Surface functionalization of polyoxovanadium clusters: Generation of highly soluble charge carriers for nonaqueous energy storage
VanGelder, Lauren E.; Pratt III, Harry D; Anderson, Travis M.; Matson, Ellen; Chemical Communications  (2019) –; doi:10.1039/C9CC05380H

data_7124205
_publ_section_title
;
 Surface functionalization of polyoxovanadium clusters: Generation of
 highly soluble charge carriers for nonaqueous energy storage
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC05380H
_journal_year                    2019
_chemical_formula_moiety         'C36 H84 O31 V6, 2(C16 H36 N)'
_chemical_formula_sum            'C68 H156 N2 O31 V6'
_chemical_formula_weight         1803.58
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2018-09-05
_audit_creation_method
;
Olex2 1.2-ac3
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2019-04-03 deposited with the CCDC.    2019-09-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.4030(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.12380(10)
_cell_length_b                   17.5194(2)
_cell_length_c                   17.40260(10)
_cell_measurement_reflns_used    22911
_cell_measurement_temperature    222.99(10)
_cell_measurement_theta_max      77.2330
_cell_measurement_theta_min      3.5700
_cell_volume                     4572.56(7)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015b)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015a)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      222.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.982
_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    -46.00  23.00   0.50    0.42    --  -49.75  19.00  90.00  138
  2  \w    -49.00 -24.00   0.50    1.67    --  -84.25 108.00 -63.00   50
  3  \w    -85.00   0.00   0.50    0.42    --  -49.75 108.00 -63.00  170
  4  \w    -98.00 -71.00   0.50    0.42    --  -49.75-125.00 -30.00   54
  5  \w   -120.00 -71.00   0.50    0.42    --  -49.75-125.00   0.00   98
  6  \w   -121.00 -77.00   0.50    0.42    --  -49.75-125.00 -90.00   88
  7  \w   -117.00 -80.00   0.50    1.67    --  -84.25-108.00-160.00   74
  8  \w    -37.00 -11.00   0.50    0.42    --  -49.75  19.00-180.00   52
  9  \w     20.00  57.00   0.50    0.42    --   49.75-108.00-160.00   74
 10  \w     43.00 111.00   0.50    1.67    --  105.75-108.00-160.00  136
 11  \w     77.00 120.00   0.50    1.67    --  105.75 -77.00-150.00   86
 12  \w     86.00 112.00   0.50    1.67    --  105.75 -61.00-120.00   52
 13  \w     73.00  99.00   0.50    1.67    --  105.75-125.00-180.00   52
 14  \w     90.00 116.00   0.50    1.67    --  105.75-125.00 -90.00   52
 15  \w     77.00 109.00   0.50    1.67    --  105.75 -94.00   0.00   64
 16  \w     84.00 126.00   0.50    1.67    --  105.75 -77.00  60.00   84
 17  \w     44.00  89.00   0.50    1.67    --  105.75 -45.00  30.00   90
 18  \w     34.00  72.00   0.50    1.67    --  105.75 -30.00   0.00   76
 19  \w     42.00  72.00   0.50    1.67    --  105.75 -30.00  30.00   60
 20  \w     33.00  58.00   0.50    1.67    --  105.75 -15.00  30.00   50
 21  \w     39.00  80.00   0.50    1.67    --  105.75 -15.00  60.00   82
 22  \w     38.00  67.00   0.50    1.67    --  105.75 -30.00  60.00   58
 23  \w     34.00  72.00   0.50    1.67    --  105.75 -15.00 120.00   76
 24  \w     35.00  70.00   0.50    1.67    --  105.75 -30.00 150.00   70
 25  \w     41.00  96.00   0.50    1.67    --  105.75 -94.00 -30.00  110
 26  \w     40.00 109.00   0.50    1.67    --  105.75 -94.00-120.00  138
 27  \w     34.00  72.00   0.50    1.67    --  105.75 -30.00-150.00   76
 28  \w     37.00  78.00   0.50    1.67    --  105.75 -15.00-120.00   82
 29  \w     35.00  62.00   0.50    1.67    --  105.75 -61.00-120.00   54
 30  \w     38.00  72.00   0.50    1.67    --  105.75 -30.00 -90.00   68
 31  \w     39.00  69.00   0.50    1.67    --  105.75 -30.00-120.00   60
 32  \w     33.00  58.00   0.50    1.67    --  105.75 -15.00 -90.00   50
 33  \w     36.00  62.00   0.50    1.67    --  105.75-125.00 -90.00   52
 34  \w    114.00 139.00   0.50    1.67    --  105.75 108.00 -63.00   50
;
_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      -0.0944833000
_diffrn_orient_matrix_UB_12      0.0314697000
_diffrn_orient_matrix_UB_13      0.0036052000
_diffrn_orient_matrix_UB_21      0.0394631000
_diffrn_orient_matrix_UB_22      0.0796289000
_diffrn_orient_matrix_UB_23      0.0203694000
_diffrn_orient_matrix_UB_31      -0.0082807000
_diffrn_orient_matrix_UB_32      0.0200305000
_diffrn_orient_matrix_UB_33      -0.0868340000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_av_unetI/netI     0.0284
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            45341
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        74.504
_diffrn_reflns_theta_max         77.922
_diffrn_reflns_theta_min         3.595
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.554
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80209
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue-green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.310
_exptl_crystal_description       needle
_exptl_crystal_F_000             1928
_exptl_crystal_size_max          0.134
_exptl_crystal_size_mid          0.111
_exptl_crystal_size_min          0.095
_refine_diff_density_max         0.469
_refine_diff_density_min         -0.403
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     508
_refine_ls_number_reflns         9586
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_gt           0.0385
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0565P)^2^+1.7695P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1027
_refine_ls_wR_factor_ref         0.1065
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8319
_reflns_number_total             9586
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc05380h2.cif
_cod_data_source_block           matlv29
_cod_database_code               7124205
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         V6O37C68H156N2
_shelx_estimated_absorpt_t_max   0.620
_shelx_estimated_absorpt_t_min   0.523
_reflns_odcompleteness_completeness 99.64
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{C20, C20'}
3. Uiso/Uaniso restraints and constraints
C21 \\sim C22: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C20) = Uanis(C20')
Uanis(C21) = Uanis(C21')
4. Same fragment restrains
{C20, C21, C22} sigma for 1-2: 0.02, 1-3: 0.04
as
{C20', C21', C22'}
5. Others
 Sof(H19C)=Sof(H19D)=Sof(C20')=Sof(H20C)=Sof(H20D)=Sof(C21')=Sof(H21C)=
 Sof(H21D)=Sof(C22')=Sof(H22D)=Sof(H22E)=Sof(H22F)=1-FVAR(1)
 Sof(H19A)=Sof(H19B)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(C21)=Sof(H21A)=Sof(H21B)=
 Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(H22C)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C4(H4A,H4B), C5(H5A,H5B), C7(H7A,H7B), C8(H8A,H8B),
 C10(H10A,H10B), C11(H11A,H11B), C13(H13A,H13B), C14(H14A,H14B), C16(H16A,H16B),
  C17(H17A,H17B), C19(H19A,H19B), C19(H19C,H19D), C20(H20A,H20B), C21(H21A,
 H21B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B), C27(H27A,H27B),
 C28(H28A,H28B), C29(H29A,H29B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B),
  C20'(H20C,H20D), C21'(H21C,H21D)
6.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C6(H6A,H6B,H6C), C9(H9A,H9B,H9C), C12(H12A,H12B,H12C),
 C15(H15A,H15B,H15C), C18(H18A,H18B,H18C), C22(H22A,H22B,H22C), C26(H26A,H26B,
 H26C), C30(H30A,H30B,H30C), C34(H34A,H34B,H34C), C22'(H22D,H22E,H22F)
;
_shelx_res_checksum              48928
_olex2_submission_original_sample_id matlv29
_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 1.315
_oxdiff_exptl_absorpt_empirical_full_min 0.798