Vanadyl sulfates: molecular structure, magnetism and electrochemical activity.
Ignaszak, Anna; Patterson, Nigel; Radtke, Mariusz; Elsegood, Mark R. J.; Frese, Josef W. A.; Lipman, Joah L. Z. F.; Yamato, Takehiko; Sanz, Sergio; Brechin, Euan K.; Prior, Timothy J.; Redshaw, Carl; Dalton transactions (Cambridge, England : 2003) 47 (2018) 15983–15993; doi:10.1039/c8dt03626h

data_7047863
_publ_section_title
;
 Vanadyl sulfates: molecular structure, magnetism and electrochemical
 activity.
;
_journal_issue                   44
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15983
_journal_page_last               15993
_journal_paper_doi               10.1039/c8dt03626h
_journal_volume                  47
_journal_year                    2018
_chemical_absolute_configuration ad
_chemical_formula_moiety         'O25 S4 V5 5-, 5(C6 H16 N 1+), H2 O'
_chemical_formula_sum            'C30 H82 N5 O26 S4 V5'
_chemical_formula_weight         1311.94
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-09-13 deposited with the CCDC.
2018-10-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.4436(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.2439(4)
_cell_length_b                   13.3679(4)
_cell_length_c                   31.3605(10)
_cell_measurement_reflns_used    24188
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.07
_cell_measurement_theta_min      2.18
_cell_volume                     5460.2(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX 2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX 2 CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0270
_diffrn_reflns_av_unetI/netI     0.0413
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            62632
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.239
_diffrn_reflns_theta_min         0.660
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.060
_exptl_absorpt_correction_T_max  0.901
_exptl_absorpt_correction_T_min  0.473
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2008/1, Sheldrick, G.M., (2008)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.596
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tablet
_exptl_crystal_F_000             2736
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichlormethane/toluene'
_exptl_crystal_size_max          0.830
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.911
_refine_diff_density_min         -0.602
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details
; 
 Flack x determined using 11479 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   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1479
_refine_ls_number_reflns         30874
_refine_ls_number_restraints     786
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0383
_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^)+(0.0520P)^2^+2.3635P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0947
_refine_ls_wR_factor_ref         0.0992
_reflns_Friedel_coverage         0.846
_reflns_Friedel_fraction_full    0.992
_reflns_Friedel_fraction_max     0.906
_reflns_number_gt                27570
_reflns_number_total             30874
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03626h2.cif
_cod_data_source_block           2_H2O
_cod_depositor_comments
'Adding full bibliography for 7047857--7047863.cif.'
_cod_database_code               7047863
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.473
_shelx_estimated_absorpt_t_max   0.901
_shelx_res_checksum              32016