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_7712090
_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_formula_moiety         'C39 H57 O4 V'
_chemical_formula_sum            'C39 H57 O4 V'
_chemical_formula_weight         640.78
_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
_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                75.111(2)
_cell_angle_beta                 69.895(2)
_cell_angle_gamma                75.358(2)
_cell_formula_units_Z            2
_cell_length_a                   11.3936(3)
_cell_length_b                   13.2903(3)
_cell_length_c                   13.4060(3)
_cell_measurement_reflns_used    9880
_cell_measurement_temperature    93.15
_cell_measurement_theta_max      73.2560
_cell_measurement_theta_min      3.5200
_cell_volume                     1811.79(8)
_computing_cell_refinement       'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.20a (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      93.15
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.965
_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 -39.00 33.00 0.50 0.50 -- 0.00 19.00 30.00 144
 2 \w -40.00 -1.00 0.50 0.50 -- 0.00 -57.00 30.00 78
 3 \w -88.00 -62.00 0.50 0.50 -- 0.00 -82.00-180.00 52
 4 \w 39.00 87.00 0.50 0.50 -- 0.00 19.00 30.00 96
 5 \w -37.00 35.00 0.50 0.50 -- 0.00 -82.00-180.00 144
 6 \w -83.00 -58.00 0.50 0.50 -- 0.00 -57.00 30.00 50
 7 \w 100.00 125.00 0.50 1.38 -- 98.20 -45.00 30.00 50
 8 \w 17.00 63.00 0.50 1.38 -- 98.20 -45.00 30.00 92
 9 \w 23.00 99.00 0.50 1.38 -- 98.20 -45.00-180.00 152
 10 \w 27.00 119.00 0.50 1.38 -- 98.20 -61.00 90.00 184
 11 \w 54.00 135.00 0.50 1.38 -- 98.20 -82.00 -90.00 162
 12 \w 23.00 49.00 0.50 1.38 -- 98.20 -82.00 150.00 52
 13 \w 74.00 100.00 0.50 1.38 -- 98.20 -82.00 150.00 52
 14 \w 9.00 90.00 0.50 1.38 -- 98.20 -15.00-120.00 162
 15 \w 81.00 131.00 0.50 1.38 -- 98.20 -82.00 -60.00 100
 16 \w 19.00 134.00 0.50 1.38 -- 98.20 -82.00-150.00 230
 17 \w 73.00 126.00 0.50 1.38 -- 98.20 -30.00 150.00 106
 18 \w 10.00 40.00 0.50 1.38 -- 98.20 -30.00 150.00 60
 19 \w 89.00 130.00 0.50 1.38 -- 98.20 -30.00 -90.00 82
 20 \w 22.00 118.00 0.50 1.38 -- 98.20 -82.00 90.00 192
 21 \w 106.00 148.00 0.50 1.38 -- 98.20 -15.00-120.00 84
 22 \w 32.00 85.00 0.50 1.38 -- 98.20 -30.00 -90.00 106
 23 \w 84.00 111.00 0.50 1.38 -- 98.20 -82.00 0.00 54
 24 \w 92.00 118.00 0.50 1.38 -- 98.20 -82.00-180.00 52
 25 \w 50.00 183.00 0.50 1.38 -- 98.20 15.00 150.00 266
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Pro: Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0268563000
_diffrn_orient_matrix_UB_12      -0.1088700000
_diffrn_orient_matrix_UB_13      0.0716231000
_diffrn_orient_matrix_UB_21      -0.0223580000
_diffrn_orient_matrix_UB_22      -0.0539281000
_diffrn_orient_matrix_UB_23      -0.0791472000
_diffrn_orient_matrix_UB_31      0.1421802000
_diffrn_orient_matrix_UB_32      -0.0106730000
_diffrn_orient_matrix_UB_33      -0.0642247000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0241
_diffrn_reflns_av_unetI/netI     0.0319
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            17500
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.417
_diffrn_reflns_theta_min         3.499
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.568
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91320
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro 1.171.39.20a (Rigaku Oxford Diffraction, 2015)'
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.175
_exptl_crystal_description       block
_exptl_crystal_F_000             692
_exptl_crystal_preparation       'sensitive to oxygene and water'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.258
_refine_diff_density_min         -0.386
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     409
_refine_ls_number_reflns         7043
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0365
_refine_ls_R_factor_gt           0.0337
_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^)+(0.0459P)^2^+0.5283P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0905
_refine_ls_wR_factor_ref         0.0922
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6522
_reflns_number_total             7043
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03436k2.cif
_cod_data_source_block           kn02214_a
_cod_depositor_comments
'Adding full bibliography for 7712089--7712090.cif.'
_cod_database_code               7712090
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         VOCH
_chemical_oxdiff_usercomment     'VOOtBuBL, RT, GB'
_shelx_estimated_absorpt_t_max   0.882
_shelx_estimated_absorpt_t_min   0.783
_reflns_odcompleteness_completeness 99.43
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C21(H21), C23(H23), C26(H26)
2.b Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C25(H25A,H25B), C24(H24A,H24B), C28(H28A,H28B), C33(H33A,
 H33B), C22(H22A,H22B), C27(H27A,H27B)
2.c Aromatic/amide H refined with riding coordinates:
 C14(H14), C8(H8), C16(H16), C10(H10)
2.d Idealised Me refined as rotating group:
 C35(H35A,H35B,H35C), C40(H40A,H40B,H40C), C36(H36A,H36B,H36C), C41(H41A,H41B,
 H41C), C37(H37A,H37B,H37C), C31(H31A,H31B,H31C), C39(H39A,H39B,H39C), C32(H32A,
 H32B,H32C), C30(H30A,H30B,H30C), C44(H44A,H44B,H44C), C42(H42A,H42B,H42C),
 C43(H43A,H43B,H43C)
;
_shelx_res_checksum              25396
_shelx_hkl_checksum              23607
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.322
_oxdiff_exptl_absorpt_empirical_full_min 0.814