Probing chirality of oxidovanadium(V) centers in complexes with tridentate sugar Schiff-base ligands: solid-state and solution behavior
Mohammadnezhad, Gholamhossein; Akintola, Oluseun; Buchholz, Axel; Görls, Helmar; Plass, Winfried; New Journal of Chemistry 43 (2019) 17735–17745; doi:10.1039/C9NJ02881A

data_7058639
_publ_section_title
;
 Probing chirality of oxidovanadium(V) centers in complexes with
 tridentate sugar Schiff-base ligands: solid-state and solution behavior
;
_journal_issue                   45
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              17735
_journal_page_last               17745
_journal_paper_doi               10.1039/C9NJ02881A
_journal_volume                  43
_journal_year                    2019
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C29 H31 N2 O11 V'
_chemical_formula_sum            'C29 H31 N2 O11 V'
_chemical_formula_weight         634.50
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-06-03 deposited with the CCDC.    2019-07-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.008(2)
_cell_angle_gamma                90
_cell_formula_units_Z            6
_cell_length_a                   10.1800(4)
_cell_length_b                   35.4503(15)
_cell_length_c                   13.1580(5)
_cell_measurement_reflns_used    47062
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      27.483
_cell_measurement_theta_min      1.723
_cell_volume                     4748.5(3)
_computing_cell_refinement       DENZO
_computing_data_collection       COLLECT
_computing_data_reduction        DENZO
_computing_molecular_graphics    SHELXTL/PC
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'phi- + omega-scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0378
_diffrn_reflns_av_unetI/netI     0.0594
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            47062
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_min         1.723
_exptl_absorpt_coefficient_mu    0.373
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6054
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker-AXS, 2002'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.331
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1980
_exptl_crystal_size_max          0.102
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.088
_refine_diff_density_max         0.588
_refine_diff_density_min         -0.464
_refine_diff_density_rms         0.074
_refine_ls_abs_structure_details
;
 Flack x determined using 6246 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.005(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1169
_refine_ls_number_reflns         19581
_refine_ls_number_restraints     523
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0746
_refine_ls_R_factor_gt           0.0591
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0422P)^2^+7.1121P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1241
_refine_ls_wR_factor_ref         0.1361
_reflns_Friedel_coverage         0.779
_reflns_Friedel_fraction_full    0.827
_reflns_Friedel_fraction_max     0.800
_reflns_number_gt                17051
_reflns_number_total             19581
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj02881a2.cif
_cod_data_source_block           FO4336
_cod_database_code               7058639
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.963
_shelx_estimated_absorpt_t_max   0.968
_platon_squeeze_void_probe_radius 1.20