Improved solubility of titanium-doped polyoxovanadate charge carriers for symmetric non-aqueous redox flow batteries.
Dagar, Mamta; Dissanyake, D. M. M. Mevan; Kesler, Daniel N.; Corr, Molly; McPherson, Joshua D.; Brennessel, William W.; McKone, James R.; Matson, Ellen M.; Dalton transactions (Cambridge, England : 2003) 53 (2023) 93–104; doi:10.1039/d3dt03642a

data_7714561
_publ_section_title
;
 Improved solubility of titanium-doped polyoxovanadate charge carriers for
 symmetric non-aqueous redox flow batteries.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              93
_journal_page_last               104
_journal_paper_doi               10.1039/d3dt03642a
_journal_volume                  53
_journal_year                    2023
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C17 H44 O20 Ti2 V4'
_chemical_formula_sum            'C17 H44 O20 Ti2 V4'
_chemical_formula_weight         868.08
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-10-07
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2020.03.28 svn.rd84adfe8 for Rigaku Oxford Diffraction, GUI svn.r6032)
;
_audit_update_record
;
2023-07-31 deposited with the CCDC.	2023-11-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.8039(2)
_cell_length_b                   16.2998(2)
_cell_length_c                   10.42640(10)
_cell_measurement_reflns_used    42086
_cell_measurement_temperature    99.98(10)
_cell_measurement_theta_max      76.2410
_cell_measurement_theta_min      3.5690
_cell_volume                     3195.69(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2015a)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.98(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -48.00  21.00   0.50    0.63    --  -49.75  50.00  61.00  138
  2  \w    -43.00 -18.00   0.50    2.53    --  -84.25  50.00  61.00   50
  3  \w   -101.00 -61.00   0.50    0.63    --  -49.75 -50.00 -85.00   80
  4  \w    -61.00 -33.00   0.50    0.63    --  -56.00 -81.00-108.83   56
  5  \w    -67.00 -42.00   0.50    0.63    --  -64.00 -79.00-139.47   50
  6  \w    -78.00 -45.00   0.50    2.53    --  -68.00 -83.00 -82.41   66
  7  \w    -74.00 -49.00   0.50    2.53    --  -72.00 -82.00 -45.80   50
  8  \w    -78.00 -49.00   0.50    2.53    --  -72.00 -82.00 -98.09   58
  9  \w    -79.00 -53.00   0.50    2.53    --  -76.00 -82.00-165.62   52
 10  \w    -83.00 -57.00   0.50    2.53    --  -80.00 -83.00-101.92   52
 11  \w    -86.00 -61.00   0.50    2.53    --  -84.25 -82.00-142.85   50
 12  \w    -88.00 -63.00   0.50    2.53    --  -84.25 -77.00-180.00   50
 13  \w    -89.00 -63.00   0.50    2.53    --  -84.25 -77.00-120.00   52
 14  \w    -91.00 -65.00   0.50    2.53    --  -84.25 -74.00-136.29   52
 15  \w    -96.00 -61.00   0.50    2.53    --  -84.25 -82.00 -90.29   70
 16  \w    -88.00 -63.00   0.50    2.53    --  -84.25 -77.00 -60.97   50
 17  \w    -81.00 -56.00   0.50    2.53    --  -76.00 -75.00 -14.81   50
 18  \w    -85.00 -55.00   0.50    2.53    --  -76.00 -77.00  11.81   60
 19  \w    -71.00 -45.00   0.50    0.63    --  -64.00 -72.00  71.95   52
 20  \w    -55.00 -29.00   0.50    0.63    --  -52.00 -82.00 127.79   52
 21  \w    -83.00 -38.00   0.50    0.63    --  -60.00 -81.00 112.32   90
 22  \w    -85.00 -60.00   0.50    2.53    --  -80.00 -74.00  25.07   50
 23  \w    -79.00 -53.00   0.50    2.53    --  -76.00 -82.00 -18.86   52
 24  \w    -90.00 -63.00   0.50    2.53    --  -84.25 -77.00   0.00   54
 25  \w    -89.00 -63.00   0.50    2.53    --  -84.25 -77.00  60.00   52
 26  \w    -86.00 -61.00   0.50    2.53    --  -84.25 -82.00  59.36   50
 27  \w    -87.00 -61.00   0.50    2.53    --  -84.25 -83.00  85.13   52
 28  \w    -87.00 -62.00   0.50    2.53    --  -84.25 -81.00 137.68   50
 29  \w    -89.00 -63.00   0.50    2.53    --  -84.25 -77.00 150.00   52
 30  \w    -87.00 -61.00   0.50    2.53    --  -84.25 -82.00 117.18   52
 31  \w    -88.00 -63.00   0.50    2.53    --  -84.25 -77.00  90.00   50
 32  \w    -93.00 -64.00   0.50    2.53    --  -84.25 -75.00  16.92   58
 33  \w    -92.00 -61.00   0.50    2.53    --  -84.25 -82.00 -25.50   62
 34  \w    -94.00 -65.00   0.50    2.53    --  -84.25 -74.00 -45.96   58
 35  \w   -121.00 -44.00   0.50    0.63    --  -49.75 -19.00  60.00  154
 36  \w      6.00  38.00   0.50    0.63    --   32.00  89.00 158.76   64
 37  \w     20.00  45.00   0.50    0.63    --   44.00  84.00 177.23   50
 38  \w     47.00  72.00   0.50    0.63    --   68.00  77.00 158.81   50
 39  \w     52.00  78.00   0.50    0.63    --   72.00  76.00 116.78   52
 40  \w     47.00 100.00   0.50    0.63    --   49.75  50.00  61.00  106
 41  \w     91.00 127.00   0.50    0.63    --   56.00  80.00  20.13   72
 42  \w     83.00 128.00   0.50    0.63    --   56.00  82.00 -65.63   90
 43  \w    143.00 168.00   0.50    2.53    --   96.00  78.00 -59.03   50
 44  \w    143.00 171.00   0.50    2.53    --  105.75  77.00 -30.00   56
 45  \w    142.00 177.00   0.50    2.53    --  105.75  77.00  30.00   70
 46  \w    136.00 161.00   0.50    2.53    --  105.75  50.00  61.00   50
 47  \w    139.00 172.00   0.50    2.53    --  105.75  77.00 120.00   66
 48  \w    143.00 173.00   0.50    2.53    --  105.75  77.00  90.00   60
 49  \w    151.00 176.00   0.50    2.53    --  105.75  77.00 150.00   50
 50  \w    123.00 158.00   0.50    2.53    --   92.00  83.00 138.36   70
 51  \w    114.00 139.00   0.50    0.63    --   68.00  77.00 158.81   50
 52  \w    123.00 166.00   0.50    2.53    --  105.75  61.00 120.00   86
 53  \w    126.00 160.00   0.50    2.53    --   96.00  74.00  34.84   68
 54  \w    125.00 151.00   0.50    2.53    --  105.75  61.00  30.00   52
 55  \w    126.00 178.00   0.50    2.53    --  105.75  15.00  30.00  104
 56  \w    123.00 152.00   0.50    2.53    --  105.75  61.00 -60.00   58
 57  \w    124.00 177.00   0.50    2.53    --  105.75  77.00-120.00  106
 58  \w    141.00 174.00   0.50    2.53    --  105.75  77.00-150.00   66
 59  \w     99.00 125.00   0.50    0.63    --   60.00  81.00-162.85   52
 60  \w     69.00  94.00   0.50    2.53    --   88.00  74.00-172.08   50
 61  \w     93.00 172.00   0.50    2.53    --  105.75  61.00-180.00  158
 62  \w     94.00 167.00   0.50    2.53    --  105.75  61.00 -30.00  146
 63  \w     86.00 138.00   0.50    2.53    --  105.75  77.00  30.00  104
 64  \w     92.00 118.00   0.50    2.53    --  105.75  61.00 120.00   52
 65  \w     92.00 143.00   0.50    2.53    --  105.75  61.00 150.00  102
 66  \w     86.00 146.00   0.50    2.53    --  105.75  77.00 150.00  120
 67  \w     92.00 158.00   0.50    2.53    --  105.75  61.00  90.00  132
 68  \w     91.00 134.00   0.50    2.53    --  105.75  77.00 -30.00   86
 69  \w     94.00 120.00   0.50    2.53    --  105.75  61.00 -60.00   52
 70  \w     92.00 178.00   0.50    2.53    --  105.75  61.00 -90.00  172
 71  \w     85.00 142.00   0.50    2.53    --  105.75  77.00 -90.00  114
 72  \w     87.00 117.00   0.50    2.53    --  105.75  77.00-150.00   60
 73  \w     92.00 169.00   0.50    2.53    --  105.75  61.00-150.00  154
 74  \w     93.00 162.00   0.50    2.53    --  105.75  61.00-120.00  138
 75  \w     92.00 117.00   0.50    2.53    --  105.75  61.00  30.00   50
 76  \w     93.00 161.00   0.50    2.53    --  105.75  61.00  60.00  136
 77  \w     78.00 104.00   0.50    2.53    --   96.00  74.00  34.84   52
 78  \w     85.00 155.00   0.50    2.53    --  105.75  77.00   0.00  140
 79  \w     85.00 132.00   0.50    2.53    --  105.75  77.00 120.00   94
 80  \w     85.00 177.00   0.50    2.53    --  105.75  77.00  60.00  184
 81  \w     85.00 177.00   0.50    2.53    --  105.75  77.00 -60.00  184
 82  \w     86.00 112.00   0.50    2.53    --  105.75  77.00-120.00   52
 83  \w     85.00 144.00   0.50    2.53    --  105.75  77.00-180.00  118
 84  \w     75.00 101.00   0.50    2.53    --   96.00  78.00 -59.03   52
 85  \w     34.00  61.00   0.50    0.63    --   56.00  80.00  20.13   54
 86  \w     39.00  67.00   0.50    0.63    --   60.00  77.00 -37.03   56
 87  \w     42.00  74.00   0.50    0.63    --   64.00  80.00 -24.33   64
 88  \w     33.00  75.00   0.50    0.63    --   56.00  82.00 -65.63   84
 89  \w     18.00  46.00   0.50    0.63    --   40.00  85.00-108.06   56
 90  \w     20.00  45.00   0.50    0.63    --   44.00  85.00-154.51   50
 91  \w     38.00  69.00   0.50    0.63    --   60.00  81.00-162.85   62
 92  \w     18.00  43.00   0.50    0.63    --   44.00  88.00 -35.15   50
 93  \w      6.00  31.00   0.50    0.63    --   36.00  96.00  38.96   50
 94  \w     13.00  38.00   0.50    0.63    --   40.00  91.00  95.34   50
 95  \w     34.00  59.00   0.50    0.63    --   56.00  81.00  90.49   50
 96  \w     37.00  63.00   0.50    0.63    --   60.00  82.00  40.92   52
 97  \w     38.00  64.00   0.50    0.63    --   60.00  80.00  69.03   52
 98  \w     69.00  95.00   0.50    2.53    --   92.00  83.00 138.36   52
 99  \w     85.00 138.00   0.50    2.53    --  105.75  77.00  90.00  106
100  \w     34.00  59.00   0.50    2.53    --  105.75 -50.00 -85.00   50
101  \w     78.00 108.00   0.50    2.53    --  105.75 -94.00 -30.00   60
102  \w     77.00 105.00   0.50    2.53    --  105.75 -94.00 -60.00   56
103  \w     76.00 116.00   0.50    2.53    --  105.75-125.00 -90.00   80
104  \w     76.00 114.00   0.50    2.53    --  105.75-125.00-120.00   76
105  \w     73.00  99.00   0.50    2.53    --  105.75 -94.00 -90.00   52
106  \w     47.00  73.00   0.50    2.53    --  105.75-125.00 -90.00   52
107  \w     45.00  71.00   0.50    2.53    --  105.75 -94.00 -30.00   52
108  \w     47.00 116.00   0.50    2.53    --  105.75-125.00 -60.00  138
109  \w     56.00  81.00   0.50    2.53    --  105.75 -61.00  30.00   50
110  \w     48.00  99.00   0.50    2.53    --  105.75 -94.00  90.00  102
111  \w     65.00 115.00   0.50    2.53    --  105.75-125.00  60.00  100
112  \w     34.00 127.00   0.50    2.53    --  105.75 -77.00  60.00  186
113  \w     38.00  64.00   0.50    2.53    --  105.75-125.00  60.00   52
114  \w     36.00 116.00   0.50    2.53    --  105.75-125.00  90.00  160
115  \w     35.00  73.00   0.50    2.53    --  105.75 -94.00 -60.00   76
116  \w     38.00  72.00   0.50    2.53    --  105.75-125.00-120.00   68
117  \w     60.00 116.00   0.50    2.53    --  105.75-125.00-180.00  112
118  \w     35.00  61.00   0.50    2.53    --  105.75 -61.00-150.00   52
119  \w     37.00  81.00   0.50    2.53    --  105.75 -61.00-180.00   88
120  \w     40.00 116.00   0.50    2.53    --  105.75-125.00-150.00  152
121  \w     34.00  73.00   0.50    2.53    --  105.75 -61.00 -30.00   78
122  \w     34.00  78.00   0.50    2.53    --  105.75 -61.00  90.00   88
123  \w    -19.00  58.00   0.50    0.63    --   49.75 -50.00 -85.00  154
124  \w    -16.00  13.00   0.50    0.63    --   16.00 100.00-114.69   58
125  \w    -38.00 -12.00   0.50    0.63    --    8.00 127.00 -28.48   52
126  \w    -39.00  -9.00   0.50    0.63    --    4.00 123.00  62.74   60
127  \w    -25.00   0.00   0.50    0.63    --   12.00 109.00 157.34   50
128  \w   -139.00-114.00   0.50    2.53    --  -84.25 -50.00 -85.00   50
129  \w   -111.00 -85.00   0.50    0.63    --  -56.00 -81.00-108.83   52
130  \w   -148.00-108.00   0.50    2.53    --  -76.00 -77.00  11.81   80
131  \w   -150.00-124.00   0.50    2.53    --  -84.25 -82.00  59.36   52
132  \w   -150.00-125.00   0.50    2.53    --  -84.25 -81.00 137.68   50
133  \w   -154.00-120.00   0.50    2.53    --  -84.25 -74.00 -45.96   68
134  \w   -151.00-126.00   0.50    2.53    --  -84.25 -77.00 -60.97   50
135  \w    -67.00 -15.00   0.50    2.53    --  -84.25  61.00-180.00  104
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0491898000
_diffrn_orient_matrix_UB_12      0.0016330000
_diffrn_orient_matrix_UB_13      -0.1180995000
_diffrn_orient_matrix_UB_21      0.0104553000
_diffrn_orient_matrix_UB_22      0.0934993000
_diffrn_orient_matrix_UB_23      -0.0109081000
_diffrn_orient_matrix_UB_31      0.0646706000
_diffrn_orient_matrix_UB_32      -0.0137562000
_diffrn_orient_matrix_UB_33      -0.0881241000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0943
_diffrn_reflns_av_unetI/netI     0.0298
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            122147
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        74.504
_diffrn_reflns_theta_max         79.150
_diffrn_reflns_theta_min         3.589
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    14.199
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.05775
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange-brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.804
_exptl_crystal_description       plate
_exptl_crystal_F_000             1768
_exptl_crystal_size_max          0.222
_exptl_crystal_size_mid          0.078
_exptl_crystal_size_min          0.046
_refine_diff_density_max         1.246
_refine_diff_density_min         -0.706
_refine_diff_density_rms         0.119
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.360(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     401
_refine_ls_number_reflns         6812
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0547
_refine_ls_R_factor_gt           0.0510
_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^)+(0.0918P)^2^+4.4272P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1377
_refine_ls_wR_factor_ref         0.1433
_reflns_Friedel_coverage         0.883
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.978
_reflns_number_gt                6387
_reflns_number_total             6812
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03642a2.cif
_cod_data_source_block           matmd09
_cod_depositor_comments          'Adding full bibliography for 7714561.cif.'
_cod_database_code               7714561
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         V4Ti2O21C17H36
_shelx_estimated_absorpt_t_max   0.561
_shelx_estimated_absorpt_t_min   0.145
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.640(11)
 0.360(11)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C16(H16A,H16B)
3.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,
 H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C),
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C17(H17A,H17B,H17C)
;
_shelx_res_checksum              72477
_olex2_submission_original_sample_id matmd09
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 12.400
_oxdiff_exptl_absorpt_empirical_full_min 0.368