"Catch and release" of the Cp<sup>N3</sup> ligand using cobalt: dissociation, protonation, and C-H bond thermochemistry.
Luhach, Sanju; Lalancette, Roger A.; Prokopchuk, Demyan E.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 18865–18872; doi:10.1039/d4dt01560f

data_7716384
_publ_section_title
;
 "Catch and release" of the Cp<sup>N3</sup> ligand using cobalt:
 dissociation, protonation, and C-H bond thermochemistry.
;
_journal_issue                   47
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              18865
_journal_page_last               18872
_journal_paper_doi               10.1039/d4dt01560f
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'B C24 F20, C24 H28 N3'
_chemical_formula_sum            'C48 H28 B F20 N3 O'
_chemical_formula_weight         1053.54
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-02-16
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-05-27 deposited with the CCDC.	2024-06-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.734(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.0766(2)
_cell_length_b                   32.5576(6)
_cell_length_c                   16.0099(4)
_cell_measurement_reflns_used    14671
_cell_measurement_temperature    100.0(7)
_cell_measurement_theta_max      76.1350
_cell_measurement_theta_min      2.7000
_cell_volume                     4595.85(18)
_computing_cell_refinement       'CrysAlisPro 1.171.43.105a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.105a (release 11-01-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.105a (Rigaku OD, 2024)'
_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      100.0(7)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.931
_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     33.00 106.00   0.50    0.33    --  106.28 -95.00 120.00  146
  2  \w     36.00 108.00   0.50    0.33    --  106.28-106.00  88.00  144
  3  \w     19.00  83.00   0.50    0.08    --   46.78-106.00  88.00  128
  4  \w     34.00  61.00   0.50    0.33    --  106.28 -45.00 120.00   54
  5  \w     33.00  77.00   0.50    0.33    --  106.28 -61.00 -30.00   88
  6  \w     34.00  61.00   0.50    0.33    --  106.28 -45.00 -90.00   54
  7  \w     34.00  61.00   0.50    0.33    --  106.28 -45.00-120.00   54
  8  \w     34.00  61.00   0.50    0.33    --  106.28 -45.00-150.00   54
  9  \w     30.00  56.00   0.50    0.33    --  106.28 -15.00-150.00   52
 10  \w    105.00 176.00   0.50    0.33    --  106.28 106.00-173.00  142
 11  \w    -37.00  29.00   0.50    0.08    --  -46.78  19.00 -90.00  132
 12  \w    -41.00 -15.00   0.50    0.33    --  -91.75  15.00-150.00   52
 13  \w    -41.00 -15.00   0.50    0.33    --  -91.75  15.00-180.00   52
 14  \w    -41.00 -15.00   0.50    0.33    --  -91.75  15.00-120.00   52
 15  \w    -41.00 -15.00   0.50    0.33    --  -91.75  15.00  30.00   52
 16  \w    -41.00 -15.00   0.50    0.33    --  -91.75  15.00 150.00   52
 17  \w    -41.00 -15.00   0.50    0.33    --  -91.75  15.00  60.00   52
 18  \w   -120.00 -32.00   0.50    0.08    --  -46.78 -38.00-120.00  176
 19  \w   -120.00 -32.00   0.50    0.08    --  -46.78 -38.00 -60.00  176
 20  \w    -82.00 -22.00   0.50    0.33    --  -91.75 106.00-173.00  120
 21  \w    -82.00   2.00   0.50    0.08    --  -46.78 106.00-173.00  168
 22  \w   -120.00 -32.00   0.50    0.08    --  -46.78 -38.00-180.00  176
 23  \w   -120.00 -32.00   0.50    0.08    --  -46.78 -38.00 -30.00  176
 24  \w   -120.00 -32.00   0.50    0.08    --  -46.78 -38.00  30.00  176
 25  \w   -120.00 -32.00   0.50    0.08    --  -46.78 -38.00  90.00  176
 26  \w   -120.00 -54.00   0.50    0.08    --  -46.78 -38.00 120.00  132
 27  \w   -162.00 -83.00   0.50    0.33    --  -91.75-106.00  88.00  158
 28  \w   -164.00 -77.00   0.50    0.33    --  -91.75 -45.00 150.00  174
 29  \w   -167.00 -74.00   0.50    0.33    --  -91.75 -15.00-120.00  186
;
_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      0.0918490000
_diffrn_orient_matrix_UB_12      0.0337379000
_diffrn_orient_matrix_UB_13      0.0570123000
_diffrn_orient_matrix_UB_21      0.1284033000
_diffrn_orient_matrix_UB_22      -0.0310183000
_diffrn_orient_matrix_UB_23      0.0341187000
_diffrn_orient_matrix_UB_31      0.0749304000
_diffrn_orient_matrix_UB_32      0.0117825000
_diffrn_orient_matrix_UB_33      -0.0734670000
_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  0.0896
_diffrn_reflns_av_unetI/netI     0.0595
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.931
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            51110
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.931
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.428
_diffrn_reflns_theta_min         2.714
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.319
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58901
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.105a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_description       needle
_exptl_crystal_F_000             2120
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.327
_refine_diff_density_min         -0.285
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     653
_refine_ls_number_reflns         8988
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0721
_refine_ls_R_factor_gt           0.0479
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0549P)^2^+1.2355P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1138
_refine_ls_wR_factor_ref         0.1262
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6437
_reflns_number_total             8988
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01560f3.cif
_cod_data_source_block           240125_ral_sk_147_149_100k_sq
_cod_depositor_comments
'Adding full bibliography for 7716380--7716384.cif.'
_cod_database_code               7716384
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C48H28BF20N3
_chemical_oxdiff_usercomment     'DIETHYL ETHER'
_shelx_estimated_absorpt_t_max   0.913
_shelx_estimated_absorpt_t_min   0.725
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C10(H10)
2.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C8(H8A,H8B)
2.c Aromatic/amide H refined with riding coordinates:
 N1(H1), C20(H20), C14(H14), C18(H18), C15(H15), C21(H21), C24(H24), C22(H22),
 C16(H16), C17(H17), C23(H23)
2.d Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C12(H12A,H12B,H12C), C11(H11A,H11B,H11C)
;
_shelx_res_checksum              67010
_shelx_fab_checksum              75880
_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 1.451
_oxdiff_exptl_absorpt_empirical_full_min 0.641