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_7717257
_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 Fe O30 V6, 2(O4 S), 7(H4 N), 7(H2 O)'
_chemical_formula_sum            'C12 H60 Fe N7 O45 S2 V6'
_chemical_formula_weight         1448.28
_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   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                 93.255(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.7200(5)
_cell_length_b                   11.1750(3)
_cell_length_c                   21.0112(4)
_cell_measurement_reflns_used    3739
_cell_measurement_temperature    195(2)
_cell_measurement_theta_max      28.3310
_cell_measurement_theta_min      3.4630
_cell_volume                     4857.2(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      195
_diffrn_detector_area_resol_mean 16.1903
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.865
_diffrn_measurement_details
;
  1 omega  -92.00   21.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.6309  -26.0000   42.0000 113

  2 omega   34.00   76.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       21.8809 -116.0000  142.0000 42

  3 omega  -27.00   42.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.6309   57.0000 -150.0000 69

  4 omega   56.00   81.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       21.8809   77.0000  -30.0000 25
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0004579000
_diffrn_orient_matrix_UB_12      -0.0120772000
_diffrn_orient_matrix_UB_13      -0.0331239000
_diffrn_orient_matrix_UB_21      0.0328209000
_diffrn_orient_matrix_UB_22      -0.0177364000
_diffrn_orient_matrix_UB_23      0.0041385000
_diffrn_orient_matrix_UB_31      -0.0098455000
_diffrn_orient_matrix_UB_32      -0.0597438000
_diffrn_orient_matrix_UB_33      0.0054815000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0301
_diffrn_reflns_av_unetI/netI     0.0423
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.865
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            10712
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.865
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.826
_diffrn_reflns_theta_min         2.878
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.608
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88633
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark blue'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.980
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2948
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.756
_refine_diff_density_min         -0.466
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     404
_refine_ls_number_reflns         5496
_refine_ls_number_restraints     47
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0346
_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^)+(0.0321P)^2^+8.4121P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0836
_refine_ls_wR_factor_ref         0.0871
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4844
_reflns_number_total             5496
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02370f2.cif
_cod_data_source_block           fev6
_cod_depositor_comments
'Adding full bibliography for 7717254--7717257.cif.'
_cod_original_cell_volume        4857.20(19)
_cod_database_code               7717257
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All O(H,H) groups, All O(H,H,H,H,H,H,H,H,H,H,H,H,H,H,H,H,
  H,H) groups
2. Restrained distances
 O1W-H1WA
 0.85 with sigma of 0.01
 O1W-H1WB
 0.85 with sigma of 0.01
 H1WA-H1WB
 1.39 with sigma of 0.01
 O2W-H2WA
 0.85 with sigma of 0.01
 O2W-H2WB
 0.85 with sigma of 0.01
 H2WA-H2WB
 1.39 with sigma of 0.01
 O3W-H3WB
 0.85 with sigma of 0.01
 O3W-H3WA
 0.85 with sigma of 0.01
 H3WB-H3WA
 1.39 with sigma of 0.01
 N2-H2A = N2-H2C = N2-H2D = N2-H2B = N3-H3E = N3-H3C = N3-H3D = N3-H3F = N4-
 H4B = N4-H4C = N4-H4A = N4-H4D = N1-H1C = N1-H1D
 0.85 with sigma of 0.02
 H2A-H2D
 1.39 with sigma of 0.02
 H2A-H2C
 1.39 with sigma of 0.02
 H2A-H2B
 1.39 with sigma of 0.02
 H2B-H2D
 1.39 with sigma of 0.02
 H2C-H2D
 1.39 with sigma of 0.02
 H2C-H2B
 1.39 with sigma of 0.02
 H3F-H3C
 1.39 with sigma of 0.02
 H3D-H3C
 1.39 with sigma of 0.02
 H3D-H3F
 1.39 with sigma of 0.02
 H3E-H3D
 1.39 with sigma of 0.02
 H3E-H3F
 1.39 with sigma of 0.02
 H3E-H3C
 1.39 with sigma of 0.02
 H4B-H4A
 1.39 with sigma of 0.02
 H4B-H4D
 1.39 with sigma of 0.02
 H4C-H4A
 1.39 with sigma of 0.02
 H4A-H4D
 1.39 with sigma of 0.02
 H4C-H4B
 1.39 with sigma of 0.02
 H4C-H4D
 1.39 with sigma of 0.02
 H1C-H1D
 1.39 with sigma of 0.02
 H1C-H1D_$1
 1.39 with sigma of 0.02
 O13-H13 = O14_$2-H14_$2 = O15-H15
 0.85 with sigma of 0.02
 H2WA-H2WA_$1
 2.3 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C3(H3A,H3B), C5(H5A,H5B)
;
_shelx_res_checksum              11968
_shelx_hkl_checksum              40279
_olex2_submission_special_instructions 'No special instructions were received'