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_7717254
_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 O30 V7, 10(H2 O), 2.5(H4 N), 0.5(N)'
_chemical_formula_sum            'C12 H48 N3 O40 V7'
_chemical_formula_weight         1231.11
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_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                90
_cell_formula_units_Z            4
_cell_length_a                   21.2465(18)
_cell_length_b                   9.7088(5)
_cell_length_c                   22.0761(13)
_cell_measurement_reflns_used    2486
_cell_measurement_temperature    223
_cell_measurement_theta_max      62.3580
_cell_measurement_theta_min      4.1400
_cell_volume                     4553.8(5)
_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 0.990
_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     42.00  81.00   1.00    5.00    --    0.00 178.00 -60.00   39
  2  \w     36.00  69.00   1.00    5.00    --    0.00 178.00-180.00   33
  3  \w   -119.00 -22.00   1.00   36.77    --  -48.75 -57.00   0.00   97
  4  \w    -77.00 -31.00   1.00   36.77    --  -48.75 126.00-180.00   46
  5  \w     87.00 117.00   1.00   36.77    --   48.75 126.00 -30.00   30
  6  \w     75.00 107.00   1.00   36.77    --   48.75 126.00 -90.00   32
  7  \w     54.00  80.00   1.00   36.77    --   97.50-112.00-180.00   26
  8  \w     69.00 163.00   1.00   36.77    --   97.50  64.00 -90.00   94
  9  \w     36.00 124.00   1.00   36.77    --   97.50 -64.00 -90.00   88
 10  \w     90.00 159.00   1.00   36.77    --   97.50  64.00  30.00   69
 11  \w     58.00 106.00   1.00   36.77    --   97.50 -64.00  30.00   48
;
_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      0.0410239000
_diffrn_orient_matrix_UB_12      -0.0606515000
_diffrn_orient_matrix_UB_13      0.0509117000
_diffrn_orient_matrix_UB_21      0.0231642000
_diffrn_orient_matrix_UB_22      -0.1134703000
_diffrn_orient_matrix_UB_23      -0.0433754000
_diffrn_orient_matrix_UB_31      0.0551493000
_diffrn_orient_matrix_UB_32      0.0929393000
_diffrn_orient_matrix_UB_33      -0.0197679000
_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  0.0624
_diffrn_reflns_av_unetI/netI     0.0647
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            8421
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        62.317
_diffrn_reflns_theta_max         62.317
_diffrn_reflns_theta_min         4.005
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.586
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38058
_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 green'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.796
_exptl_crystal_description       plank
_exptl_crystal_F_000             2488
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.444
_refine_diff_density_min         -1.466
_refine_diff_density_rms         0.206
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.164
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         3581
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      1.160
_refine_ls_R_factor_all          0.1067
_refine_ls_R_factor_gt           0.0961
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2678
_refine_ls_wR_factor_ref         0.2907
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2959
_reflns_number_total             3581
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02370f2.cif
_cod_data_source_block           v7
_cod_depositor_comments
'Adding full bibliography for 7717254--7717257.cif.'
_cod_database_code               7717254
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.787
_shelx_estimated_absorpt_t_min   0.116
_reflns_odcompleteness_completeness 99.67
_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,H,H,H,H,H,H,H,H,H,H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O14-H14 = O15-H15 = O13-H13
 0.85 with sigma of 0.02
 O5W-H5WB = O5W-H5WA
 0.85 with sigma of 0.02
 H5WB-H5WA
 1.39 with sigma of 0.02
 H3D-N3
 0.85 with sigma of 0.02
 H3C-H3D
 1.39 with sigma of 0.02
 H3D-H3C_$1
 1.39 with sigma of 0.02
 H3C-H3C_$1
 1.39 with sigma of 0.02
 H3D-H3D_$1
 1.39 with sigma of 0.02
 N1-H1F = N1-H1D = N1-H1C
 0.85 with sigma of 0.02
 H1E-H1D
 1.39 with sigma of 0.02
 H1F-H1C
 1.39 with sigma of 0.02
 H1E-N1
 0.85 with sigma of 0.02
 H1F-H1D
 1.39 with sigma of 0.02
 H1E-H1C
 1.39 with sigma of 0.02
 H1C-H1D
 1.39 with sigma of 0.02
 H1E-H1F
 1.39 with sigma of 0.02
 O2W-H2WA
 0.85 with sigma of 0.02
 N2-H5WB
 2.145 with sigma of 0.02
 O5W_$2-H2WA
 1.934 with sigma of 0.02
 H2WB-H2WA
 1.39 with sigma of 0.02
 O2W-H2WB
 0.85 with sigma of 0.02
 O2W_$3-H5WA
 3 with sigma of 0.02
 N2-H4WA
 1.734 with sigma of 0.001
 O4W-H4WA
 0.85 with sigma of 0.001
 O3_$4-H4WB
 1.896 with sigma of 0.02
 O4W-H4WB
 0.85 with sigma of 0.02
 H4WB-H4WA
 1.39 with sigma of 0.02
 H4WB-O14
 3 with sigma of 0.02
3. Others
 Fixed Sof: N3(0.25) N2(0.25) H3C(0.5) H3D(0.5)
4.a Riding coordinates:
 N2(H15,H14,H13,H5WA,H5WB,H3C,H3D,H1C,H1D,H1E,H1F,H2WA,H2WB,H4WA,H4WB)
4.b Free rotating group:
 O3W(H3WA,H3WB), O1W(H1WA,H1WB)
4.c Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C5(H5A,H5B), C3(H3A,H3B)
;
_shelx_res_checksum              53433
_shelx_hkl_checksum              6890
_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 2.196
_oxdiff_exptl_absorpt_empirical_full_min 0.531