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_7128707
_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         'C113 H137 K N5 O6 V2, C16 H40 K O8, C6 H14'
_chemical_formula_sum            'C135 H191 K2 N5 O14 V2'
_chemical_formula_weight         2288.00
_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
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-01-17
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2021-04-06 deposited with the CCDC.	2021-07-21 downloaded from the CCDC.
;
_cell_angle_alpha                78.203(3)
_cell_angle_beta                 88.731(3)
_cell_angle_gamma                83.903(3)
_cell_formula_units_Z            2
_cell_length_a                   16.6092(6)
_cell_length_b                   17.7479(6)
_cell_length_c                   22.6639(7)
_cell_measurement_reflns_used    12594
_cell_measurement_temperature    123.0
_cell_measurement_theta_max      30.1560
_cell_measurement_theta_min      1.6650
_cell_volume                     6502.7(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r16 (Rigaku, 2014)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      123.0
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 7.1429
_diffrn_detector_type            'Rigaku Saturn724+ area detector'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.987
_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   -115.00  65.00   0.50    8.00    --  -25.00  45.00   0.00  360
  2  \w   -115.00  65.00   0.50    8.00    --  -25.00  45.00  90.00  360
  3  \w   -115.00  65.00   0.50    8.00    --  -25.00  45.00 180.00  360
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku Saturn724+ (4x4 bin mode)'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0051602000
_diffrn_orient_matrix_UB_12      0.0358995000
_diffrn_orient_matrix_UB_13      -0.0194791000
_diffrn_orient_matrix_UB_21      -0.0106199000
_diffrn_orient_matrix_UB_22      0.0195214000
_diffrn_orient_matrix_UB_23      0.0238648000
_diffrn_orient_matrix_UB_31      0.0412934000
_diffrn_orient_matrix_UB_32      -0.0039022000
_diffrn_orient_matrix_UB_33      0.0085573000
_diffrn_radiation_monochromator  'multi-layer mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0926
_diffrn_reflns_av_unetI/netI     0.1362
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            67077
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.560
_diffrn_reflns_theta_min         3.018
_diffrn_source                   'rotating anode X-ray generator'
_diffrn_source_type              micromax007
_exptl_absorpt_coefficient_mu    0.268
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61688
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'reddish brown'
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.169
_exptl_crystal_description       plate
_exptl_crystal_F_000             2464
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_platon_squeeze_details
;
The unit cell contains two hexane molecules which have been 
treated as a diffuse contribution to the overall scattering 
without specific atom positions by SQEEZE/PLATON.
;
_refine_diff_density_max         0.519
_refine_diff_density_min         -0.658
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.976
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1408
_refine_ls_number_reflns         29676
_refine_ls_number_restraints     225
_refine_ls_restrained_S_all      0.981
_refine_ls_R_factor_all          0.1560
_refine_ls_R_factor_gt           0.0797
_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^)+(0.1004P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1790
_refine_ls_wR_factor_ref         0.2236
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15337
_reflns_number_total             29676
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc03463d2.cif
_cod_data_source_block           (v_ono_k)2_3ncar_sq
_cod_depositor_comments
'Adding full bibliography for 7128700--7128707.cif.'
_cod_database_code               7128707
_shelx_estimated_absorpt_t_max   0.979
_shelx_estimated_absorpt_t_min   0.969
_platon_squeeze_void_probe_radius 1.20