Synthesis, structural characterization and properties of a series of heteropolyoxomolybdates: [AlMo<sub>6</sub>(OH)<sub>6</sub>O<sub>18</sub>]<sup>3-</sup>, [GeMo<sub>12</sub>O<sub>40</sub>]<sup>4-</sup>, [GeMo<sub>6</sub>O<sub>22</sub>(Hmal)<sub>3</sub>]<sup>7-</sup>, [SiMo<sub>12</sub>O<sub>40</sub>]<sup>4-</sup>, and [TeMo<sub>6</sub>O<sub>24</sub>]<sup>6</sup>.
Kuzman, D.; Damjanović, V; Toplak, J.; Medak, G.; Halasz, I.; Hrenar, T.; Cindrić, M; Vrdoljak, V.; Dalton transactions (Cambridge, England : 2003) 55 (2026) 3442–3453; doi:10.1039/d5dt03064a

data_7720104
_publ_section_title
;
 Synthesis, structural characterization and properties of a series of
 heteropolyoxomolybdates:
 [AlMo<sub>6</sub>(OH)<sub>6</sub>O<sub>18</sub>]<sup>3-</sup>,
 [GeMo<sub>12</sub>O<sub>40</sub>]<sup>4-</sup>,
 [GeMo<sub>6</sub>O<sub>22</sub>(Hmal)<sub>3</sub>]<sup>7-</sup>,
 [SiMo<sub>12</sub>O<sub>40</sub>]<sup>4-</sup>, and
 [TeMo<sub>6</sub>O<sub>24</sub>]<sup>6</sup>.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3442
_journal_page_last               3453
_journal_paper_doi               10.1039/d5dt03064a
_journal_volume                  55
_journal_year                    2026
_chemical_formula_moiety         'Mo12 O40 Si, 4(C6 H16 Co N4 O4), 12[H2O]'
_chemical_formula_sum            'C24 H88 Co4 Mo12 N16 O68 Si'
_chemical_formula_weight         3104.19
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2025-12-10
_audit_creation_method
;
Olex2 1.5
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7314)
;
_audit_update_record
;
2025-12-10 deposited with the CCDC.	2026-01-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.415(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.0853(3)
_cell_length_b                   12.0278(3)
_cell_length_c                   25.9811(8)
_cell_measurement_reflns_used    5993
_cell_measurement_temperature    169.98(10)
_cell_measurement_theta_max      78.2130
_cell_measurement_theta_min      3.6950
_cell_volume                     4081.84(19)
_computing_cell_refinement       'CrysAlisPro 1.171.43.104a (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 41.123a 64-bit (release 20-01-2022))'
_computing_data_reduction        'CrysAlisPro 1.171.43.104a (Rigaku OD, 2023)'
_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_environment      N~2~
_diffrn_ambient_temperature      169.98(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.981
_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   -103.00 -68.00   0.50    3.50    --  -47.74 152.00  10.00   70
  2  \w    -82.00 -56.00   0.50    3.50    --  -47.74 122.00-149.00   52
  3  \w    -52.00 -19.00   0.50    3.50    --  -47.74 122.00-149.00   66
  4  \w    -92.00 -56.00   0.50    3.50    --  -47.74-152.00 -31.00   72
  5  \w     32.00  59.00   0.50    3.50    --   47.74-122.00 128.00   54
  6  \w     49.00  94.00   0.50    3.50    --   47.74-152.00 -31.00   90
  7  \w   -125.00-100.00   0.50   14.00    --  -91.75-152.00 -31.00   50
  8  \w   -143.00-118.00   0.50   14.00    --  -91.75-122.00 128.00   50
  9  \w    130.00 162.00   0.50   14.00    --  113.25 152.00  10.00   64
 10  \w     65.00  90.00   0.50   14.00    --  113.25-152.00 -31.00   50
 11  \w     76.00 101.00   0.50   14.00    --  113.25-122.00 128.00   50
 12  \w    113.00 138.00   0.50   14.00    --  113.25 122.00-149.00   50
 13  \w   -119.00 -88.00   0.50    3.50    --  -47.74 -77.00  60.00   62
 14  \w    -24.00  18.00   0.50    3.50    --  -47.74  19.00   0.00   84
 15  \w   -119.00 -92.00   0.50    3.50    --  -47.74 -77.00 150.00   54
 16  \w   -115.00 -90.00   0.50    3.50    --  -47.74 -77.00 -60.00   50
 17  \w   -119.00 -94.00   0.50    3.50    --  -47.74-125.00 -60.00   50
 18  \w    -49.00 -20.00   0.50   14.00    --  -91.75  45.00-120.00   58
 19  \w    -76.00 -51.00   0.50   14.00    --  -91.75 122.00-149.00   50
 20  \w    -51.00 -26.00   0.50   14.00    --  -91.75  45.00  60.00   50
 21  \w    100.00 126.00   0.50   14.00    --  113.25 125.00 150.00   52
 22  \w     44.00  70.00   0.50   14.00    --  113.25-125.00 150.00   52
 23  \w     42.00  69.00   0.50   14.00    --  113.25 -61.00-180.00   54
 24  \w     80.00 111.00   0.50   14.00    --  113.25-125.00 150.00   62
 25  \w     58.00  83.00   0.50   14.00    --  113.25 -95.00-180.00   50
 26  \w    132.00 177.00   0.50   14.00    --  113.25  61.00  30.00   90
 27  \w    106.00 150.00   0.50   14.00    --  113.25  61.00 -60.00   88
 28  \w     95.00 130.00   0.50   14.00    --  113.25 125.00 -60.00   70
 29  \w     52.00 106.00   0.50   14.00    --  113.25 -95.00  30.00  108
 30  \w    105.00 137.00   0.50   14.00    --  113.25  61.00 -30.00   64
 31  \w    120.00 146.00   0.50   14.00    --  113.25  30.00  30.00   52
 32  \w    100.00 144.00   0.50   14.00    --  113.25  77.00-120.00   88
 33  \w     91.00 138.00   0.50   14.00    --  113.25  77.00 -60.00   94
 34  \w    134.00 178.00   0.50   14.00    --  113.25 125.00 -60.00   88
 35  \w    105.00 153.00   0.50   14.00    --  113.25  45.00 -60.00   96
 36  \w     55.00 103.00   0.50   14.00    --  113.25 -77.00  60.00   96
 37  \w    101.00 175.00   0.50   14.00    --  113.25  61.00   0.00  148
 38  \w     42.00  84.00   0.50   14.00    --  113.25 -81.00 -94.81   84
 39  \w    100.00 125.00   0.50   14.00    --  113.25 -81.00 -94.81   50
 40  \w     46.00  86.00   0.50   14.00    --  113.25 -95.00-150.00   80
 41  \w     48.00  98.00   0.50   14.00    --  113.25 -77.00 -90.00  100
 42  \w    108.00 177.00   0.50   14.00    --  113.25 125.00-180.00  138
 43  \w     96.00 121.00   0.50   14.00    --  113.25 125.00   0.00   50
 44  \w    132.00 170.00   0.50   14.00    --  113.25  60.00   8.12   76
 45  \w     67.00 104.00   0.50   14.00    --  113.25 -77.00-120.00   74
 46  \w     73.00 116.00   0.50   14.00    --  113.25 -83.00-175.67   86
 47  \w    139.00 165.00   0.50   14.00    --  113.25 125.00   0.00   52
 48  \w     55.00  80.00   0.50   14.00    --  113.25 -95.00 -30.00   50
 49  \w    108.00 144.00   0.50   14.00    --  113.25  15.00-150.00   72
 50  \w    117.00 153.00   0.50   14.00    --  113.25  61.00  60.00   72
 51  \w    103.00 159.00   0.50   14.00    --  113.25  30.00 150.00  112
 52  \w    116.00 178.00   0.50   14.00    --  113.25  61.00 -90.00  124
 53  \w    107.00 137.00   0.50   14.00    --  113.25  45.00-120.00   60
 54  \w    135.00 168.00   0.50   14.00    --  113.25  61.00  90.00   66
 55  \w    141.00 167.00   0.50   14.00    --  113.25 125.00 150.00   52
 56  \w     63.00 101.00   0.50   14.00    --  113.25 -95.00-120.00   76
 57  \w    108.00 133.00   0.50   14.00    --  113.25  45.00  60.00   50
 58  \w    153.00 178.00   0.50   14.00    --  113.25  30.00 -30.00   50
 59  \w    132.00 158.00   0.50   14.00    --  113.25  15.00  60.00   52
 60  \w    152.00 177.00   0.50   14.00    --  113.25  61.00-180.00   50
 61  \w     59.00 109.00   0.50   14.00    --  113.25 -80.00 -30.86  100
 62  \w     42.00  67.00   0.50   14.00    --  113.25 -61.00 -90.00   50
;
_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      0.0133928000
_diffrn_orient_matrix_UB_12      -0.0137726000
_diffrn_orient_matrix_UB_13      -0.0581587000
_diffrn_orient_matrix_UB_21      0.0535790000
_diffrn_orient_matrix_UB_22      -0.1125242000
_diffrn_orient_matrix_UB_23      0.0103844000
_diffrn_orient_matrix_UB_31      -0.1042025000
_diffrn_orient_matrix_UB_32      -0.0596564000
_diffrn_orient_matrix_UB_33      -0.0061312000
_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  0.1403
_diffrn_reflns_av_unetI/netI     0.0882
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            53526
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.289
_diffrn_reflns_theta_min         4.998
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    22.021
_exptl_absorpt_correction_T_max  0.642
_exptl_absorpt_correction_T_min  0.070
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.104a (Rigaku Oxford Diffraction, 2023)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    2.526
_exptl_crystal_description       block
_exptl_crystal_F_000             3028
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         3.039
_refine_diff_density_min         -2.793
_refine_diff_density_rms         0.252
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     562
_refine_ls_number_reflns         8760
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0861
_refine_ls_R_factor_gt           0.0766
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1250P)^2^+26.6924P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2048
_refine_ls_wR_factor_ref         0.2144
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7344
_reflns_number_total             8760
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt03064a2.cif
_cod_data_source_block           exp_7898
_cod_depositor_comments
'Adding full bibliography for 7720101--7720111.cif.'
_cod_database_code               7720104
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Si Mo12 O62 Co4 N16 C24 H50'
_cell_oxdiff_angle_alpha         89.9812(19)
_cell_oxdiff_angle_beta          93.408(2)
_cell_oxdiff_angle_gamma         90.008(2)
_cell_oxdiff_length_a            13.0854(3)
_cell_oxdiff_length_b            12.0252(3)
_cell_oxdiff_length_c            25.9807(6)
_cell_oxdiff_measurement_reflns_used 6101
_cell_oxdiff_volume              4080.94(17)
_shelx_estimated_absorpt_t_max   0.558
_shelx_estimated_absorpt_t_min   0.137
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
2. Restrained distances
 O9A-O25_$1
 2.9 with sigma of 0.0001
3. Uiso/Uaniso restraints and constraints
Uanis(O14B) = Uanis(O14A)
Uanis(O17B) = Uanis(O17A)
Uanis(O21B) = Uanis(O21A)
Uanis(O19A) = Uanis(O19B)
Uanis(O20B) = Uanis(O20A)
Uanis(O6B) = Uanis(O6A)
Uanis(O15A) = Uanis(O15B)
Uanis(O9B) = Uanis(O9A)
Uanis(O8A) = Uanis(O8B)
Uanis(O7A) = Uanis(O7B)
Uanis(O12B) = Uanis(O12A)
4. Others
 Fixed Sof: O3(0.5) O2(0.5) O1(0.5) O4(0.5) O21A(0.5) O21B(0.5) O17A(0.5)
 O17B(0.5) O19B(0.5) O19A(0.5) O14B(0.5) O14A(0.5) O20A(0.5) O20B(0.5) O6A(0.5)
 O6B(0.5) O15A(0.5) O15B(0.5) O9A(0.5) O9B(0.5) O8A(0.5) O8B(0.5) O7A(0.5)
 O7B(0.5) O12B(0.5) O12A(0.5)
5.a Secondary CH2 refined with riding coordinates:
 N6(H6A,H6B), N3(H3A,H3B), N2(H2A,H2B), N5(H5A,H5B), N7(H7A,H7B), N8(H8A,H8B),
 N1(H1A,H1B), N4(H4A,H4B), C3(H3C,H3D), C8(H8C,H8D), C7(H7C,H7D), C4(H4C,H4D),
 C10(H10A,H10B), C9(H9A,H9B), C2(H2C,H2D), C1(H1C,H1D)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 240 electrons were 
found in a volume of 710\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
12[H2O] per Formula Unit 
which account for 240 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              48047
_shelx_hkl_checksum              71878
_shelx_fab_checksum              75172
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.253
_oxdiff_exptl_absorpt_empirical_full_min 0.265