Iso- and hetero-polyoxovanadium glycolates [VIV6O<sub>6</sub>(glyc)<sub>6</sub>M<sup>III</sup>(OH)<sub>6</sub>]<sup>3-</sup> (M = V, Cr, Fe, and Al) encapsulating metal hydroxides.
Jin, Wan-Ting; Xie, Zhen-Lang; Su, Xing; Gao, Chuan-Hua; Hu, Jing; Zhou, Zhao-Hui; Dalton transactions (Cambridge, England : 2003) 53 (2024) 18711–18719; doi:10.1039/d4dt02370f

data_7717255
_publ_section_title
;
 Iso- and hetero-polyoxovanadium glycolates
 [VIV6O<sub>6</sub>(glyc)<sub>6</sub>M<sup>III</sup>(OH)<sub>6</sub>]<sup>3-</sup>
 (M = V, Cr, Fe, and Al) encapsulating metal hydroxides.
;
_journal_issue                   46
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              18711
_journal_page_last               18719
_journal_paper_doi               10.1039/d4dt02370f
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety
'C12 H18 Cr O30 V6, 2(O4 S), 2(H4 N), 6(H2 O), 0.833(N6)'
_chemical_formula_sum            'C12 H38 Cr N7 O44 S2 V6'
_chemical_formula_weight         1406.25
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-08-15
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-08-15 deposited with the CCDC.	2024-10-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   11.4407(4)
_cell_length_b                   11.4407(4)
_cell_length_c                   31.3283(14)
_cell_measurement_reflns_used    1881
_cell_measurement_temperature    223
_cell_measurement_theta_max      62.3530
_cell_measurement_theta_min      4.2370
_cell_volume                     3551.2(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      223.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1903
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.975
_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    -17.00  24.00   1.00    4.00    --    0.00 -99.00 -60.00   41
  2  \w     -1.00  24.00   1.00    6.00    --   48.75-126.00  60.00   25
  3  \w     35.00  96.00   1.00    6.00    --   48.75-126.00  60.00   61
  4  \w     52.00 134.00   1.00   10.00    --   97.50 -77.00  90.00   82
  5  \w     83.00 167.00   1.00   10.00    --   97.50  64.00   0.00   84
  6  \w     75.00 113.00   1.00    6.00    --   48.75 126.00  30.00   38
  7  \w     36.00  61.00   1.00    4.00    --    0.00 178.00  60.00   25
  8  \w     37.00  81.00   1.00    4.00    --    0.00 178.00-150.00   44
  9  \w    -44.00 -18.00   1.00   10.00    --  -92.00  12.00  30.00   26
 10  \w    -78.00  23.00   1.00    6.00    --  -48.75  57.00   0.00  101
 11  \w    -25.00  38.00   1.00    6.00    --   48.75 -99.00  90.00   63
 12  \w     19.00  65.00   1.00   10.00    --   97.50-112.00 120.00   46
 13  \w     23.00 126.00   1.00   10.00    --   97.50 -50.00 -60.00  103
 14  \w     25.00  71.00   1.00   10.00    --   97.50-112.00 -60.00   46
 15  \w    -94.00 -68.00   1.00   10.00    --  -92.00  64.00-120.00   26
 16  \w   -102.00 -68.00   1.00   10.00    --  -92.00 112.00-150.00   34
 17  \w   -106.00 -50.00   1.00   10.00    --  -92.00  12.00  30.00   56
 18  \w   -163.00-134.00   1.00   10.00    --  -92.00-161.00 -22.00   29
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0030568667
_diffrn_orient_matrix_UB_12      0.1335763333
_diffrn_orient_matrix_UB_13      0.0096177333
_diffrn_orient_matrix_UB_21      0.1171978000
_diffrn_orient_matrix_UB_22      0.0393516000
_diffrn_orient_matrix_UB_23      0.0315487000
_diffrn_orient_matrix_UB_31      0.1020138000
_diffrn_orient_matrix_UB_32      0.0692205000
_diffrn_orient_matrix_UB_33      -0.0364946000
_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  0.0358
_diffrn_reflns_av_unetI/netI     0.0345
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            3723
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        62.317
_diffrn_reflns_theta_max         62.317
_diffrn_reflns_theta_min         4.234
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.342
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66579
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light blue'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.973
_exptl_crystal_description       cube
_exptl_crystal_F_000             2115
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.953
_refine_diff_density_min         -0.699
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     119
_refine_ls_number_reflns         1231
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0445
_refine_ls_R_factor_gt           0.0430
_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^)+(0.0720P)^2^+22.8306P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1224
_refine_ls_wR_factor_ref         0.1244
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1173
_reflns_number_total             1231
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02370f2.cif
_cod_data_source_block           crv6
_cod_depositor_comments
'Adding full bibliography for 7717254--7717257.cif.'
_cod_original_cell_volume        3551.2(3)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7717255
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.176
_shelx_estimated_absorpt_t_min   0.176
_reflns_odcompleteness_completeness 99.09
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     61.08
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H,H,H) groups, All O(H) groups
2. Restrained distances
 O1W-H1WB = O1W-H1WA
 0.85 with sigma of 0.02
 H1WB-H1WA
 1.39 with sigma of 0.02
 N1-H1C
 0.85 with sigma of 0.02
 N1-H1D
 0.85 with sigma of 0.02
 H1C-H1D
 1.39 with sigma of 0.02
 H1D_$1-H1D
 1.39 with sigma of 0.02
 H1D-H1D_$2
 1.39 with sigma of 0.02
 H1D_$1-H1D_$2
 1.39 with sigma of 0.02
 O5-H5
 0.85 with sigma of 0.02
3. Others
 Fixed Sof: N2(0.833333)
4.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B)
;
_shelx_res_checksum              37742
_shelx_hkl_checksum              86291
_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 1.370
_oxdiff_exptl_absorpt_empirical_full_min 0.785