A general benzylic C-H activation and C-C coupling reaction at zirconocenes mediated by C-N bond cleavage in tert-butylisocyanide ‒ unusual formation of iminoacyl complexes
Arndt, Perdita; Reiß, Melanie; Spannenberg, Anke; Schuenemann, Claas; Reiß, Fabian; Beweries, Torsten; Dalton Transactions  (2019) –; doi:10.1039/C9DT03120K

data_7701288
_publ_section_title
;
 A general benzylic C-H activation and C-C coupling reaction at
 zirconocenes mediated by C-N bond cleavage in tert-butylisocyanide --
 unusual formation of iminoacyl complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C9DT03120K
_journal_year                    2019
_chemical_formula_sum            'C82 H96 N4 Zr3'
_chemical_formula_weight         1411.28
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-07-16 deposited with the CCDC.    2019-10-01 downloaded from the CCDC.
;
_cell_angle_alpha                103.768(2)
_cell_angle_beta                 101.7318(19)
_cell_angle_gamma                91.398(2)
_cell_formula_units_Z            2
_cell_length_a                   10.7718(6)
_cell_length_b                   15.6210(9)
_cell_length_c                   20.8511(12)
_cell_measurement_reflns_used    9727
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.58
_cell_measurement_theta_min      2.44
_cell_volume                     3326.8(3)
_computing_cell_refinement       'SAINT (Bruker, 2013)'
_computing_data_collection       'APEX2 (Bruker, 2014)'
_computing_data_reduction        SAINT
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0263
_diffrn_reflns_av_unetI/netI     0.0155
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            123844
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.998
_diffrn_reflns_theta_min         1.478
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.510
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_correction_T_min  0.88
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.409
_exptl_crystal_description       prism
_exptl_crystal_F_000             1472
_exptl_crystal_size_max          0.421
_exptl_crystal_size_mid          0.324
_exptl_crystal_size_min          0.156
_refine_diff_density_max         1.598
_refine_diff_density_min         -1.488
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     900
_refine_ls_number_reflns         16077
_refine_ls_number_restraints     165
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0369
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0303P)^2^+5.1850P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0840
_refine_ls_wR_factor_ref         0.0869
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14674
_reflns_number_total             16077
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03120k2.cif
_cod_data_source_block           AX1720
_cod_database_code               7701288
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              20824