"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_7716382
_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         'F6 P, C H2 Cl2, C24 H30 N3'
_chemical_formula_sum            'C25 H32 Cl2 F6 N3 P'
_chemical_formula_weight         590.40
_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                 93.7140(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.45500(10)
_cell_length_b                   11.03070(10)
_cell_length_c                   17.1937(2)
_cell_measurement_reflns_used    17415
_cell_measurement_temperature    100.2(8)
_cell_measurement_theta_max      76.1870
_cell_measurement_theta_min      4.7370
_cell_volume                     2735.76(4)
_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      100.2(8)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.970
_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     32.00 121.00   0.50    0.05    --   46.78  38.00 150.00  178
  2  \w     32.00 121.00   0.50    0.05    --   46.78  38.00  90.00  178
  3  \w     32.00 121.00   0.50    0.05    --   46.78  38.00  60.00  178
  4  \w     32.00 121.00   0.50    0.05    --   46.78  38.00   0.00  178
  5  \w     32.00 121.00   0.50    0.05    --   46.78  38.00 -60.00  178
  6  \w     32.00 121.00   0.50    0.05    --   46.78  38.00-120.00  178
  7  \w     32.00 121.00   0.50    0.05    --   46.78  38.00-150.00  178
  8  \w     30.00  56.00   0.50    0.17    --  106.28 -15.00  30.00   52
  9  \w     34.00  61.00   0.50    0.17    --  106.28 -45.00  30.00   54
 10  \w    105.00 178.00   0.50    0.17    --  106.28  95.00 120.00  146
 11  \w     34.00  61.00   0.50    0.17    --  106.28 -45.00  60.00   54
 12  \w     34.00  61.00   0.50    0.17    --  106.28 -45.00   0.00   54
 13  \w     34.00  61.00   0.50    0.17    --  106.28 -45.00 -60.00   54
 14  \w     33.00  77.00   0.50    0.17    --  106.28 -61.00 -90.00   88
 15  \w     34.00  61.00   0.50    0.17    --  106.28 -45.00-180.00   54
 16  \w     33.00  99.00   0.50    0.17    --  106.28 -77.00-120.00  132
 17  \w     34.00  61.00   0.50    0.17    --  106.28 -45.00 150.00   54
 18  \w     30.00  56.00   0.50    0.17    --  106.28 -15.00 150.00   52
 19  \w     33.00 106.00   0.50    0.17    --  106.28 -95.00  30.00  146
 20  \w     33.00 106.00   0.50    0.17    --  106.28 -95.00  10.00  146
 21  \w     33.00 106.00   0.50    0.17    --  106.28 -95.00 120.00  146
 22  \w     34.00  94.00   0.50    0.05    --   46.78-125.00 120.00  120
 23  \w     -9.00  79.00   0.50    0.05    --   46.78 -95.00  10.00  176
 24  \w     33.00 106.00   0.50    0.17    --  106.28 -95.00-120.00  146
 25  \w     33.00 106.00   0.50    0.17    --  106.28 -95.00-180.00  146
 26  \w    -46.00 -19.00   0.50    0.17    --  -91.75  45.00 -60.00   54
 27  \w    -41.00 -15.00   0.50    0.17    --  -91.75  15.00 -60.00   52
 28  \w    -41.00 -15.00   0.50    0.17    --  -91.75  15.00 -30.00   52
 29  \w    -41.00 -15.00   0.50    0.17    --  -91.75  15.00   0.00   52
 30  \w   -164.00 -83.00   0.50    0.17    --  -91.75 -95.00  10.00  162
 31  \w   -164.00-107.00   0.50    0.17    --  -91.75 -95.00 -90.00  114
 32  \w   -164.00 -77.00   0.50    0.17    --  -91.75 -45.00  30.00  174
 33  \w   -164.00 -77.00   0.50    0.17    --  -91.75 -45.00 120.00  174
 34  \w    -79.00  26.00   0.50    0.05    --  -46.78  95.00 120.00  210
 35  \w    -80.00 -19.00   0.50    0.17    --  -91.75  95.00 120.00  122
 36  \w   -164.00 -77.00   0.50    0.17    --  -91.75 -45.00 150.00  174
 37  \w   -164.00 -77.00   0.50    0.17    --  -91.75 -45.00   0.00  174
 38  \w   -164.00 -77.00   0.50    0.17    --  -91.75 -45.00 -30.00  174
 39  \w   -164.00 -77.00   0.50    0.17    --  -91.75 -45.00 -90.00  174
 40  \w   -164.00 -77.00   0.50    0.17    --  -91.75 -45.00-150.00  174
 41  \w   -164.00 -77.00   0.50    0.17    --  -91.75 -45.00-180.00  174
 42  \w   -164.00-113.00   0.50    0.17    --  -91.75 -45.00-120.00  102
 43  \w   -166.00 -76.00   0.50    0.17    --  -91.75 -30.00-150.00  180
 44  \w   -166.00 -76.00   0.50    0.17    --  -91.75 -30.00 -90.00  180
 45  \w   -164.00 -77.00   0.50    0.17    --  -91.75 -45.00  60.00  174
 46  \w   -164.00 -77.00   0.50    0.17    --  -91.75 -45.00  90.00  174
 47  \w   -166.00 -76.00   0.50    0.17    --  -91.75 -30.00  60.00  180
;
_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      -0.0985392000
_diffrn_orient_matrix_UB_12      0.0538622000
_diffrn_orient_matrix_UB_13      -0.0075339000
_diffrn_orient_matrix_UB_21      0.0389216000
_diffrn_orient_matrix_UB_22      0.1183059000
_diffrn_orient_matrix_UB_23      -0.0325054000
_diffrn_orient_matrix_UB_31      -0.0138235000
_diffrn_orient_matrix_UB_32      -0.0508516000
_diffrn_orient_matrix_UB_33      -0.0833790000
_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  0.0885
_diffrn_reflns_av_unetI/netI     0.0393
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            60617
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.468
_diffrn_reflns_theta_min         4.766
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.236
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76403
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_description       needle
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.307
_refine_diff_density_min         -0.444
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     338
_refine_ls_number_reflns         5575
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0393
_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^)+(0.0431P)^2^+1.5983P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0966
_refine_ls_wR_factor_ref         0.1033
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4643
_reflns_number_total             5575
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01560f3.cif
_cod_data_source_block           240212ral_sk_193_100k
_cod_depositor_comments
'Adding full bibliography for 7716380--7716384.cif.'
_cod_database_code               7716382
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C23H31Cl2F6N3P
_chemical_oxdiff_usercomment     DCM/HEXANE
_shelx_estimated_absorpt_t_max   0.830
_shelx_estimated_absorpt_t_min   0.625
_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:
 C2(H2), C3(H3), C10(H10)
2.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C8(H8A,H8B), C25(H25A,H25B)
2.c Aromatic/amide H refined with riding coordinates:
 N1(H1), C18(H18), C20(H20), C24(H24), C22(H22), C17(H17), C14(H14), C21(H21),
 C23(H23), C15(H15), C16(H16)
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              42156
_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 1.442
_oxdiff_exptl_absorpt_empirical_full_min 0.717