Chiral oxidovanadium(V) complexes with tridentate Schiff bases derived from S(+)-2-amino-1-propanol: Synthesis, structure, characterization and catalytic activity
Grzegorz Romanowski; Tadeusz Lis; Inorganica Chimica Acta 394 (2013) 627–634; doi:10.1016/j.ica.2012.09.030

data_1512807
_publ_section_title
;
 Chiral oxidovanadium(V) complexes with tridentate Schiff bases derived
 from S(+)-2-amino-1-propanol: Synthesis, structure, characterization and
 catalytic activity
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              627
_journal_page_last               634
_journal_paper_doi               10.1016/j.ica.2012.09.030
_journal_volume                  394
_journal_year                    2013
_chemical_absolute_configuration rm
_chemical_formula_sum            'C20 H20 N4 O11 V2'
_chemical_formula_weight         594.28
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 96.06(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.568(3)
_cell_length_b                   11.384(4)
_cell_length_c                   11.696(4)
_cell_measurement_reflns_used    10508
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76
_cell_measurement_theta_min      3
_cell_volume                     1134.4(7)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2003)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2003)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.934
_diffrn_measurement_device_type
'Xcalibur PX kappa-geometry diffractometer with CCD Onyx camera'
_diffrn_measurement_method       '\w and \f i.e. omega and phi scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.0294
_diffrn_reflns_av_sigmaI/netI    0.0304
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            10762
_diffrn_reflns_theta_full        67.50
_diffrn_reflns_theta_max         76.53
_diffrn_reflns_theta_min         3.80
_exptl_absorpt_coefficient_mu    7.554
_exptl_absorpt_correction_T_max  0.766
_exptl_absorpt_correction_T_min  0.266
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
CrysAlis RED (Oxford Diffraction, 2003)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.740
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             604
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.25
_refine_diff_density_min         -0.43
_refine_diff_density_rms         0.059
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.004(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     336
_refine_ls_number_reflns         4002
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0321
_refine_ls_R_factor_gt           0.0290
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.053P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0731
_refine_ls_wR_factor_ref         0.0743
_reflns_number_gt                3610
_reflns_number_total             4002
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2013-394-627-634.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      P21
_cod_database_code               1512807