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_7128703
_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         'C59 H80 K N5 O4 V, C6 H14'
_chemical_formula_sum            'C65 H94 K N5 O4 V'
_chemical_formula_weight         1099.49
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2021-01-21
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2021-04-06 deposited with the CCDC.	2021-07-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.079(1)
_cell_angle_gamma                90
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_cell_length_b                   17.1396(1)
_cell_length_c                   18.6902(1)
_cell_measurement_reflns_used    25797
_cell_measurement_temperature    123.0
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_cell_measurement_theta_min      2.7960
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_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
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_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      123.0
_diffrn_detector                 'Rigaku HyPix-6000 area detector'
_diffrn_detector_area_resol_mean 10.0
_diffrn_detector_type            'HPC area detector'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.992
_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 -10.00 42.00 0.50 2.34 -- -38.95 19.00 60.00 104
 2 \w -12.00 44.00 0.50 2.34 -- -38.95 19.00 150.00 112
 3 \w -27.00 1.00 0.50 2.34 -- -38.95 103.00 153.00 56
 4 \w -38.00 40.00 0.50 2.34 -- -38.95 37.00 90.00 156
 5 \w -12.00 39.00 0.50 2.34 -- -38.95 37.00 -90.00 102
 6 \w -2.00 25.00 0.50 2.34 -- 38.95-103.00 51.00 54
 7 \w 71.00 98.00 0.50 9.36 -- 113.00-103.00 51.00 54
 8 \w 67.00 102.00 0.50 9.36 -- 113.00 -94.00 90.00 70
 9 \w 76.00 106.00 0.50 9.36 -- 113.00-111.00 150.00 60
 10 \w 46.00 74.00 0.50 9.36 -- 113.00 -61.00 120.00 56
 11 \w 34.00 70.00 0.50 9.36 -- 113.00-111.00 150.00 72
 12 \w 36.00 95.00 0.50 9.36 -- 113.00-111.00 30.00 118
 13 \w 56.00 105.00 0.50 9.36 -- 113.00 -94.00 -30.00 98
 14 \w 38.00 75.00 0.50 9.36 -- 113.00 -61.00 -60.00 74
 15 \w 33.00 96.00 0.50 9.36 -- 113.00-111.00 -30.00 126
 16 \w 36.00 90.00 0.50 9.36 -- 113.00-111.00-120.00 108
 17 \w 47.00 72.00 0.50 9.36 -- 113.00 -94.00-180.00 50
 18 \w 42.00 99.00 0.50 9.36 -- 113.00-111.00-150.00 114
 19 \w 90.00 119.00 0.50 9.36 -- 113.00 30.00 -30.00 58
 20 \w 127.00 178.00 0.50 9.36 -- 113.00 30.00 -30.00 102
 21 \w 136.00 162.00 0.50 9.36 -- 113.00 111.00 0.00 52
 22 \w 106.00 132.00 0.50 9.36 -- 113.00 111.00 0.00 52
 23 \w 86.00 112.00 0.50 9.36 -- 113.00 45.00 90.00 52
 24 \w 117.00 178.00 0.50 9.36 -- 113.00 45.00 90.00 122
 25 \w 100.00 172.00 0.50 9.36 -- 113.00 103.00 153.00 144
 26 \w 84.00 176.00 0.50 9.36 -- 113.00 61.00 120.00 184
 27 \w 82.00 129.00 0.50 9.36 -- 113.00 77.00 120.00 94
 28 \w -86.00 -32.00 0.50 2.34 -- -38.95 103.00 153.00 108
 29 \w -93.00 -67.00 0.50 9.36 -- -102.00 103.00 153.00 52
 30 \w -62.00 -37.00 0.50 9.36 -- -102.00 61.00 -30.00 50
 31 \w -153.00-128.00 0.50 9.36 -- -102.00-103.00 51.00 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      -0.0369659000
_diffrn_orient_matrix_UB_12      0.0186555000
_diffrn_orient_matrix_UB_13      0.0143440000
_diffrn_orient_matrix_UB_21      -0.0049450000
_diffrn_orient_matrix_UB_22      -0.0842002000
_diffrn_orient_matrix_UB_23      0.0262856000
_diffrn_orient_matrix_UB_31      0.0108363000
_diffrn_orient_matrix_UB_32      0.0253208000
_diffrn_orient_matrix_UB_33      0.0769360000
_diffrn_radiation_monochromator  'multi-layer mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0196
_diffrn_reflns_av_unetI/netI     0.0209
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       49
_diffrn_reflns_limit_h_min       -49
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            43475
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.504
_diffrn_reflns_theta_min         2.809
_diffrn_source                   'rotating anode X-ray generator'
_diffrn_source_type              PhotonJet-DW
_exptl_absorpt_coefficient_mu    2.260
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76568
_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            'dark brown'
_exptl_crystal_density_diffrn    1.150
_exptl_crystal_description       plate
_exptl_crystal_F_000             4744
_exptl_crystal_size_max          0.205
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.059
_refine_diff_density_max         0.452
_refine_diff_density_min         -0.393
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     758
_refine_ls_number_reflns         12888
_refine_ls_number_restraints     223
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0390
_refine_ls_R_factor_gt           0.0363
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0580P)^2^+7.1119P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1006
_refine_ls_wR_factor_ref         0.1026
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11910
_reflns_number_total             12888
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc03463d2.cif
_cod_data_source_block           v_ono_dmap_k_dme
_cod_depositor_comments
'Adding full bibliography for 7128700--7128707.cif.'
_cod_database_code               7128703