Interactions of vanadium(iv) with amidoxime ligands: redox reactivity.
Parker, B. F.; Hohloch, S.; Pankhurst, J. R.; Zhang, Z.; Love, J. B.; Arnold, J.; Rao, L.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 5695–5702; doi:10.1039/c7dt04069e

data_7046004
_publ_section_title
;
 Interactions of vanadium(iv) with amidoxime ligands: redox reactivity.
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5695
_journal_page_last               5702
_journal_paper_doi               10.1039/c7dt04069e
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         '6(C5 H14 N4 2+) 2(V10 O28 6-) 11(H2 O)'
_chemical_formula_sum            'C30 H106 N24 O67 V20'
_chemical_formula_weight         2894.11
_chemical_name_common            'Glutaramidinium decavanadate'
_chemical_name_systematic
'tris(1,5-diaminopentane-1,5-diiminium) decavanadate'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-10-28 deposited with the CCDC.
2018-03-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.6232(16)
_cell_length_b                   37.606(3)
_cell_length_c                   13.3441(11)
_cell_measurement_reflns_used    9541
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.37
_cell_measurement_theta_min      2.23
_cell_volume                     9345.5(13)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2015 (Sheldrick 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0403
_diffrn_reflns_av_unetI/netI     0.0335
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            84022
_diffrn_reflns_point_group_measured_fraction_full 0.894
_diffrn_reflns_point_group_measured_fraction_max 0.883
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.427
_diffrn_reflns_theta_min         1.083
_diffrn_source                   'microfocus sealed tube'
_exptl_absorpt_coefficient_mu    2.014
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6357
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.057
_exptl_crystal_description       block
_exptl_crystal_F_000             5800
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Water'
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.303
_refine_diff_density_min         -0.655
_refine_diff_density_rms         0.104
_refine_ls_abs_structure_details
;
 Flack x determined using 5365 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.006(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         15244
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0390
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0473P)^2^+26.0651P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0952
_refine_ls_wR_factor_ref         0.0974
_reflns_Friedel_coverage         0.694
_reflns_Friedel_fraction_full    0.778
_reflns_Friedel_fraction_max     0.758
_reflns_number_gt                14183
_reflns_number_total             15244
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04069e2.cif
_cod_data_source_block           shelx
_cod_depositor_comments          'Adding full bibliography for 7046004.cif.'
_cod_original_cell_volume        9345.6(14)
_cod_database_code               7046004
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.752
_shelx_estimated_absorpt_t_max   0.906
_shelx_res_checksum              26269