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_1561004
_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         'C11 H21 O19 V6, C16 H36 P'
_chemical_formula_sum            'C27 H57 O19 P V6'
_chemical_formula_weight         1022.33
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-11-12
_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                 92.394(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.0905(4)
_cell_length_b                   16.6569(5)
_cell_length_c                   18.2558(5)
_cell_measurement_reflns_used    11892
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.4690
_cell_measurement_theta_min      4.3150
_cell_volume                     3977.2(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 0.992
_diffrn_measured_fraction_theta_max 0.973
_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    -21.00  22.00   0.50    3.81    --  -49.62  33.00 -62.00   86
  2  \w    -42.00 -12.00   0.50   15.25    --  -84.25  45.00  30.00   60
  3  \w    -42.00 -12.00   0.50   15.25    --  -84.25  45.00  90.00   60
  4  \w    -42.00 -12.00   0.50   15.25    --  -84.25  45.00 120.00   60
  5  \w    -75.00 -12.00   0.50   15.25    --  -84.25  61.00 -60.00  126
  6  \w   -121.00 -42.00   0.50    3.81    --  -49.62 -33.00 139.00  158
  7  \w   -121.00 -29.00   0.50    3.81    --  -49.62 -77.00 120.00  184
  8  \w     43.00 122.00   0.50    3.81    --   49.62  33.00 -62.00  158
  9  \w     98.00 178.00   0.50   15.25    --  105.75  33.00 -62.00  160
 10  \w     98.00 164.00   0.50   15.25    --  105.75  15.00  60.00  132
 11  \w     92.00 178.00   0.50   15.25    --  105.75 125.00-180.00  172
 12  \w     34.00  87.00   0.50   15.25    --  105.75 -61.00-150.00  106
 13  \w     34.00 109.00   0.50   15.25    --  105.75 -94.00 -90.00  150
 14  \w     34.00 109.00   0.50   15.25    --  105.75 -94.00 -30.00  150
 15  \w     34.00  87.00   0.50   15.25    --  105.75 -61.00 120.00  106
 16  \w     34.00  87.00   0.50   15.25    --  105.75 -61.00 150.00  106
 17  \w     34.00 109.00   0.50   15.25    --  105.75 -94.00  90.00  150
 18  \w     34.00  87.00   0.50   15.25    --  105.75 -61.00  90.00  106
 19  \w     34.00  87.00   0.50   15.25    --  105.75 -61.00   0.00  106
 20  \w     34.00  87.00   0.50   15.25    --  105.75 -61.00 -60.00  106
 21  \w     34.00  87.00   0.50   15.25    --  105.75 -61.00-180.00  106
 22  \w     29.00 122.00   0.50    3.81    --   49.62  77.00   0.00  186
 23  \w    -22.00  33.00   0.50    3.81    --   49.62 -33.00 139.00  110
 24  \w    -23.00   5.00   0.50    3.81    --   49.62 -19.00   0.00   56
 25  \w    -23.00   5.00   0.50    3.81    --   49.62 -19.00 -30.00   56
 26  \w   -121.00 -42.00   0.50    3.81    --  -49.62 -38.00-120.00  158
 27  \w   -156.00 -76.00   0.50   15.25    --  -84.25 -33.00 139.00  160
;
_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      -0.1096821000
_diffrn_orient_matrix_UB_12      -0.0310211000
_diffrn_orient_matrix_UB_13      -0.0154536000
_diffrn_orient_matrix_UB_21      0.0283497000
_diffrn_orient_matrix_UB_22      -0.0247212000
_diffrn_orient_matrix_UB_23      -0.0778530000
_diffrn_orient_matrix_UB_31      0.0323986000
_diffrn_orient_matrix_UB_32      -0.0835578000
_diffrn_orient_matrix_UB_33      0.0287774000
_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  0.0728
_diffrn_reflns_av_unetI/netI     0.0331
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            23900
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        74.504
_diffrn_reflns_theta_max         77.983
_diffrn_reflns_theta_min         4.298
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.383
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.35583
_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            red-orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.707
_exptl_crystal_description       plate
_exptl_crystal_F_000             2096
_exptl_crystal_size_max          0.146
_exptl_crystal_size_mid          0.082
_exptl_crystal_size_min          0.047
_refine_diff_density_max         0.549
_refine_diff_density_min         -0.366
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     328
_refine_ls_number_reflns         4147
_refine_ls_number_restraints     108
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0472
_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^)+(0.0913P)^2^+1.6444P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1379
_refine_ls_wR_factor_ref         0.1444
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3412
_reflns_number_total             4147
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nr09201k2.cif
_cod_data_source_block           mataf27
_cod_depositor_comments
'Adding full bibliography for 1561002--1561005.cif.'
_cod_original_cell_volume        3977.1(2)
_cod_database_code               1561004
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.594
_shelx_estimated_absorpt_t_min   0.265
_reflns_odcompleteness_completeness 99.15
_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
 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
C13 \\sim C22: within 8A with sigma of 0.005 and sigma for terminal atoms of
0.01 within 8A
3. Rigid body (RIGU) restrains
 C7, C8, C9, C10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C11, C12, C13, C14
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C15, C16, C17, C18
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C19, C20, C21, C22
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Same fragment restrains
{P1, C15, C16, C17, C18} sigma for 1-2: 0.02, 1-3: 0.04
{P1, C11, C12, C13, C14} sigma for 1-2: 0.02, 1-3: 0.04
{P1, C19, C20, C21, C22} sigma for 1-2: 0.02, 1-3: 0.04
as in
{P1, C7, C8, C9, C10}
5. Others
 Fixed Sof: C6(0.5) H6A(0.5) H6B(0.5) H6C(0.5) P1(0.5) C7(0.5) H7A(0.5)
 H7B(0.5) C8(0.5) H8A(0.5) H8B(0.5) C9(0.5) H9A(0.5) H9B(0.5) C10(0.5)
 H10A(0.5) H10B(0.5) H10C(0.5) C11(0.5) H11A(0.5) H11B(0.5) C12(0.5) H12A(0.5)
 H12B(0.5) C13(0.5) H13A(0.5) H13B(0.5) C14(0.5) H14A(0.5) H14B(0.5) H14C(0.5)
 C15(0.5) H15A(0.5) H15B(0.5) C16(0.5) H16A(0.5) H16B(0.5) C17(0.5) H17A(0.5)
 H17B(0.5) C18(0.5) H18A(0.5) H18B(0.5) H18C(0.5) C19(0.5) H19A(0.5) H19B(0.5)
 C20(0.5) H20A(0.5) H20B(0.5) C21(0.5) H21A(0.5) H21B(0.5) C22(0.5) H22A(0.5)
 H22B(0.5) H22C(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B),
 C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C15(H15A,H15B), C16(H16A,H16B),
  C17(H17A,H17B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B)
6.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C10(H10A,H10B,H10C), C14(H14A,H14B,H14C),
 C18(H18A,H18B,H18C), C22(H22A,H22B,H22C)
;
_shelx_res_checksum              75460
_shelx_hkl_checksum              38152
_olex2_submission_original_sample_id mataf27
_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 2.537
_oxdiff_exptl_absorpt_empirical_full_min 0.419