Synthesis and molecular structural studies of racemic chiral-at-vanadium(V) complexes using an unsymmetric achiral phenolic bidentate ligand.
Nagata, Koichi; Hino, Ayako; Ube, Hitoshi; Sato, Hiroyasu; Shionoya, Mitsuhiko; Dalton transactions (Cambridge, England : 2003) 52 (2023) 3295–3299; doi:10.1039/d2dt03436k

data_7712089
_publ_section_title
;
 Synthesis and molecular structural studies of racemic
 chiral-at-vanadium(V) complexes using an unsymmetric achiral phenolic
 bidentate ligand.
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3295
_journal_page_last               3299
_journal_paper_doi               10.1039/d2dt03436k
_journal_volume                  52
_journal_year                    2023
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C35 H48 Cl O3 V'
_chemical_formula_sum            'C35 H48 Cl O3 V'
_chemical_formula_weight         603.12
_space_group_crystal_system      orthorhombic
_space_group_IT_number           26
_space_group_name_Hall           'P 2c -2'
_space_group_name_H-M_alt        'P m c 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-10-01
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-10-01 deposited with the CCDC.	2023-01-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.4288(2)
_cell_length_b                   27.1835(4)
_cell_length_c                   11.2290(2)
_cell_measurement_reflns_used    16652
_cell_measurement_temperature    123.15
_cell_measurement_theta_max      71.9060
_cell_measurement_theta_min      3.2280
_cell_volume                     3183.32(10)
_computing_cell_refinement       'CrysAlisPro 1.171.43.40a (Rigaku OD, 2022)'
_computing_data_collection
'CrysAlisPro system (CCD 39.46e (release 04-06-2018))'
_computing_data_reduction        'CrysAlisPro 1.171.43.40a (Rigaku OD, 2022)'
_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      123.15
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_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    -24.00   3.00   0.50    1.40    --    0.00  38.00 120.00   54
  2  \w    -39.00  27.00   0.50    1.40    --    0.00 -57.00 120.00  132
  3  \w     41.00  78.00   0.50    1.40    --    0.00  38.00 120.00   74
  4  \w    -49.00  27.00   0.50    1.40    --    0.00 -38.00-150.00  152
  5  \w    -26.00  87.00   0.50    1.40    --    0.00  38.00-150.00  226
  6  \w    142.00 181.00   0.50    5.59    --   95.70  45.00-120.00   78
  7  \w     70.00 129.00   0.50    5.59    --   95.70  45.00-120.00  118
  8  \w    116.00 142.00   0.50    5.59    --   95.70  82.00 120.00   52
  9  \w      9.00  69.00   0.50    5.59    --   95.70 -82.00 -90.00  120
 10  \w      6.00  96.00   0.50    5.59    --   95.70 -61.00 -90.00  180
 11  \w     51.00  93.00   0.50    5.59    --   95.70 -61.00-180.00   84
 12  \w      7.00 124.00   0.50    5.59    --   95.70 -61.00   0.00  234
 13  \w     72.00  98.00   0.50    5.59    --   95.70 -82.00-120.00   52
 14  \w     68.00  97.00   0.50    5.59    --   95.70 -61.00  90.00   58
 15  \w    104.00 185.00   0.50    5.59    --   95.70  61.00 -60.00  162
 16  \w     90.00 128.00   0.50    5.59    --   95.70 -82.00  60.00   76
 17  \w     82.00 109.00   0.50    5.59    --   95.70 -82.00  30.00   54
 18  \w     80.00 164.00   0.50    5.59    --   95.70  45.00 -30.00  168
 19  \w      7.00  41.00   0.50    5.59    --   95.70 -82.00  30.00   68
 20  \w     45.00 132.00   0.50    5.59    --   95.70 -82.00-180.00  174
 21  \w     68.00  95.00   0.50    5.59    --   95.70 -82.00 -60.00   54
 22  \w     76.00 110.00   0.50    5.59    --   95.70  82.00 120.00   68
 23  \w     80.00 109.00   0.50    5.59    --   95.70 -82.00 -90.00   58
 24  \w     32.00 132.00   0.50    5.59    --   95.70 -82.00   0.00  200
 25  \w     70.00 151.00   0.50    5.59    --   95.70  45.00  90.00  162
 26  \w     29.00 130.00   0.50    5.59    --   95.70 -82.00 120.00  202
 27  \w     76.00 177.00   0.50    5.59    --   95.70  45.00-150.00  202
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0223410000
_diffrn_orient_matrix_UB_12      0.0293565000
_diffrn_orient_matrix_UB_13      -0.0547711000
_diffrn_orient_matrix_UB_21      0.0307334000
_diffrn_orient_matrix_UB_22      -0.1419921000
_diffrn_orient_matrix_UB_23      -0.0090234000
_diffrn_orient_matrix_UB_31      -0.1318803000
_diffrn_orient_matrix_UB_32      -0.0281186000
_diffrn_orient_matrix_UB_33      -0.0113688000
_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  0.0384
_diffrn_reflns_av_unetI/netI     0.0265
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            35727
_diffrn_reflns_point_group_measured_fraction_full 0.905
_diffrn_reflns_point_group_measured_fraction_max 0.894
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.100
_diffrn_reflns_theta_min         3.252
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    3.623
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82235
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.40a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.258
_exptl_crystal_description       block
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.550
_refine_diff_density_min         -0.702
_refine_diff_density_rms         0.063
_refine_ls_abs_structure_details
;
 Flack x determined using 1918 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.004(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     731
_refine_ls_number_reflns         5925
_refine_ls_number_restraints     1249
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0775
_refine_ls_R_factor_gt           0.0712
_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^)+(0.1059P)^2^+4.0451P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2037
_refine_ls_wR_factor_ref         0.2112
_reflns_Friedel_coverage         0.700
_reflns_Friedel_fraction_full    0.798
_reflns_Friedel_fraction_max     0.778
_reflns_number_gt                5329
_reflns_number_total             5925
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03436k2.cif
_cod_data_source_block           vocll1_op
_cod_depositor_comments
'Adding full bibliography for 7712089--7712090.cif.'
_cod_database_code               7712089
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C33 H50 Cl V Cl O3'
_shelx_estimated_absorpt_t_max   0.691
_shelx_estimated_absorpt_t_min   0.562
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.50787
 0.49213
2. Restrained distances
 C27-C28
 1.54 with sigma of 0.01
 C20-C19 \\sim C19-C18 \\sim C18-C20
 with sigma of 0.01
 C52-C53 \\sim C52-C55 \\sim C52-C54
 with sigma of 0.01
 C20-C17 \\sim C18-C17 \\sim C19-C17
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C68(0.5) H68A(0.5) H68B(0.5) H68C(0.5) C67(0.5) H67A(0.5)
 H67B(0.5) H67C(0.5) H33A(0.5) H33B(0.5) H33C(0.5) H32A(0.5) H32B(0.5)
 H32C(0.5) V2(0.5) Cl1(0.5) O5(0.5) O6(0.5) O4(0.5) C36(0.5) C37(0.5) C38(0.5)
 H38(0.5) C39(0.5) C40(0.5) H40(0.5) C41(0.5) C70(0.5) H70A(0.5) H70B(0.5)
 C61(0.5) C60(0.5) H60(0.5) C59(0.5) C58(0.5) H58(0.5) C57(0.5) C56(0.5)
 C52(0.5) C66(0.5) C62(0.5) C64(0.5) H64A(0.5) H64B(0.5) H64C(0.5) C63(0.5)
 H63A(0.5) H63B(0.5) H63C(0.5) C65(0.5) H65A(0.5) H65B(0.5) H65C(0.5) V1(0.5)
 Cl2(0.5) O3(0.5) O2(0.5) O1(0.5) C21(0.5) C22(0.5) C23(0.5) H23(0.5) C24(0.5)
 C25(0.5) H25(0.5) C26(0.5) C35(0.5) H35A(0.5) H35B(0.5) C6(0.5) C5(0.5)
 H5(0.5) C4(0.5) C3(0.5) H3(0.5) C2(0.5) C1(0.5) C27(0.5) C29(0.5) H29A(0.5)
 H29B(0.5) H29C(0.5) C30(0.5) H30A(0.5) H30B(0.5) H30C(0.5) C28(0.5) H28A(0.5)
 H28B(0.5) H28C(0.5) C17(0.5) C34(0.5) H34A(0.5) H34B(0.5) H34C(0.5) C7(0.5)
 C16(0.5) H16A(0.5) H16B(0.5) C15(0.5) H15(0.5) C10(0.5) H10A(0.5) H10B(0.5)
 C14(0.5) H14A(0.5) H14B(0.5) C9(0.5) H9A(0.5) H9B(0.5) C13(0.5) H13(0.5)
 C12(0.5) H12A(0.5) H12B(0.5) C8(0.5) H8A(0.5) H8B(0.5) C11(0.5) H11(0.5)
 C50(0.5) H50(0.5) C44(0.5) H44A(0.5) H44B(0.5) C48(0.5) H48(0.5) C49(0.5)
 H49A(0.5) H49B(0.5) C47(0.5) H47A(0.5) H47B(0.5) C51(0.5) H51A(0.5) H51B(0.5)
 C46(0.5) H46(0.5) C43(0.5) H43A(0.5) H43B(0.5) C45(0.5) H45A(0.5) H45B(0.5)
 C42(0.5) C54(0.5) H54A(0.5) H54B(0.5) H54C(0.5) C19(0.5) H19A(0.5) H19B(0.5)
 H19C(0.5) C18(0.5) H18A(0.5) H18B(0.5) H18C(0.5) C55(0.5) H55A(0.5) H55B(0.5)
 H55C(0.5) C53(0.5) H53A(0.5) H53B(0.5) H53C(0.5) C20(0.5) H20A(0.5) H20B(0.5)
 H20C(0.5) C69(0.5) H69A(0.5) H69B(0.5) H69C(0.5)
6.a Ternary CH refined with riding coordinates:
 C15(H15), C13(H13), C11(H11), C50(H50), C48(H48), C46(H46)
6.b Secondary CH2 refined with riding coordinates:
 C70(H70A,H70B), C35(H35A,H35B), C16(H16A,H16B), C10(H10A,H10B), C14(H14A,
 H14B), C9(H9A,H9B), C12(H12A,H12B), C8(H8A,H8B), C44(H44A,H44B), C49(H49A,
 H49B), C47(H47A,H47B), C51(H51A,H51B), C43(H43A,H43B), C45(H45A,H45B)
6.c Aromatic/amide H refined with riding coordinates:
 C38(H38), C40(H40), C60(H60), C58(H58), C23(H23), C25(H25), C5(H5), C3(H3)
6.d Idealised Me refined as rotating group:
 C68(H68A,H68B,H68C), C67(H67A,H67B,H67C), C33(H33A,H33B,H33C), C32(H32A,H32B,
 H32C), C64(H64A,H64B,H64C), C63(H63A,H63B,H63C), C65(H65A,H65B,H65C), C29(H29A,
 H29B,H29C), C30(H30A,H30B,H30C), C28(H28A,H28B,H28C), C34(H34A,H34B,H34C),
 C54(H54A,H54B,H54C), C19(H19A,H19B,H19C), C18(H18A,H18B,H18C), C55(H55A,H55B,
 H55C), C53(H53A,H53B,H53C), C20(H20A,H20B,H20C), C69(H69A,H69B,H69C)
;
_shelx_res_checksum              25658
_shelx_hkl_checksum              44890
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.111
_oxdiff_exptl_absorpt_empirical_full_min 0.597