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_7047857
_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_formula_moiety         'H4 O24 S4 V4 4-, 4(N C8 H20) 1+, 0.5(O H2)'
_chemical_formula_sum            'C32 H85 N4 O24.5 S4 V4'
_chemical_formula_weight         1250.03
_chemical_properties_physical
'Crystals lost solvent and crmbled within 2 hours on the microscope slide under inert oil'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 90.541(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.424(6)
_cell_length_b                   11.429(3)
_cell_length_c                   21.431(6)
_cell_measurement_reflns_used    980
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      18.21
_cell_measurement_theta_min      2.24
_cell_volume                     5247(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1539
_diffrn_reflns_av_unetI/netI     0.1452
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            23195
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.495
_diffrn_reflns_theta_min         1.901
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.932
_exptl_absorpt_correction_T_max  0.973
_exptl_absorpt_correction_T_min  0.807
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2009/1, Sheldrick, G.M., (2009)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.582
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2628
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile'
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.728
_refine_diff_density_min         -0.643
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     328
_refine_ls_number_reflns         5418
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.1483
_refine_ls_R_factor_gt           0.0711
_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^)+(0.0773P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1619
_refine_ls_wR_factor_ref         0.2000
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2805
_reflns_number_total             5418
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03626h2.cif
_cod_data_source_block           1_half_H2O
_cod_depositor_comments
'Adding full bibliography for 7047857--7047863.cif.'
_cod_original_formula_sum        'C32 H85 N4 O24.50 S4 V4'
_cod_database_code               7047857
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.807
_shelx_estimated_absorpt_t_max   0.973
_shelx_res_checksum              98251