Racemic vanadium(V) oxo monoperoxo complexes with two achiral bidentate heteroligands. Synthesis, characterization, crystal structure and stereochemistry of K[VO(O2)(ox)(bpy)]·3H2O and Pr4N[VO(O2)(ox)(phen)]
Jozef Tatiersky; Peter Schwendt; Jaromír Marek; Michal Sivák; New J. Chem. 28 (2004) 127–133; doi:10.1039/b306090j

data_7050131
_publ_section_title
;
 Racemic vanadium(V) oxo monoperoxo complexes with two achiral
 bidentate heteroligands. Synthesis, characterization, crystal
 structure and stereochemistry of K[VO(O2)(ox)(bpy)]&#x00B7;3H2O and
 Pr4N[VO(O2)(ox)(phen)]
;
_journal_issue                   1
_journal_name_full               'New J. Chem.'
_journal_page_first              127
_journal_page_last               133
_journal_paper_doi               10.1039/b306090j
_journal_volume                  28
_journal_year                    2004
_chemical_formula_sum            'C26 H36 N3 O7 V'
_chemical_formula_weight         553.52
_space_group_IT_number           15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 112.005(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   29.5519(12)
_cell_length_b                   10.0503(5)
_cell_length_c                   19.3160(9)
_cell_measurement_temperature    120(2)
_cell_volume                     5319.0(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0401
_diffrn_reflns_av_sigmaI/netI    0.0399
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            14505
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.33
_exptl_absorpt_coefficient_mu    0.422
_exptl_absorpt_correction_T_max  0.9590
_exptl_absorpt_correction_T_min  0.9203
_exptl_crystal_density_diffrn    1.382
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2336
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.810
_refine_diff_density_min         -0.298
_refine_diff_density_rms         0.051
_refine_ls_extinction_coef       0.00017(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     479
_refine_ls_number_reflns         4654
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0576
_refine_ls_R_factor_gt           0.0417
_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^)+(0.0500P)^2^+7.5000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0954
_refine_ls_wR_factor_ref         0.1021
_reflns_number_gt                3811
_reflns_number_total             4654
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b306090j.txt
_cod_data_source_block           fp_a
_cod_database_code               7050131