A titanium redox-switch enables reversible C-C bond forming and splitting reactions.
G Jafari, Mehrafshan; Fehn, Dominik; Sandoval-Pauker, Christian; Gau, Michael R.; Meyer, Karsten; Pinter, Balazs; Mindiola, Daniel J.; Reinholdt, Anders; Chemical science 16 (2025) 17714–17724; doi:10.1039/d5sc04824a

data_1575523
_publ_section_title
;
 A titanium redox-switch enables reversible C-C bond forming and splitting
 reactions.
;
_journal_issue                   38
_journal_name_full               'Chemical science'
_journal_page_first              17714
_journal_page_last               17724
_journal_paper_doi               10.1039/d5sc04824a
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         'C57 H85 B N10 V'
_chemical_formula_sum            'C57 H85 B N10 V'
_chemical_formula_weight         972.09
_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             2021-11-29
_audit_creation_method
;
Olex2 1.5
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6396)
;
_audit_update_record
;
2025-04-21 deposited with the CCDC.	2025-08-22 downloaded from the CCDC.
;
_cell_angle_alpha                104.5687(18)
_cell_angle_beta                 90.2187(18)
_cell_angle_gamma                118.154(2)
_cell_formula_units_Z            2
_cell_length_a                   11.9108(2)
_cell_length_b                   12.6051(2)
_cell_length_c                   24.0379(5)
_cell_measurement_reflns_used    31568
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.2710
_cell_measurement_theta_min      1.7980
_cell_volume                     3047.76(12)
_computing_cell_refinement       'CrysAlisPro 1.171.41.115a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.115a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.115a (Rigaku OD, 2021)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 2012)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100
_diffrn_detector                 'HPC area detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix-6000HE
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -65.00  18.00   0.50   35.00    --    8.17 -37.00 -90.00  166
  2  \w    -63.00  23.00   0.50   35.00    --    8.17 -57.00-150.00  172
  3  \w    -14.00  81.00   0.50   35.00    --    8.17  77.00 -30.00  190
  4  \w    -81.00   5.00   0.50   35.00    --   -9.89 -57.00 150.00  172
  5  \w    -32.00  63.00   0.50   35.00    --   -9.89  77.00  30.00  190
  6  \w    -30.00  63.00   0.50   35.00    --   -9.89  71.00 -56.18  186
  7  \w    -22.00  63.00   0.50   35.00    --   -9.89  37.00 -60.00  170
  8  \w    -81.00  13.00   0.50   35.00    --   -9.89 -77.00 120.00  188
  9  \w    -81.00   5.00   0.50   35.00    --   -9.89 -57.00  30.00  172
 10  \w    -81.00   1.00   0.50   35.00    --   -9.89 -57.00 -90.00  164
;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB Synergy-S'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0354037000
_diffrn_orient_matrix_UB_12      -0.0233491000
_diffrn_orient_matrix_UB_13      -0.0281595000
_diffrn_orient_matrix_UB_21      0.0495112000
_diffrn_orient_matrix_UB_22      -0.0102166000
_diffrn_orient_matrix_UB_23      -0.0121019000
_diffrn_orient_matrix_UB_31      -0.0308732000
_diffrn_orient_matrix_UB_32      -0.0615647000
_diffrn_orient_matrix_UB_33      0.0031075000
_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  0.0545
_diffrn_reflns_av_unetI/netI     0.0357
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            89248
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.282
_diffrn_reflns_theta_min         1.769
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.204
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68677
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALE3 ABSPACK'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.059
_exptl_crystal_description       plate
_exptl_crystal_F_000             1050
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.241
_refine_diff_density_min         -0.702
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     733
_refine_ls_number_reflns         15113
_refine_ls_number_restraints     374
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0996
_refine_ls_R_factor_gt           0.0895
_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^)+(0.0819P)^2^+8.0792P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2370
_refine_ls_wR_factor_ref         0.2421
_reflns_number_gt                12958
_reflns_number_total             15113
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc04824a2.cif
_cod_data_source_block           9875_cmpd6
_cod_depositor_comments
'Adding full bibliography for 1575521--1575523.cif.'
_cod_original_cell_volume        3047.78(12)
_cod_database_code               1575523
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.994
_shelx_estimated_absorpt_t_min   0.936
_shelx_res_checksum              61047
_shelx_fab_checksum              91916
_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 1.353
_oxdiff_exptl_absorpt_empirical_full_min 0.602