Systematic reductive oligomerization of isocyanides with a vanadium(ii) complex.
Hasegawa, Sui; Ishida, Yutaka; Kawaguchi, Hiroyuki; Chemical communications (Cambridge, England) 57 (2021) 8296–8299; doi:10.1039/d1cc03463d

data_7128706
_publ_section_title
;
 Systematic reductive oligomerization of isocyanides with a vanadium(ii)
 complex.
;
_journal_issue                   67
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              8296
_journal_page_last               8299
_journal_paper_doi               10.1039/d1cc03463d
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C77 H88 K2 N5 O8 V, 0.5(C6 H14), 2(C7 H8)'
_chemical_formula_sum            'C94 H111 K2 N5 O8 V'
_chemical_formula_weight         1568.01
_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   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2021-02-22
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-04-06 deposited with the CCDC.	2021-07-21 downloaded from the CCDC.
;
_cell_angle_alpha                96.746(2)
_cell_angle_beta                 116.027(2)
_cell_angle_gamma                94.642(2)
_cell_formula_units_Z            2
_cell_length_a                   16.1228(3)
_cell_length_b                   17.1683(4)
_cell_length_c                   17.5730(6)
_cell_measurement_reflns_used    13893
_cell_measurement_temperature    123
_cell_measurement_theta_max      74.1350
_cell_measurement_theta_min      2.8220
_cell_volume                     4292.6(2)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_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  (Sheldrick, 2015)'
_diffrn_ambient_temperature      123
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.982
_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     -9.00  44.00   0.50    7.17    --  -38.95  19.00   0.00  106
  2  \w    -10.00  44.00   0.50    7.17    --  -38.95  19.00  90.00  108
  3  \w    -20.00  31.00   0.50    7.17    --  -38.95  19.00 150.00  102
  4  \w     12.00 111.00   0.50    7.17    --   38.95  57.00 150.00  198
  5  \w     66.00 115.00   0.50    7.17    --   38.95 164.00 113.00   98
  6  \w    118.00 144.00   0.50   21.50    --  113.00 164.00 113.00   52
  7  \w    143.00 171.00   0.50   21.50    --  113.00 111.00  90.00   56
  8  \w     95.00 148.00   0.50   21.50    --  113.00 116.00 -34.00  106
  9  \w    135.00 165.00   0.50   21.50    --  113.00 111.00 -60.00   60
 10  \w     89.00 139.00   0.50   21.50    --  113.00  61.00-150.00  100
 11  \w     89.00 124.00   0.50   21.50    --  113.00 111.00 -60.00   70
 12  \w     90.00 120.00   0.50   21.50    --  113.00 111.00 -90.00   60
 13  \w     93.00 175.00   0.50   21.50    --  113.00 111.00-150.00  164
 14  \w     80.00 178.00   0.50   21.50    --  113.00  77.00  30.00  196
 15  \w     87.00 115.00   0.50   21.50    --  113.00 111.00  90.00   56
 16  \w     67.00  96.00   0.50   21.50    --  113.00 178.00   0.00   58
 17  \w     49.00 123.00   0.50   21.50    --  113.00 178.00-120.00  148
 18  \w     78.00 178.00   0.50   21.50    --  113.00  30.00 -30.00  200
 19  \w     71.00 108.00   0.50   21.50    --  113.00-116.00-122.00   74
 20  \w     75.00 106.00   0.50   21.50    --  113.00 -94.00-150.00   62
 21  \w     65.00 108.00   0.50   21.50    --  113.00-111.00 -60.00   86
 22  \w     80.00 106.00   0.50   21.50    --  113.00 -94.00   0.00   52
 23  \w     76.00 107.00   0.50   21.50    --  113.00-111.00 -30.00   62
 24  \w     80.00 106.00   0.50   21.50    --  113.00 -94.00 -30.00   52
 25  \w     71.00 101.00   0.50   21.50    --  113.00 -94.00  30.00   60
 26  \w     75.00 108.00   0.50   21.50    --  113.00-111.00  90.00   66
 27  \w     75.00 105.00   0.50   21.50    --  113.00-111.00 120.00   60
 28  \w     67.00 106.00   0.50   21.50    --  113.00-111.00 150.00   78
 29  \w     59.00  92.00   0.50   21.50    --  113.00 -94.00  60.00   66
 30  \w     67.00  94.00   0.50   21.50    --  113.00-111.00   0.00   54
 31  \w     43.00  89.00   0.50   21.50    --  113.00-164.00  89.00   92
 32  \w     47.00  73.00   0.50   21.50    --  113.00-111.00 120.00   52
 33  \w     45.00  74.00   0.50   21.50    --  113.00 -61.00  90.00   58
 34  \w     34.00  66.00   0.50   21.50    --  113.00-111.00  90.00   64
 35  \w     34.00  59.00   0.50   21.50    --  113.00 -94.00  30.00   50
 36  \w     38.00  71.00   0.50   21.50    --  113.00 -61.00 -30.00   66
 37  \w     44.00  74.00   0.50   21.50    --  113.00 -61.00 -90.00   60
 38  \w     47.00  73.00   0.50   21.50    --  113.00 -94.00 -30.00   52
 39  \w     53.00  79.00   0.50   21.50    --  113.00-111.00 -90.00   52
 40  \w     39.00 106.00   0.50   21.50    --  113.00-111.00-150.00  134
 41  \w     39.00  64.00   0.50   21.50    --  113.00-111.00 -60.00   50
 42  \w     34.00 105.00   0.50   21.50    --  113.00 -94.00 -90.00  142
 43  \w     38.00 107.00   0.50   21.50    --  113.00-111.00-180.00  138
 44  \w     33.00  58.00   0.50   21.50    --  113.00 -94.00-150.00   50
 45  \w     34.00  97.00   0.50   21.50    --  113.00 -94.00-120.00  126
 46  \w     16.00  42.00   0.50    7.17    --   38.95-116.00-122.00   52
 47  \w     33.00  76.00   0.50   21.50    --  113.00-111.00  60.00   86
 48  \w     33.00  68.00   0.50   21.50    --  113.00 -94.00 120.00   70
 49  \w     30.00 178.00   0.50   21.50    --  113.00   0.00 120.00  296
 50  \w     55.00  80.00   0.50    7.17    --   38.95-164.00  89.00   50
 51  \w    -20.00  37.00   0.50    7.17    --  -38.95  19.00-120.00  114
 52  \w    -16.00  42.00   0.50    7.17    --  -38.95  19.00 -60.00  116
 53  \w    -38.00   8.00   0.50    7.17    --  -38.95  37.00 -90.00   92
 54  \w    -61.00 -32.00   0.50   21.50    -- -102.00 111.00-120.00   58
 55  \w    -93.00 -25.00   0.50    7.17    --  -38.95 116.00 -34.00  136
 56  \w    -67.00 -32.00   0.50   21.50    -- -102.00  61.00   0.00   70
 57  \w    -90.00 -65.00   0.50   21.50    -- -102.00 116.00 -34.00   50
 58  \w   -108.00 -78.00   0.50   21.50    -- -102.00 111.00   0.00   60
 59  \w   -109.00 -84.00   0.50   21.50    -- -102.00 164.00 113.00   50
 60  \w   -122.00 -91.00   0.50    7.17    --  -38.95 164.00 113.00   62
 61  \w   -108.00 -69.00   0.50   21.50    -- -102.00 111.00-120.00   78
 62  \w   -131.00-106.00   0.50   21.50    -- -102.00 -61.00 -60.00   50
 63  \w   -123.00 -87.00   0.50   21.50    -- -102.00-116.00-122.00   72
 64  \w   -170.00-136.00   0.50   21.50    -- -102.00 -61.00 -60.00   68
 65  \w   -116.00 -60.00   0.50    7.17    --  -38.95-164.00  89.00  112
 66  \w   -126.00-101.00   0.50   21.50    -- -102.00-164.00  89.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB Synergy-DW'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0185740000
_diffrn_orient_matrix_UB_12      -0.0178030000
_diffrn_orient_matrix_UB_13      0.0895417000
_diffrn_orient_matrix_UB_21      0.0361571000
_diffrn_orient_matrix_UB_22      0.0884927000
_diffrn_orient_matrix_UB_23      0.0383274000
_diffrn_orient_matrix_UB_31      -0.0995472000
_diffrn_orient_matrix_UB_32      0.0141690000
_diffrn_orient_matrix_UB_33      -0.0178106000
_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  0.0739
_diffrn_reflns_av_unetI/netI     0.0733
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            64961
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.755
_diffrn_reflns_theta_min         2.621
_diffrn_source                   'rotating anode X-ray generator'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.289
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82724
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.213
_exptl_crystal_description       plate
_exptl_crystal_F_000             1670
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_platon_squeeze_details
;
The unit cell contains two toluene molecules and one hexane 
molecule which have been treatedas a diffuse contribution to 
the overall scattering without specific atom positions by 
SQUEEZE/PLATON.
;
_refine_diff_density_max         1.095
_refine_diff_density_min         -0.462
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.986
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     927
_refine_ls_number_reflns         17765
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.986
_refine_ls_R_factor_all          0.1055
_refine_ls_R_factor_gt           0.0775
_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^)+(0.1635P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2142
_refine_ls_wR_factor_ref         0.2413
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11719
_reflns_number_total             17765
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc03463d2.cif
_cod_data_source_block           v_ono_indigo_k2_dme
_cod_depositor_comments
'Adding full bibliography for 7128700--7128707.cif.'
_cod_database_code               7128706
_shelx_estimated_absorpt_t_max   0.935
_shelx_estimated_absorpt_t_min   0.821
_platon_squeeze_void_probe_radius 1.20