Racemic monoperoxovanadium(V) complexes with achiral OO and ON donor set heteroligands: synthesis, crystal structure and stereochemistry of [NH3(CH2)2NH3][VO(O2)(ox)(pic)].2H2O and [NH3(CH2)2NH3][VO(O2)(ox)(pca)].
Tatiersky, Jozef; Schwendt, Peter; Sivák, Michal; Marek, Jaromír; Dalton transactions (Cambridge, England : 2003)  (2005) 2305–2311; doi:10.1039/b504211a

data_7008550
_publ_section_title
;
 Racemic monoperoxovanadium(V) complexes with achiral OO and ON donor
 set heteroligands: synthesis, crystal structure and stereochemistry of
 [NH3(CH2)2NH3][VO(O2)(ox)(pic)].2H2O and
 [NH3(CH2)2NH3][VO(O2)(ox)(pca)].
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2305
_journal_page_last               2311
_journal_paper_doi               10.1039/b504211a
_journal_year                    2005
_chemical_formula_moiety         'C7 H3 N2 O9 V, C2 H10 N2 '
_chemical_formula_sum            'C9 H13 N4 O9 V'
_chemical_formula_weight         372.17
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 98.12(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.635(2)
_cell_length_b                   9.938(2)
_cell_length_c                   12.829(3)
_cell_measurement_reflns_used    2445
_cell_measurement_temperature    120(2)
_cell_volume                     1342.3(5)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction)'
_computing_data_reduction        'CrysAlis RED'
_computing_molecular_graphics    'ORTEP-III (Johnson & Burnett, 1996)'
_computing_publication_material
;
SHELXL-97, PARST (Nardelli, 1995)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 16.3
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Kuma KM4 + CCD'
_diffrn_measurement_method       'rotation method, \w--scan'
_diffrn_radiation_monochromator  'Enhance (Oxford Diffraction)'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0316
_diffrn_reflns_av_sigmaI/netI    0.0278
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7935
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.81
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.799
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.842
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.485
_refine_diff_density_min         -0.310
_refine_diff_density_rms         0.056
_refine_ls_extinction_coef       0.0034(8)
_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   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         2347
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_gt           0.0308
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0315P)^2^+1.5000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0696
_refine_ls_wR_factor_ref         0.0731
_reflns_number_gt                2094
_reflns_number_total             2347
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b504211a.txt
_cod_data_source_block           fp3
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7008550