Migratory insertion of isocyanide into a ketenyl-tungsten bond as key step in cyclization reactions.
Timmermann, Christopher; Thiem, Paula; Wanitschke, Dominik; Hüttenschmidt, Mareike; Romischke, Johanna; Villinger, Alexander; Seidel, Wolfram W.; Chemical science 13 (2021) 123–132; doi:10.1039/d1sc06149f

data_1565576
_publ_section_title
;
 Migratory insertion of isocyanide into a ketenyl-tungsten bond as key
 step in cyclization reactions.
;
_journal_issue                   1
_journal_name_full               'Chemical science'
_journal_page_first              123
_journal_page_last               132
_journal_paper_doi               10.1039/d1sc06149f
_journal_volume                  13
_journal_year                    2021
_chemical_formula_moiety         'C62 H78 B2 N14 O7 W2, 3(C H2 Cl2)'
_chemical_formula_sum            'C65 H84 B2 Cl6 N14 O7 W2'
_chemical_formula_weight         1775.48
_chemical_name_systematic
Bis[di(carbonyl)-\k2-C,O-{3-(2,6-dimethylphenylamino)propan-3-ylidene-1-oate}-hydridotris(3,4,5-trimethylpyrazolyl)borato-tungsten(II)]anhydride
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
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_atom_sites_solution_hydrogens   geom
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_audit_update_record
;
2021-02-04 deposited with the CCDC.	2021-11-22 downloaded from the CCDC.
;
_cell_angle_alpha                82.881(2)
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_cell_angle_gamma                62.331(2)
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_cell_measurement_temperature    173(2)
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_cell_measurement_theta_min      2.56
_cell_volume                     3729.6(4)
_computing_cell_refinement       'Bruker Apex V7.51A'
_computing_data_collection       'Bruker Apex V7.51A'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP-3v2.01 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      173(2)
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_diffrn_measurement_device_type  'Bruker D8 QUEST diffractometer'
_diffrn_measurement_method       'phi and omega scans'
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_diffrn_reflns_av_R_equivalents  0.0781
_diffrn_reflns_av_unetI/netI     0.0598
_diffrn_reflns_Laue_measured_fraction_full 0.999
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_diffrn_reflns_limit_h_min       -21
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_diffrn_reflns_point_group_measured_fraction_full 0.999
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_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.999
_diffrn_reflns_theta_min         2.286
_diffrn_source                   'microfocus sealed tube'
_exptl_absorpt_coefficient_mu    3.356
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_exptl_absorpt_correction_type   multi-scan
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_exptl_crystal_colour            yellow
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_exptl_crystal_description       block
_exptl_crystal_F_000             1776
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane/methanol'
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.070
_platon_squeeze_details
;
The unit cell contains six dichloromethane molecules which have been treated 
as a diffuse contribution to the overall scattering without specific atom 
positions by SQUEEZE/PLATON.
;
_refine_diff_density_max         2.712
_refine_diff_density_min         -1.489
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
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_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0787
_refine_ls_R_factor_gt           0.0427
_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^)+(0.0386P)^2^+1.6821P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0801
_refine_ls_wR_factor_ref         0.0868
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15024
_reflns_number_total             21753
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc06149f2.cif
_cod_data_source_block           is_ct177
_cod_depositor_comments
'Adding full bibliography for 1565569--1565576.cif.'
_cod_database_code               1565576
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.689
_shelx_estimated_absorpt_t_max   0.799
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              19855
_shelx_hkl_checksum              50104