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_7047858
_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         'C H8 O27 S4 V6 1-, 2(C8 H20 N 1+), C2 H3 N'
_chemical_formula_sum            'C19 H31 N3 O28 S4 V6'
_chemical_formula_weight         1183.35
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2018-10-12 deposited with the CCDC.
2018-10-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.2257(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.3206(8)
_cell_length_b                   19.3232(13)
_cell_length_c                   11.4459(8)
_cell_measurement_reflns_used    9359
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.74
_cell_measurement_theta_min      2.73
_cell_volume                     2415.9(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-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX 2 CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6939
_diffrn_reflns_av_R_equivalents  0.0466
_diffrn_reflns_av_unetI/netI     0.0343
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            38192
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        24.604
_diffrn_reflns_theta_max         26.782
_diffrn_reflns_theta_min         1.800
_diffrn_source                   'Daresbury SRS station 9.8'
_exptl_absorpt_coefficient_mu    1.271
_exptl_absorpt_correction_T_max  0.975
_exptl_absorpt_correction_T_min  0.916
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS v2008/2, Sheldrick, G.M., (2008)'
_exptl_crystal_colour            'pale blue'
_exptl_crystal_density_diffrn    1.627
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1184
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitril'
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.178
_refine_diff_density_min         -0.920
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     411
_refine_ls_number_reflns         5670
_refine_ls_number_restraints     660
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0599
_refine_ls_R_factor_gt           0.0502
_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^)+(0.1035P)^2^+2.9927P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1569
_refine_ls_wR_factor_ref         0.1662
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4771
_reflns_number_total             5670
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03626h2.cif
_cod_data_source_block           3dotMeCN
_cod_depositor_comments
'Adding full bibliography for 7047857--7047863.cif.'
_cod_database_code               7047858
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.916
_shelx_estimated_absorpt_t_max   0.975
_shelx_res_checksum              37643