Physicochemical implications of surface alkylation of high-valent, Lindqvist-type polyoxovanadate-alkoxide clusters.
Fertig, Alex A.; Rabbani, S. M. Gulam; Koch, Melissa D.; Brennessel, William W.; Miró, Pere; Matson, Ellen M.; Nanoscale 13 (2021) 6162–6173; doi:10.1039/d0nr09201k

data_1561002
_publ_section_title
;
 Physicochemical implications of surface alkylation of high-valent,
 Lindqvist-type polyoxovanadate-alkoxide clusters.
;
_journal_issue                   12
_journal_name_full               Nanoscale
_journal_page_first              6162
_journal_page_last               6173
_journal_paper_doi               10.1039/d0nr09201k
_journal_volume                  13
_journal_year                    2021
_chemical_formula_moiety
'C10 H18 N2 O23 V6, 1.526(C4 H10 O), 2(C16 H36 N)'
_chemical_formula_sum            'C48.1 H105.26 N4 O24.52 V6'
_chemical_formula_weight         1437.92
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-12-05
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2020.03.28 svn.rd84adfe8 for Rigaku Oxford Diffraction, GUI svn.r6032)
;
_audit_update_record
;
2020-12-30 deposited with the CCDC.	2021-03-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.990(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.6947(4)
_cell_length_b                   15.5293(5)
_cell_length_c                   18.1049(6)
_cell_measurement_reflns_used    10176
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      74.3410
_cell_measurement_theta_min      3.7290
_cell_volume                     3354.2(2)
_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      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.978
_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    -74.00  23.00   0.50    1.08    --  -49.37  86.00 -33.00  194
  2  \w    -30.00  22.00   0.50    1.08    --  -49.37  38.00  60.00  104
  3  \w    -21.00  74.00   0.50    1.08    --   49.37 -86.00-151.00  190
  4  \w     34.00 131.00   0.50    4.31    --  105.75 -86.00-151.00  194
  5  \w     50.00 107.00   0.50    4.31    --  105.75 -94.00-120.00  114
  6  \w     38.00  67.00   0.50    4.31    --  105.75 -61.00 -60.00   58
  7  \w     34.00  87.00   0.50    4.31    --  105.75 -61.00-120.00  106
  8  \w     34.00 109.00   0.50    4.31    --  105.75 -94.00-180.00  150
  9  \w     34.00  87.00   0.50    4.31    --  105.75 -61.00-150.00  106
 10  \w    124.00 151.00   0.50    4.31    --  105.75  15.00 -90.00   54
 11  \w     98.00 178.00   0.50    4.31    --  105.75  86.00 -33.00  160
 12  \w     98.00 164.00   0.50    4.31    --  105.75  15.00  60.00  132
 13  \w     98.00 163.00   0.50    4.31    --  105.75  15.00 150.00  130
 14  \w     92.00 178.00   0.50    4.31    --  105.75 125.00  90.00  172
 15  \w     92.00 178.00   0.50    4.31    --  105.75 125.00 150.00  172
 16  \w     85.00 178.00   0.50    4.31    --  105.75  77.00 -90.00  186
 17  \w     46.00 108.00   0.50    4.31    --  105.75 -94.00 120.00  124
 18  \w     34.00  87.00   0.50    4.31    --  105.75 -61.00 120.00  106
 19  \w     34.00 116.00   0.50    4.31    --  105.75-125.00 120.00  164
 20  \w     34.00  83.00   0.50    4.31    --  105.75 -94.00   0.00   98
 21  \w    -23.00   5.00   0.50    1.08    --   49.37 -19.00-150.00   56
 22  \w   -109.00 -12.00   0.50    4.31    --  -84.25  86.00 -33.00  194
 23  \w   -156.00 -76.00   0.50    4.31    --  -84.25 -86.00-151.00  160
 24  \w   -121.00 -70.00   0.50    1.08    --  -49.37-125.00 -60.00  102
 25  \w   -121.00 -70.00   0.50    1.08    --  -49.37-125.00  30.00  102
 26  \w   -121.00 -70.00   0.50    1.08    --  -49.37-125.00  90.00  102
;
_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      -0.1280227000
_diffrn_orient_matrix_UB_12      0.0030605000
_diffrn_orient_matrix_UB_13      -0.0414419000
_diffrn_orient_matrix_UB_21      -0.0038190000
_diffrn_orient_matrix_UB_22      0.0885977000
_diffrn_orient_matrix_UB_23      0.0371367000
_diffrn_orient_matrix_UB_31      0.0165059000
_diffrn_orient_matrix_UB_32      0.0446555000
_diffrn_orient_matrix_UB_33      -0.0713293000
_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  0.0853
_diffrn_reflns_av_unetI/netI     0.0422
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            41431
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        74.504
_diffrn_reflns_theta_max         78.169
_diffrn_reflns_theta_min         3.705
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.366
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.30167
_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            'dark green'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_description       block
_exptl_crystal_F_000             1512
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.182
_exptl_crystal_size_min          0.096
_refine_diff_density_max         0.904
_refine_diff_density_min         -0.653
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     422
_refine_ls_number_reflns         7044
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0757
_refine_ls_R_factor_gt           0.0597
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1109P)^2^+1.8371P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1691
_refine_ls_wR_factor_ref         0.1827
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5465
_reflns_number_total             7044
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nr09201k2.cif
_cod_data_source_block           mataf28
_cod_depositor_comments
'Adding full bibliography for 1561002--1561005.cif.'
_cod_original_formula_sum        'C48.10 H105.26 N4 O24.52 V6'
_cod_database_code               1561002
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.538
_shelx_estimated_absorpt_t_min   0.307
_reflns_odcompleteness_completeness 99.87
_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. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.2A with sigma of 0.02 and sigma
for terminal atoms of 0.04 within 1.2A
3. Same fragment restrains
{C18, C19', C20', C21'} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C18, C19, C20, C21}
4. Others
 Sof(H18C)=Sof(H18D)=Sof(C19')=Sof(H19C)=Sof(H19D)=Sof(C20')=Sof(H20C)=
 Sof(H20D)=Sof(C21')=Sof(H21D)=Sof(H21E)=Sof(H21F)=1-FVAR(1)
 Sof(H18A)=Sof(H18B)=Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(C20)=Sof(H20A)=Sof(H20B)=
 Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(H21C)=FVAR(1)
 Sof(O13)=Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(H22C)=Sof(C23)=Sof(H23A)=Sof(H23B)=
 Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C23(H23A,H23B), C24(H24A,H24B), C6(H6A,
 H6B), C7(H7A,H7B), C8(H8A,H8B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B),
  C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C18(H18A,H18B), C18(H18C,
 H18D), C19(H19A,H19B), C20(H20A,H20B), C19'(H19C,H19D), C20'(H20C,H20D)
5.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C22(H22A,H22B,H22C), C25(H25A,H25B,H25C), C9(H9A,H9B,H9C),
 C13(H13A,H13B,H13C), C17(H17A,H17B,H17C), C21(H21A,H21B,H21C), C21'(H21D,H21E,
 H21F)
;
_shelx_res_checksum              93699
_shelx_hkl_checksum              63946
_olex2_submission_original_sample_id mataf28
_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 2.548
_oxdiff_exptl_absorpt_empirical_full_min 0.463