theta_min      2.6330
_cell_volume                     2730.08(7)
_computing_cell_refinement       'CrysAlisPro 1.171.42.84g (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.84g (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.84g (Rigaku OD, 2023)'
_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                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 100'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.956
_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    -78.00 -20.00   0.50    2.00    --  -13.50 137.00 -95.00  116
  2  \w    -75.00 -18.00   0.50    2.00    --  -13.50 133.00  86.00  114
  3  \w    -18.00  54.00   0.50    2.00    --   13.03 -99.00-120.00  144
  4  \w    -19.00  29.00   0.50    2.00    --  -13.50 -99.00-150.00   96
  5  \w    -19.00  29.00   0.50    2.00    --  -13.50 -99.00   0.00   96
  6  \w    -25.00  68.00   0.50    2.00    --  -13.50  19.00 120.00  186
  7  \w    -87.00 -42.00   0.50    2.00    --  -13.50-178.00 -90.00   90
  8  \w    -19.00  29.00   0.50    2.00    --  -13.50 -99.00-180.00   96
  9  \w    -89.00 -40.00   0.50    2.00    --  -13.50 178.00-150.00   98
 10  \w    -87.00 -42.00   0.50    2.00    --  -13.50-178.00  30.00   90
 11  \w    -25.00  68.00   0.50    2.00    --  -13.50  19.00-150.00  186
 12  \w     -7.00  94.00   0.50    2.00    --   13.03  38.00-180.00  202
 13  \w    -64.00  -8.00   0.50    2.00    --   13.03 -57.00  30.00  112
 14  \w    -19.00  29.00   0.50    2.00    --  -13.50 -99.00 -90.00   96
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix-Arc 100'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0409976000
_diffrn_orient_matrix_UB_12      0.0229135000
_diffrn_orient_matrix_UB_13      -0.0119427000
_diffrn_orient_matrix_UB_21      -0.0311797000
_diffrn_orient_matrix_UB_22      0.0300241000
_diffrn_orient_matrix_UB_23      0.0097396000
_diffrn_orient_matrix_UB_31      0.0125166000
_diffrn_orient_matrix_UB_32      -0.0003161000
_diffrn_orient_matrix_UB_33      0.0634446000
_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  0.0312
_diffrn_reflns_av_unetI/netI     0.0198
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            42315
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.923
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.667
_diffrn_reflns_theta_min         2.169
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Mova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.832
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93679
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.84g (Rigaku Oxford Diffraction, 2023)
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    1.260
_exptl_crystal_description       block
_exptl_crystal_F_000             1092
_exptl_crystal_size_max          0.162
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.076
_refine_diff_density_max         0.356
_refine_diff_density_min         -0.179
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.242(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     141
_refine_ls_number_reflns         5011
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_gt           0.0272
_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^)+(0.0422P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0636
_refine_ls_wR_factor_ref         0.0655
_reflns_Friedel_coverage         0.846
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.887
_reflns_number_gt                4411
_reflns_number_total             5011
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by -169.1362\% 
around [0.22 0.97 -0.01] (reciprocal) or [0.41 0.91 -0.02] (direct)
;
_cod_data_source_file            d3cc01216f2.cif
_cod_data_source_block           23eh059_al639
_cod_depositor_comments
'Adding full bibliography for 7131535--7131539.cif.'
_cod_original_cell_volume        2730.06(7)
_cod_database_code               7131538
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C72  Co4  F12  Li4  N8  Si16  H1  '
_shelx_estimated_absorpt_t_max   0.939
_shelx_estimated_absorpt_t_min   0.877
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.758(11)
 0.242(11)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C9(H9)
3.b Idealised Me refined as rotating group:
 C5(H5a,H5b,H5c), C3(H3a,H3b,H3c), C2(H2a,H2b,H2c), C4(H4a,H4b,H4c), C6(H6a,
 H6b,H6c), C1(H1a,H1b,H1c)
;
_shelx_res_checksum              85948
_shelx_hkl_checksum              45206
_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 1.092
_oxdiff_exptl_absorpt_empirical_full_min 0.914
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2