"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_7716380
_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         'C26 H28 Co N3 O2'
_chemical_formula_sum            'C26 H28 Co N3 O2'
_chemical_formula_weight         473.44
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-06-09
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-05-27 deposited with the CCDC.	2024-06-18 downloaded from the CCDC.
;
_cell_angle_alpha                92.141(2)
_cell_angle_beta                 96.367(2)
_cell_angle_gamma                104.230(2)
_cell_formula_units_Z            4
_cell_length_a                   11.4083(3)
_cell_length_b                   11.9826(2)
_cell_length_c                   17.9543(3)
_cell_measurement_reflns_used    20243
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      70.8470
_cell_measurement_theta_min      3.8070
_cell_volume                     2359.06(9)
_computing_cell_refinement       'CrysAlisPro 1.171.42.58a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.58a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.58a (Rigaku OD, 2022)'
_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      100.00(10)
_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 0.977
_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   -101.00 -46.00   0.50    0.05    --    0.00 178.00 150.00  110
  2  \w   -101.00 -46.00   0.50    0.05    --    0.00 178.00  90.00  110
  3  \w   -101.00 -46.00   0.50    0.05    --    0.00 178.00-120.00  110
  4  \w    -57.00  31.00   0.50    0.05    --    0.00  95.00 -57.00  176
  5  \w      0.00 138.00   0.50    0.16    --   55.97  45.00   0.00  276
  6  \w     91.00 138.00   0.50    0.16    --   55.97  61.00  30.00   94
  7  \w    100.00 138.00   0.50    0.16    --   55.97  77.00  60.00   76
  8  \w     13.00 138.00   0.50    0.16    --   55.97  56.00  65.92  250
  9  \w    -48.00  25.00   0.50    0.05    --    0.00  77.00  90.00  146
 10  \w     13.00 138.00   0.50    0.16    --   55.97  56.00 147.70  250
 11  \w    100.00 138.00   0.50    0.16    --   55.97  77.00 -90.00   76
 12  \w    100.00 138.00   0.50    0.16    --   55.97  77.00-150.00   76
 13  \w     91.00 138.00   0.50    0.16    --   55.97  61.00-180.00   94
 14  \w     11.00 138.00   0.50    0.16    --   55.97  53.00-156.58  254
 15  \w     13.00 138.00   0.50    0.16    --   55.97  56.00 -92.98  250
 16  \w     11.00 138.00   0.50    0.16    --   55.97  53.00-102.07  254
 17  \w     13.00 138.00   0.50    0.16    --   55.97  55.00  28.07  250
 18  \w     13.00 138.00   0.50    0.16    --   55.97  55.00  90.26  250
 19  \w     10.00  78.00   0.50    0.16    --   55.97  52.00  21.52  136
 20  \w    105.00 178.00   0.50    0.16    --  111.94  95.00 -57.00  146
 21  \w     63.00 146.00   0.50    0.16    --  111.94 178.00-120.00  166
 22  \w    103.00 178.00   0.50    0.16    --  111.94 112.00-180.00  150
 23  \w     24.00  80.00   0.50    0.16    --  111.94 -64.00-180.00  112
 24  \w     16.00  99.00   0.50    0.16    --  111.94 -77.00 -30.00  166
 25  \w     27.00  66.00   0.50    0.16    --  111.94 -50.00 -30.00   78
 26  \w     27.00  66.00   0.50    0.16    --  111.94 -50.00-180.00   78
 27  \w     27.00  66.00   0.50    0.16    --  111.94 -50.00-150.00   78
 28  \w     22.00  56.00   0.50    0.16    --  111.94 -38.00-120.00   68
 29  \w     22.00  56.00   0.50    0.16    --  111.94 -38.00-150.00   68
 30  \w     22.00  56.00   0.50    0.16    --  111.94 -38.00 -60.00   68
 31  \w     22.00  56.00   0.50    0.16    --  111.94 -38.00   0.00   68
 32  \w     18.00  50.00   0.50    0.16    --  111.94 -25.00   0.00   64
 33  \w     18.00  50.00   0.50    0.16    --  111.94 -25.00  30.00   64
 34  \w     18.00  50.00   0.50    0.16    --  111.94 -25.00 -90.00   64
 35  \w     18.00  50.00   0.50    0.16    --  111.94 -25.00 -30.00   64
 36  \w     18.00  50.00   0.50    0.16    --  111.94 -25.00  60.00   64
 37  \w     14.00  65.00   0.50    0.16    --  111.94 -12.00 120.00  102
 38  \w    -25.00  48.00   0.50    0.05    --    0.00 -77.00 120.00  146
 39  \w    -25.00  48.00   0.50    0.05    --    0.00 -77.00  90.00  146
 40  \w    -37.00  52.00   0.50    0.16    --   55.97 -30.00 -90.00  178
 41  \w     18.00  50.00   0.50    0.16    --  111.94 -25.00-120.00   64
 42  \w     16.00 105.00   0.50    0.16    --  111.94 -95.00-166.00  178
 43  \w     25.00 109.00   0.50    0.16    --  111.94-112.00 -90.00  168
 44  \w     25.00 109.00   0.50    0.16    --  111.94-112.00 -30.00  168
 45  \w     25.00 109.00   0.50    0.16    --  111.94-112.00-150.00  168
 46  \w     25.00 109.00   0.50    0.16    --  111.94-112.00  30.00  168
 47  \w     25.00 109.00   0.50    0.16    --  111.94-112.00 120.00  168
 48  \w     34.00 111.00   0.50    0.16    --   55.97-125.00 120.00  154
 49  \w     -1.00  59.00   0.50    0.05    --    0.00 -99.00 120.00  120
 50  \w     -9.00 105.00   0.50    0.16    --   55.97 -95.00-166.00  228
 51  \w     -8.00  56.00   0.50    0.05    --    0.00 -95.00-166.00  128
 52  \w    -79.00 -23.00   0.50    0.16    -- -106.00  95.00 -57.00  112
 53  \w    -83.00 -23.00   0.50    0.16    -- -106.00 112.00 150.00  120
 54  \w    -83.00 -23.00   0.50    0.16    -- -106.00 112.00  90.00  120
 55  \w    -86.00 -13.00   0.50    0.16    --  -55.97 125.00   0.00  146
 56  \w    -79.00  27.00   0.50    0.16    --  -55.97  95.00 -57.00  212
 57  \w    -84.00 -23.00   0.50    0.16    -- -106.00  77.00   0.00  122
 58  \w    -84.00 -23.00   0.50    0.16    -- -106.00  77.00  60.00  122
 59  \w    -84.00 -23.00   0.50    0.16    -- -106.00  77.00  90.00  122
 60  \w   -177.00-149.00   0.50    0.16    -- -106.00  38.00 120.00   56
 61  \w   -177.00-149.00   0.50    0.16    -- -106.00  38.00 -90.00   56
 62  \w   -177.00-149.00   0.50    0.16    -- -106.00  38.00-120.00   56
 63  \w   -177.00-149.00   0.50    0.16    -- -106.00  38.00-180.00   56
 64  \w   -177.00-149.00   0.50    0.16    -- -106.00  38.00-150.00   56
 65  \w    -84.00 -23.00   0.50    0.16    -- -106.00  77.00 -60.00  122
 66  \w   -177.00-146.00   0.50    0.16    -- -106.00  25.00 120.00   62
 67  \w   -177.00-146.00   0.50    0.16    -- -106.00  25.00  30.00   62
 68  \w    -46.00  27.00   0.50    0.16    --  -55.97  45.00-180.00  146
 69  \w    -41.00  27.00   0.50    0.16    --  -55.97  15.00-180.00  136
 70  \w   -141.00 -11.00   0.50    0.16    --  -55.97 -54.00-128.89  260
 71  \w   -152.00-100.00   0.50    0.16    --  -55.97 -77.00-150.00  104
 72  \w   -142.00 -91.00   0.50    0.16    --  -55.97 -61.00 -60.00  102
 73  \w   -152.00-100.00   0.50    0.16    --  -55.97 -77.00 -30.00  104
 74  \w   -142.00 -91.00   0.50    0.16    --  -55.97 -61.00  60.00  102
 75  \w   -177.00 -62.00   0.50    0.16    -- -106.00 -55.00  94.63  230
 76  \w   -141.00 -12.00   0.50    0.16    --  -55.97 -55.00-169.75  258
 77  \w   -151.00 -84.00   0.50    0.16    --  -55.97 -95.00-166.00  134
 78  \w   -177.00 -83.00   0.50    0.16    -- -106.00 -95.00-166.00  188
 79  \w   -144.00 -87.00   0.50    0.16    --  -55.97-125.00  90.00  114
 80  \w   -152.00-100.00   0.50    0.16    --  -55.97 -95.00 120.00  104
;
_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      -0.0469362000
_diffrn_orient_matrix_UB_12      -0.1271782000
_diffrn_orient_matrix_UB_13      -0.0300407000
_diffrn_orient_matrix_UB_21      -0.0516404000
_diffrn_orient_matrix_UB_22      0.0382659000
_diffrn_orient_matrix_UB_23      -0.0749952000
_diffrn_orient_matrix_UB_31      0.1218251000
_diffrn_orient_matrix_UB_32      0.0057804000
_diffrn_orient_matrix_UB_33      -0.0310017000
_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  0.0343
_diffrn_reflns_av_unetI/netI     0.0266
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            43322
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.229
_diffrn_reflns_theta_min         3.814
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.915
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79163
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.58a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear reddish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_description       irregular
_exptl_crystal_F_000             992
_refine_diff_density_max         0.585
_refine_diff_density_min         -0.625
_refine_diff_density_rms         0.045
_refine_ls_extinction_coef       0.00022(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     586
_refine_ls_number_reflns         8934
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0352
_refine_ls_R_factor_gt           0.0321
_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^)+(0.0371P)^2^+1.3048P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0787
_refine_ls_wR_factor_ref         0.0800
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8336
_reflns_number_total             8934
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01560f3.cif
_cod_data_source_block           220609_dst_skcoflorange_100k_auto
_cod_depositor_comments
'Adding full bibliography for 7716380--7716384.cif.'
_cod_database_code               7716380
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C26H28CoN3O2
_chemical_oxdiff_usercomment     Pentane
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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:
 C27(H27), C54(H54)
2.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C38(H38A,H38B), C11(H11A,H11B), C37(H37A,H37B)
2.c Aromatic/amide H refined with riding coordinates:
 N26(H26), N53(H53), C25(H25), C46(H46), C15(H15), C19(H19), C52(H52),
 C45(H45), C48(H48), C24(H24), C44(H44), C42(H42), C18(H18), C51(H51), C43(H43),
  C50(H50), C23(H23), C17(H17), C21(H21), C16(H16), C49(H49), C22(H22)
2.d Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C58(H58A,H58B,H58C), C30(H30A,H30B,H30C), C29(H29A,H29B,
 H29C), C57(H57A,H57B,H57C), C28(H28A,H28B,H28C), C56(H56A,H56B,H56C), C55(H55A,
 H55B,H55C)
;
_shelx_res_checksum              43515
_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 1.341
_oxdiff_exptl_absorpt_empirical_full_min 0.840