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_7047861
_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         'C88 H109 O10 V 2-, 2(C6 H16 N 1+), 4(C2 H3 N)'
_chemical_formula_sum            'C108 H153 N6 O10 V'
_chemical_formula_weight         1746.29
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2017-09-13 deposited with the CCDC.
2018-10-22 downloaded from the CCDC.
;
_cell_angle_alpha                101.228(7)
_cell_angle_beta                 105.150(7)
_cell_angle_gamma                105.573(7)
_cell_formula_units_Z            2
_cell_length_a                   16.7286(7)
_cell_length_b                   18.2453(8)
_cell_length_c                   18.7113(13)
_cell_measurement_reflns_used    36379
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.1
_cell_measurement_theta_min      3.0
_cell_volume                     5090.2(6)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.0 r13 (Rigaku, 2011)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r13 (Rigaku, 2011)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.0 r13 (Rigaku, 2011)
;
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device
;
AFC12 (Right): Kappa 3 circle
;
_diffrn_measurement_device_type
;
Rigaku Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support Mitegen
_diffrn_radiation_monochromator  'confocal mirrors'
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0745
_diffrn_reflns_av_unetI/netI     0.1027
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            55764
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.026
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_min         3.021
_exptl_absorpt_coefficient_mu    0.156
_exptl_absorpt_correction_T_max  0.994
_exptl_absorpt_correction_T_min  0.980
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.139
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tablet
_exptl_crystal_F_000             1892
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile'
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.753
_refine_diff_density_min         -0.594
_refine_diff_density_rms         0.067
_refine_ls_extinction_coef       0.0023(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1222
_refine_ls_number_reflns         17887
_refine_ls_number_restraints     248
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.1460
_refine_ls_R_factor_gt           0.0855
_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^)+(0.1082P)^2^+4.1350P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2060
_refine_ls_wR_factor_ref         0.2372
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10295
_reflns_number_total             17887
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03626h2.cif
_cod_data_source_block           5_4MeCN
_cod_depositor_comments
'Adding full bibliography for 7047857--7047863.cif.'
_cod_original_cell_volume        5090.1(5)
_cod_database_code               7047861
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.980
_shelx_estimated_absorpt_t_max   0.994
_shelx_res_checksum              31960