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_7050132
_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            'C12 H14 K N2 O10 V'
_chemical_formula_weight         436.29
_space_group_IT_number           14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 97.606(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.6777(5)
_cell_length_b                   13.8879(6)
_cell_length_c                   12.7353(6)
_cell_measurement_temperature    150(2)
_cell_volume                     1696.60(14)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_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  0.0248
_diffrn_reflns_av_sigmaI/netI    0.0196
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9593
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.62
_exptl_absorpt_coefficient_mu    0.887
_exptl_crystal_density_diffrn    1.708
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.275
_refine_diff_density_min         -0.319
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.004
_refine_ls_goodness_of_fit_obs   1.038
_refine_ls_matrix_type           full
_refine_ls_number_parameters     291
_refine_ls_number_reflns         2906
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.995
_refine_ls_restrained_S_obs      1.038
_refine_ls_R_factor_all          0.0301
_refine_ls_R_factor_obs          0.0245
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+1.5000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0634
_refine_ls_wR_factor_obs         0.0615
_reflns_number_observed          2603
_reflns_number_total             2968
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b306090j.txt
_cod_data_source_block           fp
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+1.5000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+1.5000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               7050132