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_7717256
_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 Al O30 V6, 2(O4 S), 2(H4 N), 6(H2 O), 0.833(N6)'
_chemical_formula_sum            'C12 H38 Al N7 O44 S2 V6'
_chemical_formula_weight         1381.23
_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                   11.3926(5)
_cell_length_b                   11.3926(5)
_cell_length_c                   31.4864(18)
_cell_measurement_reflns_used    1624
_cell_measurement_temperature    173.9(6)
_cell_measurement_theta_max      27.1800
_cell_measurement_theta_min      3.5640
_cell_volume                     3539.2(3)
_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      173.9(6)
_diffrn_detector_area_resol_mean 16.1903
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.892
_diffrn_measurement_details
;
  1 omega  -88.00    8.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.6935  -38.0000  150.0000 96

  2 omega  -86.00  -35.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.6935 -178.0000  -60.0000 51

  3 omega  -41.00   51.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.6935   38.0000  -30.0000 92

  4 omega   57.00   82.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       24.0997  178.0000   60.0000 25
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0544626333
_diffrn_orient_matrix_UB_12      0.0066767667
_diffrn_orient_matrix_UB_13      -0.0126851333
_diffrn_orient_matrix_UB_21      -0.0082254000
_diffrn_orient_matrix_UB_22      0.0445562000
_diffrn_orient_matrix_UB_23      -0.0138032000
_diffrn_orient_matrix_UB_31      0.0462205667
_diffrn_orient_matrix_UB_32      0.0559858333
_diffrn_orient_matrix_UB_33      0.0125075333
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0385
_diffrn_reflns_av_unetI/netI     0.0472
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.892
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            6126
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.892
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.793
_diffrn_reflns_theta_min         3.311
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.375
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98473
_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            'light blue'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.944
_exptl_crystal_description       block
_exptl_crystal_F_000             2082
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.366
_refine_diff_density_min         -0.650
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     119
_refine_ls_number_reflns         2018
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0710
_refine_ls_R_factor_gt           0.0582
_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^)+(0.0798P)^2^+22.9439P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1530
_refine_ls_wR_factor_ref         0.1618
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1691
_reflns_number_total             2018
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02370f2.cif
_cod_data_source_block           alv6
_cod_depositor_comments
'Adding full bibliography for 7717254--7717257.cif.'
_cod_original_cell_volume        3539.2(4)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7717256
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All O(H,H,H,H,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
3. Others
 Fixed Sof: N2(0.833333)
4.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B)
;
_shelx_res_checksum              17350
_shelx_hkl_checksum              25073
_olex2_date_sample_completion    2016-09-23
_olex2_date_sample_data_collection 2016-09-23
_olex2_submission_special_instructions 'No special instructions were received'